# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _journal_coden_Cambridge 440 _publ_requested_journal 'New Journal of Chemistry' loop_ _publ_author_name 'Yuji Kubo' 'Tatsuya Tachikawa' 'Sumio Tokita' 'Tomokazu Tozawa' _publ_contact_author_name 'Yuji Kubo ' _publ_contact_author_address ; Department of Applied Chemistry, Faculty of Engineering, Saitama University, 255 Shimo-Ohkubo, Saitama 338-8570, Japan ; _publ_contact_author_email ' Yuji@apc.saitama-u.ac.jp' _publ_section_title ; Chirality-induction of a dibenzo-30-crown-10 congener promoted by an ion-pair coordinated self-assembly ; data_compound _database_code_CSD 198784 _audit_creation_method maXus _chemical_compound_source 'Local laboratory' _exptl_crystal_description Cube _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_colour Colourless _diffrn_ambient_temperature 298 _refine_ls_hydrogen_treatment noref # Submission details _diffrn_measurement_device 'Mac Science MXC18' _diffrn_measurement_method '\q \w scans' _computing_cell_refinement 'MXC(MAC Science)' _computing_data_collection 'MXC(MAC Science)' _computing_data_reduction 'maXus (Mackay et al., 1999)' _cell_measurement_reflns_used 22 _cell_measurement_theta_min 10 _cell_measurement_theta_max 20 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 0 loop_ _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id all _diffrn_radiation_monochromator graphite _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_UB_11 -0.05038 _diffrn_orient_matrix_UB_12 0.04449 _diffrn_orient_matrix_UB_13 -0.01418 _diffrn_orient_matrix_UB_21 0.05589 _diffrn_orient_matrix_UB_22 0.03957 _diffrn_orient_matrix_UB_23 0.01671 _diffrn_orient_matrix_UB_31 0.01575 _diffrn_orient_matrix_UB_32 -0.02436 _diffrn_orient_matrix_UB_33 -0.08025 _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.36817 _exptl_crystal_density_method 'not measured' _chemical_formula_weight 1087.18 _diffrn_radiation_type ' MoK\a' loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z -X,-Y,-Z _symmetry_space_group_name_H-M 'P -1 ' _symmetry_cell_setting Triclinic _chemical_formula_moiety 'C47 H64 I K N6 O9 S2 ' _chemical_formula_sum 'C47 H64 I K N6 O9 S2 ' _cell_length_a 13.117(2) _cell_length_b 16.848(3) _cell_length_c 13.008(6) _cell_angle_alpha 112.21(2) _cell_angle_beta 95.65(2) _cell_angle_gamma 83.440(10) _cell_volume 2639.0(10) _diffrn_reflns_number 12515 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_av_R_equivalents 0.021 _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_coefficient_mu 0.82 _exptl_crystal_F_000 1064 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 'Waasmaier & Kirfel, 1995' 'H ' 'H ' 0.0000 0.0000 'Waasmaier & Kirfel, 1995' 'N ' 'N ' 0.0061 0.0033 'Waasmaier & Kirfel, 1995' 'O ' 'O ' 0.0106 0.0060 'Waasmaier & Kirfel, 1995' 'S ' 'S ' 0.1246 0.1234 'Waasmaier & Kirfel, 1995' 'K ' 'K ' 0.2009 0.2494 'Waasmaier & Kirfel, 1995' 'I ' 'I ' -0.4742 1.8119 'Waasmaier & Kirfel, 1995' _reflns_number_total 12063 _reflns_number_gt 4839 _reflns_threshold_expression 'I> 2.00 sigma(I)' _reflns_d_resolution_low 2.55 _reflns_d_resolution_high 0.62 _reflns_limit_h_max 17 _reflns_limit_h_min 0 _reflns_limit_k_max 21 _reflns_limit_k_min -21 _reflns_limit_l_max 17 _reflns_limit_l_min -2 _refine_ls_matrix_type full _refine_ls_R_factor_all 0.204 _refine_ls_wR_factor_all 0.095 _refine_ls_R_factor_gt 0.076 _refine_ls_wR_factor_gt 0.053 _refine_ls_wR_factor_ref 0.030 _refine_ls_goodness_of_fit_gt 2.311 _refine_ls_goodness_of_fit_ref 2.311 _refine_ls_goodness_of_fit_all 2.513 _refine_ls_number_parameters 683 _refine_ls_number_reflns 4839 _refine_ls_shift/su_max 0.938 _refine_ls_shift/su_mean 0.119 _refine_diff_density_max 0.51 _refine_diff_density_min 0.25 _refine_ls_structure_factor_coef F^2^ _refine_special_details ; Refinement on F^2^. ; _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ; w = 1 / ( s^2^(Fo^2^) + 0.03000 * Fo^2^) ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _computing_structure_refinement 'maxus(Mackay et al., 1999)' _computing_molecular_graphics 'Ortep (Johnson, 1976)' _computing_publication_material 'maxus(Mackay et al., 1999)' _atom_sites_solution_hydrogens 'geom, diff' #================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type I1 -0.006771(8) 0.272285(7) 0.851801(9) 0.08590(7) 1.00 Uij K2 0.31065(2) -0.24289(2) 0.70683(2) 0.0726(2) 1.00 Uij S45 0.19703(3) 0.28407(2) 1.23077(3) 0.0934(3) 1.00 Uij S55 -0.30229(2) 0.01585(2) 0.66492(3) 0.0685(2) 1.00 Uij O6 0.23465(7) -0.39162(5) 0.54877(7) 0.0668(6) 1.00 Uij O9 0.43766(7) -0.35782(6) 0.54654(7) 0.0841(7) 1.00 Uij O12 0.45386(7) -0.17554(6) 0.60882(7) 0.0784(7) 1.00 Uij O22 0.38892(7) -0.09842(5) 0.88165(6) 0.0637(6) 1.00 Uij O25 0.50243(7) -0.26028(7) 0.82153(8) 0.1013(8) 1.00 Uij O28 0.37070(10) -0.38629(7) 0.79430(10) 0.1109(9) 1.00 Uij O31 0.20075(8) -0.26939(7) 0.87781(8) 0.1018(8) 1.00 Uij O34 0.11274(6) -0.16542(5) 0.76640(7) 0.0728(6) 1.00 Uij O63 -0.25377(8) 0.50141(7) 0.79797(9) 0.1232(9) 1.00 Uij N3 0.12998(7) -0.23199(7) 0.54511(8) 0.0558(7) 1.00 Uij N15 0.30520(8) -0.02729(6) 0.73340(9) 0.0613(7) 1.00 Uij N43 0.21933(8) 0.11613(8) 1.18890(10) 0.0676(9) 1.00 Uij N46 0.20744(8) 0.19884(6) 1.36830(10) 0.0665(7) 1.00 Uij N53 -0.11918(8) 0.07372(6) 0.74559(8) 0.0638(7) 1.00 Uij N56 -0.24855(7) 0.17548(7) 0.77786(8) 0.0636(7) 1.00 Uij C4 0.08010(10) -0.30987(9) 0.51930(10) 0.0620(10) 1.00 Uij C5 0.14870(10) -0.39217(8) 0.47480(10) 0.0810(10) 1.00 Uij C7 0.31430(10) -0.45660(8) 0.50040(10) 0.0850(10) 1.00 Uij C8 0.3941(2) -0.42340(10) 0.4580(2) 0.0810(10) 1.00 Uij C10 0.51970(10) -0.32100(10) 0.52380(10) 0.1060(10) 1.00 Uij C11 0.49790(10) -0.23900(10) 0.51720(10) 0.1080(10) 1.00 Uij C13 0.44780(10) -0.09390(10) 0.60570(10) 0.0750(10) 1.00 Uij C14 0.41090(10) -0.02540(10) 0.71100(10) 0.0680(10) 1.00 Uij C16 0.28030(10) 0.01276(9) 0.84860(10) 0.0558(9) 1.00 Uij C17 0.21460(10) 0.08380(9) 0.88890(10) 0.0610(10) 1.00 Uij C18 0.18804(9) 0.11992(7) 1.00020(10) 0.0620(9) 1.00 Uij C19 0.23610(10) 0.08399(8) 1.07320(10) 0.0578(9) 1.00 Uij C20 0.30007(9) 0.01114(8) 1.03500(10) 0.0560(9) 1.00 Uij C21 0.32519(9) -0.02641(8) 0.92400(10) 0.0537(9) 1.00 Uij C23 0.45700(10) -0.12370(10) 0.95780(10) 0.0750(10) 1.00 Uij C24 0.54170(10) -0.18410(10) 0.89090(10) 0.0880(10) 1.00 Uij C26 0.5303(2) -0.33290(10) 0.8394(3) 0.216(2) 1.00 Uij C27 0.4782(2) -0.39690(10) 0.8113(2) 0.176(2) 1.00 Uij C29 0.3163(2) -0.38630(10) 0.8772(2) 0.151(2) 1.00 Uij C30 0.2139(2) -0.35420(10) 0.87630(10) 0.130(2) 1.00 Uij C32 0.09910(10) -0.23690(10) 0.88440(10) 0.123(2) 1.00 Uij C33 0.08280(10) -0.15470(10) 0.87350(10) 0.0890(10) 1.00 Uij C35 0.05512(9) -0.12085(8) 0.70860(10) 0.0501(8) 1.00 Uij C36 -0.00620(10) -0.04680(9) 0.75640(10) 0.0535(9) 1.00 Uij C37 -0.06275(9) -0.00610(8) 0.69320(10) 0.0562(9) 1.00 Uij C38 -0.05940(10) -0.04218(9) 0.58030(10) 0.0680(10) 1.00 Uij C39 0.00380(10) -0.11492(8) 0.53091(9) 0.0574(9) 1.00 Uij C40 0.06248(9) -0.15594(7) 0.59220(10) 0.0495(8) 1.00 Uij C41 0.17998(9) -0.23117(8) 0.45000(10) 0.0900(10) 1.00 Uij C42 0.23500(10) 0.01120(10) 0.66320(10) 0.0830(10) 1.00 Uij C44 0.20881(9) 0.19848(8) 1.26430(10) 0.0575(9) 1.00 Uij C47 0.20145(9) 0.26623(9) 1.47520(10) 0.0576(9) 1.00 Uij C48 0.21020(10) 0.23920(10) 1.56490(10) 0.0710(10) 1.00 Uij C49 0.20010(10) 0.30110(10) 1.66860(10) 0.0910(10) 1.00 Uij C50 0.18500(10) 0.38530(10) 1.68700(10) 0.1030(10) 1.00 Uij C51 0.17860(10) 0.41170(10) 1.60170(10) 0.1050(10) 1.00 Uij C52 0.18650(10) 0.35260(10) 1.49470(10) 0.0790(10) 1.00 Uij C54 -0.22200(10) 0.08988(8) 0.73060(10) 0.0560(9) 1.00 Uij C57 -0.34450(10) 0.22408(9) 0.78650(10) 0.0620(10) 1.00 Uij C58 -0.34230(10) 0.31064(9) 0.80280(10) 0.0700(10) 1.00 Uij C59 -0.4337(2) 0.36322(9) 0.81430(10) 0.0930(10) 1.00 Uij C60 -0.52580(10) 0.33070(10) 0.8101(2) 0.103(2) 1.00 Uij C61 -0.52740(10) 0.24730(10) 0.79560(10) 0.0950(10) 1.00 Uij C62 -0.43600(10) 0.19310(8) 0.78410(10) 0.0840(10) 1.00 Uij C64 -0.18460(10) 0.52460(10) 0.86830(10) 0.0980(10) 1.00 Uij C65 -0.08060(10) 0.52811(9) 0.84010(10) 0.1180(10) 1.00 Uij C66 -0.2036(2) 0.5501(2) 0.9817(2) 0.293(3) 1.00 Uij H17 0.1810(7) 0.1129(6) 0.8444(7) 0.040(3) 1.00 Uiso H18 0.137(5) 0.168(5) 1.024(6) 0.05(3) 1.00 Uiso H20 0.330(6) -0.017(5) 1.084(7) 0.05(4) 1.00 Uiso H38 -0.0855(6) -0.0131(5) 0.5415(7) 0.016(3) 1.00 Uiso H36 -0.0141(6) -0.0268(5) 0.8317(6) 0.018(3) 1.00 Uiso H39 0.008(6) -0.139(5) 0.452(7) 0.05(3) 1.00 Uiso H43 0.2301(6) 0.0779(5) 1.2210(7) 0.012(3) 1.00 Uiso H48 0.2185(6) 0.1751(5) 1.5511(7) 0.038(3) 1.00 Uiso H49 0.204(7) 0.283(6) 1.731(8) 0.05(4) 1.00 Uiso H4A 0.0528(6) -0.3091(5) 0.5906(6) 0.023(3) 1.00 Uiso H4B 0.0080(7) -0.3156(5) 0.4739(7) 0.054(3) 1.00 Uiso H50 0.180(5) 0.426(4) 1.762(6) 0.05(2) 1.00 Uiso H51 0.169(6) 0.472(5) 1.616(6) 0.05(3) 1.00 Uiso H52 0.182(7) 0.373(6) 1.434(8) 0.05(4) 1.00 Uiso H58 -0.279(7) 0.334(6) 0.805(9) 0.05(5) 1.00 Uiso H5A 0.110(6) -0.440(5) 0.463(6) 0.05(3) 1.00 Uiso H5B 0.170(7) -0.395(6) 0.405(8) 0.05(4) 1.00 Uiso H60 -0.5878(8) 0.3605(7) 0.8220(10) 0.085(5) 1.00 Uiso H61 -0.6000(10) 0.2270(10) 0.7970(10) 0.210(10) 1.00 Uiso H62 -0.440(7) 0.135(6) 0.777(7) 0.05(3) 1.00 Uiso H8A 0.4587(8) -0.4749(7) 0.4278(8) 0.096(5) 1.00 Uiso H8B 0.3728(9) -0.3983(8) 0.4240(10) 0.047(5) 1.00 Uiso H10A 0.550(9) -0.363(8) 0.460(10) 0.05(6) 1.00 Uiso H10B 0.570(10) -0.311(9) 0.590(10) 0.05(9) 1.00 Uiso H11A 0.560(10) -0.219(9) 0.500(10) 0.05(9) 1.00 Uiso H11B 0.447(8) -0.248(7) 0.457(9) 0.05(5) 1.00 Uiso H13A 0.40(2) -0.090(10) 0.55(2) 0.1(2) 1.00 Uiso H13B 0.510(10) -0.082(9) 0.590(10) 0.05(9) 1.00 Uiso H14A 0.4517(6) -0.0337(5) 0.7558(6) 0.002(3) 1.00 Uiso H14B 0.4287(7) 0.0373(6) 0.7157(7) 0.056(4) 1.00 Uiso H23A 0.4190(7) -0.1511(6) 0.9913(8) 0.048(4) 1.00 Uiso H23B 0.4858(7) -0.0702(6) 1.0072(7) 0.044(3) 1.00 Uiso H24A 0.5842(7) -0.2004(6) 0.9366(8) 0.042(4) 1.00 Uiso H24B 0.596(3) -0.125(2) 0.907(3) 0.65(3) 1.00 Uiso H26A 0.5263(6) -0.3101(5) 0.9188(7) 0.050(3) 1.00 Uiso H26B 0.6006(7) -0.3495(6) 0.8213(7) 0.050(4) 1.00 Uiso H27A 0.4991(7) -0.4303(6) 0.7375(8) 0.050(4) 1.00 Uiso H27B 0.4897(7) -0.4314(5) 0.8562(7) 0.050(3) 1.00 Uiso H29A 0.3442(8) -0.3441(6) 0.9437(8) 0.050(4) 1.00 Uiso H29B 0.324(2) -0.441(2) 0.884(2) 0.05(2) 1.00 Uiso H30A 0.187659 -0.392205 0.805268 0.050000 1.00 Uiso H30B 0.177015 -0.358506 0.934066 0.050000 1.00 Uiso H32A 0.074527 -0.233370 0.953354 0.050000 1.00 Uiso H32B 0.060684 -0.276284 0.823433 0.050000 1.00 Uiso H33A 0.0186(7) -0.1321(7) 0.8808(8) 0.055(4) 1.00 Uiso H33B 0.1300(10) -0.0893(9) 0.9290(10) 0.180(7) 1.00 Uiso H41A 0.225248 -0.282283 0.420299 0.050000 1.00 Uiso H41B 0.218186 -0.181486 0.471923 0.050000 1.00 Uiso H41C 0.127104 -0.229006 0.394294 0.050000 1.00 Uiso H42A 0.2643(8) 0.0842(7) 0.6813(9) 0.116(5) 1.00 Uiso H42B 0.1620(7) -0.0090(7) 0.6595(8) 0.073(4) 1.00 Uiso H42C 0.2476(7) -0.0166(6) 0.6067(6) 0.011(3) 1.00 Uiso H65A -0.080343 0.509786 0.760717 0.050000 1.00 Uiso H65B -0.034259 0.489718 0.864976 0.050000 1.00 Uiso H65C -0.058893 0.585349 0.874175 0.050000 1.00 Uiso H66A -0.2744(8) 0.5459(7) 0.9902(9) 0.050(5) 1.00 Uiso H66B -0.1861(7) 0.6080(7) 1.0228(8) 0.050(4) 1.00 Uiso H66C -0.1608(7) 0.5115(6) 1.0093(6) 0.050(3) 1.00 Uiso H46 0.210944 0.140328 1.363507 0.050000 1.00 Uiso H7A 0.283949 -0.502065 0.439402 0.050000 1.00 Uiso H7B 0.345163 -0.478645 0.555300 0.050000 1.00 Uiso H56 -0.186779 0.203185 0.810033 0.050000 1.00 Uiso H59 -0.432317 0.422531 0.824166 0.050000 1.00 Uiso H53 -0.079829 0.118809 0.796163 0.050000 1.00 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 I1 0.08055(8) 0.08597(8) 0.07732(8) -.02313(6) -.00282(6) 0.02970(6) K2 0.0617(2) 0.0768(2) 0.0604(2) 0.0016(2) 0.0029(2) 0.0128(2) S45 0.1477(4) 0.0554(3) 0.0657(3) 0.0042(3) 0.0168(3) 0.0237(2) S55 0.0580(2) 0.0546(2) 0.0800(3) -.0109(2) -.0024(2) 0.0229(2) O6 0.0562(6) 0.0616(7) 0.0638(7) 0.0071(5) 0.0022(6) 0.0101(5) O9 0.0715(7) 0.0744(7) 0.0815(8) -.0148(6) 0.0224(6) -.0019(6) O12 0.0833(7) 0.0609(7) 0.0737(7) 0.0001(6) 0.0329(6) 0.0086(6) O22 0.0703(7) 0.0506(6) 0.0545(6) 0.0122(5) -.0039(5) 0.0124(5) O25 0.0951(8) 0.0575(7) 0.1220(10) 0.0255(7) -.0300(7) 0.0200(7) O28 0.1080(10) 0.0949(9) 0.1120(10) 0.0245(8) 0.0251(8) 0.0466(8) O31 0.0868(8) 0.1089(9) 0.1034(8) 0.0237(7) 0.0246(7) 0.0727(8) O34 0.0650(6) 0.0900(7) 0.0533(6) 0.0259(5) 0.0236(5) 0.0372(6) O63 0.0986(9) 0.1380(10) 0.1035(9) -.0260(8) -.0200(7) 0.0301(8) N3 0.0503(7) 0.0713(8) 0.0373(7) -.0012(7) 0.0046(6) 0.0235(6) N15 0.0447(8) 0.0730(8) 0.0538(8) -.0103(6) 0.0004(6) 0.0203(7) N43 0.0815(9) 0.0584(9) 0.0544(9) -.0054(7) 0.0157(7) 0.0221(8) N46 0.0894(9) 0.0347(7) 0.0654(8) -.0055(6) 0.0129(7) 0.0153(7) N53 0.0548(7) 0.0398(7) 0.0791(8) 0.0009(6) -.0034(7) 0.0093(6) N56 0.0398(7) 0.0668(8) 0.0725(8) 0.0029(6) 0.0011(6) 0.0299(7) C4 0.0450(10) 0.0530(10) 0.0720(10) -.0143(8) 0.0014(9) 0.0091(9) C5 0.0680(10) 0.0610(10) 0.0910(10) -.0082(9) 0.0190(10) 0.0016(9) C7 0.0700(10) 0.0660(10) 0.0990(10) 0.0008(9) -.0090(10) 0.0200(10) C8 0.078(2) 0.0720(10) 0.0700(10) 0.0080(10) -.0010(10) 0.0080(10) C10 0.1000(10) 0.0890(10) 0.0990(10) 0.0130(10) 0.0450(10) 0.0040(10) C11 0.0830(10) 0.108(2) 0.113(2) -.0020(10) 0.0400(10) 0.0330(10) C13 0.0630(10) 0.0750(10) 0.0690(10) -.0133(9) 0.0160(8) 0.0080(10) C14 0.0550(10) 0.0650(10) 0.0690(10) -.0130(10) -.0030(10) 0.0160(10) C16 0.0425(9) 0.0610(10) 0.0500(10) -.0016(8) -.0011(8) 0.0131(9) C17 0.0500(10) 0.0710(10) 0.0520(10) 0.0009(8) -.0067(8) 0.0308(9) C18 0.0458(9) 0.0560(9) 0.0720(10) 0.0104(7) 0.0087(8) 0.0241(9) C19 0.0570(10) 0.0520(10) 0.0540(10) 0.0074(8) 0.0167(8) 0.0154(8) C20 0.0700(10) 0.0532(9) 0.0373(9) -.0044(8) -.0017(7) 0.0204(7) C21 0.0497(9) 0.0396(9) 0.0600(10) -.0103(7) -.0104(8) 0.0148(8) C23 0.0670(10) 0.0600(10) 0.0830(10) -.0060(10) -.0020(10) 0.0210(10) C24 0.0810(10) 0.0540(10) 0.0940(10) 0.0120(10) -.0450(10) -.0030(10) C26 0.116(2) 0.094(2) 0.388(4) 0.015(2) -.064(2) 0.097(2) C27 0.194(3) 0.129(2) 0.194(2) 0.101(2) 0.095(2) 0.115(2) C29 0.170(2) 0.107(2) 0.165(2) 0.035(2) 0.052(2) 0.083(2) C30 0.142(2) 0.127(2) 0.116(2) 0.0310(10) 0.0570(10) 0.0820(10) C32 0.100(2) 0.176(2) 0.0830(10) 0.0100(10) 0.0330(10) 0.0790(10) C33 0.0780(10) 0.109(2) 0.0730(10) 0.0300(10) 0.0370(10) 0.0600(10) C35 0.0425(8) 0.0505(9) 0.0507(9) 0.0062(7) 0.0090(7) 0.0259(8) C36 0.0476(9) 0.0560(10) 0.0470(10) 0.0064(7) 0.0138(8) 0.0163(9) C37 0.0427(9) 0.0442(9) 0.0700(10) 0.0047(7) 0.0083(8) 0.0199(9) C38 0.0620(10) 0.0560(10) 0.0770(10) 0.0108(8) -.0060(9) 0.0400(10) C39 0.0640(10) 0.0553(9) 0.0433(9) 0.0040(8) 0.0048(7) 0.0198(8) C40 0.0413(8) 0.0441(9) 0.0540(10) 0.0062(7) 0.0082(7) 0.0187(8) C41 0.0630(10) 0.0990(10) 0.0870(10) 0.0216(8) 0.0062(9) 0.0350(10) C42 0.0750(10) 0.116(2) 0.0390(10) -.0090(10) 0.0030(10) 0.0200(10) C44 0.0586(9) 0.0550(10) 0.0470(9) -.0137(7) 0.0101(8) 0.0081(8) C47 0.0455(9) 0.0610(10) 0.0540(10) -.0108(8) 0.0115(7) 0.0107(9) C48 0.0680(10) 0.0650(10) 0.0680(10) -.0084(9) 0.0005(9) 0.0260(10) C49 0.0830(10) 0.130(2) 0.0430(10) -.0250(10) 0.0060(9) 0.0230(10) C50 0.1220(10) 0.0870(10) 0.0610(10) -.0270(10) 0.0220(10) -.0390(10) C51 0.147(2) 0.0740(10) 0.0720(10) -.0040(10) 0.0380(10) 0.0070(10) C52 0.1100(10) 0.0580(10) 0.0610(10) -.0130(10) 0.0307(9) 0.0172(9) C54 0.0620(10) 0.0433(9) 0.0558(9) 0.0235(8) 0.0153(8) 0.0291(8) C57 0.0700(10) 0.0540(10) 0.0509(9) -.0074(9) 0.0018(8) 0.0186(8) C58 0.0740(10) 0.0600(10) 0.0630(10) 0.0062(9) 0.0232(8) 0.0205(8) C59 0.1150(10) 0.0550(10) 0.0930(10) 0.0240(10) 0.0090(10) 0.0289(9) C60 0.0610(10) 0.116(2) 0.1060(10) 0.0220(10) 0.0120(10) 0.0360(10) C61 0.0680(10) 0.0890(10) 0.1070(10) 0.0040(10) 0.0020(10) 0.0290(10) C62 0.0700(10) 0.0540(10) 0.1110(10) -.0020(9) 0.0150(10) 0.0251(9) C64 0.098(2) 0.0700(10) 0.103(2) -.0300(10) -.0270(10) 0.0190(10) C65 0.1100(10) 0.0930(10) 0.1200(10) -.0230(10) -.0340(10) 0.0190(10) C66 0.237(3) 0.536(4) 0.0530(10) -.192(3) -.007(2) 0.068(2) _geom_special_details ; All standard uncertainties (except dihedral angles between l.s. planes) are estimated using the full covariance matrix. The standard uncertainties in cell dimensions are are used in calculating the standard uncertainties of bond distances, angles and torsion angles. Angles between l.s. planes have standard uncertainties calculated from atomic positional standard uncertainties; the errors in cell dimensions are not used in this case. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag S45 C44 1.6450(10) . . ? S55 C54 1.6470(10) . . ? O6 C5 1.4070(10) . . ? O6 C7 1.4260(10) . . ? O9 C8 1.388(2) . . ? O9 C10 1.409(2) . . ? O12 C11 1.389(2) . . ? O12 C13 1.3850(10) . . ? O22 C21 1.3520(10) . . ? O22 C23 1.4210(10) . . ? O25 C24 1.3820(10) . . ? O25 C26 1.335(2) . . ? O28 C27 1.407(2) . . ? O28 C29 1.350(2) . . ? O31 C30 1.413(2) . . ? O31 C32 1.381(2) . . ? O34 C33 1.4250(10) . . ? O34 C35 1.3730(10) . . ? O63 C64 1.2080(10) . . ? N3 C4 1.4430(10) . . ? N3 C40 1.4340(10) . . ? N3 C41 1.4610(10) . . ? N15 C14 1.4500(10) . . ? N15 C16 1.4450(10) . . ? N43 C19 1.4240(10) . . ? N43 C44 1.3640(10) . . ? N46 C44 1.3520(10) . . ? N46 C47 1.4270(10) . . ? N53 C37 1.4140(10) . . ? N53 C54 1.3540(10) . . ? N56 C54 1.3550(10) . . ? N56 C57 1.4100(10) . . ? C7 C8 1.482(2) . . ? C10 C11 1.410(2) . . ? C16 C17 1.353(2) . . ? C16 C21 1.4250(10) . . ? C17 C18 1.405(2) . . ? C18 C19 1.3770(10) . . ? C19 C20 1.3570(10) . . ? C20 C21 1.3970(10) . . ? C26 C27 1.258(3) . . ? C29 C30 1.390(2) . . ? C32 C33 1.434(2) . . ? C35 C36 1.3690(10) . . ? C35 C40 1.4110(10) . . ? C36 C37 1.373(2) . . ? C37 C38 1.364(2) . . ? C38 C39 1.371(2) . . ? C39 C40 1.3720(10) . . ? C47 C48 1.395(2) . . ? C47 C52 1.3740(10) . . ? C48 C49 1.366(2) . . ? C49 C50 1.339(2) . . ? C50 C51 1.336(2) . . ? C51 C52 1.377(2) . . ? C57 C58 1.3950(10) . . ? C57 C62 1.3560(10) . . ? C58 C59 1.392(2) . . ? C59 C60 1.371(2) . . ? C60 C61 1.348(2) . . ? C61 C62 1.406(2) . . ? C64 C65 1.459(2) . . ? C64 C66 1.411(2) . . ? N43 H43 0.882(7) . . ? N46 H46 0.9601(9) . . ? N53 H53 0.9598(9) . . ? N56 H56 0.9599(9) . . ? C5 H5A 0.9610(10) . . ? C5 H5B 0.9590(10) . . ? C7 H7A 0.9610(10) . . ? C7 H7B 0.9590(10) . . ? C8 H8B 0.736(10) . . ? C10 H10A 0.9590(10) . . ? C10 H10B 0.959(2) . . ? C11 H11A 0.9590(10) . . ? C11 H11B 0.961(2) . . ? C13 H13A 0.9600(10) . . ? C13 H13B 0.9590(10) . . ? C14 H14A 0.793(7) . . ? C17 H17 0.940(8) . . ? C18 H18 0.9600(10) . . ? C20 H20 0.9600(10) . . ? C23 H23A 0.948(8) . . ? C23 H23B 0.979(8) . . ? C24 H24A 0.873(9) . . ? C26 H26A 0.960(3) . . ? C26 H26B 0.958(2) . . ? C27 H27A 0.959(2) . . ? C27 H27B 0.960(2) . . ? C29 H29A 0.959(2) . . ? C29 H29B 0.960(2) . . ? C30 H30A 0.961(2) . . ? C30 H30B 0.961(2) . . ? C32 H32A 0.9610(10) . . ? C32 H32B 0.961(2) . . ? C33 H33A 0.882(9) . . ? C36 H36 0.920(7) . . ? C38 H38 0.853(7) . . ? C39 H39 0.9600(10) . . ? C41 H41A 0.9590(10) . . ? C41 H41B 0.9590(10) . . ? C41 H41C 0.9610(10) . . ? C42 H42C 0.730(7) . . ? C49 H49 0.9600(10) . . ? C50 H50 0.9600(10) . . ? C51 H51 0.960(2) . . ? C52 H52 0.9600(10) . . ? C58 H58 0.9600(10) . . ? C59 H59 0.9600(10) . . ? C60 H60 0.900(10) . . ? C62 H62 0.9600(10) . . ? C65 H65A 0.960(2) . . ? C65 H65B 0.960(2) . . ? C65 H65C 0.9600(10) . . ? C66 H66A 0.959(2) . . ? C66 H66B 0.960(2) . . ? C66 H66C 0.960(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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 O6 C7 113.30(10) . . . ? C8 O9 C10 116.9(2) . . . ? C11 O12 C13 113.7(2) . . . ? C21 O22 C23 117.5(2) . . . ? C24 O25 C26 120.2(2) . . . ? C27 O28 C29 115.4(2) . . . ? C30 O31 C32 112.3(2) . . . ? C33 O34 C35 118.5(2) . . . ? C4 N3 C40 112.60(10) . . . ? C4 N3 C41 112.3(2) . . . ? C40 N3 C41 111.8(2) . . . ? C14 N15 C16 116.0(2) . . . ? C19 N43 C44 130.7(2) . . . ? C44 N46 C47 133.0(2) . . . ? C37 N53 C54 125.3(2) . . . ? C54 N56 C57 131.9(2) . . . ? O6 C7 C8 112.0(2) . . . ? O9 C8 C7 108.3(2) . . . ? O9 C10 C11 116.9(2) . . . ? O12 C11 C10 115.9(2) . . . ? N15 C16 C17 124.1(2) . . . ? N15 C16 C21 118.1(2) . . . ? C17 C16 C21 117.8(2) . . . ? C16 C17 C18 123.4(2) . . . ? C17 C18 C19 118.1(2) . . . ? N43 C19 C18 123.9(2) . . . ? N43 C19 C20 116.1(2) . . . ? C18 C19 C20 119.9(2) . . . ? C19 C20 C21 122.2(2) . . . ? O22 C21 C16 116.9(2) . . . ? O22 C21 C20 124.7(2) . . . ? C16 C21 C20 118.4(2) . . . ? O25 C26 C27 126.0(3) . . . ? O28 C27 C26 119.8(3) . . . ? O28 C29 C30 116.1(2) . . . ? O31 C30 C29 113.3(2) . . . ? O31 C32 C33 113.0(2) . . . ? O34 C33 C32 107.9(2) . . . ? O34 C35 C36 124.5(2) . . . ? O34 C35 C40 115.6(2) . . . ? C36 C35 C40 119.9(2) . . . ? C35 C36 C37 121.4(2) . . . ? N53 C37 C36 120.0(2) . . . ? N53 C37 C38 121.2(2) . . . ? C36 C37 C38 118.8(2) . . . ? C37 C38 C39 120.7(2) . . . ? C38 C39 C40 121.6(2) . . . ? N3 C40 C35 118.5(2) . . . ? N3 C40 C39 124.0(2) . . . ? C35 C40 C39 117.5(2) . . . ? S45 C44 N43 123.9(2) . . . ? S45 C44 N46 125.7(2) . . . ? N43 C44 N46 110.4(2) . . . ? N46 C47 C48 115.2(2) . . . ? N46 C47 C52 125.4(2) . . . ? C48 C47 C52 119.4(2) . . . ? C47 C48 C49 117.4(2) . . . ? C48 C49 C50 122.9(2) . . . ? C49 C50 C51 120.0(2) . . . ? C50 C51 C52 120.2(2) . . . ? C47 C52 C51 120.2(2) . . . ? S55 C54 N53 124.70(10) . . . ? S55 C54 N56 125.30(10) . . . ? N53 C54 N56 110.0(2) . . . ? N56 C57 C58 116.4(2) . . . ? N56 C57 C62 124.5(2) . . . ? C58 C57 C62 119.1(2) . . . ? C57 C58 C59 119.8(2) . . . ? C58 C59 C60 120.5(2) . . . ? C59 C60 C61 119.6(2) . . . ? C60 C61 C62 120.9(2) . . . ? C57 C62 C61 120.2(2) . . . ? O63 C64 C65 122.1(2) . . . ? O63 C64 C66 119.8(2) . . . ? C65 C64 C66 118.1(2) . . . ? C19 N43 H43 115.5(6) . . . ? C44 N43 H43 112.4(6) . . . ? C44 N46 H46 108.4(2) . . . ? C47 N46 H46 118.6(2) . . . ? C37 N53 H53 115.6(2) . . . ? C54 N53 H53 119.1(2) . . . ? C54 N56 H56 107.5(2) . . . ? C57 N56 H56 120.5(2) . . . ? O6 C5 H5A 110.6(2) . . . ? O6 C5 H5B 110.3(2) . . . ? H5A C5 H5B 109.4(2) . . . ? O6 C7 H7A 108.1(2) . . . ? O6 C7 H7B 109.0(2) . . . ? C8 C7 H7A 108.7(2) . . . ? C8 C7 H7B 109.6(2) . . . ? H7A C7 H7B 109.5(2) . . . ? O9 C8 H8B 98.6(11) . . . ? C7 C8 H8B 113.3(12) . . . ? O9 C10 H10A 107.8(2) . . . ? O9 C10 H10B 105.5(2) . . . ? C11 C10 H10A 112.9(2) . . . ? C11 C10 H10B 103.7(2) . . . ? H10A C10 H10B 109.6(2) . . . ? O12 C11 H11A 109.8(2) . . . ? O12 C11 H11B 106.0(2) . . . ? C10 C11 H11A 111.4(2) . . . ? C10 C11 H11B 103.8(2) . . . ? H11A C11 H11B 109.5(2) . . . ? O12 C13 H13A 109.2(2) . . . ? O12 C13 H13B 109.7(2) . . . ? H13A C13 H13B 109.5(2) . . . ? N15 C14 H14A 113.6(7) . . . ? C16 C17 H17 123.0(6) . . . ? C18 C17 H17 113.6(6) . . . ? C17 C18 H18 120.6(2) . . . ? C19 C18 H18 121.3(2) . . . ? C19 C20 H20 121.1(2) . . . ? C21 C20 H20 116.7(2) . . . ? O22 C23 H23A 107.9(7) . . . ? O22 C23 H23B 104.0(6) . . . ? H23A C23 H23B 116.6(9) . . . ? O25 C24 H24A 102.6(7) . . . ? O25 C26 H26A 98.2(2) . . . ? O25 C26 H26B 107.6(3) . . . ? C27 C26 H26A 101.3(3) . . . ? C27 C26 H26B 112.0(3) . . . ? H26A C26 H26B 109.6(3) . . . ? O28 C27 H27A 102.3(3) . . . ? O28 C27 H27B 105.1(3) . . . ? C26 C27 H27A 102.4(3) . . . ? C26 C27 H27B 116.5(4) . . . ? H27A C27 H27B 109.5(2) . . . ? O28 C29 H29A 105.5(2) . . . ? O28 C29 H29B 111.2(2) . . . ? C30 C29 H29A 101.4(2) . . . ? C30 C29 H29B 112.4(3) . . . ? H29A C29 H29B 109.5(2) . . . ? O31 C30 H30A 108.4(2) . . . ? O31 C30 H30B 110.5(2) . . . ? C29 C30 H30A 101.5(2) . . . ? C29 C30 H30B 113.3(3) . . . ? H30A C30 H30B 109.3(2) . . . ? O31 C32 H32A 109.5(2) . . . ? O31 C32 H32B 107.3(2) . . . ? C33 C32 H32A 110.4(2) . . . ? C33 C32 H32B 107.1(2) . . . ? H32A C32 H32B 109.3(2) . . . ? O34 C33 H33A 109.0(8) . . . ? C32 C33 H33A 113.9(8) . . . ? C35 C36 H36 119.0(6) . . . ? C37 C36 H36 119.4(6) . . . ? C37 C38 H38 119.0(7) . . . ? C39 C38 H38 118.7(7) . . . ? C38 C39 H39 121.2(2) . . . ? C40 C39 H39 117.3(2) . . . ? N3 C41 H41A 110.4(2) . . . ? N3 C41 H41B 110.2(2) . . . ? N3 C41 H41C 107.7(2) . . . ? H41A C41 H41B 109.6(2) . . . ? H41A C41 H41C 109.5(2) . . . ? H41B C41 H41C 109.5(2) . . . ? C48 C49 H49 117.9(2) . . . ? C50 C49 H49 119.2(3) . . . ? C49 C50 H50 119.5(3) . . . ? C51 C50 H50 120.5(3) . . . ? C50 C51 H51 119.5(2) . . . ? C52 C51 H51 120.3(2) . . . ? C47 C52 H52 120.9(2) . . . ? C51 C52 H52 119.0(2) . . . ? C57 C58 H58 121.0(2) . . . ? C59 C58 H58 119.2(2) . . . ? C58 C59 H59 119.8(2) . . . ? C60 C59 H59 119.8(2) . . . ? C59 C60 H60 126.6(9) . . . ? C61 C60 H60 113.6(9) . . . ? C57 C62 H62 121.0(2) . . . ? C61 C62 H62 118.7(2) . . . ? C64 C65 H65A 108.1(2) . . . ? C64 C65 H65B 109.0(2) . . . ? C64 C65 H65C 111.4(2) . . . ? H65A C65 H65B 109.4(2) . . . ? H65A C65 H65C 109.4(2) . . . ? H65B C65 H65C 109.4(2) . . . ? C64 C66 H66A 110.8(2) . . . ? C64 C66 H66B 110.9(2) . . . ? C64 C66 H66C 106.6(3) . . . ? H66A C66 H66B 109.5(3) . . . ? H66A C66 H66C 109.5(3) . . . ? H66B C66 H66C 109.4(2) . . . ? #==END