# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email l.p.harding@hud.ac.uk _publ_contact_author_name 'Lindsay P Harding' loop_ _publ_author_name 'Nicola M. Cox' 'Lindsay P. Harding' 'Jennifer E. Jones' 'Simon J.A. Pope' 'Craig. R. Rice' 'Harry Adams' data_mo_nicky_cu_monosub_0ma _database_code_depnum_ccdc_archive 'CCDC 845594' #TrackingRef 'mo_NIcky_Cu_monosub_0ma_final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C204 H118 Cu6 F36 N24 P6 S6' _chemical_formula_weight 4348.64 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Iba2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'x+1, -y+1, z+1/2' '-x+1, y+1, z+1/2' _cell_length_a 45.237(2) _cell_length_b 18.6322(10) _cell_length_c 23.8739(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 20122.5(19) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8745 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 22.81 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.435 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8776 _exptl_absorpt_coefficient_mu 0.824 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7612 _exptl_absorpt_correction_T_max 0.9221 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 31846 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0609 _diffrn_reflns_limit_h_min -48 _diffrn_reflns_limit_h_max 50 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 23.31 _reflns_number_total 12922 _reflns_number_gt 10183 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT, SADABS and XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1355P)^2^+38.6018P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.003(17) _refine_ls_number_reflns 12922 _refine_ls_number_parameters 1227 _refine_ls_number_restraints 949 _refine_ls_R_factor_all 0.0877 _refine_ls_R_factor_gt 0.0660 _refine_ls_wR_factor_ref 0.2000 _refine_ls_wR_factor_gt 0.1813 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.019 _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 Cu1 Cu 0.21764(2) 0.47651(5) 0.39844(6) 0.0367(3) Uani 1 1 d . . . Cu2 Cu 0.19623(2) 0.33205(5) 0.42186(6) 0.0383(3) Uani 1 1 d . . . Cu3 Cu 0.03021(2) 1.02680(7) 0.43264(7) 0.0542(3) Uani 1 1 d . . . S1 S 0.06261(8) 1.0274(2) 0.60842(13) 0.0834(10) Uani 1 1 d . . . S2 S 0.28531(5) 0.47278(13) 0.26140(12) 0.0529(6) Uani 1 1 d . . . S3 S 0.22644(5) 0.19824(13) 0.27896(11) 0.0481(6) Uani 1 1 d . . . N1 N 0.20412(14) 0.4395(3) 0.3216(3) 0.0340(15) Uani 1 1 d . . . N2 N 0.24157(14) 0.3251(3) 0.4116(3) 0.0350(16) Uani 1 1 d . . . N3 N 0.25712(15) 0.4908(3) 0.3532(3) 0.0374(16) Uani 1 1 d . . . N4 N 0.23057(14) 0.4442(3) 0.4776(3) 0.0333(16) Uani 1 1 d . . . N5 N 0.16818(13) 0.5812(3) 0.42406(19) 0.077(3) Uani 1 1 d G . . C20 C 0.19119(11) 0.5395(3) 0.4448(2) 0.0345(13) Uani 1 1 d GU . . C22 C 0.19533(11) 0.5331(3) 0.5023(2) 0.0425(11) Uani 1 1 d GU . . C83 C 0.17646(13) 0.5685(3) 0.53902(19) 0.0526(13) Uani 1 1 d GU . . H83 H 0.1793 0.5641 0.5783 0.063 Uiso 1 1 calc R . . C84 C 0.15345(12) 0.6101(3) 0.5183(2) 0.0596(15) Uani 1 1 d GU . . H84 H 0.1405 0.6343 0.5434 0.071 Uiso 1 1 calc R . . C85 C 0.14931(11) 0.6165(3) 0.4608(3) 0.0607(18) Uani 1 1 d GU . . H85 H 0.1336 0.6450 0.4467 0.073 Uiso 1 1 calc R . . N6 N 0.17748(16) 0.3387(3) 0.4969(3) 0.0428(18) Uani 1 1 d . . . N7 N 0.16141(14) 0.3993(3) 0.4016(3) 0.0409(17) Uani 1 1 d . . . N8 N 0.05615(16) 1.0157(4) 0.5028(3) 0.052(2) Uani 1 1 d . . . N9 N 0.00766(17) 1.0923(5) 0.4884(4) 0.060(2) Uani 1 1 d . . . N10 N 0.19723(14) 0.2573(4) 0.3584(3) 0.0381(16) Uani 1 1 d . . . N11 N 0.02802(12) 0.9270(3) 0.3939(3) 0.057(2) Uani 1 1 d G . . C68 C 0.02664(13) 0.8614(4) 0.4216(2) 0.077(2) Uani 1 1 d GU . . C69 C 0.03370(15) 0.7985(3) 0.3933(3) 0.0788(18) Uani 1 1 d GU . . H69 H 0.0328 0.7537 0.4122 0.095 Uiso 1 1 calc R . . C78 C 0.04214(15) 0.8011(4) 0.3373(3) 0.0801(17) Uani 1 1 d GU . . H78 H 0.0470 0.7581 0.3180 0.096 Uiso 1 1 calc R . . C80 C 0.04352(14) 0.8667(5) 0.3097(2) 0.0764(17) Uani 1 1 d GU . . H80 H 0.0493 0.8685 0.2715 0.092 Uiso 1 1 calc R . . C81 C 0.03646(13) 0.9296(3) 0.3380(3) 0.0722(16) Uani 1 1 d GU . . N12 N 0.03619(16) 1.0556(5) 0.3534(4) 0.059(2) Uani 1 1 d . . . C1 C 0.33241(19) 0.5120(5) 0.4936(4) 0.0443(12) Uani 1 1 d U . . H1 H 0.3501 0.4894 0.5060 0.053 Uiso 1 1 calc R . . C2 C 0.32260(17) 0.5007(5) 0.4395(4) 0.0422(12) Uani 1 1 d U . . H2 H 0.3337 0.4705 0.4152 0.051 Uiso 1 1 calc R . . C3 C 0.29666(17) 0.5327(4) 0.4197(4) 0.0394(10) Uani 1 1 d U . . C4 C 0.28125(17) 0.5799(4) 0.4548(4) 0.0383(10) Uani 1 1 d U . . C5 C 0.29111(18) 0.5895(4) 0.5104(4) 0.0400(10) Uani 1 1 d U . . C6 C 0.31694(19) 0.5554(5) 0.5296(4) 0.0438(11) Uani 1 1 d U . . C7 C 0.2852(2) 0.6450(5) 0.6045(4) 0.0459(11) Uani 1 1 d U . . C8 C 0.27523(19) 0.6355(4) 0.5471(4) 0.0419(10) Uani 1 1 d U . . C9 C 0.2488(2) 0.6707(4) 0.5299(4) 0.0420(10) Uani 1 1 d U . . C10 C 0.2337(2) 0.7126(5) 0.5677(4) 0.0466(12) Uani 1 1 d U . . H10 H 0.2162 0.7366 0.5558 0.056 Uiso 1 1 calc R . . C11 C 0.2433(2) 0.7210(5) 0.6234(4) 0.0489(13) Uani 1 1 d U . . H11 H 0.2319 0.7485 0.6490 0.059 Uiso 1 1 calc R . . C12 C 0.2683(2) 0.6904(5) 0.6403(4) 0.0485(13) Uani 1 1 d U . . H12 H 0.2751 0.6991 0.6773 0.058 Uiso 1 1 calc R . . C13 C 0.26289(18) 0.3526(4) 0.4438(4) 0.0420(12) Uani 1 1 d U . . C14 C 0.29263(18) 0.3369(4) 0.4339(4) 0.0445(12) Uani 1 1 d U . . H14 H 0.3074 0.3550 0.4584 0.053 Uiso 1 1 calc R . . C15 C 0.30051(19) 0.2966(4) 0.3900(4) 0.0467(13) Uani 1 1 d U . . H15 H 0.3208 0.2869 0.3831 0.056 Uiso 1 1 calc R . . C16 C 0.27889(18) 0.2691(4) 0.3547(4) 0.0441(13) Uani 1 1 d U . . H16 H 0.2840 0.2426 0.3221 0.053 Uiso 1 1 calc R . . C17 C 0.24893(17) 0.2821(4) 0.3690(4) 0.0405(13) Uani 1 1 d U . . C18 C 0.25331(19) 0.4001(4) 0.4894(4) 0.0437(13) Uani 1 1 d U . . C19 C 0.2194(2) 0.4876(4) 0.5196(4) 0.0433(12) Uani 1 1 d U . . C23 C 0.1753(2) 0.3293(6) 0.5966(5) 0.0607(15) Uani 1 1 d U . . H23 H 0.1835 0.3116 0.6305 0.073 Uiso 1 1 calc R . . C24 C 0.1882(2) 0.3147(5) 0.5461(4) 0.0567(18) Uani 1 1 d U . . H24 H 0.2056 0.2861 0.5457 0.068 Uiso 1 1 calc R . . C25 C 0.1521(2) 0.3783(5) 0.4967(4) 0.0527(14) Uani 1 1 d U . . C26 C 0.1420(2) 0.4041(5) 0.4435(4) 0.0513(13) Uani 1 1 d U . . C27 C 0.1536(2) 0.4212(5) 0.3495(4) 0.0483(13) Uani 1 1 d U . . C28 C 0.1249(2) 0.4463(5) 0.3390(4) 0.0541(14) Uani 1 1 d U . . H28 H 0.1192 0.4592 0.3021 0.065 Uiso 1 1 calc R . . C29 C 0.1052(2) 0.4519(5) 0.3828(4) 0.0567(14) Uani 1 1 d U . . H29 H 0.0861 0.4711 0.3763 0.068 Uiso 1 1 calc R . . C30 C 0.28623(18) 0.5117(4) 0.3625(4) 0.0399(12) Uani 1 1 d U . . C31 C 0.30385(19) 0.5057(5) 0.3176(4) 0.0437(15) Uani 1 1 d U . . H31 H 0.3242 0.5184 0.3173 0.052 Uiso 1 1 calc R . . C32 C 0.25408(19) 0.4685(4) 0.3025(4) 0.0401(15) Uani 1 1 d U . . C33 C 0.2254(2) 0.4408(4) 0.2820(4) 0.0426(13) Uani 1 1 d U . . C34 C 0.0180(2) 1.0910(6) 0.5413(5) 0.0699(17) Uani 1 1 d U . . C35 C 0.0446(2) 1.0473(7) 0.5471(5) 0.068(2) Uani 1 1 d U . . C36 C 0.0870(2) 0.9727(6) 0.5729(5) 0.0611(17) Uani 1 1 d U . . H36 H 0.1027 0.9465 0.5895 0.073 Uiso 1 1 calc R . . C37 C 0.0802(2) 0.9729(5) 0.5166(5) 0.0570(14) Uani 1 1 d U . . C38 C 0.2314(2) 0.4860(5) 0.5735(4) 0.0492(13) Uani 1 1 d U . . H38 H 0.2229 0.5145 0.6023 0.059 Uiso 1 1 calc R . . C39 C 0.2547(2) 0.4445(5) 0.5845(4) 0.0512(13) Uani 1 1 d U . . H39 H 0.2633 0.4450 0.6208 0.061 Uiso 1 1 calc R . . C40 C 0.2664(2) 0.4010(5) 0.5434(4) 0.0482(13) Uani 1 1 d U . . H40 H 0.2832 0.3719 0.5512 0.058 Uiso 1 1 calc R . . C41 C 0.24049(19) 0.6617(4) 0.4728(4) 0.0398(12) Uani 1 1 d U . . H41 H 0.2239 0.6876 0.4593 0.048 Uiso 1 1 calc R . . C42 C 0.25504(17) 0.6183(4) 0.4370(4) 0.0390(11) Uani 1 1 d U . . H42 H 0.2480 0.6128 0.3997 0.047 Uiso 1 1 calc R . . C43 C 0.2204(2) 0.4169(4) 0.2275(4) 0.0472(13) Uani 1 1 d U . . H43 H 0.2360 0.4166 0.2010 0.057 Uiso 1 1 calc R . . C44 C 0.1925(2) 0.3938(5) 0.2125(4) 0.0493(13) Uani 1 1 d U . . H44 H 0.1889 0.3761 0.1758 0.059 Uiso 1 1 calc R . . C45 C 0.1707(2) 0.3969(5) 0.2504(4) 0.0488(13) Uani 1 1 d U . . H45 H 0.1511 0.3845 0.2399 0.059 Uiso 1 1 calc R . . C46 C 0.1768(2) 0.4184(5) 0.3057(4) 0.0465(13) Uani 1 1 d U . . C47 C 0.3118(2) 0.6069(5) 0.6223(4) 0.0484(12) Uani 1 1 d U . . H47 H 0.3183 0.6115 0.6599 0.058 Uiso 1 1 calc R . . C48 C 0.3265(2) 0.5669(5) 0.5880(4) 0.0485(12) Uani 1 1 d U . . H48 H 0.3440 0.5441 0.6009 0.058 Uiso 1 1 calc R . . C49 C 0.1770(2) 0.2249(5) 0.3235(5) 0.0530(14) Uani 1 1 d U . . C50 C 0.1887(2) 0.1899(5) 0.2791(5) 0.0513(16) Uani 1 1 d U . . H50 H 0.1776 0.1644 0.2519 0.062 Uiso 1 1 calc R . . C51 C 0.1449(2) 0.2350(5) 0.3349(5) 0.0578(12) Uani 1 1 d U . . C52 C 0.22373(18) 0.2497(4) 0.3392(4) 0.0389(15) Uani 1 1 d U . . C53 C 0.1324(2) 0.2298(5) 0.3872(5) 0.0625(12) Uani 1 1 d U . . C54 C 0.1472(2) 0.2008(5) 0.4353(5) 0.0630(14) Uani 1 1 d U . . H54 H 0.1669 0.1838 0.4315 0.076 Uiso 1 1 calc R . . C55 C 0.1128(2) 0.4305(5) 0.4344(5) 0.0553(14) Uani 1 1 d U . . H55 H 0.0990 0.4328 0.4644 0.066 Uiso 1 1 calc R . . C56 C 0.1379(2) 0.3943(5) 0.5472(4) 0.0593(14) Uani 1 1 d U . . H56 H 0.1201 0.4213 0.5473 0.071 Uiso 1 1 calc R . . C57 C 0.10170(18) 0.9590(5) 0.4199(4) 0.0502(11) Uani 1 1 d U . . C58 C 0.0943(2) 0.9293(5) 0.4724(4) 0.0542(11) Uani 1 1 d U . . C59 C 0.10081(18) 1.0350(5) 0.4088(4) 0.0489(12) Uani 1 1 d U . . H59 H 0.0958 1.0675 0.4380 0.059 Uiso 1 1 calc R . . C60 C 0.10708(18) 1.0597(5) 0.3578(4) 0.0488(12) Uani 1 1 d U . . H60 H 0.1069 1.1101 0.3515 0.059 Uiso 1 1 calc R . . C61 C 0.0989(2) 0.8559(6) 0.4824(5) 0.0564(13) Uani 1 1 d U . . H61 H 0.0954 0.8370 0.5187 0.068 Uiso 1 1 calc R . . C62 C 0.10804(19) 0.8121(6) 0.4416(4) 0.0557(13) Uani 1 1 d U . . H62 H 0.1108 0.7627 0.4498 0.067 Uiso 1 1 calc R . . C63 C 0.11374(19) 0.8364(5) 0.3872(4) 0.0531(11) Uani 1 1 d U . . C64 C 0.11638(18) 0.9401(5) 0.3221(4) 0.0498(10) Uani 1 1 d U . . C65 C 0.11406(18) 1.0132(5) 0.3125(4) 0.0495(11) Uani 1 1 d U . . C66 C 0.12002(19) 1.0418(6) 0.2578(4) 0.0532(13) Uani 1 1 d U . . H66 H 0.1194 1.0920 0.2510 0.064 Uiso 1 1 calc R . . C67 C 0.12684(19) 0.9938(6) 0.2146(5) 0.0569(13) Uani 1 1 d U . . H67 H 0.1303 1.0118 0.1780 0.068 Uiso 1 1 calc R . . C70 C 0.0379(2) 1.0016(8) 0.3156(5) 0.0715(16) Uani 1 1 d U . . C71 C 0.0371(2) 1.1242(8) 0.3322(5) 0.073(2) Uani 1 1 d U . . H71 H 0.0372 1.1635 0.3576 0.088 Uiso 1 1 calc R . . C72 C 0.11030(18) 0.9116(5) 0.3765(4) 0.0496(10) Uani 1 1 d U . . C73 C 0.12139(19) 0.7903(6) 0.3399(5) 0.0556(13) Uani 1 1 d U . . H73 H 0.1232 0.7401 0.3457 0.067 Uiso 1 1 calc R . . C74 C 0.1257(2) 0.8167(5) 0.2898(5) 0.0563(13) Uani 1 1 d U . . H74 H 0.1305 0.7845 0.2604 0.068 Uiso 1 1 calc R . . C75 C 0.12369(19) 0.8911(5) 0.2771(4) 0.0535(11) Uani 1 1 d U . . C76 C 0.0379(2) 1.1380(8) 0.2761(5) 0.0755(18) Uani 1 1 d U . . H76 H 0.0373 1.1861 0.2629 0.091 Uiso 1 1 calc R . . C77 C 0.0395(2) 1.0839(8) 0.2398(5) 0.0770(17) Uani 1 1 d U . . H77 H 0.0405 1.0935 0.2008 0.092 Uiso 1 1 calc R . . C79 C -0.0143(3) 1.1378(7) 0.4784(5) 0.077(2) Uani 1 1 d U . . C82 C 0.0397(2) 1.0126(8) 0.2588(5) 0.0760(16) Uani 1 1 d U . . H82 H 0.0410 0.9735 0.2334 0.091 Uiso 1 1 calc R . . C86 C 0.1273(2) 0.2555(5) 0.2865(5) 0.0633(14) Uani 1 1 d U . . H86 H 0.1356 0.2565 0.2500 0.076 Uiso 1 1 calc R . . C87 C 0.0973(2) 0.2741(6) 0.2960(6) 0.0693(14) Uani 1 1 d U . . H87 H 0.0852 0.2853 0.2647 0.083 Uiso 1 1 calc R . . C88 C 0.0854(2) 0.2764(6) 0.3469(6) 0.0741(13) Uani 1 1 d U . . C89 C 0.1015(2) 0.2518(6) 0.3952(6) 0.0703(12) Uani 1 1 d U . . C90 C 0.06017(16) 0.2764(4) 0.4566(3) 0.0864(14) Uani 1 1 d GU . . C91 C 0.08854(16) 0.2493(5) 0.4495(3) 0.0787(13) Uani 1 1 d GU . . C93 C 0.10409(13) 0.2228(4) 0.4952(4) 0.0788(13) Uani 1 1 d GU . . C94 C 0.09127(17) 0.2235(4) 0.5482(3) 0.0886(16) Uani 1 1 d GU . . H94 H 0.1019 0.2054 0.5794 0.106 Uiso 1 1 calc R . . C95 C 0.06290(18) 0.2506(5) 0.5553(3) 0.0934(17) Uani 1 1 d GU . . H95 H 0.0541 0.2511 0.5915 0.112 Uiso 1 1 calc R . . C96 C 0.04735(13) 0.2771(5) 0.5095(4) 0.0941(16) Uani 1 1 d GU . . H96 H 0.0280 0.2957 0.5144 0.113 Uiso 1 1 calc R . . C92 C 0.1339(2) 0.1970(6) 0.4859(6) 0.0703(14) Uani 1 1 d U . . H92 H 0.1444 0.1767 0.5165 0.084 Uiso 1 1 calc R . . C97 C 0.0445(3) 0.3037(7) 0.4080(6) 0.0875(16) Uani 1 1 d U . . H97 H 0.0252 0.3225 0.4137 0.105 Uiso 1 1 calc R . . C98 C 0.0555(2) 0.3044(7) 0.3548(6) 0.0822(15) Uani 1 1 d U . . H98 H 0.0442 0.3222 0.3243 0.099 Uiso 1 1 calc R . . C99 C 0.0070(2) 1.1327(7) 0.5850(5) 0.0752(17) Uani 1 1 d U . . H99 H 0.0152 1.1304 0.6216 0.090 Uiso 1 1 calc R . . C100 C -0.0278(3) 1.1830(7) 0.5178(6) 0.0785(18) Uani 1 1 d U . . H100 H -0.0434 1.2149 0.5084 0.094 Uiso 1 1 calc R . . C101 C -0.0163(3) 1.1771(7) 0.5727(6) 0.0784(18) Uani 1 1 d U . . H101 H -0.0249 1.2047 0.6019 0.094 Uiso 1 1 calc R . . C102 C 0.12866(19) 0.9220(6) 0.2237(5) 0.0572(13) Uani 1 1 d U . . H102 H 0.1334 0.8913 0.1932 0.069 Uiso 1 1 calc R . . C103 C 0.1500(2) 0.3704(6) 0.5967(5) 0.0633(15) Uani 1 1 d U . . H103 H 0.1408 0.3824 0.6313 0.076 Uiso 1 1 calc R . . P1 P 0.32066(7) 0.13041(14) 0.25744(14) 0.0607(7) Uani 1 1 d . . . F7 F 0.33075(14) 0.1780(3) 0.3097(3) 0.0697(16) Uani 1 1 d . . . F8 F 0.34048(16) 0.0667(3) 0.2806(3) 0.093(2) Uani 1 1 d . . . F9 F 0.34877(15) 0.1602(3) 0.2228(3) 0.082(2) Uani 1 1 d . . . F10 F 0.31084(17) 0.0820(3) 0.2072(3) 0.089(2) Uani 1 1 d . . . F11 F 0.30191(15) 0.1953(3) 0.2350(3) 0.0730(18) Uani 1 1 d . . . F12 F 0.29360(13) 0.1042(3) 0.2940(3) 0.0763(18) Uani 1 1 d . . . P2 P 0.15384(6) 0.18781(15) 0.11557(13) 0.0586(7) Uani 1 1 d . . . F1 F 0.16773(17) 0.2060(4) 0.0565(3) 0.099(2) Uani 1 1 d . . . F2 F 0.16083(18) 0.2638(4) 0.1393(3) 0.100(2) Uani 1 1 d . . . F3 F 0.18564(15) 0.1603(4) 0.1375(3) 0.090(2) Uani 1 1 d . . . F4 F 0.14081(17) 0.1659(5) 0.1735(3) 0.105(3) Uani 1 1 d . . . F5 F 0.12305(17) 0.2141(4) 0.0954(4) 0.106(3) Uani 1 1 d . . . F6 F 0.14681(17) 0.1103(3) 0.0931(3) 0.094(2) Uani 1 1 d . . . P3 P 0.0529(2) 0.4072(5) 0.9825(4) 0.100(3) Uiso 0.463(6) 1 d PD A 1 F14 F 0.0820(4) 0.4417(10) 1.0115(8) 0.127(6) Uiso 0.463(6) 1 d PD A 1 F16 F 0.0246(5) 0.3724(12) 0.9521(10) 0.150(8) Uiso 0.463(6) 1 d PD A 1 F18 F 0.0744(6) 0.3861(14) 0.9263(10) 0.199(11) Uiso 0.463(6) 1 d PD A 1 F17 F 0.0680(5) 0.3322(9) 1.0038(10) 0.134(7) Uiso 0.463(6) 1 d PD A 1 F15 F 0.0453(5) 0.4798(11) 0.9573(10) 0.150(8) Uiso 0.463(6) 1 d PD A 1 F13 F 0.0356(5) 0.4138(11) 1.0365(9) 0.150 Uiso 0.463(6) 1 d PD A 1 P3' P 0.4973(3) 0.1969(6) 0.1995(5) 0.162(4) Uiso 0.537(6) 1 d PD A 2 F14' F 0.5303(3) 0.2167(8) 0.1933(8) 0.124(6) Uiso 0.537(6) 1 d PD A 2 F16' F 0.4996(6) 0.1953(11) 0.2638(5) 0.178(8) Uiso 0.537(6) 1 d PD A 2 F17' F 0.4901(7) 0.1915(14) 0.1366(6) 0.233(13) Uiso 0.537(6) 1 d PD A 2 F18' F 0.5076(6) 0.1183(7) 0.1969(12) 0.221(12) Uiso 0.537(6) 1 d PD A 2 F19' F 0.508(2) 0.350(6) 0.188(4) 0.57(6) Uiso 0.537(6) 1 d P A 2 F13' F 0.4874(4) 0.2758(7) 0.1957(8) 0.150 Uiso 0.537(6) 1 d PD 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 Cu1 0.0389(5) 0.0414(5) 0.0299(6) -0.0016(4) 0.0002(5) 0.0047(4) Cu2 0.0334(5) 0.0435(5) 0.0381(6) -0.0036(5) 0.0029(5) 0.0031(4) Cu3 0.0376(6) 0.0922(9) 0.0329(7) -0.0064(6) 0.0013(5) 0.0058(5) S1 0.077(2) 0.142(3) 0.0310(16) -0.0060(16) -0.0008(15) 0.0057(19) S2 0.0528(14) 0.0678(15) 0.0380(15) -0.0056(11) 0.0122(12) 0.0011(11) S3 0.0519(13) 0.0582(13) 0.0343(13) -0.0098(11) 0.0047(11) 0.0060(11) N1 0.032(3) 0.036(3) 0.034(4) -0.003(3) 0.000(3) 0.004(3) N2 0.042(4) 0.030(3) 0.033(4) 0.004(3) -0.003(3) -0.002(3) N3 0.043(4) 0.036(3) 0.033(4) 0.002(3) -0.004(3) 0.004(3) N4 0.035(4) 0.031(3) 0.034(4) 0.002(3) 0.000(3) -0.005(3) N5 0.072(6) 0.057(5) 0.101(8) -0.014(5) 0.004(6) 0.004(4) C20 0.034(3) 0.030(3) 0.040(3) -0.008(3) -0.001(3) 0.005(2) C22 0.045(2) 0.041(2) 0.041(3) -0.008(2) 0.002(2) 0.0002(19) C83 0.055(3) 0.053(3) 0.050(3) -0.012(2) 0.005(3) 0.006(2) C84 0.059(3) 0.061(3) 0.059(3) -0.014(3) 0.005(3) 0.015(3) C85 0.059(4) 0.063(4) 0.061(4) -0.012(3) 0.003(3) 0.021(3) N6 0.042(4) 0.042(4) 0.044(5) -0.009(3) 0.003(4) 0.001(3) N7 0.032(3) 0.042(3) 0.049(5) -0.003(3) 0.004(4) 0.004(3) N8 0.041(4) 0.079(5) 0.035(5) -0.010(4) -0.007(4) -0.007(4) N9 0.041(4) 0.098(6) 0.040(5) 0.003(4) -0.001(4) 0.011(4) N10 0.039(4) 0.044(4) 0.031(4) -0.007(3) 0.001(3) 0.003(3) N11 0.033(4) 0.093(6) 0.044(5) -0.012(5) -0.006(4) 0.004(4) C68 0.040(4) 0.120(5) 0.069(4) -0.019(4) -0.013(4) 0.010(4) C69 0.043(3) 0.123(4) 0.070(4) -0.020(4) -0.011(3) 0.009(3) C78 0.042(3) 0.128(4) 0.070(4) -0.023(3) -0.010(3) 0.008(3) C80 0.039(3) 0.129(4) 0.061(4) -0.024(3) -0.010(3) 0.002(3) C81 0.036(3) 0.127(4) 0.054(3) -0.021(3) -0.009(3) -0.003(3) N12 0.032(4) 0.109(7) 0.037(5) -0.006(5) 0.004(4) 0.007(4) C1 0.036(2) 0.055(3) 0.042(2) 0.008(2) 0.001(2) -0.002(2) C2 0.034(2) 0.050(2) 0.042(2) 0.006(2) 0.002(2) -0.001(2) C3 0.033(2) 0.045(2) 0.040(2) 0.0051(19) 0.0028(19) -0.0015(18) C4 0.034(2) 0.042(2) 0.039(2) 0.0058(19) 0.0012(18) -0.0033(17) C5 0.037(2) 0.046(2) 0.037(2) 0.0067(18) 0.0012(18) -0.0058(18) C6 0.040(2) 0.053(2) 0.039(2) 0.008(2) -0.0005(19) -0.0032(19) C7 0.046(2) 0.052(2) 0.039(2) 0.004(2) 0.000(2) -0.0061(19) C8 0.042(2) 0.045(2) 0.038(2) 0.0048(19) 0.0014(18) -0.0061(18) C9 0.043(2) 0.043(2) 0.040(2) 0.003(2) 0.0014(19) -0.0040(19) C10 0.050(3) 0.046(3) 0.044(3) 0.002(2) 0.005(2) -0.002(2) C11 0.052(3) 0.051(3) 0.044(3) 0.001(2) 0.005(2) -0.003(2) C12 0.051(3) 0.054(3) 0.041(3) 0.004(2) 0.003(2) -0.006(2) C13 0.040(2) 0.037(2) 0.049(3) 0.006(2) -0.004(2) -0.004(2) C14 0.040(2) 0.042(3) 0.052(3) 0.006(2) -0.002(2) -0.003(2) C15 0.041(2) 0.045(3) 0.053(3) 0.005(2) 0.003(2) -0.003(2) C16 0.039(2) 0.044(3) 0.049(3) 0.004(2) 0.008(2) 0.000(2) C17 0.038(2) 0.040(3) 0.043(3) 0.006(2) 0.005(2) 0.005(2) C18 0.045(3) 0.040(3) 0.046(3) 0.005(2) -0.005(2) -0.007(2) C19 0.049(3) 0.043(3) 0.038(3) -0.004(2) 0.000(2) -0.002(2) C23 0.064(3) 0.073(3) 0.045(3) 0.003(3) 0.013(3) 0.013(3) C24 0.060(4) 0.067(4) 0.043(4) 0.005(3) 0.012(3) 0.010(3) C25 0.048(3) 0.064(3) 0.046(3) 0.000(3) 0.010(2) 0.005(3) C26 0.044(3) 0.061(3) 0.048(3) -0.001(3) 0.006(3) 0.007(2) C27 0.044(3) 0.057(3) 0.044(3) 0.002(3) -0.009(2) 0.004(2) C28 0.046(3) 0.064(3) 0.052(3) 0.004(3) -0.007(2) 0.007(3) C29 0.046(3) 0.067(3) 0.057(3) 0.000(3) -0.003(2) 0.007(3) C30 0.033(3) 0.046(3) 0.041(3) 0.005(2) 0.003(2) 0.001(2) C31 0.038(3) 0.051(3) 0.042(3) 0.003(3) 0.003(3) 0.003(3) C32 0.047(3) 0.037(3) 0.036(3) 0.003(3) -0.001(3) 0.005(3) C33 0.051(3) 0.041(3) 0.036(3) 0.001(2) -0.003(3) 0.004(2) C34 0.054(3) 0.102(4) 0.054(4) -0.015(3) 0.015(3) -0.003(3) C35 0.053(4) 0.100(5) 0.050(4) -0.012(4) 0.011(4) -0.004(3) C36 0.048(3) 0.086(4) 0.049(3) 0.002(3) -0.007(3) -0.001(3) C37 0.043(3) 0.080(3) 0.048(3) 0.000(3) -0.006(3) -0.001(3) C38 0.057(3) 0.049(3) 0.041(3) -0.002(2) -0.005(2) -0.003(2) C39 0.059(3) 0.050(3) 0.045(3) 0.003(2) -0.009(2) -0.005(2) C40 0.052(3) 0.045(3) 0.047(3) 0.006(2) -0.010(2) -0.005(2) C41 0.040(2) 0.039(2) 0.041(2) 0.003(2) -0.002(2) -0.002(2) C42 0.037(2) 0.039(2) 0.040(2) 0.004(2) -0.001(2) -0.0009(19) C43 0.058(3) 0.046(3) 0.038(3) -0.003(2) -0.003(2) 0.001(2) C44 0.059(3) 0.050(3) 0.039(3) -0.005(2) -0.006(2) 0.000(3) C45 0.054(3) 0.052(3) 0.041(3) -0.002(3) -0.009(2) -0.002(3) C46 0.048(3) 0.051(3) 0.041(3) -0.001(3) -0.008(2) 0.002(2) C47 0.046(2) 0.058(3) 0.041(3) 0.006(2) -0.003(2) -0.005(2) C48 0.045(3) 0.060(3) 0.041(2) 0.007(2) -0.004(2) -0.002(2) C49 0.045(2) 0.052(3) 0.063(3) -0.010(3) -0.005(2) 0.002(2) C50 0.045(3) 0.051(3) 0.058(4) -0.009(3) -0.007(3) 0.002(3) C51 0.043(2) 0.058(3) 0.072(3) -0.014(2) -0.003(2) -0.001(2) C52 0.039(3) 0.038(3) 0.041(4) 0.006(3) 0.004(3) 0.006(3) C53 0.046(2) 0.064(3) 0.078(3) -0.016(2) 0.002(2) -0.006(2) C54 0.048(3) 0.066(3) 0.075(3) -0.016(3) 0.005(2) -0.011(2) C55 0.045(3) 0.066(3) 0.054(3) -0.002(3) 0.003(3) 0.007(2) C56 0.057(3) 0.073(3) 0.048(3) 0.001(3) 0.013(3) 0.013(3) C57 0.031(2) 0.069(2) 0.050(2) -0.0061(19) -0.007(2) 0.001(2) C58 0.038(2) 0.075(2) 0.050(2) -0.001(2) -0.009(2) 0.002(2) C59 0.030(2) 0.067(2) 0.050(3) -0.009(2) -0.004(2) 0.000(2) C60 0.029(2) 0.068(2) 0.050(3) -0.010(2) -0.002(2) 0.001(2) C61 0.038(3) 0.078(3) 0.053(3) 0.003(2) -0.009(2) 0.006(2) C62 0.037(3) 0.073(3) 0.057(3) 0.003(2) -0.010(2) 0.008(2) C63 0.033(2) 0.070(2) 0.057(2) -0.002(2) -0.005(2) 0.005(2) C64 0.029(2) 0.069(2) 0.052(2) -0.0078(19) -0.001(2) 0.002(2) C65 0.030(2) 0.069(2) 0.050(2) -0.008(2) 0.000(2) 0.001(2) C66 0.034(3) 0.074(3) 0.052(3) -0.006(2) 0.004(2) -0.002(2) C67 0.039(3) 0.079(3) 0.053(3) -0.008(2) 0.004(3) 0.000(3) C70 0.037(3) 0.129(4) 0.048(3) -0.017(3) -0.005(3) -0.006(3) C71 0.044(4) 0.129(5) 0.047(4) -0.007(4) 0.005(4) -0.008(4) C72 0.029(2) 0.068(2) 0.052(2) -0.0054(18) -0.005(2) 0.003(2) C73 0.034(3) 0.071(3) 0.062(3) -0.006(2) -0.003(3) 0.006(2) C74 0.037(3) 0.072(2) 0.060(3) -0.012(2) 0.000(3) 0.005(2) C75 0.034(2) 0.071(2) 0.056(2) -0.012(2) 0.002(2) 0.003(2) C76 0.047(3) 0.132(4) 0.048(3) -0.007(3) 0.003(3) -0.009(4) C77 0.048(3) 0.135(4) 0.048(3) -0.010(3) -0.001(3) -0.012(4) C79 0.054(4) 0.105(5) 0.072(4) -0.011(4) 0.019(4) 0.001(4) C82 0.045(3) 0.134(4) 0.049(3) -0.015(3) -0.002(3) -0.009(3) C86 0.046(2) 0.065(3) 0.079(3) -0.014(3) -0.008(2) -0.001(2) C87 0.047(2) 0.073(3) 0.087(3) -0.016(3) -0.008(2) 0.000(3) C88 0.049(2) 0.079(3) 0.094(3) -0.019(3) 0.000(2) -0.002(2) C89 0.048(2) 0.074(3) 0.088(3) -0.020(3) 0.005(2) -0.006(2) C90 0.059(2) 0.097(3) 0.104(3) -0.021(3) 0.017(2) -0.007(2) C91 0.055(2) 0.086(3) 0.095(3) -0.021(3) 0.014(2) -0.009(2) C93 0.059(2) 0.087(3) 0.090(3) -0.018(3) 0.019(2) -0.013(2) C94 0.069(3) 0.100(3) 0.097(3) -0.018(3) 0.026(3) -0.014(3) C95 0.071(3) 0.106(4) 0.103(4) -0.020(3) 0.028(3) -0.012(3) C96 0.068(3) 0.106(3) 0.108(3) -0.022(3) 0.024(3) -0.010(3) C92 0.055(3) 0.075(3) 0.081(3) -0.016(3) 0.012(2) -0.014(3) C97 0.057(3) 0.097(3) 0.108(3) -0.023(3) 0.011(3) -0.003(3) C98 0.053(3) 0.090(3) 0.103(3) -0.022(3) 0.002(3) 0.001(3) C99 0.058(3) 0.106(4) 0.062(4) -0.017(3) 0.018(3) -0.002(3) C100 0.057(4) 0.106(4) 0.073(4) -0.014(4) 0.018(3) 0.001(3) C101 0.059(3) 0.107(4) 0.070(4) -0.016(3) 0.020(3) -0.001(3) C102 0.039(3) 0.078(3) 0.055(3) -0.012(2) 0.005(3) 0.003(3) C103 0.065(3) 0.077(3) 0.048(3) 0.001(3) 0.013(3) 0.015(3) P1 0.0723(18) 0.0515(14) 0.0583(18) -0.0011(13) 0.0008(15) 0.0022(13) F7 0.078(4) 0.080(4) 0.051(4) -0.008(3) 0.002(3) -0.008(3) F8 0.105(5) 0.068(4) 0.107(6) 0.004(4) 0.008(5) 0.019(4) F9 0.076(4) 0.088(4) 0.082(5) -0.013(4) 0.023(4) -0.012(3) F10 0.117(6) 0.070(4) 0.079(5) -0.019(4) -0.005(4) -0.020(4) F11 0.098(5) 0.062(3) 0.059(4) 0.012(3) -0.001(3) 0.015(3) F12 0.070(4) 0.073(4) 0.085(5) 0.012(3) 0.012(4) -0.006(3) P2 0.0541(15) 0.0747(17) 0.0471(17) -0.0099(13) 0.0009(13) -0.0129(13) F1 0.103(6) 0.130(6) 0.063(5) 0.001(4) 0.003(4) -0.033(5) F2 0.115(6) 0.093(5) 0.093(6) -0.028(4) -0.022(5) -0.017(4) F3 0.070(4) 0.140(6) 0.061(5) -0.019(4) -0.007(4) 0.016(4) F4 0.089(5) 0.166(7) 0.061(5) -0.003(5) 0.023(4) -0.036(5) F5 0.087(5) 0.128(6) 0.103(6) -0.049(5) -0.030(5) 0.020(4) F6 0.100(5) 0.079(4) 0.103(6) -0.028(4) -0.014(5) -0.005(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 C20 2.008(4) . ? Cu1 N1 2.052(7) . ? Cu1 N4 2.067(7) . ? Cu1 N3 2.104(7) . ? Cu1 Cu2 2.9146(13) . ? Cu2 N6 1.987(8) . ? Cu2 N10 2.059(7) . ? Cu2 N7 2.070(6) . ? Cu2 N2 2.069(6) . ? Cu3 N12 1.986(9) . ? Cu3 N8 2.055(8) . ? Cu3 N9 2.073(8) . ? Cu3 N11 2.080(5) . ? Cu3 Cu3 2.910(2) 2_575 ? S1 C35 1.715(13) . ? S1 C36 1.726(11) . ? S2 C31 1.698(10) . ? S2 C32 1.722(9) . ? S3 C50 1.715(9) . ? S3 C52 1.733(9) . ? N1 C33 1.348(11) . ? N1 C46 1.353(11) . ? N2 C13 1.336(10) . ? N2 C17 1.338(11) . ? N3 C32 1.287(11) . ? N3 C30 1.391(11) . ? N4 C18 1.347(11) . ? N4 C19 1.384(11) . ? N5 C20 1.3900 . ? N5 C85 1.3900 . ? C20 C22 1.3900 . ? C22 C83 1.3900 . ? C22 C19 1.440(10) . ? C83 C84 1.3900 . ? C83 H83 0.9500 . ? C84 C85 1.3900 . ? C84 H84 0.9500 . ? C85 H85 0.9500 . ? N6 C24 1.346(13) . ? N6 C25 1.365(11) . ? N7 C26 1.332(11) . ? N7 C27 1.356(12) . ? N8 C35 1.318(13) . ? N8 C37 1.388(12) . ? N9 C79 1.328(14) . ? N9 C34 1.348(14) . ? N10 C52 1.291(10) . ? N10 C49 1.376(11) . ? N11 C68 1.3900 . ? N11 C81 1.3900 . ? C68 C69 1.3900 . ? C68 C79 1.466(14) 2_575 ? C69 C78 1.3900 . ? C69 H69 0.9500 . ? C78 C80 1.3900 . ? C78 H78 0.9500 . ? C80 C81 1.3900 . ? C80 H80 0.9500 . ? C81 C70 1.445(15) . ? N12 C70 1.353(15) . ? N12 C71 1.375(16) . ? C1 C6 1.372(13) . ? C1 C2 1.383(13) . ? C1 H1 0.9500 . ? C2 C3 1.399(12) . ? C2 H2 0.9500 . ? C3 C4 1.401(12) . ? C3 C30 1.497(13) . ? C4 C5 1.412(12) . ? C4 C42 1.448(11) . ? C5 C6 1.406(12) . ? C5 C8 1.421(12) . ? C6 C48 1.477(13) . ? C7 C12 1.424(14) . ? C7 C8 1.453(13) . ? C7 C47 1.459(13) . ? C8 C9 1.423(12) . ? C9 C10 1.376(12) . ? C9 C41 1.424(12) . ? C10 C11 1.409(13) . ? C10 H10 0.9500 . ? C11 C12 1.329(13) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.397(12) . ? C13 C18 1.468(13) . ? C14 C15 1.336(13) . ? C14 H14 0.9500 . ? C15 C16 1.389(13) . ? C15 H15 0.9500 . ? C16 C17 1.418(11) . ? C16 H16 0.9500 . ? C17 C52 1.472(12) . ? C18 C40 1.420(13) . ? C19 C38 1.396(13) . ? C23 C24 1.366(14) . ? C23 C103 1.376(14) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C56 1.397(13) . ? C25 C26 1.433(14) . ? C26 C55 1.429(13) . ? C27 C28 1.401(12) . ? C27 C46 1.480(13) . ? C28 C29 1.379(13) . ? C28 H28 0.9500 . ? C29 C55 1.341(14) . ? C29 H29 0.9500 . ? C30 C31 1.340(12) . ? C31 H31 0.9500 . ? C32 C33 1.481(13) . ? C33 C43 1.394(13) . ? C34 C99 1.392(15) . ? C34 C35 1.462(16) . ? C36 C37 1.379(14) . ? C36 H36 0.9500 . ? C37 C58 1.477(14) . ? C38 C39 1.336(13) . ? C38 H38 0.9500 . ? C39 C40 1.378(14) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C42 1.349(12) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.378(13) . ? C43 H43 0.9500 . ? C44 C45 1.343(13) . ? C44 H44 0.9500 . ? C45 C46 1.407(13) . ? C45 H45 0.9500 . ? C47 C48 1.291(13) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 C50 1.352(14) . ? C49 C51 1.489(13) . ? C50 H50 0.9500 . ? C51 C53 1.373(15) . ? C51 C86 1.454(15) . ? C53 C54 1.437(15) . ? C53 C89 1.471(14) . ? C54 C92 1.352(15) . ? C54 H54 0.9500 . ? C55 H55 0.9500 . ? C56 C103 1.378(14) . ? C56 H56 0.9500 . ? C57 C72 1.415(13) . ? C57 C58 1.410(14) . ? C57 C59 1.442(12) . ? C58 C61 1.404(14) . ? C59 C60 1.333(13) . ? C59 H59 0.9500 . ? C60 C65 1.421(13) . ? C60 H60 0.9500 . ? C61 C62 1.336(14) . ? C61 H61 0.9500 . ? C62 C63 1.398(14) . ? C62 H62 0.9500 . ? C63 C72 1.432(13) . ? C63 C73 1.460(14) . ? C64 C65 1.384(14) . ? C64 C72 1.432(13) . ? C64 C75 1.447(13) . ? C65 C66 1.438(14) . ? C66 C67 1.399(14) . ? C66 H66 0.9500 . ? C67 C102 1.357(15) . ? C67 H67 0.9500 . ? C70 C82 1.375(16) . ? C71 C76 1.365(16) . ? C71 H71 0.9500 . ? C73 C74 1.308(14) . ? C73 H73 0.9500 . ? C74 C75 1.423(14) . ? C74 H74 0.9500 . ? C75 C102 1.417(14) . ? C76 C77 1.331(17) . ? C76 H76 0.9500 . ? C77 C82 1.402(18) . ? C77 H77 0.9500 . ? C79 C100 1.403(16) . ? C79 C68 1.47(3) 2_575 ? C82 H82 0.9500 . ? C86 C87 1.420(14) . ? C86 H86 0.9500 . ? C87 C88 1.330(17) . ? C87 H87 0.9500 . ? C88 C89 1.436(17) . ? C88 C98 1.463(16) . ? C89 C91 1.424(14) . ? C90 C91 1.3900 . ? C90 C96 1.3900 . ? C90 C97 1.452(16) . ? C91 C93 1.3900 . ? C93 C94 1.3900 . ? C93 C92 1.449(12) . ? C94 C95 1.3900 . ? C94 H94 0.9500 . ? C95 C96 1.3900 . ? C95 H95 0.9500 . ? C96 H96 0.9500 . ? C92 H92 0.9500 . ? C97 C98 1.363(19) . ? C97 H97 0.9500 . ? C98 H98 0.9500 . ? C99 C101 1.372(17) . ? C99 H99 0.9500 . ? C100 C101 1.414(18) . ? C100 H100 0.9500 . ? C101 H101 0.9500 . ? C102 H102 0.9500 . ? C103 H103 0.9500 . ? P1 F10 1.566(7) . ? P1 F11 1.571(6) . ? P1 F12 1.581(7) . ? P1 F8 1.586(7) . ? P1 F7 1.596(7) . ? P1 F9 1.615(7) . ? P2 F4 1.559(7) . ? P2 F5 1.553(8) . ? P2 F2 1.557(7) . ? P2 F6 1.573(7) . ? P2 F1 1.581(8) . ? P2 F3 1.614(7) . ? P3 F13 1.51(2) . ? P3 F15 1.52(2) . ? P3 F16 1.61(2) . ? P3 F17 1.64(2) . ? P3 F14 1.620(19) . ? P3 F18 1.71(2) . ? P3' F18' 1.538(3) . ? P3' F16' 1.539(3) . ? P3' F13' 1.539(3) . ? P3' F17' 1.540(3) . ? P3' F14' 1.543(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C20 Cu1 N1 120.7(2) . . ? C20 Cu1 N4 80.5(2) . . ? N1 Cu1 N4 143.5(2) . . ? C20 Cu1 N3 135.6(2) . . ? N1 Cu1 N3 80.6(3) . . ? N4 Cu1 N3 105.4(3) . . ? C20 Cu1 Cu2 103.65(16) . . ? N1 Cu1 Cu2 76.26(18) . . ? N4 Cu1 Cu2 69.52(17) . . ? N3 Cu1 Cu2 119.82(18) . . ? N6 Cu2 N10 135.7(3) . . ? N6 Cu2 N7 81.3(3) . . ? N10 Cu2 N7 104.7(3) . . ? N6 Cu2 N2 122.2(3) . . ? N10 Cu2 N2 81.3(3) . . ? N7 Cu2 N2 139.9(2) . . ? N6 Cu2 Cu1 104.92(19) . . ? N10 Cu2 Cu1 118.4(2) . . ? N7 Cu2 Cu1 69.46(18) . . ? N2 Cu2 Cu1 72.91(16) . . ? N12 Cu3 N8 136.6(3) . . ? N12 Cu3 N9 121.3(3) . . ? N8 Cu3 N9 79.5(3) . . ? N12 Cu3 N11 79.9(3) . . ? N8 Cu3 N11 107.4(3) . . ? N9 Cu3 N11 142.0(3) . . ? N12 Cu3 Cu3 102.7(2) . 2_575 ? N8 Cu3 Cu3 120.1(2) . 2_575 ? N9 Cu3 Cu3 74.9(2) . 2_575 ? N11 Cu3 Cu3 69.41(16) . 2_575 ? C35 S1 C36 90.6(5) . . ? C31 S2 C32 88.3(4) . . ? C50 S3 C52 88.7(4) . . ? C33 N1 C46 117.4(8) . . ? C33 N1 Cu1 114.1(5) . . ? C46 N1 Cu1 128.4(6) . . ? C13 N2 C17 119.2(7) . . ? C13 N2 Cu2 128.6(6) . . ? C17 N2 Cu2 112.0(5) . . ? C32 N3 C30 109.9(8) . . ? C32 N3 Cu1 110.5(6) . . ? C30 N3 Cu1 139.3(6) . . ? C18 N4 C19 118.9(7) . . ? C18 N4 Cu1 125.8(6) . . ? C19 N4 Cu1 112.9(5) . . ? C20 N5 C85 120.0 . . ? N5 C20 C22 120.0 . . ? N5 C20 Cu1 125.2(3) . . ? C22 C20 Cu1 114.4(3) . . ? C83 C22 C20 120.0 . . ? C83 C22 C19 124.1(5) . . ? C20 C22 C19 115.9(5) . . ? C84 C83 C22 120.0 . . ? C84 C83 H83 120.0 . . ? C22 C83 H83 120.0 . . ? C85 C84 C83 120.0 . . ? C85 C84 H84 120.0 . . ? C83 C84 H84 120.0 . . ? C84 C85 N5 120.0 . . ? C84 C85 H85 120.0 . . ? N5 C85 H85 120.0 . . ? C24 N6 C25 119.0(8) . . ? C24 N6 Cu2 127.8(6) . . ? C25 N6 Cu2 112.9(6) . . ? C26 N7 C27 119.8(7) . . ? C26 N7 Cu2 111.4(6) . . ? C27 N7 Cu2 126.5(6) . . ? C35 N8 C37 112.0(9) . . ? C35 N8 Cu3 112.6(7) . . ? C37 N8 Cu3 134.3(7) . . ? C79 N9 C34 116.0(10) . . ? C79 N9 Cu3 129.0(8) . . ? C34 N9 Cu3 114.9(7) . . ? C52 N10 C49 110.7(7) . . ? C52 N10 Cu2 110.8(6) . . ? C49 N10 Cu2 136.7(6) . . ? C68 N11 C81 120.0 . . ? C68 N11 Cu3 125.2(4) . . ? C81 N11 Cu3 112.5(4) . . ? C69 C68 N11 120.0 . . ? C69 C68 C79 123.0(7) . 2_575 ? N11 C68 C79 116.6(7) . 2_575 ? C78 C69 C68 120.0 . . ? C78 C69 H69 120.0 . . ? C68 C69 H69 120.0 . . ? C69 C78 C80 120.0 . . ? C69 C78 H78 120.0 . . ? C80 C78 H78 120.0 . . ? C81 C80 C78 120.0 . . ? C81 C80 H80 120.0 . . ? C78 C80 H80 120.0 . . ? C80 C81 N11 120.0 . . ? C80 C81 C70 126.4(7) . . ? N11 C81 C70 113.6(7) . . ? C70 N12 C71 116.4(10) . . ? C70 N12 Cu3 116.2(9) . . ? C71 N12 Cu3 127.2(8) . . ? C6 C1 C2 120.7(8) . . ? C6 C1 H1 119.6 . . ? C2 C1 H1 119.6 . . ? C1 C2 C3 121.3(8) . . ? C1 C2 H2 119.3 . . ? C3 C2 H2 119.3 . . ? C2 C3 C4 118.9(8) . . ? C2 C3 C30 117.5(8) . . ? C4 C3 C30 123.6(7) . . ? C3 C4 C5 119.0(7) . . ? C3 C4 C42 122.8(8) . . ? C5 C4 C42 118.2(8) . . ? C6 C5 C4 120.7(8) . . ? C6 C5 C8 119.5(8) . . ? C4 C5 C8 119.7(8) . . ? C1 C6 C5 119.1(9) . . ? C1 C6 C48 121.9(8) . . ? C5 C6 C48 119.0(8) . . ? C12 C7 C8 118.1(8) . . ? C12 C7 C47 123.8(9) . . ? C8 C7 C47 118.1(8) . . ? C5 C8 C9 121.6(8) . . ? C5 C8 C7 119.8(8) . . ? C9 C8 C7 118.5(8) . . ? C10 C9 C41 124.2(8) . . ? C10 C9 C8 119.4(9) . . ? C41 C9 C8 116.3(8) . . ? C9 C10 C11 121.8(9) . . ? C9 C10 H10 119.1 . . ? C11 C10 H10 119.1 . . ? C12 C11 C10 120.2(9) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C7 122.0(10) . . ? C11 C12 H12 119.0 . . ? C7 C12 H12 119.0 . . ? N2 C13 C14 121.1(8) . . ? N2 C13 C18 116.4(7) . . ? C14 C13 C18 122.5(8) . . ? C15 C14 C13 120.5(9) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 119.6(8) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C15 C16 C17 117.7(9) . . ? C15 C16 H16 121.2 . . ? C17 C16 H16 121.2 . . ? N2 C17 C16 121.5(8) . . ? N2 C17 C52 114.8(7) . . ? C16 C17 C52 123.7(8) . . ? N4 C18 C40 120.2(8) . . ? N4 C18 C13 116.0(8) . . ? C40 C18 C13 123.9(8) . . ? N4 C19 C38 120.9(8) . . ? N4 C19 C22 114.3(7) . . ? C38 C19 C22 124.8(8) . . ? C24 C23 C103 118.0(10) . . ? C24 C23 H23 121.0 . . ? C103 C23 H23 121.0 . . ? N6 C24 C23 123.3(10) . . ? N6 C24 H24 118.3 . . ? C23 C24 H24 118.3 . . ? N6 C25 C56 119.9(9) . . ? N6 C25 C26 116.8(8) . . ? C56 C25 C26 123.2(9) . . ? N7 C26 C55 121.3(9) . . ? N7 C26 C25 115.8(8) . . ? C55 C26 C25 122.9(9) . . ? N7 C27 C28 120.4(9) . . ? N7 C27 C46 116.9(7) . . ? C28 C27 C46 122.7(9) . . ? C29 C28 C27 119.3(10) . . ? C29 C28 H28 120.4 . . ? C27 C28 H28 120.4 . . ? C55 C29 C28 120.6(9) . . ? C55 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C31 C30 N3 114.4(8) . . ? C31 C30 C3 124.3(8) . . ? N3 C30 C3 121.1(8) . . ? C30 C31 S2 111.6(7) . . ? C30 C31 H31 124.2 . . ? S2 C31 H31 124.2 . . ? N3 C32 C33 121.1(8) . . ? N3 C32 S2 115.7(7) . . ? C33 C32 S2 123.2(7) . . ? N1 C33 C43 122.3(8) . . ? N1 C33 C32 113.6(8) . . ? C43 C33 C32 124.1(9) . . ? N9 C34 C99 124.7(11) . . ? N9 C34 C35 112.6(9) . . ? C99 C34 C35 122.3(11) . . ? N8 C35 C34 119.9(11) . . ? N8 C35 S1 113.7(8) . . ? C34 C35 S1 126.3(9) . . ? C37 C36 S1 109.5(8) . . ? C37 C36 H36 125.2 . . ? S1 C36 H36 125.2 . . ? C36 C37 N8 114.1(9) . . ? C36 C37 C58 126.7(9) . . ? N8 C37 C58 119.0(9) . . ? C39 C38 C19 120.1(9) . . ? C39 C38 H38 119.9 . . ? C19 C38 H38 119.9 . . ? C38 C39 C40 120.2(10) . . ? C38 C39 H39 119.9 . . ? C40 C39 H39 119.9 . . ? C39 C40 C18 119.5(9) . . ? C39 C40 H40 120.2 . . ? C18 C40 H40 120.2 . . ? C42 C41 C9 123.3(8) . . ? C42 C41 H41 118.4 . . ? C9 C41 H41 118.4 . . ? C41 C42 C4 120.6(8) . . ? C41 C42 H42 119.7 . . ? C4 C42 H42 119.7 . . ? C33 C43 C44 119.4(9) . . ? C33 C43 H43 120.3 . . ? C44 C43 H43 120.3 . . ? C45 C44 C43 118.9(9) . . ? C45 C44 H44 120.5 . . ? C43 C44 H44 120.5 . . ? C44 C45 C46 120.1(9) . . ? C44 C45 H45 120.0 . . ? C46 C45 H45 120.0 . . ? N1 C46 C45 121.7(9) . . ? N1 C46 C27 116.1(8) . . ? C45 C46 C27 122.3(8) . . ? C48 C47 C7 121.4(9) . . ? C48 C47 H47 119.3 . . ? C7 C47 H47 119.3 . . ? C47 C48 C6 122.1(9) . . ? C47 C48 H48 118.9 . . ? C6 C48 H48 118.9 . . ? C50 C49 N10 115.3(8) . . ? C50 C49 C51 125.8(9) . . ? N10 C49 C51 118.8(8) . . ? C49 C50 S3 110.3(7) . . ? C49 C50 H50 124.9 . . ? S3 C50 H50 124.9 . . ? C53 C51 C86 121.0(9) . . ? C53 C51 C49 124.1(10) . . ? C86 C51 C49 114.9(10) . . ? N10 C52 C17 120.2(8) . . ? N10 C52 S3 114.9(6) . . ? C17 C52 S3 124.9(6) . . ? C51 C53 C54 124.1(9) . . ? C51 C53 C89 119.4(11) . . ? C54 C53 C89 116.4(10) . . ? C92 C54 C53 121.8(10) . . ? C92 C54 H54 119.1 . . ? C53 C54 H54 119.1 . . ? C29 C55 C26 118.6(10) . . ? C29 C55 H55 120.7 . . ? C26 C55 H55 120.7 . . ? C103 C56 C25 119.3(9) . . ? C103 C56 H56 120.4 . . ? C25 C56 H56 120.4 . . ? C72 C57 C58 118.1(9) . . ? C72 C57 C59 119.2(9) . . ? C58 C57 C59 122.7(9) . . ? C61 C58 C57 119.8(9) . . ? C61 C58 C37 118.6(9) . . ? C57 C58 C37 121.5(9) . . ? C60 C59 C57 120.0(9) . . ? C60 C59 H59 120.0 . . ? C57 C59 H59 120.0 . . ? C59 C60 C65 122.1(9) . . ? C59 C60 H60 118.9 . . ? C65 C60 H60 118.9 . . ? C62 C61 C58 121.1(10) . . ? C62 C61 H61 119.4 . . ? C58 C61 H61 119.4 . . ? C61 C62 C63 122.4(10) . . ? C61 C62 H62 118.8 . . ? C63 C62 H62 118.8 . . ? C62 C63 C72 117.5(9) . . ? C62 C63 C73 124.8(9) . . ? C72 C63 C73 117.6(9) . . ? C65 C64 C72 120.0(9) . . ? C65 C64 C75 121.1(9) . . ? C72 C64 C75 118.9(9) . . ? C64 C65 C60 119.5(9) . . ? C64 C65 C66 119.9(9) . . ? C60 C65 C66 120.5(9) . . ? C67 C66 C65 118.3(10) . . ? C67 C66 H66 120.8 . . ? C65 C66 H66 120.8 . . ? C102 C67 C66 121.7(11) . . ? C102 C67 H67 119.1 . . ? C66 C67 H67 119.1 . . ? N12 C70 C82 123.3(13) . . ? N12 C70 C81 116.2(10) . . ? C82 C70 C81 120.4(11) . . ? C76 C71 N12 122.4(12) . . ? C76 C71 H71 118.8 . . ? N12 C71 H71 118.8 . . ? C57 C72 C64 119.0(9) . . ? C57 C72 C63 120.6(9) . . ? C64 C72 C63 120.3(9) . . ? C74 C73 C63 121.4(10) . . ? C74 C73 H73 119.3 . . ? C63 C73 H73 119.3 . . ? C73 C74 C75 123.5(10) . . ? C73 C74 H74 118.2 . . ? C75 C74 H74 118.2 . . ? C102 C75 C74 125.2(9) . . ? C102 C75 C64 116.6(9) . . ? C74 C75 C64 118.1(10) . . ? C77 C76 C71 119.9(14) . . ? C77 C76 H76 120.1 . . ? C71 C76 H76 120.1 . . ? C76 C77 C82 120.4(12) . . ? C76 C77 H77 119.8 . . ? C82 C77 H77 119.8 . . ? N9 C79 C100 126.0(12) . . ? N9 C79 C68 117.2(10) . 2_575 ? C100 C79 C68 116.7(11) . 2_575 ? C70 C82 C77 117.4(13) . . ? C70 C82 H82 121.3 . . ? C77 C82 H82 121.3 . . ? C87 C86 C51 117.4(11) . . ? C87 C86 H86 121.3 . . ? C51 C86 H86 121.3 . . ? C88 C87 C86 122.8(12) . . ? C88 C87 H87 118.6 . . ? C86 C87 H87 118.6 . . ? C87 C88 C89 121.1(10) . . ? C87 C88 C98 120.2(13) . . ? C89 C88 C98 118.6(12) . . ? C91 C89 C88 122.2(9) . . ? C91 C89 C53 120.0(11) . . ? C88 C89 C53 117.8(11) . . ? C91 C90 C96 120.0 . . ? C91 C90 C97 118.6(7) . . ? C96 C90 C97 121.4(7) . . ? C90 C91 C93 120.0 . . ? C90 C91 C89 118.6(7) . . ? C93 C91 C89 121.3(7) . . ? C91 C93 C94 120.0 . . ? C91 C93 C92 117.9(8) . . ? C94 C93 C92 122.1(8) . . ? C95 C94 C93 120.0 . . ? C95 C94 H94 120.0 . . ? C93 C94 H94 120.0 . . ? C94 C95 C96 120.0 . . ? C94 C95 H95 120.0 . . ? C96 C95 H95 120.0 . . ? C95 C96 C90 120.0 . . ? C95 C96 H96 120.0 . . ? C90 C96 H96 120.0 . . ? C54 C92 C93 122.3(12) . . ? C54 C92 H92 118.8 . . ? C93 C92 H92 118.8 . . ? C98 C97 C90 124.9(11) . . ? C98 C97 H97 117.6 . . ? C90 C97 H97 117.6 . . ? C97 C98 C88 116.9(13) . . ? C97 C98 H98 121.6 . . ? C88 C98 H98 121.6 . . ? C101 C99 C34 116.8(12) . . ? C101 C99 H99 121.6 . . ? C34 C99 H99 121.6 . . ? C79 C100 C101 114.5(12) . . ? C79 C100 H100 122.7 . . ? C101 C100 H100 122.7 . . ? C99 C101 C100 121.9(12) . . ? C99 C101 H101 119.1 . . ? C100 C101 H101 119.1 . . ? C67 C102 C75 122.3(10) . . ? C67 C102 H102 118.9 . . ? C75 C102 H102 118.9 . . ? C23 C103 C56 120.5(10) . . ? C23 C103 H103 119.8 . . ? C56 C103 H103 119.8 . . ? F10 P1 F11 91.7(4) . . ? F10 P1 F12 91.5(4) . . ? F11 P1 F12 90.4(4) . . ? F10 P1 F8 89.8(4) . . ? F11 P1 F8 178.0(4) . . ? F12 P1 F8 90.8(4) . . ? F10 P1 F7 178.5(4) . . ? F11 P1 F7 89.6(4) . . ? F12 P1 F7 87.8(4) . . ? F8 P1 F7 88.9(4) . . ? F10 P1 F9 91.6(4) . . ? F11 P1 F9 89.2(4) . . ? F12 P1 F9 176.9(4) . . ? F8 P1 F9 89.5(4) . . ? F7 P1 F9 89.1(4) . . ? F4 P2 F5 91.1(5) . . ? F4 P2 F2 89.5(5) . . ? F5 P2 F2 90.4(4) . . ? F4 P2 F6 89.2(5) . . ? F5 P2 F6 90.2(4) . . ? F2 P2 F6 178.6(5) . . ? F4 P2 F1 177.1(5) . . ? F5 P2 F1 90.7(5) . . ? F2 P2 F1 92.8(4) . . ? F6 P2 F1 88.4(4) . . ? F4 P2 F3 88.1(4) . . ? F5 P2 F3 179.1(5) . . ? F2 P2 F3 89.4(4) . . ? F6 P2 F3 90.0(4) . . ? F1 P2 F3 90.2(4) . . ? F13 P3 F15 98.5(13) . . ? F13 P3 F16 90.4(12) . . ? F15 P3 F16 90.1(13) . . ? F13 P3 F17 91.3(12) . . ? F15 P3 F17 167.6(14) . . ? F16 P3 F17 97.5(12) . . ? F13 P3 F14 91.4(11) . . ? F15 P3 F14 89.8(12) . . ? F16 P3 F14 178.3(13) . . ? F17 P3 F14 82.3(11) . . ? F13 P3 F18 170.2(14) . . ? F15 P3 F18 91.2(13) . . ? F16 P3 F18 90.3(12) . . ? F17 P3 F18 79.0(12) . . ? F14 P3 F18 87.9(11) . . ? F18' P3' F16' 90.0(13) . . ? F18' P3' F13' 174.3(15) . . ? F16' P3' F13' 95.6(12) . . ? F18' P3' F17' 87.9(14) . . ? F16' P3' F17' 170.2(17) . . ? F13' P3' F17' 86.7(13) . . ? F18' P3' F14' 86.2(12) . . ? F16' P3' F14' 92.0(14) . . ? F13' P3' F14' 92.8(10) . . ? F17' P3' F14' 97.4(14) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.31 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.057 _refine_diff_density_min -0.617 _refine_diff_density_rms 0.108 # start Validation Reply Form _vrf_PUBL004_GLOBAL ; PROBLEM: The contact author's name and address are missing, RESPONSE: ... ; _vrf_PUBL005_GLOBAL ; PROBLEM: _publ_contact_author_email, _publ_contact_author_fax and RESPONSE: ... ; _vrf_PUBL006_GLOBAL ; PROBLEM: _publ_requested_journal is missing RESPONSE: ... ; _vrf_PUBL008_GLOBAL ; PROBLEM: _publ_section_title is missing. Title of paper. RESPONSE: ... ; _vrf_PUBL009_GLOBAL ; PROBLEM: _publ_author_name is missing. List of author(s) name(s). RESPONSE: ... ; _vrf_PUBL010_GLOBAL ; PROBLEM: _publ_author_address is missing. Author(s) address(es). RESPONSE: ... ; _vrf_PUBL012_GLOBAL ; PROBLEM: _publ_section_abstract is missing. RESPONSE: ... ; _vrf_PLAT601_I ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 580 A**3 RESPONSE: ... The crystals where highly solvated and during inspection the crystals appeared to decompose. ; # end Validation Reply Form data_I _database_code_depnum_ccdc_archive 'CCDC 845595' #TrackingRef 'Report_CddiPyrene_final.doc' _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H29 Cd Cl2 N5 O10 S2' _chemical_formula_iupac ? _chemical_formula_weight 1095.19 _chemical_melting_point ? _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.2402(8) _cell_length_b 10.3881(4) _cell_length_c 20.5791(7) _cell_angle_alpha 90 _cell_angle_beta 101.4650(10) _cell_angle_gamma 90 _cell_volume 4240.6(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9910 _cell_measurement_theta_min 2.5783 _cell_measurement_theta_max 28.2904 _cell_measurement_temperature 101.(2) _exptl_crystal_description ? _exptl_crystal_colour 'clear yellow' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.350 _exptl_crystal_size_min 0.070 _exptl_crystal_density_diffrn 1.715 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 0.812 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS)' _exptl_absorpt_correction_T_min 0.82 _exptl_absorpt_correction_T_max 0.95 _exptl_special_details ; ; _diffrn_ambient_temperature 101.(2) _diffrn_source ? _diffrn_source_type ? _diffrn_radiation_type ? _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 8.3333 _diffrn_reflns_number 38944 _diffrn_reflns_av_R_equivalents 0.0483 _diffrn_reflns_av_sigmaI/netI 0.0435 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 27.88 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _reflns_number_total 10120 _reflns_number_gt 8049 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0490 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_gt 0.0800 _refine_ls_wR_factor_ref 0.0890 _refine_ls_goodness_of_fit_ref 0.950 _refine_ls_restrained_S_all 0.950 _refine_ls_number_reflns 10120 _refine_ls_number_parameters 623 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0462P)^2^+2.7365P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.637 _refine_diff_density_min -0.653 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection 'Bruker Instrument Service v2009, 9, 0, 0' _computing_cell_refinement 'SAINT V7.68A (Bruker AXS, 2009)' _computing_data_reduction 'SAINT V7.68A (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cd Cd1 0.32465(9) 0.193871(16) 0.477808(8) 0.02163(6) Uani d . 1 . . Cl Cl1 0.40704(4) 0.41281(6) 0.38259(3) 0.03402(15) Uani d . 1 . . Cl Cl2 0.23259(3) -0.05805(6) 0.52965(3) 0.02570(13) Uani d . 1 . . S S2 0.23528(3) 0.60741(6) 0.47858(3) 0.02961(15) Uani d . 1 . . S S1 0.40886(3) -0.22137(6) 0.46374(3) 0.02941(14) Uani d . 1 . . O O1 0.40700(10) 0.30765(19) 0.42908(10) 0.0388(5) Uani d . 1 . . O O2 0.44490(16) 0.5164(2) 0.41429(15) 0.0775(9) Uani d . 1 . . O O3 0.33874(13) 0.4531(3) 0.35888(14) 0.0734(9) Uani d . 1 . . O O4 0.43525(11) 0.3665(2) 0.32870(10) 0.0466(5) Uani d . 1 . . O O5 0.25129(10) 0.07895(17) 0.53599(9) 0.0318(4) Uani d . 1 . . O O6 0.21014(11) -0.08776(19) 0.46099(9) 0.0396(5) Uani d . 1 . . O O7 0.29163(10) -0.13283(18) 0.55675(10) 0.0365(4) Uani d . 1 . . O O8 0.18079(11) -0.0806(2) 0.56594(11) 0.0455(5) Uani d . 1 . . O O9 0.6838(2) 0.2685(4) 0.7774(2) 0.1291(17) Uani d . 1 . . O O10 0.58618(14) 0.3353(3) 0.77705(16) 0.0745(8) Uani d . 1 . . N N7 0.41393(10) 0.11276(19) 0.55731(10) 0.0235(4) Uani d . 1 . . N N9 0.25521(10) 0.36827(19) 0.46196(10) 0.0216(4) Uani d . 1 . . C C1' 0.20277(12) 0.4031(2) 0.41134(12) 0.0225(5) Uani d . 1 . . N N8 0.36109(10) 0.33859(19) 0.56453(10) 0.0230(4) Uani d . 1 . . N N6 0.35783(10) 0.00235(19) 0.44034(10) 0.0218(4) Uani d . 1 . . C C4 0.43380(12) -0.0074(2) 0.54864(12) 0.0242(5) Uani d . 1 . . C C5 0.48300(13) -0.0677(3) 0.59580(13) 0.0310(6) Uani d . 1 . . H H2A 0.497 -0.1533 0.5894 0.037 Uiso calc R 1 . . C C6 0.51065(14) 0.0010(3) 0.65209(13) 0.0356(6) Uani d . 1 . . H H3 0.544 -0.0379 0.6853 0.043 Uiso calc R 1 . . C C7 0.49021(13) 0.1265(3) 0.66075(13) 0.0320(6) Uani d . 1 . . H H4 0.5096 0.1744 0.6992 0.038 Uiso calc R 1 . . C C8 0.44073(12) 0.1801(2) 0.61175(12) 0.0246(5) Uani d . 1 . . C C9 0.41297(12) 0.3126(2) 0.61389(12) 0.0247(5) Uani d . 1 . . C C10 0.43784(14) 0.4053(3) 0.66121(13) 0.0336(6) Uani d . 1 . . H H7 0.4746 0.3864 0.6964 0.04 Uiso calc R 1 . . C C11 0.40783(15) 0.5255(3) 0.65584(14) 0.0385(7) Uani d . 1 . . H H8 0.4243 0.5903 0.6875 0.046 Uiso calc R 1 . . C C12 0.35367(14) 0.5521(3) 0.60435(13) 0.0327(6) Uani d . 1 . . H H9 0.3321 0.6337 0.6004 0.039 Uiso calc R 1 . . C C13 0.33246(12) 0.4543(2) 0.55903(12) 0.0239(5) Uani d . 1 . . C C14 0.27664(12) 0.4662(2) 0.50127(12) 0.0226(5) Uani d . 1 . . C C32 0.16577(12) 0.3057(2) 0.36654(12) 0.0226(5) Uani d . 1 . . C C45 0.14823(13) 0.1903(2) 0.39373(13) 0.0271(5) Uani d . 1 . . H H13 0.1659 0.1718 0.4391 0.033 Uiso calc R 1 . . C C44 0.10555(13) 0.1023(2) 0.35584(13) 0.0285(5) Uani d . 1 . . H H14 0.096 0.0229 0.3749 0.034 Uiso calc R 1 . . C C43 0.07655(12) 0.1293(2) 0.29020(13) 0.0248(5) Uani d . 1 . . C C46 0.09479(11) 0.2443(2) 0.26066(12) 0.0220(5) Uani d . 1 . . C C47 0.06423(12) 0.2750(2) 0.19353(12) 0.0236(5) Uani d . 1 . . C C36 0.08421(13) 0.3864(2) 0.16368(12) 0.0274(5) Uani d . 1 . . C C37 0.05094(15) 0.4186(3) 0.09883(13) 0.0352(6) Uani d . 1 . . H H19 0.0641 0.4932 0.0779 0.042 Uiso calc R 1 . . C C38 -0.00050(16) 0.3425(3) 0.06582(14) 0.0413(7) Uani d . 1 . . H H20 -0.0236 0.3668 0.0228 0.05 Uiso calc R 1 . . C C39 -0.01927(14) 0.2311(3) 0.09422(14) 0.0380(7) Uani d . 1 . . H H21 -0.0544 0.1792 0.0701 0.046 Uiso calc R 1 . . C C40 0.01277(12) 0.1940(2) 0.15803(13) 0.0282(5) Uani d . 1 . . C C41 -0.00331(12) 0.0781(3) 0.18896(14) 0.0314(6) Uani d . 1 . . H H23 -0.0366 0.0222 0.165 0.038 Uiso calc R 1 . . C C42 0.02728(13) 0.0460(2) 0.25089(14) 0.0292(6) Uani d . 1 . . H H24 0.0162 -0.0333 0.2691 0.035 Uiso calc R 1 . . C C35 0.13694(13) 0.4646(2) 0.20033(12) 0.0275(5) Uani d . 1 . . H H25 0.1531 0.5359 0.1792 0.033 Uiso calc R 1 . . C C34 0.16420(12) 0.4391(2) 0.26446(13) 0.0257(5) Uani d . 1 . . H H26 0.1986 0.4936 0.2877 0.031 Uiso calc R 1 . . C C33 0.14206(11) 0.3310(2) 0.29825(12) 0.0219(5) Uani d . 1 . . C C15 0.18629(13) 0.5303(2) 0.41317(13) 0.0285(5) Uani d . 1 . . H H28 0.1518 0.5708 0.3818 0.034 Uiso calc R 1 . . C C3 0.39962(12) -0.0645(2) 0.48538(12) 0.0243(5) Uani d . 1 . . C C2 0.35407(13) -0.1949(2) 0.39040(13) 0.0284(5) Uani d . 1 . . H H30 0.3406 -0.2588 0.3574 0.034 Uiso calc R 1 . . C C1 0.33192(12) -0.0700(2) 0.38511(12) 0.0235(5) Uani d . 1 . . C C16 0.29353(12) -0.0059(2) 0.32495(12) 0.0232(5) Uani d . 1 . . C C29 0.31935(13) 0.1108(2) 0.30706(13) 0.0274(5) Uani d . 1 . . H H33 0.3557 0.1504 0.3367 0.033 Uiso calc R 1 . . C C28 0.29318(13) 0.1700(2) 0.24720(14) 0.0290(5) Uani d . 1 . . H H34 0.3117 0.2494 0.2364 0.035 Uiso calc R 1 . . C C27 0.24002(13) 0.1143(2) 0.20277(12) 0.0262(5) Uani d . 1 . . C C30 0.21101(12) -0.0013(2) 0.22112(12) 0.0226(5) Uani d . 1 . . C C17 0.23680(12) -0.0601(2) 0.28367(12) 0.0227(5) Uani d . 1 . . C C18 0.20165(13) -0.1701(2) 0.30246(13) 0.0265(5) Uani d . 1 . . H H38 0.2167 -0.2084 0.3447 0.032 Uiso calc R 1 . . C C19 0.14752(14) -0.2199(2) 0.26092(14) 0.0308(6) Uani d . 1 . . H H39 0.1249 -0.2914 0.2752 0.037 Uiso calc R 1 . . C C20 0.12327(13) -0.1683(2) 0.19617(13) 0.0300(6) Uani d . 1 . . C C31 0.15557(13) -0.0578(2) 0.17657(12) 0.0256(5) Uani d . 1 . . C C24 0.13129(13) -0.0008(3) 0.11360(13) 0.0312(6) Uani d . 1 . . C C23 0.07628(15) -0.0577(3) 0.07112(14) 0.0397(7) Uani d . 1 . . H H43 0.0603 -0.0224 0.0283 0.048 Uiso calc R 1 . . C C22 0.04504(15) -0.1650(3) 0.09119(15) 0.0425(7) Uani d . 1 . . H H44 0.0073 -0.2014 0.0622 0.051 Uiso calc R 1 . . C C21 0.06774(14) -0.2199(3) 0.15241(15) 0.0374(7) Uani d . 1 . . H H45 0.0455 -0.2936 0.1651 0.045 Uiso calc R 1 . . C C25 0.16243(14) 0.1144(3) 0.09648(14) 0.0356(6) Uani d . 1 . . H H46 0.1466 0.1525 0.0543 0.043 Uiso calc R 1 . . C C26 0.21364(14) 0.1703(3) 0.13878(14) 0.0319(6) Uani d . 1 . . H H47 0.2327 0.2478 0.1263 0.038 Uiso calc R 1 . . N N10 0.64479(15) 0.3527(3) 0.78309(13) 0.0466(7) Uani d . 1 . . C C49 0.6707(2) 0.4821(4) 0.79844(18) 0.0711(13) Uani d . 1 . . H H49A 0.6479 0.5421 0.7645 0.107 Uiso calc R 1 . . H H49B 0.7193 0.4834 0.7992 0.107 Uiso calc R 1 . . H H49C 0.6625 0.5082 0.8419 0.107 Uiso calc R 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cd1 0.02524(9) 0.01632(9) 0.02108(9) 0.00318(7) -0.00088(6) -0.00135(7) Cl1 0.0440(4) 0.0239(3) 0.0370(3) -0.0020(3) 0.0150(3) 0.0016(3) Cl2 0.0331(3) 0.0200(3) 0.0249(3) 0.0008(2) 0.0079(2) 0.0005(2) S2 0.0364(3) 0.0159(3) 0.0334(3) 0.0042(2) -0.0007(3) -0.0025(2) S1 0.0372(3) 0.0186(3) 0.0330(3) 0.0073(2) 0.0085(3) 0.0020(2) O1 0.0430(11) 0.0344(11) 0.0413(11) 0.0005(9) 0.0136(9) 0.0099(9) O2 0.113(2) 0.0412(14) 0.087(2) -0.0354(15) 0.0392(18) -0.0277(14) O3 0.0567(16) 0.095(2) 0.0745(18) 0.0321(15) 0.0278(14) 0.0421(17) O4 0.0519(13) 0.0542(14) 0.0376(12) -0.0029(11) 0.0185(10) -0.0026(10) O5 0.0429(11) 0.0195(9) 0.0348(10) 0.0002(8) 0.0120(8) -0.0022(8) O6 0.0553(13) 0.0312(11) 0.0279(10) 0.0028(9) -0.0025(9) -0.0033(8) O7 0.0418(11) 0.0274(10) 0.0382(11) 0.0059(8) 0.0026(9) 0.0018(8) O8 0.0472(12) 0.0438(12) 0.0531(13) -0.0040(10) 0.0283(11) 0.0026(11) O9 0.163(4) 0.122(3) 0.118(3) 0.084(3) 0.066(3) -0.005(3) O10 0.0549(17) 0.0672(18) 0.094(2) -0.0150(14) -0.0033(15) 0.0022(16) N7 0.0251(10) 0.0234(10) 0.0214(10) 0.0020(8) 0.0032(8) 0.0020(8) N9 0.0252(10) 0.0180(10) 0.0206(10) 0.0006(8) 0.0025(8) 0.0004(8) C1' 0.0230(11) 0.0198(11) 0.0229(11) 0.0001(9) 0.0005(9) -0.0001(9) N8 0.0247(10) 0.0234(10) 0.0199(10) -0.0013(8) 0.0021(8) -0.0019(8) N6 0.0241(10) 0.0183(10) 0.0231(10) 0.0016(8) 0.0049(8) -0.0001(8) C4 0.0258(12) 0.0237(12) 0.0243(12) 0.0019(9) 0.0076(10) 0.0049(10) C5 0.0323(14) 0.0317(14) 0.0296(13) 0.0118(11) 0.0074(11) 0.0062(11) C6 0.0297(13) 0.0463(17) 0.0281(14) 0.0133(12) -0.0007(11) 0.0079(12) C7 0.0295(13) 0.0397(16) 0.0243(13) 0.0032(11) -0.0003(10) 0.0042(11) C8 0.0217(11) 0.0302(13) 0.0207(11) -0.0011(10) 0.0014(9) 0.0016(10) C9 0.0262(12) 0.0276(13) 0.0194(11) -0.0022(10) 0.0025(9) 0.0007(10) C10 0.0345(14) 0.0366(15) 0.0255(13) -0.0039(12) -0.0038(11) -0.0041(12) C11 0.0455(17) 0.0328(15) 0.0325(15) -0.0048(12) -0.0039(13) -0.0113(12) C12 0.0415(15) 0.0218(13) 0.0319(14) -0.0015(11) 0.0001(12) -0.0067(11) C13 0.0281(12) 0.0217(12) 0.0218(11) -0.0016(9) 0.0048(10) -0.0020(9) C14 0.0265(12) 0.0195(11) 0.0215(11) -0.0001(9) 0.0042(9) -0.0007(9) C32 0.0209(11) 0.0172(11) 0.0281(12) 0.0024(9) 0.0008(9) -0.0010(9) C45 0.0280(12) 0.0226(12) 0.0287(13) 0.0020(10) 0.0006(10) 0.0035(10) C44 0.0297(13) 0.0197(12) 0.0353(14) 0.0005(10) 0.0047(11) 0.0040(10) C43 0.0211(11) 0.0222(12) 0.0309(13) 0.0020(9) 0.0049(10) -0.0037(10) C46 0.0195(11) 0.0189(11) 0.0273(12) 0.0027(9) 0.0040(9) -0.0035(10) C47 0.0210(11) 0.0246(12) 0.0250(12) 0.0027(9) 0.0045(9) -0.0060(10) C36 0.0295(13) 0.0281(13) 0.0251(12) 0.0038(10) 0.0067(10) -0.0018(10) C37 0.0446(16) 0.0338(15) 0.0263(13) 0.0022(12) 0.0051(12) 0.0021(11) C38 0.0473(17) 0.0473(18) 0.0247(14) 0.0024(14) -0.0037(12) -0.0002(13) C39 0.0342(15) 0.0446(17) 0.0314(14) -0.0016(13) -0.0023(12) -0.0114(13) C40 0.0245(12) 0.0298(13) 0.0296(13) 0.0021(10) 0.0038(10) -0.0065(11) C41 0.0224(12) 0.0317(14) 0.0394(15) -0.0046(10) 0.0044(11) -0.0109(12) C42 0.0265(12) 0.0223(12) 0.0404(15) -0.0034(10) 0.0109(11) -0.0042(11) C35 0.0333(13) 0.0219(12) 0.0278(13) 0.0003(10) 0.0071(11) 0.0018(10) C34 0.0255(12) 0.0184(12) 0.0326(13) -0.0005(9) 0.0047(10) -0.0022(10) C33 0.0204(11) 0.0183(11) 0.0263(12) 0.0039(9) 0.0029(9) -0.0002(9) C15 0.0301(13) 0.0211(12) 0.0308(13) 0.0041(10) -0.0026(10) 0.0001(10) C3 0.0264(12) 0.0182(11) 0.0295(12) 0.0026(9) 0.0082(10) 0.0012(10) C2 0.0338(13) 0.0216(12) 0.0296(13) 0.0018(10) 0.0063(11) -0.0023(10) C1 0.0247(12) 0.0201(12) 0.0268(12) -0.0008(9) 0.0079(10) -0.0020(10) C16 0.0281(12) 0.0180(11) 0.0242(12) 0.0030(9) 0.0067(10) -0.0037(9) C29 0.0298(13) 0.0229(12) 0.0298(13) -0.0017(10) 0.0065(10) -0.0037(10) C28 0.0316(13) 0.0206(12) 0.0366(14) -0.0004(10) 0.0114(11) 0.0028(11) C27 0.0304(13) 0.0240(12) 0.0263(12) 0.0055(10) 0.0111(10) 0.0019(10) C30 0.0248(11) 0.0211(12) 0.0233(12) 0.0034(9) 0.0078(9) -0.0016(9) C17 0.0270(12) 0.0185(11) 0.0240(12) 0.0024(9) 0.0080(10) -0.0035(9) C18 0.0346(13) 0.0193(12) 0.0263(12) 0.0003(10) 0.0080(10) 0.0003(10) C19 0.0338(14) 0.0218(13) 0.0374(14) -0.0038(10) 0.0086(11) -0.0030(11) C20 0.0309(13) 0.0258(13) 0.0328(14) 0.0014(10) 0.0054(11) -0.0089(11) C31 0.0279(12) 0.0245(12) 0.0251(12) 0.0043(10) 0.0074(10) -0.0045(10) C24 0.0301(13) 0.0367(15) 0.0271(13) 0.0080(11) 0.0065(11) -0.0036(11) C23 0.0389(16) 0.0485(18) 0.0283(14) 0.0088(13) -0.0009(12) -0.0073(13) C22 0.0386(16) 0.0444(18) 0.0394(16) 0.0009(13) -0.0043(13) -0.0160(14) C21 0.0356(15) 0.0303(15) 0.0441(17) -0.0006(11) 0.0027(13) -0.0102(13) C25 0.0376(15) 0.0434(17) 0.0275(13) 0.0112(13) 0.0107(12) 0.0067(12) C26 0.0353(14) 0.0307(14) 0.0328(14) 0.0069(11) 0.0138(11) 0.0072(11) N10 0.0552(17) 0.0547(17) 0.0304(13) 0.0092(14) 0.0096(12) 0.0019(12) C49 0.090(3) 0.069(3) 0.043(2) -0.035(2) -0.011(2) 0.0174(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cd1 N9 . 2.2763(19) ? Cd1 N6 . 2.2825(19) ? Cd1 N8 . 2.338(2) ? Cd1 N7 . 2.3402(19) ? Cd1 O5 . 2.4022(19) ? Cd1 O1 . 2.418(2) ? Cl1 O2 . 1.405(2) ? Cl1 O4 . 1.428(2) ? Cl1 O3 . 1.434(3) ? Cl1 O1 . 1.452(2) ? Cl2 O8 . 1.422(2) ? Cl2 O6 . 1.4294(19) ? Cl2 O7 . 1.4414(19) ? Cl2 O5 . 1.4718(18) ? S2 C15 . 1.705(3) ? S2 C14 . 1.707(2) ? S1 C2 . 1.708(3) ? S1 C3 . 1.709(2) ? O9 N10 . 1.200(4) ? O10 N10 . 1.182(4) ? N7 C4 . 1.334(3) ? N7 C8 . 1.341(3) ? N9 C14 . 1.319(3) ? N9 C1' . 1.380(3) ? C1' C15 . 1.364(3) ? C1' C32 . 1.470(3) ? N8 C13 . 1.330(3) ? N8 C9 . 1.336(3) ? N6 C3 . 1.321(3) ? N6 C1 . 1.377(3) ? C4 C5 . 1.394(3) ? C4 C3 . 1.472(3) ? C5 C6 . 1.381(4) ? C5 H2A . 0.95 ? C6 C7 . 1.390(4) ? C6 H3 . 0.95 ? C7 C8 . 1.389(3) ? C7 H4 . 0.95 ? C8 C9 . 1.491(3) ? C9 C10 . 1.390(3) ? C10 C11 . 1.384(4) ? C10 H7 . 0.95 ? C11 C12 . 1.393(4) ? C11 H8 . 0.95 ? C12 C13 . 1.388(3) ? C12 H9 . 0.95 ? C13 C14 . 1.473(3) ? C32 C45 . 1.398(3) ? C32 C33 . 1.417(3) ? C45 C44 . 1.386(3) ? C45 H13 . 0.95 ? C44 C43 . 1.390(4) ? C44 H14 . 0.95 ? C43 C46 . 1.422(3) ? C43 C42 . 1.441(3) ? C46 C33 . 1.425(3) ? C46 C47 . 1.433(3) ? C47 C36 . 1.407(4) ? C47 C40 . 1.423(3) ? C36 C37 . 1.410(4) ? C36 C35 . 1.431(4) ? C37 C38 . 1.374(4) ? C37 H19 . 0.95 ? C38 C39 . 1.383(4) ? C38 H20 . 0.95 ? C39 C40 . 1.398(4) ? C39 H21 . 0.95 ? C40 C41 . 1.429(4) ? C41 C42 . 1.344(4) ? C41 H23 . 0.95 ? C42 H24 . 0.95 ? C35 C34 . 1.351(3) ? C35 H25 . 0.95 ? C34 C33 . 1.438(3) ? C34 H26 . 0.95 ? C15 H28 . 0.95 ? C2 C1 . 1.370(3) ? C2 H30 . 0.95 ? C1 C16 . 1.483(3) ? C16 C29 . 1.398(3) ? C16 C17 . 1.403(3) ? C29 C28 . 1.385(4) ? C29 H33 . 0.95 ? C28 C27 . 1.392(4) ? C28 H34 . 0.95 ? C27 C30 . 1.420(3) ? C27 C26 . 1.441(4) ? C30 C17 . 1.427(3) ? C30 C31 . 1.427(3) ? C17 C18 . 1.439(3) ? C18 C19 . 1.351(4) ? C18 H38 . 0.95 ? C19 C20 . 1.430(4) ? C19 H39 . 0.95 ? C20 C21 . 1.400(4) ? C20 C31 . 1.418(4) ? C31 C24 . 1.421(4) ? C24 C23 . 1.402(4) ? C24 C25 . 1.430(4) ? C23 C22 . 1.385(5) ? C23 H43 . 0.95 ? C22 C21 . 1.376(4) ? C22 H44 . 0.95 ? C21 H45 . 0.95 ? C25 C26 . 1.345(4) ? C25 H46 . 0.95 ? C26 H47 . 0.95 ? N10 C49 . 1.455(5) ? C49 H49A . 0.98 ? C49 H49B . 0.98 ? C49 H49C . 0.98 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N9 Cd1 N6 . . 149.32(7) ? N9 Cd1 N8 . . 71.92(7) ? N6 Cd1 N8 . . 138.51(7) ? N9 Cd1 N7 . . 139.09(7) ? N6 Cd1 N7 . . 71.59(7) ? N8 Cd1 N7 . . 67.37(7) ? N9 Cd1 O5 . . 92.39(7) ? N6 Cd1 O5 . . 89.30(6) ? N8 Cd1 O5 . . 94.10(7) ? N7 Cd1 O5 . . 86.59(7) ? N9 Cd1 O1 . . 90.48(7) ? N6 Cd1 O1 . . 90.72(7) ? N8 Cd1 O1 . . 82.15(7) ? N7 Cd1 O1 . . 88.04(7) ? O5 Cd1 O1 . . 174.33(7) ? O2 Cl1 O4 . . 110.70(16) ? O2 Cl1 O3 . . 109.6(2) ? O4 Cl1 O3 . . 109.96(16) ? O2 Cl1 O1 . . 110.01(16) ? O4 Cl1 O1 . . 108.10(13) ? O3 Cl1 O1 . . 108.48(14) ? O8 Cl2 O6 . . 111.15(14) ? O8 Cl2 O7 . . 110.43(13) ? O6 Cl2 O7 . . 110.02(12) ? O8 Cl2 O5 . . 108.42(12) ? O6 Cl2 O5 . . 108.79(12) ? O7 Cl2 O5 . . 107.94(12) ? C15 S2 C14 . . 89.36(12) ? C2 S1 C3 . . 89.51(12) ? Cl1 O1 Cd1 . . 137.02(12) ? Cl2 O5 Cd1 . . 127.58(11) ? C4 N7 C8 . . 121.2(2) ? C4 N7 Cd1 . . 117.05(16) ? C8 N7 Cd1 . . 121.62(16) ? C14 N9 C1' . . 111.7(2) ? C14 N9 Cd1 . . 114.07(15) ? C1' N9 Cd1 . . 132.65(16) ? C15 C1' N9 . . 112.9(2) ? C15 C1' C32 . . 126.0(2) ? N9 C1' C32 . . 120.8(2) ? C13 N8 C9 . . 120.7(2) ? C13 N8 Cd1 . . 116.77(15) ? C9 N8 Cd1 . . 122.13(16) ? C3 N6 C1 . . 112.2(2) ? C3 N6 Cd1 . . 114.31(16) ? C1 N6 Cd1 . . 131.73(16) ? N7 C4 C5 . . 121.4(2) ? N7 C4 C3 . . 113.2(2) ? C5 C4 C3 . . 125.4(2) ? C6 C5 C4 . . 117.8(2) ? C6 C5 H2A . . 121.1 ? C4 C5 H2A . . 121.1 ? C5 C6 C7 . . 120.7(2) ? C5 C6 H3 . . 119.6 ? C7 C6 H3 . . 119.6 ? C8 C7 C6 . . 118.2(3) ? C8 C7 H4 . . 120.9 ? C6 C7 H4 . . 120.9 ? N7 C8 C7 . . 120.8(2) ? N7 C8 C9 . . 114.5(2) ? C7 C8 C9 . . 124.8(2) ? N8 C9 C10 . . 120.9(2) ? N8 C9 C8 . . 114.1(2) ? C10 C9 C8 . . 125.0(2) ? C11 C10 C9 . . 118.5(2) ? C11 C10 H7 . . 120.8 ? C9 C10 H7 . . 120.8 ? C10 C11 C12 . . 120.4(2) ? C10 C11 H8 . . 119.8 ? C12 C11 H8 . . 119.8 ? C13 C12 C11 . . 117.3(2) ? C13 C12 H9 . . 121.4 ? C11 C12 H9 . . 121.4 ? N8 C13 C12 . . 122.2(2) ? N8 C13 C14 . . 113.3(2) ? C12 C13 C14 . . 124.5(2) ? N9 C14 C13 . . 122.4(2) ? N9 C14 S2 . . 114.30(17) ? C13 C14 S2 . . 123.27(18) ? C45 C32 C33 . . 119.6(2) ? C45 C32 C1' . . 118.5(2) ? C33 C32 C1' . . 121.6(2) ? C44 C45 C32 . . 121.3(2) ? C44 C45 H13 . . 119.4 ? C32 C45 H13 . . 119.4 ? C45 C44 C43 . . 120.6(2) ? C45 C44 H14 . . 119.7 ? C43 C44 H14 . . 119.7 ? C44 C43 C46 . . 119.3(2) ? C44 C43 C42 . . 122.4(2) ? C46 C43 C42 . . 118.3(2) ? C43 C46 C33 . . 120.2(2) ? C43 C46 C47 . . 120.0(2) ? C33 C46 C47 . . 119.8(2) ? C36 C47 C40 . . 120.5(2) ? C36 C47 C46 . . 119.8(2) ? C40 C47 C46 . . 119.7(2) ? C47 C36 C37 . . 118.9(2) ? C47 C36 C35 . . 119.1(2) ? C37 C36 C35 . . 122.0(2) ? C38 C37 C36 . . 120.2(3) ? C38 C37 H19 . . 119.9 ? C36 C37 H19 . . 119.9 ? C37 C38 C39 . . 121.1(3) ? C37 C38 H20 . . 119.4 ? C39 C38 H20 . . 119.4 ? C38 C39 C40 . . 120.8(3) ? C38 C39 H21 . . 119.6 ? C40 C39 H21 . . 119.6 ? C39 C40 C47 . . 118.3(3) ? C39 C40 C41 . . 123.1(2) ? C47 C40 C41 . . 118.5(2) ? C42 C41 C40 . . 121.9(2) ? C42 C41 H23 . . 119.0 ? C40 C41 H23 . . 119.0 ? C41 C42 C43 . . 121.3(2) ? C41 C42 H24 . . 119.3 ? C43 C42 H24 . . 119.3 ? C34 C35 C36 . . 121.4(2) ? C34 C35 H25 . . 119.3 ? C36 C35 H25 . . 119.3 ? C35 C34 C33 . . 121.3(2) ? C35 C34 H26 . . 119.4 ? C33 C34 H26 . . 119.4 ? C32 C33 C46 . . 118.6(2) ? C32 C33 C34 . . 123.3(2) ? C46 C33 C34 . . 118.1(2) ? C1' C15 S2 . . 111.70(19) ? C1' C15 H28 . . 124.1 ? S2 C15 H28 . . 124.1 ? N6 C3 C4 . . 122.1(2) ? N6 C3 S1 . . 113.98(19) ? C4 C3 S1 . . 123.92(18) ? C1 C2 S1 . . 111.5(2) ? C1 C2 H30 . . 124.2 ? S1 C2 H30 . . 124.2 ? C2 C1 N6 . . 112.7(2) ? C2 C1 C16 . . 126.9(2) ? N6 C1 C16 . . 119.6(2) ? C29 C16 C17 . . 119.5(2) ? C29 C16 C1 . . 116.6(2) ? C17 C16 C1 . . 123.7(2) ? C28 C29 C16 . . 121.5(2) ? C28 C29 H33 . . 119.2 ? C16 C29 H33 . . 119.2 ? C29 C28 C27 . . 120.6(2) ? C29 C28 H34 . . 119.7 ? C27 C28 H34 . . 119.7 ? C28 C27 C30 . . 118.9(2) ? C28 C27 C26 . . 122.0(2) ? C30 C27 C26 . . 119.1(2) ? C27 C30 C17 . . 120.4(2) ? C27 C30 C31 . . 119.4(2) ? C17 C30 C31 . . 120.2(2) ? C16 C17 C30 . . 118.9(2) ? C16 C17 C18 . . 123.0(2) ? C30 C17 C18 . . 118.1(2) ? C19 C18 C17 . . 121.0(2) ? C19 C18 H38 . . 119.5 ? C17 C18 H38 . . 119.5 ? C18 C19 C20 . . 122.1(2) ? C18 C19 H39 . . 119.0 ? C20 C19 H39 . . 119.0 ? C21 C20 C31 . . 118.9(3) ? C21 C20 C19 . . 122.6(3) ? C31 C20 C19 . . 118.4(2) ? C20 C31 C24 . . 120.1(2) ? C20 C31 C30 . . 119.9(2) ? C24 C31 C30 . . 120.0(2) ? C23 C24 C31 . . 118.8(3) ? C23 C24 C25 . . 122.2(3) ? C31 C24 C25 . . 119.0(2) ? C22 C23 C24 . . 120.4(3) ? C22 C23 H43 . . 119.8 ? C24 C23 H43 . . 119.8 ? C21 C22 C23 . . 121.2(3) ? C21 C22 H44 . . 119.4 ? C23 C22 H44 . . 119.4 ? C22 C21 C20 . . 120.6(3) ? C22 C21 H45 . . 119.7 ? C20 C21 H45 . . 119.7 ? C26 C25 C24 . . 121.5(3) ? C26 C25 H46 . . 119.3 ? C24 C25 H46 . . 119.3 ? C25 C26 C27 . . 121.0(3) ? C25 C26 H47 . . 119.5 ? C27 C26 H47 . . 119.5 ? O10 N10 O9 . . 122.9(4) ? O10 N10 C49 . . 118.4(3) ? O9 N10 C49 . . 118.6(4) ? N10 C49 H49A . . 109.5 ? N10 C49 H49B . . 109.5 ? H49A C49 H49B . . 109.5 ? N10 C49 H49C . . 109.5 ? H49A C49 H49C . . 109.5 ? H49B C49 H49C . . 109.5 ? data_mo_nicky_pyrenecui_on_0m _database_code_depnum_ccdc_archive 'CCDC 845596' #TrackingRef '845596.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C101 H63 Cl2 Cu2 N9 O12 S4' _chemical_formula_weight 1920.82 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 15.462(2) _cell_length_b 33.213(5) _cell_length_c 16.066(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.734(2) _cell_angle_gamma 90.00 _cell_volume 8155(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5397 _cell_measurement_theta_min 2.6642 _cell_measurement_theta_max 30.5117 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3936 _exptl_absorpt_coefficient_mu 0.766 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9274 _exptl_absorpt_correction_T_max 0.9274 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 63702 _diffrn_reflns_av_R_equivalents 0.0692 _diffrn_reflns_av_sigmaI/netI 0.0850 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 26.43 _reflns_number_total 16577 _reflns_number_gt 9947 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _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^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0825P)^2^+14.4919P] 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 16577 _refine_ls_number_parameters 1175 _refine_ls_number_restraints 41 _refine_ls_R_factor_all 0.1238 _refine_ls_R_factor_gt 0.0629 _refine_ls_wR_factor_ref 0.1791 _refine_ls_wR_factor_gt 0.1498 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.77390(4) 0.065700(17) 0.68561(3) 0.02486(15) Uani 1 1 d . . . Cu2 Cu 0.76836(4) 0.124241(17) 0.80558(4) 0.02586(15) Uani 1 1 d . . . S1 S 0.66414(9) 0.12811(4) 0.44858(8) 0.0360(3) Uani 1 1 d . . . S2 S 0.86557(10) 0.05726(5) 1.03997(8) 0.0428(4) Uani 1 1 d . . . S3 S 0.92964(10) -0.03360(5) 0.82190(9) 0.0452(4) Uani 1 1 d . . . S4 S 0.61736(9) 0.22456(4) 0.66992(10) 0.0433(4) Uani 1 1 d . . . N1 N 0.6941(2) 0.08172(11) 0.5764(2) 0.0215(8) Uani 1 1 d . . . N2 N 0.8463(2) 0.11564(11) 0.6493(2) 0.0229(8) Uani 1 1 d . . . N3 N 0.8979(2) 0.10742(12) 0.8220(2) 0.0265(9) Uani 1 1 d . . . N4 N 0.7816(3) 0.10519(12) 0.9320(2) 0.0282(9) Uani 1 1 d . . . N5 N 0.8716(2) 0.02197(11) 0.7177(2) 0.0259(9) Uani 1 1 d . . . N6 N 0.7204(2) 0.03758(11) 0.7815(2) 0.0232(8) Uani 1 1 d . . . N7 N 0.6384(2) 0.11217(12) 0.7569(2) 0.0247(9) Uani 1 1 d . . . N8 N 0.7356(2) 0.17893(12) 0.7505(2) 0.0278(9) Uani 1 1 d . . . C1 C 0.6105(3) 0.07205(14) 0.5352(3) 0.0254(10) Uani 1 1 d . . . C2 C 0.5862(3) 0.09436(16) 0.4652(3) 0.0345(12) Uani 1 1 d . . . H2 H 0.5317 0.0915 0.4294 0.041 Uiso 1 1 calc R . . C3 C 0.7289(3) 0.11077(14) 0.5382(3) 0.0242(10) Uani 1 1 d . . . C4 C 0.8140(3) 0.12766(14) 0.5707(3) 0.0245(10) Uani 1 1 d . . . C5 C 0.8600(3) 0.15354(15) 0.5250(3) 0.0327(12) Uani 1 1 d . . . H5 H 0.8366 0.1608 0.4689 0.039 Uiso 1 1 calc R . . C6 C 0.9395(3) 0.16844(16) 0.5620(4) 0.0377(13) Uani 1 1 d . . . H6 H 0.9716 0.1864 0.5323 0.045 Uiso 1 1 calc R . . C7 C 0.9716(3) 0.15671(15) 0.6427(3) 0.0339(12) Uani 1 1 d . . . H7 H 1.0262 0.1668 0.6698 0.041 Uiso 1 1 calc R . . C8 C 0.9242(3) 0.13003(14) 0.6850(3) 0.0273(11) Uani 1 1 d . . . C9 C 0.9577(3) 0.11622(14) 0.7723(3) 0.0277(11) Uani 1 1 d . . . C10 C 1.0472(3) 0.11249(16) 0.8007(3) 0.0361(13) Uani 1 1 d . . . H10 H 1.0885 0.1197 0.7651 0.043 Uiso 1 1 calc R . . C11 C 1.0753(4) 0.09829(18) 0.8809(4) 0.0457(15) Uani 1 1 d . . . H11 H 1.1360 0.0953 0.9006 0.055 Uiso 1 1 calc R . . C12 C 1.0154(4) 0.08855(17) 0.9316(4) 0.0424(14) Uani 1 1 d . . . H12 H 1.0334 0.0783 0.9867 0.051 Uiso 1 1 calc R . . C13 C 0.9271(3) 0.09392(14) 0.9006(3) 0.0297(11) Uani 1 1 d . . . C14 C 0.8576(3) 0.08761(15) 0.9523(3) 0.0309(12) Uani 1 1 d . . . C15 C 0.7610(4) 0.06995(17) 1.0513(3) 0.0402(13) Uani 1 1 d . . . H15 H 0.7314 0.0602 1.0949 0.048 Uiso 1 1 calc R . . C16 C 0.7254(3) 0.09593(15) 0.9893(3) 0.0303(11) Uani 1 1 d . . . C17 C 0.5554(3) 0.04225(15) 0.5706(3) 0.0274(11) Uani 1 1 d . . . C18 C 0.4675(3) 0.05186(16) 0.5732(3) 0.0317(12) Uani 1 1 d . . . H18 H 0.4433 0.0757 0.5462 0.038 Uiso 1 1 calc R . . C19 C 0.4154(3) 0.02726(16) 0.6143(3) 0.0344(12) Uani 1 1 d . . . H19 H 0.3554 0.0338 0.6132 0.041 Uiso 1 1 calc R . . C20 C 0.4498(3) -0.00702(16) 0.6572(3) 0.0340(12) Uani 1 1 d . . . C21 C 0.4023(3) -0.03080(17) 0.7097(3) 0.0384(13) Uani 1 1 d . . . H21 H 0.3439 -0.0235 0.7145 0.046 Uiso 1 1 calc R . . C22 C 0.4377(4) -0.06271(18) 0.7518(3) 0.0416(14) Uani 1 1 d . . . H22 H 0.4047 -0.0769 0.7876 0.050 Uiso 1 1 calc R . . C23 C 0.5247(4) -0.07640(16) 0.7447(3) 0.0370(13) Uani 1 1 d . . . C24 C 0.5638(4) -0.10952(18) 0.7887(4) 0.0481(15) Uani 1 1 d . . . H24 H 0.5323 -0.1242 0.8251 0.058 Uiso 1 1 calc R . . C25 C 0.6477(4) -0.12125(17) 0.7803(4) 0.0481(15) Uani 1 1 d . . . H25 H 0.6733 -0.1437 0.8114 0.058 Uiso 1 1 calc R . . C26 C 0.6950(4) -0.10090(16) 0.7273(3) 0.0383(13) Uani 1 1 d . . . H26 H 0.7520 -0.1098 0.7211 0.046 Uiso 1 1 calc R . . C27 C 0.6591(3) -0.06724(15) 0.6831(3) 0.0313(11) Uani 1 1 d . . . C28 C 0.7055(3) -0.04414(15) 0.6286(3) 0.0291(11) Uani 1 1 d . . . H28 H 0.7607 -0.0535 0.6176 0.035 Uiso 1 1 calc R . . C29 C 0.6733(3) -0.00981(14) 0.5927(3) 0.0257(10) Uani 1 1 d . . . H29 H 0.7072 0.0049 0.5586 0.031 Uiso 1 1 calc R . . C30 C 0.5891(3) 0.00536(14) 0.6043(3) 0.0252(10) Uani 1 1 d . . . C31 C 0.5376(3) -0.01891(15) 0.6509(3) 0.0275(11) Uani 1 1 d . . . C32 C 0.5733(3) -0.05403(15) 0.6924(3) 0.0297(11) Uani 1 1 d . . . C33 C 0.6351(3) 0.11128(15) 0.9780(3) 0.0314(12) Uani 1 1 d . . . C34 C 0.5683(3) 0.08547(15) 0.9961(3) 0.0336(12) Uani 1 1 d . . . H34 H 0.5830 0.0596 1.0190 0.040 Uiso 1 1 calc R . . C35 C 0.4817(3) 0.09713(16) 0.9810(3) 0.0342(12) Uani 1 1 d . . . H35 H 0.4377 0.0793 0.9940 0.041 Uiso 1 1 calc R . . C36 C 0.4581(3) 0.13497(16) 0.9468(3) 0.0343(12) Uani 1 1 d . . . C37 C 0.3681(4) 0.14696(18) 0.9263(4) 0.0441(14) Uani 1 1 d . . . H37 H 0.3232 0.1289 0.9364 0.053 Uiso 1 1 calc R . . C38 C 0.3464(4) 0.1834(2) 0.8929(4) 0.0525(16) Uani 1 1 d . . . H38 H 0.2864 0.1902 0.8779 0.063 Uiso 1 1 calc R . . C39 C 0.4117(4) 0.21206(18) 0.8795(4) 0.0459(14) Uani 1 1 d . . . C40 C 0.3920(5) 0.2507(2) 0.8464(5) 0.067(2) Uani 1 1 d . . . H40 H 0.3326 0.2580 0.8292 0.080 Uiso 1 1 calc R . . C41 C 0.4566(5) 0.2780(2) 0.8384(5) 0.071(2) Uani 1 1 d . . . H41 H 0.4411 0.3041 0.8168 0.085 Uiso 1 1 calc R . . C42 C 0.5433(5) 0.26848(19) 0.8608(4) 0.0587(18) Uani 1 1 d . . . H42 H 0.5869 0.2880 0.8550 0.070 Uiso 1 1 calc R . . C43 C 0.5678(4) 0.23028(16) 0.8922(4) 0.0426(14) Uani 1 1 d . . . C44 C 0.6567(4) 0.21878(16) 0.9162(4) 0.0441(14) Uani 1 1 d . . . H44 H 0.7015 0.2382 0.9138 0.053 Uiso 1 1 calc R . . C45 C 0.6792(3) 0.18109(15) 0.9422(3) 0.0337(12) Uani 1 1 d . . . H45 H 0.7393 0.1743 0.9559 0.040 Uiso 1 1 calc R . . C46 C 0.6137(3) 0.15085(14) 0.9498(3) 0.0298(11) Uani 1 1 d . . . C47 C 0.5243(3) 0.16232(15) 0.9326(3) 0.0317(12) Uani 1 1 d . . . C48 C 0.5008(4) 0.20169(16) 0.9016(3) 0.0374(13) Uani 1 1 d . . . C49 C 0.9556(3) 0.01264(15) 0.7024(3) 0.0305(11) Uani 1 1 d . . . C50 C 0.9950(4) -0.01648(17) 0.7543(3) 0.0429(14) Uani 1 1 d . . . H50 H 1.0526 -0.0261 0.7527 0.051 Uiso 1 1 calc R . . C51 C 0.8504(3) 0.00005(14) 0.7802(3) 0.0250(10) Uani 1 1 d . . . C52 C 0.7675(3) 0.00506(14) 0.8119(3) 0.0247(10) Uani 1 1 d . . . C53 C 0.7392(3) -0.02182(15) 0.8690(3) 0.0310(11) Uani 1 1 d . . . H53 H 0.7751 -0.0437 0.8911 0.037 Uiso 1 1 calc R . . C54 C 0.6582(3) -0.01585(15) 0.8925(3) 0.0342(12) Uani 1 1 d . . . H54 H 0.6369 -0.0339 0.9306 0.041 Uiso 1 1 calc R . . C55 C 0.6083(3) 0.01638(15) 0.8602(3) 0.0293(11) Uani 1 1 d . . . H55 H 0.5516 0.0204 0.8747 0.035 Uiso 1 1 calc R . . C56 C 0.6413(3) 0.04321(14) 0.8063(3) 0.0252(10) Uani 1 1 d . . . C57 C 0.5918(3) 0.08026(15) 0.7756(3) 0.0263(11) Uani 1 1 d . . . C58 C 0.5009(3) 0.08155(15) 0.7679(3) 0.0284(11) Uani 1 1 d . . . H58 H 0.4693 0.0592 0.7848 0.034 Uiso 1 1 calc R . . C59 C 0.4575(3) 0.11553(16) 0.7358(3) 0.0347(12) Uani 1 1 d . . . H59 H 0.3955 0.1167 0.7297 0.042 Uiso 1 1 calc R . . C60 C 0.5042(3) 0.14781(16) 0.7124(3) 0.0330(12) Uani 1 1 d . . . H60 H 0.4753 0.1710 0.6873 0.040 Uiso 1 1 calc R . . C61 C 0.5955(3) 0.14525(15) 0.7268(3) 0.0279(11) Uani 1 1 d . . . C62 C 0.6522(3) 0.17961(15) 0.7166(3) 0.0297(11) Uani 1 1 d . . . C63 C 0.7208(4) 0.24357(17) 0.6987(4) 0.0453(15) Uani 1 1 d . . . H63 H 0.7379 0.2702 0.6872 0.054 Uiso 1 1 calc R . . C64 C 0.7760(3) 0.21492(16) 0.7408(3) 0.0340(12) Uani 1 1 d . . . C65 C 0.8681(3) 0.22112(15) 0.7799(3) 0.0314(12) Uani 1 1 d . . . C66 C 0.8944(3) 0.20357(15) 0.8587(3) 0.0343(12) Uani 1 1 d . . . H66 H 0.8540 0.1873 0.8827 0.041 Uiso 1 1 calc R . . C67 C 0.9774(3) 0.20916(15) 0.9027(3) 0.0345(12) Uani 1 1 d . . . H67 H 0.9940 0.1958 0.9550 0.041 Uiso 1 1 calc R . . C68 C 1.0372(3) 0.23422(15) 0.8711(3) 0.0320(12) Uani 1 1 d . . . C69 C 1.1211(3) 0.24376(17) 0.9178(3) 0.0395(13) Uani 1 1 d . . . H69 H 1.1387 0.2313 0.9709 0.047 Uiso 1 1 calc R . . C70 C 1.1753(3) 0.26984(16) 0.8882(3) 0.0382(13) Uani 1 1 d . . . H70 H 1.2297 0.2761 0.9216 0.046 Uiso 1 1 calc R . . C71 C 1.1528(3) 0.28840(15) 0.8073(3) 0.0341(12) Uani 1 1 d . . . C72 C 1.2073(4) 0.31655(17) 0.7751(4) 0.0399(13) Uani 1 1 d . . . H72 H 1.2621 0.3234 0.8072 0.048 Uiso 1 1 calc R . . C73 C 1.1822(4) 0.33424(17) 0.6981(3) 0.0408(13) Uani 1 1 d . . . H73 H 1.2192 0.3537 0.6781 0.049 Uiso 1 1 calc R . . C74 C 1.1046(4) 0.32422(17) 0.6498(3) 0.0409(13) Uani 1 1 d . . . H74 H 1.0897 0.3362 0.5958 0.049 Uiso 1 1 calc R . . C75 C 1.0472(3) 0.29708(15) 0.6777(3) 0.0335(12) Uani 1 1 d . . . C76 C 0.9651(3) 0.28631(16) 0.6299(3) 0.0376(13) Uani 1 1 d . . . H76 H 0.9502 0.2968 0.5745 0.045 Uiso 1 1 calc R . . C77 C 0.9080(3) 0.26200(16) 0.6601(3) 0.0365(12) Uani 1 1 d . . . H77 H 0.8538 0.2559 0.6260 0.044 Uiso 1 1 calc R . . C78 C 0.9274(3) 0.24474(14) 0.7439(3) 0.0309(11) Uani 1 1 d . . . C79 C 1.0124(3) 0.25229(14) 0.7906(3) 0.0308(11) Uani 1 1 d . . . C80 C 1.0718(3) 0.27901(15) 0.7587(3) 0.0304(11) Uani 1 1 d . . . C119 C 1.0008(3) 0.03450(15) 0.6408(3) 0.0308(11) Uani 1 1 d . . . C120 C 1.0889(3) 0.04620(15) 0.6654(3) 0.0328(12) Uani 1 1 d . . . H120 H 1.1178 0.0383 0.7193 0.039 Uiso 1 1 calc R . . C121 C 1.1337(3) 0.06820(15) 0.6155(3) 0.0342(12) Uani 1 1 d . . . H121 H 1.1928 0.0754 0.6348 0.041 Uiso 1 1 calc R . . C122 C 1.0931(3) 0.08061(15) 0.5346(3) 0.0328(12) Uani 1 1 d . . . C123 C 1.1359(3) 0.10525(16) 0.4811(3) 0.0356(12) Uani 1 1 d . . . H123 H 1.1945 0.1135 0.4997 0.043 Uiso 1 1 calc R . . C124 C 1.0963(3) 0.11714(16) 0.4057(4) 0.0380(13) Uani 1 1 d . . . H124 H 1.1268 0.1342 0.3727 0.046 Uiso 1 1 calc R . . C125 C 1.0088(3) 0.10473(15) 0.3731(3) 0.0314(11) Uani 1 1 d . . . C126 C 0.9656(4) 0.11619(16) 0.2942(4) 0.0404(13) Uani 1 1 d . . . H126 H 0.9949 0.1328 0.2592 0.049 Uiso 1 1 calc R . . C127 C 0.8810(3) 0.10380(16) 0.2659(3) 0.0362(12) Uani 1 1 d . . . H127 H 0.8527 0.1121 0.2120 0.043 Uiso 1 1 calc R . . C128 C 0.8370(3) 0.07936(16) 0.3153(3) 0.0348(12) Uani 1 1 d . . . H128 H 0.7786 0.0714 0.2950 0.042 Uiso 1 1 calc R . . C129 C 0.8773(3) 0.06622(15) 0.3947(3) 0.0298(11) Uani 1 1 d . . . C130 C 0.8363(3) 0.03957(15) 0.4466(3) 0.0299(11) Uani 1 1 d . . . H130 H 0.7800 0.0291 0.4257 0.036 Uiso 1 1 calc R . . C131 C 0.8749(3) 0.02874(15) 0.5243(3) 0.0285(11) Uani 1 1 d . . . H131 H 0.8453 0.0109 0.5565 0.034 Uiso 1 1 calc R . . C132 C 0.9607(3) 0.04378(14) 0.5596(3) 0.0284(11) Uani 1 1 d . . . C133 C 1.0064(3) 0.06778(14) 0.5062(3) 0.0250(10) Uani 1 1 d . . . C134 C 0.9641(3) 0.07910(15) 0.4250(3) 0.0285(11) Uani 1 1 d . . . Cl1 Cl 0.29010(8) 0.03130(4) 0.85828(8) 0.0339(3) Uani 1 1 d . . . Cl2 Cl 0.11264(10) 0.15106(4) 0.11982(9) 0.0498(4) Uani 1 1 d . . . O1 O 0.3730(2) 0.01283(12) 0.8886(2) 0.0454(10) Uani 1 1 d . . . O2 O 0.2989(3) 0.05987(12) 0.7936(2) 0.0524(11) Uani 1 1 d . . . O3 O 0.2296(2) 0.00073(12) 0.8233(3) 0.0533(11) Uani 1 1 d . . . O4 O 0.2594(3) 0.05137(14) 0.9266(3) 0.0573(12) Uani 1 1 d . . . O5 O 0.1351(3) 0.15855(13) 0.2085(2) 0.0553(11) Uani 1 1 d . . . O6 O 0.1590(3) 0.11664(15) 0.0953(3) 0.0745(15) Uani 1 1 d . . . O7 O 0.0211(3) 0.14055(19) 0.0999(3) 0.0893(18) Uani 1 1 d . . . O2S O 0.7611(4) 0.2519(2) 0.1199(4) 0.1075(14) Uani 1 1 d U . . O1S O 0.8824(4) 0.2821(2) 0.0891(4) 0.122(2) Uani 1 1 d U . . C3S C 0.7025(7) 0.2879(3) 0.1031(6) 0.1032(18) Uani 1 1 d U . . H3S1 H 0.7169 0.3032 0.0541 0.124 Uiso 1 1 calc R . . H3S2 H 0.6405 0.2795 0.0912 0.124 Uiso 1 1 calc R . . C1S C 0.8844(6) 0.2105(3) 0.1156(6) 0.103(2) Uani 1 1 d U . . H1S1 H 0.8712 0.1961 0.0620 0.154 Uiso 1 1 calc R . . H1S2 H 0.8593 0.1959 0.1592 0.154 Uiso 1 1 calc R . . H1S3 H 0.9479 0.2125 0.1318 0.154 Uiso 1 1 calc R . . C4S C 0.7178(6) 0.3122(3) 0.1781(6) 0.106(2) Uani 1 1 d U . . H4S1 H 0.6927 0.2988 0.2232 0.159 Uiso 1 1 calc R . . H4S2 H 0.6901 0.3386 0.1667 0.159 Uiso 1 1 calc R . . H4S3 H 0.7809 0.3157 0.1953 0.159 Uiso 1 1 calc R . . C2S C 0.8461(7) 0.2517(3) 0.1061(6) 0.1016(16) Uani 1 1 d U . . N1S N 0.8467(4) 0.33420(16) 0.9427(4) 0.0670(16) Uani 1 1 d D . . O4S O 0.8533(4) 0.36437(17) 0.9888(4) 0.0960(19) Uani 1 1 d D . . O3S O 0.7748(3) 0.31878(18) 0.9162(4) 0.0947(18) Uani 1 1 d D . . C5S C 0.9234(5) 0.3173(2) 0.9198(5) 0.077(2) Uani 1 1 d . . . H5S1 H 0.9446 0.3345 0.8776 0.116 Uiso 1 1 calc R . . H5S2 H 0.9105 0.2904 0.8963 0.116 Uiso 1 1 calc R . . H5S3 H 0.9684 0.3154 0.9697 0.116 Uiso 1 1 calc R . . O8 O 0.1295(6) 0.18520(18) 0.0787(3) 0.145(3) 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 Cu1 0.0303(3) 0.0230(3) 0.0204(3) 0.0037(3) 0.0012(2) 0.0028(2) Cu2 0.0264(3) 0.0240(3) 0.0259(3) 0.0007(3) -0.0005(2) 0.0019(2) S1 0.0454(8) 0.0330(7) 0.0256(7) 0.0083(6) -0.0072(6) -0.0023(6) S2 0.0524(9) 0.0439(9) 0.0286(7) 0.0064(6) -0.0052(6) 0.0085(7) S3 0.0505(8) 0.0446(9) 0.0422(8) 0.0209(7) 0.0125(7) 0.0235(7) S4 0.0380(7) 0.0382(8) 0.0528(9) 0.0144(7) 0.0045(7) 0.0090(6) N1 0.027(2) 0.022(2) 0.0156(19) -0.0024(16) 0.0013(15) 0.0034(16) N2 0.026(2) 0.018(2) 0.024(2) -0.0030(16) 0.0021(16) 0.0018(16) N3 0.031(2) 0.023(2) 0.024(2) -0.0044(17) -0.0012(17) 0.0040(17) N4 0.036(2) 0.024(2) 0.023(2) -0.0035(18) -0.0011(18) 0.0015(18) N5 0.034(2) 0.021(2) 0.021(2) -0.0026(17) 0.0005(17) 0.0025(17) N6 0.030(2) 0.021(2) 0.0161(19) -0.0032(16) -0.0018(16) -0.0021(16) N7 0.029(2) 0.026(2) 0.018(2) -0.0020(17) -0.0009(16) -0.0001(17) N8 0.032(2) 0.022(2) 0.030(2) 0.0001(18) 0.0078(18) 0.0031(17) C1 0.033(3) 0.023(3) 0.019(2) -0.003(2) -0.0016(19) 0.000(2) C2 0.032(3) 0.038(3) 0.030(3) 0.000(2) -0.005(2) -0.001(2) C3 0.036(3) 0.020(2) 0.016(2) 0.001(2) 0.004(2) 0.007(2) C4 0.031(2) 0.018(2) 0.025(3) -0.002(2) 0.005(2) 0.004(2) C5 0.038(3) 0.025(3) 0.035(3) 0.001(2) 0.006(2) 0.001(2) C6 0.040(3) 0.029(3) 0.048(3) 0.003(3) 0.019(3) -0.003(2) C7 0.027(3) 0.034(3) 0.042(3) -0.011(2) 0.008(2) -0.005(2) C8 0.026(2) 0.023(3) 0.034(3) -0.010(2) 0.008(2) 0.002(2) C9 0.025(2) 0.026(3) 0.030(3) -0.009(2) -0.001(2) 0.002(2) C10 0.029(3) 0.041(3) 0.038(3) -0.012(3) 0.003(2) 0.006(2) C11 0.033(3) 0.055(4) 0.044(3) -0.014(3) -0.013(3) 0.013(3) C12 0.042(3) 0.048(4) 0.033(3) -0.004(3) -0.008(3) 0.009(3) C13 0.035(3) 0.023(3) 0.027(3) -0.006(2) -0.006(2) 0.004(2) C14 0.043(3) 0.026(3) 0.019(2) -0.002(2) -0.008(2) 0.003(2) C15 0.054(3) 0.040(3) 0.027(3) -0.001(3) 0.006(2) -0.003(3) C16 0.046(3) 0.025(3) 0.020(2) -0.003(2) 0.003(2) -0.004(2) C17 0.027(2) 0.031(3) 0.022(2) -0.010(2) -0.0008(19) -0.003(2) C18 0.031(3) 0.034(3) 0.027(3) -0.009(2) -0.004(2) 0.001(2) C19 0.028(3) 0.043(3) 0.031(3) -0.016(3) 0.003(2) -0.001(2) C20 0.037(3) 0.035(3) 0.030(3) -0.013(2) 0.003(2) -0.011(2) C21 0.035(3) 0.046(4) 0.036(3) -0.015(3) 0.010(2) -0.016(3) C22 0.049(3) 0.045(4) 0.034(3) -0.007(3) 0.016(3) -0.023(3) C23 0.047(3) 0.038(3) 0.026(3) -0.010(2) 0.004(2) -0.013(3) C24 0.063(4) 0.042(3) 0.039(3) 0.002(3) 0.003(3) -0.021(3) C25 0.061(4) 0.031(3) 0.050(4) 0.003(3) 0.000(3) -0.006(3) C26 0.045(3) 0.030(3) 0.038(3) 0.000(3) 0.003(3) -0.005(2) C27 0.034(3) 0.027(3) 0.030(3) -0.007(2) -0.002(2) -0.002(2) C28 0.028(3) 0.031(3) 0.027(3) -0.005(2) 0.002(2) -0.002(2) C29 0.026(2) 0.027(3) 0.024(2) -0.004(2) 0.0024(19) -0.006(2) C30 0.030(2) 0.028(3) 0.016(2) -0.006(2) 0.0002(19) -0.006(2) C31 0.031(3) 0.034(3) 0.017(2) -0.008(2) 0.0028(19) -0.008(2) C32 0.044(3) 0.026(3) 0.017(2) -0.007(2) -0.002(2) -0.012(2) C33 0.046(3) 0.028(3) 0.020(3) -0.007(2) 0.008(2) -0.004(2) C34 0.054(3) 0.026(3) 0.021(3) -0.003(2) 0.005(2) -0.003(2) C35 0.046(3) 0.032(3) 0.027(3) -0.003(2) 0.013(2) -0.006(2) C36 0.043(3) 0.031(3) 0.029(3) -0.006(2) 0.008(2) -0.002(2) C37 0.039(3) 0.041(3) 0.052(4) -0.006(3) 0.008(3) -0.006(3) C38 0.042(3) 0.056(4) 0.058(4) 0.001(3) 0.003(3) 0.010(3) C39 0.055(4) 0.040(3) 0.044(3) 0.003(3) 0.013(3) 0.005(3) C40 0.063(4) 0.051(4) 0.087(5) 0.017(4) 0.014(4) 0.023(4) C41 0.086(5) 0.034(4) 0.096(6) 0.022(4) 0.027(5) 0.014(4) C42 0.075(5) 0.036(4) 0.072(5) 0.007(3) 0.032(4) 0.007(3) C43 0.061(4) 0.026(3) 0.045(3) 0.001(3) 0.023(3) -0.003(3) C44 0.057(4) 0.029(3) 0.052(4) -0.006(3) 0.024(3) -0.005(3) C45 0.041(3) 0.027(3) 0.037(3) -0.007(2) 0.018(2) 0.000(2) C46 0.051(3) 0.020(3) 0.021(3) -0.005(2) 0.013(2) -0.002(2) C47 0.037(3) 0.033(3) 0.025(3) -0.006(2) 0.007(2) -0.002(2) C48 0.053(3) 0.029(3) 0.032(3) -0.001(2) 0.010(2) 0.007(3) C49 0.036(3) 0.026(3) 0.029(3) -0.003(2) 0.005(2) 0.006(2) C50 0.041(3) 0.045(3) 0.044(3) 0.010(3) 0.011(3) 0.021(3) C51 0.036(3) 0.020(2) 0.018(2) 0.003(2) -0.0012(19) 0.008(2) C52 0.033(3) 0.025(3) 0.015(2) -0.002(2) 0.0003(19) -0.001(2) C53 0.044(3) 0.023(3) 0.025(3) 0.001(2) 0.002(2) 0.002(2) C54 0.048(3) 0.026(3) 0.030(3) -0.004(2) 0.011(2) -0.009(2) C55 0.034(3) 0.032(3) 0.023(3) -0.009(2) 0.009(2) -0.009(2) C56 0.027(2) 0.028(3) 0.020(2) -0.006(2) 0.0008(19) -0.005(2) C57 0.031(3) 0.032(3) 0.016(2) -0.008(2) 0.0047(19) -0.001(2) C58 0.031(3) 0.033(3) 0.021(2) -0.005(2) 0.004(2) -0.006(2) C59 0.029(3) 0.046(3) 0.027(3) -0.008(2) 0.000(2) -0.001(2) C60 0.028(3) 0.038(3) 0.031(3) -0.003(2) -0.002(2) 0.006(2) C61 0.031(3) 0.031(3) 0.021(2) 0.000(2) 0.000(2) 0.005(2) C62 0.032(3) 0.030(3) 0.028(3) 0.002(2) 0.008(2) 0.009(2) C63 0.046(3) 0.030(3) 0.062(4) 0.010(3) 0.013(3) 0.000(3) C64 0.037(3) 0.035(3) 0.031(3) 0.007(2) 0.007(2) 0.004(2) C65 0.042(3) 0.022(3) 0.032(3) 0.000(2) 0.012(2) 0.001(2) C66 0.042(3) 0.023(3) 0.039(3) 0.002(2) 0.012(2) -0.003(2) C67 0.045(3) 0.028(3) 0.030(3) 0.004(2) 0.006(2) -0.001(2) C68 0.044(3) 0.023(3) 0.030(3) 0.002(2) 0.006(2) -0.001(2) C69 0.046(3) 0.039(3) 0.032(3) 0.006(3) 0.002(2) -0.001(3) C70 0.038(3) 0.039(3) 0.035(3) 0.000(3) -0.002(2) -0.002(2) C71 0.043(3) 0.027(3) 0.034(3) -0.003(2) 0.010(2) 0.003(2) C72 0.039(3) 0.040(3) 0.042(3) 0.001(3) 0.009(3) -0.004(3) C73 0.044(3) 0.039(3) 0.041(3) 0.008(3) 0.013(3) -0.002(3) C74 0.050(3) 0.045(3) 0.030(3) 0.007(3) 0.015(3) -0.004(3) C75 0.045(3) 0.024(3) 0.033(3) 0.003(2) 0.011(2) 0.002(2) C76 0.047(3) 0.037(3) 0.029(3) 0.008(2) 0.007(2) 0.001(3) C77 0.043(3) 0.032(3) 0.035(3) 0.004(2) 0.006(2) 0.002(2) C78 0.039(3) 0.020(3) 0.033(3) -0.003(2) 0.005(2) 0.005(2) C79 0.039(3) 0.022(3) 0.033(3) -0.004(2) 0.012(2) 0.002(2) C80 0.037(3) 0.026(3) 0.029(3) -0.002(2) 0.008(2) 0.003(2) C119 0.034(3) 0.024(3) 0.034(3) -0.004(2) 0.006(2) 0.008(2) C120 0.031(3) 0.032(3) 0.034(3) -0.001(2) 0.000(2) 0.009(2) C121 0.029(3) 0.031(3) 0.042(3) -0.007(3) 0.003(2) 0.002(2) C122 0.032(3) 0.029(3) 0.040(3) -0.010(2) 0.012(2) 0.002(2) C123 0.031(3) 0.034(3) 0.043(3) -0.008(3) 0.011(2) -0.001(2) C124 0.039(3) 0.034(3) 0.046(3) 0.000(3) 0.020(3) 0.001(2) C125 0.039(3) 0.023(3) 0.034(3) 0.000(2) 0.011(2) 0.003(2) C126 0.044(3) 0.036(3) 0.045(3) 0.002(3) 0.017(3) 0.007(3) C127 0.041(3) 0.036(3) 0.031(3) 0.003(2) 0.007(2) 0.009(2) C128 0.034(3) 0.037(3) 0.032(3) -0.004(2) 0.003(2) 0.004(2) C129 0.032(3) 0.030(3) 0.028(3) -0.006(2) 0.006(2) 0.008(2) C130 0.027(2) 0.033(3) 0.030(3) -0.006(2) 0.006(2) -0.001(2) C131 0.029(2) 0.028(3) 0.030(3) -0.007(2) 0.008(2) 0.003(2) C132 0.035(3) 0.017(2) 0.034(3) -0.006(2) 0.008(2) 0.009(2) C133 0.025(2) 0.021(2) 0.031(3) -0.001(2) 0.007(2) 0.0066(19) C134 0.028(2) 0.026(3) 0.033(3) -0.005(2) 0.010(2) 0.006(2) Cl1 0.0292(6) 0.0386(7) 0.0324(7) 0.0033(6) 0.0003(5) 0.0011(5) Cl2 0.0668(10) 0.0395(8) 0.0384(8) 0.0049(7) -0.0072(7) 0.0032(7) O1 0.034(2) 0.048(2) 0.051(2) -0.009(2) -0.0026(17) 0.0135(18) O2 0.055(2) 0.053(3) 0.047(2) 0.018(2) 0.0006(19) -0.014(2) O3 0.048(2) 0.048(3) 0.055(3) 0.019(2) -0.0195(19) -0.0158(19) O4 0.051(2) 0.073(3) 0.049(3) 0.003(2) 0.012(2) 0.028(2) O5 0.067(3) 0.061(3) 0.036(2) -0.001(2) -0.001(2) 0.002(2) O6 0.073(3) 0.075(3) 0.068(3) -0.026(3) -0.013(2) 0.025(3) O7 0.054(3) 0.130(5) 0.079(4) -0.037(3) -0.006(3) -0.005(3) O2S 0.098(3) 0.106(3) 0.121(3) 0.018(3) 0.028(3) 0.010(2) O1S 0.122(4) 0.113(4) 0.124(5) 0.030(4) -0.001(4) -0.034(3) C3S 0.108(4) 0.096(4) 0.108(4) 0.014(3) 0.022(4) 0.006(3) C1S 0.097(5) 0.107(4) 0.108(6) 0.015(5) 0.030(5) 0.009(4) C4S 0.113(6) 0.087(5) 0.110(5) 0.017(4) -0.008(5) 0.002(4) C2S 0.094(3) 0.097(3) 0.116(4) 0.024(3) 0.021(3) -0.006(2) N1S 0.058(4) 0.062(4) 0.081(4) -0.001(3) 0.011(3) -0.006(3) O4S 0.095(4) 0.063(4) 0.129(5) -0.038(4) 0.017(4) 0.001(3) O3S 0.067(3) 0.094(4) 0.117(5) -0.002(4) -0.005(3) -0.020(3) C5S 0.078(5) 0.062(5) 0.098(6) 0.004(4) 0.034(5) 0.017(4) O8 0.276(9) 0.083(4) 0.056(4) 0.036(3) -0.033(4) -0.095(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 2.056(3) . ? Cu1 N6 2.078(4) . ? Cu1 N5 2.102(4) . ? Cu1 N2 2.132(4) . ? Cu1 Cu2 2.7483(9) . ? Cu2 N8 2.050(4) . ? Cu2 N3 2.057(4) . ? Cu2 N7 2.081(4) . ? Cu2 N4 2.108(4) . ? S1 C2 1.697(5) . ? S1 C3 1.723(4) . ? S2 C15 1.708(6) . ? S2 C14 1.721(5) . ? S3 C50 1.691(6) . ? S3 C51 1.717(4) . ? S4 C63 1.717(6) . ? S4 C62 1.720(5) . ? N1 C3 1.303(6) . ? N1 C1 1.397(5) . ? N2 C8 1.341(6) . ? N2 C4 1.345(6) . ? N3 C9 1.343(6) . ? N3 C13 1.351(6) . ? N4 C14 1.308(6) . ? N4 C16 1.393(6) . ? N5 C51 1.320(6) . ? N5 C49 1.394(6) . ? N6 C52 1.351(6) . ? N6 C56 1.355(6) . ? N7 C61 1.336(6) . ? N7 C57 1.340(6) . ? N8 C62 1.321(6) . ? N8 C64 1.369(6) . ? C1 C2 1.352(7) . ? C1 C17 1.476(7) . ? C2 H2 0.9500 . ? C3 C4 1.453(6) . ? C4 C5 1.394(7) . ? C5 C6 1.375(7) . ? C5 H5 0.9500 . ? C6 C7 1.373(7) . ? C6 H6 0.9500 . ? C7 C8 1.391(7) . ? C7 H7 0.9500 . ? C8 C9 1.491(7) . ? C9 C10 1.396(6) . ? C10 C11 1.378(8) . ? C10 H10 0.9500 . ? C11 C12 1.362(8) . ? C11 H11 0.9500 . ? C12 C13 1.391(7) . ? C12 H12 0.9500 . ? C13 C14 1.469(7) . ? C15 C16 1.369(7) . ? C15 H15 0.9500 . ? C16 C33 1.471(7) . ? C17 C18 1.403(6) . ? C17 C30 1.407(7) . ? C18 C19 1.383(7) . ? C18 H18 0.9500 . ? C19 C20 1.395(7) . ? C19 H19 0.9500 . ? C20 C31 1.433(7) . ? C20 C21 1.436(7) . ? C21 C22 1.330(8) . ? C21 H21 0.9500 . ? C22 C23 1.441(8) . ? C22 H22 0.9500 . ? C23 C24 1.395(8) . ? C23 C32 1.420(7) . ? C24 C25 1.381(8) . ? C24 H24 0.9500 . ? C25 C26 1.379(8) . ? C25 H25 0.9500 . ? C26 C27 1.394(7) . ? C26 H26 0.9500 . ? C27 C32 1.427(7) . ? C27 C28 1.436(7) . ? C28 C29 1.339(7) . ? C28 H28 0.9500 . ? C29 C30 1.434(6) . ? C29 H29 0.9500 . ? C30 C31 1.423(7) . ? C31 C32 1.414(7) . ? C33 C34 1.407(7) . ? C33 C46 1.413(7) . ? C34 C35 1.379(7) . ? C34 H34 0.9500 . ? C35 C36 1.398(7) . ? C35 H35 0.9500 . ? C36 C47 1.413(7) . ? C36 C37 1.437(7) . ? C37 C38 1.345(8) . ? C37 H37 0.9500 . ? C38 C39 1.427(8) . ? C38 H38 0.9500 . ? C39 C40 1.404(8) . ? C39 C48 1.413(8) . ? C40 C41 1.370(10) . ? C40 H40 0.9500 . ? C41 C42 1.370(9) . ? C41 H41 0.9500 . ? C42 C43 1.396(8) . ? C42 H42 0.9500 . ? C43 C44 1.423(8) . ? C43 C48 1.429(8) . ? C44 C45 1.349(7) . ? C44 H44 0.9500 . ? C45 C46 1.444(7) . ? C45 H45 0.9500 . ? C46 C47 1.419(7) . ? C47 C48 1.427(7) . ? C49 C50 1.359(7) . ? C49 C119 1.486(7) . ? C50 H50 0.9500 . ? C51 C52 1.459(7) . ? C52 C53 1.397(7) . ? C53 C54 1.377(7) . ? C53 H53 0.9500 . ? C54 C55 1.374(7) . ? C54 H54 0.9500 . ? C55 C56 1.393(7) . ? C55 H55 0.9500 . ? C56 C57 1.493(7) . ? C57 C58 1.394(6) . ? C58 C59 1.373(7) . ? C58 H58 0.9500 . ? C59 C60 1.376(7) . ? C59 H59 0.9500 . ? C60 C61 1.399(6) . ? C60 H60 0.9500 . ? C61 C62 1.464(7) . ? C63 C64 1.384(7) . ? C63 H63 0.9500 . ? C64 C65 1.481(7) . ? C65 C78 1.397(7) . ? C65 C66 1.398(7) . ? C66 C67 1.380(7) . ? C66 H66 0.9500 . ? C67 C68 1.395(7) . ? C67 H67 0.9500 . ? C68 C79 1.425(7) . ? C68 C69 1.432(7) . ? C69 C70 1.342(7) . ? C69 H69 0.9500 . ? C70 C71 1.433(7) . ? C70 H70 0.9500 . ? C71 C80 1.407(7) . ? C71 C72 1.408(7) . ? C72 C73 1.371(7) . ? C72 H72 0.9500 . ? C73 C74 1.368(7) . ? C73 H73 0.9500 . ? C74 C75 1.386(7) . ? C74 H74 0.9500 . ? C75 C76 1.426(7) . ? C75 C80 1.432(7) . ? C76 C77 1.340(7) . ? C76 H76 0.9500 . ? C77 C78 1.452(7) . ? C77 H77 0.9500 . ? C78 C79 1.432(7) . ? C79 C80 1.427(7) . ? C119 C132 1.391(7) . ? C119 C120 1.413(7) . ? C120 C121 1.351(7) . ? C120 H120 0.9500 . ? C121 C122 1.415(7) . ? C121 H121 0.9500 . ? C122 C133 1.415(6) . ? C122 C123 1.421(7) . ? C123 C124 1.332(7) . ? C123 H123 0.9500 . ? C124 C125 1.436(7) . ? C124 H124 0.9500 . ? C125 C126 1.393(7) . ? C125 C134 1.440(7) . ? C126 C127 1.381(7) . ? C126 H126 0.9500 . ? C127 C128 1.384(7) . ? C127 H127 0.9500 . ? C128 C129 1.402(7) . ? C128 H128 0.9500 . ? C129 C134 1.423(7) . ? C129 C130 1.429(7) . ? C130 C131 1.347(7) . ? C130 H130 0.9500 . ? C131 C132 1.450(7) . ? C131 H131 0.9500 . ? C132 C133 1.434(7) . ? C133 C134 1.418(7) . ? Cl1 O4 1.426(4) . ? Cl1 O2 1.429(4) . ? Cl1 O3 1.436(4) . ? Cl1 O1 1.438(4) . ? Cl2 O8 1.358(5) . ? Cl2 O6 1.436(5) . ? Cl2 O5 1.437(4) . ? Cl2 O7 1.445(5) . ? O2S C2S 1.365(10) . ? O2S C3S 1.501(10) . ? O1S C2S 1.207(10) . ? C3S C4S 1.438(12) . ? C3S H3S1 0.9900 . ? C3S H3S2 0.9900 . ? C1S C2S 1.488(13) . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? C4S H4S1 0.9800 . ? C4S H4S2 0.9800 . ? C4S H4S3 0.9800 . ? N1S O3S 1.240(5) . ? N1S O4S 1.241(5) . ? N1S C5S 1.409(9) . ? C5S H5S1 0.9800 . ? C5S H5S2 0.9800 . ? C5S H5S3 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N6 119.64(14) . . ? N1 Cu1 N5 134.74(14) . . ? N6 Cu1 N5 81.90(15) . . ? N1 Cu1 N2 80.61(14) . . ? N6 Cu1 N2 146.88(14) . . ? N5 Cu1 N2 102.55(15) . . ? N1 Cu1 Cu2 109.70(10) . . ? N6 Cu1 Cu2 74.90(10) . . ? N5 Cu1 Cu2 114.48(10) . . ? N2 Cu1 Cu2 73.46(10) . . ? N8 Cu2 N3 117.90(16) . . ? N8 Cu2 N7 81.23(15) . . ? N3 Cu2 N7 149.47(15) . . ? N8 Cu2 N4 131.57(15) . . ? N3 Cu2 N4 81.03(15) . . ? N7 Cu2 N4 104.55(15) . . ? N8 Cu2 Cu1 110.86(11) . . ? N3 Cu2 Cu1 76.38(11) . . ? N7 Cu2 Cu1 74.42(11) . . ? N4 Cu2 Cu1 117.05(11) . . ? C2 S1 C3 89.1(2) . . ? C15 S2 C14 89.5(3) . . ? C50 S3 C51 89.5(2) . . ? C63 S4 C62 89.1(3) . . ? C3 N1 C1 111.5(4) . . ? C3 N1 Cu1 110.9(3) . . ? C1 N1 Cu1 137.5(3) . . ? C8 N2 C4 118.5(4) . . ? C8 N2 Cu1 129.4(3) . . ? C4 N2 Cu1 110.6(3) . . ? C9 N3 C13 117.7(4) . . ? C9 N3 Cu2 127.5(3) . . ? C13 N3 Cu2 113.0(3) . . ? C14 N4 C16 111.4(4) . . ? C14 N4 Cu2 109.0(3) . . ? C16 N4 Cu2 136.4(3) . . ? C51 N5 C49 110.9(4) . . ? C51 N5 Cu1 108.4(3) . . ? C49 N5 Cu1 139.9(3) . . ? C52 N6 C56 117.7(4) . . ? C52 N6 Cu1 111.9(3) . . ? C56 N6 Cu1 129.3(3) . . ? C61 N7 C57 118.5(4) . . ? C61 N7 Cu2 112.1(3) . . ? C57 N7 Cu2 126.1(3) . . ? C62 N8 C64 111.8(4) . . ? C62 N8 Cu2 110.8(3) . . ? C64 N8 Cu2 137.4(3) . . ? C2 C1 N1 112.9(4) . . ? C2 C1 C17 125.7(4) . . ? N1 C1 C17 121.3(4) . . ? C1 C2 S1 112.2(4) . . ? C1 C2 H2 123.9 . . ? S1 C2 H2 123.9 . . ? N1 C3 C4 122.2(4) . . ? N1 C3 S1 114.3(3) . . ? C4 C3 S1 123.5(4) . . ? N2 C4 C5 122.1(4) . . ? N2 C4 C3 114.2(4) . . ? C5 C4 C3 123.7(4) . . ? C6 C5 C4 119.3(5) . . ? C6 C5 H5 120.4 . . ? C4 C5 H5 120.4 . . ? C7 C6 C5 118.5(5) . . ? C7 C6 H6 120.8 . . ? C5 C6 H6 120.8 . . ? C6 C7 C8 120.1(5) . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? N2 C8 C7 121.5(5) . . ? N2 C8 C9 117.0(4) . . ? C7 C8 C9 121.4(4) . . ? N3 C9 C10 121.7(5) . . ? N3 C9 C8 117.0(4) . . ? C10 C9 C8 121.3(5) . . ? C11 C10 C9 119.4(5) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C12 C11 C10 119.6(5) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C11 C12 C13 118.4(5) . . ? C11 C12 H12 120.8 . . ? C13 C12 H12 120.8 . . ? N3 C13 C12 123.2(5) . . ? N3 C13 C14 114.0(4) . . ? C12 C13 C14 122.8(5) . . ? N4 C14 C13 120.1(4) . . ? N4 C14 S2 114.5(4) . . ? C13 C14 S2 125.4(4) . . ? C16 C15 S2 111.1(4) . . ? C16 C15 H15 124.4 . . ? S2 C15 H15 124.4 . . ? C15 C16 N4 113.4(5) . . ? C15 C16 C33 125.3(5) . . ? N4 C16 C33 121.2(4) . . ? C18 C17 C30 119.4(5) . . ? C18 C17 C1 118.5(4) . . ? C30 C17 C1 122.0(4) . . ? C19 C18 C17 121.1(5) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C18 C19 C20 120.8(5) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C19 C20 C31 119.0(5) . . ? C19 C20 C21 123.3(5) . . ? C31 C20 C21 117.7(5) . . ? C22 C21 C20 122.0(5) . . ? C22 C21 H21 119.0 . . ? C20 C21 H21 119.0 . . ? C21 C22 C23 121.9(5) . . ? C21 C22 H22 119.1 . . ? C23 C22 H22 119.1 . . ? C24 C23 C32 119.0(5) . . ? C24 C23 C22 123.2(5) . . ? C32 C23 C22 117.8(5) . . ? C25 C24 C23 120.9(6) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C26 C25 C24 121.1(6) . . ? C26 C25 H25 119.5 . . ? C24 C25 H25 119.5 . . ? C25 C26 C27 120.0(5) . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C26 C27 C32 119.8(5) . . ? C26 C27 C28 122.9(5) . . ? C32 C27 C28 117.3(4) . . ? C29 C28 C27 122.0(5) . . ? C29 C28 H28 119.0 . . ? C27 C28 H28 119.0 . . ? C28 C29 C30 121.9(5) . . ? C28 C29 H29 119.0 . . ? C30 C29 H29 119.0 . . ? C17 C30 C31 119.4(4) . . ? C17 C30 C29 123.1(4) . . ? C31 C30 C29 117.4(4) . . ? C32 C31 C30 120.5(4) . . ? C32 C31 C20 120.0(5) . . ? C30 C31 C20 119.5(5) . . ? C31 C32 C23 120.5(5) . . ? C31 C32 C27 120.4(5) . . ? C23 C32 C27 119.1(5) . . ? C34 C33 C46 119.3(5) . . ? C34 C33 C16 118.4(5) . . ? C46 C33 C16 122.3(5) . . ? C35 C34 C33 121.1(5) . . ? C35 C34 H34 119.4 . . ? C33 C34 H34 119.4 . . ? C34 C35 C36 120.6(5) . . ? C34 C35 H35 119.7 . . ? C36 C35 H35 119.7 . . ? C35 C36 C47 119.3(5) . . ? C35 C36 C37 121.7(5) . . ? C47 C36 C37 119.0(5) . . ? C38 C37 C36 121.0(5) . . ? C38 C37 H37 119.5 . . ? C36 C37 H37 119.5 . . ? C37 C38 C39 121.4(6) . . ? C37 C38 H38 119.3 . . ? C39 C38 H38 119.3 . . ? C40 C39 C48 117.7(6) . . ? C40 C39 C38 123.3(6) . . ? C48 C39 C38 119.0(5) . . ? C41 C40 C39 121.5(6) . . ? C41 C40 H40 119.3 . . ? C39 C40 H40 119.3 . . ? C40 C41 C42 121.3(6) . . ? C40 C41 H41 119.3 . . ? C42 C41 H41 119.3 . . ? C41 C42 C43 120.4(6) . . ? C41 C42 H42 119.8 . . ? C43 C42 H42 119.8 . . ? C42 C43 C44 122.7(6) . . ? C42 C43 C48 118.7(6) . . ? C44 C43 C48 118.6(5) . . ? C45 C44 C43 121.7(5) . . ? C45 C44 H44 119.1 . . ? C43 C44 H44 119.1 . . ? C44 C45 C46 121.4(5) . . ? C44 C45 H45 119.3 . . ? C46 C45 H45 119.3 . . ? C33 C46 C47 119.1(5) . . ? C33 C46 C45 122.7(5) . . ? C47 C46 C45 118.1(5) . . ? C36 C47 C46 120.2(5) . . ? C36 C47 C48 119.6(5) . . ? C46 C47 C48 120.2(5) . . ? C39 C48 C47 119.9(5) . . ? C39 C48 C43 120.4(5) . . ? C47 C48 C43 119.7(5) . . ? C50 C49 N5 113.1(5) . . ? C50 C49 C119 123.0(5) . . ? N5 C49 C119 123.7(4) . . ? C49 C50 S3 112.2(4) . . ? C49 C50 H50 123.9 . . ? S3 C50 H50 123.9 . . ? N5 C51 C52 122.3(4) . . ? N5 C51 S3 114.3(3) . . ? C52 C51 S3 123.4(3) . . ? N6 C52 C53 122.8(4) . . ? N6 C52 C51 114.8(4) . . ? C53 C52 C51 122.4(4) . . ? C54 C53 C52 118.5(5) . . ? C54 C53 H53 120.8 . . ? C52 C53 H53 120.8 . . ? C55 C54 C53 119.4(5) . . ? C55 C54 H54 120.3 . . ? C53 C54 H54 120.3 . . ? C54 C55 C56 119.7(5) . . ? C54 C55 H55 120.1 . . ? C56 C55 H55 120.1 . . ? N6 C56 C55 121.8(4) . . ? N6 C56 C57 117.2(4) . . ? C55 C56 C57 121.0(4) . . ? N7 C57 C58 121.7(4) . . ? N7 C57 C56 117.4(4) . . ? C58 C57 C56 120.9(4) . . ? C59 C58 C57 119.2(5) . . ? C59 C58 H58 120.4 . . ? C57 C58 H58 120.4 . . ? C58 C59 C60 119.8(5) . . ? C58 C59 H59 120.1 . . ? C60 C59 H59 120.1 . . ? C59 C60 C61 117.7(5) . . ? C59 C60 H60 121.1 . . ? C61 C60 H60 121.1 . . ? N7 C61 C60 122.9(5) . . ? N7 C61 C62 114.1(4) . . ? C60 C61 C62 122.8(4) . . ? N8 C62 C61 120.3(4) . . ? N8 C62 S4 114.6(4) . . ? C61 C62 S4 124.9(4) . . ? C64 C63 S4 111.0(4) . . ? C64 C63 H63 124.5 . . ? S4 C63 H63 124.5 . . ? N8 C64 C63 113.4(5) . . ? N8 C64 C65 120.0(4) . . ? C63 C64 C65 126.4(5) . . ? C78 C65 C66 119.4(5) . . ? C78 C65 C64 123.5(5) . . ? C66 C65 C64 117.1(5) . . ? C67 C66 C65 121.8(5) . . ? C67 C66 H66 119.1 . . ? C65 C66 H66 119.1 . . ? C66 C67 C68 120.7(5) . . ? C66 C67 H67 119.7 . . ? C68 C67 H67 119.7 . . ? C67 C68 C79 118.7(5) . . ? C67 C68 C69 122.6(5) . . ? C79 C68 C69 118.7(5) . . ? C70 C69 C68 121.5(5) . . ? C70 C69 H69 119.3 . . ? C68 C69 H69 119.3 . . ? C69 C70 C71 121.4(5) . . ? C69 C70 H70 119.3 . . ? C71 C70 H70 119.3 . . ? C80 C71 C72 118.4(5) . . ? C80 C71 C70 118.7(5) . . ? C72 C71 C70 122.9(5) . . ? C73 C72 C71 120.8(5) . . ? C73 C72 H72 119.6 . . ? C71 C72 H72 119.6 . . ? C74 C73 C72 120.8(5) . . ? C74 C73 H73 119.6 . . ? C72 C73 H73 119.6 . . ? C73 C74 C75 121.6(5) . . ? C73 C74 H74 119.2 . . ? C75 C74 H74 119.2 . . ? C74 C75 C76 123.5(5) . . ? C74 C75 C80 118.1(5) . . ? C76 C75 C80 118.4(5) . . ? C77 C76 C75 122.5(5) . . ? C77 C76 H76 118.7 . . ? C75 C76 H76 118.7 . . ? C76 C77 C78 121.2(5) . . ? C76 C77 H77 119.4 . . ? C78 C77 H77 119.4 . . ? C65 C78 C79 119.3(5) . . ? C65 C78 C77 123.3(5) . . ? C79 C78 C77 117.4(5) . . ? C68 C79 C80 119.3(5) . . ? C68 C79 C78 120.0(5) . . ? C80 C79 C78 120.6(5) . . ? C71 C80 C79 120.4(5) . . ? C71 C80 C75 120.2(5) . . ? C79 C80 C75 119.4(5) . . ? C132 C119 C120 118.4(5) . . ? C132 C119 C49 123.0(4) . . ? C120 C119 C49 118.6(4) . . ? C121 C120 C119 122.8(5) . . ? C121 C120 H120 118.6 . . ? C119 C120 H120 118.6 . . ? C120 C121 C122 120.5(5) . . ? C120 C121 H121 119.8 . . ? C122 C121 H121 119.8 . . ? C121 C122 C133 118.3(5) . . ? C121 C122 C123 122.8(5) . . ? C133 C122 C123 118.9(5) . . ? C124 C123 C122 122.0(5) . . ? C124 C123 H123 119.0 . . ? C122 C123 H123 119.0 . . ? C123 C124 C125 121.7(5) . . ? C123 C124 H124 119.2 . . ? C125 C124 H124 119.2 . . ? C126 C125 C124 123.3(5) . . ? C126 C125 C134 118.9(5) . . ? C124 C125 C134 117.8(5) . . ? C127 C126 C125 121.1(5) . . ? C127 C126 H126 119.4 . . ? C125 C126 H126 119.4 . . ? C126 C127 C128 120.7(5) . . ? C126 C127 H127 119.7 . . ? C128 C127 H127 119.7 . . ? C127 C128 C129 121.0(5) . . ? C127 C128 H128 119.5 . . ? C129 C128 H128 119.5 . . ? C128 C129 C134 119.0(5) . . ? C128 C129 C130 123.3(5) . . ? C134 C129 C130 117.7(4) . . ? C131 C130 C129 122.2(5) . . ? C131 C130 H130 118.9 . . ? C129 C130 H130 118.9 . . ? C130 C131 C132 121.4(5) . . ? C130 C131 H131 119.3 . . ? C132 C131 H131 119.3 . . ? C119 C132 C133 119.6(4) . . ? C119 C132 C131 122.8(5) . . ? C133 C132 C131 117.5(4) . . ? C122 C133 C134 120.0(4) . . ? C122 C133 C132 120.2(4) . . ? C134 C133 C132 119.8(4) . . ? C133 C134 C129 121.0(5) . . ? C133 C134 C125 119.6(4) . . ? C129 C134 C125 119.3(4) . . ? O4 Cl1 O2 109.2(3) . . ? O4 Cl1 O3 111.0(3) . . ? O2 Cl1 O3 108.3(2) . . ? O4 Cl1 O1 108.8(2) . . ? O2 Cl1 O1 110.6(2) . . ? O3 Cl1 O1 109.0(2) . . ? O8 Cl2 O6 113.0(5) . . ? O8 Cl2 O5 107.7(3) . . ? O6 Cl2 O5 110.7(3) . . ? O8 Cl2 O7 110.3(4) . . ? O6 Cl2 O7 105.1(3) . . ? O5 Cl2 O7 110.1(3) . . ? C2S O2S C3S 123.0(8) . . ? C4S C3S O2S 106.2(8) . . ? C4S C3S H3S1 110.5 . . ? O2S C3S H3S1 110.5 . . ? C4S C3S H3S2 110.5 . . ? O2S C3S H3S2 110.5 . . ? H3S1 C3S H3S2 108.7 . . ? C2S C1S H1S1 109.5 . . ? C2S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? C2S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? C3S C4S H4S1 109.5 . . ? C3S C4S H4S2 109.5 . . ? H4S1 C4S H4S2 109.5 . . ? C3S C4S H4S3 109.5 . . ? H4S1 C4S H4S3 109.5 . . ? H4S2 C4S H4S3 109.5 . . ? O1S C2S O2S 121.6(10) . . ? O1S C2S C1S 126.9(10) . . ? O2S C2S C1S 111.5(9) . . ? O3S N1S O4S 121.8(6) . . ? O3S N1S C5S 119.5(6) . . ? O4S N1S C5S 118.7(6) . . ? N1S C5S H5S1 109.5 . . ? N1S C5S H5S2 109.5 . . ? H5S1 C5S H5S2 109.5 . . ? N1S C5S H5S3 109.5 . . ? H5S1 C5S H5S3 109.5 . . ? H5S2 C5S H5S3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.43 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.059 _refine_diff_density_min -0.827 _refine_diff_density_rms 0.095