# 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 _journal_year ? _journal_volume ? _journal_page_first ? _publ_requested_category FM _publ_contact_author_email cedric.fischmeister@univ-rennes1.fr _publ_contact_author_name 'Cedric Fischmeister' _publ_author_name 'Cedric Fischmeister' data_job1 _database_code_depnum_ccdc_archive 'CCDC 856296' #TrackingRef 'C3(H).cif' _audit_creation_date 2010-11-22T14:40:10-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C33 H33 Cl2 O2 P Ru' _chemical_formula_sum 'C33 H33 Cl2 O2 P Ru' _chemical_formula_weight 664.53 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c 21 n' _symmetry_space_group_name_Hall 'P -2n -2ac' _symmetry_Int_Tables_number 33 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x+1/2, y, z+1/2' 'x+1/2, y+1/2, -z+1/2' _cell_length_a 9.3880(3) _cell_length_b 13.0791(4) _cell_length_c 24.1874(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2969.89(16) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5782 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 27.49 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.486 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.791 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.602 _exptl_absorpt_correction_T_max 0.946 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_unetI/netI 0.0482 _diffrn_reflns_number 12458 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 5163 _reflns_number_gt 4806 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SAINT (Bruker, 2002)' _computing_cell_refinement 'Bruker SMART (Bruker, 2002)' _computing_data_reduction 'Bruker SAINT (Bruker, 2002)' _computing_structure_solution 'SIR97 (Altomare et al., 1999))' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 1999), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0402P)^2^+0.4954P] 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_number_reflns 5163 _refine_ls_number_parameters 345 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0352 _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_ref 0.0821 _refine_ls_wR_factor_gt 0.0795 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.04(3) _refine_diff_density_max 0.737 _refine_diff_density_min -0.418 _refine_diff_density_rms 0.077 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.45819(2) 0.37018(2) 0.367381(9) 0.01779(8) Uani 1 1 d . . . Cl1 Cl 0.44582(11) 0.26317(8) 0.44294(4) 0.0311(2) Uani 1 1 d . . . Cl2 Cl 0.61041(9) 0.46708(8) 0.31355(4) 0.0266(2) Uani 1 1 d . . . P1 P 0.45751(8) 0.24496(8) 0.30476(4) 0.0170(2) Uani 1 1 d . . . C1 C 0.3820(4) 0.1216(3) 0.32445(14) 0.0201(7) Uani 1 1 d . . . C2 C 0.2537(4) 0.1180(3) 0.35387(15) 0.0253(8) Uani 1 1 d . . . H2 H 0.2092 0.18 0.3648 0.03 Uiso 1 1 calc R . . C3 C 0.1912(4) 0.0266(4) 0.36709(16) 0.0317(10) Uani 1 1 d . . . H3 H 0.1051 0.0259 0.3877 0.038 Uiso 1 1 calc R . . C4 C 0.2527(4) -0.0651(3) 0.35061(18) 0.0334(9) Uani 1 1 d . . . H4 H 0.209 -0.1284 0.3596 0.04 Uiso 1 1 calc R . . C5 C 0.3809(4) -0.0628(3) 0.32030(18) 0.0333(9) Uani 1 1 d . . . H5 H 0.4239 -0.1246 0.3082 0.04 Uiso 1 1 calc R . . C6 C 0.4435(4) 0.0300(3) 0.30828(15) 0.0269(8) Uani 1 1 d . . . H6 H 0.5308 0.0311 0.2884 0.032 Uiso 1 1 calc R . . C7 C 0.6409(3) 0.2122(3) 0.28808(14) 0.0208(7) Uani 1 1 d . . . C8 C 0.7369(4) 0.2016(3) 0.33241(15) 0.0288(9) Uani 1 1 d . . . H8 H 0.7058 0.2137 0.3692 0.035 Uiso 1 1 calc R . . C9 C 0.8752(4) 0.1738(4) 0.32239(17) 0.0346(10) Uani 1 1 d . . . H9 H 0.9394 0.1662 0.3525 0.041 Uiso 1 1 calc R . . C10 C 0.9220(4) 0.1570(4) 0.26995(19) 0.0337(10) Uani 1 1 d . . . H10 H 1.0183 0.138 0.2637 0.04 Uiso 1 1 calc R . . C11 C 0.8299(4) 0.1676(4) 0.22564(16) 0.0333(10) Uani 1 1 d . . . H11 H 0.8626 0.1548 0.1891 0.04 Uiso 1 1 calc R . . C12 C 0.6889(4) 0.1972(3) 0.23462(15) 0.0273(8) Uani 1 1 d . . . H12 H 0.6263 0.2069 0.2042 0.033 Uiso 1 1 calc R . . C13 C 0.3689(3) 0.2733(3) 0.23879(12) 0.0189(7) Uani 1 1 d . . . C14 C 0.2853(3) 0.2003(3) 0.21256(14) 0.0224(8) Uani 1 1 d . . . H14 H 0.2784 0.1334 0.2277 0.027 Uiso 1 1 calc R . . C15 C 0.2110(4) 0.2243(3) 0.16416(14) 0.0275(9) Uani 1 1 d . . . H15 H 0.1542 0.1739 0.1464 0.033 Uiso 1 1 calc R . . C16 C 0.2207(4) 0.3216(4) 0.14222(15) 0.0304(9) Uani 1 1 d . . . H16 H 0.1692 0.3388 0.1097 0.036 Uiso 1 1 calc R . . C17 C 0.3053(4) 0.3935(3) 0.16762(15) 0.0346(10) Uani 1 1 d . . . H17 H 0.3135 0.4599 0.1521 0.042 Uiso 1 1 calc R . . C18 C 0.3791(4) 0.3699(4) 0.21585(14) 0.0311(8) Uani 1 1 d . . . H18 H 0.4367 0.4204 0.2331 0.037 Uiso 1 1 calc R . . C21 C 0.2734(3) 0.4142(3) 0.35569(14) 0.0194(7) Uani 1 1 d . . . C22 C 0.1419(3) 0.3917(3) 0.32448(14) 0.0223(8) Uani 1 1 d . . . H22 H 0.1305 0.3364 0.2994 0.027 Uiso 1 1 calc R . . C23 C 0.0408(4) 0.4610(4) 0.33675(15) 0.0282(9) Uani 1 1 d . . . H23 H -0.0535 0.461 0.3225 0.034 Uiso 1 1 calc R . . C24 C 0.0998(4) 0.5375(3) 0.37615(14) 0.0248(8) Uani 1 1 d . . . C25 C 0.2383(3) 0.5060(3) 0.38744(14) 0.0213(8) Uani 1 1 d . . . C26 C 0.0484(4) 0.6269(4) 0.39980(15) 0.0288(9) Uani 1 1 d . . . H26 H -0.0456 0.6503 0.3925 0.035 Uiso 1 1 calc R . . C27 C 0.1398(4) 0.6815(3) 0.43469(15) 0.0283(8) Uani 1 1 d . A . C28 C 0.2777(4) 0.6492(3) 0.44747(14) 0.0271(8) Uani 1 1 d . . . H28 H 0.3364 0.6873 0.4719 0.033 Uiso 1 1 calc R . . C29 C 0.3267(4) 0.5585(3) 0.42289(14) 0.0238(8) Uani 1 1 d . . . O30 O 0.4575(2) 0.5147(2) 0.42904(11) 0.0250(6) Uani 1 1 d . . . C31 C 0.5464(4) 0.5417(4) 0.47697(15) 0.0293(9) Uani 1 1 d . . . H31 H 0.5532 0.6179 0.4794 0.035 Uiso 1 1 calc R . . C32 C 0.6924(4) 0.4988(4) 0.46531(18) 0.0413(12) Uani 1 1 d . . . H32A H 0.6879 0.4239 0.4652 0.062 Uiso 1 1 calc R . . H32B H 0.7589 0.5216 0.494 0.062 Uiso 1 1 calc R . . H32C H 0.7253 0.5229 0.4291 0.062 Uiso 1 1 calc R . . C33 C 0.4793(5) 0.5018(4) 0.52894(16) 0.0397(11) Uani 1 1 d . . . H33A H 0.383 0.5299 0.5326 0.06 Uiso 1 1 calc R . . H33B H 0.5368 0.5224 0.5609 0.06 Uiso 1 1 calc R . . H33C H 0.4743 0.427 0.5273 0.06 Uiso 1 1 calc R . . O34 O 0.1036(3) 0.7762(2) 0.45657(12) 0.0386(7) Uani 1 1 d . . . C35A C -0.0371(4) 0.7844(4) 0.48028(19) 0.0418(8) Uani 0.5 1 d P A 1 H35A H -0.1124 0.7481 0.4586 0.05 Uiso 0.5 1 calc PR A 1 C36A C -0.0638(4) 0.8986(4) 0.48668(18) 0.0418(8) Uani 0.5 1 d P A 1 H36A H -0.0791 0.9292 0.4502 0.063 Uiso 0.5 1 calc PR A 1 H36B H 0.0189 0.9306 0.5043 0.063 Uiso 0.5 1 calc PR A 1 H36C H -0.1484 0.9095 0.5097 0.063 Uiso 0.5 1 calc PR A 1 C37A C -0.0145(10) 0.7401(10) 0.5393(4) 0.0418(8) Uani 0.5 1 d P A 1 H37A H 0.0029 0.6664 0.5369 0.063 Uiso 0.5 1 calc PR A 1 H37B H -0.0997 0.7526 0.5617 0.063 Uiso 0.5 1 calc PR A 1 H37C H 0.0677 0.7735 0.5566 0.063 Uiso 0.5 1 calc PR A 1 C35B C -0.0371(4) 0.7844(4) 0.48028(19) 0.0418(8) Uani 0.5 1 d P A 2 H35B H -0.1049 0.76 0.4512 0.05 Uiso 0.5 1 calc PR A 2 C36B C -0.0638(4) 0.8986(4) 0.48668(18) 0.0418(8) Uani 0.5 1 d P A 2 H36D H -0.0457 0.933 0.4514 0.063 Uiso 0.5 1 calc PR A 2 H36E H 0.0001 0.9263 0.515 0.063 Uiso 0.5 1 calc PR A 2 H36F H -0.1629 0.91 0.4978 0.063 Uiso 0.5 1 calc PR A 2 C37B C -0.0620(9) 0.7209(9) 0.5284(4) 0.0418(8) Uani 0.5 1 d P A 2 H37D H -0.0414 0.6495 0.5192 0.063 Uiso 0.5 1 calc PR A 2 H37E H -0.1617 0.7273 0.5398 0.063 Uiso 0.5 1 calc PR A 2 H37F H 0.0002 0.7431 0.5586 0.063 Uiso 0.5 1 calc PR A 2 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 0.02119(12) 0.01492(15) 0.01728(11) -0.00016(13) -0.00119(8) -0.00049(16) Cl1 0.0501(5) 0.0223(6) 0.0208(4) 0.0052(4) -0.0044(4) -0.0012(5) Cl2 0.0285(4) 0.0232(5) 0.0282(4) 0.0021(4) 0.0019(3) -0.0069(4) P1 0.0197(4) 0.0137(5) 0.0177(4) 0.0000(4) 0.0001(3) -0.0006(4) C1 0.0264(16) 0.0151(19) 0.0189(15) 0.0015(15) -0.0023(12) -0.0038(15) C2 0.0242(16) 0.026(2) 0.0252(17) 0.0018(17) 0.0004(13) -0.0005(17) C3 0.0257(17) 0.034(3) 0.035(2) 0.0078(19) 0.0032(15) -0.0068(19) C4 0.038(2) 0.020(2) 0.042(2) 0.0039(19) -0.0061(17) -0.0115(19) C5 0.043(2) 0.018(2) 0.039(2) 0.0004(18) -0.0030(18) -0.0001(19) C6 0.0346(18) 0.019(2) 0.0268(19) 0.0002(17) 0.0016(14) -0.0036(17) C7 0.0233(15) 0.0151(19) 0.0241(16) -0.0025(15) 0.0023(13) -0.0046(15) C8 0.0286(17) 0.034(2) 0.0240(17) -0.0039(17) -0.0017(14) 0.0001(18) C9 0.0266(17) 0.035(3) 0.042(2) -0.004(2) -0.0072(16) 0.0011(19) C10 0.0201(15) 0.027(3) 0.054(3) -0.007(2) 0.0071(16) 0.0001(17) C11 0.0323(18) 0.034(3) 0.034(2) -0.0120(19) 0.0106(15) -0.0053(19) C12 0.0335(18) 0.024(2) 0.0243(17) -0.0086(17) -0.0003(14) -0.0031(18) C13 0.0220(14) 0.021(2) 0.0143(14) -0.0019(15) 0.0017(12) -0.0007(15) C14 0.0228(15) 0.019(2) 0.0254(17) 0.0008(16) 0.0012(13) 0.0010(16) C15 0.0279(17) 0.031(2) 0.0234(17) -0.0028(17) -0.0053(14) -0.0028(18) C16 0.0363(19) 0.031(3) 0.0239(17) 0.0005(17) -0.0034(15) 0.0048(19) C17 0.051(2) 0.025(3) 0.0279(17) 0.0086(17) -0.0054(17) 0.001(2) C18 0.0417(18) 0.025(2) 0.0269(16) 0.004(2) -0.0029(14) -0.008(2) C21 0.0214(15) 0.0171(19) 0.0195(14) 0.0015(14) 0.0010(12) 0.0007(15) C22 0.0234(14) 0.019(2) 0.0247(15) 0.0013(15) -0.0022(12) -0.0022(15) C23 0.0276(18) 0.032(3) 0.0247(18) 0.0031(18) 0.0012(13) 0.0012(19) C24 0.0260(16) 0.027(2) 0.0213(16) 0.0046(16) 0.0011(13) -0.0016(17) C25 0.0269(16) 0.019(2) 0.0180(15) 0.0016(14) 0.0040(13) 0.0050(15) C26 0.0272(17) 0.035(3) 0.0246(18) 0.0022(18) 0.0059(14) 0.0106(17) C27 0.0386(19) 0.017(2) 0.0295(18) -0.0022(17) 0.0129(15) -0.0025(18) C28 0.0364(19) 0.023(2) 0.0218(16) -0.0023(17) 0.0039(14) -0.0030(18) C29 0.0315(17) 0.022(2) 0.0181(15) 0.0005(15) 0.0040(13) 0.0008(17) O30 0.0275(13) 0.0240(18) 0.0234(14) -0.0063(13) -0.0048(9) 0.0042(12) C31 0.040(2) 0.023(2) 0.0256(18) -0.0061(17) -0.0112(15) -0.0042(18) C32 0.0332(19) 0.052(3) 0.039(2) -0.011(2) -0.0115(17) 0.005(2) C33 0.049(2) 0.046(3) 0.0242(19) -0.003(2) -0.0059(17) -0.002(2) O34 0.0374(14) 0.0309(18) 0.0476(17) -0.0076(16) 0.0143(12) 0.0017(14) C35A 0.0389(14) 0.048(2) 0.0387(14) -0.0073(14) 0.0076(11) 0.0069(15) C36A 0.0389(14) 0.048(2) 0.0387(14) -0.0073(14) 0.0076(11) 0.0069(15) C37A 0.0389(14) 0.048(2) 0.0387(14) -0.0073(14) 0.0076(11) 0.0069(15) C35B 0.0389(14) 0.048(2) 0.0387(14) -0.0073(14) 0.0076(11) 0.0069(15) C36B 0.0389(14) 0.048(2) 0.0387(14) -0.0073(14) 0.0076(11) 0.0069(15) C37B 0.0389(14) 0.048(2) 0.0387(14) -0.0073(14) 0.0076(11) 0.0069(15) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C21 1.850(3) . ? Ru1 P1 2.2308(10) . ? Ru1 Cl1 2.3047(10) . ? Ru1 Cl2 2.3115(9) . ? Ru1 O30 2.407(3) . ? P1 C7 1.820(4) . ? P1 C1 1.826(4) . ? P1 C13 1.837(3) . ? C1 C6 1.386(6) . ? C1 C2 1.400(5) . ? C2 C3 1.369(6) . ? C2 H2 0.95 . ? C3 C4 1.390(6) . ? C3 H3 0.95 . ? C4 C5 1.409(6) . ? C4 H4 0.95 . ? C5 C6 1.379(6) . ? C5 H5 0.95 . ? C6 H6 0.95 . ? C7 C12 1.384(5) . ? C7 C8 1.407(5) . ? C8 C9 1.370(5) . ? C8 H8 0.95 . ? C9 C10 1.360(6) . ? C9 H9 0.95 . ? C10 C11 1.384(6) . ? C10 H10 0.95 . ? C11 C12 1.395(5) . ? C11 H11 0.95 . ? C12 H12 0.95 . ? C13 C18 1.382(6) . ? C13 C14 1.390(5) . ? C14 C15 1.398(5) . ? C14 H14 0.95 . ? C15 C16 1.382(6) . ? C15 H15 0.95 . ? C16 C17 1.375(6) . ? C16 H16 0.95 . ? C17 C18 1.391(5) . ? C17 H17 0.95 . ? C18 H18 0.95 . ? C21 C25 1.463(5) . ? C21 C22 1.476(4) . ? C22 C23 1.346(5) . ? C22 H22 0.95 . ? C23 C24 1.489(6) . ? C23 H23 0.95 . ? C24 C26 1.388(6) . ? C24 C25 1.391(5) . ? C25 C29 1.376(5) . ? C26 C27 1.399(6) . ? C26 H26 0.95 . ? C27 O34 1.389(5) . ? C27 C28 1.396(5) . ? C28 C29 1.405(5) . ? C28 H28 0.95 . ? C29 O30 1.364(4) . ? O30 C31 1.471(4) . ? C31 C33 1.500(5) . ? C31 C32 1.508(5) . ? C31 H31 1 . ? C32 H32A 0.98 . ? C32 H32B 0.98 . ? C32 H32C 0.98 . ? C33 H33A 0.98 . ? C33 H33B 0.98 . ? C33 H33C 0.98 . ? O34 C35A 1.445(5) . ? C35A C36A 1.523(8) . ? C35A C37A 1.555(11) . ? C35A H35A 1 . ? C36A H36A 0.98 . ? C36A H36B 0.98 . ? C36A H36C 0.98 . ? C37A H37A 0.98 . ? C37A H37B 0.98 . ? C37A H37C 0.98 . ? C37B H37D 0.98 . ? C37B H37E 0.98 . ? C37B H37F 0.98 . ? 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 C21 Ru1 P1 97.01(12) . . ? C21 Ru1 Cl1 105.24(11) . . ? P1 Ru1 Cl1 95.30(4) . . ? C21 Ru1 Cl2 108.86(11) . . ? P1 Ru1 Cl2 91.25(3) . . ? Cl1 Ru1 Cl2 144.16(4) . . ? C21 Ru1 O30 81.26(13) . . ? P1 Ru1 O30 175.51(7) . . ? Cl1 Ru1 O30 89.16(8) . . ? Cl2 Ru1 O30 85.42(7) . . ? C7 P1 C1 102.55(17) . . ? C7 P1 C13 106.45(15) . . ? C1 P1 C13 103.27(16) . . ? C7 P1 Ru1 108.69(12) . . ? C1 P1 Ru1 118.22(12) . . ? C13 P1 Ru1 116.27(13) . . ? C6 C1 C2 118.2(4) . . ? C6 C1 P1 121.9(3) . . ? C2 C1 P1 119.7(3) . . ? C3 C2 C1 121.1(4) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C2 C3 C4 120.6(4) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C3 C4 C5 119.0(4) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? C6 C5 C4 119.5(4) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? C5 C6 C1 121.6(3) . . ? C5 C6 H6 119.2 . . ? C1 C6 H6 119.2 . . ? C12 C7 C8 119.3(3) . . ? C12 C7 P1 123.3(3) . . ? C8 C7 P1 117.4(3) . . ? C9 C8 C7 119.9(3) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C10 C9 C8 120.9(4) . . ? C10 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? C9 C10 C11 120.3(4) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C10 C11 C12 120.0(4) . . ? C10 C11 H11 120 . . ? C12 C11 H11 120 . . ? C7 C12 C11 119.6(3) . . ? C7 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C18 C13 C14 118.9(3) . . ? C18 C13 P1 120.1(3) . . ? C14 C13 P1 120.9(3) . . ? C13 C14 C15 120.6(4) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C16 C15 C14 119.7(4) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C17 C16 C15 119.7(3) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C16 C17 C18 120.7(4) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C13 C18 C17 120.3(4) . . ? C13 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C25 C21 C22 104.1(3) . . ? C25 C21 Ru1 112.7(2) . . ? C22 C21 Ru1 143.1(3) . . ? C23 C22 C21 110.1(3) . . ? C23 C22 H22 125 . . ? C21 C22 H22 125 . . ? C22 C23 C24 109.4(3) . . ? C22 C23 H23 125.3 . . ? C24 C23 H23 125.3 . . ? C26 C24 C25 119.6(4) . . ? C26 C24 C23 134.5(3) . . ? C25 C24 C23 105.9(3) . . ? C29 C25 C24 122.6(4) . . ? C29 C25 C21 126.9(3) . . ? C24 C25 C21 110.5(3) . . ? C24 C26 C27 117.7(3) . . ? C24 C26 H26 121.1 . . ? C27 C26 H26 121.1 . . ? O34 C27 C28 114.3(3) . . ? O34 C27 C26 122.3(4) . . ? C28 C27 C26 123.2(4) . . ? C27 C28 C29 117.7(4) . . ? C27 C28 H28 121.1 . . ? C29 C28 H28 121.1 . . ? O30 C29 C25 113.7(3) . . ? O30 C29 C28 127.1(3) . . ? C25 C29 C28 119.2(3) . . ? C29 O30 C31 119.7(3) . . ? C29 O30 Ru1 105.3(2) . . ? C31 O30 Ru1 132.5(2) . . ? O30 C31 C33 109.8(3) . . ? O30 C31 C32 106.1(3) . . ? C33 C31 C32 114.1(4) . . ? O30 C31 H31 108.9 . . ? C33 C31 H31 108.9 . . ? C32 C31 H31 108.9 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C27 O34 C35A 116.2(3) . . ? O34 C35A C36A 105.3(4) . . ? O34 C35A C37A 102.2(4) . . ? C36A C35A C37A 107.1(6) . . ? O34 C35A H35A 113.7 . . ? C36A C35A H35A 113.7 . . ? C37A C35A H35A 113.7 . . ? C35A C36A H36A 109.5 . . ? C35A C36A H36B 109.5 . . ? H36A C36A H36B 109.5 . . ? C35A C36A H36C 109.5 . . ? H36A C36A H36C 109.5 . . ? H36B C36A H36C 109.5 . . ? C35A C37A H37A 109.5 . . ? C35A C37A H37B 109.5 . . ? H37A C37A H37B 109.5 . . ? C35A C37A H37C 109.5 . . ? H37A C37A H37C 109.5 . . ? H37B C37A H37C 109.5 . . ? H37D C37B H37E 109.5 . . ? H37D C37B H37F 109.5 . . ? H37E C37B H37F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C21 Ru1 P1 C7 160.80(17) . . . . ? Cl1 Ru1 P1 C7 -93.10(13) . . . . ? Cl2 Ru1 P1 C7 51.63(13) . . . . ? C21 Ru1 P1 C1 -82.97(16) . . . . ? Cl1 Ru1 P1 C1 23.13(13) . . . . ? Cl2 Ru1 P1 C1 167.85(13) . . . . ? C21 Ru1 P1 C13 40.76(16) . . . . ? Cl1 Ru1 P1 C13 146.87(12) . . . . ? Cl2 Ru1 P1 C13 -68.41(12) . . . . ? C7 P1 C1 C6 -20.8(3) . . . . ? C13 P1 C1 C6 89.8(3) . . . . ? Ru1 P1 C1 C6 -140.2(3) . . . . ? C7 P1 C1 C2 163.2(3) . . . . ? C13 P1 C1 C2 -86.3(3) . . . . ? Ru1 P1 C1 C2 43.7(3) . . . . ? C6 C1 C2 C3 0.9(5) . . . . ? P1 C1 C2 C3 177.1(3) . . . . ? C1 C2 C3 C4 -1.2(6) . . . . ? C2 C3 C4 C5 0.3(6) . . . . ? C3 C4 C5 C6 0.8(6) . . . . ? C4 C5 C6 C1 -1.2(6) . . . . ? C2 C1 C6 C5 0.3(5) . . . . ? P1 C1 C6 C5 -175.8(3) . . . . ? C1 P1 C7 C12 98.8(4) . . . . ? C13 P1 C7 C12 -9.3(4) . . . . ? Ru1 P1 C7 C12 -135.2(3) . . . . ? C1 P1 C7 C8 -80.9(3) . . . . ? C13 P1 C7 C8 171.0(3) . . . . ? Ru1 P1 C7 C8 45.1(3) . . . . ? C12 C7 C8 C9 -1.8(6) . . . . ? P1 C7 C8 C9 177.9(4) . . . . ? C7 C8 C9 C10 0.6(7) . . . . ? C8 C9 C10 C11 -0.2(7) . . . . ? C9 C10 C11 C12 1.0(7) . . . . ? C8 C7 C12 C11 2.6(6) . . . . ? P1 C7 C12 C11 -177.1(3) . . . . ? C10 C11 C12 C7 -2.2(7) . . . . ? C7 P1 C13 C18 -84.4(3) . . . . ? C1 P1 C13 C18 168.0(3) . . . . ? Ru1 P1 C13 C18 36.9(3) . . . . ? C7 P1 C13 C14 98.8(3) . . . . ? C1 P1 C13 C14 -8.8(3) . . . . ? Ru1 P1 C13 C14 -139.9(2) . . . . ? C18 C13 C14 C15 -0.8(5) . . . . ? P1 C13 C14 C15 176.0(3) . . . . ? C13 C14 C15 C16 -0.1(5) . . . . ? C14 C15 C16 C17 1.2(6) . . . . ? C15 C16 C17 C18 -1.3(6) . . . . ? C14 C13 C18 C17 0.7(5) . . . . ? P1 C13 C18 C17 -176.2(3) . . . . ? C16 C17 C18 C13 0.4(6) . . . . ? P1 Ru1 C21 C25 -174.5(2) . . . . ? Cl1 Ru1 C21 C25 88.0(3) . . . . ? Cl2 Ru1 C21 C25 -80.7(2) . . . . ? O30 Ru1 C21 C25 1.3(2) . . . . ? P1 Ru1 C21 C22 4.3(4) . . . . ? Cl1 Ru1 C21 C22 -93.2(4) . . . . ? Cl2 Ru1 C21 C22 98.0(4) . . . . ? O30 Ru1 C21 C22 -179.9(5) . . . . ? C25 C21 C22 C23 -0.7(4) . . . . ? Ru1 C21 C22 C23 -179.5(4) . . . . ? C21 C22 C23 C24 1.8(4) . . . . ? C22 C23 C24 C26 175.5(4) . . . . ? C22 C23 C24 C25 -2.3(4) . . . . ? C26 C24 C25 C29 2.2(6) . . . . ? C23 C24 C25 C29 -179.7(3) . . . . ? C26 C24 C25 C21 -176.4(3) . . . . ? C23 C24 C25 C21 1.8(4) . . . . ? C22 C21 C25 C29 -179.2(3) . . . . ? Ru1 C21 C25 C29 0.0(5) . . . . ? C22 C21 C25 C24 -0.8(4) . . . . ? Ru1 C21 C25 C24 178.5(3) . . . . ? C25 C24 C26 C27 -0.4(5) . . . . ? C23 C24 C26 C27 -178.0(4) . . . . ? C24 C26 C27 O34 174.3(3) . . . . ? C24 C26 C27 C28 -1.3(6) . . . . ? O34 C27 C28 C29 -174.6(3) . . . . ? C26 C27 C28 C29 1.3(6) . . . . ? C24 C25 C29 O30 179.2(3) . . . . ? C21 C25 C29 O30 -2.5(5) . . . . ? C24 C25 C29 C28 -2.1(6) . . . . ? C21 C25 C29 C28 176.1(3) . . . . ? C27 C28 C29 O30 178.9(3) . . . . ? C27 C28 C29 C25 0.4(5) . . . . ? C25 C29 O30 C31 -161.3(3) . . . . ? C28 C29 O30 C31 20.1(5) . . . . ? C25 C29 O30 Ru1 3.0(3) . . . . ? C28 C29 O30 Ru1 -175.5(3) . . . . ? C21 Ru1 O30 C29 -2.6(2) . . . . ? Cl1 Ru1 O30 C29 -108.1(2) . . . . ? Cl2 Ru1 O30 C29 107.3(2) . . . . ? C21 Ru1 O30 C31 158.9(3) . . . . ? Cl1 Ru1 O30 C31 53.3(3) . . . . ? Cl2 Ru1 O30 C31 -91.2(3) . . . . ? C29 O30 C31 C33 67.8(5) . . . . ? Ru1 O30 C31 C33 -91.5(4) . . . . ? C29 O30 C31 C32 -168.4(3) . . . . ? Ru1 O30 C31 C32 32.3(5) . . . . ? C28 C27 O34 C35A -137.3(4) . . . . ? C26 C27 O34 C35A 46.8(5) . . . . ? C27 O34 C35A C36A -165.3(4) . . . . ? C27 O34 C35A C37A 82.9(6) . . . . ? # Attachment '[CuCl(PPh3)]4.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2010-09-17 at 14:29:44 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : d:\progs\wingx\files\archive.dat # CIF files read : job struct data_job2 _database_code_depnum_ccdc_archive 'CCDC 856297' #TrackingRef '[CuCl(PPh3)]4.cif' _audit_creation_date 2010-09-17T14:29:44-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C72 H60 Cl4 Cu4 P4' _chemical_formula_sum 'C72 H60 Cl4 Cu4 P4' _chemical_formula_weight 1445.04 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c n b' _symmetry_space_group_name_Hall '-P 2b 2ac' _symmetry_Int_Tables_number 60 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' 'x+1/2, -y, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, y-1/2, -z' '-x-1/2, y, z-1/2' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.3658(5) _cell_length_b 18.0515(6) _cell_length_c 20.3269(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6372.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5016 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 27.38 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_diffrn 1.506 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2944 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.628 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.606 _exptl_absorpt_correction_T_max 0.809 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_unetI/netI 0.0333 _diffrn_reflns_number 31033 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 7302 _reflns_number_gt 6008 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SAINT (Bruker, 2002)' _computing_cell_refinement 'Bruker SMART (Bruker, 2002)' _computing_data_reduction 'Bruker SAINT (Bruker, 2002)' _computing_structure_solution 'SIR97 (Altomare et al., 1999))' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 1999), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0375P)^2^+2.6211P] 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_number_reflns 7302 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0407 _refine_ls_R_factor_gt 0.03 _refine_ls_wR_factor_ref 0.0778 _refine_ls_wR_factor_gt 0.073 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.44 _refine_diff_density_min -0.375 _refine_diff_density_rms 0.066 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' Cu Cu 0.3201 1.2651 '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' 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 Cu1 Cu 0.592606(13) 0.218820(15) 0.436930(12) 0.02532(7) Uani 1 1 d . . . Cl3 Cl 0.58960(2) 0.20659(3) 0.31545(2) 0.01917(10) Uani 1 1 d . . . P1 P 0.70448(3) 0.18901(3) 0.47920(2) 0.01962(11) Uani 1 1 d . . . C1 C 0.78748(11) 0.22711(12) 0.43510(10) 0.0238(4) Uani 1 1 d . . . C2 C 0.78923(13) 0.22134(15) 0.36664(11) 0.0357(6) Uani 1 1 d . . . H2 H 0.7481 0.1975 0.3442 0.043 Uiso 1 1 calc R . . C3 C 0.85045(14) 0.25006(18) 0.33110(12) 0.0471(7) Uani 1 1 d . . . H3 H 0.8517 0.2449 0.2846 0.057 Uiso 1 1 calc R . . C4 C 0.90992(14) 0.28630(16) 0.36320(14) 0.0460(7) Uani 1 1 d . . . H4 H 0.9513 0.3069 0.3388 0.055 Uiso 1 1 calc R . . C5 C 0.90864(13) 0.29223(15) 0.43033(14) 0.0415(6) Uani 1 1 d . . . H5 H 0.9494 0.3172 0.4523 0.05 Uiso 1 1 calc R . . C6 C 0.84844(12) 0.26225(13) 0.46685(12) 0.0310(5) Uani 1 1 d . . . H6 H 0.8489 0.2658 0.5135 0.037 Uiso 1 1 calc R . . C11 C 0.72390(11) 0.08998(11) 0.48194(9) 0.0212(4) Uani 1 1 d . . . C12 C 0.79326(12) 0.05789(12) 0.46281(10) 0.0269(4) Uani 1 1 d . . . H12 H 0.8319 0.0874 0.4426 0.032 Uiso 1 1 calc R . . C13 C 0.80598(14) -0.01717(13) 0.47321(11) 0.0340(5) Uani 1 1 d . . . H13 H 0.8531 -0.0391 0.4596 0.041 Uiso 1 1 calc R . . C14 C 0.75070(15) -0.05958(13) 0.50304(12) 0.0388(6) Uani 1 1 d . . . H14 H 0.7602 -0.1106 0.5112 0.047 Uiso 1 1 calc R . . C15 C 0.68068(15) -0.02824(14) 0.52151(12) 0.0384(6) Uani 1 1 d . . . H15 H 0.6423 -0.0579 0.5419 0.046 Uiso 1 1 calc R . . C16 C 0.66706(13) 0.04596(13) 0.51018(10) 0.0299(5) Uani 1 1 d . . . H16 H 0.6188 0.067 0.5217 0.036 Uiso 1 1 calc R . . C21 C 0.72448(11) 0.21598(11) 0.56395(9) 0.0217(4) Uani 1 1 d . . . C22 C 0.77189(13) 0.17408(13) 0.60515(10) 0.0312(5) Uani 1 1 d . . . H22 H 0.7905 0.1273 0.5909 0.037 Uiso 1 1 calc R . . C23 C 0.79190(14) 0.20072(14) 0.66695(11) 0.0340(5) Uani 1 1 d . . . H23 H 0.8243 0.1722 0.6948 0.041 Uiso 1 1 calc R . . C24 C 0.76464(13) 0.26884(13) 0.68803(11) 0.0332(5) Uani 1 1 d . . . H24 H 0.7795 0.2875 0.7298 0.04 Uiso 1 1 calc R . . C25 C 0.71601(14) 0.30953(13) 0.64849(11) 0.0315(5) Uani 1 1 d . . . H25 H 0.6965 0.3557 0.6635 0.038 Uiso 1 1 calc R . . C26 C 0.69537(12) 0.28307(12) 0.58652(10) 0.0256(4) Uani 1 1 d . . . H26 H 0.6613 0.311 0.5596 0.031 Uiso 1 1 calc R . . Cu2 Cu 0.548714(15) 0.329955(14) 0.328052(12) 0.02457(7) Uani 1 1 d . . . Cl4 Cl 0.53266(3) 0.33816(3) 0.44693(2) 0.02040(10) Uani 1 1 d . . . P2 P 0.58279(3) 0.43001(3) 0.27441(2) 0.01851(11) Uani 1 1 d . . . C51 C 0.55015(11) 0.51572(11) 0.31396(9) 0.0214(4) Uani 1 1 d . . . C52 C 0.48924(12) 0.51147(11) 0.35790(10) 0.0240(4) Uani 1 1 d . . . H52 H 0.4653 0.4651 0.3662 0.029 Uiso 1 1 calc R . . C53 C 0.46302(13) 0.57433(13) 0.38976(11) 0.0310(5) Uani 1 1 d . . . H53 H 0.4209 0.5709 0.4194 0.037 Uiso 1 1 calc R . . C54 C 0.49772(14) 0.64197(12) 0.37869(10) 0.0318(5) Uani 1 1 d . . . H54 H 0.4795 0.685 0.4007 0.038 Uiso 1 1 calc R . . C55 C 0.55907(14) 0.64695(13) 0.33549(12) 0.0355(5) Uani 1 1 d . . . H55 H 0.5832 0.6934 0.3279 0.043 Uiso 1 1 calc R . . C56 C 0.58526(13) 0.58411(12) 0.30327(11) 0.0322(5) Uani 1 1 d . . . H56 H 0.6274 0.5877 0.2737 0.039 Uiso 1 1 calc R . . C61 C 0.54048(11) 0.43200(11) 0.19194(9) 0.0215(4) Uani 1 1 d . . . C62 C 0.51770(13) 0.49689(13) 0.16023(10) 0.0308(5) Uani 1 1 d . . . H62 H 0.5254 0.5435 0.1809 0.037 Uiso 1 1 calc R . . C63 C 0.48380(14) 0.49353(16) 0.09853(11) 0.0399(6) Uani 1 1 d . . . H63 H 0.4684 0.5379 0.0771 0.048 Uiso 1 1 calc R . . C64 C 0.47231(14) 0.42620(17) 0.06822(12) 0.0426(6) Uani 1 1 d . . . H64 H 0.4489 0.4242 0.026 0.051 Uiso 1 1 calc R . . C65 C 0.49468(17) 0.36185(16) 0.09886(12) 0.0473(7) Uani 1 1 d . . . H65 H 0.487 0.3155 0.0777 0.057 Uiso 1 1 calc R . . C66 C 0.52862(14) 0.36474(14) 0.16104(11) 0.0343(5) Uani 1 1 d . . . H66 H 0.5437 0.3202 0.1823 0.041 Uiso 1 1 calc R . . C71 C 0.68426(11) 0.45087(11) 0.26105(9) 0.0205(4) Uani 1 1 d . . . C72 C 0.71167(12) 0.48971(12) 0.20706(10) 0.0254(4) Uani 1 1 d . . . H72 H 0.6779 0.5004 0.1715 0.03 Uiso 1 1 calc R . . C73 C 0.78776(12) 0.51318(13) 0.20424(11) 0.0325(5) Uani 1 1 d . . . H73 H 0.8059 0.5396 0.1669 0.039 Uiso 1 1 calc R . . C74 C 0.83657(13) 0.49817(15) 0.25555(12) 0.0397(6) Uani 1 1 d . . . H74 H 0.888 0.516 0.2546 0.048 Uiso 1 1 calc R . . C75 C 0.81078(13) 0.45686(16) 0.30895(12) 0.0425(6) Uani 1 1 d . . . H75 H 0.8451 0.4451 0.3438 0.051 Uiso 1 1 calc R . . C76 C 0.73501(13) 0.43275(13) 0.31139(11) 0.0313(5) Uani 1 1 d . . . H76 H 0.7178 0.4038 0.3475 0.038 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 Cu1 0.01755(13) 0.03256(15) 0.02584(13) 0.00158(11) -0.00432(10) 0.00485(11) Cl3 0.0167(2) 0.0221(2) 0.0187(2) -0.00149(18) 0.00218(16) 0.00081(18) P1 0.0164(2) 0.0229(3) 0.0196(2) -0.0007(2) -0.00218(19) 0.0031(2) C1 0.0185(9) 0.0252(10) 0.0276(10) 0.0032(8) -0.0005(8) 0.0048(8) C2 0.0235(11) 0.0536(16) 0.0302(11) 0.0061(11) -0.0019(9) -0.0006(11) C3 0.0297(13) 0.078(2) 0.0335(13) 0.0146(13) 0.0068(10) 0.0027(13) C4 0.0250(12) 0.0531(17) 0.0600(17) 0.0211(14) 0.0092(11) -0.0003(11) C5 0.0252(12) 0.0378(14) 0.0615(17) 0.0003(12) -0.0005(11) -0.0081(10) C6 0.0256(11) 0.0295(12) 0.0380(12) -0.0022(10) -0.0011(9) 0.0010(9) C11 0.0213(9) 0.0238(10) 0.0184(9) -0.0024(8) -0.0047(7) 0.0028(8) C12 0.0261(10) 0.0304(11) 0.0242(10) -0.0007(9) -0.0016(8) 0.0027(9) C13 0.0373(13) 0.0305(12) 0.0342(12) -0.0067(10) -0.0080(10) 0.0132(10) C14 0.0533(15) 0.0219(11) 0.0412(13) -0.0022(10) -0.0178(12) 0.0025(11) C15 0.0411(14) 0.0317(13) 0.0424(13) 0.0069(11) -0.0090(11) -0.0125(11) C16 0.0250(10) 0.0323(12) 0.0324(11) -0.0021(9) -0.0028(9) -0.0018(9) C21 0.0197(9) 0.0244(10) 0.0211(9) -0.0014(8) -0.0016(8) 0.0006(8) C22 0.0364(12) 0.0290(12) 0.0282(11) -0.0056(9) -0.0087(9) 0.0088(10) C23 0.0396(13) 0.0372(13) 0.0252(11) -0.0020(10) -0.0132(10) 0.0059(11) C24 0.0379(12) 0.0369(13) 0.0248(11) -0.0078(10) -0.0020(9) -0.0072(10) C25 0.0373(12) 0.0250(11) 0.0322(11) -0.0073(9) 0.0042(10) -0.0016(10) C26 0.0244(10) 0.0241(11) 0.0282(10) 0.0006(9) 0.0024(8) 0.0022(9) Cu2 0.02762(14) 0.02071(13) 0.02537(14) 0.00362(10) 0.00314(10) -0.00385(10) Cl4 0.0202(2) 0.0214(2) 0.0196(2) -0.00273(17) -0.00138(17) -0.00099(18) P2 0.0189(2) 0.0175(2) 0.0191(2) 0.00024(19) 0.00275(19) -0.00112(19) C51 0.0218(10) 0.0202(10) 0.0221(9) -0.0009(8) 0.0010(8) -0.0012(8) C52 0.0229(10) 0.0227(10) 0.0264(10) 0.0030(8) 0.0040(8) 0.0003(8) C53 0.0315(12) 0.0321(12) 0.0295(11) 0.0013(9) 0.0113(9) 0.0058(10) C54 0.0385(12) 0.0258(11) 0.0310(11) -0.0061(9) 0.0065(10) 0.0060(10) C55 0.0426(14) 0.0206(11) 0.0433(13) -0.0040(10) 0.0095(11) -0.0068(10) C56 0.0345(12) 0.0244(11) 0.0375(12) -0.0041(9) 0.0163(10) -0.0070(9) C61 0.0168(9) 0.0264(10) 0.0214(9) 0.0014(8) 0.0022(7) 0.0006(8) C62 0.0326(12) 0.0328(12) 0.0271(10) 0.0049(9) 0.0055(9) 0.0080(10) C63 0.0352(13) 0.0553(16) 0.0292(11) 0.0138(11) 0.0030(10) 0.0181(12) C64 0.0314(12) 0.0713(19) 0.0251(11) 0.0038(12) -0.0070(10) -0.0021(13) C65 0.0586(17) 0.0498(16) 0.0335(13) -0.0074(12) -0.0125(13) -0.0133(14) C66 0.0431(13) 0.0316(12) 0.0282(11) -0.0005(10) -0.0077(10) -0.0047(11) C71 0.0185(9) 0.0200(9) 0.0231(9) -0.0031(8) 0.0042(8) 0.0009(8) C72 0.0218(10) 0.0289(11) 0.0254(10) 0.0009(9) 0.0017(8) 0.0017(9) C73 0.0229(11) 0.0376(13) 0.0371(12) 0.0033(10) 0.0105(9) -0.0044(10) C74 0.0198(11) 0.0536(16) 0.0457(14) -0.0018(12) 0.0023(10) -0.0068(11) C75 0.0242(11) 0.0621(18) 0.0412(13) 0.0054(13) -0.0093(10) -0.0003(12) C76 0.0270(11) 0.0379(13) 0.0289(11) 0.0050(10) -0.0011(9) 0.0018(10) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Cu1 P1 2.1913(5) . ? Cu1 Cl4 2.4012(5) . ? Cu1 Cl4 2.4148(5) 2_655 ? Cu1 Cl3 2.4798(5) . ? Cl3 Cu2 2.3515(5) . ? Cl3 Cu2 2.5040(5) 2_655 ? P1 C11 1.820(2) . ? P1 C21 1.824(2) . ? P1 C1 1.831(2) . ? C1 C6 1.393(3) . ? C1 C2 1.396(3) . ? C2 C3 1.386(3) . ? C2 H2 0.95 . ? C3 C4 1.386(4) . ? C3 H3 0.95 . ? C4 C5 1.369(4) . ? C4 H4 0.95 . ? C5 C6 1.392(3) . ? C5 H5 0.95 . ? C6 H6 0.95 . ? C11 C16 1.391(3) . ? C11 C12 1.392(3) . ? C12 C13 1.389(3) . ? C12 H12 0.95 . ? C13 C14 1.369(4) . ? C13 H13 0.95 . ? C14 C15 1.393(4) . ? C14 H14 0.95 . ? C15 C16 1.380(3) . ? C15 H15 0.95 . ? C16 H16 0.95 . ? C21 C26 1.390(3) . ? C21 C22 1.397(3) . ? C22 C23 1.389(3) . ? C22 H22 0.95 . ? C23 C24 1.386(3) . ? C23 H23 0.95 . ? C24 C25 1.378(3) . ? C24 H24 0.95 . ? C25 C26 1.394(3) . ? C25 H25 0.95 . ? C26 H26 0.95 . ? Cu2 P2 2.1911(5) . ? Cu2 Cl4 2.4369(5) . ? Cu2 Cl3 2.5040(5) 2_655 ? Cl4 Cu1 2.4147(5) 2_655 ? P2 C71 1.8222(19) . ? P2 C61 1.831(2) . ? P2 C51 1.833(2) . ? C51 C52 1.387(3) . ? C51 C56 1.394(3) . ? C52 C53 1.384(3) . ? C52 H52 0.95 . ? C53 C54 1.380(3) . ? C53 H53 0.95 . ? C54 C55 1.384(3) . ? C54 H54 0.95 . ? C55 C56 1.387(3) . ? C55 H55 0.95 . ? C56 H56 0.95 . ? C61 C66 1.382(3) . ? C61 C62 1.394(3) . ? C62 C63 1.387(3) . ? C62 H62 0.95 . ? C63 C64 1.377(4) . ? C63 H63 0.95 . ? C64 C65 1.374(4) . ? C64 H64 0.95 . ? C65 C66 1.396(3) . ? C65 H65 0.95 . ? C66 H66 0.95 . ? C71 C72 1.387(3) . ? C71 C76 1.390(3) . ? C72 C73 1.389(3) . ? C72 H72 0.95 . ? C73 C74 1.371(3) . ? C73 H73 0.95 . ? C74 C75 1.391(3) . ? C74 H74 0.95 . ? C75 C76 1.387(3) . ? C75 H75 0.95 . ? C76 H76 0.95 . ? 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 P1 Cu1 Cl4 124.85(2) . . ? P1 Cu1 Cl4 131.38(2) . 2_655 ? Cl4 Cu1 Cl4 89.109(18) . 2_655 ? P1 Cu1 Cl3 112.781(19) . . ? Cl4 Cu1 Cl3 98.920(18) . . ? Cl4 Cu1 Cl3 91.544(17) 2_655 . ? Cu2 Cl3 Cu1 79.252(16) . . ? Cu2 Cl3 Cu2 87.060(17) . 2_655 ? Cu1 Cl3 Cu2 86.662(16) . 2_655 ? C11 P1 C21 101.42(9) . . ? C11 P1 C1 103.76(9) . . ? C21 P1 C1 102.25(9) . . ? C11 P1 Cu1 114.68(6) . . ? C21 P1 Cu1 118.28(7) . . ? C1 P1 Cu1 114.44(7) . . ? C6 C1 C2 118.6(2) . . ? C6 C1 P1 122.86(16) . . ? C2 C1 P1 118.50(16) . . ? C3 C2 C1 120.6(2) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C4 C3 C2 120.2(2) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C5 C4 C3 119.6(2) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 120.9(2) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C5 C6 C1 120.1(2) . . ? C5 C6 H6 120 . . ? C1 C6 H6 120 . . ? C16 C11 C12 119.4(2) . . ? C16 C11 P1 116.24(15) . . ? C12 C11 P1 124.10(16) . . ? C13 C12 C11 120.1(2) . . ? C13 C12 H12 120 . . ? C11 C12 H12 120 . . ? C14 C13 C12 120.1(2) . . ? C14 C13 H13 120 . . ? C12 C13 H13 120 . . ? C13 C14 C15 120.3(2) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C16 C15 C14 119.9(2) . . ? C16 C15 H15 120 . . ? C14 C15 H15 120 . . ? C15 C16 C11 120.1(2) . . ? C15 C16 H16 119.9 . . ? C11 C16 H16 119.9 . . ? C26 C21 C22 119.22(19) . . ? C26 C21 P1 118.36(15) . . ? C22 C21 P1 122.29(16) . . ? C23 C22 C21 120.1(2) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C24 C23 C22 120.1(2) . . ? C24 C23 H23 120 . . ? C22 C23 H23 120 . . ? C25 C24 C23 120.1(2) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C26 120.1(2) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C21 C26 C25 120.2(2) . . ? C21 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? P2 Cu2 Cl3 130.16(2) . . ? P2 Cu2 Cl4 118.31(2) . . ? Cl3 Cu2 Cl4 101.546(18) . . ? P2 Cu2 Cl3 115.17(2) . 2_655 ? Cl3 Cu2 Cl3 91.661(17) . 2_655 ? Cl4 Cu2 Cl3 90.443(17) . 2_655 ? Cu1 Cl4 Cu1 90.074(18) . 2_655 ? Cu1 Cl4 Cu2 79.161(16) . . ? Cu1 Cl4 Cu2 89.640(17) 2_655 . ? C71 P2 C61 104.33(9) . . ? C71 P2 C51 100.95(9) . . ? C61 P2 C51 105.12(9) . . ? C71 P2 Cu2 120.38(7) . . ? C61 P2 Cu2 111.31(7) . . ? C51 P2 Cu2 113.20(7) . . ? C52 C51 C56 118.89(19) . . ? C52 C51 P2 118.13(15) . . ? C56 C51 P2 122.95(15) . . ? C53 C52 C51 120.5(2) . . ? C53 C52 H52 119.8 . . ? C51 C52 H52 119.8 . . ? C54 C53 C52 120.4(2) . . ? C54 C53 H53 119.8 . . ? C52 C53 H53 119.8 . . ? C53 C54 C55 119.8(2) . . ? C53 C54 H54 120.1 . . ? C55 C54 H54 120.1 . . ? C54 C55 C56 119.9(2) . . ? C54 C55 H55 120 . . ? C56 C55 H55 120 . . ? C55 C56 C51 120.5(2) . . ? C55 C56 H56 119.8 . . ? C51 C56 H56 119.8 . . ? C66 C61 C62 119.05(19) . . ? C66 C61 P2 117.30(16) . . ? C62 C61 P2 123.62(17) . . ? C63 C62 C61 120.1(2) . . ? C63 C62 H62 119.9 . . ? C61 C62 H62 119.9 . . ? C64 C63 C62 120.3(2) . . ? C64 C63 H63 119.8 . . ? C62 C63 H63 119.8 . . ? C65 C64 C63 120.2(2) . . ? C65 C64 H64 119.9 . . ? C63 C64 H64 119.9 . . ? C64 C65 C66 119.9(2) . . ? C64 C65 H65 120.1 . . ? C66 C65 H65 120.1 . . ? C61 C66 C65 120.5(2) . . ? C61 C66 H66 119.8 . . ? C65 C66 H66 119.8 . . ? C72 C71 C76 118.95(18) . . ? C72 C71 P2 123.68(15) . . ? C76 C71 P2 117.06(15) . . ? C71 C72 C73 120.9(2) . . ? C71 C72 H72 119.5 . . ? C73 C72 H72 119.5 . . ? C74 C73 C72 119.8(2) . . ? C74 C73 H73 120.1 . . ? C72 C73 H73 120.1 . . ? C73 C74 C75 120.0(2) . . ? C73 C74 H74 120 . . ? C75 C74 H74 120 . . ? C76 C75 C74 120.1(2) . . ? C76 C75 H75 119.9 . . ? C74 C75 H75 119.9 . . ? C75 C76 C71 120.1(2) . . ? C75 C76 H76 119.9 . . ? C71 C76 H76 119.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Cu1 Cl3 Cu2 -125.79(2) . . . . ? Cl4 Cu1 Cl3 Cu2 8.103(18) . . . . ? Cl4 Cu1 Cl3 Cu2 97.443(17) 2_655 . . . ? P1 Cu1 Cl3 Cu2 146.57(2) . . . 2_655 ? Cl4 Cu1 Cl3 Cu2 -79.534(18) . . . 2_655 ? Cl4 Cu1 Cl3 Cu2 9.806(17) 2_655 . . 2_655 ? Cl4 Cu1 P1 C11 165.02(7) . . . . ? Cl4 Cu1 P1 C11 38.99(8) 2_655 . . . ? Cl3 Cu1 P1 C11 -75.15(7) . . . . ? Cl4 Cu1 P1 C21 45.39(8) . . . . ? Cl4 Cu1 P1 C21 -80.64(8) 2_655 . . . ? Cl3 Cu1 P1 C21 165.22(8) . . . . ? Cl4 Cu1 P1 C1 -75.22(8) . . . . ? Cl4 Cu1 P1 C1 158.75(8) 2_655 . . . ? Cl3 Cu1 P1 C1 44.61(8) . . . . ? C11 P1 C1 C6 -101.54(19) . . . . ? C21 P1 C1 C6 3.6(2) . . . . ? Cu1 P1 C1 C6 132.77(16) . . . . ? C11 P1 C1 C2 79.18(19) . . . . ? C21 P1 C1 C2 -175.65(18) . . . . ? Cu1 P1 C1 C2 -46.51(19) . . . . ? C6 C1 C2 C3 0.0(4) . . . . ? P1 C1 C2 C3 179.3(2) . . . . ? C1 C2 C3 C4 -1.4(4) . . . . ? C2 C3 C4 C5 1.3(4) . . . . ? C3 C4 C5 C6 0.1(4) . . . . ? C4 C5 C6 C1 -1.5(4) . . . . ? C2 C1 C6 C5 1.4(3) . . . . ? P1 C1 C6 C5 -177.84(18) . . . . ? C21 P1 C11 C16 77.54(16) . . . . ? C1 P1 C11 C16 -176.66(15) . . . . ? Cu1 P1 C11 C16 -51.12(17) . . . . ? C21 P1 C11 C12 -97.02(18) . . . . ? C1 P1 C11 C12 8.79(19) . . . . ? Cu1 P1 C11 C12 134.33(15) . . . . ? C16 C11 C12 C13 -1.4(3) . . . . ? P1 C11 C12 C13 173.03(16) . . . . ? C11 C12 C13 C14 -0.8(3) . . . . ? C12 C13 C14 C15 1.7(3) . . . . ? C13 C14 C15 C16 -0.5(4) . . . . ? C14 C15 C16 C11 -1.7(3) . . . . ? C12 C11 C16 C15 2.6(3) . . . . ? P1 C11 C16 C15 -172.21(17) . . . . ? C11 P1 C21 C26 -161.69(16) . . . . ? C1 P1 C21 C26 91.32(17) . . . . ? Cu1 P1 C21 C26 -35.38(19) . . . . ? C11 P1 C21 C22 22.6(2) . . . . ? C1 P1 C21 C22 -84.41(19) . . . . ? Cu1 P1 C21 C22 148.90(16) . . . . ? C26 C21 C22 C23 -2.4(3) . . . . ? P1 C21 C22 C23 173.27(18) . . . . ? C21 C22 C23 C24 0.3(4) . . . . ? C22 C23 C24 C25 1.7(4) . . . . ? C23 C24 C25 C26 -1.4(4) . . . . ? C22 C21 C26 C25 2.7(3) . . . . ? P1 C21 C26 C25 -173.16(16) . . . . ? C24 C25 C26 C21 -0.8(3) . . . . ? Cu1 Cl3 Cu2 P2 135.62(2) . . . . ? Cu2 Cl3 Cu2 P2 -137.22(2) 2_655 . . . ? Cu1 Cl3 Cu2 Cl4 -8.051(17) . . . . ? Cu2 Cl3 Cu2 Cl4 79.107(18) 2_655 . . . ? Cu1 Cl3 Cu2 Cl3 -98.842(16) . . . 2_655 ? Cu2 Cl3 Cu2 Cl3 -11.69(2) 2_655 . . 2_655 ? P1 Cu1 Cl4 Cu1 -152.261(19) . . . 2_655 ? Cl4 Cu1 Cl4 Cu1 -9.62(2) 2_655 . . 2_655 ? Cl3 Cu1 Cl4 Cu1 81.800(18) . . . 2_655 ? P1 Cu1 Cl4 Cu2 118.12(2) . . . . ? Cl4 Cu1 Cl4 Cu2 -99.243(16) 2_655 . . . ? Cl3 Cu1 Cl4 Cu2 -7.820(17) . . . . ? P2 Cu2 Cl4 Cu1 -140.74(2) . . . . ? Cl3 Cu2 Cl4 Cu1 8.318(18) . . . . ? Cl3 Cu2 Cl4 Cu1 100.104(17) 2_655 . . . ? P2 Cu2 Cl4 Cu1 129.12(2) . . . 2_655 ? Cl3 Cu2 Cl4 Cu1 -81.826(19) . . . 2_655 ? Cl3 Cu2 Cl4 Cu1 9.960(18) 2_655 . . 2_655 ? Cl3 Cu2 P2 C71 -48.30(8) . . . . ? Cl4 Cu2 P2 C71 90.46(7) . . . . ? Cl3 Cu2 P2 C71 -164.31(7) 2_655 . . . ? Cl3 Cu2 P2 C61 74.16(7) . . . . ? Cl4 Cu2 P2 C61 -147.09(7) . . . . ? Cl3 Cu2 P2 C61 -41.85(7) 2_655 . . . ? Cl3 Cu2 P2 C51 -167.69(7) . . . . ? Cl4 Cu2 P2 C51 -28.93(7) . . . . ? Cl3 Cu2 P2 C51 76.30(7) 2_655 . . . ? C71 P2 C51 C52 -150.77(16) . . . . ? C61 P2 C51 C52 100.96(17) . . . . ? Cu2 P2 C51 C52 -20.73(18) . . . . ? C71 P2 C51 C56 27.2(2) . . . . ? C61 P2 C51 C56 -81.0(2) . . . . ? Cu2 P2 C51 C56 157.28(17) . . . . ? C56 C51 C52 C53 1.0(3) . . . . ? P2 C51 C52 C53 179.14(16) . . . . ? C51 C52 C53 C54 -0.7(3) . . . . ? C52 C53 C54 C55 0.0(4) . . . . ? C53 C54 C55 C56 0.3(4) . . . . ? C54 C55 C56 C51 0.1(4) . . . . ? C52 C51 C56 C55 -0.8(3) . . . . ? P2 C51 C56 C55 -178.75(19) . . . . ? C71 P2 C61 C66 99.66(18) . . . . ? C51 P2 C61 C66 -154.56(17) . . . . ? Cu2 P2 C61 C66 -31.64(18) . . . . ? C71 P2 C61 C62 -82.51(18) . . . . ? C51 P2 C61 C62 23.28(19) . . . . ? Cu2 P2 C61 C62 146.20(16) . . . . ? C66 C61 C62 C63 -0.1(3) . . . . ? P2 C61 C62 C63 -177.92(17) . . . . ? C61 C62 C63 C64 0.1(3) . . . . ? C62 C63 C64 C65 -0.3(4) . . . . ? C63 C64 C65 C66 0.5(4) . . . . ? C62 C61 C66 C65 0.3(3) . . . . ? P2 C61 C66 C65 178.3(2) . . . . ? C64 C65 C66 C61 -0.5(4) . . . . ? C61 P2 C71 C72 24.42(19) . . . . ? C51 P2 C71 C72 -84.46(18) . . . . ? Cu2 P2 C71 C72 150.19(15) . . . . ? C61 P2 C71 C76 -162.06(17) . . . . ? C51 P2 C71 C76 89.06(18) . . . . ? Cu2 P2 C71 C76 -36.29(19) . . . . ? C76 C71 C72 C73 -2.8(3) . . . . ? P2 C71 C72 C73 170.59(17) . . . . ? C71 C72 C73 C74 -0.3(3) . . . . ? C72 C73 C74 C75 2.7(4) . . . . ? C73 C74 C75 C76 -2.0(4) . . . . ? C74 C75 C76 C71 -1.1(4) . . . . ? C72 C71 C76 C75 3.5(3) . . . . ? P2 C71 C76 C75 -170.35(19) . . . . ? # Attachment 'complex 10.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2010-09-29 at 15:38:02 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : d:\progs\wingx\files\archive.dat # CIF files read : sq struct data_sq _database_code_depnum_ccdc_archive 'CCDC 856298' #TrackingRef 'complex 10.cif' _audit_creation_date 2010-09-29T15:38:02-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C39 H37.50 Cl2 O2 P Ru' _chemical_formula_sum 'C39 H37.50 Cl2 O2 P Ru' _chemical_formula_weight 741.13 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3991(8) _cell_length_b 14.0465(12) _cell_length_c 16.2657(15) _cell_angle_alpha 104.160(4) _cell_angle_beta 95.607(4) _cell_angle_gamma 108.807(4) _cell_volume 1934.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9964 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 27.23 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.16 _exptl_crystal_density_diffrn 1.273 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 761 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.614 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.593 _exptl_absorpt_correction_T_max 0.906 #----------------------------------------------------------------------------# # SQUEEZE RESULTS # #----------------------------------------------------------------------------# # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.210 0.318 0.299 150 27 ' ' 2 -0.211 0.682 0.701 150 27 ' ' _platon_squeeze_details ; ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0602 _diffrn_reflns_av_unetI/netI 0.0701 _diffrn_reflns_number 28040 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.46 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.982 _diffrn_measured_fraction_theta_max 0.968 _reflns_number_total 8582 _reflns_number_gt 6621 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SAINT (Bruker, 2002)' _computing_cell_refinement 'Bruker SMART (Bruker, 2002)' _computing_data_reduction 'Bruker SAINT (Bruker, 2002)' _computing_structure_solution 'SIR97 (Altomare et al., 1999))' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 1999), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0974P)^2^+5.1602P] 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_number_reflns 8582 _refine_ls_number_parameters 329 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0832 _refine_ls_R_factor_gt 0.0664 _refine_ls_wR_factor_ref 0.194 _refine_ls_wR_factor_gt 0.1843 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.294 _refine_diff_density_min -1.481 _refine_diff_density_rms 0.128 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.63140(4) 0.30877(3) 0.82086(2) 0.02622(14) Uani 1 1 d . A . Cl1 Cl 0.37691(14) 0.28977(9) 0.81675(8) 0.0343(3) Uani 1 1 d . . . Cl2 Cl 0.85661(15) 0.41074(10) 0.79265(8) 0.0369(3) Uani 1 1 d . . . P3 P 0.58433(14) 0.18207(10) 0.69793(7) 0.0276(3) Uani 1 1 d . . . C1 C 0.4826(14) 0.0460(9) 0.6944(7) 0.0441(4) Uani 0.5 1 d P A 1 C2A C 0.3498(7) 0.0283(5) 0.7370(3) 0.0441(4) Uani 0.5 1 d P A 1 H2A H 0.3154 0.083 0.7632 0.053 Uiso 0.5 1 calc PR A 1 C3A C 0.2789(15) -0.0758(9) 0.7353(7) 0.0441(4) Uani 0.5 1 d P A 1 H3A H 0.1946 -0.0925 0.7637 0.053 Uiso 0.5 1 calc PR A 1 C4 C 0.3254(14) -0.1580(10) 0.6936(7) 0.0441(4) Uani 0.5 1 d P A 1 H4 H 0.2721 -0.2279 0.6942 0.053 Uiso 0.5 1 calc PR A 1 C5 C 0.4470(14) -0.1377(10) 0.6523(7) 0.0441(4) Uani 0.5 1 d P A 1 H5 H 0.4773 -0.1934 0.6235 0.053 Uiso 0.5 1 calc PR A 1 C6 C 0.5261(14) -0.0349(9) 0.6526(7) 0.0441(4) Uani 0.5 1 d P A 1 H6 H 0.6104 -0.0205 0.6239 0.053 Uiso 0.5 1 calc PR A 1 C13 C 0.7554(14) 0.1725(10) 0.6494(7) 0.0441(4) Uani 0.5 1 d P A 1 C11A C 0.8786(7) 0.1714(5) 0.7056(4) 0.0441(4) Uani 0.5 1 d P A 1 H11A H 0.8765 0.1762 0.7647 0.053 Uiso 0.5 1 calc PR A 1 C10A C 1.0083(15) 0.1626(10) 0.6677(7) 0.0441(4) Uani 0.5 1 d P A 1 H10A H 1.0955 0.1631 0.7029 0.053 Uiso 0.5 1 calc PR A 1 C16 C 1.0075(14) 0.1536(9) 0.5831(7) 0.0441(4) Uani 0.5 1 d P A 1 H16 H 1.0917 0.1438 0.559 0.053 Uiso 0.5 1 calc PR A 1 C15 C 0.8882(14) 0.1583(9) 0.5317(7) 0.0441(4) Uani 0.5 1 d P A 1 H15 H 0.8932 0.1562 0.4732 0.053 Uiso 0.5 1 calc PR A 1 C14 C 0.7616(14) 0.1660(9) 0.5630(7) 0.0441(4) Uani 0.5 1 d P A 1 H14 H 0.6777 0.1669 0.526 0.053 Uiso 0.5 1 calc PR A 1 C23 C 0.4695(15) 0.2028(10) 0.6094(7) 0.0441(4) Uani 0.5 1 d P A 1 C21A C 0.4972(7) 0.2903(5) 0.5980(4) 0.0441(4) Uani 0.5 1 d P A 1 H21A H 0.5665 0.3466 0.6446 0.053 Uiso 0.5 1 calc PR A 1 C20A C 0.4462(7) 0.3213(5) 0.5302(3) 0.0441(4) Uani 0.5 1 d P A 1 H20A H 0.4955 0.3853 0.5177 0.053 Uiso 0.5 1 calc PR A 1 C26 C 0.2997(14) 0.2366(9) 0.4801(7) 0.0441(4) Uani 0.5 1 d P A 1 H26 H 0.2398 0.2493 0.4363 0.053 Uiso 0.5 1 calc PR A 1 C25 C 0.2503(14) 0.1415(9) 0.4958(7) 0.0441(4) Uani 0.5 1 d P A 1 H25 H 0.1576 0.0881 0.4626 0.053 Uiso 0.5 1 calc PR A 1 C24 C 0.3358(14) 0.1233(10) 0.5601(7) 0.0441(4) Uani 0.5 1 d P A 1 H24 H 0.3034 0.0566 0.5705 0.053 Uiso 0.5 1 calc PR A 1 C30 C 0.3974(15) 0.0721(10) 0.6754(7) 0.0441(4) Uani 0.5 1 d P A 2 H30 H 0.488 0.1328 0.6893 0.053 Uiso 0.5 1 calc PR A 2 C27 C 0.3144(14) 0.0289(9) 0.5907(7) 0.0441(4) Uani 0.5 1 d P A 2 H27 H 0.3505 0.0587 0.5468 0.053 Uiso 0.5 1 calc PR A 2 C28 C 0.1798(14) -0.0573(9) 0.5706(7) 0.0441(4) Uani 0.5 1 d P A 2 H28 H 0.1238 -0.0864 0.5128 0.053 Uiso 0.5 1 calc PR A 2 C29 C 0.1272(14) -0.1003(10) 0.6324(7) 0.0441(4) Uani 0.5 1 d P A 2 H29 H 0.0356 -0.1602 0.6183 0.053 Uiso 0.5 1 calc PR A 2 C3B C 0.2109(15) -0.0548(9) 0.7190(7) 0.0441(4) Uani 0.5 1 d P A 2 H3B H 0.172 -0.081 0.764 0.053 Uiso 0.5 1 calc PR A 2 C2B C 0.3498(7) 0.0283(5) 0.7370(3) 0.0441(4) Uani 0.5 1 d P A 2 H2B H 0.4114 0.0542 0.7932 0.053 Uiso 0.5 1 calc PR A 2 C12 C 0.7179(14) 0.1119(10) 0.6833(7) 0.0441(4) Uani 0.5 1 d P A 2 C7 C 0.6696(15) 0.0038(10) 0.6484(7) 0.0441(4) Uani 0.5 1 d P A 2 H7 H 0.5631 -0.0367 0.6332 0.053 Uiso 0.5 1 calc PR A 2 C8 C 0.7728(14) -0.0452(10) 0.6355(7) 0.0441(4) Uani 0.5 1 d P A 2 H8 H 0.737 -0.1192 0.6101 0.053 Uiso 0.5 1 calc PR A 2 C9 C 0.9267(14) 0.0103(9) 0.6584(7) 0.0441(4) Uani 0.5 1 d P A 2 H9 H 0.9971 -0.025 0.6494 0.053 Uiso 0.5 1 calc PR A 2 C10B C 0.9811(15) 0.1211(10) 0.6958(7) 0.0441(4) Uani 0.5 1 d P A 2 H10B H 1.0879 0.1599 0.7139 0.053 Uiso 0.5 1 calc PR A 2 C11B C 0.8786(7) 0.1714(5) 0.7056(4) 0.0441(4) Uani 0.5 1 d P A 2 H11B H 0.9141 0.2459 0.7272 0.053 Uiso 0.5 1 calc PR A 2 C22B C 0.5725(15) 0.2370(10) 0.6094(7) 0.0441(4) Uani 0.5 1 d P A 2 C17 C 0.6722(14) 0.2319(9) 0.5497(7) 0.0441(4) Uani 0.5 1 d P A 2 H17 H 0.7464 0.2001 0.5554 0.053 Uiso 0.5 1 calc PR A 2 C18 C 0.6570(14) 0.2759(9) 0.4814(7) 0.0441(4) Uani 0.5 1 d P A 2 H18 H 0.7216 0.2733 0.4401 0.053 Uiso 0.5 1 calc PR A 2 C19 C 0.5531(14) 0.3209(9) 0.4742(7) 0.0441(4) Uani 0.5 1 d P A 2 H19 H 0.5505 0.354 0.4299 0.053 Uiso 0.5 1 calc PR A 2 C20B C 0.4462(7) 0.3213(5) 0.5302(3) 0.0441(4) Uani 0.5 1 d P A 2 H20B H 0.3576 0.3393 0.5225 0.053 Uiso 0.5 1 calc PR A 2 C21B C 0.4972(7) 0.2903(5) 0.5980(4) 0.0441(4) Uani 0.5 1 d P A 2 H21B H 0.465 0.3177 0.6493 0.053 Uiso 0.5 1 calc PR A 2 O41 O 0.6858(4) 0.4406(2) 0.95952(19) 0.0238(6) Uani 1 1 d . . . C42 C 0.7246(6) 0.5551(3) 0.9849(3) 0.0296(10) Uani 1 1 d . A . H42 H 0.6815 0.5769 1.0372 0.035 Uiso 1 1 calc R . . C43 C 0.8964(6) 0.6110(4) 1.0047(3) 0.0364(11) Uani 1 1 d . . . H43A H 0.9422 0.5887 1.0499 0.055 Uiso 1 1 calc R A . H43B H 0.9207 0.6872 1.0248 0.055 Uiso 1 1 calc R . . H43C H 0.9377 0.5934 0.9524 0.055 Uiso 1 1 calc R . . C44 C 0.6442(7) 0.5743(4) 0.9086(4) 0.0401(12) Uani 1 1 d . . . H44A H 0.6812 0.5482 0.8565 0.06 Uiso 1 1 calc R A . H44B H 0.666 0.6499 0.9198 0.06 Uiso 1 1 calc R . . H44C H 0.5335 0.5372 0.9001 0.06 Uiso 1 1 calc R . . C51 C 0.6802(6) 0.2355(3) 0.8926(3) 0.0284(10) Uani 1 1 d . . . C52 C 0.6921(6) 0.1338(4) 0.8913(3) 0.0324(11) Uani 1 1 d . A . H52 H 0.6743 0.0774 0.8406 0.039 Uiso 1 1 calc R . . C53 C 0.7325(6) 0.1318(4) 0.9736(3) 0.0319(11) Uani 1 1 d . . . C54A C 0.7529(9) 0.0423(5) 1.0006(5) 0.0606(10) Uani 0.5 1 d P A 1 C55A C 0.6479(9) -0.0561(5) 0.9676(5) 0.0606(10) Uani 0.5 1 d P A 1 H55A H 0.5646 -0.0773 0.9209 0.073 Uiso 0.5 1 calc PR A 1 C56A C 0.686(2) -0.1323(11) 1.0197(12) 0.0606(10) Uani 0.5 1 d P A 1 H56A H 0.6103 -0.1995 1.0123 0.073 Uiso 0.5 1 calc PR A 1 C57A C 0.826(2) -0.1017(13) 1.0753(11) 0.0606(10) Uani 0.5 1 d P A 1 H57A H 0.8475 -0.1517 1.0997 0.073 Uiso 0.5 1 calc PR A 1 C58A C 0.931(2) -0.0046(11) 1.0956(11) 0.0606(10) Uani 0.5 1 d P A 1 H58A H 1.03 0.0163 1.13 0.073 Uiso 0.5 1 calc PR A 1 C59A C 0.8813(9) 0.0610(5) 1.0613(5) 0.0606(10) Uani 0.5 1 d P A 1 H59A H 0.9463 0.1329 1.0829 0.073 Uiso 0.5 1 calc PR A 1 C54B C 0.7529(9) 0.0423(5) 1.0006(5) 0.0606(10) Uani 0.5 1 d P A 2 C55B C 0.6479(9) -0.0561(5) 0.9676(5) 0.0606(10) Uani 0.5 1 d P A 2 H55B H 0.557 -0.0583 0.9348 0.073 Uiso 0.5 1 calc PR A 2 C56B C 0.644(2) -0.1497(11) 0.9710(11) 0.0606(10) Uani 0.5 1 d P A 2 H56B H 0.5749 -0.2151 0.9334 0.073 Uiso 0.5 1 calc PR A 2 C57B C 0.762(2) -0.1363(11) 1.0414(11) 0.0606(10) Uani 0.5 1 d P A 2 H57B H 0.7643 -0.1949 1.0601 0.073 Uiso 0.5 1 calc PR A 2 C58B C 0.869(2) -0.0408(12) 1.0803(11) 0.0606(10) Uani 0.5 1 d P A 2 H58B H 0.9455 -0.0368 1.1251 0.073 Uiso 0.5 1 calc PR A 2 C59B C 0.8813(9) 0.0610(5) 1.0613(5) 0.0606(10) Uani 0.5 1 d P A 2 H59B H 0.9628 0.1267 1.0864 0.073 Uiso 0.5 1 calc PR A 2 C60 C 0.7507(6) 0.2341(4) 1.0347(3) 0.0275(10) Uani 1 1 d . A . C61 C 0.7187(5) 0.2938(3) 0.9841(3) 0.0255(9) Uani 1 1 d . A . C62 C 0.7222(5) 0.3945(3) 1.0201(3) 0.0245(9) Uani 1 1 d . A . C63 C 0.7587(5) 0.4380(3) 1.1104(3) 0.0269(9) Uani 1 1 d . . . H63 H 0.7619 0.5072 1.1366 0.032 Uiso 1 1 calc R A . C64 C 0.7898(6) 0.3772(4) 1.1599(3) 0.0301(10) Uani 1 1 d . A . C65 C 0.7868(6) 0.2745(4) 1.1235(3) 0.0303(10) Uani 1 1 d . . . H65 H 0.8088 0.2345 1.1589 0.036 Uiso 1 1 calc R A . O66 O 0.8308(5) 0.4124(3) 1.2487(2) 0.0376(8) Uani 1 1 d . . . C67 C 0.8063(8) 0.5052(5) 1.2953(3) 0.0481(15) Uani 1 1 d . A . H67 H 0.8404 0.5608 1.2657 0.058 Uiso 1 1 calc R . . C68 C 0.6396(10) 0.4789(8) 1.2972(5) 0.079(3) Uani 1 1 d . . . H68A H 0.5808 0.452 1.2379 0.119 Uiso 1 1 calc R A . H68B H 0.6221 0.5423 1.3278 0.119 Uiso 1 1 calc R . . H68C H 0.6064 0.4252 1.3271 0.119 Uiso 1 1 calc R . . C69 C 0.9053(11) 0.5414(6) 1.3834(4) 0.073(2) Uani 1 1 d . . . H69A H 0.8803 0.4839 1.4099 0.109 Uiso 1 1 calc R A . H69B H 0.8869 0.6015 1.4197 0.109 Uiso 1 1 calc R . . H69C H 1.0133 0.5625 1.3782 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 Ru1 0.0305(2) 0.0205(2) 0.0215(2) 0.00150(13) 0.00292(14) 0.00514(15) Cl1 0.0319(6) 0.0304(6) 0.0332(6) 0.0008(5) 0.0051(5) 0.0082(5) Cl2 0.0362(7) 0.0321(6) 0.0328(6) 0.0067(5) 0.0070(5) 0.0017(5) P3 0.0283(6) 0.0279(6) 0.0202(5) 0.0000(4) 0.0020(4) 0.0076(5) C1 0.0492(11) 0.0449(10) 0.0346(8) 0.0040(7) 0.0059(7) 0.0184(8) C2A 0.0492(11) 0.0449(10) 0.0346(8) 0.0040(7) 0.0059(7) 0.0184(8) C3A 0.0492(11) 0.0449(10) 0.0346(8) 0.0040(7) 0.0059(7) 0.0184(8) C4 0.0492(11) 0.0449(10) 0.0346(8) 0.0040(7) 0.0059(7) 0.0184(8) C5 0.0492(11) 0.0449(10) 0.0346(8) 0.0040(7) 0.0059(7) 0.0184(8) C6 0.0492(11) 0.0449(10) 0.0346(8) 0.0040(7) 0.0059(7) 0.0184(8) C13 0.0492(11) 0.0449(10) 0.0346(8) 0.0040(7) 0.0059(7) 0.0184(8) C11A 0.0492(11) 0.0449(10) 0.0346(8) 0.0040(7) 0.0059(7) 0.0184(8) C10A 0.0492(11) 0.0449(10) 0.0346(8) 0.0040(7) 0.0059(7) 0.0184(8) C16 0.0492(11) 0.0449(10) 0.0346(8) 0.0040(7) 0.0059(7) 0.0184(8) C15 0.0492(11) 0.0449(10) 0.0346(8) 0.0040(7) 0.0059(7) 0.0184(8) C14 0.0492(11) 0.0449(10) 0.0346(8) 0.0040(7) 0.0059(7) 0.0184(8) C23 0.0492(11) 0.0449(10) 0.0346(8) 0.0040(7) 0.0059(7) 0.0184(8) C21A 0.0492(11) 0.0449(10) 0.0346(8) 0.0040(7) 0.0059(7) 0.0184(8) C20A 0.0492(11) 0.0449(10) 0.0346(8) 0.0040(7) 0.0059(7) 0.0184(8) C26 0.0492(11) 0.0449(10) 0.0346(8) 0.0040(7) 0.0059(7) 0.0184(8) C25 0.0492(11) 0.0449(10) 0.0346(8) 0.0040(7) 0.0059(7) 0.0184(8) C24 0.0492(11) 0.0449(10) 0.0346(8) 0.0040(7) 0.0059(7) 0.0184(8) C30 0.0492(11) 0.0449(10) 0.0346(8) 0.0040(7) 0.0059(7) 0.0184(8) C27 0.0492(11) 0.0449(10) 0.0346(8) 0.0040(7) 0.0059(7) 0.0184(8) C28 0.0492(11) 0.0449(10) 0.0346(8) 0.0040(7) 0.0059(7) 0.0184(8) C29 0.0492(11) 0.0449(10) 0.0346(8) 0.0040(7) 0.0059(7) 0.0184(8) C3B 0.0492(11) 0.0449(10) 0.0346(8) 0.0040(7) 0.0059(7) 0.0184(8) C2B 0.0492(11) 0.0449(10) 0.0346(8) 0.0040(7) 0.0059(7) 0.0184(8) C12 0.0492(11) 0.0449(10) 0.0346(8) 0.0040(7) 0.0059(7) 0.0184(8) C7 0.0492(11) 0.0449(10) 0.0346(8) 0.0040(7) 0.0059(7) 0.0184(8) C8 0.0492(11) 0.0449(10) 0.0346(8) 0.0040(7) 0.0059(7) 0.0184(8) C9 0.0492(11) 0.0449(10) 0.0346(8) 0.0040(7) 0.0059(7) 0.0184(8) C10B 0.0492(11) 0.0449(10) 0.0346(8) 0.0040(7) 0.0059(7) 0.0184(8) C11B 0.0492(11) 0.0449(10) 0.0346(8) 0.0040(7) 0.0059(7) 0.0184(8) C22B 0.0492(11) 0.0449(10) 0.0346(8) 0.0040(7) 0.0059(7) 0.0184(8) C17 0.0492(11) 0.0449(10) 0.0346(8) 0.0040(7) 0.0059(7) 0.0184(8) C18 0.0492(11) 0.0449(10) 0.0346(8) 0.0040(7) 0.0059(7) 0.0184(8) C19 0.0492(11) 0.0449(10) 0.0346(8) 0.0040(7) 0.0059(7) 0.0184(8) C20B 0.0492(11) 0.0449(10) 0.0346(8) 0.0040(7) 0.0059(7) 0.0184(8) C21B 0.0492(11) 0.0449(10) 0.0346(8) 0.0040(7) 0.0059(7) 0.0184(8) O41 0.0300(17) 0.0140(14) 0.0249(15) 0.0046(11) 0.0014(12) 0.0066(12) C42 0.037(3) 0.016(2) 0.035(2) 0.0044(17) 0.009(2) 0.0103(19) C43 0.040(3) 0.021(2) 0.040(3) 0.0052(19) 0.004(2) 0.006(2) C44 0.043(3) 0.032(3) 0.049(3) 0.017(2) 0.007(2) 0.015(2) C51 0.032(3) 0.020(2) 0.025(2) -0.0011(17) 0.0067(18) 0.0045(19) C52 0.039(3) 0.016(2) 0.035(2) -0.0010(18) 0.010(2) 0.007(2) C53 0.041(3) 0.019(2) 0.038(3) 0.0074(18) 0.016(2) 0.012(2) C54A 0.086(3) 0.0417(17) 0.082(2) 0.0325(18) 0.049(2) 0.040(2) C55A 0.086(3) 0.0417(17) 0.082(2) 0.0325(18) 0.049(2) 0.040(2) C56A 0.086(3) 0.0417(17) 0.082(2) 0.0325(18) 0.049(2) 0.040(2) C57A 0.086(3) 0.0417(17) 0.082(2) 0.0325(18) 0.049(2) 0.040(2) C58A 0.086(3) 0.0417(17) 0.082(2) 0.0325(18) 0.049(2) 0.040(2) C59A 0.086(3) 0.0417(17) 0.082(2) 0.0325(18) 0.049(2) 0.040(2) C54B 0.086(3) 0.0417(17) 0.082(2) 0.0325(18) 0.049(2) 0.040(2) C55B 0.086(3) 0.0417(17) 0.082(2) 0.0325(18) 0.049(2) 0.040(2) C56B 0.086(3) 0.0417(17) 0.082(2) 0.0325(18) 0.049(2) 0.040(2) C57B 0.086(3) 0.0417(17) 0.082(2) 0.0325(18) 0.049(2) 0.040(2) C58B 0.086(3) 0.0417(17) 0.082(2) 0.0325(18) 0.049(2) 0.040(2) C59B 0.086(3) 0.0417(17) 0.082(2) 0.0325(18) 0.049(2) 0.040(2) C60 0.034(3) 0.022(2) 0.027(2) 0.0055(17) 0.0118(19) 0.0097(19) C61 0.028(2) 0.019(2) 0.024(2) 0.0017(16) 0.0077(17) 0.0046(18) C62 0.028(2) 0.020(2) 0.021(2) 0.0013(16) 0.0035(17) 0.0064(18) C63 0.034(3) 0.018(2) 0.026(2) 0.0011(16) 0.0057(18) 0.0088(19) C64 0.036(3) 0.032(2) 0.022(2) 0.0045(18) 0.0102(19) 0.013(2) C65 0.039(3) 0.029(2) 0.028(2) 0.0100(18) 0.011(2) 0.016(2) O66 0.053(2) 0.040(2) 0.0220(16) 0.0022(14) 0.0071(15) 0.0236(18) C67 0.080(5) 0.035(3) 0.027(3) 0.001(2) 0.017(3) 0.022(3) C68 0.098(7) 0.113(7) 0.061(4) 0.027(4) 0.036(4) 0.075(6) C69 0.112(7) 0.061(4) 0.030(3) 0.000(3) 0.013(3) 0.023(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C51 1.850(5) . ? Ru1 P3 2.2226(11) . ? Ru1 Cl2 2.3020(13) . ? Ru1 Cl1 2.3120(13) . ? Ru1 O41 2.428(3) . ? P3 C22B 1.802(12) . ? P3 C1 1.825(13) . ? P3 C12 1.830(12) . ? P3 C23 1.851(12) . ? P3 C30 1.858(13) . ? P3 C13 1.887(12) . ? C1 C6 1.376(16) . ? C1 C2A 1.467(13) . ? C2A C3A 1.390(14) . ? C2A H2A 0.95 . ? C3A C4 1.408(16) . ? C3A H3A 0.95 . ? C4 C5 1.369(17) . ? C4 H4 0.95 . ? C5 C6 1.393(17) . ? C5 H5 0.95 . ? C6 H6 0.95 . ? C13 C14 1.394(15) . ? C13 C11A 1.410(14) . ? C11A C10A 1.445(14) . ? C11A H11A 0.95 . ? C10A C16 1.350(16) . ? C10A H10A 0.95 . ? C16 C15 1.361(17) . ? C16 H16 0.95 . ? C15 C14 1.365(17) . ? C15 H15 0.95 . ? C14 H14 0.95 . ? C23 C21A 1.235(14) . ? C23 C24 1.389(17) . ? C21A C20A 1.379(8) . ? C21A H21A 0.95 . ? C20A C26 1.492(13) . ? C20A H20A 0.95 . ? C26 C25 1.362(17) . ? C26 H26 0.95 . ? C25 C24 1.380(16) . ? C25 H25 0.95 . ? C24 H24 0.95 . ? C30 C27 1.396(16) . ? C30 H30 0.95 . ? C27 C28 1.382(17) . ? C27 H27 0.95 . ? C28 C29 1.350(17) . ? C28 H28 0.95 . ? C29 C3B 1.425(16) . ? C29 H29 0.95 . ? C3B H3B 0.95 . ? C12 C7 1.384(17) . ? C7 C8 1.363(16) . ? C7 H7 0.95 . ? C8 C9 1.366(17) . ? C8 H8 0.95 . ? C9 C10B 1.420(17) . ? C9 H9 0.95 . ? C10B H10B 0.95 . ? C22B C17 1.419(17) . ? C17 C18 1.414(16) . ? C17 H17 0.95 . ? C18 C19 1.335(16) . ? C18 H18 0.95 . ? C19 H19 0.95 . ? O41 C62 1.378(5) . ? O41 C42 1.469(5) . ? C42 C43 1.512(7) . ? C42 C44 1.515(7) . ? C42 H42 1 . ? C43 H43A 0.98 . ? C43 H43B 0.98 . ? C43 H43C 0.98 . ? C44 H44A 0.98 . ? C44 H44B 0.98 . ? C44 H44C 0.98 . ? C51 C61 1.457(6) . ? C51 C52 1.463(7) . ? C52 C53 1.364(7) . ? C52 H52 0.95 . ? C53 C60 1.481(6) . ? C53 C54A 1.490(8) . ? C54A C55A 1.351(10) . ? C54A C59A 1.391(11) . ? C55A C56A 1.617(17) . ? C55A H55A 0.95 . ? C56A C57A 1.40(3) . ? C56A H56A 0.95 . ? C57A C58A 1.34(2) . ? C57A H57A 0.95 . ? C58A C59A 1.364(17) . ? C58A H58A 0.95 . ? C59A H59A 0.95 . ? C56B C57B 1.45(3) . ? C56B H56B 0.95 . ? C57B C58B 1.34(2) . ? C57B H57B 0.95 . ? C58B H58B 0.95 . ? C60 C65 1.380(6) . ? C60 C61 1.386(7) . ? C61 C62 1.380(6) . ? C62 C63 1.405(6) . ? C63 C64 1.385(7) . ? C63 H63 0.95 . ? C64 O66 1.378(5) . ? C64 C65 1.408(7) . ? C65 H65 0.95 . ? O66 C67 1.438(6) . ? C67 C68 1.495(11) . ? C67 C69 1.502(9) . ? C67 H67 1 . ? C68 H68A 0.98 . ? C68 H68B 0.98 . ? C68 H68C 0.98 . ? C69 H69A 0.98 . ? C69 H69B 0.98 . ? C69 H69C 0.98 . ? 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 C51 Ru1 P3 96.20(13) . . ? C51 Ru1 Cl2 107.69(15) . . ? P3 Ru1 Cl2 92.86(5) . . ? C51 Ru1 Cl1 107.97(15) . . ? P3 Ru1 Cl1 94.17(4) . . ? Cl2 Ru1 Cl1 142.60(5) . . ? C51 Ru1 O41 80.55(15) . . ? P3 Ru1 O41 176.75(8) . . ? Cl2 Ru1 O41 88.23(8) . . ? Cl1 Ru1 O41 86.81(8) . . ? C22B P3 C1 125.6(5) . . ? C22B P3 C12 108.3(5) . . ? C1 P3 C12 72.1(6) . . ? C1 P3 C23 104.2(6) . . ? C12 P3 C23 124.9(5) . . ? C22B P3 C30 104.0(6) . . ? C12 P3 C30 101.9(5) . . ? C23 P3 C30 76.6(6) . . ? C22B P3 C13 76.9(5) . . ? C1 P3 C13 102.1(5) . . ? C23 P3 C13 101.3(5) . . ? C30 P3 C13 124.6(5) . . ? C22B P3 Ru1 108.5(4) . . ? C1 P3 Ru1 119.1(3) . . ? C12 P3 Ru1 117.9(4) . . ? C23 P3 Ru1 111.4(3) . . ? C30 P3 Ru1 115.2(3) . . ? C13 P3 Ru1 116.6(4) . . ? C6 C1 C2A 122.4(11) . . ? C6 C1 P3 121.9(9) . . ? C2A C1 P3 115.7(7) . . ? C3A C2A C1 113.7(8) . . ? C3A C2A H2A 123.1 . . ? C1 C2A H2A 123.1 . . ? C2A C3A C4 123.5(11) . . ? C2A C3A H3A 118.2 . . ? C4 C3A H3A 118.2 . . ? C5 C4 C3A 120.3(12) . . ? C5 C4 H4 119.8 . . ? C3A C4 H4 119.8 . . ? C4 C5 C6 119.6(11) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C1 C6 C5 120.3(11) . . ? C1 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C14 C13 C11A 121.0(10) . . ? C14 C13 P3 122.8(9) . . ? C11A C13 P3 116.2(7) . . ? C13 C11A C10A 115.9(8) . . ? C13 C11A H11A 122.1 . . ? C10A C11A H11A 122.1 . . ? C16 C10A C11A 121.1(11) . . ? C16 C10A H10A 119.5 . . ? C11A C10A H10A 119.5 . . ? C10A C16 C15 121.2(11) . . ? C10A C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? C16 C15 C14 120.8(11) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C15 C14 C13 120.0(11) . . ? C15 C14 H14 120 . . ? C13 C14 H14 120 . . ? C21A C23 C24 116.7(11) . . ? C21A C23 P3 121.9(9) . . ? C24 C23 P3 120.8(10) . . ? C23 C21A C20A 132.0(8) . . ? C23 C21A H21A 114 . . ? C20A C21A H21A 114 . . ? C21A C20A C26 107.8(7) . . ? C21A C20A H20A 126.1 . . ? C26 C20A H20A 126.1 . . ? C25 C26 C20A 121.2(10) . . ? C25 C26 H26 119.4 . . ? C20A C26 H26 119.4 . . ? C26 C25 C24 119.6(12) . . ? C26 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? C25 C24 C23 119.7(12) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C27 C30 P3 118.7(9) . . ? C27 C30 H30 119.9 . . ? C28 C27 C30 120.2(12) . . ? C28 C27 H27 119.9 . . ? C30 C27 H27 119.9 . . ? C29 C28 C27 120.5(11) . . ? C29 C28 H28 119.8 . . ? C27 C28 H28 119.8 . . ? C28 C29 C3B 119.2(12) . . ? C28 C29 H29 120.4 . . ? C3B C29 H29 120.4 . . ? C29 C3B H3B 120.4 . . ? C7 C12 P3 122.6(10) . . ? C8 C7 C12 120.8(12) . . ? C8 C7 H7 119.6 . . ? C12 C7 H7 119.6 . . ? C7 C8 C9 121.2(12) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C8 C9 C10B 119.8(11) . . ? C8 C9 H9 120.1 . . ? C10B C9 H9 120.1 . . ? C9 C10B H10B 120.3 . . ? C17 C22B P3 120.1(9) . . ? C18 C17 C22B 117.5(11) . . ? C18 C17 H17 121.2 . . ? C22B C17 H17 121.2 . . ? C19 C18 C17 120.8(11) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C18 C19 H19 118.8 . . ? C62 O41 C42 119.0(3) . . ? C62 O41 Ru1 105.4(2) . . ? C42 O41 Ru1 133.1(3) . . ? O41 C42 C43 110.3(4) . . ? O41 C42 C44 104.1(4) . . ? C43 C42 C44 113.7(4) . . ? O41 C42 H42 109.5 . . ? C43 C42 H42 109.5 . . ? C44 C42 H42 109.5 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C61 C51 C52 104.0(4) . . ? C61 C51 Ru1 113.9(3) . . ? C52 C51 Ru1 142.1(3) . . ? C53 C52 C51 110.0(4) . . ? C53 C52 H52 125 . . ? C51 C52 H52 125 . . ? C52 C53 C60 109.0(4) . . ? C52 C53 C54A 127.1(5) . . ? C60 C53 C54A 123.9(5) . . ? C55A C54A C59A 119.9(6) . . ? C55A C54A C53 120.9(7) . . ? C59A C54A C53 119.2(6) . . ? C54A C55A C56A 109.7(10) . . ? C54A C55A H55A 125.1 . . ? C56A C55A H55A 125.1 . . ? C57A C56A C55A 121.7(12) . . ? C57A C56A H56A 119.2 . . ? C55A C56A H56A 119.2 . . ? C58A C57A C56A 122.5(16) . . ? C58A C57A H57A 118.8 . . ? C56A C57A H57A 118.8 . . ? C57A C58A C59A 112.6(16) . . ? C57A C58A H58A 123.7 . . ? C59A C58A H58A 123.7 . . ? C58A C59A C54A 132.0(10) . . ? C58A C59A H59A 114 . . ? C54A C59A H59A 114 . . ? C57B C56B H56B 125.7 . . ? C58B C57B C56B 119.8(15) . . ? C58B C57B H57B 120.1 . . ? C56B C57B H57B 120.1 . . ? C57B C58B H58B 116.2 . . ? C65 C60 C61 120.3(4) . . ? C65 C60 C53 134.0(4) . . ? C61 C60 C53 105.8(4) . . ? C62 C61 C60 121.7(4) . . ? C62 C61 C51 127.1(4) . . ? C60 C61 C51 111.2(4) . . ? O41 C62 C61 113.1(4) . . ? O41 C62 C63 127.4(4) . . ? C61 C62 C63 119.5(4) . . ? C64 C63 C62 118.0(4) . . ? C64 C63 H63 121 . . ? C62 C63 H63 121 . . ? O66 C64 C63 123.2(4) . . ? O66 C64 C65 114.0(4) . . ? C63 C64 C65 122.8(4) . . ? C60 C65 C64 117.8(4) . . ? C60 C65 H65 121.1 . . ? C64 C65 H65 121.1 . . ? C64 O66 C67 119.6(4) . . ? O66 C67 C68 109.3(6) . . ? O66 C67 C69 106.0(5) . . ? C68 C67 C69 113.4(6) . . ? O66 C67 H67 109.4 . . ? C68 C67 H67 109.4 . . ? C69 C67 H67 109.4 . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C67 C69 H69A 109.5 . . ? C67 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C67 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C51 Ru1 P3 C22B -167.5(5) . . . . ? Cl2 Ru1 P3 C22B -59.3(4) . . . . ? Cl1 Ru1 P3 C22B 83.9(4) . . . . ? C51 Ru1 P3 C1 40.0(5) . . . . ? Cl2 Ru1 P3 C1 148.1(5) . . . . ? Cl1 Ru1 P3 C1 -68.7(5) . . . . ? C51 Ru1 P3 C12 -44.1(5) . . . . ? Cl2 Ru1 P3 C12 64.1(5) . . . . ? Cl1 Ru1 P3 C12 -152.7(5) . . . . ? C51 Ru1 P3 C23 161.2(5) . . . . ? Cl2 Ru1 P3 C23 -90.6(5) . . . . ? Cl1 Ru1 P3 C23 52.6(5) . . . . ? C51 Ru1 P3 C30 76.5(5) . . . . ? Cl2 Ru1 P3 C30 -175.4(4) . . . . ? Cl1 Ru1 P3 C30 -32.1(4) . . . . ? C51 Ru1 P3 C13 -83.2(5) . . . . ? Cl2 Ru1 P3 C13 25.0(4) . . . . ? Cl1 Ru1 P3 C13 168.2(4) . . . . ? C22B P3 C1 C6 74.6(12) . . . . ? C12 P3 C1 C6 -25.4(10) . . . . ? C23 P3 C1 C6 97.2(11) . . . . ? C30 P3 C1 C6 130.1(15) . . . . ? C13 P3 C1 C6 -7.9(11) . . . . ? Ru1 P3 C1 C6 -138.0(9) . . . . ? C22B P3 C1 C2A -103.9(8) . . . . ? C12 P3 C1 C2A 156.1(9) . . . . ? C23 P3 C1 C2A -81.3(8) . . . . ? C30 P3 C1 C2A -48.4(9) . . . . ? C13 P3 C1 C2A 173.6(8) . . . . ? Ru1 P3 C1 C2A 43.6(9) . . . . ? C6 C1 C2A C3A 3.6(15) . . . . ? P3 C1 C2A C3A -177.9(7) . . . . ? C1 C2A C3A C4 -2.6(15) . . . . ? C2A C3A C4 C5 0.5(18) . . . . ? C3A C4 C5 C6 0.9(18) . . . . ? C2A C1 C6 C5 -2.5(17) . . . . ? P3 C1 C6 C5 179.1(9) . . . . ? C4 C5 C6 C1 0.1(18) . . . . ? C22B P3 C13 C14 -26.1(10) . . . . ? C1 P3 C13 C14 98.1(11) . . . . ? C12 P3 C13 C14 128.3(15) . . . . ? C23 P3 C13 C14 -9.3(11) . . . . ? C30 P3 C13 C14 72.1(12) . . . . ? Ru1 P3 C13 C14 -130.4(9) . . . . ? C22B P3 C13 C11A 154.4(9) . . . . ? C1 P3 C13 C11A -81.5(9) . . . . ? C12 P3 C13 C11A -51.2(9) . . . . ? C23 P3 C13 C11A 171.2(8) . . . . ? C30 P3 C13 C11A -107.5(9) . . . . ? Ru1 P3 C13 C11A 50.0(9) . . . . ? C14 C13 C11A C10A -0.4(15) . . . . ? P3 C13 C11A C10A 179.2(7) . . . . ? C13 C11A C10A C16 -1.4(15) . . . . ? C11A C10A C16 C15 3.6(18) . . . . ? C10A C16 C15 C14 -4.0(19) . . . . ? C16 C15 C14 C13 2.1(19) . . . . ? C11A C13 C14 C15 0.1(18) . . . . ? P3 C13 C14 C15 -179.4(10) . . . . ? C22B P3 C23 C21A -46.4(11) . . . . ? C1 P3 C23 C21A 173.0(9) . . . . ? C12 P3 C23 C21A -109.1(10) . . . . ? C30 P3 C23 C21A 155.5(11) . . . . ? C13 P3 C23 C21A -81.3(10) . . . . ? Ru1 P3 C23 C21A 43.4(11) . . . . ? C22B P3 C23 C24 142.4(16) . . . . ? C1 P3 C23 C24 1.8(11) . . . . ? C12 P3 C23 C24 79.6(12) . . . . ? C30 P3 C23 C24 -15.7(9) . . . . ? C13 P3 C23 C24 107.5(10) . . . . ? Ru1 P3 C23 C24 -127.8(9) . . . . ? C24 C23 C21A C20A -20.7(16) . . . . ? P3 C23 C21A C20A 167.7(6) . . . . ? C23 C21A C20A C26 21.6(12) . . . . ? C21A C20A C26 C25 -9.8(12) . . . . ? C20A C26 C25 C24 1.0(16) . . . . ? C26 C25 C24 C23 1.4(17) . . . . ? C21A C23 C24 C25 6.8(16) . . . . ? P3 C23 C24 C25 178.5(9) . . . . ? C22B P3 C30 C27 22.0(11) . . . . ? C1 P3 C30 C27 -114.3(14) . . . . ? C12 P3 C30 C27 -90.5(10) . . . . ? C23 P3 C30 C27 32.9(10) . . . . ? C13 P3 C30 C27 -61.6(12) . . . . ? Ru1 P3 C30 C27 140.6(8) . . . . ? P3 C30 C27 C28 175.9(9) . . . . ? C30 C27 C28 C29 0.1(18) . . . . ? C27 C28 C29 C3B 1.1(18) . . . . ? C22B P3 C12 C7 -99.2(11) . . . . ? C1 P3 C12 C7 23.3(10) . . . . ? C23 P3 C12 C7 -71.8(12) . . . . ? C30 P3 C12 C7 10.1(11) . . . . ? C13 P3 C12 C7 -125.6(14) . . . . ? Ru1 P3 C12 C7 137.2(9) . . . . ? P3 C12 C7 C8 177.5(9) . . . . ? C12 C7 C8 C9 1.6(18) . . . . ? C7 C8 C9 C10B -0.4(18) . . . . ? C1 P3 C22B C17 -87.9(12) . . . . ? C12 P3 C22B C17 -7.2(12) . . . . ? C23 P3 C22B C17 -137.1(16) . . . . ? C30 P3 C22B C17 -115.1(10) . . . . ? C13 P3 C22B C17 7.8(10) . . . . ? Ru1 P3 C22B C17 121.8(9) . . . . ? P3 C22B C17 C18 179.7(9) . . . . ? C22B C17 C18 C19 0.4(18) . . . . ? C51 Ru1 O41 C62 -0.9(3) . . . . ? Cl2 Ru1 O41 C62 -109.2(3) . . . . ? Cl1 Ru1 O41 C62 107.9(3) . . . . ? C51 Ru1 O41 C42 160.4(4) . . . . ? Cl2 Ru1 O41 C42 52.1(4) . . . . ? Cl1 Ru1 O41 C42 -90.8(4) . . . . ? C62 O41 C42 C43 67.3(5) . . . . ? Ru1 O41 C42 C43 -92.0(5) . . . . ? C62 O41 C42 C44 -170.4(4) . . . . ? Ru1 O41 C42 C44 30.3(5) . . . . ? P3 Ru1 C51 C61 -179.4(3) . . . . ? Cl2 Ru1 C51 C61 85.6(3) . . . . ? Cl1 Ru1 C51 C61 -82.9(3) . . . . ? O41 Ru1 C51 C61 0.6(3) . . . . ? P3 Ru1 C51 C52 -1.2(6) . . . . ? Cl2 Ru1 C51 C52 -96.2(6) . . . . ? Cl1 Ru1 C51 C52 95.3(6) . . . . ? O41 Ru1 C51 C52 178.8(6) . . . . ? C61 C51 C52 C53 0.4(6) . . . . ? Ru1 C51 C52 C53 -177.9(5) . . . . ? C51 C52 C53 C60 -0.4(6) . . . . ? C51 C52 C53 C54A 178.4(6) . . . . ? C52 C53 C54A C55A -46.7(9) . . . . ? C60 C53 C54A C55A 132.0(6) . . . . ? C52 C53 C54A C59A 134.0(6) . . . . ? C60 C53 C54A C59A -47.4(8) . . . . ? C59A C54A C55A C56A 8.6(9) . . . . ? C53 C54A C55A C56A -170.8(7) . . . . ? C54A C55A C56A C57A -13.4(14) . . . . ? C55A C56A C57A C58A 7(2) . . . . ? C56A C57A C58A C59A 4.5(19) . . . . ? C57A C58A C59A C54A -10.5(17) . . . . ? C55A C54A C59A C58A 2.8(13) . . . . ? C53 C54A C59A C58A -177.8(9) . . . . ? C52 C53 C60 C65 178.6(5) . . . . ? C54A C53 C60 C65 -0.2(9) . . . . ? C52 C53 C60 C61 0.2(6) . . . . ? C54A C53 C60 C61 -178.6(5) . . . . ? C65 C60 C61 C62 0.2(7) . . . . ? C53 C60 C61 C62 178.9(4) . . . . ? C65 C60 C61 C51 -178.7(4) . . . . ? C53 C60 C61 C51 0.0(5) . . . . ? C52 C51 C61 C62 -179.0(5) . . . . ? Ru1 C51 C61 C62 -0.2(7) . . . . ? C52 C51 C61 C60 -0.3(5) . . . . ? Ru1 C51 C61 C60 178.6(3) . . . . ? C42 O41 C62 C61 -163.5(4) . . . . ? Ru1 O41 C62 C61 1.0(4) . . . . ? C42 O41 C62 C63 17.3(7) . . . . ? Ru1 O41 C62 C63 -178.2(4) . . . . ? C60 C61 C62 O41 -179.4(4) . . . . ? C51 C61 C62 O41 -0.7(7) . . . . ? C60 C61 C62 C63 -0.1(7) . . . . ? C51 C61 C62 C63 178.6(4) . . . . ? O41 C62 C63 C64 179.1(4) . . . . ? C61 C62 C63 C64 -0.1(7) . . . . ? C62 C63 C64 O66 178.3(4) . . . . ? C62 C63 C64 C65 0.2(7) . . . . ? C61 C60 C65 C64 -0.1(7) . . . . ? C53 C60 C65 C64 -178.3(5) . . . . ? O66 C64 C65 C60 -178.3(4) . . . . ? C63 C64 C65 C60 -0.1(8) . . . . ? C63 C64 O66 C67 15.4(8) . . . . ? C65 C64 O66 C67 -166.4(5) . . . . ? C64 O66 C67 C68 75.1(6) . . . . ? C64 O66 C67 C69 -162.4(5) . . . . ? # Attachment 'complex 11.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2010-04-26 at 14:17:34 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : d:\progs\wingx\files\archive.dat # CIF files read : job struct data_job3 _database_code_depnum_ccdc_archive 'CCDC 856299' #TrackingRef 'complex 11.cif' _audit_creation_date 2010-04-26T14:17:34-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C41 H41 Cl2 O2 P Ru1' _chemical_formula_sum 'C41 H41 Cl2 O2 P Ru' _chemical_formula_weight 768.68 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c a b' _symmetry_space_group_name_Hall '-P 2bc 2ac' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' 'x+1/2, -y, -z+1/2' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' '-x-1/2, y, z-1/2' 'x-1/2, -y-1/2, z' _cell_length_a 11.3090(3) _cell_length_b 23.9659(7) _cell_length_c 26.7843(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 7259.4(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9595 _cell_measurement_theta_min 2.13 _cell_measurement_theta_max 27.4 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.09 _exptl_crystal_density_diffrn 1.407 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3168 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.658 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.647 _exptl_absorpt_correction_T_max 0.943 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.055 _diffrn_reflns_av_unetI/netI 0.05 _diffrn_reflns_number 33679 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_total 8309 _reflns_number_gt 6657 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SAINT (Bruker, 2002)' _computing_cell_refinement 'Bruker SMART (Bruker, 2002)' _computing_data_reduction 'Bruker SAINT (Bruker, 2002)' _computing_structure_solution 'SIR97 (Altomare et al., 1999))' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 1999), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0403P)^2^+0.2202P] 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_number_reflns 8309 _refine_ls_number_parameters 430 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0884 _refine_ls_wR_factor_gt 0.0824 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.608 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.072 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.373312(15) 0.064538(7) 0.355362(6) 0.01731(6) Uani 1 1 d . . . Cl1 Cl 0.27876(5) 0.09924(3) 0.28599(2) 0.02782(14) Uani 1 1 d . . . Cl2 Cl 0.54320(5) 0.07901(2) 0.40114(2) 0.02439(13) Uani 1 1 d . . . P1 P 0.26388(5) 0.11261(2) 0.40956(2) 0.01768(12) Uani 1 1 d . . . C1 C 0.3171(2) 0.10989(10) 0.47412(8) 0.0212(5) Uani 1 1 d . . . C2 C 0.3505(2) 0.05860(10) 0.49435(9) 0.0291(6) Uani 1 1 d . . . H2 H 0.3459 0.0257 0.4747 0.035 Uiso 1 1 calc R . . C3 C 0.3905(2) 0.05565(12) 0.54314(10) 0.0365(7) Uani 1 1 d . . . H3 H 0.4116 0.0205 0.5569 0.044 Uiso 1 1 calc R . . C4 C 0.3999(2) 0.10307(12) 0.57193(9) 0.0346(6) Uani 1 1 d . . . H4 H 0.4285 0.1008 0.6052 0.041 Uiso 1 1 calc R . . C5 C 0.3677(2) 0.15378(12) 0.55212(9) 0.0379(7) Uani 1 1 d . . . H5 H 0.3734 0.1866 0.5719 0.045 Uiso 1 1 calc R . . C6 C 0.3267(2) 0.15735(11) 0.50298(9) 0.0320(6) Uani 1 1 d . . . H6 H 0.3053 0.1926 0.4894 0.038 Uiso 1 1 calc R . . C7 C 0.25531(19) 0.18673(10) 0.39463(8) 0.0203(5) Uani 1 1 d . . . C8 C 0.3495(2) 0.21267(10) 0.37065(9) 0.0285(5) Uani 1 1 d . . . H8 H 0.4166 0.1913 0.3611 0.034 Uiso 1 1 calc R . . C9 C 0.3462(3) 0.26978(11) 0.36042(10) 0.0385(7) Uani 1 1 d . . . H9 H 0.4091 0.2869 0.3425 0.046 Uiso 1 1 calc R . . C10 C 0.2513(2) 0.30124(11) 0.37642(10) 0.0338(6) Uani 1 1 d . . . H10 H 0.2506 0.3404 0.3711 0.041 Uiso 1 1 calc R . . C11 C 0.1573(2) 0.27587(11) 0.40012(9) 0.0311(6) Uani 1 1 d . . . H11 H 0.0908 0.2975 0.4099 0.037 Uiso 1 1 calc R . . C12 C 0.1594(2) 0.21898(10) 0.40979(9) 0.0268(5) Uani 1 1 d . . . H12 H 0.0952 0.202 0.4268 0.032 Uiso 1 1 calc R . . C13 C 0.10883(19) 0.09232(10) 0.41425(8) 0.0219(5) Uani 1 1 d . . . C14 C 0.0428(2) 0.08830(11) 0.37060(9) 0.0304(6) Uani 1 1 d . . . H14 H 0.0782 0.0977 0.3395 0.037 Uiso 1 1 calc R . . C15 C -0.0738(2) 0.07072(12) 0.37181(11) 0.0363(6) Uani 1 1 d . . . H15 H -0.1184 0.0682 0.3419 0.044 Uiso 1 1 calc R . . C16 C -0.1251(2) 0.05671(12) 0.41751(11) 0.0389(7) Uani 1 1 d . . . H16 H -0.2048 0.0442 0.4186 0.047 Uiso 1 1 calc R . . C17 C -0.0617(2) 0.06076(11) 0.46058(11) 0.0361(6) Uani 1 1 d . . . H17 H -0.0973 0.0507 0.4914 0.043 Uiso 1 1 calc R . . C18 C 0.0552(2) 0.07954(10) 0.45983(9) 0.0276(5) Uani 1 1 d . . . H18 H 0.098 0.0836 0.4901 0.033 Uiso 1 1 calc R . . O21 O 0.48968(13) 0.00374(6) 0.29918(6) 0.0222(3) Uani 1 1 d . . . C22 C 0.6049(2) 0.01111(10) 0.27463(9) 0.0252(5) Uani 1 1 d . . . H22 H 0.6059 -0.0098 0.2423 0.03 Uiso 1 1 calc R . . C23 C 0.7018(2) -0.01019(11) 0.30809(10) 0.0336(6) Uani 1 1 d . . . H23A H 0.6999 0.01 0.3399 0.05 Uiso 1 1 calc R . . H23B H 0.7786 -0.0043 0.2919 0.05 Uiso 1 1 calc R . . H23C H 0.6902 -0.0501 0.3143 0.05 Uiso 1 1 calc R . . C24 C 0.6156(3) 0.07294(11) 0.26461(11) 0.0404(7) Uani 1 1 d . . . H24A H 0.546 0.0857 0.246 0.061 Uiso 1 1 calc R . . H24B H 0.687 0.0801 0.2449 0.061 Uiso 1 1 calc R . . H24C H 0.6205 0.0931 0.2964 0.061 Uiso 1 1 calc R . . C25 C 0.44828(19) -0.04936(9) 0.30796(8) 0.0188(4) Uani 1 1 d . . . C26 C 0.4886(2) -0.09947(10) 0.28647(8) 0.0223(5) Uani 1 1 d . . . H26 H 0.5506 -0.0994 0.2626 0.027 Uiso 1 1 calc R . . C27 C 0.4345(2) -0.14948(10) 0.30131(9) 0.0252(5) Uani 1 1 d . . . C28 C 0.3396(2) -0.15056(10) 0.33591(8) 0.0242(5) Uani 1 1 d . . . H28 H 0.3032 -0.1847 0.3452 0.029 Uiso 1 1 calc R . . C29 C 0.3020(2) -0.10085(10) 0.35554(8) 0.0203(5) Uani 1 1 d . . . C30 C 0.35684(19) -0.05076(9) 0.34167(8) 0.0187(5) Uani 1 1 d . . . O31 O 0.46634(15) -0.20086(7) 0.28395(7) 0.0357(4) Uani 1 1 d . . . C32 C 0.5840(2) -0.21098(11) 0.26524(10) 0.0332(6) Uani 1 1 d . . . H32 H 0.6006 -0.1852 0.2367 0.04 Uiso 1 1 calc R . . C33 C 0.5803(3) -0.27089(12) 0.24639(11) 0.0450(7) Uani 1 1 d . . . H33A H 0.561 -0.296 0.2741 0.067 Uiso 1 1 calc R . . H33B H 0.6576 -0.281 0.2325 0.067 Uiso 1 1 calc R . . H33C H 0.5198 -0.2743 0.2204 0.067 Uiso 1 1 calc R . . C34 C 0.6763(3) -0.20278(12) 0.30549(11) 0.0458(7) Uani 1 1 d . . . H34A H 0.6772 -0.1636 0.3158 0.069 Uiso 1 1 calc R . . H34B H 0.7543 -0.2131 0.2924 0.069 Uiso 1 1 calc R . . H34C H 0.6572 -0.2264 0.3343 0.069 Uiso 1 1 calc R . . C35 C 0.3055(2) -0.00418(10) 0.36921(8) 0.0204(5) Uani 1 1 d . . . C36 C 0.2133(2) -0.03033(10) 0.40031(9) 0.0240(5) Uani 1 1 d . . . H36 H 0.1628 -0.0107 0.4225 0.029 Uiso 1 1 calc R . . C37 C 0.2106(2) -0.08618(10) 0.39284(8) 0.0232(5) Uani 1 1 d . . . C38 C 0.1343(2) -0.12825(10) 0.41845(9) 0.0299(6) Uani 1 1 d . . . C39 C 0.0188(3) -0.13787(13) 0.40206(11) 0.0436(7) Uani 1 1 d . . . C40 C -0.0350(3) -0.1048(2) 0.36020(12) 0.0710(12) Uani 1 1 d . . . H40A H 0.0276 -0.0918 0.3377 0.106 Uiso 1 1 calc R . . H40B H -0.0774 -0.0726 0.3739 0.106 Uiso 1 1 calc R . . H40C H -0.0904 -0.1284 0.3416 0.106 Uiso 1 1 calc R . . C41 C -0.0460(3) -0.18006(16) 0.42650(14) 0.0649(11) Uani 1 1 d . . . H41 H -0.1232 -0.1891 0.4151 0.078 Uiso 1 1 calc R . . C42 C 0.0007(4) -0.20838(14) 0.46667(15) 0.0719(13) Uani 1 1 d . . . H42 H -0.0445 -0.2364 0.4829 0.086 Uiso 1 1 calc R . . C43 C 0.1124(4) -0.19619(13) 0.48317(14) 0.0616(10) Uani 1 1 d . . . H43 H 0.1427 -0.215 0.5116 0.074 Uiso 1 1 calc R . . C44 C 0.1816(3) -0.15723(12) 0.45929(11) 0.0427(7) Uani 1 1 d . . . C45 C 0.3042(3) -0.14536(16) 0.47802(12) 0.0628(10) Uani 1 1 d . . . H45A H 0.319 -0.1672 0.5083 0.094 Uiso 1 1 calc R . . H45B H 0.3117 -0.1055 0.4856 0.094 Uiso 1 1 calc R . . H45C H 0.362 -0.1557 0.4524 0.094 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 0.01527(10) 0.01508(10) 0.02157(10) -0.00083(7) -0.00019(7) -0.00015(7) Cl1 0.0282(3) 0.0304(3) 0.0248(3) 0.0004(2) -0.0055(2) 0.0031(2) Cl2 0.0169(3) 0.0248(3) 0.0315(3) -0.0024(2) -0.0025(2) -0.0006(2) P1 0.0160(3) 0.0160(3) 0.0210(3) -0.0013(2) -0.0019(2) 0.0016(2) C1 0.0184(11) 0.0241(12) 0.0212(11) 0.0008(9) -0.0018(9) -0.0007(9) C2 0.0317(14) 0.0238(13) 0.0317(13) 0.0001(10) -0.0045(11) 0.0029(10) C3 0.0380(16) 0.0374(16) 0.0342(14) 0.0124(12) -0.0051(12) 0.0037(12) C4 0.0323(15) 0.0491(18) 0.0224(12) 0.0028(12) -0.0039(11) -0.0014(12) C5 0.0484(18) 0.0391(16) 0.0261(13) -0.0054(12) -0.0076(12) -0.0009(13) C6 0.0392(15) 0.0284(14) 0.0283(13) 0.0008(11) -0.0072(11) 0.0023(12) C7 0.0199(11) 0.0193(11) 0.0218(11) -0.0003(9) -0.0048(9) 0.0034(9) C8 0.0246(13) 0.0224(13) 0.0385(13) -0.0023(11) 0.0032(10) 0.0023(10) C9 0.0385(16) 0.0238(14) 0.0533(17) 0.0048(12) 0.0047(13) -0.0038(12) C10 0.0387(15) 0.0173(12) 0.0454(15) 0.0003(11) -0.0090(12) 0.0034(11) C11 0.0327(14) 0.0241(13) 0.0364(14) -0.0048(11) -0.0062(11) 0.0089(11) C12 0.0236(13) 0.0258(13) 0.0311(13) -0.0023(10) -0.0008(10) 0.0045(10) C13 0.0163(11) 0.0190(11) 0.0303(12) -0.0037(10) 0.0002(9) 0.0044(9) C14 0.0238(13) 0.0342(14) 0.0334(13) -0.0005(11) -0.0021(10) -0.0019(11) C15 0.0224(14) 0.0411(16) 0.0455(16) -0.0042(13) -0.0058(12) -0.0033(11) C16 0.0190(14) 0.0399(17) 0.0577(18) -0.0090(14) 0.0041(12) -0.0052(11) C17 0.0264(14) 0.0384(16) 0.0435(16) -0.0003(12) 0.0130(12) 0.0009(11) C18 0.0269(13) 0.0248(13) 0.0311(13) -0.0038(10) 0.0030(10) 0.0020(10) O21 0.0195(8) 0.0185(8) 0.0285(8) 0.0003(7) 0.0058(6) -0.0017(6) C22 0.0239(12) 0.0242(12) 0.0275(12) -0.0040(10) 0.0104(9) -0.0059(10) C23 0.0225(13) 0.0362(15) 0.0422(15) -0.0098(12) 0.0046(11) -0.0057(11) C24 0.0487(18) 0.0290(15) 0.0433(16) 0.0050(12) 0.0204(13) -0.0057(13) C25 0.0160(11) 0.0193(11) 0.0209(11) 0.0001(9) -0.0033(8) -0.0017(8) C26 0.0186(12) 0.0240(12) 0.0243(11) -0.0051(10) 0.0043(9) 0.0006(9) C27 0.0225(12) 0.0196(12) 0.0335(13) -0.0084(10) 0.0006(10) -0.0011(9) C28 0.0220(12) 0.0184(12) 0.0320(12) -0.0031(10) 0.0024(10) -0.0056(9) C29 0.0171(11) 0.0202(11) 0.0237(11) -0.0012(9) -0.0008(9) -0.0026(9) C30 0.0155(11) 0.0175(11) 0.0231(11) -0.0030(9) -0.0003(9) -0.0005(8) O31 0.0301(10) 0.0213(9) 0.0558(11) -0.0151(8) 0.0121(8) -0.0028(7) C32 0.0363(15) 0.0273(14) 0.0361(14) -0.0041(11) 0.0096(11) 0.0051(11) C33 0.0591(19) 0.0291(16) 0.0467(16) -0.0131(13) 0.0081(15) 0.0093(14) C34 0.0452(17) 0.0339(16) 0.0584(18) -0.0072(14) -0.0051(14) 0.0093(14) C35 0.0180(11) 0.0201(11) 0.0232(11) -0.0027(9) 0.0003(9) 0.0011(9) C36 0.0227(12) 0.0212(12) 0.0280(12) -0.0029(10) 0.0066(9) -0.0017(9) C37 0.0191(12) 0.0231(12) 0.0272(12) -0.0006(10) 0.0031(9) -0.0020(9) C38 0.0305(14) 0.0197(12) 0.0394(14) -0.0060(11) 0.0162(11) -0.0054(10) C39 0.0360(16) 0.0516(19) 0.0432(16) -0.0185(14) 0.0161(13) -0.0182(14) C40 0.0336(19) 0.123(4) 0.056(2) -0.007(2) -0.0031(15) -0.026(2) C41 0.054(2) 0.068(3) 0.072(2) -0.032(2) 0.0377(19) -0.0397(19) C42 0.099(3) 0.0325(18) 0.084(3) -0.0096(18) 0.064(2) -0.023(2) C43 0.085(3) 0.0252(16) 0.074(2) 0.0132(16) 0.043(2) 0.0044(17) C44 0.0504(18) 0.0262(14) 0.0515(17) 0.0086(13) 0.0249(14) 0.0069(13) C45 0.050(2) 0.077(3) 0.061(2) 0.0328(19) 0.0083(16) 0.0229(18) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 1.854(2) . ? Ru1 P1 2.2285(6) . ? Ru1 Cl1 2.2995(6) . ? Ru1 Cl2 2.3054(6) . ? Ru1 O21 2.4737(15) . ? P1 C7 1.823(2) . ? P1 C13 1.824(2) . ? P1 C1 1.832(2) . ? C1 C6 1.380(3) . ? C1 C2 1.396(3) . ? C2 C3 1.384(4) . ? C2 H2 0.95 . ? C3 C4 1.378(4) . ? C3 H3 0.95 . ? C4 C5 1.375(4) . ? C4 H4 0.95 . ? C5 C6 1.398(3) . ? C5 H5 0.95 . ? C6 H6 0.95 . ? C7 C8 1.390(3) . ? C7 C12 1.392(3) . ? C8 C9 1.396(4) . ? C8 H8 0.95 . ? C9 C10 1.380(4) . ? C9 H9 0.95 . ? C10 C11 1.379(4) . ? C10 H10 0.95 . ? C11 C12 1.388(3) . ? C11 H11 0.95 . ? C12 H12 0.95 . ? C13 C14 1.390(3) . ? C13 C18 1.397(3) . ? C14 C15 1.385(4) . ? C14 H14 0.95 . ? C15 C16 1.395(4) . ? C15 H15 0.95 . ? C16 C17 1.362(4) . ? C16 H16 0.95 . ? C17 C18 1.397(4) . ? C17 H17 0.95 . ? C18 H18 0.95 . ? O21 C25 1.376(3) . ? O21 C22 1.470(3) . ? C22 C23 1.506(4) . ? C22 C24 1.511(3) . ? C22 H22 1 . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? C25 C30 1.373(3) . ? C25 C26 1.408(3) . ? C26 C27 1.403(3) . ? C26 H26 0.95 . ? C27 O31 1.365(3) . ? C27 C28 1.418(3) . ? C28 C29 1.370(3) . ? C28 H28 0.95 . ? C29 C30 1.401(3) . ? C29 C37 1.480(3) . ? C30 C35 1.458(3) . ? O31 C32 1.442(3) . ? C32 C34 1.513(4) . ? C32 C33 1.523(3) . ? C32 H32 1 . ? C33 H33A 0.98 . ? C33 H33B 0.98 . ? C33 H33C 0.98 . ? C34 H34A 0.98 . ? C34 H34B 0.98 . ? C34 H34C 0.98 . ? C35 C36 1.475(3) . ? C36 C37 1.354(3) . ? C36 H36 0.95 . ? C37 C38 1.493(3) . ? C38 C39 1.398(4) . ? C38 C44 1.402(4) . ? C39 C41 1.410(4) . ? C39 C40 1.502(5) . ? C40 H40A 0.98 . ? C40 H40B 0.98 . ? C40 H40C 0.98 . ? C41 C42 1.378(5) . ? C41 H41 0.95 . ? C42 C43 1.370(5) . ? C42 H42 0.95 . ? C43 C44 1.376(4) . ? C43 H43 0.95 . ? C44 C45 1.501(5) . ? C45 H45A 0.98 . ? C45 H45B 0.98 . ? C45 H45C 0.98 . ? 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 P1 95.70(7) . . ? C35 Ru1 Cl1 106.90(7) . . ? P1 Ru1 Cl1 94.65(2) . . ? C35 Ru1 Cl2 111.83(7) . . ? P1 Ru1 Cl2 92.21(2) . . ? Cl1 Ru1 Cl2 139.72(2) . . ? C35 Ru1 O21 79.54(8) . . ? P1 Ru1 O21 175.01(4) . . ? Cl1 Ru1 O21 88.22(4) . . ? Cl2 Ru1 O21 88.21(4) . . ? C7 P1 C13 102.93(10) . . ? C7 P1 C1 105.01(10) . . ? C13 P1 C1 103.97(10) . . ? C7 P1 Ru1 112.98(7) . . ? C13 P1 Ru1 116.16(7) . . ? C1 P1 Ru1 114.45(8) . . ? C6 C1 C2 119.2(2) . . ? C6 C1 P1 121.69(18) . . ? C2 C1 P1 119.14(18) . . ? C3 C2 C1 120.0(2) . . ? C3 C2 H2 120 . . ? C1 C2 H2 120 . . ? C4 C3 C2 120.8(2) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C5 C4 C3 119.5(2) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 120.3(3) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C1 C6 C5 120.2(2) . . ? C1 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C8 C7 C12 118.9(2) . . ? C8 C7 P1 119.75(17) . . ? C12 C7 P1 121.22(18) . . ? C7 C8 C9 120.6(2) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C10 C9 C8 119.7(3) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C11 C10 C9 120.1(2) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 120.4(2) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C11 C12 C7 120.3(2) . . ? C11 C12 H12 119.9 . . ? C7 C12 H12 119.9 . . ? C14 C13 C18 119.1(2) . . ? C14 C13 P1 118.46(18) . . ? C18 C13 P1 122.40(18) . . ? C15 C14 C13 120.8(2) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C14 C15 C16 119.3(3) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C17 C16 C15 120.5(2) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C18 120.6(3) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C17 C18 C13 119.6(2) . . ? C17 C18 H18 120.2 . . ? C13 C18 H18 120.2 . . ? C25 O21 C22 119.28(17) . . ? C25 O21 Ru1 105.05(12) . . ? C22 O21 Ru1 132.29(13) . . ? O21 C22 C23 109.78(18) . . ? O21 C22 C24 105.56(19) . . ? C23 C22 C24 112.3(2) . . ? O21 C22 H22 109.7 . . ? C23 C22 H22 109.7 . . ? C24 C22 H22 109.7 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C30 C25 O21 113.03(19) . . ? C30 C25 C26 119.5(2) . . ? O21 C25 C26 127.5(2) . . ? C27 C26 C25 118.2(2) . . ? C27 C26 H26 120.9 . . ? C25 C26 H26 120.9 . . ? O31 C27 C26 124.0(2) . . ? O31 C27 C28 114.0(2) . . ? C26 C27 C28 122.0(2) . . ? C29 C28 C27 118.0(2) . . ? C29 C28 H28 121 . . ? C27 C28 H28 121 . . ? C28 C29 C30 120.4(2) . . ? C28 C29 C37 133.0(2) . . ? C30 C29 C37 106.5(2) . . ? C25 C30 C29 121.9(2) . . ? C25 C30 C35 127.8(2) . . ? C29 C30 C35 110.2(2) . . ? C27 O31 C32 120.91(19) . . ? O31 C32 C34 111.5(2) . . ? O31 C32 C33 104.4(2) . . ? C34 C32 C33 112.2(2) . . ? O31 C32 H32 109.5 . . ? C34 C32 H32 109.5 . . ? C33 C32 H32 109.5 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C30 C35 C36 103.99(19) . . ? C30 C35 Ru1 114.47(16) . . ? C36 C35 Ru1 141.53(17) . . ? C37 C36 C35 110.7(2) . . ? C37 C36 H36 124.7 . . ? C35 C36 H36 124.7 . . ? C36 C37 C29 108.6(2) . . ? C36 C37 C38 127.8(2) . . ? C29 C37 C38 123.6(2) . . ? C39 C38 C44 121.3(3) . . ? C39 C38 C37 120.5(2) . . ? C44 C38 C37 118.2(2) . . ? C38 C39 C41 117.3(3) . . ? C38 C39 C40 121.8(3) . . ? C41 C39 C40 121.0(3) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 C39 121.1(3) . . ? C42 C41 H41 119.5 . . ? C39 C41 H41 119.5 . . ? C43 C42 C41 120.1(3) . . ? C43 C42 H42 120 . . ? C41 C42 H42 120 . . ? C42 C43 C44 121.3(4) . . ? C42 C43 H43 119.4 . . ? C44 C43 H43 119.4 . . ? C43 C44 C38 118.8(3) . . ? C43 C44 C45 119.9(3) . . ? C38 C44 C45 121.3(2) . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C35 Ru1 P1 C7 -157.85(10) . . . . ? Cl1 Ru1 P1 C7 -50.32(8) . . . . ? Cl2 Ru1 P1 C7 89.96(8) . . . . ? C35 Ru1 P1 C13 -39.22(11) . . . . ? Cl1 Ru1 P1 C13 68.30(9) . . . . ? Cl2 Ru1 P1 C13 -151.42(9) . . . . ? C35 Ru1 P1 C1 82.03(11) . . . . ? Cl1 Ru1 P1 C1 -170.44(8) . . . . ? Cl2 Ru1 P1 C1 -30.17(9) . . . . ? C7 P1 C1 C6 8.7(2) . . . . ? C13 P1 C1 C6 -99.0(2) . . . . ? Ru1 P1 C1 C6 133.22(19) . . . . ? C7 P1 C1 C2 -170.27(19) . . . . ? C13 P1 C1 C2 81.9(2) . . . . ? Ru1 P1 C1 C2 -45.8(2) . . . . ? C6 C1 C2 C3 1.3(4) . . . . ? P1 C1 C2 C3 -179.7(2) . . . . ? C1 C2 C3 C4 -1.3(4) . . . . ? C2 C3 C4 C5 0.9(4) . . . . ? C3 C4 C5 C6 -0.6(4) . . . . ? C2 C1 C6 C5 -0.9(4) . . . . ? P1 C1 C6 C5 -179.9(2) . . . . ? C4 C5 C6 C1 0.6(4) . . . . ? C13 P1 C7 C8 -156.55(19) . . . . ? C1 P1 C7 C8 94.91(19) . . . . ? Ru1 P1 C7 C8 -30.5(2) . . . . ? C13 P1 C7 C12 27.9(2) . . . . ? C1 P1 C7 C12 -80.7(2) . . . . ? Ru1 P1 C7 C12 153.93(16) . . . . ? C12 C7 C8 C9 -2.1(4) . . . . ? P1 C7 C8 C9 -177.8(2) . . . . ? C7 C8 C9 C10 3.2(4) . . . . ? C8 C9 C10 C11 -3.3(4) . . . . ? C9 C10 C11 C12 2.5(4) . . . . ? C10 C11 C12 C7 -1.5(4) . . . . ? C8 C7 C12 C11 1.3(3) . . . . ? P1 C7 C12 C11 176.90(18) . . . . ? C7 P1 C13 C14 72.9(2) . . . . ? C1 P1 C13 C14 -177.8(2) . . . . ? Ru1 P1 C13 C14 -51.1(2) . . . . ? C7 P1 C13 C18 -108.6(2) . . . . ? C1 P1 C13 C18 0.7(2) . . . . ? Ru1 P1 C13 C18 127.43(18) . . . . ? C18 C13 C14 C15 -1.4(4) . . . . ? P1 C13 C14 C15 177.2(2) . . . . ? C13 C14 C15 C16 -0.3(4) . . . . ? C14 C15 C16 C17 0.6(4) . . . . ? C15 C16 C17 C18 0.7(4) . . . . ? C16 C17 C18 C13 -2.4(4) . . . . ? C14 C13 C18 C17 2.7(4) . . . . ? P1 C13 C18 C17 -175.82(19) . . . . ? C35 Ru1 O21 C25 -1.97(13) . . . . ? Cl1 Ru1 O21 C25 -109.51(12) . . . . ? Cl2 Ru1 O21 C25 110.62(12) . . . . ? C35 Ru1 O21 C22 -160.28(19) . . . . ? Cl1 Ru1 O21 C22 92.17(17) . . . . ? Cl2 Ru1 O21 C22 -47.70(17) . . . . ? C25 O21 C22 C23 -66.1(2) . . . . ? Ru1 O21 C22 C23 89.8(2) . . . . ? C25 O21 C22 C24 172.6(2) . . . . ? Ru1 O21 C22 C24 -31.5(3) . . . . ? C22 O21 C25 C30 164.40(19) . . . . ? Ru1 O21 C25 C30 2.7(2) . . . . ? C22 O21 C25 C26 -16.0(3) . . . . ? Ru1 O21 C25 C26 -177.72(19) . . . . ? C30 C25 C26 C27 -1.2(3) . . . . ? O21 C25 C26 C27 179.2(2) . . . . ? C25 C26 C27 O31 -178.9(2) . . . . ? C25 C26 C27 C28 1.7(3) . . . . ? O31 C27 C28 C29 179.7(2) . . . . ? C26 C27 C28 C29 -0.9(3) . . . . ? C27 C28 C29 C30 -0.3(3) . . . . ? C27 C28 C29 C37 -177.8(2) . . . . ? O21 C25 C30 C29 179.75(19) . . . . ? C26 C25 C30 C29 0.1(3) . . . . ? O21 C25 C30 C35 -2.8(3) . . . . ? C26 C25 C30 C35 177.6(2) . . . . ? C28 C29 C30 C25 0.7(3) . . . . ? C37 C29 C30 C25 178.8(2) . . . . ? C28 C29 C30 C35 -177.2(2) . . . . ? C37 C29 C30 C35 0.9(3) . . . . ? C26 C27 O31 C32 25.1(3) . . . . ? C28 C27 O31 C32 -155.5(2) . . . . ? C27 O31 C32 C34 62.7(3) . . . . ? C27 O31 C32 C33 -176.0(2) . . . . ? C25 C30 C35 C36 -178.7(2) . . . . ? C29 C30 C35 C36 -1.0(3) . . . . ? C25 C30 C35 Ru1 0.8(3) . . . . ? C29 C30 C35 Ru1 178.52(15) . . . . ? P1 Ru1 C35 C30 -177.79(15) . . . . ? Cl1 Ru1 C35 C30 85.58(16) . . . . ? Cl2 Ru1 C35 C30 -83.10(16) . . . . ? O21 Ru1 C35 C30 0.69(15) . . . . ? P1 Ru1 C35 C36 1.4(3) . . . . ? Cl1 Ru1 C35 C36 -95.2(3) . . . . ? Cl2 Ru1 C35 C36 96.1(3) . . . . ? O21 Ru1 C35 C36 179.9(3) . . . . ? C30 C35 C36 C37 0.7(3) . . . . ? Ru1 C35 C36 C37 -178.5(2) . . . . ? C35 C36 C37 C29 -0.2(3) . . . . ? C35 C36 C37 C38 177.1(2) . . . . ? C28 C29 C37 C36 177.3(2) . . . . ? C30 C29 C37 C36 -0.4(3) . . . . ? C28 C29 C37 C38 -0.2(4) . . . . ? C30 C29 C37 C38 -177.9(2) . . . . ? C36 C37 C38 C39 83.3(3) . . . . ? C29 C37 C38 C39 -99.7(3) . . . . ? C36 C37 C38 C44 -96.3(3) . . . . ? C29 C37 C38 C44 80.7(3) . . . . ? C44 C38 C39 C41 -3.4(4) . . . . ? C37 C38 C39 C41 177.0(2) . . . . ? C44 C38 C39 C40 176.5(3) . . . . ? C37 C38 C39 C40 -3.0(4) . . . . ? C38 C39 C41 C42 3.5(4) . . . . ? C40 C39 C41 C42 -176.4(3) . . . . ? C39 C41 C42 C43 -0.7(5) . . . . ? C41 C42 C43 C44 -2.3(5) . . . . ? C42 C43 C44 C38 2.4(5) . . . . ? C42 C43 C44 C45 -179.3(3) . . . . ? C39 C38 C44 C43 0.6(4) . . . . ? C37 C38 C44 C43 -179.9(3) . . . . ? C39 C38 C44 C45 -177.7(3) . . . . ? C37 C38 C44 C45 1.8(4) . . . . ? # Attachment 'complex 3.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2010-05-18 at 10:19:12 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : d:\progs\wingx\files\archive.dat # CIF files read : job struct data_job4 _database_code_depnum_ccdc_archive 'CCDC 856300' #TrackingRef 'complex 3.cif' _audit_creation_date 2010-05-18T10:19:12-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C41 H59 Cl2 O2 P Ru, C H2 Cl2' _chemical_formula_sum 'C42 H61 Cl4 O2 P Ru' _chemical_formula_weight 871.75 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.6535(8) _cell_length_b 19.6215(12) _cell_length_c 15.8148(10) _cell_angle_alpha 90 _cell_angle_beta 108.752(3) _cell_angle_gamma 90 _cell_volume 4305.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9414 _cell_measurement_theta_min 2.08 _cell_measurement_theta_max 29.99 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.23 _exptl_crystal_density_diffrn 1.345 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.683 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.641 _exptl_absorpt_correction_T_max 0.855 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0768 _diffrn_reflns_av_unetI/netI 0.0339 _diffrn_reflns_number 99309 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 9796 _reflns_number_gt 8729 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SAINT (Bruker, 2002)' _computing_cell_refinement 'Bruker SMART (Bruker, 2002)' _computing_data_reduction 'Bruker SAINT (Bruker, 2002)' _computing_structure_solution 'SIR97 (Altomare et al., 1999))' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 1999), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0462P)^2^+5.4964P] 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_number_reflns 9796 _refine_ls_number_parameters 463 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.043 _refine_ls_R_factor_gt 0.037 _refine_ls_wR_factor_ref 0.1023 _refine_ls_wR_factor_gt 0.0949 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.042 _refine_diff_density_min -0.995 _refine_diff_density_rms 0.093 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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 -0.001753(11) 0.345552(8) 0.790888(11) 0.01549(6) Uani 1 1 d . . . Cl1 Cl -0.01375(4) 0.29412(3) 0.65609(4) 0.02547(12) Uani 1 1 d . . . Cl2 Cl 0.03453(4) 0.32872(3) 0.94256(4) 0.02455(12) Uani 1 1 d . . . P1 P -0.16047(4) 0.35687(3) 0.77231(4) 0.01655(11) Uani 1 1 d . . . C1 C -0.18297(15) 0.40037(11) 0.86814(14) 0.0193(4) Uani 1 1 d . . . H1 H -0.1515 0.3713 0.9215 0.023 Uiso 1 1 calc R . . C2 C -0.13492(17) 0.47094(11) 0.88977(15) 0.0228(4) Uani 1 1 d . . . H2A H -0.0661 0.4673 0.8944 0.027 Uiso 1 1 calc R . . H2B H -0.1663 0.503 0.8407 0.027 Uiso 1 1 calc R . . C3 C -0.14315(18) 0.49861(12) 0.97771(16) 0.0277(5) Uani 1 1 d . . . H3A H -0.1059 0.469 1.0275 0.033 Uiso 1 1 calc R . . H3B H -0.1149 0.5449 0.9885 0.033 Uiso 1 1 calc R . . C4 C -0.2476(2) 0.50160(13) 0.97600(17) 0.0320(5) Uani 1 1 d . . . H4A H -0.2825 0.5365 0.9323 0.038 Uiso 1 1 calc R . . H4B H -0.2495 0.5154 1.0356 0.038 Uiso 1 1 calc R . . C5 C -0.29786(19) 0.43288(14) 0.95082(18) 0.0326(5) Uani 1 1 d . . . H5A H -0.3668 0.4378 0.9453 0.039 Uiso 1 1 calc R . . H5B H -0.2687 0.3995 0.9989 0.039 Uiso 1 1 calc R . . C6 C -0.28954(17) 0.40595(13) 0.86279(16) 0.0267(5) Uani 1 1 d . . . H6A H -0.3237 0.4371 0.8135 0.032 Uiso 1 1 calc R . . H6B H -0.3204 0.3606 0.8498 0.032 Uiso 1 1 calc R . . C7 C -0.21979(16) 0.27286(11) 0.77118(15) 0.0209(4) Uani 1 1 d . . . H7 H -0.2895 0.2826 0.7608 0.025 Uiso 1 1 calc R . . C8 C -0.1831(2) 0.23443(12) 0.86026(17) 0.0308(5) Uani 1 1 d . . . H8A H -0.1871 0.2644 0.9093 0.037 Uiso 1 1 calc R . . H8B H -0.1147 0.2217 0.8723 0.037 Uiso 1 1 calc R . . C9 C -0.2435(2) 0.16978(13) 0.85738(19) 0.0343(6) Uani 1 1 d . . . H9A H -0.2164 0.1442 0.9139 0.041 Uiso 1 1 calc R . . H9B H -0.3104 0.1829 0.8519 0.041 Uiso 1 1 calc R . . C10 C -0.2444(2) 0.12422(14) 0.7791(2) 0.0432(7) Uani 1 1 d . . . H10A H -0.1789 0.1056 0.7893 0.052 Uiso 1 1 calc R . . H10B H -0.2886 0.0854 0.7758 0.052 Uiso 1 1 calc R . . C11 C -0.2764(3) 0.16283(15) 0.6912(2) 0.0439(8) Uani 1 1 d . . . H11A H -0.3449 0.176 0.6771 0.053 Uiso 1 1 calc R . . H11B H -0.2712 0.1326 0.6429 0.053 Uiso 1 1 calc R . . C12 C -0.2157(2) 0.22676(13) 0.69446(18) 0.0309(5) Uani 1 1 d . . . H12A H -0.2404 0.2517 0.6372 0.037 Uiso 1 1 calc R . . H12B H -0.148 0.2136 0.7032 0.037 Uiso 1 1 calc R . . C13 C -0.23825(16) 0.40368(12) 0.67175(15) 0.0230(4) Uani 1 1 d . . . H13 H -0.2376 0.4522 0.6912 0.028 Uiso 1 1 calc R . . C14 C -0.34548(17) 0.38306(14) 0.63814(17) 0.0307(5) Uani 1 1 d . . . H14A H -0.352 0.3369 0.6115 0.037 Uiso 1 1 calc R . . H14B H -0.3709 0.3817 0.689 0.037 Uiso 1 1 calc R . . C15 C -0.4039(2) 0.43405(17) 0.56823(19) 0.0422(7) Uani 1 1 d . . . H15A H -0.4722 0.4195 0.5463 0.051 Uiso 1 1 calc R . . H15B H -0.401 0.4795 0.5963 0.051 Uiso 1 1 calc R . . C16 C -0.3654(2) 0.43928(18) 0.48970(19) 0.0471(8) Uani 1 1 d . . . H16A H -0.3759 0.3955 0.4569 0.056 Uiso 1 1 calc R . . H16B H -0.4013 0.4751 0.4481 0.056 Uiso 1 1 calc R . . C17 C -0.2585(2) 0.45630(17) 0.52115(19) 0.0420(7) Uani 1 1 d . . . H17A H -0.249 0.5028 0.5469 0.05 Uiso 1 1 calc R . . H17B H -0.2345 0.4559 0.4693 0.05 Uiso 1 1 calc R . . C18 C -0.19993(18) 0.40531(14) 0.59150(16) 0.0291(5) Uani 1 1 d . . . H18A H -0.1312 0.4188 0.612 0.035 Uiso 1 1 calc R . . H18B H -0.205 0.3593 0.5647 0.035 Uiso 1 1 calc R . . O21 O 0.17538(11) 0.33654(7) 0.82134(11) 0.0202(3) Uani 1 1 d . . . C22 C 0.24982(17) 0.28612(11) 0.86361(16) 0.0243(5) Uani 1 1 d . . . H22 H 0.301 0.2874 0.8344 0.029 Uiso 1 1 calc R . . C23 C 0.1993(2) 0.21816(13) 0.8459(2) 0.0432(7) Uani 1 1 d . . . H23A H 0.15 0.2166 0.8755 0.065 Uiso 1 1 calc R . . H23B H 0.2463 0.1817 0.8694 0.065 Uiso 1 1 calc R . . H23C H 0.1689 0.2121 0.7815 0.065 Uiso 1 1 calc R . . C24 C 0.2943(2) 0.30243(16) 0.96233(18) 0.0385(6) Uani 1 1 d . . . H24A H 0.3248 0.3474 0.9692 0.058 Uiso 1 1 calc R . . H24B H 0.3428 0.2679 0.9907 0.058 Uiso 1 1 calc R . . H24C H 0.2439 0.3024 0.9907 0.058 Uiso 1 1 calc R . . C25 C 0.20264(15) 0.40120(11) 0.80782(14) 0.0188(4) Uani 1 1 d . . . C26 C 0.29527(16) 0.42328(12) 0.81508(16) 0.0248(5) Uani 1 1 d . . . H26 H 0.3481 0.3926 0.8331 0.03 Uiso 1 1 calc R . . C27 C 0.30951(17) 0.49137(13) 0.79555(19) 0.0302(5) Uani 1 1 d . A . C28 C 0.23321(17) 0.53871(12) 0.76900(18) 0.0277(5) Uani 1 1 d . . . H28 H 0.2438 0.5848 0.7563 0.033 Uiso 1 1 calc R . . C29 C 0.14163(16) 0.51481(11) 0.76225(15) 0.0207(4) Uani 1 1 d . . . C30 C 0.12739(15) 0.44740(11) 0.78204(14) 0.0182(4) Uani 1 1 d . . . O31 O 0.40256(13) 0.50562(10) 0.80130(17) 0.0454(5) Uani 1 1 d . . . C32A C 0.4325(2) 0.57482(15) 0.8011(3) 0.0463(8) Uani 0.80(2) 1 d PD A 1 H32A H 0.3815 0.5989 0.7528 0.056 Uiso 0.80(2) 1 calc PR A 1 C33A C 0.5221(2) 0.5728(2) 0.7732(3) 0.0600(10) Uani 0.80(2) 1 d P A 1 H33A H 0.5748 0.5516 0.8207 0.09 Uiso 0.80(2) 1 calc PR A 1 H33B H 0.5403 0.6193 0.7628 0.09 Uiso 0.80(2) 1 calc PR A 1 H33C H 0.509 0.5461 0.7182 0.09 Uiso 0.80(2) 1 calc PR A 1 C34A C 0.4434(6) 0.6105(4) 0.8827(6) 0.0643(19) Uani 0.80(2) 1 d PD A 1 H34A H 0.3819 0.6105 0.8948 0.096 Uiso 0.80(2) 1 calc PR A 1 H34B H 0.4632 0.6576 0.8773 0.096 Uiso 0.80(2) 1 calc PR A 1 H34C H 0.4927 0.5879 0.9318 0.096 Uiso 0.80(2) 1 calc PR A 1 C32B C 0.4325(2) 0.57482(15) 0.8011(3) 0.0463(8) Uani 0.20(2) 1 d PD A 2 H32B H 0.3812 0.6067 0.7656 0.056 Uiso 0.20(2) 1 calc PR A 2 C33B C 0.5221(2) 0.5728(2) 0.7732(3) 0.0600(10) Uani 0.20(2) 1 d P A 2 H33D H 0.5716 0.5452 0.816 0.09 Uiso 0.20(2) 1 calc PR A 2 H33E H 0.5462 0.6192 0.7721 0.09 Uiso 0.20(2) 1 calc PR A 2 H33F H 0.5063 0.5525 0.7136 0.09 Uiso 0.20(2) 1 calc PR A 2 C34B C 0.469(2) 0.5883(17) 0.9087(18) 0.0643(19) Uani 0.20(2) 1 d PD A 2 H34D H 0.4149 0.6042 0.927 0.096 Uiso 0.20(2) 1 calc PR A 2 H34E H 0.52 0.623 0.9236 0.096 Uiso 0.20(2) 1 calc PR A 2 H34F H 0.4945 0.5459 0.9401 0.096 Uiso 0.20(2) 1 calc PR A 2 C35 C 0.02567(15) 0.43507(11) 0.77034(14) 0.0183(4) Uani 1 1 d . . . C36 C -0.02070(16) 0.50157(11) 0.74060(15) 0.0219(4) Uani 1 1 d . . . H36 H -0.0876 0.5105 0.7272 0.026 Uiso 1 1 calc R . . C37 C 0.04571(15) 0.54839(11) 0.73512(15) 0.0198(4) Uani 1 1 d . . . C38 C 0.02853(15) 0.62083(11) 0.70467(15) 0.0195(4) Uani 1 1 d . . . C39 C 0.01442(17) 0.63632(12) 0.61485(16) 0.0251(5) Uani 1 1 d . . . C40 C 0.0153(2) 0.58104(15) 0.54876(19) 0.0408(7) Uani 1 1 d . . . H40A H 0.0725 0.5524 0.5734 0.061 Uiso 1 1 calc R . . H40B H 0.0166 0.6018 0.4928 0.061 Uiso 1 1 calc R . . H40C H -0.0428 0.553 0.5372 0.061 Uiso 1 1 calc R . . C41 C -0.00081(19) 0.70424(13) 0.58682(18) 0.0310(5) Uani 1 1 d . . . H41 H -0.0098 0.7155 0.5262 0.037 Uiso 1 1 calc R . . C42 C -0.00287(18) 0.75517(12) 0.64681(19) 0.0316(5) Uani 1 1 d . . . H42 H -0.0145 0.801 0.6269 0.038 Uiso 1 1 calc R . . C43 C 0.01182(18) 0.73985(12) 0.73520(19) 0.0299(5) Uani 1 1 d . . . H43 H 0.0108 0.7753 0.7758 0.036 Uiso 1 1 calc R . . C44 C 0.02821(16) 0.67257(12) 0.76572(16) 0.0235(4) Uani 1 1 d . . . C45 C 0.0471(2) 0.65639(14) 0.86330(18) 0.0364(6) Uani 1 1 d . . . H45A H 0.0419 0.6982 0.8954 0.055 Uiso 1 1 calc R . . H45B H 0.112 0.6374 0.8887 0.055 Uiso 1 1 calc R . . H45C H -0.0004 0.6231 0.8691 0.055 Uiso 1 1 calc R . . C51 C 0.2210(3) 0.3384(3) 0.5929(3) 0.0917(19) Uani 1 1 d . . . H51A H 0.1925 0.3535 0.6386 0.11 Uiso 1 1 calc R . . H51B H 0.1766 0.3522 0.5337 0.11 Uiso 1 1 calc R . . Cl51 Cl 0.23144(10) 0.24968(8) 0.59654(13) 0.1069(5) Uani 1 1 d . . . Cl52 Cl 0.33195(11) 0.37915(8) 0.61157(8) 0.0905(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 Ru1 0.01431(10) 0.01348(9) 0.01855(10) 0.00052(5) 0.00508(7) 0.00004(5) Cl1 0.0237(3) 0.0301(3) 0.0227(2) -0.0055(2) 0.0076(2) 0.0018(2) Cl2 0.0227(3) 0.0295(3) 0.0202(2) 0.0014(2) 0.0051(2) -0.0004(2) P1 0.0146(3) 0.0146(2) 0.0203(3) -0.00190(19) 0.0054(2) -0.00105(18) C1 0.0189(10) 0.0161(9) 0.0229(10) -0.0018(8) 0.0068(8) -0.0008(7) C2 0.0257(11) 0.0160(10) 0.0259(11) -0.0030(8) 0.0072(9) -0.0031(8) C3 0.0333(13) 0.0219(11) 0.0247(11) -0.0059(9) 0.0049(10) -0.0008(9) C4 0.0385(15) 0.0306(13) 0.0270(12) -0.0081(10) 0.0110(11) 0.0066(10) C5 0.0300(13) 0.0392(14) 0.0330(13) -0.0076(11) 0.0165(11) -0.0002(10) C6 0.0209(11) 0.0297(12) 0.0318(12) -0.0085(9) 0.0115(9) -0.0017(9) C7 0.0182(10) 0.0179(10) 0.0268(11) -0.0057(8) 0.0076(8) -0.0042(8) C8 0.0352(14) 0.0225(11) 0.0319(12) 0.0007(9) 0.0070(10) -0.0091(10) C9 0.0423(16) 0.0234(12) 0.0413(14) -0.0014(10) 0.0193(12) -0.0096(11) C10 0.0562(19) 0.0215(12) 0.0650(19) -0.0098(12) 0.0376(16) -0.0146(12) C11 0.0549(19) 0.0331(14) 0.0509(17) -0.0229(13) 0.0271(15) -0.0246(13) C12 0.0386(14) 0.0229(11) 0.0366(13) -0.0100(10) 0.0198(11) -0.0079(10) C13 0.0197(11) 0.0231(11) 0.0234(10) -0.0012(8) 0.0030(8) 0.0036(8) C14 0.0197(12) 0.0385(14) 0.0293(12) -0.0041(10) 0.0016(9) 0.0019(10) C15 0.0255(14) 0.0561(18) 0.0382(14) -0.0032(13) 0.0007(11) 0.0143(12) C16 0.0402(17) 0.061(2) 0.0298(13) 0.0050(13) -0.0025(12) 0.0227(14) C17 0.0429(17) 0.0507(17) 0.0314(13) 0.0132(12) 0.0103(12) 0.0181(13) C18 0.0263(12) 0.0350(13) 0.0245(11) 0.0039(10) 0.0061(9) 0.0079(10) O21 0.0161(8) 0.0148(7) 0.0274(8) 0.0027(6) 0.0039(6) 0.0015(5) C22 0.0204(11) 0.0184(10) 0.0320(12) 0.0033(9) 0.0055(9) 0.0073(8) C23 0.0443(17) 0.0172(12) 0.0633(19) 0.0053(12) 0.0105(14) 0.0032(11) C24 0.0324(15) 0.0450(16) 0.0312(13) 0.0085(11) 0.0006(11) 0.0104(12) C25 0.0175(10) 0.0167(10) 0.0215(10) -0.0005(8) 0.0052(8) 0.0008(7) C26 0.0163(11) 0.0210(11) 0.0363(12) 0.0020(9) 0.0075(9) 0.0030(8) C27 0.0158(11) 0.0258(12) 0.0498(15) 0.0034(11) 0.0117(10) -0.0018(9) C28 0.0185(11) 0.0188(10) 0.0462(14) 0.0051(10) 0.0112(10) -0.0010(8) C29 0.0165(10) 0.0186(10) 0.0272(11) 0.0017(8) 0.0070(8) 0.0014(8) C30 0.0145(10) 0.0165(10) 0.0234(10) 0.0011(8) 0.0058(8) -0.0004(7) O31 0.0155(9) 0.0302(10) 0.0895(17) 0.0101(10) 0.0157(10) -0.0008(7) C32A 0.0217(13) 0.0306(14) 0.085(2) 0.0169(15) 0.0152(14) -0.0020(10) C33A 0.0296(16) 0.074(3) 0.078(3) 0.021(2) 0.0189(17) -0.0121(15) C34A 0.061(4) 0.047(4) 0.090(5) 0.002(3) 0.031(4) -0.009(3) C32B 0.0217(13) 0.0306(14) 0.085(2) 0.0169(15) 0.0152(14) -0.0020(10) C33B 0.0296(16) 0.074(3) 0.078(3) 0.021(2) 0.0189(17) -0.0121(15) C34B 0.061(4) 0.047(4) 0.090(5) 0.002(3) 0.031(4) -0.009(3) C35 0.0148(10) 0.0184(10) 0.0222(10) 0.0020(8) 0.0064(8) 0.0004(7) C36 0.0154(10) 0.0206(10) 0.0302(11) 0.0048(8) 0.0078(9) 0.0019(8) C37 0.0172(10) 0.0177(10) 0.0247(10) 0.0035(8) 0.0068(8) 0.0021(8) C38 0.0143(10) 0.0174(10) 0.0275(11) 0.0037(8) 0.0076(8) 0.0013(7) C39 0.0223(11) 0.0248(11) 0.0303(12) 0.0042(9) 0.0113(9) 0.0022(9) C40 0.0563(19) 0.0367(15) 0.0326(13) -0.0005(11) 0.0190(13) 0.0103(13) C41 0.0299(13) 0.0302(13) 0.0341(13) 0.0135(10) 0.0121(10) 0.0024(10) C42 0.0282(13) 0.0200(11) 0.0456(14) 0.0111(10) 0.0105(11) 0.0021(9) C43 0.0281(13) 0.0201(11) 0.0401(13) -0.0031(10) 0.0089(10) 0.0000(9) C44 0.0188(11) 0.0232(11) 0.0281(11) 0.0019(9) 0.0067(9) 0.0011(8) C45 0.0408(16) 0.0380(15) 0.0277(13) -0.0008(10) 0.0074(11) 0.0021(11) C51 0.054(3) 0.152(5) 0.057(2) -0.030(3) 0.001(2) 0.042(3) Cl51 0.0683(8) 0.0981(10) 0.1494(14) 0.0276(9) 0.0285(8) 0.0213(7) Cl52 0.1063(10) 0.0953(9) 0.0604(6) 0.0105(6) 0.0137(6) 0.0049(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 1.854(2) . ? Ru1 P1 2.2596(6) . ? Ru1 Cl2 2.3077(6) . ? Ru1 Cl1 2.3136(6) . ? Ru1 O21 2.4893(16) . ? P1 C1 1.859(2) . ? P1 C7 1.861(2) . ? P1 C13 1.873(2) . ? C1 C6 1.540(3) . ? C1 C2 1.541(3) . ? C1 H1 1 . ? C2 C3 1.533(3) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C3 C4 1.523(4) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? C4 C5 1.527(4) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? C5 C6 1.530(3) . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? C7 C12 1.530(3) . ? C7 C8 1.535(3) . ? C7 H7 1 . ? C8 C9 1.539(3) . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? C9 C10 1.523(4) . ? C9 H9A 0.99 . ? C9 H9B 0.99 . ? C10 C11 1.519(5) . ? C10 H10A 0.99 . ? C10 H10B 0.99 . ? C11 C12 1.529(3) . ? C11 H11A 0.99 . ? C11 H11B 0.99 . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? C13 C14 1.542(3) . ? C13 C18 1.544(3) . ? C13 H13 1 . ? C14 C15 1.532(4) . ? C14 H14A 0.99 . ? C14 H14B 0.99 . ? C15 C16 1.523(4) . ? C15 H15A 0.99 . ? C15 H15B 0.99 . ? C16 C17 1.521(5) . ? C16 H16A 0.99 . ? C16 H16B 0.99 . ? C17 C18 1.537(3) . ? C17 H17A 0.99 . ? C17 H17B 0.99 . ? C18 H18A 0.99 . ? C18 H18B 0.99 . ? O21 C25 1.367(3) . ? O21 C22 1.465(3) . ? C22 C23 1.507(4) . ? C22 C24 1.520(4) . ? C22 H22 1 . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? C25 C30 1.384(3) . ? C25 C26 1.394(3) . ? C26 C27 1.402(3) . ? C26 H26 0.95 . ? C27 O31 1.366(3) . ? C27 C28 1.410(3) . ? C28 C29 1.393(3) . ? C28 H28 0.95 . ? C29 C30 1.390(3) . ? C29 C37 1.485(3) . ? C30 C35 1.462(3) . ? O31 C32A 1.428(3) . ? C32A C34A 1.431(7) . ? C32A C33A 1.512(4) . ? C32A H32A 1 . ? C33A H33A 0.98 . ? C33A H33B 0.98 . ? C33A H33C 0.98 . ? C34A H34A 0.98 . ? C34A H34B 0.98 . ? C34A H34C 0.98 . ? C34B H34D 0.98 . ? C34B H34E 0.98 . ? C34B H34F 0.98 . ? C35 C36 1.476(3) . ? C36 C37 1.361(3) . ? C36 H36 0.95 . ? C37 C38 1.496(3) . ? C38 C39 1.401(3) . ? C38 C44 1.402(3) . ? C39 C41 1.400(3) . ? C39 C40 1.509(4) . ? C40 H40A 0.98 . ? C40 H40B 0.98 . ? C40 H40C 0.98 . ? C41 C42 1.385(4) . ? C41 H41 0.95 . ? C42 C43 1.377(4) . ? C42 H42 0.95 . ? C43 C44 1.400(3) . ? C43 H43 0.95 . ? C44 C45 1.511(4) . ? C45 H45A 0.98 . ? C45 H45B 0.98 . ? C45 H45C 0.98 . ? C51 Cl51 1.747(6) . ? C51 Cl52 1.750(6) . ? C51 H51A 0.99 . ? C51 H51B 0.99 . ? 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 P1 98.98(6) . . ? C35 Ru1 Cl2 109.10(7) . . ? P1 Ru1 Cl2 91.88(2) . . ? C35 Ru1 Cl1 102.03(7) . . ? P1 Ru1 Cl1 98.79(2) . . ? Cl2 Ru1 Cl1 145.00(2) . . ? C35 Ru1 O21 80.21(7) . . ? P1 Ru1 O21 176.20(4) . . ? Cl2 Ru1 O21 84.91(4) . . ? Cl1 Ru1 O21 85.01(4) . . ? C1 P1 C7 102.11(10) . . ? C1 P1 C13 104.37(10) . . ? C7 P1 C13 105.75(10) . . ? C1 P1 Ru1 112.59(7) . . ? C7 P1 Ru1 111.86(7) . . ? C13 P1 Ru1 118.60(8) . . ? C6 C1 C2 109.33(18) . . ? C6 C1 P1 115.48(15) . . ? C2 C1 P1 113.91(15) . . ? C6 C1 H1 105.8 . . ? C2 C1 H1 105.8 . . ? P1 C1 H1 105.8 . . ? C3 C2 C1 110.84(19) . . ? C3 C2 H2A 109.5 . . ? C1 C2 H2A 109.5 . . ? C3 C2 H2B 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? C4 C3 C2 111.66(19) . . ? C4 C3 H3A 109.3 . . ? C2 C3 H3A 109.3 . . ? C4 C3 H3B 109.3 . . ? C2 C3 H3B 109.3 . . ? H3A C3 H3B 107.9 . . ? C3 C4 C5 111.6(2) . . ? C3 C4 H4A 109.3 . . ? C5 C4 H4A 109.3 . . ? C3 C4 H4B 109.3 . . ? C5 C4 H4B 109.3 . . ? H4A C4 H4B 108 . . ? C4 C5 C6 111.7(2) . . ? C4 C5 H5A 109.3 . . ? C6 C5 H5A 109.3 . . ? C4 C5 H5B 109.3 . . ? C6 C5 H5B 109.3 . . ? H5A C5 H5B 107.9 . . ? C5 C6 C1 110.5(2) . . ? C5 C6 H6A 109.5 . . ? C1 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? C12 C7 C8 110.2(2) . . ? C12 C7 P1 113.20(16) . . ? C8 C7 P1 113.69(15) . . ? C12 C7 H7 106.4 . . ? C8 C7 H7 106.4 . . ? P1 C7 H7 106.4 . . ? C7 C8 C9 110.5(2) . . ? C7 C8 H8A 109.6 . . ? C9 C8 H8A 109.6 . . ? C7 C8 H8B 109.6 . . ? C9 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? C10 C9 C8 111.3(2) . . ? C10 C9 H9A 109.4 . . ? C8 C9 H9A 109.4 . . ? C10 C9 H9B 109.4 . . ? C8 C9 H9B 109.4 . . ? H9A C9 H9B 108 . . ? C11 C10 C9 111.7(2) . . ? C11 C10 H10A 109.3 . . ? C9 C10 H10A 109.3 . . ? C11 C10 H10B 109.3 . . ? C9 C10 H10B 109.3 . . ? H10A C10 H10B 107.9 . . ? C10 C11 C12 111.9(3) . . ? C10 C11 H11A 109.2 . . ? C12 C11 H11A 109.2 . . ? C10 C11 H11B 109.2 . . ? C12 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? C11 C12 C7 109.9(2) . . ? C11 C12 H12A 109.7 . . ? C7 C12 H12A 109.7 . . ? C11 C12 H12B 109.7 . . ? C7 C12 H12B 109.7 . . ? H12A C12 H12B 108.2 . . ? C14 C13 C18 108.76(19) . . ? C14 C13 P1 116.01(17) . . ? C18 C13 P1 115.17(16) . . ? C14 C13 H13 105.3 . . ? C18 C13 H13 105.3 . . ? P1 C13 H13 105.3 . . ? C15 C14 C13 110.4(2) . . ? C15 C14 H14A 109.6 . . ? C13 C14 H14A 109.6 . . ? C15 C14 H14B 109.6 . . ? C13 C14 H14B 109.6 . . ? H14A C14 H14B 108.1 . . ? C16 C15 C14 111.4(2) . . ? C16 C15 H15A 109.3 . . ? C14 C15 H15A 109.3 . . ? C16 C15 H15B 109.3 . . ? C14 C15 H15B 109.3 . . ? H15A C15 H15B 108 . . ? C17 C16 C15 111.1(2) . . ? C17 C16 H16A 109.4 . . ? C15 C16 H16A 109.4 . . ? C17 C16 H16B 109.4 . . ? C15 C16 H16B 109.4 . . ? H16A C16 H16B 108 . . ? C16 C17 C18 111.8(3) . . ? C16 C17 H17A 109.3 . . ? C18 C17 H17A 109.3 . . ? C16 C17 H17B 109.3 . . ? C18 C17 H17B 109.3 . . ? H17A C17 H17B 107.9 . . ? C17 C18 C13 110.0(2) . . ? C17 C18 H18A 109.7 . . ? C13 C18 H18A 109.7 . . ? C17 C18 H18B 109.7 . . ? C13 C18 H18B 109.7 . . ? H18A C18 H18B 108.2 . . ? C25 O21 C22 119.06(17) . . ? C25 O21 Ru1 104.05(12) . . ? C22 O21 Ru1 135.50(13) . . ? O21 C22 C23 105.30(19) . . ? O21 C22 C24 109.69(19) . . ? C23 C22 C24 113.6(2) . . ? O21 C22 H22 109.4 . . ? C23 C22 H22 109.4 . . ? C24 C22 H22 109.4 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O21 C25 C30 114.12(18) . . ? O21 C25 C26 126.96(19) . . ? C30 C25 C26 118.9(2) . . ? C25 C26 C27 119.2(2) . . ? C25 C26 H26 120.4 . . ? C27 C26 H26 120.4 . . ? O31 C27 C26 113.4(2) . . ? O31 C27 C28 124.3(2) . . ? C26 C27 C28 122.2(2) . . ? C29 C28 C27 117.0(2) . . ? C29 C28 H28 121.5 . . ? C27 C28 H28 121.5 . . ? C30 C29 C28 120.9(2) . . ? C30 C29 C37 106.89(18) . . ? C28 C29 C37 132.2(2) . . ? C25 C30 C29 121.77(19) . . ? C25 C30 C35 127.76(19) . . ? C29 C30 C35 110.47(18) . . ? C27 O31 C32A 119.7(2) . . ? O31 C32A C34A 114.1(4) . . ? O31 C32A C33A 105.8(3) . . ? C34A C32A C33A 114.8(4) . . ? O31 C32A H32A 107.2 . . ? C34A C32A H32A 107.2 . . ? C33A C32A H32A 107.2 . . ? H34D C34B H34E 109.5 . . ? H34D C34B H34F 109.5 . . ? H34E C34B H34F 109.5 . . ? C30 C35 C36 103.89(17) . . ? C30 C35 Ru1 113.85(15) . . ? C36 C35 Ru1 142.16(16) . . ? C37 C36 C35 110.58(19) . . ? C37 C36 H36 124.7 . . ? C35 C36 H36 124.7 . . ? C36 C37 C29 108.17(18) . . ? C36 C37 C38 127.7(2) . . ? C29 C37 C38 124.07(19) . . ? C39 C38 C44 120.6(2) . . ? C39 C38 C37 119.1(2) . . ? C44 C38 C37 120.3(2) . . ? C41 C39 C38 119.0(2) . . ? C41 C39 C40 120.1(2) . . ? C38 C39 C40 121.0(2) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 C39 120.4(2) . . ? C42 C41 H41 119.8 . . ? C39 C41 H41 119.8 . . ? C43 C42 C41 120.5(2) . . ? C43 C42 H42 119.8 . . ? C41 C42 H42 119.8 . . ? C42 C43 C44 120.6(2) . . ? C42 C43 H43 119.7 . . ? C44 C43 H43 119.7 . . ? C43 C44 C38 118.9(2) . . ? C43 C44 C45 120.3(2) . . ? C38 C44 C45 120.7(2) . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? Cl51 C51 Cl52 112.5(2) . . ? Cl51 C51 H51A 109.1 . . ? Cl52 C51 H51A 109.1 . . ? Cl51 C51 H51B 109.1 . . ? Cl52 C51 H51B 109.1 . . ? H51A C51 H51B 107.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C35 Ru1 P1 C1 -74.29(10) . . . . ? Cl2 Ru1 P1 C1 35.38(8) . . . . ? Cl1 Ru1 P1 C1 -178.06(8) . . . . ? C35 Ru1 P1 C7 171.40(10) . . . . ? Cl2 Ru1 P1 C7 -78.93(8) . . . . ? Cl1 Ru1 P1 C7 67.63(8) . . . . ? C35 Ru1 P1 C13 47.91(11) . . . . ? Cl2 Ru1 P1 C13 157.59(8) . . . . ? Cl1 Ru1 P1 C13 -55.86(9) . . . . ? C7 P1 C1 C6 -56.28(18) . . . . ? C13 P1 C1 C6 53.69(19) . . . . ? Ru1 P1 C1 C6 -176.39(14) . . . . ? C7 P1 C1 C2 175.95(16) . . . . ? C13 P1 C1 C2 -74.08(18) . . . . ? Ru1 P1 C1 C2 55.84(17) . . . . ? C6 C1 C2 C3 58.0(2) . . . . ? P1 C1 C2 C3 -171.11(16) . . . . ? C1 C2 C3 C4 -56.0(3) . . . . ? C2 C3 C4 C5 53.6(3) . . . . ? C3 C4 C5 C6 -54.1(3) . . . . ? C4 C5 C6 C1 56.8(3) . . . . ? C2 C1 C6 C5 -58.3(3) . . . . ? P1 C1 C6 C5 171.64(17) . . . . ? C1 P1 C7 C12 177.58(18) . . . . ? C13 P1 C7 C12 68.66(19) . . . . ? Ru1 P1 C7 C12 -61.80(19) . . . . ? C1 P1 C7 C8 -55.63(19) . . . . ? C13 P1 C7 C8 -164.55(17) . . . . ? Ru1 P1 C7 C8 64.98(18) . . . . ? C12 C7 C8 C9 -58.2(3) . . . . ? P1 C7 C8 C9 173.43(17) . . . . ? C7 C8 C9 C10 55.6(3) . . . . ? C8 C9 C10 C11 -53.7(3) . . . . ? C9 C10 C11 C12 54.5(3) . . . . ? C10 C11 C12 C7 -56.7(3) . . . . ? C8 C7 C12 C11 58.4(3) . . . . ? P1 C7 C12 C11 -173.0(2) . . . . ? C1 P1 C13 C14 -81.05(18) . . . . ? C7 P1 C13 C14 26.25(19) . . . . ? Ru1 P1 C13 C14 152.71(14) . . . . ? C1 P1 C13 C18 150.30(17) . . . . ? C7 P1 C13 C18 -102.41(18) . . . . ? Ru1 P1 C13 C18 24.1(2) . . . . ? C18 C13 C14 C15 -59.4(3) . . . . ? P1 C13 C14 C15 168.91(18) . . . . ? C13 C14 C15 C16 57.7(3) . . . . ? C14 C15 C16 C17 -54.7(4) . . . . ? C15 C16 C17 C18 54.7(3) . . . . ? C16 C17 C18 C13 -57.3(3) . . . . ? C14 C13 C18 C17 59.0(3) . . . . ? P1 C13 C18 C17 -168.88(19) . . . . ? C35 Ru1 O21 C25 0.10(13) . . . . ? Cl2 Ru1 O21 C25 -110.32(12) . . . . ? Cl1 Ru1 O21 C25 103.24(12) . . . . ? C35 Ru1 O21 C22 165.8(2) . . . . ? Cl2 Ru1 O21 C22 55.38(18) . . . . ? Cl1 Ru1 O21 C22 -91.06(19) . . . . ? C25 O21 C22 C23 -165.0(2) . . . . ? Ru1 O21 C22 C23 30.9(3) . . . . ? C25 O21 C22 C24 72.4(3) . . . . ? Ru1 O21 C22 C24 -91.7(2) . . . . ? C22 O21 C25 C30 -169.39(19) . . . . ? Ru1 O21 C25 C30 -0.8(2) . . . . ? C22 O21 C25 C26 12.4(3) . . . . ? Ru1 O21 C25 C26 -179.0(2) . . . . ? O21 C25 C26 C27 177.7(2) . . . . ? C30 C25 C26 C27 -0.4(3) . . . . ? C25 C26 C27 O31 -177.2(2) . . . . ? C25 C26 C27 C28 0.3(4) . . . . ? O31 C27 C28 C29 176.7(3) . . . . ? C26 C27 C28 C29 -0.4(4) . . . . ? C27 C28 C29 C30 0.8(4) . . . . ? C27 C28 C29 C37 -178.6(2) . . . . ? O21 C25 C30 C29 -177.6(2) . . . . ? C26 C25 C30 C29 0.8(3) . . . . ? O21 C25 C30 C35 1.6(3) . . . . ? C26 C25 C30 C35 180.0(2) . . . . ? C28 C29 C30 C25 -1.0(3) . . . . ? C37 C29 C30 C25 178.5(2) . . . . ? C28 C29 C30 C35 179.7(2) . . . . ? C37 C29 C30 C35 -0.8(2) . . . . ? C26 C27 O31 C32A -167.5(3) . . . . ? C28 C27 O31 C32A 15.2(4) . . . . ? C27 O31 C32A C34A 73.7(5) . . . . ? C27 O31 C32A C33A -159.2(3) . . . . ? C25 C30 C35 C36 -178.7(2) . . . . ? C29 C30 C35 C36 0.5(2) . . . . ? C25 C30 C35 Ru1 -1.5(3) . . . . ? C29 C30 C35 Ru1 177.74(15) . . . . ? P1 Ru1 C35 C30 176.84(14) . . . . ? Cl2 Ru1 C35 C30 81.69(15) . . . . ? Cl1 Ru1 C35 C30 -82.09(15) . . . . ? O21 Ru1 C35 C30 0.61(15) . . . . ? P1 Ru1 C35 C36 -7.6(3) . . . . ? Cl2 Ru1 C35 C36 -102.7(3) . . . . ? Cl1 Ru1 C35 C36 93.5(3) . . . . ? O21 Ru1 C35 C36 176.2(3) . . . . ? C30 C35 C36 C37 0.0(2) . . . . ? Ru1 C35 C36 C37 -175.8(2) . . . . ? C35 C36 C37 C29 -0.5(3) . . . . ? C35 C36 C37 C38 177.6(2) . . . . ? C30 C29 C37 C36 0.8(3) . . . . ? C28 C29 C37 C36 -179.8(3) . . . . ? C30 C29 C37 C38 -177.4(2) . . . . ? C28 C29 C37 C38 2.0(4) . . . . ? C36 C37 C38 C39 -93.1(3) . . . . ? C29 C37 C38 C39 84.7(3) . . . . ? C36 C37 C38 C44 88.0(3) . . . . ? C29 C37 C38 C44 -94.2(3) . . . . ? C44 C38 C39 C41 -0.5(3) . . . . ? C37 C38 C39 C41 -179.5(2) . . . . ? C44 C38 C39 C40 179.6(2) . . . . ? C37 C38 C39 C40 0.7(3) . . . . ? C38 C39 C41 C42 -0.7(4) . . . . ? C40 C39 C41 C42 179.2(2) . . . . ? C39 C41 C42 C43 1.2(4) . . . . ? C41 C42 C43 C44 -0.6(4) . . . . ? C42 C43 C44 C38 -0.6(4) . . . . ? C42 C43 C44 C45 178.3(2) . . . . ? C39 C38 C44 C43 1.1(3) . . . . ? C37 C38 C44 C43 -179.9(2) . . . . ? C39 C38 C44 C45 -177.7(2) . . . . ? C37 C38 C44 C45 1.2(3) . . . . ?