# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Michael Wolf' _publ_contact_author_email mwolf@chem.ubc.ca loop_ _publ_author_name 'Lyndsey Earl' 'Brian Patrick' 'Michael Wolf' data_1 _database_code_depnum_ccdc_archive 'CCDC 876807' #TrackingRef '- CE-ART--04-2012-025529cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H59 N5 O11 S4 Zn2' _chemical_formula_weight 1249.07 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' 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' Zn Zn 0.2839 1.4301 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.3642(6) _cell_length_b 17.0748(6) _cell_length_c 20.6230(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.226(2) _cell_angle_gamma 90.00 _cell_volume 5762.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 35342 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 30.09 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.440 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2592 _exptl_absorpt_coefficient_mu 1.041 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7855 _exptl_absorpt_correction_T_max 0.9011 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 99492 _diffrn_reflns_av_R_equivalents 0.0538 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 30.13 _reflns_number_total 16899 _reflns_number_gt 12937 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2\s(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^)+(0.0430P)^2^+16.0711P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16899 _refine_ls_number_parameters 770 _refine_ls_number_restraints 1050 _refine_ls_R_factor_all 0.0733 _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.1425 _refine_ls_wR_factor_gt 0.1326 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.029 _refine_ls_shift/su_mean 0.001 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 0.67614(16) 0.07425(16) 0.58698(13) 0.0154(5) Uani 1 1 d U . . C2 C 0.64726(16) 0.11542(15) 0.64618(13) 0.0156(5) Uani 1 1 d U . . C3 C 0.60309(17) 0.08603(17) 0.69645(14) 0.0188(5) Uani 1 1 d U . . H3 H 0.5850 0.0344 0.6982 0.023 Uiso 1 1 calc R . . C4 C 0.58722(17) 0.14199(17) 0.74623(14) 0.0194(5) Uani 1 1 d U . . C5 C 0.62089(17) 0.21417(17) 0.73148(14) 0.0181(5) Uani 1 1 d U . . C6 C 0.62085(17) 0.28647(17) 0.77020(14) 0.0187(5) Uani 1 1 d U . . C7 C 0.58583(18) 0.35818(17) 0.75613(14) 0.0196(5) Uani 1 1 d U . . C8 C 0.60259(17) 0.41419(16) 0.80531(14) 0.0185(5) Uani 1 1 d U . . H8 H 0.5837 0.4655 0.8038 0.022 Uiso 1 1 calc R . . C9 C 0.64909(17) 0.38549(16) 0.85492(13) 0.0161(5) Uani 1 1 d U . . C10 C 0.68134(17) 0.42743(16) 0.91272(13) 0.0157(5) Uani 1 1 d U . . C11 C 0.53877(19) 0.12355(19) 0.80453(15) 0.0245(6) Uani 1 1 d U . . C12 C 0.5490(3) 0.0528(2) 0.83652(18) 0.0367(9) Uani 1 1 d U . . H12 H 0.5881 0.0174 0.8223 0.044 Uiso 1 1 calc R . . C13 C 0.5005(3) 0.0346(3) 0.8902(2) 0.0490(11) Uani 1 1 d U . . H13 H 0.5073 -0.0129 0.9116 0.059 Uiso 1 1 calc R . . C14 C 0.4424(3) 0.0876(3) 0.9113(2) 0.0513(12) Uani 1 1 d U . . H14 H 0.4100 0.0754 0.9469 0.062 Uiso 1 1 calc R . . C15 C 0.4320(2) 0.1579(3) 0.8801(2) 0.0439(10) Uani 1 1 d U . . H15 H 0.3929 0.1932 0.8946 0.053 Uiso 1 1 calc R . . C16 C 0.4798(2) 0.1765(2) 0.82714(18) 0.0344(8) Uani 1 1 d U . . H16 H 0.4727 0.2243 0.8063 0.041 Uiso 1 1 calc R . . C17 C 0.5354(2) 0.37648(19) 0.69848(16) 0.0258(6) Uani 1 1 d U . . C18 C 0.5412(2) 0.4493(2) 0.66900(17) 0.0340(8) Uani 1 1 d U . . H18 H 0.5785 0.4858 0.6847 0.041 Uiso 1 1 calc R . . C19 C 0.4923(3) 0.4682(2) 0.6166(2) 0.0434(10) Uani 1 1 d U . . H19 H 0.4968 0.5174 0.5975 0.052 Uiso 1 1 calc R . . C20 C 0.4369(3) 0.4147(3) 0.5924(2) 0.0443(10) Uani 1 1 d U . . H20 H 0.4043 0.4275 0.5569 0.053 Uiso 1 1 calc R . . C21 C 0.4302(3) 0.3424(2) 0.62098(19) 0.0406(9) Uani 1 1 d U . . H21 H 0.3928 0.3062 0.6049 0.049 Uiso 1 1 calc R . . C22 C 0.4785(2) 0.3233(2) 0.67333(18) 0.0317(7) Uani 1 1 d U . . H22 H 0.4733 0.2742 0.6923 0.038 Uiso 1 1 calc R . . C29 C 0.82310(18) -0.07885(16) 0.40960(13) 0.0175(5) Uani 1 1 d U . . C30 C 0.86762(18) -0.12364(16) 0.35917(14) 0.0185(5) Uani 1 1 d U . . C31 C 0.94086(17) -0.10683(17) 0.33155(14) 0.0186(5) Uani 1 1 d U . . H31 H 0.9726 -0.0640 0.3436 0.022 Uiso 1 1 calc R . . C32 C 0.96430(17) -0.16079(17) 0.28259(14) 0.0186(5) Uani 1 1 d U . . C33 C 0.90703(18) -0.21957(17) 0.27557(14) 0.0197(5) Uani 1 1 d U . . C34 C 1.04059(19) -0.15242(17) 0.24416(14) 0.0205(6) Uani 1 1 d U . . C35 C 1.11157(19) -0.12478(19) 0.27346(16) 0.0250(6) Uani 1 1 d U . . H35 H 1.1120 -0.1139 0.3176 0.030 Uiso 1 1 calc R . . C36 C 1.1819(2) -0.1133(2) 0.23731(18) 0.0316(7) Uani 1 1 d U . . H36 H 1.2289 -0.0939 0.2571 0.038 Uiso 1 1 calc R . . C37 C 1.1819(2) -0.1308(2) 0.17201(19) 0.0357(8) Uani 1 1 d U . . H37 H 1.2291 -0.1236 0.1478 0.043 Uiso 1 1 calc R . . C38 C 1.1119(2) -0.1589(2) 0.14239(17) 0.0324(7) Uani 1 1 d U . . H38 H 1.1123 -0.1708 0.0984 0.039 Uiso 1 1 calc R . . C39 C 1.0413(2) -0.16935(19) 0.17799(16) 0.0266(6) Uani 1 1 d U . . H39 H 0.9941 -0.1877 0.1578 0.032 Uiso 1 1 calc R . . C40 C 0.67133(17) 0.07482(16) 0.40623(13) 0.0164(5) Uani 1 1 d U . . C41 C 0.62899(17) 0.11824(16) 0.35398(13) 0.0171(5) Uani 1 1 d U . . C42 C 0.55564(18) 0.10200(17) 0.32527(14) 0.0190(5) Uani 1 1 d U . . H42 H 0.5231 0.0599 0.3374 0.023 Uiso 1 1 calc R . . C43 C 0.53335(18) 0.15535(17) 0.27503(14) 0.0201(6) Uani 1 1 d U . . C44 C 0.59243(17) 0.21267(17) 0.26759(14) 0.0187(5) Uani 1 1 d U . . C45 C 0.45795(18) 0.14797(17) 0.23611(15) 0.0210(6) Uani 1 1 d U . . C46 C 0.38459(19) 0.12528(19) 0.26491(17) 0.0255(6) Uani 1 1 d U . . H46 H 0.3827 0.1169 0.3094 0.031 Uiso 1 1 calc R . . C47 C 0.3143(2) 0.1150(2) 0.22761(19) 0.0332(8) Uani 1 1 d U . . H47 H 0.2659 0.0991 0.2472 0.040 Uiso 1 1 calc R . . C48 C 0.3162(2) 0.1285(2) 0.1615(2) 0.0359(8) Uani 1 1 d U . . H48 H 0.2692 0.1216 0.1367 0.043 Uiso 1 1 calc R . . C49 C 0.3879(2) 0.1521(2) 0.13238(18) 0.0345(8) Uani 1 1 d U . . H49 H 0.3891 0.1617 0.0880 0.041 Uiso 1 1 calc R . . C50 C 0.4577(2) 0.1614(2) 0.16924(16) 0.0282(7) Uani 1 1 d U . . H50 H 0.5058 0.1769 0.1491 0.034 Uiso 1 1 calc R . . C52 C 0.5381(2) -0.1478(2) 0.5426(2) 0.0404(9) Uani 1 1 d U . . H52A H 0.5698 -0.1522 0.5817 0.061 Uiso 1 1 calc R . . H52B H 0.5031 -0.1926 0.5384 0.061 Uiso 1 1 calc R . . H52C H 0.5055 -0.1011 0.5443 0.061 Uiso 1 1 calc R . . C51 C 0.5468(2) -0.1372(2) 0.42606(19) 0.0354(8) Uani 1 1 d U . . H51A H 0.5840 -0.1348 0.3902 0.053 Uiso 1 1 calc R . . H51B H 0.5142 -0.0905 0.4270 0.053 Uiso 1 1 calc R . . H51C H 0.5119 -0.1820 0.4213 0.053 Uiso 1 1 calc R . . C53 C 0.9487(3) 0.1345(2) 0.4262(2) 0.0430(10) Uani 1 1 d U . . H53A H 0.9138 0.1264 0.3892 0.065 Uiso 1 1 calc R . . H53B H 0.9839 0.0900 0.4316 0.065 Uiso 1 1 calc R . . H53C H 0.9811 0.1806 0.4196 0.065 Uiso 1 1 calc R . . C54 C 0.9488(3) 0.1569(3) 0.5418(2) 0.0662(17) Uani 1 1 d U . . H54A H 0.9139 0.1632 0.5787 0.099 Uiso 1 1 calc R . . H54B H 0.9812 0.2033 0.5362 0.099 Uiso 1 1 calc R . . H54C H 0.9840 0.1127 0.5484 0.099 Uiso 1 1 calc R . . O1 O 0.74977(12) -0.09693(12) 0.41881(10) 0.0186(4) Uani 1 1 d U . . O2 O 0.86358(12) -0.02670(12) 0.43855(10) 0.0194(4) Uani 1 1 d U . . O3 O 0.64866(13) 0.00684(12) 0.57622(10) 0.0189(4) Uani 1 1 d U . . O4 O 0.72760(13) 0.11093(12) 0.55278(10) 0.0189(4) Uani 1 1 d U . . O5 O 0.63066(12) 0.02387(12) 0.43599(10) 0.0180(4) Uani 1 1 d U . . O6 O 0.74504(12) 0.09298(12) 0.41657(10) 0.0199(4) Uani 1 1 d U . . O7 O 0.65405(13) 0.49537(11) 0.92313(9) 0.0182(4) Uani 1 1 d U . . O8 O 0.73357(13) 0.39132(12) 0.94603(10) 0.0185(4) Uani 1 1 d U . . S1 S 0.67437(4) 0.28891(4) 0.84221(3) 0.01861(14) Uani 1 1 d U . . S2 S 0.67196(5) 0.21202(4) 0.65869(3) 0.01914(14) Uani 1 1 d U . . S3 S 0.67354(4) 0.19965(4) 0.32029(4) 0.02073(14) Uani 1 1 d U . . S4 S 0.82510(4) -0.20685(4) 0.32696(4) 0.02134(15) Uani 1 1 d U . . Zn1 Zn 0.678963(19) -0.058875(18) 0.495615(14) 0.01343(7) Uani 1 1 d U . . Zn2 Zn 0.814390(19) 0.058729(18) 0.495281(14) 0.01369(7) Uani 1 1 d U . . N1 N 0.59316(15) -0.14380(15) 0.48651(12) 0.0187(5) Uani 1 1 d U . . N2 N 0.89890(16) 0.14418(15) 0.48393(13) 0.0198(5) Uani 1 1 d U . . H2N H 0.878(2) 0.183(2) 0.4813(18) 0.021(10) Uiso 1 1 d . . . H1N H 0.621(3) -0.188(3) 0.486(2) 0.042(12) Uiso 1 1 d . . . C55 C 0.7281(3) 0.2903(2) 0.49108(19) 0.0389(9) Uani 1 1 d DU . . H56 H 0.7085 0.2523 0.5193 0.047 Uiso 1 1 calc R . . C56 C 0.5922(3) 0.3467(4) 0.4925(3) 0.0671(15) Uani 1 1 d DU . . H56A H 0.5858 0.3107 0.5279 0.101 Uiso 1 1 calc R . . H56B H 0.5549 0.3331 0.4583 0.101 Uiso 1 1 calc R . . H56C H 0.5809 0.3989 0.5071 0.101 Uiso 1 1 calc R . . C57 C 0.6942(3) 0.3937(3) 0.4117(3) 0.0650(15) Uani 1 1 d DU . . H57A H 0.7482 0.3814 0.3968 0.098 Uiso 1 1 calc R . . H57B H 0.6921 0.4478 0.4244 0.098 Uiso 1 1 calc R . . H57C H 0.6555 0.3845 0.3775 0.098 Uiso 1 1 calc R . . O9 O 0.8005(2) 0.28725(18) 0.47802(18) 0.0587(10) Uani 1 1 d DU . . N3 N 0.6736(2) 0.3426(2) 0.4691(2) 0.0531(10) Uani 1 1 d DU . . C58 C 0.7529(2) -0.2849(2) 0.49449(17) 0.0313(7) Uani 1 1 d DU . . H58 H 0.7719 -0.2346 0.4862 0.038 Uiso 1 1 calc R . . C60 C 0.8941(3) -0.3242(3) 0.4934(3) 0.0650(15) Uani 1 1 d DU . . H60A H 0.9149 -0.3547 0.4580 0.098 Uiso 1 1 calc R . . H60B H 0.9227 -0.3378 0.5325 0.098 Uiso 1 1 calc R . . H60C H 0.9018 -0.2695 0.4844 0.098 Uiso 1 1 calc R . . C59 C 0.7849(3) -0.4210(2) 0.5127(2) 0.0466(10) Uani 1 1 d DU . . H59A H 0.7275 -0.4237 0.5218 0.070 Uiso 1 1 calc R . . H59B H 0.8152 -0.4411 0.5490 0.070 Uiso 1 1 calc R . . H59C H 0.7968 -0.4517 0.4749 0.070 Uiso 1 1 calc R . . O18 O 0.67813(16) -0.29350(15) 0.49807(13) 0.0351(6) Uani 1 1 d DU . . N4 N 0.80801(19) -0.3400(2) 0.50126(17) 0.0394(7) Uani 1 1 d DU . . C61 C 0.7785(7) -0.4164(7) 0.3262(5) 0.053(3) Uani 0.476(14) 1 d PDU A 1 H61 H 0.7428 -0.3754 0.3348 0.064 Uiso 0.476(14) 1 calc PR A 1 C62 C 0.6823(11) -0.4582(11) 0.2449(9) 0.061(5) Uani 0.476(14) 1 d PDU A 1 H62A H 0.6763 -0.5009 0.2150 0.092 Uiso 0.476(14) 1 calc PR A 1 H62B H 0.6846 -0.4098 0.2214 0.092 Uiso 0.476(14) 1 calc PR A 1 H62C H 0.6365 -0.4574 0.2738 0.092 Uiso 0.476(14) 1 calc PR A 1 C63 C 0.8061(10) -0.5348(6) 0.2622(7) 0.066(4) Uani 0.476(14) 1 d PDU A 1 H63A H 0.7787 -0.5649 0.2293 0.099 Uiso 0.476(14) 1 calc PR A 1 H63B H 0.8158 -0.5673 0.2995 0.099 Uiso 0.476(14) 1 calc PR A 1 H63C H 0.8572 -0.5161 0.2458 0.099 Uiso 0.476(14) 1 calc PR A 1 O19 O 0.8431(6) -0.4178(9) 0.3580(7) 0.067(3) Uani 0.476(14) 1 d PDU A 1 N5 N 0.7547(9) -0.4680(8) 0.2808(7) 0.063(4) Uani 0.476(14) 1 d PDU A 1 C61B C 0.8290(8) -0.4522(6) 0.3181(4) 0.059(3) Uani 0.524(14) 1 d PDU A 2 H61B H 0.8836 -0.4663 0.3234 0.071 Uiso 0.524(14) 1 calc PR A 2 C62B C 0.8206(7) -0.5564(7) 0.2382(5) 0.051(3) Uani 0.524(14) 1 d PDU A 2 H62D H 0.7802 -0.5779 0.2094 0.077 Uiso 0.524(14) 1 calc PR A 2 H62E H 0.8390 -0.5962 0.2677 0.077 Uiso 0.524(14) 1 calc PR A 2 H62F H 0.8661 -0.5375 0.2135 0.077 Uiso 0.524(14) 1 calc PR A 2 C63B C 0.6988(9) -0.4775(15) 0.2630(10) 0.098(8) Uani 0.524(14) 1 d PDU A 2 H63D H 0.6778 -0.5127 0.2306 0.147 Uiso 0.524(14) 1 calc PR A 2 H63E H 0.6920 -0.4245 0.2485 0.147 Uiso 0.524(14) 1 calc PR A 2 H63F H 0.6695 -0.4850 0.3028 0.147 Uiso 0.524(14) 1 calc PR A 2 O19B O 0.8042(9) -0.3973(7) 0.3529(7) 0.086(4) Uani 0.524(14) 1 d PDU A 2 N5B N 0.7860(7) -0.4935(8) 0.2738(5) 0.057(4) Uani 0.524(14) 1 d PDU A 2 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 0.0162(12) 0.0159(12) 0.0141(11) -0.0016(9) -0.0018(9) 0.0042(9) C2 0.0158(12) 0.0121(12) 0.0188(12) -0.0046(9) -0.0014(10) 0.0006(9) C3 0.0176(12) 0.0159(13) 0.0228(13) -0.0046(10) 0.0011(11) -0.0008(10) C4 0.0177(12) 0.0200(13) 0.0205(13) -0.0057(11) 0.0050(10) -0.0002(10) C5 0.0197(13) 0.0167(13) 0.0180(12) -0.0046(10) 0.0002(10) 0.0017(10) C6 0.0194(13) 0.0151(12) 0.0217(13) -0.0055(10) 0.0011(11) 0.0003(10) C7 0.0201(13) 0.0175(13) 0.0211(13) -0.0065(10) -0.0012(11) 0.0009(10) C8 0.0195(13) 0.0134(12) 0.0225(13) -0.0048(10) -0.0016(11) 0.0010(10) C9 0.0170(12) 0.0133(12) 0.0179(12) -0.0035(10) 0.0016(10) -0.0008(9) C10 0.0173(12) 0.0152(12) 0.0145(11) -0.0020(9) 0.0011(10) -0.0026(9) C11 0.0243(14) 0.0246(15) 0.0247(14) -0.0105(12) 0.0110(12) -0.0075(12) C12 0.052(2) 0.0257(17) 0.0320(17) -0.0082(14) 0.0194(17) -0.0093(15) C13 0.073(3) 0.032(2) 0.042(2) -0.0058(17) 0.029(2) -0.017(2) C14 0.059(3) 0.053(3) 0.043(2) -0.023(2) 0.031(2) -0.028(2) C15 0.0354(19) 0.047(2) 0.049(2) -0.0268(19) 0.0234(18) -0.0123(17) C16 0.0309(17) 0.0342(19) 0.0382(19) -0.0172(15) 0.0136(15) -0.0055(14) C17 0.0289(15) 0.0228(15) 0.0256(15) -0.0104(12) -0.0074(12) 0.0083(12) C18 0.046(2) 0.0251(17) 0.0307(17) -0.0050(13) -0.0157(16) 0.0040(15) C19 0.060(3) 0.0317(19) 0.038(2) -0.0023(16) -0.0184(19) 0.0107(18) C20 0.049(2) 0.047(2) 0.038(2) -0.0136(17) -0.0223(18) 0.0215(19) C21 0.042(2) 0.039(2) 0.040(2) -0.0187(17) -0.0193(17) 0.0088(17) C22 0.0290(16) 0.0312(18) 0.0349(18) -0.0123(14) -0.0103(14) 0.0050(13) C29 0.0242(13) 0.0147(12) 0.0136(11) -0.0017(9) -0.0010(10) 0.0042(10) C30 0.0224(13) 0.0146(12) 0.0184(12) -0.0052(10) -0.0003(11) 0.0020(10) C31 0.0202(13) 0.0159(13) 0.0197(13) -0.0040(10) 0.0004(11) 0.0008(10) C32 0.0196(13) 0.0177(13) 0.0185(13) -0.0032(10) 0.0015(10) 0.0016(10) C33 0.0201(13) 0.0185(13) 0.0204(13) -0.0071(10) 0.0030(11) 0.0022(10) C34 0.0247(14) 0.0148(13) 0.0221(13) -0.0030(10) 0.0045(11) 0.0017(11) C35 0.0233(14) 0.0239(15) 0.0279(15) 0.0036(12) 0.0023(12) 0.0037(12) C36 0.0205(15) 0.0331(18) 0.0414(19) 0.0071(15) 0.0008(14) 0.0036(13) C37 0.0293(17) 0.0333(19) 0.045(2) 0.0051(16) 0.0155(16) 0.0070(14) C38 0.0380(19) 0.0312(18) 0.0282(16) -0.0029(13) 0.0147(14) 0.0046(14) C39 0.0305(16) 0.0219(15) 0.0274(15) -0.0056(12) 0.0060(13) -0.0017(12) C40 0.0201(12) 0.0140(12) 0.0152(12) 0.0001(9) 0.0022(10) 0.0044(10) C41 0.0198(13) 0.0143(12) 0.0174(12) 0.0053(10) 0.0013(10) 0.0008(10) C42 0.0221(13) 0.0153(12) 0.0196(13) 0.0050(10) 0.0034(11) 0.0002(10) C43 0.0223(13) 0.0171(13) 0.0211(13) 0.0066(10) 0.0001(11) 0.0014(10) C44 0.0185(12) 0.0194(13) 0.0184(12) 0.0072(10) 0.0025(10) 0.0017(10) C45 0.0216(13) 0.0161(13) 0.0252(14) 0.0031(11) -0.0012(11) 0.0012(10) C46 0.0244(15) 0.0223(15) 0.0297(16) -0.0011(12) 0.0011(12) 0.0019(12) C47 0.0205(15) 0.0339(18) 0.045(2) -0.0046(16) 0.0010(14) 0.0036(13) C48 0.0279(17) 0.0344(19) 0.045(2) -0.0040(16) -0.0150(16) 0.0064(14) C49 0.041(2) 0.0342(19) 0.0277(17) 0.0064(14) -0.0124(15) 0.0033(15) C50 0.0314(17) 0.0257(16) 0.0273(16) 0.0088(13) -0.0007(13) -0.0013(13) C52 0.040(2) 0.038(2) 0.043(2) -0.0067(17) 0.0172(17) -0.0129(17) C51 0.042(2) 0.0245(17) 0.0397(19) 0.0011(14) -0.0204(16) -0.0070(14) C53 0.047(2) 0.0273(18) 0.055(2) -0.0022(17) 0.032(2) -0.0078(16) C54 0.074(3) 0.078(4) 0.046(3) 0.016(2) -0.026(2) -0.054(3) O1 0.0166(9) 0.0223(10) 0.0170(9) -0.0044(8) 0.0019(7) 0.0018(8) O2 0.0217(10) 0.0166(9) 0.0197(10) -0.0059(8) 0.0023(8) 0.0015(8) O3 0.0258(10) 0.0135(9) 0.0173(9) -0.0042(7) 0.0015(8) 0.0008(8) O4 0.0232(10) 0.0145(9) 0.0189(9) 0.0001(7) 0.0039(8) 0.0016(8) O5 0.0191(9) 0.0158(9) 0.0191(9) 0.0049(7) 0.0028(8) 0.0025(7) O6 0.0195(9) 0.0231(10) 0.0171(9) 0.0048(8) 0.0002(8) 0.0011(8) O7 0.0253(10) 0.0127(9) 0.0166(9) -0.0024(7) 0.0005(8) 0.0000(8) O8 0.0235(10) 0.0147(9) 0.0173(9) 0.0000(7) -0.0036(8) -0.0018(8) S1 0.0248(3) 0.0127(3) 0.0184(3) -0.0025(2) -0.0008(3) 0.0014(2) S2 0.0258(3) 0.0131(3) 0.0185(3) -0.0030(2) 0.0016(3) -0.0009(3) S3 0.0189(3) 0.0212(3) 0.0221(3) 0.0081(3) -0.0006(3) -0.0024(3) S4 0.0200(3) 0.0205(3) 0.0236(3) -0.0091(3) 0.0034(3) -0.0017(3) Zn1 0.01691(15) 0.01041(14) 0.01296(14) -0.00030(11) 0.00026(11) 0.00028(11) Zn2 0.01722(15) 0.01079(14) 0.01308(14) 0.00002(11) 0.00064(11) -0.00009(11) N1 0.0195(11) 0.0158(11) 0.0208(11) -0.0018(9) 0.0013(9) -0.0004(9) N2 0.0210(12) 0.0153(12) 0.0232(12) 0.0022(9) 0.0018(10) -0.0015(10) C55 0.049(2) 0.034(2) 0.0335(19) 0.0089(15) 0.0053(17) -0.0045(17) C56 0.041(2) 0.097(5) 0.064(3) 0.011(3) 0.006(2) -0.005(3) C57 0.060(3) 0.042(3) 0.093(4) 0.021(3) 0.011(3) 0.004(2) O9 0.0542(19) 0.0365(16) 0.086(2) 0.0224(16) 0.0372(18) 0.0146(14) N3 0.045(2) 0.0333(18) 0.081(3) -0.0014(18) 0.024(2) 0.0036(15) C58 0.044(2) 0.0221(16) 0.0280(16) -0.0011(12) 0.0002(15) -0.0054(14) C60 0.034(2) 0.071(4) 0.091(4) 0.002(3) 0.005(2) -0.006(2) C59 0.054(3) 0.037(2) 0.049(2) 0.0004(18) -0.001(2) 0.0088(19) O18 0.0376(14) 0.0302(13) 0.0374(14) 0.0002(11) -0.0070(11) 0.0034(11) N4 0.0325(16) 0.0351(17) 0.050(2) -0.0011(15) -0.0065(15) 0.0006(13) C61 0.058(7) 0.057(7) 0.044(6) -0.009(5) 0.002(5) 0.007(6) C62 0.070(9) 0.059(7) 0.055(11) -0.033(7) 0.023(7) -0.026(6) C63 0.144(13) 0.016(5) 0.038(7) -0.008(4) -0.014(7) -0.010(7) O19 0.068(7) 0.076(8) 0.057(6) -0.023(5) 0.002(5) 0.003(5) N5 0.099(11) 0.050(7) 0.040(5) -0.007(5) 0.015(7) -0.025(7) C61B 0.091(8) 0.051(6) 0.036(5) 0.002(4) -0.004(5) -0.028(6) C62B 0.069(7) 0.041(6) 0.044(6) -0.009(4) -0.019(5) -0.020(5) C63B 0.066(10) 0.18(2) 0.050(10) -0.055(12) 0.020(7) -0.069(11) O19B 0.117(12) 0.081(9) 0.060(7) -0.015(6) 0.012(9) -0.029(8) N5B 0.080(8) 0.060(9) 0.030(5) 0.003(5) -0.009(6) -0.042(7) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O3 1.255(3) . ? C1 O4 1.266(3) . ? C1 C2 1.487(4) . ? C2 C3 1.362(4) . ? C2 S2 1.717(3) . ? C3 C4 1.427(4) . ? C3 H3 0.9300 . ? C4 C5 1.384(4) . ? C4 C11 1.477(4) . ? C5 C6 1.470(4) . ? C5 S2 1.721(3) . ? C6 C7 1.382(4) . ? C6 S1 1.722(3) . ? C7 C8 1.420(4) . ? C7 C17 1.478(4) . ? C8 C9 1.364(4) . ? C8 H8 0.9300 . ? C9 C10 1.486(4) . ? C9 S1 1.721(3) . ? C10 O8 1.256(3) . ? C10 O7 1.262(3) . ? C11 C12 1.386(5) . ? C11 C16 1.403(5) . ? C12 C13 1.400(5) . ? C12 H12 0.9300 . ? C13 C14 1.384(6) . ? C13 H13 0.9300 . ? C14 C15 1.373(7) . ? C14 H14 0.9300 . ? C15 C16 1.382(5) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C18 1.388(5) . ? C17 C22 1.398(5) . ? C18 C19 1.381(5) . ? C18 H18 0.9300 . ? C19 C20 1.380(6) . ? C19 H19 0.9300 . ? C20 C21 1.372(6) . ? C20 H20 0.9300 . ? C21 C22 1.375(5) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C29 O1 1.254(4) . ? C29 O2 1.259(3) . ? C29 C30 1.484(4) . ? C30 C31 1.360(4) . ? C30 S4 1.715(3) . ? C31 C32 1.421(4) . ? C31 H31 0.9300 . ? C32 C33 1.380(4) . ? C32 C34 1.488(4) . ? C33 C44 1.460(4) 2_645 ? C33 S4 1.726(3) . ? C34 C35 1.390(4) . ? C34 C39 1.395(4) . ? C35 C36 1.387(4) . ? C35 H35 0.9300 . ? C36 C37 1.379(5) . ? C36 H36 0.9300 . ? C37 C38 1.382(6) . ? C37 H37 0.9300 . ? C38 C39 1.384(5) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 O5 1.257(3) . ? C40 O6 1.263(3) . ? C40 C41 1.478(4) . ? C41 C42 1.365(4) . ? C41 S3 1.718(3) . ? C42 C43 1.426(4) . ? C42 H42 0.9300 . ? C43 C44 1.385(4) . ? C43 C45 1.475(4) . ? C44 C33 1.460(4) 2_655 ? C44 S3 1.727(3) . ? C45 C46 1.396(4) . ? C45 C50 1.398(4) . ? C46 C47 1.393(5) . ? C46 H46 0.9300 . ? C47 C48 1.383(5) . ? C47 H47 0.9300 . ? C48 C49 1.380(6) . ? C48 H48 0.9300 . ? C49 C50 1.379(5) . ? C49 H49 0.9300 . ? C50 H50 0.9300 . ? C52 N1 1.470(4) . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C51 N1 1.461(4) . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C53 N2 1.455(4) . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 N2 1.459(5) . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? O1 Zn1 2.071(2) . ? O2 Zn2 2.038(2) . ? O3 Zn1 2.068(2) . ? O4 Zn2 2.057(2) . ? O5 Zn1 2.031(2) . ? O6 Zn2 2.062(2) . ? O7 Zn2 2.064(2) 2_656 ? O8 Zn1 2.051(2) 2_656 ? Zn1 N1 2.027(3) . ? Zn1 O8 2.051(2) 2_646 ? Zn1 Zn2 2.9906(8) . ? Zn2 N2 2.025(3) . ? Zn2 O7 2.064(2) 2_646 ? N1 H1N 0.88(5) . ? N2 H2N 0.74(4) . ? C55 O9 1.216(5) . ? C55 N3 1.340(5) . ? C55 H56 0.9300 . ? C56 N3 1.421(5) . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 N3 1.510(6) . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? C58 O18 1.235(4) . ? C58 N4 1.310(5) . ? C58 H58 0.9300 . ? C60 N4 1.444(5) . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? C59 N4 1.453(5) . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C61 O19 1.243(11) . ? C61 N5 1.341(11) . ? C61 H61 0.9300 . ? C62 N5 1.404(13) . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C63 N5 1.470(12) . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C61B O19B 1.248(12) . ? C61B N5B 1.351(10) . ? C61B H61B 0.9300 . ? C62B N5B 1.419(11) . ? C62B H62D 0.9600 . ? C62B H62E 0.9600 . ? C62B H62F 0.9600 . ? C63B N5B 1.469(13) . ? C63B H63D 0.9600 . ? C63B H63E 0.9600 . ? C63B H63F 0.9600 . ? 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 O3 C1 O4 126.4(3) . . ? O3 C1 C2 117.6(2) . . ? O4 C1 C2 115.9(2) . . ? C3 C2 C1 128.5(3) . . ? C3 C2 S2 111.4(2) . . ? C1 C2 S2 120.1(2) . . ? C2 C3 C4 113.5(3) . . ? C2 C3 H3 123.2 . . ? C4 C3 H3 123.2 . . ? C5 C4 C3 111.4(3) . . ? C5 C4 C11 125.7(3) . . ? C3 C4 C11 122.9(3) . . ? C4 C5 C6 128.8(3) . . ? C4 C5 S2 111.6(2) . . ? C6 C5 S2 119.5(2) . . ? C7 C6 C5 129.1(3) . . ? C7 C6 S1 111.6(2) . . ? C5 C6 S1 119.2(2) . . ? C6 C7 C8 111.6(3) . . ? C6 C7 C17 125.9(3) . . ? C8 C7 C17 122.5(3) . . ? C9 C8 C7 113.6(3) . . ? C9 C8 H8 123.2 . . ? C7 C8 H8 123.2 . . ? C8 C9 C10 128.6(3) . . ? C8 C9 S1 111.3(2) . . ? C10 C9 S1 120.0(2) . . ? O8 C10 O7 126.8(3) . . ? O8 C10 C9 116.2(2) . . ? O7 C10 C9 117.0(2) . . ? C12 C11 C16 119.0(3) . . ? C12 C11 C4 120.6(3) . . ? C16 C11 C4 120.4(3) . . ? C11 C12 C13 120.2(4) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C14 C13 C12 119.7(4) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C15 C14 C13 120.5(4) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 120.1(4) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C15 C16 C11 120.4(4) . . ? C15 C16 H16 119.8 . . ? C11 C16 H16 119.8 . . ? C18 C17 C22 117.8(3) . . ? C18 C17 C7 120.2(3) . . ? C22 C17 C7 122.0(3) . . ? C19 C18 C17 120.8(4) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C20 C19 C18 120.4(4) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C21 C20 C19 119.6(4) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C20 C21 C22 120.2(4) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C21 C22 C17 121.2(4) . . ? C21 C22 H22 119.4 . . ? C17 C22 H22 119.4 . . ? O1 C29 O2 127.2(3) . . ? O1 C29 C30 116.9(2) . . ? O2 C29 C30 116.0(3) . . ? C31 C30 C29 128.4(3) . . ? C31 C30 S4 111.7(2) . . ? C29 C30 S4 119.9(2) . . ? C30 C31 C32 113.7(3) . . ? C30 C31 H31 123.2 . . ? C32 C31 H31 123.2 . . ? C33 C32 C31 111.2(3) . . ? C33 C32 C34 125.8(3) . . ? C31 C32 C34 123.1(3) . . ? C32 C33 C44 129.4(3) . 2_645 ? C32 C33 S4 111.9(2) . . ? C44 C33 S4 118.7(2) 2_645 . ? C35 C34 C39 119.1(3) . . ? C35 C34 C32 120.2(3) . . ? C39 C34 C32 120.7(3) . . ? C36 C35 C34 120.5(3) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C37 C36 C35 119.8(3) . . ? C37 C36 H36 120.1 . . ? C35 C36 H36 120.1 . . ? C36 C37 C38 120.2(3) . . ? C36 C37 H37 119.9 . . ? C38 C37 H37 119.9 . . ? C37 C38 C39 120.2(3) . . ? C37 C38 H38 119.9 . . ? C39 C38 H38 119.9 . . ? C38 C39 C34 120.2(3) . . ? C38 C39 H39 119.9 . . ? C34 C39 H39 119.9 . . ? O5 C40 O6 126.5(3) . . ? O5 C40 C41 117.1(3) . . ? O6 C40 C41 116.4(2) . . ? C42 C41 C40 128.6(3) . . ? C42 C41 S3 111.3(2) . . ? C40 C41 S3 120.2(2) . . ? C41 C42 C43 114.0(3) . . ? C41 C42 H42 123.0 . . ? C43 C42 H42 123.0 . . ? C44 C43 C42 110.8(3) . . ? C44 C43 C45 125.7(3) . . ? C42 C43 C45 123.5(3) . . ? C43 C44 C33 129.3(3) . 2_655 ? C43 C44 S3 112.0(2) . . ? C33 C44 S3 118.6(2) 2_655 . ? C46 C45 C50 117.8(3) . . ? C46 C45 C43 120.7(3) . . ? C50 C45 C43 121.5(3) . . ? C47 C46 C45 120.6(3) . . ? C47 C46 H46 119.7 . . ? C45 C46 H46 119.7 . . ? C48 C47 C46 120.1(3) . . ? C48 C47 H47 120.0 . . ? C46 C47 H47 120.0 . . ? C49 C48 C47 120.1(3) . . ? C49 C48 H48 120.0 . . ? C47 C48 H48 120.0 . . ? C50 C49 C48 119.8(3) . . ? C50 C49 H49 120.1 . . ? C48 C49 H49 120.1 . . ? C49 C50 C45 121.6(3) . . ? C49 C50 H50 119.2 . . ? C45 C50 H50 119.2 . . ? N1 C52 H52A 109.5 . . ? N1 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? N1 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N1 C51 H51A 109.5 . . ? N1 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? N1 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? N2 C53 H53A 109.5 . . ? N2 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? N2 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N2 C54 H54A 109.5 . . ? N2 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? N2 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C29 O1 Zn1 125.24(18) . . ? C29 O2 Zn2 124.77(19) . . ? C1 O3 Zn1 123.57(18) . . ? C1 O4 Zn2 124.68(18) . . ? C40 O5 Zn1 124.86(18) . . ? C40 O6 Zn2 125.86(18) . . ? C10 O7 Zn2 122.20(18) . 2_656 ? C10 O8 Zn1 126.09(18) . 2_656 ? C9 S1 C6 91.88(14) . . ? C2 S2 C5 92.11(14) . . ? C41 S3 C44 91.85(14) . . ? C30 S4 C33 91.56(14) . . ? N1 Zn1 O5 100.01(10) . . ? N1 Zn1 O8 103.84(9) . 2_646 ? O5 Zn1 O8 155.88(8) . 2_646 ? N1 Zn1 O3 107.13(9) . . ? O5 Zn1 O3 90.88(8) . . ? O8 Zn1 O3 85.54(8) 2_646 . ? N1 Zn1 O1 95.40(9) . . ? O5 Zn1 O1 88.44(8) . . ? O8 Zn1 O1 85.84(8) 2_646 . ? O3 Zn1 O1 157.22(8) . . ? N1 Zn1 Zn2 173.38(7) . . ? O5 Zn1 Zn2 79.52(6) . . ? O8 Zn1 Zn2 76.37(6) 2_646 . ? O3 Zn1 Zn2 79.49(6) . . ? O1 Zn1 Zn2 78.00(6) . . ? N2 Zn2 O2 100.25(10) . . ? N2 Zn2 O4 103.17(10) . . ? O2 Zn2 O4 156.41(8) . . ? N2 Zn2 O6 94.51(10) . . ? O2 Zn2 O6 88.19(9) . . ? O4 Zn2 O6 87.24(8) . . ? N2 Zn2 O7 107.64(10) . 2_646 ? O2 Zn2 O7 89.70(8) . 2_646 ? O4 Zn2 O7 85.89(8) . 2_646 ? O6 Zn2 O7 157.76(8) . 2_646 ? N2 Zn2 Zn1 172.19(8) . . ? O2 Zn2 Zn1 79.34(6) . . ? O4 Zn2 Zn1 77.07(6) . . ? O6 Zn2 Zn1 77.68(6) . . ? O7 Zn2 Zn1 80.17(6) 2_646 . ? C51 N1 C52 110.9(3) . . ? C51 N1 Zn1 112.4(2) . . ? C52 N1 Zn1 112.8(2) . . ? C51 N1 H1N 108(3) . . ? C52 N1 H1N 107(3) . . ? Zn1 N1 H1N 105(3) . . ? C53 N2 C54 111.9(3) . . ? C53 N2 Zn2 113.4(2) . . ? C54 N2 Zn2 113.1(2) . . ? C53 N2 H2N 107(3) . . ? C54 N2 H2N 100(3) . . ? Zn2 N2 H2N 110(3) . . ? O9 C55 N3 126.9(4) . . ? O9 C55 H56 116.5 . . ? N3 C55 H56 116.5 . . ? N3 C56 H56A 109.5 . . ? N3 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? N3 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N3 C57 H57A 109.5 . . ? N3 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? N3 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C55 N3 C56 122.8(4) . . ? C55 N3 C57 120.0(4) . . ? C56 N3 C57 116.8(4) . . ? O18 C58 N4 126.2(3) . . ? O18 C58 H58 116.9 . . ? N4 C58 H58 116.9 . . ? N4 C60 H60A 109.5 . . ? N4 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? N4 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? N4 C59 H59A 109.5 . . ? N4 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? N4 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C58 N4 C60 121.7(4) . . ? C58 N4 C59 121.4(3) . . ? C60 N4 C59 116.8(4) . . ? O19 C61 N5 126.9(12) . . ? O19 C61 H61 116.6 . . ? N5 C61 H61 116.6 . . ? N5 C62 H62A 109.5 . . ? N5 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? N5 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? N5 C63 H63A 109.5 . . ? N5 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? N5 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 N5 C62 122.1(12) . . ? C61 N5 C63 121.8(12) . . ? C62 N5 C63 115.9(11) . . ? O19B C61B N5B 127.6(13) . . ? O19B C61B H61B 116.2 . . ? N5B C61B H61B 116.2 . . ? N5B C62B H62D 109.5 . . ? N5B C62B H62E 109.5 . . ? H62D C62B H62E 109.5 . . ? N5B C62B H62F 109.5 . . ? H62D C62B H62F 109.5 . . ? H62E C62B H62F 109.5 . . ? N5B C63B H63D 109.5 . . ? N5B C63B H63E 109.5 . . ? H63D C63B H63E 109.5 . . ? N5B C63B H63F 109.5 . . ? H63D C63B H63F 109.5 . . ? H63E C63B H63F 109.5 . . ? C61B N5B C62B 122.4(10) . . ? C61B N5B C63B 120.6(12) . . ? C62B N5B C63B 116.9(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 O3 C1 C2 C3 10.3(4) . . . . ? O4 C1 C2 C3 -168.6(3) . . . . ? O3 C1 C2 S2 -171.8(2) . . . . ? O4 C1 C2 S2 9.3(3) . . . . ? C1 C2 C3 C4 178.9(3) . . . . ? S2 C2 C3 C4 0.8(3) . . . . ? C2 C3 C4 C5 0.1(4) . . . . ? C2 C3 C4 C11 178.5(3) . . . . ? C3 C4 C5 C6 -178.0(3) . . . . ? C11 C4 C5 C6 3.6(5) . . . . ? C3 C4 C5 S2 -0.9(3) . . . . ? C11 C4 C5 S2 -179.3(3) . . . . ? C4 C5 C6 C7 -117.0(4) . . . . ? S2 C5 C6 C7 66.2(4) . . . . ? C4 C5 C6 S1 66.4(4) . . . . ? S2 C5 C6 S1 -110.5(2) . . . . ? C5 C6 C7 C8 -177.6(3) . . . . ? S1 C6 C7 C8 -0.8(3) . . . . ? C5 C6 C7 C17 3.7(5) . . . . ? S1 C6 C7 C17 -179.5(3) . . . . ? C6 C7 C8 C9 0.2(4) . . . . ? C17 C7 C8 C9 179.0(3) . . . . ? C7 C8 C9 C10 177.1(3) . . . . ? C7 C8 C9 S1 0.5(3) . . . . ? C8 C9 C10 O8 -168.8(3) . . . . ? S1 C9 C10 O8 7.6(3) . . . . ? C8 C9 C10 O7 10.9(4) . . . . ? S1 C9 C10 O7 -172.8(2) . . . . ? C5 C4 C11 C12 -140.1(4) . . . . ? C3 C4 C11 C12 41.7(5) . . . . ? C5 C4 C11 C16 42.0(5) . . . . ? C3 C4 C11 C16 -136.2(3) . . . . ? C16 C11 C12 C13 0.5(6) . . . . ? C4 C11 C12 C13 -177.5(4) . . . . ? C11 C12 C13 C14 -0.1(7) . . . . ? C12 C13 C14 C15 -0.2(7) . . . . ? C13 C14 C15 C16 0.1(7) . . . . ? C14 C15 C16 C11 0.4(6) . . . . ? C12 C11 C16 C15 -0.6(5) . . . . ? C4 C11 C16 C15 177.3(3) . . . . ? C6 C7 C17 C18 -143.4(3) . . . . ? C8 C7 C17 C18 38.0(5) . . . . ? C6 C7 C17 C22 39.1(5) . . . . ? C8 C7 C17 C22 -139.5(3) . . . . ? C22 C17 C18 C19 0.0(6) . . . . ? C7 C17 C18 C19 -177.6(3) . . . . ? C17 C18 C19 C20 -0.3(6) . . . . ? C18 C19 C20 C21 0.4(7) . . . . ? C19 C20 C21 C22 -0.2(6) . . . . ? C20 C21 C22 C17 -0.1(6) . . . . ? C18 C17 C22 C21 0.2(5) . . . . ? C7 C17 C22 C21 177.8(3) . . . . ? O1 C29 C30 C31 166.6(3) . . . . ? O2 C29 C30 C31 -13.5(4) . . . . ? O1 C29 C30 S4 -11.5(4) . . . . ? O2 C29 C30 S4 168.4(2) . . . . ? C29 C30 C31 C32 -177.5(3) . . . . ? S4 C30 C31 C32 0.7(3) . . . . ? C30 C31 C32 C33 -1.4(4) . . . . ? C30 C31 C32 C34 177.7(3) . . . . ? C31 C32 C33 C44 -178.4(3) . . . 2_645 ? C34 C32 C33 C44 2.4(5) . . . 2_645 ? C31 C32 C33 S4 1.4(3) . . . . ? C34 C32 C33 S4 -177.7(2) . . . . ? C33 C32 C34 C35 -143.6(3) . . . . ? C31 C32 C34 C35 37.4(4) . . . . ? C33 C32 C34 C39 38.7(5) . . . . ? C31 C32 C34 C39 -140.3(3) . . . . ? C39 C34 C35 C36 0.8(5) . . . . ? C32 C34 C35 C36 -176.9(3) . . . . ? C34 C35 C36 C37 -1.2(5) . . . . ? C35 C36 C37 C38 0.6(5) . . . . ? C36 C37 C38 C39 0.3(6) . . . . ? C37 C38 C39 C34 -0.7(5) . . . . ? C35 C34 C39 C38 0.2(5) . . . . ? C32 C34 C39 C38 177.9(3) . . . . ? O5 C40 C41 C42 -12.6(4) . . . . ? O6 C40 C41 C42 167.5(3) . . . . ? O5 C40 C41 S3 168.9(2) . . . . ? O6 C40 C41 S3 -11.0(4) . . . . ? C40 C41 C42 C43 -178.7(3) . . . . ? S3 C41 C42 C43 -0.1(3) . . . . ? C41 C42 C43 C44 -0.6(4) . . . . ? C41 C42 C43 C45 178.2(3) . . . . ? C42 C43 C44 C33 -176.9(3) . . . 2_655 ? C45 C43 C44 C33 4.4(5) . . . 2_655 ? C42 C43 C44 S3 1.0(3) . . . . ? C45 C43 C44 S3 -177.8(2) . . . . ? C44 C43 C45 C46 -141.6(3) . . . . ? C42 C43 C45 C46 39.8(4) . . . . ? C44 C43 C45 C50 40.1(5) . . . . ? C42 C43 C45 C50 -138.5(3) . . . . ? C50 C45 C46 C47 1.2(5) . . . . ? C43 C45 C46 C47 -177.2(3) . . . . ? C45 C46 C47 C48 -1.0(5) . . . . ? C46 C47 C48 C49 0.0(6) . . . . ? C47 C48 C49 C50 0.8(6) . . . . ? C48 C49 C50 C45 -0.5(6) . . . . ? C46 C45 C50 C49 -0.5(5) . . . . ? C43 C45 C50 C49 177.9(3) . . . . ? O2 C29 O1 Zn1 -11.2(4) . . . . ? C30 C29 O1 Zn1 168.74(18) . . . . ? O1 C29 O2 Zn2 -13.8(4) . . . . ? C30 C29 O2 Zn2 166.31(18) . . . . ? O4 C1 O3 Zn1 -2.8(4) . . . . ? C2 C1 O3 Zn1 178.46(17) . . . . ? O3 C1 O4 Zn2 -27.1(4) . . . . ? C2 C1 O4 Zn2 151.74(19) . . . . ? O6 C40 O5 Zn1 -13.8(4) . . . . ? C41 C40 O5 Zn1 166.41(18) . . . . ? O5 C40 O6 Zn2 -11.5(4) . . . . ? C41 C40 O6 Zn2 168.27(18) . . . . ? O8 C10 O7 Zn2 -5.0(4) . . . 2_656 ? C9 C10 O7 Zn2 175.38(17) . . . 2_656 ? O7 C10 O8 Zn1 -24.9(4) . . . 2_656 ? C9 C10 O8 Zn1 154.71(18) . . . 2_656 ? C8 C9 S1 C6 -0.8(2) . . . . ? C10 C9 S1 C6 -177.8(2) . . . . ? C7 C6 S1 C9 0.9(2) . . . . ? C5 C6 S1 C9 178.1(2) . . . . ? C3 C2 S2 C5 -1.1(2) . . . . ? C1 C2 S2 C5 -179.4(2) . . . . ? C4 C5 S2 C2 1.2(2) . . . . ? C6 C5 S2 C2 178.5(2) . . . . ? C42 C41 S3 C44 0.5(2) . . . . ? C40 C41 S3 C44 179.3(2) . . . . ? C43 C44 S3 C41 -0.9(2) . . . . ? C33 C44 S3 C41 177.2(2) 2_655 . . . ? C31 C30 S4 C33 0.1(2) . . . . ? C29 C30 S4 C33 178.5(2) . . . . ? C32 C33 S4 C30 -0.9(2) . . . . ? C44 C33 S4 C30 179.0(3) 2_645 . . . ? C40 O5 Zn1 N1 -152.8(2) . . . . ? C40 O5 Zn1 O8 18.6(3) . . . 2_646 ? C40 O5 Zn1 O3 99.6(2) . . . . ? C40 O5 Zn1 O1 -57.6(2) . . . . ? C40 O5 Zn1 Zn2 20.5(2) . . . . ? C1 O3 Zn1 N1 -162.0(2) . . . . ? C1 O3 Zn1 O5 -61.2(2) . . . . ? C1 O3 Zn1 O8 94.9(2) . . . 2_646 ? C1 O3 Zn1 O1 26.8(4) . . . . ? C1 O3 Zn1 Zn2 18.0(2) . . . . ? C29 O1 Zn1 N1 -161.4(2) . . . . ? C29 O1 Zn1 O5 98.7(2) . . . . ? C29 O1 Zn1 O8 -57.9(2) . . . 2_646 ? C29 O1 Zn1 O3 10.1(4) . . . . ? C29 O1 Zn1 Zn2 19.1(2) . . . . ? C29 O2 Zn2 N2 -151.7(2) . . . . ? C29 O2 Zn2 O4 21.4(4) . . . . ? C29 O2 Zn2 O6 -57.5(2) . . . . ? C29 O2 Zn2 O7 100.4(2) . . . 2_646 ? C29 O2 Zn2 Zn1 20.3(2) . . . . ? C1 O4 Zn2 N2 -158.9(2) . . . . ? C1 O4 Zn2 O2 28.0(3) . . . . ? C1 O4 Zn2 O6 107.1(2) . . . . ? C1 O4 Zn2 O7 -51.8(2) . . . 2_646 ? C1 O4 Zn2 Zn1 29.1(2) . . . . ? C40 O6 Zn2 N2 -161.0(2) . . . . ? C40 O6 Zn2 O2 98.9(2) . . . . ? C40 O6 Zn2 O4 -58.0(2) . . . . ? C40 O6 Zn2 O7 14.1(4) . . . 2_646 ? C40 O6 Zn2 Zn1 19.4(2) . . . . ? N1 Zn1 Zn2 N2 68.0(9) . . . . ? O5 Zn1 Zn2 N2 -18.5(6) . . . . ? O8 Zn1 Zn2 N2 160.7(6) 2_646 . . . ? O3 Zn1 Zn2 N2 -111.4(6) . . . . ? O1 Zn1 Zn2 N2 72.1(6) . . . . ? N1 Zn1 Zn2 O2 -19.7(7) . . . . ? O5 Zn1 Zn2 O2 -106.25(9) . . . . ? O8 Zn1 Zn2 O2 72.96(9) 2_646 . . . ? O3 Zn1 Zn2 O2 160.88(8) . . . . ? O1 Zn1 Zn2 O2 -15.62(8) . . . . ? N1 Zn1 Zn2 O4 160.7(7) . . . . ? O5 Zn1 Zn2 O4 74.19(8) . . . . ? O8 Zn1 Zn2 O4 -106.60(8) 2_646 . . . ? O3 Zn1 Zn2 O4 -18.68(8) . . . . ? O1 Zn1 Zn2 O4 164.82(8) . . . . ? N1 Zn1 Zn2 O6 70.8(7) . . . . ? O5 Zn1 Zn2 O6 -15.78(8) . . . . ? O8 Zn1 Zn2 O6 163.43(8) 2_646 . . . ? O3 Zn1 Zn2 O6 -108.65(9) . . . . ? O1 Zn1 Zn2 O6 74.85(9) . . . . ? N1 Zn1 Zn2 O7 -111.3(7) . . . 2_646 ? O5 Zn1 Zn2 O7 162.20(8) . . . 2_646 ? O8 Zn1 Zn2 O7 -18.60(8) 2_646 . . 2_646 ? O3 Zn1 Zn2 O7 69.32(8) . . . 2_646 ? O1 Zn1 Zn2 O7 -107.17(8) . . . 2_646 ? O5 Zn1 N1 C51 23.4(2) . . . . ? O8 Zn1 N1 C51 -153.0(2) 2_646 . . . ? O3 Zn1 N1 C51 117.4(2) . . . . ? O1 Zn1 N1 C51 -66.0(2) . . . . ? Zn2 Zn1 N1 C51 -62.0(7) . . . . ? O5 Zn1 N1 C52 -102.9(2) . . . . ? O8 Zn1 N1 C52 80.7(3) 2_646 . . . ? O3 Zn1 N1 C52 -8.9(3) . . . . ? O1 Zn1 N1 C52 167.7(2) . . . . ? Zn2 Zn1 N1 C52 171.7(6) . . . . ? O2 Zn2 N2 C53 20.5(3) . . . . ? O4 Zn2 N2 C53 -156.7(3) . . . . ? O6 Zn2 N2 C53 -68.5(3) . . . . ? O7 Zn2 N2 C53 113.5(3) 2_646 . . . ? Zn1 Zn2 N2 C53 -65.8(7) . . . . ? O2 Zn2 N2 C54 -108.4(3) . . . . ? O4 Zn2 N2 C54 74.4(3) . . . . ? O6 Zn2 N2 C54 162.6(3) . . . . ? O7 Zn2 N2 C54 -15.4(3) 2_646 . . . ? Zn1 Zn2 N2 C54 165.3(5) . . . . ? O9 C55 N3 C56 -173.0(5) . . . . ? O9 C55 N3 C57 14.7(8) . . . . ? O18 C58 N4 C60 177.3(4) . . . . ? O18 C58 N4 C59 1.5(6) . . . . ? O19 C61 N5 C62 -176.1(18) . . . . ? O19 C61 N5 C63 -1(3) . . . . ? O19B C61B N5B C62B -178.4(13) . . . . ? O19B C61B N5B C63B -2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 30.13 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.229 _refine_diff_density_min -0.707 _refine_diff_density_rms 0.100 #The value of b is very close to 90; however, the structure could #not be solved in an orthorhombic space group (e.g. Pnna). data_2 _database_code_depnum_ccdc_archive 'CCDC 876808' #TrackingRef '- CE-ART--04-2012-025529cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H35 N O4 S2 Zn' _chemical_formula_weight 531.02 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' 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' Zn Zn 0.2839 1.4301 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.503(3) _cell_length_b 18.281(6) _cell_length_c 19.375(6) _cell_angle_alpha 90.00 _cell_angle_beta 100.470(15) _cell_angle_gamma 90.00 _cell_volume 2613.3(16) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.409 _cell_measurement_theta_max 18.74 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.350 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 1.128 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6763 _exptl_absorpt_correction_T_max 0.9777 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11499 _diffrn_reflns_av_R_equivalents 0.1591 _diffrn_reflns_av_sigmaI/netI 0.2073 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 22.61 _reflns_number_total 3392 _reflns_number_gt 1687 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2\s(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^)+(0.0759P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3392 _refine_ls_number_parameters 293 _refine_ls_number_restraints 210 _refine_ls_R_factor_all 0.1697 _refine_ls_R_factor_gt 0.0638 _refine_ls_wR_factor_ref 0.1788 _refine_ls_wR_factor_gt 0.1349 _refine_ls_goodness_of_fit_ref 0.952 _refine_ls_restrained_S_all 0.925 _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 0.0675(12) 0.0509(5) 0.8842(5) 0.020(2) Uani 1 1 d U . . C2 C 0.0782(12) 0.0918(5) 0.8197(5) 0.023(2) Uani 1 1 d U . . C3 C 0.1681(12) 0.0781(5) 0.7683(5) 0.025(3) Uani 1 1 d U . . H3 H 0.2429 0.0361 0.7687 0.030 Uiso 1 1 calc R . . C4 C 0.1467(12) 0.1296(5) 0.7125(5) 0.022(2) Uani 1 1 d U . . C5 C 0.0344(12) 0.1871(5) 0.7283(5) 0.022(2) Uani 1 1 d U . . C6 C -0.0090(12) 0.2554(5) 0.6878(4) 0.019(2) Uani 1 1 d U . . C7 C 0.1109(12) 0.3099(5) 0.6794(5) 0.023(2) Uani 1 1 d U . . C8 C 0.0196(13) 0.3676(5) 0.6385(5) 0.028(3) Uani 1 1 d U . . H8 H 0.0811 0.4103 0.6276 0.034 Uiso 1 1 calc R . . C9 C -0.1595(12) 0.3581(5) 0.6162(5) 0.020(2) Uani 1 1 d U . . C10 C -0.2934(14) 0.4058(5) 0.5709(5) 0.024(2) Uani 1 1 d U . . C11 C 0.2239(12) 0.1231(5) 0.6472(5) 0.022(2) Uani 1 1 d U . . H11A H 0.3574 0.1196 0.6601 0.026 Uiso 1 1 calc R . . H11B H 0.1951 0.1682 0.6191 0.026 Uiso 1 1 calc R . . C12 C 0.1540(13) 0.0576(5) 0.6020(5) 0.034(3) Uani 1 1 d U . . H12A H 0.1907 0.0122 0.6287 0.041 Uiso 1 1 calc R . . H12B H 0.2111 0.0572 0.5598 0.041 Uiso 1 1 calc R . . C13 C -0.0525(13) 0.0578(5) 0.5789(6) 0.041(3) Uani 1 1 d U . . H13A H -0.1081 0.0630 0.6212 0.050 Uiso 1 1 calc R . . H13B H -0.0898 0.0097 0.5577 0.050 Uiso 1 1 calc R . . C14 C -0.1300(13) 0.1177(6) 0.5265(6) 0.042(3) Uani 1 1 d U . . H14A H -0.0898 0.1660 0.5465 0.051 Uiso 1 1 calc R . . H14B H -0.0806 0.1113 0.4829 0.051 Uiso 1 1 calc R . . C15 C -0.3360(15) 0.1167(7) 0.5085(6) 0.061(4) Uani 1 1 d U . . H15A H -0.3860 0.1204 0.5523 0.073 Uiso 1 1 calc R . . H15B H -0.3766 0.0696 0.4857 0.073 Uiso 1 1 calc R . . C16 C -0.4102(16) 0.1795(7) 0.4594(6) 0.068(4) Uani 1 1 d U . . H16A H -0.5428 0.1771 0.4491 0.102 Uiso 1 1 calc R . . H16B H -0.3629 0.1755 0.4157 0.102 Uiso 1 1 calc R . . H16C H -0.3722 0.2263 0.4822 0.102 Uiso 1 1 calc R . . C17 C 0.3100(12) 0.3111(5) 0.7098(5) 0.024(2) Uani 1 1 d U . . H17A H 0.3604 0.2615 0.7064 0.029 Uiso 1 1 calc R . . H17B H 0.3719 0.3446 0.6817 0.029 Uiso 1 1 calc R . . C18 C 0.3491(12) 0.3351(5) 0.7849(5) 0.030(3) Uani 1 1 d U . . H18A H 0.3026 0.2977 0.8140 0.036 Uiso 1 1 calc R . . H18B H 0.2832 0.3812 0.7895 0.036 Uiso 1 1 calc R . . C19 C 0.5514(13) 0.3471(6) 0.8132(5) 0.035(3) Uani 1 1 d U . . H24A H 0.5705 0.3530 0.8648 0.042 Uiso 1 1 calc R . . H24B H 0.6199 0.3034 0.8028 0.042 Uiso 1 1 calc R . . C20 C 0.6245(12) 0.4145(5) 0.7809(5) 0.031(3) Uani 1 1 d U . . H19A H 0.6024 0.4085 0.7292 0.037 Uiso 1 1 calc R . . H19B H 0.5550 0.4578 0.7915 0.037 Uiso 1 1 calc R . . C21 C 0.8224(12) 0.4292(5) 0.8057(6) 0.038(3) Uani 1 1 d U . . H20A H 0.8932 0.3867 0.7941 0.046 Uiso 1 1 calc R . . H20B H 0.8460 0.4348 0.8574 0.046 Uiso 1 1 calc R . . C22 C 0.8870(13) 0.4985(5) 0.7724(5) 0.042(3) Uani 1 1 d U . . H29A H 1.0168 0.5057 0.7899 0.062 Uiso 1 1 calc R . . H29B H 0.8197 0.5410 0.7848 0.062 Uiso 1 1 calc R . . H29C H 0.8657 0.4930 0.7212 0.062 Uiso 1 1 calc R . . C23 C -0.3122(14) 0.1981(5) 0.9944(5) 0.040(3) Uani 1 1 d U . . H30A H -0.2540 0.2033 1.0437 0.060 Uiso 1 1 calc R . . H30B H -0.4176 0.2306 0.9845 0.060 Uiso 1 1 calc R . . H30C H -0.2256 0.2112 0.9642 0.060 Uiso 1 1 calc R . . C24 C -0.4656(13) 0.1139(5) 0.9066(5) 0.035(3) Uani 1 1 d U . . H31A H -0.5074 0.0634 0.8980 0.052 Uiso 1 1 calc R . . H31B H -0.3816 0.1263 0.8751 0.052 Uiso 1 1 calc R . . H31C H -0.5699 0.1471 0.8979 0.052 Uiso 1 1 calc R . . O1 O -0.0495(8) 0.0718(3) 0.9193(3) 0.0248(17) Uani 1 1 d U . . O2 O 0.1775(8) -0.0022(3) 0.9002(3) 0.0241(16) Uani 1 1 d U . . O3 O -0.4557(8) 0.3892(3) 0.5634(3) 0.0233(16) Uani 1 1 d U . . O4 O -0.2206(8) 0.4585(3) 0.5437(3) 0.0290(17) Uani 1 1 d U . . S1 S -0.0410(3) 0.17335(12) 0.80479(13) 0.0226(7) Uani 1 1 d U . . S2 S -0.2270(3) 0.27446(13) 0.64695(13) 0.0229(7) Uani 1 1 d . . . Zn1 Zn -0.15888(14) 0.04970(6) 1.00612(6) 0.0209(4) Uani 1 1 d . . . N1 N -0.3715(12) 0.1215(4) 0.9806(5) 0.029(2) Uani 1 1 d U . . H1 H -0.443(10) 0.107(5) 1.006(4) 0.01(3) Uiso 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 0.022(5) 0.011(5) 0.024(5) -0.001(5) -0.001(4) -0.012(5) C2 0.029(5) 0.017(5) 0.025(5) -0.002(5) 0.007(4) 0.007(4) C3 0.019(6) 0.024(6) 0.031(6) -0.001(5) 0.005(5) -0.001(5) C4 0.021(5) 0.014(5) 0.031(5) -0.002(5) 0.002(4) -0.009(4) C5 0.022(5) 0.016(6) 0.029(6) 0.003(5) 0.006(5) 0.000(5) C6 0.026(6) 0.015(6) 0.016(5) -0.001(5) 0.004(4) 0.003(5) C7 0.027(6) 0.010(5) 0.032(6) -0.002(5) 0.006(5) -0.004(5) C8 0.029(6) 0.009(6) 0.044(7) -0.001(5) -0.002(5) -0.004(5) C9 0.026(5) 0.007(4) 0.025(5) 0.000(4) 0.000(4) -0.005(4) C10 0.029(5) 0.011(5) 0.028(5) 0.004(4) -0.003(4) 0.007(5) C11 0.030(6) 0.008(5) 0.031(6) 0.004(5) 0.012(5) 0.008(5) C12 0.045(7) 0.013(6) 0.046(7) -0.001(6) 0.013(5) 0.005(5) C13 0.039(6) 0.021(6) 0.062(8) -0.006(6) 0.001(6) 0.005(5) C14 0.040(7) 0.030(7) 0.053(8) 0.002(6) 0.001(6) 0.014(6) C15 0.063(8) 0.052(8) 0.058(9) -0.025(7) -0.016(7) 0.013(7) C16 0.079(10) 0.055(9) 0.059(9) -0.020(8) -0.016(7) 0.035(8) C17 0.024(6) 0.017(6) 0.026(6) -0.001(5) -0.011(5) -0.005(5) C18 0.029(6) 0.022(6) 0.039(7) 0.002(5) 0.003(5) -0.003(5) C19 0.030(6) 0.034(7) 0.039(7) 0.004(6) -0.004(5) 0.004(5) C20 0.043(7) 0.024(6) 0.026(6) -0.005(5) 0.009(5) -0.013(5) C21 0.031(6) 0.027(7) 0.055(8) -0.013(6) 0.003(5) -0.006(5) C22 0.040(7) 0.026(7) 0.055(8) -0.001(6) 0.000(6) -0.013(6) C23 0.049(6) 0.017(5) 0.049(6) -0.001(5) -0.001(5) 0.010(5) C24 0.032(6) 0.021(6) 0.045(8) 0.011(6) -0.009(6) 0.007(5) O1 0.028(4) 0.024(4) 0.023(4) 0.009(3) 0.008(3) 0.002(3) O2 0.033(4) 0.009(4) 0.028(4) 0.007(3) 0.000(3) 0.005(3) O3 0.024(4) 0.012(4) 0.032(4) 0.007(3) -0.002(3) 0.000(3) O4 0.031(4) 0.013(4) 0.040(4) 0.009(4) -0.001(3) -0.002(3) S1 0.0290(15) 0.0084(13) 0.0299(16) 0.0017(12) 0.0042(12) 0.0014(12) S2 0.0255(14) 0.0099(14) 0.0316(16) 0.0022(12) 0.0007(12) 0.0007(11) Zn1 0.0251(6) 0.0071(6) 0.0283(7) -0.0005(6) -0.0007(5) 0.0018(6) N1 0.036(6) 0.014(5) 0.036(6) 0.012(5) 0.002(5) -0.001(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O1 1.262(10) . ? C1 O2 1.275(10) . ? C1 C2 1.471(13) . ? C2 C3 1.325(12) . ? C2 S1 1.736(9) . ? C3 C4 1.419(13) . ? C3 H3 0.9500 . ? C4 C5 1.416(12) . ? C4 C11 1.490(12) . ? C5 C6 1.480(12) . ? C5 S1 1.698(9) . ? C6 C7 1.371(12) . ? C6 S2 1.719(9) . ? C7 C8 1.418(12) . ? C7 C17 1.503(12) . ? C8 C9 1.346(12) . ? C8 H8 0.9500 . ? C9 C10 1.490(12) . ? C9 S2 1.750(9) . ? C10 O3 1.237(10) . ? C10 O4 1.268(11) . ? C11 C12 1.519(12) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.532(13) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.534(13) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.521(14) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.529(15) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.496(12) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.533(12) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.529(13) . ? C19 H24A 0.9900 . ? C19 H24B 0.9900 . ? C20 C21 1.500(12) . ? C20 H19A 0.9900 . ? C20 H19B 0.9900 . ? C21 C22 1.540(13) . ? C21 H20A 0.9900 . ? C21 H20B 0.9900 . ? C22 H29A 0.9800 . ? C22 H29B 0.9800 . ? C22 H29C 0.9800 . ? C23 N1 1.480(12) . ? C23 H30A 0.9800 . ? C23 H30B 0.9800 . ? C23 H30C 0.9800 . ? C24 N1 1.485(12) . ? C24 H31A 0.9800 . ? C24 H31B 0.9800 . ? C24 H31C 0.9800 . ? O1 Zn1 2.042(6) . ? O2 Zn1 2.039(6) 3_557 ? O3 Zn1 2.047(6) 4_565 ? O4 Zn1 2.052(6) 2_456 ? Zn1 O2 2.039(6) 3_557 ? Zn1 O3 2.047(6) 4_666 ? Zn1 O4 2.052(6) 2_446 ? Zn1 N1 2.056(8) . ? Zn1 Zn1 3.041(2) 3_557 ? N1 H1 0.83(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 O2 125.6(9) . . ? O1 C1 C2 117.0(9) . . ? O2 C1 C2 117.4(9) . . ? C3 C2 C1 131.1(9) . . ? C3 C2 S1 110.7(8) . . ? C1 C2 S1 118.1(7) . . ? C2 C3 C4 116.4(9) . . ? C2 C3 H3 121.8 . . ? C4 C3 H3 121.8 . . ? C5 C4 C3 108.5(9) . . ? C5 C4 C11 125.5(8) . . ? C3 C4 C11 125.9(9) . . ? C4 C5 C6 126.5(9) . . ? C4 C5 S1 112.6(7) . . ? C6 C5 S1 120.8(7) . . ? C7 C6 C5 126.2(8) . . ? C7 C6 S2 112.9(7) . . ? C5 C6 S2 121.0(7) . . ? C6 C7 C8 110.2(8) . . ? C6 C7 C17 126.2(9) . . ? C8 C7 C17 123.6(8) . . ? C9 C8 C7 115.9(9) . . ? C9 C8 H8 122.0 . . ? C7 C8 H8 122.0 . . ? C8 C9 C10 129.9(9) . . ? C8 C9 S2 109.7(7) . . ? C10 C9 S2 120.4(7) . . ? O3 C10 O4 128.8(8) . . ? O3 C10 C9 118.0(9) . . ? O4 C10 C9 113.2(8) . . ? C4 C11 C12 113.9(8) . . ? C4 C11 H11A 108.8 . . ? C12 C11 H11A 108.8 . . ? C4 C11 H11B 108.8 . . ? C12 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? C11 C12 C13 113.0(8) . . ? C11 C12 H12A 109.0 . . ? C13 C12 H12A 109.0 . . ? C11 C12 H12B 109.0 . . ? C13 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? C12 C13 C14 115.9(9) . . ? C12 C13 H13A 108.3 . . ? C14 C13 H13A 108.3 . . ? C12 C13 H13B 108.3 . . ? C14 C13 H13B 108.3 . . ? H13A C13 H13B 107.4 . . ? C15 C14 C13 113.0(10) . . ? C15 C14 H14A 109.0 . . ? C13 C14 H14A 109.0 . . ? C15 C14 H14B 109.0 . . ? C13 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? C14 C15 C16 112.0(11) . . ? C14 C15 H15A 109.2 . . ? C16 C15 H15A 109.2 . . ? C14 C15 H15B 109.2 . . ? C16 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C7 113.0(8) . . ? C18 C17 H17A 109.0 . . ? C7 C17 H17A 109.0 . . ? C18 C17 H17B 109.0 . . ? C7 C17 H17B 109.0 . . ? H17A C17 H17B 107.8 . . ? C17 C18 C19 113.3(8) . . ? C17 C18 H18A 108.9 . . ? C19 C18 H18A 108.9 . . ? C17 C18 H18B 108.9 . . ? C19 C18 H18B 108.9 . . ? H18A C18 H18B 107.7 . . ? C20 C19 C18 112.0(8) . . ? C20 C19 H24A 109.2 . . ? C18 C19 H24A 109.2 . . ? C20 C19 H24B 109.2 . . ? C18 C19 H24B 109.2 . . ? H24A C19 H24B 107.9 . . ? C21 C20 C19 114.9(8) . . ? C21 C20 H19A 108.5 . . ? C19 C20 H19A 108.5 . . ? C21 C20 H19B 108.5 . . ? C19 C20 H19B 108.5 . . ? H19A C20 H19B 107.5 . . ? C20 C21 C22 112.5(8) . . ? C20 C21 H20A 109.1 . . ? C22 C21 H20A 109.1 . . ? C20 C21 H20B 109.1 . . ? C22 C21 H20B 109.1 . . ? H20A C21 H20B 107.8 . . ? C21 C22 H29A 109.5 . . ? C21 C22 H29B 109.5 . . ? H29A C22 H29B 109.5 . . ? C21 C22 H29C 109.5 . . ? H29A C22 H29C 109.5 . . ? H29B C22 H29C 109.5 . . ? N1 C23 H30A 109.5 . . ? N1 C23 H30B 109.5 . . ? H30A C23 H30B 109.5 . . ? N1 C23 H30C 109.5 . . ? H30A C23 H30C 109.5 . . ? H30B C23 H30C 109.5 . . ? N1 C24 H31A 109.5 . . ? N1 C24 H31B 109.5 . . ? H31A C24 H31B 109.5 . . ? N1 C24 H31C 109.5 . . ? H31A C24 H31C 109.5 . . ? H31B C24 H31C 109.5 . . ? C1 O1 Zn1 143.7(6) . . ? C1 O2 Zn1 113.3(6) . 3_557 ? C10 O3 Zn1 123.3(6) . 4_565 ? C10 O4 Zn1 128.8(6) . 2_456 ? C5 S1 C2 91.7(5) . . ? C6 S2 C9 91.4(4) . . ? O2 Zn1 O1 156.9(2) 3_557 . ? O2 Zn1 O3 85.1(2) 3_557 4_666 ? O1 Zn1 O3 88.2(2) . 4_666 ? O2 Zn1 O4 88.7(2) 3_557 2_446 ? O1 Zn1 O4 88.9(3) . 2_446 ? O3 Zn1 O4 156.9(2) 4_666 2_446 ? O2 Zn1 N1 108.1(3) 3_557 . ? O1 Zn1 N1 94.9(3) . . ? O3 Zn1 N1 104.6(3) 4_666 . ? O4 Zn1 N1 98.6(3) 2_446 . ? O2 Zn1 Zn1 89.77(18) 3_557 3_557 ? O1 Zn1 Zn1 67.40(17) . 3_557 ? O3 Zn1 Zn1 81.44(18) 4_666 3_557 ? O4 Zn1 Zn1 76.27(18) 2_446 3_557 ? N1 Zn1 Zn1 161.4(3) . 3_557 ? C23 N1 C24 109.7(8) . . ? C23 N1 Zn1 111.5(6) . . ? C24 N1 Zn1 112.6(6) . . ? C23 N1 H1 113(6) . . ? C24 N1 H1 107(6) . . ? Zn1 N1 H1 102(6) . . ? 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 O1 C1 C2 C3 -170.3(10) . . . . ? O2 C1 C2 C3 10.0(15) . . . . ? O1 C1 C2 S1 10.7(11) . . . . ? O2 C1 C2 S1 -169.0(6) . . . . ? C1 C2 C3 C4 179.5(9) . . . . ? S1 C2 C3 C4 -1.5(11) . . . . ? C2 C3 C4 C5 2.5(11) . . . . ? C2 C3 C4 C11 -175.6(9) . . . . ? C3 C4 C5 C6 173.9(8) . . . . ? C11 C4 C5 C6 -8.0(14) . . . . ? C3 C4 C5 S1 -2.3(9) . . . . ? C11 C4 C5 S1 175.8(7) . . . . ? C4 C5 C6 C7 -65.8(14) . . . . ? S1 C5 C6 C7 110.1(10) . . . . ? C4 C5 C6 S2 115.7(9) . . . . ? S1 C5 C6 S2 -68.3(9) . . . . ? C5 C6 C7 C8 -178.7(9) . . . . ? S2 C6 C7 C8 -0.1(10) . . . . ? C5 C6 C7 C17 -0.1(16) . . . . ? S2 C6 C7 C17 178.4(8) . . . . ? C6 C7 C8 C9 -0.5(13) . . . . ? C17 C7 C8 C9 -179.1(9) . . . . ? C7 C8 C9 C10 -177.6(9) . . . . ? C7 C8 C9 S2 0.9(11) . . . . ? C8 C9 C10 O3 -172.4(10) . . . . ? S2 C9 C10 O3 9.2(12) . . . . ? C8 C9 C10 O4 8.8(15) . . . . ? S2 C9 C10 O4 -169.5(7) . . . . ? C5 C4 C11 C12 -115.3(10) . . . . ? C3 C4 C11 C12 62.5(11) . . . . ? C4 C11 C12 C13 58.6(11) . . . . ? C11 C12 C13 C14 68.6(12) . . . . ? C12 C13 C14 C15 -177.4(9) . . . . ? C13 C14 C15 C16 176.8(9) . . . . ? C6 C7 C17 C18 -81.0(12) . . . . ? C8 C7 C17 C18 97.3(11) . . . . ? C7 C17 C18 C19 -171.7(8) . . . . ? C17 C18 C19 C20 70.2(11) . . . . ? C18 C19 C20 C21 -179.4(8) . . . . ? C19 C20 C21 C22 -178.9(9) . . . . ? O2 C1 O1 Zn1 -2.4(16) . . . . ? C2 C1 O1 Zn1 177.9(6) . . . . ? O1 C1 O2 Zn1 -3.3(11) . . . 3_557 ? C2 C1 O2 Zn1 176.3(6) . . . 3_557 ? O4 C10 O3 Zn1 -3.8(14) . . . 4_565 ? C9 C10 O3 Zn1 177.7(6) . . . 4_565 ? O3 C10 O4 Zn1 14.4(15) . . . 2_456 ? C9 C10 O4 Zn1 -167.0(6) . . . 2_456 ? C4 C5 S1 C2 1.4(7) . . . . ? C6 C5 S1 C2 -175.1(7) . . . . ? C3 C2 S1 C5 0.1(8) . . . . ? C1 C2 S1 C5 179.2(7) . . . . ? C7 C6 S2 C9 0.5(8) . . . . ? C5 C6 S2 C9 179.1(8) . . . . ? C8 C9 S2 C6 -0.8(8) . . . . ? C10 C9 S2 C6 177.9(8) . . . . ? C1 O1 Zn1 O2 13.2(13) . . . 3_557 ? C1 O1 Zn1 O3 86.1(10) . . . 4_666 ? C1 O1 Zn1 O4 -70.9(10) . . . 2_446 ? C1 O1 Zn1 N1 -169.5(10) . . . . ? C1 O1 Zn1 Zn1 4.6(9) . . . 3_557 ? O2 Zn1 N1 C23 102.8(7) 3_557 . . . ? O1 Zn1 N1 C23 -76.1(7) . . . . ? O3 Zn1 N1 C23 13.3(8) 4_666 . . . ? O4 Zn1 N1 C23 -165.8(7) 2_446 . . . ? Zn1 Zn1 N1 C23 -93.6(10) 3_557 . . . ? O2 Zn1 N1 C24 -133.4(7) 3_557 . . . ? O1 Zn1 N1 C24 47.7(7) . . . . ? O3 Zn1 N1 C24 137.1(7) 4_666 . . . ? O4 Zn1 N1 C24 -41.9(7) 2_446 . . . ? Zn1 Zn1 N1 C24 30.3(13) 3_557 . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 22.61 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.505 _refine_diff_density_min -0.754 _refine_diff_density_rms 0.126 # sin(theta_max) is low because diffrn_reflns_theta_max is low. This # is due to the poorly diffracting nature of 2. data_3 _database_code_depnum_ccdc_archive 'CCDC 876809' #TrackingRef '- CE-ART--04-2012-025529cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H9 N O4 S2 Zn' _chemical_formula_weight 408.73 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.1764(8) _cell_length_b 22.0141(12) _cell_length_c 9.9312(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.535(2) _cell_angle_gamma 90.00 _cell_volume 3730.8(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4193 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 27.31 _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 1.557 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8218 _exptl_absorpt_correction_T_max 0.8967 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 X8 APEX II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20371 _diffrn_reflns_av_R_equivalents 0.0438 _diffrn_reflns_av_sigmaI/netI 0.0669 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 30.00 _reflns_number_total 5427 _reflns_number_gt 3474 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2\s(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^)+(0.0570P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5427 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0772 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.1102 _refine_ls_wR_factor_gt 0.1010 _refine_ls_goodness_of_fit_ref 0.962 _refine_ls_restrained_S_all 0.962 _refine_ls_shift/su_max 0.002 _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 0.08163(14) 0.36112(12) 0.1794(3) 0.0201(6) Uani 1 1 d . . . C2 C 0.12023(15) 0.42016(12) 0.1719(3) 0.0213(6) Uani 1 1 d . . . C3 C 0.10091(16) 0.46779(13) 0.0864(3) 0.0270(6) Uani 1 1 d . . . H3 H 0.0618 0.4660 0.0136 0.032 Uiso 1 1 calc R . . C4 C 0.14678(16) 0.52015(13) 0.1205(3) 0.0283(7) Uani 1 1 d . . . H4 H 0.1408 0.5565 0.0728 0.034 Uiso 1 1 calc R . . C5 C 0.20107(16) 0.51161(12) 0.2317(3) 0.0254(6) Uani 1 1 d . . . C6 C 0.25870(16) 0.55448(13) 0.2948(3) 0.0268(6) Uani 1 1 d . . . C7 C 0.28721(18) 0.56132(13) 0.4277(3) 0.0324(7) Uani 1 1 d . . . H7 H 0.2722 0.5369 0.4966 0.039 Uiso 1 1 calc R . . C8 C 0.34136(17) 0.60881(13) 0.4503(3) 0.0302(7) Uani 1 1 d . . . H8 H 0.3656 0.6195 0.5355 0.036 Uiso 1 1 calc R . . C9 C 0.35468(15) 0.63771(12) 0.3330(3) 0.0250(6) Uani 1 1 d . . . C10 C 0.40730(15) 0.68912(12) 0.3100(3) 0.0216(6) Uani 1 1 d . . . C11 C 0.6575(3) 0.73274(17) 0.6103(4) 0.0682(14) Uani 1 1 d . . . H11 H 0.6700 0.7056 0.5442 0.082 Uiso 1 1 calc R . . C12 C 0.58695(17) 0.81203(16) 0.6730(3) 0.0377(8) Uani 1 1 d . . . H12 H 0.5489 0.8415 0.6507 0.045 Uiso 1 1 calc R . . C13 C 0.7003(3) 0.72978(16) 0.7391(4) 0.0679(14) Uani 1 1 d . . . H13 H 0.7403 0.7015 0.7570 0.081 Uiso 1 1 calc R . . C14 C 0.62576(18) 0.81267(16) 0.8023(3) 0.0413(8) Uani 1 1 d . . . H14 H 0.6141 0.8419 0.8644 0.050 Uiso 1 1 calc R . . C15 C 0.68260(17) 0.76891(13) 0.8382(3) 0.0300(7) Uani 1 1 d . . . C16 C 0.72234(17) 0.76884(14) 0.9778(3) 0.0319(7) Uani 1 1 d . . . H16 H 0.7069 0.7976 1.0380 0.038 Uiso 1 1 calc R . . N N 0.60032(13) 0.77212(10) 0.5782(2) 0.0229(5) Uani 1 1 d . . . O1 O 0.44288(10) 0.71512(8) 0.41222(19) 0.0224(4) Uani 1 1 d . . . O2 O 0.41152(10) 0.70192(8) 0.18759(19) 0.0243(4) Uani 1 1 d . . . O3 O 0.10159(10) 0.32863(8) 0.28218(19) 0.0258(4) Uani 1 1 d . . . O4 O 0.03017(10) 0.34734(8) 0.08247(19) 0.0239(4) Uani 1 1 d . . . S1 S 0.19580(4) 0.43900(3) 0.29507(7) 0.02675(17) Uani 1 1 d . . . S2 S 0.29978(4) 0.60642(3) 0.19408(7) 0.02579(17) Uani 1 1 d . . . Zn1 Zn 0.535476(16) 0.771982(13) 0.39496(3) 0.01656(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 C1 0.0206(13) 0.0192(14) 0.0208(14) -0.0024(11) 0.0038(11) -0.0017(11) C2 0.0213(13) 0.0229(15) 0.0197(14) -0.0052(11) 0.0020(11) -0.0046(11) C3 0.0251(14) 0.0255(16) 0.0295(16) 0.0001(13) -0.0011(12) -0.0043(12) C4 0.0364(16) 0.0194(15) 0.0287(17) 0.0035(12) 0.0024(13) -0.0018(13) C5 0.0279(14) 0.0234(15) 0.0254(15) -0.0040(12) 0.0045(12) -0.0085(12) C6 0.0302(15) 0.0236(15) 0.0271(16) -0.0011(12) 0.0057(12) -0.0089(12) C7 0.0443(18) 0.0293(17) 0.0237(16) 0.0014(13) 0.0042(13) -0.0140(14) C8 0.0377(16) 0.0282(17) 0.0243(16) 0.0005(12) 0.0018(13) -0.0084(13) C9 0.0259(14) 0.0222(15) 0.0265(16) -0.0032(12) 0.0018(11) -0.0031(12) C10 0.0232(13) 0.0173(13) 0.0240(15) -0.0016(12) 0.0008(11) -0.0015(11) C11 0.093(3) 0.058(3) 0.043(2) -0.0309(19) -0.039(2) 0.049(2) C12 0.0321(16) 0.054(2) 0.0243(17) -0.0076(15) -0.0062(13) 0.0173(15) C13 0.092(3) 0.051(2) 0.048(2) -0.0125(19) -0.044(2) 0.044(2) C14 0.0363(17) 0.061(2) 0.0249(17) -0.0104(16) -0.0049(14) 0.0123(16) C15 0.0325(15) 0.0331(17) 0.0218(15) 0.0059(13) -0.0072(12) -0.0078(13) C16 0.0307(15) 0.0391(19) 0.0246(16) -0.0005(13) -0.0027(12) -0.0040(13) N 0.0236(11) 0.0244(13) 0.0190(12) 0.0016(10) -0.0045(9) 0.0005(10) O1 0.0248(10) 0.0198(10) 0.0220(10) 0.0002(8) 0.0001(8) -0.0059(8) O2 0.0276(10) 0.0230(10) 0.0213(11) 0.0008(8) -0.0011(8) -0.0065(8) O3 0.0286(10) 0.0241(11) 0.0236(11) 0.0033(8) -0.0009(8) -0.0058(8) O4 0.0237(9) 0.0212(10) 0.0254(11) -0.0018(8) -0.0035(8) -0.0042(8) S1 0.0332(4) 0.0244(4) 0.0212(4) 0.0001(3) -0.0029(3) -0.0107(3) S2 0.0294(4) 0.0247(4) 0.0232(4) -0.0027(3) 0.0028(3) -0.0095(3) Zn1 0.01792(15) 0.01666(17) 0.01381(16) 0.00042(12) -0.00381(11) 0.00076(12) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O3 1.262(3) . ? C1 O4 1.267(3) . ? C1 C2 1.465(4) . ? C2 C3 1.366(4) . ? C2 S1 1.730(3) . ? C3 C4 1.415(4) . ? C3 H3 0.9300 . ? C4 C5 1.374(4) . ? C4 H4 0.9300 . ? C5 C6 1.457(4) . ? C5 S1 1.724(3) . ? C6 C7 1.363(4) . ? C6 S2 1.722(3) . ? C7 C8 1.400(4) . ? C7 H7 0.9300 . ? C8 C9 1.369(4) . ? C8 H8 0.9300 . ? C9 C10 1.482(4) . ? C9 S2 1.724(3) . ? C10 O2 1.258(3) . ? C10 O1 1.261(3) . ? C11 N 1.322(4) . ? C11 C13 1.402(5) . ? C11 H11 0.9300 . ? C12 N 1.327(4) . ? C12 C14 1.377(4) . ? C12 H12 0.9300 . ? C13 C15 1.368(5) . ? C13 H13 0.9300 . ? C14 C15 1.389(4) . ? C14 H14 0.9300 . ? C15 C16 1.474(4) . ? C16 C16 1.300(6) 7_667 ? C16 H16 0.9300 . ? N Zn1 2.023(2) . ? O1 Zn1 2.0464(17) . ? O2 Zn1 2.0124(18) 2_655 ? O3 Zn1 2.0948(18) 3_445 ? O4 Zn1 2.0325(18) 4_545 ? Zn1 O2 2.0124(18) 2_655 ? Zn1 O4 2.0325(18) 4 ? Zn1 O3 2.0948(18) 3 ? Zn1 Zn1 2.9961(6) 2_655 ? 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 O3 C1 O4 125.5(2) . . ? O3 C1 C2 117.5(2) . . ? O4 C1 C2 117.0(2) . . ? C3 C2 C1 129.3(2) . . ? C3 C2 S1 111.4(2) . . ? C1 C2 S1 119.0(2) . . ? C2 C3 C4 112.8(2) . . ? C2 C3 H3 123.6 . . ? C4 C3 H3 123.6 . . ? C5 C4 C3 112.9(3) . . ? C5 C4 H4 123.5 . . ? C3 C4 H4 123.5 . . ? C4 C5 C6 128.5(3) . . ? C4 C5 S1 111.2(2) . . ? C6 C5 S1 120.3(2) . . ? C7 C6 C5 129.8(3) . . ? C7 C6 S2 111.3(2) . . ? C5 C6 S2 118.9(2) . . ? C6 C7 C8 113.4(3) . . ? C6 C7 H7 123.3 . . ? C8 C7 H7 123.3 . . ? C9 C8 C7 112.5(3) . . ? C9 C8 H8 123.7 . . ? C7 C8 H8 123.7 . . ? C8 C9 C10 130.5(3) . . ? C8 C9 S2 111.5(2) . . ? C10 C9 S2 118.0(2) . . ? O2 C10 O1 126.9(2) . . ? O2 C10 C9 115.0(2) . . ? O1 C10 C9 118.1(2) . . ? N C11 C13 123.3(3) . . ? N C11 H11 118.4 . . ? C13 C11 H11 118.4 . . ? N C12 C14 124.3(3) . . ? N C12 H12 117.8 . . ? C14 C12 H12 117.8 . . ? C15 C13 C11 119.4(3) . . ? C15 C13 H13 120.3 . . ? C11 C13 H13 120.3 . . ? C12 C14 C15 118.9(3) . . ? C12 C14 H14 120.5 . . ? C15 C14 H14 120.5 . . ? C13 C15 C14 117.3(3) . . ? C13 C15 C16 124.0(3) . . ? C14 C15 C16 118.6(3) . . ? C16 C16 C15 124.2(4) 7_667 . ? C16 C16 H16 117.9 7_667 . ? C15 C16 H16 117.9 . . ? C11 N C12 116.6(3) . . ? C11 N Zn1 122.3(2) . . ? C12 N Zn1 121.17(19) . . ? C10 O1 Zn1 121.34(17) . . ? C10 O2 Zn1 130.07(17) . 2_655 ? C1 O3 Zn1 131.02(17) . 3_445 ? C1 O4 Zn1 117.35(17) . 4_545 ? C5 S1 C2 91.73(13) . . ? C6 S2 C9 91.35(14) . . ? O2 Zn1 N 98.01(8) 2_655 . ? O2 Zn1 O4 162.34(8) 2_655 4 ? N Zn1 O4 98.92(8) . 4 ? O2 Zn1 O1 87.55(8) 2_655 . ? N Zn1 O1 106.21(8) . . ? O4 Zn1 O1 92.51(7) 4 . ? O2 Zn1 O3 86.59(8) 2_655 3 ? N Zn1 O3 101.75(8) . 3 ? O4 Zn1 O3 85.09(7) 4 3 ? O1 Zn1 O3 151.96(7) . 3 ? O2 Zn1 Zn1 76.23(5) 2_655 2_655 ? N Zn1 Zn1 170.67(7) . 2_655 ? O4 Zn1 Zn1 86.32(5) 4 2_655 ? O1 Zn1 Zn1 81.11(5) . 2_655 ? O3 Zn1 Zn1 70.86(5) 3 2_655 ? 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 O3 C1 C2 C3 -167.5(3) . . . . ? O4 C1 C2 C3 11.7(4) . . . . ? O3 C1 C2 S1 5.4(3) . . . . ? O4 C1 C2 S1 -175.41(18) . . . . ? C1 C2 C3 C4 172.9(3) . . . . ? S1 C2 C3 C4 -0.4(3) . . . . ? C2 C3 C4 C5 0.4(4) . . . . ? C3 C4 C5 C6 179.1(3) . . . . ? C3 C4 C5 S1 -0.1(3) . . . . ? C4 C5 C6 C7 146.3(3) . . . . ? S1 C5 C6 C7 -34.6(4) . . . . ? C4 C5 C6 S2 -33.2(4) . . . . ? S1 C5 C6 S2 145.87(18) . . . . ? C5 C6 C7 C8 -178.7(3) . . . . ? S2 C6 C7 C8 0.9(4) . . . . ? C6 C7 C8 C9 -0.8(4) . . . . ? C7 C8 C9 C10 -179.3(3) . . . . ? C7 C8 C9 S2 0.3(3) . . . . ? C8 C9 C10 O2 173.9(3) . . . . ? S2 C9 C10 O2 -5.6(3) . . . . ? C8 C9 C10 O1 -5.9(4) . . . . ? S2 C9 C10 O1 174.59(19) . . . . ? N C11 C13 C15 0.4(7) . . . . ? N C12 C14 C15 -0.3(5) . . . . ? C11 C13 C15 C14 -4.2(6) . . . . ? C11 C13 C15 C16 178.4(4) . . . . ? C12 C14 C15 C13 4.2(5) . . . . ? C12 C14 C15 C16 -178.3(3) . . . . ? C13 C15 C16 C16 -0.9(6) . . . 7_667 ? C14 C15 C16 C16 -178.3(4) . . . 7_667 ? C13 C11 N C12 3.4(6) . . . . ? C13 C11 N Zn1 -176.3(4) . . . . ? C14 C12 N C11 -3.4(5) . . . . ? C14 C12 N Zn1 176.2(3) . . . . ? O2 C10 O1 Zn1 -14.6(4) . . . . ? C9 C10 O1 Zn1 165.18(17) . . . . ? O1 C10 O2 Zn1 -7.5(4) . . . 2_655 ? C9 C10 O2 Zn1 172.68(17) . . . 2_655 ? O4 C1 O3 Zn1 -36.9(4) . . . 3_445 ? C2 C1 O3 Zn1 142.16(19) . . . 3_445 ? O3 C1 O4 Zn1 8.3(3) . . . 4_545 ? C2 C1 O4 Zn1 -170.80(17) . . . 4_545 ? C4 C5 S1 C2 -0.1(2) . . . . ? C6 C5 S1 C2 -179.4(2) . . . . ? C3 C2 S1 C5 0.3(2) . . . . ? C1 C2 S1 C5 -173.8(2) . . . . ? C7 C6 S2 C9 -0.6(2) . . . . ? C5 C6 S2 C9 179.0(2) . . . . ? C8 C9 S2 C6 0.2(2) . . . . ? C10 C9 S2 C6 179.8(2) . . . . ? C11 N Zn1 O2 -0.3(3) . . . 2_655 ? C12 N Zn1 O2 -179.9(2) . . . 2_655 ? C11 N Zn1 O4 -175.2(3) . . . 4 ? C12 N Zn1 O4 5.1(2) . . . 4 ? C11 N Zn1 O1 89.5(3) . . . . ? C12 N Zn1 O1 -90.2(2) . . . . ? C11 N Zn1 O3 -88.4(3) . . . 3 ? C12 N Zn1 O3 91.9(2) . . . 3 ? C11 N Zn1 Zn1 -51.5(6) . . . 2_655 ? C12 N Zn1 Zn1 128.8(4) . . . 2_655 ? C10 O1 Zn1 O2 -57.9(2) . . . 2_655 ? C10 O1 Zn1 N -155.54(19) . . . . ? C10 O1 Zn1 O4 104.4(2) . . . 4 ? C10 O1 Zn1 O3 20.2(3) . . . 3 ? C10 O1 Zn1 Zn1 18.53(19) . . . 2_655 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.990 _refine_diff_density_min -0.452 _refine_diff_density_rms 0.095 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 -0.018 357 63 ' ' 2 0.500 0.500 -0.002 357 63 ' ' 3 0.000 0.551 0.250 13 2 ' ' 4 0.500 0.051 0.250 13 2 ' ' 5 0.000 0.449 0.750 13 2 ' ' 6 0.500 0.949 0.750 13 2 ' ' _platon_squeeze_details ; ; data_4 _database_code_depnum_ccdc_archive 'CCDC 876810' #TrackingRef '- CE-ART--04-2012-025529cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H36 N4 O6 S2 Zn' _chemical_formula_weight 798.22 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6855(15) _cell_length_b 12.7109(18) _cell_length_c 18.183(3) _cell_angle_alpha 91.810(8) _cell_angle_beta 102.910(9) _cell_angle_gamma 106.455(8) _cell_volume 1866.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1605 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 21.31 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.420 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 828 _exptl_absorpt_coefficient_mu 0.823 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7051 _exptl_absorpt_correction_T_max 0.8140 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 X8 APEX II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19580 _diffrn_reflns_av_R_equivalents 0.0892 _diffrn_reflns_av_sigmaI/netI 0.1144 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 23.33 _reflns_number_total 5356 _reflns_number_gt 3392 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2\s(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^)+(0.0596P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5356 _refine_ls_number_parameters 482 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1068 _refine_ls_R_factor_gt 0.0515 _refine_ls_wR_factor_ref 0.1314 _refine_ls_wR_factor_gt 0.1012 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _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 0.0841(8) 0.9600(4) 0.2576(3) 0.0193(14) Uani 1 1 d . . . C2 C 0.1894(7) 1.0486(4) 0.2235(3) 0.0167(13) Uani 1 1 d . . . C3 C 0.1517(7) 1.0849(4) 0.1535(3) 0.0189(14) Uani 1 1 d . . . H3 H 0.0516 1.0513 0.1164 0.023 Uiso 1 1 calc R . . C4 C 0.2787(7) 1.1787(4) 0.1417(3) 0.0154(13) Uani 1 1 d . . . C5 C 0.4090(7) 1.2106(4) 0.2037(3) 0.0179(14) Uani 1 1 d . . . C6 C 0.5553(6) 1.3098(4) 0.2175(3) 0.0150(13) Uani 1 1 d . . . C7 C 0.6780(7) 1.3418(4) 0.1792(3) 0.0195(14) Uani 1 1 d . . . C8 C 0.7807(7) 1.4503(4) 0.2069(3) 0.0213(14) Uani 1 1 d . . . H8 H 0.8701 1.4877 0.1862 0.026 Uiso 1 1 calc R . . C9 C 0.7404(7) 1.4963(4) 0.2657(3) 0.0179(13) Uani 1 1 d . . . C10 C -0.1776(7) 0.6047(4) 0.3115(3) 0.0202(14) Uani 1 1 d . . . C11 C 0.2617(7) 1.2350(4) 0.0717(3) 0.0196(14) Uani 1 1 d . . . C12 C 0.2990(7) 1.3499(5) 0.0749(3) 0.0303(16) Uani 1 1 d . . . H12 H 0.3354 1.3929 0.1227 0.036 Uiso 1 1 calc R . . C13 C 0.2830(8) 1.4013(5) 0.0088(4) 0.0377(18) Uani 1 1 d . . . H13 H 0.3102 1.4794 0.0114 0.045 Uiso 1 1 calc R . . C14 C 0.2278(8) 1.3397(5) -0.0610(4) 0.0364(17) Uani 1 1 d . . . H14 H 0.2154 1.3753 -0.1062 0.044 Uiso 1 1 calc R . . C15 C 0.1909(7) 1.2266(5) -0.0650(3) 0.0292(16) Uani 1 1 d . . . H15 H 0.1554 1.1843 -0.1130 0.035 Uiso 1 1 calc R . . C16 C 0.2050(7) 1.1742(5) 0.0006(3) 0.0230(14) Uani 1 1 d . . . H16 H 0.1758 1.0960 -0.0028 0.028 Uiso 1 1 calc R . . C17 C 0.7051(7) 1.2733(4) 0.1185(3) 0.0214(14) Uani 1 1 d . . . C18 C 0.7951(7) 1.3231(5) 0.0673(3) 0.0284(15) Uani 1 1 d . . . H18 H 0.8314 1.4012 0.0691 0.034 Uiso 1 1 calc R . . C19 C 0.8319(8) 1.2603(5) 0.0142(3) 0.0339(16) Uani 1 1 d . . . H19 H 0.8935 1.2955 -0.0199 0.041 Uiso 1 1 calc R . . C20 C 0.7799(8) 1.1465(5) 0.0103(3) 0.0332(16) Uani 1 1 d . . . H20 H 0.8047 1.1035 -0.0265 0.040 Uiso 1 1 calc R . . C21 C 0.6910(7) 1.0956(5) 0.0608(3) 0.0300(16) Uani 1 1 d . . . H21 H 0.6545 1.0175 0.0585 0.036 Uiso 1 1 calc R . . C22 C 0.6553(7) 1.1585(4) 0.1145(3) 0.0252(15) Uani 1 1 d . . . H22 H 0.5958 1.1228 0.1492 0.030 Uiso 1 1 calc R . . C23 C 0.3224(7) 0.7445(4) 0.3837(3) 0.0275(15) Uani 1 1 d . . . H23 H 0.3357 0.7889 0.3432 0.033 Uiso 1 1 calc R . . C24 C 0.1844(8) 0.6820(5) 0.4736(3) 0.0365(17) Uani 1 1 d . . . H24 H 0.0979 0.6802 0.4980 0.044 Uiso 1 1 calc R . . C25 C 0.4287(7) 0.6824(4) 0.4041(3) 0.0262(15) Uani 1 1 d . . . H25 H 0.5139 0.6856 0.3786 0.031 Uiso 1 1 calc R . . C26 C 0.2879(8) 0.6172(5) 0.4983(3) 0.0364(18) Uani 1 1 d . . . H26 H 0.2743 0.5746 0.5397 0.044 Uiso 1 1 calc R . . C27 C 0.4112(7) 0.6162(5) 0.4612(3) 0.0274(15) Uani 1 1 d . . . C28 C 0.5134(8) 0.5409(4) 0.4783(3) 0.0289(15) Uani 1 1 d . . . H28 H 0.6057 0.5520 0.4564 0.035 Uiso 1 1 calc R . . C29 C -0.4383(7) 0.9815(4) 0.5177(3) 0.0192(13) Uani 1 1 d . . . H29 H -0.4244 0.9767 0.5707 0.023 Uiso 1 1 calc R . . C30 C -0.3229(7) 0.9477(4) 0.4818(3) 0.0202(14) Uani 1 1 d . . . C31 C -0.3101(7) 0.9692(4) 0.4088(3) 0.0223(14) Uani 1 1 d . . . H31 H -0.3744 1.0104 0.3807 0.027 Uiso 1 1 calc R . . C32 C -0.2217(7) 0.8900(4) 0.5203(3) 0.0213(14) Uani 1 1 d . . . H32 H -0.2232 0.8759 0.5711 0.026 Uiso 1 1 calc R . . C33 C -0.2041(7) 0.9307(4) 0.3770(3) 0.0240(15) Uani 1 1 d . . . H33 H -0.1969 0.9466 0.3270 0.029 Uiso 1 1 calc R . . C34 C -0.1190(7) 0.8532(4) 0.4852(3) 0.0238(15) Uani 1 1 d . . . H34 H -0.0517 0.8133 0.5127 0.029 Uiso 1 1 calc R . . C35 C 0.2093(9) 0.6715(6) 0.1824(4) 0.0425(19) Uani 1 1 d . . . H35 H 0.1358 0.7117 0.1894 0.051 Uiso 1 1 calc R . . C36 C 0.4847(9) 0.6755(6) 0.1738(5) 0.067(3) Uani 1 1 d . . . H36A H 0.4555 0.6013 0.1903 0.100 Uiso 1 1 calc R . . H36B H 0.5946 0.7184 0.2039 0.100 Uiso 1 1 calc R . . H36C H 0.4858 0.6703 0.1201 0.100 Uiso 1 1 calc R . . C37 C 0.4155(9) 0.8473(5) 0.1884(4) 0.050(2) Uani 1 1 d . . . H37A H 0.3196 0.8738 0.1874 0.075 Uiso 1 1 calc R . . H37B H 0.4614 0.8710 0.1449 0.075 Uiso 1 1 calc R . . H37C H 0.4999 0.8778 0.2355 0.075 Uiso 1 1 calc R . . C38 C 0.9039(9) 0.2191(5) 0.3132(4) 0.0413(18) Uani 1 1 d . . . H38 H 0.8704 0.1599 0.2743 0.050 Uiso 1 1 calc R . . C39 C 1.0752(9) 0.4019(6) 0.3620(4) 0.064(2) Uani 1 1 d . . . H39A H 0.9952 0.3969 0.3931 0.095 Uiso 1 1 calc R . . H39B H 1.0884 0.4700 0.3370 0.095 Uiso 1 1 calc R . . H39C H 1.1821 0.4023 0.3943 0.095 Uiso 1 1 calc R . . C40 C 1.0917(9) 0.3167(6) 0.2415(4) 0.061(2) Uani 1 1 d . . . H40A H 1.0403 0.2480 0.2078 0.091 Uiso 1 1 calc R . . H40B H 1.2107 0.3274 0.2593 0.091 Uiso 1 1 calc R . . H40C H 1.0736 0.3788 0.2138 0.091 Uiso 1 1 calc R . . N1 N 0.2003(6) 0.7459(3) 0.4180(2) 0.0200(11) Uani 1 1 d . . . N2 N -0.1102(5) 0.8714(3) 0.4137(2) 0.0175(11) Uani 1 1 d . . . N3 N 0.3650(6) 0.7289(4) 0.1843(3) 0.0302(13) Uani 1 1 d . . . N4 N 1.0175(6) 0.3105(4) 0.3066(3) 0.0367(14) Uani 1 1 d . . . O1 O 0.1653(4) 0.9272(3) 0.3166(2) 0.0211(9) Uani 1 1 d . . . O2 O -0.0656(5) 0.9244(3) 0.2310(2) 0.0238(10) Uani 1 1 d . . . O3 O -0.0852(5) 0.6786(3) 0.2805(2) 0.0230(9) Uani 1 1 d . . . O4 O -0.2014(5) 0.6191(3) 0.3755(2) 0.0276(10) Uani 1 1 d . . . O5 O 0.1540(6) 0.5707(4) 0.1724(3) 0.0686(16) Uani 1 1 d . . . O6 O 0.8391(7) 0.2073(4) 0.3680(3) 0.0687(16) Uani 1 1 d . . . S1 S 0.38146(18) 1.12758(11) 0.27622(8) 0.0196(4) Uani 1 1 d . . . S2 S 0.57350(18) 1.40794(11) 0.28921(8) 0.0221(4) Uani 1 1 d . . . Zn1 Zn 0.02072(8) 0.80608(5) 0.35707(4) 0.0161(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 0.035(4) 0.011(3) 0.016(4) 0.001(3) 0.012(3) 0.009(3) C2 0.024(4) 0.012(3) 0.018(3) 0.003(3) 0.003(3) 0.012(3) C3 0.017(3) 0.016(3) 0.022(4) -0.001(3) 0.003(3) 0.004(3) C4 0.016(3) 0.012(3) 0.021(4) 0.001(3) 0.005(3) 0.007(3) C5 0.025(4) 0.017(3) 0.015(3) 0.004(3) 0.008(3) 0.009(3) C6 0.014(3) 0.010(3) 0.016(3) 0.002(2) -0.002(3) 0.001(3) C7 0.019(3) 0.014(3) 0.025(4) 0.005(3) 0.005(3) 0.003(3) C8 0.016(3) 0.021(3) 0.026(4) 0.007(3) 0.007(3) 0.003(3) C9 0.021(3) 0.013(3) 0.019(3) 0.004(3) 0.003(3) 0.006(3) C10 0.021(4) 0.014(3) 0.028(4) 0.003(3) 0.007(3) 0.009(3) C11 0.018(3) 0.020(3) 0.020(4) 0.003(3) 0.005(3) 0.003(3) C12 0.035(4) 0.027(4) 0.027(4) 0.007(3) 0.004(3) 0.009(3) C13 0.044(5) 0.030(4) 0.040(5) 0.015(4) 0.012(4) 0.009(3) C14 0.036(4) 0.044(5) 0.039(5) 0.024(4) 0.015(4) 0.019(4) C15 0.031(4) 0.042(4) 0.015(4) 0.000(3) 0.006(3) 0.009(3) C16 0.023(4) 0.025(3) 0.023(4) 0.005(3) 0.008(3) 0.009(3) C17 0.021(4) 0.021(3) 0.021(4) 0.005(3) 0.002(3) 0.005(3) C18 0.036(4) 0.023(3) 0.028(4) 0.009(3) 0.010(3) 0.009(3) C19 0.035(4) 0.043(4) 0.030(4) 0.003(3) 0.015(3) 0.015(3) C20 0.035(4) 0.039(4) 0.027(4) -0.015(3) 0.001(3) 0.020(3) C21 0.027(4) 0.019(3) 0.043(4) -0.004(3) 0.008(3) 0.004(3) C22 0.026(4) 0.024(4) 0.026(4) -0.003(3) 0.006(3) 0.009(3) C23 0.017(4) 0.024(3) 0.039(4) 0.006(3) -0.002(3) 0.009(3) C24 0.049(5) 0.040(4) 0.034(4) 0.009(3) 0.020(4) 0.025(4) C25 0.015(4) 0.019(3) 0.037(4) -0.002(3) 0.002(3) -0.003(3) C26 0.058(5) 0.042(4) 0.030(4) 0.021(3) 0.020(4) 0.040(4) C27 0.022(4) 0.030(4) 0.029(4) -0.001(3) 0.003(3) 0.010(3) C28 0.030(4) 0.032(4) 0.029(4) 0.003(3) 0.007(3) 0.015(3) C29 0.022(4) 0.023(3) 0.012(3) 0.000(3) 0.000(3) 0.009(3) C30 0.021(3) 0.013(3) 0.026(4) -0.001(3) 0.006(3) 0.003(3) C31 0.024(4) 0.022(3) 0.027(4) 0.010(3) 0.007(3) 0.014(3) C32 0.028(4) 0.024(3) 0.015(3) 0.002(3) 0.003(3) 0.015(3) C33 0.031(4) 0.023(3) 0.025(4) 0.011(3) 0.015(3) 0.012(3) C34 0.030(4) 0.021(3) 0.026(4) 0.006(3) 0.003(3) 0.017(3) C35 0.046(5) 0.029(4) 0.048(5) 0.000(4) 0.012(4) 0.004(4) C36 0.038(5) 0.052(5) 0.128(8) 0.019(5) 0.035(5) 0.028(4) C37 0.068(6) 0.040(4) 0.043(5) 0.003(4) 0.004(4) 0.023(4) C38 0.049(5) 0.027(4) 0.040(5) 0.011(3) 0.000(4) 0.007(4) C39 0.056(6) 0.037(5) 0.079(6) -0.010(4) -0.020(5) 0.014(4) C40 0.047(5) 0.065(5) 0.085(6) 0.014(5) 0.025(5) 0.032(4) N1 0.022(3) 0.016(3) 0.021(3) 0.011(2) 0.001(2) 0.007(2) N2 0.020(3) 0.013(2) 0.017(3) 0.002(2) 0.003(2) 0.002(2) N3 0.032(3) 0.022(3) 0.042(3) 0.003(2) 0.014(3) 0.011(3) N4 0.031(3) 0.022(3) 0.054(4) 0.000(3) 0.004(3) 0.010(3) O1 0.027(2) 0.017(2) 0.019(2) 0.0092(18) 0.006(2) 0.0040(18) O2 0.020(3) 0.023(2) 0.027(2) 0.0032(19) 0.006(2) 0.004(2) O3 0.028(2) 0.011(2) 0.027(2) 0.0026(18) 0.008(2) 0.0000(18) O4 0.034(3) 0.016(2) 0.029(3) -0.0081(19) 0.013(2) -0.0018(19) O5 0.060(4) 0.059(4) 0.090(4) 0.011(3) 0.041(3) 0.004(3) O6 0.089(4) 0.061(4) 0.064(4) 0.027(3) 0.031(4) 0.021(3) S1 0.0226(9) 0.0154(8) 0.0191(9) 0.0057(6) 0.0027(7) 0.0044(7) S2 0.0235(9) 0.0176(8) 0.0241(9) -0.0013(7) 0.0067(7) 0.0042(7) Zn1 0.0193(4) 0.0117(4) 0.0206(4) 0.0046(3) 0.0069(3) 0.0079(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O2 1.225(7) . ? C1 O1 1.296(6) . ? C1 C2 1.485(7) . ? C2 C3 1.369(7) . ? C2 S1 1.728(6) . ? C3 C4 1.436(7) . ? C3 H3 0.9500 . ? C4 C5 1.363(7) . ? C4 C11 1.478(7) . ? C5 C6 1.482(7) . ? C5 S1 1.731(5) . ? C6 C7 1.376(7) . ? C6 S2 1.725(5) . ? C7 C8 1.418(7) . ? C7 C17 1.483(7) . ? C8 C9 1.361(7) . ? C8 H8 0.9500 . ? C9 C10 1.485(7) 1_665 ? C9 S2 1.711(5) . ? C10 O4 1.244(6) . ? C10 O3 1.285(6) . ? C10 C9 1.485(7) 1_445 ? C11 C16 1.395(7) . ? C11 C12 1.401(7) . ? C12 C13 1.385(8) . ? C12 H12 0.9500 . ? C13 C14 1.380(8) . ? C13 H13 0.9500 . ? C14 C15 1.378(8) . ? C14 H14 0.9500 . ? C15 C16 1.382(7) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C22 1.395(7) . ? C17 C18 1.400(7) . ? C18 C19 1.381(8) . ? C18 H18 0.9500 . ? C19 C20 1.382(8) . ? C19 H19 0.9500 . ? C20 C21 1.389(8) . ? C20 H20 0.9500 . ? C21 C22 1.383(7) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 N1 1.347(7) . ? C23 C25 1.375(7) . ? C23 H23 0.9500 . ? C24 N1 1.323(7) . ? C24 C26 1.397(8) . ? C24 H24 0.9500 . ? C25 C27 1.364(8) . ? C25 H25 0.9500 . ? C26 C27 1.390(8) . ? C26 H26 0.9500 . ? C27 C28 1.475(8) . ? C28 C28 1.325(10) 2_666 ? C28 H28 0.9500 . ? C29 C29 1.335(10) 2_476 ? C29 C30 1.461(7) . ? C29 H29 0.9500 . ? C30 C31 1.385(7) . ? C30 C32 1.387(7) . ? C31 C33 1.377(7) . ? C31 H31 0.9500 . ? C32 C34 1.376(7) . ? C32 H32 0.9500 . ? C33 N2 1.347(7) . ? C33 H33 0.9500 . ? C34 N2 1.343(7) . ? C34 H34 0.9500 . ? C35 O5 1.225(7) . ? C35 N3 1.335(8) . ? C35 H35 0.9500 . ? C36 N3 1.435(7) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 N3 1.438(7) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 O6 1.243(7) . ? C38 N4 1.323(8) . ? C38 H38 0.9500 . ? C39 N4 1.409(8) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 N4 1.463(8) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? N1 Zn1 2.050(4) . ? N2 Zn1 2.011(4) . ? O1 Zn1 1.969(3) . ? O3 Zn1 1.962(4) . ? 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 O2 C1 O1 125.1(5) . . ? O2 C1 C2 121.1(5) . . ? O1 C1 C2 113.8(5) . . ? C3 C2 C1 128.4(5) . . ? C3 C2 S1 111.3(4) . . ? C1 C2 S1 120.2(4) . . ? C2 C3 C4 113.3(5) . . ? C2 C3 H3 123.4 . . ? C4 C3 H3 123.4 . . ? C5 C4 C3 111.5(5) . . ? C5 C4 C11 125.6(5) . . ? C3 C4 C11 122.8(5) . . ? C4 C5 C6 128.3(4) . . ? C4 C5 S1 112.5(4) . . ? C6 C5 S1 119.0(4) . . ? C7 C6 C5 130.6(5) . . ? C7 C6 S2 112.3(4) . . ? C5 C6 S2 116.9(4) . . ? C6 C7 C8 110.6(5) . . ? C6 C7 C17 125.9(5) . . ? C8 C7 C17 123.6(5) . . ? C9 C8 C7 114.2(5) . . ? C9 C8 H8 122.9 . . ? C7 C8 H8 122.9 . . ? C8 C9 C10 129.9(5) . 1_665 ? C8 C9 S2 111.3(4) . . ? C10 C9 S2 118.7(4) 1_665 . ? O4 C10 O3 124.4(5) . . ? O4 C10 C9 119.7(5) . 1_445 ? O3 C10 C9 116.0(5) . 1_445 ? C16 C11 C12 118.3(5) . . ? C16 C11 C4 120.6(5) . . ? C12 C11 C4 121.1(5) . . ? C13 C12 C11 120.4(6) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C14 C13 C12 120.4(6) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C15 C14 C13 119.8(6) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C16 120.3(6) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C15 C16 C11 120.7(5) . . ? C15 C16 H16 119.6 . . ? C11 C16 H16 119.6 . . ? C22 C17 C18 117.8(5) . . ? C22 C17 C7 121.6(5) . . ? C18 C17 C7 120.3(5) . . ? C19 C18 C17 121.0(5) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C18 C19 C20 120.5(6) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C19 C20 C21 119.3(5) . . ? C19 C20 H20 120.3 . . ? C21 C20 H20 120.3 . . ? C22 C21 C20 120.2(5) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C17 121.2(5) . . ? C21 C22 H22 119.4 . . ? C17 C22 H22 119.4 . . ? N1 C23 C25 123.7(5) . . ? N1 C23 H23 118.1 . . ? C25 C23 H23 118.1 . . ? N1 C24 C26 123.6(6) . . ? N1 C24 H24 118.2 . . ? C26 C24 H24 118.2 . . ? C27 C25 C23 119.7(6) . . ? C27 C25 H25 120.2 . . ? C23 C25 H25 120.2 . . ? C27 C26 C24 118.8(5) . . ? C27 C26 H26 120.6 . . ? C24 C26 H26 120.6 . . ? C25 C27 C26 117.8(5) . . ? C25 C27 C28 120.0(5) . . ? C26 C27 C28 122.0(5) . . ? C28 C28 C27 125.1(7) 2_666 . ? C28 C28 H28 117.4 2_666 . ? C27 C28 H28 117.4 . . ? C29 C29 C30 125.4(6) 2_476 . ? C29 C29 H29 117.3 2_476 . ? C30 C29 H29 117.3 . . ? C31 C30 C32 116.9(5) . . ? C31 C30 C29 122.9(5) . . ? C32 C30 C29 120.2(5) . . ? C33 C31 C30 119.9(5) . . ? C33 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C34 C32 C30 120.4(5) . . ? C34 C32 H32 119.8 . . ? C30 C32 H32 119.8 . . ? N2 C33 C31 122.9(5) . . ? N2 C33 H33 118.5 . . ? C31 C33 H33 118.5 . . ? N2 C34 C32 122.6(5) . . ? N2 C34 H34 118.7 . . ? C32 C34 H34 118.7 . . ? O5 C35 N3 125.0(7) . . ? O5 C35 H35 117.5 . . ? N3 C35 H35 117.5 . . ? N3 C36 H36A 109.5 . . ? N3 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N3 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N3 C37 H37A 109.5 . . ? N3 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N3 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? O6 C38 N4 123.0(7) . . ? O6 C38 H38 118.5 . . ? N4 C38 H38 118.5 . . ? N4 C39 H39A 109.5 . . ? N4 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N4 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N4 C40 H40A 109.5 . . ? N4 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? N4 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C24 N1 C23 116.4(5) . . ? C24 N1 Zn1 125.8(4) . . ? C23 N1 Zn1 114.7(3) . . ? C34 N2 C33 117.2(5) . . ? C34 N2 Zn1 123.7(4) . . ? C33 N2 Zn1 119.0(4) . . ? C35 N3 C36 121.6(5) . . ? C35 N3 C37 121.4(5) . . ? C36 N3 C37 116.7(5) . . ? C38 N4 C39 122.1(6) . . ? C38 N4 C40 119.6(6) . . ? C39 N4 C40 118.2(6) . . ? C1 O1 Zn1 111.9(3) . . ? C10 O3 Zn1 106.5(3) . . ? C2 S1 C5 91.5(3) . . ? C9 S2 C6 91.5(3) . . ? O3 Zn1 O1 110.94(15) . . ? O3 Zn1 N2 121.98(17) . . ? O1 Zn1 N2 107.80(15) . . ? O3 Zn1 N1 96.91(16) . . ? O1 Zn1 N1 98.10(16) . . ? N2 Zn1 N1 118.46(18) . . ? 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 O2 C1 C2 C3 -15.9(9) . . . . ? O1 C1 C2 C3 164.9(5) . . . . ? O2 C1 C2 S1 159.3(4) . . . . ? O1 C1 C2 S1 -20.0(6) . . . . ? C1 C2 C3 C4 175.0(5) . . . . ? S1 C2 C3 C4 -0.5(6) . . . . ? C2 C3 C4 C5 -0.1(7) . . . . ? C2 C3 C4 C11 -177.2(5) . . . . ? C3 C4 C5 C6 -172.9(5) . . . . ? C11 C4 C5 C6 4.1(9) . . . . ? C3 C4 C5 S1 0.6(6) . . . . ? C11 C4 C5 S1 177.6(4) . . . . ? C4 C5 C6 C7 -62.2(9) . . . . ? S1 C5 C6 C7 124.6(5) . . . . ? C4 C5 C6 S2 113.1(6) . . . . ? S1 C5 C6 S2 -60.0(5) . . . . ? C5 C6 C7 C8 172.2(5) . . . . ? S2 C6 C7 C8 -3.3(6) . . . . ? C5 C6 C7 C17 -9.3(9) . . . . ? S2 C6 C7 C17 175.1(4) . . . . ? C6 C7 C8 C9 2.3(7) . . . . ? C17 C7 C8 C9 -176.2(5) . . . . ? C7 C8 C9 C10 176.9(5) . . . 1_665 ? C7 C8 C9 S2 -0.2(6) . . . . ? C5 C4 C11 C16 136.5(6) . . . . ? C3 C4 C11 C16 -46.8(7) . . . . ? C5 C4 C11 C12 -44.7(8) . . . . ? C3 C4 C11 C12 132.0(6) . . . . ? C16 C11 C12 C13 -1.4(8) . . . . ? C4 C11 C12 C13 179.7(5) . . . . ? C11 C12 C13 C14 1.0(9) . . . . ? C12 C13 C14 C15 -1.0(9) . . . . ? C13 C14 C15 C16 1.5(9) . . . . ? C14 C15 C16 C11 -2.0(9) . . . . ? C12 C11 C16 C15 1.9(8) . . . . ? C4 C11 C16 C15 -179.2(5) . . . . ? C6 C7 C17 C22 -26.6(9) . . . . ? C8 C7 C17 C22 151.7(6) . . . . ? C6 C7 C17 C18 159.1(6) . . . . ? C8 C7 C17 C18 -22.7(8) . . . . ? C22 C17 C18 C19 0.5(9) . . . . ? C7 C17 C18 C19 175.1(5) . . . . ? C17 C18 C19 C20 0.3(9) . . . . ? C18 C19 C20 C21 -0.5(9) . . . . ? C19 C20 C21 C22 -0.1(9) . . . . ? C20 C21 C22 C17 0.9(9) . . . . ? C18 C17 C22 C21 -1.1(9) . . . . ? C7 C17 C22 C21 -175.6(5) . . . . ? N1 C23 C25 C27 1.1(9) . . . . ? N1 C24 C26 C27 -2.2(10) . . . . ? C23 C25 C27 C26 -2.0(9) . . . . ? C23 C25 C27 C28 173.8(5) . . . . ? C24 C26 C27 C25 2.5(9) . . . . ? C24 C26 C27 C28 -173.2(6) . . . . ? C25 C27 C28 C28 -166.5(7) . . . 2_666 ? C26 C27 C28 C28 9.1(12) . . . 2_666 ? C29 C29 C30 C31 12.1(10) 2_476 . . . ? C29 C29 C30 C32 -166.9(7) 2_476 . . . ? C32 C30 C31 C33 2.0(8) . . . . ? C29 C30 C31 C33 -177.1(5) . . . . ? C31 C30 C32 C34 -2.4(8) . . . . ? C29 C30 C32 C34 176.7(5) . . . . ? C30 C31 C33 N2 0.3(9) . . . . ? C30 C32 C34 N2 0.6(9) . . . . ? C26 C24 N1 C23 1.3(9) . . . . ? C26 C24 N1 Zn1 160.4(5) . . . . ? C25 C23 N1 C24 -0.7(8) . . . . ? C25 C23 N1 Zn1 -162.2(5) . . . . ? C32 C34 N2 C33 1.7(8) . . . . ? C32 C34 N2 Zn1 -173.6(4) . . . . ? C31 C33 N2 C34 -2.1(8) . . . . ? C31 C33 N2 Zn1 173.4(4) . . . . ? O5 C35 N3 C36 0.5(11) . . . . ? O5 C35 N3 C37 173.4(6) . . . . ? O6 C38 N4 C39 0.5(10) . . . . ? O6 C38 N4 C40 178.1(6) . . . . ? O2 C1 O1 Zn1 2.9(7) . . . . ? C2 C1 O1 Zn1 -177.9(3) . . . . ? O4 C10 O3 Zn1 5.4(6) . . . . ? C9 C10 O3 Zn1 -174.9(4) 1_445 . . . ? C3 C2 S1 C5 0.7(4) . . . . ? C1 C2 S1 C5 -175.3(4) . . . . ? C4 C5 S1 C2 -0.8(4) . . . . ? C6 C5 S1 C2 173.4(4) . . . . ? C8 C9 S2 C6 -1.4(4) . . . . ? C10 C9 S2 C6 -178.9(4) 1_665 . . . ? C7 C6 S2 C9 2.8(4) . . . . ? C5 C6 S2 C9 -173.5(4) . . . . ? C10 O3 Zn1 O1 -179.4(3) . . . . ? C10 O3 Zn1 N2 -50.7(4) . . . . ? C10 O3 Zn1 N1 79.2(3) . . . . ? C1 O1 Zn1 O3 59.6(4) . . . . ? C1 O1 Zn1 N2 -76.3(4) . . . . ? C1 O1 Zn1 N1 160.2(3) . . . . ? C34 N2 Zn1 O3 102.0(4) . . . . ? C33 N2 Zn1 O3 -73.2(4) . . . . ? C34 N2 Zn1 O1 -128.0(4) . . . . ? C33 N2 Zn1 O1 56.8(4) . . . . ? C34 N2 Zn1 N1 -18.0(5) . . . . ? C33 N2 Zn1 N1 166.8(4) . . . . ? C24 N1 Zn1 O3 -86.6(5) . . . . ? C23 N1 Zn1 O3 72.8(4) . . . . ? C24 N1 Zn1 O1 161.0(5) . . . . ? C23 N1 Zn1 O1 -39.6(4) . . . . ? C24 N1 Zn1 N2 45.7(5) . . . . ? C23 N1 Zn1 N2 -154.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 23.33 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.403 _refine_diff_density_min -0.392 _refine_diff_density_rms 0.100 # sin(theta_max) is low because diffrn_reflns_theta_max is low. This # is due to the poorly diffracting nature of 4. data_5 _database_code_depnum_ccdc_archive 'CCDC 876811' #TrackingRef '- CE-ART--04-2012-025529cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C201 H257 N15 O32 S12 Zn6' _chemical_formula_weight 4172.16 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.138(2) _cell_length_b 39.627(2) _cell_length_c 22.721(2) _cell_angle_alpha 90.00 _cell_angle_beta 121.737(2) _cell_angle_gamma 90.00 _cell_volume 23844(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9854 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 26.31 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.162 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8784 _exptl_absorpt_coefficient_mu 0.761 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.820 _exptl_absorpt_correction_T_max 0.906 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16035 _diffrn_reflns_av_R_equivalents 0.066 _diffrn_reflns_av_sigmaI/netI 0.0628 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 22.72 _reflns_number_total 16035 _reflns_number_gt 10893 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2\s(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^)+(0.0930P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16035 _refine_ls_number_parameters 1385 _refine_ls_number_restraints 1977 _refine_ls_R_factor_all 0.0876 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.1611 _refine_ls_wR_factor_gt 0.1488 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.035 _refine_ls_shift/su_mean 0.007 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 0.57469(19) 0.01076(12) 0.9584(3) 0.0324(12) Uani 1 1 d U . . C2 C 0.6213(2) 0.03182(12) 1.0001(3) 0.0393(13) Uani 1 1 d DU A . C3 C 0.6596(3) 0.02768(15) 1.0641(3) 0.077(2) Uani 1 1 d DU A . H3 H 0.6615 0.0099 1.0921 0.093 Uiso 1 1 calc R . . C4 C 0.6982(2) 0.05299(16) 1.0868(3) 0.088(3) Uani 1 1 d DU . . C5 C 0.68586(19) 0.07620(12) 1.0365(3) 0.0413(14) Uani 1 1 d DU A . C6 C 0.71151(18) 0.10787(12) 1.0411(3) 0.0388(13) Uani 1 1 d U . . C7 C 0.72829(18) 0.12049(13) 1.0003(3) 0.0400(13) Uani 1 1 d U A . C8 C 0.74831(18) 0.15345(12) 1.0220(3) 0.0371(13) Uani 1 1 d U . . H8 H 0.7614 0.1660 1.0005 0.045 Uiso 1 1 calc R A . C9 C 0.74662(18) 0.16503(12) 1.0769(3) 0.0351(13) Uani 1 1 d U A . C10 C 0.76238(18) 0.19785(12) 1.1132(3) 0.0369(13) Uani 1 1 d U . . C11 C 0.3995(2) -0.01516(13) 0.8155(3) 0.0360(13) Uani 1 1 d U . . C12 C 0.35893(18) 0.00999(11) 0.7960(3) 0.0339(12) Uani 1 1 d U . . C13 C 0.3082(2) 0.00528(13) 0.7593(3) 0.0500(15) Uani 1 1 d U . . H13 H 0.2934 -0.0155 0.7405 0.060 Uiso 1 1 calc R . . C14 C 0.27936(19) 0.03485(13) 0.7516(3) 0.0526(16) Uani 1 1 d U . . C15 C 0.31059(18) 0.06207(12) 0.7826(3) 0.0400(13) Uani 1 1 d U . . C16 C 0.29754(17) 0.09696(12) 0.7863(3) 0.0370(13) Uani 1 1 d U B . C17 C 0.27809(19) 0.10996(13) 0.8234(3) 0.0454(14) Uani 1 1 d U . . C18 C 0.27316(18) 0.14577(12) 0.8164(3) 0.0402(14) Uani 1 1 d U B . H18 H 0.2603 0.1588 0.8377 0.048 Uiso 1 1 calc R . . C19 C 0.28885(17) 0.15893(12) 0.7761(3) 0.0351(13) Uani 1 1 d U . . C20 C 0.78759(17) 0.30594(13) 1.2546(3) 0.0356(13) Uani 1 1 d U . . C21 C 0.69397(19) 0.27482(12) 1.0890(3) 0.0366(13) Uani 1 1 d U . . C22 C 0.64509(17) 0.28681(12) 1.0306(3) 0.0367(13) Uani 1 1 d U . . C23 C 0.63560(17) 0.30085(12) 0.9696(3) 0.0400(14) Uani 1 1 d U . . H23 H 0.6605 0.3048 0.9596 0.048 Uiso 1 1 calc R . . C24 C 0.58386(19) 0.30874(12) 0.9235(3) 0.0406(14) Uani 1 1 d U . . C25 C 0.55540(18) 0.29976(12) 0.9506(3) 0.0374(13) Uani 1 1 d U . . C26 C 0.49981(17) 0.30082(12) 0.9181(3) 0.0346(12) Uani 1 1 d U C . C27 C 0.4716(2) 0.31401(14) 0.9427(3) 0.0444(14) Uani 1 1 d U . . C28 C 0.41977(18) 0.30660(13) 0.8991(3) 0.0402(13) Uani 1 1 d U C . H28 H 0.3953 0.3137 0.9080 0.048 Uiso 1 1 calc R . . C29 C 0.40925(17) 0.28776(12) 0.8423(3) 0.0337(12) Uani 1 1 d U . . C30 C 0.85972(18) 0.22536(12) 1.2866(3) 0.0345(13) Uani 1 1 d U . . C31 C 0.50439(17) -0.06221(11) 1.0248(3) 0.0289(12) Uani 1 1 d U . . H31 H 0.5267 -0.0447 1.0492 0.035 Uiso 1 1 calc R . . C32 C 0.45336(19) -0.09008(12) 0.9239(3) 0.0415(14) Uani 1 1 d U . . H32 H 0.4390 -0.0918 0.8763 0.050 Uiso 1 1 calc R . . C33 C 0.49324(17) -0.08528(12) 1.0610(3) 0.0312(12) Uani 1 1 d U . . H33 H 0.5075 -0.0828 1.1084 0.037 Uiso 1 1 calc R . . C34 C 0.4415(2) -0.11410(13) 0.9555(3) 0.0472(15) Uani 1 1 d U . . H34 H 0.4206 -0.1320 0.9300 0.057 Uiso 1 1 calc R . . C35 C 0.46094(17) -0.11187(11) 1.0264(3) 0.0307(12) Uani 1 1 d U . . C36 C 0.44651(17) -0.13482(12) 1.0625(3) 0.0355(13) Uani 1 1 d U . . H36 H 0.4586 -0.1305 1.1089 0.043 Uiso 1 1 calc R . . C37 C 0.41705(17) -0.16175(12) 1.0336(3) 0.0363(13) Uani 1 1 d U . . H37 H 0.4099 -0.1684 0.9901 0.044 Uiso 1 1 calc R . . C38 C 0.39505(18) -0.18164(12) 1.0661(3) 0.0378(13) Uani 1 1 d U . . C39 C 0.4064(2) -0.17667(15) 1.1330(3) 0.0595(18) Uani 1 1 d U . . H39 H 0.4319 -0.1617 1.1620 0.071 Uiso 1 1 calc R . . C40 C 0.35862(17) -0.20583(12) 1.0274(3) 0.0347(12) Uani 1 1 d U . . H40 H 0.3510 -0.2112 0.9831 0.042 Uiso 1 1 calc R . . C41 C 0.8802(2) 0.30625(15) 1.1568(3) 0.0586(18) Uani 1 1 d U . . H41 H 0.8882 0.3101 1.2019 0.070 Uiso 1 1 calc R . . C42 C 0.83409(18) 0.27828(12) 1.0547(3) 0.0356(13) Uani 1 1 d U . . H42 H 0.8095 0.2624 1.0275 0.043 Uiso 1 1 calc R . . C43 C 0.6950(2) 0.22552(15) 1.2928(3) 0.0614(18) Uani 1 1 d U . . H43 H 0.6983 0.2487 1.3009 0.074 Uiso 1 1 calc R . . C44 C 0.7100(3) 0.17931(16) 1.2482(4) 0.075(2) Uani 1 1 d U . . H44 H 0.7247 0.1694 1.2260 0.090 Uiso 1 1 calc R . . C45 C 0.6701(2) 0.20734(15) 1.3164(4) 0.0676(19) Uani 1 1 d U . . H45 H 0.6589 0.2178 1.3426 0.081 Uiso 1 1 calc R . . C46 C 0.6837(3) 0.15856(16) 1.2689(4) 0.072(2) Uani 1 1 d U . . H46 H 0.6812 0.1354 1.2607 0.087 Uiso 1 1 calc R . . C47 C 0.6615(2) 0.17343(15) 1.3016(3) 0.0567(16) Uani 1 1 d U . . C48 C 0.6326(2) 0.15342(15) 1.3236(3) 0.0634(18) Uani 1 1 d U . . H48 H 0.6240 0.1640 1.3526 0.076 Uiso 1 1 calc R . . C49 C 0.6180(2) 0.12258(15) 1.3065(3) 0.0579(17) Uani 1 1 d U . . H49 H 0.6272 0.1118 1.2784 0.070 Uiso 1 1 calc R . . C50 C 0.5878(2) 0.10272(13) 1.3276(3) 0.0450(14) Uani 1 1 d U . . C51 C 0.57518(18) 0.07015(13) 1.3044(3) 0.0389(13) Uani 1 1 d U . . H51 H 0.5841 0.0612 1.2744 0.047 Uiso 1 1 calc R . . C52 C 0.5742(2) 0.11463(14) 1.3726(3) 0.0576(17) Uani 1 1 d U . . H52 H 0.5823 0.1365 1.3897 0.069 Uiso 1 1 calc R . . C53 C 0.54902(17) -0.05085(12) 0.8260(3) 0.0326(12) Uani 1 1 d U . . H53 H 0.5407 -0.0288 0.8099 0.039 Uiso 1 1 calc R . . C54 C 0.5487(2) -0.09380(13) 0.8918(3) 0.0503(16) Uani 1 1 d U . . H54 H 0.5402 -0.1021 0.9227 0.060 Uiso 1 1 calc R . . C55 C 0.7537(3) 0.0479(3) 1.1469(5) 0.068(4) Uani 0.577(8) 1 d PDU A 1 H55A H 0.7699 0.0699 1.1585 0.081 Uiso 0.577(8) 1 calc PR A 1 H55B H 0.7531 0.0401 1.1869 0.081 Uiso 0.577(8) 1 calc PR A 1 C56 C 0.7875(3) 0.0237(3) 1.1361(7) 0.089(6) Uani 0.577(8) 1 d PDU A 1 H56A H 0.7716 0.0016 1.1246 0.107 Uiso 0.577(8) 1 calc PR A 1 H56B H 0.7887 0.0315 1.0965 0.107 Uiso 0.577(8) 1 calc PR A 1 C57 C 0.8417(3) 0.0198(4) 1.1975(6) 0.098(5) Uani 0.577(8) 1 d PDU A 1 H57A H 0.8421 0.0029 1.2286 0.118 Uiso 0.577(8) 1 calc PR A 1 H57B H 0.8524 0.0410 1.2225 0.118 Uiso 0.577(8) 1 calc PR A 1 C58 C 0.8802(6) 0.0097(8) 1.1778(10) 0.258(12) Uani 0.577(8) 1 d PDU A 1 H58A H 0.8824 0.0277 1.1505 0.310 Uiso 0.577(8) 1 calc PR A 1 H58B H 0.8681 -0.0104 1.1490 0.310 Uiso 0.577(8) 1 calc PR A 1 C59 C 0.9334(6) 0.0026(8) 1.2409(13) 0.313(15) Uani 0.577(8) 1 d PDU A 1 H59A H 0.9567 0.0192 1.2418 0.376 Uiso 0.577(8) 1 calc PR A 1 H59B H 0.9326 0.0054 1.2827 0.376 Uiso 0.577(8) 1 calc PR A 1 C60 C 0.9536(11) -0.0329(8) 1.241(2) 0.43(2) Uani 0.577(8) 1 d PDU A 1 H60A H 0.9874 -0.0351 1.2805 0.643 Uiso 0.577(8) 1 calc PR A 1 H60B H 0.9536 -0.0363 1.1995 0.643 Uiso 0.577(8) 1 calc PR A 1 H60C H 0.9323 -0.0495 1.2442 0.643 Uiso 0.577(8) 1 calc PR A 1 C61 C 0.7272(2) 0.10244(14) 0.9424(3) 0.0500(15) Uani 1 1 d U . . H61A H 0.7014 0.1126 0.8991 0.060 Uiso 1 1 calc R A . H61B H 0.7175 0.0792 0.9425 0.060 Uiso 1 1 calc R . . C62 C 0.7769(2) 0.10284(15) 0.9451(3) 0.0566(16) Uani 1 1 d U A . H62A H 0.7723 0.0917 0.9041 0.068 Uiso 1 1 calc R . . H62B H 0.7864 0.1261 0.9441 0.068 Uiso 1 1 calc R . . C63 C 0.8195(2) 0.08573(16) 1.0083(4) 0.0676(19) Uani 1 1 d U . . H63A H 0.8126 0.0617 1.0057 0.081 Uiso 1 1 calc R A . H63B H 0.8211 0.0945 1.0492 0.081 Uiso 1 1 calc R . . C64 C 0.8702(3) 0.0910(2) 1.0152(5) 0.112(3) Uani 1 1 d U A . H64A H 0.8768 0.1150 1.0168 0.135 Uiso 1 1 calc R . . H64B H 0.8688 0.0818 0.9747 0.135 Uiso 1 1 calc R . . C65 C 0.9143(3) 0.0741(3) 1.0806(6) 0.163(5) Uani 1 1 d U . . H65A H 0.9077 0.0501 1.0790 0.196 Uiso 1 1 calc R A . H65B H 0.9156 0.0832 1.1212 0.196 Uiso 1 1 calc R . . C66 C 0.9664(4) 0.0795(4) 1.0881(9) 0.281(10) Uani 1 1 d U A . H66A H 0.9922 0.0687 1.1295 0.422 Uiso 1 1 calc R . . H66B H 0.9734 0.1032 1.0905 0.422 Uiso 1 1 calc R . . H66C H 0.9657 0.0700 1.0488 0.422 Uiso 1 1 calc R . . C67 C 0.2219(2) 0.03635(17) 0.7111(5) 0.091(3) Uani 1 1 d U . . H67A H 0.2113 0.0596 0.6980 0.109 Uiso 1 1 calc R . . H67B H 0.2100 0.0290 0.7409 0.109 Uiso 1 1 calc R . . C68 C 0.1971(2) 0.0144(2) 0.6458(4) 0.102(3) Uani 1 1 d U . . H68A H 0.2072 0.0226 0.6146 0.122 Uiso 1 1 calc R . . H68B H 0.2093 -0.0086 0.6585 0.122 Uiso 1 1 calc R . . C69 C 0.1400(3) 0.0142(3) 0.6082(5) 0.132(4) Uani 1 1 d U . . H69A H 0.1270 0.0364 0.5890 0.159 Uiso 1 1 calc R . . H69B H 0.1295 0.0089 0.6404 0.159 Uiso 1 1 calc R . . C70 C 0.1176(4) -0.0133(4) 0.5471(6) 0.194(6) Uani 1 1 d U . . H70A H 0.1239 -0.0064 0.5113 0.232 Uiso 1 1 calc R . . H70B H 0.1333 -0.0350 0.5649 0.232 Uiso 1 1 calc R . . C71 C 0.0606(5) -0.0155(5) 0.5175(9) 0.260(8) Uani 1 1 d U . . H71A H 0.0448 0.0063 0.5002 0.311 Uiso 1 1 calc R . . H71B H 0.0541 -0.0229 0.5528 0.311 Uiso 1 1 calc R . . C72 C 0.0393(7) -0.0424(6) 0.4559(10) 0.368(14) Uani 1 1 d U . . H72A H 0.0034 -0.0443 0.4346 0.551 Uiso 1 1 calc R . . H72B H 0.0548 -0.0639 0.4741 0.551 Uiso 1 1 calc R . . H72C H 0.0469 -0.0350 0.4222 0.551 Uiso 1 1 calc R . . C73 C 0.2696(7) 0.0897(5) 0.8783(5) 0.055(4) Uani 0.619(7) 1 d PDU B 1 H73A H 0.2336 0.0889 0.8607 0.066 Uiso 0.619(7) 1 calc PR B 1 H73B H 0.2812 0.0667 0.8817 0.066 Uiso 0.619(7) 1 calc PR B 1 C74 C 0.2967(4) 0.1053(2) 0.9510(5) 0.083(4) Uani 0.619(7) 1 d PDU B 1 H74A H 0.3329 0.1037 0.9712 0.099 Uiso 0.619(7) 1 calc PR B 1 H74B H 0.2879 0.1290 0.9475 0.099 Uiso 0.619(7) 1 calc PR B 1 C75 C 0.2828(5) 0.0877(2) 0.9989(5) 0.095(4) Uani 0.619(7) 1 d PDU B 1 H75A H 0.2956 0.1011 1.0406 0.114 Uiso 0.619(7) 1 calc PR B 1 H75B H 0.2464 0.0868 0.9760 0.114 Uiso 0.619(7) 1 calc PR B 1 C76 C 0.3039(6) 0.0521(3) 1.0187(7) 0.086(6) Uani 0.619(7) 1 d PDU B 1 H76A H 0.3402 0.0527 1.0397 0.103 Uiso 0.619(7) 1 calc PR B 1 H76B H 0.2896 0.0382 0.9776 0.103 Uiso 0.619(7) 1 calc PR B 1 C77 C 0.2911(4) 0.0366(3) 1.0705(6) 0.079(4) Uani 0.619(7) 1 d PDU B 1 H77A H 0.3062 0.0502 1.1122 0.095 Uiso 0.619(7) 1 calc PR B 1 H77B H 0.2548 0.0367 1.0500 0.095 Uiso 0.619(7) 1 calc PR B 1 C78 C 0.3110(6) 0.0003(3) 1.0891(7) 0.068(4) Uani 0.619(7) 1 d PDU B 1 H78A H 0.3025 -0.0089 1.1208 0.102 Uiso 0.619(7) 1 calc PR B 1 H78B H 0.3470 0.0003 1.1103 0.102 Uiso 0.619(7) 1 calc PR B 1 H78C H 0.2958 -0.0132 1.0479 0.102 Uiso 0.619(7) 1 calc PR B 1 C79 C 0.56409(19) 0.32487(14) 0.8535(3) 0.0487(15) Uani 1 1 d U . . H79A H 0.5444 0.3083 0.8179 0.058 Uiso 1 1 calc R . . H79B H 0.5416 0.3432 0.8479 0.058 Uiso 1 1 calc R . . C80 C 0.60470(19) 0.33846(13) 0.8427(3) 0.0453(14) Uani 1 1 d U . . H80A H 0.6248 0.3197 0.8429 0.054 Uiso 1 1 calc R . . H80B H 0.6268 0.3530 0.8813 0.054 Uiso 1 1 calc R . . C81 C 0.5848(2) 0.35823(14) 0.7757(3) 0.0506(16) Uani 1 1 d U . . H81A H 0.5599 0.3446 0.7373 0.061 Uiso 1 1 calc R . . H81B H 0.5680 0.3785 0.7776 0.061 Uiso 1 1 calc R . . C82 C 0.6260(2) 0.36815(16) 0.7625(3) 0.0646(18) Uani 1 1 d U . . H82A H 0.6508 0.3818 0.8010 0.078 Uiso 1 1 calc R . . H82B H 0.6429 0.3479 0.7610 0.078 Uiso 1 1 calc R . . C83 C 0.6070(3) 0.38769(19) 0.6960(4) 0.083(2) Uani 1 1 d U . . H83A H 0.5956 0.4098 0.7003 0.100 Uiso 1 1 calc R . . H83B H 0.5784 0.3759 0.6582 0.100 Uiso 1 1 calc R . . C84 C 0.6495(3) 0.3917(2) 0.6793(4) 0.135(4) Uani 1 1 d U . . H84A H 0.6794 0.4006 0.7191 0.203 Uiso 1 1 calc R . . H84B H 0.6383 0.4069 0.6411 0.203 Uiso 1 1 calc R . . H84C H 0.6569 0.3701 0.6676 0.203 Uiso 1 1 calc R . . C85 C 0.492(2) 0.3355(5) 1.0045(15) 0.067(2) Uani 0.525(6) 1 d PDU C 1 H85A H 0.4748 0.3572 0.9909 0.080 Uiso 0.525(6) 1 calc PR C 1 H85B H 0.5273 0.3393 1.0233 0.080 Uiso 0.525(6) 1 calc PR C 1 C86 C 0.4849(5) 0.3204(3) 1.0623(6) 0.088(5) Uani 0.525(6) 1 d PDU C 1 H86A H 0.5069 0.3009 1.0806 0.106 Uiso 0.525(6) 1 calc PR C 1 H86B H 0.4505 0.3121 1.0400 0.106 Uiso 0.525(6) 1 calc PR C 1 C87 C 0.4946(6) 0.3422(4) 1.1258(6) 0.123(6) Uani 0.525(6) 1 d PDU C 1 H87A H 0.5272 0.3529 1.1442 0.148 Uiso 0.525(6) 1 calc PR C 1 H87B H 0.4696 0.3601 1.1076 0.148 Uiso 0.525(6) 1 calc PR C 1 C88 C 0.4943(8) 0.3266(4) 1.1884(7) 0.126(6) Uani 0.525(6) 1 d PDU C 1 H88A H 0.5211 0.3100 1.2086 0.152 Uiso 0.525(6) 1 calc PR C 1 H88B H 0.4628 0.3143 1.1695 0.152 Uiso 0.525(6) 1 calc PR C 1 C89 C 0.5000 0.3483(5) 1.2500 0.266(12) Uani 0.525(6) 2 d SPDU C 1 H89C H 0.4815 0.3691 1.2302 0.320 Uiso 0.525(6) 1 calc PR C 1 H89D H 0.4825 0.3363 1.2685 0.320 Uiso 0.525(6) 1 calc PR C 1 C90 C 0.5529(7) 0.3584(17) 1.313(2) 0.67(4) Uani 0.525(6) 1 d PDU C 1 H90D H 0.5486 0.3735 1.3426 1.010 Uiso 0.525(6) 1 calc PR C 1 H90E H 0.5721 0.3694 1.2966 1.010 Uiso 0.525(6) 1 calc PR C 1 H90F H 0.5704 0.3385 1.3384 1.010 Uiso 0.525(6) 1 calc PR C 1 C91 C 0.4704(4) 0.2068(2) 0.9680(4) 0.133(4) Uani 1 1 d U . . H91A H 0.4789 0.2234 0.9449 0.200 Uiso 1 1 calc R . . H91B H 0.5007 0.1976 1.0065 0.200 Uiso 1 1 calc R . . H91C H 0.4508 0.2173 0.9844 0.200 Uiso 1 1 calc R . . N5 N 0.4406(2) 0.17952(13) 0.9191(3) 0.0670(15) Uani 1 1 d U . . C92 C 0.4341(2) 0.18182(17) 0.8529(3) 0.0670(19) Uani 1 1 d U . . H92A H 0.4171 0.1620 0.8267 0.101 Uiso 1 1 calc R . . H92B H 0.4665 0.1837 0.8576 0.101 Uiso 1 1 calc R . . H92C H 0.4142 0.2014 0.8295 0.101 Uiso 1 1 calc R . . C93 C 0.4240(3) 0.15393(18) 0.9381(4) 0.0686(19) Uani 1 1 d U . . H93 H 0.4086 0.1365 0.9062 0.082 Uiso 1 1 calc R . . O13 O 0.4267(2) 0.15063(13) 0.9937(3) 0.1015(17) Uani 1 1 d U . . C94 C 0.5452(4) 0.2381(2) 0.2048(6) 0.152(5) Uani 1 1 d U . . H94A H 0.5205 0.2326 0.2163 0.228 Uiso 1 1 calc R . . H94B H 0.5354 0.2584 0.1779 0.228 Uiso 1 1 calc R . . H94C H 0.5775 0.2413 0.2465 0.228 Uiso 1 1 calc R . . C95 C 0.5231(4) 0.1783(2) 0.1548(5) 0.149(4) Uani 1 1 d U . . H95A H 0.5009 0.1800 0.1721 0.223 Uiso 1 1 calc R . . H95B H 0.5476 0.1610 0.1795 0.223 Uiso 1 1 calc R . . H95C H 0.5038 0.1729 0.1064 0.223 Uiso 1 1 calc R . . C96 C 0.5810(4) 0.2138(2) 0.1427(4) 0.103(3) Uani 1 1 d U . . H96 H 0.5981 0.2342 0.1511 0.124 Uiso 1 1 calc R . . C97 C 0.1592(3) 0.1400(2) 0.6494(4) 0.100(3) Uani 1 1 d U . . H97A H 0.1749 0.1585 0.6405 0.150 Uiso 1 1 calc R . . H97B H 0.1299 0.1329 0.6068 0.150 Uiso 1 1 calc R . . H97C H 0.1827 0.1216 0.6692 0.150 Uiso 1 1 calc R . . C98 C 0.1308(4) 0.1247(3) 0.7335(6) 0.167(5) Uani 1 1 d U . . H98A H 0.1298 0.1027 0.7151 0.251 Uiso 1 1 calc R . . H98B H 0.0983 0.1300 0.7263 0.251 Uiso 1 1 calc R . . H98C H 0.1557 0.1250 0.7821 0.251 Uiso 1 1 calc R . . C99 C 0.1479(3) 0.1832(3) 0.7146(5) 0.107(3) Uani 1 1 d U . . H99 H 0.1586 0.1986 0.6941 0.128 Uiso 1 1 calc R . . C103 C 0.4661(4) 0.0612(3) 0.7433(9) 0.038(5) Uani 0.50 1 d PDU . . H10A H 0.4459 0.0803 0.7399 0.056 Uiso 0.50 1 calc PR . . H10B H 0.4719 0.0472 0.7813 0.056 Uiso 0.50 1 calc PR . . H10C H 0.4488 0.0484 0.7011 0.056 Uiso 0.50 1 calc PR . . C104 C 0.5235(4) 0.1054(3) 0.7595(5) 0.043(3) Uani 0.50 1 d PDU . . H104 H 0.5544 0.1117 0.7660 0.052 Uiso 0.50 1 calc PR . . C105 C 0.5486(6) 0.0466(3) 0.7624(9) 0.041(4) Uani 0.50 1 d PDU . . H10D H 0.5784 0.0568 0.7679 0.062 Uiso 0.50 1 calc PR . . H10E H 0.5331 0.0324 0.7221 0.062 Uiso 0.50 1 calc PR . . H10F H 0.5575 0.0332 0.8025 0.062 Uiso 0.50 1 calc PR . . N1 N 0.48431(13) -0.06413(9) 0.9566(2) 0.0258(9) Uani 1 1 d U . . N2 N 0.84341(14) 0.28419(10) 1.1175(2) 0.0338(10) Uani 1 1 d U . . N3 N 0.71478(15) 0.21223(11) 1.2589(2) 0.0411(11) Uani 1 1 d U A . N4 N 0.53517(14) -0.06220(9) 0.8687(2) 0.0298(10) Uani 1 1 d U . . N6 N 0.5487(3) 0.21054(18) 0.1647(4) 0.101(2) Uani 1 1 d U . . N7 N 0.1445(2) 0.15060(19) 0.6970(4) 0.094(2) Uani 1 1 d U . . O1 O 0.54933(12) 0.01468(8) 0.8946(2) 0.0390(9) Uani 1 1 d U . . O2 O 0.56413(13) -0.00963(8) 0.99058(19) 0.0422(9) Uani 1 1 d U . . O3 O 0.78592(12) 0.21778(8) 1.09740(17) 0.0378(9) Uani 1 1 d U A . O4 O 0.75051(12) 0.20322(8) 1.15752(18) 0.0381(9) Uani 1 1 d U A . O5 O 0.44425(12) -0.00283(7) 0.85170(18) 0.0363(9) Uani 1 1 d U . . O6 O 0.38901(13) -0.04475(9) 0.79771(19) 0.0451(9) Uani 1 1 d U . . O7 O 0.80558(12) 0.30038(8) 1.21709(18) 0.0396(9) Uani 1 1 d U . . O8 O 0.76755(12) 0.28423(8) 1.27326(18) 0.0426(9) Uani 1 1 d U A . O9 O 0.73196(12) 0.27769(8) 1.08359(18) 0.0422(9) Uani 1 1 d U . . O10 O 0.69364(12) 0.26239(8) 1.13973(18) 0.0407(9) Uani 1 1 d U A . O11 O 0.85981(11) 0.23923(8) 1.23665(17) 0.0359(8) Uani 1 1 d U . . O12 O 0.82266(12) 0.22176(9) 1.29424(17) 0.0403(9) Uani 1 1 d U A . O14 O 0.1372(3) 0.1941(2) 0.7578(5) 0.169(3) Uani 1 1 d U . . O15 O 0.5899(2) 0.19105(15) 0.1114(3) 0.115(2) Uani 1 1 d U . . S1 S 0.63047(5) 0.06610(3) 0.96213(7) 0.0373(3) Uani 1 1 d DU . . S2 S 0.71906(5) 0.13629(3) 1.10323(7) 0.0403(4) Uani 1 1 d U A . S3 S 0.37336(5) 0.05117(3) 0.82121(7) 0.0368(3) Uani 1 1 d U . . S4 S 0.31088(5) 0.12807(3) 0.74543(7) 0.0349(3) Uani 1 1 d U B . S5 S 0.59099(5) 0.28196(3) 1.03168(7) 0.0392(3) Uani 1 1 d U . . S6 S 0.46290(4) 0.27906(3) 0.84198(7) 0.0334(3) Uani 1 1 d U C . Zn1 Zn 0.50362(2) -0.030389(12) 0.90658(3) 0.02616(16) Uani 1 1 d U . . Zn2 Zn 0.752335(19) 0.238737(14) 1.22454(3) 0.03117(17) Uani 1 1 d U . . Zn3 Zn 0.803071(19) 0.262179(13) 1.15207(3) 0.02997(17) Uani 1 1 d U A . C73B C 0.2591(8) 0.0897(8) 0.8526(10) 0.056(6) Uani 0.381(7) 1 d PDU B 2 H73C H 0.2433 0.0703 0.8228 0.068 Uiso 0.381(7) 1 calc PR B 2 H73D H 0.2331 0.1019 0.8550 0.068 Uiso 0.381(7) 1 calc PR B 2 C74B C 0.2987(6) 0.0771(3) 0.9255(8) 0.051(4) Uani 0.381(7) 1 d PDU B 2 H74C H 0.3264 0.0667 0.9243 0.061 Uiso 0.381(7) 1 calc PR B 2 H74D H 0.3120 0.0962 0.9567 0.061 Uiso 0.381(7) 1 calc PR B 2 C75B C 0.2769(5) 0.0516(4) 0.9536(7) 0.060(5) Uani 0.381(7) 1 d PDU B 2 H75C H 0.2478 0.0615 0.9519 0.072 Uiso 0.381(7) 1 calc PR B 2 H75D H 0.2654 0.0319 0.9238 0.072 Uiso 0.381(7) 1 calc PR B 2 C76B C 0.3147(7) 0.0404(5) 1.0276(7) 0.058(5) Uani 0.381(7) 1 d PDU B 2 H76C H 0.3214 0.0592 1.0587 0.070 Uiso 0.381(7) 1 calc PR B 2 H76D H 0.3462 0.0343 1.0313 0.070 Uiso 0.381(7) 1 calc PR B 2 C77B C 0.2956(7) 0.0103(4) 1.0500(8) 0.062(5) Uani 0.381(7) 1 d PDU B 2 H77C H 0.2630 0.0159 1.0434 0.074 Uiso 0.381(7) 1 calc PR B 2 H77D H 0.2909 -0.0089 1.0206 0.074 Uiso 0.381(7) 1 calc PR B 2 C78B C 0.3318(8) 0.0003(6) 1.1257(9) 0.068(7) Uani 0.381(7) 1 d PDU B 2 H78D H 0.3175 -0.0180 1.1375 0.101 Uiso 0.381(7) 1 calc PR B 2 H78E H 0.3372 0.0192 1.1551 0.101 Uiso 0.381(7) 1 calc PR B 2 H78F H 0.3635 -0.0067 1.1319 0.101 Uiso 0.381(7) 1 calc PR B 2 C85B C 0.494(2) 0.3343(5) 1.0121(16) 0.067(2) Uani 0.475(6) 1 d PDU C 2 H85C H 0.4742 0.3297 1.0331 0.080 Uiso 0.475(6) 1 calc PR C 2 H85D H 0.5284 0.3274 1.0443 0.080 Uiso 0.475(6) 1 calc PR C 2 C86B C 0.4923(10) 0.3724(4) 0.9972(8) 0.188(11) Uani 0.475(6) 1 d PDU C 2 H86C H 0.4576 0.3794 0.9655 0.225 Uiso 0.475(6) 1 calc PR C 2 H86D H 0.5114 0.3769 0.9754 0.225 Uiso 0.475(6) 1 calc PR C 2 C87B C 0.5149(11) 0.3931(4) 1.0652(9) 0.213(13) Uani 0.475(6) 1 d PDU C 2 H87C H 0.4957 0.3887 1.0870 0.255 Uiso 0.475(6) 1 calc PR C 2 H87D H 0.5495 0.3862 1.0969 0.255 Uiso 0.475(6) 1 calc PR C 2 C88B C 0.5136(17) 0.4314(4) 1.0509(11) 0.307(18) Uani 0.475(6) 1 d PDU C 2 H88C H 0.4793 0.4380 1.0162 0.369 Uiso 0.475(6) 1 calc PR C 2 H88D H 0.5349 0.4361 1.0326 0.369 Uiso 0.475(6) 1 calc PR C 2 C89B C 0.5318(17) 0.4523(7) 1.1173(13) 0.34(2) Uani 0.475(6) 1 d PDU C 2 H89A H 0.5624 0.4424 1.1551 0.405 Uiso 0.475(6) 1 calc PR C 2 H89B H 0.5063 0.4519 1.1295 0.405 Uiso 0.475(6) 1 calc PR C 2 C90B C 0.5424(19) 0.4895(7) 1.1069(18) 0.37(3) Uani 0.475(6) 1 d PDU C 2 H90A H 0.5473 0.5029 1.1451 0.560 Uiso 0.475(6) 1 calc PR C 2 H90B H 0.5143 0.4981 1.0647 0.560 Uiso 0.475(6) 1 calc PR C 2 H90C H 0.5723 0.4904 1.1046 0.560 Uiso 0.475(6) 1 calc PR C 2 N9 N 0.5133(3) 0.0727(3) 0.7547(8) 0.034(5) Uani 0.50 1 d PDU . . O17 O 0.495(2) 0.12795(17) 0.756(3) 0.051(9) Uani 0.50 1 d PU . . O20 O 0.6818(4) 0.0853(2) 1.2092(6) 0.104(4) Uani 0.50 1 d PU . . C55B C 0.7293(5) 0.0599(3) 1.1681(8) 0.068(5) Uani 0.423(8) 1 d PDU A 2 H55C H 0.7452 0.0819 1.1793 0.081 Uiso 0.423(8) 1 calc PR A 2 H55D H 0.7085 0.0575 1.1880 0.081 Uiso 0.423(8) 1 calc PR A 2 C56B C 0.7685(5) 0.0310(4) 1.1908(7) 0.084(6) Uani 0.423(8) 1 d PDU A 2 H56C H 0.7509 0.0096 1.1761 0.101 Uiso 0.423(8) 1 calc PR A 2 H56D H 0.7896 0.0307 1.2409 0.101 Uiso 0.423(8) 1 calc PR A 2 C57B C 0.8026(6) 0.0349(5) 1.1600(11) 0.104(7) Uani 0.423(8) 1 d PDU A 2 H57C H 0.7868 0.0509 1.1219 0.124 Uiso 0.423(8) 1 calc PR A 2 H57D H 0.8348 0.0443 1.1952 0.124 Uiso 0.423(8) 1 calc PR A 2 C58B C 0.8120(8) 0.0015(7) 1.1337(11) 0.257(14) Uani 0.423(8) 1 d PDU A 2 H58C H 0.7900 -0.0157 1.1342 0.309 Uiso 0.423(8) 1 calc PR A 2 H58D H 0.8027 0.0045 1.0860 0.309 Uiso 0.423(8) 1 calc PR A 2 C59B C 0.8670(8) -0.0113(9) 1.176(2) 0.225(14) Uani 0.423(8) 1 d PDU A 2 H59C H 0.8794 -0.0088 1.2251 0.270 Uiso 0.423(8) 1 calc PR A 2 H59D H 0.8878 0.0026 1.1659 0.270 Uiso 0.423(8) 1 calc PR A 2 C60B C 0.8726(14) -0.0488(10) 1.161(3) 0.44(3) Uani 0.423(8) 1 d PDU A 2 H60D H 0.9077 -0.0546 1.1846 0.653 Uiso 0.423(8) 1 calc PR A 2 H60E H 0.8574 -0.0520 1.1123 0.653 Uiso 0.423(8) 1 calc PR A 2 H60F H 0.8560 -0.0631 1.1775 0.653 Uiso 0.423(8) 1 calc PR A 2 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 0.045(3) 0.018(3) 0.048(4) -0.006(3) 0.034(3) -0.006(2) C2 0.050(3) 0.033(3) 0.042(4) -0.010(3) 0.029(3) -0.014(3) C3 0.115(6) 0.054(4) 0.048(4) 0.005(3) 0.032(4) -0.049(4) C4 0.100(5) 0.065(4) 0.045(4) 0.011(4) 0.001(4) -0.052(4) C5 0.044(3) 0.033(3) 0.039(3) -0.001(3) 0.017(3) -0.017(2) C6 0.039(3) 0.034(3) 0.036(3) 0.001(2) 0.015(3) -0.008(2) C7 0.032(3) 0.049(3) 0.030(3) 0.001(3) 0.009(3) -0.011(2) C8 0.035(3) 0.036(3) 0.035(3) 0.001(3) 0.015(3) -0.019(2) C9 0.033(3) 0.034(3) 0.034(3) 0.003(2) 0.015(3) -0.010(2) C10 0.028(3) 0.034(3) 0.035(3) 0.002(3) 0.006(3) -0.013(2) C11 0.046(3) 0.028(3) 0.048(4) 0.006(3) 0.034(3) 0.010(3) C12 0.036(3) 0.020(3) 0.051(4) -0.001(2) 0.027(3) 0.000(2) C13 0.046(4) 0.035(3) 0.070(4) -0.008(3) 0.032(3) -0.005(3) C14 0.032(3) 0.040(3) 0.081(5) -0.007(3) 0.027(3) 0.001(3) C15 0.033(3) 0.037(3) 0.053(4) 0.004(3) 0.024(3) 0.011(2) C16 0.025(3) 0.037(3) 0.049(4) -0.004(3) 0.019(3) 0.007(2) C17 0.044(3) 0.041(3) 0.059(4) 0.008(3) 0.032(3) 0.013(3) C18 0.042(3) 0.037(3) 0.048(4) 0.007(3) 0.028(3) 0.021(2) C19 0.029(3) 0.033(3) 0.033(3) 0.000(2) 0.009(3) 0.010(2) C20 0.022(3) 0.043(3) 0.026(3) 0.003(3) 0.001(2) -0.011(2) C21 0.036(3) 0.024(3) 0.036(3) -0.004(2) 0.009(3) -0.014(2) C22 0.025(3) 0.028(3) 0.042(4) -0.003(3) 0.007(3) -0.007(2) C23 0.021(3) 0.038(3) 0.043(4) 0.006(3) 0.004(3) -0.007(2) C24 0.038(3) 0.031(3) 0.041(3) 0.000(3) 0.013(3) -0.011(2) C25 0.033(3) 0.032(3) 0.033(3) -0.002(2) 0.008(3) -0.004(2) C26 0.029(3) 0.035(3) 0.028(3) 0.000(2) 0.007(3) -0.004(2) C27 0.042(3) 0.047(3) 0.034(3) -0.012(3) 0.013(3) -0.001(3) C28 0.034(3) 0.043(3) 0.036(3) -0.008(3) 0.013(3) 0.007(2) C29 0.026(3) 0.036(3) 0.036(3) 0.004(3) 0.015(3) 0.007(2) C30 0.029(3) 0.033(3) 0.028(3) -0.005(2) 0.005(3) -0.008(2) C31 0.027(3) 0.023(3) 0.041(3) -0.008(2) 0.021(3) -0.007(2) C32 0.053(3) 0.039(3) 0.027(3) -0.005(3) 0.017(3) -0.026(3) C33 0.031(3) 0.037(3) 0.030(3) -0.003(2) 0.019(2) -0.009(2) C34 0.057(4) 0.041(3) 0.033(3) -0.005(3) 0.016(3) -0.035(3) C35 0.033(3) 0.031(3) 0.032(3) -0.004(2) 0.020(3) -0.011(2) C36 0.033(3) 0.043(3) 0.030(3) 0.001(2) 0.016(3) -0.015(2) C37 0.037(3) 0.043(3) 0.033(3) 0.000(2) 0.021(3) -0.012(2) C38 0.039(3) 0.037(3) 0.031(3) 0.005(2) 0.014(3) -0.016(2) C39 0.063(4) 0.075(4) 0.031(4) -0.012(3) 0.018(3) -0.052(3) C40 0.038(3) 0.033(3) 0.031(3) -0.004(2) 0.017(3) -0.016(2) C41 0.059(4) 0.078(4) 0.031(3) -0.007(3) 0.018(3) -0.052(3) C42 0.030(3) 0.029(3) 0.043(4) -0.001(3) 0.016(3) -0.013(2) C43 0.074(4) 0.049(4) 0.079(5) -0.006(3) 0.053(4) -0.027(3) C44 0.102(5) 0.054(4) 0.103(6) -0.006(4) 0.078(5) -0.026(4) C45 0.095(5) 0.049(4) 0.087(5) -0.016(4) 0.068(5) -0.033(4) C46 0.107(5) 0.051(4) 0.090(5) -0.007(4) 0.073(5) -0.029(4) C47 0.068(4) 0.055(4) 0.071(4) 0.004(3) 0.053(4) -0.015(3) C48 0.087(5) 0.054(4) 0.077(5) 0.000(4) 0.062(4) -0.016(4) C49 0.073(4) 0.056(4) 0.057(4) -0.008(3) 0.043(4) -0.030(3) C50 0.060(4) 0.044(3) 0.048(4) -0.010(3) 0.040(3) -0.023(3) C51 0.045(3) 0.047(3) 0.034(3) -0.005(3) 0.027(3) -0.014(3) C52 0.101(5) 0.033(3) 0.076(5) -0.019(3) 0.071(4) -0.032(3) C53 0.040(3) 0.025(3) 0.042(3) 0.002(2) 0.027(3) 0.003(2) C54 0.081(4) 0.034(3) 0.064(4) 0.011(3) 0.058(4) 0.018(3) C55 0.075(8) 0.055(8) 0.047(7) 0.001(6) 0.014(7) -0.023(6) C56 0.024(7) 0.092(10) 0.096(11) 0.029(8) -0.007(7) -0.007(7) C57 0.019(6) 0.143(11) 0.097(10) 0.053(9) 0.007(6) 0.012(6) C58 0.111(14) 0.32(2) 0.28(2) 0.03(2) 0.061(15) 0.007(17) C59 0.101(15) 0.40(3) 0.37(3) 0.07(3) 0.083(18) 0.122(18) C60 0.28(4) 0.55(5) 0.43(5) 0.13(4) 0.18(4) 0.08(4) C61 0.055(4) 0.050(4) 0.041(4) -0.005(3) 0.023(3) -0.020(3) C62 0.064(4) 0.056(4) 0.056(4) -0.004(3) 0.036(4) -0.014(3) C63 0.074(5) 0.054(4) 0.082(5) -0.016(4) 0.046(4) -0.012(3) C64 0.078(6) 0.109(7) 0.156(9) -0.058(6) 0.066(6) -0.017(5) C65 0.060(6) 0.159(9) 0.197(12) -0.058(9) 0.017(7) 0.013(6) C66 0.067(7) 0.258(15) 0.43(2) -0.190(16) 0.069(11) -0.030(8) C67 0.038(4) 0.064(5) 0.150(8) -0.015(5) 0.036(5) 0.005(3) C68 0.036(4) 0.135(7) 0.100(7) 0.011(6) 0.012(4) -0.007(4) C69 0.059(5) 0.169(9) 0.131(8) -0.005(7) 0.023(6) -0.024(6) C70 0.095(8) 0.278(14) 0.107(9) -0.024(9) -0.016(7) -0.058(9) C71 0.113(10) 0.347(19) 0.217(15) -0.082(14) 0.017(10) -0.091(11) C72 0.25(2) 0.54(3) 0.23(2) -0.19(2) 0.076(17) -0.17(2) C73 0.075(8) 0.065(8) 0.048(9) 0.019(8) 0.048(8) 0.020(7) C74 0.121(9) 0.087(9) 0.061(8) 0.015(7) 0.062(7) 0.012(7) C75 0.141(11) 0.085(9) 0.071(8) 0.001(7) 0.065(8) 0.028(8) C76 0.072(9) 0.094(11) 0.059(9) 0.008(8) 0.013(8) -0.004(8) C77 0.094(8) 0.094(9) 0.046(7) 0.013(7) 0.034(6) -0.010(7) C78 0.089(14) 0.079(10) 0.040(11) 0.012(9) 0.037(10) 0.004(9) C79 0.033(3) 0.054(4) 0.039(3) 0.012(3) 0.006(3) -0.004(3) C80 0.042(3) 0.040(3) 0.041(4) 0.004(3) 0.013(3) -0.015(3) C81 0.044(3) 0.047(3) 0.037(4) 0.008(3) 0.005(3) -0.006(3) C82 0.055(4) 0.064(4) 0.048(4) 0.005(3) 0.010(3) -0.025(3) C83 0.079(5) 0.091(5) 0.061(5) 0.015(4) 0.024(4) -0.028(4) C84 0.137(8) 0.172(9) 0.075(6) 0.002(6) 0.040(6) -0.087(7) C85 0.062(5) 0.073(5) 0.048(6) -0.018(4) 0.018(5) 0.000(4) C86 0.092(9) 0.100(10) 0.038(8) -0.037(7) 0.010(7) -0.011(8) C87 0.091(11) 0.168(15) 0.088(12) -0.060(11) 0.032(10) -0.019(10) C88 0.169(15) 0.119(14) 0.130(16) 0.002(11) 0.106(13) 0.029(12) C89 0.172(17) 0.23(2) 0.31(3) 0.000 0.067(19) 0.000 C90 0.38(5) 0.63(6) 0.66(6) -0.04(5) 0.03(5) 0.00(5) C91 0.235(11) 0.096(7) 0.054(5) -0.008(5) 0.065(7) -0.034(7) N5 0.088(4) 0.052(3) 0.052(4) 0.003(3) 0.030(3) -0.011(3) C92 0.061(4) 0.081(5) 0.051(4) 0.007(4) 0.023(4) -0.008(3) C93 0.083(5) 0.067(5) 0.046(4) 0.014(4) 0.028(4) 0.015(4) O13 0.143(5) 0.085(4) 0.078(4) 0.025(3) 0.059(4) 0.008(3) C94 0.137(8) 0.108(7) 0.165(11) -0.068(7) 0.047(8) 0.017(6) C95 0.122(8) 0.134(8) 0.130(9) 0.049(7) 0.025(7) -0.053(7) C96 0.135(8) 0.071(6) 0.070(6) -0.003(5) 0.031(6) -0.030(6) C97 0.096(6) 0.098(6) 0.086(6) -0.008(5) 0.034(5) 0.027(5) C98 0.122(8) 0.163(10) 0.219(13) 0.097(10) 0.091(9) 0.026(7) C99 0.079(6) 0.114(8) 0.113(8) -0.019(6) 0.041(5) 0.018(5) C103 0.047(15) 0.003(11) 0.051(8) -0.012(10) 0.018(11) -0.005(8) C104 0.048(6) 0.036(7) 0.019(6) -0.008(6) -0.001(6) -0.009(6) C105 0.065(10) 0.023(10) 0.050(9) -0.002(8) 0.039(9) 0.011(7) N1 0.031(2) 0.020(2) 0.032(3) -0.0061(18) 0.021(2) -0.0048(17) N2 0.032(2) 0.038(2) 0.025(3) 0.002(2) 0.010(2) -0.0171(19) N3 0.037(3) 0.038(3) 0.053(3) 0.002(2) 0.027(2) -0.011(2) N4 0.040(2) 0.019(2) 0.038(3) 0.0085(19) 0.026(2) 0.0080(18) N6 0.101(5) 0.097(5) 0.090(5) -0.009(4) 0.040(5) -0.026(4) N7 0.066(4) 0.088(5) 0.116(6) 0.011(5) 0.040(4) 0.011(4) O1 0.035(2) 0.0283(19) 0.053(3) -0.0030(18) 0.023(2) -0.0033(15) O2 0.057(2) 0.030(2) 0.056(3) -0.0078(18) 0.042(2) -0.0169(17) O3 0.0375(19) 0.035(2) 0.038(2) -0.0005(17) 0.0172(18) -0.0199(16) O4 0.038(2) 0.035(2) 0.040(2) -0.0047(17) 0.0199(19) -0.0141(16) O5 0.035(2) 0.0249(18) 0.058(3) 0.0077(17) 0.031(2) 0.0089(16) O6 0.056(2) 0.031(2) 0.059(3) -0.0050(19) 0.037(2) 0.0059(18) O7 0.035(2) 0.037(2) 0.040(2) -0.0026(17) 0.0159(19) -0.0114(16) O8 0.043(2) 0.036(2) 0.043(2) 0.0011(17) 0.0184(19) -0.0159(17) O9 0.029(2) 0.046(2) 0.040(2) 0.0071(18) 0.0094(18) -0.0118(16) O10 0.0282(19) 0.046(2) 0.034(2) 0.0068(18) 0.0068(17) -0.0051(16) O11 0.0277(18) 0.043(2) 0.032(2) 0.0089(17) 0.0118(17) -0.0044(15) O12 0.0220(18) 0.056(2) 0.038(2) 0.0077(18) 0.0126(17) -0.0078(16) O14 0.167(7) 0.177(7) 0.199(9) -0.046(6) 0.120(7) -0.003(6) O15 0.169(6) 0.086(4) 0.087(4) -0.032(3) 0.066(4) -0.036(4) S1 0.0355(7) 0.0308(7) 0.0445(9) -0.0010(6) 0.0203(7) -0.0103(6) S2 0.0436(8) 0.0377(8) 0.0391(8) -0.0023(6) 0.0214(7) -0.0206(6) S3 0.0308(7) 0.0271(7) 0.0564(9) -0.0015(6) 0.0255(7) 0.0050(5) S4 0.0325(7) 0.0354(7) 0.0355(8) -0.0025(6) 0.0169(6) 0.0094(6) S5 0.0287(7) 0.0431(8) 0.0349(8) 0.0002(6) 0.0092(6) -0.0059(6) S6 0.0233(7) 0.0382(7) 0.0301(8) -0.0019(6) 0.0082(6) 0.0020(5) Zn1 0.0346(3) 0.0164(3) 0.0385(4) -0.0004(2) 0.0267(3) 0.0002(2) Zn2 0.0236(3) 0.0333(3) 0.0321(4) 0.0060(3) 0.0116(3) -0.0110(2) Zn3 0.0232(3) 0.0323(3) 0.0282(3) 0.0040(3) 0.0093(3) -0.0130(2) C73B 0.089(14) 0.060(11) 0.054(12) 0.043(10) 0.061(11) 0.054(10) C74B 0.108(11) 0.018(7) 0.054(10) 0.007(7) 0.061(9) 0.013(8) C75B 0.061(10) 0.056(10) 0.066(11) 0.007(9) 0.036(9) -0.010(8) C76B 0.063(11) 0.078(12) 0.042(10) -0.006(9) 0.033(9) -0.004(10) C77B 0.100(13) 0.059(12) 0.043(11) 0.008(10) 0.049(11) 0.012(10) C78B 0.054(14) 0.088(14) 0.047(16) -0.005(13) 0.017(12) 0.014(11) C85B 0.062(5) 0.073(5) 0.048(6) -0.018(4) 0.018(5) 0.000(4) C86B 0.236(18) 0.111(14) 0.085(13) -0.045(11) -0.006(14) 0.036(14) C87B 0.27(2) 0.112(16) 0.126(17) -0.064(14) 0.019(17) 0.055(17) C88B 0.36(3) 0.21(2) 0.20(2) -0.08(2) 0.04(2) 0.00(3) C89B 0.40(3) 0.21(3) 0.24(3) -0.13(2) 0.06(3) 0.03(3) C90B 0.47(5) 0.15(3) 0.32(4) 0.03(3) 0.09(4) -0.04(4) N9 0.038(15) 0.031(7) 0.043(7) 0.006(7) 0.028(12) 0.014(5) O17 0.049(17) 0.022(3) 0.053(15) -0.009(7) 0.007(7) -0.008(7) O20 0.112(8) 0.052(6) 0.149(11) -0.018(6) 0.070(8) -0.023(5) C55B 0.096(12) 0.046(9) 0.045(9) -0.001(7) 0.027(8) -0.036(8) C56B 0.065(10) 0.091(11) 0.070(11) 0.019(10) 0.017(9) -0.029(9) C57B 0.044(11) 0.157(15) 0.073(13) 0.014(12) 0.006(10) -0.036(11) C58B 0.154(18) 0.23(2) 0.208(19) 0.037(18) -0.028(17) -0.035(17) C59B 0.130(18) 0.21(2) 0.23(2) 0.04(2) 0.026(17) -0.018(19) C60B 0.34(5) 0.34(5) 0.33(5) -0.01(4) -0.02(4) -0.16(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O1 1.242(6) . ? C1 O2 1.245(6) . ? C1 C2 1.501(7) . ? C1 Zn1 2.490(5) . ? C2 C3 1.319(8) . ? C2 S1 1.712(5) . ? C3 C4 1.436(8) . ? C4 C5 1.357(7) . ? C4 C55 1.553(5) . ? C4 C55B 1.594(16) . ? C5 C6 1.461(7) . ? C5 S1 1.710(5) . ? C6 C7 1.377(7) . ? C6 S2 1.722(5) . ? C7 C8 1.419(7) . ? C7 C61 1.481(7) . ? C8 C9 1.356(7) . ? C9 C10 1.478(7) . ? C9 S2 1.712(5) . ? C10 O3 1.252(6) . ? C10 O4 1.260(6) . ? C11 O6 1.227(6) . ? C11 O5 1.284(6) . ? C11 C12 1.483(7) . ? C12 C13 1.356(7) . ? C12 S3 1.710(5) . ? C13 C14 1.431(7) . ? C14 C15 1.373(7) . ? C14 C67 1.524(8) . ? C15 C16 1.456(7) . ? C15 S3 1.724(5) . ? C16 C17 1.372(7) . ? C16 S4 1.720(5) . ? C17 C73B 1.36(2) . ? C17 C18 1.427(7) . ? C17 C73 1.618(15) . ? C18 C19 1.350(7) . ? C19 C20 1.469(7) 8_455 ? C19 S4 1.719(5) . ? C20 O8 1.259(6) . ? C20 O7 1.262(6) . ? C20 C19 1.469(7) 8_556 ? C21 O9 1.257(6) . ? C21 O10 1.259(6) . ? C21 C22 1.475(7) . ? C22 C23 1.373(7) . ? C22 S5 1.708(5) . ? C23 C24 1.420(7) . ? C24 C25 1.367(7) . ? C24 C79 1.511(7) . ? C25 C26 1.483(7) . ? C25 S5 1.723(5) . ? C26 C27 1.369(7) . ? C26 S6 1.722(5) . ? C27 C28 1.410(7) . ? C27 C85 1.47(2) . ? C27 C85B 1.57(2) . ? C28 C29 1.374(7) . ? C29 C30 1.482(7) 8_455 ? C29 S6 1.709(5) . ? C30 O12 1.262(6) . ? C30 O11 1.263(6) . ? C30 C29 1.482(7) 8_556 ? C31 N1 1.335(6) . ? C31 C33 1.390(6) . ? C32 N1 1.336(6) . ? C32 C34 1.355(7) . ? C33 C35 1.381(6) . ? C34 C35 1.394(7) . ? C35 C36 1.446(6) . ? C36 C37 1.334(6) . ? C37 C38 1.472(6) . ? C38 C39 1.381(7) . ? C38 C40 1.389(6) . ? C39 C41 1.372(7) 3_445 ? C40 C42 1.364(6) 3_445 ? C41 N2 1.341(6) . ? C41 C39 1.372(7) 3 ? C42 N2 1.319(6) . ? C42 C40 1.364(7) 3 ? C43 N3 1.323(7) . ? C43 C45 1.357(8) . ? C44 N3 1.321(7) . ? C44 C46 1.404(8) . ? C45 C47 1.377(8) . ? C46 C47 1.384(8) . ? C47 C48 1.472(8) . ? C48 C49 1.291(8) . ? C49 C50 1.485(7) . ? C50 C51 1.371(7) . ? C50 C52 1.381(7) . ? C51 C53 1.382(6) 6_556 ? C52 C54 1.367(7) 6_556 ? C53 N4 1.331(6) . ? C53 C51 1.382(6) 6 ? C54 N4 1.337(6) . ? C54 C52 1.367(7) 6 ? C55 C56 1.536(5) . ? C56 C57 1.532(9) . ? C57 C58 1.536(10) . ? C58 C59 1.543(10) . ? C59 C60 1.538(10) . ? C61 C62 1.519(7) . ? C62 C63 1.509(8) . ? C63 C64 1.517(9) . ? C64 C65 1.547(12) . ? C65 C66 1.556(14) . ? C67 C68 1.534(10) . ? C68 C69 1.514(9) . ? C69 C70 1.608(14) . ? C70 C71 1.532(14) . ? C71 C72 1.60(2) . ? C73 C74 1.534(4) . ? C74 C75 1.530(7) . ? C75 C76 1.520(8) . ? C76 C77 1.553(9) . ? C77 C78 1.534(8) . ? C79 C80 1.509(7) . ? C80 C81 1.525(7) . ? C81 C82 1.515(8) . ? C82 C83 1.514(8) . ? C83 C84 1.566(10) . ? C85 C86 1.552(4) . ? C86 C87 1.567(8) . ? C87 C88 1.555(9) . ? C88 C89 1.571(8) . ? C89 C90 1.561(7) . ? C91 N5 1.477(9) . ? N5 C93 1.311(8) . ? N5 C92 1.411(7) . ? C93 O13 1.228(7) . ? C94 N6 1.462(10) . ? C95 N6 1.458(10) . ? C96 O15 1.267(10) . ? C96 N6 1.344(11) . ? C97 N7 1.443(10) . ? C98 N7 1.512(10) . ? C99 O14 1.266(10) . ? C99 N7 1.341(10) . ? C103 N9 1.425(9) . ? C104 O17 1.23(3) . ? C104 N9 1.325(15) . ? C105 N9 1.449(8) . ? N1 Zn1 2.039(4) . ? N2 Zn3 1.999(4) . ? N3 Zn2 2.010(4) . ? N4 Zn1 2.046(4) . ? O1 Zn1 2.387(3) . ? O2 Zn1 2.021(3) . ? O3 Zn3 2.056(3) . ? O4 Zn2 2.052(4) . ? O5 Zn1 1.934(3) . ? O7 Zn3 2.088(4) . ? O8 Zn2 2.037(3) . ? O9 Zn3 2.019(3) . ? O10 Zn2 2.056(3) . ? O11 Zn3 2.017(3) . ? O12 Zn2 2.027(3) . ? Zn2 Zn3 2.9676(8) . ? C73B C74B 1.537(5) . ? C74B C75B 1.529(9) . ? C75B C76B 1.525(10) . ? C76B C77B 1.535(10) . ? C77B C78B 1.531(9) . ? C85B C86B 1.542(5) . ? C86B C87B 1.553(10) . ? C87B C88B 1.545(10) . ? C88B C89B 1.545(11) . ? C89B C90B 1.552(11) . ? C55B C56B 1.551(5) . ? C56B C57B 1.556(10) . ? C57B C58B 1.545(10) . ? C58B C59B 1.545(10) . ? C59B C60B 1.557(10) . ? 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 O1 C1 O2 124.4(5) . . ? O1 C1 C2 118.5(4) . . ? O2 C1 C2 117.1(5) . . ? O1 C1 Zn1 70.7(3) . . ? O2 C1 Zn1 53.8(2) . . ? C2 C1 Zn1 170.4(4) . . ? C3 C2 C1 129.8(5) . . ? C3 C2 S1 111.1(4) . . ? C1 C2 S1 119.0(4) . . ? C2 C3 C4 114.2(5) . . ? C5 C4 C3 111.0(5) . . ? C5 C4 C55 121.2(7) . . ? C3 C4 C55 124.1(7) . . ? C5 C4 C55B 126.2(7) . . ? C3 C4 C55B 114.9(7) . . ? C55 C4 C55B 44.4(6) . . ? C4 C5 C6 128.3(5) . . ? C4 C5 S1 111.4(4) . . ? C6 C5 S1 120.1(4) . . ? C7 C6 C5 130.5(5) . . ? C7 C6 S2 112.2(4) . . ? C5 C6 S2 117.1(4) . . ? C6 C7 C8 110.6(5) . . ? C6 C7 C61 125.7(5) . . ? C8 C7 C61 123.7(5) . . ? C9 C8 C7 114.2(4) . . ? C8 C9 C10 130.4(5) . . ? C8 C9 S2 111.4(4) . . ? C10 C9 S2 118.1(4) . . ? O3 C10 O4 125.8(5) . . ? O3 C10 C9 117.9(5) . . ? O4 C10 C9 116.3(4) . . ? O6 C11 O5 125.9(4) . . ? O6 C11 C12 120.4(5) . . ? O5 C11 C12 113.8(4) . . ? C13 C12 C11 128.7(5) . . ? C13 C12 S3 110.7(4) . . ? C11 C12 S3 120.6(4) . . ? C12 C13 C14 114.6(5) . . ? C15 C14 C13 110.6(5) . . ? C15 C14 C67 124.7(5) . . ? C13 C14 C67 124.6(5) . . ? C14 C15 C16 129.2(4) . . ? C14 C15 S3 111.8(4) . . ? C16 C15 S3 119.0(4) . . ? C17 C16 C15 128.3(5) . . ? C17 C16 S4 111.9(4) . . ? C15 C16 S4 119.7(4) . . ? C73B C17 C16 121.6(15) . . ? C73B C17 C18 126.4(15) . . ? C16 C17 C18 111.2(5) . . ? C73B C17 C73 16.5(11) . . ? C16 C17 C73 126.4(8) . . ? C18 C17 C73 121.7(8) . . ? C19 C18 C17 113.8(5) . . ? C18 C19 C20 129.5(5) . 8_455 ? C18 C19 S4 111.4(4) . . ? C20 C19 S4 119.1(4) 8_455 . ? O8 C20 O7 125.6(5) . . ? O8 C20 C19 117.9(5) . 8_556 ? O7 C20 C19 116.5(5) . 8_556 ? O9 C21 O10 125.9(5) . . ? O9 C21 C22 117.5(5) . . ? O10 C21 C22 116.6(5) . . ? C23 C22 C21 127.6(5) . . ? C23 C22 S5 111.7(4) . . ? C21 C22 S5 120.7(4) . . ? C22 C23 C24 113.1(5) . . ? C25 C24 C23 111.2(5) . . ? C25 C24 C79 125.7(5) . . ? C23 C24 C79 123.1(5) . . ? C24 C25 C26 129.2(5) . . ? C24 C25 S5 112.6(4) . . ? C26 C25 S5 118.1(4) . . ? C27 C26 C25 129.7(5) . . ? C27 C26 S6 111.6(4) . . ? C25 C26 S6 118.3(4) . . ? C26 C27 C28 112.2(5) . . ? C26 C27 C85 125(2) . . ? C28 C27 C85 123(2) . . ? C26 C27 C85B 125(2) . . ? C28 C27 C85B 123(2) . . ? C85 C27 C85B 4.5(14) . . ? C29 C28 C27 113.1(5) . . ? C28 C29 C30 128.3(5) . 8_455 ? C28 C29 S6 111.3(4) . . ? C30 C29 S6 120.4(4) 8_455 . ? O12 C30 O11 127.4(5) . . ? O12 C30 C29 117.4(5) . 8_556 ? O11 C30 C29 115.3(5) . 8_556 ? N1 C31 C33 122.7(4) . . ? N1 C32 C34 124.3(5) . . ? C35 C33 C31 119.9(5) . . ? C32 C34 C35 119.6(5) . . ? C33 C35 C34 116.7(4) . . ? C33 C35 C36 120.5(5) . . ? C34 C35 C36 122.7(4) . . ? C37 C36 C35 124.2(5) . . ? C36 C37 C38 124.2(5) . . ? C39 C38 C40 116.5(4) . . ? C39 C38 C37 123.9(4) . . ? C40 C38 C37 119.5(5) . . ? C41 C39 C38 120.2(5) 3_445 . ? C42 C40 C38 119.8(5) 3_445 . ? N2 C41 C39 122.3(5) . 3 ? N2 C42 C40 123.5(4) . 3 ? N3 C43 C45 123.8(6) . . ? N3 C44 C46 123.2(6) . . ? C43 C45 C47 120.0(6) . . ? C47 C46 C44 118.2(6) . . ? C45 C47 C46 117.3(5) . . ? C45 C47 C48 121.2(6) . . ? C46 C47 C48 121.4(6) . . ? C49 C48 C47 126.1(6) . . ? C48 C49 C50 125.9(6) . . ? C51 C50 C52 117.9(5) . . ? C51 C50 C49 118.5(5) . . ? C52 C50 C49 123.5(5) . . ? C50 C51 C53 119.2(5) . 6_556 ? C54 C52 C50 119.1(5) 6_556 . ? N4 C53 C51 123.4(4) . 6 ? N4 C54 C52 123.8(5) . 6 ? C56 C55 C4 118.6(7) . . ? C57 C56 C55 115.9(9) . . ? C56 C57 C58 114.6(11) . . ? C57 C58 C59 113.4(12) . . ? C60 C59 C58 114.1(12) . . ? C7 C61 C62 114.3(5) . . ? C63 C62 C61 113.6(5) . . ? C62 C63 C64 112.5(6) . . ? C63 C64 C65 112.9(8) . . ? C64 C65 C66 113.0(11) . . ? C14 C67 C68 113.3(6) . . ? C69 C68 C67 113.0(7) . . ? C68 C69 C70 109.7(8) . . ? C71 C70 C69 107.1(11) . . ? C70 C71 C72 105.9(15) . . ? C74 C73 C17 114.3(10) . . ? C75 C74 C73 112.5(7) . . ? C76 C75 C74 113.2(7) . . ? C75 C76 C77 110.5(9) . . ? C78 C77 C76 110.8(8) . . ? C80 C79 C24 114.2(4) . . ? C79 C80 C81 114.3(4) . . ? C82 C81 C80 112.9(4) . . ? C83 C82 C81 113.6(5) . . ? C82 C83 C84 110.8(6) . . ? C27 C85 C86 114.0(13) . . ? C85 C86 C87 121.4(9) . . ? C88 C87 C86 122.3(11) . . ? C87 C88 C89 123.1(10) . . ? C90 C89 C88 121.8(11) . . ? C93 N5 C92 122.7(6) . . ? C93 N5 C91 121.3(6) . . ? C92 N5 C91 115.9(6) . . ? O13 C93 N5 126.6(7) . . ? O15 C96 N6 124.5(8) . . ? O14 C99 N7 123.1(11) . . ? O17 C104 N9 125.1(19) . . ? C31 N1 C32 116.7(4) . . ? C31 N1 Zn1 121.0(3) . . ? C32 N1 Zn1 122.2(3) . . ? C42 N2 C41 117.5(4) . . ? C42 N2 Zn3 121.5(3) . . ? C41 N2 Zn3 121.0(4) . . ? C44 N3 C43 117.2(5) . . ? C44 N3 Zn2 118.6(4) . . ? C43 N3 Zn2 124.2(4) . . ? C53 N4 C54 116.6(4) . . ? C53 N4 Zn1 120.7(3) . . ? C54 N4 Zn1 122.2(3) . . ? C96 N6 C95 119.0(8) . . ? C96 N6 C94 118.3(8) . . ? C95 N6 C94 122.3(9) . . ? C99 N7 C97 119.7(8) . . ? C99 N7 C98 119.5(9) . . ? C97 N7 C98 120.4(8) . . ? C1 O1 Zn1 79.9(3) . . ? C1 O2 Zn1 96.5(3) . . ? C10 O3 Zn3 111.8(3) . . ? C10 O4 Zn2 143.5(3) . . ? C11 O5 Zn1 123.0(3) . . ? C20 O7 Zn3 137.7(3) . . ? C20 O8 Zn2 115.9(3) . . ? C21 O9 Zn3 127.2(3) . . ? C21 O10 Zn2 127.3(3) . . ? C30 O11 Zn3 129.6(3) . . ? C30 O12 Zn2 123.1(3) . . ? C5 S1 C2 92.1(3) . . ? C9 S2 C6 91.5(3) . . ? C12 S3 C15 92.3(2) . . ? C19 S4 C16 91.7(2) . . ? C22 S5 C25 91.3(3) . . ? C29 S6 C26 91.9(2) . . ? O5 Zn1 O2 118.63(14) . . ? O5 Zn1 N1 105.52(14) . . ? O2 Zn1 N1 98.18(15) . . ? O5 Zn1 N4 125.78(15) . . ? O2 Zn1 N4 103.44(15) . . ? N1 Zn1 N4 100.23(14) . . ? O5 Zn1 O1 85.94(12) . . ? O2 Zn1 O1 59.16(13) . . ? N1 Zn1 O1 157.26(15) . . ? N4 Zn1 O1 88.07(13) . . ? O5 Zn1 C1 104.21(15) . . ? O2 Zn1 C1 29.78(15) . . ? N1 Zn1 C1 127.96(17) . . ? N4 Zn1 C1 95.64(15) . . ? O1 Zn1 C1 29.41(13) . . ? N3 Zn2 O12 97.66(16) . . ? N3 Zn2 O8 105.55(17) . . ? O12 Zn2 O8 91.28(14) . . ? N3 Zn2 O4 97.75(16) . . ? O12 Zn2 O4 87.08(14) . . ? O8 Zn2 O4 156.64(14) . . ? N3 Zn2 O10 100.96(16) . . ? O12 Zn2 O10 161.11(14) . . ? O8 Zn2 O10 86.78(14) . . ? O4 Zn2 O10 87.32(14) . . ? N3 Zn2 Zn3 165.30(14) . . ? O12 Zn2 Zn3 82.28(10) . . ? O8 Zn2 Zn3 89.14(10) . . ? O4 Zn2 Zn3 67.54(9) . . ? O10 Zn2 Zn3 78.90(10) . . ? N2 Zn3 O11 98.91(15) . . ? N2 Zn3 O9 103.01(15) . . ? O11 Zn3 O9 158.01(14) . . ? N2 Zn3 O3 98.80(15) . . ? O11 Zn3 O3 90.50(13) . . ? O9 Zn3 O3 87.93(14) . . ? N2 Zn3 O7 99.47(15) . . ? O11 Zn3 O7 87.98(14) . . ? O9 Zn3 O7 86.69(14) . . ? O3 Zn3 O7 161.68(13) . . ? N2 Zn3 Zn2 169.39(12) . . ? O11 Zn3 Zn2 77.61(9) . . ? O9 Zn3 Zn2 80.50(10) . . ? O3 Zn3 Zn2 91.29(9) . . ? O7 Zn3 Zn2 70.55(9) . . ? C17 C73B C74B 114.2(14) . . ? C75B C74B C73B 112.6(10) . . ? C76B C75B C74B 113.5(11) . . ? C75B C76B C77B 112.6(12) . . ? C78B C77B C76B 112.9(12) . . ? C86B C85B C27 109.6(13) . . ? C85B C86B C87B 110.7(12) . . ? C88B C87B C86B 111.1(14) . . ? C87B C88B C89B 111.5(15) . . ? C88B C89B C90B 111.1(15) . . ? C104 N9 C103 120.3(9) . . ? C104 N9 C105 123.7(12) . . ? C103 N9 C105 115.9(14) . . ? C56B C55B C4 98.8(9) . . ? C55B C56B C57B 112.2(11) . . ? C58B C57B C56B 113.6(13) . . ? C59B C58B C57B 114.4(14) . . ? C58B C59B C60B 113.0(14) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.475 _refine_diff_density_min -0.496 _refine_diff_density_rms 0.076 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.269 0.250 49 3 ' ' 2 0.000 0.731 0.750 49 3 ' ' 3 0.250 0.250 1.000 694 144 ' ' 4 0.250 0.750 0.500 694 144 ' ' 5 0.500 0.231 0.750 49 3 ' ' 6 0.500 0.769 0.250 49 3 ' ' 7 0.750 0.250 0.500 694 144 ' ' 8 0.750 0.750 1.000 694 144 ' ' _platon_squeeze_details ; ; # sin(theta_max) is low because diffrn_reflns_theta_max is low. This # is due to the poorly diffracting nature of 5.