####################################################################### # # 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_1 _database_code_depnum_ccdc_archive 'CCDC 771363' #Adrian Mena-Cruz,Pablo Lorenzo-Luis,Vincenzo Passarelli,Antonio Romerosa,Manuel Serrano-Ruiz _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H52 Cl N3 Ni O5 P2 Ru' _chemical_formula_weight 912.02 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' Ni Ni 0.3393 1.1124 '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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.2303(7) _cell_length_b 35.554(2) _cell_length_c 9.9058(6) _cell_angle_alpha 90.00 _cell_angle_beta 106.9850(10) _cell_angle_gamma 90.00 _cell_volume 4119.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 1902 _cell_measurement_theta_min 4.583 _cell_measurement_theta_max 46.938 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.203 _exptl_crystal_size_mid 0.077 _exptl_crystal_size_min 0.035 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.470 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 1.012 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 21573 _diffrn_reflns_av_R_equivalents 0.0886 _diffrn_reflns_av_sigmaI/netI 0.1002 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 24.44 _reflns_number_total 6775 _reflns_number_gt 5442 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker APEX' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0443P)^2^+7.7196P] 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 6775 _refine_ls_number_parameters 492 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1039 _refine_ls_R_factor_gt 0.0793 _refine_ls_wR_factor_ref 0.1725 _refine_ls_wR_factor_gt 0.1635 _refine_ls_goodness_of_fit_ref 1.233 _refine_ls_restrained_S_all 1.233 _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 0.58175(5) 0.171541(17) 0.68593(7) 0.02373(19) Uani 1 1 d . . . Ni1 Ni 0.29972(8) 0.08406(3) 0.22132(11) 0.0268(3) Uani 1 1 d . . . Cl1 Cl 0.61166(17) 0.23602(5) 0.6199(2) 0.0331(5) Uani 1 1 d . . . P2 P 0.48415(17) 0.15855(5) 0.4561(2) 0.0230(5) Uani 1 1 d . . . P1 P 0.76492(17) 0.15816(5) 0.6787(2) 0.0264(5) Uani 1 1 d . . . O4 O 0.2217(5) 0.09947(15) 0.0200(6) 0.0347(14) Uani 1 1 d . . . O3 O 0.3402(5) 0.03322(15) 0.1501(7) 0.0404(15) Uani 1 1 d . . . O2 O 0.1529(5) 0.06003(15) 0.2399(6) 0.0397(15) Uani 1 1 d . . . O1 O 0.3798(5) 0.06529(16) 0.4191(6) 0.0392(15) Uani 1 1 d . . . N1 N 0.4574(5) 0.11193(17) 0.2161(6) 0.0255(15) Uani 1 1 d . . . N2 N 0.2584(5) 0.13952(18) 0.2888(6) 0.0277(15) Uani 1 1 d . . . N3 N 0.3832(5) 0.17707(16) 0.1848(7) 0.0278(15) Uani 1 1 d . . . C31 C 0.8166(7) 0.1126(2) 0.7628(8) 0.0288(18) Uani 1 1 d . . . C36 C 0.7540(7) 0.0803(2) 0.7082(9) 0.035(2) Uani 1 1 d . . . H36 H 0.6894 0.0825 0.6272 0.042 Uiso 1 1 calc R . . C35 C 0.7836(8) 0.0457(2) 0.7689(10) 0.043(2) Uani 1 1 d . . . H35 H 0.7409 0.0239 0.7301 0.051 Uiso 1 1 calc R . . C34 C 0.8780(8) 0.0431(2) 0.8891(11) 0.047(3) Uani 1 1 d . . . H34 H 0.9002 0.0193 0.9321 0.057 Uiso 1 1 calc R . . C33 C 0.9383(7) 0.0746(3) 0.9450(10) 0.045(2) Uani 1 1 d . . . H33 H 1.0015 0.0727 1.0276 0.054 Uiso 1 1 calc R . . C32 C 0.9076(7) 0.1093(2) 0.8819(9) 0.034(2) Uani 1 1 d . . . H32 H 0.9501 0.1310 0.9216 0.041 Uiso 1 1 calc R . . C21 C 0.8775(7) 0.1900(2) 0.7738(9) 0.031(2) Uani 1 1 d . . . C26 C 0.8639(8) 0.2128(2) 0.8829(11) 0.047(3) Uani 1 1 d . . . H26 H 0.7920 0.2134 0.9014 0.056 Uiso 1 1 calc R . . C25 C 0.9539(9) 0.2345(3) 0.9652(12) 0.067(3) Uani 1 1 d . . . H25 H 0.9436 0.2493 1.0404 0.080 Uiso 1 1 calc R . . C24 C 1.0568(9) 0.2344(3) 0.9372(13) 0.065(3) Uani 1 1 d . . . H24 H 1.1175 0.2495 0.9929 0.078 Uiso 1 1 calc R . . C23 C 1.0740(8) 0.2129(3) 0.8294(12) 0.053(3) Uani 1 1 d . . . H23 H 1.1457 0.2131 0.8101 0.064 Uiso 1 1 calc R . . C22 C 0.9846(7) 0.1906(2) 0.7493(10) 0.040(2) Uani 1 1 d . . . H22 H 0.9966 0.1754 0.6760 0.047 Uiso 1 1 calc R . . C11 C 0.7992(6) 0.1551(2) 0.5093(9) 0.0312(19) Uani 1 1 d . . . C16 C 0.8491(7) 0.1237(2) 0.4670(10) 0.039(2) Uani 1 1 d . . . H16 H 0.8677 0.1024 0.5271 0.047 Uiso 1 1 calc R . . C15 C 0.8717(8) 0.1234(3) 0.3396(11) 0.051(3) Uani 1 1 d . . . H15 H 0.9064 0.1019 0.3123 0.061 Uiso 1 1 calc R . . C14 C 0.8444(7) 0.1541(3) 0.2502(10) 0.045(2) Uani 1 1 d . . . H14 H 0.8573 0.1534 0.1602 0.054 Uiso 1 1 calc R . . C13 C 0.7982(7) 0.1859(2) 0.2930(9) 0.038(2) Uani 1 1 d . . . H13 H 0.7834 0.2075 0.2343 0.045 Uiso 1 1 calc R . . C12 C 0.7732(7) 0.1863(2) 0.4209(9) 0.034(2) Uani 1 1 d . . . H12 H 0.7386 0.2078 0.4480 0.041 Uiso 1 1 calc R . . C51 C 0.5196(9) 0.1917(3) 0.8606(10) 0.050(3) Uani 1 1 d . . . H51 H 0.5157 0.2176 0.8816 0.060 Uiso 1 1 calc R . . C55 C 0.4335(8) 0.1711(3) 0.7709(9) 0.046(2) Uani 1 1 d . . . H55 H 0.3597 0.1802 0.7207 0.055 Uiso 1 1 calc R . . C54 C 0.4748(9) 0.1340(3) 0.7667(10) 0.047(3) Uani 1 1 d . . . H54 H 0.4334 0.1137 0.7132 0.057 Uiso 1 1 calc R . . C53 C 0.5862(10) 0.1325(3) 0.8543(11) 0.056(3) Uani 1 1 d . . . H53 H 0.6349 0.1111 0.8696 0.067 Uiso 1 1 calc R . . C52 C 0.6148(10) 0.1682(4) 0.9167(10) 0.067(3) Uani 1 1 d . . . H52 H 0.6848 0.1750 0.9838 0.080 Uiso 1 1 calc R . . C43 C 0.4594(7) 0.1935(2) 0.3145(8) 0.0302(19) Uani 1 1 d . . . H43A H 0.4241 0.2163 0.3409 0.036 Uiso 1 1 calc R . . H43B H 0.5330 0.2007 0.2990 0.036 Uiso 1 1 calc R . . C41 C 0.5317(6) 0.1200(2) 0.3630(8) 0.0225(17) Uani 1 1 d . . . H41A H 0.6096 0.1260 0.3582 0.027 Uiso 1 1 calc R . . H41B H 0.5373 0.0969 0.4200 0.027 Uiso 1 1 calc R . . C42 C 0.3308(6) 0.1489(2) 0.4334(8) 0.0285(19) Uani 1 1 d . . . H42A H 0.3259 0.1278 0.4965 0.034 Uiso 1 1 calc R . . H42B H 0.2975 0.1713 0.4660 0.034 Uiso 1 1 calc R . . C46 C 0.2689(7) 0.1698(2) 0.1903(9) 0.0310(19) Uani 1 1 d . . . H46A H 0.2210 0.1630 0.0942 0.037 Uiso 1 1 calc R . . H46B H 0.2376 0.1933 0.2178 0.037 Uiso 1 1 calc R . . C47 C 0.4372(7) 0.1468(2) 0.1316(8) 0.0282(18) Uani 1 1 d . . . H47A H 0.5117 0.1559 0.1240 0.034 Uiso 1 1 calc R . . H47B H 0.3892 0.1406 0.0351 0.034 Uiso 1 1 calc R . . C44 C 0.5218(7) 0.0859(2) 0.1514(9) 0.033(2) Uani 1 1 d . . . H44A H 0.4758 0.0797 0.0552 0.050 Uiso 1 1 calc R . . H44B H 0.5392 0.0628 0.2076 0.050 Uiso 1 1 calc R . . H44C H 0.5933 0.0978 0.1486 0.050 Uiso 1 1 calc R . . C45 C 0.1384(7) 0.1401(2) 0.2927(10) 0.041(2) Uani 1 1 d . . . H45A H 0.1192 0.1654 0.3181 0.061 Uiso 1 1 calc R . . H45B H 0.1289 0.1220 0.3630 0.061 Uiso 1 1 calc R . . H45C H 0.0876 0.1333 0.1995 0.061 Uiso 1 1 calc R . . C75 C 0.1570(9) 0.0991(3) -0.2276(9) 0.058(3) Uani 1 1 d . . . H75A H 0.1870 0.1247 -0.2272 0.088 Uiso 1 1 calc R . . H75B H 0.0743 0.1002 -0.2425 0.088 Uiso 1 1 calc R . . H75C H 0.1730 0.0846 -0.3038 0.088 Uiso 1 1 calc R . . C74 C 0.2133(7) 0.0806(2) -0.0890(9) 0.032(2) Uani 1 1 d . . . C73 C 0.2506(7) 0.0440(2) -0.0937(9) 0.041(2) Uani 1 1 d . . . H73 H 0.2329 0.0324 -0.1839 0.049 Uiso 1 1 calc R . . C72 C 0.3119(7) 0.0226(2) 0.0219(10) 0.037(2) Uani 1 1 d . . . C71 C 0.3520(9) -0.0167(2) -0.0035(12) 0.056(3) Uani 1 1 d . . . H71A H 0.3940 -0.0281 0.0869 0.084 Uiso 1 1 calc R . . H71B H 0.4021 -0.0150 -0.0645 0.084 Uiso 1 1 calc R . . H71C H 0.2855 -0.0324 -0.0494 0.084 Uiso 1 1 calc R . . C65 C 0.0217(8) 0.0239(3) 0.3205(12) 0.060(3) Uani 1 1 d . . . H65A H -0.0106 0.0349 0.3913 0.091 Uiso 1 1 calc R . . H65B H 0.0270 -0.0034 0.3325 0.091 Uiso 1 1 calc R . . H65C H -0.0278 0.0300 0.2258 0.091 Uiso 1 1 calc R . . C64 C 0.1412(8) 0.0402(2) 0.3393(10) 0.041(2) Uani 1 1 d . . . C63 C 0.2287(8) 0.0320(3) 0.4618(10) 0.048(3) Uani 1 1 d . . . H63 H 0.2088 0.0172 0.5311 0.058 Uiso 1 1 calc R . . C62 C 0.3412(8) 0.0431(2) 0.4920(9) 0.037(2) Uani 1 1 d . . . C61 C 0.4280(9) 0.0288(3) 0.6270(10) 0.055(3) Uani 1 1 d . . . H61A H 0.4672 0.0066 0.6049 0.083 Uiso 1 1 calc R . . H61B H 0.3882 0.0220 0.6962 0.083 Uiso 1 1 calc R . . H61C H 0.4842 0.0485 0.6661 0.083 Uiso 1 1 calc R . . O1W O 0.3398(6) 0.2484(2) 0.5364(9) 0.062(2) Uani 1 1 d . . . H2W H 0.338(10) 0.272(3) 0.563(13) 0.10(5) Uiso 1 1 d . . . H1W H 0.405(9) 0.237(3) 0.569(11) 0.07(4) 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 0.0274(4) 0.0241(3) 0.0182(4) -0.0005(3) 0.0043(3) -0.0002(3) Ni1 0.0276(6) 0.0259(5) 0.0236(6) 0.0015(4) 0.0021(5) -0.0030(4) Cl1 0.0363(12) 0.0222(9) 0.0378(12) -0.0008(9) 0.0063(10) 0.0003(8) P2 0.0248(11) 0.0224(10) 0.0206(11) -0.0008(9) 0.0051(9) 0.0007(8) P1 0.0259(11) 0.0239(10) 0.0245(12) 0.0024(9) -0.0004(9) -0.0016(9) O4 0.038(3) 0.037(3) 0.022(3) -0.002(3) -0.002(3) -0.001(3) O3 0.037(4) 0.028(3) 0.054(4) -0.004(3) 0.009(3) -0.006(3) O2 0.030(3) 0.040(3) 0.042(4) 0.011(3) -0.001(3) -0.004(3) O1 0.044(4) 0.042(3) 0.027(3) 0.015(3) 0.002(3) -0.005(3) N1 0.027(4) 0.029(3) 0.019(4) -0.004(3) 0.005(3) 0.007(3) N2 0.025(4) 0.038(4) 0.017(4) -0.004(3) 0.001(3) -0.003(3) N3 0.031(4) 0.025(3) 0.023(4) 0.000(3) 0.000(3) -0.006(3) C31 0.033(5) 0.028(4) 0.024(4) 0.008(4) 0.006(4) 0.006(4) C36 0.035(5) 0.038(5) 0.027(5) 0.002(4) 0.000(4) 0.005(4) C35 0.047(6) 0.029(5) 0.048(6) 0.004(4) 0.007(5) 0.004(4) C34 0.043(6) 0.035(5) 0.063(7) 0.016(5) 0.013(5) 0.005(4) C33 0.030(5) 0.057(6) 0.038(6) 0.023(5) -0.007(4) 0.000(4) C32 0.023(4) 0.039(5) 0.034(5) 0.009(4) -0.001(4) -0.002(4) C21 0.032(5) 0.022(4) 0.030(5) 0.005(4) -0.006(4) 0.002(3) C26 0.030(5) 0.043(5) 0.054(7) -0.003(5) -0.010(5) 0.002(4) C25 0.053(7) 0.049(6) 0.071(8) -0.024(6) -0.025(6) 0.009(5) C24 0.037(6) 0.043(6) 0.083(9) 0.002(6) -0.032(6) -0.007(5) C23 0.031(5) 0.040(5) 0.074(8) 0.018(6) -0.007(5) -0.008(4) C22 0.039(5) 0.032(5) 0.038(6) 0.005(4) -0.003(4) -0.007(4) C11 0.016(4) 0.038(5) 0.036(5) -0.007(4) 0.001(4) -0.006(4) C16 0.032(5) 0.034(5) 0.051(6) 0.014(4) 0.015(5) 0.004(4) C15 0.038(6) 0.062(6) 0.054(7) 0.004(6) 0.016(5) 0.018(5) C14 0.036(5) 0.063(6) 0.038(6) -0.003(5) 0.016(4) 0.012(5) C13 0.038(5) 0.040(5) 0.033(5) 0.015(4) 0.006(4) 0.003(4) C12 0.021(4) 0.034(4) 0.044(6) 0.005(4) 0.005(4) 0.004(4) C51 0.076(8) 0.045(6) 0.038(6) -0.003(5) 0.033(6) -0.002(5) C55 0.050(6) 0.071(7) 0.024(5) 0.010(5) 0.020(5) 0.004(5) C54 0.062(7) 0.051(6) 0.031(5) -0.002(5) 0.016(5) -0.022(5) C53 0.083(8) 0.060(7) 0.037(6) 0.027(5) 0.037(6) 0.031(6) C52 0.060(7) 0.124(11) 0.013(5) 0.001(6) 0.004(5) -0.024(7) C43 0.029(5) 0.029(4) 0.029(5) 0.001(4) 0.002(4) 0.000(3) C41 0.019(4) 0.026(4) 0.021(4) -0.002(3) 0.004(3) -0.002(3) C42 0.030(5) 0.030(4) 0.028(5) -0.008(4) 0.013(4) -0.003(4) C46 0.029(5) 0.026(4) 0.032(5) 0.001(4) -0.001(4) 0.002(4) C47 0.034(5) 0.030(4) 0.021(4) -0.003(4) 0.007(4) -0.006(4) C44 0.033(5) 0.036(5) 0.032(5) -0.002(4) 0.009(4) 0.002(4) C45 0.025(5) 0.040(5) 0.054(6) -0.009(5) 0.006(4) -0.007(4) C75 0.069(7) 0.073(7) 0.025(5) 0.004(5) 0.002(5) 0.021(6) C74 0.027(5) 0.037(5) 0.029(5) -0.002(4) 0.001(4) -0.003(4) C73 0.046(6) 0.044(5) 0.028(5) -0.016(4) 0.003(4) -0.001(4) C72 0.035(5) 0.029(4) 0.047(6) -0.012(4) 0.011(5) -0.011(4) C71 0.060(7) 0.033(5) 0.077(8) -0.010(5) 0.021(6) 0.007(5) C65 0.055(7) 0.052(6) 0.078(8) 0.009(6) 0.026(6) -0.013(5) C64 0.052(6) 0.035(5) 0.038(6) 0.000(4) 0.017(5) -0.002(4) C63 0.057(7) 0.049(6) 0.044(6) 0.018(5) 0.023(5) -0.002(5) C62 0.044(6) 0.037(5) 0.027(5) 0.000(4) 0.006(4) 0.007(4) C61 0.068(7) 0.051(6) 0.038(6) 0.026(5) 0.002(5) 0.006(5) O1W 0.039(4) 0.054(5) 0.084(6) -0.030(4) 0.007(4) 0.011(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C53 2.159(9) . ? Ru1 C54 2.178(9) . ? Ru1 C51 2.202(9) . ? Ru1 C52 2.206(9) . ? Ru1 C55 2.211(9) . ? Ru1 P2 2.288(2) . ? Ru1 P1 2.312(2) . ? Ru1 Cl1 2.4410(19) . ? Ni1 O4 2.019(5) . ? Ni1 O1 2.030(6) . ? Ni1 O2 2.044(6) . ? Ni1 O3 2.053(6) . ? Ni1 N1 2.182(6) . ? Ni1 N2 2.188(6) . ? P2 C43 1.831(8) . ? P2 C41 1.837(7) . ? P2 C42 1.854(8) . ? P1 C21 1.819(8) . ? P1 C31 1.846(7) . ? P1 C11 1.848(9) . ? O4 C74 1.250(9) . ? O3 C72 1.272(10) . ? O2 C64 1.252(10) . ? O1 C62 1.250(10) . ? N1 C47 1.476(9) . ? N1 C44 1.479(9) . ? N1 C41 1.501(9) . ? N2 C45 1.480(10) . ? N2 C46 1.483(9) . ? N2 C42 1.485(9) . ? N3 C46 1.438(10) . ? N3 C47 1.441(9) . ? N3 C43 1.470(9) . ? C31 C32 1.370(11) . ? C31 C36 1.398(11) . ? C36 C35 1.374(11) . ? C35 C34 1.398(13) . ? C34 C33 1.366(12) . ? C33 C32 1.384(11) . ? C21 C26 1.398(12) . ? C21 C22 1.399(12) . ? C26 C25 1.397(13) . ? C25 C24 1.365(15) . ? C24 C23 1.380(14) . ? C23 C22 1.395(12) . ? C11 C12 1.390(11) . ? C11 C16 1.394(11) . ? C16 C15 1.369(12) . ? C15 C14 1.383(13) . ? C14 C13 1.384(12) . ? C13 C12 1.388(11) . ? C51 C55 1.373(13) . ? C51 C52 1.408(15) . ? C55 C54 1.419(13) . ? C54 C53 1.385(14) . ? C53 C52 1.410(15) . ? C75 C74 1.497(12) . ? C74 C73 1.384(11) . ? C73 C72 1.397(12) . ? C72 C71 1.526(11) . ? C65 C64 1.533(12) . ? C64 C63 1.395(13) . ? C63 C62 1.379(12) . ? C62 C61 1.532(12) . ? 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 C53 Ru1 C54 37.3(4) . . ? C53 Ru1 C51 62.5(4) . . ? C54 Ru1 C51 61.9(4) . . ? C53 Ru1 C52 37.7(4) . . ? C54 Ru1 C52 62.2(4) . . ? C51 Ru1 C52 37.3(4) . . ? C53 Ru1 C55 62.6(4) . . ? C54 Ru1 C55 37.7(3) . . ? C51 Ru1 C55 36.3(3) . . ? C52 Ru1 C55 61.8(4) . . ? C53 Ru1 P2 121.8(3) . . ? C54 Ru1 P2 92.7(3) . . ? C51 Ru1 P2 130.4(3) . . ? C52 Ru1 P2 154.8(3) . . ? C55 Ru1 P2 97.5(3) . . ? C53 Ru1 P1 94.9(3) . . ? C54 Ru1 P1 125.2(3) . . ? C51 Ru1 P1 130.6(3) . . ? C52 Ru1 P1 97.8(3) . . ? C55 Ru1 P1 157.0(3) . . ? P2 Ru1 P1 98.99(8) . . ? C53 Ru1 Cl1 147.1(3) . . ? C54 Ru1 Cl1 145.8(3) . . ? C51 Ru1 Cl1 91.1(3) . . ? C52 Ru1 Cl1 109.4(3) . . ? C55 Ru1 Cl1 108.2(3) . . ? P2 Ru1 Cl1 89.90(7) . . ? P1 Ru1 Cl1 87.85(7) . . ? O4 Ni1 O1 176.4(2) . . ? O4 Ni1 O2 91.6(2) . . ? O1 Ni1 O2 88.0(2) . . ? O4 Ni1 O3 89.5(2) . . ? O1 Ni1 O3 86.9(2) . . ? O2 Ni1 O3 88.2(2) . . ? O4 Ni1 N1 91.1(2) . . ? O1 Ni1 N1 89.5(2) . . ? O2 Ni1 N1 175.7(2) . . ? O3 Ni1 N1 95.1(2) . . ? O4 Ni1 N2 88.4(2) . . ? O1 Ni1 N2 95.2(2) . . ? O2 Ni1 N2 93.6(2) . . ? O3 Ni1 N2 177.3(2) . . ? N1 Ni1 N2 83.2(2) . . ? C43 P2 C41 97.3(4) . . ? C43 P2 C42 95.6(4) . . ? C41 P2 C42 105.0(3) . . ? C43 P2 Ru1 123.1(3) . . ? C41 P2 Ru1 120.0(2) . . ? C42 P2 Ru1 111.9(3) . . ? C21 P1 C31 101.8(4) . . ? C21 P1 C11 99.7(4) . . ? C31 P1 C11 102.6(4) . . ? C21 P1 Ru1 116.7(3) . . ? C31 P1 Ru1 112.0(3) . . ? C11 P1 Ru1 121.3(3) . . ? C74 O4 Ni1 127.1(5) . . ? C72 O3 Ni1 125.6(6) . . ? C64 O2 Ni1 127.7(6) . . ? C62 O1 Ni1 127.4(6) . . ? C47 N1 C44 107.6(6) . . ? C47 N1 C41 110.0(6) . . ? C44 N1 C41 107.0(6) . . ? C47 N1 Ni1 113.1(5) . . ? C44 N1 Ni1 108.2(5) . . ? C41 N1 Ni1 110.7(4) . . ? C45 N2 C46 106.5(6) . . ? C45 N2 C42 106.8(6) . . ? C46 N2 C42 109.3(6) . . ? C45 N2 Ni1 109.8(5) . . ? C46 N2 Ni1 112.4(5) . . ? C42 N2 Ni1 111.8(5) . . ? C46 N3 C47 115.7(6) . . ? C46 N3 C43 114.5(6) . . ? C47 N3 C43 112.0(6) . . ? C32 C31 C36 118.5(7) . . ? C32 C31 P1 123.3(6) . . ? C36 C31 P1 117.9(6) . . ? C35 C36 C31 121.5(8) . . ? C36 C35 C34 118.6(8) . . ? C33 C34 C35 120.3(8) . . ? C34 C33 C32 120.3(8) . . ? C31 C32 C33 120.7(8) . . ? C26 C21 C22 117.0(8) . . ? C26 C21 P1 121.1(7) . . ? C22 C21 P1 121.6(7) . . ? C25 C26 C21 121.3(10) . . ? C24 C25 C26 119.8(11) . . ? C25 C24 C23 121.1(9) . . ? C24 C23 C22 118.9(10) . . ? C23 C22 C21 121.8(9) . . ? C12 C11 C16 119.2(8) . . ? C12 C11 P1 117.0(6) . . ? C16 C11 P1 123.8(7) . . ? C15 C16 C11 120.5(8) . . ? C16 C15 C14 120.5(9) . . ? C15 C14 C13 119.5(9) . . ? C14 C13 C12 120.4(8) . . ? C13 C12 C11 119.7(8) . . ? C55 C51 C52 109.2(9) . . ? C55 C51 Ru1 72.2(5) . . ? C52 C51 Ru1 71.5(5) . . ? C51 C55 C54 107.5(9) . . ? C51 C55 Ru1 71.6(5) . . ? C54 C55 Ru1 69.9(5) . . ? C53 C54 C55 108.2(9) . . ? C53 C54 Ru1 70.6(5) . . ? C55 C54 Ru1 72.4(5) . . ? C54 C53 C52 108.2(9) . . ? C54 C53 Ru1 72.1(5) . . ? C52 C53 Ru1 72.9(5) . . ? C51 C52 C53 106.9(9) . . ? C51 C52 Ru1 71.3(5) . . ? C53 C52 Ru1 69.4(5) . . ? N3 C43 P2 108.7(5) . . ? N1 C41 P2 116.0(5) . . ? N2 C42 P2 117.1(5) . . ? N3 C46 N2 115.3(6) . . ? N3 C47 N1 116.0(6) . . ? O4 C74 C73 126.1(8) . . ? O4 C74 C75 117.1(7) . . ? C73 C74 C75 116.8(8) . . ? C74 C73 C72 126.1(8) . . ? O3 C72 C73 125.5(8) . . ? O3 C72 C71 115.5(9) . . ? C73 C72 C71 119.1(8) . . ? O2 C64 C63 124.6(9) . . ? O2 C64 C65 116.2(9) . . ? C63 C64 C65 119.1(8) . . ? C62 C63 C64 126.2(9) . . ? O1 C62 C63 125.3(8) . . ? O1 C62 C61 115.5(8) . . ? C63 C62 C61 119.1(8) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 24.44 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.605 _refine_diff_density_min -0.712 _refine_diff_density_rms 0.113 data_c:\sir2004\adrian\adruzn_241110\adruzns _database_code_depnum_ccdc_archive 'CCDC 771364' #TrackingRef 'adruzns-P21c-ffffff.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H52 Cl N3 O5 P2 Ru Zn' _chemical_formula_weight 918.68 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' Zn Zn 0.2839 1.4301 '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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.2069(14) _cell_length_b 35.572(4) _cell_length_c 9.9461(12) _cell_angle_alpha 90.00 _cell_angle_beta 107.068(2) _cell_angle_gamma 90.00 _cell_volume 4128.6(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2908 _cell_measurement_theta_min 4.580 _cell_measurement_theta_max 47.097 _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.552 _exptl_crystal_size_mid 0.381 _exptl_crystal_size_min 0.085 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.478 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1896 _exptl_absorpt_coefficient_mu 1.135 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6725 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _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 22298 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_sigmaI/netI 0.0526 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 25.09 _reflns_number_total 7309 _reflns_number_gt 6530 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker APEX' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0530P)^2^+46.1999P] 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 7309 _refine_ls_number_parameters 491 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0834 _refine_ls_R_factor_gt 0.0773 _refine_ls_wR_factor_ref 0.1984 _refine_ls_wR_factor_gt 0.1954 _refine_ls_goodness_of_fit_ref 1.204 _refine_ls_restrained_S_all 1.204 _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 0.91670(5) 0.171687(17) 0.31041(6) 0.02082(19) Uani 1 1 d . . . Zn1 Zn 1.20215(8) 0.08328(3) 0.77904(9) 0.0258(2) Uani 1 1 d . . . Cl1 Cl 0.88394(17) 0.23627(5) 0.3743(2) 0.0285(4) Uani 1 1 d . . . P1 P 0.73241(17) 0.15787(6) 0.3167(2) 0.0226(4) Uani 1 1 d . . . P2 P 1.01459(16) 0.15921(6) 0.54066(19) 0.0202(4) Uani 1 1 d . . . O1 O 1.1189(5) 0.06399(18) 0.5761(6) 0.0364(14) Uani 1 1 d . . . O2 O 1.3510(5) 0.06017(18) 0.7514(6) 0.0365(14) Uani 1 1 d . . . O3 O 1.1634(5) 0.03212(16) 0.8586(6) 0.0345(14) Uani 1 1 d . . . O4 O 1.2802(5) 0.09943(16) 0.9835(6) 0.0304(13) Uani 1 1 d . . . O1W O 0.1561(6) 0.2518(2) 0.9608(8) 0.0486(18) Uani 1 1 d D . . H1W1 H 0.086(4) 0.263(2) 0.929(11) 0.058 Uiso 1 1 d D . . H1W2 H 0.145(7) 0.2261(7) 0.948(11) 0.05(3) Uiso 1 1 d D . . N1 N 1.0397(5) 0.11247(18) 0.7793(6) 0.0231(14) Uani 1 1 d . . . N2 N 1.2409(5) 0.14158(19) 0.7097(6) 0.0247(14) Uani 1 1 d . . . N3 N 1.1109(5) 0.17799(19) 0.8116(6) 0.0253(14) Uani 1 1 d . . . C11 C 0.6979(6) 0.1546(2) 0.4853(8) 0.0242(16) Uani 1 1 d . . . C12 C 0.7225(7) 0.1859(2) 0.5735(8) 0.0278(17) Uani 1 1 d . . . H12 H 0.7557 0.2076 0.5456 0.033 Uiso 1 1 calc R . . C13 C 0.6989(7) 0.1856(3) 0.7024(9) 0.0315(19) Uani 1 1 d . . . H13 H 0.7146 0.2072 0.7611 0.038 Uiso 1 1 calc R . . C14 C 0.6523(7) 0.1537(3) 0.7450(9) 0.037(2) Uani 1 1 d . . . H14 H 0.6378 0.1533 0.8337 0.045 Uiso 1 1 calc R . . C15 C 0.6270(7) 0.1224(3) 0.6580(9) 0.036(2) Uani 1 1 d . . . H15 H 0.5949 0.1007 0.6871 0.043 Uiso 1 1 calc R . . C16 C 0.6488(7) 0.1229(2) 0.5267(9) 0.0306(18) Uani 1 1 d . . . H16 H 0.6301 0.1016 0.4663 0.037 Uiso 1 1 calc R . . C21 C 0.6180(7) 0.1903(2) 0.2190(8) 0.0288(18) Uani 1 1 d . . . C22 C 0.5124(7) 0.1910(3) 0.2468(10) 0.035(2) Uani 1 1 d . . . H22 H 0.5013 0.1763 0.3214 0.042 Uiso 1 1 calc R . . C23 C 0.4223(8) 0.2134(3) 0.1653(10) 0.041(2) Uani 1 1 d . . . H23 H 0.3505 0.2138 0.1844 0.050 Uiso 1 1 calc R . . C24 C 0.4392(8) 0.2350(3) 0.0560(11) 0.045(2) Uani 1 1 d . . . H24 H 0.3787 0.2501 0.0002 0.054 Uiso 1 1 calc R . . C25 C 0.5434(9) 0.2344(3) 0.0291(10) 0.046(2) Uani 1 1 d . . . H25 H 0.5548 0.2489 -0.0459 0.055 Uiso 1 1 calc R . . C26 C 0.6317(8) 0.2126(3) 0.1117(10) 0.038(2) Uani 1 1 d . . . H26 H 0.7040 0.2131 0.0938 0.046 Uiso 1 1 calc R . . C31 C 0.6832(7) 0.1123(2) 0.2334(8) 0.0250(16) Uani 1 1 d . . . C32 C 0.5895(7) 0.1088(2) 0.1136(8) 0.0286(18) Uani 1 1 d . . . H32 H 0.5457 0.1303 0.0749 0.034 Uiso 1 1 calc R . . C33 C 0.5596(7) 0.0737(3) 0.0501(9) 0.037(2) Uani 1 1 d . . . H33 H 0.4965 0.0715 -0.0326 0.045 Uiso 1 1 calc R . . C34 C 0.6222(7) 0.0422(3) 0.1080(10) 0.038(2) Uani 1 1 d . . . H34 H 0.6014 0.0182 0.0658 0.046 Uiso 1 1 calc R . . C35 C 0.7160(8) 0.0454(3) 0.2284(10) 0.037(2) Uani 1 1 d . . . H35 H 0.7589 0.0238 0.2687 0.044 Uiso 1 1 calc R . . C36 C 0.7452(7) 0.0802(2) 0.2874(8) 0.0285(18) Uani 1 1 d . . . H36 H 0.8101 0.0824 0.3680 0.034 Uiso 1 1 calc R . . C41 C 0.9658(6) 0.1208(2) 0.6345(7) 0.0225(16) Uani 1 1 d . . . H41A H 0.8883 0.1272 0.6398 0.027 Uiso 1 1 calc R . . H41B H 0.9589 0.0977 0.5776 0.027 Uiso 1 1 calc R . . C42 C 1.1688(6) 0.1501(2) 0.5650(8) 0.0253(17) Uani 1 1 d . . . H42A H 1.1748 0.1287 0.5039 0.030 Uiso 1 1 calc R . . H42B H 1.2015 0.1724 0.5312 0.030 Uiso 1 1 calc R . . C43 C 1.0372(7) 0.1945(2) 0.6806(7) 0.0250(16) Uani 1 1 d . . . H43A H 1.0743 0.2171 0.6555 0.030 Uiso 1 1 calc R . . H43B H 0.9628 0.2021 0.6932 0.030 Uiso 1 1 calc R . . C44 C 0.9741(7) 0.0863(2) 0.8431(9) 0.0307(18) Uani 1 1 d . . . H44A H 1.0208 0.0795 0.9381 0.046 Uiso 1 1 calc R . . H44B H 0.9548 0.0636 0.7853 0.046 Uiso 1 1 calc R . . H44C H 0.9035 0.0986 0.8479 0.046 Uiso 1 1 calc R . . C45 C 1.3627(7) 0.1426(3) 0.7100(10) 0.036(2) Uani 1 1 d . . . H45A H 1.3735 0.1256 0.6374 0.055 Uiso 1 1 calc R . . H45B H 1.4120 0.1347 0.8022 0.055 Uiso 1 1 calc R . . H45C H 1.3830 0.1683 0.6904 0.055 Uiso 1 1 calc R . . C46 C 1.2273(7) 0.1716(2) 0.8094(8) 0.0260(17) Uani 1 1 d . . . H46A H 1.2742 0.1647 0.9055 0.031 Uiso 1 1 calc R . . H46B H 1.2581 0.1954 0.7841 0.031 Uiso 1 1 calc R . . C47 C 1.0582(7) 0.1474(2) 0.8646(8) 0.0284(18) Uani 1 1 d . . . H47A H 0.9832 0.1561 0.8722 0.034 Uiso 1 1 calc R . . H47B H 1.1068 0.1413 0.9607 0.034 Uiso 1 1 calc R . . C51 C 0.9793(9) 0.1919(3) 0.1339(9) 0.041(2) Uani 1 1 d . . . H51 H 0.9831 0.2177 0.1112 0.049 Uiso 1 1 calc R . . C52 C 0.8847(9) 0.1683(3) 0.0785(9) 0.049(3) Uani 1 1 d . . . H52 H 0.8146 0.1750 0.0110 0.058 Uiso 1 1 calc R . . C53 C 0.9131(9) 0.1323(3) 0.1424(9) 0.043(2) Uani 1 1 d . . . H53 H 0.8643 0.1109 0.1280 0.052 Uiso 1 1 calc R . . C54 C 1.0270(8) 0.1342(3) 0.2312(9) 0.036(2) Uani 1 1 d . . . H54 H 1.0697 0.1140 0.2843 0.043 Uiso 1 1 calc R . . C55 C 1.0663(8) 0.1717(3) 0.2267(9) 0.038(2) Uani 1 1 d . . . H55 H 1.1392 0.1813 0.2782 0.046 Uiso 1 1 calc R . . C61 C 1.0704(8) 0.0266(3) 0.3709(9) 0.042(2) Uani 1 1 d . . . H61A H 0.9930 0.0305 0.3787 0.063 Uiso 1 1 calc R . . H61B H 1.0832 -0.0003 0.3604 0.063 Uiso 1 1 calc R . . H61C H 1.0785 0.0402 0.2885 0.063 Uiso 1 1 calc R . . C62 C 1.1590(8) 0.0415(2) 0.5041(8) 0.0303(18) Uani 1 1 d . . . C63 C 1.2711(8) 0.0299(3) 0.5312(9) 0.035(2) Uani 1 1 d . . . H63 H 1.2897 0.0147 0.4624 0.042 Uiso 1 1 calc R . . C64 C 1.3603(8) 0.0390(2) 0.6531(10) 0.036(2) Uani 1 1 d . . . C65 C 1.4797(9) 0.0227(3) 0.6732(12) 0.048(2) Uani 1 1 d . . . H65A H 1.5037 0.0277 0.5892 0.072 Uiso 1 1 calc R . . H65B H 1.4780 -0.0045 0.6883 0.072 Uiso 1 1 calc R . . H65C H 1.5339 0.0345 0.7551 0.072 Uiso 1 1 calc R . . C71 C 1.1513(9) -0.0166(3) 1.0166(11) 0.045(2) Uani 1 1 d . . . H71A H 1.1134 -0.0294 0.9277 0.067 Uiso 1 1 calc R . . H71B H 1.0976 -0.0143 1.0725 0.067 Uiso 1 1 calc R . . H71C H 1.2182 -0.0313 1.0691 0.067 Uiso 1 1 calc R . . C72 C 1.1897(7) 0.0222(2) 0.9863(9) 0.0329(19) Uani 1 1 d . . . C73 C 1.2493(7) 0.0446(3) 1.1002(9) 0.035(2) Uani 1 1 d . . . H73 H 1.2662 0.0334 1.1908 0.042 Uiso 1 1 calc R . . C74 C 1.2862(7) 0.0810(3) 1.0949(8) 0.0319(19) Uani 1 1 d . . . C75 C 1.3400(8) 0.1018(3) 1.2315(9) 0.044(2) Uani 1 1 d . . . H75A H 1.4235 0.1020 1.2511 0.066 Uiso 1 1 calc R . . H75B H 1.3198 0.0891 1.3084 0.066 Uiso 1 1 calc R . . H75C H 1.3114 0.1277 1.2232 0.066 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 0.0193(3) 0.0323(4) 0.0115(3) 0.0001(2) 0.0054(2) -0.0001(2) Zn1 0.0226(5) 0.0367(5) 0.0173(4) -0.0021(4) 0.0046(4) 0.0039(4) Cl1 0.0265(10) 0.0318(10) 0.0260(10) -0.0002(8) 0.0059(8) -0.0001(8) P1 0.0187(10) 0.0321(11) 0.0152(9) -0.0001(8) 0.0020(8) -0.0002(8) P2 0.0177(9) 0.0320(11) 0.0116(9) -0.0001(7) 0.0054(7) -0.0002(8) O1 0.030(3) 0.050(4) 0.022(3) -0.014(3) -0.003(3) 0.004(3) O2 0.026(3) 0.053(4) 0.026(3) -0.008(3) 0.001(3) 0.011(3) O3 0.037(3) 0.033(3) 0.032(3) 0.001(2) 0.007(3) 0.003(3) O4 0.025(3) 0.045(3) 0.018(3) -0.002(2) 0.001(2) 0.001(2) O1W 0.032(4) 0.053(5) 0.058(5) -0.017(4) 0.008(3) 0.005(3) N1 0.022(3) 0.035(4) 0.014(3) 0.003(3) 0.009(3) 0.000(3) N2 0.014(3) 0.043(4) 0.015(3) 0.002(3) 0.002(2) 0.002(3) N3 0.017(3) 0.038(4) 0.014(3) -0.001(3) -0.005(3) 0.004(3) C11 0.018(4) 0.037(4) 0.018(4) 0.002(3) 0.007(3) 0.005(3) C12 0.019(4) 0.038(5) 0.024(4) 0.002(3) 0.001(3) -0.001(3) C13 0.018(4) 0.049(5) 0.026(4) -0.005(4) 0.003(3) -0.001(4) C14 0.028(5) 0.062(6) 0.027(4) -0.001(4) 0.017(4) -0.006(4) C15 0.025(4) 0.052(6) 0.034(5) 0.002(4) 0.014(4) -0.011(4) C16 0.019(4) 0.039(5) 0.033(5) -0.004(4) 0.006(3) -0.005(3) C21 0.024(4) 0.032(4) 0.025(4) -0.003(3) -0.001(3) 0.001(3) C22 0.026(4) 0.041(5) 0.033(5) -0.007(4) -0.001(4) 0.003(4) C23 0.021(4) 0.054(6) 0.044(5) -0.009(4) 0.001(4) 0.005(4) C24 0.031(5) 0.039(5) 0.055(6) -0.001(4) -0.006(4) 0.003(4) C25 0.043(6) 0.049(6) 0.035(5) 0.012(4) -0.007(4) -0.003(4) C26 0.022(4) 0.048(5) 0.036(5) 0.010(4) -0.006(4) -0.001(4) C31 0.023(4) 0.034(4) 0.020(4) -0.003(3) 0.010(3) -0.005(3) C32 0.019(4) 0.044(5) 0.023(4) -0.004(3) 0.006(3) 0.002(3) C33 0.021(4) 0.062(6) 0.026(4) -0.014(4) 0.002(4) 0.000(4) C34 0.024(4) 0.041(5) 0.049(6) -0.016(4) 0.011(4) -0.009(4) C35 0.038(5) 0.034(5) 0.042(5) 0.002(4) 0.016(4) 0.002(4) C36 0.024(4) 0.040(5) 0.019(4) 0.000(3) 0.002(3) -0.001(3) C41 0.022(4) 0.038(4) 0.009(3) -0.001(3) 0.007(3) 0.002(3) C42 0.016(4) 0.041(5) 0.020(4) 0.003(3) 0.007(3) 0.001(3) C43 0.028(4) 0.035(4) 0.012(3) -0.001(3) 0.005(3) 0.001(3) C44 0.024(4) 0.043(5) 0.028(4) 0.008(4) 0.012(4) 0.000(4) C45 0.019(4) 0.054(6) 0.037(5) 0.007(4) 0.009(4) 0.004(4) C46 0.022(4) 0.036(4) 0.018(4) 0.001(3) 0.004(3) 0.000(3) C47 0.030(4) 0.035(5) 0.020(4) -0.001(3) 0.008(3) 0.004(3) C51 0.069(7) 0.049(6) 0.018(4) 0.008(4) 0.033(5) 0.003(5) C52 0.045(6) 0.086(8) 0.015(4) -0.003(5) 0.010(4) 0.013(5) C53 0.047(6) 0.061(6) 0.030(5) -0.024(4) 0.025(4) -0.021(5) C54 0.043(5) 0.050(6) 0.020(4) 0.003(4) 0.019(4) 0.017(4) C55 0.036(5) 0.062(6) 0.028(5) -0.010(4) 0.025(4) -0.003(4) C61 0.040(5) 0.061(6) 0.023(4) -0.011(4) 0.005(4) -0.003(4) C62 0.040(5) 0.036(5) 0.016(4) -0.001(3) 0.008(4) -0.004(4) C63 0.036(5) 0.056(6) 0.021(4) -0.007(4) 0.020(4) 0.001(4) C64 0.039(5) 0.033(5) 0.037(5) 0.000(4) 0.015(4) 0.004(4) C65 0.044(6) 0.056(6) 0.052(6) -0.005(5) 0.025(5) 0.006(5) C71 0.044(6) 0.044(6) 0.047(6) 0.005(4) 0.015(5) -0.003(4) C72 0.025(4) 0.040(5) 0.034(5) 0.004(4) 0.009(4) 0.006(4) C73 0.033(5) 0.053(6) 0.020(4) 0.009(4) 0.005(4) -0.002(4) C74 0.033(5) 0.047(5) 0.015(4) 0.001(3) 0.007(3) 0.006(4) C75 0.037(5) 0.067(7) 0.022(4) -0.002(4) -0.002(4) -0.014(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 C53 2.172(8) . ? Ru1 C54 2.199(8) . ? Ru1 C55 2.218(8) . ? Ru1 C52 2.227(9) . ? Ru1 C51 2.230(8) . ? Ru1 P2 2.2941(19) . ? Ru1 P1 2.321(2) . ? Ru1 Cl1 2.448(2) . ? Zn1 O4 2.058(5) . ? Zn1 O2 2.085(6) . ? Zn1 O1 2.091(5) . ? Zn1 O3 2.093(6) . ? Zn1 N1 2.239(6) . ? Zn1 N2 2.279(7) . ? P1 C31 1.839(8) . ? P1 C11 1.849(8) . ? P1 C21 1.852(8) . ? P2 C43 1.834(8) . ? P2 C41 1.848(8) . ? P2 C42 1.855(8) . ? O1 C62 1.264(10) . ? O2 C64 1.266(10) . ? O3 C72 1.265(10) . ? O4 C74 1.271(10) . ? O1W H1W1 0.92(2) . ? O1W H1W2 0.93(2) . ? N1 C47 1.484(10) . ? N1 C44 1.486(10) . ? N1 C41 1.488(9) . ? N2 C42 1.481(9) . ? N2 C45 1.486(10) . ? N2 C46 1.499(10) . ? N3 C47 1.440(11) . ? N3 C46 1.446(10) . ? N3 C43 1.471(9) . ? C11 C12 1.395(11) . ? C11 C16 1.395(11) . ? C12 C13 1.394(12) . ? C12 H12 0.9500 . ? C13 C14 1.389(13) . ? C13 H13 0.9500 . ? C14 C15 1.388(13) . ? C14 H14 0.9500 . ? C15 C16 1.407(12) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C21 C26 1.379(12) . ? C21 C22 1.396(12) . ? C22 C23 1.405(12) . ? C22 H22 0.9500 . ? C23 C24 1.395(15) . ? C23 H23 0.9500 . ? C24 C25 1.374(15) . ? C24 H24 0.9500 . ? C25 C26 1.384(12) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C31 C36 1.388(11) . ? C31 C32 1.394(11) . ? C32 C33 1.397(12) . ? C32 H32 0.9500 . ? C33 C34 1.385(13) . ? C33 H33 0.9500 . ? C34 C35 1.397(13) . ? C34 H34 0.9500 . ? C35 C36 1.374(12) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C51 C55 1.385(14) . ? C51 C52 1.404(15) . ? C51 H51 0.9500 . ? C52 C53 1.426(15) . ? C52 H52 0.9500 . ? C53 C54 1.413(13) . ? C53 H53 0.9500 . ? C54 C55 1.425(13) . ? C54 H54 0.9500 . ? C55 H55 0.9500 . ? C61 C62 1.537(11) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 C63 1.378(12) . ? C63 C64 1.409(13) . ? C63 H63 0.9500 . ? C64 C65 1.525(13) . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C71 C72 1.517(13) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 C73 1.402(13) . ? C73 C74 1.379(13) . ? C73 H73 0.9500 . ? C74 C75 1.516(12) . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? 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 C53 Ru1 C54 37.7(4) . . ? C53 Ru1 C55 62.9(3) . . ? C54 Ru1 C55 37.6(3) . . ? C53 Ru1 C52 37.8(4) . . ? C54 Ru1 C52 62.3(3) . . ? C55 Ru1 C52 61.6(4) . . ? C53 Ru1 C51 62.4(4) . . ? C54 Ru1 C51 61.7(3) . . ? C55 Ru1 C51 36.3(4) . . ? C52 Ru1 C51 36.7(4) . . ? C53 Ru1 P2 122.0(3) . . ? C54 Ru1 P2 92.6(2) . . ? C55 Ru1 P2 97.5(3) . . ? C52 Ru1 P2 154.8(3) . . ? C51 Ru1 P2 130.5(3) . . ? C53 Ru1 P1 94.8(3) . . ? C54 Ru1 P1 125.5(3) . . ? C55 Ru1 P1 157.1(2) . . ? C52 Ru1 P1 98.0(3) . . ? C51 Ru1 P1 130.4(3) . . ? P2 Ru1 P1 99.04(7) . . ? C53 Ru1 Cl1 146.9(3) . . ? C54 Ru1 Cl1 145.7(3) . . ? C55 Ru1 Cl1 108.2(3) . . ? C52 Ru1 Cl1 109.1(3) . . ? C51 Ru1 Cl1 91.3(3) . . ? P2 Ru1 Cl1 89.96(7) . . ? P1 Ru1 Cl1 87.61(7) . . ? O4 Zn1 O2 94.1(2) . . ? O4 Zn1 O1 176.5(3) . . ? O2 Zn1 O1 86.5(2) . . ? O4 Zn1 O3 87.7(2) . . ? O2 Zn1 O3 90.5(2) . . ? O1 Zn1 O3 88.8(2) . . ? O4 Zn1 N1 91.3(2) . . ? O2 Zn1 N1 171.7(2) . . ? O1 Zn1 N1 88.5(2) . . ? O3 Zn1 N1 96.0(2) . . ? O4 Zn1 N2 88.2(2) . . ? O2 Zn1 N2 93.0(2) . . ? O1 Zn1 N2 95.3(2) . . ? O3 Zn1 N2 174.7(2) . . ? N1 Zn1 N2 80.9(2) . . ? C31 P1 C11 102.8(4) . . ? C31 P1 C21 102.5(4) . . ? C11 P1 C21 100.2(4) . . ? C31 P1 Ru1 111.4(3) . . ? C11 P1 Ru1 121.2(3) . . ? C21 P1 Ru1 116.2(3) . . ? C43 P2 C41 96.9(3) . . ? C43 P2 C42 95.7(4) . . ? C41 P2 C42 105.6(4) . . ? C43 P2 Ru1 122.9(3) . . ? C41 P2 Ru1 119.8(2) . . ? C42 P2 Ru1 112.1(2) . . ? C62 O1 Zn1 126.5(5) . . ? C64 O2 Zn1 128.0(6) . . ? C72 O3 Zn1 127.1(6) . . ? C74 O4 Zn1 127.5(6) . . ? H1W1 O1W H1W2 107(4) . . ? C47 N1 C44 106.9(6) . . ? C47 N1 C41 109.4(6) . . ? C44 N1 C41 106.8(6) . . ? C47 N1 Zn1 113.7(5) . . ? C44 N1 Zn1 107.4(5) . . ? C41 N1 Zn1 112.2(4) . . ? C42 N2 C45 107.8(6) . . ? C42 N2 C46 110.3(6) . . ? C45 N2 C46 106.6(6) . . ? C42 N2 Zn1 111.3(5) . . ? C45 N2 Zn1 108.6(5) . . ? C46 N2 Zn1 112.0(5) . . ? C47 N3 C46 115.6(6) . . ? C47 N3 C43 113.8(6) . . ? C46 N3 C43 113.4(6) . . ? C12 C11 C16 119.5(7) . . ? C12 C11 P1 117.1(6) . . ? C16 C11 P1 123.4(6) . . ? C13 C12 C11 120.5(8) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C14 C13 C12 120.0(8) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C15 C14 C13 120.1(8) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 120.1(8) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C11 C16 C15 119.8(8) . . ? C11 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C26 C21 C22 118.1(8) . . ? C26 C21 P1 121.4(7) . . ? C22 C21 P1 120.4(7) . . ? C21 C22 C23 120.5(9) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C24 C23 C22 119.4(9) . . ? C24 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? C25 C24 C23 120.0(9) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 119.8(10) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C21 C26 C25 122.1(9) . . ? C21 C26 H26 119.0 . . ? C25 C26 H26 119.0 . . ? C36 C31 C32 118.3(7) . . ? C36 C31 P1 118.8(6) . . ? C32 C31 P1 122.9(6) . . ? C31 C32 C33 120.5(8) . . ? C31 C32 H32 119.8 . . ? C33 C32 H32 119.8 . . ? C34 C33 C32 119.7(8) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C33 C34 C35 120.3(8) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C36 C35 C34 119.0(8) . . ? C36 C35 H35 120.5 . . ? C34 C35 H35 120.5 . . ? C35 C36 C31 122.2(8) . . ? C35 C36 H36 118.9 . . ? C31 C36 H36 118.9 . . ? N1 C41 P2 116.3(5) . . ? N1 C41 H41A 108.2 . . ? P2 C41 H41A 108.2 . . ? N1 C41 H41B 108.2 . . ? P2 C41 H41B 108.2 . . ? H41A C41 H41B 107.4 . . ? N2 C42 P2 117.0(5) . . ? N2 C42 H42A 108.0 . . ? P2 C42 H42A 108.0 . . ? N2 C42 H42B 108.0 . . ? P2 C42 H42B 108.0 . . ? H42A C42 H42B 107.3 . . ? N3 C43 P2 108.4(5) . . ? N3 C43 H43A 110.0 . . ? P2 C43 H43A 110.0 . . ? N3 C43 H43B 110.0 . . ? P2 C43 H43B 110.0 . . ? H43A C43 H43B 108.4 . . ? N1 C44 H44A 109.5 . . ? N1 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? N1 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N2 C45 H45A 109.5 . . ? N2 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? N2 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N3 C46 N2 115.0(6) . . ? N3 C46 H46A 108.5 . . ? N2 C46 H46A 108.5 . . ? N3 C46 H46B 108.5 . . ? N2 C46 H46B 108.5 . . ? H46A C46 H46B 107.5 . . ? N3 C47 N1 115.7(6) . . ? N3 C47 H47A 108.4 . . ? N1 C47 H47A 108.4 . . ? N3 C47 H47B 108.4 . . ? N1 C47 H47B 108.4 . . ? H47A C47 H47B 107.4 . . ? C55 C51 C52 109.5(9) . . ? C55 C51 Ru1 71.4(5) . . ? C52 C51 Ru1 71.5(5) . . ? C55 C51 H51 125.3 . . ? C52 C51 H51 125.3 . . ? Ru1 C51 H51 123.4 . . ? C51 C52 C53 107.3(9) . . ? C51 C52 Ru1 71.8(5) . . ? C53 C52 Ru1 69.0(5) . . ? C51 C52 H52 126.3 . . ? C53 C52 H52 126.3 . . ? Ru1 C52 H52 124.5 . . ? C54 C53 C52 107.5(8) . . ? C54 C53 Ru1 72.2(5) . . ? C52 C53 Ru1 73.2(5) . . ? C54 C53 H53 126.2 . . ? C52 C53 H53 126.2 . . ? Ru1 C53 H53 120.2 . . ? C53 C54 C55 107.7(8) . . ? C53 C54 Ru1 70.1(5) . . ? C55 C54 Ru1 71.9(5) . . ? C53 C54 H54 126.1 . . ? C55 C54 H54 126.1 . . ? Ru1 C54 H54 123.5 . . ? C51 C55 C54 107.9(9) . . ? C51 C55 Ru1 72.3(5) . . ? C54 C55 Ru1 70.5(5) . . ? C51 C55 H55 126.1 . . ? C54 C55 H55 126.1 . . ? Ru1 C55 H55 122.8 . . ? C62 C61 H61A 109.5 . . ? C62 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C62 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? O1 C62 C63 127.3(8) . . ? O1 C62 C61 114.5(8) . . ? C63 C62 C61 118.2(8) . . ? C62 C63 C64 124.9(8) . . ? C62 C63 H63 117.5 . . ? C64 C63 H63 117.5 . . ? O2 C64 C63 125.4(8) . . ? O2 C64 C65 115.0(8) . . ? C63 C64 C65 119.6(8) . . ? C64 C65 H65A 109.5 . . ? C64 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C64 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C72 C71 H71A 109.5 . . ? C72 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C72 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? O3 C72 C73 124.9(8) . . ? O3 C72 C71 116.8(8) . . ? C73 C72 C71 118.3(8) . . ? C74 C73 C72 127.0(8) . . ? C74 C73 H73 116.5 . . ? C72 C73 H73 116.5 . . ? O4 C74 C73 125.6(8) . . ? O4 C74 C75 115.4(8) . . ? C73 C74 C75 119.0(8) . . ? C74 C75 H75A 109.5 . . ? C74 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C74 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.09 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.830 _refine_diff_density_min -1.040 _refine_diff_density_rms 0.150