# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 #TrackingRef '18802_web_deposit_cif_file_0_Chien-Nan,Lin_1364080827.1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H25 Cu2 Fe3 N O9 P2 S' _chemical_formula_sum 'C36 H25 Cu2 Fe3 N O9 P2 S' _chemical_formula_weight 1004.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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' _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 11.4929(6) _cell_length_b 12.3565(6) _cell_length_c 15.8187(8) _cell_angle_alpha 67.9240(10) _cell_angle_beta 73.6060(10) _cell_angle_gamma 77.9750(10) _cell_volume 1983.86(17) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.681 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1004 _exptl_absorpt_coefficient_mu 2.311 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3150 _exptl_absorpt_correction_T_max 0.3912 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12650 _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_av_sigmaI/netI 0.0421 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6884 _reflns_number_gt 5824 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1099P)^2^+9.5008P] 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 fixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6884 _refine_ls_number_parameters 488 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0448 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.1182 _refine_ls_wR_factor_gt 0.0912 _refine_ls_goodness_of_fit_ref 0.621 _refine_ls_restrained_S_all 0.621 _refine_ls_shift/su_max 0.046 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.0318(4) 0.6628(4) 0.4068(3) 0.0466(10) Uani 1 1 d . . . C2 C 0.1869(4) 0.6516(4) 0.4453(3) 0.0491(10) Uani 1 1 d . . . C3 C 0.0412(4) 0.8464(4) 0.4122(3) 0.0437(9) Uani 1 1 d . . . C4 C -0.0955(4) 0.8648(4) 0.2216(3) 0.0526(11) Uani 1 1 d . . . C5 C 0.0698(5) 0.8290(5) 0.0791(3) 0.0673(14) Uani 1 1 d . . . C6 C -0.0285(6) 0.6481(5) 0.2225(4) 0.0687(14) Uani 1 1 d . . . C7 C 0.2556(6) 0.5666(5) 0.1561(4) 0.0769(18) Uani 1 1 d . . . C8 C 0.1258(5) 0.4777(4) 0.3293(3) 0.0529(11) Uani 1 1 d . . . C9 C 0.3395(5) 0.5407(5) 0.3073(5) 0.0786(18) Uani 1 1 d . . . C10 C 0.5189(5) 0.7138(4) 0.3559(4) 0.0642(14) Uani 1 1 d . . . C11 C 0.6295(7) 0.6373(7) 0.3750(8) 0.128(3) Uani 1 1 d . . . H11A H 0.6087 0.5677 0.4274 0.192 Uiso 1 1 calc R . . H11B H 0.6804 0.6777 0.3892 0.192 Uiso 1 1 calc R . . H11C H 0.6726 0.6159 0.3210 0.192 Uiso 1 1 calc R . . C12 C 0.3229(3) 1.0762(3) 0.3919(3) 0.0357(8) Uani 1 1 d . . . C13 C 0.2851(5) 0.9985(4) 0.4804(3) 0.0576(12) Uani 1 1 d . . . H13 H 0.2432 0.9371 0.4887 0.069 Uiso 1 1 calc R . . C14 C 0.3087(5) 1.0110(5) 0.5572(3) 0.0691(14) Uani 1 1 d . . . H14 H 0.2819 0.9586 0.6169 0.083 Uiso 1 1 calc R . . C15 C 0.3706(5) 1.0990(5) 0.5457(4) 0.0662(14) Uani 1 1 d . . . H15 H 0.3865 1.1070 0.5973 0.079 Uiso 1 1 calc R . . C16 C 0.4096(7) 1.1759(6) 0.4586(4) 0.087(2) Uani 1 1 d . . . H16 H 0.4528 1.2360 0.4509 0.105 Uiso 1 1 calc R . . C17 C 0.3856(6) 1.1653(5) 0.3816(4) 0.0710(16) Uani 1 1 d . . . H17 H 0.4119 1.2189 0.3223 0.085 Uiso 1 1 calc R . . C18 C 0.3916(4) 1.1263(3) 0.1894(3) 0.0408(9) Uani 1 1 d . . . C19 C 0.4817(6) 1.0548(5) 0.1527(5) 0.091(2) Uani 1 1 d . . . H19 H 0.4871 0.9739 0.1834 0.109 Uiso 1 1 calc R . . C20 C 0.5655(7) 1.1013(6) 0.0698(6) 0.128(4) Uani 1 1 d . . . H20 H 0.6275 1.0512 0.0466 0.154 Uiso 1 1 calc R . . C21 C 0.5585(7) 1.2161(6) 0.0234(4) 0.095(2) Uani 1 1 d . . . H21 H 0.6135 1.2458 -0.0332 0.114 Uiso 1 1 calc R . . C22 C 0.4700(5) 1.2908(5) 0.0591(4) 0.0655(13) Uani 1 1 d . . . H22 H 0.4660 1.3715 0.0275 0.079 Uiso 1 1 calc R . . C23 C 0.3867(4) 1.2460(4) 0.1419(3) 0.0479(10) Uani 1 1 d . . . H23 H 0.3269 1.2969 0.1660 0.057 Uiso 1 1 calc R . . C24 C 0.1371(3) 1.1527(3) 0.2905(3) 0.0336(7) Uani 1 1 d . . . H24A H 0.0861 1.1366 0.3532 0.040 Uiso 1 1 calc R . . H24B H 0.1531 1.2341 0.2672 0.040 Uiso 1 1 calc R . . C25 C 0.1249(4) 1.2188(4) 0.0972(3) 0.0410(9) Uani 1 1 d . . . C26 C 0.1976(5) 1.1631(5) 0.0362(3) 0.0609(12) Uani 1 1 d . . . H26 H 0.2071 1.0815 0.0545 0.073 Uiso 1 1 calc R . . C27 C 0.2565(7) 1.2296(7) -0.0526(4) 0.089(2) Uani 1 1 d . . . H27 H 0.3055 1.1920 -0.0936 0.107 Uiso 1 1 calc R . . C28 C 0.2431(7) 1.3490(7) -0.0800(4) 0.090(2) Uani 1 1 d . . . H28 H 0.2838 1.3925 -0.1393 0.108 Uiso 1 1 calc R . . C29 C 0.1708(6) 1.4051(5) -0.0213(4) 0.0786(17) Uani 1 1 d . . . H29 H 0.1615 1.4868 -0.0408 0.094 Uiso 1 1 calc R . . C30 C 0.1110(5) 1.3415(4) 0.0673(4) 0.0596(12) Uani 1 1 d . . . H30 H 0.0615 1.3805 0.1072 0.071 Uiso 1 1 calc R . . C31 C -0.0959(3) 1.2110(3) 0.2380(3) 0.0370(8) Uani 1 1 d . . . C32 C -0.1344(4) 1.2713(4) 0.3002(4) 0.0626(13) Uani 1 1 d . . . H32 H -0.0822 1.2731 0.3350 0.075 Uiso 1 1 calc R . . C33 C -0.2525(5) 1.3298(5) 0.3104(5) 0.0785(17) Uani 1 1 d . . . H33 H -0.2785 1.3712 0.3521 0.094 Uiso 1 1 calc R . . C34 C -0.3291(5) 1.3274(5) 0.2614(5) 0.0749(16) Uani 1 1 d . . . H34 H -0.4072 1.3677 0.2688 0.090 Uiso 1 1 calc R . . C35 C -0.2939(5) 1.2670(6) 0.2014(4) 0.0779(17) Uani 1 1 d . . . H35 H -0.3478 1.2649 0.1681 0.093 Uiso 1 1 calc R . . C36 C -0.1777(4) 1.2083(5) 0.1895(4) 0.0618(13) Uani 1 1 d . . . H36 H -0.1541 1.1663 0.1482 0.074 Uiso 1 1 calc R . . Cu1 Cu 0.27835(4) 0.87113(4) 0.30965(4) 0.03984(14) Uani 1 1 d . . . Cu2 Cu 0.06550(5) 0.94334(4) 0.24059(4) 0.04309(15) Uani 1 1 d . . . Fe1 Fe 0.10163(4) 0.73619(4) 0.35980(3) 0.02935(14) Uani 1 1 d . . . Fe2 Fe 0.04200(5) 0.77185(5) 0.20295(4) 0.03887(15) Uani 1 1 d . . . Fe3 Fe 0.20782(6) 0.60130(5) 0.26135(5) 0.04609(17) Uani 1 1 d . . . N1 N 0.4328(4) 0.7717(3) 0.3418(3) 0.0627(11) Uani 1 1 d . . . O1 O -0.1188(3) 0.6183(4) 0.4415(3) 0.0750(11) Uani 1 1 d . . . O2 O 0.2384(4) 0.5994(3) 0.5030(3) 0.0807(12) Uani 1 1 d . . . O3 O 0.0020(4) 0.9050(3) 0.4579(3) 0.0712(10) Uani 1 1 d . . . O4 O -0.1924(4) 0.9134(4) 0.2315(3) 0.0864(12) Uani 1 1 d . . . O5 O 0.0871(5) 0.8702(6) -0.0006(3) 0.1181(19) Uani 1 1 d . . . O6 O -0.0821(5) 0.5738(4) 0.2314(4) 0.1132(19) Uani 1 1 d . . . O7 O 0.2839(6) 0.5428(4) 0.0902(4) 0.134(2) Uani 1 1 d . . . O8 O 0.0768(4) 0.3951(3) 0.3708(3) 0.0761(11) Uani 1 1 d . . . O9 O 0.4252(5) 0.5002(5) 0.3379(5) 0.130(2) Uani 1 1 d . . . P1 P 0.28237(8) 1.05701(8) 0.29547(6) 0.0313(2) Uani 1 1 d . . . P2 P 0.05479(8) 1.13178(8) 0.21507(6) 0.0321(2) Uani 1 1 d . . . S1 S 0.22462(9) 0.79002(8) 0.21560(6) 0.0365(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.050(2) 0.049(2) 0.041(2) -0.0102(18) -0.0087(18) -0.017(2) C2 0.053(2) 0.037(2) 0.054(3) -0.0054(19) -0.016(2) -0.0099(18) C3 0.048(2) 0.042(2) 0.040(2) -0.0170(18) -0.0036(17) -0.0065(18) C4 0.055(3) 0.059(3) 0.049(2) -0.019(2) -0.016(2) -0.009(2) C5 0.078(4) 0.086(4) 0.046(3) -0.031(3) -0.012(2) -0.010(3) C6 0.088(4) 0.056(3) 0.078(4) -0.017(3) -0.044(3) -0.018(3) C7 0.102(4) 0.052(3) 0.078(4) -0.045(3) 0.022(3) -0.029(3) C8 0.068(3) 0.037(2) 0.058(3) -0.020(2) -0.017(2) -0.004(2) C9 0.058(3) 0.046(3) 0.146(6) -0.054(3) -0.024(3) 0.007(2) C10 0.051(3) 0.043(2) 0.105(4) -0.022(3) -0.038(3) 0.006(2) C11 0.090(5) 0.106(6) 0.225(10) -0.080(6) -0.102(6) 0.050(4) C12 0.0323(18) 0.0380(19) 0.039(2) -0.0150(16) -0.0110(15) -0.0019(15) C13 0.068(3) 0.061(3) 0.047(2) -0.010(2) -0.016(2) -0.026(2) C14 0.084(4) 0.083(4) 0.039(2) -0.010(2) -0.016(2) -0.021(3) C15 0.071(3) 0.091(4) 0.053(3) -0.035(3) -0.023(2) -0.012(3) C16 0.126(5) 0.091(4) 0.070(4) -0.026(3) -0.030(4) -0.055(4) C17 0.107(4) 0.067(3) 0.051(3) -0.011(2) -0.023(3) -0.046(3) C18 0.039(2) 0.041(2) 0.041(2) -0.0132(17) -0.0060(16) -0.0069(16) C19 0.089(4) 0.048(3) 0.093(4) -0.020(3) 0.039(3) -0.003(3) C20 0.117(6) 0.077(4) 0.125(6) -0.035(4) 0.077(5) -0.015(4) C21 0.106(5) 0.083(4) 0.070(4) -0.024(3) 0.036(4) -0.038(4) C22 0.073(3) 0.058(3) 0.055(3) -0.003(2) -0.006(2) -0.026(3) C23 0.046(2) 0.042(2) 0.051(2) -0.0088(19) -0.0104(19) -0.0091(18) C24 0.0336(18) 0.0316(18) 0.0367(19) -0.0134(15) -0.0094(15) -0.0001(14) C25 0.042(2) 0.043(2) 0.038(2) -0.0083(17) -0.0169(16) -0.0038(17) C26 0.076(3) 0.063(3) 0.045(2) -0.021(2) -0.009(2) -0.008(2) C27 0.103(5) 0.117(6) 0.044(3) -0.031(3) 0.003(3) -0.023(4) C28 0.105(5) 0.105(5) 0.045(3) 0.008(3) -0.017(3) -0.041(4) C29 0.089(4) 0.061(3) 0.068(4) 0.018(3) -0.035(3) -0.023(3) C30 0.063(3) 0.047(3) 0.059(3) -0.002(2) -0.023(2) -0.002(2) C31 0.0354(19) 0.0295(18) 0.044(2) -0.0101(15) -0.0110(16) 0.0005(15) C32 0.050(3) 0.064(3) 0.095(4) -0.053(3) -0.023(2) 0.009(2) C33 0.054(3) 0.079(4) 0.125(5) -0.074(4) -0.014(3) 0.013(3) C34 0.041(3) 0.067(3) 0.110(5) -0.032(3) -0.015(3) 0.010(2) C35 0.046(3) 0.107(5) 0.088(4) -0.039(4) -0.033(3) 0.012(3) C36 0.049(3) 0.085(4) 0.062(3) -0.038(3) -0.026(2) 0.015(2) Cu1 0.0367(3) 0.0286(2) 0.0577(3) -0.0154(2) -0.0165(2) -0.00136(18) Cu2 0.0532(3) 0.0272(2) 0.0533(3) -0.0152(2) -0.0198(2) 0.0001(2) Fe1 0.0335(3) 0.0252(2) 0.0292(3) -0.00845(19) -0.0067(2) -0.00494(19) Fe2 0.0506(3) 0.0376(3) 0.0349(3) -0.0155(2) -0.0125(2) -0.0087(2) Fe3 0.0505(4) 0.0317(3) 0.0596(4) -0.0261(3) -0.0037(3) -0.0037(2) N1 0.048(2) 0.0383(19) 0.105(3) -0.018(2) -0.035(2) 0.0006(17) O1 0.063(2) 0.095(3) 0.065(2) -0.012(2) -0.0041(17) -0.048(2) O2 0.091(3) 0.067(2) 0.080(3) 0.005(2) -0.056(2) -0.007(2) O3 0.087(3) 0.067(2) 0.064(2) -0.0456(19) 0.0088(18) -0.0095(19) O4 0.053(2) 0.101(3) 0.110(3) -0.048(3) -0.022(2) 0.008(2) O5 0.144(5) 0.166(5) 0.039(2) -0.032(3) -0.014(2) -0.020(4) O6 0.142(4) 0.069(3) 0.162(5) -0.016(3) -0.096(4) -0.039(3) O7 0.210(6) 0.096(3) 0.098(4) -0.074(3) 0.048(4) -0.061(4) O8 0.105(3) 0.049(2) 0.072(2) -0.0114(18) -0.017(2) -0.026(2) O9 0.090(3) 0.089(3) 0.250(8) -0.093(4) -0.086(4) 0.043(3) P1 0.0306(4) 0.0278(4) 0.0365(5) -0.0112(4) -0.0087(4) -0.0033(3) P2 0.0341(5) 0.0264(4) 0.0369(5) -0.0111(4) -0.0126(4) 0.0014(4) S1 0.0400(5) 0.0327(4) 0.0371(5) -0.0173(4) 0.0019(4) -0.0088(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.139(5) . ? C1 Fe1 1.776(4) . ? C2 O2 1.141(5) . ? C2 Fe1 1.772(4) . ? C3 O3 1.151(5) . ? C3 Fe1 1.776(4) . ? C3 Cu2 2.479(4) . ? C4 O4 1.148(6) . ? C4 Fe2 1.772(5) . ? C4 Cu2 2.396(5) . ? C5 O5 1.143(6) . ? C5 Fe2 1.772(5) . ? C6 O6 1.154(6) . ? C6 Fe2 1.763(5) . ? C7 O7 1.130(7) . ? C7 Fe3 1.783(5) . ? C8 O8 1.148(6) . ? C8 Fe3 1.780(5) . ? C9 O9 1.156(7) . ? C9 Fe3 1.766(6) . ? C10 N1 1.118(6) . ? C10 C11 1.449(7) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C17 1.374(6) . ? C12 C13 1.375(6) . ? C12 P1 1.821(4) . ? C13 C14 1.386(7) . ? C13 H13 0.9300 . ? C14 C15 1.349(8) . ? C14 H14 0.9300 . ? C15 C16 1.358(8) . ? C15 H15 0.9300 . ? C16 C17 1.380(7) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.362(6) . ? C18 C23 1.382(6) . ? C18 P1 1.817(4) . ? C19 C20 1.389(8) . ? C19 H19 0.9300 . ? C20 C21 1.327(9) . ? C20 H20 0.9300 . ? C21 C22 1.372(8) . ? C21 H21 0.9300 . ? C22 C23 1.381(6) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 P2 1.832(4) . ? C24 P1 1.836(4) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C30 1.396(6) . ? C25 C26 1.381(6) . ? C25 P2 1.813(4) . ? C26 C27 1.391(8) . ? C26 H26 0.9300 . ? C27 C28 1.361(10) . ? C27 H27 0.9300 . ? C28 C29 1.357(10) . ? C28 H28 0.9300 . ? C29 C30 1.382(7) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C36 1.383(6) . ? C31 C32 1.373(6) . ? C31 P2 1.815(4) . ? C32 C33 1.396(7) . ? C32 H32 0.9300 . ? C33 C34 1.339(8) . ? C33 H33 0.9300 . ? C34 C35 1.344(8) . ? C34 H34 0.9300 . ? C35 C36 1.379(7) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? Cu1 N1 2.012(4) . ? Cu1 P1 2.2314(10) . ? Cu1 S1 2.3445(10) . ? Cu1 Fe1 2.6536(7) . ? Cu1 Cu2 2.8000(7) . ? Cu2 P2 2.1913(10) . ? Cu2 S1 2.4085(10) . ? Cu2 Fe2 2.4892(7) . ? Cu2 Fe1 2.5790(7) . ? Fe1 S1 2.2527(10) . ? Fe1 Fe3 2.5930(7) . ? Fe1 Fe2 2.6140(7) . ? Fe2 S1 2.2278(11) . ? Fe2 Fe3 2.6046(9) . ? Fe3 S1 2.1998(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 Fe1 175.7(4) . . ? O2 C2 Fe1 177.0(5) . . ? O3 C3 Fe1 170.3(4) . . ? O3 C3 Cu2 117.2(3) . . ? Fe1 C3 Cu2 72.49(13) . . ? O4 C4 Fe2 169.9(4) . . ? O4 C4 Cu2 118.5(4) . . ? Fe2 C4 Cu2 71.58(16) . . ? O5 C5 Fe2 177.3(6) . . ? O6 C6 Fe2 174.1(5) . . ? O7 C7 Fe3 178.4(5) . . ? O8 C8 Fe3 176.9(4) . . ? O9 C9 Fe3 179.4(7) . . ? N1 C10 C11 179.2(7) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C17 C12 C13 118.4(4) . . ? C17 C12 P1 123.9(3) . . ? C13 C12 P1 117.6(3) . . ? C12 C13 C14 120.5(4) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C15 C14 C13 120.2(5) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 120.1(5) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C17 120.4(5) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C12 C17 C16 120.4(5) . . ? C12 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C19 C18 C23 118.0(4) . . ? C19 C18 P1 117.6(3) . . ? C23 C18 P1 124.4(3) . . ? C18 C19 C20 120.7(5) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C21 C20 C19 121.0(6) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C20 C21 C22 119.8(5) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C21 C22 C23 119.9(5) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C22 C23 C18 120.6(4) . . ? C22 C23 H23 119.7 . . ? C18 C23 H23 119.7 . . ? P2 C24 P1 112.48(19) . . ? P2 C24 H24A 109.1 . . ? P1 C24 H24A 109.1 . . ? P2 C24 H24B 109.1 . . ? P1 C24 H24B 109.1 . . ? H24A C24 H24B 107.8 . . ? C30 C25 C26 118.8(4) . . ? C30 C25 P2 121.6(3) . . ? C26 C25 P2 119.6(3) . . ? C27 C26 C25 119.7(5) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C28 C27 C26 120.6(6) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C27 C28 C29 120.4(5) . . ? C27 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? C28 C29 C30 120.3(6) . . ? C28 C29 H29 119.8 . . ? C30 C29 H29 119.8 . . ? C25 C30 C29 120.1(5) . . ? C25 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C36 C31 C32 118.2(4) . . ? C36 C31 P2 116.8(3) . . ? C32 C31 P2 125.0(3) . . ? C31 C32 C33 119.3(5) . . ? C31 C32 H32 120.4 . . ? C33 C32 H32 120.4 . . ? C34 C33 C32 121.2(5) . . ? C34 C33 H33 119.4 . . ? C32 C33 H33 119.4 . . ? C35 C34 C33 120.4(5) . . ? C35 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? C34 C35 C36 119.9(5) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C31 C36 C35 121.0(5) . . ? C31 C36 H36 119.5 . . ? C35 C36 H36 119.5 . . ? N1 Cu1 P1 110.59(11) . . ? N1 Cu1 S1 104.39(13) . . ? P1 Cu1 S1 131.73(4) . . ? N1 Cu1 Fe1 110.04(11) . . ? P1 Cu1 Fe1 134.16(3) . . ? S1 Cu1 Fe1 53.14(3) . . ? N1 Cu1 Cu2 159.02(12) . . ? P1 Cu1 Cu2 88.70(3) . . ? S1 Cu1 Cu2 54.97(3) . . ? Fe1 Cu1 Cu2 56.369(17) . . ? P2 Cu2 C4 120.67(12) . . ? P2 Cu2 S1 135.96(4) . . ? C4 Cu2 S1 96.53(12) . . ? P2 Cu2 C3 105.59(10) . . ? C4 Cu2 C3 98.42(15) . . ? S1 Cu2 C3 89.84(10) . . ? P2 Cu2 Fe2 153.59(4) . . ? C4 Cu2 Fe2 42.48(12) . . ? S1 Cu2 Fe2 54.08(3) . . ? C3 Cu2 Fe2 98.07(10) . . ? P2 Cu2 Fe1 144.13(3) . . ? C4 Cu2 Fe1 84.13(11) . . ? S1 Cu2 Fe1 53.57(3) . . ? C3 Cu2 Fe1 41.04(9) . . ? Fe2 Cu2 Fe1 62.07(2) . . ? P2 Cu2 Cu1 97.83(3) . . ? C4 Cu2 Cu1 141.05(12) . . ? S1 Cu2 Cu1 52.85(3) . . ? C3 Cu2 Cu1 62.74(10) . . ? Fe2 Cu2 Cu1 103.40(2) . . ? Fe1 Cu2 Cu1 58.947(17) . . ? C2 Fe1 C1 99.77(19) . . ? C2 Fe1 C3 94.1(2) . . ? C1 Fe1 C3 94.8(2) . . ? C2 Fe1 S1 110.91(15) . . ? C1 Fe1 S1 132.40(14) . . ? C3 Fe1 S1 117.44(13) . . ? C2 Fe1 Cu2 143.16(14) . . ? C1 Fe1 Cu2 112.28(14) . . ? C3 Fe1 Cu2 66.47(13) . . ? S1 Fe1 Cu2 59.34(3) . . ? C2 Fe1 Fe3 89.69(15) . . ? C1 Fe1 Fe3 92.75(14) . . ? C3 Fe1 Fe3 170.87(13) . . ? S1 Fe1 Fe3 53.44(3) . . ? Cu2 Fe1 Fe3 105.84(2) . . ? C2 Fe1 Fe2 149.67(15) . . ? C1 Fe1 Fe2 81.38(14) . . ? C3 Fe1 Fe2 116.14(14) . . ? S1 Fe1 Fe2 53.87(3) . . ? Cu2 Fe1 Fe2 57.279(19) . . ? Fe3 Fe1 Fe2 60.03(2) . . ? C2 Fe1 Cu1 80.36(14) . . ? C1 Fe1 Cu1 168.97(15) . . ? C3 Fe1 Cu1 74.20(13) . . ? S1 Fe1 Cu1 56.38(3) . . ? Cu2 Fe1 Cu1 64.684(19) . . ? Fe3 Fe1 Cu1 98.28(2) . . ? Fe2 Fe1 Cu1 104.15(2) . . ? C6 Fe2 C5 98.8(3) . . ? C6 Fe2 C4 95.8(3) . . ? C5 Fe2 C4 95.4(2) . . ? C6 Fe2 S1 132.23(19) . . ? C5 Fe2 S1 97.20(19) . . ? C4 Fe2 S1 127.00(15) . . ? C6 Fe2 Cu2 153.5(2) . . ? C5 Fe2 Cu2 101.79(19) . . ? C4 Fe2 Cu2 65.94(15) . . ? S1 Fe2 Cu2 61.11(3) . . ? C6 Fe2 Fe3 78.81(18) . . ? C5 Fe2 Fe3 111.93(19) . . ? C4 Fe2 Fe3 152.66(15) . . ? S1 Fe2 Fe3 53.47(3) . . ? Cu2 Fe2 Fe3 108.18(3) . . ? C6 Fe2 Fe1 105.66(18) . . ? C5 Fe2 Fe1 151.09(19) . . ? C4 Fe2 Fe1 97.16(15) . . ? S1 Fe2 Fe1 54.75(3) . . ? Cu2 Fe2 Fe1 60.654(19) . . ? Fe3 Fe2 Fe1 59.59(2) . . ? C9 Fe3 C7 99.6(3) . . ? C9 Fe3 C8 95.3(2) . . ? C7 Fe3 C8 96.3(2) . . ? C9 Fe3 S1 100.42(17) . . ? C7 Fe3 S1 104.54(17) . . ? C8 Fe3 S1 151.21(15) . . ? C9 Fe3 Fe1 100.25(19) . . ? C7 Fe3 Fe1 154.0(2) . . ? C8 Fe3 Fe1 98.31(15) . . ? S1 Fe3 Fe1 55.34(3) . . ? C9 Fe3 Fe2 153.64(16) . . ? C7 Fe3 Fe2 95.2(2) . . ? C8 Fe3 Fe2 104.66(16) . . ? S1 Fe3 Fe2 54.47(3) . . ? Fe1 Fe3 Fe2 60.39(2) . . ? C10 N1 Cu1 176.1(5) . . ? C18 P1 C12 106.96(18) . . ? C18 P1 C24 106.48(18) . . ? C12 P1 C24 101.12(16) . . ? C18 P1 Cu1 110.01(14) . . ? C12 P1 Cu1 115.27(13) . . ? C24 P1 Cu1 116.14(12) . . ? C25 P2 C31 103.83(18) . . ? C25 P2 C24 104.90(18) . . ? C31 P2 C24 105.10(17) . . ? C25 P2 Cu2 115.33(14) . . ? C31 P2 Cu2 117.46(13) . . ? C24 P2 Cu2 109.06(12) . . ? Fe3 S1 Fe2 72.06(3) . . ? Fe3 S1 Fe1 71.22(3) . . ? Fe2 S1 Fe1 71.38(3) . . ? Fe3 S1 Cu1 121.65(5) . . ? Fe2 S1 Cu1 130.66(4) . . ? Fe1 S1 Cu1 70.48(3) . . ? Fe3 S1 Cu2 127.06(4) . . ? Fe2 S1 Cu2 64.81(3) . . ? Fe1 S1 Cu2 67.09(3) . . ? Cu1 S1 Cu2 72.17(3) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.672 _refine_diff_density_min -0.772 _refine_diff_density_rms 0.231 _database_code_depnum_ccdc_archive 'CCDC 930774' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 #TrackingRef '18803_web_deposit_cif_file_1_Chien-Nan,Lin_1364080827.2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H24 Cu2 Fe3 O9 P2 S' _chemical_formula_sum 'C35 H24 Cu2 Fe3 O9 P2 S' _chemical_formula_weight 977.17 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' Fe Fe 0.3463 0.8444 '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' 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' O O 0.0106 0.0060 '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 13.1357(2) _cell_length_b 13.7196(2) _cell_length_c 20.6528(4) _cell_angle_alpha 97.8100(10) _cell_angle_beta 90.0210(10) _cell_angle_gamma 91.1150(10) _cell_volume 3686.74(11) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 60661 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 25.028 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.761 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 2.484 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4572 _exptl_absorpt_correction_T_max 0.5679 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46495 _diffrn_reflns_av_R_equivalents 0.0878 _diffrn_reflns_av_sigmaI/netI 0.0598 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 25.11 _reflns_number_total 12946 _reflns_number_gt 10876 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0907P)^2^+66.7220P] 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 fixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0109(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12946 _refine_ls_number_parameters 932 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1129 _refine_ls_R_factor_gt 0.0975 _refine_ls_wR_factor_ref 0.2717 _refine_ls_wR_factor_gt 0.2603 _refine_ls_goodness_of_fit_ref 1.150 _refine_ls_restrained_S_all 1.150 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.0782(12) 0.3156(11) 0.9127(7) 0.056(4) Uani 1 1 d . . . C2 C 0.0940(13) 0.4036(10) 0.9531(7) 0.057(4) Uani 1 1 d . . . C3 C 0.0146(11) 0.4362(11) 0.8418(7) 0.052(3) Uani 1 1 d . . . C4 C 0.2971(10) 0.3172(11) 0.8989(6) 0.046(3) Uani 1 1 d . . . C5 C 0.2660(9) 0.3440(9) 0.7832(6) 0.038(3) Uani 1 1 d . . . C6 C 0.3045(12) 0.1561(11) 0.8134(7) 0.056(4) Uani 1 1 d . . . C7 C -0.0026(10) 0.1825(10) 0.7199(6) 0.045(3) Uani 1 1 d . . . C8 C 0.0910(11) 0.0424(11) 0.7797(7) 0.053(3) Uani 1 1 d . . . C9 C -0.0805(10) 0.1270(10) 0.8212(7) 0.049(3) Uani 1 1 d . . . C10 C 0.1319(9) 0.5393(9) 0.6837(6) 0.038(3) Uani 1 1 d . . . C11 C 0.2351(10) 0.5744(10) 0.6790(7) 0.049(3) Uani 1 1 d . . . H11 H 0.2882 0.5288 0.6658 0.058 Uiso 1 1 d R . . C12 C 0.2557(11) 0.6731(10) 0.6951(7) 0.053(3) Uani 1 1 d . . . H12 H 0.3240 0.6980 0.6916 0.064 Uiso 1 1 d R . . C13 C 0.1819(12) 0.7394(11) 0.7140(9) 0.065(4) Uani 1 1 d . . . H13 H 0.1985 0.8084 0.7230 0.078 Uiso 1 1 d R . . C14 C 0.0853(12) 0.7055(11) 0.7200(10) 0.071(5) Uani 1 1 d . . . H14 H 0.0335 0.7505 0.7368 0.085 Uiso 1 1 d R . . C15 C 0.0615(12) 0.6051(10) 0.7047(9) 0.066(4) Uani 1 1 d . . . H15 H -0.0074 0.5824 0.7092 0.079 Uiso 1 1 d R . . C16 C -0.0180(9) 0.4025(9) 0.6235(6) 0.042(3) Uani 1 1 d . . . C17 C -0.0241(10) 0.4051(10) 0.5564(6) 0.046(3) Uani 1 1 d . . . H17 H 0.0362 0.4116 0.5309 0.056 Uiso 1 1 d R . . C18 C -0.1178(15) 0.3994(11) 0.5264(8) 0.072(5) Uani 1 1 d . . . H18 H -0.1230 0.3977 0.4799 0.086 Uiso 1 1 d R . . C19 C -0.2059(13) 0.3934(11) 0.5609(10) 0.070(5) Uani 1 1 d . . . H19 H -0.2703 0.3898 0.5386 0.083 Uiso 1 1 d R . . C20 C -0.2037(10) 0.3960(12) 0.6278(8) 0.063(4) Uani 1 1 d . . . H20 H -0.2659 0.3937 0.6520 0.076 Uiso 1 1 d R . . C21 C -0.1100(9) 0.3984(11) 0.6593(7) 0.051(3) Uani 1 1 d . . . H21 H -0.1067 0.3977 0.7057 0.061 Uiso 1 1 d R . . C22 C 0.1922(9) 0.3601(9) 0.6079(6) 0.038(3) Uani 1 1 d . . . H22A H 0.1937 0.4005 0.5734 0.046 Uiso 1 1 d R . . H22B H 0.2583 0.3608 0.6277 0.046 Uiso 1 1 d R . . C23 C 0.1779(9) 0.2564(9) 0.5736(6) 0.039(3) Uani 1 1 d . . . H23A H 0.2086 0.2552 0.5314 0.047 Uiso 1 1 d R . . H23B H 0.1056 0.2464 0.5687 0.047 Uiso 1 1 d R . . C24 C 0.3682(9) 0.1653(9) 0.6023(6) 0.040(3) Uani 1 1 d . . . C25 C 0.4267(11) 0.2231(14) 0.6483(8) 0.073(5) Uani 1 1 d . . . H25 H 0.3960 0.2550 0.6875 0.087 Uiso 1 1 d R . . C26 C 0.5328(14) 0.2328(16) 0.6370(12) 0.102(8) Uani 1 1 d . . . H26 H 0.5743 0.2726 0.6690 0.123 Uiso 1 1 d R . . C27 C 0.5765(11) 0.1826(13) 0.5836(8) 0.067(4) Uani 1 1 d . . . H27 H 0.6484 0.1891 0.5766 0.080 Uiso 1 1 d R . . C28 C 0.5207(11) 0.1282(13) 0.5394(9) 0.069(4) Uani 1 1 d . . . H28 H 0.5524 0.0962 0.5006 0.083 Uiso 1 1 d R . . C29 C 0.4138(10) 0.1177(12) 0.5490(8) 0.061(4) Uani 1 1 d . . . H29 H 0.3739 0.0764 0.5169 0.073 Uiso 1 1 d R . . C30 C 0.1866(9) 0.0469(9) 0.5650(5) 0.036(2) Uani 1 1 d . . . C31 C 0.1719(12) 0.0430(11) 0.4969(7) 0.057(4) Uani 1 1 d . . . H31 H 0.1864 0.1005 0.4764 0.068 Uiso 1 1 d R . . C32 C 0.1376(13) -0.0437(11) 0.4612(7) 0.061(4) Uani 1 1 d . . . H32 H 0.1260 -0.0487 0.4150 0.074 Uiso 1 1 d R . . C33 C 0.1157(11) -0.1240(11) 0.4880(8) 0.061(4) Uani 1 1 d . . . H33 H 0.0948 -0.1834 0.4608 0.073 Uiso 1 1 d R . . C34 C 0.1277(15) -0.1209(12) 0.5575(9) 0.078(5) Uani 1 1 d . . . H34 H 0.1113 -0.1784 0.5775 0.093 Uiso 1 1 d R . . C35 C 0.1608(12) -0.0361(10) 0.5936(7) 0.054(3) Uani 1 1 d . . . H35 H 0.1651 -0.0319 0.6403 0.065 Uiso 1 1 d R . . C36 C 0.5456(12) 0.3089(13) 0.4166(7) 0.061(4) Uani 1 1 d . . . C37 C 0.3804(12) 0.3973(12) 0.4516(7) 0.059(4) Uani 1 1 d . . . C38 C 0.4692(11) 0.4290(11) 0.3417(7) 0.054(3) Uani 1 1 d . . . C39 C 0.4913(10) 0.1679(10) 0.2251(7) 0.050(3) Uani 1 1 d . . . C40 C 0.3779(14) 0.0302(13) 0.2816(7) 0.065(4) Uani 1 1 d . . . C41 C 0.5465(13) 0.1134(12) 0.3303(7) 0.064(4) Uani 1 1 d . . . C42 C 0.1775(13) 0.3113(12) 0.3904(7) 0.061(4) Uani 1 1 d . . . C43 C 0.2148(9) 0.3204(10) 0.2703(6) 0.044(3) Uani 1 1 d . . . C44 C 0.1685(11) 0.1403(11) 0.3101(6) 0.051(3) Uani 1 1 d . . . C45 C 0.5312(8) 0.3867(9) 0.1267(6) 0.037(3) Uani 1 1 d . . . C46 C 0.6173(10) 0.3799(10) 0.1640(7) 0.047(3) Uani 1 1 d . . . H46 H 0.6099 0.3757 0.2098 0.057 Uiso 1 1 d R . . C47 C 0.7126(10) 0.3791(12) 0.1353(7) 0.058(4) Uani 1 1 d . . . H47 H 0.7730 0.3757 0.1610 0.070 Uiso 1 1 d R . . C48 C 0.7207(10) 0.3817(11) 0.0674(8) 0.056(4) Uani 1 1 d . . . H48 H 0.7865 0.3795 0.0472 0.068 Uiso 1 1 d R . . C49 C 0.6370(10) 0.3885(10) 0.0312(7) 0.051(3) Uani 1 1 d . . . H49 H 0.6449 0.3905 -0.0149 0.062 Uiso 1 1 d R . . C50 C 0.5404(10) 0.3911(9) 0.0594(6) 0.044(3) Uani 1 1 d . . . H50 H 0.4800 0.3974 0.0342 0.053 Uiso 1 1 d R . . C51 C 0.3860(10) 0.5297(9) 0.1809(6) 0.041(3) Uani 1 1 d . . . C52 C 0.4665(10) 0.5963(10) 0.1665(9) 0.062(4) Uani 1 1 d . . . H52 H 0.5312 0.5704 0.1519 0.074 Uiso 1 1 d R . . C53 C 0.4440(13) 0.6956(12) 0.1704(11) 0.083(6) Uani 1 1 d . . . H53 H 0.4968 0.7409 0.1608 0.100 Uiso 1 1 d R . . C54 C 0.3500(13) 0.7309(11) 0.1912(9) 0.069(5) Uani 1 1 d . . . H54 H 0.3366 0.7999 0.1943 0.083 Uiso 1 1 d R . . C55 C 0.2753(13) 0.6658(11) 0.2023(9) 0.068(4) Uani 1 1 d . . . H55 H 0.2101 0.6906 0.2167 0.081 Uiso 1 1 d R . . C56 C 0.2935(11) 0.5668(10) 0.1972(9) 0.069(5) Uani 1 1 d . . . H56 H 0.2386 0.5229 0.2053 0.083 Uiso 1 1 d R . . C57 C 0.3124(9) 0.3582(9) 0.1052(6) 0.038(3) Uani 1 1 d . . . H57A H 0.2460 0.3621 0.1247 0.045 Uiso 1 1 d R . . H57B H 0.3163 0.4005 0.0719 0.045 Uiso 1 1 d R . . C58 C 0.3202(10) 0.2532(9) 0.0710(6) 0.041(3) Uani 1 1 d . . . H58A H 0.3918 0.2417 0.0659 0.049 Uiso 1 1 d R . . H58B H 0.2897 0.2543 0.0288 0.049 Uiso 1 1 d R . . C59 C 0.1258(9) 0.1581(9) 0.0930(5) 0.037(3) Uani 1 1 d . . . C60 C 0.0778(14) 0.2463(13) 0.0911(13) 0.105(8) Uani 1 1 d . . . H60 H 0.1167 0.3065 0.0926 0.126 Uiso 1 1 d R . . C61 C -0.0279(12) 0.2464(15) 0.0835(16) 0.131(12) Uani 1 1 d . . . H61 H -0.0589 0.3095 0.0851 0.157 Uiso 1 1 d R . . C62 C -0.0839(13) 0.1660(14) 0.0731(11) 0.085(4) Uani 1 1 d . . . H62 H -0.1565 0.1681 0.0687 0.103 Uiso 1 1 d R . . C63 C -0.0398(13) 0.0795(14) 0.0696(11) 0.085(4) Uani 1 1 d . . . H63 H -0.0791 0.0193 0.0618 0.103 Uiso 1 1 d R . . C64 C 0.0653(12) 0.0747(13) 0.0779(12) 0.089(7) Uani 1 1 d . . . H64 H 0.0959 0.0112 0.0740 0.107 Uiso 1 1 d R . . C65 C 0.3068(8) 0.0463(9) 0.0571(6) 0.036(2) Uani 1 1 d . . . C66 C 0.2980(11) 0.0375(10) -0.0100(6) 0.048(3) Uani 1 1 d . . . H66 H 0.2617 0.0868 -0.0290 0.058 Uiso 1 1 d R . . C67 C 0.3385(11) -0.0407(10) -0.0500(7) 0.055(3) Uani 1 1 d . . . H67 H 0.3322 -0.0439 -0.0965 0.066 Uiso 1 1 d R . . C68 C 0.3865(12) -0.1132(11) -0.0217(8) 0.060(4) Uani 1 1 d . . . H68 H 0.4150 -0.1693 -0.0478 0.072 Uiso 1 1 d R . . C69 C 0.3962(13) -0.1062(11) 0.0442(8) 0.064(4) Uani 1 1 d . . . H69 H 0.4293 -0.1574 0.0632 0.077 Uiso 1 1 d R . . C70 C 0.3567(11) -0.0253(11) 0.0836(7) 0.054(3) Uani 1 1 d . . . H70 H 0.3665 -0.0185 0.1301 0.065 Uiso 1 1 d R . . Fe1 Fe 0.04731(14) 0.33110(13) 0.88067(8) 0.0396(4) Uani 1 1 d . . . Fe2 Fe 0.22089(13) 0.25671(12) 0.83481(8) 0.0358(4) Uani 1 1 d . . . Fe3 Fe 0.04372(13) 0.16424(12) 0.79884(8) 0.0365(4) Uani 1 1 d . . . Fe4 Fe 0.42666(14) 0.32299(14) 0.38071(8) 0.0422(4) Uani 1 1 d . . . Fe5 Fe 0.42997(14) 0.15257(13) 0.30119(8) 0.0406(4) Uani 1 1 d . . . Fe6 Fe 0.25444(13) 0.24426(13) 0.32825(8) 0.0384(4) Uani 1 1 d . . . Cu1 Cu 0.09044(11) 0.33306(10) 0.76152(6) 0.0353(4) Uani 1 1 d . . . Cu2 Cu 0.18831(11) 0.17652(11) 0.71945(7) 0.0387(4) Uani 1 1 d . . . Cu3 Cu 0.39801(11) 0.32202(11) 0.26035(7) 0.0367(4) Uani 1 1 d . . . Cu4 Cu 0.29855(11) 0.16540(11) 0.21492(7) 0.0388(4) Uani 1 1 d . . . P1 P 0.0995(2) 0.4075(2) 0.66915(13) 0.0324(6) Uani 1 1 d . . . P2 P 0.2314(2) 0.1578(2) 0.61509(14) 0.0352(7) Uani 1 1 d . . . P3 P 0.4088(2) 0.3973(2) 0.16876(14) 0.0334(6) Uani 1 1 d . . . P4 P 0.2601(2) 0.1534(2) 0.11019(14) 0.0340(6) Uani 1 1 d . . . S1 S 0.1100(2) 0.1905(2) 0.89728(14) 0.0421(7) Uani 1 1 d . . . S2 S 0.3543(3) 0.1830(3) 0.39629(15) 0.0465(8) Uani 1 1 d . . . O1 O -0.1575(9) 0.3050(10) 0.9335(6) 0.079(3) Uani 1 1 d . . . O2 O 0.1220(9) 0.4506(9) 0.9991(5) 0.072(3) Uani 1 1 d . . . O3 O -0.0126(12) 0.5104(9) 0.8292(6) 0.090(4) Uani 1 1 d . . . O4 O 0.3446(8) 0.3595(9) 0.9399(5) 0.069(3) Uani 1 1 d . . . O5 O 0.3100(7) 0.3993(7) 0.7571(4) 0.052(2) Uani 1 1 d . . . O6 O 0.3609(9) 0.0924(9) 0.8051(6) 0.074(3) Uani 1 1 d . . . O7 O -0.0441(8) 0.1815(8) 0.6710(5) 0.063(3) Uani 1 1 d . . . O8 O 0.1169(10) -0.0362(8) 0.7689(6) 0.078(3) Uani 1 1 d . . . O9 O -0.1622(8) 0.1017(9) 0.8333(6) 0.073(3) Uani 1 1 d . . . O36 O 0.6249(9) 0.2989(10) 0.4426(6) 0.085(4) Uani 1 1 d . . . O37 O 0.3530(10) 0.4425(9) 0.4997(5) 0.080(3) Uani 1 1 d . . . O38 O 0.4993(10) 0.5009(9) 0.3297(5) 0.076(3) Uani 1 1 d . . . O39 O 0.5362(8) 0.1661(8) 0.1772(5) 0.068(3) Uani 1 1 d . . . O40 O 0.3431(13) -0.0471(8) 0.2734(7) 0.096(5) Uani 1 1 d . . . O41 O 0.6234(10) 0.0849(12) 0.3467(7) 0.105(5) Uani 1 1 d . . . O42 O 0.1231(9) 0.3497(10) 0.4286(5) 0.081(4) Uani 1 1 d . . . O43 O 0.1734(7) 0.3715(8) 0.2390(5) 0.064(3) Uani 1 1 d . . . O44 O 0.1120(10) 0.0766(9) 0.2998(7) 0.085(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.065(10) 0.062(9) 0.035(7) -0.011(6) 0.018(7) 0.001(7) C2 0.075(10) 0.048(8) 0.046(8) 0.002(6) 0.000(7) -0.001(7) C3 0.058(8) 0.058(9) 0.039(7) -0.003(6) 0.008(6) 0.014(7) C4 0.040(7) 0.068(9) 0.031(6) 0.010(6) -0.005(5) -0.009(6) C5 0.033(6) 0.046(7) 0.033(6) 0.008(5) -0.010(5) -0.008(5) C6 0.061(9) 0.059(9) 0.047(8) 0.007(7) -0.005(7) -0.019(8) C7 0.040(7) 0.050(7) 0.042(7) -0.001(6) 0.000(6) -0.006(5) C8 0.056(8) 0.063(10) 0.040(7) 0.005(6) 0.004(6) -0.009(7) C9 0.043(7) 0.055(8) 0.047(8) 0.005(6) 0.004(6) -0.001(6) C10 0.040(6) 0.046(7) 0.030(6) 0.009(5) 0.004(5) 0.005(5) C11 0.044(7) 0.043(7) 0.058(8) 0.005(6) -0.003(6) 0.004(6) C12 0.054(8) 0.046(7) 0.062(9) 0.014(6) -0.004(7) -0.009(6) C13 0.062(9) 0.038(7) 0.094(12) 0.001(7) 0.009(8) 0.002(7) C14 0.055(9) 0.043(8) 0.114(15) 0.003(8) 0.011(9) 0.011(7) C15 0.054(9) 0.041(8) 0.101(13) 0.006(8) 0.006(8) 0.001(6) C16 0.040(7) 0.046(7) 0.038(7) 0.000(5) -0.006(5) 0.002(5) C17 0.045(7) 0.057(8) 0.038(7) 0.006(6) -0.001(5) 0.005(6) C18 0.104(14) 0.051(9) 0.058(10) -0.002(7) -0.046(10) 0.015(9) C19 0.058(10) 0.053(9) 0.094(13) 0.002(8) -0.037(10) -0.003(7) C20 0.026(6) 0.088(11) 0.074(11) 0.003(8) -0.015(6) 0.000(7) C21 0.032(6) 0.076(9) 0.044(7) 0.005(7) -0.001(5) -0.001(6) C22 0.031(6) 0.052(7) 0.033(6) 0.008(5) 0.008(5) 0.010(5) C23 0.036(6) 0.054(7) 0.030(6) 0.010(5) -0.003(5) 0.001(5) C24 0.039(6) 0.046(7) 0.034(6) 0.002(5) 0.001(5) 0.001(5) C25 0.042(8) 0.103(13) 0.063(10) -0.026(9) 0.009(7) -0.006(8) C26 0.054(10) 0.110(16) 0.124(18) -0.049(14) 0.008(11) -0.022(10) C27 0.034(7) 0.093(12) 0.073(11) 0.011(9) 0.002(7) -0.003(7) C28 0.044(8) 0.085(11) 0.076(11) 0.000(9) 0.021(8) 0.001(8) C29 0.032(7) 0.080(10) 0.065(9) -0.008(8) 0.000(6) 0.003(7) C30 0.037(6) 0.047(7) 0.021(5) -0.004(5) -0.003(4) 0.006(5) C31 0.078(10) 0.052(8) 0.042(7) 0.008(6) -0.005(7) -0.010(7) C32 0.085(11) 0.062(9) 0.032(7) -0.012(6) -0.022(7) 0.000(8) C33 0.055(9) 0.050(8) 0.073(10) -0.012(7) -0.014(7) 0.005(7) C34 0.106(14) 0.049(9) 0.080(12) 0.014(8) -0.035(11) -0.007(9) C35 0.066(9) 0.045(7) 0.050(8) 0.004(6) -0.003(7) 0.000(6) C36 0.057(9) 0.088(11) 0.034(7) 0.002(7) -0.010(6) -0.006(8) C37 0.066(9) 0.063(9) 0.047(8) 0.011(7) -0.012(7) -0.011(7) C38 0.058(9) 0.060(9) 0.043(8) 0.003(7) -0.004(6) -0.003(7) C39 0.045(7) 0.049(7) 0.056(9) 0.009(6) 0.001(6) 0.011(6) C40 0.082(11) 0.067(11) 0.043(8) -0.001(7) -0.016(7) 0.019(9) C41 0.071(10) 0.073(10) 0.049(8) 0.005(7) -0.017(7) 0.014(8) C42 0.067(10) 0.074(10) 0.044(8) 0.015(7) 0.009(7) 0.004(8) C43 0.027(6) 0.065(8) 0.041(7) 0.007(6) 0.015(5) 0.002(6) C44 0.053(8) 0.067(9) 0.034(7) 0.015(6) -0.008(6) -0.001(7) C45 0.028(6) 0.043(6) 0.038(6) 0.000(5) 0.004(5) -0.001(5) C46 0.042(7) 0.056(8) 0.042(7) 0.000(6) 0.000(5) 0.006(6) C47 0.036(7) 0.078(10) 0.058(9) -0.002(7) -0.001(6) 0.009(7) C48 0.035(7) 0.065(9) 0.066(10) -0.002(7) 0.010(6) -0.001(6) C49 0.049(8) 0.059(8) 0.045(7) 0.003(6) 0.017(6) 0.003(6) C50 0.046(7) 0.052(7) 0.035(6) 0.005(5) 0.000(5) -0.003(6) C51 0.047(7) 0.047(7) 0.030(6) 0.007(5) 0.004(5) 0.002(5) C52 0.027(6) 0.051(8) 0.105(13) -0.002(8) -0.004(7) -0.004(6) C53 0.055(10) 0.056(10) 0.138(18) 0.010(10) -0.027(11) -0.011(8) C54 0.075(11) 0.035(7) 0.095(13) 0.000(7) -0.028(9) 0.005(7) C55 0.067(10) 0.055(9) 0.082(12) 0.013(8) 0.018(9) 0.018(8) C56 0.049(8) 0.041(7) 0.114(14) 0.000(8) 0.046(9) 0.005(6) C57 0.039(6) 0.042(6) 0.034(6) 0.006(5) -0.003(5) 0.002(5) C58 0.042(7) 0.050(7) 0.030(6) 0.002(5) 0.004(5) -0.001(5) C59 0.032(6) 0.051(7) 0.028(6) 0.004(5) 0.004(5) 0.003(5) C60 0.060(11) 0.053(10) 0.19(3) -0.013(12) -0.040(13) 0.008(8) C61 0.031(8) 0.072(12) 0.27(3) -0.045(16) -0.039(13) 0.023(8) C62 0.049(7) 0.075(8) 0.135(12) 0.026(8) -0.018(7) -0.011(6) C63 0.049(7) 0.075(8) 0.135(12) 0.026(8) -0.018(7) -0.011(6) C64 0.042(9) 0.063(10) 0.17(2) 0.048(12) -0.021(11) -0.008(7) C65 0.029(6) 0.043(6) 0.037(6) 0.005(5) 0.008(5) -0.004(5) C66 0.066(9) 0.043(7) 0.035(7) 0.002(5) 0.005(6) 0.003(6) C67 0.060(9) 0.054(8) 0.049(8) 0.001(6) 0.018(7) -0.001(7) C68 0.059(9) 0.047(8) 0.070(10) -0.006(7) 0.019(7) 0.009(7) C69 0.078(11) 0.057(9) 0.059(9) 0.010(7) 0.013(8) 0.023(8) C70 0.061(9) 0.059(8) 0.043(7) 0.005(6) -0.001(6) 0.011(7) Fe1 0.0457(10) 0.0446(10) 0.0274(8) 0.0006(7) 0.0040(7) 0.0017(7) Fe2 0.0386(9) 0.0423(9) 0.0264(8) 0.0051(7) -0.0058(7) -0.0020(7) Fe3 0.0388(9) 0.0394(9) 0.0303(8) 0.0019(7) 0.0034(7) -0.0045(7) Fe4 0.0446(10) 0.0527(11) 0.0280(9) 0.0017(7) -0.0019(7) -0.0020(8) Fe5 0.0455(10) 0.0452(10) 0.0314(9) 0.0061(7) -0.0054(7) 0.0075(8) Fe6 0.0378(9) 0.0476(10) 0.0302(9) 0.0070(7) 0.0054(7) 0.0019(7) Cu1 0.0374(8) 0.0416(8) 0.0268(7) 0.0048(6) 0.0004(5) 0.0007(6) Cu2 0.0429(8) 0.0458(8) 0.0267(7) 0.0022(6) 0.0014(6) 0.0021(6) Cu3 0.0370(8) 0.0455(8) 0.0278(7) 0.0059(6) 0.0009(6) 0.0008(6) Cu4 0.0422(8) 0.0469(8) 0.0274(7) 0.0056(6) -0.0016(6) 0.0015(6) P1 0.0289(14) 0.0436(16) 0.0249(14) 0.0046(12) 0.0020(11) 0.0026(12) P2 0.0360(15) 0.0410(16) 0.0273(14) -0.0003(12) -0.0003(12) 0.0020(12) P3 0.0330(15) 0.0412(16) 0.0260(14) 0.0043(12) 0.0022(11) 0.0018(12) P4 0.0318(15) 0.0417(16) 0.0284(14) 0.0050(12) -0.0005(11) 0.0010(12) S1 0.0485(17) 0.0483(17) 0.0303(15) 0.0091(12) 0.0033(12) -0.0018(13) S2 0.0528(19) 0.060(2) 0.0287(15) 0.0118(14) -0.0015(13) -0.0012(15) O1 0.053(7) 0.121(10) 0.058(7) -0.004(7) 0.013(5) 0.008(6) O2 0.085(8) 0.083(8) 0.041(6) -0.016(5) -0.015(5) -0.003(6) O3 0.142(12) 0.061(7) 0.069(8) 0.012(6) 0.026(8) 0.046(8) O4 0.066(7) 0.099(8) 0.042(6) 0.018(5) -0.020(5) -0.028(6) O5 0.051(5) 0.060(6) 0.047(5) 0.017(5) -0.013(4) -0.015(5) O6 0.062(7) 0.064(7) 0.097(9) 0.007(6) -0.003(6) 0.019(6) O7 0.069(7) 0.067(6) 0.050(6) 0.002(5) -0.016(5) -0.023(5) O8 0.105(10) 0.043(6) 0.084(8) -0.002(5) 0.015(7) 0.022(6) O9 0.049(6) 0.089(8) 0.081(8) 0.014(6) 0.012(5) -0.017(6) O36 0.065(7) 0.118(10) 0.073(8) 0.021(7) -0.039(6) -0.010(7) O37 0.097(9) 0.092(9) 0.043(6) -0.013(6) 0.014(6) 0.004(7) O38 0.108(10) 0.063(7) 0.057(7) 0.010(5) -0.011(6) -0.034(7) O39 0.066(7) 0.073(7) 0.067(7) 0.013(6) 0.031(6) 0.027(5) O40 0.147(13) 0.037(6) 0.101(10) 0.000(6) -0.024(9) -0.011(7) O41 0.073(8) 0.131(12) 0.112(11) 0.014(9) -0.050(8) 0.043(8) O42 0.072(7) 0.126(10) 0.048(6) 0.011(6) 0.027(6) 0.040(7) O43 0.042(5) 0.088(7) 0.074(7) 0.050(6) 0.017(5) 0.024(5) O44 0.072(8) 0.069(7) 0.112(10) 0.008(7) 0.005(7) -0.030(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.141(17) . ? C1 Fe1 1.796(15) . ? C2 O2 1.130(17) . ? C2 Fe1 1.782(15) . ? C3 O3 1.147(17) . ? C3 Fe1 1.802(15) . ? C3 Cu1 2.272(13) . ? C4 O4 1.139(15) . ? C4 Fe2 1.763(13) . ? C5 O5 1.138(14) . ? C5 Fe2 1.800(12) . ? C5 Cu1 2.347(11) . ? C6 O6 1.151(19) . ? C6 Fe2 1.790(18) . ? C6 Cu2 2.517(15) . ? C7 O7 1.145(16) . ? C7 Fe3 1.791(14) . ? C7 Cu1 2.433(13) . ? C7 Cu2 2.511(13) . ? C8 O8 1.130(17) . ? C8 Fe3 1.788(16) . ? C9 O9 1.158(16) . ? C9 Fe3 1.781(13) . ? C10 C15 1.336(19) . ? C10 C11 1.438(18) . ? C10 P1 1.834(13) . ? C11 C12 1.372(19) . ? C11 H11 0.9601 . ? C12 C13 1.36(2) . ? C12 H12 0.9599 . ? C13 C14 1.35(2) . ? C13 H13 0.9600 . ? C14 C15 1.40(2) . ? C14 H14 0.9601 . ? C15 H15 0.9601 . ? C16 C17 1.394(17) . ? C16 C21 1.422(18) . ? C16 P1 1.803(12) . ? C17 C18 1.37(2) . ? C17 H17 0.9601 . ? C18 C19 1.37(3) . ? C18 H18 0.9600 . ? C19 C20 1.38(2) . ? C19 H19 0.9600 . ? C20 C21 1.390(18) . ? C20 H20 0.9600 . ? C21 H21 0.9600 . ? C22 C23 1.508(17) . ? C22 P1 1.821(11) . ? C22 H22A 0.9600 . ? C22 H22B 0.9598 . ? C23 P2 1.847(12) . ? C23 H23A 0.9598 . ? C23 H23B 0.9600 . ? C24 C29 1.349(19) . ? C24 C25 1.377(19) . ? C24 P2 1.819(12) . ? C25 C26 1.42(2) . ? C25 H25 0.9600 . ? C26 C27 1.35(2) . ? C26 H26 0.9600 . ? C27 C28 1.31(2) . ? C27 H27 0.9600 . ? C28 C29 1.43(2) . ? C28 H28 0.9601 . ? C29 H29 0.9599 . ? C30 C35 1.389(18) . ? C30 C31 1.414(17) . ? C30 P2 1.807(12) . ? C31 C32 1.379(19) . ? C31 H31 0.9600 . ? C32 C33 1.33(2) . ? C32 H32 0.9599 . ? C33 C34 1.44(2) . ? C33 H33 0.9599 . ? C34 C35 1.36(2) . ? C34 H34 0.9599 . ? C35 H35 0.9599 . ? C36 O36 1.190(18) . ? C36 Fe4 1.754(15) . ? C37 O37 1.159(18) . ? C37 Fe4 1.781(17) . ? C38 O38 1.115(17) . ? C38 Fe4 1.834(16) . ? C38 Cu3 2.263(14) . ? C39 O39 1.149(16) . ? C39 Fe5 1.803(15) . ? C39 Cu3 2.487(13) . ? C39 Cu4 2.539(14) . ? C40 O40 1.14(2) . ? C40 Fe5 1.795(18) . ? C41 O41 1.157(18) . ? C41 Fe5 1.764(15) . ? C42 O42 1.145(18) . ? C42 Fe6 1.798(16) . ? C43 O43 1.158(16) . ? C43 Fe6 1.777(14) . ? C43 Cu3 2.416(11) . ? C43 Cu4 2.545(13) . ? C44 O44 1.133(17) . ? C44 Fe6 1.801(15) . ? C45 C46 1.380(17) . ? C45 C50 1.406(17) . ? C45 P3 1.826(11) . ? C46 C47 1.384(19) . ? C46 H46 0.9599 . ? C47 C48 1.41(2) . ? C47 H47 0.9599 . ? C48 C49 1.34(2) . ? C48 H48 0.9601 . ? C49 C50 1.395(18) . ? C49 H49 0.9600 . ? C50 H50 0.9600 . ? C51 C56 1.351(18) . ? C51 C52 1.441(19) . ? C51 P3 1.831(13) . ? C52 C53 1.39(2) . ? C52 H52 0.9600 . ? C53 C54 1.38(3) . ? C53 H53 0.9599 . ? C54 C55 1.35(2) . ? C54 H54 0.9601 . ? C55 C56 1.37(2) . ? C55 H55 0.9599 . ? C56 H56 0.9599 . ? C57 C58 1.521(17) . ? C57 P3 1.843(12) . ? C57 H57A 0.9601 . ? C57 H57B 0.9600 . ? C58 P4 1.847(12) . ? C58 H58A 0.9601 . ? C58 H58B 0.9599 . ? C59 C64 1.38(2) . ? C59 C60 1.38(2) . ? C59 P4 1.803(12) . ? C60 C61 1.40(2) . ? C60 H60 0.9599 . ? C61 C62 1.31(3) . ? C61 H61 0.9599 . ? C62 C63 1.32(3) . ? C62 H62 0.9600 . ? C63 C64 1.39(2) . ? C63 H63 0.9599 . ? C64 H64 0.9601 . ? C65 C70 1.365(18) . ? C65 C66 1.380(17) . ? C65 P4 1.826(12) . ? C66 C67 1.378(18) . ? C66 H66 0.9599 . ? C67 C68 1.38(2) . ? C67 H67 0.9598 . ? C68 C69 1.36(2) . ? C68 H68 0.9601 . ? C69 C70 1.39(2) . ? C69 H69 0.9601 . ? C70 H70 0.9601 . ? Fe1 S1 2.181(4) . ? Fe1 Cu1 2.529(2) . ? Fe1 Fe2 2.639(2) . ? Fe1 Fe3 2.654(2) . ? Fe2 S1 2.209(3) . ? Fe2 Cu2 2.518(2) . ? Fe2 Cu1 2.612(2) . ? Fe2 Fe3 2.684(2) . ? Fe3 S1 2.193(3) . ? Fe3 Cu2 2.528(2) . ? Fe3 Cu1 2.601(2) . ? Fe4 S2 2.189(4) . ? Fe4 Cu3 2.512(2) . ? Fe4 Fe6 2.654(2) . ? Fe4 Fe5 2.670(2) . ? Fe5 S2 2.194(4) . ? Fe5 Cu4 2.506(2) . ? Fe5 Cu3 2.620(2) . ? Fe5 Fe6 2.671(2) . ? Fe6 S2 2.183(4) . ? Fe6 Cu4 2.514(2) . ? Fe6 Cu3 2.644(2) . ? Cu1 P1 2.285(3) . ? Cu1 Cu2 2.573(2) . ? Cu2 P2 2.211(3) . ? Cu3 P3 2.278(3) . ? Cu3 Cu4 2.559(2) . ? Cu4 P4 2.204(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 Fe1 179.2(16) . . ? O2 C2 Fe1 178.7(15) . . ? O3 C3 Fe1 166.4(12) . . ? O3 C3 Cu1 117.9(11) . . ? Fe1 C3 Cu1 75.8(5) . . ? O4 C4 Fe2 177.4(14) . . ? O5 C5 Fe2 167.7(10) . . ? O5 C5 Cu1 115.2(9) . . ? Fe2 C5 Cu1 76.8(4) . . ? O6 C6 Fe2 174.1(14) . . ? O6 C6 Cu2 116.6(11) . . ? Fe2 C6 Cu2 69.2(5) . . ? O7 C7 Fe3 168.2(12) . . ? O7 C7 Cu1 116.7(10) . . ? Fe3 C7 Cu1 74.3(4) . . ? O7 C7 Cu2 118.3(10) . . ? Fe3 C7 Cu2 69.7(4) . . ? Cu1 C7 Cu2 62.7(3) . . ? O8 C8 Fe3 176.7(14) . . ? O9 C9 Fe3 177.4(13) . . ? C15 C10 C11 117.8(12) . . ? C15 C10 P1 120.6(10) . . ? C11 C10 P1 121.3(9) . . ? C12 C11 C10 118.6(12) . . ? C12 C11 H11 121.4 . . ? C10 C11 H11 120.0 . . ? C13 C12 C11 122.6(14) . . ? C13 C12 H12 117.6 . . ? C11 C12 H12 119.7 . . ? C14 C13 C12 118.4(14) . . ? C14 C13 H13 121.1 . . ? C12 C13 H13 120.5 . . ? C13 C14 C15 120.6(14) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.8 . . ? C10 C15 C14 121.9(15) . . ? C10 C15 H15 118.7 . . ? C14 C15 H15 119.4 . . ? C17 C16 C21 118.5(11) . . ? C17 C16 P1 124.4(10) . . ? C21 C16 P1 117.1(9) . . ? C18 C17 C16 119.5(14) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 121.0 . . ? C19 C18 C17 121.7(15) . . ? C19 C18 H18 117.9 . . ? C17 C18 H18 120.4 . . ? C18 C19 C20 120.7(14) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.5 . . ? C19 C20 C21 119.0(15) . . ? C19 C20 H20 120.4 . . ? C21 C20 H20 120.6 . . ? C20 C21 C16 120.5(13) . . ? C20 C21 H21 120.3 . . ? C16 C21 H21 119.2 . . ? C23 C22 P1 118.6(9) . . ? C23 C22 H22A 104.9 . . ? P1 C22 H22A 109.5 . . ? C23 C22 H22B 104.5 . . ? P1 C22 H22B 109.4 . . ? H22A C22 H22B 109.5 . . ? C22 C23 P2 116.4(8) . . ? C22 C23 H23A 106.3 . . ? P2 C23 H23A 109.4 . . ? C22 C23 H23B 105.4 . . ? P2 C23 H23B 109.6 . . ? H23A C23 H23B 109.5 . . ? C29 C24 C25 119.0(12) . . ? C29 C24 P2 122.4(10) . . ? C25 C24 P2 118.6(10) . . ? C24 C25 C26 118.8(15) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 121.2 . . ? C27 C26 C25 120.7(16) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.3 . . ? C28 C27 C26 120.6(15) . . ? C28 C27 H27 119.2 . . ? C26 C27 H27 120.2 . . ? C27 C28 C29 120.1(15) . . ? C27 C28 H28 119.4 . . ? C29 C28 H28 120.5 . . ? C24 C29 C28 120.8(14) . . ? C24 C29 H29 119.7 . . ? C28 C29 H29 119.4 . . ? C35 C30 C31 118.0(12) . . ? C35 C30 P2 120.1(9) . . ? C31 C30 P2 121.7(10) . . ? C32 C31 C30 119.2(13) . . ? C32 C31 H31 121.4 . . ? C30 C31 H31 119.5 . . ? C33 C32 C31 122.9(14) . . ? C33 C32 H32 115.7 . . ? C31 C32 H32 121.4 . . ? C32 C33 C34 118.8(13) . . ? C32 C33 H33 119.8 . . ? C34 C33 H33 121.4 . . ? C35 C34 C33 119.2(15) . . ? C35 C34 H34 121.2 . . ? C33 C34 H34 119.5 . . ? C34 C35 C30 121.7(14) . . ? C34 C35 H35 120.0 . . ? C30 C35 H35 118.2 . . ? O36 C36 Fe4 178.0(14) . . ? O37 C37 Fe4 176.3(14) . . ? O38 C38 Fe4 166.8(13) . . ? O38 C38 Cu3 118.3(11) . . ? Fe4 C38 Cu3 74.8(5) . . ? O39 C39 Fe5 171.0(12) . . ? O39 C39 Cu3 115.6(10) . . ? Fe5 C39 Cu3 73.3(5) . . ? O39 C39 Cu4 116.3(11) . . ? Fe5 C39 Cu4 68.1(4) . . ? Cu3 C39 Cu4 61.2(3) . . ? O40 C40 Fe5 175.5(16) . . ? O41 C41 Fe5 176.9(15) . . ? O42 C42 Fe6 175.3(16) . . ? O43 C43 Fe6 168.0(10) . . ? O43 C43 Cu3 114.7(9) . . ? Fe6 C43 Cu3 76.5(4) . . ? O43 C43 Cu4 119.7(10) . . ? Fe6 C43 Cu4 68.5(4) . . ? Cu3 C43 Cu4 62.0(3) . . ? O44 C44 Fe6 177.7(15) . . ? C46 C45 C50 119.8(11) . . ? C46 C45 P3 117.8(9) . . ? C50 C45 P3 122.3(9) . . ? C45 C46 C47 120.0(13) . . ? C45 C46 H46 118.9 . . ? C47 C46 H46 121.0 . . ? C46 C47 C48 119.6(13) . . ? C46 C47 H47 120.6 . . ? C48 C47 H47 119.8 . . ? C49 C48 C47 120.4(13) . . ? C49 C48 H48 119.8 . . ? C47 C48 H48 119.8 . . ? C48 C49 C50 120.9(13) . . ? C48 C49 H49 118.5 . . ? C50 C49 H49 120.6 . . ? C49 C50 C45 119.3(12) . . ? C49 C50 H50 121.8 . . ? C45 C50 H50 118.9 . . ? C56 C51 C52 118.6(12) . . ? C56 C51 P3 122.2(10) . . ? C52 C51 P3 119.0(10) . . ? C53 C52 C51 117.7(13) . . ? C53 C52 H52 122.8 . . ? C51 C52 H52 119.4 . . ? C54 C53 C52 121.6(16) . . ? C54 C53 H53 119.6 . . ? C52 C53 H53 118.7 . . ? C55 C54 C53 118.8(14) . . ? C55 C54 H54 120.7 . . ? C53 C54 H54 120.3 . . ? C54 C55 C56 121.1(15) . . ? C54 C55 H55 118.6 . . ? C56 C55 H55 120.2 . . ? C51 C56 C55 122.0(14) . . ? C51 C56 H56 119.3 . . ? C55 C56 H56 118.7 . . ? C58 C57 P3 116.0(8) . . ? C58 C57 H57A 105.6 . . ? P3 C57 H57A 109.1 . . ? C58 C57 H57B 106.8 . . ? P3 C57 H57B 109.6 . . ? H57A C57 H57B 109.5 . . ? C57 C58 P4 118.1(8) . . ? C57 C58 H58A 105.4 . . ? P4 C58 H58A 109.4 . . ? C57 C58 H58B 104.8 . . ? P4 C58 H58B 109.2 . . ? H58A C58 H58B 109.5 . . ? C64 C59 C60 115.5(13) . . ? C64 C59 P4 122.8(10) . . ? C60 C59 P4 121.6(11) . . ? C59 C60 C61 119.2(17) . . ? C59 C60 H60 120.6 . . ? C61 C60 H60 120.1 . . ? C62 C61 C60 123.2(18) . . ? C62 C61 H61 120.1 . . ? C60 C61 H61 116.7 . . ? C61 C62 C63 119.4(17) . . ? C61 C62 H62 121.6 . . ? C63 C62 H62 119.0 . . ? C62 C63 C64 120.0(17) . . ? C62 C63 H63 121.1 . . ? C64 C63 H63 118.9 . . ? C59 C64 C63 122.1(16) . . ? C59 C64 H64 119.3 . . ? C63 C64 H64 118.6 . . ? C70 C65 C66 118.3(12) . . ? C70 C65 P4 119.8(10) . . ? C66 C65 P4 121.8(10) . . ? C67 C66 C65 121.6(13) . . ? C67 C66 H66 119.6 . . ? C65 C66 H66 118.8 . . ? C66 C67 C68 118.8(14) . . ? C66 C67 H67 119.5 . . ? C68 C67 H67 121.7 . . ? C69 C68 C67 120.7(13) . . ? C69 C68 H68 117.9 . . ? C67 C68 H68 121.4 . . ? C68 C69 C70 119.5(14) . . ? C68 C69 H69 119.8 . . ? C70 C69 H69 120.7 . . ? C65 C70 C69 121.1(13) . . ? C65 C70 H70 119.2 . . ? C69 C70 H70 119.6 . . ? C2 Fe1 C1 94.4(7) . . ? C2 Fe1 C3 94.0(7) . . ? C1 Fe1 C3 94.2(7) . . ? C2 Fe1 S1 98.1(5) . . ? C1 Fe1 S1 98.7(5) . . ? C3 Fe1 S1 161.5(4) . . ? C2 Fe1 Cu1 131.6(5) . . ? C1 Fe1 Cu1 125.5(5) . . ? C3 Fe1 Cu1 60.5(4) . . ? S1 Fe1 Cu1 101.02(10) . . ? C2 Fe1 Fe2 98.9(5) . . ? C1 Fe1 Fe2 150.5(5) . . ? C3 Fe1 Fe2 110.8(4) . . ? S1 Fe1 Fe2 53.52(10) . . ? Cu1 Fe1 Fe2 60.68(6) . . ? C2 Fe1 Fe3 150.4(5) . . ? C1 Fe1 Fe3 95.6(4) . . ? C3 Fe1 Fe3 112.9(4) . . ? S1 Fe1 Fe3 52.85(10) . . ? Cu1 Fe1 Fe3 60.19(6) . . ? Fe2 Fe1 Fe3 60.94(6) . . ? C4 Fe2 C6 95.9(6) . . ? C4 Fe2 C5 89.1(5) . . ? C6 Fe2 C5 102.0(6) . . ? C4 Fe2 S1 96.6(4) . . ? C6 Fe2 S1 101.0(5) . . ? C5 Fe2 S1 155.7(4) . . ? C4 Fe2 Cu2 154.2(4) . . ? C6 Fe2 Cu2 69.2(5) . . ? C5 Fe2 Cu2 74.4(4) . . ? S1 Fe2 Cu2 106.65(11) . . ? C4 Fe2 Cu1 128.3(5) . . ? C6 Fe2 Cu1 129.1(5) . . ? C5 Fe2 Cu1 61.0(4) . . ? S1 Fe2 Cu1 97.76(11) . . ? Cu2 Fe2 Cu1 60.18(6) . . ? C4 Fe2 Fe1 95.6(4) . . ? C6 Fe2 Fe1 152.2(5) . . ? C5 Fe2 Fe1 103.4(4) . . ? S1 Fe2 Fe1 52.56(10) . . ? Cu2 Fe2 Fe1 107.28(8) . . ? Cu1 Fe2 Fe1 57.57(6) . . ? C4 Fe2 Fe3 147.4(4) . . ? C6 Fe2 Fe3 98.7(4) . . ? C5 Fe2 Fe3 115.8(4) . . ? S1 Fe2 Fe3 52.16(10) . . ? Cu2 Fe2 Fe3 58.04(6) . . ? Cu1 Fe2 Fe3 58.81(6) . . ? Fe1 Fe2 Fe3 59.80(6) . . ? C9 Fe3 C8 95.6(6) . . ? C9 Fe3 C7 90.3(6) . . ? C8 Fe3 C7 99.5(6) . . ? C9 Fe3 S1 97.7(5) . . ? C8 Fe3 S1 95.3(5) . . ? C7 Fe3 S1 162.4(4) . . ? C9 Fe3 Cu2 154.0(4) . . ? C8 Fe3 Cu2 74.0(4) . . ? C7 Fe3 Cu2 68.7(4) . . ? S1 Fe3 Cu2 106.80(11) . . ? C9 Fe3 Cu1 125.1(5) . . ? C8 Fe3 Cu1 134.2(4) . . ? C7 Fe3 Cu1 64.2(4) . . ? S1 Fe3 Cu1 98.50(10) . . ? Cu2 Fe3 Cu1 60.21(6) . . ? C9 Fe3 Fe1 95.1(4) . . ? C8 Fe3 Fe1 147.1(5) . . ? C7 Fe3 Fe1 111.4(4) . . ? S1 Fe3 Fe1 52.44(10) . . ? Cu2 Fe3 Fe1 106.54(8) . . ? Cu1 Fe3 Fe1 57.52(6) . . ? C9 Fe3 Fe2 148.3(4) . . ? C8 Fe3 Fe2 98.0(5) . . ? C7 Fe3 Fe2 115.2(4) . . ? S1 Fe3 Fe2 52.69(9) . . ? Cu2 Fe3 Fe2 57.68(6) . . ? Cu1 Fe3 Fe2 59.21(6) . . ? Fe1 Fe3 Fe2 59.26(6) . . ? C36 Fe4 C37 93.0(7) . . ? C36 Fe4 C38 93.8(7) . . ? C37 Fe4 C38 93.7(7) . . ? C36 Fe4 S2 99.3(6) . . ? C37 Fe4 S2 98.5(5) . . ? C38 Fe4 S2 161.6(5) . . ? C36 Fe4 Cu3 124.4(5) . . ? C37 Fe4 Cu3 133.3(5) . . ? C38 Fe4 Cu3 60.4(4) . . ? S2 Fe4 Cu3 101.33(11) . . ? C36 Fe4 Fe6 149.8(6) . . ? C37 Fe4 Fe6 101.2(5) . . ? C38 Fe4 Fe6 111.6(5) . . ? S2 Fe4 Fe6 52.52(10) . . ? Cu3 Fe4 Fe6 61.49(6) . . ? C36 Fe4 Fe5 95.3(5) . . ? C37 Fe4 Fe5 150.8(5) . . ? C38 Fe4 Fe5 113.6(5) . . ? S2 Fe4 Fe5 52.57(10) . . ? Cu3 Fe4 Fe5 60.65(6) . . ? Fe6 Fe4 Fe5 60.23(6) . . ? C41 Fe5 C40 94.3(8) . . ? C41 Fe5 C39 89.2(7) . . ? C40 Fe5 C39 100.4(7) . . ? C41 Fe5 S2 97.1(5) . . ? C40 Fe5 S2 95.4(5) . . ? C39 Fe5 S2 162.4(4) . . ? C41 Fe5 Cu4 154.0(5) . . ? C40 Fe5 Cu4 75.1(5) . . ? C39 Fe5 Cu4 70.1(4) . . ? S2 Fe5 Cu4 107.34(12) . . ? C41 Fe5 Cu3 126.1(6) . . ? C40 Fe5 Cu3 135.0(5) . . ? C39 Fe5 Cu3 65.4(4) . . ? S2 Fe5 Cu3 97.92(11) . . ? Cu4 Fe5 Cu3 59.84(6) . . ? C41 Fe5 Fe4 95.8(5) . . ? C40 Fe5 Fe4 147.2(6) . . ? C39 Fe5 Fe4 110.8(4) . . ? S2 Fe5 Fe4 52.38(11) . . ? Cu4 Fe5 Fe4 105.91(8) . . ? Cu3 Fe5 Fe4 56.70(6) . . ? C41 Fe5 Fe6 147.9(5) . . ? C40 Fe5 Fe6 97.5(5) . . ? C39 Fe5 Fe6 117.6(4) . . ? S2 Fe5 Fe6 52.20(10) . . ? Cu4 Fe5 Fe6 58.01(6) . . ? Cu3 Fe5 Fe6 59.96(6) . . ? Fe4 Fe5 Fe6 59.60(7) . . ? C43 Fe6 C42 91.0(6) . . ? C43 Fe6 C44 101.3(6) . . ? C42 Fe6 C44 96.5(7) . . ? C43 Fe6 S2 158.7(4) . . ? C42 Fe6 S2 95.3(5) . . ? C44 Fe6 S2 98.2(4) . . ? C43 Fe6 Cu4 70.4(4) . . ? C42 Fe6 Cu4 156.3(5) . . ? C44 Fe6 Cu4 74.0(4) . . ? S2 Fe6 Cu4 107.42(12) . . ? C43 Fe6 Cu3 62.7(4) . . ? C42 Fe6 Cu3 125.3(5) . . ? C44 Fe6 Cu3 133.3(4) . . ? S2 Fe6 Cu3 97.49(11) . . ? Cu4 Fe6 Cu3 59.41(6) . . ? C43 Fe6 Fe4 106.8(4) . . ? C42 Fe6 Fe4 92.9(5) . . ? C44 Fe6 Fe4 150.2(4) . . ? S2 Fe6 Fe4 52.72(11) . . ? Cu4 Fe6 Fe4 106.13(8) . . ? Cu3 Fe6 Fe4 56.61(6) . . ? C43 Fe6 Fe5 115.3(4) . . ? C42 Fe6 Fe5 146.0(5) . . ? C44 Fe6 Fe5 98.8(5) . . ? S2 Fe6 Fe5 52.59(10) . . ? Cu4 Fe6 Fe5 57.71(6) . . ? Cu3 Fe6 Fe5 59.06(6) . . ? Fe4 Fe6 Fe5 60.17(7) . . ? C3 Cu1 P1 108.9(4) . . ? C3 Cu1 C5 106.6(5) . . ? P1 Cu1 C5 95.3(3) . . ? C3 Cu1 C7 117.0(5) . . ? P1 Cu1 C7 100.4(3) . . ? C5 Cu1 C7 125.0(4) . . ? C3 Cu1 Fe1 43.7(4) . . ? P1 Cu1 Fe1 152.51(11) . . ? C5 Cu1 Fe1 92.5(3) . . ? C7 Cu1 Fe1 96.6(3) . . ? C3 Cu1 Cu2 152.5(4) . . ? P1 Cu1 Cu2 98.22(9) . . ? C5 Cu1 Cu2 65.6(3) . . ? C7 Cu1 Cu2 60.1(3) . . ? Fe1 Cu1 Cu2 108.99(7) . . ? C3 Cu1 Fe3 100.2(4) . . ? P1 Cu1 Fe3 140.71(10) . . ? C5 Cu1 Fe3 101.2(3) . . ? C7 Cu1 Fe3 41.5(3) . . ? Fe1 Cu1 Fe3 62.29(6) . . ? Cu2 Cu1 Fe3 58.48(6) . . ? C3 Cu1 Fe2 97.8(4) . . ? P1 Cu1 Fe2 135.63(10) . . ? C5 Cu1 Fe2 42.2(3) . . ? C7 Cu1 Fe2 98.0(3) . . ? Fe1 Cu1 Fe2 61.76(6) . . ? Cu2 Cu1 Fe2 58.09(6) . . ? Fe3 Cu1 Fe2 61.98(6) . . ? P2 Cu2 C7 105.2(3) . . ? P2 Cu2 C6 125.7(4) . . ? C7 Cu2 C6 127.8(5) . . ? P2 Cu2 Fe2 149.19(11) . . ? C7 Cu2 Fe2 98.5(3) . . ? C6 Cu2 Fe2 41.6(4) . . ? P2 Cu2 Fe3 144.81(11) . . ? C7 Cu2 Fe3 41.6(3) . . ? C6 Cu2 Fe3 86.1(4) . . ? Fe2 Cu2 Fe3 64.28(6) . . ? P2 Cu2 Cu1 116.35(10) . . ? C7 Cu2 Cu1 57.2(3) . . ? C6 Cu2 Cu1 103.2(4) . . ? Fe2 Cu2 Cu1 61.73(6) . . ? Fe3 Cu2 Cu1 61.31(6) . . ? C38 Cu3 P3 105.9(4) . . ? C38 Cu3 C43 110.4(5) . . ? P3 Cu3 C43 97.7(3) . . ? C38 Cu3 C39 116.9(5) . . ? P3 Cu3 C39 101.1(3) . . ? C43 Cu3 C39 121.0(5) . . ? C38 Cu3 Fe4 44.8(4) . . ? P3 Cu3 Fe4 150.63(11) . . ? C43 Cu3 Fe4 93.6(3) . . ? C39 Cu3 Fe4 96.0(3) . . ? C38 Cu3 Cu4 153.8(4) . . ? P3 Cu3 Cu4 100.07(9) . . ? C43 Cu3 Cu4 61.5(3) . . ? C39 Cu3 Cu4 60.4(3) . . ? Fe4 Cu3 Cu4 109.14(7) . . ? C38 Cu3 Fe5 101.8(4) . . ? P3 Cu3 Fe5 141.24(10) . . ? C43 Cu3 Fe5 97.5(3) . . ? C39 Cu3 Fe5 41.2(3) . . ? Fe4 Cu3 Fe5 62.65(6) . . ? Cu4 Cu3 Fe5 57.87(6) . . ? C38 Cu3 Fe6 99.0(4) . . ? P3 Cu3 Fe6 137.68(10) . . ? C43 Cu3 Fe6 40.8(3) . . ? C39 Cu3 Fe6 97.3(3) . . ? Fe4 Cu3 Fe6 61.90(6) . . ? Cu4 Cu3 Fe6 57.77(6) . . ? Fe5 Cu3 Fe6 60.98(6) . . ? P4 Cu4 Fe5 148.35(11) . . ? P4 Cu4 Fe6 145.51(11) . . ? Fe5 Cu4 Fe6 64.28(6) . . ? P4 Cu4 C39 107.8(3) . . ? Fe5 Cu4 C39 41.9(3) . . ? Fe6 Cu4 C39 99.3(3) . . ? P4 Cu4 C43 106.6(3) . . ? Fe5 Cu4 C43 97.2(3) . . ? Fe6 Cu4 C43 41.1(3) . . ? C39 Cu4 C43 114.2(4) . . ? P4 Cu4 Cu3 114.77(10) . . ? Fe5 Cu4 Cu3 62.29(6) . . ? Fe6 Cu4 Cu3 62.82(6) . . ? C39 Cu4 Cu3 58.4(3) . . ? C43 Cu4 Cu3 56.5(3) . . ? C16 P1 C22 103.3(6) . . ? C16 P1 C10 103.6(6) . . ? C22 P1 C10 102.8(5) . . ? C16 P1 Cu1 114.2(4) . . ? C22 P1 Cu1 116.8(4) . . ? C10 P1 Cu1 114.6(4) . . ? C30 P2 C24 106.4(5) . . ? C30 P2 C23 103.0(5) . . ? C24 P2 C23 105.2(6) . . ? C30 P2 Cu2 117.1(4) . . ? C24 P2 Cu2 113.3(4) . . ? C23 P2 Cu2 110.8(4) . . ? C45 P3 C51 103.9(6) . . ? C45 P3 C57 105.4(5) . . ? C51 P3 C57 99.2(5) . . ? C45 P3 Cu3 115.3(4) . . ? C51 P3 Cu3 115.4(4) . . ? C57 P3 Cu3 115.7(4) . . ? C59 P4 C65 105.9(5) . . ? C59 P4 C58 105.6(6) . . ? C65 P4 C58 100.1(5) . . ? C59 P4 Cu4 114.6(4) . . ? C65 P4 Cu4 117.1(4) . . ? C58 P4 Cu4 112.1(4) . . ? Fe1 S1 Fe3 74.71(12) . . ? Fe1 S1 Fe2 73.92(11) . . ? Fe3 S1 Fe2 75.15(11) . . ? Fe6 S2 Fe4 74.77(12) . . ? Fe6 S2 Fe5 75.21(11) . . ? Fe4 S2 Fe5 75.05(12) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.11 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.656 _refine_diff_density_min -1.580 _refine_diff_density_rms 0.320 _database_code_depnum_ccdc_archive 'CCDC 930775' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3 #TrackingRef '18804_web_deposit_cif_file_2_Chien-Nan,Lin_1364080827.3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C78 H60 Cu4 Fe6 N4 O18 P4 S2' _chemical_formula_sum 'C78 H60 Cu4 Fe6 N4 O18 P4 S2' _chemical_formula_weight 2118.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 35.4086(10) _cell_length_b 10.2025(3) _cell_length_c 24.5709(8) _cell_angle_alpha 90.00 _cell_angle_beta 107.170(2) _cell_angle_gamma 90.00 _cell_volume 8480.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour red-brown(dark) _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.659 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4256 _exptl_absorpt_coefficient_mu 2.168 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4702 _exptl_absorpt_correction_T_max 0.7658 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25505 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 25.04 _reflns_number_total 10787 _reflns_number_gt 10175 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0357P)^2^+14.4481P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.341(9) _refine_ls_number_reflns 10787 _refine_ls_number_parameters 1049 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0319 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0716 _refine_ls_wR_factor_gt 0.0691 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.30876(15) 1.0440(5) 0.4114(3) 0.0375(14) Uani 1 1 d . . . C2 C 0.2835(2) 0.8683(6) 0.3148(3) 0.0484(15) Uani 1 1 d . . . C3 C 0.33179(18) 1.0732(7) 0.3199(3) 0.0567(19) Uani 1 1 d . . . C4 C 0.3024(2) 1.3586(7) 0.3178(3) 0.0613(19) Uani 1 1 d . . . C5 C 0.2277(2) 1.4055(6) 0.3094(3) 0.0596(18) Uani 1 1 d . . . C6 C 0.27584(19) 1.3073(6) 0.4076(3) 0.0487(15) Uani 1 1 d . . . C7 C 0.16935(16) 1.1815(7) 0.2897(3) 0.063(2) Uani 1 1 d . . . C8 C 0.21184(15) 1.1283(5) 0.3925(3) 0.0388(13) Uani 1 1 d . . . C9 C 0.18908(18) 0.9327(7) 0.3036(3) 0.0563(18) Uani 1 1 d . . . C10 C 0.09337(16) 1.0788(7) 0.3698(3) 0.0572(17) Uani 1 1 d . . . C11 C 0.05610(17) 0.8560(7) 0.3405(3) 0.0498(16) Uani 1 1 d . . . C12 C 0.06014(19) 1.0514(9) 0.2604(3) 0.073(2) Uani 1 1 d . . . C13 C -0.03666(15) 0.8569(6) 0.3125(2) 0.0369(13) Uani 1 1 d . . . C14 C -0.04968(15) 1.0449(5) 0.2217(3) 0.0355(13) Uani 1 1 d . . . C15 C -0.07545(17) 1.0860(5) 0.3075(3) 0.0410(14) Uani 1 1 d . . . C16 C 0.0033(3) 1.2731(6) 0.2345(3) 0.068(2) Uani 1 1 d . . . C17 C -0.0287(2) 1.3494(6) 0.3175(3) 0.0568(18) Uani 1 1 d . . . C18 C 0.0488(2) 1.3461(7) 0.3358(3) 0.0617(18) Uani 1 1 d . . . C19 C 0.22168(13) 0.6549(4) 0.4593(2) 0.0231(11) Uani 1 1 d . . . C20 C 0.18849(18) 0.6559(6) 0.4126(3) 0.0507(17) Uani 1 1 d . . . H20 H 0.1854 0.7213 0.3841 0.061 Uiso 1 1 calc R . . C21 C 0.1595(2) 0.5607(7) 0.4074(3) 0.064(2) Uani 1 1 d . . . H21 H 0.1364 0.5624 0.3756 0.077 Uiso 1 1 calc R . . C22 C 0.16390(18) 0.4655(6) 0.4473(3) 0.0503(16) Uani 1 1 d . . . H22 H 0.1444 0.3989 0.4427 0.060 Uiso 1 1 calc R . . C23 C 0.19630(19) 0.4656(5) 0.4941(3) 0.0551(19) Uani 1 1 d . . . H23 H 0.1989 0.4013 0.5229 0.066 Uiso 1 1 calc R . . C24 C 0.22527(17) 0.5590(5) 0.4996(3) 0.0441(15) Uani 1 1 d . . . H24 H 0.2481 0.5569 0.5318 0.053 Uiso 1 1 calc R . . C25 C 0.30532(14) 0.6797(4) 0.4800(2) 0.0258(11) Uani 1 1 d . . . C26 C 0.31661(16) 0.6312(5) 0.4348(3) 0.0404(13) Uani 1 1 d . . . H26 H 0.3008 0.6502 0.3971 0.048 Uiso 1 1 calc R . . C27 C 0.35005(18) 0.5563(6) 0.4427(3) 0.0536(17) Uani 1 1 d . . . H27 H 0.3578 0.5272 0.4109 0.064 Uiso 1 1 calc R . . C28 C 0.37242(16) 0.5235(5) 0.4975(3) 0.0450(15) Uani 1 1 d . . . H28 H 0.3949 0.4685 0.5035 0.054 Uiso 1 1 calc R . . C29 C 0.36172(17) 0.5709(6) 0.5425(3) 0.0482(16) Uani 1 1 d . . . H29 H 0.3770 0.5503 0.5803 0.058 Uiso 1 1 calc R . . C30 C 0.32838(16) 0.6497(6) 0.5333(3) 0.0414(14) Uani 1 1 d . . . H30 H 0.3216 0.6835 0.5652 0.050 Uiso 1 1 calc R . . C31 C 0.26393(13) 0.8555(4) 0.5336(2) 0.0223(10) Uani 1 1 d . . . H31A H 0.2687 0.7870 0.5634 0.027 Uiso 1 1 calc R . . H31B H 0.2869 0.9155 0.5435 0.027 Uiso 1 1 calc R . . C32 C 0.22702(13) 0.9320(4) 0.5331(2) 0.0216(10) Uani 1 1 d . . . H32A H 0.2034 0.8757 0.5185 0.026 Uiso 1 1 calc R . . H32B H 0.2242 1.0086 0.5075 0.026 Uiso 1 1 calc R . . C33 C 0.18523(13) 1.0817(4) 0.5979(2) 0.0229(11) Uani 1 1 d . . . C34 C 0.17204(14) 1.0940(5) 0.6455(2) 0.0320(12) Uani 1 1 d . . . H34 H 0.1861 1.0518 0.6800 0.038 Uiso 1 1 calc R . . C35 C 0.13859(16) 1.1671(5) 0.6433(3) 0.0399(14) Uani 1 1 d . . . H35 H 0.1298 1.1753 0.6761 0.048 Uiso 1 1 calc R . . C36 C 0.11820(14) 1.2278(5) 0.5930(3) 0.0387(14) Uani 1 1 d . . . H36 H 0.0956 1.2792 0.5916 0.046 Uiso 1 1 calc R . . C37 C 0.13017(15) 1.2148(5) 0.5456(3) 0.0404(14) Uani 1 1 d . . . H37 H 0.1156 1.2556 0.5111 0.048 Uiso 1 1 calc R . . C38 C 0.16368(15) 1.1421(5) 0.5475(3) 0.0328(12) Uani 1 1 d . . . H38 H 0.1719 1.1335 0.5142 0.039 Uiso 1 1 calc R . . C39 C 0.26895(13) 1.1148(4) 0.6202(2) 0.0239(10) Uani 1 1 d . . . C40 C 0.29346(15) 1.1267(5) 0.6759(3) 0.0352(13) Uani 1 1 d . . . H40 H 0.2901 1.0692 0.7045 0.042 Uiso 1 1 calc R . . C41 C 0.32253(18) 1.2214(6) 0.6897(3) 0.0490(16) Uani 1 1 d . . . H41 H 0.3388 1.2303 0.7279 0.059 Uiso 1 1 calc R . . C42 C 0.32783(18) 1.3023(6) 0.6484(3) 0.0510(17) Uani 1 1 d . . . H42 H 0.3483 1.3661 0.6580 0.061 Uiso 1 1 calc R . . C43 C 0.30411(18) 1.2930(6) 0.5934(3) 0.0481(16) Uani 1 1 d . . . H43 H 0.3077 1.3508 0.5651 0.058 Uiso 1 1 calc R . . C44 C 0.27460(16) 1.1978(5) 0.5795(3) 0.0382(13) Uani 1 1 d . . . H44 H 0.2582 1.1904 0.5413 0.046 Uiso 1 1 calc R . . C45 C 0.22028(17) 0.5357(5) 0.6628(3) 0.0418(14) Uani 1 1 d . . . C46 C 0.2168(3) 0.3956(6) 0.6694(4) 0.082(3) Uani 1 1 d . . . H46A H 0.1984 0.3592 0.6347 0.123 Uiso 1 1 calc R . . H46B H 0.2067 0.3784 0.7019 0.123 Uiso 1 1 calc R . . H46C H 0.2428 0.3546 0.6762 0.123 Uiso 1 1 calc R . . C47 C 0.33366(16) 0.7358(6) 0.6945(3) 0.0391(13) Uani 1 1 d . . . C48 C 0.37441(17) 0.6877(8) 0.7118(3) 0.070(2) Uani 1 1 d . . . H48A H 0.3824 0.6666 0.6779 0.105 Uiso 1 1 calc R . . H48B H 0.3762 0.6088 0.7352 0.105 Uiso 1 1 calc R . . H48C H 0.3919 0.7555 0.7340 0.105 Uiso 1 1 calc R . . C49 C 0.03620(14) 0.6550(4) 0.1708(2) 0.0250(11) Uani 1 1 d . . . C50 C 0.07016(16) 0.6646(5) 0.2160(3) 0.0394(13) Uani 1 1 d . . . H50 H 0.0726 0.7315 0.2437 0.047 Uiso 1 1 calc R . . C51 C 0.10073(18) 0.5766(7) 0.2208(3) 0.0550(18) Uani 1 1 d . . . H51 H 0.1241 0.5835 0.2520 0.066 Uiso 1 1 calc R . . C52 C 0.09749(19) 0.4807(6) 0.1815(3) 0.0572(19) Uani 1 1 d . . . H52 H 0.1182 0.4188 0.1858 0.069 Uiso 1 1 calc R . . C53 C 0.06367(18) 0.4728(6) 0.1346(3) 0.0535(18) Uani 1 1 d . . . H53 H 0.0617 0.4077 0.1062 0.064 Uiso 1 1 calc R . . C54 C 0.03341(16) 0.5594(5) 0.1297(3) 0.0418(15) Uani 1 1 d . . . H54 H 0.0103 0.5541 0.0980 0.050 Uiso 1 1 calc R . . C55 C -0.04759(13) 0.6664(4) 0.1500(2) 0.0257(11) Uani 1 1 d . . . C56 C -0.07591(15) 0.6637(5) 0.0966(3) 0.0349(13) Uani 1 1 d . . . H56 H -0.0728 0.7174 0.0666 0.042 Uiso 1 1 calc R . . C57 C -0.10862(16) 0.5822(6) 0.0875(3) 0.0412(14) Uani 1 1 d . . . H57 H -0.1282 0.5829 0.0515 0.049 Uiso 1 1 calc R . . C58 C -0.11314(17) 0.5018(6) 0.1289(3) 0.0548(18) Uani 1 1 d . . . H58 H -0.1353 0.4449 0.1217 0.066 Uiso 1 1 calc R . . C59 C -0.08525(19) 0.5032(7) 0.1818(3) 0.072(2) Uani 1 1 d . . . H59 H -0.0885 0.4485 0.2114 0.087 Uiso 1 1 calc R . . C60 C -0.05225(17) 0.5850(6) 0.1918(3) 0.0543(18) Uani 1 1 d . . . H60 H -0.0328 0.5840 0.2279 0.065 Uiso 1 1 calc R . . C61 C -0.00893(13) 0.8584(4) 0.0993(2) 0.0226(10) Uani 1 1 d . . . H61A H -0.0125 0.7938 0.0681 0.027 Uiso 1 1 calc R . . H61B H -0.0328 0.9144 0.0904 0.027 Uiso 1 1 calc R . . C62 C 0.02733(13) 0.9440(4) 0.1023(2) 0.0225(10) Uani 1 1 d . . . H62A H 0.0517 0.8919 0.1178 0.027 Uiso 1 1 calc R . . H62B H 0.0281 1.0190 0.1282 0.027 Uiso 1 1 calc R . . C63 C 0.07061(13) 1.0979(4) 0.0416(2) 0.0206(10) Uani 1 1 d . . . C64 C 0.08314(16) 1.1201(5) -0.0062(2) 0.0368(13) Uani 1 1 d . . . H64 H 0.0685 1.0839 -0.0418 0.044 Uiso 1 1 calc R . . C65 C 0.11636(16) 1.1937(6) -0.0027(3) 0.0453(15) Uani 1 1 d . . . H65 H 0.1242 1.2097 -0.0360 0.054 Uiso 1 1 calc R . . C66 C 0.13820(15) 1.2438(5) 0.0488(3) 0.0387(14) Uani 1 1 d . . . H66 H 0.1608 1.2965 0.0513 0.046 Uiso 1 1 calc R . . C67 C 0.12717(14) 1.2171(5) 0.0968(3) 0.0373(13) Uani 1 1 d . . . H67 H 0.1430 1.2479 0.1328 0.045 Uiso 1 1 calc R . . C68 C 0.09314(14) 1.1456(5) 0.0933(2) 0.0313(12) Uani 1 1 d . . . H68 H 0.0854 1.1296 0.1266 0.038 Uiso 1 1 calc R . . C69 C -0.01350(13) 1.1297(5) 0.0165(2) 0.0253(11) Uani 1 1 d . . . C70 C -0.03888(16) 1.1418(5) -0.0384(3) 0.0400(14) Uani 1 1 d . . . H70 H -0.0357 1.0858 -0.0676 0.048 Uiso 1 1 calc R . . C71 C -0.06847(17) 1.2340(7) -0.0509(3) 0.0561(18) Uani 1 1 d . . . H71 H -0.0852 1.2428 -0.0889 0.067 Uiso 1 1 calc R . . C72 C -0.07414(19) 1.3136(6) -0.0087(3) 0.0549(18) Uani 1 1 d . . . H72 H -0.0951 1.3755 -0.0172 0.066 Uiso 1 1 calc R . . C73 C -0.0492(2) 1.3025(6) 0.0456(3) 0.0605(19) Uani 1 1 d . . . H73 H -0.0528 1.3574 0.0749 0.073 Uiso 1 1 calc R . . C74 C -0.01920(17) 1.2124(6) 0.0577(3) 0.0450(15) Uani 1 1 d . . . H74 H -0.0019 1.2069 0.0954 0.054 Uiso 1 1 calc R . . C75 C -0.07469(15) 0.7265(5) -0.0682(3) 0.0386(13) Uani 1 1 d . . . C76 C -0.11053(19) 0.6499(7) -0.0905(4) 0.069(2) Uani 1 1 d . . . H76A H -0.1245 0.6435 -0.0616 0.104 Uiso 1 1 calc R . . H76B H -0.1036 0.5618 -0.1004 0.104 Uiso 1 1 calc R . . H76C H -0.1276 0.6927 -0.1246 0.104 Uiso 1 1 calc R . . C77 C 0.03466(19) 0.5589(6) -0.0319(3) 0.0485(16) Uani 1 1 d . . . C78 C 0.0357(4) 0.4194(7) -0.0438(6) 0.126(5) Uani 1 1 d . . . H78A H 0.0264 0.3697 -0.0161 0.189 Uiso 1 1 calc R . . H78B H 0.0628 0.3933 -0.0410 0.189 Uiso 1 1 calc R . . H78C H 0.0185 0.4014 -0.0823 0.189 Uiso 1 1 calc R . . N1 N 0.22343(13) 0.6449(4) 0.6587(2) 0.0376(11) Uani 1 1 d . . . N2 N 0.30292(12) 0.7738(5) 0.6826(2) 0.0385(11) Uani 1 1 d . . . N3 N -0.04654(13) 0.7846(4) -0.0516(2) 0.0399(11) Uani 1 1 d . . . N4 N 0.03264(13) 0.6656(4) -0.0248(2) 0.0360(11) Uani 1 1 d . . . O1 O 0.32591(12) 1.0515(4) 0.45908(19) 0.0538(12) Uani 1 1 d . . . O2 O 0.2814(2) 0.7619(5) 0.2999(2) 0.0876(19) Uani 1 1 d . . . O3 O 0.36088(14) 1.0945(7) 0.3096(3) 0.099(2) Uani 1 1 d . . . O4 O 0.3287(2) 1.4098(6) 0.3076(3) 0.109(3) Uani 1 1 d . . . O5 O 0.20627(19) 1.4896(5) 0.2943(3) 0.096(2) Uani 1 1 d . . . O6 O 0.28419(16) 1.3302(5) 0.4550(2) 0.0703(14) Uani 1 1 d . . . O7 O 0.14205(14) 1.2438(7) 0.2695(3) 0.117(3) Uani 1 1 d . . . O8 O 0.20926(11) 1.1631(4) 0.43613(19) 0.0469(10) Uani 1 1 d . . . O9 O 0.17183(19) 0.8374(5) 0.2889(2) 0.102(2) Uani 1 1 d . . . O10 O 0.12219(13) 1.1146(7) 0.4007(2) 0.099(2) Uani 1 1 d . . . O11 O 0.06261(17) 0.7474(5) 0.3529(2) 0.0796(16) Uani 1 1 d . . . O12 O 0.07284(18) 1.0733(8) 0.2231(2) 0.119(3) Uani 1 1 d . . . O13 O -0.04041(14) 0.7500(4) 0.3247(2) 0.0599(12) Uani 1 1 d . . . O14 O -0.06509(13) 1.0614(5) 0.17365(19) 0.0573(12) Uani 1 1 d . . . O15 O -0.10460(12) 1.1234(5) 0.3128(2) 0.0684(15) Uani 1 1 d . . . O16 O -0.0003(3) 1.2963(6) 0.1876(2) 0.116(3) Uani 1 1 d . . . O17 O -0.05129(19) 1.4205(5) 0.3265(3) 0.0881(19) Uani 1 1 d . . . O18 O 0.07503(17) 1.4144(6) 0.3552(3) 0.102(2) Uani 1 1 d . . . P1 P 0.25992(3) 0.77828(11) 0.46506(5) 0.0207(2) Uani 1 1 d . . . P2 P 0.23034(3) 0.98810(10) 0.60568(5) 0.0190(2) Uani 1 1 d . . . P3 P -0.00377(3) 0.77143(10) 0.16631(5) 0.0199(2) Uani 1 1 d . . . P4 P 0.02510(3) 1.00462(11) 0.03139(5) 0.0196(2) Uani 1 1 d . . . S1 S 0.24601(3) 1.13334(11) 0.26403(5) 0.0258(3) Uani 1 1 d . . . S2 S 0.01113(3) 1.10126(11) 0.37367(5) 0.0253(3) Uani 1 1 d . . . Fe1 Fe 0.287750(19) 1.03648(7) 0.33639(3) 0.02886(17) Uani 1 1 d . . . Fe2 Fe 0.26259(2) 1.27580(7) 0.33319(3) 0.03378(17) Uani 1 1 d . . . Fe3 Fe 0.212077(19) 1.08688(7) 0.32292(3) 0.03117(17) Uani 1 1 d . . . Fe4 Fe 0.047439(19) 1.02344(8) 0.32428(3) 0.03495(18) Uani 1 1 d . . . Fe5 Fe -0.031452(18) 1.02516(7) 0.29731(3) 0.02520(16) Uani 1 1 d . . . Fe6 Fe 0.00788(2) 1.24234(7) 0.30723(3) 0.03869(19) Uani 1 1 d . . . Cu1 Cu 0.249739(16) 0.92022(5) 0.39342(2) 0.02696(14) Uani 1 1 d . . . Cu2 Cu 0.244997(16) 0.82950(5) 0.67068(2) 0.02436(13) Uani 1 1 d . . . Cu3 Cu 0.004724(16) 0.90093(5) 0.24179(2) 0.02685(14) Uani 1 1 d . . . Cu4 Cu 0.011041(16) 0.85029(5) -0.03391(2) 0.02490(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.027(3) 0.046(3) 0.039(4) 0.008(3) 0.009(3) -0.004(2) C2 0.073(4) 0.051(4) 0.029(3) 0.009(3) 0.028(3) 0.012(3) C3 0.034(3) 0.089(5) 0.052(4) 0.033(4) 0.020(3) 0.018(3) C4 0.095(5) 0.063(4) 0.036(4) -0.026(3) 0.033(4) -0.035(4) C5 0.090(5) 0.046(4) 0.051(4) -0.004(3) 0.034(4) 0.002(3) C6 0.063(4) 0.046(3) 0.038(4) -0.008(3) 0.018(3) -0.014(3) C7 0.033(3) 0.091(5) 0.060(5) 0.043(4) 0.008(3) -0.001(3) C8 0.034(3) 0.045(3) 0.039(4) 0.016(3) 0.014(3) 0.007(2) C9 0.060(4) 0.070(4) 0.025(3) 0.018(3) -0.009(3) -0.029(3) C10 0.033(3) 0.107(5) 0.035(3) -0.019(4) 0.014(3) -0.017(3) C11 0.040(3) 0.082(5) 0.026(3) -0.010(3) 0.007(2) 0.011(3) C12 0.055(4) 0.136(7) 0.034(4) -0.034(4) 0.020(3) -0.059(4) C13 0.034(3) 0.051(3) 0.026(3) -0.012(3) 0.009(2) -0.009(2) C14 0.032(3) 0.039(3) 0.033(4) -0.006(2) 0.005(3) 0.000(2) C15 0.037(3) 0.046(3) 0.036(3) -0.017(3) 0.005(3) -0.003(2) C16 0.122(6) 0.052(4) 0.032(4) 0.002(3) 0.029(4) -0.034(4) C17 0.085(5) 0.041(3) 0.039(4) 0.012(3) 0.010(4) -0.010(3) C18 0.084(5) 0.059(4) 0.047(4) -0.009(3) 0.026(4) -0.031(4) C19 0.024(2) 0.021(2) 0.029(3) -0.008(2) 0.014(2) -0.0010(17) C20 0.045(3) 0.065(4) 0.035(4) 0.012(3) 0.000(3) -0.022(3) C21 0.053(4) 0.084(5) 0.046(4) 0.002(4) -0.001(3) -0.037(3) C22 0.049(3) 0.045(3) 0.058(4) -0.008(3) 0.017(3) -0.023(3) C23 0.057(4) 0.032(3) 0.075(5) 0.022(3) 0.018(4) -0.008(3) C24 0.035(3) 0.037(3) 0.053(4) 0.016(3) 0.003(3) -0.004(2) C25 0.025(2) 0.025(2) 0.029(3) -0.004(2) 0.010(2) 0.0000(18) C26 0.045(3) 0.049(3) 0.031(3) -0.007(3) 0.018(3) 0.007(2) C27 0.056(4) 0.057(4) 0.054(4) -0.017(3) 0.026(3) 0.013(3) C28 0.032(3) 0.038(3) 0.067(4) -0.010(3) 0.017(3) 0.008(2) C29 0.034(3) 0.057(3) 0.051(4) 0.001(3) 0.008(3) 0.010(3) C30 0.035(3) 0.055(3) 0.036(3) -0.007(3) 0.013(3) 0.011(2) C31 0.025(2) 0.023(2) 0.021(3) -0.004(2) 0.009(2) -0.0004(17) C32 0.025(2) 0.021(2) 0.020(3) -0.0038(19) 0.009(2) -0.0007(17) C33 0.021(2) 0.015(2) 0.033(3) -0.0017(19) 0.009(2) -0.0002(16) C34 0.030(2) 0.035(3) 0.030(3) 0.003(2) 0.008(2) 0.007(2) C35 0.043(3) 0.043(3) 0.043(4) 0.001(3) 0.028(3) 0.009(2) C36 0.027(2) 0.031(3) 0.062(4) 0.000(3) 0.019(3) 0.008(2) C37 0.029(3) 0.045(3) 0.049(4) 0.012(3) 0.015(3) 0.014(2) C38 0.032(3) 0.036(3) 0.032(3) 0.003(2) 0.011(2) 0.005(2) C39 0.023(2) 0.021(2) 0.031(3) -0.005(2) 0.012(2) -0.0031(18) C40 0.036(3) 0.042(3) 0.029(3) -0.008(2) 0.011(2) -0.015(2) C41 0.049(3) 0.066(4) 0.031(3) -0.012(3) 0.010(3) -0.021(3) C42 0.049(3) 0.051(3) 0.053(4) -0.015(3) 0.015(3) -0.028(3) C43 0.050(3) 0.043(3) 0.050(4) -0.001(3) 0.014(3) -0.022(3) C44 0.041(3) 0.035(3) 0.035(3) 0.000(2) 0.006(3) -0.009(2) C45 0.051(3) 0.031(3) 0.040(4) -0.001(2) 0.009(3) 0.001(2) C46 0.114(7) 0.032(3) 0.109(8) -0.003(4) 0.045(6) -0.004(4) C47 0.036(3) 0.051(3) 0.033(3) 0.007(3) 0.014(3) 0.009(2) C48 0.033(3) 0.108(6) 0.066(5) 0.008(4) 0.011(3) 0.033(3) C49 0.026(2) 0.021(2) 0.031(3) 0.005(2) 0.012(2) 0.0012(17) C50 0.040(3) 0.049(3) 0.029(3) 0.002(3) 0.010(3) 0.012(2) C51 0.041(3) 0.076(4) 0.047(4) 0.015(4) 0.010(3) 0.029(3) C52 0.056(4) 0.042(3) 0.077(5) 0.016(3) 0.025(4) 0.028(3) C53 0.054(4) 0.033(3) 0.075(5) -0.008(3) 0.022(4) 0.009(3) C54 0.038(3) 0.031(3) 0.054(4) -0.009(3) 0.009(3) 0.002(2) C55 0.024(2) 0.024(2) 0.031(3) 0.000(2) 0.011(2) -0.0002(17) C56 0.032(3) 0.044(3) 0.029(3) 0.002(2) 0.009(2) -0.008(2) C57 0.026(3) 0.053(3) 0.041(4) -0.008(3) 0.005(3) -0.009(2) C58 0.032(3) 0.052(3) 0.076(5) 0.008(3) 0.009(3) -0.016(3) C59 0.058(4) 0.080(5) 0.069(5) 0.034(4) 0.004(4) -0.038(4) C60 0.040(3) 0.062(4) 0.050(4) 0.024(3) -0.003(3) -0.022(3) C61 0.021(2) 0.025(2) 0.021(3) -0.002(2) 0.005(2) -0.0043(18) C62 0.025(2) 0.023(2) 0.018(2) -0.0039(19) 0.004(2) -0.0068(17) C63 0.023(2) 0.018(2) 0.022(3) 0.0058(18) 0.008(2) 0.0007(16) C64 0.038(3) 0.044(3) 0.029(3) 0.000(2) 0.011(2) -0.011(2) C65 0.035(3) 0.062(4) 0.042(4) 0.010(3) 0.017(3) -0.011(3) C66 0.027(2) 0.032(3) 0.059(4) 0.005(3) 0.015(3) -0.006(2) C67 0.030(3) 0.036(3) 0.044(4) -0.012(3) 0.007(3) -0.004(2) C68 0.031(3) 0.034(3) 0.032(3) -0.009(2) 0.014(2) -0.007(2) C69 0.028(2) 0.027(2) 0.022(3) 0.003(2) 0.011(2) 0.0027(19) C70 0.046(3) 0.042(3) 0.033(3) 0.003(3) 0.014(3) 0.012(2) C71 0.041(3) 0.068(4) 0.053(4) 0.028(4) 0.004(3) 0.023(3) C72 0.054(4) 0.048(3) 0.067(5) 0.011(3) 0.026(4) 0.027(3) C73 0.074(4) 0.052(4) 0.058(5) -0.003(3) 0.024(4) 0.028(3) C74 0.049(3) 0.051(3) 0.032(3) -0.005(3) 0.008(3) 0.020(3) C75 0.037(3) 0.042(3) 0.038(3) 0.000(3) 0.011(3) -0.008(2) C76 0.052(4) 0.064(4) 0.088(6) -0.004(4) 0.015(4) -0.027(3) C77 0.060(4) 0.037(3) 0.052(4) 0.010(3) 0.022(3) 0.008(3) C78 0.223(13) 0.030(4) 0.157(12) -0.001(5) 0.105(10) 0.011(5) N1 0.046(3) 0.033(2) 0.030(3) -0.004(2) 0.003(2) 0.0014(19) N2 0.030(2) 0.052(3) 0.033(3) 0.006(2) 0.008(2) 0.018(2) N3 0.034(2) 0.046(3) 0.039(3) -0.003(2) 0.011(2) -0.013(2) N4 0.044(3) 0.022(2) 0.040(3) 0.0034(19) 0.008(2) 0.0024(17) O1 0.045(2) 0.079(3) 0.028(3) 0.009(2) -0.005(2) -0.012(2) O2 0.184(6) 0.039(3) 0.054(3) 0.002(2) 0.059(4) 0.013(3) O3 0.039(3) 0.160(6) 0.109(5) 0.081(5) 0.039(3) 0.024(3) O4 0.142(5) 0.125(5) 0.091(5) -0.050(4) 0.080(4) -0.098(4) O5 0.128(5) 0.069(3) 0.096(5) 0.021(3) 0.042(4) 0.054(3) O6 0.105(4) 0.079(3) 0.032(3) -0.013(2) 0.027(3) -0.026(3) O7 0.041(3) 0.158(6) 0.141(6) 0.098(5) 0.009(3) 0.030(3) O8 0.053(2) 0.053(2) 0.041(3) 0.014(2) 0.024(2) 0.0121(18) O9 0.140(5) 0.093(4) 0.049(3) 0.015(3) -0.011(3) -0.084(4) O10 0.045(3) 0.198(6) 0.047(3) -0.030(4) 0.004(2) -0.046(3) O11 0.109(4) 0.075(3) 0.047(3) 0.004(3) 0.010(3) 0.040(3) O12 0.109(4) 0.224(7) 0.038(3) -0.052(4) 0.045(3) -0.116(5) O13 0.089(3) 0.036(2) 0.057(3) 0.008(2) 0.025(3) -0.016(2) O14 0.060(3) 0.073(3) 0.029(3) 0.007(2) -0.003(2) 0.016(2) O15 0.031(2) 0.099(3) 0.074(4) -0.032(3) 0.014(2) 0.007(2) O16 0.228(8) 0.092(4) 0.032(3) -0.004(3) 0.045(4) -0.058(5) O17 0.115(5) 0.057(3) 0.099(5) 0.020(3) 0.041(4) 0.029(3) O18 0.094(4) 0.097(4) 0.109(5) -0.026(4) 0.021(4) -0.071(3) P1 0.0228(5) 0.0219(6) 0.0195(6) -0.0015(5) 0.0095(5) -0.0004(4) P2 0.0204(5) 0.0182(5) 0.0190(6) -0.0007(5) 0.0068(5) 0.0017(4) P3 0.0217(5) 0.0209(5) 0.0176(6) 0.0010(5) 0.0066(5) -0.0010(4) P4 0.0231(5) 0.0185(5) 0.0178(6) 0.0002(5) 0.0071(5) -0.0013(4) S1 0.0299(6) 0.0300(6) 0.0175(6) 0.0030(5) 0.0070(5) -0.0048(5) S2 0.0274(6) 0.0319(6) 0.0167(6) -0.0031(5) 0.0068(5) -0.0056(5) Fe1 0.0263(3) 0.0375(4) 0.0242(4) 0.0092(3) 0.0096(3) 0.0017(3) Fe2 0.0455(4) 0.0334(4) 0.0259(4) -0.0030(3) 0.0159(3) -0.0065(3) Fe3 0.0234(3) 0.0446(4) 0.0241(4) 0.0126(3) 0.0048(3) -0.0024(3) Fe4 0.0233(3) 0.0617(5) 0.0202(4) -0.0122(4) 0.0069(3) -0.0095(3) Fe5 0.0223(3) 0.0318(3) 0.0212(4) -0.0056(3) 0.0059(3) -0.0044(3) Fe6 0.0550(4) 0.0384(4) 0.0221(4) 0.0003(3) 0.0105(3) -0.0199(4) Cu1 0.0319(3) 0.0280(3) 0.0217(3) 0.0043(3) 0.0089(3) -0.0030(2) Cu2 0.0275(3) 0.0243(3) 0.0211(3) 0.0015(2) 0.0070(2) 0.0045(2) Cu3 0.0308(3) 0.0310(3) 0.0194(3) -0.0040(3) 0.0084(3) -0.0016(2) Cu4 0.0313(3) 0.0242(3) 0.0196(3) -0.0029(2) 0.0081(2) -0.0029(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.152(7) . ? C1 Fe1 1.774(6) . ? C1 Cu1 2.369(5) . ? C2 O2 1.141(7) . ? C2 Fe1 1.789(7) . ? C3 O3 1.153(8) . ? C3 Fe1 1.763(6) . ? C4 O4 1.158(8) . ? C4 Fe2 1.776(7) . ? C5 O5 1.132(8) . ? C5 Fe2 1.787(7) . ? C6 O6 1.137(8) . ? C6 Fe2 1.778(7) . ? C7 O7 1.141(7) . ? C7 Fe3 1.777(6) . ? C8 O8 1.159(7) . ? C8 Fe3 1.763(7) . ? C8 Cu1 2.508(5) . ? C9 O9 1.149(7) . ? C9 Fe3 1.770(6) . ? C10 O10 1.137(7) . ? C10 Fe4 1.773(6) . ? C11 O11 1.155(8) . ? C11 Fe4 1.760(8) . ? C12 O12 1.155(8) . ? C12 Fe4 1.779(7) . ? C12 Cu3 2.426(6) . ? C13 O13 1.148(7) . ? C13 Fe5 1.778(6) . ? C14 O14 1.157(7) . ? C14 Fe5 1.790(6) . ? C14 Cu3 2.356(5) . ? C15 O15 1.143(7) . ? C15 Fe5 1.762(6) . ? C16 O16 1.146(8) . ? C16 Fe6 1.774(7) . ? C17 O17 1.149(9) . ? C17 Fe6 1.767(8) . ? C18 O18 1.146(7) . ? C18 Fe6 1.765(6) . ? C19 C24 1.371(8) . ? C19 C20 1.379(8) . ? C19 P1 1.824(4) . ? C20 C21 1.391(8) . ? C20 H20 0.9500 . ? C21 C22 1.357(10) . ? C21 H21 0.9500 . ? C22 C23 1.363(9) . ? C22 H22 0.9500 . ? C23 C24 1.377(8) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C30 1.359(8) . ? C25 C26 1.378(8) . ? C25 P1 1.839(5) . ? C26 C27 1.374(8) . ? C26 H26 0.9500 . ? C27 C28 1.386(9) . ? C27 H27 0.9500 . ? C28 C29 1.360(9) . ? C28 H28 0.9500 . ? C29 C30 1.390(8) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.519(6) . ? C31 P1 1.827(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 P2 1.843(5) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.388(8) . ? C33 C38 1.391(7) . ? C33 P2 1.822(4) . ? C34 C35 1.387(7) . ? C34 H34 0.9500 . ? C35 C36 1.380(8) . ? C35 H35 0.9500 . ? C36 C37 1.358(9) . ? C36 H36 0.9500 . ? C37 C38 1.388(7) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C44 1.369(8) . ? C39 C40 1.394(7) . ? C39 P2 1.838(4) . ? C40 C41 1.380(7) . ? C40 H40 0.9500 . ? C41 C42 1.363(9) . ? C41 H41 0.9500 . ? C42 C43 1.367(9) . ? C42 H42 0.9500 . ? C43 C44 1.393(7) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 N1 1.127(6) . ? C45 C46 1.448(8) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 N2 1.110(6) . ? C47 C48 1.464(7) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C50 1.377(8) . ? C49 C54 1.387(8) . ? C49 P3 1.826(5) . ? C50 C51 1.384(8) . ? C50 H50 0.9500 . ? C51 C52 1.357(10) . ? C51 H51 0.9500 . ? C52 C53 1.398(10) . ? C52 H52 0.9500 . ? C53 C54 1.366(8) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 C60 1.367(8) . ? C55 C56 1.397(7) . ? C55 P3 1.830(5) . ? C56 C57 1.389(7) . ? C56 H56 0.9500 . ? C57 C58 1.353(9) . ? C57 H57 0.9500 . ? C58 C59 1.381(9) . ? C58 H58 0.9500 . ? C59 C60 1.398(8) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C61 C62 1.536(6) . ? C61 P3 1.831(5) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 P4 1.829(5) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C68 1.373(7) . ? C63 C64 1.391(8) . ? C63 P4 1.824(4) . ? C64 C65 1.377(7) . ? C64 H64 0.9500 . ? C65 C66 1.374(9) . ? C65 H65 0.9500 . ? C66 C67 1.374(9) . ? C66 H66 0.9500 . ? C67 C68 1.389(7) . ? C67 H67 0.9500 . ? C68 H68 0.9500 . ? C69 C74 1.378(8) . ? C69 C70 1.388(8) . ? C69 P4 1.826(5) . ? C70 C71 1.373(8) . ? C70 H70 0.9500 . ? C71 C72 1.377(10) . ? C71 H71 0.9500 . ? C72 C73 1.370(10) . ? C72 H72 0.9500 . ? C73 C74 1.370(8) . ? C73 H73 0.9500 . ? C74 H74 0.9500 . ? C75 N3 1.128(6) . ? C75 C76 1.453(8) . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 N4 1.109(7) . ? C77 C78 1.455(9) . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? N1 Cu2 2.021(4) . ? N2 Cu2 2.064(4) . ? N3 Cu4 2.067(4) . ? N4 Cu4 2.021(4) . ? P1 Cu1 2.2250(14) . ? P2 Cu2 2.2245(13) . ? P3 Cu3 2.2241(14) . ? P4 Cu4 2.1978(13) . ? S1 Fe2 2.1807(14) . ? S1 Fe1 2.1842(14) . ? S1 Fe3 2.1881(15) . ? S1 Cu2 2.3148(14) 2_574 ? S2 Fe6 2.1538(15) . ? S2 Fe4 2.1625(15) . ? S2 Fe5 2.1739(13) . ? S2 Cu4 2.3250(14) 2_575 ? Fe1 Cu1 2.5092(9) . ? Fe1 Fe2 2.5924(10) . ? Fe1 Fe3 2.6514(9) . ? Fe2 Fe3 2.5906(10) . ? Fe3 Cu1 2.5113(9) . ? Fe4 Cu3 2.4796(9) . ? Fe4 Fe6 2.6036(12) . ? Fe4 Fe5 2.6739(9) . ? Fe5 Cu3 2.4779(9) . ? Fe5 Fe6 2.5901(9) . ? Cu2 S1 2.3148(14) 2_575 ? Cu4 S2 2.3250(14) 2_574 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 Fe1 173.2(5) . . ? O1 C1 Cu1 113.3(4) . . ? Fe1 C1 Cu1 72.96(19) . . ? O2 C2 Fe1 178.1(6) . . ? O3 C3 Fe1 178.5(6) . . ? O4 C4 Fe2 178.5(7) . . ? O5 C5 Fe2 178.4(7) . . ? O6 C6 Fe2 178.6(6) . . ? O7 C7 Fe3 178.5(9) . . ? O8 C8 Fe3 174.3(5) . . ? O8 C8 Cu1 116.0(4) . . ? Fe3 C8 Cu1 69.5(2) . . ? O9 C9 Fe3 175.2(6) . . ? O10 C10 Fe4 177.4(6) . . ? O11 C11 Fe4 177.7(6) . . ? O12 C12 Fe4 171.8(5) . . ? O12 C12 Cu3 117.1(4) . . ? Fe4 C12 Cu3 70.4(2) . . ? O13 C13 Fe5 176.8(6) . . ? O14 C14 Fe5 173.0(5) . . ? O14 C14 Cu3 114.5(4) . . ? Fe5 C14 Cu3 71.93(18) . . ? O15 C15 Fe5 178.0(5) . . ? O16 C16 Fe6 177.9(9) . . ? O17 C17 Fe6 177.0(7) . . ? O18 C18 Fe6 178.5(7) . . ? C24 C19 C20 118.7(5) . . ? C24 C19 P1 121.9(4) . . ? C20 C19 P1 119.4(4) . . ? C19 C20 C21 119.7(6) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C22 C21 C20 120.6(6) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C21 C22 C23 119.8(5) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C22 C23 C24 120.0(6) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C19 C24 C23 121.0(6) . . ? C19 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C30 C25 C26 117.5(5) . . ? C30 C25 P1 123.8(4) . . ? C26 C25 P1 118.7(4) . . ? C27 C26 C25 121.9(6) . . ? C27 C26 H26 119.0 . . ? C25 C26 H26 119.0 . . ? C26 C27 C28 119.6(6) . . ? C26 C27 H27 120.2 . . ? C28 C27 H27 120.2 . . ? C29 C28 C27 119.1(5) . . ? C29 C28 H28 120.4 . . ? C27 C28 H28 120.4 . . ? C28 C29 C30 120.1(6) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C25 C30 C29 121.7(6) . . ? C25 C30 H30 119.1 . . ? C29 C30 H30 119.1 . . ? C32 C31 P1 112.4(3) . . ? C32 C31 H31A 109.1 . . ? P1 C31 H31A 109.1 . . ? C32 C31 H31B 109.1 . . ? P1 C31 H31B 109.1 . . ? H31A C31 H31B 107.8 . . ? C31 C32 P2 110.0(3) . . ? C31 C32 H32A 109.7 . . ? P2 C32 H32A 109.7 . . ? C31 C32 H32B 109.7 . . ? P2 C32 H32B 109.7 . . ? H32A C32 H32B 108.2 . . ? C34 C33 C38 118.5(4) . . ? C34 C33 P2 117.4(4) . . ? C38 C33 P2 124.0(4) . . ? C35 C34 C33 120.7(5) . . ? C35 C34 H34 119.6 . . ? C33 C34 H34 119.6 . . ? C36 C35 C34 119.5(6) . . ? C36 C35 H35 120.3 . . ? C34 C35 H35 120.3 . . ? C37 C36 C35 120.7(5) . . ? C37 C36 H36 119.7 . . ? C35 C36 H36 119.7 . . ? C36 C37 C38 120.2(5) . . ? C36 C37 H37 119.9 . . ? C38 C37 H37 119.9 . . ? C37 C38 C33 120.3(5) . . ? C37 C38 H38 119.8 . . ? C33 C38 H38 119.8 . . ? C44 C39 C40 118.8(4) . . ? C44 C39 P2 123.7(4) . . ? C40 C39 P2 117.6(4) . . ? C41 C40 C39 120.4(6) . . ? C41 C40 H40 119.8 . . ? C39 C40 H40 119.8 . . ? C42 C41 C40 119.8(6) . . ? C42 C41 H41 120.1 . . ? C40 C41 H41 120.1 . . ? C41 C42 C43 121.0(5) . . ? C41 C42 H42 119.5 . . ? C43 C42 H42 119.5 . . ? C42 C43 C44 119.3(6) . . ? C42 C43 H43 120.4 . . ? C44 C43 H43 120.4 . . ? C39 C44 C43 120.8(5) . . ? C39 C44 H44 119.6 . . ? C43 C44 H44 119.6 . . ? N1 C45 C46 178.7(8) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N2 C47 C48 178.2(7) . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C50 C49 C54 119.6(5) . . ? C50 C49 P3 118.7(4) . . ? C54 C49 P3 121.7(4) . . ? C49 C50 C51 119.9(6) . . ? C49 C50 H50 120.1 . . ? C51 C50 H50 120.1 . . ? C52 C51 C50 120.5(6) . . ? C52 C51 H51 119.8 . . ? C50 C51 H51 119.8 . . ? C51 C52 C53 120.0(5) . . ? C51 C52 H52 120.0 . . ? C53 C52 H52 120.0 . . ? C54 C53 C52 119.6(6) . . ? C54 C53 H53 120.2 . . ? C52 C53 H53 120.2 . . ? C53 C54 C49 120.4(6) . . ? C53 C54 H54 119.8 . . ? C49 C54 H54 119.8 . . ? C60 C55 C56 118.7(5) . . ? C60 C55 P3 118.3(4) . . ? C56 C55 P3 123.0(4) . . ? C57 C56 C55 119.7(5) . . ? C57 C56 H56 120.1 . . ? C55 C56 H56 120.1 . . ? C58 C57 C56 121.4(6) . . ? C58 C57 H57 119.3 . . ? C56 C57 H57 119.3 . . ? C57 C58 C59 119.4(5) . . ? C57 C58 H58 120.3 . . ? C59 C58 H58 120.3 . . ? C58 C59 C60 119.9(6) . . ? C58 C59 H59 120.0 . . ? C60 C59 H59 120.0 . . ? C55 C60 C59 120.8(6) . . ? C55 C60 H60 119.6 . . ? C59 C60 H60 119.6 . . ? C62 C61 P3 111.8(3) . . ? C62 C61 H61A 109.3 . . ? P3 C61 H61A 109.3 . . ? C62 C61 H61B 109.3 . . ? P3 C61 H61B 109.3 . . ? H61A C61 H61B 107.9 . . ? C61 C62 P4 110.2(3) . . ? C61 C62 H62A 109.6 . . ? P4 C62 H62A 109.6 . . ? C61 C62 H62B 109.6 . . ? P4 C62 H62B 109.6 . . ? H62A C62 H62B 108.1 . . ? C68 C63 C64 118.7(4) . . ? C68 C63 P4 124.1(4) . . ? C64 C63 P4 117.2(4) . . ? C65 C64 C63 121.1(5) . . ? C65 C64 H64 119.4 . . ? C63 C64 H64 119.4 . . ? C66 C65 C64 119.8(6) . . ? C66 C65 H65 120.1 . . ? C64 C65 H65 120.1 . . ? C65 C66 C67 119.5(5) . . ? C65 C66 H66 120.2 . . ? C67 C66 H66 120.2 . . ? C66 C67 C68 120.8(5) . . ? C66 C67 H67 119.6 . . ? C68 C67 H67 119.6 . . ? C63 C68 C67 120.0(5) . . ? C63 C68 H68 120.0 . . ? C67 C68 H68 120.0 . . ? C74 C69 C70 117.8(5) . . ? C74 C69 P4 123.0(4) . . ? C70 C69 P4 119.2(4) . . ? C71 C70 C69 120.7(6) . . ? C71 C70 H70 119.7 . . ? C69 C70 H70 119.7 . . ? C70 C71 C72 120.4(6) . . ? C70 C71 H71 119.8 . . ? C72 C71 H71 119.8 . . ? C73 C72 C71 119.3(5) . . ? C73 C72 H72 120.3 . . ? C71 C72 H72 120.3 . . ? C72 C73 C74 120.1(6) . . ? C72 C73 H73 119.9 . . ? C74 C73 H73 119.9 . . ? C73 C74 C69 121.6(6) . . ? C73 C74 H74 119.2 . . ? C69 C74 H74 119.2 . . ? N3 C75 C76 178.7(7) . . ? C75 C76 H76A 109.5 . . ? C75 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C75 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? N4 C77 C78 177.1(9) . . ? C77 C78 H78A 109.5 . . ? C77 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C77 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C45 N1 Cu2 162.0(5) . . ? C47 N2 Cu2 171.7(5) . . ? C75 N3 Cu4 163.4(5) . . ? C77 N4 Cu4 159.8(5) . . ? C19 P1 C31 102.9(2) . . ? C19 P1 C25 102.9(2) . . ? C31 P1 C25 103.1(2) . . ? C19 P1 Cu1 116.39(17) . . ? C31 P1 Cu1 113.51(16) . . ? C25 P1 Cu1 116.23(18) . . ? C33 P2 C39 103.3(2) . . ? C33 P2 C32 104.9(2) . . ? C39 P2 C32 103.7(2) . . ? C33 P2 Cu2 117.94(17) . . ? C39 P2 Cu2 111.71(17) . . ? C32 P2 Cu2 113.81(15) . . ? C49 P3 C55 103.0(2) . . ? C49 P3 C61 103.9(2) . . ? C55 P3 C61 103.5(2) . . ? C49 P3 Cu3 115.09(17) . . ? C55 P3 Cu3 115.29(18) . . ? C61 P3 Cu3 114.53(15) . . ? C63 P4 C69 104.0(2) . . ? C63 P4 C62 104.9(2) . . ? C69 P4 C62 104.3(2) . . ? C63 P4 Cu4 118.36(17) . . ? C69 P4 Cu4 111.08(16) . . ? C62 P4 Cu4 112.97(15) . . ? Fe2 S1 Fe1 72.87(5) . . ? Fe2 S1 Fe3 72.74(5) . . ? Fe1 S1 Fe3 74.66(5) . . ? Fe2 S1 Cu2 125.79(6) . 2_574 ? Fe1 S1 Cu2 133.59(6) . 2_574 ? Fe3 S1 Cu2 147.13(6) . 2_574 ? Fe6 S2 Fe4 74.20(5) . . ? Fe6 S2 Fe5 73.52(5) . . ? Fe4 S2 Fe5 76.14(5) . . ? Fe6 S2 Cu4 125.66(6) . 2_575 ? Fe4 S2 Cu4 142.99(6) . 2_575 ? Fe5 S2 Cu4 135.92(6) . 2_575 ? C3 Fe1 C1 95.8(3) . . ? C3 Fe1 C2 97.9(3) . . ? C1 Fe1 C2 108.8(3) . . ? C3 Fe1 S1 98.6(2) . . ? C1 Fe1 S1 143.28(19) . . ? C2 Fe1 S1 102.4(2) . . ? C3 Fe1 Cu1 152.3(2) . . ? C1 Fe1 Cu1 64.52(17) . . ? C2 Fe1 Cu1 72.6(2) . . ? S1 Fe1 Cu1 108.83(4) . . ? C3 Fe1 Fe2 96.4(2) . . ? C1 Fe1 Fe2 91.47(18) . . ? C2 Fe1 Fe2 153.7(2) . . ? S1 Fe1 Fe2 53.50(4) . . ? Cu1 Fe1 Fe2 103.06(3) . . ? C3 Fe1 Fe3 149.3(2) . . ? C1 Fe1 Fe3 102.69(18) . . ? C2 Fe1 Fe3 99.0(2) . . ? S1 Fe1 Fe3 52.74(4) . . ? Cu1 Fe1 Fe3 58.16(3) . . ? Fe2 Fe1 Fe3 59.20(3) . . ? C4 Fe2 C6 98.5(3) . . ? C4 Fe2 C5 95.4(4) . . ? C6 Fe2 C5 98.6(3) . . ? C4 Fe2 S1 101.5(2) . . ? C6 Fe2 S1 148.3(2) . . ? C5 Fe2 S1 103.7(2) . . ? C4 Fe2 Fe3 154.3(2) . . ? C6 Fe2 Fe3 101.51(19) . . ? C5 Fe2 Fe3 97.4(2) . . ? S1 Fe2 Fe3 53.76(4) . . ? C4 Fe2 Fe1 99.6(2) . . ? C6 Fe2 Fe1 98.9(2) . . ? C5 Fe2 Fe1 154.9(2) . . ? S1 Fe2 Fe1 53.63(4) . . ? Fe3 Fe2 Fe1 61.54(3) . . ? C8 Fe3 C9 109.9(3) . . ? C8 Fe3 C7 93.9(3) . . ? C9 Fe3 C7 95.6(3) . . ? C8 Fe3 S1 138.58(18) . . ? C9 Fe3 S1 108.3(2) . . ? C7 Fe3 S1 97.9(2) . . ? C8 Fe3 Cu1 69.33(17) . . ? C9 Fe3 Cu1 72.08(19) . . ? C7 Fe3 Cu1 153.0(2) . . ? S1 Fe3 Cu1 108.63(4) . . ? C8 Fe3 Fe2 85.88(18) . . ? C9 Fe3 Fe2 159.5(2) . . ? C7 Fe3 Fe2 96.3(2) . . ? S1 Fe3 Fe2 53.50(4) . . ? Cu1 Fe3 Fe2 103.05(3) . . ? C8 Fe3 Fe1 102.67(17) . . ? C9 Fe3 Fe1 103.2(2) . . ? C7 Fe3 Fe1 148.7(2) . . ? S1 Fe3 Fe1 52.60(4) . . ? Cu1 Fe3 Fe1 58.08(2) . . ? Fe2 Fe3 Fe1 59.26(3) . . ? C11 Fe4 C10 95.8(3) . . ? C11 Fe4 C12 106.4(4) . . ? C10 Fe4 C12 94.7(3) . . ? C11 Fe4 S2 108.8(2) . . ? C10 Fe4 S2 96.6(2) . . ? C12 Fe4 S2 141.6(3) . . ? C11 Fe4 Cu3 73.69(19) . . ? C10 Fe4 Cu3 154.3(2) . . ? C12 Fe4 Cu3 67.15(18) . . ? S2 Fe4 Cu3 108.88(4) . . ? C11 Fe4 Fe6 156.7(2) . . ? C10 Fe4 Fe6 100.2(2) . . ? C12 Fe4 Fe6 89.1(3) . . ? S2 Fe4 Fe6 52.75(4) . . ? Cu3 Fe4 Fe6 97.56(3) . . ? C11 Fe4 Fe5 99.32(19) . . ? C10 Fe4 Fe5 148.3(2) . . ? C12 Fe4 Fe5 107.3(2) . . ? S2 Fe4 Fe5 52.12(4) . . ? Cu3 Fe4 Fe5 57.33(2) . . ? Fe6 Fe4 Fe5 58.77(3) . . ? C15 Fe5 C13 99.2(3) . . ? C15 Fe5 C14 92.6(3) . . ? C13 Fe5 C14 107.4(2) . . ? C15 Fe5 S2 99.69(18) . . ? C13 Fe5 S2 104.58(18) . . ? C14 Fe5 S2 143.29(18) . . ? C15 Fe5 Cu3 151.75(18) . . ? C13 Fe5 Cu3 74.01(19) . . ? C14 Fe5 Cu3 64.69(17) . . ? S2 Fe5 Cu3 108.56(4) . . ? C15 Fe5 Fe6 99.12(18) . . ? C13 Fe5 Fe6 153.18(17) . . ? C14 Fe5 Fe6 91.17(17) . . ? S2 Fe5 Fe6 52.88(4) . . ? Cu3 Fe5 Fe6 97.96(3) . . ? C15 Fe5 Fe4 150.42(18) . . ? C13 Fe5 Fe4 96.15(17) . . ? C14 Fe5 Fe4 106.76(18) . . ? S2 Fe5 Fe4 51.74(4) . . ? Cu3 Fe5 Fe4 57.39(3) . . ? Fe6 Fe5 Fe4 59.26(3) . . ? C18 Fe6 C17 97.1(3) . . ? C18 Fe6 C16 96.5(3) . . ? C17 Fe6 C16 100.5(4) . . ? C18 Fe6 S2 104.2(2) . . ? C17 Fe6 S2 100.5(2) . . ? C16 Fe6 S2 148.2(2) . . ? C18 Fe6 Fe5 155.0(3) . . ? C17 Fe6 Fe5 98.4(2) . . ? C16 Fe6 Fe5 99.8(2) . . ? S2 Fe6 Fe5 53.60(4) . . ? C18 Fe6 Fe4 96.4(3) . . ? C17 Fe6 Fe4 152.7(2) . . ? C16 Fe6 Fe4 101.4(3) . . ? S2 Fe6 Fe4 53.05(4) . . ? Fe5 Fe6 Fe4 61.97(3) . . ? P1 Cu1 C1 105.76(15) . . ? P1 Cu1 C8 121.31(15) . . ? C1 Cu1 C8 89.47(18) . . ? P1 Cu1 Fe1 139.56(4) . . ? C1 Cu1 Fe1 42.52(15) . . ? C8 Cu1 Fe1 88.20(13) . . ? P1 Cu1 Fe3 156.27(4) . . ? C1 Cu1 Fe3 91.55(14) . . ? C8 Cu1 Fe3 41.12(15) . . ? Fe1 Cu1 Fe3 63.76(3) . . ? N1 Cu2 N2 94.66(19) . . ? N1 Cu2 P2 125.10(14) . . ? N2 Cu2 P2 108.28(14) . . ? N1 Cu2 S1 101.06(15) . 2_575 ? N2 Cu2 S1 100.38(14) . 2_575 ? P2 Cu2 S1 121.62(5) . 2_575 ? P3 Cu3 C14 107.13(14) . . ? P3 Cu3 C12 115.84(17) . . ? C14 Cu3 C12 102.2(3) . . ? P3 Cu3 Fe5 142.97(4) . . ? C14 Cu3 Fe5 43.37(15) . . ? C12 Cu3 Fe5 95.35(19) . . ? P3 Cu3 Fe4 151.74(4) . . ? C14 Cu3 Fe4 96.94(13) . . ? C12 Cu3 Fe4 42.50(16) . . ? Fe5 Cu3 Fe4 65.28(3) . . ? N4 Cu4 N3 92.20(18) . . ? N4 Cu4 P4 126.17(14) . . ? N3 Cu4 P4 112.48(15) . . ? N4 Cu4 S2 101.37(15) . 2_574 ? N3 Cu4 S2 98.61(15) . 2_574 ? P4 Cu4 S2 119.70(5) . 2_574 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.547 _refine_diff_density_min -0.381 _refine_diff_density_rms 0.062 _database_code_depnum_ccdc_archive 'CCDC 930776'