# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_1b #========================================================================= _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H35 Cl2 N6 O2 P Ru' _chemical_formula_sum 'C23 H35 Cl2 N6 O2 P Ru' _chemical_formula_weight 630.51 _chemical_compound_source synthesis loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 11.7278(1) _cell_length_b 12.5536(1) _cell_length_c 18.5962(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2737.85(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11745 _cell_measurement_theta_min 3.5168 _cell_measurement_theta_max 73.6709 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.046 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 7.246 _exptl_absorpt_correction_T_min 0.87897 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET) (compiled Oct 24 2008,09:44:38) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ; 165 mm Onyx CCD detector in \k-geometry diffractometer ; _diffrn_measurement_device_type 'Xcalibur, Onyx, Nova' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.2640 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15044 _diffrn_reflns_av_R_equivalents 0.0429 _diffrn_reflns_av_unetI/netI 0.0333 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 4.25 _diffrn_reflns_theta_max 73.85 _reflns_number_total 5210 _reflns_number_gt 4986 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET) (compiled Oct 24 2008,09:44:38) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET) (compiled Oct 24 2008,09:44:38) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET) (compiled Oct 24 2008,09:44:38) ; _computing_structure_solution 'DIRDIF-2008 ( Beurskens, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2007)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999' _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^)+(0.0743P)^2^+0.6797P] 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 ? _chemical_absolute_configuration ad _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.020(11) _refine_ls_number_reflns 5210 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0384 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.1062 _refine_ls_wR_factor_gt 0.0998 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _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 C1 C 0.4022(4) 0.1361(4) 0.2587(3) 0.0494(11) Uani 1 1 d . . . H1A H 0.3400 0.1724 0.2828 0.059 Uiso 1 1 calc R . . H1B H 0.3970 0.0610 0.2703 0.059 Uiso 1 1 calc R . . C2 C 0.4322(5) 0.2930(4) 0.1515(3) 0.0517(12) Uani 1 1 d . . . H2A H 0.4469 0.3081 0.1012 0.062 Uiso 1 1 calc R . . H2B H 0.3706 0.3391 0.1671 0.062 Uiso 1 1 calc R . . C3 C 0.5279(4) 0.0951(5) 0.1354(3) 0.0531(11) Uani 1 1 d . . . H3A H 0.5262 0.0189 0.1437 0.064 Uiso 1 1 calc R . . H3B H 0.5413 0.1067 0.0845 0.064 Uiso 1 1 calc R . . C4 C 0.5250(5) 0.2910(5) 0.2685(4) 0.0617(14) Uani 1 1 d . . . H4A H 0.4600 0.3292 0.2879 0.074 Uiso 1 1 calc R . . H4B H 0.5923 0.3169 0.2933 0.074 Uiso 1 1 calc R . . C5 C 0.6083(5) 0.1230(5) 0.2534(4) 0.0624(14) Uani 1 1 d . . . H5A H 0.6773 0.1451 0.2780 0.075 Uiso 1 1 calc R . . H5B H 0.5993 0.0470 0.2612 0.075 Uiso 1 1 calc R . . C6 C 0.6327(5) 0.2563(5) 0.1650(3) 0.0595(13) Uani 1 1 d . . . H6A H 0.6390 0.2696 0.1138 0.071 Uiso 1 1 calc R . . H6B H 0.7024 0.2812 0.1875 0.071 Uiso 1 1 calc R . . C7 C 0.0747(7) 0.4056(6) 0.1918(4) 0.0808(12) Uani 1 1 d . . . H7A H 0.0587 0.3708 0.1470 0.121 Uiso 1 1 calc R . . H7B H 0.1192 0.4685 0.1830 0.121 Uiso 1 1 calc R . . H7C H 0.0044 0.4250 0.2148 0.121 Uiso 1 1 calc R . . C8 C 0.1545(7) 0.3773(5) 0.3145(4) 0.0808(12) Uani 1 1 d . . . H8A H 0.2025 0.3316 0.3428 0.121 Uiso 1 1 calc R . . H8B H 0.0811 0.3831 0.3370 0.121 Uiso 1 1 calc R . . H8C H 0.1886 0.4466 0.3111 0.121 Uiso 1 1 calc R . . C9 C 0.1408(7) 0.3309(5) 0.2401(4) 0.0808(12) Uani 1 1 d . . . H9 H 0.2173 0.3232 0.2196 0.097 Uiso 1 1 calc R . . C10 C 0.0900(4) 0.2212(4) 0.2451(3) 0.0442(10) Uani 1 1 d . . . H10 H 0.1324 0.1800 0.2810 0.053 Uiso 1 1 calc R . . C11 C -0.0396(4) 0.2166(5) 0.2637(3) 0.0549(13) Uani 1 1 d . . . H11A H -0.0533 0.1691 0.3039 0.066 Uiso 1 1 calc R . . H11B H -0.0682 0.2869 0.2758 0.066 Uiso 1 1 calc R . . C12 C -0.0095(4) 0.1450(4) 0.1553(3) 0.0411(9) Uani 1 1 d . . . C13 C -0.0306(4) 0.0892(3) 0.0881(3) 0.0407(9) Uani 1 1 d . . . C14 C -0.1326(5) 0.0655(4) 0.0544(3) 0.0515(12) Uani 1 1 d . . . H14 H -0.2018 0.0858 0.0745 0.062 Uiso 1 1 calc R . . C15 C -0.1288(5) 0.0109(4) -0.0099(3) 0.0588(15) Uani 1 1 d . . . H15 H -0.1966 -0.0061 -0.0331 0.071 Uiso 1 1 calc R . . C16 C -0.0281(5) -0.0185(4) -0.0398(3) 0.0526(12) Uani 1 1 d . . . H16 H -0.0265 -0.0553 -0.0832 0.063 Uiso 1 1 calc R . . C17 C 0.0729(5) 0.0076(4) -0.0044(3) 0.0475(11) Uani 1 1 d . . . C18 C 0.1893(5) -0.0132(4) -0.0236(3) 0.0501(11) Uani 1 1 d . . . C19 C 0.3413(7) -0.0612(8) -0.0883(4) 0.094(2) Uani 1 1 d . . . H19A H 0.3660 -0.0099 -0.1241 0.113 Uiso 1 1 calc R . . H19B H 0.3731 -0.1304 -0.1001 0.113 Uiso 1 1 calc R . . C20 C 0.3776(7) -0.0265(8) -0.0130(4) 0.094(2) Uani 1 1 d . . . H20 H 0.4359 0.0293 -0.0159 0.113 Uiso 1 1 calc R . . C21 C 0.4215(8) -0.1223(8) 0.0330(7) 0.119(2) Uani 1 1 d . . . H21 H 0.4289 -0.0967 0.0826 0.142 Uiso 1 1 calc R . . C22 C 0.3369(8) -0.2162(8) 0.0343(6) 0.119(2) Uani 1 1 d . . . H22A H 0.2630 -0.1910 0.0486 0.178 Uiso 1 1 calc R . . H22B H 0.3629 -0.2689 0.0679 0.178 Uiso 1 1 calc R . . H22C H 0.3321 -0.2471 -0.0128 0.178 Uiso 1 1 calc R . . C23 C 0.5409(8) -0.1503(9) 0.0069(6) 0.119(2) Uani 1 1 d . . . H23A H 0.5358 -0.1891 -0.0375 0.178 Uiso 1 1 calc R . . H23B H 0.5785 -0.1935 0.0423 0.178 Uiso 1 1 calc R . . H23C H 0.5838 -0.0861 -0.0006 0.178 Uiso 1 1 calc R . . Cl1 Cl 0.21187(14) 0.25882(9) 0.03523(7) 0.0593(3) Uani 1 1 d . . . Cl2 Cl 0.21392(11) -0.05507(8) 0.18198(7) 0.0514(3) Uani 1 1 d . . . N1 N 0.5112(4) 0.1781(4) 0.2859(2) 0.0560(11) Uani 1 1 d . . . N2 N 0.5357(4) 0.3182(3) 0.1938(3) 0.0536(10) Uani 1 1 d . . . N3 N 0.6224(3) 0.1421(4) 0.1767(3) 0.0567(11) Uani 1 1 d . . . N4 N 0.0945(3) 0.1644(3) 0.1752(2) 0.0359(7) Uani 1 1 d . . . N5 N 0.0689(3) 0.0593(3) 0.0591(2) 0.0390(8) Uani 1 1 d . . . N6 N 0.2727(4) 0.0158(3) 0.0181(2) 0.0493(9) Uani 1 1 d . . . O1 O -0.0950(3) 0.1763(3) 0.1982(2) 0.0577(9) Uani 1 1 d . . . O2 O 0.2179(5) -0.0661(5) -0.0847(2) 0.0837(15) Uani 1 1 d . . . P1 P 0.38611(9) 0.15314(8) 0.16019(6) 0.0353(2) Uani 1 1 d . . . Ru1 Ru 0.21705(2) 0.10098(2) 0.107066(15) 0.03191(10) 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 0.040(2) 0.065(3) 0.043(2) 0.005(2) -0.0061(19) -0.010(2) C2 0.049(3) 0.041(2) 0.065(3) 0.005(2) -0.006(2) -0.0067(19) C3 0.040(2) 0.058(2) 0.061(3) -0.013(2) -0.004(2) 0.002(2) C4 0.048(3) 0.067(3) 0.070(4) -0.020(3) -0.002(2) -0.010(2) C5 0.039(3) 0.068(3) 0.080(4) 0.009(3) -0.017(3) 0.000(2) C6 0.038(2) 0.073(3) 0.067(3) -0.001(3) -0.001(2) -0.017(2) C7 0.087(3) 0.0603(19) 0.095(3) -0.023(2) 0.013(2) -0.0014(19) C8 0.087(3) 0.0603(19) 0.095(3) -0.023(2) 0.013(2) -0.0014(19) C9 0.087(3) 0.0603(19) 0.095(3) -0.023(2) 0.013(2) -0.0014(19) C10 0.041(2) 0.048(2) 0.044(2) -0.0084(19) 0.0041(18) 0.0070(18) C11 0.035(2) 0.064(3) 0.066(3) -0.013(3) 0.014(2) 0.003(2) C12 0.034(2) 0.0392(18) 0.050(2) -0.0010(18) -0.0002(18) 0.0061(17) C13 0.0295(18) 0.0392(18) 0.054(2) 0.0077(18) -0.0058(17) 0.0017(16) C14 0.045(3) 0.044(2) 0.066(3) 0.012(2) -0.016(2) -0.0050(19) C15 0.053(3) 0.051(2) 0.072(4) 0.011(2) -0.032(3) -0.014(2) C16 0.058(3) 0.047(2) 0.052(3) 0.004(2) -0.016(2) -0.015(2) C17 0.064(3) 0.042(2) 0.036(2) -0.0004(18) -0.010(2) -0.011(2) C18 0.053(3) 0.061(3) 0.037(2) -0.015(2) 0.0045(19) -0.011(2) C19 0.081(4) 0.136(5) 0.066(3) -0.055(3) 0.026(3) -0.032(3) C20 0.081(4) 0.136(5) 0.066(3) -0.055(3) 0.026(3) -0.032(3) C21 0.076(3) 0.121(4) 0.159(5) -0.076(4) -0.021(3) 0.028(3) C22 0.076(3) 0.121(4) 0.159(5) -0.076(4) -0.021(3) 0.028(3) C23 0.076(3) 0.121(4) 0.159(5) -0.076(4) -0.021(3) 0.028(3) Cl1 0.0737(8) 0.0546(5) 0.0496(6) 0.0199(5) -0.0125(6) -0.0196(6) Cl2 0.0459(5) 0.0396(4) 0.0688(7) 0.0159(5) -0.0006(6) 0.0005(5) N1 0.050(2) 0.075(3) 0.043(2) 0.000(2) -0.0112(18) -0.009(2) N2 0.040(2) 0.052(2) 0.069(3) 0.001(2) -0.0065(19) -0.0148(18) N3 0.0290(19) 0.072(2) 0.069(3) -0.010(2) -0.0056(18) -0.0007(18) N4 0.0312(16) 0.0373(16) 0.0393(18) 0.0000(14) 0.0028(13) 0.0037(13) N5 0.0417(19) 0.0328(15) 0.0424(19) 0.0041(14) -0.0049(15) -0.0058(14) N6 0.050(2) 0.058(2) 0.0402(19) -0.0154(16) 0.0068(18) -0.0082(19) O1 0.0329(16) 0.069(2) 0.071(2) -0.0071(19) 0.0073(15) 0.0105(15) O2 0.078(3) 0.116(4) 0.057(2) -0.043(2) 0.010(2) -0.025(3) P1 0.0313(5) 0.0384(4) 0.0362(5) 0.0006(4) -0.0020(4) -0.0050(4) Ru1 0.03025(15) 0.03280(14) 0.03268(15) -0.00026(11) -0.00020(11) -0.00350(10) _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 1.472(6) . ? C1 P1 1.853(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.480(7) . ? C2 P1 1.844(5) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N3 1.472(6) . ? C3 P1 1.873(5) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 N2 1.437(8) . ? C4 N1 1.463(8) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N3 1.456(8) . ? C5 N1 1.463(8) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N3 1.455(8) . ? C6 N2 1.479(8) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C9 1.513(12) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C9 1.510(10) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.503(8) . ? C9 H9 0.9800 . ? C10 N4 1.483(6) . ? C10 C11 1.560(7) . ? C10 H10 0.9800 . ? C11 O1 1.470(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N4 1.298(6) . ? C12 O1 1.339(6) . ? C12 C13 1.455(7) . ? C13 N5 1.339(6) . ? C13 C14 1.383(6) . ? C14 C15 1.378(9) . ? C14 H14 0.9300 . ? C15 C16 1.356(9) . ? C15 H15 0.9300 . ? C16 C17 1.394(7) . ? C16 H16 0.9300 . ? C17 N5 1.349(6) . ? C17 C18 1.435(8) . ? C18 N6 1.300(7) . ? C18 O2 1.357(6) . ? C19 O2 1.451(9) . ? C19 C20 1.526(9) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 N6 1.460(9) . ? C20 C21 1.563(15) . ? C20 H20 0.9800 . ? C21 C23 1.524(13) . ? C21 C22 1.540(15) . ? C21 H21 0.9800 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? Cl1 Ru1 2.3905(11) . ? Cl2 Ru1 2.4041(10) . ? N4 Ru1 2.076(3) . ? N5 Ru1 2.022(4) . ? N6 Ru1 2.075(4) . ? P1 Ru1 2.3100(10) . ? 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 P1 112.8(3) . . ? N1 C1 H1A 109.0 . . ? P1 C1 H1A 109.0 . . ? N1 C1 H1B 109.0 . . ? P1 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? N2 C2 P1 113.4(4) . . ? N2 C2 H2A 108.9 . . ? P1 C2 H2A 108.9 . . ? N2 C2 H2B 108.9 . . ? P1 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? N3 C3 P1 112.6(4) . . ? N3 C3 H3A 109.1 . . ? P1 C3 H3A 109.1 . . ? N3 C3 H3B 109.1 . . ? P1 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? N2 C4 N1 117.0(5) . . ? N2 C4 H4A 108.1 . . ? N1 C4 H4A 108.1 . . ? N2 C4 H4B 108.1 . . ? N1 C4 H4B 108.1 . . ? H4A C4 H4B 107.3 . . ? N3 C5 N1 114.5(4) . . ? N3 C5 H5A 108.6 . . ? N1 C5 H5A 108.6 . . ? N3 C5 H5B 108.6 . . ? N1 C5 H5B 108.6 . . ? H5A C5 H5B 107.6 . . ? N3 C6 N2 113.6(4) . . ? N3 C6 H6A 108.9 . . ? N2 C6 H6A 108.9 . . ? N3 C6 H6B 108.9 . . ? N2 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? C9 C7 H7A 109.5 . . ? C9 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C9 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C9 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 C8 109.8(6) . . ? C10 C9 C7 113.7(7) . . ? C8 C9 C7 111.1(6) . . ? C10 C9 H9 107.3 . . ? C8 C9 H9 107.3 . . ? C7 C9 H9 107.3 . . ? N4 C10 C9 111.8(5) . . ? N4 C10 C11 102.1(4) . . ? C9 C10 C11 115.7(5) . . ? N4 C10 H10 109.0 . . ? C9 C10 H10 109.0 . . ? C11 C10 H10 109.0 . . ? O1 C11 C10 105.1(4) . . ? O1 C11 H11A 110.7 . . ? C10 C11 H11A 110.7 . . ? O1 C11 H11B 110.7 . . ? C10 C11 H11B 110.7 . . ? H11A C11 H11B 108.8 . . ? N4 C12 O1 118.6(4) . . ? N4 C12 C13 119.7(4) . . ? O1 C12 C13 121.7(4) . . ? N5 C13 C14 120.7(5) . . ? N5 C13 C12 109.5(4) . . ? C14 C13 C12 129.8(5) . . ? C15 C14 C13 118.2(5) . . ? C15 C14 H14 120.9 . . ? C13 C14 H14 120.9 . . ? C16 C15 C14 121.3(5) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C15 C16 C17 118.8(5) . . ? C15 C16 H16 120.6 . . ? C17 C16 H16 120.6 . . ? N5 C17 C16 119.8(5) . . ? N5 C17 C18 109.8(4) . . ? C16 C17 C18 130.4(5) . . ? N6 C18 O2 116.8(5) . . ? N6 C18 C17 121.1(4) . . ? O2 C18 C17 122.1(5) . . ? O2 C19 C20 104.3(5) . . ? O2 C19 H19A 110.9 . . ? C20 C19 H19A 110.9 . . ? O2 C19 H19B 110.9 . . ? C20 C19 H19B 110.9 . . ? H19A C19 H19B 108.9 . . ? N6 C20 C19 103.4(7) . . ? N6 C20 C21 109.9(7) . . ? C19 C20 C21 112.0(8) . . ? N6 C20 H20 110.5 . . ? C19 C20 H20 110.5 . . ? C21 C20 H20 110.5 . . ? C23 C21 C22 114.8(7) . . ? C23 C21 C20 107.8(10) . . ? C22 C21 C20 112.7(8) . . ? C23 C21 H21 107.0 . . ? C22 C21 H21 107.0 . . ? C20 C21 H21 107.0 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C5 N1 C4 106.3(5) . . ? C5 N1 C1 111.4(4) . . ? C4 N1 C1 111.5(5) . . ? C4 N2 C6 107.0(5) . . ? C4 N2 C2 113.1(4) . . ? C6 N2 C2 109.1(4) . . ? C5 N3 C6 108.6(5) . . ? C5 N3 C3 111.1(5) . . ? C6 N3 C3 112.3(5) . . ? C12 N4 C10 107.9(4) . . ? C12 N4 Ru1 113.9(3) . . ? C10 N4 Ru1 138.1(3) . . ? C13 N5 C17 121.2(4) . . ? C13 N5 Ru1 119.9(3) . . ? C17 N5 Ru1 118.7(3) . . ? C18 N6 C20 107.2(4) . . ? C18 N6 Ru1 112.6(3) . . ? C20 N6 Ru1 140.2(4) . . ? C12 O1 C11 105.3(4) . . ? C18 O2 C19 105.3(5) . . ? C2 P1 C1 99.6(3) . . ? C2 P1 C3 95.1(3) . . ? C1 P1 C3 96.2(3) . . ? C2 P1 Ru1 118.94(17) . . ? C1 P1 Ru1 118.51(16) . . ? C3 P1 Ru1 123.12(17) . . ? N5 Ru1 N6 77.58(17) . . ? N5 Ru1 N4 76.92(15) . . ? N6 Ru1 N4 154.47(16) . . ? N5 Ru1 P1 178.40(10) . . ? N6 Ru1 P1 102.55(13) . . ? N4 Ru1 P1 102.97(11) . . ? N5 Ru1 Cl1 86.92(10) . . ? N6 Ru1 Cl1 89.41(13) . . ? N4 Ru1 Cl1 90.32(10) . . ? P1 Ru1 Cl1 91.48(4) . . ? N5 Ru1 Cl2 91.80(10) . . ? N6 Ru1 Cl2 92.68(12) . . ? N4 Ru1 Cl2 87.04(10) . . ? P1 Ru1 Cl2 89.79(4) . . ? Cl1 Ru1 Cl2 177.27(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C8 C9 C10 N4 -169.5(6) . . . . ? C7 C9 C10 N4 65.4(7) . . . . ? C8 C9 C10 C11 74.1(8) . . . . ? C7 C9 C10 C11 -51.0(8) . . . . ? N4 C10 C11 O1 -9.6(5) . . . . ? C9 C10 C11 O1 112.1(6) . . . . ? N4 C12 C13 N5 4.6(6) . . . . ? O1 C12 C13 N5 -174.7(4) . . . . ? N4 C12 C13 C14 -175.9(5) . . . . ? O1 C12 C13 C14 4.9(8) . . . . ? N5 C13 C14 C15 -0.4(7) . . . . ? C12 C13 C14 C15 -179.9(5) . . . . ? C13 C14 C15 C16 -0.4(7) . . . . ? C14 C15 C16 C17 -0.1(8) . . . . ? C15 C16 C17 N5 1.3(7) . . . . ? C15 C16 C17 C18 -180.0(5) . . . . ? N5 C17 C18 N6 0.7(7) . . . . ? C16 C17 C18 N6 -178.2(5) . . . . ? N5 C17 C18 O2 178.8(5) . . . . ? C16 C17 C18 O2 0.0(9) . . . . ? O2 C19 C20 N6 -16.8(10) . . . . ? O2 C19 C20 C21 101.4(9) . . . . ? N6 C20 C21 C23 -169.8(6) . . . . ? C19 C20 C21 C23 75.8(8) . . . . ? N6 C20 C21 C22 62.4(9) . . . . ? C19 C20 C21 C22 -51.9(10) . . . . ? N3 C5 N1 C4 -54.6(6) . . . . ? N3 C5 N1 C1 67.0(6) . . . . ? N2 C4 N1 C5 55.7(6) . . . . ? N2 C4 N1 C1 -65.9(6) . . . . ? P1 C1 N1 C5 -61.1(5) . . . . ? P1 C1 N1 C4 57.5(6) . . . . ? N1 C4 N2 C6 -56.0(6) . . . . ? N1 C4 N2 C2 64.1(7) . . . . ? N3 C6 N2 C4 55.0(6) . . . . ? N3 C6 N2 C2 -67.6(6) . . . . ? P1 C2 N2 C4 -54.4(6) . . . . ? P1 C2 N2 C6 64.5(5) . . . . ? N1 C5 N3 C6 56.8(6) . . . . ? N1 C5 N3 C3 -67.1(6) . . . . ? N2 C6 N3 C5 -56.2(6) . . . . ? N2 C6 N3 C3 67.0(6) . . . . ? P1 C3 N3 C5 61.0(6) . . . . ? P1 C3 N3 C6 -60.7(6) . . . . ? O1 C12 N4 C10 -0.5(6) . . . . ? C13 C12 N4 C10 -179.8(4) . . . . ? O1 C12 N4 Ru1 175.5(3) . . . . ? C13 C12 N4 Ru1 -3.7(5) . . . . ? C9 C10 N4 C12 -117.9(5) . . . . ? C11 C10 N4 C12 6.5(5) . . . . ? C9 C10 N4 Ru1 67.5(6) . . . . ? C11 C10 N4 Ru1 -168.2(4) . . . . ? C14 C13 N5 C17 1.7(6) . . . . ? C12 C13 N5 C17 -178.7(4) . . . . ? C14 C13 N5 Ru1 177.1(3) . . . . ? C12 C13 N5 Ru1 -3.3(5) . . . . ? C16 C17 N5 C13 -2.1(7) . . . . ? C18 C17 N5 C13 178.9(4) . . . . ? C16 C17 N5 Ru1 -177.6(4) . . . . ? C18 C17 N5 Ru1 3.4(5) . . . . ? O2 C18 N6 C20 -4.0(8) . . . . ? C17 C18 N6 C20 174.3(6) . . . . ? O2 C18 N6 Ru1 177.7(4) . . . . ? C17 C18 N6 Ru1 -4.1(6) . . . . ? C19 C20 N6 C18 12.9(9) . . . . ? C21 C20 N6 C18 -106.8(6) . . . . ? C19 C20 N6 Ru1 -169.5(5) . . . . ? C21 C20 N6 Ru1 70.8(9) . . . . ? N4 C12 O1 C11 -6.1(6) . . . . ? C13 C12 O1 C11 173.1(4) . . . . ? C10 C11 O1 C12 9.5(6) . . . . ? N6 C18 O2 C19 -7.4(8) . . . . ? C17 C18 O2 C19 174.4(6) . . . . ? C20 C19 O2 C18 14.8(10) . . . . ? N2 C2 P1 C1 44.1(5) . . . . ? N2 C2 P1 C3 -53.1(4) . . . . ? N2 C2 P1 Ru1 174.4(3) . . . . ? N1 C1 P1 C2 -46.2(5) . . . . ? N1 C1 P1 C3 50.0(4) . . . . ? N1 C1 P1 Ru1 -176.8(3) . . . . ? N3 C3 P1 C2 50.1(4) . . . . ? N3 C3 P1 C1 -50.1(4) . . . . ? N3 C3 P1 Ru1 179.7(3) . . . . ? C13 N5 Ru1 N6 -179.9(4) . . . . ? C17 N5 Ru1 N6 -4.3(3) . . . . ? C13 N5 Ru1 N4 1.3(3) . . . . ? C17 N5 Ru1 N4 176.8(3) . . . . ? C13 N5 Ru1 P1 -85(4) . . . . ? C17 N5 Ru1 P1 91(4) . . . . ? C13 N5 Ru1 Cl1 -89.8(3) . . . . ? C17 N5 Ru1 Cl1 85.8(3) . . . . ? C13 N5 Ru1 Cl2 87.8(3) . . . . ? C17 N5 Ru1 Cl2 -96.6(3) . . . . ? C18 N6 Ru1 N5 4.3(4) . . . . ? C20 N6 Ru1 N5 -173.2(8) . . . . ? C18 N6 Ru1 N4 6.8(6) . . . . ? C20 N6 Ru1 N4 -170.7(7) . . . . ? C18 N6 Ru1 P1 -174.1(3) . . . . ? C20 N6 Ru1 P1 8.4(8) . . . . ? C18 N6 Ru1 Cl1 -82.7(4) . . . . ? C20 N6 Ru1 Cl1 99.8(8) . . . . ? C18 N6 Ru1 Cl2 95.5(4) . . . . ? C20 N6 Ru1 Cl2 -82.0(8) . . . . ? C12 N4 Ru1 N5 1.4(3) . . . . ? C10 N4 Ru1 N5 175.8(5) . . . . ? C12 N4 Ru1 N6 -1.2(5) . . . . ? C10 N4 Ru1 N6 173.2(4) . . . . ? C12 N4 Ru1 P1 179.7(3) . . . . ? C10 N4 Ru1 P1 -5.8(4) . . . . ? C12 N4 Ru1 Cl1 88.1(3) . . . . ? C10 N4 Ru1 Cl1 -97.4(4) . . . . ? C12 N4 Ru1 Cl2 -91.2(3) . . . . ? C10 N4 Ru1 Cl2 83.2(4) . . . . ? C2 P1 Ru1 N5 11(4) . . . . ? C1 P1 Ru1 N5 132(4) . . . . ? C3 P1 Ru1 N5 -108(4) . . . . ? C2 P1 Ru1 N6 105.2(3) . . . . ? C1 P1 Ru1 N6 -133.7(2) . . . . ? C3 P1 Ru1 N6 -13.6(3) . . . . ? C2 P1 Ru1 N4 -75.2(2) . . . . ? C1 P1 Ru1 N4 45.9(2) . . . . ? C3 P1 Ru1 N4 166.0(3) . . . . ? C2 P1 Ru1 Cl1 15.5(2) . . . . ? C1 P1 Ru1 Cl1 136.6(2) . . . . ? C3 P1 Ru1 Cl1 -103.3(2) . . . . ? C2 P1 Ru1 Cl2 -162.1(2) . . . . ? C1 P1 Ru1 Cl2 -41.0(2) . . . . ? C3 P1 Ru1 Cl2 79.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 73.85 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.592 _refine_diff_density_min -0.678 _refine_diff_density_rms 0.086 _database_code_depnum_ccdc_archive 'CCDC 937041' ####################################################################### # # 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_2a #========================================================================= _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H32 Cl2 N6 O2 P Ru, C H2 Cl2, Cl' _chemical_formula_sum 'C30 H34 Cl5 N6 O2 P Ru' _chemical_formula_weight 819.92 _chemical_compound_source synthesis loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.2960 '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' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.5635(1) _cell_length_b 14.7654(1) _cell_length_c 11.8752(1) _cell_angle_alpha 90.00 _cell_angle_beta 107.283(1) _cell_angle_gamma 90.00 _cell_volume 1768.60(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4929 _cell_measurement_theta_min 2.9896 _cell_measurement_theta_max 73.8376 _exptl_crystal_description prism _exptl_crystal_colour violet _exptl_crystal_size_max 0.145 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.008 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.540 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 7.797 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.83869 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET) (compiled Jan 27 2009,14:17:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ; 165 mm Onyx CCD detector in \k-geometry diffractometer ; _diffrn_measurement_device_type 'Xcalibur, Onyx, Nova' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.2640 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6937 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_sigmaI/netI 0.0446 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.90 _diffrn_reflns_theta_max 73.97 _reflns_number_total 4524 _reflns_number_gt 4087 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET) (compiled Jan 27 2009,14:17:37) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET) (compiled Jan 27 2009,14:17:37) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET) (compiled Jan 27 2009,14:17:37) ; _computing_structure_solution 'DIRDIF-2008 ( Beurskens, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2007)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999' _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^)+(0.0625P)^2^+1.8399P] 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 ? _chemical_absolute_configuration ad _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.022(15) _refine_ls_number_reflns 4524 _refine_ls_number_parameters 419 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0441 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.1160 _refine_ls_wR_factor_gt 0.0974 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _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 C1 C 0.0767(8) 0.6910(5) 0.8675(6) 0.0401(17) Uani 1 1 d . . . H1A H 0.1438 0.7295 0.8514 0.048 Uiso 1 1 calc R . . H1B H 0.0077 0.6810 0.7938 0.048 Uiso 1 1 calc R . . C2 C 0.0128(9) 0.5356(6) 0.9731(7) 0.0480(19) Uani 1 1 d . . . H2A H -0.0595 0.5203 0.9036 0.058 Uiso 1 1 calc R . . H2B H 0.0410 0.4804 1.0179 0.058 Uiso 1 1 calc R . . C3 C 0.2538(7) 0.6256(6) 1.0719(7) 0.0456(19) Uani 1 1 d . . . H3A H 0.2930 0.5751 1.1224 0.055 Uiso 1 1 calc R . . H3B H 0.3254 0.6619 1.0602 0.055 Uiso 1 1 calc R . . C4 C 0.1243(9) 0.7616(6) 1.0672(8) 0.0476(19) Uani 1 1 d . . . H4A H 0.1953 0.7949 1.0495 0.057 Uiso 1 1 calc R . . H4B H 0.0863 0.8000 1.1150 0.057 Uiso 1 1 calc R . . C5 C 0.0682(9) 0.6305(6) 1.1535(7) 0.051(2) Uani 1 1 d . . . H5A H 0.0271 0.6678 1.2000 0.062 Uiso 1 1 calc R . . H5B H 0.1045 0.5774 1.2001 0.062 Uiso 1 1 calc R . . C6 C -0.0893(8) 0.6815(6) 0.9797(8) 0.0482(19) Uani 1 1 d . . . H6A H -0.1341 0.7176 1.0245 0.058 Uiso 1 1 calc R . . H6B H -0.1542 0.6643 0.9062 0.058 Uiso 1 1 calc R . . C7 C -0.1170(7) 0.5741(6) 0.6164(6) 0.0400(17) Uani 1 1 d . . . C8 C -0.1495(7) 0.4893(7) 0.6475(7) 0.0494(18) Uani 1 1 d . . . H8 H -0.0955 0.4401 0.6448 0.059 Uiso 1 1 calc R . . C9 C -0.2627(9) 0.4768(7) 0.6828(9) 0.064(3) Uani 1 1 d . . . H9 H -0.2830 0.4193 0.7044 0.076 Uiso 1 1 calc R . . C10 C -0.3453(9) 0.5488(8) 0.6863(10) 0.064(3) Uani 1 1 d . . . H10 H -0.4221 0.5398 0.7079 0.077 Uiso 1 1 calc R . . C11 C -0.3132(9) 0.6309(9) 0.6582(9) 0.068(3) Uani 1 1 d . . . H11 H -0.3677 0.6794 0.6629 0.081 Uiso 1 1 calc R . . C12 C -0.1995(8) 0.6479(7) 0.6214(8) 0.055(2) Uani 1 1 d . . . H12 H -0.1800 0.7060 0.6013 0.066 Uiso 1 1 calc R . . C13 C 0.0045(7) 0.5903(6) 0.5793(7) 0.0413(17) Uani 1 1 d . . . H13 H 0.0320 0.6536 0.5947 0.050 Uiso 1 1 calc R . . C14 C -0.0179(8) 0.5691(8) 0.4474(7) 0.056(2) Uani 1 1 d . . . H14A H -0.0995 0.5354 0.4153 0.067 Uiso 1 1 calc R . . H14B H -0.0227 0.6245 0.4025 0.067 Uiso 1 1 calc R . . C15 C 0.1608(6) 0.4962(7) 0.5568(5) 0.0389(13) Uani 1 1 d . . . C16 C 0.2747(6) 0.4358(5) 0.5843(6) 0.0353(15) Uani 1 1 d . . . C17 C 0.3273(8) 0.3866(7) 0.5095(7) 0.053(2) Uani 1 1 d . . . H17 H 0.2925 0.3920 0.4281 0.063 Uiso 1 1 calc R . . C18 C 0.4338(8) 0.3288(7) 0.5592(9) 0.054(2) Uani 1 1 d . . . H18 H 0.4690 0.2939 0.5106 0.065 Uiso 1 1 calc R . . C19 C 0.4869(8) 0.3232(6) 0.6799(9) 0.051(2) Uani 1 1 d . . . H19 H 0.5596 0.2862 0.7133 0.061 Uiso 1 1 calc R . . C20 C 0.4298(7) 0.3738(6) 0.7507(7) 0.0400(16) Uani 1 1 d . . . C21 C 0.4647(7) 0.3786(6) 0.8773(7) 0.0419(17) Uani 1 1 d . . . C22 C 0.5426(11) 0.3350(7) 1.0640(8) 0.067(3) Uani 1 1 d . . . H22A H 0.6283 0.3461 1.1209 0.080 Uiso 1 1 calc R . . H22B H 0.5040 0.2813 1.0875 0.080 Uiso 1 1 calc R . . C23 C 0.4510(8) 0.4170(6) 1.0558(7) 0.0470(19) Uani 1 1 d . . . H23 H 0.3765 0.3992 1.0842 0.056 Uiso 1 1 calc R . . C24 C 0.5212(7) 0.4949(8) 1.1278(6) 0.0487(17) Uani 1 1 d . . . C25 C 0.5851(9) 0.5606(7) 1.0814(10) 0.061(2) Uani 1 1 d . . . H25 H 0.5807 0.5592 1.0021 0.073 Uiso 1 1 calc R . . C26 C 0.6554(10) 0.6285(9) 1.1541(12) 0.083(4) Uani 1 1 d . . . H26 H 0.6978 0.6731 1.1232 0.099 Uiso 1 1 calc R . . C27 C 0.6629(12) 0.6303(10) 1.2724(13) 0.094(5) Uani 1 1 d . . . H27 H 0.7115 0.6755 1.3210 0.113 Uiso 1 1 calc R . . C28 C 0.5997(13) 0.5665(10) 1.3177(10) 0.087(4) Uani 1 1 d . . . H28 H 0.6044 0.5684 1.3971 0.104 Uiso 1 1 calc R . . C29 C 0.5294(9) 0.4994(12) 1.2478(7) 0.073(3) Uani 1 1 d . . . H29 H 0.4863 0.4561 1.2799 0.088 Uiso 1 1 calc R . . C30 C 0.2533(15) 0.8004(11) 0.5688(14) 0.125(7) Uani 1 1 d D . . H30A H 0.3087 0.8531 0.5711 0.150 Uiso 1 1 calc R A 1 H30B H 0.2918 0.7644 0.6390 0.150 Uiso 1 1 calc R A 1 Cl1 Cl 0.1214(2) 0.36339(13) 0.81923(19) 0.0478(5) Uani 1 1 d . . . Cl2 Cl 0.3696(2) 0.63016(14) 0.79168(18) 0.0470(4) Uani 1 1 d . . . Cl3 Cl 0.8226(2) 0.87055(17) 0.79772(19) 0.0616(6) Uani 1 1 d . . . Cl4 Cl 0.2410(4) 0.7366(3) 0.4426(4) 0.1196(14) Uani 1 1 d . B . N1 N 0.0187(7) 0.7378(5) 0.9532(6) 0.0402(14) Uani 1 1 d . . . N2 N -0.0353(7) 0.6007(5) 1.0459(6) 0.0468(16) Uani 1 1 d . . . N3 N 0.1767(7) 0.6812(5) 1.1315(6) 0.0517(18) Uani 1 1 d . . . N4 N 0.1181(5) 0.5297(4) 0.6393(5) 0.0335(13) Uani 1 1 d . . . N5 N 0.3263(6) 0.4284(5) 0.7011(6) 0.0368(13) Uani 1 1 d . . . N6 N 0.4013(6) 0.4337(5) 0.9286(5) 0.0386(13) Uani 1 1 d . . . O1 O 0.5558(6) 0.3240(4) 0.9460(6) 0.0574(16) Uani 1 1 d . . . O2 O 0.0968(5) 0.5147(5) 0.4434(4) 0.0518(18) Uani 1 1 d . . . P1 P 0.15181(18) 0.58121(12) 0.92703(15) 0.0342(4) Uani 1 1 d . . . Ru1 Ru 0.24243(4) 0.49893(4) 0.80724(4) 0.03044(12) Uani 1 1 d . . . Cl5A Cl 0.091(2) 0.8337(16) 0.562(3) 0.194(12) Uani 0.50 1 d PD B 1 Cl5B Cl 0.104(2) 0.8260(12) 0.593(2) 0.188(12) Uani 0.50 1 d PD B 2 H1N H -0.028(16) 0.786(12) 0.929(14) 0.14(6) 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 0.044(4) 0.039(4) 0.040(4) -0.003(3) 0.017(3) 0.016(3) C2 0.063(5) 0.036(4) 0.052(4) -0.007(4) 0.027(4) 0.003(4) C3 0.036(4) 0.053(5) 0.042(4) -0.016(4) 0.002(3) 0.005(4) C4 0.055(5) 0.028(4) 0.064(5) -0.009(4) 0.024(4) -0.001(4) C5 0.072(6) 0.044(5) 0.045(4) -0.001(4) 0.027(4) 0.007(4) C6 0.036(4) 0.054(5) 0.057(5) -0.013(4) 0.018(3) 0.003(4) C7 0.032(3) 0.049(5) 0.034(3) -0.007(3) 0.004(3) 0.004(3) C8 0.042(4) 0.042(5) 0.067(4) 0.006(5) 0.020(3) 0.000(5) C9 0.048(5) 0.067(9) 0.081(6) -0.001(5) 0.026(4) -0.011(5) C10 0.042(5) 0.069(7) 0.087(7) -0.010(6) 0.029(5) -0.003(5) C11 0.040(5) 0.092(8) 0.069(6) -0.010(6) 0.014(4) 0.017(5) C12 0.037(4) 0.060(6) 0.062(5) 0.002(4) 0.007(4) 0.005(4) C13 0.032(3) 0.037(4) 0.050(4) 0.006(3) 0.004(3) 0.005(3) C14 0.045(4) 0.083(7) 0.036(4) 0.007(4) 0.007(3) 0.018(5) C15 0.039(3) 0.041(4) 0.037(3) -0.006(5) 0.012(2) -0.012(5) C16 0.029(3) 0.036(4) 0.044(3) -0.014(3) 0.015(3) -0.005(3) C17 0.047(4) 0.069(6) 0.046(4) -0.018(4) 0.019(3) -0.009(4) C18 0.042(4) 0.055(5) 0.071(6) -0.025(5) 0.024(4) 0.003(4) C19 0.035(4) 0.046(5) 0.077(6) -0.016(4) 0.023(4) 0.003(4) C20 0.028(3) 0.037(4) 0.052(4) -0.004(3) 0.008(3) 0.005(3) C21 0.032(3) 0.042(4) 0.051(4) 0.008(4) 0.010(3) 0.014(3) C22 0.076(6) 0.061(6) 0.051(5) 0.003(4) 0.001(4) 0.034(5) C23 0.042(4) 0.049(5) 0.047(4) 0.010(4) 0.007(3) 0.008(4) C24 0.037(3) 0.049(4) 0.049(3) -0.003(5) -0.004(3) 0.017(5) C25 0.042(4) 0.055(6) 0.075(6) -0.017(5) 0.000(4) 0.009(4) C26 0.047(5) 0.077(8) 0.110(9) -0.021(7) 0.003(6) 0.008(5) C27 0.062(7) 0.077(9) 0.113(11) -0.047(8) -0.023(7) 0.015(6) C28 0.085(8) 0.096(10) 0.055(6) -0.024(6) -0.016(5) 0.036(8) C29 0.072(6) 0.090(7) 0.046(4) -0.005(7) -0.001(4) 0.022(8) C30 0.21(2) 0.079(10) 0.083(9) 0.002(8) 0.030(11) -0.022(12) Cl1 0.0477(10) 0.0356(10) 0.0621(11) 0.0062(9) 0.0193(9) -0.0065(8) Cl2 0.0466(10) 0.0382(10) 0.0592(11) -0.0028(9) 0.0202(9) -0.0081(8) Cl3 0.0743(14) 0.0549(13) 0.0491(10) 0.0047(10) 0.0087(10) 0.0116(12) Cl4 0.117(3) 0.108(3) 0.147(4) -0.025(3) 0.060(3) -0.044(3) N1 0.044(4) 0.031(3) 0.049(3) -0.009(3) 0.019(3) 0.005(3) N2 0.053(4) 0.045(4) 0.051(3) 0.002(3) 0.029(3) 0.003(3) N3 0.051(4) 0.060(5) 0.044(4) -0.007(3) 0.015(3) 0.017(4) N4 0.028(3) 0.043(3) 0.030(2) 0.001(2) 0.009(2) 0.007(2) N5 0.027(3) 0.036(3) 0.049(3) -0.014(3) 0.012(2) -0.003(2) N6 0.041(3) 0.035(3) 0.039(3) 0.000(3) 0.011(2) 0.005(3) O1 0.052(3) 0.047(4) 0.066(4) 0.003(3) 0.007(3) 0.021(3) O2 0.046(3) 0.078(5) 0.031(2) -0.002(3) 0.0104(18) 0.001(3) P1 0.0395(9) 0.0293(9) 0.0358(8) -0.0039(7) 0.0145(7) 0.0051(7) Ru1 0.0311(2) 0.0280(2) 0.0332(2) -0.0008(3) 0.01109(14) 0.0019(3) Cl5A 0.29(2) 0.104(10) 0.28(3) 0.113(12) 0.213(19) 0.082(12) Cl5B 0.40(3) 0.052(6) 0.193(15) 0.023(10) 0.211(19) 0.007(11) _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 1.504(9) . ? C1 P1 1.851(8) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.481(10) . ? C2 P1 1.840(9) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N3 1.477(10) . ? C3 P1 1.857(7) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 N3 1.431(11) . ? C4 N1 1.517(11) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N3 1.456(12) . ? C5 N2 1.480(11) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N2 1.449(11) . ? C6 N1 1.518(11) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.377(13) . ? C7 C12 1.408(12) . ? C7 C13 1.496(11) . ? C8 C9 1.392(11) . ? C8 H8 0.9300 . ? C9 C10 1.384(14) . ? C9 H9 0.9300 . ? C10 C11 1.328(16) . ? C10 H10 0.9300 . ? C11 C12 1.417(13) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 N4 1.497(9) . ? C13 C14 1.545(11) . ? C13 H13 0.9800 . ? C14 O2 1.467(10) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 N4 1.293(9) . ? C15 O2 1.343(8) . ? C15 C16 1.454(11) . ? C16 N5 1.337(10) . ? C16 C17 1.384(10) . ? C17 C18 1.396(13) . ? C17 H17 0.9300 . ? C18 C19 1.377(13) . ? C18 H18 0.9300 . ? C19 C20 1.390(11) . ? C19 H19 0.9300 . ? C20 N5 1.346(10) . ? C20 C21 1.438(11) . ? C21 N6 1.313(10) . ? C21 O1 1.333(9) . ? C22 O1 1.458(12) . ? C22 C23 1.534(12) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 N6 1.465(9) . ? C23 C24 1.493(14) . ? C23 H23 0.9800 . ? C24 C25 1.385(15) . ? C24 C29 1.404(11) . ? C25 C26 1.386(15) . ? C25 H25 0.9300 . ? C26 C27 1.385(19) . ? C26 H26 0.9300 . ? C27 C28 1.36(2) . ? C27 H27 0.9300 . ? C28 C29 1.362(19) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 Cl5B 1.722(18) . ? C30 Cl4 1.742(15) . ? C30 Cl5A 1.761(18) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? Cl1 Ru1 2.402(2) . ? Cl2 Ru1 2.396(2) . ? N1 H1N 0.87(17) . ? N4 Ru1 2.086(5) . ? N5 Ru1 2.029(6) . ? N6 Ru1 2.094(6) . ? P1 Ru1 2.2858(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 N1 C1 P1 111.0(5) . . ? N1 C1 H1A 109.4 . . ? P1 C1 H1A 109.4 . . ? N1 C1 H1B 109.4 . . ? P1 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? N2 C2 P1 112.2(6) . . ? N2 C2 H2A 109.2 . . ? P1 C2 H2A 109.2 . . ? N2 C2 H2B 109.2 . . ? P1 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? N3 C3 P1 112.9(5) . . ? N3 C3 H3A 109.0 . . ? P1 C3 H3A 109.0 . . ? N3 C3 H3B 109.0 . . ? P1 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? N3 C4 N1 110.4(7) . . ? N3 C4 H4A 109.6 . . ? N1 C4 H4A 109.6 . . ? N3 C4 H4B 109.6 . . ? N1 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? N3 C5 N2 114.6(6) . . ? N3 C5 H5A 108.6 . . ? N2 C5 H5A 108.6 . . ? N3 C5 H5B 108.6 . . ? N2 C5 H5B 108.6 . . ? H5A C5 H5B 107.6 . . ? N2 C6 N1 111.3(6) . . ? N2 C6 H6A 109.4 . . ? N1 C6 H6A 109.4 . . ? N2 C6 H6B 109.4 . . ? N1 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? C8 C7 C12 119.1(7) . . ? C8 C7 C13 121.9(7) . . ? C12 C7 C13 119.0(8) . . ? C7 C8 C9 120.4(9) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C10 C9 C8 120.8(10) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? C11 C10 C9 118.9(9) . . ? C11 C10 H10 120.5 . . ? C9 C10 H10 120.5 . . ? C10 C11 C12 122.8(10) . . ? C10 C11 H11 118.6 . . ? C12 C11 H11 118.6 . . ? C7 C12 C11 117.9(10) . . ? C7 C12 H12 121.1 . . ? C11 C12 H12 121.1 . . ? C7 C13 N4 113.6(6) . . ? C7 C13 C14 112.3(6) . . ? N4 C13 C14 102.8(6) . . ? C7 C13 H13 109.3 . . ? N4 C13 H13 109.3 . . ? C14 C13 H13 109.3 . . ? O2 C14 C13 105.3(6) . . ? O2 C14 H14A 110.7 . . ? C13 C14 H14A 110.7 . . ? O2 C14 H14B 110.7 . . ? C13 C14 H14B 110.7 . . ? H14A C14 H14B 108.8 . . ? N4 C15 O2 119.8(8) . . ? N4 C15 C16 121.1(6) . . ? O2 C15 C16 119.0(6) . . ? N5 C16 C17 120.4(7) . . ? N5 C16 C15 109.7(6) . . ? C17 C16 C15 129.9(7) . . ? C16 C17 C18 118.5(8) . . ? C16 C17 H17 120.8 . . ? C18 C17 H17 120.8 . . ? C19 C18 C17 120.3(8) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C20 118.8(8) . . ? C18 C19 H19 120.6 . . ? C20 C19 H19 120.6 . . ? N5 C20 C19 120.0(8) . . ? N5 C20 C21 110.5(7) . . ? C19 C20 C21 129.5(7) . . ? N6 C21 O1 117.7(7) . . ? N6 C21 C20 120.5(6) . . ? O1 C21 C20 121.6(7) . . ? O1 C22 C23 105.4(7) . . ? O1 C22 H22A 110.7 . . ? C23 C22 H22A 110.7 . . ? O1 C22 H22B 110.7 . . ? C23 C22 H22B 110.7 . . ? H22A C22 H22B 108.8 . . ? N6 C23 C24 115.1(7) . . ? N6 C23 C22 103.0(7) . . ? C24 C23 C22 112.0(7) . . ? N6 C23 H23 108.8 . . ? C24 C23 H23 108.8 . . ? C22 C23 H23 108.8 . . ? C25 C24 C29 118.7(11) . . ? C25 C24 C23 122.0(7) . . ? C29 C24 C23 119.2(11) . . ? C24 C25 C26 119.6(11) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? C27 C26 C25 120.3(14) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C28 C27 C26 120.2(11) . . ? C28 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C27 C28 C29 120.5(12) . . ? C27 C28 H28 119.7 . . ? C29 C28 H28 119.7 . . ? C28 C29 C24 120.7(14) . . ? C28 C29 H29 119.6 . . ? C24 C29 H29 119.6 . . ? Cl5B C30 Cl4 115.1(13) . . ? Cl5B C30 Cl5A 12.3(18) . . ? Cl4 C30 Cl5A 106.6(13) . . ? Cl5B C30 H30A 113.1 . . ? Cl4 C30 H30A 110.4 . . ? Cl5A C30 H30A 110.4 . . ? Cl5B C30 H30B 98.5 . . ? Cl4 C30 H30B 110.4 . . ? Cl5A C30 H30B 110.4 . . ? H30A C30 H30B 108.6 . . ? C1 N1 C4 111.8(6) . . ? C1 N1 C6 111.8(6) . . ? C4 N1 C6 109.9(6) . . ? C1 N1 H1N 118(10) . . ? C4 N1 H1N 107(10) . . ? C6 N1 H1N 97(10) . . ? C6 N2 C5 107.2(7) . . ? C6 N2 C2 111.5(7) . . ? C5 N2 C2 113.8(7) . . ? C4 N3 C5 108.8(7) . . ? C4 N3 C3 112.7(7) . . ? C5 N3 C3 112.1(7) . . ? C15 N4 C13 106.2(6) . . ? C15 N4 Ru1 112.3(5) . . ? C13 N4 Ru1 140.7(5) . . ? C16 N5 C20 122.1(7) . . ? C16 N5 Ru1 119.0(5) . . ? C20 N5 Ru1 118.9(5) . . ? C21 N6 C23 107.4(6) . . ? C21 N6 Ru1 112.3(5) . . ? C23 N6 Ru1 139.1(5) . . ? C21 O1 C22 105.2(6) . . ? C15 O2 C14 104.7(6) . . ? C2 P1 C1 98.3(4) . . ? C2 P1 C3 98.6(4) . . ? C1 P1 C3 96.3(4) . . ? C2 P1 Ru1 120.6(3) . . ? C1 P1 Ru1 116.0(2) . . ? C3 P1 Ru1 121.9(3) . . ? N5 Ru1 N4 77.6(2) . . ? N5 Ru1 N6 77.5(3) . . ? N4 Ru1 N6 155.0(2) . . ? N5 Ru1 P1 178.5(2) . . ? N4 Ru1 P1 102.59(16) . . ? N6 Ru1 P1 102.37(18) . . ? N5 Ru1 Cl2 90.49(19) . . ? N4 Ru1 Cl2 87.61(18) . . ? N6 Ru1 Cl2 94.11(19) . . ? P1 Ru1 Cl2 88.07(7) . . ? N5 Ru1 Cl1 87.0(2) . . ? N4 Ru1 Cl1 92.48(18) . . ? N6 Ru1 Cl1 84.73(19) . . ? P1 Ru1 Cl1 94.43(7) . . ? Cl2 Ru1 Cl1 177.41(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C12 C7 C8 C9 0.3(12) . . . . ? C13 C7 C8 C9 179.3(8) . . . . ? C7 C8 C9 C10 0.7(14) . . . . ? C8 C9 C10 C11 -1.7(15) . . . . ? C9 C10 C11 C12 1.8(16) . . . . ? C8 C7 C12 C11 -0.2(11) . . . . ? C13 C7 C12 C11 -179.3(7) . . . . ? C10 C11 C12 C7 -0.9(14) . . . . ? C8 C7 C13 N4 -32.7(10) . . . . ? C12 C7 C13 N4 146.3(7) . . . . ? C8 C7 C13 C14 83.5(9) . . . . ? C12 C7 C13 C14 -97.5(9) . . . . ? C7 C13 C14 O2 -133.3(8) . . . . ? N4 C13 C14 O2 -10.8(9) . . . . ? N4 C15 C16 N5 -4.0(11) . . . . ? O2 C15 C16 N5 178.1(7) . . . . ? N4 C15 C16 C17 173.1(8) . . . . ? O2 C15 C16 C17 -4.8(14) . . . . ? N5 C16 C17 C18 0.7(12) . . . . ? C15 C16 C17 C18 -176.1(8) . . . . ? C16 C17 C18 C19 -1.8(14) . . . . ? C17 C18 C19 C20 2.0(14) . . . . ? C18 C19 C20 N5 -1.3(13) . . . . ? C18 C19 C20 C21 178.8(9) . . . . ? N5 C20 C21 N6 -2.5(11) . . . . ? C19 C20 C21 N6 177.4(8) . . . . ? N5 C20 C21 O1 173.3(7) . . . . ? C19 C20 C21 O1 -6.8(14) . . . . ? O1 C22 C23 N6 10.3(10) . . . . ? O1 C22 C23 C24 -114.0(9) . . . . ? N6 C23 C24 C25 -26.7(11) . . . . ? C22 C23 C24 C25 90.5(10) . . . . ? N6 C23 C24 C29 156.9(8) . . . . ? C22 C23 C24 C29 -85.9(10) . . . . ? C29 C24 C25 C26 0.3(14) . . . . ? C23 C24 C25 C26 -176.2(8) . . . . ? C24 C25 C26 C27 0.6(15) . . . . ? C25 C26 C27 C28 -1.0(18) . . . . ? C26 C27 C28 C29 0.7(18) . . . . ? C27 C28 C29 C24 0.2(18) . . . . ? C25 C24 C29 C28 -0.7(15) . . . . ? C23 C24 C29 C28 175.9(9) . . . . ? P1 C1 N1 C4 63.3(8) . . . . ? P1 C1 N1 C6 -60.4(7) . . . . ? N3 C4 N1 C1 -68.4(9) . . . . ? N3 C4 N1 C6 56.3(8) . . . . ? N2 C6 N1 C1 68.3(8) . . . . ? N2 C6 N1 C4 -56.4(8) . . . . ? N1 C6 N2 C5 55.9(8) . . . . ? N1 C6 N2 C2 -69.2(8) . . . . ? N3 C5 N2 C6 -59.6(9) . . . . ? N3 C5 N2 C2 64.1(10) . . . . ? P1 C2 N2 C6 63.8(8) . . . . ? P1 C2 N2 C5 -57.5(8) . . . . ? N1 C4 N3 C5 -57.2(8) . . . . ? N1 C4 N3 C3 67.8(9) . . . . ? N2 C5 N3 C4 60.9(9) . . . . ? N2 C5 N3 C3 -64.4(9) . . . . ? P1 C3 N3 C4 -63.6(9) . . . . ? P1 C3 N3 C5 59.5(8) . . . . ? O2 C15 N4 C13 -4.1(11) . . . . ? C16 C15 N4 C13 178.0(7) . . . . ? O2 C15 N4 Ru1 -175.7(6) . . . . ? C16 C15 N4 Ru1 6.5(10) . . . . ? C7 C13 N4 C15 130.7(7) . . . . ? C14 C13 N4 C15 9.0(9) . . . . ? C7 C13 N4 Ru1 -61.7(10) . . . . ? C14 C13 N4 Ru1 176.6(6) . . . . ? C17 C16 N5 C20 0.0(12) . . . . ? C15 C16 N5 C20 177.4(7) . . . . ? C17 C16 N5 Ru1 -178.2(6) . . . . ? C15 C16 N5 Ru1 -0.7(8) . . . . ? C19 C20 N5 C16 0.3(12) . . . . ? C21 C20 N5 C16 -179.8(7) . . . . ? C19 C20 N5 Ru1 178.4(6) . . . . ? C21 C20 N5 Ru1 -1.7(9) . . . . ? O1 C21 N6 C23 -1.0(10) . . . . ? C20 C21 N6 C23 174.9(7) . . . . ? O1 C21 N6 Ru1 -170.8(6) . . . . ? C20 C21 N6 Ru1 5.1(10) . . . . ? C24 C23 N6 C21 116.2(8) . . . . ? C22 C23 N6 C21 -6.0(10) . . . . ? C24 C23 N6 Ru1 -78.3(10) . . . . ? C22 C23 N6 Ru1 159.5(7) . . . . ? N6 C21 O1 C22 8.0(11) . . . . ? C20 C21 O1 C22 -167.9(8) . . . . ? C23 C22 O1 C21 -10.9(10) . . . . ? N4 C15 O2 C14 -3.2(11) . . . . ? C16 C15 O2 C14 174.7(8) . . . . ? C13 C14 O2 C15 8.7(10) . . . . ? N2 C2 P1 C1 -50.4(7) . . . . ? N2 C2 P1 C3 47.3(7) . . . . ? N2 C2 P1 Ru1 -177.5(5) . . . . ? N1 C1 P1 C2 48.9(6) . . . . ? N1 C1 P1 C3 -50.7(6) . . . . ? N1 C1 P1 Ru1 179.0(4) . . . . ? N3 C3 P1 C2 -48.8(7) . . . . ? N3 C3 P1 C1 50.6(7) . . . . ? N3 C3 P1 Ru1 176.7(5) . . . . ? C16 N5 Ru1 N4 3.0(5) . . . . ? C20 N5 Ru1 N4 -175.1(6) . . . . ? C16 N5 Ru1 N6 -178.5(6) . . . . ? C20 N5 Ru1 N6 3.3(6) . . . . ? C16 N5 Ru1 P1 -95(8) . . . . ? C20 N5 Ru1 P1 87(8) . . . . ? C16 N5 Ru1 Cl2 -84.4(6) . . . . ? C20 N5 Ru1 Cl2 97.4(6) . . . . ? C16 N5 Ru1 Cl1 96.2(6) . . . . ? C20 N5 Ru1 Cl1 -81.9(6) . . . . ? C15 N4 Ru1 N5 -4.9(6) . . . . ? C13 N4 Ru1 N5 -172.0(8) . . . . ? C15 N4 Ru1 N6 -8.5(10) . . . . ? C13 N4 Ru1 N6 -175.6(7) . . . . ? C15 N4 Ru1 P1 173.6(6) . . . . ? C13 N4 Ru1 P1 6.5(8) . . . . ? C15 N4 Ru1 Cl2 86.1(6) . . . . ? C13 N4 Ru1 Cl2 -81.0(8) . . . . ? C15 N4 Ru1 Cl1 -91.3(6) . . . . ? C13 N4 Ru1 Cl1 101.6(8) . . . . ? C21 N6 Ru1 N5 -4.3(6) . . . . ? C23 N6 Ru1 N5 -169.4(9) . . . . ? C21 N6 Ru1 N4 -0.8(10) . . . . ? C23 N6 Ru1 N4 -165.8(7) . . . . ? C21 N6 Ru1 P1 177.2(5) . . . . ? C23 N6 Ru1 P1 12.1(9) . . . . ? C21 N6 Ru1 Cl2 -93.9(6) . . . . ? C23 N6 Ru1 Cl2 101.0(8) . . . . ? C21 N6 Ru1 Cl1 83.8(6) . . . . ? C23 N6 Ru1 Cl1 -81.3(8) . . . . ? C2 P1 Ru1 N5 -178(100) . . . . ? C1 P1 Ru1 N5 63(8) . . . . ? C3 P1 Ru1 N5 -53(8) . . . . ? C2 P1 Ru1 N4 84.6(4) . . . . ? C1 P1 Ru1 N4 -33.8(4) . . . . ? C3 P1 Ru1 N4 -150.4(4) . . . . ? C2 P1 Ru1 N6 -94.5(4) . . . . ? C1 P1 Ru1 N6 147.1(4) . . . . ? C3 P1 Ru1 N6 30.5(4) . . . . ? C2 P1 Ru1 Cl2 171.8(3) . . . . ? C1 P1 Ru1 Cl2 53.3(3) . . . . ? C3 P1 Ru1 Cl2 -63.3(4) . . . . ? C2 P1 Ru1 Cl1 -8.9(3) . . . . ? C1 P1 Ru1 Cl1 -127.4(3) . . . . ? C3 P1 Ru1 Cl1 116.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 73.97 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 1.031 _refine_diff_density_min -0.841 _refine_diff_density_rms 0.093 _database_code_depnum_ccdc_archive 'CCDC 937042' ####################################################################### # # 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_3b #========================================================================= # start Validation Reply Form ============================================ _vrf_PLAT029_3b ; PROBLEM: diffrn_measured_fraction_theta_full Low ....... 0.958 RESPONSE: Due to the poor diffraction quality of the crystal ; # end Validation Reply Form ============================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H38 Cl2 N6 O2 P Ru, I' _chemical_formula_sum 'C24 H38 Cl2 I N6 O2 P Ru' _chemical_formula_weight 772.44 _chemical_compound_source synthesis loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C 2 2 21' _symmetry_space_group_name_Hall 'C 2c 2' _symmetry_Int_Tables_number 20 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.081 0.250 567 99 ' ' 2 0.000 -0.081 0.750 567 99 ' ' 3 0.500 0.581 0.250 567 99 ' ' 4 0.500 0.419 0.750 567 99 ' ' _platon_squeeze_details ; ; loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 13.5047(2) _cell_length_b 23.2490(5) _cell_length_c 24.3739(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7652.7(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11745 _cell_measurement_theta_min 3.5168 _cell_measurement_theta_max 73.6709 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.046 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.341 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3088 _exptl_absorpt_coefficient_mu 11.540 _exptl_absorpt_correction_T_min 0.87897 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET) (compiled Oct 24 2008,09:44:38) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ; 165 mm Onyx CCD detector in \k-geometry diffractometer ; _diffrn_measurement_device_type 'Xcalibur, Onyx, Nova' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.2640 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10478 _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_av_unetI/netI 0.0256 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.63 _diffrn_reflns_theta_max 74.01 _reflns_number_total 6104 _reflns_number_gt 5418 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET) (compiled Oct 24 2008,09:44:38) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET) (compiled Oct 24 2008,09:44:38) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET) (compiled Oct 24 2008,09:44:38) ; _computing_structure_solution 'SIR92 (Altomare, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2007)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999' _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. For the anisotropic refinement especially of disordered atoms DELU and SIMU commands have been used: DELU 0.010 0.010 C16 C17 SIMU 0.040 0.080 1.700 C16 C17 DELU 0.010 0.010 C12 O1 SIMU 0.040 0.080 1.700 C12 O1 ; _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^)+(0.0947P)^2^+7.9303P] 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 ? _chemical_absolute_configuration ad _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.041(11) _refine_ls_number_reflns 6104 _refine_ls_number_parameters 335 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0555 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.1446 _refine_ls_wR_factor_gt 0.1395 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 C1 C 0.5299(4) 0.1739(3) 0.5284(3) 0.0540(14) Uani 1 1 d . . . H1A H 0.5477 0.1408 0.5063 0.065 Uiso 1 1 calc R . . H1B H 0.5819 0.2024 0.5244 0.065 Uiso 1 1 calc R . . C2 C 0.3317(5) 0.1457(4) 0.5270(3) 0.075(2) Uani 1 1 d . . . H2A H 0.2632 0.1567 0.5215 0.090 Uiso 1 1 calc R . . H2B H 0.3442 0.1116 0.5053 0.090 Uiso 1 1 calc R . . C3 C 0.3889(6) 0.2535(3) 0.5601(3) 0.0705(19) Uani 1 1 d . . . H3A H 0.4358 0.2851 0.5584 0.085 Uiso 1 1 calc R . . H3B H 0.3229 0.2695 0.5563 0.085 Uiso 1 1 calc R . . C4 C 0.4427(5) 0.1101(3) 0.5953(3) 0.0645(17) Uani 1 1 d . . . H4A H 0.4556 0.0778 0.5711 0.077 Uiso 1 1 calc R . . H4B H 0.4452 0.0962 0.6328 0.077 Uiso 1 1 calc R . . C5 C 0.3265(6) 0.1805(6) 0.6202(4) 0.095(3) Uani 1 1 d . . . H5A H 0.2605 0.1950 0.6127 0.114 Uiso 1 1 calc R . . H5B H 0.3283 0.1677 0.6580 0.114 Uiso 1 1 calc R . . C6 C 0.4990(6) 0.2074(4) 0.6241(3) 0.0679(17) Uani 1 1 d . . . H6A H 0.5053 0.1964 0.6623 0.082 Uiso 1 1 calc R . . H6B H 0.5446 0.2388 0.6170 0.082 Uiso 1 1 calc R . . C7 C 0.6196(5) 0.1314(4) 0.6054(3) 0.072(2) Uani 1 1 d . . . H7A H 0.6145 0.1201 0.6432 0.108 Uiso 1 1 calc R . . H7B H 0.6709 0.1596 0.6015 0.108 Uiso 1 1 calc R . . H7C H 0.6353 0.0983 0.5834 0.108 Uiso 1 1 calc R . . C8 C 0.5262(10) 0.4116(6) 0.5309(7) 0.134(5) Uani 1 1 d . . . H8A H 0.4972 0.4486 0.5239 0.201 Uiso 1 1 calc R . . H8B H 0.5950 0.4162 0.5396 0.201 Uiso 1 1 calc R . . H8C H 0.4928 0.3938 0.5613 0.201 Uiso 1 1 calc R . . C9 C 0.5751(7) 0.3969(4) 0.4310(7) 0.125(5) Uani 1 1 d . . . H9A H 0.5504 0.4341 0.4206 0.188 Uiso 1 1 calc R . . H9B H 0.5679 0.3707 0.4009 0.188 Uiso 1 1 calc R . . H9C H 0.6438 0.4000 0.4406 0.188 Uiso 1 1 calc R . . C10 C 0.5159(7) 0.3743(4) 0.4809(5) 0.096(3) Uani 1 1 d . . . H10 H 0.5412 0.3360 0.4900 0.115 Uiso 1 1 calc R . . C11 C 0.4036(7) 0.3684(3) 0.4669(4) 0.076(2) Uani 1 1 d . . . H11 H 0.3654 0.3580 0.4996 0.092 Uiso 1 1 calc R . . C12 C 0.3587(7) 0.4214(4) 0.4385(6) 0.095(3) Uani 1 1 d U . . H12A H 0.2920 0.4284 0.4517 0.114 Uiso 1 1 calc R . . H12B H 0.3987 0.4553 0.4454 0.114 Uiso 1 1 calc R . . C13 C 0.3711(5) 0.3502(4) 0.3797(4) 0.0682(19) Uani 1 1 d . . . C14 C 0.3685(6) 0.3202(5) 0.3279(4) 0.084(3) Uani 1 1 d . . . C15 C 0.3555(8) 0.3408(7) 0.2747(5) 0.110(4) Uani 1 1 d . . . H15 H 0.3440 0.3797 0.2686 0.132 Uiso 1 1 calc R . . C16 C 0.3599(8) 0.3034(9) 0.2317(5) 0.122(4) Uani 1 1 d U . . H16 H 0.3537 0.3172 0.1960 0.146 Uiso 1 1 calc R . . C17 C 0.3739(7) 0.2436(7) 0.2409(4) 0.106(3) Uani 1 1 d U . . H17 H 0.3745 0.2173 0.2121 0.127 Uiso 1 1 calc R . . C18 C 0.3868(5) 0.2264(4) 0.2954(3) 0.075(2) Uani 1 1 d . . . C19 C 0.3980(6) 0.1674(4) 0.3153(3) 0.077(2) Uani 1 1 d . . . C20 C 0.4285(9) 0.0766(6) 0.3171(5) 0.116(4) Uani 1 1 d . . . H20A H 0.4989 0.0685 0.3150 0.140 Uiso 1 1 calc R . . H20B H 0.3922 0.0423 0.3068 0.140 Uiso 1 1 calc R . . C21 C 0.4004(7) 0.0957(3) 0.3745(4) 0.075(2) Uani 1 1 d . . . H21 H 0.4501 0.0831 0.4013 0.091 Uiso 1 1 calc R . . C22 C 0.2939(7) 0.0765(4) 0.3925(5) 0.083(2) Uani 1 1 d . . . H22 H 0.2743 0.0995 0.4243 0.100 Uiso 1 1 calc R . . C23 C 0.2202(7) 0.0866(6) 0.3477(5) 0.101(3) Uani 1 1 d . . . H23A H 0.2200 0.1266 0.3381 0.151 Uiso 1 1 calc R . . H23B H 0.1555 0.0756 0.3602 0.151 Uiso 1 1 calc R . . H23C H 0.2378 0.0641 0.3162 0.151 Uiso 1 1 calc R . . C24 C 0.2972(9) 0.0132(4) 0.4100(7) 0.123(4) Uani 1 1 d . . . H24A H 0.3151 -0.0103 0.3791 0.185 Uiso 1 1 calc R . . H24B H 0.2333 0.0017 0.4233 0.185 Uiso 1 1 calc R . . H24C H 0.3454 0.0084 0.4386 0.185 Uiso 1 1 calc R . . N1 N 0.5239(4) 0.1561(2) 0.5870(2) 0.0561(11) Uani 1 1 d . . . N2 N 0.3468(4) 0.1322(3) 0.5843(3) 0.0725(17) Uani 1 1 d . . . N3 N 0.3971(5) 0.2261(3) 0.6127(3) 0.0727(16) Uani 1 1 d . . . N4 N 0.3918(4) 0.3248(2) 0.4235(3) 0.0619(14) Uani 1 1 d . . . N5 N 0.3839(4) 0.2647(4) 0.3360(2) 0.0680(15) Uani 1 1 d . . . N6 N 0.4025(5) 0.1594(3) 0.3678(2) 0.0615(13) Uani 1 1 d . . . O1 O 0.3580(5) 0.4073(3) 0.3799(3) 0.0898(17) Uani 1 1 d U . . O2 O 0.4032(6) 0.1235(4) 0.2819(3) 0.100(2) Uani 1 1 d . . . P1 P 0.41251(11) 0.20427(7) 0.50259(6) 0.0515(3) Uani 1 1 d . . . Cl1 Cl 0.22482(10) 0.22859(7) 0.42465(8) 0.0634(4) Uani 1 1 d . . . Cl2 Cl 0.57934(10) 0.23815(9) 0.40542(7) 0.0696(4) Uani 1 1 d . . . Ru1 Ru 0.40169(3) 0.23488(2) 0.41413(2) 0.05213(14) Uani 1 1 d . . . I1 I 0.59157(9) 0.0000 0.5000 0.1238(4) Uani 1 2 d S . . I2 I 0.5000 0.08720(7) 0.7500 0.1912(11) Uani 1 2 d S . . 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 0.037(3) 0.056(3) 0.069(4) -0.003(3) 0.005(2) 0.000(2) C2 0.039(3) 0.106(6) 0.078(5) 0.011(5) -0.007(3) -0.026(4) C3 0.071(4) 0.060(4) 0.081(4) 0.000(4) 0.009(3) 0.020(3) C4 0.055(4) 0.067(4) 0.072(4) 0.011(4) -0.003(3) -0.009(3) C5 0.051(4) 0.152(10) 0.082(5) 0.027(6) 0.022(4) 0.033(5) C6 0.066(4) 0.077(4) 0.061(4) -0.008(4) -0.001(3) -0.004(4) C7 0.045(4) 0.095(5) 0.075(4) 0.012(4) -0.013(3) 0.003(3) C8 0.097(8) 0.115(9) 0.191(15) -0.010(10) -0.052(9) -0.010(7) C9 0.067(6) 0.075(5) 0.233(17) 0.037(8) -0.033(7) -0.003(4) C10 0.069(5) 0.073(5) 0.146(9) 0.004(6) -0.036(6) -0.003(4) C11 0.063(4) 0.054(3) 0.112(6) -0.007(4) -0.017(4) -0.004(4) C12 0.064(4) 0.059(4) 0.161(7) 0.003(5) -0.024(5) -0.006(4) C13 0.047(3) 0.070(4) 0.088(5) 0.014(4) -0.004(3) 0.008(3) C14 0.047(4) 0.115(7) 0.092(6) 0.032(6) -0.001(4) 0.012(4) C15 0.069(5) 0.164(12) 0.096(8) 0.057(8) -0.009(5) 0.007(6) C16 0.073(6) 0.217(12) 0.076(6) 0.043(9) -0.010(5) 0.004(8) C17 0.068(5) 0.183(10) 0.066(5) 0.003(7) -0.006(4) -0.012(6) C18 0.056(4) 0.102(6) 0.066(4) -0.007(5) 0.000(3) 0.002(4) C19 0.054(4) 0.108(6) 0.070(4) -0.025(5) 0.004(4) 0.002(4) C20 0.085(7) 0.136(10) 0.128(9) -0.053(9) 0.011(6) 0.030(6) C21 0.062(4) 0.062(4) 0.103(6) -0.030(4) -0.006(4) 0.010(4) C22 0.063(4) 0.068(4) 0.118(7) -0.027(5) -0.012(4) 0.005(4) C23 0.060(5) 0.123(8) 0.119(8) -0.026(7) -0.016(5) -0.014(5) C24 0.103(8) 0.074(6) 0.192(14) -0.022(8) -0.012(9) -0.002(5) N1 0.040(2) 0.065(3) 0.064(3) 0.002(3) -0.001(2) -0.003(2) N2 0.039(3) 0.097(4) 0.081(4) 0.014(4) 0.001(3) -0.013(3) N3 0.081(4) 0.069(3) 0.068(3) 0.002(3) 0.017(3) 0.026(4) N4 0.044(3) 0.051(2) 0.090(4) 0.018(3) -0.004(3) 0.000(2) N5 0.042(3) 0.101(4) 0.061(3) 0.007(4) -0.007(2) 0.001(3) N6 0.048(3) 0.071(3) 0.065(3) -0.020(3) 0.003(3) 0.011(3) O1 0.071(3) 0.067(3) 0.132(5) 0.026(4) -0.018(4) 0.001(3) O2 0.086(4) 0.127(6) 0.086(4) -0.041(4) -0.003(4) 0.019(4) P1 0.0404(7) 0.0560(8) 0.0580(8) -0.0007(7) 0.0025(6) -0.0010(6) Cl1 0.0387(7) 0.0609(8) 0.0906(11) -0.0028(9) 0.0010(6) 0.0084(6) Cl2 0.0396(7) 0.0941(11) 0.0751(9) 0.0065(10) 0.0044(6) -0.0064(7) Ru1 0.0391(2) 0.0584(2) 0.0589(2) -0.0004(2) 0.00013(18) 0.00036(19) I1 0.0910(6) 0.1160(7) 0.1645(10) -0.0620(8) 0.000 0.000 I2 0.385(3) 0.1200(10) 0.0691(6) 0.000 0.0038(11) 0.000 _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 1.489(9) . ? C1 P1 1.846(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.446(11) . ? C2 P1 1.843(8) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N3 1.436(11) . ? C3 P1 1.838(8) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 N2 1.419(10) . ? C4 N1 1.544(8) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N3 1.436(14) . ? C5 N2 1.450(14) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N3 1.469(11) . ? C6 N1 1.534(10) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N1 1.483(8) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C10 1.503(18) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.55(2) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.560(13) . ? C10 H10 0.9800 . ? C11 N4 1.474(11) . ? C11 C12 1.537(13) . ? C11 H11 0.9800 . ? C12 O1 1.465(14) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N4 1.252(10) . ? C13 O1 1.341(10) . ? C13 C14 1.443(15) . ? C14 N5 1.322(13) . ? C14 C15 1.392(15) . ? C15 C16 1.36(2) . ? C15 H15 0.9300 . ? C16 C17 1.42(2) . ? C16 H16 0.9300 . ? C17 C18 1.398(14) . ? C17 H17 0.9300 . ? C18 N5 1.332(11) . ? C18 C19 1.463(14) . ? C19 N6 1.295(10) . ? C19 O2 1.308(11) . ? C20 O2 1.428(17) . ? C20 C21 1.517(15) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 N6 1.489(10) . ? C21 C22 1.569(14) . ? C21 H21 0.9800 . ? C22 C23 1.494(15) . ? C22 C24 1.533(15) . ? C22 H22 0.9800 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? N4 Ru1 2.107(6) . ? N5 Ru1 2.041(6) . ? N6 Ru1 2.087(5) . ? P1 Ru1 2.2752(17) . ? Cl1 Ru1 2.4068(14) . ? Cl2 Ru1 2.4096(14) . ? 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 P1 112.8(4) . . ? N1 C1 H1A 109.0 . . ? P1 C1 H1A 109.0 . . ? N1 C1 H1B 109.0 . . ? P1 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? N2 C2 P1 112.9(5) . . ? N2 C2 H2A 109.0 . . ? P1 C2 H2A 109.0 . . ? N2 C2 H2B 109.0 . . ? P1 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? N3 C3 P1 113.0(5) . . ? N3 C3 H3A 109.0 . . ? P1 C3 H3A 109.0 . . ? N3 C3 H3B 109.0 . . ? P1 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? N2 C4 N1 111.9(6) . . ? N2 C4 H4A 109.2 . . ? N1 C4 H4A 109.2 . . ? N2 C4 H4B 109.2 . . ? N1 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? N3 C5 N2 111.7(6) . . ? N3 C5 H5A 109.3 . . ? N2 C5 H5A 109.3 . . ? N3 C5 H5B 109.3 . . ? N2 C5 H5B 109.3 . . ? H5A C5 H5B 107.9 . . ? N3 C6 N1 108.9(6) . . ? N3 C6 H6A 109.9 . . ? N1 C6 H6A 109.9 . . ? N3 C6 H6B 109.9 . . ? N1 C6 H6B 109.9 . . ? H6A C6 H6B 108.3 . . ? N1 C7 H7A 109.5 . . ? N1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C10 C8 H8A 109.5 . . ? C10 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C10 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C10 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 C9 113.2(10) . . ? C8 C10 C11 108.5(10) . . ? C9 C10 C11 111.2(9) . . ? C8 C10 H10 107.9 . . ? C9 C10 H10 107.9 . . ? C11 C10 H10 107.9 . . ? N4 C11 C12 100.7(7) . . ? N4 C11 C10 108.8(8) . . ? C12 C11 C10 114.3(7) . . ? N4 C11 H11 110.9 . . ? C12 C11 H11 110.9 . . ? C10 C11 H11 110.9 . . ? O1 C12 C11 105.3(8) . . ? O1 C12 H12A 110.7 . . ? C11 C12 H12A 110.7 . . ? O1 C12 H12B 110.7 . . ? C11 C12 H12B 110.7 . . ? H12A C12 H12B 108.8 . . ? N4 C13 O1 119.5(9) . . ? N4 C13 C14 121.6(8) . . ? O1 C13 C14 118.6(8) . . ? N5 C14 C15 119.6(12) . . ? N5 C14 C13 109.7(8) . . ? C15 C14 C13 130.7(11) . . ? C16 C15 C14 119.5(13) . . ? C16 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? C15 C16 C17 120.5(10) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C18 C17 C16 116.5(12) . . ? C18 C17 H17 121.7 . . ? C16 C17 H17 121.7 . . ? N5 C18 C17 120.8(11) . . ? N5 C18 C19 112.5(7) . . ? C17 C18 C19 126.6(10) . . ? N6 C19 O2 120.0(9) . . ? N6 C19 C18 117.9(7) . . ? O2 C19 C18 122.1(8) . . ? O2 C20 C21 105.8(8) . . ? O2 C20 H20A 110.6 . . ? C21 C20 H20A 110.6 . . ? O2 C20 H20B 110.6 . . ? C21 C20 H20B 110.6 . . ? H20A C20 H20B 108.7 . . ? N6 C21 C20 100.6(9) . . ? N6 C21 C22 109.3(6) . . ? C20 C21 C22 113.8(8) . . ? N6 C21 H21 110.9 . . ? C20 C21 H21 110.9 . . ? C22 C21 H21 110.9 . . ? C23 C22 C24 112.0(9) . . ? C23 C22 C21 111.3(9) . . ? C24 C22 C21 108.9(8) . . ? C23 C22 H22 108.2 . . ? C24 C22 H22 108.2 . . ? C21 C22 H22 108.2 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C7 N1 C1 110.5(5) . . ? C7 N1 C6 108.3(6) . . ? C1 N1 C6 111.1(5) . . ? C7 N1 C4 108.1(6) . . ? C1 N1 C4 110.9(5) . . ? C6 N1 C4 107.8(5) . . ? C4 N2 C2 112.9(7) . . ? C4 N2 C5 109.9(7) . . ? C2 N2 C5 112.8(7) . . ? C5 N3 C3 112.9(7) . . ? C5 N3 C6 112.4(6) . . ? C3 N3 C6 111.7(6) . . ? C13 N4 C11 108.2(6) . . ? C13 N4 Ru1 112.9(6) . . ? C11 N4 Ru1 138.9(5) . . ? C14 N5 C18 123.1(8) . . ? C14 N5 Ru1 119.3(6) . . ? C18 N5 Ru1 117.6(6) . . ? C19 N6 C21 104.6(7) . . ? C19 N6 Ru1 114.4(6) . . ? C21 N6 Ru1 140.9(5) . . ? C13 O1 C12 102.9(7) . . ? C19 O2 C20 103.6(7) . . ? C3 P1 C2 96.4(4) . . ? C3 P1 C1 97.3(3) . . ? C2 P1 C1 96.6(3) . . ? C3 P1 Ru1 121.1(3) . . ? C2 P1 Ru1 119.9(3) . . ? C1 P1 Ru1 119.9(2) . . ? N5 Ru1 N6 77.4(3) . . ? N5 Ru1 N4 75.9(3) . . ? N6 Ru1 N4 153.3(3) . . ? N5 Ru1 P1 176.48(17) . . ? N6 Ru1 P1 104.43(18) . . ? N4 Ru1 P1 102.20(19) . . ? N5 Ru1 Cl1 90.19(15) . . ? N6 Ru1 Cl1 90.66(18) . . ? N4 Ru1 Cl1 89.17(15) . . ? P1 Ru1 Cl1 86.78(6) . . ? N5 Ru1 Cl2 91.38(15) . . ? N6 Ru1 Cl2 88.50(18) . . ? N4 Ru1 Cl2 92.39(16) . . ? P1 Ru1 Cl2 91.69(6) . . ? Cl1 Ru1 Cl2 178.01(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C8 C10 C11 N4 -171.1(9) . . . . ? C9 C10 C11 N4 63.8(10) . . . . ? C8 C10 C11 C12 77.3(13) . . . . ? C9 C10 C11 C12 -47.8(12) . . . . ? N4 C11 C12 O1 -17.9(9) . . . . ? C10 C11 C12 O1 98.5(9) . . . . ? N4 C13 C14 N5 4.2(10) . . . . ? O1 C13 C14 N5 179.2(7) . . . . ? N4 C13 C14 C15 -174.0(9) . . . . ? O1 C13 C14 C15 1.1(13) . . . . ? N5 C14 C15 C16 -0.6(15) . . . . ? C13 C14 C15 C16 177.4(10) . . . . ? C14 C15 C16 C17 2.3(17) . . . . ? C15 C16 C17 C18 -2.6(16) . . . . ? C16 C17 C18 N5 1.2(13) . . . . ? C16 C17 C18 C19 177.1(9) . . . . ? N5 C18 C19 N6 0.8(11) . . . . ? C17 C18 C19 N6 -175.4(8) . . . . ? N5 C18 C19 O2 -179.4(7) . . . . ? C17 C18 C19 O2 4.4(14) . . . . ? O2 C20 C21 N6 -23.1(10) . . . . ? O2 C20 C21 C22 93.6(10) . . . . ? N6 C21 C22 C23 66.9(10) . . . . ? C20 C21 C22 C23 -44.6(11) . . . . ? N6 C21 C22 C24 -169.2(9) . . . . ? C20 C21 C22 C24 79.3(12) . . . . ? P1 C1 N1 C7 179.3(5) . . . . ? P1 C1 N1 C6 -60.4(6) . . . . ? P1 C1 N1 C4 59.4(6) . . . . ? N3 C6 N1 C7 -170.3(6) . . . . ? N3 C6 N1 C1 68.2(7) . . . . ? N3 C6 N1 C4 -53.5(7) . . . . ? N2 C4 N1 C7 173.6(7) . . . . ? N2 C4 N1 C1 -65.1(8) . . . . ? N2 C4 N1 C6 56.7(8) . . . . ? N1 C4 N2 C2 67.9(9) . . . . ? N1 C4 N2 C5 -58.9(9) . . . . ? P1 C2 N2 C4 -64.6(9) . . . . ? P1 C2 N2 C5 60.7(8) . . . . ? N3 C5 N2 C4 59.7(9) . . . . ? N3 C5 N2 C2 -67.2(8) . . . . ? N2 C5 N3 C3 67.8(8) . . . . ? N2 C5 N3 C6 -59.7(9) . . . . ? P1 C3 N3 C5 -61.8(7) . . . . ? P1 C3 N3 C6 66.0(8) . . . . ? N1 C6 N3 C5 57.0(8) . . . . ? N1 C6 N3 C3 -71.2(8) . . . . ? O1 C13 N4 C11 -3.9(10) . . . . ? C14 C13 N4 C11 171.1(7) . . . . ? O1 C13 N4 Ru1 177.1(6) . . . . ? C14 C13 N4 Ru1 -7.9(9) . . . . ? C12 C11 N4 C13 13.6(9) . . . . ? C10 C11 N4 C13 -106.9(8) . . . . ? C12 C11 N4 Ru1 -167.8(6) . . . . ? C10 C11 N4 Ru1 71.8(10) . . . . ? C15 C14 N5 C18 -0.8(12) . . . . ? C13 C14 N5 C18 -179.2(6) . . . . ? C15 C14 N5 Ru1 -179.5(7) . . . . ? C13 C14 N5 Ru1 2.1(8) . . . . ? C17 C18 N5 C14 0.5(11) . . . . ? C19 C18 N5 C14 -176.0(7) . . . . ? C17 C18 N5 Ru1 179.2(6) . . . . ? C19 C18 N5 Ru1 2.7(8) . . . . ? O2 C19 N6 C21 -6.9(11) . . . . ? C18 C19 N6 C21 172.9(7) . . . . ? O2 C19 N6 Ru1 176.4(6) . . . . ? C18 C19 N6 Ru1 -3.8(9) . . . . ? C20 C21 N6 C19 18.0(9) . . . . ? C22 C21 N6 C19 -102.0(8) . . . . ? C20 C21 N6 Ru1 -166.8(7) . . . . ? C22 C21 N6 Ru1 73.2(11) . . . . ? N4 C13 O1 C12 -8.4(10) . . . . ? C14 C13 O1 C12 176.4(7) . . . . ? C11 C12 O1 C13 16.2(9) . . . . ? N6 C19 O2 C20 -8.6(11) . . . . ? C18 C19 O2 C20 171.6(9) . . . . ? C21 C20 O2 C19 19.8(11) . . . . ? N3 C3 P1 C2 47.8(7) . . . . ? N3 C3 P1 C1 -49.8(6) . . . . ? N3 C3 P1 Ru1 178.6(5) . . . . ? N2 C2 P1 C3 -47.4(7) . . . . ? N2 C2 P1 C1 50.8(7) . . . . ? N2 C2 P1 Ru1 -179.0(5) . . . . ? N1 C1 P1 C3 47.6(5) . . . . ? N1 C1 P1 C2 -49.7(6) . . . . ? N1 C1 P1 Ru1 -180.0(4) . . . . ? C14 N5 Ru1 N6 175.2(6) . . . . ? C18 N5 Ru1 N6 -3.6(5) . . . . ? C14 N5 Ru1 N4 -4.6(5) . . . . ? C18 N5 Ru1 N4 176.7(5) . . . . ? C14 N5 Ru1 P1 54(4) . . . . ? C18 N5 Ru1 P1 -125(3) . . . . ? C14 N5 Ru1 Cl1 84.5(5) . . . . ? C18 N5 Ru1 Cl1 -94.2(5) . . . . ? C14 N5 Ru1 Cl2 -96.7(5) . . . . ? C18 N5 Ru1 Cl2 84.5(5) . . . . ? C19 N6 Ru1 N5 3.9(5) . . . . ? C21 N6 Ru1 N5 -171.0(9) . . . . ? C19 N6 Ru1 N4 4.5(9) . . . . ? C21 N6 Ru1 N4 -170.4(7) . . . . ? C19 N6 Ru1 P1 -179.2(5) . . . . ? C21 N6 Ru1 P1 5.9(9) . . . . ? C19 N6 Ru1 Cl1 94.0(6) . . . . ? C21 N6 Ru1 Cl1 -80.9(8) . . . . ? C19 N6 Ru1 Cl2 -87.8(6) . . . . ? C21 N6 Ru1 Cl2 97.3(8) . . . . ? C13 N4 Ru1 N5 6.4(5) . . . . ? C11 N4 Ru1 N5 -172.2(8) . . . . ? C13 N4 Ru1 N6 5.8(8) . . . . ? C11 N4 Ru1 N6 -172.8(7) . . . . ? C13 N4 Ru1 P1 -170.5(5) . . . . ? C11 N4 Ru1 P1 10.8(8) . . . . ? C13 N4 Ru1 Cl1 -84.0(5) . . . . ? C11 N4 Ru1 Cl1 97.4(7) . . . . ? C13 N4 Ru1 Cl2 97.2(5) . . . . ? C11 N4 Ru1 Cl2 -81.4(7) . . . . ? C3 P1 Ru1 N5 -47(4) . . . . ? C2 P1 Ru1 N5 73(4) . . . . ? C1 P1 Ru1 N5 -168(4) . . . . ? C3 P1 Ru1 N6 -167.3(4) . . . . ? C2 P1 Ru1 N6 -47.4(4) . . . . ? C1 P1 Ru1 N6 71.6(3) . . . . ? C3 P1 Ru1 N4 11.0(4) . . . . ? C2 P1 Ru1 N4 130.9(4) . . . . ? C1 P1 Ru1 N4 -110.1(3) . . . . ? C3 P1 Ru1 Cl1 -77.4(3) . . . . ? C2 P1 Ru1 Cl1 42.4(4) . . . . ? C1 P1 Ru1 Cl1 161.4(3) . . . . ? C3 P1 Ru1 Cl2 103.9(3) . . . . ? C2 P1 Ru1 Cl2 -136.3(4) . . . . ? C1 P1 Ru1 Cl2 -17.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 67.00 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 1.287 _refine_diff_density_min -0.683 _refine_diff_density_rms 0.097 #===END _database_code_depnum_ccdc_archive 'CCDC 937043'