data_ja1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H28 Fe I N2 O P Zn' _chemical_formula_weight 699.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.936(4) _cell_length_b 15.982(6) _cell_length_c 16.338(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.362(8) _cell_angle_gamma 90.00 _cell_volume 2855.3(19) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.627 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 2.509 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 14607 _diffrn_reflns_av_R_equivalents 0.1461 _diffrn_reflns_av_sigmaI/netI 0.1958 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5017 _reflns_number_gt 2374 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.2000P)^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 5017 _refine_ls_number_parameters 326 _refine_ls_number_restraints 245 _refine_ls_R_factor_all 0.2795 _refine_ls_R_factor_gt 0.2084 _refine_ls_wR_factor_ref 0.5354 _refine_ls_wR_factor_gt 0.5187 _refine_ls_goodness_of_fit_ref 1.641 _refine_ls_restrained_S_all 1.604 _refine_ls_shift/su_max 0.439 _refine_ls_shift/su_mean 0.057 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 0.8004(5) 0.9336(2) 0.3510(2) 0.0652(15) Uani 1 1 d . . . I1 I 0.7421(3) 0.97728(14) 0.20938(11) 0.0599(10) Uani 1.038(10) 1 d P A 1 O1 O 0.751(2) 0.8099(17) 0.3630(14) 0.088(3) Uani 1.038(10) 1 d PDU A 1 C1D C 0.6891(8) 0.7693(18) 0.4228(11) 0.090(3) Uani 1.038(10) 1 d PDU A 1 H1DA H 0.6038 0.7594 0.4047 0.108 Uiso 1.038(10) 1 calc PR A 1 H1DB H 0.6870 0.8047 0.4726 0.108 Uiso 1.038(10) 1 calc PR A 1 C2D C 0.846(3) 0.684(2) 0.401(2) 0.092(3) Uani 1.038(10) 1 d PDU A 1 H2DA H 0.8649 0.6275 0.3805 0.110 Uiso 1.038(10) 1 calc PR A 1 H2DB H 0.9173 0.7051 0.4332 0.110 Uiso 1.038(10) 1 calc PR A 1 C3D C 0.751(4) 0.684(2) 0.444(2) 0.091(3) Uani 1.038(10) 1 d PDU A 1 H3DA H 0.7708 0.6805 0.5027 0.109 Uiso 1.038(10) 1 calc PR A 1 H3DB H 0.6969 0.6369 0.4284 0.109 Uiso 1.038(10) 1 calc PR A 1 C4D C 0.814(3) 0.745(2) 0.3296(16) 0.091(3) Uani 1.038(10) 1 d PDU A 1 H4DA H 0.8897 0.7658 0.3033 0.109 Uiso 1.038(10) 1 calc PR A 1 H4DB H 0.7637 0.7162 0.2878 0.109 Uiso 1.038(10) 1 calc PR A 1 Fe1 Fe 0.7476(4) 1.0469(2) 0.6237(2) 0.0339(12) Uani 1 1 d . . . N1 N 0.733(2) 0.9811(14) 0.4505(12) 0.036(4) Uani 1 1 d U A . N2 N 0.988(4) 0.926(2) 0.3713(16) 0.083(6) Uani 1 1 d U A . P1 P 0.7571(8) 0.9202(5) 0.6733(4) 0.039(2) Uani 1 1 d . . . C1 C 0.743(3) 1.0045(17) 0.5189(15) 0.036(4) Uani 1 1 d U . . C2 C 1.101(5) 0.938(3) 0.373(2) 0.082(6) Uani 1 1 d U . . C1A C 0.705(2) 1.1129(15) 0.7303(13) 0.073(3) Uani 1 1 d DU . . H1AA H 0.7441 1.1055 0.7852 0.087 Uiso 1 1 calc R A . C2A C 0.746(2) 1.1691(15) 0.6657(13) 0.072(3) Uani 1 1 d DU A . H2AA H 0.8176 1.2076 0.6688 0.086 Uiso 1 1 calc R . . C3A C 0.663(2) 1.1599(16) 0.5959(14) 0.072(3) Uani 1 1 d DU . . H3AA H 0.6679 1.1907 0.5427 0.087 Uiso 1 1 calc R A . C4A C 0.572(2) 1.0961(17) 0.6168(15) 0.073(3) Uani 1 1 d DU A . H4AA H 0.5042 1.0757 0.5805 0.088 Uiso 1 1 calc R . . C5A C 0.593(2) 1.0716(17) 0.7017(15) 0.073(3) Uani 1 1 d DU A . H5AA H 0.5455 1.0287 0.7326 0.088 Uiso 1 1 calc R . . C1C C 0.904(3) 0.855(2) 0.649(2) 0.066(3) Uani 1 1 d DU . . C2C C 0.940(3) 0.8007(19) 0.702(2) 0.067(3) Uani 1 1 d DU . . H2CA H 0.9000 0.7973 0.7537 0.081 Uiso 1 1 calc R . . C3C C 1.044(3) 0.743(2) 0.682(2) 0.068(3) Uani 1 1 d DU . . H3CA H 1.0748 0.7031 0.7208 0.082 Uiso 1 1 calc R . . C4C C 1.090(3) 0.751(2) 0.607(2) 0.068(3) Uani 1 1 d DU . . H4CA H 1.1496 0.7122 0.5890 0.081 Uiso 1 1 calc R . . C5C C 1.049(3) 0.817(2) 0.554(2) 0.067(3) Uani 1 1 d DU . . H5CA H 1.0916 0.8260 0.5045 0.081 Uiso 1 1 calc R . . C6C C 0.952(3) 0.867(2) 0.571(2) 0.067(3) Uani 1 1 d DU . . H6CA H 0.9206 0.9069 0.5336 0.080 Uiso 1 1 calc R . . C7C C 0.7791(17) 0.9224(17) 0.7825(11) 0.069(3) Uani 1 1 d DU . . C8C C 0.8877(18) 0.9464(16) 0.8191(11) 0.070(3) Uani 1 1 d DU . . H8CA H 0.9560 0.9601 0.7861 0.084 Uiso 1 1 calc R . . C9C C 0.8979(19) 0.9506(18) 0.9040(12) 0.072(3) Uani 1 1 d DU . . H9CA H 0.9742 0.9632 0.9291 0.086 Uiso 1 1 calc R . . C10C C 0.795(2) 0.936(2) 0.9512(12) 0.071(3) Uani 1 1 d DU . . H10A H 0.7963 0.9497 1.0078 0.086 Uiso 1 1 calc R . . C11C C 0.691(2) 0.902(2) 0.9154(12) 0.072(3) Uani 1 1 d DU . . H11A H 0.6296 0.8769 0.9484 0.087 Uiso 1 1 calc R . . C12C C 0.677(2) 0.905(2) 0.8308(12) 0.070(3) Uani 1 1 d DU . . H12A H 0.5997 0.8945 0.8061 0.084 Uiso 1 1 calc R . . C13C C 0.642(4) 0.851(2) 0.6521(18) 0.072(3) Uani 1 1 d DU . . C14C C 0.652(4) 0.758(2) 0.6557(16) 0.073(3) Uani 1 1 d DU . . H14A H 0.7299 0.7351 0.6694 0.087 Uiso 1 1 calc R . . C15C C 0.562(4) 0.704(2) 0.6412(18) 0.074(3) Uani 1 1 d DU . . H15A H 0.5746 0.6453 0.6424 0.089 Uiso 1 1 calc R . . C16C C 0.444(4) 0.739(2) 0.624(2) 0.074(3) Uani 1 1 d DU . . H16A H 0.3751 0.7026 0.6192 0.089 Uiso 1 1 calc R . . C17C C 0.427(4) 0.823(2) 0.614(2) 0.074(3) Uani 1 1 d DU . . H17A H 0.3512 0.8460 0.5951 0.089 Uiso 1 1 calc R . . C18C C 0.526(4) 0.872(2) 0.632(2) 0.073(3) Uani 1 1 d DU . . H18A H 0.5107 0.9309 0.6312 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 0.105(4) 0.044(2) 0.047(2) -0.0036(17) 0.014(2) -0.003(2) I1 0.083(2) 0.0655(16) 0.0313(11) 0.0037(9) 0.0031(10) -0.0048(13) O1 0.117(6) 0.072(6) 0.077(6) 0.002(5) 0.021(6) -0.002(6) C1D 0.117(6) 0.074(6) 0.079(6) 0.002(6) 0.021(6) -0.002(6) C2D 0.119(6) 0.076(6) 0.081(6) 0.000(6) 0.018(6) -0.001(6) C3D 0.118(6) 0.075(6) 0.080(6) 0.001(6) 0.019(6) -0.002(6) C4D 0.119(7) 0.075(6) 0.079(6) 0.001(6) 0.020(6) -0.002(6) Fe1 0.052(3) 0.027(2) 0.0231(19) -0.0018(15) -0.0039(18) -0.0034(19) N1 0.048(10) 0.035(8) 0.026(7) 0.005(7) -0.011(7) 0.012(8) N2 0.120(13) 0.092(11) 0.038(9) -0.007(9) 0.024(12) 0.036(12) P1 0.062(6) 0.034(4) 0.022(3) 0.004(3) 0.007(3) 0.002(4) C1 0.048(10) 0.035(9) 0.025(7) 0.006(7) -0.008(8) 0.013(8) C2 0.119(14) 0.091(12) 0.036(9) -0.008(9) 0.027(12) 0.037(13) C1A 0.078(6) 0.062(6) 0.079(6) -0.021(6) 0.010(6) 0.012(6) C2A 0.076(6) 0.061(6) 0.078(6) -0.020(6) 0.010(6) 0.013(6) C3A 0.077(6) 0.062(6) 0.079(6) -0.019(6) 0.010(6) 0.013(6) C4A 0.077(6) 0.063(6) 0.080(6) -0.018(6) 0.010(6) 0.013(6) C5A 0.077(7) 0.063(6) 0.080(6) -0.019(6) 0.010(6) 0.012(6) C1C 0.062(6) 0.051(6) 0.085(6) 0.005(5) 0.023(6) 0.013(5) C2C 0.062(6) 0.053(6) 0.087(6) 0.006(5) 0.024(6) 0.013(5) C3C 0.063(6) 0.053(6) 0.088(6) 0.007(6) 0.024(6) 0.013(6) C4C 0.064(6) 0.053(6) 0.087(6) 0.006(6) 0.023(6) 0.014(6) C5C 0.063(6) 0.052(6) 0.087(6) 0.006(6) 0.023(6) 0.014(6) C6C 0.063(6) 0.051(6) 0.086(6) 0.006(6) 0.023(6) 0.014(6) C7C 0.066(6) 0.070(6) 0.070(6) -0.008(5) 0.002(6) -0.014(6) C8C 0.067(6) 0.071(6) 0.072(6) -0.007(6) 0.002(6) -0.014(6) C9C 0.068(6) 0.073(6) 0.074(6) -0.007(6) 0.002(6) -0.015(6) C10C 0.068(6) 0.073(6) 0.073(6) -0.006(6) 0.003(6) -0.015(6) C11C 0.068(6) 0.075(6) 0.073(6) -0.008(6) 0.003(6) -0.014(6) C12C 0.067(6) 0.073(6) 0.071(6) -0.007(6) 0.002(6) -0.015(6) C13C 0.071(6) 0.051(6) 0.093(6) -0.003(6) 0.005(6) -0.008(6) C14C 0.071(6) 0.052(6) 0.095(6) -0.002(6) 0.003(6) -0.007(6) C15C 0.072(6) 0.053(6) 0.097(6) -0.003(6) 0.003(6) -0.007(6) C16C 0.071(6) 0.052(6) 0.099(6) -0.003(6) 0.004(6) -0.008(6) C17C 0.072(6) 0.053(6) 0.098(6) -0.004(6) 0.005(6) -0.007(6) C18C 0.072(6) 0.052(6) 0.096(6) -0.004(6) 0.006(6) -0.007(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 Zn1 N1 1.94(2) . ? Zn1 O1 2.06(3) . ? Zn1 N2 2.08(4) . ? Zn1 I1 2.496(5) . ? O1 C1D 1.36(2) . ? O1 C4D 1.36(3) . ? C1D C3D 1.55(4) . ? C2D C3D 1.26(5) . ? C2D C4D 1.56(4) . ? Fe1 C2 1.67(5) 3_776 ? Fe1 C1 1.84(3) . ? Fe1 C4A 2.08(3) . ? Fe1 C2A 2.07(2) . ? Fe1 C3A 2.08(3) . ? Fe1 C1A 2.09(2) . ? Fe1 C5A 2.16(3) . ? Fe1 P1 2.183(8) . ? N1 C1 1.18(3) . ? N2 C2 1.25(6) . ? P1 C13C 1.71(4) . ? P1 C7C 1.80(2) . ? P1 C1C 1.96(3) . ? C2 Fe1 1.67(5) 3_776 ? C1A C2A 1.46(2) . ? C1A C5A 1.46(2) . ? C2A C3A 1.46(2) . ? C3A C4A 1.46(2) . ? C4A C5A 1.46(2) . ? C1C C2C 1.29(5) . ? C1C C6C 1.39(5) . ? C2C C3C 1.51(5) . ? C3C C4C 1.33(5) . ? C4C C5C 1.44(5) . ? C5C C6C 1.35(5) . ? C7C C8C 1.380(16) . ? C7C C12C 1.399(17) . ? C8C C9C 1.392(16) . ? C9C C10C 1.385(17) . ? C10C C11C 1.393(17) . ? C11C C12C 1.391(17) . ? C13C C18C 1.35(5) . ? C13C C14C 1.49(5) . ? C14C C15C 1.33(5) . ? C15C C16C 1.43(5) . ? C16C C17C 1.37(5) . ? C17C C18C 1.38(5) . ? 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 Zn1 O1 101.2(9) . . ? N1 Zn1 N2 105.5(11) . . ? O1 Zn1 N2 101.0(12) . . ? N1 Zn1 I1 124.8(7) . . ? O1 Zn1 I1 106.9(7) . . ? N2 Zn1 I1 114.2(8) . . ? C1D O1 C4D 101(2) . . ? C1D O1 Zn1 131.3(18) . . ? C4D O1 Zn1 124(2) . . ? O1 C1D C3D 111.0(15) . . ? C3D C2D C4D 103.2(16) . . ? C2D C3D C1D 103.9(15) . . ? O1 C4D C2D 106.6(18) . . ? C2 Fe1 C1 96.0(15) 3_776 . ? C2 Fe1 C4A 149.3(16) 3_776 . ? C1 Fe1 C4A 94.0(12) . . ? C2 Fe1 C2A 82.2(15) 3_776 . ? C1 Fe1 C2A 130.9(10) . . ? C4A Fe1 C2A 69.5(9) . . ? C2 Fe1 C3A 108.7(16) 3_776 . ? C1 Fe1 C3A 96.2(10) . . ? C4A Fe1 C3A 41.2(6) . . ? C2A Fe1 C3A 41.2(6) . . ? C2 Fe1 C1A 97.3(13) 3_776 . ? C1 Fe1 C1A 162.7(12) . . ? C4A Fe1 C1A 69.0(9) . . ? C2A Fe1 C1A 41.1(6) . . ? C3A Fe1 C1A 69.0(8) . . ? C2 Fe1 C5A 137.0(13) 3_776 . ? C1 Fe1 C5A 126.9(13) . . ? C4A Fe1 C5A 40.2(6) . . ? C2A Fe1 C5A 67.8(9) . . ? C3A Fe1 C5A 67.7(9) . . ? C1A Fe1 C5A 40.1(6) . . ? C2 Fe1 P1 94.5(15) 3_776 . ? C1 Fe1 P1 90.3(8) . . ? C4A Fe1 P1 114.4(8) . . ? C2A Fe1 P1 138.8(7) . . ? C3A Fe1 P1 155.0(8) . . ? C1A Fe1 P1 99.7(7) . . ? C5A Fe1 P1 89.2(8) . . ? C1 N1 Zn1 152(2) . . ? C2 N2 Zn1 166(3) . . ? C13C P1 C7C 107.9(13) . . ? C13C P1 C1C 102.6(17) . . ? C7C P1 C1C 96.2(13) . . ? C13C P1 Fe1 119.5(14) . . ? C7C P1 Fe1 110.8(9) . . ? C1C P1 Fe1 117.0(11) . . ? N1 C1 Fe1 175(3) . . ? N2 C2 Fe1 179(3) . 3_776 ? C2A C1A C5A 107.9(7) . . ? C2A C1A Fe1 68.7(10) . . ? C5A C1A Fe1 72.4(12) . . ? C1A C2A C3A 108.1(7) . . ? C1A C2A Fe1 70.3(10) . . ? C3A C2A Fe1 69.8(10) . . ? C4A C3A C2A 107.9(7) . . ? C4A C3A Fe1 69.4(12) . . ? C2A C3A Fe1 69.0(10) . . ? C5A C4A C3A 107.7(7) . . ? C5A C4A Fe1 72.8(14) . . ? C3A C4A Fe1 69.4(12) . . ? C1A C5A C4A 108.1(8) . . ? C1A C5A Fe1 67.4(11) . . ? C4A C5A Fe1 67.0(13) . . ? C2C C1C C6C 127(3) . . ? C2C C1C P1 117(3) . . ? C6C C1C P1 115(3) . . ? C1C C2C C3C 120(3) . . ? C4C C3C C2C 115(3) . . ? C3C C4C C5C 121(3) . . ? C6C C5C C4C 123(3) . . ? C5C C6C C1C 114(3) . . ? C8C C7C C12C 119.9(10) . . ? C8C C7C P1 123.0(12) . . ? C12C C7C P1 117.0(12) . . ? C7C C8C C9C 120.6(10) . . ? C10C C9C C8C 119.1(10) . . ? C9C C10C C11C 119.8(10) . . ? C12C C11C C10C 119.2(11) . . ? C11C C12C C7C 119.1(10) . . ? C18C C13C C14C 109(4) . . ? C18C C13C P1 125(3) . . ? C14C C13C P1 126(3) . . ? C15C C14C C13C 126(4) . . ? C14C C15C C16C 117(4) . . ? C15C C16C C17C 122(4) . . ? C18C C17C C16C 115(4) . . ? C13C C18C C17C 130(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 8.520 _refine_diff_density_min -1.935 _refine_diff_density_rms 0.400 #===END data_ja1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C125 H105 Ag2 Fe4 I4 N13 P4 Zn3' _chemical_formula_weight 2821.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Ag' 'Ag' -0.8971 1.1015 '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' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.240(4) _cell_length_b 16.089(5) _cell_length_c 17.644(5) _cell_angle_alpha 63.302(6) _cell_angle_beta 69.002(6) _cell_angle_gamma 79.220(6) _cell_volume 3370.1(17) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.493 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1517 _exptl_absorpt_coefficient_mu 1.835 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 13358 _diffrn_reflns_av_R_equivalents 0.0701 _diffrn_reflns_av_sigmaI/netI 0.2368 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 23.23 _reflns_number_total 9409 _reflns_number_gt 4351 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.2000P)^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 9409 _refine_ls_number_parameters 812 _refine_ls_number_restraints 750 _refine_ls_R_factor_all 0.2637 _refine_ls_R_factor_gt 0.1902 _refine_ls_wR_factor_ref 0.5102 _refine_ls_wR_factor_gt 0.4874 _refine_ls_goodness_of_fit_ref 1.468 _refine_ls_restrained_S_all 2.178 _refine_ls_shift/su_max 15.000 _refine_ls_shift/su_mean 0.215 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 0.0747(4) 0.6869(4) 0.8274(4) 0.0314(14) Uani 1 1 d . A . Zn2 Zn 0.4240(8) 1.0062(7) 0.4766(7) 0.040(4) Uani 0.50(2) 1 d PD . . Fe1 Fe -0.0053(5) 0.6154(4) 1.1449(4) 0.0299(17) Uani 1 1 d . . . Fe2 Fe 0.4415(5) 0.7013(4) 0.7168(4) 0.031(3) Uani 0.99(2) 1 d P . . Ag1 Ag 0.4947(6) 0.9922(5) 0.0445(5) 0.056(3) Uani 0.557(14) 1 d P . . I1 I 0.2487(9) 1.0604(9) 0.5124(8) 0.091(5) Uani 0.433(15) 1 d P . . I2 I 0.6627(3) 0.9014(2) 0.0040(2) 0.0518(12) Uani 1 1 d . . . P1 P 0.1462(10) 0.5615(8) 1.1466(9) 0.034(3) Uani 1 1 d . . . P2 P 0.4543(10) 0.6359(8) 0.6290(8) 0.033(3) Uani 1 1 d . . . N1A N 0.056(3) 0.570(3) 0.825(3) 0.041(11) Uani 1 1 d . . . N2A N 0.029(3) 0.680(2) 0.951(2) 0.027(7) Uiso 1 1 d U . . N1B N 0.462(3) 0.896(3) 0.573(3) 0.050(9) Uani 1 1 d U . . N2B N 0.217(3) 0.717(3) 0.770(3) 0.041(8) Uani 1 1 d U . . C1A C -0.037(3) 0.501(3) 1.167(3) 0.028(11) Uani 1 1 d . . . C2A C 0.021(3) 0.663(3) 1.023(3) 0.025(8) Uiso 1 1 d U . . C3A C -0.146(4) 0.625(3) 1.233(3) 0.051(6) Uani 1 1 d DU . . H3AA H -0.2036 0.5829 1.2587 0.061 Uiso 1 1 calc R . . C4A C -0.129(4) 0.708(3) 1.155(3) 0.044(6) Uani 1 1 d DU . . H4AA H -0.1709 0.7311 1.1140 0.053 Uiso 1 1 calc R . . C5A C -0.040(3) 0.755(3) 1.139(3) 0.040(6) Uani 1 1 d DU . . H5AA H -0.0118 0.8162 1.0921 0.048 Uiso 1 1 calc R . . C6A C -0.017(4) 0.692(3) 1.218(3) 0.038(5) Uiso 1 1 d DU . . H6AA H 0.0443 0.7008 1.2280 0.046 Uiso 1 1 calc R . . C7A C -0.069(4) 0.615(3) 1.272(3) 0.064(6) Uani 1 1 d DU . . H7AA H -0.0620 0.5656 1.3302 0.077 Uiso 1 1 calc R . . C8A C 0.251(2) 0.6432(18) 1.088(2) 0.045(6) Uani 1 1 d DU . . C9A C 0.232(2) 0.7402(18) 1.044(2) 0.048(6) Uani 1 1 d DU . . H9AA H 0.1661 0.7633 1.0424 0.057 Uiso 1 1 calc R . . C10A C 0.312(2) 0.802(2) 1.003(3) 0.049(6) Uani 1 1 d DU . . H10A H 0.2998 0.8671 0.9720 0.059 Uiso 1 1 calc R . . C11A C 0.409(2) 0.7688(19) 1.009(3) 0.049(6) Uani 1 1 d DU . . H11A H 0.4618 0.8113 0.9845 0.059 Uiso 1 1 calc R . . C12A C 0.429(2) 0.6719(19) 1.051(3) 0.049(6) Uani 1 1 d DU . . H12A H 0.4950 0.6488 1.0527 0.059 Uiso 1 1 calc R . . C13A C 0.350(2) 0.609(2) 1.089(3) 0.046(6) Uani 1 1 d DU . . H13A H 0.3632 0.5443 1.1156 0.055 Uiso 1 1 calc R . . C14A C 0.147(3) 0.508(2) 1.266(2) 0.049(6) Uani 1 1 d DU . . C15A C 0.186(2) 0.555(2) 1.2973(19) 0.050(6) Uani 1 1 d DU . . H15A H 0.2205 0.6117 1.2570 0.060 Uiso 1 1 calc R . . C16A C 0.174(3) 0.520(2) 1.389(2) 0.052(6) Uani 1 1 d DU . . H16A H 0.2012 0.5517 1.4098 0.062 Uiso 1 1 calc R . . C17A C 0.124(3) 0.437(2) 1.449(2) 0.053(6) Uani 1 1 d DU . . H17A H 0.1164 0.4128 1.5107 0.064 Uiso 1 1 calc R . . C18A C 0.085(3) 0.391(3) 1.417(2) 0.052(6) Uani 1 1 d DU . . H18A H 0.0497 0.3351 1.4577 0.062 Uiso 1 1 calc R . . C19A C 0.096(3) 0.425(2) 1.327(2) 0.049(6) Uani 1 1 d DU . . H19A H 0.0689 0.3923 1.3060 0.059 Uiso 1 1 calc R . . C20A C 0.1975(17) 0.4701(12) 1.1077(15) 0.050(6) Uani 1 1 d DU . . C21A C 0.2488(19) 0.3924(12) 1.1527(15) 0.050(6) Uani 1 1 d DU . . H21A H 0.2584 0.3857 1.2058 0.060 Uiso 1 1 calc R . . C22A C 0.286(2) 0.3246(14) 1.1210(17) 0.050(6) Uani 1 1 d DU . . H22A H 0.3202 0.2708 1.1530 0.060 Uiso 1 1 calc R . . C23A C 0.274(2) 0.3349(17) 1.0429(18) 0.049(6) Uani 1 1 d DU . . H23A H 0.3030 0.2899 1.0194 0.059 Uiso 1 1 calc R . . C24A C 0.220(3) 0.4110(14) 0.9992(18) 0.049(6) Uani 1 1 d DU . . H24A H 0.2083 0.4166 0.9475 0.059 Uiso 1 1 calc R . . C25A C 0.183(3) 0.4789(18) 1.031(2) 0.050(7) Uani 1 1 d DU . . H25A H 0.1483 0.5321 0.9996 0.060 Uiso 1 1 calc R . . C1B C 0.457(4) 0.825(4) 0.623(4) 0.046(9) Uani 1 1 d U . . C2B C 0.306(4) 0.713(3) 0.747(3) 0.043(8) Uani 1 1 d U . . C3B C 0.4301(16) 0.6589(18) 0.8505(19) 0.037(6) Uani 0.98(11) 1 d PDU . . H3BA H 0.3665 0.6558 0.9002 0.044 Uiso 1.0(7) 1 calc PR . . C4B C 0.491(2) 0.7330(13) 0.799(2) 0.037(7) Uani 0.60(10) 1 d PDU . . H4BA H 0.4797 0.7938 0.8038 0.045 Uiso 0.3(7) 1 calc PR . . C5B C 0.571(2) 0.7090(18) 0.741(2) 0.040(7) Uani 1.00(11) 1 d DU . . H5BA H 0.6298 0.7487 0.6965 0.048 Uiso 0.5(8) 1 calc PR . . C6B C 0.561(2) 0.619(2) 0.758(2) 0.039(7) Uani 0.97(11) 1 d PDU . . H6BA H 0.6102 0.5818 0.7280 0.047 Uiso 0.5(7) 1 calc PR . . C7B C 0.471(2) 0.5895(19) 0.823(2) 0.038(7) Uani 0.91(11) 1 d PDU . . H7BA H 0.4440 0.5257 0.8506 0.045 Uiso 1.0(7) 1 calc R . . C8B C 0.345(2) 0.653(2) 0.585(2) 0.060(6) Uani 1 1 d DU . . C9B C 0.311(2) 0.579(2) 0.584(2) 0.059(6) Uani 1 1 d DU . . H9BA H 0.3387 0.5185 0.6079 0.071 Uiso 1 1 calc R . . C10B C 0.235(3) 0.595(2) 0.547(3) 0.061(6) Uani 1 1 d DU . . H10B H 0.2124 0.5448 0.5443 0.073 Uiso 1 1 calc R . . C11B C 0.192(3) 0.683(2) 0.515(3) 0.064(6) Uani 1 1 d DU . . H11B H 0.1365 0.6922 0.4936 0.077 Uiso 1 1 calc R . . C12B C 0.228(3) 0.756(2) 0.514(3) 0.062(7) Uani 1 1 d DU . . H12B H 0.2014 0.8174 0.4888 0.075 Uiso 1 1 calc R . . C13B C 0.304(3) 0.741(2) 0.551(3) 0.060(7) Uani 1 1 d DU . . H13B H 0.3281 0.7910 0.5531 0.072 Uiso 1 1 calc R . . C14B C 0.557(2) 0.673(2) 0.5218(18) 0.040(6) Uani 1 1 d DU . . C15B C 0.560(2) 0.655(2) 0.4501(17) 0.040(6) Uani 1 1 d DU . . H15B H 0.5076 0.6224 0.4548 0.048 Uiso 1 1 calc R . . C16B C 0.642(2) 0.684(2) 0.372(2) 0.042(6) Uani 1 1 d DU . . H16B H 0.6446 0.6715 0.3236 0.051 Uiso 1 1 calc R . . C17B C 0.721(3) 0.730(3) 0.364(2) 0.044(6) Uani 1 1 d DU . . H17B H 0.7769 0.7490 0.3108 0.053 Uiso 1 1 calc R . . C18B C 0.717(3) 0.749(3) 0.435(2) 0.042(6) Uani 1 1 d DU . . H18B H 0.7678 0.7843 0.4293 0.050 Uiso 1 1 calc R . . C19B C 0.637(2) 0.717(3) 0.515(2) 0.042(6) Uani 1 1 d DU . . H19B H 0.6376 0.7255 0.5647 0.050 Uiso 1 1 calc R . . C20B C 0.472(2) 0.5085(19) 0.679(2) 0.043(6) Uani 1 1 d DU . . C21B C 0.561(2) 0.4616(18) 0.647(2) 0.046(6) Uani 1 1 d DU . . H21B H 0.6111 0.4952 0.5932 0.055 Uiso 1 1 calc R . . C22B C 0.574(2) 0.3645(19) 0.694(2) 0.047(6) Uani 1 1 d DU . . H22B H 0.6332 0.3330 0.6723 0.056 Uiso 1 1 calc R . . C23B C 0.498(2) 0.314(2) 0.774(2) 0.048(6) Uani 1 1 d DU . . H23B H 0.5078 0.2491 0.8057 0.058 Uiso 1 1 calc R . . C24B C 0.409(3) 0.361(2) 0.806(2) 0.048(6) Uani 1 1 d DU . . H24B H 0.3575 0.3269 0.8580 0.058 Uiso 1 1 calc R . . C25B C 0.397(3) 0.458(2) 0.759(2) 0.046(6) Uani 1 1 d DU . . H25B H 0.3387 0.4898 0.7815 0.055 Uiso 1 1 calc R . . N1C N 0.4233(11) 0.9683(9) 0.3863(8) 0.094(7) Uani 1 1 d DU . . C1C C 0.4680(17) 0.8890(10) 0.3725(11) 0.094(7) Uani 1 1 d DU . . H1CA H 0.4878 0.8372 0.4187 0.113 Uiso 1 1 calc R . . C2C C 0.4838(18) 0.8856(12) 0.2912(12) 0.096(8) Uani 1 1 d DU . . H2CA H 0.5235 0.8362 0.2784 0.115 Uiso 1 1 calc R . . C3C C 0.441(2) 0.9550(13) 0.2285(11) 0.096(8) Uani 1 1 d DU . . H3CA H 0.4475 0.9507 0.1749 0.115 Uiso 1 1 calc R . . C4C C 0.389(2) 1.0306(14) 0.2454(13) 0.095(8) Uani 1 1 d DU . . H4CA H 0.3594 1.0777 0.2032 0.114 Uiso 1 1 calc R . . C5C C 0.380(3) 1.0375(16) 0.3237(16) 0.092(8) Uani 1 1 d DU . . H5CA H 0.3446 1.0892 0.3347 0.111 Uiso 1 1 calc R . . N2C N 0.1193(10) 0.905(2) 0.1701(9) 0.099(7) Uani 1 1 d DU . . C6C C 0.0202(9) 0.895(2) 0.2271(10) 0.098(8) Uani 1 1 d DU . . H6CA H -0.0334 0.9266 0.2037 0.118 Uiso 1 1 calc R . . C7C C 0.0000(9) 0.840(3) 0.3185(10) 0.100(8) Uani 1 1 d DU . . H7CA H -0.0674 0.8331 0.3573 0.120 Uiso 1 1 calc R . . C8C C 0.0789(12) 0.793(3) 0.3529(11) 0.100(8) Uani 1 1 d DU . . H8CA H 0.0650 0.7545 0.4148 0.120 Uiso 1 1 calc R . . C9C C 0.1781(11) 0.804(3) 0.2960(13) 0.100(8) Uani 1 1 d DU . . H9CA H 0.2318 0.7733 0.3195 0.120 Uiso 1 1 calc R . . C10C C 0.1983(9) 0.860(3) 0.2047(12) 0.098(8) Uani 1 1 d DU . . H10C H 0.2658 0.8680 0.1661 0.118 Uiso 1 1 calc R . . N3C N 0.1149(11) 0.9283(17) 0.8139(13) 0.203(9) Uani 1 1 d DU . . C11C C 0.1107(9) 0.9088(16) 0.7451(14) 0.204(9) Uani 1 1 d DU . . H11C H 0.0527 0.8814 0.7524 0.245 Uiso 1 1 calc R . . C12C C 0.1933(11) 0.930(2) 0.6643(14) 0.204(9) Uani 1 1 d DU . . H12C H 0.1869 0.9264 0.6140 0.245 Uiso 1 1 calc R . . C13C C 0.2834(10) 0.9558(17) 0.6610(17) 0.202(9) Uani 1 1 d DU . . H13C H 0.3447 0.9485 0.6189 0.243 Uiso 1 1 calc R . . C14C C 0.2843(14) 0.993(2) 0.720(2) 0.202(9) Uani 1 1 d DU . . H14A H 0.3384 1.0286 0.7072 0.243 Uiso 1 1 calc R . . C15C C 0.200(2) 0.974(4) 0.799(2) 0.205(10) Uani 1 1 d DU . . H15C H 0.2014 0.9927 0.8425 0.246 Uiso 1 1 calc R . . N4C N -0.0117(12) 0.7893(11) 0.7671(13) 0.055(6) Uani 1 1 d DU . . C16C C -0.0799(13) 0.8454(12) 0.8049(11) 0.056(6) Uani 1 1 d DU A . H16C H -0.0816 0.8416 0.8607 0.068 Uiso 1 1 calc R . . C17C C -0.1457(14) 0.9071(12) 0.7607(14) 0.057(6) Uani 1 1 d DU . . H17C H -0.2081 0.9235 0.7967 0.069 Uiso 1 1 d R A . C18C C -0.1440(17) 0.9120(18) 0.6791(15) 0.057(6) Uani 0.50(4) 1 d PDU A 1 H18C H -0.1879 0.9557 0.6480 0.068 Uiso 0.50(4) 1 d PR A 1 C19C C -0.0768(18) 0.855(2) 0.6420(15) 0.056(7) Uani 0.50(4) 1 d PDU A 1 H19C H -0.0763 0.8579 0.5862 0.067 Uiso 0.50(4) 1 d PR A 1 C20C C -0.011(3) 0.793(3) 0.686(2) 0.055(6) Uani 0.50(4) 1 d PDU A 1 H20A H 0.0343 0.7533 0.6610 0.066 Uiso 0.50(4) 1 d PR A 1 C18' C -0.088(8) 0.975(8) 0.682(7) 0.057(6) Uani 0.50(4) 1 d PU A 2 H18D H -0.1160 1.0373 0.6617 0.068 Uiso 0.50(4) 1 d PR A 2 C19' C 0.001(8) 0.954(7) 0.640(8) 0.057(7) Uani 0.50(4) 1 d PU A 2 H19D H 0.0310 0.9914 0.5777 0.068 Uiso 0.50(4) 1 d PR A 2 C20' C 0.040(9) 0.862(7) 0.686(7) 0.055(6) Uani 0.50(4) 1 d PU A 2 H20B H 0.1111 0.8540 0.6630 0.067 Uiso 0.50(4) 1 d PR 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 Zn1 0.031(3) 0.032(3) 0.033(3) -0.016(3) -0.010(3) 0.001(2) Zn2 0.044(8) 0.031(7) 0.043(7) -0.014(6) -0.013(6) -0.004(5) Fe1 0.026(4) 0.034(4) 0.030(4) -0.017(3) -0.006(3) 0.001(3) Fe2 0.034(5) 0.032(4) 0.024(4) -0.010(3) -0.006(3) -0.003(3) Ag1 0.062(6) 0.053(5) 0.051(5) -0.022(4) -0.017(4) 0.002(4) I1 0.084(9) 0.125(10) 0.081(8) -0.063(7) -0.033(6) 0.031(7) I2 0.063(3) 0.046(2) 0.048(2) -0.0187(18) -0.0238(19) 0.0052(18) P1 0.037(8) 0.033(7) 0.040(7) -0.017(6) -0.018(6) 0.000(6) P2 0.038(8) 0.033(7) 0.026(7) -0.013(6) -0.008(6) -0.002(6) N1A 0.05(3) 0.05(3) 0.03(2) -0.02(2) -0.01(2) 0.00(2) N1B 0.030(14) 0.061(17) 0.036(16) -0.014(13) 0.008(14) 0.000(15) N2B 0.069(17) 0.035(13) 0.023(13) -0.006(11) -0.022(14) -0.012(15) C1A 0.03(3) 0.04(3) 0.02(2) -0.03(2) 0.00(2) 0.01(2) C3A 0.035(8) 0.038(8) 0.033(8) 0.002(7) 0.010(7) 0.016(7) C4A 0.035(8) 0.038(8) 0.034(8) -0.008(7) 0.000(7) 0.009(7) C5A 0.037(7) 0.038(7) 0.036(7) -0.014(6) -0.007(6) 0.003(6) C7A 0.038(7) 0.038(7) 0.034(7) 0.017(7) 0.023(7) 0.026(6) C8A 0.043(9) 0.039(8) 0.040(9) -0.010(8) -0.001(8) -0.011(8) C9A 0.044(9) 0.040(9) 0.041(9) -0.008(8) -0.001(8) -0.011(8) C10A 0.045(9) 0.042(9) 0.042(9) -0.008(8) 0.000(9) -0.011(8) C11A 0.045(9) 0.043(9) 0.042(9) -0.009(8) 0.000(9) -0.011(8) C12A 0.046(9) 0.042(9) 0.041(9) -0.011(8) 0.001(9) -0.010(8) C13A 0.043(9) 0.040(9) 0.041(9) -0.012(8) -0.001(9) -0.011(8) C14A 0.044(9) 0.047(9) 0.047(9) -0.003(8) -0.021(8) -0.009(8) C15A 0.046(9) 0.047(9) 0.046(9) -0.005(8) -0.019(8) -0.008(8) C16A 0.047(9) 0.048(9) 0.047(9) -0.004(8) -0.018(8) -0.007(8) C17A 0.047(9) 0.049(9) 0.047(9) -0.002(8) -0.017(9) -0.008(8) C18A 0.047(9) 0.049(9) 0.047(9) -0.003(8) -0.018(9) -0.008(9) C19A 0.044(9) 0.048(9) 0.046(9) -0.004(9) -0.021(9) -0.009(9) C20A 0.030(9) 0.059(9) 0.060(9) -0.026(8) -0.021(8) 0.016(8) C21A 0.030(9) 0.059(9) 0.060(9) -0.026(8) -0.022(8) 0.016(8) C22A 0.031(9) 0.059(9) 0.061(9) -0.025(8) -0.024(8) 0.016(8) C23A 0.031(9) 0.058(9) 0.060(9) -0.026(8) -0.023(8) 0.015(8) C24A 0.031(9) 0.058(9) 0.059(9) -0.027(8) -0.021(8) 0.017(8) C25A 0.031(9) 0.058(9) 0.059(9) -0.025(9) -0.021(8) 0.017(8) C1B 0.027(15) 0.059(18) 0.035(17) -0.016(14) 0.006(14) -0.001(16) C2B 0.070(18) 0.036(14) 0.024(14) -0.004(12) -0.022(15) -0.012(16) C3B 0.045(10) 0.053(9) 0.043(9) -0.034(8) -0.039(8) 0.017(9) C4B 0.045(10) 0.053(10) 0.043(9) -0.033(8) -0.038(8) 0.018(9) C5B 0.046(10) 0.053(9) 0.045(9) -0.031(8) -0.036(8) 0.020(9) C6B 0.045(10) 0.053(10) 0.045(9) -0.032(8) -0.037(8) 0.021(9) C7B 0.045(10) 0.053(10) 0.044(9) -0.033(8) -0.038(8) 0.018(9) C8B 0.066(9) 0.085(9) 0.033(9) -0.023(8) -0.013(8) -0.019(9) C9B 0.066(9) 0.085(9) 0.033(9) -0.023(8) -0.014(8) -0.020(9) C10B 0.066(10) 0.086(10) 0.035(9) -0.022(8) -0.015(8) -0.021(9) C11B 0.068(10) 0.087(10) 0.037(9) -0.020(9) -0.015(9) -0.020(9) C12B 0.067(10) 0.086(10) 0.035(9) -0.022(9) -0.015(9) -0.018(9) C13B 0.067(10) 0.085(10) 0.033(9) -0.023(9) -0.015(9) -0.018(9) C14B 0.060(9) 0.034(9) 0.021(8) -0.015(7) 0.001(8) -0.007(8) C15B 0.059(9) 0.034(9) 0.021(8) -0.014(7) 0.000(8) -0.006(8) C16B 0.060(9) 0.035(9) 0.022(8) -0.012(8) -0.001(8) -0.005(8) C17B 0.061(9) 0.035(9) 0.023(8) -0.010(8) 0.000(8) -0.005(8) C18B 0.060(9) 0.035(9) 0.023(8) -0.012(8) -0.002(8) -0.007(8) C19B 0.060(10) 0.035(9) 0.023(8) -0.013(8) 0.000(8) -0.006(8) C20B 0.048(9) 0.041(9) 0.042(9) -0.013(8) -0.016(8) -0.017(8) C21B 0.050(9) 0.042(9) 0.044(9) -0.012(8) -0.014(8) -0.016(8) C22B 0.051(9) 0.042(9) 0.044(9) -0.012(8) -0.013(8) -0.015(8) C23B 0.052(9) 0.043(9) 0.045(9) -0.012(8) -0.012(8) -0.014(8) C24B 0.052(9) 0.043(9) 0.044(9) -0.012(8) -0.012(8) -0.014(8) C25B 0.050(9) 0.043(9) 0.043(9) -0.012(8) -0.013(9) -0.016(9) N1C 0.073(9) 0.090(10) 0.121(10) -0.039(9) -0.041(9) 0.000(9) C1C 0.073(10) 0.092(10) 0.120(10) -0.040(9) -0.041(9) 0.000(9) C2C 0.074(10) 0.093(10) 0.121(10) -0.040(9) -0.040(9) 0.001(9) C3C 0.074(10) 0.093(10) 0.121(10) -0.039(10) -0.041(10) -0.001(9) C4C 0.074(10) 0.091(10) 0.121(10) -0.039(10) -0.040(10) -0.002(9) C5C 0.073(10) 0.090(10) 0.120(10) -0.040(10) -0.042(10) -0.002(10) N2C 0.130(10) 0.065(9) 0.088(10) -0.006(9) -0.045(9) -0.017(9) C6C 0.129(10) 0.065(10) 0.089(10) -0.006(9) -0.047(9) -0.017(10) C7C 0.129(10) 0.066(10) 0.089(10) -0.005(9) -0.046(10) -0.016(10) C8C 0.128(10) 0.066(10) 0.089(10) -0.005(9) -0.046(10) -0.015(10) C9C 0.128(10) 0.066(10) 0.089(10) -0.005(9) -0.045(10) -0.015(10) C10C 0.128(11) 0.065(10) 0.088(10) -0.006(10) -0.046(10) -0.017(10) N3C 0.152(10) 0.155(10) 0.191(10) 0.004(10) -0.015(10) -0.035(10) C11C 0.152(10) 0.156(10) 0.191(11) 0.004(10) -0.014(10) -0.034(10) C12C 0.151(11) 0.156(10) 0.191(11) 0.004(10) -0.013(11) -0.034(10) C13C 0.150(11) 0.155(11) 0.191(11) 0.003(11) -0.015(11) -0.034(11) C14C 0.150(11) 0.155(11) 0.191(11) 0.004(11) -0.016(11) -0.034(11) C15C 0.152(11) 0.157(11) 0.191(11) 0.005(11) -0.015(11) -0.033(11) N4C 0.048(7) 0.058(7) 0.053(7) -0.017(7) -0.019(7) 0.007(7) C16C 0.048(8) 0.057(8) 0.054(8) -0.016(7) -0.019(8) 0.006(7) C17C 0.048(7) 0.057(7) 0.054(7) -0.014(7) -0.018(7) 0.007(7) C18C 0.048(7) 0.057(7) 0.054(7) -0.015(7) -0.019(7) 0.006(7) C19C 0.048(8) 0.057(8) 0.054(8) -0.016(8) -0.019(8) 0.006(8) C20C 0.049(8) 0.057(8) 0.053(7) -0.017(7) -0.020(7) 0.006(7) C18' 0.048(8) 0.057(8) 0.054(8) -0.015(7) -0.018(7) 0.006(7) C19' 0.049(8) 0.057(8) 0.054(8) -0.016(8) -0.018(8) 0.006(8) C20' 0.048(8) 0.057(8) 0.053(8) -0.017(7) -0.019(7) 0.006(7) _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 N1A 1.96(4) . ? Zn1 N2B 1.95(5) . ? Zn1 N2A 1.99(4) . ? Zn1 N4C 1.991(14) . ? Zn2 N1C 1.948(8) . ? Zn2 N1B 1.98(5) . ? Zn2 N1B 2.14(5) 2_676 ? Zn2 I1 2.437(16) . ? Zn2 Zn2 2.53(2) 2_676 ? Fe1 C1A 1.82(5) . ? Fe1 C2A 1.84(4) . ? Fe1 C4A 2.09(4) . ? Fe1 C6A 2.09(5) . ? Fe1 C3A 2.09(4) . ? Fe1 C7A 2.10(5) . ? Fe1 C5A 2.17(4) . ? Fe1 P1 2.176(14) . ? Fe2 C2B 1.81(6) . ? Fe2 C1B 1.92(5) . ? Fe2 C7B 2.04(4) . ? Fe2 C5B 2.07(4) . ? Fe2 C4B 2.09(4) . ? Fe2 C6B 2.08(4) . ? Fe2 C3B 2.09(3) . ? Fe2 P2 2.176(14) . ? Ag1 Ag1 1.428(16) 2_675 ? Ag1 I2 2.603(9) . ? Ag1 I2 2.703(9) 2_675 ? I2 Ag1 2.703(9) 2_675 ? P1 C20A 1.82(2) . ? P1 C8A 1.85(3) . ? P1 C14A 1.88(3) . ? P2 C20B 1.84(3) . ? P2 C14B 1.84(3) . ? P2 C8B 1.89(3) . ? N1A C1A 1.16(5) 2_567 ? N2A C2A 1.15(5) . ? N1B C1B 1.09(6) . ? N1B Zn2 2.14(5) 2_676 ? N2B C2B 1.19(6) . ? C1A N1A 1.16(5) 2_567 ? C3A C4A 1.40(6) . ? C3A C7A 1.44(8) . ? C4A C5A 1.47(7) . ? C5A C6A 1.42(7) . ? C6A C7A 1.33(7) . ? C8A C13A 1.42(3) . ? C8A C9A 1.42(2) . ? C9A C10A 1.42(3) . ? C10A C11A 1.41(3) . ? C11A C12A 1.42(3) . ? C12A C13A 1.42(3) . ? C14A C15A 1.40(3) . ? C14A C19A 1.41(3) . ? C15A C16A 1.40(3) . ? C16A C17A 1.40(3) . ? C17A C18A 1.39(3) . ? C18A C19A 1.39(3) . ? C20A C25A 1.381(8) . ? C20A C21A 1.381(8) . ? C21A C22A 1.380(8) . ? C22A C23A 1.382(8) . ? C23A C24A 1.382(8) . ? C24A C25A 1.380(8) . ? C3B C4B 1.357(18) . ? C3B C7B 1.36(2) . ? C4B C5B 1.362(17) . ? C5B C6B 1.361(18) . ? C6B C7B 1.37(2) . ? C8B C13B 1.37(3) . ? C8B C9B 1.38(3) . ? C9B C10B 1.37(3) . ? C10B C11B 1.38(3) . ? C11B C12B 1.37(3) . ? C12B C13B 1.39(3) . ? C14B C19B 1.40(3) . ? C14B C15B 1.41(3) . ? C15B C16B 1.40(3) . ? C16B C17B 1.39(3) . ? C17B C18B 1.40(3) . ? C18B C19B 1.40(3) . ? C20B C21B 1.41(3) . ? C20B C25B 1.41(3) . ? C21B C22B 1.42(3) . ? C22B C23B 1.41(3) . ? C23B C24B 1.42(3) . ? C24B C25B 1.41(3) . ? N1C C1C 1.399(7) . ? N1C C5C 1.402(7) . ? C1C C2C 1.396(7) . ? C2C C3C 1.400(7) . ? C3C C4C 1.396(7) . ? C4C C5C 1.395(7) . ? N2C C10C 1.397(7) . ? N2C C6C 1.397(7) . ? C6C C7C 1.398(7) . ? C7C C8C 1.397(7) . ? C8C C9C 1.397(7) . ? C9C C10C 1.397(7) . ? N3C C11C 1.406(7) . ? N3C C15C 1.420(7) . ? C11C C12C 1.429(7) . ? C12C C13C 1.396(7) . ? C13C C14C 1.414(7) . ? C14C C15C 1.424(8) . ? N4C C20' 1.42(11) . ? N4C C20C 1.397(7) . ? N4C C16C 1.397(7) . ? C16C C17C 1.397(7) . ? C17C C18' 1.40(11) . ? C17C C18C 1.398(7) . ? C18C C19C 1.397(7) . ? C19C C20C 1.397(7) . ? C18' C19' 1.28(14) . ? C19' C20' 1.45(14) . ? 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 N1A Zn1 N2B 108.9(16) . . ? N1A Zn1 N2A 112.4(15) . . ? N2B Zn1 N2A 109.9(15) . . ? N1A Zn1 N4C 110.8(14) . . ? N2B Zn1 N4C 111.3(13) . . ? N2A Zn1 N4C 103.5(12) . . ? N1C Zn2 N1B 108.5(15) . . ? N1C Zn2 N1B 111.9(13) . 2_676 ? N1B Zn2 N1B 104.4(16) . 2_676 ? N1C Zn2 I1 97.4(6) . . ? N1B Zn2 I1 116.2(13) . . ? N1B Zn2 I1 118.2(12) 2_676 . ? N1C Zn2 Zn2 124.4(8) . 2_676 ? N1B Zn2 Zn2 55.0(14) . 2_676 ? N1B Zn2 Zn2 49.4(13) 2_676 2_676 ? I1 Zn2 Zn2 138.2(7) . 2_676 ? C1A Fe1 C2A 94.9(19) . . ? C1A Fe1 C4A 114(2) . . ? C2A Fe1 C4A 90.5(19) . . ? C1A Fe1 C6A 138.1(19) . . ? C2A Fe1 C6A 126.0(18) . . ? C4A Fe1 C6A 62(2) . . ? C1A Fe1 C3A 88.6(19) . . ? C2A Fe1 C3A 123(2) . . ? C4A Fe1 C3A 39.2(17) . . ? C6A Fe1 C3A 63(2) . . ? C1A Fe1 C7A 101(2) . . ? C2A Fe1 C7A 155.8(18) . . ? C4A Fe1 C7A 66.5(19) . . ? C6A Fe1 C7A 37(2) . . ? C3A Fe1 C7A 40(2) . . ? C1A Fe1 C5A 154.3(19) . . ? C2A Fe1 C5A 89.9(18) . . ? C4A Fe1 C5A 40.2(19) . . ? C6A Fe1 C5A 38.8(18) . . ? C3A Fe1 C5A 67.9(17) . . ? C7A Fe1 C5A 67.9(18) . . ? C1A Fe1 P1 88.7(14) . . ? C2A Fe1 P1 97.0(14) . . ? C4A Fe1 P1 155.2(16) . . ? C6A Fe1 P1 94.4(14) . . ? C3A Fe1 P1 139.6(16) . . ? C7A Fe1 P1 101.2(16) . . ? C5A Fe1 P1 115.9(14) . . ? C2B Fe2 C1B 92(2) . . ? C2B Fe2 C7B 105.4(17) . . ? C1B Fe2 C7B 156(2) . . ? C2B Fe2 C5B 147.9(18) . . ? C1B Fe2 C5B 91.9(18) . . ? C7B Fe2 C5B 64.9(10) . . ? C2B Fe2 C4B 109.7(18) . . ? C1B Fe2 C4B 94.9(19) . . ? C7B Fe2 C4B 64.5(9) . . ? C5B Fe2 C4B 38.2(8) . . ? C2B Fe2 C6B 143.9(17) . . ? C1B Fe2 C6B 123.3(18) . . ? C7B Fe2 C6B 38.7(8) . . ? C5B Fe2 C6B 38.3(7) . . ? C4B Fe2 C6B 63.7(8) . . ? C2B Fe2 C3B 89.2(17) . . ? C1B Fe2 C3B 128.4(19) . . ? C7B Fe2 C3B 38.5(7) . . ? C5B Fe2 C3B 63.9(7) . . ? C4B Fe2 C3B 37.9(7) . . ? C6B Fe2 C3B 63.7(9) . . ? C2B Fe2 P2 93.8(16) . . ? C1B Fe2 P2 94.0(17) . . ? C7B Fe2 P2 100.7(9) . . ? C5B Fe2 P2 117.6(9) . . ? C4B Fe2 P2 154.5(9) . . ? C6B Fe2 P2 91.6(9) . . ? C3B Fe2 P2 137.5(9) . . ? Ag1 Ag1 I2 78.3(6) 2_675 . ? Ag1 Ag1 I2 70.5(6) 2_675 2_675 ? I2 Ag1 I2 148.8(3) . 2_675 ? Ag1 I2 Ag1 31.2(3) . 2_675 ? C20A P1 C8A 102.6(14) . . ? C20A P1 C14A 104.6(14) . . ? C8A P1 C14A 102.5(16) . . ? C20A P1 Fe1 117.7(10) . . ? C8A P1 Fe1 119.3(10) . . ? C14A P1 Fe1 108.2(12) . . ? C20B P2 C14B 103.6(15) . . ? C20B P2 C8B 103.0(16) . . ? C14B P2 C8B 98.8(16) . . ? C20B P2 Fe2 114.1(13) . . ? C14B P2 Fe2 117.2(11) . . ? C8B P2 Fe2 117.8(12) . . ? C1A N1A Zn1 172(4) 2_567 . ? C2A N2A Zn1 165(3) . . ? C1B N1B Zn2 155(5) . . ? C1B N1B Zn2 129(5) . 2_676 ? Zn2 N1B Zn2 75.6(16) . 2_676 ? C2B N2B Zn1 164(4) . . ? N1A C1A Fe1 176(4) 2_567 . ? N2A C2A Fe1 168(4) . . ? C4A C3A C7A 107(5) . . ? C4A C3A Fe1 70(2) . . ? C7A C3A Fe1 70(3) . . ? C3A C4A C5A 112(5) . . ? C3A C4A Fe1 70(2) . . ? C5A C4A Fe1 73(2) . . ? C6A C5A C4A 97(4) . . ? C6A C5A Fe1 68(2) . . ? C4A C5A Fe1 67(2) . . ? C7A C6A C5A 120(5) . . ? C7A C6A Fe1 72(3) . . ? C5A C6A Fe1 73(3) . . ? C6A C7A C3A 103(4) . . ? C6A C7A Fe1 71(3) . . ? C3A C7A Fe1 69(3) . . ? C13A C8A C9A 119.5(15) . . ? C13A C8A P1 120.1(17) . . ? C9A C8A P1 120.4(17) . . ? C10A C9A C8A 119.9(15) . . ? C9A C10A C11A 120.4(15) . . ? C10A C11A C12A 119.8(16) . . ? C11A C12A C13A 119.6(16) . . ? C8A C13A C12A 120.7(16) . . ? C15A C14A C19A 119.1(17) . . ? C15A C14A P1 121.0(18) . . ? C19A C14A P1 119(2) . . ? C16A C15A C14A 119.9(16) . . ? C17A C16A C15A 121(2) . . ? C18A C17A C16A 119(2) . . ? C17A C18A C19A 121(2) . . ? C18A C19A C14A 120.0(16) . . ? C25A C20A C21A 119.3(13) . . ? C25A C20A P1 118.4(13) . . ? C21A C20A P1 122.3(15) . . ? C22A C21A C20A 120.4(13) . . ? C21A C22A C23A 120.1(13) . . ? C22A C23A C24A 119.6(13) . . ? C25A C24A C23A 119.9(13) . . ? C24A C25A C20A 120.5(13) . . ? N1B C1B Fe2 176(5) . . ? N2B C2B Fe2 177(5) . . ? C4B C3B C7B 108.3(11) . . ? C4B C3B Fe2 70.9(17) . . ? C7B C3B Fe2 68.8(19) . . ? C3B C4B C5B 108.1(10) . . ? C3B C4B Fe2 71.2(16) . . ? C5B C4B Fe2 70.2(16) . . ? C6B C5B C4B 107.9(10) . . ? C6B C5B Fe2 71.3(19) . . ? C4B C5B Fe2 71.6(17) . . ? C5B C6B C7B 108.1(11) . . ? C5B C6B Fe2 70.5(19) . . ? C7B C6B Fe2 69(2) . . ? C3B C7B C6B 107.4(13) . . ? C3B C7B Fe2 72.7(18) . . ? C6B C7B Fe2 72(2) . . ? C13B C8B C9B 120.1(16) . . ? C13B C8B P2 119(2) . . ? C9B C8B P2 120.9(19) . . ? C10B C9B C8B 119.7(16) . . ? C9B C10B C11B 120.2(16) . . ? C12B C11B C10B 120.0(16) . . ? C11B C12B C13B 119.6(16) . . ? C8B C13B C12B 120.2(16) . . ? C19B C14B C15B 119.2(17) . . ? C19B C14B P2 117.2(18) . . ? C15B C14B P2 123.4(19) . . ? C16B C15B C14B 119.4(16) . . ? C17B C16B C15B 121(2) . . ? C16B C17B C18B 119(2) . . ? C19B C18B C17B 120(2) . . ? C18B C19B C14B 120.7(16) . . ? C21B C20B C25B 119.7(15) . . ? C21B C20B P2 123.1(17) . . ? C25B C20B P2 116.9(18) . . ? C20B C21B C22B 120.0(15) . . ? C23B C22B C21B 120.2(16) . . ? C22B C23B C24B 119.9(15) . . ? C25B C24B C23B 119.6(16) . . ? C24B C25B C20B 120.5(16) . . ? C1C N1C C5C 119.0(6) . . ? C1C N1C Zn2 128.8(10) . . ? C5C N1C Zn2 111.9(10) . . ? C2C C1C N1C 120.3(6) . . ? C1C C2C C3C 119.8(6) . . ? C4C C3C C2C 119.5(6) . . ? C5C C4C C3C 120.4(6) . . ? C4C C5C N1C 120.2(6) . . ? C10C N2C C6C 120.0(6) . . ? N2C C6C C7C 120.0(6) . . ? C8C C7C C6C 120.0(6) . . ? C7C C8C C9C 120.0(6) . . ? C8C C9C C10C 120.0(6) . . ? N2C C10C C9C 120.0(6) . . ? C11C N3C C15C 118.3(6) . . ? N3C C11C C12C 120.3(6) . . ? C13C C12C C11C 118.5(7) . . ? C12C C13C C14C 120.5(7) . . ? C13C C14C C15C 117.0(6) . . ? C14C C15C N3C 121.7(7) . . ? C20' N4C C20C 61(5) . . ? C20' N4C C16C 97(4) . . ? C20C N4C C16C 120.0(6) . . ? C20' N4C Zn1 116(5) . . ? C20C N4C Zn1 114.2(12) . . ? C16C N4C Zn1 125.2(11) . . ? C17C C16C N4C 120.0(6) . . ? C18' C17C C16C 108(5) . . ? C18' C17C C18C 62(5) . . ? C16C C17C C18C 120.0(6) . . ? C19C C18C C17C 120.0(6) . . ? C18C C19C C20C 120.0(6) . . ? N4C C20C C19C 120.0(6) . . ? C19' C18' C17C 120(10) . . ? C18' C19' C20' 115(10) . . ? N4C C20' C19' 128(9) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 23.23 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 3.615 _refine_diff_density_min -2.192 _refine_diff_density_rms 0.301 #===END data_ja1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H30 Ag Fe I2 N4 P Zn' _chemical_formula_weight 1020.49 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' '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' 'Ag' 'Ag' -0.8971 1.1015 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/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 13.415(4) _cell_length_b 11.005(3) _cell_length_c 25.062(7) _cell_angle_alpha 90.00 _cell_angle_beta 104.232(5) _cell_angle_gamma 90.00 _cell_volume 3586.4(18) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.890 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1968 _exptl_absorpt_coefficient_mu 3.399 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 31347 _diffrn_reflns_av_R_equivalents 0.0563 _diffrn_reflns_av_sigmaI/netI 0.0483 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 23.27 _reflns_number_total 5142 _reflns_number_gt 4174 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0110P)^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 5142 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0321 _refine_ls_R_factor_gt 0.0229 _refine_ls_wR_factor_ref 0.0407 _refine_ls_wR_factor_gt 0.0389 _refine_ls_goodness_of_fit_ref 0.824 _refine_ls_restrained_S_all 0.824 _refine_ls_shift/su_max 0.003 _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 0.52803(4) 0.25957(5) 0.09911(2) 0.01510(14) Uani 1 1 d . . . Zn1 Zn 0.73676(3) -0.04351(4) 0.033819(17) 0.01737(12) Uani 1 1 d . . . Ag1 Ag 0.98051(3) 0.42465(3) 0.060348(13) 0.03164(10) Uani 1 1 d . . . P1 P 0.51681(8) 0.12289(9) 0.16112(4) 0.0156(2) Uani 1 1 d . . . I1 I 1.16009(2) 0.45033(3) 0.025257(11) 0.03006(8) Uani 1 1 d . . . I2 I 0.93204(2) 0.31018(2) 0.145047(11) 0.02764(8) Uani 1 1 d . . . N1 N 0.6702(2) 0.0960(3) 0.05614(12) 0.0194(8) Uani 1 1 d . . . N2 N 0.6533(2) -0.1603(3) -0.01497(12) 0.0188(8) Uani 1 1 d . . . N3 N 0.8309(2) 0.0225(3) -0.01119(12) 0.0168(8) Uani 1 1 d . . . N4 N 0.8143(2) -0.1283(3) 0.10338(12) 0.0169(8) Uani 1 1 d . . . C1 C 0.6157(3) 0.1582(3) 0.07331(15) 0.0178(10) Uani 1 1 d . . . C2 C 0.4158(3) 0.1967(3) 0.04859(15) 0.0160(9) Uani 1 1 d . . . C3 C 0.6057(3) 0.4099(3) 0.07938(16) 0.0247(10) Uani 1 1 d . . . H3C H 0.6551 0.4093 0.0553 0.030 Uiso 1 1 calc R . . C4 C 0.6319(3) 0.3948(3) 0.13707(16) 0.0210(10) Uani 1 1 d . . . H4C H 0.7025 0.3816 0.1611 0.025 Uiso 1 1 calc R . . C5 C 0.5402(3) 0.4047(3) 0.15457(15) 0.0185(10) Uani 1 1 d . . . H5C H 0.5344 0.3983 0.1935 0.022 Uiso 1 1 calc R . . C6 C 0.4583(3) 0.4256(3) 0.10852(15) 0.0202(10) Uani 1 1 d . . . H6C H 0.3846 0.4381 0.1088 0.024 Uiso 1 1 calc R . . C7 C 0.4995(3) 0.4288(3) 0.06174(16) 0.0236(10) Uani 1 1 d . . . H7A H 0.4600 0.4444 0.0230 0.028 Uiso 1 1 calc R . . C1A C 0.3937(3) 0.1107(3) 0.17997(14) 0.0164(9) Uani 1 1 d . . . C2A C 0.3274(3) 0.2095(3) 0.17371(15) 0.0218(10) Uani 1 1 d . . . H2A H 0.3466 0.2839 0.1598 0.026 Uiso 1 1 calc R . . C3A C 0.2340(3) 0.2011(4) 0.18732(15) 0.0266(10) Uani 1 1 d . . . H3A H 0.1903 0.2702 0.1833 0.032 Uiso 1 1 calc R . . C4A C 0.2035(3) 0.0939(4) 0.20666(15) 0.0258(10) Uani 1 1 d . . . H4A H 0.1388 0.0883 0.2155 0.031 Uiso 1 1 calc R . . C5A C 0.2687(3) -0.0062(4) 0.21308(15) 0.0257(10) Uani 1 1 d . . . H5A H 0.2489 -0.0804 0.2269 0.031 Uiso 1 1 calc R . . C6A C 0.3620(3) 0.0020(3) 0.19938(14) 0.0205(10) Uani 1 1 d . . . H6A H 0.4054 -0.0673 0.2032 0.025 Uiso 1 1 calc R . . C7A C 0.5402(3) -0.0365(3) 0.14528(15) 0.0146(9) Uani 1 1 d . . . C8A C 0.4909(3) -0.0838(3) 0.09428(15) 0.0212(10) Uani 1 1 d . . . H8A H 0.4460 -0.0334 0.0683 0.025 Uiso 1 1 calc R . . C9A C 0.5057(3) -0.2025(3) 0.08074(15) 0.0222(10) Uani 1 1 d . . . H9A H 0.4709 -0.2335 0.0457 0.027 Uiso 1 1 calc R . . C10A C 0.5710(3) -0.2762(3) 0.11796(16) 0.0230(10) Uani 1 1 d . . . H10A H 0.5823 -0.3577 0.1084 0.028 Uiso 1 1 calc R . . C11A C 0.6204(3) -0.2313(3) 0.16936(16) 0.0208(10) Uani 1 1 d . . . H11A H 0.6647 -0.2824 0.1953 0.025 Uiso 1 1 calc R . . C12A C 0.6048(3) -0.1121(3) 0.18273(15) 0.0198(10) Uani 1 1 d . . . H12A H 0.6388 -0.0816 0.2180 0.024 Uiso 1 1 calc R . . C13A C 0.6127(3) 0.1439(3) 0.22627(14) 0.0156(9) Uani 1 1 d . . . C14A C 0.7150(3) 0.1510(3) 0.22436(16) 0.0222(10) Uani 1 1 d . . . H14A H 0.7319 0.1540 0.1897 0.027 Uiso 1 1 calc R . . C15A C 0.7922(3) 0.1538(3) 0.27192(17) 0.0277(11) Uani 1 1 d . . . H15A H 0.8619 0.1561 0.2698 0.033 Uiso 1 1 calc R . . C16A C 0.7695(3) 0.1533(3) 0.32288(16) 0.0291(11) Uani 1 1 d . . . H16A H 0.8232 0.1542 0.3556 0.035 Uiso 1 1 calc R . . C17A C 0.6679(3) 0.1515(3) 0.32555(16) 0.0274(11) Uani 1 1 d . . . H17A H 0.6513 0.1547 0.3602 0.033 Uiso 1 1 calc R . . C18A C 0.5900(3) 0.1449(3) 0.27743(15) 0.0188(10) Uani 1 1 d . . . H18A H 0.5204 0.1409 0.2796 0.023 Uiso 1 1 calc R . . C1B C 0.8699(3) -0.0512(3) -0.04348(15) 0.0200(9) Uani 1 1 d . . . H1B H 0.8586 -0.1362 -0.0419 0.024 Uiso 1 1 calc R . . C2B C 0.9256(3) -0.0084(3) -0.07878(15) 0.0206(10) Uani 1 1 d . . . H2B H 0.9528 -0.0629 -0.1009 0.025 Uiso 1 1 calc R . . C3B C 0.9410(3) 0.1141(4) -0.08145(15) 0.0228(10) Uani 1 1 d . . . H3B H 0.9782 0.1458 -0.1061 0.027 Uiso 1 1 calc R . . C4B C 0.9023(3) 0.1909(4) -0.04822(15) 0.0240(10) Uani 1 1 d . . . H4B H 0.9129 0.2762 -0.0493 0.029 Uiso 1 1 calc R . . C5B C 0.8480(3) 0.1426(3) -0.01339(15) 0.0208(10) Uani 1 1 d . . . H5B H 0.8217 0.1956 0.0098 0.025 Uiso 1 1 calc R . . C6B C 0.8232(3) -0.2501(3) 0.10497(16) 0.0228(10) Uani 1 1 d . . . H6B H 0.7928 -0.2962 0.0731 0.027 Uiso 1 1 calc R . . C7B C 0.8758(3) -0.3097(4) 0.15220(16) 0.0252(10) Uani 1 1 d . . . H7B H 0.8831 -0.3956 0.1525 0.030 Uiso 1 1 calc R . . C8B C 0.9174(3) -0.2427(4) 0.19867(17) 0.0269(11) Uani 1 1 d . . . H8B H 0.9533 -0.2820 0.2316 0.032 Uiso 1 1 calc R . . C9B C 0.9066(3) -0.1186(4) 0.19705(16) 0.0256(10) Uani 1 1 d . . . H9B H 0.9344 -0.0708 0.2288 0.031 Uiso 1 1 calc R . . C10B C 0.8548(3) -0.0648(4) 0.14864(15) 0.0205(10) Uani 1 1 d . . . H10B H 0.8476 0.0211 0.1475 0.025 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0201(3) 0.0105(3) 0.0153(3) -0.0009(2) 0.0055(3) 0.0002(3) Zn1 0.0188(3) 0.0166(3) 0.0170(3) -0.0014(2) 0.0051(2) 0.0013(2) Ag1 0.0406(2) 0.0272(2) 0.0279(2) -0.00237(16) 0.00993(17) -0.00110(17) P1 0.0188(6) 0.0128(6) 0.0155(6) -0.0002(5) 0.0051(5) 0.0011(5) I1 0.02778(18) 0.03325(18) 0.02875(17) -0.00158(14) 0.00616(14) 0.00836(14) I2 0.02627(17) 0.02822(17) 0.02847(17) 0.00188(14) 0.00683(13) 0.00237(13) N1 0.022(2) 0.0148(19) 0.022(2) -0.0031(16) 0.0076(17) 0.0003(16) N2 0.019(2) 0.0193(19) 0.017(2) 0.0015(16) 0.0033(17) 0.0024(16) N3 0.019(2) 0.0150(19) 0.0165(19) 0.0001(15) 0.0054(16) 0.0034(15) N4 0.017(2) 0.0175(19) 0.0180(19) 0.0001(16) 0.0070(16) 0.0010(15) C1 0.019(3) 0.015(2) 0.017(2) 0.0034(18) 0.000(2) -0.0083(19) C2 0.024(3) 0.011(2) 0.017(2) 0.0064(19) 0.011(2) 0.0123(19) C3 0.037(3) 0.010(2) 0.033(3) 0.0012(19) 0.022(2) -0.006(2) C4 0.023(3) 0.010(2) 0.027(3) -0.0037(19) 0.001(2) 0.0004(18) C5 0.028(3) 0.009(2) 0.018(2) -0.0046(18) 0.004(2) 0.0004(18) C6 0.024(3) 0.010(2) 0.029(3) 0.0009(19) 0.009(2) 0.0009(18) C7 0.036(3) 0.012(2) 0.020(2) 0.0056(19) 0.002(2) 0.000(2) C1A 0.019(2) 0.018(2) 0.013(2) -0.0020(18) 0.0053(19) -0.0021(18) C2A 0.024(3) 0.015(2) 0.028(3) -0.0002(19) 0.009(2) -0.0019(19) C3A 0.020(3) 0.028(3) 0.032(3) -0.005(2) 0.007(2) 0.006(2) C4A 0.019(3) 0.038(3) 0.022(2) -0.009(2) 0.008(2) -0.005(2) C5A 0.027(3) 0.030(3) 0.023(3) 0.002(2) 0.010(2) -0.010(2) C6A 0.021(3) 0.019(2) 0.021(2) 0.0016(19) 0.004(2) 0.0034(19) C7A 0.014(2) 0.013(2) 0.018(2) -0.0008(18) 0.0068(19) 0.0011(18) C8A 0.026(3) 0.016(2) 0.021(2) 0.0032(19) 0.003(2) 0.0031(19) C9A 0.032(3) 0.016(2) 0.019(2) -0.0017(19) 0.008(2) -0.005(2) C10A 0.031(3) 0.009(2) 0.035(3) -0.003(2) 0.018(2) -0.0009(19) C11A 0.023(3) 0.014(2) 0.026(3) 0.0039(19) 0.007(2) 0.0039(19) C12A 0.020(2) 0.020(2) 0.022(2) -0.0034(19) 0.009(2) -0.0020(19) C13A 0.024(3) 0.006(2) 0.016(2) 0.0003(17) 0.0043(19) 0.0016(17) C14A 0.027(3) 0.019(2) 0.021(2) 0.0002(19) 0.007(2) 0.0039(19) C15A 0.017(3) 0.029(3) 0.034(3) 0.001(2) 0.002(2) -0.001(2) C16A 0.035(3) 0.025(3) 0.020(3) -0.001(2) -0.006(2) -0.009(2) C17A 0.046(3) 0.024(3) 0.012(2) 0.0019(19) 0.006(2) -0.007(2) C18A 0.024(3) 0.014(2) 0.019(2) -0.0029(18) 0.006(2) -0.0046(18) C1B 0.020(2) 0.019(2) 0.019(2) 0.000(2) 0.002(2) 0.0023(19) C2B 0.018(2) 0.028(3) 0.016(2) -0.0055(19) 0.004(2) 0.0049(19) C3B 0.016(3) 0.034(3) 0.018(2) 0.003(2) 0.004(2) 0.000(2) C4B 0.026(3) 0.021(2) 0.024(2) 0.005(2) 0.005(2) -0.003(2) C5B 0.021(3) 0.020(2) 0.019(2) -0.0030(19) 0.001(2) 0.0051(19) C6B 0.024(3) 0.021(2) 0.027(3) -0.001(2) 0.013(2) -0.004(2) C7B 0.026(3) 0.019(2) 0.033(3) 0.008(2) 0.013(2) 0.002(2) C8B 0.018(3) 0.042(3) 0.023(3) 0.011(2) 0.009(2) 0.007(2) C9B 0.026(3) 0.033(3) 0.018(2) -0.001(2) 0.005(2) -0.003(2) C10B 0.019(2) 0.021(2) 0.022(2) -0.006(2) 0.006(2) 0.0000(19) _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 C2 1.847(4) . ? Fe1 C1 1.849(4) . ? Fe1 C7 2.077(4) . ? Fe1 C3 2.079(4) . ? Fe1 C6 2.092(4) . ? Fe1 C5 2.097(3) . ? Fe1 C4 2.100(4) . ? Fe1 P1 2.1945(12) . ? Zn1 N1 1.927(3) . ? Zn1 N2 1.931(3) . ? Zn1 N3 2.023(3) . ? Zn1 N4 2.025(3) . ? Ag1 I2 2.6823(7) . ? Ag1 I1 2.7746(8) . ? Ag1 I1 2.8396(7) 3_765 ? P1 C13A 1.828(4) . ? P1 C1A 1.832(4) . ? P1 C7A 1.842(4) . ? I1 Ag1 2.8396(7) 3_765 ? N1 C1 1.159(4) . ? N2 C2 1.160(4) 3_655 ? N3 C1B 1.340(4) . ? N3 C5B 1.346(4) . ? N4 C10B 1.329(4) . ? N4 C6B 1.345(4) . ? C2 N2 1.160(4) 3_655 ? C3 C7 1.400(5) . ? C3 C4 1.411(5) . ? C4 C5 1.408(5) . ? C5 C6 1.403(5) . ? C6 C7 1.414(5) . ? C1A C2A 1.388(5) . ? C1A C6A 1.396(5) . ? C2A C3A 1.380(5) . ? C3A C4A 1.376(5) . ? C4A C5A 1.391(5) . ? C5A C6A 1.380(5) . ? C7A C12A 1.388(5) . ? C7A C8A 1.388(5) . ? C8A C9A 1.376(5) . ? C9A C10A 1.376(5) . ? C10A C11A 1.386(5) . ? C11A C12A 1.382(5) . ? C13A C14A 1.386(5) . ? C13A C18A 1.389(5) . ? C14A C15A 1.374(5) . ? C15A C16A 1.384(5) . ? C16A C17A 1.381(5) . ? C17A C18A 1.390(5) . ? C1B C2B 1.374(5) . ? C2B C3B 1.368(5) . ? C3B C4B 1.376(5) . ? C4B C5B 1.374(5) . ? C6B C7B 1.385(5) . ? C7B C8B 1.375(5) . ? C8B C9B 1.373(5) . ? C9B C10B 1.375(5) . ? 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 C2 Fe1 C1 90.90(15) . . ? C2 Fe1 C7 89.88(15) . . ? C1 Fe1 C7 116.46(15) . . ? C2 Fe1 C3 120.46(16) . . ? C1 Fe1 C3 89.86(15) . . ? C7 Fe1 C3 39.38(14) . . ? C2 Fe1 C6 95.32(15) . . ? C1 Fe1 C6 155.04(15) . . ? C7 Fe1 C6 39.66(13) . . ? C3 Fe1 C6 66.19(15) . . ? C2 Fe1 C5 131.09(15) . . ? C1 Fe1 C5 137.61(15) . . ? C7 Fe1 C5 65.91(14) . . ? C3 Fe1 C5 65.78(15) . . ? C6 Fe1 C5 39.14(13) . . ? C2 Fe1 C4 156.11(15) . . ? C1 Fe1 C4 100.23(15) . . ? C7 Fe1 C4 66.24(15) . . ? C3 Fe1 C4 39.47(14) . . ? C6 Fe1 C4 66.13(15) . . ? C5 Fe1 C4 39.21(13) . . ? C2 Fe1 P1 92.44(11) . . ? C1 Fe1 P1 89.68(11) . . ? C7 Fe1 P1 153.73(11) . . ? C3 Fe1 P1 147.10(12) . . ? C6 Fe1 P1 114.10(11) . . ? C5 Fe1 P1 93.46(11) . . ? C4 Fe1 P1 108.56(11) . . ? N1 Zn1 N2 118.43(13) . . ? N1 Zn1 N3 105.86(12) . . ? N2 Zn1 N3 103.30(12) . . ? N1 Zn1 N4 107.08(12) . . ? N2 Zn1 N4 109.48(12) . . ? N3 Zn1 N4 112.76(12) . . ? I2 Ag1 I1 134.185(16) . . ? I2 Ag1 I1 125.47(2) . 3_765 ? I1 Ag1 I1 100.27(2) . 3_765 ? C13A P1 C1A 105.09(17) . . ? C13A P1 C7A 101.15(16) . . ? C1A P1 C7A 101.43(16) . . ? C13A P1 Fe1 112.95(12) . . ? C1A P1 Fe1 117.13(12) . . ? C7A P1 Fe1 117.07(12) . . ? Ag1 I1 Ag1 79.73(2) . 3_765 ? C1 N1 Zn1 163.4(3) . . ? C2 N2 Zn1 157.7(3) 3_655 . ? C1B N3 C5B 118.3(3) . . ? C1B N3 Zn1 120.6(2) . . ? C5B N3 Zn1 120.8(2) . . ? C10B N4 C6B 118.9(3) . . ? C10B N4 Zn1 120.5(3) . . ? C6B N4 Zn1 120.5(3) . . ? N1 C1 Fe1 178.6(3) . . ? N2 C2 Fe1 176.8(3) 3_655 . ? C7 C3 C4 108.6(3) . . ? C7 C3 Fe1 70.2(2) . . ? C4 C3 Fe1 71.1(2) . . ? C5 C4 C3 107.1(3) . . ? C5 C4 Fe1 70.3(2) . . ? C3 C4 Fe1 69.5(2) . . ? C6 C5 C4 108.9(3) . . ? C6 C5 Fe1 70.2(2) . . ? C4 C5 Fe1 70.5(2) . . ? C5 C6 C7 107.4(3) . . ? C5 C6 Fe1 70.6(2) . . ? C7 C6 Fe1 69.6(2) . . ? C3 C7 C6 108.0(3) . . ? C3 C7 Fe1 70.4(2) . . ? C6 C7 Fe1 70.8(2) . . ? C2A C1A C6A 118.0(3) . . ? C2A C1A P1 120.5(3) . . ? C6A C1A P1 121.6(3) . . ? C3A C2A C1A 121.0(4) . . ? C4A C3A C2A 120.7(4) . . ? C3A C4A C5A 119.2(4) . . ? C6A C5A C4A 120.1(4) . . ? C5A C6A C1A 121.0(4) . . ? C12A C7A C8A 118.3(3) . . ? C12A C7A P1 122.4(3) . . ? C8A C7A P1 119.2(3) . . ? C9A C8A C7A 121.2(4) . . ? C10A C9A C8A 119.9(4) . . ? C9A C10A C11A 119.9(4) . . ? C12A C11A C10A 119.8(4) . . ? C11A C12A C7A 120.8(4) . . ? C14A C13A C18A 118.3(4) . . ? C14A C13A P1 117.5(3) . . ? C18A C13A P1 124.0(3) . . ? C15A C14A C13A 120.8(4) . . ? C14A C15A C16A 120.7(4) . . ? C17A C16A C15A 119.2(4) . . ? C16A C17A C18A 119.9(4) . . ? C13A C18A C17A 120.9(4) . . ? N3 C1B C2B 122.4(4) . . ? C3B C2B C1B 118.8(4) . . ? C2B C3B C4B 119.5(4) . . ? C5B C4B C3B 119.0(4) . . ? N3 C5B C4B 121.9(4) . . ? N4 C6B C7B 121.3(4) . . ? C8B C7B C6B 119.1(4) . . ? C9B C8B C7B 119.3(4) . . ? C8B C9B C10B 118.8(4) . . ? N4 C10B C9B 122.6(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.511 _refine_diff_density_min -0.377 _refine_diff_density_rms 0.080 #===END data_ja1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H52 Fe2 I2 N4 O2 P2 Zn2' _chemical_formula_weight 1239.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 29.029(11) _cell_length_b 18.924(7) _cell_length_c 9.052(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4973(3) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.077 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3012 _exptl_absorpt_coefficient_mu 4.282 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 31287 _diffrn_reflns_av_R_equivalents 0.1347 _diffrn_reflns_av_sigmaI/netI 0.1758 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 28.33 _reflns_number_total 6279 _reflns_number_gt 2692 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0478P)^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 6279 _refine_ls_number_parameters 332 _refine_ls_number_restraints 230 _refine_ls_R_factor_all 0.1619 _refine_ls_R_factor_gt 0.0541 _refine_ls_wR_factor_ref 0.1509 _refine_ls_wR_factor_gt 0.1276 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.272 _refine_ls_shift/su_max 1.850 _refine_ls_shift/su_mean 0.093 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 0.29918(5) 0.7500 0.66077(19) 0.0222(4) Uani 1 2 d S . . Zn2 Zn 0.51723(5) 0.7500 0.52312(19) 0.0217(4) Uani 1 2 d S . . Fe1 Fe 0.39964(4) 0.56090(7) 0.49494(16) 0.0192(3) Uani 1 1 d . . . I1 I 0.23112(3) 0.7500 0.48313(13) 0.0340(3) Uani 1 2 d S . . I2 I 0.58356(3) 0.7500 0.70582(13) 0.0350(3) Uani 1 2 d S . . N1 N 0.3368(3) 0.6655(4) 0.6437(9) 0.023(2) Uani 1 1 d . . . H1A H 0.3331 0.6461 0.7288 0.028 Uiso 1 1 calc R . . N2 N 0.4774(3) 0.6676(4) 0.5086(9) 0.023(2) Uani 1 1 d . . . O1 O 0.2722(3) 0.7500 0.8709(11) 0.028(3) Uani 1 2 d S . . P6 P 0.37827(8) 0.59822(14) 0.2754(3) 0.0189(6) Uani 1 1 d . . . C1 C 0.3616(3) 0.6254(5) 0.5852(11) 0.018(2) Uani 1 1 d . . . C2 C 0.4469(3) 0.6265(5) 0.5015(11) 0.021(2) Uani 1 1 d . . . C3 C 0.4302(3) 0.4926(5) 0.6450(13) 0.029(2) Uani 1 1 d U . . H3A H 0.4531 0.5053 0.7201 0.035 Uiso 1 1 calc R . . C4 C 0.4397(4) 0.4696(5) 0.4982(12) 0.029(2) Uani 1 1 d U . . H4A H 0.4704 0.4644 0.4543 0.035 Uiso 1 1 calc R . . C5 C 0.3981(4) 0.4540(5) 0.4287(13) 0.030(2) Uani 1 1 d U . . H5A H 0.3943 0.4365 0.3275 0.037 Uiso 1 1 calc R . . C6 C 0.3623(4) 0.4677(5) 0.5315(12) 0.029(2) Uani 1 1 d U . . H6A H 0.3293 0.4610 0.5141 0.035 Uiso 1 1 calc R . . C7 C 0.3827(3) 0.4907(5) 0.6641(13) 0.028(2) Uani 1 1 d U . . H7A H 0.3662 0.5028 0.7551 0.033 Uiso 1 1 calc R . . C1A C 0.4209(3) 0.6047(6) 0.1281(12) 0.026(2) Uani 1 1 d U . . C2A C 0.4640(4) 0.5795(6) 0.1487(13) 0.037(2) Uani 1 1 d U . . H2AA H 0.4714 0.5572 0.2372 0.044 Uiso 1 1 calc R . . C3A C 0.4981(4) 0.5866(7) 0.0372(13) 0.044(3) Uani 1 1 d U . . H3AA H 0.5274 0.5678 0.0511 0.052 Uiso 1 1 calc R . . C4A C 0.4874(4) 0.6215(6) -0.0920(12) 0.037(2) Uani 1 1 d U . . H4AA H 0.5100 0.6285 -0.1635 0.044 Uiso 1 1 calc R . . C5A C 0.4434(4) 0.6459(6) -0.1155(13) 0.034(2) Uani 1 1 d U . . H5AA H 0.4358 0.6685 -0.2035 0.041 Uiso 1 1 calc R . . C6A C 0.4105(4) 0.6366(6) -0.0062(12) 0.032(2) Uani 1 1 d U . . H6AA H 0.3805 0.6521 -0.0231 0.038 Uiso 1 1 calc R . . C7A C 0.3335(3) 0.5419(5) 0.1938(12) 0.024(2) Uani 1 1 d U . . C8A C 0.3439(4) 0.4895(5) 0.0906(12) 0.029(2) Uani 1 1 d U . . H8AA H 0.3736 0.4861 0.0523 0.035 Uiso 1 1 calc R . . C9A C 0.3104(4) 0.4431(6) 0.0456(12) 0.033(2) Uani 1 1 d U . . H9AA H 0.3173 0.4081 -0.0229 0.040 Uiso 1 1 calc R . . C10A C 0.2657(4) 0.4484(6) 0.1028(12) 0.036(2) Uani 1 1 d U . . H10A H 0.2430 0.4167 0.0731 0.044 Uiso 1 1 calc R . . C11A C 0.2554(4) 0.4998(6) 0.2010(12) 0.033(2) Uani 1 1 d U . . H11A H 0.2256 0.5034 0.2374 0.039 Uiso 1 1 calc R . . C12A C 0.2885(3) 0.5469(6) 0.2484(12) 0.029(2) Uani 1 1 d U . . H12A H 0.2809 0.5819 0.3163 0.035 Uiso 1 1 calc R . . C13A C 0.3495(3) 0.6837(5) 0.2627(11) 0.020(2) Uani 1 1 d U . . H13A H 0.3373 0.6888 0.1636 0.025 Uiso 1 1 calc R . . H13B H 0.3236 0.6836 0.3303 0.025 Uiso 1 1 calc R . . C14A C 0.3800(4) 0.7500 0.2975(17) 0.022(3) Uani 1 2 d SU . . C1B C 0.2474(4) 0.6880(7) 0.9176(14) 0.051(3) Uani 1 1 d U . . H1BA H 0.2688 0.6523 0.9523 0.061 Uiso 1 1 calc R . . H1BB H 0.2301 0.6686 0.8356 0.061 Uiso 1 1 calc R . . C2B C 0.2157(4) 0.7089(6) 1.0387(14) 0.052(3) Uani 1 1 d U . . O2 O 0.54840(13) 0.7500 0.3204(6) 0.088(3) Uani 1 2 d SD . 1 C1C C 0.5865(3) 0.6988(3) 0.3104(13) 0.094(3) Uani 0.50 1 d PDU . 1 H1CA H 0.5746 0.6517 0.3204 0.112 Uiso 0.50 1 d PR . 1 H1CB H 0.6104 0.7062 0.3819 0.112 Uiso 0.50 1 d PR . 1 C2C C 0.60328(17) 0.7118(2) 0.1502(8) 0.093(2) Uani 0.50 1 d PDU . 1 H2CA H 0.5828 0.6924 0.0774 0.112 Uiso 0.50 1 d PR . 1 H2CB H 0.6338 0.6937 0.1348 0.112 Uiso 0.50 1 d PR . 1 C3C C 0.60088(19) 0.7914(2) 0.1468(9) 0.092(3) Uani 0.00 1 d PDU . 1 H3CA H 0.5810 0.8095 0.0711 0.110 Uiso 0.00 1 d PR . 1 H3CB H 0.6312 0.8108 0.1342 0.110 Uiso 0.00 1 d PR . 1 C4C C 0.5831(4) 0.8060(4) 0.3033(18) 0.091(4) Uani 0.00 1 d PDU . 1 H4CA H 0.6069 0.8033 0.3767 0.110 Uiso 0.00 1 d PR . 1 H4CB H 0.5690 0.8519 0.3074 0.110 Uiso 0.00 1 d PR . 1 O2' O 0.54840(13) 0.7500 0.3204(6) 0.088(3) Uani 0.50 2 d SPD . 2 C1C' C 0.5595(2) 0.69174(17) 0.2204(8) 0.114(3) Uani 1 1 d DU . 2 H1CC H 0.5356 0.6880 0.1475 0.136 Uiso 1 1 d R . 2 H1CD H 0.5620 0.6475 0.2719 0.136 Uiso 1 1 d R . 2 C2C' C 0.60328(17) 0.7118(2) 0.1502(8) 0.093(2) Uani 0.25 1 d PDU . 2 H2CC H 0.6056 0.6923 0.0522 0.112 Uiso 0.25 1 d PR . 2 H2CD H 0.6292 0.6928 0.2075 0.112 Uiso 0.25 1 d PR . 2 C3C' C 0.60088(19) 0.7914(2) 0.1468(9) 0.092(3) Uani 0.00 1 d PDU . 2 H3CC H 0.6049 0.8087 0.0526 0.110 Uiso 0.00 1 d PR . 2 H3CD H 0.6275 0.8092 0.2096 0.110 Uiso 0.00 1 d PR . 2 C4C' C 0.5554(2) 0.8063(2) 0.2117(9) 0.091(4) Uani 0.00 1 d PDU . 2 H4CC H 0.5561 0.8512 0.2607 0.110 Uiso 0.00 1 d PR . 2 H4CD H 0.5317 0.8070 0.1377 0.110 Uiso 0.00 1 d PR . 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 Zn1 0.0196(8) 0.0241(10) 0.0230(10) 0.000 0.0044(8) 0.000 Zn2 0.0158(8) 0.0216(9) 0.0275(10) 0.000 0.0002(8) 0.000 Fe1 0.0174(7) 0.0172(7) 0.0229(8) 0.0017(7) -0.0008(7) 0.0002(6) I1 0.0234(5) 0.0370(7) 0.0415(7) 0.000 -0.0049(5) 0.000 I2 0.0284(6) 0.0355(6) 0.0410(7) 0.000 -0.0108(5) 0.000 N1 0.025(5) 0.027(5) 0.018(5) 0.007(4) 0.007(4) -0.002(4) N2 0.020(4) 0.019(5) 0.031(5) 0.001(4) 0.007(4) 0.000(4) O1 0.033(6) 0.026(6) 0.024(6) 0.000 0.011(5) 0.000 P6 0.0190(13) 0.0173(14) 0.0204(15) -0.0012(12) -0.0017(12) -0.0022(11) C1 0.015(5) 0.022(6) 0.017(6) 0.000(5) 0.001(5) -0.007(4) C2 0.026(5) 0.025(6) 0.013(6) 0.003(5) -0.006(5) 0.014(5) C3 0.034(5) 0.019(4) 0.034(5) 0.009(4) -0.001(4) 0.001(4) C4 0.032(4) 0.019(4) 0.036(5) 0.005(4) 0.003(5) -0.001(4) C5 0.043(5) 0.018(4) 0.031(5) 0.005(4) -0.002(4) -0.001(4) C6 0.029(4) 0.019(4) 0.039(5) 0.008(4) 0.001(4) -0.001(4) C7 0.030(4) 0.021(4) 0.032(5) 0.011(4) 0.007(4) 0.007(4) C1A 0.021(4) 0.032(5) 0.025(5) 0.000(4) 0.001(4) 0.002(4) C2A 0.028(4) 0.052(5) 0.031(5) 0.006(5) 0.005(4) 0.003(4) C3A 0.034(5) 0.061(6) 0.036(5) 0.010(5) 0.007(5) 0.005(5) C4A 0.040(5) 0.047(5) 0.024(5) 0.004(4) 0.010(5) -0.005(5) C5A 0.045(5) 0.036(5) 0.022(5) -0.001(4) 0.003(4) -0.007(4) C6A 0.031(4) 0.041(5) 0.025(5) -0.004(4) 0.004(4) -0.001(4) C7A 0.026(4) 0.020(4) 0.026(5) 0.004(4) -0.003(4) -0.008(4) C8A 0.032(4) 0.024(5) 0.031(5) -0.002(4) 0.000(4) -0.011(4) C9A 0.039(5) 0.028(5) 0.033(5) -0.004(4) -0.003(4) -0.014(4) C10A 0.039(5) 0.034(5) 0.037(5) -0.001(4) -0.006(5) -0.014(4) C11A 0.029(4) 0.034(5) 0.036(5) 0.001(4) 0.001(4) -0.008(4) C12A 0.027(4) 0.031(5) 0.031(5) 0.008(4) 0.000(4) -0.005(4) C13A 0.018(4) 0.024(5) 0.020(5) 0.002(4) 0.002(4) 0.002(4) C14A 0.020(6) 0.015(6) 0.031(7) 0.000 -0.005(6) 0.000 C1B 0.064(7) 0.044(7) 0.043(7) 0.001(6) 0.021(6) -0.011(6) C2B 0.065(7) 0.040(7) 0.052(7) -0.006(6) 0.028(6) -0.011(6) O2 0.077(7) 0.075(7) 0.111(9) 0.000 0.041(7) 0.000 C1C 0.113(6) 0.071(6) 0.096(6) -0.030(6) 0.035(6) 0.024(6) C2C 0.110(4) 0.074(4) 0.095(4) -0.026(4) 0.040(4) 0.018(4) C3C 0.108(5) 0.074(5) 0.093(5) -0.025(5) 0.039(5) 0.018(5) C4C 0.108(7) 0.074(7) 0.093(7) -0.025(7) 0.039(7) 0.018(7) O2' 0.077(7) 0.075(7) 0.111(9) 0.000 0.041(7) 0.000 C1C' 0.142(6) 0.086(6) 0.113(6) -0.031(6) 0.036(6) 0.014(6) C2C' 0.110(4) 0.074(4) 0.095(4) -0.026(4) 0.040(4) 0.018(4) C3C' 0.108(5) 0.074(5) 0.093(5) -0.025(5) 0.039(5) 0.018(5) C4C' 0.108(7) 0.074(7) 0.093(7) -0.025(7) 0.039(7) 0.018(7) _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 N1 1.943(8) . ? Zn1 N1 1.943(8) 7_575 ? Zn1 O1 2.058(10) . ? Zn1 I1 2.547(2) . ? Zn2 N2 1.946(8) 7_575 ? Zn2 N2 1.946(8) . ? Zn2 O2 2.046(5) . ? Zn2 I2 2.538(2) . ? Fe1 C2 1.851(11) . ? Fe1 C1 1.838(10) . ? Fe1 C3 2.075(11) . ? Fe1 C4 2.084(10) . ? Fe1 C7 2.086(10) . ? Fe1 C6 2.097(10) . ? Fe1 C5 2.110(11) . ? Fe1 P6 2.198(3) . ? N1 C1 1.171(11) . ? N2 C2 1.179(12) . ? O1 C1B 1.438(12) 7_575 ? O1 C1B 1.438(12) . ? P6 C1A 1.824(10) . ? P6 C7A 1.836(10) . ? P6 C13A 1.824(9) . ? C3 C7 1.391(13) . ? C3 C4 1.425(15) . ? C4 C5 1.393(14) . ? C5 C6 1.420(14) . ? C6 C7 1.408(15) . ? C1A C2A 1.351(13) . ? C1A C6A 1.391(14) . ? C2A C3A 1.420(14) . ? C3A C4A 1.379(15) . ? C4A C5A 1.375(15) . ? C5A C6A 1.387(14) . ? C7A C8A 1.396(14) . ? C7A C12A 1.399(13) . ? C8A C9A 1.374(13) . ? C9A C10A 1.401(14) . ? C10A C11A 1.350(15) . ? C11A C12A 1.378(14) . ? C13A C14A 1.567(12) . ? C14A C13A 1.567(12) 7_575 ? C1B C2B 1.486(16) . ? C2B C2B 1.56(2) 7_575 ? O2 C4C 1.470(3) . ? O2 C1C 1.473(3) 7_575 ? O2 C1C 1.473(3) . ? C1C C2C 1.549(8) . ? C1C C1C 1.938(13) 7_575 ? C2C C2C 1.447(8) 7_575 ? C2C C3C 1.510(2) . ? C3C C2C 0.097(9) 7_575 ? C3C C4C 1.533(10) . ? C3C C1C 1.549(9) 7_575 ? C4C C1C 0.15(2) 7_575 ? C4C C2C 1.542(10) 7_575 ? C4C' C1C' 0.148(15) 7_575 ? C4C' C2C' 1.536(6) 7_575 ? 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 Zn1 N1 110.8(5) . 7_575 ? N1 Zn1 O1 106.7(3) . . ? N1 Zn1 O1 106.7(3) 7_575 . ? N1 Zn1 I1 112.7(2) . . ? N1 Zn1 I1 112.7(2) 7_575 . ? O1 Zn1 I1 106.7(3) . . ? N2 Zn2 N2 106.5(4) 7_575 . ? N2 Zn2 O2 101.7(3) 7_575 . ? N2 Zn2 O2 101.7(3) . . ? N2 Zn2 I2 119.7(2) 7_575 . ? N2 Zn2 I2 119.7(2) . . ? O2 Zn2 I2 104.41(14) . . ? C2 Fe1 C1 89.2(4) . . ? C2 Fe1 C3 94.5(4) . . ? C1 Fe1 C3 112.4(4) . . ? C2 Fe1 C4 98.1(4) . . ? C1 Fe1 C4 151.7(4) . . ? C3 Fe1 C4 40.1(4) . . ? C2 Fe1 C7 125.3(4) . . ? C1 Fe1 C7 87.4(4) . . ? C3 Fe1 C7 39.1(4) . . ? C4 Fe1 C7 66.0(4) . . ? C2 Fe1 C6 160.4(4) . . ? C1 Fe1 C6 100.3(4) . . ? C3 Fe1 C6 66.0(4) . . ? C4 Fe1 C6 65.7(4) . . ? C7 Fe1 C6 39.3(4) . . ? C2 Fe1 C5 131.8(4) . . ? C1 Fe1 C5 138.7(4) . . ? C3 Fe1 C5 66.3(4) . . ? C4 Fe1 C5 38.8(4) . . ? C7 Fe1 C5 66.0(4) . . ? C6 Fe1 C5 39.4(4) . . ? C2 Fe1 P6 91.3(3) . . ? C1 Fe1 P6 91.1(3) . . ? C3 Fe1 P6 155.9(3) . . ? C4 Fe1 P6 115.9(3) . . ? C7 Fe1 P6 143.3(3) . . ? C6 Fe1 P6 105.5(3) . . ? C5 Fe1 P6 92.6(3) . . ? C1 N1 Zn1 156.0(8) . . ? C2 N2 Zn2 167.9(7) . . ? C1B O1 C1B 109.2(12) 7_575 . ? C1B O1 Zn1 117.5(6) 7_575 . ? C1B O1 Zn1 117.5(6) . . ? C1A P6 C7A 103.0(5) . . ? C1A P6 C13A 101.8(5) . . ? C7A P6 C13A 99.5(4) . . ? C1A P6 Fe1 119.4(3) . . ? C7A P6 Fe1 112.1(3) . . ? C13A P6 Fe1 118.1(3) . . ? N1 C1 Fe1 178.6(9) . . ? N2 C2 Fe1 178.5(9) . . ? C7 C3 C4 107.5(10) . . ? C7 C3 Fe1 70.9(6) . . ? C4 C3 Fe1 70.3(6) . . ? C5 C4 C3 108.5(9) . . ? C5 C4 Fe1 71.6(6) . . ? C3 C4 Fe1 69.6(6) . . ? C4 C5 C6 107.5(10) . . ? C4 C5 Fe1 69.6(6) . . ? C6 C5 Fe1 69.8(6) . . ? C5 C6 C7 107.9(9) . . ? C5 C6 Fe1 70.8(6) . . ? C7 C6 Fe1 69.9(6) . . ? C3 C7 C6 108.6(10) . . ? C3 C7 Fe1 70.1(6) . . ? C6 C7 Fe1 70.7(6) . . ? C2A C1A C6A 118.4(10) . . ? C2A C1A P6 120.3(9) . . ? C6A C1A P6 121.3(8) . . ? C1A C2A C3A 120.9(11) . . ? C4A C3A C2A 119.4(11) . . ? C5A C4A C3A 120.1(11) . . ? C4A C5A C6A 119.2(11) . . ? C1A C6A C5A 121.9(10) . . ? C8A C7A C12A 119.1(9) . . ? C8A C7A P6 121.9(8) . . ? C12A C7A P6 118.7(8) . . ? C9A C8A C7A 119.9(10) . . ? C8A C9A C10A 120.1(11) . . ? C11A C10A C9A 119.9(10) . . ? C10A C11A C12A 121.2(10) . . ? C11A C12A C7A 119.8(10) . . ? C14A C13A P6 116.1(6) . . ? C13A C14A C13A 106.4(10) . 7_575 ? O1 C1B C2B 108.0(10) . . ? C1B C2B C2B 105.4(7) . 7_575 ? C4C O2 C1C 5.8(8) . 7_575 ? C4C O2 C1C 87.4(6) . . ? C1C O2 C1C 82.3(7) 7_575 . ? C4C O2 Zn2 113.4(5) . . ? C1C O2 Zn2 112.8(4) 7_575 . ? C1C O2 Zn2 112.8(4) . . ? O2 C1C C2C 100.9(4) . . ? O2 C1C C1C 48.8(3) . 7_575 ? C2C C1C C1C 80.9(3) . 7_575 ? C2C C2C C3C 2.9(3) 7_575 . ? C2C C2C C1C 99.1(3) 7_575 . ? C3C C2C C1C 99.4(3) . . ? C2C C3C C4C 94(4) 7_575 . ? C2C C3C C2C 49(5) 7_575 . ? C4C C3C C2C 100.1(4) . . ? C2C C3C C1C 88(4) 7_575 7_575 ? C4C C3C C1C 5.5(8) . 7_575 ? C2C C3C C1C 96.4(4) . 7_575 ? C1C C4C O2 88.3(15) 7_575 . ? C1C C4C C3C 94(4) 7_575 . ? O2 C4C C3C 101.4(5) . . ? C1C C4C C2C 90(4) 7_575 7_575 ? O2 C4C C2C 101.4(5) . 7_575 ? C3C C4C C2C 3.6(3) . 7_575 ? C1C' C4C' C2C' 61(2) 7_575 7_575 ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.520 _refine_diff_density_min -2.098 _refine_diff_density_rms 0.187