# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #=============================================================================== _audit_creation_date 2011-08-05 # 1. SUBMISSION DETAILS _publ_contact_author_name 'Duncan Carmichael' _publ_contact_author_address ;Laboratoire DCPH Ecole Polytechnique Route de Saclay F91128 Palaiseau France ; _publ_contact_author_email duncan.carmichael@polytechnique.edu _publ_contact_author_phone 330169334415 _publ_contact_author_fax 330169334440 _publ_contact_letter ; Please consider this CIF submission for publication as a new structure paper in DALTON TRANSACTIONS. The figures, chemical structure diagram (scheme), Transfert of Copyright Agreement form and structure factors will be sent on receipt of your acknowledgement letter ; #=============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #=============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Diastereoselective synthesis and coordination chemistry of enantiopure keto-bis-(2-phosphametallocene)s ; _publ_author_address ; a) Laboratoire Heteroelements et Coordination, Ecole Polytechnique, CNRS F-91128 Palaiseau Cedex France b) Department of Organic Chemistry, Marie-Curie Sklodowska University, ul. Gliniana 33/120, 20-614 Lublin, Poland ; #=============================================================================== # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ; _publ_section_exptl_prep ;All structures were solved using SIR97 (Altomare et al.) and refined with SHELXL97 (Sheldrick). Figures were drawn with Platon (Spek, 1990). ; _publ_section_references ;Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993) J. Appl. Cryst. 26, 343-350. Sheldrick, G.M. SHELXL97. Program for crystal structure refinement. University of G\\"ottingen, Germany, 1997. Sluis, P. v.d., Spek, A.L. (1990). Acta Cryst. A46, 194-201. Spek, A.L. (1990). Acta Cryst. A46, C-34. Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7 ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; loop_ _publ_author_name D.Carmichael 'X.F.Le Goff' E.Muller L.Ricard M.Stankevic #=============================================================================== # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the ? in the data_? line below # by a unique identifier. #=============================================================================== #compound 17 data_em182 _database_code_depnum_ccdc_archive 'CCDC 837330' #TrackingRef '2011_carmichael_dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C45 H52 Fe2 O P2),C H2 Cl2' _chemical_formula_sum 'C91 H106 Cl2 Fe4 O2 P4' _chemical_formula_weight 1649.94 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.874(1) _cell_length_b 13.415(1) _cell_length_c 15.872(1) _cell_angle_alpha 93.293(1) _cell_angle_beta 101.481(1) _cell_angle_gamma 105.439(1) _cell_volume 1972.4(3) _cell_formula_units_Z 1 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 8836 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 866 _exptl_absorpt_coefficient_mu 0.919 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8233 _exptl_absorpt_correction_T_max 0.8821 _exptl_absorpt_process_details 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _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 28613 _diffrn_reflns_av_R_equivalents 0.0231 _diffrn_reflns_av_sigmaI/netI 0.0350 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 30.04 _reflns_number_total 11516 _reflns_number_gt 9566 _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^)+(0.0528P)^2^+1.0754P] 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 11516 _refine_ls_number_parameters 492 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0472 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.1093 _refine_ls_wR_factor_gt 0.0970 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 0.15147(3) 0.573727(17) 0.296311(15) 0.02279(7) Uani 1 1 d . . . Fe2 Fe -0.11384(3) 0.096115(17) 0.196737(14) 0.01980(6) Uani 1 1 d . . . P1 P 0.11480(4) 0.44147(3) 0.38127(3) 0.01939(9) Uani 1 1 d . . . P2 P -0.02233(5) 0.19355(3) 0.32916(3) 0.02130(9) Uani 1 1 d . . . O1 O -0.00343(17) 0.35373(10) 0.12847(8) 0.0343(3) Uani 1 1 d . . . C1 C 0.28577(17) 0.53752(12) 0.40307(10) 0.0206(3) Uani 1 1 d . . . C2 C 0.35173(18) 0.54544(13) 0.33037(11) 0.0241(3) Uani 1 1 d . . . C3 C 0.2631(2) 0.47774(13) 0.25546(11) 0.0256(3) Uani 1 1 d . . . C4 C 0.13060(18) 0.41551(12) 0.27242(10) 0.0211(3) Uani 1 1 d . . . C5 C 0.01332(19) 0.34194(13) 0.20587(10) 0.0235(3) Uani 1 1 d . . . C6 C -0.08308(18) 0.25270(12) 0.23642(10) 0.0201(3) Uani 1 1 d . . . C7 C -0.23012(18) 0.20250(13) 0.19318(11) 0.0228(3) Uani 1 1 d . . . C8 C -0.29366(18) 0.11735(13) 0.23587(11) 0.0242(3) Uani 1 1 d . . . C9 C -0.19519(19) 0.10037(13) 0.30885(11) 0.0248(3) Uani 1 1 d . . . C10 C 0.34748(18) 0.59482(12) 0.49103(10) 0.0214(3) Uani 1 1 d . . . C11 C 0.25561(19) 0.61606(14) 0.54219(11) 0.0263(3) Uani 1 1 d . . . H11 H 0.1548 0.5971 0.5185 0.032 Uiso 1 1 calc R . . C12 C 0.3081(2) 0.66382(15) 0.62615(12) 0.0313(4) Uani 1 1 d . . . H12 H 0.2435 0.6774 0.6593 0.038 Uiso 1 1 calc R . . C13 C 0.4552(2) 0.69213(15) 0.66238(12) 0.0314(4) Uani 1 1 d . . . H13 H 0.4916 0.7258 0.7199 0.038 Uiso 1 1 calc R . . C14 C 0.5481(2) 0.67084(14) 0.61382(12) 0.0285(4) Uani 1 1 d . . . H14 H 0.6486 0.6893 0.6384 0.034 Uiso 1 1 calc R . . C15 C 0.49516(18) 0.62250(13) 0.52907(11) 0.0247(3) Uani 1 1 d . . . H15 H 0.5602 0.6081 0.4966 0.030 Uiso 1 1 calc R . . C16 C 0.4994(2) 0.61472(16) 0.33058(13) 0.0343(4) Uani 1 1 d . . . H16A H 0.5716 0.5781 0.3500 0.052 Uiso 1 1 calc R . . H16B H 0.5197 0.6785 0.3700 0.052 Uiso 1 1 calc R . . H16C H 0.5032 0.6327 0.2719 0.052 Uiso 1 1 calc R . . C17 C 0.3131(3) 0.46713(17) 0.17280(13) 0.0387(5) Uani 1 1 d . . . H17A H 0.3799 0.4242 0.1794 0.058 Uiso 1 1 calc R . . H17B H 0.3621 0.5362 0.1597 0.058 Uiso 1 1 calc R . . H17C H 0.2298 0.4340 0.1254 0.058 Uiso 1 1 calc R . . C18 C -0.3152(2) 0.23951(15) 0.11800(13) 0.0336(4) Uani 1 1 d . . . H18A H -0.3716 0.2812 0.1395 0.050 Uiso 1 1 calc R . . H18B H -0.3802 0.1793 0.0787 0.050 Uiso 1 1 calc R . . H18C H -0.2489 0.2821 0.0869 0.050 Uiso 1 1 calc R . . C19 C -0.4486(2) 0.05296(16) 0.20727(14) 0.0353(4) Uani 1 1 d . . . H19A H -0.5085 0.0836 0.2370 0.053 Uiso 1 1 calc R . . H19B H -0.4572 -0.0182 0.2216 0.053 Uiso 1 1 calc R . . H19C H -0.4808 0.0516 0.1446 0.053 Uiso 1 1 calc R . . C20 C -0.2275(2) 0.02081(16) 0.36853(12) 0.0384(5) Uani 1 1 d . . . C21 C -0.3504(3) 0.0038(3) 0.40160(16) 0.0716(10) Uani 1 1 d . . . H21 H -0.4195 0.0403 0.3838 0.086 Uiso 1 1 calc R . . C22 C -0.3713(4) -0.0696(4) 0.4630(2) 0.109(2) Uani 1 1 d . . . H22 H -0.4560 -0.0829 0.4853 0.131 Uiso 1 1 calc R . . C23 C -0.2702(6) -0.1212(3) 0.4901(2) 0.111(2) Uani 1 1 d . . . H23 H -0.2850 -0.1693 0.5312 0.133 Uiso 1 1 calc R . . C24 C -0.1505(5) -0.1036(2) 0.45846(18) 0.0896(14) Uani 1 1 d . . . H24 H -0.0808 -0.1393 0.4774 0.108 Uiso 1 1 calc R . . C25 C -0.1286(4) -0.03341(18) 0.39833(15) 0.0567(7) Uani 1 1 d . . . H25 H -0.0433 -0.0219 0.3767 0.068 Uiso 1 1 calc R . . C26 C -0.0371(2) 0.60190(15) 0.23598(15) 0.0405(5) Uani 1 1 d . . . C27 C 0.0108(2) 0.65727(15) 0.32027(14) 0.0346(4) Uani 1 1 d . . . C28 C 0.1510(2) 0.72635(13) 0.32595(13) 0.0306(4) Uani 1 1 d . . . C29 C 0.1885(3) 0.71340(14) 0.24443(13) 0.0375(5) Uani 1 1 d . . . C30 C 0.0706(3) 0.63648(15) 0.18843(13) 0.0433(6) Uani 1 1 d . . . C31 C -0.1832(3) 0.5249(2) 0.2023(2) 0.0650(9) Uani 1 1 d . . . H31A H -0.2077 0.4803 0.2470 0.097 Uiso 1 1 calc R . . H31B H -0.1813 0.4818 0.1507 0.097 Uiso 1 1 calc R . . H31C H -0.2556 0.5624 0.1871 0.097 Uiso 1 1 calc R . . C32 C -0.0775(3) 0.6496(2) 0.38805(19) 0.0514(6) Uani 1 1 d . . . H32A H -0.1438 0.6926 0.3760 0.077 Uiso 1 1 calc R . . H32B H -0.0134 0.6743 0.4453 0.077 Uiso 1 1 calc R . . H32C H -0.1329 0.5769 0.3870 0.077 Uiso 1 1 calc R . . C33 C 0.2370(3) 0.80227(16) 0.40249(15) 0.0428(5) Uani 1 1 d . . . H33A H 0.3395 0.8081 0.4082 0.064 Uiso 1 1 calc R . . H33B H 0.2070 0.7781 0.4548 0.064 Uiso 1 1 calc R . . H33C H 0.2209 0.8705 0.3947 0.064 Uiso 1 1 calc R . . C34 C 0.3236(3) 0.77438(18) 0.22050(19) 0.0566(7) Uani 1 1 d . . . H34A H 0.3051 0.8332 0.1909 0.085 Uiso 1 1 calc R . . H34B H 0.3541 0.7293 0.1819 0.085 Uiso 1 1 calc R . . H34C H 0.3998 0.8006 0.2730 0.085 Uiso 1 1 calc R . . C35 C 0.0588(4) 0.6033(2) 0.09485(15) 0.0729(11) Uani 1 1 d . . . H35A H 0.0194 0.5275 0.0830 0.109 Uiso 1 1 calc R . . H35B H 0.1545 0.6244 0.0816 0.109 Uiso 1 1 calc R . . H35C H -0.0053 0.6364 0.0587 0.109 Uiso 1 1 calc R . . C36 C 0.0343(2) 0.01409(16) 0.18776(14) 0.0352(4) Uani 1 1 d . . . C37 C 0.0405(2) 0.08957(16) 0.12874(14) 0.0357(4) Uani 1 1 d . . . C38 C -0.0981(3) 0.06667(15) 0.07082(12) 0.0342(4) Uani 1 1 d . . . C39 C -0.1901(2) -0.02289(14) 0.09570(12) 0.0299(4) Uani 1 1 d . . . C40 C -0.1074(2) -0.05589(14) 0.16740(12) 0.0309(4) Uani 1 1 d . . . C41 C 0.1599(3) 0.0062(2) 0.25590(19) 0.0585(7) Uani 1 1 d . . . H41A H 0.2169 -0.0311 0.2296 0.088 Uiso 1 1 calc R . . H41B H 0.1242 -0.0317 0.3017 0.088 Uiso 1 1 calc R . . H41C H 0.2205 0.0763 0.2807 0.088 Uiso 1 1 calc R . . C42 C 0.1738(3) 0.1740(2) 0.1252(2) 0.0616(8) Uani 1 1 d . . . H42A H 0.2178 0.2118 0.1831 0.092 Uiso 1 1 calc R . . H42B H 0.1480 0.2224 0.0852 0.092 Uiso 1 1 calc R . . H42C H 0.2425 0.1428 0.1049 0.092 Uiso 1 1 calc R . . C43 C -0.1361(4) 0.12213(19) -0.00545(14) 0.0537(7) Uani 1 1 d . . . H43A H -0.0986 0.0988 -0.0534 0.080 Uiso 1 1 calc R . . H43B H -0.0934 0.1973 0.0103 0.080 Uiso 1 1 calc R . . H43C H -0.2411 0.1067 -0.0232 0.080 Uiso 1 1 calc R . . C44 C -0.3434(3) -0.07855(19) 0.05259(16) 0.0471(6) Uani 1 1 d . . . H44A H -0.3887 -0.0298 0.0227 0.071 Uiso 1 1 calc R . . H44B H -0.3960 -0.1064 0.0963 0.071 Uiso 1 1 calc R . . H44C H -0.3460 -0.1359 0.0106 0.071 Uiso 1 1 calc R . . C45 C -0.1578(3) -0.15450(17) 0.20626(16) 0.0510(6) Uani 1 1 d . . . H45A H -0.1589 -0.2140 0.1670 0.076 Uiso 1 1 calc R . . H45B H -0.2552 -0.1618 0.2152 0.076 Uiso 1 1 calc R . . H45C H -0.0922 -0.1522 0.2620 0.076 Uiso 1 1 calc R . . C46 C 0.5507(7) 0.4725(6) 0.0198(3) 0.0547(13) Uani 0.50 1 d P A 1 H46A H 0.6472 0.4789 0.0078 0.066 Uiso 0.50 1 calc PR A 1 H46B H 0.5568 0.4629 0.0817 0.066 Uiso 0.50 1 calc PR A 1 Cl1 Cl 0.5049(2) 0.58788(14) 0.00067(12) 0.0684(4) Uani 0.50 1 d P . 1 Cl2 Cl 0.4287(2) 0.36391(14) -0.04278(13) 0.0844(6) Uani 0.50 1 d P . 1 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 0.02783(13) 0.01578(11) 0.02156(12) 0.00320(8) 0.00165(9) 0.00341(9) Fe2 0.02328(12) 0.01662(11) 0.01935(11) 0.00113(8) 0.00458(9) 0.00572(8) P1 0.02003(19) 0.01790(18) 0.01901(18) 0.00177(14) 0.00430(15) 0.00341(14) P2 0.0232(2) 0.01909(19) 0.01863(18) 0.00338(14) 0.00265(15) 0.00209(15) O1 0.0489(8) 0.0263(6) 0.0192(6) 0.0044(5) 0.0026(6) -0.0002(6) C1 0.0195(7) 0.0186(7) 0.0228(7) 0.0030(6) 0.0037(6) 0.0048(5) C2 0.0235(8) 0.0208(7) 0.0266(8) 0.0029(6) 0.0080(6) 0.0025(6) C3 0.0305(9) 0.0211(7) 0.0243(8) 0.0029(6) 0.0105(7) 0.0025(6) C4 0.0276(8) 0.0153(7) 0.0197(7) 0.0022(5) 0.0056(6) 0.0043(6) C5 0.0313(9) 0.0188(7) 0.0202(7) 0.0031(6) 0.0054(6) 0.0066(6) C6 0.0237(7) 0.0156(7) 0.0198(7) 0.0009(5) 0.0038(6) 0.0047(5) C7 0.0226(8) 0.0200(7) 0.0236(7) -0.0025(6) 0.0002(6) 0.0070(6) C8 0.0208(7) 0.0225(7) 0.0268(8) -0.0035(6) 0.0063(6) 0.0023(6) C9 0.0269(8) 0.0223(8) 0.0224(7) 0.0007(6) 0.0084(6) 0.0002(6) C10 0.0221(7) 0.0173(7) 0.0238(7) 0.0021(6) 0.0036(6) 0.0053(6) C11 0.0237(8) 0.0284(8) 0.0266(8) -0.0001(6) 0.0040(6) 0.0091(6) C12 0.0332(9) 0.0333(9) 0.0278(8) -0.0039(7) 0.0068(7) 0.0120(7) C13 0.0365(10) 0.0280(9) 0.0254(8) -0.0043(7) 0.0005(7) 0.0080(7) C14 0.0260(8) 0.0243(8) 0.0297(8) -0.0001(6) -0.0026(7) 0.0049(6) C15 0.0226(8) 0.0214(7) 0.0287(8) 0.0007(6) 0.0041(6) 0.0056(6) C16 0.0286(9) 0.0341(10) 0.0351(10) 0.0005(8) 0.0123(8) -0.0029(7) C17 0.0476(12) 0.0345(10) 0.0295(9) -0.0006(8) 0.0202(9) -0.0035(9) C18 0.0332(10) 0.0275(9) 0.0341(9) 0.0007(7) -0.0073(8) 0.0099(7) C19 0.0231(9) 0.0337(10) 0.0424(11) -0.0055(8) 0.0062(8) -0.0003(7) C20 0.0478(12) 0.0287(9) 0.0237(8) -0.0001(7) 0.0076(8) -0.0133(8) C21 0.0482(15) 0.102(2) 0.0332(12) 0.0069(13) 0.0114(11) -0.0334(15) C22 0.083(3) 0.141(4) 0.0364(15) 0.0054(19) 0.0120(16) -0.079(3) C23 0.154(4) 0.070(2) 0.0363(15) 0.0194(14) -0.016(2) -0.064(3) C24 0.175(4) 0.0348(13) 0.0360(13) 0.0142(11) 0.0041(19) 0.0019(19) C25 0.102(2) 0.0317(11) 0.0318(11) 0.0113(9) 0.0096(13) 0.0127(12) C26 0.0410(11) 0.0241(9) 0.0459(11) 0.0068(8) -0.0153(9) 0.0094(8) C27 0.0352(10) 0.0250(9) 0.0441(11) 0.0090(8) 0.0009(8) 0.0142(7) C28 0.0379(10) 0.0173(7) 0.0336(9) 0.0028(6) 0.0008(8) 0.0082(7) C29 0.0570(13) 0.0179(8) 0.0358(10) 0.0098(7) 0.0089(9) 0.0072(8) C30 0.0739(16) 0.0222(9) 0.0276(9) 0.0072(7) -0.0051(10) 0.0140(9) C31 0.0439(14) 0.0390(13) 0.091(2) 0.0061(13) -0.0296(14) 0.0095(10) C32 0.0433(13) 0.0476(13) 0.0776(18) 0.0208(12) 0.0224(12) 0.0278(11) C33 0.0538(13) 0.0237(9) 0.0428(11) -0.0034(8) -0.0041(10) 0.0099(9) C34 0.0790(19) 0.0291(11) 0.0697(17) 0.0229(11) 0.0360(15) 0.0108(11) C35 0.147(3) 0.0366(13) 0.0269(11) 0.0089(9) 0.0003(15) 0.0250(16) C36 0.0364(10) 0.0343(10) 0.0394(10) -0.0036(8) 0.0077(8) 0.0197(8) C37 0.0407(11) 0.0307(9) 0.0401(10) -0.0029(8) 0.0216(9) 0.0099(8) C38 0.0581(13) 0.0268(9) 0.0234(8) 0.0009(7) 0.0157(8) 0.0174(8) C39 0.0403(10) 0.0235(8) 0.0245(8) -0.0066(6) 0.0042(7) 0.0108(7) C40 0.0434(11) 0.0193(8) 0.0327(9) 0.0005(7) 0.0088(8) 0.0141(7) C41 0.0464(14) 0.0719(18) 0.0625(16) -0.0041(14) -0.0021(12) 0.0391(13) C42 0.0570(16) 0.0496(14) 0.086(2) -0.0034(14) 0.0492(16) 0.0054(12) C43 0.105(2) 0.0419(12) 0.0242(9) 0.0083(9) 0.0218(12) 0.0321(14) C44 0.0450(12) 0.0429(12) 0.0424(12) -0.0188(10) -0.0034(10) 0.0087(10) C45 0.0829(19) 0.0237(10) 0.0490(13) 0.0076(9) 0.0147(13) 0.0189(11) C46 0.052(3) 0.071(4) 0.035(2) 0.012(3) 0.002(2) 0.013(3) Cl1 0.0928(13) 0.0521(9) 0.0591(9) 0.0076(7) 0.0274(9) 0.0107(9) Cl2 0.0979(13) 0.0495(8) 0.0747(11) 0.0130(8) -0.0217(10) -0.0024(8) _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 C26 2.057(2) . ? Fe1 C3 2.0583(18) . ? Fe1 C29 2.0628(18) . ? Fe1 C30 2.0633(19) . ? Fe1 C28 2.0758(17) . ? Fe1 C27 2.078(2) . ? Fe1 C4 2.0820(15) . ? Fe1 C2 2.0842(18) . ? Fe1 C1 2.0997(16) . ? Fe1 P1 2.2857(5) . ? Fe2 C37 2.052(2) . ? Fe2 C7 2.0529(16) . ? Fe2 C38 2.0591(18) . ? Fe2 C39 2.0671(16) . ? Fe2 C36 2.0716(18) . ? Fe2 C8 2.0754(17) . ? Fe2 C6 2.0817(15) . ? Fe2 C40 2.0858(17) . ? Fe2 C9 2.0968(17) . ? Fe2 P2 2.2895(5) . ? P1 C1 1.7854(17) . ? P1 C4 1.7881(16) . ? P2 C9 1.7828(17) . ? P2 C6 1.7866(16) . ? O1 C5 1.232(2) . ? C1 C2 1.430(2) . ? C1 C10 1.483(2) . ? C2 C3 1.429(2) . ? C2 C16 1.506(2) . ? C3 C4 1.437(2) . ? C3 C17 1.503(3) . ? C4 C5 1.488(2) . ? C5 C6 1.489(2) . ? C6 C7 1.436(2) . ? C7 C8 1.426(2) . ? C7 C18 1.505(2) . ? C8 C9 1.428(2) . ? C8 C19 1.506(2) . ? C9 C20 1.481(3) . ? C10 C15 1.402(2) . ? C10 C11 1.403(2) . ? C11 C12 1.380(2) . ? C12 C13 1.390(3) . ? C13 C14 1.383(3) . ? C14 C15 1.394(2) . ? C20 C21 1.386(4) . ? C20 C25 1.393(4) . ? C21 C22 1.429(5) . ? C22 C23 1.375(7) . ? C23 C24 1.344(7) . ? C24 C25 1.386(3) . ? C26 C27 1.418(3) . ? C26 C30 1.419(4) . ? C26 C31 1.507(3) . ? C27 C28 1.428(3) . ? C27 C32 1.506(3) . ? C28 C29 1.429(3) . ? C28 C33 1.490(3) . ? C29 C30 1.433(3) . ? C29 C34 1.500(3) . ? C30 C35 1.498(3) . ? C36 C37 1.416(3) . ? C36 C40 1.424(3) . ? C36 C41 1.506(3) . ? C37 C38 1.434(3) . ? C37 C42 1.504(3) . ? C38 C39 1.428(3) . ? C38 C43 1.493(3) . ? C39 C40 1.427(3) . ? C39 C44 1.499(3) . ? C40 C45 1.498(3) . ? C46 Cl2 1.728(7) . ? C46 Cl1 1.750(7) . ? Cl1 C46 0.852(6) 2_665 ? Cl1 Cl2 0.919(2) 2_665 ? Cl1 Cl1 2.333(4) 2_665 ? Cl2 Cl1 0.919(2) 2_665 ? Cl2 C46 2.152(7) 2_665 ? 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 C26 Fe1 C3 130.56(8) . . ? C26 Fe1 C29 67.95(9) . . ? C3 Fe1 C29 113.07(8) . . ? C26 Fe1 C30 40.28(10) . . ? C3 Fe1 C30 106.37(9) . . ? C29 Fe1 C30 40.64(8) . . ? C26 Fe1 C28 67.65(8) . . ? C3 Fe1 C28 145.99(8) . . ? C29 Fe1 C28 40.39(8) . . ? C30 Fe1 C28 67.92(8) . . ? C26 Fe1 C27 40.11(9) . . ? C3 Fe1 C27 170.38(8) . . ? C29 Fe1 C27 67.80(9) . . ? C30 Fe1 C27 67.67(9) . . ? C28 Fe1 C27 40.21(8) . . ? C26 Fe1 C4 108.72(7) . . ? C3 Fe1 C4 40.61(7) . . ? C29 Fe1 C4 144.50(8) . . ? C30 Fe1 C4 113.29(7) . . ? C28 Fe1 C4 173.33(8) . . ? C27 Fe1 C4 133.50(8) . . ? C26 Fe1 C2 167.43(9) . . ? C3 Fe1 C2 40.36(7) . . ? C29 Fe1 C2 105.85(8) . . ? C30 Fe1 C2 128.06(9) . . ? C28 Fe1 C2 115.30(7) . . ? C27 Fe1 C2 149.26(7) . . ? C4 Fe1 C2 69.52(7) . . ? C26 Fe1 C1 152.51(9) . . ? C3 Fe1 C1 69.81(7) . . ? C29 Fe1 C1 126.01(8) . . ? C30 Fe1 C1 164.66(9) . . ? C28 Fe1 C1 106.47(7) . . ? C27 Fe1 C1 117.98(7) . . ? C4 Fe1 C1 74.02(6) . . ? C2 Fe1 C1 39.96(6) . . ? C26 Fe1 P1 112.86(7) . . ? C3 Fe1 P1 76.49(5) . . ? C29 Fe1 P1 167.35(6) . . ? C30 Fe1 P1 147.07(7) . . ? C28 Fe1 P1 127.32(6) . . ? C27 Fe1 P1 104.25(6) . . ? C4 Fe1 P1 48.05(5) . . ? C2 Fe1 P1 75.70(5) . . ? C1 Fe1 P1 47.82(5) . . ? C37 Fe2 C7 127.45(8) . . ? C37 Fe2 C38 40.83(9) . . ? C7 Fe2 C38 105.10(7) . . ? C37 Fe2 C39 68.24(8) . . ? C7 Fe2 C39 114.72(7) . . ? C38 Fe2 C39 40.50(8) . . ? C37 Fe2 C36 40.17(9) . . ? C7 Fe2 C36 166.86(8) . . ? C38 Fe2 C36 67.94(8) . . ? C39 Fe2 C36 67.82(8) . . ? C37 Fe2 C8 164.68(8) . . ? C7 Fe2 C8 40.42(7) . . ? C38 Fe2 C8 125.91(8) . . ? C39 Fe2 C8 106.28(7) . . ? C36 Fe2 C8 152.66(8) . . ? C37 Fe2 C6 106.86(7) . . ? C7 Fe2 C6 40.64(6) . . ? C38 Fe2 C6 113.94(7) . . ? C39 Fe2 C6 146.78(7) . . ? C36 Fe2 C6 130.55(8) . . ? C8 Fe2 C6 69.40(7) . . ? C37 Fe2 C40 67.57(8) . . ? C7 Fe2 C40 149.21(7) . . ? C38 Fe2 C40 67.67(8) . . ? C39 Fe2 C40 40.20(7) . . ? C36 Fe2 C40 40.07(8) . . ? C8 Fe2 C40 118.17(8) . . ? C6 Fe2 C40 170.13(7) . . ? C37 Fe2 C9 154.75(8) . . ? C7 Fe2 C9 69.92(7) . . ? C38 Fe2 C9 162.51(8) . . ? C39 Fe2 C9 125.09(7) . . ? C36 Fe2 C9 120.07(8) . . ? C8 Fe2 C9 40.02(7) . . ? C6 Fe2 C9 73.80(7) . . ? C40 Fe2 C9 107.57(7) . . ? C37 Fe2 P2 113.42(6) . . ? C7 Fe2 P2 76.62(5) . . ? C38 Fe2 P2 149.06(6) . . ? C39 Fe2 P2 165.18(6) . . ? C36 Fe2 P2 103.45(6) . . ? C8 Fe2 P2 75.71(5) . . ? C6 Fe2 P2 47.96(4) . . ? C40 Fe2 P2 125.60(6) . . ? C9 Fe2 P2 47.71(5) . . ? C1 P1 C4 89.57(8) . . ? C1 P1 Fe1 60.63(5) . . ? C4 P1 Fe1 60.00(5) . . ? C9 P2 C6 89.32(8) . . ? C9 P2 Fe2 60.47(6) . . ? C6 P2 Fe2 59.92(5) . . ? C2 C1 C10 127.19(15) . . ? C2 C1 P1 112.87(12) . . ? C10 C1 P1 119.85(12) . . ? C2 C1 Fe1 69.44(9) . . ? C10 C1 Fe1 129.90(11) . . ? P1 C1 Fe1 71.56(6) . . ? C3 C2 C1 112.67(15) . . ? C3 C2 C16 122.19(16) . . ? C1 C2 C16 125.13(15) . . ? C3 C2 Fe1 68.84(10) . . ? C1 C2 Fe1 70.61(9) . . ? C16 C2 Fe1 129.70(13) . . ? C2 C3 C4 111.92(15) . . ? C2 C3 C17 122.46(16) . . ? C4 C3 C17 125.32(16) . . ? C2 C3 Fe1 70.79(10) . . ? C4 C3 Fe1 70.58(10) . . ? C17 C3 Fe1 131.21(14) . . ? C3 C4 C5 124.28(15) . . ? C3 C4 P1 112.92(12) . . ? C5 C4 P1 122.69(13) . . ? C3 C4 Fe1 68.80(9) . . ? C5 C4 Fe1 124.26(11) . . ? P1 C4 Fe1 71.94(6) . . ? O1 C5 C4 121.60(16) . . ? O1 C5 C6 121.04(15) . . ? C4 C5 C6 117.36(14) . . ? C7 C6 C5 124.24(14) . . ? C7 C6 P2 113.26(12) . . ? C5 C6 P2 122.44(12) . . ? C7 C6 Fe2 68.60(9) . . ? C5 C6 Fe2 125.37(11) . . ? P2 C6 Fe2 72.12(6) . . ? C8 C7 C6 111.55(14) . . ? C8 C7 C18 122.53(16) . . ? C6 C7 C18 125.62(16) . . ? C8 C7 Fe2 70.64(9) . . ? C6 C7 Fe2 70.76(9) . . ? C18 C7 Fe2 131.01(13) . . ? C7 C8 C9 112.86(14) . . ? C7 C8 C19 123.43(16) . . ? C9 C8 C19 123.72(17) . . ? C7 C8 Fe2 68.94(9) . . ? C9 C8 Fe2 70.79(10) . . ? C19 C8 Fe2 128.90(12) . . ? C8 C9 C20 126.61(16) . . ? C8 C9 P2 112.97(13) . . ? C20 C9 P2 120.28(14) . . ? C8 C9 Fe2 69.18(10) . . ? C20 C9 Fe2 130.76(14) . . ? P2 C9 Fe2 71.82(6) . . ? C15 C10 C11 117.29(15) . . ? C15 C10 C1 122.71(15) . . ? C11 C10 C1 119.81(15) . . ? C12 C11 C10 121.60(17) . . ? C11 C12 C13 120.29(18) . . ? C14 C13 C12 119.34(17) . . ? C13 C14 C15 120.42(17) . . ? C14 C15 C10 121.04(17) . . ? C21 C20 C25 118.0(2) . . ? C21 C20 C9 121.4(3) . . ? C25 C20 C9 120.4(2) . . ? C20 C21 C22 118.8(4) . . ? C23 C22 C21 120.8(4) . . ? C24 C23 C22 120.2(3) . . ? C23 C24 C25 120.1(4) . . ? C24 C25 C20 122.2(3) . . ? C27 C26 C30 108.72(18) . . ? C27 C26 C31 124.6(3) . . ? C30 C26 C31 126.5(2) . . ? C27 C26 Fe1 70.73(11) . . ? C30 C26 Fe1 70.08(12) . . ? C31 C26 Fe1 128.32(15) . . ? C26 C27 C28 107.9(2) . . ? C26 C27 C32 125.1(2) . . ? C28 C27 C32 126.8(2) . . ? C26 C27 Fe1 69.16(12) . . ? C28 C27 Fe1 69.80(11) . . ? C32 C27 Fe1 130.30(14) . . ? C27 C28 C29 107.89(18) . . ? C27 C28 C33 125.1(2) . . ? C29 C28 C33 126.9(2) . . ? C27 C28 Fe1 69.98(10) . . ? C29 C28 Fe1 69.32(10) . . ? C33 C28 Fe1 128.89(14) . . ? C28 C29 C30 107.8(2) . . ? C28 C29 C34 125.8(2) . . ? C30 C29 C34 126.3(2) . . ? C28 C29 Fe1 70.30(10) . . ? C30 C29 Fe1 69.70(10) . . ? C34 C29 Fe1 128.23(17) . . ? C26 C30 C29 107.68(19) . . ? C26 C30 C35 125.9(2) . . ? C29 C30 C35 126.3(3) . . ? C26 C30 Fe1 69.64(11) . . ? C29 C30 Fe1 69.66(11) . . ? C35 C30 Fe1 129.01(17) . . ? C37 C36 C40 108.20(18) . . ? C37 C36 C41 125.1(2) . . ? C40 C36 C41 126.6(2) . . ? C37 C36 Fe2 69.16(11) . . ? C40 C36 Fe2 70.50(10) . . ? C41 C36 Fe2 129.13(16) . . ? C36 C37 C38 108.16(18) . . ? C36 C37 C42 124.9(2) . . ? C38 C37 C42 126.9(2) . . ? C36 C37 Fe2 70.67(11) . . ? C38 C37 Fe2 69.86(11) . . ? C42 C37 Fe2 128.23(15) . . ? C39 C38 C37 107.66(17) . . ? C39 C38 C43 126.3(2) . . ? C37 C38 C43 125.9(2) . . ? C39 C38 Fe2 70.05(10) . . ? C37 C38 Fe2 69.31(11) . . ? C43 C38 Fe2 129.20(14) . . ? C40 C39 C38 107.85(18) . . ? C40 C39 C44 124.60(19) . . ? C38 C39 C44 127.46(19) . . ? C40 C39 Fe2 70.60(10) . . ? C38 C39 Fe2 69.45(10) . . ? C44 C39 Fe2 128.25(14) . . ? C36 C40 C39 108.12(17) . . ? C36 C40 C45 126.5(2) . . ? C39 C40 C45 125.0(2) . . ? C36 C40 Fe2 69.43(10) . . ? C39 C40 Fe2 69.19(9) . . ? C45 C40 Fe2 132.59(15) . . ? Cl2 C46 Cl1 113.1(3) . . ? C46 Cl1 Cl2 154.5(4) 2_665 2_665 ? C46 Cl1 C46 56.4(5) 2_665 . ? Cl2 Cl1 C46 103.0(3) 2_665 . ? C46 Cl1 Cl1 38.7(4) 2_665 2_665 ? Cl2 Cl1 Cl1 119.9(2) 2_665 2_665 ? C46 Cl1 Cl1 17.7(2) . 2_665 ? Cl1 Cl2 C46 12.3(2) 2_665 . ? Cl1 Cl2 C46 52.4(2) 2_665 2_665 ? C46 Cl2 C46 42.5(3) . 2_665 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.586 _refine_diff_density_min -0.626 _refine_diff_density_rms 0.075 #===END #compound 32 data_em171 _database_code_depnum_ccdc_archive 'CCDC 837331' #TrackingRef '2011_carmichael_dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C55 H67 Cl O P2 Ru3, 2(C H2 Cl2)' _chemical_formula_sum 'C57 H71 Cl5 O P2 Ru3' _chemical_formula_weight 1314.54 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' Cl Cl 0.1484 0.1585 '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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21 ' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.427(1) _cell_length_b 13.624(1) _cell_length_c 17.850(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.415(1) _cell_angle_gamma 90.00 _cell_volume 2778.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 1636 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description Plate _exptl_crystal_colour Orange _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.571 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 1.142 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8752 _exptl_absorpt_correction_T_max 0.9775 _exptl_absorpt_process_details 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _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 20289 _diffrn_reflns_av_R_equivalents 0.0237 _diffrn_reflns_av_sigmaI/netI 0.0680 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.20 _diffrn_reflns_theta_max 30.03 _reflns_number_total 14094 _reflns_number_gt 12010 _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^)+(0.0516P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(2) _refine_ls_number_reflns 14094 _refine_ls_number_parameters 632 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0538 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.1018 _refine_ls_wR_factor_gt 0.0967 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _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 Ru1 Ru 0.86328(3) 1.04294(3) 0.348905(19) 0.02166(8) Uani 1 1 d . . . Ru2 Ru 0.81139(3) 0.86662(2) 0.038990(18) 0.01780(8) Uani 1 1 d . . . Ru3 Ru 0.56826(3) 0.88080(2) 0.230651(18) 0.01837(8) Uani 1 1 d . . . Cl1 Cl 0.62439(10) 0.70628(8) 0.22591(7) 0.0272(2) Uani 1 1 d . . . P1 P 0.74126(10) 0.92400(8) 0.28554(7) 0.0212(2) Uani 1 1 d . . . P2 P 0.66526(10) 0.91582(8) 0.12409(6) 0.0184(2) Uani 1 1 d . . . O1 O 0.9578(3) 1.0737(3) 0.15620(19) 0.0394(9) Uani 1 1 d . . . C1 C 0.6817(5) 0.7597(4) 0.4217(3) 0.0344(12) Uani 1 1 d . . . H1 H 0.6622 0.7379 0.3726 0.041 Uiso 1 1 calc R . . C2 C 0.6300(5) 0.7163(4) 0.4828(3) 0.0387(13) Uani 1 1 d . . . H2 H 0.5773 0.6631 0.4755 0.046 Uiso 1 1 calc R . . C3 C 0.6538(5) 0.7491(4) 0.5542(3) 0.0377(13) Uani 1 1 d . . . H3 H 0.6164 0.7201 0.5961 0.045 Uiso 1 1 calc R . . C4 C 0.7332(5) 0.8253(4) 0.5644(3) 0.0372(12) Uani 1 1 d . . . H4 H 0.7498 0.8484 0.6135 0.045 Uiso 1 1 calc R . . C5 C 0.7871(4) 0.8668(4) 0.5052(3) 0.0346(11) Uani 1 1 d . . . H5 H 0.8424 0.9177 0.5135 0.041 Uiso 1 1 calc R . . C6 C 0.7627(4) 0.8358(3) 0.4313(3) 0.0256(10) Uani 1 1 d . . . C7 C 0.8191(4) 0.8810(4) 0.3651(2) 0.0243(9) Uani 1 1 d . . . C8 C 0.9420(4) 0.8943(4) 0.3565(3) 0.0312(11) Uani 1 1 d . . . C9 C 0.9734(4) 0.9410(4) 0.2876(3) 0.0272(10) Uani 1 1 d . . . C10 C 0.8727(4) 0.9620(3) 0.2421(3) 0.0218(9) Uani 1 1 d . . . C11 C 0.8781(4) 1.0159(3) 0.1681(3) 0.0251(10) Uani 1 1 d . . . C12 C 0.7878(4) 0.9945(3) 0.1113(2) 0.0209(9) Uani 1 1 d . . . C13 C 0.7982(4) 1.0265(3) 0.0341(2) 0.0198(9) Uani 1 1 d . . . C14 C 0.7083(4) 0.9838(3) -0.0128(2) 0.0203(9) Uani 1 1 d . . . C15 C 0.6293(4) 0.9212(3) 0.0267(2) 0.0187(9) Uani 1 1 d . . . C16 C 0.5321(3) 0.8669(3) -0.0082(2) 0.0204(8) Uani 1 1 d . . . C17 C 0.4568(4) 0.9110(4) -0.0610(3) 0.0303(11) Uani 1 1 d . . . H17 H 0.4673 0.9780 -0.0740 0.036 Uiso 1 1 calc R . . C18 C 0.3673(5) 0.8572(4) -0.0943(3) 0.0395(13) Uani 1 1 d . . . H18 H 0.3168 0.8880 -0.1297 0.047 Uiso 1 1 calc R . . C19 C 0.3510(5) 0.7607(4) -0.0768(3) 0.0419(14) Uani 1 1 d . . . H19 H 0.2914 0.7239 -0.1014 0.050 Uiso 1 1 calc R . . C20 C 0.4225(4) 0.7157(4) -0.0221(3) 0.0342(12) Uani 1 1 d . . . H20 H 0.4098 0.6492 -0.0084 0.041 Uiso 1 1 calc R . . C21 C 0.5106(4) 0.7686(3) 0.0110(3) 0.0275(10) Uani 1 1 d . . . H21 H 0.5584 0.7381 0.0480 0.033 Uiso 1 1 calc R . . C22 C 0.7019(4) 1.0019(4) -0.0955(2) 0.0274(10) Uani 1 1 d . . . H22A H 0.6536 1.0600 -0.1054 0.041 Uiso 1 1 calc R . . H22B H 0.6669 0.9447 -0.1205 0.041 Uiso 1 1 calc R . . H22C H 0.7808 1.0128 -0.1149 0.041 Uiso 1 1 calc R . . C23 C 0.8876(4) 1.0976(3) 0.0052(3) 0.0292(11) Uani 1 1 d . . . H23A H 0.8855 1.0978 -0.0497 0.044 Uiso 1 1 calc R . . H23B H 0.9656 1.0777 0.0226 0.044 Uiso 1 1 calc R . . H23C H 0.8700 1.1636 0.0239 0.044 Uiso 1 1 calc R . . C24 C 1.0995(4) 0.9544(4) 0.2660(3) 0.0386(13) Uani 1 1 d . . . H24A H 1.1425 0.9847 0.3077 0.058 Uiso 1 1 calc R . . H24B H 1.1040 0.9970 0.2218 0.058 Uiso 1 1 calc R . . H24C H 1.1341 0.8904 0.2545 0.058 Uiso 1 1 calc R . . C25 C 1.0332(5) 0.8543(4) 0.4098(3) 0.0385(12) Uani 1 1 d . . . H25A H 1.0663 0.7938 0.3892 0.058 Uiso 1 1 calc R . . H25B H 0.9970 0.8402 0.4583 0.058 Uiso 1 1 calc R . . H25C H 1.0956 0.9030 0.4167 0.058 Uiso 1 1 calc R . . C26 C 0.7776(5) 1.1805(3) 0.3951(3) 0.0282(10) Uani 1 1 d . . . C27 C 0.8519(5) 1.1374(3) 0.4501(3) 0.0294(11) Uani 1 1 d . . . C28 C 0.9690(4) 1.1376(3) 0.4224(3) 0.0276(10) Uani 1 1 d . . . C29 C 0.9661(4) 1.1779(3) 0.3493(3) 0.0277(10) Uani 1 1 d . . . C30 C 0.8480(5) 1.2013(3) 0.3318(3) 0.0286(11) Uani 1 1 d . . . C31 C 0.6549(5) 1.2109(4) 0.4080(3) 0.0386(13) Uani 1 1 d . . . H31A H 0.6540 1.2737 0.4347 0.058 Uiso 1 1 calc R . . H31B H 0.6153 1.1609 0.4381 0.058 Uiso 1 1 calc R . . H31C H 0.6143 1.2180 0.3598 0.058 Uiso 1 1 calc R . . C32 C 0.8151(5) 1.1143(4) 0.5298(3) 0.0406(13) Uani 1 1 d . . . H32A H 0.8101 1.1753 0.5586 0.061 Uiso 1 1 calc R . . H32B H 0.8729 1.0706 0.5531 0.061 Uiso 1 1 calc R . . H32C H 0.7384 1.0820 0.5290 0.061 Uiso 1 1 calc R . . C33 C 1.0745(5) 1.1067(4) 0.4661(3) 0.0376(12) Uani 1 1 d . . . H33A H 1.1312 1.0764 0.4322 0.056 Uiso 1 1 calc R . . H33B H 1.0516 1.0591 0.5045 0.056 Uiso 1 1 calc R . . H33C H 1.1099 1.1642 0.4901 0.056 Uiso 1 1 calc R . . C34 C 1.0678(5) 1.2011(4) 0.2999(3) 0.0407(13) Uani 1 1 d . . . H34A H 1.0840 1.2717 0.3019 0.061 Uiso 1 1 calc R . . H34B H 1.0492 1.1820 0.2483 0.061 Uiso 1 1 calc R . . H34C H 1.1369 1.1648 0.3174 0.061 Uiso 1 1 calc R . . C35 C 0.8052(6) 1.2502(4) 0.2597(3) 0.0422(14) Uani 1 1 d . . . H35A H 0.7209 1.2389 0.2536 0.063 Uiso 1 1 calc R . . H35B H 0.8467 1.2222 0.2169 0.063 Uiso 1 1 calc R . . H35C H 0.8203 1.3209 0.2623 0.063 Uiso 1 1 calc R . . C36 C 0.8413(4) 0.7082(3) 0.0305(3) 0.0243(10) Uani 1 1 d . . . C37 C 0.9276(4) 0.7504(3) 0.0783(3) 0.0249(10) Uani 1 1 d . . . C38 C 0.9937(4) 0.8185(3) 0.0347(3) 0.0248(10) Uani 1 1 d . . . C39 C 0.9480(4) 0.8182(3) -0.0400(3) 0.0259(10) Uani 1 1 d . . . C40 C 0.8514(4) 0.7504(3) -0.0429(3) 0.0230(9) Uani 1 1 d . . . C41 C 0.7633(5) 0.6227(3) 0.0499(3) 0.0309(11) Uani 1 1 d . . . H41A H 0.6999 0.6178 0.0128 0.046 Uiso 1 1 calc R . . H41B H 0.7300 0.6329 0.0998 0.046 Uiso 1 1 calc R . . H41C H 0.8092 0.5620 0.0498 0.046 Uiso 1 1 calc R . . C42 C 0.9489(5) 0.7189(4) 0.1578(3) 0.0333(11) Uani 1 1 d . . . H42A H 0.8737 0.7089 0.1828 0.050 Uiso 1 1 calc R . . H42B H 0.9935 0.7698 0.1843 0.050 Uiso 1 1 calc R . . H42C H 0.9933 0.6574 0.1583 0.050 Uiso 1 1 calc R . . C43 C 1.0985(4) 0.8757(4) 0.0596(3) 0.0324(10) Uani 1 1 d . . . H43A H 1.1685 0.8495 0.0353 0.049 Uiso 1 1 calc R . . H43B H 1.1073 0.8704 0.1141 0.049 Uiso 1 1 calc R . . H43C H 1.0884 0.9448 0.0458 0.049 Uiso 1 1 calc R . . C44 C 0.9974(4) 0.8754(4) -0.1045(3) 0.0351(11) Uani 1 1 d . . . H44A H 1.0250 0.9394 -0.0866 0.053 Uiso 1 1 calc R . . H44B H 0.9365 0.8850 -0.1427 0.053 Uiso 1 1 calc R . . H44C H 1.0630 0.8391 -0.1262 0.053 Uiso 1 1 calc R . . C45 C 0.7823(5) 0.7243(4) -0.1110(3) 0.0312(11) Uani 1 1 d . . . H45A H 0.8228 0.6724 -0.1386 0.047 Uiso 1 1 calc R . . H45B H 0.7741 0.7824 -0.1431 0.047 Uiso 1 1 calc R . . H45C H 0.7047 0.7011 -0.0963 0.047 Uiso 1 1 calc R . . C46 C 0.3798(4) 0.8468(3) 0.2205(3) 0.0226(9) Uani 1 1 d . . . C47 C 0.4106(4) 0.8470(3) 0.3004(3) 0.0247(10) Uani 1 1 d . . . C48 C 0.4515(4) 0.9420(4) 0.3178(3) 0.0266(10) Uani 1 1 d . . . C49 C 0.4476(4) 1.0014(3) 0.2505(3) 0.0254(10) Uani 1 1 d . . . C50 C 0.3987(4) 0.9411(3) 0.1915(3) 0.0208(9) Uani 1 1 d . . . C51 C 0.3298(4) 0.7585(3) 0.1820(3) 0.0292(11) Uani 1 1 d . . . H51A H 0.2478 0.7504 0.1964 0.044 Uiso 1 1 calc R . . H51B H 0.3744 0.7001 0.1967 0.044 Uiso 1 1 calc R . . H51C H 0.3345 0.7673 0.1276 0.044 Uiso 1 1 calc R . . C52 C 0.3926(5) 0.7629(4) 0.3498(3) 0.0347(12) Uani 1 1 d . . . H52A H 0.4248 0.7776 0.3995 0.052 Uiso 1 1 calc R . . H52B H 0.4323 0.7053 0.3291 0.052 Uiso 1 1 calc R . . H52C H 0.3086 0.7494 0.3538 0.052 Uiso 1 1 calc R . . C53 C 0.4860(5) 0.9783(4) 0.3939(3) 0.0354(12) Uani 1 1 d . . . H53A H 0.4981 0.9222 0.4275 0.053 Uiso 1 1 calc R . . H53B H 0.4238 1.0202 0.4137 0.053 Uiso 1 1 calc R . . H53C H 0.5587 1.0161 0.3904 0.053 Uiso 1 1 calc R . . C54 C 0.4727(5) 1.1107(3) 0.2454(3) 0.0366(13) Uani 1 1 d . . . H54A H 0.4841 1.1290 0.1929 0.055 Uiso 1 1 calc R . . H54B H 0.5436 1.1260 0.2743 0.055 Uiso 1 1 calc R . . H54C H 0.4065 1.1475 0.2658 0.055 Uiso 1 1 calc R . . C55 C 0.3638(4) 0.9790(3) 0.1156(3) 0.0275(10) Uani 1 1 d . . . H55A H 0.3531 0.9238 0.0811 0.041 Uiso 1 1 calc R . . H55B H 0.4253 1.0224 0.0967 0.041 Uiso 1 1 calc R . . H55C H 0.2904 1.0158 0.1195 0.041 Uiso 1 1 calc R . . Cl2 Cl 0.0357(2) 0.01001(19) 0.69046(15) 0.0965(8) Uani 1 1 d . . . Cl3 Cl 0.2591(3) -0.01747(18) 0.61797(16) 0.0986(8) Uani 1 1 d . . . C56 C 0.1695(8) 0.0628(7) 0.6708(6) 0.094(3) Uani 1 1 d . . . H56A H 0.2099 0.0797 0.7184 0.113 Uiso 1 1 calc R . . H56B H 0.1569 0.1243 0.6424 0.113 Uiso 1 1 calc R . . Cl4 Cl 0.4600(2) 0.37296(18) 0.26347(12) 0.0931(7) Uani 1 1 d . . . Cl5 Cl 0.2796(2) 0.51757(15) 0.28982(12) 0.0807(6) Uani 1 1 d . . . C57 C 0.4342(10) 0.4926(7) 0.3012(8) 0.120(4) Uani 1 1 d . . . H57A H 0.4810 0.5422 0.2741 0.144 Uiso 1 1 calc R . . H57B H 0.4565 0.4946 0.3549 0.144 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 Ru1 0.01905(17) 0.02485(17) 0.02111(18) -0.00193(15) 0.00135(13) -0.00250(15) Ru2 0.01588(15) 0.01690(15) 0.02066(16) -0.00130(14) 0.00325(12) -0.00074(14) Ru3 0.01499(15) 0.01945(16) 0.02070(17) -0.00025(14) 0.00256(12) -0.00081(14) Cl1 0.0296(6) 0.0210(5) 0.0312(6) 0.0015(5) 0.0036(5) 0.0034(5) P1 0.0178(5) 0.0226(5) 0.0232(6) 0.0001(4) 0.0019(5) -0.0013(4) P2 0.0149(5) 0.0179(5) 0.0225(6) -0.0006(4) 0.0029(4) -0.0005(4) O1 0.037(2) 0.054(2) 0.0269(19) -0.0056(17) 0.0045(16) -0.0253(18) C1 0.032(3) 0.040(3) 0.031(3) 0.004(2) 0.004(2) -0.003(2) C2 0.032(3) 0.048(3) 0.036(3) 0.015(3) 0.001(2) -0.004(3) C3 0.037(3) 0.050(3) 0.026(3) 0.011(2) 0.006(2) 0.005(3) C4 0.047(3) 0.037(3) 0.027(3) 0.002(2) 0.001(2) 0.006(3) C5 0.036(3) 0.037(3) 0.031(3) 0.003(2) -0.004(2) 0.006(3) C6 0.023(2) 0.022(2) 0.031(3) 0.0026(19) 0.001(2) 0.0048(18) C7 0.023(2) 0.025(2) 0.025(2) -0.0003(19) -0.0038(17) -0.001(2) C8 0.027(2) 0.034(3) 0.032(3) -0.006(2) -0.003(2) 0.006(2) C9 0.019(2) 0.034(2) 0.028(3) -0.008(2) 0.0030(19) 0.000(2) C10 0.019(2) 0.022(2) 0.024(2) -0.0040(17) -0.0001(18) -0.0052(18) C11 0.021(2) 0.026(2) 0.028(2) -0.0086(19) 0.0086(19) -0.0039(18) C12 0.022(2) 0.0168(19) 0.024(2) -0.0041(17) 0.0041(18) -0.0003(17) C13 0.023(2) 0.0135(19) 0.023(2) -0.0008(16) 0.0041(18) -0.0004(17) C14 0.019(2) 0.0195(19) 0.022(2) 0.0033(17) 0.0034(17) 0.0070(17) C15 0.0118(19) 0.0193(19) 0.025(2) 0.0012(17) 0.0011(17) 0.0022(16) C16 0.0159(18) 0.025(2) 0.020(2) -0.0042(19) 0.0037(15) -0.0035(19) C17 0.028(3) 0.036(3) 0.027(3) -0.001(2) 0.000(2) 0.002(2) C18 0.029(3) 0.061(4) 0.028(3) -0.003(3) -0.005(2) 0.001(3) C19 0.035(3) 0.055(3) 0.036(3) -0.011(3) 0.005(2) -0.025(3) C20 0.032(3) 0.038(3) 0.032(3) -0.003(2) 0.001(2) -0.019(2) C21 0.021(2) 0.032(3) 0.030(3) 0.000(2) 0.000(2) -0.006(2) C22 0.029(3) 0.031(2) 0.022(2) 0.0053(19) 0.001(2) 0.001(2) C23 0.030(3) 0.027(2) 0.031(3) 0.007(2) 0.004(2) -0.008(2) C24 0.015(2) 0.056(3) 0.045(3) -0.014(3) 0.002(2) 0.004(2) C25 0.029(3) 0.042(3) 0.045(3) 0.003(2) -0.008(2) 0.006(2) C26 0.032(3) 0.020(2) 0.033(3) -0.0045(19) -0.002(2) -0.0011(19) C27 0.036(3) 0.026(2) 0.026(3) -0.009(2) 0.005(2) -0.007(2) C28 0.028(2) 0.028(2) 0.027(3) -0.007(2) 0.000(2) -0.010(2) C29 0.029(3) 0.028(2) 0.026(3) -0.003(2) 0.001(2) -0.010(2) C30 0.042(3) 0.018(2) 0.026(3) -0.0015(19) -0.003(2) -0.005(2) C31 0.034(3) 0.035(3) 0.047(3) -0.009(2) -0.001(2) -0.001(2) C32 0.053(4) 0.043(3) 0.026(3) -0.004(2) 0.009(3) -0.005(3) C33 0.031(3) 0.041(3) 0.041(3) -0.006(2) -0.006(2) -0.009(2) C34 0.036(3) 0.050(3) 0.036(3) 0.001(3) 0.006(2) -0.015(3) C35 0.057(4) 0.030(3) 0.040(3) 0.001(2) -0.005(3) 0.000(3) C36 0.029(2) 0.0144(19) 0.030(3) -0.0026(18) 0.007(2) 0.0017(19) C37 0.023(2) 0.022(2) 0.030(3) -0.0026(19) 0.0050(19) 0.0059(19) C38 0.018(2) 0.025(2) 0.031(3) -0.0033(19) 0.0021(19) 0.0057(18) C39 0.021(2) 0.028(2) 0.029(3) -0.003(2) 0.0096(19) 0.0011(19) C40 0.025(2) 0.019(2) 0.025(2) -0.0075(17) 0.0063(19) 0.0006(18) C41 0.032(3) 0.021(2) 0.040(3) 0.002(2) 0.007(2) -0.003(2) C42 0.030(3) 0.035(3) 0.035(3) 0.000(2) -0.002(2) 0.006(2) C43 0.017(2) 0.037(2) 0.044(3) -0.005(3) 0.0019(19) 0.002(2) C44 0.031(2) 0.041(3) 0.034(3) -0.004(3) 0.010(2) -0.001(3) C45 0.036(3) 0.029(2) 0.029(3) -0.005(2) 0.007(2) -0.006(2) C46 0.0108(18) 0.029(2) 0.028(2) 0.0014(18) 0.0051(17) -0.0021(17) C47 0.020(2) 0.031(2) 0.024(2) 0.0002(18) 0.0070(18) -0.0041(18) C48 0.024(2) 0.032(2) 0.024(2) -0.004(2) 0.0061(19) 0.006(2) C49 0.025(2) 0.022(2) 0.029(3) -0.0044(19) 0.003(2) 0.0027(19) C50 0.0126(19) 0.021(2) 0.029(2) 0.0003(18) 0.0049(17) 0.0009(17) C51 0.023(2) 0.028(2) 0.037(3) 0.000(2) -0.003(2) -0.005(2) C52 0.031(3) 0.036(3) 0.036(3) 0.011(2) 0.004(2) -0.008(2) C53 0.039(3) 0.039(3) 0.028(3) -0.008(2) 0.002(2) 0.002(2) C54 0.049(3) 0.021(2) 0.040(3) -0.009(2) 0.004(3) 0.007(2) C55 0.019(2) 0.030(2) 0.034(3) 0.009(2) -0.0039(19) 0.0018(19) Cl2 0.0828(16) 0.0945(16) 0.1121(19) 0.0178(14) -0.0079(14) -0.0242(13) Cl3 0.1010(19) 0.0744(13) 0.120(2) 0.0137(14) -0.0008(16) 0.0113(13) C56 0.087(7) 0.094(7) 0.101(7) -0.008(6) -0.008(5) -0.030(6) Cl4 0.1226(19) 0.0793(14) 0.0776(14) 0.0065(13) 0.0105(13) 0.0329(16) Cl5 0.0996(17) 0.0668(12) 0.0757(13) 0.0013(10) 0.0133(12) 0.0056(11) C57 0.107(8) 0.055(5) 0.198(12) 0.013(6) 0.031(8) 0.021(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C9 2.175(5) . ? Ru1 C29 2.181(4) . ? Ru1 C30 2.186(5) . ? Ru1 C28 2.195(4) . ? Ru1 C10 2.205(4) . ? Ru1 C8 2.220(5) . ? Ru1 C27 2.223(5) . ? Ru1 C26 2.271(5) . ? Ru1 C7 2.282(5) . ? Ru1 P1 2.4138(12) . ? Ru2 C37 2.179(4) . ? Ru2 C14 2.185(4) . ? Ru2 C13 2.186(4) . ? Ru2 C38 2.186(4) . ? Ru2 C12 2.187(4) . ? Ru2 C36 2.191(4) . ? Ru2 C40 2.205(4) . ? Ru2 C39 2.211(5) . ? Ru2 C15 2.219(4) . ? Ru2 P2 2.3626(12) . ? Ru3 C49 2.175(5) . ? Ru3 C46 2.209(4) . ? Ru3 C50 2.213(4) . ? Ru3 C48 2.219(5) . ? Ru3 C47 2.245(4) . ? Ru3 P2 2.2594(12) . ? Ru3 P1 2.2773(12) . ? Ru3 Cl1 2.4644(12) . ? P1 C7 1.770(4) . ? P1 C10 1.772(5) . ? P2 C12 1.780(5) . ? P2 C15 1.785(4) . ? O1 C11 1.223(5) . ? C1 C2 1.378(7) . ? C1 C6 1.399(7) . ? C1 H1 0.9500 . ? C2 C3 1.377(8) . ? C2 H2 0.9500 . ? C3 C4 1.389(8) . ? C3 H3 0.9500 . ? C4 C5 1.350(7) . ? C4 H4 0.9500 . ? C5 C6 1.412(7) . ? C5 H5 0.9500 . ? C6 C7 1.483(7) . ? C7 C8 1.426(7) . ? C8 C9 1.434(7) . ? C8 C25 1.508(7) . ? C9 C10 1.431(6) . ? C9 C24 1.506(7) . ? C10 C11 1.514(6) . ? C11 C12 1.470(6) . ? C12 C13 1.452(6) . ? C13 C14 1.443(6) . ? C13 C23 1.501(6) . ? C14 C15 1.431(6) . ? C14 C22 1.499(6) . ? C15 C16 1.470(6) . ? C16 C21 1.405(7) . ? C16 C17 1.405(6) . ? C17 C18 1.388(7) . ? C17 H17 0.9500 . ? C18 C19 1.365(8) . ? C18 H18 0.9500 . ? C19 C20 1.409(8) . ? C19 H19 0.9500 . ? C20 C21 1.369(6) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C30 1.420(8) . ? C26 C27 1.420(7) . ? C26 C31 1.481(7) . ? C27 C28 1.430(7) . ? C27 C32 1.519(7) . ? C28 C29 1.416(7) . ? C28 C33 1.491(7) . ? C29 C30 1.419(7) . ? C29 C34 1.498(7) . ? C30 C35 1.527(7) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.421(7) . ? C36 C40 1.435(7) . ? C36 C41 1.508(7) . ? C37 C38 1.430(7) . ? C37 C42 1.501(7) . ? C38 C39 1.427(7) . ? C38 C43 1.495(6) . ? C39 C40 1.440(6) . ? C39 C44 1.505(7) . ? C40 C45 1.489(6) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C50 1.402(6) . ? C46 C47 1.466(6) . ? C46 C51 1.496(6) . ? C47 C48 1.411(7) . ? C47 C52 1.461(7) . ? C48 C49 1.449(7) . ? C48 C53 1.495(6) . ? C49 C50 1.446(6) . ? C49 C54 1.519(7) . ? C50 C55 1.500(6) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? Cl2 C56 1.728(9) . ? Cl3 C56 1.775(10) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? Cl4 C57 1.789(10) . ? Cl5 C57 1.810(11) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? 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 C9 Ru1 C29 103.09(19) . . ? C9 Ru1 C30 127.3(2) . . ? C29 Ru1 C30 37.94(19) . . ? C9 Ru1 C28 111.00(18) . . ? C29 Ru1 C28 37.75(18) . . ? C30 Ru1 C28 63.06(18) . . ? C9 Ru1 C10 38.14(17) . . ? C29 Ru1 C10 113.23(17) . . ? C30 Ru1 C10 112.16(17) . . ? C28 Ru1 C10 141.28(18) . . ? C9 Ru1 C8 38.06(19) . . ? C29 Ru1 C8 123.41(19) . . ? C30 Ru1 C8 160.2(2) . . ? C28 Ru1 C8 106.16(18) . . ? C10 Ru1 C8 64.81(17) . . ? C9 Ru1 C27 144.75(19) . . ? C29 Ru1 C27 62.88(18) . . ? C30 Ru1 C27 62.40(18) . . ? C28 Ru1 C27 37.75(18) . . ? C10 Ru1 C27 174.55(18) . . ? C8 Ru1 C27 120.32(19) . . ? C9 Ru1 C26 164.11(18) . . ? C29 Ru1 C26 62.45(19) . . ? C30 Ru1 C26 37.09(19) . . ? C28 Ru1 C26 62.32(18) . . ? C10 Ru1 C26 138.58(17) . . ? C8 Ru1 C26 154.94(18) . . ? C27 Ru1 C26 36.82(18) . . ? C9 Ru1 C7 64.90(18) . . ? C29 Ru1 C7 159.05(17) . . ? C30 Ru1 C7 162.61(18) . . ? C28 Ru1 C7 127.82(17) . . ? C10 Ru1 C7 68.81(16) . . ? C8 Ru1 C7 36.89(17) . . ? C27 Ru1 C7 116.27(17) . . ? C26 Ru1 C7 130.91(18) . . ? C9 Ru1 P1 70.70(12) . . ? C29 Ru1 P1 151.21(13) . . ? C30 Ru1 P1 123.49(14) . . ? C28 Ru1 P1 171.01(13) . . ? C10 Ru1 P1 44.85(12) . . ? C8 Ru1 P1 69.43(13) . . ? C27 Ru1 P1 137.10(13) . . ? C26 Ru1 P1 118.33(13) . . ? C7 Ru1 P1 44.17(11) . . ? C37 Ru2 C14 172.93(17) . . ? C37 Ru2 C13 141.16(17) . . ? C14 Ru2 C13 38.56(16) . . ? C37 Ru2 C38 38.25(18) . . ? C14 Ru2 C38 135.68(17) . . ? C13 Ru2 C38 111.30(17) . . ? C37 Ru2 C12 117.79(17) . . ? C14 Ru2 C12 66.38(16) . . ? C13 Ru2 C12 38.79(16) . . ? C38 Ru2 C12 112.44(17) . . ? C37 Ru2 C36 37.96(17) . . ? C14 Ru2 C36 140.73(17) . . ? C13 Ru2 C36 171.94(17) . . ? C38 Ru2 C36 63.43(18) . . ? C12 Ru2 C36 147.78(17) . . ? C37 Ru2 C40 64.08(18) . . ? C14 Ru2 C40 110.98(17) . . ? C13 Ru2 C40 134.74(17) . . ? C38 Ru2 C40 63.82(17) . . ? C12 Ru2 C40 172.19(17) . . ? C36 Ru2 C40 38.12(17) . . ? C37 Ru2 C39 63.71(18) . . ? C14 Ru2 C39 109.23(17) . . ? C13 Ru2 C39 108.71(17) . . ? C38 Ru2 C39 37.87(17) . . ? C12 Ru2 C39 134.81(17) . . ? C36 Ru2 C39 63.30(18) . . ? C40 Ru2 C39 38.07(17) . . ? C37 Ru2 C15 147.57(17) . . ? C14 Ru2 C15 37.90(16) . . ? C13 Ru2 C15 66.26(16) . . ? C38 Ru2 C15 171.99(17) . . ? C12 Ru2 C15 70.83(16) . . ? C36 Ru2 C15 118.03(17) . . ? C40 Ru2 C15 111.96(17) . . ? C39 Ru2 C15 134.65(17) . . ? C37 Ru2 P2 115.53(13) . . ? C14 Ru2 P2 71.53(12) . . ? C13 Ru2 P2 72.18(12) . . ? C38 Ru2 P2 141.82(13) . . ? C12 Ru2 P2 45.85(12) . . ? C36 Ru2 P2 115.81(13) . . ? C40 Ru2 P2 141.32(12) . . ? C39 Ru2 P2 179.10(13) . . ? C15 Ru2 P2 45.71(12) . . ? C49 Ru3 C46 63.47(17) . . ? C49 Ru3 C50 38.46(17) . . ? C46 Ru3 C50 36.96(16) . . ? C49 Ru3 C48 38.49(18) . . ? C46 Ru3 C48 62.99(17) . . ? C50 Ru3 C48 63.43(17) . . ? C49 Ru3 C47 63.43(18) . . ? C46 Ru3 C47 38.42(17) . . ? C50 Ru3 C47 63.05(17) . . ? C48 Ru3 C47 36.84(17) . . ? C49 Ru3 P2 107.03(14) . . ? C46 Ru3 P2 117.32(12) . . ? C50 Ru3 P2 95.13(12) . . ? C48 Ru3 P2 144.28(13) . . ? C47 Ru3 P2 155.58(12) . . ? C49 Ru3 P1 106.49(13) . . ? C46 Ru3 P1 158.79(12) . . ? C50 Ru3 P1 142.69(12) . . ? C48 Ru3 P1 97.21(13) . . ? C47 Ru3 P1 120.82(12) . . ? P2 Ru3 P1 83.00(4) . . ? C49 Ru3 Cl1 154.13(13) . . ? C46 Ru3 Cl1 92.79(12) . . ? C50 Ru3 Cl1 125.07(12) . . ? C48 Ru3 Cl1 123.00(13) . . ? C47 Ru3 Cl1 91.79(12) . . ? P2 Ru3 Cl1 92.60(4) . . ? P1 Ru3 Cl1 92.22(4) . . ? C7 P1 C10 91.4(2) . . ? C7 P1 Ru3 133.57(17) . . ? C10 P1 Ru3 128.55(16) . . ? C7 P1 Ru1 63.96(17) . . ? C10 P1 Ru1 61.33(14) . . ? Ru3 P1 Ru1 150.67(6) . . ? C12 P2 C15 91.5(2) . . ? C12 P2 Ru3 128.77(15) . . ? C15 P2 Ru3 135.87(15) . . ? C12 P2 Ru2 61.85(14) . . ? C15 P2 Ru2 62.89(14) . . ? Ru3 P2 Ru2 146.59(5) . . ? C2 C1 C6 120.6(5) . . ? C2 C1 H1 119.7 . . ? C6 C1 H1 119.7 . . ? C3 C2 C1 120.7(5) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C2 C3 C4 119.2(5) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C5 C4 C3 120.8(5) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 121.2(5) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C1 C6 C5 117.5(5) . . ? C1 C6 C7 120.1(4) . . ? C5 C6 C7 122.4(4) . . ? C8 C7 C6 124.9(4) . . ? C8 C7 P1 111.2(4) . . ? C6 C7 P1 123.9(3) . . ? C8 C7 Ru1 69.2(3) . . ? C6 C7 Ru1 126.9(3) . . ? P1 C7 Ru1 71.87(18) . . ? C7 C8 C9 113.7(4) . . ? C7 C8 C25 124.3(5) . . ? C9 C8 C25 121.7(5) . . ? C7 C8 Ru1 73.9(3) . . ? C9 C8 Ru1 69.3(3) . . ? C25 C8 Ru1 130.2(4) . . ? C10 C9 C8 111.7(4) . . ? C10 C9 C24 126.7(5) . . ? C8 C9 C24 121.3(5) . . ? C10 C9 Ru1 72.1(3) . . ? C8 C9 Ru1 72.7(3) . . ? C24 C9 Ru1 127.5(4) . . ? C9 C10 C11 123.6(4) . . ? C9 C10 P1 112.0(3) . . ? C11 C10 P1 124.3(3) . . ? C9 C10 Ru1 69.8(3) . . ? C11 C10 Ru1 121.0(3) . . ? P1 C10 Ru1 73.82(17) . . ? O1 C11 C12 121.9(4) . . ? O1 C11 C10 119.9(4) . . ? C12 C11 C10 118.2(4) . . ? C13 C12 C11 122.2(4) . . ? C13 C12 P2 111.9(3) . . ? C11 C12 P2 125.5(3) . . ? C13 C12 Ru2 70.6(2) . . ? C11 C12 Ru2 118.4(3) . . ? P2 C12 Ru2 72.30(15) . . ? C14 C13 C12 111.5(4) . . ? C14 C13 C23 123.0(4) . . ? C12 C13 C23 125.5(4) . . ? C14 C13 Ru2 70.7(2) . . ? C12 C13 Ru2 70.6(2) . . ? C23 C13 Ru2 127.5(3) . . ? C15 C14 C13 113.8(4) . . ? C15 C14 C22 123.9(4) . . ? C13 C14 C22 122.3(4) . . ? C15 C14 Ru2 72.3(2) . . ? C13 C14 Ru2 70.8(2) . . ? C22 C14 Ru2 124.0(3) . . ? C14 C15 C16 124.6(4) . . ? C14 C15 P2 111.3(3) . . ? C16 C15 P2 124.1(3) . . ? C14 C15 Ru2 69.8(2) . . ? C16 C15 Ru2 125.3(3) . . ? P2 C15 Ru2 71.40(14) . . ? C21 C16 C17 117.6(4) . . ? C21 C16 C15 120.6(4) . . ? C17 C16 C15 121.8(4) . . ? C18 C17 C16 120.5(5) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C19 C18 C17 120.7(5) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C18 C19 C20 119.9(5) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C21 C20 C19 119.4(5) . . ? C21 C20 H20 120.3 . . ? C19 C20 H20 120.3 . . ? C20 C21 C16 121.7(5) . . ? C20 C21 H21 119.1 . . ? C16 C21 H21 119.1 . . ? C14 C22 H22A 109.5 . . ? C14 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C14 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C13 C23 H23A 109.5 . . ? C13 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C13 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C9 C24 H24A 109.5 . . ? C9 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C9 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C8 C25 H25A 109.5 . . ? C8 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C8 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C30 C26 C27 107.1(5) . . ? C30 C26 C31 127.6(5) . . ? C27 C26 C31 124.7(5) . . ? C30 C26 Ru1 68.2(3) . . ? C27 C26 Ru1 69.7(3) . . ? C31 C26 Ru1 134.3(3) . . ? C26 C27 C28 108.5(4) . . ? C26 C27 C32 124.4(5) . . ? C28 C27 C32 126.1(5) . . ? C26 C27 Ru1 73.5(3) . . ? C28 C27 Ru1 70.1(3) . . ? C32 C27 Ru1 131.2(3) . . ? C29 C28 C27 107.6(4) . . ? C29 C28 C33 127.2(5) . . ? C27 C28 C33 125.1(5) . . ? C29 C28 Ru1 70.6(3) . . ? C27 C28 Ru1 72.1(3) . . ? C33 C28 Ru1 125.8(3) . . ? C28 C29 C30 107.8(4) . . ? C28 C29 C34 127.7(5) . . ? C30 C29 C34 124.3(5) . . ? C28 C29 Ru1 71.7(3) . . ? C30 C29 Ru1 71.2(3) . . ? C34 C29 Ru1 126.6(4) . . ? C29 C30 C26 108.9(4) . . ? C29 C30 C35 125.6(5) . . ? C26 C30 C35 125.3(5) . . ? C29 C30 Ru1 70.9(3) . . ? C26 C30 Ru1 74.7(3) . . ? C35 C30 Ru1 125.0(3) . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C27 C32 H32A 109.5 . . ? C27 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C27 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C28 C33 H33A 109.5 . . ? C28 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C28 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C29 C34 H34A 109.5 . . ? C29 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C29 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C30 C35 H35A 109.5 . . ? C30 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C30 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 C36 C40 109.0(4) . . ? C37 C36 C41 125.7(4) . . ? C40 C36 C41 124.8(4) . . ? C37 C36 Ru2 70.6(3) . . ? C40 C36 Ru2 71.5(2) . . ? C41 C36 Ru2 130.7(3) . . ? C36 C37 C38 107.6(4) . . ? C36 C37 C42 124.0(4) . . ? C38 C37 C42 128.2(4) . . ? C36 C37 Ru2 71.5(3) . . ? C38 C37 Ru2 71.1(3) . . ? C42 C37 Ru2 127.3(3) . . ? C39 C38 C37 108.4(4) . . ? C39 C38 C43 124.5(4) . . ? C37 C38 C43 127.0(4) . . ? C39 C38 Ru2 72.0(3) . . ? C37 C38 Ru2 70.6(3) . . ? C43 C38 Ru2 126.5(3) . . ? C38 C39 C40 108.1(4) . . ? C38 C39 C44 125.2(4) . . ? C40 C39 C44 126.6(4) . . ? C38 C39 Ru2 70.1(3) . . ? C40 C39 Ru2 70.7(3) . . ? C44 C39 Ru2 127.2(3) . . ? C36 C40 C39 106.9(4) . . ? C36 C40 C45 127.2(4) . . ? C39 C40 C45 125.7(4) . . ? C36 C40 Ru2 70.4(2) . . ? C39 C40 Ru2 71.2(3) . . ? C45 C40 Ru2 127.0(3) . . ? C36 C41 H41A 109.5 . . ? C36 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C36 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C37 C42 H42A 109.5 . . ? C37 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C37 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C38 C43 H43A 109.5 . . ? C38 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C38 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C39 C44 H44A 109.5 . . ? C39 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C39 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C40 C45 H45A 109.5 . . ? C40 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C40 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C50 C46 C47 108.7(4) . . ? C50 C46 C51 128.7(4) . . ? C47 C46 C51 122.4(4) . . ? C50 C46 Ru3 71.7(2) . . ? C47 C46 Ru3 72.1(2) . . ? C51 C46 Ru3 125.1(3) . . ? C48 C47 C52 129.4(4) . . ? C48 C47 C46 107.0(4) . . ? C52 C47 C46 123.5(4) . . ? C48 C47 Ru3 70.6(3) . . ? C52 C47 Ru3 127.8(4) . . ? C46 C47 Ru3 69.5(2) . . ? C47 C48 C49 108.7(4) . . ? C47 C48 C53 126.0(4) . . ? C49 C48 C53 125.1(4) . . ? C47 C48 Ru3 72.6(3) . . ? C49 C48 Ru3 69.1(3) . . ? C53 C48 Ru3 127.2(3) . . ? C50 C49 C48 107.2(4) . . ? C50 C49 C54 125.9(5) . . ? C48 C49 C54 126.3(4) . . ? C50 C49 Ru3 72.2(2) . . ? C48 C49 Ru3 72.4(3) . . ? C54 C49 Ru3 127.7(4) . . ? C46 C50 C49 108.2(4) . . ? C46 C50 C55 127.5(4) . . ? C49 C50 C55 124.1(4) . . ? C46 C50 Ru3 71.4(2) . . ? C49 C50 Ru3 69.4(2) . . ? C55 C50 Ru3 129.7(3) . . ? C46 C51 H51A 109.5 . . ? C46 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C46 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C47 C52 H52A 109.5 . . ? C47 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C47 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C48 C53 H53A 109.5 . . ? C48 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C48 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C49 C54 H54A 109.5 . . ? C49 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C49 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C50 C55 H55A 109.5 . . ? C50 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C50 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? Cl2 C56 Cl3 111.5(5) . . ? Cl2 C56 H56A 109.3 . . ? Cl3 C56 H56A 109.3 . . ? Cl2 C56 H56B 109.3 . . ? Cl3 C56 H56B 109.3 . . ? H56A C56 H56B 108.0 . . ? Cl4 C57 Cl5 107.0(6) . . ? Cl4 C57 H57A 110.3 . . ? Cl5 C57 H57A 110.3 . . ? Cl4 C57 H57B 110.3 . . ? Cl5 C57 H57B 110.3 . . ? H57A C57 H57B 108.6 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.033 _refine_diff_density_min -1.218 _refine_diff_density_rms 0.118 #===END #compound 33 data_em159 _database_code_depnum_ccdc_archive 'CCDC 837332' #TrackingRef '2011_carmichael_dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C57 H71 Cl5 Fe O P2 Ru2' _chemical_formula_sum 'C57 H71 Cl5 Fe O P2 Ru2' _chemical_formula_weight 1269.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21 ' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.357(1) _cell_length_b 13.490(1) _cell_length_c 17.956(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.110(1) _cell_angle_gamma 90.00 _cell_volume 2751.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 4038 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 30.034 _exptl_crystal_description Plate _exptl_crystal_colour Red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.532 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1300 _exptl_absorpt_coefficient_mu 1.142 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8751 _exptl_absorpt_correction_T_max 0.9775 _exptl_absorpt_process_details 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _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 11232 _diffrn_reflns_av_R_equivalents 0.0603 _diffrn_reflns_av_sigmaI/netI 0.1230 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 25.02 _reflns_number_total 7436 _reflns_number_gt 5389 _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^)+(0.0271P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.05(3) _refine_ls_number_reflns 7436 _refine_ls_number_parameters 632 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0820 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.1000 _refine_ls_wR_factor_gt 0.0897 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.947 _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 Ru1 Ru 0.86594(6) 1.04321(5) 0.34650(4) 0.02517(19) Uani 1 1 d . . . Fe1 Fe 0.81260(8) 0.86860(9) 0.03825(6) 0.0158(3) Uani 1 1 d . . . Ru2 Ru 0.57153(5) 0.87837(5) 0.22848(4) 0.02322(19) Uani 1 1 d . . . Cl1 Cl 0.6223(2) 0.70086(17) 0.22768(14) 0.0321(6) Uani 1 1 d . . . P1 P 0.74434(19) 0.92180(17) 0.28354(13) 0.0233(6) Uani 1 1 d . . . P2 P 0.67188(19) 0.91143(16) 0.12252(13) 0.0245(6) Uani 1 1 d . . . O1 O 0.9631(5) 1.0723(5) 0.1542(3) 0.046(2) Uani 1 1 d . . . C1 C 0.6794(8) 0.7609(7) 0.4205(6) 0.033(2) Uani 1 1 d . . . H1 H 0.6584 0.7398 0.3718 0.039 Uiso 1 1 calc R . . C2 C 0.6273(8) 0.7182(7) 0.4823(6) 0.041(3) Uani 1 1 d . . . H2 H 0.5728 0.6656 0.4757 0.049 Uiso 1 1 calc R . . C3 C 0.6533(8) 0.7510(8) 0.5537(6) 0.039(3) Uani 1 1 d . . . H3 H 0.6167 0.7208 0.5955 0.047 Uiso 1 1 calc R . . C4 C 0.7329(9) 0.8281(7) 0.5639(6) 0.040(3) Uani 1 1 d . . . H4 H 0.7493 0.8522 0.6126 0.048 Uiso 1 1 calc R . . C5 C 0.7886(7) 0.8701(8) 0.5020(5) 0.036(2) Uani 1 1 d . . . H5 H 0.8437 0.9222 0.5091 0.043 Uiso 1 1 calc R . . C6 C 0.7651(7) 0.8370(7) 0.4308(5) 0.029(2) Uani 1 1 d . . . C7 C 0.8200(7) 0.8802(8) 0.3628(5) 0.0252(19) Uani 1 1 d . . . C8 C 0.9454(7) 0.8930(7) 0.3549(5) 0.031(2) Uani 1 1 d . . . C9 C 0.9767(7) 0.9419(7) 0.2887(5) 0.028(2) Uani 1 1 d . . . C10 C 0.8764(7) 0.9608(6) 0.2415(5) 0.027(2) Uani 1 1 d . . . C11 C 0.8841(7) 1.0114(7) 0.1673(5) 0.026(2) Uani 1 1 d . . . C12 C 0.7979(7) 0.9894(6) 0.1095(5) 0.026(2) Uani 1 1 d . . . C13 C 0.8064(7) 1.0234(7) 0.0329(5) 0.023(2) Uani 1 1 d . . . C14 C 0.7185(8) 0.9805(6) -0.0147(5) 0.026(2) Uani 1 1 d . . . C15 C 0.6377(7) 0.9181(6) 0.0264(5) 0.025(2) Uani 1 1 d . . . C16 C 0.5366(7) 0.8646(7) -0.0085(5) 0.027(2) Uani 1 1 d . . . C17 C 0.4658(7) 0.9081(7) -0.0627(5) 0.031(2) Uani 1 1 d . . . H17 H 0.4805 0.9746 -0.0774 0.037 Uiso 1 1 calc R . . C18 C 0.3737(7) 0.8561(8) -0.0957(5) 0.036(3) Uani 1 1 d . . . H18 H 0.3268 0.8865 -0.1332 0.043 Uiso 1 1 calc R . . C19 C 0.3515(8) 0.7621(9) -0.0743(6) 0.045(3) Uani 1 1 d . . . H19 H 0.2888 0.7270 -0.0974 0.054 Uiso 1 1 calc R . . C20 C 0.4171(8) 0.7155(8) -0.0200(6) 0.038(3) Uani 1 1 d . . . H20 H 0.3994 0.6493 -0.0058 0.046 Uiso 1 1 calc R . . C21 C 0.5093(8) 0.7663(6) 0.0138(5) 0.030(2) Uani 1 1 d . . . H21 H 0.5542 0.7351 0.0519 0.036 Uiso 1 1 calc R . . C22 C 0.7112(8) 0.9992(7) -0.0950(5) 0.033(2) Uani 1 1 d . . . H22A H 0.6623 1.0578 -0.1041 0.049 Uiso 1 1 calc R . . H22B H 0.6761 0.9416 -0.1198 0.049 Uiso 1 1 calc R . . H22C H 0.7904 1.0106 -0.1147 0.049 Uiso 1 1 calc R . . C23 C 0.8949(8) 1.0965(7) 0.0060(5) 0.033(2) Uani 1 1 d . . . H23A H 0.8929 1.0991 -0.0485 0.050 Uiso 1 1 calc R . . H23B H 0.9736 1.0763 0.0226 0.050 Uiso 1 1 calc R . . H23C H 0.8765 1.1622 0.0262 0.050 Uiso 1 1 calc R . . C24 C 1.1057(7) 0.9520(8) 0.2664(5) 0.037(3) Uani 1 1 d . . . H24A H 1.1520 0.9740 0.3094 0.055 Uiso 1 1 calc R . . H24B H 1.1127 1.0008 0.2262 0.055 Uiso 1 1 calc R . . H24C H 1.1352 0.8878 0.2491 0.055 Uiso 1 1 calc R . . C25 C 1.0363(7) 0.8523(7) 0.4091(5) 0.039(3) Uani 1 1 d . . . H25A H 1.0682 0.7900 0.3896 0.058 Uiso 1 1 calc R . . H25B H 0.9990 0.8401 0.4574 0.058 Uiso 1 1 calc R . . H25C H 1.1002 0.9005 0.4152 0.058 Uiso 1 1 calc R . . C26 C 0.7809(8) 1.1818(7) 0.3914(6) 0.033(2) Uani 1 1 d . . . C27 C 0.8519(8) 1.1393(7) 0.4459(5) 0.030(2) Uani 1 1 d . . . C28 C 0.9692(8) 1.1397(7) 0.4203(5) 0.030(2) Uani 1 1 d . . . C29 C 0.9700(8) 1.1783(7) 0.3465(6) 0.032(2) Uani 1 1 d . . . C30 C 0.8514(8) 1.2027(7) 0.3277(5) 0.029(2) Uani 1 1 d . . . C31 C 0.6548(7) 1.2149(7) 0.4029(6) 0.037(3) Uani 1 1 d . . . H31A H 0.6540 1.2772 0.4310 0.055 Uiso 1 1 calc R . . H31B H 0.6120 1.1639 0.4307 0.055 Uiso 1 1 calc R . . H31C H 0.6169 1.2250 0.3544 0.055 Uiso 1 1 calc R . . C32 C 0.8114(8) 1.1184(7) 0.5245(5) 0.042(3) Uani 1 1 d . . . H32A H 0.7968 1.1812 0.5504 0.063 Uiso 1 1 calc R . . H32B H 0.8724 1.0811 0.5510 0.063 Uiso 1 1 calc R . . H32C H 0.7386 1.0794 0.5230 0.063 Uiso 1 1 calc R . . C33 C 1.0759(7) 1.1083(8) 0.4658(6) 0.041(3) Uani 1 1 d . . . H33A H 1.1304 1.0712 0.4341 0.062 Uiso 1 1 calc R . . H33B H 1.0504 1.0663 0.5073 0.062 Uiso 1 1 calc R . . H33C H 1.1156 1.1673 0.4854 0.062 Uiso 1 1 calc R . . C34 C 1.0739(8) 1.2006(8) 0.2982(5) 0.044(3) Uani 1 1 d . . . H34A H 1.0892 1.2721 0.2986 0.066 Uiso 1 1 calc R . . H34B H 1.0576 1.1790 0.2472 0.066 Uiso 1 1 calc R . . H34C H 1.1431 1.1654 0.3173 0.066 Uiso 1 1 calc R . . C35 C 0.8127(9) 1.2519(7) 0.2565(6) 0.046(3) Uani 1 1 d . . . H35A H 0.7273 1.2446 0.2507 0.068 Uiso 1 1 calc R . . H35B H 0.8526 1.2206 0.2142 0.068 Uiso 1 1 calc R . . H35C H 0.8329 1.3225 0.2581 0.068 Uiso 1 1 calc R . . C36 C 0.8350(8) 0.7155(7) 0.0313(5) 0.025(2) Uani 1 1 d . . . C37 C 0.9198(7) 0.7565(6) 0.0785(5) 0.026(2) Uani 1 1 d . . . C38 C 0.9891(7) 0.8250(6) 0.0356(5) 0.026(2) Uani 1 1 d . . . C39 C 0.9444(7) 0.8272(7) -0.0384(6) 0.032(2) Uani 1 1 d . . . C40 C 0.8452(7) 0.7587(6) -0.0419(5) 0.026(2) Uani 1 1 d . . . C41 C 0.7574(8) 0.6279(7) 0.0497(5) 0.034(3) Uani 1 1 d . . . H41A H 0.6906 0.6259 0.0151 0.052 Uiso 1 1 calc R . . H41B H 0.7282 0.6343 0.1008 0.052 Uiso 1 1 calc R . . H41C H 0.8031 0.5665 0.0451 0.052 Uiso 1 1 calc R . . C42 C 0.9422(8) 0.7247(8) 0.1574(5) 0.040(3) Uani 1 1 d . . . H42A H 0.8673 0.7085 0.1814 0.060 Uiso 1 1 calc R . . H42B H 0.9808 0.7786 0.1846 0.060 Uiso 1 1 calc R . . H42C H 0.9933 0.6661 0.1575 0.060 Uiso 1 1 calc R . . C43 C 1.0976(6) 0.8807(8) 0.0607(5) 0.037(2) Uani 1 1 d . . . H43A H 1.1662 0.8570 0.0329 0.056 Uiso 1 1 calc R . . H43B H 1.1102 0.8696 0.1140 0.056 Uiso 1 1 calc R . . H43C H 1.0867 0.9517 0.0514 0.056 Uiso 1 1 calc R . . C44 C 0.9960(7) 0.8831(8) -0.1039(5) 0.040(2) Uani 1 1 d . . . H44A H 1.0097 0.9523 -0.0896 0.060 Uiso 1 1 calc R . . H44B H 0.9409 0.8807 -0.1459 0.060 Uiso 1 1 calc R . . H44C H 1.0708 0.8525 -0.1184 0.060 Uiso 1 1 calc R . . C45 C 0.7753(9) 0.7321(8) -0.1086(5) 0.041(3) Uani 1 1 d . . . H45A H 0.8081 0.6722 -0.1314 0.061 Uiso 1 1 calc R . . H45B H 0.7780 0.7868 -0.1446 0.061 Uiso 1 1 calc R . . H45C H 0.6934 0.7199 -0.0941 0.061 Uiso 1 1 calc R . . C46 C 0.3806(7) 0.8473(6) 0.2185(5) 0.024(2) Uani 1 1 d . . . C47 C 0.4104(8) 0.8479(7) 0.2960(5) 0.030(2) Uani 1 1 d . . . C48 C 0.4532(7) 0.9453(7) 0.3142(5) 0.027(2) Uani 1 1 d . . . C49 C 0.4524(7) 1.0020(6) 0.2469(5) 0.022(2) Uani 1 1 d . . . C50 C 0.4004(7) 0.9417(7) 0.1892(5) 0.028(2) Uani 1 1 d . . . C51 C 0.3277(7) 0.7587(6) 0.1812(5) 0.029(2) Uani 1 1 d . . . H51A H 0.2481 0.7478 0.2005 0.044 Uiso 1 1 calc R . . H51B H 0.3764 0.7003 0.1915 0.044 Uiso 1 1 calc R . . H51C H 0.3240 0.7701 0.1274 0.044 Uiso 1 1 calc R . . C52 C 0.3891(8) 0.7642(7) 0.3477(5) 0.037(3) Uani 1 1 d . . . H52A H 0.4118 0.7837 0.3983 0.056 Uiso 1 1 calc R . . H52B H 0.4359 0.7069 0.3321 0.056 Uiso 1 1 calc R . . H52C H 0.3053 0.7468 0.3468 0.056 Uiso 1 1 calc R . . C53 C 0.4893(9) 0.9824(7) 0.3897(5) 0.040(3) Uani 1 1 d . . . H53A H 0.4968 0.9262 0.4240 0.059 Uiso 1 1 calc R . . H53B H 0.4296 1.0284 0.4085 0.059 Uiso 1 1 calc R . . H53C H 0.5651 1.0167 0.3860 0.059 Uiso 1 1 calc R . . C54 C 0.4802(8) 1.1141(7) 0.2395(6) 0.044(3) Uani 1 1 d . . . H54A H 0.5042 1.1286 0.1882 0.066 Uiso 1 1 calc R . . H54B H 0.5442 1.1317 0.2737 0.066 Uiso 1 1 calc R . . H54C H 0.4099 1.1528 0.2518 0.066 Uiso 1 1 calc R . . C55 C 0.3692(7) 0.9792(7) 0.1134(5) 0.028(2) Uani 1 1 d . . . H55A H 0.3553 0.9230 0.0800 0.042 Uiso 1 1 calc R . . H55B H 0.4340 1.0196 0.0941 0.042 Uiso 1 1 calc R . . H55C H 0.2977 1.0197 0.1164 0.042 Uiso 1 1 calc R . . Cl2 Cl 0.0284(3) 0.0139(3) 0.6882(2) 0.0964(14) Uani 1 1 d . . . Cl3 Cl 0.2557(4) -0.0161(3) 0.6203(3) 0.0968(13) Uani 1 1 d . . . C56 C 0.1654(10) 0.0618(12) 0.6695(8) 0.093(5) Uani 1 1 d . . . H56A H 0.1557 0.1241 0.6410 0.111 Uiso 1 1 calc R . . H56B H 0.2044 0.0787 0.7172 0.111 Uiso 1 1 calc R . . Cl4 Cl 0.4588(3) 0.3741(3) 0.26315(17) 0.0837(10) Uani 1 1 d . . . Cl5 Cl 0.2770(3) 0.5191(2) 0.29082(18) 0.0717(10) Uani 1 1 d . . . C57 C 0.4290(10) 0.4911(9) 0.2985(9) 0.088(5) Uani 1 1 d . . . H57A H 0.4753 0.5412 0.2709 0.106 Uiso 1 1 calc R . . H57B H 0.4530 0.4939 0.3515 0.106 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 Ru1 0.0213(4) 0.0302(4) 0.0241(4) -0.0019(4) -0.0008(3) -0.0014(4) Fe1 0.0129(5) 0.0177(6) 0.0167(7) -0.0019(6) 0.0020(5) -0.0009(6) Ru2 0.0187(4) 0.0269(4) 0.0241(4) 0.0004(4) 0.0010(3) -0.0015(4) Cl1 0.0307(13) 0.0305(14) 0.0351(16) -0.0004(12) 0.0012(11) 0.0021(12) P1 0.0213(12) 0.0278(13) 0.0208(14) -0.0006(11) -0.0007(10) -0.0001(11) P2 0.0224(12) 0.0252(14) 0.0259(15) 0.0002(11) -0.0001(11) -0.0004(10) O1 0.042(4) 0.068(6) 0.028(4) -0.011(4) 0.007(3) -0.020(4) C1 0.034(6) 0.037(6) 0.027(6) 0.005(5) 0.000(5) 0.003(5) C2 0.035(6) 0.040(6) 0.048(8) 0.010(6) -0.002(5) -0.012(5) C3 0.033(6) 0.052(7) 0.031(7) 0.009(6) 0.000(5) 0.005(6) C4 0.055(7) 0.042(6) 0.024(6) 0.002(5) 0.008(5) 0.011(6) C5 0.037(5) 0.028(5) 0.042(6) 0.000(6) -0.002(5) 0.007(5) C6 0.029(5) 0.033(6) 0.026(6) 0.003(5) -0.008(4) 0.014(4) C7 0.021(4) 0.029(5) 0.026(5) 0.001(5) 0.002(4) -0.006(5) C8 0.029(5) 0.037(6) 0.027(6) 0.003(5) -0.008(4) 0.009(5) C9 0.025(5) 0.037(6) 0.023(6) -0.006(5) 0.001(4) 0.005(5) C10 0.017(5) 0.024(5) 0.039(7) -0.001(5) -0.001(4) 0.011(4) C11 0.019(5) 0.034(6) 0.026(6) -0.012(5) 0.003(4) -0.001(4) C12 0.020(5) 0.025(5) 0.034(7) 0.001(5) 0.000(4) -0.006(4) C13 0.014(4) 0.034(6) 0.022(5) -0.003(5) 0.009(4) 0.009(4) C14 0.025(5) 0.024(5) 0.030(6) 0.002(4) 0.009(4) -0.004(4) C15 0.021(5) 0.014(4) 0.040(6) -0.004(4) -0.006(4) 0.004(4) C16 0.024(4) 0.030(5) 0.027(5) -0.002(5) 0.002(4) -0.005(5) C17 0.034(5) 0.036(6) 0.023(6) 0.003(5) -0.007(4) 0.001(5) C18 0.030(5) 0.051(8) 0.026(6) 0.002(5) -0.008(4) -0.006(5) C19 0.024(6) 0.070(8) 0.040(7) -0.011(6) -0.001(5) -0.020(6) C20 0.042(6) 0.041(6) 0.031(7) 0.000(5) -0.007(5) -0.016(5) C21 0.026(5) 0.037(6) 0.027(6) -0.006(5) -0.012(5) -0.003(5) C22 0.031(5) 0.041(6) 0.026(6) 0.003(5) -0.006(5) -0.005(5) C23 0.043(6) 0.025(5) 0.031(6) 0.008(5) 0.002(5) -0.003(5) C24 0.024(5) 0.062(7) 0.025(6) -0.008(5) 0.003(4) 0.007(5) C25 0.033(5) 0.044(7) 0.039(6) 0.004(5) -0.015(5) 0.003(5) C26 0.037(6) 0.031(6) 0.029(6) -0.007(5) -0.001(5) -0.010(5) C27 0.031(5) 0.033(6) 0.025(6) -0.003(5) 0.006(5) -0.009(5) C28 0.039(6) 0.031(6) 0.021(6) -0.003(5) -0.004(5) -0.009(5) C29 0.037(6) 0.026(6) 0.032(7) -0.006(5) -0.012(5) -0.001(5) C30 0.037(6) 0.028(6) 0.022(6) 0.002(5) -0.004(5) -0.007(5) C31 0.033(5) 0.030(6) 0.046(7) -0.005(5) 0.002(5) -0.003(5) C32 0.046(6) 0.041(6) 0.040(7) -0.013(5) 0.008(5) -0.009(5) C33 0.023(5) 0.063(7) 0.038(7) -0.011(6) -0.011(5) -0.009(5) C34 0.045(6) 0.060(7) 0.028(6) -0.003(6) 0.002(5) -0.020(6) C35 0.064(7) 0.038(6) 0.034(7) 0.003(5) -0.001(6) 0.006(6) C36 0.035(6) 0.023(5) 0.018(6) -0.003(4) 0.004(5) 0.000(5) C37 0.025(5) 0.027(5) 0.025(6) -0.005(5) 0.000(4) 0.000(4) C38 0.027(5) 0.026(5) 0.024(6) -0.005(4) 0.001(4) 0.010(4) C39 0.025(5) 0.028(5) 0.042(7) -0.003(5) 0.007(5) 0.002(4) C40 0.023(5) 0.030(5) 0.026(6) -0.004(4) 0.003(4) 0.001(4) C41 0.032(5) 0.034(6) 0.037(7) -0.003(5) 0.009(5) 0.006(5) C42 0.043(6) 0.047(7) 0.031(7) -0.001(5) -0.002(5) 0.002(5) C43 0.017(4) 0.047(6) 0.048(6) -0.004(6) -0.008(4) 0.006(5) C44 0.033(5) 0.056(6) 0.030(6) -0.008(6) 0.018(4) -0.010(6) C45 0.046(6) 0.054(7) 0.022(6) -0.003(5) 0.003(5) -0.002(6) C46 0.015(4) 0.035(6) 0.021(6) -0.003(4) -0.008(4) -0.003(4) C47 0.033(5) 0.036(6) 0.020(6) 0.006(4) 0.002(4) -0.001(4) C48 0.017(5) 0.041(6) 0.022(6) -0.001(5) 0.003(4) 0.005(4) C49 0.008(4) 0.028(5) 0.029(6) 0.004(4) 0.001(4) -0.005(4) C50 0.024(5) 0.034(6) 0.025(6) 0.005(5) -0.001(4) 0.005(5) C51 0.017(5) 0.035(6) 0.036(6) -0.004(5) 0.004(4) -0.001(4) C52 0.029(6) 0.044(7) 0.038(7) 0.017(5) 0.013(5) -0.001(5) C53 0.046(6) 0.047(7) 0.026(6) -0.005(5) 0.015(5) 0.007(5) C54 0.041(6) 0.031(6) 0.061(8) -0.015(6) -0.009(6) 0.005(5) C55 0.023(5) 0.032(6) 0.030(6) 0.008(5) -0.004(4) 0.009(4) Cl2 0.071(2) 0.115(4) 0.104(3) 0.021(3) -0.015(2) -0.027(2) Cl3 0.104(3) 0.071(2) 0.116(4) 0.005(2) 0.005(3) 0.014(2) C56 0.061(9) 0.117(13) 0.100(12) -0.041(10) 0.012(8) -0.025(9) Cl4 0.110(3) 0.079(2) 0.062(2) 0.005(2) 0.0068(19) 0.027(3) Cl5 0.084(2) 0.069(2) 0.062(2) 0.0055(17) 0.0078(17) 0.0050(18) C57 0.060(9) 0.058(8) 0.146(15) 0.007(9) 0.025(9) 0.003(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 Ru1 C9 2.129(8) . ? Ru1 C29 2.172(9) . ? Ru1 C30 2.185(10) . ? Ru1 C10 2.192(9) . ? Ru1 C28 2.194(9) . ? Ru1 C27 2.213(9) . ? Ru1 C8 2.223(9) . ? Ru1 C26 2.254(10) . ? Ru1 C7 2.279(10) . ? Ru1 P1 2.421(2) . ? Fe1 C37 2.071(9) . ? Fe1 C14 2.078(9) . ? Fe1 C12 2.079(9) . ? Fe1 C36 2.084(9) . ? Fe1 C38 2.090(8) . ? Fe1 C13 2.092(9) . ? Fe1 C40 2.099(9) . ? Fe1 C15 2.106(8) . ? Fe1 C39 2.110(8) . ? Fe1 P2 2.278(2) . ? Ru2 C49 2.173(8) . ? Ru2 C46 2.216(8) . ? Ru2 C47 2.234(8) . ? Ru2 C48 2.235(9) . ? Ru2 C50 2.236(9) . ? Ru2 P2 2.264(2) . ? Ru2 P1 2.273(2) . ? Ru2 Cl1 2.463(2) . ? P1 C7 1.753(9) . ? P1 C10 1.761(9) . ? P2 C15 1.771(10) . ? P2 C12 1.792(8) . ? O1 C11 1.240(10) . ? C1 C2 1.384(12) . ? C1 C6 1.426(12) . ? C1 H1 0.9500 . ? C2 C3 1.387(13) . ? C2 H2 0.9500 . ? C3 C4 1.390(13) . ? C3 H3 0.9500 . ? C4 C5 1.401(12) . ? C4 H4 0.9500 . ? C5 C6 1.379(12) . ? C5 H5 0.9500 . ? C6 C7 1.492(12) . ? C7 C8 1.441(11) . ? C8 C9 1.406(12) . ? C8 C25 1.520(12) . ? C9 C10 1.442(12) . ? C9 C24 1.525(11) . ? C10 C11 1.500(13) . ? C11 C12 1.456(12) . ? C12 C13 1.453(12) . ? C13 C14 1.435(12) . ? C13 C23 1.489(11) . ? C14 C15 1.447(11) . ? C14 C22 1.466(12) . ? C15 C16 1.493(11) . ? C16 C17 1.391(12) . ? C16 C21 1.420(13) . ? C17 C18 1.391(12) . ? C17 H17 0.9500 . ? C18 C19 1.349(13) . ? C18 H18 0.9500 . ? C19 C20 1.377(13) . ? C19 H19 0.9500 . ? C20 C21 1.391(12) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.391(13) . ? C26 C30 1.425(13) . ? C26 C31 1.515(12) . ? C27 C28 1.410(11) . ? C27 C32 1.511(12) . ? C28 C29 1.424(13) . ? C28 C33 1.521(12) . ? C29 C30 1.426(12) . ? C29 C34 1.496(12) . ? C30 C35 1.506(13) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.396(12) . ? C36 C40 1.442(12) . ? C36 C41 1.511(12) . ? C37 C38 1.439(11) . ? C37 C42 1.500(12) . ? C38 C39 1.422(12) . ? C38 C43 1.511(11) . ? C39 C40 1.458(12) . ? C39 C44 1.516(12) . ? C40 C45 1.480(12) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C50 1.396(12) . ? C46 C47 1.432(12) . ? C46 C51 1.494(11) . ? C47 C48 1.438(12) . ? C47 C52 1.482(12) . ? C48 C49 1.429(12) . ? C48 C53 1.503(13) . ? C49 C50 1.443(13) . ? C49 C54 1.551(12) . ? C50 C55 1.494(12) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? Cl2 C56 1.718(12) . ? Cl3 C56 1.715(13) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? Cl4 C57 1.734(13) . ? Cl5 C57 1.772(12) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? 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 C9 Ru1 C29 102.5(4) . . ? C9 Ru1 C30 127.0(4) . . ? C29 Ru1 C30 38.2(3) . . ? C9 Ru1 C10 38.9(3) . . ? C29 Ru1 C10 113.3(4) . . ? C30 Ru1 C10 111.8(3) . . ? C9 Ru1 C28 111.0(3) . . ? C29 Ru1 C28 38.1(3) . . ? C30 Ru1 C28 63.2(4) . . ? C10 Ru1 C28 142.2(3) . . ? C9 Ru1 C27 144.4(4) . . ? C29 Ru1 C27 63.2(3) . . ? C30 Ru1 C27 62.7(3) . . ? C10 Ru1 C27 174.5(4) . . ? C28 Ru1 C27 37.3(3) . . ? C9 Ru1 C8 37.6(3) . . ? C29 Ru1 C8 123.0(3) . . ? C30 Ru1 C8 159.9(3) . . ? C10 Ru1 C8 64.8(3) . . ? C28 Ru1 C8 106.4(3) . . ? C27 Ru1 C8 120.6(4) . . ? C9 Ru1 C26 163.9(3) . . ? C29 Ru1 C26 62.4(3) . . ? C30 Ru1 C26 37.4(3) . . ? C10 Ru1 C26 138.8(3) . . ? C28 Ru1 C26 61.4(3) . . ? C27 Ru1 C26 36.3(3) . . ? C8 Ru1 C26 154.9(3) . . ? C9 Ru1 C7 65.1(3) . . ? C29 Ru1 C7 159.1(3) . . ? C30 Ru1 C7 162.4(3) . . ? C10 Ru1 C7 68.5(3) . . ? C28 Ru1 C7 128.1(3) . . ? C27 Ru1 C7 116.4(3) . . ? C8 Ru1 C7 37.3(3) . . ? C26 Ru1 C7 131.0(3) . . ? C9 Ru1 P1 71.1(3) . . ? C29 Ru1 P1 151.3(3) . . ? C30 Ru1 P1 123.5(3) . . ? C10 Ru1 P1 44.5(2) . . ? C28 Ru1 P1 170.6(3) . . ? C27 Ru1 P1 137.0(2) . . ? C8 Ru1 P1 69.3(2) . . ? C26 Ru1 P1 118.9(2) . . ? C7 Ru1 P1 43.7(2) . . ? C37 Fe1 C14 172.5(3) . . ? C37 Fe1 C12 113.9(4) . . ? C14 Fe1 C12 70.7(4) . . ? C37 Fe1 C36 39.3(3) . . ? C14 Fe1 C36 139.0(4) . . ? C12 Fe1 C36 145.4(4) . . ? C37 Fe1 C38 40.5(3) . . ? C14 Fe1 C38 133.4(3) . . ? C12 Fe1 C38 108.2(3) . . ? C36 Fe1 C38 66.6(3) . . ? C37 Fe1 C13 139.9(3) . . ? C14 Fe1 C13 40.2(3) . . ? C12 Fe1 C13 40.8(3) . . ? C36 Fe1 C13 172.1(3) . . ? C38 Fe1 C13 108.2(3) . . ? C37 Fe1 C40 67.6(4) . . ? C14 Fe1 C40 106.9(4) . . ? C12 Fe1 C40 171.8(3) . . ? C36 Fe1 C40 40.3(3) . . ? C38 Fe1 C40 67.4(3) . . ? C13 Fe1 C40 132.8(4) . . ? C37 Fe1 C15 145.1(3) . . ? C14 Fe1 C15 40.5(3) . . ? C12 Fe1 C15 74.7(3) . . ? C36 Fe1 C15 115.0(3) . . ? C38 Fe1 C15 172.5(4) . . ? C13 Fe1 C15 69.3(3) . . ? C40 Fe1 C15 108.8(3) . . ? C37 Fe1 C39 67.5(4) . . ? C14 Fe1 C39 105.0(4) . . ? C12 Fe1 C39 131.8(3) . . ? C36 Fe1 C39 67.2(3) . . ? C38 Fe1 C39 39.6(3) . . ? C13 Fe1 C39 105.0(3) . . ? C40 Fe1 C39 40.5(3) . . ? C15 Fe1 C39 133.5(4) . . ? C37 Fe1 P2 111.5(2) . . ? C14 Fe1 P2 76.0(2) . . ? C12 Fe1 P2 48.3(2) . . ? C36 Fe1 P2 112.1(2) . . ? C38 Fe1 P2 139.6(3) . . ? C13 Fe1 P2 75.7(2) . . ? C40 Fe1 P2 139.4(2) . . ? C15 Fe1 P2 47.4(3) . . ? C39 Fe1 P2 179.0(3) . . ? C49 Ru2 C46 63.1(3) . . ? C49 Ru2 C47 63.1(3) . . ? C46 Ru2 C47 37.5(3) . . ? C49 Ru2 C48 37.8(3) . . ? C46 Ru2 C48 62.8(3) . . ? C47 Ru2 C48 37.5(3) . . ? C49 Ru2 C50 38.2(3) . . ? C46 Ru2 C50 36.5(3) . . ? C47 Ru2 C50 61.9(3) . . ? C48 Ru2 C50 62.6(3) . . ? C49 Ru2 P2 106.9(2) . . ? C46 Ru2 P2 117.6(2) . . ? C47 Ru2 P2 154.9(3) . . ? C48 Ru2 P2 143.4(3) . . ? C50 Ru2 P2 95.6(2) . . ? C49 Ru2 P1 105.9(2) . . ? C46 Ru2 P1 158.2(2) . . ? C47 Ru2 P1 121.3(3) . . ? C48 Ru2 P1 96.7(2) . . ? C50 Ru2 P1 142.0(3) . . ? P2 Ru2 P1 83.06(8) . . ? C49 Ru2 Cl1 153.2(2) . . ? C46 Ru2 Cl1 92.6(2) . . ? C47 Ru2 Cl1 90.9(2) . . ? C48 Ru2 Cl1 122.5(2) . . ? C50 Ru2 Cl1 124.9(3) . . ? P2 Ru2 Cl1 93.93(8) . . ? P1 Ru2 Cl1 92.95(9) . . ? C7 P1 C10 91.5(4) . . ? C7 P1 Ru2 133.8(3) . . ? C10 P1 Ru2 128.8(3) . . ? C7 P1 Ru1 63.8(3) . . ? C10 P1 Ru1 60.8(3) . . ? Ru2 P1 Ru1 150.33(11) . . ? C15 P2 C12 90.9(4) . . ? C15 P2 Ru2 136.0(3) . . ? C12 P2 Ru2 129.0(3) . . ? C15 P2 Fe1 61.2(3) . . ? C12 P2 Fe1 60.0(3) . . ? Ru2 P2 Fe1 149.70(12) . . ? C2 C1 C6 119.2(10) . . ? C2 C1 H1 120.4 . . ? C6 C1 H1 120.4 . . ? C1 C2 C3 121.2(9) . . ? C1 C2 H2 119.4 . . ? C3 C2 H2 119.4 . . ? C2 C3 C4 119.9(9) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C3 C4 C5 119.5(10) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C6 C5 C4 121.2(10) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C5 C6 C1 119.0(9) . . ? C5 C6 C7 123.5(9) . . ? C1 C6 C7 117.5(9) . . ? C8 C7 C6 122.8(8) . . ? C8 C7 P1 111.4(6) . . ? C6 C7 P1 125.8(6) . . ? C8 C7 Ru1 69.2(5) . . ? C6 C7 Ru1 125.3(7) . . ? P1 C7 Ru1 72.5(4) . . ? C9 C8 C7 113.0(8) . . ? C9 C8 C25 122.5(8) . . ? C7 C8 C25 124.3(8) . . ? C9 C8 Ru1 67.6(5) . . ? C7 C8 Ru1 73.5(6) . . ? C25 C8 Ru1 130.4(7) . . ? C8 C9 C10 112.3(8) . . ? C8 C9 C24 120.6(8) . . ? C10 C9 C24 126.0(8) . . ? C8 C9 Ru1 74.8(5) . . ? C10 C9 Ru1 72.9(5) . . ? C24 C9 Ru1 129.8(7) . . ? C9 C10 C11 123.7(7) . . ? C9 C10 P1 111.6(7) . . ? C11 C10 P1 124.6(6) . . ? C9 C10 Ru1 68.1(5) . . ? C11 C10 Ru1 122.4(6) . . ? P1 C10 Ru1 74.6(3) . . ? O1 C11 C12 119.1(9) . . ? O1 C11 C10 120.9(8) . . ? C12 C11 C10 120.0(8) . . ? C13 C12 C11 124.4(8) . . ? C13 C12 P2 111.3(7) . . ? C11 C12 P2 124.2(7) . . ? C13 C12 Fe1 70.1(5) . . ? C11 C12 Fe1 122.9(6) . . ? P2 C12 Fe1 71.6(3) . . ? C14 C13 C12 112.9(8) . . ? C14 C13 C23 122.9(8) . . ? C12 C13 C23 124.2(8) . . ? C14 C13 Fe1 69.4(5) . . ? C12 C13 Fe1 69.1(5) . . ? C23 C13 Fe1 130.7(6) . . ? C13 C14 C15 111.9(8) . . ? C13 C14 C22 123.6(8) . . ? C15 C14 C22 124.5(8) . . ? C13 C14 Fe1 70.4(5) . . ? C15 C14 Fe1 70.8(5) . . ? C22 C14 Fe1 127.1(6) . . ? C14 C15 C16 123.7(8) . . ? C14 C15 P2 112.8(6) . . ? C16 C15 P2 123.4(6) . . ? C14 C15 Fe1 68.7(5) . . ? C16 C15 Fe1 127.8(6) . . ? P2 C15 Fe1 71.4(3) . . ? C17 C16 C21 117.7(8) . . ? C17 C16 C15 122.2(9) . . ? C21 C16 C15 120.1(8) . . ? C16 C17 C18 121.2(9) . . ? C16 C17 H17 119.4 . . ? C18 C17 H17 119.4 . . ? C19 C18 C17 119.5(9) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C18 C19 C20 122.0(9) . . ? C18 C19 H19 119.0 . . ? C20 C19 H19 119.0 . . ? C19 C20 C21 119.3(9) . . ? C19 C20 H20 120.3 . . ? C21 C20 H20 120.3 . . ? C20 C21 C16 120.1(9) . . ? C20 C21 H21 119.9 . . ? C16 C21 H21 119.9 . . ? C14 C22 H22A 109.5 . . ? C14 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C14 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C13 C23 H23A 109.5 . . ? C13 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C13 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C9 C24 H24A 109.5 . . ? C9 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C9 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C8 C25 H25A 109.5 . . ? C8 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C8 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C30 108.7(9) . . ? C27 C26 C31 124.9(9) . . ? C30 C26 C31 125.7(9) . . ? C27 C26 Ru1 70.3(6) . . ? C30 C26 Ru1 68.7(6) . . ? C31 C26 Ru1 134.4(6) . . ? C26 C27 C28 108.4(8) . . ? C26 C27 C32 123.9(8) . . ? C28 C27 C32 126.5(9) . . ? C26 C27 Ru1 73.5(6) . . ? C28 C27 Ru1 70.6(5) . . ? C32 C27 Ru1 131.8(6) . . ? C27 C28 C29 108.2(9) . . ? C27 C28 C33 125.2(9) . . ? C29 C28 C33 126.5(8) . . ? C27 C28 Ru1 72.0(5) . . ? C29 C28 Ru1 70.1(5) . . ? C33 C28 Ru1 125.7(7) . . ? C28 C29 C30 107.2(8) . . ? C28 C29 C34 128.2(9) . . ? C30 C29 C34 124.2(9) . . ? C28 C29 Ru1 71.8(5) . . ? C30 C29 Ru1 71.4(5) . . ? C34 C29 Ru1 126.8(7) . . ? C26 C30 C29 107.3(9) . . ? C26 C30 C35 127.2(9) . . ? C29 C30 C35 125.2(9) . . ? C26 C30 Ru1 73.9(6) . . ? C29 C30 Ru1 70.4(5) . . ? C35 C30 Ru1 125.9(7) . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C27 C32 H32A 109.5 . . ? C27 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C27 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C28 C33 H33A 109.5 . . ? C28 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C28 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C29 C34 H34A 109.5 . . ? C29 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C29 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C30 C35 H35A 109.5 . . ? C30 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C30 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 C36 C40 109.7(8) . . ? C37 C36 C41 125.4(9) . . ? C40 C36 C41 124.2(8) . . ? C37 C36 Fe1 69.9(5) . . ? C40 C36 Fe1 70.4(5) . . ? C41 C36 Fe1 133.7(6) . . ? C36 C37 C38 107.8(8) . . ? C36 C37 C42 125.1(9) . . ? C38 C37 C42 126.7(8) . . ? C36 C37 Fe1 70.9(5) . . ? C38 C37 Fe1 70.5(5) . . ? C42 C37 Fe1 129.6(6) . . ? C39 C38 C37 108.6(8) . . ? C39 C38 C43 123.9(8) . . ? C37 C38 C43 127.3(9) . . ? C39 C38 Fe1 71.0(5) . . ? C37 C38 Fe1 69.1(5) . . ? C43 C38 Fe1 129.4(6) . . ? C38 C39 C40 107.6(8) . . ? C38 C39 C44 126.6(8) . . ? C40 C39 C44 125.6(9) . . ? C38 C39 Fe1 69.5(5) . . ? C40 C39 Fe1 69.3(5) . . ? C44 C39 Fe1 130.5(6) . . ? C36 C40 C39 106.3(8) . . ? C36 C40 C45 126.6(8) . . ? C39 C40 C45 127.0(9) . . ? C36 C40 Fe1 69.3(5) . . ? C39 C40 Fe1 70.1(5) . . ? C45 C40 Fe1 129.1(6) . . ? C36 C41 H41A 109.5 . . ? C36 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C36 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C37 C42 H42A 109.5 . . ? C37 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C37 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C38 C43 H43A 109.5 . . ? C38 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C38 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C39 C44 H44A 109.5 . . ? C39 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C39 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C40 C45 H45A 109.5 . . ? C40 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C40 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C50 C46 C47 108.8(8) . . ? C50 C46 C51 128.8(9) . . ? C47 C46 C51 122.3(8) . . ? C50 C46 Ru2 72.5(5) . . ? C47 C46 Ru2 71.9(5) . . ? C51 C46 Ru2 125.4(6) . . ? C46 C47 C48 107.8(8) . . ? C46 C47 C52 124.4(9) . . ? C48 C47 C52 127.5(9) . . ? C46 C47 Ru2 70.5(5) . . ? C48 C47 Ru2 71.3(5) . . ? C52 C47 Ru2 127.9(6) . . ? C49 C48 C47 107.2(8) . . ? C49 C48 C53 125.9(9) . . ? C47 C48 C53 126.9(9) . . ? C49 C48 Ru2 68.8(5) . . ? C47 C48 Ru2 71.2(5) . . ? C53 C48 Ru2 126.3(6) . . ? C48 C49 C50 107.9(8) . . ? C48 C49 C54 126.4(9) . . ? C50 C49 C54 124.8(9) . . ? C48 C49 Ru2 73.5(5) . . ? C50 C49 Ru2 73.3(5) . . ? C54 C49 Ru2 127.4(6) . . ? C46 C50 C49 108.1(8) . . ? C46 C50 C55 127.8(9) . . ? C49 C50 C55 124.0(9) . . ? C46 C50 Ru2 70.9(5) . . ? C49 C50 Ru2 68.6(5) . . ? C55 C50 Ru2 128.4(6) . . ? C46 C51 H51A 109.5 . . ? C46 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C46 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C47 C52 H52A 109.5 . . ? C47 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C47 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C48 C53 H53A 109.5 . . ? C48 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C48 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C49 C54 H54A 109.5 . . ? C49 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C49 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C50 C55 H55A 109.5 . . ? C50 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C50 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? Cl3 C56 Cl2 114.4(8) . . ? Cl3 C56 H56A 108.7 . . ? Cl2 C56 H56A 108.7 . . ? Cl3 C56 H56B 108.7 . . ? Cl2 C56 H56B 108.7 . . ? H56A C56 H56B 107.6 . . ? Cl4 C57 Cl5 110.9(8) . . ? Cl4 C57 H57A 109.5 . . ? Cl5 C57 H57A 109.5 . . ? Cl4 C57 H57B 109.5 . . ? Cl5 C57 H57B 109.5 . . ? H57A C57 H57B 108.1 . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.729 _refine_diff_density_min -0.654 _refine_diff_density_rms 0.112 #===END # compound 40 data_em194 _database_code_depnum_ccdc_archive 'CCDC 837333' #TrackingRef '2011_carmichael_dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H52 Cl2 Fe O P2 Pt Ru' _chemical_formula_sum 'C45 H52 Cl2 Fe O P2 Pt Ru' _chemical_formula_weight 1093.72 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' 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' 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' Pt Pt -1.7033 8.3905 '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 Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 9.980(1) _cell_length_b 15.620(1) _cell_length_c 26.652(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4154.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 2676 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 25.028 _exptl_crystal_description Needle _exptl_crystal_colour Red _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.749 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2168 _exptl_absorpt_coefficient_mu 4.302 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5460 _exptl_absorpt_correction_T_max 0.7823 _exptl_absorpt_process_details 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _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 12876 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.0808 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 25.02 _reflns_number_total 7135 _reflns_number_gt 5679 _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^)+(0.0358P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.017(7) _refine_ls_number_reflns 7135 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0616 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.0845 _refine_ls_wR_factor_gt 0.0769 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.975 _refine_ls_shift/su_max 0.005 _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 Pt1 Pt 0.50236(3) 0.167313(18) 0.338875(9) 0.02642(10) Uani 1 1 d . A . Ru1A Ru 0.4404(5) -0.0286(3) 0.44583(15) 0.0240(11) Uani 0.530(5) 1 d P A 1 Fe1A Fe 0.1510(11) 0.0950(7) 0.2687(4) 0.043(2) Uani 0.530(5) 1 d P A 1 Ru1B Ru 0.1490(7) 0.0961(3) 0.26788(18) 0.0193(12) Uani 0.470(5) 1 d P A 2 Fe1B Fe 0.4427(10) -0.0295(7) 0.4453(4) 0.043(2) Uani 0.470(5) 1 d P A 2 Cl1 Cl 0.5651(2) 0.23472(14) 0.26433(7) 0.0392(5) Uani 1 1 d . . . Cl2 Cl 0.6377(2) 0.26401(14) 0.38222(7) 0.0361(5) Uani 1 1 d . . . P1 P 0.3570(2) 0.08189(14) 0.30074(7) 0.0280(5) Uani 1 1 d . . . P2 P 0.4426(2) 0.10064(14) 0.40822(7) 0.0287(5) Uani 1 1 d . . . O1 O 0.0672(6) 0.0182(4) 0.39561(19) 0.0393(14) Uani 1 1 d . A . C1 C 0.1837(8) 0.0318(5) 0.3840(3) 0.0297(19) Uani 1 1 d . . . C2 C 0.2288(8) 0.0229(5) 0.3305(3) 0.0295(19) Uani 1 1 d . A . C3 C 0.1648(8) -0.0320(6) 0.2953(3) 0.031(2) Uani 1 1 d . . . C4 C 0.2246(8) -0.0286(5) 0.2462(3) 0.0284(19) Uani 1 1 d . A . C5 C 0.3315(9) 0.0303(5) 0.2426(3) 0.031(2) Uani 1 1 d . A . C6 C 0.0561(9) -0.0971(6) 0.3064(3) 0.043(2) Uani 1 1 d . A . H6A H 0.0330 -0.0949 0.3421 0.064 Uiso 1 1 calc R . . H6B H 0.0884 -0.1545 0.2979 0.064 Uiso 1 1 calc R . . H6C H -0.0236 -0.0839 0.2863 0.064 Uiso 1 1 calc R . . C7 C 0.1790(9) -0.0837(6) 0.2037(3) 0.041(2) Uani 1 1 d . . . H7A H 0.1996 -0.0554 0.1718 0.062 Uiso 1 1 calc R A . H7B H 0.0821 -0.0930 0.2062 0.062 Uiso 1 1 calc R . . H7C H 0.2254 -0.1390 0.2052 0.062 Uiso 1 1 calc R . . C8 C 0.4190(8) 0.0386(5) 0.1967(3) 0.030(2) Uani 1 1 d . . . C9 C 0.4798(10) -0.0337(6) 0.1782(3) 0.052(3) Uani 1 1 d . A . H9 H 0.4698 -0.0859 0.1961 0.062 Uiso 1 1 calc R . . C10 C 0.5553(11) -0.0337(8) 0.1344(4) 0.066(3) Uani 1 1 d . . . H10 H 0.5981 -0.0841 0.1225 0.080 Uiso 1 1 calc R A . C11 C 0.5653(11) 0.0436(8) 0.1088(4) 0.067(3) Uani 1 1 d . A . H11 H 0.6139 0.0458 0.0782 0.081 Uiso 1 1 calc R . . C12 C 0.5056(14) 0.1181(7) 0.1272(3) 0.058(3) Uani 1 1 d . . . H12 H 0.5142 0.1706 0.1094 0.070 Uiso 1 1 calc R A . C13 C 0.4350(9) 0.1147(6) 0.1706(3) 0.038(2) Uani 1 1 d . A . H13 H 0.3956 0.1655 0.1835 0.046 Uiso 1 1 calc R . . C14 C 0.1093(10) 0.2299(6) 0.2587(3) 0.043(2) Uani 1 1 d . . . C15 C 0.0783(9) 0.1849(6) 0.2138(3) 0.040(2) Uani 1 1 d . A . C16 C -0.0234(10) 0.1243(6) 0.2241(3) 0.044(3) Uani 1 1 d . . . C17 C -0.0544(9) 0.1304(6) 0.2763(4) 0.045(2) Uani 1 1 d . A . C18 C 0.0266(10) 0.1938(5) 0.2979(3) 0.041(2) Uani 1 1 d . A . C19 C 0.0204(13) 0.2262(7) 0.3506(3) 0.065(3) Uani 1 1 d . . . H19A H -0.0559 0.2652 0.3542 0.098 Uiso 1 1 calc R A . H19B H 0.1034 0.2568 0.3586 0.098 Uiso 1 1 calc R . . H19C H 0.0095 0.1778 0.3737 0.098 Uiso 1 1 calc R . . C20 C -0.1627(11) 0.0793(8) 0.3031(5) 0.085(4) Uani 1 1 d . . . H20A H -0.1266 0.0560 0.3344 0.127 Uiso 1 1 calc R A . H20B H -0.1924 0.0322 0.2815 0.127 Uiso 1 1 calc R . . H20C H -0.2389 0.1168 0.3106 0.127 Uiso 1 1 calc R . . C21 C -0.0952(12) 0.0691(7) 0.1862(4) 0.071(4) Uani 1 1 d . A . H21A H -0.1690 0.1017 0.1712 0.107 Uiso 1 1 calc R . . H21B H -0.1310 0.0181 0.2029 0.107 Uiso 1 1 calc R . . H21C H -0.0323 0.0518 0.1599 0.107 Uiso 1 1 calc R . . C22 C 0.1286(11) 0.2046(7) 0.1616(3) 0.069(3) Uani 1 1 d . . . H22A H 0.0605 0.2373 0.1434 0.103 Uiso 1 1 calc R A . H22B H 0.1467 0.1509 0.1438 0.103 Uiso 1 1 calc R . . H22C H 0.2112 0.2383 0.1639 0.103 Uiso 1 1 calc R . . C23 C 0.2106(10) 0.2990(6) 0.2661(5) 0.064(3) Uani 1 1 d . A . H23A H 0.2742 0.2987 0.2381 0.095 Uiso 1 1 calc R . . H23B H 0.2589 0.2891 0.2976 0.095 Uiso 1 1 calc R . . H23C H 0.1653 0.3546 0.2676 0.095 Uiso 1 1 calc R . . C24 C 0.2856(9) 0.0552(5) 0.4218(3) 0.030(2) Uani 1 1 d . A . C25 C 0.2725(8) 0.0414(5) 0.4756(3) 0.030(2) Uani 1 1 d . . . C26 C 0.3890(9) 0.0654(6) 0.5022(3) 0.033(2) Uani 1 1 d . A . C27 C 0.4940(10) 0.1007(4) 0.4718(2) 0.0278(17) Uani 1 1 d . A . C28 C 0.1492(9) 0.0045(6) 0.5008(3) 0.047(3) Uani 1 1 d . A . H28A H 0.1767 -0.0337 0.5281 0.071 Uiso 1 1 calc R . . H28B H 0.0968 -0.0279 0.4761 0.071 Uiso 1 1 calc R . . H28C H 0.0945 0.0511 0.5144 0.071 Uiso 1 1 calc R . . C29 C 0.3990(9) 0.0572(5) 0.5586(3) 0.039(2) Uani 1 1 d . . . H29A H 0.3503 0.1044 0.5745 0.058 Uiso 1 1 calc R A . H29B H 0.4933 0.0591 0.5687 0.058 Uiso 1 1 calc R . . H29C H 0.3597 0.0025 0.5691 0.058 Uiso 1 1 calc R . . C30 C 0.6256(9) 0.1302(5) 0.4890(3) 0.032(2) Uani 1 1 d . . . C31 C 0.6389(9) 0.1797(5) 0.5331(3) 0.034(2) Uani 1 1 d . A . H31 H 0.5616 0.1947 0.5519 0.041 Uiso 1 1 calc R . . C32 C 0.7637(9) 0.2062(6) 0.5488(3) 0.042(2) Uani 1 1 d . . . H32 H 0.7713 0.2379 0.5791 0.051 Uiso 1 1 calc R A . C33 C 0.8780(9) 0.1880(6) 0.5217(3) 0.042(2) Uani 1 1 d . A . H33 H 0.9634 0.2064 0.5331 0.050 Uiso 1 1 calc R . . C34 C 0.8654(9) 0.1418(5) 0.4770(3) 0.035(2) Uani 1 1 d . . . H34 H 0.9425 0.1290 0.4575 0.042 Uiso 1 1 calc R A . C35 C 0.7404(9) 0.1150(5) 0.4614(3) 0.034(2) Uani 1 1 d . A . H35 H 0.7330 0.0849 0.4306 0.041 Uiso 1 1 calc R . . C36 C 0.3912(10) -0.1569(6) 0.4259(4) 0.045(2) Uani 1 1 d . . . C37 C 0.4333(12) -0.1545(7) 0.4775(3) 0.049(3) Uani 1 1 d . A . C38 C 0.5673(12) -0.1237(6) 0.4793(3) 0.042(3) Uani 1 1 d . . . C39 C 0.6096(10) -0.1110(6) 0.4292(3) 0.043(3) Uani 1 1 d . A . C40 C 0.5008(13) -0.1290(5) 0.3968(3) 0.041(2) Uani 1 1 d . A . C41 C 0.5034(15) -0.1272(6) 0.3402(3) 0.074(4) Uani 1 1 d . . . H41A H 0.5717 -0.0865 0.3288 0.112 Uiso 1 1 calc R A . H41B H 0.4154 -0.1095 0.3276 0.112 Uiso 1 1 calc R . . H41C H 0.5248 -0.1845 0.3275 0.112 Uiso 1 1 calc R . . C42 C 0.7510(11) -0.0871(7) 0.4138(5) 0.071(3) Uani 1 1 d . . . H42A H 0.7960 -0.0584 0.4418 0.107 Uiso 1 1 calc R A . H42B H 0.7477 -0.0485 0.3848 0.107 Uiso 1 1 calc R . . H42C H 0.8007 -0.1390 0.4048 0.107 Uiso 1 1 calc R . . C43 C 0.6512(13) -0.1100(8) 0.5252(4) 0.083(4) Uani 1 1 d . A . H43A H 0.7198 -0.1548 0.5273 0.124 Uiso 1 1 calc R . . H43B H 0.5942 -0.1124 0.5551 0.124 Uiso 1 1 calc R . . H43C H 0.6946 -0.0538 0.5233 0.124 Uiso 1 1 calc R . . C44 C 0.3485(17) -0.1845(7) 0.5217(4) 0.096(5) Uani 1 1 d . . . H44A H 0.2533 -0.1795 0.5132 0.144 Uiso 1 1 calc R A . H44B H 0.3680 -0.1489 0.5511 0.144 Uiso 1 1 calc R . . H44C H 0.3697 -0.2443 0.5293 0.144 Uiso 1 1 calc R . . C45 C 0.2601(11) -0.1878(7) 0.4055(5) 0.073(4) Uani 1 1 d . A . H45A H 0.2378 -0.1556 0.3750 0.109 Uiso 1 1 calc R . . H45B H 0.1898 -0.1792 0.4306 0.109 Uiso 1 1 calc R . . H45C H 0.2668 -0.2489 0.3974 0.109 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 Pt1 0.02583(15) 0.03166(18) 0.02176(14) 0.00024(13) 0.00011(19) -0.00268(19) Ru1A 0.044(2) 0.0158(15) 0.0118(13) 0.0013(12) -0.0018(14) -0.0022(14) Fe1A 0.015(3) 0.069(5) 0.045(4) -0.002(3) -0.001(3) 0.004(3) Ru1B 0.030(2) 0.0174(18) 0.0103(16) -0.0012(14) -0.0021(17) 0.0022(17) Fe1B 0.015(3) 0.069(5) 0.045(4) -0.002(3) -0.001(3) 0.004(3) Cl1 0.0448(11) 0.0473(14) 0.0254(9) 0.0057(10) 0.0004(10) -0.0099(11) Cl2 0.0380(11) 0.0394(13) 0.0309(10) 0.0010(10) -0.0036(10) -0.0096(10) P1 0.0289(11) 0.0358(14) 0.0194(10) 0.0021(10) 0.0011(10) -0.0024(11) P2 0.0279(10) 0.0373(14) 0.0207(9) -0.0020(9) -0.0004(9) -0.0063(10) O1 0.025(3) 0.059(4) 0.033(3) 0.003(3) 0.004(3) -0.007(3) C1 0.023(4) 0.035(5) 0.031(4) -0.002(4) 0.003(4) -0.001(4) C2 0.023(4) 0.039(5) 0.026(4) 0.000(4) 0.000(4) -0.008(4) C3 0.029(4) 0.045(6) 0.020(4) 0.004(4) 0.001(4) 0.001(4) C4 0.029(4) 0.017(5) 0.039(5) 0.000(4) 0.003(4) -0.006(4) C5 0.042(5) 0.029(5) 0.023(4) 0.000(4) -0.003(4) 0.009(4) C6 0.044(5) 0.050(6) 0.034(4) 0.006(4) 0.014(4) -0.010(5) C7 0.040(5) 0.055(7) 0.029(4) -0.001(4) -0.004(4) -0.001(5) C8 0.030(5) 0.034(5) 0.027(4) -0.002(4) 0.009(4) -0.011(4) C9 0.046(6) 0.048(6) 0.062(5) -0.041(5) -0.004(5) 0.006(5) C10 0.061(7) 0.076(8) 0.062(6) -0.035(6) 0.043(6) -0.020(6) C11 0.062(7) 0.087(9) 0.053(6) -0.018(6) 0.027(6) -0.031(7) C12 0.074(7) 0.064(7) 0.038(5) 0.014(5) -0.002(7) -0.017(8) C13 0.041(5) 0.039(6) 0.035(5) -0.003(4) -0.003(4) -0.005(4) C14 0.051(6) 0.033(6) 0.044(5) 0.001(4) -0.007(5) 0.010(5) C15 0.039(5) 0.052(7) 0.028(4) 0.003(4) -0.004(4) 0.006(5) C16 0.043(7) 0.048(6) 0.041(5) -0.011(4) -0.016(5) 0.010(5) C17 0.029(5) 0.047(6) 0.057(6) 0.012(5) 0.002(5) 0.005(5) C18 0.049(7) 0.036(5) 0.036(4) -0.006(4) -0.010(5) 0.017(4) C19 0.089(9) 0.072(7) 0.034(4) -0.009(4) -0.011(6) 0.039(7) C20 0.031(6) 0.070(9) 0.153(13) 0.018(9) 0.015(8) 0.013(6) C21 0.062(7) 0.064(8) 0.088(8) -0.019(6) -0.036(7) 0.015(6) C22 0.064(7) 0.107(9) 0.035(5) 0.021(6) 0.020(6) 0.036(6) C23 0.047(6) 0.042(7) 0.102(8) 0.001(6) -0.028(7) 0.005(5) C24 0.037(5) 0.031(5) 0.023(4) -0.001(4) -0.006(4) -0.007(4) C25 0.030(5) 0.037(6) 0.025(4) -0.001(4) 0.008(4) 0.001(4) C26 0.040(5) 0.039(6) 0.020(4) -0.004(4) 0.001(4) -0.002(4) C27 0.034(4) 0.029(4) 0.020(3) -0.007(3) -0.007(5) 0.004(5) C28 0.038(5) 0.074(8) 0.030(4) 0.015(5) 0.012(4) -0.011(5) C29 0.050(6) 0.049(6) 0.018(4) -0.006(4) 0.001(4) -0.006(4) C30 0.041(5) 0.035(5) 0.019(4) -0.007(4) -0.001(4) -0.002(4) C31 0.032(5) 0.043(6) 0.029(4) 0.000(4) -0.003(4) 0.001(4) C32 0.043(6) 0.050(6) 0.035(5) -0.012(4) -0.019(5) 0.005(5) C33 0.036(5) 0.058(7) 0.031(5) -0.001(4) -0.008(4) -0.008(5) C34 0.031(5) 0.035(6) 0.040(5) -0.002(4) -0.002(4) 0.006(4) C35 0.042(5) 0.032(6) 0.029(4) 0.000(4) -0.007(4) 0.001(4) C36 0.058(6) 0.026(6) 0.052(6) -0.004(5) -0.002(5) -0.002(5) C37 0.074(7) 0.037(6) 0.037(5) 0.013(5) 0.002(5) 0.005(6) C38 0.056(6) 0.040(6) 0.030(5) -0.004(4) -0.017(5) 0.002(5) C39 0.052(6) 0.032(6) 0.046(6) -0.004(5) -0.006(5) 0.014(5) C40 0.057(5) 0.033(5) 0.033(4) -0.001(3) -0.013(6) 0.022(6) C41 0.137(11) 0.041(5) 0.045(5) -0.016(4) -0.025(10) 0.053(8) C42 0.049(6) 0.048(7) 0.118(10) -0.018(7) 0.014(7) 0.010(6) C43 0.087(9) 0.081(9) 0.080(8) -0.008(7) -0.053(8) 0.034(8) C44 0.167(15) 0.052(8) 0.070(7) 0.028(6) 0.028(10) -0.025(9) C45 0.063(7) 0.048(8) 0.107(9) -0.012(7) -0.042(7) 0.001(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P2 2.2036(19) . ? Pt1 P1 2.217(2) . ? Pt1 Cl2 2.332(2) . ? Pt1 Cl1 2.3341(19) . ? Ru1A C24 2.123(10) . ? Ru1A C40 2.129(9) . ? Ru1A C36 2.132(10) . ? Ru1A C37 2.141(11) . ? Ru1A C38 2.147(11) . ? Ru1A C25 2.153(9) . ? Ru1A C26 2.163(9) . ? Ru1A C39 2.170(11) . ? Ru1A C27 2.201(8) . ? Ru1A P2 2.253(4) . ? Fe1A C3 2.111(14) . ? Fe1A C18 2.127(13) . ? Fe1A C17 2.133(14) . ? Fe1A C2 2.141(13) . ? Fe1A C4 2.152(13) . ? Fe1A C15 2.153(13) . ? Fe1A C16 2.156(14) . ? Fe1A C14 2.164(14) . ? Fe1A C5 2.181(14) . ? Fe1A P1 2.236(11) . ? Ru1B C17 2.112(11) . ? Ru1B C18 2.112(10) . ? Ru1B C15 2.120(10) . ? Ru1B C16 2.124(11) . ? Ru1B C3 2.136(10) . ? Ru1B C14 2.141(10) . ? Ru1B C4 2.168(10) . ? Ru1B C2 2.174(9) . ? Ru1B C5 2.198(10) . ? Ru1B P1 2.264(7) . ? Fe1B C40 2.102(13) . ? Fe1B C36 2.119(14) . ? Fe1B C38 2.130(14) . ? Fe1B C37 2.134(14) . ? Fe1B C39 2.140(14) . ? Fe1B C24 2.145(13) . ? Fe1B C25 2.184(13) . ? Fe1B C26 2.189(13) . ? Fe1B C27 2.214(13) . ? Fe1B P2 2.260(11) . ? P1 C2 1.765(8) . ? P1 C5 1.766(8) . ? P2 C24 1.757(9) . ? P2 C27 1.772(7) . ? O1 C1 1.221(9) . ? C1 C24 1.479(11) . ? C1 C2 1.502(11) . ? C2 C3 1.422(11) . ? C3 C4 1.438(10) . ? C3 C6 1.516(11) . ? C4 C5 1.412(11) . ? C4 C7 1.494(11) . ? C5 C8 1.509(11) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.373(11) . ? C8 C13 1.385(11) . ? C9 C10 1.389(13) . ? C9 H9 0.9500 . ? C10 C11 1.392(15) . ? C10 H10 0.9500 . ? C11 C12 1.396(14) . ? C11 H11 0.9500 . ? C12 C13 1.358(13) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.421(12) . ? C14 C18 1.446(12) . ? C14 C23 1.492(13) . ? C15 C16 1.414(13) . ? C15 C22 1.511(11) . ? C16 C17 1.427(12) . ? C16 C21 1.510(13) . ? C17 C18 1.402(13) . ? C17 C20 1.521(14) . ? C18 C19 1.495(11) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.456(10) . ? C25 C26 1.413(11) . ? C25 C28 1.515(11) . ? C26 C27 1.435(12) . ? C26 C29 1.511(10) . ? C27 C30 1.465(13) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C35 1.382(12) . ? C30 C31 1.411(11) . ? C31 C32 1.378(12) . ? C31 H31 0.9500 . ? C32 C33 1.380(13) . ? C32 H32 0.9500 . ? C33 C34 1.397(12) . ? C33 H33 0.9500 . ? C34 C35 1.380(12) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C40 1.410(14) . ? C36 C37 1.438(13) . ? C36 C45 1.497(13) . ? C37 C38 1.422(14) . ? C37 C44 1.526(15) . ? C38 C39 1.416(13) . ? C38 C43 1.498(13) . ? C39 C40 1.415(13) . ? C39 C42 1.516(14) . ? C40 C41 1.508(10) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? 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 P2 Pt1 P1 85.58(7) . . ? P2 Pt1 Cl2 92.71(7) . . ? P1 Pt1 Cl2 174.53(8) . . ? P2 Pt1 Cl1 178.57(8) . . ? P1 Pt1 Cl1 93.26(7) . . ? Cl2 Pt1 Cl1 88.52(7) . . ? C24 Ru1A C40 118.4(4) . . ? C24 Ru1A C36 109.7(4) . . ? C40 Ru1A C36 38.7(4) . . ? C24 Ru1A C37 131.3(5) . . ? C40 Ru1A C37 64.8(4) . . ? C36 Ru1A C37 39.3(4) . . ? C24 Ru1A C38 168.8(5) . . ? C40 Ru1A C38 65.1(4) . . ? C36 Ru1A C38 65.7(4) . . ? C37 Ru1A C38 38.7(4) . . ? C24 Ru1A C25 39.8(3) . . ? C40 Ru1A C25 145.2(5) . . ? C36 Ru1A C25 113.0(4) . . ? C37 Ru1A C25 107.2(4) . . ? C38 Ru1A C25 131.1(4) . . ? C24 Ru1A C26 67.6(3) . . ? C40 Ru1A C26 173.7(4) . . ? C36 Ru1A C26 139.2(4) . . ? C37 Ru1A C26 110.0(4) . . ? C38 Ru1A C26 108.7(4) . . ? C25 Ru1A C26 38.2(3) . . ? C24 Ru1A C39 150.5(4) . . ? C40 Ru1A C39 38.4(4) . . ? C36 Ru1A C39 64.5(4) . . ? C37 Ru1A C39 64.0(4) . . ? C38 Ru1A C39 38.3(4) . . ? C25 Ru1A C39 169.4(4) . . ? C26 Ru1A C39 136.9(4) . . ? C24 Ru1A C27 72.9(3) . . ? C40 Ru1A C27 143.2(5) . . ? C36 Ru1A C27 176.0(4) . . ? C37 Ru1A C27 136.6(4) . . ? C38 Ru1A C27 111.2(4) . . ? C25 Ru1A C27 66.9(4) . . ? C26 Ru1A C27 38.4(3) . . ? C39 Ru1A C27 114.8(4) . . ? C24 Ru1A P2 47.2(2) . . ? C40 Ru1A P2 112.6(3) . . ? C36 Ru1A P2 137.2(3) . . ? C37 Ru1A P2 176.5(4) . . ? C38 Ru1A P2 143.1(4) . . ? C25 Ru1A P2 73.5(3) . . ? C26 Ru1A P2 72.7(3) . . ? C39 Ru1A P2 115.7(3) . . ? C27 Ru1A P2 46.86(19) . . ? C3 Fe1A C18 126.7(6) . . ? C3 Fe1A C17 105.9(6) . . ? C18 Fe1A C17 38.4(4) . . ? C3 Fe1A C2 39.1(3) . . ? C18 Fe1A C2 108.2(6) . . ? C17 Fe1A C2 114.4(6) . . ? C3 Fe1A C4 39.4(3) . . ? C18 Fe1A C4 162.2(7) . . ? C17 Fe1A C4 126.0(6) . . ? C2 Fe1A C4 67.5(4) . . ? C3 Fe1A C15 149.6(6) . . ? C18 Fe1A C15 65.1(4) . . ? C17 Fe1A C15 64.6(5) . . ? C2 Fe1A C15 171.1(7) . . ? C4 Fe1A C15 120.7(6) . . ? C3 Fe1A C16 115.9(6) . . ? C18 Fe1A C16 64.9(4) . . ? C17 Fe1A C16 38.9(4) . . ? C2 Fe1A C16 145.9(6) . . ? C4 Fe1A C16 108.2(6) . . ? C15 Fe1A C16 38.3(4) . . ? C3 Fe1A C14 165.7(7) . . ? C18 Fe1A C14 39.4(4) . . ? C17 Fe1A C14 64.8(5) . . ? C2 Fe1A C14 132.6(6) . . ? C4 Fe1A C14 154.8(6) . . ? C15 Fe1A C14 38.4(4) . . ? C16 Fe1A C14 64.5(4) . . ? C3 Fe1A C5 67.5(4) . . ? C18 Fe1A C5 159.3(7) . . ? C17 Fe1A C5 160.9(7) . . ? C2 Fe1A C5 72.6(4) . . ? C4 Fe1A C5 38.0(3) . . ? C15 Fe1A C5 111.3(6) . . ? C16 Fe1A C5 126.1(6) . . ? C14 Fe1A C5 124.8(6) . . ? C3 Fe1A P1 74.1(4) . . ? C18 Fe1A P1 117.6(5) . . ? C17 Fe1A P1 150.7(6) . . ? C2 Fe1A P1 47.5(3) . . ? C4 Fe1A P1 73.1(4) . . ? C15 Fe1A P1 129.0(6) . . ? C16 Fe1A P1 166.4(6) . . ? C14 Fe1A P1 108.3(5) . . ? C5 Fe1A P1 47.1(3) . . ? C17 Ru1B C18 38.8(4) . . ? C17 Ru1B C15 65.6(4) . . ? C18 Ru1B C15 65.9(4) . . ? C17 Ru1B C16 39.4(4) . . ? C18 Ru1B C16 65.8(4) . . ? C15 Ru1B C16 38.9(4) . . ? C17 Ru1B C3 105.8(4) . . ? C18 Ru1B C3 126.1(4) . . ? C15 Ru1B C3 150.4(4) . . ? C16 Ru1B C3 116.2(4) . . ? C17 Ru1B C14 65.6(4) . . ? C18 Ru1B C14 39.7(3) . . ? C15 Ru1B C14 39.0(3) . . ? C16 Ru1B C14 65.5(4) . . ? C3 Ru1B C14 165.3(4) . . ? C17 Ru1B C4 126.2(4) . . ? C18 Ru1B C4 162.1(5) . . ? C15 Ru1B C4 121.5(4) . . ? C16 Ru1B C4 108.8(4) . . ? C3 Ru1B C4 39.0(3) . . ? C14 Ru1B C4 155.7(4) . . ? C17 Ru1B C2 113.8(4) . . ? C18 Ru1B C2 107.6(4) . . ? C15 Ru1B C2 170.9(4) . . ? C16 Ru1B C2 145.8(4) . . ? C3 Ru1B C2 38.5(3) . . ? C14 Ru1B C2 132.0(4) . . ? C4 Ru1B C2 66.6(3) . . ? C17 Ru1B C5 161.5(4) . . ? C18 Ru1B C5 159.0(5) . . ? C15 Ru1B C5 111.9(4) . . ? C16 Ru1B C5 126.9(4) . . ? C3 Ru1B C5 66.8(3) . . ? C14 Ru1B C5 125.1(4) . . ? C4 Ru1B C5 37.7(3) . . ? C2 Ru1B C5 71.7(3) . . ? C17 Ru1B P1 149.9(4) . . ? C18 Ru1B P1 117.1(3) . . ? C15 Ru1B P1 129.2(4) . . ? C16 Ru1B P1 167.2(4) . . ? C3 Ru1B P1 73.0(3) . . ? C14 Ru1B P1 108.1(4) . . ? C4 Ru1B P1 72.3(3) . . ? C2 Ru1B P1 46.8(2) . . ? C5 Ru1B P1 46.6(2) . . ? C40 Fe1B C36 39.0(4) . . ? C40 Fe1B C38 65.8(5) . . ? C36 Fe1B C38 66.2(5) . . ? C40 Fe1B C37 65.4(5) . . ? C36 Fe1B C37 39.5(4) . . ? C38 Fe1B C37 39.0(4) . . ? C40 Fe1B C39 39.0(4) . . ? C36 Fe1B C39 65.2(5) . . ? C38 Fe1B C39 38.7(4) . . ? C37 Fe1B C39 64.6(5) . . ? C40 Fe1B C24 118.6(6) . . ? C36 Fe1B C24 109.4(6) . . ? C38 Fe1B C24 167.8(7) . . ? C37 Fe1B C24 130.5(6) . . ? C39 Fe1B C24 151.4(6) . . ? C40 Fe1B C25 144.8(7) . . ? C36 Fe1B C25 112.2(6) . . ? C38 Fe1B C25 130.3(6) . . ? C37 Fe1B C25 106.3(6) . . ? C39 Fe1B C25 169.0(6) . . ? C24 Fe1B C25 39.3(3) . . ? C40 Fe1B C26 174.0(6) . . ? C36 Fe1B C26 138.3(6) . . ? C38 Fe1B C26 108.4(6) . . ? C37 Fe1B C26 109.3(6) . . ? C39 Fe1B C26 137.1(6) . . ? C24 Fe1B C26 66.7(4) . . ? C25 Fe1B C26 37.7(3) . . ? C40 Fe1B C27 144.2(6) . . ? C36 Fe1B C27 175.5(6) . . ? C38 Fe1B C27 111.3(6) . . ? C37 Fe1B C27 136.2(6) . . ? C39 Fe1B C27 115.5(6) . . ? C24 Fe1B C27 72.3(5) . . ? C25 Fe1B C27 66.1(5) . . ? C26 Fe1B C27 38.0(4) . . ? C40 Fe1B P2 113.3(5) . . ? C36 Fe1B P2 137.6(6) . . ? C38 Fe1B P2 143.9(6) . . ? C37 Fe1B P2 176.7(6) . . ? C39 Fe1B P2 116.6(5) . . ? C24 Fe1B P2 46.9(3) . . ? C25 Fe1B P2 72.8(4) . . ? C26 Fe1B P2 72.1(4) . . ? C27 Fe1B P2 46.6(3) . . ? C2 P1 C5 92.9(4) . . ? C2 P1 Pt1 125.6(3) . . ? C5 P1 Pt1 140.5(3) . . ? C2 P1 Fe1A 63.4(4) . . ? C5 P1 Fe1A 64.8(4) . . ? Pt1 P1 Fe1A 136.2(3) . . ? C2 P1 Ru1B 63.9(3) . . ? C5 P1 Ru1B 64.7(3) . . ? Pt1 P1 Ru1B 135.88(17) . . ? Fe1A P1 Ru1B 0.5(4) . . ? C24 P2 C27 93.5(4) . . ? C24 P2 Pt1 127.2(3) . . ? C27 P2 Pt1 136.4(3) . . ? C24 P2 Ru1A 62.5(3) . . ? C27 P2 Ru1A 65.0(3) . . ? Pt1 P2 Ru1A 143.03(15) . . ? C24 P2 Fe1B 63.1(4) . . ? C27 P2 Fe1B 65.3(4) . . ? Pt1 P2 Fe1B 142.3(3) . . ? Ru1A P2 Fe1B 0.8(4) . . ? O1 C1 C24 121.7(7) . . ? O1 C1 C2 120.7(7) . . ? C24 C1 C2 117.6(7) . . ? C3 C2 C1 123.2(7) . . ? C3 C2 P1 110.2(5) . . ? C1 C2 P1 126.5(6) . . ? C3 C2 Fe1A 69.3(5) . . ? C1 C2 Fe1A 124.9(6) . . ? P1 C2 Fe1A 69.1(4) . . ? C3 C2 Ru1B 69.3(5) . . ? C1 C2 Ru1B 124.7(6) . . ? P1 C2 Ru1B 69.3(3) . . ? Fe1A C2 Ru1B 0.2(5) . . ? C2 C3 C4 113.0(7) . . ? C2 C3 C6 126.7(7) . . ? C4 C3 C6 119.9(7) . . ? C2 C3 Fe1A 71.6(6) . . ? C4 C3 Fe1A 71.8(6) . . ? C6 C3 Fe1A 130.5(7) . . ? C2 C3 Ru1B 72.2(5) . . ? C4 C3 Ru1B 71.7(5) . . ? C6 C3 Ru1B 130.0(6) . . ? Fe1A C3 Ru1B 0.6(5) . . ? C5 C4 C3 113.6(7) . . ? C5 C4 C7 123.6(7) . . ? C3 C4 C7 122.8(7) . . ? C5 C4 Fe1A 72.1(5) . . ? C3 C4 Fe1A 68.8(6) . . ? C7 C4 Fe1A 128.6(7) . . ? C5 C4 Ru1B 72.3(5) . . ? C3 C4 Ru1B 69.3(5) . . ? C7 C4 Ru1B 127.9(6) . . ? Fe1A C4 Ru1B 0.8(4) . . ? C4 C5 C8 123.3(7) . . ? C4 C5 P1 110.2(6) . . ? C8 C5 P1 126.1(6) . . ? C4 C5 Fe1A 69.9(5) . . ? C8 C5 Fe1A 134.2(6) . . ? P1 C5 Fe1A 68.1(4) . . ? C4 C5 Ru1B 70.0(5) . . ? C8 C5 Ru1B 133.5(6) . . ? P1 C5 Ru1B 68.7(3) . . ? Fe1A C5 Ru1B 0.8(4) . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C13 118.4(8) . . ? C9 C8 C5 118.4(8) . . ? C13 C8 C5 123.2(8) . . ? C8 C9 C10 122.8(10) . . ? C8 C9 H9 118.6 . . ? C10 C9 H9 118.6 . . ? C9 C10 C11 116.8(10) . . ? C9 C10 H10 121.6 . . ? C11 C10 H10 121.6 . . ? C10 C11 C12 121.4(9) . . ? C10 C11 H11 119.3 . . ? C12 C11 H11 119.3 . . ? C13 C12 C11 119.2(9) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C12 C13 C8 121.4(9) . . ? C12 C13 H13 119.3 . . ? C8 C13 H13 119.3 . . ? C15 C14 C18 106.9(8) . . ? C15 C14 C23 128.1(9) . . ? C18 C14 C23 125.0(9) . . ? C15 C14 Ru1B 69.7(5) . . ? C18 C14 Ru1B 69.1(5) . . ? C23 C14 Ru1B 124.4(7) . . ? C15 C14 Fe1A 70.4(6) . . ? C18 C14 Fe1A 68.9(5) . . ? C23 C14 Fe1A 123.9(7) . . ? Ru1B C14 Fe1A 0.7(4) . . ? C16 C15 C14 108.9(7) . . ? C16 C15 C22 123.6(9) . . ? C14 C15 C22 127.0(9) . . ? C16 C15 Ru1B 70.7(5) . . ? C14 C15 Ru1B 71.3(5) . . ? C22 C15 Ru1B 130.4(7) . . ? C16 C15 Fe1A 71.0(6) . . ? C14 C15 Fe1A 71.2(6) . . ? C22 C15 Fe1A 130.3(7) . . ? Ru1B C15 Fe1A 0.2(5) . . ? C15 C16 C17 107.5(8) . . ? C15 C16 C21 126.3(8) . . ? C17 C16 C21 126.0(9) . . ? C15 C16 Ru1B 70.4(5) . . ? C17 C16 Ru1B 69.8(5) . . ? C21 C16 Ru1B 129.3(6) . . ? C15 C16 Fe1A 70.7(6) . . ? C17 C16 Fe1A 69.7(6) . . ? C21 C16 Fe1A 129.1(7) . . ? Ru1B C16 Fe1A 0.4(5) . . ? C18 C17 C16 108.7(8) . . ? C18 C17 C20 126.0(9) . . ? C16 C17 C20 125.2(10) . . ? C18 C17 Ru1B 70.6(5) . . ? C16 C17 Ru1B 70.8(6) . . ? C20 C17 Ru1B 126.9(7) . . ? C18 C17 Fe1A 70.6(6) . . ? C16 C17 Fe1A 71.4(6) . . ? C20 C17 Fe1A 126.2(7) . . ? Ru1B C17 Fe1A 0.7(4) . . ? C17 C18 C14 108.0(7) . . ? C17 C18 C19 126.9(10) . . ? C14 C18 C19 124.8(9) . . ? C17 C18 Ru1B 70.6(5) . . ? C14 C18 Ru1B 71.2(5) . . ? C19 C18 Ru1B 128.6(7) . . ? C17 C18 Fe1A 71.0(6) . . ? C14 C18 Fe1A 71.7(6) . . ? C19 C18 Fe1A 127.8(7) . . ? Ru1B C18 Fe1A 0.8(4) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C15 C22 H22A 109.5 . . ? C15 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C15 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C14 C23 H23A 109.5 . . ? C14 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C14 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C1 124.9(7) . . ? C25 C24 P2 110.1(6) . . ? C1 C24 P2 124.9(6) . . ? C25 C24 Ru1A 71.2(5) . . ? C1 C24 Ru1A 123.6(6) . . ? P2 C24 Ru1A 70.3(3) . . ? C25 C24 Fe1B 71.8(5) . . ? C1 C24 Fe1B 123.3(6) . . ? P2 C24 Fe1B 70.0(4) . . ? Ru1A C24 Fe1B 0.6(4) . . ? C26 C25 C24 112.4(7) . . ? C26 C25 C28 123.2(7) . . ? C24 C25 C28 124.4(8) . . ? C26 C25 Ru1A 71.3(5) . . ? C24 C25 Ru1A 69.0(5) . . ? C28 C25 Ru1A 127.0(6) . . ? C26 C25 Fe1B 71.3(6) . . ? C24 C25 Fe1B 68.9(5) . . ? C28 C25 Fe1B 127.0(7) . . ? Ru1A C25 Fe1B 0.1(4) . . ? C25 C26 C27 114.9(6) . . ? C25 C26 C29 122.0(7) . . ? C27 C26 C29 123.1(7) . . ? C25 C26 Ru1A 70.5(5) . . ? C27 C26 Ru1A 72.3(4) . . ? C29 C26 Ru1A 128.1(6) . . ? C25 C26 Fe1B 71.0(5) . . ? C27 C26 Fe1B 71.9(5) . . ? C29 C26 Fe1B 128.0(7) . . ? Ru1A C26 Fe1B 0.4(4) . . ? C26 C27 C30 126.8(6) . . ? C26 C27 P2 109.1(6) . . ? C30 C27 P2 124.0(6) . . ? C26 C27 Ru1A 69.4(5) . . ? C30 C27 Ru1A 127.2(6) . . ? P2 C27 Ru1A 68.1(3) . . ? C26 C27 Fe1B 70.0(5) . . ? C30 C27 Fe1B 126.6(6) . . ? P2 C27 Fe1B 68.0(4) . . ? Ru1A C27 Fe1B 0.7(4) . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C35 C30 C31 117.3(8) . . ? C35 C30 C27 121.5(7) . . ? C31 C30 C27 121.1(8) . . ? C32 C31 C30 120.2(9) . . ? C32 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? C31 C32 C33 121.7(8) . . ? C31 C32 H32 119.2 . . ? C33 C32 H32 119.2 . . ? C32 C33 C34 118.6(8) . . ? C32 C33 H33 120.7 . . ? C34 C33 H33 120.7 . . ? C35 C34 C33 119.6(9) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C34 C35 C30 122.5(8) . . ? C34 C35 H35 118.8 . . ? C30 C35 H35 118.8 . . ? C40 C36 C37 106.9(9) . . ? C40 C36 C45 125.4(9) . . ? C37 C36 C45 127.6(10) . . ? C40 C36 Fe1B 69.8(6) . . ? C37 C36 Fe1B 70.8(6) . . ? C45 C36 Fe1B 127.1(8) . . ? C40 C36 Ru1A 70.6(5) . . ? C37 C36 Ru1A 70.7(6) . . ? C45 C36 Ru1A 126.5(7) . . ? Fe1B C36 Ru1A 0.8(4) . . ? C38 C37 C36 108.5(9) . . ? C38 C37 C44 126.7(11) . . ? C36 C37 C44 124.7(11) . . ? C38 C37 Fe1B 70.4(6) . . ? C36 C37 Fe1B 69.7(6) . . ? C44 C37 Fe1B 128.1(8) . . ? C38 C37 Ru1A 70.9(6) . . ? C36 C37 Ru1A 70.0(6) . . ? C44 C37 Ru1A 127.3(8) . . ? Fe1B C37 Ru1A 0.8(4) . . ? C39 C38 C37 107.1(9) . . ? C39 C38 C43 125.7(11) . . ? C37 C38 C43 127.1(11) . . ? C39 C38 Fe1B 71.0(6) . . ? C37 C38 Fe1B 70.7(6) . . ? C43 C38 Fe1B 125.2(8) . . ? C39 C38 Ru1A 71.7(6) . . ? C37 C38 Ru1A 70.4(6) . . ? C43 C38 Ru1A 124.8(7) . . ? Fe1B C38 Ru1A 0.7(4) . . ? C40 C39 C38 108.6(9) . . ? C40 C39 C42 126.7(9) . . ? C38 C39 C42 124.6(10) . . ? C40 C39 Fe1B 69.1(6) . . ? C38 C39 Fe1B 70.2(6) . . ? C42 C39 Fe1B 129.2(8) . . ? C40 C39 Ru1A 69.2(5) . . ? C38 C39 Ru1A 70.0(6) . . ? C42 C39 Ru1A 129.3(7) . . ? Fe1B C39 Ru1A 0.2(4) . . ? C36 C40 C39 108.7(7) . . ? C36 C40 C41 124.6(11) . . ? C39 C40 C41 126.4(11) . . ? C36 C40 Fe1B 71.1(6) . . ? C39 C40 Fe1B 72.0(6) . . ? C41 C40 Fe1B 127.3(6) . . ? C36 C40 Ru1A 70.8(5) . . ? C39 C40 Ru1A 72.3(5) . . ? C41 C40 Ru1A 127.3(6) . . ? Fe1B C40 Ru1A 0.4(4) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C39 C42 H42A 109.5 . . ? C39 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C39 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C38 C43 H43A 109.5 . . ? C38 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C38 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C37 C44 H44A 109.5 . . ? C37 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C37 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C36 C45 H45A 109.5 . . ? C36 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C36 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.994 _refine_diff_density_min -1.170 _refine_diff_density_rms 0.140 #===END