# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_global #TrackingRef '1_final.CIF' #========================================================================== _audit_creation_method SHELXL-97 _audit_creation_date '9 November 2005' data_1a _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H14 Fe N4' _chemical_formula_sum 'C13 H14 Fe N4' _chemical_formula_weight 282.13 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.274(3) _cell_length_b 7.4430(15) _cell_length_c 10.573(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.16(3) _cell_angle_gamma 90.00 _cell_volume 1186.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 493 _cell_measurement_theta_min 3.351 _cell_measurement_theta_max 18.061 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.579 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 584 _exptl_absorpt_coefficient_mu 1.256 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7044 _exptl_absorpt_correction_T_max 0.7044 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex 2' _diffrn_measurement_method 'scans in phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 24252 _diffrn_reflns_av_R_equivalents 0.0945 _diffrn_reflns_av_sigmaI/netI 0.0532 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 30.80 _reflns_number_total 3661 _reflns_number_gt 3278 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BrukerAXS, 1997)' _computing_cell_refinement 'SMART (BrukerAXS, 1997)' _computing_data_reduction 'SAINT+ (BrukerAXS, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XSEED _computing_publication_material CIFTAB _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^)+(0.0637P)^2^+2.2161P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3661 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0609 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.1558 _refine_ls_wR_factor_gt 0.1281 _refine_ls_goodness_of_fit_ref 1.158 _refine_ls_restrained_S_all 1.158 _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 Fe1 Fe 0.33799(2) 0.50661(4) 0.61264(3) 0.01487(13) Uani 1 1 d . . . N1 N -0.09839(16) 0.1535(4) 0.6194(2) 0.0298(5) Uani 1 1 d . . . N2 N -0.05380(16) 0.1388(3) 0.7442(2) 0.0273(5) Uani 1 1 d . . . C3 C 0.02630(19) 0.2007(4) 0.7448(2) 0.0263(5) Uani 1 1 d . . . H3 H 0.0711 0.2060 0.8181 0.032 Uiso 1 1 calc R . . N4 N 0.03630(14) 0.2565(3) 0.6253(2) 0.0202(4) Uani 1 1 d . . . C5 C -0.04269(18) 0.2257(4) 0.5514(3) 0.0265(5) Uani 1 1 d . . . H5 H -0.0562 0.2525 0.4625 0.032 Uiso 1 1 calc R . . N6 N 0.11020(15) 0.3361(3) 0.5834(2) 0.0218(4) Uani 1 1 d . . . H6 H 0.1119 0.4473 0.5555 0.026 Uiso 1 1 calc R . . C7 C 0.18420(17) 0.2080(3) 0.5927(2) 0.0211(5) Uani 1 1 d . . . H7B H 0.1650 0.0996 0.5414 0.025 Uiso 1 1 calc R . . H7A H 0.2017 0.1706 0.6830 0.025 Uiso 1 1 calc R . . C8 C 0.26218(16) 0.2913(3) 0.5449(2) 0.0175(4) Uani 1 1 d . . . C9 C 0.35181(17) 0.2372(3) 0.5856(2) 0.0191(4) Uani 1 1 d . . . H9 H 0.3717 0.1506 0.6498 0.023 Uiso 1 1 calc R . . C10 C 0.40662(17) 0.3367(3) 0.5125(2) 0.0197(4) Uani 1 1 d . . . H10 H 0.4692 0.3275 0.5196 0.024 Uiso 1 1 calc R . . C11 C 0.35102(17) 0.4515(3) 0.4276(2) 0.0197(4) Uani 1 1 d . . . H11 H 0.3700 0.5329 0.3683 0.024 Uiso 1 1 calc R . . C12 C 0.26175(16) 0.4234(3) 0.4470(2) 0.0192(4) Uani 1 1 d . . . H12 H 0.2108 0.4824 0.4025 0.023 Uiso 1 1 calc R . . C13 C 0.3647(3) 0.7710(4) 0.6371(3) 0.0408(9) Uani 1 1 d . . . H13 H 0.3753 0.8515 0.5715 0.049 Uiso 1 1 calc R . . C14 C 0.2816(2) 0.7326(5) 0.6718(4) 0.0446(10) Uani 1 1 d . . . H14 H 0.2263 0.7827 0.6343 0.054 Uiso 1 1 calc R . . C15 C 0.2951(2) 0.6055(5) 0.7731(3) 0.0360(7) Uani 1 1 d . . . H15 H 0.2506 0.5557 0.8159 0.043 Uiso 1 1 calc R . . C16 C 0.3865(2) 0.5665(4) 0.7987(2) 0.0269(5) Uani 1 1 d . . . H16 H 0.4144 0.4842 0.8611 0.032 Uiso 1 1 calc R . . C17 C 0.42931(19) 0.6700(4) 0.7160(3) 0.0307(6) Uani 1 1 d . . . H17 H 0.4912 0.6715 0.7137 0.037 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0200(2) 0.01141(18) 0.0135(2) -0.00137(10) 0.00336(13) -0.00031(10) N1 0.0249(11) 0.0422(14) 0.0234(11) -0.0003(10) 0.0072(9) -0.0078(10) N2 0.0284(11) 0.0327(12) 0.0228(11) 0.0043(9) 0.0098(9) -0.0024(9) C3 0.0284(13) 0.0340(14) 0.0173(11) 0.0025(10) 0.0061(9) -0.0038(10) N4 0.0222(10) 0.0228(10) 0.0161(9) -0.0001(7) 0.0047(7) -0.0044(8) C5 0.0233(12) 0.0367(14) 0.0199(11) 0.0022(10) 0.0048(9) -0.0039(10) N6 0.0231(10) 0.0180(9) 0.0261(11) 0.0015(8) 0.0094(8) -0.0028(7) C7 0.0237(11) 0.0172(10) 0.0235(11) -0.0004(9) 0.0066(9) -0.0025(8) C8 0.0218(10) 0.0152(9) 0.0158(10) -0.0023(8) 0.0034(8) -0.0015(8) C9 0.0276(11) 0.0127(9) 0.0181(10) -0.0004(8) 0.0068(9) 0.0016(8) C10 0.0240(11) 0.0162(10) 0.0206(11) -0.0020(8) 0.0085(9) 0.0024(8) C11 0.0276(12) 0.0178(10) 0.0146(10) -0.0014(8) 0.0064(8) -0.0016(9) C12 0.0225(11) 0.0216(11) 0.0128(9) 0.0001(8) 0.0002(8) -0.0013(8) C13 0.085(3) 0.0156(12) 0.0193(12) -0.0053(10) 0.0015(14) -0.0140(14) C14 0.0435(18) 0.0312(15) 0.052(2) -0.0275(15) -0.0152(15) 0.0206(13) C15 0.0359(15) 0.0386(16) 0.0396(16) -0.0254(13) 0.0245(13) -0.0149(12) C16 0.0416(15) 0.0281(13) 0.0087(10) -0.0016(9) -0.0035(9) 0.0038(11) C17 0.0269(13) 0.0409(16) 0.0259(13) -0.0175(12) 0.0093(10) -0.0133(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C13 2.018(3) . ? Fe1 C17 2.033(3) . ? Fe1 C14 2.033(3) . ? Fe1 C16 2.038(3) . ? Fe1 C11 2.039(2) . ? Fe1 C8 2.039(2) . ? Fe1 C12 2.039(2) . ? Fe1 C9 2.041(2) . ? Fe1 C10 2.042(2) . ? Fe1 C15 2.050(3) . ? N1 C5 1.314(3) . ? N1 N2 1.389(3) . ? N2 C3 1.306(4) . ? C3 N4 1.361(3) . ? C3 H3 0.9500 . ? N4 C5 1.349(3) . ? N4 N6 1.407(3) . ? C5 H5 0.9500 . ? N6 C7 1.470(3) . ? N6 H6 0.8800 . ? C7 C8 1.500(3) . ? C7 H7B 0.9900 . ? C7 H7A 0.9900 . ? C8 C9 1.426(3) . ? C8 C12 1.427(3) . ? C9 C10 1.433(3) . ? C9 H9 0.9500 . ? C10 C11 1.419(4) . ? C10 H10 0.9500 . ? C11 C12 1.426(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C17 1.405(5) . ? C13 C14 1.406(6) . ? C13 H13 0.9500 . ? C14 C15 1.419(6) . ? C14 H14 0.9500 . ? C15 C16 1.410(4) . ? C15 H15 0.9500 . ? C16 C17 1.402(4) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 Fe1 C17 40.57(15) . . ? C13 Fe1 C14 40.62(17) . . ? C17 Fe1 C14 68.16(14) . . ? C13 Fe1 C16 68.15(12) . . ? C17 Fe1 C16 40.29(12) . . ? C14 Fe1 C16 68.22(13) . . ? C13 Fe1 C11 105.69(12) . . ? C17 Fe1 C11 118.20(11) . . ? C14 Fe1 C11 124.93(14) . . ? C16 Fe1 C11 153.35(12) . . ? C13 Fe1 C8 154.61(14) . . ? C17 Fe1 C8 164.05(13) . . ? C14 Fe1 C8 120.89(13) . . ? C16 Fe1 C8 127.58(11) . . ? C11 Fe1 C8 69.00(10) . . ? C13 Fe1 C12 118.84(12) . . ? C17 Fe1 C12 153.19(12) . . ? C14 Fe1 C12 107.66(12) . . ? C16 Fe1 C12 164.96(12) . . ? C11 Fe1 C12 40.94(10) . . ? C8 Fe1 C12 40.97(9) . . ? C13 Fe1 C9 162.29(16) . . ? C17 Fe1 C9 125.84(13) . . ? C14 Fe1 C9 156.06(15) . . ? C16 Fe1 C9 108.68(11) . . ? C11 Fe1 C9 68.90(10) . . ? C8 Fe1 C9 40.91(10) . . ? C12 Fe1 C9 68.84(10) . . ? C13 Fe1 C10 124.07(14) . . ? C17 Fe1 C10 106.50(11) . . ? C14 Fe1 C10 161.66(16) . . ? C16 Fe1 C10 119.86(11) . . ? C11 Fe1 C10 40.69(10) . . ? C8 Fe1 C10 68.96(10) . . ? C12 Fe1 C10 68.71(10) . . ? C9 Fe1 C10 41.08(9) . . ? C13 Fe1 C15 68.19(14) . . ? C17 Fe1 C15 67.84(12) . . ? C14 Fe1 C15 40.66(16) . . ? C16 Fe1 C15 40.35(13) . . ? C11 Fe1 C15 163.51(14) . . ? C8 Fe1 C15 109.54(11) . . ? C12 Fe1 C15 127.28(12) . . ? C9 Fe1 C15 121.50(12) . . ? C10 Fe1 C15 155.40(14) . . ? C5 N1 N2 106.9(2) . . ? C3 N2 N1 107.1(2) . . ? N2 C3 N4 110.3(2) . . ? N2 C3 H3 124.9 . . ? N4 C3 H3 124.9 . . ? C5 N4 C3 105.3(2) . . ? C5 N4 N6 125.3(2) . . ? C3 N4 N6 129.4(2) . . ? N1 C5 N4 110.5(2) . . ? N1 C5 H5 124.8 . . ? N4 C5 H5 124.8 . . ? N4 N6 C7 110.6(2) . . ? N4 N6 H6 124.7 . . ? C7 N6 H6 124.7 . . ? N6 C7 C8 110.7(2) . . ? N6 C7 H7B 109.5 . . ? C8 C7 H7B 109.5 . . ? N6 C7 H7A 109.5 . . ? C8 C7 H7A 109.5 . . ? H7B C7 H7A 108.1 . . ? C9 C8 C12 107.8(2) . . ? C9 C8 C7 123.9(2) . . ? C12 C8 C7 128.1(2) . . ? C9 C8 Fe1 69.60(13) . . ? C12 C8 Fe1 69.50(14) . . ? C7 C8 Fe1 130.03(17) . . ? C8 C9 C10 107.9(2) . . ? C8 C9 Fe1 69.49(13) . . ? C10 C9 Fe1 69.52(13) . . ? C8 C9 H9 126.1 . . ? C10 C9 H9 126.1 . . ? Fe1 C9 H9 126.5 . . ? C11 C10 C9 108.1(2) . . ? C11 C10 Fe1 69.53(13) . . ? C9 C10 Fe1 69.40(13) . . ? C11 C10 H10 126.0 . . ? C9 C10 H10 126.0 . . ? Fe1 C10 H10 126.7 . . ? C10 C11 C12 108.1(2) . . ? C10 C11 Fe1 69.79(14) . . ? C12 C11 Fe1 69.52(14) . . ? C10 C11 H11 126.0 . . ? C12 C11 H11 126.0 . . ? Fe1 C11 H11 126.3 . . ? C11 C12 C8 108.1(2) . . ? C11 C12 Fe1 69.54(14) . . ? C8 C12 Fe1 69.54(13) . . ? C11 C12 H12 125.9 . . ? C8 C12 H12 125.9 . . ? Fe1 C12 H12 126.6 . . ? C17 C13 C14 108.3(3) . . ? C17 C13 Fe1 70.29(17) . . ? C14 C13 Fe1 70.28(17) . . ? C17 C13 H13 125.8 . . ? C14 C13 H13 125.8 . . ? Fe1 C13 H13 125.2 . . ? C13 C14 C15 107.7(3) . . ? C13 C14 Fe1 69.10(17) . . ? C15 C14 Fe1 70.30(16) . . ? C13 C14 H14 126.2 . . ? C15 C14 H14 126.2 . . ? Fe1 C14 H14 126.0 . . ? C16 C15 C14 107.6(3) . . ? C16 C15 Fe1 69.36(15) . . ? C14 C15 Fe1 69.05(17) . . ? C16 C15 H15 126.2 . . ? C14 C15 H15 126.2 . . ? Fe1 C15 H15 127.0 . . ? C17 C16 C15 108.2(3) . . ? C17 C16 Fe1 69.67(15) . . ? C15 C16 Fe1 70.29(16) . . ? C17 C16 H16 125.9 . . ? C15 C16 H16 125.9 . . ? Fe1 C16 H16 125.7 . . ? C16 C17 C13 108.1(3) . . ? C16 C17 Fe1 70.04(16) . . ? C13 C17 Fe1 69.14(17) . . ? C16 C17 H17 125.9 . . ? C13 C17 H17 125.9 . . ? Fe1 C17 H17 126.5 . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.420 _refine_diff_density_min -1.056 _refine_diff_density_rms 0.141 _database_code_depnum_ccdc_archive 'CCDC 922180' ####################################################################### # # 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_global #TrackingRef '1_final.CIF' #========================================================================== _audit_creation_method SHELXL-97 _audit_creation_date '9 November 2005' # Attachment '6_final.CIF' #========================================================================== data_1 #TrackingRef '6_final.CIF' #========================================================================== _audit_creation_method SHELXL-97 _audit_creation_date '9 November 2005' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; 2(C27 H26 Cu Fe2 N9 S), 2(Cl O4), C4 H10 O, 2(C2 H3 N) ; _chemical_formula_sum 'C62 H68 Cl2 Cu2 Fe4 N20 O9 S2' _chemical_formula_weight 1722.86 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' 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' Cl Cl 0.1484 0.1585 '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 monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 26.769(5) _cell_length_b 7.1730(14) _cell_length_c 37.396(8) _cell_angle_alpha 90.00 _cell_angle_beta 91.33(3) _cell_angle_gamma 90.00 _cell_volume 7179(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.594 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3520 _exptl_absorpt_coefficient_mu 1.570 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6502 _exptl_absorpt_correction_T_max 0.6502 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Australian synchrotron' _diffrn_radiation_monochromator silicon _diffrn_measurement_device_type 'ADSC Quantum 210r' _diffrn_measurement_method 'scans in phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 58288 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_sigmaI/netI 0.0362 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -49 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 28.59 _reflns_number_total 16940 _reflns_number_gt 14255 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Blu-Ice (McPhillips et al, 2002)' _computing_cell_refinement 'XDS (Kabsch, 1993)' _computing_data_reduction 'XDS (Kabsch, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-SEED _computing_publication_material 'XCIF V6.12 (BrukerAXS, 2001).' _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^)+(0.0460P)^2^+55.0899P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16940 _refine_ls_number_parameters 914 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0843 _refine_ls_R_factor_gt 0.0734 _refine_ls_wR_factor_ref 0.1871 _refine_ls_wR_factor_gt 0.1815 _refine_ls_goodness_of_fit_ref 1.156 _refine_ls_restrained_S_all 1.156 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.24699(2) 0.09056(9) 0.749087(17) 0.02177(14) Uani 1 1 d . . . Fe1 Fe 0.10954(3) 0.03442(11) 0.90209(2) 0.02522(17) Uani 1 1 d . . . Fe2 Fe 0.42768(3) -0.10771(13) 0.94669(2) 0.02862(18) Uani 1 1 d . . . S1 S 0.25072(8) -0.1060(3) 0.63586(5) 0.0581(6) Uani 1 1 d . . . N6 N 0.28735(15) -0.0592(6) 0.78639(11) 0.0218(8) Uani 1 1 d . . . N2 N 0.18754(15) -0.0701(6) 0.76049(11) 0.0202(8) Uani 1 1 d . . . N1 N 0.26854(17) -0.1614(8) 0.70886(12) 0.0307(10) Uani 1 1 d . . . N4 N 0.11753(15) -0.1742(7) 0.78031(11) 0.0240(9) Uani 1 1 d . . . N8 N 0.33429(15) -0.1373(6) 0.83207(11) 0.0234(9) Uani 1 1 d . . . C2 C 0.14874(17) -0.3193(8) 0.77655(14) 0.0237(10) Uani 1 1 d . . . H2 H 0.1409 -0.4451 0.7820 0.028 Uiso 1 1 calc R . . N5 N 0.06993(16) -0.1886(8) 0.79534(13) 0.0316(11) Uani 1 1 d . . . C3 C 0.14275(19) -0.0224(8) 0.77007(13) 0.0255(10) Uani 1 1 d . . . H3 H 0.1299 0.1011 0.7698 0.031 Uiso 1 1 calc R . . C1 C 0.2622(2) -0.1334(8) 0.67838(15) 0.0306(12) Uani 1 1 d . . . N3 N 0.19156(14) -0.2625(6) 0.76425(11) 0.0204(8) Uani 1 1 d . . . N7 N 0.29390(15) -0.2487(6) 0.78580(11) 0.0207(8) Uani 1 1 d . . . N9 N 0.36330(16) -0.1300(7) 0.86415(11) 0.0281(10) Uani 1 1 d . . . C15 C 0.31187(18) 0.0058(8) 0.81454(14) 0.0260(11) Uani 1 1 d . . . H15 H 0.3136 0.1331 0.8215 0.031 Uiso 1 1 calc R . . C16 C 0.32255(18) -0.2943(8) 0.81365(13) 0.0228(10) Uani 1 1 d . . . H16 H 0.3331 -0.4169 0.8197 0.027 Uiso 1 1 calc R . . C4 C 0.0663(2) -0.0603(10) 0.82678(15) 0.0336(13) Uani 1 1 d . . . H4A H 0.0692 0.0703 0.8185 0.040 Uiso 1 1 calc R . . H4B H 0.0331 -0.0751 0.8376 0.040 Uiso 1 1 calc R . . C18 C 0.3576(2) -0.0410(9) 0.92754(14) 0.0319(12) Uani 1 1 d . . . C17 C 0.3297(2) -0.1055(10) 0.89482(15) 0.0350(13) Uani 1 1 d . . . H17A H 0.3130 -0.2255 0.8999 0.042 Uiso 1 1 calc R . . H17B H 0.3035 -0.0132 0.8884 0.042 Uiso 1 1 calc R . . C22 C 0.3878(2) 0.1216(9) 0.93105(16) 0.0358(13) Uani 1 1 d . . . H22 H 0.3961 0.2051 0.9124 0.043 Uiso 1 1 calc R . . C24 C 0.4551(3) -0.3727(11) 0.9451(2) 0.0498(18) Uani 1 1 d . . . H24 H 0.4368 -0.4833 0.9496 0.060 Uiso 1 1 calc R . . C7 C 0.1780(2) -0.0738(10) 0.88973(18) 0.0405(15) Uani 1 1 d . . . H7 H 0.2097 -0.0348 0.8989 0.049 Uiso 1 1 calc R . . C5 C 0.10603(18) -0.0986(8) 0.85436(14) 0.0262(11) Uani 1 1 d . . . C13 C 0.1110(3) 0.3065(10) 0.91794(19) 0.0429(15) Uani 1 1 d . . . H13 H 0.1352 0.3966 0.9114 0.052 Uiso 1 1 calc R . . C8 C 0.1481(3) -0.2124(10) 0.90423(19) 0.0439(16) Uani 1 1 d . . . H8 H 0.1559 -0.2834 0.9251 0.053 Uiso 1 1 calc R . . C6 C 0.15251(19) -0.0001(9) 0.85857(15) 0.0315(12) Uani 1 1 d . . . H6 H 0.1643 0.0962 0.8435 0.038 Uiso 1 1 calc R . . C23 C 0.4603(3) -0.2856(12) 0.91148(19) 0.0496(19) Uani 1 1 d . . . H23 H 0.4462 -0.3294 0.8895 0.060 Uiso 1 1 calc R . . C20 C 0.3828(2) -0.0112(10) 0.98652(16) 0.0385(14) Uani 1 1 d . . . H20 H 0.3866 -0.0331 1.0115 0.046 Uiso 1 1 calc R . . C21 C 0.4034(2) 0.1367(10) 0.96771(16) 0.0380(14) Uani 1 1 d . . . H21 H 0.4242 0.2316 0.9776 0.046 Uiso 1 1 calc R . . C26 C 0.5037(2) -0.1108(11) 0.95249(18) 0.0408(15) Uani 1 1 d . . . H26 H 0.5240 -0.0160 0.9631 0.049 Uiso 1 1 calc R . . C11 C 0.0700(4) 0.0795(12) 0.9475(2) 0.063(2) Uani 1 1 d . . . H11 H 0.0617 -0.0112 0.9650 0.076 Uiso 1 1 calc R . . C14 C 0.0662(3) 0.2659(12) 0.8991(2) 0.056(2) Uani 1 1 d . . . H14 H 0.0548 0.3241 0.8776 0.068 Uiso 1 1 calc R . . C25 C 0.4822(2) -0.2652(11) 0.97084(18) 0.0428(15) Uani 1 1 d . . . H25 H 0.4855 -0.2911 0.9957 0.051 Uiso 1 1 calc R . . C19 C 0.3553(2) -0.1225(10) 0.96206(16) 0.0375(14) Uani 1 1 d . . . H19 H 0.3381 -0.2341 0.9677 0.045 Uiso 1 1 calc R . . C10 C 0.0411(3) 0.1248(13) 0.9175(3) 0.070(3) Uani 1 1 d . . . H10 H 0.0100 0.0702 0.9107 0.084 Uiso 1 1 calc R . . C12 C 0.1136(3) 0.1902(11) 0.94792(17) 0.0455(16) Uani 1 1 d . . . H12 H 0.1399 0.1864 0.9654 0.055 Uiso 1 1 calc R . . C27 C 0.4896(2) -0.1235(11) 0.91573(17) 0.0435(16) Uani 1 1 d . . . H27 H 0.4983 -0.0385 0.8974 0.052 Uiso 1 1 calc R . . Fe3 Fe 0.57679(3) 0.04003(10) 0.552392(18) 0.02013(15) Uani 1 1 d . . . Cu2 Cu 0.74543(2) -0.24693(9) 0.753648(16) 0.01907(13) Uani 1 1 d . . . Fe4 Fe 0.86808(4) -0.01741(15) 0.59442(2) 0.0432(2) Uani 1 1 d . . . Cl1 Cl 0.57288(4) -0.56739(19) 0.68473(3) 0.0257(3) Uani 1 1 d . . . S2 S 0.75617(6) 0.0490(3) 0.86405(4) 0.0388(3) Uani 1 1 d . . . N12 N 0.71400(14) 0.0916(6) 0.71141(11) 0.0195(8) Uani 1 1 d . . . O5 O 0.57064(16) -0.7506(7) 0.66866(12) 0.0396(10) Uani 1 1 d . . . N16 N 0.81287(14) 0.0826(6) 0.73733(11) 0.0197(8) Uani 1 1 d . . . N17 N 0.88232(15) -0.0425(7) 0.72068(11) 0.0238(9) Uani 1 1 d . . . N13 N 0.66736(14) -0.0096(6) 0.66736(11) 0.0201(8) Uani 1 1 d . . . N15 N 0.80820(14) -0.1103(6) 0.73896(10) 0.0181(8) Uani 1 1 d . . . N11 N 0.70649(14) -0.0967(6) 0.71607(10) 0.0188(8) Uani 1 1 d . . . C42 C 0.85049(18) -0.1817(8) 0.72901(13) 0.0235(10) Uani 1 1 d . . . H42 H 0.8578 -0.3112 0.7278 0.028 Uiso 1 1 calc R . . C29 C 0.67778(18) -0.1551(8) 0.68922(13) 0.0221(10) Uani 1 1 d . . . H29 H 0.6663 -0.2792 0.6858 0.026 Uiso 1 1 calc R . . N14 N 0.63873(15) -0.0259(7) 0.63561(11) 0.0250(9) Uani 1 1 d . . . O3 O 0.62326(14) -0.5321(6) 0.69718(11) 0.0321(9) Uani 1 1 d . . . N10 N 0.73007(17) -0.0130(8) 0.79255(13) 0.0330(11) Uani 1 1 d . . . C28 C 0.7397(2) 0.0149(8) 0.82236(15) 0.0298(11) Uani 1 1 d . . . O2 O 0.53979(14) -0.5626(7) 0.71497(10) 0.0350(9) Uani 1 1 d . . . C30 C 0.69004(18) 0.1419(8) 0.68210(13) 0.0231(10) Uani 1 1 d . . . H30 H 0.6887 0.2648 0.6727 0.028 Uiso 1 1 calc R . . C39 C 0.5659(2) 0.3149(8) 0.54181(15) 0.0284(11) Uani 1 1 d . . . H39 H 0.5881 0.3940 0.5294 0.034 Uiso 1 1 calc R . . N18 N 0.92950(15) -0.0547(7) 0.70484(12) 0.0292(10) Uani 1 1 d . . . C32 C 0.64013(18) -0.0819(7) 0.57219(13) 0.0229(10) Uani 1 1 d . . . C36 C 0.6473(2) -0.0226(8) 0.53620(14) 0.0275(11) Uani 1 1 d . . . H36 H 0.6718 0.0630 0.5284 0.033 Uiso 1 1 calc R . . C37 C 0.50257(19) 0.1087(8) 0.55361(14) 0.0272(11) Uani 1 1 d . . . H37 H 0.4751 0.0256 0.5507 0.033 Uiso 1 1 calc R . . C44 C 0.9232(2) -0.1273(9) 0.66753(15) 0.0330(13) Uani 1 1 d . . . H44A H 0.9561 -0.1343 0.6562 0.040 Uiso 1 1 calc R . . H44B H 0.9089 -0.2545 0.6681 0.040 Uiso 1 1 calc R . . C33 C 0.59958(19) -0.2139(7) 0.57237(15) 0.0254(10) Uani 1 1 d . . . H33 H 0.5870 -0.2770 0.5926 0.030 Uiso 1 1 calc R . . C31 C 0.67073(18) -0.0230(8) 0.60395(13) 0.0244(10) Uani 1 1 d . . . H31A H 0.6993 -0.1090 0.6076 0.029 Uiso 1 1 calc R . . H31B H 0.6840 0.1042 0.6002 0.029 Uiso 1 1 calc R . . C38 C 0.52683(19) 0.2070(8) 0.52591(14) 0.0253(10) Uani 1 1 d . . . H38 H 0.5184 0.2015 0.5011 0.030 Uiso 1 1 calc R . . O4 O 0.55811(17) -0.4310(7) 0.65859(12) 0.0457(12) Uani 1 1 d . . . C46 C 0.8360(2) -0.0188(10) 0.64348(16) 0.0371(14) Uani 1 1 d . . . H46 H 0.8163 -0.1145 0.6536 0.045 Uiso 1 1 calc R . . C34 C 0.5821(2) -0.2313(8) 0.53619(15) 0.0292(11) Uani 1 1 d . . . H34 H 0.5552 -0.3088 0.5282 0.035 Uiso 1 1 calc R . . C45 C 0.8898(2) -0.0042(9) 0.64636(15) 0.0328(12) Uani 1 1 d . . . C41 C 0.5272(2) 0.1581(8) 0.58689(14) 0.0284(11) Uani 1 1 d . . . H41 H 0.5188 0.1135 0.6099 0.034 Uiso 1 1 calc R . . C35 C 0.6108(2) -0.1155(9) 0.51410(15) 0.0307(12) Uani 1 1 d . . . H35 H 0.6066 -0.1017 0.4889 0.037 Uiso 1 1 calc R . . C40 C 0.5661(2) 0.2848(8) 0.57929(14) 0.0269(11) Uani 1 1 d . . . H40 H 0.5884 0.3401 0.5963 0.032 Uiso 1 1 calc R . . C54 C 0.8458(3) -0.2533(12) 0.56922(18) 0.0481(17) Uani 1 1 d . . . H54 H 0.8230 -0.3425 0.5781 0.058 Uiso 1 1 calc R . . C53 C 0.8324(5) -0.0995(15) 0.5484(2) 0.077(3) Uani 1 1 d . . . H53 H 0.7996 -0.0648 0.5408 0.093 Uiso 1 1 calc R . . C51 C 0.9173(5) -0.104(2) 0.5573(3) 0.108(5) Uani 1 1 d . . . H51 H 0.9517 -0.0710 0.5565 0.129 Uiso 1 1 calc R . . C50 C 0.8974(3) -0.2576(14) 0.5751(2) 0.062(2) Uani 1 1 d . . . H50 H 0.9156 -0.3479 0.5887 0.074 Uiso 1 1 calc R . . C49 C 0.9042(3) 0.1629(11) 0.62822(19) 0.0507(18) Uani 1 1 d . . . H49 H 0.9372 0.2103 0.6260 0.061 Uiso 1 1 calc R . . C47 C 0.8176(3) 0.1344(12) 0.6229(2) 0.057(2) Uani 1 1 d . . . H47 H 0.7837 0.1576 0.6163 0.068 Uiso 1 1 calc R . . Cl2 Cl 0.93121(5) 0.1849(2) 0.31611(4) 0.0317(3) Uani 1 1 d . . . O8 O 0.96419(15) 0.2042(7) 0.28604(11) 0.0396(10) Uani 1 1 d . . . O7 O 0.88041(15) 0.1748(7) 0.30311(12) 0.0404(10) Uani 1 1 d . . . O6 O 0.93717(19) 0.3414(9) 0.33960(15) 0.0617(16) Uani 1 1 d . . . O9 O 0.9436(2) 0.0198(10) 0.33516(17) 0.076(2) Uani 1 1 d . . . C9 C 0.1036(2) -0.2301(8) 0.88256(15) 0.0320(12) Uani 1 1 d . . . H9 H 0.0771 -0.3152 0.8864 0.038 Uiso 1 1 calc R . . C48 C 0.8587(4) 0.2445(12) 0.6140(2) 0.066(2) Uani 1 1 d . . . H48 H 0.8569 0.3568 0.6006 0.079 Uiso 1 1 calc R . . C52 C 0.8769(7) -0.0060(18) 0.5407(2) 0.112(6) Uani 1 1 d . . . H52 H 0.8795 0.1041 0.5267 0.134 Uiso 1 1 calc R . . C62 C 0.9506(3) -0.3334(11) 0.2785(2) 0.0482(17) Uani 1 1 d . . . C55 C 0.2142(3) -0.0095(12) 1.0403(2) 0.056(2) Uani 1 1 d . . . H55A H 0.2295 0.0588 1.0604 0.084 Uiso 1 1 calc R . . H55B H 0.2174 -0.1438 1.0445 0.084 Uiso 1 1 calc R . . H55C H 0.1788 0.0238 1.0380 0.084 Uiso 1 1 calc R . . C60 C 0.5503(3) -1.0457(10) 0.7244(2) 0.0464(16) Uani 1 1 d . . . C59 C 0.5127(3) -1.0785(11) 0.6957(2) 0.0492(17) Uani 1 1 d . . . H59A H 0.4932 -1.1899 0.7013 0.074 Uiso 1 1 calc R . . H59B H 0.5295 -1.0970 0.6729 0.074 Uiso 1 1 calc R . . H59C H 0.4903 -0.9705 0.6937 0.074 Uiso 1 1 calc R . . C61 C 0.9913(3) -0.3296(12) 0.3051(2) 0.0528(19) Uani 1 1 d . . . H61A H 1.0140 -0.4339 0.3009 0.079 Uiso 1 1 calc R . . H61B H 0.9776 -0.3407 0.3291 0.079 Uiso 1 1 calc R . . H61C H 1.0095 -0.2118 0.3032 0.079 Uiso 1 1 calc R . . C57 C 0.2572(4) 0.2908(13) 0.9678(2) 0.065(2) Uani 1 1 d . . . H57A H 0.2453 0.2162 0.9470 0.077 Uiso 1 1 calc R . . H57B H 0.2937 0.2714 0.9707 0.077 Uiso 1 1 calc R . . C56 C 0.2397(4) 0.0399(13) 1.0071(3) 0.071(3) Uani 1 1 d . . . H56A H 0.2758 0.0122 1.0099 0.085 Uiso 1 1 calc R . . H56B H 0.2261 -0.0369 0.9871 0.085 Uiso 1 1 calc R . . N20 N 0.9191(2) -0.3326(9) 0.2568(2) 0.0579(18) Uani 1 1 d . . . N19 N 0.5792(2) -1.0186(10) 0.7470(2) 0.062(2) Uani 1 1 d . . . O1 O 0.23320(16) 0.2307(7) 0.99880(11) 0.0375(10) Uani 1 1 d . . . C58 C 0.2469(3) 0.4907(12) 0.9612(2) 0.055(2) Uani 1 1 d . . . H58A H 0.2107 0.5101 0.9588 0.082 Uiso 1 1 calc R . . H58B H 0.2628 0.5296 0.9390 0.082 Uiso 1 1 calc R . . H58C H 0.2602 0.5648 0.9812 0.082 Uiso 1 1 calc R . . C43 C 0.85791(17) 0.1186(8) 0.72591(13) 0.0219(10) Uani 1 1 d . . . H43 H 0.8711 0.2395 0.7220 0.026 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0165(3) 0.0183(3) 0.0301(3) 0.0062(2) -0.0074(2) -0.0030(2) Fe1 0.0222(3) 0.0256(4) 0.0280(4) -0.0043(3) 0.0011(3) -0.0018(3) Fe2 0.0218(4) 0.0379(5) 0.0259(4) -0.0017(3) -0.0030(3) -0.0022(3) S1 0.0724(13) 0.0706(14) 0.0317(8) 0.0106(8) 0.0074(8) 0.0304(11) N6 0.0187(19) 0.015(2) 0.031(2) 0.0027(16) -0.0056(15) -0.0027(15) N2 0.0213(19) 0.018(2) 0.0212(18) 0.0006(15) -0.0051(14) 0.0018(16) N1 0.022(2) 0.042(3) 0.028(2) -0.001(2) -0.0014(17) -0.004(2) N4 0.0180(19) 0.029(2) 0.025(2) -0.0044(17) -0.0041(15) 0.0016(17) N8 0.0182(19) 0.027(2) 0.025(2) 0.0021(17) -0.0061(15) -0.0013(16) C2 0.016(2) 0.024(3) 0.031(3) -0.0032(19) -0.0036(18) -0.0003(18) N5 0.017(2) 0.045(3) 0.033(2) -0.010(2) 0.0006(17) -0.0008(19) C3 0.025(2) 0.025(3) 0.027(2) 0.0007(19) -0.0014(19) 0.004(2) C1 0.029(3) 0.028(3) 0.036(3) 0.000(2) 0.004(2) 0.001(2) N3 0.0156(18) 0.015(2) 0.030(2) -0.0021(16) -0.0061(15) -0.0015(15) N7 0.0182(18) 0.018(2) 0.025(2) -0.0008(15) -0.0045(15) 0.0031(15) N9 0.020(2) 0.042(3) 0.022(2) 0.0000(18) -0.0081(16) 0.0004(19) C15 0.020(2) 0.024(3) 0.033(3) 0.001(2) -0.0083(19) -0.0046(19) C16 0.018(2) 0.025(3) 0.025(2) 0.0020(19) -0.0036(17) 0.0045(19) C4 0.020(2) 0.047(4) 0.034(3) -0.009(3) -0.003(2) 0.007(2) C18 0.022(2) 0.048(4) 0.026(3) 0.001(2) -0.0033(19) 0.004(2) C17 0.024(3) 0.053(4) 0.028(3) 0.002(3) -0.001(2) -0.005(3) C22 0.037(3) 0.036(4) 0.034(3) 0.000(2) -0.002(2) 0.006(3) C24 0.042(4) 0.035(4) 0.072(5) -0.004(3) -0.017(3) 0.012(3) C7 0.024(3) 0.050(4) 0.048(4) -0.015(3) -0.009(2) 0.006(3) C5 0.018(2) 0.029(3) 0.031(3) -0.006(2) 0.0016(18) 0.002(2) C13 0.045(4) 0.029(4) 0.054(4) -0.010(3) 0.011(3) -0.006(3) C8 0.048(4) 0.034(4) 0.050(4) 0.002(3) -0.006(3) 0.018(3) C6 0.020(2) 0.041(4) 0.034(3) -0.006(2) 0.005(2) -0.002(2) C23 0.040(3) 0.065(5) 0.044(4) -0.021(3) -0.014(3) 0.015(3) C20 0.028(3) 0.057(4) 0.031(3) -0.001(3) 0.001(2) 0.004(3) C21 0.039(3) 0.042(4) 0.033(3) -0.008(3) -0.004(2) 0.011(3) C26 0.017(2) 0.058(4) 0.048(4) -0.010(3) 0.000(2) 0.002(3) C11 0.090(6) 0.046(5) 0.056(5) -0.013(4) 0.041(5) -0.015(4) C14 0.052(4) 0.056(5) 0.061(5) -0.024(4) -0.018(3) 0.033(4) C25 0.031(3) 0.054(4) 0.043(3) 0.004(3) -0.007(2) 0.011(3) C19 0.022(3) 0.055(4) 0.035(3) 0.004(3) 0.003(2) -0.006(3) C10 0.029(3) 0.071(6) 0.111(7) -0.063(6) 0.016(4) -0.007(4) C12 0.059(4) 0.043(4) 0.034(3) -0.015(3) 0.001(3) 0.003(3) C27 0.032(3) 0.064(5) 0.035(3) -0.006(3) 0.005(2) 0.002(3) Fe3 0.0208(3) 0.0187(4) 0.0207(3) 0.0001(3) -0.0047(2) -0.0002(3) Cu2 0.0135(2) 0.0170(3) 0.0263(3) 0.0046(2) -0.0072(2) -0.0018(2) Fe4 0.0580(6) 0.0426(6) 0.0289(4) 0.0015(4) 0.0000(4) -0.0139(5) Cl1 0.0183(5) 0.0304(7) 0.0283(6) -0.0002(5) -0.0042(4) -0.0016(5) S2 0.0438(8) 0.0424(9) 0.0301(7) -0.0044(6) -0.0006(6) -0.0053(7) N12 0.0173(18) 0.015(2) 0.026(2) 0.0009(15) -0.0060(14) 0.0016(15) O5 0.039(2) 0.037(3) 0.043(2) -0.0126(19) 0.0001(18) -0.0109(19) N16 0.0175(18) 0.017(2) 0.0244(19) -0.0008(15) -0.0069(14) -0.0023(15) N17 0.0143(18) 0.028(2) 0.029(2) -0.0023(17) -0.0015(15) -0.0005(16) N13 0.0156(17) 0.023(2) 0.0211(19) 0.0001(15) -0.0065(14) 0.0008(15) N15 0.0168(18) 0.014(2) 0.0230(19) -0.0010(14) -0.0053(14) 0.0020(15) N11 0.0146(17) 0.019(2) 0.0229(19) 0.0008(15) -0.0037(14) -0.0026(15) C42 0.019(2) 0.025(3) 0.026(2) 0.0010(19) -0.0061(18) 0.0013(19) C29 0.019(2) 0.024(3) 0.023(2) 0.0018(18) -0.0054(17) -0.0047(18) N14 0.0196(19) 0.034(3) 0.022(2) -0.0003(17) -0.0078(15) -0.0048(17) O3 0.0200(17) 0.038(2) 0.038(2) 0.0006(17) -0.0052(15) -0.0069(16) N10 0.026(2) 0.038(3) 0.034(2) -0.009(2) -0.0099(18) 0.008(2) C28 0.024(2) 0.029(3) 0.037(3) -0.004(2) 0.002(2) 0.001(2) O2 0.0230(18) 0.054(3) 0.0280(19) -0.0028(18) -0.0007(14) -0.0003(18) C30 0.020(2) 0.023(3) 0.027(2) -0.0004(19) -0.0067(18) 0.0036(18) C39 0.029(3) 0.021(3) 0.035(3) 0.002(2) -0.002(2) 0.008(2) N18 0.0125(18) 0.040(3) 0.035(2) -0.003(2) -0.0003(16) 0.0030(18) C32 0.023(2) 0.020(3) 0.025(2) -0.0004(18) -0.0053(18) 0.0044(19) C36 0.026(2) 0.031(3) 0.026(2) 0.000(2) -0.0008(19) 0.005(2) C37 0.022(2) 0.027(3) 0.033(3) 0.000(2) -0.0043(19) 0.002(2) C44 0.020(2) 0.042(4) 0.037(3) -0.008(2) 0.005(2) 0.005(2) C33 0.025(2) 0.014(3) 0.036(3) 0.0011(19) -0.007(2) 0.0031(19) C31 0.018(2) 0.029(3) 0.026(2) 0.000(2) -0.0043(18) 0.0013(19) C38 0.022(2) 0.026(3) 0.027(2) 0.0016(19) -0.0058(18) 0.005(2) O4 0.040(2) 0.054(3) 0.043(2) 0.017(2) 0.0002(19) 0.014(2) C46 0.032(3) 0.048(4) 0.031(3) -0.008(3) -0.004(2) 0.004(3) C34 0.034(3) 0.021(3) 0.032(3) -0.007(2) -0.009(2) 0.004(2) C45 0.031(3) 0.038(4) 0.029(3) -0.006(2) 0.003(2) 0.000(2) C41 0.028(3) 0.033(3) 0.024(2) 0.000(2) 0.0008(19) 0.005(2) C35 0.033(3) 0.032(3) 0.026(3) -0.004(2) -0.004(2) 0.010(2) C40 0.030(3) 0.023(3) 0.028(2) -0.0059(19) -0.007(2) 0.004(2) C54 0.049(4) 0.061(5) 0.034(3) -0.010(3) 0.002(3) -0.007(3) C53 0.113(8) 0.080(7) 0.038(4) -0.008(4) -0.023(5) -0.006(6) C51 0.088(8) 0.162(14) 0.074(7) -0.055(8) 0.040(6) -0.080(9) C50 0.049(4) 0.080(6) 0.056(4) -0.035(4) 0.006(3) -0.007(4) C49 0.064(5) 0.041(4) 0.047(4) -0.003(3) -0.002(3) -0.021(4) C47 0.060(5) 0.045(5) 0.064(5) -0.006(4) -0.024(4) 0.016(4) Cl2 0.0207(6) 0.0394(8) 0.0347(7) -0.0010(5) -0.0033(5) 0.0022(5) O8 0.0225(19) 0.058(3) 0.038(2) -0.001(2) 0.0019(16) 0.0034(19) O7 0.0230(19) 0.054(3) 0.044(2) -0.002(2) -0.0050(17) -0.0033(19) O6 0.043(3) 0.079(4) 0.063(3) -0.035(3) 0.009(2) -0.018(3) O9 0.074(4) 0.082(5) 0.071(4) 0.041(4) 0.006(3) 0.024(4) C9 0.034(3) 0.025(3) 0.037(3) -0.005(2) 0.002(2) -0.001(2) C48 0.095(7) 0.034(5) 0.067(5) 0.001(4) -0.023(5) 0.003(4) C52 0.219(17) 0.088(9) 0.029(4) 0.001(4) 0.021(7) -0.071(10) C62 0.038(4) 0.044(4) 0.063(5) -0.002(3) -0.004(3) 0.001(3) C55 0.049(4) 0.053(5) 0.067(5) 0.019(4) 0.002(4) -0.001(4) C60 0.038(3) 0.033(4) 0.067(5) 0.006(3) -0.008(3) -0.003(3) C59 0.041(4) 0.041(4) 0.066(5) -0.004(3) -0.002(3) -0.006(3) C61 0.036(3) 0.061(5) 0.061(5) -0.008(4) -0.008(3) -0.008(3) C57 0.078(6) 0.062(6) 0.054(5) 0.003(4) 0.028(4) 0.005(5) C56 0.077(6) 0.051(6) 0.085(6) 0.016(5) 0.028(5) 0.023(5) N20 0.045(3) 0.040(4) 0.088(5) -0.007(3) -0.019(3) 0.011(3) N19 0.046(4) 0.042(4) 0.095(5) 0.016(3) -0.032(4) -0.008(3) O1 0.034(2) 0.042(3) 0.036(2) 0.0056(18) 0.0038(17) 0.0037(19) C58 0.061(5) 0.063(5) 0.040(4) 0.011(3) -0.005(3) -0.017(4) C43 0.015(2) 0.024(3) 0.026(2) -0.0013(18) -0.0044(17) -0.0016(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N2 2.018(4) . ? Cu1 N3 2.026(4) 2_556 ? Cu1 N7 2.040(4) 2_556 ? Cu1 N6 2.049(4) . ? Cu1 N1 2.417(5) 2_556 ? Cu1 N1 2.429(5) . ? Fe1 C5 2.024(5) . ? Fe1 C14 2.027(7) . ? Fe1 C6 2.030(5) . ? Fe1 C9 2.038(6) . ? Fe1 C10 2.039(7) . ? Fe1 C13 2.039(7) . ? Fe1 C12 2.047(6) . ? Fe1 C11 2.049(7) . ? Fe1 C8 2.050(6) . ? Fe1 C7 2.052(6) . ? Fe2 C21 2.034(7) . ? Fe2 C19 2.036(6) . ? Fe2 C24 2.039(7) . ? Fe2 C22 2.040(6) . ? Fe2 C25 2.040(6) . ? Fe2 C26 2.042(6) . ? Fe2 C23 2.044(7) . ? Fe2 C27 2.047(6) . ? Fe2 C18 2.049(5) . ? Fe2 C20 2.055(6) . ? S1 C1 1.624(6) . ? N6 C15 1.313(6) . ? N6 N7 1.371(6) . ? N2 C3 1.305(7) . ? N2 N3 1.391(6) . ? N1 C1 1.166(7) . ? N1 Cu1 2.417(5) 2_546 ? N4 C3 1.342(7) . ? N4 C2 1.344(7) . ? N4 N5 1.408(6) . ? N8 C15 1.351(7) . ? N8 C16 1.354(7) . ? N8 N9 1.415(5) . ? C2 N3 1.310(6) . ? C2 H2 0.9500 . ? N5 C4 1.498(7) . ? C3 H3 0.9500 . ? N3 Cu1 2.026(4) 2_546 ? N7 C16 1.320(6) . ? N7 Cu1 2.040(4) 2_546 ? N9 C17 1.485(7) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C4 C5 1.489(7) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C18 C19 1.420(8) . ? C18 C22 1.423(9) . ? C18 C17 1.492(8) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C22 C21 1.428(8) . ? C22 H22 0.9500 . ? C24 C23 1.412(11) . ? C24 C25 1.420(10) . ? C24 H24 0.9500 . ? C7 C8 1.394(10) . ? C7 C6 1.437(9) . ? C7 H7 0.9500 . ? C5 C9 1.418(8) . ? C5 C6 1.436(7) . ? C13 C12 1.398(10) . ? C13 C14 1.408(10) . ? C13 H13 0.9500 . ? C8 C9 1.429(9) . ? C8 H8 0.9500 . ? C6 H6 0.9500 . ? C23 C27 1.410(11) . ? C23 H23 0.9500 . ? C20 C21 1.393(10) . ? C20 C19 1.409(9) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C26 C27 1.420(9) . ? C26 C25 1.431(10) . ? C26 H26 0.9500 . ? C11 C10 1.385(14) . ? C11 C12 1.412(11) . ? C11 H11 0.9500 . ? C14 C10 1.403(14) . ? C14 H14 0.9500 . ? C25 H25 0.9500 . ? C19 H19 0.9500 . ? C10 H10 0.9500 . ? C12 H12 0.9500 . ? C27 H27 0.9500 . ? Fe3 C39 2.031(6) . ? Fe3 C32 2.032(5) . ? Fe3 C38 2.035(5) . ? Fe3 C36 2.044(5) . ? Fe3 C34 2.044(6) . ? Fe3 C35 2.045(6) . ? Fe3 C40 2.047(5) . ? Fe3 C37 2.048(5) . ? Fe3 C41 2.055(5) . ? Fe3 C33 2.056(5) . ? Cu2 N16 2.017(4) 2_646 ? Cu2 N15 2.032(4) . ? Cu2 N11 2.038(4) . ? Cu2 N12 2.040(4) 2_646 ? Cu2 N10 2.265(5) . ? Cu2 N10 2.667(6) 2_646 ? Fe4 C45 2.017(6) . ? Fe4 C54 2.020(8) . ? Fe4 C52 2.030(8) . ? Fe4 C50 2.033(9) . ? Fe4 C51 2.033(11) . ? Fe4 C48 2.034(9) . ? Fe4 C53 2.037(8) . ? Fe4 C49 2.037(7) . ? Fe4 C46 2.044(6) . ? Fe4 C47 2.052(9) . ? Cl1 O4 1.432(5) . ? Cl1 O3 1.439(4) . ? Cl1 O5 1.445(5) . ? Cl1 O2 1.453(4) . ? S2 C28 1.628(6) . ? N12 C30 1.308(6) . ? N12 N11 1.377(6) . ? N12 Cu2 2.040(4) 2_656 ? N16 C43 1.314(6) . ? N16 N15 1.391(6) . ? N16 Cu2 2.017(4) 2_656 ? N17 C43 1.344(7) . ? N17 C42 1.354(7) . ? N17 N18 1.410(6) . ? N13 C29 1.351(6) . ? N13 C30 1.356(7) . ? N13 N14 1.403(5) . ? N15 C42 1.305(6) . ? N11 C29 1.318(6) . ? C42 H42 0.9500 . ? C29 H29 0.9500 . ? N14 C31 1.478(7) . ? N10 C28 1.156(7) . ? C30 H30 0.9500 . ? C39 C40 1.418(7) . ? C39 C38 1.420(8) . ? C39 H39 0.9500 . ? N18 C44 1.495(7) . ? C32 C36 1.428(7) . ? C32 C33 1.441(7) . ? C32 C31 1.488(7) . ? C36 C35 1.430(8) . ? C36 H36 0.9500 . ? C37 C38 1.423(8) . ? C37 C41 1.439(7) . ? C37 H37 0.9500 . ? C44 C45 1.473(8) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C33 C34 1.427(7) . ? C33 H33 0.9500 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C38 H38 0.9500 . ? C46 C47 1.424(10) . ? C46 C45 1.446(8) . ? C46 H46 0.9500 . ? C34 C35 1.412(9) . ? C34 H34 0.9500 . ? C45 C49 1.435(10) . ? C41 C40 1.416(8) . ? C41 H41 0.9500 . ? C35 H35 0.9500 . ? C40 H40 0.9500 . ? C54 C53 1.393(13) . ? C54 C50 1.394(11) . ? C54 H54 0.9500 . ? C53 C52 1.402(17) . ? C53 H53 0.9500 . ? C51 C50 1.401(16) . ? C51 C52 1.42(2) . ? C51 H51 0.9500 . ? C50 H50 0.9500 . ? C49 C48 1.442(12) . ? C49 H49 0.9500 . ? C47 C48 1.401(13) . ? C47 H47 0.9500 . ? Cl2 O9 1.417(6) . ? Cl2 O6 1.432(5) . ? Cl2 O7 1.435(4) . ? Cl2 O8 1.452(4) . ? C9 H9 0.9500 . ? C48 H48 0.9500 . ? C52 H52 0.9500 . ? C62 N20 1.157(9) . ? C62 C61 1.457(10) . ? C55 C56 1.472(11) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C60 N19 1.149(9) . ? C60 C59 1.474(10) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C57 O1 1.407(8) . ? C57 C58 1.481(12) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C56 O1 1.413(10) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C43 H43 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cu1 N3 176.21(18) . 2_556 ? N2 Cu1 N7 92.52(16) . 2_556 ? N3 Cu1 N7 88.57(16) 2_556 2_556 ? N2 Cu1 N6 87.86(16) . . ? N3 Cu1 N6 91.27(16) 2_556 . ? N7 Cu1 N6 176.62(18) 2_556 . ? N2 Cu1 N1 97.73(17) . 2_556 ? N3 Cu1 N1 85.99(17) 2_556 2_556 ? N7 Cu1 N1 84.39(17) 2_556 2_556 ? N6 Cu1 N1 92.24(17) . 2_556 ? N2 Cu1 N1 84.60(17) . . ? N3 Cu1 N1 91.64(17) 2_556 . ? N7 Cu1 N1 98.98(17) 2_556 . ? N6 Cu1 N1 84.40(17) . . ? N1 Cu1 N1 175.85(4) 2_556 . ? C5 Fe1 C14 108.8(3) . . ? C5 Fe1 C6 41.5(2) . . ? C14 Fe1 C6 113.0(3) . . ? C5 Fe1 C9 40.9(2) . . ? C14 Fe1 C9 134.7(3) . . ? C6 Fe1 C9 68.9(2) . . ? C5 Fe1 C10 112.1(3) . . ? C14 Fe1 C10 40.4(4) . . ? C6 Fe1 C10 142.7(4) . . ? C9 Fe1 C10 109.6(3) . . ? C5 Fe1 C13 135.0(3) . . ? C14 Fe1 C13 40.5(3) . . ? C6 Fe1 C13 110.0(3) . . ? C9 Fe1 C13 174.7(3) . . ? C10 Fe1 C13 68.0(3) . . ? C5 Fe1 C12 175.0(3) . . ? C14 Fe1 C12 67.5(3) . . ? C6 Fe1 C12 135.9(3) . . ? C9 Fe1 C12 144.2(3) . . ? C10 Fe1 C12 67.6(3) . . ? C13 Fe1 C12 40.0(3) . . ? C5 Fe1 C11 142.3(3) . . ? C14 Fe1 C11 67.0(4) . . ? C6 Fe1 C11 176.2(3) . . ? C9 Fe1 C11 114.0(3) . . ? C10 Fe1 C11 39.6(4) . . ? C13 Fe1 C11 67.4(3) . . ? C12 Fe1 C11 40.3(3) . . ? C5 Fe1 C8 68.9(3) . . ? C14 Fe1 C8 175.2(3) . . ? C6 Fe1 C8 68.4(3) . . ? C9 Fe1 C8 40.9(3) . . ? C10 Fe1 C8 135.9(4) . . ? C13 Fe1 C8 144.0(3) . . ? C12 Fe1 C8 115.0(3) . . ? C11 Fe1 C8 111.9(4) . . ? C5 Fe1 C7 69.3(2) . . ? C14 Fe1 C7 144.1(4) . . ? C6 Fe1 C7 41.2(2) . . ? C9 Fe1 C7 68.2(3) . . ? C10 Fe1 C7 175.2(4) . . ? C13 Fe1 C7 114.6(3) . . ? C12 Fe1 C7 111.4(3) . . ? C11 Fe1 C7 136.7(4) . . ? C8 Fe1 C7 39.7(3) . . ? C21 Fe2 C19 67.7(3) . . ? C21 Fe2 C24 159.0(3) . . ? C19 Fe2 C24 107.8(3) . . ? C21 Fe2 C22 41.0(2) . . ? C19 Fe2 C22 68.1(3) . . ? C24 Fe2 C22 158.4(3) . . ? C21 Fe2 C25 122.6(3) . . ? C19 Fe2 C25 121.5(3) . . ? C24 Fe2 C25 40.8(3) . . ? C22 Fe2 C25 159.8(3) . . ? C21 Fe2 C26 107.2(3) . . ? C19 Fe2 C26 157.2(3) . . ? C24 Fe2 C26 68.5(3) . . ? C22 Fe2 C26 123.6(3) . . ? C25 Fe2 C26 41.0(3) . . ? C21 Fe2 C23 158.8(3) . . ? C19 Fe2 C23 124.9(3) . . ? C24 Fe2 C23 40.5(3) . . ? C22 Fe2 C23 123.2(3) . . ? C25 Fe2 C23 68.1(3) . . ? C26 Fe2 C23 67.8(3) . . ? C21 Fe2 C27 122.5(3) . . ? C19 Fe2 C27 160.9(3) . . ? C24 Fe2 C27 68.6(3) . . ? C22 Fe2 C27 107.9(3) . . ? C25 Fe2 C27 68.9(3) . . ? C26 Fe2 C27 40.6(2) . . ? C23 Fe2 C27 40.3(3) . . ? C21 Fe2 C18 68.6(3) . . ? C19 Fe2 C18 40.7(2) . . ? C24 Fe2 C18 122.3(3) . . ? C22 Fe2 C18 40.7(3) . . ? C25 Fe2 C18 157.5(3) . . ? C26 Fe2 C18 160.4(3) . . ? C23 Fe2 C18 108.8(2) . . ? C27 Fe2 C18 124.2(2) . . ? C21 Fe2 C20 39.8(3) . . ? C19 Fe2 C20 40.3(3) . . ? C24 Fe2 C20 123.6(3) . . ? C22 Fe2 C20 68.0(3) . . ? C25 Fe2 C20 106.9(3) . . ? C26 Fe2 C20 121.7(3) . . ? C23 Fe2 C20 160.5(3) . . ? C27 Fe2 C20 157.4(3) . . ? C18 Fe2 C20 68.2(2) . . ? C15 N6 N7 107.7(4) . . ? C15 N6 Cu1 127.2(4) . . ? N7 N6 Cu1 125.1(3) . . ? C3 N2 N3 107.6(4) . . ? C3 N2 Cu1 130.0(4) . . ? N3 N2 Cu1 121.9(3) . . ? C1 N1 Cu1 137.7(5) . 2_546 ? C1 N1 Cu1 116.5(5) . . ? Cu1 N1 Cu1 95.61(16) 2_546 . ? C3 N4 C2 106.3(4) . . ? C3 N4 N5 129.7(5) . . ? C2 N4 N5 123.7(5) . . ? C15 N8 C16 106.9(4) . . ? C15 N8 N9 127.8(5) . . ? C16 N8 N9 125.3(4) . . ? N3 C2 N4 110.3(5) . . ? N3 C2 H2 124.8 . . ? N4 C2 H2 124.8 . . ? N4 N5 C4 110.1(4) . . ? N2 C3 N4 109.7(5) . . ? N2 C3 H3 125.1 . . ? N4 C3 H3 125.1 . . ? N1 C1 S1 176.2(6) . . ? C2 N3 N2 106.1(4) . . ? C2 N3 Cu1 130.3(4) . 2_546 ? N2 N3 Cu1 123.5(3) . 2_546 ? C16 N7 N6 107.8(4) . . ? C16 N7 Cu1 131.1(4) . 2_546 ? N6 N7 Cu1 120.2(3) . 2_546 ? N8 N9 C17 109.2(4) . . ? N6 C15 N8 109.1(5) . . ? N6 C15 H15 125.5 . . ? N8 C15 H15 125.5 . . ? N7 C16 N8 108.6(5) . . ? N7 C16 H16 125.7 . . ? N8 C16 H16 125.7 . . ? C5 C4 N5 111.8(5) . . ? C5 C4 H4A 109.3 . . ? N5 C4 H4A 109.3 . . ? C5 C4 H4B 109.3 . . ? N5 C4 H4B 109.3 . . ? H4A C4 H4B 107.9 . . ? C19 C18 C22 106.9(5) . . ? C19 C18 C17 125.9(6) . . ? C22 C18 C17 127.0(5) . . ? C19 C18 Fe2 69.2(3) . . ? C22 C18 Fe2 69.3(3) . . ? C17 C18 Fe2 130.6(4) . . ? N9 C17 C18 111.7(4) . . ? N9 C17 H17A 109.3 . . ? C18 C17 H17A 109.3 . . ? N9 C17 H17B 109.3 . . ? C18 C17 H17B 109.3 . . ? H17A C17 H17B 107.9 . . ? C18 C22 C21 107.6(6) . . ? C18 C22 Fe2 70.0(3) . . ? C21 C22 Fe2 69.3(4) . . ? C18 C22 H22 126.2 . . ? C21 C22 H22 126.2 . . ? Fe2 C22 H22 126.1 . . ? C23 C24 C25 107.7(7) . . ? C23 C24 Fe2 70.0(4) . . ? C25 C24 Fe2 69.7(4) . . ? C23 C24 H24 126.1 . . ? C25 C24 H24 126.1 . . ? Fe2 C24 H24 125.8 . . ? C8 C7 C6 108.2(5) . . ? C8 C7 Fe1 70.0(4) . . ? C6 C7 Fe1 68.6(3) . . ? C8 C7 H7 125.9 . . ? C6 C7 H7 125.9 . . ? Fe1 C7 H7 127.1 . . ? C9 C5 C6 107.4(5) . . ? C9 C5 C4 126.4(5) . . ? C6 C5 C4 126.0(6) . . ? C9 C5 Fe1 70.1(3) . . ? C6 C5 Fe1 69.5(3) . . ? C4 C5 Fe1 122.8(4) . . ? C12 C13 C14 107.6(7) . . ? C12 C13 Fe1 70.3(4) . . ? C14 C13 Fe1 69.3(4) . . ? C12 C13 H13 126.2 . . ? C14 C13 H13 126.2 . . ? Fe1 C13 H13 125.8 . . ? C7 C8 C9 108.7(6) . . ? C7 C8 Fe1 70.2(4) . . ? C9 C8 Fe1 69.1(3) . . ? C7 C8 H8 125.7 . . ? C9 C8 H8 125.7 . . ? Fe1 C8 H8 126.6 . . ? C5 C6 C7 107.5(5) . . ? C5 C6 Fe1 69.0(3) . . ? C7 C6 Fe1 70.2(3) . . ? C5 C6 H6 126.2 . . ? C7 C6 H6 126.2 . . ? Fe1 C6 H6 126.1 . . ? C27 C23 C24 109.3(6) . . ? C27 C23 Fe2 69.9(4) . . ? C24 C23 Fe2 69.6(4) . . ? C27 C23 H23 125.4 . . ? C24 C23 H23 125.4 . . ? Fe2 C23 H23 126.7 . . ? C21 C20 C19 108.1(6) . . ? C21 C20 Fe2 69.3(3) . . ? C19 C20 Fe2 69.1(3) . . ? C21 C20 H20 126.0 . . ? C19 C20 H20 126.0 . . ? Fe2 C20 H20 127.2 . . ? C20 C21 C22 108.5(6) . . ? C20 C21 Fe2 70.9(4) . . ? C22 C21 Fe2 69.7(4) . . ? C20 C21 H21 125.7 . . ? C22 C21 H21 125.7 . . ? Fe2 C21 H21 125.3 . . ? C27 C26 C25 108.3(6) . . ? C27 C26 Fe2 69.8(3) . . ? C25 C26 Fe2 69.4(3) . . ? C27 C26 H26 125.9 . . ? C25 C26 H26 125.9 . . ? Fe2 C26 H26 126.5 . . ? C10 C11 C12 108.7(8) . . ? C10 C11 Fe1 69.8(4) . . ? C12 C11 Fe1 69.8(4) . . ? C10 C11 H11 125.6 . . ? C12 C11 H11 125.6 . . ? Fe1 C11 H11 126.4 . . ? C10 C14 C13 108.4(7) . . ? C10 C14 Fe1 70.2(5) . . ? C13 C14 Fe1 70.2(4) . . ? C10 C14 H14 125.8 . . ? C13 C14 H14 125.8 . . ? Fe1 C14 H14 125.3 . . ? C24 C25 C26 107.4(6) . . ? C24 C25 Fe2 69.6(4) . . ? C26 C25 Fe2 69.6(4) . . ? C24 C25 H25 126.3 . . ? C26 C25 H25 126.3 . . ? Fe2 C25 H25 126.1 . . ? C20 C19 C18 108.9(6) . . ? C20 C19 Fe2 70.6(3) . . ? C18 C19 Fe2 70.2(3) . . ? C20 C19 H19 125.5 . . ? C18 C19 H19 125.5 . . ? Fe2 C19 H19 125.3 . . ? C11 C10 C14 107.6(7) . . ? C11 C10 Fe1 70.6(5) . . ? C14 C10 Fe1 69.4(4) . . ? C11 C10 H10 126.2 . . ? C14 C10 H10 126.2 . . ? Fe1 C10 H10 125.4 . . ? C13 C12 C11 107.6(7) . . ? C13 C12 Fe1 69.7(4) . . ? C11 C12 Fe1 69.9(4) . . ? C13 C12 H12 126.2 . . ? C11 C12 H12 126.2 . . ? Fe1 C12 H12 125.7 . . ? C23 C27 C26 107.3(7) . . ? C23 C27 Fe2 69.7(4) . . ? C26 C27 Fe2 69.5(3) . . ? C23 C27 H27 126.4 . . ? C26 C27 H27 126.4 . . ? Fe2 C27 H27 126.0 . . ? C39 Fe3 C32 127.2(2) . . ? C39 Fe3 C38 40.9(2) . . ? C32 Fe3 C38 164.5(2) . . ? C39 Fe3 C36 106.6(2) . . ? C32 Fe3 C36 41.0(2) . . ? C38 Fe3 C36 125.8(2) . . ? C39 Fe3 C34 151.3(2) . . ? C32 Fe3 C34 68.6(2) . . ? C38 Fe3 C34 117.7(2) . . ? C36 Fe3 C34 68.4(2) . . ? C39 Fe3 C35 117.2(2) . . ? C32 Fe3 C35 68.9(2) . . ? C38 Fe3 C35 106.1(2) . . ? C36 Fe3 C35 40.9(2) . . ? C34 Fe3 C35 40.4(2) . . ? C39 Fe3 C40 40.7(2) . . ? C32 Fe3 C40 108.4(2) . . ? C38 Fe3 C40 68.7(2) . . ? C36 Fe3 C40 118.4(2) . . ? C34 Fe3 C40 166.8(2) . . ? C35 Fe3 C40 151.8(2) . . ? C39 Fe3 C37 68.6(2) . . ? C32 Fe3 C37 153.7(2) . . ? C38 Fe3 C37 40.8(2) . . ? C36 Fe3 C37 164.0(2) . . ? C34 Fe3 C37 108.0(2) . . ? C35 Fe3 C37 126.4(2) . . ? C40 Fe3 C37 68.6(2) . . ? C39 Fe3 C41 68.3(2) . . ? C32 Fe3 C41 119.6(2) . . ? C38 Fe3 C41 68.7(2) . . ? C36 Fe3 C41 152.9(2) . . ? C34 Fe3 C41 128.9(2) . . ? C35 Fe3 C41 165.6(2) . . ? C40 Fe3 C41 40.4(2) . . ? C37 Fe3 C41 41.1(2) . . ? C39 Fe3 C33 166.2(2) . . ? C32 Fe3 C33 41.3(2) . . ? C38 Fe3 C33 152.2(2) . . ? C36 Fe3 C33 69.2(2) . . ? C34 Fe3 C33 40.7(2) . . ? C35 Fe3 C33 68.8(2) . . ? C40 Fe3 C33 128.7(2) . . ? C37 Fe3 C33 119.0(2) . . ? C41 Fe3 C33 109.1(2) . . ? N16 Cu2 N15 170.21(17) 2_646 . ? N16 Cu2 N11 92.89(16) 2_646 . ? N15 Cu2 N11 88.38(16) . . ? N16 Cu2 N12 87.20(16) 2_646 2_646 ? N15 Cu2 N12 90.89(16) . 2_646 ? N11 Cu2 N12 176.18(17) . 2_646 ? N16 Cu2 N10 100.90(18) 2_646 . ? N15 Cu2 N10 88.86(18) . . ? N11 Cu2 N10 87.36(17) . . ? N12 Cu2 N10 96.37(17) 2_646 . ? N16 Cu2 N10 82.95(16) 2_646 2_646 ? N15 Cu2 N10 87.28(16) . 2_646 ? N11 Cu2 N10 93.50(16) . 2_646 ? N12 Cu2 N10 82.72(15) 2_646 2_646 ? N10 Cu2 N10 176.02(11) . 2_646 ? C45 Fe4 C54 124.3(3) . . ? C45 Fe4 C52 156.0(5) . . ? C54 Fe4 C52 67.2(4) . . ? C45 Fe4 C50 106.1(3) . . ? C54 Fe4 C50 40.2(3) . . ? C52 Fe4 C50 68.2(5) . . ? C45 Fe4 C51 119.6(5) . . ? C54 Fe4 C51 67.4(4) . . ? C52 Fe4 C51 41.0(6) . . ? C50 Fe4 C51 40.3(5) . . ? C45 Fe4 C48 69.2(3) . . ? C54 Fe4 C48 154.7(4) . . ? C52 Fe4 C48 109.7(5) . . ? C50 Fe4 C48 164.3(4) . . ? C51 Fe4 C48 127.9(5) . . ? C45 Fe4 C53 161.3(4) . . ? C54 Fe4 C53 40.2(4) . . ? C52 Fe4 C53 40.3(5) . . ? C50 Fe4 C53 68.4(4) . . ? C51 Fe4 C53 68.5(5) . . ? C48 Fe4 C53 120.8(4) . . ? C45 Fe4 C49 41.4(3) . . ? C54 Fe4 C49 162.2(3) . . ? C52 Fe4 C49 121.6(4) . . ? C50 Fe4 C49 125.2(3) . . ? C51 Fe4 C49 108.1(4) . . ? C48 Fe4 C49 41.5(3) . . ? C53 Fe4 C49 156.2(4) . . ? C45 Fe4 C46 41.7(2) . . ? C54 Fe4 C46 106.8(3) . . ? C52 Fe4 C46 161.7(6) . . ? C50 Fe4 C46 119.2(3) . . ? C51 Fe4 C46 154.7(6) . . ? C48 Fe4 C46 67.9(3) . . ? C53 Fe4 C46 124.0(4) . . ? C49 Fe4 C46 69.5(3) . . ? C45 Fe4 C47 69.8(3) . . ? C54 Fe4 C47 119.7(3) . . ? C52 Fe4 C47 125.8(6) . . ? C50 Fe4 C47 153.9(4) . . ? C51 Fe4 C47 164.0(6) . . ? C48 Fe4 C47 40.1(4) . . ? C53 Fe4 C47 106.9(4) . . ? C49 Fe4 C47 69.5(3) . . ? C46 Fe4 C47 40.7(3) . . ? O4 Cl1 O3 110.0(3) . . ? O4 Cl1 O5 109.2(3) . . ? O3 Cl1 O5 108.9(3) . . ? O4 Cl1 O2 110.6(3) . . ? O3 Cl1 O2 109.1(2) . . ? O5 Cl1 O2 109.0(3) . . ? C30 N12 N11 107.8(4) . . ? C30 N12 Cu2 128.6(4) . 2_656 ? N11 N12 Cu2 123.6(3) . 2_656 ? C43 N16 N15 107.1(4) . . ? C43 N16 Cu2 130.9(4) . 2_656 ? N15 N16 Cu2 121.7(3) . 2_656 ? C43 N17 C42 106.9(4) . . ? C43 N17 N18 123.9(5) . . ? C42 N17 N18 128.7(5) . . ? C29 N13 C30 106.8(4) . . ? C29 N13 N14 123.3(4) . . ? C30 N13 N14 129.9(4) . . ? C42 N15 N16 107.4(4) . . ? C42 N15 Cu2 128.1(4) . . ? N16 N15 Cu2 124.6(3) . . ? C29 N11 N12 107.4(4) . . ? C29 N11 Cu2 129.6(4) . . ? N12 N11 Cu2 122.1(3) . . ? N15 C42 N17 109.3(5) . . ? N15 C42 H42 125.3 . . ? N17 C42 H42 125.3 . . ? N11 C29 N13 108.9(4) . . ? N11 C29 H29 125.5 . . ? N13 C29 H29 125.5 . . ? N13 N14 C31 111.2(4) . . ? C28 N10 Cu2 135.1(5) . . ? N10 C28 S2 176.9(5) . . ? N12 C30 N13 109.0(5) . . ? N12 C30 H30 125.5 . . ? N13 C30 H30 125.5 . . ? C40 C39 C38 108.5(5) . . ? C40 C39 Fe3 70.3(3) . . ? C38 C39 Fe3 69.7(3) . . ? C40 C39 H39 125.8 . . ? C38 C39 H39 125.8 . . ? Fe3 C39 H39 125.8 . . ? N17 N18 C44 109.3(4) . . ? C36 C32 C33 108.5(4) . . ? C36 C32 C31 125.8(5) . . ? C33 C32 C31 125.7(5) . . ? C36 C32 Fe3 69.9(3) . . ? C33 C32 Fe3 70.3(3) . . ? C31 C32 Fe3 127.4(4) . . ? C32 C36 C35 107.6(5) . . ? C32 C36 Fe3 69.0(3) . . ? C35 C36 Fe3 69.6(3) . . ? C32 C36 H36 126.2 . . ? C35 C36 H36 126.2 . . ? Fe3 C36 H36 126.7 . . ? C38 C37 C41 107.5(5) . . ? C38 C37 Fe3 69.1(3) . . ? C41 C37 Fe3 69.7(3) . . ? C38 C37 H37 126.3 . . ? C41 C37 H37 126.3 . . ? Fe3 C37 H37 126.4 . . ? C45 C44 N18 110.3(5) . . ? C45 C44 H44A 109.6 . . ? N18 C44 H44A 109.6 . . ? C45 C44 H44B 109.6 . . ? N18 C44 H44B 109.6 . . ? H44A C44 H44B 108.1 . . ? C34 C33 C32 106.5(5) . . ? C34 C33 Fe3 69.2(3) . . ? C32 C33 Fe3 68.5(3) . . ? C34 C33 H33 126.7 . . ? C32 C33 H33 126.7 . . ? Fe3 C33 H33 127.1 . . ? N14 C31 C32 108.5(4) . . ? N14 C31 H31A 110.0 . . ? C32 C31 H31A 110.0 . . ? N14 C31 H31B 110.0 . . ? C32 C31 H31B 110.0 . . ? H31A C31 H31B 108.4 . . ? C39 C38 C37 108.0(5) . . ? C39 C38 Fe3 69.4(3) . . ? C37 C38 Fe3 70.1(3) . . ? C39 C38 H38 126.0 . . ? C37 C38 H38 126.0 . . ? Fe3 C38 H38 126.1 . . ? C47 C46 C45 108.4(7) . . ? C47 C46 Fe4 70.0(4) . . ? C45 C46 Fe4 68.2(3) . . ? C47 C46 H46 125.8 . . ? C45 C46 H46 125.8 . . ? Fe4 C46 H46 127.6 . . ? C35 C34 C33 109.4(5) . . ? C35 C34 Fe3 69.8(3) . . ? C33 C34 Fe3 70.1(3) . . ? C35 C34 H34 125.3 . . ? C33 C34 H34 125.3 . . ? Fe3 C34 H34 126.4 . . ? C49 C45 C46 107.7(6) . . ? C49 C45 C44 126.1(6) . . ? C46 C45 C44 125.9(6) . . ? C49 C45 Fe4 70.0(4) . . ? C46 C45 Fe4 70.1(3) . . ? C44 C45 Fe4 130.3(4) . . ? C40 C41 C37 107.9(5) . . ? C40 C41 Fe3 69.5(3) . . ? C37 C41 Fe3 69.2(3) . . ? C40 C41 H41 126.0 . . ? C37 C41 H41 126.0 . . ? Fe3 C41 H41 126.8 . . ? C34 C35 C36 108.1(5) . . ? C34 C35 Fe3 69.8(3) . . ? C36 C35 Fe3 69.5(3) . . ? C34 C35 H35 126.0 . . ? C36 C35 H35 126.0 . . ? Fe3 C35 H35 126.3 . . ? C41 C40 C39 108.1(5) . . ? C41 C40 Fe3 70.1(3) . . ? C39 C40 Fe3 69.0(3) . . ? C41 C40 H40 126.0 . . ? C39 C40 H40 126.0 . . ? Fe3 C40 H40 126.4 . . ? C53 C54 C50 110.3(9) . . ? C53 C54 Fe4 70.6(5) . . ? C50 C54 Fe4 70.4(5) . . ? C53 C54 H54 124.8 . . ? C50 C54 H54 124.8 . . ? Fe4 C54 H54 125.8 . . ? C54 C53 C52 106.6(11) . . ? C54 C53 Fe4 69.3(4) . . ? C52 C53 Fe4 69.6(5) . . ? C54 C53 H53 126.7 . . ? C52 C53 H53 126.7 . . ? Fe4 C53 H53 126.0 . . ? C50 C51 C52 107.6(9) . . ? C50 C51 Fe4 69.8(5) . . ? C52 C51 Fe4 69.4(7) . . ? C50 C51 H51 126.2 . . ? C52 C51 H51 126.2 . . ? Fe4 C51 H51 126.1 . . ? C54 C50 C51 107.1(10) . . ? C54 C50 Fe4 69.4(5) . . ? C51 C50 Fe4 69.9(7) . . ? C54 C50 H50 126.4 . . ? C51 C50 H50 126.4 . . ? Fe4 C50 H50 125.9 . . ? C45 C49 C48 106.2(7) . . ? C45 C49 Fe4 68.5(4) . . ? C48 C49 Fe4 69.1(5) . . ? C45 C49 H49 126.9 . . ? C48 C49 H49 126.9 . . ? Fe4 C49 H49 127.0 . . ? C48 C47 C46 107.4(7) . . ? C48 C47 Fe4 69.3(5) . . ? C46 C47 Fe4 69.3(4) . . ? C48 C47 H47 126.3 . . ? C46 C47 H47 126.3 . . ? Fe4 C47 H47 126.7 . . ? O9 Cl2 O6 109.0(4) . . ? O9 Cl2 O7 109.7(4) . . ? O6 Cl2 O7 109.8(3) . . ? O9 Cl2 O8 109.2(3) . . ? O6 Cl2 O8 109.8(3) . . ? O7 Cl2 O8 109.3(3) . . ? C5 C9 C8 108.1(5) . . ? C5 C9 Fe1 69.1(3) . . ? C8 C9 Fe1 70.0(4) . . ? C5 C9 H9 125.9 . . ? C8 C9 H9 125.9 . . ? Fe1 C9 H9 126.6 . . ? C47 C48 C49 110.2(7) . . ? C47 C48 Fe4 70.6(5) . . ? C49 C48 Fe4 69.4(5) . . ? C47 C48 H48 124.9 . . ? C49 C48 H48 124.9 . . ? Fe4 C48 H48 126.7 . . ? C53 C52 C51 108.4(10) . . ? C53 C52 Fe4 70.1(5) . . ? C51 C52 Fe4 69.6(6) . . ? C53 C52 H52 125.8 . . ? C51 C52 H52 125.8 . . ? Fe4 C52 H52 126.1 . . ? N20 C62 C61 178.0(9) . . ? C56 C55 H55A 109.5 . . ? C56 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C56 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? N19 C60 C59 179.1(9) . . ? C60 C59 H59A 109.5 . . ? C60 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C60 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C62 C61 H61A 109.5 . . ? C62 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C62 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? O1 C57 C58 110.3(7) . . ? O1 C57 H57A 109.6 . . ? C58 C57 H57A 109.6 . . ? O1 C57 H57B 109.6 . . ? C58 C57 H57B 109.6 . . ? H57A C57 H57B 108.1 . . ? O1 C56 C55 111.2(7) . . ? O1 C56 H56A 109.4 . . ? C55 C56 H56A 109.4 . . ? O1 C56 H56B 109.4 . . ? C55 C56 H56B 109.4 . . ? H56A C56 H56B 108.0 . . ? C57 O1 C56 114.9(6) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? N16 C43 N17 109.4(5) . . ? N16 C43 H43 125.3 . . ? N17 C43 H43 125.3 . . ? _diffrn_measured_fraction_theta_max 0.922 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 1.967 _refine_diff_density_min -1.461 _refine_diff_density_rms 0.128 _database_code_depnum_ccdc_archive 'CCDC 922181'