# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 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_d1324 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H50 Cl2 N2 P2 Ru, C1 H2 Cl2' _chemical_formula_sum 'C53 H52 Cl4 N2 P2 Ru' _chemical_formula_weight 1021.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' 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 39.366(4) _cell_length_b 10.3992(11) _cell_length_c 24.505(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.747(2) _cell_angle_gamma 90.00 _cell_volume 9701.5(18) _cell_formula_units_Z 8 _cell_measurement_temperature 150 _cell_measurement_reflns_used 44235 _cell_measurement_theta_min 1.07 _cell_measurement_theta_max 27.52 _exptl_crystal_description Needle _exptl_crystal_colour Bronze _exptl_crystal_size_max 0.360 _exptl_crystal_size_mid 0.220 _exptl_crystal_size_min 0.200 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.399 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4208 _exptl_absorpt_coefficient_mu 0.648 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6786 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details 'SADABS (sheldrick, 1996)' _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 'Bruker Triumph' _diffrn_measurement_device_type 'Bruker Kappa APEX-DUO CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 9 _diffrn_reflns_number 42646 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_sigmaI/netI 0.0529 _diffrn_reflns_limit_h_min -50 _diffrn_reflns_limit_h_max 51 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.07 _diffrn_reflns_theta_max 27.52 _reflns_number_total 11151 _reflns_number_gt 8534 _reflns_threshold_expression >2\s(I) _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement APEX2 _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'CAMERON (Watkin, Prout & Pearce, 1996)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0312P)^2^+9.5954P] 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_number_reflns 11151 _refine_ls_number_parameters 569 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0579 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0834 _refine_ls_wR_factor_gt 0.0736 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.18003(6) 0.3994(2) 0.24706(11) 0.0208(5) Uani 1 1 d . . . C1S C 0.09486(12) 0.8740(4) 0.23555(15) 0.0717(12) Uani 1 1 d . . . H1S1 H 0.1007 0.7986 0.2164 0.086 Uiso 1 1 calc R . . H1S2 H 0.0953 0.9481 0.2117 0.086 Uiso 1 1 calc R . . C2 C 0.23730(6) 0.4551(3) 0.27682(12) 0.0328(7) Uani 1 1 d . . . H3 H 0.2596 0.4837 0.2764 0.039 Uiso 1 1 calc R . . C3 C 0.22720(6) 0.4136(3) 0.32168(13) 0.0352(7) Uani 1 1 d . . . H2 H 0.2412 0.4085 0.3584 0.042 Uiso 1 1 calc R . . C4 C 0.20826(6) 0.4926(2) 0.17551(11) 0.0239(6) Uani 1 1 d . . . C5 C 0.22401(6) 0.4158(2) 0.14227(11) 0.0243(6) Uani 1 1 d . . . C6 C 0.22411(6) 0.4616(3) 0.08909(12) 0.0284(6) Uani 1 1 d . . . H6 H 0.2340 0.4110 0.0658 0.034 Uiso 1 1 calc R . . C7 C 0.20997(6) 0.5807(3) 0.06943(13) 0.0332(7) Uani 1 1 d . . . C8 C 0.19513(6) 0.6547(3) 0.10461(13) 0.0337(7) Uani 1 1 d . . . H8 H 0.1854 0.7340 0.0917 0.040 Uiso 1 1 calc R . . C9 C 0.19431(6) 0.6144(2) 0.15833(12) 0.0287(6) Uani 1 1 d . . . C10 C 0.17921(7) 0.6998(2) 0.19570(14) 0.0373(7) Uani 1 1 d . . . H10A H 0.1787 0.7870 0.1826 0.056 Uiso 1 1 calc R . . H10B H 0.1935 0.6948 0.2337 0.056 Uiso 1 1 calc R . . H10C H 0.1558 0.6723 0.1946 0.056 Uiso 1 1 calc R . . C11 C 0.24105(7) 0.2894(3) 0.16288(12) 0.0325(6) Uani 1 1 d . . . H11A H 0.2452 0.2418 0.1316 0.049 Uiso 1 1 calc R . . H11B H 0.2259 0.2408 0.1802 0.049 Uiso 1 1 calc R . . H11C H 0.2630 0.3047 0.1900 0.049 Uiso 1 1 calc R . . C12 C 0.21236(8) 0.6269(3) 0.01240(14) 0.0472(9) Uani 1 1 d . . . H12A H 0.1959 0.6955 0.0000 0.071 Uiso 1 1 calc R . . H12B H 0.2070 0.5573 -0.0141 0.071 Uiso 1 1 calc R . . H12C H 0.2357 0.6576 0.0149 0.071 Uiso 1 1 calc R . . C13 C 0.17209(6) 0.3410(3) 0.34308(11) 0.0250(6) Uani 1 1 d . . . C14 C 0.17467(6) 0.2154(3) 0.36326(11) 0.0272(6) Uani 1 1 d . . . C15 C 0.15462(7) 0.1829(3) 0.40045(11) 0.0308(6) Uani 1 1 d . . . H15 H 0.1552 0.0986 0.4134 0.037 Uiso 1 1 calc R . . C16 C 0.13369(7) 0.2720(3) 0.41893(12) 0.0345(7) Uani 1 1 d . . . C17 C 0.13377(7) 0.3979(3) 0.40006(12) 0.0339(7) Uani 1 1 d . . . H17 H 0.1206 0.4592 0.4133 0.041 Uiso 1 1 calc R . . C18 C 0.15272(6) 0.4357(3) 0.36226(11) 0.0278(6) Uani 1 1 d . . . C19 C 0.15266(7) 0.5732(3) 0.34309(13) 0.0369(7) Uani 1 1 d . . . H19A H 0.1408 0.6259 0.3646 0.055 Uiso 1 1 calc R . . H19B H 0.1407 0.5789 0.3038 0.055 Uiso 1 1 calc R . . H19C H 0.1764 0.6025 0.3486 0.055 Uiso 1 1 calc R . . C20 C 0.19827(7) 0.1180(3) 0.34621(12) 0.0348(7) Uani 1 1 d . . . H20A H 0.1920 0.1095 0.3059 0.052 Uiso 1 1 calc R . . H20B H 0.1956 0.0365 0.3631 0.052 Uiso 1 1 calc R . . H20C H 0.2222 0.1459 0.3588 0.052 Uiso 1 1 calc R . . C21 C 0.11224(8) 0.2332(4) 0.45930(14) 0.0523(9) Uani 1 1 d . . . H21A H 0.0877 0.2352 0.4401 0.078 Uiso 1 1 calc R . . H21B H 0.1167 0.2919 0.4906 0.078 Uiso 1 1 calc R . . H21C H 0.1187 0.1477 0.4729 0.078 Uiso 1 1 calc R . . C22 C 0.10574(6) 0.3617(2) 0.23697(10) 0.0190(5) Uani 1 1 d . . . C23 C 0.08034(6) 0.4549(3) 0.23805(11) 0.0250(6) Uani 1 1 d . . . H23 H 0.0816 0.5346 0.2214 0.030 Uiso 1 1 calc R . . C24 C 0.05326(7) 0.4306(3) 0.26362(12) 0.0337(7) Uani 1 1 d . . . H24 H 0.0364 0.4934 0.2635 0.040 Uiso 1 1 calc R . . C25 C 0.05130(7) 0.3134(3) 0.28912(12) 0.0361(7) Uani 1 1 d . . . H25 H 0.0333 0.2973 0.3065 0.043 Uiso 1 1 calc R . . C26 C 0.07622(7) 0.2202(3) 0.28864(11) 0.0309(6) Uani 1 1 d . . . H26 H 0.0750 0.1416 0.3061 0.037 Uiso 1 1 calc R . . C27 C 0.10300(6) 0.2425(2) 0.26241(11) 0.0231(5) Uani 1 1 d . . . H27 H 0.1192 0.1780 0.2617 0.028 Uiso 1 1 calc R . . C28 C 0.14945(6) 0.2796(2) 0.08323(11) 0.0208(5) Uani 1 1 d . . . C29 C 0.16989(6) 0.2039(2) 0.05219(11) 0.0213(5) Uani 1 1 d . . . C30 C 0.18174(6) 0.0782(2) 0.06741(12) 0.0272(6) Uani 1 1 d . . . H30 H 0.1772 0.0395 0.0990 0.033 Uiso 1 1 calc R . . C31 C 0.20020(7) 0.0122(3) 0.03514(12) 0.0309(6) Uani 1 1 d . . . H31 H 0.2086 -0.0700 0.0460 0.037 Uiso 1 1 calc R . . C32 C 0.20631(7) 0.0663(3) -0.01281(13) 0.0354(7) Uani 1 1 d . . . H32 H 0.2185 0.0204 -0.0342 0.042 Uiso 1 1 calc R . . C33 C 0.19427(7) 0.1884(3) -0.02899(13) 0.0385(7) Uani 1 1 d . . . H33 H 0.1981 0.2248 -0.0615 0.046 Uiso 1 1 calc R . . C34 C 0.17641(7) 0.2565(3) 0.00344(12) 0.0290(6) Uani 1 1 d . . . H34 H 0.1686 0.3393 -0.0075 0.035 Uiso 1 1 calc R . . C35 C 0.07354(6) 0.3142(2) 0.00352(11) 0.0222(5) Uani 1 1 d . . . C36 C 0.08491(7) 0.2083(3) -0.02194(12) 0.0295(6) Uani 1 1 d . . . H36 H 0.0935 0.1362 -0.0004 0.035 Uiso 1 1 calc R . . C37 C 0.08351(7) 0.2097(3) -0.07916(12) 0.0358(7) Uani 1 1 d . . . H37 H 0.0912 0.1386 -0.0957 0.043 Uiso 1 1 calc R . . C38 C 0.07071(7) 0.3159(3) -0.11158(12) 0.0385(7) Uani 1 1 d . . . H38 H 0.0698 0.3164 -0.1499 0.046 Uiso 1 1 calc R . . C39 C 0.05917(7) 0.4214(3) -0.08719(12) 0.0358(7) Uani 1 1 d . . . H39 H 0.0506 0.4931 -0.1091 0.043 Uiso 1 1 calc R . . C40 C 0.06029(6) 0.4209(3) -0.02985(11) 0.0270(6) Uani 1 1 d . . . H40 H 0.0522 0.4917 -0.0137 0.032 Uiso 1 1 calc R . . C41 C 0.06640(6) 0.4779(2) 0.09206(10) 0.0184(5) Uani 1 1 d . . . C42 C 0.09177(6) 0.5698(2) 0.08966(11) 0.0220(5) Uani 1 1 d . . . H42 H 0.1132 0.5437 0.0838 0.026 Uiso 1 1 calc R . . C43 C 0.08552(7) 0.6993(2) 0.09591(11) 0.0268(6) Uani 1 1 d . . . H43 H 0.1025 0.7598 0.0937 0.032 Uiso 1 1 calc R . . C44 C 0.05393(7) 0.7384(2) 0.10550(12) 0.0299(6) Uani 1 1 d . . . H44 H 0.0496 0.8254 0.1095 0.036 Uiso 1 1 calc R . . C45 C 0.02882(7) 0.6487(2) 0.10915(12) 0.0299(6) Uani 1 1 d . . . H45 H 0.0078 0.6751 0.1163 0.036 Uiso 1 1 calc R . . C46 C 0.03492(6) 0.5182(2) 0.10218(11) 0.0239(6) Uani 1 1 d . . . H46 H 0.0178 0.4580 0.1043 0.029 Uiso 1 1 calc R . . C47 C 0.03665(6) 0.2228(2) 0.08360(11) 0.0201(5) Uani 1 1 d . . . C48 C 0.01025(7) 0.1915(3) 0.03637(12) 0.0332(7) Uani 1 1 d . . . H48 H 0.0116 0.2195 0.0010 0.040 Uiso 1 1 calc R . . C49 C -0.01823(7) 0.1186(3) 0.04145(14) 0.0452(8) Uani 1 1 d . . . H49 H -0.0357 0.0970 0.0094 0.054 Uiso 1 1 calc R . . C50 C -0.02078(7) 0.0779(3) 0.09358(14) 0.0403(8) Uani 1 1 d . . . H50 H -0.0398 0.0281 0.0967 0.048 Uiso 1 1 calc R . . C51 C 0.00495(7) 0.1108(3) 0.14150(13) 0.0346(7) Uani 1 1 d . . . H51 H 0.0031 0.0844 0.1769 0.042 Uiso 1 1 calc R . . C52 C 0.03344(6) 0.1830(2) 0.13648(12) 0.0271(6) Uani 1 1 d . . . H52 H 0.0507 0.2053 0.1687 0.032 Uiso 1 1 calc R . . Cl1 Cl 0.102963(17) 0.01489(5) 0.09824(3) 0.03077(16) Uani 1 1 d . . . Cl1S Cl 0.05257(3) 0.85623(11) 0.24533(5) 0.0781(3) Uani 1 1 d . . . Cl2 Cl 0.171152(16) 0.09609(6) 0.20057(3) 0.02773(15) Uani 1 1 d . . . Cl2S Cl 0.12631(3) 0.89412(8) 0.29950(4) 0.0653(3) Uani 1 1 d . . . N1 N 0.20833(5) 0.44755(19) 0.23105(9) 0.0231(5) Uani 1 1 d . . . N2 N 0.19190(5) 0.3791(2) 0.30359(9) 0.0251(5) Uani 1 1 d . . . P1 P 0.136977(15) 0.40014(6) 0.19468(3) 0.01765(14) Uani 1 1 d . . . P2 P 0.076131(15) 0.31060(5) 0.07955(3) 0.01719(13) Uani 1 1 d . . . Ru1 Ru 0.127008(5) 0.217616(17) 0.135205(9) 0.01668(6) Uani 1 1 d . . . H28 H 0.1455(6) 0.365(3) 0.0686(11) 0.025(7) 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 C1 0.0197(11) 0.0179(11) 0.0246(15) -0.0008(11) 0.0052(10) 0.0007(9) C1S 0.127(4) 0.052(2) 0.042(2) -0.0038(19) 0.034(2) -0.025(2) C2 0.0172(12) 0.0409(16) 0.0343(18) -0.0017(14) -0.0043(12) -0.0025(11) C3 0.0198(12) 0.0483(17) 0.0314(17) -0.0006(15) -0.0048(12) -0.0007(12) C4 0.0156(11) 0.0262(12) 0.0272(15) 0.0025(12) 0.0006(10) -0.0067(10) C5 0.0148(11) 0.0272(13) 0.0298(16) 0.0047(12) 0.0034(10) -0.0065(10) C6 0.0182(11) 0.0349(14) 0.0310(16) 0.0035(13) 0.0043(11) -0.0065(11) C7 0.0189(12) 0.0416(16) 0.0353(18) 0.0143(14) -0.0002(12) -0.0092(12) C8 0.0229(12) 0.0257(13) 0.048(2) 0.0134(14) 0.0014(13) -0.0063(11) C9 0.0178(11) 0.0225(12) 0.0420(18) 0.0039(13) 0.0004(11) -0.0077(10) C10 0.0354(14) 0.0207(13) 0.052(2) -0.0042(13) 0.0045(14) -0.0026(12) C11 0.0293(13) 0.0313(14) 0.0381(18) 0.0062(13) 0.0108(12) 0.0047(12) C12 0.0355(16) 0.057(2) 0.048(2) 0.0244(18) 0.0077(15) -0.0040(15) C13 0.0202(11) 0.0339(14) 0.0178(14) -0.0018(12) -0.0008(10) 0.0039(11) C14 0.0241(12) 0.0377(15) 0.0165(14) -0.0012(12) -0.0011(10) 0.0056(12) C15 0.0302(13) 0.0375(15) 0.0216(15) 0.0037(13) 0.0008(11) 0.0045(12) C16 0.0286(13) 0.0512(17) 0.0225(16) 0.0004(14) 0.0041(12) 0.0068(13) C17 0.0274(13) 0.0436(17) 0.0289(17) -0.0079(14) 0.0038(12) 0.0101(13) C18 0.0251(12) 0.0346(14) 0.0194(15) -0.0030(12) -0.0022(11) 0.0055(11) C19 0.0394(15) 0.0323(15) 0.0356(18) -0.0080(14) 0.0033(14) 0.0034(13) C20 0.0358(15) 0.0438(16) 0.0232(16) 0.0072(14) 0.0045(12) 0.0152(13) C21 0.0495(18) 0.071(2) 0.043(2) 0.0074(19) 0.0239(16) 0.0061(18) C22 0.0173(10) 0.0222(11) 0.0155(13) -0.0039(10) 0.0005(9) -0.0015(9) C23 0.0232(12) 0.0288(13) 0.0212(15) -0.0055(12) 0.0020(11) 0.0004(11) C24 0.0232(13) 0.0483(17) 0.0300(17) -0.0080(14) 0.0074(12) 0.0054(12) C25 0.0272(13) 0.0573(19) 0.0263(16) -0.0061(15) 0.0117(12) -0.0082(13) C26 0.0345(14) 0.0369(15) 0.0211(15) 0.0005(13) 0.0067(12) -0.0076(13) C27 0.0228(11) 0.0262(12) 0.0187(14) -0.0016(11) 0.0024(10) -0.0005(10) C28 0.0194(11) 0.0171(11) 0.0249(15) 0.0014(11) 0.0040(10) -0.0013(10) C29 0.0202(11) 0.0227(12) 0.0230(14) -0.0031(11) 0.0090(10) -0.0033(10) C30 0.0315(13) 0.0264(13) 0.0268(16) -0.0025(12) 0.0132(12) -0.0006(11) C31 0.0334(14) 0.0265(13) 0.0360(18) -0.0039(13) 0.0144(13) 0.0007(12) C32 0.0332(14) 0.0414(16) 0.0378(19) -0.0117(14) 0.0205(13) -0.0037(13) C33 0.0432(16) 0.0496(18) 0.0288(17) 0.0009(15) 0.0204(14) -0.0064(14) C34 0.0283(13) 0.0316(14) 0.0286(16) 0.0042(12) 0.0099(12) -0.0037(11) C35 0.0212(11) 0.0268(12) 0.0184(14) -0.0031(11) 0.0048(10) -0.0110(10) C36 0.0326(13) 0.0314(14) 0.0253(16) -0.0060(12) 0.0089(12) -0.0114(12) C37 0.0362(14) 0.0453(17) 0.0295(17) -0.0147(15) 0.0148(13) -0.0168(14) C38 0.0366(15) 0.062(2) 0.0175(15) -0.0055(15) 0.0084(12) -0.0209(15) C39 0.0314(14) 0.0515(18) 0.0226(16) 0.0079(14) 0.0031(12) -0.0135(14) C40 0.0238(12) 0.0339(14) 0.0233(15) 0.0015(12) 0.0061(11) -0.0063(11) C41 0.0215(11) 0.0159(11) 0.0155(13) 0.0007(10) 0.0003(10) -0.0006(9) C42 0.0213(11) 0.0211(12) 0.0225(14) 0.0004(11) 0.0034(10) -0.0025(10) C43 0.0296(13) 0.0201(12) 0.0286(16) 0.0011(11) 0.0037(11) -0.0040(10) C44 0.0340(14) 0.0187(12) 0.0335(17) -0.0017(12) 0.0020(12) 0.0044(11) C45 0.0240(12) 0.0277(13) 0.0362(17) -0.0038(13) 0.0043(12) 0.0038(11) C46 0.0198(11) 0.0248(12) 0.0252(15) -0.0027(11) 0.0023(10) -0.0034(10) C47 0.0204(11) 0.0180(11) 0.0228(14) -0.0032(11) 0.0073(10) -0.0043(10) C48 0.0277(13) 0.0466(17) 0.0242(16) -0.0023(13) 0.0047(11) -0.0162(12) C49 0.0334(15) 0.063(2) 0.0373(19) -0.0135(17) 0.0060(14) -0.0259(15) C50 0.0304(14) 0.0432(17) 0.050(2) -0.0070(16) 0.0143(14) -0.0214(13) C51 0.0338(14) 0.0371(15) 0.0368(18) 0.0050(14) 0.0161(13) -0.0082(13) C52 0.0233(12) 0.0313(13) 0.0258(16) -0.0003(12) 0.0049(11) -0.0086(11) Cl1 0.0384(3) 0.0143(3) 0.0406(4) -0.0039(3) 0.0118(3) -0.0067(3) Cl1S 0.1024(8) 0.0729(7) 0.0562(7) 0.0092(6) 0.0151(6) 0.0119(6) Cl2 0.0320(3) 0.0255(3) 0.0263(4) 0.0057(3) 0.0086(3) 0.0098(3) Cl2S 0.1046(8) 0.0430(5) 0.0501(6) 0.0070(4) 0.0231(5) -0.0066(5) N1 0.0184(9) 0.0251(10) 0.0231(12) 0.0012(10) 0.0002(9) -0.0027(8) N2 0.0198(10) 0.0332(12) 0.0199(12) 0.0010(10) 0.0006(9) 0.0022(9) P1 0.0156(3) 0.0161(3) 0.0197(4) -0.0005(3) 0.0018(2) -0.0004(2) P2 0.0181(3) 0.0153(3) 0.0181(3) -0.0015(3) 0.0044(2) -0.0045(2) Ru1 0.01902(9) 0.01264(9) 0.01935(11) 0.00045(8) 0.00666(7) -0.00118(7) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.361(3) . ? C1 N1 1.367(3) . ? C1 P1 1.847(2) . ? C1S Cl2S 1.745(4) . ? C1S Cl1S 1.751(4) . ? C2 C3 1.332(4) . ? C2 N1 1.383(3) . ? C3 N2 1.394(3) . ? C4 C5 1.394(4) . ? C4 C9 1.402(3) . ? C4 N1 1.439(3) . ? C5 C6 1.389(4) . ? C5 C11 1.503(3) . ? C6 C7 1.393(4) . ? C7 C8 1.390(4) . ? C7 C12 1.503(4) . ? C8 C9 1.390(4) . ? C9 C10 1.503(4) . ? C13 C14 1.391(4) . ? C13 C18 1.398(4) . ? C13 N2 1.445(3) . ? C14 C15 1.391(4) . ? C14 C20 1.504(4) . ? C15 C16 1.390(4) . ? C16 C17 1.389(4) . ? C16 C21 1.510(4) . ? C17 C18 1.386(4) . ? C18 C19 1.505(4) . ? C22 C23 1.398(3) . ? C22 C27 1.404(3) . ? C22 P1 1.843(3) . ? C23 C24 1.390(4) . ? C24 C25 1.380(4) . ? C25 C26 1.381(4) . ? C26 C27 1.387(4) . ? C28 C29 1.469(3) . ? C28 Ru1 1.841(3) . ? C29 C34 1.396(4) . ? C29 C30 1.406(3) . ? C30 C31 1.385(4) . ? C31 C32 1.378(4) . ? C32 C33 1.378(4) . ? C33 C34 1.383(4) . ? C35 C36 1.394(4) . ? C35 C40 1.398(4) . ? C35 P2 1.840(3) . ? C36 C37 1.389(4) . ? C37 C38 1.379(4) . ? C38 C39 1.381(4) . ? C39 C40 1.395(4) . ? C41 C46 1.389(3) . ? C41 C42 1.394(3) . ? C41 P2 1.824(2) . ? C42 C43 1.384(3) . ? C43 C44 1.384(4) . ? C44 C45 1.379(4) . ? C45 C46 1.397(3) . ? C47 C48 1.383(3) . ? C47 C52 1.396(4) . ? C47 P2 1.827(2) . ? C48 C49 1.385(4) . ? C49 C50 1.373(4) . ? C50 C51 1.384(4) . ? C51 C52 1.381(3) . ? Cl1 Ru1 2.3925(6) . ? Cl2 Ru1 2.4012(6) . ? P1 Ru1 2.3643(7) . ? P2 Ru1 2.3272(6) . ? 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 C1 N1 104.77(19) . . ? N2 C1 P1 136.43(19) . . ? N1 C1 P1 118.01(18) . . ? Cl2S C1S Cl1S 111.8(2) . . ? C3 C2 N1 107.0(2) . . ? C2 C3 N2 107.7(2) . . ? C5 C4 C9 122.7(3) . . ? C5 C4 N1 118.2(2) . . ? C9 C4 N1 119.0(2) . . ? C6 C5 C4 117.4(2) . . ? C6 C5 C11 120.5(2) . . ? C4 C5 C11 122.1(2) . . ? C5 C6 C7 122.2(3) . . ? C8 C7 C6 118.1(3) . . ? C8 C7 C12 122.4(3) . . ? C6 C7 C12 119.5(3) . . ? C9 C8 C7 122.4(3) . . ? C8 C9 C4 117.1(3) . . ? C8 C9 C10 120.5(2) . . ? C4 C9 C10 122.5(3) . . ? C14 C13 C18 122.6(3) . . ? C14 C13 N2 119.5(2) . . ? C18 C13 N2 117.8(2) . . ? C15 C14 C13 117.3(2) . . ? C15 C14 C20 120.8(3) . . ? C13 C14 C20 121.9(2) . . ? C16 C15 C14 122.3(3) . . ? C17 C16 C15 117.9(3) . . ? C17 C16 C21 121.3(3) . . ? C15 C16 C21 120.8(3) . . ? C18 C17 C16 122.5(3) . . ? C17 C18 C13 117.2(3) . . ? C17 C18 C19 121.3(3) . . ? C13 C18 C19 121.5(3) . . ? C23 C22 C27 117.9(2) . . ? C23 C22 P1 116.32(19) . . ? C27 C22 P1 125.37(18) . . ? C24 C23 C22 121.1(3) . . ? C25 C24 C23 120.2(3) . . ? C24 C25 C26 119.6(3) . . ? C25 C26 C27 120.8(3) . . ? C26 C27 C22 120.4(2) . . ? C29 C28 Ru1 126.40(18) . . ? C34 C29 C30 118.1(2) . . ? C34 C29 C28 118.5(2) . . ? C30 C29 C28 123.3(2) . . ? C31 C30 C29 119.8(3) . . ? C32 C31 C30 121.0(3) . . ? C33 C32 C31 120.0(3) . . ? C32 C33 C34 119.7(3) . . ? C33 C34 C29 121.5(3) . . ? C36 C35 C40 118.6(2) . . ? C36 C35 P2 119.7(2) . . ? C40 C35 P2 121.6(2) . . ? C37 C36 C35 120.6(3) . . ? C38 C37 C36 120.3(3) . . ? C37 C38 C39 120.0(3) . . ? C38 C39 C40 120.2(3) . . ? C39 C40 C35 120.3(3) . . ? C46 C41 C42 118.8(2) . . ? C46 C41 P2 123.56(18) . . ? C42 C41 P2 117.60(18) . . ? C43 C42 C41 120.8(2) . . ? C44 C43 C42 119.8(2) . . ? C45 C44 C43 120.1(2) . . ? C44 C45 C46 120.1(2) . . ? C41 C46 C45 120.3(2) . . ? C48 C47 C52 118.7(2) . . ? C48 C47 P2 122.7(2) . . ? C52 C47 P2 118.54(18) . . ? C47 C48 C49 120.4(3) . . ? C50 C49 C48 120.3(3) . . ? C49 C50 C51 120.1(3) . . ? C52 C51 C50 119.6(3) . . ? C51 C52 C47 120.8(2) . . ? C1 N1 C2 110.6(2) . . ? C1 N1 C4 125.82(19) . . ? C2 N1 C4 123.5(2) . . ? C1 N2 C3 109.9(2) . . ? C1 N2 C13 128.3(2) . . ? C3 N2 C13 121.5(2) . . ? C22 P1 C1 103.53(11) . . ? C22 P1 Ru1 98.20(8) . . ? C1 P1 Ru1 113.81(8) . . ? C41 P2 C47 104.46(11) . . ? C41 P2 C35 101.00(11) . . ? C47 P2 C35 103.68(11) . . ? C41 P2 Ru1 118.95(7) . . ? C47 P2 Ru1 112.19(8) . . ? C35 P2 Ru1 114.79(8) . . ? C28 Ru1 P2 86.69(7) . . ? C28 Ru1 P1 96.43(8) . . ? P2 Ru1 P1 90.61(2) . . ? C28 Ru1 Cl1 105.05(8) . . ? P2 Ru1 Cl1 86.89(2) . . ? P1 Ru1 Cl1 158.18(2) . . ? C28 Ru1 Cl2 104.61(7) . . ? P2 Ru1 Cl2 168.06(2) . . ? P1 Ru1 Cl2 91.89(2) . . ? Cl1 Ru1 Cl2 86.45(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.589 _refine_diff_density_min -0.555 _refine_diff_density_rms 0.083 _database_code_depnum_ccdc_archive 'CCDC 945573' ####################################################################### # # 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_d12283 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H49 Cl N2 P2 Ru' _chemical_formula_sum 'C52 H49 Cl N2 P2 Ru' _chemical_formula_weight 900.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 11.796(3) _cell_length_b 18.979(5) _cell_length_c 20.473(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.625(7) _cell_angle_gamma 90.00 _cell_volume 4519(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 40744 _cell_measurement_theta_min 1.47 _cell_measurement_theta_max 27.42 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.020 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.323 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1864 _exptl_absorpt_coefficient_mu 0.514 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7022 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details 'SADABS (sheldrick, 1996)' _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 'Bruker Triumph' _diffrn_measurement_device_type 'Bruker Kappa APEX-DUO CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 9 _diffrn_reflns_number 40082 _diffrn_reflns_av_R_equivalents 0.0505 _diffrn_reflns_av_sigmaI/netI 0.0498 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 27.42 _reflns_number_total 10285 _reflns_number_gt 8113 _reflns_threshold_expression >2\s(I) _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement APEX2 _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0272P)^2^+2.0931P] 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 10285 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0506 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.0736 _refine_ls_wR_factor_gt 0.0675 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _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 C1 C 0.53366(18) 0.07226(9) 0.30816(11) 0.0146(4) Uani 1 1 d . . . C2 C 0.5888(2) -0.01774(11) 0.37699(12) 0.0244(5) Uani 1 1 d . . . H2 H 0.5940 -0.0481 0.4130 0.029 Uiso 1 1 calc R . . C3 C 0.6477(2) -0.02305(10) 0.32632(12) 0.0231(5) Uani 1 1 d . . . H3 H 0.7010 -0.0577 0.3206 0.028 Uiso 1 1 calc R . . C4 C 0.44790(19) 0.06746(10) 0.41228(11) 0.0165(4) Uani 1 1 d . . . C5 C 0.49418(19) 0.11941(10) 0.45676(11) 0.0185(5) Uani 1 1 d . . . C6 C 0.4209(2) 0.14917(11) 0.49616(11) 0.0209(5) Uani 1 1 d . . . H6 H 0.4493 0.1841 0.5263 0.025 Uiso 1 1 calc R . . C7 C 0.3069(2) 0.12819(11) 0.49171(11) 0.0228(5) Uani 1 1 d . . . C8 C 0.2675(2) 0.07269(11) 0.44949(12) 0.0237(5) Uani 1 1 d . . . H8 H 0.1927 0.0566 0.4481 0.028 Uiso 1 1 calc R . . C9 C 0.3370(2) 0.04040(10) 0.40918(11) 0.0206(5) Uani 1 1 d . . . C10 C 0.6164(2) 0.14484(12) 0.46219(13) 0.0279(5) Uani 1 1 d . . . H10A H 0.6226 0.1755 0.4256 0.042 Uiso 1 1 calc R . . H10B H 0.6666 0.1052 0.4613 0.042 Uiso 1 1 calc R . . H10C H 0.6378 0.1701 0.5030 0.042 Uiso 1 1 calc R . . C11 C 0.2289(3) 0.16415(14) 0.53262(14) 0.0394(7) Uani 1 1 d . . . H11A H 0.2240 0.1362 0.5712 0.059 Uiso 1 1 calc R . . H11B H 0.1537 0.1694 0.5067 0.059 Uiso 1 1 calc R . . H11C H 0.2594 0.2098 0.5461 0.059 Uiso 1 1 calc R . . C12 C 0.2942(2) -0.02120(11) 0.36562(13) 0.0308(6) Uani 1 1 d . . . H12A H 0.3182 -0.0159 0.3233 0.046 Uiso 1 1 calc R . . H12B H 0.2118 -0.0229 0.3596 0.046 Uiso 1 1 calc R . . H12C H 0.3254 -0.0641 0.3861 0.046 Uiso 1 1 calc R . . C13 C 0.66599(19) 0.05198(10) 0.22732(11) 0.0168(5) Uani 1 1 d . . . C14 C 0.6515(2) 0.00761(10) 0.17280(12) 0.0223(5) Uani 1 1 d . . . C15 C 0.7078(2) 0.02655(11) 0.12019(12) 0.0262(5) Uani 1 1 d . . . H15 H 0.7002 -0.0022 0.0829 0.031 Uiso 1 1 calc R . . C16 C 0.7744(2) 0.08687(12) 0.12233(12) 0.0256(5) Uani 1 1 d . . . C17 C 0.7852(2) 0.13073(11) 0.17776(11) 0.0210(5) Uani 1 1 d . . . H17 H 0.8286 0.1717 0.1784 0.025 Uiso 1 1 calc R . . C18 C 0.73216(18) 0.11471(10) 0.23301(11) 0.0163(4) Uani 1 1 d . . . C19 C 0.5784(2) -0.05803(11) 0.16923(13) 0.0310(6) Uani 1 1 d . . . H19A H 0.6201 -0.0946 0.1953 0.047 Uiso 1 1 calc R . . H19B H 0.5595 -0.0733 0.1240 0.047 Uiso 1 1 calc R . . H19C H 0.5089 -0.0480 0.1861 0.047 Uiso 1 1 calc R . . C20 C 0.8380(3) 0.10514(14) 0.06603(13) 0.0400(7) Uani 1 1 d . . . H20A H 0.9161 0.0891 0.0767 0.060 Uiso 1 1 calc R . . H20B H 0.8371 0.1553 0.0597 0.060 Uiso 1 1 calc R . . H20C H 0.8011 0.0826 0.0261 0.060 Uiso 1 1 calc R . . C21 C 0.73879(18) 0.16243(10) 0.28983(11) 0.0160(4) Uani 1 1 d . . . H21A H 0.8110 0.1878 0.2998 0.019 Uiso 1 1 calc R . . H21B H 0.7199 0.1401 0.3293 0.019 Uiso 1 1 calc R . . C22 C 0.3642(2) 0.10156(10) 0.20135(12) 0.0210(5) Uani 1 1 d . . . C23 C 0.3895(2) 0.08602(11) 0.13885(12) 0.0259(5) Uani 1 1 d . . . H23 H 0.4590 0.1006 0.1276 0.031 Uiso 1 1 calc R . . C24 C 0.3112(3) 0.04882(15) 0.09321(15) 0.0424(7) Uani 1 1 d . . . H24 H 0.3286 0.0387 0.0516 0.051 Uiso 1 1 calc R . . C25 C 0.2078(3) 0.02680(17) 0.10944(17) 0.0571(9) Uani 1 1 d . . . H25 H 0.1559 0.0017 0.0789 0.068 Uiso 1 1 calc R . . C26 C 0.1815(3) 0.04215(17) 0.17136(17) 0.0554(9) Uani 1 1 d . . . H26 H 0.1120 0.0272 0.1823 0.066 Uiso 1 1 calc R . . C27 C 0.2585(2) 0.07978(14) 0.21710(14) 0.0357(6) Uani 1 1 d . . . H27 H 0.2399 0.0906 0.2583 0.043 Uiso 1 1 calc R . . C28 C 0.56254(19) 0.27212(10) 0.31883(10) 0.0169(4) Uani 1 1 d . . . C29 C 0.6387(2) 0.32098(11) 0.35446(11) 0.0237(5) Uani 1 1 d . . . H29 H 0.7077 0.3308 0.3400 0.028 Uiso 1 1 calc R . . C30 C 0.6139(3) 0.35505(12) 0.41055(13) 0.0338(6) Uani 1 1 d . . . H30 H 0.6664 0.3870 0.4330 0.041 Uiso 1 1 calc R . . C31 C 0.5113(3) 0.34176(12) 0.43345(13) 0.0364(7) Uani 1 1 d . . . H31 H 0.4936 0.3658 0.4701 0.044 Uiso 1 1 calc R . . C32 C 0.4357(2) 0.29224(11) 0.40090(13) 0.0283(6) Uani 1 1 d . . . H32 H 0.3674 0.2827 0.4162 0.034 Uiso 1 1 calc R . . C33 C 0.4611(2) 0.25641(10) 0.34530(11) 0.0199(5) Uani 1 1 d . . . C34 C 0.38315(19) 0.19847(10) 0.31291(11) 0.0188(5) Uani 1 1 d . . . H34A H 0.3144 0.2181 0.2866 0.023 Uiso 1 1 calc R . . H34B H 0.3609 0.1671 0.3460 0.023 Uiso 1 1 calc R . . C35 C 0.4650(2) 0.26269(10) 0.07445(11) 0.0197(5) Uani 1 1 d . . . C36 C 0.5409(2) 0.21057(10) 0.06025(12) 0.0240(5) Uani 1 1 d . . . H36 H 0.5936 0.1912 0.0944 0.029 Uiso 1 1 calc R . . C37 C 0.5384(2) 0.18743(12) -0.00448(13) 0.0344(6) Uani 1 1 d . . . H37 H 0.5884 0.1521 -0.0131 0.041 Uiso 1 1 calc R . . C38 C 0.4623(3) 0.21656(13) -0.05595(13) 0.0365(6) Uani 1 1 d . . . H38 H 0.4623 0.2018 -0.0993 0.044 Uiso 1 1 calc R . . C39 C 0.3859(2) 0.26790(13) -0.04263(13) 0.0351(6) Uani 1 1 d . . . H39 H 0.3339 0.2873 -0.0771 0.042 Uiso 1 1 calc R . . C40 C 0.3865(2) 0.29052(12) 0.02193(12) 0.0270(5) Uani 1 1 d . . . H40 H 0.3342 0.3246 0.0304 0.032 Uiso 1 1 calc R . . C41 C 0.50384(19) 0.38712(10) 0.15701(11) 0.0178(5) Uani 1 1 d . . . C42 C 0.50653(19) 0.42443(10) 0.09864(12) 0.0217(5) Uani 1 1 d . . . H42 H 0.4922 0.4012 0.0581 0.026 Uiso 1 1 calc R . . C43 C 0.5308(2) 0.49675(11) 0.10089(13) 0.0271(6) Uani 1 1 d . . . H43 H 0.5338 0.5210 0.0617 0.033 Uiso 1 1 calc R . . C44 C 0.5502(2) 0.53234(11) 0.16021(13) 0.0287(6) Uani 1 1 d . . . H44 H 0.5627 0.5807 0.1611 0.034 Uiso 1 1 calc R . . C45 C 0.5509(2) 0.49537(11) 0.21883(13) 0.0287(6) Uani 1 1 d . . . H45 H 0.5661 0.5189 0.2592 0.034 Uiso 1 1 calc R . . C46 C 0.5289(2) 0.42317(11) 0.21734(12) 0.0237(5) Uani 1 1 d . . . H46 H 0.5309 0.3987 0.2569 0.028 Uiso 1 1 calc R . . C47 C 0.3180(2) 0.29452(11) 0.16982(12) 0.0243(5) Uani 1 1 d . . . C48 C 0.2838(2) 0.33652(12) 0.21920(13) 0.0309(6) Uani 1 1 d . . . H48 H 0.3367 0.3664 0.2442 0.037 Uiso 1 1 calc R . . C49 C 0.1705(3) 0.33396(14) 0.23132(16) 0.0442(8) Uani 1 1 d . . . H49 H 0.1489 0.3621 0.2644 0.053 Uiso 1 1 calc R . . C50 C 0.0904(3) 0.29003(16) 0.19464(19) 0.0542(10) Uani 1 1 d . . . H50 H 0.0152 0.2887 0.2028 0.065 Uiso 1 1 calc R . . C51 C 0.1231(2) 0.24831(15) 0.14602(17) 0.0459(8) Uani 1 1 d . . . H51 H 0.0695 0.2188 0.1211 0.055 Uiso 1 1 calc R . . C52 C 0.2364(2) 0.24990(13) 0.13376(14) 0.0324(6) Uani 1 1 d . . . H52 H 0.2575 0.2209 0.1012 0.039 Uiso 1 1 calc R . . Cl1 Cl 0.75392(5) 0.30586(2) 0.21278(3) 0.02037(12) Uani 1 1 d . . . N1 N 0.51871(16) 0.04144(8) 0.36567(9) 0.0169(4) Uani 1 1 d . . . N2 N 0.61362(16) 0.03300(8) 0.28434(9) 0.0166(4) Uani 1 1 d . . . P1 P 0.46985(5) 0.15144(2) 0.26007(3) 0.01446(12) Uani 1 1 d . . . P2 P 0.47222(5) 0.29153(3) 0.16094(3) 0.01642(12) Uani 1 1 d . . . Ru1 Ru 0.600325(15) 0.224260(8) 0.236137(8) 0.01295(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0151(11) 0.0124(8) 0.0160(11) -0.0009(8) 0.0018(9) -0.0027(7) C2 0.0277(14) 0.0191(10) 0.0271(14) 0.0090(9) 0.0066(11) 0.0049(9) C3 0.0262(13) 0.0152(9) 0.0281(14) 0.0045(9) 0.0053(11) 0.0056(9) C4 0.0186(12) 0.0168(9) 0.0145(11) 0.0052(8) 0.0041(9) 0.0011(8) C5 0.0176(12) 0.0208(9) 0.0167(12) 0.0047(8) 0.0017(10) -0.0033(8) C6 0.0279(13) 0.0210(10) 0.0133(12) 0.0012(9) 0.0021(10) -0.0019(9) C7 0.0282(14) 0.0241(10) 0.0180(12) 0.0054(9) 0.0094(11) 0.0005(9) C8 0.0177(13) 0.0291(11) 0.0251(14) 0.0037(10) 0.0058(11) -0.0060(9) C9 0.0242(13) 0.0194(9) 0.0185(12) 0.0030(9) 0.0044(10) -0.0048(9) C10 0.0215(13) 0.0336(12) 0.0284(14) -0.0031(11) 0.0032(11) -0.0087(10) C11 0.0361(17) 0.0489(15) 0.0380(17) -0.0072(13) 0.0197(14) -0.0006(12) C12 0.0326(15) 0.0274(11) 0.0334(15) -0.0059(10) 0.0090(13) -0.0115(10) C13 0.0166(12) 0.0173(9) 0.0174(12) 0.0012(8) 0.0052(10) 0.0055(8) C14 0.0229(13) 0.0192(10) 0.0239(13) -0.0025(9) 0.0015(11) 0.0052(9) C15 0.0324(15) 0.0291(11) 0.0175(13) -0.0075(9) 0.0054(11) 0.0067(10) C16 0.0275(14) 0.0329(11) 0.0176(13) 0.0033(10) 0.0075(11) 0.0085(10) C17 0.0191(12) 0.0220(10) 0.0223(13) 0.0042(9) 0.0049(10) 0.0028(9) C18 0.0129(11) 0.0178(9) 0.0180(12) 0.0027(8) 0.0021(9) 0.0055(8) C19 0.0397(16) 0.0220(11) 0.0305(15) -0.0066(10) 0.0036(13) -0.0012(10) C20 0.0452(18) 0.0517(15) 0.0277(16) 0.0003(12) 0.0193(14) 0.0046(13) C21 0.0132(11) 0.0178(9) 0.0168(12) 0.0018(8) 0.0021(9) 0.0011(8) C22 0.0188(12) 0.0204(10) 0.0218(13) 0.0048(9) -0.0022(10) -0.0025(8) C23 0.0242(14) 0.0278(11) 0.0241(14) 0.0006(10) -0.0007(11) -0.0034(9) C24 0.0431(19) 0.0512(16) 0.0300(16) -0.0113(13) -0.0018(14) -0.0080(13) C25 0.046(2) 0.072(2) 0.047(2) -0.0167(17) -0.0100(17) -0.0283(17) C26 0.0332(18) 0.079(2) 0.052(2) -0.0072(18) 0.0028(16) -0.0313(16) C27 0.0279(15) 0.0475(15) 0.0322(16) 0.0029(12) 0.0061(13) -0.0136(12) C28 0.0224(12) 0.0150(9) 0.0138(11) 0.0035(8) 0.0043(9) 0.0014(8) C29 0.0283(14) 0.0248(10) 0.0186(13) 0.0002(9) 0.0056(11) -0.0056(9) C30 0.0483(18) 0.0312(12) 0.0232(14) -0.0083(10) 0.0094(13) -0.0127(11) C31 0.056(2) 0.0291(12) 0.0299(15) -0.0099(11) 0.0246(15) -0.0035(12) C32 0.0371(15) 0.0222(10) 0.0308(15) 0.0018(10) 0.0205(13) 0.0016(10) C33 0.0241(13) 0.0157(9) 0.0213(13) 0.0037(8) 0.0079(10) 0.0038(8) C34 0.0187(12) 0.0169(9) 0.0226(13) 0.0060(8) 0.0088(10) 0.0036(8) C35 0.0198(12) 0.0171(9) 0.0211(12) 0.0023(8) 0.0006(10) -0.0043(8) C36 0.0249(13) 0.0207(10) 0.0253(13) 0.0039(9) 0.0009(11) 0.0016(9) C37 0.0450(18) 0.0264(12) 0.0325(16) -0.0041(11) 0.0083(14) 0.0051(11) C38 0.0504(19) 0.0362(13) 0.0209(14) -0.0066(11) 0.0001(13) -0.0038(12) C39 0.0377(16) 0.0402(14) 0.0223(14) 0.0021(11) -0.0092(12) 0.0006(12) C40 0.0221(13) 0.0307(11) 0.0258(14) 0.0009(10) -0.0033(11) 0.0021(10) C41 0.0137(11) 0.0160(9) 0.0237(13) 0.0036(8) 0.0033(10) 0.0031(8) C42 0.0189(12) 0.0212(10) 0.0253(13) 0.0039(9) 0.0047(10) 0.0027(9) C43 0.0243(14) 0.0239(11) 0.0330(15) 0.0119(10) 0.0045(12) 0.0002(9) C44 0.0220(14) 0.0188(10) 0.0439(17) 0.0028(10) 0.0013(12) -0.0017(9) C45 0.0250(14) 0.0255(11) 0.0340(15) -0.0069(10) 0.0008(12) -0.0007(10) C46 0.0217(13) 0.0242(10) 0.0242(13) 0.0030(9) 0.0013(11) -0.0001(9) C47 0.0176(12) 0.0235(10) 0.0318(14) 0.0158(10) 0.0040(11) 0.0038(9) C48 0.0288(15) 0.0281(11) 0.0384(16) 0.0159(11) 0.0131(13) 0.0101(10) C49 0.0369(18) 0.0420(14) 0.061(2) 0.0254(14) 0.0293(17) 0.0182(13) C50 0.0235(16) 0.0581(18) 0.086(3) 0.0385(18) 0.0236(18) 0.0109(14) C51 0.0195(15) 0.0524(16) 0.063(2) 0.0268(16) -0.0012(15) -0.0049(12) C52 0.0195(14) 0.0361(12) 0.0398(17) 0.0159(12) 0.0002(12) -0.0004(10) Cl1 0.0185(3) 0.0187(2) 0.0253(3) 0.0036(2) 0.0077(2) -0.00224(19) N1 0.0179(10) 0.0158(7) 0.0177(10) 0.0036(7) 0.0052(8) 0.0001(7) N2 0.0192(10) 0.0137(7) 0.0176(10) 0.0007(7) 0.0049(8) 0.0015(7) P1 0.0140(3) 0.0144(2) 0.0152(3) 0.0026(2) 0.0031(2) 0.00016(19) P2 0.0149(3) 0.0165(2) 0.0177(3) 0.0043(2) 0.0026(2) 0.0008(2) Ru1 0.01261(9) 0.01375(7) 0.01275(9) 0.00217(6) 0.00289(6) -0.00004(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.352(3) . ? C1 N2 1.355(2) . ? C1 P1 1.883(2) . ? C2 C3 1.345(3) . ? C2 N1 1.391(3) . ? C3 N2 1.384(3) . ? C4 C5 1.390(3) . ? C4 C9 1.397(3) . ? C4 N1 1.456(3) . ? C5 C6 1.396(3) . ? C5 C10 1.506(3) . ? C6 C7 1.391(3) . ? C7 C8 1.392(3) . ? C7 C11 1.507(3) . ? C8 C9 1.398(3) . ? C9 C12 1.505(3) . ? C13 C14 1.386(3) . ? C13 C18 1.418(3) . ? C13 N2 1.454(3) . ? C14 C15 1.404(3) . ? C14 C19 1.510(3) . ? C15 C16 1.385(3) . ? C16 C17 1.396(3) . ? C16 C20 1.517(3) . ? C17 C18 1.414(3) . ? C18 C21 1.466(3) . ? C21 Ru1 2.157(2) . ? C22 C23 1.393(3) . ? C22 C27 1.401(3) . ? C22 P1 1.842(2) . ? C23 C24 1.391(4) . ? C24 C25 1.382(4) . ? C25 C26 1.385(4) . ? C26 C27 1.389(4) . ? C28 C29 1.407(3) . ? C28 C33 1.426(3) . ? C28 Ru1 2.035(2) . ? C29 C30 1.391(3) . ? C30 C31 1.393(4) . ? C31 C32 1.387(4) . ? C32 C33 1.400(3) . ? C33 C34 1.513(3) . ? C34 P1 1.839(2) . ? C35 C36 1.397(3) . ? C35 C40 1.400(3) . ? C35 P2 1.842(2) . ? C36 C37 1.392(3) . ? C37 C38 1.381(4) . ? C38 C39 1.385(4) . ? C39 C40 1.388(3) . ? C41 C42 1.394(3) . ? C41 C46 1.400(3) . ? C41 P2 1.857(2) . ? C42 C43 1.401(3) . ? C43 C44 1.375(4) . ? C44 C45 1.389(3) . ? C45 C46 1.394(3) . ? C47 C52 1.397(4) . ? C47 C48 1.399(3) . ? C47 P2 1.859(2) . ? C48 C49 1.400(4) . ? C49 C50 1.384(5) . ? C50 C51 1.377(5) . ? C51 C52 1.400(4) . ? Cl1 Ru1 2.4899(7) . ? P1 Ru1 2.1843(6) . ? P2 Ru1 2.3464(7) . ? 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 N1 C1 N2 105.98(17) . . ? N1 C1 P1 134.54(15) . . ? N2 C1 P1 119.48(15) . . ? C3 C2 N1 107.53(19) . . ? C2 C3 N2 106.70(18) . . ? C5 C4 C9 123.54(19) . . ? C5 C4 N1 117.68(19) . . ? C9 C4 N1 118.76(19) . . ? C4 C5 C6 116.9(2) . . ? C4 C5 C10 122.79(19) . . ? C6 C5 C10 120.3(2) . . ? C7 C6 C5 122.1(2) . . ? C6 C7 C8 118.4(2) . . ? C6 C7 C11 120.5(2) . . ? C8 C7 C11 121.1(2) . . ? C7 C8 C9 122.0(2) . . ? C4 C9 C8 116.7(2) . . ? C4 C9 C12 122.1(2) . . ? C8 C9 C12 121.3(2) . . ? C14 C13 C18 124.64(19) . . ? C14 C13 N2 118.96(18) . . ? C18 C13 N2 116.37(18) . . ? C13 C14 C15 116.9(2) . . ? C13 C14 C19 122.2(2) . . ? C15 C14 C19 120.9(2) . . ? C16 C15 C14 121.7(2) . . ? C15 C16 C17 119.5(2) . . ? C15 C16 C20 121.0(2) . . ? C17 C16 C20 119.5(2) . . ? C16 C17 C18 122.0(2) . . ? C17 C18 C13 115.21(19) . . ? C17 C18 C21 122.00(18) . . ? C13 C18 C21 122.65(18) . . ? C18 C21 Ru1 89.78(13) . . ? C23 C22 C27 119.0(2) . . ? C23 C22 P1 118.83(17) . . ? C27 C22 P1 122.16(19) . . ? C24 C23 C22 120.3(2) . . ? C25 C24 C23 120.4(3) . . ? C24 C25 C26 119.9(3) . . ? C25 C26 C27 120.2(3) . . ? C26 C27 C22 120.2(3) . . ? C29 C28 C33 116.41(19) . . ? C29 C28 Ru1 121.04(15) . . ? C33 C28 Ru1 122.51(16) . . ? C30 C29 C28 122.0(2) . . ? C29 C30 C31 120.5(2) . . ? C32 C31 C30 119.1(2) . . ? C31 C32 C33 120.8(2) . . ? C32 C33 C28 120.9(2) . . ? C32 C33 C34 120.84(19) . . ? C28 C33 C34 118.19(18) . . ? C33 C34 P1 104.70(14) . . ? C36 C35 C40 118.1(2) . . ? C36 C35 P2 118.84(18) . . ? C40 C35 P2 123.01(17) . . ? C37 C36 C35 120.6(2) . . ? C38 C37 C36 120.5(2) . . ? C37 C38 C39 119.5(2) . . ? C38 C39 C40 120.3(2) . . ? C39 C40 C35 120.8(2) . . ? C42 C41 C46 118.46(19) . . ? C42 C41 P2 124.54(17) . . ? C46 C41 P2 116.99(16) . . ? C41 C42 C43 120.2(2) . . ? C44 C43 C42 120.9(2) . . ? C43 C44 C45 119.4(2) . . ? C44 C45 C46 120.2(2) . . ? C45 C46 C41 120.7(2) . . ? C52 C47 C48 118.1(2) . . ? C52 C47 P2 121.95(19) . . ? C48 C47 P2 119.6(2) . . ? C47 C48 C49 120.5(3) . . ? C50 C49 C48 120.7(3) . . ? C51 C50 C49 119.3(3) . . ? C50 C51 C52 120.6(3) . . ? C47 C52 C51 120.8(3) . . ? C1 N1 C2 109.51(17) . . ? C1 N1 C4 126.63(16) . . ? C2 N1 C4 123.71(17) . . ? C1 N2 C3 110.28(17) . . ? C1 N2 C13 124.55(16) . . ? C3 N2 C13 124.78(17) . . ? C34 P1 C22 104.54(11) . . ? C34 P1 C1 107.02(9) . . ? C22 P1 C1 95.67(9) . . ? C34 P1 Ru1 107.87(7) . . ? C22 P1 Ru1 127.16(7) . . ? C1 P1 Ru1 112.77(7) . . ? C35 P2 C41 103.07(9) . . ? C35 P2 C47 102.37(11) . . ? C41 P2 C47 100.45(9) . . ? C35 P2 Ru1 112.97(7) . . ? C41 P2 Ru1 116.62(8) . . ? C47 P2 Ru1 119.07(7) . . ? C28 Ru1 C21 94.09(8) . . ? C28 Ru1 P1 80.52(6) . . ? C21 Ru1 P1 92.48(6) . . ? C28 Ru1 P2 95.53(6) . . ? C21 Ru1 P2 168.55(6) . . ? P1 Ru1 P2 95.21(3) . . ? C28 Ru1 Cl1 98.61(6) . . ? C21 Ru1 Cl1 85.58(6) . . ? P1 Ru1 Cl1 177.83(2) . . ? P2 Ru1 Cl1 86.85(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.42 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.374 _refine_diff_density_min -0.363 _refine_diff_density_rms 0.070 _database_code_depnum_ccdc_archive 'CCDC 945574'