# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Safin, Damir' _publ_contact_author_email damir.safin@ksu.ru _publ_section_title ; Versatile structures and photophysical properties of poly- and mononuclear CuI complexes with N-thiophosphorylated thioureas RNHC(S)NHP(S)(OiPr)2 and phosphines ; _publ_author_name D.Safin # Attachment '- 2.cif' data_safin53 _database_code_depnum_ccdc_archive 'CCDC 749077' #TrackingRef '- 2.cif' # start Validation Reply Form _vrf_PLAT220_safin53 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.53 Ratio RESPONSE: One of the atoms of an isopropyl group shows increased thermal motion but no model for a disordered refinement could be found. ; _vrf_PLAT222_safin53 ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 5.22 Ratio RESPONSE: One of the atoms of an isopropyl group shows increased thermal motion but no model for a disordered refinement could be found. ; _vrf_PLAT723_safin53 ; PROBLEM: Torsion Calc 179.2(3), Rep 18.00 Dev... 161.20 Sigma RESPONSE: This must be a PLATON bug. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H66 Cu3 N6 O6 P3 S6' _chemical_formula_sum 'C42 H66 Cu3 N6 O6 P3 S6' _chemical_formula_weight 1226.90 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' Cu Cu 0.3201 1.2651 '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' 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' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M R-3 _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 17.7250(5) _cell_length_b 17.7250(5) _cell_length_c 63.211(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 17198.7(11) _cell_formula_units_Z 12 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 20659 _cell_measurement_theta_min 2.7 _cell_measurement_theta_max 26.4 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.41 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.421 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7632 _exptl_absorpt_coefficient_mu 1.451 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5612 _exptl_absorpt_correction_T_max 0.5876 _exptl_absorpt_process_details 'MULABS (Spek, 2003; Blessing, 1995)' _exptl_special_details ; ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS II two-circle-diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 38559 _diffrn_reflns_av_R_equivalents 0.0563 _diffrn_reflns_av_sigmaI/netI 0.0480 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -77 _diffrn_reflns_limit_l_max 64 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 26.01 _reflns_number_total 7491 _reflns_number_gt 4716 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'X-Area (Stoe & Cie, 2001)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2001)' _computing_data_reduction 'X-Area (Stoe & Cie, 2001)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008) ' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008) ' _computing_molecular_graphics 'XP in SHELXTL-Plus (Sheldrick, 1991)' _computing_publication_material SHELXL97 _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^)+(0.0497P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7491 _refine_ls_number_parameters 407 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0653 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.0879 _refine_ls_wR_factor_gt 0.0808 _refine_ls_goodness_of_fit_ref 0.856 _refine_ls_restrained_S_all 0.856 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.97566(2) 0.86442(2) 0.368282(6) 0.02603(10) Uani 1 1 d . . . P1 P 0.81011(5) 0.68403(5) 0.368223(12) 0.02158(16) Uani 1 1 d . . . S1 S 0.93033(5) 0.72941(5) 0.379693(13) 0.02967(18) Uani 1 1 d . . . S2 S 0.86963(5) 0.89393(4) 0.361420(12) 0.02656(16) Uani 1 1 d . . . N1 N 0.75647(15) 0.73010(14) 0.37591(4) 0.0247(5) Uani 1 1 d . . . N2 N 0.71950(15) 0.83549(16) 0.38102(4) 0.0294(6) Uani 1 1 d . . . H2 H 0.732(2) 0.888(2) 0.3775(6) 0.042(10) Uiso 1 1 d . . . O1 O 0.80586(13) 0.68102(13) 0.34354(3) 0.0295(5) Uani 1 1 d . . . O2 O 0.75269(12) 0.58519(12) 0.37453(3) 0.0244(4) Uani 1 1 d . . . C1 C 0.77605(18) 0.81097(18) 0.37370(5) 0.0234(6) Uani 1 1 d . . . C2 C 0.8493(2) 0.6435(2) 0.33096(5) 0.0370(7) Uani 1 1 d . . . H2B H 0.8822 0.6258 0.3407 0.044 Uiso 1 1 calc R . . C3 C 0.9114(3) 0.7125(3) 0.31644(8) 0.0751(14) Uani 1 1 d . . . H3A H 0.9553 0.7616 0.3247 0.113 Uiso 1 1 calc R . . H3B H 0.8798 0.7324 0.3074 0.113 Uiso 1 1 calc R . . H3C H 0.9402 0.6890 0.3076 0.113 Uiso 1 1 calc R . . C4 C 0.7784(3) 0.5639(3) 0.32016(7) 0.0600(11) Uani 1 1 d . . . H4A H 0.7405 0.5219 0.3308 0.084 Uiso 1 1 calc R . . H4B H 0.8045 0.5374 0.3114 0.084 Uiso 1 1 calc R . . H4C H 0.7440 0.5806 0.3112 0.084 Uiso 1 1 calc R . . C5 C 0.73883(19) 0.55888(19) 0.39687(5) 0.0289(7) Uani 1 1 d . . . H5 H 0.7727 0.6114 0.4060 0.035 Uiso 1 1 calc R . . C6 C 0.64237(19) 0.5193(2) 0.40154(5) 0.0350(7) Uani 1 1 d . . . H6A H 0.6251 0.5633 0.3994 0.053 Uiso 1 1 calc R . . H6B H 0.6309 0.4990 0.4162 0.053 Uiso 1 1 calc R . . H6C H 0.6089 0.4699 0.3920 0.053 Uiso 1 1 calc R . . C7 C 0.7721(2) 0.4964(2) 0.40015(7) 0.0512(10) Uani 1 1 d . . . H7A H 0.8345 0.5258 0.3969 0.077 Uiso 1 1 calc R . . H7B H 0.7408 0.4461 0.3907 0.077 Uiso 1 1 calc R . . H7C H 0.7626 0.4766 0.4149 0.077 Uiso 1 1 calc R . . C11 C 0.63249(18) 0.77662(18) 0.38791(5) 0.0304(7) Uani 1 1 d . . . C12 C 0.5645(2) 0.7754(2) 0.37705(6) 0.0365(7) Uani 1 1 d . . . C13 C 0.4798(2) 0.7145(2) 0.38385(7) 0.0492(10) Uani 1 1 d . . . H13 H 0.4312 0.7115 0.3767 0.059 Uiso 1 1 calc R . . C14 C 0.4654(2) 0.6595(2) 0.40045(7) 0.0489(10) Uani 1 1 d . . . H14 H 0.4074 0.6186 0.4045 0.059 Uiso 1 1 calc R . . C15 C 0.5338(2) 0.6630(2) 0.41121(7) 0.0472(9) Uani 1 1 d . . . H15 H 0.5237 0.6250 0.4228 0.057 Uiso 1 1 calc R . . C16 C 0.6191(2) 0.72314(19) 0.40503(6) 0.0369(8) Uani 1 1 d . . . H16 H 0.6673 0.7270 0.4126 0.044 Uiso 1 1 calc R . . C17 C 0.5796(3) 0.8355(3) 0.35907(7) 0.0611(11) Uani 1 1 d . . . H17A H 0.6151 0.8959 0.3639 0.092 Uiso 1 1 calc R . . H17B H 0.5236 0.8261 0.3538 0.092 Uiso 1 1 calc R . . H17C H 0.6102 0.8242 0.3477 0.092 Uiso 1 1 calc R . . Cu1A Cu 0.55449(2) 0.35515(2) 0.199847(6) 0.02882(10) Uani 1 1 d . . . P1A P 0.53271(5) 0.51767(5) 0.199737(12) 0.02416(17) Uani 1 1 d . . . S1A S 0.46666(5) 0.39983(5) 0.212608(13) 0.03225(19) Uani 1 1 d . . . S2A S 0.68835(5) 0.46234(5) 0.192125(14) 0.03176(18) Uani 1 1 d . . . N1A N 0.63505(15) 0.57646(15) 0.20485(4) 0.0275(6) Uani 1 1 d . . . N2A N 0.78131(16) 0.62358(16) 0.20621(4) 0.0316(6) Uani 1 1 d . . . H2A H 0.826(2) 0.614(2) 0.2029(5) 0.032(9) Uiso 1 1 d . . . O1A O 0.49241(12) 0.57508(13) 0.20710(3) 0.0279(5) Uani 1 1 d . . . O2A O 0.51515(13) 0.50929(13) 0.17544(3) 0.0310(5) Uani 1 1 d . . . C1A C 0.69858(18) 0.55994(18) 0.20209(5) 0.0265(7) Uani 1 1 d . . . C2A C 0.49363(19) 0.5984(2) 0.22936(5) 0.0307(7) Uani 1 1 d . . . H2A1 H 0.5192 0.5695 0.2380 0.037 Uiso 1 1 calc R . . C3A C 0.4002(2) 0.5639(3) 0.23585(6) 0.0576(11) Uani 1 1 d . . . H3A1 H 0.3677 0.5004 0.2342 0.086 Uiso 1 1 calc R . . H3A2 H 0.3740 0.5898 0.2269 0.086 Uiso 1 1 calc R . . H3A3 H 0.3981 0.5790 0.2507 0.086 Uiso 1 1 calc R . . C4A C 0.5500(2) 0.6957(2) 0.23135(6) 0.0439(9) Uani 1 1 d . . . H4A1 H 0.6094 0.7134 0.2268 0.066 Uiso 1 1 calc R . . H4A2 H 0.5509 0.7128 0.2461 0.066 Uiso 1 1 calc R . . H4A3 H 0.5265 0.7243 0.2224 0.066 Uiso 1 1 calc R . . C5A C 0.5579(2) 0.5868(2) 0.16135(5) 0.0395(8) Uani 1 1 d . . . H5A H 0.6031 0.6382 0.1694 0.047 Uiso 1 1 calc R . . C6A C 0.5995(5) 0.5634(4) 0.14404(9) 0.120(3) Uani 1 1 d . . . H6A1 H 0.6444 0.5528 0.1500 0.167 Uiso 1 1 calc R . . H6A2 H 0.6263 0.6114 0.1338 0.167 Uiso 1 1 calc R . . H6A3 H 0.5553 0.5107 0.1369 0.167 Uiso 1 1 calc R . . C7A C 0.4882(3) 0.6044(3) 0.15369(8) 0.0769(15) Uani 1 1 d . . . H7A1 H 0.4639 0.6201 0.1657 0.108 Uiso 1 1 calc R . . H7A2 H 0.4420 0.5521 0.1468 0.108 Uiso 1 1 calc R . . H7A3 H 0.5132 0.6526 0.1435 0.108 Uiso 1 1 calc R . . C11A C 0.80596(17) 0.71334(18) 0.20996(5) 0.0281(7) Uani 1 1 d . . . C12A C 0.78864(18) 0.73855(19) 0.22928(5) 0.0286(6) Uani 1 1 d . . . C13A C 0.81405(19) 0.82652(19) 0.23160(5) 0.0324(7) Uani 1 1 d . . . H13A H 0.8022 0.8458 0.2445 0.039 Uiso 1 1 calc R . . C14A C 0.8560(2) 0.88631(19) 0.21561(6) 0.0387(8) Uani 1 1 d . . . H14A H 0.8729 0.9458 0.2177 0.046 Uiso 1 1 calc R . . C15A C 0.8731(2) 0.8597(2) 0.19671(6) 0.0439(9) Uani 1 1 d . . . H15A H 0.9024 0.9007 0.1857 0.053 Uiso 1 1 calc R . . C16A C 0.8474(2) 0.7725(2) 0.19375(5) 0.0369(7) Uani 1 1 d . . . H16A H 0.8582 0.7534 0.1806 0.044 Uiso 1 1 calc R . . C17A C 0.7465(2) 0.6763(2) 0.24733(6) 0.0395(8) Uani 1 1 d . . . H17D H 0.7756 0.6422 0.2494 0.059 Uiso 1 1 calc R . . H17E H 0.6848 0.6370 0.2441 0.059 Uiso 1 1 calc R . . H17F H 0.7516 0.7090 0.2603 0.059 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 Cu1 0.01767(19) 0.02161(19) 0.0357(2) -0.00119(15) -0.00028(15) 0.00753(15) P1 0.0195(4) 0.0183(4) 0.0268(4) -0.0005(3) 0.0014(3) 0.0093(3) S1 0.0206(4) 0.0243(4) 0.0426(5) 0.0040(3) -0.0024(3) 0.0102(3) S2 0.0193(4) 0.0180(4) 0.0418(4) 0.0006(3) 0.0031(3) 0.0089(3) N1 0.0200(12) 0.0179(12) 0.0355(14) -0.0036(10) 0.0027(10) 0.0090(10) N2 0.0196(12) 0.0185(13) 0.0489(17) -0.0019(11) 0.0060(11) 0.0087(10) O1 0.0329(11) 0.0344(11) 0.0295(12) -0.0011(9) 0.0013(9) 0.0231(10) O2 0.0255(10) 0.0165(10) 0.0288(11) -0.0038(8) -0.0015(8) 0.0087(8) C1 0.0168(14) 0.0200(14) 0.0312(16) -0.0058(11) -0.0035(11) 0.0075(12) C2 0.0434(19) 0.0422(19) 0.0352(19) -0.0018(14) 0.0096(14) 0.0286(16) C3 0.087(3) 0.065(3) 0.069(3) 0.011(2) 0.046(3) 0.035(3) C4 0.059(3) 0.067(3) 0.056(3) -0.027(2) 0.002(2) 0.034(2) C5 0.0270(16) 0.0228(15) 0.0327(17) 0.0026(12) -0.0014(13) 0.0094(13) C6 0.0272(17) 0.0326(18) 0.0353(19) 0.0013(14) 0.0032(13) 0.0075(14) C7 0.052(2) 0.050(2) 0.065(3) 0.0196(19) 0.0031(19) 0.035(2) C11 0.0199(14) 0.0178(14) 0.051(2) -0.0095(13) 0.0073(13) 0.0077(12) C12 0.0282(16) 0.0355(17) 0.047(2) -0.0082(15) -0.0004(14) 0.0167(14) C13 0.0216(16) 0.050(2) 0.073(3) -0.021(2) -0.0012(16) 0.0158(16) C14 0.0269(18) 0.0308(18) 0.076(3) -0.0115(18) 0.0148(17) 0.0043(15) C15 0.044(2) 0.0260(17) 0.067(3) 0.0004(16) 0.0213(18) 0.0139(16) C16 0.0287(17) 0.0262(16) 0.054(2) -0.0014(15) 0.0084(15) 0.0123(14) C17 0.048(2) 0.082(3) 0.055(3) 0.002(2) -0.0047(19) 0.034(2) Cu1A 0.0249(2) 0.01994(19) 0.0396(2) 0.00278(16) -0.00226(16) 0.00972(16) P1A 0.0198(4) 0.0243(4) 0.0292(4) -0.0001(3) -0.0005(3) 0.0116(3) S1A 0.0250(4) 0.0286(4) 0.0412(5) 0.0070(3) 0.0063(3) 0.0119(3) S2A 0.0218(4) 0.0192(4) 0.0549(5) -0.0038(3) 0.0021(3) 0.0106(3) N1A 0.0208(12) 0.0223(13) 0.0396(15) -0.0033(11) -0.0015(10) 0.0109(11) N2A 0.0193(13) 0.0204(13) 0.0563(18) -0.0074(11) 0.0000(12) 0.0108(11) O1A 0.0270(11) 0.0345(12) 0.0295(12) -0.0009(9) -0.0011(9) 0.0208(10) O2A 0.0324(12) 0.0269(11) 0.0282(12) 0.0012(9) -0.0003(9) 0.0108(9) C1A 0.0217(15) 0.0177(14) 0.0404(18) 0.0006(12) 0.0002(12) 0.0101(12) C2A 0.0275(16) 0.0379(18) 0.0304(17) -0.0006(13) -0.0005(13) 0.0191(15) C3A 0.036(2) 0.094(3) 0.046(2) -0.010(2) 0.0050(17) 0.034(2) C4A 0.062(2) 0.037(2) 0.040(2) -0.0047(15) -0.0079(17) 0.0304(19) C5A 0.052(2) 0.0276(16) 0.0350(19) 0.0078(13) 0.0039(15) 0.0167(15) C6A 0.199(7) 0.093(4) 0.103(5) 0.061(3) 0.110(5) 0.100(5) C7A 0.086(3) 0.055(3) 0.081(3) 0.017(2) -0.027(3) 0.029(3) C11A 0.0153(13) 0.0208(14) 0.048(2) -0.0039(13) -0.0029(12) 0.0088(12) C12A 0.0213(14) 0.0255(15) 0.0370(18) -0.0012(13) -0.0049(12) 0.0102(12) C13A 0.0286(16) 0.0282(16) 0.0409(19) -0.0080(13) -0.0022(13) 0.0145(14) C14A 0.0370(18) 0.0210(15) 0.055(2) -0.0038(14) 0.0002(15) 0.0126(14) C15A 0.041(2) 0.0266(17) 0.054(2) 0.0068(15) 0.0101(16) 0.0095(15) C16A 0.0356(18) 0.0282(16) 0.041(2) -0.0048(14) 0.0078(14) 0.0119(14) C17A 0.0400(19) 0.0348(18) 0.042(2) 0.0020(14) -0.0009(15) 0.0176(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 S2 2.2052(8) 2_765 ? Cu1 S1 2.2293(8) . ? Cu1 S2 2.2307(8) . ? P1 O1 1.562(2) . ? P1 O2 1.575(2) . ? P1 N1 1.607(2) . ? P1 S1 1.9997(10) . ? S2 C1 1.754(3) . ? S2 Cu1 2.2051(8) 3_675 ? N1 C1 1.303(3) . ? N2 C1 1.358(4) . ? N2 C11 1.431(4) . ? N2 H2 0.87(3) . ? O1 C2 1.476(3) . ? O2 C5 1.469(3) . ? C2 C3 1.485(5) . ? C2 C4 1.505(5) . ? C2 H2B 1.0000 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C7 1.507(4) . ? C5 C6 1.517(4) . ? C5 H5 1.0000 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C11 C12 1.378(5) . ? C11 C16 1.379(5) . ? C12 C13 1.409(5) . ? C12 C17 1.488(5) . ? C13 C14 1.366(6) . ? C13 H13 0.9500 . ? C14 C15 1.364(6) . ? C14 H14 0.9500 . ? C15 C16 1.401(4) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? Cu1A S2A 2.2099(8) 2_655 ? Cu1A S1A 2.2215(9) . ? Cu1A S2A 2.2293(8) . ? P1A O2A 1.559(2) . ? P1A O1A 1.578(2) . ? P1A N1A 1.609(2) . ? P1A S1A 1.9874(11) . ? S2A C1A 1.763(3) . ? S2A Cu1A 2.2098(8) 3_665 ? N1A C1A 1.309(4) . ? N2A C1A 1.355(4) . ? N2A C11A 1.443(4) . ? N2A H2A 0.91(3) . ? O1A C2A 1.463(4) . ? O2A C5A 1.489(4) . ? C2A C4A 1.505(4) . ? C2A C3A 1.508(4) . ? C2A H2A1 1.0000 . ? C3A H3A1 0.9800 . ? C3A H3A2 0.9800 . ? C3A H3A3 0.9800 . ? C4A H4A1 0.9800 . ? C4A H4A2 0.9800 . ? C4A H4A3 0.9800 . ? C5A C6A 1.490(5) . ? C5A C7A 1.496(5) . ? C5A H5A 1.0000 . ? C6A H6A1 0.9800 . ? C6A H6A2 0.9800 . ? C6A H6A3 0.9800 . ? C7A H7A1 0.9800 . ? C7A H7A2 0.9800 . ? C7A H7A3 0.9800 . ? C11A C16A 1.385(4) . ? C11A C12A 1.387(4) . ? C12A C13A 1.398(4) . ? C12A C17A 1.501(4) . ? C13A C14A 1.382(5) . ? C13A H13A 0.9500 . ? C14A C15A 1.373(5) . ? C14A H14A 0.9500 . ? C15A C16A 1.389(4) . ? C15A H15A 0.9500 . ? C16A H16A 0.9500 . ? C17A H17D 0.9800 . ? C17A H17E 0.9800 . ? C17A H17F 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 S2 Cu1 S1 132.68(3) 2_765 . ? S2 Cu1 S2 112.41(4) 2_765 . ? S1 Cu1 S2 114.89(3) . . ? O1 P1 O2 102.81(11) . . ? O1 P1 N1 106.78(12) . . ? O2 P1 N1 105.73(12) . . ? O1 P1 S1 113.55(9) . . ? O2 P1 S1 108.76(8) . . ? N1 P1 S1 117.90(10) . . ? P1 S1 Cu1 93.11(4) . . ? C1 S2 Cu1 112.15(10) . 3_675 ? C1 S2 Cu1 105.77(10) . . ? Cu1 S2 Cu1 120.10(4) 3_675 . ? C1 N1 P1 128.8(2) . . ? C1 N2 C11 124.7(2) . . ? C1 N2 H2 115(2) . . ? C11 N2 H2 117(2) . . ? C2 O1 P1 121.75(19) . . ? C5 O2 P1 120.60(17) . . ? N1 C1 N2 118.9(3) . . ? N1 C1 S2 126.1(2) . . ? N2 C1 S2 115.0(2) . . ? O1 C2 C3 107.5(3) . . ? O1 C2 C4 106.7(3) . . ? C3 C2 C4 114.8(4) . . ? O1 C2 H2B 109.2 . . ? C3 C2 H2B 109.2 . . ? C4 C2 H2B 109.2 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O2 C5 C7 107.5(3) . . ? O2 C5 C6 107.7(2) . . ? C7 C5 C6 113.4(3) . . ? O2 C5 H5 109.4 . . ? C7 C5 H5 109.4 . . ? C6 C5 H5 109.4 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C12 C11 C16 122.2(3) . . ? C12 C11 N2 118.4(3) . . ? C16 C11 N2 119.5(3) . . ? C11 C12 C13 116.6(3) . . ? C11 C12 C17 121.8(3) . . ? C13 C12 C17 121.6(3) . . ? C14 C13 C12 121.9(3) . . ? C14 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? C15 C14 C13 120.4(3) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 119.5(4) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C11 C16 C15 119.4(3) . . ? C11 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? S2A Cu1A S1A 133.93(3) 2_655 . ? S2A Cu1A S2A 111.68(4) 2_655 . ? S1A Cu1A S2A 114.37(3) . . ? O2A P1A O1A 102.63(11) . . ? O2A P1A N1A 111.47(13) . . ? O1A P1A N1A 104.50(12) . . ? O2A P1A S1A 108.57(9) . . ? O1A P1A S1A 109.77(9) . . ? N1A P1A S1A 118.65(10) . . ? P1A S1A Cu1A 94.38(4) . . ? C1A S2A Cu1A 113.32(10) . 3_665 ? C1A S2A Cu1A 107.55(10) . . ? Cu1A S2A Cu1A 118.90(4) 3_665 . ? C1A N1A P1A 130.2(2) . . ? C1A N2A C11A 123.7(2) . . ? C1A N2A H2A 118(2) . . ? C11A N2A H2A 116(2) . . ? C2A O1A P1A 121.21(17) . . ? C5A O2A P1A 121.1(2) . . ? N1A C1A N2A 118.8(3) . . ? N1A C1A S2A 126.1(2) . . ? N2A C1A S2A 115.0(2) . . ? O1A C2A C4A 108.2(3) . . ? O1A C2A C3A 106.8(3) . . ? C4A C2A C3A 114.1(3) . . ? O1A C2A H2A1 109.2 . . ? C4A C2A H2A1 109.2 . . ? C3A C2A H2A1 109.2 . . ? C2A C3A H3A1 109.5 . . ? C2A C3A H3A2 109.5 . . ? H3A1 C3A H3A2 109.5 . . ? C2A C3A H3A3 109.5 . . ? H3A1 C3A H3A3 109.5 . . ? H3A2 C3A H3A3 109.5 . . ? C2A C4A H4A1 109.5 . . ? C2A C4A H4A2 109.5 . . ? H4A1 C4A H4A2 109.5 . . ? C2A C4A H4A3 109.5 . . ? H4A1 C4A H4A3 109.5 . . ? H4A2 C4A H4A3 109.5 . . ? O2A C5A C6A 106.1(3) . . ? O2A C5A C7A 107.1(3) . . ? C6A C5A C7A 113.3(4) . . ? O2A C5A H5A 110.1 . . ? C6A C5A H5A 110.1 . . ? C7A C5A H5A 110.1 . . ? C5A C6A H6A1 109.5 . . ? C5A C6A H6A2 109.5 . . ? H6A1 C6A H6A2 109.5 . . ? C5A C6A H6A3 109.5 . . ? H6A1 C6A H6A3 109.5 . . ? H6A2 C6A H6A3 109.5 . . ? C5A C7A H7A1 109.5 . . ? C5A C7A H7A2 109.5 . . ? H7A1 C7A H7A2 109.5 . . ? C5A C7A H7A3 109.5 . . ? H7A1 C7A H7A3 109.5 . . ? H7A2 C7A H7A3 109.5 . . ? C16A C11A C12A 121.8(3) . . ? C16A C11A N2A 117.8(3) . . ? C12A C11A N2A 120.4(3) . . ? C11A C12A C13A 116.9(3) . . ? C11A C12A C17A 122.8(3) . . ? C13A C12A C17A 120.3(3) . . ? C14A C13A C12A 121.9(3) . . ? C14A C13A H13A 119.0 . . ? C12A C13A H13A 119.0 . . ? C15A C14A C13A 120.0(3) . . ? C15A C14A H14A 120.0 . . ? C13A C14A H14A 120.0 . . ? C14A C15A C16A 119.6(3) . . ? C14A C15A H15A 120.2 . . ? C16A C15A H15A 120.2 . . ? C11A C16A C15A 119.8(3) . . ? C11A C16A H16A 120.1 . . ? C15A C16A H16A 120.1 . . ? C12A C17A H17D 109.5 . . ? C12A C17A H17E 109.5 . . ? H17D C17A H17E 109.5 . . ? C12A C17A H17F 109.5 . . ? H17D C17A H17F 109.5 . . ? H17E C17A H17F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 P1 S1 Cu1 69.34(9) . . . . ? O2 P1 S1 Cu1 -176.87(8) . . . . ? N1 P1 S1 Cu1 -56.61(11) . . . . ? S2 Cu1 S1 P1 -158.14(4) 2_765 . . . ? S2 Cu1 S1 P1 19.83(5) . . . . ? S2 Cu1 S2 C1 -165.72(10) 2_765 . . . ? S1 Cu1 S2 C1 15.89(11) . . . . ? S2 Cu1 S2 Cu1 -37.66(7) 2_765 . . 3_675 ? S1 Cu1 S2 Cu1 143.96(4) . . . 3_675 ? O1 P1 N1 C1 -68.9(3) . . . . ? O2 P1 N1 C1 -177.9(3) . . . . ? S1 P1 N1 C1 60.3(3) . . . . ? O2 P1 O1 C2 -69.6(2) . . . . ? N1 P1 O1 C2 179.3(2) . . . . ? S1 P1 O1 C2 47.7(2) . . . . ? O1 P1 O2 C5 -179.48(19) . . . . ? N1 P1 O2 C5 -67.7(2) . . . . ? S1 P1 O2 C5 59.9(2) . . . . ? P1 N1 C1 N2 178.3(2) . . . . ? P1 N1 C1 S2 -0.3(4) . . . . ? C11 N2 C1 N1 -11.0(5) . . . . ? C11 N2 C1 S2 167.7(3) . . . . ? Cu1 S2 C1 N1 -166.3(2) 3_675 . . . ? Cu1 S2 C1 N1 -33.7(3) . . . . ? Cu1 S2 C1 N2 15.1(3) 3_675 . . . ? Cu1 S2 C1 N2 147.7(2) . . . . ? P1 O1 C2 C3 -121.8(3) . . . . ? P1 O1 C2 C4 114.5(3) . . . . ? P1 O2 C5 C7 -121.3(2) . . . . ? P1 O2 C5 C6 116.1(2) . . . . ? C1 N2 C11 C12 -117.6(3) . . . . ? C1 N2 C11 C16 62.3(4) . . . . ? C16 C11 C12 C13 -2.1(5) . . . . ? N2 C11 C12 C13 177.8(3) . . . . ? C16 C11 C12 C17 177.9(3) . . . . ? N2 C11 C12 C17 -2.2(5) . . . . ? C11 C12 C13 C14 0.4(5) . . . . ? C17 C12 C13 C14 -179.5(4) . . . . ? C12 C13 C14 C15 0.8(6) . . . . ? C13 C14 C15 C16 -0.4(5) . . . . ? C12 C11 C16 C15 2.5(5) . . . . ? N2 C11 C16 C15 -177.4(3) . . . . ? C14 C15 C16 C11 -1.2(5) . . . . ? O2A P1A S1A Cu1A 73.17(9) . . . . ? O1A P1A S1A Cu1A -175.37(8) . . . . ? N1A P1A S1A Cu1A -55.41(12) . . . . ? S2A Cu1A S1A P1A -154.58(5) 2_655 . . . ? S2A Cu1A S1A P1A 23.39(5) . . . . ? S2A Cu1A S2A C1A -172.38(11) 2_655 . . . ? S1A Cu1A S2A C1A 9.19(12) . . . . ? S2A Cu1A S2A Cu1A -41.92(7) 2_655 . . 3_665 ? S1A Cu1A S2A Cu1A 139.65(4) . . . 3_665 ? O2A P1A N1A C1A -70.6(3) . . . . ? O1A P1A N1A C1A 179(60) . . . . ? S1A P1A N1A C1A 56.6(3) . . . . ? O2A P1A O1A C2A 179.2(2) . . . . ? N1A P1A O1A C2A -64.4(2) . . . . ? S1A P1A O1A C2A 63.9(2) . . . . ? O1A P1A O2A C5A 65.5(2) . . . . ? N1A P1A O2A C5A -45.8(3) . . . . ? S1A P1A O2A C5A -178.3(2) . . . . ? P1A N1A C1A N2A 174.9(2) . . . . ? P1A N1A C1A S2A -1.9(5) . . . . ? C11A N2A C1A N1A -11.2(5) . . . . ? C11A N2A C1A S2A 166.0(2) . . . . ? Cu1A S2A C1A N1A -160.9(2) 3_665 . . . ? Cu1A S2A C1A N1A -27.4(3) . . . . ? Cu1A S2A C1A N2A 22.2(3) 3_665 . . . ? Cu1A S2A C1A N2A 155.7(2) . . . . ? P1A O1A C2A C4A 115.3(2) . . . . ? P1A O1A C2A C3A -121.6(3) . . . . ? P1A O2A C5A C6A 127.7(4) . . . . ? P1A O2A C5A C7A -111.0(3) . . . . ? C1A N2A C11A C16A -103.6(4) . . . . ? C1A N2A C11A C12A 76.8(4) . . . . ? C16A C11A C12A C13A 0.7(4) . . . . ? N2A C11A C12A C13A -179.6(3) . . . . ? C16A C11A C12A C17A -178.0(3) . . . . ? N2A C11A C12A C17A 1.7(4) . . . . ? C11A C12A C13A C14A -1.2(4) . . . . ? C17A C12A C13A C14A 177.5(3) . . . . ? C12A C13A C14A C15A 0.6(5) . . . . ? C13A C14A C15A C16A 0.6(5) . . . . ? C12A C11A C16A C15A 0.3(5) . . . . ? N2A C11A C16A C15A -179.3(3) . . . . ? C14A C15A C16A C11A -1.0(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2 S1 0.87(3) 2.83(4) 3.657(3) 161(3) 3_675 N2A H2A S1A 0.91(3) 2.96(3) 3.778(3) 151(3) 3_665 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.090 _refine_diff_density_min -0.618 _refine_diff_density_rms 0.093 # Attachment '- 13.cif' data_safin40 _database_code_depnum_ccdc_archive 'CCDC 749078' #TrackingRef '- 13.cif' # start Validation Reply Form _vrf_PLAT220_safin40 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 8.12 Ratio RESPONSE: One isopropyl group is disordered and already refined using a split model. ; _vrf_PLAT222_safin40 ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 8.43 Ratio RESPONSE: One isopropyl group is disordered and already refined using a split model. ; _vrf_PLAT242_safin40 ; PROBLEM: Check Low Ueq as Compared to Neighbors for C3 RESPONSE: The central C atom of the isopropyl group is not disordered. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H46 Cu Fe N2 O2 P3 S2' _chemical_formula_sum 'C42 H46 Cu Fe N2 O2 P3 S2' _chemical_formula_weight 887.23 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4051(8) _cell_length_b 12.9190(12) _cell_length_c 16.2445(15) _cell_angle_alpha 80.986(7) _cell_angle_beta 76.688(7) _cell_angle_gamma 79.581(7) _cell_volume 2074.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 13667 _cell_measurement_theta_min 3.6 _cell_measurement_theta_max 26.1 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.420 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 1.116 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7235 _exptl_absorpt_correction_T_max 0.8777 _exptl_absorpt_process_details 'MULABS (Spek, 2003; Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS II two-circle-diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 17701 _diffrn_reflns_av_R_equivalents 0.1058 _diffrn_reflns_av_sigmaI/netI 0.1358 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.49 _diffrn_reflns_theta_max 25.03 _reflns_number_total 7292 _reflns_number_gt 4950 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'X-Area (Stoe & Cie, 2001)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2001)' _computing_data_reduction 'X-Area (Stoe & Cie, 2001)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008) ' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008) ' _computing_molecular_graphics 'XP in SHELXTL-Plus (Sheldrick, 1991)' _computing_publication_material SHELXL97 _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^)+(0.1722P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7292 _refine_ls_number_parameters 478 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1292 _refine_ls_R_factor_gt 0.0999 _refine_ls_wR_factor_ref 0.2705 _refine_ls_wR_factor_gt 0.2523 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.77024(8) 0.57622(8) 0.72940(6) 0.0340(3) Uani 1 1 d . . . Fe1 Fe 0.50255(10) 0.79934(10) 0.85443(8) 0.0412(4) Uani 1 1 d . . . P1 P 0.76000(17) 0.31448(17) 0.78341(13) 0.0326(5) Uani 1 1 d . . . P2 P 0.83579(17) 0.68986(17) 0.79850(13) 0.0338(5) Uani 1 1 d . . . P3 P 0.58977(16) 0.66468(17) 0.67426(13) 0.0335(5) Uani 1 1 d . . . S1 S 0.67169(19) 0.44694(17) 0.83096(13) 0.0407(5) Uani 1 1 d . . . S2 S 0.94242(17) 0.48719(17) 0.63912(13) 0.0378(5) Uani 1 1 d . . . O1 O 0.6625(5) 0.2278(4) 0.8099(3) 0.0378(12) Uani 1 1 d D A . O2 O 0.8724(5) 0.2615(5) 0.8344(4) 0.0432(14) Uani 1 1 d . . . N1 N 0.8125(6) 0.3117(5) 0.6830(4) 0.0364(15) Uani 1 1 d . . . N2 N 0.9056(6) 0.3546(6) 0.5437(4) 0.0393(16) Uani 1 1 d . . . H2 H 0.9508 0.3968 0.5041 0.047 Uiso 1 1 calc R . . C1 C 0.8805(6) 0.3772(6) 0.6239(5) 0.0324(17) Uani 1 1 d . . . C2 C 0.8646(9) 0.2664(8) 0.5168(6) 0.049(2) Uani 1 1 d . . . H2A H 0.8846 0.2019 0.5552 0.073 Uiso 1 1 calc R . . H2B H 0.9129 0.2564 0.4586 0.073 Uiso 1 1 calc R . . H2C H 0.7683 0.2811 0.5184 0.073 Uiso 1 1 calc R . . C3 C 0.5552(7) 0.2304(6) 0.7644(5) 0.0401(19) Uani 1 1 d D . . H3 H 0.5807 0.2698 0.7064 0.048 Uiso 0.81(3) 1 calc PR A 1 H3' H 0.5422 0.3075 0.7425 0.048 Uiso 0.19(3) 1 calc PR A 2 C4 C 0.4258(11) 0.2879(13) 0.8085(9) 0.059(4) Uiso 0.81(3) 1 d PD A 1 H4A H 0.4335 0.3628 0.8063 0.088 Uiso 0.81(3) 1 calc PR A 1 H4B H 0.4046 0.2566 0.8681 0.088 Uiso 0.81(3) 1 calc PR A 1 H4C H 0.3545 0.2820 0.7800 0.088 Uiso 0.81(3) 1 calc PR A 1 C5 C 0.5537(15) 0.1159(11) 0.7535(10) 0.074(5) Uiso 0.81(3) 1 d PD A 1 H5A H 0.6426 0.0849 0.7248 0.111 Uiso 0.81(3) 1 calc PR A 1 H5B H 0.4885 0.1135 0.7190 0.111 Uiso 0.81(3) 1 calc PR A 1 H5C H 0.5288 0.0754 0.8095 0.111 Uiso 0.81(3) 1 calc PR A 1 C4' C 0.4259(18) 0.226(4) 0.8315(18) 0.037(12) Uiso 0.19(3) 1 d PD A 2 H4'1 H 0.4045 0.2903 0.8602 0.056 Uiso 0.19(3) 1 calc PR A 2 H4'2 H 0.4372 0.1636 0.8735 0.056 Uiso 0.19(3) 1 calc PR A 2 H4'3 H 0.3530 0.2217 0.8039 0.056 Uiso 0.19(3) 1 calc PR A 2 C5' C 0.625(17) 0.184(12) 0.6788(14) 0.26(10) Uiso 0.19(3) 1 d PD A 2 H5'1 H 0.7085 0.2129 0.6548 0.396 Uiso 0.19(3) 1 calc PR A 2 H5'2 H 0.5657 0.2025 0.6383 0.396 Uiso 0.19(3) 1 calc PR A 2 H5'3 H 0.6454 0.1063 0.6900 0.396 Uiso 0.19(3) 1 calc PR A 2 C6 C 0.9517(11) 0.1617(9) 0.8148(7) 0.064(3) Uani 1 1 d . . . H6 H 0.9337 0.1414 0.7620 0.076 Uiso 1 1 calc R . . C7 C 0.9189(17) 0.0790(11) 0.8885(10) 0.102(5) Uani 1 1 d . . . H7A H 0.8258 0.0685 0.8956 0.153 Uiso 1 1 calc R . . H7B H 0.9313 0.1021 0.9404 0.153 Uiso 1 1 calc R . . H7C H 0.9781 0.0122 0.8778 0.153 Uiso 1 1 calc R . . C8 C 1.0959(11) 0.1801(14) 0.8003(9) 0.102(5) Uani 1 1 d . . . H8A H 1.1141 0.2343 0.7515 0.153 Uiso 1 1 calc R . . H8B H 1.1557 0.1138 0.7888 0.153 Uiso 1 1 calc R . . H8C H 1.1106 0.2039 0.8512 0.153 Uiso 1 1 calc R . . C11 C 0.9559(7) 0.6385(7) 0.8664(5) 0.0411(19) Uani 1 1 d . . . C12 C 0.9636(9) 0.6911(8) 0.9340(6) 0.050(2) Uani 1 1 d . . . H12 H 0.9041 0.7543 0.9465 0.060 Uiso 1 1 calc R . . C13 C 1.0596(9) 0.6497(10) 0.9829(6) 0.058(3) Uani 1 1 d . . . H13 H 1.0620 0.6820 1.0311 0.069 Uiso 1 1 calc R . . C14 C 1.1521(9) 0.5606(10) 0.9605(7) 0.062(3) Uani 1 1 d . . . H14 H 1.2208 0.5342 0.9914 0.075 Uiso 1 1 calc R . . C15 C 1.1428(8) 0.5122(9) 0.8946(7) 0.059(3) Uani 1 1 d . . . H15 H 1.2052 0.4511 0.8803 0.070 Uiso 1 1 calc R . . C16 C 1.0452(8) 0.5490(7) 0.8471(6) 0.0425(19) Uani 1 1 d . . . H16 H 1.0401 0.5126 0.8017 0.051 Uiso 1 1 calc R . . C21 C 0.9076(7) 0.8006(7) 0.7327(5) 0.0358(17) Uani 1 1 d . . . C22 C 0.8383(7) 0.8681(7) 0.6760(5) 0.0401(18) Uani 1 1 d . . . H22 H 0.7510 0.8569 0.6749 0.048 Uiso 1 1 calc R . . C23 C 0.8914(9) 0.9502(8) 0.6215(6) 0.051(2) Uani 1 1 d . . . H23 H 0.8420 0.9935 0.5830 0.061 Uiso 1 1 calc R . . C24 C 1.0184(9) 0.9688(8) 0.6238(6) 0.051(2) Uani 1 1 d . . . H24 H 1.0552 1.0260 0.5874 0.061 Uiso 1 1 calc R . . C25 C 1.0897(9) 0.9054(8) 0.6778(7) 0.054(2) Uani 1 1 d . . . H25 H 1.1766 0.9180 0.6783 0.065 Uiso 1 1 calc R . . C26 C 1.0367(8) 0.8217(8) 0.7328(6) 0.047(2) Uani 1 1 d . . . H26 H 1.0876 0.7786 0.7705 0.056 Uiso 1 1 calc R . . C31 C 0.4795(7) 0.5826(7) 0.6510(5) 0.0367(17) Uani 1 1 d . . . C32 C 0.5381(9) 0.4891(8) 0.6180(6) 0.047(2) Uani 1 1 d . . . H32 H 0.6320 0.4687 0.6115 0.057 Uiso 1 1 calc R . . C33 C 0.4644(11) 0.4239(8) 0.5940(7) 0.059(3) Uani 1 1 d . . . H33 H 0.5073 0.3609 0.5699 0.070 Uiso 1 1 calc R . . C34 C 0.3262(10) 0.4526(9) 0.6060(6) 0.056(3) Uani 1 1 d . . . H34 H 0.2736 0.4085 0.5910 0.067 Uiso 1 1 calc R . . C35 C 0.2660(8) 0.5458(10) 0.6397(6) 0.060(3) Uani 1 1 d . . . H35 H 0.1718 0.5651 0.6479 0.072 Uiso 1 1 calc R . . C36 C 0.3417(8) 0.6114(9) 0.6618(6) 0.052(2) Uani 1 1 d . . . H36 H 0.2995 0.6756 0.6841 0.063 Uiso 1 1 calc R . . C41 C 0.6208(7) 0.7490(7) 0.5729(5) 0.0384(18) Uani 1 1 d . . . C42 C 0.7491(8) 0.7445(7) 0.5238(5) 0.0417(19) Uani 1 1 d . . . H42 H 0.8203 0.6997 0.5450 0.050 Uiso 1 1 calc R . . C43 C 0.7761(9) 0.8021(9) 0.4464(6) 0.054(2) Uani 1 1 d . . . H43 H 0.8651 0.7952 0.4141 0.064 Uiso 1 1 calc R . . C44 C 0.6770(10) 0.8708(9) 0.4133(7) 0.058(2) Uani 1 1 d . . . H44 H 0.6969 0.9123 0.3595 0.070 Uiso 1 1 calc R . . C45 C 0.5437(10) 0.8774(9) 0.4626(7) 0.060(3) Uani 1 1 d . . . H45 H 0.4731 0.9228 0.4413 0.073 Uiso 1 1 calc R . . C46 C 0.5176(8) 0.8183(8) 0.5406(6) 0.049(2) Uani 1 1 d . . . H46 H 0.4289 0.8240 0.5734 0.059 Uiso 1 1 calc R . . C51 C 0.6969(7) 0.7521(7) 0.8714(5) 0.0410(19) Uani 1 1 d . . . C52 C 0.6054(8) 0.6948(9) 0.9335(5) 0.049(2) Uani 1 1 d . . . H52 H 0.6092 0.6199 0.9423 0.058 Uiso 1 1 calc R . . C53 C 0.5080(9) 0.7684(10) 0.9798(6) 0.060(3) Uani 1 1 d . . . H53 H 0.4354 0.7509 1.0243 0.072 Uiso 1 1 calc R . . C54 C 0.5366(9) 0.8705(10) 0.9494(7) 0.061(3) Uani 1 1 d . . . H54 H 0.4869 0.9341 0.9697 0.073 Uiso 1 1 calc R . . C55 C 0.6557(9) 0.8633(8) 0.8812(7) 0.054(2) Uani 1 1 d . . . H55 H 0.6981 0.9206 0.8494 0.064 Uiso 1 1 calc R . . C61 C 0.4736(7) 0.7524(7) 0.7434(5) 0.0382(18) Uani 1 1 d . . . C62 C 0.3785(7) 0.7164(9) 0.8175(6) 0.051(2) Uani 1 1 d . . . H62 H 0.3675 0.6448 0.8375 0.061 Uiso 1 1 calc R . . C63 C 0.3034(8) 0.8082(9) 0.8558(8) 0.062(3) Uani 1 1 d . . . H63 H 0.2328 0.8079 0.9047 0.074 Uiso 1 1 calc R . . C64 C 0.3540(8) 0.8999(8) 0.8069(7) 0.054(2) Uani 1 1 d . . . H64 H 0.3239 0.9715 0.8176 0.064 Uiso 1 1 calc R . . C65 C 0.4571(7) 0.8641(7) 0.7400(6) 0.045(2) Uani 1 1 d . . . H65 H 0.5085 0.9089 0.6982 0.054 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 Cu1 0.0195(4) 0.0378(6) 0.0461(6) -0.0046(4) -0.0099(4) -0.0040(4) Fe1 0.0213(5) 0.0485(8) 0.0559(8) -0.0155(6) -0.0070(5) -0.0041(5) P1 0.0206(8) 0.0376(11) 0.0400(10) -0.0018(9) -0.0091(7) -0.0039(7) P2 0.0214(8) 0.0382(12) 0.0438(11) -0.0036(9) -0.0124(7) -0.0038(8) P3 0.0169(8) 0.0394(12) 0.0454(11) -0.0029(9) -0.0112(7) -0.0036(7) S1 0.0340(9) 0.0384(12) 0.0458(11) -0.0033(9) -0.0019(8) -0.0050(8) S2 0.0213(8) 0.0460(12) 0.0474(11) -0.0082(9) -0.0035(7) -0.0106(8) O1 0.028(2) 0.040(3) 0.048(3) 0.000(3) -0.014(2) -0.007(2) O2 0.030(3) 0.051(4) 0.052(3) -0.006(3) -0.016(2) -0.004(2) N1 0.023(3) 0.033(4) 0.054(4) 0.001(3) -0.011(3) -0.009(3) N2 0.030(3) 0.049(4) 0.039(4) -0.010(3) -0.003(3) -0.010(3) C1 0.011(3) 0.040(4) 0.046(4) -0.006(4) -0.008(3) -0.002(3) C2 0.050(5) 0.048(5) 0.052(5) -0.015(4) -0.006(4) -0.017(4) C3 0.027(4) 0.047(5) 0.052(5) 0.004(4) -0.019(3) -0.013(3) C6 0.067(6) 0.051(6) 0.071(7) -0.010(5) -0.034(5) 0.024(5) C7 0.127(13) 0.062(9) 0.117(12) -0.002(8) -0.056(10) 0.014(8) C8 0.046(6) 0.152(15) 0.094(10) -0.023(10) -0.015(6) 0.031(7) C11 0.030(4) 0.055(6) 0.039(4) 0.005(4) -0.010(3) -0.014(4) C12 0.047(5) 0.057(6) 0.050(5) 0.000(4) -0.022(4) -0.012(4) C13 0.043(5) 0.085(8) 0.052(5) 0.010(5) -0.030(4) -0.019(5) C14 0.034(4) 0.088(8) 0.067(6) 0.027(6) -0.034(4) -0.018(5) C15 0.029(4) 0.062(7) 0.081(7) 0.010(5) -0.019(4) -0.002(4) C16 0.032(4) 0.042(5) 0.050(5) -0.001(4) -0.008(3) -0.002(3) C21 0.027(3) 0.041(5) 0.042(4) -0.006(4) -0.007(3) -0.009(3) C22 0.028(4) 0.040(5) 0.054(5) 0.002(4) -0.018(3) -0.003(3) C23 0.053(5) 0.041(5) 0.059(6) 0.013(4) -0.018(4) -0.014(4) C24 0.045(5) 0.049(6) 0.060(6) 0.006(5) -0.011(4) -0.021(4) C25 0.031(4) 0.056(6) 0.076(6) -0.002(5) -0.007(4) -0.016(4) C26 0.029(4) 0.049(5) 0.066(6) -0.002(4) -0.018(4) -0.009(4) C31 0.030(4) 0.047(5) 0.037(4) 0.000(4) -0.014(3) -0.009(3) C32 0.041(4) 0.048(5) 0.056(5) 0.002(4) -0.024(4) -0.006(4) C33 0.069(6) 0.040(5) 0.077(7) -0.005(5) -0.040(5) -0.003(5) C34 0.057(5) 0.069(7) 0.055(5) 0.004(5) -0.024(4) -0.035(5) C35 0.028(4) 0.097(9) 0.064(6) -0.014(6) -0.008(4) -0.034(5) C36 0.024(4) 0.069(7) 0.070(6) -0.016(5) -0.011(4) -0.015(4) C41 0.029(4) 0.034(4) 0.053(5) -0.002(4) -0.012(3) -0.006(3) C42 0.031(4) 0.047(5) 0.050(5) 0.003(4) -0.016(3) -0.012(3) C43 0.039(4) 0.068(7) 0.057(6) 0.002(5) -0.018(4) -0.014(4) C44 0.055(5) 0.053(6) 0.066(6) 0.012(5) -0.020(5) -0.013(5) C45 0.050(5) 0.055(6) 0.076(7) 0.004(5) -0.028(5) 0.002(5) C46 0.036(4) 0.054(6) 0.053(5) 0.011(4) -0.017(4) -0.004(4) C51 0.029(4) 0.058(6) 0.042(4) -0.006(4) -0.015(3) -0.011(4) C52 0.029(4) 0.079(7) 0.038(4) -0.012(4) -0.004(3) -0.007(4) C53 0.037(4) 0.097(9) 0.046(5) -0.024(5) -0.003(4) -0.006(5) C54 0.032(4) 0.077(8) 0.079(7) -0.041(6) -0.009(4) 0.000(4) C55 0.037(4) 0.048(6) 0.083(7) -0.024(5) -0.025(4) 0.004(4) C61 0.018(3) 0.048(5) 0.054(5) -0.006(4) -0.012(3) -0.012(3) C62 0.024(4) 0.071(7) 0.060(5) -0.022(5) 0.004(4) -0.019(4) C63 0.024(4) 0.077(7) 0.092(8) -0.041(6) -0.008(4) -0.006(4) C64 0.029(4) 0.054(6) 0.080(7) -0.020(5) -0.020(4) 0.009(4) C65 0.024(3) 0.046(5) 0.065(5) -0.007(4) -0.019(3) 0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 P2 2.261(2) . ? Cu1 S2 2.293(2) . ? Cu1 P3 2.305(2) . ? Cu1 S1 2.354(2) . ? Fe1 C53 2.026(10) . ? Fe1 C65 2.039(9) . ? Fe1 C54 2.041(9) . ? Fe1 C64 2.045(9) . ? Fe1 C52 2.046(10) . ? Fe1 C63 2.050(8) . ? Fe1 C62 2.057(8) . ? Fe1 C51 2.072(8) . ? Fe1 C55 2.078(9) . ? Fe1 C61 2.091(8) . ? P1 O2 1.581(6) . ? P1 O1 1.590(6) . ? P1 N1 1.600(7) . ? P1 S1 1.972(3) . ? P2 C51 1.797(8) . ? P2 C21 1.813(8) . ? P2 C11 1.823(8) . ? P3 C61 1.812(8) . ? P3 C41 1.823(9) . ? P3 C31 1.830(8) . ? S2 C1 1.735(8) . ? O1 C3 1.467(8) . ? O2 C6 1.437(11) . ? N1 C1 1.337(10) . ? N2 C1 1.336(10) . ? N2 C2 1.446(11) . ? N2 H2 0.8800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.497(12) . ? C3 C5 1.521(13) . ? C3 C4' 1.528(17) . ? C3 C5' 1.57(11) . ? C3 H3 1.0000 . ? C3 H3' 1.0000 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C4' H4'1 0.9800 . ? C4' H4'2 0.9800 . ? C4' H4'3 0.9800 . ? C5' H5'1 0.9800 . ? C5' H5'2 0.9800 . ? C5' H5'3 0.9800 . ? C6 C7 1.495(19) . ? C6 C8 1.520(18) . ? C6 H6 1.0000 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C11 C16 1.375(12) . ? C11 C12 1.403(12) . ? C12 C13 1.397(12) . ? C12 H12 0.9500 . ? C13 C14 1.398(16) . ? C13 H13 0.9500 . ? C14 C15 1.350(16) . ? C14 H14 0.9500 . ? C15 C16 1.387(12) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C21 C22 1.398(12) . ? C21 C26 1.417(10) . ? C22 C23 1.381(13) . ? C22 H22 0.9500 . ? C23 C24 1.395(13) . ? C23 H23 0.9500 . ? C24 C25 1.359(14) . ? C24 H24 0.9500 . ? C25 C26 1.399(14) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C31 C32 1.380(12) . ? C31 C36 1.392(11) . ? C32 C33 1.387(13) . ? C32 H32 0.9500 . ? C33 C34 1.394(14) . ? C33 H33 0.9500 . ? C34 C35 1.385(16) . ? C34 H34 0.9500 . ? C35 C36 1.390(13) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C41 C42 1.385(11) . ? C41 C46 1.412(12) . ? C42 C43 1.354(13) . ? C42 H42 0.9500 . ? C43 C44 1.384(14) . ? C43 H43 0.9500 . ? C44 C45 1.428(15) . ? C44 H44 0.9500 . ? C45 C46 1.368(14) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C51 C52 1.432(12) . ? C51 C55 1.445(13) . ? C52 C53 1.422(13) . ? C52 H52 0.9500 . ? C53 C54 1.394(17) . ? C53 H53 0.9500 . ? C54 C55 1.460(14) . ? C54 H54 0.9500 . ? C55 H55 0.9500 . ? C61 C65 1.416(12) . ? C61 C62 1.444(12) . ? C62 C63 1.441(13) . ? C62 H62 0.9500 . ? C63 C64 1.432(16) . ? C63 H63 0.9500 . ? C64 C65 1.410(13) . ? C64 H64 0.9500 . ? C65 H65 0.9500 . ? 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 P2 Cu1 S2 113.73(7) . . ? P2 Cu1 P3 107.85(8) . . ? S2 Cu1 P3 117.51(8) . . ? P2 Cu1 S1 108.60(8) . . ? S2 Cu1 S1 106.69(8) . . ? P3 Cu1 S1 101.46(8) . . ? C53 Fe1 C65 164.0(4) . . ? C53 Fe1 C54 40.1(5) . . ? C65 Fe1 C54 130.0(5) . . ? C53 Fe1 C64 124.2(4) . . ? C65 Fe1 C64 40.4(4) . . ? C54 Fe1 C64 105.7(4) . . ? C53 Fe1 C52 40.9(4) . . ? C65 Fe1 C52 155.1(3) . . ? C54 Fe1 C52 68.2(4) . . ? C64 Fe1 C52 162.7(4) . . ? C53 Fe1 C63 102.6(4) . . ? C65 Fe1 C63 68.0(4) . . ? C54 Fe1 C63 113.0(4) . . ? C64 Fe1 C63 40.9(4) . . ? C52 Fe1 C63 125.0(4) . . ? C53 Fe1 C62 114.1(4) . . ? C65 Fe1 C62 67.9(4) . . ? C54 Fe1 C62 146.6(4) . . ? C64 Fe1 C62 68.9(4) . . ? C52 Fe1 C62 106.8(4) . . ? C63 Fe1 C62 41.1(4) . . ? C53 Fe1 C51 68.9(3) . . ? C65 Fe1 C51 123.0(3) . . ? C54 Fe1 C51 69.1(3) . . ? C64 Fe1 C51 154.1(4) . . ? C52 Fe1 C51 40.7(3) . . ? C63 Fe1 C51 164.9(5) . . ? C62 Fe1 C51 129.7(4) . . ? C53 Fe1 C55 68.7(4) . . ? C65 Fe1 C55 112.4(4) . . ? C54 Fe1 C55 41.5(4) . . ? C64 Fe1 C55 118.6(4) . . ? C52 Fe1 C55 68.3(4) . . ? C63 Fe1 C55 149.3(4) . . ? C62 Fe1 C55 169.5(3) . . ? C51 Fe1 C55 40.8(3) . . ? C53 Fe1 C61 150.3(4) . . ? C65 Fe1 C61 40.1(3) . . ? C54 Fe1 C61 169.6(4) . . ? C64 Fe1 C61 68.4(4) . . ? C52 Fe1 C61 120.0(4) . . ? C63 Fe1 C61 68.6(3) . . ? C62 Fe1 C61 40.7(3) . . ? C51 Fe1 C61 112.2(3) . . ? C55 Fe1 C61 132.8(4) . . ? O2 P1 O1 100.2(3) . . ? O2 P1 N1 111.5(3) . . ? O1 P1 N1 103.7(3) . . ? O2 P1 S1 107.9(2) . . ? O1 P1 S1 110.0(2) . . ? N1 P1 S1 121.5(3) . . ? C51 P2 C21 103.7(4) . . ? C51 P2 C11 102.1(4) . . ? C21 P2 C11 102.6(4) . . ? C51 P2 Cu1 111.2(3) . . ? C21 P2 Cu1 116.3(3) . . ? C11 P2 Cu1 119.0(3) . . ? C61 P3 C41 102.9(4) . . ? C61 P3 C31 102.0(3) . . ? C41 P3 C31 99.9(4) . . ? C61 P3 Cu1 114.5(3) . . ? C41 P3 Cu1 118.5(3) . . ? C31 P3 Cu1 116.5(3) . . ? P1 S1 Cu1 102.10(10) . . ? C1 S2 Cu1 104.6(2) . . ? C3 O1 P1 120.7(5) . . ? C6 O2 P1 120.3(6) . . ? C1 N1 P1 131.0(6) . . ? C1 N2 C2 125.2(7) . . ? C1 N2 H2 117.4 . . ? C2 N2 H2 117.4 . . ? N2 C1 N1 116.4(7) . . ? N2 C1 S2 116.0(6) . . ? N1 C1 S2 127.6(6) . . ? N2 C2 H2A 109.5 . . ? N2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O1 C3 C4 111.5(7) . . ? O1 C3 C5 106.1(7) . . ? C4 C3 C5 115.5(10) . . ? O1 C3 C4' 107.1(12) . . ? O1 C3 C5' 106(6) . . ? C4' C3 C5' 139(3) . . ? O1 C3 H3 107.8 . . ? C4 C3 H3 107.8 . . ? C5 C3 H3 107.8 . . ? C4' C3 H3 135.2 . . ? C5' C3 H3 51.9 . . ? O1 C3 H3' 99.5 . . ? C4 C3 H3' 67.8 . . ? C5 C3 H3' 149.8 . . ? C4' C3 H3' 99.5 . . ? C5' C3 H3' 99.5 . . ? H3 C3 H3' 47.6 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C4' H4'1 109.5 . . ? C3 C4' H4'2 109.5 . . ? H4'1 C4' H4'2 109.5 . . ? C3 C4' H4'3 109.5 . . ? H4'1 C4' H4'3 109.5 . . ? H4'2 C4' H4'3 109.5 . . ? C3 C5' H5'1 109.5 . . ? C3 C5' H5'2 109.5 . . ? H5'1 C5' H5'2 109.5 . . ? C3 C5' H5'3 109.5 . . ? H5'1 C5' H5'3 109.5 . . ? H5'2 C5' H5'3 109.5 . . ? O2 C6 C7 108.9(10) . . ? O2 C6 C8 105.2(10) . . ? C7 C6 C8 111.6(11) . . ? O2 C6 H6 110.3 . . ? C7 C6 H6 110.3 . . ? C8 C6 H6 110.3 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C16 C11 C12 119.9(8) . . ? C16 C11 P2 118.3(6) . . ? C12 C11 P2 121.7(7) . . ? C13 C12 C11 119.4(10) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C12 C13 C14 119.6(9) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C15 C14 C13 119.4(8) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C14 C15 C16 122.2(10) . . ? C14 C15 H15 118.9 . . ? C16 C15 H15 118.9 . . ? C11 C16 C15 119.3(9) . . ? C11 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C22 C21 C26 116.3(8) . . ? C22 C21 P2 120.6(6) . . ? C26 C21 P2 123.0(7) . . ? C23 C22 C21 122.8(7) . . ? C23 C22 H22 118.6 . . ? C21 C22 H22 118.6 . . ? C22 C23 C24 119.2(9) . . ? C22 C23 H23 120.4 . . ? C24 C23 H23 120.4 . . ? C25 C24 C23 120.2(9) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C26 120.9(8) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C25 C26 C21 120.6(9) . . ? C25 C26 H26 119.7 . . ? C21 C26 H26 119.7 . . ? C32 C31 C36 118.8(7) . . ? C32 C31 P3 117.5(6) . . ? C36 C31 P3 123.6(7) . . ? C31 C32 C33 122.1(8) . . ? C31 C32 H32 118.9 . . ? C33 C32 H32 118.9 . . ? C32 C33 C34 118.7(9) . . ? C32 C33 H33 120.7 . . ? C34 C33 H33 120.7 . . ? C35 C34 C33 119.8(8) . . ? C35 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? C34 C35 C36 120.8(8) . . ? C34 C35 H35 119.6 . . ? C36 C35 H35 119.6 . . ? C35 C36 C31 119.8(9) . . ? C35 C36 H36 120.1 . . ? C31 C36 H36 120.1 . . ? C42 C41 C46 117.8(8) . . ? C42 C41 P3 119.8(6) . . ? C46 C41 P3 122.4(6) . . ? C43 C42 C41 121.9(8) . . ? C43 C42 H42 119.1 . . ? C41 C42 H42 119.1 . . ? C42 C43 C44 121.5(9) . . ? C42 C43 H43 119.2 . . ? C44 C43 H43 119.2 . . ? C43 C44 C45 117.8(9) . . ? C43 C44 H44 121.1 . . ? C45 C44 H44 121.1 . . ? C46 C45 C44 120.1(9) . . ? C46 C45 H45 119.9 . . ? C44 C45 H45 119.9 . . ? C45 C46 C41 120.9(8) . . ? C45 C46 H46 119.6 . . ? C41 C46 H46 119.6 . . ? C52 C51 C55 107.2(8) . . ? C52 C51 P2 123.6(7) . . ? C55 C51 P2 129.2(7) . . ? C52 C51 Fe1 68.7(5) . . ? C55 C51 Fe1 69.8(5) . . ? P2 C51 Fe1 127.2(4) . . ? C53 C52 C51 108.7(9) . . ? C53 C52 Fe1 68.8(6) . . ? C51 C52 Fe1 70.6(5) . . ? C53 C52 H52 125.6 . . ? C51 C52 H52 125.6 . . ? Fe1 C52 H52 126.5 . . ? C54 C53 C52 108.9(9) . . ? C54 C53 Fe1 70.5(6) . . ? C52 C53 Fe1 70.3(5) . . ? C54 C53 H53 125.6 . . ? C52 C53 H53 125.6 . . ? Fe1 C53 H53 125.1 . . ? C53 C54 C55 108.5(9) . . ? C53 C54 Fe1 69.4(5) . . ? C55 C54 Fe1 70.6(5) . . ? C53 C54 H54 125.8 . . ? C55 C54 H54 125.8 . . ? Fe1 C54 H54 125.8 . . ? C51 C55 C54 106.8(9) . . ? C51 C55 Fe1 69.4(5) . . ? C54 C55 Fe1 67.9(5) . . ? C51 C55 H55 126.6 . . ? C54 C55 H55 126.6 . . ? Fe1 C55 H55 127.6 . . ? C65 C61 C62 106.2(8) . . ? C65 C61 P3 129.9(6) . . ? C62 C61 P3 123.9(7) . . ? C65 C61 Fe1 68.0(5) . . ? C62 C61 Fe1 68.4(5) . . ? P3 C61 Fe1 127.0(4) . . ? C63 C62 C61 108.1(9) . . ? C63 C62 Fe1 69.2(5) . . ? C61 C62 Fe1 70.9(4) . . ? C63 C62 H62 126.0 . . ? C61 C62 H62 126.0 . . ? Fe1 C62 H62 125.5 . . ? C64 C63 C62 107.8(8) . . ? C64 C63 Fe1 69.3(5) . . ? C62 C63 Fe1 69.7(5) . . ? C64 C63 H63 126.1 . . ? C62 C63 H63 126.1 . . ? Fe1 C63 H63 126.4 . . ? C65 C64 C63 107.1(8) . . ? C65 C64 Fe1 69.6(5) . . ? C63 C64 Fe1 69.7(5) . . ? C65 C64 H64 126.4 . . ? C63 C64 H64 126.4 . . ? Fe1 C64 H64 125.8 . . ? C64 C65 C61 110.8(9) . . ? C64 C65 Fe1 70.0(6) . . ? C61 C65 Fe1 71.9(5) . . ? C64 C65 H65 124.6 . . ? C61 C65 H65 124.6 . . ? Fe1 C65 H65 125.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S2 Cu1 P2 C51 -177.4(3) . . . . ? P3 Cu1 P2 C51 50.4(3) . . . . ? S1 Cu1 P2 C51 -58.8(3) . . . . ? S2 Cu1 P2 C21 64.3(3) . . . . ? P3 Cu1 P2 C21 -67.9(3) . . . . ? S1 Cu1 P2 C21 -177.1(3) . . . . ? S2 Cu1 P2 C11 -59.2(3) . . . . ? P3 Cu1 P2 C11 168.6(3) . . . . ? S1 Cu1 P2 C11 59.4(3) . . . . ? P2 Cu1 P3 C61 -39.0(3) . . . . ? S2 Cu1 P3 C61 -169.1(3) . . . . ? S1 Cu1 P3 C61 75.1(3) . . . . ? P2 Cu1 P3 C41 82.8(3) . . . . ? S2 Cu1 P3 C41 -47.3(3) . . . . ? S1 Cu1 P3 C41 -163.2(3) . . . . ? P2 Cu1 P3 C31 -157.8(3) . . . . ? S2 Cu1 P3 C31 72.1(3) . . . . ? S1 Cu1 P3 C31 -43.7(3) . . . . ? O2 P1 S1 Cu1 101.7(3) . . . . ? O1 P1 S1 Cu1 -150.0(2) . . . . ? N1 P1 S1 Cu1 -28.8(3) . . . . ? P2 Cu1 S1 P1 -132.37(10) . . . . ? S2 Cu1 S1 P1 -9.40(12) . . . . ? P3 Cu1 S1 P1 114.16(11) . . . . ? P2 Cu1 S2 C1 159.9(3) . . . . ? P3 Cu1 S2 C1 -72.8(3) . . . . ? S1 Cu1 S2 C1 40.2(3) . . . . ? O2 P1 O1 C3 -167.1(5) . . . . ? N1 P1 O1 C3 -51.9(6) . . . . ? S1 P1 O1 C3 79.4(5) . . . . ? O1 P1 O2 C6 63.5(8) . . . . ? N1 P1 O2 C6 -45.7(8) . . . . ? S1 P1 O2 C6 178.5(7) . . . . ? O2 P1 N1 C1 -84.6(7) . . . . ? O1 P1 N1 C1 168.5(6) . . . . ? S1 P1 N1 C1 44.4(8) . . . . ? C2 N2 C1 N1 0.4(11) . . . . ? C2 N2 C1 S2 179.4(7) . . . . ? P1 N1 C1 N2 -177.6(6) . . . . ? P1 N1 C1 S2 3.4(10) . . . . ? Cu1 S2 C1 N2 135.6(5) . . . . ? Cu1 S2 C1 N1 -45.5(7) . . . . ? P1 O1 C3 C4 -94.8(9) . . . . ? P1 O1 C3 C5 138.7(8) . . . . ? P1 O1 C3 C4' -128(2) . . . . ? P1 O1 C3 C5' 78(4) . . . . ? P1 O2 C6 C7 -112.7(10) . . . . ? P1 O2 C6 C8 127.6(8) . . . . ? C51 P2 C11 C16 150.8(7) . . . . ? C21 P2 C11 C16 -102.0(7) . . . . ? Cu1 P2 C11 C16 28.1(8) . . . . ? C51 P2 C11 C12 -32.7(8) . . . . ? C21 P2 C11 C12 74.5(8) . . . . ? Cu1 P2 C11 C12 -155.5(6) . . . . ? C16 C11 C12 C13 -2.1(13) . . . . ? P2 C11 C12 C13 -178.5(7) . . . . ? C11 C12 C13 C14 4.1(14) . . . . ? C12 C13 C14 C15 -3.5(15) . . . . ? C13 C14 C15 C16 0.9(16) . . . . ? C12 C11 C16 C15 -0.5(13) . . . . ? P2 C11 C16 C15 176.0(7) . . . . ? C14 C15 C16 C11 1.1(14) . . . . ? C51 P2 C21 C22 -68.3(7) . . . . ? C11 P2 C21 C22 -174.3(7) . . . . ? Cu1 P2 C21 C22 54.0(7) . . . . ? C51 P2 C21 C26 114.3(7) . . . . ? C11 P2 C21 C26 8.2(8) . . . . ? Cu1 P2 C21 C26 -123.4(6) . . . . ? C26 C21 C22 C23 1.0(13) . . . . ? P2 C21 C22 C23 -176.6(7) . . . . ? C21 C22 C23 C24 -1.3(14) . . . . ? C22 C23 C24 C25 1.3(15) . . . . ? C23 C24 C25 C26 -0.9(15) . . . . ? C24 C25 C26 C21 0.6(15) . . . . ? C22 C21 C26 C25 -0.6(13) . . . . ? P2 C21 C26 C25 177.0(7) . . . . ? C61 P3 C31 C32 -163.5(7) . . . . ? C41 P3 C31 C32 90.9(7) . . . . ? Cu1 P3 C31 C32 -38.1(7) . . . . ? C61 P3 C31 C36 19.1(9) . . . . ? C41 P3 C31 C36 -86.5(8) . . . . ? Cu1 P3 C31 C36 144.4(7) . . . . ? C36 C31 C32 C33 1.0(14) . . . . ? P3 C31 C32 C33 -176.6(8) . . . . ? C31 C32 C33 C34 -1.8(15) . . . . ? C32 C33 C34 C35 1.2(15) . . . . ? C33 C34 C35 C36 0.1(16) . . . . ? C34 C35 C36 C31 -0.9(16) . . . . ? C32 C31 C36 C35 0.4(14) . . . . ? P3 C31 C36 C35 177.8(8) . . . . ? C61 P3 C41 C42 138.7(7) . . . . ? C31 P3 C41 C42 -116.5(7) . . . . ? Cu1 P3 C41 C42 11.2(8) . . . . ? C61 P3 C41 C46 -42.7(8) . . . . ? C31 P3 C41 C46 62.1(8) . . . . ? Cu1 P3 C41 C46 -170.2(6) . . . . ? C46 C41 C42 C43 -1.6(13) . . . . ? P3 C41 C42 C43 177.1(7) . . . . ? C41 C42 C43 C44 1.8(15) . . . . ? C42 C43 C44 C45 -1.5(15) . . . . ? C43 C44 C45 C46 1.1(16) . . . . ? C44 C45 C46 C41 -1.0(16) . . . . ? C42 C41 C46 C45 1.2(14) . . . . ? P3 C41 C46 C45 -177.4(8) . . . . ? C21 P2 C51 C52 176.8(6) . . . . ? C11 P2 C51 C52 -76.9(7) . . . . ? Cu1 P2 C51 C52 51.1(7) . . . . ? C21 P2 C51 C55 -4.3(8) . . . . ? C11 P2 C51 C55 102.1(8) . . . . ? Cu1 P2 C51 C55 -130.0(7) . . . . ? C21 P2 C51 Fe1 89.2(6) . . . . ? C11 P2 C51 Fe1 -164.4(6) . . . . ? Cu1 P2 C51 Fe1 -36.4(7) . . . . ? C53 Fe1 C51 C52 37.4(6) . . . . ? C65 Fe1 C51 C52 -154.6(5) . . . . ? C54 Fe1 C51 C52 80.4(6) . . . . ? C64 Fe1 C51 C52 163.2(8) . . . . ? C63 Fe1 C51 C52 -20.5(16) . . . . ? C62 Fe1 C51 C52 -67.1(6) . . . . ? C55 Fe1 C51 C52 118.8(8) . . . . ? C61 Fe1 C51 C52 -110.7(5) . . . . ? C53 Fe1 C51 C55 -81.4(7) . . . . ? C65 Fe1 C51 C55 86.6(7) . . . . ? C54 Fe1 C51 C55 -38.3(7) . . . . ? C64 Fe1 C51 C55 44.5(10) . . . . ? C52 Fe1 C51 C55 -118.8(8) . . . . ? C63 Fe1 C51 C55 -139.3(14) . . . . ? C62 Fe1 C51 C55 174.1(6) . . . . ? C61 Fe1 C51 C55 130.6(6) . . . . ? C53 Fe1 C51 P2 154.1(8) . . . . ? C65 Fe1 C51 P2 -37.9(8) . . . . ? C54 Fe1 C51 P2 -162.9(8) . . . . ? C64 Fe1 C51 P2 -80.1(10) . . . . ? C52 Fe1 C51 P2 116.7(8) . . . . ? C63 Fe1 C51 P2 96.2(14) . . . . ? C62 Fe1 C51 P2 49.6(8) . . . . ? C55 Fe1 C51 P2 -124.5(9) . . . . ? C61 Fe1 C51 P2 6.0(7) . . . . ? C55 C51 C52 C53 1.1(9) . . . . ? P2 C51 C52 C53 -179.7(6) . . . . ? Fe1 C51 C52 C53 -58.4(6) . . . . ? C55 C51 C52 Fe1 59.5(6) . . . . ? P2 C51 C52 Fe1 -121.4(6) . . . . ? C65 Fe1 C52 C53 178.8(8) . . . . ? C54 Fe1 C52 C53 37.2(6) . . . . ? C64 Fe1 C52 C53 -34.8(16) . . . . ? C63 Fe1 C52 C53 -66.3(7) . . . . ? C62 Fe1 C52 C53 -107.7(6) . . . . ? C51 Fe1 C52 C53 120.1(8) . . . . ? C55 Fe1 C52 C53 82.1(6) . . . . ? C61 Fe1 C52 C53 -150.0(6) . . . . ? C53 Fe1 C52 C51 -120.1(8) . . . . ? C65 Fe1 C52 C51 58.7(11) . . . . ? C54 Fe1 C52 C51 -82.9(6) . . . . ? C64 Fe1 C52 C51 -154.9(12) . . . . ? C63 Fe1 C52 C51 173.6(5) . . . . ? C62 Fe1 C52 C51 132.2(5) . . . . ? C55 Fe1 C52 C51 -38.0(5) . . . . ? C61 Fe1 C52 C51 89.9(6) . . . . ? C51 C52 C53 C54 -0.8(10) . . . . ? Fe1 C52 C53 C54 -60.3(7) . . . . ? C51 C52 C53 Fe1 59.5(6) . . . . ? C65 Fe1 C53 C54 -58.8(16) . . . . ? C64 Fe1 C53 C54 -72.5(7) . . . . ? C52 Fe1 C53 C54 119.3(8) . . . . ? C63 Fe1 C53 C54 -110.9(6) . . . . ? C62 Fe1 C53 C54 -152.6(5) . . . . ? C51 Fe1 C53 C54 82.2(6) . . . . ? C55 Fe1 C53 C54 38.3(5) . . . . ? C61 Fe1 C53 C54 -179.7(6) . . . . ? C65 Fe1 C53 C52 -178.1(12) . . . . ? C54 Fe1 C53 C52 -119.3(8) . . . . ? C64 Fe1 C53 C52 168.1(6) . . . . ? C63 Fe1 C53 C52 129.8(6) . . . . ? C62 Fe1 C53 C52 88.0(6) . . . . ? C51 Fe1 C53 C52 -37.2(5) . . . . ? C55 Fe1 C53 C52 -81.0(6) . . . . ? C61 Fe1 C53 C52 61.0(9) . . . . ? C52 C53 C54 C55 0.1(11) . . . . ? Fe1 C53 C54 C55 -60.0(7) . . . . ? C52 C53 C54 Fe1 60.2(6) . . . . ? C65 Fe1 C54 C53 162.1(5) . . . . ? C64 Fe1 C54 C53 125.0(6) . . . . ? C52 Fe1 C54 C53 -37.9(5) . . . . ? C63 Fe1 C54 C53 82.1(7) . . . . ? C62 Fe1 C54 C53 49.6(10) . . . . ? C51 Fe1 C54 C53 -81.8(6) . . . . ? C55 Fe1 C54 C53 -119.4(9) . . . . ? C61 Fe1 C54 C53 179.1(15) . . . . ? C53 Fe1 C54 C55 119.4(9) . . . . ? C65 Fe1 C54 C55 -78.5(7) . . . . ? C64 Fe1 C54 C55 -115.6(6) . . . . ? C52 Fe1 C54 C55 81.5(6) . . . . ? C63 Fe1 C54 C55 -158.4(6) . . . . ? C62 Fe1 C54 C55 169.1(7) . . . . ? C51 Fe1 C54 C55 37.6(6) . . . . ? C61 Fe1 C54 C55 -61.5(19) . . . . ? C52 C51 C55 C54 -1.0(9) . . . . ? P2 C51 C55 C54 179.9(6) . . . . ? Fe1 C51 C55 C54 57.8(6) . . . . ? C52 C51 C55 Fe1 -58.7(5) . . . . ? P2 C51 C55 Fe1 122.2(7) . . . . ? C53 C54 C55 C51 0.5(11) . . . . ? Fe1 C54 C55 C51 -58.7(6) . . . . ? C53 C54 C55 Fe1 59.3(7) . . . . ? C53 Fe1 C55 C51 82.1(6) . . . . ? C65 Fe1 C55 C51 -115.2(6) . . . . ? C54 Fe1 C55 C51 119.1(9) . . . . ? C64 Fe1 C55 C51 -159.6(5) . . . . ? C52 Fe1 C55 C51 38.0(5) . . . . ? C63 Fe1 C55 C51 160.6(8) . . . . ? C62 Fe1 C55 C51 -26(3) . . . . ? C61 Fe1 C55 C51 -73.4(7) . . . . ? C53 Fe1 C55 C54 -37.0(7) . . . . ? C65 Fe1 C55 C54 125.8(7) . . . . ? C64 Fe1 C55 C54 81.3(8) . . . . ? C52 Fe1 C55 C54 -81.1(7) . . . . ? C63 Fe1 C55 C54 41.5(12) . . . . ? C62 Fe1 C55 C54 -145(2) . . . . ? C51 Fe1 C55 C54 -119.1(9) . . . . ? C61 Fe1 C55 C54 167.5(6) . . . . ? C41 P3 C61 C65 -27.9(8) . . . . ? C31 P3 C61 C65 -131.2(7) . . . . ? Cu1 P3 C61 C65 102.1(7) . . . . ? C41 P3 C61 C62 153.9(7) . . . . ? C31 P3 C61 C62 50.6(7) . . . . ? Cu1 P3 C61 C62 -76.1(7) . . . . ? C41 P3 C61 Fe1 -118.9(5) . . . . ? C31 P3 C61 Fe1 137.8(5) . . . . ? Cu1 P3 C61 Fe1 11.1(6) . . . . ? C53 Fe1 C61 C65 158.4(7) . . . . ? C54 Fe1 C61 C65 -20.4(19) . . . . ? C64 Fe1 C61 C65 36.6(5) . . . . ? C52 Fe1 C61 C65 -160.2(5) . . . . ? C63 Fe1 C61 C65 80.8(6) . . . . ? C62 Fe1 C61 C65 118.9(7) . . . . ? C51 Fe1 C61 C65 -115.4(5) . . . . ? C55 Fe1 C61 C65 -72.9(6) . . . . ? C53 Fe1 C61 C62 39.5(9) . . . . ? C65 Fe1 C61 C62 -118.9(7) . . . . ? C54 Fe1 C61 C62 -139.3(17) . . . . ? C64 Fe1 C61 C62 -82.3(6) . . . . ? C52 Fe1 C61 C62 80.8(6) . . . . ? C63 Fe1 C61 C62 -38.2(6) . . . . ? C51 Fe1 C61 C62 125.6(6) . . . . ? C55 Fe1 C61 C62 168.1(6) . . . . ? C53 Fe1 C61 P3 -77.5(8) . . . . ? C65 Fe1 C61 P3 124.1(7) . . . . ? C54 Fe1 C61 P3 103.8(18) . . . . ? C64 Fe1 C61 P3 160.7(7) . . . . ? C52 Fe1 C61 P3 -36.1(7) . . . . ? C63 Fe1 C61 P3 -155.1(7) . . . . ? C62 Fe1 C61 P3 -116.9(8) . . . . ? C51 Fe1 C61 P3 8.7(7) . . . . ? C55 Fe1 C61 P3 51.2(8) . . . . ? C65 C61 C62 C63 1.8(9) . . . . ? P3 C61 C62 C63 -179.6(6) . . . . ? Fe1 C61 C62 C63 59.5(6) . . . . ? C65 C61 C62 Fe1 -57.6(5) . . . . ? P3 C61 C62 Fe1 120.9(6) . . . . ? C53 Fe1 C62 C63 81.3(8) . . . . ? C65 Fe1 C62 C63 -81.4(7) . . . . ? C54 Fe1 C62 C63 48.8(11) . . . . ? C64 Fe1 C62 C63 -37.8(7) . . . . ? C52 Fe1 C62 C63 124.4(7) . . . . ? C51 Fe1 C62 C63 163.3(7) . . . . ? C55 Fe1 C62 C63 -175(2) . . . . ? C61 Fe1 C62 C63 -118.8(9) . . . . ? C53 Fe1 C62 C61 -159.8(5) . . . . ? C65 Fe1 C62 C61 37.5(5) . . . . ? C54 Fe1 C62 C61 167.7(7) . . . . ? C64 Fe1 C62 C61 81.0(6) . . . . ? C52 Fe1 C62 C61 -116.7(5) . . . . ? C63 Fe1 C62 C61 118.8(9) . . . . ? C51 Fe1 C62 C61 -77.9(7) . . . . ? C55 Fe1 C62 C61 -56(3) . . . . ? C61 C62 C63 C64 -1.4(10) . . . . ? Fe1 C62 C63 C64 59.1(6) . . . . ? C61 C62 C63 Fe1 -60.5(6) . . . . ? C53 Fe1 C63 C64 128.4(6) . . . . ? C65 Fe1 C63 C64 -38.0(6) . . . . ? C54 Fe1 C63 C64 87.6(7) . . . . ? C52 Fe1 C63 C64 166.3(5) . . . . ? C62 Fe1 C63 C64 -119.2(9) . . . . ? C51 Fe1 C63 C64 -177.5(12) . . . . ? C55 Fe1 C63 C64 59.1(11) . . . . ? C61 Fe1 C63 C64 -81.3(6) . . . . ? C53 Fe1 C63 C62 -112.4(7) . . . . ? C65 Fe1 C63 C62 81.2(6) . . . . ? C54 Fe1 C63 C62 -153.2(7) . . . . ? C64 Fe1 C63 C62 119.2(9) . . . . ? C52 Fe1 C63 C62 -74.5(7) . . . . ? C51 Fe1 C63 C62 -58.3(16) . . . . ? C55 Fe1 C63 C62 178.3(8) . . . . ? C61 Fe1 C63 C62 37.9(6) . . . . ? C62 C63 C64 C65 0.5(10) . . . . ? Fe1 C63 C64 C65 59.8(6) . . . . ? C62 C63 C64 Fe1 -59.3(6) . . . . ? C53 Fe1 C64 C65 174.2(6) . . . . ? C54 Fe1 C64 C65 134.6(6) . . . . ? C52 Fe1 C64 C65 -158.9(12) . . . . ? C63 Fe1 C64 C65 -118.2(8) . . . . ? C62 Fe1 C64 C65 -80.3(6) . . . . ? C51 Fe1 C64 C65 60.3(10) . . . . ? C55 Fe1 C64 C65 91.7(6) . . . . ? C61 Fe1 C64 C65 -36.4(5) . . . . ? C53 Fe1 C64 C63 -67.6(7) . . . . ? C65 Fe1 C64 C63 118.2(8) . . . . ? C54 Fe1 C64 C63 -107.2(6) . . . . ? C52 Fe1 C64 C63 -40.7(15) . . . . ? C62 Fe1 C64 C63 37.9(5) . . . . ? C51 Fe1 C64 C63 178.5(7) . . . . ? C55 Fe1 C64 C63 -150.1(6) . . . . ? C61 Fe1 C64 C63 81.8(6) . . . . ? C63 C64 C65 C61 0.7(10) . . . . ? Fe1 C64 C65 C61 60.6(6) . . . . ? C63 C64 C65 Fe1 -59.9(6) . . . . ? C62 C61 C65 C64 -1.6(9) . . . . ? P3 C61 C65 C64 180.0(6) . . . . ? Fe1 C61 C65 C64 -59.5(6) . . . . ? C62 C61 C65 Fe1 57.9(5) . . . . ? P3 C61 C65 Fe1 -120.5(6) . . . . ? C53 Fe1 C65 C64 -17.6(17) . . . . ? C54 Fe1 C65 C64 -63.6(7) . . . . ? C52 Fe1 C65 C64 165.3(8) . . . . ? C63 Fe1 C65 C64 38.5(6) . . . . ? C62 Fe1 C65 C64 83.0(6) . . . . ? C51 Fe1 C65 C64 -153.1(6) . . . . ? C55 Fe1 C65 C64 -108.3(6) . . . . ? C61 Fe1 C65 C64 121.1(7) . . . . ? C53 Fe1 C65 C61 -138.7(14) . . . . ? C54 Fe1 C65 C61 175.3(4) . . . . ? C64 Fe1 C65 C61 -121.1(7) . . . . ? C52 Fe1 C65 C61 44.2(10) . . . . ? C63 Fe1 C65 C61 -82.5(5) . . . . ? C62 Fe1 C65 C61 -38.0(4) . . . . ? C51 Fe1 C65 C61 85.8(5) . . . . ? C55 Fe1 C65 C61 130.7(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2 S2 0.88 2.69 3.550(7) 167.3 2_766 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.562 _refine_diff_density_min -1.507 _refine_diff_density_rms 0.173 # Attachment '- 7.cif' data_safin47 _database_code_depnum_ccdc_archive 'CCDC 749079' #TrackingRef '- 7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C50 H52 Cu N2 O2 P3 S2), C2 H4 Cl4, C H2 Cl2' _chemical_formula_sum 'C103 H110 Cl6 Cu2 N4 O4 P6 S4' _chemical_formula_weight 2121.80 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.7676(7) _cell_length_b 13.8533(8) _cell_length_c 16.8992(8) _cell_angle_alpha 67.726(4) _cell_angle_beta 66.131(4) _cell_angle_gamma 63.955(4) _cell_volume 2567.4(2) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 23129 _cell_measurement_theta_min 3.4 _cell_measurement_theta_max 25.9 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.43 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.372 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1102 _exptl_absorpt_coefficient_mu 0.798 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7154 _exptl_absorpt_correction_T_max 0.7255 _exptl_absorpt_process_details 'MULABS (Spek, 2003; Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS II two-circle-diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 27475 _diffrn_reflns_av_R_equivalents 0.0611 _diffrn_reflns_av_sigmaI/netI 0.0608 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.32 _diffrn_reflns_theta_max 25.62 _reflns_number_total 9580 _reflns_number_gt 7135 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'X-Area (Stoe & Cie, 2001)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2001)' _computing_data_reduction 'X-Area (Stoe & Cie, 2001)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008) ' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008) ' _computing_molecular_graphics 'XP in SHELXTL-Plus (Sheldrick, 1991)' _computing_publication_material SHELXL97 _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^)+(0.1594P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9580 _refine_ls_number_parameters 580 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0755 _refine_ls_R_factor_gt 0.0581 _refine_ls_wR_factor_ref 0.1776 _refine_ls_wR_factor_gt 0.1652 _refine_ls_goodness_of_fit_ref 0.828 _refine_ls_restrained_S_all 0.828 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.55297(3) 0.69490(3) 0.24409(3) 0.02562(14) Uani 1 1 d . . . P1 P 0.47075(8) 0.89868(7) 0.34137(7) 0.0323(2) Uani 1 1 d . . . P2 P 0.72528(7) 0.62894(8) 0.14865(6) 0.0283(2) Uani 1 1 d . . . P3 P 0.40937(7) 0.67565(7) 0.22010(6) 0.0268(2) Uani 1 1 d . . . S1 S 0.50355(8) 0.88823(8) 0.21961(7) 0.0378(2) Uani 1 1 d . A . S2 S 0.57127(7) 0.62088(7) 0.38815(6) 0.0268(2) Uani 1 1 d . A . O1 O 0.3860(2) 1.0188(2) 0.3524(2) 0.0381(6) Uani 1 1 d . A . C2 C 0.2720(3) 1.0541(3) 0.3468(3) 0.0339(8) Uani 1 1 d . . . H2A H 0.2679 1.0003 0.3231 0.041 Uiso 1 1 calc R A . C3 C 0.1894(4) 1.0554(4) 0.4384(3) 0.0573(13) Uani 1 1 d . A . H3A H 0.2075 0.9807 0.4777 0.086 Uiso 1 1 calc R . . H3B H 0.1127 1.0799 0.4344 0.086 Uiso 1 1 calc R . . H3C H 0.1943 1.1065 0.4628 0.086 Uiso 1 1 calc R . . C4 C 0.2501(4) 1.1657(3) 0.2819(3) 0.0439(10) Uani 1 1 d . A . H4A H 0.3062 1.1600 0.2238 0.066 Uiso 1 1 calc R . . H4B H 0.2554 1.2187 0.3041 0.066 Uiso 1 1 calc R . . H4C H 0.1744 1.1913 0.2756 0.066 Uiso 1 1 calc R . . O2 O 0.5904(4) 0.8978(4) 0.3373(4) 0.0323(13) Uiso 0.577(8) 1 d P A 1 C5 C 0.6091(7) 0.8968(7) 0.4146(6) 0.051(2) Uiso 0.577(8) 1 d P A 1 H5 H 0.5524 0.8710 0.4691 0.061 Uiso 0.577(8) 1 calc PR A 1 C6 C 0.5967(10) 1.0122(10) 0.4101(8) 0.080(3) Uiso 0.577(8) 1 d P A 1 H6A H 0.5196 1.0617 0.4096 0.120 Uiso 0.577(8) 1 calc PR A 1 H6B H 0.6503 1.0386 0.3554 0.120 Uiso 0.577(8) 1 calc PR A 1 H6C H 0.6121 1.0113 0.4621 0.120 Uiso 0.577(8) 1 calc PR A 1 C7 C 0.7245(8) 0.8156(9) 0.4157(7) 0.066(3) Uiso 0.577(8) 1 d P A 1 H7A H 0.7272 0.7419 0.4201 0.098 Uiso 0.577(8) 1 calc PR A 1 H7B H 0.7423 0.8133 0.4671 0.098 Uiso 0.577(8) 1 calc PR A 1 H7C H 0.7797 0.8383 0.3605 0.098 Uiso 0.577(8) 1 calc PR A 1 O2' O 0.5605(5) 0.8903(5) 0.3825(5) 0.0265(16) Uiso 0.423(8) 1 d P A 2 C5' C 0.6506(9) 0.9366(9) 0.3230(7) 0.042(3) Uiso 0.423(8) 1 d P A 2 H5' H 0.6769 0.9224 0.2627 0.051 Uiso 0.423(8) 1 calc PR A 2 C6' C 0.6049(13) 1.0591(12) 0.3161(10) 0.069(4) Uiso 0.423(8) 1 d P A 2 H6'1 H 0.5469 1.0953 0.2847 0.104 Uiso 0.423(8) 1 calc PR A 2 H6'2 H 0.6663 1.0898 0.2831 0.104 Uiso 0.423(8) 1 calc PR A 2 H6'3 H 0.5717 1.0721 0.3761 0.104 Uiso 0.423(8) 1 calc PR A 2 C7' C 0.7440(13) 0.8753(14) 0.3673(11) 0.074(4) Uiso 0.423(8) 1 d P A 2 H7'1 H 0.7710 0.7962 0.3698 0.111 Uiso 0.423(8) 1 calc PR A 2 H7'2 H 0.7155 0.8853 0.4280 0.111 Uiso 0.423(8) 1 calc PR A 2 H7'3 H 0.8064 0.9045 0.3329 0.111 Uiso 0.423(8) 1 calc PR A 2 N1 N 0.4137(3) 0.8168(2) 0.4247(2) 0.0304(7) Uani 1 1 d . A . N2 N 0.3846(3) 0.6568(3) 0.5191(2) 0.0309(7) Uani 1 1 d . A . H2 H 0.401(4) 0.586(4) 0.530(3) 0.047(13) Uiso 1 1 d . . . C1 C 0.4486(3) 0.7083(3) 0.4456(2) 0.0256(7) Uani 1 1 d . . . C11 C 0.2792(3) 0.7130(3) 0.5745(3) 0.0352(9) Uani 1 1 d . . . C12 C 0.1829(3) 0.6912(4) 0.5881(3) 0.0477(11) Uani 1 1 d . A . C13 C 0.0823(4) 0.7497(4) 0.6416(4) 0.0686(18) Uani 1 1 d . . . H13 H 0.0149 0.7379 0.6514 0.082 Uiso 1 1 calc R A . C14 C 0.0763(5) 0.8229(5) 0.6805(4) 0.0699(18) Uani 1 1 d . A . H14 H 0.0058 0.8615 0.7159 0.084 Uiso 1 1 calc R . . C15 C 0.1735(5) 0.8408(4) 0.6679(3) 0.0616(15) Uani 1 1 d . . . H15 H 0.1705 0.8906 0.6956 0.074 Uiso 1 1 calc R A . C16 C 0.2753(4) 0.7852(4) 0.6146(3) 0.0468(10) Uani 1 1 d . A . H16 H 0.3424 0.7969 0.6058 0.056 Uiso 1 1 calc R . . C17 C 0.1854(4) 0.6114(4) 0.5472(4) 0.0616(15) Uani 1 1 d . . . H17A H 0.2441 0.6107 0.4897 0.092 Uiso 1 1 calc R A . H17B H 0.1119 0.6341 0.5378 0.092 Uiso 1 1 calc R . . H17C H 0.2020 0.5370 0.5871 0.092 Uiso 1 1 calc R . . C21 C 0.8459(3) 0.5793(3) 0.1916(3) 0.0353(9) Uani 1 1 d . . . C22 C 0.8439(4) 0.6424(4) 0.2396(3) 0.0476(11) Uani 1 1 d . . . H22 H 0.7796 0.7054 0.2523 0.057 Uiso 1 1 calc R . . C23 C 0.9366(4) 0.6134(5) 0.2694(4) 0.0628(14) Uani 1 1 d . . . H23 H 0.9358 0.6576 0.3011 0.075 Uiso 1 1 calc R . . C24 C 1.0284(4) 0.5210(6) 0.2527(4) 0.0707(18) Uani 1 1 d . . . H24 H 1.0910 0.5011 0.2734 0.085 Uiso 1 1 calc R . . C25 C 1.0303(4) 0.4572(5) 0.2064(4) 0.0652(17) Uani 1 1 d . . . H25 H 1.0944 0.3934 0.1951 0.078 Uiso 1 1 calc R . . C26 C 0.9389(3) 0.4853(4) 0.1757(3) 0.0464(11) Uani 1 1 d . . . H26 H 0.9402 0.4404 0.1442 0.056 Uiso 1 1 calc R . . C31 C 0.7642(3) 0.7290(3) 0.0446(2) 0.0308(8) Uani 1 1 d . . . C32 C 0.6785(3) 0.8108(3) 0.0074(3) 0.0390(9) Uani 1 1 d . . . H32 H 0.6026 0.8128 0.0363 0.047 Uiso 1 1 calc R . . C33 C 0.7032(4) 0.8882(4) -0.0708(3) 0.0450(10) Uani 1 1 d . . . H33 H 0.6443 0.9426 -0.0957 0.054 Uiso 1 1 calc R . . C34 C 0.8122(4) 0.8879(4) -0.1131(3) 0.0452(10) Uani 1 1 d . . . H34 H 0.8283 0.9431 -0.1660 0.054 Uiso 1 1 calc R . . C35 C 0.8980(4) 0.8068(4) -0.0782(3) 0.0479(11) Uani 1 1 d . . . H35 H 0.9737 0.8049 -0.1081 0.057 Uiso 1 1 calc R . . C36 C 0.8746(3) 0.7283(3) -0.0003(3) 0.0389(9) Uani 1 1 d . . . H36 H 0.9344 0.6730 0.0231 0.047 Uiso 1 1 calc R . . C41 C 0.7422(3) 0.5127(3) 0.1123(3) 0.0336(8) Uani 1 1 d . . . C42 C 0.6982(4) 0.4319(3) 0.1761(3) 0.0420(9) Uani 1 1 d . . . H42 H 0.6667 0.4356 0.2367 0.050 Uiso 1 1 calc R . . C43 C 0.6998(4) 0.3467(4) 0.1522(4) 0.0522(11) Uani 1 1 d . . . H43 H 0.6686 0.2926 0.1963 0.063 Uiso 1 1 calc R . . C44 C 0.7466(5) 0.3393(4) 0.0642(4) 0.0588(13) Uani 1 1 d . . . H44 H 0.7477 0.2803 0.0478 0.071 Uiso 1 1 calc R . . C45 C 0.7919(4) 0.4184(4) 0.0004(4) 0.0571(12) Uani 1 1 d . . . H45 H 0.8244 0.4137 -0.0601 0.068 Uiso 1 1 calc R . . C46 C 0.7900(4) 0.5043(4) 0.0243(3) 0.0463(10) Uani 1 1 d . . . H46 H 0.8216 0.5581 -0.0198 0.056 Uiso 1 1 calc R . . C51 C 0.2629(3) 0.7597(3) 0.2632(3) 0.0313(8) Uani 1 1 d . . . C52 C 0.1765(4) 0.7734(4) 0.2320(4) 0.0517(12) Uani 1 1 d . . . H52 H 0.1940 0.7434 0.1838 0.062 Uiso 1 1 calc R . . C53 C 0.0648(4) 0.8310(5) 0.2716(4) 0.0576(13) Uani 1 1 d . . . H53 H 0.0066 0.8407 0.2498 0.069 Uiso 1 1 calc R . . C54 C 0.0383(3) 0.8736(4) 0.3417(3) 0.0482(11) Uani 1 1 d . . . H54 H -0.0381 0.9117 0.3691 0.058 Uiso 1 1 calc R . . C55 C 0.1229(4) 0.8610(4) 0.3722(3) 0.0431(10) Uani 1 1 d . . . H55 H 0.1048 0.8911 0.4203 0.052 Uiso 1 1 calc R . . C56 C 0.2343(3) 0.8045(3) 0.3330(3) 0.0338(8) Uani 1 1 d . . . H56 H 0.2919 0.7965 0.3547 0.041 Uiso 1 1 calc R . . C61 C 0.3954(3) 0.5384(3) 0.2633(2) 0.0296(7) Uani 1 1 d . . . C62 C 0.4246(3) 0.4720(3) 0.3415(3) 0.0365(9) Uani 1 1 d . . . H62 H 0.4542 0.4977 0.3685 0.044 Uiso 1 1 calc R . . C63 C 0.4114(4) 0.3697(4) 0.3805(3) 0.0449(10) Uani 1 1 d . . . H63 H 0.4305 0.3262 0.4345 0.054 Uiso 1 1 calc R . . C64 C 0.3700(4) 0.3302(4) 0.3407(3) 0.0463(10) Uani 1 1 d . . . H64 H 0.3622 0.2591 0.3666 0.056 Uiso 1 1 calc R . . C65 C 0.3407(4) 0.3954(4) 0.2635(3) 0.0430(10) Uani 1 1 d . . . H65 H 0.3123 0.3687 0.2363 0.052 Uiso 1 1 calc R . . C66 C 0.3517(3) 0.4990(3) 0.2248(3) 0.0374(9) Uani 1 1 d . . . H66 H 0.3297 0.5434 0.1721 0.045 Uiso 1 1 calc R . . C71 C 0.4272(3) 0.7117(3) 0.1006(3) 0.0319(8) Uani 1 1 d . . . C72 C 0.3852(4) 0.8222(4) 0.0571(3) 0.0441(10) Uani 1 1 d . . . H72 H 0.3386 0.8763 0.0907 0.053 Uiso 1 1 calc R . . C73 C 0.4112(4) 0.8539(5) -0.0359(3) 0.0571(14) Uani 1 1 d . . . H73 H 0.3839 0.9299 -0.0653 0.069 Uiso 1 1 calc R . . C74 C 0.4758(4) 0.7763(5) -0.0850(3) 0.0584(13) Uani 1 1 d . . . H74 H 0.4921 0.7982 -0.1482 0.070 Uiso 1 1 calc R . . C75 C 0.5173(4) 0.6662(5) -0.0425(3) 0.0562(12) Uani 1 1 d . . . H75 H 0.5614 0.6122 -0.0765 0.067 Uiso 1 1 calc R . . C76 C 0.4947(4) 0.6339(4) 0.0501(3) 0.0395(9) Uani 1 1 d . . . H76 H 0.5255 0.5584 0.0787 0.047 Uiso 1 1 calc R . . C1L C 0.999(7) 0.975(7) -0.072(6) 0.24(3) Uiso 0.245(5) 1 d P B 1 H1L1 H 1.0100 0.9064 -0.0840 0.292 Uiso 0.245(5) 1 calc PR B 1 H1L2 H 0.9937 1.0408 -0.1234 0.292 Uiso 0.245(5) 1 calc PR B 1 C1L' C 0.8725(10) 0.9341(11) 0.0884(9) 0.109(4) Uiso 0.755(5) 1 d P B 2 H1L3 H 0.8248 0.8866 0.1160 0.131 Uiso 0.755(5) 1 calc PR B 2 H1L4 H 0.8602 0.9778 0.0294 0.131 Uiso 0.755(5) 1 calc PR B 2 Cl1 Cl 1.0641(15) 0.9645(16) -0.0038(14) 0.193(2) Uiso 0.245(5) 1 d P . 1 Cl1' Cl 1.0027(5) 0.8539(5) 0.0720(4) 0.193(2) Uiso 0.755(5) 1 d P B 2 Cl2 Cl 0.8262(6) 1.0215(5) 0.1508(5) 0.274(3) Uani 1 1 d . . . C2L C 0.9097(11) 0.5278(10) 0.5285(9) 0.071(3) Uiso 0.50 1 d P C -1 H2L1 H 0.8646 0.5349 0.4922 0.085 Uiso 0.50 1 calc PR C -1 H2L2 H 0.8685 0.5046 0.5919 0.085 Uiso 0.50 1 calc PR C -1 Cl3 Cl 0.9129(4) 0.6493(4) 0.5119(3) 0.0999(11) Uiso 0.50 1 d P C -1 Cl4 Cl 1.0398(4) 0.4196(4) 0.5045(3) 0.1079(13) Uiso 0.50 1 d P C -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0227(2) 0.0251(2) 0.0250(2) -0.00528(17) -0.00587(17) -0.00620(17) P1 0.0317(5) 0.0190(4) 0.0499(6) -0.0068(4) -0.0207(4) -0.0050(4) P2 0.0226(4) 0.0271(5) 0.0263(5) -0.0043(4) -0.0044(4) -0.0052(3) P3 0.0240(4) 0.0275(4) 0.0296(5) -0.0096(4) -0.0088(4) -0.0060(3) S1 0.0385(5) 0.0229(4) 0.0359(5) 0.0000(4) -0.0049(4) -0.0080(4) S2 0.0261(4) 0.0220(4) 0.0261(4) -0.0047(3) -0.0088(3) -0.0027(3) O1 0.0438(15) 0.0194(12) 0.0596(18) -0.0106(12) -0.0290(14) -0.0043(11) C2 0.0344(19) 0.0214(17) 0.043(2) -0.0077(16) -0.0144(17) -0.0047(14) C3 0.061(3) 0.043(3) 0.039(3) -0.007(2) -0.010(2) 0.000(2) C4 0.042(2) 0.032(2) 0.053(3) -0.0004(18) -0.022(2) -0.0101(17) N1 0.0349(16) 0.0239(15) 0.0303(16) -0.0078(12) -0.0130(13) -0.0038(12) N2 0.0290(16) 0.0233(16) 0.0302(17) -0.0047(13) -0.0061(13) -0.0039(12) C1 0.0259(16) 0.0261(17) 0.0267(18) -0.0080(14) -0.0123(14) -0.0047(13) C11 0.0290(19) 0.0261(18) 0.030(2) -0.0014(15) -0.0052(15) 0.0006(14) C12 0.031(2) 0.037(2) 0.046(3) 0.0066(19) -0.0056(18) -0.0056(17) C13 0.034(2) 0.047(3) 0.072(4) 0.011(3) 0.002(2) -0.005(2) C14 0.047(3) 0.055(3) 0.046(3) -0.001(2) 0.010(2) 0.004(2) C15 0.070(3) 0.046(3) 0.034(2) -0.018(2) -0.009(2) 0.012(2) C16 0.045(2) 0.044(2) 0.036(2) -0.0120(19) -0.0106(19) -0.0004(19) C17 0.040(2) 0.042(3) 0.093(4) 0.003(3) -0.026(3) -0.016(2) C21 0.0235(17) 0.039(2) 0.029(2) 0.0030(16) -0.0049(15) -0.0103(15) C22 0.032(2) 0.062(3) 0.046(3) -0.012(2) -0.0098(19) -0.016(2) C23 0.047(3) 0.096(4) 0.053(3) -0.014(3) -0.019(2) -0.030(3) C24 0.038(3) 0.108(5) 0.051(3) 0.012(3) -0.022(2) -0.030(3) C25 0.030(2) 0.064(3) 0.060(3) 0.015(3) -0.012(2) -0.006(2) C26 0.033(2) 0.039(2) 0.041(2) 0.0029(18) -0.0084(18) -0.0034(17) C31 0.0312(18) 0.0262(17) 0.0283(19) -0.0056(14) -0.0058(15) -0.0072(14) C32 0.033(2) 0.040(2) 0.036(2) -0.0051(17) -0.0085(17) -0.0097(17) C33 0.048(2) 0.034(2) 0.040(2) -0.0004(18) -0.018(2) -0.0048(18) C34 0.057(3) 0.039(2) 0.032(2) -0.0007(17) -0.0082(19) -0.021(2) C35 0.046(2) 0.055(3) 0.035(2) -0.003(2) -0.0021(19) -0.026(2) C36 0.033(2) 0.040(2) 0.034(2) -0.0057(17) -0.0059(17) -0.0102(17) C41 0.0279(18) 0.0277(18) 0.036(2) -0.0084(15) -0.0045(16) -0.0050(14) C42 0.042(2) 0.033(2) 0.040(2) -0.0041(17) -0.0089(18) -0.0095(17) C43 0.059(3) 0.033(2) 0.059(3) -0.005(2) -0.014(2) -0.018(2) C44 0.062(3) 0.042(3) 0.075(4) -0.027(2) -0.011(3) -0.018(2) C45 0.066(3) 0.056(3) 0.051(3) -0.028(2) 0.001(2) -0.026(2) C46 0.048(2) 0.043(2) 0.041(2) -0.0149(19) 0.0023(19) -0.020(2) C51 0.0271(18) 0.0306(19) 0.038(2) -0.0128(16) -0.0092(15) -0.0080(14) C52 0.031(2) 0.070(3) 0.064(3) -0.041(3) -0.015(2) -0.003(2) C53 0.029(2) 0.071(3) 0.082(4) -0.036(3) -0.022(2) -0.004(2) C54 0.0249(19) 0.046(2) 0.064(3) -0.022(2) -0.0069(19) -0.0022(17) C55 0.039(2) 0.040(2) 0.048(3) -0.0201(19) -0.0054(19) -0.0096(18) C56 0.0310(19) 0.0288(18) 0.042(2) -0.0096(16) -0.0128(16) -0.0070(15) C61 0.0261(17) 0.0311(18) 0.0296(19) -0.0104(15) -0.0047(14) -0.0085(14) C62 0.036(2) 0.034(2) 0.042(2) -0.0081(17) -0.0154(17) -0.0120(16) C63 0.050(2) 0.041(2) 0.049(3) -0.0011(19) -0.025(2) -0.0187(19) C64 0.051(3) 0.037(2) 0.053(3) -0.0056(19) -0.015(2) -0.0205(19) C65 0.051(2) 0.047(2) 0.043(2) -0.0107(19) -0.013(2) -0.027(2) C66 0.043(2) 0.040(2) 0.035(2) -0.0093(17) -0.0127(17) -0.0176(18) C71 0.0344(19) 0.0327(19) 0.031(2) -0.0046(15) -0.0127(16) -0.0134(15) C72 0.043(2) 0.039(2) 0.046(3) -0.0021(19) -0.020(2) -0.0105(18) C73 0.059(3) 0.058(3) 0.048(3) 0.017(2) -0.029(2) -0.026(2) C74 0.062(3) 0.084(4) 0.030(2) 0.001(2) -0.016(2) -0.035(3) C75 0.062(3) 0.073(3) 0.034(2) -0.020(2) -0.006(2) -0.025(3) C76 0.044(2) 0.044(2) 0.031(2) -0.0092(17) -0.0110(17) -0.0149(18) Cl2 0.313(7) 0.216(5) 0.311(8) -0.097(5) -0.179(6) 0.005(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 P2 2.2762(10) . ? Cu1 P3 2.3103(9) . ? Cu1 S2 2.3279(9) . ? Cu1 S1 2.3653(10) . ? P1 O1 1.588(3) . ? P1 O2' 1.592(6) . ? P1 N1 1.601(3) . ? P1 O2 1.615(5) . ? P1 S1 1.9686(15) . ? P2 C41 1.824(4) . ? P2 C21 1.831(4) . ? P2 C31 1.828(4) . ? P3 C61 1.827(4) . ? P3 C71 1.825(4) . ? P3 C51 1.829(4) . ? S2 C1 1.740(4) . ? O1 C2 1.458(4) . ? C2 C3 1.506(6) . ? C2 C4 1.502(5) . ? C2 H2A 1.0000 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? O2 C5 1.425(10) . ? C5 C7 1.492(13) . ? C5 C6 1.506(14) . ? C5 H5 1.0000 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? O2' C5' 1.469(12) . ? C5' C6' 1.503(18) . ? C5' C7' 1.509(17) . ? C5' H5' 1.0000 . ? C6' H6'1 0.9800 . ? C6' H6'2 0.9800 . ? C6' H6'3 0.9800 . ? C7' H7'1 0.9800 . ? C7' H7'2 0.9800 . ? C7' H7'3 0.9800 . ? N1 C1 1.310(5) . ? N2 C1 1.350(5) . ? N2 C11 1.431(5) . ? N2 H2 0.86(5) . ? C11 C16 1.379(6) . ? C11 C12 1.398(6) . ? C12 C13 1.397(7) . ? C12 C17 1.492(8) . ? C13 C14 1.361(10) . ? C13 H13 0.9500 . ? C14 C15 1.386(9) . ? C14 H14 0.9500 . ? C15 C16 1.388(7) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C21 C22 1.386(7) . ? C21 C26 1.389(6) . ? C22 C23 1.399(6) . ? C22 H22 0.9500 . ? C23 C24 1.370(9) . ? C23 H23 0.9500 . ? C24 C25 1.372(10) . ? C24 H24 0.9500 . ? C25 C26 1.397(7) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C31 C32 1.399(5) . ? C31 C36 1.395(5) . ? C32 C33 1.376(6) . ? C32 H32 0.9500 . ? C33 C34 1.376(6) . ? C33 H33 0.9500 . ? C34 C35 1.379(6) . ? C34 H34 0.9500 . ? C35 C36 1.378(6) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C41 C42 1.392(6) . ? C41 C46 1.389(6) . ? C42 C43 1.373(7) . ? C42 H42 0.9500 . ? C43 C44 1.386(8) . ? C43 H43 0.9500 . ? C44 C45 1.383(7) . ? C44 H44 0.9500 . ? C45 C46 1.381(7) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C51 C56 1.378(6) . ? C51 C52 1.400(5) . ? C52 C53 1.394(6) . ? C52 H52 0.9500 . ? C53 C54 1.369(7) . ? C53 H53 0.9500 . ? C54 C55 1.376(6) . ? C54 H54 0.9500 . ? C55 C56 1.385(6) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C61 C66 1.400(5) . ? C61 C62 1.391(5) . ? C62 C63 1.378(6) . ? C62 H62 0.9500 . ? C63 C64 1.391(6) . ? C63 H63 0.9500 . ? C64 C65 1.377(6) . ? C64 H64 0.9500 . ? C65 C66 1.382(6) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? C71 C76 1.389(6) . ? C71 C72 1.390(6) . ? C72 C73 1.396(7) . ? C72 H72 0.9500 . ? C73 C74 1.369(8) . ? C73 H73 0.9500 . ? C74 C75 1.380(8) . ? C74 H74 0.9500 . ? C75 C76 1.393(6) . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? C1L Cl1 1.65(8) . ? C1L H1L1 0.9900 . ? C1L H1L2 0.9900 . ? C1L' Cl1' 1.615(13) . ? C1L' H1L3 0.9900 . ? C1L' H1L4 0.9900 . ? Cl1 C1L 1.53(9) 2_775 ? C2L Cl3 1.617(14) . ? C2L Cl4 1.771(13) . ? C2L H2L1 0.9900 . ? C2L H2L2 0.9900 . ? 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 P2 Cu1 P3 113.21(4) . . ? P2 Cu1 S2 107.63(3) . . ? P3 Cu1 S2 116.85(4) . . ? P2 Cu1 S1 109.29(4) . . ? P3 Cu1 S1 104.56(4) . . ? S2 Cu1 S1 104.76(4) . . ? O1 P1 O2' 97.9(2) . . ? O1 P1 N1 104.04(17) . . ? O2' P1 N1 97.1(3) . . ? O1 P1 O2 104.3(2) . . ? N1 P1 O2 117.9(2) . . ? O1 P1 S1 109.66(12) . . ? O2' P1 S1 125.2(3) . . ? N1 P1 S1 119.36(12) . . ? O2 P1 S1 100.7(2) . . ? C41 P2 C21 104.27(19) . . ? C41 P2 C31 104.10(18) . . ? C21 P2 C31 101.64(17) . . ? C41 P2 Cu1 114.17(13) . . ? C21 P2 Cu1 115.54(14) . . ? C31 P2 Cu1 115.51(12) . . ? C61 P3 C71 105.57(17) . . ? C61 P3 C51 99.69(17) . . ? C71 P3 C51 102.68(17) . . ? C61 P3 Cu1 117.20(12) . . ? C71 P3 Cu1 110.00(12) . . ? C51 P3 Cu1 119.86(12) . . ? P1 S1 Cu1 100.45(5) . . ? C1 S2 Cu1 100.88(11) . . ? C2 O1 P1 119.3(2) . . ? O1 C2 C3 109.6(3) . . ? O1 C2 C4 107.3(3) . . ? C3 C2 C4 113.1(4) . . ? O1 C2 H2A 108.9 . . ? C3 C2 H2A 108.9 . . ? C4 C2 H2A 108.9 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C5 O2 P1 120.9(5) . . ? O2 C5 C7 106.3(7) . . ? O2 C5 C6 109.3(7) . . ? C7 C5 C6 113.0(8) . . ? O2 C5 H5 109.4 . . ? C7 C5 H5 109.4 . . ? C6 C5 H5 109.4 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5' O2' P1 118.1(6) . . ? O2' C5' C6' 108.3(9) . . ? O2' C5' C7' 104.5(9) . . ? C6' C5' C7' 112.8(10) . . ? O2' C5' H5' 110.4 . . ? C6' C5' H5' 110.4 . . ? C7' C5' H5' 110.4 . . ? C5' C6' H6'1 109.5 . . ? C5' C6' H6'2 109.5 . . ? H6'1 C6' H6'2 109.5 . . ? C5' C6' H6'3 109.5 . . ? H6'1 C6' H6'3 109.5 . . ? H6'2 C6' H6'3 109.5 . . ? C5' C7' H7'1 109.5 . . ? C5' C7' H7'2 109.5 . . ? H7'1 C7' H7'2 109.5 . . ? C5' C7' H7'3 109.5 . . ? H7'1 C7' H7'3 109.5 . . ? H7'2 C7' H7'3 109.5 . . ? C1 N1 P1 128.7(3) . . ? C1 N2 C11 124.3(3) . . ? C1 N2 H2 119(3) . . ? C11 N2 H2 115(3) . . ? N1 C1 N2 118.0(3) . . ? N1 C1 S2 126.7(3) . . ? N2 C1 S2 115.3(3) . . ? C16 C11 C12 121.6(4) . . ? C16 C11 N2 119.5(4) . . ? C12 C11 N2 118.9(4) . . ? C13 C12 C11 116.3(5) . . ? C13 C12 C17 121.1(5) . . ? C11 C12 C17 122.6(4) . . ? C14 C13 C12 123.0(5) . . ? C14 C13 H13 118.5 . . ? C12 C13 H13 118.5 . . ? C13 C14 C15 119.6(5) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C14 C15 C16 119.5(6) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C11 C16 C15 120.0(5) . . ? C11 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C22 C21 C26 119.6(4) . . ? C22 C21 P2 117.1(3) . . ? C26 C21 P2 123.3(4) . . ? C21 C22 C23 120.1(5) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C24 C23 C22 119.9(6) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 C25 120.4(5) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C24 C25 C26 120.5(5) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C25 C26 C21 119.5(5) . . ? C25 C26 H26 120.2 . . ? C21 C26 H26 120.2 . . ? C32 C31 C36 117.9(4) . . ? C32 C31 P2 118.3(3) . . ? C36 C31 P2 123.8(3) . . ? C33 C32 C31 120.6(4) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C34 C33 C32 120.8(4) . . ? C34 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C33 C34 C35 119.4(4) . . ? C33 C34 H34 120.3 . . ? C35 C34 H34 120.3 . . ? C34 C35 C36 120.4(4) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C35 C36 C31 120.9(4) . . ? C35 C36 H36 119.6 . . ? C31 C36 H36 119.6 . . ? C42 C41 C46 118.6(4) . . ? C42 C41 P2 117.5(3) . . ? C46 C41 P2 123.8(3) . . ? C43 C42 C41 120.7(4) . . ? C43 C42 H42 119.6 . . ? C41 C42 H42 119.6 . . ? C42 C43 C44 120.3(4) . . ? C42 C43 H43 119.8 . . ? C44 C43 H43 119.8 . . ? C45 C44 C43 119.5(5) . . ? C45 C44 H44 120.2 . . ? C43 C44 H44 120.2 . . ? C44 C45 C46 120.1(5) . . ? C44 C45 H45 119.9 . . ? C46 C45 H45 119.9 . . ? C45 C46 C41 120.7(4) . . ? C45 C46 H46 119.7 . . ? C41 C46 H46 119.7 . . ? C56 C51 C52 118.3(4) . . ? C56 C51 P3 119.4(3) . . ? C52 C51 P3 122.1(3) . . ? C51 C52 C53 120.0(4) . . ? C51 C52 H52 120.0 . . ? C53 C52 H52 120.0 . . ? C54 C53 C52 120.6(4) . . ? C54 C53 H53 119.7 . . ? C52 C53 H53 119.7 . . ? C53 C54 C55 119.6(4) . . ? C53 C54 H54 120.2 . . ? C55 C54 H54 120.2 . . ? C54 C55 C56 120.4(4) . . ? C54 C55 H55 119.8 . . ? C56 C55 H55 119.8 . . ? C51 C56 C55 121.0(4) . . ? C51 C56 H56 119.5 . . ? C55 C56 H56 119.5 . . ? C66 C61 C62 118.4(4) . . ? C66 C61 P3 123.6(3) . . ? C62 C61 P3 117.9(3) . . ? C63 C62 C61 121.3(4) . . ? C63 C62 H62 119.3 . . ? C61 C62 H62 119.3 . . ? C62 C63 C64 119.9(4) . . ? C62 C63 H63 120.0 . . ? C64 C63 H63 120.0 . . ? C65 C64 C63 119.2(4) . . ? C65 C64 H64 120.4 . . ? C63 C64 H64 120.4 . . ? C64 C65 C66 121.3(4) . . ? C64 C65 H65 119.4 . . ? C66 C65 H65 119.4 . . ? C65 C66 C61 119.9(4) . . ? C65 C66 H66 120.1 . . ? C61 C66 H66 120.1 . . ? C76 C71 C72 118.9(4) . . ? C76 C71 P3 121.4(3) . . ? C72 C71 P3 119.1(3) . . ? C71 C72 C73 120.3(5) . . ? C71 C72 H72 119.9 . . ? C73 C72 H72 119.9 . . ? C74 C73 C72 120.4(5) . . ? C74 C73 H73 119.8 . . ? C72 C73 H73 119.8 . . ? C75 C74 C73 119.9(4) . . ? C75 C74 H74 120.1 . . ? C73 C74 H74 120.1 . . ? C74 C75 C76 120.2(5) . . ? C74 C75 H75 119.9 . . ? C76 C75 H75 119.9 . . ? C71 C76 C75 120.3(4) . . ? C71 C76 H76 119.8 . . ? C75 C76 H76 119.8 . . ? Cl1 C1L Cl2 62(3) . . ? Cl1 C1L H1L1 117.5 . . ? Cl2 C1L H1L1 117.5 . . ? Cl1 C1L H1L2 117.5 . . ? Cl2 C1L H1L2 117.5 . . ? H1L1 C1L H1L2 114.6 . . ? Cl1' C1L' Cl2 118.0(8) . . ? Cl1' C1L' H1L3 107.8 . . ? Cl2 C1L' H1L3 107.8 . . ? Cl1' C1L' H1L4 107.8 . . ? Cl2 C1L' H1L4 107.8 . . ? H1L3 C1L' H1L4 107.2 . . ? C1L Cl1 C1L 121(4) . 2_775 ? Cl3 C2L Cl4 118.0(9) . . ? Cl3 C2L H2L1 107.8 . . ? Cl4 C2L H2L1 107.8 . . ? Cl3 C2L H2L2 107.8 . . ? Cl4 C2L H2L2 107.8 . . ? H2L1 C2L H2L2 107.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P3 Cu1 P2 C41 -30.97(14) . . . . ? S2 Cu1 P2 C41 99.70(14) . . . . ? S1 Cu1 P2 C41 -147.07(14) . . . . ? P3 Cu1 P2 C21 -151.90(15) . . . . ? S2 Cu1 P2 C21 -21.22(15) . . . . ? S1 Cu1 P2 C21 92.01(15) . . . . ? P3 Cu1 P2 C31 89.69(14) . . . . ? S2 Cu1 P2 C31 -139.63(14) . . . . ? S1 Cu1 P2 C31 -26.40(14) . . . . ? P2 Cu1 P3 C61 78.39(14) . . . . ? S2 Cu1 P3 C61 -47.51(14) . . . . ? S1 Cu1 P3 C61 -162.75(14) . . . . ? P2 Cu1 P3 C71 -42.15(14) . . . . ? S2 Cu1 P3 C71 -168.05(14) . . . . ? S1 Cu1 P3 C71 76.71(14) . . . . ? P2 Cu1 P3 C51 -160.73(15) . . . . ? S2 Cu1 P3 C51 73.37(15) . . . . ? S1 Cu1 P3 C51 -41.86(15) . . . . ? O1 P1 S1 Cu1 -154.86(12) . . . . ? O2' P1 S1 Cu1 89.6(3) . . . . ? N1 P1 S1 Cu1 -35.08(14) . . . . ? O2 P1 S1 Cu1 95.63(17) . . . . ? P2 Cu1 S1 P1 -126.14(5) . . . . ? P3 Cu1 S1 P1 112.37(5) . . . . ? S2 Cu1 S1 P1 -11.05(6) . . . . ? P2 Cu1 S2 C1 163.54(12) . . . . ? P3 Cu1 S2 C1 -67.83(12) . . . . ? S1 Cu1 S2 C1 47.30(12) . . . . ? O2' P1 O1 C2 -163.2(4) . . . . ? N1 P1 O1 C2 -63.8(3) . . . . ? O2 P1 O1 C2 172.1(3) . . . . ? S1 P1 O1 C2 64.9(3) . . . . ? P1 O1 C2 C3 107.0(4) . . . . ? P1 O1 C2 C4 -129.8(3) . . . . ? O1 P1 O2 C5 70.5(5) . . . . ? O2' P1 O2 C5 -7.4(6) . . . . ? N1 P1 O2 C5 -44.2(6) . . . . ? S1 P1 O2 C5 -175.8(5) . . . . ? P1 O2 C5 C7 137.2(6) . . . . ? P1 O2 C5 C6 -100.5(8) . . . . ? O1 P1 O2' C5' -86.0(6) . . . . ? N1 P1 O2' C5' 168.7(6) . . . . ? O2 P1 O2' C5' 20.9(6) . . . . ? S1 P1 O2' C5' 34.9(7) . . . . ? P1 O2' C5' C6' 83.1(10) . . . . ? P1 O2' C5' C7' -156.4(8) . . . . ? O1 P1 N1 C1 178.3(3) . . . . ? O2' P1 N1 C1 -81.8(4) . . . . ? O2 P1 N1 C1 -66.9(4) . . . . ? S1 P1 N1 C1 55.7(3) . . . . ? P1 N1 C1 N2 -178.8(3) . . . . ? P1 N1 C1 S2 1.5(5) . . . . ? C11 N2 C1 N1 2.0(5) . . . . ? C11 N2 C1 S2 -178.3(3) . . . . ? Cu1 S2 C1 N1 -52.4(3) . . . . ? Cu1 S2 C1 N2 128.0(2) . . . . ? C1 N2 C11 C16 -58.8(5) . . . . ? C1 N2 C11 C12 122.5(4) . . . . ? C16 C11 C12 C13 2.3(6) . . . . ? N2 C11 C12 C13 -179.1(4) . . . . ? C16 C11 C12 C17 -178.5(4) . . . . ? N2 C11 C12 C17 0.1(6) . . . . ? C11 C12 C13 C14 -1.1(7) . . . . ? C17 C12 C13 C14 179.8(5) . . . . ? C12 C13 C14 C15 -0.6(8) . . . . ? C13 C14 C15 C16 1.2(8) . . . . ? C12 C11 C16 C15 -1.9(6) . . . . ? N2 C11 C16 C15 179.5(4) . . . . ? C14 C15 C16 C11 0.1(7) . . . . ? C41 P2 C21 C22 -168.0(3) . . . . ? C31 P2 C21 C22 84.0(3) . . . . ? Cu1 P2 C21 C22 -41.9(4) . . . . ? C41 P2 C21 C26 14.2(4) . . . . ? C31 P2 C21 C26 -93.8(4) . . . . ? Cu1 P2 C21 C26 140.4(3) . . . . ? C26 C21 C22 C23 2.0(7) . . . . ? P2 C21 C22 C23 -175.8(4) . . . . ? C21 C22 C23 C24 -1.4(8) . . . . ? C22 C23 C24 C25 0.5(8) . . . . ? C23 C24 C25 C26 -0.1(8) . . . . ? C24 C25 C26 C21 0.7(7) . . . . ? C22 C21 C26 C25 -1.6(6) . . . . ? P2 C21 C26 C25 176.1(3) . . . . ? C41 P2 C31 C32 93.0(3) . . . . ? C21 P2 C31 C32 -158.9(3) . . . . ? Cu1 P2 C31 C32 -33.0(4) . . . . ? C41 P2 C31 C36 -86.6(4) . . . . ? C21 P2 C31 C36 21.6(4) . . . . ? Cu1 P2 C31 C36 147.4(3) . . . . ? C36 C31 C32 C33 -0.6(6) . . . . ? P2 C31 C32 C33 179.9(4) . . . . ? C31 C32 C33 C34 -0.9(7) . . . . ? C32 C33 C34 C35 2.1(7) . . . . ? C33 C34 C35 C36 -1.7(7) . . . . ? C34 C35 C36 C31 0.2(7) . . . . ? C32 C31 C36 C35 0.9(6) . . . . ? P2 C31 C36 C35 -179.5(4) . . . . ? C21 P2 C41 C42 85.9(3) . . . . ? C31 P2 C41 C42 -168.0(3) . . . . ? Cu1 P2 C41 C42 -41.1(3) . . . . ? C21 P2 C41 C46 -98.2(4) . . . . ? C31 P2 C41 C46 7.9(4) . . . . ? Cu1 P2 C41 C46 134.8(3) . . . . ? C46 C41 C42 C43 -1.3(6) . . . . ? P2 C41 C42 C43 174.8(3) . . . . ? C41 C42 C43 C44 0.8(7) . . . . ? C42 C43 C44 C45 0.0(8) . . . . ? C43 C44 C45 C46 -0.2(8) . . . . ? C44 C45 C46 C41 -0.3(8) . . . . ? C42 C41 C46 C45 1.1(7) . . . . ? P2 C41 C46 C45 -174.7(4) . . . . ? C61 P3 C51 C56 107.3(3) . . . . ? C71 P3 C51 C56 -144.1(3) . . . . ? Cu1 P3 C51 C56 -21.9(4) . . . . ? C61 P3 C51 C52 -67.7(4) . . . . ? C71 P3 C51 C52 40.8(4) . . . . ? Cu1 P3 C51 C52 163.0(3) . . . . ? C56 C51 C52 C53 -0.1(7) . . . . ? P3 C51 C52 C53 175.0(4) . . . . ? C51 C52 C53 C54 -0.7(9) . . . . ? C52 C53 C54 C55 1.1(8) . . . . ? C53 C54 C55 C56 -0.7(7) . . . . ? C52 C51 C56 C55 0.5(6) . . . . ? P3 C51 C56 C55 -174.7(3) . . . . ? C54 C55 C56 C51 -0.1(7) . . . . ? C71 P3 C61 C66 -28.1(4) . . . . ? C51 P3 C61 C66 78.1(4) . . . . ? Cu1 P3 C61 C66 -151.0(3) . . . . ? C71 P3 C61 C62 155.2(3) . . . . ? C51 P3 C61 C62 -98.6(3) . . . . ? Cu1 P3 C61 C62 32.4(3) . . . . ? C66 C61 C62 C63 0.1(6) . . . . ? P3 C61 C62 C63 176.9(3) . . . . ? C61 C62 C63 C64 1.2(7) . . . . ? C62 C63 C64 C65 -1.3(7) . . . . ? C63 C64 C65 C66 0.1(7) . . . . ? C64 C65 C66 C61 1.2(7) . . . . ? C62 C61 C66 C65 -1.3(6) . . . . ? P3 C61 C66 C65 -177.9(3) . . . . ? C61 P3 C71 C76 -41.0(4) . . . . ? C51 P3 C71 C76 -145.0(3) . . . . ? Cu1 P3 C71 C76 86.3(3) . . . . ? C61 P3 C71 C72 147.9(3) . . . . ? C51 P3 C71 C72 43.9(3) . . . . ? Cu1 P3 C71 C72 -84.8(3) . . . . ? C76 C71 C72 C73 -0.3(6) . . . . ? P3 C71 C72 C73 171.0(3) . . . . ? C71 C72 C73 C74 1.7(7) . . . . ? C72 C73 C74 C75 -1.2(7) . . . . ? C73 C74 C75 C76 -0.7(8) . . . . ? C72 C71 C76 C75 -1.6(6) . . . . ? P3 C71 C76 C75 -172.7(3) . . . . ? C74 C75 C76 C71 2.1(7) . . . . ? Cl2 C1L Cl1 C1L -24(2) . . . 2_775 ? Cl1' C1L' Cl2 C1L 75(2) . . . . ? Cl1 C1L Cl2 C1L' -111(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2 S2 0.86(5) 2.60(5) 3.431(3) 163(4) 2_666 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.055 _refine_diff_density_min -1.164 _refine_diff_density_rms 0.095 # Attachment '- 3.cif' data_safin59 _database_code_depnum_ccdc_archive 'CCDC 749645' #TrackingRef '- 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H84 Cu4 N12 O8 P4 S8' _chemical_formula_sum 'C52 H84 Cu4 N12 O8 P4 S8' _chemical_formula_weight 1639.83 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' Cu Cu 0.3201 1.2651 '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' 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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I41/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 26.9217(6) _cell_length_b 26.9217(6) _cell_length_c 10.2810(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7451.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 56340 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 26.0 _exptl_crystal_description block _exptl_crystal_colour 'light red' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3392 _exptl_absorpt_coefficient_mu 1.490 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7070 _exptl_absorpt_correction_T_max 0.7162 _exptl_absorpt_process_details 'MULABS (Spek, 2003; Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS II two-circle-diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 82703 _diffrn_reflns_av_R_equivalents 0.0702 _diffrn_reflns_av_sigmaI/netI 0.0221 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.37 _diffrn_reflns_theta_max 25.66 _reflns_number_total 3509 _reflns_number_gt 3055 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'X-Area (Stoe & Cie, 2001)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2001)' _computing_data_reduction 'X-Area (Stoe & Cie, 2001)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008) ' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008) ' _computing_molecular_graphics 'XP in SHELXTL-Plus (Sheldrick, 1991)' _computing_publication_material SHELXL97 _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^)+(0.0351P)^2^+3.3826P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3509 _refine_ls_number_parameters 204 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0402 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0661 _refine_ls_wR_factor_gt 0.0625 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.568240(10) 0.697524(10) 0.60277(3) 0.03108(9) Uani 1 1 d . . . P1 P 0.604407(19) 0.63179(2) 0.37822(5) 0.02667(12) Uani 1 1 d . . . S1 S 0.63561(2) 0.65379(2) 0.54255(5) 0.03196(13) Uani 1 1 d . . . S2 S 0.500515(19) 0.682873(19) 0.48279(6) 0.03015(13) Uani 1 1 d . . . O1 O 0.59728(6) 0.67459(6) 0.27580(15) 0.0333(3) Uani 1 1 d . . . O2 O 0.64172(5) 0.59330(6) 0.31789(16) 0.0363(4) Uani 1 1 d . . . N1 N 0.55149(6) 0.60302(6) 0.38327(18) 0.0279(4) Uani 1 1 d . . . N2 N 0.46765(7) 0.59391(7) 0.42232(19) 0.0292(4) Uani 1 1 d . . . H2 H 0.4434(10) 0.6081(10) 0.451(3) 0.039(7) Uiso 1 1 d . . . C1 C 0.50973(7) 0.62131(8) 0.4252(2) 0.0259(4) Uani 1 1 d . . . C2 C 0.62186(10) 0.72328(9) 0.2786(2) 0.0427(6) Uani 1 1 d . . . H2A H 0.6228 0.7356 0.3703 0.051 Uiso 1 1 calc R . . C3 C 0.67418(12) 0.71840(14) 0.2288(3) 0.0728(10) Uani 1 1 d . . . H3A H 0.6931 0.6963 0.2863 0.109 Uiso 1 1 calc R . . H3B H 0.6899 0.7512 0.2269 0.109 Uiso 1 1 calc R . . H3C H 0.6736 0.7045 0.1407 0.109 Uiso 1 1 calc R . . C4 C 0.58877(15) 0.75707(11) 0.1991(4) 0.0726(10) Uani 1 1 d . . . H4A H 0.5557 0.7585 0.2387 0.109 Uiso 1 1 calc R . . H4B H 0.5860 0.7441 0.1103 0.109 Uiso 1 1 calc R . . H4C H 0.6031 0.7905 0.1966 0.109 Uiso 1 1 calc R . . C5 C 0.62984(10) 0.56060(11) 0.2076(3) 0.0537(7) Uani 1 1 d . . . H5 H 0.5931 0.5558 0.2016 0.064 Uiso 1 1 calc R . . C6 C 0.6540(2) 0.51317(13) 0.2355(5) 0.1109(17) Uani 1 1 d . . . H6A H 0.6401 0.4990 0.3153 0.166 Uiso 1 1 calc R . . H6B H 0.6898 0.5185 0.2470 0.166 Uiso 1 1 calc R . . H6C H 0.6485 0.4902 0.1629 0.166 Uiso 1 1 calc R . . C7 C 0.6489(2) 0.58505(17) 0.0848(4) 0.1015(15) Uani 1 1 d . . . H7A H 0.6314 0.6166 0.0713 0.152 Uiso 1 1 calc R . . H7B H 0.6429 0.5631 0.0104 0.152 Uiso 1 1 calc R . . H7C H 0.6846 0.5913 0.0932 0.152 Uiso 1 1 calc R . . C11 C 0.45830(8) 0.54495(8) 0.3791(2) 0.0265(4) Uani 1 1 d . . . N12 N 0.40975(7) 0.53461(7) 0.38232(19) 0.0322(4) Uani 1 1 d . . . C13 C 0.39501(9) 0.48936(8) 0.3423(2) 0.0369(5) Uani 1 1 d . . . C14 C 0.42864(9) 0.45420(8) 0.2985(2) 0.0398(5) Uani 1 1 d . . . H14 H 0.4175 0.4227 0.2686 0.048 Uiso 1 1 calc R . . C15 C 0.47850(9) 0.46552(8) 0.2990(2) 0.0374(5) Uani 1 1 d . . . H15 H 0.5020 0.4414 0.2712 0.045 Uiso 1 1 calc R . . C16 C 0.49454(8) 0.51174(8) 0.3399(2) 0.0315(5) Uani 1 1 d . . . H16 H 0.5288 0.5203 0.3410 0.038 Uiso 1 1 calc R . . C17 C 0.34031(10) 0.47894(10) 0.3519(4) 0.0571(8) Uani 1 1 d . . . H17A H 0.3321 0.4690 0.4411 0.086 Uiso 1 1 calc R . . H17B H 0.3315 0.4521 0.2918 0.086 Uiso 1 1 calc R . . H17C H 0.3216 0.5089 0.3291 0.086 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 Cu1 0.03392(15) 0.02777(14) 0.03156(15) -0.00088(11) -0.00210(11) -0.00529(11) P1 0.0226(3) 0.0283(3) 0.0292(3) 0.0005(2) 0.0021(2) -0.0028(2) S1 0.0282(3) 0.0357(3) 0.0321(3) 0.0014(2) -0.0039(2) -0.0023(2) S2 0.0255(3) 0.0262(3) 0.0388(3) -0.0044(2) 0.0026(2) -0.0018(2) O1 0.0364(8) 0.0331(8) 0.0303(8) 0.0042(6) -0.0018(6) -0.0084(6) O2 0.0252(8) 0.0397(9) 0.0439(9) -0.0094(7) 0.0055(7) -0.0014(6) N1 0.0237(9) 0.0295(9) 0.0307(10) -0.0014(7) 0.0018(7) -0.0036(7) N2 0.0217(9) 0.0296(9) 0.0362(10) -0.0066(8) 0.0042(8) -0.0023(7) C1 0.0260(10) 0.0279(10) 0.0238(10) -0.0018(8) 0.0001(8) -0.0029(8) C2 0.0531(15) 0.0379(13) 0.0371(13) 0.0111(10) -0.0029(11) -0.0175(11) C3 0.0611(19) 0.095(3) 0.062(2) 0.0114(18) 0.0142(16) -0.0384(18) C4 0.099(3) 0.0452(17) 0.073(2) 0.0250(16) -0.024(2) -0.0108(17) C5 0.0384(14) 0.0615(17) 0.0614(18) -0.0282(14) 0.0173(13) -0.0090(12) C6 0.204(6) 0.0404(18) 0.088(3) -0.0182(19) -0.007(3) 0.013(3) C7 0.154(4) 0.095(3) 0.056(2) -0.012(2) 0.034(3) 0.021(3) C11 0.0287(10) 0.0266(10) 0.0242(10) 0.0008(8) -0.0009(8) -0.0040(8) N12 0.0272(9) 0.0296(9) 0.0398(11) 0.0023(8) -0.0018(8) -0.0057(7) C13 0.0339(12) 0.0307(11) 0.0460(14) 0.0057(10) -0.0025(10) -0.0077(9) C14 0.0479(14) 0.0261(11) 0.0454(14) -0.0007(10) -0.0036(11) -0.0082(10) C15 0.0442(13) 0.0290(11) 0.0392(13) -0.0016(10) 0.0041(10) 0.0019(10) C16 0.0311(11) 0.0306(11) 0.0327(11) 0.0006(9) 0.0022(9) -0.0019(9) C17 0.0378(14) 0.0412(14) 0.092(2) 0.0023(15) -0.0079(14) -0.0142(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 S2 2.2123(6) 12_767 ? Cu1 S2 2.2364(6) . ? Cu1 S1 2.2492(6) . ? P1 O2 1.5709(16) . ? P1 O1 1.5726(16) . ? P1 N1 1.6223(17) . ? P1 S1 1.9776(8) . ? S2 C1 1.778(2) . ? S2 Cu1 2.2124(6) 15_566 ? O1 C2 1.469(3) . ? O2 C5 1.471(3) . ? N1 C1 1.301(3) . ? N2 C1 1.352(3) . ? N2 C11 1.414(3) . ? N2 H2 0.81(3) . ? C2 C3 1.504(4) . ? C2 C4 1.513(4) . ? C2 H2A 1.0000 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.462(5) . ? C5 C7 1.513(5) . ? C5 H5 1.0000 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C11 N12 1.337(3) . ? C11 C16 1.383(3) . ? N12 C13 1.346(3) . ? C13 C14 1.385(3) . ? C13 C17 1.502(3) . ? C14 C15 1.377(3) . ? C14 H14 0.9500 . ? C15 C16 1.383(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 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 S2 Cu1 S2 121.61(3) 12_767 . ? S2 Cu1 S1 123.97(2) 12_767 . ? S2 Cu1 S1 114.41(2) . . ? O2 P1 O1 107.28(9) . . ? O2 P1 N1 105.02(9) . . ? O1 P1 N1 105.31(9) . . ? O2 P1 S1 105.26(7) . . ? O1 P1 S1 113.85(6) . . ? N1 P1 S1 119.25(7) . . ? P1 S1 Cu1 92.83(3) . . ? C1 S2 Cu1 109.40(7) . 15_566 ? C1 S2 Cu1 103.56(7) . . ? Cu1 S2 Cu1 96.12(2) 15_566 . ? C2 O1 P1 125.86(14) . . ? C5 O2 P1 124.07(15) . . ? C1 N1 P1 126.08(15) . . ? C1 N2 C11 131.66(19) . . ? C1 N2 H2 114.2(19) . . ? C11 N2 H2 114.2(19) . . ? N1 C1 N2 120.70(19) . . ? N1 C1 S2 125.73(15) . . ? N2 C1 S2 113.51(15) . . ? O1 C2 C3 109.7(2) . . ? O1 C2 C4 105.1(2) . . ? C3 C2 C4 114.8(3) . . ? O1 C2 H2A 109.0 . . ? C3 C2 H2A 109.0 . . ? C4 C2 H2A 109.0 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 O2 105.9(3) . . ? C6 C5 C7 113.1(3) . . ? O2 C5 C7 108.0(3) . . ? C6 C5 H5 109.9 . . ? O2 C5 H5 109.9 . . ? C7 C5 H5 109.9 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N12 C11 C16 124.21(19) . . ? N12 C11 N2 111.13(18) . . ? C16 C11 N2 124.65(19) . . ? C11 N12 C13 117.99(19) . . ? N12 C13 C14 121.7(2) . . ? N12 C13 C17 116.0(2) . . ? C14 C13 C17 122.3(2) . . ? C15 C14 C13 119.0(2) . . ? C15 C14 H14 120.5 . . ? C13 C14 H14 120.5 . . ? C14 C15 C16 120.3(2) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C15 C16 C11 116.7(2) . . ? C15 C16 H16 121.6 . . ? C11 C16 H16 121.6 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 P1 S1 Cu1 -173.13(7) . . . . ? O1 P1 S1 Cu1 69.65(7) . . . . ? N1 P1 S1 Cu1 -55.70(8) . . . . ? S2 Cu1 S1 P1 -168.84(3) 12_767 . . . ? S2 Cu1 S1 P1 11.65(3) . . . . ? S2 Cu1 S2 C1 -152.60(7) 12_767 . . . ? S1 Cu1 S2 C1 26.92(7) . . . . ? S2 Cu1 S2 Cu1 -40.92(2) 12_767 . . 15_566 ? S1 Cu1 S2 Cu1 138.60(2) . . . 15_566 ? O2 P1 O1 C2 -100.00(19) . . . . ? N1 P1 O1 C2 148.49(18) . . . . ? S1 P1 O1 C2 16.0(2) . . . . ? O1 P1 O2 C5 -70.0(2) . . . . ? N1 P1 O2 C5 41.7(2) . . . . ? S1 P1 O2 C5 168.41(18) . . . . ? O2 P1 N1 C1 -179.14(18) . . . . ? O1 P1 N1 C1 -66.0(2) . . . . ? S1 P1 N1 C1 63.3(2) . . . . ? P1 N1 C1 N2 178.74(16) . . . . ? P1 N1 C1 S2 1.8(3) . . . . ? C11 N2 C1 N1 -0.2(4) . . . . ? C11 N2 C1 S2 177.08(18) . . . . ? Cu1 S2 C1 N1 -142.98(17) 15_566 . . . ? Cu1 S2 C1 N1 -41.4(2) . . . . ? Cu1 S2 C1 N2 39.90(17) 15_566 . . . ? Cu1 S2 C1 N2 141.51(15) . . . . ? P1 O1 C2 C3 78.8(3) . . . . ? P1 O1 C2 C4 -157.2(2) . . . . ? P1 O2 C5 C6 -142.3(3) . . . . ? P1 O2 C5 C7 96.2(3) . . . . ? C1 N2 C11 N12 -173.7(2) . . . . ? C1 N2 C11 C16 7.0(4) . . . . ? C16 C11 N12 C13 -1.4(3) . . . . ? N2 C11 N12 C13 179.2(2) . . . . ? C11 N12 C13 C14 -0.2(3) . . . . ? C11 N12 C13 C17 178.0(2) . . . . ? N12 C13 C14 C15 1.6(4) . . . . ? C17 C13 C14 C15 -176.5(3) . . . . ? C13 C14 C15 C16 -1.5(4) . . . . ? C14 C15 C16 C11 0.0(3) . . . . ? N12 C11 C16 C15 1.5(3) . . . . ? N2 C11 C16 C15 -179.2(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2 S1 0.81(3) 2.85(3) 3.443(2) 132(2) 15_566 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.410 _refine_diff_density_min -0.276 _refine_diff_density_rms 0.048