# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1653 #========================================================================== data_global #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Dr. Duan Chun-ying' _publ_contact_author_address ; Coordination Chemistry Institute The State Key Laboratory of Coordinaiton Chemistry Nanjing University , Nanjing 210093 P. R. China ; _publ_contact_author_email duancy@nju.edu.cn _publ_contact_author_fax '00 86 25 331 7761' _publ_contact_author_phone '00 86 25 359 3763' _publ_requested_journal 'Chemical Communications ' _publ_requested_category ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; A double-helix generated from ferrocenyl-thiosemicarbazato metallo-synthons and its novel hydrogen-bonding cavities ; loop_ _publ_author_name _publ_author_address 'Fang Chen-jie' ; Coordination Chemistry Institute and State Key Laboratory of Coordination Chemistry, Nanjing University,Nanjing,210093, People's Republic of China ; 'Duan Chun-ying' ; Coordination Chemistry Institute and State Key Laboratory of Coordination Chemistry, Nanjing University,Nanjing,210093, People's Republic of China ; 'He Cheng' ; Coordination Chemistry Institute and State Key Laboratory of Coordination Chemistry, Nanjing University,Nanjing,210093, People's Republic of China ; 'Meng Qing-jin' ; Coordination Chemistry Institute and State Key Laboratory of Coordination Chemistry, Nanjing University,Nanjing,210093, People's Republic of China ; data_H2L _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H22 Fe N6 O S2' _chemical_formula_weight 434.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M '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 29.0219(14) _cell_length_b 8.797(2) _cell_length_c 18.447(2) _cell_angle_alpha 90.00 _cell_angle_beta 125.944(12) _cell_angle_gamma 90.00 _cell_volume 3812.7(11) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 59 _cell_measurement_theta_min 4.91 _cell_measurement_theta_max 11.97 _exptl_crystal_description 'prism ' _exptl_crystal_colour 'red ' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.513 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 1.029 _exptl_absorpt_correction_type 'psi-scan' _exptl_absorpt_correction_T_min 0.5154 _exptl_absorpt_correction_T_max 0.7044 _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 ? _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_decay_% 10.29 _diffrn_reflns_number 4079 _diffrn_reflns_av_R_equivalents 0.0680 _diffrn_reflns_av_sigmaI/netI 0.0767 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3350 _reflns_number_gt 2297 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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^)+(0.1051P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3350 _refine_ls_number_parameters 323 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1003 _refine_ls_R_factor_gt 0.0647 _refine_ls_wR_factor_ref 0.1739 _refine_ls_wR_factor_gt 0.1512 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.13706(3) 0.96472(9) 0.36644(5) 0.0304(3) Uani 1 1 d . . . S2 S 0.00267(7) 0.2987(2) 0.45243(11) 0.0507(5) Uani 1 1 d . . . S1 S 0.17546(6) 0.57258(17) 0.75892(9) 0.0389(4) Uani 1 1 d . . . N1 N 0.2394(2) 0.7733(8) 0.7476(4) 0.0535(15) Uani 1 1 d . . . H1NB H 0.246(3) 0.848(7) 0.726(4) 0.043(19) Uiso 1 1 d . . . H1NA H 0.262(6) 0.754(14) 0.799(9) 0.17(6) Uiso 1 1 d . . . N2 N 0.1448(2) 0.7762(6) 0.6324(3) 0.0384(11) Uani 1 1 d . . . H2NA H 0.112(2) 0.743(6) 0.606(4) 0.028(15) Uiso 1 1 d . . . N3 N 0.1578(2) 0.8796(5) 0.5903(3) 0.0379(11) Uani 1 1 d . . . N4 N 0.06824(18) 0.5823(5) 0.3713(3) 0.0325(10) Uani 1 1 d . . . N5 N 0.0623(2) 0.4793(5) 0.4214(3) 0.0345(11) Uani 1 1 d . . . H5NA H 0.089(2) 0.436(6) 0.460(4) 0.027(16) Uiso 1 1 d . . . N6 N -0.0342(2) 0.4871(7) 0.3179(3) 0.0476(13) Uani 1 1 d . . . H6NA H -0.026(4) 0.553(9) 0.286(6) 0.09(3) Uiso 1 1 d . . . H6NB H -0.079(5) 0.481(12) 0.300(7) 0.13(4) Uiso 1 1 d . . . C1 C 0.1875(2) 0.7160(6) 0.7114(3) 0.0341(12) Uani 1 1 d . . . C2 C 0.1164(2) 0.9325(6) 0.5136(3) 0.0319(12) Uani 1 1 d . . . C3 C 0.0549(3) 0.8970(9) 0.4682(5) 0.0476(16) Uani 1 1 d . . . H3C H 0.047(3) 0.782(8) 0.456(4) 0.054(19) Uiso 1 1 d . . . H3B H 0.045(4) 0.930(11) 0.498(7) 0.10(4) Uiso 1 1 d . . . H3A H 0.036(4) 0.942(9) 0.418(6) 0.08(3) Uiso 1 1 d . . . C4 C 0.1330(2) 1.0332(6) 0.4690(4) 0.0342(12) Uani 1 1 d . . . C5 C 0.1887(3) 1.0577(7) 0.4923(4) 0.0395(14) Uani 1 1 d . . . H5A H 0.224(2) 1.012(6) 0.542(4) 0.030(14) Uiso 1 1 d . . . C6 C 0.1842(3) 1.1571(7) 0.4272(4) 0.0444(15) Uani 1 1 d . . . H6A H 0.214(3) 1.192(8) 0.430(4) 0.06(2) Uiso 1 1 d . . . C7 C 0.1257(3) 1.1924(7) 0.3639(4) 0.0481(16) Uani 1 1 d . . . H7A H 0.105(2) 1.255(7) 0.308(4) 0.044(16) Uiso 1 1 d . . . C8 C 0.0946(3) 1.1195(7) 0.3892(4) 0.0434(14) Uani 1 1 d . . . H8A H 0.055(2) 1.124(6) 0.357(3) 0.023(13) Uiso 1 1 d . . . C9 C 0.0787(3) 0.8181(7) 0.2714(4) 0.0412(14) Uani 1 1 d . . . H9A H 0.043(2) 0.802(6) 0.242(3) 0.023(13) Uiso 1 1 d . . . C10 C 0.1019(3) 0.9072(8) 0.2354(4) 0.0513(17) Uani 1 1 d . . . H10A H 0.091(3) 0.986(9) 0.197(5) 0.07(2) Uiso 1 1 d . . . C11 C 0.1611(3) 0.8832(7) 0.2893(5) 0.0493(17) Uani 1 1 d . . . H11A H 0.192(3) 0.931(8) 0.289(5) 0.06(2) Uiso 1 1 d . . . C12 C 0.1745(3) 0.7772(8) 0.3560(5) 0.0435(15) Uani 1 1 d . . . H12A H 0.203(3) 0.758(8) 0.399(4) 0.04(2) Uiso 1 1 d . . . C13 C 0.1239(2) 0.7339(6) 0.3460(3) 0.0333(12) Uani 1 1 d . . . C14 C 0.1188(2) 0.6251(6) 0.4004(3) 0.0311(12) Uani 1 1 d . . . C15 C 0.1720(3) 0.5665(8) 0.4849(5) 0.0471(16) Uani 1 1 d . . . H15B H 0.210(3) 0.600(8) 0.490(5) 0.07(2) Uiso 1 1 d . . . H15C H 0.167(3) 0.464(8) 0.496(5) 0.07(2) Uiso 1 1 d . . . H15A H 0.182(4) 0.609(10) 0.537(6) 0.10(3) Uiso 1 1 d . . . C16 C 0.0105(2) 0.4299(6) 0.3932(4) 0.0318(12) Uani 1 1 d . . . O1W O 0.1402(2) 0.3225(7) 0.5992(3) 0.0625(14) Uani 1 1 d . . . H1WA H 0.139(3) 0.383(8) 0.628(4) 0.05(2) Uiso 1 1 d . . . H1WB H 0.099(4) 0.261(11) 0.569(7) 0.12(3) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0307(4) 0.0328(4) 0.0305(4) -0.0020(3) 0.0196(3) -0.0066(3) S2 0.0447(9) 0.0552(10) 0.0551(10) 0.0200(8) 0.0309(8) -0.0002(7) S1 0.0343(8) 0.0496(9) 0.0311(7) 0.0078(6) 0.0182(6) 0.0052(6) N1 0.032(3) 0.076(4) 0.042(3) 0.007(3) 0.016(3) -0.012(3) N2 0.030(3) 0.053(3) 0.032(2) 0.007(2) 0.018(2) -0.003(2) N3 0.039(3) 0.043(3) 0.036(3) -0.001(2) 0.025(2) -0.006(2) N4 0.031(2) 0.035(2) 0.029(2) 0.0003(19) 0.016(2) -0.0079(19) N5 0.028(3) 0.038(3) 0.032(2) 0.006(2) 0.015(2) -0.001(2) N6 0.030(3) 0.059(3) 0.042(3) 0.015(3) 0.015(2) 0.000(2) C1 0.035(3) 0.041(3) 0.030(3) -0.006(2) 0.021(3) -0.001(3) C2 0.035(3) 0.034(3) 0.031(3) -0.006(2) 0.022(2) -0.004(2) C3 0.037(3) 0.063(5) 0.050(4) 0.015(4) 0.029(3) 0.001(3) C4 0.045(3) 0.027(3) 0.038(3) -0.002(2) 0.028(3) 0.000(2) C5 0.042(3) 0.042(3) 0.033(3) -0.008(3) 0.021(3) -0.012(3) C6 0.056(4) 0.037(3) 0.051(4) -0.013(3) 0.037(3) -0.024(3) C7 0.078(5) 0.029(3) 0.052(4) 0.004(3) 0.047(4) -0.006(3) C8 0.044(4) 0.045(3) 0.048(3) 0.007(3) 0.030(3) 0.009(3) C9 0.033(3) 0.055(4) 0.027(3) -0.007(3) 0.013(3) -0.017(3) C10 0.062(4) 0.055(4) 0.039(3) -0.005(3) 0.031(3) -0.015(3) C11 0.061(4) 0.051(4) 0.063(4) -0.016(3) 0.052(4) -0.023(3) C12 0.042(4) 0.046(4) 0.052(4) -0.008(3) 0.033(4) -0.007(3) C13 0.034(3) 0.032(3) 0.037(3) -0.014(2) 0.023(3) -0.013(2) C14 0.026(3) 0.029(3) 0.036(3) -0.008(2) 0.017(2) -0.005(2) C15 0.031(3) 0.048(4) 0.050(4) 0.003(3) 0.017(3) -0.002(3) C16 0.032(3) 0.030(3) 0.036(3) 0.001(2) 0.022(3) -0.001(2) O1W 0.063(3) 0.069(4) 0.039(3) -0.002(3) 0.020(3) 0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C7 2.026(6) . ? Fe1 C9 2.030(6) . ? Fe1 C8 2.038(6) . ? Fe1 C12 2.046(7) . ? Fe1 C11 2.047(6) . ? Fe1 C6 2.048(6) . ? Fe1 C4 2.053(5) . ? Fe1 C5 2.054(6) . ? Fe1 C13 2.060(5) . ? Fe1 C10 2.060(6) . ? S2 C16 1.693(5) . ? S1 C1 1.686(6) . ? N1 C1 1.336(8) . ? N2 C1 1.349(7) . ? N2 N3 1.386(6) . ? N3 C2 1.292(7) . ? N4 C14 1.286(6) . ? N4 N5 1.375(6) . ? N5 C16 1.343(7) . ? N6 C16 1.322(7) . ? C2 C4 1.468(8) . ? C2 C3 1.494(8) . ? C4 C5 1.426(8) . ? C4 C8 1.435(8) . ? C5 C6 1.427(8) . ? C6 C7 1.420(10) . ? C7 C8 1.393(8) . ? C9 C10 1.426(9) . ? C9 C13 1.429(8) . ? C10 C11 1.408(10) . ? C11 C12 1.404(10) . ? C12 C13 1.422(8) . ? C13 C14 1.456(8) . ? C14 C15 1.501(8) . ? 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 C7 Fe1 C9 124.5(3) . . ? C7 Fe1 C8 40.1(2) . . ? C9 Fe1 C8 107.6(3) . . ? C7 Fe1 C12 152.0(3) . . ? C9 Fe1 C12 68.1(3) . . ? C8 Fe1 C12 167.6(2) . . ? C7 Fe1 C11 116.6(3) . . ? C9 Fe1 C11 68.2(3) . . ? C8 Fe1 C11 150.6(3) . . ? C12 Fe1 C11 40.1(3) . . ? C7 Fe1 C6 40.8(3) . . ? C9 Fe1 C6 161.6(2) . . ? C8 Fe1 C6 68.0(3) . . ? C12 Fe1 C6 119.8(3) . . ? C11 Fe1 C6 106.2(2) . . ? C7 Fe1 C4 68.6(2) . . ? C9 Fe1 C4 120.8(2) . . ? C8 Fe1 C4 41.0(2) . . ? C12 Fe1 C4 130.1(3) . . ? C11 Fe1 C4 166.0(3) . . ? C6 Fe1 C4 68.6(2) . . ? C7 Fe1 C5 68.5(3) . . ? C9 Fe1 C5 156.1(2) . . ? C8 Fe1 C5 68.3(3) . . ? C12 Fe1 C5 110.6(3) . . ? C11 Fe1 C5 127.2(3) . . ? C6 Fe1 C5 40.7(2) . . ? C4 Fe1 C5 40.6(2) . . ? C7 Fe1 C13 163.8(3) . . ? C9 Fe1 C13 40.9(2) . . ? C8 Fe1 C13 128.8(2) . . ? C12 Fe1 C13 40.5(2) . . ? C11 Fe1 C13 68.3(2) . . ? C6 Fe1 C13 155.2(3) . . ? C4 Fe1 C13 110.6(2) . . ? C5 Fe1 C13 122.2(2) . . ? C7 Fe1 C10 104.7(3) . . ? C9 Fe1 C10 40.8(2) . . ? C8 Fe1 C10 117.5(3) . . ? C12 Fe1 C10 67.4(3) . . ? C11 Fe1 C10 40.1(3) . . ? C6 Fe1 C10 123.9(3) . . ? C4 Fe1 C10 153.6(3) . . ? C5 Fe1 C10 162.6(3) . . ? C13 Fe1 C10 68.4(3) . . ? C1 N2 N3 118.8(5) . . ? C2 N3 N2 117.8(5) . . ? C14 N4 N5 118.3(4) . . ? C16 N5 N4 120.5(5) . . ? N1 C1 N2 116.3(5) . . ? N1 C1 S1 122.7(5) . . ? N2 C1 S1 121.0(4) . . ? N3 C2 C4 115.6(5) . . ? N3 C2 C3 125.1(5) . . ? C4 C2 C3 119.3(5) . . ? C5 C4 C8 106.8(5) . . ? C5 C4 C2 127.5(5) . . ? C8 C4 C2 125.5(5) . . ? C5 C4 Fe1 69.7(3) . . ? C8 C4 Fe1 68.9(3) . . ? C2 C4 Fe1 123.6(4) . . ? C4 C5 C6 108.2(5) . . ? C4 C5 Fe1 69.7(3) . . ? C6 C5 Fe1 69.4(3) . . ? C7 C6 C5 107.5(5) . . ? C7 C6 Fe1 68.8(3) . . ? C5 C6 Fe1 69.9(3) . . ? C8 C7 C6 108.7(5) . . ? C8 C7 Fe1 70.5(4) . . ? C6 C7 Fe1 70.4(3) . . ? C7 C8 C4 108.8(6) . . ? C7 C8 Fe1 69.5(4) . . ? C4 C8 Fe1 70.0(3) . . ? C10 C9 C13 108.5(6) . . ? C10 C9 Fe1 70.7(4) . . ? C13 C9 Fe1 70.7(3) . . ? C11 C10 C9 107.6(6) . . ? C11 C10 Fe1 69.5(4) . . ? C9 C10 Fe1 68.5(3) . . ? C12 C11 C10 108.3(6) . . ? C12 C11 Fe1 69.9(4) . . ? C10 C11 Fe1 70.4(4) . . ? C11 C12 C13 109.3(6) . . ? C11 C12 Fe1 70.0(4) . . ? C13 C12 Fe1 70.3(3) . . ? C12 C13 C9 106.3(5) . . ? C12 C13 C14 127.1(5) . . ? C9 C13 C14 126.7(5) . . ? C12 C13 Fe1 69.2(3) . . ? C9 C13 Fe1 68.4(3) . . ? C14 C13 Fe1 127.3(4) . . ? N4 C14 C13 117.2(5) . . ? N4 C14 C15 124.0(5) . . ? C13 C14 C15 118.8(5) . . ? N6 C16 N5 117.9(5) . . ? N6 C16 S2 121.2(4) . . ? N5 C16 S2 120.9(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.737 _refine_diff_density_min -1.588 _refine_diff_density_rms 0.118 ##END ############### data_zn2l2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H44 Cl4 Fe2 N12 O2 S4 Zn2' _chemical_formula_weight 1165.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' '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' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'C2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 30.076(6) _cell_length_b 9.6742(18) _cell_length_c 21.693(5) _cell_angle_alpha 90.00 _cell_angle_beta 132.206(17) _cell_angle_gamma 90.00 _cell_volume 4675.4(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 54 _cell_measurement_theta_min 4.90 _cell_measurement_theta_max 11.78 _exptl_crystal_description 'plate' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.655 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2368 _exptl_absorpt_coefficient_mu 2.075 _exptl_absorpt_correction_type 'psi-scan' _exptl_absorpt_correction_T_min 0.5008 _exptl_absorpt_correction_T_max 0.9096 _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 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_decay_% 9.75 _diffrn_reflns_number 5145 _diffrn_reflns_av_R_equivalents 0.0584 _diffrn_reflns_av_sigmaI/netI 0.0479 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4849 _reflns_number_gt 4240 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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^)+(0.1507P)^2^+3.2095P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.07(3) _refine_ls_number_reflns 4849 _refine_ls_number_parameters 553 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0803 _refine_ls_R_factor_gt 0.0695 _refine_ls_wR_factor_ref 0.1882 _refine_ls_wR_factor_gt 0.1770 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.39203(5) 0.28341(13) 0.25969(7) 0.0315(3) Uani 1 1 d . . . Fe1 Fe 0.61141(6) 0.28926(19) 0.51309(9) 0.0329(4) Uani 1 1 d . . . S11 S 0.31452(13) 0.4373(3) 0.1882(2) 0.0477(8) Uani 1 1 d . . . S12 S 0.58778(14) 0.1313(3) 0.79792(18) 0.0404(7) Uani 1 1 d . . . N11 N 0.3325(5) 0.6900(13) 0.2397(7) 0.059(3) Uani 1 1 d . . . H11B H 0.3526 0.7626 0.2683 0.071 Uiso 1 1 calc R . . H11C H 0.2940 0.6908 0.2057 0.071 Uiso 1 1 calc R . . N12 N 0.4193(4) 0.5801(10) 0.3002(6) 0.040(2) Uani 1 1 d . . . N13 N 0.4484(4) 0.4532(9) 0.3184(5) 0.0307(19) Uani 1 1 d . . . N14 N 0.6179(4) 0.1169(9) 0.6920(5) 0.0294(19) Uani 1 1 d . . . N15 N 0.6076(5) -0.0121(10) 0.7091(6) 0.039(2) Uani 1 1 d . . . N16 N 0.5728(6) -0.1306(12) 0.7594(8) 0.058(3) Uani 1 1 d . . . H16A H 0.5729 -0.2048 0.7376 0.069 Uiso 1 1 calc R . . H16B H 0.5614 -0.1335 0.7866 0.069 Uiso 1 1 calc R . . C1 C 0.3615(6) 0.5750(12) 0.2482(7) 0.041(3) Uani 1 1 d . . . C2 C 0.5048(5) 0.4593(13) 0.3564(7) 0.037(3) Uani 1 1 d . . . C3 C 0.5331(6) 0.5938(18) 0.3676(10) 0.069(5) Uani 1 1 d . . . H3A H 0.5035 0.6658 0.3424 0.104 Uiso 1 1 calc R . . H3B H 0.5493 0.5904 0.3417 0.104 Uiso 1 1 calc R . . H3C H 0.5647 0.6125 0.4259 0.104 Uiso 1 1 calc R . . C4 C 0.5397(5) 0.3323(13) 0.3890(6) 0.039(3) Uani 1 1 d . . . C5 C 0.5297(5) 0.2086(15) 0.4152(6) 0.042(3) Uani 1 1 d . . . H5A H 0.4966 0.1940 0.4133 0.050 Uiso 1 1 calc R . . C6 C 0.5742(7) 0.1145(17) 0.4435(8) 0.065(4) Uani 1 1 d . . . H6A H 0.5779 0.0212 0.4641 0.078 Uiso 1 1 calc R . . C7 C 0.6138(7) 0.177(2) 0.4352(9) 0.069(5) Uani 1 1 d . . . H7A H 0.6498 0.1334 0.4514 0.083 Uiso 1 1 calc R . . C8 C 0.5948(6) 0.3089(17) 0.4044(7) 0.054(3) Uani 1 1 d . . . H8A H 0.6140 0.3743 0.3940 0.064 Uiso 1 1 calc R . . C9 C 0.6940(4) 0.2759(17) 0.6306(6) 0.045(3) Uani 1 1 d . . . H9A H 0.7273 0.2160 0.6490 0.054 Uiso 1 1 calc R . . C10 C 0.6830(7) 0.4136(17) 0.6003(9) 0.057(4) Uani 1 1 d . . . H10A H 0.7072 0.4637 0.5925 0.068 Uiso 1 1 calc R . . C11 C 0.6336(8) 0.4635(15) 0.5819(9) 0.059(4) Uani 1 1 d . . . H11A H 0.6165 0.5555 0.5589 0.071 Uiso 1 1 calc R . . C12 C 0.6096(6) 0.3637(12) 0.5991(7) 0.039(3) Uani 1 1 d . . . H12A H 0.5740 0.3741 0.5920 0.047 Uiso 1 1 calc R . . C13 C 0.6485(5) 0.2441(11) 0.6326(6) 0.033(2) Uani 1 1 d . . . C14 C 0.6434(4) 0.1121(12) 0.6612(6) 0.029(2) Uani 1 1 d . . . C15 C 0.6675(7) -0.0144(15) 0.6552(8) 0.051(3) Uani 1 1 d . . . H15A H 0.6610 -0.0914 0.6763 0.077 Uiso 1 1 calc R . . H15B H 0.7097 -0.0033 0.6873 0.077 Uiso 1 1 calc R . . H15C H 0.6474 -0.0310 0.5981 0.077 Uiso 1 1 calc R . . C16 C 0.5907(5) -0.0097(12) 0.7510(7) 0.033(2) Uani 1 1 d . . . Zn2 Zn 0.09319(5) 0.20221(12) 0.23752(7) 0.0310(3) Uani 1 1 d . . . Fe2 Fe -0.11994(6) 0.19950(18) -0.03502(9) 0.0311(4) Uani 1 1 d . . . S21 S 0.17050(14) 0.0512(3) 0.31771(19) 0.0458(8) Uani 1 1 d . . . S22 S -0.05858(14) 0.3543(3) -0.27672(18) 0.0389(7) Uani 1 1 d . . . N21 N 0.1548(5) -0.2132(13) 0.2775(7) 0.058(3) Uani 1 1 d . . . H21B H 0.1350 -0.2869 0.2502 0.070 Uiso 1 1 calc R . . H21C H 0.1933 -0.2161 0.3163 0.070 Uiso 1 1 calc R . . N22 N 0.0672(4) -0.0946(10) 0.2000(6) 0.036(2) Uani 1 1 d . . . N23 N 0.0382(4) 0.0334(10) 0.1750(5) 0.0287(19) Uani 1 1 d . . . N24 N -0.1082(4) 0.3709(10) -0.1945(5) 0.0306(19) Uani 1 1 d . . . N25 N -0.0931(4) 0.5003(9) -0.2056(6) 0.034(2) Uani 1 1 d . . . N26 N -0.0447(5) 0.6132(11) -0.2359(7) 0.051(3) Uani 1 1 d . . . H26B H -0.0472 0.6873 -0.2166 0.061 Uiso 1 1 calc R . . H26C H -0.0274 0.6151 -0.2553 0.061 Uiso 1 1 calc R . . C17 C 0.1250(5) -0.0910(12) 0.2591(7) 0.036(3) Uani 1 1 d . . . C18 C -0.0197(5) 0.0299(12) 0.1284(7) 0.034(2) Uani 1 1 d . . . C19 C -0.0531(6) -0.0980(15) 0.1151(9) 0.056(4) Uani 1 1 d . . . H19A H -0.0255 -0.1740 0.1437 0.084 Uiso 1 1 calc R . . H19B H -0.0829 -0.1181 0.0566 0.084 Uiso 1 1 calc R . . H19C H -0.0723 -0.0840 0.1363 0.084 Uiso 1 1 calc R . . C20 C -0.0533(5) 0.1591(12) 0.0903(6) 0.036(3) Uani 1 1 d . . . C21 C -0.1099(5) 0.1854(17) 0.0674(7) 0.047(3) Uani 1 1 d . . . H21A H -0.1316 0.1243 0.0754 0.057 Uiso 1 1 calc R . . C22 C -0.1261(8) 0.3252(17) 0.0344(9) 0.065(5) Uani 1 1 d . . . H22A H -0.1621 0.3751 0.0141 0.079 Uiso 1 1 calc R . . C23 C -0.0830(6) 0.3745(14) 0.0340(8) 0.055(4) Uani 1 1 d . . . H23A H -0.0844 0.4651 0.0124 0.067 Uiso 1 1 calc R . . C24 C -0.0362(5) 0.2740(13) 0.0687(6) 0.039(2) Uani 1 1 d . . . H24A H -0.0003 0.2826 0.0763 0.047 Uiso 1 1 calc R . . C25 C -0.1121(5) 0.1260(13) -0.1150(7) 0.038(3) Uani 1 1 d . . . H25A H -0.0743 0.1149 -0.1025 0.046 Uiso 1 1 calc R . . C26 C -0.1395(8) 0.0226(15) -0.1014(8) 0.060(4) Uani 1 1 d . . . H26A H -0.1238 -0.0701 -0.0783 0.072 Uiso 1 1 calc R . . C27 C -0.1913(6) 0.0810(19) -0.1242(9) 0.061(4) Uani 1 1 d . . . H27A H -0.2184 0.0355 -0.1202 0.073 Uiso 1 1 calc R . . C28 C -0.1987(5) 0.2132(17) -0.1550(7) 0.047(3) Uani 1 1 d . . . H28A H -0.2318 0.2763 -0.1760 0.057 Uiso 1 1 calc R . . C29 C -0.1485(5) 0.2436(13) -0.1499(7) 0.038(3) Uani 1 1 d . . . C30 C -0.1398(5) 0.3738(13) -0.1741(7) 0.035(3) Uani 1 1 d . . . C31 C -0.1683(6) 0.5030(14) -0.1769(9) 0.053(4) Uani 1 1 d . . . H31A H -0.1578 0.5790 -0.1935 0.079 Uiso 1 1 calc R . . H31B H -0.1542 0.5211 -0.1227 0.079 Uiso 1 1 calc R . . H31C H -0.2111 0.4919 -0.2162 0.079 Uiso 1 1 calc R . . C32 C -0.0675(5) 0.4956(11) -0.2360(7) 0.033(2) Uani 1 1 d . . . C33 C 0.2213(9) 0.7478(16) 0.0161(13) 0.122(7) Uani 1 1 d DU . . H33A H 0.2499 0.6753 0.0334 0.146 Uiso 1 1 calc R . . H33B H 0.1921 0.7490 -0.0442 0.146 Uiso 1 1 calc R . . Cl1 Cl 0.18495(18) 0.7018(6) 0.0469(3) 0.0898(14) Uani 1 1 d DU . . Cl2 Cl 0.2582(3) 0.8982(7) 0.0487(4) 0.1102(19) Uani 1 1 d DU . . C34 C 0.2957(10) 0.868(2) 0.5036(15) 0.160(8) Uani 1 1 d DU . . H34C H 0.2799 0.9538 0.4740 0.192 Uiso 0.56(3) 1 d PR A 2 H34D H 0.3333 0.8870 0.5584 0.192 Uiso 0.56(3) 1 d PR A 2 H34A H 0.2725 0.9374 0.4614 0.192 Uiso 0.44(3) 1 d PR A 1 H34B H 0.3349 0.9081 0.5435 0.192 Uiso 0.44(3) 1 d PR A 1 Cl3 Cl 0.3111(3) 0.7663(10) 0.4595(4) 0.134(3) Uani 1 1 d DU A . Cl4 Cl 0.2731(12) 0.889(4) 0.5544(14) 0.152(7) Uani 0.44(3) 1 d PDU A 1 Cl4' Cl 0.2507(7) 0.804(3) 0.5153(12) 0.147(6) Uani 0.56(3) 1 d PDU A 2 O1W O 0.0000 -0.1365(18) 0.0000 0.075(5) Uani 1 2 d S . . O2W O 0.5000 -0.046(2) 0.5000 0.075(5) Uani 1 2 d S . . O3W O 0.0000 0.558(3) 0.0000 0.105(7) Uani 1 2 d S . . O4W O 0.5000 0.653(3) 0.5000 0.121(8) 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 Zn1 0.0364(6) 0.0253(6) 0.0292(6) 0.0007(6) 0.0206(5) -0.0011(6) Fe1 0.0328(7) 0.0389(9) 0.0284(7) 0.0074(8) 0.0211(6) 0.0067(8) S11 0.0324(15) 0.0296(16) 0.0429(16) -0.0015(13) 0.0098(13) 0.0010(13) S12 0.0591(18) 0.0330(15) 0.0430(15) -0.0046(13) 0.0399(15) -0.0027(14) N11 0.042(6) 0.030(5) 0.077(7) 0.004(6) 0.029(6) 0.003(5) N12 0.041(5) 0.034(6) 0.050(6) -0.004(5) 0.032(5) -0.004(5) N13 0.031(5) 0.018(4) 0.032(4) 0.012(4) 0.017(4) 0.005(4) N14 0.040(5) 0.023(4) 0.029(4) 0.005(4) 0.025(4) 0.004(4) N15 0.055(6) 0.026(5) 0.045(6) 0.005(4) 0.038(5) 0.006(5) N16 0.093(9) 0.033(6) 0.093(9) -0.006(6) 0.082(8) -0.004(6) C1 0.047(7) 0.027(6) 0.040(6) 0.006(5) 0.025(6) 0.012(6) C2 0.036(6) 0.037(6) 0.036(6) 0.006(5) 0.023(5) -0.004(5) C3 0.045(8) 0.062(10) 0.067(9) 0.029(8) 0.024(7) -0.004(7) C4 0.043(6) 0.049(7) 0.027(5) 0.005(5) 0.024(5) 0.002(6) C5 0.040(6) 0.039(6) 0.025(5) 0.004(6) 0.013(5) 0.001(6) C6 0.074(10) 0.044(8) 0.030(6) -0.002(6) 0.016(7) 0.018(8) C7 0.081(10) 0.089(13) 0.052(8) 0.021(8) 0.051(8) 0.045(10) C8 0.063(8) 0.065(9) 0.037(6) 0.005(7) 0.035(6) 0.013(8) C9 0.023(5) 0.069(9) 0.034(5) 0.015(7) 0.016(4) 0.008(6) C10 0.056(8) 0.063(10) 0.056(8) -0.004(7) 0.040(7) -0.020(8) C11 0.097(12) 0.033(7) 0.055(8) 0.005(6) 0.054(9) -0.003(8) C12 0.055(7) 0.025(6) 0.041(6) 0.006(5) 0.034(6) 0.007(6) C13 0.032(5) 0.035(6) 0.026(5) 0.000(4) 0.018(4) -0.003(4) C14 0.022(5) 0.030(6) 0.021(5) 0.008(4) 0.009(4) 0.008(4) C15 0.064(8) 0.058(9) 0.058(8) 0.016(7) 0.051(7) 0.023(7) C16 0.034(5) 0.039(6) 0.032(5) 0.005(5) 0.024(5) 0.003(5) Zn2 0.0388(6) 0.0198(6) 0.0315(6) -0.0009(5) 0.0225(5) -0.0018(6) Fe2 0.0279(7) 0.0367(8) 0.0295(7) 0.0090(8) 0.0196(6) 0.0054(7) S21 0.0358(15) 0.0304(15) 0.0355(15) -0.0013(13) 0.0094(13) -0.0012(13) S22 0.0607(18) 0.0295(14) 0.0446(15) -0.0010(13) 0.0428(15) 0.0011(14) N21 0.043(6) 0.028(5) 0.061(6) 0.001(6) 0.018(5) 0.005(6) N22 0.035(5) 0.024(5) 0.044(5) 0.003(4) 0.023(5) 0.000(4) N23 0.024(4) 0.029(5) 0.023(4) 0.001(4) 0.012(4) -0.005(4) N24 0.035(5) 0.029(5) 0.032(4) 0.004(4) 0.024(4) 0.002(4) N25 0.047(5) 0.014(4) 0.050(6) -0.006(4) 0.037(5) -0.003(4) N26 0.085(8) 0.029(5) 0.077(7) -0.009(5) 0.071(7) -0.008(6) C17 0.032(6) 0.031(6) 0.036(6) 0.004(5) 0.019(5) 0.006(5) C18 0.040(6) 0.026(6) 0.027(5) 0.003(4) 0.018(5) -0.007(5) C19 0.035(6) 0.044(8) 0.065(8) 0.015(7) 0.023(6) -0.014(6) C20 0.032(5) 0.037(7) 0.026(5) -0.001(5) 0.015(5) 0.001(5) C21 0.049(6) 0.068(9) 0.040(6) 0.021(7) 0.036(6) 0.023(7) C22 0.080(10) 0.067(11) 0.054(8) 0.026(8) 0.046(8) 0.042(9) C23 0.060(8) 0.025(6) 0.043(7) 0.008(6) 0.018(7) 0.019(6) C24 0.043(6) 0.026(6) 0.023(5) 0.004(5) 0.011(5) -0.002(6) C25 0.050(7) 0.036(6) 0.034(6) 0.004(5) 0.031(6) 0.002(6) C26 0.098(12) 0.037(7) 0.045(7) -0.008(6) 0.048(8) -0.030(8) C27 0.046(8) 0.076(11) 0.049(8) 0.004(8) 0.027(7) -0.017(8) C28 0.024(5) 0.067(9) 0.033(5) 0.016(7) 0.012(5) -0.004(6) C29 0.031(5) 0.049(8) 0.034(5) 0.000(5) 0.021(5) -0.007(5) C30 0.035(6) 0.033(6) 0.042(6) 0.014(5) 0.027(5) 0.013(5) C31 0.063(8) 0.045(8) 0.071(9) 0.024(7) 0.053(8) 0.029(7) C32 0.042(6) 0.020(5) 0.037(6) 0.002(4) 0.027(5) 0.004(5) C33 0.112(11) 0.115(12) 0.093(10) -0.005(10) 0.050(9) 0.006(11) Cl1 0.056(2) 0.072(3) 0.095(3) 0.024(3) 0.032(2) 0.004(2) Cl2 0.148(5) 0.111(4) 0.131(5) 0.004(4) 0.117(5) -0.005(4) C34 0.108(11) 0.210(16) 0.124(11) 0.023(12) 0.062(9) 0.040(12) Cl3 0.094(4) 0.166(7) 0.110(4) 0.007(5) 0.056(3) 0.037(5) Cl4 0.108(11) 0.221(19) 0.127(12) 0.033(12) 0.079(10) 0.054(11) Cl4' 0.111(9) 0.228(17) 0.109(9) 0.057(10) 0.078(8) 0.048(10) O1W 0.115(13) 0.057(9) 0.061(9) 0.000 0.063(10) 0.000 O2W 0.068(10) 0.080(11) 0.046(8) 0.000 0.025(8) 0.000 O3W 0.069(11) 0.094(15) 0.116(16) 0.000 0.048(12) 0.000 O4W 0.16(2) 0.105(19) 0.148(19) 0.000 0.126(19) 0.000 _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 N14 2.050(9) 2_656 ? Zn1 N13 2.073(9) . ? Zn1 S12 2.262(3) 2_656 ? Zn1 S11 2.280(3) . ? Fe1 C6 2.030(15) . ? Fe1 C12 2.035(11) . ? Fe1 C5 2.035(12) . ? Fe1 C11 2.044(14) . ? Fe1 C9 2.045(10) . ? Fe1 C10 2.047(15) . ? Fe1 C7 2.049(14) . ? Fe1 C8 2.065(11) . ? Fe1 C13 2.066(10) . ? Fe1 C4 2.067(11) . ? S11 C1 1.730(13) . ? S12 C16 1.739(12) . ? S12 Zn1 2.262(3) 2_656 ? N11 C1 1.348(16) . ? N12 C1 1.289(16) . ? N12 N13 1.401(13) . ? N13 C2 1.297(14) . ? N14 C14 1.312(13) . ? N14 N15 1.396(13) . ? N14 Zn1 2.050(9) 2_656 ? N15 C16 1.305(13) . ? N16 C16 1.350(16) . ? C2 C4 1.453(17) . ? C2 C3 1.482(19) . ? C4 C5 1.441(18) . ? C4 C8 1.471(17) . ? C5 C6 1.376(19) . ? C6 C7 1.45(2) . ? C7 C8 1.37(2) . ? C9 C10 1.42(2) . ? C9 C13 1.433(14) . ? C10 C11 1.34(2) . ? C11 C12 1.398(19) . ? C12 C13 1.446(16) . ? C13 C14 1.473(15) . ? C14 C15 1.472(17) . ? Zn2 N23 2.056(9) . ? Zn2 N24 2.075(9) 2 ? Zn2 S21 2.266(3) . ? Zn2 S22 2.272(3) 2 ? Fe2 C27 2.021(15) . ? Fe2 C23 2.027(14) . ? Fe2 C25 2.030(11) . ? Fe2 C28 2.030(10) . ? Fe2 C21 2.035(10) . ? Fe2 C22 2.037(15) . ? Fe2 C26 2.052(14) . ? Fe2 C20 2.059(11) . ? Fe2 C29 2.062(11) . ? Fe2 C24 2.077(11) . ? S21 C17 1.744(12) . ? S22 C32 1.744(11) . ? S22 Zn2 2.272(3) 2 ? N21 C17 1.371(16) . ? N22 C17 1.295(15) . ? N22 N23 1.398(13) . ? N23 C18 1.300(14) . ? N24 C30 1.290(13) . ? N24 N25 1.407(12) . ? N24 Zn2 2.075(9) 2 ? N25 C32 1.307(14) . ? N26 C32 1.328(15) . ? C18 C20 1.465(16) . ? C18 C19 1.493(16) . ? C20 C24 1.430(16) . ? C20 C21 1.439(15) . ? C21 C22 1.45(2) . ? C22 C23 1.39(2) . ? C23 C24 1.439(17) . ? C25 C29 1.397(17) . ? C25 C26 1.447(17) . ? C26 C27 1.40(2) . ? C27 C28 1.39(2) . ? C28 C29 1.467(15) . ? C29 C30 1.455(16) . ? C30 C31 1.493(16) . ? C33 Cl2 1.671(10) . ? C33 Cl1 1.680(10) . ? C34 Cl3 1.639(10) . ? C34 Cl4 1.651(10) . ? C34 Cl4' 1.652(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N14 Zn1 N13 130.4(3) 2_656 . ? N14 Zn1 S12 87.5(2) 2_656 2_656 ? N13 Zn1 S12 116.3(3) . 2_656 ? N14 Zn1 S11 115.3(3) 2_656 . ? N13 Zn1 S11 86.6(3) . . ? S12 Zn1 S11 125.48(12) 2_656 . ? C6 Fe1 C12 129.5(6) . . ? C6 Fe1 C5 39.6(6) . . ? C12 Fe1 C5 109.6(5) . . ? C6 Fe1 C11 167.6(7) . . ? C12 Fe1 C11 40.1(5) . . ? C5 Fe1 C11 130.6(6) . . ? C6 Fe1 C9 118.4(6) . . ? C12 Fe1 C9 68.8(5) . . ? C5 Fe1 C9 151.7(6) . . ? C11 Fe1 C9 67.3(6) . . ? C6 Fe1 C10 152.7(7) . . ? C12 Fe1 C10 66.7(5) . . ? C5 Fe1 C10 166.5(6) . . ? C11 Fe1 C10 38.3(6) . . ? C9 Fe1 C10 40.7(6) . . ? C6 Fe1 C7 41.7(7) . . ? C12 Fe1 C7 168.8(6) . . ? C5 Fe1 C7 67.9(6) . . ? C11 Fe1 C7 149.7(7) . . ? C9 Fe1 C7 107.9(6) . . ? C10 Fe1 C7 118.4(7) . . ? C6 Fe1 C8 68.8(7) . . ? C12 Fe1 C8 151.6(6) . . ? C5 Fe1 C8 69.3(5) . . ? C11 Fe1 C8 117.9(6) . . ? C9 Fe1 C8 126.0(5) . . ? C10 Fe1 C8 107.4(6) . . ? C7 Fe1 C8 39.0(7) . . ? C6 Fe1 C13 108.7(5) . . ? C12 Fe1 C13 41.3(4) . . ? C5 Fe1 C13 119.0(4) . . ? C11 Fe1 C13 67.8(5) . . ? C9 Fe1 C13 40.8(4) . . ? C10 Fe1 C13 67.6(5) . . ? C7 Fe1 C13 129.4(5) . . ? C8 Fe1 C13 164.7(5) . . ? C6 Fe1 C4 68.2(5) . . ? C12 Fe1 C4 118.5(5) . . ? C5 Fe1 C4 41.1(5) . . ? C11 Fe1 C4 109.2(6) . . ? C9 Fe1 C4 165.4(5) . . ? C10 Fe1 C4 127.9(6) . . ? C7 Fe1 C4 67.4(5) . . ? C8 Fe1 C4 41.7(5) . . ? C13 Fe1 C4 152.7(4) . . ? C1 S11 Zn1 92.6(4) . . ? C16 S12 Zn1 92.8(4) . 2_656 ? C1 N12 N13 115.7(10) . . ? C2 N13 N12 116.3(9) . . ? C2 N13 Zn1 127.4(8) . . ? N12 N13 Zn1 115.0(6) . . ? C14 N14 N15 114.5(9) . . ? C14 N14 Zn1 128.6(8) . 2_656 ? N15 N14 Zn1 115.6(6) . 2_656 ? C16 N15 N14 115.5(9) . . ? N12 C1 N11 117.2(11) . . ? N12 C1 S11 128.8(9) . . ? N11 C1 S11 114.0(9) . . ? N13 C2 C4 118.7(10) . . ? N13 C2 C3 120.3(11) . . ? C4 C2 C3 121.0(10) . . ? C5 C4 C2 128.3(10) . . ? C5 C4 C8 106.5(11) . . ? C2 C4 C8 125.2(11) . . ? C5 C4 Fe1 68.3(6) . . ? C2 C4 Fe1 125.8(8) . . ? C8 C4 Fe1 69.1(6) . . ? C6 C5 C4 109.2(12) . . ? C6 C5 Fe1 70.0(8) . . ? C4 C5 Fe1 70.6(7) . . ? C5 C6 C7 107.5(14) . . ? C5 C6 Fe1 70.4(8) . . ? C7 C6 Fe1 69.9(9) . . ? C8 C7 C6 109.9(13) . . ? C8 C7 Fe1 71.1(8) . . ? C6 C7 Fe1 68.4(7) . . ? C7 C8 C4 106.9(14) . . ? C7 C8 Fe1 69.9(7) . . ? C4 C8 Fe1 69.2(6) . . ? C10 C9 C13 106.4(12) . . ? C10 C9 Fe1 69.7(7) . . ? C13 C9 Fe1 70.4(6) . . ? C11 C10 C9 110.0(12) . . ? C11 C10 Fe1 70.7(9) . . ? C9 C10 Fe1 69.6(8) . . ? C10 C11 C12 109.8(13) . . ? C10 C11 Fe1 70.9(9) . . ? C12 C11 Fe1 69.6(8) . . ? C11 C12 C13 107.3(11) . . ? C11 C12 Fe1 70.3(7) . . ? C13 C12 Fe1 70.5(6) . . ? C9 C13 C12 106.3(10) . . ? C9 C13 C14 124.8(11) . . ? C12 C13 C14 128.8(9) . . ? C9 C13 Fe1 68.8(6) . . ? C12 C13 Fe1 68.2(6) . . ? C14 C13 Fe1 126.2(7) . . ? N14 C14 C15 124.4(10) . . ? N14 C14 C13 116.5(10) . . ? C15 C14 C13 119.1(9) . . ? N15 C16 N16 117.1(10) . . ? N15 C16 S12 128.1(9) . . ? N16 C16 S12 114.8(7) . . ? N23 Zn2 N24 130.5(3) . 2 ? N23 Zn2 S21 87.1(3) . . ? N24 Zn2 S21 115.6(3) 2 . ? N23 Zn2 S22 113.2(3) . 2 ? N24 Zn2 S22 87.2(3) 2 2 ? S21 Zn2 S22 128.48(12) . 2 ? C27 Fe2 C23 152.1(6) . . ? C27 Fe2 C25 69.0(6) . . ? C23 Fe2 C25 127.0(6) . . ? C27 Fe2 C28 40.1(6) . . ? C23 Fe2 C28 118.8(6) . . ? C25 Fe2 C28 68.5(5) . . ? C27 Fe2 C21 106.9(6) . . ? C23 Fe2 C21 69.2(6) . . ? C25 Fe2 C21 153.1(5) . . ? C28 Fe2 C21 126.4(5) . . ? C27 Fe2 C22 118.8(7) . . ? C23 Fe2 C22 39.9(6) . . ? C25 Fe2 C22 163.8(6) . . ? C28 Fe2 C22 107.5(6) . . ? C21 Fe2 C22 41.8(6) . . ? C27 Fe2 C26 40.1(7) . . ? C23 Fe2 C26 166.3(7) . . ? C25 Fe2 C26 41.5(5) . . ? C28 Fe2 C26 67.5(7) . . ? C21 Fe2 C26 118.2(6) . . ? C22 Fe2 C26 153.0(7) . . ? C27 Fe2 C20 128.5(5) . . ? C23 Fe2 C20 67.6(5) . . ? C25 Fe2 C20 119.5(5) . . ? C28 Fe2 C20 165.4(4) . . ? C21 Fe2 C20 41.1(4) . . ? C22 Fe2 C20 68.2(5) . . ? C26 Fe2 C20 109.5(5) . . ? C27 Fe2 C29 69.4(5) . . ? C23 Fe2 C29 107.2(5) . . ? C25 Fe2 C29 39.9(5) . . ? C28 Fe2 C29 42.0(4) . . ? C21 Fe2 C29 165.6(5) . . ? C22 Fe2 C29 126.7(5) . . ? C26 Fe2 C29 68.5(5) . . ? C20 Fe2 C29 151.7(4) . . ? C27 Fe2 C24 165.7(6) . . ? C23 Fe2 C24 41.0(5) . . ? C25 Fe2 C24 107.1(5) . . ? C28 Fe2 C24 152.6(5) . . ? C21 Fe2 C24 70.0(5) . . ? C22 Fe2 C24 68.8(6) . . ? C26 Fe2 C24 128.1(6) . . ? C20 Fe2 C24 40.5(4) . . ? C29 Fe2 C24 117.1(4) . . ? C17 S21 Zn2 92.9(4) . . ? C32 S22 Zn2 93.0(4) . 2 ? C17 N22 N23 115.7(9) . . ? C18 N23 N22 116.0(9) . . ? C18 N23 Zn2 126.7(8) . . ? N22 N23 Zn2 115.6(6) . . ? C30 N24 N25 115.9(9) . . ? C30 N24 Zn2 127.2(8) . 2 ? N25 N24 Zn2 115.5(6) . 2 ? C32 N25 N24 115.0(8) . . ? N22 C17 N21 116.5(11) . . ? N22 C17 S21 128.1(9) . . ? N21 C17 S21 115.4(8) . . ? N23 C18 C20 118.2(10) . . ? N23 C18 C19 123.2(11) . . ? C20 C18 C19 118.6(10) . . ? C24 C20 C21 110.6(11) . . ? C24 C20 C18 125.8(10) . . ? C21 C20 C18 123.6(11) . . ? C24 C20 Fe2 70.5(6) . . ? C21 C20 Fe2 68.5(6) . . ? C18 C20 Fe2 126.7(8) . . ? C20 C21 C22 105.2(12) . . ? C20 C21 Fe2 70.3(6) . . ? C22 C21 Fe2 69.2(7) . . ? C23 C22 C21 108.6(12) . . ? C23 C22 Fe2 69.6(8) . . ? C21 C22 Fe2 69.0(7) . . ? C22 C23 C24 110.7(12) . . ? C22 C23 Fe2 70.5(9) . . ? C24 C23 Fe2 71.4(7) . . ? C20 C24 C23 104.9(11) . . ? C20 C24 Fe2 69.1(6) . . ? C23 C24 Fe2 67.6(7) . . ? C29 C25 C26 109.1(11) . . ? C29 C25 Fe2 71.3(7) . . ? C26 C25 Fe2 70.1(7) . . ? C27 C26 C25 107.4(13) . . ? C27 C26 Fe2 68.7(9) . . ? C25 C26 Fe2 68.4(7) . . ? C28 C27 C26 108.9(12) . . ? C28 C27 Fe2 70.3(8) . . ? C26 C27 Fe2 71.2(8) . . ? C27 C28 C29 108.8(13) . . ? C27 C28 Fe2 69.6(7) . . ? C29 C28 Fe2 70.2(6) . . ? C25 C29 C30 129.4(10) . . ? C25 C29 C28 105.7(11) . . ? C30 C29 C28 124.9(11) . . ? C25 C29 Fe2 68.8(6) . . ? C30 C29 Fe2 125.8(8) . . ? C28 C29 Fe2 67.8(6) . . ? N24 C30 C29 117.3(10) . . ? N24 C30 C31 122.6(11) . . ? C29 C30 C31 120.1(9) . . ? N25 C32 N26 116.7(10) . . ? N25 C32 S22 128.7(9) . . ? N26 C32 S22 114.6(8) . . ? Cl2 C33 Cl1 119.2(9) . . ? Cl3 C34 Cl4 150.4(19) . . ? Cl3 C34 Cl4' 116.6(13) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.056 _refine_diff_density_min -2.233 _refine_diff_density_rms 0.178