# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1537 # cifs for 3 structures, 1=2-Cd butyl, 2=1-Cd propyl and 3=2-Zn butyl data_1 #2-Cd butyl _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C288 H450 Cd6 N18 O48 S24' _chemical_formula_weight 6376.5 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting rhombohedral _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, z+1/2' 'x, x-y, z+1/2' '-x+y, y, z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-y+2/3, -x+1/3, z+5/6' 'x+2/3, x-y+1/3, z+5/6' '-x+y+2/3, y+1/3, z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-y+1/3, -x+2/3, z+7/6' 'x+1/3, x-y+2/3, z+7/6' '-x+y+1/3, y+2/3, z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'y, x, -z-1/2' '-x, -x+y, -z-1/2' 'x-y, -y, -z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' 'y+2/3, x+1/3, -z-1/6' '-x+2/3, -x+y+1/3, -z-1/6' 'x-y+2/3, -y+1/3, -z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' 'y+1/3, x+2/3, -z+1/6' '-x+1/3, -x+y+2/3, -z+1/6' 'x-y+1/3, -y+2/3, -z+1/6' _cell_length_a 37.653(42) _cell_length_b 37.653(42) _cell_length_c 55.359(63) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 67970.1(1322) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.935 _exptl_crystal_density_method ? _exptl_crystal_F_000 20160 _exptl_absorpt_coefficient_mu 0.44 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 10 min.' _diffrn_standards_number all _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12685 _diffrn_reflns_av_R_equivalents 0.0438 _diffrn_reflns_av_sigmaI/netI 0.0578 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -59 _diffrn_reflns_limit_l_max 59 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 20.00 _reflns_number_total 6903 _reflns_number_observed 4005 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _refine_special_details ; bonds and angles in the alkyl chains were constrained to geometric values dimensions of the solvent molecules were also constrained. all solvent molecules, 5 ethanol and 3 water molecules were given occupancies of 0.5. 3 of the ethanol molecules were disordered over symmetry elements. the relatively high ls_shift/esd_max value is due to the rotation of hydrogen atoms of methyl groups, and not to parameters of heavy atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.2794P)^2^+355.7769P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6899 _refine_ls_number_parameters 515 _refine_ls_number_restraints 39 _refine_ls_R_factor_all 0.2044 _refine_ls_R_factor_obs 0.1406 _refine_ls_wR_factor_all 0.4427 _refine_ls_wR_factor_obs 0.3873 _refine_ls_goodness_of_fit_all 1.103 _refine_ls_goodness_of_fit_obs 1.269 _refine_ls_restrained_S_all 1.107 _refine_ls_restrained_S_obs 1.268 _refine_ls_shift/esd_max 3.309 _refine_ls_shift/esd_mean 0.101 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cd1 Cd 0.89735(4) 0.34584(4) 0.02288(3) 0.1311(9) Uani 1 d . . N51 N 0.9521(5) 0.3708(4) 0.0505(3) 0.117(4) Uani 1 d . . C52 C 0.9835(10) 0.3692(10) 0.0420(4) 0.168(11) Uani 1 d . . H52 H 0.9819(10) 0.3592(10) 0.0265(4) 0.202 Uiso 1 calc R . C53 C 1.0160(16) 0.3806(11) 0.0539(7) 0.238(18) Uani 1 d . . H53 H 1.0372(16) 0.3781(11) 0.0469(7) 0.285 Uiso 1 calc R . C54 C 1.0211(11) 0.3958(16) 0.0757(9) 0.285(26) Uani 1 d . . H54 H 1.0468(11) 0.4076(16) 0.0830(9) 0.342 Uiso 1 calc R . C55 C 0.9883(15) 0.3945(8) 0.0881(5) 0.234(19) Uani 1 d . . H55 H 0.9898(15) 0.4008(8) 0.1045(5) 0.281 Uiso 1 calc R . C56 C 0.9512(9) 0.3827(6) 0.0739(5) 0.157(9) Uani 1 d . . H56 H 0.9286(9) 0.3832(6) 0.0803(5) 0.189 Uiso 1 calc R . S1 S 0.83234(14) 0.28117(13) 0.04071(9) 0.120(2) Uani 1 d . . S2 S 0.89234(14) 0.27746(13) 0.00706(9) 0.124(2) Uani 1 d . . C3 C 0.8460(4) 0.2529(5) 0.0233(3) 0.099(5) Uani 1 d . . N4 N 0.8227(4) 0.2130(4) 0.0207(2) 0.094(3) Uani 1 d . . C5 C 0.7793(5) 0.1924(5) 0.0313(3) 0.125(6) Uani 1 d . . H5A H 0.7612(5) 0.1944(5) 0.0196(3) 0.150 Uiso 1 calc R . H5B H 0.7796(5) 0.2072(5) 0.0456(3) 0.150 Uiso 1 calc R . C11 C 0.7619(6) 0.1468(6) 0.0379(4) 0.109(6) Uani 1 d . . C12 C 0.7334(5) 0.1138(6) 0.0242(4) 0.103(5) Uani 1 d . . C13 C 0.7175(4) 0.0756(5) 0.0326(3) 0.095(5) Uani 1 d . . C14 C 0.7309(4) 0.0671(5) 0.0550(3) 0.084(4) Uani 1 d . . H14 H 0.7195(4) 0.0404(5) 0.0609(3) 0.101 Uiso 1 calc R . C15 C 0.7616(4) 0.1000(6) 0.0677(3) 0.091(4) Uani 1 d . . C16 C 0.7760(5) 0.1387(5) 0.0595(4) 0.098(5) Uani 1 d . . O17 O 0.8079(3) 0.1712(3) 0.0732(2) 0.121(4) Uani 1 d . . C18 C 0.7936(6) 0.1840(5) 0.0939(4) 0.128(6) Uani 1 d . . H18A H 0.8098(6) 0.2136(5) 0.0955(4) 0.154 Uiso 1 calc R . H18B H 0.7653(6) 0.1769(5) 0.0913(4) 0.154 Uiso 1 calc R . O19 O 0.7962(3) 0.1657(4) 0.1154(2) 0.111(3) Uani 1 d . . C21 C 0.7603(5) 0.1304(5) 0.1229(3) 0.085(4) Uani 1 d . . C22 C 0.7389(5) 0.1347(5) 0.1419(3) 0.097(5) Uani 1 d . . C23 C 0.7040(6) 0.0999(6) 0.1502(3) 0.097(5) Uani 1 d . . C24 C 0.6910(5) 0.0615(6) 0.1405(3) 0.093(5) Uani 1 d . . C25 C 0.7138(6) 0.0583(5) 0.1225(3) 0.096(5) Uani 1 d . . H25 H 0.7058(6) 0.0325(5) 0.1161(3) 0.115 Uiso 1 calc R . C26 C 0.7487(5) 0.0920(6) 0.1133(3) 0.089(4) Uani 1 d . . C27 C 0.7758(5) 0.0910(5) 0.0916(3) 0.111(5) Uani 1 d . . H27 H 0.8041(5) 0.1130(5) 0.6503(5) 0.134(5) Uiso 1 calc R . C28 C 0.6503(5) 0.0253(4) 0.1495(3) 0.095(4) Uani 1 d . . H28 H 0.6463(5) 0.0306(4) 0.1663(3) 0.112 Uiso 1 calc R . O29 O 0.6816(3) 0.1032(3) 0.1700(2) 0.105(3) Uani 1 d . . C30 C 0.6463(5) 0.1069(5) 0.1644(3) 0.111(5) Uani 1 d . . H30A H 0.6436(5) 0.1243(5) 0.1764(3) 0.134 Uiso 1 calc R . H30B H 0.6500(5) 0.1198(5) 0.1487(3) 0.134 Uiso 1 calc R . O31 O 0.6106(3) 0.0686(4) 0.1642(2) 0.113(3) Uani 1 d . . S45 S 0.80829(14) 0.26327(13) 0.13625(9) 0.122(2) Uani 1 d . . S44 S 0.86327(14) 0.26056(13) 0.17368(8) 0.115(2) Uani 1 d . . C43 C 0.8180(5) 0.2371(5) 0.1580(2) 0.090(4) Uani 1 d . . N42 N 0.7896(4) 0.1979(4) 0.1633(2) 0.094(3) Uani 1 d . . C41 C 0.7481(4) 0.1762(5) 0.1512(3) 0.102(5) Uani 1 d . . H41A H 0.7477(4) 0.1927(5) 0.1379(3) 0.122 Uiso 1 calc R . H41B H 0.7271(4) 0.1727(5) 0.1627(3) 0.122 Uiso 1 calc R . C100 C 0.8309(6) 0.1880(6) 0.0040(4) 0.150(8) Uani 1 d D . H10A H 0.8452(6) 0.2043(6) -0.0100(4) 0.180 Uiso 1 calc R . H10B H 0.8052(6) 0.1650(6) -0.0014(4) 0.180 Uiso 1 calc R . C101 C 0.8569(9) 0.1718(8) 0.0159(5) 0.216(13) Uani 1 d D . H10C H 0.8430(9) 0.1558(8) 0.0301(5) 0.259 Uiso 1 calc R . H10D H 0.8832(9) 0.1946(8) 0.0208(5) 0.259 Uiso 1 calc R . C102 C 0.8639(15) 0.1435(13) -0.0036(6) 0.342(21) Uiso 1 d D . H10E H 0.8388(15) 0.1265(13) -0.0125(6) 0.411 Uiso 1 calc R . H10F H 0.8852(15) 0.1606(13) -0.0150(6) 0.411 Uiso 1 calc R . C103 C 0.8765(23) 0.1167(18) 0.0109(10) 0.561(44) Uiso 1 d D . H10G H 0.8935(201) 0.1103(203) 0.0011(49) 0.673 Uiso 1 calc R . H10H H 0.8524(25) 0.0918(110) 0.0157(123) 0.673 Uiso 1 calc R . H10I H 0.8915(211) 0.1314(96) 0.0251(76) 0.673 Uiso 1 calc R . C200 C 0.7953(5) 0.1758(5) 0.1834(3) 0.116(5) Uiso 0.50 d PD 1 H20A H 0.8238(5) 0.1923(5) 0.1881(3) 0.139 Uiso 0.50 calc PR 1 H20B H 0.7925(5) 0.1509(5) 0.1764(3) 0.139 Uiso 0.50 calc PR 1 C202 C 0.7639(18) 0.1970(14) 0.2164(7) 0.210(22) Uiso 0.50 d PD 1 H20C H 0.7478(18) 0.2015(14) 0.2044(7) 0.252 Uiso 0.50 calc PR 1 H20D H 0.7904(18) 0.2220(14) 0.2175(7) 0.252 Uiso 0.50 calc PR 1 C201 C 0.7707(14) 0.1621(12) 0.2077(6) 0.167(17) Uiso 0.50 d PD 1 H20E H 0.7445(14) 0.1373(12) 0.2052(6) 0.200 Uiso 0.50 calc PR 1 H20F H 0.7860(14) 0.1564(12) 0.2197(6) 0.200 Uiso 0.50 calc PR 1 C203 C 0.7422(16) 0.1891(16) 0.2409(8) 0.196(22) Uiso 0.50 d PD 1 H20G H 0.7275(94) 0.2038(92) 0.2417(27) 0.235 Uiso 0.50 calc PR 1 H20H H 0.7622(18) 0.1983(102) 0.2536(8) 0.235 Uiso 0.50 calc PR 1 H20I H 0.7234(82) 0.1603(21) 0.2428(29) 0.235 Uiso 0.50 calc PR 1 C210 C 0.7953(5) 0.1758(5) 0.1834(3) 0.116(5) Uiso 0.50 d PD 2 H21A H 0.8240(5) 0.1850(5) 0.1862(3) 0.139 Uiso 0.50 calc PR 2 H21B H 0.7805(5) 0.1464(5) 0.1808(3) 0.139 Uiso 0.50 calc PR 2 C211 C 0.7759(17) 0.1887(17) 0.2050(6) 0.195(20) Uiso 0.50 d PD 2 H21C H 0.7857(17) 0.2179(17) 0.2038(6) 0.234 Uiso 0.50 calc PR 2 H21D H 0.7463(17) 0.1745(17) 0.2030(6) 0.234 Uiso 0.50 calc PR 2 C212 C 0.7854(23) 0.1798(37) 0.2297(6) 0.454(71) Uiso 0.50 d PD 2 H21E H 0.8105(23) 0.2035(37) 0.2354(6) 0.545 Uiso 0.50 calc PR 2 H21F H 0.7904(23) 0.1569(37) 0.2287(6) 0.545 Uiso 0.50 calc PR 2 C213 C 0.7510(17) 0.1695(18) 0.2482(7) 0.203(22) Uiso 0.50 d PD 2 H21G H 0.7414(80) 0.1425(48) 0.2546(50) 0.244 Uiso 0.50 calc PR 2 H21H H 0.7287(48) 0.1704(111) 0.2405(16) 0.244 Uiso 0.50 calc PR 2 H21I H 0.7614(34) 0.1891(68) 0.2612(34) 0.244 Uiso 0.50 calc PR 2 C300 C 0.6496(5) -0.0166(5) 0.1485(3) 0.123(5) Uiso 1 d D . H30A H 0.6518(5) -0.0228(5) 0.1317(3) 0.147 Uiso 1 calc R . H30B H 0.6736(5) -0.0135(5) 0.1569(3) 0.147 Uiso 1 calc R . C301 C 0.6117(7) -0.0529(7) 0.1593(4) 0.182(9) Uiso 1 d D . H30C H 0.5887(7) -0.0588(7) 0.1489(4) 0.219 Uiso 1 calc R . H30D H 0.6157(7) -0.0764(7) 0.1586(4) 0.219 Uiso 1 calc R . C302 C 0.5997(10) -0.0499(9) 0.1841(5) 0.306(19) Uiso 1 d D . H30E H 0.5914(10) -0.0294(9) 0.1844(5) 0.367 Uiso 1 calc R . H30F H 0.6237(10) -0.0402(9) 0.1944(5) 0.367 Uiso 1 calc R . C303 C 0.5636(11) -0.0912(11) 0.1957(6) 0.312(20) Uiso 1 d D . H30G H 0.5666(11) -0.0895(11) 0.2131(6) 0.374 Uiso 1 calc R . H30H H 0.5376(11) -0.0931(11) 0.1918(6) 0.374 Uiso 1 calc R . C304 C 0.5624(17) -0.1289(11) 0.1875(11) 0.478(37) Uiso 1 d D . H30I H 0.5881(69) -0.1221(18) 0.1800(97) 0.574 Uiso 1 calc R . H30J H 0.5407(119) -0.1427(96) 0.1760(83) 0.574 Uiso 1 calc R . H30K H 0.5578(184) -0.1466(80) 0.2011(19) 0.574 Uiso 1 calc R . C400 C 0.7759(5) 0.0487(5) 0.0920(3) 0.116(5) Uiso 1 d D . H40A H 0.7826(5) 0.0437(5) 0.1081(3) 0.139 Uiso 1 calc R . H40B H 0.7487(5) 0.0264(5) 0.0880(3) 0.139 Uiso 1 calc R . C401 C 0.8071(6) 0.0496(6) 0.0739(4) 0.159(7) Uiso 1 d D . H40C H 0.8346(6) 0.0686(6) 0.0796(4) 0.191 Uiso 1 calc R . H40D H 0.8033(6) 0.0593(6) 0.0585(4) 0.191 Uiso 1 calc R . C402 C 0.8024(8) 0.0058(7) 0.0706(5) 0.202(10) Uiso 1 d D . H40E H 0.7753(8) -0.0135(7) 0.0645(5) 0.242 Uiso 1 calc R . H40F H 0.8061(8) -0.0044(7) 0.0860(5) 0.242 Uiso 1 calc R . C403 C 0.8366(13) 0.0109(12) 0.0519(8) 0.385(26) Uiso 1 d D . H40G H 0.8354(13) 0.0249(12) 0.0375(8) 0.462 Uiso 1 calc R . H40H H 0.8637(13) 0.0269(12) 0.0590(8) 0.462 Uiso 1 calc R . C404 C 0.8279(16) -0.0332(13) 0.0456(10) 0.456(33) Uiso 1 d D . H40I H 0.8508(73) -0.0314(15) 0.0369(87) 0.547 Uiso 1 calc R . H40J H 0.8037(97) -0.0468(62) 0.0357(83) 0.547 Uiso 1 calc R . H40K H 0.8238(166) -0.0485(56) 0.0602(10) 0.547 Uiso 1 calc R . O900 O 0.6720(15) 0.9427(12) 0.0730(7) 0.249(19) Uiso 0.50 d PD 1 H900 H 0.6619(167) 0.9540(96) 0.0653(65) 0.298 Uiso 0.50 calc PR 1 C901 C 0.6616(18) 0.9039(14) 0.0616(10) 0.202(23) Uiso 0.50 d PD 1 H90A H 0.6852(18) 0.9000(14) 0.0620(10) 0.242 Uiso 0.50 calc PR 1 H90B H 0.6545(18) 0.9044(14) 0.0448(10) 0.242 Uiso 0.50 calc PR 1 C902 C 0.6245(20) 0.8672(14) 0.0750(13) 0.309(38) Uiso 0.50 d PD 1 H90C H 0.6110(113) 0.8775(21) 0.0850(83) 0.371 Uiso 0.50 calc PR 1 H90D H 0.6344(31) 0.8529(112) 0.0848(87) 0.371 Uiso 0.50 calc PR 1 H90E H 0.6055(93) 0.8486(96) 0.0632(13) 0.371 Uiso 0.50 calc PR 1 O910 O 0.6681(12) 0.1309(10) 0.0729(4) 0.170(11) Uiso 0.50 d P 2 H910 H 0.6776(122) 0.1177(83) 0.0666(38) 0.204 Uiso 0.50 calc PR 2 C911 C 0.6741(15) 0.1615(15) 0.0585(8) 0.170(16) Uiso 0.50 d P 2 H91A H 0.7027(15) 0.1769(15) 0.0535(8) 0.204 Uiso 0.50 calc PR 2 H91B H 0.6573(15) 0.1510(15) 0.0441(8) 0.204 Uiso 0.50 calc PR 2 C912 C 0.6644(17) 0.1846(14) 0.0703(7) 0.188(19) Uiso 0.50 d P 2 H91C H 0.6356(19) 0.1697(35) 0.0739(50) 0.226 Uiso 0.50 calc PR 2 H91D H 0.6705(96) 0.2083(51) 0.0609(22) 0.226 Uiso 0.50 calc PR 2 H91E H 0.6797(65) 0.1931(77) 0.0851(26) 0.226 Uiso 0.50 calc PR 2 O920 O 0.6519(16) 0.4496(15) 0.0776(8) 0.237(20) Uiso 0.50 d PD 3 H920 H 0.6638(21) 0.4698(113) 0.0863(92) 0.285 Uiso 0.50 calc PR 3 C921 C 0.6817(29) 0.4413(32) 0.0662(18) 0.348(47) Uiso 0.50 d PD 3 H92A H 0.7089(29) 0.4610(32) 0.0720(18) 0.418 Uiso 0.50 calc PR 3 H92B H 0.6813(29) 0.4451(32) 0.0489(18) 0.418 Uiso 0.50 calc PR 3 C922 C 0.6742(20) 0.3992(16) 0.0709(9) 0.203(22) Uiso 0.50 d P 3 H92C H 0.6493(57) 0.3841(37) 0.0800(54) 0.244 Uiso 0.50 calc PR 3 H92D H 0.6967(51) 0.4007(16) 0.0798(58) 0.244 Uiso 0.50 calc PR 3 H92E H 0.6715(115) 0.3855(43) 0.0558(9) 0.244 Uiso 0.50 calc PR 3 C932 C 0.7976(25) 0.2719(21) -0.0372(15) 0.349(46) Uiso 0.50 d PD 4 H93A H 0.8132(112) 0.2712(64) -0.0508(79) 0.418 Uiso 0.50 calc PR 4 H93B H 0.7709(83) 0.2657(86) -0.0426(115) 0.418 Uiso 0.50 calc PR 4 H93C H 0.7950(190) 0.2520(31) -0.0255(40) 0.418 Uiso 0.50 calc PR 4 C931 C 0.8203(17) 0.3160(21) -0.0255(12) 0.256(29) Uiso 0.50 d PD 4 H93D H 0.8234(17) 0.3132(21) -0.0084(12) 0.307 Uiso 0.50 calc PR 4 H93E H 0.8476(17) 0.3314(21) -0.0324(12) 0.307 Uiso 0.50 calc PR 4 O930 O 0.7999(33) 0.3388(26) -0.0288(17) 0.462(46) Uiso 0.50 d PD 4 H930 H 0.8083(298) 0.3574(256) -0.0188(164) 0.554 Uiso 0.50 calc PR 4 O940 O 0.6397(17) 0.2150(20) 0.0008(15) 0.374(31) Uiso 0.50 d PD 5 H940 H 0.6257(106) 0.2049(316) -0.0113(64) 0.449 Uiso 0.50 calc PR 5 C941 C 0.6790(21) 0.2202(26) -0.0028(15) 0.368(48) Uiso 0.50 d PD 5 H94A H 0.6869(21) 0.2276(26) -0.0195(15) 0.441 Uiso 0.50 calc PR 5 H94B H 0.6778(21) 0.1942(26) 0.0001(15) 0.441 Uiso 0.50 calc PR 5 C942 C 0.7126(17) 0.2535(22) 0.0139(12) 0.285(33) Uiso 0.50 d PD 5 H94C H 0.7123(112) 0.2416(46) 0.0293(36) 0.342 Uiso 0.50 calc PR 5 H94D H 0.7070(96) 0.2755(78) 0.0162(80) 0.342 Uiso 0.50 calc PR 5 H94E H 0.7390(23) 0.2639(120) 0.0065(49) 0.342 Uiso 0.50 calc PR 5 O400 O 0.7167(23) 0.4691(24) 0.0940(12) 0.335(29) Uiso 0.50 d P 6 O401 O 0.6411(15) 0.9080(15) 0.0653(9) 0.247(18) Uiso 0.50 d P 6 O402 O 0.6964(25) 0.4248(25) 0.0984(13) 0.344(32) Uiso 0.50 d P 6 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.1352(13) 0.0891(11) 0.1536(15) -0.0042(8) 0.0360(9) 0.0445(9) N51 0.097(10) 0.108(10) 0.139(15) -0.007(9) 0.013(10) 0.047(8) C52 0.189(27) 0.261(31) 0.091(16) -0.023(16) -0.029(17) 0.140(25) C53 0.359(67) 0.232(35) 0.153(30) 0.008(26) 0.039(33) 0.170(42) C54 0.137(25) 0.428(69) 0.230(42) -0.043(42) -0.025(27) 0.096(33) C55 0.272(41) 0.142(21) 0.142(23) -0.001(16) -0.056(30) -0.005(25) C56 0.208(27) 0.112(15) 0.139(19) -0.010(14) 0.056(19) 0.071(17) S1 0.118(3) 0.090(3) 0.145(4) -0.016(3) 0.037(3) 0.046(3) S2 0.109(3) 0.102(3) 0.138(4) -0.015(3) 0.041(3) 0.035(3) C3 0.087(10) 0.060(10) 0.113(12) -0.007(9) -0.003(9) 0.010(8) N4 0.087(9) 0.098(10) 0.093(8) -0.010(7) 0.014(7) 0.043(8) C5 0.098(13) 0.100(13) 0.170(16) -0.016(12) 0.020(12) 0.044(10) C11 0.123(14) 0.103(16) 0.109(13) 0.040(12) 0.045(12) 0.063(14) C12 0.068(10) 0.071(12) 0.150(17) -0.042(13) -0.019(11) 0.019(10) C13 0.048(8) 0.079(12) 0.145(15) -0.059(11) -0.012(9) 0.021(9) C14 0.070(9) 0.115(12) 0.086(10) -0.027(9) -0.034(8) 0.060(10) C15 0.067(9) 0.113(14) 0.092(11) -0.030(11) -0.031(9) 0.045(10) C16 0.089(12) 0.064(11) 0.130(16) -0.017(12) 0.026(11) 0.030(10) O17 0.069(6) 0.112(8) 0.135(9) -0.041(7) 0.001(6) 0.009(6) C18 0.129(15) 0.089(12) 0.143(17) -0.027(12) 0.003(14) 0.036(11) O19 0.084(8) 0.104(8) 0.124(9) -0.054(8) -0.033(7) 0.031(7) C21 0.075(11) 0.088(12) 0.095(11) -0.038(10) -0.027(9) 0.044(11) C22 0.078(11) 0.078(11) 0.129(13) -0.072(11) -0.036(11) 0.036(10) C23 0.096(13) 0.113(14) 0.112(13) -0.052(12) -0.047(11) 0.074(13) C24 0.117(14) 0.122(16) 0.070(10) -0.020(10) -0.014(10) 0.081(13) C25 0.091(12) 0.075(11) 0.119(14) -0.035(10) -0.051(11) 0.039(11) C26 0.078(11) 0.110(13) 0.092(11) -0.054(11) -0.046(9) 0.058(11) C27 0.108(12) 0.107(12) 0.127(14) -0.047(10) -0.023(11) 0.061(10) C28 0.081(10) 0.082(10) 0.119(12) 0.003(9) -0.009(9) 0.040(9) O29 0.111(8) 0.121(8) 0.091(7) -0.034(6) -0.014(6) 0.065(7) C30 0.100(13) 0.120(14) 0.138(14) -0.028(11) -0.002(11) 0.074(13) O31 0.083(8) 0.119(9) 0.119(9) -0.015(8) -0.013(7) 0.038(7) S45 0.125(3) 0.102(3) 0.134(4) -0.014(3) -0.053(3) 0.054(3) S44 0.112(3) 0.099(3) 0.104(3) -0.007(2) -0.039(3) 0.030(2) C43 0.089(10) 0.094(11) 0.080(9) -0.016(9) -0.024(8) 0.041(10) N42 0.111(10) 0.099(10) 0.075(7) -0.012(7) -0.017(7) 0.055(9) C41 0.071(10) 0.127(13) 0.106(11) -0.036(10) -0.033(8) 0.049(9) C100 0.152(18) 0.089(12) 0.165(18) -0.025(13) 0.060(15) 0.026(12) C101 0.260(33) 0.181(25) 0.243(31) -0.021(22) 0.071(26) 0.137(26) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N51 2.354(15) . ? Cd1 S44 2.590(5) 36 ? Cd1 S45 2.633(5) 36 ? Cd1 S1 2.633(5) . ? Cd1 S2 2.635(5) . ? N51 C52 1.30(3) . ? N51 C56 1.38(2) . ? C52 C53 1.26(5) . ? C53 C54 1.31(5) . ? C54 C55 1.39(5) . ? C55 C56 1.46(4) . ? S1 C3 1.69(2) . ? S2 C3 1.76(2) . ? C3 N4 1.32(2) . ? N4 C100 1.46(2) . ? N4 C5 1.53(2) . ? C5 C11 1.54(2) . ? C11 C12 1.39(2) . ? C11 C16 1.41(2) . ? C12 C13 1.34(2) . ? C12 O31 1.39(2) 35_655 ? C13 C14 1.43(2) . ? C13 C28 1.55(2) 35_655 ? C14 C15 1.39(2) . ? C15 C16 1.35(2) . ? C15 C27 1.53(2) . ? C16 O17 1.43(2) . ? O17 C18 1.45(2) . ? C18 O19 1.40(2) . ? O19 C21 1.40(2) . ? C21 C22 1.38(2) . ? C21 C26 1.39(2) . ? C22 C23 1.39(2) . ? C22 C41 1.51(2) . ? C23 C24 1.38(2) . ? C23 O29 1.42(2) . ? C24 C25 1.36(2) . ? C24 C28 1.54(2) . ? C25 C26 1.39(2) . ? C26 C27 1.59(2) . ? C27 C400 1.60(2) . ? C28 C13 1.55(2) 35_655 ? C28 C300 1.57(2) . ? O29 C30 1.44(2) . ? C30 O31 1.40(2) . ? O31 C12 1.39(2) 35_655 ? S45 C43 1.71(2) . ? S45 Cd1 2.633(5) 36 ? S44 C43 1.711(14) . ? S44 Cd1 2.590(5) 36 ? C43 N42 1.35(2) . ? N42 C210 1.47(2) . ? N42 C200 1.47(2) . ? N42 C41 1.51(2) . ? C100 C101 1.53(2) . ? C101 C102 1.62(2) . ? C102 C103 1.54(3) . ? C200 C201 1.57(3) . ? C202 C201 1.54(3) . ? C202 C203 1.54(3) . ? C210 C211 1.60(3) . ? C211 C212 1.50(3) . ? C212 C213 1.54(3) . ? C300 C301 1.52(2) . ? C301 C302 1.47(2) . ? C302 C303 1.60(2) . ? C303 C304 1.47(3) . ? C400 C401 1.53(2) . ? C401 C402 1.58(2) . ? C402 C403 1.59(2) . ? C403 C404 1.56(3) . ? O900 C901 1.45(3) . ? C901 C902 1.58(3) . ? O910 C911 1.32(4) . ? C911 C912 1.28(5) . ? O920 C921 1.46(3) . ? C921 C922 1.49(9) . ? C932 C931 1.58(3) . ? C931 O930 1.42(3) . ? O940 C941 1.41(3) . ? C941 C942 1.56(3) . ? O400 O402 1.47(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N51 Cd1 S44 93.9(4) . 36 ? N51 Cd1 S45 96.5(4) . 36 ? S44 Cd1 S45 69.23(14) 36 36 ? N51 Cd1 S1 110.5(4) . . ? S44 Cd1 S1 154.9(2) 36 . ? S45 Cd1 S1 101.09(14) 36 . ? N51 Cd1 S2 103.1(4) . . ? S44 Cd1 S2 112.19(15) 36 . ? S45 Cd1 S2 160.1(2) 36 . ? S1 Cd1 S2 69.01(13) . . ? C52 N51 C56 121.7(20) . . ? C52 N51 Cd1 112.4(17) . . ? C56 N51 Cd1 125.7(18) . . ? C53 C52 N51 123.1(29) . . ? C52 C53 C54 122.3(44) . . ? C53 C54 C55 120.4(38) . . ? C54 C55 C56 116.1(30) . . ? N51 C56 C55 115.5(24) . . ? C3 S1 Cd1 86.2(5) . . ? C3 S2 Cd1 84.9(5) . . ? N4 C3 S1 122.7(11) . . ? N4 C3 S2 117.7(11) . . ? S1 C3 S2 119.6(9) . . ? C3 N4 C100 124.7(13) . . ? C3 N4 C5 118.1(12) . . ? C100 N4 C5 115.6(13) . . ? N4 C5 C11 114.0(13) . . ? C12 C11 C16 118.5(16) . . ? C12 C11 C5 124.9(19) . . ? C16 C11 C5 116.6(18) . . ? C13 C12 O31 125.3(16) . 35_655 ? C13 C12 C11 120.1(19) . . ? O31 C12 C11 114.6(17) 35_655 . ? C12 C13 C14 121.6(14) . . ? C12 C13 C28 115.8(17) . 35_655 ? C14 C13 C28 122.6(16) . 35_655 ? C15 C14 C13 117.8(15) . . ? C16 C15 C14 120.0(15) . . ? C16 C15 C27 122.1(15) . . ? C14 C15 C27 117.8(16) . . ? C15 C16 C11 121.8(15) . . ? C15 C16 O17 117.4(18) . . ? C11 C16 O17 120.7(17) . . ? C16 O17 C18 114.4(11) . . ? O19 C18 O17 112.4(15) . . ? C21 O19 C18 116.5(12) . . ? C22 C21 C26 121.1(16) . . ? C22 C21 O19 117.0(14) . . ? C26 C21 O19 121.7(15) . . ? C21 C22 C23 118.1(14) . . ? C21 C22 C41 122.3(17) . . ? C23 C22 C41 118.8(15) . . ? C24 C23 C22 122.1(16) . . ? C24 C23 O29 118.3(18) . . ? C22 C23 O29 119.6(15) . . ? C25 C24 C23 117.9(17) . . ? C25 C24 C28 123.5(16) . . ? C23 C24 C28 118.5(16) . . ? C24 C25 C26 122.4(14) . . ? C21 C26 C25 118.2(14) . . ? C21 C26 C27 116.3(16) . . ? C25 C26 C27 125.4(15) . . ? C15 C27 C26 110.5(12) . . ? C15 C27 C400 114.1(13) . . ? C26 C27 C400 109.6(14) . . ? C24 C28 C13 107.0(11) . 35_655 ? C24 C28 C300 112.9(12) . . ? C13 C28 C300 112.0(13) 35_655 . ? C23 O29 C30 117.5(11) . . ? O31 C30 O29 111.1(13) . . ? C12 O31 C30 117.3(12) 35_655 . ? C43 S45 Cd1 84.3(5) . 36 ? C43 S44 Cd1 85.6(6) . 36 ? N42 C43 S45 120.1(10) . . ? N42 C43 S44 119.5(11) . . ? S45 C43 S44 120.4(10) . . ? C43 N42 C210 121.6(12) . . ? C43 N42 C200 121.6(12) . . ? C43 N42 C41 122.2(12) . . ? C210 N42 C41 115.8(13) . . ? C200 N42 C41 115.8(13) . . ? N42 C41 C22 110.5(12) . . ? N4 C100 C101 111.7(17) . . ? C100 C101 C102 108.8(19) . . ? C103 C102 C101 106.7(23) . . ? N42 C200 C201 127.5(20) . . ? C201 C202 C203 114.3(27) . . ? C202 C201 C200 108.1(23) . . ? N42 C210 C211 100.1(18) . . ? C212 C211 C210 114.6(29) . . ? C211 C212 C213 113.5(31) . . ? C301 C300 C28 115.3(15) . . ? C302 C301 C300 119.2(19) . . ? C301 C302 C303 116.5(21) . . ? C304 C303 C302 114.6(23) . . ? C401 C400 C27 110.7(14) . . ? C400 C401 C402 111.6(15) . . ? C401 C402 C403 106.7(18) . . ? C404 C403 C402 106.9(24) . . ? O900 C901 C902 110.7(27) . . ? C912 C911 O910 107.4(42) . . ? O920 C921 C922 113.3(70) . . ? O930 C931 C932 114.3(31) . . ? O940 C941 C942 113.5(32) . . ? _refine_diff_density_max 1.298 _refine_diff_density_min -0.508 _refine_diff_density_rms 0.127 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands ; #====END data_2 #1-Cd Cd_propyl _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C258 H408 Cd6 N18 O57 S24' _chemical_formula_weight 6117.86 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting rhombohedral _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, z+1/2' 'x, x-y, z+1/2' '-x+y, y, z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-y+2/3, -x+1/3, z+5/6' 'x+2/3, x-y+1/3, z+5/6' '-x+y+2/3, y+1/3, z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-y+1/3, -x+2/3, z+7/6' 'x+1/3, x-y+2/3, z+7/6' '-x+y+1/3, y+2/3, z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'y, x, -z-1/2' '-x, -x+y, -z-1/2' 'x-y, -y, -z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' 'y+2/3, x+1/3, -z-1/6' '-x+2/3, -x+y+1/3, -z-1/6' 'x-y+2/3, -y+1/3, -z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' 'y+1/3, x+2/3, -z+1/6' '-x+1/3, -x+y+2/3, -z+1/6' 'x-y+1/3, -y+2/3, -z+1/6' _cell_length_a 37.517(44) _cell_length_b 37.517(44) _cell_length_c 56.042(65) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 68312.5(1393) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.892 _exptl_crystal_density_method ? _exptl_crystal_F_000 19260 _exptl_absorpt_coefficient_mu 0.432 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 10 min' _diffrn_standards_number n/a _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13623 _diffrn_reflns_av_R_equivalents 0.1040 _diffrn_reflns_av_sigmaI/netI 0.1286 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 53 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 20.00 _reflns_number_total 7091 _reflns_number_observed 2754 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _refine_special_details ; bonds and angles in the alkyl chains were constrained to geometric values dimensions of the solvent molecules were also constrained. the 2 ethanol solvent molecules were given occupancies of 0.5. as were the 7 water molecules. the relatively high ls_shift/esd_max value is due to the rotation of hydrogen atoms of methyl groups, and not to parameters of heavy atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1913P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7089 _refine_ls_number_parameters 299 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.2427 _refine_ls_R_factor_obs 0.1120 _refine_ls_wR_factor_all 0.3646 _refine_ls_wR_factor_obs 0.2956 _refine_ls_goodness_of_fit_all 1.001 _refine_ls_goodness_of_fit_obs 1.282 _refine_ls_restrained_S_all 1.010 _refine_ls_restrained_S_obs 1.291 _refine_ls_shift/esd_max -1.453 _refine_ls_shift/esd_mean 0.067 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cd1 Cd 0.89904(5) 0.34539(4) 0.02370(3) 0.1463(8) Uani 1 d . . N51 N 0.9528(5) 0.3683(5) 0.0507(3) 0.158(6) Uiso 1 d . . C52 C 0.9860(9) 0.3686(8) 0.0433(5) 0.217(11) Uiso 1 d . . H52 H 0.9865(9) 0.3560(8) 0.0291(5) 0.260 Uiso 1 calc R . C53 C 1.0270(12) 0.3929(11) 0.0606(7) 0.322(18) Uiso 1 d . . H53 H 1.0533(12) 0.4029(11) 0.0544(7) 0.387 Uiso 1 calc R . C54 C 1.0211(10) 0.3981(9) 0.0853(6) 0.252(13) Uiso 1 d . . H54 H 1.0397(10) 0.4025(9) 0.0975(6) 0.303 Uiso 1 calc R . C55 C 0.9837(8) 0.3955(7) 0.0881(5) 0.206(10) Uiso 1 d . . H55 H 0.9809(8) 0.4061(7) 0.1025(5) 0.247 Uiso 1 calc R . C56 C 0.9479(7) 0.3797(7) 0.0731(4) 0.179(8) Uiso 1 d . . H56 H 0.9232(7) 0.3774(7) 0.0783(4) 0.215 Uiso 1 calc R . S1 S 0.83340(14) 0.28068(13) 0.04149(10) 0.128(2) Uani 1 d . . S2 S 0.89274(13) 0.27666(13) 0.00834(9) 0.126(2) Uani 1 d . . C3 C 0.8471(5) 0.2529(5) 0.0236(3) 0.111(5) Uiso 1 d . . N4 N 0.8229(4) 0.2132(4) 0.0215(2) 0.111(4) Uiso 1 d D . C5 C 0.7796(4) 0.1925(4) 0.0319(3) 0.110(5) Uiso 1 d . . H5A H 0.7794(4) 0.2078(4) 0.0458(3) 0.132 Uiso 1 calc R . H5B H 0.7609(4) 0.1932(4) 0.0202(3) 0.132 Uiso 1 calc R . C11 C 0.7645(4) 0.1477(4) 0.0391(3) 0.089(4) Uiso 1 d . . C12 C 0.7330(4) 0.1146(5) 0.0248(3) 0.098(5) Uiso 1 d . . C13 C 0.7172(4) 0.0749(4) 0.0332(3) 0.088(4) Uiso 1 d . . C14 C 0.7301(4) 0.0668(4) 0.0537(2) 0.086(4) Uiso 1 d . . H14 H 0.7180(4) 0.0395(4) 0.0586(2) 0.104 Uiso 1 calc R . C15 C 0.7627(5) 0.0990(5) 0.0691(3) 0.102(5) Uiso 1 d . . C16 C 0.7767(4) 0.1371(4) 0.0594(3) 0.085(4) Uiso 1 d . . O17 O 0.8086(3) 0.1721(3) 0.0725(2) 0.132(4) Uiso 1 d . . C18 C 0.7950(5) 0.1855(5) 0.0929(3) 0.117(5) Uiso 1 d . . H18A H 0.8117(5) 0.2151(5) 0.0944(3) 0.141 Uiso 1 calc R . H18B H 0.7666(5) 0.1786(5) 0.0905(3) 0.141 Uiso 1 calc R . O19 O 0.7978(3) 0.1668(3) 0.1141(2) 0.102(3) Uiso 1 d . . C21 C 0.7619(4) 0.1330(4) 0.1229(3) 0.084(4) Uiso 1 d . . C22 C 0.7379(4) 0.1339(4) 0.1407(3) 0.085(4) Uiso 1 d . . C23 C 0.7048(4) 0.1001(4) 0.1498(3) 0.084(4) Uiso 1 d . . C24 C 0.6923(4) 0.0614(4) 0.1398(3) 0.086(4) Uiso 1 d . . C25 C 0.7147(4) 0.0592(4) 0.1220(2) 0.086(4) Uiso 1 d . . H25 H 0.7057(4) 0.0333(4) 0.1154(2) 0.103 Uiso 1 calc R . C26 C 0.7489(4) 0.0905(4) 0.1126(3) 0.097(5) Uiso 1 d . . C27 C 0.7771(5) 0.0917(5) 0.0914(3) 0.107(5) Uiso 1 d . . H27 H 0.8052(5) 0.1147(5) 0.0941(3) 0.128 Uiso 1 calc R . C28 C 0.6522(4) 0.0248(4) 0.1486(2) 0.085(4) Uiso 1 d . . H28 H 0.6488(4) 0.0296(4) 0.1653(2) 0.102 Uiso 1 calc R . O29 O 0.6832(3) 0.1035(3) 0.1682(2) 0.108(3) Uiso 1 d . . C30 C 0.6493(5) 0.1075(5) 0.1628(3) 0.123(6) Uiso 1 d . . H30A H 0.6527(5) 0.1192(5) 0.1469(3) 0.148 Uiso 1 calc R . H30B H 0.6477(5) 0.1264(5) 0.1740(3) 0.148 Uiso 1 calc R . O31 O 0.6108(3) 0.0676(3) 0.1637(2) 0.117(3) Uiso 1 d . . S45 S 0.80992(14) 0.26397(13) 0.13524(10) 0.130(2) Uani 1 d . . S44 S 0.86461(14) 0.26064(13) 0.17284(9) 0.129(2) Uani 1 d . . C43 C 0.8179(4) 0.2370(4) 0.1570(3) 0.096(5) Uiso 1 d . . N42 N 0.7896(4) 0.1978(4) 0.1630(2) 0.099(4) Uiso 1 d D . C41 C 0.7499(4) 0.1776(4) 0.1485(3) 0.101(5) Uiso 1 d . . H41A H 0.7279(4) 0.1766(4) 0.1581(3) 0.121 Uiso 1 calc R . H41B H 0.7534(4) 0.1942(4) 0.1345(3) 0.121 Uiso 1 calc R . C100 C 0.8292(6) 0.1878(6) 0.0023(3) 0.156(7) Uiso 1 d D . H10A H 0.8433(6) 0.2047(6) -0.0115(3) 0.187 Uiso 1 calc R . H10B H 0.8030(6) 0.1650(6) -0.0029(3) 0.187 Uiso 1 calc R . C101 C 0.8551(8) 0.1721(8) 0.0140(4) 0.236(12) Uiso 1 d D . H10C H 0.8413(8) 0.1552(8) 0.0278(4) 0.283 Uiso 1 calc R . H10D H 0.8817(8) 0.1947(8) 0.0188(4) 0.283 Uiso 1 calc R . C102 C 0.8597(12) 0.1447(11) -0.0076(6) 0.428(25) Uiso 1 d D . H10E H 0.8584(116) 0.1204(59) -0.0010(10) 0.513 Uiso 1 calc R . H10F H 0.8857(51) 0.1608(41) -0.0155(44) 0.513 Uiso 1 calc R . H10G H 0.8379(67) 0.1368(98) -0.0190(36) 0.513 Uiso 1 calc R . C200 C 0.7931(5) 0.1742(5) 0.1837(3) 0.123(6) Uiso 1 d D . H20A H 0.8217(5) 0.1825(5) 0.1866(3) 0.147 Uiso 1 calc R . H20B H 0.7781(5) 0.1448(5) 0.1804(3) 0.147 Uiso 1 calc R . C201 C 0.7733(7) 0.1848(7) 0.2068(3) 0.202(10) Uiso 1 d D . H20C H 0.7902(7) 0.2132(7) 0.2118(3) 0.243 Uiso 1 calc R . H20D H 0.7456(7) 0.1793(7) 0.2035(3) 0.243 Uiso 1 calc R . C202 C 0.7733(14) 0.1549(12) 0.2257(5) 0.500 Uiso 1 d D . H20E H 0.8000(49) 0.1668(71) 0.2329(66) 0.600 Uiso 1 calc R . H20F H 0.7668(158) 0.1294(58) 0.2182(17) 0.600 Uiso 1 calc R . H20G H 0.7531(114) 0.1500(127) 0.2377(50) 0.600 Uiso 1 calc R . C300 C 0.6498(4) -0.0173(4) 0.1474(3) 0.116(5) Uiso 1 d D . H30A H 0.6525(4) -0.0228(4) 0.1307(3) 0.139 Uiso 1 calc R . H30B H 0.6737(4) -0.0148(4) 0.1556(3) 0.139 Uiso 1 calc R . C301 C 0.6124(5) -0.0548(5) 0.1572(3) 0.156(7) Uiso 1 d D . H30C H 0.5892(5) -0.0621(5) 0.1467(3) 0.188 Uiso 1 calc R . H30D H 0.6175(5) -0.0777(5) 0.1575(3) 0.188 Uiso 1 calc R . C302 C 0.6018(7) -0.0483(7) 0.1813(4) 0.234(11) Uiso 1 d D . H30E H 0.5984(7) -0.0243(7) 0.1815(4) 0.281 Uiso 1 calc R . H30F H 0.6240(7) -0.0432(7) 0.1922(4) 0.281 Uiso 1 calc R . C303 C 0.5596(11) -0.0883(11) 0.1901(7) 0.224(21) Uiso 1 d D . H30G H 0.5538(11) -0.0853(11) 0.2066(7) 0.269 Uiso 1 calc R . H30H H 0.5366(11) -0.0921(11) 0.1803(7) 0.269 Uiso 1 calc R . C304 C 0.5665(12) -0.1241(9) 0.1874(8) 0.458(28) Uiso 1 d D . H30I H 0.5426(57) -0.1468(48) 0.1803(76) 0.549 Uiso 1 calc R . H30J H 0.5713(141) -0.1321(90) 0.2028(12) 0.549 Uiso 1 calc R . H30K H 0.5900(86) -0.1164(45) 0.1774(67) 0.549 Uiso 1 calc R . C400 C 0.7770(5) 0.0494(5) 0.0931(3) 0.128(6) Uiso 1 d D . H40A H 0.7881(5) 0.0476(5) 0.1084(3) 0.154 Uiso 1 calc R . H40B H 0.7489(5) 0.0266(5) 0.0920(3) 0.154 Uiso 1 calc R . C401 C 0.8024(6) 0.0466(6) 0.0734(4) 0.182(8) Uiso 1 d D . H40C H 0.7900(6) 0.0464(6) 0.0582(4) 0.218 Uiso 1 calc R . H40D H 0.8026(6) 0.0209(6) 0.0748(4) 0.218 Uiso 1 calc R . C402 C 0.8468(9) 0.0828(12) 0.0740(8) 0.508(32) Uiso 1 d D . H40E H 0.8591(9) 0.0843(12) 0.0895(8) 0.610 Uiso 1 calc R . H40F H 0.8472(9) 0.1085(12) 0.0712(8) 0.610 Uiso 1 calc R . C403 C 0.8723(10) 0.0750(13) 0.0533(8) 0.500 Uiso 1 d D . H40G H 0.8597(10) 0.0725(13) 0.0378(8) 0.600 Uiso 1 calc R . H40H H 0.8733(10) 0.0501(13) 0.0565(8) 0.600 Uiso 1 calc R . C404 C 0.9175(10) 0.1143(13) 0.0539(8) 0.500 Uiso 1 d D . H40I H 0.9314(57) 0.1137(83) 0.0681(46) 0.600 Uiso 1 calc R . H40J H 0.9157(10) 0.1389(13) 0.0538(93) 0.600 Uiso 1 calc R . H40K H 0.9327(53) 0.1141(84) 0.0402(48) 0.600 Uiso 1 calc R . O900 O 0.6624(20) 0.9333(16) 0.0722(8) 0.323(26) Uiso 0.50 d P 1 C912 C 0.6667 0.1875(12) 0.0833 0.323(24) Uiso 1 d S 2 H91A H 0.6876(106) 0.1936(139) 0.0951(49) 0.387 Uiso 0.50 calc PR 2 H91B H 0.6401(59) 0.1729(69) 0.0907(64) 0.387 Uiso 0.50 calc PR 2 H91C H 0.6705(166) 0.2127(73) 0.0766(15) 0.387 Uiso 0.50 calc PR 2 C911 C 0.6701(13) 0.1569(13) 0.0605(8) 0.169(16) Uiso 0.50 d P 2 H91D H 0.6461(13) 0.1451(13) 0.0503(8) 0.203 Uiso 0.50 calc PR 2 H91E H 0.6947(13) 0.1723(13) 0.0509(8) 0.203 Uiso 0.50 calc PR 2 O910 O 0.6719(11) 0.1286(8) 0.0734(4) 0.154(12) Uiso 0.50 d P 2 H910 H 0.6938(59) 0.1390(34) 0.0806(68) 0.185 Uiso 0.50 calc PR 2 O920 O 0.8080(20) 0.2898(20) -0.0438(12) 0.405(31) Uiso 0.50 d P 3 H920 H 0.7887(186) 0.2695(86) -0.0377(51) 0.486 Uiso 0.50 calc PR 3 C921 C 0.8286(14) 0.3294(14) -0.0236(8) 0.192(18) Uiso 0.50 d P 3 H92A H 0.8148(14) 0.3208(14) -0.0083(8) 0.230 Uiso 0.50 calc PR 3 H92B H 0.8578(14) 0.3398(14) -0.0213(8) 0.230 Uiso 0.50 calc PR 3 C922 C 0.8220(18) 0.3578(18) -0.0337(11) 0.285(29) Uiso 0.50 d P 3 H92C H 0.8013(103) 0.3451(32) -0.0458(58) 0.342 Uiso 0.50 calc PR 3 H92D H 0.8471(38) 0.3788(77) -0.0407(73) 0.342 Uiso 0.50 calc PR 3 H92E H 0.8128(140) 0.3698(103) -0.0218(18) 0.342 Uiso 0.50 calc PR 3 O930 O 0.6487(14) 0.8964(14) 0.0652(8) 0.280(19) Uiso 0.50 d P 4 O931 O 0.7085(18) 0.4596(17) 0.0950(10) 0.365(26) Uiso 0.50 d P 4 O932 O 0.6667 0.4593(12) 0.0833 0.404(23) Uiso 1 d S 4 O933 O 1.0927(19) 0.3270(21) 0.1023(10) 0.446(36) Uiso 0.50 d P 4 O934 O 0.6629(13) 0.3970(11) 0.0959(6) 0.252(17) Uiso 0.50 d P 4 O935 O 0.6612(19) 0.2150(18) -0.0131(13) 0.389(29) Uiso 0.50 d P 4 O936 O 0.7054(19) 0.2535(19) 0.0098(11) 0.410(30) Uiso 0.50 d P 4 O937 O 0.6406(15) 0.2247(14) 0.0106(10) 0.326(22) Uiso 0.50 d P 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.1387(13) 0.1054(11) 0.181(2) -0.0049(10) 0.0309(11) 0.0505(10) S1 0.117(4) 0.104(3) 0.151(5) -0.004(3) 0.033(3) 0.046(3) S2 0.104(3) 0.102(3) 0.156(5) -0.009(3) 0.028(3) 0.039(3) S45 0.114(3) 0.093(3) 0.180(5) -0.024(3) -0.054(3) 0.051(3) S44 0.123(4) 0.100(3) 0.135(4) -0.015(3) -0.042(3) 0.035(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N51 2.32(2) . ? Cd1 S44 2.603(5) 36 ? Cd1 S2 2.615(5) . ? Cd1 S45 2.637(5) 36 ? Cd1 S1 2.641(5) . ? N51 C52 1.30(2) . ? N51 C56 1.37(2) . ? C52 C53 1.65(4) . ? C53 C54 1.43(4) . ? C54 C55 1.36(3) . ? C55 C56 1.44(3) . ? S1 C3 1.70(2) . ? S2 C3 1.71(2) . ? C3 N4 1.31(2) . ? N4 C100 1.53(2) . ? N4 C5 1.52(2) . ? C5 C11 1.54(2) . ? C11 C16 1.36(2) . ? C11 C12 1.45(2) . ? C12 O31 1.37(2) 35_655 ? C12 C13 1.38(2) . ? C13 C14 1.34(2) . ? C13 C28 1.59(2) 35_655 ? C14 C15 1.49(2) . ? C15 C16 1.36(2) . ? C15 C27 1.44(2) . ? C16 O17 1.460(15) . ? O17 C18 1.44(2) . ? C18 O19 1.409(15) . ? O19 C21 1.400(14) . ? C21 C22 1.36(2) . ? C21 C26 1.53(2) . ? C22 C23 1.36(2) . ? C22 C41 1.53(2) . ? C23 O29 1.356(14) . ? C23 C24 1.40(2) . ? C24 C25 1.33(2) . ? C24 C28 1.52(2) . ? C25 C26 1.34(2) . ? C26 C27 1.58(2) . ? C27 C400 1.59(2) . ? C28 C300 1.54(2) . ? C28 C13 1.59(2) 35_655 ? O29 C30 1.39(2) . ? C30 O31 1.47(2) . ? O31 C12 1.374(15) 35_655 ? S45 C43 1.705(15) . ? S44 C43 1.759(15) . ? S44 Cd1 2.603(5) 36 ? C43 N42 1.36(2) . ? N42 C200 1.50(2) . ? N42 C41 1.52(2) . ? C100 C101 1.51(2) . ? C101 C102 1.66(2) . ? C200 C201 1.64(2) . ? C201 C202 1.54(2) . ? C300 C301 1.51(2) . ? C301 C302 1.46(2) . ? C302 C303 1.62(2) . ? C303 C304 1.50(3) . ? C400 C401 1.50(2) . ? C401 C402 1.54(2) . ? C402 C403 1.62(3) . ? C403 C404 1.60(3) . ? C912 C911 1.77(4) . ? C911 O910 1.31(4) . ? O920 C921 1.72(6) . ? C921 C922 1.33(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N51 Cd1 S44 95.7(4) . 36 ? N51 Cd1 S2 102.3(4) . . ? S44 Cd1 S2 112.9(2) 36 . ? N51 Cd1 S45 98.0(5) . 36 ? S44 Cd1 S45 69.5(2) 36 36 ? S2 Cd1 S45 159.2(2) . 36 ? N51 Cd1 S1 109.4(5) . . ? S44 Cd1 S1 154.1(2) 36 . ? S2 Cd1 S1 68.57(15) . . ? S45 Cd1 S1 100.05(15) 36 . ? C52 N51 C56 124.5(22) . . ? C52 N51 Cd1 116.4(19) . . ? C56 N51 Cd1 119.1(16) . . ? N51 C52 C53 116.1(26) . . ? C54 C53 C52 118.5(33) . . ? C55 C54 C53 108.8(32) . . ? C54 C55 C56 132.8(30) . . ? N51 C56 C55 114.7(22) . . ? C3 S1 Cd1 85.0(6) . . ? C3 S2 Cd1 85.6(6) . . ? N4 C3 S2 119.5(13) . . ? N4 C3 S1 120.2(13) . . ? S2 C3 S1 120.3(10) . . ? C3 N4 C100 122.6(14) . . ? C3 N4 C5 120.1(13) . . ? C100 N4 C5 114.2(13) . . ? C11 C5 N4 111.9(12) . . ? C16 C11 C12 117.4(14) . . ? C16 C11 C5 123.2(13) . . ? C12 C11 C5 119.2(13) . . ? O31 C12 C13 123.0(14) 35_655 . ? O31 C12 C11 119.4(14) 35_655 . ? C13 C12 C11 117.4(15) . . ? C14 C13 C12 122.0(14) . . ? C14 C13 C28 121.2(13) . 35_655 ? C12 C13 C28 116.7(13) . 35_655 ? C13 C14 C15 123.7(14) . . ? C16 C15 C27 124.2(15) . . ? C16 C15 C14 110.3(14) . . ? C27 C15 C14 125.5(14) . . ? C15 C16 C11 129.2(15) . . ? C15 C16 O17 116.9(13) . . ? C11 C16 O17 113.9(13) . . ? C18 O17 C16 116.1(11) . . ? O19 C18 O17 111.3(12) . . ? C21 O19 C18 117.9(11) . . ? C22 C21 O19 126.1(13) . . ? C22 C21 C26 115.7(13) . . ? O19 C21 C26 118.1(12) . . ? C21 C22 C23 124.3(14) . . ? C21 C22 C41 113.1(13) . . ? C23 C22 C41 122.4(13) . . ? C22 C23 O29 120.6(13) . . ? C22 C23 C24 119.6(14) . . ? O29 C23 C24 119.8(13) . . ? C25 C24 C23 118.0(13) . . ? C25 C24 C28 123.8(13) . . ? C23 C24 C28 118.1(13) . . ? C26 C25 C24 126.6(14) . . ? C25 C26 C21 115.7(13) . . ? C25 C26 C27 130.9(14) . . ? C21 C26 C27 113.3(12) . . ? C15 C27 C26 110.2(13) . . ? C15 C27 C400 115.4(14) . . ? C26 C27 C400 105.1(12) . . ? C300 C28 C24 115.7(11) . . ? C300 C28 C13 110.6(11) . 35_655 ? C24 C28 C13 106.8(11) . 35_655 ? C23 O29 C30 117.9(12) . . ? O29 C30 O31 111.7(12) . . ? C12 O31 C30 112.4(12) 35_655 . ? C43 S45 Cd1 85.4(5) . 36 ? C43 S44 Cd1 85.5(5) . 36 ? N42 C43 S45 123.2(11) . . ? N42 C43 S44 117.6(11) . . ? S45 C43 S44 119.2(9) . . ? C43 N42 C200 125.4(13) . . ? C43 N42 C41 116.5(12) . . ? C200 N42 C41 118.0(11) . . ? C22 C41 N42 112.1(11) . . ? N4 C100 C101 105.4(14) . . ? C100 C101 C102 102.2(17) . . ? N42 C200 C201 106.4(12) . . ? C202 C201 C200 101.6(17) . . ? C301 C300 C28 119.3(13) . . ? C302 C301 C300 112.7(15) . . ? C301 C302 C303 110.1(19) . . ? C304 C303 C302 105.9(21) . . ? C401 C400 C27 110.0(14) . . ? C400 C401 C402 111.6(17) . . ? C401 C402 C403 107.6(23) . . ? C402 C403 C404 105.6(22) . . ? O910 C911 C912 100.3(32) . . ? C922 C921 O920 103.0(49) . . ? _refine_diff_density_max 0.764 _refine_diff_density_min -0.339 _refine_diff_density_rms 0.102 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands ; #====END data_3 #2-Zn butyl _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C276 H417 N18 O43.50 S24 Zn6' _chemical_formula_weight 5844.93 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Rhombohedral _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, z+1/2' 'x, x-y, z+1/2' '-x+y, y, z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-y+2/3, -x+1/3, z+5/6' 'x+2/3, x-y+1/3, z+5/6' '-x+y+2/3, y+1/3, z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-y+1/3, -x+2/3, z+7/6' 'x+1/3, x-y+2/3, z+7/6' '-x+y+1/3, y+2/3, z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'y, x, -z-1/2' '-x, -x+y, -z-1/2' 'x-y, -y, -z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' 'y+2/3, x+1/3, -z-1/6' '-x+2/3, -x+y+1/3, -z-1/6' 'x-y+2/3, -y+1/3, -z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' 'y+1/3, x+2/3, -z+1/6' '-x+1/3, -x+y+2/3, -z+1/6' 'x-y+1/3, -y+2/3, -z+1/6' _cell_length_a 37.228(39) _cell_length_b 37.228(39) _cell_length_c 55.630(72) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 66769.6(1314) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.872 _exptl_crystal_density_method ? _exptl_crystal_F_000 18666 _exptl_absorpt_coefficient_mu 0.48 _exptl_absorpt_correction_type n/a _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 10 min.' _diffrn_standards_number all _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16824 _diffrn_reflns_av_R_equivalents 0.0738 _diffrn_reflns_av_sigmaI/netI 0.0760 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 59 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 22.50 _reflns_number_total 9055 _reflns_number_observed 4582 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _refine_special_details ; bonds and angles in the alkyl chains were constrained to geometric values the alkyl chain on c300 was disordered over two sets of positions, each were given 0.5 occupancy. dimensions of the solvent molecules were also constrained. the three ethanol solvent molecules were given 0.5 occupancy. 2 of the ethanol molecules were disordered over symmetry elements. of the six water solvent molecules, one was given 0.5 occupancy and the others 0.25 occupancy. the relatively high ls_shift/esd_max value is due to the rotation of hydrogen atoms of methyl groups, and not to parameters of heavy atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.3533P)^2^+347.0802P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9055 _refine_ls_number_parameters 343 _refine_ls_number_restraints 47 _refine_ls_R_factor_all 0.2120 _refine_ls_R_factor_obs 0.1413 _refine_ls_wR_factor_all 0.4644 _refine_ls_wR_factor_obs 0.3982 _refine_ls_goodness_of_fit_all 0.877 _refine_ls_goodness_of_fit_obs 1.004 _refine_ls_restrained_S_all 0.879 _refine_ls_restrained_S_obs 1.007 _refine_ls_shift/esd_max -2.435 _refine_ls_shift/esd_mean 0.064 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Zn1 Zn 0.89968(4) 0.34743(4) 0.02415(2) 0.0951(7) Uani 1 d . . N51 N 0.9495(3) 0.3686(3) 0.04898(15) 0.080(2) Uiso 1 d . . C52 C 0.9842(4) 0.3711(4) 0.0409(3) 0.121(4) Uiso 1 d . . H52 H 0.9852(4) 0.3643(4) 0.0249(3) 0.145 Uiso 1 calc R . C53 C 1.0183(6) 0.3830(5) 0.0548(3) 0.160(6) Uiso 1 d . . H53 H 1.0419(6) 0.3832(5) 0.0491(3) 0.192 Uiso 1 calc R . C54 C 1.0156(6) 0.3953(5) 0.0790(3) 0.154(6) Uiso 1 d . . H54 H 1.0383(6) 0.4057(5) 0.0893(3) 0.185 Uiso 1 calc R . C55 C 0.9807(5) 0.3916(4) 0.0862(3) 0.119(4) Uiso 1 d . . H55 H 0.9785(5) 0.3980(4) 0.1021(3) 0.143 Uiso 1 calc R . C56 C 0.9473(4) 0.3788(3) 0.0716(2) 0.095(3) Uiso 1 d . . H56 H 0.9231(4) 0.3772(3) 0.0773(2) 0.114 Uiso 1 calc R . S1 S 0.83773(10) 0.28771(10) 0.04181(6) 0.0996(10) Uani 1 d . . S2 S 0.89570(11) 0.28362(11) 0.00700(7) 0.1144(12) Uani 1 d . . C3 C 0.8508(3) 0.2600(4) 0.0230(2) 0.087(3) Uiso 1 d . . N4 N 0.8259(3) 0.2179(3) 0.0216(2) 0.090(3) Uiso 1 d . . C5 C 0.7826(4) 0.1974(4) 0.0316(2) 0.111(4) Uiso 1 d . . H5A H 0.7642(4) 0.1978(4) 0.0194(2) 0.133 Uiso 1 calc R . H5B H 0.7821(4) 0.2135(4) 0.0451(2) 0.133 Uiso 1 calc R . C11 C 0.7659(4) 0.1527(4) 0.0398(2) 0.093(3) Uiso 1 d . . C12 C 0.7360(4) 0.1201(4) 0.0251(2) 0.094(3) Uiso 1 d . . C13 C 0.7181(3) 0.0797(3) 0.0340(2) 0.083(3) Uiso 1 d . . C14 C 0.7312(3) 0.0699(3) 0.0553(2) 0.074(3) Uiso 1 d . . H14 H 0.7194(3) 0.0424(3) 0.0602(2) 0.089 Uiso 1 calc R . C15 C 0.7620(3) 0.1016(3) 0.0692(2) 0.077(3) Uiso 1 d . . C16 C 0.7772(4) 0.1404(4) 0.0608(2) 0.092(3) Uiso 1 d . . O17 O 0.8099(3) 0.1748(3) 0.07372(15) 0.110(3) Uiso 1 d . . C18 C 0.7969(4) 0.1879(4) 0.0952(2) 0.103(4) Uiso 1 d . . H18A H 0.8146(4) 0.2176(4) 0.0972(2) 0.124 Uiso 1 calc R . H18B H 0.7687(4) 0.1823(4) 0.0929(2) 0.124 Uiso 1 calc R . O19 O 0.7984(2) 0.1690(2) 0.11516(14) 0.102(2) Uiso 1 d . . C21 C 0.7613(3) 0.1338(3) 0.1232(2) 0.084(3) Uiso 1 d . . C22 C 0.7391(3) 0.1386(3) 0.1412(2) 0.072(3) Uiso 1 d . . C23 C 0.7056(3) 0.1039(3) 0.1495(2) 0.072(3) Uiso 1 d . . C24 C 0.6915(4) 0.0629(4) 0.1402(2) 0.091(3) Uiso 1 d . . C25 C 0.7152(3) 0.0608(3) 0.1218(2) 0.080(3) Uiso 1 d . . H25 H 0.7067(3) 0.0350(3) 0.1149(2) 0.096 Uiso 1 calc R . C26 C 0.7508(3) 0.0947(3) 0.1128(2) 0.088(3) Uiso 1 d . . C27 C 0.7775(4) 0.0936(4) 0.0921(2) 0.092(3) Uiso 1 d . . H27 H 0.8061(4) 0.1158(4) 0.0946(1) 0.112(3) Uiso 1 calc R . C28 C 0.6489(3) 0.0273(3) 0.1486(2) 0.085(3) Uiso 1 d . . H28 H 0.6445(3) 0.0331(3) 0.1652(1) 0.104(3) Uiso 1 calc R . O29 O 0.6820(2) 0.1068(2) 0.16892(13) 0.094(2) Uiso 1 d . . C30 C 0.6476(3) 0.1115(3) 0.1633(2) 0.092(3) Uiso 1 d . . H30A H 0.6521(3) 0.1251(3) 0.1478(2) 0.110 Uiso 1 calc R . H30B H 0.6452(3) 0.1292(3) 0.1753(2) 0.110 Uiso 1 calc R . O31 O 0.6094(2) 0.0722(2) 0.16263(14) 0.099(2) Uiso 1 d . . S45 S 0.81261(11) 0.26838(11) 0.13553(7) 0.1104(12) Uani 1 d . . S44 S 0.86716(11) 0.26541(11) 0.17305(6) 0.1183(13) Uani 1 d . . C43 C 0.8194(4) 0.2403(4) 0.1579(2) 0.098(3) Uiso 1 d . . N42 N 0.7928(3) 0.2022(3) 0.16356(15) 0.088(2) Uiso 1 d . . C41 C 0.7512(3) 0.1806(3) 0.1509(2) 0.091(3) Uiso 1 d . . H41A H 0.7300(3) 0.1779(3) 0.1621(2) 0.109 Uiso 1 calc R . H41B H 0.7518(3) 0.1980(3) 0.1378(2) 0.109 Uiso 1 calc R . C100 C 0.8329(5) 0.1919(5) 0.0041(3) 0.135(5) Uiso 1 d D . H10A H 0.8469(5) 0.2081(5) -0.0100(3) 0.163 Uiso 1 calc R . H10B H 0.8066(5) 0.1686(5) -0.0008(3) 0.163 Uiso 1 calc R . C101 C 0.8593(7) 0.1763(7) 0.0158(4) 0.199(8) Uiso 1 d D . H10C H 0.8471(7) 0.1626(7) 0.0310(4) 0.239 Uiso 1 calc R . H10D H 0.8870(7) 0.1991(7) 0.0189(4) 0.239 Uiso 1 calc R . C102 C 0.8609(13) 0.1432(11) -0.0032(6) 0.350(19) Uiso 1 d D . H10E H 0.8336(13) 0.1247(11) -0.0098(6) 0.420 Uiso 1 calc R . H10F H 0.8798(13) 0.1578(11) -0.0163(6) 0.420 Uiso 1 calc R . C103 C 0.8768(29) 0.1184(22) 0.0123(10) 0.755(65) Uiso 1 d D . H10G H 0.8539(69) 0.0964(230) 0.0207(167) 0.906 Uiso 1 calc R . H10H H 0.8971(272) 0.1368(85) 0.0236(145) 0.906 Uiso 1 calc R . H10I H 0.8891(331) 0.1070(309) 0.0018(25) 0.906 Uiso 1 calc R . C200 C 0.7966(4) 0.1795(4) 0.1828(2) 0.116(4) Uiso 0.50 d PD 1 H20A H 0.8251(4) 0.1960(4) 0.1883(2) 0.140 Uiso 0.50 calc PR 1 H20B H 0.7946(4) 0.1549(4) 0.1755(2) 0.140 Uiso 0.50 calc PR 1 C201 C 0.7704(11) 0.1640(10) 0.2061(5) 0.152(12) Uiso 0.50 d PD 1 H20C H 0.7431(11) 0.1408(10) 0.2024(5) 0.182 Uiso 0.50 calc PR 1 H20D H 0.7837(11) 0.1546(10) 0.2175(5) 0.182 Uiso 0.50 calc PR 1 C202 C 0.7662(12) 0.1992(10) 0.2171(6) 0.178(15) Uiso 0.50 d PD 1 H20E H 0.7564(12) 0.2105(10) 0.2047(6) 0.213 Uiso 0.50 calc PR 1 H20F H 0.7936(12) 0.2210(10) 0.2218(6) 0.213 Uiso 0.50 calc PR 1 C203 C 0.7373(13) 0.1882(14) 0.2388(7) 0.186(17) Uiso 0.50 d PD 1 H20G H 0.7305(72) 0.2096(45) 0.2413(32) 0.223 Uiso 0.50 calc PR 1 H20H H 0.7510(34) 0.1858(86) 0.2528(11) 0.223 Uiso 0.50 calc PR 1 H20I H 0.7124(38) 0.1623(45) 0.2359(21) 0.223 Uiso 0.50 calc PR 1 C210 C 0.7966(4) 0.1795(4) 0.1828(2) 0.116(4) Uiso 0.50 d PD 2 H21A H 0.8255(4) 0.1891(4) 0.1866(2) 0.140 Uiso 0.50 calc PR 2 H21B H 0.7826(4) 0.1500(4) 0.1794(2) 0.140 Uiso 0.50 calc PR 2 C211 C 0.7739(11) 0.1899(11) 0.2043(4) 0.141(11) Uiso 0.50 d PD 2 H21C H 0.7891(11) 0.2196(11) 0.2073(4) 0.170 Uiso 0.50 calc PR 2 H21D H 0.7462(11) 0.1827(11) 0.1991(4) 0.170 Uiso 0.50 calc PR 2 C212 C 0.7709(21) 0.1674(20) 0.2271(6) 0.314(34) Uiso 0.50 d PD 2 H21E H 0.7987(21) 0.1779(20) 0.2333(6) 0.376 Uiso 0.50 calc PR 2 H21F H 0.7599(21) 0.1383(20) 0.2233(6) 0.376 Uiso 0.50 calc PR 2 C213 C 0.7444(11) 0.1703(11) 0.2470(5) 0.151(13) Uiso 0.50 d PD 2 H21G H 0.7555(41) 0.1988(14) 0.2515(28) 0.181 Uiso 0.50 calc PR 2 H21H H 0.7445(59) 0.1546(60) 0.2607(16) 0.181 Uiso 0.50 calc PR 2 H21I H 0.7165(18) 0.1592(63) 0.2413(14) 0.181 Uiso 0.50 calc PR 2 C300 C 0.6505(4) -0.0145(4) 0.1485(2) 0.105(4) Uiso 1 d D . H30A H 0.6542(4) -0.0213(4) 0.1322(2) 0.126 Uiso 1 calc R 1 H30B H 0.6739(4) -0.0110(4) 0.1580(2) 0.126 Uiso 1 calc R 1 C31A C 0.6115(5) -0.0486(5) 0.1586(3) 0.164(6) Uiso 0.50 d PD 1 H31A H 0.5886(5) -0.0494(5) 0.1498(3) 0.196 Uiso 0.50 calc PR 1 H31B H 0.6109(5) -0.0745(5) 0.1555(3) 0.196 Uiso 0.50 calc PR 1 C32A C 0.6038(7) -0.0468(8) 0.1845(4) 0.112(8) Uiso 0.50 d PD 1 H32A H 0.6014(7) -0.0224(8) 0.1876(4) 0.135 Uiso 0.50 calc PR 1 H32B H 0.6275(7) -0.0438(8) 0.1935(4) 0.135 Uiso 0.50 calc PR 1 C33A C 0.5638(15) -0.0859(14) 0.1941(10) 0.265(30) Uiso 0.50 d PD 1 H33A H 0.5569(15) -0.0794(14) 0.2098(10) 0.318 Uiso 0.50 calc PR 1 H33B H 0.5409(15) -0.0921(14) 0.1834(10) 0.318 Uiso 0.50 calc PR 1 C34A C 0.5686(21) -0.1242(12) 0.1964(16) 0.331(41) Uiso 0.50 d PD 1 H34A H 0.5616(182) -0.1389(103) 0.1814(37) 0.397 Uiso 0.50 calc PR 1 H34B H 0.5505(138) -0.1420(91) 0.2088(77) 0.397 Uiso 0.50 calc PR 1 H34C H 0.5968(47) -0.1158(17) 0.2005(107) 0.397 Uiso 0.50 calc PR 1 C31B C 0.6115(5) -0.0486(5) 0.1586(3) 0.164(6) Uiso 0.50 d PD 2 H31C H 0.6017(5) -0.0353(5) 0.1697(3) 0.196 Uiso 0.50 calc PR 2 H31D H 0.5919(5) -0.0584(5) 0.1454(3) 0.196 Uiso 0.50 calc PR 2 C32B C 0.6052(13) -0.0857(12) 0.1709(10) 0.320(34) Uiso 0.50 d PD 2 H32C H 0.6260(13) -0.0777(12) 0.1834(10) 0.384 Uiso 0.50 calc PR 2 H32D H 0.6095(13) -0.1029(12) 0.1595(10) 0.384 Uiso 0.50 calc PR 2 C33B C 0.5605(12) -0.1126(10) 0.1827(7) 0.184(16) Uiso 0.50 d PD 2 H33C H 0.5400(12) -0.1117(10) 0.1724(7) 0.221 Uiso 0.50 calc PR 2 H33D H 0.5539(12) -0.1413(10) 0.1839(7) 0.221 Uiso 0.50 calc PR 2 C34B C 0.5587(21) -0.0967(24) 0.2076(10) 0.323(39) Uiso 0.50 d PD 2 H34D H 0.5806(106) -0.0684(61) 0.2092(37) 0.388 Uiso 0.50 calc PR 2 H34E H 0.5618(174) -0.1134(109) 0.2195(10) 0.388 Uiso 0.50 calc PR 2 H34F H 0.5324(69) -0.0981(161) 0.2097(38) 0.388 Uiso 0.50 calc PR 2 C400 C 0.7766(5) 0.0514(4) 0.0919(3) 0.129(5) Uiso 1 d D . H40A H 0.7486(5) 0.0292(4) 0.0886(3) 0.155 Uiso 1 calc R . H40B H 0.7848(5) 0.0464(4) 0.1076(3) 0.155 Uiso 1 calc R . C401 C 0.8065(5) 0.0520(5) 0.0725(3) 0.131(5) Uiso 1 d D . H40C H 0.7974(5) 0.0558(5) 0.0568(3) 0.158 Uiso 1 calc R . H40D H 0.8341(5) 0.0753(5) 0.0753(3) 0.158 Uiso 1 calc R . C402 C 0.8084(8) 0.0111(7) 0.0725(5) 0.247(12) Uiso 1 d D . H40E H 0.7815(8) -0.0120(7) 0.0681(5) 0.297 Uiso 1 calc R 1 H40F H 0.8153(8) 0.0060(7) 0.0884(5) 0.297 Uiso 1 calc R 1 C403 C 0.8424(10) 0.0153(10) 0.0538(7) 0.328(17) Uiso 0.50 d PD 1 H40G H 0.8441(10) 0.0332(10) 0.0407(7) 0.394 Uiso 0.50 calc PR 1 H40H H 0.8693(10) 0.0277(10) 0.0616(7) 0.394 Uiso 0.50 calc PR 1 C404 C 0.8307(24) -0.0280(17) 0.0441(15) 0.453(57) Uiso 0.50 d PD 1 H40I H 0.8030(105) -0.0477(54) 0.0491(137) 0.543 Uiso 0.50 calc PR 1 H40J H 0.8496(173) -0.0361(122) 0.0504(131) 0.543 Uiso 0.50 calc PR 1 H40K H 0.8322(273) -0.0271(69) 0.0269(18) 0.543 Uiso 0.50 calc PR 1 C413 C 0.8424(10) 0.0153(10) 0.0538(7) 0.328(17) Uiso 0.50 d PD 2 H41A H 0.8488(10) -0.0066(10) 0.0566(7) 0.394 Uiso 0.50 calc PR 2 H41B H 0.8316(10) 0.0122(10) 0.0376(7) 0.394 Uiso 0.50 calc PR 2 C414 C 0.8823(25) 0.0579(31) 0.0563(27) 0.751(152) Uiso 0.50 d PD 2 H41C H 0.8794(302) 0.0728(316) 0.0696(280) 0.901 Uiso 0.50 calc PR 2 H41D H 0.8868(416) 0.0735(304) 0.0418(168) 0.901 Uiso 0.50 calc PR 2 H41E H 0.9055(124) 0.0539(32) 0.0591(443) 0.901 Uiso 0.50 calc PR 2 O900 O 0.6608(21) 0.9352(16) 0.0729(9) 0.314(23) Uiso 0.50 d P 1 O901 O 0.6347(15) 0.8908(15) 0.0660(10) 0.267(17) Uiso 0.50 d P 2 H901 H 0.6266(74) 0.9070(18) 0.0695(131) 0.321 Uiso 0.50 calc PR 2 C902 C 0.6682(14) 0.9090(14) 0.0598(8) 0.170(14) Uiso 0.50 d P 2 H90A H 0.6770(14) 0.9383(14) 0.0600(8) 0.204 Uiso 0.50 calc PR 2 H90B H 0.6696(14) 0.9015(14) 0.0433(8) 0.204 Uiso 0.50 calc PR 2 C903 C 0.6977(16) 0.9023(18) 0.0743(12) 0.269(26) Uiso 0.50 d P 2 H90C H 0.7124(101) 0.8934(137) 0.0640(18) 0.323 Uiso 0.50 calc PR 2 H90D H 0.6828(21) 0.8815(100) 0.0863(54) 0.323 Uiso 0.50 calc PR 2 H90E H 0.7171(87) 0.9278(38) 0.0820(65) 0.323 Uiso 0.50 calc PR 2 O920 O 0.5687(21) 0.1049(17) 0.2206(15) 0.401(31) Uiso 0.50 d PD 3 H920 H 0.5450(63) 0.0851(115) 0.2207(148) 0.481 Uiso 0.50 calc PR 3 C921 C 0.5950(20) 0.0948(18) 0.2339(14) 0.327(36) Uiso 0.50 d PD 3 H92A H 0.5973(20) 0.1052(18) 0.2501(14) 0.393 Uiso 0.50 calc PR 3 H92B H 0.6224(20) 0.1095(18) 0.2267(14) 0.393 Uiso 0.50 calc PR 3 C922 C 0.5822(18) 0.0491(18) 0.2355(11) 0.251(23) Uiso 0.50 d PD 3 H92C H 0.5568(66) 0.0345(28) 0.2444(61) 0.301 Uiso 0.50 calc PR 3 H92D H 0.6036(56) 0.0464(20) 0.2435(64) 0.301 Uiso 0.50 calc PR 3 H92E H 0.5783(120) 0.0377(35) 0.2196(11) 0.301 Uiso 0.50 calc PR 3 C912 C 0.8104(35) 0.4467(26) 0.0732(23) 0.612(110) Uiso 0.50 d PD 4 H91A H 0.8315(258) 0.4486(92) 0.0625(245) 0.735 Uiso 0.50 calc PR 4 H91B H 0.7847(272) 0.4361(230) 0.0647(267) 0.735 Uiso 0.50 calc PR 4 H91C H 0.8071(524) 0.4283(144) 0.0862(33) 0.735 Uiso 0.50 calc PR 4 C911 C 0.8233(30) 0.4900(30) 0.0833 0.669(90) Uiso 1 d SD 4 H91D H 0.7986(30) 0.4920(30) 0.0857 0.803 Uiso 0.50 calc PR 4 H91E H 0.8361(30) 0.4928(30) 0.0989 0.803 Uiso 0.50 calc PR 4 O910 O 0.8512(29) 0.5234(28) 0.0686(21) 0.522(54) Uiso 0.50 d PD 4 H910 H 0.8647(328) 0.5161(137) 0.0603(188) 0.626 Uiso 0.50 calc PR 4 O930 O 0.8799(12) 0.5466(12) 0.0833 0.179(13) Uiso 0.50 d SP 5 O931 O 0.3419(30) -0.2328(29) 0.0114(18) 0.315(39) Uiso 0.25 d P 5 O932 O 0.8231(19) 0.3597(20) 0.1931(11) 0.217(23) Uiso 0.25 d P 5 O933 O 0.8547(25) 0.4175(26) 0.2037(14) 0.272(33) Uiso 0.25 d P 5 O938 O 0.5569(45) 0.0045(82) 0.2463(41) 0.306(45) Uiso 0.25 d P 5 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.1009(11) 0.0893(11) 0.0907(10) -0.0103(7) 0.0042(7) 0.0442(8) S1 0.091(2) 0.092(2) 0.111(2) -0.008(2) 0.009(2) 0.043(2) S2 0.100(2) 0.102(2) 0.115(3) -0.016(2) 0.018(2) 0.030(2) S45 0.106(2) 0.102(2) 0.121(3) -0.009(2) -0.021(2) 0.051(2) S44 0.113(3) 0.111(3) 0.093(2) -0.009(2) -0.019(2) 0.028(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N51 2.124(9) . ? Zn1 S45 2.444(4) 36 ? Zn1 S44 2.449(4) 36 ? Zn1 S1 2.470(4) . ? Zn1 S2 2.495(4) . ? N51 C52 1.325(15) . ? N51 C56 1.329(13) . ? C52 C53 1.36(2) . ? C53 C54 1.44(2) . ? C54 C55 1.30(2) . ? C55 C56 1.36(2) . ? S1 C3 1.701(11) . ? S2 C3 1.700(12) . ? C3 N4 1.367(13) . ? N4 C100 1.49(2) . ? N4 C5 1.501(14) . ? C5 C11 1.53(2) . ? C11 C16 1.398(15) . ? C11 C12 1.43(2) . ? C12 O31 1.361(13) 35_655 ? C12 C13 1.394(14) . ? C13 C14 1.397(13) . ? C13 C28 1.551(14) 35_655 ? C14 C15 1.399(13) . ? C15 C16 1.342(14) . ? C15 C27 1.493(15) . ? C16 O17 1.441(13) . ? O17 C18 1.460(13) . ? C18 O19 1.330(12) . ? O19 C21 1.420(13) . ? C21 C22 1.366(13) . ? C21 C26 1.429(14) . ? C22 C23 1.349(13) . ? C22 C41 1.494(14) . ? C23 O29 1.430(11) . ? C23 C24 1.437(14) . ? C24 C25 1.381(14) . ? C24 C28 1.544(15) . ? C25 C26 1.390(14) . ? C26 C27 1.53(2) . ? C27 C400 1.55(2) . ? C28 C13 1.551(14) 35_655 ? C28 C300 1.59(2) . ? O29 C30 1.414(12) . ? C30 O31 1.443(12) . ? O31 C12 1.361(13) 35_655 ? S45 C43 1.723(13) . ? S45 Zn1 2.444(4) 36 ? S44 C43 1.757(13) . ? S44 Zn1 2.449(4) 36 ? C43 N42 1.300(13) . ? N42 C210 1.416(14) . ? N42 C200 1.416(14) . ? N42 C41 1.514(13) . ? C100 C101 1.52(2) . ? C101 C102 1.65(2) . ? C102 C103 1.58(3) . ? C200 C201 1.55(2) . ? C201 C202 1.52(3) . ? C202 C203 1.53(2) . ? C210 C211 1.62(2) . ? C211 C212 1.50(3) . ? C212 C213 1.52(3) . ? C300 C31B 1.481(14) . ? C300 C31A 1.481(14) . ? C31A C32A 1.48(2) . ? C32A C33A 1.56(3) . ? C33A C34A 1.53(3) . ? C31B C32B 1.45(2) . ? C32B C33B 1.59(3) . ? C33B C34B 1.52(3) . ? C400 C401 1.55(2) . ? C401 C402 1.56(2) . ? C402 C413 1.58(2) . ? C402 C403 1.58(2) . ? C403 C404 1.54(3) . ? C413 C414 1.54(3) . ? O901 C902 1.14(5) . ? C902 C903 1.48(6) . ? O920 C921 1.42(3) . ? C921 C922 1.52(3) . ? C912 C911 1.53(2) . ? C911 O910 1.42(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N51 Zn1 S45 100.3(2) . 36 ? N51 Zn1 S44 97.7(3) . 36 ? S45 Zn1 S44 74.24(13) 36 36 ? N51 Zn1 S1 108.9(3) . . ? S45 Zn1 S1 96.29(12) 36 . ? S44 Zn1 S1 152.99(14) 36 . ? N51 Zn1 S2 103.1(3) . . ? S45 Zn1 S2 156.35(14) 36 . ? S44 Zn1 S2 105.39(14) 36 . ? S1 Zn1 S2 73.19(12) . . ? C52 N51 C56 120.0(11) . . ? C52 N51 Zn1 116.4(8) . . ? C56 N51 Zn1 123.6(7) . . ? N51 C52 C53 123.3(15) . . ? C52 C53 C54 115.6(17) . . ? C55 C54 C53 118.8(18) . . ? C54 C55 C56 122.9(16) . . ? N51 C56 C55 119.3(12) . . ? C3 S1 Zn1 83.1(4) . . ? C3 S2 Zn1 82.3(4) . . ? N4 C3 S1 119.6(8) . . ? N4 C3 S2 119.4(8) . . ? S1 C3 S2 120.9(7) . . ? C3 N4 C100 123.0(10) . . ? C3 N4 C5 120.2(9) . . ? C100 N4 C5 113.8(10) . . ? N4 C5 C11 114.5(10) . . ? C16 C11 C12 115.9(11) . . ? C16 C11 C5 125.6(11) . . ? C12 C11 C5 118.5(11) . . ? O31 C12 C13 122.9(10) 35_655 . ? O31 C12 C11 119.3(10) 35_655 . ? C13 C12 C11 117.6(11) . . ? C14 C13 C12 122.8(10) . . ? C14 C13 C28 120.6(9) . 35_655 ? C12 C13 C28 116.4(9) . 35_655 ? C13 C14 C15 119.5(9) . . ? C16 C15 C14 116.4(10) . . ? C16 C15 C27 120.9(10) . . ? C14 C15 C27 122.7(9) . . ? C15 C16 C11 127.4(11) . . ? C15 C16 O17 120.0(10) . . ? C11 C16 O17 112.6(10) . . ? C16 O17 C18 115.5(9) . . ? O19 C18 O17 113.5(10) . . ? C18 O19 C21 118.1(9) . . ? C22 C21 O19 119.1(9) . . ? C22 C21 C26 123.8(10) . . ? O19 C21 C26 117.0(9) . . ? C23 C22 C21 117.1(9) . . ? C23 C22 C41 121.9(9) . . ? C21 C22 C41 121.0(9) . . ? C22 C23 O29 119.6(9) . . ? C22 C23 C24 124.5(10) . . ? O29 C23 C24 115.9(9) . . ? C25 C24 C23 114.9(10) . . ? C25 C24 C28 125.9(10) . . ? C23 C24 C28 118.5(10) . . ? C24 C25 C26 124.3(10) . . ? C25 C26 C21 115.4(10) . . ? C25 C26 C27 125.6(10) . . ? C21 C26 C27 118.9(10) . . ? C15 C27 C26 108.4(9) . . ? C15 C27 C400 112.4(10) . . ? C26 C27 C400 110.3(10) . . ? C24 C28 C13 107.5(9) . 35_655 ? C24 C28 C300 108.4(9) . . ? C13 C28 C300 116.5(9) 35_655 . ? C30 O29 C23 118.1(8) . . ? O29 C30 O31 112.1(9) . . ? C12 O31 C30 119.1(9) 35_655 . ? C43 S45 Zn1 84.9(4) . 36 ? C43 S44 Zn1 84.1(4) . 36 ? N42 C43 S45 125.1(9) . . ? N42 C43 S44 118.7(9) . . ? S45 C43 S44 116.1(7) . . ? C43 N42 C210 125.9(10) . . ? C43 N42 C200 125.9(10) . . ? C43 N42 C41 119.1(9) . . ? C210 N42 C41 114.6(9) . . ? C200 N42 C41 114.6(9) . . ? C22 C41 N42 114.7(9) . . ? N4 C100 C101 109.3(13) . . ? C100 C101 C102 106.4(16) . . ? C103 C102 C101 104.5(22) . . ? N42 C200 C201 128.5(16) . . ? C202 C201 C200 109.3(21) . . ? C201 C202 C203 116.4(24) . . ? N42 C210 C211 101.2(13) . . ? C212 C211 C210 113.1(23) . . ? C211 C212 C213 116.6(29) . . ? C31B C300 C28 109.6(11) . . ? C31A C300 C28 109.6(11) . . ? C32A C31A C300 117.5(15) . . ? C31A C32A C33A 114.1(23) . . ? C34A C33A C32A 113.2(27) . . ? C32B C31B C300 128.0(20) . . ? C31B C32B C33B 114.4(27) . . ? C34B C33B C32B 111.5(25) . . ? C27 C400 C401 109.9(11) . . ? C402 C401 C400 111.7(13) . . ? C401 C402 C413 109.1(16) . . ? C401 C402 C403 109.1(16) . . ? C404 C403 C402 109.4(24) . . ? C414 C413 C402 110.8(26) . . ? O901 C902 C903 115.0(49) . . ? O920 C921 C922 117.2(32) . . ? O910 C911 C912 114.8(30) . . ? _refine_diff_density_max 0.962 _refine_diff_density_min -0.342 _refine_diff_density_rms 0.121 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands ; #===END