Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal SOciety of Chemistry 2008 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Chun-ying Duan' _publ_contact_author_address ; State Key Laboratory of Fine Chemicals Dalian University of Technology Dalian 116012 CHINA ; _publ_contact_author_email DUANCY@NJU.EDU.CN _publ_section_title ;Stereoselective Association of Ferrocene-contained Molecular Clips in Coordination Polymers ; loop_ _publ_author_name 'Chun-ying Duan.' 'Cheng He.' 'Yang Liu.' 'Lixia Xie.' 'Bing-guang Zhang.' # Attachment 'complex 1and 1.cif' data_complex1 _database_code_depnum_ccdc_archive 'CCDC 662089' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H26 Fe N6 O4 Zn' _chemical_formula_weight 559.71 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' 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.0436(5) _cell_length_b 12.9919(6) _cell_length_c 16.8564(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2418.5(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 block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.537 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 1.632 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7361 _exptl_absorpt_correction_T_max 0.7723 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10257 _diffrn_reflns_av_R_equivalents 0.0745 _diffrn_reflns_av_sigmaI/netI 0.0649 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4029 _reflns_number_gt 3400 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0290P)^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 'riding mode' _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 0.026(15) _refine_ls_number_reflns 4029 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0451 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0802 _refine_ls_wR_factor_gt 0.0779 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _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 0.36517(4) 0.65629(3) 0.02977(3) 0.04249(14) Uani 1 1 d . . . Fe1 Fe -0.23455(5) 0.68757(4) 0.32591(4) 0.04576(17) Uani 1 1 d . . . N1 N -0.2458(3) 0.8680(2) 0.06455(19) 0.0450(9) Uani 1 1 d . . . N2 N -0.3226(4) 0.9414(3) 0.1729(2) 0.0598(10) Uani 1 1 d . . . N3 N -0.3634(3) 0.8431(2) 0.16419(19) 0.0468(8) Uani 1 1 d . . . N4 N 0.1263(3) 0.7136(2) 0.2132(2) 0.0475(8) Uani 1 1 d . . . N5 N 0.2005(3) 0.6484(3) 0.2530(2) 0.0559(10) Uani 1 1 d . . . N6 N 0.2626(3) 0.6672(3) 0.12825(18) 0.0436(8) Uani 1 1 d . . . O1 O 0.4580(3) 0.5293(2) 0.01312(19) 0.0646(9) Uani 1 1 d . . . O2 O 0.5377(3) 0.5762(2) 0.1251(2) 0.0676(9) Uani 1 1 d . . . O3 O 0.4598(3) 0.7775(2) 0.00120(18) 0.0523(8) Uani 1 1 d . . . O4 O 0.2903(3) 0.8651(2) 0.0155(2) 0.0643(9) Uani 1 1 d . . . C1 C -0.3176(4) 0.8027(3) 0.0998(2) 0.0445(10) Uani 1 1 d . . . H1A H -0.3340 0.7365 0.0817 0.053 Uiso 1 1 calc R . . C2 C -0.2511(5) 0.9532(3) 0.1108(3) 0.0593(12) Uani 1 1 d . . . H2A H -0.2089 1.0135 0.0999 0.071 Uiso 1 1 calc R . . C3 C -0.4452(4) 0.7958(3) 0.2225(3) 0.0501(11) Uani 1 1 d . . . H3A H -0.4691 0.7283 0.2018 0.060 Uiso 1 1 calc R . . C4 C -0.5560(4) 0.8586(4) 0.2304(3) 0.0638(13) Uani 1 1 d . . . H4A H -0.5935 0.8662 0.1794 0.096 Uiso 1 1 calc R . . H4B H -0.5353 0.9253 0.2510 0.096 Uiso 1 1 calc R . . H4C H -0.6113 0.8252 0.2661 0.096 Uiso 1 1 calc R . . C5 C -0.3802(4) 0.7783(3) 0.3003(2) 0.0507(11) Uani 1 1 d . . . C6 C -0.4150(4) 0.6973(4) 0.3542(3) 0.0666(14) Uani 1 1 d . . . H6A H -0.4773 0.6446 0.3458 0.080 Uiso 1 1 calc R . . C7 C -0.3403(5) 0.7108(5) 0.4233(3) 0.0790(17) Uani 1 1 d . . . H7A H -0.3418 0.6667 0.4705 0.095 Uiso 1 1 calc R . . C8 C -0.2625(5) 0.7958(4) 0.4121(3) 0.0713(15) Uani 1 1 d . . . H8A H -0.2021 0.8212 0.4500 0.086 Uiso 1 1 calc R . . C9 C -0.2885(4) 0.8382(4) 0.3370(3) 0.0573(12) Uani 1 1 d . . . H9A H -0.2478 0.8977 0.3133 0.069 Uiso 1 1 calc R . . C10 C -0.0722(4) 0.6161(3) 0.3431(3) 0.0481(11) Uani 1 1 d . . . H10A H -0.0196 0.6249 0.3894 0.058 Uiso 1 1 calc R . . C11 C -0.1651(4) 0.5428(3) 0.3359(3) 0.0600(13) Uani 1 1 d . . . H11A H -0.1878 0.4912 0.3755 0.072 Uiso 1 1 calc R . . C12 C -0.2178(5) 0.5564(4) 0.2623(3) 0.0666(14) Uani 1 1 d . . . H12A H -0.2851 0.5157 0.2411 0.080 Uiso 1 1 calc R . . C13 C -0.1594(4) 0.6381(4) 0.2223(3) 0.0542(12) Uani 1 1 d . . . H13A H -0.1787 0.6635 0.1690 0.065 Uiso 1 1 calc R . . C14 C -0.0682(3) 0.6765(3) 0.2729(2) 0.0402(9) Uani 1 1 d . . . C15 C 0.0195(4) 0.7607(3) 0.2531(3) 0.0562(12) Uani 1 1 d . . . H15A H -0.0199 0.8067 0.2150 0.067 Uiso 1 1 calc R . . C16 C 0.0593(6) 0.8239(5) 0.3218(4) 0.127(3) Uani 1 1 d . . . H16A H 0.1134 0.8768 0.3037 0.190 Uiso 1 1 calc R . . H16B H 0.1003 0.7809 0.3595 0.190 Uiso 1 1 calc R . . H16C H -0.0101 0.8549 0.3465 0.190 Uiso 1 1 calc R . . C17 C 0.2797(4) 0.6232(3) 0.1999(3) 0.0507(11) Uani 1 1 d . . . H17A H 0.3434 0.5783 0.2102 0.061 Uiso 1 1 calc R . . C18 C 0.1646(4) 0.7246(3) 0.1391(2) 0.0451(11) Uani 1 1 d . . . H18A H 0.1285 0.7659 0.1008 0.054 Uiso 1 1 calc R . . C19 C 0.5327(4) 0.5178(3) 0.0682(3) 0.0468(10) Uani 1 1 d . . . C20 C 0.6168(5) 0.4281(3) 0.0620(3) 0.0599(13) Uani 1 1 d . . . H20A H 0.6692 0.4267 0.1074 0.090 Uiso 1 1 calc R . . H20B H 0.6645 0.4343 0.0147 0.090 Uiso 1 1 calc R . . H20C H 0.5706 0.3655 0.0599 0.090 Uiso 1 1 calc R . . C21 C 0.3987(4) 0.8596(3) 0.0004(2) 0.0497(11) Uani 1 1 d . . . C22 C 0.4675(5) 0.9570(3) -0.0221(4) 0.0811(16) Uani 1 1 d . . . H22A H 0.4133 1.0148 -0.0210 0.122 Uiso 1 1 calc R . . H22B H 0.5004 0.9495 -0.0744 0.122 Uiso 1 1 calc R . . H22C H 0.5321 0.9682 0.0151 0.122 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 0.0475(3) 0.0505(3) 0.0295(2) 0.0000(2) 0.0019(2) 0.0019(2) Fe1 0.0436(3) 0.0556(4) 0.0381(3) 0.0034(3) 0.0072(3) 0.0041(3) N1 0.050(2) 0.050(2) 0.0355(19) -0.0028(16) 0.0054(17) -0.0097(18) N2 0.080(3) 0.055(2) 0.045(2) -0.010(2) 0.016(2) -0.0019(19) N3 0.0491(19) 0.0508(19) 0.0406(19) 0.0011(18) 0.0078(18) -0.0028(18) N4 0.050(2) 0.0479(19) 0.045(2) 0.0092(17) 0.0184(19) -0.0016(18) N5 0.060(2) 0.069(2) 0.038(2) 0.018(2) 0.0104(18) 0.011(2) N6 0.045(2) 0.052(2) 0.0331(19) 0.0009(16) 0.0020(16) -0.0001(18) O1 0.074(2) 0.070(2) 0.050(2) -0.0041(17) -0.0124(18) 0.0207(17) O2 0.073(2) 0.061(2) 0.069(2) -0.0209(19) 0.0067(19) 0.0046(17) O3 0.0502(18) 0.0447(17) 0.062(2) 0.0088(14) 0.0042(15) 0.0059(14) O4 0.055(2) 0.069(2) 0.069(2) 0.0009(18) 0.0022(17) 0.0108(15) C1 0.046(2) 0.051(2) 0.036(2) -0.001(2) -0.007(2) -0.001(2) C2 0.079(4) 0.053(3) 0.045(3) -0.003(2) 0.011(3) -0.013(3) C3 0.054(3) 0.052(3) 0.044(3) 0.002(2) 0.010(2) 0.003(2) C4 0.057(3) 0.087(4) 0.047(3) -0.009(3) 0.002(2) 0.003(3) C5 0.039(3) 0.070(3) 0.043(3) 0.007(2) 0.013(2) 0.013(2) C6 0.045(3) 0.100(4) 0.054(3) 0.023(3) 0.020(2) 0.011(3) C7 0.074(4) 0.116(5) 0.047(3) 0.022(3) 0.021(3) 0.036(4) C8 0.080(4) 0.085(4) 0.049(3) -0.013(3) 0.001(3) 0.031(3) C9 0.071(3) 0.059(3) 0.042(3) -0.001(2) 0.009(2) 0.019(2) C10 0.045(3) 0.055(3) 0.044(3) 0.005(2) 0.004(2) 0.009(2) C11 0.058(3) 0.041(2) 0.081(4) 0.005(3) 0.016(3) -0.002(2) C12 0.050(3) 0.067(3) 0.082(4) -0.022(3) 0.008(3) -0.010(2) C13 0.050(3) 0.074(3) 0.039(2) -0.009(2) 0.001(2) 0.013(2) C14 0.039(2) 0.041(2) 0.040(2) 0.0002(19) 0.0095(19) 0.0011(18) C15 0.059(3) 0.050(3) 0.059(3) 0.002(2) 0.020(2) 0.004(2) C16 0.118(5) 0.114(5) 0.149(6) -0.074(5) 0.074(5) -0.059(4) C17 0.046(3) 0.058(3) 0.048(3) 0.015(2) 0.005(2) 0.006(2) C18 0.051(3) 0.051(2) 0.034(2) 0.0056(19) 0.001(2) 0.003(2) C19 0.051(3) 0.047(2) 0.043(3) -0.003(2) 0.006(2) -0.002(2) C20 0.072(3) 0.063(3) 0.045(3) 0.001(2) -0.001(2) 0.024(3) C21 0.061(3) 0.052(3) 0.037(2) 0.003(2) -0.007(2) -0.005(2) C22 0.080(4) 0.054(3) 0.110(5) 0.013(3) -0.003(4) 0.002(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 O3 1.951(3) . ? Zn1 O1 1.963(3) . ? Zn1 N6 2.015(3) . ? Zn1 N1 2.032(3) 4_565 ? Fe1 C12 2.023(5) . ? Fe1 C11 2.038(4) . ? Fe1 C13 2.038(4) . ? Fe1 C7 2.038(5) . ? Fe1 C10 2.040(4) . ? Fe1 C5 2.040(4) . ? Fe1 C8 2.046(5) . ? Fe1 C14 2.048(4) . ? Fe1 C6 2.053(4) . ? Fe1 C9 2.054(4) . ? N1 C1 1.305(5) . ? N1 C2 1.355(5) . ? N1 Zn1 2.032(3) 4_465 ? N2 C2 1.320(6) . ? N2 N3 1.362(5) . ? N3 C1 1.307(5) . ? N3 C3 1.470(5) . ? N4 C18 1.326(5) . ? N4 N5 1.357(5) . ? N4 C15 1.489(5) . ? N5 C17 1.294(5) . ? N6 C18 1.327(5) . ? N6 C17 1.349(5) . ? O1 C19 1.251(5) . ? O2 C19 1.225(5) . ? O3 C21 1.262(5) . ? O4 C21 1.225(5) . ? C1 H1A 0.9300 . ? C2 H2A 0.9300 . ? C3 C4 1.477(6) . ? C3 C5 1.511(6) . ? C3 H3A 0.9800 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C9 1.419(7) . ? C5 C6 1.444(6) . ? C6 C7 1.438(7) . ? C6 H6A 0.9800 . ? C7 C8 1.411(7) . ? C7 H7A 0.9800 . ? C8 C9 1.410(6) . ? C8 H8A 0.9800 . ? C9 H9A 0.9800 . ? C10 C11 1.405(6) . ? C10 C14 1.421(6) . ? C10 H10A 0.9800 . ? C11 C12 1.382(7) . ? C11 H11A 0.9800 . ? C12 C13 1.413(6) . ? C12 H12A 0.9800 . ? C13 C14 1.411(6) . ? C13 H13A 0.9800 . ? C14 C15 1.498(6) . ? C15 C16 1.486(7) . ? C15 H15A 0.9800 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? C19 C20 1.494(6) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.525(6) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? 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 O3 Zn1 O1 111.32(13) . . ? O3 Zn1 N6 116.60(13) . . ? O1 Zn1 N6 118.09(14) . . ? O3 Zn1 N1 104.80(13) . 4_565 ? O1 Zn1 N1 94.17(13) . 4_565 ? N6 Zn1 N1 108.45(13) . 4_565 ? C12 Fe1 C11 39.8(2) . . ? C12 Fe1 C13 40.73(18) . . ? C11 Fe1 C13 68.1(2) . . ? C12 Fe1 C7 127.2(2) . . ? C11 Fe1 C7 106.6(2) . . ? C13 Fe1 C7 166.2(2) . . ? C12 Fe1 C10 67.11(19) . . ? C11 Fe1 C10 40.30(17) . . ? C13 Fe1 C10 67.67(17) . . ? C7 Fe1 C10 117.2(2) . . ? C12 Fe1 C5 116.5(2) . . ? C11 Fe1 C5 147.9(2) . . ? C13 Fe1 C5 108.76(17) . . ? C7 Fe1 C5 68.49(19) . . ? C10 Fe1 C5 170.37(17) . . ? C12 Fe1 C8 165.9(2) . . ? C11 Fe1 C8 129.2(2) . . ? C13 Fe1 C8 152.5(2) . . ? C7 Fe1 C8 40.4(2) . . ? C10 Fe1 C8 110.2(2) . . ? C5 Fe1 C8 68.56(19) . . ? C12 Fe1 C14 68.12(18) . . ? C11 Fe1 C14 68.52(17) . . ? C13 Fe1 C14 40.40(17) . . ? C7 Fe1 C14 151.2(2) . . ? C10 Fe1 C14 40.68(16) . . ? C5 Fe1 C14 130.91(17) . . ? C8 Fe1 C14 119.6(2) . . ? C12 Fe1 C6 105.3(2) . . ? C11 Fe1 C6 113.7(2) . . ? C13 Fe1 C6 127.9(2) . . ? C7 Fe1 C6 41.2(2) . . ? C10 Fe1 C6 148.00(18) . . ? C5 Fe1 C6 41.31(18) . . ? C8 Fe1 C6 69.3(2) . . ? C14 Fe1 C6 167.54(19) . . ? C12 Fe1 C9 151.4(2) . . ? C11 Fe1 C9 168.7(2) . . ? C13 Fe1 C9 119.79(18) . . ? C7 Fe1 C9 67.6(2) . . ? C10 Fe1 C9 132.50(19) . . ? C5 Fe1 C9 40.56(18) . . ? C8 Fe1 C9 40.23(17) . . ? C14 Fe1 C9 111.51(18) . . ? C6 Fe1 C9 68.8(2) . . ? C1 N1 C2 104.0(4) . . ? C1 N1 Zn1 128.5(3) . 4_465 ? C2 N1 Zn1 127.1(3) . 4_465 ? C2 N2 N3 102.7(3) . . ? C1 N3 N2 109.8(3) . . ? C1 N3 C3 128.7(4) . . ? N2 N3 C3 121.5(3) . . ? C18 N4 N5 109.9(3) . . ? C18 N4 C15 129.4(4) . . ? N5 N4 C15 120.7(3) . . ? C17 N5 N4 102.9(3) . . ? C18 N6 C17 103.2(3) . . ? C18 N6 Zn1 127.7(3) . . ? C17 N6 Zn1 129.0(3) . . ? C19 O1 Zn1 109.8(3) . . ? C21 O3 Zn1 113.4(3) . . ? N1 C1 N3 110.6(4) . . ? N1 C1 H1A 124.7 . . ? N3 C1 H1A 124.7 . . ? N2 C2 N1 112.8(4) . . ? N2 C2 H2A 123.6 . . ? N1 C2 H2A 123.6 . . ? N3 C3 C4 109.8(4) . . ? N3 C3 C5 110.6(4) . . ? C4 C3 C5 113.5(4) . . ? N3 C3 H3A 107.6 . . ? C4 C3 H3A 107.6 . . ? C5 C3 H3A 107.6 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C9 C5 C6 108.3(4) . . ? C9 C5 C3 129.4(4) . . ? C6 C5 C3 122.0(4) . . ? C9 C5 Fe1 70.2(3) . . ? C6 C5 Fe1 69.8(2) . . ? C3 C5 Fe1 130.2(3) . . ? C7 C6 C5 105.5(5) . . ? C7 C6 Fe1 68.9(3) . . ? C5 C6 Fe1 68.9(2) . . ? C7 C6 H6A 127.2 . . ? C5 C6 H6A 127.2 . . ? Fe1 C6 H6A 127.2 . . ? C8 C7 C6 109.7(5) . . ? C8 C7 Fe1 70.1(3) . . ? C6 C7 Fe1 70.0(3) . . ? C8 C7 H7A 125.2 . . ? C6 C7 H7A 125.2 . . ? Fe1 C7 H7A 125.2 . . ? C9 C8 C7 107.6(5) . . ? C9 C8 Fe1 70.2(3) . . ? C7 C8 Fe1 69.5(3) . . ? C9 C8 H8A 126.2 . . ? C7 C8 H8A 126.2 . . ? Fe1 C8 H8A 126.2 . . ? C8 C9 C5 108.9(5) . . ? C8 C9 Fe1 69.6(3) . . ? C5 C9 Fe1 69.2(3) . . ? C8 C9 H9A 125.6 . . ? C5 C9 H9A 125.6 . . ? Fe1 C9 H9A 125.6 . . ? C11 C10 C14 109.0(4) . . ? C11 C10 Fe1 69.8(2) . . ? C14 C10 Fe1 70.0(2) . . ? C11 C10 H10A 125.5 . . ? C14 C10 H10A 125.5 . . ? Fe1 C10 H10A 125.5 . . ? C12 C11 C10 107.4(4) . . ? C12 C11 Fe1 69.5(3) . . ? C10 C11 Fe1 69.9(2) . . ? C12 C11 H11A 126.3 . . ? C10 C11 H11A 126.3 . . ? Fe1 C11 H11A 126.3 . . ? C11 C12 C13 109.4(4) . . ? C11 C12 Fe1 70.7(3) . . ? C13 C12 Fe1 70.2(3) . . ? C11 C12 H12A 125.3 . . ? C13 C12 H12A 125.3 . . ? Fe1 C12 H12A 125.3 . . ? C14 C13 C12 107.7(4) . . ? C14 C13 Fe1 70.2(2) . . ? C12 C13 Fe1 69.1(3) . . ? C14 C13 H13A 126.2 . . ? C12 C13 H13A 126.2 . . ? Fe1 C13 H13A 126.2 . . ? C13 C14 C10 106.6(4) . . ? C13 C14 C15 125.8(4) . . ? C10 C14 C15 127.5(4) . . ? C13 C14 Fe1 69.4(2) . . ? C10 C14 Fe1 69.3(2) . . ? C15 C14 Fe1 128.7(3) . . ? C16 C15 N4 110.2(4) . . ? C16 C15 C14 114.9(4) . . ? N4 C15 C14 108.2(3) . . ? C16 C15 H15A 107.8 . . ? N4 C15 H15A 107.8 . . ? C14 C15 H15A 107.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N5 C17 N6 114.7(4) . . ? N5 C17 H17A 122.6 . . ? N6 C17 H17A 122.6 . . ? N4 C18 N6 109.3(4) . . ? N4 C18 H18A 125.4 . . ? N6 C18 H18A 125.4 . . ? O2 C19 O1 122.5(4) . . ? O2 C19 C20 120.7(4) . . ? O1 C19 C20 116.8(4) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O4 C21 O3 124.8(4) . . ? O4 C21 C22 119.3(4) . . ? O3 C21 C22 115.9(4) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.339 _refine_diff_density_min -0.218 _refine_diff_density_rms 0.055 #===========================END============================= data_complex1' _database_code_depnum_ccdc_archive 'CCDC 662090' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H26 Fe N6 O4 Zn' _chemical_formula_weight 559.71 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' 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P2(1)2(1)2(1) ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.0485(3) _cell_length_b 12.9858(4) _cell_length_c 16.8845(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2422.48(12) _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 yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 1.629 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2236 _exptl_absorpt_correction_T_max 0.2790 _exptl_absorpt_process_details ? _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17836 _diffrn_reflns_av_R_equivalents 0.0684 _diffrn_reflns_av_sigmaI/netI 0.0518 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.51 _reflns_number_total 4467 _reflns_number_gt 3786 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0169P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.015(11) _refine_ls_number_reflns 4467 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0383 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0596 _refine_ls_wR_factor_gt 0.0579 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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 0.63338(3) 0.15591(3) 0.03024(2) 0.04006(10) Uani 1 1 d . . . Fe1 Fe 1.23371(4) 0.18644(3) 0.32537(3) 0.04243(13) Uani 1 1 d . . . N1 N 1.2441(2) 0.36740(18) 0.06388(13) 0.0405(6) Uani 1 1 d . . . N2 N 1.3226(3) 0.4404(2) 0.17223(17) 0.0557(8) Uani 1 1 d . . . N3 N 1.3625(2) 0.34231(18) 0.16398(14) 0.0408(6) Uani 1 1 d . . . N4 N 0.8721(2) 0.21340(18) 0.21401(15) 0.0434(6) Uani 1 1 d . . . N5 N 0.7982(2) 0.1483(2) 0.25406(16) 0.0526(7) Uani 1 1 d . . . N6 N 0.7353(2) 0.16731(19) 0.12908(14) 0.0399(6) Uani 1 1 d . . . C1 C 1.2511(3) 0.4522(2) 0.1106(2) 0.0547(9) Uani 1 1 d . . . H1A H 1.2094 0.5128 0.1001 0.066 Uiso 1 1 calc R . . C2 C 1.3159(3) 0.3008(2) 0.09879(17) 0.0400(7) Uani 1 1 d . . . H2A H 1.3317 0.2345 0.0806 0.048 Uiso 1 1 calc R . . C3 C 1.4432(3) 0.2946(2) 0.22209(18) 0.0443(8) Uani 1 1 d . . . H3A H 1.4672 0.2271 0.2014 0.053 Uiso 1 1 calc R . . C4 C 1.5565(3) 0.3592(3) 0.2299(2) 0.0530(9) Uani 1 1 d . . . H4A H 1.5933 0.3673 0.1788 0.079 Uiso 1 1 calc R . . H4B H 1.6122 0.3257 0.2651 0.079 Uiso 1 1 calc R . . H4C H 1.5358 0.4256 0.2509 0.079 Uiso 1 1 calc R . . C5 C 1.3795(3) 0.2773(2) 0.29923(18) 0.0458(8) Uani 1 1 d . . . C6 C 1.4135(3) 0.1971(3) 0.3530(2) 0.0582(10) Uani 1 1 d . . . H6A H 1.4754 0.1442 0.3440 0.070 Uiso 1 1 calc R . . C7 C 1.3406(4) 0.2088(3) 0.4224(2) 0.0708(12) Uani 1 1 d . . . H7A H 1.3432 0.1645 0.4694 0.085 Uiso 1 1 calc R . . C8 C 1.2625(4) 0.2942(3) 0.4114(2) 0.0664(11) Uani 1 1 d . . . H8A H 1.2024 0.3197 0.4494 0.080 Uiso 1 1 calc R . . C9 C 1.2877(3) 0.3366(3) 0.33626(19) 0.0515(9) Uani 1 1 d . . . H9A H 1.2467 0.3961 0.3128 0.062 Uiso 1 1 calc R . . C10 C 1.0710(3) 0.1152(2) 0.3433(2) 0.0459(8) Uani 1 1 d . . . H10A H 1.0189 0.1239 0.3898 0.055 Uiso 1 1 calc R . . C11 C 1.1629(3) 0.0417(2) 0.3353(2) 0.0590(10) Uani 1 1 d . . . H11A H 1.1857 -0.0100 0.3748 0.071 Uiso 1 1 calc R . . C12 C 1.2170(3) 0.0555(3) 0.2613(2) 0.0616(10) Uani 1 1 d . . . H12A H 1.2838 0.0146 0.2397 0.074 Uiso 1 1 calc R . . C13 C 1.1571(3) 0.1366(3) 0.22231(19) 0.0487(8) Uani 1 1 d . . . H13A H 1.1759 0.1624 0.1692 0.058 Uiso 1 1 calc R . . C14 C 1.0669(3) 0.1759(2) 0.27341(19) 0.0379(7) Uani 1 1 d . . . C15 C 0.9796(3) 0.2594(3) 0.2534(2) 0.0505(9) Uani 1 1 d . . . H15A H 1.0188 0.3059 0.2156 0.061 Uiso 1 1 calc R . . C16 C 0.9391(4) 0.3221(4) 0.3231(3) 0.1063(17) Uani 1 1 d . . . H16A H 0.8843 0.3747 0.3056 0.159 Uiso 1 1 calc R . . H16B H 1.0082 0.3534 0.3478 0.159 Uiso 1 1 calc R . . H16C H 0.8989 0.2782 0.3606 0.159 Uiso 1 1 calc R . . C17 C 0.7179(3) 0.1228(2) 0.20071(18) 0.0467(8) Uani 1 1 d . . . H17A H 0.6542 0.0780 0.2111 0.056 Uiso 1 1 calc R . . C18 C 0.8341(3) 0.2243(2) 0.14007(19) 0.0434(8) Uani 1 1 d . . . H18A H 0.8707 0.2653 0.1018 0.052 Uiso 1 1 calc R . . O3 O 0.53866(18) 0.27727(16) 0.00157(13) 0.0508(6) Uani 1 1 d . . . C21 C 0.6000(3) 0.3601(2) 0.00041(19) 0.0463(8) Uani 1 1 d . . . O1 O 0.5417(2) 0.02832(17) 0.01319(15) 0.0617(7) Uani 1 1 d . . . O2 O 0.4600(2) 0.07584(18) 0.12508(15) 0.0635(7) Uani 1 1 d . . . C19 C 0.4660(3) 0.0171(3) 0.0685(2) 0.0436(8) Uani 1 1 d . . . O4 O 0.7087(2) 0.36469(17) 0.01615(15) 0.0619(7) Uani 1 1 d . . . C22 C 0.5326(3) 0.4570(2) -0.0214(3) 0.0736(12) Uani 1 1 d . . . H22A H 0.5871 0.5145 -0.0202 0.110 Uiso 1 1 calc R . . H22B H 0.4681 0.4682 0.0157 0.110 Uiso 1 1 calc R . . H22C H 0.4995 0.4499 -0.0737 0.110 Uiso 1 1 calc R . . C20 C 0.3827(3) -0.0735(2) 0.0623(2) 0.0587(10) Uani 1 1 d . . . H20A H 0.3296 -0.0748 0.1072 0.088 Uiso 1 1 calc R . . H20B H 0.4295 -0.1358 0.0609 0.088 Uiso 1 1 calc R . . H20C H 0.3357 -0.0681 0.0146 0.088 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 0.0387(2) 0.0489(2) 0.03259(19) 0.00017(17) -0.00099(18) -0.00223(17) Fe1 0.0353(3) 0.0509(3) 0.0411(3) 0.0027(2) -0.0068(2) -0.0029(2) N1 0.0404(15) 0.0453(15) 0.0357(14) -0.0005(12) -0.0031(13) 0.0059(13) N2 0.070(2) 0.0494(17) 0.0474(17) -0.0120(14) -0.0150(17) 0.0067(14) N3 0.0402(14) 0.0424(14) 0.0398(14) -0.0010(13) -0.0046(13) 0.0021(13) N4 0.0386(15) 0.0474(15) 0.0442(16) 0.0082(13) -0.0118(15) -0.0012(14) N5 0.0493(17) 0.0656(18) 0.0429(17) 0.0147(15) -0.0113(14) -0.0090(15) N6 0.0343(14) 0.0471(15) 0.0381(15) 0.0018(12) -0.0029(12) -0.0011(14) C1 0.065(2) 0.0470(19) 0.052(2) -0.0013(17) -0.010(2) 0.0140(19) C2 0.0356(17) 0.0476(18) 0.0366(19) -0.0032(15) 0.0059(15) -0.0009(15) C3 0.0422(19) 0.0477(19) 0.043(2) -0.0016(16) -0.0093(16) 0.0003(16) C4 0.045(2) 0.065(2) 0.049(2) -0.0056(18) -0.0014(17) -0.0056(18) C5 0.0379(19) 0.059(2) 0.040(2) 0.0018(16) -0.0106(17) -0.0128(17) C6 0.0425(19) 0.077(2) 0.055(2) 0.019(2) -0.0178(18) -0.0107(19) C7 0.064(3) 0.105(3) 0.044(2) 0.022(2) -0.019(2) -0.027(2) C8 0.066(3) 0.081(3) 0.052(2) -0.017(2) 0.006(2) -0.023(2) C9 0.056(2) 0.052(2) 0.046(2) -0.0082(18) -0.0060(18) -0.0157(18) C10 0.0409(19) 0.054(2) 0.043(2) 0.0046(16) -0.0044(16) -0.0110(17) C11 0.049(2) 0.0423(19) 0.085(3) 0.011(2) -0.017(2) -0.0011(17) C12 0.042(2) 0.059(2) 0.084(3) -0.023(2) -0.006(2) 0.0073(18) C13 0.042(2) 0.062(2) 0.0418(19) -0.0077(16) -0.0028(17) -0.0143(17) C14 0.0333(16) 0.0377(18) 0.0426(19) -0.0004(15) -0.0090(14) 0.0003(14) C15 0.049(2) 0.047(2) 0.055(2) 0.0013(17) -0.0186(18) -0.0002(17) C16 0.092(3) 0.099(3) 0.128(4) -0.053(3) -0.054(3) 0.042(3) C17 0.040(2) 0.053(2) 0.046(2) 0.0119(16) -0.0029(17) -0.0070(16) C18 0.043(2) 0.0508(19) 0.0368(19) 0.0072(15) -0.0025(16) -0.0045(16) O3 0.0434(14) 0.0463(13) 0.0627(16) 0.0090(11) -0.0040(12) -0.0029(11) C21 0.052(2) 0.048(2) 0.0392(19) 0.0023(15) 0.0070(16) 0.0037(17) O1 0.0608(17) 0.0668(15) 0.0576(17) -0.0026(13) 0.0110(14) -0.0176(13) O2 0.0672(16) 0.0610(15) 0.0624(17) -0.0190(13) -0.0028(14) -0.0061(13) C19 0.040(2) 0.0453(19) 0.045(2) 0.0012(16) -0.0057(17) 0.0007(16) O4 0.0488(15) 0.0684(15) 0.0686(17) 0.0007(13) -0.0053(13) -0.0085(12) C22 0.072(3) 0.049(2) 0.100(3) 0.013(2) 0.004(3) -0.0005(19) C20 0.066(2) 0.064(2) 0.047(2) 0.0000(17) -0.0014(19) -0.025(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 O3 1.953(2) . ? Zn1 O1 1.963(2) . ? Zn1 N6 2.018(2) . ? Zn1 N1 2.028(2) 4_455 ? Fe1 C12 2.024(3) . ? Fe1 C7 2.040(3) . ? Fe1 C13 2.040(3) . ? Fe1 C8 2.042(3) . ? Fe1 C11 2.043(3) . ? Fe1 C10 2.044(3) . ? Fe1 C5 2.045(3) . ? Fe1 C14 2.046(3) . ? Fe1 C6 2.046(3) . ? Fe1 C9 2.047(3) . ? N1 C2 1.313(4) . ? N1 C1 1.357(4) . ? N1 Zn1 2.028(2) 4 ? N2 C1 1.314(4) . ? N2 N3 1.356(3) . ? N3 C2 1.330(3) . ? N3 C3 1.463(4) . ? N4 C18 1.325(4) . ? N4 N5 1.356(3) . ? N4 C15 1.487(4) . ? N5 C17 1.307(4) . ? N6 C18 1.332(4) . ? N6 C17 1.354(4) . ? C1 H1A 0.9300 . ? C2 H2A 0.9300 . ? C3 C5 1.498(4) . ? C3 C4 1.512(4) . ? C3 H3A 0.9800 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C9 1.419(4) . ? C5 C6 1.432(4) . ? C6 C7 1.431(5) . ? C6 H6A 0.9800 . ? C7 C8 1.418(5) . ? C7 H7A 0.9800 . ? C8 C9 1.411(4) . ? C8 H8A 0.9800 . ? C9 H9A 0.9800 . ? C10 C11 1.400(4) . ? C10 C14 1.420(4) . ? C10 H10A 0.9800 . ? C11 C12 1.397(5) . ? C11 H11A 0.9800 . ? C12 C13 1.407(4) . ? C12 H12A 0.9800 . ? C13 C14 1.413(4) . ? C13 H13A 0.9800 . ? C14 C15 1.490(4) . ? C15 C16 1.499(5) . ? C15 H15A 0.9800 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? O3 C21 1.272(3) . ? C21 O4 1.232(4) . ? C21 C22 1.508(4) . ? O1 C19 1.262(4) . ? O2 C19 1.225(4) . ? C19 C20 1.497(4) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? 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 O3 Zn1 O1 111.60(9) . . ? O3 Zn1 N6 116.40(10) . . ? O1 Zn1 N6 118.10(10) . . ? O3 Zn1 N1 104.44(9) . 4_455 ? O1 Zn1 N1 94.04(10) . 4_455 ? N6 Zn1 N1 108.81(9) . 4_455 ? C12 Fe1 C7 126.98(17) . . ? C12 Fe1 C13 40.51(13) . . ? C7 Fe1 C13 165.94(16) . . ? C12 Fe1 C8 166.01(17) . . ? C7 Fe1 C8 40.64(15) . . ? C13 Fe1 C8 152.70(16) . . ? C12 Fe1 C11 40.17(15) . . ? C7 Fe1 C11 106.67(15) . . ? C13 Fe1 C11 67.60(14) . . ? C8 Fe1 C11 129.20(15) . . ? C12 Fe1 C10 67.59(14) . . ? C7 Fe1 C10 117.02(14) . . ? C13 Fe1 C10 67.54(13) . . ? C8 Fe1 C10 109.99(15) . . ? C11 Fe1 C10 40.05(12) . . ? C12 Fe1 C5 116.18(15) . . ? C7 Fe1 C5 68.62(14) . . ? C13 Fe1 C5 109.01(12) . . ? C8 Fe1 C5 68.62(14) . . ? C11 Fe1 C5 148.25(15) . . ? C10 Fe1 C5 170.32(13) . . ? C12 Fe1 C14 68.43(13) . . ? C7 Fe1 C14 151.07(15) . . ? C13 Fe1 C14 40.47(12) . . ? C8 Fe1 C14 119.42(15) . . ? C11 Fe1 C14 68.18(13) . . ? C10 Fe1 C14 40.62(12) . . ? C5 Fe1 C14 130.98(12) . . ? C12 Fe1 C6 105.50(16) . . ? C7 Fe1 C6 41.00(14) . . ? C13 Fe1 C6 128.23(14) . . ? C8 Fe1 C6 68.92(16) . . ? C11 Fe1 C6 114.57(14) . . ? C10 Fe1 C6 148.32(14) . . ? C5 Fe1 C6 40.98(12) . . ? C14 Fe1 C6 167.78(14) . . ? C12 Fe1 C9 151.01(16) . . ? C7 Fe1 C9 67.91(15) . . ? C13 Fe1 C9 119.97(13) . . ? C8 Fe1 C9 40.36(12) . . ? C11 Fe1 C9 168.68(16) . . ? C10 Fe1 C9 132.37(14) . . ? C5 Fe1 C9 40.57(12) . . ? C14 Fe1 C9 111.39(13) . . ? C6 Fe1 C9 68.42(14) . . ? C2 N1 C1 103.8(3) . . ? C2 N1 Zn1 128.1(2) . 4 ? C1 N1 Zn1 127.7(2) . 4 ? C1 N2 N3 102.9(2) . . ? C2 N3 N2 109.9(2) . . ? C2 N3 C3 128.3(3) . . ? N2 N3 C3 121.8(2) . . ? C18 N4 N5 110.2(3) . . ? C18 N4 C15 129.2(3) . . ? N5 N4 C15 120.6(3) . . ? C17 N5 N4 102.9(3) . . ? C18 N6 C17 103.2(3) . . ? C18 N6 Zn1 127.8(2) . . ? C17 N6 Zn1 128.9(2) . . ? N2 C1 N1 113.6(3) . . ? N2 C1 H1A 123.2 . . ? N1 C1 H1A 123.2 . . ? N1 C2 N3 109.8(3) . . ? N1 C2 H2A 125.1 . . ? N3 C2 H2A 125.1 . . ? N3 C3 C5 111.1(2) . . ? N3 C3 C4 109.2(3) . . ? C5 C3 C4 113.3(3) . . ? N3 C3 H3A 107.7 . . ? C5 C3 H3A 107.7 . . ? C4 C3 H3A 107.7 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C9 C5 C6 107.6(3) . . ? C9 C5 C3 129.7(3) . . ? C6 C5 C3 122.5(3) . . ? C9 C5 Fe1 69.78(18) . . ? C6 C5 Fe1 69.53(18) . . ? C3 C5 Fe1 130.1(2) . . ? C7 C6 C5 107.1(3) . . ? C7 C6 Fe1 69.30(19) . . ? C5 C6 Fe1 69.49(18) . . ? C7 C6 H6A 126.4 . . ? C5 C6 H6A 126.4 . . ? Fe1 C6 H6A 126.4 . . ? C8 C7 C6 108.6(3) . . ? C8 C7 Fe1 69.8(2) . . ? C6 C7 Fe1 69.70(19) . . ? C8 C7 H7A 125.7 . . ? C6 C7 H7A 125.7 . . ? Fe1 C7 H7A 125.7 . . ? C9 C8 C7 107.6(3) . . ? C9 C8 Fe1 69.99(19) . . ? C7 C8 Fe1 69.6(2) . . ? C9 C8 H8A 126.2 . . ? C7 C8 H8A 126.2 . . ? Fe1 C8 H8A 126.2 . . ? C8 C9 C5 109.0(3) . . ? C8 C9 Fe1 69.65(19) . . ? C5 C9 Fe1 69.65(18) . . ? C8 C9 H9A 125.5 . . ? C5 C9 H9A 125.5 . . ? Fe1 C9 H9A 125.5 . . ? C11 C10 C14 108.7(3) . . ? C11 C10 Fe1 69.92(18) . . ? C14 C10 Fe1 69.74(17) . . ? C11 C10 H10A 125.6 . . ? C14 C10 H10A 125.6 . . ? Fe1 C10 H10A 125.6 . . ? C12 C11 C10 108.1(3) . . ? C12 C11 Fe1 69.2(2) . . ? C10 C11 Fe1 70.03(18) . . ? C12 C11 H11A 126.0 . . ? C10 C11 H11A 126.0 . . ? Fe1 C11 H11A 126.0 . . ? C11 C12 C13 108.2(3) . . ? C11 C12 Fe1 70.6(2) . . ? C13 C12 Fe1 70.36(19) . . ? C11 C12 H12A 125.9 . . ? C13 C12 H12A 125.9 . . ? Fe1 C12 H12A 125.9 . . ? C12 C13 C14 108.4(3) . . ? C12 C13 Fe1 69.13(19) . . ? C14 C13 Fe1 69.96(17) . . ? C12 C13 H13A 125.8 . . ? C14 C13 H13A 125.8 . . ? Fe1 C13 H13A 125.8 . . ? C13 C14 C10 106.5(3) . . ? C13 C14 C15 125.5(3) . . ? C10 C14 C15 127.8(3) . . ? C13 C14 Fe1 69.56(16) . . ? C10 C14 Fe1 69.64(17) . . ? C15 C14 Fe1 129.2(2) . . ? N4 C15 C14 109.0(3) . . ? N4 C15 C16 109.3(3) . . ? C14 C15 C16 114.2(3) . . ? N4 C15 H15A 108.0 . . ? C14 C15 H15A 108.0 . . ? C16 C15 H15A 108.0 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N5 C17 N6 114.3(3) . . ? N5 C17 H17A 122.9 . . ? N6 C17 H17A 122.9 . . ? N4 C18 N6 109.4(3) . . ? N4 C18 H18A 125.3 . . ? N6 C18 H18A 125.3 . . ? C21 O3 Zn1 113.62(19) . . ? O4 C21 O3 123.9(3) . . ? O4 C21 C22 119.7(3) . . ? O3 C21 C22 116.5(3) . . ? C19 O1 Zn1 109.3(2) . . ? O2 C19 O1 122.8(3) . . ? O2 C19 C20 120.7(3) . . ? O1 C19 C20 116.5(3) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.51 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.338 _refine_diff_density_min -0.177 _refine_diff_density_rms 0.048 # Attachment 'CD1.cif' data_cd1 _database_code_depnum_ccdc_archive 'CCDC 662091' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H80 Cd3 Fe4 I6 N24' _chemical_formula_weight 2603.60 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I4/m ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 12.914(3) _cell_length_b 12.914(3) _cell_length_c 29.512(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4921.6(19) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 992 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 20.37 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.757 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2492 _exptl_absorpt_coefficient_mu 3.138 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1733 _exptl_absorpt_correction_T_max 0.3434 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 12127 _diffrn_reflns_av_R_equivalents 0.0882 _diffrn_reflns_av_sigmaI/netI 0.1290 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 24.98 _reflns_number_total 2182 _reflns_number_gt 912 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0350P)^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 'riding mode' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2182 _refine_ls_number_parameters 142 _refine_ls_number_restraints 85 _refine_ls_R_factor_all 0.1359 _refine_ls_R_factor_gt 0.0711 _refine_ls_wR_factor_ref 0.1586 _refine_ls_wR_factor_gt 0.1490 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.084 _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 Cd1 Cd 0.0000 0.0000 0.80996(5) 0.0666(5) Uani 1 4 d S . . I1 I 0.0000 0.0000 0.71651(7) 0.1564(9) Uani 1 4 d S . . Fe1 Fe 0.5000 0.0000 0.85949(8) 0.0783(7) Uani 1 2 d S . . N1 N 0.1507(5) -0.1004(5) 0.8217(3) 0.068(2) Uani 1 1 d . . . N2 N 0.2864(6) -0.1715(6) 0.8455(3) 0.088(3) Uani 1 1 d . . . N3 N 0.2912(6) -0.1878(6) 0.8022(3) 0.100(3) Uani 1 1 d . . . C1 C 0.2066(9) -0.1377(8) 0.7858(3) 0.108(4) Uani 1 1 d DU . . H1A H 0.1895 -0.1301 0.7554 0.130 Uiso 1 1 calc R . . C2 C 0.2027(7) -0.1206(7) 0.8589(3) 0.073(3) Uani 1 1 d DU . . H2A H 0.1847 -0.1028 0.8884 0.088 Uiso 1 1 calc R . . C3 C 0.3675(8) -0.2095(8) 0.8795(4) 0.100(4) Uani 1 1 d U . . H3A H 0.3474 -0.1881 0.9101 0.120 Uiso 1 1 calc R . . C5 C 0.4746(8) -0.1526(7) 0.8655(4) 0.085(3) Uani 1 1 d U . . C6 C 0.5211(9) -0.1307(7) 0.8227(4) 0.100(4) Uani 1 1 d . . . H6A H 0.4921 -0.1458 0.7927 0.120 Uiso 1 1 calc R . . C7 C 0.6205(7) -0.0826(7) 0.8323(4) 0.087(4) Uani 1 1 d . . . H7A H 0.6708 -0.0576 0.8100 0.104 Uiso 1 1 calc R . . C8 C 0.6306(8) -0.0792(7) 0.8775(4) 0.086(4) Uani 1 1 d U . . H8A H 0.6897 -0.0475 0.8931 0.103 Uiso 1 1 calc R . . C9 C 0.5406(8) -0.1221(7) 0.9008(4) 0.098(4) Uani 1 1 d . . . H9A H 0.5295 -0.1292 0.9335 0.117 Uiso 1 1 calc R . . C4 C 0.3791(10) -0.3160(9) 0.8782(5) 0.154(5) Uani 1 1 d U . . H4A H 0.3141 -0.3485 0.8852 0.231 Uiso 1 1 calc R . . H4B H 0.4300 -0.3367 0.9001 0.231 Uiso 1 1 calc R . . H4C H 0.4011 -0.3368 0.8485 0.231 Uiso 1 1 calc R . . Cd2 Cd 0.0552(5) -0.0916(4) 1.0000 0.1243(18) Uani 0.25 2 d SPU . . I2 I 0.0000 0.0000 0.92567(6) 0.1424(8) Uani 1 4 d SU . . I3 I -0.0437(5) -0.2791(3) 1.0000 0.1469(19) Uani 0.331(2) 2 d SPU A 1 I3' I 0.2526(8) -0.1356(9) 1.0000 0.153(3) Uani 0.169(2) 2 d SPU A 2 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 Cd1 0.0417(5) 0.0417(5) 0.1164(13) 0.000 0.000 0.000 I1 0.1652(12) 0.1652(12) 0.1386(18) 0.000 0.000 0.000 Fe1 0.0402(11) 0.0434(11) 0.151(2) 0.000 0.000 0.0048(9) N1 0.064(5) 0.054(5) 0.085(6) -0.023(4) 0.002(4) -0.004(4) N2 0.072(6) 0.050(5) 0.142(8) -0.015(5) -0.005(6) -0.012(5) N3 0.065(6) 0.085(6) 0.152(9) -0.044(6) -0.013(6) 0.025(5) C1 0.099(7) 0.106(7) 0.119(7) -0.026(6) -0.017(6) -0.002(6) C2 0.058(5) 0.069(6) 0.092(7) 0.006(5) -0.001(5) -0.003(5) C3 0.084(6) 0.074(6) 0.141(7) -0.003(5) -0.015(6) 0.006(5) C5 0.080(6) 0.057(5) 0.118(7) 0.003(5) -0.005(5) 0.016(5) C6 0.111(9) 0.061(7) 0.127(10) -0.038(6) -0.018(8) 0.044(6) C7 0.039(6) 0.063(7) 0.158(11) -0.017(7) 0.009(6) 0.013(5) C8 0.069(6) 0.072(6) 0.117(7) 0.003(5) -0.005(5) 0.013(5) C9 0.087(8) 0.068(7) 0.137(10) 0.017(7) -0.041(8) 0.023(6) C4 0.136(8) 0.137(8) 0.190(9) 0.014(7) -0.005(7) -0.015(7) Cd2 0.159(4) 0.129(4) 0.085(3) 0.000 0.000 0.027(3) I2 0.1662(12) 0.1662(12) 0.0949(14) 0.000 0.000 0.000 I3 0.224(4) 0.107(3) 0.110(3) 0.000 0.000 -0.013(3) I3' 0.160(6) 0.197(7) 0.101(5) 0.000 0.000 0.062(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N1 2.364(7) 4 ? Cd1 N1 2.364(7) 3 ? Cd1 N1 2.364(7) . ? Cd1 N1 2.364(7) 2 ? Cd1 I1 2.758(3) . ? Fe1 C5 2.005(9) . ? Fe1 C5 2.005(9) 2_655 ? Fe1 C6 2.025(9) . ? Fe1 C6 2.025(9) 2_655 ? Fe1 C8 2.042(9) . ? Fe1 C8 2.042(9) 2_655 ? Fe1 C7 2.051(9) 2_655 ? Fe1 C7 2.051(9) . ? Fe1 C9 2.062(10) 2_655 ? Fe1 C9 2.062(10) . ? N1 C2 1.312(10) . ? N1 C1 1.370(11) . ? N2 N3 1.296(11) . ? N2 C2 1.325(11) . ? N2 C3 1.531(12) . ? N3 C1 1.358(12) . ? C1 H1A 0.9300 . ? C2 H2A 0.9300 . ? C3 C4 1.385(13) . ? C3 C5 1.620(13) . ? C3 H3A 0.9800 . ? C5 C9 1.404(13) . ? C5 C6 1.426(14) . ? C6 C7 1.454(13) . ? C6 H6A 0.9800 . ? C7 C8 1.340(14) . ? C7 H7A 0.9800 . ? C8 C9 1.460(14) . ? C8 H8A 0.9800 . ? C9 H9A 0.9800 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? Cd2 Cd2 1.953(8) 11_557 ? Cd2 Cd2 1.953(8) 3 ? Cd2 I2 2.592(3) 9_557 ? Cd2 I2 2.592(3) . ? Cd2 I3' 2.612(11) . ? Cd2 I3 2.737(8) . ? Cd2 Cd2 2.762(11) 9_557 ? Cd2 I3 2.957(8) 3 ? Cd2 I3' 3.224(12) 11_557 ? I2 Cd2 2.592(3) 3 ? I2 Cd2 2.592(3) 11_557 ? I2 Cd2 2.592(3) 9_557 ? I3 Cd2 2.957(8) 11_557 ? I3' Cd2 3.224(12) 3 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cd1 N1 163.1(4) 4 3 ? N1 Cd1 N1 88.76(5) 4 . ? N1 Cd1 N1 88.76(5) 3 . ? N1 Cd1 N1 88.76(5) 4 2 ? N1 Cd1 N1 88.76(5) 3 2 ? N1 Cd1 N1 163.1(4) . 2 ? N1 Cd1 I1 98.44(18) 4 . ? N1 Cd1 I1 98.44(18) 3 . ? N1 Cd1 I1 98.44(18) . . ? N1 Cd1 I1 98.44(18) 2 . ? C5 Fe1 C5 169.9(7) . 2_655 ? C5 Fe1 C6 41.4(4) . . ? C5 Fe1 C6 147.6(5) 2_655 . ? C5 Fe1 C6 147.6(5) . 2_655 ? C5 Fe1 C6 41.4(4) 2_655 2_655 ? C6 Fe1 C6 115.2(7) . 2_655 ? C5 Fe1 C8 67.7(4) . . ? C5 Fe1 C8 109.5(4) 2_655 . ? C6 Fe1 C8 67.1(4) . . ? C6 Fe1 C8 131.9(4) 2_655 . ? C5 Fe1 C8 109.5(4) . 2_655 ? C5 Fe1 C8 67.7(4) 2_655 2_655 ? C6 Fe1 C8 131.9(4) . 2_655 ? C6 Fe1 C8 67.1(4) 2_655 2_655 ? C8 Fe1 C8 149.9(6) . 2_655 ? C5 Fe1 C7 114.9(4) . 2_655 ? C5 Fe1 C7 69.3(4) 2_655 2_655 ? C6 Fe1 C7 109.0(4) . 2_655 ? C6 Fe1 C7 41.8(4) 2_655 2_655 ? C8 Fe1 C7 171.5(5) . 2_655 ? C8 Fe1 C7 38.2(4) 2_655 2_655 ? C5 Fe1 C7 69.3(4) . . ? C5 Fe1 C7 114.9(4) 2_655 . ? C6 Fe1 C7 41.8(4) . . ? C6 Fe1 C7 109.0(4) 2_655 . ? C8 Fe1 C7 38.2(4) . . ? C8 Fe1 C7 171.5(5) 2_655 . ? C7 Fe1 C7 133.9(7) 2_655 . ? C5 Fe1 C9 131.1(5) . 2_655 ? C5 Fe1 C9 40.4(4) 2_655 2_655 ? C6 Fe1 C9 171.4(5) . 2_655 ? C6 Fe1 C9 69.3(5) 2_655 2_655 ? C8 Fe1 C9 116.0(4) . 2_655 ? C8 Fe1 C9 41.7(4) 2_655 2_655 ? C7 Fe1 C9 68.9(4) 2_655 2_655 ? C7 Fe1 C9 145.4(4) . 2_655 ? C5 Fe1 C9 40.4(4) . . ? C5 Fe1 C9 131.1(5) 2_655 . ? C6 Fe1 C9 69.3(5) . . ? C6 Fe1 C9 171.4(5) 2_655 . ? C8 Fe1 C9 41.7(4) . . ? C8 Fe1 C9 116.0(4) 2_655 . ? C7 Fe1 C9 145.4(4) 2_655 . ? C7 Fe1 C9 68.9(4) . . ? C9 Fe1 C9 107.4(7) 2_655 . ? C2 N1 C1 107.9(7) . . ? C2 N1 Cd1 130.8(6) . . ? C1 N1 Cd1 120.9(6) . . ? N3 N2 C2 114.4(8) . . ? N3 N2 C3 124.1(9) . . ? C2 N2 C3 121.4(9) . . ? N2 N3 C1 103.6(8) . . ? N3 C1 N1 108.4(8) . . ? N3 C1 H1A 125.8 . . ? N1 C1 H1A 125.8 . . ? N1 C2 N2 105.5(7) . . ? N1 C2 H2A 127.3 . . ? N2 C2 H2A 127.3 . . ? C4 C3 N2 112.0(10) . . ? C4 C3 C5 110.6(10) . . ? N2 C3 C5 105.8(8) . . ? C4 C3 H3A 109.5 . . ? N2 C3 H3A 109.5 . . ? C5 C3 H3A 109.5 . . ? C9 C5 C6 110.3(10) . . ? C9 C5 C3 117.1(10) . . ? C6 C5 C3 132.4(10) . . ? C9 C5 Fe1 72.0(6) . . ? C6 C5 Fe1 70.0(6) . . ? C3 C5 Fe1 127.4(7) . . ? C5 C6 C7 106.5(10) . . ? C5 C6 Fe1 68.5(6) . . ? C7 C6 Fe1 70.0(5) . . ? C5 C6 H6A 126.8 . . ? C7 C6 H6A 126.8 . . ? Fe1 C6 H6A 126.8 . . ? C8 C7 C6 107.1(10) . . ? C8 C7 Fe1 70.6(6) . . ? C6 C7 Fe1 68.2(5) . . ? C8 C7 H7A 126.4 . . ? C6 C7 H7A 126.4 . . ? Fe1 C7 H7A 126.4 . . ? C7 C8 C9 112.3(10) . . ? C7 C8 Fe1 71.2(6) . . ? C9 C8 Fe1 69.9(5) . . ? C7 C8 H8A 123.8 . . ? C9 C8 H8A 123.8 . . ? Fe1 C8 H8A 123.8 . . ? C5 C9 C8 103.8(11) . . ? C5 C9 Fe1 67.7(6) . . ? C8 C9 Fe1 68.4(6) . . ? C5 C9 H9A 128.1 . . ? C8 C9 H9A 128.1 . . ? Fe1 C9 H9A 128.1 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Cd2 Cd2 Cd2 90.000(2) 11_557 3 ? Cd2 Cd2 I2 67.87(7) 11_557 9_557 ? Cd2 Cd2 I2 67.87(7) 3 9_557 ? Cd2 Cd2 I2 67.87(7) 11_557 . ? Cd2 Cd2 I2 67.87(7) 3 . ? I2 Cd2 I2 115.6(2) 9_557 . ? Cd2 Cd2 I3' 178.6(5) 11_557 . ? Cd2 Cd2 I3' 88.6(5) 3 . ? I2 Cd2 I3' 111.57(19) 9_557 . ? I2 Cd2 I3' 111.57(19) . . ? Cd2 Cd2 I3 76.1(4) 11_557 . ? Cd2 Cd2 I3 166.1(4) 3 . ? I2 Cd2 I3 105.99(18) 9_557 . ? I2 Cd2 I3 105.99(18) . . ? I3' Cd2 I3 105.2(3) . . ? Cd2 Cd2 Cd2 45.000(2) 11_557 9_557 ? Cd2 Cd2 Cd2 45.000(1) 3 9_557 ? I2 Cd2 Cd2 57.81(11) 9_557 9_557 ? I2 Cd2 Cd2 57.81(11) . 9_557 ? I3' Cd2 Cd2 133.6(5) . 9_557 ? I3 Cd2 Cd2 121.1(4) . 9_557 ? Cd2 Cd2 I3 154.0(3) 11_557 3 ? Cd2 Cd2 I3 64.0(4) 3 3 ? I2 Cd2 I3 99.98(17) 9_557 3 ? I2 Cd2 I3 99.98(17) . 3 ? I3' Cd2 I3 24.6(3) . 3 ? I3 Cd2 I3 129.9(2) . 3 ? Cd2 Cd2 I3 109.0(4) 9_557 3 ? Cd2 Cd2 I3' 54.1(4) 11_557 11_557 ? Cd2 Cd2 I3' 144.1(4) 3 11_557 ? I2 Cd2 I3' 94.8(2) 9_557 11_557 ? I2 Cd2 I3' 94.8(2) . 11_557 ? I3' Cd2 I3' 127.3(2) . 11_557 ? I3 Cd2 I3' 22.0(2) . 11_557 ? Cd2 Cd2 I3' 99.1(4) 9_557 11_557 ? I3 Cd2 I3' 151.9(3) 3 11_557 ? Cd2 I2 Cd2 64.4(2) 3 11_557 ? Cd2 I2 Cd2 44.26(14) 3 9_557 ? Cd2 I2 Cd2 44.26(14) 11_557 9_557 ? Cd2 I2 Cd2 44.26(14) 3 . ? Cd2 I2 Cd2 44.26(14) 11_557 . ? Cd2 I2 Cd2 64.4(2) 9_557 . ? Cd2 I3 Cd2 39.9(2) . 11_557 ? Cd2 I3' Cd2 37.3(2) . 3 ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.981 _refine_diff_density_min -0.574 _refine_diff_density_rms 0.115