# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Cheng Li' _publ_contact_author_email CHLI@NJU.EDU.CN _publ_section_title ; Synthesis, structure and chiroptical study of chiral macrocyclic imine nickel(II) coordination compounds derived from camphor ; loop_ _publ_author_name 'Cheng Li.' 'Yi-Zhi Li.' 'Atsuya Muranaka' 'Tao Wu.' 'Xiao-Zeng You.' 'Muri Yukie' ; Zhao-Gui Zhang ; data_80320am _database_code_depnum_ccdc_archive 'CCDC 753362' #TrackingRef 'nju01 RMC.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C24 H40 N4 O4 S2), 0.7(H2 O), 0.3(H O), 0.3(H)' _chemical_formula_sum 'C48 H82 N8 O9 S4' _chemical_formula_weight 1043.46 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1) ' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.9463(11) _cell_length_b 28.733(3) _cell_length_c 11.1330(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.905(2) _cell_angle_gamma 90.00 _cell_volume 2861.5(6) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 4575 _cell_measurement_theta_min 2.11 _cell_measurement_theta_max 24.36 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.211 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1124 _exptl_absorpt_coefficient_mu 0.222 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.95 _exptl_absorpt_correction_T_max 0.97 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Aepex CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21142 _diffrn_reflns_av_R_equivalents 0.0230 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 26.00 _reflns_number_total 11133 _reflns_number_gt 10426 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.04P)^2^+0.55P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.09(4) _chemical_absolute_configuration unk _refine_ls_number_reflns 11133 _refine_ls_number_parameters 648 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0378 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0791 _refine_ls_wR_factor_gt 0.0782 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0882(2) 0.68644(7) 0.4006(2) 0.0325(5) Uani 1 1 d . . . C2 C 0.0257(2) 0.65326(7) 0.49224(18) 0.0306(4) Uani 1 1 d . . . C3 C -0.1317(2) 0.66866(8) 0.51220(19) 0.0358(5) Uani 1 1 d . . . H3A H -0.2015 0.6437 0.4938 0.043 Uiso 1 1 calc R . . H3B H -0.1450 0.6783 0.5949 0.043 Uiso 1 1 calc R . . C4 C -0.1546(3) 0.70804(9) 0.4300(2) 0.0404(5) Uani 1 1 d . . . H4A H -0.2594 0.7151 0.4106 0.049 Uiso 1 1 calc R . . C5 C -0.0636(3) 0.74928(9) 0.4845(2) 0.0414(5) Uani 1 1 d . . . H5A H -0.0835 0.7780 0.4415 0.050 Uiso 1 1 calc R . . H5B H -0.0854 0.7536 0.5689 0.050 Uiso 1 1 calc R . . C6 C 0.1001(3) 0.73274(8) 0.4671(2) 0.0387(5) Uani 1 1 d . . . H6A H 0.1553 0.7552 0.4202 0.046 Uiso 1 1 calc R . . H6B H 0.1506 0.7287 0.5441 0.046 Uiso 1 1 calc R . . C7 C -0.0590(3) 0.69465(8) 0.3216(2) 0.0372(5) Uani 1 1 d . . . C8 C -0.1109(3) 0.65000(9) 0.2584(2) 0.0424(6) Uani 1 1 d . . . H8A H -0.0831 0.6235 0.3064 0.064 Uiso 1 1 calc R . . H8B H -0.0646 0.6478 0.1814 0.064 Uiso 1 1 calc R . . H8C H -0.2176 0.6507 0.2477 0.064 Uiso 1 1 calc R . . C9 C -0.0334(3) 0.73195(9) 0.2226(2) 0.0460(6) Uani 1 1 d . . . H9A H 0.0348 0.7200 0.1644 0.069 Uiso 1 1 calc R . . H9B H 0.0080 0.7595 0.2586 0.069 Uiso 1 1 calc R . . H9C H -0.1270 0.7393 0.1837 0.069 Uiso 1 1 calc R . . C10 C 0.2213(2) 0.67175(8) 0.33033(18) 0.0339(4) Uani 1 1 d . . . H10A H 0.2303 0.6932 0.2636 0.041 Uiso 1 1 calc R . . H10B H 0.1990 0.6414 0.2963 0.041 Uiso 1 1 calc R . . C11 C 0.4415(3) 0.58009(8) 0.4025(2) 0.0402(5) Uani 1 1 d . . . H11A H 0.5430 0.5833 0.3742 0.048 Uiso 1 1 calc R . . H11B H 0.3761 0.5824 0.3324 0.048 Uiso 1 1 calc R . . C12 C 0.4266(3) 0.53141(8) 0.45045(19) 0.0389(5) Uani 1 1 d . . . H12A H 0.3409 0.5172 0.4107 0.047 Uiso 1 1 calc R . . H12B H 0.5142 0.5140 0.4264 0.047 Uiso 1 1 calc R . . C13 C 0.6034(2) 0.57103(8) 0.72749(18) 0.0322(4) Uani 1 1 d . . . H13A H 0.7090 0.5701 0.7483 0.039 Uiso 1 1 calc R . . H13B H 0.5902 0.5943 0.6651 0.039 Uiso 1 1 calc R . . C14 C 0.5185(3) 0.58736(8) 0.8384(2) 0.0361(5) Uani 1 1 d . . . C15 C 0.3569(2) 0.59962(7) 0.82860(18) 0.0331(5) Uani 1 1 d . . . C16 C 0.3202(3) 0.63037(8) 0.9394(2) 0.0379(5) Uani 1 1 d . . . H16A H 0.2776 0.6601 0.9154 0.046 Uiso 1 1 calc R . . H16B H 0.2524 0.6147 0.9932 0.046 Uiso 1 1 calc R . . C17 C 0.4706(3) 0.63602(9) 0.9946(2) 0.0449(6) Uani 1 1 d . . . H17 H 0.4801 0.6636 1.0458 0.054 Uiso 1 1 calc R . . C18 C 0.5075(3) 0.58935(9) 1.0616(2) 0.0445(6) Uani 1 1 d . . . H18A H 0.4234 0.5786 1.1080 0.053 Uiso 1 1 calc R . . H18B H 0.5945 0.5926 1.1141 0.053 Uiso 1 1 calc R . . C19 C 0.5395(2) 0.55586(8) 0.95363(18) 0.0342(5) Uani 1 1 d . . . H19A H 0.4696 0.5301 0.9522 0.041 Uiso 1 1 calc R . . H19B H 0.6405 0.5436 0.9590 0.041 Uiso 1 1 calc R . . C20 C 0.5840(3) 0.63492(7) 0.88940(19) 0.0348(5) Uani 1 1 d . . . C21 C 0.7476(3) 0.63389(9) 0.9220(2) 0.0430(5) Uani 1 1 d . . . H21A H 0.7725 0.6608 0.9692 0.065 Uiso 1 1 calc R . . H21B H 0.8053 0.6339 0.8500 0.065 Uiso 1 1 calc R . . H21C H 0.7695 0.6063 0.9675 0.065 Uiso 1 1 calc R . . C22 C 0.5529(3) 0.67553(8) 0.7984(2) 0.0420(5) Uani 1 1 d . . . H22A H 0.4488 0.6757 0.7761 0.063 Uiso 1 1 calc R . . H22B H 0.6119 0.6711 0.7281 0.063 Uiso 1 1 calc R . . H22C H 0.5790 0.7047 0.8354 0.063 Uiso 1 1 calc R . . C23 C 0.1131(2) 0.60129(8) 0.75190(19) 0.0337(5) Uani 1 1 d . . . H23A H 0.1099 0.6344 0.7690 0.040 Uiso 1 1 calc R . . H23B H 0.0627 0.5850 0.8159 0.040 Uiso 1 1 calc R . . C24 C 0.0354(3) 0.59151(10) 0.6331(2) 0.0447(6) Uani 1 1 d . . . H24A H 0.0471 0.5589 0.6126 0.054 Uiso 1 1 calc R . . H24B H -0.0706 0.5980 0.6396 0.054 Uiso 1 1 calc R . . C25 C -0.0162(2) 0.95062(7) 1.04693(18) 0.0297(4) Uani 1 1 d . . . C26 C 0.1503(2) 0.93794(7) 1.03556(18) 0.0301(4) Uani 1 1 d . . . C27 C 0.1809(3) 0.90457(9) 1.1405(2) 0.0404(5) Uani 1 1 d . . . H27A H 0.2132 0.8744 1.1119 0.049 Uiso 1 1 calc R . . H27B H 0.2567 0.9170 1.1949 0.049 Uiso 1 1 calc R . . C28 C 0.0299(3) 0.90107(9) 1.2021(2) 0.0407(5) Uani 1 1 d . . . H28 H 0.0185 0.8737 1.2537 0.049 Uiso 1 1 calc R . . C29 C 0.0011(3) 0.94796(9) 1.2646(2) 0.0440(6) Uani 1 1 d . . . H29A H -0.0850 0.9459 1.3162 0.053 Uiso 1 1 calc R . . H29B H 0.0874 0.9574 1.3125 0.053 Uiso 1 1 calc R . . C30 C -0.0277(3) 0.98207(8) 1.1631(2) 0.0426(6) Uani 1 1 d . . . H30A H 0.0469 1.0066 1.1631 0.051 Uiso 1 1 calc R . . H30B H -0.1261 0.9960 1.1689 0.051 Uiso 1 1 calc R . . C31 C -0.0818(3) 0.90309(8) 1.0918(2) 0.0369(5) Uani 1 1 d . . . C32 C -0.0584(3) 0.86302(8) 1.0034(2) 0.0383(5) Uani 1 1 d . . . H32A H -0.0922 0.8345 1.0385 0.057 Uiso 1 1 calc R . . H32B H 0.0460 0.8605 0.9855 0.057 Uiso 1 1 calc R . . H32C H -0.1142 0.8690 0.9307 0.057 Uiso 1 1 calc R . . C33 C -0.2478(3) 0.90624(9) 1.1311(2) 0.0426(5) Uani 1 1 d . . . H33A H -0.2558 0.9279 1.1964 0.064 Uiso 1 1 calc R . . H33B H -0.2812 0.8761 1.1565 0.064 Uiso 1 1 calc R . . H33C H -0.3087 0.9167 1.0646 0.064 Uiso 1 1 calc R . . C34 C -0.0991(2) 0.96856(8) 0.9354(2) 0.0345(5) Uani 1 1 d . . . H34A H -0.2046 0.9700 0.9539 0.041 Uiso 1 1 calc R . . H34B H -0.0879 0.9455 0.8724 0.041 Uiso 1 1 calc R . . C35 C 0.0962(3) 1.01233(9) 0.6643(2) 0.0408(5) Uani 1 1 d . . . H35A H 0.1967 1.0192 0.6381 0.049 Uiso 1 1 calc R . . H35B H 0.0309 1.0362 0.6311 0.049 Uiso 1 1 calc R . . C36 C 0.0488(3) 0.96501(9) 0.6087(2) 0.0461(6) Uani 1 1 d . . . H36A H -0.0590 0.9654 0.5977 0.055 Uiso 1 1 calc R . . H36B H 0.0919 0.9629 0.5295 0.055 Uiso 1 1 calc R . . C37 C 0.2809(2) 0.87603(7) 0.52683(19) 0.0314(4) Uani 1 1 d . . . H37A H 0.2712 0.8567 0.4556 0.038 Uiso 1 1 calc R . . H37B H 0.3010 0.9075 0.4998 0.038 Uiso 1 1 calc R . . C38 C 0.4190(2) 0.85916(7) 0.59815(19) 0.0306(4) Uani 1 1 d . . . C39 C 0.4765(3) 0.89141(8) 0.6972(2) 0.0360(5) Uani 1 1 d . . . C40 C 0.6360(3) 0.87715(8) 0.7147(2) 0.0385(5) Uani 1 1 d . . . H40A H 0.6535 0.8659 0.7959 0.046 Uiso 1 1 calc R . . H40B H 0.7023 0.9032 0.7002 0.046 Uiso 1 1 calc R . . C41 C 0.6622(3) 0.83816(7) 0.6230(2) 0.0371(5) Uani 1 1 d . . . H41 H 0.7671 0.8327 0.6030 0.045 Uiso 1 1 calc R . . C42 C 0.5592(2) 0.85552(8) 0.5145(2) 0.0351(5) Uani 1 1 d . . . C43 C 0.5794(2) 0.79612(8) 0.6650(2) 0.0373(5) Uani 1 1 d . . . H43B H 0.6065 0.7888 0.7477 0.045 Uiso 1 1 calc R . . H43A H 0.6015 0.7694 0.6151 0.045 Uiso 1 1 calc R . . C44 C 0.4103(2) 0.80941(7) 0.65398(18) 0.0316(4) Uani 1 1 d . . . H44A H 0.3563 0.7881 0.6015 0.038 Uiso 1 1 calc R . . H44B H 0.3633 0.8100 0.7319 0.038 Uiso 1 1 calc R . . C45 C 0.4718(2) 0.94777(9) 0.8476(2) 0.0389(5) Uani 1 1 d . . . H45A H 0.4653 0.9809 0.8317 0.047 Uiso 1 1 calc R . . H45B H 0.5765 0.9394 0.8557 0.047 Uiso 1 1 calc R . . C46 C 0.3916(2) 0.93636(8) 0.96180(19) 0.0347(5) Uani 1 1 d . . . H46A H 0.3958 0.9030 0.9755 0.042 Uiso 1 1 calc R . . H46B H 0.4419 0.9516 1.0288 0.042 Uiso 1 1 calc R . . C47 C 0.6115(3) 0.90185(8) 0.4662(2) 0.0416(5) Uani 1 1 d . . . H47A H 0.7183 0.9015 0.4590 0.062 Uiso 1 1 calc R . . H47B H 0.5831 0.9262 0.5202 0.062 Uiso 1 1 calc R . . H47C H 0.5662 0.9072 0.3887 0.062 Uiso 1 1 calc R . . C48 C 0.5431(3) 0.82039(8) 0.4127(2) 0.0370(5) Uani 1 1 d . . . H48A H 0.4932 0.8348 0.3454 0.055 Uiso 1 1 calc R . . H48B H 0.4854 0.7943 0.4394 0.055 Uiso 1 1 calc R . . H48C H 0.6403 0.8100 0.3893 0.055 Uiso 1 1 calc R . . N1 N 0.4131(2) 0.61794(6) 0.47333(17) 0.0356(4) Uani 1 1 d . . . H1 H 0.4014 0.6156 0.5496 0.043 Uiso 1 1 calc R . . N2 N 0.4100(2) 0.52519(7) 0.57822(16) 0.0383(4) Uani 1 1 d . . . H2 H 0.3223 0.5266 0.6085 0.046 Uiso 1 1 calc R . . N3 N 0.0994(2) 0.62076(7) 0.53801(16) 0.0343(4) Uani 1 1 d . . . N4 N 0.2705(2) 0.58556(6) 0.74568(15) 0.0332(4) Uani 1 1 d . . . N5 N 0.0944(2) 1.01613(7) 0.79238(17) 0.0387(4) Uani 1 1 d . . . H5 H 0.1792 1.0135 0.8291 0.046 Uiso 1 1 calc R . . N6 N 0.0872(2) 0.92406(7) 0.67205(16) 0.0351(4) Uani 1 1 d . . . H6 H 0.1753 0.9292 0.7098 0.042 Uiso 1 1 d R . . N7 N 0.23205(19) 0.95157(6) 0.95638(16) 0.0325(4) Uani 1 1 d . . . N8 N 0.40153(19) 0.92131(7) 0.74656(16) 0.0338(4) Uani 1 1 d . . . O1 O 0.41288(18) 0.70372(6) 0.49235(14) 0.0405(4) Uani 1 1 d . . . O2 O 0.50790(18) 0.66567(6) 0.30459(14) 0.0410(4) Uani 1 1 d . . . O3 O 0.50714(17) 0.48684(5) 0.75805(13) 0.0350(3) Uani 1 1 d . . . O4 O 0.66912(19) 0.50240(6) 0.59197(15) 0.0434(4) Uani 1 1 d . . . O5 O 0.00252(18) 1.05333(6) 0.97089(14) 0.0391(3) Uani 1 1 d . . . O6 O -0.16334(18) 1.03989(6) 0.79585(15) 0.0423(4) Uani 1 1 d . . . O7 O 0.09698(18) 0.83929(6) 0.68654(16) 0.0439(4) Uani 1 1 d . . . O8 O -0.00919(17) 0.87879(6) 0.50302(14) 0.0408(4) Uani 1 1 d . . . O9 O 0.5768(5) 0.27436(12) 0.8922(4) 0.0408(9) Uani 0.40 1 d P . . H9D H 0.6585 0.2789 0.9303 0.049 Uiso 0.40 1 d PR . . H9F H 0.5905 0.2546 0.8365 0.049 Uiso 0.40 1 d PR . . O10 O 0.7468(5) 0.24816(15) 0.0208(4) 0.0276(9) Uani 0.30 1 d P . . H10D H 0.6640 0.2508 -0.0172 0.033 Uiso 0.30 1 d PR . . H10E H 0.8057 0.2696 -0.0011 0.033 Uiso 0.30 1 d PR . . O11 O 0.0091(7) 0.2475(2) 0.1407(5) 0.0488(14) Uani 0.30 1 d P . . H11F H 0.1020 0.2475 0.1257 0.059 Uiso 0.30 1 d PR . . H11D H -0.0110 0.2245 0.1859 0.059 Uiso 0.30 1 d PR . . S1 S 0.40303(5) 0.667832(17) 0.40278(5) 0.03111(11) Uani 1 1 d . . . S2 S 0.10156(6) 0.876475(19) 0.60011(5) 0.03241(11) Uani 1 1 d . . . S3 S -0.04602(6) 1.024665(17) 0.87420(4) 0.03153(11) Uani 1 1 d . . . S4 S 0.55234(6) 0.515601(18) 0.66530(4) 0.03346(12) Uani 1 1 d . . . 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 C1 0.0267(10) 0.0297(10) 0.0408(12) 0.0026(9) -0.0127(9) -0.0002(8) C2 0.0271(10) 0.0366(11) 0.0278(10) -0.0052(8) -0.0075(8) -0.0028(8) C3 0.0278(10) 0.0430(12) 0.0366(11) -0.0129(10) -0.0031(8) 0.0005(9) C4 0.0307(11) 0.0457(13) 0.0446(13) -0.0121(10) -0.0106(10) 0.0044(10) C5 0.0441(13) 0.0394(12) 0.0406(13) -0.0084(10) -0.0047(10) 0.0023(10) C6 0.0400(13) 0.0338(11) 0.0420(12) -0.0053(10) -0.0078(10) -0.0053(9) C7 0.0365(12) 0.0381(12) 0.0366(12) -0.0036(9) -0.0148(9) 0.0077(9) C8 0.0423(13) 0.0475(14) 0.0371(12) -0.0121(10) -0.0129(10) -0.0012(10) C9 0.0441(14) 0.0455(14) 0.0479(14) 0.0043(11) -0.0128(11) 0.0169(10) C10 0.0323(11) 0.0459(12) 0.0234(9) 0.0028(9) -0.0068(8) -0.0036(9) C11 0.0430(13) 0.0385(13) 0.0395(12) -0.0036(10) 0.0082(10) -0.0053(10) C12 0.0480(13) 0.0354(12) 0.0329(11) -0.0045(9) -0.0109(9) 0.0079(9) C13 0.0314(11) 0.0383(11) 0.0270(10) -0.0073(9) -0.0004(8) -0.0061(9) C14 0.0451(13) 0.0312(11) 0.0318(11) -0.0083(9) -0.0007(9) 0.0007(9) C15 0.0396(12) 0.0322(11) 0.0278(10) -0.0031(8) 0.0083(9) -0.0007(9) C16 0.0500(13) 0.0332(11) 0.0311(11) -0.0015(9) 0.0176(10) -0.0057(9) C17 0.0564(15) 0.0482(14) 0.0305(11) -0.0111(10) 0.0112(11) -0.0106(11) C18 0.0469(14) 0.0551(15) 0.0315(11) -0.0020(11) 0.0019(10) -0.0153(11) C19 0.0307(11) 0.0391(12) 0.0328(11) -0.0004(9) -0.0033(8) -0.0157(9) C20 0.0422(12) 0.0296(11) 0.0326(11) -0.0060(9) 0.0023(9) 0.0015(9) C21 0.0476(14) 0.0461(14) 0.0352(12) -0.0026(10) -0.0037(10) -0.0078(10) C22 0.0490(13) 0.0356(12) 0.0414(12) 0.0079(10) -0.0020(10) -0.0060(10) C23 0.0379(11) 0.0342(11) 0.0294(10) 0.0066(9) 0.0131(9) -0.0013(9) C24 0.0370(13) 0.0556(15) 0.0416(13) 0.0145(11) 0.0016(10) -0.0089(11) C25 0.0314(11) 0.0302(10) 0.0273(10) -0.0002(8) -0.0028(8) 0.0035(8) C26 0.0319(11) 0.0292(10) 0.0289(10) -0.0041(8) -0.0087(8) 0.0023(8) C27 0.0389(12) 0.0467(13) 0.0353(12) 0.0048(10) -0.0129(10) 0.0062(10) C28 0.0465(14) 0.0431(12) 0.0322(11) 0.0058(10) -0.0098(10) -0.0055(10) C29 0.0457(14) 0.0585(15) 0.0278(11) -0.0041(10) 0.0034(10) -0.0093(12) C30 0.0499(14) 0.0407(13) 0.0377(12) -0.0082(10) 0.0121(10) 0.0014(10) C31 0.0360(12) 0.0381(12) 0.0362(12) 0.0043(9) -0.0095(9) -0.0059(9) C32 0.0378(12) 0.0360(12) 0.0409(12) 0.0030(9) -0.0087(9) -0.0144(9) C33 0.0385(12) 0.0521(14) 0.0371(12) 0.0156(11) -0.0047(10) -0.0060(11) C34 0.0271(10) 0.0401(12) 0.0360(11) 0.0073(9) -0.0062(8) -0.0032(9) C35 0.0391(12) 0.0453(13) 0.0382(11) 0.0067(10) 0.0134(9) 0.0081(10) C36 0.0469(14) 0.0523(15) 0.0390(13) 0.0013(11) -0.0019(10) 0.0162(12) C37 0.0320(10) 0.0242(9) 0.0380(11) 0.0023(9) 0.0046(8) 0.0009(8) C38 0.0296(11) 0.0307(10) 0.0317(11) -0.0028(8) 0.0065(8) -0.0011(8) C39 0.0309(11) 0.0412(12) 0.0362(11) -0.0050(9) 0.0091(9) -0.0088(9) C40 0.0377(12) 0.0385(12) 0.0392(11) -0.0032(10) -0.0015(9) -0.0033(10) C41 0.0308(12) 0.0294(11) 0.0510(14) -0.0019(9) -0.0033(10) -0.0044(8) C42 0.0314(11) 0.0352(11) 0.0387(12) 0.0032(9) 0.0069(9) -0.0003(9) C43 0.0326(12) 0.0317(11) 0.0475(13) 0.0074(9) -0.0060(10) -0.0030(9) C44 0.0352(11) 0.0348(11) 0.0247(10) 0.0041(8) -0.0036(8) -0.0039(9) C45 0.0294(11) 0.0503(14) 0.0369(12) -0.0129(10) -0.0045(9) -0.0118(10) C46 0.0326(11) 0.0395(12) 0.0316(11) -0.0114(9) -0.0052(9) 0.0089(9) C47 0.0474(14) 0.0327(11) 0.0452(13) 0.0057(10) 0.0213(11) 0.0057(10) C48 0.0355(12) 0.0383(12) 0.0375(12) 0.0009(9) 0.0097(9) 0.0069(9) N1 0.0361(10) 0.0353(10) 0.0354(10) 0.0041(8) 0.0036(8) 0.0062(8) N2 0.0401(10) 0.0366(10) 0.0378(9) -0.0019(8) -0.0121(8) -0.0071(8) N3 0.0316(9) 0.0406(10) 0.0307(9) 0.0057(8) 0.0046(7) 0.0010(8) N4 0.0420(10) 0.0358(10) 0.0218(8) 0.0069(7) 0.0024(7) 0.0044(8) N5 0.0378(10) 0.0381(10) 0.0404(10) 0.0028(9) 0.0046(8) -0.0021(8) N6 0.0269(9) 0.0458(11) 0.0324(9) 0.0015(8) -0.0003(7) 0.0058(8) N7 0.0287(9) 0.0349(9) 0.0339(9) -0.0059(8) -0.0006(7) 0.0037(7) N8 0.0272(9) 0.0415(10) 0.0327(9) -0.0096(8) 0.0027(7) -0.0074(7) O1 0.0421(9) 0.0382(9) 0.0409(9) -0.0011(7) -0.0121(7) -0.0082(7) O2 0.0390(8) 0.0470(9) 0.0370(8) 0.0110(7) 0.0039(7) -0.0047(7) O3 0.0431(9) 0.0289(8) 0.0327(8) -0.0068(6) -0.0075(6) 0.0057(6) O4 0.0444(9) 0.0417(9) 0.0445(9) -0.0138(7) 0.0060(7) 0.0031(7) O5 0.0385(8) 0.0414(9) 0.0377(8) -0.0008(7) 0.0059(7) -0.0020(7) O6 0.0408(9) 0.0414(9) 0.0445(9) 0.0071(7) -0.0088(7) 0.0161(7) O7 0.0358(9) 0.0471(9) 0.0488(10) 0.0180(8) -0.0021(7) -0.0076(7) O8 0.0349(8) 0.0506(9) 0.0366(8) 0.0022(8) -0.0095(6) -0.0095(7) O9 0.049(2) 0.0178(17) 0.056(2) 0.0022(16) 0.0120(19) 0.0066(16) O10 0.031(2) 0.022(2) 0.030(2) 0.0037(18) -0.0027(19) -0.0068(18) O11 0.047(3) 0.043(3) 0.056(4) 0.011(3) 0.000(3) 0.021(3) S1 0.0252(2) 0.0320(3) 0.0360(3) 0.0021(2) -0.00018(19) -0.0078(2) S2 0.0257(2) 0.0405(3) 0.0309(3) 0.0047(2) -0.00398(19) -0.0071(2) S3 0.0372(3) 0.0274(2) 0.0300(2) 0.0034(2) 0.00002(19) 0.0157(2) S4 0.0388(3) 0.0324(3) 0.0291(2) -0.0067(2) -0.0041(2) 0.0095(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 C1 C10 1.496(3) . ? C1 C2 1.510(3) . ? C1 C6 1.525(3) . ? C1 C7 1.590(3) . ? C2 N3 1.247(3) . ? C2 C3 1.496(3) . ? C3 C4 1.468(3) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C7 1.539(3) . ? C4 C5 1.556(3) . ? C4 H4A 0.9800 . ? C5 C6 1.555(3) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.532(3) . ? C7 C9 1.557(3) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 S1 1.807(2) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N1 1.369(3) . ? C11 C12 1.504(3) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N2 1.444(3) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.533(3) . ? C13 S4 1.793(2) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.490(3) . ? C14 C19 1.579(3) . ? C14 C20 1.588(3) . ? C15 N4 1.262(3) . ? C15 C16 1.557(3) . ? C16 C17 1.479(4) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C20 1.562(3) . ? C17 C18 1.567(4) . ? C17 H17 0.9800 . ? C18 C19 1.569(3) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.503(3) . ? C20 C22 1.567(3) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 N4 1.481(3) . ? C23 C24 1.511(3) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 N3 1.475(3) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C34 1.526(3) . ? C25 C26 1.540(3) . ? C25 C31 1.571(3) . ? C25 C30 1.582(3) . ? C26 N7 1.219(3) . ? C26 C27 1.533(3) . ? C27 C28 1.528(4) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.540(4) . ? C28 C31 1.572(3) . ? C28 H28 0.9800 . ? C29 C30 1.515(3) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.531(3) . ? C31 C33 1.558(3) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 S3 1.816(2) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 N5 1.431(3) . ? C35 C36 1.550(4) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 N6 1.411(3) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.536(3) . ? C37 S2 1.812(2) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.523(3) . ? C38 C44 1.561(3) . ? C38 C42 1.578(3) . ? C39 N8 1.226(3) . ? C39 C40 1.495(3) . ? C40 C41 1.536(3) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C43 1.496(3) . ? C41 C42 1.588(3) . ? C41 H41 0.9800 . ? C42 C47 1.512(3) . ? C42 C48 1.523(3) . ? C43 C44 1.564(3) . ? C43 H43B 0.9700 . ? C43 H43A 0.9700 . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 N8 1.488(3) . ? C45 C46 1.506(3) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 N7 1.493(3) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? N1 S1 1.6365(19) . ? N1 H1 0.8600 . ? N2 S4 1.6118(18) . ? N2 H2 0.8600 . ? N5 S3 1.5822(19) . ? N5 H5 0.8600 . ? N6 S2 1.591(2) . ? N6 H6 0.9000 . ? O1 S1 1.4362(17) . ? O2 S1 1.4531(16) . ? O3 S4 1.3879(17) . ? O4 S4 1.3888(17) . ? O5 S3 1.4181(16) . ? O6 S3 1.4230(15) . ? O7 S2 1.4389(17) . ? O8 S2 1.4562(15) . ? O9 H9D 0.8500 . ? O9 H9F 0.8500 . ? O10 H10D 0.8500 . ? O10 H10E 0.8500 . ? O11 H11F 0.8500 . ? O11 H11D 0.8500 . ? 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 C10 C1 C2 118.78(18) . . ? C10 C1 C6 116.73(18) . . ? C2 C1 C6 104.28(18) . . ? C10 C1 C7 114.33(18) . . ? C2 C1 C7 98.92(17) . . ? C6 C1 C7 100.95(17) . . ? N3 C2 C3 130.8(2) . . ? N3 C2 C1 123.33(19) . . ? C3 C2 C1 105.84(18) . . ? C4 C3 C2 104.92(19) . . ? C4 C3 H3A 110.8 . . ? C2 C3 H3A 110.8 . . ? C4 C3 H3B 110.8 . . ? C2 C3 H3B 110.8 . . ? H3A C3 H3B 108.8 . . ? C3 C4 C7 102.87(18) . . ? C3 C4 C5 106.06(19) . . ? C7 C4 C5 101.71(19) . . ? C3 C4 H4A 114.9 . . ? C7 C4 H4A 114.9 . . ? C5 C4 H4A 114.9 . . ? C6 C5 C4 101.91(18) . . ? C6 C5 H5A 111.4 . . ? C4 C5 H5A 111.4 . . ? C6 C5 H5B 111.4 . . ? C4 C5 H5B 111.4 . . ? H5A C5 H5B 109.3 . . ? C1 C6 C5 105.58(17) . . ? C1 C6 H6A 110.6 . . ? C5 C6 H6A 110.6 . . ? C1 C6 H6B 110.6 . . ? C5 C6 H6B 110.6 . . ? H6A C6 H6B 108.8 . . ? C8 C7 C4 113.7(2) . . ? C8 C7 C9 107.35(19) . . ? C4 C7 C9 118.23(19) . . ? C8 C7 C1 111.87(18) . . ? C4 C7 C1 93.96(17) . . ? C9 C7 C1 111.32(19) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C1 C10 S1 120.15(14) . . ? C1 C10 H10A 107.3 . . ? S1 C10 H10A 107.3 . . ? C1 C10 H10B 107.3 . . ? S1 C10 H10B 107.3 . . ? H10A C10 H10B 106.9 . . ? N1 C11 C12 121.04(19) . . ? N1 C11 H11A 107.1 . . ? C12 C11 H11A 107.1 . . ? N1 C11 H11B 107.1 . . ? C12 C11 H11B 107.1 . . ? H11A C11 H11B 106.8 . . ? N2 C12 C11 118.44(19) . . ? N2 C12 H12A 107.7 . . ? C11 C12 H12A 107.7 . . ? N2 C12 H12B 107.7 . . ? C11 C12 H12B 107.7 . . ? H12A C12 H12B 107.1 . . ? C14 C13 S4 117.17(15) . . ? C14 C13 H13A 108.0 . . ? S4 C13 H13A 108.0 . . ? C14 C13 H13B 108.0 . . ? S4 C13 H13B 108.0 . . ? H13A C13 H13B 107.2 . . ? C15 C14 C13 120.35(18) . . ? C15 C14 C19 107.33(18) . . ? C13 C14 C19 115.15(18) . . ? C15 C14 C20 100.05(17) . . ? C13 C14 C20 111.52(18) . . ? C19 C14 C20 99.47(16) . . ? N4 C15 C14 124.12(19) . . ? N4 C15 C16 128.8(2) . . ? C14 C15 C16 107.04(18) . . ? C17 C16 C15 100.90(18) . . ? C17 C16 H16A 111.6 . . ? C15 C16 H16A 111.6 . . ? C17 C16 H16B 111.6 . . ? C15 C16 H16B 111.6 . . ? H16A C16 H16B 109.4 . . ? C16 C17 C20 106.49(19) . . ? C16 C17 C18 106.7(2) . . ? C20 C17 C18 101.82(19) . . ? C16 C17 H17 113.6 . . ? C20 C17 H17 113.6 . . ? C18 C17 H17 113.6 . . ? C17 C18 C19 101.54(18) . . ? C17 C18 H18A 111.5 . . ? C19 C18 H18A 111.5 . . ? C17 C18 H18B 111.5 . . ? C19 C18 H18B 111.5 . . ? H18A C18 H18B 109.3 . . ? C18 C19 C14 104.47(18) . . ? C18 C19 H19A 110.9 . . ? C14 C19 H19A 110.9 . . ? C18 C19 H19B 110.9 . . ? C14 C19 H19B 110.9 . . ? H19A C19 H19B 108.9 . . ? C21 C20 C17 117.5(2) . . ? C21 C20 C22 109.5(2) . . ? C17 C20 C22 111.02(19) . . ? C21 C20 C14 114.93(19) . . ? C17 C20 C14 92.58(17) . . ? C22 C20 C14 110.43(18) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N4 C23 C24 109.09(18) . . ? N4 C23 H23A 109.9 . . ? C24 C23 H23A 109.9 . . ? N4 C23 H23B 109.9 . . ? C24 C23 H23B 109.9 . . ? H23A C23 H23B 108.3 . . ? N3 C24 C23 110.11(19) . . ? N3 C24 H24A 109.6 . . ? C23 C24 H24A 109.6 . . ? N3 C24 H24B 109.6 . . ? C23 C24 H24B 109.6 . . ? H24A C24 H24B 108.2 . . ? C34 C25 C26 118.11(17) . . ? C34 C25 C31 111.90(17) . . ? C26 C25 C31 100.77(16) . . ? C34 C25 C30 115.79(18) . . ? C26 C25 C30 106.13(17) . . ? C31 C25 C30 101.97(17) . . ? N7 C26 C27 130.6(2) . . ? N7 C26 C25 125.12(19) . . ? C27 C26 C25 104.28(18) . . ? C28 C27 C26 103.56(17) . . ? C28 C27 H27A 111.0 . . ? C26 C27 H27A 111.0 . . ? C28 C27 H27B 111.0 . . ? C26 C27 H27B 111.0 . . ? H27A C27 H27B 109.0 . . ? C27 C28 C29 107.5(2) . . ? C27 C28 C31 101.68(18) . . ? C29 C28 C31 102.23(19) . . ? C27 C28 H28 114.6 . . ? C29 C28 H28 114.6 . . ? C31 C28 H28 114.6 . . ? C30 C29 C28 104.89(18) . . ? C30 C29 H29A 110.8 . . ? C28 C29 H29A 110.8 . . ? C30 C29 H29B 110.8 . . ? C28 C29 H29B 110.8 . . ? H29A C29 H29B 108.8 . . ? C29 C30 C25 103.16(18) . . ? C29 C30 H30A 111.1 . . ? C25 C30 H30A 111.1 . . ? C29 C30 H30B 111.1 . . ? C25 C30 H30B 111.1 . . ? H30A C30 H30B 109.1 . . ? C32 C31 C33 111.41(19) . . ? C32 C31 C25 113.20(18) . . ? C33 C31 C25 113.66(19) . . ? C32 C31 C28 112.51(19) . . ? C33 C31 C28 112.30(19) . . ? C25 C31 C28 92.55(16) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C25 C34 S3 118.59(15) . . ? C25 C34 H34A 107.7 . . ? S3 C34 H34A 107.7 . . ? C25 C34 H34B 107.7 . . ? S3 C34 H34B 107.7 . . ? H34A C34 H34B 107.1 . . ? N5 C35 C36 117.2(2) . . ? N5 C35 H35A 108.0 . . ? C36 C35 H35A 108.0 . . ? N5 C35 H35B 108.0 . . ? C36 C35 H35B 108.0 . . ? H35A C35 H35B 107.2 . . ? N6 C36 C35 118.0(2) . . ? N6 C36 H36A 107.8 . . ? C35 C36 H36A 107.8 . . ? N6 C36 H36B 107.8 . . ? C35 C36 H36B 107.8 . . ? H36A C36 H36B 107.2 . . ? C38 C37 S2 118.69(14) . . ? C38 C37 H37A 107.6 . . ? S2 C37 H37A 107.6 . . ? C38 C37 H37B 107.6 . . ? S2 C37 H37B 107.6 . . ? H37A C37 H37B 107.1 . . ? C39 C38 C37 116.21(18) . . ? C39 C38 C44 106.68(17) . . ? C37 C38 C44 116.74(17) . . ? C39 C38 C42 101.82(17) . . ? C37 C38 C42 110.87(17) . . ? C44 C38 C42 102.67(17) . . ? N8 C39 C40 131.4(2) . . ? N8 C39 C38 124.8(2) . . ? C40 C39 C38 103.80(18) . . ? C39 C40 C41 105.59(18) . . ? C39 C40 H40A 110.6 . . ? C41 C40 H40A 110.6 . . ? C39 C40 H40B 110.6 . . ? C41 C40 H40B 110.6 . . ? H40A C40 H40B 108.8 . . ? C43 C41 C40 107.4(2) . . ? C43 C41 C42 101.98(17) . . ? C40 C41 C42 100.56(18) . . ? C43 C41 H41 115.1 . . ? C40 C41 H41 115.1 . . ? C42 C41 H41 115.1 . . ? C47 C42 C48 110.18(19) . . ? C47 C42 C38 113.88(18) . . ? C48 C42 C38 114.58(18) . . ? C47 C42 C41 111.60(19) . . ? C48 C42 C41 113.88(18) . . ? C38 C42 C41 91.68(17) . . ? C41 C43 C44 105.16(18) . . ? C41 C43 H43B 110.7 . . ? C44 C43 H43B 110.7 . . ? C41 C43 H43A 110.7 . . ? C44 C43 H43A 110.7 . . ? H43B C43 H43A 108.8 . . ? C38 C44 C43 101.58(16) . . ? C38 C44 H44A 111.5 . . ? C43 C44 H44A 111.5 . . ? C38 C44 H44B 111.5 . . ? C43 C44 H44B 111.5 . . ? H44A C44 H44B 109.3 . . ? N8 C45 C46 109.01(17) . . ? N8 C45 H45A 109.9 . . ? C46 C45 H45A 109.9 . . ? N8 C45 H45B 109.9 . . ? C46 C45 H45B 109.9 . . ? H45A C45 H45B 108.3 . . ? N7 C46 C45 111.72(18) . . ? N7 C46 H46A 109.3 . . ? C45 C46 H46A 109.3 . . ? N7 C46 H46B 109.3 . . ? C45 C46 H46B 109.3 . . ? H46A C46 H46B 107.9 . . ? C42 C47 H47A 109.5 . . ? C42 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C42 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C42 C48 H48A 109.5 . . ? C42 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C42 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C11 N1 S1 115.37(16) . . ? C11 N1 H1 122.3 . . ? S1 N1 H1 122.3 . . ? C12 N2 S4 121.41(17) . . ? C12 N2 H2 119.3 . . ? S4 N2 H2 119.3 . . ? C2 N3 C24 120.72(19) . . ? C15 N4 C23 116.13(18) . . ? C35 N5 S3 127.41(16) . . ? C35 N5 H5 116.3 . . ? S3 N5 H5 116.3 . . ? C36 N6 S2 119.07(16) . . ? C36 N6 H6 107.5 . . ? S2 N6 H6 107.4 . . ? C26 N7 C46 117.44(19) . . ? C39 N8 C45 118.0(2) . . ? H9D O9 H9F 109.5 . . ? H10D O10 H10E 109.5 . . ? H11F O11 H11D 109.5 . . ? O1 S1 O2 121.32(10) . . ? O1 S1 N1 107.06(10) . . ? O2 S1 N1 106.98(10) . . ? O1 S1 C10 108.07(10) . . ? O2 S1 C10 104.71(10) . . ? N1 S1 C10 108.14(10) . . ? O7 S2 O8 120.27(10) . . ? O7 S2 N6 107.34(10) . . ? O8 S2 N6 105.96(10) . . ? O7 S2 C37 109.32(10) . . ? O8 S2 C37 105.26(10) . . ? N6 S2 C37 108.19(10) . . ? O5 S3 O6 120.05(10) . . ? O5 S3 N5 106.90(10) . . ? O6 S3 N5 106.22(10) . . ? O5 S3 C34 108.03(10) . . ? O6 S3 C34 107.95(10) . . ? N5 S3 C34 107.03(11) . . ? O3 S4 O4 120.36(10) . . ? O3 S4 N2 108.22(10) . . ? O4 S4 N2 106.72(11) . . ? O3 S4 C13 108.49(9) . . ? O4 S4 C13 106.27(10) . . ? N2 S4 C13 105.93(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 C1 C2 N3 21.3(3) . . . . ? C6 C1 C2 N3 -110.7(2) . . . . ? C7 C1 C2 N3 145.5(2) . . . . ? C10 C1 C2 C3 -159.29(18) . . . . ? C6 C1 C2 C3 68.70(19) . . . . ? C7 C1 C2 C3 -35.1(2) . . . . ? N3 C2 C3 C4 -178.6(2) . . . . ? C1 C2 C3 C4 2.0(2) . . . . ? C2 C3 C4 C7 33.7(2) . . . . ? C2 C3 C4 C5 -72.7(2) . . . . ? C3 C4 C5 C6 69.0(2) . . . . ? C7 C4 C5 C6 -38.2(2) . . . . ? C10 C1 C6 C5 156.69(19) . . . . ? C2 C1 C6 C5 -70.1(2) . . . . ? C7 C1 C6 C5 32.1(2) . . . . ? C4 C5 C6 C1 2.8(2) . . . . ? C3 C4 C7 C8 62.7(2) . . . . ? C5 C4 C7 C8 172.35(18) . . . . ? C3 C4 C7 C9 -170.12(19) . . . . ? C5 C4 C7 C9 -60.4(2) . . . . ? C3 C4 C7 C1 -53.33(19) . . . . ? C5 C4 C7 C1 56.38(19) . . . . ? C10 C1 C7 C8 62.4(3) . . . . ? C2 C1 C7 C8 -64.9(2) . . . . ? C6 C1 C7 C8 -171.4(2) . . . . ? C10 C1 C7 C4 179.87(19) . . . . ? C2 C1 C7 C4 52.58(19) . . . . ? C6 C1 C7 C4 -54.0(2) . . . . ? C10 C1 C7 C9 -57.7(2) . . . . ? C2 C1 C7 C9 174.99(18) . . . . ? C6 C1 C7 C9 68.4(2) . . . . ? C2 C1 C10 S1 -71.3(2) . . . . ? C6 C1 C10 S1 54.9(3) . . . . ? C7 C1 C10 S1 172.40(15) . . . . ? N1 C11 C12 N2 -11.7(3) . . . . ? S4 C13 C14 C15 -67.8(3) . . . . ? S4 C13 C14 C19 63.2(2) . . . . ? S4 C13 C14 C20 175.55(15) . . . . ? C13 C14 C15 N4 21.4(3) . . . . ? C19 C14 C15 N4 -112.9(2) . . . . ? C20 C14 C15 N4 143.8(2) . . . . ? C13 C14 C15 C16 -160.42(19) . . . . ? C19 C14 C15 C16 65.3(2) . . . . ? C20 C14 C15 C16 -38.1(2) . . . . ? N4 C15 C16 C17 -176.7(2) . . . . ? C14 C15 C16 C17 5.3(2) . . . . ? C15 C16 C17 C20 31.0(2) . . . . ? C15 C16 C17 C18 -77.2(2) . . . . ? C16 C17 C18 C19 73.5(2) . . . . ? C20 C17 C18 C19 -38.0(2) . . . . ? C17 C18 C19 C14 0.5(2) . . . . ? C15 C14 C19 C18 -67.6(2) . . . . ? C13 C14 C19 C18 155.38(18) . . . . ? C20 C14 C19 C18 36.1(2) . . . . ? C16 C17 C20 C21 -172.41(19) . . . . ? C18 C17 C20 C21 -60.8(2) . . . . ? C16 C17 C20 C22 60.6(2) . . . . ? C18 C17 C20 C22 172.19(18) . . . . ? C16 C17 C20 C14 -52.5(2) . . . . ? C18 C17 C20 C14 59.12(19) . . . . ? C15 C14 C20 C21 174.53(19) . . . . ? C13 C14 C20 C21 -57.1(3) . . . . ? C19 C14 C20 C21 64.9(2) . . . . ? C15 C14 C20 C17 52.52(19) . . . . ? C13 C14 C20 C17 -179.06(19) . . . . ? C19 C14 C20 C17 -57.13(19) . . . . ? C15 C14 C20 C22 -61.1(2) . . . . ? C13 C14 C20 C22 67.4(2) . . . . ? C19 C14 C20 C22 -170.71(18) . . . . ? N4 C23 C24 N3 -66.6(2) . . . . ? C34 C25 C26 N7 19.8(3) . . . . ? C31 C25 C26 N7 142.0(2) . . . . ? C30 C25 C26 N7 -112.1(2) . . . . ? C34 C25 C26 C27 -158.28(18) . . . . ? C31 C25 C26 C27 -36.1(2) . . . . ? C30 C25 C26 C27 69.8(2) . . . . ? N7 C26 C27 C28 -177.8(2) . . . . ? C25 C26 C27 C28 0.1(2) . . . . ? C26 C27 C28 C29 -70.9(2) . . . . ? C26 C27 C28 C31 36.0(2) . . . . ? C27 C28 C29 C30 70.1(2) . . . . ? C31 C28 C29 C30 -36.5(2) . . . . ? C28 C29 C30 C25 1.3(2) . . . . ? C34 C25 C30 C29 156.04(19) . . . . ? C26 C25 C30 C29 -70.8(2) . . . . ? C31 C25 C30 C29 34.3(2) . . . . ? C34 C25 C31 C32 66.0(2) . . . . ? C26 C25 C31 C32 -60.4(2) . . . . ? C30 C25 C31 C32 -169.59(18) . . . . ? C34 C25 C31 C33 -62.4(2) . . . . ? C26 C25 C31 C33 171.22(18) . . . . ? C30 C25 C31 C33 62.0(2) . . . . ? C34 C25 C31 C28 -178.11(18) . . . . ? C26 C25 C31 C28 55.49(18) . . . . ? C30 C25 C31 C28 -53.74(19) . . . . ? C27 C28 C31 C32 60.4(2) . . . . ? C29 C28 C31 C32 171.41(19) . . . . ? C27 C28 C31 C33 -172.98(19) . . . . ? C29 C28 C31 C33 -61.9(2) . . . . ? C27 C28 C31 C25 -56.1(2) . . . . ? C29 C28 C31 C25 55.0(2) . . . . ? C26 C25 C34 S3 -66.8(2) . . . . ? C31 C25 C34 S3 176.90(16) . . . . ? C30 C25 C34 S3 60.6(2) . . . . ? N5 C35 C36 N6 -35.1(3) . . . . ? S2 C37 C38 C39 -71.4(2) . . . . ? S2 C37 C38 C44 55.9(2) . . . . ? S2 C37 C38 C42 172.99(15) . . . . ? C37 C38 C39 N8 22.2(3) . . . . ? C44 C38 C39 N8 -110.0(2) . . . . ? C42 C38 C39 N8 142.8(2) . . . . ? C37 C38 C39 C40 -157.83(18) . . . . ? C44 C38 C39 C40 70.0(2) . . . . ? C42 C38 C39 C40 -37.2(2) . . . . ? N8 C39 C40 C41 -178.9(2) . . . . ? C38 C39 C40 C41 1.1(2) . . . . ? C39 C40 C41 C43 -71.3(2) . . . . ? C39 C40 C41 C42 35.0(2) . . . . ? C39 C38 C42 C47 -58.8(2) . . . . ? C37 C38 C42 C47 65.4(2) . . . . ? C44 C38 C42 C47 -169.16(19) . . . . ? C39 C38 C42 C48 173.06(18) . . . . ? C37 C38 C42 C48 -62.7(2) . . . . ? C44 C38 C42 C48 62.7(2) . . . . ? C39 C38 C42 C41 55.75(19) . . . . ? C37 C38 C42 C41 180.00(16) . . . . ? C44 C38 C42 C41 -54.59(18) . . . . ? C43 C41 C42 C47 173.07(19) . . . . ? C40 C41 C42 C47 62.5(2) . . . . ? C43 C41 C42 C48 -61.4(2) . . . . ? C40 C41 C42 C48 -171.94(18) . . . . ? C43 C41 C42 C38 56.5(2) . . . . ? C40 C41 C42 C38 -54.03(18) . . . . ? C40 C41 C43 C44 66.9(2) . . . . ? C42 C41 C43 C44 -38.4(2) . . . . ? C39 C38 C44 C43 -72.5(2) . . . . ? C37 C38 C44 C43 155.59(18) . . . . ? C42 C38 C44 C43 34.1(2) . . . . ? C41 C43 C44 C38 2.8(2) . . . . ? N8 C45 C46 N7 -63.4(2) . . . . ? C12 C11 N1 S1 -168.92(18) . . . . ? C11 C12 N2 S4 -93.9(2) . . . . ? C3 C2 N3 C24 -3.5(3) . . . . ? C1 C2 N3 C24 175.8(2) . . . . ? C23 C24 N3 C2 -110.0(2) . . . . ? C14 C15 N4 C23 179.60(19) . . . . ? C16 C15 N4 C23 1.9(3) . . . . ? C24 C23 N4 C15 166.40(19) . . . . ? C36 C35 N5 S3 -79.7(3) . . . . ? C35 C36 N6 S2 -155.60(17) . . . . ? C27 C26 N7 C46 -3.7(3) . . . . ? C25 C26 N7 C46 178.68(18) . . . . ? C45 C46 N7 C26 169.00(19) . . . . ? C40 C39 N8 C45 -4.1(4) . . . . ? C38 C39 N8 C45 175.9(2) . . . . ? C46 C45 N8 C39 -114.4(2) . . . . ? C11 N1 S1 O1 -165.01(17) . . . . ? C11 N1 S1 O2 -33.54(19) . . . . ? C11 N1 S1 C10 78.76(18) . . . . ? C1 C10 S1 O1 -34.1(2) . . . . ? C1 C10 S1 O2 -164.70(17) . . . . ? C1 C10 S1 N1 81.49(19) . . . . ? C36 N6 S2 O7 -163.29(18) . . . . ? C36 N6 S2 O8 -33.6(2) . . . . ? C36 N6 S2 C37 78.85(19) . . . . ? C38 C37 S2 O7 -31.27(19) . . . . ? C38 C37 S2 O8 -161.76(16) . . . . ? C38 C37 S2 N6 85.32(17) . . . . ? C35 N5 S3 O5 -144.2(2) . . . . ? C35 N5 S3 O6 -14.9(2) . . . . ? C35 N5 S3 C34 100.3(2) . . . . ? C25 C34 S3 O5 -31.9(2) . . . . ? C25 C34 S3 O6 -163.15(16) . . . . ? C25 C34 S3 N5 82.88(19) . . . . ? C12 N2 S4 O3 -146.98(17) . . . . ? C12 N2 S4 O4 -16.1(2) . . . . ? C12 N2 S4 C13 96.85(19) . . . . ? C14 C13 S4 O3 -32.0(2) . . . . ? C14 C13 S4 O4 -162.75(17) . . . . ? C14 C13 S4 N2 83.99(19) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.147 _refine_diff_density_min -0.166 _refine_diff_density_rms 0.032 data_s _database_code_depnum_ccdc_archive 'CCDC 753363' #TrackingRef 'nju02 SMC.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C24 H40 N4 O4 S2), 0.7(H2 O), 0.3(H O), 0.3(H)' _chemical_formula_sum 'C48 H82 N8 O9 S4' _chemical_formula_weight 1043.46 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1) ' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.9319(16) _cell_length_b 28.833(2) _cell_length_c 11.1309(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.439(4) _cell_angle_gamma 90.00 _cell_volume 2866.5(7) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 3153 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 24.25 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.209 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1124 _exptl_absorpt_coefficient_mu 0.222 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.97 _exptl_absorpt_correction_T_max 0.97 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Aepex CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15503 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0542 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10429 _reflns_number_gt 8767 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.05P)^2^+0.99P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(6) _chemical_absolute_configuration unk _refine_ls_number_reflns 10429 _refine_ls_number_parameters 648 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0664 _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_ref 0.1163 _refine_ls_wR_factor_gt 0.1137 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0.002 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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9951(4) 0.75267(12) -0.0647(3) 0.0352(8) Uani 1 1 d . . . C2 C 1.0070(5) 0.72112(13) -0.1727(3) 0.0402(9) Uani 1 1 d . . . H2C H 0.9325 0.6967 -0.1702 0.048 Uiso 1 1 calc R . . H2D H 1.1058 0.7073 -0.1776 0.048 Uiso 1 1 calc R . . C3 C 0.9774(5) 0.75485(15) -0.2802(3) 0.0483(10) Uani 1 1 d . . . H3C H 1.0628 0.7564 -0.3333 0.058 Uiso 1 1 calc R . . H3D H 0.8894 0.7457 -0.3260 0.058 Uiso 1 1 calc R . . C4 C 0.9530(5) 0.80053(14) -0.2158(3) 0.0417(9) Uani 1 1 d . . . H4C H 0.9644 0.8278 -0.2676 0.050 Uiso 1 1 calc R . . C5 C 0.8014(4) 0.79770(13) -0.1546(3) 0.0402(9) Uani 1 1 d . . . H5C H 0.7691 0.8279 -0.1268 0.048 Uiso 1 1 calc R . . H5D H 0.7258 0.7850 -0.2082 0.048 Uiso 1 1 calc R . . C6 C 0.8326(4) 0.76527(11) -0.0499(3) 0.0297(7) Uani 1 1 d . . . C7 C 1.0658(5) 0.79854(14) -0.1124(3) 0.0453(10) Uani 1 1 d . . . C8 C 1.0472(4) 0.84017(13) -0.0188(3) 0.0439(9) Uani 1 1 d . . . H8C H 1.0907 0.8678 -0.0514 0.066 Uiso 1 1 calc R . . H8D H 1.0970 0.8324 0.0553 0.066 Uiso 1 1 calc R . . H8E H 0.9428 0.8453 -0.0040 0.066 Uiso 1 1 calc R . . C9 C 1.2250(5) 0.79518(15) -0.1454(4) 0.0503(10) Uani 1 1 d . . . H9A H 1.2385 0.7696 -0.1995 0.075 Uiso 1 1 calc R . . H9B H 1.2845 0.7903 -0.0744 0.075 Uiso 1 1 calc R . . H9C H 1.2555 0.8234 -0.1839 0.075 Uiso 1 1 calc R . . C10 C 1.0795(4) 0.73544(13) 0.0512(3) 0.0366(8) Uani 1 1 d . . . H10A H 1.0649 0.7585 0.1135 0.044 Uiso 1 1 calc R . . H10B H 1.1857 0.7349 0.0337 0.044 Uiso 1 1 calc R . . C11 C 0.8744(5) 0.69236(14) 0.3183(3) 0.0427(9) Uani 1 1 d . . . H11A H 0.9261 0.6663 0.3548 0.051 Uiso 1 1 calc R . . H11B H 0.7704 0.6907 0.3423 0.051 Uiso 1 1 calc R . . C12 C 0.9395(5) 0.73554(14) 0.3677(3) 0.0398(9) Uani 1 1 d . . . H12A H 0.9134 0.7373 0.4521 0.048 Uiso 1 1 calc R . . H12B H 1.0476 0.7330 0.3637 0.048 Uiso 1 1 calc R . . C13 C 0.7159(4) 0.82785(13) 0.4616(3) 0.0329(7) Uani 1 1 d . . . H13A H 0.6942 0.7967 0.4896 0.039 Uiso 1 1 calc R . . H13B H 0.7296 0.8471 0.5323 0.039 Uiso 1 1 calc R . . C14 C 0.5775(4) 0.84553(12) 0.3944(3) 0.0290(7) Uani 1 1 d . . . C15 C 0.5864(4) 0.89565(12) 0.3447(4) 0.0415(9) Uani 1 1 d . . . H15A H 0.6440 0.9155 0.3980 0.050 Uiso 1 1 calc R . . H15B H 0.6312 0.8961 0.2656 0.050 Uiso 1 1 calc R . . C16 C 0.4232(4) 0.91080(14) 0.3390(4) 0.0435(9) Uani 1 1 d . . . H16A H 0.4051 0.9365 0.3933 0.052 Uiso 1 1 calc R . . H16B H 0.3952 0.9201 0.2581 0.052 Uiso 1 1 calc R . . C17 C 0.3386(4) 0.86900(12) 0.3765(4) 0.0377(9) Uani 1 1 d . . . H17A H 0.2356 0.8754 0.4012 0.045 Uiso 1 1 calc R . . C18 C 0.3516(4) 0.83055(14) 0.2812(3) 0.0435(9) Uani 1 1 d . . . H18A H 0.2829 0.8053 0.2970 0.052 Uiso 1 1 calc R . . H18B H 0.3328 0.8425 0.2010 0.052 Uiso 1 1 calc R . . C19 C 0.5155(4) 0.81507(11) 0.2966(3) 0.0318(7) Uani 1 1 d . . . C20 C 0.4401(4) 0.84957(11) 0.4788(3) 0.0348(8) Uani 1 1 d . . . C21 C 0.3852(4) 0.80343(13) 0.5271(4) 0.0400(9) Uani 1 1 d . . . H21A H 0.3013 0.8086 0.5789 0.060 Uiso 1 1 calc R . . H21B H 0.4643 0.7887 0.5717 0.060 Uiso 1 1 calc R . . H21C H 0.3552 0.7839 0.4614 0.060 Uiso 1 1 calc R . . C22 C 0.4585(5) 0.88288(15) 0.5823(4) 0.0475(10) Uani 1 1 d . . . H22A H 0.3678 0.8838 0.6280 0.071 Uiso 1 1 calc R . . H22B H 0.4799 0.9133 0.5519 0.071 Uiso 1 1 calc R . . H22C H 0.5397 0.8728 0.6330 0.071 Uiso 1 1 calc R . . C23 C 0.5147(5) 0.75954(16) 0.1413(4) 0.0477(10) Uani 1 1 d . . . H23A H 0.4105 0.7686 0.1334 0.057 Uiso 1 1 calc R . . H23B H 0.5181 0.7266 0.1588 0.057 Uiso 1 1 calc R . . C24 C 0.5934(4) 0.76885(14) 0.0273(3) 0.0406(9) Uani 1 1 d . . . H24A H 0.5412 0.7534 -0.0381 0.049 Uiso 1 1 calc R . . H24B H 0.5922 0.8019 0.0113 0.049 Uiso 1 1 calc R . . C25 C 0.0906(4) 0.51706(13) 0.3801(3) 0.0351(8) Uani 1 1 d . . . C26 C 0.1039(5) 0.46998(15) 0.4396(4) 0.0477(10) Uani 1 1 d . . . H26A H 0.1453 0.4728 0.5201 0.057 Uiso 1 1 calc R . . H26B H 0.1670 0.4494 0.3931 0.057 Uiso 1 1 calc R . . C27 C -0.0625(5) 0.45147(16) 0.4431(5) 0.0580(12) Uani 1 1 d . . . H27A H -0.0756 0.4244 0.3923 0.070 Uiso 1 1 calc R . . H27B H -0.0928 0.4440 0.5243 0.070 Uiso 1 1 calc R . . C28 C -0.1492(5) 0.49363(14) 0.3934(4) 0.0491(10) Uani 1 1 d . . . H28A H -0.2521 0.4868 0.3681 0.059 Uiso 1 1 calc R . . C29 C -0.1353(5) 0.53299(16) 0.4843(4) 0.0520(11) Uani 1 1 d . . . H29A H -0.2043 0.5579 0.4649 0.062 Uiso 1 1 calc R . . H29B H -0.1560 0.5220 0.5648 0.062 Uiso 1 1 calc R . . C30 C 0.0218(4) 0.54890(13) 0.4747(3) 0.0358(8) Uani 1 1 d . . . C31 C -0.0502(4) 0.50945(14) 0.2946(3) 0.0405(9) Uani 1 1 d . . . C32 C -0.1020(5) 0.55506(15) 0.2346(4) 0.0497(10) Uani 1 1 d . . . H32A H -0.1901 0.5493 0.1869 0.075 Uiso 1 1 calc R . . H32B H -0.0238 0.5667 0.1842 0.075 Uiso 1 1 calc R . . H32C H -0.1244 0.5775 0.2955 0.075 Uiso 1 1 calc R . . C33 C -0.0193(5) 0.47179(15) 0.1964(4) 0.0519(11) Uani 1 1 d . . . H33A H -0.1085 0.4668 0.1495 0.078 Uiso 1 1 calc R . . H33B H 0.0099 0.4433 0.2345 0.078 Uiso 1 1 calc R . . H33C H 0.0597 0.4822 0.1450 0.078 Uiso 1 1 calc R . . C34 C 0.2279(4) 0.53413(14) 0.3118(3) 0.0369(8) Uani 1 1 d . . . H34A H 0.2045 0.5645 0.2793 0.044 Uiso 1 1 calc R . . H34B H 0.2428 0.5135 0.2440 0.044 Uiso 1 1 calc R . . C35 C 0.4472(5) 0.62944(14) 0.3949(4) 0.0485(11) Uani 1 1 d . . . H35A H 0.5555 0.6318 0.3946 0.058 Uiso 1 1 calc R . . H35B H 0.4141 0.6258 0.3122 0.058 Uiso 1 1 calc R . . C36 C 0.3864(5) 0.67247(13) 0.4413(3) 0.0439(9) Uani 1 1 d . . . H36A H 0.4400 0.6978 0.4036 0.053 Uiso 1 1 calc R . . H36B H 0.2830 0.6746 0.4145 0.053 Uiso 1 1 calc R . . C37 C 0.5821(4) 0.63397(12) 0.7139(3) 0.0328(8) Uani 1 1 d . . . H37A H 0.5665 0.6105 0.6527 0.039 Uiso 1 1 calc R . . H37B H 0.6884 0.6344 0.7323 0.039 Uiso 1 1 calc R . . C38 C 0.4989(4) 0.61792(11) 0.8290(3) 0.0290(7) Uani 1 1 d . . . C39 C 0.5099(5) 0.64863(14) 0.9382(3) 0.0399(9) Uani 1 1 d . . . H39A H 0.6070 0.6636 0.9422 0.048 Uiso 1 1 calc R . . H39B H 0.4328 0.6723 0.9360 0.048 Uiso 1 1 calc R . . C40 C 0.4886(5) 0.61701(16) 1.0441(3) 0.0498(10) Uani 1 1 d . . . H40A H 0.4055 0.6270 1.0934 0.060 Uiso 1 1 calc R . . H40B H 0.5785 0.6153 1.0934 0.060 Uiso 1 1 calc R . . C41 C 0.4557(5) 0.57126(14) 0.9837(3) 0.0468(10) Uani 1 1 d . . . H41A H 0.4657 0.5445 1.0373 0.056 Uiso 1 1 calc R . . C42 C 0.2985(5) 0.57507(14) 0.9217(3) 0.0435(9) Uani 1 1 d . . . H42A H 0.2616 0.5449 0.8968 0.052 Uiso 1 1 calc R . . H42B H 0.2259 0.5895 0.9743 0.052 Uiso 1 1 calc R . . C43 C 0.3322(4) 0.60575(12) 0.8137(3) 0.0325(8) Uani 1 1 d . . . C44 C 0.5626(5) 0.57017(12) 0.8770(3) 0.0385(8) Uani 1 1 d . . . C45 C 0.7260(5) 0.57116(15) 0.9127(4) 0.0511(11) Uani 1 1 d . . . H45A H 0.7553 0.5412 0.9421 0.077 Uiso 1 1 calc R . . H45B H 0.7413 0.5939 0.9746 0.077 Uiso 1 1 calc R . . H45C H 0.7853 0.5790 0.8441 0.077 Uiso 1 1 calc R . . C46 C 0.5365(5) 0.52972(13) 0.7916(4) 0.0452(10) Uani 1 1 d . . . H46A H 0.5777 0.5019 0.8260 0.068 Uiso 1 1 calc R . . H46B H 0.5843 0.5360 0.7164 0.068 Uiso 1 1 calc R . . H46C H 0.4309 0.5257 0.7784 0.068 Uiso 1 1 calc R . . C47 C 0.0952(4) 0.60159(15) 0.7352(3) 0.0429(9) Uani 1 1 d . . . H47A H 0.0415 0.6181 0.7973 0.051 Uiso 1 1 calc R . . H47B H 0.0947 0.5688 0.7550 0.051 Uiso 1 1 calc R . . C48 C 0.0185(4) 0.60917(15) 0.6142(3) 0.0426(9) Uani 1 1 d U . . H48A H -0.0866 0.6009 0.6197 0.051 Uiso 1 1 calc R . . H48B H 0.0250 0.6416 0.5918 0.051 Uiso 1 1 calc R . . N1 N 0.8807(4) 0.68727(11) 0.1907(3) 0.0419(7) Uani 1 1 d . . . H1B H 0.7972 0.6886 0.1519 0.050 Uiso 1 1 calc R . . N2 N 0.8973(3) 0.77795(11) 0.3130(2) 0.0359(7) Uani 1 1 d . . . H2B H 0.8737 0.7778 0.2379 0.043 Uiso 1 1 calc R . . N3 N 0.7466(3) 0.75279(10) 0.0323(3) 0.0357(7) Uani 1 1 d . . . N4 N 0.5842(4) 0.78519(11) 0.2394(3) 0.0400(7) Uani 1 1 d . . . N5 N 0.4058(3) 0.58801(10) 0.4613(3) 0.0354(7) Uani 1 1 d . . . H5B H 0.3826 0.5898 0.5360 0.042 Uiso 1 1 calc R . . N6 N 0.3890(4) 0.68036(11) 0.5682(3) 0.0412(7) Uani 1 1 d . . . H6B H 0.3041 0.6807 0.6041 0.049 Uiso 1 1 calc R . . N7 N 0.0896(3) 0.58091(10) 0.5237(3) 0.0339(6) Uani 1 1 d U . . N8 N 0.2475(3) 0.61818(9) 0.7299(2) 0.0281(6) Uani 1 1 d . . . O1 O 0.9927(3) 0.64931(9) 0.0187(2) 0.0449(6) Uani 1 1 d . . . O2 O 1.1432(3) 0.66602(10) 0.1939(3) 0.0515(7) Uani 1 1 d . . . O3 O 0.8974(3) 0.86252(10) 0.3016(3) 0.0503(7) Uani 1 1 d . . . O4 O 1.0059(3) 0.82294(10) 0.4771(2) 0.0445(6) Uani 1 1 d . . . O5 O 0.4100(3) 0.50454(10) 0.4802(3) 0.0521(8) Uani 1 1 d . . . O6 O 0.5146(3) 0.54140(11) 0.3007(3) 0.0527(7) Uani 1 1 d . . . O7 O 0.4983(3) 0.71898(8) 0.7427(2) 0.0421(6) Uani 1 1 d . . . O8 O 0.6512(3) 0.70083(9) 0.5694(3) 0.0512(7) Uani 1 1 d . . . O9 O 0.9591(9) 0.9586(2) 0.1453(6) 0.0438(16) Uani 0.40 1 d P . . H9E H 1.0471 0.9682 0.1608 0.053 Uiso 0.40 1 d PR . . H9F H 0.9183 0.9762 0.0934 0.053 Uiso 0.40 1 d PR . . O10 O 0.4186(11) 0.4390(3) 0.0978(8) 0.050(2) Uani 0.30 1 d P . . H10D H 0.3874 0.4328 0.0273 0.060 Uiso 0.30 1 d PR . . H10E H 0.4910 0.4211 0.1159 0.060 Uiso 0.30 1 d PR . . O11 O 0.9065(10) 0.4450(3) 0.8462(8) 0.043(2) Uani 0.30 1 d P . . H11C H 0.9010 0.4184 0.8787 0.052 Uiso 0.30 1 d PR . . H11D H 0.9980 0.4522 0.8368 0.052 Uiso 0.30 1 d PR . . S1 S 1.02976(11) 0.67930(3) 0.11337(8) 0.0377(2) Uani 1 1 d . . . S2 S 0.89165(10) 0.82594(3) 0.38377(8) 0.0361(2) Uani 1 1 d . . . S3 S 0.40374(10) 0.53850(3) 0.39264(8) 0.0370(2) Uani 1 1 d . . . S4 S 0.53473(11) 0.68866(3) 0.64932(7) 0.0350(2) Uani 1 1 d . . . 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 C1 0.043(2) 0.0329(19) 0.0298(18) 0.0018(14) -0.0006(15) -0.0013(15) C2 0.050(2) 0.040(2) 0.0299(18) -0.0002(15) 0.0054(16) -0.0016(17) C3 0.056(3) 0.058(3) 0.031(2) 0.0016(18) 0.0009(17) -0.012(2) C4 0.049(2) 0.050(2) 0.0267(17) 0.0104(16) -0.0109(16) -0.0076(18) C5 0.044(2) 0.045(2) 0.0313(18) 0.0053(16) -0.0145(16) -0.0028(17) C6 0.042(2) 0.0267(17) 0.0204(15) -0.0038(13) -0.0119(14) -0.0034(14) C7 0.050(2) 0.052(2) 0.034(2) 0.0054(17) -0.0109(17) -0.0107(19) C8 0.037(2) 0.046(2) 0.048(2) -0.0047(18) -0.0164(17) -0.0141(17) C9 0.050(3) 0.053(2) 0.048(2) 0.021(2) -0.0053(19) -0.008(2) C10 0.036(2) 0.039(2) 0.0342(18) 0.0014(15) -0.0026(15) 0.0018(16) C11 0.046(2) 0.051(2) 0.0311(18) 0.0099(17) 0.0058(15) 0.0029(18) C12 0.051(2) 0.057(2) 0.0108(14) 0.0059(15) -0.0052(14) 0.0111(19) C13 0.0270(17) 0.0416(19) 0.0300(16) -0.0016(15) 0.0039(13) 0.0034(15) C14 0.0300(18) 0.0303(17) 0.0268(16) -0.0012(13) 0.0041(13) 0.0011(14) C15 0.044(2) 0.0322(19) 0.048(2) 0.0013(17) -0.0042(18) -0.0072(16) C16 0.044(2) 0.036(2) 0.051(2) 0.0087(17) -0.0016(18) 0.0016(17) C17 0.030(2) 0.0324(19) 0.051(2) 0.0097(16) -0.0024(16) 0.0088(15) C18 0.042(2) 0.044(2) 0.045(2) 0.0006(18) -0.0038(16) -0.0058(17) C19 0.0371(19) 0.0267(18) 0.0316(17) 0.0022(14) -0.0015(14) -0.0038(14) C20 0.0325(19) 0.0267(17) 0.045(2) 0.0012(15) 0.0026(15) 0.0079(14) C21 0.0280(19) 0.043(2) 0.050(2) 0.0185(17) 0.0117(16) 0.0079(15) C22 0.043(2) 0.053(2) 0.046(2) -0.0204(19) 0.0058(17) 0.0190(19) C23 0.039(2) 0.054(2) 0.050(2) -0.0201(19) 0.0014(18) -0.0099(18) C24 0.034(2) 0.049(2) 0.038(2) -0.0057(17) -0.0078(16) 0.0085(17) C25 0.0272(18) 0.042(2) 0.0358(19) -0.0027(16) -0.0054(14) -0.0003(15) C26 0.047(2) 0.047(2) 0.050(2) 0.0120(19) -0.0010(19) 0.0055(18) C27 0.058(3) 0.046(3) 0.070(3) 0.015(2) 0.000(2) -0.003(2) C28 0.036(2) 0.045(2) 0.066(3) 0.008(2) -0.0023(19) -0.0096(18) C29 0.038(2) 0.063(3) 0.056(3) -0.002(2) 0.0145(18) -0.016(2) C30 0.0298(18) 0.049(2) 0.0288(17) 0.0042(16) -0.0008(14) -0.0062(16) C31 0.039(2) 0.047(2) 0.0355(19) -0.0032(17) -0.0085(16) -0.0065(17) C32 0.044(2) 0.058(3) 0.046(2) 0.013(2) -0.0088(18) 0.0103(19) C33 0.045(2) 0.053(2) 0.058(3) -0.016(2) -0.010(2) -0.0136(19) C34 0.0260(18) 0.054(2) 0.0306(17) -0.0025(16) -0.0054(13) -0.0033(16) C35 0.056(3) 0.047(2) 0.043(2) -0.0033(18) 0.0265(19) -0.024(2) C36 0.049(2) 0.039(2) 0.043(2) 0.0130(17) -0.0238(17) -0.0045(17) C37 0.0308(18) 0.0359(19) 0.0317(17) 0.0081(14) 0.0060(14) 0.0120(14) C38 0.0343(18) 0.0268(17) 0.0260(16) 0.0043(13) 0.0017(13) 0.0061(14) C39 0.044(2) 0.046(2) 0.0300(18) -0.0092(16) 0.0012(15) 0.0036(17) C40 0.058(3) 0.063(3) 0.0277(19) -0.0003(18) -0.0086(18) 0.016(2) C41 0.062(3) 0.046(2) 0.0329(19) 0.0137(17) 0.0045(18) 0.0179(19) C42 0.054(2) 0.042(2) 0.0344(19) 0.0041(16) 0.0143(17) -0.0031(18) C43 0.0325(19) 0.042(2) 0.0236(16) -0.0013(14) 0.0121(14) -0.0004(15) C44 0.045(2) 0.0264(18) 0.044(2) 0.0065(15) 0.0016(17) 0.0057(15) C45 0.055(3) 0.054(3) 0.044(2) 0.0144(19) -0.0103(19) 0.022(2) C46 0.045(2) 0.033(2) 0.057(2) -0.0012(17) 0.0210(19) 0.0082(16) C47 0.042(2) 0.049(2) 0.037(2) -0.0059(17) 0.0085(17) -0.0057(18) C48 0.0256(19) 0.054(2) 0.048(2) -0.0096(16) -0.0028(15) 0.0064(16) N1 0.0448(18) 0.0434(18) 0.0375(16) -0.0040(15) -0.0019(13) -0.0059(15) N2 0.0398(17) 0.0499(18) 0.0183(13) 0.0076(12) 0.0034(12) 0.0105(14) N3 0.0318(17) 0.0379(17) 0.0374(16) 0.0059(13) -0.0049(13) -0.0014(13) N4 0.0402(18) 0.0386(17) 0.0412(17) -0.0123(14) -0.0070(14) 0.0037(14) N5 0.0397(18) 0.0393(17) 0.0271(14) -0.0019(12) 0.0031(12) -0.0048(13) N6 0.0439(18) 0.0385(17) 0.0411(16) 0.0066(15) -0.0122(13) 0.0024(14) N7 0.0240(15) 0.0390(17) 0.0386(15) -0.0012(12) -0.0036(12) 0.0039(12) N8 0.0328(15) 0.0266(14) 0.0248(14) -0.0109(11) 0.0010(11) -0.0042(11) O1 0.0504(17) 0.0412(15) 0.0431(15) -0.0008(12) 0.0074(12) 0.0053(12) O2 0.0518(18) 0.0536(18) 0.0489(16) 0.0082(13) -0.0054(13) 0.0180(13) O3 0.0463(17) 0.0497(16) 0.0548(18) 0.0106(14) 0.0033(13) -0.0122(13) O4 0.0283(13) 0.0509(16) 0.0541(16) -0.0039(13) -0.0076(11) -0.0081(12) O5 0.0518(18) 0.0440(16) 0.0601(18) -0.0005(14) -0.0231(14) 0.0119(13) O6 0.0357(15) 0.0584(18) 0.0638(18) -0.0188(15) 0.0034(13) 0.0115(13) O7 0.0477(16) 0.0281(13) 0.0503(15) 0.0007(11) -0.0169(12) 0.0025(11) O8 0.0570(18) 0.0423(16) 0.0544(17) 0.0096(13) 0.0025(14) -0.0195(13) O9 0.069(5) 0.025(3) 0.037(4) 0.010(3) -0.009(3) 0.006(3) O10 0.073(7) 0.038(5) 0.038(5) 0.020(4) -0.010(4) -0.002(4) O11 0.036(5) 0.050(5) 0.043(5) -0.005(4) -0.003(4) -0.010(4) S1 0.0494(5) 0.0338(5) 0.0300(4) 0.0033(4) 0.0002(4) 0.0135(4) S2 0.0251(4) 0.0466(5) 0.0364(5) 0.0031(4) -0.0028(3) -0.0076(4) S3 0.0269(4) 0.0399(5) 0.0441(5) -0.0086(4) -0.0073(4) 0.0044(4) S4 0.0494(5) 0.0266(4) 0.0288(4) 0.0066(3) -0.0094(4) -0.0126(4) _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 C1 C6 1.506(5) . ? C1 C2 1.512(5) . ? C1 C7 1.560(5) . ? C1 C10 1.571(5) . ? C2 C3 1.563(5) . ? C2 H2C 0.9700 . ? C2 H2D 0.9700 . ? C3 C4 1.516(6) . ? C3 H3C 0.9700 . ? C3 H3D 0.9700 . ? C4 C5 1.523(6) . ? C4 C7 1.526(5) . ? C4 H4C 0.9800 . ? C5 C6 1.518(5) . ? C5 H5C 0.9700 . ? C5 H5D 0.9700 . ? C6 N3 1.252(4) . ? C7 C9 1.474(6) . ? C7 C8 1.599(6) . ? C8 H8C 0.9600 . ? C8 H8D 0.9600 . ? C8 H8E 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 S1 1.817(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N1 1.429(5) . ? C11 C12 1.478(6) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N2 1.416(5) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.528(5) . ? C13 S2 1.800(3) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C19 1.501(5) . ? C14 C15 1.550(5) . ? C14 C20 1.556(5) . ? C15 C16 1.522(6) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.484(5) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.540(5) . ? C17 C20 1.554(5) . ? C17 H17A 0.9800 . ? C18 C19 1.539(5) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 N4 1.238(5) . ? C20 C22 1.508(5) . ? C20 C21 1.518(5) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 N4 1.454(5) . ? C23 C24 1.481(6) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 N3 1.445(5) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.515(5) . ? C25 C34 1.529(5) . ? C25 C30 1.529(5) . ? C25 C31 1.587(5) . ? C26 C27 1.580(6) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.542(6) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C31 1.488(6) . ? C28 C29 1.525(6) . ? C28 H28A 0.9800 . ? C29 C30 1.481(5) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 N7 1.229(5) . ? C31 C32 1.544(5) . ? C31 C33 1.567(6) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 S3 1.809(3) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.451(6) . ? C35 N5 1.454(5) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 N6 1.431(5) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.556(4) . ? C37 S4 1.782(3) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.507(5) . ? C38 C43 1.538(5) . ? C38 C44 1.581(5) . ? C39 C40 1.504(5) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 C41 1.508(6) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C44 1.530(6) . ? C41 C42 1.564(6) . ? C41 H41A 0.9800 . ? C42 C43 1.524(5) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 N8 1.250(4) . ? C44 C45 1.510(6) . ? C44 C46 1.521(5) . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 N8 1.443(5) . ? C47 C48 1.522(5) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 N7 1.446(5) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? N1 S1 1.608(3) . ? N1 H1B 0.8600 . ? N2 S2 1.593(3) . ? N2 H2B 0.8600 . ? N5 S3 1.619(3) . ? N5 H5B 0.8600 . ? N6 S4 1.597(3) . ? N6 H6B 0.8600 . ? O1 S1 1.401(3) . ? O2 S1 1.401(3) . ? O3 S2 1.397(3) . ? O4 S2 1.453(3) . ? O5 S3 1.383(3) . ? O6 S3 1.432(3) . ? O7 S4 1.399(3) . ? O8 S4 1.419(3) . ? O9 O11 1.265(11) 2_756 ? O9 H9E 0.8500 . ? O9 H9F 0.8500 . ? O10 H10D 0.8499 . ? O10 H10E 0.8499 . ? O11 O9 1.265(11) 2_746 ? O11 H11C 0.8499 . ? O11 H11D 0.8500 . ? 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 C6 C1 C2 107.8(3) . . ? C6 C1 C7 103.0(3) . . ? C2 C1 C7 102.0(3) . . ? C6 C1 C10 116.3(3) . . ? C2 C1 C10 115.3(3) . . ? C7 C1 C10 110.7(3) . . ? C1 C2 C3 102.8(3) . . ? C1 C2 H2C 111.2 . . ? C3 C2 H2C 111.2 . . ? C1 C2 H2D 111.2 . . ? C3 C2 H2D 111.2 . . ? H2C C2 H2D 109.1 . . ? C4 C3 C2 101.7(3) . . ? C4 C3 H3C 111.4 . . ? C2 C3 H3C 111.4 . . ? C4 C3 H3D 111.4 . . ? C2 C3 H3D 111.4 . . ? H3C C3 H3D 109.3 . . ? C3 C4 C5 107.3(3) . . ? C3 C4 C7 103.2(3) . . ? C5 C4 C7 104.1(3) . . ? C3 C4 H4C 113.8 . . ? C5 C4 H4C 113.8 . . ? C7 C4 H4C 113.8 . . ? C6 C5 C4 102.6(3) . . ? C6 C5 H5C 111.2 . . ? C4 C5 H5C 111.2 . . ? C6 C5 H5D 111.2 . . ? C4 C5 H5D 111.2 . . ? H5C C5 H5D 109.2 . . ? N3 C6 C1 127.4(3) . . ? N3 C6 C5 128.9(3) . . ? C1 C6 C5 103.7(3) . . ? C9 C7 C4 116.5(3) . . ? C9 C7 C1 115.0(3) . . ? C4 C7 C1 91.2(3) . . ? C9 C7 C8 108.5(3) . . ? C4 C7 C8 113.1(3) . . ? C1 C7 C8 111.7(3) . . ? C7 C8 H8C 109.5 . . ? C7 C8 H8D 109.5 . . ? H8C C8 H8D 109.5 . . ? C7 C8 H8E 109.5 . . ? H8C C8 H8E 109.5 . . ? H8D C8 H8E 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C1 C10 S1 118.5(3) . . ? C1 C10 H10A 107.7 . . ? S1 C10 H10A 107.7 . . ? C1 C10 H10B 107.7 . . ? S1 C10 H10B 107.7 . . ? H10A C10 H10B 107.1 . . ? N1 C11 C12 116.0(3) . . ? N1 C11 H11A 108.3 . . ? C12 C11 H11A 108.3 . . ? N1 C11 H11B 108.3 . . ? C12 C11 H11B 108.3 . . ? H11A C11 H11B 107.4 . . ? N2 C12 C11 117.7(3) . . ? N2 C12 H12A 107.9 . . ? C11 C12 H12A 107.9 . . ? N2 C12 H12B 107.9 . . ? C11 C12 H12B 107.9 . . ? H12A C12 H12B 107.2 . . ? C14 C13 S2 118.7(2) . . ? C14 C13 H13A 107.6 . . ? S2 C13 H13A 107.6 . . ? C14 C13 H13B 107.6 . . ? S2 C13 H13B 107.6 . . ? H13A C13 H13B 107.1 . . ? C19 C14 C13 116.9(3) . . ? C19 C14 C15 107.8(3) . . ? C13 C14 C15 116.3(3) . . ? C19 C14 C20 101.1(3) . . ? C13 C14 C20 111.6(3) . . ? C15 C14 C20 100.9(3) . . ? C16 C15 C14 103.3(3) . . ? C16 C15 H15A 111.1 . . ? C14 C15 H15A 111.1 . . ? C16 C15 H15B 111.1 . . ? C14 C15 H15B 111.1 . . ? H15A C15 H15B 109.1 . . ? C17 C16 C15 104.2(3) . . ? C17 C16 H16A 110.9 . . ? C15 C16 H16A 110.9 . . ? C17 C16 H16B 110.9 . . ? C15 C16 H16B 110.9 . . ? H16A C16 H16B 108.9 . . ? C16 C17 C18 110.4(3) . . ? C16 C17 C20 101.7(3) . . ? C18 C17 C20 101.5(3) . . ? C16 C17 H17A 114.0 . . ? C18 C17 H17A 114.0 . . ? C20 C17 H17A 114.0 . . ? C19 C18 C17 102.0(3) . . ? C19 C18 H18A 111.4 . . ? C17 C18 H18A 111.4 . . ? C19 C18 H18B 111.4 . . ? C17 C18 H18B 111.4 . . ? H18A C18 H18B 109.2 . . ? N4 C19 C14 126.8(3) . . ? N4 C19 C18 128.3(3) . . ? C14 C19 C18 104.9(3) . . ? C22 C20 C21 108.7(3) . . ? C22 C20 C17 113.0(3) . . ? C21 C20 C17 112.8(3) . . ? C22 C20 C14 115.3(3) . . ? C21 C20 C14 114.0(3) . . ? C17 C20 C14 92.5(3) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N4 C23 C24 110.4(3) . . ? N4 C23 H23A 109.6 . . ? C24 C23 H23A 109.6 . . ? N4 C23 H23B 109.6 . . ? C24 C23 H23B 109.6 . . ? H23A C23 H23B 108.1 . . ? N3 C24 C23 111.4(3) . . ? N3 C24 H24A 109.3 . . ? C23 C24 H24A 109.3 . . ? N3 C24 H24B 109.3 . . ? C23 C24 H24B 109.3 . . ? H24A C24 H24B 108.0 . . ? C26 C25 C34 116.5(3) . . ? C26 C25 C30 105.5(3) . . ? C34 C25 C30 118.5(3) . . ? C26 C25 C31 101.4(3) . . ? C34 C25 C31 112.4(3) . . ? C30 C25 C31 100.1(3) . . ? C25 C26 C27 104.1(3) . . ? C25 C26 H26A 110.9 . . ? C27 C26 H26A 110.9 . . ? C25 C26 H26B 110.9 . . ? C27 C26 H26B 110.9 . . ? H26A C26 H26B 109.0 . . ? C28 C27 C26 101.2(3) . . ? C28 C27 H27A 111.5 . . ? C26 C27 H27A 111.5 . . ? C28 C27 H27B 111.5 . . ? C26 C27 H27B 111.5 . . ? H27A C27 H27B 109.3 . . ? C31 C28 C29 102.5(3) . . ? C31 C28 C27 102.0(4) . . ? C29 C28 C27 108.1(4) . . ? C31 C28 H28A 114.3 . . ? C29 C28 H28A 114.3 . . ? C27 C28 H28A 114.3 . . ? C30 C29 C28 104.7(3) . . ? C30 C29 H29A 110.8 . . ? C28 C29 H29A 110.8 . . ? C30 C29 H29B 110.8 . . ? C28 C29 H29B 110.8 . . ? H29A C29 H29B 108.9 . . ? N7 C30 C29 131.6(4) . . ? N7 C30 C25 123.9(3) . . ? C29 C30 C25 104.5(3) . . ? C28 C31 C32 113.7(3) . . ? C28 C31 C33 114.3(3) . . ? C32 C31 C33 110.0(3) . . ? C28 C31 C25 94.1(3) . . ? C32 C31 C25 112.0(3) . . ? C33 C31 C25 111.8(3) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C25 C34 S3 118.1(2) . . ? C25 C34 H34A 107.8 . . ? S3 C34 H34A 107.8 . . ? C25 C34 H34B 107.8 . . ? S3 C34 H34B 107.8 . . ? H34A C34 H34B 107.1 . . ? C36 C35 N5 115.1(3) . . ? C36 C35 H35A 108.5 . . ? N5 C35 H35A 108.5 . . ? C36 C35 H35B 108.5 . . ? N5 C35 H35B 108.5 . . ? H35A C35 H35B 107.5 . . ? N6 C36 C35 118.9(3) . . ? N6 C36 H36A 107.6 . . ? C35 C36 H36A 107.6 . . ? N6 C36 H36B 107.6 . . ? C35 C36 H36B 107.6 . . ? H36A C36 H36B 107.0 . . ? C38 C37 S4 118.8(2) . . ? C38 C37 H37A 107.6 . . ? S4 C37 H37A 107.6 . . ? C38 C37 H37B 107.6 . . ? S4 C37 H37B 107.6 . . ? H37A C37 H37B 107.1 . . ? C39 C38 C43 106.3(3) . . ? C39 C38 C37 117.4(3) . . ? C43 C38 C37 116.5(3) . . ? C39 C38 C44 102.6(3) . . ? C43 C38 C44 100.6(3) . . ? C37 C38 C44 111.4(3) . . ? C40 C39 C38 105.6(3) . . ? C40 C39 H39A 110.6 . . ? C38 C39 H39A 110.6 . . ? C40 C39 H39B 110.6 . . ? C38 C39 H39B 110.6 . . ? H39A C39 H39B 108.8 . . ? C39 C40 C41 101.9(3) . . ? C39 C40 H40A 111.4 . . ? C41 C40 H40A 111.4 . . ? C39 C40 H40B 111.4 . . ? C41 C40 H40B 111.4 . . ? H40A C40 H40B 109.3 . . ? C40 C41 C44 104.1(3) . . ? C40 C41 C42 107.9(3) . . ? C44 C41 C42 102.8(3) . . ? C40 C41 H41A 113.7 . . ? C44 C41 H41A 113.7 . . ? C42 C41 H41A 113.7 . . ? C43 C42 C41 101.9(3) . . ? C43 C42 H42A 111.4 . . ? C41 C42 H42A 111.4 . . ? C43 C42 H42B 111.4 . . ? C41 C42 H42B 111.4 . . ? H42A C42 H42B 109.2 . . ? N8 C43 C42 129.3(3) . . ? N8 C43 C38 126.7(3) . . ? C42 C43 C38 104.0(3) . . ? C45 C44 C46 108.8(3) . . ? C45 C44 C41 113.7(3) . . ? C46 C44 C41 114.1(3) . . ? C45 C44 C38 114.6(3) . . ? C46 C44 C38 113.8(3) . . ? C41 C44 C38 91.1(3) . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N8 C47 C48 109.5(3) . . ? N8 C47 H47A 109.8 . . ? C48 C47 H47A 109.8 . . ? N8 C47 H47B 109.8 . . ? C48 C47 H47B 109.8 . . ? H47A C47 H47B 108.2 . . ? N7 C48 C47 109.7(3) . . ? N7 C48 H48A 109.7 . . ? C47 C48 H48A 109.7 . . ? N7 C48 H48B 109.7 . . ? C47 C48 H48B 109.7 . . ? H48A C48 H48B 108.2 . . ? C11 N1 S1 125.9(3) . . ? C11 N1 H1B 117.1 . . ? S1 N1 H1B 117.1 . . ? C12 N2 S2 123.1(2) . . ? C12 N2 H2B 118.4 . . ? S2 N2 H2B 118.4 . . ? C6 N3 C24 117.8(3) . . ? C19 N4 C23 122.0(3) . . ? C35 N5 S3 119.1(2) . . ? C35 N5 H5B 120.4 . . ? S3 N5 H5B 120.4 . . ? C36 N6 S4 126.1(3) . . ? C36 N6 H6B 116.9 . . ? S4 N6 H6B 116.9 . . ? C30 N7 C48 121.0(3) . . ? C43 N8 C47 116.1(3) . . ? O11 O9 H9F 129.7 2_756 . ? H9E O9 H9F 109.5 . . ? H10D O10 H10E 109.5 . . ? O9 O11 H11C 107.9 2_746 . ? H11C O11 H11D 109.5 . . ? O2 S1 O1 118.56(17) . . ? O2 S1 N1 107.09(17) . . ? O1 S1 N1 107.45(17) . . ? O2 S1 C10 108.00(18) . . ? O1 S1 C10 108.70(16) . . ? N1 S1 C10 106.42(18) . . ? O3 S2 O4 118.93(17) . . ? O3 S2 N2 109.27(17) . . ? O4 S2 N2 106.08(16) . . ? O3 S2 C13 109.19(18) . . ? O4 S2 C13 105.55(16) . . ? N2 S2 C13 107.22(17) . . ? O5 S3 O6 121.39(19) . . ? O5 S3 N5 106.95(16) . . ? O6 S3 N5 106.30(17) . . ? O5 S3 C34 109.38(18) . . ? O6 S3 C34 104.54(17) . . ? N5 S3 C34 107.62(18) . . ? O7 S4 O8 119.19(17) . . ? O7 S4 N6 108.70(17) . . ? O8 S4 N6 106.33(18) . . ? O7 S4 C37 108.01(16) . . ? O8 S4 C37 107.38(17) . . ? N6 S4 C37 106.60(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 71.7(4) . . . . ? C7 C1 C2 C3 -36.4(4) . . . . ? C10 C1 C2 C3 -156.5(3) . . . . ? C1 C2 C3 C4 0.0(4) . . . . ? C2 C3 C4 C5 -71.9(4) . . . . ? C2 C3 C4 C7 37.7(4) . . . . ? C3 C4 C5 C6 73.6(3) . . . . ? C7 C4 C5 C6 -35.3(4) . . . . ? C2 C1 C6 N3 110.9(4) . . . . ? C7 C1 C6 N3 -141.7(3) . . . . ? C10 C1 C6 N3 -20.4(5) . . . . ? C2 C1 C6 C5 -71.2(3) . . . . ? C7 C1 C6 C5 36.2(3) . . . . ? C10 C1 C6 C5 157.6(3) . . . . ? C4 C5 C6 N3 176.7(3) . . . . ? C4 C5 C6 C1 -1.2(3) . . . . ? C3 C4 C7 C9 61.3(4) . . . . ? C5 C4 C7 C9 173.2(4) . . . . ? C3 C4 C7 C1 -57.7(3) . . . . ? C5 C4 C7 C1 54.2(3) . . . . ? C3 C4 C7 C8 -172.0(3) . . . . ? C5 C4 C7 C8 -60.1(4) . . . . ? C6 C1 C7 C9 -174.9(3) . . . . ? C2 C1 C7 C9 -63.2(4) . . . . ? C10 C1 C7 C9 60.0(4) . . . . ? C6 C1 C7 C4 -54.7(3) . . . . ? C2 C1 C7 C4 57.1(3) . . . . ? C10 C1 C7 C4 -179.8(3) . . . . ? C6 C1 C7 C8 60.8(4) . . . . ? C2 C1 C7 C8 172.6(3) . . . . ? C10 C1 C7 C8 -64.2(4) . . . . ? C6 C1 C10 S1 69.4(4) . . . . ? C2 C1 C10 S1 -58.3(4) . . . . ? C7 C1 C10 S1 -173.4(3) . . . . ? N1 C11 C12 N2 48.2(5) . . . . ? S2 C13 C14 C19 70.1(4) . . . . ? S2 C13 C14 C15 -59.2(4) . . . . ? S2 C13 C14 C20 -174.1(2) . . . . ? C19 C14 C15 C16 72.3(4) . . . . ? C13 C14 C15 C16 -154.1(3) . . . . ? C20 C14 C15 C16 -33.2(4) . . . . ? C14 C15 C16 C17 -3.4(4) . . . . ? C15 C16 C17 C18 -68.0(4) . . . . ? C15 C16 C17 C20 39.1(4) . . . . ? C16 C17 C18 C19 71.4(4) . . . . ? C20 C17 C18 C19 -35.9(3) . . . . ? C13 C14 C19 N4 -23.7(5) . . . . ? C15 C14 C19 N4 109.5(4) . . . . ? C20 C14 C19 N4 -145.1(4) . . . . ? C13 C14 C19 C18 158.3(3) . . . . ? C15 C14 C19 C18 -68.4(3) . . . . ? C20 C14 C19 C18 36.9(3) . . . . ? C17 C18 C19 N4 -178.6(4) . . . . ? C17 C18 C19 C14 -0.7(4) . . . . ? C16 C17 C20 C22 61.2(4) . . . . ? C18 C17 C20 C22 175.2(3) . . . . ? C16 C17 C20 C21 -175.0(3) . . . . ? C18 C17 C20 C21 -61.1(4) . . . . ? C16 C17 C20 C14 -57.6(3) . . . . ? C18 C17 C20 C14 56.3(3) . . . . ? C19 C14 C20 C22 -173.6(3) . . . . ? C13 C14 C20 C22 61.4(4) . . . . ? C15 C14 C20 C22 -62.7(4) . . . . ? C19 C14 C20 C21 59.6(4) . . . . ? C13 C14 C20 C21 -65.4(4) . . . . ? C15 C14 C20 C21 170.5(3) . . . . ? C19 C14 C20 C17 -56.7(3) . . . . ? C13 C14 C20 C17 178.3(3) . . . . ? C15 C14 C20 C17 54.2(3) . . . . ? N4 C23 C24 N3 63.3(4) . . . . ? C34 C25 C26 C27 -152.6(3) . . . . ? C30 C25 C26 C27 73.7(4) . . . . ? C31 C25 C26 C27 -30.2(4) . . . . ? C25 C26 C27 C28 -4.6(4) . . . . ? C26 C27 C28 C31 40.8(4) . . . . ? C26 C27 C28 C29 -66.8(4) . . . . ? C31 C28 C29 C30 -35.1(4) . . . . ? C27 C28 C29 C30 72.1(4) . . . . ? C28 C29 C30 N7 176.3(4) . . . . ? C28 C29 C30 C25 -1.0(4) . . . . ? C26 C25 C30 N7 111.5(4) . . . . ? C34 C25 C30 N7 -21.1(5) . . . . ? C31 C25 C30 N7 -143.6(4) . . . . ? C26 C25 C30 C29 -70.9(4) . . . . ? C34 C25 C30 C29 156.5(3) . . . . ? C31 C25 C30 C29 34.0(4) . . . . ? C29 C28 C31 C32 -62.6(4) . . . . ? C27 C28 C31 C32 -174.4(3) . . . . ? C29 C28 C31 C33 169.9(3) . . . . ? C27 C28 C31 C33 58.0(4) . . . . ? C29 C28 C31 C25 53.7(4) . . . . ? C27 C28 C31 C25 -58.1(4) . . . . ? C26 C25 C31 C28 54.5(3) . . . . ? C34 C25 C31 C28 179.6(3) . . . . ? C30 C25 C31 C28 -53.7(3) . . . . ? C26 C25 C31 C32 172.2(3) . . . . ? C34 C25 C31 C32 -62.7(4) . . . . ? C30 C25 C31 C32 64.0(4) . . . . ? C26 C25 C31 C33 -63.7(4) . . . . ? C34 C25 C31 C33 61.4(4) . . . . ? C30 C25 C31 C33 -172.0(3) . . . . ? C26 C25 C34 S3 -57.0(4) . . . . ? C30 C25 C34 S3 70.6(4) . . . . ? C31 C25 C34 S3 -173.3(3) . . . . ? N5 C35 C36 N6 43.6(5) . . . . ? S4 C37 C38 C39 -58.8(4) . . . . ? S4 C37 C38 C43 68.8(4) . . . . ? S4 C37 C38 C44 -176.7(3) . . . . ? C43 C38 C39 C40 74.0(4) . . . . ? C37 C38 C39 C40 -153.6(3) . . . . ? C44 C38 C39 C40 -31.2(4) . . . . ? C38 C39 C40 C41 -4.1(4) . . . . ? C39 C40 C41 C44 39.7(4) . . . . ? C39 C40 C41 C42 -69.0(4) . . . . ? C40 C41 C42 C43 73.9(4) . . . . ? C44 C41 C42 C43 -35.8(4) . . . . ? C41 C42 C43 N8 176.2(4) . . . . ? C41 C42 C43 C38 -2.8(4) . . . . ? C39 C38 C43 N8 113.1(4) . . . . ? C37 C38 C43 N8 -19.8(5) . . . . ? C44 C38 C43 N8 -140.3(4) . . . . ? C39 C38 C43 C42 -67.9(3) . . . . ? C37 C38 C43 C42 159.2(3) . . . . ? C44 C38 C43 C42 38.7(3) . . . . ? C40 C41 C44 C45 62.0(4) . . . . ? C42 C41 C44 C45 174.4(3) . . . . ? C40 C41 C44 C46 -172.4(3) . . . . ? C42 C41 C44 C46 -60.0(4) . . . . ? C40 C41 C44 C38 -55.7(3) . . . . ? C42 C41 C44 C38 56.8(3) . . . . ? C39 C38 C44 C45 -65.3(4) . . . . ? C43 C38 C44 C45 -174.8(3) . . . . ? C37 C38 C44 C45 61.2(4) . . . . ? C39 C38 C44 C46 168.6(3) . . . . ? C43 C38 C44 C46 59.1(4) . . . . ? C37 C38 C44 C46 -64.9(4) . . . . ? C39 C38 C44 C41 51.6(3) . . . . ? C43 C38 C44 C41 -57.9(3) . . . . ? C37 C38 C44 C41 178.1(3) . . . . ? N8 C47 C48 N7 65.1(4) . . . . ? C12 C11 N1 S1 69.0(5) . . . . ? C11 C12 N2 S2 150.8(3) . . . . ? C1 C6 N3 C24 -179.3(3) . . . . ? C5 C6 N3 C24 3.3(5) . . . . ? C23 C24 N3 C6 -168.3(3) . . . . ? C14 C19 N4 C23 -176.3(3) . . . . ? C18 C19 N4 C23 1.2(6) . . . . ? C24 C23 N4 C19 117.9(4) . . . . ? C36 C35 N5 S3 154.2(3) . . . . ? C35 C36 N6 S4 68.3(5) . . . . ? C29 C30 N7 C48 4.3(6) . . . . ? C25 C30 N7 C48 -178.9(3) . . . . ? C47 C48 N7 C30 114.0(4) . . . . ? C42 C43 N8 C47 0.4(5) . . . . ? C38 C43 N8 C47 179.2(3) . . . . ? C48 C47 N8 C43 -165.9(3) . . . . ? C11 N1 S1 O2 15.5(4) . . . . ? C11 N1 S1 O1 143.9(3) . . . . ? C11 N1 S1 C10 -99.8(3) . . . . ? C1 C10 S1 O2 164.5(3) . . . . ? C1 C10 S1 O1 34.6(3) . . . . ? C1 C10 S1 N1 -80.8(3) . . . . ? C12 N2 S2 O3 159.9(3) . . . . ? C12 N2 S2 O4 30.5(3) . . . . ? C12 N2 S2 C13 -81.9(3) . . . . ? C14 C13 S2 O3 32.8(3) . . . . ? C14 C13 S2 O4 161.7(3) . . . . ? C14 C13 S2 N2 -85.5(3) . . . . ? C35 N5 S3 O5 160.8(3) . . . . ? C35 N5 S3 O6 29.8(3) . . . . ? C35 N5 S3 C34 -81.7(3) . . . . ? C25 C34 S3 O5 31.8(4) . . . . ? C25 C34 S3 O6 163.2(3) . . . . ? C25 C34 S3 N5 -84.0(3) . . . . ? C36 N6 S4 O7 147.0(3) . . . . ? C36 N6 S4 O8 17.6(4) . . . . ? C36 N6 S4 C37 -96.8(3) . . . . ? C38 C37 S4 O7 34.1(3) . . . . ? C38 C37 S4 O8 163.8(3) . . . . ? C38 C37 S4 N6 -82.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.238 _refine_diff_density_min -0.276 _refine_diff_density_rms 0.049 data_081106bm _database_code_depnum_ccdc_archive 'CCDC 753364' #TrackingRef 'nju03 RMC-Ni.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H38 N4 Ni O4 S2' _chemical_formula_sum 'C24 H38 N4 Ni O4 S2' _chemical_formula_weight 569.41 _chemical_absolute_configuration unknown 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.047(2) _cell_length_b 12.258(2) _cell_length_c 17.014(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2512.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1873 _cell_measurement_theta_min 1.95 _cell_measurement_theta_max 25.52 _exptl_crystal_description Prism _exptl_crystal_colour Green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.505 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 0.978 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.79 _exptl_absorpt_correction_T_max 0.86 _exptl_absorpt_process_details '(SADABS; Bruker, 2002)' _diffrn_ambient_temperature 298(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_type 'Bruker smart apex II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13137 _diffrn_reflns_av_R_equivalents 0.0417 _diffrn_reflns_av_sigmaI/netI 0.0584 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 25.50 _reflns_number_total 4679 _reflns_number_gt 4151 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Bruker, 2002)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0290P)^2^] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.009(16) _refine_ls_number_reflns 4679 _refine_ls_number_parameters 320 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.0795 _refine_ls_wR_factor_gt 0.0771 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.986 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.10874(4) 1.09476(3) 0.75171(2) 0.02706(12) Uani 1 1 d . . . S1 S 0.26688(8) 1.04168(8) 0.62015(5) 0.0366(2) Uani 1 1 d . . . N3 N 0.0645(3) 1.1199(2) 0.85922(16) 0.0285(7) Uani 1 1 d . . . N2 N 0.2511(2) 1.0944(2) 0.79815(14) 0.0285(6) Uani 1 1 d . . . C7 C 0.3140(3) 0.9111(3) 0.7563(2) 0.0282(7) Uani 1 1 d . . . N1 N 0.1550(3) 1.1028(2) 0.64570(15) 0.0346(7) Uani 1 1 d . . . N4 N -0.0379(2) 1.0931(2) 0.71221(15) 0.0326(7) Uani 1 1 d . . . C3 C 0.4343(3) 0.8651(3) 0.7660(2) 0.0358(9) Uani 1 1 d . . . C6 C 0.2468(3) 0.8366(3) 0.8124(2) 0.0387(10) Uani 1 1 d . . . H6A H 0.1807 0.8734 0.8312 0.046 Uiso 1 1 calc R . . H6B H 0.2253 0.7694 0.7864 0.046 Uiso 1 1 calc R . . C10 C 0.2541(3) 1.1889(3) 0.8502(2) 0.0381(9) Uani 1 1 d . . . H10A H 0.2540 1.2559 0.8199 0.046 Uiso 1 1 calc R . . H10B H 0.3205 1.1874 0.8825 0.046 Uiso 1 1 calc R . . O2 O 0.3627(2) 1.1028(2) 0.64369(14) 0.0483(7) Uani 1 1 d . . . C8 C 0.3191(3) 1.0156(3) 0.80404(19) 0.0308(9) Uani 1 1 d . . . O1 O 0.2606(2) 1.0115(2) 0.53842(14) 0.0525(8) Uani 1 1 d . . . C14 C -0.0228(3) 1.1000(3) 0.89708(18) 0.0340(9) Uani 1 1 d . . . C9 C 0.2690(3) 0.9152(3) 0.67236(19) 0.0376(9) Uani 1 1 d . . . H9A H 0.1935 0.8879 0.6738 0.045 Uiso 1 1 calc R . . H9B H 0.3120 0.8640 0.6413 0.045 Uiso 1 1 calc R . . C12 C 0.0636(3) 1.0985(3) 0.58918(19) 0.0376(9) Uani 1 1 d . . . H12A H 0.0499 1.0240 0.5724 0.045 Uiso 1 1 calc R . . H12B H 0.0801 1.1426 0.5433 0.045 Uiso 1 1 calc R . . C1 C 0.4062(3) 0.9986(3) 0.8674(2) 0.0391(9) Uani 1 1 d . . . H1A H 0.3768 1.0136 0.9194 0.047 Uiso 1 1 calc R . . H1B H 0.4714 1.0434 0.8584 0.047 Uiso 1 1 calc R . . C4 C 0.4469(3) 0.7467(3) 0.7399(2) 0.0499(11) Uani 1 1 d . . . H4A H 0.5175 0.7193 0.7571 0.075 Uiso 1 1 calc R . . H4B H 0.4428 0.7428 0.6836 0.075 Uiso 1 1 calc R . . H4C H 0.3886 0.7037 0.7625 0.075 Uiso 1 1 calc R . . C13 C -0.0352(3) 1.1436(3) 0.6331(2) 0.0378(10) Uani 1 1 d . . . H13A H -0.0289 1.2222 0.6377 0.045 Uiso 1 1 calc R . . H13B H -0.1031 1.1268 0.6049 0.045 Uiso 1 1 calc R . . C11 C 0.1515(3) 1.1824(3) 0.9013(2) 0.0354(9) Uani 1 1 d . . . H11A H 0.1692 1.1467 0.9506 0.042 Uiso 1 1 calc R . . H11B H 0.1247 1.2553 0.9129 0.042 Uiso 1 1 calc R . . C5 C 0.5241(3) 0.9307(3) 0.7261(2) 0.0503(11) Uani 1 1 d . . . H5A H 0.5224 0.9169 0.6706 0.075 Uiso 1 1 calc R . . H5B H 0.5952 0.9099 0.7468 0.075 Uiso 1 1 calc R . . H5C H 0.5119 1.0070 0.7356 0.075 Uiso 1 1 calc R . . O5 O -0.2103(3) 0.9861(3) 0.68816(16) 0.0777(11) Uani 1 1 d . . . C2 C 0.3281(4) 0.8139(3) 0.8803(2) 0.0497(11) Uani 1 1 d . . . H2A H 0.2990 0.8407 0.9298 0.060 Uiso 1 1 calc R . . H2B H 0.3432 0.7365 0.8851 0.060 Uiso 1 1 calc R . . C21 C -0.0485(4) 0.9102(4) 0.9917(2) 0.0542(12) Uani 1 1 d . . . H21A H -0.0453 0.8395 0.9675 0.081 Uiso 1 1 calc R . . H21B H -0.0592 0.9020 1.0473 0.081 Uiso 1 1 calc R . . H21C H 0.0197 0.9484 0.9821 0.081 Uiso 1 1 calc R . . C18 C -0.1188(3) 1.0255(3) 0.8741(2) 0.0345(9) Uani 1 1 d . . . C23 C -0.0924(4) 0.9405(3) 0.81213(19) 0.0372(9) Uani 1 1 d . . . H23A H -0.1436 0.8802 0.8196 0.045 Uiso 1 1 calc R . . H23B H -0.0186 0.9128 0.8231 0.045 Uiso 1 1 calc R . . C20 C -0.2483(4) 0.9021(4) 0.9569(2) 0.0699(14) Uani 1 1 d . . . H20A H -0.3099 0.9411 0.9345 0.105 Uiso 1 1 calc R . . H20B H -0.2658 0.8815 1.0099 0.105 Uiso 1 1 calc R . . H20C H -0.2339 0.8379 0.9263 0.105 Uiso 1 1 calc R . . C24 C 0.4317(3) 0.8762(3) 0.8563(2) 0.0413(10) Uani 1 1 d . . . H24 H 0.4996 0.8516 0.8825 0.050 Uiso 1 1 calc R . . C17 C -0.2194(3) 1.0995(4) 0.8601(2) 0.0498(11) Uani 1 1 d . . . H17A H -0.2801 1.0589 0.8367 0.060 Uiso 1 1 calc R . . H17B H -0.2002 1.1599 0.8259 0.060 Uiso 1 1 calc R . . C22 C -0.1457(3) 0.9752(3) 0.9568(2) 0.0414(10) Uani 1 1 d . . . C19 C -0.1622(4) 1.0872(4) 0.9953(2) 0.0531(12) Uani 1 1 d . . . H19 H -0.1816 1.0841 1.0512 0.064 Uiso 1 1 calc R . . C15 C -0.0529(4) 1.1435(4) 0.9783(2) 0.0522(12) Uani 1 1 d . . . H15A H 0.0030 1.1240 1.0168 0.063 Uiso 1 1 calc R . . H15B H -0.0615 1.2221 0.9776 0.063 Uiso 1 1 calc R . . C16 C -0.2510(4) 1.1407(4) 0.9431(2) 0.0675(15) Uani 1 1 d . . . H16A H -0.2472 1.2196 0.9461 0.081 Uiso 1 1 calc R . . H16B H -0.3249 1.1169 0.9578 0.081 Uiso 1 1 calc R . . S4 S -0.09655(10) 0.97639(9) 0.71223(6) 0.0467(3) Uani 1 1 d . . . O7 O -0.0368(3) 0.8909(3) 0.67202(17) 0.0720(10) Uani 1 1 d . . . 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 Ni1 0.0297(2) 0.0301(2) 0.0214(2) -0.0013(2) -0.0001(2) 0.0006(2) S1 0.0370(6) 0.0483(6) 0.0244(5) 0.0026(4) 0.0046(4) 0.0065(5) N3 0.0387(19) 0.0267(17) 0.0202(15) 0.0010(12) 0.0010(13) 0.0034(14) N2 0.0274(17) 0.0324(15) 0.0256(15) -0.0028(14) -0.0045(12) -0.0016(16) C7 0.0264(17) 0.0289(16) 0.0293(17) -0.004(2) -0.0005(16) 0.0001(15) N1 0.0416(19) 0.0403(18) 0.0218(15) -0.0006(15) 0.0012(13) 0.0006(17) N4 0.0324(18) 0.0430(17) 0.0225(14) -0.0005(15) -0.0013(12) 0.0005(16) C3 0.031(2) 0.0349(19) 0.042(2) -0.0029(17) -0.0018(17) 0.0027(16) C6 0.042(3) 0.032(2) 0.042(2) -0.0001(17) 0.002(2) -0.001(2) C10 0.040(2) 0.034(2) 0.041(2) -0.0048(18) -0.0092(19) 0.001(2) O2 0.0389(17) 0.0579(17) 0.0482(16) 0.0088(15) 0.0062(12) -0.0069(15) C8 0.026(2) 0.038(2) 0.028(2) 0.0035(17) 0.0046(16) -0.0036(19) O1 0.0542(19) 0.076(2) 0.0272(14) 0.0000(13) 0.0049(13) 0.0177(17) C14 0.049(3) 0.031(2) 0.0214(18) 0.0032(18) 0.0024(17) 0.011(2) C9 0.042(2) 0.037(2) 0.034(2) -0.0076(18) -0.0033(17) 0.002(2) C12 0.042(2) 0.047(2) 0.0244(18) 0.0028(19) -0.0009(16) 0.004(2) C1 0.034(2) 0.047(2) 0.036(2) -0.0054(17) -0.0087(19) 0.003(2) C4 0.046(3) 0.041(2) 0.063(3) -0.007(2) -0.004(2) 0.0149(19) C13 0.036(2) 0.051(2) 0.027(2) -0.0007(18) -0.0051(18) 0.007(2) C11 0.049(3) 0.033(2) 0.0246(19) -0.0044(16) -0.0051(17) -0.0012(19) C5 0.031(2) 0.065(3) 0.055(3) -0.003(2) 0.0027(19) 0.008(2) O5 0.057(2) 0.131(3) 0.0452(19) 0.0122(19) -0.0129(15) -0.038(2) C2 0.060(3) 0.047(3) 0.043(2) 0.013(2) -0.003(2) -0.001(2) C21 0.059(3) 0.059(3) 0.045(2) 0.023(2) -0.001(2) -0.005(3) C18 0.037(2) 0.040(2) 0.0261(19) 0.0059(16) 0.0038(17) 0.003(2) C23 0.035(2) 0.036(2) 0.040(2) -0.0006(16) 0.0024(18) -0.007(2) C20 0.057(3) 0.094(4) 0.059(3) 0.028(3) 0.014(2) -0.008(3) C24 0.038(3) 0.045(2) 0.040(2) 0.0031(18) -0.0097(18) 0.0071(19) C17 0.047(3) 0.065(3) 0.037(2) 0.011(2) 0.0040(19) 0.014(2) C22 0.037(2) 0.055(3) 0.031(2) 0.010(2) 0.0081(17) -0.002(2) C19 0.059(3) 0.073(3) 0.028(2) 0.006(2) 0.019(2) 0.005(3) C15 0.073(3) 0.055(3) 0.028(2) -0.008(2) 0.012(2) -0.001(3) C16 0.069(4) 0.083(4) 0.050(3) 0.002(2) 0.021(3) 0.024(3) S4 0.0457(7) 0.0606(7) 0.0339(5) -0.0104(5) 0.0013(5) -0.0220(6) O7 0.103(3) 0.055(2) 0.0587(19) -0.0267(17) 0.0276(18) -0.027(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 Ni1 N2 1.888(3) . ? Ni1 N4 1.890(3) . ? Ni1 N1 1.890(3) . ? Ni1 N3 1.930(3) . ? S1 O2 1.433(3) . ? S1 O1 1.441(3) . ? S1 N1 1.602(3) . ? S1 C9 1.787(4) . ? N3 C14 1.258(5) . ? N3 C11 1.482(4) . ? N2 C8 1.271(4) . ? N2 C10 1.459(4) . ? C7 C8 1.518(4) . ? C7 C9 1.528(4) . ? C7 C6 1.549(5) . ? C7 C3 1.563(5) . ? N1 C12 1.463(4) . ? N4 C13 1.482(4) . ? N4 S4 1.595(3) . ? C3 C5 1.510(5) . ? C3 C4 1.525(5) . ? C3 C24 1.541(5) . ? C6 C2 1.539(5) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C10 C11 1.514(5) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C8 C1 1.519(5) . ? C14 C15 1.524(5) . ? C14 C18 1.525(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C12 C13 1.510(5) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C1 C24 1.544(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? O5 S4 1.436(3) . ? C2 C24 1.519(5) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C21 C22 1.536(6) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C18 C23 1.516(5) . ? C18 C17 1.533(5) . ? C18 C22 1.570(5) . ? C23 S4 1.756(3) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C20 C22 1.527(6) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C24 H24 0.9800 . ? C17 C16 1.547(5) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C22 C19 1.535(6) . ? C19 C15 1.515(6) . ? C19 C16 1.537(6) . ? C19 H19 0.9800 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? S4 O7 1.444(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 N2 Ni1 N4 176.02(12) . . ? N2 Ni1 N1 97.55(13) . . ? N4 Ni1 N1 86.39(13) . . ? N2 Ni1 N3 81.62(12) . . ? N4 Ni1 N3 94.64(13) . . ? N1 Ni1 N3 167.80(13) . . ? O2 S1 O1 116.48(17) . . ? O2 S1 N1 110.96(16) . . ? O1 S1 N1 109.75(16) . . ? O2 S1 C9 107.62(17) . . ? O1 S1 C9 104.94(17) . . ? N1 S1 C9 106.44(17) . . ? C14 N3 C11 116.4(3) . . ? C14 N3 Ni1 133.3(3) . . ? C11 N3 Ni1 110.2(2) . . ? C8 N2 C10 122.7(3) . . ? C8 N2 Ni1 128.3(2) . . ? C10 N2 Ni1 106.0(2) . . ? C8 C7 C9 119.1(3) . . ? C8 C7 C6 100.9(3) . . ? C9 C7 C6 114.2(3) . . ? C8 C7 C3 102.1(3) . . ? C9 C7 C3 116.1(3) . . ? C6 C7 C3 102.0(3) . . ? C12 N1 S1 116.0(2) . . ? C12 N1 Ni1 113.8(2) . . ? S1 N1 Ni1 118.88(17) . . ? C13 N4 S4 112.6(2) . . ? C13 N4 Ni1 107.3(2) . . ? S4 N4 Ni1 115.07(17) . . ? C5 C3 C4 107.7(3) . . ? C5 C3 C24 114.6(3) . . ? C4 C3 C24 112.1(3) . . ? C5 C3 C7 115.1(3) . . ? C4 C3 C7 113.9(3) . . ? C24 C3 C7 93.1(3) . . ? C2 C6 C7 103.7(3) . . ? C2 C6 H6A 111.0 . . ? C7 C6 H6A 111.0 . . ? C2 C6 H6B 111.0 . . ? C7 C6 H6B 111.0 . . ? H6A C6 H6B 109.0 . . ? N2 C10 C11 106.6(3) . . ? N2 C10 H10A 110.4 . . ? C11 C10 H10A 110.4 . . ? N2 C10 H10B 110.4 . . ? C11 C10 H10B 110.4 . . ? H10A C10 H10B 108.6 . . ? N2 C8 C7 125.0(3) . . ? N2 C8 C1 127.3(3) . . ? C7 C8 C1 107.0(3) . . ? N3 C14 C15 126.5(4) . . ? N3 C14 C18 128.2(3) . . ? C15 C14 C18 105.2(3) . . ? C7 C9 S1 119.9(3) . . ? C7 C9 H9A 107.4 . . ? S1 C9 H9A 107.3 . . ? C7 C9 H9B 107.3 . . ? S1 C9 H9B 107.3 . . ? H9A C9 H9B 106.9 . . ? N1 C12 C13 104.8(3) . . ? N1 C12 H12A 110.8 . . ? C13 C12 H12A 110.8 . . ? N1 C12 H12B 110.8 . . ? C13 C12 H12B 110.8 . . ? H12A C12 H12B 108.9 . . ? C8 C1 C24 100.5(3) . . ? C8 C1 H1A 111.7 . . ? C24 C1 H1A 111.7 . . ? C8 C1 H1B 111.7 . . ? C24 C1 H1B 111.7 . . ? H1A C1 H1B 109.4 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N4 C13 C12 108.3(3) . . ? N4 C13 H13A 110.0 . . ? C12 C13 H13A 110.0 . . ? N4 C13 H13B 110.0 . . ? C12 C13 H13B 110.0 . . ? H13A C13 H13B 108.4 . . ? N3 C11 C10 109.1(3) . . ? N3 C11 H11A 109.9 . . ? C10 C11 H11A 109.9 . . ? N3 C11 H11B 109.9 . . ? C10 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C24 C2 C6 103.3(3) . . ? C24 C2 H2A 111.1 . . ? C6 C2 H2A 111.1 . . ? C24 C2 H2B 111.1 . . ? C6 C2 H2B 111.1 . . ? H2A C2 H2B 109.1 . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C18 C14 115.6(3) . . ? C23 C18 C17 117.7(3) . . ? C14 C18 C17 106.5(3) . . ? C23 C18 C22 113.4(3) . . ? C14 C18 C22 99.3(3) . . ? C17 C18 C22 102.0(3) . . ? C18 C23 S4 119.7(3) . . ? C18 C23 H23A 107.4 . . ? S4 C23 H23A 107.4 . . ? C18 C23 H23B 107.4 . . ? S4 C23 H23B 107.4 . . ? H23A C23 H23B 106.9 . . ? C22 C20 H20A 109.5 . . ? C22 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C22 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C2 C24 C3 103.9(3) . . ? C2 C24 C1 107.0(3) . . ? C3 C24 C1 102.3(3) . . ? C2 C24 H24 114.2 . . ? C3 C24 H24 114.2 . . ? C1 C24 H24 114.2 . . ? C18 C17 C16 104.3(3) . . ? C18 C17 H17A 110.9 . . ? C16 C17 H17A 110.9 . . ? C18 C17 H17B 110.9 . . ? C16 C17 H17B 110.9 . . ? H17A C17 H17B 108.9 . . ? C20 C22 C19 114.8(4) . . ? C20 C22 C21 108.2(3) . . ? C19 C22 C21 113.4(4) . . ? C20 C22 C18 113.5(3) . . ? C19 C22 C18 93.3(3) . . ? C21 C22 C18 113.1(3) . . ? C15 C19 C22 102.3(3) . . ? C15 C19 C16 107.5(4) . . ? C22 C19 C16 103.0(4) . . ? C15 C19 H19 114.3 . . ? C22 C19 H19 114.3 . . ? C16 C19 H19 114.3 . . ? C19 C15 C14 102.7(3) . . ? C19 C15 H15A 111.2 . . ? C14 C15 H15A 111.2 . . ? C19 C15 H15B 111.2 . . ? C14 C15 H15B 111.2 . . ? H15A C15 H15B 109.1 . . ? C19 C16 C17 102.5(3) . . ? C19 C16 H16A 111.3 . . ? C17 C16 H16A 111.3 . . ? C19 C16 H16B 111.3 . . ? C17 C16 H16B 111.3 . . ? H16A C16 H16B 109.2 . . ? O5 S4 O7 113.7(2) . . ? O5 S4 N4 110.4(2) . . ? O7 S4 N4 115.46(18) . . ? O5 S4 C23 108.9(2) . . ? O7 S4 C23 105.2(2) . . ? N4 S4 C23 102.26(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ni1 N3 C14 -153.6(4) . . . . ? N4 Ni1 N3 C14 25.0(4) . . . . ? N1 Ni1 N3 C14 119.4(6) . . . . ? N2 Ni1 N3 C11 31.4(2) . . . . ? N4 Ni1 N3 C11 -150.0(2) . . . . ? N1 Ni1 N3 C11 -55.6(7) . . . . ? N4 Ni1 N2 C8 93.8(19) . . . . ? N1 Ni1 N2 C8 -78.4(3) . . . . ? N3 Ni1 N2 C8 113.9(3) . . . . ? N4 Ni1 N2 C10 -67(2) . . . . ? N1 Ni1 N2 C10 121.3(2) . . . . ? N3 Ni1 N2 C10 -46.4(2) . . . . ? O2 S1 N1 C12 141.0(3) . . . . ? O1 S1 N1 C12 10.8(3) . . . . ? C9 S1 N1 C12 -102.2(3) . . . . ? O2 S1 N1 Ni1 -77.7(2) . . . . ? O1 S1 N1 Ni1 152.17(19) . . . . ? C9 S1 N1 Ni1 39.1(2) . . . . ? N2 Ni1 N1 C12 176.7(3) . . . . ? N4 Ni1 N1 C12 -2.7(3) . . . . ? N3 Ni1 N1 C12 -98.0(7) . . . . ? N2 Ni1 N1 S1 34.6(2) . . . . ? N4 Ni1 N1 S1 -144.9(2) . . . . ? N3 Ni1 N1 S1 119.8(6) . . . . ? N2 Ni1 N4 C13 164.7(18) . . . . ? N1 Ni1 N4 C13 -23.1(2) . . . . ? N3 Ni1 N4 C13 144.7(2) . . . . ? N2 Ni1 N4 S4 -69(2) . . . . ? N1 Ni1 N4 S4 103.05(18) . . . . ? N3 Ni1 N4 S4 -89.14(17) . . . . ? C8 C7 C3 C5 -68.3(4) . . . . ? C9 C7 C3 C5 62.9(4) . . . . ? C6 C7 C3 C5 -172.4(3) . . . . ? C8 C7 C3 C4 166.6(3) . . . . ? C9 C7 C3 C4 -62.2(4) . . . . ? C6 C7 C3 C4 62.6(4) . . . . ? C8 C7 C3 C24 50.7(3) . . . . ? C9 C7 C3 C24 -178.0(3) . . . . ? C6 C7 C3 C24 -53.3(3) . . . . ? C8 C7 C6 C2 -70.5(3) . . . . ? C9 C7 C6 C2 160.5(3) . . . . ? C3 C7 C6 C2 34.5(3) . . . . ? C8 N2 C10 C11 -110.8(4) . . . . ? Ni1 N2 C10 C11 50.9(3) . . . . ? C10 N2 C8 C7 174.5(3) . . . . ? Ni1 N2 C8 C7 17.1(5) . . . . ? C10 N2 C8 C1 5.8(6) . . . . ? Ni1 N2 C8 C1 -151.6(3) . . . . ? C9 C7 C8 N2 32.1(5) . . . . ? C6 C7 C8 N2 -93.7(4) . . . . ? C3 C7 C8 N2 161.4(3) . . . . ? C9 C7 C8 C1 -157.3(3) . . . . ? C6 C7 C8 C1 77.0(3) . . . . ? C3 C7 C8 C1 -27.9(3) . . . . ? C11 N3 C14 C15 6.7(5) . . . . ? Ni1 N3 C14 C15 -168.0(3) . . . . ? C11 N3 C14 C18 -170.9(3) . . . . ? Ni1 N3 C14 C18 14.3(6) . . . . ? C8 C7 C9 S1 20.9(5) . . . . ? C6 C7 C9 S1 140.0(3) . . . . ? C3 C7 C9 S1 -101.8(3) . . . . ? O2 S1 C9 C7 34.6(3) . . . . ? O1 S1 C9 C7 159.3(3) . . . . ? N1 S1 C9 C7 -84.4(3) . . . . ? S1 N1 C12 C13 170.3(2) . . . . ? Ni1 N1 C12 C13 27.0(4) . . . . ? N2 C8 C1 C24 162.7(4) . . . . ? C7 C8 C1 C24 -7.7(4) . . . . ? S4 N4 C13 C12 -83.5(3) . . . . ? Ni1 N4 C13 C12 44.2(3) . . . . ? N1 C12 C13 N4 -45.3(4) . . . . ? C14 N3 C11 C10 174.4(3) . . . . ? Ni1 N3 C11 C10 -9.7(3) . . . . ? N2 C10 C11 N3 -25.7(4) . . . . ? C7 C6 C2 C24 -0.2(4) . . . . ? N3 C14 C18 C23 20.0(5) . . . . ? C15 C14 C18 C23 -158.0(3) . . . . ? N3 C14 C18 C17 -112.8(4) . . . . ? C15 C14 C18 C17 69.2(3) . . . . ? N3 C14 C18 C22 141.6(4) . . . . ? C15 C14 C18 C22 -36.4(4) . . . . ? C14 C18 C23 S4 -83.1(4) . . . . ? C17 C18 C23 S4 44.3(5) . . . . ? C22 C18 C23 S4 163.1(3) . . . . ? C6 C2 C24 C3 -35.0(4) . . . . ? C6 C2 C24 C1 72.7(4) . . . . ? C5 C3 C24 C2 173.9(3) . . . . ? C4 C3 C24 C2 -63.0(4) . . . . ? C7 C3 C24 C2 54.3(3) . . . . ? C5 C3 C24 C1 62.7(4) . . . . ? C4 C3 C24 C1 -174.2(3) . . . . ? C7 C3 C24 C1 -56.9(3) . . . . ? C8 C1 C24 C2 -67.4(4) . . . . ? C8 C1 C24 C3 41.5(4) . . . . ? C23 C18 C17 C16 158.1(4) . . . . ? C14 C18 C17 C16 -70.3(4) . . . . ? C22 C18 C17 C16 33.4(4) . . . . ? C23 C18 C22 C20 -62.3(5) . . . . ? C14 C18 C22 C20 174.5(4) . . . . ? C17 C18 C22 C20 65.2(4) . . . . ? C23 C18 C22 C19 178.7(3) . . . . ? C14 C18 C22 C19 55.5(3) . . . . ? C17 C18 C22 C19 -53.7(4) . . . . ? C23 C18 C22 C21 61.5(5) . . . . ? C14 C18 C22 C21 -61.7(4) . . . . ? C17 C18 C22 C21 -171.0(3) . . . . ? C20 C22 C19 C15 -174.0(3) . . . . ? C21 C22 C19 C15 60.8(4) . . . . ? C18 C22 C19 C15 -56.2(4) . . . . ? C20 C22 C19 C16 -62.6(4) . . . . ? C21 C22 C19 C16 172.2(3) . . . . ? C18 C22 C19 C16 55.2(4) . . . . ? C22 C19 C15 C14 35.3(4) . . . . ? C16 C19 C15 C14 -72.8(4) . . . . ? N3 C14 C15 C19 -176.6(4) . . . . ? C18 C14 C15 C19 1.5(4) . . . . ? C15 C19 C16 C17 70.9(4) . . . . ? C22 C19 C16 C17 -36.7(4) . . . . ? C18 C17 C16 C19 1.3(5) . . . . ? C13 N4 S4 O5 -62.0(3) . . . . ? Ni1 N4 S4 O5 174.60(17) . . . . ? C13 N4 S4 O7 68.7(3) . . . . ? Ni1 N4 S4 O7 -54.8(2) . . . . ? C13 N4 S4 C23 -177.7(3) . . . . ? Ni1 N4 S4 C23 58.8(2) . . . . ? C18 C23 S4 O5 -74.5(4) . . . . ? C18 C23 S4 O7 163.3(3) . . . . ? C18 C23 S4 N4 42.3(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.511 _refine_diff_density_min -0.240 _refine_diff_density_rms 0.061 data_081121am _database_code_depnum_ccdc_archive 'CCDC 753365' #TrackingRef 'nju04 SMC-Ni.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H38 N4 Ni O4 S2' _chemical_formula_sum 'C24 H38 N4 Ni O4 S2' _chemical_formula_weight 569.41 _chemical_absolute_configuration unknown 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.012(3) _cell_length_b 12.244(3) _cell_length_c 16.996(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2499.6(10) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1873 _cell_measurement_theta_min 1.95 _cell_measurement_theta_max 25.52 _exptl_crystal_description Prism _exptl_crystal_colour Green _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.513 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 0.983 _exptl_absorpt_correction_type Multi-scan' _exptl_absorpt_correction_T_min 0.8255 _exptl_absorpt_correction_T_max 0.8729 _exptl_absorpt_process_details '(SADABS; Bruker, 2002)' _diffrn_ambient_temperature 298(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_type 'Bruker smart apex II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13100 _diffrn_reflns_av_R_equivalents 0.0646 _diffrn_reflns_av_sigmaI/netI 0.1046 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 25.50 _reflns_number_total 4652 _reflns_number_gt 3430 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Bruker, 2002)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0013P)^2^] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.07(2) _refine_ls_number_reflns 4652 _refine_ls_number_parameters 320 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0832 _refine_ls_R_factor_gt 0.0598 _refine_ls_wR_factor_ref 0.0787 _refine_ls_wR_factor_gt 0.0740 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.10901(6) 0.59461(5) 0.74834(4) 0.03044(17) Uani 1 1 d . . . O1 O 0.2604(3) 0.5102(4) 0.96157(19) 0.0565(12) Uani 1 1 d . . . O2 O 0.3629(3) 0.6022(3) 0.85669(19) 0.0509(11) Uani 1 1 d . . . O3 O -0.2103(4) 0.4856(4) 0.8115(2) 0.0797(17) Uani 1 1 d . . . O4 O -0.0364(4) 0.3906(4) 0.8283(2) 0.0742(16) Uani 1 1 d . . . S1 S 0.26709(13) 0.54084(13) 0.87977(8) 0.0401(4) Uani 1 1 d . . . S2 S -0.09611(16) 0.47644(15) 0.78778(9) 0.0490(5) Uani 1 1 d . . . N1 N 0.2523(4) 0.5939(4) 0.7028(2) 0.0311(10) Uani 1 1 d . . . N2 N 0.0644(4) 0.6195(3) 0.6407(2) 0.0316(12) Uani 1 1 d . . . N3 N 0.1544(4) 0.6023(4) 0.8542(2) 0.0362(12) Uani 1 1 d . . . N4 N -0.0372(4) 0.5925(4) 0.7865(2) 0.0340(11) Uani 1 1 d . . . C1 C 0.4067(5) 0.4988(4) 0.6331(3) 0.0395(15) Uani 1 1 d . . . H1A H 0.4719 0.5438 0.6422 0.047 Uiso 1 1 calc R . . H1B H 0.3771 0.5141 0.5812 0.047 Uiso 1 1 calc R . . C2 C 0.3269(5) 0.3156(5) 0.6199(3) 0.0536(19) Uani 1 1 d . . . H2A H 0.3418 0.2380 0.6152 0.064 Uiso 1 1 calc R . . H2B H 0.2973 0.3422 0.5704 0.064 Uiso 1 1 calc R . . C3 C 0.4337(5) 0.3657(4) 0.7344(3) 0.0404(16) Uani 1 1 d . . . C4 C 0.5250(5) 0.4307(5) 0.7725(3) 0.0559(19) Uani 1 1 d . . . H4A H 0.5140 0.5069 0.7617 0.084 Uiso 1 1 calc R . . H4B H 0.5956 0.4080 0.7517 0.084 Uiso 1 1 calc R . . H4C H 0.5237 0.4188 0.8283 0.084 Uiso 1 1 calc R . . C5 C 0.4458(5) 0.2457(4) 0.7587(4) 0.0599(19) Uani 1 1 d . . . H5A H 0.5165 0.2184 0.7413 0.090 Uiso 1 1 calc R . . H5B H 0.3872 0.2035 0.7352 0.090 Uiso 1 1 calc R . . H5C H 0.4412 0.2399 0.8150 0.090 Uiso 1 1 calc R . . C6 C 0.2460(5) 0.3386(4) 0.6878(3) 0.0400(15) Uani 1 1 d . . . H6A H 0.2239 0.2716 0.7139 0.048 Uiso 1 1 calc R . . H6B H 0.1800 0.3764 0.6694 0.048 Uiso 1 1 calc R . . C7 C 0.3148(4) 0.4113(4) 0.7428(3) 0.0323(12) Uani 1 1 d . . . C8 C 0.3195(5) 0.5160(5) 0.6965(3) 0.0348(15) Uani 1 1 d . . . C9 C 0.2685(5) 0.4162(4) 0.8276(3) 0.0407(15) Uani 1 1 d . . . H9A H 0.3106 0.3643 0.8588 0.049 Uiso 1 1 calc R . . H9B H 0.1924 0.3897 0.8257 0.049 Uiso 1 1 calc R . . C10 C 0.2547(5) 0.6879(4) 0.6507(3) 0.0390(15) Uani 1 1 d . . . H10A H 0.3209 0.6861 0.6181 0.047 Uiso 1 1 calc R . . H10B H 0.2552 0.7550 0.6811 0.047 Uiso 1 1 calc R . . C11 C 0.1508(5) 0.6820(4) 0.5999(3) 0.0354(15) Uani 1 1 d . . . H11A H 0.1239 0.7552 0.5891 0.043 Uiso 1 1 calc R . . H11B H 0.1683 0.6473 0.5501 0.043 Uiso 1 1 calc R . . C12 C 0.0630(4) 0.5981(5) 0.9107(3) 0.0366(15) Uani 1 1 d . . . H12A H 0.0793 0.6425 0.9565 0.044 Uiso 1 1 calc R . . H12B H 0.0492 0.5236 0.9276 0.044 Uiso 1 1 calc R . . C13 C -0.0363(5) 0.6431(5) 0.8661(3) 0.0442(17) Uani 1 1 d . . . H13A H -0.1047 0.6258 0.8938 0.053 Uiso 1 1 calc R . . H13B H -0.0305 0.7219 0.8617 0.053 Uiso 1 1 calc R . . C14 C -0.0242(5) 0.5998(5) 0.6035(3) 0.0330(14) Uani 1 1 d . . . C15 C -0.0525(5) 0.6421(5) 0.5220(3) 0.0510(19) Uani 1 1 d . . . H15A H -0.0596 0.7210 0.5219 0.061 Uiso 1 1 calc R . . H15B H 0.0036 0.6208 0.4840 0.061 Uiso 1 1 calc R . . C16 C -0.2507(6) 0.6408(6) 0.5559(3) 0.068(2) Uani 1 1 d . . . H16A H -0.3248 0.6167 0.5412 0.081 Uiso 1 1 calc R . . H16B H -0.2472 0.7198 0.5525 0.081 Uiso 1 1 calc R . . C17 C -0.2188(5) 0.6000(5) 0.6400(3) 0.0511(18) Uani 1 1 d . . . H17A H -0.1985 0.6606 0.6738 0.061 Uiso 1 1 calc R . . H17B H -0.2798 0.5601 0.6639 0.061 Uiso 1 1 calc R . . C18 C -0.1192(5) 0.5253(5) 0.6253(3) 0.0371(14) Uani 1 1 d . . . C19 C -0.1626(6) 0.5878(6) 0.5047(3) 0.0568(19) Uani 1 1 d . . . H19 H -0.1817 0.5849 0.4487 0.068 Uiso 1 1 calc R . . C20 C -0.2490(5) 0.4036(6) 0.5428(3) 0.071(2) Uani 1 1 d . . . H20A H -0.2731 0.3918 0.4896 0.106 Uiso 1 1 calc R . . H20B H -0.3073 0.4390 0.5719 0.106 Uiso 1 1 calc R . . H20C H -0.2319 0.3347 0.5669 0.106 Uiso 1 1 calc R . . C21 C -0.0481(5) 0.4108(5) 0.5086(3) 0.0603(19) Uani 1 1 d . . . H21A H -0.0589 0.4016 0.4530 0.090 Uiso 1 1 calc R . . H21B H -0.0446 0.3405 0.5334 0.090 Uiso 1 1 calc R . . H21C H 0.0202 0.4495 0.5177 0.090 Uiso 1 1 calc R . . C22 C -0.1452(5) 0.4759(5) 0.5429(3) 0.0442(16) Uani 1 1 d . . . C23 C -0.0914(5) 0.4396(4) 0.6876(3) 0.0429(17) Uani 1 1 d . . . H23A H -0.0170 0.4127 0.6767 0.051 Uiso 1 1 calc R . . H23B H -0.1420 0.3787 0.6802 0.051 Uiso 1 1 calc R . . C24 C 0.4329(5) 0.3786(5) 0.6433(3) 0.0467(18) Uani 1 1 d . . . H24 H 0.5010 0.3541 0.6169 0.056 Uiso 1 1 calc R . . 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 Ni1 0.0354(4) 0.0351(4) 0.0208(3) 0.0026(4) -0.0006(4) 0.0005(4) O1 0.065(3) 0.083(3) 0.022(2) 0.005(2) -0.001(2) 0.020(3) O2 0.039(3) 0.069(3) 0.045(2) -0.014(2) -0.0062(19) -0.011(3) O3 0.053(3) 0.143(5) 0.043(3) -0.016(3) 0.014(2) -0.035(3) O4 0.109(4) 0.061(3) 0.053(3) 0.025(3) -0.029(3) -0.019(3) S1 0.0424(10) 0.0537(11) 0.0241(8) -0.0030(8) -0.0051(7) 0.0073(9) S2 0.0504(12) 0.0643(12) 0.0323(9) 0.0078(8) -0.0002(8) -0.0206(11) N1 0.032(3) 0.038(3) 0.023(2) 0.008(2) -0.002(2) -0.003(3) N2 0.045(3) 0.030(3) 0.020(2) -0.001(2) -0.002(2) 0.003(2) N3 0.047(3) 0.045(3) 0.017(2) -0.001(2) 0.000(2) 0.000(3) N4 0.038(3) 0.049(3) 0.015(2) -0.004(2) -0.0002(18) 0.005(3) C1 0.042(4) 0.047(4) 0.029(3) 0.002(3) 0.005(3) -0.003(3) C2 0.065(5) 0.058(5) 0.038(4) -0.002(4) -0.004(4) -0.004(4) C3 0.038(4) 0.041(4) 0.042(4) 0.000(3) 0.005(3) 0.002(3) C4 0.045(4) 0.068(5) 0.055(5) -0.003(4) -0.003(3) 0.009(4) C5 0.062(5) 0.060(4) 0.059(5) 0.006(4) 0.012(4) 0.021(3) C6 0.039(4) 0.036(4) 0.046(4) 0.003(3) 0.001(3) 0.002(3) C7 0.037(3) 0.033(3) 0.027(3) 0.010(3) 0.006(3) 0.002(3) C8 0.029(4) 0.046(4) 0.029(3) -0.009(3) -0.002(3) 0.009(3) C9 0.055(4) 0.030(3) 0.037(3) 0.010(3) -0.002(3) -0.001(4) C10 0.038(4) 0.038(4) 0.041(4) 0.001(3) 0.008(3) 0.001(3) C11 0.050(4) 0.036(4) 0.021(3) 0.004(3) 0.009(3) 0.001(3) C12 0.044(4) 0.045(4) 0.021(3) -0.007(3) -0.001(3) 0.001(3) C13 0.052(5) 0.050(4) 0.031(4) 0.002(3) 0.008(3) 0.006(4) C14 0.049(4) 0.030(4) 0.020(3) -0.004(3) -0.003(3) 0.003(3) C15 0.060(5) 0.063(5) 0.030(4) 0.011(3) -0.011(3) -0.005(4) C16 0.068(6) 0.094(6) 0.041(4) -0.006(4) -0.016(4) 0.030(5) C17 0.049(4) 0.073(5) 0.032(3) -0.009(4) -0.002(3) 0.020(4) C18 0.043(4) 0.044(4) 0.024(3) -0.007(3) 0.001(3) 0.004(3) C19 0.062(5) 0.078(5) 0.030(3) -0.003(4) -0.017(3) 0.010(5) C20 0.064(5) 0.102(6) 0.045(4) -0.025(4) -0.012(3) -0.013(5) C21 0.081(5) 0.058(4) 0.041(4) -0.015(4) -0.001(3) -0.005(5) C22 0.039(4) 0.062(4) 0.032(4) -0.008(3) -0.007(3) 0.000(4) C23 0.048(4) 0.040(4) 0.040(4) -0.003(3) 0.000(3) -0.013(3) C24 0.042(4) 0.060(5) 0.038(4) 0.001(3) 0.012(3) 0.015(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 Ni1 N4 1.872(4) . ? Ni1 N3 1.882(4) . ? Ni1 N1 1.887(4) . ? Ni1 N2 1.931(4) . ? O1 S1 1.442(3) . ? O2 S1 1.429(4) . ? O3 S2 1.434(4) . ? O4 S2 1.448(4) . ? S1 N3 1.608(5) . ? S1 C9 1.765(5) . ? S2 N4 1.587(5) . ? S2 C23 1.762(5) . ? N1 C8 1.253(6) . ? N1 C10 1.452(6) . ? N2 C14 1.261(6) . ? N2 C11 1.464(6) . ? N3 C12 1.460(6) . ? N4 C13 1.489(6) . ? C1 C8 1.517(7) . ? C1 C24 1.515(7) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C24 1.541(7) . ? C2 C6 1.535(7) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.502(7) . ? C3 C5 1.533(6) . ? C3 C7 1.540(7) . ? C3 C24 1.557(7) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.532(7) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.505(7) . ? C7 C9 1.546(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.520(7) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.517(7) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C18 1.506(7) . ? C14 C15 1.518(7) . ? C15 C19 1.509(8) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C19 1.515(8) . ? C16 C17 1.562(7) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.527(7) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C23 1.528(7) . ? C18 C22 1.557(7) . ? C19 C22 1.530(8) . ? C19 H19 0.9800 . ? C20 C22 1.530(8) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.528(8) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24 0.9800 . ? 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 N4 Ni1 N3 86.63(18) . . ? N4 Ni1 N1 175.92(18) . . ? N3 Ni1 N1 97.36(19) . . ? N4 Ni1 N2 94.06(19) . . ? N3 Ni1 N2 168.1(2) . . ? N1 Ni1 N2 82.23(18) . . ? O2 S1 O1 116.5(2) . . ? O2 S1 N3 110.9(2) . . ? O1 S1 N3 109.6(2) . . ? O2 S1 C9 108.0(3) . . ? O1 S1 C9 105.1(3) . . ? N3 S1 C9 106.1(3) . . ? O3 S2 O4 113.4(3) . . ? O3 S2 N4 111.1(3) . . ? O4 S2 N4 115.8(3) . . ? O3 S2 C23 108.8(3) . . ? O4 S2 C23 105.0(3) . . ? N4 S2 C23 101.6(2) . . ? C8 N1 C10 122.5(5) . . ? C8 N1 Ni1 128.8(4) . . ? C10 N1 Ni1 105.3(3) . . ? C14 N2 C11 117.5(5) . . ? C14 N2 Ni1 132.7(4) . . ? C11 N2 Ni1 109.6(3) . . ? C12 N3 S1 116.0(3) . . ? C12 N3 Ni1 114.1(3) . . ? S1 N3 Ni1 118.6(2) . . ? C13 N4 S2 111.3(3) . . ? C13 N4 Ni1 107.6(3) . . ? S2 N4 Ni1 115.8(3) . . ? C8 C1 C24 101.4(5) . . ? C8 C1 H1A 111.5 . . ? C24 C1 H1A 111.5 . . ? C8 C1 H1B 111.5 . . ? C24 C1 H1B 111.5 . . ? H1A C1 H1B 109.3 . . ? C24 C2 C6 103.7(4) . . ? C24 C2 H2A 111.0 . . ? C6 C2 H2A 111.0 . . ? C24 C2 H2B 111.0 . . ? C6 C2 H2B 111.0 . . ? H2A C2 H2B 109.0 . . ? C4 C3 C5 108.8(5) . . ? C4 C3 C7 116.4(5) . . ? C5 C3 C7 114.3(5) . . ? C4 C3 C24 112.3(5) . . ? C5 C3 C24 111.5(5) . . ? C7 C3 C24 92.8(4) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C2 C6 C7 102.9(5) . . ? C2 C6 H6A 111.2 . . ? C7 C6 H6A 111.2 . . ? C2 C6 H6B 111.2 . . ? C7 C6 H6B 111.2 . . ? H6A C6 H6B 109.1 . . ? C8 C7 C9 117.9(5) . . ? C8 C7 C3 103.1(4) . . ? C9 C7 C3 115.7(5) . . ? C8 C7 C6 101.3(4) . . ? C9 C7 C6 113.3(4) . . ? C3 C7 C6 103.5(4) . . ? N1 C8 C1 127.7(5) . . ? N1 C8 C7 125.4(5) . . ? C1 C8 C7 106.2(5) . . ? C7 C9 S1 120.4(4) . . ? C7 C9 H9A 107.2 . . ? S1 C9 H9A 107.2 . . ? C7 C9 H9B 107.2 . . ? S1 C9 H9B 107.2 . . ? H9A C9 H9B 106.9 . . ? N1 C10 C11 107.0(4) . . ? N1 C10 H10A 110.3 . . ? C11 C10 H10A 110.3 . . ? N1 C10 H10B 110.3 . . ? C11 C10 H10B 110.3 . . ? H10A C10 H10B 108.6 . . ? N2 C11 C10 109.7(4) . . ? N2 C11 H11A 109.7 . . ? C10 C11 H11A 109.7 . . ? N2 C11 H11B 109.7 . . ? C10 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? N3 C12 C13 104.5(4) . . ? N3 C12 H12A 110.9 . . ? C13 C12 H12A 110.9 . . ? N3 C12 H12B 110.9 . . ? C13 C12 H12B 110.9 . . ? H12A C12 H12B 108.9 . . ? N4 C13 C12 107.9(4) . . ? N4 C13 H13A 110.1 . . ? C12 C13 H13A 110.1 . . ? N4 C13 H13B 110.1 . . ? C12 C13 H13B 110.1 . . ? H13A C13 H13B 108.4 . . ? N2 C14 C18 129.2(5) . . ? N2 C14 C15 125.5(6) . . ? C18 C14 C15 105.1(5) . . ? C19 C15 C14 102.9(5) . . ? C19 C15 H15A 111.2 . . ? C14 C15 H15A 111.2 . . ? C19 C15 H15B 111.2 . . ? C14 C15 H15B 111.2 . . ? H15A C15 H15B 109.1 . . ? C19 C16 C17 102.5(5) . . ? C19 C16 H16A 111.3 . . ? C17 C16 H16A 111.3 . . ? C19 C16 H16B 111.3 . . ? C17 C16 H16B 111.3 . . ? H16A C16 H16B 109.2 . . ? C18 C17 C16 103.5(4) . . ? C18 C17 H17A 111.1 . . ? C16 C17 H17A 111.1 . . ? C18 C17 H17B 111.1 . . ? C16 C17 H17B 111.1 . . ? H17A C17 H17B 109.0 . . ? C14 C18 C23 114.9(5) . . ? C14 C18 C17 105.7(5) . . ? C23 C18 C17 118.0(5) . . ? C14 C18 C22 99.6(4) . . ? C23 C18 C22 113.6(5) . . ? C17 C18 C22 102.9(5) . . ? C15 C19 C16 108.2(5) . . ? C15 C19 C22 101.1(5) . . ? C16 C19 C22 103.6(5) . . ? C15 C19 H19 114.2 . . ? C16 C19 H19 114.2 . . ? C22 C19 H19 114.2 . . ? C22 C20 H20A 109.5 . . ? C22 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C22 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C21 C22 C20 108.7(5) . . ? C21 C22 C19 114.2(5) . . ? C20 C22 C19 114.0(5) . . ? C21 C22 C18 113.1(5) . . ? C20 C22 C18 112.9(5) . . ? C19 C22 C18 93.5(4) . . ? C18 C23 S2 119.1(4) . . ? C18 C23 H23A 107.5 . . ? S2 C23 H23A 107.5 . . ? C18 C23 H23B 107.5 . . ? S2 C23 H23B 107.5 . . ? H23A C23 H23B 107.0 . . ? C1 C24 C2 106.6(5) . . ? C1 C24 C3 102.3(4) . . ? C2 C24 C3 102.2(5) . . ? C1 C24 H24 114.8 . . ? C2 C24 H24 114.8 . . ? C3 C24 H24 114.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Ni1 N1 C8 -89(3) . . . . ? N3 Ni1 N1 C8 79.0(5) . . . . ? N2 Ni1 N1 C8 -113.0(5) . . . . ? N4 Ni1 N1 C10 71(3) . . . . ? N3 Ni1 N1 C10 -121.7(3) . . . . ? N2 Ni1 N1 C10 46.2(3) . . . . ? N4 Ni1 N2 C14 -24.1(6) . . . . ? N3 Ni1 N2 C14 -116.9(10) . . . . ? N1 Ni1 N2 C14 154.3(6) . . . . ? N4 Ni1 N2 C11 149.8(3) . . . . ? N3 Ni1 N2 C11 56.9(12) . . . . ? N1 Ni1 N2 C11 -31.9(3) . . . . ? O2 S1 N3 C12 -140.6(4) . . . . ? O1 S1 N3 C12 -10.5(5) . . . . ? C9 S1 N3 C12 102.4(4) . . . . ? O2 S1 N3 Ni1 77.7(3) . . . . ? O1 S1 N3 Ni1 -152.2(3) . . . . ? C9 S1 N3 Ni1 -39.3(3) . . . . ? N4 Ni1 N3 C12 2.5(4) . . . . ? N1 Ni1 N3 C12 -176.6(4) . . . . ? N2 Ni1 N3 C12 96.2(11) . . . . ? N4 Ni1 N3 S1 144.9(3) . . . . ? N1 Ni1 N3 S1 -34.2(3) . . . . ? N2 Ni1 N3 S1 -121.4(10) . . . . ? O3 S2 N4 C13 61.7(4) . . . . ? O4 S2 N4 C13 -69.6(4) . . . . ? C23 S2 N4 C13 177.3(4) . . . . ? O3 S2 N4 Ni1 -175.0(2) . . . . ? O4 S2 N4 Ni1 53.7(3) . . . . ? C23 S2 N4 Ni1 -59.4(3) . . . . ? N3 Ni1 N4 C13 23.3(3) . . . . ? N1 Ni1 N4 C13 -169(3) . . . . ? N2 Ni1 N4 C13 -144.7(3) . . . . ? N3 Ni1 N4 S2 -102.0(3) . . . . ? N1 Ni1 N4 S2 66(3) . . . . ? N2 Ni1 N4 S2 90.0(3) . . . . ? C24 C2 C6 C7 -0.4(6) . . . . ? C4 C3 C7 C8 66.1(6) . . . . ? C5 C3 C7 C8 -165.7(5) . . . . ? C24 C3 C7 C8 -50.6(5) . . . . ? C4 C3 C7 C9 -64.1(6) . . . . ? C5 C3 C7 C9 64.1(7) . . . . ? C24 C3 C7 C9 179.2(5) . . . . ? C4 C3 C7 C6 171.3(5) . . . . ? C5 C3 C7 C6 -60.5(6) . . . . ? C24 C3 C7 C6 54.6(5) . . . . ? C2 C6 C7 C8 71.4(5) . . . . ? C2 C6 C7 C9 -161.3(5) . . . . ? C2 C6 C7 C3 -35.1(5) . . . . ? C10 N1 C8 C1 -5.2(9) . . . . ? Ni1 N1 C8 C1 150.8(4) . . . . ? C10 N1 C8 C7 -173.5(5) . . . . ? Ni1 N1 C8 C7 -17.5(8) . . . . ? C24 C1 C8 N1 -162.9(6) . . . . ? C24 C1 C8 C7 7.2(6) . . . . ? C9 C7 C8 N1 -31.9(8) . . . . ? C3 C7 C8 N1 -160.8(5) . . . . ? C6 C7 C8 N1 92.4(6) . . . . ? C9 C7 C8 C1 157.7(5) . . . . ? C3 C7 C8 C1 28.8(5) . . . . ? C6 C7 C8 C1 -78.0(5) . . . . ? C8 C7 C9 S1 -21.5(7) . . . . ? C3 C7 C9 S1 101.1(5) . . . . ? C6 C7 C9 S1 -139.6(4) . . . . ? O2 S1 C9 C7 -33.9(5) . . . . ? O1 S1 C9 C7 -158.8(4) . . . . ? N3 S1 C9 C7 85.1(5) . . . . ? C8 N1 C10 C11 110.9(6) . . . . ? Ni1 N1 C10 C11 -50.0(5) . . . . ? C14 N2 C11 C10 -174.6(5) . . . . ? Ni1 N2 C11 C10 10.5(5) . . . . ? N1 C10 C11 N2 24.9(6) . . . . ? S1 N3 C12 C13 -170.1(4) . . . . ? Ni1 N3 C12 C13 -26.7(6) . . . . ? S2 N4 C13 C12 83.9(5) . . . . ? Ni1 N4 C13 C12 -44.0(5) . . . . ? N3 C12 C13 N4 44.7(6) . . . . ? C11 N2 C14 C18 170.3(5) . . . . ? Ni1 N2 C14 C18 -16.2(10) . . . . ? C11 N2 C14 C15 -4.4(9) . . . . ? Ni1 N2 C14 C15 169.0(4) . . . . ? N2 C14 C15 C19 176.2(6) . . . . ? C18 C14 C15 C19 0.4(6) . . . . ? C19 C16 C17 C18 -2.2(7) . . . . ? N2 C14 C18 C23 -18.6(9) . . . . ? C15 C14 C18 C23 157.0(5) . . . . ? N2 C14 C18 C17 113.3(7) . . . . ? C15 C14 C18 C17 -71.1(5) . . . . ? N2 C14 C18 C22 -140.3(6) . . . . ? C15 C14 C18 C22 35.3(6) . . . . ? C16 C17 C18 C14 71.6(6) . . . . ? C16 C17 C18 C23 -158.3(5) . . . . ? C16 C17 C18 C22 -32.4(6) . . . . ? C14 C15 C19 C16 71.7(6) . . . . ? C14 C15 C19 C22 -36.8(6) . . . . ? C17 C16 C19 C15 -69.8(6) . . . . ? C17 C16 C19 C22 36.9(6) . . . . ? C15 C19 C22 C21 -60.3(6) . . . . ? C16 C19 C22 C21 -172.3(5) . . . . ? C15 C19 C22 C20 174.0(5) . . . . ? C16 C19 C22 C20 62.0(6) . . . . ? C15 C19 C22 C18 57.0(5) . . . . ? C16 C19 C22 C18 -55.0(6) . . . . ? C14 C18 C22 C21 62.4(6) . . . . ? C23 C18 C22 C21 -60.3(7) . . . . ? C17 C18 C22 C21 171.0(5) . . . . ? C14 C18 C22 C20 -173.7(5) . . . . ? C23 C18 C22 C20 63.6(7) . . . . ? C17 C18 C22 C20 -65.0(6) . . . . ? C14 C18 C22 C19 -55.8(5) . . . . ? C23 C18 C22 C19 -178.5(5) . . . . ? C17 C18 C22 C19 52.8(6) . . . . ? C14 C18 C23 S2 82.8(6) . . . . ? C17 C18 C23 S2 -42.9(7) . . . . ? C22 C18 C23 S2 -163.4(4) . . . . ? O3 S2 C23 C18 74.3(6) . . . . ? O4 S2 C23 C18 -164.1(5) . . . . ? N4 S2 C23 C18 -43.1(5) . . . . ? C8 C1 C24 C2 66.5(5) . . . . ? C8 C1 C24 C3 -40.4(5) . . . . ? C6 C2 C24 C1 -71.7(6) . . . . ? C6 C2 C24 C3 35.2(6) . . . . ? C4 C3 C24 C1 -64.1(6) . . . . ? C5 C3 C24 C1 173.5(5) . . . . ? C7 C3 C24 C1 56.0(5) . . . . ? C4 C3 C24 C2 -174.3(5) . . . . ? C5 C3 C24 C2 63.3(6) . . . . ? C7 C3 C24 C2 -54.2(5) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.926 _refine_diff_density_min -0.591 _refine_diff_density_rms 0.078