# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_address ;Department of Inorganic and Physical Chemistry Indian Institute of Science Bangalore 560 012. INDIA ; _publ_contact_author_email arc@ipc.iisc.ernet.in _publ_contact_author_fax 91-080-23600683 _publ_contact_author_phone 91-080-22932533 _publ_contact_author_name 'Prof. A. R. Chakravarty' _publ_author_name A.Chakravarty data_arc _database_code_depnum_ccdc_archive 'CCDC 829878' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H45 Cl2 Co Fe2 N7 O9' _chemical_formula_sum 'C54 H45 Cl2 Co Fe2 N7 O9' _chemical_formula_weight 1177.50 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' Cl Cl 0.1484 0.1585 '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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M c2/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' '-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 20.8487(12) _cell_length_b 19.1791(11) _cell_length_c 12.9275(7) _cell_angle_alpha 90.00 _cell_angle_beta 96.567(3) _cell_angle_gamma 90.00 _cell_volume 5135.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.523 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2412 _exptl_absorpt_coefficient_mu 1.046 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8026 _exptl_absorpt_correction_T_max 0.8674 _exptl_absorpt_process_details SADABS(Sheldrick,1997) _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 Smart CCD Area Detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25803 _diffrn_reflns_av_R_equivalents 0.0776 _diffrn_reflns_av_sigmaI/netI 0.0945 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 28.00 _reflns_number_total 6212 _reflns_number_gt 2941 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Smart' _computing_data_reduction 'Bruker Saint' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.1129P)^2^+1.1584P] 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 6212 _refine_ls_number_parameters 345 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1615 _refine_ls_R_factor_gt 0.0676 _refine_ls_wR_factor_ref 0.2281 _refine_ls_wR_factor_gt 0.1793 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.5000 0.21323(5) 0.7500 0.0401(3) Uani 1 2 d S . . Fe2 Fe 0.31157(4) 0.23316(5) 0.20892(6) 0.0529(3) Uani 1 1 d . . . N1 N 0.4277(2) 0.1391(2) 0.7675(3) 0.0430(10) Uani 1 1 d . . . N2 N 0.4555(2) 0.2087(2) 0.6094(3) 0.0427(10) Uani 1 1 d . . . N3 N 0.5471(2) 0.2920(2) 0.6761(4) 0.0525(12) Uani 1 1 d . . . N4 N 0.5000 0.3682(6) 0.2500 0.097(3) Uani 1 2 d S . . O1 O 0.6923(4) 0.5275(4) 0.5530(5) 0.191(4) Uani 1 1 d . . . O2 O 0.6487(5) 0.5146(4) 0.3828(6) 0.201(5) Uani 1 1 d . . . O4 O 0.7256(7) 0.5905(10) 0.4327(8) 0.348(12) Uani 1 1 d . . . O3 O 0.6436(11) 0.5972(11) 0.4652(11) 0.408(15) Uani 1 1 d . . . O5 O 0.4860(8) 0.0313(9) 0.114(3) 0.276(17) Uani 0.50 1 d P . . C1 C 0.2860(4) 0.3111(4) 0.3024(7) 0.086(2) Uani 1 1 d . . . H1 H 0.3038 0.3197 0.3705 0.103 Uiso 1 1 calc R . . C2 C 0.3073(4) 0.3388(4) 0.2129(8) 0.092(3) Uani 1 1 d . . . H2 H 0.3419 0.3692 0.2109 0.110 Uiso 1 1 calc R . . C3 C 0.2674(4) 0.3130(4) 0.1258(7) 0.084(2) Uani 1 1 d . . . H3 H 0.2713 0.3229 0.0563 0.101 Uiso 1 1 calc R . . C4 C 0.2215(3) 0.2704(4) 0.1625(6) 0.078(2) Uani 1 1 d . . . H4 H 0.1886 0.2474 0.1214 0.094 Uiso 1 1 calc R . . C5 C 0.2326(3) 0.2675(4) 0.2717(6) 0.074(2) Uani 1 1 d . . . H5 H 0.2092 0.2417 0.3155 0.089 Uiso 1 1 calc R . . C6 C 0.4052(3) 0.2057(4) 0.2067(5) 0.0637(17) Uani 1 1 d . . . H6 H 0.4397 0.2365 0.2078 0.076 Uiso 1 1 calc R . . C7 C 0.3671(3) 0.1789(4) 0.1160(5) 0.0710(19) Uani 1 1 d . . . H7 H 0.3731 0.1888 0.0473 0.085 Uiso 1 1 calc R . . C8 C 0.3190(3) 0.1351(4) 0.1485(5) 0.0679(18) Uani 1 1 d . . . H8 H 0.2878 0.1115 0.1047 0.081 Uiso 1 1 calc R . . C9 C 0.3259(3) 0.1329(3) 0.2579(4) 0.0594(15) Uani 1 1 d . . . H9 H 0.3000 0.1078 0.2987 0.071 Uiso 1 1 calc R . . C10 C 0.3798(3) 0.1759(3) 0.2957(4) 0.0502(14) Uani 1 1 d . . . C11 C 0.4044(3) 0.1892(3) 0.4039(4) 0.0473(13) Uani 1 1 d . . . C12 C 0.3822(3) 0.1511(3) 0.4841(4) 0.0484(13) Uani 1 1 d . . . H12 H 0.3497 0.1181 0.4690 0.058 Uiso 1 1 calc R . . C13 C 0.4080(2) 0.1618(3) 0.5863(4) 0.0430(12) Uani 1 1 d . . . C14 C 0.3900(2) 0.1241(3) 0.6776(4) 0.0403(11) Uani 1 1 d . . . C15 C 0.3372(3) 0.0803(3) 0.6754(5) 0.0543(14) Uani 1 1 d . . . H15 H 0.3114 0.0716 0.6131 0.065 Uiso 1 1 calc R . . C16 C 0.3232(3) 0.0497(3) 0.7655(6) 0.0635(17) Uani 1 1 d . . . H16 H 0.2881 0.0198 0.7650 0.076 Uiso 1 1 calc R . . C17 C 0.3611(3) 0.0634(3) 0.8564(5) 0.0649(18) Uani 1 1 d . . . H17 H 0.3518 0.0433 0.9183 0.078 Uiso 1 1 calc R . . C18 C 0.4139(3) 0.1079(3) 0.8555(5) 0.0577(15) Uani 1 1 d . . . H18 H 0.4402 0.1162 0.9173 0.069 Uiso 1 1 calc R . . C19 C 0.4519(3) 0.2386(3) 0.4316(4) 0.0521(14) Uani 1 1 d . . . H19 H 0.4669 0.2662 0.3804 0.063 Uiso 1 1 calc R . . C20 C 0.4769(3) 0.2471(3) 0.5341(4) 0.0469(13) Uani 1 1 d . . . C21 C 0.5289(3) 0.2964(3) 0.5730(4) 0.0582(15) Uani 1 1 d . . . C22 C 0.5553(4) 0.3434(4) 0.5126(6) 0.101(3) Uani 1 1 d . . . H22 H 0.5408 0.3461 0.4419 0.122 Uiso 1 1 calc R . . C23 C 0.6036(5) 0.3874(5) 0.5552(7) 0.127(4) Uani 1 1 d . . . H23 H 0.6243 0.4175 0.5135 0.153 Uiso 1 1 calc R . . C24 C 0.6202(5) 0.3854(5) 0.6620(7) 0.116(3) Uani 1 1 d . . . H24 H 0.6503 0.4164 0.6945 0.140 Uiso 1 1 calc R . . C25 C 0.5913(3) 0.3367(4) 0.7185(5) 0.0714(19) Uani 1 1 d . . . H25 H 0.6032 0.3347 0.7900 0.086 Uiso 1 1 calc R . . Cl1 Cl 0.68260(10) 0.55288(11) 0.45620(14) 0.0771(5) Uani 1 1 d . . . C26 C 0.5000 0.4222(7) 0.2500 0.123(5) Uani 1 2 d S . . C27 C 0.5215(10) 0.4976(10) 0.201(2) 0.333(18) Uani 1 1 d . . . C28 C 0.5000 0.0417(8) 0.2500 0.158(10) Uani 1 2 d S . . 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 Co1 0.0444(6) 0.0443(6) 0.0311(5) 0.000 0.0025(4) 0.000 Fe2 0.0547(5) 0.0596(6) 0.0422(5) -0.0023(4) -0.0031(4) 0.0137(4) N1 0.048(2) 0.047(3) 0.035(2) 0.004(2) 0.0073(19) 0.000(2) N2 0.049(2) 0.041(2) 0.038(2) 0.003(2) 0.0008(19) 0.001(2) N3 0.057(3) 0.055(3) 0.046(3) -0.007(2) 0.006(2) -0.007(2) N4 0.145(9) 0.078(7) 0.067(6) 0.000 0.007(6) 0.000 O1 0.268(10) 0.171(7) 0.110(5) 0.061(5) -0.079(6) -0.126(7) O2 0.308(11) 0.154(7) 0.113(6) 0.011(5) -0.099(6) -0.092(8) O4 0.295(14) 0.60(3) 0.146(8) 0.041(12) 0.006(9) -0.337(19) O3 0.54(3) 0.45(2) 0.204(13) -0.150(15) -0.126(17) 0.32(2) O5 0.078(10) 0.128(15) 0.62(5) 0.15(2) 0.02(2) 0.041(9) C1 0.089(6) 0.086(5) 0.079(5) -0.033(5) -0.010(4) 0.033(5) C2 0.075(5) 0.057(5) 0.139(8) 0.000(5) -0.006(5) 0.015(4) C3 0.080(5) 0.085(5) 0.084(5) 0.031(5) -0.004(4) 0.028(4) C4 0.063(4) 0.090(6) 0.077(5) 0.000(4) -0.013(4) 0.030(4) C5 0.068(4) 0.083(5) 0.072(5) -0.003(4) 0.015(4) 0.024(4) C6 0.061(4) 0.084(5) 0.045(3) -0.003(3) 0.000(3) 0.020(3) C7 0.085(5) 0.089(5) 0.038(3) -0.008(3) 0.001(3) 0.035(4) C8 0.080(5) 0.068(4) 0.051(4) -0.015(3) -0.015(3) 0.018(4) C9 0.076(4) 0.052(4) 0.047(3) -0.003(3) -0.009(3) 0.006(3) C10 0.061(3) 0.050(3) 0.038(3) -0.003(3) 0.003(3) 0.017(3) C11 0.053(3) 0.048(3) 0.039(3) -0.001(3) -0.001(2) 0.014(3) C12 0.048(3) 0.049(3) 0.046(3) -0.004(3) -0.005(2) -0.003(3) C13 0.044(3) 0.043(3) 0.041(3) 0.001(2) 0.001(2) 0.001(2) C14 0.042(3) 0.035(3) 0.043(3) 0.003(2) 0.005(2) 0.002(2) C15 0.052(3) 0.049(3) 0.063(4) 0.006(3) 0.009(3) 0.001(3) C16 0.062(4) 0.049(4) 0.082(5) 0.012(3) 0.018(4) -0.005(3) C17 0.073(4) 0.064(4) 0.064(4) 0.016(3) 0.035(4) 0.005(3) C18 0.062(4) 0.066(4) 0.047(3) 0.006(3) 0.012(3) 0.009(3) C19 0.065(4) 0.056(3) 0.035(3) 0.006(3) 0.004(3) 0.001(3) C20 0.052(3) 0.047(3) 0.041(3) 0.005(3) 0.005(2) -0.003(3) C21 0.077(4) 0.056(4) 0.041(3) 0.003(3) 0.006(3) -0.021(3) C22 0.162(8) 0.080(5) 0.059(4) 0.006(4) -0.001(5) -0.062(5) C23 0.194(10) 0.111(7) 0.076(6) 0.013(5) 0.012(6) -0.100(7) C24 0.144(8) 0.112(7) 0.093(6) -0.023(6) 0.016(6) -0.084(6) C25 0.079(4) 0.073(5) 0.061(4) -0.019(4) 0.001(3) -0.027(4) Cl1 0.0902(13) 0.0757(12) 0.0629(11) 0.0059(9) -0.0021(9) -0.0235(10) C26 0.113(10) 0.053(7) 0.192(16) 0.000 -0.033(10) 0.000 C27 0.23(3) 0.224(18) 0.54(6) 0.17(3) 0.01(2) -0.001(17) C28 0.087(12) 0.050(7) 0.35(3) 0.000 0.070(19) 0.000 _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Co1 N2 1.945(4) . ? Co1 N2 1.945(4) 2_656 ? Co1 N3 2.092(5) 2_656 ? Co1 N3 2.092(5) . ? Co1 N1 2.104(4) . ? Co1 N1 2.104(4) 2_656 ? Fe2 C6 2.025(6) . ? Fe2 C5 2.028(6) . ? Fe2 C2 2.029(7) . ? Fe2 C10 2.031(5) . ? Fe2 C3 2.030(7) . ? Fe2 C1 2.031(7) . ? Fe2 C4 2.035(6) . ? Fe2 C9 2.036(6) . ? Fe2 C7 2.045(6) . ? Fe2 C8 2.048(6) . ? N1 C18 1.345(7) . ? N1 C14 1.358(6) . ? N2 C20 1.336(6) . ? N2 C13 1.347(6) . ? N3 C25 1.330(7) . ? N3 C21 1.345(7) . ? N4 C26 1.036(13) . ? O1 Cl1 1.336(6) . ? O2 Cl1 1.336(6) . ? O4 Cl1 1.216(8) . ? O4 O3 1.81(2) . ? O3 Cl1 1.191(13) . ? O5 C28 1.76(3) . ? C1 C2 1.391(11) . ? C1 C5 1.414(11) . ? C1 H1 0.9300 . ? C2 C3 1.411(11) . ? C2 H2 0.9300 . ? C3 C4 1.383(10) . ? C3 H3 0.9300 . ? C4 C5 1.406(10) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.435(9) . ? C6 C10 1.439(8) . ? C6 H6 0.9300 . ? C7 C8 1.408(10) . ? C7 H7 0.9300 . ? C8 C9 1.405(8) . ? C8 H8 0.9300 . ? C9 C10 1.434(8) . ? C9 H9 0.9300 . ? C10 C11 1.456(7) . ? C11 C19 1.386(8) . ? C11 C12 1.392(8) . ? C12 C13 1.383(7) . ? C12 H12 0.9300 . ? C13 C14 1.469(7) . ? C14 C15 1.383(7) . ? C15 C16 1.364(8) . ? C15 H15 0.9300 . ? C16 C17 1.364(9) . ? C16 H16 0.9300 . ? C17 C18 1.392(8) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.378(7) . ? C19 H19 0.9300 . ? C20 C21 1.482(8) . ? C21 C22 1.351(9) . ? C22 C23 1.379(10) . ? C22 H22 0.9300 . ? C23 C24 1.385(11) . ? C23 H23 0.9300 . ? C24 C25 1.366(10) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C27 1.659(19) . ? C26 C27 1.659(19) 2_655 ? C27 C27 1.63(5) 2_655 ? C28 O5 1.76(3) 2_655 ? 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 Co1 N2 174.9(2) . 2_656 ? N2 Co1 N3 105.09(18) . 2_656 ? N2 Co1 N3 78.68(18) 2_656 2_656 ? N2 Co1 N3 78.68(18) . . ? N2 Co1 N3 105.09(18) 2_656 . ? N3 Co1 N3 87.5(3) 2_656 . ? N2 Co1 N1 78.47(17) . . ? N2 Co1 N1 98.05(17) 2_656 . ? N3 Co1 N1 93.42(17) 2_656 . ? N3 Co1 N1 156.55(17) . . ? N2 Co1 N1 98.05(17) . 2_656 ? N2 Co1 N1 78.47(17) 2_656 2_656 ? N3 Co1 N1 156.55(17) 2_656 2_656 ? N3 Co1 N1 93.42(17) . 2_656 ? N1 Co1 N1 94.9(2) . 2_656 ? C6 Fe2 C5 156.7(3) . . ? C6 Fe2 C2 107.8(3) . . ? C5 Fe2 C2 68.0(3) . . ? C6 Fe2 C10 41.6(2) . . ? C5 Fe2 C10 120.3(3) . . ? C2 Fe2 C10 123.8(3) . . ? C6 Fe2 C3 124.6(3) . . ? C5 Fe2 C3 68.1(3) . . ? C2 Fe2 C3 40.7(3) . . ? C10 Fe2 C3 161.3(3) . . ? C6 Fe2 C1 121.2(3) . . ? C5 Fe2 C1 40.8(3) . . ? C2 Fe2 C1 40.1(3) . . ? C10 Fe2 C1 106.5(3) . . ? C3 Fe2 C1 68.1(3) . . ? C6 Fe2 C4 161.0(3) . . ? C5 Fe2 C4 40.5(3) . . ? C2 Fe2 C4 67.4(3) . . ? C10 Fe2 C4 156.6(3) . . ? C3 Fe2 C4 39.8(3) . . ? C1 Fe2 C4 67.7(3) . . ? C6 Fe2 C9 69.6(3) . . ? C5 Fe2 C9 106.2(3) . . ? C2 Fe2 C9 160.1(3) . . ? C10 Fe2 C9 41.3(2) . . ? C3 Fe2 C9 156.7(3) . . ? C1 Fe2 C9 123.3(3) . . ? C4 Fe2 C9 121.4(3) . . ? C6 Fe2 C7 41.3(2) . . ? C5 Fe2 C7 160.1(3) . . ? C2 Fe2 C7 123.5(4) . . ? C10 Fe2 C7 69.0(2) . . ? C3 Fe2 C7 109.0(3) . . ? C1 Fe2 C7 158.2(4) . . ? C4 Fe2 C7 124.8(3) . . ? C9 Fe2 C7 68.3(3) . . ? C6 Fe2 C8 68.9(3) . . ? C5 Fe2 C8 123.5(3) . . ? C2 Fe2 C8 158.7(4) . . ? C10 Fe2 C8 68.6(2) . . ? C3 Fe2 C8 122.7(3) . . ? C1 Fe2 C8 159.8(4) . . ? C4 Fe2 C8 108.5(3) . . ? C9 Fe2 C8 40.3(2) . . ? C7 Fe2 C8 40.2(3) . . ? C18 N1 C14 118.1(5) . . ? C18 N1 Co1 128.1(4) . . ? C14 N1 Co1 113.7(3) . . ? C20 N2 C13 120.3(5) . . ? C20 N2 Co1 119.6(4) . . ? C13 N2 Co1 119.8(3) . . ? C25 N3 C21 118.2(5) . . ? C25 N3 Co1 128.0(4) . . ? C21 N3 Co1 113.8(4) . . ? Cl1 O4 O3 40.7(7) . . ? Cl1 O3 O4 41.8(8) . . ? C2 C1 C5 108.0(7) . . ? C2 C1 Fe2 69.9(4) . . ? C5 C1 Fe2 69.5(4) . . ? C2 C1 H1 126.0 . . ? C5 C1 H1 126.0 . . ? Fe2 C1 H1 126.2 . . ? C1 C2 C3 108.4(7) . . ? C1 C2 Fe2 70.1(4) . . ? C3 C2 Fe2 69.7(4) . . ? C1 C2 H2 125.8 . . ? C3 C2 H2 125.8 . . ? Fe2 C2 H2 126.0 . . ? C4 C3 C2 107.5(8) . . ? C4 C3 Fe2 70.3(4) . . ? C2 C3 Fe2 69.6(4) . . ? C4 C3 H3 126.2 . . ? C2 C3 H3 126.2 . . ? Fe2 C3 H3 125.5 . . ? C3 C4 C5 109.1(7) . . ? C3 C4 Fe2 69.9(4) . . ? C5 C4 Fe2 69.5(4) . . ? C3 C4 H4 125.4 . . ? C5 C4 H4 125.4 . . ? Fe2 C4 H4 126.7 . . ? C4 C5 C1 107.0(7) . . ? C4 C5 Fe2 70.0(4) . . ? C1 C5 Fe2 69.8(4) . . ? C4 C5 H5 126.5 . . ? C1 C5 H5 126.5 . . ? Fe2 C5 H5 125.3 . . ? C7 C6 C10 107.0(6) . . ? C7 C6 Fe2 70.1(4) . . ? C10 C6 Fe2 69.4(3) . . ? C7 C6 H6 126.5 . . ? C10 C6 H6 126.5 . . ? Fe2 C6 H6 125.5 . . ? C8 C7 C6 108.4(6) . . ? C8 C7 Fe2 70.0(4) . . ? C6 C7 Fe2 68.6(3) . . ? C8 C7 H7 125.8 . . ? C6 C7 H7 125.8 . . ? Fe2 C7 H7 127.2 . . ? C9 C8 C7 109.0(6) . . ? C9 C8 Fe2 69.4(3) . . ? C7 C8 Fe2 69.8(4) . . ? C9 C8 H8 125.5 . . ? C7 C8 H8 125.5 . . ? Fe2 C8 H8 126.9 . . ? C8 C9 C10 108.1(6) . . ? C8 C9 Fe2 70.3(4) . . ? C10 C9 Fe2 69.1(3) . . ? C8 C9 H9 125.9 . . ? C10 C9 H9 125.9 . . ? Fe2 C9 H9 126.2 . . ? C9 C10 C6 107.6(5) . . ? C9 C10 C11 127.2(5) . . ? C6 C10 C11 125.2(6) . . ? C9 C10 Fe2 69.6(3) . . ? C6 C10 Fe2 69.0(3) . . ? C11 C10 Fe2 125.7(4) . . ? C19 C11 C12 117.1(5) . . ? C19 C11 C10 122.0(5) . . ? C12 C11 C10 120.8(5) . . ? C13 C12 C11 120.4(5) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? N2 C13 C12 120.5(5) . . ? N2 C13 C14 113.5(4) . . ? C12 C13 C14 125.9(5) . . ? N1 C14 C15 121.8(5) . . ? N1 C14 C13 114.1(4) . . ? C15 C14 C13 124.0(5) . . ? C16 C15 C14 119.4(6) . . ? C16 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? C17 C16 C15 119.6(6) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C16 C17 C18 119.4(6) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? N1 C18 C17 121.7(6) . . ? N1 C18 H18 119.2 . . ? C17 C18 H18 119.2 . . ? C20 C19 C11 120.6(5) . . ? C20 C19 H19 119.7 . . ? C11 C19 H19 119.7 . . ? N2 C20 C19 121.0(5) . . ? N2 C20 C21 113.3(5) . . ? C19 C20 C21 125.7(5) . . ? N3 C21 C22 121.8(6) . . ? N3 C21 C20 114.2(5) . . ? C22 C21 C20 124.0(6) . . ? C21 C22 C23 120.3(7) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C22 C23 C24 118.0(7) . . ? C22 C23 H23 121.0 . . ? C24 C23 H23 121.0 . . ? C25 C24 C23 118.5(7) . . ? C25 C24 H24 120.8 . . ? C23 C24 H24 120.8 . . ? N3 C25 C24 123.1(7) . . ? N3 C25 H25 118.5 . . ? C24 C25 H25 118.5 . . ? O3 Cl1 O4 97.6(14) . . ? O3 Cl1 O1 101.5(9) . . ? O4 Cl1 O1 114.4(7) . . ? O3 Cl1 O2 98.6(10) . . ? O4 Cl1 O2 119.6(7) . . ? O1 Cl1 O2 118.4(5) . . ? N4 C26 C27 150.6(9) . . ? N4 C26 C27 150.6(9) . 2_655 ? C27 C26 C27 58.9(18) . 2_655 ? C27 C27 C26 60.6(9) 2_655 . ? O5 C28 O5 166.9(17) . 2_655 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Co1 N1 C18 -175.4(5) . . . . ? N2 Co1 N1 C18 8.3(5) 2_656 . . . ? N3 Co1 N1 C18 -70.7(5) 2_656 . . . ? N3 Co1 N1 C18 -162.3(5) . . . . ? N1 Co1 N1 C18 87.3(5) 2_656 . . . ? N2 Co1 N1 C14 2.0(3) . . . . ? N2 Co1 N1 C14 -174.2(3) 2_656 . . . ? N3 Co1 N1 C14 106.7(3) 2_656 . . . ? N3 Co1 N1 C14 15.1(6) . . . . ? N1 Co1 N1 C14 -95.2(3) 2_656 . . . ? N2 Co1 N2 C20 -131.1(4) 2_656 . . . ? N3 Co1 N2 C20 91.4(4) 2_656 . . . ? N3 Co1 N2 C20 7.1(4) . . . . ? N1 Co1 N2 C20 -178.2(4) . . . . ? N1 Co1 N2 C20 -84.8(4) 2_656 . . . ? N2 Co1 N2 C13 41.8(4) 2_656 . . . ? N3 Co1 N2 C13 -95.7(4) 2_656 . . . ? N3 Co1 N2 C13 -179.9(4) . . . . ? N1 Co1 N2 C13 -5.2(4) . . . . ? N1 Co1 N2 C13 88.2(4) 2_656 . . . ? N2 Co1 N3 C25 174.5(6) . . . . ? N2 Co1 N3 C25 -9.0(6) 2_656 . . . ? N3 Co1 N3 C25 68.6(5) 2_656 . . . ? N1 Co1 N3 C25 161.4(5) . . . . ? N1 Co1 N3 C25 -87.9(5) 2_656 . . . ? N2 Co1 N3 C21 -5.3(4) . . . . ? N2 Co1 N3 C21 171.2(4) 2_656 . . . ? N3 Co1 N3 C21 -111.2(5) 2_656 . . . ? N1 Co1 N3 C21 -18.4(7) . . . . ? N1 Co1 N3 C21 92.2(4) 2_656 . . . ? C6 Fe2 C1 C2 80.4(5) . . . . ? C5 Fe2 C1 C2 -119.2(7) . . . . ? C10 Fe2 C1 C2 123.3(5) . . . . ? C3 Fe2 C1 C2 -37.7(5) . . . . ? C4 Fe2 C1 C2 -80.8(5) . . . . ? C9 Fe2 C1 C2 165.3(4) . . . . ? C7 Fe2 C1 C2 48.6(10) . . . . ? C8 Fe2 C1 C2 -164.0(7) . . . . ? C6 Fe2 C1 C5 -160.4(4) . . . . ? C2 Fe2 C1 C5 119.2(7) . . . . ? C10 Fe2 C1 C5 -117.5(5) . . . . ? C3 Fe2 C1 C5 81.5(5) . . . . ? C4 Fe2 C1 C5 38.4(5) . . . . ? C9 Fe2 C1 C5 -75.5(5) . . . . ? C7 Fe2 C1 C5 167.9(7) . . . . ? C8 Fe2 C1 C5 -44.8(10) . . . . ? C5 C1 C2 C3 0.1(8) . . . . ? Fe2 C1 C2 C3 59.4(5) . . . . ? C5 C1 C2 Fe2 -59.2(5) . . . . ? C6 Fe2 C2 C1 -117.7(5) . . . . ? C5 Fe2 C2 C1 37.9(5) . . . . ? C10 Fe2 C2 C1 -74.7(5) . . . . ? C3 Fe2 C2 C1 119.5(7) . . . . ? C4 Fe2 C2 C1 81.9(5) . . . . ? C9 Fe2 C2 C1 -38.7(11) . . . . ? C7 Fe2 C2 C1 -160.4(4) . . . . ? C8 Fe2 C2 C1 164.8(7) . . . . ? C6 Fe2 C2 C3 122.8(5) . . . . ? C5 Fe2 C2 C3 -81.5(5) . . . . ? C10 Fe2 C2 C3 165.9(4) . . . . ? C1 Fe2 C2 C3 -119.5(7) . . . . ? C4 Fe2 C2 C3 -37.6(5) . . . . ? C9 Fe2 C2 C3 -158.2(8) . . . . ? C7 Fe2 C2 C3 80.1(5) . . . . ? C8 Fe2 C2 C3 45.4(10) . . . . ? C1 C2 C3 C4 0.7(8) . . . . ? Fe2 C2 C3 C4 60.3(5) . . . . ? C1 C2 C3 Fe2 -59.6(5) . . . . ? C6 Fe2 C3 C4 165.2(4) . . . . ? C5 Fe2 C3 C4 -37.0(5) . . . . ? C2 Fe2 C3 C4 -118.3(7) . . . . ? C10 Fe2 C3 C4 -157.5(7) . . . . ? C1 Fe2 C3 C4 -81.1(5) . . . . ? C9 Fe2 C3 C4 43.0(10) . . . . ? C7 Fe2 C3 C4 122.0(5) . . . . ? C8 Fe2 C3 C4 79.6(6) . . . . ? C6 Fe2 C3 C2 -76.5(6) . . . . ? C5 Fe2 C3 C2 81.3(5) . . . . ? C10 Fe2 C3 C2 -39.2(11) . . . . ? C1 Fe2 C3 C2 37.2(5) . . . . ? C4 Fe2 C3 C2 118.3(7) . . . . ? C9 Fe2 C3 C2 161.4(7) . . . . ? C7 Fe2 C3 C2 -119.7(5) . . . . ? C8 Fe2 C3 C2 -162.1(5) . . . . ? C2 C3 C4 C5 -1.4(8) . . . . ? Fe2 C3 C4 C5 58.6(5) . . . . ? C2 C3 C4 Fe2 -59.9(5) . . . . ? C6 Fe2 C4 C3 -40.2(12) . . . . ? C5 Fe2 C4 C3 120.6(7) . . . . ? C2 Fe2 C4 C3 38.5(5) . . . . ? C10 Fe2 C4 C3 162.0(6) . . . . ? C1 Fe2 C4 C3 82.0(6) . . . . ? C9 Fe2 C4 C3 -161.6(5) . . . . ? C7 Fe2 C4 C3 -77.6(6) . . . . ? C8 Fe2 C4 C3 -119.2(5) . . . . ? C6 Fe2 C4 C5 -160.8(8) . . . . ? C2 Fe2 C4 C5 -82.2(5) . . . . ? C10 Fe2 C4 C5 41.4(9) . . . . ? C3 Fe2 C4 C5 -120.6(7) . . . . ? C1 Fe2 C4 C5 -38.6(5) . . . . ? C9 Fe2 C4 C5 77.8(5) . . . . ? C7 Fe2 C4 C5 161.8(5) . . . . ? C8 Fe2 C4 C5 120.2(5) . . . . ? C3 C4 C5 C1 1.4(8) . . . . ? Fe2 C4 C5 C1 60.3(5) . . . . ? C3 C4 C5 Fe2 -58.8(5) . . . . ? C2 C1 C5 C4 -1.0(8) . . . . ? Fe2 C1 C5 C4 -60.4(5) . . . . ? C2 C1 C5 Fe2 59.5(5) . . . . ? C6 Fe2 C5 C4 164.3(7) . . . . ? C2 Fe2 C5 C4 80.4(5) . . . . ? C10 Fe2 C5 C4 -162.3(4) . . . . ? C3 Fe2 C5 C4 36.4(5) . . . . ? C1 Fe2 C5 C4 117.7(7) . . . . ? C9 Fe2 C5 C4 -119.7(5) . . . . ? C7 Fe2 C5 C4 -49.0(11) . . . . ? C8 Fe2 C5 C4 -79.2(5) . . . . ? C6 Fe2 C5 C1 46.6(10) . . . . ? C2 Fe2 C5 C1 -37.3(5) . . . . ? C10 Fe2 C5 C1 80.0(5) . . . . ? C3 Fe2 C5 C1 -81.3(5) . . . . ? C4 Fe2 C5 C1 -117.7(7) . . . . ? C9 Fe2 C5 C1 122.6(5) . . . . ? C7 Fe2 C5 C1 -166.7(8) . . . . ? C8 Fe2 C5 C1 163.1(5) . . . . ? C5 Fe2 C6 C7 163.6(7) . . . . ? C2 Fe2 C6 C7 -120.9(5) . . . . ? C10 Fe2 C6 C7 117.8(6) . . . . ? C3 Fe2 C6 C7 -79.2(5) . . . . ? C1 Fe2 C6 C7 -162.7(5) . . . . ? C4 Fe2 C6 C7 -49.1(11) . . . . ? C9 Fe2 C6 C7 79.9(4) . . . . ? C8 Fe2 C6 C7 36.7(4) . . . . ? C5 Fe2 C6 C10 45.7(9) . . . . ? C2 Fe2 C6 C10 121.2(4) . . . . ? C3 Fe2 C6 C10 163.0(4) . . . . ? C1 Fe2 C6 C10 79.4(5) . . . . ? C4 Fe2 C6 C10 -166.9(8) . . . . ? C9 Fe2 C6 C10 -37.9(3) . . . . ? C7 Fe2 C6 C10 -117.8(6) . . . . ? C8 Fe2 C6 C10 -81.1(4) . . . . ? C10 C6 C7 C8 1.1(7) . . . . ? Fe2 C6 C7 C8 -58.8(4) . . . . ? C10 C6 C7 Fe2 59.9(4) . . . . ? C6 Fe2 C7 C8 120.2(6) . . . . ? C5 Fe2 C7 C8 -40.6(10) . . . . ? C2 Fe2 C7 C8 -161.3(4) . . . . ? C10 Fe2 C7 C8 81.3(4) . . . . ? C3 Fe2 C7 C8 -118.5(4) . . . . ? C1 Fe2 C7 C8 163.3(8) . . . . ? C4 Fe2 C7 C8 -77.2(5) . . . . ? C9 Fe2 C7 C8 36.8(4) . . . . ? C5 Fe2 C7 C6 -160.8(8) . . . . ? C2 Fe2 C7 C6 78.5(5) . . . . ? C10 Fe2 C7 C6 -38.9(4) . . . . ? C3 Fe2 C7 C6 121.2(5) . . . . ? C1 Fe2 C7 C6 43.0(10) . . . . ? C4 Fe2 C7 C6 162.6(4) . . . . ? C9 Fe2 C7 C6 -83.4(4) . . . . ? C8 Fe2 C7 C6 -120.2(6) . . . . ? C6 C7 C8 C9 -0.5(7) . . . . ? Fe2 C7 C8 C9 -58.5(4) . . . . ? C6 C7 C8 Fe2 58.0(4) . . . . ? C6 Fe2 C8 C9 82.9(4) . . . . ? C5 Fe2 C8 C9 -74.8(5) . . . . ? C2 Fe2 C8 C9 167.9(7) . . . . ? C10 Fe2 C8 C9 38.2(4) . . . . ? C3 Fe2 C8 C9 -158.7(4) . . . . ? C1 Fe2 C8 C9 -41.3(10) . . . . ? C4 Fe2 C8 C9 -117.1(4) . . . . ? C7 Fe2 C8 C9 120.6(5) . . . . ? C6 Fe2 C8 C7 -37.6(4) . . . . ? C5 Fe2 C8 C7 164.6(4) . . . . ? C2 Fe2 C8 C7 47.3(9) . . . . ? C10 Fe2 C8 C7 -82.4(4) . . . . ? C3 Fe2 C8 C7 80.8(5) . . . . ? C1 Fe2 C8 C7 -161.9(8) . . . . ? C4 Fe2 C8 C7 122.4(4) . . . . ? C9 Fe2 C8 C7 -120.6(5) . . . . ? C7 C8 C9 C10 -0.3(7) . . . . ? Fe2 C8 C9 C10 -59.0(4) . . . . ? C7 C8 C9 Fe2 58.7(5) . . . . ? C6 Fe2 C9 C8 -81.1(4) . . . . ? C5 Fe2 C9 C8 123.0(4) . . . . ? C2 Fe2 C9 C8 -167.0(8) . . . . ? C10 Fe2 C9 C8 -119.3(6) . . . . ? C3 Fe2 C9 C8 50.9(9) . . . . ? C1 Fe2 C9 C8 164.2(4) . . . . ? C4 Fe2 C9 C8 81.6(5) . . . . ? C7 Fe2 C9 C8 -36.8(4) . . . . ? C6 Fe2 C9 C10 38.2(3) . . . . ? C5 Fe2 C9 C10 -117.7(4) . . . . ? C2 Fe2 C9 C10 -47.7(10) . . . . ? C3 Fe2 C9 C10 170.2(7) . . . . ? C1 Fe2 C9 C10 -76.5(4) . . . . ? C4 Fe2 C9 C10 -159.1(4) . . . . ? C7 Fe2 C9 C10 82.5(4) . . . . ? C8 Fe2 C9 C10 119.3(6) . . . . ? C8 C9 C10 C6 1.0(6) . . . . ? Fe2 C9 C10 C6 -58.8(4) . . . . ? C8 C9 C10 C11 179.7(5) . . . . ? Fe2 C9 C10 C11 119.9(5) . . . . ? C8 C9 C10 Fe2 59.8(4) . . . . ? C7 C6 C10 C9 -1.3(6) . . . . ? Fe2 C6 C10 C9 59.1(4) . . . . ? C7 C6 C10 C11 180.0(5) . . . . ? Fe2 C6 C10 C11 -119.6(5) . . . . ? C7 C6 C10 Fe2 -60.4(4) . . . . ? C6 Fe2 C10 C9 -119.2(5) . . . . ? C5 Fe2 C10 C9 80.0(4) . . . . ? C2 Fe2 C10 C9 162.4(4) . . . . ? C3 Fe2 C10 C9 -167.9(9) . . . . ? C1 Fe2 C10 C9 122.1(4) . . . . ? C4 Fe2 C10 C9 50.2(8) . . . . ? C7 Fe2 C10 C9 -80.5(4) . . . . ? C8 Fe2 C10 C9 -37.2(4) . . . . ? C5 Fe2 C10 C6 -160.9(4) . . . . ? C2 Fe2 C10 C6 -78.4(5) . . . . ? C3 Fe2 C10 C6 -48.7(10) . . . . ? C1 Fe2 C10 C6 -118.7(4) . . . . ? C4 Fe2 C10 C6 169.3(7) . . . . ? C9 Fe2 C10 C6 119.2(5) . . . . ? C7 Fe2 C10 C6 38.7(4) . . . . ? C8 Fe2 C10 C6 82.0(4) . . . . ? C6 Fe2 C10 C11 119.0(7) . . . . ? C5 Fe2 C10 C11 -41.9(6) . . . . ? C2 Fe2 C10 C11 40.6(7) . . . . ? C3 Fe2 C10 C11 70.3(11) . . . . ? C1 Fe2 C10 C11 0.3(6) . . . . ? C4 Fe2 C10 C11 -71.7(9) . . . . ? C9 Fe2 C10 C11 -121.8(6) . . . . ? C7 Fe2 C10 C11 157.7(6) . . . . ? C8 Fe2 C10 C11 -159.0(6) . . . . ? C9 C10 C11 C19 -171.8(5) . . . . ? C6 C10 C11 C19 6.7(8) . . . . ? Fe2 C10 C11 C19 -81.5(7) . . . . ? C9 C10 C11 C12 10.0(8) . . . . ? C6 C10 C11 C12 -171.6(5) . . . . ? Fe2 C10 C11 C12 100.3(6) . . . . ? C19 C11 C12 C13 -1.4(8) . . . . ? C10 C11 C12 C13 177.0(5) . . . . ? C20 N2 C13 C12 2.1(8) . . . . ? Co1 N2 C13 C12 -170.8(4) . . . . ? C20 N2 C13 C14 -179.9(5) . . . . ? Co1 N2 C13 C14 7.2(6) . . . . ? C11 C12 C13 N2 -0.8(8) . . . . ? C11 C12 C13 C14 -178.5(5) . . . . ? C18 N1 C14 C15 2.3(7) . . . . ? Co1 N1 C14 C15 -175.4(4) . . . . ? C18 N1 C14 C13 178.7(5) . . . . ? Co1 N1 C14 C13 1.0(5) . . . . ? N2 C13 C14 N1 -5.1(6) . . . . ? C12 C13 C14 N1 172.9(5) . . . . ? N2 C13 C14 C15 171.3(5) . . . . ? C12 C13 C14 C15 -10.8(8) . . . . ? N1 C14 C15 C16 -1.5(8) . . . . ? C13 C14 C15 C16 -177.6(5) . . . . ? C14 C15 C16 C17 0.6(9) . . . . ? C15 C16 C17 C18 -0.7(9) . . . . ? C14 N1 C18 C17 -2.3(8) . . . . ? Co1 N1 C18 C17 175.0(4) . . . . ? C16 C17 C18 N1 1.5(9) . . . . ? C12 C11 C19 C20 2.2(8) . . . . ? C10 C11 C19 C20 -176.1(5) . . . . ? C13 N2 C20 C19 -1.2(8) . . . . ? Co1 N2 C20 C19 171.7(4) . . . . ? C13 N2 C20 C21 179.6(5) . . . . ? Co1 N2 C20 C21 -7.5(6) . . . . ? C11 C19 C20 N2 -0.9(9) . . . . ? C11 C19 C20 C21 178.1(6) . . . . ? C25 N3 C21 C22 1.5(10) . . . . ? Co1 N3 C21 C22 -178.7(6) . . . . ? C25 N3 C21 C20 -176.8(5) . . . . ? Co1 N3 C21 C20 3.0(7) . . . . ? N2 C20 C21 N3 2.5(8) . . . . ? C19 C20 C21 N3 -176.7(6) . . . . ? N2 C20 C21 C22 -175.8(7) . . . . ? C19 C20 C21 C22 5.1(11) . . . . ? N3 C21 C22 C23 1.9(14) . . . . ? C20 C21 C22 C23 180.0(8) . . . . ? C21 C22 C23 C24 -4.9(16) . . . . ? C22 C23 C24 C25 4.6(16) . . . . ? C21 N3 C25 C24 -1.7(11) . . . . ? Co1 N3 C25 C24 178.5(7) . . . . ? C23 C24 C25 N3 -1.4(15) . . . . ? O4 O3 Cl1 O1 116.9(6) . . . . ? O4 O3 Cl1 O2 -121.6(7) . . . . ? O3 O4 Cl1 O1 -106.4(9) . . . . ? O3 O4 Cl1 O2 104.4(9) . . . . ? N4 C26 C27 C27 180.000(10) . . . 2_655 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.973 _refine_diff_density_min -0.706 _refine_diff_density_rms 0.088 data_arc2 _database_code_depnum_ccdc_archive 'CCDC 829879' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H44 Cl2 Fe2 N8 O8 Zn' _chemical_formula_sum 'C54 H44 Cl2 Fe2 N8 O8 Zn' _chemical_formula_weight 1180.94 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' Zn Zn 0.2839 1.4301 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M c2/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' '-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 20.804(2) _cell_length_b 19.191(2) _cell_length_c 13.0849(12) _cell_angle_alpha 90.00 _cell_angle_beta 96.236(8) _cell_angle_gamma 90.00 _cell_volume 5193.2(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.510 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2416 _exptl_absorpt_coefficient_mu 1.175 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6838 _exptl_absorpt_correction_T_max 0.7904 _exptl_absorpt_process_details SADABS(Sheldrick,1997) _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 Smart CCD Area Detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16597 _diffrn_reflns_av_R_equivalents 0.0864 _diffrn_reflns_av_sigmaI/netI 0.0994 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5093 _reflns_number_gt 2469 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Smart' _computing_data_reduction 'Bruker Saint' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.1572P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5093 _refine_ls_number_parameters 350 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1657 _refine_ls_R_factor_gt 0.0832 _refine_ls_wR_factor_ref 0.2806 _refine_ls_wR_factor_gt 0.2283 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.076 _refine_ls_shift/su_mean 0.004 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 0.68815(6) 0.23262(7) 0.79355(8) 0.0698(5) Uani 1 1 d . . . Zn1 Zn 0.5000 0.21600(6) 0.2500 0.0518(4) Uani 1 2 d S . . N1 N 0.4541(4) 0.2963(3) 0.3329(5) 0.0665(19) Uani 1 1 d . . . N2 N 0.5465(3) 0.2101(3) 0.3971(4) 0.0525(15) Uani 1 1 d . . . N3 N 0.5764(3) 0.1371(3) 0.2394(4) 0.0484(14) Uani 1 1 d . . . N4 N 0.5000 0.3699(8) 0.7500 0.123(5) Uani 1 2 d S . . N5 N 0.483(2) 0.023(2) 0.560(3) 0.23(2) Uani 0.50 1 d P . . Cl1 Cl 0.32159(15) 0.44272(15) 0.04896(19) 0.0852(8) Uani 1 1 d . . . O1 O 0.3593(7) 0.4751(6) 0.1200(9) 0.214(7) Uani 1 1 d . . . O2 O 0.3316(15) 0.3782(9) 0.0511(11) 0.338(15) Uani 1 1 d . . . O3 O 0.2650(9) 0.443(2) 0.0707(17) 0.43(2) Uani 1 1 d . . . O4 O 0.3138(8) 0.4679(7) -0.0455(8) 0.222(7) Uani 1 1 d . . . C1 C 0.7672(6) 0.2667(6) 0.7329(9) 0.093(3) Uani 1 1 d . . . H1 H 0.7908 0.2408 0.6899 0.112 Uiso 1 1 calc R . . C2 C 0.7778(6) 0.2690(6) 0.8394(9) 0.097(3) Uani 1 1 d . . . H2 H 0.8097 0.2449 0.8803 0.117 Uiso 1 1 calc R . . C3 C 0.7320(6) 0.3138(7) 0.8746(8) 0.097(3) Uani 1 1 d . . . H3 H 0.7289 0.3240 0.9434 0.116 Uiso 1 1 calc R . . C4 C 0.6917(6) 0.3410(6) 0.7920(11) 0.107(4) Uani 1 1 d . . . H4 H 0.6575 0.3721 0.7943 0.129 Uiso 1 1 calc R . . C5 C 0.7147(6) 0.3102(6) 0.7020(9) 0.100(4) Uani 1 1 d . . . H5 H 0.6975 0.3180 0.6344 0.120 Uiso 1 1 calc R . . C6 C 0.6747(5) 0.1324(5) 0.7448(6) 0.076(3) Uani 1 1 d . . . H6 H 0.7016 0.1080 0.7052 0.091 Uiso 1 1 calc R . . C7 C 0.6789(6) 0.1346(6) 0.8543(7) 0.088(3) Uani 1 1 d . . . H7 H 0.7089 0.1103 0.8985 0.106 Uiso 1 1 calc R . . C8 C 0.6311(6) 0.1789(7) 0.8854(7) 0.092(3) Uani 1 1 d . . . H8 H 0.6244 0.1893 0.9529 0.111 Uiso 1 1 calc R . . C9 C 0.5946(5) 0.2049(5) 0.7957(6) 0.080(3) Uani 1 1 d . . . H9 H 0.5600 0.2356 0.7940 0.096 Uiso 1 1 calc R . . C10 C 0.6206(4) 0.1756(4) 0.7080(6) 0.066(2) Uani 1 1 d . . . C11 C 0.5963(4) 0.1898(4) 0.5981(5) 0.058(2) Uani 1 1 d . . . C12 C 0.6192(4) 0.1505(4) 0.5205(6) 0.058(2) Uani 1 1 d . . . H12 H 0.6510 0.1169 0.5357 0.069 Uiso 1 1 calc R . . C13 C 0.5932(4) 0.1627(4) 0.4191(5) 0.0486(17) Uani 1 1 d . . . C14 C 0.6131(4) 0.1232(4) 0.3278(5) 0.0515(18) Uani 1 1 d . . . C15 C 0.6646(4) 0.0803(4) 0.3337(6) 0.064(2) Uani 1 1 d . . . H15 H 0.6886 0.0718 0.3966 0.076 Uiso 1 1 calc R . . C16 C 0.6813(4) 0.0492(4) 0.2459(8) 0.068(2) Uani 1 1 d . . . H16 H 0.7171 0.0200 0.2482 0.082 Uiso 1 1 calc R . . C17 C 0.6441(4) 0.0619(5) 0.1550(7) 0.069(2) Uani 1 1 d . . . H17 H 0.6537 0.0406 0.0947 0.083 Uiso 1 1 calc R . . C18 C 0.5929(4) 0.1061(4) 0.1538(6) 0.059(2) Uani 1 1 d . . . H18 H 0.5684 0.1152 0.0915 0.071 Uiso 1 1 calc R . . C19 C 0.4101(5) 0.3425(5) 0.2924(7) 0.092(3) Uani 1 1 d . . . H19 H 0.3988 0.3422 0.2216 0.110 Uiso 1 1 calc R . . C20 C 0.3813(8) 0.3899(7) 0.3506(9) 0.163(7) Uani 1 1 d . . . H20 H 0.3492 0.4197 0.3209 0.196 Uiso 1 1 calc R . . C21 C 0.4015(10) 0.3924(9) 0.4561(10) 0.206(11) Uani 1 1 d . . . H21 H 0.3844 0.4253 0.4979 0.248 Uiso 1 1 calc R . . C22 C 0.4471(9) 0.3452(6) 0.4966(8) 0.153(7) Uani 1 1 d . . . H22 H 0.4598 0.3450 0.5670 0.184 Uiso 1 1 calc R . . C23 C 0.4740(6) 0.2985(5) 0.4345(6) 0.088(3) Uani 1 1 d . . . C24 C 0.5258(5) 0.2481(4) 0.4712(6) 0.064(2) Uani 1 1 d . . . C25 C 0.5516(5) 0.2399(4) 0.5725(6) 0.071(3) Uani 1 1 d . . . H25 H 0.5383 0.2689 0.6231 0.085 Uiso 1 1 calc R . . C26 C 0.5000 0.4241(13) 0.7500 0.181(13) Uani 1 2 d S . . C27 C 0.5000 0.4926(16) 0.7500 0.56(7) Uani 1 2 d S . . C28 C 0.5000 0.0387(15) 0.7500 0.150(12) Uani 1 2 d S . . C29 C 0.4928(14) 0.0351(16) 0.648(5) 0.16(2) Uani 0.50 1 d P . . 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 0.0820(10) 0.0835(9) 0.0418(6) 0.0006(5) -0.0026(6) -0.0311(7) Zn1 0.0638(9) 0.0583(8) 0.0321(6) 0.000 0.0003(5) 0.000 N1 0.100(6) 0.057(4) 0.044(4) 0.003(3) 0.013(4) 0.020(4) N2 0.067(4) 0.050(3) 0.038(3) 0.006(3) -0.004(3) -0.002(3) N3 0.053(4) 0.057(4) 0.035(3) -0.007(3) 0.000(3) -0.002(3) N4 0.211(17) 0.091(10) 0.068(8) 0.000 0.021(9) 0.000 N5 0.25(5) 0.21(4) 0.20(4) 0.06(3) -0.05(3) 0.07(3) Cl1 0.099(2) 0.0846(17) 0.0688(15) 0.0079(13) -0.0039(14) -0.0227(14) O1 0.275(15) 0.174(10) 0.161(9) 0.048(8) -0.120(10) -0.107(10) O2 0.66(5) 0.176(13) 0.141(11) -0.040(10) -0.106(18) 0.11(2) O3 0.146(14) 0.88(7) 0.26(2) -0.08(3) 0.045(14) -0.12(2) O4 0.331(17) 0.204(11) 0.112(7) 0.063(8) -0.060(9) -0.147(12) C1 0.096(9) 0.097(8) 0.090(8) -0.007(6) 0.026(7) -0.038(7) C2 0.087(8) 0.114(9) 0.088(8) -0.002(6) -0.004(6) -0.043(7) C3 0.100(8) 0.121(9) 0.067(6) -0.028(7) 0.002(6) -0.034(7) C4 0.111(10) 0.088(8) 0.122(10) -0.008(7) 0.015(9) -0.039(6) C5 0.114(10) 0.091(8) 0.088(8) 0.028(7) -0.021(7) -0.054(7) C6 0.088(7) 0.083(6) 0.054(5) 0.010(4) -0.011(5) -0.021(5) C7 0.101(8) 0.106(8) 0.051(5) 0.034(5) -0.021(5) -0.038(6) C8 0.103(8) 0.134(9) 0.039(5) 0.008(5) -0.002(5) -0.051(7) C9 0.093(7) 0.105(7) 0.043(5) 0.000(4) 0.009(5) -0.041(5) C10 0.082(6) 0.073(5) 0.041(4) 0.014(4) -0.010(4) -0.029(5) C11 0.076(6) 0.063(5) 0.033(4) 0.003(3) -0.008(4) -0.019(4) C12 0.061(5) 0.059(5) 0.050(4) 0.000(4) -0.008(4) -0.016(4) C13 0.058(5) 0.047(4) 0.038(4) 0.001(3) -0.003(3) -0.008(3) C14 0.053(5) 0.048(4) 0.052(4) 0.004(3) 0.000(4) -0.008(4) C15 0.060(5) 0.073(5) 0.055(5) 0.010(4) -0.008(4) 0.003(4) C16 0.054(5) 0.067(5) 0.087(6) 0.005(5) 0.017(5) 0.002(4) C17 0.063(6) 0.076(6) 0.070(6) -0.007(4) 0.022(5) 0.001(5) C18 0.066(5) 0.066(5) 0.047(4) -0.004(4) 0.013(4) -0.007(4) C19 0.127(9) 0.091(7) 0.056(5) 0.013(5) 0.003(6) 0.041(6) C20 0.274(19) 0.139(11) 0.080(8) 0.029(8) 0.037(10) 0.147(13) C21 0.37(3) 0.174(14) 0.076(8) 0.004(8) 0.020(11) 0.200(18) C22 0.31(2) 0.098(8) 0.056(6) 0.002(6) 0.018(9) 0.096(11) C23 0.157(10) 0.063(5) 0.043(4) 0.011(4) 0.008(5) 0.024(6) C24 0.104(7) 0.053(4) 0.036(4) -0.004(3) 0.010(4) 0.013(4) C25 0.124(8) 0.053(5) 0.038(4) 0.002(4) 0.015(5) -0.006(5) C26 0.17(2) 0.087(14) 0.25(3) 0.000 -0.10(2) 0.000 C27 0.47(7) 0.10(2) 0.96(15) 0.000 -0.55(10) 0.000 C28 0.17(3) 0.117(18) 0.17(3) 0.000 0.07(3) 0.000 C29 0.056(17) 0.09(2) 0.33(7) 0.07(4) 0.02(3) 0.006(13) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 2.011(10) . ? Fe1 C2 2.020(10) . ? Fe1 C10 2.021(8) . ? Fe1 C5 2.025(10) . ? Fe1 C9 2.020(9) . ? Fe1 C6 2.035(9) . ? Fe1 C3 2.043(10) . ? Fe1 C7 2.059(9) . ? Fe1 C8 2.057(9) . ? Fe1 C4 2.082(11) . ? Zn1 N2 2.061(6) 2_655 ? Zn1 N2 2.061(6) . ? Zn1 N1 2.165(6) 2_655 ? Zn1 N1 2.165(6) . ? Zn1 N3 2.211(6) 2_655 ? Zn1 N3 2.211(6) . ? N1 C19 1.340(10) . ? N1 C23 1.350(10) . ? N2 C24 1.323(9) . ? N2 C13 1.339(9) . ? N3 C14 1.341(9) . ? N3 C18 1.345(9) . ? N4 C26 1.04(2) . ? N5 C29 1.18(6) . ? Cl1 O2 1.256(16) . ? Cl1 O1 1.307(9) . ? Cl1 O4 1.321(9) . ? Cl1 O3 1.241(17) . ? C1 C2 1.387(15) . ? C1 C5 1.399(16) . ? C1 H1 0.9300 . ? C2 C3 1.398(16) . ? C2 H2 0.9300 . ? C3 C4 1.396(16) . ? C3 H3 0.9300 . ? C4 C5 1.446(16) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.426(12) . ? C6 C10 1.439(12) . ? C6 H6 0.9300 . ? C7 C8 1.402(15) . ? C7 H7 0.9300 . ? C8 C9 1.417(13) . ? C8 H8 0.9300 . ? C9 C10 1.436(12) . ? C9 H9 0.9300 . ? C10 C11 1.496(10) . ? C11 C25 1.355(12) . ? C11 C12 1.390(11) . ? C12 C13 1.397(10) . ? C12 H12 0.9300 . ? C13 C14 1.509(10) . ? C14 C15 1.348(11) . ? C15 C16 1.371(12) . ? C15 H15 0.9300 . ? C16 C17 1.369(12) . ? C16 H16 0.9300 . ? C17 C18 1.360(11) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.367(14) . ? C19 H19 0.9300 . ? C20 C21 1.400(18) . ? C20 H20 0.9300 . ? C21 C22 1.376(16) . ? C21 H21 0.9300 . ? C22 C23 1.370(13) . ? C22 H22 0.9300 . ? C23 C24 1.490(13) . ? C24 C25 1.384(11) . ? C25 H25 0.9300 . ? C26 C27 1.32(3) . ? C28 C29 1.33(7) . ? C28 C29 1.33(7) 2_656 ? 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 C1 Fe1 C2 40.3(4) . . ? C1 Fe1 C10 120.4(4) . . ? C2 Fe1 C10 156.3(5) . . ? C1 Fe1 C5 40.6(5) . . ? C2 Fe1 C5 67.6(5) . . ? C10 Fe1 C5 106.8(4) . . ? C1 Fe1 C9 157.1(4) . . ? C2 Fe1 C9 161.1(4) . . ? C10 Fe1 C9 41.6(4) . . ? C5 Fe1 C9 121.8(5) . . ? C1 Fe1 C6 105.9(4) . . ? C2 Fe1 C6 120.7(5) . . ? C10 Fe1 C6 41.5(3) . . ? C5 Fe1 C6 123.1(5) . . ? C9 Fe1 C6 69.9(4) . . ? C1 Fe1 C3 67.6(4) . . ? C2 Fe1 C3 40.2(4) . . ? C10 Fe1 C3 160.9(5) . . ? C5 Fe1 C3 67.2(4) . . ? C9 Fe1 C3 124.7(5) . . ? C6 Fe1 C3 157.1(5) . . ? C1 Fe1 C7 124.3(5) . . ? C2 Fe1 C7 108.8(5) . . ? C10 Fe1 C7 68.3(3) . . ? C5 Fe1 C7 160.5(6) . . ? C9 Fe1 C7 67.9(4) . . ? C6 Fe1 C7 40.8(4) . . ? C3 Fe1 C7 123.4(4) . . ? C1 Fe1 C8 160.5(5) . . ? C2 Fe1 C8 124.9(4) . . ? C10 Fe1 C8 69.0(3) . . ? C5 Fe1 C8 157.9(6) . . ? C9 Fe1 C8 40.7(4) . . ? C6 Fe1 C8 69.0(4) . . ? C3 Fe1 C8 109.4(4) . . ? C7 Fe1 C8 39.8(4) . . ? C1 Fe1 C4 68.9(5) . . ? C2 Fe1 C4 68.0(5) . . ? C10 Fe1 C4 124.0(4) . . ? C5 Fe1 C4 41.2(5) . . ? C9 Fe1 C4 107.4(5) . . ? C6 Fe1 C4 160.9(5) . . ? C3 Fe1 C4 39.6(5) . . ? C7 Fe1 C4 157.1(5) . . ? C8 Fe1 C4 122.0(5) . . ? N2 Zn1 N2 173.7(3) 2_655 . ? N2 Zn1 N1 76.1(3) 2_655 2_655 ? N2 Zn1 N1 108.6(2) . 2_655 ? N2 Zn1 N1 108.6(2) 2_655 . ? N2 Zn1 N1 76.1(3) . . ? N1 Zn1 N1 89.3(4) 2_655 . ? N2 Zn1 N3 75.7(2) 2_655 2_655 ? N2 Zn1 N3 99.9(2) . 2_655 ? N1 Zn1 N3 151.4(2) 2_655 2_655 ? N1 Zn1 N3 95.5(3) . 2_655 ? N2 Zn1 N3 99.9(2) 2_655 . ? N2 Zn1 N3 75.7(2) . . ? N1 Zn1 N3 95.5(3) 2_655 . ? N1 Zn1 N3 151.4(2) . . ? N3 Zn1 N3 93.5(3) 2_655 . ? C19 N1 C23 119.5(7) . . ? C19 N1 Zn1 126.3(6) . . ? C23 N1 Zn1 114.3(6) . . ? C24 N2 C13 120.2(6) . . ? C24 N2 Zn1 119.8(5) . . ? C13 N2 Zn1 119.6(5) . . ? C14 N3 C18 117.3(7) . . ? C14 N3 Zn1 115.3(5) . . ? C18 N3 Zn1 127.2(5) . . ? O2 Cl1 O1 111.6(11) . . ? O2 Cl1 O4 112.7(9) . . ? O1 Cl1 O4 119.6(7) . . ? O2 Cl1 O3 99.1(18) . . ? O1 Cl1 O3 110.3(14) . . ? O4 Cl1 O3 100.9(15) . . ? C2 C1 C5 107.8(11) . . ? C2 C1 Fe1 70.2(6) . . ? C5 C1 Fe1 70.2(6) . . ? C2 C1 H1 126.1 . . ? C5 C1 H1 126.1 . . ? Fe1 C1 H1 125.0 . . ? C1 C2 C3 108.2(12) . . ? C1 C2 Fe1 69.5(6) . . ? C3 C2 Fe1 70.8(6) . . ? C1 C2 H2 125.9 . . ? C3 C2 H2 125.9 . . ? Fe1 C2 H2 125.4 . . ? C4 C3 C2 110.4(11) . . ? C4 C3 Fe1 71.7(6) . . ? C2 C3 Fe1 69.0(6) . . ? C4 C3 H3 124.8 . . ? C2 C3 H3 124.8 . . ? Fe1 C3 H3 126.1 . . ? C3 C4 C5 104.6(12) . . ? C3 C4 Fe1 68.7(7) . . ? C5 C4 Fe1 67.3(6) . . ? C3 C4 H4 127.7 . . ? C5 C4 H4 127.7 . . ? Fe1 C4 H4 127.8 . . ? C1 C5 C4 109.0(10) . . ? C1 C5 Fe1 69.2(6) . . ? C4 C5 Fe1 71.5(6) . . ? C1 C5 H5 125.5 . . ? C4 C5 H5 125.5 . . ? Fe1 C5 H5 125.4 . . ? C7 C6 C10 106.2(9) . . ? C7 C6 Fe1 70.5(6) . . ? C10 C6 Fe1 68.7(5) . . ? C7 C6 H6 126.9 . . ? C10 C6 H6 126.9 . . ? Fe1 C6 H6 125.5 . . ? C8 C7 C6 110.0(9) . . ? C8 C7 Fe1 70.0(6) . . ? C6 C7 Fe1 68.7(5) . . ? C8 C7 H7 125.0 . . ? C6 C7 H7 125.0 . . ? Fe1 C7 H7 127.9 . . ? C7 C8 C9 107.8(8) . . ? C7 C8 Fe1 70.2(6) . . ? C9 C8 Fe1 68.3(5) . . ? C7 C8 H8 126.1 . . ? C9 C8 H8 126.1 . . ? Fe1 C8 H8 127.0 . . ? C8 C9 C10 108.1(10) . . ? C8 C9 Fe1 71.1(6) . . ? C10 C9 Fe1 69.3(5) . . ? C8 C9 H9 125.9 . . ? C10 C9 H9 125.9 . . ? Fe1 C9 H9 125.3 . . ? C9 C10 C6 107.8(7) . . ? C9 C10 C11 125.5(9) . . ? C6 C10 C11 126.7(8) . . ? C9 C10 Fe1 69.1(5) . . ? C6 C10 Fe1 69.7(5) . . ? C11 C10 Fe1 125.1(5) . . ? C25 C11 C12 119.0(7) . . ? C25 C11 C10 121.2(8) . . ? C12 C11 C10 119.8(8) . . ? C11 C12 C13 118.4(7) . . ? C11 C12 H12 120.8 . . ? C13 C12 H12 120.8 . . ? N2 C13 C12 121.0(7) . . ? N2 C13 C14 115.2(6) . . ? C12 C13 C14 123.9(7) . . ? N3 C14 C15 123.0(7) . . ? N3 C14 C13 113.8(6) . . ? C15 C14 C13 123.1(7) . . ? C14 C15 C16 119.4(8) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C15 C16 C17 118.7(8) . . ? C15 C16 H16 120.7 . . ? C17 C16 H16 120.7 . . ? C18 C17 C16 119.3(8) . . ? C18 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? N3 C18 C17 122.4(8) . . ? N3 C18 H18 118.8 . . ? C17 C18 H18 118.8 . . ? N1 C19 C20 122.8(9) . . ? N1 C19 H19 118.6 . . ? C20 C19 H19 118.6 . . ? C19 C20 C21 118.0(10) . . ? C19 C20 H20 121.0 . . ? C21 C20 H20 121.0 . . ? C22 C21 C20 118.6(10) . . ? C22 C21 H21 120.7 . . ? C20 C21 H21 120.7 . . ? C23 C22 C21 120.8(10) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? N1 C23 C22 120.3(9) . . ? N1 C23 C24 115.5(7) . . ? C22 C23 C24 124.2(9) . . ? N2 C24 C25 121.1(8) . . ? N2 C24 C23 113.8(7) . . ? C25 C24 C23 125.1(7) . . ? C11 C25 C24 120.1(8) . . ? C11 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? N4 C26 C27 180.000(11) . . ? C29 C28 C29 174(4) . 2_656 ? N5 C29 C28 171(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Zn1 N1 C19 -10.2(9) 2_655 . . . ? N2 Zn1 N1 C19 174.2(9) . . . . ? N1 Zn1 N1 C19 64.9(8) 2_655 . . . ? N3 Zn1 N1 C19 -86.9(8) 2_655 . . . ? N3 Zn1 N1 C19 165.2(7) . . . . ? N2 Zn1 N1 C23 170.9(7) 2_655 . . . ? N2 Zn1 N1 C23 -4.7(7) . . . . ? N1 Zn1 N1 C23 -114.0(8) 2_655 . . . ? N3 Zn1 N1 C23 94.2(7) 2_655 . . . ? N3 Zn1 N1 C23 -13.7(10) . . . . ? N2 Zn1 N2 C24 -131.9(6) 2_655 . . . ? N1 Zn1 N2 C24 90.9(6) 2_655 . . . ? N1 Zn1 N2 C24 6.5(6) . . . . ? N3 Zn1 N2 C24 -86.8(6) 2_655 . . . ? N3 Zn1 N2 C24 -178.0(6) . . . . ? N2 Zn1 N2 C13 41.3(5) 2_655 . . . ? N1 Zn1 N2 C13 -95.8(5) 2_655 . . . ? N1 Zn1 N2 C13 179.7(6) . . . . ? N3 Zn1 N2 C13 86.4(5) 2_655 . . . ? N3 Zn1 N2 C13 -4.7(5) . . . . ? N2 Zn1 N3 C14 -174.3(5) 2_655 . . . ? N2 Zn1 N3 C14 1.1(5) . . . . ? N1 Zn1 N3 C14 108.9(5) 2_655 . . . ? N1 Zn1 N3 C14 10.1(8) . . . . ? N3 Zn1 N3 C14 -98.2(5) 2_655 . . . ? N2 Zn1 N3 C18 11.2(6) 2_655 . . . ? N2 Zn1 N3 C18 -173.4(6) . . . . ? N1 Zn1 N3 C18 -65.6(6) 2_655 . . . ? N1 Zn1 N3 C18 -164.3(6) . . . . ? N3 Zn1 N3 C18 87.3(6) 2_655 . . . ? C10 Fe1 C1 C2 -161.7(7) . . . . ? C5 Fe1 C1 C2 118.3(10) . . . . ? C9 Fe1 C1 C2 165.2(11) . . . . ? C6 Fe1 C1 C2 -119.0(8) . . . . ? C3 Fe1 C1 C2 37.7(7) . . . . ? C7 Fe1 C1 C2 -78.4(8) . . . . ? C8 Fe1 C1 C2 -47.3(16) . . . . ? C4 Fe1 C1 C2 80.4(8) . . . . ? C2 Fe1 C1 C5 -118.3(10) . . . . ? C10 Fe1 C1 C5 80.1(8) . . . . ? C9 Fe1 C1 C5 47.0(15) . . . . ? C6 Fe1 C1 C5 122.7(7) . . . . ? C3 Fe1 C1 C5 -80.5(7) . . . . ? C7 Fe1 C1 C5 163.3(6) . . . . ? C8 Fe1 C1 C5 -165.6(12) . . . . ? C4 Fe1 C1 C5 -37.8(7) . . . . ? C5 C1 C2 C3 0.0(11) . . . . ? Fe1 C1 C2 C3 -60.5(7) . . . . ? C5 C1 C2 Fe1 60.5(7) . . . . ? C10 Fe1 C2 C1 42.4(14) . . . . ? C5 Fe1 C2 C1 -38.3(7) . . . . ? C9 Fe1 C2 C1 -162.2(13) . . . . ? C6 Fe1 C2 C1 78.0(8) . . . . ? C3 Fe1 C2 C1 -118.9(11) . . . . ? C7 Fe1 C2 C1 121.3(8) . . . . ? C8 Fe1 C2 C1 162.5(8) . . . . ? C4 Fe1 C2 C1 -82.9(8) . . . . ? C1 Fe1 C2 C3 118.9(11) . . . . ? C10 Fe1 C2 C3 161.3(9) . . . . ? C5 Fe1 C2 C3 80.6(8) . . . . ? C9 Fe1 C2 C3 -43.3(18) . . . . ? C6 Fe1 C2 C3 -163.1(6) . . . . ? C7 Fe1 C2 C3 -119.9(8) . . . . ? C8 Fe1 C2 C3 -78.6(9) . . . . ? C4 Fe1 C2 C3 35.9(7) . . . . ? C1 C2 C3 C4 -0.2(12) . . . . ? Fe1 C2 C3 C4 -59.9(8) . . . . ? C1 C2 C3 Fe1 59.7(7) . . . . ? C1 Fe1 C3 C4 83.6(8) . . . . ? C2 Fe1 C3 C4 121.3(10) . . . . ? C10 Fe1 C3 C4 -35.4(16) . . . . ? C5 Fe1 C3 C4 39.5(7) . . . . ? C9 Fe1 C3 C4 -74.4(8) . . . . ? C6 Fe1 C3 C4 161.2(10) . . . . ? C7 Fe1 C3 C4 -159.1(7) . . . . ? C8 Fe1 C3 C4 -117.1(8) . . . . ? C1 Fe1 C3 C2 -37.7(7) . . . . ? C10 Fe1 C3 C2 -156.7(10) . . . . ? C5 Fe1 C3 C2 -81.8(8) . . . . ? C9 Fe1 C3 C2 164.3(6) . . . . ? C6 Fe1 C3 C2 39.8(14) . . . . ? C7 Fe1 C3 C2 79.6(8) . . . . ? C8 Fe1 C3 C2 121.6(7) . . . . ? C4 Fe1 C3 C2 -121.3(10) . . . . ? C2 C3 C4 C5 0.3(12) . . . . ? Fe1 C3 C4 C5 -58.0(7) . . . . ? C2 C3 C4 Fe1 58.3(8) . . . . ? C1 Fe1 C4 C3 -79.9(8) . . . . ? C2 Fe1 C4 C3 -36.5(7) . . . . ? C10 Fe1 C4 C3 166.8(7) . . . . ? C5 Fe1 C4 C3 -117.2(11) . . . . ? C9 Fe1 C4 C3 124.0(7) . . . . ? C6 Fe1 C4 C3 -157.5(13) . . . . ? C7 Fe1 C4 C3 49.9(15) . . . . ? C8 Fe1 C4 C3 81.9(8) . . . . ? C1 Fe1 C4 C5 37.3(7) . . . . ? C2 Fe1 C4 C5 80.7(8) . . . . ? C10 Fe1 C4 C5 -76.0(8) . . . . ? C9 Fe1 C4 C5 -118.8(7) . . . . ? C6 Fe1 C4 C5 -40.3(18) . . . . ? C3 Fe1 C4 C5 117.2(11) . . . . ? C7 Fe1 C4 C5 167.1(11) . . . . ? C8 Fe1 C4 C5 -160.9(7) . . . . ? C2 C1 C5 C4 0.2(11) . . . . ? Fe1 C1 C5 C4 60.7(7) . . . . ? C2 C1 C5 Fe1 -60.5(7) . . . . ? C3 C4 C5 C1 -0.3(11) . . . . ? Fe1 C4 C5 C1 -59.2(7) . . . . ? C3 C4 C5 Fe1 58.9(7) . . . . ? C2 Fe1 C5 C1 38.0(7) . . . . ? C10 Fe1 C5 C1 -117.5(7) . . . . ? C9 Fe1 C5 C1 -160.5(6) . . . . ? C6 Fe1 C5 C1 -75.0(8) . . . . ? C3 Fe1 C5 C1 81.7(7) . . . . ? C7 Fe1 C5 C1 -45.3(14) . . . . ? C8 Fe1 C5 C1 167.2(9) . . . . ? C4 Fe1 C5 C1 119.7(10) . . . . ? C1 Fe1 C5 C4 -119.7(10) . . . . ? C2 Fe1 C5 C4 -81.7(8) . . . . ? C10 Fe1 C5 C4 122.8(7) . . . . ? C9 Fe1 C5 C4 79.9(8) . . . . ? C6 Fe1 C5 C4 165.4(7) . . . . ? C3 Fe1 C5 C4 -37.9(7) . . . . ? C7 Fe1 C5 C4 -165.0(11) . . . . ? C8 Fe1 C5 C4 47.5(13) . . . . ? C1 Fe1 C6 C7 124.6(7) . . . . ? C2 Fe1 C6 C7 83.5(8) . . . . ? C10 Fe1 C6 C7 -117.2(9) . . . . ? C5 Fe1 C6 C7 165.3(7) . . . . ? C9 Fe1 C6 C7 -79.1(7) . . . . ? C3 Fe1 C6 C7 54.8(14) . . . . ? C8 Fe1 C6 C7 -35.5(6) . . . . ? C4 Fe1 C6 C7 -164.1(13) . . . . ? C1 Fe1 C6 C10 -118.3(6) . . . . ? C2 Fe1 C6 C10 -159.3(6) . . . . ? C5 Fe1 C6 C10 -77.5(7) . . . . ? C9 Fe1 C6 C10 38.1(5) . . . . ? C3 Fe1 C6 C10 171.9(10) . . . . ? C7 Fe1 C6 C10 117.2(9) . . . . ? C8 Fe1 C6 C10 81.6(6) . . . . ? C4 Fe1 C6 C10 -47.0(16) . . . . ? C10 C6 C7 C8 -1.9(10) . . . . ? Fe1 C6 C7 C8 57.8(7) . . . . ? C10 C6 C7 Fe1 -59.7(6) . . . . ? C1 Fe1 C7 C8 164.4(6) . . . . ? C2 Fe1 C7 C8 122.4(6) . . . . ? C10 Fe1 C7 C8 -82.8(6) . . . . ? C5 Fe1 C7 C8 -161.6(11) . . . . ? C9 Fe1 C7 C8 -37.7(5) . . . . ? C6 Fe1 C7 C8 -122.2(8) . . . . ? C3 Fe1 C7 C8 80.2(7) . . . . ? C4 Fe1 C7 C8 44.5(14) . . . . ? C1 Fe1 C7 C6 -73.5(7) . . . . ? C2 Fe1 C7 C6 -115.5(7) . . . . ? C10 Fe1 C7 C6 39.4(6) . . . . ? C5 Fe1 C7 C6 -39.5(15) . . . . ? C9 Fe1 C7 C6 84.4(6) . . . . ? C3 Fe1 C7 C6 -157.6(7) . . . . ? C8 Fe1 C7 C6 122.2(8) . . . . ? C4 Fe1 C7 C6 166.7(11) . . . . ? C6 C7 C8 C9 1.0(11) . . . . ? Fe1 C7 C8 C9 58.1(6) . . . . ? C6 C7 C8 Fe1 -57.1(6) . . . . ? C1 Fe1 C8 C7 -41.7(15) . . . . ? C2 Fe1 C8 C7 -77.1(8) . . . . ? C10 Fe1 C8 C7 81.0(6) . . . . ? C5 Fe1 C8 C7 163.8(10) . . . . ? C9 Fe1 C8 C7 119.5(8) . . . . ? C6 Fe1 C8 C7 36.3(5) . . . . ? C3 Fe1 C8 C7 -119.3(7) . . . . ? C4 Fe1 C8 C7 -161.3(6) . . . . ? C1 Fe1 C8 C9 -161.3(12) . . . . ? C2 Fe1 C8 C9 163.3(7) . . . . ? C10 Fe1 C8 C9 -38.6(6) . . . . ? C5 Fe1 C8 C9 44.2(14) . . . . ? C6 Fe1 C8 C9 -83.2(6) . . . . ? C3 Fe1 C8 C9 121.1(7) . . . . ? C7 Fe1 C8 C9 -119.5(8) . . . . ? C4 Fe1 C8 C9 79.2(8) . . . . ? C7 C8 C9 C10 0.3(10) . . . . ? Fe1 C8 C9 C10 59.6(6) . . . . ? C7 C8 C9 Fe1 -59.2(7) . . . . ? C1 Fe1 C9 C8 164.0(11) . . . . ? C2 Fe1 C9 C8 -46.6(18) . . . . ? C10 Fe1 C9 C8 118.8(9) . . . . ? C5 Fe1 C9 C8 -162.0(7) . . . . ? C6 Fe1 C9 C8 80.8(7) . . . . ? C3 Fe1 C9 C8 -79.3(9) . . . . ? C7 Fe1 C9 C8 37.0(6) . . . . ? C4 Fe1 C9 C8 -119.2(8) . . . . ? C1 Fe1 C9 C10 45.2(14) . . . . ? C2 Fe1 C9 C10 -165.4(14) . . . . ? C5 Fe1 C9 C10 79.2(7) . . . . ? C6 Fe1 C9 C10 -38.0(5) . . . . ? C3 Fe1 C9 C10 162.0(6) . . . . ? C7 Fe1 C9 C10 -81.8(6) . . . . ? C8 Fe1 C9 C10 -118.8(9) . . . . ? C4 Fe1 C9 C10 122.0(6) . . . . ? C8 C9 C10 C6 -1.5(9) . . . . ? Fe1 C9 C10 C6 59.2(6) . . . . ? C8 C9 C10 C11 -179.7(7) . . . . ? Fe1 C9 C10 C11 -119.0(8) . . . . ? C8 C9 C10 Fe1 -60.7(6) . . . . ? C7 C6 C10 C9 2.0(9) . . . . ? Fe1 C6 C10 C9 -58.8(6) . . . . ? C7 C6 C10 C11 -179.8(7) . . . . ? Fe1 C6 C10 C11 119.4(8) . . . . ? C7 C6 C10 Fe1 60.9(6) . . . . ? C1 Fe1 C10 C9 -161.3(6) . . . . ? C2 Fe1 C10 C9 168.3(10) . . . . ? C5 Fe1 C10 C9 -119.4(7) . . . . ? C6 Fe1 C10 C9 119.3(7) . . . . ? C3 Fe1 C10 C9 -51.1(13) . . . . ? C7 Fe1 C10 C9 80.6(6) . . . . ? C8 Fe1 C10 C9 37.7(6) . . . . ? C4 Fe1 C10 C9 -77.5(7) . . . . ? C1 Fe1 C10 C6 79.4(7) . . . . ? C2 Fe1 C10 C6 49.0(11) . . . . ? C5 Fe1 C10 C6 121.3(6) . . . . ? C9 Fe1 C10 C6 -119.3(7) . . . . ? C3 Fe1 C10 C6 -170.4(11) . . . . ? C7 Fe1 C10 C6 -38.7(6) . . . . ? C8 Fe1 C10 C6 -81.6(6) . . . . ? C4 Fe1 C10 C6 163.2(6) . . . . ? C1 Fe1 C10 C11 -41.9(10) . . . . ? C2 Fe1 C10 C11 -72.3(14) . . . . ? C5 Fe1 C10 C11 0.1(10) . . . . ? C9 Fe1 C10 C11 119.4(10) . . . . ? C6 Fe1 C10 C11 -121.3(10) . . . . ? C3 Fe1 C10 C11 68.4(15) . . . . ? C7 Fe1 C10 C11 -160.0(9) . . . . ? C8 Fe1 C10 C11 157.1(10) . . . . ? C4 Fe1 C10 C11 41.9(10) . . . . ? C9 C10 C11 C25 8.7(12) . . . . ? C6 C10 C11 C25 -169.2(8) . . . . ? Fe1 C10 C11 C25 -79.4(10) . . . . ? C9 C10 C11 C12 -170.5(8) . . . . ? C6 C10 C11 C12 11.6(12) . . . . ? Fe1 C10 C11 C12 101.4(9) . . . . ? C25 C11 C12 C13 -2.4(11) . . . . ? C10 C11 C12 C13 176.9(7) . . . . ? C24 N2 C13 C12 2.5(11) . . . . ? Zn1 N2 C13 C12 -170.7(5) . . . . ? C24 N2 C13 C14 -179.4(7) . . . . ? Zn1 N2 C13 C14 7.4(8) . . . . ? C11 C12 C13 N2 -1.3(10) . . . . ? C11 C12 C13 C14 -179.2(7) . . . . ? C18 N3 C14 C15 -0.1(10) . . . . ? Zn1 N3 C14 C15 -175.1(6) . . . . ? C18 N3 C14 C13 177.2(6) . . . . ? Zn1 N3 C14 C13 2.2(7) . . . . ? N2 C13 C14 N3 -6.1(9) . . . . ? C12 C13 C14 N3 172.0(6) . . . . ? N2 C13 C14 C15 171.3(7) . . . . ? C12 C13 C14 C15 -10.7(11) . . . . ? N3 C14 C15 C16 0.4(12) . . . . ? C13 C14 C15 C16 -176.7(7) . . . . ? C14 C15 C16 C17 -1.1(12) . . . . ? C15 C16 C17 C18 1.6(12) . . . . ? C14 N3 C18 C17 0.6(11) . . . . ? Zn1 N3 C18 C17 174.9(6) . . . . ? C16 C17 C18 N3 -1.3(12) . . . . ? C23 N1 C19 C20 -3.9(18) . . . . ? Zn1 N1 C19 C20 177.3(11) . . . . ? N1 C19 C20 C21 4(2) . . . . ? C19 C20 C21 C22 -3(3) . . . . ? C20 C21 C22 C23 2(3) . . . . ? C19 N1 C23 C22 3.4(17) . . . . ? Zn1 N1 C23 C22 -177.7(11) . . . . ? C19 N1 C23 C24 -176.3(9) . . . . ? Zn1 N1 C23 C24 2.7(11) . . . . ? C21 C22 C23 N1 -3(2) . . . . ? C21 C22 C23 C24 176.9(16) . . . . ? C13 N2 C24 C25 0.0(12) . . . . ? Zn1 N2 C24 C25 173.2(7) . . . . ? C13 N2 C24 C23 179.8(7) . . . . ? Zn1 N2 C24 C23 -6.9(10) . . . . ? N1 C23 C24 N2 2.5(13) . . . . ? C22 C23 C24 N2 -177.1(12) . . . . ? N1 C23 C24 C25 -177.7(9) . . . . ? C22 C23 C24 C25 2.7(19) . . . . ? C12 C11 C25 C24 4.8(13) . . . . ? C10 C11 C25 C24 -174.4(8) . . . . ? N2 C24 C25 C11 -3.7(14) . . . . ? C23 C24 C25 C11 176.4(9) . . . . ? C29 C28 C29 N5 23(26) 2_656 . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.773 _refine_diff_density_min -0.621 _refine_diff_density_rms 0.127 # Attachment '- complex_5.cif' data_5 _database_code_depnum_ccdc_archive 'CCDC 829880' #TrackingRef '- complex_5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H30 Cl2 N6 O8 Zn' _chemical_formula_sum 'C42 H30 Cl2 N6 O8 Zn' _chemical_formula_weight 882.99 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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 9.5145(3) _cell_length_b 12.8131(5) _cell_length_c 31.5604(12) _cell_angle_alpha 90.00 _cell_angle_beta 97.368(2) _cell_angle_gamma 90.00 _cell_volume 3815.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description niddle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.537 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 0.849 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6619 _exptl_absorpt_correction_T_max 0.7729 _exptl_absorpt_process_details SADABS(Sheldrick,1997) _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 Smart CCD Area Detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23784 _diffrn_reflns_av_R_equivalents 0.0456 _diffrn_reflns_av_sigmaI/netI 0.0575 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6994 _reflns_number_gt 4628 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Smart' _computing_data_reduction 'Bruker Saint' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.1057P)^2^+4.4709P] 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 6994 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1007 _refine_ls_R_factor_gt 0.0642 _refine_ls_wR_factor_ref 0.2005 _refine_ls_wR_factor_gt 0.1766 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.45416(5) 0.17786(5) 0.883710(16) 0.0378(2) Uani 1 1 d . . . Cl1 Cl -0.01900(19) 0.28464(17) 0.99023(5) 0.0747(5) Uani 1 1 d . . . O11 O -0.0295(7) 0.1730(5) 0.99506(19) 0.114(2) Uani 1 1 d . . . O12 O 0.0201(12) 0.3308(6) 1.0269(2) 0.202(5) Uani 1 1 d . . . O13 O -0.1665(7) 0.3219(6) 0.9816(2) 0.147(3) Uani 1 1 d . . . Cl2 Cl 0.22226(18) 0.42604(15) 0.75161(5) 0.0689(5) Uani 1 1 d . . . O21 O 0.2554(10) 0.4571(11) 0.7155(3) 0.256(7) Uani 1 1 d . . . O22 O 0.3329(9) 0.3825(7) 0.7770(2) 0.169(4) Uani 1 1 d . . . O23 O 0.1213(12) 0.3604(10) 0.7408(5) 0.300(8) Uani 1 1 d . . . O24 O 0.1705(13) 0.5077(9) 0.7705(3) 0.247(6) Uani 1 1 d . . . O14 O 0.0267(8) 0.3136(6) 0.9516(2) 0.146(3) Uani 1 1 d . . . N1 N 0.2369(4) 0.1176(3) 0.87777(12) 0.0397(9) Uani 1 1 d . . . N2 N 0.3988(4) 0.1556(3) 0.81877(12) 0.0362(9) Uani 1 1 d . . . N3 N 0.6344(4) 0.2395(3) 0.85464(12) 0.0374(9) Uani 1 1 d . . . N4 N 0.3727(4) 0.3254(3) 0.90466(13) 0.0403(10) Uani 1 1 d . . . N5 N 0.5207(4) 0.1828(3) 0.94945(12) 0.0354(9) Uani 1 1 d . . . N6 N 0.5675(4) 0.0285(3) 0.89856(13) 0.0399(9) Uani 1 1 d . . . C1 C 0.7504(5) 0.2861(4) 0.87517(17) 0.0455(12) Uani 1 1 d . . . H1 H 0.7584 0.2938 0.9047 0.055 Uiso 1 1 calc R . . C2 C 0.8576(5) 0.3227(4) 0.8537(2) 0.0542(14) Uani 1 1 d . . . H2 H 0.9373 0.3537 0.8687 0.065 Uiso 1 1 calc R . . C3 C 0.8467(6) 0.3135(5) 0.8107(2) 0.0603(16) Uani 1 1 d . . . H3 H 0.9165 0.3402 0.7957 0.072 Uiso 1 1 calc R . . C4 C 0.7284(6) 0.2630(5) 0.78953(18) 0.0570(15) Uani 1 1 d . . . H4 H 0.7202 0.2533 0.7601 0.068 Uiso 1 1 calc R . . C5 C 0.6248(5) 0.2279(4) 0.81190(15) 0.0397(11) Uani 1 1 d . . . C6 C 0.4931(5) 0.1753(4) 0.79196(15) 0.0381(11) Uani 1 1 d . . . C8 C 0.3350(5) 0.1070(4) 0.73286(15) 0.0411(12) Uani 1 1 d . . . C7 C 0.4656(5) 0.1509(4) 0.74933(15) 0.0441(12) Uani 1 1 d . . . H7 H 0.5338 0.1635 0.7313 0.053 Uiso 1 1 calc R . . C9 C 0.2381(5) 0.0891(4) 0.76138(15) 0.0418(12) Uani 1 1 d . . . H9 H 0.1497 0.0608 0.7518 0.050 Uiso 1 1 calc R . . C10 C 0.2731(5) 0.1133(4) 0.80412(15) 0.0378(11) Uani 1 1 d . . . C11 C 0.1769(5) 0.0992(4) 0.83736(15) 0.0371(11) Uani 1 1 d . . . C12 C 0.0370(5) 0.0718(4) 0.82816(18) 0.0507(14) Uani 1 1 d . . . H12 H -0.0022 0.0586 0.8002 0.061 Uiso 1 1 calc R . . C13 C -0.0441(6) 0.0644(5) 0.8608(2) 0.0594(16) Uani 1 1 d . . . H13 H -0.1392 0.0459 0.8552 0.071 Uiso 1 1 calc R . . C14 C 0.0150(6) 0.0841(5) 0.90190(19) 0.0557(15) Uani 1 1 d . . . H14 H -0.0392 0.0798 0.9244 0.067 Uiso 1 1 calc R . . C15 C 0.1563(5) 0.1106(4) 0.90930(17) 0.0483(13) Uani 1 1 d . . . H15 H 0.1968 0.1241 0.9372 0.058 Uiso 1 1 calc R . . C16 C 0.3005(5) 0.0871(4) 0.68665(15) 0.0405(12) Uani 1 1 d . . . C17 C 0.3991(5) 0.0429(4) 0.66343(16) 0.0489(13) Uani 1 1 d . . . H17 H 0.4873 0.0227 0.6772 0.059 Uiso 1 1 calc R . . C18 C 0.3670(6) 0.0284(5) 0.61976(17) 0.0583(15) Uani 1 1 d . . . H18 H 0.4335 -0.0021 0.6044 0.070 Uiso 1 1 calc R . . C19 C 0.2375(6) 0.0588(5) 0.59882(17) 0.0531(14) Uani 1 1 d . . . H19 H 0.2167 0.0495 0.5695 0.064 Uiso 1 1 calc R . . C20 C 0.1392(6) 0.1031(5) 0.62184(17) 0.0522(14) Uani 1 1 d . . . H20 H 0.0517 0.1243 0.6079 0.063 Uiso 1 1 calc R . . C21 C 0.1699(5) 0.1162(4) 0.66552(16) 0.0480(13) Uani 1 1 d . . . H21 H 0.1021 0.1448 0.6809 0.058 Uiso 1 1 calc R . . C22 C 0.2902(5) 0.3917(5) 0.88034(18) 0.0517(14) Uani 1 1 d . . . H22 H 0.2731 0.3788 0.8511 0.062 Uiso 1 1 calc R . . C23 C 0.2298(6) 0.4768(5) 0.89575(19) 0.0553(15) Uani 1 1 d . . . H23 H 0.1737 0.5213 0.8774 0.066 Uiso 1 1 calc R . . C24 C 0.2528(6) 0.4966(4) 0.9389(2) 0.0565(15) Uani 1 1 d . . . H24 H 0.2119 0.5543 0.9504 0.068 Uiso 1 1 calc R . . C25 C 0.3382(5) 0.4286(4) 0.96502(18) 0.0477(13) Uani 1 1 d . . . H25 H 0.3551 0.4398 0.9943 0.057 Uiso 1 1 calc R . . C26 C 0.3971(5) 0.3447(4) 0.94692(15) 0.0352(11) Uani 1 1 d . . . C27 C 0.4875(5) 0.2649(4) 0.97190(15) 0.0353(11) Uani 1 1 d . . . C28 C 0.5386(5) 0.2747(4) 1.01509(15) 0.0403(11) Uani 1 1 d . . . H28 H 0.5135 0.3323 1.0304 0.048 Uiso 1 1 calc R . . C29 C 0.6268(5) 0.1988(4) 1.03527(15) 0.0375(11) Uani 1 1 d . . . C30 C 0.6564(5) 0.1125(4) 1.01071(15) 0.0410(12) Uani 1 1 d . . . H30 H 0.7128 0.0588 1.0233 0.049 Uiso 1 1 calc R . . C31 C 0.6032(5) 0.1063(4) 0.96817(15) 0.0357(11) Uani 1 1 d . . . C32 C 0.6328(5) 0.0200(4) 0.93916(15) 0.0370(11) Uani 1 1 d . . . C33 C 0.7224(5) -0.0615(4) 0.95114(17) 0.0479(13) Uani 1 1 d . . . H33 H 0.7673 -0.0659 0.9790 0.057 Uiso 1 1 calc R . . C34 C 0.7459(6) -0.1372(5) 0.9217(2) 0.0585(15) Uani 1 1 d . . . H34 H 0.8059 -0.1932 0.9296 0.070 Uiso 1 1 calc R . . C35 C 0.6803(6) -0.1288(4) 0.8811(2) 0.0563(15) Uani 1 1 d . . . H35 H 0.6948 -0.1787 0.8607 0.068 Uiso 1 1 calc R . . C36 C 0.5913(6) -0.0449(4) 0.87053(17) 0.0507(14) Uani 1 1 d . . . H36 H 0.5463 -0.0395 0.8427 0.061 Uiso 1 1 calc R . . C37 C 0.6921(5) 0.2097(4) 1.07983(16) 0.0422(12) Uani 1 1 d . . . C38 C 0.8273(6) 0.1698(4) 1.09313(18) 0.0524(14) Uani 1 1 d . . . H38 H 0.8757 0.1340 1.0738 0.063 Uiso 1 1 calc R . . C39 C 0.8895(7) 0.1831(5) 1.13470(18) 0.0615(16) Uani 1 1 d . . . H39 H 0.9806 0.1579 1.1429 0.074 Uiso 1 1 calc R . . C40 C 0.8197(7) 0.2325(6) 1.16400(19) 0.0691(18) Uani 1 1 d . . . H40 H 0.8605 0.2381 1.1923 0.083 Uiso 1 1 calc R . . C41 C 0.6891(8) 0.2736(7) 1.1512(2) 0.082(2) Uani 1 1 d . . . H41 H 0.6430 0.3104 1.1707 0.099 Uiso 1 1 calc R . . C42 C 0.6231(6) 0.2618(5) 1.10963(17) 0.0591(16) Uani 1 1 d . . . H42 H 0.5327 0.2888 1.1018 0.071 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 Zn1 0.0385(3) 0.0440(4) 0.0302(3) -0.0023(3) 0.0017(2) -0.0017(2) Cl1 0.0787(11) 0.0972(14) 0.0500(9) -0.0237(9) 0.0151(8) -0.0196(10) O11 0.152(6) 0.103(5) 0.096(4) -0.021(3) 0.047(4) -0.012(4) O12 0.331(12) 0.147(7) 0.095(5) -0.064(5) -0.096(6) 0.042(7) O13 0.099(5) 0.185(8) 0.156(7) 0.016(5) 0.010(4) 0.011(5) Cl2 0.0780(10) 0.0755(12) 0.0498(9) 0.0144(8) -0.0054(7) 0.0027(9) O21 0.173(8) 0.48(2) 0.129(6) 0.162(10) 0.071(6) 0.111(10) O22 0.211(8) 0.180(7) 0.096(5) -0.002(5) -0.051(5) 0.111(6) O23 0.180(10) 0.190(11) 0.51(2) -0.036(13) -0.020(12) -0.087(9) O24 0.330(14) 0.223(11) 0.166(8) -0.061(8) -0.047(8) 0.181(11) O14 0.161(7) 0.179(7) 0.103(5) -0.007(5) 0.039(4) -0.054(5) N1 0.040(2) 0.042(3) 0.038(2) -0.001(2) 0.0069(17) -0.0047(18) N2 0.032(2) 0.043(2) 0.034(2) -0.0007(18) 0.0027(16) -0.0044(17) N3 0.035(2) 0.043(3) 0.034(2) -0.0017(19) 0.0024(16) -0.0043(18) N4 0.039(2) 0.039(2) 0.042(2) 0.002(2) 0.0021(17) 0.0004(18) N5 0.036(2) 0.034(2) 0.037(2) -0.0001(19) 0.0049(16) 0.0007(17) N6 0.041(2) 0.037(2) 0.042(2) -0.006(2) 0.0054(18) -0.0009(18) C1 0.044(3) 0.049(3) 0.042(3) -0.008(3) -0.002(2) -0.007(2) C2 0.039(3) 0.053(4) 0.068(4) -0.013(3) -0.001(3) -0.007(2) C3 0.045(3) 0.075(4) 0.063(4) -0.005(3) 0.013(3) -0.018(3) C4 0.059(3) 0.074(4) 0.040(3) -0.002(3) 0.014(3) -0.024(3) C5 0.037(2) 0.045(3) 0.037(3) -0.006(2) 0.002(2) -0.005(2) C6 0.036(2) 0.046(3) 0.032(3) -0.002(2) 0.0052(19) -0.003(2) C8 0.043(3) 0.049(3) 0.030(3) -0.001(2) 0.001(2) 0.001(2) C7 0.041(3) 0.060(4) 0.032(3) 0.000(2) 0.005(2) -0.009(2) C9 0.035(2) 0.052(3) 0.037(3) -0.002(2) -0.004(2) -0.007(2) C10 0.037(2) 0.039(3) 0.038(3) 0.001(2) 0.004(2) -0.002(2) C11 0.037(2) 0.037(3) 0.038(3) -0.004(2) 0.006(2) -0.004(2) C12 0.039(3) 0.065(4) 0.049(3) -0.009(3) 0.009(2) -0.013(3) C13 0.042(3) 0.063(4) 0.076(4) -0.014(3) 0.019(3) -0.013(3) C14 0.058(3) 0.058(4) 0.057(4) -0.009(3) 0.029(3) -0.010(3) C15 0.054(3) 0.053(4) 0.040(3) -0.003(3) 0.013(2) -0.003(3) C16 0.046(3) 0.040(3) 0.033(3) -0.001(2) -0.004(2) -0.009(2) C17 0.046(3) 0.060(4) 0.039(3) -0.006(3) -0.004(2) -0.002(3) C18 0.065(4) 0.066(4) 0.045(3) -0.013(3) 0.009(3) -0.001(3) C19 0.066(4) 0.059(4) 0.032(3) -0.001(3) -0.003(3) -0.008(3) C20 0.049(3) 0.061(4) 0.042(3) 0.006(3) -0.009(2) -0.005(3) C21 0.051(3) 0.056(4) 0.038(3) 0.000(3) 0.006(2) 0.000(3) C22 0.048(3) 0.055(4) 0.050(3) 0.010(3) -0.003(2) 0.002(3) C23 0.052(3) 0.050(4) 0.062(4) 0.010(3) -0.002(3) 0.012(3) C24 0.047(3) 0.045(3) 0.077(4) -0.001(3) 0.008(3) 0.009(3) C25 0.050(3) 0.044(3) 0.049(3) -0.006(3) 0.007(2) 0.003(2) C26 0.031(2) 0.037(3) 0.038(3) -0.002(2) 0.0050(19) -0.0024(19) C27 0.033(2) 0.037(3) 0.037(3) 0.001(2) 0.0080(19) 0.001(2) C28 0.046(3) 0.038(3) 0.037(3) -0.006(2) 0.006(2) -0.003(2) C29 0.041(3) 0.039(3) 0.033(3) 0.004(2) 0.007(2) -0.006(2) C30 0.044(3) 0.043(3) 0.034(3) 0.001(2) -0.002(2) 0.002(2) C31 0.035(2) 0.035(3) 0.037(3) 0.004(2) 0.0045(19) -0.002(2) C32 0.036(2) 0.036(3) 0.039(3) 0.001(2) 0.005(2) -0.003(2) C33 0.053(3) 0.044(3) 0.046(3) 0.003(3) 0.006(2) 0.006(3) C34 0.063(4) 0.048(3) 0.064(4) -0.008(3) 0.005(3) 0.014(3) C35 0.064(4) 0.039(3) 0.067(4) -0.016(3) 0.014(3) 0.005(3) C36 0.054(3) 0.054(4) 0.043(3) -0.014(3) 0.002(2) -0.004(3) C37 0.051(3) 0.038(3) 0.038(3) 0.002(2) 0.006(2) -0.009(2) C38 0.058(3) 0.052(4) 0.047(3) -0.004(3) 0.004(3) 0.008(3) C39 0.068(4) 0.071(4) 0.041(3) 0.000(3) -0.011(3) -0.001(3) C40 0.082(5) 0.087(5) 0.036(3) 0.002(3) -0.003(3) 0.000(4) C41 0.091(5) 0.121(6) 0.038(4) -0.003(4) 0.016(3) 0.013(5) C42 0.062(4) 0.078(4) 0.040(3) 0.006(3) 0.012(3) 0.004(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Zn1 N2 2.069(4) . ? Zn1 N5 2.091(4) . ? Zn1 N4 2.178(4) . ? Zn1 N1 2.192(4) . ? Zn1 N3 2.193(4) . ? Zn1 N6 2.217(4) . ? Cl1 O12 1.310(6) . ? Cl1 O14 1.397(7) . ? Cl1 O11 1.444(6) . ? Cl1 O13 1.474(7) . ? Cl2 O21 1.285(7) . ? Cl2 O23 1.289(10) . ? Cl2 O24 1.328(8) . ? Cl2 O22 1.358(6) . ? N1 C15 1.335(6) . ? N1 C11 1.349(6) . ? N2 C6 1.334(6) . ? N2 C10 1.341(6) . ? N3 C1 1.346(6) . ? N3 C5 1.348(6) . ? N4 C22 1.332(6) . ? N4 C26 1.347(6) . ? N5 C27 1.329(6) . ? N5 C31 1.344(6) . ? N6 C36 1.330(6) . ? N6 C32 1.355(6) . ? C1 C2 1.378(8) . ? C1 H1 0.9300 . ? C2 C3 1.351(8) . ? C2 H2 0.9300 . ? C3 C4 1.393(8) . ? C3 H3 0.9300 . ? C4 C5 1.360(7) . ? C4 H4 0.9300 . ? C5 C6 1.490(6) . ? C6 C7 1.373(6) . ? C8 C9 1.388(7) . ? C8 C7 1.401(7) . ? C8 C16 1.475(6) . ? C7 H7 0.9300 . ? C9 C10 1.383(6) . ? C9 H9 0.9300 . ? C10 C11 1.489(6) . ? C11 C12 1.372(7) . ? C12 C13 1.368(7) . ? C12 H12 0.9300 . ? C13 C14 1.369(8) . ? C13 H13 0.9300 . ? C14 C15 1.377(7) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C21 1.384(7) . ? C16 C17 1.384(7) . ? C17 C18 1.385(7) . ? C17 H17 0.9300 . ? C18 C19 1.377(8) . ? C18 H18 0.9300 . ? C19 C20 1.379(8) . ? C19 H19 0.9300 . ? C20 C21 1.382(7) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.352(8) . ? C22 H22 0.9300 . ? C23 C24 1.376(8) . ? C23 H23 0.9300 . ? C24 C25 1.387(7) . ? C24 H24 0.9300 . ? C25 C26 1.371(7) . ? C25 H25 0.9300 . ? C26 C27 1.494(7) . ? C27 C28 1.393(7) . ? C28 C29 1.385(7) . ? C28 H28 0.9300 . ? C29 C30 1.399(7) . ? C29 C37 1.469(7) . ? C30 C31 1.375(6) . ? C30 H30 0.9300 . ? C31 C32 1.485(7) . ? C32 C33 1.371(7) . ? C33 C34 1.382(8) . ? C33 H33 0.9300 . ? C34 C35 1.355(8) . ? C34 H34 0.9300 . ? C35 C36 1.382(8) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C42 1.385(7) . ? C37 C38 1.399(7) . ? C38 C39 1.379(8) . ? C38 H38 0.9300 . ? C39 C40 1.362(9) . ? C39 H39 0.9300 . ? C40 C41 1.363(9) . ? C40 H40 0.9300 . ? C41 C42 1.387(8) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Zn1 N5 173.22(15) . . ? N2 Zn1 N4 111.42(15) . . ? N5 Zn1 N4 75.34(15) . . ? N2 Zn1 N1 75.49(14) . . ? N5 Zn1 N1 104.94(14) . . ? N4 Zn1 N1 87.91(15) . . ? N2 Zn1 N3 75.44(14) . . ? N5 Zn1 N3 104.51(14) . . ? N4 Zn1 N3 98.18(15) . . ? N1 Zn1 N3 150.52(14) . . ? N2 Zn1 N6 98.35(15) . . ? N5 Zn1 N6 74.87(15) . . ? N4 Zn1 N6 150.17(15) . . ? N1 Zn1 N6 98.16(15) . . ? N3 Zn1 N6 90.79(15) . . ? O12 Cl1 O14 124.5(6) . . ? O12 Cl1 O11 111.7(5) . . ? O14 Cl1 O11 112.9(4) . . ? O12 Cl1 O13 100.0(6) . . ? O14 Cl1 O13 98.5(5) . . ? O11 Cl1 O13 105.3(4) . . ? O21 Cl2 O23 103.1(10) . . ? O21 Cl2 O24 107.5(8) . . ? O23 Cl2 O24 109.0(9) . . ? O21 Cl2 O22 113.0(6) . . ? O23 Cl2 O22 112.5(8) . . ? O24 Cl2 O22 111.3(5) . . ? C15 N1 C11 118.6(4) . . ? C15 N1 Zn1 125.8(3) . . ? C11 N1 Zn1 115.0(3) . . ? C6 N2 C10 120.1(4) . . ? C6 N2 Zn1 119.7(3) . . ? C10 N2 Zn1 120.0(3) . . ? C1 N3 C5 118.4(4) . . ? C1 N3 Zn1 126.5(3) . . ? C5 N3 Zn1 115.0(3) . . ? C22 N4 C26 117.9(4) . . ? C22 N4 Zn1 125.8(4) . . ? C26 N4 Zn1 115.9(3) . . ? C27 N5 C31 120.6(4) . . ? C27 N5 Zn1 119.3(3) . . ? C31 N5 Zn1 120.0(3) . . ? C36 N6 C32 118.4(4) . . ? C36 N6 Zn1 126.1(4) . . ? C32 N6 Zn1 114.9(3) . . ? N3 C1 C2 121.8(5) . . ? N3 C1 H1 119.1 . . ? C2 C1 H1 119.1 . . ? C3 C2 C1 119.8(5) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 118.4(5) . . ? C2 C3 H3 120.8 . . ? C4 C3 H3 120.8 . . ? C5 C4 C3 119.9(5) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? N3 C5 C4 121.5(4) . . ? N3 C5 C6 114.7(4) . . ? C4 C5 C6 123.8(5) . . ? N2 C6 C7 121.3(4) . . ? N2 C6 C5 114.5(4) . . ? C7 C6 C5 124.2(4) . . ? C9 C8 C7 117.2(4) . . ? C9 C8 C16 122.0(4) . . ? C7 C8 C16 120.7(4) . . ? C6 C7 C8 120.2(4) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C10 C9 C8 119.9(4) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? N2 C10 C9 121.3(4) . . ? N2 C10 C11 114.1(4) . . ? C9 C10 C11 124.6(4) . . ? N1 C11 C12 121.7(4) . . ? N1 C11 C10 114.9(4) . . ? C12 C11 C10 123.3(4) . . ? C13 C12 C11 119.0(5) . . ? C13 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C12 C13 C14 119.9(5) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C13 C14 C15 118.7(5) . . ? C13 C14 H14 120.7 . . ? C15 C14 H14 120.7 . . ? N1 C15 C14 122.1(5) . . ? N1 C15 H15 118.9 . . ? C14 C15 H15 118.9 . . ? C21 C16 C17 118.9(5) . . ? C21 C16 C8 120.1(5) . . ? C17 C16 C8 120.9(4) . . ? C16 C17 C18 120.2(5) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C19 C18 C17 120.6(5) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C18 C19 C20 119.3(5) . . ? C18 C19 H19 120.4 . . ? C20 C19 H19 120.4 . . ? C19 C20 C21 120.3(5) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C20 C21 C16 120.7(5) . . ? C20 C21 H21 119.7 . . ? C16 C21 H21 119.7 . . ? N4 C22 C23 123.6(5) . . ? N4 C22 H22 118.2 . . ? C23 C22 H22 118.2 . . ? C22 C23 C24 118.9(5) . . ? C22 C23 H23 120.5 . . ? C24 C23 H23 120.5 . . ? C23 C24 C25 118.6(5) . . ? C23 C24 H24 120.7 . . ? C25 C24 H24 120.7 . . ? C26 C25 C24 119.0(5) . . ? C26 C25 H25 120.5 . . ? C24 C25 H25 120.5 . . ? N4 C26 C25 121.9(4) . . ? N4 C26 C27 114.3(4) . . ? C25 C26 C27 123.7(4) . . ? N5 C27 C28 121.0(4) . . ? N5 C27 C26 114.9(4) . . ? C28 C27 C26 124.1(4) . . ? C29 C28 C27 120.1(5) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C28 C29 C30 116.9(4) . . ? C28 C29 C37 122.0(5) . . ? C30 C29 C37 121.0(4) . . ? C31 C30 C29 120.8(5) . . ? C31 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? N5 C31 C30 120.5(4) . . ? N5 C31 C32 114.7(4) . . ? C30 C31 C32 124.7(4) . . ? N6 C32 C33 121.0(5) . . ? N6 C32 C31 115.0(4) . . ? C33 C32 C31 123.9(4) . . ? C32 C33 C34 119.9(5) . . ? C32 C33 H33 120.1 . . ? C34 C33 H33 120.1 . . ? C35 C34 C33 119.0(5) . . ? C35 C34 H34 120.5 . . ? C33 C34 H34 120.5 . . ? C34 C35 C36 118.9(5) . . ? C34 C35 H35 120.5 . . ? C36 C35 H35 120.5 . . ? N6 C36 C35 122.7(5) . . ? N6 C36 H36 118.6 . . ? C35 C36 H36 118.6 . . ? C42 C37 C38 118.1(5) . . ? C42 C37 C29 121.1(5) . . ? C38 C37 C29 120.8(5) . . ? C39 C38 C37 120.4(5) . . ? C39 C38 H38 119.8 . . ? C37 C38 H38 119.8 . . ? C40 C39 C38 121.1(6) . . ? C40 C39 H39 119.5 . . ? C38 C39 H39 119.5 . . ? C39 C40 C41 118.9(6) . . ? C39 C40 H40 120.5 . . ? C41 C40 H40 120.5 . . ? C40 C41 C42 121.6(6) . . ? C40 C41 H41 119.2 . . ? C42 C41 H41 119.2 . . ? C37 C42 C41 119.8(6) . . ? C37 C42 H42 120.1 . . ? C41 C42 H42 120.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Zn1 N1 C15 -172.5(5) . . . . ? N5 Zn1 N1 C15 14.5(5) . . . . ? N4 Zn1 N1 C15 -59.8(4) . . . . ? N3 Zn1 N1 C15 -162.8(4) . . . . ? N6 Zn1 N1 C15 90.9(4) . . . . ? N2 Zn1 N1 C11 -1.4(3) . . . . ? N5 Zn1 N1 C11 -174.4(3) . . . . ? N4 Zn1 N1 C11 111.4(4) . . . . ? N3 Zn1 N1 C11 8.4(5) . . . . ? N6 Zn1 N1 C11 -98.0(4) . . . . ? N5 Zn1 N2 C6 -83.6(13) . . . . ? N4 Zn1 N2 C6 100.1(4) . . . . ? N1 Zn1 N2 C6 -178.1(4) . . . . ? N3 Zn1 N2 C6 6.9(4) . . . . ? N6 Zn1 N2 C6 -81.8(4) . . . . ? N5 Zn1 N2 C10 90.9(12) . . . . ? N4 Zn1 N2 C10 -85.4(4) . . . . ? N1 Zn1 N2 C10 -3.6(4) . . . . ? N3 Zn1 N2 C10 -178.7(4) . . . . ? N6 Zn1 N2 C10 92.7(4) . . . . ? N2 Zn1 N3 C1 176.8(4) . . . . ? N5 Zn1 N3 C1 -10.2(4) . . . . ? N4 Zn1 N3 C1 66.7(4) . . . . ? N1 Zn1 N3 C1 167.0(4) . . . . ? N6 Zn1 N3 C1 -84.7(4) . . . . ? N2 Zn1 N3 C5 -3.4(3) . . . . ? N5 Zn1 N3 C5 169.6(3) . . . . ? N4 Zn1 N3 C5 -113.5(4) . . . . ? N1 Zn1 N3 C5 -13.2(5) . . . . ? N6 Zn1 N3 C5 95.0(4) . . . . ? N2 Zn1 N4 C22 4.0(5) . . . . ? N5 Zn1 N4 C22 -175.6(4) . . . . ? N1 Zn1 N4 C22 -69.5(4) . . . . ? N3 Zn1 N4 C22 81.5(4) . . . . ? N6 Zn1 N4 C22 -172.4(4) . . . . ? N2 Zn1 N4 C26 176.8(3) . . . . ? N5 Zn1 N4 C26 -2.8(3) . . . . ? N1 Zn1 N4 C26 103.2(3) . . . . ? N3 Zn1 N4 C26 -105.7(3) . . . . ? N6 Zn1 N4 C26 0.4(5) . . . . ? N2 Zn1 N5 C27 -176.7(11) . . . . ? N4 Zn1 N5 C27 -0.2(3) . . . . ? N1 Zn1 N5 C27 -84.0(4) . . . . ? N3 Zn1 N5 C27 94.6(3) . . . . ? N6 Zn1 N5 C27 -178.6(4) . . . . ? N2 Zn1 N5 C31 7.1(14) . . . . ? N4 Zn1 N5 C31 -176.4(4) . . . . ? N1 Zn1 N5 C31 99.8(3) . . . . ? N3 Zn1 N5 C31 -81.6(3) . . . . ? N6 Zn1 N5 C31 5.2(3) . . . . ? N2 Zn1 N6 C36 2.7(4) . . . . ? N5 Zn1 N6 C36 -177.5(4) . . . . ? N4 Zn1 N6 C36 179.3(4) . . . . ? N1 Zn1 N6 C36 79.2(4) . . . . ? N3 Zn1 N6 C36 -72.7(4) . . . . ? N2 Zn1 N6 C32 173.7(3) . . . . ? N5 Zn1 N6 C32 -6.6(3) . . . . ? N4 Zn1 N6 C32 -9.8(5) . . . . ? N1 Zn1 N6 C32 -109.9(3) . . . . ? N3 Zn1 N6 C32 98.3(3) . . . . ? C5 N3 C1 C2 0.6(8) . . . . ? Zn1 N3 C1 C2 -179.6(4) . . . . ? N3 C1 C2 C3 1.0(9) . . . . ? C1 C2 C3 C4 -2.5(9) . . . . ? C2 C3 C4 C5 2.5(9) . . . . ? C1 N3 C5 C4 -0.6(8) . . . . ? Zn1 N3 C5 C4 179.6(4) . . . . ? C1 N3 C5 C6 179.8(4) . . . . ? Zn1 N3 C5 C6 0.0(5) . . . . ? C3 C4 C5 N3 -0.9(9) . . . . ? C3 C4 C5 C6 178.6(5) . . . . ? C10 N2 C6 C7 -1.5(7) . . . . ? Zn1 N2 C6 C7 172.9(4) . . . . ? C10 N2 C6 C5 176.5(4) . . . . ? Zn1 N2 C6 C5 -9.0(6) . . . . ? N3 C5 C6 N2 5.6(7) . . . . ? C4 C5 C6 N2 -174.0(5) . . . . ? N3 C5 C6 C7 -176.4(5) . . . . ? C4 C5 C6 C7 4.0(9) . . . . ? N2 C6 C7 C8 1.7(8) . . . . ? C5 C6 C7 C8 -176.1(5) . . . . ? C9 C8 C7 C6 -0.6(8) . . . . ? C16 C8 C7 C6 175.8(5) . . . . ? C7 C8 C9 C10 -0.8(8) . . . . ? C16 C8 C9 C10 -177.1(5) . . . . ? C6 N2 C10 C9 0.1(7) . . . . ? Zn1 N2 C10 C9 -174.3(4) . . . . ? C6 N2 C10 C11 -178.0(4) . . . . ? Zn1 N2 C10 C11 7.6(6) . . . . ? C8 C9 C10 N2 1.0(8) . . . . ? C8 C9 C10 C11 178.9(5) . . . . ? C15 N1 C11 C12 -1.3(7) . . . . ? Zn1 N1 C11 C12 -173.1(4) . . . . ? C15 N1 C11 C10 177.4(4) . . . . ? Zn1 N1 C11 C10 5.6(5) . . . . ? N2 C10 C11 N1 -8.5(6) . . . . ? C9 C10 C11 N1 173.5(5) . . . . ? N2 C10 C11 C12 170.1(5) . . . . ? C9 C10 C11 C12 -7.9(8) . . . . ? N1 C11 C12 C13 0.9(8) . . . . ? C10 C11 C12 C13 -177.7(5) . . . . ? C11 C12 C13 C14 0.0(9) . . . . ? C12 C13 C14 C15 -0.4(9) . . . . ? C11 N1 C15 C14 0.8(8) . . . . ? Zn1 N1 C15 C14 171.7(4) . . . . ? C13 C14 C15 N1 0.0(9) . . . . ? C9 C8 C16 C21 42.6(7) . . . . ? C7 C8 C16 C21 -133.6(5) . . . . ? C9 C8 C16 C17 -139.8(5) . . . . ? C7 C8 C16 C17 44.0(8) . . . . ? C21 C16 C17 C18 0.2(8) . . . . ? C8 C16 C17 C18 -177.5(5) . . . . ? C16 C17 C18 C19 0.7(9) . . . . ? C17 C18 C19 C20 -0.6(9) . . . . ? C18 C19 C20 C21 -0.5(9) . . . . ? C19 C20 C21 C16 1.4(9) . . . . ? C17 C16 C21 C20 -1.2(8) . . . . ? C8 C16 C21 C20 176.5(5) . . . . ? C26 N4 C22 C23 0.0(8) . . . . ? Zn1 N4 C22 C23 172.6(4) . . . . ? N4 C22 C23 C24 -0.7(9) . . . . ? C22 C23 C24 C25 0.5(8) . . . . ? C23 C24 C25 C26 0.3(8) . . . . ? C22 N4 C26 C25 0.9(7) . . . . ? Zn1 N4 C26 C25 -172.5(4) . . . . ? C22 N4 C26 C27 178.4(4) . . . . ? Zn1 N4 C26 C27 5.0(5) . . . . ? C24 C25 C26 N4 -1.1(8) . . . . ? C24 C25 C26 C27 -178.3(5) . . . . ? C31 N5 C27 C28 1.0(7) . . . . ? Zn1 N5 C27 C28 -175.2(3) . . . . ? C31 N5 C27 C26 179.1(4) . . . . ? Zn1 N5 C27 C26 2.9(5) . . . . ? N4 C26 C27 N5 -5.2(6) . . . . ? C25 C26 C27 N5 172.2(4) . . . . ? N4 C26 C27 C28 172.8(4) . . . . ? C25 C26 C27 C28 -9.7(7) . . . . ? N5 C27 C28 C29 0.7(7) . . . . ? C26 C27 C28 C29 -177.2(4) . . . . ? C27 C28 C29 C30 -2.1(7) . . . . ? C27 C28 C29 C37 175.2(4) . . . . ? C28 C29 C30 C31 2.0(7) . . . . ? C37 C29 C30 C31 -175.3(4) . . . . ? C27 N5 C31 C30 -1.0(7) . . . . ? Zn1 N5 C31 C30 175.1(3) . . . . ? C27 N5 C31 C32 -179.4(4) . . . . ? Zn1 N5 C31 C32 -3.3(5) . . . . ? C29 C30 C31 N5 -0.5(7) . . . . ? C29 C30 C31 C32 177.7(4) . . . . ? C36 N6 C32 C33 0.6(7) . . . . ? Zn1 N6 C32 C33 -171.1(4) . . . . ? C36 N6 C32 C31 178.7(4) . . . . ? Zn1 N6 C32 C31 7.0(5) . . . . ? N5 C31 C32 N6 -2.8(6) . . . . ? C30 C31 C32 N6 178.9(4) . . . . ? N5 C31 C32 C33 175.2(4) . . . . ? C30 C31 C32 C33 -3.1(8) . . . . ? N6 C32 C33 C34 -0.7(8) . . . . ? C31 C32 C33 C34 -178.6(5) . . . . ? C32 C33 C34 C35 0.5(9) . . . . ? C33 C34 C35 C36 -0.3(9) . . . . ? C32 N6 C36 C35 -0.3(8) . . . . ? Zn1 N6 C36 C35 170.3(4) . . . . ? C34 C35 C36 N6 0.2(9) . . . . ? C28 C29 C37 C42 32.6(7) . . . . ? C30 C29 C37 C42 -150.2(5) . . . . ? C28 C29 C37 C38 -146.0(5) . . . . ? C30 C29 C37 C38 31.2(7) . . . . ? C42 C37 C38 C39 -0.5(8) . . . . ? C29 C37 C38 C39 178.1(5) . . . . ? C37 C38 C39 C40 1.9(10) . . . . ? C38 C39 C40 C41 -3.2(11) . . . . ? C39 C40 C41 C42 3.2(12) . . . . ? C38 C37 C42 C41 0.5(9) . . . . ? C29 C37 C42 C41 -178.1(6) . . . . ? C40 C41 C42 C37 -1.9(11) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.548 _refine_diff_density_min -0.557 _refine_diff_density_rms 0.087 # Attachment '- complex_6.cif' data_6 _database_code_depnum_ccdc_archive 'CCDC 829881' #TrackingRef '- complex_6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H46 F12 Fe2 N6 P2 Zn' _chemical_formula_sum 'C46 H46 F12 Fe2 N6 P2 Zn' _chemical_formula_weight 1149.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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 orthorhombic _symmetry_space_group_name_H-M pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 21.776(2) _cell_length_b 11.5108(11) _cell_length_c 19.0161(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4766.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.602 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2336 _exptl_absorpt_coefficient_mu 1.255 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7202 _exptl_absorpt_correction_T_max 0.8439 _exptl_absorpt_process_details SADABS(Sheldrick,1997) _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 Smart CCD Area Detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39648 _diffrn_reflns_av_R_equivalents 0.0894 _diffrn_reflns_av_sigmaI/netI 0.0683 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 28.35 _reflns_number_total 5798 _reflns_number_gt 3231 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Smart' _computing_data_reduction 'Bruker Saint' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0952P)^2^+6.2663P] 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 5798 _refine_ls_number_parameters 305 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1420 _refine_ls_R_factor_gt 0.0716 _refine_ls_wR_factor_ref 0.2071 _refine_ls_wR_factor_gt 0.1700 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.002 _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 Zn1 Zn 0.5000 0.11975(7) 0.2500 0.0393(2) Uani 1 2 d S . . Fe1 Fe 0.33117(3) -0.22840(7) 0.42918(4) 0.0496(3) Uani 1 1 d . . . N1 N 0.58910(18) 0.0751(4) 0.2947(2) 0.0438(10) Uani 1 1 d . . . N2 N 0.48045(17) 0.0039(3) 0.3472(2) 0.0364(9) Uani 1 1 d . . . N3 N 0.4633(2) 0.2407(3) 0.3227(2) 0.0449(10) Uani 1 1 d . . . P1 P 0.61355(8) 0.57098(18) 0.35122(10) 0.0709(5) Uani 1 1 d . . . F1 F 0.6511(2) 0.4896(5) 0.3000(3) 0.144(2) Uani 1 1 d . . . F2 F 0.5704(4) 0.4751(7) 0.3713(5) 0.226(4) Uani 1 1 d . . . F3 F 0.5712(4) 0.5998(8) 0.2917(3) 0.233(5) Uani 1 1 d . . . F4 F 0.5800(3) 0.6631(5) 0.3968(3) 0.1290(19) Uani 1 1 d . . . F5 F 0.6537(3) 0.5289(7) 0.4138(3) 0.169(3) Uani 1 1 d . . . F6 F 0.6636(4) 0.6593(6) 0.3364(5) 0.215(4) Uani 1 1 d . . . C1 C 0.2911(3) -0.3494(7) 0.3670(5) 0.095(3) Uani 1 1 d . . . H1 H 0.3114 -0.4118 0.3464 0.114 Uiso 1 1 calc R . . C2 C 0.2821(5) -0.2425(10) 0.3373(5) 0.105(2) Uani 1 1 d . . . H2 H 0.2952 -0.2190 0.2930 0.126 Uiso 1 1 calc R . . C3 C 0.2526(5) -0.1819(8) 0.3810(6) 0.104(2) Uani 1 1 d . . . H3 H 0.2403 -0.1060 0.3719 0.124 Uiso 1 1 calc R . . C4 C 0.2640(5) -0.3480(8) 0.4351(5) 0.112(2) Uani 1 1 d . . . H4 H 0.2625 -0.4083 0.4677 0.135 Uiso 1 1 calc R . . C5 C 0.2405(4) -0.2368(9) 0.4421(6) 0.1034(15) Uani 1 1 d . . . H5 H 0.2203 -0.2062 0.4810 0.124 Uiso 1 1 calc R . . C6 C 0.4242(3) -0.2421(5) 0.4270(3) 0.0601(16) Uani 1 1 d . . . H6 H 0.4471 -0.2889 0.3970 0.072 Uiso 1 1 calc R . . C7 C 0.4022(3) -0.2745(7) 0.4926(4) 0.079(2) Uani 1 1 d . . . H7 H 0.4081 -0.3464 0.5139 0.095 Uiso 1 1 calc R . . C8 C 0.3695(4) -0.1801(7) 0.5216(3) 0.083(2) Uani 1 1 d . . . H8 H 0.3495 -0.1789 0.5648 0.100 Uiso 1 1 calc R . . C9 C 0.3725(3) -0.0875(6) 0.4727(3) 0.0614(16) Uani 1 1 d . . . H9 H 0.3553 -0.0142 0.4786 0.074 Uiso 1 1 calc R . . C10 C 0.4061(2) -0.1252(4) 0.4131(3) 0.0408(11) Uani 1 1 d . . . C11 C 0.4194(2) -0.0561(4) 0.3489(3) 0.0408(11) Uani 1 1 d . . . H11A H 0.3875 0.0022 0.3438 0.049 Uiso 1 1 calc R . . H11B H 0.4168 -0.1073 0.3085 0.049 Uiso 1 1 calc R . . C12 C 0.4860(2) 0.0873(4) 0.4061(3) 0.0409(11) Uani 1 1 d . . . H12A H 0.5291 0.0962 0.4179 0.049 Uiso 1 1 calc R . . H12B H 0.4653 0.0556 0.4469 0.049 Uiso 1 1 calc R . . C13 C 0.4596(2) 0.2043(4) 0.3900(2) 0.0399(11) Uani 1 1 d . . . C14 C 0.4365(3) 0.2755(5) 0.4410(3) 0.0585(15) Uani 1 1 d . . . H14 H 0.4334 0.2489 0.4870 0.070 Uiso 1 1 calc R . . C15 C 0.4179(3) 0.3858(6) 0.4245(4) 0.075(2) Uani 1 1 d . . . H15 H 0.4035 0.4354 0.4594 0.090 Uiso 1 1 calc R . . C16 C 0.4207(3) 0.4222(5) 0.3564(4) 0.0660(17) Uani 1 1 d . . . H16 H 0.4076 0.4962 0.3437 0.079 Uiso 1 1 calc R . . C17 C 0.4431(3) 0.3475(5) 0.3076(3) 0.0586(15) Uani 1 1 d . . . H17 H 0.4445 0.3719 0.2610 0.070 Uiso 1 1 calc R . . C18 C 0.6422(3) 0.1293(5) 0.2793(3) 0.0567(15) Uani 1 1 d . . . H18 H 0.6409 0.1984 0.2539 0.068 Uiso 1 1 calc R . . C19 C 0.6984(3) 0.0863(7) 0.2995(3) 0.0716(19) Uani 1 1 d . . . H19 H 0.7344 0.1242 0.2866 0.086 Uiso 1 1 calc R . . C20 C 0.7006(3) -0.0125(6) 0.3387(4) 0.0721(19) Uani 1 1 d . . . H20 H 0.7381 -0.0421 0.3535 0.087 Uiso 1 1 calc R . . C21 C 0.6465(3) -0.0684(5) 0.3562(3) 0.0570(15) Uani 1 1 d . . . H21 H 0.6472 -0.1359 0.3831 0.068 Uiso 1 1 calc R . . C22 C 0.5915(2) -0.0222(4) 0.3331(3) 0.0418(11) Uani 1 1 d . . . C23 C 0.5316(2) -0.0796(4) 0.3504(3) 0.0417(11) Uani 1 1 d . . . H23A H 0.5241 -0.1423 0.3174 0.050 Uiso 1 1 calc R . . H23B H 0.5338 -0.1128 0.3972 0.050 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 Zn1 0.0480(5) 0.0365(4) 0.0335(4) 0.000 0.0003(4) 0.000 Fe1 0.0444(4) 0.0438(4) 0.0605(5) -0.0032(4) 0.0038(4) -0.0100(3) N1 0.043(2) 0.056(3) 0.033(2) 0.001(2) 0.0027(18) -0.008(2) N2 0.041(2) 0.034(2) 0.035(2) 0.0034(17) -0.0025(17) -0.0053(17) N3 0.060(3) 0.035(2) 0.040(2) -0.0004(19) -0.003(2) 0.000(2) P1 0.0616(10) 0.0780(12) 0.0732(12) -0.0128(10) 0.0044(9) 0.0004(9) F1 0.105(4) 0.171(5) 0.156(5) -0.085(4) -0.008(3) 0.032(4) F2 0.146(6) 0.187(7) 0.343(12) 0.080(8) 0.007(7) -0.069(5) F3 0.227(8) 0.362(12) 0.112(5) -0.051(6) -0.057(5) 0.198(8) F4 0.140(4) 0.135(4) 0.112(4) -0.028(3) 0.033(3) 0.045(4) F5 0.141(5) 0.252(8) 0.115(4) -0.007(5) -0.034(4) 0.059(5) F6 0.200(7) 0.109(5) 0.335(11) -0.053(6) 0.151(7) -0.052(5) C1 0.063(4) 0.062(5) 0.159(9) -0.045(5) -0.039(5) 0.002(4) C2 0.110(7) 0.121 0.084 -0.003(6) -0.028(5) -0.050(6) C3 0.105(7) 0.077(5) 0.129 -0.014(6) -0.049(6) 0.000(5) C4 0.127(7) 0.102 0.108 0.040(5) -0.027(6) -0.080(5) C5 0.068(4) 0.120 0.122 -0.063(5) 0.021(5) -0.008(5) C6 0.041(3) 0.059(4) 0.081(4) 0.020(3) -0.004(3) -0.004(3) C7 0.079(5) 0.080(5) 0.078(5) 0.041(4) -0.024(4) -0.035(4) C8 0.105(6) 0.095(6) 0.049(4) 0.002(4) 0.006(4) -0.056(5) C9 0.065(4) 0.063(4) 0.056(4) -0.012(3) 0.011(3) -0.024(3) C10 0.038(2) 0.038(3) 0.047(3) -0.001(2) 0.001(2) -0.007(2) C11 0.040(3) 0.042(3) 0.040(3) 0.006(2) -0.003(2) -0.005(2) C12 0.046(3) 0.042(3) 0.035(3) 0.005(2) 0.002(2) -0.006(2) C13 0.038(3) 0.045(3) 0.037(3) -0.003(2) 0.002(2) -0.007(2) C14 0.062(4) 0.067(4) 0.046(3) -0.013(3) 0.006(3) 0.004(3) C15 0.078(5) 0.067(4) 0.079(5) -0.028(4) 0.008(4) 0.020(4) C16 0.074(4) 0.047(3) 0.077(5) -0.007(3) -0.001(3) 0.014(3) C17 0.075(4) 0.048(3) 0.053(3) 0.006(3) 0.001(3) 0.013(3) C18 0.058(4) 0.069(4) 0.043(3) 0.010(3) 0.000(3) -0.019(3) C19 0.043(3) 0.109(6) 0.063(4) 0.010(4) 0.003(3) -0.016(3) C20 0.041(3) 0.094(5) 0.082(5) 0.008(4) -0.005(3) 0.006(3) C21 0.050(3) 0.055(3) 0.066(4) 0.008(3) -0.005(3) 0.007(3) C22 0.045(3) 0.043(3) 0.037(3) -0.001(2) 0.000(2) -0.002(2) C23 0.045(3) 0.038(3) 0.043(3) 0.007(2) 0.001(2) -0.001(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 Zn1 N3 2.118(4) 4_655 ? Zn1 N3 2.118(4) . ? Zn1 N1 2.180(4) . ? Zn1 N1 2.180(4) 4_655 ? Zn1 N2 2.318(4) 4_655 ? Zn1 N2 2.318(4) . ? Fe1 C5 1.993(8) . ? Fe1 C4 2.012(7) . ? Fe1 C3 2.014(9) . ? Fe1 C8 2.022(7) . ? Fe1 C1 2.024(7) . ? Fe1 C9 2.030(6) . ? Fe1 C7 2.033(7) . ? Fe1 C6 2.033(6) . ? Fe1 C10 2.041(5) . ? Fe1 C2 2.055(8) . ? N1 C22 1.337(6) . ? N1 C18 1.347(6) . ? N2 C23 1.472(6) . ? N2 C12 1.480(6) . ? N2 C11 1.499(6) . ? N3 C17 1.337(6) . ? N3 C13 1.349(6) . ? P1 F3 1.496(6) . ? P1 F2 1.499(6) . ? P1 F6 1.517(6) . ? P1 F4 1.552(5) . ? P1 F5 1.554(6) . ? P1 F1 1.578(5) . ? C1 C2 1.368(11) . ? C1 C4 1.424(12) . ? C1 H1 0.9300 . ? C2 C3 1.261(12) . ? C2 H2 0.9300 . ? C3 C5 1.349(12) . ? C3 H3 0.9300 . ? C4 C5 1.386(12) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.388(9) . ? C6 C10 1.427(7) . ? C6 H6 0.9300 . ? C7 C8 1.412(11) . ? C7 H7 0.9300 . ? C8 C9 1.416(9) . ? C8 H8 0.9300 . ? C9 C10 1.417(7) . ? C9 H9 0.9300 . ? C10 C11 1.486(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.496(7) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.366(7) . ? C14 C15 1.370(8) . ? C14 H14 0.9300 . ? C15 C16 1.362(9) . ? C15 H15 0.9300 . ? C16 C17 1.356(8) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.375(8) . ? C18 H18 0.9300 . ? C19 C20 1.359(9) . ? C19 H19 0.9300 . ? C20 C21 1.382(8) . ? C20 H20 0.9300 . ? C21 C22 1.383(7) . ? C21 H21 0.9300 . ? C22 C23 1.500(7) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? 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 N3 Zn1 N3 97.8(2) 4_655 . ? N3 Zn1 N1 94.22(16) 4_655 . ? N3 Zn1 N1 103.67(16) . . ? N3 Zn1 N1 103.67(16) 4_655 4_655 ? N3 Zn1 N1 94.22(16) . 4_655 ? N1 Zn1 N1 152.7(2) . 4_655 ? N3 Zn1 N2 77.80(15) 4_655 4_655 ? N3 Zn1 N2 165.33(15) . 4_655 ? N1 Zn1 N2 90.68(14) . 4_655 ? N1 Zn1 N2 73.56(14) 4_655 4_655 ? N3 Zn1 N2 165.33(15) 4_655 . ? N3 Zn1 N2 77.80(15) . . ? N1 Zn1 N2 73.56(14) . . ? N1 Zn1 N2 90.68(14) 4_655 . ? N2 Zn1 N2 109.77(19) 4_655 . ? C5 Fe1 C4 40.5(4) . . ? C5 Fe1 C3 39.3(4) . . ? C4 Fe1 C3 65.8(4) . . ? C5 Fe1 C8 108.4(4) . . ? C4 Fe1 C8 116.0(3) . . ? C3 Fe1 C8 132.3(4) . . ? C5 Fe1 C1 67.1(3) . . ? C4 Fe1 C1 41.3(3) . . ? C3 Fe1 C1 63.3(3) . . ? C8 Fe1 C1 150.9(4) . . ? C5 Fe1 C9 115.3(3) . . ? C4 Fe1 C9 147.8(4) . . ? C3 Fe1 C9 110.5(3) . . ? C8 Fe1 C9 40.9(3) . . ? C1 Fe1 C9 168.0(4) . . ? C5 Fe1 C7 132.0(4) . . ? C4 Fe1 C7 110.0(3) . . ? C3 Fe1 C7 170.6(4) . . ? C8 Fe1 C7 40.8(3) . . ? C1 Fe1 C7 119.7(3) . . ? C9 Fe1 C7 68.3(3) . . ? C5 Fe1 C6 170.7(4) . . ? C4 Fe1 C6 132.3(4) . . ? C3 Fe1 C6 149.1(4) . . ? C8 Fe1 C6 68.2(3) . . ? C1 Fe1 C6 111.4(3) . . ? C9 Fe1 C6 68.2(3) . . ? C7 Fe1 C6 39.9(3) . . ? C5 Fe1 C10 147.0(3) . . ? C4 Fe1 C10 171.0(4) . . ? C3 Fe1 C10 117.2(3) . . ? C8 Fe1 C10 68.9(2) . . ? C1 Fe1 C10 131.1(3) . . ? C9 Fe1 C10 40.7(2) . . ? C7 Fe1 C10 68.4(2) . . ? C6 Fe1 C10 41.0(2) . . ? C5 Fe1 C2 65.5(4) . . ? C4 Fe1 C2 67.4(3) . . ? C3 Fe1 C2 36.1(3) . . ? C8 Fe1 C2 167.1(5) . . ? C1 Fe1 C2 39.2(3) . . ? C9 Fe1 C2 129.8(4) . . ? C7 Fe1 C2 151.7(4) . . ? C6 Fe1 C2 119.7(4) . . ? C10 Fe1 C2 109.6(3) . . ? C22 N1 C18 118.2(5) . . ? C22 N1 Zn1 116.4(3) . . ? C18 N1 Zn1 124.8(4) . . ? C23 N2 C12 109.3(4) . . ? C23 N2 C11 111.7(4) . . ? C12 N2 C11 110.8(4) . . ? C23 N2 Zn1 105.7(3) . . ? C12 N2 Zn1 102.4(3) . . ? C11 N2 Zn1 116.4(3) . . ? C17 N3 C13 118.0(5) . . ? C17 N3 Zn1 126.1(4) . . ? C13 N3 Zn1 115.9(3) . . ? F3 P1 F2 88.3(5) . . ? F3 P1 F6 98.9(6) . . ? F2 P1 F6 172.4(6) . . ? F3 P1 F4 88.9(3) . . ? F2 P1 F4 93.8(4) . . ? F6 P1 F4 89.1(4) . . ? F3 P1 F5 174.0(5) . . ? F2 P1 F5 85.9(5) . . ? F6 P1 F5 87.0(5) . . ? F4 P1 F5 92.9(3) . . ? F3 P1 F1 89.1(3) . . ? F2 P1 F1 92.6(5) . . ? F6 P1 F1 84.9(3) . . ? F4 P1 F1 173.3(4) . . ? F5 P1 F1 89.8(4) . . ? C2 C1 C4 107.8(8) . . ? C2 C1 Fe1 71.6(4) . . ? C4 C1 Fe1 68.9(4) . . ? C2 C1 H1 126.1 . . ? C4 C1 H1 126.1 . . ? Fe1 C1 H1 125.0 . . ? C3 C2 C1 107.4(9) . . ? C3 C2 Fe1 70.2(5) . . ? C1 C2 Fe1 69.2(5) . . ? C3 C2 H2 126.3 . . ? C1 C2 H2 126.3 . . ? Fe1 C2 H2 125.9 . . ? C2 C3 C5 114.0(9) . . ? C2 C3 Fe1 73.7(6) . . ? C5 C3 Fe1 69.5(5) . . ? C2 C3 H3 123.0 . . ? C5 C3 H3 123.0 . . ? Fe1 C3 H3 125.4 . . ? C5 C4 C1 104.5(8) . . ? C5 C4 Fe1 69.0(4) . . ? C1 C4 Fe1 69.8(4) . . ? C5 C4 H4 127.7 . . ? C1 C4 H4 127.7 . . ? Fe1 C4 H4 125.0 . . ? C3 C5 C4 106.2(8) . . ? C3 C5 Fe1 71.2(5) . . ? C4 C5 Fe1 70.5(5) . . ? C3 C5 H5 126.9 . . ? C4 C5 H5 126.9 . . ? Fe1 C5 H5 123.1 . . ? C7 C6 C10 108.9(6) . . ? C7 C6 Fe1 70.0(4) . . ? C10 C6 Fe1 69.8(3) . . ? C7 C6 H6 125.5 . . ? C10 C6 H6 125.5 . . ? Fe1 C6 H6 126.3 . . ? C6 C7 C8 108.5(6) . . ? C6 C7 Fe1 70.1(3) . . ? C8 C7 Fe1 69.2(4) . . ? C6 C7 H7 125.7 . . ? C8 C7 H7 125.7 . . ? Fe1 C7 H7 126.5 . . ? C7 C8 C9 107.4(6) . . ? C7 C8 Fe1 70.0(4) . . ? C9 C8 Fe1 69.9(4) . . ? C7 C8 H8 126.3 . . ? C9 C8 H8 126.3 . . ? Fe1 C8 H8 125.4 . . ? C8 C9 C10 108.6(6) . . ? C8 C9 Fe1 69.3(4) . . ? C10 C9 Fe1 70.0(3) . . ? C8 C9 H9 125.7 . . ? C10 C9 H9 125.7 . . ? Fe1 C9 H9 126.6 . . ? C9 C10 C6 106.5(5) . . ? C9 C10 C11 126.4(5) . . ? C6 C10 C11 127.1(5) . . ? C9 C10 Fe1 69.2(3) . . ? C6 C10 Fe1 69.2(3) . . ? C11 C10 Fe1 126.2(3) . . ? C10 C11 N2 115.9(4) . . ? C10 C11 H11A 108.3 . . ? N2 C11 H11A 108.3 . . ? C10 C11 H11B 108.3 . . ? N2 C11 H11B 108.3 . . ? H11A C11 H11B 107.4 . . ? N2 C12 C13 113.4(4) . . ? N2 C12 H12A 108.9 . . ? C13 C12 H12A 108.9 . . ? N2 C12 H12B 108.9 . . ? C13 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? N3 C13 C14 120.6(5) . . ? N3 C13 C12 116.8(4) . . ? C14 C13 C12 122.4(5) . . ? C13 C14 C15 120.1(6) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C16 C15 C14 119.4(6) . . ? C16 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? C17 C16 C15 118.1(6) . . ? C17 C16 H16 121.0 . . ? C15 C16 H16 121.0 . . ? N3 C17 C16 123.7(6) . . ? N3 C17 H17 118.1 . . ? C16 C17 H17 118.1 . . ? N1 C18 C19 122.5(6) . . ? N1 C18 H18 118.8 . . ? C19 C18 H18 118.8 . . ? C20 C19 C18 119.0(6) . . ? C20 C19 H19 120.5 . . ? C18 C19 H19 120.5 . . ? C19 C20 C21 119.5(6) . . ? C19 C20 H20 120.3 . . ? C21 C20 H20 120.3 . . ? C22 C21 C20 118.8(6) . . ? C22 C21 H21 120.6 . . ? C20 C21 H21 120.6 . . ? N1 C22 C21 122.0(5) . . ? N1 C22 C23 117.1(4) . . ? C21 C22 C23 121.0(5) . . ? N2 C23 C22 111.2(4) . . ? N2 C23 H23A 109.4 . . ? C22 C23 H23A 109.4 . . ? N2 C23 H23B 109.4 . . ? C22 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Zn1 N1 C22 -164.0(4) 4_655 . . . ? N3 Zn1 N1 C22 96.9(4) . . . . ? N1 Zn1 N1 C22 -32.7(3) 4_655 . . . ? N2 Zn1 N1 C22 -86.2(4) 4_655 . . . ? N2 Zn1 N1 C22 24.2(3) . . . . ? N3 Zn1 N1 C18 7.2(5) 4_655 . . . ? N3 Zn1 N1 C18 -92.0(4) . . . . ? N1 Zn1 N1 C18 138.5(4) 4_655 . . . ? N2 Zn1 N1 C18 85.0(4) 4_655 . . . ? N2 Zn1 N1 C18 -164.6(5) . . . . ? N3 Zn1 N2 C23 -68.3(7) 4_655 . . . ? N3 Zn1 N2 C23 -142.3(3) . . . . ? N1 Zn1 N2 C23 -33.9(3) . . . . ? N1 Zn1 N2 C23 123.5(3) 4_655 . . . ? N2 Zn1 N2 C23 50.8(3) 4_655 . . . ? N3 Zn1 N2 C12 46.0(7) 4_655 . . . ? N3 Zn1 N2 C12 -27.9(3) . . . . ? N1 Zn1 N2 C12 80.5(3) . . . . ? N1 Zn1 N2 C12 -122.1(3) 4_655 . . . ? N2 Zn1 N2 C12 165.2(3) 4_655 . . . ? N3 Zn1 N2 C11 167.1(5) 4_655 . . . ? N3 Zn1 N2 C11 93.1(3) . . . . ? N1 Zn1 N2 C11 -158.5(4) . . . . ? N1 Zn1 N2 C11 -1.0(3) 4_655 . . . ? N2 Zn1 N2 C11 -73.8(3) 4_655 . . . ? N3 Zn1 N3 C17 29.0(4) 4_655 . . . ? N1 Zn1 N3 C17 125.3(5) . . . . ? N1 Zn1 N3 C17 -75.4(5) 4_655 . . . ? N2 Zn1 N3 C17 -42.4(9) 4_655 . . . ? N2 Zn1 N3 C17 -165.2(5) . . . . ? N3 Zn1 N3 C13 -151.9(4) 4_655 . . . ? N1 Zn1 N3 C13 -55.6(4) . . . . ? N1 Zn1 N3 C13 103.7(4) 4_655 . . . ? N2 Zn1 N3 C13 136.6(5) 4_655 . . . ? N2 Zn1 N3 C13 13.9(3) . . . . ? C5 Fe1 C1 C2 78.7(6) . . . . ? C4 Fe1 C1 C2 118.3(8) . . . . ? C3 Fe1 C1 C2 35.4(6) . . . . ? C8 Fe1 C1 C2 165.6(8) . . . . ? C9 Fe1 C1 C2 -25.8(17) . . . . ? C7 Fe1 C1 C2 -154.8(6) . . . . ? C6 Fe1 C1 C2 -111.2(6) . . . . ? C10 Fe1 C1 C2 -68.5(7) . . . . ? C5 Fe1 C1 C4 -39.6(6) . . . . ? C3 Fe1 C1 C4 -82.9(6) . . . . ? C8 Fe1 C1 C4 47.3(9) . . . . ? C9 Fe1 C1 C4 -144.0(14) . . . . ? C7 Fe1 C1 C4 87.0(6) . . . . ? C6 Fe1 C1 C4 130.5(5) . . . . ? C10 Fe1 C1 C4 173.2(5) . . . . ? C2 Fe1 C1 C4 -118.3(8) . . . . ? C4 C1 C2 C3 -0.4(9) . . . . ? Fe1 C1 C2 C3 -60.1(6) . . . . ? C4 C1 C2 Fe1 59.6(5) . . . . ? C5 Fe1 C2 C3 35.2(6) . . . . ? C4 Fe1 C2 C3 79.5(7) . . . . ? C8 Fe1 C2 C3 -28.6(18) . . . . ? C1 Fe1 C2 C3 118.5(9) . . . . ? C9 Fe1 C2 C3 -68.2(7) . . . . ? C7 Fe1 C2 C3 169.8(6) . . . . ? C6 Fe1 C2 C3 -153.5(6) . . . . ? C10 Fe1 C2 C3 -109.6(6) . . . . ? C5 Fe1 C2 C1 -83.3(6) . . . . ? C4 Fe1 C2 C1 -39.0(6) . . . . ? C3 Fe1 C2 C1 -118.5(9) . . . . ? C8 Fe1 C2 C1 -147.1(13) . . . . ? C9 Fe1 C2 C1 173.3(5) . . . . ? C7 Fe1 C2 C1 51.3(9) . . . . ? C6 Fe1 C2 C1 87.9(6) . . . . ? C10 Fe1 C2 C1 131.9(5) . . . . ? C1 C2 C3 C5 1.4(11) . . . . ? Fe1 C2 C3 C5 -58.0(7) . . . . ? C1 C2 C3 Fe1 59.4(6) . . . . ? C5 Fe1 C3 C2 -124.2(9) . . . . ? C4 Fe1 C3 C2 -84.3(7) . . . . ? C8 Fe1 C3 C2 171.7(5) . . . . ? C1 Fe1 C3 C2 -38.4(6) . . . . ? C9 Fe1 C3 C2 130.4(6) . . . . ? C7 Fe1 C3 C2 -149.2(19) . . . . ? C6 Fe1 C3 C2 49.0(9) . . . . ? C10 Fe1 C3 C2 86.3(6) . . . . ? C4 Fe1 C3 C5 39.9(5) . . . . ? C8 Fe1 C3 C5 -64.1(7) . . . . ? C1 Fe1 C3 C5 85.8(6) . . . . ? C9 Fe1 C3 C5 -105.4(5) . . . . ? C7 Fe1 C3 C5 -25(2) . . . . ? C6 Fe1 C3 C5 173.2(5) . . . . ? C10 Fe1 C3 C5 -149.5(5) . . . . ? C2 Fe1 C3 C5 124.2(9) . . . . ? C2 C1 C4 C5 -0.7(9) . . . . ? Fe1 C1 C4 C5 60.7(5) . . . . ? C2 C1 C4 Fe1 -61.4(5) . . . . ? C3 Fe1 C4 C5 -38.8(5) . . . . ? C8 Fe1 C4 C5 88.2(7) . . . . ? C1 Fe1 C4 C5 -115.3(8) . . . . ? C9 Fe1 C4 C5 51.5(9) . . . . ? C7 Fe1 C4 C5 132.1(6) . . . . ? C6 Fe1 C4 C5 171.5(6) . . . . ? C10 Fe1 C4 C5 -149.9(18) . . . . ? C2 Fe1 C4 C5 -78.2(6) . . . . ? C5 Fe1 C4 C1 115.3(8) . . . . ? C3 Fe1 C4 C1 76.5(6) . . . . ? C8 Fe1 C4 C1 -156.6(5) . . . . ? C9 Fe1 C4 C1 166.8(5) . . . . ? C7 Fe1 C4 C1 -112.6(5) . . . . ? C6 Fe1 C4 C1 -73.2(6) . . . . ? C10 Fe1 C4 C1 -35(2) . . . . ? C2 Fe1 C4 C1 37.1(5) . . . . ? C2 C3 C5 C4 -1.9(11) . . . . ? Fe1 C3 C5 C4 -62.2(6) . . . . ? C2 C3 C5 Fe1 60.4(8) . . . . ? C1 C4 C5 C3 1.4(9) . . . . ? Fe1 C4 C5 C3 62.7(6) . . . . ? C1 C4 C5 Fe1 -61.3(5) . . . . ? C4 Fe1 C5 C3 -115.7(8) . . . . ? C8 Fe1 C5 C3 135.5(6) . . . . ? C1 Fe1 C5 C3 -75.3(6) . . . . ? C9 Fe1 C5 C3 91.9(6) . . . . ? C7 Fe1 C5 C3 174.7(6) . . . . ? C6 Fe1 C5 C3 -157.9(18) . . . . ? C10 Fe1 C5 C3 56.1(8) . . . . ? C2 Fe1 C5 C3 -32.4(5) . . . . ? C3 Fe1 C5 C4 115.7(8) . . . . ? C8 Fe1 C5 C4 -108.9(6) . . . . ? C1 Fe1 C5 C4 40.4(5) . . . . ? C9 Fe1 C5 C4 -152.5(5) . . . . ? C7 Fe1 C5 C4 -69.7(7) . . . . ? C6 Fe1 C5 C4 -42(2) . . . . ? C10 Fe1 C5 C4 171.7(5) . . . . ? C2 Fe1 C5 C4 83.3(6) . . . . ? C5 Fe1 C6 C7 -32(2) . . . . ? C4 Fe1 C6 C7 -68.4(6) . . . . ? C3 Fe1 C6 C7 175.4(7) . . . . ? C8 Fe1 C6 C7 37.5(4) . . . . ? C1 Fe1 C6 C7 -111.1(5) . . . . ? C9 Fe1 C6 C7 81.7(5) . . . . ? C10 Fe1 C6 C7 120.1(6) . . . . ? C2 Fe1 C6 C7 -153.8(5) . . . . ? C5 Fe1 C6 C10 -152.4(18) . . . . ? C4 Fe1 C6 C10 171.5(4) . . . . ? C3 Fe1 C6 C10 55.3(8) . . . . ? C8 Fe1 C6 C10 -82.6(4) . . . . ? C1 Fe1 C6 C10 128.7(4) . . . . ? C9 Fe1 C6 C10 -38.4(3) . . . . ? C7 Fe1 C6 C10 -120.1(6) . . . . ? C2 Fe1 C6 C10 86.1(5) . . . . ? C10 C6 C7 C8 0.4(7) . . . . ? Fe1 C6 C7 C8 -58.7(5) . . . . ? C10 C6 C7 Fe1 59.1(4) . . . . ? C5 Fe1 C7 C6 173.3(4) . . . . ? C4 Fe1 C7 C6 132.9(5) . . . . ? C3 Fe1 C7 C6 -165.6(19) . . . . ? C8 Fe1 C7 C6 -119.9(6) . . . . ? C1 Fe1 C7 C6 88.4(5) . . . . ? C9 Fe1 C7 C6 -81.6(4) . . . . ? C10 Fe1 C7 C6 -37.6(4) . . . . ? C2 Fe1 C7 C6 53.8(8) . . . . ? C5 Fe1 C7 C8 -66.7(5) . . . . ? C4 Fe1 C7 C8 -107.1(5) . . . . ? C3 Fe1 C7 C8 -46(2) . . . . ? C1 Fe1 C7 C8 -151.6(5) . . . . ? C9 Fe1 C7 C8 38.4(4) . . . . ? C6 Fe1 C7 C8 119.9(6) . . . . ? C10 Fe1 C7 C8 82.4(4) . . . . ? C2 Fe1 C7 C8 173.8(6) . . . . ? C6 C7 C8 C9 -0.9(8) . . . . ? Fe1 C7 C8 C9 -60.1(4) . . . . ? C6 C7 C8 Fe1 59.2(4) . . . . ? C5 Fe1 C8 C7 134.0(5) . . . . ? C4 Fe1 C8 C7 90.9(5) . . . . ? C3 Fe1 C8 C7 170.9(5) . . . . ? C1 Fe1 C8 C7 58.2(8) . . . . ? C9 Fe1 C8 C7 -118.2(6) . . . . ? C6 Fe1 C8 C7 -36.8(4) . . . . ? C10 Fe1 C8 C7 -81.0(4) . . . . ? C2 Fe1 C8 C7 -166.7(14) . . . . ? C5 Fe1 C8 C9 -107.8(5) . . . . ? C4 Fe1 C8 C9 -150.9(5) . . . . ? C3 Fe1 C8 C9 -70.8(6) . . . . ? C1 Fe1 C8 C9 176.4(6) . . . . ? C7 Fe1 C8 C9 118.2(6) . . . . ? C6 Fe1 C8 C9 81.5(4) . . . . ? C10 Fe1 C8 C9 37.3(4) . . . . ? C2 Fe1 C8 C9 -48.4(16) . . . . ? C7 C8 C9 C10 1.0(7) . . . . ? Fe1 C8 C9 C10 -59.2(4) . . . . ? C7 C8 C9 Fe1 60.2(5) . . . . ? C5 Fe1 C9 C8 89.2(6) . . . . ? C4 Fe1 C9 C8 55.0(8) . . . . ? C3 Fe1 C9 C8 131.8(6) . . . . ? C1 Fe1 C9 C8 -171.6(13) . . . . ? C7 Fe1 C9 C8 -38.3(4) . . . . ? C6 Fe1 C9 C8 -81.4(5) . . . . ? C10 Fe1 C9 C8 -120.0(6) . . . . ? C2 Fe1 C9 C8 167.5(6) . . . . ? C5 Fe1 C9 C10 -150.8(5) . . . . ? C4 Fe1 C9 C10 175.0(6) . . . . ? C3 Fe1 C9 C10 -108.2(5) . . . . ? C8 Fe1 C9 C10 120.0(6) . . . . ? C1 Fe1 C9 C10 -51.6(15) . . . . ? C7 Fe1 C9 C10 81.7(4) . . . . ? C6 Fe1 C9 C10 38.6(3) . . . . ? C2 Fe1 C9 C10 -72.5(6) . . . . ? C8 C9 C10 C6 -0.8(6) . . . . ? Fe1 C9 C10 C6 -59.5(4) . . . . ? C8 C9 C10 C11 179.0(5) . . . . ? Fe1 C9 C10 C11 120.3(5) . . . . ? C8 C9 C10 Fe1 58.7(4) . . . . ? C7 C6 C10 C9 0.2(6) . . . . ? Fe1 C6 C10 C9 59.5(4) . . . . ? C7 C6 C10 C11 -179.6(5) . . . . ? Fe1 C6 C10 C11 -120.3(5) . . . . ? C7 C6 C10 Fe1 -59.2(4) . . . . ? C5 Fe1 C10 C9 54.1(7) . . . . ? C4 Fe1 C10 C9 -162.6(18) . . . . ? C3 Fe1 C10 C9 90.4(5) . . . . ? C8 Fe1 C10 C9 -37.4(4) . . . . ? C1 Fe1 C10 C9 167.5(4) . . . . ? C7 Fe1 C10 C9 -81.3(4) . . . . ? C6 Fe1 C10 C9 -117.9(5) . . . . ? C2 Fe1 C10 C9 128.9(5) . . . . ? C5 Fe1 C10 C6 172.1(6) . . . . ? C4 Fe1 C10 C6 -45(2) . . . . ? C3 Fe1 C10 C6 -151.7(5) . . . . ? C8 Fe1 C10 C6 80.5(5) . . . . ? C1 Fe1 C10 C6 -74.5(5) . . . . ? C9 Fe1 C10 C6 117.9(5) . . . . ? C7 Fe1 C10 C6 36.6(4) . . . . ? C2 Fe1 C10 C6 -113.1(5) . . . . ? C5 Fe1 C10 C11 -66.5(8) . . . . ? C4 Fe1 C10 C11 77(2) . . . . ? C3 Fe1 C10 C11 -30.2(6) . . . . ? C8 Fe1 C10 C11 -158.0(6) . . . . ? C1 Fe1 C10 C11 47.0(6) . . . . ? C9 Fe1 C10 C11 -120.6(6) . . . . ? C7 Fe1 C10 C11 158.1(5) . . . . ? C6 Fe1 C10 C11 121.5(6) . . . . ? C2 Fe1 C10 C11 8.4(6) . . . . ? C9 C10 C11 N2 96.0(6) . . . . ? C6 C10 C11 N2 -84.3(6) . . . . ? Fe1 C10 C11 N2 -174.4(3) . . . . ? C23 N2 C11 C10 61.5(5) . . . . ? C12 N2 C11 C10 -60.5(5) . . . . ? Zn1 N2 C11 C10 -177.0(3) . . . . ? C23 N2 C12 C13 150.8(4) . . . . ? C11 N2 C12 C13 -85.8(5) . . . . ? Zn1 N2 C12 C13 39.1(4) . . . . ? C17 N3 C13 C14 -0.7(8) . . . . ? Zn1 N3 C13 C14 -179.8(4) . . . . ? C17 N3 C13 C12 -176.4(5) . . . . ? Zn1 N3 C13 C12 4.4(5) . . . . ? N2 C12 C13 N3 -32.5(6) . . . . ? N2 C12 C13 C14 151.8(5) . . . . ? N3 C13 C14 C15 -1.3(9) . . . . ? C12 C13 C14 C15 174.2(5) . . . . ? C13 C14 C15 C16 2.3(10) . . . . ? C14 C15 C16 C17 -1.2(10) . . . . ? C13 N3 C17 C16 1.8(9) . . . . ? Zn1 N3 C17 C16 -179.1(5) . . . . ? C15 C16 C17 N3 -0.9(10) . . . . ? C22 N1 C18 C19 2.1(8) . . . . ? Zn1 N1 C18 C19 -168.9(5) . . . . ? N1 C18 C19 C20 -2.3(10) . . . . ? C18 C19 C20 C21 1.1(11) . . . . ? C19 C20 C21 C22 0.2(10) . . . . ? C18 N1 C22 C21 -0.8(8) . . . . ? Zn1 N1 C22 C21 171.0(4) . . . . ? C18 N1 C22 C23 179.1(5) . . . . ? Zn1 N1 C22 C23 -9.1(6) . . . . ? C20 C21 C22 N1 -0.4(9) . . . . ? C20 C21 C22 C23 179.8(5) . . . . ? C12 N2 C23 C22 -69.4(5) . . . . ? C11 N2 C23 C22 167.7(4) . . . . ? Zn1 N2 C23 C22 40.2(4) . . . . ? N1 C22 C23 N2 -23.2(6) . . . . ? C21 C22 C23 N2 156.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.852 _refine_diff_density_min -0.717 _refine_diff_density_rms 0.093