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Supplemental Data The crystal structure of a valinomycin•2Ca 2+ complex and the multi-step solution equilibria in acetonitrile characterized by 1 H NMR, UV-Vis, and mass spectrometry Alisha A. Contractor, § Amaan M. Kazerouni, § Anna R. Michmerhuizen, † Margaret L. Falkenberry, § Rigoberto Segovia, § Nicholas M. Blair, § SeongEun Kim, † Douglas A. Vander Griend, † John Bacsa, ‡ Farooq A. Khan, § Megumi Fujita* § § Department of Chemistry, University of West Georgia, Carrollton, GA 30118 † Department of Chemistry and Biochemistry, Calvin College, Grand Rapids, MI 49546 ‡ X-ray Crystallography Center, Emory University, Atlanta, GA 30322 Contents: I. 13 C and 1 H NMR spectra of the crystal sample E (valinomycin·Ca 2 ·(OTf) 4 ·5.0 H 2 O·1.0CH 3 CN) II. Global analysis results (Sivvu™) III. X-ray crystallography data of the crystal sample A IV. X-ray crystallography data of the crystal sample B I. 1 H and 13 C NMR spectra of the crystal sample E (valinomycin·Ca 2 ·(OTf) 4 ·5.0 H 2 O·1.0CH 3 CN) S1
Transcript of s3-eu-west-1.amazonaws.com€¦ · Web view‡ X-ray Crystallography Center, Emory University,...
Supplemental DataThe crystal structure of a valinomycin•2Ca2+ complex and the multi-step solution equilibria in acetonitrile characterized by 1H NMR, UV-Vis, and mass spectrometry
Alisha A. Contractor,§ Amaan M. Kazerouni,§ Anna R. Michmerhuizen,† Margaret L. Falkenberry,§ Rigoberto Segovia,§ Nicholas M. Blair,§ SeongEun Kim,† Douglas A. Vander Griend,† John Bacsa,‡ Farooq A. Khan,§ Megumi Fujita*§
§ Department of Chemistry, University of West Georgia, Carrollton, GA 30118 † Department of Chemistry and Biochemistry, Calvin College, Grand Rapids, MI 49546‡ X-ray Crystallography Center, Emory University, Atlanta, GA 30322
Contents:
I. 13C and 1H NMR spectra of the crystal sample E (valinomycin·Ca2·(OTf)4·5.0 H2O·1.0CH3CN)
II. Global analysis results (Sivvu™) III. X-ray crystallography data of the crystal sample AIV. X-ray crystallography data of the crystal sample B
I. 1H and 13C NMR spectra of the crystal sample E (valinomycin·Ca2·(OTf)4·5.0 H2O·1.0CH3CN)
0.51.01.52.02.53.03.54.04.55.05.56.06.57.07.58.08.59.0f1 (ppm)
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80MFCV050_xtals
MFCV-050 Crystals from Val + 3Ca(OTf)2 batch in wet CH3CN
integrate H2O and CH3CN!15
.95
40.0
2
9.04
13.0
3
6.39
18.8
31.
78
3.96
2.00
5.04
0.95
2.14
2.13
2.00
0.81
1.02
1.35
1.36
1.42
1.43
1.47
1.48
2.08
2.09
2.10
2.12
2.29
2.44
3.98
3.99
4.00
4.02
4.03
4.04
4.06
4.07
4.08
4.61
4.63
4.67
4.69
4.93
4.94
4.97
4.98
4.99
5.00
5.01
5.02
5.03
5.05
5.23
5.24
7.61
7.64
7.66
7.79
7.83
7.94
S1
1H NMR spectrum / CD3CN
0102030405060708090100110120130140150160170180f1 (ppm)
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180MFCV050_xtals_13C
MFCV-050 Crystals from Val + 3Ca(OTf)2 batch in wet CH3CN
integrate H2O and CH3CN!
13C NMR spectra, selected regions
162163164165166167168169170171172173174175176177178179180181182f1 (ppm)
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MFCV-050 Crystals from Val + 3Ca(OTf)2 batch in wet CH3CN
integrate H2O and CH3CN!
169.26
169.91
170.04
170.15
170.28
17
0.7
8
171.46
17
1.7
5
172.29
172.83
172.89
173.57
Carbonyl x 12
556065707580859095100105
f1 (ppm)
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MFCV050_xtals_13C
MFCV-050 Crystals from Val + 3Ca(OTf)2 batch in wet CH3CN
integrate H2O and CH3CN!
56
.22
56
.25
56
.35
56
.46
59
.44
59
.53
59
.58
59
.94
60
.03
60
.19
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.30
68
.56
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.70
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.06
69
.17
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.06
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.19
76
.32
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.46
78
.14
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.23
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.11
79
.19
alpha-C x3L-LA
alpha-C x 3D-HiVA
alpha-C x 6 D/L-Val
14151617181920212223242526272829303132333435363738394041424344454647484950f1 (ppm)
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MFCV-050 Crystals from Val + 3Ca(OTf)2 batch in wet CH3CN
integrate H2O and CH3CN!
14.9
015.5
515.8
116.0
316.0
916.5
116.5
516.6
517.2
117.5
31
7.7
517.9
217.9
618.2
118.3
718.6
318.8
718.8
9
28.7
828.8
428.8
929.0
029.6
530.0
530.3
531.4
9
beta-C (3x3 = 9)L-LA CH3 (1 x 3 = 4 )iPr CH3s(3 x 3 = 9)
S2
13C NMR spectrum
/ CD3CN
II. Global analysis results (Sivvu™)
II-a) 1.00 mM valinomycin in semi-dried acetonitrile (ca. 0.08M H2O) titrated with (10.0 mM Ca(OTf)2 and 1.00 mM valinomycin) from 0 to 2.6 equivalents of Ca2+ at 293 K.
Binding model logKV + (CaOTf)+ V(CaOTf)+
V(CaOTf)+ + OTf- [VCa(OTf)2]+
logK1 = 5.3(2)logK2 = 4.30(3)
Table S1. Summary of three titration experiments
Exp. A B ClogK1 5.20 5.52 5.25logK1 stdev 0.004 0.02 0.01logK2 4.26 4.31 4.32logK2 stdev 0.01 0.02 0.01RMS Residual 0.003479 0.003583 0.003452% Reconstruction 99.66% 99.33% 99.54%R2 0.999371 0.999357 0.999644
SIVVU output from Experiment A
S3
S4
II-b) 1.00 mM valinomycin in water-added acetonitrile (ca. 0.64 M H2O) titrated with (10.0 mM Ca(OTf)2 and 1.00 mM valinomycin) from 0 to 2.6 equivalents of Ca2+ at 293 K.
Binding model logKV + Ca2+ VCa2+
V + VCa2+ V2Ca2+
logK1 = 4.0(2)logK2 = 3.6(5)
Table S2. Summary of three titration experiments
Exp. D E FlogK1 3.84 3.95 4.21logK1 stdev 0.02 0.03 0.04logK2 3.08 3.73 3.96logK2 stdev 0.05 0.02 0.05RMS Residual 0.002215 0.00198 0.001504% Reconstruction 99.77% 99.72% 99.73%R2 0.9985 0.998854 0.999825
SIVVU output from Experiment F
S5
II-c) 1.00 mM valinomycin in semi-dried acetonitrile titrated with (10.00 mM KOTf and 1.00 mM valinomycin) from 0 t0 1.5 equivalents of K+ at 293 K.
Binding model logKV + K+ [VK]+ logK =
6.4(6)
Table S3. Summary of three titration experiments
Exp. G H IlogK 6.08 6.06 7.03logK stdev 0.004 0.003 0.001RMS Residual 0.007152 0.011474 0.00583% Reconstruction 99.58% 99.53% 99.82%R2 0.997785 0.996073 0.998902
SIVVU output from Experiment H
S6
II-d) 1.00 mM valinomycin in water-added acetonitrile titrated with (10.00 mM KOTf and 1.00 mM valinomycin) from 0 to 1.5 equivalents of K+ at 293 K.
Binding model logKV + K+ [VK]+ logK =
6.5(3)
Table S4. Summary of three titration experiments
Exp. J K LlogK 6.95 6.44 6.14logK stdev 0.038 0.014 0.019RMS Residual 0.006101 0.006439 0.006951% Reconstruction 99.66% 99.86% 99.40%R2 0.998746 0.998765 0.998512
SIVVU output from Experiment J
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S8
III. X-ray crystallography data of the crystal samples A, [(valinomycin)Ca2(OTf)2(H2O)2](OTf)2·4(CH3CN)Crystal Data and Experimental
Experimental. A suitable crystal (0.23 × 0.20 × 0.13 mm3) was selected and mounted on a loop with paratone oil on a Bruker APEX-II CCD diffractometer. The crystal was cooled to T = 110(2) K during data collection. The structure was solved with the Superflip (L. Palatinus & G.
Chapuis, 2007) using the Charge Flipping solution method. The structure was refined with version 2014/6 of XL (Sheldrick, 2008) using Least Squares minimization.Crystal Data. C66H106Ca2F12N10O32S4, Mr = 1988.00, triclinic, P1 (No. 1), a = 12.0584(12) Å, b = 14.2293(14) Å, c = 15.0829(15) Å, = 69.9040(10)°, = 79.4170(10)°, = 77.4120(10)°, V = 2355.2(4) Å3, T = 110(2) K, Z = 1, Z' = 1, (MoK) = 0.314, 23236 reflections measured, 16942 unique (Rint = 0.0288) which were used in all calculations. The final wR2 was 0.1316 (all data) and R1 was 0.0526 (I > 2(σI)).
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Sample AFormula C
66H106Ca2F12N10O32S4Dcalc./ g cm-3 1.402/mm-1 0.314Formula Weight 1988.00Color colorlessShape prismMax Size/mm 0.23Mid Size/mm 0.20Min Size/mm 0.13T/K 110(2)Crystal System triclinicSpace Group P1a/Å 12.0584(12)b/Å 14.2293(14)c/Å 15.0829(15)/° 69.9040(10)/° 79.4170(10)/° 77.4120(10)V/Å3 2355.2(4)Z 1Z' 1min/° 1.448max/° 26.733Measured Refl. 23236Independent Refl. 16942Reflections I > 2(σI) 14328Rint 0.0288Parameters 1201Restraints 218Largest Peak 0.721Deepest Hole -0.707GooF 1.027wR2 (all data) 0.1316wR2 0.1235R1 (all data) 0.0656R1 0.0526Experimental Extended. A colorless prism-shaped crystal with dimensions 0.23 × 0.20 × 0.13 mm3 was mounted on a loop with paratone oil. Data were collected using a Bruker APEX-II CCD diffractometer equipped with an Oxford Cryostream low-temperature apparatus operating at T = 110(2) K.Data were measured using and scans of 0.50° per frame for 60 s using MoK radiation (fine-focus sealed tube, 45 kV, 35 mA). The total number of runs and images was based on the strategy calculation from the program APEX2 (Bruker, 2014). The resolution that was achieved was = 26.733°.Unit cell indexing was performed by using the APEX2 (Bruker, 2014) software and the cell parameters were refined using SAINT (Bruker, V8.34A, 2013) on 7074 reflections, 30% of the observed reflections.Data reduction was performed using the SAINT (Bruker, V8.34A, 2013) software. The final completeness is 100% out to 26.733° in . The absorption coefficient (μ) of this
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material is 0.314 mm-1 and the minimum and maximum transmissions are 0.5905 and 0.7456.The structure was solved by Charge Flipping using the Superflip (L. Palatinus & G. Chapuis, 2007) structure solution program and refined by Least Squares using version 2014/6 of XL (Sheldrick, 2008).The structure was solved in the space group P1 (# 1). All non-hydrogen atoms were refined anisotropically. Hydrogen positions were calculated geometrically and refined using the riding model.The Flack parameter was refined to 0.015(19), confirming the absolute stereochemistry. Determination of absolute structure using Bayesian statistics on Bijvoet differences using the program within PLATON (Spek, 2003) also report that we have the correct enantiomer based on this comparison. ________________________________________________________________________________ Table 1. Atomic coordinates ( x 104) and equivalent isotropic displacement parameters (Å2x 103)for Sample A. U(eq) is defined as one third of the trace of the orthogonalized Uij tensor.________________________________________________________________________________
x y z U(eq)________________________________________________________________________________ C(13) -736(4) 526(4) 9244(4) 21(1)C(7) 5662(4) 2629(4) 4218(3) 21(1)C(55) 1304(5) 2214(5) 4173(4) 36(1)C(11) 1588(4) -107(4) 7467(4) 24(1)C(14) -632(4) 2228(4) 9201(4) 20(1)C(38) 1379(5) -501(4) 6707(4) 28(1)C(12) 490(5) 322(4) 8783(4) 23(1)C(9) 3762(4) 1665(4) 6441(4) 24(1)C(8) 4510(4) 1638(4) 5514(4) 22(1)C(10) 2067(4) 878(4) 7018(4) 20(1)C(6) 4866(4) 2998(4) 3455(4) 20(1)C(5) 4334(5) 2889(4) 2033(4) 26(1)C(4) 4363(4) 3995(4) 1440(4) 24(1)C(3) 3252(5) 5448(4) 503(4) 28(1)C(2) 3266(4) 6125(4) 1102(4) 23(1)C(1) 3389(5) 7820(4) 1088(4) 25(1)C(24) 2215(4) 7930(4) 1655(4) 22(1)C(23) 1308(4) 8149(4) 3134(4) 22(1)C(22) 720(5) 7217(4) 3391(4) 24(1)C(21) -1056(5) 6546(4) 3763(4) 25(1)C(20) -1831(5) 6574(4) 4668(4) 26(1)C(19) -3030(4) 5620(4) 5935(4) 25(1)C(18) -2176(5) 5201(4) 6663(4) 25(1)N(5) -2215(4) 5719(3) 7248(3) 28(1)C(17) -1360(5) 5443(4) 7890(4) 30(1)C(16) -1604(5) 4489(4) 8722(4) 26(1)C(15) -678(5) 2953(4) 9762(4) 25(1)C(42) 337(5) 2679(4) 10321(4) 33(1)C(43) 279(7) 3450(5) 10836(5) 44(2)C(44) 1468(5) 2580(5) 9702(5) 42(2)C(45) -1309(5) 6367(5) 8183(4) 37(1)C(47) -953(7) 7233(5) 7309(6) 54(2)C(46) -500(6) 6116(5) 8918(5) 41(2)C(48) -3818(5) 4901(5) 6035(4) 34(1)C(49) -1684(5) 6561(4) 2965(4) 31(1)C(50) -2500(5) 7566(5) 2621(5) 40(2)C(51) -845(6) 6333(5) 2147(4) 42(2)C(52) 1708(5) 8211(5) 4016(4) 30(1)C(54) 2384(5) 9091(5) 3740(5) 39(2)
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C(53) 700(5) 8321(5) 4772(4) 42(2)C(25) 3598(5) 8847(4) 329(4) 29(1)C(26) 3201(7) 9713(5) 761(5) 44(2)C(27) 4876(6) 8778(5) -42(5) 42(2)C(28) 2129(6) 5715(5) 104(5) 38(2)C(29) 4653(6) 2195(5) 1409(5) 45(1)C(30) 5815(7) 2242(6) 875(5) 57(2)C(31) 4483(8) 1128(6) 1978(6) 68(2)C(32) 6389(4) 3420(4) 4129(4) 23(1)C(33) 6972(5) 3817(5) 3126(4) 34(1)C(34) 7247(5) 2972(5) 4856(4) 32(1)C(35) 4484(5) 1759(5) 7161(4) 33(1)C(36) 5490(5) 888(5) 7364(4) 40(2)C(37) 3698(6) 1813(6) 8060(5) 46(2)C(39) -1138(5) -432(4) 9966(4) 26(1)C(41) -2442(5) -218(5) 10208(4) 36(1)C(40) -803(6) -1350(5) 9599(5) 41(2)O(22A) 678(5) 5710(4) 5735(4) 33(1)S(1A) 1583(1) 4866(1) 5984(1) 21(1)C(56A) 2497(5) 5243(3) 6599(4) 36(2)F(4A) 2918(6) 6065(4) 6036(5) 60(2)F(5A) 1927(5) 5447(6) 7371(4) 54(2)F(6A) 3372(4) 4507(4) 6882(4) 42(1)O(22B) 3378(11) 4094(10) 6783(13) 42(1)S(1B) 2377(3) 4417(3) 6298(2) 28(1)C(56B) 1789(7) 5680(6) 6395(7) 36(2)F(4B) 2515(11) 6323(7) 5952(14) 60(2)F(5B) 1566(15) 5659(11) 7297(8) 54(2)F(6B) 812(8) 6049(7) 6014(9) 42(1)N(4) -826(4) 1292(3) 9710(3) 23(1)N(3) 3193(4) 792(3) 6835(3) 22(1)N(2) 5093(4) 2569(3) 2775(3) 25(1)N(1) 3476(4) 7056(3) 610(3) 24(1)N(6) -395(4) 7374(3) 3472(3) 22(1)O(6) -2352(3) 5748(3) 5010(3) 24(1)O(4) -631(3) 3948(3) 9068(3) 28(1)O(19) 1313(4) 6368(3) 3545(3) 39(1)O(7) 2336(3) 8001(3) 2498(3) 24(1)O(3) 486(3) 90(3) 7987(3) 22(1)O(1) 3363(3) 4407(3) 1090(3) 26(1)O(21) 1352(3) 3925(2) 6726(3) 39(1)O(20) 2473(3) 4621(3) 5256(2) 40(1)O(24) 275(4) 3451(3) 5069(3) 38(1)O(25) -347(4) 3671(4) 3562(3) 44(1)O(15) -391(3) 2483(3) 8338(3) 25(1)O(23) 1470(3) 4102(3) 3608(3) 30(1)O(14) 1339(3) 336(3) 9080(3) 26(1)O(13) 1416(3) 1707(3) 6821(3) 26(1)O(2) 4956(3) 2486(3) 5124(3) 24(1)O(11) 4052(3) 3688(3) 3460(3) 28(1)O(10) 5163(3) 4428(3) 1272(3) 30(1)O(9) 3032(3) 5840(3) 1969(3) 26(1)O(8) 1312(3) 7983(3) 1400(3) 27(1)O(18) -1972(4) 7220(3) 5030(3) 43(1)O(17) -1486(4) 4417(3) 6685(3) 37(1)O(16) -2526(4) 4266(4) 9024(3) 42(1)O(12) 4697(3) 949(3) 5186(3) 31(1)O(1W) -1477(3) 2048(3) 6846(3) 32(1)O(2W) 4279(3) 5863(3) 3669(3) 32(1)
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F(1) 1592(4) 2118(3) 3308(3) 55(1)F(2) 633(4) 1550(3) 4671(3) 58(1)F(3) 2251(3) 1987(3) 4577(3) 50(1)S(2) 576(1) 3505(1) 4086(1) 25(1)Ca(1) 2784(1) 5082(1) 3593(1) 21(1)Ca(2) -94(1) 3016(1) 6714(1) 23(1)C(58) -840(6) 1053(5) 3000(5) 40(1)O(29) -1566(4) -578(3) 3209(4) 48(1)O(31) -2963(4) 917(3) 3093(3) 38(1)O(30) -1671(4) 768(5) 1706(3) 62(2)F(7) -931(4) 872(4) 3922(3) 71(1)F(8) -1016(4) 2053(3) 2603(4) 74(1)F(9) 210(3) 718(3) 2683(3) 51(1)S(3) -1876(1) 486(1) 2702(1) 28(1)C(57) 3830(5) 7147(4) 7355(4) 34(1)O(28) 5887(4) 7471(3) 7204(3) 37(1)O(26) 4320(4) 8671(3) 7646(3) 41(1)O(27) 4822(4) 7016(3) 8768(3) 40(1)F(10) 4210(4) 6177(3) 7426(4) 67(1)F(11) 3709(4) 7660(3) 6452(3) 50(1)F(12) 2812(3) 7218(3) 7851(3) 50(1)S(4) 4837(1) 7637(1) 7785(1) 26(1)C(6S) 5070(5) 7951(5) 4514(4) 34(1)C(7S) 5372(7) 8844(5) 4615(6) 49(2)N(3S) 4835(5) 7253(4) 4451(4) 42(1)C(8S) 6215(5) 6151(5) 1283(5) 39(1)C(9S) 6805(7) 5946(7) 424(6) 63(2)N(4S) 5768(4) 6312(4) 1943(4) 42(1)C(4S) 5909(6) 3121(6) 8394(5) 50(2)C(5S) 5028(7) 3870(6) 8687(6) 67(2)N(2S) 6596(5) 2548(5) 8148(4) 49(1)C(1S) -1963(5) -101(5) 6003(4) 33(1)C(2S) -2574(5) -586(5) 5583(5) 35(1)N(1S) -1515(5) 308(4) 6315(4) 48(1)________________________________________________________________________________
________________________________________________________________________________________ Table 2. Bond lengths [Å] and angles [°] for Sample A.________________________________________________________________________________________ C(13)-H(13) 0.9800C(13)-C(12) 1.526(7)C(13)-C(39) 1.533(7)C(13)-N(4) 1.463(6)C(7)-H(7) 0.9800C(7)-C(6) 1.513(7)C(7)-C(32) 1.529(8)C(7)-O(2) 1.446(6)C(55)-F(1) 1.333(7)C(55)-F(2) 1.317(7)C(55)-F(3) 1.318(7)C(55)-S(2) 1.827(6)C(11)-H(11) 0.9800C(11)-C(38) 1.517(7)C(11)-C(10) 1.522(8)C(11)-O(3) 1.438(6)C(14)-C(15) 1.531(7)C(14)-N(4) 1.337(7)C(14)-O(15) 1.222(6)
C(38)-H(38A) 0.9600C(38)-H(38B) 0.9600C(38)-H(38C) 0.9600C(12)-O(3) 1.350(6)C(12)-O(14) 1.198(6)C(9)-H(9) 0.9800C(9)-C(8) 1.525(7)C(9)-C(35) 1.566(8)C(9)-N(3) 1.443(7)C(8)-O(2) 1.331(6)C(8)-O(12) 1.205(6)C(10)-N(3) 1.322(7)C(10)-O(13) 1.240(6)C(6)-N(2) 1.324(6)C(6)-O(11) 1.228(6)C(5)-H(5) 0.9800C(5)-C(4) 1.524(8)C(5)-C(29) 1.533(8)C(5)-N(2) 1.463(7)
C(4)-O(1) 1.338(6)C(4)-O(10) 1.199(6)C(3)-H(3) 0.9800C(3)-C(2) 1.535(7)C(3)-C(28) 1.502(8)C(3)-O(1) 1.433(7)C(2)-N(1) 1.330(7)C(2)-O(9) 1.227(7)C(1)-H(1) 0.9800C(1)-C(24) 1.521(7)C(1)-C(25) 1.553(8)C(1)-N(1) 1.476(7)C(24)-O(7) 1.346(6)C(24)-O(8) 1.199(6)C(23)-H(23) 0.9800C(23)-C(22) 1.539(8)C(23)-C(52) 1.532(7)C(23)-O(7) 1.445(6)C(22)-N(6) 1.303(7)
S13
C(22)-O(19) 1.232(6)C(21)-H(21) 0.9800C(21)-C(20) 1.514(7)C(21)-C(49) 1.527(8)C(21)-N(6) 1.464(7)C(20)-O(6) 1.353(7)C(20)-O(18) 1.189(7)C(19)-H(19) 0.9800C(19)-C(18) 1.523(8)C(19)-C(48) 1.495(8)C(19)-O(6) 1.455(6)C(18)-N(5) 1.320(7)C(18)-O(17) 1.232(6)N(5)-H(5A) 0.8600N(5)-C(17) 1.444(7)C(17)-H(17) 0.9800C(17)-C(16) 1.540(8)C(17)-C(45) 1.540(8)C(16)-O(4) 1.340(6)C(16)-O(16) 1.189(7)C(15)-H(15) 0.9800C(15)-C(42) 1.518(8)C(15)-O(4) 1.449(7)C(42)-H(42) 0.9800C(42)-C(43) 1.531(8)C(42)-C(44) 1.513(9)C(43)-H(43A) 0.9600C(43)-H(43B) 0.9600C(43)-H(43C) 0.9600C(44)-H(44A) 0.9600C(44)-H(44B) 0.9600C(44)-H(44C) 0.9600C(45)-H(45) 0.9800C(45)-C(47) 1.532(10)C(45)-C(46) 1.512(9)C(47)-H(47A) 0.9600C(47)-H(47B) 0.9600C(47)-H(47C) 0.9600C(46)-H(46A) 0.9600C(46)-H(46B) 0.9600C(46)-H(46C) 0.9600C(48)-H(48A) 0.9600C(48)-H(48B) 0.9600C(48)-H(48C) 0.9600C(49)-H(49) 0.9800C(49)-C(50) 1.532(9)C(49)-C(51) 1.525(8)C(50)-H(50A) 0.9600C(50)-H(50B) 0.9600C(50)-H(50C) 0.9600C(51)-H(51A) 0.9600C(51)-H(51B) 0.9600C(51)-H(51C) 0.9600C(52)-H(52) 0.9800C(52)-C(54) 1.537(9)C(52)-C(53) 1.526(8)C(54)-H(54A) 0.9600C(54)-H(54B) 0.9600C(54)-H(54C) 0.9600
C(53)-H(53A) 0.9600C(53)-H(53B) 0.9600C(53)-H(53C) 0.9600C(25)-H(25) 0.9800C(25)-C(26) 1.534(8)C(25)-C(27) 1.534(9)C(26)-H(26A) 0.9600C(26)-H(26B) 0.9600C(26)-H(26C) 0.9600C(27)-H(27A) 0.9600C(27)-H(27B) 0.9600C(27)-H(27C) 0.9600C(28)-H(28A) 0.9600C(28)-H(28B) 0.9600C(28)-H(28C) 0.9600C(29)-H(29) 0.9800C(29)-C(30) 1.485(10)C(29)-C(31) 1.503(11)C(30)-H(30A) 0.9600C(30)-H(30B) 0.9600C(30)-H(30C) 0.9600C(31)-H(31A) 0.9600C(31)-H(31B) 0.9600C(31)-H(31C) 0.9600C(32)-H(32) 0.9800C(32)-C(33) 1.516(8)C(32)-C(34) 1.525(7)C(33)-H(33A) 0.9600C(33)-H(33B) 0.9600C(33)-H(33C) 0.9600C(34)-H(34A) 0.9600C(34)-H(34B) 0.9600C(34)-H(34C) 0.9600C(35)-H(35) 0.9800C(35)-C(36) 1.523(9)C(35)-C(37) 1.520(8)C(36)-H(36A) 0.9600C(36)-H(36B) 0.9600C(36)-H(36C) 0.9600C(37)-H(37A) 0.9600C(37)-H(37B) 0.9600C(37)-H(37C) 0.9600C(39)-H(39) 0.9800C(39)-C(41) 1.535(8)C(39)-C(40) 1.537(8)C(41)-H(41A) 0.9600C(41)-H(41B) 0.9600C(41)-H(41C) 0.9600C(40)-H(40A) 0.9600C(40)-H(40B) 0.9600C(40)-H(40C) 0.9600O(22A)-S(1A) 1.430(5)S(1A)-C(56A) 1.828(7)S(1A)-O(21) 1.463(3)S(1A)-O(20) 1.464(3)C(56A)-F(4A) 1.329(4)C(56A)-F(5A) 1.328(4)C(56A)-F(6A) 1.330(4)O(22B)-S(1B) 1.433(6)
S(1B)-C(56B) 1.829(8)S(1B)-O(21) 1.486(3)S(1B)-O(20) 1.484(3)C(56B)-F(4B) 1.328(4)C(56B)-F(5B) 1.328(4)C(56B)-F(6B) 1.328(4)N(4)-H(4) 0.8803N(3)-H(3A) 0.8600N(2)-H(2) 0.8799N(1)-H(1A) 0.8803N(6)-H(6) 0.8600O(19)-Ca(1) 2.245(4)O(21)-Ca(2) 2.392(4)O(20)-Ca(1) 2.344(3)O(24)-S(2) 1.439(4)O(24)-Ca(2) 2.324(4)O(25)-S(2) 1.414(4)O(15)-Ca(2) 2.285(4)O(23)-S(2) 1.448(4)O(23)-Ca(1) 2.320(4)O(13)-Ca(2) 2.287(3)O(11)-Ca(1) 2.270(4)O(9)-Ca(1) 2.304(4)O(17)-Ca(2) 2.303(4)O(1W)-H(1WA) 0.97(3)O(1W)-Ca(2) 2.327(4)O(1W)-H(1WB) 0.97(3)O(2W)-Ca(1) 2.353(4)O(2W)-H(2WA) 0.93(2)O(2W)-H(2WB) 0.95(3)C(58)-F(7) 1.312(8)C(58)-F(8) 1.326(8)C(58)-F(9) 1.315(7)C(58)-S(3) 1.820(7)O(29)-S(3) 1.442(5)O(31)-S(3) 1.434(4)O(30)-S(3) 1.405(5)C(57)-F(10) 1.330(7)C(57)-F(11) 1.323(7)C(57)-F(12) 1.319(7)C(57)-S(4) 1.830(6)O(28)-S(4) 1.424(4)O(26)-S(4) 1.427(4)O(27)-S(4) 1.442(4)C(6S)-C(7S) 1.457(9)C(6S)-N(3S) 1.128(8)C(7S)-H(7SA) 0.9600C(7S)-H(7SB) 0.9600C(7S)-H(7SC) 0.9600C(8S)-C(9S) 1.449(9)C(8S)-N(4S) 1.114(8)C(9S)-H(9SA) 0.9600C(9S)-H(9SB) 0.9600C(9S)-H(9SC) 0.9600C(4S)-C(5S) 1.455(10)C(4S)-N(2S) 1.136(9)C(5S)-H(5SA) 0.9600C(5S)-H(5SB) 0.9600C(5S)-H(5SC) 0.9600
S14
C(1S)-C(2S) 1.456(9)C(1S)-N(1S) 1.126(8)C(2S)-H(2SA) 0.9600C(2S)-H(2SB) 0.9600C(2S)-H(2SC) 0.9600
C(12)-C(13)-H(13) 108.3C(12)-C(13)-C(39) 112.9(4)C(39)-C(13)-H(13) 108.3N(4)-C(13)-H(13) 108.3N(4)-C(13)-C(12) 109.2(4)N(4)-C(13)-C(39) 109.7(4)C(6)-C(7)-H(7) 110.3C(6)-C(7)-C(32) 111.9(4)C(32)-C(7)-H(7) 110.3O(2)-C(7)-H(7) 110.3O(2)-C(7)-C(6) 107.3(4)O(2)-C(7)-C(32) 106.5(4)F(1)-C(55)-S(2) 110.0(4)F(2)-C(55)-F(1) 108.2(5)F(2)-C(55)-F(3) 108.6(5)F(2)-C(55)-S(2) 110.7(4)F(3)-C(55)-F(1) 107.6(5)F(3)-C(55)-S(2) 111.5(4)C(38)-C(11)-H(11) 110.4C(38)-C(11)-C(10) 110.7(4)C(10)-C(11)-H(11) 110.4O(3)-C(11)-H(11) 110.4O(3)-C(11)-C(38) 105.8(4)O(3)-C(11)-C(10) 109.1(4)N(4)-C(14)-C(15) 116.4(5)O(15)-C(14)-C(15) 121.6(5)O(15)-C(14)-N(4) 122.0(5)C(11)-C(38)-H(38A) 109.5C(11)-C(38)-H(38B) 109.5C(11)-C(38)-H(38C) 109.5H(38A)-C(38)-H(38B) 109.5H(38A)-C(38)-H(38C) 109.5H(38B)-C(38)-H(38C) 109.5O(3)-C(12)-C(13) 109.5(4)O(14)-C(12)-C(13) 126.2(5)O(14)-C(12)-O(3) 124.2(5)C(8)-C(9)-H(9) 107.7C(8)-C(9)-C(35) 110.6(4)C(35)-C(9)-H(9) 107.7N(3)-C(9)-H(9) 107.7N(3)-C(9)-C(8) 110.7(4)N(3)-C(9)-C(35) 112.1(5)O(2)-C(8)-C(9) 109.8(4)O(12)-C(8)-C(9) 125.9(5)O(12)-C(8)-O(2) 124.3(5)N(3)-C(10)-C(11) 116.5(4)O(13)-C(10)-C(11) 120.5(4)O(13)-C(10)-N(3) 123.0(5)N(2)-C(6)-C(7) 117.8(4)O(11)-C(6)-C(7) 120.7(4)O(11)-C(6)-N(2) 121.5(5)C(4)-C(5)-H(5) 108.1C(4)-C(5)-C(29) 111.3(5)
C(29)-C(5)-H(5) 108.1N(2)-C(5)-H(5) 108.1N(2)-C(5)-C(4) 110.3(4)N(2)-C(5)-C(29) 110.9(5)O(1)-C(4)-C(5) 109.3(4)O(10)-C(4)-C(5) 126.2(5)O(10)-C(4)-O(1) 124.4(5)C(2)-C(3)-H(3) 109.9C(28)-C(3)-H(3) 109.9C(28)-C(3)-C(2) 110.0(5)O(1)-C(3)-H(3) 109.9O(1)-C(3)-C(2) 109.7(4)O(1)-C(3)-C(28) 107.4(5)N(1)-C(2)-C(3) 115.3(5)O(9)-C(2)-C(3) 121.7(5)O(9)-C(2)-N(1) 122.9(5)C(24)-C(1)-H(1) 109.1C(24)-C(1)-C(25) 111.0(4)C(25)-C(1)-H(1) 109.1N(1)-C(1)-H(1) 109.1N(1)-C(1)-C(24) 109.5(4)N(1)-C(1)-C(25) 109.2(4)O(7)-C(24)-C(1) 108.8(4)O(8)-C(24)-C(1) 126.9(5)O(8)-C(24)-O(7) 124.3(5)C(22)-C(23)-H(23) 110.8C(52)-C(23)-H(23) 110.8C(52)-C(23)-C(22) 110.7(4)O(7)-C(23)-H(23) 110.8O(7)-C(23)-C(22) 107.7(4)O(7)-C(23)-C(52) 105.8(4)N(6)-C(22)-C(23) 117.3(4)O(19)-C(22)-C(23) 118.9(5)O(19)-C(22)-N(6) 123.7(5)C(20)-C(21)-H(21) 107.3C(20)-C(21)-C(49) 113.8(5)C(49)-C(21)-H(21) 107.3N(6)-C(21)-H(21) 107.3N(6)-C(21)-C(20) 108.6(4)N(6)-C(21)-C(49) 112.2(4)O(6)-C(20)-C(21) 109.6(4)O(18)-C(20)-C(21) 125.9(5)O(18)-C(20)-O(6) 124.5(5)C(18)-C(19)-H(19) 110.3C(48)-C(19)-H(19) 110.3C(48)-C(19)-C(18) 113.0(5)O(6)-C(19)-H(19) 110.3O(6)-C(19)-C(18) 105.9(4)O(6)-C(19)-C(48) 106.8(4)N(5)-C(18)-C(19) 116.9(4)O(17)-C(18)-C(19) 120.3(5)O(17)-C(18)-N(5) 122.9(5)C(18)-N(5)-H(5A) 119.7C(18)-N(5)-C(17) 120.6(4)C(17)-N(5)-H(5A) 119.7N(5)-C(17)-H(17) 107.7N(5)-C(17)-C(16) 109.2(5)N(5)-C(17)-C(45) 109.3(4)C(16)-C(17)-H(17) 107.7
C(16)-C(17)-C(45) 115.0(5)C(45)-C(17)-H(17) 107.7O(4)-C(16)-C(17) 110.6(5)O(16)-C(16)-C(17) 124.9(5)O(16)-C(16)-O(4) 124.5(5)C(14)-C(15)-H(15) 110.0C(42)-C(15)-C(14) 112.5(4)C(42)-C(15)-H(15) 110.0O(4)-C(15)-C(14) 106.4(4)O(4)-C(15)-H(15) 110.0O(4)-C(15)-C(42) 107.8(4)C(15)-C(42)-H(42) 107.6C(15)-C(42)-C(43) 110.5(5)C(43)-C(42)-H(42) 107.6C(44)-C(42)-C(15) 112.2(5)C(44)-C(42)-H(42) 107.6C(44)-C(42)-C(43) 111.0(5)C(42)-C(43)-H(43A) 109.5C(42)-C(43)-H(43B) 109.5C(42)-C(43)-H(43C) 109.5H(43A)-C(43)-H(43B) 109.5H(43A)-C(43)-H(43C) 109.5H(43B)-C(43)-H(43C) 109.5C(42)-C(44)-H(44A) 109.5C(42)-C(44)-H(44B) 109.5C(42)-C(44)-H(44C) 109.5H(44A)-C(44)-H(44B) 109.5H(44A)-C(44)-H(44C) 109.5H(44B)-C(44)-H(44C) 109.5C(17)-C(45)-H(45) 108.1C(47)-C(45)-C(17) 110.2(5)C(47)-C(45)-H(45) 108.1C(46)-C(45)-C(17) 112.6(5)C(46)-C(45)-H(45) 108.1C(46)-C(45)-C(47) 109.5(6)C(45)-C(47)-H(47A) 109.5C(45)-C(47)-H(47B) 109.5C(45)-C(47)-H(47C) 109.5H(47A)-C(47)-H(47B) 109.5H(47A)-C(47)-H(47C) 109.5H(47B)-C(47)-H(47C) 109.5C(45)-C(46)-H(46A) 109.5C(45)-C(46)-H(46B) 109.5C(45)-C(46)-H(46C) 109.5H(46A)-C(46)-H(46B) 109.5H(46A)-C(46)-H(46C) 109.5H(46B)-C(46)-H(46C) 109.5C(19)-C(48)-H(48A) 109.5C(19)-C(48)-H(48B) 109.5C(19)-C(48)-H(48C) 109.5H(48A)-C(48)-H(48B) 109.5H(48A)-C(48)-H(48C) 109.5H(48B)-C(48)-H(48C) 109.5C(21)-C(49)-H(49) 107.5C(21)-C(49)-C(50) 111.4(5)C(50)-C(49)-H(49) 107.5C(51)-C(49)-C(21) 111.2(5)C(51)-C(49)-H(49) 107.5C(51)-C(49)-C(50) 111.5(5)
S15
C(49)-C(50)-H(50A) 109.5C(49)-C(50)-H(50B) 109.5C(49)-C(50)-H(50C) 109.5H(50A)-C(50)-H(50B) 109.5H(50A)-C(50)-H(50C) 109.5H(50B)-C(50)-H(50C) 109.5C(49)-C(51)-H(51A) 109.5C(49)-C(51)-H(51B) 109.5C(49)-C(51)-H(51C) 109.5H(51A)-C(51)-H(51B) 109.5H(51A)-C(51)-H(51C) 109.5H(51B)-C(51)-H(51C) 109.5C(23)-C(52)-H(52) 108.0C(23)-C(52)-C(54) 110.4(5)C(54)-C(52)-H(52) 108.0C(53)-C(52)-C(23) 111.2(5)C(53)-C(52)-H(52) 108.0C(53)-C(52)-C(54) 111.0(5)C(52)-C(54)-H(54A) 109.5C(52)-C(54)-H(54B) 109.5C(52)-C(54)-H(54C) 109.5H(54A)-C(54)-H(54B) 109.5H(54A)-C(54)-H(54C) 109.5H(54B)-C(54)-H(54C) 109.5C(52)-C(53)-H(53A) 109.5C(52)-C(53)-H(53B) 109.5C(52)-C(53)-H(53C) 109.5H(53A)-C(53)-H(53B) 109.5H(53A)-C(53)-H(53C) 109.5H(53B)-C(53)-H(53C) 109.5C(1)-C(25)-H(25) 109.0C(26)-C(25)-C(1) 110.2(5)C(26)-C(25)-H(25) 109.0C(26)-C(25)-C(27) 110.5(5)C(27)-C(25)-C(1) 109.1(5)C(27)-C(25)-H(25) 109.0C(25)-C(26)-H(26A) 109.5C(25)-C(26)-H(26B) 109.5C(25)-C(26)-H(26C) 109.5H(26A)-C(26)-H(26B) 109.5H(26A)-C(26)-H(26C) 109.5H(26B)-C(26)-H(26C) 109.5C(25)-C(27)-H(27A) 109.5C(25)-C(27)-H(27B) 109.5C(25)-C(27)-H(27C) 109.5H(27A)-C(27)-H(27B) 109.5H(27A)-C(27)-H(27C) 109.5H(27B)-C(27)-H(27C) 109.5C(3)-C(28)-H(28A) 109.5C(3)-C(28)-H(28B) 109.5C(3)-C(28)-H(28C) 109.5H(28A)-C(28)-H(28B) 109.5H(28A)-C(28)-H(28C) 109.5H(28B)-C(28)-H(28C) 109.5C(5)-C(29)-H(29) 106.6C(30)-C(29)-C(5) 112.9(6)C(30)-C(29)-H(29) 106.6C(30)-C(29)-C(31) 112.5(7)C(31)-C(29)-C(5) 111.0(6)
C(31)-C(29)-H(29) 106.6C(29)-C(30)-H(30A) 109.5C(29)-C(30)-H(30B) 109.5C(29)-C(30)-H(30C) 109.5H(30A)-C(30)-H(30B) 109.5H(30A)-C(30)-H(30C) 109.5H(30B)-C(30)-H(30C) 109.5C(29)-C(31)-H(31A) 109.5C(29)-C(31)-H(31B) 109.5C(29)-C(31)-H(31C) 109.5H(31A)-C(31)-H(31B) 109.5H(31A)-C(31)-H(31C) 109.5H(31B)-C(31)-H(31C) 109.5C(7)-C(32)-H(32) 107.8C(33)-C(32)-C(7) 111.8(4)C(33)-C(32)-H(32) 107.8C(33)-C(32)-C(34) 111.9(4)C(34)-C(32)-C(7) 109.5(5)C(34)-C(32)-H(32) 107.8C(32)-C(33)-H(33A) 109.5C(32)-C(33)-H(33B) 109.5C(32)-C(33)-H(33C) 109.5H(33A)-C(33)-H(33B) 109.5H(33A)-C(33)-H(33C) 109.5H(33B)-C(33)-H(33C) 109.5C(32)-C(34)-H(34A) 109.5C(32)-C(34)-H(34B) 109.5C(32)-C(34)-H(34C) 109.5H(34A)-C(34)-H(34B) 109.5H(34A)-C(34)-H(34C) 109.5H(34B)-C(34)-H(34C) 109.5C(9)-C(35)-H(35) 108.2C(36)-C(35)-C(9) 111.3(5)C(36)-C(35)-H(35) 108.2C(37)-C(35)-C(9) 108.7(5)C(37)-C(35)-H(35) 108.2C(37)-C(35)-C(36) 112.2(5)C(35)-C(36)-H(36A) 109.5C(35)-C(36)-H(36B) 109.5C(35)-C(36)-H(36C) 109.5H(36A)-C(36)-H(36B) 109.5H(36A)-C(36)-H(36C) 109.5H(36B)-C(36)-H(36C) 109.5C(35)-C(37)-H(37A) 109.5C(35)-C(37)-H(37B) 109.5C(35)-C(37)-H(37C) 109.5H(37A)-C(37)-H(37B) 109.5H(37A)-C(37)-H(37C) 109.5H(37B)-C(37)-H(37C) 109.5C(13)-C(39)-H(39) 108.4C(13)-C(39)-C(41) 109.2(5)C(13)-C(39)-C(40) 112.5(4)C(41)-C(39)-H(39) 108.4C(41)-C(39)-C(40) 109.8(5)C(40)-C(39)-H(39) 108.4C(39)-C(41)-H(41A) 109.5C(39)-C(41)-H(41B) 109.5C(39)-C(41)-H(41C) 109.5H(41A)-C(41)-H(41B) 109.5
H(41A)-C(41)-H(41C) 109.5H(41B)-C(41)-H(41C) 109.5C(39)-C(40)-H(40A) 109.5C(39)-C(40)-H(40B) 109.5C(39)-C(40)-H(40C) 109.5H(40A)-C(40)-H(40B) 109.5H(40A)-C(40)-H(40C) 109.5H(40B)-C(40)-H(40C) 109.5O(22A)-S(1A)-C(56A) 105.4(3)O(22A)-S(1A)-O(21) 120.1(3)O(22A)-S(1A)-O(20) 120.9(3)O(21)-S(1A)-C(56A) 98.2(2)O(21)-S(1A)-O(20) 109.2(2)O(20)-S(1A)-C(56A) 97.2(2)F(4A)-C(56A)-S(1A) 111.0(4)F(4A)-C(56A)-F(6A) 108.0(6)F(5A)-C(56A)-S(1A) 111.7(4)F(5A)-C(56A)-F(4A) 107.9(5)F(5A)-C(56A)-F(6A) 106.9(5)F(6A)-C(56A)-S(1A) 111.2(4)O(22B)-S(1B)-C(56B) 104.7(4)O(22B)-S(1B)-O(21) 119.8(8)O(22B)-S(1B)-O(20) 120.9(8)O(21)-S(1B)-C(56B) 98.8(4)O(20)-S(1B)-C(56B) 101.4(4)O(20)-S(1B)-O(21) 107.0(3)F(4B)-C(56B)-S(1B) 111.0(5)F(4B)-C(56B)-F(5B) 107.9(6)F(4B)-C(56B)-F(6B) 108.2(6)F(5B)-C(56B)-S(1B) 111.4(5)F(6B)-C(56B)-S(1B) 110.9(5)F(6B)-C(56B)-F(5B) 107.1(6)C(13)-N(4)-H(4) 119.7C(14)-N(4)-C(13) 120.4(4)C(14)-N(4)-H(4) 119.8C(9)-N(3)-H(3A) 118.9C(10)-N(3)-C(9) 122.2(4)C(10)-N(3)-H(3A) 118.9C(6)-N(2)-C(5) 119.6(4)C(6)-N(2)-H(2) 120.3C(5)-N(2)-H(2) 120.0C(2)-N(1)-C(1) 120.8(4)C(2)-N(1)-H(1A) 119.1C(1)-N(1)-H(1A) 120.0C(22)-N(6)-C(21) 122.5(4)C(22)-N(6)-H(6) 118.7C(21)-N(6)-H(6) 118.7C(20)-O(6)-C(19) 115.5(4)C(16)-O(4)-C(15) 117.9(4)C(22)-O(19)-Ca(1) 163.7(4)C(24)-O(7)-C(23) 117.6(4)C(12)-O(3)-C(11) 115.8(4)C(4)-O(1)-C(3) 116.4(4)S(1A)-O(21)-Ca(2) 123.6(2)S(1B)-O(21)-Ca(2) 153.4(3)S(1A)-O(20)-Ca(1) 137.6(2)S(1B)-O(20)-Ca(1) 172.8(3)S(2)-O(24)-Ca(2) 168.5(3)C(14)-O(15)-Ca(2) 175.4(4)
S16
S(2)-O(23)-Ca(1) 151.9(2)C(10)-O(13)-Ca(2) 166.2(4)C(8)-O(2)-C(7) 118.7(4)C(6)-O(11)-Ca(1) 168.5(4)C(2)-O(9)-Ca(1) 171.3(4)C(18)-O(17)-Ca(2) 175.9(4)H(1WA)-O(1W)-H(1WB) 112(5)Ca(2)-O(1W)-H(1WA) 126(4)Ca(2)-O(1W)-H(1WB) 120(4)Ca(1)-O(2W)-H(2WA) 110(3)Ca(1)-O(2W)-H(2WB) 127(4)H(2WA)-O(2W)-H(2WB) 116(5)O(24)-S(2)-C(55) 102.3(3)O(24)-S(2)-O(23) 113.1(3)O(25)-S(2)-C(55) 105.0(3)O(25)-S(2)-O(24) 116.1(3)O(25)-S(2)-O(23) 115.4(3)O(23)-S(2)-C(55) 102.5(3)O(19)-Ca(1)-O(20) 88.14(15)O(19)-Ca(1)-O(23) 87.50(15)O(19)-Ca(1)-O(11) 167.88(16)O(19)-Ca(1)-O(9) 83.90(15)O(19)-Ca(1)-O(2W) 99.81(16)O(20)-Ca(1)-O(2W) 87.00(15)O(23)-Ca(1)-O(20) 90.33(15)O(23)-Ca(1)-O(2W) 172.12(15)O(11)-Ca(1)-O(20) 98.42(14)O(11)-Ca(1)-O(23) 82.31(14)O(11)-Ca(1)-O(9) 90.71(14)O(11)-Ca(1)-O(2W) 90.74(14)O(9)-Ca(1)-O(20) 169.29(14)O(9)-Ca(1)-O(23) 96.46(14)O(9)-Ca(1)-O(2W) 87.30(14)O(24)-Ca(2)-O(21) 90.01(15)
O(24)-Ca(2)-O(1W) 94.80(16)O(15)-Ca(2)-O(21) 90.91(13)O(15)-Ca(2)-O(24) 176.19(15)O(15)-Ca(2)-O(13) 87.82(13)O(15)-Ca(2)-O(17) 89.56(14)O(15)-Ca(2)-O(1W) 84.15(14)O(13)-Ca(2)-O(21) 82.74(14)O(13)-Ca(2)-O(24) 88.63(14)O(13)-Ca(2)-O(17) 173.15(16)O(13)-Ca(2)-O(1W) 95.33(14)O(17)-Ca(2)-O(21) 90.98(15)O(17)-Ca(2)-O(24) 94.12(15)O(17)-Ca(2)-O(1W) 90.69(16)O(1W)-Ca(2)-O(21) 174.78(14)F(7)-C(58)-F(8) 106.9(5)F(7)-C(58)-F(9) 110.1(6)F(7)-C(58)-S(3) 110.7(5)F(8)-C(58)-S(3) 111.0(5)F(9)-C(58)-F(8) 106.7(6)F(9)-C(58)-S(3) 111.2(4)O(29)-S(3)-C(58) 102.6(3)O(31)-S(3)-C(58) 104.5(3)O(31)-S(3)-O(29) 112.0(3)O(30)-S(3)-C(58) 102.9(3)O(30)-S(3)-O(29) 116.2(3)O(30)-S(3)-O(31) 116.3(3)F(10)-C(57)-S(4) 110.1(4)F(11)-C(57)-F(10) 108.1(5)F(11)-C(57)-S(4) 110.9(4)F(12)-C(57)-F(10) 108.4(5)F(12)-C(57)-F(11) 107.9(5)F(12)-C(57)-S(4) 111.2(4)O(28)-S(4)-C(57) 103.9(3)O(28)-S(4)-O(26) 116.0(3)
O(28)-S(4)-O(27) 114.8(3)O(26)-S(4)-C(57) 102.9(3)O(26)-S(4)-O(27) 114.1(3)O(27)-S(4)-C(57) 102.6(3)N(3S)-C(6S)-C(7S) 178.9(7)C(6S)-C(7S)-H(7SA) 109.5C(6S)-C(7S)-H(7SB) 109.5C(6S)-C(7S)-H(7SC) 109.5H(7SA)-C(7S)-H(7SB) 109.5H(7SA)-C(7S)-H(7SC) 109.5H(7SB)-C(7S)-H(7SC) 109.5N(4S)-C(8S)-C(9S) 179.5(7)C(8S)-C(9S)-H(9SA) 109.5C(8S)-C(9S)-H(9SB) 109.5C(8S)-C(9S)-H(9SC) 109.5H(9SA)-C(9S)-H(9SB) 109.5H(9SA)-C(9S)-H(9SC) 109.5H(9SB)-C(9S)-H(9SC) 109.5N(2S)-C(4S)-C(5S) 178.6(8)C(4S)-C(5S)-H(5SA) 109.5C(4S)-C(5S)-H(5SB) 109.5C(4S)-C(5S)-H(5SC) 109.5H(5SA)-C(5S)-H(5SB) 109.5H(5SA)-C(5S)-H(5SC) 109.5H(5SB)-C(5S)-H(5SC) 109.5N(1S)-C(1S)-C(2S) 177.5(7)C(1S)-C(2S)-H(2SA) 109.5C(1S)-C(2S)-H(2SB) 109.5C(1S)-C(2S)-H(2SC) 109.5H(2SA)-C(2S)-H(2SB) 109.5H(2SA)-C(2S)-H(2SC) 109.5H(2SB)-C(2S)-H(2SC) 109.5
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Table 3. Anisotropic displacement parameters (Å2x 103) for SAMPLE A. The anisotropicdisplacement factor exponent takes the form: -22[ h2 a*2U11 + ... + 2 h k a* b* U12 ]___________________________________________________________________________________________________________________________________________________________________________________________________
U11 U22 U33 U23 U13 U12___________________________________________________________________________________________________________________________________________________________________________________________________
C(13) 24(3) 17(3) 22(2) -3(2) -4(2) -7(2)C(7) 26(3) 16(3) 21(3) -8(2) -1(2) 0(2)C(55) 44(3) 27(3) 41(3) -12(3) -6(3) -10(3)C(11) 19(2) 20(3) 30(3) -7(2) -4(2) 1(2)C(14) 17(2) 14(2) 26(3) -5(2) -1(2) -2(2)C(38) 27(3) 23(3) 37(3) -15(2) -1(2) -4(2)C(12) 28(3) 14(2) 23(3) -2(2) -2(2) -4(2)C(9) 21(2) 20(3) 31(3) -11(2) -1(2) -4(2)C(8) 19(2) 20(3) 24(3) -5(2) -3(2) -3(2)C(10) 22(3) 14(2) 23(3) -6(2) -2(2) 0(2)C(6) 14(2) 15(2) 29(3) -8(2) 4(2) -6(2)C(5) 28(2) 19(2) 32(2) -4(2) -12(2) -5(2)C(4) 24(3) 26(2) 25(2) -11(2) -3(2) -4(2)C(3) 33(3) 21(3) 30(3) -6(2) -5(2) -10(2)C(2) 15(2) 23(3) 32(3) -10(2) -7(2) 0(2)
S17
C(1) 27(2) 21(3) 29(3) -7(2) -4(2) -7(2)C(24) 28(2) 9(2) 27(2) -1(2) -5(2) -4(2)C(23) 23(2) 12(2) 27(3) -3(2) -4(2) 1(2)C(22) 31(3) 16(3) 21(3) -4(2) 0(2) 0(2)C(21) 31(3) 13(3) 28(3) -6(2) 0(2) -3(2)C(20) 31(3) 14(3) 31(3) -5(2) -3(2) 0(2)C(19) 26(3) 19(3) 23(3) -5(2) -1(2) 4(2)C(18) 27(3) 14(3) 29(3) -5(2) 3(2) -2(2)N(5) 30(2) 16(2) 38(3) -8(2) -12(2) 3(2)C(17) 32(3) 22(3) 35(3) -11(2) -10(2) 4(2)C(16) 27(3) 29(3) 28(3) -19(2) -6(2) 1(2)C(15) 29(3) 18(3) 26(3) -7(2) 2(2) -6(2)C(42) 51(4) 17(3) 30(3) -3(2) -13(3) -6(3)C(43) 73(5) 28(3) 39(3) -8(3) -19(3) -17(3)C(44) 41(3) 34(4) 53(4) -12(3) -13(3) -5(3)C(45) 38(3) 29(3) 45(4) -14(3) -7(3) -2(3)C(47) 63(5) 30(4) 68(5) -3(3) -23(4) -11(3)C(46) 46(4) 32(3) 48(4) -15(3) -10(3) -4(3)C(48) 36(3) 26(3) 35(3) -7(3) 4(3) -9(3)C(49) 42(3) 25(3) 32(3) -9(2) -1(3) -20(3)C(50) 36(3) 42(4) 45(4) -12(3) -10(3) -10(3)C(51) 63(4) 37(4) 27(3) -11(3) 2(3) -15(3)C(52) 25(3) 31(3) 33(3) -12(2) -9(2) 5(2)C(54) 33(3) 50(4) 45(4) -23(3) -12(3) -4(3)C(53) 43(4) 47(4) 37(3) -18(3) -8(3) -1(3)C(25) 40(3) 23(3) 23(3) -1(2) -7(2) -13(2)C(26) 69(5) 27(3) 38(4) -4(3) -9(3) -21(3)C(27) 51(4) 43(4) 35(3) -5(3) -3(3) -28(3)C(28) 46(4) 24(3) 47(4) -4(3) -27(3) -6(3)C(29) 57(2) 40(2) 49(2) -23(2) -17(2) -4(2)C(30) 69(3) 52(3) 53(3) -27(3) -19(3) 11(3)C(31) 93(4) 46(3) 79(4) -28(3) -29(3) -11(3)C(32) 22(3) 23(3) 27(3) -11(2) -5(2) -2(2)C(33) 24(3) 33(3) 40(3) -3(3) -7(2) -6(2)C(34) 29(3) 37(3) 31(3) -11(3) -7(2) -5(2)C(35) 40(3) 38(4) 25(3) -11(3) 7(2) -22(3)C(36) 35(3) 51(4) 34(3) -5(3) -11(3) -16(3)C(37) 50(4) 67(5) 34(3) -27(3) 11(3) -32(4)C(39) 33(3) 18(3) 24(3) 0(2) -1(2) -11(2)C(41) 33(3) 38(4) 34(3) -4(3) -1(2) -15(3)C(40) 57(4) 23(3) 39(3) -7(3) 9(3) -17(3)O(22A) 31(3) 28(3) 38(3) -10(3) -7(2) 0(2)S(1A) 21(1) 20(1) 22(1) -7(1) -3(1) -5(1)C(56A) 37(3) 38(3) 41(3) -17(3) -10(2) -13(2)F(4A) 74(5) 49(3) 67(3) -8(3) -22(3) -36(3)F(5A) 51(4) 74(4) 55(2) -42(3) -11(2) -10(3)F(6A) 38(2) 48(3) 46(3) -16(2) -16(2) -11(2)O(22B) 38(2) 48(3) 46(3) -16(2) -16(2) -11(2)S(1B) 26(3) 20(2) 35(3) -3(2) -7(2) -5(2)C(56B) 37(3) 38(3) 41(3) -17(3) -10(2) -13(2)F(4B) 74(5) 49(3) 67(3) -8(3) -22(3) -36(3)F(5B) 51(4) 74(4) 55(2) -42(3) -11(2) -10(3)F(6B) 38(2) 48(3) 46(3) -16(2) -16(2) -11(2)N(4) 30(2) 19(2) 19(2) -6(2) 0(2) -4(2)N(3) 21(2) 12(2) 31(2) -7(2) -1(2) 1(2)N(2) 24(2) 19(2) 33(2) -9(2) -7(2) 1(2)N(1) 28(2) 21(2) 24(2) -5(2) -1(2) -10(2)N(6) 28(2) 9(2) 25(2) -2(2) 0(2) -1(2)O(6) 30(2) 17(2) 27(2) -8(2) 0(2) -5(2)
S18
O(4) 32(2) 16(2) 34(2) -5(2) -9(2) -1(2)O(19) 33(2) 18(2) 52(3) -4(2) 10(2) 1(2)O(7) 26(2) 20(2) 26(2) -6(2) -5(1) -3(2)O(3) 19(2) 21(2) 28(2) -10(2) 0(1) -3(2)O(1) 27(2) 16(2) 36(2) -6(2) -8(2) -4(2)O(21) 51(3) 26(2) 42(2) -10(2) 3(2) -17(2)O(20) 47(2) 40(3) 30(2) -11(2) 4(2) -12(2)O(24) 38(2) 36(2) 32(2) -7(2) -3(2) 2(2)O(25) 31(2) 53(3) 40(2) 1(2) -10(2) -14(2)O(15) 34(2) 18(2) 23(2) -6(2) 0(2) -8(2)O(23) 30(2) 28(2) 31(2) -7(2) -1(2) -9(2)O(14) 21(2) 26(2) 32(2) -11(2) -7(2) -2(2)O(13) 23(2) 19(2) 32(2) -6(2) -2(2) 2(2)O(2) 26(2) 20(2) 27(2) -10(2) 4(2) -6(2)O(11) 21(2) 22(2) 36(2) -8(2) -2(2) 0(2)O(10) 28(2) 30(2) 33(2) -6(2) -9(2) -7(2)O(9) 29(2) 20(2) 28(2) -4(2) -3(2) -6(2)O(8) 28(2) 22(2) 30(2) -5(2) -7(2) -4(2)O(18) 64(3) 25(2) 42(2) -18(2) 20(2) -20(2)O(17) 40(2) 26(2) 35(2) -9(2) -1(2) 10(2)O(16) 32(2) 50(3) 36(2) -7(2) -4(2) -1(2)O(12) 34(2) 27(2) 35(2) -16(2) 1(2) -9(2)O(1W) 33(2) 32(2) 35(2) -12(2) -9(2) -4(2)O(2W) 33(2) 32(2) 37(2) -14(2) -4(2) -11(2)F(1) 85(3) 39(2) 49(2) -24(2) -8(2) -8(2)F(2) 77(3) 34(2) 65(3) -1(2) -14(2) -31(2)F(3) 45(2) 36(2) 64(3) -17(2) -18(2) 11(2)S(2) 24(1) 25(1) 25(1) -5(1) -2(1) -5(1)Ca(1) 20(1) 14(1) 26(1) -5(1) 0(1) -1(1)Ca(2) 26(1) 15(1) 22(1) -4(1) -1(1) 3(1)C(58) 50(3) 23(3) 50(3) -15(2) -5(2) -8(2)O(29) 39(2) 25(2) 82(3) -22(2) -13(2) 6(2)O(31) 41(2) 31(2) 32(2) -8(2) 0(2) 6(2)O(30) 45(3) 102(4) 36(2) -22(2) -1(2) -10(3)F(7) 94(3) 89(3) 51(2) -29(2) -5(2) -47(3)F(8) 78(3) 26(2) 104(3) -17(2) 17(3) -8(2)F(9) 42(2) 41(2) 73(3) -18(2) -9(2) -7(2)S(3) 28(1) 27(1) 28(1) -12(1) -4(1) 7(1)C(57) 43(3) 24(3) 41(3) -14(2) -10(2) -7(2)O(28) 36(2) 26(2) 41(2) -8(2) 0(2) 4(2)O(26) 35(2) 23(2) 67(3) -22(2) -11(2) 3(2)O(27) 40(2) 47(3) 30(2) -10(2) -2(2) -9(2)F(10) 85(3) 28(2) 103(3) -32(2) -37(3) -1(2)F(11) 63(2) 47(2) 43(2) -16(2) -17(2) -4(2)F(12) 43(2) 50(2) 58(2) -11(2) -9(2) -15(2)S(4) 28(1) 18(1) 30(1) -9(1) -1(1) 0(1)C(6S) 28(3) 35(4) 40(3) -13(3) -5(2) -3(3)C(7S) 56(4) 34(4) 64(5) -16(4) -16(4) -14(3)N(3S) 43(3) 36(3) 58(4) -24(3) -7(3) -11(3)C(8S) 34(3) 44(4) 46(4) -15(3) -4(3) -15(3)C(9S) 50(4) 92(7) 58(5) -33(5) 6(4) -25(4)N(4S) 36(3) 48(3) 45(3) -15(3) -6(2) -11(3)C(4S) 44(4) 54(5) 41(4) -1(3) 4(3) -16(4)C(5S) 60(5) 56(5) 55(5) 2(4) 1(4) 11(4)N(2S) 49(3) 42(3) 57(4) -17(3) 5(3) -13(3)C(1S) 30(3) 26(3) 43(3) -12(3) -3(3) -3(2)C(2S) 35(3) 33(3) 42(3) -16(3) -8(3) -8(3)N(1S) 45(3) 40(3) 70(4) -27(3) -13(3) -10(3)______________________________________________________________________________
S19
________________________________________________________________________________________________________________________________________________________________________________________________________
Table 4. Hydrogen coordinates ( x 104) and isotropic displacement parameters (Å2x 10 3)for SAMPLE A.________________________________________________________________________________________________________________________________________________________________________________________________________
x y z U(eq)________________________________________________________________________________________________________________________________________________________________________________________________________ H(1WA) -1370(60) 1450(40) 6640(50) 60(20)H(13) -1242 798 8742 25H(7) 6154 1989 4196 26H(11) 2110 -618 7890 29H(38A) 1089 -1128 7003 41H(38B) 2085 -615 6314 41H(38C) 832 -11 6322 41H(9) 3172 2272 6294 28H(5) 3552 2834 2343 31H(3) 3881 5536 -16 33H(1) 3976 7595 1523 30H(23) 797 8773 2836 26H(21) -511 5908 3917 30H(19) -3471 6274 5971 30H(5A) -2755 6227 7247 34H(17) -617 5268 7543 35H(15) -1393 2966 10192 30H(42) 288 2017 10806 39H(43A) 385 4096 10378 66H(43B) 870 3220 11248 66H(43C) -455 3517 11206 66H(44A) 1512 2050 9432 64H(44B) 2084 2416 10081 64H(44C) 1524 3210 9201 64H(45) -2078 6602 8456 45H(47A) -939 7809 7498 81H(47B) -1491 7418 6856 81H(47C) -205 7015 7024 81H(46A) 246 5831 8684 62H(46B) -777 5634 9495 62H(46C) -455 6724 9043 62H(48A) -4280 5169 5521 50H(48B) -4303 4816 6628 50H(48C) -3376 4256 6022 50H(49) -2148 6020 3225 37H(50A) -3055 7661 3141 60H(50B) -2885 7551 2123 60H(50C) -2073 8116 2382 60H(51A) -329 6815 1914 63H(51B) -1260 6379 1643 63H(51C) -418 5660 2367 63H(52) 2222 7578 4286 36H(54A) 3024 8995 3279 59H(54B) 2654 9105 4295 59H(54C) 1895 9721 3474 59H(53A) 162 8917 4510 63H(53B) 972 8380 5307 63H(53C) 334 7734 4973 63H(25) 3161 8977 -200 35H(26A) 3621 9587 1284 66H(26B) 2399 9751 984 66
S20
H(26C) 3334 10343 287 66H(27A) 5306 8686 466 63H(27B) 5002 9392 -544 63H(27C) 5119 8212 -281 63H(28A) 2107 5258 -232 58H(28B) 2048 6398 -324 58H(28C) 1514 5660 614 58H(29) 4112 2446 934 54H(30A) 5884 2936 528 86H(30B) 5933 1861 439 86H(30C) 6377 1958 1313 86H(31A) 5011 846 2446 102H(31B) 4617 723 1563 102H(31C) 3714 1134 2291 102H(32) 5877 3994 4284 28H(33A) 7428 3260 2936 51H(33B) 7454 4281 3106 51H(33C) 6403 4162 2701 51H(34A) 6847 2726 5480 48H(34B) 7657 3487 4838 48H(34C) 7776 2422 4707 48H(35) 4788 2396 6876 40H(36A) 5211 254 7609 59H(36B) 5899 951 7824 59H(36C) 5992 911 6787 59H(37A) 3032 2317 7894 68H(37B) 4096 1992 8459 68H(37C) 3471 1164 8395 68H(39) -783 -597 10547 31H(41A) -2802 -47 9643 54H(41B) -2645 339 10462 54H(41C) -2694 -811 10672 54H(40A) -1083 -1178 8997 61H(40B) -1131 -1912 10047 61H(40C) 16 -1533 9523 61H(4) -1008 1133 10330 28H(3A) 3600 196 6956 27H(2) 5693 2090 2771 30H(1A) 3671 7212 -9 29H(6) -756 7988 3349 27H(7SA) 6014 9044 4158 73H(7SB) 5568 8686 5245 73H(7SC) 4732 9389 4508 73H(9SA) 6281 6148 -42 95H(9SB) 7097 5233 566 95H(9SC) 7427 6321 179 95H(5SA) 4571 4242 8179 100H(5SB) 5381 4329 8839 100H(5SC) 4551 3532 9237 100H(2SA) -2035 -959 5220 52H(2SB) -3085 -78 5173 52H(2SC) -3006 -1043 6078 52H(1WB) -2180(40) 2110(50) 7270(40) 60(20)H(2WA) 4720(40) 6040(40) 3080(20) 24(14)H(2WB) 4280(60) 6260(50) 4070(40) 60(20)______________________________________________________________________________ ______________________________________________________________________________________________________________________________________________________________________________________________________________________________
Table 5. Torsion angles [°] for SAMPLE A.______________________________________________________________________________________________________________________________________________________________________________________________________________________________
S21
C(13)-C(12)-O(3)-C(11) 179.1(4)C(7)-C(6)-N(2)-C(5) 178.9(5)C(7)-C(6)-O(11)-Ca(1) 33(2)C(11)-C(10)-N(3)-C(9) -177.9(4)C(11)-C(10)-O(13)-Ca(2) 19.7(18)C(14)-C(15)-C(42)-C(43) 177.7(5)C(14)-C(15)-C(42)-C(44) 53.1(6)C(14)-C(15)-O(4)-C(16) 81.2(5)C(38)-C(11)-C(10)-N(3) -89.0(6)C(38)-C(11)-C(10)-O(13) 89.4(6)C(38)-C(11)-O(3)-C(12) 171.5(4)C(12)-C(13)-C(39)-C(41) -166.4(5)C(12)-C(13)-C(39)-C(40) -44.2(7)C(12)-C(13)-N(4)-C(14) 62.5(6)C(9)-C(8)-O(2)-C(7) -177.7(4)C(8)-C(9)-C(35)-C(36) -57.6(6)C(8)-C(9)-C(35)-C(37) 178.4(5)C(8)-C(9)-N(3)-C(10) -122.9(5)C(10)-C(11)-O(3)-C(12) -69.4(5)C(6)-C(7)-C(32)-C(33) -50.2(5)C(6)-C(7)-C(32)-C(34) -174.9(4)C(6)-C(7)-O(2)-C(8) 80.5(5)C(5)-C(4)-O(1)-C(3) -179.3(4)C(4)-C(5)-C(29)-C(30) 59.6(7)C(4)-C(5)-C(29)-C(31) -173.0(6)C(4)-C(5)-N(2)-C(6) 64.4(6)C(3)-C(2)-N(1)-C(1) 173.3(4)C(2)-C(3)-O(1)-C(4) -66.7(6)C(1)-C(24)-O(7)-C(23) 177.7(4)C(24)-C(1)-C(25)-C(26) 44.0(6)C(24)-C(1)-C(25)-C(27) 165.5(5)C(24)-C(1)-N(1)-C(2) -54.5(6)C(23)-C(22)-N(6)-C(21) -176.6(5)C(23)-C(22)-O(19)-Ca(1) -20.1(18)C(22)-C(23)-C(52)-C(54) 175.2(4)C(22)-C(23)-C(52)-C(53) -61.1(6)C(22)-C(23)-O(7)-C(24) 62.2(5)C(21)-C(20)-O(6)-C(19) 173.7(4)C(20)-C(21)-C(49)-C(50) 65.5(6)C(20)-C(21)-C(49)-C(51) -169.4(5)C(20)-C(21)-N(6)-C(22) 119.8(5)C(19)-C(18)-N(5)-C(17) -173.2(5)C(18)-C(19)-O(6)-C(20) -77.6(5)C(18)-N(5)-C(17)-C(16) -75.8(6)C(18)-N(5)-C(17)-C(45) 157.6(5)N(5)-C(17)-C(16)-O(4) 151.4(4)N(5)-C(17)-C(16)-O(16) -29.4(7)N(5)-C(17)-C(45)-C(47) -62.1(6)N(5)-C(17)-C(45)-C(46) 175.4(5)C(17)-C(16)-O(4)-C(15) -171.3(4)C(16)-C(17)-C(45)-C(47) 174.7(5)C(16)-C(17)-C(45)-C(46) 52.1(7)C(15)-C(14)-N(4)-C(13) -176.4(4)C(42)-C(15)-O(4)-C(16) -157.9(4)C(45)-C(17)-C(16)-O(4) -85.3(5)C(45)-C(17)-C(16)-O(16) 93.9(7)C(48)-C(19)-C(18)-N(5) -119.4(5)C(48)-C(19)-C(18)-O(17) 60.9(7)C(48)-C(19)-O(6)-C(20) 161.7(4)
C(49)-C(21)-C(20)-O(6) 61.2(6)C(49)-C(21)-C(20)-O(18) -118.7(7)C(49)-C(21)-N(6)-C(22) -113.4(6)C(52)-C(23)-C(22)-N(6) 102.4(5)C(52)-C(23)-C(22)-O(19) -74.7(6)C(52)-C(23)-O(7)-C(24) -179.4(4)C(25)-C(1)-C(24)-O(7) -101.0(5)C(25)-C(1)-C(24)-O(8) 76.6(7)C(25)-C(1)-N(1)-C(2) -176.1(5)C(28)-C(3)-C(2)-N(1) -79.3(6)C(28)-C(3)-C(2)-O(9) 96.7(6)C(28)-C(3)-O(1)-C(4) 173.8(5)C(29)-C(5)-C(4)-O(1) 84.6(6)C(29)-C(5)-C(4)-O(10) -92.5(7)C(29)-C(5)-N(2)-C(6) -171.8(5)C(32)-C(7)-C(6)-N(2) 109.3(5)C(32)-C(7)-C(6)-O(11) -69.2(6)C(32)-C(7)-O(2)-C(8) -159.5(4)C(35)-C(9)-C(8)-O(2) -59.9(6)C(35)-C(9)-C(8)-O(12) 118.5(6)C(35)-C(9)-N(3)-C(10) 113.0(5)C(39)-C(13)-C(12)-O(3) 90.1(5)C(39)-C(13)-C(12)-O(14) -88.1(6)C(39)-C(13)-N(4)-C(14) -173.3(5)O(22A)-S(1A)-C(56A)-F(4A) -60.6(5)O(22A)-S(1A)-C(56A)-F(5A) 59.8(5)O(22A)-S(1A)-C(56A)-F(6A) 179.1(4)O(22A)-S(1A)-O(21)-Ca(2) 54.3(4)O(22A)-S(1A)-O(20)-Ca(1) -12.7(6)C(56A)-S(1A)-O(21)-Ca(2) 167.4(2)C(56A)-S(1A)-O(20)-Ca(1) -125.5(4)O(22B)-S(1B)-C(56B)-F(4B) 63.0(12)O(22B)-S(1B)-C(56B)-F(5B) -57.4(12)O(22B)-S(1B)-C(56B)-F(6B) -176.6(10)O(22B)-S(1B)-O(21)-Ca(2) -122.9(7)C(56B)-S(1B)-O(21)-Ca(2) 124.4(6)N(4)-C(13)-C(12)-O(3) -147.6(4)N(4)-C(13)-C(12)-O(14) 34.2(7)N(4)-C(13)-C(39)-C(41) 71.6(6)N(4)-C(13)-C(39)-C(40) -166.3(5)N(4)-C(14)-C(15)-C(42) 71.3(6)N(4)-C(14)-C(15)-O(4) -170.9(4)N(3)-C(9)-C(8)-O(2) 175.2(4)N(3)-C(9)-C(8)-O(12) -6.4(7)N(3)-C(9)-C(35)-C(36) 66.5(6)N(3)-C(9)-C(35)-C(37) -57.5(6)N(3)-C(10)-O(13)-Ca(2) -162.1(12)N(2)-C(6)-O(11)-Ca(1) -145.1(16)N(2)-C(5)-C(4)-O(1) -151.9(4)N(2)-C(5)-C(4)-O(10) 31.1(7)N(2)-C(5)-C(29)-C(30) -63.6(7)N(2)-C(5)-C(29)-C(31) 63.8(7)N(1)-C(1)-C(24)-O(7) 138.5(4)N(1)-C(1)-C(24)-O(8) -44.0(7)N(1)-C(1)-C(25)-C(26) 164.8(5)N(1)-C(1)-C(25)-C(27) -73.7(6)N(6)-C(22)-O(19)-Ca(1) 162.9(12)N(6)-C(21)-C(20)-O(6) -172.9(4)N(6)-C(21)-C(20)-O(18) 7.2(8)
S22
N(6)-C(21)-C(49)-C(50) -58.4(6)N(6)-C(21)-C(49)-C(51) 66.7(6)O(6)-C(19)-C(18)-N(5) 124.0(5)O(6)-C(19)-C(18)-O(17) -55.6(6)O(4)-C(15)-C(42)-C(43) 60.7(6)O(4)-C(15)-C(42)-C(44) -63.9(6)O(19)-C(22)-N(6)-C(21) 0.4(8)O(7)-C(23)-C(22)-N(6) -142.4(5)O(7)-C(23)-C(22)-O(19) 40.5(6)O(7)-C(23)-C(52)-C(54) 58.9(5)O(7)-C(23)-C(52)-C(53) -177.5(5)O(3)-C(11)-C(10)-N(3) 154.9(4)O(3)-C(11)-C(10)-O(13) -26.7(6)O(1)-C(3)-C(2)-N(1) 162.8(4)O(1)-C(3)-C(2)-O(9) -21.3(7)O(21)-S(1A)-C(56A)-F(4A) 174.9(4)O(21)-S(1A)-C(56A)-F(5A) -64.6(4)O(21)-S(1A)-C(56A)-F(6A) 54.7(4)O(21)-S(1A)-O(20)-Ca(1) 133.2(4)O(21)-S(1B)-C(56B)-F(4B) -172.9(8)O(21)-S(1B)-C(56B)-F(5B) 66.8(8)O(21)-S(1B)-C(56B)-F(6B) -52.5(7)O(20)-S(1A)-C(56A)-F(4A) 64.2(4)O(20)-S(1A)-C(56A)-F(5A) -175.4(4)O(20)-S(1A)-C(56A)-F(6A) -56.0(4)O(20)-S(1A)-O(21)-Ca(2) -92.0(3)O(20)-S(1B)-C(56B)-F(4B) -63.5(8)O(20)-S(1B)-C(56B)-F(5B) 176.2(8)O(20)-S(1B)-C(56B)-F(6B) 56.9(7)O(20)-S(1B)-O(21)-Ca(2) 19.6(7)O(15)-C(14)-C(15)-C(42) -106.2(6)O(15)-C(14)-C(15)-O(4) 11.6(7)O(15)-C(14)-N(4)-C(13) 1.1(8)O(14)-C(12)-O(3)-C(11) -2.6(7)O(13)-C(10)-N(3)-C(9) 3.8(8)O(2)-C(7)-C(6)-N(2) -134.2(5)O(2)-C(7)-C(6)-O(11) 47.2(6)O(2)-C(7)-C(32)-C(33) -167.2(4)O(2)-C(7)-C(32)-C(34) 68.2(5)O(11)-C(6)-N(2)-C(5) -2.6(8)
O(10)-C(4)-O(1)-C(3) -2.1(7)O(9)-C(2)-N(1)-C(1) -2.6(8)O(8)-C(24)-O(7)-C(23) 0.1(7)O(18)-C(20)-O(6)-C(19) -6.4(8)O(17)-C(18)-N(5)-C(17) 6.4(8)O(16)-C(16)-O(4)-C(15) 9.5(7)O(12)-C(8)-O(2)-C(7) 3.8(7)F(1)-C(55)-S(2)-O(24) 176.7(4)F(1)-C(55)-S(2)-O(25) 55.1(5)F(1)-C(55)-S(2)-O(23) -65.9(5)F(2)-C(55)-S(2)-O(24) 57.2(5)F(2)-C(55)-S(2)-O(25) -64.5(5)F(2)-C(55)-S(2)-O(23) 174.5(4)F(3)-C(55)-S(2)-O(24) -64.0(5)F(3)-C(55)-S(2)-O(25) 174.4(4)F(3)-C(55)-S(2)-O(23) 53.4(5)Ca(1)-O(23)-S(2)-C(55) -108.4(5)Ca(1)-O(23)-S(2)-O(24) 0.9(6)Ca(1)-O(23)-S(2)-O(25) 138.0(5)Ca(2)-O(24)-S(2)-C(55) -9.6(15)Ca(2)-O(24)-S(2)-O(25) 104.1(14)Ca(2)-O(24)-S(2)-O(23) -119.2(14)F(7)-C(58)-S(3)-O(29) -60.0(5)F(7)-C(58)-S(3)-O(31) 57.1(5)F(7)-C(58)-S(3)-O(30) 179.0(5)F(8)-C(58)-S(3)-O(29) -178.6(5)F(8)-C(58)-S(3)-O(31) -61.6(5)F(8)-C(58)-S(3)-O(30) 60.3(5)F(9)-C(58)-S(3)-O(29) 62.7(5)F(9)-C(58)-S(3)-O(31) 179.8(4)F(9)-C(58)-S(3)-O(30) -58.3(5)F(10)-C(57)-S(4)-O(28) 57.7(5)F(10)-C(57)-S(4)-O(26) 179.1(5)F(10)-C(57)-S(4)-O(27) -62.2(5)F(11)-C(57)-S(4)-O(28) -61.9(5)F(11)-C(57)-S(4)-O(26) 59.4(5)F(11)-C(57)-S(4)-O(27) 178.2(4)F(12)-C(57)-S(4)-O(28) 177.9(4)F(12)-C(57)-S(4)-O(26) -60.7(5)F(12)-C(57)-S(4)-O(27) 58.0(5)
______________________________________________________________________________________________________________________________________________________________________________________________________________________________
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Table 6. Hydrogen bonds for Sample A [Å and °].____________________________________________________________________________ D-H...A d(D-H) d(H...A) d(D...A) <(DHA)______________________________________________________________________________________________________________________________________________________________________________________________ N(4)-H(4)...O(30)#1 0.88 2.01 2.884(6) 170.9 N(6)-H(6)...O(29)#2 0.86 2.02 2.874(6) 173.4 O(1W)-H(1WB)...N(2S)#30.97(3) 1.94(3) 2.885(7) 163(6) O(2W)-H(2WA)...N(4S) 0.93(2) 1.91(3) 2.836(7) 173(5) O(2W)-H(2WB)...N(3S) 0.95(3) 1.98(4) 2.868(6) 154(6)____________________________________________________________________________ Symmetry transformations used to generate equivalent atoms: #1 x,y,z+1 #2 x,y+1,z #3 x-1,y,z
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IV. X-ray crystallography data of the crystal sample B, [(valinomycin)Ca2(OTf)2(H2O)2](OTf)2·2H2O·5THFCrystal Data and Experimental
Experimental. A suitable crystal (0.91 × 0.47 × 0.25 mm3) was selected and mounted on a Bruker APEX-II CCD diffractometer. The crystal was cooled to T = 110(2) K during data collection. The structure was solved with the Superflip (L. Palatinus & G. Chapuis, 2007) structure solution program using Olex2 (Dolomanov et al., 2009),
using the Charge Flipping solution method. The structure was refined with version 2014/6 of XL (Sheldrick, 2008) using Least Squares minimization.Crystal Data. C78H138Ca2F12N6O39S4, Mr = 2220.34, triclinic, P1 (No. 1), a = 12.9742(12) Å, b = 13.6801(12) Å, c = 15.9369(14) Å, = 99.8400(10)°, = 100.9590(10)°, = 101.4430(10)°, V = 2657.1(4) Å3, T = 110(2) K, Z = 1, Z' = 1, (MoK) = 0.290, 44495 reflections measured, 31711 unique (Rint = 0.0454) which were used in all calculations. The final wR2 was 0.1297 (all data) and R1 was 0.0484 (I > 2(σI)).
S24
Compound Compound BFormula C
78H138Ca2F12N6O39S4Dcalc./ g cm-3 1.388/mm-1 0.290Formula Weight 2220.34Color colourlessShape prismMax Size/mm 0.91Mid Size/mm 0.47Min Size/mm 0.25T/K 110(2)Crystal System triclinicSpace Group P1a/Å 12.9742(12)b/Å 13.6801(12)c/Å 15.9369(14)/° 99.8400(10)/° 100.9590(10)/° 101.4430(10)V/Å3 2657.1(4)Z 1Z' 1min/° 1.556max/° 31.023Measured Refl. 44495Independent Refl. 31711Reflections I > 2(σI) 28704Rint 0.0454Parameters 1335Restraints 19Largest Peak 0.703Deepest Hole -0.395GooF 1.037wR2 (all data) 0.1297wR2 0.1243R1 (all data) 0.0540R1 0.0484Experimental Extended. A colorless prism-shaped crystal with dimensions 0.91 × 0.47 × 0.25 mm3 was mounted on a Bruker APEX-II CCD diffractometer equipped with an Oxford Cryostream low-temperature apparatus operating at T = 110(2) K.Data were measured using and scans scans of 0.50° per frame using MoK radiation (fine-focus sealed tube, 45 kV, 35 mA). The total number of runs and images was based on the strategy calculation from the program APEX2 (Bruker, 2013). The resolution that was achieved was = 31.023°.Unit cell indexing was performed by using the APEX2 (Bruker, 2013) software and the cell parameters were refined using SAINT (Bruker, V8.34A, 2013) on 9918 reflections, 22% of the observed reflections.Data reduction was performed using the SAINT (Bruker, V8.34A, 2013) software. The final completeness is 100% out to 31.023° in . The absorption coefficient (μ) of this
S25
material is 0.290 mm-1 and the minimum and maximum transmissions are 0.6752 and 0.7462.The structure was solved by Charge Flipping using the Superflip (L. Palatinus & G. Chapuis, 2007) structure solution program and refined by Least Squares using version 2014/6 of XL (Sheldrick, 2008).The structure was solved in the space group P1 (# 1). All non-hydrogen atoms were refined anisotropically. Hydrogen positions were calculated geometrically and refined using the riding model.The Flack parameter was refined to 0.031(13), confirming the absolute stereochemistry. Determination of absolute structure using Bayesian statistics on Bijvoet differences using the program within PLATON (Spek, 2003) also report that we have the correct enantiomer based on this comparison_________________________________________________________________________________________________________________________________________________________________________________________________________
Table 7. Atomic coordinates ( x 104) and equivalent isotropic displacement parameters (Å2x 103)for Sample B. U(eq) is defined as one third of the trace of the orthogonalized Uij tensor._________________________________________________________________________________________________________________________________________________________________________________________________________
x y z U(eq)________________________________________________________________________________ Ca(1) 4507(1) 2097(1) 8982(1) 14(1)Ca(2) 2048(1) 115(1) 11080(1) 13(1)S(1) 4038(1) -381(1) 9790(1) 16(1)S(2) 2459(1) 2487(1) 10190(1) 15(1)F(1) 1005(2) 2795(2) 8947(2) 42(1)F(3) 1251(2) 1269(2) 8746(2) 39(1)F(2) 369(2) 1749(2) 9693(2) 35(1)F(4) 6092(2) -325(2) 10280(2) 42(1)F(6) 5078(2) -1139(3) 10986(2) 62(1)F(5) 5446(2) 506(3) 11255(2) 59(1)O(7) 7540(2) 3681(2) 9816(1) 17(1)O(12) 468(2) -386(2) 7082(2) 22(1)O(1W) 1020(2) 1092(2) 11728(2) 26(1)O(21) 3189(2) -506(2) 10260(2) 22(1)O(2W) 5679(2) 1294(2) 8353(2) 26(1)O(20) 4269(2) 593(2) 9546(2) 28(1)O(1) 3380(2) 4175(2) 7681(1) 19(1)O(10) 3705(2) 3166(2) 6539(2) 20(1)O(11) 3080(2) 1592(2) 7780(1) 19(1)O(2) 2198(2) -525(2) 7310(1) 18(1)O(9) 5091(2) 3528(2) 8478(2) 20(1)O(13) 802(2) -622(2) 9800(1) 20(1)O(3) -1074(2) -1268(2) 10260(1) 15(1)O(14) -566(2) -2757(2) 10051(1) 20(1)O(15) 1296(2) -1244(2) 11629(1) 18(1)O(4) 2946(2) -1961(2) 12426(1) 16(1)O(8) 6928(2) 5117(2) 9967(1) 21(1)O(17) 3484(2) 526(2) 12290(1) 18(1)O(6) 4265(2) 2659(2) 12752(1) 16(1)O(18) 5987(2) 2508(2) 12924(2) 24(1)O(19) 5706(2) 2940(2) 10259(1) 21(1)O(16) 2682(2) -969(2) 13610(2) 24(1)O(23) 3262(2) 2729(2) 9696(2) 20(1)O(22) 3972(2) -1248(2) 9119(2) 31(1)O(24) 2530(2) 1611(2) 10566(2) 26(1)O(25) 2315(2) 3355(2) 10766(2) 28(1)
S26
N(1) 6303(2) 4711(2) 8122(2) 18(1)N(2) 1895(2) 1678(2) 6580(2) 16(1)N(3) 95(2) -1424(2) 8381(2) 17(1)N(4) 18(2) -2446(2) 11894(2) 16(1)N(5) 4573(2) 451(2) 13544(2) 16(1)N(6) 6369(2) 3622(2) 11697(2) 16(1)C(15) 1868(2) -2590(2) 12280(2) 15(1)C(5) 1962(2) 2754(2) 6915(2) 18(1)C(20) 5254(2) 2828(2) 12580(2) 16(1)C(43) 2521(3) -4198(2) 12066(2) 29(1)C(4) 3112(2) 3367(2) 7004(2) 16(1)C(3) 4442(2) 4838(2) 7827(2) 20(1)C(28) 4483(3) 5770(3) 8521(3) 36(1)C(2) 5295(2) 4286(2) 8152(2) 17(1)C(1) 7220(2) 4366(2) 8559(2) 15(1)C(6) 2475(2) 1180(2) 7053(2) 15(1)C(7) 2393(2) 66(2) 6656(2) 15(1)C(8) 1192(2) -689(2) 7456(2) 16(1)C(9) 1133(2) -1334(2) 8138(2) 17(1)C(10) 19(2) -1088(2) 9195(2) 15(1)C(11) -1127(2) -1267(2) 9347(2) 16(1)C(12) -797(2) -2088(2) 10514(2) 16(1)C(13) -867(2) -2064(2) 11466(2) 15(1)C(14) 1044(2) -2019(2) 11914(2) 15(1)C(24) 7189(2) 4445(2) 9520(2) 17(1)C(16) 3251(2) -1185(2) 13133(2) 16(1)C(17) 4449(2) -649(2) 13268(2) 15(1)C(18) 4056(2) 957(2) 13026(2) 14(1)C(19) 4158(2) 2075(2) 13420(2) 16(1)C(21) 5314(2) 3483(2) 11902(2) 16(1)C(22) 6476(2) 3391(2) 10874(2) 15(1)C(23) 7615(2) 3700(2) 10733(2) 16(1)C(52) 8324(3) 2983(3) 10991(2) 22(1)C(54) 9465(3) 3383(4) 10892(2) 36(1)C(53) 7844(3) 1888(3) 10485(2) 33(1)C(49) 5036(2) 4519(2) 12201(2) 20(1)C(50) 5793(3) 5121(3) 13066(2) 28(1)C(51) 5040(3) 5119(3) 11477(2) 27(1)C(48) 3145(3) 2198(2) 13732(2) 21(1)C(45) 5161(2) -1043(2) 13955(2) 20(1)C(47) 6361(2) -544(3) 14065(3) 29(1)C(46) 4975(3) -2203(3) 13702(3) 32(1)C(42) 1795(2) -3590(2) 11636(2) 20(1)C(44) 2038(3) -3403(3) 10769(2) 31(1)C(39) -1962(2) -2744(2) 11493(2) 18(1)C(41) -2096(3) -2628(3) 12435(2) 24(1)C(40) -2909(2) -2503(3) 10909(2) 25(1)C(38) -1652(3) -414(3) 9148(2) 23(1)C(35) 1358(3) -2385(2) 7803(2) 21(1)C(36) 554(3) -2963(3) 6950(2) 28(1)C(37) 1367(3) -3002(3) 8517(3) 29(1)C(32) 3456(2) -78(2) 6444(2) 18(1)C(33) 3766(3) 580(3) 5805(2) 25(1)C(34) 3391(3) -1199(3) 6079(3) 30(1)C(29) 1082(3) 3106(3) 6329(2) 26(1)C(30) 1281(3) 3121(3) 5409(2) 31(1)C(31) 943(3) 4132(3) 6780(3) 37(1)C(25) 8283(2) 5029(2) 8465(2) 18(1)C(26) 9267(2) 4849(2) 9060(2) 23(1)
S27
C(27) 8367(3) 4815(3) 7508(2) 27(1)C(55) 1205(2) 2052(3) 9349(2) 24(1)C(56) 5230(3) -330(3) 10623(2) 33(1)S(3) 6845(1) -2819(1) 6881(1) 21(1)F(7) 7750(2) -3747(2) 5757(2) 45(1)F(8) 6186(2) -3587(2) 5185(1) 45(1)F(9) 7538(2) -2278(2) 5551(2) 47(1)O(27) 6333(2) -3797(2) 7019(2) 27(1)O(28) 6124(3) -2143(2) 6782(2) 45(1)O(29) 7908(2) -2377(3) 7413(2) 57(1)C(57) 7090(3) -3120(3) 5787(2) 26(1)S(4) -434(1) 5023(1) 13153(1) 20(1)F(10) -1038(3) 6233(2) 14313(2) 64(1)F(11) -358(3) 5097(3) 14813(2) 61(1)F(12) 649(3) 6408(3) 14543(2) 85(1)O(30) -290(3) 5813(3) 12669(2) 54(1)O(31) 397(2) 4469(2) 13225(2) 39(1)O(32) -1515(2) 4401(2) 12955(2) 40(1)C(58) -278(3) 5717(3) 14266(3) 39(1)O(33) 488(2) 485(2) 14935(2) 27(1)C(59) -498(3) -119(3) 15042(2) 31(1)C(60) -455(3) -1226(3) 14770(2) 35(1)C(61) 449(3) -1194(3) 14274(3) 35(1)C(62) 737(3) -94(3) 14191(2) 30(1)O(34) -661(2) 849(2) 12507(2) 34(1)C(63) -1799(3) 425(3) 12339(3) 28(1)C(64) -2279(3) 1270(3) 12730(2) 26(1)C(65) -1340(3) 1922(3) 13476(3) 32(1)C(66) -390(3) 1868(3) 13062(3) 34(1)O(35) 7168(2) 1659(2) 7363(2) 32(1)C(67) 6828(3) 722(3) 6687(2) 31(1)C(68) 7788(4) 267(4) 6690(3) 46(1)C(69) 8737(3) 1150(4) 7154(3) 44(1)C(70) 8271(3) 1768(3) 7800(3) 39(1)O(36) 6027(2) 2005(2) 5104(2) 22(1)C(71) 7080(3) 2419(3) 4986(3) 32(1)C(72) 7232(3) 3588(3) 5119(3) 34(1)C(73) 6216(3) 3784(3) 5393(2) 28(1)C(74) 5774(3) 2810(3) 5686(2) 26(1)O(37) 3302(2) 5251(2) 6010(2) 33(1)C(75) 3890(3) 4915(3) 5375(2) 30(1)C(76) 3463(3) 5315(3) 4578(3) 36(1)C(77) 3339(5) 6362(4) 5018(4) 59(1)C(78) 3105(6) 6184(5) 5901(4) 71(2)O(4W) 1693(2) 3193(2) 12387(2) 28(1)O(3W) 5515(2) -769(2) 8079(2) 37(1)________________________________________________________________________________
Table 8. Bond lengths [Å] and angles [°] for Sample B.________________________________________________________________________________________________________________________________________________________________________________________________________________________________________
Ca(1)-O(2W) 2.321(2)Ca(1)-O(20) 2.371(2)Ca(1)-O(11) 2.295(2)Ca(1)-O(9) 2.288(2)Ca(1)-O(19) 2.276(2)Ca(1)-O(23) 2.360(2)Ca(2)-O(1W) 2.323(2)
Ca(2)-O(21) 2.340(2)Ca(2)-O(13) 2.278(2)Ca(2)-O(15) 2.310(2)Ca(2)-O(17) 2.314(2)Ca(2)-O(24) 2.347(2)S(1)-O(21) 1.445(2)S(1)-O(20) 1.442(2)
S(1)-O(22) 1.431(3)S(1)-C(56) 1.818(3)S(2)-O(23) 1.442(2)S(2)-O(24) 1.440(2)S(2)-O(25) 1.439(2)S(2)-C(55) 1.820(3)F(1)-C(55) 1.332(4)
S28
F(3)-C(55) 1.331(4)F(2)-C(55) 1.332(4)F(4)-C(56) 1.334(4)F(6)-C(56) 1.332(5)F(5)-C(56) 1.331(5)O(7)-C(24) 1.342(4)O(7)-C(23) 1.441(3)O(12)-C(8) 1.199(4)O(1W)-H(1WA)
0.967(14)O(1W)-H(1WB)
0.965(14)O(2W)-H(2WA)
0.965(14)O(2W)-H(2WB)
0.965(14)O(1)-C(4) 1.343(4)O(1)-C(3) 1.444(4)O(10)-C(4) 1.203(4)O(11)-C(6) 1.237(4)O(2)-C(7) 1.452(3)O(2)-C(8) 1.351(3)O(9)-C(2) 1.241(4)O(13)-C(10) 1.236(4)O(3)-C(11) 1.444(3)O(3)-C(12) 1.345(4)O(14)-C(12) 1.197(4)O(15)-C(14) 1.234(4)O(4)-C(15) 1.442(3)O(4)-C(16) 1.345(4)O(8)-C(24) 1.208(4)O(17)-C(18) 1.239(3)O(6)-C(20) 1.346(3)O(6)-C(19) 1.448(3)O(18)-C(20) 1.201(4)O(19)-C(22) 1.231(4)O(16)-C(16) 1.196(4)N(1)-C(2) 1.336(4)N(1)-C(1) 1.464(4)N(1)-H(1) 0.93(2)N(2)-C(5) 1.456(4)N(2)-C(6) 1.328(4)N(2)-H(2) 0.92(2)N(3)-C(9) 1.458(4)N(3)-C(10) 1.330(4)N(3)-H(3) 0.94(2)N(4)-H(4) 0.8600N(4)-C(13) 1.454(4)N(4)-C(14) 1.335(4)N(5)-C(17) 1.461(4)N(5)-C(18) 1.334(4)N(5)-H(5) 0.92(2)N(6)-H(6) 0.8600N(6)-C(21) 1.450(4)N(6)-C(22) 1.337(4)
C(15)-H(15) 0.9800C(15)-C(14) 1.530(4)C(15)-C(42) 1.538(4)C(5)-H(5A) 0.9800C(5)-C(4) 1.528(4)C(5)-C(29) 1.541(4)C(20)-C(21) 1.521(4)C(43)-H(43A) 0.9600C(43)-H(43B) 0.9600C(43)-H(43C) 0.9600C(43)-C(42) 1.520(4)C(3)-H(3A) 0.9800C(3)-C(28) 1.524(5)C(3)-C(2) 1.520(4)C(28)-H(28A) 0.9600C(28)-H(28B) 0.9600C(28)-H(28C) 0.9600C(1)-H(1A) 0.9800C(1)-C(24) 1.525(4)C(1)-C(25) 1.542(4)C(6)-C(7) 1.521(4)C(7)-H(7) 0.9800C(7)-C(32) 1.523(4)C(8)-C(9) 1.515(4)C(9)-H(9) 0.9800C(9)-C(35) 1.550(4)C(10)-C(11) 1.530(4)C(11)-H(11) 0.9800C(11)-C(38) 1.513(4)C(12)-C(13) 1.533(4)C(13)-H(13) 0.9800C(13)-C(39) 1.549(4)C(16)-C(17) 1.538(4)C(17)-H(17) 0.9800C(17)-C(45) 1.535(4)C(18)-C(19) 1.520(4)C(19)-H(19) 0.9800C(19)-C(48) 1.519(4)C(21)-H(21) 0.9800C(21)-C(49) 1.551(4)C(22)-C(23) 1.524(4)C(23)-H(23) 0.9800C(23)-C(52) 1.526(4)C(52)-H(52) 0.9800C(52)-C(54) 1.521(5)C(52)-C(53) 1.519(5)C(54)-H(54A) 0.9600C(54)-H(54B) 0.9600C(54)-H(54C) 0.9600C(53)-H(53A) 0.9600C(53)-H(53B) 0.9600C(53)-H(53C) 0.9600C(49)-H(49) 0.9800C(49)-C(50) 1.522(5)C(49)-C(51) 1.526(4)C(50)-H(50A) 0.9600C(50)-H(50B) 0.9600C(50)-H(50C) 0.9600C(51)-H(51A) 0.9600
C(51)-H(51B) 0.9600C(51)-H(51C) 0.9600C(48)-H(48A) 0.9600C(48)-H(48B) 0.9600C(48)-H(48C) 0.9600C(45)-H(45) 0.9800C(45)-C(47) 1.535(4)C(45)-C(46) 1.527(4)C(47)-H(47A) 0.9600C(47)-H(47B) 0.9600C(47)-H(47C) 0.9600C(46)-H(46A) 0.9600C(46)-H(46B) 0.9600C(46)-H(46C) 0.9600C(42)-H(42) 0.9800C(42)-C(44) 1.525(5)C(44)-H(44A) 0.9600C(44)-H(44B) 0.9600C(44)-H(44C) 0.9600C(39)-H(39) 0.9800C(39)-C(41) 1.528(4)C(39)-C(40) 1.522(4)C(41)-H(41A) 0.9600C(41)-H(41B) 0.9600C(41)-H(41C) 0.9600C(40)-H(40A) 0.9600C(40)-H(40B) 0.9600C(40)-H(40C) 0.9600C(38)-H(38A) 0.9600C(38)-H(38B) 0.9600C(38)-H(38C) 0.9600C(35)-H(35) 0.9800C(35)-C(36) 1.526(5)C(35)-C(37) 1.528(5)C(36)-H(36A) 0.9600C(36)-H(36B) 0.9600C(36)-H(36C) 0.9600C(37)-H(37A) 0.9600C(37)-H(37B) 0.9600C(37)-H(37C) 0.9600C(32)-H(32) 0.9800C(32)-C(33) 1.529(4)C(32)-C(34) 1.524(4)C(33)-H(33A) 0.9600C(33)-H(33B) 0.9600C(33)-H(33C) 0.9600C(34)-H(34A) 0.9600C(34)-H(34B) 0.9600C(34)-H(34C) 0.9600C(29)-H(29) 0.9800C(29)-C(30) 1.539(5)C(29)-C(31) 1.524(5)C(30)-H(30A) 0.9600C(30)-H(30B) 0.9600C(30)-H(30C) 0.9600C(31)-H(31A) 0.9600C(31)-H(31B) 0.9600C(31)-H(31C) 0.9600C(25)-H(25) 0.9800
S29
C(25)-C(26) 1.527(4)C(25)-C(27) 1.532(4)C(26)-H(26A) 0.9600C(26)-H(26B) 0.9600C(26)-H(26C) 0.9600C(27)-H(27A) 0.9600C(27)-H(27B) 0.9600C(27)-H(27C) 0.9600S(3)-O(27) 1.443(2)S(3)-O(28) 1.446(3)S(3)-O(29) 1.427(3)S(3)-C(57) 1.824(3)F(7)-C(57) 1.329(4)F(8)-C(57) 1.330(4)F(9)-C(57) 1.330(4)S(4)-O(30) 1.434(3)S(4)-O(31) 1.434(3)S(4)-O(32) 1.434(3)S(4)-C(58) 1.817(4)F(10)-C(58) 1.327(6)F(11)-C(58) 1.320(5)F(12)-C(58) 1.319(5)O(33)-C(59) 1.435(4)O(33)-C(62) 1.437(4)C(59)-H(59A) 0.9700C(59)-H(59B) 0.9700C(59)-C(60) 1.517(6)C(60)-H(60A) 0.9700C(60)-H(60B) 0.9700C(60)-C(61) 1.531(5)C(61)-H(61A) 0.9700C(61)-H(61B) 0.9700C(61)-C(62) 1.511(5)C(62)-H(62A) 0.9700C(62)-H(62B) 0.9700O(34)-C(63) 1.430(4)O(34)-C(66) 1.455(5)C(63)-H(63A) 0.9700C(63)-H(63B) 0.9700C(63)-C(64) 1.517(5)C(64)-H(64A) 0.9700C(64)-H(64B) 0.9700C(64)-C(65) 1.533(5)C(65)-H(65A) 0.9700C(65)-H(65B) 0.9700C(65)-C(66) 1.513(5)C(66)-H(66A) 0.9700C(66)-H(66B) 0.9700O(35)-C(67) 1.457(5)O(35)-C(70) 1.433(5)C(67)-H(67A) 0.9700C(67)-H(67B) 0.9700C(67)-C(68) 1.497(5)C(68)-H(68A) 0.9700C(68)-H(68B) 0.9700C(68)-C(69) 1.510(6)C(69)-H(69A) 0.9700C(69)-H(69B) 0.9700C(69)-C(70) 1.511(6)
C(70)-H(70A) 0.9700C(70)-H(70B) 0.9700O(36)-C(71) 1.432(4)O(36)-C(74) 1.445(4)C(71)-H(71A) 0.9700C(71)-H(71B) 0.9700C(71)-C(72) 1.544(6)C(72)-H(72A) 0.9700C(72)-H(72B) 0.9700C(72)-C(73) 1.523(5)C(73)-H(73A) 0.9700C(73)-H(73B) 0.9700C(73)-C(74) 1.527(5)C(74)-H(74A) 0.9700C(74)-H(74B) 0.9700O(37)-C(75) 1.447(4)O(37)-C(78) 1.384(5)C(75)-H(75A) 0.9700C(75)-H(75B) 0.9700C(75)-C(76) 1.520(5)C(76)-H(76A) 0.9700C(76)-H(76B) 0.9700C(76)-C(77) 1.536(6)C(77)-H(77A) 0.9700C(77)-H(77B) 0.9700C(77)-C(78) 1.543(7)C(78)-H(78A) 0.9700C(78)-H(78B) 0.9700O(4W)-H(4WA)
0.967(14)O(4W)-H(4WB)
0.972(14)O(3W)-H(3WA)
0.951(13)O(3W)-H(3WB)
0.952(14)
O(2W)-Ca(1)-O(20) 80.17(9)O(2W)-Ca(1)-O(23)172.78(9)O(11)-Ca(1)-O(2W) 96.57(9)O(11)-Ca(1)-O(20) 99.42(9)O(11)-Ca(1)-O(23) 84.29(8)O(9)-Ca(1)-O(2W) 90.66(9)O(9)-Ca(1)-O(20) 168.51(9)O(9)-Ca(1)-O(11) 88.41(8)O(9)-Ca(1)-O(23) 96.54(8)O(19)-Ca(1)-O(2W) 97.23(9)O(19)-Ca(1)-O(20) 89.21(9)O(19)-Ca(1)-O(11)164.80(9)O(19)-Ca(1)-O(9) 85.08(8)O(19)-Ca(1)-O(23) 82.83(8)O(23)-Ca(1)-O(20) 92.61(8)O(1W)-Ca(2)-O(21)165.10(9)O(1W)-Ca(2)-O(24) 80.23(9)O(21)-Ca(2)-O(24) 84.92(9)
O(13)-Ca(2)-O(1W) 97.51(9)O(13)-Ca(2)-O(21) 81.33(8)O(13)-Ca(2)-O(15) 87.09(8)O(13)-Ca(2)-O(17)166.12(8)O(13)-Ca(2)-O(24) 90.61(9)O(15)-Ca(2)-O(1W) 89.70(9)O(15)-Ca(2)-O(21)105.04(8)O(15)-Ca(2)-O(17) 87.88(8)O(15)-Ca(2)-O(24)169.29(8)O(17)-Ca(2)-O(1W) 95.39(9)O(17)-Ca(2)-O(21) 87.51(8)O(17)-Ca(2)-O(24) 96.62(8)O(21)-S(1)-C(56)102.42(15)O(20)-S(1)-O(21)114.24(14)O(20)-S(1)-C(56)103.95(18)O(22)-S(1)-O(21)114.47(15)O(22)-S(1)-O(20)115.16(16)O(22)-S(1)-C(56)104.52(18)O(23)-S(2)-C(55)103.02(14)O(24)-S(2)-O(23)113.56(14)O(24)-S(2)-C(55)103.66(15)O(25)-S(2)-O(23)114.53(15)O(25)-S(2)-O(24)115.30(16)O(25)-S(2)-C(55)104.83(16)C(24)-O(7)-C(23) 116.0(2)Ca(2)-O(1W)-H(1WA)126(3)Ca(2)-O(1W)-H(1WB)125(3)H(1WA)-O(1W)-H(1WB)106(2)S(1)-O(21)-Ca(2)153.04(15)Ca(1)-O(2W)-H(2WA)126(3)Ca(1)-O(2W)-H(2WB)126(3)H(2WA)-O(2W)-H(2WB)107(2)S(1)-O(20)-Ca(1)173.21(18)C(4)-O(1)-C(3) 116.3(2)C(6)-O(11)-Ca(1) 164.2(2)C(8)-O(2)-C(7) 116.5(2)C(2)-O(9)-Ca(1) 173.1(2)C(10)-O(13)-Ca(2) 169.1(2)C(12)-O(3)-C(11) 114.5(2)C(14)-O(15)-Ca(2) 169.8(2)C(16)-O(4)-C(15) 115.8(2)C(18)-O(17)-Ca(2) 159.3(2)C(20)-O(6)-C(19) 114.0(2)C(22)-O(19)-Ca(1) 169.8(2)S(2)-O(23)-Ca(1)144.79(14)S(2)-O(24)-Ca(2)161.71(15)C(2)-N(1)-C(1) 120.7(2)C(2)-N(1)-H(1) 117(2)C(1)-N(1)-H(1) 122(2)C(5)-N(2)-H(2) 118(3)C(6)-N(2)-C(5) 119.8(2)C(6)-N(2)-H(2) 122(3)C(9)-N(3)-H(3) 119(2)C(10)-N(3)-C(9) 122.3(2)C(10)-N(3)-H(3) 118(2)C(13)-N(4)-H(4) 119.4C(14)-N(4)-H(4) 119.4C(14)-N(4)-C(13) 121.2(2)C(17)-N(5)-H(5) 120(3)
S30
C(18)-N(5)-C(17) 120.6(2)C(18)-N(5)-H(5) 119(3)C(21)-N(6)-H(6) 119.2C(22)-N(6)-H(6) 119.2C(22)-N(6)-C(21) 121.5(2)O(4)-C(15)-H(15) 109.4O(4)-C(15)-C(14) 109.5(2)O(4)-C(15)-C(42) 107.7(2)C(14)-C(15)-H(15) 109.4C(14)-C(15)-C(42) 111.5(2)C(42)-C(15)-H(15) 109.4N(2)-C(5)-H(5A) 107.9N(2)-C(5)-C(4) 109.0(2)N(2)-C(5)-C(29) 109.8(2)C(4)-C(5)-H(5A) 107.9C(4)-C(5)-C(29) 114.2(3)C(29)-C(5)-H(5A) 107.9O(6)-C(20)-C(21) 110.7(2)O(18)-C(20)-O(6) 124.2(3)O(18)-C(20)-C(21) 125.1(3)H(43A)-C(43)-H(43B) 109.5H(43A)-C(43)-H(43C) 109.5H(43B)-C(43)-H(43C) 109.5C(42)-C(43)-H(43A) 109.5C(42)-C(43)-H(43B) 109.5C(42)-C(43)-H(43C) 109.5O(1)-C(4)-C(5) 110.4(2)O(10)-C(4)-O(1) 124.0(3)O(10)-C(4)-C(5) 125.5(3)O(1)-C(3)-H(3A) 110.2O(1)-C(3)-C(28) 106.3(3)O(1)-C(3)-C(2) 109.5(2)C(28)-C(3)-H(3A) 110.2C(2)-C(3)-H(3A) 110.2C(2)-C(3)-C(28) 110.4(3)C(3)-C(28)-H(28A) 109.5C(3)-C(28)-H(28B) 109.5C(3)-C(28)-H(28C) 109.5H(28A)-C(28)-H(28B) 109.5H(28A)-C(28)-H(28C) 109.5H(28B)-C(28)-H(28C) 109.5O(9)-C(2)-N(1) 121.5(3)O(9)-C(2)-C(3) 122.8(3)N(1)-C(2)-C(3) 115.6(3)N(1)-C(1)-H(1A) 109.3N(1)-C(1)-C(24) 108.5(2)N(1)-C(1)-C(25) 109.5(2)C(24)-C(1)-H(1A) 109.3C(24)-C(1)-C(25) 111.0(2)C(25)-C(1)-H(1A) 109.3O(11)-C(6)-N(2) 122.6(3)O(11)-C(6)-C(7) 120.2(3)N(2)-C(6)-C(7) 117.2(2)O(2)-C(7)-C(6) 107.9(2)O(2)-C(7)-H(7) 110.4O(2)-C(7)-C(32) 106.6(2)C(6)-C(7)-H(7) 110.4C(6)-C(7)-C(32) 111.0(2)C(32)-C(7)-H(7) 110.4
O(12)-C(8)-O(2) 124.4(3)O(12)-C(8)-C(9) 126.5(3)O(2)-C(8)-C(9) 109.1(2)N(3)-C(9)-C(8) 110.2(2)N(3)-C(9)-H(9) 107.8N(3)-C(9)-C(35) 112.7(2)C(8)-C(9)-H(9) 107.8C(8)-C(9)-C(35) 110.3(2)C(35)-C(9)-H(9) 107.8O(13)-C(10)-N(3) 123.7(3)O(13)-C(10)-C(11) 120.4(3)N(3)-C(10)-C(11) 115.8(2)O(3)-C(11)-C(10) 109.0(2)O(3)-C(11)-H(11) 109.9O(3)-C(11)-C(38) 106.6(2)C(10)-C(11)-H(11) 109.9C(38)-C(11)-C(10) 111.3(2)C(38)-C(11)-H(11) 109.9O(3)-C(12)-C(13) 110.3(2)O(14)-C(12)-O(3) 124.7(3)O(14)-C(12)-C(13) 125.0(3)N(4)-C(13)-C(12) 108.5(2)N(4)-C(13)-H(13) 109.5N(4)-C(13)-C(39) 109.8(2)C(12)-C(13)-H(13) 109.5C(12)-C(13)-C(39) 109.9(2)C(39)-C(13)-H(13) 109.5O(15)-C(14)-N(4) 122.0(3)O(15)-C(14)-C(15) 123.0(2)N(4)-C(14)-C(15) 115.0(2)O(7)-C(24)-C(1) 110.3(2)O(8)-C(24)-O(7) 124.1(3)O(8)-C(24)-C(1) 125.6(3)O(4)-C(16)-C(17) 110.4(2)O(16)-C(16)-O(4) 124.7(3)O(16)-C(16)-C(17) 124.9(3)N(5)-C(17)-C(16) 108.5(2)N(5)-C(17)-H(17) 109.1N(5)-C(17)-C(45) 110.6(2)C(16)-C(17)-H(17) 109.1C(45)-C(17)-C(16) 110.6(2)C(45)-C(17)-H(17) 109.1O(17)-C(18)-N(5) 121.8(3)O(17)-C(18)-C(19) 122.4(3)N(5)-C(18)-C(19) 115.7(2)O(6)-C(19)-C(18) 108.8(2)O(6)-C(19)-H(19) 109.9O(6)-C(19)-C(48) 108.3(2)C(18)-C(19)-H(19) 109.9C(48)-C(19)-C(18) 109.9(2)C(48)-C(19)-H(19) 109.9N(6)-C(21)-C(20) 110.0(2)N(6)-C(21)-H(21) 107.7N(6)-C(21)-C(49) 111.8(2)C(20)-C(21)-H(21) 107.7C(20)-C(21)-C(49) 111.8(2)C(49)-C(21)-H(21) 107.7O(19)-C(22)-N(6) 122.4(3)O(19)-C(22)-C(23) 121.2(3)
N(6)-C(22)-C(23) 116.4(2)O(7)-C(23)-C(22) 108.6(2)O(7)-C(23)-H(23) 109.2O(7)-C(23)-C(52) 107.4(2)C(22)-C(23)-H(23) 109.2C(22)-C(23)-C(52) 113.3(2)C(52)-C(23)-H(23) 109.2C(23)-C(52)-H(52) 107.4C(54)-C(52)-C(23) 110.1(3)C(54)-C(52)-H(52) 107.4C(53)-C(52)-C(23) 112.2(3)C(53)-C(52)-H(52) 107.4C(53)-C(52)-C(54) 111.9(3)C(52)-C(54)-H(54A) 109.5C(52)-C(54)-H(54B) 109.5C(52)-C(54)-H(54C) 109.5H(54A)-C(54)-H(54B) 109.5H(54A)-C(54)-H(54C) 109.5H(54B)-C(54)-H(54C) 109.5C(52)-C(53)-H(53A) 109.5C(52)-C(53)-H(53B) 109.5C(52)-C(53)-H(53C) 109.5H(53A)-C(53)-H(53B) 109.5H(53A)-C(53)-H(53C) 109.5H(53B)-C(53)-H(53C) 109.5C(21)-C(49)-H(49) 107.7C(50)-C(49)-C(21) 111.3(3)C(50)-C(49)-H(49) 107.7C(50)-C(49)-C(51) 112.4(3)C(51)-C(49)-C(21) 109.7(3)C(51)-C(49)-H(49) 107.7C(49)-C(50)-H(50A) 109.5C(49)-C(50)-H(50B) 109.5C(49)-C(50)-H(50C) 109.5H(50A)-C(50)-H(50B) 109.5H(50A)-C(50)-H(50C) 109.5H(50B)-C(50)-H(50C) 109.5C(49)-C(51)-H(51A) 109.5C(49)-C(51)-H(51B) 109.5C(49)-C(51)-H(51C) 109.5H(51A)-C(51)-H(51B) 109.5H(51A)-C(51)-H(51C) 109.5H(51B)-C(51)-H(51C) 109.5C(19)-C(48)-H(48A) 109.5C(19)-C(48)-H(48B) 109.5C(19)-C(48)-H(48C) 109.5H(48A)-C(48)-H(48B) 109.5H(48A)-C(48)-H(48C) 109.5H(48B)-C(48)-H(48C) 109.5C(17)-C(45)-H(45) 108.5C(17)-C(45)-C(47) 110.8(2)C(47)-C(45)-H(45) 108.5C(46)-C(45)-C(17) 110.9(2)C(46)-C(45)-H(45) 108.5C(46)-C(45)-C(47) 109.5(3)C(45)-C(47)-H(47A) 109.5C(45)-C(47)-H(47B) 109.5C(45)-C(47)-H(47C) 109.5H(47A)-C(47)-H(47B) 109.5
S31
H(47A)-C(47)-H(47C) 109.5H(47B)-C(47)-H(47C) 109.5C(45)-C(46)-H(46A) 109.5C(45)-C(46)-H(46B) 109.5C(45)-C(46)-H(46C) 109.5H(46A)-C(46)-H(46B) 109.5H(46A)-C(46)-H(46C) 109.5H(46B)-C(46)-H(46C) 109.5C(15)-C(42)-H(42) 107.4C(43)-C(42)-C(15) 109.9(3)C(43)-C(42)-H(42) 107.4C(43)-C(42)-C(44) 112.3(3)C(44)-C(42)-C(15) 112.2(3)C(44)-C(42)-H(42) 107.4C(42)-C(44)-H(44A) 109.5C(42)-C(44)-H(44B) 109.5C(42)-C(44)-H(44C) 109.5H(44A)-C(44)-H(44B) 109.5H(44A)-C(44)-H(44C) 109.5H(44B)-C(44)-H(44C) 109.5C(13)-C(39)-H(39) 108.0C(41)-C(39)-C(13) 110.3(2)C(41)-C(39)-H(39) 108.0C(40)-C(39)-C(13) 111.7(2)C(40)-C(39)-H(39) 108.0C(40)-C(39)-C(41) 110.7(3)C(39)-C(41)-H(41A) 109.5C(39)-C(41)-H(41B) 109.5C(39)-C(41)-H(41C) 109.5H(41A)-C(41)-H(41B) 109.5H(41A)-C(41)-H(41C) 109.5H(41B)-C(41)-H(41C) 109.5C(39)-C(40)-H(40A) 109.5C(39)-C(40)-H(40B) 109.5C(39)-C(40)-H(40C) 109.5H(40A)-C(40)-H(40B) 109.5H(40A)-C(40)-H(40C) 109.5H(40B)-C(40)-H(40C) 109.5C(11)-C(38)-H(38A) 109.5C(11)-C(38)-H(38B) 109.5C(11)-C(38)-H(38C) 109.5H(38A)-C(38)-H(38B) 109.5H(38A)-C(38)-H(38C) 109.5H(38B)-C(38)-H(38C) 109.5C(9)-C(35)-H(35) 107.7C(36)-C(35)-C(9) 111.6(3)C(36)-C(35)-H(35) 107.7C(36)-C(35)-C(37) 112.2(3)C(37)-C(35)-C(9) 109.8(3)C(37)-C(35)-H(35) 107.7C(35)-C(36)-H(36A) 109.5C(35)-C(36)-H(36B) 109.5C(35)-C(36)-H(36C) 109.5H(36A)-C(36)-H(36B) 109.5H(36A)-C(36)-H(36C) 109.5H(36B)-C(36)-H(36C) 109.5C(35)-C(37)-H(37A) 109.5C(35)-C(37)-H(37B) 109.5C(35)-C(37)-H(37C) 109.5
H(37A)-C(37)-H(37B) 109.5H(37A)-C(37)-H(37C) 109.5H(37B)-C(37)-H(37C) 109.5C(7)-C(32)-H(32) 108.2C(7)-C(32)-C(33) 110.1(2)C(7)-C(32)-C(34) 111.1(2)C(33)-C(32)-H(32) 108.2C(34)-C(32)-H(32) 108.2C(34)-C(32)-C(33) 111.0(3)C(32)-C(33)-H(33A) 109.5C(32)-C(33)-H(33B) 109.5C(32)-C(33)-H(33C) 109.5H(33A)-C(33)-H(33B) 109.5H(33A)-C(33)-H(33C) 109.5H(33B)-C(33)-H(33C) 109.5C(32)-C(34)-H(34A) 109.5C(32)-C(34)-H(34B) 109.5C(32)-C(34)-H(34C) 109.5H(34A)-C(34)-H(34B) 109.5H(34A)-C(34)-H(34C) 109.5H(34B)-C(34)-H(34C) 109.5C(5)-C(29)-H(29) 107.0C(30)-C(29)-C(5) 112.7(3)C(30)-C(29)-H(29) 107.0C(31)-C(29)-C(5) 110.9(3)C(31)-C(29)-H(29) 107.0C(31)-C(29)-C(30) 112.0(3)C(29)-C(30)-H(30A) 109.5C(29)-C(30)-H(30B) 109.5C(29)-C(30)-H(30C) 109.5H(30A)-C(30)-H(30B) 109.5H(30A)-C(30)-H(30C) 109.5H(30B)-C(30)-H(30C) 109.5C(29)-C(31)-H(31A) 109.5C(29)-C(31)-H(31B) 109.5C(29)-C(31)-H(31C) 109.5H(31A)-C(31)-H(31B) 109.5H(31A)-C(31)-H(31C) 109.5H(31B)-C(31)-H(31C) 109.5C(1)-C(25)-H(25) 108.2C(26)-C(25)-C(1) 111.7(2)C(26)-C(25)-H(25) 108.2C(26)-C(25)-C(27) 110.6(3)C(27)-C(25)-C(1) 109.9(2)C(27)-C(25)-H(25) 108.2C(25)-C(26)-H(26A) 109.5C(25)-C(26)-H(26B) 109.5C(25)-C(26)-H(26C) 109.5H(26A)-C(26)-H(26B) 109.5H(26A)-C(26)-H(26C) 109.5H(26B)-C(26)-H(26C) 109.5C(25)-C(27)-H(27A) 109.5C(25)-C(27)-H(27B) 109.5C(25)-C(27)-H(27C) 109.5H(27A)-C(27)-H(27B) 109.5H(27A)-C(27)-H(27C) 109.5H(27B)-C(27)-H(27C) 109.5F(1)-C(55)-S(2) 111.1(2)F(3)-C(55)-S(2) 110.9(2)
F(3)-C(55)-F(1) 107.9(3)F(3)-C(55)-F(2) 108.0(3)F(2)-C(55)-S(2) 111.0(2)F(2)-C(55)-F(1) 107.7(3)F(4)-C(56)-S(1) 111.1(2)F(6)-C(56)-S(1) 110.6(3)F(6)-C(56)-F(4) 107.8(3)F(5)-C(56)-S(1) 110.8(3)F(5)-C(56)-F(4) 108.5(3)F(5)-C(56)-F(6) 108.0(3)O(27)-S(3)-O(28)113.41(18)O(27)-S(3)-C(57)103.85(15)O(28)-S(3)-C(57)102.57(17)O(29)-S(3)-O(27) 115.0(2)O(29)-S(3)-O(28) 116.9(2)O(29)-S(3)-C(57)102.60(17)F(7)-C(57)-S(3) 110.8(2)F(7)-C(57)-F(8) 106.5(3)F(7)-C(57)-F(9) 108.1(3)F(8)-C(57)-S(3) 112.2(2)F(8)-C(57)-F(9) 108.0(3)F(9)-C(57)-S(3) 111.1(2)O(30)-S(4)-O(32) 114.5(2)O(30)-S(4)-C(58) 103.7(2)O(31)-S(4)-O(30) 115.2(2)O(31)-S(4)-O(32)114.77(19)O(31)-S(4)-C(58) 104.0(2)O(32)-S(4)-C(58)102.38(18)F(10)-C(58)-S(4) 111.0(3)F(11)-C(58)-S(4) 111.8(3)F(11)-C(58)-F(10) 107.0(4)F(12)-C(58)-S(4) 111.5(3)F(12)-C(58)-F(10) 105.6(4)F(12)-C(58)-F(11) 109.7(4)C(59)-O(33)-C(62) 105.5(3)O(33)-C(59)-H(59A) 110.5O(33)-C(59)-H(59B) 110.5O(33)-C(59)-C(60) 106.3(3)H(59A)-C(59)-H(59B) 108.7C(60)-C(59)-H(59A) 110.5C(60)-C(59)-H(59B) 110.5C(59)-C(60)-H(60A) 110.8C(59)-C(60)-H(60B) 110.8C(59)-C(60)-C(61) 104.9(3)H(60A)-C(60)-H(60B) 108.9C(61)-C(60)-H(60A) 110.8C(61)-C(60)-H(60B) 110.8C(60)-C(61)-H(61A) 111.0C(60)-C(61)-H(61B) 111.0H(61A)-C(61)-H(61B) 109.0C(62)-C(61)-C(60) 103.6(3)C(62)-C(61)-H(61A) 111.0C(62)-C(61)-H(61B) 111.0O(33)-C(62)-C(61) 105.3(3)O(33)-C(62)-H(62A) 110.7O(33)-C(62)-H(62B) 110.7C(61)-C(62)-H(62A) 110.7C(61)-C(62)-H(62B) 110.7H(62A)-C(62)-H(62B) 108.8
S32
C(63)-O(34)-C(66) 109.5(3)O(34)-C(63)-H(63A) 110.5O(34)-C(63)-H(63B) 110.5O(34)-C(63)-C(64) 106.3(3)H(63A)-C(63)-H(63B) 108.7C(64)-C(63)-H(63A) 110.5C(64)-C(63)-H(63B) 110.5C(63)-C(64)-H(64A) 111.2C(63)-C(64)-H(64B) 111.2C(63)-C(64)-C(65) 102.7(3)H(64A)-C(64)-H(64B) 109.1C(65)-C(64)-H(64A) 111.2C(65)-C(64)-H(64B) 111.2C(64)-C(65)-H(65A) 111.6C(64)-C(65)-H(65B) 111.6H(65A)-C(65)-H(65B) 109.4C(66)-C(65)-C(64) 100.9(3)C(66)-C(65)-H(65A) 111.6C(66)-C(65)-H(65B) 111.6O(34)-C(66)-C(65) 105.4(3)O(34)-C(66)-H(66A) 110.7O(34)-C(66)-H(66B) 110.7C(65)-C(66)-H(66A) 110.7C(65)-C(66)-H(66B) 110.7H(66A)-C(66)-H(66B) 108.8C(70)-O(35)-C(67) 108.5(3)O(35)-C(67)-H(67A) 110.3O(35)-C(67)-H(67B) 110.3O(35)-C(67)-C(68) 107.3(3)H(67A)-C(67)-H(67B) 108.5C(68)-C(67)-H(67A) 110.3C(68)-C(67)-H(67B) 110.3C(67)-C(68)-H(68A) 111.0C(67)-C(68)-H(68B) 111.0
C(67)-C(68)-C(69) 103.9(3)H(68A)-C(68)-H(68B) 109.0C(69)-C(68)-H(68A) 111.0C(69)-C(68)-H(68B) 111.0C(68)-C(69)-H(69A) 111.2C(68)-C(69)-H(69B) 111.2C(68)-C(69)-C(70) 102.6(3)H(69A)-C(69)-H(69B) 109.2C(70)-C(69)-H(69A) 111.2C(70)-C(69)-H(69B) 111.2O(35)-C(70)-C(69) 105.3(3)O(35)-C(70)-H(70A) 110.7O(35)-C(70)-H(70B) 110.7C(69)-C(70)-H(70A) 110.7C(69)-C(70)-H(70B) 110.7H(70A)-C(70)-H(70B) 108.8C(71)-O(36)-C(74) 105.9(3)O(36)-C(71)-H(71A) 110.2O(36)-C(71)-H(71B) 110.2O(36)-C(71)-C(72) 107.4(3)H(71A)-C(71)-H(71B) 108.5C(72)-C(71)-H(71A) 110.2C(72)-C(71)-H(71B) 110.2C(71)-C(72)-H(72A) 110.9C(71)-C(72)-H(72B) 110.9H(72A)-C(72)-H(72B) 108.9C(73)-C(72)-C(71) 104.2(3)C(73)-C(72)-H(72A) 110.9C(73)-C(72)-H(72B) 110.9C(72)-C(73)-H(73A) 111.1C(72)-C(73)-H(73B) 111.1C(72)-C(73)-C(74) 103.1(3)H(73A)-C(73)-H(73B) 109.1C(74)-C(73)-H(73A) 111.1
C(74)-C(73)-H(73B) 111.1O(36)-C(74)-C(73) 104.6(2)O(36)-C(74)-H(74A) 110.8O(36)-C(74)-H(74B) 110.8C(73)-C(74)-H(74A) 110.8C(73)-C(74)-H(74B) 110.8H(74A)-C(74)-H(74B) 108.9C(78)-O(37)-C(75) 108.6(3)O(37)-C(75)-H(75A) 110.8O(37)-C(75)-H(75B) 110.8O(37)-C(75)-C(76) 104.5(3)H(75A)-C(75)-H(75B) 108.9C(76)-C(75)-H(75A) 110.8C(76)-C(75)-H(75B) 110.8C(75)-C(76)-H(76A) 111.6C(75)-C(76)-H(76B) 111.6C(75)-C(76)-C(77) 100.8(3)H(76A)-C(76)-H(76B) 109.4C(77)-C(76)-H(76A) 111.6C(77)-C(76)-H(76B) 111.6C(76)-C(77)-H(77A) 111.2C(76)-C(77)-H(77B) 111.2C(76)-C(77)-C(78) 103.0(4)H(77A)-C(77)-H(77B) 109.1C(78)-C(77)-H(77A) 111.2C(78)-C(77)-H(77B) 111.2O(37)-C(78)-C(77) 108.3(4)O(37)-C(78)-H(78A) 110.0O(37)-C(78)-H(78B) 110.0C(77)-C(78)-H(78A) 110.0C(77)-C(78)-H(78B) 110.0H(78A)-C(78)-H(78B) 108.4H(4WA)-O(4W)-H(4WB)106(2)H(3WA)-O(3W)-H(3WB)110(2)
_____________________________________________________________
Table 9. Anisotropic displacement parameters (Å2x 103) for Sample B. The anisotropicdisplacement factor exponent takes the form: -22[ h2 a*2U11 + ... + 2 h k a* b* U12 ]______________________________________________________________________________
U11 U22 U33 U23 U13 U12______________________________________________________________________________ Ca(1) 14(1) 14(1) 13(1) 2(1) 3(1) 2(1)Ca(2) 12(1) 13(1) 13(1) 2(1) 2(1) 2(1)S(1) 15(1) 17(1) 19(1) 5(1) 5(1) 4(1)S(2) 15(1) 15(1) 16(1) 3(1) 5(1) 3(1)F(1) 32(1) 55(2) 44(1) 27(1) 0(1) 14(1)F(3) 31(1) 43(1) 29(1) -13(1) 3(1) -1(1)F(2) 16(1) 44(1) 42(1) 5(1) 10(1) 0(1)F(4) 19(1) 64(2) 47(1) 17(1) 10(1) 16(1)F(6) 48(2) 98(2) 74(2) 67(2) 26(1) 42(2)F(5) 28(1) 96(2) 33(1) -14(1) -3(1) 3(1)O(7) 20(1) 21(1) 12(1) 4(1) 5(1) 8(1)O(12) 21(1) 25(1) 25(1) 10(1) 9(1) 9(1)O(1W) 26(1) 21(1) 34(1) 1(1) 14(1) 9(1)O(21) 18(1) 23(1) 26(1) 5(1) 10(1) 6(1)O(2W) 25(1) 25(1) 30(1) 4(1) 14(1) 8(1)O(20) 35(1) 22(1) 36(1) 16(1) 16(1) 11(1)O(1) 16(1) 17(1) 21(1) 1(1) 2(1) 2(1)
S33
O(10) 21(1) 18(1) 24(1) 5(1) 9(1) 5(1)O(11) 17(1) 21(1) 15(1) 1(1) 2(1) 2(1)O(2) 16(1) 20(1) 19(1) 9(1) 5(1) 1(1)O(9) 18(1) 18(1) 21(1) 7(1) 4(1) 0(1)O(13) 16(1) 25(1) 16(1) 0(1) 2(1) 1(1)O(3) 17(1) 18(1) 13(1) 4(1) 5(1) 6(1)O(14) 24(1) 19(1) 19(1) 2(1) 6(1) 7(1)O(15) 17(1) 15(1) 22(1) 6(1) 3(1) 1(1)O(4) 15(1) 14(1) 18(1) 1(1) 3(1) 2(1)O(8) 23(1) 21(1) 20(1) 1(1) 5(1) 7(1)O(17) 19(1) 17(1) 16(1) 2(1) 1(1) 3(1)O(6) 16(1) 16(1) 18(1) 7(1) 5(1) 3(1)O(18) 22(1) 29(1) 29(1) 13(1) 10(1) 11(1)O(19) 18(1) 26(1) 15(1) 0(1) 1(1) 1(1)O(16) 21(1) 24(1) 24(1) 0(1) 9(1) 2(1)O(23) 17(1) 21(1) 22(1) 5(1) 8(1) 4(1)O(22) 31(1) 24(1) 38(1) -3(1) 19(1) 2(1)O(24) 26(1) 22(1) 33(1) 13(1) 7(1) 5(1)O(25) 33(1) 24(1) 27(1) -3(1) 12(1) 8(1)N(1) 18(1) 16(1) 18(1) 7(1) 3(1) 2(1)N(2) 15(1) 16(1) 16(1) 2(1) 3(1) 1(1)N(3) 14(1) 19(1) 14(1) 2(1) 4(1) -2(1)N(4) 15(1) 16(1) 17(1) 7(1) 4(1) 3(1)N(5) 16(1) 13(1) 16(1) 2(1) 0(1) 1(1)N(6) 13(1) 20(1) 13(1) 1(1) 3(1) 2(1)C(15) 15(1) 11(1) 18(1) 3(1) 3(1) 0(1)C(5) 15(1) 17(1) 21(1) 3(1) 5(1) 4(1)C(20) 17(1) 13(1) 16(1) 1(1) 4(1) 3(1)C(43) 31(2) 18(1) 39(2) 4(1) 6(1) 12(1)C(4) 16(1) 15(1) 19(1) 5(1) 3(1) 6(1)C(3) 17(1) 18(1) 24(1) 4(1) 2(1) 2(1)C(28) 29(2) 19(2) 51(2) -7(2) 2(2) 5(1)C(2) 19(1) 16(1) 15(1) 2(1) 4(1) 1(1)C(1) 16(1) 14(1) 15(1) 4(1) 5(1) 1(1)C(6) 13(1) 16(1) 16(1) 2(1) 6(1) 1(1)C(7) 15(1) 15(1) 13(1) 3(1) 3(1) 0(1)C(8) 18(1) 13(1) 15(1) 1(1) 6(1) 1(1)C(9) 16(1) 19(1) 14(1) 4(1) 4(1) 1(1)C(10) 15(1) 15(1) 14(1) 3(1) 2(1) 3(1)C(11) 14(1) 20(1) 13(1) 4(1) 3(1) 3(1)C(12) 13(1) 18(1) 16(1) 3(1) 3(1) 2(1)C(13) 14(1) 14(1) 16(1) 4(1) 3(1) 3(1)C(14) 15(1) 14(1) 14(1) 0(1) 2(1) 3(1)C(24) 14(1) 18(1) 17(1) 4(1) 4(1) 1(1)C(16) 16(1) 13(1) 18(1) 2(1) 2(1) 2(1)C(17) 15(1) 14(1) 16(1) 3(1) 3(1) 4(1)C(18) 13(1) 14(1) 15(1) 3(1) 4(1) 2(1)C(19) 18(1) 14(1) 15(1) 4(1) 4(1) 2(1)C(21) 13(1) 17(1) 17(1) 4(1) 4(1) 2(1)C(22) 17(1) 13(1) 15(1) 4(1) 5(1) 4(1)C(23) 15(1) 20(1) 12(1) 4(1) 3(1) 5(1)C(52) 26(1) 28(2) 17(1) 7(1) 7(1) 14(1)C(54) 28(2) 62(3) 31(2) 16(2) 14(1) 25(2)C(53) 52(2) 28(2) 25(2) 6(1) 6(2) 23(2)C(49) 21(1) 16(1) 25(2) 6(1) 9(1) 6(1)C(50) 41(2) 20(2) 26(2) 2(1) 14(1) 7(1)C(51) 29(2) 21(2) 37(2) 16(1) 13(1) 9(1)C(48) 23(1) 20(1) 21(1) 5(1) 11(1) 5(1)C(45) 17(1) 20(1) 22(1) 7(1) 1(1) 7(1)
S34
C(47) 16(1) 29(2) 39(2) 12(1) -2(1) 4(1)C(46) 31(2) 20(1) 41(2) 9(1) -7(1) 7(1)C(42) 18(1) 14(1) 25(1) -1(1) 3(1) 3(1)C(44) 38(2) 29(2) 24(2) -2(1) 8(1) 9(1)C(39) 15(1) 16(1) 23(1) 6(1) 6(1) 1(1)C(41) 25(1) 24(2) 28(2) 9(1) 13(1) 5(1)C(40) 16(1) 26(2) 36(2) 13(1) 6(1) 4(1)C(38) 24(1) 30(2) 22(1) 11(1) 6(1) 13(1)C(35) 23(1) 17(1) 27(2) 9(1) 12(1) 5(1)C(36) 38(2) 18(1) 25(2) 0(1) 8(1) 5(1)C(37) 32(2) 27(2) 32(2) 16(1) 11(1) 6(1)C(32) 18(1) 18(1) 17(1) 3(1) 6(1) 3(1)C(33) 27(1) 26(2) 27(2) 10(1) 16(1) 7(1)C(34) 33(2) 23(2) 40(2) 5(1) 18(1) 10(1)C(29) 19(1) 23(1) 35(2) 6(1) -1(1) 7(1)C(30) 34(2) 27(2) 28(2) 10(1) -4(1) 7(1)C(31) 30(2) 34(2) 50(2) 8(2) 9(2) 18(2)C(25) 17(1) 16(1) 22(1) 6(1) 6(1) 1(1)C(26) 18(1) 21(1) 29(2) 7(1) 6(1) 0(1)C(27) 25(2) 34(2) 25(2) 11(1) 13(1) 4(1)C(55) 16(1) 32(2) 24(1) 4(1) 4(1) 4(1)C(56) 17(1) 58(2) 30(2) 17(2) 6(1) 12(2)S(3) 22(1) 20(1) 20(1) 1(1) 8(1) 0(1)F(7) 53(2) 50(2) 43(1) 6(1) 26(1) 27(1)F(8) 44(1) 60(2) 21(1) 7(1) -2(1) 1(1)F(9) 65(2) 37(1) 45(1) 14(1) 33(1) -1(1)O(27) 34(1) 25(1) 24(1) 12(1) 8(1) 4(1)O(28) 62(2) 37(2) 54(2) 18(1) 36(2) 26(2)O(29) 29(1) 90(3) 24(1) -10(2) -2(1) -24(2)C(57) 27(2) 30(2) 20(1) 7(1) 7(1) 2(1)S(4) 22(1) 20(1) 21(1) 8(1) 7(1) 6(1)F(10) 99(2) 52(2) 56(2) 3(1) 44(2) 34(2)F(11) 91(2) 70(2) 25(1) 18(1) 12(1) 22(2)F(12) 72(2) 71(2) 69(2) -27(2) 4(2) -29(2)O(30) 92(3) 42(2) 62(2) 39(2) 51(2) 38(2)O(31) 35(1) 40(2) 47(2) 12(1) 12(1) 20(1)O(32) 24(1) 53(2) 32(1) -5(1) -1(1) -2(1)C(58) 43(2) 36(2) 28(2) -6(2) 6(2) -1(2)O(33) 23(1) 29(1) 25(1) 0(1) 3(1) 3(1)C(59) 25(2) 41(2) 26(2) 4(1) 9(1) 8(1)C(60) 33(2) 36(2) 27(2) -2(1) 8(1) -6(2)C(61) 34(2) 32(2) 33(2) -5(1) 11(1) 1(1)C(62) 29(2) 36(2) 26(2) 6(1) 11(1) 6(1)O(34) 25(1) 36(1) 39(1) -5(1) 13(1) 8(1)C(63) 27(2) 23(2) 35(2) 4(1) 9(1) 7(1)C(64) 26(2) 24(2) 34(2) 9(1) 12(1) 10(1)C(65) 34(2) 32(2) 32(2) 1(1) 16(2) 9(2)C(66) 29(2) 40(2) 31(2) -2(2) 12(1) 7(1)O(35) 30(1) 32(1) 43(2) 12(1) 19(1) 15(1)C(67) 27(2) 40(2) 28(2) 9(1) 11(1) 8(1)C(68) 39(2) 49(3) 40(2) -13(2) -3(2) 23(2)C(69) 22(2) 49(2) 58(3) -3(2) 9(2) 12(2)C(70) 34(2) 29(2) 47(2) -2(2) 1(2) 11(2)O(36) 21(1) 23(1) 20(1) 2(1) 6(1) 4(1)C(71) 22(2) 37(2) 41(2) 11(2) 11(1) 8(1)C(72) 31(2) 34(2) 29(2) 2(1) 8(1) -5(1)C(73) 32(2) 21(1) 25(2) -1(1) 4(1) 2(1)C(74) 28(2) 27(2) 24(2) 3(1) 11(1) 7(1)O(37) 38(1) 30(1) 32(1) 7(1) 11(1) 6(1)
S35
C(75) 35(2) 25(2) 31(2) 7(1) 7(1) 8(1)C(76) 40(2) 36(2) 31(2) 10(2) 6(2) 6(2)C(77) 87(4) 49(3) 73(3) 38(3) 51(3) 41(3)C(78) 121(5) 58(3) 74(4) 38(3) 57(4) 59(4)O(4W) 31(1) 27(1) 32(1) 10(1) 11(1) 12(1)O(3W) 46(2) 25(1) 47(2) 5(1) 29(1) 10(1)________________________________________________________________________________________________________________________________________________________________________________________________________
Table 10. Hydrogen coordinates ( x 104) and isotropic displacement parameters (Å2x 10 3)for Sample B.________________________________________________________________________________________________________________________________________________________________________________________________________
x y z U(eq)________________________________________________________________________________________________________________________________________________________________________________________________________
H(4) -123 -2955 12138 19H(6) 6939 3859 12116 19H(15) 1740 -2743 12835 18H(5A) 1818 2825 7501 21H(43A) 3255 -3800 12235 44H(43B) 2475 -4819 11661 44H(43C) 2293 -4357 12576 44H(3A) 4550 5043 7284 24H(28A) 3901 6076 8327 54H(28B) 5161 6257 8615 54H(28C) 4414 5565 9059 54H(1A) 7156 3651 8285 18H(7) 1803 -179 6129 18H(9) 1702 -980 8661 20H(11) -1567 -1923 8983 19H(13) -803 -1360 11767 18H(17) 4665 -791 12711 18H(19) 4793 2327 13912 19H(21) 4776 3113 11366 19H(23) 7960 4396 11072 19H(52) 8367 2989 11612 27H(54A) 9453 3366 10285 54H(54B) 9920 2962 11105 54H(54C) 9742 4073 11223 54H(53A) 7109 1680 10531 50H(53B) 8257 1449 10724 50H(53C) 7861 1844 9880 50H(49) 4300 4373 12295 23H(50A) 5752 4721 13503 42H(50B) 5584 5745 13247 42H(50C) 6521 5278 12992 42H(51A) 5755 5280 11378 40H(51B) 4822 5740 11650 40H(51C) 4546 4714 10949 40H(48A) 3164 2911 13895 31H(48B) 3113 1894 14230 31H(48C) 2519 1866 13269 31H(45) 4967 -864 14517 23H(47A) 6562 -710 13518 43H(47B) 6791 -794 14501 43H(47C) 6482 184 14244 43H(46A) 4239 -2516 13684 49H(46B) 5450 -2429 14127 49H(46C) 5121 -2393 13136 49H(42) 1049 -3997 11508 24H(44A) 1524 -3068 10497 47
S36
H(44B) 1988 -4044 10389 47H(44C) 2754 -2979 10875 47H(39) -1958 -3457 11276 22H(41A) -1531 -2849 12780 37H(41B) -2785 -3039 12441 37H(41C) -2055 -1925 12675 37H(40A) -2894 -1791 11079 38H(40B) -3575 -2907 10969 38H(40C) -2856 -2657 10310 38H(38A) -2367 -545 9251 35H(38B) -1694 -378 8547 35H(38C) -1229 223 9520 35H(35) 2081 -2261 7684 25H(36A) -164 -3092 7047 42H(36B) 727 -3601 6752 42H(36C) 592 -2561 6514 42H(37A) 1929 -2640 9022 43H(37B) 1497 -3655 8304 43H(37C) 681 -3097 8674 43H(32) 4020 150 6989 21H(33A) 3244 343 5255 37H(33B) 4468 533 5718 37H(33C) 3781 1278 6041 37H(34A) 3236 -1592 6504 46H(34B) 4068 -1269 5948 46H(34C) 2826 -1444 5554 46H(29) 399 2605 6254 31H(30A) 1884 3674 5446 46H(30B) 648 3210 5036 46H(30C) 1434 2486 5171 46H(31A) 786 4083 7338 55H(31B) 357 4314 6422 55H(31C) 1597 4646 6862 55H(25) 8269 5748 8637 22H(26A) 9235 5046 9660 35H(26B) 9915 5249 8966 35H(26C) 9269 4138 8927 35H(27A) 8352 4106 7320 40H(27B) 9032 5228 7455 40H(27C) 7769 4978 7149 40H(59A) -1118 17 14676 37H(59B) -551 35 15647 37H(60A) -1140 -1629 14394 42H(60B) -292 -1518 15278 42H(61A) 1065 -1379 14601 42H(61B) 196 -1653 13703 42H(62A) 1498 119 14199 36H(62B) 314 -6 13650 36H(63A) -1943 -155 12611 34H(63B) -2107 200 11715 34H(64A) -2899 998 12950 32H(64B) -2497 1662 12303 32H(65A) -1412 2619 13630 39H(65B) -1282 1632 13992 39H(66A) -290 2384 12717 40H(66B) 268 1972 13507 40H(67A) 6580 869 6120 37H(67B) 6242 249 6810 37H(68A) 7839 6 6098 55
S37
H(68B) 7748 -283 7003 55H(69A) 8984 1544 6748 53H(69B) 9334 914 7451 53H(70A) 8309 1508 8331 46H(70B) 8662 2480 7950 46H(71A) 7141 2133 4403 39H(71B) 7629 2258 5409 39H(72A) 7874 3943 5571 40H(72B) 7292 3810 4580 40H(73A) 5701 3883 4906 33H(73B) 6387 4379 5870 33H(74A) 6121 2848 6290 31H(74B) 5000 2698 5629 31H(75A) 3752 4176 5233 36H(75B) 4661 5198 5595 36H(76A) 2775 4881 4236 43H(76B) 3975 5382 4208 43H(77A) 2746 6559 4672 71H(77B) 3998 6886 5106 71H(78A) 3566 6726 6376 85H(78B) 2357 6184 5903 85H(1) 6400(30) 5270(20) 7860(20) 22(5)H(5) 5030(30) 810(30) 14074(19) 22(5)H(2) 1470(30) 1370(30) 6029(18) 22(9)H(3) -540(20) -1730(30) 7950(20) 22(5)H(2WA) 6170(40) 1580(30) 8030(40) 80(20)H(2WB) 5720(40) 592(15) 8320(30) 43(13)H(3WA) 5720(30) -1210(30) 7640(20) 39(12)H(3WB) 4990(30) -1150(30) 8310(30) 48(14)H(1WA) 450(30) 850(30) 12010(30) 51(15)H(4WA) 1210(40) 3570(40) 12610(30) 62(17)H(4WB) 1910(50) 3500(50) 11920(30) 93H(1WB) 1230(50) 1826(11) 11920(40) 93________________________________________________________________________________
Table 11. Torsion angles [°] for Sample B.________________________________________________________________ Ca(1)-O(11)-C(6)-N(2) -139.1(6)Ca(1)-O(11)-C(6)-C(7) 39.3(9)Ca(1)-O(19)-C(22)-N(6) -172.9(11)Ca(1)-O(19)-C(22)-C(23) 6.0(14)Ca(2)-O(13)-C(10)-N(3) -153.6(10)Ca(2)-O(13)-C(10)-C(11) 29.2(13)Ca(2)-O(15)-C(14)-N(4) -159.3(10)Ca(2)-O(15)-C(14)-C(15) 18.0(13)Ca(2)-O(17)-C(18)-N(5) 141.3(5)Ca(2)-O(17)-C(18)-C(19) -34.6(7)O(7)-C(23)-C(52)-C(54) 64.1(3)O(7)-C(23)-C(52)-C(53) -61.3(3)O(12)-C(8)-C(9)-N(3) -8.2(4)O(12)-C(8)-C(9)-C(35) 116.9(3)O(21)-S(1)-C(56)-F(4) 173.2(3)O(21)-S(1)-C(56)-F(6) 53.5(3)O(21)-S(1)-C(56)-F(5) -66.2(3)O(20)-S(1)-O(21)-Ca(2) -17.5(4)O(20)-S(1)-C(56)-F(4) -67.6(3)O(20)-S(1)-C(56)-F(6) 172.7(3)O(20)-S(1)-C(56)-F(5) 53.0(3)O(1)-C(3)-C(2)-O(9) -19.3(4)
O(1)-C(3)-C(2)-N(1) 165.2(3)O(11)-C(6)-C(7)-O(2) 50.3(3)O(11)-C(6)-C(7)-C(32) -66.1(3)O(2)-C(7)-C(32)-C(33) -176.0(2)O(2)-C(7)-C(32)-C(34) 60.6(3)O(2)-C(8)-C(9)-N(3) 173.5(2)O(2)-C(8)-C(9)-C(35) -61.4(3)O(13)-C(10)-C(11)-O(3) -26.2(4)O(13)-C(10)-C(11)-C(38) 91.2(3)O(3)-C(12)-C(13)-N(4) -142.6(2)O(3)-C(12)-C(13)-C(39) 97.3(3)O(14)-C(12)-C(13)-N(4) 39.9(4)O(14)-C(12)-C(13)-C(39) -80.3(3)O(4)-C(15)-C(14)-O(15) 13.7(4)O(4)-C(15)-C(14)-N(4) -168.9(2)O(4)-C(15)-C(42)-C(43) 67.0(3)O(4)-C(15)-C(42)-C(44) -58.6(3)O(4)-C(16)-C(17)-N(5) 140.7(2)O(4)-C(16)-C(17)-C(45) -97.9(3)O(17)-C(18)-C(19)-O(6) -42.8(4)O(17)-C(18)-C(19)-C(48) 75.7(3)O(6)-C(20)-C(21)-N(6) -177.6(2)
S38
O(6)-C(20)-C(21)-C(49) 57.5(3)O(18)-C(20)-C(21)-N(6) 3.0(4)O(18)-C(20)-C(21)-C(49) -121.9(3)O(19)-C(22)-C(23)-O(7) 18.1(4)O(19)-C(22)-C(23)-C(52) -101.1(3)O(16)-C(16)-C(17)-N(5) -42.1(4)O(16)-C(16)-C(17)-C(45) 79.3(4)O(23)-S(2)-O(24)-Ca(2) -145.6(5)O(23)-S(2)-C(55)-F(1) -62.9(3)O(23)-S(2)-C(55)-F(3) 57.2(3)O(23)-S(2)-C(55)-F(2) 177.2(2)O(22)-S(1)-O(21)-Ca(2) -153.3(3)O(22)-S(1)-C(56)-F(4) 53.5(3)O(22)-S(1)-C(56)-F(6) -66.2(3)O(22)-S(1)-C(56)-F(5) 174.2(3)O(24)-S(2)-O(23)-Ca(1) 18.1(3)O(24)-S(2)-C(55)-F(1) 178.5(2)O(24)-S(2)-C(55)-F(3) -61.4(3)O(24)-S(2)-C(55)-F(2) 58.7(3)O(25)-S(2)-O(23)-Ca(1) 153.4(2)O(25)-S(2)-O(24)-Ca(2) 79.4(6)O(25)-S(2)-C(55)-F(1) 57.2(3)O(25)-S(2)-C(55)-F(3) 177.3(2)O(25)-S(2)-C(55)-F(2) -62.6(3)N(1)-C(1)-C(24)-O(7) 145.1(2)N(1)-C(1)-C(24)-O(8) -37.5(4)N(1)-C(1)-C(25)-C(26) 168.5(3)N(1)-C(1)-C(25)-C(27) -68.4(3)N(2)-C(5)-C(4)-O(1) -147.6(2)N(2)-C(5)-C(4)-O(10) 32.3(4)N(2)-C(5)-C(29)-C(30) -67.8(3)N(2)-C(5)-C(29)-C(31) 165.7(3)N(2)-C(6)-C(7)-O(2) -131.2(3)N(2)-C(6)-C(7)-C(32) 112.4(3)N(3)-C(9)-C(35)-C(36) 65.0(3)N(3)-C(9)-C(35)-C(37) -60.0(3)N(3)-C(10)-C(11)-O(3) 156.4(2)N(3)-C(10)-C(11)-C(38) -86.2(3)N(4)-C(13)-C(39)-C(41) 67.2(3)N(4)-C(13)-C(39)-C(40) -169.2(3)N(5)-C(17)-C(45)-C(47) -62.2(3)N(5)-C(17)-C(45)-C(46) 176.0(3)N(5)-C(18)-C(19)-O(6) 141.1(2)N(5)-C(18)-C(19)-C(48) -100.5(3)N(6)-C(21)-C(49)-C(50) -65.5(3)N(6)-C(21)-C(49)-C(51) 59.6(3)N(6)-C(22)-C(23)-O(7) -162.9(2)N(6)-C(22)-C(23)-C(52) 77.8(3)C(15)-O(4)-C(16)-O(16) -3.2(4)C(15)-O(4)-C(16)-C(17) 174.0(2)C(5)-N(2)-C(6)-O(11) 0.1(4)C(5)-N(2)-C(6)-C(7) -178.3(2)C(20)-O(6)-C(19)-C(18) -76.5(3)C(20)-O(6)-C(19)-C(48) 164.0(2)C(20)-C(21)-C(49)-C(50) 58.4(3)C(20)-C(21)-C(49)-C(51) -176.6(2)C(4)-O(1)-C(3)-C(28) 171.1(3)C(4)-O(1)-C(3)-C(2) -69.6(3)C(4)-C(5)-C(29)-C(30) 54.9(4)
C(4)-C(5)-C(29)-C(31) -71.5(4)C(3)-O(1)-C(4)-O(10) 1.6(4)C(3)-O(1)-C(4)-C(5) -178.5(2)C(28)-C(3)-C(2)-O(9) 97.4(4)C(28)-C(3)-C(2)-N(1) -78.1(4)C(2)-N(1)-C(1)-C(24) -55.2(3)C(2)-N(1)-C(1)-C(25) -176.5(3)C(1)-N(1)-C(2)-O(9) -6.8(5)C(1)-N(1)-C(2)-C(3) 168.9(3)C(6)-N(2)-C(5)-C(4) 63.8(3)C(6)-N(2)-C(5)-C(29) -170.4(3)C(6)-C(7)-C(32)-C(33) -58.8(3)C(6)-C(7)-C(32)-C(34) 177.8(3)C(7)-O(2)-C(8)-O(12) 0.3(4)C(7)-O(2)-C(8)-C(9) 178.7(2)C(8)-O(2)-C(7)-C(6) 74.6(3)C(8)-O(2)-C(7)-C(32) -166.1(2)C(8)-C(9)-C(35)-C(36) -58.6(3)C(8)-C(9)-C(35)-C(37) 176.4(3)C(9)-N(3)-C(10)-O(13) 4.3(5)C(9)-N(3)-C(10)-C(11) -178.4(3)C(10)-N(3)-C(9)-C(8) -119.2(3)C(10)-N(3)-C(9)-C(35) 117.2(3)C(11)-O(3)-C(12)-O(14) 2.9(4)C(11)-O(3)-C(12)-C(13) -174.7(2)C(12)-O(3)-C(11)-C(10) -70.5(3)C(12)-O(3)-C(11)-C(38) 169.2(2)C(12)-C(13)-C(39)-C(41) -173.5(2)C(12)-C(13)-C(39)-C(40) -49.8(3)C(13)-N(4)-C(14)-O(15) 5.1(4)C(13)-N(4)-C(14)-C(15) -172.3(2)C(14)-N(4)-C(13)-C(12) 56.3(3)C(14)-N(4)-C(13)-C(39) 176.5(3)C(14)-C(15)-C(42)-C(43) -172.8(3)C(14)-C(15)-C(42)-C(44) 61.5(3)C(24)-O(7)-C(23)-C(22) 73.7(3)C(24)-O(7)-C(23)-C(52) -163.5(2)C(24)-C(1)-C(25)-C(26) 48.7(3)C(24)-C(1)-C(25)-C(27) 171.8(3)C(16)-O(4)-C(15)-C(14) 75.4(3)C(16)-O(4)-C(15)-C(42) -163.2(2)C(16)-C(17)-C(45)-C(47) 177.7(3)C(16)-C(17)-C(45)-C(46) 55.8(3)C(17)-N(5)-C(18)-O(17) -2.1(4)C(17)-N(5)-C(18)-C(19) 174.1(2)C(18)-N(5)-C(17)-C(16) -61.2(3)C(18)-N(5)-C(17)-C(45) 177.4(3)C(19)-O(6)-C(20)-O(18) 1.9(4)C(19)-O(6)-C(20)-C(21) -177.5(2)C(21)-N(6)-C(22)-O(19) -8.8(4)C(21)-N(6)-C(22)-C(23) 172.3(2)C(22)-N(6)-C(21)-C(20) 125.8(3)C(22)-N(6)-C(21)-C(49) -109.3(3)C(22)-C(23)-C(52)-C(54) -176.0(3)C(22)-C(23)-C(52)-C(53) 58.6(3)C(23)-O(7)-C(24)-O(8) -1.1(4)C(23)-O(7)-C(24)-C(1) 176.3(2)C(42)-C(15)-C(14)-O(15) -105.4(3)C(42)-C(15)-C(14)-N(4) 72.1(3)
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C(29)-C(5)-C(4)-O(1) 89.2(3)C(29)-C(5)-C(4)-O(10) -90.9(4)C(25)-C(1)-C(24)-O(7) -94.5(3)C(25)-C(1)-C(24)-O(8) 82.9(3)C(55)-S(2)-O(23)-Ca(1) -93.3(3)C(55)-S(2)-O(24)-Ca(2) -34.6(6)C(56)-S(1)-O(21)-Ca(2) 94.2(3)O(27)-S(3)-C(57)-F(7) -61.6(3)O(27)-S(3)-C(57)-F(8) 57.2(3)O(27)-S(3)-C(57)-F(9) 178.2(2)O(28)-S(3)-C(57)-F(7) -179.9(3)O(28)-S(3)-C(57)-F(8) -61.1(3)O(28)-S(3)-C(57)-F(9) 59.9(3)O(29)-S(3)-C(57)-F(7) 58.4(3)O(29)-S(3)-C(57)-F(8) 177.3(3)O(29)-S(3)-C(57)-F(9) -61.7(3)O(30)-S(4)-C(58)-F(10) 62.4(4)O(30)-S(4)-C(58)-F(11) -178.2(3)O(30)-S(4)-C(58)-F(12) -54.9(4)O(31)-S(4)-C(58)-F(10) -176.8(3)O(31)-S(4)-C(58)-F(11) -57.4(4)O(31)-S(4)-C(58)-F(12) 65.8(4)O(32)-S(4)-C(58)-F(10) -57.0(4)O(32)-S(4)-C(58)-F(11) 62.4(4)O(32)-S(4)-C(58)-F(12) -174.4(4)
O(33)-C(59)-C(60)-C(61) -15.2(4)C(59)-O(33)-C(62)-C(61) -39.2(4)C(59)-C(60)-C(61)-C(62) -7.9(4)C(60)-C(61)-C(62)-O(33) 28.4(4)C(62)-O(33)-C(59)-C(60) 33.9(4)O(34)-C(63)-C(64)-C(65) -28.0(4)C(63)-O(34)-C(66)-C(65) 18.5(4)C(63)-C(64)-C(65)-C(66) 37.8(4)C(64)-C(65)-C(66)-O(34) -34.8(4)C(66)-O(34)-C(63)-C(64) 6.3(4)O(35)-C(67)-C(68)-C(69) -19.1(5)C(67)-O(35)-C(70)-C(69) 23.4(4)C(67)-C(68)-C(69)-C(70) 32.3(5)C(68)-C(69)-C(70)-O(35) -34.6(5)C(70)-O(35)-C(67)-C(68) -2.6(4)O(36)-C(71)-C(72)-C(73) 4.6(4)C(71)-O(36)-C(74)-C(73) 39.1(3)C(71)-C(72)-C(73)-C(74) 18.2(4)C(72)-C(73)-C(74)-O(36) -35.1(3)C(74)-O(36)-C(71)-C(72) -27.2(4)O(37)-C(75)-C(76)-C(77) 38.4(4)C(75)-O(37)-C(78)-C(77) 13.5(7)C(75)-C(76)-C(77)-C(78) -29.5(6)C(76)-C(77)-C(78)-O(37) 11.2(7)C(78)-O(37)-C(75)-C(76) -33.3(5)
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Table 12. Hydrogen bonds for Sample B [Å and °].____________________________________________________________________________ D-H...A d(D-H) d(H...A) d(D...A) <(DHA)____________________________________________________________________________ O(2W)-H(2WA)...O(35) 0.965(14) 1.82(2) 2.742(3) 159(4) O(2W)-H(2WB)...O(3W)0.965(14) 1.790(18) 2.739(4) 167(5) O(1W)-H(1WA)...O(34) 0.967(14) 1.77(2) 2.700(3) 160(4) O(1W)-H(1WB)...O(4W)0.965(14) 1.822(16) 2.784(3) 175(7)____________________________________________________________________________
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