# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1673 data_ab052 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C18 H10 Fe2 O6 P S' _chemical_formula_weight 496.99 _chemical_melting_point ? _chemical_compound_source ? 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.271(2) _cell_length_b 10.675(2) _cell_length_c 11.517(2) _cell_angle_alpha 102.19(3) _cell_angle_beta 102.93(3) _cell_angle_gamma 117.93(3) _cell_volume 1011.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour orange _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.632 _exptl_crystal_density_method ? _exptl_crystal_F_000 498 _exptl_absorpt_coefficient_mu 1.647 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5182 _exptl_absorpt_correction_T_max 0.6217 _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 'Siemens P4' _diffrn_measurement_method theta/2theta _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.1 _diffrn_reflns_number 5778 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_sigmaI/netI 0.0572 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 30.00 _reflns_number_total 5024 _reflns_number_observed 3379 _reflns_observed_criterion >2sigma(I) _computing_data_collection XSCANS _computing_cell_refinement XSCANS _computing_data_reduction XSCANS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0367P)^2^+0.1780P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5024 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0812 _refine_ls_R_factor_obs 0.0449 _refine_ls_wR_factor_all 0.0986 _refine_ls_wR_factor_obs 0.0845 _refine_ls_goodness_of_fit_all 1.023 _refine_ls_goodness_of_fit_obs 1.082 _refine_ls_restrained_S_all 1.023 _refine_ls_restrained_S_obs 1.082 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe1 Fe 0.40524(6) 0.78508(5) 0.11722(4) 0.03535(13) Uani 1 d . . Fe2 Fe 0.68499(6) 0.89308(5) 0.10160(4) 0.03746(14) Uani 1 d . . P P 0.63733(10) 0.90680(9) 0.28274(7) 0.0315(2) Uani 1 d . . S S 0.54893(10) 1.00923(9) 0.09557(7) 0.0363(2) Uani 1 d .. . C11 C 0.2719(5) 0.8260(5) 0.1680(4) 0.0545(10) Uani 1 d . . C12 C 0.2874(5) 0.6784(4) -0.0518(4) 0.0548(11) Uani 1 d . . C13 C 0.3343(5) 0.6120(4) 0.1467(3) 0.0499(10) Uani 1 d . . C21 C 0.7649(6) 0.7801(5) 0.1263(4) 0.0597(11) Uani 1 d . . C22 C 0.8703(5) 1.0632(5) 0.1345(4) 0.0580(11) Uani 1 d . . C23 C 0.6185(5) 0.8041(5) -0.0702(4) 0.0568(10) Uani 1 d . . O11 O 0.1868(4) 0.8518(4) 0.1985(4) 0.0918(11) Uani 1 d . . O12 O 0.2099(4) 0.6071(3) -0.1573(3) 0.0923(12) Uani 1 d . . O13 O 0.2816(4) 0.4997(3) 0.1639(3) 0.0761(10) Uani 1 d . . O21 O 0.8199(5) 0.7107(5) 0.1411(4) 0.1031(13) Uani 1 d . . O22 O 0.9839(4) 1.1726(4) 0.1508(4) 0.1043(14) Uani 1 d . . O23 O 0.5813(5) 0.7459(4) -0.1774(3) 0.0886(11) Uani 1 d . . C111 C 0.7146(4) 1.0972(3) 0.3941(3) 0.0322(7) Uani 1 d . . C112 C 0.6158(4) 1.1384(4) 0.4290(3) 0.0386(8) Uani 1 d . . H112 H 0.5062(4) 1.0711(4) 0.3904(3) 0.046 Uiso 1 calc R . C113 C 0.6801(4) 1.2807(4) 0.5221(3) 0.0467(9) Uani 1 d . . H113 H 0.6129(4) 1.3083(4) 0.5443(3) 0.056 Uiso 1 calc R . C114 C 0.8406(5) 1.3795(4) 0.5807(4) 0.0503(10) Uani 1 d . . H114 H 0.8828(5) 1.4734(4) 0.6438(4) 0.060 Uiso 1 calc R . C115 C 0.9411(4) 1.3397(4) 0.5460(4) 0.0528(10) Uani 1 d . . H115 H 1.0506(4) 1.4070(4) 0.5856(4) 0.063 Uiso 1 calc R . C116 C 0.8782(4) 1.1999(4) 0.4526(3) 0.0442(9) Uani 1 d . . H116 H 0.9458(4) 1.1743(4) 0.4287(3) 0.053 Uiso 1 calc R . C211 C 0.6796(4) 0.8157(4) 0.3913(3) 0.0330(7) Uani 1 d . . C212 C 0.7391(4) 0.8899(4) 0.5237(3) 0.0393(8) Uani 1 d . . H212 H 0.7663(4) 0.9899(4) 0.5574(3) 0.047 Uiso 1 calc R . C213 C 0.7581(4) 0.8162(4) 0.6054(3) 0.0460(9) Uani 1 d . . H213 H 0.7983(4) 0.8670(4) 0.6936(3) 0.055 Uiso 1 calc R . C214 C 0.7177(5) 0.6687(5) 0.5568(4) 0.0516(10) Uani 1 d . . H214 H 0.7280(5) 0.6189(5) 0.6120(4) 0.062 Uiso 1 calc R . C215 C 0.6620(4) 0.5942(4) 0.4271(4) 0.0479(9) Uani 1 d . . H215 H 0.6372(4) 0.4949(4) 0.3948(4) 0.058 Uiso 1 calc R . C216 C 0.6426(4) 0.6669(4) 0.3434(3) 0.0439(9) Uani 1 d . . H216 H 0.6049(4) 0.6160(4) 0.2556(3) 0.053 Uiso 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 0.0325(3) 0.0316(3) 0.0347(2) 0.0095(2) 0.0095(2) 0.0146(2) Fe2 0.0397(3) 0.0413(3) 0.0364(2) 0.0153(2) 0.0175(2) 0.0237(2) P 0.0327(5) 0.0311(4) 0.0321(4) 0.0119(3) 0.0121(3) 0.0180(4) S 0.0400(5) 0.0336(4) 0.0321(4) 0.0122(3) 0.0090(3) 0.0195(4) C11 0.041(2) 0.054(2) 0.057(2) 0.011(2) 0.017(2) 0.022(2) C12 0.057(3) 0.036(2) 0.047(2) 0.012(2) 0.007(2) 0.015(2) C13 0.046(2) 0.043(2) 0.051(2) 0.014(2) 0.013(2) 0.020(2) C21 0.075(3) 0.077(3) 0.063(2) 0.037(2) 0.043(2) 0.055(3) C22 0.047(3) 0.067(3) 0.056(2) 0.030(2) 0.018(2) 0.026(2) C23 0.066(3) 0.065(3) 0.050(2) 0.021(2) 0.026(2) 0.042(2) O11 0.059(2) 0.100(3) 0.106(3) 0.008(2) 0.033(2) 0.047(2) O12 0.103(3) 0.058(2) 0.045(2) 0.0018(14) -0.008(2) 0.015(2) O13 0.072(2) 0.046(2) 0.087(2) 0.035(2) 0.020(2) 0.015(2) O21 0.137(4) 0.143(3) 0.134(3) 0.086(3) 0.087(3) 0.121(3) O22 0.051(2) 0.102(3) 0.120(3) 0.067(2) 0.016(2) 0.009(2) O23 0.117(3) 0.111(3) 0.044(2) 0.011(2) 0.032(2) 0.072(2) C111 0.033(2) 0.029(2) 0.0334(15) 0.0122(12) 0.0108(13) 0.0160(14) C112 0.033(2) 0.036(2) 0.043(2) 0.0112(14) 0.0144(15) 0.017(2) C113 0.045(2) 0.042(2) 0.057(2) 0.014(2) 0.026(2) 0.026(2) C114 0.047(2) 0.032(2) 0.054(2) 0.004(2) 0.014(2) 0.015(2) C115 0.031(2) 0.038(2) 0.063(2) 0.006(2) 0.014(2) 0.007(2) C116 0.036(2) 0.041(2) 0.050(2) 0.007(2) 0.017(2) 0.020(2) C211 0.028(2) 0.039(2) 0.038(2) 0.0181(14) 0.0161(13) 0.0202(15) C212 0.042(2) 0.043(2) 0.041(2) 0.0176(15) 0.0176(15) 0.026(2) C213 0.050(2) 0.064(2) 0.043(2) 0.029(2) 0.022(2) 0.039(2) C214 0.047(2) 0.063(3) 0.063(2) 0.042(2) 0.024(2) 0.034(2) C215 0.044(2) 0.040(2) 0.067(2) 0.026(2) 0.020(2) 0.026(2) C216 0.046(2) 0.044(2) 0.046(2) 0.017(2) 0.018(2) 0.026(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C13 1.781(4) . ? Fe1 C11 1.794(5) . ? Fe1 C12 1.809(4) . ? Fe1 P 2.242(2) . ? Fe1 S 2.2526(13) . ? Fe1 Fe2 2.6141(11) . ? Fe2 C21 1.783(4) . ? Fe2 C22 1.792(5) . ? Fe2 C23 1.810(4) . ? Fe2 P 2.2379(11) . ? Fe2 S 2.2608(11) . ? P C111 1.827(3) . ? P C211 1.834(3) . ? S S 2.130(2) 2_675 ? C11 O11 1.134(5) . ? C12 O12 1.139(4) . ? C13 O13 1.145(4) . ? C21 O21 1.139(5) . ? C22 O22 1.137(5) . ? C23 O23 1.140(4) . ? C111 C112 1.382(5) . ? C111 C116 1.391(5) . ? C112 C113 1.396(5) . ? C113 C114 1.364(5) . ? C114 C115 1.389(5) . ? C115 C116 1.381(5) . ? C211 C212 1.394(4) . ? C211 C216 1.394(4) . ? C212 C213 1.385(4) . ? C213 C214 1.369(5) . ? C214 C215 1.372(5) . ? C215 C216 1.394(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 Fe1 C11 94.5(2) . . ? C13 Fe1 C12 90.3(2) . . ? C11 Fe1 C12 100.3(2) . . ? C13 Fe1 P 92.93(13) . . ? C11 Fe1 P 108.87(13) . . ? C12 Fe1 P 150.3(2) . . ? C13 Fe1 S 166.87(13) . . ? C11 Fe1 S 96.13(14) . . ? C12 Fe1 S 95.39(13) . . ? P Fe1 S 76.35(5) . . ? C13 Fe1 Fe2 112.79(14) . . ? C11 Fe1 Fe2 147.19(13) . . ? C12 Fe1 Fe2 97.6(2) . . ? P Fe1 Fe2 54.23(4) . . ? S Fe1 Fe2 54.75(4) . . ? C21 Fe2 C22 96.2(2) . . ? C21 Fe2 C23 90.7(2) . . ? C22 Fe2 C23 100.9(2) . . ? C21 Fe2 P 92.11(13) . . ? C22 Fe2 P 108.12(14) . . ? C23 Fe2 P 150.37(15) . . ? C21 Fe2 S 166.52(14) . . ? C22 Fe2 S 93.91(15) . . ? C23 Fe2 S 96.10(14) . . ? P Fe2 S 76.26(4) . . ? C21 Fe2 Fe1 113.15(15) . . ? C22 Fe2 Fe1 144.88(15) . . ? C23 Fe2 Fe1 97.71(15) . . ? P Fe2 Fe1 54.36(4) . . ? S Fe2 Fe1 54.46(3) . . ? C111 P C211 102.04(14) . . ? C111 P Fe2 116.61(11) . . ? C211 P Fe2 124.52(11) . . ? C111 P Fe1 119.76(11) . . ? C211 P Fe1 121.91(11) . . ? Fe2 P Fe1 71.41(4) . . ? S S Fe1 109.85(7) 2_675 . ? S S Fe2 109.88(6) 2_675 . ? Fe1 S Fe2 70.79(4) . . ? O11 C11 Fe1 179.0(4) . . ? O12 C12 Fe1 177.6(4) . . ? O13 C13 Fe1 176.7(4) . . ? O21 C21 Fe2 177.8(4) . . ? O22 C22 Fe2 176.5(4) . . ? O23 C23 Fe2 176.8(4) . . ? C112 C111 C116 118.9(3) . . ? C112 C111 P 121.9(3) . . ? C116 C111 P 119.0(3) . . ? C111 C112 C113 120.2(3) . . ? C114 C113 C112 120.5(4) . . ? C113 C114 C115 119.9(3) . . ? C116 C115 C114 119.9(3) . . ? C115 C116 C111 120.6(3) . . ? C212 C211 C216 118.5(3) . . ? C212 C211 P 120.7(2) . . ? C216 C211 P 120.7(2) . . ? C213 C212 C211 120.7(3) . . ? C214 C213 C212 120.2(3) . . ? C215 C214 C213 120.3(3) . . ? C214 C215 C216 120.2(3) . . ? C215 C216 C211 120.1(3) . . ? _refine_diff_density_max 0.417 _refine_diff_density_min -0.309 _refine_diff_density_rms 0.071 data_ab048 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H31 Fe3 O6 P3 S' _chemical_formula_weight 876.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P212121 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 12.574(2) _cell_length_b 16.1199(13) _cell_length_c 18.8859(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3827.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour black _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.34 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1784 _exptl_absorpt_coefficient_mu 1.346 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.608 _exptl_absorpt_correction_T_max 0.883 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 570(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4699 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0778 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4476 _reflns_number_gt 3260 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0296P)^2^+0.4836P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_number_reflns 4476 _refine_ls_number_parameters 462 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0818 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.0893 _refine_ls_wR_factor_gt 0.0760 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.143 _refine_ls_shift/su_mean 0.018 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 0.58903(9) 0.59621(6) 0.10423(6) 0.0364(3) Uani 1 1 d . . . Fe2 Fe 0.40645(9) 0.58038(6) 0.05322(6) 0.0401(3) Uani 1 1 d . . . Fe3 Fe 0.51827(8) 0.45099(6) 0.06814(6) 0.0318(3) Uani 1 1 d . . . P1 P 0.65836(19) 0.66515(14) 0.19574(13) 0.0497(6) Uani 1 1 d . . . P2 P 0.34855(15) 0.45570(13) 0.03318(10) 0.0369(5) Uani 1 1 d . . . P3 P 0.67719(15) 0.47661(12) 0.11458(10) 0.0328(5) Uani 1 1 d . . . S S 0.45535(16) 0.52934(12) 0.15844(10) 0.0410(5) Uani 1 1 d . . . C1 C 0.5035(7) 0.6851(5) 0.0770(5) 0.057(2) Uani 1 1 d . . . O1 O 0.4904(5) 0.7560(3) 0.0643(4) 0.083(2) Uani 1 1 d . . . C11 C 0.6771(7) 0.6319(5) 0.0392(4) 0.049(2) Uani 1 1 d . . . O11 O 0.7340(5) 0.6586(4) -0.0028(3) 0.087(2) Uani 1 1 d . . . C22 C 0.2877(7) 0.6349(5) 0.0678(5) 0.061(3) Uani 1 1 d . . . O22 O 0.2082(5) 0.6693(4) 0.0756(5) 0.106(3) Uani 1 1 d . . . C31 C 0.5672(6) 0.4432(5) -0.0198(4) 0.045(2) Uani 1 1 d . . . O31 O 0.5988(5) 0.4423(4) -0.0765(3) 0.0720(19) Uani 1 1 d . . . C32 C 0.5190(6) 0.3470(5) 0.0965(4) 0.046(2) Uani 1 1 d . . . O32 O 0.5203(6) 0.2792(3) 0.1162(4) 0.087(2) Uani 1 1 d . . . C21 C 0.4238(7) 0.6020(5) -0.0373(5) 0.052(2) Uani 1 1 d . . . O21 O 0.4371(6) 0.6137(4) -0.0973(3) 0.082(2) Uani 1 1 d . . . C121 C 0.6360(7) 0.7773(5) 0.2003(6) 0.091(4) Uani 1 1 d . . . H12A H 0.6594 0.8027 0.1571 0.137 Uiso 1 1 calc R . . H12B H 0.6753 0.8000 0.2394 0.137 Uiso 1 1 calc R . . H12C H 0.5615 0.7880 0.2069 0.137 Uiso 1 1 calc R . . C131 C 0.6117(7) 0.6342(6) 0.2835(4) 0.087(4) Uani 1 1 d . . . H13A H 0.6522 0.6628 0.3191 0.130 Uiso 1 1 calc R . . H13B H 0.6207 0.5755 0.2892 0.130 Uiso 1 1 calc R . . H13C H 0.5379 0.6481 0.2884 0.130 Uiso 1 1 calc R . . C111 C 0.8029(6) 0.6584(5) 0.2021(4) 0.045(2) Uani 1 1 d . . . C112 C 0.8539(7) 0.6098(5) 0.2518(4) 0.049(2) Uani 1 1 d . . . H112 H 0.8140 0.5805 0.2849 0.058 Uiso 1 1 calc R . . C113 C 0.9639(8) 0.6041(6) 0.2528(5) 0.065(3) Uani 1 1 d . . . H113 H 0.9973 0.5725 0.2875 0.078 Uiso 1 1 calc R . . C114 C 1.0241(7) 0.6451(6) 0.2027(5) 0.066(3) Uani 1 1 d . . . H114 H 1.0977 0.6395 0.2021 0.079 Uiso 1 1 calc R . . C115 C 0.9744(7) 0.6937(5) 0.1543(5) 0.061(3) Uani 1 1 d . . . H115 H 1.0148 0.7224 0.1211 0.073 Uiso 1 1 calc R . . C116 C 0.8648(6) 0.7014(5) 0.1534(4) 0.044(2) Uani 1 1 d . . . H116 H 0.8324 0.7354 0.1200 0.053 Uiso 1 1 calc R . . C211 C 0.3079(6) 0.4232(5) -0.0558(4) 0.0405(19) Uani 1 1 d . . . C212 C 0.3408(7) 0.3501(5) -0.0849(4) 0.055(2) Uani 1 1 d . . . H212 H 0.3897 0.3174 -0.0607 0.066 Uiso 1 1 calc R . . C213 C 0.3023(8) 0.3239(7) -0.1501(5) 0.079(3) Uani 1 1 d . . . H213 H 0.3258 0.2742 -0.1696 0.095 Uiso 1 1 calc R . . C214 C 0.2288(9) 0.3723(8) -0.1857(5) 0.086(4) Uani 1 1 d . . . H214 H 0.2003 0.3539 -0.2283 0.104 Uiso 1 1 calc R . . C215 C 0.1981(8) 0.4466(8) -0.1586(5) 0.082(4) Uani 1 1 d . . . H215 H 0.1519 0.4806 -0.1840 0.098 Uiso 1 1 calc R . . C216 C 0.2361(6) 0.4718(6) -0.0928(4) 0.057(3) Uani 1 1 d . . . H216 H 0.2130 0.5217 -0.0735 0.069 Uiso 1 1 calc R . . C221 C 0.2468(6) 0.4057(5) 0.0884(4) 0.040(2) Uani 1 1 d . . . C222 C 0.2097(6) 0.4438(5) 0.1496(4) 0.053(2) Uani 1 1 d . . . H222 H 0.2329 0.4967 0.1618 0.064 Uiso 1 1 calc R . . C223 C 0.1379(6) 0.4023(6) 0.1920(5) 0.060(3) Uani 1 1 d . . . H223 H 0.1118 0.4279 0.2325 0.073 Uiso 1 1 calc R . . C224 C 0.1042(7) 0.3237(5) 0.1750(5) 0.064(3) Uani 1 1 d . . . H224 H 0.0571 0.2957 0.2046 0.077 Uiso 1 1 calc R . . C225 C 0.1403(7) 0.2872(5) 0.1151(5) 0.066(3) Uani 1 1 d . . . H225 H 0.1164 0.2346 0.1027 0.079 Uiso 1 1 calc R . . C226 C 0.2117(7) 0.3276(5) 0.0724(5) 0.056(2) Uani 1 1 d . . . H226 H 0.2368 0.3013 0.0318 0.067 Uiso 1 1 calc R . . C311 C 0.7934(5) 0.4537(5) 0.0608(4) 0.0357(18) Uani 1 1 d . . . C312 C 0.8792(6) 0.5079(6) 0.0546(5) 0.061(3) Uani 1 1 d . . . H312 H 0.8768 0.5587 0.0779 0.073 Uiso 1 1 calc R . . C313 C 0.9673(7) 0.4884(6) 0.0149(6) 0.077(3) Uani 1 1 d . . . H313 H 1.0238 0.5254 0.0116 0.093 Uiso 1 1 calc R . . C314 C 0.9708(7) 0.4134(6) -0.0199(5) 0.068(3) Uani 1 1 d . . . H314 H 1.0298 0.3998 -0.0472 0.081 Uiso 1 1 calc R . . C315 C 0.8888(7) 0.3591(6) -0.0145(5) 0.063(3) Uani 1 1 d . . . H315 H 0.8917 0.3085 -0.0380 0.076 Uiso 1 1 calc R . . C316 C 0.8012(6) 0.3791(5) 0.0258(4) 0.048(2) Uani 1 1 d . . . H316 H 0.7458 0.3410 0.0295 0.058 Uiso 1 1 calc R . . C321 C 0.7144(7) 0.4278(5) 0.1980(4) 0.042(2) Uani 1 1 d . . . C322 C 0.8190(6) 0.4102(5) 0.2143(4) 0.047(2) Uani 1 1 d . . . H322 H 0.8715 0.4226 0.1813 0.056 Uiso 1 1 calc R . . C323 C 0.8482(8) 0.3751(6) 0.2775(5) 0.075(3) Uani 1 1 d . . . H323 H 0.9193 0.3633 0.2866 0.090 Uiso 1 1 calc R . . C324 C 0.7727(10) 0.3577(7) 0.3265(5) 0.084(4) Uani 1 1 d . . . H324 H 0.7920 0.3341 0.3696 0.100 Uiso 1 1 calc R . . C325 C 0.6680(9) 0.3747(7) 0.3128(5) 0.097(4) Uani 1 1 d . . . H325 H 0.6165 0.3627 0.3466 0.117 Uiso 1 1 calc R . . C326 C 0.6384(7) 0.4097(6) 0.2486(4) 0.070(3) Uani 1 1 d . . . H326 H 0.5671 0.4210 0.2396 0.084 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 0.0375(6) 0.0330(6) 0.0388(7) -0.0034(6) 0.0020(6) -0.0017(6) Fe2 0.0361(6) 0.0349(6) 0.0493(7) 0.0005(6) 0.0024(6) 0.0011(6) Fe3 0.0337(6) 0.0330(6) 0.0288(6) -0.0004(5) 0.0001(5) -0.0015(5) P1 0.0408(13) 0.0505(14) 0.0578(15) -0.0204(13) 0.0063(13) -0.0048(13) P2 0.0332(10) 0.0404(12) 0.0373(11) 0.0019(11) -0.0002(10) -0.0034(11) P3 0.0356(11) 0.0345(11) 0.0283(10) -0.0013(10) 0.0013(10) -0.0018(9) S 0.0403(11) 0.0447(12) 0.0378(12) -0.0075(10) 0.0069(10) -0.0046(10) C1 0.053(5) 0.050(5) 0.067(6) -0.007(5) 0.004(5) 0.006(5) O1 0.071(4) 0.033(3) 0.145(7) 0.006(4) -0.024(5) -0.004(3) C11 0.058(6) 0.044(5) 0.046(5) 0.002(5) -0.013(5) -0.004(5) O11 0.090(5) 0.106(6) 0.064(5) 0.041(5) 0.023(4) -0.011(5) C22 0.059(6) 0.047(5) 0.077(7) 0.008(6) 0.011(6) 0.005(5) O22 0.060(4) 0.076(5) 0.181(9) 0.018(6) 0.041(5) 0.029(4) C31 0.047(5) 0.041(5) 0.047(5) -0.009(4) -0.009(4) 0.003(4) O31 0.069(4) 0.117(5) 0.030(3) -0.006(4) 0.006(3) 0.004(5) C32 0.047(5) 0.039(5) 0.051(5) 0.007(4) -0.011(5) -0.003(4) O32 0.115(6) 0.039(3) 0.105(6) 0.021(4) -0.040(5) -0.020(4) C21 0.046(5) 0.043(5) 0.066(6) 0.009(5) -0.003(5) 0.007(5) O21 0.100(6) 0.085(5) 0.060(4) 0.032(4) 0.005(4) -0.005(4) C121 0.051(6) 0.053(6) 0.170(11) -0.050(7) -0.023(7) 0.013(5) C131 0.070(7) 0.135(10) 0.054(6) -0.043(6) 0.022(6) -0.015(7) C111 0.042(5) 0.051(5) 0.043(5) -0.022(5) -0.004(4) -0.008(5) C112 0.059(6) 0.050(6) 0.036(5) -0.005(5) -0.008(5) -0.013(5) C113 0.068(7) 0.060(6) 0.067(7) 0.005(6) -0.014(6) 0.001(6) C114 0.050(6) 0.067(7) 0.081(7) -0.022(6) -0.026(6) 0.014(6) C115 0.048(6) 0.060(6) 0.075(7) -0.018(6) 0.004(6) -0.012(5) C116 0.043(5) 0.037(5) 0.052(6) 0.007(5) -0.007(4) -0.008(4) C211 0.041(4) 0.047(5) 0.034(4) 0.000(4) -0.003(4) -0.008(4) C212 0.063(6) 0.064(6) 0.038(5) -0.009(5) -0.002(5) -0.018(5) C213 0.075(8) 0.101(9) 0.061(7) -0.028(7) 0.021(6) -0.027(7) C214 0.059(7) 0.156(13) 0.045(7) -0.020(8) 0.002(6) -0.039(8) C215 0.056(6) 0.144(11) 0.044(6) 0.021(8) -0.012(5) -0.007(8) C216 0.044(5) 0.076(7) 0.051(6) 0.007(5) -0.007(5) -0.009(5) C221 0.039(4) 0.040(5) 0.041(5) 0.006(4) -0.006(4) -0.002(4) C222 0.052(5) 0.051(5) 0.056(6) -0.002(5) 0.013(5) -0.010(5) C223 0.046(5) 0.076(7) 0.059(6) 0.006(6) 0.027(5) 0.005(5) C224 0.054(6) 0.051(6) 0.087(8) 0.019(6) 0.011(6) -0.006(5) C225 0.080(7) 0.035(5) 0.082(7) 0.002(5) 0.023(7) -0.005(5) C226 0.066(6) 0.039(5) 0.063(6) 0.004(5) 0.013(6) -0.010(5) C311 0.037(4) 0.045(5) 0.026(4) -0.001(4) -0.001(4) 0.001(4) C312 0.055(6) 0.065(6) 0.062(6) -0.017(6) 0.001(5) -0.006(5) C313 0.046(6) 0.085(7) 0.101(9) -0.012(7) 0.031(6) -0.022(6) C314 0.056(6) 0.083(7) 0.063(6) -0.005(6) 0.026(6) 0.009(6) C315 0.055(6) 0.061(6) 0.074(7) -0.012(6) 0.013(6) 0.003(5) C316 0.039(5) 0.049(5) 0.058(6) -0.007(5) 0.007(5) 0.001(4) C321 0.062(5) 0.037(5) 0.027(4) 0.007(4) -0.009(4) -0.009(5) C322 0.044(5) 0.054(5) 0.043(5) 0.003(5) -0.008(4) 0.009(5) C323 0.078(7) 0.098(8) 0.049(6) 0.017(6) -0.020(6) 0.018(7) C324 0.115(9) 0.100(9) 0.036(6) 0.022(6) -0.013(7) 0.013(9) C325 0.084(8) 0.150(12) 0.058(7) 0.052(7) 0.011(7) -0.012(9) C326 0.069(6) 0.100(8) 0.040(5) 0.021(6) -0.003(5) -0.012(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 Fe1 C11 1.750(9) . ? Fe1 C1 1.863(9) . ? Fe1 P3 2.232(2) . ? Fe1 P1 2.232(3) . ? Fe1 S 2.244(2) . ? Fe1 Fe2 2.5027(16) . ? Fe1 Fe3 2.5954(14) . ? Fe2 C22 1.755(9) . ? Fe2 C21 1.757(9) . ? Fe2 C1 2.130(9) . ? Fe2 P2 2.171(2) . ? Fe2 S 2.237(2) . ? Fe2 Fe3 2.5312(14) . ? Fe3 C32 1.761(8) . ? Fe3 C31 1.775(8) . ? Fe3 P3 2.221(2) . ? Fe3 P2 2.235(2) . ? Fe3 S 2.265(2) . ? P1 C131 1.828(8) . ? P1 C121 1.831(8) . ? P1 C111 1.825(8) . ? P2 C211 1.834(7) . ? P2 C221 1.837(8) . ? P3 C311 1.817(7) . ? P3 C321 1.822(7) . ? C1 O1 1.180(9) . ? C11 O11 1.153(9) . ? C22 O22 1.152(9) . ? C31 O31 1.143(8) . ? C32 O32 1.153(8) . ? C21 O21 1.162(9) . ? C111 C112 1.380(11) . ? C111 C116 1.390(10) . ? C112 C113 1.386(10) . ? C113 C114 1.381(12) . ? C114 C115 1.356(11) . ? C115 C116 1.384(10) . ? C211 C212 1.364(10) . ? C211 C216 1.384(10) . ? C212 C213 1.388(11) . ? C213 C214 1.384(13) . ? C214 C215 1.359(13) . ? C215 C216 1.392(11) . ? C221 C222 1.390(10) . ? C221 C226 1.369(10) . ? C222 C223 1.380(10) . ? C223 C224 1.374(11) . ? C224 C225 1.354(11) . ? C225 C226 1.371(11) . ? C311 C316 1.375(10) . ? C311 C312 1.394(10) . ? C312 C313 1.374(11) . ? C313 C314 1.377(12) . ? C314 C315 1.356(11) . ? C315 C316 1.377(10) . ? C321 C322 1.381(10) . ? C321 C326 1.382(10) . ? C322 C323 1.370(10) . ? C323 C324 1.356(13) . ? C324 C325 1.369(13) . ? C325 C326 1.388(11) . ? 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 C11 Fe1 C1 85.4(4) . . ? C11 Fe1 P3 91.8(3) . . ? C1 Fe1 P3 167.0(3) . . ? C11 Fe1 P1 97.6(3) . . ? C1 Fe1 P1 93.2(3) . . ? P3 Fe1 P1 99.69(9) . . ? C11 Fe1 S 162.1(3) . . ? C1 Fe1 S 93.6(3) . . ? P3 Fe1 S 85.25(8) . . ? P1 Fe1 S 100.28(9) . . ? C11 Fe1 Fe2 110.1(3) . . ? C1 Fe1 Fe2 56.1(3) . . ? P3 Fe1 Fe2 113.65(7) . . ? P1 Fe1 Fe2 135.00(8) . . ? S Fe1 Fe2 55.91(6) . . ? C11 Fe1 Fe3 109.2(3) . . ? C1 Fe1 Fe3 115.0(3) . . ? P3 Fe1 Fe3 54.15(6) . . ? P1 Fe1 Fe3 141.85(8) . . ? S Fe1 Fe3 55.23(6) . . ? Fe2 Fe1 Fe3 59.50(4) . . ? C22 Fe2 C21 99.1(4) . . ? C22 Fe2 C1 93.3(4) . . ? C21 Fe2 C1 88.7(4) . . ? C22 Fe2 P2 101.9(3) . . ? C21 Fe2 P2 93.2(3) . . ? C1 Fe2 P2 164.2(2) . . ? C22 Fe2 S 106.2(3) . . ? C21 Fe2 S 154.5(3) . . ? C1 Fe2 S 86.9(3) . . ? P2 Fe2 S 84.63(8) . . ? C22 Fe2 Fe1 132.0(3) . . ? C21 Fe2 Fe1 103.9(3) . . ? C1 Fe2 Fe1 46.6(2) . . ? P2 Fe2 Fe1 117.97(7) . . ? S Fe2 Fe1 56.18(6) . . ? C22 Fe2 Fe3 150.2(3) . . ? C21 Fe2 Fe3 101.7(3) . . ? C1 Fe2 Fe3 108.1(2) . . ? P2 Fe2 Fe3 56.14(6) . . ? S Fe2 Fe3 56.31(6) . . ? Fe1 Fe2 Fe3 62.07(4) . . ? C32 Fe3 C31 102.5(4) . . ? C32 Fe3 P3 93.0(3) . . ? C31 Fe3 P3 94.1(2) . . ? C32 Fe3 P2 97.3(3) . . ? C31 Fe3 P2 93.2(2) . . ? P3 Fe3 P2 165.78(9) . . ? C32 Fe3 S 107.7(3) . . ? C31 Fe3 S 149.8(3) . . ? P3 Fe3 S 85.02(8) . . ? P2 Fe3 S 82.53(8) . . ? C32 Fe3 Fe2 145.3(3) . . ? C31 Fe3 Fe2 98.4(3) . . ? P3 Fe3 Fe2 112.98(7) . . ? P2 Fe3 Fe2 53.75(6) . . ? S Fe3 Fe2 55.27(6) . . ? C32 Fe3 Fe1 141.0(3) . . ? C31 Fe3 Fe1 101.0(3) . . ? P3 Fe3 Fe1 54.56(6) . . ? P2 Fe3 Fe1 111.98(7) . . ? S Fe3 Fe1 54.48(6) . . ? Fe2 Fe3 Fe1 58.43(4) . . ? C131 P1 C121 100.2(5) . . ? C131 P1 C111 104.1(4) . . ? C121 P1 C111 102.1(4) . . ? C131 P1 Fe1 116.2(3) . . ? C121 P1 Fe1 117.9(4) . . ? C111 P1 Fe1 114.2(3) . . ? C211 P2 C221 101.6(3) . . ? C211 P2 Fe2 121.2(3) . . ? C221 P2 Fe2 122.7(3) . . ? C211 P2 Fe3 121.8(3) . . ? C221 P2 Fe3 118.8(2) . . ? Fe2 P2 Fe3 70.11(7) . . ? C311 P3 C321 100.9(4) . . ? C311 P3 Fe3 117.7(2) . . ? C321 P3 Fe3 119.5(3) . . ? C311 P3 Fe1 121.7(3) . . ? C321 P3 Fe1 125.2(3) . . ? Fe3 P3 Fe1 71.29(7) . . ? Fe2 S Fe1 67.91(7) . . ? Fe2 S Fe3 68.42(7) . . ? Fe1 S Fe3 70.29(7) . . ? O1 C1 Fe1 151.8(8) . . ? O1 C1 Fe2 130.1(7) . . ? Fe1 C1 Fe2 77.3(3) . . ? O11 C11 Fe1 177.2(8) . . ? O22 C22 Fe2 177.7(10) . . ? O31 C31 Fe3 176.7(8) . . ? O32 C32 Fe3 178.9(8) . . ? O21 C21 Fe2 177.7(9) . . ? C112 C111 C116 118.2(7) . . ? C112 C111 P1 122.8(7) . . ? C116 C111 P1 118.9(7) . . ? C111 C112 C113 120.7(9) . . ? C114 C113 C112 120.4(9) . . ? C113 C114 C115 119.1(9) . . ? C116 C115 C114 121.2(10) . . ? C115 C116 C111 120.3(9) . . ? C212 C211 C216 118.9(8) . . ? C212 C211 P2 122.1(6) . . ? C216 C211 P2 118.8(7) . . ? C211 C212 C213 120.9(10) . . ? C214 C213 C212 119.5(11) . . ? C215 C214 C213 120.3(11) . . ? C214 C215 C216 119.7(11) . . ? C211 C216 C215 120.6(10) . . ? C222 C221 C226 118.9(8) . . ? C222 C221 P2 120.8(6) . . ? C226 C221 P2 120.2(7) . . ? C221 C222 C223 119.2(8) . . ? C224 C223 C222 120.9(9) . . ? C223 C224 C225 119.4(9) . . ? C224 C225 C226 120.4(8) . . ? C225 C226 C221 121.2(8) . . ? C316 C311 C312 116.9(8) . . ? C316 C311 P3 120.3(6) . . ? C312 C311 P3 122.8(6) . . ? C311 C312 C313 121.8(8) . . ? C314 C313 C312 119.2(9) . . ? C315 C314 C313 120.4(9) . . ? C314 C315 C316 120.0(9) . . ? C311 C316 C315 121.8(8) . . ? C322 C321 C326 117.4(7) . . ? C322 C321 P3 121.8(6) . . ? C326 C321 P3 120.8(6) . . ? C321 C322 C323 122.3(9) . . ? C324 C323 C322 119.5(9) . . ? C323 C324 C325 120.2(9) . . ? C324 C325 C326 120.3(10) . . ? C325 C326 C321 120.3(9) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.313 _refine_diff_density_min -0.305 _refine_diff_density_rms 0.077