# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Stepnicka, P.' _publ_contact_author_name 'Dr P Stepnicka' _publ_contact_author_address ; Department of Inorganic Chemistry Charles University Hlavova 2030 Prague 2 128 40 CZECH REPUBLIC ; _publ_contact_author_email 'STEPNIC@MAIL.NATUR.CUNI.CZ' _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Synthesis, characterization and diastereoselective coordination ; data_amid _database_code_CSD 167918 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H32 Fe N O4 P' _chemical_formula_weight 557.39 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' _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+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 8.5942(1) _cell_length_b 16.0218(3) _cell_length_c 19.5448(3) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 90.0 _cell_volume 2691.21(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0 _cell_measurement_reflns_used 30385 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 27.1 _exptl_crystal_description bar _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.33 _exptl_crystal_density_diffrn 1.376 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1168 _exptl_absorpt_coefficient_mu 0.656 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 150 _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 'Nonius Kappa CCD' _diffrn_measurement_method ; CCD (rotation scans, rotation per image 1.8\% \w, exposure per frame 81 s, 277 images collected) ; _diffrn_detector_area_resol_mean 0.110 _diffrn_reflns_number 5920 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0346 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 27.13 _reflns_number_total 5920 _reflns_number_gt 5314 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR-92 (Giacovazzo, 1994)' _computing_structure_refinement '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^)+(0.0309P)^2^+1.3860P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom + difmap' _refine_ls_hydrogen_treatment 'free isotropic refinement' _refine_ls_extinction_method none _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.015(13) _refine_ls_number_reflns 5920 _refine_ls_number_parameters 462 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0425 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0741 _refine_ls_wR_factor_gt 0.0702 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 Fe Fe -0.29640(3) -0.137195(18) 0.615896(15) 0.01865(8) Uani 1 1 d . . . P P 0.07849(7) -0.07423(4) 0.64527(3) 0.02073(13) Uani 1 1 d . . . O1 O -0.36577(19) 0.09512(10) 0.60756(9) 0.0299(4) Uani 1 1 d . . . O2 O -0.10555(19) 0.07616(10) 0.60101(8) 0.0256(4) Uani 1 1 d . . . O3 O 0.1164(2) -0.06778(13) 0.57274(10) 0.0434(5) Uani 1 1 d . . . O4 O 0.2513(2) 0.16021(12) 0.42016(10) 0.0431(5) Uani 1 1 d . . . N N 0.1077(3) 0.08376(13) 0.49473(11) 0.0288(5) Uani 1 1 d . . . H90 H 0.102(3) 0.0401(16) 0.5202(12) 0.016(6) Uiso 1 1 d . . . C1 C -0.2502(3) -0.02462(13) 0.65833(11) 0.0198(5) Uani 1 1 d . . . C2 C -0.1226(3) -0.08238(14) 0.67026(11) 0.0190(5) Uani 1 1 d . . . C3 C -0.1864(3) -0.15105(14) 0.70866(11) 0.0212(5) Uani 1 1 d . . . H3 H -0.137(3) -0.1978(18) 0.7219(14) 0.031(8) Uiso 1 1 d . . . C4 C -0.3477(3) -0.13622(17) 0.71892(11) 0.0235(5) Uani 1 1 d . . . H4 H -0.415(3) -0.1703(17) 0.7395(13) 0.027(7) Uiso 1 1 d . . . C5 C -0.3873(3) -0.05917(15) 0.68835(12) 0.0225(5) Uani 1 1 d . . . H5 H -0.489(3) -0.0333(16) 0.6850(12) 0.024(7) Uiso 1 1 d . . . C6 C -0.2104(3) -0.16498(15) 0.52147(11) 0.0271(5) Uani 1 1 d . . . H6 H -0.106(3) -0.1501(18) 0.5080(13) 0.031(7) Uiso 1 1 d . . . C7 C -0.2503(3) -0.23926(15) 0.55645(13) 0.0306(6) Uani 1 1 d . . . H7 H -0.179(4) -0.281(2) 0.5658(16) 0.049(9) Uiso 1 1 d . . . C8 C -0.4106(3) -0.23630(15) 0.57281(13) 0.0293(6) Uani 1 1 d . . . H8 H -0.469(3) -0.2785(18) 0.5975(14) 0.037(8) Uiso 1 1 d . . . C9 C -0.4708(3) -0.15965(16) 0.54717(13) 0.0284(6) Uani 1 1 d . . . H9 H -0.575(4) -0.1418(18) 0.5499(13) 0.033(7) Uiso 1 1 d . . . C10 C -0.3476(3) -0.11641(16) 0.51535(12) 0.0260(6) Uani 1 1 d . . . H10 H -0.353(3) -0.0668(17) 0.4963(14) 0.026(7) Uiso 1 1 d . . . C11 C -0.2499(3) 0.05472(13) 0.61939(12) 0.0219(5) Uani 1 1 d . . . C12 C 0.1516(3) 0.01057(14) 0.69719(12) 0.0225(5) Uani 1 1 d . . . C13 C 0.0954(3) 0.02628(16) 0.76274(13) 0.0326(6) Uani 1 1 d . . . H13 H 0.012(4) -0.0065(18) 0.7796(14) 0.037(8) Uiso 1 1 d . . . C14 C 0.1585(4) 0.09056(18) 0.80163(15) 0.0387(7) Uani 1 1 d . . . H14 H 0.122(4) 0.099(2) 0.8423(18) 0.051(10) Uiso 1 1 d . . . C15 C 0.2779(3) 0.13930(16) 0.77489(14) 0.0342(6) Uani 1 1 d . . . H15 H 0.325(4) 0.1853(19) 0.8054(15) 0.047(9) Uiso 1 1 d . . . C16 C 0.3311(3) 0.12513(15) 0.70929(14) 0.0311(6) Uani 1 1 d . . . H16 H 0.418(4) 0.1580(19) 0.6909(14) 0.042(8) Uiso 1 1 d . . . C17 C 0.2680(3) 0.06092(14) 0.67046(13) 0.0252(5) Uani 1 1 d . . . H17 H 0.309(3) 0.0485(15) 0.6220(13) 0.027(6) Uiso 1 1 d . . . C18 C 0.1618(3) -0.16926(14) 0.67977(11) 0.0212(5) Uani 1 1 d . . . C19 C 0.1716(3) -0.23767(14) 0.63571(12) 0.0248(5) Uani 1 1 d . . . H19 H 0.141(4) -0.227(2) 0.5889(18) 0.056(10) Uiso 1 1 d . . . C20 C 0.2278(3) -0.31371(15) 0.65920(12) 0.0290(5) Uani 1 1 d . . . H20 H 0.234(3) -0.3628(16) 0.6306(12) 0.030(6) Uiso 1 1 d . . . C21 C 0.2750(3) -0.32233(16) 0.72711(12) 0.0291(6) Uani 1 1 d . . . H21 H 0.316(3) -0.3762(16) 0.7426(12) 0.025(6) Uiso 1 1 d . . . C22 C 0.2666(3) -0.25453(16) 0.77098(13) 0.0292(6) Uani 1 1 d . . . H22 H 0.302(4) -0.2571(17) 0.8167(15) 0.044(8) Uiso 1 1 d . . . C23 C 0.2101(3) -0.17872(15) 0.74769(12) 0.0266(5) Uani 1 1 d . . . H23 H 0.204(3) -0.1335(17) 0.7777(13) 0.031(7) Uiso 1 1 d . . . C24 C -0.0819(4) 0.15503(15) 0.56487(14) 0.0325(6) Uani 1 1 d . . . H24A H -0.002(3) 0.1832(17) 0.5907(13) 0.030(7) Uiso 1 1 d . . . H24B H -0.178(4) 0.1878(18) 0.5649(14) 0.040(8) Uiso 1 1 d . . . C25 C -0.0292(3) 0.13715(16) 0.49248(13) 0.0294(5) Uani 1 1 d . . . H25 H 0.002(3) 0.1896(17) 0.4713(14) 0.034(7) Uiso 1 1 d . . . C26 C -0.1616(3) 0.10216(19) 0.44752(14) 0.0395(7) Uani 1 1 d . . . H26 H -0.212(4) 0.0603(19) 0.4752(15) 0.048(9) Uiso 1 1 d . . . C27 C -0.1000(5) 0.0560(3) 0.3848(2) 0.0610(9) Uani 1 1 d . . . H27A H -0.191(5) 0.041(2) 0.355(2) 0.074(11) Uiso 1 1 d . . . H27B H -0.027(5) 0.003(3) 0.396(2) 0.089(13) Uiso 1 1 d . . . H27C H -0.040(5) 0.093(3) 0.357(2) 0.077(13) Uiso 1 1 d . . . C28 C -0.2704(5) 0.1722(3) 0.4272(2) 0.0625(10) Uani 1 1 d . . . H28A H -0.308(5) 0.203(2) 0.469(2) 0.072(12) Uiso 1 1 d . . . H28B H -0.350(5) 0.149(3) 0.393(2) 0.087(13) Uiso 1 1 d . . . H28C H -0.209(4) 0.210(2) 0.4005(17) 0.056(10) Uiso 1 1 d . . . C29 C 0.2378(3) 0.10037(15) 0.45847(13) 0.0305(6) Uani 1 1 d . . . C30 C 0.3697(4) 0.0398(2) 0.46954(17) 0.0411(7) Uani 1 1 d . . . H30A H 0.421(4) 0.023(2) 0.4255(17) 0.054(9) Uiso 1 1 d . . . H30B H 0.337(4) -0.014(2) 0.4876(17) 0.054(10) Uiso 1 1 d . . . H30C H 0.444(5) 0.067(2) 0.505(2) 0.076(12) Uiso 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 Fe 0.01916(15) 0.01867(14) 0.01814(14) -0.00210(13) -0.00044(13) -0.00088(13) P 0.0196(3) 0.0204(3) 0.0222(3) -0.0031(2) 0.0009(2) -0.0013(2) O1 0.0270(9) 0.0258(9) 0.0368(10) 0.0040(8) 0.0014(8) 0.0050(7) O2 0.0247(8) 0.0191(8) 0.0330(10) 0.0065(7) 0.0040(7) 0.0003(6) O3 0.0472(12) 0.0419(11) 0.0411(11) 0.0035(9) 0.0011(10) -0.0021(10) O4 0.0448(12) 0.0402(11) 0.0444(11) 0.0185(9) 0.0116(9) -0.0010(9) N 0.0329(12) 0.0251(11) 0.0284(11) 0.0115(9) 0.0040(9) 0.0037(9) C1 0.0200(12) 0.0201(10) 0.0194(10) -0.0032(8) -0.0002(9) -0.0003(9) C2 0.0216(12) 0.0196(11) 0.0160(10) -0.0019(8) -0.0015(9) -0.0016(9) C3 0.0244(12) 0.0201(12) 0.0190(10) 0.0005(9) -0.0019(9) -0.0034(10) C4 0.0260(12) 0.0253(11) 0.0193(11) 0.0004(10) 0.0044(9) -0.0016(11) C5 0.0207(13) 0.0245(12) 0.0224(12) -0.0047(9) 0.0020(10) 0.0004(10) C6 0.0301(14) 0.0338(13) 0.0173(11) -0.0086(9) -0.0009(11) -0.0011(12) C7 0.0414(17) 0.0238(12) 0.0266(13) -0.0094(10) -0.0062(11) 0.0036(11) C8 0.0371(14) 0.0251(13) 0.0258(13) -0.0032(10) -0.0062(12) -0.0079(11) C9 0.0245(14) 0.0348(14) 0.0258(13) -0.0035(10) -0.0089(10) -0.0031(11) C10 0.0336(14) 0.0259(13) 0.0184(11) -0.0011(9) -0.0041(10) -0.0022(10) C11 0.0246(12) 0.0205(10) 0.0205(10) -0.0037(9) 0.0009(10) 0.0000(9) C12 0.0218(12) 0.0194(11) 0.0263(12) 0.0000(9) -0.0025(10) 0.0006(9) C13 0.0363(16) 0.0265(13) 0.0350(15) -0.0072(11) 0.0064(13) -0.0083(12) C14 0.0481(18) 0.0350(15) 0.0332(15) -0.0142(12) 0.0013(13) -0.0036(13) C15 0.0361(14) 0.0224(11) 0.0441(14) -0.0074(11) -0.0108(12) -0.0010(13) C16 0.0232(13) 0.0231(12) 0.0469(15) 0.0018(11) -0.0068(11) -0.0029(10) C17 0.0191(12) 0.0241(11) 0.0325(13) 0.0020(10) -0.0025(10) 0.0005(9) C18 0.0182(12) 0.0224(11) 0.0231(11) -0.0026(9) 0.0014(9) -0.0015(9) C19 0.0253(13) 0.0264(12) 0.0225(12) -0.0011(9) -0.0014(9) 0.0017(10) C20 0.0361(15) 0.0239(12) 0.0271(12) -0.0018(10) 0.0021(11) 0.0025(11) C21 0.0301(14) 0.0280(13) 0.0292(13) 0.0062(10) -0.0005(11) 0.0039(11) C22 0.0274(14) 0.0348(13) 0.0253(13) 0.0021(10) -0.0032(11) 0.0007(11) C23 0.0240(12) 0.0307(12) 0.0250(12) -0.0059(10) -0.0009(11) 0.0002(11) C24 0.0345(14) 0.0193(13) 0.0436(15) 0.0067(11) 0.0030(13) 0.0007(11) C25 0.0282(13) 0.0245(12) 0.0354(13) 0.0104(12) 0.0009(10) 0.0015(11) C26 0.0391(17) 0.0456(16) 0.0336(15) 0.0158(13) -0.0040(12) -0.0057(13) C27 0.067(2) 0.078(3) 0.0387(17) -0.0021(19) -0.012(2) -0.005(2) C28 0.043(2) 0.066(2) 0.079(3) 0.026(2) -0.017(2) 0.0026(18) C29 0.0311(15) 0.0308(13) 0.0295(13) 0.0040(11) 0.0031(11) -0.0034(11) C30 0.0381(17) 0.0462(18) 0.0391(17) 0.0055(14) 0.0092(14) 0.0084(14) _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 Fe C1 2.024(2) . ? Fe C2 2.032(2) . ? Fe C6 2.037(2) . ? Fe C10 2.041(2) . ? Fe C5 2.044(2) . ? Fe C7 2.045(2) . ? Fe C9 2.045(2) . ? Fe C8 2.048(2) . ? Fe C3 2.057(2) . ? Fe C4 2.061(2) . ? P O3 1.458(2) . ? P C2 1.801(2) . ? P C12 1.808(2) . ? P C18 1.813(2) . ? O1 C11 1.210(3) . ? O2 C11 1.336(3) . ? O2 C24 1.462(3) . ? O4 C29 1.222(3) . ? N C29 1.350(3) . ? N C25 1.456(3) . ? C1 C5 1.428(3) . ? C1 C2 1.453(3) . ? C1 C11 1.482(3) . ? C2 C3 1.440(3) . ? C3 C4 1.420(3) . ? C4 C5 1.413(4) . ? C6 C7 1.415(4) . ? C6 C10 1.418(4) . ? C7 C8 1.414(4) . ? C8 C9 1.424(4) . ? C9 C10 1.410(4) . ? C12 C17 1.387(3) . ? C12 C13 1.392(4) . ? C13 C14 1.390(4) . ? C14 C15 1.392(4) . ? C15 C16 1.380(4) . ? C16 C17 1.389(3) . ? C18 C19 1.396(3) . ? C18 C23 1.399(3) . ? C19 C20 1.388(3) . ? C20 C21 1.395(3) . ? C21 C22 1.386(4) . ? C22 C23 1.385(3) . ? C24 C25 1.513(4) . ? C25 C26 1.543(4) . ? C26 C28 1.514(5) . ? C26 C27 1.525(5) . ? C29 C30 1.508(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Fe C2 41.98(9) . . ? C1 Fe C6 119.64(10) . . ? C2 Fe C6 107.54(10) . . ? C1 Fe C10 106.94(10) . . ? C2 Fe C10 126.25(10) . . ? C6 Fe C10 40.70(10) . . ? C1 Fe C5 41.10(9) . . ? C2 Fe C5 69.78(9) . . ? C6 Fe C5 154.14(10) . . ? C10 Fe C5 119.00(10) . . ? C1 Fe C7 155.13(11) . . ? C2 Fe C7 120.03(10) . . ? C6 Fe C7 40.56(10) . . ? C10 Fe C7 67.99(10) . . ? C5 Fe C7 163.09(10) . . ? C1 Fe C9 124.73(10) . . ? C2 Fe C9 163.38(10) . . ? C6 Fe C9 68.45(11) . . ? C10 Fe C9 40.37(10) . . ? C5 Fe C9 106.41(10) . . ? C7 Fe C9 68.16(11) . . ? C1 Fe C8 162.42(10) . . ? C2 Fe C8 154.45(10) . . ? C6 Fe C8 68.40(11) . . ? C10 Fe C8 68.11(10) . . ? C5 Fe C8 125.17(11) . . ? C7 Fe C8 40.44(11) . . ? C9 Fe C8 40.72(10) . . ? C1 Fe C3 69.20(9) . . ? C2 Fe C3 41.24(9) . . ? C6 Fe C3 127.46(10) . . ? C10 Fe C3 164.90(10) . . ? C5 Fe C3 68.34(10) . . ? C7 Fe C3 109.01(10) . . ? C9 Fe C3 153.77(10) . . ? C8 Fe C3 119.94(10) . . ? C1 Fe C4 68.60(10) . . ? C2 Fe C4 69.09(9) . . ? C6 Fe C4 164.60(10) . . ? C10 Fe C4 153.27(9) . . ? C5 Fe C4 40.27(10) . . ? C7 Fe C4 127.05(11) . . ? C9 Fe C4 119.10(10) . . ? C8 Fe C4 107.77(11) . . ? C3 Fe C4 40.34(10) . . ? O3 P C2 118.91(11) . . ? O3 P C12 114.50(12) . . ? C2 P C12 103.62(11) . . ? O3 P C18 109.44(12) . . ? C2 P C18 102.56(10) . . ? C12 P C18 106.57(10) . . ? C11 O2 C24 118.75(19) . . ? C29 N C25 122.5(2) . . ? C5 C1 C2 108.04(19) . . ? C5 C1 C11 123.0(2) . . ? C2 C1 C11 128.87(19) . . ? C5 C1 Fe 70.19(13) . . ? C2 C1 Fe 69.30(12) . . ? C11 C1 Fe 123.66(15) . . ? C3 C2 C1 106.44(19) . . ? C3 C2 P 124.20(17) . . ? C1 C2 P 129.36(16) . . ? C3 C2 Fe 70.28(13) . . ? C1 C2 Fe 68.72(12) . . ? P C2 Fe 126.50(11) . . ? C4 C3 C2 108.5(2) . . ? C4 C3 Fe 70.01(14) . . ? C2 C3 Fe 68.48(12) . . ? C5 C4 C3 108.8(2) . . ? C5 C4 Fe 69.21(13) . . ? C3 C4 Fe 69.65(13) . . ? C4 C5 C1 108.3(2) . . ? C4 C5 Fe 70.52(13) . . ? C1 C5 Fe 68.72(13) . . ? C7 C6 C10 107.5(2) . . ? C7 C6 Fe 70.00(14) . . ? C10 C6 Fe 69.80(14) . . ? C8 C7 C6 108.5(2) . . ? C8 C7 Fe 69.89(14) . . ? C6 C7 Fe 69.44(13) . . ? C7 C8 C9 107.7(2) . . ? C7 C8 Fe 69.67(14) . . ? C9 C8 Fe 69.53(14) . . ? C10 C9 C8 107.8(2) . . ? C10 C9 Fe 69.68(14) . . ? C8 C9 Fe 69.75(14) . . ? C9 C10 C6 108.5(2) . . ? C9 C10 Fe 69.95(14) . . ? C6 C10 Fe 69.50(13) . . ? O1 C11 O2 125.1(2) . . ? O1 C11 C1 123.8(2) . . ? O2 C11 C1 111.11(18) . . ? C17 C12 C13 119.4(2) . . ? C17 C12 P 118.42(18) . . ? C13 C12 P 122.13(19) . . ? C14 C13 C12 120.1(3) . . ? C13 C14 C15 119.9(3) . . ? C16 C15 C14 120.0(2) . . ? C15 C16 C17 120.0(2) . . ? C12 C17 C16 120.4(2) . . ? C19 C18 C23 118.8(2) . . ? C19 C18 P 116.98(17) . . ? C23 C18 P 124.13(17) . . ? C20 C19 C18 120.4(2) . . ? C19 C20 C21 120.2(2) . . ? C22 C21 C20 119.7(2) . . ? C23 C22 C21 120.1(2) . . ? C22 C23 C18 120.7(2) . . ? O2 C24 C25 109.2(2) . . ? N C25 C24 109.0(2) . . ? N C25 C26 113.6(2) . . ? C24 C25 C26 112.4(2) . . ? C28 C26 C27 111.2(3) . . ? C28 C26 C25 109.6(3) . . ? C27 C26 C25 112.2(3) . . ? O4 C29 N 123.7(2) . . ? O4 C29 C30 121.4(2) . . ? N C29 C30 114.8(2) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.13 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.219 _refine_diff_density_min -0.362 _refine_diff_density_rms 0.054 #===END data_hpfco _database_code_CSD 167919 _audit_creation_method SHELXL-97 _chemical_name_systematic ; (Sp)-2-(diphenylphosphinoyl)ferrocenecarboxylic acid ; _chemical_formula_sum 'C23 H19 Fe O3 P' _chemical_formula_weight 430.20 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' 'Fe' 'Fe' 0.3463 0.8444 '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' _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+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 8.7508(3) _cell_length_b 14.1915(6) _cell_length_c 15.6483(8) _cell_angle_alpha 90. _cell_angle_beta 90. _cell_angle_gamma 90. _cell_volume 1943.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150 _cell_measurement_reflns_used 10490 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description fragment _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.470 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 0.880 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 150 _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 'Nonius Kappa CCD' _diffrn_measurement_method ; CCD (rotation scans, rotation per image 2.0\% \w, exposure per frame 180 s, 102 images collected) ; _diffrn_detector_area_resol_mean 0.110 _diffrn_reflns_number 3383 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0455 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3383 _reflns_number_gt 3101 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR-92 (Giacovazzo, 1994)' _computing_structure_refinement '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^)+(0.0311P)^2^+1.4405P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.05(2) _refine_ls_number_reflns 3383 _refine_ls_number_parameters 257 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0446 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0828 _refine_ls_wR_factor_gt 0.0785 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 Fe Fe 0.55729(5) 0.19492(3) 0.72504(3) 0.02711(14) Uani 1 1 d . . . P P 0.19012(9) 0.14807(6) 0.66093(6) 0.0274(2) Uani 1 1 d . . . O1 O 0.3880(2) 0.18591(17) 0.50077(14) 0.0319(5) Uani 1 1 d . . . O2 O 0.6439(3) 0.16628(17) 0.49901(17) 0.0316(6) Uani 1 1 d . . . O3 O 0.1564(3) 0.24679(19) 0.6438(2) 0.0550(8) Uani 1 1 d . . . C1 C 0.5120(3) 0.1173(2) 0.6200(2) 0.0253(7) Uani 1 1 d . . . C2 C 0.3848(3) 0.1132(2) 0.6791(2) 0.0254(7) Uani 1 1 d . . . C3 C 0.4422(4) 0.0738(2) 0.7571(2) 0.0269(7) Uani 1 1 d . . . H3 H 0.3856 0.0626 0.8063 0.032 Uiso 1 1 calc R . . C4 C 0.6009(4) 0.0547(2) 0.7462(2) 0.0268(8) Uani 1 1 d . . . H4 H 0.6656 0.0294 0.7874 0.032 Uiso 1 1 calc R . . C5 C 0.6438(4) 0.0808(2) 0.6619(2) 0.0286(8) Uani 1 1 d . . . H5 H 0.7408 0.0751 0.6382 0.034 Uiso 1 1 calc R . . C6 C 0.6123(5) 0.3274(2) 0.6832(3) 0.0494(11) Uani 1 1 d . . . H6 H 0.6188 0.3469 0.6265 0.059 Uiso 1 1 calc R . . C7 C 0.4821(5) 0.3299(2) 0.7337(3) 0.0527(12) Uani 1 1 d . . . H7 H 0.3861 0.3509 0.7167 0.063 Uiso 1 1 calc R . . C8 C 0.5208(5) 0.2948(3) 0.8158(3) 0.0496(10) Uani 1 1 d . . . H8 H 0.4554 0.2891 0.8624 0.060 Uiso 1 1 calc R . . C9 C 0.6759(5) 0.2701(3) 0.8136(3) 0.0456(11) Uani 1 1 d . . . H9 H 0.7318 0.2447 0.8586 0.055 Uiso 1 1 calc R . . C10 C 0.7320(4) 0.2906(3) 0.7318(3) 0.0464(10) Uani 1 1 d . . . H10 H 0.8317 0.2813 0.7132 0.056 Uiso 1 1 calc R . . C11 C 0.5055(4) 0.1600(2) 0.5339(2) 0.0267(8) Uani 1 1 d . . . C12 C 0.1186(4) 0.0635(2) 0.5852(2) 0.0255(7) Uani 1 1 d . . . C13 C -0.0118(4) 0.0854(3) 0.5388(2) 0.0283(8) Uani 1 1 d . . . H13 H -0.0565 0.1445 0.5442 0.034 Uiso 1 1 calc R . . C14 C -0.0758(4) 0.0190(2) 0.4842(2) 0.0335(8) Uani 1 1 d . . . H14 H -0.1632 0.0343 0.4533 0.040 Uiso 1 1 calc R . . C15 C -0.0112(4) -0.0695(3) 0.4751(2) 0.0361(9) Uani 1 1 d . . . H15 H -0.0562 -0.1139 0.4394 0.043 Uiso 1 1 calc R . . C16 C 0.1208(4) -0.0912(2) 0.5196(2) 0.0372(9) Uani 1 1 d . . . H16 H 0.1669 -0.1497 0.5123 0.045 Uiso 1 1 calc R . . C17 C 0.1849(4) -0.0255(2) 0.5754(2) 0.0329(8) Uani 1 1 d . . . H17 H 0.2722 -0.0409 0.6062 0.040 Uiso 1 1 calc R . . C18 C 0.1012(3) 0.1172(2) 0.7622(2) 0.0320(8) Uani 1 1 d . . . C19 C 0.0882(4) 0.1857(3) 0.8247(2) 0.0404(9) Uani 1 1 d . . . H19 H 0.1184 0.2472 0.8132 0.048 Uiso 1 1 calc R . . C20 C 0.0302(5) 0.1625(3) 0.9050(3) 0.0531(12) Uani 1 1 d . . . H20 H 0.0221 0.2086 0.9470 0.064 Uiso 1 1 calc R . . C21 C -0.0154(5) 0.0716(4) 0.9223(3) 0.0556(12) Uani 1 1 d . . . H21 H -0.0533 0.0564 0.9761 0.067 Uiso 1 1 calc R . . C22 C -0.0050(5) 0.0034(3) 0.8607(3) 0.0554(12) Uani 1 1 d . . . H22 H -0.0370 -0.0578 0.8724 0.066 Uiso 1 1 calc R . . C23 C 0.0533(4) 0.0260(3) 0.7807(3) 0.0435(9) Uani 1 1 d . . . H23 H 0.0604 -0.0205 0.7390 0.052 Uiso 1 1 calc R . . H90 H 0.640(4) 0.196(3) 0.458(2) 0.030(11) Uiso 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 Fe 0.0274(2) 0.0206(2) 0.0333(3) 0.0014(2) -0.0075(2) -0.0024(2) P 0.0222(4) 0.0267(5) 0.0332(5) -0.0022(4) -0.0011(4) 0.0007(3) O1 0.0250(11) 0.0374(14) 0.0333(13) 0.0050(12) -0.0048(10) 0.0026(11) O2 0.0254(12) 0.0350(14) 0.0344(15) 0.0113(13) 0.0023(11) 0.0007(10) O3 0.0613(19) 0.0452(17) 0.058(2) 0.0048(15) -0.0022(16) 0.0047(14) C1 0.0246(16) 0.0202(16) 0.0312(18) 0.0024(15) -0.0040(14) -0.0021(13) C2 0.0232(15) 0.0209(16) 0.032(2) 0.0026(15) -0.0030(14) -0.0017(13) C3 0.0262(15) 0.0233(16) 0.0311(19) 0.0021(14) -0.0007(15) -0.0012(14) C4 0.0268(17) 0.0233(16) 0.030(2) 0.0051(14) -0.0057(14) 0.0015(13) C5 0.0216(16) 0.0232(17) 0.041(2) 0.0039(17) 0.0001(16) 0.0002(13) C6 0.070(3) 0.024(2) 0.054(3) 0.0031(18) -0.019(2) -0.0124(18) C7 0.052(2) 0.0216(19) 0.085(3) -0.012(2) -0.020(3) 0.0020(16) C8 0.060(3) 0.035(2) 0.053(3) -0.013(2) -0.003(2) -0.004(2) C9 0.055(2) 0.036(2) 0.046(3) -0.0010(19) -0.022(2) -0.0123(19) C10 0.045(2) 0.034(2) 0.060(3) 0.000(2) -0.014(2) -0.0158(17) C11 0.0220(16) 0.0250(17) 0.0332(19) -0.0060(15) -0.0034(14) -0.0018(13) C12 0.0224(15) 0.0278(18) 0.0262(18) 0.0033(15) -0.0002(14) -0.0022(14) C13 0.0245(17) 0.0349(19) 0.0255(18) 0.0017(15) 0.0035(15) 0.0013(14) C14 0.0259(18) 0.045(2) 0.0295(19) -0.0029(17) -0.0029(16) 0.0028(17) C15 0.036(2) 0.044(2) 0.0280(19) -0.0086(17) -0.0035(16) -0.0096(17) C16 0.0383(19) 0.0253(18) 0.048(2) -0.0043(17) 0.0003(18) 0.0019(16) C17 0.0260(17) 0.0328(19) 0.040(2) -0.0010(17) -0.0079(16) 0.0015(15) C18 0.0195(15) 0.042(2) 0.035(2) 0.0016(17) -0.0005(15) 0.0034(14) C19 0.0352(19) 0.046(2) 0.040(2) -0.006(2) 0.0002(16) 0.0042(17) C20 0.045(2) 0.079(3) 0.036(2) -0.012(2) 0.0030(19) 0.024(2) C21 0.039(2) 0.088(4) 0.040(2) 0.013(3) 0.0064(19) 0.006(2) C22 0.045(2) 0.069(3) 0.052(3) 0.023(2) 0.008(2) -0.005(2) C23 0.0406(19) 0.050(2) 0.040(2) 0.0021(19) 0.003(2) -0.0026(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe C1 2.018(3) . ? Fe C7 2.030(3) . ? Fe C8 2.031(4) . ? Fe C9 2.034(4) . ? Fe C2 2.036(3) . ? Fe C5 2.042(3) . ? Fe C10 2.047(3) . ? Fe C6 2.048(4) . ? Fe C4 2.053(3) . ? Fe C3 2.054(3) . ? P O3 1.456(3) . ? P C2 1.796(3) . ? P C12 1.799(3) . ? P C18 1.819(4) . ? O1 C11 1.209(4) . ? O2 C11 1.332(4) . ? C1 C5 1.424(4) . ? C1 C2 1.448(4) . ? C1 C11 1.479(5) . ? C2 C3 1.433(5) . ? C3 C4 1.425(4) . ? C4 C5 1.421(5) . ? C6 C7 1.388(6) . ? C6 C10 1.396(5) . ? C7 C8 1.419(6) . ? C8 C9 1.402(6) . ? C9 C10 1.402(6) . ? C12 C13 1.388(4) . ? C12 C17 1.398(5) . ? C13 C14 1.389(5) . ? C14 C15 1.384(5) . ? C15 C16 1.384(5) . ? C16 C17 1.395(5) . ? C18 C19 1.383(5) . ? C18 C23 1.392(5) . ? C19 C20 1.394(5) . ? C20 C21 1.378(6) . ? C21 C22 1.369(7) . ? C22 C23 1.389(6) . ? 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 Fe C7 120.39(16) . . ? C1 Fe C8 156.82(15) . . ? C7 Fe C8 40.90(18) . . ? C1 Fe C9 160.35(15) . . ? C7 Fe C9 67.97(17) . . ? C8 Fe C9 40.36(17) . . ? C1 Fe C2 41.85(13) . . ? C7 Fe C2 108.72(14) . . ? C8 Fe C2 121.86(15) . . ? C9 Fe C2 156.68(16) . . ? C1 Fe C5 41.06(13) . . ? C7 Fe C5 154.25(18) . . ? C8 Fe C5 161.72(15) . . ? C9 Fe C5 123.82(16) . . ? C2 Fe C5 69.63(13) . . ? C1 Fe C10 123.44(16) . . ? C7 Fe C10 67.21(16) . . ? C8 Fe C10 67.58(18) . . ? C9 Fe C10 40.17(16) . . ? C2 Fe C10 161.84(15) . . ? C5 Fe C10 105.93(15) . . ? C1 Fe C6 106.67(15) . . ? C7 Fe C6 39.79(17) . . ? C8 Fe C6 67.70(18) . . ? C9 Fe C6 67.45(16) . . ? C2 Fe C6 125.77(15) . . ? C5 Fe C6 119.07(17) . . ? C10 Fe C6 39.85(16) . . ? C1 Fe C4 68.82(13) . . ? C7 Fe C4 164.60(17) . . ? C8 Fe C4 126.33(15) . . ? C9 Fe C4 107.67(15) . . ? C2 Fe C4 69.05(13) . . ? C5 Fe C4 40.59(14) . . ? C10 Fe C4 119.71(14) . . ? C6 Fe C4 153.82(16) . . ? C1 Fe C3 69.23(13) . . ? C7 Fe C3 127.91(16) . . ? C8 Fe C3 109.63(16) . . ? C9 Fe C3 121.52(15) . . ? C2 Fe C3 41.03(13) . . ? C5 Fe C3 68.65(13) . . ? C10 Fe C3 155.28(15) . . ? C6 Fe C3 164.01(15) . . ? C4 Fe C3 40.60(12) . . ? O3 P C2 119.09(16) . . ? O3 P C12 116.77(17) . . ? C2 P C12 104.46(15) . . ? O3 P C18 107.75(18) . . ? C2 P C18 101.64(15) . . ? C12 P C18 105.34(15) . . ? C5 C1 C2 108.3(3) . . ? C5 C1 C11 126.8(3) . . ? C2 C1 C11 124.7(3) . . ? C5 C1 Fe 70.40(19) . . ? C2 C1 Fe 69.73(18) . . ? C11 C1 Fe 121.7(2) . . ? C3 C2 C1 106.8(3) . . ? C3 C2 P 125.1(2) . . ? C1 C2 P 128.1(2) . . ? C3 C2 Fe 70.19(18) . . ? C1 C2 Fe 68.41(17) . . ? P C2 Fe 127.01(17) . . ? C4 C3 C2 108.3(3) . . ? C4 C3 Fe 69.67(18) . . ? C2 C3 Fe 68.78(18) . . ? C5 C4 C3 108.5(3) . . ? C5 C4 Fe 69.28(18) . . ? C3 C4 Fe 69.73(18) . . ? C4 C5 C1 108.0(3) . . ? C4 C5 Fe 70.1(2) . . ? C1 C5 Fe 68.55(18) . . ? C7 C6 C10 108.4(4) . . ? C7 C6 Fe 69.4(2) . . ? C10 C6 Fe 70.0(2) . . ? C6 C7 C8 108.1(4) . . ? C6 C7 Fe 70.8(2) . . ? C8 C7 Fe 69.6(2) . . ? C9 C8 C7 107.3(4) . . ? C9 C8 Fe 69.9(2) . . ? C7 C8 Fe 69.5(2) . . ? C10 C9 C8 108.0(4) . . ? C10 C9 Fe 70.4(2) . . ? C8 C9 Fe 69.7(2) . . ? C6 C10 C9 108.3(4) . . ? C6 C10 Fe 70.1(2) . . ? C9 C10 Fe 69.4(2) . . ? O1 C11 O2 125.3(3) . . ? O1 C11 C1 123.2(3) . . ? O2 C11 C1 111.5(3) . . ? C13 C12 C17 119.1(3) . . ? C13 C12 P 118.8(3) . . ? C17 C12 P 122.0(3) . . ? C12 C13 C14 120.1(3) . . ? C15 C14 C13 120.9(3) . . ? C16 C15 C14 119.4(3) . . ? C15 C16 C17 120.2(3) . . ? C16 C17 C12 120.4(3) . . ? C19 C18 C23 118.8(3) . . ? C19 C18 P 118.8(3) . . ? C23 C18 P 122.3(3) . . ? C18 C19 C20 120.1(4) . . ? C21 C20 C19 120.2(4) . . ? C22 C21 C20 120.3(4) . . ? C21 C22 C23 119.7(4) . . ? C22 C23 C18 120.8(4) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.219 _refine_diff_density_min -0.382 _refine_diff_density_rms 0.058 #===END data_cyrupfc _database_code_CSD 167920 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C33H32ClFeO2PRu * 0.7 CH2Cl2' _chemical_formula_sum 'C33.70 H33.40 Cl2.40 Fe O2 P Ru' _chemical_formula_weight 743.37 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' 'Cl' 'Cl' 0.1484 0.1585 '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' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P41212' _symmetry_Int_Tables_number 92 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, -z+3/4' '-x+1/2, y+1/2, -z+1/4' '-y, -x, -z+1/2' 'y, x, -z' 'y+1/2, -x+1/2, z+3/4' '-y+1/2, x+1/2, z+1/4' _cell_length_a 23.9653(2) _cell_length_b 23.9653(2) _cell_length_c 11.3015(1) _cell_angle_alpha 90. _cell_angle_beta 90. _cell_angle_gamma 90. _cell_volume 6490.9(1) _cell_formula_units_Z 8 _cell_measurement_temperature 150 _cell_measurement_reflns_used 115407 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description prism _exptl_crystal_colour 'rusty orange' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.23 _exptl_crystal_density_diffrn 1.521 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3019 _exptl_absorpt_coefficient_mu 1.188 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.609 _exptl_absorpt_correction_T_max 0.800 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 150 _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 'Nonius Kappa CCD' _diffrn_measurement_method ; CCD (rotation scans, rotation per image 1.4\% \w, exposure per frame 210 s, 350 images collected) ; _diffrn_detector_area_resol_mean 0.110 _diffrn_reflns_number 90352 _diffrn_reflns_av_R_equivalents 0.0581 _diffrn_reflns_av_sigmaI/netI 0.0209 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5727 _reflns_number_gt 5328 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR-92 (Giacovazzo, 1994)' _computing_structure_refinement '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^)+(0.0930P)^2^+6.5210P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(4) _refine_ls_number_reflns 5727 _refine_ls_number_parameters 357 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0539 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_ref 0.1460 _refine_ls_wR_factor_gt 0.1427 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _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 Ru Ru 0.21818(2) 0.12073(2) 0.70000(4) 0.05084(17) Uani 1 1 d . . . Fe Fe 0.32707(4) -0.03646(4) 0.57721(7) 0.0537(2) Uani 1 1 d . . . P P 0.27979(6) 0.05804(6) 0.78719(12) 0.0457(3) Uani 1 1 d . . . Cl Cl 0.29010(8) 0.14071(10) 0.55957(15) 0.0793(6) Uani 1 1 d . . . O1 O 0.1877(2) -0.0059(2) 0.4464(4) 0.0674(12) Uani 1 1 d . . . O2 O 0.1939(2) 0.06395(19) 0.5724(4) 0.0637(12) Uani 1 1 d . . . C1 C 0.2450(3) -0.0219(2) 0.6119(5) 0.0479(13) Uani 1 1 d . . . C2 C 0.2786(2) -0.0090(2) 0.7124(5) 0.0461(12) Uani 1 1 d . . . C3 C 0.3064(3) -0.0585(3) 0.7466(6) 0.0565(15) Uani 1 1 d . . . H3 H 0.3308 -0.0623 0.8102 0.068 Uiso 1 1 calc R . . C4 C 0.2905(3) -0.1015(3) 0.6667(6) 0.0650(17) Uani 1 1 d . . . H4 H 0.3029 -0.1382 0.6687 0.078 Uiso 1 1 calc R . . C5 C 0.2532(3) -0.0791(3) 0.5846(6) 0.0619(16) Uani 1 1 d . . . H5 H 0.2365 -0.0984 0.5226 0.074 Uiso 1 1 calc R . . C6 C 0.3470(3) 0.0098(4) 0.4339(6) 0.078(2) Uani 1 1 d . . . H6 H 0.3234 0.0344 0.3944 0.094 Uiso 1 1 calc R . . C7 C 0.3831(3) 0.0230(3) 0.5315(6) 0.0677(18) Uani 1 1 d . . . H7 H 0.3873 0.0577 0.5670 0.081 Uiso 1 1 calc R . . C8 C 0.4107(3) -0.0265(4) 0.5633(7) 0.076(2) Uani 1 1 d . . . H8 H 0.4366 -0.0303 0.6240 0.091 Uiso 1 1 calc R . . C9 C 0.3921(4) -0.0698(4) 0.4860(8) 0.089(3) Uani 1 1 d . . . H9 H 0.4034 -0.1070 0.4867 0.107 Uiso 1 1 calc R . . C10 C 0.3540(4) -0.0456(4) 0.4101(6) 0.086(3) Uani 1 1 d . . . H10 H 0.3355 -0.0647 0.3502 0.103 Uiso 1 1 calc R . . C11 C 0.2080(3) 0.0154(3) 0.5383(5) 0.0540(14) Uani 1 1 d . . . C12 C 0.3520(3) 0.0792(3) 0.8093(5) 0.0510(14) Uani 1 1 d . . . C13 C 0.3666(3) 0.1359(3) 0.8001(6) 0.0657(18) Uani 1 1 d . . . H13 H 0.3402 0.1623 0.7774 0.079 Uiso 1 1 calc R . . C14 C 0.4219(4) 0.1521(4) 0.8262(6) 0.081(2) Uani 1 1 d . . . H14 H 0.4320 0.1894 0.8191 0.098 Uiso 1 1 calc R . . C15 C 0.4600(3) 0.1151(4) 0.8605(6) 0.076(2) Uani 1 1 d . . . H15 H 0.4961 0.1268 0.8780 0.091 Uiso 1 1 calc R . . C16 C 0.4462(3) 0.0591(3) 0.8703(7) 0.0699(19) Uani 1 1 d . . . H16 H 0.4728 0.0331 0.8940 0.084 Uiso 1 1 calc R . . C17 C 0.3925(3) 0.0426(3) 0.8444(6) 0.0610(16) Uani 1 1 d . . . H17 H 0.3834 0.0050 0.8512 0.073 Uiso 1 1 calc R . . C18 C 0.2601(3) 0.0397(3) 0.9388(5) 0.0545(15) Uani 1 1 d . . . C19 C 0.2215(4) -0.0013(3) 0.9592(6) 0.075(2) Uani 1 1 d . . . H19 H 0.2077 -0.0217 0.8956 0.090 Uiso 1 1 calc R . . C20 C 0.2024(4) -0.0134(4) 1.0725(7) 0.087(3) Uani 1 1 d . . . H20 H 0.1761 -0.0414 1.0843 0.105 Uiso 1 1 calc R . . C21 C 0.2228(4) 0.0167(4) 1.1672(6) 0.082(3) Uani 1 1 d . . . H21 H 0.2109 0.0088 1.2437 0.099 Uiso 1 1 calc R . . C22 C 0.2620(4) 0.0593(4) 1.1463(6) 0.079(3) Uani 1 1 d . . . H22 H 0.2751 0.0804 1.2095 0.095 Uiso 1 1 calc R . . C23 C 0.2810(3) 0.0701(3) 1.0352(5) 0.0638(17) Uani 1 1 d . . . H23 H 0.3078 0.0976 1.0232 0.077 Uiso 1 1 calc R . . C24 C 0.1295(3) 0.1219(4) 0.7530(8) 0.085(2) Uani 1 1 d . . . C25 C 0.1354(4) 0.1633(4) 0.6636(7) 0.090(3) Uani 1 1 d . . . H25 H 0.1118 0.1635 0.5983 0.108 Uiso 1 1 calc R . . C26 C 0.1779(5) 0.2045(4) 0.6756(7) 0.095(3) Uani 1 1 d . . . H26 H 0.1815 0.2313 0.6166 0.114 Uiso 1 1 calc R . . C27 C 0.2150(5) 0.2066(3) 0.7730(7) 0.088(3) Uani 1 1 d . . . C28 C 0.2071(4) 0.1666(3) 0.8639(6) 0.070(2) Uani 1 1 d . . . H28 H 0.2299 0.1673 0.9305 0.084 Uiso 1 1 calc R . . C29 C 0.1641(3) 0.1251(4) 0.8542(6) 0.071(2) Uani 1 1 d . . . H29 H 0.1590 0.0998 0.9156 0.086 Uiso 1 1 calc R . . C30 C 0.0883(5) 0.0761(6) 0.7410(13) 0.138(5) Uani 1 1 d . . . H30A H 0.0901 0.0524 0.8094 0.165 Uiso 1 1 calc R . . H30B H 0.0966 0.0547 0.6714 0.165 Uiso 1 1 calc R . . H30C H 0.0515 0.0916 0.7343 0.165 Uiso 1 1 calc R . . C31 C 0.2559(6) 0.2506(3) 0.7911(12) 0.128(5) Uani 1 1 d . . . H31 H 0.2816 0.2334 0.8478 0.154 Uiso 1 1 calc R . . C32 C 0.2952(7) 0.2682(6) 0.6904(16) 0.190(8) Uani 1 1 d . . . H32A H 0.3095 0.2356 0.6516 0.227 Uiso 1 1 calc R . . H32B H 0.3256 0.2895 0.7222 0.227 Uiso 1 1 calc R . . H32C H 0.2750 0.2905 0.6343 0.227 Uiso 1 1 calc R . . C33 C 0.2353(2) 0.3003(2) 0.8580(5) 0.203(9) Uani 1 1 d . . . H33A H 0.2653 0.3264 0.8682 0.244 Uiso 1 1 calc R . . H33B H 0.2218 0.2888 0.9341 0.244 Uiso 1 1 calc R . . H33C H 0.2056 0.3178 0.8146 0.244 Uiso 1 1 calc R . . Cl91 Cl 0.3679(2) 0.3924(2) -0.0474(5) 0.115(2) Uiso 0.40 1 d PR . . Cl92 Cl 0.3677(2) 0.2741(2) 0.0109(5) 0.113(2) Uiso 0.40 1 d PR . . C91 C 0.3812(2) 0.3429(2) 0.0617(5) 0.083(5) Uiso 0.40 1 d PR . . H911 H 0.3575 0.3507 0.1316 0.100 Uiso 0.40 1 d PR . . H912 H 0.4207 0.3457 0.0866 0.100 Uiso 0.40 1 d PR . . Cl93 Cl 0.5985(2) 0.5984(2) 0.1294(5) 0.146(3) Uiso 0.15 1 d PR . . Cl94 Cl 0.5984(2) 0.5982(2) -0.1281(5) 0.146(3) Uiso 0.15 1 d PR . . C92 C 0.6275(2) 0.6275(2) 0.0000(5) 0.152(12) Uiso 0.30 2 d SPR . . H921 H 0.6683 0.6210 0.0024 0.182 Uiso 0.15 1 d PR . . H922 H 0.6211 0.6682 0.0025 0.182 Uiso 0.15 1 d PR . . Cl95 Cl 0.6376(2) 0.6698(2) 0.1199(5) 0.146(3) Uiso 0.15 1 d PR . . Cl96 Cl 0.6702(2) 0.6374(2) -0.1185(5) 0.146(3) Uiso 0.15 1 d PR . . C93 C 0.6246(2) 0.6246(2) 0.0000(5) 0.152(12) Uiso 0.30 2 d SPR . . H931 H 0.5855 0.6294 -0.0244 0.182 Uiso 0.15 1 d PR . . H932 H 0.6292 0.5857 0.0292 0.182 Uiso 0.15 1 d PR . . 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 Ru 0.0657(3) 0.0563(3) 0.0305(2) 0.0056(2) 0.0039(2) 0.0134(2) Fe 0.0644(5) 0.0660(5) 0.0307(4) -0.0008(4) 0.0005(4) 0.0131(4) P 0.0550(8) 0.0552(8) 0.0268(6) 0.0040(6) 0.0027(6) 0.0047(6) Cl 0.0687(10) 0.1282(16) 0.0410(8) 0.0304(9) -0.0023(8) -0.0089(10) O1 0.080(3) 0.076(3) 0.047(2) 0.000(2) -0.019(2) 0.007(2) O2 0.071(3) 0.063(3) 0.057(3) -0.007(2) -0.017(2) 0.014(2) C1 0.056(3) 0.054(3) 0.034(3) 0.004(2) 0.004(2) 0.001(3) C2 0.054(3) 0.056(3) 0.029(3) 0.007(2) 0.003(2) 0.003(3) C3 0.067(4) 0.058(3) 0.044(3) 0.010(3) 0.006(3) 0.014(3) C4 0.085(5) 0.058(4) 0.053(4) 0.008(3) -0.006(3) 0.011(3) C5 0.085(4) 0.054(3) 0.047(4) 0.001(3) -0.015(3) -0.006(3) C6 0.075(5) 0.128(7) 0.032(3) 0.016(4) 0.004(3) 0.000(4) C7 0.065(4) 0.095(5) 0.044(3) 0.015(3) 0.017(3) -0.001(4) C8 0.061(4) 0.116(6) 0.050(4) 0.010(4) 0.004(3) 0.013(4) C9 0.090(6) 0.111(7) 0.066(5) -0.009(5) 0.023(4) 0.026(5) C10 0.103(6) 0.118(7) 0.037(4) -0.022(4) 0.016(4) 0.009(5) C11 0.051(3) 0.068(4) 0.043(3) 0.011(3) -0.003(3) 0.003(3) C12 0.070(4) 0.061(3) 0.022(3) -0.004(2) -0.001(3) -0.001(3) C13 0.087(5) 0.070(4) 0.040(3) 0.005(3) -0.018(3) -0.018(3) C14 0.120(7) 0.082(5) 0.042(4) 0.008(4) -0.007(4) -0.035(5) C15 0.066(4) 0.112(7) 0.049(4) -0.007(4) -0.007(3) -0.007(4) C16 0.064(4) 0.083(5) 0.063(4) -0.011(4) -0.007(3) 0.001(4) C17 0.055(4) 0.071(4) 0.057(4) 0.001(3) -0.002(3) -0.003(3) C18 0.060(3) 0.068(4) 0.036(3) 0.017(3) 0.005(3) 0.018(3) C19 0.088(5) 0.094(5) 0.042(3) 0.029(4) 0.024(4) 0.025(4) C20 0.098(6) 0.104(6) 0.060(5) 0.028(5) 0.039(4) 0.012(5) C21 0.086(5) 0.120(7) 0.041(4) 0.026(4) 0.022(4) 0.033(5) C22 0.088(5) 0.113(6) 0.038(4) 0.006(4) -0.003(3) 0.054(5) C23 0.070(4) 0.084(5) 0.037(3) 0.006(3) 0.003(3) 0.029(4) C24 0.069(5) 0.110(6) 0.075(5) -0.016(5) 0.016(4) 0.028(5) C25 0.104(7) 0.116(7) 0.049(4) 0.005(4) 0.005(4) 0.071(6) C26 0.156(9) 0.082(6) 0.047(4) 0.013(4) 0.019(5) 0.054(6) C27 0.154(8) 0.060(4) 0.051(4) 0.005(3) 0.007(5) 0.034(5) C28 0.112(6) 0.065(4) 0.032(3) 0.001(3) 0.009(3) 0.027(4) C29 0.085(5) 0.084(5) 0.045(4) 0.009(4) 0.023(3) 0.033(4) C30 0.080(6) 0.189(13) 0.144(11) -0.066(10) 0.028(7) -0.006(7) C31 0.214(13) 0.045(4) 0.126(9) 0.004(5) 0.048(10) -0.017(6) C32 0.249(19) 0.116(10) 0.204(18) 0.016(11) 0.085(16) 0.071(12) C33 0.205(19) 0.140(13) 0.26(2) 0.000(14) 0.073(18) 0.004(12) _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 Ru O2 2.066(4) . ? Ru C28 2.171(6) . ? Ru C29 2.174(6) . ? Ru C24 2.209(8) . ? Ru C27 2.218(8) . ? Ru C26 2.244(8) . ? Ru C25 2.269(7) . ? Ru P 2.3253(15) . ? Ru Cl 2.3913(18) . ? Fe C10 2.008(7) . ? Fe C6 2.021(7) . ? Fe C7 2.024(7) . ? Fe C8 2.025(7) . ? Fe C2 2.029(5) . ? Fe C9 2.033(8) . ? Fe C1 2.036(6) . ? Fe C5 2.046(7) . ? Fe C3 2.047(6) . ? Fe C4 2.053(7) . ? P C2 1.816(6) . ? P C12 1.821(7) . ? P C18 1.831(6) . ? O1 C11 1.256(8) . ? O2 C11 1.271(8) . ? C1 C5 1.419(9) . ? C1 C2 1.427(8) . ? C1 C11 1.508(8) . ? C2 C3 1.416(8) . ? C3 C4 1.421(10) . ? C4 C5 1.395(9) . ? C6 C10 1.366(13) . ? C6 C7 1.436(10) . ? C7 C8 1.404(11) . ? C8 C9 1.429(13) . ? C9 C10 1.381(13) . ? C12 C17 1.367(9) . ? C12 C13 1.407(9) . ? C13 C14 1.414(11) . ? C14 C15 1.330(13) . ? C15 C16 1.387(12) . ? C16 C17 1.379(10) . ? C18 C19 1.371(11) . ? C18 C23 1.402(10) . ? C19 C20 1.390(9) . ? C20 C21 1.380(13) . ? C21 C22 1.407(13) . ? C22 C23 1.361(10) . ? C24 C29 1.416(11) . ? C24 C25 1.422(13) . ? C24 C30 1.483(14) . ? C25 C26 1.425(14) . ? C26 C27 1.415(14) . ? C27 C28 1.417(10) . ? C27 C31 1.453(15) . ? C28 C29 1.435(12) . ? C31 C33 1.496(11) . ? C31 C32 1.537(18) . ? Cl91 C91 0.677(4) 6 ? Cl91 Cl91 1.357(10) 6 ? Cl91 C91 1.7417 . ? Cl91 Cl92 2.359(5) 6 ? Cl92 C91 1.7738 . ? Cl92 Cl91 2.360(5) 6 ? C91 Cl91 0.677(4) 6 ? C91 C91 1.906(10) 6 ? Cl93 Cl94 0.017(10) 6 ? Cl93 C93 1.7099 . ? Cl93 C92 1.7638 . ? Cl93 Cl95 1.9533 . ? Cl93 Cl96 1.961(3) 6 ? Cl94 Cl93 0.017(10) 6 ? Cl94 C93 1.6998 . ? Cl94 C92 1.7543 . ? Cl94 Cl95 1.956(3) 6 ? Cl94 Cl96 1.9635 . ? C92 Cl96 1.701(9) 6 ? C92 Cl96 1.7012 . ? C92 Cl95 1.708(9) 6 ? C92 Cl95 1.7085 . ? C92 Cl94 1.754(9) 6 ? C92 Cl93 1.764(9) 6 ? Cl95 Cl96 0.019(11) 6 ? Cl95 C93 1.7624 . ? Cl95 Cl94 1.956(3) 6 ? Cl96 Cl95 0.019(11) 6 ? Cl96 C93 1.7556 . ? Cl96 Cl93 1.961(3) 6 ? C93 Cl94 1.700(9) 6 ? C93 Cl93 1.710(9) 6 ? C93 Cl96 1.755(9) 6 ? C93 Cl95 1.762(9) 6 ? 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 O2 Ru C28 153.5(3) . . ? O2 Ru C29 115.1(3) . . ? C28 Ru C29 38.6(3) . . ? O2 Ru C24 85.8(3) . . ? C28 Ru C24 69.1(3) . . ? C29 Ru C24 37.7(3) . . ? O2 Ru C27 149.4(3) . . ? C28 Ru C27 37.7(3) . . ? C29 Ru C27 68.7(3) . . ? C24 Ru C27 81.6(4) . . ? O2 Ru C26 112.5(3) . . ? C28 Ru C26 66.3(3) . . ? C29 Ru C26 78.4(3) . . ? C24 Ru C26 66.9(4) . . ? C27 Ru C26 37.0(4) . . ? O2 Ru C25 85.6(3) . . ? C28 Ru C25 79.6(3) . . ? C29 Ru C25 66.6(3) . . ? C24 Ru C25 37.0(3) . . ? C27 Ru C25 67.7(4) . . ? C26 Ru C25 36.8(4) . . ? O2 Ru P 92.81(13) . . ? C28 Ru P 92.52(19) . . ? C29 Ru P 94.00(19) . . ? C24 Ru P 120.3(3) . . ? C27 Ru P 117.6(2) . . ? C26 Ru P 154.5(3) . . ? C25 Ru P 157.3(3) . . ? O2 Ru Cl 82.61(16) . . ? C28 Ru Cl 123.6(2) . . ? C29 Ru Cl 162.1(3) . . ? C24 Ru Cl 150.6(3) . . ? C27 Ru Cl 94.9(3) . . ? C26 Ru Cl 92.8(3) . . ? C25 Ru Cl 114.8(2) . . ? P Ru Cl 87.31(6) . . ? C10 Fe C6 39.6(4) . . ? C10 Fe C7 67.9(4) . . ? C6 Fe C7 41.6(3) . . ? C10 Fe C8 67.8(4) . . ? C6 Fe C8 68.8(3) . . ? C7 Fe C8 40.6(3) . . ? C10 Fe C2 158.1(3) . . ? C6 Fe C2 124.1(3) . . ? C7 Fe C2 110.1(3) . . ? C8 Fe C2 125.9(3) . . ? C10 Fe C9 40.0(4) . . ? C6 Fe C9 68.2(4) . . ? C7 Fe C9 68.8(4) . . ? C8 Fe C9 41.2(4) . . ? C2 Fe C9 161.5(3) . . ? C10 Fe C1 120.7(3) . . ? C6 Fe C1 106.8(3) . . ? C7 Fe C1 124.7(3) . . ? C8 Fe C1 162.0(3) . . ? C2 Fe C1 41.1(2) . . ? C9 Fe C1 155.0(3) . . ? C10 Fe C5 105.2(3) . . ? C6 Fe C5 120.8(3) . . ? C7 Fe C5 159.4(3) . . ? C8 Fe C5 156.8(3) . . ? C2 Fe C5 68.6(3) . . ? C9 Fe C5 119.2(4) . . ? C1 Fe C5 40.7(3) . . ? C10 Fe C3 158.3(3) . . ? C6 Fe C3 161.6(3) . . ? C7 Fe C3 125.5(3) . . ? C8 Fe C3 110.0(3) . . ? C2 Fe C3 40.6(2) . . ? C9 Fe C3 123.9(3) . . ? C1 Fe C3 68.3(2) . . ? C5 Fe C3 67.9(3) . . ? C10 Fe C4 121.2(4) . . ? C6 Fe C4 155.8(3) . . ? C7 Fe C4 160.5(3) . . ? C8 Fe C4 123.4(3) . . ? C2 Fe C4 68.4(3) . . ? C9 Fe C4 106.2(3) . . ? C1 Fe C4 67.9(3) . . ? C5 Fe C4 39.8(3) . . ? C3 Fe C4 40.6(3) . . ? C2 P C12 109.0(3) . . ? C2 P C18 102.7(3) . . ? C12 P C18 100.6(3) . . ? C2 P Ru 111.38(19) . . ? C12 P Ru 118.8(2) . . ? C18 P Ru 112.81(19) . . ? C11 O2 Ru 137.7(4) . . ? C5 C1 C2 107.6(5) . . ? C5 C1 C11 122.3(6) . . ? C2 C1 C11 130.0(6) . . ? C5 C1 Fe 70.0(4) . . ? C2 C1 Fe 69.2(3) . . ? C11 C1 Fe 124.3(4) . . ? C3 C2 C1 107.6(5) . . ? C3 C2 P 127.4(5) . . ? C1 C2 P 124.8(4) . . ? C3 C2 Fe 70.4(4) . . ? C1 C2 Fe 69.8(3) . . ? P C2 Fe 129.0(3) . . ? C2 C3 C4 107.9(6) . . ? C2 C3 Fe 69.0(3) . . ? C4 C3 Fe 69.9(4) . . ? C5 C4 C3 108.4(6) . . ? C5 C4 Fe 69.8(4) . . ? C3 C4 Fe 69.5(4) . . ? C4 C5 C1 108.4(6) . . ? C4 C5 Fe 70.4(4) . . ? C1 C5 Fe 69.3(4) . . ? C10 C6 C7 106.9(8) . . ? C10 C6 Fe 69.7(5) . . ? C7 C6 Fe 69.3(4) . . ? C8 C7 C6 107.2(8) . . ? C8 C7 Fe 69.8(4) . . ? C6 C7 Fe 69.1(4) . . ? C7 C8 C9 108.1(7) . . ? C7 C8 Fe 69.7(4) . . ? C9 C8 Fe 69.7(5) . . ? C10 C9 C8 106.3(8) . . ? C10 C9 Fe 69.1(5) . . ? C8 C9 Fe 69.1(4) . . ? C6 C10 C9 111.6(8) . . ? C6 C10 Fe 70.7(4) . . ? C9 C10 Fe 71.0(5) . . ? O1 C11 O2 121.4(6) . . ? O1 C11 C1 116.3(6) . . ? O2 C11 C1 122.1(6) . . ? C17 C12 C13 117.8(6) . . ? C17 C12 P 122.4(5) . . ? C13 C12 P 119.6(5) . . ? C12 C13 C14 118.8(7) . . ? C15 C14 C13 121.5(8) . . ? C14 C15 C16 120.3(8) . . ? C17 C16 C15 119.0(7) . . ? C12 C17 C16 122.7(7) . . ? C19 C18 C23 118.9(6) . . ? C19 C18 P 120.2(5) . . ? C23 C18 P 120.7(5) . . ? C18 C19 C20 121.8(8) . . ? C21 C20 C19 119.3(9) . . ? C20 C21 C22 119.1(7) . . ? C23 C22 C21 121.1(8) . . ? C22 C23 C18 119.9(8) . . ? C29 C24 C25 118.5(9) . . ? C29 C24 C30 120.3(10) . . ? C25 C24 C30 121.2(10) . . ? C29 C24 Ru 69.8(4) . . ? C25 C24 Ru 73.8(5) . . ? C30 C24 Ru 127.3(7) . . ? C24 C25 C26 119.1(8) . . ? C24 C25 Ru 69.2(4) . . ? C26 C25 Ru 70.6(5) . . ? C27 C26 C25 123.2(8) . . ? C27 C26 Ru 70.5(4) . . ? C25 C26 Ru 72.5(4) . . ? C26 C27 C28 117.1(9) . . ? C26 C27 C31 124.0(9) . . ? C28 C27 C31 118.6(9) . . ? C26 C27 Ru 72.5(5) . . ? C28 C27 Ru 69.4(4) . . ? C31 C27 Ru 134.6(8) . . ? C27 C28 C29 120.6(8) . . ? C27 C28 Ru 73.0(4) . . ? C29 C28 Ru 70.8(4) . . ? C24 C29 C28 121.3(7) . . ? C24 C29 Ru 72.5(4) . . ? C28 C29 Ru 70.6(4) . . ? C27 C31 C33 115.3(10) . . ? C27 C31 C32 120.5(11) . . ? C33 C31 C32 110.9(8) . . ? C91 Cl91 Cl91 113.6(8) 6 6 ? C91 Cl91 C91 93.4(8) 6 . ? Cl91 Cl91 C91 20.86(6) 6 . ? C91 Cl91 Cl92 25.6(7) 6 6 ? Cl91 Cl91 Cl92 99.6(4) 6 6 ? C91 Cl91 Cl92 83.1(2) . 6 ? C91 Cl92 Cl91 9.5(3) . 6 ? Cl91 C91 Cl91 45.6(8) 6 . ? Cl91 C91 Cl92 144.9(9) 6 . ? Cl91 C91 Cl92 111.8 . . ? Cl91 C91 C91 65.8(8) 6 6 ? Cl91 C91 C91 20.8 . 6 ? Cl92 C91 C91 97.1(2) . 6 ? Cl94 Cl93 C93 52(10) 6 . ? Cl94 Cl93 C92 54(10) 6 . ? C93 Cl93 C92 2.8 . . ? Cl94 Cl93 Cl95 100(10) 6 . ? C93 Cl93 Cl95 57.1 . . ? C92 Cl93 Cl95 54.4 . . ? Cl94 Cl93 Cl96 99(10) 6 6 ? C93 Cl93 Cl96 56.6(3) . 6 ? C92 Cl93 Cl96 54.0(3) . 6 ? Cl95 Cl93 Cl96 0.5(3) . 6 ? Cl93 Cl94 C93 127(10) 6 . ? Cl93 Cl94 C92 125(10) 6 . ? C93 Cl94 C92 2.8 . . ? Cl93 Cl94 Cl95 79(10) 6 6 ? C93 Cl94 Cl95 57.1(3) . 6 ? C92 Cl94 Cl95 54.5(3) . 6 ? Cl93 Cl94 Cl96 80(10) 6 . ? C93 Cl94 Cl96 56.7 . . ? C92 Cl94 Cl96 54.1 . . ? Cl95 Cl94 Cl96 0.5(3) 6 . ? Cl96 C92 Cl96 116.90(19) 6 . ? Cl96 C92 Cl95 117.2 6 6 ? Cl96 C92 Cl95 0.6(3) . 6 ? Cl96 C92 Cl95 0.6(3) 6 . ? Cl96 C92 Cl95 117.2 . . ? Cl95 C92 Cl95 117.53(19) 6 . ? Cl96 C92 Cl94 69.2(4) 6 6 ? Cl96 C92 Cl94 161.0(3) . 6 ? Cl95 C92 Cl94 161.4(7) 6 6 ? Cl95 C92 Cl94 68.8(2) . 6 ? Cl96 C92 Cl94 161.0(3) 6 . ? Cl96 C92 Cl94 69.2 . . ? Cl95 C92 Cl94 68.8(2) 6 . ? Cl95 C92 Cl94 161.4 . . ? Cl94 C92 Cl94 111.2(2) 6 . ? Cl96 C92 Cl93 160.9(7) 6 6 ? Cl96 C92 Cl93 68.9(2) . 6 ? Cl95 C92 Cl93 68.4(4) 6 6 ? Cl95 C92 Cl93 161.3(3) . 6 ? Cl94 C92 Cl93 111.6 6 6 ? Cl94 C92 Cl93 0.4(2) . 6 ? Cl96 C92 Cl93 68.9(2) 6 . ? Cl96 C92 Cl93 160.9 . . ? Cl95 C92 Cl93 161.3(3) 6 . ? Cl95 C92 Cl93 68.4 . . ? Cl94 C92 Cl93 0.4(2) 6 . ? Cl94 C92 Cl93 111.6 . . ? Cl93 C92 Cl93 112.1(2) 6 . ? Cl96 Cl95 C92 66(10) 6 . ? Cl96 Cl95 C93 68(10) 6 . ? C92 Cl95 C93 2.8 . . ? Cl96 Cl95 Cl93 113(10) 6 . ? C92 Cl95 Cl93 57.1 . . ? C93 Cl95 Cl93 54.5 . . ? Cl96 Cl95 Cl94 113(10) 6 6 ? C92 Cl95 Cl94 56.7(3) . 6 ? C93 Cl95 Cl94 54.1(3) . 6 ? Cl93 Cl95 Cl94 0.5(3) . 6 ? Cl95 Cl96 C92 113(10) 6 . ? Cl95 Cl96 C93 111(10) 6 . ? C92 Cl96 C93 2.8 . . ? Cl95 Cl96 Cl93 66(10) 6 6 ? C92 Cl96 Cl93 57.1(3) . 6 ? C93 Cl96 Cl93 54.5(3) . 6 ? Cl95 Cl96 Cl94 66(10) 6 . ? C92 Cl96 Cl94 56.7 . . ? C93 Cl96 Cl94 54.0 . . ? Cl93 Cl96 Cl94 0.5(3) 6 . ? Cl94 C93 Cl94 116.80(19) 6 . ? Cl94 C93 Cl93 117.2 6 6 ? Cl94 C93 Cl93 0.4(2) . 6 ? Cl94 C93 Cl93 0.4(2) 6 . ? Cl94 C93 Cl93 117.2 . . ? Cl93 C93 Cl93 117.62(19) 6 . ? Cl94 C93 Cl96 69.2(4) 6 6 ? Cl94 C93 Cl96 161.0(3) . 6 ? Cl93 C93 Cl96 160.8(6) 6 6 ? Cl93 C93 Cl96 68.9(2) . 6 ? Cl94 C93 Cl96 161.0(3) 6 . ? Cl94 C93 Cl96 69.2 . . ? Cl93 C93 Cl96 68.9(2) 6 . ? Cl93 C93 Cl96 160.8 . . ? Cl96 C93 Cl96 111.3(2) 6 . ? Cl94 C93 Cl95 161.5(7) 6 6 ? Cl94 C93 Cl95 68.8(2) . 6 ? Cl93 C93 Cl95 68.4(4) 6 6 ? Cl93 C93 Cl95 161.3(3) . 6 ? Cl96 C93 Cl95 111.6 6 6 ? Cl96 C93 Cl95 0.6(3) . 6 ? Cl94 C93 Cl95 68.8(2) 6 . ? Cl94 C93 Cl95 161.5 . . ? Cl93 C93 Cl95 161.2(3) 6 . ? Cl93 C93 Cl95 68.4 . . ? Cl96 C93 Cl95 0.6(3) 6 . ? Cl96 C93 Cl95 111.6 . . ? Cl95 C93 Cl95 112.0(2) 6 . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.642 _refine_diff_density_min -0.738 _refine_diff_density_rms 0.091