# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Datong Song' _publ_contact_author_email DSONG@CHEM.UTORONTO.CA _publ_section_title ; Coordination Promoted C-H Bond Oxidation by Air ; _publ_contact_author 'Datong Song' loop_ _publ_author_name 'Datong Song.' 'Huiling Jiang.' 'Elzbieta Stepowska' # Attachment 'CIF.txt' data_1 _database_code_depnum_ccdc_archive 'CCDC 695676' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H42 Cl6 N2 P2 Ru' _chemical_formula_weight 1034.56 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' _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 10.4092(3) _cell_length_b 25.9838(13) _cell_length_c 16.4249(7) _cell_angle_alpha 90.00 _cell_angle_beta 91.285(3) _cell_angle_gamma 90.00 _cell_volume 4441.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 26688 _cell_measurement_theta_min 2.93 _cell_measurement_theta_max 26.00 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2104 _exptl_absorpt_coefficient_mu 0.825 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.735 _exptl_absorpt_correction_T_max 0.994 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26688 _diffrn_reflns_av_R_equivalents 0.1056 _diffrn_reflns_av_sigmaI/netI 0.1153 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8656 _reflns_number_gt 5442 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0562P)^2^+12.5210P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8656 _refine_ls_number_parameters 541 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1184 _refine_ls_R_factor_gt 0.0605 _refine_ls_wR_factor_ref 0.1577 _refine_ls_wR_factor_gt 0.1304 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.002 _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 1.20558(4) 0.622213(18) 1.40277(3) 0.01705(14) Uani 1 1 d . . . Cl1 Cl 0.98173(12) 0.61511(5) 1.36470(9) 0.0228(3) Uani 1 1 d . . . Cl2 Cl 1.25182(13) 0.53707(5) 1.34394(9) 0.0216(3) Uani 1 1 d . . . Cl3 Cl 1.3545(3) 0.44293(12) 0.95458(17) 0.0906(9) Uani 1 1 d . . . Cl4 Cl 1.2986(2) 0.52316(10) 0.83839(14) 0.0719(7) Uani 1 1 d . . . Cl5 Cl 0.8672(3) 0.58395(11) 0.88568(15) 0.0821(8) Uani 1 1 d . . . Cl6 Cl 0.6359(3) 0.58015(12) 0.78947(19) 0.1051(11) Uani 1 1 d . . . P1 P 1.26032(13) 0.65184(6) 1.27235(9) 0.0190(3) Uani 1 1 d . . . P2 P 1.17084(13) 0.69620(6) 1.48040(9) 0.0186(3) Uani 1 1 d . . . N1 N 1.3978(4) 0.61442(17) 1.4557(3) 0.0180(10) Uani 1 1 d . . . N2 N 1.1604(4) 0.57552(17) 1.5056(3) 0.0193(11) Uani 1 1 d . . . C1 C 1.5180(5) 0.6317(2) 1.4449(4) 0.0197(13) Uani 1 1 d . . . H1A H 1.5306 0.6590 1.4073 0.024 Uiso 1 1 calc R . . C2 C 1.6247(5) 0.6116(2) 1.4861(4) 0.0229(14) Uani 1 1 d . . . H2A H 1.7075 0.6247 1.4744 0.027 Uiso 1 1 calc R . . C3 C 1.6137(5) 0.5728(2) 1.5444(4) 0.0227(14) Uani 1 1 d . . . H3A H 1.6867 0.5588 1.5723 0.027 Uiso 1 1 calc R . . C4 C 1.4897(5) 0.5557(2) 1.5592(4) 0.0223(13) Uani 1 1 d . . . C5 C 1.4319(5) 0.5176(2) 1.6190(4) 0.0231(14) Uani 1 1 d . . . H5A H 1.4533 0.5272 1.6760 0.028 Uiso 1 1 calc R . . H5B H 1.4625 0.4822 1.6089 0.028 Uiso 1 1 calc R . . C6 C 1.2872(5) 0.5225(2) 1.6009(4) 0.0225(13) Uani 1 1 d . . . C7 C 1.1767(5) 0.5025(2) 1.6349(4) 0.0250(14) Uani 1 1 d . . . H7A H 1.1806 0.4781 1.6779 0.030 Uiso 1 1 calc R . . C8 C 1.0588(5) 0.5205(2) 1.6024(4) 0.0233(14) Uani 1 1 d . . . H8A H 0.9810 0.5077 1.6237 0.028 Uiso 1 1 calc R . . C9 C 1.0530(5) 0.5564(2) 1.5401(4) 0.0215(13) Uani 1 1 d . . . H9A H 0.9713 0.5680 1.5209 0.026 Uiso 1 1 calc R . . C10 C 1.2698(5) 0.5572(2) 1.5383(3) 0.0193(13) Uani 1 1 d . . . C11 C 1.3912(5) 0.5775(2) 1.5131(4) 0.0185(13) Uani 1 1 d . . . C12 C 1.2164(6) 0.6094(2) 1.1847(4) 0.0249(14) Uani 1 1 d . . . C13 C 1.2954(6) 0.6036(2) 1.1183(4) 0.0281(15) Uani 1 1 d . . . H13A H 1.3777 0.6194 1.1193 0.034 Uiso 1 1 calc R . . C14 C 1.2568(6) 0.5752(2) 1.0502(4) 0.0315(16) Uani 1 1 d . . . H14A H 1.3134 0.5712 1.0060 0.038 Uiso 1 1 calc R . . C15 C 1.1374(6) 0.5529(2) 1.0467(4) 0.0329(16) Uani 1 1 d . . . H15A H 1.1105 0.5337 1.0001 0.039 Uiso 1 1 calc R . . C16 C 1.0563(6) 0.5587(3) 1.1120(4) 0.0329(16) Uani 1 1 d . . . H16A H 0.9733 0.5434 1.1102 0.039 Uiso 1 1 calc R . . C17 C 1.0961(6) 0.5866(2) 1.1798(4) 0.0265(14) Uani 1 1 d . . . H17A H 1.0396 0.5902 1.2241 0.032 Uiso 1 1 calc R . . C18 C 1.1934(5) 0.7119(2) 1.2293(4) 0.0209(13) Uani 1 1 d . . . C19 C 1.0880(6) 0.7335(2) 1.2666(4) 0.0258(14) Uani 1 1 d . . . H19A H 1.0525 0.7172 1.3127 0.031 Uiso 1 1 calc R . . C20 C 1.0338(6) 0.7789(3) 1.2366(4) 0.0307(15) Uani 1 1 d . . . H20A H 0.9618 0.7935 1.2625 0.037 Uiso 1 1 calc R . . C21 C 1.0839(6) 0.8027(2) 1.1697(4) 0.0306(15) Uani 1 1 d . . . H21A H 1.0496 0.8346 1.1512 0.037 Uiso 1 1 calc R . . C22 C 1.1847(5) 0.7800(2) 1.1294(4) 0.0281(15) Uani 1 1 d . . . H22A H 1.2166 0.7955 1.0815 0.034 Uiso 1 1 calc R . . C23 C 1.2395(5) 0.7346(2) 1.1587(4) 0.0233(14) Uani 1 1 d . . . H23A H 1.3083 0.7190 1.1307 0.028 Uiso 1 1 calc R . . C24 C 1.4342(5) 0.6585(2) 1.2578(3) 0.0180(13) Uani 1 1 d . . . C25 C 1.5094(6) 0.6135(2) 1.2606(4) 0.0268(14) Uani 1 1 d . . . H25A H 1.4691 0.5808 1.2644 0.032 Uiso 1 1 calc R . . C26 C 1.6427(6) 0.6169(3) 1.2579(4) 0.0314(16) Uani 1 1 d . . . H26A H 1.6926 0.5862 1.2586 0.038 Uiso 1 1 calc R . . C27 C 1.7033(6) 0.6637(3) 1.2543(4) 0.0315(16) Uani 1 1 d . . . H27A H 1.7944 0.6655 1.2532 0.038 Uiso 1 1 calc R . . C28 C 1.6305(6) 0.7085(3) 1.2522(4) 0.0284(15) Uani 1 1 d . . . H28A H 1.6717 0.7411 1.2502 0.034 Uiso 1 1 calc R . . C29 C 1.4967(5) 0.7055(2) 1.2530(4) 0.0213(13) Uani 1 1 d . . . H29A H 1.4474 0.7363 1.2501 0.026 Uiso 1 1 calc R . . C30 C 1.3048(5) 0.7412(2) 1.4935(4) 0.0192(13) Uani 1 1 d . . . C31 C 1.3275(6) 0.7686(2) 1.5653(4) 0.0275(15) Uani 1 1 d . . . H31A H 1.2777 0.7615 1.6118 0.033 Uiso 1 1 calc R . . C32 C 1.4230(6) 0.8063(3) 1.5694(4) 0.0327(16) Uani 1 1 d . . . H32A H 1.4362 0.8255 1.6181 0.039 Uiso 1 1 calc R . . C33 C 1.4978(6) 0.8159(2) 1.5032(4) 0.0301(15) Uani 1 1 d . . . H33A H 1.5645 0.8409 1.5065 0.036 Uiso 1 1 calc R . . C34 C 1.4755(5) 0.7890(2) 1.4319(4) 0.0257(14) Uani 1 1 d . . . H34A H 1.5253 0.7963 1.3856 0.031 Uiso 1 1 calc R . . C35 C 1.3803(5) 0.7513(2) 1.4274(4) 0.0236(14) Uani 1 1 d . . . H35A H 1.3674 0.7324 1.3783 0.028 Uiso 1 1 calc R . . C36 C 1.0381(5) 0.7426(2) 1.4611(3) 0.0201(13) Uani 1 1 d . . . C37 C 1.0599(6) 0.7955(2) 1.4571(4) 0.0304(16) Uani 1 1 d . . . H37A H 1.1446 0.8085 1.4646 0.036 Uiso 1 1 calc R . . C38 C 0.9594(6) 0.8291(2) 1.4422(4) 0.0305(15) Uani 1 1 d . . . H38A H 0.9759 0.8651 1.4400 0.037 Uiso 1 1 calc R . . C39 C 0.8368(6) 0.8117(3) 1.4305(4) 0.0320(16) Uani 1 1 d . . . H39A H 0.7685 0.8352 1.4200 0.038 Uiso 1 1 calc R . . C40 C 0.8130(6) 0.7593(3) 1.4341(4) 0.0312(16) Uani 1 1 d . . . H40A H 0.7278 0.7468 1.4263 0.037 Uiso 1 1 calc R . . C41 C 0.9124(5) 0.7251(2) 1.4490(4) 0.0261(14) Uani 1 1 d . . . H41A H 0.8950 0.6892 1.4511 0.031 Uiso 1 1 calc R . . C42 C 1.1428(5) 0.6777(2) 1.5878(4) 0.0208(13) Uani 1 1 d . . . C43 C 1.2463(5) 0.6596(2) 1.6340(4) 0.0237(14) Uani 1 1 d . . . H43A H 1.3299 0.6603 1.6119 0.028 Uiso 1 1 calc R . . C44 C 1.2302(6) 0.6407(3) 1.7117(4) 0.0311(15) Uani 1 1 d . . . H44A H 1.3027 0.6293 1.7430 0.037 Uiso 1 1 calc R . . C45 C 1.1079(6) 0.6381(2) 1.7441(4) 0.0319(16) Uani 1 1 d . . . H45A H 1.0955 0.6235 1.7964 0.038 Uiso 1 1 calc R . . C46 C 1.0052(6) 0.6571(2) 1.6991(4) 0.0323(16) Uani 1 1 d . . . H46A H 0.9218 0.6568 1.7216 0.039 Uiso 1 1 calc R . . C47 C 1.0216(5) 0.6765(2) 1.6218(4) 0.0243(14) Uani 1 1 d . . . H47A H 0.9495 0.6892 1.5916 0.029 Uiso 1 1 calc R . . C48 C 1.4315(11) 0.4923(5) 0.8848(6) 0.119(6) Uani 1 1 d . . . H48A H 1.4851 0.5170 0.9164 0.143 Uiso 1 1 calc R . . H48B H 1.4852 0.4752 0.8437 0.143 Uiso 1 1 calc R . . C49 C 0.7756(10) 0.5496(4) 0.8139(6) 0.075(3) Uani 1 1 d . . . H49A H 0.8261 0.5449 0.7641 0.090 Uiso 1 1 calc R . . H49B H 0.7562 0.5151 0.8359 0.090 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 0.0154(2) 0.0149(2) 0.0209(3) 0.0010(2) 0.00101(17) -0.00018(19) Cl1 0.0174(7) 0.0220(8) 0.0287(8) -0.0001(7) -0.0017(6) 0.0001(6) Cl2 0.0231(7) 0.0158(7) 0.0260(8) -0.0020(6) 0.0022(6) 0.0008(6) Cl3 0.113(2) 0.093(2) 0.0658(18) 0.0092(16) 0.0001(15) 0.0303(17) Cl4 0.0840(16) 0.0840(18) 0.0476(14) -0.0022(12) -0.0051(11) 0.0200(13) Cl5 0.0990(19) 0.0875(19) 0.0599(16) -0.0134(14) 0.0026(13) -0.0458(15) Cl6 0.121(2) 0.099(2) 0.093(2) -0.0259(18) -0.0438(18) 0.0577(19) P1 0.0186(7) 0.0175(8) 0.0210(9) 0.0021(7) 0.0004(6) 0.0010(6) P2 0.0171(7) 0.0165(8) 0.0222(9) -0.0006(7) 0.0017(6) -0.0018(6) N1 0.023(3) 0.012(3) 0.019(3) 0.000(2) 0.0015(19) 0.002(2) N2 0.024(3) 0.014(3) 0.020(3) 0.002(2) 0.003(2) 0.000(2) C1 0.018(3) 0.014(3) 0.027(3) 0.002(3) 0.002(2) -0.004(2) C2 0.019(3) 0.020(3) 0.029(4) -0.006(3) 0.002(2) -0.002(2) C3 0.020(3) 0.027(4) 0.021(3) -0.003(3) -0.003(2) 0.005(3) C4 0.023(3) 0.023(3) 0.020(3) -0.002(3) -0.004(2) 0.002(3) C5 0.027(3) 0.016(3) 0.026(4) 0.004(3) -0.001(3) 0.000(2) C6 0.026(3) 0.017(3) 0.024(3) -0.007(3) 0.000(2) 0.002(3) C7 0.034(4) 0.015(3) 0.026(4) 0.001(3) 0.002(3) -0.007(3) C8 0.025(3) 0.019(3) 0.025(4) -0.001(3) 0.002(3) -0.006(3) C9 0.019(3) 0.017(3) 0.029(4) -0.004(3) 0.003(2) 0.000(2) C10 0.020(3) 0.018(3) 0.020(3) 0.003(3) 0.000(2) 0.004(2) C11 0.022(3) 0.013(3) 0.021(3) -0.002(3) 0.001(2) 0.001(2) C12 0.028(3) 0.018(3) 0.029(4) -0.001(3) 0.000(3) 0.004(3) C13 0.031(3) 0.026(3) 0.027(4) -0.005(3) -0.002(3) 0.001(3) C14 0.041(4) 0.029(4) 0.025(4) -0.003(3) 0.004(3) 0.004(3) C15 0.049(4) 0.024(4) 0.025(4) -0.003(3) -0.003(3) 0.002(3) C16 0.034(4) 0.033(4) 0.031(4) -0.003(3) -0.001(3) -0.005(3) C17 0.031(3) 0.023(3) 0.026(4) 0.001(3) 0.001(3) 0.001(3) C18 0.020(3) 0.018(3) 0.023(4) -0.004(3) -0.007(2) -0.004(2) C19 0.027(3) 0.026(4) 0.025(4) 0.003(3) 0.003(3) 0.004(3) C20 0.031(4) 0.033(4) 0.028(4) 0.000(3) 0.007(3) 0.010(3) C21 0.033(4) 0.022(4) 0.037(4) 0.010(3) 0.000(3) 0.002(3) C22 0.020(3) 0.034(4) 0.031(4) 0.012(3) 0.002(3) -0.002(3) C23 0.018(3) 0.029(4) 0.023(4) 0.007(3) 0.001(2) 0.005(3) C24 0.023(3) 0.018(3) 0.014(3) -0.002(2) 0.000(2) 0.001(2) C25 0.032(3) 0.024(4) 0.024(4) 0.008(3) 0.004(3) 0.000(3) C26 0.027(3) 0.036(4) 0.032(4) 0.002(3) 0.005(3) 0.011(3) C27 0.020(3) 0.050(5) 0.025(4) 0.005(3) 0.002(3) -0.002(3) C28 0.027(3) 0.030(4) 0.028(4) 0.007(3) 0.004(3) -0.006(3) C29 0.023(3) 0.020(3) 0.021(3) -0.001(3) 0.002(2) 0.006(2) C30 0.019(3) 0.015(3) 0.024(3) 0.004(3) 0.002(2) 0.005(2) C31 0.029(3) 0.029(4) 0.025(4) -0.003(3) 0.004(3) -0.007(3) C32 0.038(4) 0.029(4) 0.031(4) -0.008(3) -0.003(3) -0.009(3) C33 0.024(3) 0.024(4) 0.042(4) -0.002(3) 0.000(3) -0.009(3) C34 0.024(3) 0.023(3) 0.030(4) 0.005(3) 0.010(3) 0.004(3) C35 0.027(3) 0.017(3) 0.027(4) -0.006(3) 0.001(3) -0.001(3) C36 0.020(3) 0.021(3) 0.019(3) 0.001(3) 0.003(2) 0.002(2) C37 0.023(3) 0.027(4) 0.042(4) -0.002(3) 0.006(3) 0.000(3) C38 0.034(4) 0.020(3) 0.038(4) 0.000(3) 0.005(3) 0.010(3) C39 0.028(4) 0.035(4) 0.033(4) -0.002(3) 0.000(3) 0.014(3) C40 0.020(3) 0.040(4) 0.034(4) -0.006(3) -0.003(3) 0.006(3) C41 0.025(3) 0.022(3) 0.031(4) -0.003(3) 0.004(3) 0.000(3) C42 0.024(3) 0.014(3) 0.025(4) -0.006(3) 0.006(2) 0.001(2) C43 0.022(3) 0.022(3) 0.027(4) -0.007(3) 0.002(3) 0.000(3) C44 0.042(4) 0.031(4) 0.020(4) -0.003(3) -0.004(3) 0.005(3) C45 0.053(4) 0.026(4) 0.017(4) 0.002(3) 0.005(3) -0.004(3) C46 0.036(4) 0.024(4) 0.038(4) -0.003(3) 0.016(3) -0.003(3) C47 0.024(3) 0.024(3) 0.025(4) -0.004(3) 0.008(3) 0.001(3) C48 0.156(11) 0.151(11) 0.047(6) -0.054(7) -0.055(7) 0.125(9) C49 0.104(8) 0.054(6) 0.066(7) -0.018(5) -0.029(6) 0.007(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N2 2.140(5) . ? Ru1 N1 2.173(4) . ? Ru1 P2 2.3394(16) . ? Ru1 P1 2.3582(16) . ? Ru1 Cl1 2.4061(14) . ? Ru1 Cl2 2.4660(15) . ? Cl3 C48 1.908(15) . ? Cl4 C48 1.759(8) . ? Cl5 C49 1.745(9) . ? Cl6 C49 1.697(9) . ? P1 C24 1.839(6) . ? P1 C18 1.844(6) . ? P1 C12 1.862(6) . ? P2 C30 1.829(6) . ? P2 C36 1.856(6) . ? P2 C42 1.858(6) . ? N1 C1 1.345(7) . ? N1 C11 1.347(7) . ? N2 C10 1.336(7) . ? N2 C9 1.359(7) . ? C1 C2 1.390(8) . ? C2 C3 1.398(8) . ? C3 C4 1.391(8) . ? C4 C11 1.383(8) . ? C4 C5 1.526(8) . ? C5 C6 1.534(8) . ? C6 C10 1.376(8) . ? C6 C7 1.391(8) . ? C7 C8 1.408(8) . ? C8 C9 1.383(8) . ? C10 C11 1.438(8) . ? C12 C17 1.386(8) . ? C12 C13 1.390(8) . ? C13 C14 1.391(9) . ? C14 C15 1.371(9) . ? C15 C16 1.388(9) . ? C16 C17 1.386(9) . ? C18 C19 1.387(8) . ? C18 C23 1.395(8) . ? C19 C20 1.393(9) . ? C20 C21 1.373(9) . ? C21 C22 1.385(9) . ? C22 C23 1.392(8) . ? C24 C29 1.387(8) . ? C24 C25 1.407(8) . ? C25 C26 1.393(8) . ? C26 C27 1.372(9) . ? C27 C28 1.389(9) . ? C28 C29 1.395(8) . ? C30 C35 1.380(8) . ? C30 C31 1.394(8) . ? C31 C32 1.397(8) . ? C32 C33 1.374(9) . ? C33 C34 1.378(9) . ? C34 C35 1.394(8) . ? C36 C41 1.395(8) . ? C36 C37 1.396(8) . ? C37 C38 1.380(8) . ? C38 C39 1.364(9) . ? C39 C40 1.384(9) . ? C40 C41 1.383(8) . ? C42 C43 1.386(8) . ? C42 C47 1.391(8) . ? C43 C44 1.381(9) . ? C44 C45 1.393(9) . ? C45 C46 1.377(9) . ? C46 C47 1.380(9) . ? 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 N2 Ru1 N1 81.26(17) . . ? N2 Ru1 P2 89.79(13) . . ? N1 Ru1 P2 90.62(12) . . ? N2 Ru1 P1 164.51(13) . . ? N1 Ru1 P1 98.91(13) . . ? P2 Ru1 P1 105.68(6) . . ? N2 Ru1 Cl1 86.16(13) . . ? N1 Ru1 Cl1 167.02(13) . . ? P2 Ru1 Cl1 92.52(5) . . ? P1 Ru1 Cl1 92.36(5) . . ? N2 Ru1 Cl2 81.31(13) . . ? N1 Ru1 Cl2 83.52(12) . . ? P2 Ru1 Cl2 169.98(6) . . ? P1 Ru1 Cl2 83.32(5) . . ? Cl1 Ru1 Cl2 91.47(5) . . ? C24 P1 C18 103.6(3) . . ? C24 P1 C12 100.4(3) . . ? C18 P1 C12 97.0(3) . . ? C24 P1 Ru1 114.02(19) . . ? C18 P1 Ru1 121.8(2) . . ? C12 P1 Ru1 116.7(2) . . ? C30 P2 C36 99.7(3) . . ? C30 P2 C42 100.9(3) . . ? C36 P2 C42 101.4(3) . . ? C30 P2 Ru1 117.56(19) . . ? C36 P2 Ru1 124.35(19) . . ? C42 P2 Ru1 109.52(19) . . ? C1 N1 C11 113.1(5) . . ? C1 N1 Ru1 140.1(4) . . ? C11 N1 Ru1 106.6(3) . . ? C10 N2 C9 113.8(5) . . ? C10 N2 Ru1 108.6(4) . . ? C9 N2 Ru1 137.2(4) . . ? N1 C1 C2 123.1(5) . . ? C1 C2 C3 121.9(5) . . ? C4 C3 C2 116.1(5) . . ? C11 C4 C3 116.9(6) . . ? C11 C4 C5 108.7(5) . . ? C3 C4 C5 134.4(5) . . ? C4 C5 C6 102.8(5) . . ? C10 C6 C7 116.7(5) . . ? C10 C6 C5 108.1(5) . . ? C7 C6 C5 135.1(6) . . ? C6 C7 C8 116.4(6) . . ? C9 C8 C7 121.8(5) . . ? N2 C9 C8 122.2(5) . . ? N2 C10 C6 129.1(5) . . ? N2 C10 C11 120.0(5) . . ? C6 C10 C11 110.7(5) . . ? N1 C11 C4 128.8(5) . . ? N1 C11 C10 121.4(5) . . ? C4 C11 C10 109.7(5) . . ? C17 C12 C13 117.2(6) . . ? C17 C12 P1 120.2(5) . . ? C13 C12 P1 122.2(5) . . ? C12 C13 C14 121.6(6) . . ? C15 C14 C13 120.2(6) . . ? C14 C15 C16 119.2(6) . . ? C17 C16 C15 120.2(6) . . ? C16 C17 C12 121.6(6) . . ? C19 C18 C23 119.1(5) . . ? C19 C18 P1 118.0(5) . . ? C23 C18 P1 122.8(4) . . ? C18 C19 C20 120.3(6) . . ? C21 C20 C19 120.4(6) . . ? C20 C21 C22 119.8(6) . . ? C21 C22 C23 120.2(6) . . ? C22 C23 C18 120.0(6) . . ? C29 C24 C25 118.2(5) . . ? C29 C24 P1 123.7(4) . . ? C25 C24 P1 117.7(4) . . ? C26 C25 C24 120.1(6) . . ? C27 C26 C25 121.0(6) . . ? C26 C27 C28 119.5(6) . . ? C27 C28 C29 119.9(6) . . ? C24 C29 C28 121.2(5) . . ? C35 C30 C31 118.7(5) . . ? C35 C30 P2 118.4(5) . . ? C31 C30 P2 122.7(4) . . ? C30 C31 C32 120.3(6) . . ? C33 C32 C31 120.3(6) . . ? C32 C33 C34 119.5(6) . . ? C33 C34 C35 120.6(6) . . ? C30 C35 C34 120.5(6) . . ? C41 C36 C37 117.9(5) . . ? C41 C36 P2 120.3(4) . . ? C37 C36 P2 121.8(4) . . ? C38 C37 C36 120.6(6) . . ? C39 C38 C37 121.1(6) . . ? C38 C39 C40 119.3(6) . . ? C41 C40 C39 120.4(6) . . ? C40 C41 C36 120.8(6) . . ? C43 C42 C47 118.2(6) . . ? C43 C42 P2 118.1(4) . . ? C47 C42 P2 123.4(5) . . ? C44 C43 C42 121.2(6) . . ? C43 C44 C45 120.1(6) . . ? C46 C45 C44 118.9(6) . . ? C45 C46 C47 120.9(6) . . ? C46 C47 C42 120.7(6) . . ? Cl4 C48 Cl3 103.3(7) . . ? Cl6 C49 Cl5 111.9(5) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.603 _refine_diff_density_min -1.147 _refine_diff_density_rms 0.126 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 695677' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H38 Cl4 N2 O P2 Ru' _chemical_formula_weight 963.61 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)/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 14.1185(5) _cell_length_b 10.4850(4) _cell_length_c 29.4109(10) _cell_angle_alpha 90.00 _cell_angle_beta 103.404(2) _cell_angle_gamma 90.00 _cell_volume 4235.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 19828 _cell_measurement_theta_min 2.97 _cell_measurement_theta_max 25.00 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.511 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1960 _exptl_absorpt_coefficient_mu 0.739 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8544 _exptl_absorpt_correction_T_max 0.9640 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19828 _diffrn_reflns_av_R_equivalents 0.0868 _diffrn_reflns_av_sigmaI/netI 0.0898 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7337 _reflns_number_gt 4732 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1208P)^2^+0.8408P] 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 7337 _refine_ls_number_parameters 541 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1091 _refine_ls_R_factor_gt 0.0652 _refine_ls_wR_factor_ref 0.2085 _refine_ls_wR_factor_gt 0.1740 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.44909(4) 0.13916(5) 0.114747(16) 0.0403(2) Uani 1 1 d . . . Cl1 Cl 0.40593(12) 0.35873(14) 0.12710(6) 0.0495(4) Uani 1 1 d . . . Cl2 Cl 0.42443(12) 0.15813(15) 0.03063(5) 0.0467(4) Uani 1 1 d . . . P1 P 0.61412(12) 0.21531(15) 0.13071(5) 0.0400(4) Uani 1 1 d . . . P2 P 0.28430(12) 0.06972(16) 0.10344(6) 0.0447(4) Uani 1 1 d . . . O1 O 0.5600(4) -0.3317(5) 0.24097(18) 0.0672(14) Uani 1 1 d . . . N1 N 0.4732(4) 0.0916(5) 0.18582(17) 0.0429(12) Uani 1 1 d . . . N2 N 0.4883(4) -0.0514(5) 0.10889(17) 0.0422(12) Uani 1 1 d . . . C1 C 0.4668(5) 0.1492(6) 0.2264(2) 0.0501(17) Uani 1 1 d . . . H1A H 0.4463 0.2357 0.2257 0.060 Uiso 1 1 calc R . . C2 C 0.4894(5) 0.0847(8) 0.2692(2) 0.0561(17) Uani 1 1 d . . . H2A H 0.4867 0.1298 0.2969 0.067 Uiso 1 1 calc R . . C3 C 0.5158(5) -0.0440(8) 0.2725(2) 0.060(2) Uani 1 1 d . . . H3A H 0.5288 -0.0885 0.3015 0.072 Uiso 1 1 calc R . . C4 C 0.5218(5) -0.1030(7) 0.2312(2) 0.0535(17) Uani 1 1 d . . . C5 C 0.5444(5) -0.2385(7) 0.2166(3) 0.0562(18) Uani 1 1 d . . . C6 C 0.5347(5) -0.2303(6) 0.1633(2) 0.0520(17) Uani 1 1 d . . . C7 C 0.5358(5) -0.3134(7) 0.1275(3) 0.0570(18) Uani 1 1 d . . . H7A H 0.5515 -0.4011 0.1330 0.068 Uiso 1 1 calc R . . C8 C 0.5129(5) -0.2627(6) 0.0827(3) 0.0531(17) Uani 1 1 d . . . H8A H 0.5129 -0.3174 0.0569 0.064 Uiso 1 1 calc R . . C9 C 0.4897(5) -0.1339(6) 0.0741(2) 0.0442(15) Uani 1 1 d . . . H9A H 0.4746 -0.1038 0.0428 0.053 Uiso 1 1 calc R . . C10 C 0.5096(5) -0.1048(6) 0.1516(2) 0.0463(16) Uani 1 1 d . . . C11 C 0.5020(4) -0.0306(6) 0.1914(2) 0.0438(15) Uani 1 1 d . . . C12 C 0.6475(5) 0.3624(5) 0.1049(2) 0.0425(15) Uani 1 1 d . . . C13 C 0.7280(5) 0.4348(6) 0.1265(2) 0.0482(16) Uani 1 1 d . . . H13A H 0.7635 0.4120 0.1570 0.058 Uiso 1 1 calc R . . C14 C 0.7574(5) 0.5385(6) 0.1046(2) 0.0531(17) Uani 1 1 d . . . H14A H 0.8118 0.5875 0.1203 0.064 Uiso 1 1 calc R . . C15 C 0.7078(5) 0.5720(6) 0.0596(2) 0.0498(16) Uani 1 1 d . . . H15A H 0.7281 0.6436 0.0445 0.060 Uiso 1 1 calc R . . C16 C 0.6292(5) 0.5009(6) 0.0374(2) 0.0536(17) Uani 1 1 d . . . H16A H 0.5959 0.5230 0.0065 0.064 Uiso 1 1 calc R . . C17 C 0.5971(5) 0.3967(6) 0.0592(2) 0.0472(16) Uani 1 1 d . . . H17A H 0.5419 0.3491 0.0434 0.057 Uiso 1 1 calc R . . C18 C 0.7108(5) 0.1118(6) 0.1183(2) 0.0433(15) Uani 1 1 d . . . C19 C 0.6872(5) 0.0291(6) 0.0802(2) 0.0419(15) Uani 1 1 d . . . H19A H 0.6222 0.0261 0.0619 0.050 Uiso 1 1 calc R . . C20 C 0.7580(5) -0.0492(6) 0.0684(2) 0.0525(17) Uani 1 1 d . . . H20A H 0.7402 -0.1082 0.0434 0.063 Uiso 1 1 calc R . . C21 C 0.8548(5) -0.0409(7) 0.0934(2) 0.0550(17) Uani 1 1 d . . . H21A H 0.9031 -0.0937 0.0853 0.066 Uiso 1 1 calc R . . C22 C 0.8801(5) 0.0462(7) 0.1307(2) 0.0526(17) Uani 1 1 d . . . H22A H 0.9460 0.0540 0.1474 0.063 Uiso 1 1 calc R . . C23 C 0.8084(5) 0.1211(6) 0.1428(2) 0.0490(16) Uani 1 1 d . . . H23A H 0.8258 0.1793 0.1681 0.059 Uiso 1 1 calc R . . C24 C 0.6541(4) 0.2463(5) 0.1940(2) 0.0416(14) Uani 1 1 d . . . C25 C 0.6262(5) 0.3601(6) 0.2125(2) 0.0450(16) Uani 1 1 d . . . H25A H 0.5932 0.4245 0.1921 0.054 Uiso 1 1 calc R . . C26 C 0.6472(5) 0.3786(6) 0.2608(2) 0.0475(16) Uani 1 1 d . . . H26A H 0.6277 0.4553 0.2733 0.057 Uiso 1 1 calc R . . C27 C 0.6958(5) 0.2866(6) 0.2905(2) 0.0516(17) Uani 1 1 d . . . H27A H 0.7119 0.3011 0.3233 0.062 Uiso 1 1 calc R . . C28 C 0.7212(5) 0.1728(7) 0.2727(2) 0.0488(16) Uani 1 1 d . . . H28A H 0.7532 0.1080 0.2932 0.059 Uiso 1 1 calc R . . C29 C 0.6999(5) 0.1540(6) 0.2251(2) 0.0454(15) Uani 1 1 d . . . H29A H 0.7171 0.0753 0.2132 0.055 Uiso 1 1 calc R . . C30 C 0.2324(4) 0.0706(7) 0.1549(2) 0.0530(17) Uani 1 1 d . . . C31 C 0.2463(5) 0.1827(8) 0.1832(3) 0.064(2) Uani 1 1 d . . . H31A H 0.2841 0.2510 0.1757 0.076 Uiso 1 1 calc R . . C32 C 0.2052(6) 0.1934(11) 0.2216(3) 0.086(3) Uani 1 1 d . . . H32A H 0.2146 0.2687 0.2401 0.103 Uiso 1 1 calc R . . C33 C 0.1499(7) 0.0922(12) 0.2328(3) 0.094(3) Uani 1 1 d . . . H33A H 0.1242 0.0981 0.2599 0.113 Uiso 1 1 calc R . . C34 C 0.1326(6) -0.0130(10) 0.2060(3) 0.080(3) Uani 1 1 d . . . H34A H 0.0930 -0.0792 0.2136 0.096 Uiso 1 1 calc R . . C35 C 0.1735(5) -0.0253(8) 0.1665(3) 0.068(2) Uani 1 1 d . . . H35A H 0.1606 -0.0997 0.1476 0.082 Uiso 1 1 calc R . . C36 C 0.1867(5) 0.1507(6) 0.0615(2) 0.0492(16) Uani 1 1 d . . . C37 C 0.0913(6) 0.1013(8) 0.0536(3) 0.076(2) Uani 1 1 d . . . H37A H 0.0796 0.0243 0.0685 0.091 Uiso 1 1 calc R . . C38 C 0.0154(6) 0.1637(8) 0.0247(3) 0.081(3) Uani 1 1 d . . . H38A H -0.0485 0.1295 0.0198 0.097 Uiso 1 1 calc R . . C39 C 0.0301(5) 0.2747(8) 0.0027(3) 0.069(2) Uani 1 1 d . . . H39A H -0.0230 0.3167 -0.0174 0.083 Uiso 1 1 calc R . . C40 C 0.1225(5) 0.3249(7) 0.0101(2) 0.0560(18) Uani 1 1 d . . . H40A H 0.1331 0.4024 -0.0047 0.067 Uiso 1 1 calc R . . C41 C 0.1998(5) 0.2626(6) 0.0391(2) 0.0504(16) Uani 1 1 d . . . H41A H 0.2633 0.2978 0.0437 0.060 Uiso 1 1 calc R . . C42 C 0.2701(5) -0.0966(6) 0.0826(2) 0.0506(17) Uani 1 1 d . . . C43 C 0.2471(5) -0.1222(7) 0.0350(2) 0.0533(18) Uani 1 1 d . . . H43A H 0.2320 -0.0539 0.0133 0.064 Uiso 1 1 calc R . . C44 C 0.2461(5) -0.2452(8) 0.0192(3) 0.067(2) Uani 1 1 d . . . H44A H 0.2284 -0.2613 -0.0135 0.081 Uiso 1 1 calc R . . C45 C 0.2702(6) -0.3460(8) 0.0498(4) 0.076(2) Uani 1 1 d . . . H45A H 0.2714 -0.4306 0.0384 0.092 Uiso 1 1 calc R . . C46 C 0.2927(6) -0.3213(7) 0.0977(4) 0.075(2) Uani 1 1 d . . . H46A H 0.3068 -0.3903 0.1192 0.090 Uiso 1 1 calc R . . C47 C 0.2949(5) -0.1991(7) 0.1143(3) 0.0576(18) Uani 1 1 d . . . H47A H 0.3131 -0.1832 0.1469 0.069 Uiso 1 1 calc R . . Cl3 Cl 1.1861(3) 0.5114(4) 0.17450(13) 0.1410(12) Uani 1 1 d . . . Cl4 Cl 1.0039(5) 0.4992(9) 0.10398(17) 0.095(2) Uani 0.40 1 d P . . C48 C 1.1150(9) 0.4616(12) 0.1201(4) 0.124(4) Uani 1 1 d . . . Cl4A Cl 1.0417(6) 0.6248(12) 0.1116(2) 0.096(3) Uani 0.30 1 d P . . Cl4B Cl 1.0104(8) 0.3628(12) 0.1125(3) 0.124(4) Uani 0.30 1 d P . . 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 0.0405(3) 0.0408(3) 0.0358(3) -0.0002(2) 0.0010(2) 0.0015(2) Cl1 0.0503(10) 0.0443(9) 0.0486(9) -0.0034(7) 0.0008(8) 0.0048(7) Cl2 0.0486(10) 0.0504(9) 0.0367(8) 0.0008(7) 0.0008(7) 0.0004(7) P1 0.0403(9) 0.0410(9) 0.0341(8) -0.0007(7) -0.0008(7) 0.0006(7) P2 0.0399(9) 0.0471(9) 0.0432(9) -0.0003(8) 0.0019(7) 0.0003(8) O1 0.059(3) 0.065(3) 0.076(4) 0.029(3) 0.013(3) 0.003(3) N1 0.040(3) 0.049(3) 0.036(3) -0.001(2) 0.001(2) 0.001(2) N2 0.036(3) 0.041(3) 0.047(3) -0.001(2) 0.004(2) 0.004(2) C1 0.041(4) 0.055(4) 0.051(4) -0.001(3) 0.006(3) -0.004(3) C2 0.054(4) 0.073(5) 0.040(4) -0.004(4) 0.009(3) -0.004(4) C3 0.050(4) 0.088(6) 0.042(4) 0.016(4) 0.009(3) -0.004(4) C4 0.044(4) 0.064(4) 0.049(4) 0.011(3) 0.003(3) -0.001(3) C5 0.038(4) 0.064(5) 0.064(5) 0.015(4) 0.004(3) -0.001(3) C6 0.047(4) 0.050(4) 0.055(4) 0.008(3) 0.004(3) 0.003(3) C7 0.049(4) 0.045(4) 0.076(5) 0.008(4) 0.012(4) 0.010(3) C8 0.050(4) 0.042(4) 0.068(5) -0.009(3) 0.015(4) 0.000(3) C9 0.040(4) 0.052(4) 0.039(3) 0.000(3) 0.008(3) 0.000(3) C10 0.044(4) 0.046(4) 0.044(4) 0.004(3) -0.001(3) 0.001(3) C11 0.042(4) 0.049(4) 0.035(3) 0.002(3) -0.002(3) -0.002(3) C12 0.046(4) 0.042(3) 0.037(3) -0.002(3) 0.003(3) -0.001(3) C13 0.047(4) 0.048(4) 0.047(4) -0.002(3) 0.005(3) 0.002(3) C14 0.051(4) 0.048(4) 0.060(4) -0.001(3) 0.014(4) -0.009(3) C15 0.056(4) 0.041(4) 0.057(4) 0.005(3) 0.024(4) 0.001(3) C16 0.066(5) 0.048(4) 0.044(4) 0.006(3) 0.007(3) 0.007(4) C17 0.051(4) 0.043(4) 0.044(4) 0.000(3) 0.004(3) 0.002(3) C18 0.042(4) 0.049(4) 0.036(3) 0.006(3) 0.003(3) -0.001(3) C19 0.043(4) 0.043(3) 0.037(3) 0.007(3) 0.003(3) 0.001(3) C20 0.060(5) 0.048(4) 0.049(4) 0.004(3) 0.012(3) 0.000(3) C21 0.050(4) 0.057(4) 0.056(4) 0.004(3) 0.009(3) 0.009(3) C22 0.037(4) 0.064(4) 0.050(4) 0.000(3) -0.004(3) 0.005(3) C23 0.053(4) 0.049(4) 0.040(4) 0.000(3) 0.001(3) -0.003(3) C24 0.042(4) 0.041(3) 0.040(3) -0.002(3) 0.006(3) -0.005(3) C25 0.047(4) 0.046(4) 0.038(3) 0.004(3) 0.002(3) -0.004(3) C26 0.052(4) 0.047(4) 0.041(4) -0.008(3) 0.006(3) -0.005(3) C27 0.061(4) 0.054(4) 0.036(3) 0.003(3) 0.004(3) -0.006(3) C28 0.045(4) 0.063(4) 0.034(3) 0.007(3) 0.001(3) 0.007(3) C29 0.045(4) 0.045(4) 0.045(4) 0.001(3) 0.007(3) 0.002(3) C30 0.032(3) 0.075(5) 0.048(4) 0.010(4) 0.003(3) 0.000(3) C31 0.045(4) 0.085(5) 0.056(5) -0.008(4) 0.004(4) 0.002(4) C32 0.064(6) 0.137(8) 0.058(5) -0.024(5) 0.015(4) 0.014(6) C33 0.064(6) 0.152(10) 0.070(6) 0.008(7) 0.020(5) 0.027(7) C34 0.066(6) 0.110(7) 0.068(6) 0.018(5) 0.025(5) 0.009(5) C35 0.049(4) 0.082(6) 0.068(5) 0.014(4) 0.006(4) 0.010(4) C36 0.048(4) 0.049(4) 0.046(4) 0.003(3) 0.001(3) 0.002(3) C37 0.055(5) 0.060(5) 0.100(7) 0.020(5) -0.005(5) -0.006(4) C38 0.041(4) 0.080(6) 0.106(7) 0.024(5) -0.013(4) -0.010(4) C39 0.040(4) 0.076(5) 0.083(6) 0.017(4) -0.004(4) 0.009(4) C40 0.060(5) 0.052(4) 0.055(4) 0.015(3) 0.010(4) 0.008(4) C41 0.045(4) 0.055(4) 0.049(4) -0.005(3) 0.006(3) 0.002(3) C42 0.040(4) 0.051(4) 0.060(4) -0.001(3) 0.009(3) -0.005(3) C43 0.049(4) 0.060(4) 0.047(4) -0.011(3) 0.005(3) -0.007(3) C44 0.051(5) 0.072(6) 0.077(5) -0.019(5) 0.010(4) -0.014(4) C45 0.060(5) 0.060(5) 0.113(8) -0.021(5) 0.026(5) -0.014(4) C46 0.059(5) 0.044(4) 0.121(8) 0.013(5) 0.020(5) 0.009(4) C47 0.047(4) 0.055(4) 0.067(5) 0.008(4) 0.006(4) 0.003(3) Cl3 0.131(3) 0.151(3) 0.153(3) -0.024(2) 0.058(2) 0.003(2) Cl4 0.093(4) 0.146(6) 0.041(3) 0.014(4) 0.008(3) 0.071(5) C48 0.142(11) 0.134(10) 0.093(8) -0.026(7) 0.025(7) -0.039(8) Cl4A 0.062(5) 0.183(10) 0.041(4) 0.034(5) 0.010(3) -0.009(5) Cl4B 0.131(8) 0.186(11) 0.076(5) -0.078(7) 0.066(6) -0.056(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N2 2.091(5) . ? Ru1 N1 2.098(5) . ? Ru1 P2 2.3864(17) . ? Ru1 P1 2.4041(17) . ? Ru1 Cl2 2.4252(16) . ? Ru1 Cl1 2.4303(16) . ? P1 C12 1.828(6) . ? P1 C24 1.844(6) . ? P1 C18 1.846(7) . ? P2 C30 1.828(7) . ? P2 C36 1.831(7) . ? P2 C42 1.844(7) . ? O1 C5 1.202(8) . ? N1 C11 1.343(8) . ? N1 C1 1.359(8) . ? N2 C9 1.344(8) . ? N2 C10 1.345(8) . ? C1 C2 1.401(9) . ? C2 C3 1.397(10) . ? C3 C4 1.383(10) . ? C4 C11 1.369(9) . ? C4 C5 1.539(10) . ? C5 C6 1.545(10) . ? C6 C7 1.370(10) . ? C6 C10 1.384(9) . ? C7 C8 1.388(10) . ? C8 C9 1.399(8) . ? C10 C11 1.430(9) . ? C12 C13 1.392(9) . ? C12 C17 1.416(9) . ? C13 C14 1.376(9) . ? C14 C15 1.391(9) . ? C15 C16 1.371(9) . ? C16 C17 1.395(9) . ? C18 C19 1.396(8) . ? C18 C23 1.402(9) . ? C19 C20 1.397(9) . ? C20 C21 1.396(9) . ? C21 C22 1.408(9) . ? C22 C23 1.392(9) . ? C24 C29 1.384(8) . ? C24 C25 1.405(8) . ? C25 C26 1.398(9) . ? C26 C27 1.373(9) . ? C27 C28 1.383(9) . ? C28 C29 1.378(9) . ? C30 C35 1.396(10) . ? C30 C31 1.428(11) . ? C31 C32 1.388(11) . ? C32 C33 1.401(14) . ? C33 C34 1.345(13) . ? C34 C35 1.418(11) . ? C36 C41 1.379(9) . ? C36 C37 1.412(10) . ? C37 C38 1.370(10) . ? C38 C39 1.371(11) . ? C39 C40 1.376(10) . ? C40 C41 1.383(9) . ? C42 C43 1.387(9) . ? C42 C47 1.412(10) . ? C43 C44 1.371(9) . ? C44 C45 1.379(11) . ? C45 C46 1.396(13) . ? C46 C47 1.369(11) . ? Cl3 C48 1.759(11) . ? Cl4 Cl4A 1.420(12) . ? Cl4 Cl4B 1.452(13) . ? Cl4 C48 1.581(14) . ? C48 Cl4B 1.775(14) . ? C48 Cl4A 1.986(17) . ? 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 N2 Ru1 N1 82.5(2) . . ? N2 Ru1 P2 88.01(14) . . ? N1 Ru1 P2 89.68(14) . . ? N2 Ru1 P1 94.02(14) . . ? N1 Ru1 P1 87.60(14) . . ? P2 Ru1 P1 176.36(6) . . ? N2 Ru1 Cl2 88.42(14) . . ? N1 Ru1 Cl2 170.88(15) . . ? P2 Ru1 Cl2 88.74(6) . . ? P1 Ru1 Cl2 94.33(6) . . ? N2 Ru1 Cl1 176.22(14) . . ? N1 Ru1 Cl1 93.69(15) . . ? P2 Ru1 Cl1 92.28(6) . . ? P1 Ru1 Cl1 85.49(6) . . ? Cl2 Ru1 Cl1 95.35(6) . . ? C12 P1 C24 102.8(3) . . ? C12 P1 C18 98.1(3) . . ? C24 P1 C18 103.6(3) . . ? C12 P1 Ru1 122.0(2) . . ? C24 P1 Ru1 108.2(2) . . ? C18 P1 Ru1 119.6(2) . . ? C30 P2 C36 99.9(3) . . ? C30 P2 C42 104.3(3) . . ? C36 P2 C42 102.0(3) . . ? C30 P2 Ru1 116.6(2) . . ? C36 P2 Ru1 120.6(2) . . ? C42 P2 Ru1 111.3(2) . . ? C11 N1 C1 113.3(5) . . ? C11 N1 Ru1 108.9(4) . . ? C1 N1 Ru1 137.8(4) . . ? C9 N2 C10 113.9(5) . . ? C9 N2 Ru1 136.8(4) . . ? C10 N2 Ru1 109.1(4) . . ? N1 C1 C2 121.8(6) . . ? C3 C2 C1 122.1(6) . . ? C4 C3 C2 116.1(6) . . ? C11 C4 C3 117.5(7) . . ? C11 C4 C5 106.7(6) . . ? C3 C4 C5 135.8(6) . . ? O1 C5 C4 127.3(7) . . ? O1 C5 C6 127.7(7) . . ? C4 C5 C6 104.9(5) . . ? C7 C6 C10 117.6(6) . . ? C7 C6 C5 136.9(6) . . ? C10 C6 C5 105.2(6) . . ? C6 C7 C8 116.3(6) . . ? C7 C8 C9 122.4(6) . . ? N2 C9 C8 121.8(6) . . ? N2 C10 C6 128.0(6) . . ? N2 C10 C11 119.7(6) . . ? C6 C10 C11 112.2(6) . . ? N1 C11 C4 129.1(6) . . ? N1 C11 C10 119.8(5) . . ? C4 C11 C10 111.0(6) . . ? C13 C12 C17 118.2(6) . . ? C13 C12 P1 122.2(5) . . ? C17 C12 P1 119.2(5) . . ? C14 C13 C12 121.4(6) . . ? C13 C14 C15 120.3(6) . . ? C16 C15 C14 119.4(6) . . ? C15 C16 C17 121.3(6) . . ? C16 C17 C12 119.4(6) . . ? C19 C18 C23 118.7(6) . . ? C19 C18 P1 118.3(5) . . ? C23 C18 P1 122.7(5) . . ? C18 C19 C20 120.8(6) . . ? C21 C20 C19 120.2(6) . . ? C20 C21 C22 119.4(6) . . ? C23 C22 C21 119.8(6) . . ? C22 C23 C18 121.0(6) . . ? C29 C24 C25 117.9(6) . . ? C29 C24 P1 122.1(5) . . ? C25 C24 P1 119.5(5) . . ? C26 C25 C24 119.9(6) . . ? C27 C26 C25 120.4(6) . . ? C26 C27 C28 120.1(6) . . ? C29 C28 C27 119.5(6) . . ? C28 C29 C24 122.1(6) . . ? C35 C30 C31 117.3(7) . . ? C35 C30 P2 125.1(6) . . ? C31 C30 P2 117.4(6) . . ? C32 C31 C30 121.0(8) . . ? C31 C32 C33 119.4(9) . . ? C34 C33 C32 121.2(9) . . ? C33 C34 C35 120.1(9) . . ? C30 C35 C34 120.9(8) . . ? C41 C36 C37 117.5(6) . . ? C41 C36 P2 123.6(5) . . ? C37 C36 P2 118.7(5) . . ? C38 C37 C36 120.4(7) . . ? C37 C38 C39 121.1(7) . . ? C38 C39 C40 119.5(7) . . ? C39 C40 C41 120.0(7) . . ? C36 C41 C40 121.5(7) . . ? C43 C42 C47 118.8(7) . . ? C43 C42 P2 120.0(5) . . ? C47 C42 P2 120.6(5) . . ? C44 C43 C42 120.5(7) . . ? C43 C44 C45 121.1(8) . . ? C44 C45 C46 118.8(8) . . ? C47 C46 C45 120.9(8) . . ? C46 C47 C42 119.8(7) . . ? Cl4A Cl4 Cl4B 151.7(8) . . ? Cl4A Cl4 C48 82.7(7) . . ? Cl4B Cl4 C48 71.5(6) . . ? Cl4 C48 Cl3 121.0(8) . . ? Cl4 C48 Cl4B 50.9(6) . . ? Cl3 C48 Cl4B 124.7(7) . . ? Cl4 C48 Cl4A 45.2(5) . . ? Cl3 C48 Cl4A 91.6(6) . . ? Cl4B C48 Cl4A 95.3(8) . . ? Cl4 Cl4A C48 52.1(6) . . ? Cl4 Cl4B C48 57.6(6) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.354 _refine_diff_density_min -1.105 _refine_diff_density_rms 0.117