[Fe2(m4-O)2(m-OH)6(m-O2CArTol)4Cl4(2-Ph2P(O)py)2] (7) data_043004t _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C122 H110 Cl12 Fe6 N2 O18 P2' _chemical_formula_weight 2714.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.508(2) _cell_length_b 15.852(3) _cell_length_c 15.904(3) _cell_angle_alpha 78.407(3) _cell_angle_beta 77.951(3) _cell_angle_gamma 63.832(3) _cell_volume 3185.5(9) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 620 _cell_measurement_theta_min 2.69 _cell_measurement_theta_max 17.31 _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.415 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1390 _exptl_absorpt_coefficient_mu 1.004 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23654 _diffrn_reflns_av_R_equivalents 0.1312 _diffrn_reflns_av_sigmaI/netI 0.2644 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11127 _reflns_number_gt 4907 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11127 _refine_ls_number_parameters 730 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.2173 _refine_ls_R_factor_gt 0.1032 _refine_ls_wR_factor_ref 0.2243 _refine_ls_wR_factor_gt 0.1827 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.996 _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 0.60909(11) 0.95137(10) 0.31030(9) 0.0181(4) Uani 1 1 d . . . Fe2 Fe 0.55383(11) 1.06421(10) 0.49489(9) 0.0160(4) Uani 1 1 d . . . Fe3 Fe 0.69049(11) 0.84640(10) 0.48855(10) 0.0202(4) Uani 1 1 d . . . N1 N 0.6973(9) 0.8281(9) -0.0219(7) 0.065(4) Uani 1 1 d . . . O1 O 0.6918(5) 0.9100(5) 0.1962(4) 0.0278(19) Uani 1 1 d . . . O2 O 0.7279(5) 0.8440(4) 0.3676(4) 0.0229(18) Uani 1 1 d . . . H2B H 0.7904 0.8008 0.3390 0.027 Uiso 1 1 calc R . . O3 O 0.5567(5) 0.9681(4) 0.4293(4) 0.0179(17) Uani 1 1 d . . . O4 O 0.5474(5) 0.8585(5) 0.3060(4) 0.0207(17) Uani 1 1 d . . . O5 O 0.6862(5) 1.0361(5) 0.2929(4) 0.0201(17) Uani 1 1 d . . . O6 O 0.6337(5) 1.1240(4) 0.4010(4) 0.0205(17) Uani 1 1 d . . . O7 O 0.4277(5) 1.1796(4) 0.4587(4) 0.0206(17) Uani 1 1 d . . . O8 O 0.5748(5) 1.1303(4) 0.5796(4) 0.0182(16) Uani 1 1 d U . . O9 O 0.6823(5) 0.9537(4) 0.5306(4) 0.0201(17) Uani 1 1 d . . . H9B H 0.7301 0.9549 0.5626 0.024 Uiso 1 1 calc R . . P1 P 0.7394(2) 0.8880(2) 0.10647(19) 0.0268(7) Uani 1 1 d . . . Cl1 Cl 0.4729(2) 1.0763(2) 0.2526(2) 0.0402(8) Uani 1 1 d . . . Cl2 Cl 0.8185(2) 0.7230(2) 0.5463(2) 0.0410(8) Uani 1 1 d . . . C1 C 0.7612(8) 0.9839(7) 0.0397(7) 0.024(3) Uani 1 1 d . . . C2 C 0.7531(9) 1.0560(9) 0.0798(7) 0.040(3) Uani 1 1 d . . . H2A H 0.7343 1.0544 0.1409 0.048 Uiso 1 1 calc R . . C3 C 0.7720(10) 1.1307(9) 0.0326(8) 0.046(4) Uani 1 1 d . . . H3A H 0.7643 1.1821 0.0597 0.055 Uiso 1 1 calc R . . C4 C 0.8026(10) 1.1287(10) -0.0557(8) 0.052(4) Uani 1 1 d . . . H4A H 0.8177 1.1788 -0.0895 0.062 Uiso 1 1 calc R . . C5 C 0.8113(9) 1.0568(9) -0.0947(8) 0.043(3) Uani 1 1 d . . . H5A H 0.8315 1.0568 -0.1555 0.052 Uiso 1 1 calc R . . C6 C 0.6587(9) 0.8589(8) 0.0556(7) 0.030(3) Uani 1 1 d . . . C7 C 0.7911(8) 0.9850(8) -0.0466(7) 0.032(3) Uani 1 1 d . . . H7A H 0.7980 0.9341 -0.0740 0.038 Uiso 1 1 calc R . . C8 C 0.6366(12) 0.8085(11) -0.0611(9) 0.066(5) Uani 1 1 d . . . H8A H 0.6629 0.7874 -0.1166 0.079 Uiso 1 1 calc R . . C9 C 0.5384(11) 0.8174(10) -0.0249(9) 0.057(4) Uani 1 1 d . . . H9A H 0.4977 0.8036 -0.0551 0.068 Uiso 1 1 calc R . . C10 C 0.5015(12) 0.8459(13) 0.0541(10) 0.090(6) Uani 1 1 d . . . H10A H 0.4346 0.8517 0.0815 0.108 Uiso 1 1 calc R . . C11 C 0.5660(12) 0.8673(12) 0.0960(9) 0.082(6) Uani 1 1 d . . . H11A H 0.5425 0.8872 0.1521 0.098 Uiso 1 1 calc R . . C12 C 0.8641(8) 0.7872(7) 0.1099(7) 0.025(3) Uani 1 1 d . . . C13 C 0.9502(9) 0.7828(9) 0.0508(8) 0.042(3) Uani 1 1 d . . . H13A H 0.9457 0.8323 0.0047 0.051 Uiso 1 1 calc R . . C14 C 1.0404(10) 0.7070(10) 0.0603(8) 0.047(4) Uani 1 1 d . . . H14A H 1.1001 0.7022 0.0195 0.057 Uiso 1 1 calc R . . C15 C 1.0477(11) 0.6368(10) 0.1277(9) 0.057(4) Uani 1 1 d . . . H15A H 1.1126 0.5846 0.1348 0.068 Uiso 1 1 calc R . . C16 C 0.9620(12) 0.6415(9) 0.1848(9) 0.057(4) Uani 1 1 d . . . H16A H 0.9670 0.5915 0.2306 0.068 Uiso 1 1 calc R . . C17 C 0.8704(10) 0.7159(8) 0.1772(8) 0.046(4) Uani 1 1 d . . . H17A H 0.8108 0.7194 0.2176 0.055 Uiso 1 1 calc R . . C18 C 0.4723(7) 0.8424(7) 0.3497(6) 0.017(2) Uani 1 1 d . . . C19 C 0.4358(9) 0.7850(8) 0.3103(6) 0.025(3) Uani 1 1 d . . . C20 C 0.5025(9) 0.6921(8) 0.2952(7) 0.029(3) Uani 1 1 d . . . C21 C 0.4640(10) 0.6420(8) 0.2620(8) 0.041(3) Uani 1 1 d . . . H21A H 0.5084 0.5797 0.2484 0.049 Uiso 1 1 calc R . . C22 C 0.3615(12) 0.6814(10) 0.2482(8) 0.052(4) Uani 1 1 d . . . H22A H 0.3365 0.6449 0.2267 0.062 Uiso 1 1 calc R . . C23 C 0.2958(10) 0.7707(9) 0.2645(7) 0.037(3) Uani 1 1 d . . . H23A H 0.2254 0.7959 0.2554 0.044 Uiso 1 1 calc R . . C24 C 0.3327(8) 0.8258(8) 0.2951(6) 0.023(3) Uani 1 1 d . . . C25 C 0.6081(10) 0.6421(8) 0.3178(8) 0.032(3) Uani 1 1 d . . . C26 C 0.6276(9) 0.6478(8) 0.3976(8) 0.037(3) Uani 1 1 d . . . H26A H 0.5731 0.6867 0.4362 0.044 Uiso 1 1 calc R . . C27 C 0.7244(11) 0.5978(8) 0.4211(8) 0.047(4) Uani 1 1 d . . . H27A H 0.7368 0.6045 0.4752 0.056 Uiso 1 1 calc R . . C28 C 0.8066(10) 0.5365(9) 0.3672(10) 0.051(4) Uani 1 1 d . . . C29 C 0.7838(11) 0.5338(9) 0.2884(9) 0.053(4) Uani 1 1 d . . . H29A H 0.8370 0.4945 0.2494 0.063 Uiso 1 1 calc R . . C30 C 0.6874(10) 0.5855(8) 0.2643(8) 0.041(3) Uani 1 1 d . . . H30A H 0.6755 0.5818 0.2089 0.050 Uiso 1 1 calc R . . C31 C 0.9142(10) 0.4798(10) 0.3993(10) 0.077(5) Uani 1 1 d . . . H31A H 0.9630 0.4404 0.3553 0.116 Uiso 1 1 calc R . . H31B H 0.9074 0.4394 0.4534 0.116 Uiso 1 1 calc R . . H31C H 0.9400 0.5241 0.4094 0.116 Uiso 1 1 calc R . . C32 C 0.2618(8) 0.9248(8) 0.3074(7) 0.026(3) Uani 1 1 d . . . C33 C 0.2880(9) 1.0000(8) 0.2639(7) 0.032(3) Uani 1 1 d . . . H33A H 0.3535 0.9855 0.2290 0.039 Uiso 1 1 calc R . . C34 C 0.2227(9) 1.0922(9) 0.2703(7) 0.038(3) Uani 1 1 d . . . H34A H 0.2435 1.1408 0.2412 0.045 Uiso 1 1 calc R . . C35 C 0.1256(9) 1.1156(9) 0.3194(8) 0.038(3) Uani 1 1 d . . . C36 C 0.0979(10) 1.0431(11) 0.3624(8) 0.049(4) Uani 1 1 d . . . H36A H 0.0321 1.0584 0.3970 0.058 Uiso 1 1 calc R . . C37 C 0.1632(9) 0.9501(9) 0.3561(7) 0.037(3) Uani 1 1 d . . . H37A H 0.1415 0.9020 0.3851 0.044 Uiso 1 1 calc R . . C38 C 0.0520(10) 1.2203(9) 0.3245(9) 0.060(4) Uani 1 1 d . . . H38A H -0.0130 1.2250 0.3611 0.091 Uiso 1 1 calc R . . H38B H 0.0375 1.2523 0.2661 0.091 Uiso 1 1 calc R . . H38C H 0.0844 1.2505 0.3494 0.091 Uiso 1 1 calc R . . C39 C 0.6812(8) 1.1007(7) 0.3279(6) 0.017(2) Uani 1 1 d . . . C40 C 0.7427(8) 1.1569(8) 0.2774(6) 0.022(3) Uani 1 1 d . . . C41 C 0.8487(8) 1.1064(7) 0.2562(6) 0.023(3) Uani 1 1 d . . . C42 C 0.9039(9) 1.1563(9) 0.2081(7) 0.035(3) Uani 1 1 d . . . H42A H 0.9763 1.1229 0.1917 0.042 Uiso 1 1 calc R . . C43 C 0.8595(10) 1.2495(10) 0.1839(8) 0.044(4) Uani 1 1 d . . . H43A H 0.9000 1.2818 0.1519 0.053 Uiso 1 1 calc R . . C44 C 0.7520(10) 1.2995(8) 0.2065(7) 0.038(3) Uani 1 1 d . . . H44A H 0.7201 1.3661 0.1908 0.045 Uiso 1 1 calc R . . C45 C 0.6914(8) 1.2518(8) 0.2518(7) 0.026(3) Uani 1 1 d . . . C46 C 0.9026(8) 1.0041(8) 0.2851(7) 0.023(3) Uani 1 1 d U . . C47 C 0.8960(7) 0.9711(8) 0.3736(7) 0.027(3) Uani 1 1 d . . . H47A H 0.8571 1.0145 0.4147 0.033 Uiso 1 1 calc R . . C48 C 0.9464(8) 0.8748(8) 0.4017(8) 0.032(3) Uani 1 1 d . . . H48A H 0.9440 0.8539 0.4621 0.038 Uiso 1 1 calc R . . C49 C 0.9988(8) 0.8100(8) 0.3452(8) 0.031(3) Uani 1 1 d . . . C50 C 1.0536(9) 0.7076(8) 0.3747(8) 0.049(4) Uani 1 1 d . . . H50A H 1.0425 0.6968 0.4381 0.074 Uiso 1 1 calc R . . H50B H 1.1279 0.6865 0.3542 0.074 Uiso 1 1 calc R . . H50C H 1.0264 0.6718 0.3512 0.074 Uiso 1 1 calc R . . C51 C 1.0032(8) 0.8436(8) 0.2572(8) 0.031(3) Uani 1 1 d . . . H51A H 1.0400 0.8001 0.2160 0.037 Uiso 1 1 calc R . . C52 C 0.9556(8) 0.9382(8) 0.2290(7) 0.027(3) Uani 1 1 d . . . H52A H 0.9596 0.9586 0.1684 0.033 Uiso 1 1 calc R . . C53 C 0.5768(10) 1.3055(8) 0.2709(7) 0.034(3) Uani 1 1 d . . . C54 C 0.5117(9) 1.2757(8) 0.2461(7) 0.036(3) Uani 1 1 d . . . H54A H 0.5405 1.2202 0.2180 0.043 Uiso 1 1 calc R . . C55 C 0.4060(9) 1.3246(9) 0.2612(8) 0.042(3) Uani 1 1 d . . . H55A H 0.3632 1.3017 0.2440 0.050 Uiso 1 1 calc R . . C56 C 0.3608(10) 1.4052(9) 0.3005(8) 0.045(4) Uani 1 1 d . . . C57 C 0.4274(12) 1.4322(9) 0.3260(8) 0.048(4) Uani 1 1 d . . . H57A H 0.3987 1.4864 0.3558 0.057 Uiso 1 1 calc R . . C58 C 0.5334(10) 1.3850(8) 0.3108(8) 0.040(3) Uani 1 1 d . . . H58A H 0.5762 1.4079 0.3282 0.048 Uiso 1 1 calc R . . C59 C 0.2419(9) 1.4607(9) 0.3153(9) 0.068(5) Uani 1 1 d . . . H59A H 0.2240 1.5162 0.3440 0.102 Uiso 1 1 calc R . . H59B H 0.2108 1.4197 0.3520 0.102 Uiso 1 1 calc R . . H59C H 0.2154 1.4813 0.2594 0.102 Uiso 1 1 calc R . . C60 C 0.6869(10) 0.2812(9) 0.4874(8) 0.053(4) Uani 1 1 d . . . H60A H 0.6773 0.2478 0.5460 0.064 Uiso 1 1 calc R . . H60B H 0.6487 0.2691 0.4498 0.064 Uiso 1 1 calc R . . Cl3 Cl 0.8167(3) 0.2365(4) 0.4471(3) 0.0976(16) Uani 1 1 d . . . Cl4 Cl 0.6352(4) 0.4020(3) 0.4934(3) 0.1088(18) Uani 1 1 d . . . C61 C 0.900(2) 0.603(2) 0.989(2) 0.27(2) Uani 1 1 d . . . H61A H 0.8708 0.6658 1.0098 0.324 Uiso 1 1 calc R . . H61B H 0.9676 0.5639 1.0098 0.324 Uiso 1 1 calc R . . Cl5 Cl 0.8150(7) 0.5481(7) 1.0279(5) 0.227(4) Uani 1 1 d . . . Cl6 Cl 0.9144(8) 0.6159(5) 0.8798(7) 0.245(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0181(9) 0.0245(10) 0.0169(9) -0.0038(7) 0.0001(7) -0.0140(8) Fe2 0.0144(8) 0.0203(9) 0.0165(9) -0.0022(7) 0.0000(7) -0.0110(7) Fe3 0.0151(8) 0.0215(10) 0.0237(10) 0.0001(7) -0.0043(7) -0.0078(7) N1 0.078(9) 0.103(10) 0.053(8) -0.033(7) 0.003(7) -0.067(8) O1 0.036(5) 0.043(5) 0.017(4) -0.012(4) 0.006(4) -0.030(4) O2 0.011(4) 0.015(4) 0.031(5) -0.003(3) -0.001(3) 0.005(3) O3 0.030(4) 0.029(4) 0.011(4) -0.003(3) 0.004(3) -0.029(4) O4 0.020(4) 0.026(4) 0.025(4) -0.003(3) -0.002(3) -0.018(4) O5 0.022(4) 0.023(4) 0.023(4) -0.008(3) 0.002(3) -0.017(4) O6 0.022(4) 0.023(4) 0.022(4) -0.003(3) -0.001(3) -0.014(3) O7 0.015(4) 0.019(4) 0.029(4) -0.007(3) -0.001(3) -0.008(3) O8 0.023(4) 0.027(4) 0.017(4) -0.013(3) 0.001(3) -0.019(3) O9 0.020(4) 0.017(4) 0.024(4) -0.004(3) -0.009(3) -0.005(3) P1 0.0315(18) 0.0349(19) 0.0198(17) -0.0024(14) -0.0006(14) -0.0206(16) Cl1 0.0357(18) 0.0333(19) 0.056(2) 0.0136(15) -0.0252(16) -0.0183(15) Cl2 0.0305(18) 0.0350(19) 0.054(2) 0.0087(15) -0.0209(16) -0.0096(15) C1 0.024(6) 0.018(6) 0.027(7) -0.005(5) 0.000(5) -0.007(5) C2 0.044(8) 0.061(9) 0.019(7) 0.009(6) 0.002(6) -0.036(7) C3 0.074(10) 0.043(9) 0.033(8) -0.001(6) -0.004(7) -0.038(8) C4 0.067(10) 0.066(10) 0.038(9) 0.024(7) -0.017(8) -0.051(9) C5 0.049(9) 0.058(10) 0.034(8) -0.005(7) -0.005(7) -0.033(8) C6 0.039(8) 0.042(8) 0.021(7) -0.001(6) -0.002(6) -0.029(6) C7 0.030(7) 0.040(8) 0.028(7) -0.006(6) 0.003(6) -0.020(6) C8 0.076(11) 0.104(13) 0.049(10) -0.025(9) -0.005(9) -0.059(11) C9 0.066(10) 0.085(12) 0.045(10) -0.013(8) -0.024(8) -0.044(9) C10 0.068(12) 0.181(19) 0.059(12) -0.039(12) 0.006(9) -0.082(13) C11 0.082(12) 0.172(18) 0.031(9) -0.036(10) 0.015(8) -0.088(13) C12 0.029(7) 0.024(7) 0.024(7) -0.009(5) -0.005(5) -0.009(6) C13 0.032(8) 0.056(9) 0.040(8) -0.006(7) -0.009(6) -0.016(7) C14 0.036(8) 0.058(10) 0.040(9) -0.010(7) -0.001(7) -0.013(8) C15 0.052(10) 0.040(9) 0.058(11) -0.022(8) -0.015(8) 0.010(8) C16 0.076(11) 0.038(9) 0.060(10) -0.002(7) -0.002(9) -0.032(9) C17 0.043(8) 0.025(8) 0.054(9) -0.001(7) -0.008(7) -0.002(7) C18 0.012(6) 0.019(6) 0.013(6) -0.003(5) 0.001(5) -0.002(5) C19 0.040(7) 0.044(8) 0.010(6) 0.001(5) -0.004(5) -0.034(7) C20 0.045(8) 0.035(8) 0.017(6) -0.003(5) -0.005(6) -0.027(7) C21 0.053(9) 0.023(7) 0.053(9) -0.006(6) -0.014(7) -0.018(7) C22 0.084(12) 0.051(10) 0.049(9) -0.003(7) -0.017(8) -0.053(9) C23 0.045(8) 0.049(9) 0.028(7) 0.003(6) -0.012(6) -0.031(7) C24 0.028(7) 0.036(7) 0.016(6) 0.004(5) -0.006(5) -0.025(6) C25 0.049(8) 0.028(7) 0.033(8) 0.000(6) -0.008(7) -0.028(7) C26 0.028(7) 0.024(7) 0.051(9) 0.005(6) -0.003(6) -0.009(6) C27 0.080(11) 0.027(8) 0.041(9) 0.002(6) -0.012(8) -0.031(8) C28 0.044(9) 0.022(8) 0.081(12) 0.000(8) -0.003(8) -0.015(7) C29 0.062(10) 0.024(8) 0.056(10) -0.013(7) 0.012(8) -0.009(7) C30 0.041(8) 0.031(8) 0.048(9) -0.002(7) -0.005(7) -0.012(7) C31 0.056(10) 0.048(10) 0.091(13) 0.017(9) -0.013(9) 0.002(8) C32 0.022(6) 0.042(8) 0.026(7) -0.003(6) -0.007(5) -0.022(6) C33 0.025(7) 0.036(8) 0.036(8) 0.000(6) -0.012(6) -0.012(6) C34 0.038(8) 0.047(9) 0.035(8) -0.003(6) -0.007(6) -0.024(7) C35 0.024(7) 0.041(9) 0.046(9) -0.016(7) -0.018(6) 0.000(6) C36 0.027(8) 0.078(11) 0.049(9) -0.004(8) -0.008(7) -0.030(8) C37 0.029(7) 0.052(9) 0.039(8) 0.000(7) -0.010(6) -0.026(7) C38 0.046(9) 0.063(11) 0.080(12) -0.013(8) -0.017(8) -0.025(8) C39 0.018(6) 0.020(6) 0.011(6) -0.001(5) -0.005(5) -0.005(5) C40 0.028(7) 0.033(7) 0.007(6) 0.002(5) -0.004(5) -0.016(6) C41 0.028(7) 0.026(7) 0.019(6) -0.003(5) -0.004(5) -0.014(6) C42 0.031(7) 0.047(9) 0.034(8) 0.005(6) -0.008(6) -0.026(7) C43 0.048(9) 0.070(11) 0.036(8) 0.002(7) -0.003(7) -0.048(8) C44 0.063(9) 0.035(8) 0.029(7) 0.006(6) -0.013(7) -0.036(7) C45 0.033(7) 0.035(7) 0.023(7) 0.003(5) -0.011(5) -0.025(6) C46 0.016(5) 0.032(6) 0.028(6) -0.003(5) 0.001(4) -0.019(5) C47 0.009(6) 0.032(7) 0.043(8) -0.016(6) 0.001(5) -0.008(5) C48 0.022(6) 0.044(8) 0.032(7) -0.008(6) -0.005(6) -0.015(6) C49 0.022(7) 0.034(8) 0.047(8) 0.002(6) -0.006(6) -0.022(6) C50 0.052(9) 0.039(9) 0.054(9) -0.007(7) 0.007(7) -0.021(7) C51 0.014(6) 0.037(8) 0.048(8) -0.021(6) 0.003(6) -0.011(6) C52 0.019(6) 0.043(8) 0.018(6) -0.001(6) 0.000(5) -0.014(6) C53 0.054(9) 0.020(7) 0.031(7) 0.008(5) -0.007(6) -0.022(7) C54 0.038(8) 0.030(7) 0.038(8) -0.002(6) -0.007(6) -0.013(6) C55 0.028(7) 0.042(9) 0.059(9) 0.010(7) -0.021(7) -0.018(7) C56 0.044(9) 0.022(8) 0.050(9) 0.007(6) -0.006(7) -0.002(7) C57 0.078(11) 0.021(7) 0.037(8) 0.002(6) -0.014(8) -0.013(8) C58 0.051(9) 0.020(7) 0.046(9) 0.007(6) -0.016(7) -0.012(7) C59 0.045(9) 0.043(9) 0.085(12) 0.010(8) -0.006(8) 0.001(8) C60 0.075(10) 0.069(10) 0.046(9) 0.012(7) -0.018(8) -0.062(9) Cl3 0.060(3) 0.146(5) 0.094(4) -0.040(3) 0.008(3) -0.046(3) Cl4 0.147(5) 0.093(4) 0.102(4) -0.042(3) -0.032(3) -0.045(3) C61 0.35(5) 0.47(6) 0.20(3) -0.10(4) 0.05(3) -0.37(5) Cl5 0.225(9) 0.254(10) 0.160(8) -0.097(7) 0.026(6) -0.054(8) Cl6 0.318(12) 0.135(7) 0.253(11) -0.039(7) 0.050(9) -0.100(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 O3 1.911(6) . ? Fe1 O1 2.010(7) . ? Fe1 O2 2.036(6) . ? Fe1 O5 2.044(6) . ? Fe1 O4 2.049(6) . ? Fe1 Cl1 2.290(3) . ? Fe1 Fe3 3.157(2) . ? Fe2 O3 1.990(6) 2_676 ? Fe2 O3 1.993(6) . ? Fe2 O8 2.007(6) . ? Fe2 O9 2.007(6) . ? Fe2 O7 2.022(6) . ? Fe2 O6 2.036(7) . ? Fe2 Fe2 3.029(3) 2_676 ? Fe2 Fe3 3.143(2) . ? Fe2 Fe3 3.158(2) 2_676 ? Fe3 O2 1.890(7) . ? Fe3 O9 1.898(6) . ? Fe3 O7 1.922(6) 2_676 ? Fe3 Cl2 2.215(3) . ? Fe3 O3 2.260(7) . ? N1 C6 1.335(14) . ? N1 C8 1.345(15) . ? O1 P1 1.487(7) . ? O3 Fe2 1.990(6) 2_676 ? O4 C18 1.262(11) . ? O5 C39 1.231(11) . ? O6 C39 1.255(11) . ? O7 Fe3 1.922(6) 2_676 ? O8 C18 1.238(10) 2_676 ? P1 C1 1.781(10) . ? P1 C6 1.806(11) . ? P1 C12 1.813(11) . ? C1 C7 1.349(14) . ? C1 C2 1.369(14) . ? C2 C3 1.371(14) . ? C3 C4 1.384(16) . ? C4 C5 1.351(16) . ? C5 C7 1.348(15) . ? C6 C11 1.325(16) . ? C8 C9 1.376(18) . ? C9 C10 1.342(17) . ? C10 C11 1.438(18) . ? C12 C17 1.376(15) . ? C12 C13 1.381(14) . ? C13 C14 1.342(15) . ? C14 C15 1.366(17) . ? C15 C16 1.361(17) . ? C16 C17 1.342(16) . ? C18 O8 1.238(10) 2_676 ? C18 C19 1.515(13) . ? C19 C24 1.396(14) . ? C19 C20 1.396(14) . ? C20 C21 1.381(14) . ? C20 C25 1.466(15) . ? C21 C22 1.382(16) . ? C22 C23 1.355(16) . ? C23 C24 1.406(14) . ? C24 C32 1.474(14) . ? C25 C30 1.356(15) . ? C25 C26 1.384(15) . ? C26 C27 1.363(15) . ? C27 C28 1.410(17) . ? C28 C29 1.374(17) . ? C28 C31 1.555(17) . ? C29 C30 1.365(16) . ? C32 C37 1.400(14) . ? C32 C33 1.416(14) . ? C33 C34 1.357(14) . ? C34 C35 1.388(15) . ? C35 C36 1.389(16) . ? C35 C38 1.535(16) . ? C36 C37 1.368(16) . ? C39 C40 1.531(13) . ? C40 C45 1.370(13) . ? C40 C41 1.388(14) . ? C41 C42 1.383(14) . ? C41 C46 1.477(13) . ? C42 C43 1.336(15) . ? C43 C44 1.407(16) . ? C44 C45 1.401(14) . ? C45 C53 1.492(15) . ? C46 C52 1.364(14) . ? C46 C47 1.398(14) . ? C47 C48 1.395(14) . ? C48 C49 1.356(15) . ? C49 C51 1.392(15) . ? C49 C50 1.482(15) . ? C51 C52 1.368(14) . ? C53 C58 1.358(15) . ? C53 C54 1.377(14) . ? C54 C55 1.372(15) . ? C55 C56 1.366(16) . ? C56 C57 1.372(16) . ? C56 C59 1.542(16) . ? C57 C58 1.373(16) . ? C60 Cl3 1.722(13) . ? C60 Cl4 1.736(13) . ? C61 Cl6 1.69(3) . ? C61 Cl5 1.75(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Fe1 O1 167.1(3) . . ? O3 Fe1 O2 80.0(3) . . ? O1 Fe1 O2 87.1(3) . . ? O3 Fe1 O5 95.2(3) . . ? O1 Fe1 O5 84.3(3) . . ? O2 Fe1 O5 89.7(3) . . ? O3 Fe1 O4 95.2(3) . . ? O1 Fe1 O4 84.9(3) . . ? O2 Fe1 O4 89.8(3) . . ? O5 Fe1 O4 169.3(3) . . ? O3 Fe1 Cl1 97.0(2) . . ? O1 Fe1 Cl1 95.8(2) . . ? O2 Fe1 Cl1 176.8(2) . . ? O5 Fe1 Cl1 89.4(2) . . ? O4 Fe1 Cl1 91.7(2) . . ? O3 Fe1 Fe3 45.1(2) . . ? O1 Fe1 Fe3 122.0(2) . . ? O2 Fe1 Fe3 34.91(19) . . ? O5 Fe1 Fe3 93.29(19) . . ? O4 Fe1 Fe3 92.40(19) . . ? Cl1 Fe1 Fe3 142.16(11) . . ? O3 Fe2 O3 81.0(3) 2_676 . ? O3 Fe2 O8 96.8(3) 2_676 . ? O3 Fe2 O8 164.8(3) . . ? O3 Fe2 O9 101.5(3) 2_676 . ? O3 Fe2 O9 80.5(3) . . ? O8 Fe2 O9 85.3(3) . . ? O3 Fe2 O7 80.6(3) 2_676 . ? O3 Fe2 O7 101.6(3) . . ? O8 Fe2 O7 92.7(3) . . ? O9 Fe2 O7 177.3(3) . . ? O3 Fe2 O6 164.3(3) 2_676 . ? O3 Fe2 O6 98.5(3) . . ? O8 Fe2 O6 87.6(3) . . ? O9 Fe2 O6 93.9(3) . . ? O7 Fe2 O6 84.2(3) . . ? O3 Fe2 Fe2 40.53(18) 2_676 2_676 ? O3 Fe2 Fe2 40.45(17) . 2_676 ? O8 Fe2 Fe2 135.5(2) . 2_676 ? O9 Fe2 Fe2 91.3(2) . 2_676 ? O7 Fe2 Fe2 91.42(19) . 2_676 ? O6 Fe2 Fe2 136.9(2) . 2_676 ? O3 Fe2 Fe3 88.45(19) 2_676 . ? O3 Fe2 Fe3 45.73(19) . . ? O8 Fe2 Fe3 119.5(2) . . ? O9 Fe2 Fe3 35.24(18) . . ? O7 Fe2 Fe3 147.08(19) . . ? O6 Fe2 Fe3 102.49(19) . . ? Fe2 Fe2 Fe3 61.51(6) 2_676 . ? O3 Fe2 Fe3 45.40(19) 2_676 2_676 ? O3 Fe2 Fe3 87.99(19) . 2_676 ? O8 Fe2 Fe3 101.19(19) . 2_676 ? O9 Fe2 Fe3 146.5(2) . 2_676 ? O7 Fe2 Fe3 35.73(18) . 2_676 ? O6 Fe2 Fe3 119.02(19) . 2_676 ? Fe2 Fe2 Fe3 61.03(5) 2_676 2_676 ? Fe3 Fe2 Fe3 122.54(5) . 2_676 ? O2 Fe3 O9 115.5(3) . . ? O2 Fe3 O7 117.2(3) . 2_676 ? O9 Fe3 O7 109.7(3) . 2_676 ? O2 Fe3 Cl2 104.9(2) . . ? O9 Fe3 Cl2 105.9(2) . . ? O7 Fe3 Cl2 101.9(2) 2_676 . ? O2 Fe3 O3 74.9(2) . . ? O9 Fe3 O3 76.3(2) . . ? O7 Fe3 O3 76.2(2) 2_676 . ? Cl2 Fe3 O3 177.57(19) . . ? O2 Fe3 Fe2 100.37(19) . . ? O9 Fe3 Fe2 37.60(19) . . ? O7 Fe3 Fe2 89.97(19) 2_676 . ? Cl2 Fe3 Fe2 142.84(11) . . ? O3 Fe3 Fe2 39.16(15) . . ? O2 Fe3 Fe1 38.06(19) . . ? O9 Fe3 Fe1 97.1(2) . . ? O7 Fe3 Fe1 97.2(2) 2_676 . ? Cl2 Fe3 Fe1 142.86(11) . . ? O3 Fe3 Fe1 36.83(16) . . ? Fe2 Fe3 Fe1 67.72(5) . . ? C6 N1 C8 117.6(12) . . ? P1 O1 Fe1 172.0(5) . . ? Fe3 O2 Fe1 107.0(3) . . ? Fe1 O3 Fe2 129.0(3) . 2_676 ? Fe1 O3 Fe2 128.1(3) . . ? Fe2 O3 Fe2 99.0(3) 2_676 . ? Fe1 O3 Fe3 98.0(3) . . ? Fe2 O3 Fe3 95.8(3) 2_676 . ? Fe2 O3 Fe3 95.1(2) . . ? C18 O4 Fe1 134.0(7) . . ? C39 O5 Fe1 136.8(7) . . ? C39 O6 Fe2 131.1(6) . . ? Fe3 O7 Fe2 106.4(3) 2_676 . ? C18 O8 Fe2 134.2(6) 2_676 . ? Fe3 O9 Fe2 107.2(3) . . ? O1 P1 C1 112.4(5) . . ? O1 P1 C6 111.1(5) . . ? C1 P1 C6 108.2(5) . . ? O1 P1 C12 109.2(5) . . ? C1 P1 C12 107.4(5) . . ? C6 P1 C12 108.4(5) . . ? C7 C1 C2 119.6(10) . . ? C7 C1 P1 122.9(9) . . ? C2 C1 P1 117.4(8) . . ? C1 C2 C3 120.5(11) . . ? C2 C3 C4 117.9(12) . . ? C5 C4 C3 121.2(12) . . ? C7 C5 C4 119.4(12) . . ? C11 C6 N1 122.9(12) . . ? C11 C6 P1 119.7(10) . . ? N1 C6 P1 117.3(9) . . ? C5 C7 C1 121.4(11) . . ? N1 C8 C9 123.4(14) . . ? C10 C9 C8 118.5(13) . . ? C9 C10 C11 118.2(14) . . ? C6 C11 C10 119.3(13) . . ? C17 C12 C13 121.0(11) . . ? C17 C12 P1 116.5(9) . . ? C13 C12 P1 122.4(9) . . ? C14 C13 C12 118.4(12) . . ? C13 C14 C15 120.9(13) . . ? C16 C15 C14 120.0(13) . . ? C17 C16 C15 120.7(13) . . ? C16 C17 C12 118.9(13) . . ? O8 C18 O4 126.7(10) 2_676 . ? O8 C18 C19 117.1(9) 2_676 . ? O4 C18 C19 116.1(9) . . ? C24 C19 C20 121.8(10) . . ? C24 C19 C18 117.9(10) . . ? C20 C19 C18 120.1(9) . . ? C21 C20 C19 117.7(11) . . ? C21 C20 C25 117.7(11) . . ? C19 C20 C25 124.5(10) . . ? C20 C21 C22 120.7(12) . . ? C23 C22 C21 121.8(12) . . ? C22 C23 C24 119.4(12) . . ? C19 C24 C23 118.5(11) . . ? C19 C24 C32 122.9(9) . . ? C23 C24 C32 118.6(10) . . ? C30 C25 C26 118.4(12) . . ? C30 C25 C20 121.7(11) . . ? C26 C25 C20 119.9(11) . . ? C27 C26 C25 120.4(12) . . ? C26 C27 C28 121.7(13) . . ? C29 C28 C27 115.7(13) . . ? C29 C28 C31 125.5(13) . . ? C27 C28 C31 118.8(14) . . ? C30 C29 C28 122.4(13) . . ? C25 C30 C29 121.3(13) . . ? C37 C32 C33 116.6(11) . . ? C37 C32 C24 122.7(10) . . ? C33 C32 C24 120.5(10) . . ? C34 C33 C32 122.3(11) . . ? C33 C34 C35 120.1(12) . . ? C34 C35 C36 118.7(12) . . ? C34 C35 C38 119.4(12) . . ? C36 C35 C38 121.9(12) . . ? C37 C36 C35 121.4(12) . . ? C36 C37 C32 120.9(11) . . ? O5 C39 O6 127.2(10) . . ? O5 C39 C40 116.0(9) . . ? O6 C39 C40 116.8(9) . . ? C45 C40 C41 123.3(10) . . ? C45 C40 C39 119.6(9) . . ? C41 C40 C39 117.1(9) . . ? C42 C41 C40 117.2(10) . . ? C42 C41 C46 120.3(10) . . ? C40 C41 C46 122.4(9) . . ? C43 C42 C41 122.6(11) . . ? C42 C43 C44 119.2(11) . . ? C45 C44 C43 120.6(11) . . ? C40 C45 C44 116.9(11) . . ? C40 C45 C53 123.5(9) . . ? C44 C45 C53 119.6(10) . . ? C52 C46 C47 117.3(10) . . ? C52 C46 C41 123.0(10) . . ? C47 C46 C41 119.6(10) . . ? C48 C47 C46 120.2(10) . . ? C49 C48 C47 121.8(11) . . ? C48 C49 C51 117.3(11) . . ? C48 C49 C50 122.0(11) . . ? C51 C49 C50 120.6(11) . . ? C52 C51 C49 121.3(11) . . ? C46 C52 C51 122.0(11) . . ? C58 C53 C54 118.1(12) . . ? C58 C53 C45 122.1(11) . . ? C54 C53 C45 119.8(11) . . ? C55 C54 C53 121.2(12) . . ? C56 C55 C54 121.7(12) . . ? C55 C56 C57 115.8(12) . . ? C55 C56 C59 121.2(13) . . ? C57 C56 C59 123.0(13) . . ? C56 C57 C58 123.5(12) . . ? C53 C58 C57 119.6(12) . . ? Cl3 C60 Cl4 112.2(7) . . ? Cl6 C61 Cl5 107.8(15) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.028 _refine_diff_density_min -0.551 _refine_diff_density_rms 0.122