# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'P G Edwards' 'Martin Hanton' 'Paul Newman' 'Andreas Stasch' 'R P Tooze' 'Christopher Wallis' _publ_contact_author_name 'P G Edwards' _publ_contact_author_email EDWARDSPG@CARDIFF.AC.UK _publ_section_title ; Coordination Chemistry of 2,6-Dixylyl-4-phenylphosphabarrelene with Selected Transition Metals ; # Attachment 'Compound_3.CIF' data_pna21 _database_code_depnum_ccdc_archive 'CCDC 703036' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H42 Fe O2 P Si, P F6' _chemical_formula_sum 'C43 H42 F6 Fe O2 P2 Si' _chemical_formula_weight 850.65 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' F F 0.0171 0.0103 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 17.285(4) _cell_length_b 18.104(4) _cell_length_c 12.811(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4008.8(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6568 _cell_measurement_theta_min 3 _cell_measurement_theta_max 26.07 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760 _exptl_absorpt_coefficient_mu 0.550 _exptl_absorpt_correction_T_min 0.8747 _exptl_absorpt_correction_T_max 0.8979 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details DENZO/SCALEPACK _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'CCD scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21094 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_sigmaI/netI 0.0538 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 26.07 _reflns_number_total 7708 _reflns_number_gt 6568 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'cOLLECT,Nonius BV, 1997-2001' _computing_cell_refinement DENZO/SCALEPACK _computing_data_reduction DENZO/SCALEPACK _computing_structure_solution SHELXs-97 _computing_structure_refinement SHELXL-97 _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^)+(0.0661P)^2^+2.7096P] 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 0.01(2) _refine_ls_number_reflns 7708 _refine_ls_number_parameters 504 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0662 _refine_ls_R_factor_gt 0.0532 _refine_ls_wR_factor_ref 0.1352 _refine_ls_wR_factor_gt 0.1274 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 C1 C -0.0345(2) 0.8308(2) 1.0198(3) 0.0364(9) Uani 1 1 d . . . C2 C -0.0790(2) 0.7905(2) 1.0823(3) 0.0361(9) Uani 1 1 d . . . H2 H -0.1232 0.8125 1.1136 0.043 Uiso 1 1 calc R . . C3 C -0.0608(2) 0.7090(2) 1.1054(3) 0.0359(9) Uani 1 1 d . . . C4 C -0.0571(2) 0.6703(2) 0.9995(3) 0.0358(9) Uani 1 1 d . . . H4 H -0.0894 0.6288 0.9866 0.043 Uiso 1 1 calc R . . C5 C -0.0097(2) 0.6937(2) 0.9254(3) 0.0365(9) Uani 1 1 d . . . C6 C -0.0440(2) 0.9104(2) 0.9946(3) 0.0439(10) Uani 1 1 d . . . C7 C -0.0026(3) 0.9625(2) 1.0495(4) 0.0490(11) Uani 1 1 d . . . C8 C -0.0095(4) 1.0371(3) 1.0175(6) 0.082(2) Uani 1 1 d . . . H8 H 0.0189 1.0742 1.0531 0.098 Uiso 1 1 calc R . . C9 C -0.0573(5) 1.0566(4) 0.9347(6) 0.100(3) Uani 1 1 d . . . C10 C -0.0996(4) 1.0040(4) 0.8848(7) 0.091(3) Uani 1 1 d . . . H10 H -0.1335 1.0179 0.8299 0.109 Uiso 1 1 calc R . . C11 C -0.0940(3) 0.9319(3) 0.9126(5) 0.0653(15) Uani 1 1 d . . . H11 H -0.1238 0.8957 0.8769 0.078 Uiso 1 1 calc R . . C12 C 0.0394(4) 0.9447(4) 1.1390(6) 0.086(2) Uani 1 1 d . . . H12A H 0.0059 0.9493 1.2004 0.129 Uiso 1 1 calc R . . H12B H 0.0834 0.9785 1.1459 0.129 Uiso 1 1 calc R . . H12C H 0.0584 0.8938 1.1336 0.129 Uiso 1 1 calc R . . C13 C -0.0605(6) 1.1398(4) 0.9050(8) 0.138(4) Uani 1 1 d . . . H13A H -0.0581 1.1449 0.8289 0.207 Uiso 1 1 calc R . . H13B H -0.0166 1.1657 0.9366 0.207 Uiso 1 1 calc R . . H13C H -0.1089 1.1613 0.9307 0.207 Uiso 1 1 calc R . . C14 C -0.1190(2) 0.6764(2) 1.1825(3) 0.0377(9) Uani 1 1 d . . . C15 C -0.1295(2) 0.7128(2) 1.2775(4) 0.0456(10) Uani 1 1 d . . . H15 H -0.1029 0.7578 1.2903 0.055 Uiso 1 1 calc R . . C16 C -0.1781(2) 0.6841(3) 1.3534(4) 0.0497(10) Uani 1 1 d . . . H16 H -0.1843 0.7097 1.4176 0.060 Uiso 1 1 calc R . . C17 C -0.2180(3) 0.6186(3) 1.3368(4) 0.0547(12) Uani 1 1 d . . . H17 H -0.2511 0.5987 1.3889 0.066 Uiso 1 1 calc R . . C18 C -0.2079(3) 0.5830(3) 1.2417(4) 0.0542(12) Uani 1 1 d . . . H18 H -0.2348 0.5381 1.2291 0.065 Uiso 1 1 calc R . . C19 C -0.1600(3) 0.6106(2) 1.1650(4) 0.0454(10) Uani 1 1 d . . . H19 H -0.1548 0.5852 1.1005 0.054 Uiso 1 1 calc R . . C20 C 0.0228(2) 0.7071(2) 1.1496(3) 0.0332(8) Uani 1 1 d . . . C21 C 0.0809(2) 0.7399(2) 1.0896(3) 0.0352(8) Uani 1 1 d . . . C22 C 0.1558(2) 0.7445(2) 1.1258(3) 0.0410(10) Uani 1 1 d . . . H22 H 0.1944 0.7685 1.0856 0.049 Uiso 1 1 calc R . . C23 C 0.1742(2) 0.7135(3) 1.2219(4) 0.0480(11) Uani 1 1 d . . . H23 H 0.2256 0.7172 1.2476 0.058 Uiso 1 1 calc R . . C24 C 0.1201(3) 0.6782(2) 1.2791(4) 0.0489(11) Uani 1 1 d . . . H24 H 0.1341 0.6560 1.3436 0.059 Uiso 1 1 calc R . . C25 C 0.0429(2) 0.6740(2) 1.2440(3) 0.0408(9) Uani 1 1 d . . . H25 H 0.0050 0.6488 1.2842 0.049 Uiso 1 1 calc R . . C26 C -0.0037(2) 0.6596(2) 0.8198(3) 0.0386(9) Uani 1 1 d . . . C27 C 0.0545(3) 0.6089(2) 0.7979(3) 0.0451(10) Uani 1 1 d . . . C28 C 0.0575(3) 0.5787(3) 0.6972(4) 0.0554(12) Uani 1 1 d . . . H28 H 0.0967 0.5437 0.6813 0.067 Uiso 1 1 calc R . . C29 C 0.0049(3) 0.5983(3) 0.6199(4) 0.0558(12) Uani 1 1 d . . . C30 C -0.0517(3) 0.6486(3) 0.6434(4) 0.0518(12) Uani 1 1 d . . . H30 H -0.0875 0.6631 0.5910 0.062 Uiso 1 1 calc R . . C31 C -0.0574(3) 0.6786(2) 0.7433(4) 0.0451(10) Uani 1 1 d . . . H31 H -0.0980 0.7121 0.7593 0.054 Uiso 1 1 calc R . . C32 C 0.1148(3) 0.5868(3) 0.8769(4) 0.0549(12) Uani 1 1 d . . . H32A H 0.1127 0.5333 0.8879 0.082 Uiso 1 1 calc R . . H32B H 0.1047 0.6122 0.9431 0.082 Uiso 1 1 calc R . . H32C H 0.1662 0.6005 0.8511 0.082 Uiso 1 1 calc R . . C33 C 0.0113(4) 0.5639(4) 0.5122(4) 0.086(2) Uani 1 1 d . . . H33A H -0.0190 0.5930 0.4623 0.128 Uiso 1 1 calc R . . H33B H -0.0087 0.5132 0.5143 0.128 Uiso 1 1 calc R . . H33C H 0.0656 0.5632 0.4904 0.128 Uiso 1 1 calc R . . C34 C 0.1543(2) 0.9086(2) 0.7402(3) 0.0402(9) Uani 1 1 d . . . C35 C 0.0739(2) 0.9112(2) 0.7697(4) 0.0442(10) Uani 1 1 d . . . H35 H 0.0482 0.9525 0.7994 0.053 Uiso 1 1 calc R . . C36 C 0.0394(3) 0.8420(3) 0.7471(4) 0.0485(11) Uani 1 1 d . . . H36 H -0.0134 0.8295 0.7579 0.058 Uiso 1 1 calc R . . C37 C 0.0965(3) 0.7951(3) 0.7060(4) 0.0512(11) Uani 1 1 d . . . H37 H 0.0895 0.7451 0.6854 0.061 Uiso 1 1 calc R . . C38 C 0.1675(3) 0.8364(2) 0.7008(4) 0.0472(11) Uani 1 1 d . . . H38 H 0.2155 0.8184 0.6751 0.057 Uiso 1 1 calc R . . C39 C 0.1667(3) 1.0701(3) 0.7850(5) 0.0600(13) Uani 1 1 d . . . H39A H 0.1454 1.0596 0.8543 0.090 Uiso 1 1 calc R . . H39B H 0.1243 1.0792 0.7358 0.090 Uiso 1 1 calc R . . H39C H 0.2000 1.1139 0.7887 0.090 Uiso 1 1 calc R . . C40 C 0.2565(4) 1.0009(4) 0.6007(4) 0.0772(18) Uani 1 1 d . . . H40A H 0.2878 1.0458 0.5943 0.116 Uiso 1 1 calc R . . H40B H 0.2109 1.0049 0.5555 0.116 Uiso 1 1 calc R . . H40C H 0.2873 0.9580 0.5796 0.116 Uiso 1 1 calc R . . C41 C 0.3096(3) 0.9721(3) 0.8252(4) 0.0540(12) Uani 1 1 d . . . H41A H 0.3248 0.9201 0.8200 0.081 Uiso 1 1 calc R . . H41B H 0.2960 0.9836 0.8977 0.081 Uiso 1 1 calc R . . H41C H 0.3529 1.0035 0.8032 0.081 Uiso 1 1 calc R . . C42 C 0.2056(3) 0.7647(3) 0.8800(4) 0.0530(12) Uani 1 1 d . . . C43 C 0.1634(2) 0.8899(3) 0.9551(4) 0.0457(10) Uani 1 1 d . . . O1 O 0.2572(2) 0.7267(2) 0.8949(3) 0.0761(12) Uani 1 1 d . . . O2 O 0.1878(2) 0.92956(19) 1.0158(3) 0.0593(9) Uani 1 1 d . . . P1 P 0.04623(5) 0.77604(5) 0.96456(8) 0.0335(2) Uani 1 1 d . . . Si1 Si 0.22471(7) 0.98947(7) 0.73956(10) 0.0435(3) Uani 1 1 d . . . Fe1 Fe 0.12969(3) 0.82907(3) 0.85666(5) 0.03821(15) Uani 1 1 d . . . F1 F 0.2220(2) 0.6577(2) 0.6854(3) 0.1041(14) Uani 1 1 d . . . F2 F 0.2180(4) 0.6879(5) 0.5241(5) 0.214(4) Uani 1 1 d . . . F3 F 0.3058(3) 0.7321(3) 0.6173(6) 0.165(3) Uani 1 1 d . . . F4 F 0.3419(5) 0.6178(7) 0.6611(7) 0.269(6) Uani 1 1 d . . . F5 F 0.2445(6) 0.5766(3) 0.5635(7) 0.219(4) Uani 1 1 d . . . F6 F 0.3400(5) 0.6529(4) 0.5023(5) 0.184(3) Uani 1 1 d . . . P2 P 0.27840(11) 0.65242(9) 0.59271(13) 0.0736(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0357(19) 0.034(2) 0.040(2) 0.0034(17) -0.0050(17) 0.0053(16) C2 0.0294(18) 0.037(2) 0.042(2) 0.0028(18) -0.0031(17) 0.0070(16) C3 0.037(2) 0.033(2) 0.038(2) 0.0005(17) -0.0046(17) 0.0019(16) C4 0.034(2) 0.037(2) 0.036(2) -0.0030(17) -0.0037(17) -0.0039(16) C5 0.035(2) 0.030(2) 0.045(2) 0.0022(17) -0.0068(18) -0.0020(16) C6 0.041(2) 0.037(2) 0.053(3) 0.0101(19) 0.010(2) 0.0076(18) C7 0.060(3) 0.035(2) 0.053(3) 0.000(2) 0.013(2) 0.005(2) C8 0.106(5) 0.037(3) 0.103(5) -0.005(3) 0.050(4) 0.009(3) C9 0.112(5) 0.065(4) 0.122(6) 0.061(4) 0.062(5) 0.052(4) C10 0.070(4) 0.071(4) 0.132(7) 0.053(5) 0.032(4) 0.032(3) C11 0.047(3) 0.071(3) 0.078(3) 0.040(3) 0.013(3) 0.023(2) C12 0.088(4) 0.070(4) 0.101(5) -0.018(4) -0.013(4) 0.004(3) C13 0.158(8) 0.064(4) 0.193(9) 0.068(5) 0.079(7) 0.046(5) C14 0.035(2) 0.036(2) 0.042(2) 0.0057(18) -0.0056(17) -0.0011(16) C15 0.049(2) 0.040(2) 0.049(2) 0.005(2) -0.005(2) 0.0034(19) C16 0.053(2) 0.058(3) 0.038(2) 0.003(2) 0.004(2) 0.006(2) C17 0.046(2) 0.066(3) 0.052(3) 0.022(2) 0.006(2) 0.003(2) C18 0.054(3) 0.047(3) 0.062(3) 0.013(2) 0.004(2) -0.012(2) C19 0.053(2) 0.039(2) 0.044(2) 0.0004(19) 0.000(2) -0.002(2) C20 0.0334(19) 0.028(2) 0.038(2) -0.0020(16) -0.0077(17) -0.0004(15) C21 0.036(2) 0.027(2) 0.042(2) -0.0020(17) -0.0048(18) 0.0027(16) C22 0.034(2) 0.035(2) 0.054(3) -0.0023(19) -0.0048(19) 0.0027(17) C23 0.036(2) 0.045(3) 0.063(3) 0.000(2) -0.017(2) 0.0070(19) C24 0.054(3) 0.043(3) 0.049(2) 0.005(2) -0.015(2) 0.006(2) C25 0.038(2) 0.036(2) 0.048(2) 0.0038(19) 0.0016(19) 0.0027(16) C26 0.037(2) 0.036(2) 0.042(2) -0.0003(17) 0.0020(17) -0.0121(17) C27 0.054(3) 0.035(2) 0.046(2) -0.0016(19) 0.003(2) -0.0049(19) C28 0.070(3) 0.042(3) 0.054(3) -0.007(2) -0.001(2) 0.003(2) C29 0.071(3) 0.049(3) 0.047(3) -0.005(2) 0.000(2) -0.017(2) C30 0.054(3) 0.057(3) 0.044(3) 0.000(2) -0.010(2) -0.007(2) C31 0.048(2) 0.042(2) 0.045(3) -0.001(2) -0.003(2) -0.0083(18) C32 0.063(3) 0.050(3) 0.051(3) 0.002(2) -0.005(2) 0.010(2) C33 0.117(5) 0.087(5) 0.053(3) -0.023(3) 0.001(3) -0.014(4) C34 0.043(2) 0.039(2) 0.039(2) 0.0072(18) 0.0003(19) -0.0024(18) C35 0.045(2) 0.037(2) 0.050(2) 0.0073(19) -0.0025(19) 0.0013(18) C36 0.047(2) 0.046(3) 0.053(3) 0.011(2) -0.003(2) -0.007(2) C37 0.065(3) 0.043(3) 0.045(2) 0.003(2) -0.004(2) -0.016(2) C38 0.055(3) 0.040(3) 0.046(3) 0.0004(19) 0.011(2) -0.002(2) C39 0.058(3) 0.042(3) 0.080(4) 0.004(2) -0.005(3) -0.005(2) C40 0.077(4) 0.102(5) 0.053(3) 0.004(3) 0.012(3) -0.036(3) C41 0.045(2) 0.053(3) 0.064(3) 0.007(2) 0.001(2) 0.001(2) C42 0.050(2) 0.053(3) 0.056(3) 0.003(2) 0.006(2) -0.002(2) C43 0.043(2) 0.041(2) 0.054(3) 0.005(2) 0.000(2) -0.0064(19) O1 0.058(2) 0.092(3) 0.078(3) 0.005(2) 0.000(2) 0.035(2) O2 0.065(2) 0.054(2) 0.060(2) -0.0097(17) -0.0033(17) -0.0152(17) P1 0.0316(4) 0.0300(5) 0.0387(5) 0.0012(4) -0.0022(4) -0.0006(4) Si1 0.0416(6) 0.0431(7) 0.0457(6) 0.0048(5) 0.0037(5) -0.0052(5) Fe1 0.0371(3) 0.0338(3) 0.0437(3) 0.0017(3) 0.0018(3) -0.0024(2) F1 0.109(3) 0.119(3) 0.084(3) -0.003(2) 0.041(2) 0.000(2) F2 0.200(7) 0.285(10) 0.157(6) 0.064(6) -0.105(6) -0.040(6) F3 0.116(3) 0.132(4) 0.248(7) -0.097(5) 0.087(4) -0.051(3) F4 0.200(7) 0.380(14) 0.228(8) 0.114(9) 0.025(7) 0.185(9) F5 0.339(10) 0.083(4) 0.235(8) -0.068(4) 0.111(8) -0.028(5) F6 0.216(6) 0.187(6) 0.148(5) -0.026(5) 0.111(5) 0.021(5) P2 0.1009(12) 0.0637(10) 0.0562(8) -0.0097(7) 0.0164(8) 0.0003(9) _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 C1 C2 1.330(6) . ? C1 C6 1.485(6) . ? C1 P1 1.852(4) . ? C2 C3 1.537(5) . ? C3 C14 1.528(6) . ? C3 C4 1.528(6) . ? C3 C20 1.553(5) . ? C4 C5 1.324(6) . ? C5 C26 1.491(6) . ? C5 P1 1.847(4) . ? C6 C7 1.378(7) . ? C6 C11 1.415(7) . ? C7 C12 1.395(8) . ? C7 C8 1.416(7) . ? C8 C9 1.389(11) . ? C9 C10 1.361(11) . ? C9 C13 1.554(8) . ? C10 C11 1.357(8) . ? C14 C15 1.395(6) . ? C14 C19 1.405(6) . ? C15 C16 1.387(6) . ? C16 C17 1.388(7) . ? C17 C18 1.390(7) . ? C18 C19 1.378(6) . ? C20 C25 1.393(6) . ? C20 C21 1.397(6) . ? C21 C22 1.376(6) . ? C21 P1 1.832(4) . ? C22 C23 1.390(6) . ? C23 C24 1.348(7) . ? C24 C25 1.411(6) . ? C26 C27 1.388(6) . ? C26 C31 1.393(6) . ? C27 C28 1.403(7) . ? C27 C32 1.507(6) . ? C28 C29 1.390(7) . ? C29 C30 1.370(7) . ? C29 C33 1.518(7) . ? C30 C31 1.394(7) . ? C34 C38 1.419(6) . ? C34 C35 1.442(6) . ? C34 Si1 1.904(4) . ? C34 Fe1 2.117(4) . ? C35 C36 1.417(6) . ? C35 Fe1 2.093(4) . ? C36 C37 1.405(7) . ? C36 Fe1 2.113(5) . ? C37 C38 1.440(7) . ? C37 Fe1 2.106(5) . ? C38 Fe1 2.106(4) . ? C39 Si1 1.864(5) . ? C40 Si1 1.873(5) . ? C41 Si1 1.860(5) . ? C42 O1 1.143(5) . ? C42 Fe1 1.780(5) . ? C43 O2 1.138(5) . ? C43 Fe1 1.774(5) . ? P1 Fe1 2.2165(12) . ? F1 P2 1.539(4) . ? F2 P2 1.509(6) . ? F3 P2 1.550(5) . ? F4 P2 1.537(7) . ? F5 P2 1.538(6) . ? F6 P2 1.574(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 126.8(4) . . ? C2 C1 P1 111.8(3) . . ? C6 C1 P1 121.3(3) . . ? C1 C2 C3 121.6(4) . . ? C14 C3 C4 115.1(3) . . ? C14 C3 C2 111.0(3) . . ? C4 C3 C2 106.1(3) . . ? C14 C3 C20 111.6(3) . . ? C4 C3 C20 106.0(3) . . ? C2 C3 C20 106.3(3) . . ? C5 C4 C3 121.0(4) . . ? C4 C5 C26 124.2(4) . . ? C4 C5 P1 112.8(3) . . ? C26 C5 P1 123.0(3) . . ? C7 C6 C11 120.5(4) . . ? C7 C6 C1 119.7(4) . . ? C11 C6 C1 119.8(4) . . ? C6 C7 C12 122.2(5) . . ? C6 C7 C8 117.5(5) . . ? C12 C7 C8 120.1(6) . . ? C9 C8 C7 121.0(6) . . ? C10 C9 C8 119.9(6) . . ? C10 C9 C13 123.0(8) . . ? C8 C9 C13 117.1(9) . . ? C11 C10 C9 120.9(7) . . ? C10 C11 C6 120.2(7) . . ? C15 C14 C19 118.2(4) . . ? C15 C14 C3 117.9(4) . . ? C19 C14 C3 123.8(4) . . ? C16 C15 C14 121.0(4) . . ? C15 C16 C17 120.8(5) . . ? C16 C17 C18 118.0(4) . . ? C19 C18 C17 122.1(4) . . ? C18 C19 C14 119.9(4) . . ? C25 C20 C21 118.8(4) . . ? C25 C20 C3 123.9(4) . . ? C21 C20 C3 117.4(3) . . ? C22 C21 C20 121.1(4) . . ? C22 C21 P1 125.5(3) . . ? C20 C21 P1 113.4(3) . . ? C21 C22 C23 119.3(4) . . ? C24 C23 C22 120.9(4) . . ? C23 C24 C25 120.5(4) . . ? C20 C25 C24 119.3(4) . . ? C27 C26 C31 120.3(4) . . ? C27 C26 C5 120.5(4) . . ? C31 C26 C5 119.3(4) . . ? C26 C27 C28 118.0(4) . . ? C26 C27 C32 122.8(4) . . ? C28 C27 C32 119.2(4) . . ? C29 C28 C27 122.1(5) . . ? C30 C29 C28 118.6(5) . . ? C30 C29 C33 121.6(5) . . ? C28 C29 C33 119.7(5) . . ? C29 C30 C31 120.7(5) . . ? C26 C31 C30 120.2(4) . . ? C38 C34 C35 106.1(4) . . ? C38 C34 Si1 127.2(3) . . ? C35 C34 Si1 126.3(3) . . ? C38 C34 Fe1 69.9(2) . . ? C35 C34 Fe1 69.1(2) . . ? Si1 C34 Fe1 130.9(2) . . ? C36 C35 C34 108.9(4) . . ? C36 C35 Fe1 71.1(3) . . ? C34 C35 Fe1 70.9(2) . . ? C37 C36 C35 108.4(4) . . ? C37 C36 Fe1 70.3(3) . . ? C35 C36 Fe1 69.6(3) . . ? C36 C37 C38 107.6(4) . . ? C36 C37 Fe1 70.8(3) . . ? C38 C37 Fe1 70.0(3) . . ? C34 C38 C37 109.0(4) . . ? C34 C38 Fe1 70.8(2) . . ? C37 C38 Fe1 70.0(3) . . ? O1 C42 Fe1 176.0(4) . . ? O2 C43 Fe1 177.1(4) . . ? C21 P1 C5 96.96(18) . . ? C21 P1 C1 95.95(18) . . ? C5 P1 C1 98.14(19) . . ? C21 P1 Fe1 119.14(13) . . ? C5 P1 Fe1 121.39(14) . . ? C1 P1 Fe1 119.77(14) . . ? C41 Si1 C39 111.9(2) . . ? C41 Si1 C40 110.4(3) . . ? C39 Si1 C40 111.5(3) . . ? C41 Si1 C34 111.8(2) . . ? C39 Si1 C34 104.9(2) . . ? C40 Si1 C34 106.0(2) . . ? C43 Fe1 C42 92.6(2) . . ? C43 Fe1 C35 95.12(19) . . ? C42 Fe1 C35 153.4(2) . . ? C43 Fe1 C38 122.21(19) . . ? C42 Fe1 C38 88.4(2) . . ? C35 Fe1 C38 66.00(18) . . ? C43 Fe1 C37 157.4(2) . . ? C42 Fe1 C37 99.4(2) . . ? C35 Fe1 C37 66.05(19) . . ? C38 Fe1 C37 39.98(19) . . ? C43 Fe1 C36 130.3(2) . . ? C42 Fe1 C36 136.8(2) . . ? C35 Fe1 C36 39.38(17) . . ? C38 Fe1 C36 65.93(19) . . ? C37 Fe1 C36 38.9(2) . . ? C43 Fe1 C34 90.73(18) . . ? C42 Fe1 C34 114.55(19) . . ? C35 Fe1 C34 40.07(16) . . ? C38 Fe1 C34 39.26(17) . . ? C37 Fe1 C34 66.89(17) . . ? C36 Fe1 C34 66.74(17) . . ? C43 Fe1 P1 92.27(15) . . ? C42 Fe1 P1 95.22(15) . . ? C35 Fe1 P1 109.85(13) . . ? C38 Fe1 P1 145.18(14) . . ? C37 Fe1 P1 105.52(13) . . ? C36 Fe1 P1 88.93(13) . . ? C34 Fe1 P1 149.91(12) . . ? F2 P2 F4 178.2(5) . . ? F2 P2 F5 88.5(5) . . ? F4 P2 F5 92.7(6) . . ? F2 P2 F1 89.1(4) . . ? F4 P2 F1 92.2(4) . . ? F5 P2 F1 90.1(3) . . ? F2 P2 F3 86.2(4) . . ? F4 P2 F3 92.6(6) . . ? F5 P2 F3 174.7(5) . . ? F1 P2 F3 88.8(3) . . ? F2 P2 F6 92.1(4) . . ? F4 P2 F6 86.5(4) . . ? F5 P2 F6 94.8(4) . . ? F1 P2 F6 175.0(4) . . ? F3 P2 F6 86.4(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.07 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.891 _refine_diff_density_min -0.406 _refine_diff_density_rms 0.058 # Attachment 'Compound_4.CIF' data_cj444 _database_code_depnum_ccdc_archive 'CCDC 703037' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H43 Cl2 P Ru, 0.5(C H2 Cl2)' _chemical_formula_sum 'C43.50 H44 Cl3 P Ru' _chemical_formula_weight 805.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.238(2) _cell_length_b 13.693(3) _cell_length_c 16.451(3) _cell_angle_alpha 107.20(3) _cell_angle_beta 103.59(3) _cell_angle_gamma 106.38(3) _cell_volume 1982.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6038 _cell_measurement_theta_min 2.92 _cell_measurement_theta_max 25.9 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 830 _exptl_absorpt_coefficient_mu 0.667 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.800 _exptl_absorpt_correction_T_max 0.906 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13631 _diffrn_reflns_av_R_equivalents 0.0352 _diffrn_reflns_av_sigmaI/netI 0.0586 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 25.90 _reflns_number_total 7520 _reflns_number_gt 6038 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'cOLLECT,Nonius BV, 1997-2001' _computing_cell_refinement DENZO/SCALEPACK _computing_data_reduction DENZO/SCALEPACK _computing_structure_solution SHELXs-97 _computing_structure_refinement SHELXL-97 _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^)+(0.0770P)^2^+2.3610P] 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 7520 _refine_ls_number_parameters 458 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0675 _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.1500 _refine_ls_wR_factor_gt 0.1409 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.49056(4) 0.13804(3) 0.16316(2) 0.03321(13) Uani 1 1 d . . . Cl1 Cl 0.45964(12) -0.04708(9) 0.15087(7) 0.0394(3) Uani 1 1 d . . . P1 P 0.54221(11) 0.17649(9) 0.31954(7) 0.0310(2) Uani 1 1 d . . . C1 C 0.6639(4) 0.1264(3) 0.3831(3) 0.0319(9) Uani 1 1 d . . . Cl2 Cl 0.74295(12) 0.17292(10) 0.18656(8) 0.0426(3) Uani 1 1 d . . . C2 C 0.6758(4) 0.1541(3) 0.4747(3) 0.0321(9) Uani 1 1 d . . . Cl3 Cl -0.0801(3) -0.3294(2) -0.1244(2) 0.0726(9) Uani 0.50 1 d P . . C3 C 0.5888(4) 0.2236(3) 0.5099(3) 0.0346(9) Uani 1 1 d . . . Cl4 Cl -0.1170(4) -0.4210(2) 0.0133(2) 0.0727(8) Uani 0.50 1 d P . . C4 C 0.6356(5) 0.3266(4) 0.4890(3) 0.0387(10) Uani 1 1 d . . . H4 H 0.6749 0.3973 0.5372 0.046 Uiso 1 1 calc R . . C5 C 0.6228(5) 0.3201(4) 0.4051(3) 0.0369(9) Uani 1 1 d . . . C6 C 0.4315(5) 0.1558(3) 0.4489(3) 0.0345(9) Uani 1 1 d . . . H6 H 0.3609 0.1340 0.4752 0.041 Uiso 1 1 calc R . . C7 C 0.3905(4) 0.1265(3) 0.3596(3) 0.0326(9) Uani 1 1 d . . . C8 C 0.7610(5) 0.1182(4) 0.5288(3) 0.0372(10) Uani 1 1 d . . . H8 H 0.7688 0.1359 0.5906 0.045 Uiso 1 1 calc R . . C9 C 0.8348(5) 0.0561(4) 0.4919(3) 0.0387(10) Uani 1 1 d . . . H9 H 0.8933 0.0317 0.5289 0.046 Uiso 1 1 calc R . . C10 C 0.8240(5) 0.0295(4) 0.4019(3) 0.0380(10) Uani 1 1 d . . . H10 H 0.8756 -0.0124 0.3776 0.046 Uiso 1 1 calc R . . C11 C 0.7371(4) 0.0642(3) 0.3469(3) 0.0343(9) Uani 1 1 d . . . H11 H 0.7284 0.0451 0.2849 0.041 Uiso 1 1 calc R . . C12 C 0.6160(5) 0.2520(4) 0.6111(3) 0.0375(10) Uani 1 1 d . . . C13 C 0.5222(5) 0.1906(4) 0.6425(3) 0.0396(10) Uani 1 1 d . . . H13 H 0.4397 0.1274 0.6001 0.048 Uiso 1 1 calc R . . C14 C 0.5473(5) 0.2203(4) 0.7349(3) 0.0465(11) Uani 1 1 d . . . H14 H 0.4796 0.1796 0.7552 0.056 Uiso 1 1 calc R . . C15 C 0.6709(6) 0.3089(4) 0.7975(3) 0.0573(14) Uani 1 1 d . . . H15 H 0.6893 0.3287 0.8607 0.069 Uiso 1 1 calc R . . C16 C 0.7664(6) 0.3676(5) 0.7670(3) 0.0634(15) Uani 1 1 d . . . H16 H 0.8522 0.4278 0.8096 0.076 Uiso 1 1 calc R . . C17 C 0.7399(6) 0.3406(4) 0.6750(3) 0.0529(12) Uani 1 1 d . . . H17 H 0.8068 0.3830 0.6553 0.063 Uiso 1 1 calc R . . C18 C 0.6727(5) 0.4227(4) 0.3871(3) 0.0408(10) Uani 1 1 d . . . C19 C 0.8102(5) 0.4652(4) 0.3829(4) 0.0502(12) Uani 1 1 d . . . C20 C 0.8526(6) 0.5674(4) 0.3741(4) 0.0602(14) Uani 1 1 d . . . H20 H 0.9468 0.5978 0.3719 0.072 Uiso 1 1 calc R . . C21 C 0.7612(6) 0.6253(4) 0.3685(4) 0.0602(14) Uani 1 1 d . . . C22 C 0.6282(6) 0.5826(4) 0.3732(4) 0.0569(14) Uani 1 1 d . . . H22 H 0.5650 0.6216 0.3698 0.068 Uiso 1 1 calc R . . C23 C 0.5839(6) 0.4842(4) 0.3827(3) 0.0487(12) Uani 1 1 d . . . H23 H 0.4904 0.4565 0.3866 0.058 Uiso 1 1 calc R . . C24 C 0.9147(6) 0.4094(5) 0.3919(5) 0.0716(17) Uani 1 1 d . . . H24A H 0.9111 0.3807 0.4397 0.107 Uiso 1 1 calc R . . H24B H 1.0130 0.4624 0.4078 0.107 Uiso 1 1 calc R . . H24C H 0.8891 0.3482 0.3342 0.107 Uiso 1 1 calc R . . C25 C 0.8126(7) 0.7354(5) 0.3580(5) 0.080(2) Uani 1 1 d . . . H25A H 0.8406 0.7961 0.4164 0.121 Uiso 1 1 calc R . . H25B H 0.7339 0.7387 0.3129 0.121 Uiso 1 1 calc R . . H25C H 0.8964 0.7422 0.3379 0.121 Uiso 1 1 calc R . . C26 C 0.2382(4) 0.0514(4) 0.2994(3) 0.0342(9) Uani 1 1 d . . . C27 C 0.1252(5) 0.0911(4) 0.2858(3) 0.0421(11) Uani 1 1 d . . . C28 C -0.0147(5) 0.0156(5) 0.2333(3) 0.0473(12) Uani 1 1 d . . . H28 H -0.0906 0.0422 0.2215 0.057 Uiso 1 1 calc R . . C29 C -0.0481(5) -0.0978(5) 0.1973(3) 0.0476(12) Uani 1 1 d . . . C30 C 0.0636(5) -0.1348(4) 0.2123(3) 0.0448(11) Uani 1 1 d . . . H30 H 0.0431 -0.2119 0.1885 0.054 Uiso 1 1 calc R . . C31 C 0.2052(5) -0.0615(4) 0.2616(3) 0.0383(10) Uani 1 1 d . . . H31 H 0.2809 -0.0888 0.2698 0.046 Uiso 1 1 calc R . . C32 C 0.1553(6) 0.2127(5) 0.3298(4) 0.0645(15) Uani 1 1 d . . . H32A H 0.1713 0.2329 0.3947 0.097 Uiso 1 1 calc R . . H32B H 0.0721 0.2280 0.3014 0.097 Uiso 1 1 calc R . . H32C H 0.2420 0.2560 0.3219 0.097 Uiso 1 1 calc R . . C33 C -0.2049(6) -0.1789(6) 0.1422(4) 0.0695(17) Uani 1 1 d . . . H33A H -0.2712 -0.1403 0.1502 0.104 Uiso 1 1 calc R . . H33B H -0.2273 -0.2394 0.1633 0.104 Uiso 1 1 calc R . . H33C H -0.2165 -0.2088 0.0778 0.104 Uiso 1 1 calc R . . C34 C 0.4935(5) 0.2793(4) 0.1203(3) 0.0426(11) Uani 1 1 d . . . C35 C 0.3921(5) 0.2598(4) 0.1633(3) 0.0399(10) Uani 1 1 d . . . H35 H 0.3991 0.3187 0.2145 0.048 Uiso 1 1 calc R . . C36 C 0.2781(5) 0.1543(4) 0.1332(3) 0.0388(10) Uani 1 1 d . . . H36 H 0.2093 0.1447 0.1630 0.047 Uiso 1 1 calc R . . C37 C 0.2682(5) 0.0650(4) 0.0592(3) 0.0400(10) Uani 1 1 d . . . C38 C 0.3743(5) 0.0835(4) 0.0157(3) 0.0426(11) Uani 1 1 d . . . H38 H 0.3703 0.0240 -0.0339 0.051 Uiso 1 1 calc R . . C39 C 0.4829(5) 0.1878(4) 0.0454(3) 0.0426(11) Uani 1 1 d . . . H39 H 0.5511 0.1982 0.0152 0.051 Uiso 1 1 calc R . . C40 C 0.6003(5) 0.3942(4) 0.1484(4) 0.0541(13) Uani 1 1 d . . . H40 H 0.6359 0.4292 0.2162 0.065 Uiso 1 1 calc R . . C41 C 0.5211(7) 0.4609(5) 0.1122(5) 0.080(2) Uani 1 1 d . . . H41A H 0.4932 0.4333 0.0460 0.120 Uiso 1 1 calc R . . H41B H 0.5856 0.5390 0.1387 0.120 Uiso 1 1 calc R . . H41C H 0.4339 0.4531 0.1288 0.120 Uiso 1 1 calc R . . C42 C 0.7347(7) 0.4010(6) 0.1195(5) 0.084(2) Uani 1 1 d . . . H42A H 0.7857 0.3602 0.1449 0.127 Uiso 1 1 calc R . . H42B H 0.8000 0.4785 0.1422 0.127 Uiso 1 1 calc R . . H42C H 0.7036 0.3687 0.0532 0.127 Uiso 1 1 calc R . . C43 C 0.1530(5) -0.0473(4) 0.0261(3) 0.0502(12) Uani 1 1 d . . . H43A H 0.1050 -0.0506 0.0708 0.075 Uiso 1 1 calc R . . H43B H 0.1970 -0.1028 0.0177 0.075 Uiso 1 1 calc R . . H43C H 0.0813 -0.0622 -0.0318 0.075 Uiso 1 1 calc R . . C44 C -0.0059(14) -0.3368(11) -0.0194(8) 0.072(3) Uani 0.50 1 d PU . . H44A H 0.0767 -0.3603 -0.0214 0.086 Uiso 0.50 1 calc PR . . H44B H 0.0340 -0.2613 0.0281 0.086 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0383(2) 0.0464(2) 0.0310(2) 0.02253(16) 0.01854(15) 0.02545(17) Cl1 0.0480(6) 0.0478(6) 0.0365(6) 0.0236(5) 0.0202(5) 0.0257(5) P1 0.0362(6) 0.0400(6) 0.0308(5) 0.0199(5) 0.0175(4) 0.0229(5) C1 0.035(2) 0.038(2) 0.031(2) 0.0173(18) 0.0159(17) 0.0185(18) Cl2 0.0398(6) 0.0576(7) 0.0466(6) 0.0300(5) 0.0211(5) 0.0260(5) C2 0.034(2) 0.036(2) 0.034(2) 0.0177(18) 0.0163(18) 0.0166(18) Cl3 0.0480(15) 0.0467(14) 0.121(3) 0.0425(16) 0.0094(15) 0.0209(12) C3 0.041(2) 0.043(2) 0.030(2) 0.0176(19) 0.0179(18) 0.022(2) Cl4 0.084(2) 0.0460(15) 0.0695(18) 0.0146(13) 0.0211(16) 0.0105(14) C4 0.043(2) 0.041(2) 0.037(2) 0.014(2) 0.0158(19) 0.023(2) C5 0.040(2) 0.040(2) 0.041(2) 0.021(2) 0.0169(19) 0.0226(19) C6 0.039(2) 0.042(2) 0.034(2) 0.0186(19) 0.0202(18) 0.0220(19) C7 0.035(2) 0.042(2) 0.034(2) 0.0197(19) 0.0180(18) 0.0230(19) C8 0.040(2) 0.048(3) 0.031(2) 0.021(2) 0.0140(18) 0.019(2) C9 0.040(2) 0.048(3) 0.037(2) 0.025(2) 0.0118(19) 0.023(2) C10 0.041(2) 0.045(2) 0.039(2) 0.021(2) 0.0164(19) 0.025(2) C11 0.039(2) 0.045(2) 0.033(2) 0.0210(19) 0.0172(18) 0.026(2) C12 0.046(3) 0.044(2) 0.032(2) 0.0143(19) 0.0177(19) 0.026(2) C13 0.049(3) 0.045(2) 0.030(2) 0.0149(19) 0.0143(19) 0.025(2) C14 0.059(3) 0.058(3) 0.042(3) 0.029(2) 0.026(2) 0.033(3) C15 0.080(4) 0.061(3) 0.031(2) 0.012(2) 0.020(3) 0.032(3) C16 0.071(4) 0.061(3) 0.036(3) 0.007(3) 0.011(3) 0.012(3) C17 0.050(3) 0.062(3) 0.037(3) 0.015(2) 0.013(2) 0.015(2) C18 0.042(3) 0.041(2) 0.042(2) 0.018(2) 0.012(2) 0.019(2) C19 0.039(3) 0.062(3) 0.061(3) 0.037(3) 0.015(2) 0.022(2) C20 0.042(3) 0.062(3) 0.074(4) 0.037(3) 0.013(3) 0.011(2) C21 0.057(3) 0.051(3) 0.070(4) 0.033(3) 0.007(3) 0.018(3) C22 0.048(3) 0.049(3) 0.075(4) 0.029(3) 0.012(3) 0.022(2) C23 0.053(3) 0.042(3) 0.060(3) 0.025(2) 0.020(2) 0.025(2) C24 0.051(3) 0.070(4) 0.100(5) 0.035(4) 0.025(3) 0.031(3) C25 0.067(4) 0.061(4) 0.103(5) 0.047(4) 0.009(4) 0.010(3) C26 0.036(2) 0.053(3) 0.030(2) 0.0230(19) 0.0196(18) 0.025(2) C27 0.043(3) 0.066(3) 0.040(2) 0.030(2) 0.024(2) 0.036(2) C28 0.036(2) 0.084(4) 0.045(3) 0.036(3) 0.022(2) 0.037(3) C29 0.032(2) 0.081(4) 0.041(3) 0.036(3) 0.015(2) 0.022(2) C30 0.045(3) 0.055(3) 0.038(2) 0.025(2) 0.014(2) 0.018(2) C31 0.041(2) 0.050(3) 0.035(2) 0.022(2) 0.0167(19) 0.024(2) C32 0.072(4) 0.078(4) 0.070(4) 0.033(3) 0.031(3) 0.055(3) C33 0.039(3) 0.102(5) 0.063(4) 0.046(3) 0.009(3) 0.013(3) C34 0.050(3) 0.054(3) 0.043(3) 0.034(2) 0.018(2) 0.029(2) C35 0.046(3) 0.049(3) 0.039(2) 0.023(2) 0.017(2) 0.031(2) C36 0.036(2) 0.061(3) 0.036(2) 0.025(2) 0.0167(19) 0.031(2) C37 0.042(2) 0.056(3) 0.032(2) 0.025(2) 0.0108(19) 0.027(2) C38 0.057(3) 0.061(3) 0.028(2) 0.024(2) 0.019(2) 0.039(3) C39 0.050(3) 0.067(3) 0.038(2) 0.038(2) 0.024(2) 0.035(2) C40 0.055(3) 0.061(3) 0.063(3) 0.044(3) 0.021(3) 0.024(3) C41 0.085(4) 0.066(4) 0.108(5) 0.060(4) 0.026(4) 0.032(3) C42 0.072(4) 0.085(5) 0.129(6) 0.069(5) 0.052(4) 0.032(4) C43 0.047(3) 0.060(3) 0.041(3) 0.018(2) 0.010(2) 0.022(2) C44 0.074(5) 0.074(5) 0.063(5) 0.017(4) 0.036(4) 0.021(4) _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 C35 2.177(4) . ? Ru1 C36 2.204(4) . ? Ru1 C38 2.221(4) . ? Ru1 C39 2.228(4) . ? Ru1 C37 2.232(4) . ? Ru1 C34 2.240(4) . ? Ru1 P1 2.3619(12) . ? Ru1 Cl2 2.4044(12) . ? Ru1 Cl1 2.4043(12) . ? P1 C1 1.846(4) . ? P1 C5 1.852(5) . ? P1 C7 1.862(4) . ? C1 C11 1.383(5) . ? C1 C2 1.407(6) . ? C2 C8 1.390(6) . ? C2 C3 1.559(5) . ? Cl3 C44 1.761(13) . ? C3 C6 1.520(6) . ? C3 C4 1.524(6) . ? C3 C12 1.529(6) . ? Cl4 C44 1.681(12) . ? C4 C5 1.329(6) . ? C5 C18 1.497(6) . ? C6 C7 1.326(6) . ? C7 C26 1.496(6) . ? C8 C9 1.391(6) . ? C9 C10 1.385(6) . ? C10 C11 1.396(5) . ? C12 C13 1.389(6) . ? C12 C17 1.391(7) . ? C13 C14 1.392(6) . ? C14 C15 1.384(7) . ? C15 C16 1.371(8) . ? C16 C17 1.386(7) . ? C18 C19 1.389(7) . ? C18 C23 1.407(6) . ? C19 C20 1.405(7) . ? C19 C24 1.485(7) . ? C20 C21 1.392(7) . ? C21 C22 1.353(8) . ? C21 C25 1.525(7) . ? C22 C23 1.363(7) . ? C26 C31 1.389(6) . ? C26 C27 1.411(6) . ? C27 C28 1.386(7) . ? C27 C32 1.511(7) . ? C28 C29 1.393(7) . ? C29 C30 1.376(6) . ? C29 C33 1.533(7) . ? C30 C31 1.383(6) . ? C34 C35 1.396(6) . ? C34 C39 1.431(7) . ? C34 C40 1.500(7) . ? C35 C36 1.431(7) . ? C36 C37 1.407(6) . ? C37 C38 1.440(6) . ? C37 C43 1.494(7) . ? C38 C39 1.397(7) . ? C40 C41 1.536(7) . ? C40 C42 1.546(8) . ? 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 C35 Ru1 C36 38.12(17) . . ? C35 Ru1 C38 79.05(17) . . ? C36 Ru1 C38 67.04(16) . . ? C35 Ru1 C39 66.48(17) . . ? C36 Ru1 C39 79.09(16) . . ? C38 Ru1 C39 36.60(18) . . ? C35 Ru1 C37 67.65(17) . . ? C36 Ru1 C37 36.97(16) . . ? C38 Ru1 C37 37.74(16) . . ? C39 Ru1 C37 67.18(17) . . ? C35 Ru1 C34 36.82(16) . . ? C36 Ru1 C34 67.77(17) . . ? C38 Ru1 C34 67.10(18) . . ? C39 Ru1 C34 37.36(17) . . ? C37 Ru1 C34 80.15(17) . . ? C35 Ru1 P1 94.54(12) . . ? C36 Ru1 P1 98.05(12) . . ? C38 Ru1 P1 162.77(13) . . ? C39 Ru1 P1 152.95(14) . . ? C37 Ru1 P1 125.04(12) . . ? C34 Ru1 P1 116.53(13) . . ? C35 Ru1 Cl2 124.79(13) . . ? C36 Ru1 Cl2 161.74(12) . . ? C38 Ru1 Cl2 108.05(13) . . ? C39 Ru1 Cl2 87.12(12) . . ? C37 Ru1 Cl2 144.77(12) . . ? C34 Ru1 Cl2 94.03(12) . . ? P1 Ru1 Cl2 88.78(5) . . ? C35 Ru1 Cl1 147.70(13) . . ? C36 Ru1 Cl1 109.95(13) . . ? C38 Ru1 Cl1 92.76(13) . . ? C39 Ru1 Cl1 122.32(13) . . ? C37 Ru1 Cl1 86.70(13) . . ? C34 Ru1 Cl1 159.27(13) . . ? P1 Ru1 Cl1 84.15(5) . . ? Cl2 Ru1 Cl1 87.50(5) . . ? C1 P1 C5 95.32(19) . . ? C1 P1 C7 95.03(18) . . ? C5 P1 C7 96.50(19) . . ? C1 P1 Ru1 123.09(13) . . ? C5 P1 Ru1 121.56(14) . . ? C7 P1 Ru1 118.87(14) . . ? C11 C1 C2 120.3(4) . . ? C11 C1 P1 125.3(3) . . ? C2 C1 P1 114.5(3) . . ? C8 C2 C1 119.8(4) . . ? C8 C2 C3 123.1(4) . . ? C1 C2 C3 117.1(3) . . ? C6 C3 C4 106.6(3) . . ? C6 C3 C12 114.5(3) . . ? C4 C3 C12 112.0(4) . . ? C6 C3 C2 105.1(3) . . ? C4 C3 C2 106.1(3) . . ? C12 C3 C2 111.8(3) . . ? C5 C4 C3 121.6(4) . . ? C4 C5 C18 120.3(4) . . ? C4 C5 P1 113.6(3) . . ? C18 C5 P1 126.1(3) . . ? C7 C6 C3 121.6(4) . . ? C6 C7 C26 121.1(4) . . ? C6 C7 P1 113.6(3) . . ? C26 C7 P1 125.1(3) . . ? C2 C8 C9 119.5(4) . . ? C10 C9 C8 120.8(4) . . ? C9 C10 C11 119.9(4) . . ? C1 C11 C10 119.7(4) . . ? C13 C12 C17 118.0(4) . . ? C13 C12 C3 122.2(4) . . ? C17 C12 C3 119.8(4) . . ? C12 C13 C14 121.0(4) . . ? C15 C14 C13 120.1(5) . . ? C16 C15 C14 119.1(5) . . ? C15 C16 C17 121.0(5) . . ? C16 C17 C12 120.6(5) . . ? C19 C18 C23 118.5(4) . . ? C19 C18 C5 122.0(4) . . ? C23 C18 C5 119.2(4) . . ? C18 C19 C20 118.0(4) . . ? C18 C19 C24 122.5(5) . . ? C20 C19 C24 119.5(5) . . ? C21 C20 C19 122.1(5) . . ? C22 C21 C20 118.8(5) . . ? C22 C21 C25 121.4(5) . . ? C20 C21 C25 119.8(5) . . ? C21 C22 C23 120.7(5) . . ? C22 C23 C18 121.8(5) . . ? C31 C26 C27 119.1(4) . . ? C31 C26 C7 119.0(4) . . ? C27 C26 C7 121.7(4) . . ? C28 C27 C26 118.4(4) . . ? C28 C27 C32 120.8(4) . . ? C26 C27 C32 120.7(4) . . ? C27 C28 C29 122.3(4) . . ? C30 C29 C28 118.2(4) . . ? C30 C29 C33 121.0(5) . . ? C28 C29 C33 120.8(5) . . ? C29 C30 C31 120.9(5) . . ? C30 C31 C26 120.9(4) . . ? C35 C34 C39 117.3(4) . . ? C35 C34 C40 120.0(4) . . ? C39 C34 C40 122.5(4) . . ? C35 C34 Ru1 69.1(2) . . ? C39 C34 Ru1 70.8(2) . . ? C40 C34 Ru1 135.2(3) . . ? C34 C35 C36 122.4(4) . . ? C34 C35 Ru1 74.1(2) . . ? C36 C35 Ru1 72.0(2) . . ? C37 C36 C35 119.8(4) . . ? C37 C36 Ru1 72.6(2) . . ? C35 C36 Ru1 69.9(2) . . ? C36 C37 C38 118.2(4) . . ? C36 C37 C43 121.9(4) . . ? C38 C37 C43 119.8(4) . . ? C36 C37 Ru1 70.4(2) . . ? C38 C37 Ru1 70.7(2) . . ? C43 C37 Ru1 129.7(3) . . ? C39 C38 C37 120.8(4) . . ? C39 C38 Ru1 72.0(3) . . ? C37 C38 Ru1 71.6(2) . . ? C38 C39 C34 121.3(4) . . ? C38 C39 Ru1 71.4(2) . . ? C34 C39 Ru1 71.8(2) . . ? C34 C40 C41 109.0(4) . . ? C34 C40 C42 114.8(5) . . ? C41 C40 C42 110.6(5) . . ? Cl4 C44 Cl3 117.5(7) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 25.90 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 1.460 _refine_diff_density_min -0.637 _refine_diff_density_rms 0.102