# Copyright The Royal Society of Chemistry, 1998 # CCDC Number: 186/1185 # P.Li, I.J. Scowen, J.E. Davies and M.A. Halcrow # Coordination Chemistry of Bis-(ferrocenylcarbaldimine) Schiff Bases data_ib001/PL1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,2-Bis-[ferrocen-1-ylcarbaldimino]ethane-dichlorozinc(II) ; _chemical_name_common ? _chemical_formula_moiety 'C24 H24 Cl2 Fe2 N2 Zn' _chemical_formula_sum 'C24 H24 Cl2 Fe2 N2 Zn' _chemical_formula_weight 588.42 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 '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 11.297(2) _cell_length_b 14.614(3) _cell_length_c 14.625(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2414.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 955 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description octahedron _exptl_crystal_colour red _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.619 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 2.406 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 1.143 _exptl_absorpt_correction_T_max 0.861 _exptl_absorpt_process_details 'XABS: Parkin, S et al. (1995), J. Appl. Cryst. 28, 53' _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 'Stoe IPDS' _diffrn_measurement_method 'image plate' _diffrn_detector_area_resol_mean 0.70 _diffrn_standards_number 100 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 4174 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 6.03 _diffrn_reflns_theta_max 24.99 _reflns_number_total 4174 _reflns_number_gt 3913 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS' _computing_cell_refinement 'Stoe IPDS' _computing_data_reduction 'Stoe IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL (Sheldrick, 1987)' _computing_publication_material 'Siemens SHELXTL (Sheldrick, 1987)' _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. One Cp-ring is disordered: C(41)-C(45): 0.65 occupancy C(412)-C(452): 0.35 occupancy ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0431P)^2^+1.2850P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.002(17) _refine_ls_number_reflns 4174 _refine_ls_number_parameters 275 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0383 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0872 _refine_ls_wR_factor_gt 0.0844 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.101 _refine_ls_shift/su_mean 0.011 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn -0.47617(4) -0.89638(3) -0.14170(3) 0.05020(13) Uani 1 d . . . Fe1 Fe -0.56551(6) -0.93421(5) 0.17714(5) 0.06531(19) Uani 1 d . . . Fe2 Fe -0.36097(5) -0.88058(4) -0.45220(4) 0.05412(16) Uani 1 d . . . Cl1 Cl -0.28340(10) -0.86606(10) -0.13742(9) 0.0792(4) Uani 1 d . . . Cl2 Cl -0.51936(12) -1.04337(7) -0.12933(8) 0.0741(3) Uani 1 d . . . N1 N -0.5832(3) -0.8170(2) -0.0583(3) 0.0604(9) Uani 1 d . . . N2 N -0.5620(3) -0.8296(3) -0.2468(2) 0.0594(8) Uani 1 d . . . C1 C -0.6774(5) -0.7803(4) -0.1167(3) 0.0756(14) Uani 1 d . . . H1A H -0.7153 -0.7289 -0.0866 0.091 Uiso 1 calc R . . H1B H -0.7368 -0.8270 -0.1275 0.091 Uiso 1 calc R . . C2 C -0.6245(6) -0.7499(4) -0.2062(3) 0.0825(16) Uani 1 d . . . H2A H -0.6864 -0.7288 -0.2471 0.099 Uiso 1 calc R . . H2B H -0.5694 -0.7000 -0.1962 0.099 Uiso 1 calc R . . C10 C -0.5853(4) -0.7957(3) 0.0267(3) 0.0661(11) Uani 1 d . . . H10 H -0.6429 -0.7539 0.0445 0.079 Uiso 1 calc R . . C11 C -0.5084(4) -0.8295(3) 0.0975(3) 0.0630(11) Uani 1 d . . . C12 C -0.4256(4) -0.9039(4) 0.0957(3) 0.0629(10) Uani 1 d . . . H12 H -0.4024 -0.9364 0.0441 0.075 Uiso 1 calc R . . C13 C -0.3855(4) -0.9195(4) 0.1861(3) 0.0726(13) Uani 1 d . . . H13 H -0.3306 -0.9632 0.2043 0.087 Uiso 1 calc R . . C14 C -0.4445(5) -0.8560(4) 0.2438(3) 0.0785(15) Uani 1 d . . . H14 H -0.4347 -0.8518 0.3068 0.094 Uiso 1 calc R . . C15 C -0.5200(5) -0.8005(4) 0.1911(3) 0.0719(12) Uani 1 d . . . H15 H -0.5684 -0.7538 0.2128 0.086 Uiso 1 calc R . . C20 C -0.5704(4) -0.8405(3) -0.3327(3) 0.0630(11) Uani 1 d . . . H20 H -0.6176 -0.7989 -0.3641 0.076 Uiso 1 calc R . . C21 C -0.5141(4) -0.9108(3) -0.3864(3) 0.0579(10) Uani 1 d . . . C22 C -0.4231(4) -0.9751(3) -0.3620(3) 0.0558(9) Uani 1 d . . . H22 H -0.3941 -0.9857 -0.3034 0.067 Uiso 1 calc R . . C23 C -0.3858(4) -1.0190(3) -0.4426(3) 0.0616(10) Uani 1 d . . . H23 H -0.3277 -1.0640 -0.4464 0.074 Uiso 1 calc R . . C24 C -0.4506(5) -0.9838(4) -0.5165(3) 0.0697(12) Uani 1 d . . . H24 H -0.4423 -1.0017 -0.5772 0.084 Uiso 1 calc R . . C25 C -0.5295(5) -0.9174(4) -0.4846(3) 0.0686(12) Uani 1 d . . . H25 H -0.5822 -0.8837 -0.5199 0.082 Uiso 1 calc R . . C31 C -0.7358(9) -0.9497(9) 0.2151(10) 0.147(4) Uani 1 d . . . H31 H -0.7856 -0.9040 0.2369 0.176 Uiso 1 calc R . . C32 C -0.6691(12) -0.9981(10) 0.2695(6) 0.144(5) Uani 1 d . . . H32 H -0.6616 -0.9927 0.3326 0.173 Uiso 1 calc R . . C33 C -0.6055(7) -1.0662(6) 0.2062(15) 0.179(6) Uani 1 d . . . H33 H -0.5506 -1.1118 0.2191 0.215 Uiso 1 calc R . . C34 C -0.6570(12) -1.0375(8) 0.1208(7) 0.129(3) Uani 1 d . . . H34 H -0.6406 -1.0651 0.0649 0.155 Uiso 1 calc R . . C35 C -0.7285(10) -0.9691(10) 0.1303(12) 0.155(4) Uani 1 d . . . H35 H -0.7680 -0.9392 0.0832 0.186 Uiso 1 calc R . . C41 C -0.3204(9) -0.7454(6) -0.4340(9) 0.072(2) Uiso 0.65 d PD A 1 H41 H -0.3674 -0.7011 -0.4063 0.086 Uiso 0.65 calc PR A 1 C42 C -0.2377(10) -0.8022(8) -0.3885(6) 0.078(3) Uiso 0.65 d PD A 1 H42 H -0.2230 -0.8032 -0.3260 0.093 Uiso 0.65 calc PR A 1 C43 C -0.1808(6) -0.8579(5) -0.4561(7) 0.0583(19) Uiso 0.65 d PD A 1 H43 H -0.1207 -0.9001 -0.4459 0.070 Uiso 0.65 calc PR A 1 C44 C -0.2342(7) -0.8361(6) -0.5426(5) 0.0648(17) Uiso 0.65 d PD A 1 H44 H -0.2158 -0.8626 -0.5986 0.078 Uiso 0.65 calc PR A 1 C45 C -0.3199(9) -0.7667(7) -0.5273(7) 0.075(2) Uiso 0.65 d PD A 1 H45 H -0.3677 -0.7400 -0.5717 0.090 Uiso 0.65 calc PR A 1 C412 C -0.2909(16) -0.7629(12) -0.3866(12) 0.078(4) Uiso 0.35 d PD B 2 H412 H -0.3136 -0.7346 -0.3324 0.094 Uiso 0.35 calc PR B 2 C422 C -0.2038(17) -0.8306(14) -0.3927(11) 0.080(5) Uiso 0.35 d PD B 2 H422 H -0.1615 -0.8579 -0.3455 0.096 Uiso 0.35 calc PR B 2 C432 C -0.1952(14) -0.8481(11) -0.4906(13) 0.069(4) Uiso 0.35 d PD B 2 H432 H -0.1443 -0.8902 -0.5177 0.083 Uiso 0.35 calc PR B 2 C442 C -0.2758(19) -0.7917(15) -0.5382(11) 0.097(6) Uiso 0.35 d PD B 2 H442 H -0.2851 -0.7873 -0.6012 0.116 Uiso 0.35 calc PR B 2 C452 C -0.3388(14) -0.7435(11) -0.4711(14) 0.070(4) Uiso 0.35 d PD B 2 H452 H -0.4026 -0.7048 -0.4819 0.084 Uiso 0.35 calc PR B 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 0.0505(2) 0.0495(2) 0.0506(2) -0.0009(2) -0.00410(19) 0.0061(2) Fe1 0.0587(3) 0.0756(4) 0.0616(4) -0.0109(3) 0.0118(3) -0.0134(3) Fe2 0.0581(3) 0.0479(3) 0.0563(3) 0.0065(3) 0.0074(3) 0.0044(3) Cl1 0.0586(6) 0.1067(10) 0.0722(7) 0.0019(7) -0.0101(6) -0.0191(6) Cl2 0.0887(8) 0.0559(6) 0.0778(7) 0.0099(5) -0.0185(6) -0.0084(6) N1 0.060(2) 0.061(2) 0.060(2) -0.0035(17) -0.0012(18) 0.0114(17) N2 0.0581(19) 0.063(2) 0.057(2) 0.0042(17) -0.0019(16) 0.0184(17) C1 0.074(3) 0.082(3) 0.071(3) -0.006(2) 0.000(2) 0.030(3) C2 0.098(4) 0.081(3) 0.069(3) 0.003(2) 0.001(3) 0.044(3) C10 0.071(3) 0.065(3) 0.062(3) -0.011(2) 0.001(2) 0.010(2) C11 0.065(3) 0.064(3) 0.060(2) -0.010(2) 0.001(2) 0.002(2) C12 0.057(2) 0.072(3) 0.059(2) 0.002(2) 0.0040(19) 0.004(2) C13 0.057(2) 0.094(4) 0.067(3) 0.012(3) -0.001(2) -0.007(2) C14 0.079(3) 0.101(4) 0.056(3) 0.000(3) -0.002(3) -0.020(3) C15 0.080(3) 0.076(3) 0.060(3) -0.015(2) 0.005(2) -0.005(3) C20 0.060(2) 0.074(3) 0.055(2) 0.016(2) 0.001(2) 0.019(2) C21 0.052(2) 0.070(3) 0.052(2) 0.0057(18) -0.0016(17) 0.004(2) C22 0.058(2) 0.054(2) 0.055(2) 0.0067(19) 0.0002(19) 0.0036(18) C23 0.065(2) 0.052(2) 0.067(2) 0.001(2) 0.008(2) -0.0010(19) C24 0.075(3) 0.081(3) 0.054(2) -0.004(2) 0.002(2) -0.006(2) C25 0.071(3) 0.084(3) 0.050(2) 0.005(2) -0.010(2) 0.010(2) C31 0.090(6) 0.199(12) 0.151(9) -0.038(9) 0.048(6) -0.043(6) C32 0.156(9) 0.193(11) 0.084(5) 0.023(6) 0.007(5) -0.103(9) C33 0.089(5) 0.084(5) 0.364(19) 0.076(9) 0.010(9) -0.028(4) C34 0.158(9) 0.096(6) 0.133(7) -0.032(5) 0.036(7) -0.068(6) C35 0.102(6) 0.148(10) 0.214(14) 0.032(9) -0.034(8) -0.060(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 N2 2.063(3) . ? Zn1 N1 2.073(4) . ? Zn1 Cl2 2.2102(12) . ? Zn1 Cl1 2.2232(13) . ? N1 C10 1.281(6) . ? N1 C1 1.466(6) . ? N2 C20 1.270(6) . ? N2 C2 1.487(6) . ? C1 C2 1.506(7) . ? C10 C11 1.440(6) . ? C11 C12 1.435(7) . ? C11 C15 1.439(6) . ? C12 C13 1.415(6) . ? C13 C14 1.420(8) . ? C14 C15 1.406(8) . ? C20 C21 1.441(6) . ? C21 C22 1.438(6) . ? C21 C25 1.449(6) . ? C22 C23 1.408(6) . ? C23 C24 1.403(6) . ? C24 C25 1.397(7) . ? C31 C35 1.276(16) . ? C31 C32 1.304(16) . ? C33 C32 1.537(16) . ? C34 C33 1.440(16) . ? C34 C35 1.292(15) . ? C41 C45 1.399(13) . ? C41 C42 1.415(14) . ? C42 C43 1.432(12) . ? C43 C44 1.437(11) . ? C44 C45 1.420(13) . ? C412 C452 1.379(18) . ? C412 C422 1.397(18) . ? C422 C432 1.458(17) . ? C432 C442 1.412(18) . ? C442 C452 1.401(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Zn1 N1 84.26(14) . . ? N2 Zn1 Cl2 114.63(11) . . ? N1 Zn1 Cl2 111.55(11) . . ? N2 Zn1 Cl1 112.77(12) . . ? N1 Zn1 Cl1 116.29(11) . . ? Cl2 Zn1 Cl1 114.06(6) . . ? C10 N1 C1 117.6(4) . . ? C10 N1 Zn1 135.9(3) . . ? C1 N1 Zn1 106.6(3) . . ? C20 N2 C2 117.3(4) . . ? C20 N2 Zn1 135.5(3) . . ? C2 N2 Zn1 107.2(3) . . ? N1 C1 C2 109.1(4) . . ? N2 C2 C1 107.7(4) . . ? N1 C10 C11 127.1(4) . . ? C12 C11 C15 107.4(4) . . ? C12 C11 C10 129.8(4) . . ? C15 C11 C10 121.9(4) . . ? C13 C12 C11 108.3(4) . . ? C12 C13 C14 107.5(5) . . ? C15 C14 C13 109.6(4) . . ? C14 C15 C11 107.2(5) . . ? N2 C20 C21 126.6(4) . . ? C22 C21 C20 130.2(4) . . ? C22 C21 C25 106.7(4) . . ? C20 C21 C25 122.3(4) . . ? C23 C22 C21 107.7(4) . . ? C24 C23 C22 108.7(4) . . ? C25 C24 C23 109.3(4) . . ? C24 C25 C21 107.5(4) . . ? C31 C32 C33 104.7(9) . . ? C35 C31 C32 115.8(13) . . ? C32 C33 C34 98.3(8) . . ? C33 C34 C35 112.6(11) . . ? C31 C35 C34 108.5(12) . . ? C45 C41 C42 109.0(8) . . ? C41 C42 C43 107.8(8) . . ? C42 C43 C44 107.0(7) . . ? C45 C44 C43 107.8(7) . . ? C41 C45 C44 108.4(8) . . ? C452 C412 C422 111.4(13) . . ? C412 C422 C432 103.6(13) . . ? C442 C432 C422 109.7(13) . . ? C452 C442 C432 106.1(13) . . ? C412 C452 C442 108.9(13) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.301 _refine_diff_density_min -0.231 _refine_diff_density_rms 0.049 #=END data_ia009/PL4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1-(ferrocenylmethyl)-2-(ferrocenyl)benzimidazolium tetrafluoroborate ; _chemical_name_common ? _chemical_formula_moiety '[C28 H25 Fe2 N2] [B F4]' _chemical_formula_sum 'C28 H25 B F4 Fe2 N2' _chemical_formula_weight 588.01 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' 'B' 'B' 0.0013 0.0007 '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 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 10.966(2) _cell_length_b 15.935(3) _cell_length_c 14.829(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.45(3) _cell_angle_gamma 90.00 _cell_volume 2458.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 356 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'block' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.589 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 1.232 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.204 _exptl_absorpt_correction_T_max 0.672 _exptl_absorpt_process_details 'DIFABS: Walker, N & Stuart, D (1983), Acta Cryst. A39, 158' _exptl_special_details ; crystal mounted on glass fibre for data collection ; _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 'Stoe IPDS' _diffrn_measurement_method 'image plate' _diffrn_detector_area_resol_mean 0.70 _diffrn_standards_number 100 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8511 _diffrn_reflns_av_R_equivalents 0.0744 _diffrn_reflns_av_sigmaI/netI 0.0474 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.34 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3770 _reflns_number_gt 2971 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS 1.04' _computing_cell_refinement 'Stoe IPDS 1.04' _computing_data_reduction 'Stoe IPDS 1.04' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL (Sheldrick, 1987)' _computing_publication_material 'Siemens SHELXTL (Sheldrick, 1987)' _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. One Cp-ring is disordered: C(41)-C(45): 0.80 occupancy C(412)-C(452): 0.20 occupancy ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0957P)^2^+2.0595P] 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 3770 _refine_ls_number_parameters 346 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0777 _refine_ls_R_factor_gt 0.0614 _refine_ls_wR_factor_ref 0.1747 _refine_ls_wR_factor_gt 0.1643 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.066 _refine_ls_shift/su_mean 0.007 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.66140(7) 0.21420(4) 0.54736(5) 0.0564(3) Uani 1 d . . . Fe2 Fe 0.75506(7) 0.55817(4) 0.76324(5) 0.0610(3) Uani 1 d . . . N1 N 0.8656(4) 0.4408(2) 0.5565(3) 0.0570(10) Uani 1 d . . . N2 N 0.8376(5) 0.5761(3) 0.5422(3) 0.0631(10) Uani 1 d D . . C1 C 0.8674(5) 0.5122(3) 0.6064(4) 0.0548(11) Uani 1 d . . . C2 C 0.8171(5) 0.5465(3) 0.4521(4) 0.0603(12) Uani 1 d . . . C3 C 0.7848(6) 0.5864(3) 0.3638(4) 0.0711(14) Uani 1 d . . . H3 H 0.7736 0.6442 0.3582 0.085 Uiso 1 calc R . . C4 C 0.7702(6) 0.5361(4) 0.2853(4) 0.0740(15) Uani 1 d . . . H4 H 0.7501 0.5605 0.2255 0.089 Uiso 1 calc R . . C5 C 0.7850(7) 0.4503(3) 0.2942(5) 0.0801(17) Uani 1 d . . . H5 H 0.7728 0.4185 0.2395 0.096 Uiso 1 calc R . . C6 C 0.8170(5) 0.4099(3) 0.3802(4) 0.0671(13) Uani 1 d . . . H6 H 0.8272 0.3519 0.3849 0.080 Uiso 1 calc R . . C7 C 0.8335(5) 0.4600(3) 0.4603(4) 0.0583(12) Uani 1 d . . . C10 C 0.8890(5) 0.3547(3) 0.5969(4) 0.0571(11) Uani 1 d . . . H10A H 0.9552 0.3566 0.6584 0.068 Uiso 1 calc R . . H10B H 0.9193 0.3192 0.5553 0.068 Uiso 1 calc R . . C11 C 0.7678(5) 0.3180(3) 0.6079(4) 0.0563(11) Uani 1 d . . . C12 C 0.6400(5) 0.3407(3) 0.5576(4) 0.0662(12) Uani 1 d . . . C13 C 0.5556(6) 0.2957(3) 0.5980(5) 0.0775(16) Uani 1 d . . . C14 C 0.6335(6) 0.2455(3) 0.6728(4) 0.0709(14) Uani 1 d . . . C15 C 0.7648(5) 0.2591(3) 0.6799(4) 0.0627(12) Uani 1 d . . . C21 C 0.7389(6) 0.1574(3) 0.4543(5) 0.0761(15) Uani 1 d . . . C22 C 0.6115(7) 0.1847(4) 0.4066(4) 0.0843(17) Uani 1 d . . . C23 C 0.5292(6) 0.1438(4) 0.4476(5) 0.0818(16) Uani 1 d . . . C24 C 0.6055(6) 0.0921(3) 0.5222(5) 0.0763(15) Uani 1 d . . . C25 C 0.7357(6) 0.0997(3) 0.5263(4) 0.0753(15) Uani 1 d . . . C31 C 0.8939(5) 0.5243(3) 0.7064(4) 0.0590(11) Uani 1 d . . . C32 C 0.9219(5) 0.6052(3) 0.7520(4) 0.0658(13) Uani 1 d . . . C33 C 0.9330(6) 0.5950(3) 0.8486(4) 0.0723(14) Uani 1 d . . . C34 C 0.9114(5) 0.5080(3) 0.8645(4) 0.0685(13) Uani 1 d . . . C35 C 0.8888(5) 0.4640(3) 0.7799(4) 0.0619(12) Uani 1 d . . . C41 C 0.6129(11) 0.5564(8) 0.8260(8) 0.079(3) Uiso 0.65 d PD A 1 C42 C 0.6294(11) 0.6386(7) 0.7931(10) 0.078(3) Uiso 0.65 d PD A 1 C43 C 0.6102(12) 0.6372(8) 0.6948(11) 0.079(3) Uiso 0.65 d PD A 1 C44 C 0.5763(10) 0.5510(7) 0.6580(7) 0.076(2) Uiso 0.65 d PD A 1 C45 C 0.5784(10) 0.4992(5) 0.7419(10) 0.078(2) Uiso 0.65 d PD A 1 C412 C 0.5896(17) 0.5284(11) 0.7933(15) 0.065(4) Uiso 0.35 d PD A 2 C422 C 0.624(2) 0.6127(16) 0.8213(15) 0.091(7) Uiso 0.35 d PD A 2 C432 C 0.637(2) 0.6645(11) 0.748(2) 0.104(6) Uiso 0.35 d PD A 2 C442 C 0.595(2) 0.6123(14) 0.6631(14) 0.077(5) Uiso 0.35 d PD A 2 C452 C 0.566(2) 0.5269(12) 0.6895(16) 0.095(6) Uiso 0.35 d PD A 2 F1 F 0.7703(4) 0.7431(2) 0.5499(4) 0.1118(14) Uani 1 d . . . F2 F 0.8289(5) 0.8784(2) 0.5477(4) 0.1289(16) Uani 1 d . . . F3 F 0.8934(7) 0.8047(3) 0.6804(4) 0.164(3) Uani 1 d . . . F4 F 0.9704(6) 0.7735(4) 0.5687(7) 0.203(4) Uani 1 d . . . B1 B 0.8668(7) 0.8018(4) 0.5835(6) 0.0743(17) Uani 1 d . . . H2 H 0.824(6) 0.620(2) 0.557(5) 0.075(18) Uiso 1 d D . . H12 H 0.6019 0.3682 0.4947 0.10(2) Uiso 1 d . . . H14 H 0.6026 0.2125 0.7214 0.090(18) Uiso 1 d . . . H35 H 0.9018 0.3911 0.7832 0.13(2) Uiso 1 d . . . H23 H 0.4222 0.1614 0.4209 0.12(2) Uiso 1 d . . . H21 H 0.8224 0.1804 0.4570 0.091(19) Uiso 1 d . . . H22 H 0.5828 0.2254 0.3419 0.089(17) Uiso 1 d . . . H25 H 0.8215 0.0714 0.5806 0.083(17) Uiso 1 d . . . H24 H 0.5813 0.0470 0.5680 0.074(15) Uiso 1 d . . . H33 H 0.9581 0.6410 0.9122 0.10(2) Uiso 1 d . . . H22 H 0.9180 0.6642 0.7176 0.080(16) Uiso 1 d . . . H13 H 0.4625 0.2945 0.5678 0.067(14) Uiso 1 d . . . H34 H 0.9208 0.4857 0.9344 0.091(18) Uiso 1 d . . . H15 H 0.8626 0.2244 0.7287 0.068(14) Uiso 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0570(4) 0.0559(4) 0.0566(5) -0.0023(3) 0.0183(4) -0.0044(3) Fe2 0.0566(4) 0.0669(5) 0.0580(5) 0.0035(3) 0.0158(4) 0.0054(3) N1 0.059(2) 0.050(2) 0.066(3) -0.0002(17) 0.025(2) -0.0029(16) N2 0.079(3) 0.050(2) 0.062(3) -0.0011(19) 0.025(2) 0.001(2) C1 0.055(3) 0.052(2) 0.058(3) -0.0023(19) 0.019(2) -0.0039(19) C2 0.062(3) 0.055(3) 0.066(3) 0.001(2) 0.024(3) -0.004(2) C3 0.078(3) 0.066(3) 0.070(4) 0.012(2) 0.024(3) 0.001(3) C4 0.081(4) 0.085(4) 0.055(3) 0.006(3) 0.020(3) -0.002(3) C5 0.101(5) 0.080(4) 0.063(4) -0.009(3) 0.030(4) -0.006(3) C6 0.078(3) 0.060(3) 0.064(3) -0.005(2) 0.025(3) 0.000(2) C7 0.060(3) 0.058(3) 0.060(3) 0.003(2) 0.023(3) -0.001(2) C10 0.057(3) 0.048(2) 0.066(3) 0.002(2) 0.019(3) 0.0009(19) C11 0.058(3) 0.053(2) 0.057(3) -0.0006(19) 0.018(2) 0.001(2) C12 0.060(3) 0.064(3) 0.070(3) 0.002(2) 0.014(3) 0.003(2) C13 0.065(3) 0.072(3) 0.101(5) -0.017(3) 0.034(3) -0.010(3) C14 0.078(3) 0.073(3) 0.069(3) -0.013(3) 0.034(3) -0.014(3) C15 0.071(3) 0.061(3) 0.057(3) -0.004(2) 0.023(3) -0.013(2) C21 0.090(4) 0.069(3) 0.082(4) -0.015(3) 0.044(4) -0.010(3) C22 0.107(5) 0.086(4) 0.055(3) -0.010(3) 0.018(3) 0.008(3) C23 0.067(3) 0.091(4) 0.080(4) -0.028(3) 0.013(3) -0.007(3) C24 0.084(4) 0.069(3) 0.081(4) -0.017(3) 0.033(4) -0.021(3) C25 0.086(4) 0.065(3) 0.076(4) -0.012(3) 0.027(3) -0.006(3) C31 0.057(3) 0.058(3) 0.058(3) -0.001(2) 0.012(2) -0.002(2) C32 0.065(3) 0.062(3) 0.070(4) -0.011(2) 0.021(3) -0.008(2) C33 0.069(3) 0.073(3) 0.069(4) -0.014(3) 0.015(3) -0.006(3) C34 0.066(3) 0.074(3) 0.062(3) 0.005(2) 0.015(3) 0.011(2) C35 0.064(3) 0.062(3) 0.055(3) 0.007(2) 0.013(3) 0.011(2) F1 0.086(3) 0.067(2) 0.161(4) -0.009(2) 0.009(3) -0.0084(18) F2 0.176(4) 0.061(2) 0.119(4) 0.018(2) 0.004(3) -0.007(2) F3 0.278(8) 0.101(3) 0.094(4) 0.002(2) 0.033(4) -0.021(4) F4 0.128(5) 0.157(5) 0.366(12) 0.004(5) 0.138(7) 0.011(4) B1 0.079(4) 0.065(3) 0.076(5) 0.006(3) 0.020(4) -0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C13 2.037(5) . ? Fe1 C22 2.039(6) . ? Fe1 C24 2.038(5) . ? Fe1 C12 2.041(5) . ? Fe1 C14 2.040(5) . ? Fe1 C21 2.047(5) . ? Fe1 C23 2.047(6) . ? Fe1 C11 2.060(5) . ? Fe1 C25 2.061(5) . ? Fe1 C15 2.062(5) . ? Fe2 C43 2.029(11) . ? Fe2 C42 2.031(10) . ? Fe2 C31 2.032(5) . ? Fe2 C32 2.032(5) . ? Fe2 C33 2.047(6) . ? Fe2 C34 2.050(6) . ? Fe2 C41 2.053(9) . ? Fe2 C412 2.056(15) . ? Fe2 C35 2.058(5) . ? Fe2 C452 2.07(2) . ? Fe2 C422 2.081(19) . ? Fe2 C45 2.085(9) . ? N1 C1 1.355(6) . ? N1 C7 1.392(7) . ? N1 C10 1.485(5) . ? N2 C1 1.362(6) . ? N2 C2 1.367(7) . ? N2 H2 0.77(3) . ? C1 C31 1.432(7) . ? C2 C7 1.389(6) . ? C2 C3 1.396(8) . ? C3 C4 1.380(8) . ? C3 H3 0.9300 . ? C4 C5 1.378(8) . ? C4 H4 0.9300 . ? C5 C6 1.372(8) . ? C5 H5 0.9300 . ? C6 C7 1.394(7) . ? C6 H6 0.9300 . ? C10 C11 1.507(6) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.411(7) . ? C11 C15 1.430(7) . ? C12 C13 1.443(7) . ? C12 H12 0.995(6) . ? C13 C14 1.414(9) . ? C13 H13 0.977(6) . ? C14 C15 1.426(7) . ? C14 H14 1.032(5) . ? C15 H15 1.221(6) . ? C21 C25 1.418(8) . ? C21 C22 1.420(9) . ? C21 H21 0.975(6) . ? C22 C23 1.398(9) . ? C22 H22 1.118(6) . ? C23 C24 1.420(9) . ? C23 H23 1.148(6) . ? C24 C25 1.415(8) . ? C24 H24 1.079(6) . ? C25 H25 1.121(7) . ? C31 C32 1.442(7) . ? C31 C35 1.468(7) . ? C32 C33 1.408(8) . ? C32 H22 1.065(5) . ? C33 C34 1.439(7) . ? C33 H33 1.157(5) . ? C34 C35 1.390(8) . ? C34 H34 1.069(6) . ? C35 H35 1.169(5) . ? C41 C42 1.429(14) . ? C41 C45 1.493(14) . ? C42 C43 1.405(16) . ? C43 C44 1.481(16) . ? C44 C45 1.487(14) . ? C412 C422 1.422(19) . ? C412 C452 1.48(2) . ? C422 C432 1.40(2) . ? C432 C442 1.46(2) . ? C442 C452 1.48(2) . ? F1 B1 1.383(8) . ? F2 B1 1.343(8) . ? F3 B1 1.373(9) . ? F4 B1 1.304(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 Fe1 C22 121.7(3) . . ? C13 Fe1 C24 120.2(2) . . ? C22 Fe1 C24 67.9(3) . . ? C13 Fe1 C12 41.4(2) . . ? C22 Fe1 C12 107.7(2) . . ? C24 Fe1 C12 157.1(2) . . ? C13 Fe1 C14 40.6(2) . . ? C22 Fe1 C14 157.1(3) . . ? C24 Fe1 C14 106.1(2) . . ? C12 Fe1 C14 68.7(2) . . ? C13 Fe1 C21 159.6(3) . . ? C22 Fe1 C21 40.7(3) . . ? C24 Fe1 C21 67.6(2) . . ? C12 Fe1 C21 124.7(2) . . ? C14 Fe1 C21 159.5(3) . . ? C13 Fe1 C23 105.1(2) . . ? C22 Fe1 C23 40.0(3) . . ? C24 Fe1 C23 40.7(3) . . ? C12 Fe1 C23 121.5(2) . . ? C14 Fe1 C23 121.1(2) . . ? C21 Fe1 C23 67.7(2) . . ? C13 Fe1 C11 68.7(2) . . ? C22 Fe1 C11 124.3(2) . . ? C24 Fe1 C11 160.5(2) . . ? C12 Fe1 C11 40.2(2) . . ? C14 Fe1 C11 68.55(19) . . ? C21 Fe1 C11 110.5(2) . . ? C23 Fe1 C11 158.3(2) . . ? C13 Fe1 C25 156.7(2) . . ? C22 Fe1 C25 68.4(3) . . ? C24 Fe1 C25 40.4(2) . . ? C12 Fe1 C25 161.0(2) . . ? C14 Fe1 C25 122.3(2) . . ? C21 Fe1 C25 40.4(2) . . ? C23 Fe1 C25 68.2(2) . . ? C11 Fe1 C25 125.5(2) . . ? C13 Fe1 C15 68.4(2) . . ? C22 Fe1 C15 160.9(2) . . ? C24 Fe1 C15 123.3(2) . . ? C12 Fe1 C15 68.1(2) . . ? C14 Fe1 C15 40.7(2) . . ? C21 Fe1 C15 125.2(2) . . ? C23 Fe1 C15 158.3(2) . . ? C11 Fe1 C15 40.62(18) . . ? C25 Fe1 C15 109.1(2) . . ? C43 Fe2 C42 40.5(5) . . ? C43 Fe2 C31 121.9(4) . . ? C42 Fe2 C31 155.1(4) . . ? C43 Fe2 C32 108.3(3) . . ? C42 Fe2 C32 118.4(4) . . ? C31 Fe2 C32 41.55(19) . . ? C43 Fe2 C33 125.0(4) . . ? C42 Fe2 C33 105.3(3) . . ? C31 Fe2 C33 68.9(2) . . ? C32 Fe2 C33 40.4(2) . . ? C43 Fe2 C34 161.6(5) . . ? C42 Fe2 C34 123.6(4) . . ? C31 Fe2 C34 68.8(2) . . ? C32 Fe2 C34 68.8(2) . . ? C33 Fe2 C34 41.1(2) . . ? C43 Fe2 C41 69.4(4) . . ? C42 Fe2 C41 41.0(4) . . ? C31 Fe2 C41 163.8(4) . . ? C32 Fe2 C41 151.0(4) . . ? C33 Fe2 C41 115.8(4) . . ? C34 Fe2 C41 104.0(3) . . ? C43 Fe2 C412 69.3(5) . . ? C42 Fe2 C412 52.5(6) . . ? C31 Fe2 C412 149.0(6) . . ? C32 Fe2 C412 169.1(7) . . ? C33 Fe2 C412 131.8(6) . . ? C34 Fe2 C412 110.0(5) . . ? C41 Fe2 C412 18.2(5) . . ? C43 Fe2 C35 158.1(5) . . ? C42 Fe2 C35 160.2(5) . . ? C31 Fe2 C35 42.06(19) . . ? C32 Fe2 C35 69.7(2) . . ? C33 Fe2 C35 68.4(2) . . ? C34 Fe2 C35 39.5(2) . . ? C41 Fe2 C35 123.4(3) . . ? C412 Fe2 C35 116.8(5) . . ? C43 Fe2 C452 52.6(7) . . ? C42 Fe2 C452 68.5(6) . . ? C31 Fe2 C452 118.2(6) . . ? C32 Fe2 C452 145.1(7) . . ? C33 Fe2 C452 173.0(6) . . ? C34 Fe2 C452 139.2(7) . . ? C41 Fe2 C452 57.4(7) . . ? C412 Fe2 C452 41.9(6) . . ? C35 Fe2 C452 116.3(5) . . ? C43 Fe2 C422 54.2(7) . . ? C42 Fe2 C422 16.8(5) . . ? C31 Fe2 C422 170.6(8) . . ? C32 Fe2 C422 129.5(7) . . ? C33 Fe2 C422 105.7(6) . . ? C34 Fe2 C422 112.7(7) . . ? C41 Fe2 C422 25.5(6) . . ? C412 Fe2 C422 40.2(6) . . ? C35 Fe2 C422 144.4(8) . . ? C452 Fe2 C422 67.4(7) . . ? C43 Fe2 C45 70.2(4) . . ? C42 Fe2 C45 69.8(4) . . ? C31 Fe2 C45 126.9(3) . . ? C32 Fe2 C45 166.2(4) . . ? C33 Fe2 C45 151.8(4) . . ? C34 Fe2 C45 117.2(3) . . ? C41 Fe2 C45 42.3(4) . . ? C412 Fe2 C45 24.2(5) . . ? C35 Fe2 C45 106.4(3) . . ? C452 Fe2 C45 24.0(5) . . ? C422 Fe2 C45 61.5(6) . . ? C1 N1 C7 109.3(4) . . ? C1 N1 C10 125.8(5) . . ? C7 N1 C10 124.9(4) . . ? C1 N2 C2 110.7(4) . . ? C1 N2 H2 121(5) . . ? C2 N2 H2 128(5) . . ? N1 C1 N2 106.7(4) . . ? N1 C1 C31 130.0(4) . . ? N2 C1 C31 123.3(4) . . ? N2 C2 C7 106.3(4) . . ? N2 C2 C3 132.3(4) . . ? C7 C2 C3 121.4(5) . . ? C4 C3 C2 116.9(5) . . ? C4 C3 H3 121.5 . . ? C2 C3 H3 121.5 . . ? C5 C4 C3 121.1(5) . . ? C5 C4 H4 119.4 . . ? C3 C4 H4 119.4 . . ? C6 C5 C4 122.9(5) . . ? C6 C5 H5 118.6 . . ? C4 C5 H5 118.6 . . ? C5 C6 C7 116.6(5) . . ? C5 C6 H6 121.7 . . ? C7 C6 H6 121.7 . . ? C2 C7 N1 107.0(4) . . ? C2 C7 C6 121.0(5) . . ? N1 C7 C6 132.0(4) . . ? N1 C10 C11 110.9(4) . . ? N1 C10 H10A 109.5 . . ? C11 C10 H10A 109.5 . . ? N1 C10 H10B 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 108.1 . . ? C12 C11 C15 108.0(4) . . ? C12 C11 C10 127.3(4) . . ? C15 C11 C10 124.4(5) . . ? C12 C11 Fe1 69.2(3) . . ? C15 C11 Fe1 69.8(3) . . ? C10 C11 Fe1 131.5(3) . . ? C11 C12 C13 108.3(5) . . ? C11 C12 Fe1 70.6(3) . . ? C13 C12 Fe1 69.1(3) . . ? C11 C12 H12 131.4(5) . . ? C13 C12 H12 118.3(5) . . ? Fe1 C12 H12 112.9(4) . . ? C14 C13 C12 107.4(5) . . ? C14 C13 Fe1 69.8(3) . . ? C12 C13 Fe1 69.4(3) . . ? C14 C13 H13 129.2(5) . . ? C12 C13 H13 122.3(6) . . ? Fe1 C13 H13 116.9(4) . . ? C13 C14 C15 108.5(4) . . ? C13 C14 Fe1 69.6(3) . . ? C15 C14 Fe1 70.5(3) . . ? C13 C14 H14 125.8(5) . . ? C15 C14 H14 124.9(6) . . ? Fe1 C14 H14 133.6(4) . . ? C14 C15 C11 107.9(5) . . ? C14 C15 Fe1 68.9(3) . . ? C11 C15 Fe1 69.6(3) . . ? C14 C15 H15 130.7(4) . . ? C11 C15 H15 121.1(4) . . ? Fe1 C15 H15 121.5(3) . . ? C25 C21 C22 108.6(5) . . ? C25 C21 Fe1 70.4(3) . . ? C22 C21 Fe1 69.4(3) . . ? C25 C21 H21 117.4(7) . . ? C22 C21 H21 131.9(6) . . ? Fe1 C21 H21 113.0(4) . . ? C23 C22 C21 108.0(6) . . ? C23 C22 Fe1 70.3(3) . . ? C21 C22 Fe1 70.0(4) . . ? C23 C22 H22 126.8(7) . . ? C21 C22 H22 124.8(6) . . ? Fe1 C22 H22 131.0(4) . . ? C22 C23 C24 107.9(5) . . ? C22 C23 Fe1 69.7(3) . . ? C24 C23 Fe1 69.3(3) . . ? C22 C23 H23 117.8(6) . . ? C24 C23 H23 134.1(6) . . ? Fe1 C23 H23 121.9(4) . . ? C25 C24 C23 108.8(5) . . ? C25 C24 Fe1 70.7(3) . . ? C23 C24 Fe1 70.0(3) . . ? C25 C24 H24 118.4(6) . . ? C23 C24 H24 132.5(6) . . ? Fe1 C24 H24 129.8(4) . . ? C24 C25 C21 106.7(6) . . ? C24 C25 Fe1 68.9(3) . . ? C21 C25 Fe1 69.3(3) . . ? C24 C25 H25 127.1(5) . . ? C21 C25 H25 125.9(5) . . ? Fe1 C25 H25 122.0(4) . . ? C1 C31 C32 123.4(5) . . ? C1 C31 C35 129.6(4) . . ? C32 C31 C35 106.9(5) . . ? C1 C31 Fe2 122.2(4) . . ? C32 C31 Fe2 69.2(3) . . ? C35 C31 Fe2 69.9(3) . . ? C33 C32 C31 108.1(4) . . ? C33 C32 Fe2 70.4(3) . . ? C31 C32 Fe2 69.2(3) . . ? C33 C32 H22 124.5(5) . . ? C31 C32 H22 126.5(5) . . ? Fe2 C32 H22 117.6(4) . . ? C32 C33 C34 108.2(4) . . ? C32 C33 Fe2 69.2(3) . . ? C34 C33 Fe2 69.5(3) . . ? C32 C33 H33 132.7(5) . . ? C34 C33 H33 119.0(5) . . ? Fe2 C33 H33 128.3(4) . . ? C35 C34 C33 109.3(4) . . ? C35 C34 Fe2 70.5(3) . . ? C33 C34 Fe2 69.4(3) . . ? C35 C34 H34 129.9(5) . . ? C33 C34 H34 120.6(5) . . ? Fe2 C34 H34 129.9(4) . . ? C34 C35 C31 107.5(4) . . ? C34 C35 Fe2 69.9(3) . . ? C31 C35 Fe2 68.0(3) . . ? C34 C35 H35 118.7(4) . . ? C31 C35 H35 130.5(4) . . ? Fe2 C35 H35 143.3(4) . . ? C42 C41 C45 107.5(8) . . ? C42 C41 Fe2 68.7(5) . . ? C45 C41 Fe2 70.0(5) . . ? C43 C42 C41 110.2(10) . . ? C43 C42 Fe2 69.7(6) . . ? C41 C42 Fe2 70.4(5) . . ? C42 C43 C44 109.6(9) . . ? C42 C43 Fe2 69.8(6) . . ? C44 C43 Fe2 71.0(6) . . ? C43 C44 C45 105.6(9) . . ? C43 C44 Fe2 66.8(7) . . ? C45 C44 Fe2 69.0(6) . . ? C44 C45 C41 107.1(7) . . ? C44 C45 Fe2 69.2(5) . . ? C41 C45 Fe2 67.7(5) . . ? C422 C412 C452 105.2(13) . . ? C422 C412 Fe2 70.9(10) . . ? C452 C412 Fe2 69.6(10) . . ? C432 C422 C412 114.5(15) . . ? C432 C422 Fe2 71.3(12) . . ? C412 C422 Fe2 69.0(9) . . ? C422 C432 C442 104.6(14) . . ? C422 C432 Fe2 69.6(11) . . ? C442 C432 Fe2 69.2(11) . . ? C432 C442 C452 109.2(14) . . ? C432 C442 Fe2 70.0(11) . . ? C452 C442 Fe2 68.6(11) . . ? C442 C452 C412 106.2(13) . . ? C442 C452 Fe2 69.9(11) . . ? C412 C452 Fe2 68.4(10) . . ? F4 B1 F2 115.2(6) . . ? F4 B1 F3 106.3(8) . . ? F2 B1 F3 108.7(6) . . ? F4 B1 F1 108.2(6) . . ? F2 B1 F1 111.5(7) . . ? F3 B1 F1 106.6(5) . . ? _diffrn_measured_fraction_theta_max 0.839 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.839 _refine_diff_density_max 0.417 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.065 #=END data_mh9807/PL6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis-[1,2-Bis-[ferrocen-1-ylcarbaldimino]-4-methylbenzene]copper(I) hexafluorophosphate dichloromethane solvate ; _chemical_name_common ? _chemical_formula_moiety '[C58 H52 Cu Fe4 N4] [F6 P] 1.7[C H2 Cl2]' _chemical_formula_sum 'C59.7 H55.4 Cl3.4 Cu F6 Fe4 N4 P' _chemical_formula_weight 1381.32 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 17.091(5) _cell_length_b 20.019(5) _cell_length_c 17.797(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.67(4) _cell_angle_gamma 90.00 _cell_volume 6059(3) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 491 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.510 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2789 _exptl_absorpt_coefficient_mu 1.518 _exptl_absorpt_correction_type None _exptl_special_details ; No. of orientations: 2 \f range per orientation: 180 deg \D\f per frame: 5 deg Exposure per frame: 30 mins R(int): 0.096 (orientation 1), 0.090 (orientation 2) Mosaic spread: 0.886 deg (orientation 1), 0.852 (orientation 2) Sample-to-plate distance 80 mm ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS IIc' _diffrn_measurement_method 'Image plate' _diffrn_detector_area_resol_mean 'Low resolution (950x950 pixels)' _diffrn_standards_number None _diffrn_reflns_number 12736 _diffrn_reflns_av_R_equivalents 0.1118 _diffrn_reflns_av_sigmaI/netI 0.2205 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.51 _diffrn_reflns_theta_max 22.50 _reflns_number_total 7409 _reflns_number_gt 3663 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rigaku control software' _computing_cell_refinement 'Rigaku control software' _computing_data_reduction 'TEXSAN (Molecular Structure Corporation, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL (Sheldrick, 1987)' _computing_publication_material 'Siemens SHELXTL (Sheldrick, 1987)' _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. Solvent disorder sites and occupancies: CL1-C1S-CL2: 0.2 CL3 C1S-CL4: 0.2 CL5-C2S-CL6: 0.4 CL7-C2S-CL8: 0.1 CL9-C3S-CL10: 0.2 CL11-C4S-CL12: 0.2 CL13-C4S-CL14: 0.1 CL3-C5S-CL10: 0.2 CL15-CL9-CL16: 0.1 (CL9 assigned an additional occupancy of 0.05 to allow for 0.1C on this site) ; _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^)+(0.0078P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7409 _refine_ls_number_parameters 754 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1492 _refine_ls_R_factor_gt 0.0754 _refine_ls_wR_factor_ref 0.1671 _refine_ls_wR_factor_gt 0.1388 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.947 _refine_ls_shift/su_max 0.065 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.31897(7) -0.60296(7) 1.26320(7) 0.0352(4) Uani 1 1 d . . . Fe1 Fe 0.55519(9) -0.63189(8) 1.14349(9) 0.0408(5) Uani 1 1 d . . . Fe2 Fe 0.06488(9) -0.58677(9) 1.38990(9) 0.0463(5) Uani 1 1 d . . . Fe3 Fe 0.33694(9) -0.81215(8) 1.37737(9) 0.0461(5) Uani 1 1 d . . . Fe4 Fe 0.25460(10) -0.36798(9) 1.18219(10) 0.0541(5) Uani 1 1 d . . . N1A N 0.4327(4) -0.5732(4) 1.2986(4) 0.029(2) Uani 1 1 d . . . N2A N 0.3006(5) -0.5739(4) 1.3705(5) 0.035(2) Uani 1 1 d . . . C1A C 0.4409(6) -0.5747(5) 1.3791(6) 0.032(3) Uani 1 1 d . . . C2A C 0.3732(6) -0.5758(5) 1.4168(5) 0.029(2) Uani 1 1 d . . . C3A C 0.3783(7) -0.5846(5) 1.4934(6) 0.044(3) Uani 1 1 d . . . H3A H 0.3314 -0.5864 1.5178 0.052 Uiso 1 1 calc R . . C4A C 0.4500(7) -0.5910(5) 1.5366(6) 0.044(3) Uani 1 1 d . . . C5A C 0.5182(6) -0.5880(5) 1.4997(6) 0.041(3) Uani 1 1 d . . . C6A C 0.5131(7) -0.5819(5) 1.4219(6) 0.046(3) Uani 1 1 d . . . H6A H 0.5599 -0.5825 1.3972 0.056 Uiso 1 1 calc R . . C7A C 0.4536(11) -0.6039(10) 1.6196(10) 0.032(5) Uiso 0.50 1 d P . . H7A1 H 0.4116 -0.5790 1.6409 0.048 Uiso 0.50 1 calc PR . . H7A2 H 0.5048 -0.5893 1.6439 0.048 Uiso 0.50 1 calc PR . . H7A3 H 0.4469 -0.6518 1.6284 0.048 Uiso 0.50 1 calc PR . . C8A C 0.5950(14) -0.5987(13) 1.5492(13) 0.065(7) Uiso 0.50 1 d P . . H8A1 H 0.6269 -0.6320 1.5257 0.097 Uiso 0.50 1 calc PR . . H8A2 H 0.5836 -0.6145 1.5991 0.097 Uiso 0.50 1 calc PR . . H8A3 H 0.6239 -0.5564 1.5546 0.097 Uiso 0.50 1 calc PR . . C10 C 0.4902(5) -0.5501(5) 1.2621(6) 0.031(2) Uani 1 1 d . . . H10 H 0.5324 -0.5284 1.2910 0.037 Uiso 1 1 calc R . . C11 C 0.4945(6) -0.5548(5) 1.1838(6) 0.032(3) Uani 1 1 d . . . C12 C 0.4461(6) -0.5912(6) 1.1291(5) 0.044(3) Uani 1 1 d . . . H12 H 0.3985 -0.6134 1.1371 0.053 Uiso 1 1 calc R . . C13 C 0.4810(7) -0.5889(6) 1.0608(6) 0.048(3) Uani 1 1 d . . . H13 H 0.4611 -0.6087 1.0143 0.058 Uiso 1 1 calc R . . C14 C 0.5520(7) -0.5511(6) 1.0744(7) 0.056(3) Uani 1 1 d . . . H14 H 0.5878 -0.5416 1.0383 0.067 Uiso 1 1 calc R . . C15 C 0.5596(6) -0.5307(5) 1.1501(6) 0.044(3) Uani 1 1 d . . . H15 H 0.6016 -0.5050 1.1743 0.053 Uiso 1 1 calc R . . C20 C 0.2403(6) -0.5446(5) 1.3974(6) 0.040(3) Uani 1 1 d . . . H20 H 0.2489 -0.5239 1.4456 0.048 Uiso 1 1 calc R . . C21 C 0.1615(6) -0.5417(6) 1.3585(6) 0.048(3) Uani 1 1 d . . . C22 C 0.1283(7) -0.5855(8) 1.2989(6) 0.066(4) Uani 1 1 d . . . H22 H 0.1538 -0.6223 1.2782 0.079 Uiso 1 1 calc R . . C23 C 0.0499(7) -0.5629(9) 1.2771(7) 0.079(5) Uani 1 1 d . . . H23 H 0.0142 -0.5825 1.2390 0.095 Uiso 1 1 calc R . . C24 C 0.0340(7) -0.5068(7) 1.3212(8) 0.067(4) Uani 1 1 d . . . H24 H -0.0138 -0.4823 1.3177 0.081 Uiso 1 1 calc R . . C25 C 0.1012(7) -0.4932(6) 1.3714(7) 0.057(3) Uani 1 1 d . . . H25 H 0.1061 -0.4581 1.4076 0.068 Uiso 1 1 calc R . . N1B N 0.2817(5) -0.6900(4) 1.2133(4) 0.033(2) Uani 1 1 d . . . N2B N 0.2585(5) -0.5637(4) 1.1688(5) 0.036(2) Uani 1 1 d . . . C1B C 0.2190(6) -0.6763(6) 1.1576(6) 0.043(3) Uani 1 1 d . . . C2B C 0.2062(6) -0.6111(6) 1.1343(5) 0.039(3) Uani 1 1 d . . . C3B C 0.1441(7) -0.5946(7) 1.0824(7) 0.065(4) Uani 1 1 d . . . H3B H 0.1370 -0.5494 1.0667 0.078 Uiso 1 1 calc R . . C4B C 0.0926(9) -0.6421(9) 1.0532(8) 0.091(5) Uani 1 1 d . . . C5B C 0.1004(10) -0.7086(9) 1.0770(10) 0.108(6) Uani 1 1 d . . . H5B H 0.0640 -0.7418 1.0578 0.129 Uiso 1 1 calc R . . C6B C 0.1635(7) -0.7247(7) 1.1302(8) 0.080(5) Uani 1 1 d . . . H6B H 0.1691 -0.7692 1.1482 0.096 Uiso 1 1 calc R . . C7B C 0.0240(10) -0.6267(10) 0.9934(10) 0.149(9) Uani 1 1 d . . . H7B1 H 0.0367 -0.6427 0.9441 0.223 Uiso 1 1 calc R . . H7B2 H 0.0150 -0.5784 0.9911 0.223 Uiso 1 1 calc R . . H7B3 H -0.0236 -0.6492 1.0070 0.223 Uiso 1 1 calc R . . C30 C 0.3067(6) -0.7513(6) 1.2222(6) 0.040(3) Uani 1 1 d . . . H30 H 0.2830 -0.7834 1.1878 0.048 Uiso 1 1 calc R . . C31 C 0.3667(6) -0.7761(5) 1.2788(6) 0.037(3) Uani 1 1 d . . . C32 C 0.4075(7) -0.7395(6) 1.3413(6) 0.043(3) Uani 1 1 d . . . H32 H 0.4036 -0.6929 1.3503 0.052 Uiso 1 1 calc R . . C33 C 0.4542(6) -0.7855(6) 1.3863(7) 0.049(3) Uani 1 1 d . . . H33 H 0.4875 -0.7756 1.4309 0.059 Uiso 1 1 calc R . . C34 C 0.4417(6) -0.8504(5) 1.3515(7) 0.043(3) Uani 1 1 d . . . H34 H 0.4651 -0.8908 1.3705 0.051 Uiso 1 1 calc R . . C35 C 0.3899(7) -0.8447(6) 1.2858(6) 0.045(3) Uani 1 1 d . . . H35 H 0.3733 -0.8799 1.2522 0.054 Uiso 1 1 calc R . . C40 C 0.2715(6) -0.5117(6) 1.1307(7) 0.050(3) Uani 1 1 d . . . H40 H 0.2519 -0.5115 1.0788 0.060 Uiso 1 1 calc R . . C41 C 0.3129(7) -0.4537(6) 1.1591(8) 0.057(3) Uani 1 1 d . . . C42 C 0.3294(7) -0.4345(6) 1.2365(9) 0.069(4) Uani 1 1 d . . . H42 H 0.3189 -0.4622 1.2777 0.083 Uiso 1 1 calc R . . C43 C 0.3633(8) -0.3693(7) 1.2456(9) 0.078(5) Uani 1 1 d . . . H43 H 0.3790 -0.3466 1.2915 0.094 Uiso 1 1 calc R . . C44 C 0.3684(7) -0.3461(8) 1.1701(10) 0.080(5) Uani 1 1 d . . . H44 H 0.3882 -0.3037 1.1571 0.096 Uiso 1 1 calc R . . C45 C 0.3393(7) -0.3956(7) 1.1177(9) 0.070(4) Uani 1 1 d . . . H45 H 0.3372 -0.3919 1.0643 0.084 Uiso 1 1 calc R . . C51 C 0.5913(9) -0.6913(7) 1.2322(8) 0.068(4) Uani 1 1 d . . . H51 H 0.5826 -0.6830 1.2832 0.081 Uiso 1 1 calc R . . C52 C 0.5399(8) -0.7269(6) 1.1829(9) 0.069(4) Uani 1 1 d . . . H52 H 0.4916 -0.7468 1.1929 0.083 Uiso 1 1 calc R . . C53 C 0.5753(9) -0.7275(6) 1.1131(7) 0.067(4) Uani 1 1 d . . . H53 H 0.5543 -0.7483 1.0675 0.080 Uiso 1 1 calc R . . C54 C 0.6474(8) -0.6916(7) 1.1242(10) 0.080(5) Uani 1 1 d . . . H54 H 0.6833 -0.6839 1.0876 0.096 Uiso 1 1 calc R . . C55 C 0.6554(9) -0.6693(7) 1.2007(10) 0.076(4) Uani 1 1 d . . . H55 H 0.6976 -0.6438 1.2249 0.091 Uiso 1 1 calc R . . C61 C 0.0621(8) -0.6829(7) 1.4294(8) 0.069(4) Uani 1 1 d . . . H61 H 0.0868 -0.7205 1.4093 0.083 Uiso 1 1 calc R . . C63 C -0.0281(7) -0.6013(7) 1.4507(7) 0.058(4) Uani 1 1 d . . . H63 H -0.0742 -0.5746 1.4477 0.070 Uiso 1 1 calc R . . C62 C -0.0179(8) -0.6585(7) 1.4060(8) 0.072(4) Uani 1 1 d . . . H62 H -0.0549 -0.6773 1.3686 0.086 Uiso 1 1 calc R . . C64 C 0.0392(7) -0.5899(6) 1.4995(6) 0.050(3) Uani 1 1 d . . . H64 H 0.0466 -0.5545 1.5350 0.060 Uiso 1 1 calc R . . C65 C 0.0953(7) -0.6404(7) 1.4870(7) 0.059(4) Uani 1 1 d . . . H65 H 0.1463 -0.6446 1.5131 0.070 Uiso 1 1 calc R . . C71 C 0.2584(10) -0.7646(9) 1.4358(11) 0.095(6) Uani 1 1 d . . . H71 H 0.2549 -0.7178 1.4433 0.113 Uiso 1 1 calc R . . C72 C 0.3047(10) -0.8101(11) 1.4850(10) 0.091(5) Uani 1 1 d . . . H72 H 0.3380 -0.7989 1.5292 0.109 Uiso 1 1 calc R . . C73 C 0.2908(8) -0.8735(11) 1.4547(9) 0.088(6) Uani 1 1 d . . . H73 H 0.3124 -0.9138 1.4759 0.105 Uiso 1 1 calc R . . C74 C 0.2393(10) -0.8689(9) 1.3871(11) 0.094(5) Uani 1 1 d . . . H74 H 0.2211 -0.9048 1.3551 0.113 Uiso 1 1 calc R . . C75 C 0.2201(8) -0.7993(11) 1.3765(10) 0.092(6) Uani 1 1 d . . . H75 H 0.1870 -0.7807 1.3358 0.110 Uiso 1 1 calc R . . C81 C 0.1372(8) -0.3835(8) 1.1485(13) 0.094(6) Uani 1 1 d . . . H81 H 0.1144 -0.4210 1.1220 0.112 Uiso 1 1 calc R . . C82 C 0.1524(11) -0.3753(11) 1.2301(12) 0.104(6) Uani 1 1 d . . . H82 H 0.1412 -0.4071 1.2671 0.125 Uiso 1 1 calc R . . C83 C 0.1874(12) -0.3104(13) 1.2447(10) 0.115(8) Uani 1 1 d . . . H83 H 0.2033 -0.2924 1.2931 0.138 Uiso 1 1 calc R . . C84 C 0.1936(8) -0.2798(8) 1.1784(15) 0.100(6) Uani 1 1 d . . . H84 H 0.2143 -0.2364 1.1719 0.120 Uiso 1 1 calc R . . C85 C 0.1631(8) -0.3251(10) 1.1181(10) 0.093(5) Uani 1 1 d . . . H85 H 0.1613 -0.3156 1.0656 0.111 Uiso 1 1 calc R . . P1 P 0.23423(18) -0.50720(19) 1.66083(17) 0.0551(10) Uani 1 1 d . . . F1 F 0.1517(4) -0.5338(5) 1.6827(5) 0.120(3) Uani 1 1 d . . . F2 F 0.2065(6) -0.4339(4) 1.6765(4) 0.107(3) Uani 1 1 d . . . F3 F 0.3162(5) -0.4830(5) 1.6386(5) 0.121(3) Uani 1 1 d . . . F4 F 0.2682(5) -0.5141(4) 1.7466(4) 0.099(3) Uani 1 1 d . . . F5 F 0.2592(5) -0.5830(4) 1.6449(4) 0.094(3) Uani 1 1 d . . . F6 F 0.2011(5) -0.5002(4) 1.5749(4) 0.094(3) Uani 1 1 d . . . C1S C 0.1409(18) -0.0668(10) 1.3543(13) 0.061(11) Uiso 0.40 1 d PD . . C2S C 0.7496(12) -0.6484(11) 1.4865(10) 0.079(9) Uiso 0.50 1 d PD . . C3S C -0.014(2) -0.3308(14) 1.3103(17) 0.019(11) Uiso 0.20 1 d PD . . C4S C 0.1589(14) -0.0183(15) 1.4182(17) 0.051(10) Uiso 0.30 1 d PD . . C5S C 0.094(2) -0.2257(13) 1.389(2) 0.026(12) Uiso 0.20 1 d PD . . Cl1 Cl 0.2091(10) -0.0528(9) 1.4302(8) 0.045(5) Uiso 0.20 1 d PD . . Cl2 Cl 0.1810(10) -0.0616(10) 1.4439(8) 0.033(4) Uiso 0.20 1 d PD . . Cl3 Cl 0.1258(9) -0.1528(6) 1.3529(8) 0.125(5) Uiso 0.40 1 d PD . . Cl4 Cl 0.1318(10) -0.1463(7) 1.3186(10) 0.054(5) Uiso 0.20 1 d PD . . Cl5 Cl 0.6790(5) -0.7019(4) 1.4455(5) 0.039(3) Uiso 0.40 1 d PD . . Cl6 Cl 0.7405(5) -0.6319(4) 1.5818(4) 0.065(2) Uiso 0.40 1 d PD . . Cl7 Cl 0.8118(14) -0.6851(13) 1.5523(13) 0.042(7) Uiso 0.10 1 d PD . . Cl8 Cl 0.6946(16) -0.7164(13) 1.4588(16) 0.022(8) Uiso 0.10 1 d PD . . Cl9 Cl -0.0133(11) -0.2604(9) 1.2591(10) 0.112(6) Uiso 0.25 1 d PD . . Cl10 Cl 0.0511(12) -0.2992(10) 1.3802(12) 0.225(8) Uiso 0.40 1 d PD . . Cl11 Cl 0.0719(12) 0.0020(15) 1.3762(16) 0.082(11) Uiso 0.20 1 d PD . . Cl12 Cl 0.2022(11) -0.0867(9) 1.4460(9) 0.053(5) Uiso 0.20 1 d PD . . Cl13 Cl 0.0670(19) 0.012(3) 1.391(3) 0.08(2) Uiso 0.10 1 d PD . . Cl14 Cl 0.171(3) -0.062(2) 1.340(2) 0.093(15) Uiso 0.10 1 d PD . . Cl15 Cl -0.051(2) -0.3368(13) 1.260(2) 0.074(10) Uiso 0.10 1 d PD . . Cl16 Cl 0.052(2) -0.224(2) 1.325(2) 0.118(15) Uiso 0.10 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0347(7) 0.0379(8) 0.0318(7) -0.0056(6) -0.0033(6) -0.0015(6) Fe1 0.0421(10) 0.0358(10) 0.0456(10) 0.0002(8) 0.0095(8) 0.0054(8) Fe2 0.0302(9) 0.0584(12) 0.0517(10) 0.0025(9) 0.0104(8) 0.0013(8) Fe3 0.0431(10) 0.0486(11) 0.0483(10) 0.0071(9) 0.0136(8) 0.0076(9) Fe4 0.0431(10) 0.0484(11) 0.0703(12) 0.0121(10) 0.0037(9) 0.0054(9) N1A 0.033(5) 0.029(5) 0.023(5) -0.009(4) -0.012(4) 0.005(4) N2A 0.034(5) 0.030(5) 0.042(5) -0.001(4) 0.006(4) -0.003(4) C1A 0.031(6) 0.025(6) 0.040(7) -0.004(5) 0.001(6) 0.000(5) C2A 0.038(6) 0.030(6) 0.016(5) 0.001(5) -0.014(5) -0.002(5) C3A 0.050(7) 0.046(8) 0.035(7) 0.006(6) -0.003(6) -0.009(6) C4A 0.054(8) 0.030(7) 0.046(7) -0.007(6) -0.006(6) -0.002(6) C5A 0.033(6) 0.038(7) 0.051(7) -0.006(6) 0.001(6) 0.004(5) C6A 0.062(8) 0.030(7) 0.048(8) 0.005(6) 0.007(6) 0.006(6) C10 0.024(6) 0.032(6) 0.036(7) -0.006(5) 0.001(5) -0.002(5) C11 0.038(6) 0.024(6) 0.033(6) -0.011(5) 0.000(5) -0.001(5) C12 0.053(7) 0.054(8) 0.027(6) -0.001(6) 0.008(6) -0.006(6) C13 0.055(8) 0.043(8) 0.045(7) -0.006(6) -0.001(6) 0.002(6) C14 0.067(9) 0.047(8) 0.055(8) 0.001(7) 0.015(7) 0.012(7) C15 0.043(7) 0.039(7) 0.054(8) 0.000(6) 0.015(6) -0.002(6) C20 0.036(7) 0.045(7) 0.040(7) -0.007(6) 0.001(6) -0.002(6) C21 0.042(7) 0.060(9) 0.039(7) 0.004(6) -0.005(6) -0.005(6) C22 0.034(7) 0.119(13) 0.046(8) 0.005(8) 0.013(6) -0.004(8) C23 0.039(8) 0.150(16) 0.045(8) 0.020(9) -0.009(7) 0.006(9) C24 0.027(7) 0.082(11) 0.093(11) 0.030(9) 0.003(8) 0.023(7) C25 0.052(8) 0.046(8) 0.072(9) 0.020(7) 0.001(7) 0.004(7) N1B 0.026(5) 0.039(6) 0.032(5) -0.001(4) 0.003(4) -0.001(4) N2B 0.038(5) 0.028(6) 0.042(6) 0.003(5) 0.005(5) 0.002(4) C1B 0.034(7) 0.067(9) 0.028(6) -0.018(6) 0.002(6) 0.009(7) C2B 0.035(7) 0.057(9) 0.023(6) -0.009(6) -0.006(5) 0.010(6) C3B 0.057(8) 0.079(10) 0.056(8) -0.020(8) -0.016(7) 0.009(8) C4B 0.075(10) 0.108(14) 0.078(11) -0.051(11) -0.055(9) 0.024(10) C5B 0.100(13) 0.075(12) 0.135(15) -0.060(11) -0.056(11) 0.017(10) C6B 0.061(9) 0.061(10) 0.106(12) -0.038(9) -0.050(9) -0.008(8) C7B 0.118(16) 0.18(2) 0.132(15) -0.060(15) -0.095(13) 0.043(14) C30 0.040(7) 0.046(8) 0.036(7) -0.005(6) 0.011(6) -0.008(6) C31 0.046(7) 0.037(7) 0.028(6) 0.000(6) 0.005(5) -0.002(6) C32 0.066(8) 0.029(7) 0.035(7) 0.002(5) 0.008(6) 0.005(6) C33 0.043(7) 0.043(8) 0.060(8) 0.012(7) -0.009(6) -0.003(6) C34 0.034(6) 0.030(7) 0.067(8) 0.011(6) 0.023(6) 0.003(5) C35 0.058(8) 0.040(8) 0.037(7) -0.007(6) -0.004(6) -0.001(6) C40 0.047(8) 0.046(9) 0.052(8) -0.009(7) -0.012(6) 0.012(7) C41 0.064(8) 0.039(8) 0.066(10) 0.025(7) -0.001(7) 0.010(7) C42 0.063(9) 0.049(9) 0.093(12) 0.026(8) -0.007(8) -0.008(7) C43 0.082(11) 0.043(9) 0.100(13) 0.017(9) -0.044(9) 0.007(8) C44 0.036(8) 0.083(12) 0.119(14) 0.010(11) -0.002(9) -0.014(8) C45 0.032(7) 0.078(11) 0.104(11) 0.039(10) 0.032(8) 0.023(7) C51 0.078(11) 0.057(10) 0.068(10) 0.006(8) 0.005(9) 0.035(8) C52 0.061(9) 0.046(9) 0.099(12) 0.008(8) 0.004(9) 0.008(7) C53 0.097(11) 0.047(9) 0.054(9) -0.025(7) -0.009(8) 0.025(8) C54 0.061(10) 0.047(9) 0.140(15) 0.000(10) 0.050(10) 0.001(8) C55 0.054(10) 0.059(10) 0.110(13) -0.007(9) -0.010(10) 0.018(8) C61 0.065(10) 0.047(9) 0.100(11) 0.007(9) 0.031(9) -0.004(8) C63 0.034(7) 0.065(10) 0.079(9) 0.000(8) 0.027(7) 0.003(7) C62 0.046(8) 0.084(11) 0.089(11) -0.018(9) 0.024(8) -0.029(8) C64 0.058(8) 0.039(7) 0.052(8) -0.003(6) 0.004(7) 0.001(7) C65 0.046(8) 0.054(9) 0.077(10) 0.030(8) 0.008(7) 0.004(7) C71 0.086(12) 0.121(15) 0.087(12) 0.009(13) 0.058(11) 0.041(13) C72 0.071(12) 0.125(16) 0.084(12) 0.008(13) 0.046(10) 0.003(12) C73 0.039(8) 0.153(19) 0.073(11) 0.062(12) 0.013(8) 0.002(10) C74 0.071(11) 0.073(12) 0.142(17) 0.010(12) 0.030(12) -0.020(10) C75 0.039(9) 0.16(2) 0.080(12) -0.003(13) 0.012(8) 0.012(10) C81 0.040(8) 0.065(12) 0.17(2) 0.011(13) -0.006(10) -0.007(8) C82 0.101(14) 0.108(17) 0.113(16) 0.039(14) 0.064(13) 0.010(12) C83 0.137(19) 0.14(2) 0.076(13) 0.010(14) 0.029(12) 0.063(16) C84 0.044(9) 0.050(11) 0.20(2) -0.030(14) -0.019(12) 0.016(8) C85 0.046(9) 0.120(16) 0.111(14) 0.024(13) -0.001(9) 0.043(10) P1 0.0405(19) 0.083(3) 0.041(2) 0.0072(19) -0.0012(16) 0.0118(19) F1 0.052(5) 0.194(10) 0.120(7) -0.007(7) 0.037(5) -0.015(6) F2 0.162(9) 0.089(7) 0.069(5) -0.021(5) -0.005(5) 0.051(6) F3 0.066(5) 0.154(9) 0.144(8) 0.003(7) 0.023(6) -0.041(6) F4 0.110(7) 0.116(7) 0.065(5) 0.009(5) -0.026(4) 0.029(6) F5 0.115(7) 0.070(6) 0.101(6) -0.001(5) 0.026(5) 0.028(5) F6 0.124(7) 0.116(7) 0.039(4) -0.003(4) -0.015(4) 0.029(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 Cu1 N1B 2.030(9) . ? Cu1 N2B 2.041(9) . ? Cu1 N2A 2.050(8) . ? Cu1 N1A 2.071(8) . ? Fe1 C51 2.023(13) . ? Fe1 C12 2.027(11) . ? Fe1 C53 2.028(12) . ? Fe1 C14 2.028(12) . ? Fe1 C11 2.030(9) . ? Fe1 C15 2.031(11) . ? Fe1 C54 2.034(12) . ? Fe1 C13 2.036(11) . ? Fe1 C55 2.046(13) . ? Fe1 C52 2.052(13) . ? Fe2 C21 2.009(11) . ? Fe2 C25 2.011(12) . ? Fe2 C63 2.029(10) . ? Fe2 C22 2.035(10) . ? Fe2 C64 2.042(11) . ? Fe2 C24 2.051(13) . ? Fe2 C61 2.052(13) . ? Fe2 C62 2.055(12) . ? Fe2 C23 2.055(12) . ? Fe2 C65 2.057(12) . ? Fe3 C31 2.009(10) . ? Fe3 C75 2.011(13) . ? Fe3 C71 2.016(13) . ? Fe3 C32 2.034(11) . ? Fe3 C74 2.039(14) . ? Fe3 C34 2.040(10) . ? Fe3 C72 2.046(15) . ? Fe3 C35 2.047(11) . ? Fe3 C73 2.059(13) . ? Fe3 C33 2.065(11) . ? Fe4 C45 2.011(11) . ? Fe4 C82 2.023(14) . ? Fe4 C44 2.025(12) . ? Fe4 C42 2.024(13) . ? Fe4 C85 2.033(14) . ? Fe4 C83 2.034(16) . ? Fe4 C41 2.046(12) . ? Fe4 C84 2.047(14) . ? Fe4 C81 2.060(14) . ? Fe4 C43 2.077(13) . ? N1A C10 1.315(11) . ? N1A C1A 1.425(12) . ? N2A C20 1.317(11) . ? N2A C2A 1.420(12) . ? C1A C2A 1.394(13) . ? C1A C6A 1.393(14) . ? C2A C3A 1.369(13) . ? C3A C4A 1.386(14) . ? C4A C5A 1.395(14) . ? C4A C7A 1.49(2) . ? C5A C6A 1.384(14) . ? C5A C8A 1.52(2) . ? C10 C11 1.404(13) . ? C11 C15 1.401(13) . ? C11 C12 1.417(13) . ? C12 C13 1.406(13) . ? C13 C14 1.430(15) . ? C14 C15 1.402(15) . ? C20 C21 1.454(14) . ? C21 C22 1.448(16) . ? C21 C25 1.450(15) . ? C22 C23 1.432(16) . ? C23 C24 1.411(18) . ? C24 C25 1.409(17) . ? N1B C30 1.304(13) . ? N1B C1B 1.413(13) . ? N2B C40 1.274(13) . ? N2B C2B 1.403(13) . ? C1B C2B 1.380(15) . ? C1B C6B 1.408(15) . ? C2B C3B 1.377(15) . ? C3B C4B 1.364(18) . ? C4B C5B 1.40(2) . ? C4B C7B 1.534(18) . ? C5B C6B 1.401(19) . ? C30 C31 1.451(14) . ? C31 C35 1.433(14) . ? C31 C32 1.451(14) . ? C32 C33 1.414(14) . ? C33 C34 1.445(15) . ? C34 C35 1.399(14) . ? C40 C41 1.425(16) . ? C41 C42 1.431(18) . ? C41 C45 1.471(16) . ? C42 C43 1.430(16) . ? C43 C44 1.433(19) . ? C44 C45 1.418(18) . ? C51 C55 1.352(17) . ? C51 C52 1.378(17) . ? C52 C53 1.433(17) . ? C53 C54 1.423(17) . ? C54 C55 1.427(19) . ? C61 C65 1.409(17) . ? C61 C62 1.472(17) . ? C63 C64 1.390(15) . ? C63 C62 1.415(16) . ? C64 C65 1.424(15) . ? C71 C75 1.37(2) . ? C71 C72 1.44(2) . ? C72 C73 1.39(2) . ? C73 C74 1.42(2) . ? C74 C75 1.44(2) . ? C81 C85 1.38(2) . ? C81 C82 1.46(2) . ? C82 C83 1.44(2) . ? C83 C84 1.34(2) . ? C84 C85 1.46(2) . ? P1 F3 1.570(8) . ? P1 F2 1.575(8) . ? P1 F6 1.583(7) . ? P1 F4 1.585(8) . ? P1 F1 1.592(8) . ? P1 F5 1.609(8) . ? C1S Cl14 0.60(5) . ? C1S C4S 1.50(4) . ? C1S Cl2 1.676(19) . ? C1S Cl4 1.714(19) . ? C1S Cl1 1.718(19) . ? C1S Cl3 1.740(19) . ? C1S Cl11 1.88(4) . ? C1S Cl12 1.89(3) . ? C1S Cl13 2.17(5) . ? C2S Cl7 1.67(2) . ? C2S Cl8 1.70(2) . ? C2S Cl5 1.720(17) . ? C2S Cl6 1.751(17) . ? C3S Cl15 1.04(4) . ? C3S Cl9 1.68(2) . ? C3S Cl10 1.71(2) . ? C4S Cl2 1.04(2) . ? C4S Cl1 1.11(3) . ? C4S Cl12 1.612(19) . ? C4S Cl11 1.65(2) . ? C4S Cl14 1.68(2) . ? C4S Cl13 1.71(2) . ? C5S Cl16 1.28(5) . ? C5S Cl10 1.644(19) . ? C5S Cl3 1.703(19) . ? C5S Cl4 2.16(3) . ? Cl1 Cl2 0.588(19) . ? Cl1 Cl12 0.75(2) . ? Cl1 Cl14 1.69(4) . ? Cl2 Cl12 0.62(2) . ? Cl2 Cl14 1.84(4) . ? Cl2 Cl11 2.47(3) . ? Cl3 Cl4 0.64(2) . ? Cl3 Cl16 1.94(4) . ? Cl3 Cl14 1.99(5) . ? Cl3 Cl12 2.40(2) . ? Cl4 Cl14 1.83(4) . ? Cl4 Cl16 2.08(4) . ? Cl6 Cl7 1.74(3) . ? Cl9 Cl15 1.66(2) . ? Cl9 Cl16 1.70(2) . ? Cl9 Cl10 2.45(3) . ? Cl10 Cl16 1.80(5) . ? Cl11 Cl14 2.27(5) . ? Cl12 Cl14 1.97(4) . ? 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 N1B Cu1 N2B 81.9(4) . . ? N1B Cu1 N2A 125.5(3) . . ? N2B Cu1 N2A 123.1(3) . . ? N1B Cu1 N1A 128.7(3) . . ? N2B Cu1 N1A 121.5(3) . . ? N2A Cu1 N1A 81.9(3) . . ? C51 Fe1 C12 122.7(5) . . ? C51 Fe1 C53 66.8(5) . . ? C12 Fe1 C53 121.6(5) . . ? C51 Fe1 C14 158.3(6) . . ? C12 Fe1 C14 68.5(5) . . ? C53 Fe1 C14 125.9(5) . . ? C51 Fe1 C11 107.3(5) . . ? C12 Fe1 C11 40.9(4) . . ? C53 Fe1 C11 156.7(5) . . ? C14 Fe1 C11 67.9(4) . . ? C51 Fe1 C15 122.3(6) . . ? C12 Fe1 C15 68.6(4) . . ? C53 Fe1 C15 162.0(5) . . ? C14 Fe1 C15 40.4(4) . . ? C11 Fe1 C15 40.4(4) . . ? C51 Fe1 C54 66.7(6) . . ? C12 Fe1 C54 158.9(6) . . ? C53 Fe1 C54 41.0(5) . . ? C14 Fe1 C54 109.9(5) . . ? C11 Fe1 C54 159.7(6) . . ? C15 Fe1 C54 124.8(5) . . ? C51 Fe1 C13 158.8(6) . . ? C12 Fe1 C13 40.5(4) . . ? C53 Fe1 C13 108.4(5) . . ? C14 Fe1 C13 41.2(4) . . ? C11 Fe1 C13 68.3(4) . . ? C15 Fe1 C13 68.8(5) . . ? C54 Fe1 C13 124.3(6) . . ? C51 Fe1 C55 38.8(5) . . ? C12 Fe1 C55 157.5(6) . . ? C53 Fe1 C55 68.4(6) . . ? C14 Fe1 C55 124.4(6) . . ? C11 Fe1 C55 122.3(5) . . ? C15 Fe1 C55 108.1(5) . . ? C54 Fe1 C55 40.9(5) . . ? C13 Fe1 C55 161.0(6) . . ? C51 Fe1 C52 39.5(5) . . ? C12 Fe1 C52 105.6(5) . . ? C53 Fe1 C52 41.1(5) . . ? C14 Fe1 C52 161.6(6) . . ? C11 Fe1 C52 119.8(5) . . ? C15 Fe1 C52 155.5(5) . . ? C54 Fe1 C52 68.9(5) . . ? C13 Fe1 C52 123.2(6) . . ? C55 Fe1 C52 67.6(6) . . ? C21 Fe2 C25 42.3(4) . . ? C21 Fe2 C63 157.0(5) . . ? C25 Fe2 C63 119.4(5) . . ? C21 Fe2 C22 41.9(4) . . ? C25 Fe2 C22 70.2(6) . . ? C63 Fe2 C22 158.8(5) . . ? C21 Fe2 C64 122.6(5) . . ? C25 Fe2 C64 106.5(5) . . ? C63 Fe2 C64 39.9(4) . . ? C22 Fe2 C64 160.3(5) . . ? C21 Fe2 C24 69.7(5) . . ? C25 Fe2 C24 40.6(5) . . ? C63 Fe2 C24 105.1(5) . . ? C22 Fe2 C24 69.0(5) . . ? C64 Fe2 C24 121.7(5) . . ? C21 Fe2 C61 124.4(5) . . ? C25 Fe2 C61 161.5(6) . . ? C63 Fe2 C61 68.7(5) . . ? C22 Fe2 C61 108.5(6) . . ? C64 Fe2 C61 68.2(5) . . ? C24 Fe2 C61 157.4(6) . . ? C21 Fe2 C62 161.6(5) . . ? C25 Fe2 C62 154.3(5) . . ? C63 Fe2 C62 40.5(5) . . ? C22 Fe2 C62 123.2(6) . . ? C64 Fe2 C62 68.3(5) . . ? C24 Fe2 C62 119.2(6) . . ? C61 Fe2 C62 42.0(5) . . ? C21 Fe2 C23 69.5(5) . . ? C25 Fe2 C23 68.5(6) . . ? C63 Fe2 C23 121.7(5) . . ? C22 Fe2 C23 41.0(4) . . ? C64 Fe2 C23 157.3(5) . . ? C24 Fe2 C23 40.2(5) . . ? C61 Fe2 C23 123.3(7) . . ? C62 Fe2 C23 106.1(6) . . ? C21 Fe2 C65 108.8(5) . . ? C25 Fe2 C65 124.6(6) . . ? C63 Fe2 C65 67.9(5) . . ? C22 Fe2 C65 124.4(5) . . ? C64 Fe2 C65 40.7(4) . . ? C24 Fe2 C65 159.5(6) . . ? C61 Fe2 C65 40.1(5) . . ? C62 Fe2 C65 68.8(6) . . ? C23 Fe2 C65 159.9(6) . . ? C31 Fe3 C75 106.5(6) . . ? C31 Fe3 C71 121.3(6) . . ? C75 Fe3 C71 39.9(6) . . ? C31 Fe3 C32 42.1(4) . . ? C75 Fe3 C32 121.7(7) . . ? C71 Fe3 C32 105.8(6) . . ? C31 Fe3 C74 123.7(7) . . ? C75 Fe3 C74 41.6(6) . . ? C71 Fe3 C74 68.1(7) . . ? C32 Fe3 C74 160.2(7) . . ? C31 Fe3 C34 68.6(4) . . ? C75 Fe3 C34 159.8(7) . . ? C71 Fe3 C34 159.5(8) . . ? C32 Fe3 C34 68.6(4) . . ? C74 Fe3 C34 123.6(6) . . ? C31 Fe3 C72 157.8(7) . . ? C75 Fe3 C72 69.3(7) . . ? C71 Fe3 C72 41.7(6) . . ? C32 Fe3 C72 120.3(7) . . ? C74 Fe3 C72 68.5(7) . . ? C34 Fe3 C72 122.8(6) . . ? C31 Fe3 C35 41.4(4) . . ? C75 Fe3 C35 123.5(6) . . ? C71 Fe3 C35 158.5(7) . . ? C32 Fe3 C35 69.7(4) . . ? C74 Fe3 C35 108.7(6) . . ? C34 Fe3 C35 40.0(4) . . ? C72 Fe3 C35 158.9(7) . . ? C31 Fe3 C73 160.9(7) . . ? C75 Fe3 C73 68.7(6) . . ? C71 Fe3 C73 67.6(7) . . ? C32 Fe3 C73 156.4(7) . . ? C74 Fe3 C73 40.6(6) . . ? C34 Fe3 C73 109.2(6) . . ? C72 Fe3 C73 39.6(6) . . ? C35 Fe3 C73 124.8(7) . . ? C31 Fe3 C33 69.3(5) . . ? C75 Fe3 C33 157.3(7) . . ? C71 Fe3 C33 121.9(7) . . ? C32 Fe3 C33 40.4(4) . . ? C74 Fe3 C33 158.9(7) . . ? C34 Fe3 C33 41.2(4) . . ? C72 Fe3 C33 105.8(6) . . ? C35 Fe3 C33 69.0(5) . . ? C73 Fe3 C33 122.4(5) . . ? C45 Fe4 C82 156.9(9) . . ? C45 Fe4 C44 41.1(5) . . ? C82 Fe4 C44 159.8(9) . . ? C45 Fe4 C42 68.6(5) . . ? C82 Fe4 C42 106.4(7) . . ? C44 Fe4 C42 68.0(6) . . ? C45 Fe4 C85 110.7(6) . . ? C82 Fe4 C85 67.6(7) . . ? C44 Fe4 C85 122.8(7) . . ? C42 Fe4 C85 163.8(8) . . ? C45 Fe4 C83 160.9(9) . . ? C82 Fe4 C83 41.6(7) . . ? C44 Fe4 C83 122.4(9) . . ? C42 Fe4 C83 118.4(7) . . ? C85 Fe4 C83 67.8(7) . . ? C45 Fe4 C41 42.5(5) . . ? C82 Fe4 C41 118.8(7) . . ? C44 Fe4 C41 70.7(6) . . ? C42 Fe4 C41 41.2(5) . . ? C85 Fe4 C41 127.2(7) . . ? C83 Fe4 C41 153.8(8) . . ? C45 Fe4 C84 127.7(8) . . ? C82 Fe4 C84 67.6(7) . . ? C44 Fe4 C84 107.5(7) . . ? C42 Fe4 C84 151.4(8) . . ? C85 Fe4 C84 42.0(6) . . ? C83 Fe4 C84 38.4(6) . . ? C41 Fe4 C84 166.6(8) . . ? C45 Fe4 C81 121.8(8) . . ? C82 Fe4 C81 41.8(7) . . ? C44 Fe4 C81 156.8(8) . . ? C42 Fe4 C81 126.2(6) . . ? C85 Fe4 C81 39.4(6) . . ? C83 Fe4 C81 70.0(8) . . ? C41 Fe4 C81 107.1(6) . . ? C84 Fe4 C81 69.0(6) . . ? C45 Fe4 C43 69.6(6) . . ? C82 Fe4 C43 122.2(8) . . ? C44 Fe4 C43 40.9(5) . . ? C42 Fe4 C43 40.8(5) . . ? C85 Fe4 C43 155.2(7) . . ? C83 Fe4 C43 103.5(8) . . ? C41 Fe4 C43 70.8(6) . . ? C84 Fe4 C43 117.0(6) . . ? C81 Fe4 C43 161.7(8) . . ? C10 N1A C1A 120.1(8) . . ? C10 N1A Cu1 132.4(7) . . ? C1A N1A Cu1 107.2(6) . . ? C20 N2A C2A 118.1(9) . . ? C20 N2A Cu1 131.5(7) . . ? C2A N2A Cu1 109.1(6) . . ? C2A C1A C6A 117.9(10) . . ? C2A C1A N1A 118.7(9) . . ? C6A C1A N1A 123.1(9) . . ? C3A C2A C1A 120.4(10) . . ? C3A C2A N2A 123.2(9) . . ? C1A C2A N2A 116.1(8) . . ? C2A C3A C4A 122.0(10) . . ? C3A C4A C5A 118.0(10) . . ? C3A C4A C7A 120.8(11) . . ? C5A C4A C7A 121.1(12) . . ? C6A C5A C4A 120.1(10) . . ? C6A C5A C8A 123.8(12) . . ? C4A C5A C8A 115.8(12) . . ? C5A C6A C1A 121.4(10) . . ? N1A C10 C11 125.7(9) . . ? C15 C11 C10 121.6(10) . . ? C15 C11 C12 108.5(9) . . ? C10 C11 C12 129.1(9) . . ? C15 C11 Fe1 69.8(6) . . ? C10 C11 Fe1 118.7(7) . . ? C12 C11 Fe1 69.4(6) . . ? C13 C12 C11 108.0(9) . . ? C13 C12 Fe1 70.1(6) . . ? C11 C12 Fe1 69.7(6) . . ? C12 C13 C14 107.2(10) . . ? C12 C13 Fe1 69.4(6) . . ? C14 C13 Fe1 69.1(7) . . ? C15 C14 C13 108.3(10) . . ? C15 C14 Fe1 69.9(7) . . ? C13 C14 Fe1 69.7(7) . . ? C11 C15 C14 108.0(10) . . ? C11 C15 Fe1 69.8(6) . . ? C14 C15 Fe1 69.7(7) . . ? N2A C20 C21 124.5(10) . . ? C22 C21 C25 106.8(10) . . ? C22 C21 C20 127.0(11) . . ? C25 C21 C20 126.2(11) . . ? C22 C21 Fe2 70.0(6) . . ? C25 C21 Fe2 68.9(6) . . ? C20 C21 Fe2 126.7(8) . . ? C23 C22 C21 107.2(12) . . ? C23 C22 Fe2 70.3(7) . . ? C21 C22 Fe2 68.0(6) . . ? C24 C23 C22 109.0(12) . . ? C24 C23 Fe2 69.8(7) . . ? C22 C23 Fe2 68.8(7) . . ? C25 C24 C23 108.5(11) . . ? C25 C24 Fe2 68.2(7) . . ? C23 C24 Fe2 70.0(7) . . ? C24 C25 C21 108.5(12) . . ? C24 C25 Fe2 71.2(8) . . ? C21 C25 Fe2 68.8(7) . . ? C30 N1B C1B 119.0(10) . . ? C30 N1B Cu1 132.1(8) . . ? C1B N1B Cu1 108.9(7) . . ? C40 N2B C2B 117.2(10) . . ? C40 N2B Cu1 130.7(8) . . ? C2B N2B Cu1 110.4(7) . . ? C2B C1B C6B 117.7(11) . . ? C2B C1B N1B 118.8(10) . . ? C6B C1B N1B 123.2(12) . . ? C3B C2B C1B 121.2(12) . . ? C3B C2B N2B 123.2(11) . . ? C1B C2B N2B 115.6(10) . . ? C4B C3B C2B 120.9(14) . . ? C3B C4B C5B 120.6(13) . . ? C3B C4B C7B 122.9(17) . . ? C5B C4B C7B 116.4(16) . . ? C4B C5B C6B 117.9(14) . . ? C5B C6B C1B 121.6(14) . . ? N1B C30 C31 127.3(11) . . ? C35 C31 C32 108.0(10) . . ? C35 C31 C30 124.0(10) . . ? C32 C31 C30 127.8(10) . . ? C35 C31 Fe3 70.7(6) . . ? C32 C31 Fe3 69.9(6) . . ? C30 C31 Fe3 120.4(7) . . ? C33 C32 C31 108.0(10) . . ? C33 C32 Fe3 71.0(6) . . ? C31 C32 Fe3 68.0(6) . . ? C32 C33 C34 106.9(10) . . ? C32 C33 Fe3 68.6(6) . . ? C34 C33 Fe3 68.5(6) . . ? C35 C34 C33 109.9(10) . . ? C35 C34 Fe3 70.2(6) . . ? C33 C34 Fe3 70.3(6) . . ? C34 C35 C31 107.3(10) . . ? C34 C35 Fe3 69.7(6) . . ? C31 C35 Fe3 67.9(6) . . ? N2B C40 C41 125.7(11) . . ? C40 C41 C42 127.2(11) . . ? C40 C41 C45 129.2(13) . . ? C42 C41 C45 103.2(12) . . ? C40 C41 Fe4 121.3(9) . . ? C42 C41 Fe4 68.6(7) . . ? C45 C41 Fe4 67.5(7) . . ? C43 C42 C41 113.2(13) . . ? C43 C42 Fe4 71.6(7) . . ? C41 C42 Fe4 70.2(7) . . ? C42 C43 C44 104.5(13) . . ? C42 C43 Fe4 67.6(7) . . ? C44 C43 Fe4 67.6(7) . . ? C45 C44 C43 109.9(13) . . ? C45 C44 Fe4 68.9(7) . . ? C43 C44 Fe4 71.5(8) . . ? C44 C45 C41 109.2(13) . . ? C44 C45 Fe4 70.0(8) . . ? C41 C45 Fe4 70.0(7) . . ? C55 C51 C52 113.4(13) . . ? C55 C51 Fe1 71.5(8) . . ? C52 C51 Fe1 71.4(8) . . ? C51 C52 C53 105.0(12) . . ? C51 C52 Fe1 69.1(8) . . ? C53 C52 Fe1 68.5(7) . . ? C54 C53 C52 108.1(12) . . ? C54 C53 Fe1 69.7(7) . . ? C52 C53 Fe1 70.4(7) . . ? C53 C54 C55 106.8(12) . . ? C53 C54 Fe1 69.2(7) . . ? C55 C54 Fe1 70.0(7) . . ? C51 C55 C54 106.8(14) . . ? C51 C55 Fe1 69.7(8) . . ? C54 C55 Fe1 69.1(8) . . ? C65 C61 C62 107.5(12) . . ? C65 C61 Fe2 70.2(7) . . ? C62 C61 Fe2 69.1(7) . . ? C64 C63 C62 110.1(11) . . ? C64 C63 Fe2 70.5(6) . . ? C62 C63 Fe2 70.7(6) . . ? C63 C62 C61 105.8(12) . . ? C63 C62 Fe2 68.8(7) . . ? C61 C62 Fe2 68.9(7) . . ? C63 C64 C65 108.3(11) . . ? C63 C64 Fe2 69.6(6) . . ? C65 C64 Fe2 70.3(7) . . ? C61 C65 C64 108.3(12) . . ? C61 C65 Fe2 69.7(7) . . ? C64 C65 Fe2 69.1(7) . . ? C75 C71 C72 109.8(17) . . ? C75 C71 Fe3 69.9(8) . . ? C72 C71 Fe3 70.3(8) . . ? C73 C72 C71 106.1(17) . . ? C73 C72 Fe3 70.7(9) . . ? C71 C72 Fe3 68.1(8) . . ? C72 C73 C74 109.7(17) . . ? C72 C73 Fe3 69.7(9) . . ? C74 C73 Fe3 69.0(8) . . ? C73 C74 C75 106.8(17) . . ? C73 C74 Fe3 70.4(9) . . ? C75 C74 Fe3 68.1(8) . . ? C71 C75 C74 107.6(17) . . ? C71 C75 Fe3 70.3(8) . . ? C74 C75 Fe3 70.2(8) . . ? C85 C81 C82 105.2(16) . . ? C85 C81 Fe4 69.2(8) . . ? C82 C81 Fe4 67.7(9) . . ? C83 C82 C81 108.1(15) . . ? C83 C82 Fe4 69.6(9) . . ? C81 C82 Fe4 70.4(8) . . ? C84 C83 C82 108.7(18) . . ? C84 C83 Fe4 71.3(9) . . ? C82 C83 Fe4 68.8(9) . . ? C83 C84 C85 108.0(17) . . ? C83 C84 Fe4 70.3(10) . . ? C85 C84 Fe4 68.5(8) . . ? C81 C85 C84 110.0(17) . . ? C81 C85 Fe4 71.4(9) . . ? C84 C85 Fe4 69.5(9) . . ? F3 P1 F2 92.8(6) . . ? F3 P1 F6 88.4(5) . . ? F2 P1 F6 90.2(4) . . ? F3 P1 F4 91.1(5) . . ? F2 P1 F4 90.0(5) . . ? F6 P1 F4 179.5(5) . . ? F3 P1 F1 178.4(6) . . ? F2 P1 F1 88.8(5) . . ? F6 P1 F1 91.4(5) . . ? F4 P1 F1 89.1(5) . . ? F3 P1 F5 89.3(5) . . ? F2 P1 F5 177.8(6) . . ? F6 P1 F5 89.4(5) . . ? F4 P1 F5 90.5(5) . . ? F1 P1 F5 89.1(5) . . ? Cl14 C1S C4S 96(4) . . ? Cl14 C1S Cl2 96(5) . . ? C4S C1S Cl2 37.5(10) . . ? Cl14 C1S Cl4 92(5) . . ? C4S C1S Cl4 152(2) . . ? Cl2 C1S Cl4 115.1(16) . . ? Cl14 C1S Cl1 77(4) . . ? C4S C1S Cl1 39.5(10) . . ? Cl2 C1S Cl1 19.9(7) . . ? Cl4 C1S Cl1 118.3(17) . . ? Cl14 C1S Cl3 106(5) . . ? C4S C1S Cl3 132(2) . . ? Cl2 C1S Cl3 97.0(14) . . ? Cl4 C1S Cl3 21.4(7) . . ? Cl1 C1S Cl3 105.2(15) . . ? Cl14 C1S Cl11 124(5) . . ? C4S C1S Cl11 57.0(13) . . ? Cl2 C1S Cl11 87.9(14) . . ? Cl4 C1S Cl11 136.1(19) . . ? Cl1 C1S Cl11 96.2(13) . . ? Cl3 C1S Cl11 129(2) . . ? Cl14 C1S Cl12 89(5) . . ? C4S C1S Cl12 55.3(10) . . ? Cl2 C1S Cl12 18.7(7) . . ? Cl4 C1S Cl12 98.4(14) . . ? Cl1 C1S Cl12 23.3(8) . . ? Cl3 C1S Cl12 82.7(12) . . ? Cl11 C1S Cl12 106.3(14) . . ? Cl14 C1S Cl13 125(5) . . ? C4S C1S Cl13 51.6(16) . . ? Cl2 C1S Cl13 81.9(17) . . ? Cl4 C1S Cl13 139(2) . . ? Cl1 C1S Cl13 90.6(16) . . ? Cl3 C1S Cl13 129(2) . . ? Cl11 C1S Cl13 6.0(17) . . ? Cl12 C1S Cl13 100.3(17) . . ? Cl7 C2S Cl8 98.4(19) . . ? Cl7 C2S Cl5 113.2(16) . . ? Cl8 C2S Cl5 15.0(11) . . ? Cl7 C2S Cl6 61.0(11) . . ? Cl8 C2S Cl6 109.4(15) . . ? Cl5 C2S Cl6 113.8(12) . . ? Cl15 C3S Cl9 70.9(16) . . ? Cl15 C3S Cl10 163(2) . . ? Cl9 C3S Cl10 92.5(17) . . ? Cl2 C4S Cl1 31.6(12) . . ? Cl2 C4S C1S 80(2) . . ? Cl1 C4S C1S 80.8(19) . . ? Cl2 C4S Cl12 9.9(14) . . ? Cl1 C4S Cl12 23.9(13) . . ? C1S C4S Cl12 74.7(15) . . ? Cl2 C4S Cl11 133(3) . . ? Cl1 C4S Cl11 153(3) . . ? C1S C4S Cl11 73(2) . . ? Cl12 C4S Cl11 136(3) . . ? Cl2 C4S Cl14 82(3) . . ? Cl1 C4S Cl14 71(2) . . ? C1S C4S Cl14 21(2) . . ? Cl12 C4S Cl14 74(2) . . ? Cl11 C4S Cl14 86(2) . . ? Cl2 C4S Cl13 135(4) . . ? Cl1 C4S Cl13 162(4) . . ? C1S C4S Cl13 85(3) . . ? Cl12 C4S Cl13 140(3) . . ? Cl11 C4S Cl13 12(3) . . ? Cl14 C4S Cl13 98(3) . . ? Cl16 C5S Cl10 75(3) . . ? Cl16 C5S Cl3 80(3) . . ? Cl10 C5S Cl3 153(3) . . ? Cl16 C5S Cl4 69(2) . . ? Cl10 C5S Cl4 140(3) . . ? Cl3 C5S Cl4 13.5(7) . . ? Cl2 Cl1 Cl12 54(2) . . ? Cl2 Cl1 C4S 67(3) . . ? Cl12 Cl1 C4S 119(3) . . ? Cl2 Cl1 Cl14 96(3) . . ? Cl12 Cl1 Cl14 101(2) . . ? C4S Cl1 Cl14 70.5(19) . . ? Cl2 Cl1 C1S 76(2) . . ? Cl12 Cl1 C1S 91(2) . . ? C4S Cl1 C1S 59.8(18) . . ? Cl14 Cl1 C1S 20.3(18) . . ? Cl1 Cl2 Cl12 77(3) . . ? Cl1 Cl2 C4S 81(3) . . ? Cl12 Cl2 C4S 153(4) . . ? Cl1 Cl2 C1S 84(2) . . ? Cl12 Cl2 C1S 101(3) . . ? C4S Cl2 C1S 62.2(19) . . ? Cl1 Cl2 Cl14 65(2) . . ? Cl12 Cl2 Cl14 93(3) . . ? C4S Cl2 Cl14 64(2) . . ? C1S Cl2 Cl14 18.9(17) . . ? Cl1 Cl2 Cl11 105(3) . . ? Cl12 Cl2 Cl11 149(3) . . ? C4S Cl2 Cl11 29(2) . . ? C1S Cl2 Cl11 49.5(12) . . ? Cl14 Cl2 Cl11 61.5(16) . . ? Cl4 Cl3 C5S 128(3) . . ? Cl4 Cl3 C1S 77.0(18) . . ? C5S Cl3 C1S 154(2) . . ? Cl4 Cl3 Cl16 94(3) . . ? C5S Cl3 Cl16 40.5(19) . . ? C1S Cl3 Cl16 145.7(19) . . ? Cl4 Cl3 Cl14 67(2) . . ? C5S Cl3 Cl14 165(2) . . ? C1S Cl3 Cl14 16.9(16) . . ? Cl16 Cl3 Cl14 153(2) . . ? Cl4 Cl3 Cl12 115(2) . . ? C5S Cl3 Cl12 112.7(17) . . ? C1S Cl3 Cl12 51.4(9) . . ? Cl16 Cl3 Cl12 151.5(16) . . ? Cl14 Cl3 Cl12 52.4(12) . . ? Cl3 Cl4 C1S 81.6(19) . . ? Cl3 Cl4 Cl14 95(2) . . ? C1S Cl4 Cl14 19.1(16) . . ? Cl3 Cl4 Cl16 68(2) . . ? C1S Cl4 Cl16 135.5(19) . . ? Cl14 Cl4 Cl16 155(2) . . ? Cl3 Cl4 C5S 38(2) . . ? C1S Cl4 C5S 119.5(16) . . ? Cl14 Cl4 C5S 132.8(19) . . ? Cl16 Cl4 C5S 35.1(14) . . ? Cl7 Cl6 C2S 57.3(8) . . ? C2S Cl7 Cl6 61.7(9) . . ? Cl15 Cl9 C3S 36.3(15) . . ? Cl15 Cl9 Cl16 128(3) . . ? C3S Cl9 Cl16 91(2) . . ? Cl15 Cl9 Cl10 80.6(15) . . ? C3S Cl9 Cl10 44.3(10) . . ? Cl16 Cl9 Cl10 47.2(18) . . ? C5S Cl10 C3S 131(2) . . ? C5S Cl10 Cl16 43.4(17) . . ? C3S Cl10 Cl16 87.2(16) . . ? C5S Cl10 Cl9 87.4(18) . . ? C3S Cl10 Cl9 43.2(9) . . ? Cl16 Cl10 Cl9 44.0(9) . . ? C4S Cl11 C1S 50.0(14) . . ? C4S Cl11 Cl14 47.6(13) . . ? C1S Cl11 Cl14 12.7(14) . . ? C4S Cl11 Cl2 17.9(13) . . ? C1S Cl11 Cl2 42.7(7) . . ? Cl14 Cl11 Cl2 45.5(11) . . ? Cl2 Cl12 Cl1 50(2) . . ? Cl2 Cl12 C4S 17(2) . . ? Cl1 Cl12 C4S 37(2) . . ? Cl2 Cl12 C1S 60(2) . . ? Cl1 Cl12 C1S 65.2(18) . . ? C4S Cl12 C1S 50.1(13) . . ? Cl2 Cl12 Cl14 69(2) . . ? Cl1 Cl12 Cl14 57(2) . . ? C4S Cl12 Cl14 54.7(12) . . ? C1S Cl12 Cl14 17.7(16) . . ? Cl2 Cl12 Cl3 98(3) . . ? Cl1 Cl12 Cl3 110(2) . . ? C4S Cl12 Cl3 93.1(14) . . ? C1S Cl12 Cl3 45.9(7) . . ? Cl14 Cl12 Cl3 53.0(14) . . ? C4S Cl13 C1S 43.8(16) . . ? C1S Cl14 Cl1 83(4) . . ? C1S Cl14 C4S 63(3) . . ? Cl1 Cl14 C4S 38.4(11) . . ? C1S Cl14 Cl4 69(4) . . ? Cl1 Cl14 Cl4 114(3) . . ? C4S Cl14 Cl4 125(3) . . ? C1S Cl14 Cl2 65(4) . . ? Cl1 Cl14 Cl2 18.5(8) . . ? C4S Cl14 Cl2 33.8(10) . . ? Cl4 Cl14 Cl2 102(2) . . ? C1S Cl14 Cl12 74(5) . . ? Cl1 Cl14 Cl12 21.9(9) . . ? C4S Cl14 Cl12 51.6(11) . . ? Cl4 Cl14 Cl12 92(2) . . ? Cl2 Cl14 Cl12 18.3(7) . . ? C1S Cl14 Cl3 57(4) . . ? Cl1 Cl14 Cl3 96(2) . . ? C4S Cl14 Cl3 108(3) . . ? Cl4 Cl14 Cl3 18.7(8) . . ? Cl2 Cl14 Cl3 83.6(19) . . ? Cl12 Cl14 Cl3 74.6(18) . . ? C1S Cl14 Cl11 43(4) . . ? Cl1 Cl14 Cl11 83.9(16) . . ? C4S Cl14 Cl11 46.4(13) . . ? Cl4 Cl14 Cl11 108(2) . . ? Cl2 Cl14 Cl11 73.0(15) . . ? Cl12 Cl14 Cl11 90.4(16) . . ? Cl3 Cl14 Cl11 100(2) . . ? C3S Cl15 Cl9 72.8(16) . . ? C5S Cl16 Cl9 151(4) . . ? C5S Cl16 Cl10 62(2) . . ? Cl9 Cl16 Cl10 89(2) . . ? C5S Cl16 Cl3 59.8(15) . . ? Cl9 Cl16 Cl3 149(3) . . ? Cl10 Cl16 Cl3 121(2) . . ? C5S Cl16 Cl4 75.7(18) . . ? Cl9 Cl16 Cl4 132(3) . . ? Cl10 Cl16 Cl4 134(2) . . ? Cl3 Cl16 Cl4 17.9(7) . . ? _diffrn_measured_fraction_theta_max 0.935 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.935 _refine_diff_density_max 0.758 _refine_diff_density_min -0.440 _refine_diff_density_rms 0.107