# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global #TrackingRef '- cif-1.cif' _journal_coden_Cambridge 222 _publ_requested_journal Dalton _publ_contact_author_name 'Subrato Bhattacharya' _publ_contact_author_address ;Lab No. 13, Department of Chemistry, Faculty of Science, Banaras Hindu University, Varanasi-221005 ; _publ_contact_author_email s_bhatt@bhu.ac.in loop_ _publ_author_address ;Lab No. 13, Department of Chemistry, Faculty of Science, Banaras Hindu University, Varanasi-221005 ; _publ_author_name 'Subrato Bhattacharya' # Attachment '- cif-3a.cif' data_29febb _database_code_depnum_ccdc_archive 'CCDC 776679' #TrackingRef '- cif-3a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H23 Cl3 Cu N2 O4 S2' _exptl_crystal_recrystallization_method 'Chloroform and Acetonitrile' _chemical_melting_point ? _exptl_crystal_description Rod _exptl_crystal_colour Bloue _diffrn_ambient_temperature 100(2) _chemical_formula_weight 553.41 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' 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' Cu Cu 0.3201 1.2651 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c 21' _symmetry_int_tables_number 29 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y+1/2, z' 'x, -y+1/2, z+1/2' _cell_length_a 17.575(4) _cell_length_b 17.691(3) _cell_length_c 15.398(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4787.5(16) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.37 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.541 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2280 _exptl_absorpt_coefficient_mu 1.447 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30700 _diffrn_reflns_av_R_equivalents 0.0598 _diffrn_reflns_av_sigmaI/netI 0.0761 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 28.44 _reflns_number_total 11587 _reflns_number_gt 6857 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1194P)^2^+4.4584P] 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 11587 _refine_ls_number_parameters 479 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.1282 _refine_ls_R_factor_gt 0.0756 _refine_ls_wR_factor_ref 0.2470 _refine_ls_wR_factor_gt 0.1955 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.063 _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 S01 S 0.0665(3) 0.1683(3) 0.0888(3) 0.0630(7) Uani 0.659(3) 1 d PD A 1 C08 C 0.0860(5) 0.2479(5) 0.1430(7) 0.0630(7) Uani 0.659(3) 1 d PD A 1 C09 C 0.0367(9) 0.3103(11) 0.1251(13) 0.0630(7) Uani 0.659(3) 1 d PD A 1 H09 H 0.0403 0.3588 0.1481 0.076 Uiso 0.659(3) 1 calc PR A 1 C10 C -0.0188(8) 0.2840(9) 0.0657(10) 0.0630(7) Uani 0.659(3) 1 d PD A 1 H10 H -0.0569 0.3156 0.0448 0.076 Uiso 0.659(3) 1 calc PR A 1 C11 C -0.0141(9) 0.2096(9) 0.0403(11) 0.0630(7) Uani 0.659(3) 1 d PD A 1 H11 H -0.0479 0.1851 0.0033 0.076 Uiso 0.659(3) 1 calc PR A 1 C09A C 0.0663(15) 0.1784(12) 0.1007(18) 0.0630(7) Uani 0.341(3) 1 d PD A 2 H09A H 0.0917 0.1325 0.1048 0.076 Uiso 0.341(3) 1 calc PR A 2 C08A C 0.0860(5) 0.2479(5) 0.1430(7) 0.0630(7) Uani 0.341(3) 1 d PD A 2 S01A S 0.0242(5) 0.3164(6) 0.1228(8) 0.0630(7) Uani 0.341(3) 1 d PD A 2 C11A C -0.0328(14) 0.2659(13) 0.0535(19) 0.0630(7) Uani 0.341(3) 1 d PD A 2 H11A H -0.0758 0.2831 0.0242 0.076 Uiso 0.341(3) 1 calc PR A 2 C10A C -0.0015(16) 0.1945(15) 0.050(2) 0.0630(7) Uani 0.341(3) 1 d PD A 2 H10A H -0.0236 0.1571 0.0160 0.076 Uiso 0.341(3) 1 calc PR A 2 S02 S 0.5126(2) 0.1762(2) 0.1186(3) 0.0593(8) Uani 0.659(3) 1 d PD A 3 C13 C 0.4485(5) 0.2449(4) 0.1357(7) 0.0593(8) Uani 0.659(3) 1 d PD A 3 C14 C 0.4655(10) 0.3099(9) 0.0882(11) 0.0593(8) Uani 0.659(3) 1 d PD A 3 H14 H 0.4363 0.3536 0.0923 0.071 Uiso 0.659(3) 1 calc PR A 3 C15 C 0.5278(9) 0.3053(8) 0.0352(11) 0.0593(8) Uani 0.659(3) 1 d PD A 3 H15 H 0.5451 0.3425 -0.0026 0.071 Uiso 0.659(3) 1 calc PR A 3 C16 C 0.5597(9) 0.2362(7) 0.0481(11) 0.0593(8) Uani 0.659(3) 1 d PD A 3 H16 H 0.6045 0.2219 0.0204 0.071 Uiso 0.659(3) 1 calc PR A 3 C14A C 0.5065(13) 0.1953(17) 0.1124(18) 0.0593(8) Uani 0.341(3) 1 d PD A 4 H14A H 0.5082 0.1481 0.1388 0.071 Uiso 0.341(3) 1 calc PR A 4 C13A C 0.4485(5) 0.2449(4) 0.1357(7) 0.0593(8) Uani 0.341(3) 1 d PD A 4 S02A S 0.4585(6) 0.3237(5) 0.0822(7) 0.0593(8) Uani 0.341(3) 1 d PD A 4 C16A C 0.5389(14) 0.2853(15) 0.033(2) 0.0593(8) Uani 0.341(3) 1 d PD A 4 H16A H 0.5669 0.3141 -0.0058 0.071 Uiso 0.341(3) 1 calc PR A 4 C15A C 0.5611(17) 0.2130(13) 0.0521(19) 0.0593(8) Uani 0.341(3) 1 d PD A 4 H15A H 0.6012 0.1844 0.0305 0.071 Uiso 0.341(3) 1 calc PR A 4 S03 S 0.8185(3) 0.4656(3) 1.0808(3) 0.0634(8) Uani 0.659(3) 1 d PD A 5 C24 C 0.7403(5) 0.4284(5) 1.0318(6) 0.0634(8) Uani 0.659(3) 1 d PD A 5 C25 C 0.6785(9) 0.4736(9) 1.0565(11) 0.0634(8) Uani 0.659(3) 1 d PD A 5 H25 H 0.6301 0.4634 1.0350 0.076 Uiso 0.659(3) 1 calc PR A 5 C26 C 0.6896(8) 0.5325(10) 1.1120(11) 0.0634(8) Uani 0.659(3) 1 d PD A 5 H26 H 0.6524 0.5643 1.1346 0.076 Uiso 0.659(3) 1 calc PR A 5 C27 C 0.7670(8) 0.5358(8) 1.1282(11) 0.0634(8) Uani 0.659(3) 1 d PD A 5 H27 H 0.7890 0.5733 1.1622 0.076 Uiso 0.659(3) 1 calc PR A 5 C25A C 0.8114(12) 0.4546(16) 1.0685(18) 0.0634(8) Uani 0.341(3) 1 d PD A 6 H25A H 0.8608 0.4374 1.0601 0.076 Uiso 0.341(3) 1 calc PR A 6 C24A C 0.7403(5) 0.4284(5) 1.0318(6) 0.0634(8) Uani 0.341(3) 1 d PD A 6 S03A S 0.6592(5) 0.4676(5) 1.0559(6) 0.0634(8) Uani 0.341(3) 1 d PD A 6 C27A C 0.7057(13) 0.5321(16) 1.125(2) 0.0634(8) Uani 0.341(3) 1 d PD A 6 H27A H 0.6830 0.5704 1.1569 0.076 Uiso 0.341(3) 1 calc PR A 6 C26A C 0.7833(14) 0.5150(16) 1.1216(19) 0.0634(8) Uani 0.341(3) 1 d PD A 6 H26A H 0.8172 0.5433 1.1546 0.076 Uiso 0.341(3) 1 calc PR A 6 S04 S 0.6849(3) 0.0471(3) 1.0782(3) 0.0623(7) Uani 0.659(3) 1 d PD A 7 C29 C 0.7710(5) 0.0682(5) 1.0385(6) 0.0623(7) Uani 0.659(3) 1 d PD A 7 C30 C 0.8200(9) 0.0124(8) 1.0772(10) 0.0623(7) Uani 0.659(3) 1 d PD A 7 H30 H 0.8713 0.0124 1.0626 0.075 Uiso 0.659(3) 1 calc PR A 7 C31 C 0.7957(8) -0.0373(9) 1.1308(12) 0.0623(7) Uani 0.659(3) 1 d PD A 7 H31 H 0.8250 -0.0728 1.1603 0.075 Uiso 0.659(3) 1 calc PR A 7 C32 C 0.7169(8) -0.0285(9) 1.1369(11) 0.0623(7) Uani 0.659(3) 1 d PD A 7 H32 H 0.6854 -0.0601 1.1692 0.075 Uiso 0.659(3) 1 calc PR A 7 C30A C 0.6942(12) 0.0536(17) 1.072(2) 0.0623(7) Uani 0.341(3) 1 d PD A 8 H30A H 0.6493 0.0800 1.0622 0.075 Uiso 0.341(3) 1 calc PR A 8 C29A C 0.7710(5) 0.0682(5) 1.0385(6) 0.0623(7) Uani 0.341(3) 1 d PD A 8 S04A S 0.8435(4) 0.0138(5) 1.0690(6) 0.0623(7) Uani 0.341(3) 1 d PD A 8 C32A C 0.7793(12) -0.0430(16) 1.128(2) 0.0623(7) Uani 0.341(3) 1 d PD A 8 H32A H 0.7919 -0.0874 1.1566 0.075 Uiso 0.341(3) 1 calc PR A 8 C31A C 0.7067(15) -0.0113(17) 1.124(2) 0.0623(7) Uani 0.341(3) 1 d PD A 8 H31A H 0.6670 -0.0325 1.1559 0.075 Uiso 0.341(3) 1 calc PR A 8 Cu01 Cu 0.26714(5) 0.24727(5) 0.29792(6) 0.0390(3) Uani 1 1 d . A . Cu02 Cu 0.76887(5) 0.24982(5) 0.88051(6) 0.0390(3) Uani 1 1 d . A . Cl06 Cl 0.4933(2) 0.9647(2) 0.2243(3) 0.0985(10) Uani 1 1 d . . . Cl05 Cl 0.57150(16) 1.07102(16) 0.3329(2) 0.0838(9) Uani 1 1 d . . . Cl01 Cl 0.0487(2) 0.08923(19) 0.8333(3) 0.0993(11) Uani 1 1 d . . . Cl02 Cl 0.0081(2) -0.0363(2) 0.9414(3) 0.1065(11) Uani 1 1 d . . . Cl03 Cl -0.0525(3) -0.0237(3) 0.7709(3) 0.1426(18) Uani 1 1 d . . . Cl04 Cl 0.4374(2) 0.9964(2) 0.3950(3) 0.1073(11) Uani 1 1 d . . . O06 O 0.6871(3) 0.3472(3) 0.9268(4) 0.0527(14) Uani 1 1 d . A . C12 C 0.3844(5) 0.2321(5) 0.2007(5) 0.0450(18) Uani 1 1 d . . . O03 O 0.3373(3) 0.2851(3) 0.2077(3) 0.0468(12) Uani 1 1 d . A . O04 O 0.3825(3) 0.1731(3) 0.2422(4) 0.0580(15) Uani 1 1 d . A . C33 C -0.0221(6) 0.0289(6) 0.8625(8) 0.072(3) Uani 1 1 d . . . H026 H -0.0651 0.0580 0.8854 0.087 Uiso 1 1 calc R . . C21 C 0.7231(6) 0.1193(6) 0.7721(7) 0.071(3) Uani 1 1 d . A . H02A H 0.7067 0.0929 0.8232 0.107 Uiso 1 1 calc R . . H02B H 0.7767 0.1115 0.7638 0.107 Uiso 1 1 calc R . . H02C H 0.6959 0.1006 0.7225 0.107 Uiso 1 1 calc R . . C22 C 0.6234(5) 0.2115(6) 0.8008(7) 0.065(2) Uani 1 1 d . A . H02D H 0.6102 0.1844 0.8527 0.097 Uiso 1 1 calc R . . H02E H 0.5945 0.1921 0.7528 0.097 Uiso 1 1 calc R . . H02F H 0.6123 0.2642 0.8084 0.097 Uiso 1 1 calc R . . C20 C 0.8225(7) 0.3794(6) 0.7803(7) 0.082(3) Uani 1 1 d . A . H03A H 0.8374 0.4023 0.8341 0.122 Uiso 1 1 calc R . . H03B H 0.7695 0.3890 0.7699 0.122 Uiso 1 1 calc R . . H03C H 0.8521 0.4004 0.7338 0.122 Uiso 1 1 calc R . . C03 C 0.3932(6) 0.3120(8) 0.3968(8) 0.090(4) Uani 1 1 d . A . H03D H 0.4165 0.3280 0.3435 0.135 Uiso 1 1 calc R . . H03E H 0.4065 0.2603 0.4081 0.135 Uiso 1 1 calc R . . H03F H 0.4108 0.3433 0.4436 0.135 Uiso 1 1 calc R . . O07 O 0.7314(3) 0.1760(3) 0.9662(4) 0.0470(13) Uani 1 1 d . A . O08 O 0.8477(3) 0.1345(3) 0.9367(4) 0.0585(15) Uani 1 1 d . A . C05 C 0.1439(5) 0.1922(6) 0.4093(7) 0.071(3) Uani 1 1 d . A . H04A H 0.1170 0.1770 0.3579 0.107 Uiso 1 1 calc R . . H04B H 0.1327 0.2441 0.4219 0.107 Uiso 1 1 calc R . . H04C H 0.1282 0.1612 0.4573 0.107 Uiso 1 1 calc R . . O01 O 0.1962(3) 0.2007(3) 0.2107(4) 0.0485(13) Uani 1 1 d . A . C06 C 0.2453(7) 0.1035(5) 0.3794(8) 0.077(3) Uani 1 1 d . A . H04D H 0.2994 0.0990 0.3720 0.116 Uiso 1 1 calc R . . H04E H 0.2200 0.0862 0.3278 0.116 Uiso 1 1 calc R . . H04F H 0.2295 0.0733 0.4280 0.116 Uiso 1 1 calc R . . C02 C 0.2759(6) 0.2930(6) 0.4718(6) 0.065(3) Uani 1 1 d . A . H04G H 0.2261 0.3162 0.4779 0.078 Uiso 1 1 calc R . . H04H H 0.3071 0.3092 0.5203 0.078 Uiso 1 1 calc R . . C23 C 0.7436(5) 0.3619(4) 0.9738(5) 0.0456(18) Uani 1 1 d . . . C19 C 0.9151(5) 0.2819(6) 0.8044(8) 0.070(3) Uani 1 1 d . A . H04I H 0.9227 0.2283 0.8085 0.105 Uiso 1 1 calc R . . H04J H 0.9285 0.3052 0.8586 0.105 Uiso 1 1 calc R . . H04K H 0.9466 0.3020 0.7590 0.105 Uiso 1 1 calc R . . O05 O 0.8051(3) 0.3238(3) 0.9703(3) 0.0456(12) Uani 1 1 d . A . C17 C 0.8128(7) 0.2586(7) 0.7048(7) 0.080(3) Uani 1 1 d . A . H05A H 0.8263 0.2896 0.6551 0.096 Uiso 1 1 calc R . . H05B H 0.8403 0.2112 0.7002 0.096 Uiso 1 1 calc R . . O02 O 0.1597(3) 0.3154(3) 0.2446(4) 0.0529(14) Uani 1 1 d . A . C01 C 0.2677(6) 0.2084(6) 0.4738(6) 0.071(3) Uani 1 1 d . A . H06A H 0.3176 0.1850 0.4749 0.085 Uiso 1 1 calc R . . H06B H 0.2404 0.1933 0.5257 0.085 Uiso 1 1 calc R . . C18 C 0.7311(6) 0.2437(5) 0.7036(7) 0.067(3) Uani 1 1 d . A . H06C H 0.7184 0.2145 0.6524 0.080 Uiso 1 1 calc R . . H06D H 0.7037 0.2912 0.7008 0.080 Uiso 1 1 calc R . . C04 C 0.2856(9) 0.3971(5) 0.3693(9) 0.095(4) Uani 1 1 d . A . H06E H 0.3081 0.4134 0.3157 0.142 Uiso 1 1 calc R . . H06F H 0.3009 0.4304 0.4153 0.142 Uiso 1 1 calc R . . H06G H 0.2311 0.3979 0.3640 0.142 Uiso 1 1 calc R . . C07 C 0.1510(4) 0.2563(4) 0.2026(5) 0.0419(17) Uani 1 1 d . . . C28 C 0.7866(5) 0.1298(5) 0.9773(5) 0.0471(19) Uani 1 1 d . . . C34 C 0.4839(6) 1.0350(6) 0.3038(9) 0.076(3) Uani 1 1 d . . . H009 H 0.4527 1.0761 0.2804 0.091 Uiso 1 1 calc R . . N03 N 0.8355(5) 0.2975(4) 0.7848(4) 0.0547(18) Uani 1 1 d . . . N01 N 0.2254(4) 0.1833(4) 0.3955(5) 0.0552(19) Uani 1 1 d . . . N04 N 0.7077(4) 0.2016(4) 0.7825(5) 0.0532(18) Uani 1 1 d . . . N02 N 0.3113(4) 0.3186(4) 0.3894(5) 0.0583(19) 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 S01 0.0513(14) 0.0781(17) 0.0598(16) 0.0034(13) -0.0120(13) -0.0053(13) C08 0.0513(14) 0.0781(17) 0.0598(16) 0.0034(13) -0.0120(13) -0.0053(13) C09 0.0513(14) 0.0781(17) 0.0598(16) 0.0034(13) -0.0120(13) -0.0053(13) C10 0.0513(14) 0.0781(17) 0.0598(16) 0.0034(13) -0.0120(13) -0.0053(13) C11 0.0513(14) 0.0781(17) 0.0598(16) 0.0034(13) -0.0120(13) -0.0053(13) C09A 0.0513(14) 0.0781(17) 0.0598(16) 0.0034(13) -0.0120(13) -0.0053(13) C08A 0.0513(14) 0.0781(17) 0.0598(16) 0.0034(13) -0.0120(13) -0.0053(13) S01A 0.0513(14) 0.0781(17) 0.0598(16) 0.0034(13) -0.0120(13) -0.0053(13) C11A 0.0513(14) 0.0781(17) 0.0598(16) 0.0034(13) -0.0120(13) -0.0053(13) C10A 0.0513(14) 0.0781(17) 0.0598(16) 0.0034(13) -0.0120(13) -0.0053(13) S02 0.0550(13) 0.066(2) 0.0566(14) -0.0010(13) 0.0067(12) 0.0075(13) C13 0.0550(13) 0.066(2) 0.0566(14) -0.0010(13) 0.0067(12) 0.0075(13) C14 0.0550(13) 0.066(2) 0.0566(14) -0.0010(13) 0.0067(12) 0.0075(13) C15 0.0550(13) 0.066(2) 0.0566(14) -0.0010(13) 0.0067(12) 0.0075(13) C16 0.0550(13) 0.066(2) 0.0566(14) -0.0010(13) 0.0067(12) 0.0075(13) C14A 0.0550(13) 0.066(2) 0.0566(14) -0.0010(13) 0.0067(12) 0.0075(13) C13A 0.0550(13) 0.066(2) 0.0566(14) -0.0010(13) 0.0067(12) 0.0075(13) S02A 0.0550(13) 0.066(2) 0.0566(14) -0.0010(13) 0.0067(12) 0.0075(13) C16A 0.0550(13) 0.066(2) 0.0566(14) -0.0010(13) 0.0067(12) 0.0075(13) C15A 0.0550(13) 0.066(2) 0.0566(14) -0.0010(13) 0.0067(12) 0.0075(13) S03 0.0754(18) 0.0632(17) 0.0515(15) -0.0168(12) 0.0083(13) -0.0139(13) C24 0.0754(18) 0.0632(17) 0.0515(15) -0.0168(12) 0.0083(13) -0.0139(13) C25 0.0754(18) 0.0632(17) 0.0515(15) -0.0168(12) 0.0083(13) -0.0139(13) C26 0.0754(18) 0.0632(17) 0.0515(15) -0.0168(12) 0.0083(13) -0.0139(13) C27 0.0754(18) 0.0632(17) 0.0515(15) -0.0168(12) 0.0083(13) -0.0139(13) C25A 0.0754(18) 0.0632(17) 0.0515(15) -0.0168(12) 0.0083(13) -0.0139(13) C24A 0.0754(18) 0.0632(17) 0.0515(15) -0.0168(12) 0.0083(13) -0.0139(13) S03A 0.0754(18) 0.0632(17) 0.0515(15) -0.0168(12) 0.0083(13) -0.0139(13) C27A 0.0754(18) 0.0632(17) 0.0515(15) -0.0168(12) 0.0083(13) -0.0139(13) C26A 0.0754(18) 0.0632(17) 0.0515(15) -0.0168(12) 0.0083(13) -0.0139(13) S04 0.0749(18) 0.0609(15) 0.0512(15) 0.0131(12) 0.0010(13) -0.0092(14) C29 0.0749(18) 0.0609(15) 0.0512(15) 0.0131(12) 0.0010(13) -0.0092(14) C30 0.0749(18) 0.0609(15) 0.0512(15) 0.0131(12) 0.0010(13) -0.0092(14) C31 0.0749(18) 0.0609(15) 0.0512(15) 0.0131(12) 0.0010(13) -0.0092(14) C32 0.0749(18) 0.0609(15) 0.0512(15) 0.0131(12) 0.0010(13) -0.0092(14) C30A 0.0749(18) 0.0609(15) 0.0512(15) 0.0131(12) 0.0010(13) -0.0092(14) C29A 0.0749(18) 0.0609(15) 0.0512(15) 0.0131(12) 0.0010(13) -0.0092(14) S04A 0.0749(18) 0.0609(15) 0.0512(15) 0.0131(12) 0.0010(13) -0.0092(14) C32A 0.0749(18) 0.0609(15) 0.0512(15) 0.0131(12) 0.0010(13) -0.0092(14) C31A 0.0749(18) 0.0609(15) 0.0512(15) 0.0131(12) 0.0010(13) -0.0092(14) Cu01 0.0382(5) 0.0447(6) 0.0342(5) -0.0004(4) 0.0003(5) -0.0007(4) Cu02 0.0437(6) 0.0395(5) 0.0338(5) 0.0007(4) 0.0019(5) 0.0009(4) Cl06 0.101(2) 0.090(2) 0.105(3) -0.0352(19) -0.0058(19) -0.0110(17) Cl05 0.0747(17) 0.0741(17) 0.103(2) 0.0004(15) -0.0230(16) -0.0182(14) Cl01 0.097(2) 0.0804(19) 0.120(3) 0.0056(18) 0.021(2) -0.0251(17) Cl02 0.104(2) 0.108(2) 0.108(3) 0.034(2) 0.003(2) 0.016(2) Cl03 0.147(4) 0.171(4) 0.109(3) -0.004(3) -0.032(3) -0.060(3) Cl04 0.100(2) 0.119(3) 0.103(3) 0.010(2) 0.020(2) -0.015(2) O06 0.051(3) 0.048(3) 0.058(4) -0.007(3) -0.012(3) 0.012(3) C12 0.045(4) 0.053(5) 0.037(4) -0.007(3) -0.003(3) -0.004(4) O03 0.052(3) 0.049(3) 0.039(3) 0.004(2) 0.008(3) -0.002(3) O04 0.059(4) 0.056(3) 0.059(4) 0.015(3) 0.010(3) 0.006(3) C33 0.066(6) 0.073(6) 0.079(7) 0.012(5) 0.006(6) 0.002(6) C21 0.087(8) 0.065(6) 0.062(6) -0.025(5) -0.011(5) -0.003(5) C22 0.053(5) 0.081(7) 0.060(6) 0.001(5) -0.019(5) -0.006(5) C20 0.094(8) 0.073(7) 0.077(8) 0.045(6) 0.012(6) -0.004(6) C03 0.069(7) 0.138(11) 0.064(7) -0.016(7) -0.024(6) -0.029(7) O07 0.052(3) 0.042(3) 0.046(3) 0.011(2) 0.009(3) -0.001(2) O08 0.050(3) 0.068(4) 0.058(4) 0.004(3) 0.011(3) 0.003(3) C05 0.055(6) 0.098(8) 0.061(6) 0.012(5) 0.015(5) -0.016(5) O01 0.047(3) 0.043(3) 0.056(3) -0.012(3) -0.016(3) 0.009(2) C06 0.108(8) 0.040(5) 0.084(8) 0.016(5) 0.012(7) -0.007(5) C02 0.079(7) 0.077(7) 0.040(5) -0.010(5) -0.002(5) -0.015(5) C23 0.060(5) 0.042(4) 0.034(4) 0.004(3) -0.006(4) -0.001(4) C19 0.050(5) 0.076(6) 0.084(7) 0.005(6) 0.016(5) -0.012(5) O05 0.044(3) 0.052(3) 0.040(3) -0.010(2) -0.003(2) 0.003(2) C17 0.094(9) 0.102(9) 0.044(6) 0.010(5) 0.014(6) 0.002(6) O02 0.062(4) 0.041(3) 0.055(3) -0.005(3) -0.005(3) 0.003(3) C01 0.099(8) 0.088(8) 0.025(4) 0.009(5) -0.001(5) -0.025(6) C18 0.095(9) 0.074(7) 0.032(5) 0.004(4) 0.003(5) -0.010(5) C04 0.160(13) 0.039(5) 0.085(8) -0.018(5) -0.025(8) 0.001(6) C07 0.046(4) 0.050(4) 0.030(4) 0.003(3) 0.001(3) -0.005(3) C28 0.052(5) 0.054(5) 0.035(4) -0.004(3) -0.004(4) 0.001(4) C34 0.058(6) 0.074(7) 0.095(8) 0.000(6) -0.010(6) 0.007(5) N03 0.072(5) 0.057(4) 0.036(4) 0.004(3) 0.019(3) -0.014(4) N01 0.058(4) 0.062(5) 0.046(4) 0.016(3) 0.009(3) -0.014(3) N04 0.068(5) 0.050(4) 0.043(4) -0.007(3) -0.013(3) -0.009(3) N02 0.061(5) 0.072(5) 0.042(4) -0.011(4) -0.009(4) -0.015(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 S01 C08 1.672(10) . ? S01 C11 1.761(12) . ? C08 C09 1.431(16) . ? C08 C07 1.474(12) . ? C09 C10 1.416(16) . ? C09 H09 0.9300 . ? C10 C11 1.376(15) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C09A C10A 1.451(18) . ? C09A H09A 0.9300 . ? S01A C11A 1.715(17) . ? C11A C10A 1.379(18) . ? C11A H11A 0.9300 . ? C10A H10A 0.9300 . ? S02 C13 1.678(9) . ? S02 C16 1.730(13) . ? C13 C14 1.396(15) . ? C13 C12 1.523(12) . ? C14 C15 1.368(16) . ? C14 H14 0.9300 . ? C15 C16 1.359(14) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C14A C15A 1.371(19) . ? C14A H14A 0.9300 . ? S02A C16A 1.739(17) . ? C16A C15A 1.369(18) . ? C16A H16A 0.9300 . ? C15A H15A 0.9300 . ? S03 C24 1.700(10) . ? S03 C27 1.700(12) . ? C24 C25 1.401(15) . ? C24 C23 1.477(11) . ? C25 C26 1.362(15) . ? C25 H25 0.9300 . ? C26 C27 1.384(15) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C25A C26A 1.433(18) . ? C25A H25A 0.9300 . ? S03A C27A 1.758(17) . ? C27A C26A 1.396(18) . ? C27A H27A 0.9300 . ? C26A H26A 0.9300 . ? S04 C29 1.674(10) . ? S04 C32 1.708(12) . ? C29 C30 1.440(15) . ? C29 C28 1.466(12) . ? C30 C31 1.280(15) . ? C30 H30 0.9300 . ? C31 C32 1.397(15) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C30A C31A 1.418(18) . ? C30A H30A 0.9300 . ? S04A C32A 1.761(17) . ? C32A C31A 1.394(18) . ? C32A H32A 0.9300 . ? C31A H31A 0.9300 . ? Cu01 O03 1.975(5) . ? Cu01 O01 2.010(5) . ? Cu01 N01 2.018(7) . ? Cu01 N02 2.044(7) . ? Cu01 O02 2.386(6) . ? Cu01 C07 2.518(8) . ? Cu02 O07 1.970(5) . ? Cu02 O05 2.008(5) . ? Cu02 N04 2.039(7) . ? Cu02 N03 2.062(7) . ? Cu02 O06 2.355(6) . ? Cu02 C23 2.489(8) . ? Cl06 C34 1.753(12) . ? Cl05 C34 1.726(10) . ? Cl01 C33 1.700(11) . ? Cl02 C33 1.758(11) . ? Cl03 C33 1.773(12) . ? Cl04 C34 1.762(13) . ? O06 C23 1.257(10) . ? C12 O04 1.226(10) . ? C12 O03 1.254(10) . ? C33 H026 0.9800 . ? C21 N04 1.490(12) . ? C21 H02A 0.9600 . ? C21 H02B 0.9600 . ? C21 H02C 0.9600 . ? C22 N04 1.517(12) . ? C22 H02D 0.9600 . ? C22 H02E 0.9600 . ? C22 H02F 0.9600 . ? C20 N03 1.469(12) . ? C20 H03A 0.9600 . ? C20 H03B 0.9600 . ? C20 H03C 0.9600 . ? C03 N02 1.449(13) . ? C03 H03D 0.9600 . ? C03 H03E 0.9600 . ? C03 H03F 0.9600 . ? O07 C28 1.281(10) . ? O08 C28 1.245(10) . ? C05 N01 1.457(12) . ? C05 H04A 0.9600 . ? C05 H04B 0.9600 . ? C05 H04C 0.9600 . ? O01 C07 1.270(9) . ? C06 N01 1.476(12) . ? C06 H04D 0.9600 . ? C06 H04E 0.9600 . ? C06 H04F 0.9600 . ? C02 N02 1.483(12) . ? C02 C01 1.504(15) . ? C02 H04G 0.9700 . ? C02 H04H 0.9700 . ? C23 O05 1.275(10) . ? C19 N03 1.458(12) . ? C19 H04I 0.9600 . ? C19 H04J 0.9600 . ? C19 H04K 0.9600 . ? C17 C18 1.460(16) . ? C17 N03 1.466(14) . ? C17 H05A 0.9700 . ? C17 H05B 0.9700 . ? O02 C07 1.238(9) . ? C01 N01 1.484(12) . ? C01 H06A 0.9700 . ? C01 H06B 0.9700 . ? C18 N04 1.483(12) . ? C18 H06C 0.9700 . ? C18 H06D 0.9700 . ? C04 N02 1.493(13) . ? C04 H06E 0.9600 . ? C04 H06F 0.9600 . ? C04 H06G 0.9600 . ? C34 H009 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 C08 S01 C11 91.5(7) . . ? C09 C08 C07 120.8(10) . . ? C09 C08 S01 115.5(10) . . ? C07 C08 S01 123.7(6) . . ? C10 C09 C08 106.7(15) . . ? C10 C09 H09 126.6 . . ? C08 C09 H09 126.6 . . ? C11 C10 C09 117.2(15) . . ? C11 C10 H10 121.4 . . ? C09 C10 H10 121.4 . . ? C10 C11 S01 109.0(11) . . ? C10 C11 H11 125.5 . . ? S01 C11 H11 125.5 . . ? C10A C09A H09A 127.0 . . ? C10A C11A S01A 105.5(15) . . ? C10A C11A H11A 127.2 . . ? S01A C11A H11A 127.2 . . ? C11A C10A C09A 119(2) . . ? C11A C10A H10A 120.4 . . ? C09A C10A H10A 120.4 . . ? C13 S02 C16 88.6(6) . . ? C14 C13 C12 128.6(10) . . ? C14 C13 S02 111.8(10) . . ? C12 C13 S02 119.5(6) . . ? C15 C14 C13 115.8(16) . . ? C15 C14 H14 122.1 . . ? C13 C14 H14 122.1 . . ? C16 C15 C14 107.2(16) . . ? C16 C15 H15 126.4 . . ? C14 C15 H15 126.4 . . ? C15 C16 S02 116.5(12) . . ? C15 C16 H16 121.7 . . ? S02 C16 H16 121.7 . . ? C15A C14A H14A 118.5 . . ? C15A C16A S02A 120(2) . . ? C15A C16A H16A 119.8 . . ? S02A C16A H16A 119.8 . . ? C16A C15A C14A 99(3) . . ? C16A C15A H15A 130.5 . . ? C14A C15A H15A 130.5 . . ? C24 S03 C27 92.5(6) . . ? C25 C24 C23 130.4(10) . . ? C25 C24 S03 106.5(9) . . ? C23 C24 S03 123.0(7) . . ? C26 C25 C24 119.7(15) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C27 106.7(14) . . ? C25 C26 H26 126.7 . . ? C27 C26 H26 126.7 . . ? C26 C27 S03 114.5(11) . . ? C26 C27 H27 122.8 . . ? S03 C27 H27 122.8 . . ? C26A C25A H25A 130.3 . . ? C26A C27A S03A 107.0(15) . . ? C26A C27A H27A 126.5 . . ? S03A C27A H27A 126.5 . . ? C27A C26A C25A 121.1(19) . . ? C27A C26A H26A 119.4 . . ? C25A C26A H26A 119.4 . . ? C29 S04 C32 94.1(6) . . ? C30 C29 C28 131.5(9) . . ? C30 C29 S04 103.7(8) . . ? C28 C29 S04 124.8(7) . . ? C31 C30 C29 122.6(15) . . ? C31 C30 H30 118.7 . . ? C29 C30 H30 118.7 . . ? C30 C31 C32 107.3(14) . . ? C30 C31 H31 126.4 . . ? C32 C31 H31 126.4 . . ? C31 C32 S04 112.2(11) . . ? C31 C32 H32 123.9 . . ? S04 C32 H32 123.9 . . ? C31A C30A H30A 129.2 . . ? C31A C32A S04A 109.7(16) . . ? C31A C32A H32A 125.2 . . ? S04A C32A H32A 125.2 . . ? C32A C31A C30A 119.3(19) . . ? C32A C31A H31A 120.4 . . ? C30A C31A H31A 120.4 . . ? O03 Cu01 O01 93.2(3) . . ? O03 Cu01 N01 160.1(3) . . ? O01 Cu01 N01 92.4(3) . . ? O03 Cu01 N02 92.2(3) . . ? O01 Cu01 N02 161.6(3) . . ? N01 Cu01 N02 88.3(3) . . ? O03 Cu01 O02 94.6(2) . . ? O01 Cu01 O02 59.0(2) . . ? N01 Cu01 O02 104.6(3) . . ? N02 Cu01 O02 103.0(3) . . ? O03 Cu01 C07 94.3(2) . . ? O01 Cu01 C07 30.0(2) . . ? N01 Cu01 C07 100.1(3) . . ? N02 Cu01 C07 132.0(3) . . ? O02 Cu01 C07 29.1(2) . . ? O07 Cu02 O05 94.4(3) . . ? O07 Cu02 N04 92.4(3) . . ? O05 Cu02 N04 161.7(3) . . ? O07 Cu02 N03 160.0(3) . . ? O05 Cu02 N03 92.6(3) . . ? N04 Cu02 N03 86.6(3) . . ? O07 Cu02 O06 94.5(2) . . ? O05 Cu02 O06 60.5(2) . . ? N04 Cu02 O06 102.0(3) . . ? N03 Cu02 O06 105.3(3) . . ? O07 Cu02 C23 94.7(3) . . ? O05 Cu02 C23 30.6(2) . . ? N04 Cu02 C23 131.8(3) . . ? N03 Cu02 C23 100.8(3) . . ? O06 Cu02 C23 29.9(2) . . ? C23 O06 Cu02 81.0(5) . . ? O04 C12 O03 125.0(8) . . ? O04 C12 C13 119.3(7) . . ? O03 C12 C13 115.7(7) . . ? C12 O03 Cu01 102.7(5) . . ? Cl01 C33 Cl02 111.9(6) . . ? Cl01 C33 Cl03 109.9(7) . . ? Cl02 C33 Cl03 107.2(6) . . ? Cl01 C33 H026 109.3 . . ? Cl02 C33 H026 109.3 . . ? Cl03 C33 H026 109.3 . . ? N04 C21 H02A 109.5 . . ? N04 C21 H02B 109.5 . . ? H02A C21 H02B 109.5 . . ? N04 C21 H02C 109.5 . . ? H02A C21 H02C 109.5 . . ? H02B C21 H02C 109.5 . . ? N04 C22 H02D 109.5 . . ? N04 C22 H02E 109.5 . . ? H02D C22 H02E 109.5 . . ? N04 C22 H02F 109.5 . . ? H02D C22 H02F 109.5 . . ? H02E C22 H02F 109.5 . . ? N03 C20 H03A 109.5 . . ? N03 C20 H03B 109.5 . . ? H03A C20 H03B 109.5 . . ? N03 C20 H03C 109.5 . . ? H03A C20 H03C 109.5 . . ? H03B C20 H03C 109.5 . . ? N02 C03 H03D 109.5 . . ? N02 C03 H03E 109.5 . . ? H03D C03 H03E 109.5 . . ? N02 C03 H03F 109.5 . . ? H03D C03 H03F 109.5 . . ? H03E C03 H03F 109.5 . . ? C28 O07 Cu02 105.0(5) . . ? N01 C05 H04A 109.5 . . ? N01 C05 H04B 109.5 . . ? H04A C05 H04B 109.5 . . ? N01 C05 H04C 109.5 . . ? H04A C05 H04C 109.5 . . ? H04B C05 H04C 109.5 . . ? C07 O01 Cu01 97.8(4) . . ? N01 C06 H04D 109.5 . . ? N01 C06 H04E 109.5 . . ? H04D C06 H04E 109.5 . . ? N01 C06 H04F 109.5 . . ? H04D C06 H04F 109.5 . . ? H04E C06 H04F 109.5 . . ? N02 C02 C01 111.2(7) . . ? N02 C02 H04G 109.4 . . ? C01 C02 H04G 109.4 . . ? N02 C02 H04H 109.4 . . ? C01 C02 H04H 109.4 . . ? H04G C02 H04H 108.0 . . ? O06 C23 O05 122.5(7) . . ? O06 C23 C24 118.8(7) . . ? O05 C23 C24 118.7(7) . . ? O06 C23 Cu02 69.1(4) . . ? O05 C23 Cu02 53.4(4) . . ? C24 C23 Cu02 171.9(6) . . ? N03 C19 H04I 109.5 . . ? N03 C19 H04J 109.5 . . ? H04I C19 H04J 109.5 . . ? N03 C19 H04K 109.5 . . ? H04I C19 H04K 109.5 . . ? H04J C19 H04K 109.5 . . ? C23 O05 Cu02 96.0(5) . . ? C18 C17 N03 111.2(9) . . ? C18 C17 H05A 109.4 . . ? N03 C17 H05A 109.4 . . ? C18 C17 H05B 109.4 . . ? N03 C17 H05B 109.4 . . ? H05A C17 H05B 108.0 . . ? C07 O02 Cu01 81.4(5) . . ? N01 C01 C02 109.2(8) . . ? N01 C01 H06A 109.8 . . ? C02 C01 H06A 109.8 . . ? N01 C01 H06B 109.8 . . ? C02 C01 H06B 109.8 . . ? H06A C01 H06B 108.3 . . ? C17 C18 N04 110.7(9) . . ? C17 C18 H06C 109.5 . . ? N04 C18 H06C 109.5 . . ? C17 C18 H06D 109.5 . . ? N04 C18 H06D 109.5 . . ? H06C C18 H06D 108.1 . . ? N02 C04 H06E 109.5 . . ? N02 C04 H06F 109.5 . . ? H06E C04 H06F 109.5 . . ? N02 C04 H06G 109.5 . . ? H06E C04 H06G 109.5 . . ? H06F C04 H06G 109.5 . . ? O02 C07 O01 121.8(7) . . ? O02 C07 C08 120.4(7) . . ? O01 C07 C08 117.8(7) . . ? O02 C07 Cu01 69.5(4) . . ? O01 C07 Cu01 52.2(4) . . ? C08 C07 Cu01 170.1(6) . . ? O08 C28 O07 122.9(8) . . ? O08 C28 C29 122.4(8) . . ? O07 C28 C29 114.7(7) . . ? Cl05 C34 Cl06 111.0(6) . . ? Cl05 C34 Cl04 110.5(7) . . ? Cl06 C34 Cl04 109.1(6) . . ? Cl05 C34 H009 108.7 . . ? Cl06 C34 H009 108.7 . . ? Cl04 C34 H009 108.7 . . ? C19 N03 C17 110.2(8) . . ? C19 N03 C20 110.2(8) . . ? C17 N03 C20 112.4(8) . . ? C19 N03 Cu02 108.7(6) . . ? C17 N03 Cu02 104.8(6) . . ? C20 N03 Cu02 110.5(6) . . ? C05 N01 C06 111.1(8) . . ? C05 N01 C01 110.0(8) . . ? C06 N01 C01 107.7(8) . . ? C05 N01 Cu01 114.0(6) . . ? C06 N01 Cu01 109.0(6) . . ? C01 N01 Cu01 104.8(5) . . ? C18 N04 C21 110.6(8) . . ? C18 N04 C22 111.4(8) . . ? C21 N04 C22 108.1(8) . . ? C18 N04 Cu02 104.5(6) . . ? C21 N04 Cu02 113.1(6) . . ? C22 N04 Cu02 109.2(6) . . ? C03 N02 C02 108.9(8) . . ? C03 N02 C04 113.1(10) . . ? C02 N02 C04 109.5(9) . . ? C03 N02 Cu01 112.4(7) . . ? C02 N02 Cu01 104.0(5) . . ? C04 N02 Cu01 108.5(6) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.901 _refine_diff_density_min -0.834 _refine_diff_density_rms 0.120 data_in-1 _database_code_depnum_ccdc_archive 'CCDC 776680' #TrackingRef '- cif-1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H0 Cu In0 O P2 S2' _exptl_crystal_recrystallization_method Toluene _chemical_melting_point ? _exptl_crystal_description Rod _exptl_crystal_colour Yellow _diffrn_ambient_temperature 293(2) _chemical_formula_weight 698.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2597(15) _cell_length_b 12.9616(6) _cell_length_c 14.459(2) _cell_angle_alpha 86.108(7) _cell_angle_beta 75.151(14) _cell_angle_gamma 74.714(7) _cell_volume 1792.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.293 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 690 _exptl_absorpt_coefficient_mu 0.844 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12577 _diffrn_reflns_av_R_equivalents 0.0461 _diffrn_reflns_av_sigmaI/netI 0.0535 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 27.80 _reflns_number_total 7722 _reflns_number_gt 5289 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0886P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7722 _refine_ls_number_parameters 441 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.0745 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.1366 _refine_ls_wR_factor_gt 0.1277 _refine_ls_goodness_of_fit_ref 0.935 _refine_ls_restrained_S_all 0.941 _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 Cu01 Cu 0.91308(3) 0.66774(3) 0.76980(2) 0.04018(12) Uani 1 1 d . . . S01 S 1.13108(8) 0.70075(8) 0.70268(6) 0.0557(2) Uani 1 1 d . A . P02 P 0.88474(7) 0.50301(6) 0.75488(5) 0.03737(17) Uani 1 1 d . . . P01 P 0.75924(7) 0.80365(6) 0.86242(5) 0.03641(17) Uani 1 1 d . . . O01 O 0.9325(2) 0.7645(2) 0.61611(18) 0.0729(7) Uani 1 1 d . A . C30 C 0.8474(3) 0.4359(2) 0.87007(19) 0.0378(6) Uani 1 1 d . . . S02 S 1.2906(3) 0.8326(3) 0.53140(19) 0.0947(10) Uani 0.595(4) 1 d PD A 1 C02 C 1.1331(3) 0.8195(3) 0.5385(2) 0.0638(9) Uani 0.595(4) 1 d PD A 1 C03 C 1.0837(10) 0.8713(9) 0.4611(7) 0.0947(10) Uani 0.595(4) 1 d PD A 1 H03 H 0.9941 0.8747 0.4561 0.114 Uiso 0.595(4) 1 calc PR A 1 C04 C 1.1704(10) 0.9157(9) 0.3944(7) 0.101(3) Uani 0.595(4) 1 d PD A 1 H04 H 1.1520 0.9477 0.3379 0.122 Uiso 0.595(4) 1 calc PR A 1 C05 C 1.2909(12) 0.9061(10) 0.4235(6) 0.097(4) Uani 0.595(4) 1 d PD A 1 H05 H 1.3637 0.9348 0.3904 0.117 Uiso 0.595(4) 1 calc PR A 1 S02A S 1.0772(6) 0.8738(4) 0.4463(3) 0.1110(17) Uani 0.405(4) 1 d PD A 2 C02A C 1.1331(3) 0.8195(3) 0.5385(2) 0.0638(9) Uani 0.405(4) 1 d PD A 2 C03A C 1.2687(11) 0.8316(12) 0.5260(11) 0.1110(17) Uani 0.405(4) 1 d PD A 2 H03A H 1.3149 0.8064 0.5738 0.133 Uiso 0.405(4) 1 calc PR A 2 C04A C 1.3351(18) 0.8777(14) 0.4486(9) 0.101(3) Uani 0.405(4) 1 d PD A 2 H04A H 1.4265 0.8839 0.4326 0.122 Uiso 0.405(4) 1 calc PR A 2 C05A C 1.2337(14) 0.9133(18) 0.3988(13) 0.097(4) Uani 0.405(4) 1 d PD A 2 H05A H 1.2466 0.9552 0.3441 0.117 Uiso 0.405(4) 1 calc PR A 2 C01 C 1.0543(3) 0.7652(3) 0.6164(2) 0.0513(8) Uani 1 1 d . . . C18 C 0.7056(3) 0.7756(2) 0.99040(19) 0.0385(6) Uani 1 1 d . . . C16 C 0.3471(3) 0.8744(3) 0.8530(3) 0.0537(8) Uani 1 1 d . . . H16 H 0.2611 0.8767 0.8952 0.064 Uiso 1 1 calc R . . C20 C 0.6519(4) 0.8220(3) 1.1565(2) 0.0639(9) Uani 1 1 d . . . H20 H 0.6421 0.8714 1.2032 0.077 Uiso 1 1 calc R . . C23 C 0.6810(3) 0.6771(2) 1.0187(2) 0.0503(7) Uani 1 1 d . . . H23 H 0.6914 0.6272 0.9723 0.060 Uiso 1 1 calc R . . C06 C 0.8048(3) 0.9319(2) 0.8619(2) 0.0396(6) Uani 1 1 d . . . C34 C 0.9184(4) 0.3722(3) 1.0150(2) 0.0568(8) Uani 1 1 d . . . H34 H 0.9867 0.3561 1.0491 0.068 Uiso 1 1 calc R . . C33 C 0.7897(4) 0.3554(3) 1.0560(2) 0.0584(9) Uani 1 1 d . . . H33 H 0.7701 0.3294 1.1182 0.070 Uiso 1 1 calc R . . C07 C 0.9375(3) 0.9306(3) 0.8675(3) 0.0666(10) Uani 1 1 d . . . H7 H 1.0046 0.8659 0.8650 0.080 Uiso 1 1 calc R . . C13 C 0.6030(3) 0.8652(3) 0.7282(2) 0.0507(7) Uani 1 1 d . . . H13 H 0.6890 0.8611 0.6853 0.061 Uiso 1 1 calc R . . C32 C 0.6897(3) 0.3772(3) 1.0047(2) 0.0543(8) Uani 1 1 d . . . H32 H 0.6026 0.3650 1.0322 0.065 Uiso 1 1 calc R . . C36 C 1.0335(3) 0.4070(2) 0.6805(2) 0.0427(6) Uani 1 1 d . . . C10 C 0.7441(4) 1.1239(3) 0.8675(2) 0.0533(8) Uani 1 1 d . . . H10 H 0.6791 1.1890 0.8659 0.064 Uiso 1 1 calc R . . C24 C 0.7378(3) 0.4992(2) 0.7065(2) 0.0412(6) Uani 1 1 d . . . C21 C 0.6276(4) 0.7241(3) 1.1834(3) 0.0656(9) Uani 1 1 d . . . H21 H 0.6019 0.7070 1.2479 0.079 Uiso 1 1 calc R . . C17 C 0.4661(3) 0.8495(2) 0.8869(2) 0.0455(7) Uani 1 1 d . . . H17 H 0.4592 0.8362 0.9518 0.055 Uiso 1 1 calc R . . C12 C 0.5951(3) 0.8440(2) 0.8254(2) 0.0385(6) Uani 1 1 d . . . C14 C 0.4825(3) 0.8923(3) 0.6962(2) 0.0576(8) Uani 1 1 d . . . H14 H 0.4878 0.9084 0.6319 0.069 Uiso 1 1 calc R . . C28 C 0.6190(5) 0.4168(4) 0.6222(3) 0.0885(14) Uani 1 1 d . . . H28 H 0.6190 0.3596 0.5868 0.106 Uiso 1 1 calc R . . C25 C 0.6210(3) 0.5844(2) 0.7255(2) 0.0482(7) Uani 1 1 d . . . H25 H 0.6209 0.6425 0.7599 0.058 Uiso 1 1 calc R . . C09 C 0.8754(4) 1.1216(3) 0.8767(3) 0.0612(9) Uani 1 1 d . . . H9 H 0.8987 1.1850 0.8828 0.073 Uiso 1 1 calc R . . C27 C 0.5031(4) 0.5019(3) 0.6425(3) 0.0668(10) Uani 1 1 d . . . H27 H 0.4248 0.5024 0.6210 0.080 Uiso 1 1 calc R . . C08 C 0.9711(4) 1.0258(3) 0.8768(3) 0.0769(12) Uani 1 1 d . . . H8 H 1.0596 1.0243 0.8832 0.092 Uiso 1 1 calc R . . C26 C 0.5044(3) 0.5851(3) 0.6943(2) 0.0571(8) Uani 1 1 d . . . H26 H 0.4263 0.6428 0.7088 0.068 Uiso 1 1 calc R . . C40 C 1.2214(5) 0.3757(5) 0.5403(3) 0.0982(16) Uani 1 1 d . . . H40 H 1.2728 0.4019 0.4855 0.118 Uiso 1 1 calc R . . C37 C 1.0669(4) 0.2990(3) 0.7003(3) 0.0710(10) Uani 1 1 d . . . H37 H 1.0151 0.2723 0.7545 0.085 Uiso 1 1 calc R . . C11 C 0.7095(3) 1.0288(2) 0.8605(2) 0.0460(7) Uani 1 1 d . . . H11 H 0.6207 1.0305 0.8549 0.055 Uiso 1 1 calc R . . C38 C 1.1789(5) 0.2298(4) 0.6387(3) 0.0861(13) Uani 1 1 d . . . H38 H 1.2019 0.1570 0.6524 0.103 Uiso 1 1 calc R . . C29 C 0.7358(4) 0.4154(3) 0.6538(3) 0.0713(11) Uani 1 1 d . . . H29 H 0.8135 0.3574 0.6394 0.086 Uiso 1 1 calc R . . C31 C 0.7176(3) 0.4170(2) 0.9127(2) 0.0436(7) Uani 1 1 d . . . H31 H 0.6490 0.4315 0.8789 0.052 Uiso 1 1 calc R . . C35 C 0.9476(3) 0.4130(3) 0.9230(2) 0.0482(7) Uani 1 1 d . . . H35 H 1.0349 0.4251 0.8963 0.058 Uiso 1 1 calc R . . C15 C 0.3547(3) 0.8960(3) 0.7581(2) 0.0556(8) Uani 1 1 d . . . H15 H 0.2744 0.9128 0.7356 0.067 Uiso 1 1 calc R . . C22 C 0.6413(3) 0.6509(3) 1.1144(2) 0.0584(8) Uani 1 1 d . . . H22 H 0.6241 0.5845 1.1320 0.070 Uiso 1 1 calc R . . C39 C 1.2534(5) 0.2681(4) 0.5599(3) 0.0908(14) Uani 1 1 d . . . H39 H 1.3266 0.2216 0.5186 0.109 Uiso 1 1 calc R . . C41 C 1.1131(4) 0.4450(3) 0.6017(2) 0.0714(10) Uani 1 1 d . . . H41 H 1.0942 0.5181 0.5893 0.086 Uiso 1 1 calc R . . C019 C 0.6906(3) 0.8487(3) 1.0611(2) 0.0535(8) Uani 1 1 d . . . H019 H 0.7067 0.9156 1.0441 0.064 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu01 0.0386(2) 0.0316(2) 0.0506(2) -0.00170(15) -0.00608(15) -0.01386(15) S01 0.0430(4) 0.0644(6) 0.0628(5) 0.0051(4) -0.0103(4) -0.0231(4) P02 0.0359(4) 0.0294(4) 0.0470(4) -0.0025(3) -0.0068(3) -0.0114(3) P01 0.0353(4) 0.0276(4) 0.0480(4) -0.0028(3) -0.0086(3) -0.0118(3) O01 0.0537(14) 0.097(2) 0.0741(16) 0.0056(14) -0.0224(12) -0.0251(14) C30 0.0384(14) 0.0233(13) 0.0502(16) -0.0070(11) -0.0052(12) -0.0090(11) S02 0.1045(16) 0.126(2) 0.0732(14) -0.0065(11) 0.0059(11) -0.0879(16) C02 0.090(3) 0.055(2) 0.0469(18) -0.0072(16) -0.0047(18) -0.030(2) C03 0.1045(16) 0.126(2) 0.0732(14) -0.0065(11) 0.0059(11) -0.0879(16) C04 0.147(9) 0.095(6) 0.060(4) 0.018(4) -0.006(5) -0.050(6) C05 0.114(11) 0.104(6) 0.091(8) 0.024(5) -0.011(6) -0.078(9) S02A 0.193(4) 0.068(2) 0.062(2) 0.0017(15) -0.047(2) -0.003(2) C02A 0.090(3) 0.055(2) 0.0469(18) -0.0072(16) -0.0047(18) -0.030(2) C03A 0.193(4) 0.068(2) 0.062(2) 0.0017(15) -0.047(2) -0.003(2) C04A 0.147(9) 0.095(6) 0.060(4) 0.018(4) -0.006(5) -0.050(6) C05A 0.114(11) 0.104(6) 0.091(8) 0.024(5) -0.011(6) -0.078(9) C01 0.0574(19) 0.049(2) 0.0471(17) -0.0105(14) -0.0037(14) -0.0193(16) C18 0.0356(14) 0.0329(15) 0.0470(15) -0.0038(12) -0.0097(12) -0.0079(12) C16 0.0361(15) 0.048(2) 0.076(2) -0.0056(16) -0.0083(15) -0.0129(14) C20 0.088(3) 0.052(2) 0.054(2) -0.0094(16) -0.0202(18) -0.018(2) C23 0.0534(18) 0.0354(17) 0.0611(19) -0.0071(14) -0.0076(15) -0.0141(14) C06 0.0376(14) 0.0349(15) 0.0486(16) -0.0024(12) -0.0077(12) -0.0154(12) C34 0.061(2) 0.053(2) 0.061(2) -0.0009(16) -0.0239(17) -0.0148(17) C33 0.079(2) 0.044(2) 0.0509(18) 0.0018(14) -0.0123(17) -0.0176(18) C07 0.0467(18) 0.0341(18) 0.124(3) -0.0117(19) -0.0267(19) -0.0100(15) C13 0.0459(17) 0.053(2) 0.0539(18) -0.0025(14) -0.0087(14) -0.0168(15) C32 0.0556(18) 0.049(2) 0.0586(19) 0.0028(15) -0.0032(15) -0.0243(16) C36 0.0370(14) 0.0446(18) 0.0433(15) -0.0070(13) -0.0055(12) -0.0076(13) C10 0.063(2) 0.0296(16) 0.064(2) -0.0020(14) -0.0103(16) -0.0110(14) C24 0.0437(15) 0.0352(16) 0.0462(16) -0.0033(12) -0.0114(12) -0.0118(13) C21 0.075(2) 0.064(3) 0.0519(19) 0.0019(17) -0.0112(17) -0.013(2) C17 0.0424(16) 0.0376(17) 0.0559(17) -0.0051(13) -0.0073(13) -0.0126(13) C12 0.0373(14) 0.0286(14) 0.0515(16) -0.0055(12) -0.0078(12) -0.0132(11) C14 0.059(2) 0.063(2) 0.0572(19) -0.0033(16) -0.0220(16) -0.0181(17) C28 0.085(3) 0.076(3) 0.122(4) -0.042(3) -0.040(3) -0.024(2) C25 0.0488(17) 0.0389(17) 0.0572(18) -0.0095(14) -0.0119(14) -0.0106(14) C09 0.070(2) 0.0403(19) 0.075(2) -0.0116(16) -0.0019(18) -0.0288(17) C27 0.060(2) 0.077(3) 0.075(2) -0.005(2) -0.0268(19) -0.028(2) C08 0.0472(19) 0.053(2) 0.137(4) -0.022(2) -0.017(2) -0.0242(17) C26 0.0440(17) 0.062(2) 0.065(2) -0.0061(17) -0.0135(15) -0.0106(16) C40 0.095(3) 0.114(4) 0.064(3) -0.022(3) 0.025(2) -0.028(3) C37 0.078(2) 0.044(2) 0.069(2) -0.0018(17) 0.0019(19) 0.0038(18) C11 0.0502(17) 0.0329(16) 0.0570(18) -0.0023(13) -0.0126(14) -0.0142(13) C38 0.092(3) 0.060(3) 0.077(3) -0.015(2) -0.009(2) 0.024(2) C29 0.066(2) 0.047(2) 0.104(3) -0.034(2) -0.026(2) -0.0063(17) C31 0.0424(15) 0.0363(16) 0.0543(17) 0.0008(13) -0.0105(13) -0.0153(13) C35 0.0436(16) 0.0464(19) 0.0573(18) -0.0023(14) -0.0133(14) -0.0149(14) C15 0.0454(18) 0.052(2) 0.076(2) -0.0088(17) -0.0243(17) -0.0110(15) C22 0.064(2) 0.045(2) 0.064(2) 0.0066(16) -0.0062(17) -0.0204(17) C39 0.073(3) 0.102(4) 0.075(3) -0.038(3) -0.003(2) 0.011(3) C41 0.081(3) 0.060(2) 0.058(2) -0.0081(17) 0.0123(18) -0.019(2) C019 0.069(2) 0.0355(17) 0.0580(19) -0.0037(14) -0.0198(16) -0.0122(15) _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 Cu01 P02 2.2610(8) . ? Cu01 P01 2.2712(8) . ? Cu01 S01 2.3373(9) . ? S01 C01 1.700(4) . ? P02 C30 1.825(3) . ? P02 C24 1.830(3) . ? P02 C36 1.837(3) . ? P01 C18 1.831(3) . ? P01 C12 1.832(3) . ? P01 C06 1.840(3) . ? O01 C01 1.253(4) . ? C30 C31 1.394(4) . ? C30 C35 1.394(4) . ? S02 C02 1.646(4) . ? S02 C05 1.772(7) . ? C02 C03 1.403(8) . ? C02 C01 1.464(5) . ? C03 C04 1.345(10) . ? C03 H03 0.9300 . ? C04 C05 1.378(10) . ? C04 H04 0.9300 . ? C05 H05 0.9300 . ? S02A C05A 1.770(7) . ? C03A C04A 1.344(10) . ? C03A H03A 0.9300 . ? C04A C05A 1.378(11) . ? C04A H04A 0.9300 . ? C05A H05A 0.9300 . ? C18 C23 1.382(4) . ? C18 C019 1.393(4) . ? C16 C15 1.369(5) . ? C16 C17 1.383(4) . ? C16 H16 0.9300 . ? C20 C21 1.369(5) . ? C20 C019 1.380(5) . ? C20 H20 0.9300 . ? C23 C22 1.384(4) . ? C23 H23 0.9300 . ? C06 C11 1.376(4) . ? C06 C07 1.380(4) . ? C34 C33 1.369(5) . ? C34 C35 1.387(5) . ? C34 H34 0.9300 . ? C33 C32 1.376(5) . ? C33 H33 0.9300 . ? C07 C08 1.390(5) . ? C07 H7 0.9300 . ? C13 C14 1.381(4) . ? C13 C12 1.399(4) . ? C13 H13 0.9300 . ? C32 C31 1.381(4) . ? C32 H32 0.9300 . ? C36 C41 1.366(4) . ? C36 C37 1.379(5) . ? C10 C09 1.380(5) . ? C10 C11 1.387(4) . ? C10 H10 0.9300 . ? C24 C29 1.375(4) . ? C24 C25 1.381(4) . ? C21 C22 1.379(5) . ? C21 H21 0.9300 . ? C17 C12 1.380(4) . ? C17 H17 0.9300 . ? C14 C15 1.376(5) . ? C14 H14 0.9300 . ? C28 C27 1.374(6) . ? C28 C29 1.383(5) . ? C28 H28 0.9300 . ? C25 C26 1.380(4) . ? C25 H25 0.9300 . ? C09 C08 1.365(5) . ? C09 H9 0.9300 . ? C27 C26 1.360(5) . ? C27 H27 0.9300 . ? C08 H8 0.9300 . ? C26 H26 0.9300 . ? C40 C39 1.374(7) . ? C40 C41 1.381(6) . ? C40 H40 0.9300 . ? C37 C38 1.400(5) . ? C37 H37 0.9300 . ? C11 H11 0.9300 . ? C38 C39 1.343(6) . ? C38 H38 0.9300 . ? C29 H29 0.9300 . ? C31 H31 0.9300 . ? C35 H35 0.9300 . ? C15 H15 0.9300 . ? C22 H22 0.9300 . ? C39 H39 0.9300 . ? C41 H41 0.9300 . ? C019 H019 0.9300 . ? 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 P02 Cu01 P01 126.72(3) . . ? P02 Cu01 S01 119.01(3) . . ? P01 Cu01 S01 113.68(3) . . ? C01 S01 Cu01 84.20(11) . . ? C30 P02 C24 102.67(12) . . ? C30 P02 C36 104.49(13) . . ? C24 P02 C36 103.88(13) . . ? C30 P02 Cu01 112.24(9) . . ? C24 P02 Cu01 115.56(10) . . ? C36 P02 Cu01 116.48(10) . . ? C18 P01 C12 104.03(12) . . ? C18 P01 C06 102.52(12) . . ? C12 P01 C06 102.14(12) . . ? C18 P01 Cu01 116.47(9) . . ? C12 P01 Cu01 110.90(9) . . ? C06 P01 Cu01 118.87(9) . . ? C31 C30 C35 118.0(3) . . ? C31 C30 P02 123.1(2) . . ? C35 C30 P02 118.6(2) . . ? C02 S02 C05 91.2(4) . . ? C03 C02 C01 125.1(4) . . ? C03 C02 S02 110.1(4) . . ? C01 C02 S02 124.7(3) . . ? C04 C03 C02 117.8(8) . . ? C04 C03 H03 121.1 . . ? C02 C03 H03 121.1 . . ? C03 C04 C05 108.7(9) . . ? C03 C04 H04 125.6 . . ? C05 C04 H04 125.6 . . ? C04 C05 S02 112.0(7) . . ? C04 C05 H05 124.0 . . ? S02 C05 H05 124.0 . . ? C04A C03A H03A 118.3 . . ? C03A C04A C05A 102.5(15) . . ? C03A C04A H04A 128.7 . . ? C05A C04A H04A 128.7 . . ? C04A C05A S02A 115.3(12) . . ? C04A C05A H05A 122.3 . . ? S02A C05A H05A 122.3 . . ? O01 C01 C02 118.8(3) . . ? O01 C01 S01 121.4(3) . . ? C02 C01 S01 119.7(2) . . ? C23 C18 C019 118.2(3) . . ? C23 C18 P01 118.9(2) . . ? C019 C18 P01 123.0(2) . . ? C15 C16 C17 120.7(3) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C21 C20 C019 121.0(3) . . ? C21 C20 H20 119.5 . . ? C019 C20 H20 119.5 . . ? C18 C23 C22 121.5(3) . . ? C18 C23 H23 119.2 . . ? C22 C23 H23 119.2 . . ? C11 C06 C07 118.9(3) . . ? C11 C06 P01 122.3(2) . . ? C07 C06 P01 118.7(2) . . ? C33 C34 C35 120.6(3) . . ? C33 C34 H34 119.7 . . ? C35 C34 H34 119.7 . . ? C34 C33 C32 119.6(3) . . ? C34 C33 H33 120.2 . . ? C32 C33 H33 120.2 . . ? C06 C07 C08 120.1(3) . . ? C06 C07 H7 119.9 . . ? C08 C07 H7 119.9 . . ? C14 C13 C12 119.7(3) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C33 C32 C31 120.5(3) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C41 C36 C37 119.1(3) . . ? C41 C36 P02 118.0(3) . . ? C37 C36 P02 122.9(2) . . ? C09 C10 C11 119.7(3) . . ? C09 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C29 C24 C25 118.0(3) . . ? C29 C24 P02 123.9(3) . . ? C25 C24 P02 118.1(2) . . ? C20 C21 C22 119.7(3) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C12 C17 C16 120.6(3) . . ? C12 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C17 C12 C13 118.7(3) . . ? C17 C12 P01 123.7(2) . . ? C13 C12 P01 117.5(2) . . ? C15 C14 C13 121.0(3) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C27 C28 C29 120.8(3) . . ? C27 C28 H28 119.6 . . ? C29 C28 H28 119.6 . . ? C26 C25 C24 121.2(3) . . ? C26 C25 H25 119.4 . . ? C24 C25 H25 119.4 . . ? C08 C09 C10 119.8(3) . . ? C08 C09 H9 120.1 . . ? C10 C09 H9 120.1 . . ? C26 C27 C28 119.1(3) . . ? C26 C27 H27 120.5 . . ? C28 C27 H27 120.5 . . ? C09 C08 C07 120.5(3) . . ? C09 C08 H8 119.7 . . ? C07 C08 H8 119.7 . . ? C27 C26 C25 120.4(3) . . ? C27 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C39 C40 C41 120.1(4) . . ? C39 C40 H40 119.9 . . ? C41 C40 H40 119.9 . . ? C36 C37 C38 119.9(4) . . ? C36 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? C06 C11 C10 120.9(3) . . ? C06 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C39 C38 C37 120.2(4) . . ? C39 C38 H38 119.9 . . ? C37 C38 H38 119.9 . . ? C24 C29 C28 120.5(3) . . ? C24 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C32 C31 C30 120.8(3) . . ? C32 C31 H31 119.6 . . ? C30 C31 H31 119.6 . . ? C34 C35 C30 120.6(3) . . ? C34 C35 H35 119.7 . . ? C30 C35 H35 119.7 . . ? C16 C15 C14 119.3(3) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C21 C22 C23 119.4(3) . . ? C21 C22 H22 120.3 . . ? C23 C22 H22 120.3 . . ? C38 C39 C40 120.1(4) . . ? C38 C39 H39 119.9 . . ? C40 C39 H39 119.9 . . ? C36 C41 C40 120.5(4) . . ? C36 C41 H41 119.8 . . ? C40 C41 H41 119.8 . . ? C20 C019 C18 120.1(3) . . ? C20 C019 H019 119.9 . . ? C18 C019 H019 119.9 . . ? _diffrn_measured_fraction_theta_max 0.926 _diffrn_reflns_theta_full 27.80 _diffrn_measured_fraction_theta_full 0.826 _refine_diff_density_max 0.703 _refine_diff_density_min -0.764 _refine_diff_density_rms 0.076 # Attachment '- cif-2.cif' data_cd-cu _database_code_depnum_ccdc_archive 'CCDC 776681' #TrackingRef '- cif-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H37 Cu O2 P2 S4' _exptl_crystal_recrystallization_method 'Chloroform and Petroleum ether(60-80)' _chemical_melting_point ? _exptl_crystal_description rod _exptl_crystal_colour red _diffrn_ambient_temperature 293(2) _chemical_formula_weight 875.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'P 21 21 21' _symmetry_int_tables_number 19 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 13.1000(3) _cell_length_b 17.9804(4) _cell_length_c 18.1855(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4283.47(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.37 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.358 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 0.817 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.83403 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16813 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0671 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 29.01 _reflns_number_total 9378 _reflns_number_gt 6339 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0539P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.003(13) _refine_ls_number_reflns 9378 _refine_ls_number_parameters 478 _refine_ls_number_restraints 32 _refine_ls_R_factor_all 0.0727 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.0980 _refine_ls_wR_factor_gt 0.0914 _refine_ls_goodness_of_fit_ref 0.916 _refine_ls_restrained_S_all 0.958 _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 S03 S 0.8556(2) 0.74163(14) 0.46479(15) 0.0677(5) Uani 0.637(2) 1 d PD A 1 C38 C 0.9525(4) 0.7387(2) 0.5284(2) 0.0677(5) Uani 0.637(2) 1 d PD A 1 C39 C 0.9659(7) 0.8093(5) 0.5477(4) 0.0677(5) Uani 0.637(2) 1 d PD A 1 H39 H 1.0122 0.8219 0.5844 0.081 Uiso 0.637(2) 1 calc PR A 1 C40 C 0.9103(7) 0.8636(5) 0.5127(5) 0.0677(5) Uani 0.637(2) 1 d PD A 1 H40 H 0.9168 0.9142 0.5221 0.081 Uiso 0.637(2) 1 calc PR A 1 C41 C 0.8446(7) 0.8345(5) 0.4626(5) 0.0677(5) Uani 0.637(2) 1 d PD A 1 H41 H 0.8010 0.8614 0.4323 0.081 Uiso 0.637(2) 1 calc PR A 1 C39A C 0.8697(14) 0.7556(9) 0.4784(10) 0.0677(5) Uani 0.363(2) 1 d PD A 2 H39A H 0.8285 0.7238 0.4511 0.081 Uiso 0.363(2) 1 calc PR A 2 C38A C 0.9525(4) 0.7387(2) 0.5284(2) 0.0677(5) Uani 0.363(2) 1 d PD A 2 S03A S 1.0032(3) 0.8172(2) 0.5687(2) 0.0677(5) Uani 0.363(2) 1 d PD A 2 C41A C 0.9410(12) 0.8750(7) 0.5252(8) 0.0677(5) Uani 0.363(2) 1 d PD A 2 H41A H 0.9500 0.9262 0.5269 0.081 Uiso 0.363(2) 1 calc PR A 2 C40A C 0.8690(13) 0.8372(8) 0.4828(8) 0.0677(5) Uani 0.363(2) 1 d PD A 2 H40A H 0.8200 0.8640 0.4570 0.081 Uiso 0.363(2) 1 calc PR A 2 S04 S 1.17130(16) 0.44206(13) 0.82330(12) 0.0675(4) Uani 0.637(2) 1 d PD A 3 C43 C 1.2079(3) 0.5059(3) 0.7629(2) 0.0675(4) Uani 0.637(2) 1 d PD A 3 C44 C 1.3120(9) 0.5374(6) 0.7814(6) 0.0675(4) Uani 0.637(2) 1 d PD A 3 H44 H 1.3472 0.5752 0.7573 0.081 Uiso 0.637(2) 1 calc PR A 3 C45 C 1.3436(7) 0.4956(5) 0.8446(6) 0.0675(4) Uani 0.637(2) 1 d PD A 3 H45 H 1.4082 0.5007 0.8653 0.081 Uiso 0.637(2) 1 calc PR A 3 C46 C 1.2743(6) 0.4490(6) 0.8715(5) 0.0675(4) Uani 0.637(2) 1 d PD A 3 H46 H 1.2844 0.4225 0.9148 0.081 Uiso 0.637(2) 1 calc PR A 3 C44A C 1.2154(10) 0.4387(8) 0.8108(7) 0.0675(4) Uani 0.363(2) 1 d PD A 4 H44A H 1.1728 0.3973 0.8096 0.081 Uiso 0.363(2) 1 calc PR A 4 C43A C 1.2079(3) 0.5059(3) 0.7629(2) 0.0675(4) Uani 0.363(2) 1 d PD A 4 S04A S 1.3218(4) 0.5492(3) 0.7672(3) 0.0675(4) Uani 0.363(2) 1 d PD A 4 C46A C 1.3598(12) 0.5105(8) 0.8422(9) 0.0675(4) Uani 0.363(2) 1 d PD A 4 H46A H 1.4145 0.5270 0.8704 0.081 Uiso 0.363(2) 1 calc PR A 4 C45A C 1.3008(11) 0.4499(10) 0.8590(8) 0.0675(4) Uani 0.363(2) 1 d PD A 4 H45A H 1.3150 0.4186 0.8984 0.081 Uiso 0.363(2) 1 calc PR A 4 Cu01 Cu 0.94729(3) 0.49419(2) 0.58978(2) 0.03774(11) Uani 1 1 d . . . S01 S 0.97743(9) 0.59056(5) 0.50468(5) 0.0504(3) Uani 1 1 d . A . P02 P 1.01704(8) 0.38506(5) 0.55117(5) 0.0356(2) Uani 1 1 d . . . P01 P 0.77436(7) 0.50584(6) 0.60451(4) 0.0384(2) Uani 1 1 d . . . S02 S 1.01619(7) 0.50139(7) 0.70736(4) 0.0479(2) Uani 1 1 d . A . O02 O 1.1725(2) 0.57944(15) 0.66011(15) 0.0553(7) Uani 1 1 d . A . O01 O 1.0577(3) 0.67463(17) 0.60795(16) 0.0617(8) Uani 1 1 d . A . C31 C 1.1549(3) 0.37797(19) 0.56735(17) 0.0376(8) Uani 1 1 d . . . C13 C 0.7385(3) 0.6022(2) 0.6270(2) 0.0432(9) Uani 1 1 d . . . C02 C 0.7634(4) 0.3979(3) 0.7133(2) 0.0594(11) Uani 1 1 d . . . H015 H 0.8306 0.3873 0.7006 0.071 Uiso 1 1 calc R . . C37 C 1.0003(3) 0.6692(2) 0.5518(2) 0.0461(10) Uani 1 1 d . . . C07 C 0.6994(3) 0.4812(2) 0.52283(18) 0.0415(9) Uani 1 1 d . . . C01 C 0.7108(3) 0.4541(2) 0.6770(2) 0.0420(9) Uani 1 1 d . . . C30 C 0.9286(3) 0.3936(2) 0.4140(2) 0.0602(11) Uani 1 1 d . . . H020 H 0.8861 0.4284 0.4361 0.072 Uiso 1 1 calc R . . C32 C 1.2029(3) 0.3157(2) 0.5939(2) 0.0561(10) Uani 1 1 d . . . H021 H 1.1651 0.2730 0.6033 0.067 Uiso 1 1 calc R . . C14 C 0.6560(4) 0.6389(3) 0.5988(3) 0.0714(14) Uani 1 1 d . . . H023 H 0.6141 0.6150 0.5649 0.086 Uiso 1 1 calc R . . C20 C 0.8936(3) 0.2594(2) 0.5698(2) 0.0545(11) Uani 1 1 d . . . H20 H 0.8757 0.2655 0.5207 0.065 Uiso 1 1 calc R . . C17 C 0.7773(4) 0.7108(3) 0.6982(3) 0.0803(16) Uani 1 1 d . . . H025 H 0.8173 0.7342 0.7336 0.096 Uiso 1 1 calc R . . C21 C 0.8484(4) 0.2030(3) 0.6113(3) 0.0738(14) Uani 1 1 d . . . H026 H 0.8005 0.1715 0.5899 0.089 Uiso 1 1 calc R . . C04 C 0.6169(5) 0.3707(3) 0.7863(3) 0.0811(18) Uani 1 1 d . . . H027 H 0.5863 0.3439 0.8242 0.097 Uiso 1 1 calc R . . C25 C 1.0024(3) 0.3592(2) 0.45474(19) 0.0431(9) Uani 1 1 d . . . C22 C 0.8749(5) 0.1942(3) 0.6836(3) 0.0815(16) Uani 1 1 d . . . H030 H 0.8455 0.1562 0.7111 0.098 Uiso 1 1 calc R . . C23 C 0.9442(4) 0.2409(3) 0.7158(3) 0.0782(15) Uani 1 1 d . . . H23 H 0.9611 0.2350 0.7652 0.094 Uiso 1 1 calc R . . C33 C 1.3067(4) 0.3158(3) 0.6070(3) 0.0710(14) Uani 1 1 d . . . H032 H 1.3382 0.2733 0.6254 0.085 Uiso 1 1 calc R . . C11 C 0.6547(4) 0.5046(3) 0.3967(2) 0.0799(14) Uani 1 1 d . . . H033 H 0.6585 0.5344 0.3550 0.096 Uiso 1 1 calc R . . C35 C 1.3167(4) 0.4392(3) 0.5658(3) 0.0786(16) Uani 1 1 d . . . H034 H 1.3556 0.4812 0.5553 0.094 Uiso 1 1 calc R . . C12 C 0.7066(4) 0.5250(2) 0.4596(2) 0.0647(13) Uani 1 1 d . . . H035 H 0.7464 0.5678 0.4598 0.078 Uiso 1 1 calc R . . C26 C 1.0657(4) 0.3074(2) 0.4216(2) 0.0638(12) Uani 1 1 d . . . H26 H 1.1162 0.2835 0.4488 0.077 Uiso 1 1 calc R . . C06 C 0.6103(4) 0.4643(3) 0.6965(3) 0.0764(15) Uani 1 1 d . . . H038 H 0.5731 0.5013 0.6728 0.092 Uiso 1 1 calc R . . C24 C 0.9887(4) 0.2966(2) 0.6751(2) 0.0563(11) Uani 1 1 d . . . H24 H 1.0355 0.3283 0.6973 0.068 Uiso 1 1 calc R . . C36 C 1.2134(3) 0.4406(2) 0.5536(2) 0.0538(11) Uani 1 1 d . . . H36 H 1.1826 0.4837 0.5361 0.065 Uiso 1 1 calc R . . C18 C 0.8011(4) 0.6394(3) 0.6760(3) 0.0619(12) Uani 1 1 d . . . H041 H 0.8595 0.6162 0.6940 0.074 Uiso 1 1 calc R . . C29 C 0.9164(5) 0.3770(4) 0.3394(3) 0.092(2) Uani 1 1 d . . . H042 H 0.8661 0.4003 0.3116 0.111 Uiso 1 1 calc R . . C03 C 0.7162(5) 0.3575(3) 0.7685(3) 0.0773(15) Uani 1 1 d . . . H043 H 0.7526 0.3211 0.7936 0.093 Uiso 1 1 calc R . . C08 C 0.6436(4) 0.4174(3) 0.5200(2) 0.0620(12) Uani 1 1 d . . . H044 H 0.6398 0.3871 0.5614 0.074 Uiso 1 1 calc R . . C34 C 1.3629(4) 0.3777(3) 0.5931(3) 0.0771(14) Uani 1 1 d . . . H34 H 1.4328 0.3778 0.6021 0.092 Uiso 1 1 calc R . . C05 C 0.5625(5) 0.4228(3) 0.7489(3) 0.0903(18) Uani 1 1 d . . . H046 H 0.4936 0.4301 0.7590 0.108 Uiso 1 1 calc R . . C19 C 0.9648(3) 0.30617(18) 0.60130(19) 0.0404(9) Uani 1 1 d . . . C16 C 0.6944(5) 0.7478(3) 0.6683(3) 0.0768(15) Uani 1 1 d . . . H048 H 0.6802 0.7968 0.6811 0.092 Uiso 1 1 calc R . . C15 C 0.6340(5) 0.7105(3) 0.6196(3) 0.094(2) Uani 1 1 d . . . H049 H 0.5769 0.7340 0.6001 0.113 Uiso 1 1 calc R . . C10 C 0.5971(4) 0.4403(3) 0.3952(3) 0.0759(14) Uani 1 1 d . . . H050 H 0.5619 0.4269 0.3528 0.091 Uiso 1 1 calc R . . C09 C 0.5921(4) 0.3966(3) 0.4563(3) 0.0811(16) Uani 1 1 d . . . H053 H 0.5543 0.3529 0.4555 0.097 Uiso 1 1 calc R . . C27 C 1.0532(5) 0.2914(3) 0.3476(3) 0.0901(19) Uani 1 1 d . . . H27 H 1.0956 0.2567 0.3252 0.108 Uiso 1 1 calc R . . C28 C 0.9807(6) 0.3254(5) 0.3081(3) 0.108(3) Uani 1 1 d . . . H055 H 0.9736 0.3140 0.2584 0.129 Uiso 1 1 calc R . . C42 C 1.1372(3) 0.5321(2) 0.7056(2) 0.0414(9) Uani 1 1 d . . . H001 H 1.091(5) 0.630(3) 0.622(3) 0.11(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S03 0.0764(12) 0.0541(9) 0.0725(11) 0.0029(8) -0.0073(8) 0.0092(9) C38 0.0764(12) 0.0541(9) 0.0725(11) 0.0029(8) -0.0073(8) 0.0092(9) C39 0.0764(12) 0.0541(9) 0.0725(11) 0.0029(8) -0.0073(8) 0.0092(9) C40 0.0764(12) 0.0541(9) 0.0725(11) 0.0029(8) -0.0073(8) 0.0092(9) C41 0.0764(12) 0.0541(9) 0.0725(11) 0.0029(8) -0.0073(8) 0.0092(9) C39A 0.0764(12) 0.0541(9) 0.0725(11) 0.0029(8) -0.0073(8) 0.0092(9) C38A 0.0764(12) 0.0541(9) 0.0725(11) 0.0029(8) -0.0073(8) 0.0092(9) S03A 0.0764(12) 0.0541(9) 0.0725(11) 0.0029(8) -0.0073(8) 0.0092(9) C41A 0.0764(12) 0.0541(9) 0.0725(11) 0.0029(8) -0.0073(8) 0.0092(9) C40A 0.0764(12) 0.0541(9) 0.0725(11) 0.0029(8) -0.0073(8) 0.0092(9) S04 0.0563(10) 0.0757(10) 0.0706(10) 0.0006(7) -0.0192(8) 0.0048(9) C43 0.0563(10) 0.0757(10) 0.0706(10) 0.0006(7) -0.0192(8) 0.0048(9) C44 0.0563(10) 0.0757(10) 0.0706(10) 0.0006(7) -0.0192(8) 0.0048(9) C45 0.0563(10) 0.0757(10) 0.0706(10) 0.0006(7) -0.0192(8) 0.0048(9) C46 0.0563(10) 0.0757(10) 0.0706(10) 0.0006(7) -0.0192(8) 0.0048(9) C44A 0.0563(10) 0.0757(10) 0.0706(10) 0.0006(7) -0.0192(8) 0.0048(9) C43A 0.0563(10) 0.0757(10) 0.0706(10) 0.0006(7) -0.0192(8) 0.0048(9) S04A 0.0563(10) 0.0757(10) 0.0706(10) 0.0006(7) -0.0192(8) 0.0048(9) C46A 0.0563(10) 0.0757(10) 0.0706(10) 0.0006(7) -0.0192(8) 0.0048(9) C45A 0.0563(10) 0.0757(10) 0.0706(10) 0.0006(7) -0.0192(8) 0.0048(9) Cu01 0.0364(2) 0.0365(2) 0.0404(2) -0.0011(2) -0.00339(17) -0.0017(2) S01 0.0703(8) 0.0419(5) 0.0390(5) 0.0022(4) 0.0021(5) -0.0048(5) P02 0.0397(5) 0.0322(5) 0.0351(5) 0.0028(4) -0.0009(4) -0.0026(4) P01 0.0343(4) 0.0438(5) 0.0372(4) 0.0003(5) -0.0035(3) -0.0026(5) S02 0.0389(4) 0.0677(6) 0.0372(4) 0.0001(5) -0.0056(4) -0.0093(6) O02 0.0511(18) 0.0480(16) 0.0668(18) 0.0055(14) 0.0003(15) -0.0109(15) O01 0.083(2) 0.0446(16) 0.0575(18) 0.0010(14) -0.0171(17) -0.0017(17) C31 0.039(2) 0.037(2) 0.0370(19) -0.0056(15) 0.0006(16) 0.0019(17) C13 0.039(2) 0.047(2) 0.044(2) 0.0002(18) 0.0026(17) -0.006(2) C02 0.052(3) 0.070(3) 0.057(3) 0.013(2) 0.001(2) -0.008(3) C37 0.058(3) 0.039(2) 0.041(2) 0.0085(17) 0.008(2) -0.001(2) C07 0.0347(19) 0.050(3) 0.0394(19) -0.0039(17) -0.0015(15) -0.0018(18) C01 0.038(2) 0.047(2) 0.040(2) -0.0056(17) -0.0009(17) -0.0047(19) C30 0.068(3) 0.067(3) 0.046(2) 0.006(2) -0.012(2) -0.017(2) C32 0.048(3) 0.049(2) 0.072(3) 0.011(2) -0.001(2) 0.000(2) C14 0.079(4) 0.067(3) 0.068(3) -0.013(2) -0.020(3) 0.019(3) C20 0.048(3) 0.047(2) 0.069(3) 0.004(2) 0.005(2) -0.006(2) C17 0.063(3) 0.081(4) 0.097(4) -0.046(3) 0.012(3) -0.007(3) C21 0.059(3) 0.049(3) 0.113(4) 0.014(3) -0.002(3) -0.018(2) C04 0.106(5) 0.092(4) 0.046(3) 0.002(3) 0.028(3) -0.032(4) C25 0.048(2) 0.044(2) 0.0369(18) -0.0003(17) 0.0020(19) -0.0155(19) C22 0.078(4) 0.057(3) 0.110(4) 0.039(3) 0.004(3) -0.010(3) C23 0.087(4) 0.072(3) 0.076(3) 0.036(3) 0.002(3) 0.003(3) C33 0.063(3) 0.065(3) 0.085(3) 0.005(3) -0.008(3) 0.021(3) C11 0.098(4) 0.098(4) 0.044(2) 0.008(3) -0.021(2) -0.006(4) C35 0.045(3) 0.059(3) 0.131(5) 0.003(3) 0.012(3) -0.015(3) C12 0.067(3) 0.072(3) 0.055(3) 0.003(2) -0.010(2) -0.017(2) C26 0.071(3) 0.068(3) 0.053(3) -0.014(2) 0.014(2) -0.017(3) C06 0.064(3) 0.086(4) 0.079(3) 0.006(3) 0.026(3) 0.015(3) C24 0.063(3) 0.053(2) 0.052(2) 0.014(2) -0.005(2) -0.010(2) C36 0.051(3) 0.038(2) 0.072(3) 0.005(2) 0.007(2) -0.004(2) C18 0.048(3) 0.057(3) 0.080(3) -0.019(2) 0.001(2) -0.003(2) C29 0.107(5) 0.123(5) 0.046(3) 0.011(3) -0.018(3) -0.057(4) C03 0.084(4) 0.081(3) 0.067(3) 0.023(3) -0.006(3) -0.014(3) C08 0.072(3) 0.065(3) 0.049(2) 0.008(2) -0.010(2) -0.018(3) C34 0.043(3) 0.091(4) 0.098(4) -0.016(3) -0.006(3) 0.007(3) C05 0.082(4) 0.096(4) 0.093(4) 0.003(3) 0.051(4) -0.003(4) C19 0.040(2) 0.0317(18) 0.049(2) 0.0053(16) 0.0031(18) 0.0049(16) C16 0.088(4) 0.055(3) 0.088(4) -0.002(3) 0.022(3) 0.008(3) C15 0.126(5) 0.084(4) 0.071(3) 0.006(3) -0.007(3) 0.061(4) C10 0.084(4) 0.088(4) 0.056(3) -0.009(3) -0.022(3) -0.014(3) C09 0.093(4) 0.081(3) 0.069(3) -0.007(3) -0.024(3) -0.037(3) C27 0.100(5) 0.108(4) 0.062(3) -0.040(3) 0.023(3) -0.047(4) C28 0.128(6) 0.161(7) 0.035(3) -0.013(3) 0.000(3) -0.093(6) C42 0.037(2) 0.042(2) 0.045(2) -0.0155(17) 0.0015(17) -0.0016(18) _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 S03 C41 1.676(8) . ? S03 C38 1.718(6) . ? C38 C39 1.329(9) . ? C38 C37 1.460(6) . ? C39 C40 1.374(10) . ? C39 H39 0.9300 . ? C40 C41 1.357(9) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C39A C40A 1.470(15) . ? C39A H39A 0.9300 . ? S03A C41A 1.539(12) . ? C41A C40A 1.395(14) . ? C41A H41A 0.9300 . ? C40A H40A 0.9300 . ? S04 C46 1.615(9) . ? S04 C43 1.659(5) . ? C43 C42 1.471(5) . ? C43 C44 1.514(12) . ? C44 C45 1.436(11) . ? C44 H44 0.9300 . ? C45 C46 1.328(11) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C44A C45A 1.435(15) . ? C44A H44A 0.9300 . ? S04A C46A 1.610(14) . ? C46A C45A 1.369(16) . ? C46A H46A 0.9300 . ? C45A H45A 0.9300 . ? Cu01 P02 2.2755(10) . ? Cu01 P01 2.2907(10) . ? Cu01 S02 2.3244(9) . ? Cu01 S01 2.3567(10) . ? S01 C37 1.680(4) . ? P02 C19 1.820(4) . ? P02 C25 1.824(4) . ? P02 C31 1.834(4) . ? P01 C01 1.815(4) . ? P01 C07 1.835(3) . ? P01 C13 1.842(4) . ? S02 C42 1.679(4) . ? O02 C42 1.274(4) . ? O01 C37 1.272(5) . ? O01 H001 0.95(6) . ? C31 C32 1.372(5) . ? C31 C36 1.386(5) . ? C13 C14 1.367(6) . ? C13 C18 1.382(6) . ? C02 C03 1.383(6) . ? C02 C01 1.390(6) . ? C02 H015 0.9300 . ? C07 C08 1.361(5) . ? C07 C12 1.397(5) . ? C01 C06 1.377(6) . ? C30 C25 1.366(6) . ? C30 C29 1.398(6) . ? C30 H020 0.9300 . ? C32 C33 1.380(6) . ? C32 H021 0.9300 . ? C14 C15 1.371(7) . ? C14 H023 0.9300 . ? C20 C19 1.380(5) . ? C20 C21 1.395(6) . ? C20 H20 0.9300 . ? C17 C18 1.382(6) . ? C17 C16 1.386(7) . ? C17 H025 0.9300 . ? C21 C22 1.370(7) . ? C21 H026 0.9300 . ? C04 C03 1.361(8) . ? C04 C05 1.361(8) . ? C04 H027 0.9300 . ? C25 C26 1.385(6) . ? C22 C23 1.368(7) . ? C22 H030 0.9300 . ? C23 C24 1.375(6) . ? C23 H23 0.9300 . ? C33 C34 1.358(7) . ? C33 H032 0.9300 . ? C11 C12 1.379(6) . ? C11 C10 1.381(7) . ? C11 H033 0.9300 . ? C35 C34 1.356(7) . ? C35 C36 1.371(6) . ? C35 H034 0.9300 . ? C12 H035 0.9300 . ? C26 C27 1.385(6) . ? C26 H26 0.9300 . ? C06 C05 1.363(7) . ? C06 H038 0.9300 . ? C24 C19 1.388(5) . ? C24 H24 0.9300 . ? C36 H36 0.9300 . ? C18 H041 0.9300 . ? C29 C28 1.376(10) . ? C29 H042 0.9300 . ? C03 H043 0.9300 . ? C08 C09 1.391(6) . ? C08 H044 0.9300 . ? C34 H34 0.9300 . ? C05 H046 0.9300 . ? C16 C15 1.364(8) . ? C16 H048 0.9300 . ? C15 H049 0.9300 . ? C10 C09 1.363(7) . ? C10 H050 0.9300 . ? C09 H053 0.9300 . ? C27 C28 1.340(10) . ? C27 H27 0.9300 . ? C28 H055 0.9300 . ? 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 C41 S03 C38 96.3(3) . . ? C39 C38 C37 133.2(5) . . ? C39 C38 S03 104.2(5) . . ? C37 C38 S03 122.6(3) . . ? C38 C39 C40 119.1(7) . . ? C38 C39 H39 120.4 . . ? C40 C39 H39 120.4 . . ? C41 C40 C39 111.9(7) . . ? C41 C40 H40 124.0 . . ? C39 C40 H40 124.0 . . ? C40 C41 S03 108.3(6) . . ? C40 C41 H41 125.9 . . ? S03 C41 H41 125.9 . . ? C40A C39A H39A 129.8 . . ? C40A C41A S03A 108.3(9) . . ? C40A C41A H41A 125.8 . . ? S03A C41A H41A 125.8 . . ? C41A C40A C39A 120.8(12) . . ? C41A C40A H40A 119.6 . . ? C39A C40A H40A 119.6 . . ? C46 S04 C43 93.7(4) . . ? C42 C43 C44 127.1(5) . . ? C42 C43 S04 120.5(3) . . ? C44 C43 S04 111.9(5) . . ? C45 C44 C43 104.0(7) . . ? C45 C44 H44 128.0 . . ? C43 C44 H44 128.0 . . ? C46 C45 C44 115.3(8) . . ? C46 C45 H45 122.3 . . ? C44 C45 H45 122.3 . . ? C45 C46 S04 114.8(7) . . ? C45 C46 H46 122.6 . . ? S04 C46 H46 122.6 . . ? C45A C44A H44A 126.5 . . ? C45A C46A S04A 111.0(10) . . ? C45A C46A H46A 124.5 . . ? S04A C46A H46A 124.5 . . ? C46A C45A C44A 114.6(13) . . ? C46A C45A H45A 122.7 . . ? C44A C45A H45A 122.7 . . ? P02 Cu01 P01 120.80(4) . . ? P02 Cu01 S02 100.13(4) . . ? P01 Cu01 S02 105.74(3) . . ? P02 Cu01 S01 111.35(4) . . ? P01 Cu01 S01 100.09(4) . . ? S02 Cu01 S01 119.87(4) . . ? C37 S01 Cu01 108.31(12) . . ? C19 P02 C25 104.06(16) . . ? C19 P02 C31 103.64(16) . . ? C25 P02 C31 103.87(17) . . ? C19 P02 Cu01 111.50(12) . . ? C25 P02 Cu01 118.33(14) . . ? C31 P02 Cu01 113.94(11) . . ? C01 P01 C07 102.59(17) . . ? C01 P01 C13 101.81(17) . . ? C07 P01 C13 105.72(17) . . ? C01 P01 Cu01 119.42(13) . . ? C07 P01 Cu01 114.37(12) . . ? C13 P01 Cu01 111.35(13) . . ? C42 S02 Cu01 111.58(13) . . ? C37 O01 H001 116(3) . . ? C32 C31 C36 118.2(4) . . ? C32 C31 P02 124.4(3) . . ? C36 C31 P02 117.3(3) . . ? C14 C13 C18 118.6(4) . . ? C14 C13 P01 124.9(3) . . ? C18 C13 P01 116.5(3) . . ? C03 C02 C01 120.3(5) . . ? C03 C02 H015 119.8 . . ? C01 C02 H015 119.8 . . ? O01 C37 C38 115.0(4) . . ? O01 C37 S01 125.4(3) . . ? C38 C37 S01 119.7(3) . . ? C08 C07 C12 118.7(3) . . ? C08 C07 P01 121.4(3) . . ? C12 C07 P01 119.6(3) . . ? C06 C01 C02 116.6(4) . . ? C06 C01 P01 123.9(3) . . ? C02 C01 P01 119.4(3) . . ? C25 C30 C29 120.8(5) . . ? C25 C30 H020 119.6 . . ? C29 C30 H020 119.6 . . ? C31 C32 C33 120.8(4) . . ? C31 C32 H021 119.6 . . ? C33 C32 H021 119.6 . . ? C13 C14 C15 121.0(5) . . ? C13 C14 H023 119.5 . . ? C15 C14 H023 119.5 . . ? C19 C20 C21 120.4(4) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? C18 C17 C16 120.5(5) . . ? C18 C17 H025 119.7 . . ? C16 C17 H025 119.7 . . ? C22 C21 C20 119.7(5) . . ? C22 C21 H026 120.2 . . ? C20 C21 H026 120.2 . . ? C03 C04 C05 120.1(5) . . ? C03 C04 H027 120.0 . . ? C05 C04 H027 120.0 . . ? C30 C25 C26 119.5(4) . . ? C30 C25 P02 118.7(3) . . ? C26 C25 P02 121.8(3) . . ? C23 C22 C21 120.6(4) . . ? C23 C22 H030 119.7 . . ? C21 C22 H030 119.7 . . ? C22 C23 C24 119.8(5) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C34 C33 C32 120.2(4) . . ? C34 C33 H032 119.9 . . ? C32 C33 H032 119.9 . . ? C12 C11 C10 120.5(4) . . ? C12 C11 H033 119.7 . . ? C10 C11 H033 119.7 . . ? C34 C35 C36 121.0(5) . . ? C34 C35 H034 119.5 . . ? C36 C35 H034 119.5 . . ? C11 C12 C07 120.0(4) . . ? C11 C12 H035 120.0 . . ? C07 C12 H035 120.0 . . ? C25 C26 C27 119.4(5) . . ? C25 C26 H26 120.3 . . ? C27 C26 H26 120.3 . . ? C05 C06 C01 123.1(5) . . ? C05 C06 H038 118.4 . . ? C01 C06 H038 118.4 . . ? C23 C24 C19 121.1(4) . . ? C23 C24 H24 119.5 . . ? C19 C24 H24 119.5 . . ? C35 C36 C31 120.1(4) . . ? C35 C36 H36 119.9 . . ? C31 C36 H36 119.9 . . ? C13 C18 C17 120.2(5) . . ? C13 C18 H041 119.9 . . ? C17 C18 H041 119.9 . . ? C28 C29 C30 118.4(6) . . ? C28 C29 H042 120.8 . . ? C30 C29 H042 120.8 . . ? C04 C03 C02 120.6(5) . . ? C04 C03 H043 119.7 . . ? C02 C03 H043 119.7 . . ? C07 C08 C09 121.2(4) . . ? C07 C08 H044 119.4 . . ? C09 C08 H044 119.4 . . ? C35 C34 C33 119.7(4) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C04 C05 C06 119.1(5) . . ? C04 C05 H046 120.4 . . ? C06 C05 H046 120.4 . . ? C20 C19 C24 118.5(3) . . ? C20 C19 P02 121.5(3) . . ? C24 C19 P02 119.8(3) . . ? C15 C16 C17 118.3(5) . . ? C15 C16 H048 120.9 . . ? C17 C16 H048 120.9 . . ? C16 C15 C14 121.3(5) . . ? C16 C15 H049 119.4 . . ? C14 C15 H049 119.4 . . ? C09 C10 C11 119.5(4) . . ? C09 C10 H050 120.3 . . ? C11 C10 H050 120.3 . . ? C10 C09 C08 120.1(4) . . ? C10 C09 H053 119.9 . . ? C08 C09 H053 119.9 . . ? C28 C27 C26 120.8(6) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C27 C28 C29 121.3(5) . . ? C27 C28 H055 119.4 . . ? C29 C28 H055 119.4 . . ? O02 C42 C43 116.5(4) . . ? O02 C42 S02 125.1(3) . . ? C43 C42 S02 118.4(3) . . ? _diffrn_measured_fraction_theta_max 0.867 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.889 _refine_diff_density_min -0.591 _refine_diff_density_rms 0.060 # Attachment '- cif-4b.cif' data_phencuta _database_code_depnum_ccdc_archive 'CCDC 808499' #TrackingRef '- cif-4b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H14 Cu N2 O5 S2' _exptl_crystal_recrystallization_method Methanol _chemical_melting_point ? _exptl_crystal_description Rectangular _exptl_crystal_colour Blue _diffrn_ambient_temperature 293(2) _chemical_formula_weight 514.04 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' 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 'P 21' _symmetry_int_tables_number 4 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.5195(10) _cell_length_b 13.8376(12) _cell_length_c 14.5830(12) _cell_angle_alpha 90.00 _cell_angle_beta 92.567(8) _cell_angle_gamma 90.00 _cell_volume 2120.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.610 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1044 _exptl_absorpt_coefficient_mu 1.265 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.76032 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10879 _diffrn_reflns_av_R_equivalents 0.0372 _diffrn_reflns_av_sigmaI/netI 0.0867 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 29.20 _reflns_number_total 8141 _reflns_number_gt 5115 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1981P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 8141 _refine_ls_number_parameters 527 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.1432 _refine_ls_R_factor_gt 0.1081 _refine_ls_wR_factor_ref 0.2986 _refine_ls_wR_factor_gt 0.2794 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.005 _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 S1 S 0.4437(6) 0.7738(5) 1.0287(4) 0.0539(11) Uani 0.602(5) 1 d PD A 1 C2 C 0.5675(10) 0.7731(10) 0.9551(8) 0.0539(11) Uani 0.602(5) 1 d PD A 1 C3 C 0.6892(19) 0.776(2) 1.0006(15) 0.0539(11) Uani 0.602(5) 1 d PD A 1 H3 H 0.7678 0.7771 0.9737 0.065 Uiso 0.602(5) 1 calc PR A 1 C4 C 0.667(2) 0.776(2) 1.0936(14) 0.0539(11) Uani 0.602(5) 1 d PD A 1 H4 H 0.7339 0.7760 1.1374 0.065 Uiso 0.602(5) 1 calc PR A 1 C5 C 0.545(2) 0.775(2) 1.1183(15) 0.0539(11) Uani 0.602(5) 1 d PD A 1 H5 H 0.5212 0.7750 1.1789 0.065 Uiso 0.602(5) 1 calc PR A 1 C3A C 0.497(3) 0.783(2) 1.0308(16) 0.0539(11) Uani 0.398(5) 1 d PD A 2 H3A H 0.4081 0.7856 1.0262 0.065 Uiso 0.398(5) 1 calc PR A 2 C2A C 0.5675(10) 0.7731(10) 0.9551(8) 0.0539(11) Uani 0.398(5) 1 d PD A 2 S1A S 0.7213(9) 0.7699(9) 0.9932(7) 0.0539(11) Uani 0.398(5) 1 d PD A 2 C5A C 0.691(3) 0.782(4) 1.1059(15) 0.0539(11) Uani 0.398(5) 1 d PD A 2 H5A H 0.7512 0.7839 1.1542 0.065 Uiso 0.398(5) 1 calc PR A 2 C4A C 0.563(3) 0.788(3) 1.114(2) 0.0539(11) Uani 0.398(5) 1 d PD A 2 H4A H 0.5241 0.7959 1.1695 0.065 Uiso 0.398(5) 1 calc PR A 2 S2 S 0.2678(7) 1.1482(4) 0.6967(4) 0.0541(11) Uani 0.602(5) 1 d PD A 3 C7 C 0.3756(12) 1.0959(9) 0.6338(8) 0.0541(11) Uani 0.602(5) 1 d PD A 3 C8 C 0.443(2) 1.1666(14) 0.5865(13) 0.0541(11) Uani 0.602(5) 1 d PD A 3 H8 H 0.5123 1.1564 0.5499 0.065 Uiso 0.602(5) 1 calc PR A 3 C9 C 0.386(2) 1.2557(15) 0.6055(14) 0.0541(11) Uani 0.602(5) 1 d PD A 3 H9 H 0.4192 1.3119 0.5810 0.065 Uiso 0.602(5) 1 calc PR A 3 C10 C 0.281(2) 1.2626(13) 0.6600(16) 0.0541(11) Uani 0.602(5) 1 d PD A 3 H10 H 0.2313 1.3162 0.6726 0.065 Uiso 0.602(5) 1 calc PR A 3 C8A C 0.301(3) 1.1631(19) 0.681(2) 0.0541(11) Uani 0.398(5) 1 d PD A 4 H8A H 0.2479 1.1463 0.7279 0.065 Uiso 0.398(5) 1 calc PR A 4 C7A C 0.3756(12) 1.0959(9) 0.6338(8) 0.0541(11) Uani 0.398(5) 1 d PD A 4 S2A S 0.4482(10) 1.1591(7) 0.5557(6) 0.0541(11) Uani 0.398(5) 1 d PD A 4 C10A C 0.397(3) 1.2699(16) 0.580(2) 0.0541(11) Uani 0.398(5) 1 d PD A 4 H10A H 0.4193 1.3277 0.5522 0.065 Uiso 0.398(5) 1 calc PR A 4 C9A C 0.315(3) 1.257(2) 0.649(2) 0.0541(11) Uani 0.398(5) 1 d PD A 4 H9A H 0.2702 1.3088 0.6727 0.065 Uiso 0.398(5) 1 calc PR A 4 S3 S 1.1698(6) 0.4764(6) 0.5099(5) 0.0544(10) Uani 0.602(5) 1 d PD A 5 C25 C 0.9156(18) 0.477(2) 0.4927(12) 0.0544(10) Uani 0.602(5) 1 d PD A 5 H25 H 0.8304 0.4765 0.5072 0.065 Uiso 0.602(5) 1 calc PR A 5 C24 C 1.0274(10) 0.4762(11) 0.5528(8) 0.0544(10) Uani 0.602(5) 1 d PD A 5 C27 C 1.1043(17) 0.478(2) 0.3989(12) 0.0544(10) Uani 0.602(5) 1 d PD A 5 H27 H 1.1498 0.4781 0.3457 0.065 Uiso 0.602(5) 1 calc PR A 5 C26 C 0.9711(18) 0.4790(18) 0.4025(13) 0.0544(10) Uani 0.602(5) 1 d PD A 5 H26 H 0.9196 0.4810 0.3490 0.065 Uiso 0.602(5) 1 calc PR A 5 C25A C 1.147(3) 0.475(3) 0.511(3) 0.0544(10) Uani 0.398(5) 1 d PD A 6 H25A H 1.2246 0.4715 0.5437 0.065 Uiso 0.398(5) 1 calc PR A 6 S3A S 0.9161(9) 0.4829(9) 0.4715(6) 0.0544(10) Uani 0.398(5) 1 d PD A 6 C24A C 1.0274(10) 0.4762(11) 0.5528(8) 0.0544(10) Uani 0.398(5) 1 d PD A 6 C26A C 1.137(3) 0.480(3) 0.415(2) 0.0544(10) Uani 0.398(5) 1 d PD A 6 H26A H 1.2065 0.4805 0.3785 0.065 Uiso 0.398(5) 1 calc PR A 6 C27A C 1.013(2) 0.484(3) 0.3808(17) 0.0544(10) Uani 0.398(5) 1 d PD A 6 H27A H 0.9863 0.4865 0.3191 0.065 Uiso 0.398(5) 1 calc PR A 6 S4 S 0.8936(9) 0.0489(5) 0.8734(6) 0.0735(15) Uani 0.602(5) 1 d PD A 7 C29 C 0.8234(14) 0.1492(9) 0.8364(10) 0.0735(15) Uani 0.602(5) 1 d PD A 7 C30 C 0.711(2) 0.1173(16) 0.788(2) 0.0735(15) Uani 0.602(5) 1 d PD A 7 H30 H 0.6530 0.1592 0.7587 0.088 Uiso 0.602(5) 1 calc PR A 7 C31 C 0.694(3) 0.0137(16) 0.789(2) 0.0735(15) Uani 0.602(5) 1 d PD A 7 H31 H 0.6230 -0.0161 0.7611 0.088 Uiso 0.602(5) 1 calc PR A 7 C32 C 0.791(2) -0.0396(14) 0.8368(18) 0.0735(15) Uani 0.602(5) 1 d PD A 7 H32 H 0.7976 -0.1060 0.8455 0.088 Uiso 0.602(5) 1 calc PR A 7 C30A C 0.902(3) 0.081(2) 0.885(2) 0.0735(15) Uani 0.398(5) 1 d PD A 8 H30A H 0.9744 0.0925 0.9223 0.088 Uiso 0.398(5) 1 calc PR A 8 C29A C 0.8234(14) 0.1492(9) 0.8364(10) 0.0735(15) Uani 0.398(5) 1 d PD A 8 S4A S 0.6999(13) 0.1053(9) 0.7780(11) 0.0735(15) Uani 0.398(5) 1 d PD A 8 C32A C 0.732(4) -0.0114(17) 0.806(3) 0.0735(15) Uani 0.398(5) 1 d PD A 8 H32A H 0.6868 -0.0662 0.7874 0.088 Uiso 0.398(5) 1 calc PR A 8 C31A C 0.841(4) -0.007(3) 0.864(3) 0.0735(15) Uani 0.398(5) 1 d PD A 8 H31A H 0.8751 -0.0640 0.8895 0.088 Uiso 0.398(5) 1 calc PR A 8 C28 C 0.8518(17) 0.2477(12) 0.8406(11) 0.063(4) Uani 1 1 d . . . Cu1 Cu 0.33877(13) 0.78509(10) 0.70855(9) 0.0400(4) Uani 1 1 d . . . Cu2 Cu 0.82862(14) 0.46248(10) 0.79916(9) 0.0405(4) Uani 1 1 d . . . O1 O 0.4204(8) 0.7798(7) 0.8319(6) 0.051(2) Uani 1 1 d . A . N4 N 0.6526(10) 0.4997(7) 0.7465(8) 0.046(3) Uani 1 1 d . A . O6 O 0.8933(7) 0.4707(7) 0.6755(5) 0.0450(19) Uani 1 1 d . A . O5 O 0.5003(8) 0.7793(8) 0.6434(6) 0.054(2) Uani 1 1 d . . . O3 O 0.3309(8) 0.9428(7) 0.6967(6) 0.048(2) Uani 1 1 d . A . O8 O 0.7841(9) 0.3084(6) 0.8003(6) 0.046(2) Uani 1 1 d . A . C14 C 0.0200(13) 0.7261(9) 0.5356(9) 0.043(3) Uani 1 1 d . . . O7 O 1.1010(9) 0.4723(11) 0.7043(7) 0.079(3) Uani 1 1 d . A . O10 O 0.9962(8) 0.4487(8) 0.8594(6) 0.058(3) Uani 1 1 d . A . O2 O 0.6215(8) 0.7575(8) 0.8035(6) 0.057(3) Uani 1 1 d . A . N3 N 0.7499(9) 0.4919(7) 0.9182(7) 0.041(2) Uani 1 1 d . A . O4 O 0.4696(13) 0.9560(10) 0.5873(8) 0.083(3) Uani 1 1 d . A . N1 N 0.2362(9) 0.7605(7) 0.5933(6) 0.038(2) Uani 1 1 d . . . C21 C 0.0718(10) 0.7370(9) 0.7006(7) 0.033(2) Uani 1 1 d . . . N2 N 0.1683(9) 0.7554(8) 0.7643(7) 0.044(2) Uani 1 1 d U . . C38 C 0.3632(13) 0.5402(9) 0.8719(11) 0.052(4) Uani 1 1 d . A . H38 H 0.2766 0.5500 0.8601 0.063 Uiso 1 1 calc R . . C39 C 0.4433(13) 0.5291(10) 0.7969(12) 0.057(4) Uani 1 1 d . A . C23 C 1.0067(10) 0.4725(10) 0.6558(7) 0.036(2) Uani 1 1 d . . . C17 C -0.0502(12) 0.7187(8) 0.7183(9) 0.039(3) Uani 1 1 d . . . C44 C 0.6282(12) 0.5078(8) 0.9091(9) 0.043(3) Uani 1 1 d . . . C15 C -0.1109(14) 0.7087(9) 0.5573(11) 0.055(4) Uani 1 1 d . . . H15 H -0.1734 0.6999 0.5109 0.066 Uiso 1 1 calc R . . C36 C 0.5433(12) 0.5226(7) 0.9800(9) 0.040(3) Uani 1 1 d . A . C1 C 0.5366(10) 0.7717(9) 0.8541(7) 0.035(2) Uani 1 1 d . . . C35 C 0.5983(16) 0.5168(11) 1.0705(10) 0.061(4) Uani 1 1 d . . . H35 H 0.5497 0.5252 1.1216 0.073 Uiso 1 1 calc R A . C16 C -0.1405(11) 0.7054(9) 0.6465(10) 0.049(3) Uani 1 1 d . . . H16 H -0.2245 0.6937 0.6605 0.059 Uiso 1 1 calc R . . C43 C 0.5720(9) 0.5102(8) 0.8131(10) 0.040(3) Uani 1 1 d . A . C22 C 0.1094(11) 0.7451(9) 0.6041(8) 0.037(3) Uani 1 1 d . . . C37 C 0.4096(16) 0.5367(10) 0.9615(11) 0.064(5) Uani 1 1 d . . . H37 H 0.3549 0.5435 1.0095 0.077 Uiso 1 1 calc R A . C13 C 0.0572(14) 0.7363(9) 0.4422(9) 0.048(3) Uani 1 1 d . . . H13 H -0.0010 0.7322 0.3925 0.058 Uiso 1 1 calc R . . C12 C 0.1805(15) 0.7519(10) 0.4319(8) 0.050(3) Uani 1 1 d . . . H12 H 0.2107 0.7521 0.3729 0.060 Uiso 1 1 calc R . . C33 C 0.7921(15) 0.4868(10) 1.0020(9) 0.052(3) Uani 1 1 d . . . H33 H 0.8783 0.4736 1.0116 0.063 Uiso 1 1 calc R A . C34 C 0.7233(17) 0.4987(12) 1.0791(9) 0.064(4) Uani 1 1 d . A . H34 H 0.7635 0.4943 1.1370 0.076 Uiso 1 1 calc R . . C19 C 0.0195(12) 0.7264(11) 0.8780(11) 0.054(4) Uani 1 1 d . . . H19 H 0.0036 0.7217 0.9401 0.065 Uiso 1 1 calc R . . C20 C 0.1407(12) 0.7453(10) 0.8505(9) 0.044(2) Uani 1 1 d . . . H20 H 0.2060 0.7512 0.8952 0.053 Uiso 1 1 calc R . . C11 C 0.2663(14) 0.7681(10) 0.5060(9) 0.053(3) Uani 1 1 d . . . H11 H 0.3494 0.7851 0.4936 0.064 Uiso 1 1 calc R . . C6 C 0.3902(17) 0.9906(10) 0.6400(11) 0.061(4) Uani 1 1 d . . . C18 C -0.0708(13) 0.7155(10) 0.8171(11) 0.054(4) Uani 1 1 d . . . H18 H -0.1528 0.7051 0.8362 0.064 Uiso 1 1 calc R . . C42 C 0.6158(12) 0.4995(8) 0.6604(9) 0.041(3) Uani 1 1 d . . . H42 H 0.6739 0.4892 0.6152 0.049 Uiso 1 1 calc R A . O9 O 0.9525(14) 0.2676(11) 0.8872(10) 0.101(5) Uani 1 1 d . A . C40 C 0.4054(11) 0.5298(11) 0.7075(12) 0.059(4) Uani 1 1 d . . . H40 H 0.3196 0.5406 0.6929 0.071 Uiso 1 1 calc R A . C41 C 0.4846(13) 0.5154(12) 0.6363(10) 0.056(4) Uani 1 1 d . A . H41 H 0.4541 0.5161 0.5754 0.068 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.060(3) 0.060(2) 0.0411(18) 0.0063(19) -0.0034(19) -0.001(2) C2 0.060(3) 0.060(2) 0.0411(18) 0.0063(19) -0.0034(19) -0.001(2) C3 0.060(3) 0.060(2) 0.0411(18) 0.0063(19) -0.0034(19) -0.001(2) C4 0.060(3) 0.060(2) 0.0411(18) 0.0063(19) -0.0034(19) -0.001(2) C5 0.060(3) 0.060(2) 0.0411(18) 0.0063(19) -0.0034(19) -0.001(2) C3A 0.060(3) 0.060(2) 0.0411(18) 0.0063(19) -0.0034(19) -0.001(2) C2A 0.060(3) 0.060(2) 0.0411(18) 0.0063(19) -0.0034(19) -0.001(2) S1A 0.060(3) 0.060(2) 0.0411(18) 0.0063(19) -0.0034(19) -0.001(2) C5A 0.060(3) 0.060(2) 0.0411(18) 0.0063(19) -0.0034(19) -0.001(2) C4A 0.060(3) 0.060(2) 0.0411(18) 0.0063(19) -0.0034(19) -0.001(2) S2 0.060(3) 0.052(2) 0.050(3) 0.006(2) 0.008(2) -0.0096(19) C7 0.060(3) 0.052(2) 0.050(3) 0.006(2) 0.008(2) -0.0096(19) C8 0.060(3) 0.052(2) 0.050(3) 0.006(2) 0.008(2) -0.0096(19) C9 0.060(3) 0.052(2) 0.050(3) 0.006(2) 0.008(2) -0.0096(19) C10 0.060(3) 0.052(2) 0.050(3) 0.006(2) 0.008(2) -0.0096(19) C8A 0.060(3) 0.052(2) 0.050(3) 0.006(2) 0.008(2) -0.0096(19) C7A 0.060(3) 0.052(2) 0.050(3) 0.006(2) 0.008(2) -0.0096(19) S2A 0.060(3) 0.052(2) 0.050(3) 0.006(2) 0.008(2) -0.0096(19) C10A 0.060(3) 0.052(2) 0.050(3) 0.006(2) 0.008(2) -0.0096(19) C9A 0.060(3) 0.052(2) 0.050(3) 0.006(2) 0.008(2) -0.0096(19) S3 0.053(2) 0.065(2) 0.045(2) 0.005(2) 0.0128(17) 0.0014(19) C25 0.053(2) 0.065(2) 0.045(2) 0.005(2) 0.0128(17) 0.0014(19) C24 0.053(2) 0.065(2) 0.045(2) 0.005(2) 0.0128(17) 0.0014(19) C27 0.053(2) 0.065(2) 0.045(2) 0.005(2) 0.0128(17) 0.0014(19) C26 0.053(2) 0.065(2) 0.045(2) 0.005(2) 0.0128(17) 0.0014(19) C25A 0.053(2) 0.065(2) 0.045(2) 0.005(2) 0.0128(17) 0.0014(19) S3A 0.053(2) 0.065(2) 0.045(2) 0.005(2) 0.0128(17) 0.0014(19) C24A 0.053(2) 0.065(2) 0.045(2) 0.005(2) 0.0128(17) 0.0014(19) C26A 0.053(2) 0.065(2) 0.045(2) 0.005(2) 0.0128(17) 0.0014(19) C27A 0.053(2) 0.065(2) 0.045(2) 0.005(2) 0.0128(17) 0.0014(19) S4 0.098(4) 0.048(3) 0.075(3) 0.000(3) 0.011(3) -0.002(3) C29 0.098(4) 0.048(3) 0.075(3) 0.000(3) 0.011(3) -0.002(3) C30 0.098(4) 0.048(3) 0.075(3) 0.000(3) 0.011(3) -0.002(3) C31 0.098(4) 0.048(3) 0.075(3) 0.000(3) 0.011(3) -0.002(3) C32 0.098(4) 0.048(3) 0.075(3) 0.000(3) 0.011(3) -0.002(3) C30A 0.098(4) 0.048(3) 0.075(3) 0.000(3) 0.011(3) -0.002(3) C29A 0.098(4) 0.048(3) 0.075(3) 0.000(3) 0.011(3) -0.002(3) S4A 0.098(4) 0.048(3) 0.075(3) 0.000(3) 0.011(3) -0.002(3) C32A 0.098(4) 0.048(3) 0.075(3) 0.000(3) 0.011(3) -0.002(3) C31A 0.098(4) 0.048(3) 0.075(3) 0.000(3) 0.011(3) -0.002(3) C28 0.069(11) 0.060(9) 0.058(9) 0.013(8) -0.003(8) 0.021(8) Cu1 0.0386(8) 0.0463(8) 0.0349(7) 0.0005(7) -0.0009(5) 0.0020(7) Cu2 0.0376(8) 0.0499(8) 0.0342(7) -0.0023(7) 0.0029(5) -0.0009(7) O1 0.050(5) 0.058(5) 0.045(5) 0.013(5) -0.004(4) -0.003(5) N4 0.043(6) 0.037(6) 0.061(7) 0.004(5) 0.028(5) 0.001(4) O6 0.028(4) 0.067(5) 0.041(4) 0.004(5) 0.009(3) 0.012(4) O5 0.051(5) 0.071(6) 0.041(4) -0.011(5) 0.015(4) -0.014(5) O3 0.048(5) 0.049(6) 0.049(5) 0.004(4) 0.011(4) 0.003(4) O8 0.052(5) 0.040(5) 0.048(5) -0.004(4) 0.006(4) 0.000(4) C14 0.049(8) 0.032(6) 0.049(7) 0.001(5) 0.000(6) 0.016(5) O7 0.036(5) 0.144(11) 0.056(6) 0.000(7) 0.007(4) 0.011(7) O10 0.030(4) 0.090(8) 0.056(5) -0.016(5) 0.010(4) -0.016(5) O2 0.026(4) 0.098(8) 0.046(5) 0.003(5) -0.005(4) 0.008(4) N3 0.036(5) 0.050(6) 0.038(5) -0.007(5) 0.007(4) 0.010(4) O4 0.103(10) 0.078(8) 0.069(7) 0.011(7) 0.018(7) 0.001(7) N1 0.041(5) 0.046(6) 0.028(4) 0.001(4) 0.004(4) 0.002(4) C21 0.022(5) 0.049(6) 0.026(5) 0.012(5) -0.007(4) -0.008(5) N2 0.028(4) 0.056(5) 0.047(4) -0.013(4) -0.007(3) 0.013(3) C38 0.041(8) 0.038(7) 0.079(11) -0.008(7) 0.016(7) 0.006(5) C39 0.034(7) 0.049(8) 0.088(11) -0.016(8) 0.004(7) -0.009(6) C23 0.019(5) 0.049(6) 0.040(5) -0.003(5) 0.002(4) -0.016(5) C17 0.037(7) 0.026(6) 0.055(7) 0.001(5) 0.011(6) -0.004(5) C44 0.040(7) 0.028(6) 0.062(8) -0.002(6) 0.022(6) -0.001(5) C15 0.061(9) 0.039(7) 0.063(9) -0.004(6) -0.019(7) 0.011(6) C36 0.051(7) 0.019(5) 0.054(7) -0.014(5) 0.039(6) -0.003(5) C1 0.022(5) 0.042(6) 0.040(6) -0.001(5) -0.001(4) 0.002(5) C35 0.072(11) 0.059(8) 0.054(9) -0.010(7) 0.043(8) 0.001(7) C16 0.021(6) 0.050(7) 0.078(10) -0.005(7) 0.001(6) 0.000(5) C43 0.009(5) 0.035(6) 0.077(9) -0.004(6) -0.001(5) -0.002(4) C22 0.027(6) 0.049(6) 0.034(6) 0.004(5) -0.010(4) 0.006(5) C37 0.079(12) 0.049(8) 0.070(10) -0.020(7) 0.053(9) 0.005(7) C13 0.063(9) 0.047(7) 0.033(6) 0.000(6) -0.010(6) 0.009(6) C12 0.071(10) 0.058(8) 0.020(5) -0.008(5) 0.004(5) 0.013(7) C33 0.066(9) 0.050(8) 0.040(7) -0.013(6) -0.003(6) 0.005(6) C34 0.078(11) 0.084(11) 0.030(6) -0.009(7) 0.017(6) 0.001(9) C19 0.028(7) 0.065(9) 0.069(9) 0.006(7) -0.001(6) -0.010(6) C20 0.028(4) 0.056(5) 0.047(4) -0.013(4) -0.007(3) 0.013(3) C11 0.056(8) 0.051(8) 0.053(8) -0.011(7) 0.010(6) 0.018(6) C6 0.085(12) 0.043(8) 0.053(8) 0.000(7) -0.028(8) 0.005(7) C18 0.036(7) 0.051(8) 0.075(10) 0.010(7) 0.023(7) 0.013(6) C42 0.036(7) 0.037(6) 0.052(7) -0.005(6) 0.014(5) 0.007(5) O9 0.104(10) 0.104(11) 0.093(9) 0.053(9) -0.018(8) 0.001(8) C40 0.005(5) 0.067(9) 0.104(13) -0.025(9) -0.002(6) -0.003(5) C41 0.039(8) 0.078(10) 0.050(8) 0.003(7) -0.019(6) -0.008(7) _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 S1 C5 1.650(17) . ? S1 C2 1.725(12) . ? C2 C3 1.416(18) . ? C2 C1 1.493(15) . ? C3 C4 1.387(18) . ? C3 H3 0.9300 . ? C4 C5 1.345(18) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C3A C4A 1.371(19) . ? C3A H3A 0.9300 . ? S1A C5A 1.697(18) . ? C5A C4A 1.359(19) . ? C5A H5A 0.9300 . ? C4A H4A 0.9300 . ? S2 C7 1.657(13) . ? S2 C10 1.678(16) . ? C7 C8 1.408(17) . ? C7 C6 1.469(19) . ? C8 C9 1.406(17) . ? C8 H8 0.9300 . ? C9 C10 1.392(17) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C8A C9A 1.396(19) . ? C8A H8A 0.9300 . ? S2A C10A 1.668(19) . ? C10A C9A 1.366(19) . ? C10A H10A 0.9300 . ? C9A H9A 0.9300 . ? S3 C24 1.649(12) . ? S3 C27 1.730(16) . ? C25 C24 1.435(18) . ? C25 C26 1.463(16) . ? C25 H25 0.9300 . ? C24 C23 1.529(15) . ? C27 C26 1.405(17) . ? C27 H27 0.9300 . ? C26 H26 0.9300 . ? C25A C26A 1.39(2) . ? C25A H25A 0.9300 . ? S3A C27A 1.703(18) . ? C26A C27A 1.378(19) . ? C26A H26A 0.9300 . ? C27A H27A 0.9300 . ? S4 C29 1.652(14) . ? S4 C32 1.701(17) . ? C29 C28 1.40(2) . ? C29 C30 1.421(19) . ? C30 C31 1.444(18) . ? C30 H30 0.9300 . ? C31 C32 1.419(18) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C30A C31A 1.41(2) . ? C30A H30A 0.9300 . ? S4A C32A 1.697(19) . ? C32A C31A 1.40(2) . ? C32A H32A 0.9300 . ? C31A H31A 0.9300 . ? C28 O8 1.233(17) . ? C28 O9 1.26(2) . ? Cu1 O1 1.960(8) . ? Cu1 N1 1.986(10) . ? Cu1 O5 1.986(8) . ? Cu1 N2 2.044(11) . ? Cu1 O3 2.191(9) . ? Cu2 O10 1.944(9) . ? Cu2 O6 1.959(7) . ? Cu2 N3 1.998(9) . ? Cu2 N4 2.039(11) . ? Cu2 O8 2.183(8) . ? O1 C1 1.255(13) . ? N4 C42 1.297(17) . ? N4 C43 1.325(15) . ? O6 C23 1.239(12) . ? O3 C6 1.246(19) . ? C14 C22 1.366(17) . ? C14 C13 1.441(18) . ? C14 C15 1.45(2) . ? O7 C23 1.192(14) . ? O2 C1 1.200(14) . ? N3 C33 1.283(17) . ? N3 C44 1.301(16) . ? O4 C6 1.26(2) . ? N1 C11 1.330(16) . ? N1 C22 1.367(15) . ? C21 C17 1.344(15) . ? C21 N2 1.369(14) . ? C21 C22 1.484(15) . ? N2 C20 1.309(17) . ? C38 C37 1.38(2) . ? C38 C39 1.42(2) . ? C38 H38 0.9300 . ? C39 C40 1.35(2) . ? C39 C43 1.389(17) . ? C17 C16 1.394(19) . ? C17 C18 1.466(19) . ? C44 C36 1.410(15) . ? C44 C43 1.50(2) . ? C15 C16 1.35(2) . ? C15 H15 0.9300 . ? C36 C35 1.42(2) . ? C36 C37 1.43(2) . ? C35 C34 1.34(2) . ? C35 H35 0.9300 . ? C16 H16 0.9300 . ? C37 H37 0.9300 . ? C13 C12 1.33(2) . ? C13 H13 0.9300 . ? C12 C11 1.39(2) . ? C12 H12 0.9300 . ? C33 C34 1.374(18) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C19 C18 1.28(2) . ? C19 C20 1.379(18) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C11 H11 0.9300 . ? C18 H18 0.9300 . ? C42 C41 1.426(18) . ? C42 H42 0.9300 . ? C40 C41 1.37(2) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? 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 C5 S1 C2 90.8(10) . . ? C3 C2 C1 127.9(13) . . ? C3 C2 S1 113.6(12) . . ? C1 C2 S1 118.5(8) . . ? C4 C3 C2 105.6(17) . . ? C4 C3 H3 127.2 . . ? C2 C3 H3 127.2 . . ? C5 C4 C3 118(2) . . ? C5 C4 H4 121.1 . . ? C3 C4 H4 121.1 . . ? C4 C5 S1 112.2(18) . . ? C4 C5 H5 123.9 . . ? S1 C5 H5 123.9 . . ? C4A C3A H3A 121.8 . . ? C4A C5A S1A 109(2) . . ? C4A C5A H5A 125.6 . . ? S1A C5A H5A 125.6 . . ? C5A C4A C3A 113(3) . . ? C5A C4A H4A 123.6 . . ? C3A C4A H4A 123.6 . . ? C7 S2 C10 99.6(8) . . ? C8 C7 C6 131.8(14) . . ? C8 C7 S2 110.0(12) . . ? C6 C7 S2 118.1(10) . . ? C9 C8 C7 106.3(15) . . ? C9 C8 H8 126.9 . . ? C7 C8 H8 126.9 . . ? C10 C9 C8 122.1(16) . . ? C10 C9 H9 119.0 . . ? C8 C9 H9 119.0 . . ? C9 C10 S2 101.3(12) . . ? C9 C10 H10 129.3 . . ? S2 C10 H10 129.3 . . ? C9A C8A H8A 123.9 . . ? C9A C10A S2A 105(2) . . ? C9A C10A H10A 127.5 . . ? S2A C10A H10A 127.5 . . ? C10A C9A C8A 117(3) . . ? C10A C9A H9A 121.7 . . ? C8A C9A H9A 121.7 . . ? C24 S3 C27 91.4(9) . . ? C24 C25 C26 101.6(14) . . ? C24 C25 H25 129.2 . . ? C26 C25 H25 129.2 . . ? C25 C24 C23 116.9(11) . . ? C25 C24 S3 120.1(11) . . ? C23 C24 S3 123.0(8) . . ? C26 C27 S3 108.7(13) . . ? C26 C27 H27 125.6 . . ? S3 C27 H27 125.6 . . ? C27 C26 C25 118.2(16) . . ? C27 C26 H26 120.9 . . ? C25 C26 H26 120.9 . . ? C26A C25A H25A 123.3 . . ? C27A C26A C25A 113(3) . . ? C27A C26A H26A 123.3 . . ? C25A C26A H26A 123.3 . . ? C26A C27A S3A 108(2) . . ? C26A C27A H27A 126.2 . . ? S3A C27A H27A 126.2 . . ? C29 S4 C32 103.6(10) . . ? C28 C29 C30 119.9(15) . . ? C28 C29 S4 135.5(12) . . ? C30 C29 S4 104.6(13) . . ? C29 C30 C31 113.8(17) . . ? C29 C30 H30 123.1 . . ? C31 C30 H30 123.1 . . ? C32 C31 C30 115.8(18) . . ? C32 C31 H31 122.1 . . ? C30 C31 H31 122.1 . . ? C31 C32 S4 102.3(14) . . ? C31 C32 H32 128.9 . . ? S4 C32 H32 128.9 . . ? C31A C30A H30A 128.6 . . ? C31A C32A S4A 105(3) . . ? C31A C32A H32A 127.5 . . ? S4A C32A H32A 127.5 . . ? C32A C31A C30A 121(4) . . ? C32A C31A H31A 119.4 . . ? C30A C31A H31A 119.4 . . ? O8 C28 O9 124.1(16) . . ? O8 C28 C29 121.7(16) . . ? O9 C28 C29 114.2(14) . . ? O1 Cu1 N1 165.9(4) . . ? O1 Cu1 O5 95.1(4) . . ? N1 Cu1 O5 91.8(4) . . ? O1 Cu1 N2 89.1(4) . . ? N1 Cu1 N2 81.3(4) . . ? O5 Cu1 N2 165.3(4) . . ? O1 Cu1 O3 97.1(4) . . ? N1 Cu1 O3 95.0(4) . . ? O5 Cu1 O3 91.9(4) . . ? N2 Cu1 O3 101.6(4) . . ? O10 Cu2 O6 94.4(3) . . ? O10 Cu2 N3 91.7(4) . . ? O6 Cu2 N3 164.2(4) . . ? O10 Cu2 N4 170.2(4) . . ? O6 Cu2 N4 89.2(4) . . ? N3 Cu2 N4 82.6(4) . . ? O10 Cu2 O8 95.2(4) . . ? O6 Cu2 O8 98.5(4) . . ? N3 Cu2 O8 95.4(4) . . ? N4 Cu2 O8 93.3(4) . . ? C1 O1 Cu1 128.4(8) . . ? C42 N4 C43 122.4(11) . . ? C42 N4 Cu2 126.2(8) . . ? C43 N4 Cu2 110.6(9) . . ? C23 O6 Cu2 126.3(7) . . ? C6 O3 Cu1 124.2(9) . . ? C28 O8 Cu2 123.3(11) . . ? C22 C14 C13 117.7(13) . . ? C22 C14 C15 120.2(12) . . ? C13 C14 C15 121.7(12) . . ? C33 N3 C44 113.7(12) . . ? C33 N3 Cu2 132.7(9) . . ? C44 N3 Cu2 113.0(9) . . ? C11 N1 C22 113.5(11) . . ? C11 N1 Cu1 130.8(9) . . ? C22 N1 Cu1 115.2(7) . . ? C17 C21 N2 126.1(11) . . ? C17 C21 C22 119.6(10) . . ? N2 C21 C22 114.1(10) . . ? C20 N2 C21 116.2(11) . . ? C20 N2 Cu1 129.7(8) . . ? C21 N2 Cu1 113.9(8) . . ? C37 C38 C39 122.1(14) . . ? C37 C38 H38 118.9 . . ? C39 C38 H38 118.9 . . ? C40 C39 C43 114.3(13) . . ? C40 C39 C38 125.9(14) . . ? C43 C39 C38 119.8(15) . . ? O7 C23 O6 130.3(11) . . ? O7 C23 C24 115.5(10) . . ? O6 C23 C24 114.2(9) . . ? C21 C17 C16 120.3(12) . . ? C21 C17 C18 112.2(11) . . ? C16 C17 C18 127.5(12) . . ? N3 C44 C36 127.1(13) . . ? N3 C44 C43 116.4(10) . . ? C36 C44 C43 116.5(12) . . ? C16 C15 C14 118.6(12) . . ? C16 C15 H15 120.7 . . ? C14 C15 H15 120.7 . . ? C44 C36 C35 115.4(12) . . ? C44 C36 C37 122.0(13) . . ? C35 C36 C37 122.5(11) . . ? O2 C1 O1 126.8(11) . . ? O2 C1 C2 118.2(10) . . ? O1 C1 C2 114.8(10) . . ? C34 C35 C36 117.0(11) . . ? C34 C35 H35 121.5 . . ? C36 C35 H35 121.5 . . ? C15 C16 C17 122.7(12) . . ? C15 C16 H16 118.6 . . ? C17 C16 H16 118.6 . . ? N4 C43 C39 123.1(14) . . ? N4 C43 C44 116.4(10) . . ? C39 C43 C44 120.3(12) . . ? N1 C22 C14 126.1(12) . . ? N1 C22 C21 115.1(9) . . ? C14 C22 C21 118.3(11) . . ? C38 C37 C36 119.1(11) . . ? C38 C37 H37 120.5 . . ? C36 C37 H37 120.5 . . ? C12 C13 C14 115.5(12) . . ? C12 C13 H13 122.3 . . ? C14 C13 H13 122.3 . . ? C13 C12 C11 122.7(12) . . ? C13 C12 H12 118.7 . . ? C11 C12 H12 118.7 . . ? N3 C33 C34 126.9(15) . . ? N3 C33 H33 116.5 . . ? C34 C33 H33 116.5 . . ? C35 C34 C33 119.8(15) . . ? C35 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? C18 C19 C20 119.1(15) . . ? C18 C19 H19 120.4 . . ? C20 C19 H19 120.4 . . ? N2 C20 C19 123.2(12) . . ? N2 C20 H20 118.4 . . ? C19 C20 H20 118.4 . . ? N1 C11 C12 123.7(13) . . ? N1 C11 H11 118.1 . . ? C12 C11 H11 118.1 . . ? O3 C6 O4 124.8(13) . . ? O3 C6 C7 120.9(15) . . ? O4 C6 C7 114.2(15) . . ? C19 C18 C17 122.7(13) . . ? C19 C18 H18 118.6 . . ? C17 C18 H18 118.6 . . ? N4 C42 C41 118.8(11) . . ? N4 C42 H42 120.6 . . ? C41 C42 H42 120.6 . . ? C39 C40 C41 124.5(12) . . ? C39 C40 H40 117.7 . . ? C41 C40 H40 117.7 . . ? C40 C41 C42 116.7(13) . . ? C40 C41 H41 121.7 . . ? C42 C41 H41 121.7 . . ? _diffrn_measured_fraction_theta_max 0.850 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.861 _refine_diff_density_min -0.965 _refine_diff_density_rms 0.182