# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_dw0944 _database_code_depnum_ccdc_archive 'CCDC 768905' #TrackingRef 'compound 5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H36 Fe4 P4' _chemical_formula_sum 'C40 H36 Fe4 P4' _chemical_formula_weight 863.97 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' 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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P-4 _symmetry_space_group_name_Hall P-4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' _cell_length_a 11.6520(16) _cell_length_b 11.6520(16) _cell_length_c 6.2473(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 848.2(2) _cell_formula_units_Z 1 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 12296 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 29.13 _exptl_crystal_description block _exptl_crystal_colour dark-red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.691 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 440 _exptl_absorpt_coefficient_mu 1.896 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.742 _exptl_absorpt_correction_T_max 0.934 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 11580 _diffrn_reflns_av_R_equivalents 0.0529 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 3.70 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1499 _reflns_number_gt 1478 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _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^)+(0.0603P)^2^+1.3579P] 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 0.48(7) _refine_ls_number_reflns 1499 _refine_ls_number_parameters 119 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0421 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.1077 _refine_ls_wR_factor_gt 0.1065 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.23260(7) 0.28199(8) -0.23737(19) 0.0335(3) Uani 1 1 d . A . P1 P 0.0412(3) 0.1218(2) 0.0559(4) 0.0234(6) Uani 0.70 1 d P A 1 P2 P 0.0403(6) 0.1224(6) -0.5542(12) 0.0346(15) Uani 0.30 1 d P A 2 C11 C 0.0793(9) 0.2174(10) -0.1540(15) 0.045(2) Uani 1 1 d . . . H11 H 0.0714 0.1606 -0.0459 0.054 Uiso 0.30 1 calc PR A 2 C12 C 0.0928(10) 0.2050(12) -0.3689(15) 0.058(3) Uani 1 1 d . A . H12 H 0.0830 0.1338 -0.4409 0.070 Uiso 0.70 1 calc PR B 1 C13 C 0.1228(7) 0.3084(9) -0.4759(17) 0.055(2) Uani 1 1 d . . . H13 H 0.1479 0.3166 -0.6197 0.066 Uiso 1 1 calc R A . C14 C 0.1077(9) 0.3940(10) -0.3273(14) 0.055(3) Uani 1 1 d . A . H14 H 0.1153 0.4739 -0.3539 0.066 Uiso 1 1 calc R . . C15 C 0.0801(8) 0.3455(10) -0.1350(17) 0.055(3) Uani 1 1 d . A . H15 H 0.0638 0.3870 -0.0076 0.066 Uiso 1 1 calc R . . C21 C 0.3462(7) 0.2088(8) -0.0173(18) 0.056(3) Uani 1 1 d . . . H21 H 0.3281 0.1581 0.0969 0.067 Uiso 1 1 calc R A . C22 C 0.3512(7) 0.3336(7) -0.0016(17) 0.0429(19) Uani 1 1 d . A . H22 H 0.3367 0.3798 0.1207 0.051 Uiso 1 1 calc R . . C23 C 0.3839(7) 0.3718(7) -0.218(2) 0.057(3) Uani 1 1 d . . . H23 H 0.3965 0.4488 -0.2626 0.069 Uiso 1 1 calc R A . C24 C 0.3931(8) 0.2736(11) -0.3474(17) 0.065(3) Uani 1 1 d . A . H24 H 0.4110 0.2739 -0.4958 0.078 Uiso 1 1 calc R . . C25 C 0.3721(6) 0.1755(6) -0.2257(16) 0.0429(18) Uani 1 1 d . A . H25 H 0.3749 0.0987 -0.2766 0.052 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 0.0231(4) 0.0274(4) 0.0501(5) 0.0032(6) 0.0011(6) -0.0010(4) P1 0.0294(16) 0.0265(13) 0.0142(10) -0.0019(11) -0.0002(10) -0.0019(14) P2 0.025(4) 0.016(3) 0.064(4) -0.004(3) 0.003(3) -0.002(3) C11 0.050(5) 0.041(5) 0.044(4) -0.004(4) 0.007(4) -0.028(5) C12 0.060(7) 0.075(8) 0.041(4) 0.022(5) -0.019(4) -0.037(7) C13 0.033(4) 0.069(6) 0.063(6) 0.026(5) -0.015(4) -0.023(4) C14 0.057(6) 0.057(6) 0.051(5) 0.027(5) 0.008(5) 0.016(5) C15 0.023(5) 0.063(6) 0.080(7) -0.021(5) 0.010(4) 0.019(4) C21 0.036(4) 0.044(5) 0.088(7) 0.015(5) -0.017(5) 0.002(4) C22 0.026(4) 0.032(4) 0.070(5) -0.002(4) -0.010(4) -0.004(3) C23 0.023(3) 0.037(4) 0.111(9) 0.013(6) -0.006(6) -0.012(3) C24 0.039(4) 0.083(7) 0.072(5) 0.016(6) 0.033(4) 0.007(5) C25 0.033(4) 0.039(4) 0.056(5) 0.004(5) 0.010(5) 0.006(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 1.988(9) . ? Fe1 C11 2.007(9) . ? Fe1 C15 2.028(9) . ? Fe1 C23 2.054(8) . ? Fe1 C12 2.033(10) . ? Fe1 C25 2.046(7) . ? Fe1 C22 2.107(9) . ? Fe1 C24 1.995(8) . ? Fe1 C14 2.034(9) . ? Fe1 C21 2.090(9) . ? P1 C11 1.777(11) . ? P1 P1 2.230(4) 3 ? P1 P1 2.230(4) 4 ? P2 C12 1.625(12) . ? P2 P2 2.228(10) 3_554 ? P2 P2 2.228(10) 4_554 ? C11 C12 1.360(12) . ? C11 C15 1.497(15) . ? C11 H11 0.9500 . ? C12 C13 1.422(15) . ? C12 H12 0.9500 . ? C13 C14 1.373(15) . ? C13 H13 0.9500 . ? C14 C15 1.366(13) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C21 C25 1.391(15) . ? C21 C22 1.458(11) . ? C21 H21 0.9500 . ? C22 C23 1.476(17) . ? C22 H22 0.9500 . ? C23 C24 1.403(15) . ? C23 H23 0.9500 . ? C24 C25 1.394(13) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? 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 C11 71.3(4) . . ? C13 Fe1 C15 67.4(5) . . ? C11 Fe1 C15 43.5(4) . . ? C13 Fe1 C23 121.1(4) . . ? C11 Fe1 C23 160.1(5) . . ? C15 Fe1 C23 123.2(4) . . ? C13 Fe1 C12 41.4(4) . . ? C11 Fe1 C12 39.3(3) . . ? C15 Fe1 C12 65.6(5) . . ? C23 Fe1 C12 159.4(4) . . ? C13 Fe1 C25 129.2(4) . . ? C11 Fe1 C25 118.1(4) . . ? C15 Fe1 C25 154.9(4) . . ? C23 Fe1 C25 68.0(3) . . ? C12 Fe1 C25 112.5(5) . . ? C13 Fe1 C22 154.4(4) . . ? C11 Fe1 C22 120.6(4) . . ? C15 Fe1 C22 104.5(4) . . ? C23 Fe1 C22 41.5(5) . . ? C12 Fe1 C22 159.0(3) . . ? C25 Fe1 C22 68.1(4) . . ? C13 Fe1 C24 110.7(4) . . ? C11 Fe1 C24 154.9(5) . . ? C15 Fe1 C24 161.4(5) . . ? C23 Fe1 C24 40.5(5) . . ? C12 Fe1 C24 126.2(5) . . ? C25 Fe1 C24 40.4(4) . . ? C22 Fe1 C24 68.9(4) . . ? C13 Fe1 C14 39.9(4) . . ? C11 Fe1 C14 71.1(6) . . ? C15 Fe1 C14 39.3(4) . . ? C23 Fe1 C14 107.7(4) . . ? C12 Fe1 C14 66.3(5) . . ? C25 Fe1 C14 165.3(4) . . ? C22 Fe1 C14 118.6(4) . . ? C24 Fe1 C14 127.4(5) . . ? C13 Fe1 C21 164.5(4) . . ? C11 Fe1 C21 103.9(4) . . ? C15 Fe1 C21 119.7(4) . . ? C23 Fe1 C21 68.0(4) . . ? C12 Fe1 C21 126.4(4) . . ? C25 Fe1 C21 39.3(4) . . ? C22 Fe1 C21 40.6(3) . . ? C24 Fe1 C21 67.2(4) . . ? C14 Fe1 C21 153.7(4) . . ? C11 P1 P1 101.4(4) . 3 ? C11 P1 P1 104.2(4) . 4 ? P1 P1 P1 84.38(7) 3 4 ? C12 P2 P2 97.3(7) . 3_554 ? C12 P2 P2 111.0(6) . 4_554 ? P2 P2 P2 84.7(2) 3_554 4_554 ? C12 C11 C15 100.6(12) . . ? C12 C11 P1 133.7(12) . . ? C15 C11 P1 124.6(8) . . ? C12 C11 Fe1 71.4(7) . . ? C15 C11 Fe1 69.0(5) . . ? P1 C11 Fe1 130.5(7) . . ? C12 C11 H11 129.7 . . ? C15 C11 H11 129.7 . . ? P1 C11 H11 9.8 . . ? Fe1 C11 H11 122.1 . . ? C11 C12 C13 113.8(14) . . ? C11 C12 P2 136.3(11) . . ? C13 C12 P2 105.1(7) . . ? C11 C12 Fe1 69.3(7) . . ? C13 C12 Fe1 67.6(6) . . ? P2 C12 Fe1 148.3(8) . . ? C11 C12 H12 123.1 . . ? C13 C12 H12 123.1 . . ? P2 C12 H12 25.9 . . ? Fe1 C12 H12 132.2 . . ? C12 C13 C14 105.4(9) . . ? C12 C13 Fe1 71.0(5) . . ? C14 C13 Fe1 71.8(6) . . ? C12 C13 H13 127.3 . . ? C14 C13 H13 127.3 . . ? Fe1 C13 H13 121.7 . . ? C15 C14 C13 108.9(10) . . ? C15 C14 Fe1 70.1(6) . . ? C13 C14 Fe1 68.3(6) . . ? C15 C14 H14 125.5 . . ? C13 C14 H14 125.5 . . ? Fe1 C14 H14 127.7 . . ? C14 C15 C11 110.1(10) . . ? C14 C15 Fe1 70.6(6) . . ? C11 C15 Fe1 67.5(6) . . ? C14 C15 H15 124.9 . . ? C11 C15 H15 124.9 . . ? Fe1 C15 H15 128.7 . . ? C25 C21 C22 109.4(9) . . ? C25 C21 Fe1 68.6(5) . . ? C22 C21 Fe1 70.3(5) . . ? C25 C21 H21 125.3 . . ? C22 C21 H21 125.3 . . ? Fe1 C21 H21 127.4 . . ? C23 C22 C21 104.4(8) . . ? C23 C22 Fe1 67.3(5) . . ? C21 C22 Fe1 69.0(5) . . ? C23 C22 H22 127.8 . . ? C21 C22 H22 127.8 . . ? Fe1 C22 H22 127.4 . . ? C22 C23 C24 107.5(8) . . ? C22 C23 Fe1 71.2(5) . . ? C24 C23 Fe1 67.5(5) . . ? C22 C23 H23 126.3 . . ? C24 C23 H23 126.3 . . ? Fe1 C23 H23 126.6 . . ? C23 C24 C25 110.0(8) . . ? C23 C24 Fe1 72.0(5) . . ? C25 C24 Fe1 71.8(5) . . ? C23 C24 H24 125.0 . . ? C25 C24 H24 125.0 . . ? Fe1 C24 H24 122.8 . . ? C21 C25 C24 108.6(8) . . ? C21 C25 Fe1 72.1(5) . . ? C24 C25 Fe1 67.9(5) . . ? C21 C25 H25 125.7 . . ? C24 C25 H25 125.7 . . ? Fe1 C25 H25 125.9 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.583 _refine_diff_density_min -0.315 _refine_diff_density_rms 0.086 data_dw0946 _database_code_depnum_ccdc_archive 'CCDC 768906' #TrackingRef 'compound 6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H45 Fe5 P5, C6 H6' _chemical_formula_sum 'C56 H51 Fe5 P5' _chemical_formula_weight 1158.07 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' 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' 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' '-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 10.85880(10) _cell_length_b 24.6233(2) _cell_length_c 36.4979(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9758.79(14) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 156454 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description Plate _exptl_crystal_colour Orange _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.576 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4736 _exptl_absorpt_coefficient_mu 1.654 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.795 _exptl_absorpt_correction_T_max 0.930 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 88631 _diffrn_reflns_av_R_equivalents 0.1023 _diffrn_reflns_av_sigmaI/netI 0.0532 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 26.37 _reflns_number_total 9973 _reflns_number_gt 7272 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _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. The lattice solvent (benzene) is disordered rotationally. The disorder was not modelled, but because of the disorder, it was necessary to use AFIX 66 to model the benzene, and leading to a relatively high displacement para- meters for all carbon on the benzene. ; _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^)+(0.0210P)^2^+21.7979P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9973 _refine_ls_number_parameters 583 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0786 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.0897 _refine_ls_wR_factor_gt 0.0793 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.42899(8) 0.26339(4) 0.66550(2) 0.0216(2) Uani 1 1 d . . . P2 P 0.54147(8) 0.33810(4) 0.66407(2) 0.0218(2) Uani 1 1 d . . . P3 P 0.57539(9) 0.33537(4) 0.60468(2) 0.0218(2) Uani 1 1 d . . . P4 P 0.65868(8) 0.25288(4) 0.59890(2) 0.0213(2) Uani 1 1 d . . . P5 P 0.50036(9) 0.20738(4) 0.62288(3) 0.0231(2) Uani 1 1 d . . . Fe1 Fe 0.14232(5) 0.24700(2) 0.626230(14) 0.02333(12) Uani 1 1 d . . . C1 C 0.2935(3) 0.29028(15) 0.64263(9) 0.0220(8) Uani 1 1 d . . . C2 C 0.2685(3) 0.29969(15) 0.60466(10) 0.0243(8) Uani 1 1 d . . . H2A H 0.3233 0.2923 0.5850 0.029 Uiso 1 1 calc R . . C3 C 0.1484(3) 0.32177(15) 0.60120(10) 0.0264(8) Uani 1 1 d . . . H3A H 0.1088 0.3315 0.5789 0.032 Uiso 1 1 calc R . . C4 C 0.0981(3) 0.32681(15) 0.63687(10) 0.0282(9) Uani 1 1 d . . . H4A H 0.0189 0.3408 0.6427 0.034 Uiso 1 1 calc R . . C5 C 0.1860(3) 0.30740(15) 0.66235(10) 0.0246(8) Uani 1 1 d . . . H5A H 0.1755 0.3059 0.6882 0.030 Uiso 1 1 calc R . . C6 C 0.1817(4) 0.16636(15) 0.63338(11) 0.0327(9) Uani 1 1 d . . . H6A H 0.2571 0.1519 0.6422 0.039 Uiso 1 1 calc R . . C7 C 0.1536(4) 0.17684(16) 0.59659(11) 0.0353(10) Uani 1 1 d . . . H7A H 0.2067 0.1710 0.5763 0.042 Uiso 1 1 calc R . . C8 C 0.0327(4) 0.19755(17) 0.59506(12) 0.0381(10) Uani 1 1 d . . . H8A H -0.0105 0.2080 0.5735 0.046 Uiso 1 1 calc R . . C9 C -0.0126(4) 0.20000(16) 0.63126(12) 0.0364(10) Uani 1 1 d . . . H9A H -0.0919 0.2125 0.6384 0.044 Uiso 1 1 calc R . . C10 C 0.0799(4) 0.18076(16) 0.65509(11) 0.0334(10) Uani 1 1 d . . . H10A H 0.0743 0.1780 0.6810 0.040 Uiso 1 1 calc R . . Fe2 Fe 0.80630(5) 0.35958(2) 0.714044(14) 0.02368(13) Uani 1 1 d . . . C11 C 0.6751(3) 0.31260(14) 0.68854(9) 0.0215(8) Uani 1 1 d . . . C12 C 0.6752(3) 0.30325(15) 0.72751(10) 0.0254(8) Uani 1 1 d . . . H12A H 0.6074 0.3088 0.7435 0.030 Uiso 1 1 calc R . . C13 C 0.7941(3) 0.28434(15) 0.73799(10) 0.0276(9) Uani 1 1 d . . . H13A H 0.8191 0.2749 0.7621 0.033 Uiso 1 1 calc R . . C14 C 0.8684(3) 0.28215(15) 0.70608(10) 0.0255(8) Uani 1 1 d . . . H14A H 0.9520 0.2709 0.7051 0.031 Uiso 1 1 calc R . . C15 C 0.7964(3) 0.29956(14) 0.67590(10) 0.0236(8) Uani 1 1 d . . . H15A H 0.8241 0.3022 0.6513 0.028 Uiso 1 1 calc R . . C16 C 0.7621(4) 0.43918(17) 0.70503(13) 0.0432(11) Uani 1 1 d . . . H16A H 0.6892 0.4521 0.6936 0.052 Uiso 1 1 calc R . . C17 C 0.7783(4) 0.42969(17) 0.74307(13) 0.0454(12) Uani 1 1 d . . . H17A H 0.7184 0.4351 0.7617 0.054 Uiso 1 1 calc R . . C18 C 0.8999(4) 0.41064(16) 0.74823(12) 0.0404(11) Uani 1 1 d . . . H18A H 0.9363 0.4008 0.7710 0.048 Uiso 1 1 calc R . . C19 C 0.9573(4) 0.40880(16) 0.71380(12) 0.0370(10) Uani 1 1 d . . . H19A H 1.0396 0.3977 0.7092 0.044 Uiso 1 1 calc R . . C20 C 0.8725(4) 0.42608(16) 0.68747(12) 0.0389(11) Uani 1 1 d . . . H20A H 0.8875 0.4285 0.6619 0.047 Uiso 1 1 calc R . . Fe3 Fe 0.74239(5) 0.42015(2) 0.550199(14) 0.02430(13) Uani 1 1 d . . . C21 C 0.7060(3) 0.38133(15) 0.59879(9) 0.0230(8) Uani 1 1 d . . . C22 C 0.8305(3) 0.37140(16) 0.58757(9) 0.0250(8) Uani 1 1 d . . . H22A H 0.8661 0.3368 0.5829 0.030 Uiso 1 1 calc R . . C23 C 0.8910(4) 0.42216(17) 0.58462(10) 0.0323(9) Uani 1 1 d . . . H23A H 0.9745 0.4275 0.5777 0.039 Uiso 1 1 calc R . . C24 C 0.8061(4) 0.46371(17) 0.59377(10) 0.0332(10) Uani 1 1 d . . . H24A H 0.8227 0.5016 0.5941 0.040 Uiso 1 1 calc R . . C25 C 0.6920(4) 0.43861(16) 0.60229(10) 0.0288(9) Uani 1 1 d . . . H25A H 0.6186 0.4569 0.6092 0.035 Uiso 1 1 calc R . . C26 C 0.6416(4) 0.38485(17) 0.50920(11) 0.0368(10) Uani 1 1 d . . . H26A H 0.5990 0.3512 0.5107 0.044 Uiso 1 1 calc R . . C27 C 0.7652(4) 0.39191(19) 0.49781(10) 0.0397(11) Uani 1 1 d . . . H27A H 0.8202 0.3639 0.4905 0.048 Uiso 1 1 calc R . . C28 C 0.7922(4) 0.44780(19) 0.49928(10) 0.0386(11) Uani 1 1 d . . . H28A H 0.8684 0.4642 0.4929 0.046 Uiso 1 1 calc R . . C29 C 0.6856(4) 0.47541(17) 0.51204(11) 0.0378(10) Uani 1 1 d . . . H29A H 0.6781 0.5134 0.5159 0.045 Uiso 1 1 calc R . . C30 C 0.5925(4) 0.43622(17) 0.51802(11) 0.0348(10) Uani 1 1 d . . . H30A H 0.5113 0.4433 0.5265 0.042 Uiso 1 1 calc R . . Fe4 Fe 0.66435(5) 0.17456(2) 0.520788(14) 0.02443(13) Uani 1 1 d . . . C31 C 0.6274(3) 0.24343(14) 0.55031(9) 0.0229(8) Uani 1 1 d . . . C32 C 0.5195(4) 0.22551(16) 0.53112(10) 0.0296(9) Uani 1 1 d . . . H32A H 0.4428 0.2161 0.5419 0.035 Uiso 1 1 calc R . . C33 C 0.5473(4) 0.22435(17) 0.49308(10) 0.0347(10) Uani 1 1 d . . . H33A H 0.4924 0.2138 0.4741 0.042 Uiso 1 1 calc R . . C34 C 0.6700(4) 0.24147(16) 0.48821(10) 0.0331(10) Uani 1 1 d . . . H34A H 0.7120 0.2447 0.4655 0.040 Uiso 1 1 calc R . . C35 C 0.7192(4) 0.25290(15) 0.52313(10) 0.0285(9) Uani 1 1 d . . . H35A H 0.8008 0.2650 0.5278 0.034 Uiso 1 1 calc R . . C36 C 0.7313(4) 0.11612(17) 0.55570(11) 0.0376(10) Uani 1 1 d . . . H36A H 0.7464 0.1201 0.5812 0.045 Uiso 1 1 calc R . . C37 C 0.6197(4) 0.09875(17) 0.53952(12) 0.0417(11) Uani 1 1 d . . . H37A H 0.5465 0.0891 0.5522 0.050 Uiso 1 1 calc R . . C38 C 0.6369(5) 0.09840(17) 0.50083(12) 0.0443(12) Uani 1 1 d . . . H38A H 0.5771 0.0881 0.4831 0.053 Uiso 1 1 calc R . . C39 C 0.7582(4) 0.11598(17) 0.49328(11) 0.0393(11) Uani 1 1 d . . . H39A H 0.7940 0.1200 0.4697 0.047 Uiso 1 1 calc R . . C40 C 0.8165(4) 0.12647(17) 0.52717(11) 0.0372(10) Uani 1 1 d . . . H40A H 0.8990 0.1384 0.5303 0.045 Uiso 1 1 calc R . . Fe5 Fe 0.54092(5) 0.11485(2) 0.695913(14) 0.02712(13) Uani 1 1 d . . . C41 C 0.5863(3) 0.15821(15) 0.64970(10) 0.0255(8) Uani 1 1 d . . . C42 C 0.5797(4) 0.10119(16) 0.64227(10) 0.0333(10) Uani 1 1 d . . . H42A H 0.5262 0.0845 0.6250 0.040 Uiso 1 1 calc R . . C43 C 0.6659(4) 0.07378(17) 0.66470(11) 0.0398(11) Uani 1 1 d . . . H43A H 0.6804 0.0357 0.6651 0.048 Uiso 1 1 calc R . . C44 C 0.7261(4) 0.11282(18) 0.68635(12) 0.0390(11) Uani 1 1 d . . . H44A H 0.7885 0.1057 0.7039 0.047 Uiso 1 1 calc R . . C45 C 0.6779(3) 0.16459(17) 0.67745(11) 0.0317(9) Uani 1 1 d . . . H45A H 0.7025 0.1980 0.6882 0.038 Uiso 1 1 calc R . . C46 C 0.3738(4) 0.13857(19) 0.71665(11) 0.0395(10) Uani 1 1 d . . . H46A H 0.3198 0.1648 0.7064 0.047 Uiso 1 1 calc R . . C47 C 0.3730(4) 0.0824(2) 0.70910(13) 0.0486(12) Uani 1 1 d . . . H47A H 0.3191 0.0641 0.6927 0.058 Uiso 1 1 calc R . . C48 C 0.4680(5) 0.05815(19) 0.73050(13) 0.0508(13) Uani 1 1 d . . . H48A H 0.4881 0.0206 0.7312 0.061 Uiso 1 1 calc R . . C49 C 0.5265(5) 0.0995(2) 0.75039(12) 0.0491(12) Uani 1 1 d . . . H49A H 0.5939 0.0949 0.7667 0.059 Uiso 1 1 calc R . . C50 C 0.4680(4) 0.14902(19) 0.74198(10) 0.0419(11) Uani 1 1 d . . . H50A H 0.4888 0.1836 0.7518 0.050 Uiso 1 1 calc R . . C1S C 0.6821(5) 0.53973(19) 0.3682(3) 0.150(5) Uani 1 1 d G . . H1SA H 0.7324 0.5702 0.3628 0.180 Uiso 1 1 calc R . . C2S C 0.6116(7) 0.5159(3) 0.34084(16) 0.118(4) Uani 1 1 d G . . H2SA H 0.6136 0.5301 0.3167 0.142 Uiso 1 1 calc R . . C3S C 0.5380(5) 0.4712(3) 0.34885(15) 0.097(3) Uani 1 1 d G . . H3SA H 0.4898 0.4549 0.3301 0.117 Uiso 1 1 calc R . . C4S C 0.5350(5) 0.45044(17) 0.3843(2) 0.097(3) Uani 1 1 d G . . H4SA H 0.4847 0.4199 0.3897 0.116 Uiso 1 1 calc R . . C5S C 0.6056(7) 0.4743(3) 0.41164(11) 0.121(4) Uani 1 1 d G . . H5SA H 0.6035 0.4601 0.4358 0.145 Uiso 1 1 calc R . . C6S C 0.6791(5) 0.5190(3) 0.4036(2) 0.148(5) Uani 1 1 d G . . H6SA H 0.7274 0.5353 0.4224 0.178 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 P1 0.0191(5) 0.0282(5) 0.0173(4) 0.0004(4) 0.0011(4) 0.0008(4) P2 0.0201(5) 0.0262(5) 0.0192(4) -0.0023(4) 0.0002(4) 0.0008(4) P3 0.0209(5) 0.0259(5) 0.0186(5) -0.0003(4) -0.0007(4) 0.0008(4) P4 0.0202(5) 0.0258(5) 0.0178(4) -0.0004(4) 0.0004(4) 0.0006(4) P5 0.0233(5) 0.0256(5) 0.0204(5) -0.0011(4) 0.0021(4) -0.0001(4) Fe1 0.0205(3) 0.0280(3) 0.0215(3) -0.0001(2) -0.0011(2) -0.0017(2) C1 0.0189(18) 0.027(2) 0.0199(18) -0.0009(16) -0.0026(15) -0.0025(16) C2 0.024(2) 0.028(2) 0.0212(18) 0.0008(16) 0.0007(15) -0.0006(17) C3 0.026(2) 0.030(2) 0.0225(19) 0.0040(16) -0.0069(16) -0.0010(17) C4 0.0217(19) 0.030(2) 0.033(2) -0.0079(18) -0.0038(16) 0.0031(18) C5 0.0187(18) 0.032(2) 0.0230(18) -0.0040(17) 0.0000(15) -0.0003(16) C6 0.030(2) 0.024(2) 0.044(2) 0.0025(19) -0.0025(18) -0.0009(18) C7 0.044(3) 0.030(2) 0.032(2) -0.0053(18) 0.0084(19) -0.008(2) C8 0.045(3) 0.033(2) 0.037(2) -0.002(2) -0.017(2) -0.010(2) C9 0.021(2) 0.032(2) 0.056(3) -0.005(2) 0.0036(19) -0.0058(18) C10 0.034(2) 0.035(2) 0.032(2) 0.0035(19) 0.0048(18) -0.0110(19) Fe2 0.0238(3) 0.0263(3) 0.0210(3) -0.0014(2) -0.0037(2) -0.0015(2) C11 0.0220(19) 0.0242(19) 0.0183(17) -0.0018(15) -0.0035(15) -0.0033(16) C12 0.026(2) 0.029(2) 0.0213(18) 0.0024(16) 0.0002(16) -0.0028(17) C13 0.031(2) 0.029(2) 0.0220(18) 0.0033(17) -0.0044(16) -0.0030(18) C14 0.0209(19) 0.027(2) 0.029(2) -0.0016(16) -0.0077(16) 0.0014(16) C15 0.0230(19) 0.028(2) 0.0202(18) -0.0038(16) -0.0006(15) -0.0022(17) C16 0.040(3) 0.027(2) 0.062(3) 0.000(2) -0.018(2) 0.001(2) C17 0.049(3) 0.035(3) 0.052(3) -0.018(2) 0.017(2) -0.010(2) C18 0.055(3) 0.034(2) 0.032(2) -0.005(2) -0.018(2) -0.012(2) C19 0.031(2) 0.032(2) 0.047(3) -0.008(2) -0.002(2) -0.0106(19) C20 0.057(3) 0.027(2) 0.033(2) 0.0021(19) -0.005(2) -0.011(2) Fe3 0.0265(3) 0.0264(3) 0.0200(3) 0.0025(2) -0.0016(2) -0.0004(2) C21 0.0229(19) 0.028(2) 0.0179(17) 0.0017(16) -0.0012(15) -0.0007(17) C22 0.026(2) 0.030(2) 0.0194(18) -0.0006(16) -0.0033(15) 0.0004(17) C23 0.029(2) 0.043(2) 0.025(2) 0.0012(19) -0.0023(17) -0.008(2) C24 0.044(2) 0.033(2) 0.0224(19) -0.0008(18) -0.0050(18) -0.011(2) C25 0.036(2) 0.030(2) 0.0201(18) -0.0012(17) 0.0012(17) 0.0026(19) C26 0.049(3) 0.030(2) 0.031(2) 0.0002(19) -0.017(2) -0.001(2) C27 0.054(3) 0.045(3) 0.019(2) -0.0025(19) -0.002(2) 0.010(2) C28 0.041(3) 0.052(3) 0.022(2) 0.010(2) 0.0030(19) -0.004(2) C29 0.055(3) 0.027(2) 0.031(2) 0.0065(18) -0.012(2) 0.003(2) C30 0.035(2) 0.038(2) 0.032(2) 0.0024(19) -0.0125(19) 0.004(2) Fe4 0.0248(3) 0.0282(3) 0.0203(3) -0.0034(2) 0.0012(2) 0.0018(2) C31 0.0243(19) 0.024(2) 0.0205(17) 0.0003(16) 0.0017(15) 0.0058(16) C32 0.023(2) 0.043(2) 0.0234(19) -0.0065(18) 0.0009(16) 0.0050(18) C33 0.036(2) 0.047(3) 0.0210(19) -0.0050(18) -0.0064(18) 0.014(2) C34 0.046(3) 0.034(2) 0.0202(19) 0.0022(17) 0.0031(18) 0.006(2) C35 0.034(2) 0.026(2) 0.0256(19) -0.0040(17) 0.0072(17) -0.0006(18) C36 0.049(3) 0.037(2) 0.027(2) 0.0003(19) -0.003(2) 0.009(2) C37 0.052(3) 0.029(2) 0.043(3) 0.006(2) 0.001(2) -0.005(2) C38 0.062(3) 0.031(2) 0.040(3) -0.012(2) -0.009(2) -0.003(2) C39 0.054(3) 0.033(2) 0.031(2) -0.0066(19) 0.004(2) 0.014(2) C40 0.034(2) 0.036(2) 0.041(2) -0.003(2) -0.003(2) 0.014(2) Fe5 0.0330(3) 0.0260(3) 0.0223(3) 0.0023(2) 0.0023(2) 0.0002(3) C41 0.026(2) 0.028(2) 0.0225(18) -0.0011(16) 0.0060(16) 0.0014(17) C42 0.049(3) 0.029(2) 0.0217(19) -0.0034(17) 0.0060(19) 0.001(2) C43 0.055(3) 0.027(2) 0.037(2) 0.0081(19) 0.014(2) 0.016(2) C44 0.031(2) 0.046(3) 0.040(2) 0.012(2) 0.0011(19) 0.008(2) C45 0.024(2) 0.031(2) 0.040(2) 0.0059(19) -0.0009(18) -0.0029(18) C46 0.037(2) 0.048(3) 0.033(2) 0.010(2) 0.011(2) 0.005(2) C47 0.042(3) 0.053(3) 0.051(3) 0.002(2) 0.014(2) -0.015(2) C48 0.066(3) 0.034(3) 0.052(3) 0.016(2) 0.028(3) 0.003(3) C49 0.057(3) 0.065(3) 0.026(2) 0.011(2) 0.006(2) 0.012(3) C50 0.056(3) 0.047(3) 0.023(2) -0.006(2) 0.007(2) 0.003(2) C1S 0.106(8) 0.073(6) 0.271(16) 0.022(9) 0.039(10) 0.010(5) C2S 0.131(8) 0.133(8) 0.091(6) 0.060(6) 0.056(6) 0.081(6) C3S 0.105(6) 0.118(6) 0.069(5) -0.036(4) -0.012(4) 0.062(5) C4S 0.111(6) 0.047(4) 0.133(6) 0.012(4) 0.045(5) 0.045(4) C5S 0.162(9) 0.156(9) 0.045(4) -0.012(5) -0.010(5) 0.099(7) C6S 0.115(8) 0.135(10) 0.196(12) -0.092(8) -0.048(8) 0.034(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 P1 C1 1.817(4) . ? P1 P2 2.2087(13) . ? P1 P5 2.2187(13) . ? P2 C11 1.816(4) . ? P2 P3 2.1998(13) . ? P3 C21 1.827(4) . ? P3 P4 2.2334(13) . ? P4 C31 1.821(4) . ? P4 P5 2.2309(13) . ? P5 C41 1.815(4) . ? Fe1 C7 2.042(4) . ? Fe1 C5 2.043(4) . ? Fe1 C2 2.044(4) . ? Fe1 C1 2.047(4) . ? Fe1 C6 2.048(4) . ? Fe1 C8 2.048(4) . ? Fe1 C9 2.050(4) . ? Fe1 C3 2.056(4) . ? Fe1 C10 2.057(4) . ? Fe1 C4 2.060(4) . ? C1 C2 1.431(5) . ? C1 C5 1.435(5) . ? C2 C3 1.418(5) . ? C2 H2A 0.9500 . ? C3 C4 1.418(5) . ? C3 H3A 0.9500 . ? C4 C5 1.416(5) . ? C4 H4A 0.9500 . ? C5 H5A 0.9500 . ? C6 C7 1.401(5) . ? C6 C10 1.406(5) . ? C6 H6A 0.9500 . ? C7 C8 1.410(6) . ? C7 H7A 0.9500 . ? C8 C9 1.411(6) . ? C8 H8A 0.9500 . ? C9 C10 1.411(6) . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? Fe2 C15 2.033(3) . ? Fe2 C20 2.034(4) . ? Fe2 C19 2.039(4) . ? Fe2 C18 2.042(4) . ? Fe2 C14 2.043(4) . ? Fe2 C16 2.045(4) . ? Fe2 C12 2.047(4) . ? Fe2 C17 2.048(4) . ? Fe2 C13 2.053(4) . ? Fe2 C11 2.058(3) . ? C11 C15 1.432(5) . ? C11 C12 1.441(5) . ? C12 C13 1.424(5) . ? C12 H12A 0.9500 . ? C13 C14 1.418(5) . ? C13 H13A 0.9500 . ? C14 C15 1.417(5) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 C20 1.398(6) . ? C16 C17 1.419(6) . ? C16 H16A 0.9500 . ? C17 C18 1.413(6) . ? C17 H17A 0.9500 . ? C18 C19 1.403(6) . ? C18 H18A 0.9500 . ? C19 C20 1.397(6) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? Fe3 C25 2.030(4) . ? Fe3 C24 2.039(4) . ? Fe3 C29 2.043(4) . ? Fe3 C30 2.046(4) . ? Fe3 C23 2.046(4) . ? Fe3 C26 2.048(4) . ? Fe3 C27 2.050(4) . ? Fe3 C28 2.052(4) . ? Fe3 C21 2.053(3) . ? Fe3 C22 2.053(4) . ? C21 C25 1.424(5) . ? C21 C22 1.434(5) . ? C22 C23 1.416(5) . ? C22 H22A 0.9500 . ? C23 C24 1.417(6) . ? C23 H23A 0.9500 . ? C24 C25 1.420(5) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? C26 C30 1.410(6) . ? C26 C27 1.416(6) . ? C26 H26A 0.9500 . ? C27 C28 1.408(6) . ? C27 H27A 0.9500 . ? C28 C29 1.421(6) . ? C28 H28A 0.9500 . ? C29 C30 1.414(6) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? Fe4 C35 2.021(4) . ? Fe4 C39 2.031(4) . ? Fe4 C34 2.033(4) . ? Fe4 C38 2.034(4) . ? Fe4 C33 2.035(4) . ? Fe4 C40 2.046(4) . ? Fe4 C37 2.046(4) . ? Fe4 C32 2.047(4) . ? Fe4 C31 2.049(4) . ? Fe4 C36 2.055(4) . ? C31 C35 1.426(5) . ? C31 C32 1.435(5) . ? C32 C33 1.421(5) . ? C32 H32A 0.9500 . ? C33 C34 1.408(6) . ? C33 H33A 0.9500 . ? C34 C35 1.410(5) . ? C34 H34A 0.9500 . ? C35 H35A 0.9500 . ? C36 C37 1.414(6) . ? C36 C40 1.416(6) . ? C36 H36A 0.9500 . ? C37 C38 1.424(6) . ? C37 H37A 0.9500 . ? C38 C39 1.413(6) . ? C38 H38A 0.9500 . ? C39 C40 1.414(6) . ? C39 H39A 0.9500 . ? C40 H40A 0.9500 . ? Fe5 C49 2.030(4) . ? Fe5 C42 2.031(4) . ? Fe5 C43 2.040(4) . ? Fe5 C50 2.040(4) . ? Fe5 C45 2.041(4) . ? Fe5 C44 2.042(4) . ? Fe5 C48 2.042(4) . ? Fe5 C47 2.048(4) . ? Fe5 C46 2.051(4) . ? Fe5 C41 2.056(4) . ? C41 C45 1.429(5) . ? C41 C42 1.432(5) . ? C42 C43 1.414(6) . ? C42 H42A 0.9500 . ? C43 C44 1.406(6) . ? C43 H43A 0.9500 . ? C44 C45 1.416(5) . ? C44 H44A 0.9500 . ? C45 H45A 0.9500 . ? C46 C50 1.403(6) . ? C46 C47 1.410(6) . ? C46 H46A 0.9500 . ? C47 C48 1.425(7) . ? C47 H47A 0.9500 . ? C48 C49 1.403(7) . ? C48 H48A 0.9500 . ? C49 C50 1.409(6) . ? C49 H49A 0.9500 . ? C50 H50A 0.9500 . ? C1S C2S 1.3900 . ? C1S C6S 1.3900 . ? C1S H1SA 0.9500 . ? C2S C3S 1.3900 . ? C2S H2SA 0.9500 . ? C3S C4S 1.3900 . ? C3S H3SA 0.9500 . ? C4S C5S 1.3900 . ? C4S H4SA 0.9500 . ? C5S C6S 1.3900 . ? C5S H5SA 0.9500 . ? C6S H6SA 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 P1 P2 97.67(12) . . ? C1 P1 P5 100.79(12) . . ? P2 P1 P5 107.94(5) . . ? C11 P2 P3 109.89(12) . . ? C11 P2 P1 98.18(12) . . ? P3 P2 P1 95.19(5) . . ? C21 P3 P2 103.12(12) . . ? C21 P3 P4 103.77(12) . . ? P2 P3 P4 100.87(5) . . ? C31 P4 P5 100.03(12) . . ? C31 P4 P3 97.63(12) . . ? P5 P4 P3 96.18(5) . . ? C41 P5 P1 102.48(12) . . ? C41 P5 P4 98.66(13) . . ? P1 P5 P4 103.42(5) . . ? C7 Fe1 C5 160.68(16) . . ? C7 Fe1 C2 107.02(15) . . ? C5 Fe1 C2 68.35(14) . . ? C7 Fe1 C1 123.18(16) . . ? C5 Fe1 C1 41.08(14) . . ? C2 Fe1 C1 40.95(13) . . ? C7 Fe1 C6 40.06(15) . . ? C5 Fe1 C6 125.11(15) . . ? C2 Fe1 C6 121.65(16) . . ? C1 Fe1 C6 107.48(15) . . ? C7 Fe1 C8 40.33(17) . . ? C5 Fe1 C8 157.83(16) . . ? C2 Fe1 C8 123.56(16) . . ? C1 Fe1 C8 159.76(16) . . ? C6 Fe1 C8 67.39(17) . . ? C7 Fe1 C9 67.62(17) . . ? C5 Fe1 C9 122.92(16) . . ? C2 Fe1 C9 160.47(16) . . ? C1 Fe1 C9 157.81(16) . . ? C6 Fe1 C9 67.20(16) . . ? C8 Fe1 C9 40.28(16) . . ? C7 Fe1 C3 121.34(15) . . ? C5 Fe1 C3 68.13(15) . . ? C2 Fe1 C3 40.46(14) . . ? C1 Fe1 C3 68.77(14) . . ? C6 Fe1 C3 156.65(16) . . ? C8 Fe1 C3 107.71(16) . . ? C9 Fe1 C3 124.85(16) . . ? C7 Fe1 C10 67.68(16) . . ? C5 Fe1 C10 108.86(16) . . ? C2 Fe1 C10 157.15(16) . . ? C1 Fe1 C10 121.85(15) . . ? C6 Fe1 C10 40.05(15) . . ? C8 Fe1 C10 67.75(17) . . ? C9 Fe1 C10 40.18(16) . . ? C3 Fe1 C10 161.47(16) . . ? C7 Fe1 C4 157.07(16) . . ? C5 Fe1 C4 40.36(14) . . ? C2 Fe1 C4 67.88(15) . . ? C1 Fe1 C4 68.60(15) . . ? C6 Fe1 C4 161.74(16) . . ? C8 Fe1 C4 122.44(16) . . ? C9 Fe1 C4 109.28(16) . . ? C3 Fe1 C4 40.29(14) . . ? C10 Fe1 C4 125.66(16) . . ? C2 C1 C5 106.5(3) . . ? C2 C1 P1 131.1(3) . . ? C5 C1 P1 122.4(3) . . ? C2 C1 Fe1 69.4(2) . . ? C5 C1 Fe1 69.3(2) . . ? P1 C1 Fe1 126.5(2) . . ? C3 C2 C1 108.8(3) . . ? C3 C2 Fe1 70.2(2) . . ? C1 C2 Fe1 69.6(2) . . ? C3 C2 H2A 125.6 . . ? C1 C2 H2A 125.6 . . ? Fe1 C2 H2A 126.2 . . ? C4 C3 C2 107.8(3) . . ? C4 C3 Fe1 70.0(2) . . ? C2 C3 Fe1 69.3(2) . . ? C4 C3 H3A 126.1 . . ? C2 C3 H3A 126.1 . . ? Fe1 C3 H3A 126.2 . . ? C5 C4 C3 108.3(3) . . ? C5 C4 Fe1 69.2(2) . . ? C3 C4 Fe1 69.7(2) . . ? C5 C4 H4A 125.9 . . ? C3 C4 H4A 125.9 . . ? Fe1 C4 H4A 126.8 . . ? C4 C5 C1 108.5(3) . . ? C4 C5 Fe1 70.5(2) . . ? C1 C5 Fe1 69.6(2) . . ? C4 C5 H5A 125.7 . . ? C1 C5 H5A 125.7 . . ? Fe1 C5 H5A 125.8 . . ? C7 C6 C10 108.9(4) . . ? C7 C6 Fe1 69.8(2) . . ? C10 C6 Fe1 70.3(2) . . ? C7 C6 H6A 125.6 . . ? C10 C6 H6A 125.6 . . ? Fe1 C6 H6A 125.9 . . ? C6 C7 C8 107.9(4) . . ? C6 C7 Fe1 70.2(2) . . ? C8 C7 Fe1 70.1(2) . . ? C6 C7 H7A 126.1 . . ? C8 C7 H7A 126.1 . . ? Fe1 C7 H7A 125.3 . . ? C7 C8 C9 107.6(4) . . ? C7 C8 Fe1 69.6(2) . . ? C9 C8 Fe1 69.9(2) . . ? C7 C8 H8A 126.2 . . ? C9 C8 H8A 126.2 . . ? Fe1 C8 H8A 125.8 . . ? C10 C9 C8 108.4(4) . . ? C10 C9 Fe1 70.2(2) . . ? C8 C9 Fe1 69.8(2) . . ? C10 C9 H9A 125.8 . . ? C8 C9 H9A 125.8 . . ? Fe1 C9 H9A 125.8 . . ? C6 C10 C9 107.3(4) . . ? C6 C10 Fe1 69.6(2) . . ? C9 C10 Fe1 69.7(2) . . ? C6 C10 H10A 126.4 . . ? C9 C10 H10A 126.4 . . ? Fe1 C10 H10A 125.9 . . ? C15 Fe2 C20 106.11(16) . . ? C15 Fe2 C19 118.15(16) . . ? C20 Fe2 C19 40.11(17) . . ? C15 Fe2 C18 153.16(17) . . ? C20 Fe2 C18 67.65(17) . . ? C19 Fe2 C18 40.23(17) . . ? C15 Fe2 C14 40.68(14) . . ? C20 Fe2 C14 124.52(17) . . ? C19 Fe2 C14 106.79(16) . . ? C18 Fe2 C14 119.82(17) . . ? C15 Fe2 C16 125.04(17) . . ? C20 Fe2 C16 40.08(18) . . ? C19 Fe2 C16 67.56(18) . . ? C18 Fe2 C16 67.98(17) . . ? C14 Fe2 C16 161.66(17) . . ? C15 Fe2 C12 68.59(15) . . ? C20 Fe2 C12 154.89(17) . . ? C19 Fe2 C12 164.34(16) . . ? C18 Fe2 C12 128.05(17) . . ? C14 Fe2 C12 68.36(15) . . ? C16 Fe2 C12 121.65(17) . . ? C15 Fe2 C17 163.54(18) . . ? C20 Fe2 C17 67.70(18) . . ? C19 Fe2 C17 67.69(18) . . ? C18 Fe2 C17 40.43(18) . . ? C14 Fe2 C17 155.38(18) . . ? C16 Fe2 C17 40.58(18) . . ? C12 Fe2 C17 110.11(17) . . ? C15 Fe2 C13 68.41(15) . . ? C20 Fe2 C13 162.22(18) . . ? C19 Fe2 C13 126.19(17) . . ? C18 Fe2 C13 109.13(16) . . ? C14 Fe2 C13 40.51(14) . . ? C16 Fe2 C13 156.70(18) . . ? C12 Fe2 C13 40.65(14) . . ? C17 Fe2 C13 122.07(17) . . ? C15 Fe2 C11 40.97(14) . . ? C20 Fe2 C11 118.79(16) . . ? C19 Fe2 C11 152.74(16) . . ? C18 Fe2 C11 165.24(17) . . ? C14 Fe2 C11 68.87(14) . . ? C16 Fe2 C11 107.66(16) . . ? C12 Fe2 C11 41.10(13) . . ? C17 Fe2 C11 127.24(17) . . ? C13 Fe2 C11 68.93(14) . . ? C15 C11 C12 106.3(3) . . ? C15 C11 P2 130.9(3) . . ? C12 C11 P2 122.8(3) . . ? C15 C11 Fe2 68.58(19) . . ? C12 C11 Fe2 69.0(2) . . ? P2 C11 Fe2 125.55(19) . . ? C13 C12 C11 108.6(3) . . ? C13 C12 Fe2 69.9(2) . . ? C11 C12 Fe2 69.9(2) . . ? C13 C12 H12A 125.7 . . ? C11 C12 H12A 125.7 . . ? Fe2 C12 H12A 126.1 . . ? C14 C13 C12 107.9(3) . . ? C14 C13 Fe2 69.4(2) . . ? C12 C13 Fe2 69.5(2) . . ? C14 C13 H13A 126.0 . . ? C12 C13 H13A 126.0 . . ? Fe2 C13 H13A 126.7 . . ? C15 C14 C13 108.2(3) . . ? C15 C14 Fe2 69.3(2) . . ? C13 C14 Fe2 70.1(2) . . ? C15 C14 H14A 125.9 . . ? C13 C14 H14A 125.9 . . ? Fe2 C14 H14A 126.3 . . ? C14 C15 C11 109.0(3) . . ? C14 C15 Fe2 70.0(2) . . ? C11 C15 Fe2 70.4(2) . . ? C14 C15 H15A 125.5 . . ? C11 C15 H15A 125.5 . . ? Fe2 C15 H15A 125.6 . . ? C20 C16 C17 107.7(4) . . ? C20 C16 Fe2 69.6(2) . . ? C17 C16 Fe2 69.8(2) . . ? C20 C16 H16A 126.2 . . ? C17 C16 H16A 126.2 . . ? Fe2 C16 H16A 126.0 . . ? C18 C17 C16 107.5(4) . . ? C18 C17 Fe2 69.6(2) . . ? C16 C17 Fe2 69.6(2) . . ? C18 C17 H17A 126.2 . . ? C16 C17 H17A 126.2 . . ? Fe2 C17 H17A 126.2 . . ? C19 C18 C17 107.8(4) . . ? C19 C18 Fe2 69.8(2) . . ? C17 C18 Fe2 70.0(2) . . ? C19 C18 H18A 126.1 . . ? C17 C18 H18A 126.1 . . ? Fe2 C18 H18A 125.7 . . ? C20 C19 C18 108.3(4) . . ? C20 C19 Fe2 69.8(2) . . ? C18 C19 Fe2 70.0(2) . . ? C20 C19 H19A 125.9 . . ? C18 C19 H19A 125.9 . . ? Fe2 C19 H19A 125.9 . . ? C19 C20 C16 108.7(4) . . ? C19 C20 Fe2 70.1(2) . . ? C16 C20 Fe2 70.4(3) . . ? C19 C20 H20A 125.7 . . ? C16 C20 H20A 125.7 . . ? Fe2 C20 H20A 125.5 . . ? C25 Fe3 C24 40.83(15) . . ? C25 Fe3 C29 114.08(17) . . ? C24 Fe3 C29 106.49(17) . . ? C25 Fe3 C30 106.25(17) . . ? C24 Fe3 C30 128.03(17) . . ? C29 Fe3 C30 40.47(16) . . ? C25 Fe3 C23 68.42(16) . . ? C24 Fe3 C23 40.59(16) . . ? C29 Fe3 C23 129.86(17) . . ? C30 Fe3 C23 167.29(17) . . ? C25 Fe3 C26 129.44(18) . . ? C24 Fe3 C26 167.06(18) . . ? C29 Fe3 C26 67.85(17) . . ? C30 Fe3 C26 40.29(16) . . ? C23 Fe3 C26 151.73(17) . . ? C25 Fe3 C27 169.20(18) . . ? C24 Fe3 C27 149.87(18) . . ? C29 Fe3 C27 68.06(17) . . ? C30 Fe3 C27 68.05(18) . . ? C23 Fe3 C27 119.05(18) . . ? C26 Fe3 C27 40.44(17) . . ? C25 Fe3 C28 147.68(17) . . ? C24 Fe3 C28 116.25(17) . . ? C29 Fe3 C28 40.63(17) . . ? C30 Fe3 C28 68.01(17) . . ? C23 Fe3 C28 109.88(17) . . ? C26 Fe3 C28 67.66(18) . . ? C27 Fe3 C28 40.15(17) . . ? C25 Fe3 C21 40.82(14) . . ? C24 Fe3 C21 68.69(15) . . ? C29 Fe3 C21 147.24(17) . . ? C30 Fe3 C21 115.64(16) . . ? C23 Fe3 C21 68.46(15) . . ? C26 Fe3 C21 109.31(16) . . ? C27 Fe3 C21 132.16(17) . . ? C28 Fe3 C21 170.99(17) . . ? C25 Fe3 C22 68.55(15) . . ? C24 Fe3 C22 68.37(16) . . ? C29 Fe3 C22 169.45(17) . . ? C30 Fe3 C22 149.89(16) . . ? C23 Fe3 C22 40.43(15) . . ? C26 Fe3 C22 119.10(16) . . ? C27 Fe3 C22 111.41(16) . . ? C28 Fe3 C22 132.28(16) . . ? C21 Fe3 C22 40.87(14) . . ? C25 C21 C22 107.2(3) . . ? C25 C21 P3 121.3(3) . . ? C22 C21 P3 131.3(3) . . ? C25 C21 Fe3 68.7(2) . . ? C22 C21 Fe3 69.6(2) . . ? P3 C21 Fe3 122.65(18) . . ? C23 C22 C21 108.0(3) . . ? C23 C22 Fe3 69.5(2) . . ? C21 C22 Fe3 69.5(2) . . ? C23 C22 H22A 126.0 . . ? C21 C22 H22A 126.0 . . ? Fe3 C22 H22A 126.5 . . ? C22 C23 C24 108.5(4) . . ? C22 C23 Fe3 70.1(2) . . ? C24 C23 Fe3 69.5(2) . . ? C22 C23 H23A 125.8 . . ? C24 C23 H23A 125.8 . . ? Fe3 C23 H23A 126.3 . . ? C23 C24 C25 107.8(4) . . ? C23 C24 Fe3 70.0(2) . . ? C25 C24 Fe3 69.2(2) . . ? C23 C24 H24A 126.1 . . ? C25 C24 H24A 126.1 . . ? Fe3 C24 H24A 126.3 . . ? C24 C25 C21 108.6(3) . . ? C24 C25 Fe3 69.9(2) . . ? C21 C25 Fe3 70.5(2) . . ? C24 C25 H25A 125.7 . . ? C21 C25 H25A 125.7 . . ? Fe3 C25 H25A 125.5 . . ? C30 C26 C27 108.4(4) . . ? C30 C26 Fe3 69.8(2) . . ? C27 C26 Fe3 69.9(2) . . ? C30 C26 H26A 125.8 . . ? C27 C26 H26A 125.8 . . ? Fe3 C26 H26A 126.1 . . ? C28 C27 C26 107.8(4) . . ? C28 C27 Fe3 70.0(2) . . ? C26 C27 Fe3 69.7(2) . . ? C28 C27 H27A 126.1 . . ? C26 C27 H27A 126.1 . . ? Fe3 C27 H27A 125.8 . . ? C27 C28 C29 108.1(4) . . ? C27 C28 Fe3 69.8(2) . . ? C29 C28 Fe3 69.3(2) . . ? C27 C28 H28A 126.0 . . ? C29 C28 H28A 126.0 . . ? Fe3 C28 H28A 126.4 . . ? C30 C29 C28 107.8(4) . . ? C30 C29 Fe3 69.9(2) . . ? C28 C29 Fe3 70.0(2) . . ? C30 C29 H29A 126.1 . . ? C28 C29 H29A 126.1 . . ? Fe3 C29 H29A 125.6 . . ? C26 C30 C29 107.9(4) . . ? C26 C30 Fe3 69.9(2) . . ? C29 C30 Fe3 69.6(2) . . ? C26 C30 H30A 126.1 . . ? C29 C30 H30A 126.1 . . ? Fe3 C30 H30A 125.9 . . ? C35 Fe4 C39 123.42(17) . . ? C35 Fe4 C34 40.72(15) . . ? C39 Fe4 C34 105.74(17) . . ? C35 Fe4 C38 159.81(17) . . ? C39 Fe4 C38 40.69(18) . . ? C34 Fe4 C38 122.84(17) . . ? C35 Fe4 C33 68.29(17) . . ? C39 Fe4 C33 119.69(16) . . ? C34 Fe4 C33 40.51(16) . . ? C38 Fe4 C33 106.62(18) . . ? C35 Fe4 C40 108.03(17) . . ? C39 Fe4 C40 40.57(16) . . ? C34 Fe4 C40 120.76(17) . . ? C38 Fe4 C40 68.00(19) . . ? C33 Fe4 C40 155.45(16) . . ? C35 Fe4 C37 157.91(16) . . ? C39 Fe4 C37 68.67(19) . . ? C34 Fe4 C37 160.38(17) . . ? C38 Fe4 C37 40.86(17) . . ? C33 Fe4 C37 124.59(19) . . ? C40 Fe4 C37 67.99(19) . . ? C35 Fe4 C32 68.53(16) . . ? C39 Fe4 C32 155.72(17) . . ? C34 Fe4 C32 68.55(16) . . ? C38 Fe4 C32 121.22(18) . . ? C33 Fe4 C32 40.75(14) . . ? C40 Fe4 C32 162.60(16) . . ? C37 Fe4 C32 108.38(18) . . ? C35 Fe4 C31 41.02(14) . . ? C39 Fe4 C31 161.06(17) . . ? C34 Fe4 C31 69.07(15) . . ? C38 Fe4 C31 157.34(18) . . ? C33 Fe4 C31 68.93(15) . . ? C40 Fe4 C31 125.26(16) . . ? C37 Fe4 C31 122.20(16) . . ? C32 Fe4 C31 41.02(14) . . ? C35 Fe4 C36 122.55(17) . . ? C39 Fe4 C36 68.41(16) . . ? C34 Fe4 C36 156.88(18) . . ? C38 Fe4 C36 68.17(18) . . ? C33 Fe4 C36 161.98(18) . . ? C40 Fe4 C36 40.41(16) . . ? C37 Fe4 C36 40.34(17) . . ? C32 Fe4 C36 125.91(16) . . ? C31 Fe4 C36 108.82(15) . . ? C35 C31 C32 106.4(3) . . ? C35 C31 P4 121.8(3) . . ? C32 C31 P4 131.8(3) . . ? C35 C31 Fe4 68.4(2) . . ? C32 C31 Fe4 69.4(2) . . ? P4 C31 Fe4 125.56(19) . . ? C33 C32 C31 108.0(3) . . ? C33 C32 Fe4 69.1(2) . . ? C31 C32 Fe4 69.5(2) . . ? C33 C32 H32A 126.0 . . ? C31 C32 H32A 126.0 . . ? Fe4 C32 H32A 126.9 . . ? C34 C33 C32 108.6(4) . . ? C34 C33 Fe4 69.7(2) . . ? C32 C33 Fe4 70.1(2) . . ? C34 C33 H33A 125.7 . . ? C32 C33 H33A 125.7 . . ? Fe4 C33 H33A 126.1 . . ? C33 C34 C35 107.7(3) . . ? C33 C34 Fe4 69.8(2) . . ? C35 C34 Fe4 69.2(2) . . ? C33 C34 H34A 126.1 . . ? C35 C34 H34A 126.1 . . ? Fe4 C34 H34A 126.4 . . ? C34 C35 C31 109.3(3) . . ? C34 C35 Fe4 70.1(2) . . ? C31 C35 Fe4 70.5(2) . . ? C34 C35 H35A 125.3 . . ? C31 C35 H35A 125.3 . . ? Fe4 C35 H35A 125.6 . . ? C37 C36 C40 107.9(4) . . ? C37 C36 Fe4 69.5(2) . . ? C40 C36 Fe4 69.5(2) . . ? C37 C36 H36A 126.1 . . ? C40 C36 H36A 126.1 . . ? Fe4 C36 H36A 126.6 . . ? C36 C37 C38 107.7(4) . . ? C36 C37 Fe4 70.2(2) . . ? C38 C37 Fe4 69.1(2) . . ? C36 C37 H37A 126.2 . . ? C38 C37 H37A 126.2 . . ? Fe4 C37 H37A 126.2 . . ? C39 C38 C37 108.3(4) . . ? C39 C38 Fe4 69.6(2) . . ? C37 C38 Fe4 70.0(2) . . ? C39 C38 H38A 125.9 . . ? C37 C38 H38A 125.9 . . ? Fe4 C38 H38A 126.1 . . ? C40 C39 C38 107.6(4) . . ? C40 C39 Fe4 70.3(2) . . ? C38 C39 Fe4 69.7(2) . . ? C40 C39 H39A 126.2 . . ? C38 C39 H39A 126.2 . . ? Fe4 C39 H39A 125.4 . . ? C39 C40 C36 108.5(4) . . ? C39 C40 Fe4 69.2(2) . . ? C36 C40 Fe4 70.1(2) . . ? C39 C40 H40A 125.7 . . ? C36 C40 H40A 125.7 . . ? Fe4 C40 H40A 126.5 . . ? C49 Fe5 C42 158.35(18) . . ? C49 Fe5 C43 120.39(18) . . ? C42 Fe5 C43 40.67(16) . . ? C49 Fe5 C50 40.51(17) . . ? C42 Fe5 C50 160.64(17) . . ? C43 Fe5 C50 157.36(18) . . ? C49 Fe5 C45 119.42(19) . . ? C42 Fe5 C45 68.28(17) . . ? C43 Fe5 C45 68.19(17) . . ? C50 Fe5 C45 107.91(18) . . ? C49 Fe5 C44 103.81(19) . . ? C42 Fe5 C44 68.09(18) . . ? C43 Fe5 C44 40.30(17) . . ? C50 Fe5 C44 122.24(19) . . ? C45 Fe5 C44 40.58(15) . . ? C49 Fe5 C48 40.30(19) . . ? C42 Fe5 C48 124.27(19) . . ? C43 Fe5 C48 105.31(18) . . ? C50 Fe5 C48 67.79(19) . . ? C45 Fe5 C48 153.75(19) . . ? C44 Fe5 C48 118.09(19) . . ? C49 Fe5 C47 68.2(2) . . ? C42 Fe5 C47 110.28(19) . . ? C43 Fe5 C47 122.01(19) . . ? C50 Fe5 C47 67.75(19) . . ? C45 Fe5 C47 163.81(18) . . ? C44 Fe5 C47 155.17(19) . . ? C48 Fe5 C47 40.78(19) . . ? C49 Fe5 C46 67.88(18) . . ? C42 Fe5 C46 125.90(18) . . ? C43 Fe5 C46 159.33(19) . . ? C50 Fe5 C46 40.09(17) . . ? C45 Fe5 C46 126.57(17) . . ? C44 Fe5 C46 160.31(19) . . ? C48 Fe5 C46 67.88(18) . . ? C47 Fe5 C46 40.23(18) . . ? C49 Fe5 C41 156.74(19) . . ? C42 Fe5 C41 41.01(15) . . ? C43 Fe5 C41 68.90(15) . . ? C50 Fe5 C41 123.71(17) . . ? C45 Fe5 C41 40.81(15) . . ? C44 Fe5 C41 68.69(16) . . ? C48 Fe5 C41 162.75(19) . . ? C47 Fe5 C41 127.48(18) . . ? C46 Fe5 C41 111.52(16) . . ? C45 C41 C42 106.1(3) . . ? C45 C41 P5 131.8(3) . . ? C42 C41 P5 121.8(3) . . ? C45 C41 Fe5 69.0(2) . . ? C42 C41 Fe5 68.6(2) . . ? P5 C41 Fe5 131.7(2) . . ? C43 C42 C41 109.0(4) . . ? C43 C42 Fe5 70.0(2) . . ? C41 C42 Fe5 70.4(2) . . ? C43 C42 H42A 125.5 . . ? C41 C42 H42A 125.5 . . ? Fe5 C42 H42A 125.6 . . ? C44 C43 C42 107.9(4) . . ? C44 C43 Fe5 69.9(2) . . ? C42 C43 Fe5 69.3(2) . . ? C44 C43 H43A 126.1 . . ? C42 C43 H43A 126.1 . . ? Fe5 C43 H43A 126.3 . . ? C43 C44 C45 108.3(4) . . ? C43 C44 Fe5 69.8(2) . . ? C45 C44 Fe5 69.7(2) . . ? C43 C44 H44A 125.8 . . ? C45 C44 H44A 125.8 . . ? Fe5 C44 H44A 126.3 . . ? C44 C45 C41 108.7(4) . . ? C44 C45 Fe5 69.7(2) . . ? C41 C45 Fe5 70.1(2) . . ? C44 C45 H45A 125.6 . . ? C41 C45 H45A 125.6 . . ? Fe5 C45 H45A 126.1 . . ? C50 C46 C47 108.2(4) . . ? C50 C46 Fe5 69.5(2) . . ? C47 C46 Fe5 69.7(3) . . ? C50 C46 H46A 125.9 . . ? C47 C46 H46A 125.9 . . ? Fe5 C46 H46A 126.4 . . ? C46 C47 C48 107.5(4) . . ? C46 C47 Fe5 70.0(2) . . ? C48 C47 Fe5 69.4(3) . . ? C46 C47 H47A 126.3 . . ? C48 C47 H47A 126.3 . . ? Fe5 C47 H47A 125.9 . . ? C49 C48 C47 107.9(4) . . ? C49 C48 Fe5 69.4(3) . . ? C47 C48 Fe5 69.8(2) . . ? C49 C48 H48A 126.1 . . ? C47 C48 H48A 126.1 . . ? Fe5 C48 H48A 126.3 . . ? C48 C49 C50 108.1(4) . . ? C48 C49 Fe5 70.3(3) . . ? C50 C49 Fe5 70.1(2) . . ? C48 C49 H49A 125.9 . . ? C50 C49 H49A 125.9 . . ? Fe5 C49 H49A 125.2 . . ? C46 C50 C49 108.3(4) . . ? C46 C50 Fe5 70.4(2) . . ? C49 C50 Fe5 69.4(2) . . ? C46 C50 H50A 125.9 . . ? C49 C50 H50A 125.9 . . ? Fe5 C50 H50A 126.0 . . ? C2S C1S C6S 120.0 . . ? C2S C1S H1SA 120.0 . . ? C6S C1S H1SA 120.0 . . ? C3S C2S C1S 120.0 . . ? C3S C2S H2SA 120.0 . . ? C1S C2S H2SA 120.0 . . ? C2S C3S C4S 120.0 . . ? C2S C3S H3SA 120.0 . . ? C4S C3S H3SA 120.0 . . ? C5S C4S C3S 120.0 . . ? C5S C4S H4SA 120.0 . . ? C3S C4S H4SA 120.0 . . ? C4S C5S C6S 120.0 . . ? C4S C5S H5SA 120.0 . . ? C6S C5S H5SA 120.0 . . ? C5S C6S C1S 120.0 . . ? C5S C6S H6SA 120.0 . . ? C1S C6S H6SA 120.0 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.907 _refine_diff_density_min -0.624 _refine_diff_density_rms 0.100 data_dw0926 _database_code_depnum_ccdc_archive 'CCDC 768907' #TrackingRef 'compound 7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H48 Cl4 Fe4 P4 Sn4' _chemical_formula_sum 'C52 H48 Cl4 Fe4 P4 Sn4' _chemical_formula_weight 1636.74 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Cmcm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z-1/2' 'x+1/2, -y+1/2, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 18.245(4) _cell_length_b 15.165(3) _cell_length_c 19.997(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5532.8(19) _cell_formula_units_Z 4 _cell_measurement_temperature 260(2) _cell_measurement_reflns_used 31083 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 26.02 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.965 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3168 _exptl_absorpt_coefficient_mu 3.136 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.802 _exptl_absorpt_correction_T_max 0.961 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 260(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 19629 _diffrn_reflns_av_R_equivalents 0.0564 _diffrn_reflns_av_sigmaI/netI 0.0322 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 26.02 _reflns_number_total 2892 _reflns_number_gt 2108 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _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^)+(0.0471P)^2^+15.6539P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2892 _refine_ls_number_parameters 137 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0568 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.1002 _refine_ls_wR_factor_gt 0.0891 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.0000 0.56223(4) 0.2500 0.04122(18) Uani 0.98 4 d SP . . Sn2 Sn 0.0000 0.37199(3) 0.10441(2) 0.04295(15) Uani 0.98 2 d SP . . Sn3 Sn 0.0000 0.18108(4) 0.2500 0.04489(19) Uani 0.98 4 d SP . . Cl1 Cl -0.06671(13) 0.53337(15) 0.12757(12) 0.0524(6) Uani 0.50 1 d P . . Cl2 Cl 0.06712(13) 0.21043(16) 0.12880(13) 0.0580(6) Uani 0.50 1 d P . . P1 P 0.07587(11) 0.42389(13) 0.20925(10) 0.0330(4) Uani 0.50 1 d P . . P2 P -0.07671(11) 0.31989(12) 0.21119(10) 0.0334(4) Uani 0.50 1 d P . . Fe1 Fe 0.21047(6) 0.52867(7) 0.12277(5) 0.0370(3) Uani 0.50 1 d P . -1 C10 C 0.1711(2) 0.4416(4) 0.1908(3) 0.0368(17) Uiso 0.50 1 d PG A -1 C11 C 0.2113(3) 0.3961(4) 0.1407(3) 0.045(2) Uiso 0.50 1 d PG A -1 H11 H 0.1930 0.3524 0.1126 0.054 Uiso 0.50 1 calc PR A -1 C12 C 0.2841(3) 0.4291(4) 0.1409(3) 0.053(2) Uiso 0.50 1 d PG A -1 H12 H 0.3220 0.4107 0.1131 0.064 Uiso 0.50 1 calc PR A -1 C13 C 0.2890(3) 0.4949(4) 0.1912(3) 0.053(2) Uiso 0.50 1 d PG A -1 H13 H 0.3307 0.5273 0.2021 0.063 Uiso 0.50 1 calc PR A -1 C14 C 0.2192(3) 0.5027(3) 0.2220(3) 0.0432(19) Uiso 0.50 1 d PG A -1 H14 H 0.2071 0.5410 0.2566 0.052 Uiso 0.50 1 calc PR A -1 C15 C 0.24734(18) 0.6417(3) 0.0794(2) 0.055(2) Uiso 0.50 1 d PG B -1 H15 H 0.2908 0.6704 0.0903 0.065 Uiso 0.50 1 calc PR B -1 C16 C 0.1778(2) 0.6566(3) 0.1093(3) 0.058(2) Uiso 0.50 1 d PG B -1 H16 H 0.1677 0.6969 0.1431 0.070 Uiso 0.50 1 calc PR B -1 C17 C 0.12644(16) 0.5993(2) 0.0783(2) 0.055(2) Uiso 0.50 1 d PG . -1 H17 H 0.0768 0.5955 0.0884 0.066 Uiso 0.50 1 calc PR B -1 C18 C 0.16422(19) 0.5489(3) 0.0294(2) 0.054(2) Uiso 0.50 1 d PG B -1 H18 H 0.1436 0.5063 0.0018 0.065 Uiso 0.50 1 calc PR B -1 C19 C 0.23894(19) 0.5751(3) 0.0301(3) 0.059(2) Uiso 0.50 1 d PG B -1 H19 H 0.2759 0.5526 0.0030 0.071 Uiso 0.50 1 calc PR B -1 Fe2 Fe -0.21312(6) 0.21446(7) 0.12946(6) 0.0399(3) Uani 0.50 1 d PG . -1 C20 C -0.1720(2) 0.3017(4) 0.1961(3) 0.0374(17) Uiso 0.50 1 d PG C -1 C21 C -0.2147(3) 0.3464(4) 0.1473(3) 0.049(2) Uiso 0.50 1 d PG C -1 H21 H -0.1980 0.3899 0.1183 0.059 Uiso 0.50 1 calc PR C -1 C22 C -0.2873(3) 0.3130(4) 0.1506(3) 0.057(2) Uiso 0.50 1 d PG C -1 H22 H -0.3265 0.3308 0.1242 0.068 Uiso 0.50 1 calc PR C -1 C23 C -0.2895(3) 0.2476(4) 0.2014(3) 0.054(2) Uiso 0.50 1 d PG C -1 H23 H -0.3304 0.2151 0.2141 0.065 Uiso 0.50 1 calc PR C -1 C24 C -0.2182(3) 0.2407(3) 0.2295(2) 0.047(2) Uiso 0.50 1 d PG C -1 H24 H -0.2043 0.2028 0.2638 0.056 Uiso 0.50 1 calc PR C -1 C25 C -0.1755(4) 0.0881(4) 0.1159(3) 0.061(3) Uiso 0.50 1 d PG D -1 H25 H -0.1608 0.0496 0.1495 0.073 Uiso 0.50 1 calc PR D -1 C26 C -0.2476(3) 0.0967(5) 0.0900(4) 0.064(3) Uiso 0.50 1 d PG D -1 H26 H -0.2884 0.0648 0.1037 0.077 Uiso 0.50 1 calc PR D -1 C27 C -0.2464(4) 0.1627(6) 0.0396(4) 0.077(3) Uiso 0.50 1 d PG D -1 H27 H -0.2863 0.1815 0.0145 0.092 Uiso 0.50 1 calc PR D -1 C28 C -0.1735(4) 0.1949(4) 0.0344(3) 0.067(3) Uiso 0.50 1 d PG D -1 H28 H -0.1573 0.2385 0.0052 0.080 Uiso 0.50 1 calc PR D -1 C29 C -0.1297(3) 0.1488(5) 0.0816(4) 0.056(2) Uiso 0.50 1 d PG . -1 H29 H -0.0798 0.1569 0.0887 0.067 Uiso 0.50 1 calc PR D -1 C1X C 0.0145(13) 0.9355(10) 0.3586(10) 0.126(10) Uiso 0.25 1 d PG E -1 H1X H 0.0293 0.9834 0.3329 0.151 Uiso 0.25 1 calc PR E -1 C2X C 0.0274(14) 0.8502(14) 0.3362(7) 0.107(10) Uiso 0.25 1 d PG E -1 H2X H 0.0509 0.8409 0.2955 0.128 Uiso 0.25 1 calc PR E -1 C3X C 0.0052(13) 0.7786(8) 0.3746(9) 0.071(5) Uiso 0.25 1 d PG E -1 H3X H 0.0138 0.7215 0.3596 0.086 Uiso 0.25 1 calc PR E -1 C4X C -0.0299(12) 0.7924(10) 0.4354(9) 0.080(7) Uiso 0.25 1 d PG E -1 H4X H -0.0448 0.7445 0.4611 0.095 Uiso 0.25 1 calc PR E -1 C5X C -0.0429(11) 0.8778(13) 0.4578(8) 0.111(10) Uiso 0.25 1 d PG E -1 H5X H -0.0664 0.8870 0.4985 0.134 Uiso 0.25 1 calc PR E -1 C6X C -0.0207(12) 0.9493(8) 0.4194(11) 0.073(6) Uiso 0.25 1 d PG E -1 H6X H -0.0293 1.0065 0.4343 0.088 Uiso 0.25 1 calc PR E -1 C1Y C -0.0205(12) 0.7747(7) 0.0990(8) 0.082(7) Uiso 0.25 1 d PG F -2 H1Y H -0.0261 0.7141 0.0939 0.098 Uiso 0.25 1 calc PR F -2 C2Y C 0.0140(12) 0.8081(7) 0.1556(7) 0.088(7) Uiso 0.25 1 d PG F -2 H2Y H 0.0314 0.7698 0.1883 0.106 Uiso 0.25 1 calc PR F -2 C3Y C 0.0225(11) 0.8986(8) 0.1633(6) 0.089(8) Uiso 0.25 1 d PG F -2 H3Y H 0.0455 0.9209 0.2012 0.106 Uiso 0.25 1 calc PR F -2 C4Y C -0.0035(13) 0.9557(6) 0.1144(7) 0.072(5) Uiso 0.25 1 d PG F -2 H4Y H 0.0021 1.0163 0.1196 0.087 Uiso 0.50 2 calc SPR F -2 C5Y C -0.0380(12) 0.9223(11) 0.0578(7) 0.073(6) Uiso 0.25 1 d PG F -2 H5Y H -0.0554 0.9606 0.0251 0.088 Uiso 0.25 1 calc PR F -2 C6Y C -0.0465(10) 0.8318(12) 0.0501(7) 0.080(7) Uiso 0.25 1 d PG F -2 H6Y H -0.0695 0.8095 0.0123 0.096 Uiso 0.25 1 calc PR F -2 Sn11 Sn 0.005(3) 1.0674(14) 0.2514(13) 0.045(8) Uiso 0.01 2 d SPR . -3 Sn20 Sn 0.0009(8) 0.8806(6) 0.1048(5) 0.072(7) Uiso 0.02 2 d SPR F -3 Sn30 Sn -0.002(3) 0.6896(14) 0.2489(12) 0.060(9) Uiso 0.02 4 d SPR F -3 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 Sn1 0.0416(4) 0.0288(3) 0.0532(4) 0.000 0.000 0.000 Sn2 0.0411(2) 0.0529(3) 0.0349(2) -0.00234(18) 0.000 0.000 Sn3 0.0443(4) 0.0294(3) 0.0609(4) 0.000 0.000 0.000 Cl1 0.0459(13) 0.0510(12) 0.0604(14) 0.0103(10) -0.0148(11) 0.0035(10) Cl2 0.0481(14) 0.0601(14) 0.0657(15) -0.0192(11) 0.0044(11) 0.0084(11) P1 0.0309(10) 0.0322(10) 0.0358(11) 0.0028(8) -0.0020(9) -0.0001(8) P2 0.0281(10) 0.0329(11) 0.0394(11) -0.0031(8) -0.0041(9) -0.0020(8) Fe1 0.0336(6) 0.0407(6) 0.0368(6) 0.0031(5) 0.0000(5) -0.0049(5) Fe2 0.0387(7) 0.0408(7) 0.0403(6) -0.0038(5) -0.0058(5) -0.0077(5) _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 Sn1 Sn30 1.93(2) . ? Sn1 P1 2.642(2) 12 ? Sn1 P1 2.642(2) . ? Sn1 P1 2.642(2) 10_556 ? Sn1 P1 2.642(2) 3 ? Sn1 Cl1 2.769(2) . ? Sn1 Cl1 2.769(2) 12 ? Sn1 Cl1 2.769(2) 3 ? Sn1 Cl1 2.769(2) 10_556 ? Sn2 P1 2.633(2) . ? Sn2 P1 2.633(2) 12 ? Sn2 P2 2.672(2) 12 ? Sn2 P2 2.672(2) . ? Sn2 Cl1 2.772(2) 12 ? Sn2 Cl1 2.772(2) . ? Sn2 Cl2 2.782(3) 12 ? Sn2 Cl2 2.782(3) . ? Sn3 Sn11 1.73(2) 1_545 ? Sn3 P2 2.644(2) 3 ? Sn3 P2 2.644(2) 12 ? Sn3 P2 2.644(2) 10_556 ? Sn3 P2 2.644(2) . ? Sn3 Cl2 2.752(3) 10_556 ? Sn3 Cl2 2.752(3) 12 ? Sn3 Cl2 2.752(3) 3 ? Sn3 Cl2 2.752(3) . ? Cl1 C17 1.777(7) 12 ? Cl1 P1 2.335(3) 12 ? Cl1 Cl1 2.434(5) 12 ? Cl1 Fe1 2.626(3) 12 ? Cl2 C29 1.75(2) 12 ? Cl2 P2 2.345(3) 12 ? Cl2 Cl2 2.449(5) 12 ? Cl2 Fe2 2.664(3) 12 ? P1 P2 1.578(3) 12 ? P1 P1 1.630(4) 10_556 ? P1 C10 1.797(5) . ? P1 P2 2.240(3) 3 ? P1 Cl1 2.335(3) 12 ? P2 P2 1.552(4) 10_556 ? P2 P1 1.578(3) 12 ? P2 C20 1.786(5) . ? P2 P1 2.240(3) 3 ? P2 Cl2 2.345(3) 12 ? Fe1 C10 2.027(6) . ? Fe1 C14 2.030(6) . ? Fe1 C15 2.035(3) . ? Fe1 C11 2.042(6) . ? Fe1 C16 2.048(6) . ? Fe1 C13 2.047(6) . ? Fe1 C19 2.049(5) . ? Fe1 C12 2.054(6) . ? Fe1 C17 2.071(4) . ? Fe1 C18 2.072(5) . ? Fe1 Cl1 2.626(3) 12 ? C10 C14 1.4200 . ? C10 C11 1.4200 . ? C11 C12 1.4200 . ? C12 C13 1.4200 . ? C13 C14 1.4200 . ? C15 C16 1.4200 . ? C15 C19 1.4200 . ? C16 C17 1.4200 . ? C17 C18 1.4200 . ? C17 Cl1 1.777(3) 12 ? C18 C19 1.4200 . ? Fe2 C20 2.022(6) . ? Fe2 C21 2.033(6) . ? Fe2 C24 2.042(5) . ? Fe2 C26 2.051(7) . ? Fe2 C25 2.053(7) . ? Fe2 C27 2.052(7) . ? Fe2 C29 2.056(7) . ? Fe2 C28 2.055(7) . ? Fe2 C22 2.060(6) . ? Fe2 C23 2.065(6) . ? Fe2 Cl2 2.664(3) 12 ? C20 C21 1.4200 . ? C20 C24 1.4200 . ? C21 C22 1.4200 . ? C22 C23 1.4200 . ? C23 C24 1.4200 . ? C25 C26 1.4200 . ? C25 C29 1.4200 . ? C26 C27 1.4200 . ? C27 C28 1.4200 . ? C28 C29 1.4200 . ? C29 Cl2 1.752(7) 12 ? C1X C2X 1.3900 . ? C1X C6X 1.3900 . ? C2X C3X 1.3900 . ? C3X C4X 1.3900 . ? C4X C5X 1.3900 . ? C5X C6X 1.3900 . ? C1Y C2Y 1.3900 . ? C1Y C6Y 1.3900 . ? C2Y C3Y 1.3900 . ? C3Y C4Y 1.3900 . ? C4Y C5Y 1.3900 . ? C5Y C6Y 1.3900 . ? Sn11 Sn3 1.73(2) 1_565 ? 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 Sn30 Sn1 P1 141.3(14) . 12 ? Sn30 Sn1 P1 143.2(13) . . ? P1 Sn1 P1 63.19(9) 12 . ? Sn30 Sn1 P1 143.9(14) . 10_556 ? P1 Sn1 P1 74.88(9) 12 10_556 ? P1 Sn1 P1 35.92(9) . 10_556 ? Sn30 Sn1 P1 141.9(14) . 3 ? P1 Sn1 P1 35.92(9) 12 3 ? P1 Sn1 P1 74.88(9) . 3 ? P1 Sn1 P1 63.19(9) 10_556 3 ? Sn30 Sn1 Cl1 98.0(10) . . ? P1 Sn1 Cl1 51.07(6) 12 . ? P1 Sn1 Cl1 80.34(6) . . ? P1 Sn1 Cl1 112.18(6) 10_556 . ? P1 Sn1 Cl1 85.23(7) 3 . ? Sn30 Sn1 Cl1 99.0(9) . 12 ? P1 Sn1 Cl1 80.34(6) 12 12 ? P1 Sn1 Cl1 51.07(6) . 12 ? P1 Sn1 Cl1 85.23(7) 10_556 12 ? P1 Sn1 Cl1 112.18(6) 3 12 ? Cl1 Sn1 Cl1 52.15(10) . 12 ? Sn30 Sn1 Cl1 100.2(10) . 3 ? P1 Sn1 Cl1 112.18(6) 12 3 ? P1 Sn1 Cl1 85.23(7) . 3 ? P1 Sn1 Cl1 51.07(6) 10_556 3 ? P1 Sn1 Cl1 80.34(6) 3 3 ? Cl1 Sn1 Cl1 161.81(9) . 3 ? Cl1 Sn1 Cl1 124.31(10) 12 3 ? Sn30 Sn1 Cl1 99.2(9) . 10_556 ? P1 Sn1 Cl1 85.23(7) 12 10_556 ? P1 Sn1 Cl1 112.18(6) . 10_556 ? P1 Sn1 Cl1 80.34(6) 10_556 10_556 ? P1 Sn1 Cl1 51.07(6) 3 10_556 ? Cl1 Sn1 Cl1 124.31(10) . 10_556 ? Cl1 Sn1 Cl1 161.81(9) 12 10_556 ? Cl1 Sn1 Cl1 52.15(10) 3 10_556 ? P1 Sn2 P1 63.45(9) . 12 ? P1 Sn2 P2 34.59(6) . 12 ? P1 Sn2 P2 74.19(6) 12 12 ? P1 Sn2 P2 74.19(6) . . ? P1 Sn2 P2 34.59(6) 12 . ? P2 Sn2 P2 63.17(9) 12 . ? P1 Sn2 Cl1 51.12(7) . 12 ? P1 Sn2 Cl1 80.44(6) 12 12 ? P2 Sn2 Cl1 84.13(7) 12 12 ? P2 Sn2 Cl1 110.95(6) . 12 ? P1 Sn2 Cl1 80.44(6) . . ? P1 Sn2 Cl1 51.12(7) 12 . ? P2 Sn2 Cl1 110.95(6) 12 . ? P2 Sn2 Cl1 84.13(7) . . ? Cl1 Sn2 Cl1 52.08(10) 12 . ? P1 Sn2 Cl2 110.80(7) . 12 ? P1 Sn2 Cl2 83.81(7) 12 12 ? P2 Sn2 Cl2 80.22(7) 12 12 ? P2 Sn2 Cl2 50.88(6) . 12 ? Cl1 Sn2 Cl2 160.29(7) 12 12 ? Cl1 Sn2 Cl2 123.71(7) . 12 ? P1 Sn2 Cl2 83.81(7) . . ? P1 Sn2 Cl2 110.80(7) 12 . ? P2 Sn2 Cl2 50.88(6) 12 . ? P2 Sn2 Cl2 80.22(7) . . ? Cl1 Sn2 Cl2 123.71(7) 12 . ? Cl1 Sn2 Cl2 160.29(7) . . ? Cl2 Sn2 Cl2 52.23(10) 12 . ? Sn11 Sn3 P2 140(5) 1_545 3 ? Sn11 Sn3 P2 141(5) 1_545 12 ? P2 Sn3 P2 34.14(9) 3 12 ? Sn11 Sn3 P2 145(5) 1_545 10_556 ? P2 Sn3 P2 63.91(9) 3 10_556 ? P2 Sn3 P2 74.49(9) 12 10_556 ? Sn11 Sn3 P2 146(5) 1_545 . ? P2 Sn3 P2 74.49(9) 3 . ? P2 Sn3 P2 63.91(9) 12 . ? P2 Sn3 P2 34.14(9) 10_556 . ? Sn11 Sn3 Cl2 97(4) 1_545 10_556 ? P2 Sn3 Cl2 51.48(7) 3 10_556 ? P2 Sn3 Cl2 83.93(7) 12 10_556 ? P2 Sn3 Cl2 81.28(7) 10_556 10_556 ? P2 Sn3 Cl2 111.43(7) . 10_556 ? Sn11 Sn3 Cl2 101(4) 1_545 12 ? P2 Sn3 Cl2 111.43(7) 3 12 ? P2 Sn3 Cl2 81.28(7) 12 12 ? P2 Sn3 Cl2 83.93(7) 10_556 12 ? P2 Sn3 Cl2 51.48(7) . 12 ? Cl2 Sn3 Cl2 161.39(10) 10_556 12 ? Sn11 Sn3 Cl2 100(4) 1_545 3 ? P2 Sn3 Cl2 81.28(7) 3 3 ? P2 Sn3 Cl2 111.43(7) 12 3 ? P2 Sn3 Cl2 51.48(7) 10_556 3 ? P2 Sn3 Cl2 83.93(7) . 3 ? Cl2 Sn3 Cl2 52.86(10) 10_556 3 ? Cl2 Sn3 Cl2 123.47(10) 12 3 ? Sn11 Sn3 Cl2 99(4) 1_545 . ? P2 Sn3 Cl2 83.93(7) 3 . ? P2 Sn3 Cl2 51.48(7) 12 . ? P2 Sn3 Cl2 111.43(7) 10_556 . ? P2 Sn3 Cl2 81.28(7) . . ? Cl2 Sn3 Cl2 123.47(10) 10_556 . ? Cl2 Sn3 Cl2 52.86(10) 12 . ? Cl2 Sn3 Cl2 161.39(10) 3 . ? C17 Cl1 P1 138.1(2) 12 12 ? C17 Cl1 Cl1 127.8(2) 12 12 ? P1 Cl1 Cl1 94.11(8) 12 12 ? C17 Cl1 Fe1 51.86(19) 12 12 ? P1 Cl1 Fe1 86.26(10) 12 12 ? Cl1 Cl1 Fe1 177.39(6) 12 12 ? C17 Cl1 Sn1 132.1(4) 12 . ? P1 Cl1 Sn1 61.66(7) 12 . ? Cl1 Cl1 Sn1 63.92(5) 12 . ? Fe1 Cl1 Sn1 118.41(10) 12 . ? C17 Cl1 Sn2 132.4(4) 12 . ? P1 Cl1 Sn2 61.35(7) 12 . ? Cl1 Cl1 Sn2 63.96(5) 12 . ? Fe1 Cl1 Sn2 114.11(9) 12 . ? Sn1 Cl1 Sn2 95.41(7) . . ? C29 Cl2 P2 135.1(7) 12 12 ? C29 Cl2 Cl2 130.7(7) 12 12 ? P2 Cl2 Cl2 94.28(8) 12 12 ? C29 Cl2 Fe2 50.5(8) 12 12 ? P2 Cl2 Fe2 84.6(4) 12 12 ? Cl2 Cl2 Fe2 178.7(2) 12 12 ? C29 Cl2 Sn3 132.7(9) 12 . ? P2 Cl2 Sn3 61.90(8) 12 . ? Cl2 Cl2 Sn3 63.57(5) 12 . ? Fe2 Cl2 Sn3 116.4(4) 12 . ? C29 Cl2 Sn2 131.5(9) 12 . ? P2 Cl2 Sn2 62.13(8) 12 . ? Cl2 Cl2 Sn2 63.89(5) 12 . ? Fe2 Cl2 Sn2 114.88(12) 12 . ? Sn3 Cl2 Sn2 95.79(7) . . ? P2 P1 P1 88.60(10) 12 10_556 ? P2 P1 C10 98.4(2) 12 . ? P1 P1 C10 101.85(19) 10_556 . ? P2 P1 P2 43.84(13) 12 3 ? P1 P1 P2 44.75(7) 10_556 3 ? C10 P1 P2 104.2(2) . 3 ? P2 P1 Cl1 136.77(15) 12 12 ? P1 P1 Cl1 134.39(8) 10_556 12 ? C10 P1 Cl1 79.6(2) . 12 ? P2 P1 Cl1 176.22(14) 3 12 ? P2 P1 Sn2 74.08(11) 12 . ? P1 P1 Sn2 142.78(4) 10_556 . ? C10 P1 Sn2 112.9(2) . . ? P2 P1 Sn2 111.02(10) 3 . ? Cl1 P1 Sn2 67.53(8) 12 . ? P2 P1 Sn1 142.31(14) 12 . ? P1 P1 Sn1 72.04(4) 10_556 . ? C10 P1 Sn1 116.8(2) . . ? P2 P1 Sn1 110.10(10) 3 . ? Cl1 P1 Sn1 67.27(8) 12 . ? Sn2 P1 Sn1 101.97(7) . . ? P2 P2 P1 91.40(10) 10_556 12 ? P2 P2 C20 99.75(19) 10_556 . ? P1 P2 C20 99.2(2) 12 . ? P2 P2 P1 44.75(7) 10_556 3 ? P1 P2 P1 46.65(13) 12 3 ? C20 P2 P1 103.6(2) . 3 ? P2 P2 Cl2 134.62(8) 10_556 12 ? P1 P2 Cl2 133.61(15) 12 12 ? C20 P2 Cl2 81.1(2) . 12 ? P1 P2 Cl2 175.31(13) 3 12 ? P2 P2 Sn3 72.93(4) 10_556 . ? P1 P2 Sn3 142.92(14) 12 . ? C20 P2 Sn3 116.2(2) . . ? P1 P2 Sn3 110.39(10) 3 . ? Cl2 P2 Sn3 66.62(8) 12 . ? P2 P2 Sn2 143.03(4) 10_556 . ? P1 P2 Sn2 71.32(11) 12 . ? C20 P2 Sn2 114.8(2) . . ? P1 P2 Sn2 110.83(9) 3 . ? Cl2 P2 Sn2 66.99(8) 12 . ? Sn3 P2 Sn2 101.11(7) . . ? C10 Fe1 C14 40.98(10) . . ? C10 Fe1 C15 162.1(2) . . ? C14 Fe1 C15 123.6(2) . . ? C10 Fe1 C11 40.86(10) . . ? C14 Fe1 C11 68.71(13) . . ? C15 Fe1 C11 154.4(2) . . ? C10 Fe1 C16 127.06(19) . . ? C14 Fe1 C16 109.6(2) . . ? C15 Fe1 C16 40.70(9) . . ? C11 Fe1 C16 163.35(19) . . ? C10 Fe1 C13 68.67(13) . . ? C14 Fe1 C13 40.77(10) . . ? C15 Fe1 C13 105.30(19) . . ? C11 Fe1 C13 68.39(14) . . ? C16 Fe1 C13 121.9(2) . . ? C10 Fe1 C19 157.00(19) . . ? C14 Fe1 C19 158.59(19) . . ? C15 Fe1 C19 40.69(7) . . ? C11 Fe1 C19 119.7(2) . . ? C16 Fe1 C19 68.21(12) . . ? C13 Fe1 C19 120.9(2) . . ? C10 Fe1 C12 68.53(14) . . ? C14 Fe1 C12 68.47(13) . . ? C15 Fe1 C12 118.6(2) . . ? C11 Fe1 C12 40.57(11) . . ? C16 Fe1 C12 155.58(19) . . ? C13 Fe1 C12 40.52(11) . . ? C19 Fe1 C12 104.3(2) . . ? C10 Fe1 C17 111.27(16) . . ? C14 Fe1 C17 125.3(2) . . ? C15 Fe1 C17 68.05(14) . . ? C11 Fe1 C17 126.14(17) . . ? C16 Fe1 C17 40.33(10) . . ? C13 Fe1 C17 159.2(2) . . ? C19 Fe1 C17 67.78(14) . . ? C12 Fe1 C17 160.2(2) . . ? C10 Fe1 C18 123.86(16) . . ? C14 Fe1 C18 160.38(18) . . ? C15 Fe1 C18 68.04(13) . . ? C11 Fe1 C18 107.87(18) . . ? C16 Fe1 C18 67.79(13) . . ? C13 Fe1 C18 157.7(2) . . ? C19 Fe1 C18 40.31(10) . . ? C12 Fe1 C18 122.3(2) . . ? C17 Fe1 C18 40.10(8) . . ? C10 Fe1 Cl1 68.87(15) . 12 ? C14 Fe1 Cl1 92.75(17) . 12 ? C15 Fe1 Cl1 108.84(14) . 12 ? C11 Fe1 Cl1 91.57(17) . 12 ? C16 Fe1 Cl1 71.85(10) . 12 ? C13 Fe1 Cl1 132.99(17) . 12 ? C19 Fe1 Cl1 106.08(14) . 12 ? C12 Fe1 Cl1 131.84(17) . 12 ? C17 Fe1 Cl1 42.44(8) . 12 ? C18 Fe1 Cl1 67.79(10) . 12 ? C14 C10 C11 108.0 . . ? C14 C10 P1 127.2(3) . . ? C11 C10 P1 124.8(3) . . ? C14 C10 Fe1 69.6(2) . . ? C11 C10 Fe1 70.1(2) . . ? P1 C10 Fe1 125.3(3) . . ? C12 C11 C10 108.0 . . ? C12 C11 Fe1 70.2(2) . . ? C10 C11 Fe1 69.0(2) . . ? C13 C12 C11 108.0 . . ? C13 C12 Fe1 69.5(2) . . ? C11 C12 Fe1 69.2(2) . . ? C12 C13 C14 108.0 . . ? C12 C13 Fe1 70.0(2) . . ? C14 C13 Fe1 69.0(2) . . ? C10 C14 C13 108.0 . . ? C10 C14 Fe1 69.4(2) . . ? C13 C14 Fe1 70.3(2) . . ? C16 C15 C19 108.0 . . ? C16 C15 Fe1 70.15(18) . . ? C19 C15 Fe1 70.2(2) . . ? C15 C16 C17 108.0 . . ? C15 C16 Fe1 69.15(12) . . ? C17 C16 Fe1 70.69(9) . . ? C16 C17 C18 108.0 . . ? C16 C17 Cl1 120.54(14) . 12 ? C18 C17 Cl1 112.12(14) . 12 ? C16 C17 Fe1 68.98(13) . . ? C18 C17 Fe1 70.0(2) . . ? Cl1 C17 Fe1 85.71(18) 12 . ? C19 C18 C17 108.0 . . ? C19 C18 Fe1 69.01(8) . . ? C17 C18 Fe1 69.9(2) . . ? C18 C19 C15 108.0 . . ? C18 C19 Fe1 70.68(7) . . ? C15 C19 Fe1 69.10(17) . . ? C20 Fe2 C21 41.00(11) . . ? C20 Fe2 C24 40.90(10) . . ? C21 Fe2 C24 68.65(13) . . ? C20 Fe2 C26 159.5(3) . . ? C21 Fe2 C26 157.0(3) . . ? C24 Fe2 C26 122.1(2) . . ? C20 Fe2 C25 125.0(2) . . ? C21 Fe2 C25 161.1(3) . . ? C24 Fe2 C25 109.0(2) . . ? C26 Fe2 C25 40.49(13) . . ? C20 Fe2 C27 159.5(3) . . ? C21 Fe2 C27 121.8(3) . . ? C24 Fe2 C27 156.7(3) . . ? C26 Fe2 C27 40.50(13) . . ? C25 Fe2 C27 68.07(16) . . ? C20 Fe2 C29 110.4(2) . . ? C21 Fe2 C29 124.7(2) . . ? C24 Fe2 C29 125.8(2) . . ? C26 Fe2 C29 68.04(16) . . ? C25 Fe2 C29 40.43(12) . . ? C27 Fe2 C29 68.02(16) . . ? C20 Fe2 C28 125.0(3) . . ? C21 Fe2 C28 108.0(2) . . ? C24 Fe2 C28 161.9(3) . . ? C26 Fe2 C28 68.06(16) . . ? C25 Fe2 C28 68.01(16) . . ? C27 Fe2 C28 40.46(13) . . ? C29 Fe2 C28 40.42(13) . . ? C20 Fe2 C22 68.51(14) . . ? C21 Fe2 C22 40.60(11) . . ? C24 Fe2 C22 68.13(13) . . ? C26 Fe2 C22 120.6(3) . . ? C25 Fe2 C22 157.5(3) . . ? C27 Fe2 C22 105.3(2) . . ? C29 Fe2 C22 159.0(3) . . ? C28 Fe2 C22 121.7(2) . . ? C20 Fe2 C23 68.40(13) . . ? C21 Fe2 C23 68.20(14) . . ? C24 Fe2 C23 40.45(10) . . ? C26 Fe2 C23 105.8(2) . . ? C25 Fe2 C23 123.0(2) . . ? C27 Fe2 C23 120.2(3) . . ? C29 Fe2 C23 160.4(3) . . ? C28 Fe2 C23 156.5(3) . . ? C22 Fe2 C23 40.27(11) . . ? C20 Fe2 Cl2 69.35(15) . 12 ? C21 Fe2 Cl2 92.15(18) . 12 ? C24 Fe2 Cl2 93.16(17) . 12 ? C26 Fe2 Cl2 106.5(2) . 12 ? C25 Fe2 Cl2 69.1(2) . 12 ? C27 Fe2 Cl2 106.4(2) . 12 ? C29 Fe2 Cl2 41.09(18) . 12 ? C28 Fe2 Cl2 68.9(2) . 12 ? C22 Fe2 Cl2 132.42(18) . 12 ? C23 Fe2 Cl2 133.12(17) . 12 ? C21 C20 C24 108.0 . . ? C21 C20 P2 125.2(3) . . ? C24 C20 P2 126.8(3) . . ? C21 C20 Fe2 69.9(2) . . ? C24 C20 Fe2 70.3(2) . . ? P2 C20 Fe2 125.0(3) . . ? C20 C21 C22 108.0 . . ? C20 C21 Fe2 69.1(2) . . ? C22 C21 Fe2 70.7(2) . . ? C23 C22 C21 108.0 . . ? C23 C22 Fe2 70.1(2) . . ? C21 C22 Fe2 68.7(2) . . ? C22 C23 C24 108.0 . . ? C22 C23 Fe2 69.6(2) . . ? C24 C23 Fe2 68.9(2) . . ? C23 C24 C20 108.0 . . ? C23 C24 Fe2 70.7(2) . . ? C20 C24 Fe2 68.8(2) . . ? C26 C25 C29 108.0 . . ? C26 C25 Fe2 69.7(3) . . ? C29 C25 Fe2 69.9(3) . . ? C25 C26 C27 108.0 . . ? C25 C26 Fe2 69.9(3) . . ? C27 C26 Fe2 69.8(3) . . ? C28 C27 C26 108.0 . . ? C28 C27 Fe2 69.9(3) . . ? C26 C27 Fe2 69.7(3) . . ? C29 C28 C27 108.0 . . ? C29 C28 Fe2 69.8(3) . . ? C27 C28 Fe2 69.7(3) . . ? C28 C29 C25 108.0 . . ? C28 C29 Cl2 117.5(4) . 12 ? C25 C29 Cl2 117.9(4) . 12 ? C28 C29 Fe2 69.8(3) . . ? C25 C29 Fe2 69.7(3) . . ? Cl2 C29 Fe2 88.4(3) 12 . ? C2X C1X C6X 120.0 . . ? C3X C2X C1X 120.0 . . ? C2X C3X C4X 120.0 . . ? C5X C4X C3X 120.0 . . ? C4X C5X C6X 120.0 . . ? C5X C6X C1X 120.0 . . ? C2Y C1Y C6Y 120.0 . . ? C1Y C2Y C3Y 120.0 . . ? C4Y C3Y C2Y 120.0 . . ? C5Y C4Y C3Y 120.0 . . ? C4Y C5Y C6Y 120.0 . . ? C5Y C6Y C1Y 120.0 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.753 _refine_diff_density_min -0.552 _refine_diff_density_rms 0.090