# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound3 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C45 H45 Cl N2 O2 P2 Ru' _chemical_formula_weight 844.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2192(4) _cell_length_b 13.8275(6) _cell_length_c 14.7190(6) _cell_angle_alpha 105.817(2) _cell_angle_beta 93.474(2) _cell_angle_gamma 101.154(2) _cell_volume 1949.13(14) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9961 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 27.50 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.439 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 0.594 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7024 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33119 _diffrn_reflns_av_R_equivalents 0.0513 _diffrn_reflns_av_sigmaI/netI 0.0700 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 27.57 _reflns_number_total 8958 _reflns_number_gt 6406 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+0.7411P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8958 _refine_ls_number_parameters 476 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0748 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.0901 _refine_ls_wR_factor_gt 0.0798 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.71906(2) 0.745022(18) 0.703575(16) 0.01802(7) Uani 1 1 d . . . Cl1 Cl 0.73155(7) 0.62368(6) 0.55007(5) 0.02831(18) Uani 1 1 d . B . P1 P 0.77975(7) 0.63156(6) 0.78365(5) 0.01977(17) Uani 1 1 d . B . P2 P 0.64174(7) 0.84919(6) 0.62050(5) 0.01906(17) Uani 1 1 d . B . O2 O 0.2982(2) 0.68014(18) 0.92087(16) 0.0399(6) Uani 1 1 d . B . N1 N 0.7146(2) 0.88903(19) 0.88780(18) 0.0278(6) Uani 1 1 d . . . N2 N 0.5137(2) 0.7977(2) 0.84510(18) 0.0286(6) Uani 1 1 d . . . C1 C 0.6405(3) 0.8106(2) 0.8164(2) 0.0224(6) Uani 1 1 d . B . C2 C 0.8544(3) 0.9221(3) 0.8776(2) 0.0368(8) Uani 1 1 d . B . H2A H 0.9121 0.9034 0.9236 0.044 Uiso 1 1 calc R A 1 H2B H 0.8781 0.9977 0.8897 0.044 Uiso 1 1 calc R A 1 C5 C 0.6395(4) 0.9249(3) 0.9596(2) 0.0374(8) Uani 1 1 d . B . H5A H 0.6706 0.9793 1.0167 0.045 Uiso 1 1 calc R . . C6 C 0.5147(3) 0.8680(3) 0.9330(2) 0.0358(8) Uani 1 1 d . B . H6A H 0.4401 0.8744 0.9679 0.043 Uiso 1 1 calc R . . C7 C 0.3951(3) 0.7246(3) 0.7894(2) 0.0355(8) Uani 1 1 d . B . H7A H 0.4170 0.6941 0.7247 0.043 Uiso 1 1 calc R . . H7B H 0.3232 0.7620 0.7835 0.043 Uiso 1 1 calc R . . C8 C 0.3438(3) 0.6401(3) 0.8316(2) 0.0346(8) Uani 1 1 d . . . H8A H 0.2689 0.5895 0.7876 0.041 Uiso 1 1 calc R B . H8B H 0.4163 0.6040 0.8404 0.041 Uiso 1 1 calc R . . C9 C 0.2498(4) 0.5986(3) 0.9602(3) 0.0486(10) Uani 1 1 d . . . H9A H 0.2187 0.6267 1.0216 0.073 Uiso 1 1 calc R B . H9B H 0.3224 0.5638 0.9693 0.073 Uiso 1 1 calc R . . H9C H 0.1751 0.5492 0.9167 0.073 Uiso 1 1 calc R . . O1 O 0.9963(3) 0.8316(3) 0.7728(2) 0.0361(11) Uiso 0.676(6) 1 d P B 1 C3 C 0.8754(5) 0.8665(5) 0.7731(5) 0.0255(18) Uiso 0.676(6) 1 d P B 1 H3A H 0.8837 0.9182 0.7366 0.031 Uiso 0.676(6) 1 calc PR B 1 C4 C 1.1148(6) 0.9103(5) 0.8039(5) 0.0549(17) Uiso 0.676(6) 1 d P B 1 H4A H 1.1933 0.8791 0.8028 0.082 Uiso 0.676(6) 1 calc PR B 1 H4B H 1.1109 0.9519 0.8688 0.082 Uiso 0.676(6) 1 calc PR B 1 H4C H 1.1223 0.9543 0.7614 0.082 Uiso 0.676(6) 1 calc PR B 1 O1A O 0.9654(7) 0.9054(6) 0.7355(5) 0.050(3) Uiso 0.324(6) 1 d PD B 2 C3A C 0.8811(14) 0.8511(11) 0.7879(10) 0.039(5) Uiso 0.324(6) 1 d PD B 2 H3AA H 0.9379 0.8084 0.8096 0.046 Uiso 0.324(6) 1 calc PR B 2 C4A C 1.1059(10) 0.9404(12) 0.7726(10) 0.059(4) Uiso 0.324(6) 1 d PD B 2 H4AA H 1.1537 0.9768 0.7317 0.089 Uiso 0.324(6) 1 calc PR B 2 H4AB H 1.1441 0.8810 0.7740 0.089 Uiso 0.324(6) 1 calc PR B 2 H4AC H 1.1152 0.9870 0.8372 0.089 Uiso 0.324(6) 1 calc PR B 2 C10 C 0.6342(3) 0.5303(2) 0.7849(2) 0.0218(6) Uani 1 1 d . . . C11 C 0.5461(3) 0.4856(2) 0.7009(2) 0.0252(7) Uani 1 1 d . B . H11A H 0.5632 0.5081 0.6465 0.030 Uiso 1 1 calc R . . C12 C 0.4344(3) 0.4091(2) 0.6961(2) 0.0315(8) Uani 1 1 d . . . H12A H 0.3760 0.3789 0.6383 0.038 Uiso 1 1 calc R B . C13 C 0.4077(3) 0.3765(3) 0.7754(2) 0.0342(8) Uani 1 1 d . B . H13A H 0.3298 0.3251 0.7727 0.041 Uiso 1 1 calc R . . C14 C 0.4948(3) 0.4191(2) 0.8582(2) 0.0328(8) Uani 1 1 d . . . H14A H 0.4769 0.3964 0.9124 0.039 Uiso 1 1 calc R B . C15 C 0.6079(3) 0.4944(2) 0.8631(2) 0.0277(7) Uani 1 1 d . B . H15A H 0.6681 0.5219 0.9202 0.033 Uiso 1 1 calc R . . C16 C 0.9018(3) 0.5522(2) 0.73972(19) 0.0196(6) Uani 1 1 d . . . C17 C 0.9106(3) 0.4679(2) 0.7715(2) 0.0294(7) Uani 1 1 d . B . H17A H 0.8568 0.4530 0.8184 0.035 Uiso 1 1 calc R . . C18 C 0.9974(3) 0.4050(2) 0.7353(2) 0.0344(8) Uani 1 1 d . . . H18A H 1.0039 0.3479 0.7581 0.041 Uiso 1 1 calc R B . C19 C 1.0741(3) 0.4255(3) 0.6662(2) 0.0339(8) Uani 1 1 d . B . H19A H 1.1315 0.3814 0.6398 0.041 Uiso 1 1 calc R . . C20 C 1.0673(3) 0.5101(3) 0.6355(2) 0.0319(8) Uani 1 1 d . . . H20A H 1.1213 0.5249 0.5885 0.038 Uiso 1 1 calc R B . C21 C 0.9822(3) 0.5741(2) 0.6725(2) 0.0253(7) Uani 1 1 d . B . H21A H 0.9793 0.6330 0.6516 0.030 Uiso 1 1 calc R . . C22 C 0.8466(3) 0.6894(2) 0.9094(2) 0.0231(6) Uani 1 1 d . . . C23 C 0.7641(3) 0.7227(2) 0.9786(2) 0.0271(7) Uani 1 1 d . B . H23A H 0.6697 0.7084 0.9616 0.033 Uiso 1 1 calc R . . C24 C 0.8181(3) 0.7762(3) 1.0716(2) 0.0346(8) Uani 1 1 d . . . H24A H 0.7610 0.7980 1.1180 0.042 Uiso 1 1 calc R B . C25 C 0.9559(4) 0.7977(3) 1.0964(2) 0.0411(9) Uani 1 1 d . B . H25A H 0.9931 0.8337 1.1602 0.049 Uiso 1 1 calc R . . C26 C 1.0386(3) 0.7674(3) 1.0296(2) 0.0390(9) Uani 1 1 d . . . H26A H 1.1331 0.7839 1.0468 0.047 Uiso 1 1 calc R B . C27 C 0.9847(3) 0.7126(2) 0.9366(2) 0.0315(8) Uani 1 1 d . B . H27A H 1.0428 0.6908 0.8909 0.038 Uiso 1 1 calc R . . C28 C 0.4611(3) 0.8051(2) 0.5776(2) 0.0213(6) Uani 1 1 d . . . C29 C 0.4124(3) 0.7008(2) 0.5301(2) 0.0255(7) Uani 1 1 d . B . H29A H 0.4730 0.6559 0.5181 0.031 Uiso 1 1 calc R . . C30 C 0.2768(3) 0.6622(2) 0.5004(2) 0.0295(7) Uani 1 1 d . . . H30A H 0.2451 0.5916 0.4663 0.035 Uiso 1 1 calc R B . C31 C 0.1873(3) 0.7259(3) 0.5200(2) 0.0345(8) Uani 1 1 d . B . H31A H 0.0938 0.6987 0.5014 0.041 Uiso 1 1 calc R . . C32 C 0.2336(3) 0.8289(3) 0.5665(2) 0.0380(8) Uani 1 1 d . . . H32A H 0.1721 0.8729 0.5798 0.046 Uiso 1 1 calc R B . C33 C 0.3702(3) 0.8688(2) 0.5940(2) 0.0314(8) Uani 1 1 d . B . H33A H 0.4017 0.9405 0.6243 0.038 Uiso 1 1 calc R . . C34 C 0.7191(3) 0.8548(2) 0.5123(2) 0.0199(6) Uani 1 1 d . . . C35 C 0.6504(3) 0.8675(2) 0.4333(2) 0.0261(7) Uani 1 1 d . B . H35A H 0.5574 0.8680 0.4320 0.031 Uiso 1 1 calc R . . C36 C 0.7171(3) 0.8793(2) 0.3565(2) 0.0320(7) Uani 1 1 d . . . H36A H 0.6701 0.8887 0.3030 0.038 Uiso 1 1 calc R B . C37 C 0.8514(3) 0.8776(3) 0.3576(2) 0.0362(8) Uani 1 1 d . B . H37A H 0.8969 0.8864 0.3051 0.043 Uiso 1 1 calc R . . C38 C 0.9200(3) 0.8631(3) 0.4346(2) 0.0331(8) Uani 1 1 d . . . H38A H 1.0124 0.8612 0.4348 0.040 Uiso 1 1 calc R B . C39 C 0.8543(3) 0.8513(2) 0.5114(2) 0.0268(7) Uani 1 1 d . B . H39A H 0.9017 0.8407 0.5641 0.032 Uiso 1 1 calc R . . C40 C 0.6569(3) 0.9880(2) 0.6802(2) 0.0211(6) Uani 1 1 d . . . C41 C 0.5982(3) 1.0189(2) 0.7636(2) 0.0270(7) Uani 1 1 d . B . H41A H 0.5534 0.9684 0.7905 0.032 Uiso 1 1 calc R . . C42 C 0.6046(3) 1.1224(3) 0.8075(2) 0.0315(8) Uani 1 1 d . . . H42A H 0.5651 1.1422 0.8646 0.038 Uiso 1 1 calc R B . C43 C 0.6678(3) 1.1965(2) 0.7691(2) 0.0347(8) Uani 1 1 d . B . H43A H 0.6712 1.2673 0.7987 0.042 Uiso 1 1 calc R . . C44 C 0.7260(3) 1.1665(2) 0.6871(3) 0.0385(8) Uani 1 1 d . . . H44A H 0.7703 1.2172 0.6602 0.046 Uiso 1 1 calc R B . C45 C 0.7208(3) 1.0641(2) 0.6436(2) 0.0307(7) Uani 1 1 d . B . H45A H 0.7622 1.0452 0.5872 0.037 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 0.02321(11) 0.01614(13) 0.01562(13) 0.00363(10) 0.00458(8) 0.00718(9) Cl1 0.0441(4) 0.0258(4) 0.0181(4) 0.0035(3) 0.0055(3) 0.0186(3) P1 0.0248(3) 0.0201(4) 0.0155(4) 0.0037(3) 0.0025(3) 0.0098(3) P2 0.0256(3) 0.0159(4) 0.0175(4) 0.0050(3) 0.0059(3) 0.0075(3) O2 0.0479(13) 0.0453(16) 0.0345(14) 0.0165(12) 0.0210(11) 0.0172(12) N1 0.0374(14) 0.0226(15) 0.0237(15) 0.0045(12) 0.0021(11) 0.0103(11) N2 0.0372(13) 0.0303(16) 0.0246(15) 0.0093(12) 0.0136(11) 0.0174(12) C1 0.0321(15) 0.0178(16) 0.0206(16) 0.0071(13) 0.0046(12) 0.0105(12) C2 0.0412(18) 0.0231(19) 0.040(2) 0.0042(16) -0.0019(15) 0.0018(14) C5 0.063(2) 0.031(2) 0.0217(18) 0.0018(15) 0.0116(16) 0.0233(18) C6 0.051(2) 0.037(2) 0.0277(19) 0.0090(16) 0.0179(16) 0.0249(17) C7 0.0290(15) 0.051(2) 0.0302(19) 0.0150(17) 0.0060(14) 0.0118(15) C8 0.0310(16) 0.045(2) 0.0279(19) 0.0094(17) 0.0070(14) 0.0091(15) C9 0.054(2) 0.060(3) 0.044(2) 0.028(2) 0.0163(18) 0.018(2) C10 0.0234(13) 0.0196(16) 0.0237(17) 0.0048(13) 0.0066(12) 0.0091(12) C11 0.0264(14) 0.0289(18) 0.0209(17) 0.0047(14) 0.0054(12) 0.0103(13) C12 0.0316(15) 0.032(2) 0.0251(18) -0.0007(15) 0.0009(13) 0.0059(14) C13 0.0337(16) 0.0271(19) 0.038(2) 0.0055(16) 0.0084(15) 0.0024(14) C14 0.0406(17) 0.030(2) 0.032(2) 0.0147(16) 0.0096(15) 0.0087(15) C15 0.0301(15) 0.0248(18) 0.0287(18) 0.0086(15) 0.0026(13) 0.0062(13) C16 0.0243(13) 0.0174(16) 0.0151(15) 0.0000(12) -0.0007(11) 0.0077(11) C17 0.0294(15) 0.0261(18) 0.0354(19) 0.0113(15) 0.0069(13) 0.0077(13) C18 0.0311(16) 0.0220(18) 0.050(2) 0.0089(16) 0.0005(15) 0.0094(14) C19 0.0230(14) 0.0278(19) 0.043(2) -0.0069(16) -0.0016(14) 0.0121(13) C20 0.0245(14) 0.043(2) 0.0272(18) 0.0045(16) 0.0062(13) 0.0124(14) C21 0.0245(13) 0.0259(18) 0.0261(17) 0.0062(14) 0.0017(12) 0.0096(12) C22 0.0337(15) 0.0184(16) 0.0173(16) 0.0043(13) 0.0016(12) 0.0074(12) C23 0.0358(16) 0.0250(18) 0.0227(17) 0.0086(14) 0.0057(13) 0.0085(13) C24 0.056(2) 0.033(2) 0.0171(17) 0.0064(15) 0.0115(15) 0.0115(16) C25 0.060(2) 0.036(2) 0.0187(18) -0.0023(16) -0.0059(16) 0.0080(17) C26 0.0406(18) 0.040(2) 0.029(2) 0.0026(17) -0.0075(15) 0.0074(16) C27 0.0336(16) 0.034(2) 0.0262(18) 0.0056(15) -0.0001(13) 0.0111(14) C28 0.0272(14) 0.0213(17) 0.0183(16) 0.0078(13) 0.0071(12) 0.0081(12) C29 0.0311(15) 0.0222(17) 0.0237(17) 0.0042(14) 0.0075(12) 0.0092(13) C30 0.0383(16) 0.0185(17) 0.0261(18) 0.0020(14) 0.0024(14) 0.0000(13) C31 0.0292(15) 0.036(2) 0.035(2) 0.0077(17) 0.0019(14) 0.0037(14) C32 0.0301(16) 0.032(2) 0.051(2) 0.0054(17) 0.0005(15) 0.0156(14) C33 0.0320(15) 0.0219(18) 0.039(2) 0.0055(15) -0.0011(14) 0.0089(13) C34 0.0274(13) 0.0126(15) 0.0203(16) 0.0037(12) 0.0063(12) 0.0061(11) C35 0.0317(15) 0.0211(17) 0.0271(18) 0.0064(14) 0.0045(13) 0.0098(13) C36 0.0518(19) 0.0286(19) 0.0191(17) 0.0077(15) 0.0063(14) 0.0156(15) C37 0.0481(19) 0.035(2) 0.0288(19) 0.0116(16) 0.0203(16) 0.0088(16) C38 0.0296(15) 0.037(2) 0.036(2) 0.0110(16) 0.0134(14) 0.0117(14) C39 0.0303(15) 0.0274(18) 0.0248(17) 0.0096(14) 0.0067(13) 0.0073(13) C40 0.0237(13) 0.0192(16) 0.0201(16) 0.0043(13) 0.0014(11) 0.0061(12) C41 0.0396(16) 0.0238(18) 0.0241(17) 0.0108(14) 0.0084(13) 0.0149(14) C42 0.0460(18) 0.033(2) 0.0173(17) 0.0005(15) 0.0044(14) 0.0227(16) C43 0.0447(18) 0.0172(18) 0.037(2) -0.0004(16) -0.0042(15) 0.0084(14) C44 0.0493(19) 0.0172(18) 0.042(2) 0.0022(16) 0.0108(16) -0.0016(15) C45 0.0348(16) 0.0203(18) 0.0316(19) 0.0000(15) 0.0098(14) 0.0018(13) _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 C1 1.961(3) . ? Ru1 C3 2.061(6) . ? Ru1 C3A 2.062(14) . ? Ru1 P2 2.3405(8) . ? Ru1 P1 2.3518(8) . ? Ru1 Cl1 2.4470(8) . ? P1 C22 1.833(3) . ? P1 C10 1.840(3) . ? P1 C16 1.849(3) . ? P2 C34 1.834(3) . ? P2 C28 1.842(3) . ? P2 C40 1.852(3) . ? O2 C9 1.423(4) . ? O2 C8 1.425(4) . ? N1 C1 1.349(4) . ? N1 C5 1.383(4) . ? N1 C2 1.444(4) . ? N2 C1 1.381(3) . ? N2 C6 1.388(4) . ? N2 C7 1.455(4) . ? C2 C3A 1.491(15) . ? C2 C3 1.569(7) . ? C5 C6 1.335(5) . ? C7 C8 1.492(5) . ? O1 C3 1.411(7) . ? O1 C4 1.418(7) . ? O1A C3A 1.430(9) . ? O1A C4A 1.444(9) . ? C10 C15 1.393(4) . ? C10 C11 1.398(4) . ? C11 C12 1.381(4) . ? C12 C13 1.386(4) . ? C13 C14 1.377(4) . ? C14 C15 1.382(4) . ? C16 C21 1.383(4) . ? C16 C17 1.385(4) . ? C17 C18 1.391(4) . ? C18 C19 1.377(5) . ? C19 C20 1.376(5) . ? C20 C21 1.389(4) . ? C22 C27 1.394(4) . ? C22 C23 1.400(4) . ? C23 C24 1.387(4) . ? C24 C25 1.386(5) . ? C25 C26 1.368(5) . ? C26 C27 1.391(4) . ? C28 C33 1.388(4) . ? C28 C29 1.395(4) . ? C29 C30 1.382(4) . ? C30 C31 1.379(4) . ? C31 C32 1.374(5) . ? C32 C33 1.388(4) . ? C34 C35 1.391(4) . ? C34 C39 1.393(4) . ? C35 C36 1.386(4) . ? C36 C37 1.376(4) . ? C37 C38 1.378(4) . ? C38 C39 1.380(4) . ? C40 C45 1.381(4) . ? C40 C41 1.398(4) . ? C41 C42 1.387(4) . ? C42 C43 1.376(5) . ? C43 C44 1.375(5) . ? C44 C45 1.376(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru1 C3 78.63(19) . . ? C1 Ru1 C3A 76.8(4) . . ? C3 Ru1 C3A 9.8(4) . . ? C1 Ru1 P2 90.74(8) . . ? C3 Ru1 P2 89.5(2) . . ? C3A Ru1 P2 99.1(4) . . ? C1 Ru1 P1 88.77(8) . . ? C3 Ru1 P1 94.8(2) . . ? C3A Ru1 P1 85.2(4) . . ? P2 Ru1 P1 175.44(3) . . ? C1 Ru1 Cl1 158.45(9) . . ? C3 Ru1 Cl1 122.87(17) . . ? C3A Ru1 Cl1 124.6(4) . . ? P2 Ru1 Cl1 88.18(3) . . ? P1 Ru1 Cl1 90.62(3) . . ? C22 P1 C10 104.01(13) . . ? C22 P1 C16 101.73(13) . . ? C10 P1 C16 100.34(13) . . ? C22 P1 Ru1 115.84(10) . . ? C10 P1 Ru1 111.35(9) . . ? C16 P1 Ru1 121.23(10) . . ? C34 P2 C28 103.34(13) . . ? C34 P2 C40 100.77(13) . . ? C28 P2 C40 102.30(12) . . ? C34 P2 Ru1 115.69(9) . . ? C28 P2 Ru1 112.52(9) . . ? C40 P2 Ru1 120.01(9) . . ? C9 O2 C8 109.9(3) . . ? C1 N1 C5 112.1(3) . . ? C1 N1 C2 116.9(2) . . ? C5 N1 C2 130.9(3) . . ? C1 N2 C6 110.0(3) . . ? C1 N2 C7 125.0(3) . . ? C6 N2 C7 124.9(3) . . ? N1 C1 N2 103.7(2) . . ? N1 C1 Ru1 121.5(2) . . ? N2 C1 Ru1 134.8(2) . . ? N1 C2 C3A 107.0(5) . . ? N1 C2 C3 107.3(3) . . ? C3A C2 C3 12.9(6) . . ? C6 C5 N1 106.4(3) . . ? C5 C6 N2 107.6(3) . . ? N2 C7 C8 113.4(3) . . ? O2 C8 C7 110.6(3) . . ? C3 O1 C4 115.1(4) . . ? O1 C3 C2 110.1(4) . . ? O1 C3 Ru1 109.4(4) . . ? C2 C3 Ru1 113.7(3) . . ? C3A O1A C4A 116.4(10) . . ? O1A C3A C2 111.6(10) . . ? O1A C3A Ru1 113.0(9) . . ? C2 C3A Ru1 117.4(7) . . ? C15 C10 C11 118.3(3) . . ? C15 C10 P1 124.3(2) . . ? C11 C10 P1 117.3(2) . . ? C12 C11 C10 120.9(3) . . ? C11 C12 C13 120.0(3) . . ? C14 C13 C12 119.6(3) . . ? C13 C14 C15 120.7(3) . . ? C14 C15 C10 120.4(3) . . ? C21 C16 C17 119.1(3) . . ? C21 C16 P1 120.5(2) . . ? C17 C16 P1 120.3(2) . . ? C16 C17 C18 120.6(3) . . ? C19 C18 C17 119.8(3) . . ? C20 C19 C18 119.8(3) . . ? C19 C20 C21 120.5(3) . . ? C16 C21 C20 120.1(3) . . ? C27 C22 C23 117.9(3) . . ? C27 C22 P1 120.0(2) . . ? C23 C22 P1 121.6(2) . . ? C24 C23 C22 121.0(3) . . ? C25 C24 C23 119.6(3) . . ? C26 C25 C24 120.4(3) . . ? C25 C26 C27 120.2(3) . . ? C26 C27 C22 120.9(3) . . ? C33 C28 C29 118.4(3) . . ? C33 C28 P2 123.6(2) . . ? C29 C28 P2 117.9(2) . . ? C30 C29 C28 120.6(3) . . ? C31 C30 C29 120.3(3) . . ? C32 C31 C30 119.8(3) . . ? C31 C32 C33 120.2(3) . . ? C28 C33 C32 120.6(3) . . ? C35 C34 C39 118.9(3) . . ? C35 C34 P2 122.8(2) . . ? C39 C34 P2 118.2(2) . . ? C36 C35 C34 120.2(3) . . ? C37 C36 C35 120.2(3) . . ? C36 C37 C38 120.3(3) . . ? C37 C38 C39 119.9(3) . . ? C38 C39 C34 120.6(3) . . ? C45 C40 C41 117.6(3) . . ? C45 C40 P2 122.5(2) . . ? C41 C40 P2 119.9(2) . . ? C42 C41 C40 120.7(3) . . ? C43 C42 C41 120.5(3) . . ? C44 C43 C42 118.9(3) . . ? C43 C44 C45 120.8(3) . . ? C44 C45 C40 121.4(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.466 _refine_diff_density_min -0.573 _refine_diff_density_rms 0.089 _database_code_depnum_ccdc_archive 'CCDC 973557' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound4 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C52.50 H58 Cl N2 O2 P2 Ru' _chemical_formula_weight 947.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 13.009(3) _cell_length_b 18.484(4) _cell_length_c 20.315(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.490(12) _cell_angle_gamma 90.00 _cell_volume 4729.4(19) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8984 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 27.53 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.331 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1976 _exptl_absorpt_coefficient_mu 0.497 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8451 _exptl_absorpt_correction_T_max 0.9070 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 77428 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_unetI/netI 0.0313 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 27.54 _reflns_number_total 10871 _reflns_number_gt 8829 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0664P)^2^+11.1804P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10871 _refine_ls_number_parameters 528 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0657 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1463 _refine_ls_wR_factor_gt 0.1364 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.82310(2) 0.307090(14) 0.918455(13) 0.02238(9) Uani 1 1 d . . . Cl1 Cl 0.94342(7) 0.33869(5) 1.02857(4) 0.0320(2) Uani 1 1 d . . . P1 P 0.68402(7) 0.35922(5) 0.95781(4) 0.02512(19) Uani 1 1 d . . . P2 P 0.96649(7) 0.27779(5) 0.87437(4) 0.02476(19) Uani 1 1 d . . . O1 O 0.7456(3) 0.42397(17) 0.67732(15) 0.0497(8) Uani 1 1 d . . . O2 O 0.7159(3) 0.1853(2) 0.96954(19) 0.0614(9) Uani 1 1 d . . . N1 N 0.6888(2) 0.22365(16) 0.80996(15) 0.0283(6) Uani 1 1 d . . . N2 N 0.6673(2) 0.33314(16) 0.77507(14) 0.0258(6) Uani 1 1 d . . . C1 C 0.7125(3) 0.45598(19) 0.96878(17) 0.0259(7) Uani 1 1 d . . . C2 C 0.7903(3) 0.4839(2) 0.93994(17) 0.0267(7) Uani 1 1 d . . . H2A H 0.8267 0.4524 0.9165 0.032 Uiso 1 1 calc R . . C3 C 0.8159(3) 0.5570(2) 0.94475(19) 0.0345(8) Uani 1 1 d . . . H3A H 0.8689 0.5753 0.9244 0.041 Uiso 1 1 calc R . . C4 C 0.7643(4) 0.6026(2) 0.9789(2) 0.0419(10) Uani 1 1 d . . . H4A H 0.7815 0.6526 0.9822 0.050 Uiso 1 1 calc R . . C5 C 0.6871(4) 0.5761(2) 1.0087(2) 0.0446(10) Uani 1 1 d . . . H5A H 0.6513 0.6081 1.0321 0.054 Uiso 1 1 calc R . . C6 C 0.6619(3) 0.5031(2) 1.0046(2) 0.0366(9) Uani 1 1 d . . . H6A H 0.6102 0.4851 1.0261 0.044 Uiso 1 1 calc R . . C7 C 0.5515(3) 0.3565(2) 0.89902(19) 0.0339(8) Uani 1 1 d . . . C8 C 0.4937(3) 0.4182(3) 0.8732(2) 0.0446(10) Uani 1 1 d . . . H8A H 0.5205 0.4647 0.8886 0.054 Uiso 1 1 calc R . . C9 C 0.3963(4) 0.4122(4) 0.8249(3) 0.0622(15) Uani 1 1 d . . . H9A H 0.3565 0.4544 0.8082 0.075 Uiso 1 1 calc R . . C10 C 0.3584(4) 0.3451(4) 0.8016(3) 0.0650(16) Uani 1 1 d . . . H10A H 0.2929 0.3412 0.7683 0.078 Uiso 1 1 calc R . . C11 C 0.4141(4) 0.2838(3) 0.8260(2) 0.0568(14) Uani 1 1 d . . . H11A H 0.3867 0.2376 0.8100 0.068 Uiso 1 1 calc R . . C12 C 0.5104(3) 0.2891(3) 0.8742(2) 0.0432(10) Uani 1 1 d . . . H12A H 0.5490 0.2464 0.8907 0.052 Uiso 1 1 calc R . . C13 C 0.6561(3) 0.3352(2) 1.03943(19) 0.0323(8) Uani 1 1 d . . . C14 C 0.7299(4) 0.3546(3) 1.0990(2) 0.0513(12) Uani 1 1 d . . . H14A H 0.7912 0.3814 1.0967 0.062 Uiso 1 1 calc R . . C15 C 0.7146(4) 0.3352(3) 1.1617(2) 0.0610(14) Uani 1 1 d . . . H15A H 0.7661 0.3480 1.2021 0.073 Uiso 1 1 calc R . . C16 C 0.6252(4) 0.2976(3) 1.1659(3) 0.0570(13) Uani 1 1 d . . . H16A H 0.6153 0.2834 1.2088 0.068 Uiso 1 1 calc R . . C17 C 0.5517(4) 0.2812(3) 1.1082(3) 0.0585(13) Uani 1 1 d . . . H17A H 0.4894 0.2558 1.1109 0.070 Uiso 1 1 calc R . . C18 C 0.5654(3) 0.3007(3) 1.0448(2) 0.0464(11) Uani 1 1 d . . . H18A H 0.5114 0.2900 1.0049 0.056 Uiso 1 1 calc R . . C19 C 0.7226(3) 0.29183(18) 0.82833(18) 0.0254(7) Uani 1 1 d . . . C20 C 0.6152(3) 0.2206(2) 0.74780(18) 0.0316(8) Uani 1 1 d . . . C21 C 0.6006(3) 0.2896(2) 0.72564(18) 0.0311(8) Uani 1 1 d . . . C22 C 0.6720(3) 0.41164(19) 0.77270(19) 0.0315(8) Uani 1 1 d . . . H22A H 0.6781 0.4307 0.8191 0.038 Uiso 1 1 calc R . . H22B H 0.6042 0.4296 0.7434 0.038 Uiso 1 1 calc R . . C23 C 0.7616(3) 0.4418(2) 0.74683(19) 0.0335(8) Uani 1 1 d . . . H23A H 0.7645 0.4950 0.7525 0.040 Uiso 1 1 calc R . . H23B H 0.8298 0.4213 0.7732 0.040 Uiso 1 1 calc R . . C24 C 0.8230(5) 0.4549(3) 0.6486(3) 0.0612(14) Uani 1 1 d . . . H24A H 0.8088 0.4414 0.6006 0.092 Uiso 1 1 calc R . . H24B H 0.8934 0.4372 0.6728 0.092 Uiso 1 1 calc R . . H24C H 0.8209 0.5077 0.6526 0.092 Uiso 1 1 calc R . . C25 C 0.5256(3) 0.3201(2) 0.6636(2) 0.0410(9) Uani 1 1 d . . . H25A H 0.4866 0.2806 0.6361 0.062 Uiso 1 1 calc R . . H25B H 0.5657 0.3471 0.6368 0.062 Uiso 1 1 calc R . . H25C H 0.4752 0.3527 0.6774 0.062 Uiso 1 1 calc R . . C26 C 0.5666(4) 0.1512(2) 0.7176(2) 0.0471(11) Uani 1 1 d . . . H26A H 0.5168 0.1609 0.6736 0.071 Uiso 1 1 calc R . . H26B H 0.5286 0.1287 0.7482 0.071 Uiso 1 1 calc R . . H26C H 0.6225 0.1185 0.7111 0.071 Uiso 1 1 calc R . . C27 C 0.7307(3) 0.1662(2) 0.8579(2) 0.0345(8) Uani 1 1 d . . . H27A H 0.7818 0.1366 0.8406 0.041 Uiso 1 1 calc R . . H27B H 0.6722 0.1344 0.8634 0.041 Uiso 1 1 calc R . . C28 C 0.7854(3) 0.1992(2) 0.9253(2) 0.0345(8) Uani 1 1 d . . . H28A H 0.8530 0.1721 0.9436 0.041 Uiso 1 1 calc R . . C29 C 0.7745(6) 0.1808(3) 1.0405(3) 0.0738(17) Uani 1 1 d . . . H29A H 0.7251 0.1713 1.0689 0.111 Uiso 1 1 calc R . . H29B H 0.8116 0.2265 1.0544 0.111 Uiso 1 1 calc R . . H29C H 0.8264 0.1413 1.0462 0.111 Uiso 1 1 calc R . . C30 C 1.0179(3) 0.35940(19) 0.84222(18) 0.0261(7) Uani 1 1 d . . . C31 C 1.0290(3) 0.42056(19) 0.88361(19) 0.0300(7) Uani 1 1 d . . . H31A H 1.0082 0.4184 0.9252 0.036 Uiso 1 1 calc R . . C32 C 1.0700(3) 0.4847(2) 0.8649(2) 0.0375(9) Uani 1 1 d . . . H32A H 1.0770 0.5260 0.8935 0.045 Uiso 1 1 calc R . . C33 C 1.1002(4) 0.4879(2) 0.8046(2) 0.0441(10) Uani 1 1 d . . . H33A H 1.1288 0.5314 0.7916 0.053 Uiso 1 1 calc R . . C34 C 1.0889(4) 0.4274(2) 0.7628(2) 0.0462(10) Uani 1 1 d . . . H34A H 1.1091 0.4298 0.7210 0.055 Uiso 1 1 calc R . . C35 C 1.0485(3) 0.3638(2) 0.7816(2) 0.0387(9) Uani 1 1 d . . . H35A H 1.0415 0.3227 0.7527 0.046 Uiso 1 1 calc R . . C36 C 0.9446(3) 0.21409(19) 0.80314(18) 0.0281(7) Uani 1 1 d . . . C37 C 0.8721(3) 0.2308(2) 0.74135(19) 0.0325(8) Uani 1 1 d . . . H37A H 0.8409 0.2776 0.7348 0.039 Uiso 1 1 calc R . . C38 C 0.8454(3) 0.1801(2) 0.6898(2) 0.0401(9) Uani 1 1 d . . . H38A H 0.7951 0.1918 0.6485 0.048 Uiso 1 1 calc R . . C39 C 0.8921(3) 0.1123(2) 0.6983(2) 0.0435(10) Uani 1 1 d . . . H39A H 0.8747 0.0777 0.6626 0.052 Uiso 1 1 calc R . . C40 C 0.9639(3) 0.0948(2) 0.7586(2) 0.0423(10) Uani 1 1 d . . . H40A H 0.9955 0.0481 0.7644 0.051 Uiso 1 1 calc R . . C41 C 0.9902(3) 0.1453(2) 0.8110(2) 0.0343(8) Uani 1 1 d . . . H41A H 1.0395 0.1328 0.8524 0.041 Uiso 1 1 calc R . . C42 C 1.0907(3) 0.24175(18) 0.92890(18) 0.0269(7) Uani 1 1 d . . . C43 C 1.0908(3) 0.2086(2) 0.9903(2) 0.0355(8) Uani 1 1 d . . . H43A H 1.0267 0.2045 1.0044 0.043 Uiso 1 1 calc R . . C44 C 1.1852(3) 0.1812(2) 1.0311(2) 0.0451(10) Uani 1 1 d . . . H44A H 1.1853 0.1592 1.0734 0.054 Uiso 1 1 calc R . . C45 C 1.2780(3) 0.1857(2) 1.0109(2) 0.0446(10) Uani 1 1 d . . . H45A H 1.3418 0.1664 1.0388 0.054 Uiso 1 1 calc R . . C46 C 1.2787(3) 0.2182(2) 0.9501(2) 0.0397(9) Uani 1 1 d . . . H46A H 1.3431 0.2216 0.9363 0.048 Uiso 1 1 calc R . . C47 C 1.1858(3) 0.2460(2) 0.9091(2) 0.0313(8) Uani 1 1 d . . . H47A H 1.1868 0.2682 0.8670 0.038 Uiso 1 1 calc R . . C81 C 1.022(2) 0.5750(17) 0.5789(13) 0.262(18) Uiso 0.50 1 d PD A -1 H81A H 1.0885 0.5687 0.6139 0.392 Uiso 0.50 1 calc PR A -1 H81B H 0.9619 0.5718 0.5998 0.392 Uiso 0.50 1 calc PR A -1 H81C H 1.0217 0.6225 0.5575 0.392 Uiso 0.50 1 calc PR A -1 C82 C 1.012(2) 0.5162(17) 0.5254(14) 0.240(17) Uiso 0.50 1 d PD A -1 H82A H 1.0120 0.4681 0.5469 0.287 Uiso 0.50 1 calc PR A -1 H82B H 1.0740 0.5183 0.5053 0.287 Uiso 0.50 1 calc PR A -1 C83 C 0.9093(15) 0.5260(12) 0.4693(11) 0.197(12) Uiso 0.50 1 d PD A -1 H83A H 0.9072 0.5750 0.4493 0.236 Uiso 0.50 1 calc PR A -1 H83B H 0.8470 0.5206 0.4886 0.236 Uiso 0.50 1 calc PR A -1 C84 C 0.9061(19) 0.4683(17) 0.4141(13) 0.247(17) Uiso 0.50 1 d PD A -1 H84A H 0.9590 0.4801 0.3881 0.296 Uiso 0.50 1 calc PR A -1 H84B H 0.9240 0.4203 0.4356 0.296 Uiso 0.50 1 calc PR A -1 C85 C 0.795(2) 0.4661(17) 0.3661(13) 0.241(15) Uiso 0.50 1 d PD A -1 H85A H 0.7920 0.4281 0.3320 0.362 Uiso 0.50 1 calc PR A -1 H85B H 0.7790 0.5130 0.3433 0.362 Uiso 0.50 1 calc PR A -1 H85C H 0.7427 0.4558 0.3922 0.362 Uiso 0.50 1 calc PR A -1 C90 C 1.0470(12) -0.0027(8) 0.9442(8) 0.191(6) Uiso 1 1 d D . . H90A H 1.0801 -0.0047 0.9075 0.229 Uiso 1 1 calc R . . C91 C 0.9375(12) 0.0099(9) 0.9320(7) 0.219(7) Uiso 1 1 d D . . H91A H 0.8954 0.0165 0.8869 0.263 Uiso 1 1 calc R . . C92 C 0.8916(11) 0.0125(8) 0.9869(9) 0.193(6) Uiso 1 1 d D . . H92A H 0.8174 0.0210 0.9786 0.232 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 0.02203(14) 0.02417(14) 0.01989(14) -0.00159(10) 0.00326(10) -0.00080(10) Cl1 0.0289(4) 0.0391(5) 0.0239(4) -0.0025(3) -0.0010(3) 0.0002(4) P1 0.0206(4) 0.0325(5) 0.0226(4) -0.0015(3) 0.0059(3) -0.0052(3) P2 0.0248(4) 0.0262(4) 0.0226(4) -0.0008(3) 0.0046(3) 0.0020(3) O1 0.067(2) 0.0498(18) 0.0368(16) -0.0108(14) 0.0217(15) -0.0205(15) O2 0.065(2) 0.063(2) 0.056(2) 0.0057(17) 0.0138(18) -0.0136(17) N1 0.0310(15) 0.0248(14) 0.0271(15) -0.0038(12) 0.0037(12) -0.0033(12) N2 0.0257(14) 0.0263(14) 0.0227(14) -0.0041(11) 0.0012(11) 0.0008(11) C1 0.0207(15) 0.0319(17) 0.0236(17) -0.0029(13) 0.0029(13) 0.0008(13) C2 0.0214(15) 0.0350(18) 0.0221(16) 0.0007(14) 0.0023(13) -0.0004(13) C3 0.0351(19) 0.037(2) 0.0253(18) 0.0048(15) -0.0032(15) -0.0086(16) C4 0.055(3) 0.0286(19) 0.031(2) -0.0011(16) -0.0093(18) -0.0013(18) C5 0.055(3) 0.037(2) 0.037(2) -0.0086(17) 0.0022(19) 0.0160(19) C6 0.0325(19) 0.043(2) 0.035(2) -0.0050(17) 0.0103(16) 0.0051(16) C7 0.0216(16) 0.054(2) 0.0253(18) -0.0014(16) 0.0049(14) -0.0076(16) C8 0.0279(19) 0.068(3) 0.036(2) 0.007(2) 0.0058(17) 0.0012(19) C9 0.031(2) 0.107(5) 0.044(3) 0.016(3) 0.003(2) 0.002(3) C10 0.027(2) 0.121(5) 0.042(3) 0.002(3) 0.0006(19) -0.015(3) C11 0.034(2) 0.094(4) 0.043(3) -0.015(3) 0.012(2) -0.029(3) C12 0.0297(19) 0.065(3) 0.035(2) -0.011(2) 0.0099(17) -0.0157(19) C13 0.0288(18) 0.043(2) 0.0273(18) 0.0004(16) 0.0117(15) -0.0063(16) C14 0.048(3) 0.069(3) 0.037(2) 0.000(2) 0.013(2) -0.020(2) C15 0.061(3) 0.090(4) 0.033(2) 0.006(2) 0.013(2) -0.020(3) C16 0.069(3) 0.069(3) 0.041(3) 0.005(2) 0.028(2) -0.022(3) C17 0.053(3) 0.077(4) 0.055(3) -0.001(3) 0.031(2) -0.024(3) C18 0.036(2) 0.067(3) 0.040(2) 0.000(2) 0.0170(18) -0.012(2) C19 0.0240(16) 0.0273(17) 0.0255(17) -0.0015(13) 0.0076(13) -0.0002(13) C20 0.0332(19) 0.0353(19) 0.0249(18) -0.0101(15) 0.0051(15) -0.0063(15) C21 0.0275(17) 0.039(2) 0.0246(18) -0.0099(15) 0.0020(14) -0.0041(15) C22 0.0348(19) 0.0275(18) 0.0295(19) -0.0030(14) 0.0031(15) 0.0051(14) C23 0.041(2) 0.0263(17) 0.0307(19) -0.0035(14) 0.0054(16) 0.0008(15) C24 0.089(4) 0.047(3) 0.058(3) -0.008(2) 0.037(3) -0.025(3) C25 0.037(2) 0.051(2) 0.029(2) -0.0055(17) -0.0025(16) 0.0016(18) C26 0.052(3) 0.041(2) 0.043(2) -0.0128(19) 0.001(2) -0.017(2) C27 0.035(2) 0.0284(18) 0.039(2) 0.0030(16) 0.0080(16) -0.0034(15) C28 0.041(2) 0.0286(18) 0.032(2) 0.0011(15) 0.0061(16) -0.0043(15) C29 0.097(5) 0.073(4) 0.046(3) 0.013(3) 0.008(3) -0.013(3) C30 0.0246(16) 0.0267(16) 0.0276(17) 0.0032(13) 0.0079(13) 0.0048(13) C31 0.0247(16) 0.0312(18) 0.0322(19) -0.0008(15) 0.0036(14) 0.0049(14) C32 0.035(2) 0.0310(19) 0.045(2) 0.0004(17) 0.0067(17) 0.0034(15) C33 0.047(2) 0.031(2) 0.056(3) 0.0093(18) 0.016(2) 0.0012(17) C34 0.055(3) 0.044(2) 0.047(3) 0.0107(19) 0.026(2) 0.006(2) C35 0.048(2) 0.034(2) 0.039(2) 0.0031(17) 0.0213(18) 0.0075(17) C36 0.0260(17) 0.0298(17) 0.0292(18) -0.0047(14) 0.0084(14) -0.0019(14) C37 0.0329(19) 0.037(2) 0.0285(19) -0.0027(15) 0.0088(15) 0.0061(15) C38 0.038(2) 0.052(2) 0.028(2) -0.0081(17) 0.0023(16) 0.0022(18) C39 0.046(2) 0.042(2) 0.040(2) -0.0166(18) 0.0089(19) -0.0046(18) C40 0.046(2) 0.030(2) 0.048(2) -0.0087(17) 0.0076(19) -0.0003(17) C41 0.0348(19) 0.0313(19) 0.036(2) -0.0032(15) 0.0063(16) -0.0008(15) C42 0.0255(16) 0.0254(16) 0.0289(18) -0.0025(13) 0.0053(14) -0.0002(13) C43 0.0278(18) 0.041(2) 0.038(2) 0.0085(17) 0.0081(16) 0.0046(15) C44 0.038(2) 0.053(3) 0.043(2) 0.020(2) 0.0074(18) 0.0092(19) C45 0.0281(19) 0.046(2) 0.054(3) 0.016(2) -0.0006(18) 0.0067(17) C46 0.0253(18) 0.044(2) 0.050(2) 0.0043(19) 0.0089(17) 0.0012(16) C47 0.0293(18) 0.0319(18) 0.0327(19) 0.0003(15) 0.0078(15) 0.0004(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C19 1.986(3) . ? Ru1 C28 2.066(4) . ? Ru1 P2 2.3261(10) . ? Ru1 P1 2.3591(10) . ? Ru1 Cl1 2.4582(10) . ? P1 C1 1.829(4) . ? P1 C7 1.836(4) . ? P1 C13 1.838(4) . ? P2 C36 1.832(4) . ? P2 C30 1.835(4) . ? P2 C42 1.840(4) . ? O1 C24 1.405(6) . ? O1 C23 1.414(5) . ? O2 C28 1.449(5) . ? O2 C29 1.456(6) . ? N1 C19 1.356(4) . ? N1 C20 1.382(5) . ? N1 C27 1.451(5) . ? N2 C19 1.371(4) . ? N2 C21 1.405(4) . ? N2 C22 1.454(5) . ? C1 C2 1.390(5) . ? C1 C6 1.400(5) . ? C2 C3 1.388(5) . ? C2 H2A 0.9500 . ? C3 C4 1.370(6) . ? C3 H3A 0.9500 . ? C4 C5 1.384(7) . ? C4 H4A 0.9500 . ? C5 C6 1.386(6) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C8 1.394(6) . ? C7 C12 1.399(6) . ? C8 C9 1.400(6) . ? C8 H8A 0.9500 . ? C9 C10 1.373(9) . ? C9 H9A 0.9500 . ? C10 C11 1.370(9) . ? C10 H10A 0.9500 . ? C11 C12 1.388(6) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C18 1.369(5) . ? C13 C14 1.391(6) . ? C14 C15 1.384(6) . ? C14 H14A 0.9500 . ? C15 C16 1.376(7) . ? C15 H15A 0.9500 . ? C16 C17 1.349(7) . ? C16 H16A 0.9500 . ? C17 C18 1.391(6) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C20 C21 1.349(6) . ? C20 C26 1.492(5) . ? C21 C25 1.498(5) . ? C22 C23 1.500(5) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.506(5) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C35 1.389(5) . ? C30 C31 1.395(5) . ? C31 C32 1.391(5) . ? C31 H31A 0.9500 . ? C32 C33 1.379(6) . ? C32 H32A 0.9500 . ? C33 C34 1.390(6) . ? C33 H33A 0.9500 . ? C34 C35 1.378(6) . ? C34 H34A 0.9500 . ? C35 H35A 0.9500 . ? C36 C41 1.395(5) . ? C36 C37 1.403(5) . ? C37 C38 1.384(5) . ? C37 H37A 0.9500 . ? C38 C39 1.385(6) . ? C38 H38A 0.9500 . ? C39 C40 1.381(6) . ? C39 H39A 0.9500 . ? C40 C41 1.392(5) . ? C40 H40A 0.9500 . ? C41 H41A 0.9500 . ? C42 C43 1.390(5) . ? C42 C47 1.396(5) . ? C43 C44 1.393(5) . ? C43 H43A 0.9500 . ? C44 C45 1.372(6) . ? C44 H44A 0.9500 . ? C45 C46 1.374(6) . ? C45 H45A 0.9500 . ? C46 C47 1.385(5) . ? C46 H46A 0.9500 . ? C47 H47A 0.9500 . ? C81 C82 1.521(10) . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C82 C83 1.537(10) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C83 C84 1.542(10) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C84 C85 1.529(10) . ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? C85 H85A 0.9800 . ? C85 H85B 0.9800 . ? C85 H85C 0.9800 . ? C90 C91 1.402(9) . ? C90 C92 1.440(16) 3_757 ? C90 H90A 0.9500 . ? C91 C92 1.392(9) . ? C91 H91A 0.9500 . ? C92 C90 1.439(16) 3_757 ? C92 H92A 0.9500 . ? 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 C19 Ru1 C28 79.18(15) . . ? C19 Ru1 P2 91.06(10) . . ? C28 Ru1 P2 91.60(12) . . ? C19 Ru1 P1 89.23(10) . . ? C28 Ru1 P1 98.99(12) . . ? P2 Ru1 P1 169.27(3) . . ? C19 Ru1 Cl1 174.38(10) . . ? C28 Ru1 Cl1 106.01(11) . . ? P2 Ru1 Cl1 90.94(4) . . ? P1 Ru1 Cl1 87.84(4) . . ? C1 P1 C7 103.57(17) . . ? C1 P1 C13 101.90(17) . . ? C7 P1 C13 102.42(17) . . ? C1 P1 Ru1 106.97(11) . . ? C7 P1 Ru1 116.30(13) . . ? C13 P1 Ru1 123.23(13) . . ? C36 P2 C30 104.23(17) . . ? C36 P2 C42 100.53(16) . . ? C30 P2 C42 99.71(16) . . ? C36 P2 Ru1 118.19(12) . . ? C30 P2 Ru1 110.15(11) . . ? C42 P2 Ru1 121.35(12) . . ? C24 O1 C23 112.2(3) . . ? C28 O2 C29 111.8(4) . . ? C19 N1 C20 113.1(3) . . ? C19 N1 C27 117.0(3) . . ? C20 N1 C27 129.9(3) . . ? C19 N2 C21 110.6(3) . . ? C19 N2 C22 124.3(3) . . ? C21 N2 C22 124.9(3) . . ? C2 C1 C6 118.3(3) . . ? C2 C1 P1 117.3(3) . . ? C6 C1 P1 124.4(3) . . ? C3 C2 C1 121.3(4) . . ? C3 C2 H2A 119.4 . . ? C1 C2 H2A 119.4 . . ? C4 C3 C2 119.7(4) . . ? C4 C3 H3A 120.2 . . ? C2 C3 H3A 120.2 . . ? C3 C4 C5 120.3(4) . . ? C3 C4 H4A 119.8 . . ? C5 C4 H4A 119.8 . . ? C4 C5 C6 120.2(4) . . ? C4 C5 H5A 119.9 . . ? C6 C5 H5A 119.9 . . ? C5 C6 C1 120.2(4) . . ? C5 C6 H6A 119.9 . . ? C1 C6 H6A 119.9 . . ? C8 C7 C12 118.1(4) . . ? C8 C7 P1 123.5(3) . . ? C12 C7 P1 118.1(3) . . ? C7 C8 C9 120.5(5) . . ? C7 C8 H8A 119.8 . . ? C9 C8 H8A 119.8 . . ? C10 C9 C8 119.8(5) . . ? C10 C9 H9A 120.1 . . ? C8 C9 H9A 120.1 . . ? C11 C10 C9 120.7(4) . . ? C11 C10 H10A 119.6 . . ? C9 C10 H10A 119.6 . . ? C10 C11 C12 120.0(5) . . ? C10 C11 H11A 120.0 . . ? C12 C11 H11A 120.0 . . ? C11 C12 C7 120.9(5) . . ? C11 C12 H12A 119.6 . . ? C7 C12 H12A 119.6 . . ? C18 C13 C14 118.1(4) . . ? C18 C13 P1 123.5(3) . . ? C14 C13 P1 118.3(3) . . ? C15 C14 C13 120.5(4) . . ? C15 C14 H14A 119.8 . . ? C13 C14 H14A 119.8 . . ? C16 C15 C14 120.4(5) . . ? C16 C15 H15A 119.8 . . ? C14 C15 H15A 119.8 . . ? C17 C16 C15 119.0(4) . . ? C17 C16 H16A 120.5 . . ? C15 C16 H16A 120.5 . . ? C16 C17 C18 121.4(4) . . ? C16 C17 H17A 119.3 . . ? C18 C17 H17A 119.3 . . ? C13 C18 C17 120.4(4) . . ? C13 C18 H18A 119.8 . . ? C17 C18 H18A 119.8 . . ? N1 C19 N2 103.3(3) . . ? N1 C19 Ru1 118.6(2) . . ? N2 C19 Ru1 137.9(3) . . ? C21 C20 N1 105.9(3) . . ? C21 C20 C26 131.7(4) . . ? N1 C20 C26 122.4(4) . . ? C20 C21 N2 107.0(3) . . ? C20 C21 C25 130.1(3) . . ? N2 C21 C25 122.7(3) . . ? N2 C22 C23 115.1(3) . . ? N2 C22 H22A 108.5 . . ? C23 C22 H22A 108.5 . . ? N2 C22 H22B 108.5 . . ? C23 C22 H22B 108.5 . . ? H22A C22 H22B 107.5 . . ? O1 C23 C22 109.3(3) . . ? O1 C23 H23A 109.8 . . ? C22 C23 H23A 109.8 . . ? O1 C23 H23B 109.8 . . ? C22 C23 H23B 109.8 . . ? H23A C23 H23B 108.3 . . ? O1 C24 H24A 109.5 . . ? O1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 H25A 109.5 . . ? C21 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C21 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C20 C26 H26A 109.5 . . ? C20 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C20 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N1 C27 C28 109.1(3) . . ? N1 C27 H27A 109.9 . . ? C28 C27 H27A 109.9 . . ? N1 C27 H27B 109.9 . . ? C28 C27 H27B 109.9 . . ? H27A C27 H27B 108.3 . . ? O2 C28 C27 105.4(3) . . ? O2 C28 Ru1 114.1(3) . . ? C27 C28 Ru1 113.3(3) . . ? O2 C28 H28A 107.9 . . ? C27 C28 H28A 107.9 . . ? Ru1 C28 H28A 107.9 . . ? O2 C29 H29A 109.5 . . ? O2 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? O2 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C35 C30 C31 118.5(3) . . ? C35 C30 P2 125.1(3) . . ? C31 C30 P2 116.3(3) . . ? C32 C31 C30 121.0(4) . . ? C32 C31 H31A 119.5 . . ? C30 C31 H31A 119.5 . . ? C33 C32 C31 119.5(4) . . ? C33 C32 H32A 120.2 . . ? C31 C32 H32A 120.2 . . ? C32 C33 C34 119.9(4) . . ? C32 C33 H33A 120.1 . . ? C34 C33 H33A 120.1 . . ? C35 C34 C33 120.4(4) . . ? C35 C34 H34A 119.8 . . ? C33 C34 H34A 119.8 . . ? C34 C35 C30 120.6(4) . . ? C34 C35 H35A 119.7 . . ? C30 C35 H35A 119.7 . . ? C41 C36 C37 118.3(3) . . ? C41 C36 P2 121.2(3) . . ? C37 C36 P2 120.2(3) . . ? C38 C37 C36 120.9(4) . . ? C38 C37 H37A 119.5 . . ? C36 C37 H37A 119.5 . . ? C37 C38 C39 119.9(4) . . ? C37 C38 H38A 120.0 . . ? C39 C38 H38A 120.0 . . ? C40 C39 C38 120.1(4) . . ? C40 C39 H39A 120.0 . . ? C38 C39 H39A 120.0 . . ? C39 C40 C41 120.2(4) . . ? C39 C40 H40A 119.9 . . ? C41 C40 H40A 119.9 . . ? C40 C41 C36 120.5(4) . . ? C40 C41 H41A 119.7 . . ? C36 C41 H41A 119.7 . . ? C43 C42 C47 118.8(3) . . ? C43 C42 P2 120.3(3) . . ? C47 C42 P2 120.9(3) . . ? C42 C43 C44 119.8(4) . . ? C42 C43 H43A 120.1 . . ? C44 C43 H43A 120.1 . . ? C45 C44 C43 120.7(4) . . ? C45 C44 H44A 119.7 . . ? C43 C44 H44A 119.7 . . ? C44 C45 C46 120.0(4) . . ? C44 C45 H45A 120.0 . . ? C46 C45 H45A 120.0 . . ? C45 C46 C47 120.2(4) . . ? C45 C46 H46A 119.9 . . ? C47 C46 H46A 119.9 . . ? C46 C47 C42 120.6(4) . . ? C46 C47 H47A 119.7 . . ? C42 C47 H47A 119.7 . . ? C82 C81 H81A 109.5 . . ? C82 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C82 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C81 C82 C83 110.2(10) . . ? C81 C82 H82A 109.6 . . ? C83 C82 H82A 109.6 . . ? C81 C82 H82B 109.6 . . ? C83 C82 H82B 109.6 . . ? H82A C82 H82B 108.1 . . ? C82 C83 C84 108.5(9) . . ? C82 C83 H83A 110.0 . . ? C84 C83 H83A 110.0 . . ? C82 C83 H83B 110.0 . . ? C84 C83 H83B 110.0 . . ? H83A C83 H83B 108.4 . . ? C85 C84 C83 109.4(10) . . ? C85 C84 H84A 109.8 . . ? C83 C84 H84A 109.8 . . ? C85 C84 H84B 109.8 . . ? C83 C84 H84B 109.8 . . ? H84A C84 H84B 108.2 . . ? C84 C85 H85A 109.5 . . ? C84 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? C84 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? C91 C90 C92 119.0(13) . 3_757 ? C91 C90 H90A 120.5 . . ? C92 C90 H90A 120.5 3_757 . ? C92 C91 C90 119.0(10) . . ? C92 C91 H91A 120.5 . . ? C90 C91 H91A 120.5 . . ? C91 C92 C90 122.0(13) . 3_757 ? C91 C92 H92A 119.0 . . ? C90 C92 H92A 119.0 3_757 . ? 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 C19 Ru1 P1 C1 -109.66(15) . . . . ? C28 Ru1 P1 C1 171.42(16) . . . . ? P2 Ru1 P1 C1 -18.0(2) . . . . ? Cl1 Ru1 P1 C1 65.54(12) . . . . ? C19 Ru1 P1 C7 5.46(18) . . . . ? C28 Ru1 P1 C7 -73.46(19) . . . . ? P2 Ru1 P1 C7 97.1(2) . . . . ? Cl1 Ru1 P1 C7 -179.33(15) . . . . ? C19 Ru1 P1 C13 133.10(18) . . . . ? C28 Ru1 P1 C13 54.18(19) . . . . ? P2 Ru1 P1 C13 -135.3(2) . . . . ? Cl1 Ru1 P1 C13 -51.69(15) . . . . ? C19 Ru1 P2 C36 -29.78(17) . . . . ? C28 Ru1 P2 C36 49.43(18) . . . . ? P1 Ru1 P2 C36 -121.2(2) . . . . ? Cl1 Ru1 P2 C36 155.48(14) . . . . ? C19 Ru1 P2 C30 89.81(16) . . . . ? C28 Ru1 P2 C30 169.02(16) . . . . ? P1 Ru1 P2 C30 -1.6(2) . . . . ? Cl1 Ru1 P2 C30 -84.93(12) . . . . ? C19 Ru1 P2 C42 -154.48(17) . . . . ? C28 Ru1 P2 C42 -75.28(17) . . . . ? P1 Ru1 P2 C42 114.1(2) . . . . ? Cl1 Ru1 P2 C42 30.77(13) . . . . ? C7 P1 C1 C2 -109.8(3) . . . . ? C13 P1 C1 C2 144.1(3) . . . . ? Ru1 P1 C1 C2 13.6(3) . . . . ? C7 P1 C1 C6 70.8(3) . . . . ? C13 P1 C1 C6 -35.3(3) . . . . ? Ru1 P1 C1 C6 -165.8(3) . . . . ? C6 C1 C2 C3 -1.6(5) . . . . ? P1 C1 C2 C3 178.9(3) . . . . ? C1 C2 C3 C4 0.5(5) . . . . ? C2 C3 C4 C5 0.1(6) . . . . ? C3 C4 C5 C6 0.4(6) . . . . ? C4 C5 C6 C1 -1.6(6) . . . . ? C2 C1 C6 C5 2.2(5) . . . . ? P1 C1 C6 C5 -178.4(3) . . . . ? C1 P1 C7 C8 -0.9(4) . . . . ? C13 P1 C7 C8 104.8(4) . . . . ? Ru1 P1 C7 C8 -117.9(3) . . . . ? C1 P1 C7 C12 173.4(3) . . . . ? C13 P1 C7 C12 -80.9(3) . . . . ? Ru1 P1 C7 C12 56.4(3) . . . . ? C12 C7 C8 C9 1.2(6) . . . . ? P1 C7 C8 C9 175.5(3) . . . . ? C7 C8 C9 C10 -1.3(7) . . . . ? C8 C9 C10 C11 1.1(8) . . . . ? C9 C10 C11 C12 -0.7(7) . . . . ? C10 C11 C12 C7 0.6(7) . . . . ? C8 C7 C12 C11 -0.8(6) . . . . ? P1 C7 C12 C11 -175.4(3) . . . . ? C1 P1 C13 C18 126.4(4) . . . . ? C7 P1 C13 C18 19.4(4) . . . . ? Ru1 P1 C13 C18 -114.0(4) . . . . ? C1 P1 C13 C14 -51.9(4) . . . . ? C7 P1 C13 C14 -158.9(4) . . . . ? Ru1 P1 C13 C14 67.7(4) . . . . ? C18 C13 C14 C15 4.2(8) . . . . ? P1 C13 C14 C15 -177.4(4) . . . . ? C13 C14 C15 C16 -1.2(9) . . . . ? C14 C15 C16 C17 -1.3(9) . . . . ? C15 C16 C17 C18 0.9(9) . . . . ? C14 C13 C18 C17 -4.6(7) . . . . ? P1 C13 C18 C17 177.1(4) . . . . ? C16 C17 C18 C13 2.2(9) . . . . ? C20 N1 C19 N2 0.0(4) . . . . ? C27 N1 C19 N2 -177.9(3) . . . . ? C20 N1 C19 Ru1 176.9(2) . . . . ? C27 N1 C19 Ru1 -0.9(4) . . . . ? C21 N2 C19 N1 0.4(4) . . . . ? C22 N2 C19 N1 176.4(3) . . . . ? C21 N2 C19 Ru1 -175.6(3) . . . . ? C22 N2 C19 Ru1 0.4(6) . . . . ? C28 Ru1 C19 N1 -7.7(3) . . . . ? P2 Ru1 C19 N1 83.8(3) . . . . ? P1 Ru1 C19 N1 -107.0(3) . . . . ? Cl1 Ru1 C19 N1 -165.5(8) . . . . ? C28 Ru1 C19 N2 167.9(4) . . . . ? P2 Ru1 C19 N2 -100.7(4) . . . . ? P1 Ru1 C19 N2 68.6(4) . . . . ? Cl1 Ru1 C19 N2 10.0(13) . . . . ? C19 N1 C20 C21 -0.4(4) . . . . ? C27 N1 C20 C21 177.1(4) . . . . ? C19 N1 C20 C26 -179.6(4) . . . . ? C27 N1 C20 C26 -2.1(6) . . . . ? N1 C20 C21 N2 0.6(4) . . . . ? C26 C20 C21 N2 179.8(4) . . . . ? N1 C20 C21 C25 -175.8(4) . . . . ? C26 C20 C21 C25 3.3(8) . . . . ? C19 N2 C21 C20 -0.7(4) . . . . ? C22 N2 C21 C20 -176.6(3) . . . . ? C19 N2 C21 C25 176.1(3) . . . . ? C22 N2 C21 C25 0.2(6) . . . . ? C19 N2 C22 C23 85.7(4) . . . . ? C21 N2 C22 C23 -98.9(4) . . . . ? C24 O1 C23 C22 175.9(4) . . . . ? N2 C22 C23 O1 66.8(4) . . . . ? C19 N1 C27 C28 12.6(5) . . . . ? C20 N1 C27 C28 -164.9(4) . . . . ? C29 O2 C28 C27 152.0(4) . . . . ? C29 O2 C28 Ru1 -83.0(4) . . . . ? N1 C27 C28 O2 107.3(4) . . . . ? N1 C27 C28 Ru1 -18.2(4) . . . . ? C19 Ru1 C28 O2 -106.5(3) . . . . ? P2 Ru1 C28 O2 162.8(3) . . . . ? P1 Ru1 C28 O2 -19.0(3) . . . . ? Cl1 Ru1 C28 O2 71.3(3) . . . . ? C19 Ru1 C28 C27 14.2(3) . . . . ? P2 Ru1 C28 C27 -76.5(3) . . . . ? P1 Ru1 C28 C27 101.7(3) . . . . ? Cl1 Ru1 C28 C27 -168.0(3) . . . . ? C36 P2 C30 C35 -9.6(4) . . . . ? C42 P2 C30 C35 94.0(3) . . . . ? Ru1 P2 C30 C35 -137.4(3) . . . . ? C36 P2 C30 C31 172.1(3) . . . . ? C42 P2 C30 C31 -84.3(3) . . . . ? Ru1 P2 C30 C31 44.3(3) . . . . ? C35 C30 C31 C32 -0.2(5) . . . . ? P2 C30 C31 C32 178.2(3) . . . . ? C30 C31 C32 C33 -0.1(6) . . . . ? C31 C32 C33 C34 0.5(6) . . . . ? C32 C33 C34 C35 -0.7(7) . . . . ? C33 C34 C35 C30 0.4(7) . . . . ? C31 C30 C35 C34 0.0(6) . . . . ? P2 C30 C35 C34 -178.2(3) . . . . ? C30 P2 C36 C41 125.4(3) . . . . ? C42 P2 C36 C41 22.4(3) . . . . ? Ru1 P2 C36 C41 -112.0(3) . . . . ? C30 P2 C36 C37 -61.5(3) . . . . ? C42 P2 C36 C37 -164.4(3) . . . . ? Ru1 P2 C36 C37 61.1(3) . . . . ? C41 C36 C37 C38 0.8(6) . . . . ? P2 C36 C37 C38 -172.5(3) . . . . ? C36 C37 C38 C39 -1.3(6) . . . . ? C37 C38 C39 C40 1.1(7) . . . . ? C38 C39 C40 C41 -0.3(7) . . . . ? C39 C40 C41 C36 -0.1(6) . . . . ? C37 C36 C41 C40 -0.1(6) . . . . ? P2 C36 C41 C40 173.1(3) . . . . ? C36 P2 C42 C43 -110.6(3) . . . . ? C30 P2 C42 C43 142.9(3) . . . . ? Ru1 P2 C42 C43 22.0(4) . . . . ? C36 P2 C42 C47 68.3(3) . . . . ? C30 P2 C42 C47 -38.3(3) . . . . ? Ru1 P2 C42 C47 -159.1(2) . . . . ? C47 C42 C43 C44 0.9(6) . . . . ? P2 C42 C43 C44 179.8(3) . . . . ? C42 C43 C44 C45 -1.0(7) . . . . ? C43 C44 C45 C46 0.8(7) . . . . ? C44 C45 C46 C47 -0.4(7) . . . . ? C45 C46 C47 C42 0.3(6) . . . . ? C43 C42 C47 C46 -0.5(6) . . . . ? P2 C42 C47 C46 -179.4(3) . . . . ? C81 C82 C83 C84 176.5(15) . . . . ? C82 C83 C84 C85 167.7(19) . . . . ? C92 C90 C91 C92 0(3) 3_757 . . . ? C90 C91 C92 C90 0(3) . . . 3_757 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.060 _refine_diff_density_min -0.872 _refine_diff_density_rms 0.103 _database_code_depnum_ccdc_archive 'CCDC 973558' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound8 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C48 H54 Cl3 N4 O2 P Ru' _chemical_formula_weight 957.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.9860(6) _cell_length_b 19.2471(12) _cell_length_c 24.3594(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.793(2) _cell_angle_gamma 90.00 _cell_volume 4681.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8892 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 27.26 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.358 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1984 _exptl_absorpt_coefficient_mu 0.582 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7171 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41374 _diffrn_reflns_av_R_equivalents 0.0831 _diffrn_reflns_av_unetI/netI 0.2036 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 27.56 _reflns_number_total 19065 _reflns_number_gt 10494 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.023(16) _refine_ls_number_reflns 19065 _refine_ls_number_parameters 1085 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1042 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.0656 _refine_ls_wR_factor_gt 0.0531 _refine_ls_goodness_of_fit_ref 0.662 _refine_ls_restrained_S_all 0.662 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.66259(4) 0.613711(19) 0.858284(17) 0.01902(11) Uani 1 1 d . . . Ru2 Ru 0.92650(4) 0.630229(19) 0.381309(16) 0.01748(10) Uani 1 1 d . . . Cl1 Cl 0.80005(16) 0.71926(7) 0.85820(6) 0.0360(4) Uani 1 1 d . . . Cl2 Cl 0.62272(15) 0.64716(8) 1.09740(6) 0.0451(5) Uani 1 1 d . . . Cl3 Cl 0.37698(17) 0.74846(10) 1.03325(7) 0.0568(5) Uani 1 1 d . . . Cl4 Cl 0.80792(16) 0.73975(7) 0.39683(6) 0.0395(4) Uani 1 1 d . . . Cl5 Cl 0.95685(16) 0.69557(8) 0.14616(6) 0.0459(5) Uani 1 1 d . . . Cl6 Cl 1.21802(16) 0.77862(9) 0.21433(6) 0.0475(5) Uani 1 1 d . . . P1 P 0.67839(13) 0.59917(7) 0.76432(6) 0.0179(3) Uani 1 1 d . . . P2 P 0.91807(13) 0.60242(7) 0.47347(5) 0.0190(3) Uani 1 1 d . . . O1 O 1.0402(3) 0.42223(19) 0.84266(16) 0.0358(11) Uani 1 1 d . . . O2 O 0.3431(4) 0.36390(19) 0.89427(18) 0.0439(12) Uani 1 1 d . . . O3 O 0.5027(3) 0.45618(19) 0.38554(15) 0.0314(10) Uani 1 1 d . . . N1 N 0.7828(4) 0.4778(2) 0.88205(16) 0.0206(10) Uani 1 1 d . . . N2 N 0.5736(4) 0.4588(2) 0.86713(17) 0.0224(11) Uani 1 1 d . . . N3 N 0.6591(4) 0.6245(2) 0.98877(15) 0.0226(10) Uani 1 1 d . . . N4 N 0.5062(4) 0.6867(2) 0.94915(18) 0.0232(11) Uani 1 1 d . . . N5 N 0.7722(4) 0.5072(2) 0.34881(17) 0.0201(10) Uani 1 1 d . . . N6 N 0.9767(4) 0.4757(2) 0.34874(19) 0.0294(12) Uani 1 1 d . B . N7 N 1.0866(4) 0.7109(2) 0.29589(16) 0.0202(10) Uani 1 1 d . . . N8 N 0.9234(4) 0.6600(2) 0.25338(17) 0.0220(11) Uani 1 1 d . . . C1 C 0.6650(5) 0.5121(2) 0.8697(2) 0.0183(12) Uani 1 1 d . . . C2 C 0.7635(5) 0.4064(3) 0.8867(2) 0.0293(15) Uani 1 1 d . . . H2A H 0.8296 0.3723 0.8949 0.035 Uiso 1 1 calc R . . C3 C 0.6326(5) 0.3956(3) 0.8773(2) 0.0271(14) Uani 1 1 d . . . H3A H 0.5884 0.3519 0.8776 0.033 Uiso 1 1 calc R . . C4 C 0.9133(5) 0.5112(2) 0.8837(2) 0.0264(14) Uani 1 1 d . . . H4A H 0.9605 0.4981 0.9181 0.032 Uiso 1 1 calc R . . H4B H 0.9008 0.5622 0.8840 0.032 Uiso 1 1 calc R . . C5 C 0.9993(5) 0.4917(3) 0.8355(2) 0.0293(15) Uani 1 1 d . . . H5A H 0.9474 0.4967 0.8008 0.035 Uiso 1 1 calc R . . H5B H 1.0784 0.5226 0.8339 0.035 Uiso 1 1 calc R . . C6 C 1.1053(6) 0.3975(3) 0.7946(3) 0.059(2) Uani 1 1 d . . . H6A H 1.1330 0.3491 0.8002 0.089 Uiso 1 1 calc R . . H6B H 1.1842 0.4262 0.7875 0.089 Uiso 1 1 calc R . . H6C H 1.0432 0.4001 0.7632 0.089 Uiso 1 1 calc R . . C7 C 0.4330(5) 0.4664(3) 0.8528(2) 0.0273(14) Uani 1 1 d . . . H7A H 0.4152 0.4426 0.8174 0.033 Uiso 1 1 calc R . . H7B H 0.4125 0.5163 0.8477 0.033 Uiso 1 1 calc R . . C8 C 0.3411(5) 0.4368(3) 0.8959(2) 0.0289(14) Uani 1 1 d . . . H8A H 0.3705 0.4529 0.9327 0.035 Uiso 1 1 calc R . . H8B H 0.2486 0.4536 0.8892 0.035 Uiso 1 1 calc R . . C9 C 0.2540(6) 0.3349(3) 0.9346(3) 0.060(2) Uani 1 1 d . . . H9A H 0.2564 0.2841 0.9325 0.090 Uiso 1 1 calc R . . H9B H 0.1625 0.3512 0.9273 0.090 Uiso 1 1 calc R . . H9C H 0.2828 0.3498 0.9714 0.090 Uiso 1 1 calc R . . C10 C 0.8423(5) 0.5917(2) 0.7302(2) 0.0185(13) Uani 1 1 d . . . C11 C 0.9462(5) 0.6336(3) 0.7506(2) 0.0280(13) Uani 1 1 d . . . H11A H 0.9311 0.6624 0.7815 0.034 Uiso 1 1 calc R . . C12 C 1.0704(5) 0.6337(3) 0.7263(2) 0.0349(15) Uani 1 1 d . . . H12A H 1.1394 0.6631 0.7401 0.042 Uiso 1 1 calc R . . C13 C 1.0942(5) 0.5910(3) 0.6819(2) 0.0289(15) Uani 1 1 d . . . H13A H 1.1796 0.5913 0.6651 0.035 Uiso 1 1 calc R . . C14 C 0.9949(5) 0.5481(3) 0.6617(2) 0.0264(14) Uani 1 1 d . . . H14A H 1.0119 0.5182 0.6316 0.032 Uiso 1 1 calc R . . C15 C 0.8689(5) 0.5488(3) 0.6858(2) 0.0220(13) Uani 1 1 d . . . H15A H 0.8002 0.5194 0.6716 0.026 Uiso 1 1 calc R . . C16 C 0.6045(5) 0.6721(2) 0.7252(2) 0.0179(13) Uani 1 1 d . . . C17 C 0.5048(5) 0.7120(3) 0.7486(2) 0.0285(15) Uani 1 1 d . . . H17A H 0.4787 0.7029 0.7853 0.034 Uiso 1 1 calc R . . C18 C 0.4424(6) 0.7650(3) 0.7194(3) 0.0366(17) Uani 1 1 d . . . H18A H 0.3724 0.7910 0.7356 0.044 Uiso 1 1 calc R . . C19 C 0.4824(6) 0.7799(3) 0.6669(2) 0.0356(16) Uani 1 1 d . . . H19A H 0.4411 0.8167 0.6469 0.043 Uiso 1 1 calc R . . C20 C 0.5839(6) 0.7408(3) 0.6430(2) 0.0392(17) Uani 1 1 d . . . H20A H 0.6124 0.7506 0.6067 0.047 Uiso 1 1 calc R . . C21 C 0.6421(5) 0.6877(3) 0.6727(2) 0.0285(15) Uani 1 1 d . . . H21A H 0.7108 0.6609 0.6563 0.034 Uiso 1 1 calc R . . C22 C 0.5844(5) 0.5255(3) 0.7349(2) 0.0174(12) Uani 1 1 d . . . C23 C 0.6366(5) 0.4583(2) 0.7389(2) 0.0219(13) Uani 1 1 d . . . H23A H 0.7221 0.4511 0.7555 0.026 Uiso 1 1 calc R . . C24 C 0.5644(5) 0.4019(3) 0.7187(2) 0.0278(14) Uani 1 1 d . . . H24A H 0.6016 0.3565 0.7213 0.033 Uiso 1 1 calc R . . C25 C 0.4388(5) 0.4108(3) 0.6948(2) 0.0271(14) Uani 1 1 d . . . H25A H 0.3905 0.3723 0.6804 0.032 Uiso 1 1 calc R . . C26 C 0.3856(5) 0.4767(3) 0.6923(2) 0.0305(15) Uani 1 1 d . . . H26A H 0.2984 0.4833 0.6771 0.037 Uiso 1 1 calc R . . C27 C 0.4579(5) 0.5343(3) 0.7119(2) 0.0204(13) Uani 1 1 d . . . H27A H 0.4200 0.5794 0.7093 0.025 Uiso 1 1 calc R . . C28 C 0.6083(5) 0.6411(3) 0.9366(2) 0.0202(13) Uani 1 1 d . . . C29 C 0.7695(5) 0.5784(3) 1.0023(2) 0.0258(14) Uani 1 1 d . . . C30 C 0.8973(6) 0.6067(4) 1.0087(2) 0.0374(17) Uani 1 1 d . . . C31 C 1.0010(6) 0.5623(4) 1.0279(2) 0.0440(18) Uani 1 1 d . . . H31A H 1.0890 0.5801 1.0328 0.053 Uiso 1 1 calc R . . C32 C 0.9752(8) 0.4932(4) 1.0394(3) 0.063(2) Uani 1 1 d . . . C33 C 0.8482(7) 0.4687(3) 1.0333(2) 0.051(2) Uani 1 1 d . . . H33A H 0.8309 0.4215 1.0421 0.061 Uiso 1 1 calc R . . C34 C 0.7428(6) 0.5098(3) 1.0147(2) 0.0418(17) Uani 1 1 d . . . C35 C 0.9272(6) 0.6808(3) 0.9974(2) 0.0437(18) Uani 1 1 d . . . H35A H 0.8457 0.7041 0.9843 0.066 Uiso 1 1 calc R . . H35B H 0.9963 0.6839 0.9694 0.066 Uiso 1 1 calc R . . H35C H 0.9593 0.7032 1.0312 0.066 Uiso 1 1 calc R . . C36 C 1.0893(7) 0.4464(4) 1.0608(3) 0.104(3) Uani 1 1 d . . . H36A H 1.0551 0.3993 1.0667 0.156 Uiso 1 1 calc R . . H36B H 1.1245 0.4650 1.0956 0.156 Uiso 1 1 calc R . . H36C H 1.1611 0.4450 1.0338 0.156 Uiso 1 1 calc R . . C37 C 0.6019(6) 0.4818(3) 1.0107(2) 0.0494(19) Uani 1 1 d . . . H37A H 0.6017 0.4327 1.0213 0.074 Uiso 1 1 calc R . . H37B H 0.5684 0.4863 0.9729 0.074 Uiso 1 1 calc R . . H37C H 0.5440 0.5081 1.0354 0.074 Uiso 1 1 calc R . . C38 C 0.5889(6) 0.6582(3) 1.0297(2) 0.0313(15) Uani 1 1 d . . . C39 C 0.4950(6) 0.6964(3) 1.0046(2) 0.0313(15) Uani 1 1 d . . . C40 C 0.4132(5) 0.7182(3) 0.9113(2) 0.0216(13) Uani 1 1 d . . . C41 C 0.4353(5) 0.7855(3) 0.8920(3) 0.0299(15) Uani 1 1 d . . . C42 C 0.3378(6) 0.8148(3) 0.8593(2) 0.0352(16) Uani 1 1 d . . . H42A H 0.3512 0.8605 0.8457 0.042 Uiso 1 1 calc R . . C43 C 0.2193(6) 0.7800(3) 0.8454(2) 0.0324(16) Uani 1 1 d . . . C44 C 0.1983(6) 0.7152(3) 0.8667(2) 0.0312(15) Uani 1 1 d . . . H44A H 0.1164 0.6920 0.8586 0.037 Uiso 1 1 calc R . . C45 C 0.2948(5) 0.6821(3) 0.9001(2) 0.0239(13) Uani 1 1 d . . . C46 C 0.5593(5) 0.8267(3) 0.9091(3) 0.051(2) Uani 1 1 d . . . H46A H 0.5570 0.8724 0.8915 0.077 Uiso 1 1 calc R . . H46B H 0.6398 0.8016 0.8979 0.077 Uiso 1 1 calc R . . H46C H 0.5608 0.8326 0.9491 0.077 Uiso 1 1 calc R . . C47 C 0.1134(6) 0.8145(3) 0.8095(3) 0.058(2) Uani 1 1 d . . . H47A H 0.0377 0.7827 0.8042 0.086 Uiso 1 1 calc R . . H47B H 0.1516 0.8260 0.7738 0.086 Uiso 1 1 calc R . . H47C H 0.0825 0.8571 0.8273 0.086 Uiso 1 1 calc R . . C48 C 0.2696(5) 0.6130(3) 0.9252(2) 0.0327(14) Uani 1 1 d . . . H48A H 0.3485 0.5985 0.9467 0.049 Uiso 1 1 calc R . . H48B H 0.2516 0.5788 0.8962 0.049 Uiso 1 1 calc R . . H48C H 0.1920 0.6160 0.9493 0.049 Uiso 1 1 calc R . . C49 C 0.8991(5) 0.5329(3) 0.3586(2) 0.0212(13) Uani 1 1 d . . . C50 C 0.7744(5) 0.4378(3) 0.3326(2) 0.0273(14) Uani 1 1 d . . . H50A H 0.6992 0.4099 0.3230 0.033 Uiso 1 1 calc R . . C51 C 0.9019(5) 0.4181(3) 0.3331(2) 0.0339(16) Uani 1 1 d . . . H51A H 0.9353 0.3732 0.3244 0.041 Uiso 1 1 calc R . . C52 C 0.6503(5) 0.5464(3) 0.3561(2) 0.0248(13) Uani 1 1 d . . . H52A H 0.5970 0.5451 0.3216 0.030 Uiso 1 1 calc R . . H52B H 0.6736 0.5955 0.3637 0.030 Uiso 1 1 calc R . . C53 C 0.5660(5) 0.5192(3) 0.4022(2) 0.0278(14) Uani 1 1 d . . . H53A H 0.6231 0.5107 0.4351 0.033 Uiso 1 1 calc R . . H53B H 0.4972 0.5541 0.4119 0.033 Uiso 1 1 calc R . . C54 C 0.4284(6) 0.4273(3) 0.4292(2) 0.054(2) Uani 1 1 d . . . H54A H 0.3868 0.3837 0.4171 0.081 Uiso 1 1 calc R . . H54B H 0.3586 0.4601 0.4401 0.081 Uiso 1 1 calc R . . H54C H 0.4884 0.4182 0.4605 0.081 Uiso 1 1 calc R . . C55 C 1.1227(6) 0.4721(3) 0.3583(3) 0.055(2) Uani 1 1 d . . . H55A H 1.1548 0.5189 0.3692 0.065 Uiso 1 1 calc R A 1 H55B H 1.1404 0.4404 0.3896 0.065 Uiso 1 1 calc R A 1 C56 C 1.1982(8) 0.4495(6) 0.3133(4) 0.031(3) Uani 0.76(2) 1 d P B 1 H56A H 1.2945 0.4518 0.3234 0.037 Uiso 0.76(2) 1 calc PR B 1 H56B H 1.1826 0.4817 0.2822 0.037 Uiso 0.76(2) 1 calc PR B 1 O4 O 1.1676(6) 0.3813(4) 0.2960(4) 0.051(4) Uani 0.76(2) 1 d P B 1 C57 C 1.235(3) 0.3582(15) 0.2466(12) 0.051(8) Uani 0.76(2) 1 d P B 1 H57A H 1.2106 0.3097 0.2391 0.076 Uiso 0.76(2) 1 calc PR B 1 H57B H 1.3318 0.3619 0.2520 0.076 Uiso 0.76(2) 1 calc PR B 1 H57C H 1.2065 0.3874 0.2156 0.076 Uiso 0.76(2) 1 calc PR B 1 C56A C 1.200(4) 0.417(2) 0.3209(15) 0.034(10) Uiso 0.24(2) 1 d P B 2 H56C H 1.2963 0.4292 0.3226 0.040 Uiso 0.24(2) 1 calc PR B 2 H56D H 1.1899 0.3711 0.3380 0.040 Uiso 0.24(2) 1 calc PR B 2 O4A O 1.1624(16) 0.4106(11) 0.2636(9) 0.026(7) Uiso 0.24(2) 1 d P B 2 C57A C 1.243(11) 0.358(6) 0.243(5) 0.09(4) Uiso 0.24(2) 1 d P B 2 H57D H 1.2062 0.3420 0.2078 0.131 Uiso 0.24(2) 1 calc PR B 2 H57E H 1.2466 0.3195 0.2690 0.131 Uiso 0.24(2) 1 calc PR B 2 H57F H 1.3338 0.3763 0.2376 0.131 Uiso 0.24(2) 1 calc PR B 2 C58 C 0.9785(5) 0.6672(2) 0.3062(2) 0.0182(12) Uani 1 1 d . . . C59 C 0.9955(6) 0.6957(3) 0.2149(2) 0.0278(14) Uani 1 1 d . . . C60 C 1.0956(5) 0.7274(3) 0.2410(2) 0.0241(13) Uani 1 1 d . . . C61 C 1.1801(5) 0.7367(3) 0.3365(2) 0.0228(13) Uani 1 1 d . . . C62 C 1.1609(6) 0.8028(3) 0.3585(2) 0.0259(14) Uani 1 1 d . . . C63 C 1.2599(6) 0.8283(3) 0.3945(2) 0.0325(15) Uani 1 1 d . . . H63A H 1.2472 0.8721 0.4117 0.039 Uiso 1 1 calc R . . C64 C 1.3773(6) 0.7908(4) 0.4056(2) 0.0392(17) Uani 1 1 d . . . C65 C 1.3933(6) 0.7265(3) 0.3819(2) 0.0366(16) Uani 1 1 d . . . H65A H 1.4725 0.7007 0.3895 0.044 Uiso 1 1 calc R . . C66 C 1.2959(5) 0.6984(3) 0.3470(2) 0.0267(14) Uani 1 1 d . . . C67 C 1.0427(5) 0.8486(3) 0.3443(2) 0.0388(17) Uani 1 1 d . . . H67A H 1.0107 0.8712 0.3777 0.058 Uiso 1 1 calc R . . H67B H 0.9706 0.8202 0.3283 0.058 Uiso 1 1 calc R . . H67C H 1.0699 0.8840 0.3179 0.058 Uiso 1 1 calc R . . C68 C 1.4845(6) 0.8223(3) 0.4427(2) 0.053(2) Uani 1 1 d . . . H68A H 1.5594 0.7896 0.4466 0.080 Uiso 1 1 calc R . . H68B H 1.4469 0.8318 0.4789 0.080 Uiso 1 1 calc R . . H68C H 1.5166 0.8657 0.4265 0.080 Uiso 1 1 calc R . . C69 C 1.3156(5) 0.6287(3) 0.3221(2) 0.0400(15) Uani 1 1 d . . . H69A H 1.4024 0.6098 0.3341 0.060 Uiso 1 1 calc R . . H69B H 1.3135 0.6327 0.2820 0.060 Uiso 1 1 calc R . . H69C H 1.2439 0.5975 0.3338 0.060 Uiso 1 1 calc R . . C70 C 0.8022(5) 0.6231(3) 0.23887(19) 0.0229(12) Uani 1 1 d . . . C71 C 0.6808(6) 0.6584(3) 0.2404(2) 0.0267(15) Uani 1 1 d . . . C72 C 0.5664(5) 0.6240(3) 0.22320(19) 0.0324(14) Uani 1 1 d . . . H72A H 0.4829 0.6477 0.2236 0.039 Uiso 1 1 calc R . . C73 C 0.5711(6) 0.5550(3) 0.2052(2) 0.0409(17) Uani 1 1 d . . . C74 C 0.6937(6) 0.5223(3) 0.2034(2) 0.0415(18) Uani 1 1 d . . . H74A H 0.6976 0.4752 0.1918 0.050 Uiso 1 1 calc R . . C75 C 0.8122(6) 0.5562(3) 0.2180(2) 0.0284(14) Uani 1 1 d . . . C76 C 0.6707(5) 0.7342(3) 0.2575(2) 0.0396(17) Uani 1 1 d . . . H76A H 0.5768 0.7490 0.2557 0.059 Uiso 1 1 calc R . . H76B H 0.7237 0.7629 0.2327 0.059 Uiso 1 1 calc R . . H76C H 0.7050 0.7395 0.2951 0.059 Uiso 1 1 calc R . . C77 C 0.4421(6) 0.5188(3) 0.1870(3) 0.072(2) Uani 1 1 d . . . H77A H 0.3665 0.5507 0.1910 0.108 Uiso 1 1 calc R . . H77B H 0.4279 0.4776 0.2098 0.108 Uiso 1 1 calc R . . H77C H 0.4491 0.5047 0.1485 0.108 Uiso 1 1 calc R . . C78 C 0.9439(6) 0.5209(3) 0.2116(2) 0.048(2) Uani 1 1 d . . . H78A H 0.9297 0.4743 0.1962 0.073 Uiso 1 1 calc R . . H78B H 0.9887 0.5170 0.2475 0.073 Uiso 1 1 calc R . . H78C H 0.9999 0.5480 0.1867 0.073 Uiso 1 1 calc R . . C79 C 0.9994(5) 0.6688(2) 0.5158(2) 0.0194(13) Uani 1 1 d . . . C80 C 1.1194(5) 0.6986(3) 0.4968(2) 0.0266(14) Uani 1 1 d . . . H80A H 1.1511 0.6875 0.4613 0.032 Uiso 1 1 calc R . . C81 C 1.1915(6) 0.7447(3) 0.5304(2) 0.0304(15) Uani 1 1 d . . . H81A H 1.2730 0.7642 0.5179 0.036 Uiso 1 1 calc R . . C82 C 1.1453(6) 0.7617(3) 0.5812(2) 0.0338(16) Uani 1 1 d . . . H82A H 1.1955 0.7928 0.6038 0.041 Uiso 1 1 calc R . . C83 C 1.0267(6) 0.7345(3) 0.6002(2) 0.0381(16) Uani 1 1 d . . . H83A H 0.9940 0.7475 0.6352 0.046 Uiso 1 1 calc R . . C84 C 0.9561(6) 0.6881(3) 0.5675(2) 0.0290(15) Uani 1 1 d . . . H84A H 0.8754 0.6687 0.5810 0.035 Uiso 1 1 calc R . . C85 C 1.0091(5) 0.5240(3) 0.4954(2) 0.0200(13) Uani 1 1 d . . . C86 C 1.1297(5) 0.5251(3) 0.5235(2) 0.0218(14) Uani 1 1 d . . . H86A H 1.1682 0.5687 0.5330 0.026 Uiso 1 1 calc R . . C87 C 1.1965(5) 0.4648(3) 0.5385(2) 0.0302(15) Uani 1 1 d . . . H87A H 1.2785 0.4676 0.5586 0.036 Uiso 1 1 calc R . . C88 C 1.1455(5) 0.4012(3) 0.5245(2) 0.0315(15) Uani 1 1 d . . . H88A H 1.1915 0.3598 0.5345 0.038 Uiso 1 1 calc R . . C89 C 1.0255(6) 0.3983(3) 0.4955(3) 0.0427(18) Uani 1 1 d . . . H89A H 0.9885 0.3544 0.4859 0.051 Uiso 1 1 calc R . . C90 C 0.9587(5) 0.4583(3) 0.4803(2) 0.0327(15) Uani 1 1 d . . . H90A H 0.8778 0.4552 0.4594 0.039 Uiso 1 1 calc R . . C91 C 0.7573(5) 0.5915(3) 0.5095(2) 0.0197(13) Uani 1 1 d . . . C92 C 0.6557(5) 0.6378(3) 0.4973(2) 0.0249(13) Uani 1 1 d . . . H92A H 0.6712 0.6739 0.4716 0.030 Uiso 1 1 calc R . . C93 C 0.5306(5) 0.6327(3) 0.5219(2) 0.0314(14) Uani 1 1 d . . . H93A H 0.4615 0.6646 0.5123 0.038 Uiso 1 1 calc R . . C94 C 0.5079(6) 0.5818(3) 0.5597(2) 0.0361(16) Uani 1 1 d . . . H94A H 0.4230 0.5782 0.5767 0.043 Uiso 1 1 calc R . . C95 C 0.6078(6) 0.5361(3) 0.5731(2) 0.0366(17) Uani 1 1 d . . . H95A H 0.5917 0.5008 0.5995 0.044 Uiso 1 1 calc R . . C96 C 0.7320(6) 0.5402(3) 0.5488(2) 0.0280(15) Uani 1 1 d . . . H96A H 0.8005 0.5082 0.5588 0.034 Uiso 1 1 calc R . . H98 H 0.518(4) 0.601(2) 0.8452(18) 0.052(16) Uiso 1 1 d . . . H99 H 1.078(4) 0.606(2) 0.3850(16) 0.032(13) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0229(3) 0.0198(3) 0.0144(2) 0.0001(2) 0.0026(2) 0.0010(2) Ru2 0.0224(2) 0.0160(2) 0.0140(2) -0.0004(2) 0.0007(2) -0.0025(2) Cl1 0.0504(10) 0.0277(8) 0.0301(9) -0.0065(7) 0.0128(8) -0.0136(7) Cl2 0.0494(10) 0.0705(13) 0.0154(8) -0.0059(8) 0.0009(7) 0.0020(9) Cl3 0.0515(12) 0.0817(14) 0.0373(11) -0.0277(10) 0.0034(9) 0.0275(10) Cl4 0.0648(12) 0.0199(8) 0.0343(9) 0.0010(7) 0.0174(9) 0.0071(8) Cl5 0.0547(11) 0.0669(12) 0.0160(8) 0.0106(8) -0.0073(8) -0.0273(9) Cl6 0.0492(11) 0.0661(12) 0.0271(9) 0.0105(9) 0.0015(8) -0.0355(9) P1 0.0191(8) 0.0189(8) 0.0158(8) 0.0017(6) 0.0025(6) 0.0032(6) P2 0.0219(8) 0.0196(8) 0.0154(7) -0.0010(7) -0.0007(6) -0.0049(6) O1 0.025(2) 0.032(2) 0.050(3) -0.007(2) 0.007(2) 0.0077(19) O2 0.034(3) 0.032(3) 0.066(3) 0.012(2) 0.010(2) 0.000(2) O3 0.030(2) 0.034(2) 0.030(2) 0.000(2) 0.005(2) -0.017(2) N1 0.020(3) 0.022(2) 0.020(3) 0.002(2) 0.000(2) 0.000(2) N2 0.020(3) 0.021(3) 0.026(3) 0.003(2) -0.003(2) -0.003(2) N3 0.025(2) 0.032(3) 0.012(2) 0.002(2) 0.0028(19) 0.000(2) N4 0.029(3) 0.021(2) 0.020(3) 0.000(2) 0.006(2) 0.001(2) N5 0.016(3) 0.019(2) 0.026(3) -0.005(2) 0.005(2) 0.003(2) N6 0.020(3) 0.019(3) 0.050(3) -0.007(2) 0.002(3) -0.005(2) N7 0.025(3) 0.024(3) 0.011(2) 0.004(2) 0.000(2) -0.006(2) N8 0.027(3) 0.024(3) 0.014(3) 0.001(2) -0.004(2) -0.009(2) C1 0.024(3) 0.022(3) 0.010(3) -0.001(2) -0.002(2) 0.007(3) C2 0.033(4) 0.017(3) 0.039(4) 0.006(3) 0.004(3) 0.001(3) C3 0.032(4) 0.022(3) 0.028(4) 0.008(3) 0.001(3) -0.003(3) C4 0.019(3) 0.020(3) 0.041(4) 0.000(3) -0.004(3) 0.003(3) C5 0.025(3) 0.040(4) 0.023(3) 0.002(3) -0.004(3) 0.003(3) C6 0.039(4) 0.080(6) 0.060(5) -0.040(4) 0.007(4) 0.011(4) C7 0.019(3) 0.037(4) 0.026(3) 0.008(3) 0.002(3) 0.002(3) C8 0.029(4) 0.023(3) 0.035(4) -0.001(3) 0.000(3) 0.003(3) C9 0.054(5) 0.044(4) 0.082(6) 0.034(4) 0.023(4) 0.000(4) C10 0.024(3) 0.021(3) 0.010(3) 0.002(2) 0.004(3) 0.007(2) C11 0.021(3) 0.038(4) 0.025(3) 0.002(3) -0.002(3) -0.002(3) C12 0.022(3) 0.047(4) 0.036(3) -0.008(4) 0.005(3) -0.001(3) C13 0.022(3) 0.034(4) 0.031(4) 0.004(3) 0.009(3) 0.007(3) C14 0.028(3) 0.028(3) 0.023(3) -0.005(3) 0.012(3) 0.011(3) C15 0.020(3) 0.028(3) 0.019(3) 0.000(3) 0.001(3) 0.003(2) C16 0.024(3) 0.013(3) 0.017(3) 0.001(2) 0.003(3) 0.010(2) C17 0.030(4) 0.025(3) 0.031(4) 0.011(3) 0.007(3) 0.004(3) C18 0.027(4) 0.030(4) 0.053(5) 0.009(3) 0.003(3) 0.012(3) C19 0.053(4) 0.023(3) 0.031(4) 0.008(3) -0.008(3) 0.012(3) C20 0.063(5) 0.036(4) 0.019(3) 0.003(3) 0.001(3) 0.011(3) C21 0.035(4) 0.026(3) 0.025(4) 0.001(3) 0.009(3) 0.015(3) C22 0.023(3) 0.022(3) 0.008(3) -0.004(2) 0.002(2) -0.006(2) C23 0.022(3) 0.021(3) 0.023(3) -0.002(3) -0.003(3) 0.005(2) C24 0.034(4) 0.017(3) 0.033(4) -0.002(3) 0.003(3) 0.009(3) C25 0.031(4) 0.023(3) 0.027(3) 0.002(3) 0.006(3) -0.002(3) C26 0.024(3) 0.033(4) 0.034(4) 0.002(3) -0.011(3) 0.003(3) C27 0.015(3) 0.022(3) 0.025(3) 0.007(3) 0.004(3) 0.001(2) C28 0.023(3) 0.017(3) 0.020(3) 0.001(3) 0.003(2) -0.005(2) C29 0.030(4) 0.037(4) 0.010(3) 0.000(3) 0.004(3) 0.007(3) C30 0.033(4) 0.066(5) 0.014(3) -0.013(3) -0.001(3) 0.009(4) C31 0.038(4) 0.076(5) 0.017(4) -0.007(4) -0.008(3) 0.015(4) C32 0.075(6) 0.081(6) 0.033(5) -0.002(4) -0.006(5) 0.039(5) C33 0.080(6) 0.045(4) 0.027(4) 0.011(3) 0.008(4) 0.028(4) C34 0.052(5) 0.055(5) 0.018(4) 0.006(3) 0.005(3) 0.011(4) C35 0.028(4) 0.071(5) 0.033(4) -0.018(4) 0.009(3) -0.011(3) C36 0.104(7) 0.150(9) 0.058(6) 0.001(6) -0.017(5) 0.077(6) C37 0.069(5) 0.046(4) 0.033(4) 0.008(3) 0.006(4) -0.020(4) C38 0.029(4) 0.044(4) 0.021(3) -0.010(3) 0.005(3) -0.010(3) C39 0.029(4) 0.046(4) 0.019(3) -0.017(3) 0.005(3) 0.006(3) C40 0.024(3) 0.024(3) 0.017(3) -0.007(3) -0.003(3) 0.003(3) C41 0.021(3) 0.022(3) 0.048(4) -0.005(3) 0.014(3) 0.004(3) C42 0.041(4) 0.012(3) 0.052(5) 0.009(3) -0.003(4) 0.002(3) C43 0.027(4) 0.028(4) 0.043(4) 0.009(3) 0.004(3) 0.008(3) C44 0.024(3) 0.033(4) 0.037(4) -0.006(3) 0.002(3) 0.007(3) C45 0.026(3) 0.028(3) 0.018(3) -0.003(3) 0.002(3) 0.005(3) C46 0.033(4) 0.031(4) 0.090(6) -0.008(4) 0.004(4) -0.004(3) C47 0.040(5) 0.057(5) 0.076(6) 0.032(4) -0.002(4) 0.006(4) C48 0.032(3) 0.031(4) 0.035(3) 0.007(3) 0.005(3) -0.004(3) C49 0.022(3) 0.024(3) 0.017(3) -0.001(3) 0.001(3) -0.001(3) C50 0.030(4) 0.018(3) 0.034(4) 0.000(3) 0.006(3) -0.007(3) C51 0.033(4) 0.017(3) 0.052(4) -0.015(3) -0.003(3) 0.001(3) C52 0.024(3) 0.029(3) 0.022(3) -0.002(3) -0.004(3) -0.005(3) C53 0.030(4) 0.032(3) 0.022(3) -0.005(3) 0.005(3) -0.002(3) C54 0.047(5) 0.073(5) 0.043(5) 0.011(4) 0.014(4) -0.022(4) C55 0.027(4) 0.044(4) 0.093(7) -0.032(4) -0.014(4) 0.007(3) C56 0.023(5) 0.033(7) 0.036(6) 0.004(5) -0.001(4) -0.001(5) O4 0.047(4) 0.030(4) 0.076(8) -0.023(5) 0.022(4) -0.006(3) C57 0.038(9) 0.059(11) 0.055(12) -0.025(7) 0.009(6) 0.020(5) C58 0.023(3) 0.015(3) 0.017(3) 0.002(2) -0.002(3) -0.003(2) C59 0.038(4) 0.033(3) 0.013(3) 0.005(3) -0.001(3) -0.012(3) C60 0.032(3) 0.027(3) 0.013(3) 0.010(3) 0.000(3) -0.007(3) C61 0.022(3) 0.025(3) 0.021(3) 0.000(3) -0.001(3) -0.012(3) C62 0.028(4) 0.025(3) 0.025(4) 0.001(3) 0.006(3) -0.011(3) C63 0.037(4) 0.028(3) 0.033(4) -0.011(3) 0.004(3) -0.013(3) C64 0.026(4) 0.065(5) 0.027(4) 0.011(4) -0.002(3) -0.021(3) C65 0.025(4) 0.049(4) 0.036(4) 0.009(3) -0.006(3) -0.007(3) C66 0.028(3) 0.029(3) 0.023(3) 0.005(3) 0.007(3) -0.003(3) C67 0.047(4) 0.025(3) 0.045(4) 0.013(3) -0.002(4) -0.001(3) C68 0.038(4) 0.083(6) 0.038(4) 0.002(4) -0.014(4) -0.026(4) C69 0.027(3) 0.038(4) 0.056(4) -0.002(4) 0.020(3) 0.004(3) C70 0.029(3) 0.024(3) 0.015(3) 0.005(3) -0.003(2) -0.010(3) C71 0.039(4) 0.027(3) 0.015(3) -0.001(3) 0.007(3) -0.014(3) C72 0.030(3) 0.050(4) 0.018(3) 0.001(3) 0.003(2) -0.009(3) C73 0.045(4) 0.051(4) 0.027(4) -0.001(3) 0.002(3) -0.024(4) C74 0.052(5) 0.033(4) 0.039(4) 0.007(3) -0.002(4) -0.013(3) C75 0.044(4) 0.024(3) 0.018(3) 0.009(3) -0.003(3) -0.003(3) C76 0.045(4) 0.029(4) 0.045(4) -0.007(3) 0.000(3) -0.004(3) C77 0.064(5) 0.085(6) 0.067(6) -0.015(5) 0.003(5) -0.046(5) C78 0.069(5) 0.032(4) 0.044(5) -0.008(3) -0.013(4) 0.009(4) C79 0.025(3) 0.016(3) 0.018(3) 0.005(2) -0.001(3) 0.004(2) C80 0.028(3) 0.027(3) 0.024(3) -0.008(3) -0.002(3) 0.001(3) C81 0.020(4) 0.031(3) 0.040(4) -0.004(3) -0.002(3) 0.001(3) C82 0.038(4) 0.031(4) 0.031(4) -0.014(3) -0.011(3) -0.003(3) C83 0.057(5) 0.036(4) 0.021(4) -0.011(3) 0.004(3) -0.004(3) C84 0.036(4) 0.023(3) 0.028(4) -0.007(3) 0.000(3) -0.007(3) C85 0.024(3) 0.023(3) 0.013(3) 0.001(2) 0.004(3) 0.001(3) C86 0.019(3) 0.022(3) 0.024(3) 0.002(3) 0.000(3) -0.003(2) C87 0.024(4) 0.036(4) 0.030(4) 0.001(3) 0.000(3) 0.012(3) C88 0.038(4) 0.027(3) 0.030(4) 0.007(3) 0.006(3) 0.000(3) C89 0.061(5) 0.020(3) 0.047(4) 0.006(3) -0.005(4) -0.001(3) C90 0.039(4) 0.025(3) 0.034(4) -0.002(3) -0.010(3) -0.006(3) C91 0.016(3) 0.026(3) 0.017(3) -0.001(2) 0.001(3) -0.005(2) C92 0.029(3) 0.026(3) 0.019(3) 0.002(3) 0.002(3) -0.002(3) C93 0.027(3) 0.038(4) 0.029(3) 0.003(3) 0.006(3) 0.006(3) C94 0.023(4) 0.050(4) 0.035(4) -0.006(3) 0.006(3) -0.011(3) C95 0.035(4) 0.057(4) 0.018(3) 0.001(3) 0.008(3) -0.021(3) C96 0.033(4) 0.032(3) 0.019(3) 0.000(3) -0.006(3) -0.008(3) _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 C1 1.975(5) . ? Ru1 C28 2.059(5) . ? Ru1 P1 2.3136(14) . ? Ru1 Cl1 2.4517(14) . ? Ru1 H98 1.49(4) . ? Ru2 C49 1.971(5) . ? Ru2 C58 2.036(5) . ? Ru2 P2 2.3106(14) . ? Ru2 Cl4 2.4496(14) . ? Ru2 H99 1.58(4) . ? Cl2 C38 1.693(6) . ? Cl3 C39 1.704(6) . ? Cl5 C59 1.714(5) . ? Cl6 C60 1.706(5) . ? P1 C22 1.839(5) . ? P1 C16 1.845(5) . ? P1 C10 1.851(5) . ? P2 C79 1.826(5) . ? P2 C85 1.837(5) . ? P2 C91 1.852(5) . ? O1 C5 1.409(6) . ? O1 C6 1.428(6) . ? O2 C8 1.403(6) . ? O2 C9 1.446(6) . ? O3 C54 1.419(6) . ? O3 C53 1.425(6) . ? N1 C1 1.380(6) . ? N1 C2 1.392(6) . ? N1 C4 1.454(6) . ? N2 C3 1.373(6) . ? N2 C1 1.374(6) . ? N2 C7 1.449(6) . ? N3 C38 1.387(6) . ? N3 C28 1.398(5) . ? N3 C29 1.450(6) . ? N4 C39 1.370(6) . ? N4 C28 1.383(6) . ? N4 C40 1.434(6) . ? N5 C49 1.377(6) . ? N5 C50 1.394(6) . ? N5 C52 1.445(6) . ? N6 C49 1.370(6) . ? N6 C51 1.388(6) . ? N6 C55 1.475(6) . ? N7 C60 1.378(6) . ? N7 C58 1.394(6) . ? N7 C61 1.440(6) . ? N8 C59 1.375(6) . ? N8 C58 1.401(6) . ? N8 C70 1.443(6) . ? C2 C3 1.340(6) . ? C2 H2A 0.9500 . ? C3 H3A 0.9500 . ? C4 C5 1.511(7) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.516(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C15 1.390(6) . ? C10 C11 1.398(6) . ? C11 C12 1.382(6) . ? C11 H11A 0.9500 . ? C12 C13 1.381(7) . ? C12 H12A 0.9500 . ? C13 C14 1.376(7) . ? C13 H13A 0.9500 . ? C14 C15 1.395(6) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 C21 1.371(7) . ? C16 C17 1.387(7) . ? C17 C18 1.387(7) . ? C17 H17A 0.9500 . ? C18 C19 1.375(7) . ? C18 H18A 0.9500 . ? C19 C20 1.397(7) . ? C19 H19A 0.9500 . ? C20 C21 1.377(7) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 C27 1.386(6) . ? C22 C23 1.399(6) . ? C23 C24 1.389(6) . ? C23 H23A 0.9500 . ? C24 C25 1.386(6) . ? C24 H24A 0.9500 . ? C25 C26 1.375(6) . ? C25 H25A 0.9500 . ? C26 C27 1.402(7) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? C29 C34 1.382(7) . ? C29 C30 1.394(7) . ? C30 C31 1.417(8) . ? C30 C35 1.483(8) . ? C31 C32 1.384(9) . ? C31 H31A 0.9500 . ? C32 C33 1.359(9) . ? C32 C36 1.538(8) . ? C33 C34 1.388(8) . ? C33 H33A 0.9500 . ? C34 C37 1.508(7) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.332(7) . ? C40 C45 1.395(7) . ? C40 C41 1.396(7) . ? C41 C42 1.371(7) . ? C41 C46 1.523(7) . ? C42 C43 1.397(7) . ? C42 H42A 0.9500 . ? C43 C44 1.369(7) . ? C43 C47 1.515(7) . ? C44 C45 1.406(7) . ? C44 H44A 0.9500 . ? C45 C48 1.488(7) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C50 C51 1.328(6) . ? C50 H50A 0.9500 . ? C51 H51A 0.9500 . ? C52 C53 1.507(6) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.408(10) . ? C55 C56A 1.60(3) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 O4 1.410(14) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? O4 C57 1.45(3) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C56A O4A 1.45(4) . ? C56A H56C 0.9900 . ? C56A H56D 0.9900 . ? O4A C57A 1.39(9) . ? C57A H57D 0.9800 . ? C57A H57E 0.9800 . ? C57A H57F 0.9800 . ? C59 C60 1.326(7) . ? C61 C66 1.392(7) . ? C61 C62 1.393(7) . ? C62 C63 1.402(7) . ? C62 C67 1.509(7) . ? C63 C64 1.400(8) . ? C63 H63A 0.9500 . ? C64 C65 1.377(8) . ? C64 C68 1.518(7) . ? C65 C66 1.391(7) . ? C65 H65A 0.9500 . ? C66 C69 1.488(7) . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 C75 1.389(7) . ? C70 C71 1.391(7) . ? C71 C72 1.380(7) . ? C71 C76 1.520(7) . ? C72 C73 1.401(8) . ? C72 H72A 0.9500 . ? C73 C74 1.378(8) . ? C73 C77 1.525(7) . ? C74 C75 1.393(7) . ? C74 H74A 0.9500 . ? C75 C78 1.490(7) . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 C84 1.388(7) . ? C79 C80 1.413(7) . ? C80 C81 1.400(7) . ? C80 H80A 0.9500 . ? C81 C82 1.365(7) . ? C81 H81A 0.9500 . ? C82 C83 1.382(7) . ? C82 H82A 0.9500 . ? C83 C84 1.382(7) . ? C83 H83A 0.9500 . ? C84 H84A 0.9500 . ? C85 C86 1.378(7) . ? C85 C90 1.408(7) . ? C86 C87 1.386(7) . ? C86 H86A 0.9500 . ? C87 C88 1.367(7) . ? C87 H87A 0.9500 . ? C88 C89 1.383(7) . ? C88 H88A 0.9500 . ? C89 C90 1.382(7) . ? C89 H89A 0.9500 . ? C90 H90A 0.9500 . ? C91 C92 1.379(7) . ? C91 C96 1.401(7) . ? C92 C93 1.396(6) . ? C92 H92A 0.9500 . ? C93 C94 1.367(7) . ? C93 H93A 0.9500 . ? C94 C95 1.367(7) . ? C94 H94A 0.9500 . ? C95 C96 1.384(7) . ? C95 H95A 0.9500 . ? C96 H96A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru1 C28 97.2(2) . . ? C1 Ru1 P1 91.04(14) . . ? C28 Ru1 P1 165.96(14) . . ? C1 Ru1 Cl1 144.57(15) . . ? C28 Ru1 Cl1 86.75(14) . . ? P1 Ru1 Cl1 93.07(5) . . ? C1 Ru1 H98 82.9(18) . . ? C28 Ru1 H98 88.5(17) . . ? P1 Ru1 H98 81.3(17) . . ? Cl1 Ru1 H98 132.5(18) . . ? C49 Ru2 C58 96.7(2) . . ? C49 Ru2 P2 92.59(15) . . ? C58 Ru2 P2 165.16(14) . . ? C49 Ru2 Cl4 142.69(16) . . ? C58 Ru2 Cl4 88.14(14) . . ? P2 Ru2 Cl4 91.44(5) . . ? C49 Ru2 H99 82.4(16) . . ? C58 Ru2 H99 84.1(14) . . ? P2 Ru2 H99 85.7(14) . . ? Cl4 Ru2 H99 134.9(16) . . ? C22 P1 C16 100.8(2) . . ? C22 P1 C10 102.4(2) . . ? C16 P1 C10 100.2(2) . . ? C22 P1 Ru1 115.90(17) . . ? C16 P1 Ru1 112.76(17) . . ? C10 P1 Ru1 121.74(17) . . ? C79 P2 C85 101.3(2) . . ? C79 P2 C91 101.1(2) . . ? C85 P2 C91 101.4(2) . . ? C79 P2 Ru2 111.42(17) . . ? C85 P2 Ru2 116.62(17) . . ? C91 P2 Ru2 122.00(17) . . ? C5 O1 C6 110.5(5) . . ? C8 O2 C9 110.9(4) . . ? C54 O3 C53 110.7(4) . . ? C1 N1 C2 111.9(4) . . ? C1 N1 C4 123.7(4) . . ? C2 N1 C4 124.1(4) . . ? C3 N2 C1 111.7(4) . . ? C3 N2 C7 123.0(4) . . ? C1 N2 C7 125.2(4) . . ? C38 N3 C28 111.5(4) . . ? C38 N3 C29 120.9(4) . . ? C28 N3 C29 127.7(4) . . ? C39 N4 C28 112.0(4) . . ? C39 N4 C40 121.1(4) . . ? C28 N4 C40 126.8(4) . . ? C49 N5 C50 112.0(4) . . ? C49 N5 C52 124.4(4) . . ? C50 N5 C52 123.5(4) . . ? C49 N6 C51 112.8(4) . . ? C49 N6 C55 124.8(5) . . ? C51 N6 C55 122.2(5) . . ? C60 N7 C58 112.1(4) . . ? C60 N7 C61 122.4(4) . . ? C58 N7 C61 125.5(4) . . ? C59 N8 C58 111.9(4) . . ? C59 N8 C70 121.7(4) . . ? C58 N8 C70 126.3(4) . . ? N2 C1 N1 102.5(4) . . ? N2 C1 Ru1 136.6(4) . . ? N1 C1 Ru1 120.9(4) . . ? C3 C2 N1 105.9(5) . . ? C3 C2 H2A 127.0 . . ? N1 C2 H2A 127.0 . . ? C2 C3 N2 108.0(5) . . ? C2 C3 H3A 126.0 . . ? N2 C3 H3A 126.0 . . ? N1 C4 C5 112.8(4) . . ? N1 C4 H4A 109.0 . . ? C5 C4 H4A 109.0 . . ? N1 C4 H4B 109.0 . . ? C5 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? O1 C5 C4 107.9(4) . . ? O1 C5 H5A 110.1 . . ? C4 C5 H5A 110.1 . . ? O1 C5 H5B 110.1 . . ? C4 C5 H5B 110.1 . . ? H5A C5 H5B 108.4 . . ? O1 C6 H6A 109.5 . . ? O1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? O1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 C8 112.9(4) . . ? N2 C7 H7A 109.0 . . ? C8 C7 H7A 109.0 . . ? N2 C7 H7B 109.0 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? O2 C8 C7 110.3(4) . . ? O2 C8 H8A 109.6 . . ? C7 C8 H8A 109.6 . . ? O2 C8 H8B 109.6 . . ? C7 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? O2 C9 H9A 109.5 . . ? O2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C15 C10 C11 118.0(5) . . ? C15 C10 P1 125.1(4) . . ? C11 C10 P1 116.9(4) . . ? C12 C11 C10 121.0(5) . . ? C12 C11 H11A 119.5 . . ? C10 C11 H11A 119.5 . . ? C13 C12 C11 120.0(5) . . ? C13 C12 H12A 120.0 . . ? C11 C12 H12A 120.0 . . ? C14 C13 C12 120.3(5) . . ? C14 C13 H13A 119.9 . . ? C12 C13 H13A 119.9 . . ? C13 C14 C15 119.7(5) . . ? C13 C14 H14A 120.2 . . ? C15 C14 H14A 120.2 . . ? C10 C15 C14 121.0(5) . . ? C10 C15 H15A 119.5 . . ? C14 C15 H15A 119.5 . . ? C21 C16 C17 118.1(5) . . ? C21 C16 P1 122.4(4) . . ? C17 C16 P1 119.5(4) . . ? C16 C17 C18 121.0(5) . . ? C16 C17 H17A 119.5 . . ? C18 C17 H17A 119.5 . . ? C19 C18 C17 119.8(6) . . ? C19 C18 H18A 120.1 . . ? C17 C18 H18A 120.1 . . ? C18 C19 C20 119.8(5) . . ? C18 C19 H19A 120.1 . . ? C20 C19 H19A 120.1 . . ? C21 C20 C19 119.0(5) . . ? C21 C20 H20A 120.5 . . ? C19 C20 H20A 120.5 . . ? C16 C21 C20 122.3(5) . . ? C16 C21 H21A 118.9 . . ? C20 C21 H21A 118.9 . . ? C27 C22 C23 118.5(5) . . ? C27 C22 P1 121.5(4) . . ? C23 C22 P1 119.9(4) . . ? C24 C23 C22 120.5(5) . . ? C24 C23 H23A 119.7 . . ? C22 C23 H23A 119.7 . . ? C25 C24 C23 120.9(5) . . ? C25 C24 H24A 119.5 . . ? C23 C24 H24A 119.5 . . ? C26 C25 C24 118.6(5) . . ? C26 C25 H25A 120.7 . . ? C24 C25 H25A 120.7 . . ? C25 C26 C27 121.1(5) . . ? C25 C26 H26A 119.4 . . ? C27 C26 H26A 119.4 . . ? C22 C27 C26 120.3(5) . . ? C22 C27 H27A 119.9 . . ? C26 C27 H27A 119.9 . . ? N4 C28 N3 101.7(4) . . ? N4 C28 Ru1 124.8(4) . . ? N3 C28 Ru1 133.4(4) . . ? C34 C29 C30 121.9(6) . . ? C34 C29 N3 119.1(5) . . ? C30 C29 N3 118.6(5) . . ? C29 C30 C31 117.7(6) . . ? C29 C30 C35 122.7(6) . . ? C31 C30 C35 119.5(6) . . ? C32 C31 C30 120.6(7) . . ? C32 C31 H31A 119.7 . . ? C30 C31 H31A 119.7 . . ? C33 C32 C31 119.1(7) . . ? C33 C32 C36 121.3(8) . . ? C31 C32 C36 119.5(8) . . ? C32 C33 C34 122.7(7) . . ? C32 C33 H33A 118.7 . . ? C34 C33 H33A 118.7 . . ? C29 C34 C33 117.9(6) . . ? C29 C34 C37 120.7(6) . . ? C33 C34 C37 121.3(6) . . ? C30 C35 H35A 109.5 . . ? C30 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C30 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C32 C36 H36A 109.5 . . ? C32 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C32 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C34 C37 H37A 109.5 . . ? C34 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C34 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C39 C38 N3 106.8(5) . . ? C39 C38 Cl2 130.2(5) . . ? N3 C38 Cl2 123.1(4) . . ? C38 C39 N4 108.1(5) . . ? C38 C39 Cl3 128.6(5) . . ? N4 C39 Cl3 123.3(4) . . ? C45 C40 C41 122.3(5) . . ? C45 C40 N4 117.0(5) . . ? C41 C40 N4 120.3(5) . . ? C42 C41 C40 117.6(5) . . ? C42 C41 C46 120.8(5) . . ? C40 C41 C46 121.5(5) . . ? C41 C42 C43 122.4(5) . . ? C41 C42 H42A 118.8 . . ? C43 C42 H42A 118.8 . . ? C44 C43 C42 118.6(5) . . ? C44 C43 C47 120.6(5) . . ? C42 C43 C47 120.8(5) . . ? C43 C44 C45 121.7(5) . . ? C43 C44 H44A 119.2 . . ? C45 C44 H44A 119.2 . . ? C40 C45 C44 117.4(5) . . ? C40 C45 C48 120.9(5) . . ? C44 C45 C48 121.7(5) . . ? C41 C46 H46A 109.5 . . ? C41 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C41 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C43 C47 H47A 109.5 . . ? C43 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C43 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N6 C49 N5 101.7(4) . . ? N6 C49 Ru2 137.4(4) . . ? N5 C49 Ru2 120.9(4) . . ? C51 C50 N5 106.9(5) . . ? C51 C50 H50A 126.6 . . ? N5 C50 H50A 126.6 . . ? C50 C51 N6 106.6(5) . . ? C50 C51 H51A 126.7 . . ? N6 C51 H51A 126.7 . . ? N5 C52 C53 113.0(4) . . ? N5 C52 H52A 109.0 . . ? C53 C52 H52A 109.0 . . ? N5 C52 H52B 109.0 . . ? C53 C52 H52B 109.0 . . ? H52A C52 H52B 107.8 . . ? O3 C53 C52 109.5(4) . . ? O3 C53 H53A 109.8 . . ? C52 C53 H53A 109.8 . . ? O3 C53 H53B 109.8 . . ? C52 C53 H53B 109.8 . . ? H53A C53 H53B 108.2 . . ? O3 C54 H54A 109.5 . . ? O3 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? O3 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C56 C55 N6 115.5(6) . . ? C56 C55 C56A 23.7(12) . . ? N6 C55 C56A 115.1(13) . . ? C56 C55 H55A 108.4 . . ? N6 C55 H55A 108.4 . . ? C56A C55 H55A 126.5 . . ? C56 C55 H55B 108.4 . . ? N6 C55 H55B 108.4 . . ? C56A C55 H55B 87.1 . . ? H55A C55 H55B 107.5 . . ? C55 C56 O4 113.9(9) . . ? C55 C56 H56A 108.8 . . ? O4 C56 H56A 108.8 . . ? C55 C56 H56B 108.8 . . ? O4 C56 H56B 108.8 . . ? H56A C56 H56B 107.7 . . ? C56 O4 C57 115.6(15) . . ? O4 C57 H57A 109.5 . . ? O4 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? O4 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? O4A C56A C55 119(3) . . ? O4A C56A H56C 107.5 . . ? C55 C56A H56C 107.5 . . ? O4A C56A H56D 107.5 . . ? C55 C56A H56D 107.5 . . ? H56C C56A H56D 107.0 . . ? C57A O4A C56A 106(5) . . ? O4A C57A H57D 109.5 . . ? O4A C57A H57E 109.5 . . ? H57D C57A H57E 109.5 . . ? O4A C57A H57F 109.5 . . ? H57D C57A H57F 109.5 . . ? H57E C57A H57F 109.5 . . ? N7 C58 N8 100.9(4) . . ? N7 C58 Ru2 125.5(4) . . ? N8 C58 Ru2 133.5(4) . . ? C60 C59 N8 107.6(5) . . ? C60 C59 Cl5 128.9(5) . . ? N8 C59 Cl5 123.5(4) . . ? C59 C60 N7 107.4(5) . . ? C59 C60 Cl6 128.5(4) . . ? N7 C60 Cl6 124.1(4) . . ? C66 C61 C62 122.1(5) . . ? C66 C61 N7 118.2(5) . . ? C62 C61 N7 119.2(5) . . ? C61 C62 C63 117.4(5) . . ? C61 C62 C67 123.8(5) . . ? C63 C62 C67 118.7(5) . . ? C64 C63 C62 121.4(5) . . ? C64 C63 H63A 119.3 . . ? C62 C63 H63A 119.3 . . ? C65 C64 C63 119.0(5) . . ? C65 C64 C68 121.6(6) . . ? C63 C64 C68 119.4(6) . . ? C64 C65 C66 121.4(6) . . ? C64 C65 H65A 119.3 . . ? C66 C65 H65A 119.3 . . ? C65 C66 C61 118.6(5) . . ? C65 C66 C69 120.2(5) . . ? C61 C66 C69 121.2(5) . . ? C62 C67 H67A 109.5 . . ? C62 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C62 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C64 C68 H68A 109.5 . . ? C64 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C64 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C66 C69 H69A 109.5 . . ? C66 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C66 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C75 C70 C71 122.1(5) . . ? C75 C70 N8 118.8(5) . . ? C71 C70 N8 118.7(5) . . ? C72 C71 C70 118.3(5) . . ? C72 C71 C76 119.1(5) . . ? C70 C71 C76 122.5(5) . . ? C71 C72 C73 121.3(6) . . ? C71 C72 H72A 119.4 . . ? C73 C72 H72A 119.4 . . ? C74 C73 C72 118.5(5) . . ? C74 C73 C77 122.0(6) . . ? C72 C73 C77 119.5(6) . . ? C73 C74 C75 122.0(6) . . ? C73 C74 H74A 119.0 . . ? C75 C74 H74A 119.0 . . ? C70 C75 C74 117.6(5) . . ? C70 C75 C78 122.0(5) . . ? C74 C75 C78 120.5(5) . . ? C71 C76 H76A 109.5 . . ? C71 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C71 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C73 C77 H77A 109.5 . . ? C73 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C73 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C75 C78 H78A 109.5 . . ? C75 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C75 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C84 C79 C80 117.7(5) . . ? C84 C79 P2 124.0(4) . . ? C80 C79 P2 118.1(4) . . ? C81 C80 C79 119.8(5) . . ? C81 C80 H80A 120.1 . . ? C79 C80 H80A 120.1 . . ? C82 C81 C80 120.3(6) . . ? C82 C81 H81A 119.9 . . ? C80 C81 H81A 119.9 . . ? C81 C82 C83 121.0(5) . . ? C81 C82 H82A 119.5 . . ? C83 C82 H82A 119.5 . . ? C82 C83 C84 119.0(5) . . ? C82 C83 H83A 120.5 . . ? C84 C83 H83A 120.5 . . ? C83 C84 C79 122.2(5) . . ? C83 C84 H84A 118.9 . . ? C79 C84 H84A 118.9 . . ? C86 C85 C90 116.8(5) . . ? C86 C85 P2 123.8(4) . . ? C90 C85 P2 119.2(4) . . ? C85 C86 C87 122.1(5) . . ? C85 C86 H86A 118.9 . . ? C87 C86 H86A 118.9 . . ? C88 C87 C86 120.6(5) . . ? C88 C87 H87A 119.7 . . ? C86 C87 H87A 119.7 . . ? C87 C88 C89 118.7(5) . . ? C87 C88 H88A 120.6 . . ? C89 C88 H88A 120.6 . . ? C90 C89 C88 121.0(6) . . ? C90 C89 H89A 119.5 . . ? C88 C89 H89A 119.5 . . ? C89 C90 C85 120.7(5) . . ? C89 C90 H90A 119.7 . . ? C85 C90 H90A 119.7 . . ? C92 C91 C96 117.6(5) . . ? C92 C91 P2 117.7(4) . . ? C96 C91 P2 124.7(4) . . ? C91 C92 C93 121.5(5) . . ? C91 C92 H92A 119.3 . . ? C93 C92 H92A 119.3 . . ? C94 C93 C92 119.8(5) . . ? C94 C93 H93A 120.1 . . ? C92 C93 H93A 120.1 . . ? C95 C94 C93 119.7(6) . . ? C95 C94 H94A 120.2 . . ? C93 C94 H94A 120.2 . . ? C94 C95 C96 121.1(6) . . ? C94 C95 H95A 119.4 . . ? C96 C95 H95A 119.4 . . ? C95 C96 C91 120.2(6) . . ? C95 C96 H96A 119.9 . . ? C91 C96 H96A 119.9 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.573 _refine_diff_density_min -0.444 _refine_diff_density_rms 0.081 _database_code_depnum_ccdc_archive 'CCDC 973559' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound9 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C50 H53 Cl N4 O P Ru' _chemical_formula_weight 893.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 34.768(5) _cell_length_b 14.8467(17) _cell_length_c 21.575(4) _cell_angle_alpha 90.00 _cell_angle_beta 128.344(9) _cell_angle_gamma 90.00 _cell_volume 8735(2) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9997 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 27.38 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.359 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3720 _exptl_absorpt_coefficient_mu 0.499 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9068 _exptl_absorpt_correction_T_max 0.9426 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 74117 _diffrn_reflns_av_R_equivalents 0.0699 _diffrn_reflns_av_unetI/netI 0.0526 _diffrn_reflns_limit_h_min -43 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 27.59 _reflns_number_total 10076 _reflns_number_gt 7422 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0342P)^2^+14.3378P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10076 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0655 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.0903 _refine_ls_wR_factor_gt 0.0794 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.143826(7) 0.224859(13) 0.648096(12) 0.01860(6) Uani 1 1 d . . . Cl1 Cl 0.20235(3) 0.34809(4) 0.72279(5) 0.03591(18) Uani 1 1 d . . . P1 P 0.08138(2) 0.32913(4) 0.59512(4) 0.01960(15) Uani 1 1 d . . . O1 O 0.09009(11) 0.18184(18) 0.84997(17) 0.0661(8) Uani 1 1 d . . . N1 N 0.24415(8) 0.11732(14) 0.76045(13) 0.0235(5) Uani 1 1 d . . . N2 N 0.22165(8) 0.12724(14) 0.64329(13) 0.0256(5) Uani 1 1 d . . . N3 N 0.08347(8) 0.07645(14) 0.62739(14) 0.0278(5) Uani 1 1 d . . . N4 N 0.11177(8) 0.13872(15) 0.73905(14) 0.0268(5) Uani 1 1 d . . . C1 C 0.20621(9) 0.14759(16) 0.68688(16) 0.0213(6) Uani 1 1 d . . . C2 C 0.28149(10) 0.07945(19) 0.76231(18) 0.0333(7) Uani 1 1 d . . . H2A H 0.3111 0.0539 0.8069 0.040 Uiso 1 1 calc R . . C3 C 0.26749(10) 0.0861(2) 0.68914(19) 0.0357(7) Uani 1 1 d . . . H3A H 0.2854 0.0664 0.6718 0.043 Uiso 1 1 calc R . . C4 C 0.24693(9) 0.11577(17) 0.83015(16) 0.0253(6) Uani 1 1 d . . . C5 C 0.27698(10) 0.17783(18) 0.89080(17) 0.0274(6) Uani 1 1 d . . . C6 C 0.28100(10) 0.1696(2) 0.95878(17) 0.0335(7) Uani 1 1 d . . . H6A H 0.3000 0.2127 0.9998 0.040 Uiso 1 1 calc R . . C7 C 0.25835(11) 0.1010(2) 0.96886(18) 0.0359(7) Uani 1 1 d . . . C8 C 0.23032(11) 0.0389(2) 0.90823(19) 0.0359(7) Uani 1 1 d . . . H8A H 0.2149 -0.0088 0.9148 0.043 Uiso 1 1 calc R . . C9 C 0.22414(10) 0.04464(18) 0.83774(18) 0.0301(7) Uani 1 1 d . . . C10 C 0.30540(11) 0.24852(19) 0.88482(19) 0.0367(7) Uani 1 1 d . . . H10A H 0.3240 0.2851 0.9330 0.055 Uiso 1 1 calc R . . H10B H 0.2827 0.2872 0.8391 0.055 Uiso 1 1 calc R . . H10C H 0.3281 0.2194 0.8785 0.055 Uiso 1 1 calc R . . C11 C 0.26488(14) 0.0930(3) 1.0449(2) 0.0563(10) Uani 1 1 d . . . H11A H 0.2463 0.0410 1.0416 0.084 Uiso 1 1 calc R . . H11B H 0.2528 0.1479 1.0529 0.084 Uiso 1 1 calc R . . H11C H 0.2997 0.0850 1.0893 0.084 Uiso 1 1 calc R . . C12 C 0.19588(11) -0.02618(19) 0.77399(19) 0.0393(8) Uani 1 1 d . . . H12A H 0.1954 -0.0105 0.7294 0.059 Uiso 1 1 calc R . . H12B H 0.1622 -0.0290 0.7560 0.059 Uiso 1 1 calc R . . H12C H 0.2117 -0.0849 0.7953 0.059 Uiso 1 1 calc R . . C13 C 0.19596(10) 0.14431(18) 0.56046(16) 0.0256(6) Uani 1 1 d . . . C14 C 0.16775(10) 0.07538(19) 0.50633(18) 0.0311(7) Uani 1 1 d . . . C15 C 0.14470(11) 0.0926(2) 0.42742(19) 0.0362(7) Uani 1 1 d . . . H15A H 0.1249 0.0468 0.3896 0.043 Uiso 1 1 calc R . . C16 C 0.14946(11) 0.1743(2) 0.40152(18) 0.0364(7) Uani 1 1 d . . . C17 C 0.17938(11) 0.2395(2) 0.45773(18) 0.0330(7) Uani 1 1 d . . . H17A H 0.1837 0.2950 0.4409 0.040 Uiso 1 1 calc R . . C18 C 0.20331(10) 0.22630(18) 0.53784(16) 0.0265(6) Uani 1 1 d . . . C19 C 0.23629(11) 0.29767(19) 0.59703(19) 0.0363(7) Uani 1 1 d . . . H19A H 0.2367 0.3498 0.5696 0.055 Uiso 1 1 calc R . . H19B H 0.2696 0.2737 0.6345 0.055 Uiso 1 1 calc R . . H19C H 0.2241 0.3162 0.6257 0.055 Uiso 1 1 calc R . . C20 C 0.12304(12) 0.1927(3) 0.31509(19) 0.0533(10) Uani 1 1 d . . . H20A H 0.1310 0.2537 0.3087 0.080 Uiso 1 1 calc R . . H20B H 0.0876 0.1877 0.2862 0.080 Uiso 1 1 calc R . . H20C H 0.1334 0.1488 0.2941 0.080 Uiso 1 1 calc R . . C21 C 0.16218(13) -0.01488(19) 0.5326(2) 0.0460(9) Uani 1 1 d . . . H21A H 0.1412 -0.0541 0.4865 0.069 Uiso 1 1 calc R . . H21B H 0.1473 -0.0062 0.5586 0.069 Uiso 1 1 calc R . . H21C H 0.1945 -0.0429 0.5698 0.069 Uiso 1 1 calc R . . C22 C 0.11322(9) 0.14486(16) 0.67713(15) 0.0218(6) Uani 1 1 d . . . C23 C 0.10023(10) 0.14376(18) 0.55228(17) 0.0277(6) Uani 1 1 d . . . H23A H 0.0973 0.1535 0.5060 0.033 Uiso 1 1 calc R . . C24 C 0.07594(10) 0.07721(18) 0.55510(18) 0.0315(7) Uani 1 1 d . . . H24A H 0.0559 0.0352 0.5136 0.038 Uiso 1 1 calc R . . C25 C 0.06409(11) 0.02849(19) 0.6573(2) 0.0377(8) Uani 1 1 d . . . H25A H 0.0425 -0.0216 0.6334 0.045 Uiso 1 1 calc R . . C26 C 0.08188(11) 0.0669(2) 0.7268(2) 0.0373(8) Uani 1 1 d . . . H26A H 0.0753 0.0484 0.7615 0.045 Uiso 1 1 calc R . . C27 C 0.13695(11) 0.2009(2) 0.80522(17) 0.0327(7) Uani 1 1 d . . . H27A H 0.1532 0.2477 0.7962 0.039 Uiso 1 1 calc R . . H27B H 0.1628 0.1677 0.8538 0.039 Uiso 1 1 calc R . . C28 C 0.10370(12) 0.2459(2) 0.81805(18) 0.0360(7) Uani 1 1 d . . . H28A H 0.1209 0.2972 0.8549 0.043 Uiso 1 1 calc R . . H28B H 0.0741 0.2692 0.7673 0.043 Uiso 1 1 calc R . . C29 C 0.05964(17) 0.2183(3) 0.8662(3) 0.0801(14) Uani 1 1 d . . . H29A H 0.0515 0.1712 0.8881 0.120 Uiso 1 1 calc R . . H29B H 0.0295 0.2415 0.8172 0.120 Uiso 1 1 calc R . . H29C H 0.0769 0.2675 0.9045 0.120 Uiso 1 1 calc R . . C30 C 0.09193(9) 0.41363(17) 0.54517(15) 0.0216(5) Uani 1 1 d . . . C31 C 0.08829(10) 0.50579(17) 0.55068(16) 0.0263(6) Uani 1 1 d . . . H31A H 0.0776 0.5283 0.5789 0.032 Uiso 1 1 calc R . . C32 C 0.10017(10) 0.56564(19) 0.51537(17) 0.0320(7) Uani 1 1 d . . . H32A H 0.0974 0.6287 0.5194 0.038 Uiso 1 1 calc R . . C33 C 0.11596(11) 0.5339(2) 0.47446(18) 0.0378(8) Uani 1 1 d . . . H33A H 0.1245 0.5749 0.4509 0.045 Uiso 1 1 calc R . . C34 C 0.11931(11) 0.4420(2) 0.46789(19) 0.0379(8) Uani 1 1 d . . . H34A H 0.1296 0.4199 0.4389 0.045 Uiso 1 1 calc R . . C35 C 0.10780(11) 0.38213(19) 0.50307(18) 0.0320(7) Uani 1 1 d . . . H35A H 0.1106 0.3192 0.4988 0.038 Uiso 1 1 calc R . . C36 C 0.01837(10) 0.29144(16) 0.51690(16) 0.0233(6) Uani 1 1 d . . . C37 C -0.00993(10) 0.32660(19) 0.44075(16) 0.0280(6) Uani 1 1 d . . . H37A H 0.0030 0.3738 0.4287 0.034 Uiso 1 1 calc R . . C38 C -0.05661(11) 0.2940(2) 0.38208(19) 0.0390(8) Uani 1 1 d . . . H38A H -0.0754 0.3188 0.3304 0.047 Uiso 1 1 calc R . . C39 C -0.07596(11) 0.2255(2) 0.3987(2) 0.0396(8) Uani 1 1 d . . . H39A H -0.1078 0.2025 0.3583 0.048 Uiso 1 1 calc R . . C40 C -0.04885(11) 0.1907(2) 0.4739(2) 0.0367(7) Uani 1 1 d . . . H40A H -0.0622 0.1441 0.4856 0.044 Uiso 1 1 calc R . . C41 C -0.00196(10) 0.22346(18) 0.53317(18) 0.0314(6) Uani 1 1 d . . . H41A H 0.0163 0.1993 0.5850 0.038 Uiso 1 1 calc R . . C42 C 0.07273(10) 0.39920(16) 0.65646(16) 0.0225(6) Uani 1 1 d . . . C43 C 0.02667(11) 0.41664(19) 0.63567(17) 0.0307(6) Uani 1 1 d . . . H43A H -0.0016 0.3914 0.5884 0.037 Uiso 1 1 calc R . . C44 C 0.02138(11) 0.4700(2) 0.68252(18) 0.0380(8) Uani 1 1 d . . . H44A H -0.0104 0.4804 0.6674 0.046 Uiso 1 1 calc R . . C45 C 0.06150(12) 0.5078(2) 0.75047(18) 0.0361(7) Uani 1 1 d . . . H45A H 0.0577 0.5448 0.7823 0.043 Uiso 1 1 calc R . . C46 C 0.10740(11) 0.4918(2) 0.77221(19) 0.0369(7) Uani 1 1 d . . . H46A H 0.1353 0.5184 0.8191 0.044 Uiso 1 1 calc R . . C47 C 0.11335(11) 0.43709(19) 0.72620(18) 0.0324(7) Uani 1 1 d . . . H47A H 0.1453 0.4256 0.7425 0.039 Uiso 1 1 calc R . . C100 C 0.00750(15) 0.7444(3) 0.7863(2) 0.0684(12) Uani 1 1 d . . . H10E H 0.0124 0.6885 0.8117 0.082 Uiso 1 1 calc R . . C101 C 0.01598(14) 0.8197(4) 0.8253(2) 0.0697(13) Uani 1 1 d . . . H10D H 0.0271 0.8166 0.8781 0.084 Uiso 1 1 calc R . . C102 C 0.00899(16) 0.9039(3) 0.7909(3) 0.0917(19) Uani 1 1 d . . . H10F H 0.0156 0.9582 0.8191 0.110 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 0.01871(11) 0.01758(10) 0.02133(12) 0.00328(9) 0.01332(9) 0.00381(8) Cl1 0.0241(4) 0.0250(3) 0.0500(5) -0.0068(3) 0.0187(4) -0.0004(3) P1 0.0208(3) 0.0193(3) 0.0224(4) 0.0037(3) 0.0153(3) 0.0044(3) O1 0.101(2) 0.0649(16) 0.089(2) 0.0140(15) 0.087(2) 0.0140(15) N1 0.0214(12) 0.0230(11) 0.0264(13) 0.0045(9) 0.0150(11) 0.0063(9) N2 0.0242(12) 0.0266(11) 0.0262(13) 0.0003(10) 0.0157(11) 0.0069(9) N3 0.0245(12) 0.0221(11) 0.0343(14) 0.0010(10) 0.0170(12) -0.0009(9) N4 0.0267(13) 0.0300(12) 0.0269(13) 0.0071(10) 0.0183(11) 0.0033(10) C1 0.0226(14) 0.0169(12) 0.0256(15) 0.0005(10) 0.0156(13) 0.0011(10) C2 0.0248(15) 0.0351(16) 0.0336(18) 0.0032(13) 0.0149(14) 0.0131(12) C3 0.0258(16) 0.0401(17) 0.0399(19) 0.0001(14) 0.0198(15) 0.0125(13) C4 0.0206(14) 0.0259(13) 0.0285(16) 0.0098(12) 0.0149(13) 0.0085(11) C5 0.0217(14) 0.0275(14) 0.0278(16) 0.0058(12) 0.0127(13) 0.0063(11) C6 0.0252(16) 0.0434(17) 0.0231(16) 0.0025(13) 0.0106(14) 0.0069(13) C7 0.0293(16) 0.0486(18) 0.0291(17) 0.0157(15) 0.0178(15) 0.0166(14) C8 0.0292(16) 0.0357(16) 0.046(2) 0.0208(15) 0.0251(16) 0.0129(13) C9 0.0221(15) 0.0268(14) 0.0355(18) 0.0104(12) 0.0150(14) 0.0102(11) C10 0.0328(17) 0.0347(16) 0.0345(18) 0.0004(13) 0.0168(15) -0.0047(13) C11 0.053(2) 0.082(3) 0.043(2) 0.021(2) 0.034(2) 0.017(2) C12 0.0331(17) 0.0267(15) 0.051(2) 0.0063(14) 0.0229(17) 0.0020(13) C13 0.0207(14) 0.0311(14) 0.0269(16) -0.0032(12) 0.0158(13) 0.0053(11) C14 0.0268(15) 0.0315(15) 0.0383(18) -0.0107(13) 0.0219(15) 0.0002(12) C15 0.0239(15) 0.0467(18) 0.0373(19) -0.0170(15) 0.0187(15) -0.0016(13) C16 0.0250(16) 0.059(2) 0.0266(17) -0.0060(15) 0.0169(14) 0.0107(14) C17 0.0327(16) 0.0401(16) 0.0346(18) 0.0049(14) 0.0251(15) 0.0082(13) C18 0.0237(14) 0.0319(14) 0.0295(16) -0.0035(13) 0.0192(13) 0.0020(12) C19 0.0386(18) 0.0351(16) 0.044(2) -0.0092(14) 0.0300(17) -0.0089(13) C20 0.037(2) 0.090(3) 0.0300(19) -0.0001(18) 0.0193(17) 0.0156(19) C21 0.049(2) 0.0279(16) 0.070(3) -0.0121(16) 0.041(2) -0.0039(14) C22 0.0197(13) 0.0218(12) 0.0222(14) 0.0054(11) 0.0121(12) 0.0050(10) C23 0.0244(15) 0.0332(15) 0.0235(15) -0.0003(12) 0.0138(13) 0.0088(12) C24 0.0273(16) 0.0296(14) 0.0302(17) -0.0095(13) 0.0142(14) 0.0010(12) C25 0.0363(18) 0.0250(14) 0.054(2) 0.0047(14) 0.0291(17) -0.0020(13) C26 0.0370(18) 0.0362(16) 0.052(2) 0.0210(15) 0.0337(17) 0.0083(14) C27 0.0295(16) 0.0459(17) 0.0216(15) 0.0045(13) 0.0153(14) 0.0088(13) C28 0.0379(18) 0.0470(18) 0.0274(17) 0.0075(14) 0.0223(15) 0.0100(14) C29 0.088(3) 0.113(4) 0.089(3) -0.010(3) 0.079(3) -0.004(3) C30 0.0196(13) 0.0248(13) 0.0184(14) 0.0048(11) 0.0108(12) 0.0042(10) C31 0.0239(14) 0.0286(14) 0.0221(15) 0.0019(12) 0.0122(13) 0.0002(11) C32 0.0312(16) 0.0261(14) 0.0273(16) 0.0043(12) 0.0125(14) -0.0043(12) C33 0.0304(17) 0.0448(18) 0.0353(18) 0.0143(15) 0.0190(15) -0.0042(14) C34 0.0377(18) 0.0509(19) 0.0391(19) 0.0158(15) 0.0308(17) 0.0124(15) C35 0.0352(17) 0.0326(15) 0.0377(18) 0.0102(13) 0.0274(15) 0.0118(13) C36 0.0226(14) 0.0231(13) 0.0276(15) -0.0003(11) 0.0172(13) 0.0048(10) C37 0.0280(15) 0.0336(15) 0.0242(16) -0.0020(12) 0.0171(14) 0.0012(12) C38 0.0337(17) 0.052(2) 0.0270(17) -0.0086(14) 0.0168(15) 0.0012(14) C39 0.0283(16) 0.0463(18) 0.042(2) -0.0196(16) 0.0208(16) -0.0071(14) C40 0.0341(17) 0.0303(15) 0.056(2) -0.0053(15) 0.0333(18) -0.0026(13) C41 0.0300(16) 0.0278(14) 0.0409(18) 0.0061(13) 0.0242(15) 0.0056(12) C42 0.0255(14) 0.0212(12) 0.0256(15) 0.0070(11) 0.0182(13) 0.0076(10) C43 0.0279(16) 0.0384(16) 0.0255(16) -0.0004(13) 0.0165(14) 0.0077(12) C44 0.0320(17) 0.0529(19) 0.0356(19) -0.0022(15) 0.0242(16) 0.0121(14) C45 0.0449(19) 0.0397(17) 0.0350(19) -0.0010(14) 0.0303(17) 0.0082(14) C46 0.0344(18) 0.0411(17) 0.0361(19) -0.0116(14) 0.0224(16) -0.0019(14) C47 0.0287(16) 0.0363(16) 0.0357(18) -0.0051(13) 0.0218(15) 0.0009(12) C100 0.049(2) 0.092(3) 0.069(3) 0.006(2) 0.039(3) 0.003(2) C101 0.035(2) 0.130(4) 0.038(2) -0.016(3) 0.0194(19) -0.016(3) C102 0.056(3) 0.091(3) 0.157(6) -0.065(3) 0.081(4) -0.032(3) _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 C22 1.940(3) . ? Ru1 C23 2.033(3) . ? Ru1 C1 2.114(2) . ? Ru1 P1 2.3104(7) . ? Ru1 Cl1 2.4528(8) . ? P1 C30 1.833(3) . ? P1 C36 1.837(3) . ? P1 C42 1.849(3) . ? O1 C29 1.412(4) . ? O1 C28 1.417(4) . ? N1 C1 1.365(3) . ? N1 C2 1.392(3) . ? N1 C4 1.446(3) . ? N2 C1 1.375(3) . ? N2 C3 1.392(3) . ? N2 C13 1.441(3) . ? N3 C22 1.370(3) . ? N3 C25 1.384(4) . ? N3 C24 1.413(4) . ? N4 C22 1.371(3) . ? N4 C26 1.395(4) . ? N4 C27 1.451(4) . ? C2 C3 1.336(4) . ? C2 H2A 0.9500 . ? C3 H3A 0.9500 . ? C4 C9 1.390(4) . ? C4 C5 1.399(4) . ? C5 C6 1.390(4) . ? C5 C10 1.501(4) . ? C6 C7 1.385(4) . ? C6 H6A 0.9500 . ? C7 C8 1.389(4) . ? C7 C11 1.514(4) . ? C8 C9 1.400(4) . ? C8 H8A 0.9500 . ? C9 C12 1.512(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C18 1.393(4) . ? C13 C14 1.397(4) . ? C14 C15 1.383(4) . ? C14 C21 1.514(4) . ? C15 C16 1.388(4) . ? C15 H15A 0.9500 . ? C16 C17 1.387(4) . ? C16 C20 1.507(4) . ? C17 C18 1.391(4) . ? C17 H17A 0.9500 . ? C18 C19 1.501(4) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C23 C24 1.325(4) . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? C25 C26 1.344(4) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C27 C28 1.503(4) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.386(4) . ? C30 C35 1.403(4) . ? C31 C32 1.390(4) . ? C31 H31A 0.9500 . ? C32 C33 1.380(4) . ? C32 H32A 0.9500 . ? C33 C34 1.385(4) . ? C33 H33A 0.9500 . ? C34 C35 1.379(4) . ? C34 H34A 0.9500 . ? C35 H35A 0.9500 . ? C36 C37 1.391(4) . ? C36 C41 1.396(4) . ? C37 C38 1.386(4) . ? C37 H37A 0.9500 . ? C38 C39 1.384(4) . ? C38 H38A 0.9500 . ? C39 C40 1.376(4) . ? C39 H39A 0.9500 . ? C40 C41 1.394(4) . ? C40 H40A 0.9500 . ? C41 H41A 0.9500 . ? C42 C47 1.392(4) . ? C42 C43 1.393(4) . ? C43 C44 1.383(4) . ? C43 H43A 0.9500 . ? C44 C45 1.369(4) . ? C44 H44A 0.9500 . ? C45 C46 1.376(4) . ? C45 H45A 0.9500 . ? C46 C47 1.394(4) . ? C46 H46A 0.9500 . ? C47 H47A 0.9500 . ? C100 C100 1.310(8) 2_556 ? C100 C101 1.316(6) . ? C100 H10E 0.9500 . ? C101 C102 1.396(6) . ? C101 H10D 0.9500 . ? C102 C102 1.460(10) 2_556 ? C102 H10F 0.9500 . ? 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 C22 Ru1 C23 75.72(12) . . ? C22 Ru1 C1 100.00(10) . . ? C23 Ru1 C1 90.91(10) . . ? C22 Ru1 P1 91.98(7) . . ? C23 Ru1 P1 90.84(7) . . ? C1 Ru1 P1 167.96(7) . . ? C22 Ru1 Cl1 129.96(8) . . ? C23 Ru1 Cl1 154.31(9) . . ? C1 Ru1 Cl1 85.15(7) . . ? P1 Ru1 Cl1 88.12(3) . . ? C30 P1 C36 103.18(12) . . ? C30 P1 C42 102.50(11) . . ? C36 P1 C42 101.43(12) . . ? C30 P1 Ru1 106.26(8) . . ? C36 P1 Ru1 118.01(8) . . ? C42 P1 Ru1 122.90(9) . . ? C29 O1 C28 113.0(3) . . ? C1 N1 C2 112.2(2) . . ? C1 N1 C4 127.4(2) . . ? C2 N1 C4 120.3(2) . . ? C1 N2 C3 111.8(2) . . ? C1 N2 C13 127.3(2) . . ? C3 N2 C13 120.9(2) . . ? C22 N3 C25 111.5(2) . . ? C22 N3 C24 113.1(2) . . ? C25 N3 C24 135.1(3) . . ? C22 N4 C26 109.9(2) . . ? C22 N4 C27 123.5(2) . . ? C26 N4 C27 126.6(2) . . ? N1 C1 N2 102.6(2) . . ? N1 C1 Ru1 130.75(18) . . ? N2 C1 Ru1 126.06(19) . . ? C3 C2 N1 106.7(2) . . ? C3 C2 H2A 126.7 . . ? N1 C2 H2A 126.7 . . ? C2 C3 N2 106.8(2) . . ? C2 C3 H3A 126.6 . . ? N2 C3 H3A 126.6 . . ? C9 C4 C5 122.7(3) . . ? C9 C4 N1 117.4(2) . . ? C5 C4 N1 119.4(2) . . ? C6 C5 C4 117.2(3) . . ? C6 C5 C10 120.8(3) . . ? C4 C5 C10 122.0(3) . . ? C7 C6 C5 122.4(3) . . ? C7 C6 H6A 118.8 . . ? C5 C6 H6A 118.8 . . ? C6 C7 C8 118.4(3) . . ? C6 C7 C11 120.7(3) . . ? C8 C7 C11 120.9(3) . . ? C7 C8 C9 121.9(3) . . ? C7 C8 H8A 119.1 . . ? C9 C8 H8A 119.1 . . ? C4 C9 C8 117.4(3) . . ? C4 C9 C12 121.2(3) . . ? C8 C9 C12 121.4(3) . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C7 C11 H11A 109.5 . . ? C7 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C7 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C18 C13 C14 122.2(3) . . ? C18 C13 N2 118.8(2) . . ? C14 C13 N2 118.8(2) . . ? C15 C14 C13 117.6(3) . . ? C15 C14 C21 120.9(3) . . ? C13 C14 C21 121.5(3) . . ? C14 C15 C16 122.3(3) . . ? C14 C15 H15A 118.9 . . ? C16 C15 H15A 118.9 . . ? C17 C16 C15 118.0(3) . . ? C17 C16 C20 120.4(3) . . ? C15 C16 C20 121.6(3) . . ? C16 C17 C18 122.3(3) . . ? C16 C17 H17A 118.8 . . ? C18 C17 H17A 118.8 . . ? C17 C18 C13 117.4(3) . . ? C17 C18 C19 120.7(3) . . ? C13 C18 C19 121.9(3) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C16 C20 H20A 109.5 . . ? C16 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C16 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C14 C21 H21A 109.5 . . ? C14 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C14 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N3 C22 N4 104.3(2) . . ? N3 C22 Ru1 119.99(19) . . ? N4 C22 Ru1 135.6(2) . . ? C24 C23 Ru1 119.3(2) . . ? C24 C23 H23A 120.4 . . ? Ru1 C23 H23A 120.4 . . ? C23 C24 N3 111.7(2) . . ? C23 C24 H24A 124.2 . . ? N3 C24 H24A 124.2 . . ? C26 C25 N3 106.4(3) . . ? C26 C25 H25A 126.8 . . ? N3 C25 H25A 126.8 . . ? C25 C26 N4 108.0(3) . . ? C25 C26 H26A 126.0 . . ? N4 C26 H26A 126.0 . . ? N4 C27 C28 113.6(2) . . ? N4 C27 H27A 108.8 . . ? C28 C27 H27A 108.8 . . ? N4 C27 H27B 108.8 . . ? C28 C27 H27B 108.8 . . ? H27A C27 H27B 107.7 . . ? O1 C28 C27 108.5(2) . . ? O1 C28 H28A 110.0 . . ? C27 C28 H28A 110.0 . . ? O1 C28 H28B 110.0 . . ? C27 C28 H28B 110.0 . . ? H28A C28 H28B 108.4 . . ? O1 C29 H29A 109.5 . . ? O1 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? O1 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 C35 118.6(2) . . ? C31 C30 P1 124.3(2) . . ? C35 C30 P1 117.05(19) . . ? C30 C31 C32 120.7(3) . . ? C30 C31 H31A 119.7 . . ? C32 C31 H31A 119.7 . . ? C33 C32 C31 120.2(3) . . ? C33 C32 H32A 119.9 . . ? C31 C32 H32A 119.9 . . ? C32 C33 C34 119.6(3) . . ? C32 C33 H33A 120.2 . . ? C34 C33 H33A 120.2 . . ? C35 C34 C33 120.5(3) . . ? C35 C34 H34A 119.8 . . ? C33 C34 H34A 119.8 . . ? C34 C35 C30 120.4(3) . . ? C34 C35 H35A 119.8 . . ? C30 C35 H35A 119.8 . . ? C37 C36 C41 118.1(3) . . ? C37 C36 P1 122.5(2) . . ? C41 C36 P1 119.4(2) . . ? C38 C37 C36 121.2(3) . . ? C38 C37 H37A 119.4 . . ? C36 C37 H37A 119.4 . . ? C39 C38 C37 120.1(3) . . ? C39 C38 H38A 119.9 . . ? C37 C38 H38A 119.9 . . ? C40 C39 C38 119.6(3) . . ? C40 C39 H39A 120.2 . . ? C38 C39 H39A 120.2 . . ? C39 C40 C41 120.5(3) . . ? C39 C40 H40A 119.8 . . ? C41 C40 H40A 119.8 . . ? C40 C41 C36 120.5(3) . . ? C40 C41 H41A 119.7 . . ? C36 C41 H41A 119.7 . . ? C47 C42 C43 117.7(2) . . ? C47 C42 P1 119.7(2) . . ? C43 C42 P1 122.6(2) . . ? C44 C43 C42 121.2(3) . . ? C44 C43 H43A 119.4 . . ? C42 C43 H43A 119.4 . . ? C45 C44 C43 120.6(3) . . ? C45 C44 H44A 119.7 . . ? C43 C44 H44A 119.7 . . ? C44 C45 C46 119.3(3) . . ? C44 C45 H45A 120.3 . . ? C46 C45 H45A 120.3 . . ? C45 C46 C47 120.7(3) . . ? C45 C46 H46A 119.6 . . ? C47 C46 H46A 119.6 . . ? C42 C47 C46 120.4(3) . . ? C42 C47 H47A 119.8 . . ? C46 C47 H47A 119.8 . . ? C100 C100 C101 121.9(3) 2_556 . ? C100 C100 H10E 119.0 2_556 . ? C101 C100 H10E 119.0 . . ? C100 C101 C102 121.6(4) . . ? C100 C101 H10D 119.2 . . ? C102 C101 H10D 119.2 . . ? C101 C102 C102 116.4(3) . 2_556 ? C101 C102 H10F 121.8 . . ? C102 C102 H10F 121.8 2_556 . ? 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 C22 Ru1 P1 C30 -171.62(12) . . . . ? C23 Ru1 P1 C30 -95.88(12) . . . . ? C1 Ru1 P1 C30 2.5(4) . . . . ? Cl1 Ru1 P1 C30 58.45(9) . . . . ? C22 Ru1 P1 C36 -56.53(13) . . . . ? C23 Ru1 P1 C36 19.21(13) . . . . ? C1 Ru1 P1 C36 117.5(4) . . . . ? Cl1 Ru1 P1 C36 173.54(10) . . . . ? C22 Ru1 P1 C42 71.17(13) . . . . ? C23 Ru1 P1 C42 146.92(13) . . . . ? C1 Ru1 P1 C42 -114.8(4) . . . . ? Cl1 Ru1 P1 C42 -58.76(10) . . . . ? C2 N1 C1 N2 -0.2(3) . . . . ? C4 N1 C1 N2 -175.8(2) . . . . ? C2 N1 C1 Ru1 -171.4(2) . . . . ? C4 N1 C1 Ru1 13.1(4) . . . . ? C3 N2 C1 N1 -0.1(3) . . . . ? C13 N2 C1 N1 -179.9(2) . . . . ? C3 N2 C1 Ru1 171.66(19) . . . . ? C13 N2 C1 Ru1 -8.2(4) . . . . ? C22 Ru1 C1 N1 -60.9(2) . . . . ? C23 Ru1 C1 N1 -136.6(2) . . . . ? P1 Ru1 C1 N1 125.1(3) . . . . ? Cl1 Ru1 C1 N1 68.8(2) . . . . ? C22 Ru1 C1 N2 129.8(2) . . . . ? C23 Ru1 C1 N2 54.1(2) . . . . ? P1 Ru1 C1 N2 -44.2(5) . . . . ? Cl1 Ru1 C1 N2 -100.5(2) . . . . ? C1 N1 C2 C3 0.4(3) . . . . ? C4 N1 C2 C3 176.3(2) . . . . ? N1 C2 C3 N2 -0.4(3) . . . . ? C1 N2 C3 C2 0.3(3) . . . . ? C13 N2 C3 C2 -179.8(2) . . . . ? C1 N1 C4 C9 81.7(3) . . . . ? C2 N1 C4 C9 -93.6(3) . . . . ? C1 N1 C4 C5 -106.3(3) . . . . ? C2 N1 C4 C5 78.4(3) . . . . ? C9 C4 C5 C6 -4.2(4) . . . . ? N1 C4 C5 C6 -175.7(2) . . . . ? C9 C4 C5 C10 173.6(3) . . . . ? N1 C4 C5 C10 2.1(4) . . . . ? C4 C5 C6 C7 2.9(4) . . . . ? C10 C5 C6 C7 -174.9(3) . . . . ? C5 C6 C7 C8 -0.6(4) . . . . ? C5 C6 C7 C11 178.2(3) . . . . ? C6 C7 C8 C9 -0.7(4) . . . . ? C11 C7 C8 C9 -179.5(3) . . . . ? C5 C4 C9 C8 3.0(4) . . . . ? N1 C4 C9 C8 174.7(2) . . . . ? C5 C4 C9 C12 -174.1(2) . . . . ? N1 C4 C9 C12 -2.4(4) . . . . ? C7 C8 C9 C4 -0.5(4) . . . . ? C7 C8 C9 C12 176.6(3) . . . . ? C1 N2 C13 C18 89.2(3) . . . . ? C3 N2 C13 C18 -90.6(3) . . . . ? C1 N2 C13 C14 -95.9(3) . . . . ? C3 N2 C13 C14 84.3(3) . . . . ? C18 C13 C14 C15 -3.4(4) . . . . ? N2 C13 C14 C15 -178.0(2) . . . . ? C18 C13 C14 C21 177.0(3) . . . . ? N2 C13 C14 C21 2.4(4) . . . . ? C13 C14 C15 C16 1.0(4) . . . . ? C21 C14 C15 C16 -179.4(3) . . . . ? C14 C15 C16 C17 1.4(4) . . . . ? C14 C15 C16 C20 -178.4(3) . . . . ? C15 C16 C17 C18 -1.7(4) . . . . ? C20 C16 C17 C18 178.1(3) . . . . ? C16 C17 C18 C13 -0.4(4) . . . . ? C16 C17 C18 C19 178.6(3) . . . . ? C14 C13 C18 C17 3.1(4) . . . . ? N2 C13 C18 C17 177.7(2) . . . . ? C14 C13 C18 C19 -176.0(2) . . . . ? N2 C13 C18 C19 -1.3(4) . . . . ? C25 N3 C22 N4 -0.3(3) . . . . ? C24 N3 C22 N4 173.7(2) . . . . ? C25 N3 C22 Ru1 -178.36(18) . . . . ? C24 N3 C22 Ru1 -4.4(3) . . . . ? C26 N4 C22 N3 0.6(3) . . . . ? C27 N4 C22 N3 -177.7(2) . . . . ? C26 N4 C22 Ru1 178.2(2) . . . . ? C27 N4 C22 Ru1 -0.1(4) . . . . ? C23 Ru1 C22 N3 4.33(19) . . . . ? C1 Ru1 C22 N3 -84.0(2) . . . . ? P1 Ru1 C22 N3 94.70(19) . . . . ? Cl1 Ru1 C22 N3 -176.10(15) . . . . ? C23 Ru1 C22 N4 -173.0(3) . . . . ? C1 Ru1 C22 N4 98.6(3) . . . . ? P1 Ru1 C22 N4 -82.6(3) . . . . ? Cl1 Ru1 C22 N4 6.6(3) . . . . ? C22 Ru1 C23 C24 -3.8(2) . . . . ? C1 Ru1 C23 C24 96.3(2) . . . . ? P1 Ru1 C23 C24 -95.6(2) . . . . ? Cl1 Ru1 C23 C24 176.98(14) . . . . ? Ru1 C23 C24 N3 2.6(3) . . . . ? C22 N3 C24 C23 1.0(3) . . . . ? C25 N3 C24 C23 173.1(3) . . . . ? C22 N3 C25 C26 -0.1(3) . . . . ? C24 N3 C25 C26 -172.3(3) . . . . ? N3 C25 C26 N4 0.5(3) . . . . ? C22 N4 C26 C25 -0.7(3) . . . . ? C27 N4 C26 C25 177.5(3) . . . . ? C22 N4 C27 C28 123.9(3) . . . . ? C26 N4 C27 C28 -54.1(4) . . . . ? C29 O1 C28 C27 178.5(3) . . . . ? N4 C27 C28 O1 72.9(3) . . . . ? C36 P1 C30 C31 99.4(2) . . . . ? C42 P1 C30 C31 -5.7(3) . . . . ? Ru1 P1 C30 C31 -135.8(2) . . . . ? C36 P1 C30 C35 -85.0(2) . . . . ? C42 P1 C30 C35 169.9(2) . . . . ? Ru1 P1 C30 C35 39.8(2) . . . . ? C35 C30 C31 C32 -0.1(4) . . . . ? P1 C30 C31 C32 175.5(2) . . . . ? C30 C31 C32 C33 -0.2(4) . . . . ? C31 C32 C33 C34 0.8(4) . . . . ? C32 C33 C34 C35 -1.1(5) . . . . ? C33 C34 C35 C30 0.8(5) . . . . ? C31 C30 C35 C34 -0.2(4) . . . . ? P1 C30 C35 C34 -176.1(2) . . . . ? C30 P1 C36 C37 -0.6(2) . . . . ? C42 P1 C36 C37 105.3(2) . . . . ? Ru1 P1 C36 C37 -117.4(2) . . . . ? C30 P1 C36 C41 177.8(2) . . . . ? C42 P1 C36 C41 -76.3(2) . . . . ? Ru1 P1 C36 C41 61.1(2) . . . . ? C41 C36 C37 C38 -1.3(4) . . . . ? P1 C36 C37 C38 177.2(2) . . . . ? C36 C37 C38 C39 0.1(4) . . . . ? C37 C38 C39 C40 0.9(4) . . . . ? C38 C39 C40 C41 -0.7(4) . . . . ? C39 C40 C41 C36 -0.5(4) . . . . ? C37 C36 C41 C40 1.5(4) . . . . ? P1 C36 C41 C40 -177.0(2) . . . . ? C30 P1 C42 C47 -77.3(2) . . . . ? C36 P1 C42 C47 176.3(2) . . . . ? Ru1 P1 C42 C47 41.7(2) . . . . ? C30 P1 C42 C43 102.4(2) . . . . ? C36 P1 C42 C43 -4.1(2) . . . . ? Ru1 P1 C42 C43 -138.6(2) . . . . ? C47 C42 C43 C44 0.2(4) . . . . ? P1 C42 C43 C44 -179.5(2) . . . . ? C42 C43 C44 C45 0.7(5) . . . . ? C43 C44 C45 C46 -0.5(5) . . . . ? C44 C45 C46 C47 -0.6(5) . . . . ? C43 C42 C47 C46 -1.2(4) . . . . ? P1 C42 C47 C46 178.5(2) . . . . ? C45 C46 C47 C42 1.4(5) . . . . ? C100 C100 C101 C102 0.6(8) 2_556 . . . ? C100 C101 C102 C102 1.0(7) . . . 2_556 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.59 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.688 _refine_diff_density_min -0.460 _refine_diff_density_rms 0.078 _database_code_depnum_ccdc_archive 'CCDC 973560' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound10 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C50 H55 Cl N4 O P Ru' _chemical_formula_weight 895.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M I2/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 21.7335(12) _cell_length_b 14.9240(6) _cell_length_c 26.9039(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.324(4) _cell_angle_gamma 90.00 _cell_volume 8726.2(7) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9972 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 27.50 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.363 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3736 _exptl_absorpt_coefficient_mu 0.499 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6992 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 69611 _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_unetI/netI 0.0392 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 27.56 _reflns_number_total 10073 _reflns_number_gt 7770 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+20.5148P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10073 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0587 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0906 _refine_ls_wR_factor_gt 0.0803 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.006040(9) 0.724689(12) 0.144694(7) 0.01909(6) Uani 1 1 d . . . Cl1 Cl 0.02235(4) 0.84658(4) 0.20483(2) 0.03477(16) Uani 1 1 d . . . P1 P 0.01464(3) 0.82883(4) 0.08127(2) 0.02086(14) Uani 1 1 d . . . O1 O 0.26095(11) 0.68830(19) 0.09291(11) 0.0689(8) Uani 1 1 d . . . N1 N 0.04781(11) 0.57848(14) 0.08373(8) 0.0301(5) Uani 1 1 d . . . N2 N 0.12934(10) 0.64268(15) 0.11326(8) 0.0292(5) Uani 1 1 d . . . N3 N 0.02008(9) 0.62508(13) 0.24660(7) 0.0223(4) Uani 1 1 d . . . N4 N -0.07442(10) 0.62669(14) 0.22164(8) 0.0263(5) Uani 1 1 d . . . C1 C 0.06660(12) 0.64697(16) 0.11421(9) 0.0237(5) Uani 1 1 d . . . C2 C 0.09732(16) 0.53231(19) 0.06485(11) 0.0419(8) Uani 1 1 d . . . H2A H 0.0959 0.4823 0.0430 0.050 Uiso 1 1 calc R . . C3 C 0.14789(15) 0.5719(2) 0.08340(11) 0.0420(8) Uani 1 1 d . . . H3A H 0.1892 0.5545 0.0772 0.050 Uiso 1 1 calc R . . C4 C -0.01612(14) 0.57745(18) 0.07536(10) 0.0345(7) Uani 1 1 d . . . H4A H -0.0367 0.5351 0.0548 0.041 Uiso 1 1 calc R . . C5 C -0.04416(13) 0.64298(17) 0.09975(9) 0.0293(6) Uani 1 1 d . . . H5A H -0.0873 0.6516 0.0962 0.035 Uiso 1 1 calc R . . C6 C 0.16900(13) 0.7060(2) 0.13901(10) 0.0344(6) Uani 1 1 d . . . H6A H 0.1917 0.6741 0.1657 0.041 Uiso 1 1 calc R . . H6B H 0.1432 0.7524 0.1549 0.041 Uiso 1 1 calc R . . C7 C 0.21474(13) 0.7512(2) 0.10522(11) 0.0391(7) Uani 1 1 d . . . H7A H 0.1938 0.7725 0.0747 0.047 Uiso 1 1 calc R . . H7B H 0.2334 0.8035 0.1222 0.047 Uiso 1 1 calc R . . C8 C -0.01660(11) 0.64864(14) 0.20828(9) 0.0208(5) Uani 1 1 d . . . C9 C -0.01277(12) 0.58463(17) 0.28902(9) 0.0284(6) Uani 1 1 d . . . H9A H -0.0073 0.6208 0.3196 0.034 Uiso 1 1 calc R . . H9B H 0.0015 0.5227 0.2954 0.034 Uiso 1 1 calc R . . C10 C -0.07875(13) 0.5858(2) 0.27159(10) 0.0381(7) Uani 1 1 d . . . H10D H -0.0958 0.5244 0.2697 0.046 Uiso 1 1 calc R . . H10E H -0.1047 0.6224 0.2939 0.046 Uiso 1 1 calc R . . C11 C -0.13098(11) 0.64425(16) 0.19576(9) 0.0232(5) Uani 1 1 d . . . C12 C -0.15750(13) 0.57649(17) 0.16693(10) 0.0304(6) Uani 1 1 d . . . C13 C -0.21372(14) 0.5933(2) 0.14444(10) 0.0367(7) Uani 1 1 d . . . H13A H -0.2318 0.5481 0.1243 0.044 Uiso 1 1 calc R . . C14 C -0.24462(13) 0.6740(2) 0.15026(10) 0.0356(7) Uani 1 1 d . . . C15 C -0.21835(12) 0.73794(19) 0.18077(10) 0.0316(6) Uani 1 1 d . . . H15A H -0.2396 0.7927 0.1860 0.038 Uiso 1 1 calc R . . C16 C -0.16173(12) 0.72493(17) 0.20411(9) 0.0253(5) Uani 1 1 d . . . C17 C -0.12586(16) 0.48726(18) 0.15976(13) 0.0472(8) Uani 1 1 d . . . H17A H -0.0866 0.4872 0.1779 0.071 Uiso 1 1 calc R . . H17B H -0.1183 0.4776 0.1243 0.071 Uiso 1 1 calc R . . H17C H -0.1522 0.4392 0.1725 0.071 Uiso 1 1 calc R . . C18 C -0.30540(14) 0.6911(3) 0.12443(12) 0.0534(9) Uani 1 1 d . . . H18A H -0.3200 0.7514 0.1327 0.080 Uiso 1 1 calc R . . H18B H -0.3357 0.6468 0.1355 0.080 Uiso 1 1 calc R . . H18C H -0.3000 0.6861 0.0884 0.080 Uiso 1 1 calc R . . C19 C -0.13570(14) 0.79626(19) 0.23760(11) 0.0367(7) Uani 1 1 d . . . H19A H -0.0960 0.7763 0.2510 0.055 Uiso 1 1 calc R . . H19B H -0.1642 0.8073 0.2650 0.055 Uiso 1 1 calc R . . H19C H -0.1300 0.8516 0.2186 0.055 Uiso 1 1 calc R . . C20 C 0.08599(12) 0.61941(16) 0.24708(9) 0.0232(5) Uani 1 1 d . . . C21 C 0.11358(12) 0.54625(16) 0.22404(9) 0.0267(6) Uani 1 1 d . . . C22 C 0.17716(13) 0.53630(18) 0.22900(10) 0.0328(6) Uani 1 1 d . . . H22A H 0.1968 0.4871 0.2132 0.039 Uiso 1 1 calc R . . C23 C 0.21254(13) 0.5962(2) 0.25636(10) 0.0339(6) Uani 1 1 d . . . C24 C 0.18317(13) 0.66717(19) 0.27931(10) 0.0324(6) Uani 1 1 d . . . H24A H 0.2071 0.7090 0.2977 0.039 Uiso 1 1 calc R . . C25 C 0.11979(12) 0.67942(17) 0.27639(9) 0.0270(6) Uani 1 1 d . . . C26 C 0.07555(14) 0.47753(17) 0.19647(10) 0.0334(6) Uani 1 1 d . . . H26A H 0.1027 0.4312 0.1829 0.050 Uiso 1 1 calc R . . H26B H 0.0531 0.5068 0.1692 0.050 Uiso 1 1 calc R . . H26C H 0.0461 0.4500 0.2193 0.050 Uiso 1 1 calc R . . C27 C 0.28111(14) 0.5842(3) 0.26116(13) 0.0538(9) Uani 1 1 d . . . H27A H 0.2938 0.5314 0.2422 0.081 Uiso 1 1 calc R . . H27B H 0.2921 0.5760 0.2962 0.081 Uiso 1 1 calc R . . H27C H 0.3020 0.6374 0.2482 0.081 Uiso 1 1 calc R . . C28 C 0.09021(14) 0.75318(18) 0.30576(11) 0.0353(7) Uani 1 1 d . . . H28A H 0.0457 0.7531 0.2995 0.053 Uiso 1 1 calc R . . H28B H 0.1075 0.8110 0.2957 0.053 Uiso 1 1 calc R . . H28C H 0.0981 0.7436 0.3413 0.053 Uiso 1 1 calc R . . C29 C -0.04593(12) 0.91165(16) 0.09207(9) 0.0233(5) Uani 1 1 d . . . C30 C -0.03779(13) 1.00351(17) 0.08761(9) 0.0278(6) Uani 1 1 d . . . H30A H 0.0003 1.0263 0.0760 0.033 Uiso 1 1 calc R . . C31 C -0.08460(14) 1.06233(18) 0.09984(10) 0.0363(7) Uani 1 1 d . . . H31A H -0.0784 1.1251 0.0967 0.044 Uiso 1 1 calc R . . C32 C -0.14008(15) 1.0301(2) 0.11647(10) 0.0405(7) Uani 1 1 d . . . H32A H -0.1719 1.0707 0.1254 0.049 Uiso 1 1 calc R . . C33 C -0.14963(14) 0.9388(2) 0.12026(11) 0.0431(8) Uani 1 1 d . . . H33A H -0.1883 0.9164 0.1309 0.052 Uiso 1 1 calc R . . C34 C -0.10264(13) 0.87988(19) 0.10843(10) 0.0345(6) Uani 1 1 d . . . H34A H -0.1091 0.8172 0.1115 0.041 Uiso 1 1 calc R . . C35 C 0.08371(11) 0.89949(15) 0.07313(9) 0.0232(5) Uani 1 1 d . . . C36 C 0.10935(13) 0.91577(19) 0.02684(10) 0.0337(6) Uani 1 1 d . . . H36A H 0.0912 0.8897 -0.0019 0.040 Uiso 1 1 calc R . . C37 C 0.16103(14) 0.9696(2) 0.02195(11) 0.0402(7) Uani 1 1 d . . . H37A H 0.1781 0.9796 -0.0100 0.048 Uiso 1 1 calc R . . C38 C 0.18769(13) 1.0085(2) 0.06298(11) 0.0380(7) Uani 1 1 d . . . H38A H 0.2231 1.0452 0.0596 0.046 Uiso 1 1 calc R . . C39 C 0.16249(14) 0.9935(2) 0.10888(11) 0.0395(7) Uani 1 1 d . . . H39A H 0.1803 1.0210 0.1374 0.047 Uiso 1 1 calc R . . C40 C 0.11130(13) 0.93877(19) 0.11428(11) 0.0347(6) Uani 1 1 d . . . H40A H 0.0950 0.9281 0.1464 0.042 Uiso 1 1 calc R . . C41 C -0.00036(12) 0.79141(16) 0.01714(9) 0.0250(5) Uani 1 1 d . . . C42 C 0.03628(14) 0.72462(18) -0.00328(10) 0.0338(6) Uani 1 1 d . . . H42A H 0.0700 0.7014 0.0153 0.041 Uiso 1 1 calc R . . C43 C 0.02391(15) 0.6916(2) -0.05047(11) 0.0407(7) Uani 1 1 d . . . H43A H 0.0491 0.6456 -0.0639 0.049 Uiso 1 1 calc R . . C44 C -0.02483(15) 0.7250(2) -0.07809(11) 0.0433(8) Uani 1 1 d . . . H44A H -0.0333 0.7019 -0.1103 0.052 Uiso 1 1 calc R . . C45 C -0.06080(14) 0.7918(2) -0.05859(11) 0.0420(7) Uani 1 1 d . . . H45A H -0.0941 0.8154 -0.0775 0.050 Uiso 1 1 calc R . . C46 C -0.04874(12) 0.82513(18) -0.01146(10) 0.0309(6) Uani 1 1 d . . . H46A H -0.0738 0.8716 0.0015 0.037 Uiso 1 1 calc R . . C47 C 0.30602(18) 0.7239(3) 0.06101(17) 0.0805(14) Uani 1 1 d . . . H47A H 0.3367 0.6777 0.0536 0.121 Uiso 1 1 calc R . . H47B H 0.3262 0.7750 0.0772 0.121 Uiso 1 1 calc R . . H47C H 0.2865 0.7438 0.0300 0.121 Uiso 1 1 calc R . . C100 C -0.2783(2) 0.7583(4) -0.00775(15) 0.0760(13) Uani 1 1 d . . . H10A H -0.2986 0.8138 -0.0132 0.091 Uiso 1 1 calc R . . C101 C -0.3085(2) 0.6824(4) -0.01622(14) 0.0777(14) Uani 1 1 d . . . H10B H -0.3500 0.6853 -0.0275 0.093 Uiso 1 1 calc R . . C102 C -0.2818(2) 0.5996(4) -0.00915(17) 0.100(2) Uani 1 1 d . . . H10C H -0.3034 0.5455 -0.0158 0.120 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 0.01774(11) 0.01833(9) 0.02120(10) 0.00428(7) 0.00151(7) 0.00087(8) Cl1 0.0546(5) 0.0229(3) 0.0269(3) 0.0007(2) 0.0033(3) -0.0038(3) P1 0.0191(3) 0.0209(3) 0.0226(3) 0.0053(2) 0.0018(3) 0.0003(2) O1 0.0314(13) 0.0762(17) 0.100(2) 0.0175(16) 0.0287(14) 0.0084(13) N1 0.0400(14) 0.0224(10) 0.0279(12) -0.0010(9) 0.0042(10) 0.0017(10) N2 0.0237(12) 0.0347(11) 0.0294(12) 0.0047(9) 0.0043(10) 0.0062(10) N3 0.0200(11) 0.0246(10) 0.0224(10) 0.0073(8) 0.0011(9) -0.0008(8) N4 0.0212(12) 0.0314(11) 0.0264(11) 0.0104(9) 0.0009(9) -0.0018(9) C1 0.0248(14) 0.0249(11) 0.0214(12) 0.0046(9) 0.0012(10) 0.0019(10) C2 0.057(2) 0.0287(14) 0.0401(17) -0.0039(12) 0.0136(16) 0.0080(14) C3 0.0431(19) 0.0402(16) 0.0429(18) 0.0052(13) 0.0153(15) 0.0204(15) C4 0.0386(18) 0.0351(14) 0.0298(15) -0.0006(11) -0.0013(13) -0.0158(13) C5 0.0255(15) 0.0357(14) 0.0266(14) 0.0077(11) -0.0049(11) -0.0100(11) C6 0.0217(14) 0.0515(17) 0.0299(15) 0.0094(12) -0.0024(12) 0.0015(12) C7 0.0234(15) 0.0561(18) 0.0379(16) 0.0131(14) -0.0005(13) 0.0024(13) C8 0.0206(13) 0.0143(10) 0.0275(13) 0.0018(9) 0.0016(10) 0.0000(9) C9 0.0297(15) 0.0299(13) 0.0257(13) 0.0087(10) 0.0010(11) -0.0034(11) C10 0.0300(16) 0.0507(17) 0.0336(16) 0.0223(13) 0.0028(13) -0.0031(14) C11 0.0180(13) 0.0281(12) 0.0235(13) 0.0059(10) 0.0023(10) -0.0039(10) C12 0.0305(16) 0.0287(13) 0.0320(15) 0.0034(11) 0.0073(12) -0.0083(11) C13 0.0332(17) 0.0478(17) 0.0290(15) 0.0000(12) 0.0013(13) -0.0188(14) C14 0.0217(15) 0.0574(18) 0.0276(15) 0.0134(13) -0.0007(12) -0.0099(13) C15 0.0231(14) 0.0385(14) 0.0333(15) 0.0095(12) 0.0068(12) 0.0034(12) C16 0.0224(13) 0.0294(12) 0.0241(13) 0.0038(10) 0.0044(10) -0.0029(11) C17 0.056(2) 0.0274(14) 0.058(2) -0.0014(13) 0.0163(17) -0.0082(14) C18 0.0253(17) 0.096(3) 0.0392(18) 0.0167(18) -0.0048(14) -0.0077(17) C19 0.0339(17) 0.0370(15) 0.0392(16) -0.0066(12) 0.0074(13) -0.0031(12) C20 0.0217(13) 0.0258(12) 0.0220(12) 0.0072(9) 0.0001(10) 0.0016(10) C21 0.0311(15) 0.0267(12) 0.0224(13) 0.0078(10) 0.0014(11) 0.0040(11) C22 0.0333(16) 0.0348(14) 0.0303(15) 0.0096(11) 0.0065(12) 0.0104(12) C23 0.0242(15) 0.0489(16) 0.0286(14) 0.0149(12) -0.0003(12) 0.0049(13) C24 0.0300(16) 0.0414(15) 0.0258(14) 0.0063(11) -0.0054(12) -0.0055(12) C25 0.0275(15) 0.0299(13) 0.0237(13) 0.0069(10) -0.0007(11) -0.0021(11) C26 0.0430(18) 0.0253(12) 0.0318(15) 0.0010(11) 0.0025(13) 0.0030(12) C27 0.0286(18) 0.078(2) 0.055(2) 0.0149(18) 0.0010(15) 0.0086(17) C28 0.0373(17) 0.0334(14) 0.0351(16) -0.0019(11) -0.0026(13) -0.0039(12) C29 0.0228(14) 0.0263(12) 0.0206(12) 0.0045(9) 0.0002(10) 0.0050(10) C30 0.0299(15) 0.0288(12) 0.0248(13) 0.0010(10) -0.0061(11) 0.0025(11) C31 0.0456(19) 0.0288(13) 0.0344(16) -0.0062(11) -0.0107(14) 0.0119(13) C32 0.0397(19) 0.0521(18) 0.0298(15) -0.0045(13) -0.0025(13) 0.0234(15) C33 0.0274(16) 0.0588(19) 0.0431(18) 0.0155(15) 0.0106(14) 0.0128(15) C34 0.0294(16) 0.0379(14) 0.0362(16) 0.0140(12) 0.0061(12) 0.0048(12) C35 0.0179(13) 0.0225(11) 0.0293(13) 0.0057(10) 0.0009(10) 0.0017(10) C36 0.0300(16) 0.0438(15) 0.0271(14) 0.0089(12) -0.0019(12) -0.0073(13) C37 0.0301(17) 0.0577(19) 0.0328(16) 0.0117(14) 0.0043(13) -0.0125(14) C38 0.0246(15) 0.0439(16) 0.0455(18) 0.0107(13) 0.0008(13) -0.0113(13) C39 0.0363(18) 0.0428(16) 0.0393(17) -0.0039(13) 0.0007(14) -0.0128(14) C40 0.0352(17) 0.0389(15) 0.0301(15) -0.0001(12) 0.0082(13) -0.0091(13) C41 0.0268(14) 0.0232(11) 0.0251(13) 0.0042(9) 0.0044(11) -0.0055(10) C42 0.0408(17) 0.0324(13) 0.0282(14) 0.0069(11) 0.0087(12) 0.0027(13) C43 0.053(2) 0.0338(14) 0.0358(16) -0.0047(12) 0.0165(15) -0.0051(14) C44 0.047(2) 0.0518(18) 0.0314(16) -0.0093(14) 0.0029(14) -0.0195(16) C45 0.0287(16) 0.061(2) 0.0362(16) -0.0007(14) -0.0065(13) -0.0104(15) C46 0.0241(15) 0.0364(14) 0.0322(15) -0.0008(11) 0.0001(12) -0.0047(12) C47 0.040(2) 0.117(4) 0.085(3) 0.002(3) 0.030(2) -0.010(2) C100 0.072(3) 0.104(3) 0.052(3) 0.002(2) 0.011(2) 0.010(3) C101 0.051(3) 0.143(5) 0.039(2) -0.018(3) -0.0021(18) -0.006(3) C102 0.139(5) 0.099(3) 0.063(3) -0.033(3) 0.062(4) -0.056(3) _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 C1 1.940(2) . ? Ru1 C5 2.031(3) . ? Ru1 C8 2.113(2) . ? Ru1 P1 2.3164(6) . ? Ru1 Cl1 2.4589(7) . ? P1 C29 1.830(2) . ? P1 C41 1.841(3) . ? P1 C35 1.848(2) . ? O1 C47 1.410(4) . ? O1 C7 1.415(4) . ? N1 C1 1.371(3) . ? N1 C2 1.377(4) . ? N1 C4 1.406(4) . ? N2 C1 1.365(3) . ? N2 C3 1.388(4) . ? N2 C6 1.452(4) . ? N3 C8 1.346(3) . ? N3 C20 1.435(3) . ? N3 C9 1.478(3) . ? N4 C8 1.349(3) . ? N4 C11 1.433(3) . ? N4 C10 1.480(3) . ? C2 C3 1.342(5) . ? C4 C5 1.328(4) . ? C6 C7 1.510(4) . ? C9 C10 1.506(4) . ? C11 C16 1.396(3) . ? C11 C12 1.397(4) . ? C12 C13 1.384(4) . ? C12 C17 1.512(4) . ? C13 C14 1.388(4) . ? C14 C15 1.380(4) . ? C14 C18 1.511(4) . ? C15 C16 1.392(4) . ? C16 C19 1.503(4) . ? C20 C21 1.393(3) . ? C20 C25 1.399(4) . ? C21 C22 1.395(4) . ? C21 C26 1.509(4) . ? C22 C23 1.388(4) . ? C23 C24 1.383(4) . ? C23 C27 1.506(4) . ? C24 C25 1.391(4) . ? C25 C28 1.502(4) . ? C29 C30 1.388(3) . ? C29 C34 1.394(4) . ? C30 C31 1.385(4) . ? C31 C32 1.375(4) . ? C32 C33 1.383(4) . ? C33 C34 1.386(4) . ? C35 C40 1.386(4) . ? C35 C36 1.389(4) . ? C36 C37 1.388(4) . ? C37 C38 1.372(4) . ? C38 C39 1.372(4) . ? C39 C40 1.389(4) . ? C41 C42 1.391(4) . ? C41 C46 1.394(4) . ? C42 C43 1.387(4) . ? C43 C44 1.384(5) . ? C44 C45 1.373(4) . ? C45 C46 1.385(4) . ? C100 C100 1.296(9) 2_455 ? C100 C101 1.329(6) . ? C101 C102 1.378(7) . ? C102 C102 1.463(11) 2_455 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru1 C5 75.68(11) . . ? C1 Ru1 C8 100.53(9) . . ? C5 Ru1 C8 91.88(9) . . ? C1 Ru1 P1 91.83(7) . . ? C5 Ru1 P1 90.55(7) . . ? C8 Ru1 P1 167.62(7) . . ? C1 Ru1 Cl1 128.68(8) . . ? C5 Ru1 Cl1 155.64(9) . . ? C8 Ru1 Cl1 84.15(6) . . ? P1 Ru1 Cl1 88.64(2) . . ? C29 P1 C41 103.30(11) . . ? C29 P1 C35 102.64(11) . . ? C41 P1 C35 101.63(11) . . ? C29 P1 Ru1 105.97(8) . . ? C41 P1 Ru1 118.18(8) . . ? C35 P1 Ru1 122.62(8) . . ? C47 O1 C7 112.9(3) . . ? C1 N1 C2 111.3(2) . . ? C1 N1 C4 113.2(2) . . ? C2 N1 C4 135.1(2) . . ? C1 N2 C3 109.9(2) . . ? C1 N2 C6 123.4(2) . . ? C3 N2 C6 126.7(2) . . ? C8 N3 C20 127.5(2) . . ? C8 N3 C9 114.3(2) . . ? C20 N3 C9 117.09(19) . . ? C8 N4 C11 128.6(2) . . ? C8 N4 C10 114.0(2) . . ? C11 N4 C10 117.2(2) . . ? N2 C1 N1 104.4(2) . . ? N2 C1 Ru1 135.73(19) . . ? N1 C1 Ru1 119.87(19) . . ? C3 C2 N1 106.4(3) . . ? C2 C3 N2 108.1(3) . . ? C5 C4 N1 111.6(2) . . ? C4 C5 Ru1 119.3(2) . . ? N2 C6 C7 113.2(2) . . ? O1 C7 C6 108.4(2) . . ? N3 C8 N4 106.3(2) . . ? N3 C8 Ru1 128.36(17) . . ? N4 C8 Ru1 124.57(17) . . ? N3 C9 C10 102.6(2) . . ? N4 C10 C9 102.8(2) . . ? C16 C11 C12 121.2(2) . . ? C16 C11 N4 119.3(2) . . ? C12 C11 N4 119.2(2) . . ? C13 C12 C11 118.2(3) . . ? C13 C12 C17 120.4(3) . . ? C11 C12 C17 121.5(3) . . ? C12 C13 C14 122.3(3) . . ? C15 C14 C13 117.9(3) . . ? C15 C14 C18 121.0(3) . . ? C13 C14 C18 121.1(3) . . ? C14 C15 C16 122.3(3) . . ? C15 C16 C11 118.1(2) . . ? C15 C16 C19 120.0(2) . . ? C11 C16 C19 121.9(2) . . ? C21 C20 C25 121.8(2) . . ? C21 C20 N3 118.3(2) . . ? C25 C20 N3 119.2(2) . . ? C20 C21 C22 118.0(2) . . ? C20 C21 C26 121.0(2) . . ? C22 C21 C26 120.9(2) . . ? C23 C22 C21 121.8(3) . . ? C24 C23 C22 118.3(3) . . ? C24 C23 C27 120.8(3) . . ? C22 C23 C27 120.9(3) . . ? C23 C24 C25 122.3(3) . . ? C24 C25 C20 117.7(2) . . ? C24 C25 C28 119.6(2) . . ? C20 C25 C28 122.7(2) . . ? C30 C29 C34 118.5(2) . . ? C30 C29 P1 124.1(2) . . ? C34 C29 P1 117.28(19) . . ? C31 C30 C29 120.8(3) . . ? C32 C31 C30 120.2(3) . . ? C31 C32 C33 120.0(3) . . ? C32 C33 C34 119.8(3) . . ? C33 C34 C29 120.7(3) . . ? C40 C35 C36 117.9(2) . . ? C40 C35 P1 119.63(19) . . ? C36 C35 P1 122.4(2) . . ? C37 C36 C35 121.0(3) . . ? C38 C37 C36 120.4(3) . . ? C39 C38 C37 119.1(3) . . ? C38 C39 C40 120.9(3) . . ? C35 C40 C39 120.6(3) . . ? C42 C41 C46 118.2(2) . . ? C42 C41 P1 119.3(2) . . ? C46 C41 P1 122.5(2) . . ? C43 C42 C41 120.5(3) . . ? C44 C43 C42 120.5(3) . . ? C45 C44 C43 119.5(3) . . ? C44 C45 C46 120.3(3) . . ? C45 C46 C41 120.9(3) . . ? C100 C100 C101 121.5(3) 2_455 . ? C100 C101 C102 122.1(5) . . ? C101 C102 C102 116.3(3) . 2_455 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.513 _refine_diff_density_min -0.506 _refine_diff_density_rms 0.075 _database_code_depnum_ccdc_archive 'CCDC 973561'