# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global #TrackingRef _journal_coden_Cambridge 182 _publ_section_title ;Synthesis and Characterization of the Tetraphosphine Complexes trans-MCl2(PH3)4 (M = Ru, Os) ; _publ_section_abstract ;The air stable tetraphosphine complexes trans-MCl2(PH3)4 (M = Ru, Os) are formed in high yield from the reaction of MCl3 * 3 H2O with PH3 in methanol at 70 \%C. ; _publ_requested_journal Chem.Commun. _publ_contact_author_name 'Richard A. Jones' _publ_contact_author_address ;Department of Chemistry and Biochemistry The University of Texas at Austin 1 University Station A5300 Austin, Texas, 78712-0165 ; _publ_contact_author_email rajones@mail.utexas.edu _publ_contact_author_phone '(512) 471-1706' loop_ _publ_author_name _publ_author_address 'Justin W. Hall' ;Department of Chemistry and Biochemistry The University of Texas at Austin 1 University Station A5300 Austin, Texas, 78712-0165 ; 'William J. McCarty' ;Department of Chemistry and Biochemistry The University of Texas at Austin 1 University Station A5300 Austin, Texas, 78712-0165 ; 'Xiaoping Yang.' ;Department of Chemistry and Biochemistry The University of Texas at Austin 1 University Station A5300 Austin, Texas, 78712-0165 ; 'Richard A. Jones' ;Department of Chemistry and Biochemistry The University of Texas at Austin 1 University Station A5300 Austin, Texas, 78712-0165 ; _publ_section_comment none _publ_section_references ; Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (2008). SHELXL-97. Acat Cryst., A64, 112-122. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; data_trans-OsCl2(PH3)4 _database_code_depnum_ccdc_archive 'CCDC 775884' #TrackingRef 'trans-OsCl2-PH3-4.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic trans-dichloridotetraphosphaneosmium _chemical_name_common . _chemical_formula_moiety 'Cl2 H12 Os P4' _chemical_formula_sum 'Cl2 H12 Os P4' _exptl_crystal_recrystallization_method 'crystallized from methanol at -50 \%C' _chemical_melting_point . _exptl_crystal_description 'clear tetragonal crystals' _exptl_crystal_colour 'intense yellow' _diffrn_ambient_temperature 153(1) _diffrn_ambient_pressure . _chemical_formula_weight 397.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Os Os -1.2165 7.6030 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 42/m n m' _symmetry_Int_Tables_number 136 _chemical_absolute_configuration . _symmetry_space_group_name_Hall '-P 4n 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+1/2, x+1/2, z+1/2' '-x, -y, z' 'y+1/2, -x+1/2, z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y, x, -z' '-x+1/2, y+1/2, -z+1/2' '-y, -x, -z' '-x, -y, -z' 'y-1/2, -x-1/2, -z-1/2' 'x, y, -z' '-y-1/2, x-1/2, -z-1/2' '-x-1/2, y-1/2, z-1/2' '-y, -x, z' 'x-1/2, -y-1/2, z-1/2' 'y, x, z' _cell_length_a 6.5759(9) _cell_length_b 6.5759(9) _cell_length_c 11.744(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 507.84(13) _cell_formula_units_Z 2 _cell_measurement_temperature 153(1) _cell_measurement_reflns_used 1165 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 2.597 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 364 _exptl_absorpt_coefficient_mu 13.628 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.716 _exptl_absorpt_correction_T_max 0.876 _exptl_absorpt_process_details 'Scalepack (Otwinoski and Minor, 1997)' _exptl_special_details none _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f-scans and \w-scans to fill asymmetric unit' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 2954 _diffrn_reflns_av_R_equivalents 0.0495 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.47 _diffrn_reflns_theta_max 27.47 _reflns_number_total 344 _reflns_number_gt 302 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction 'Denzo (Otwinoski and Minor, 1997)' _computing_structure_solution 'XS SHELXTL/PC v5.1, Bruker AXS' _computing_structure_refinement 'XL SHELXTL/PC v5.1, Bruker AXS' _computing_molecular_graphics 'XP SHELXTL/PC v5.1, Bruker AXS' _computing_publication_material . _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Rotational disorder of the hydrogen positions due to rotation of phosphine about the Ru-P bond was refined by assignment of two rotationally antiparallel groups, whose site occupancy factors were refined subject to restraint of the sum to unity. The P-H bond lengths, H-H distances, and Ru-H distances were restrained to be equal and the distances refined. A single isotropic displacement parameter was assigned for all of the hydrogens and refined. ; _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^)+(0.0120P)^2^+0.9560P] 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 344 _refine_ls_number_parameters 26 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.0245 _refine_ls_R_factor_gt 0.0189 _refine_ls_wR_factor_ref 0.0393 _refine_ls_wR_factor_gt 0.0375 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.037 _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 Os1 Os 0.5000 0.5000 0.0000 0.02333(14) Uani 1 8 d SD . . Cl1 Cl 0.23727(19) 0.23727(19) 0.0000 0.0367(4) Uani 1 4 d S . . P1 P 0.32129(14) 0.67871(14) 0.13659(12) 0.0327(3) Uani 1 2 d SD . . H1 H 0.3565(19) 0.6435(19) 0.2474(12) 0.050(14) Uiso 0.76(5) 2 d SPD A 1 H2 H 0.3345(17) 0.882(2) 0.1405(12) 0.050(14) Uiso 0.76(5) 1 d PD A 1 H2Z H 0.421(3) 0.7953(14) 0.2117(10) 0.050(14) Uiso 0.24(5) 1 d PD A 2 H1Z H 0.1827(15) 0.8173(15) 0.1048(15) 0.050(14) Uiso 0.24(5) 2 d SPD A 2 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 Os1 0.02466(16) 0.02466(16) 0.0207(2) 0.000 0.000 0.00181(16) Cl1 0.0360(6) 0.0360(6) 0.0382(9) 0.000 0.000 -0.0096(7) P1 0.0353(4) 0.0353(4) 0.0277(6) -0.0034(4) 0.0034(4) 0.0053(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 Os1 P1 2.3099(13) 9_665 ? Os1 P1 2.3099(13) 11 ? Os1 P1 2.3099(13) 3_665 ? Os1 P1 2.3099(13) . ? Os1 Cl1 2.4433(18) 9_665 ? Os1 Cl1 2.4433(18) . ? P1 H1 1.342(14) . ? P1 H2 1.342(14) . ? P1 H2Z 1.342(14) . ? P1 H1Z 1.342(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 P1 Os1 P1 92.03(7) 9_665 11 ? P1 Os1 P1 87.97(7) 9_665 3_665 ? P1 Os1 P1 180.00(5) 11 3_665 ? P1 Os1 P1 180.00(4) 9_665 . ? P1 Os1 P1 87.97(7) 11 . ? P1 Os1 P1 92.03(7) 3_665 . ? P1 Os1 Cl1 90.0 9_665 9_665 ? P1 Os1 Cl1 90.0 11 9_665 ? P1 Os1 Cl1 90.0 3_665 9_665 ? P1 Os1 Cl1 90.0 . 9_665 ? P1 Os1 Cl1 90.0 9_665 . ? P1 Os1 Cl1 90.0 11 . ? P1 Os1 Cl1 90.0 3_665 . ? P1 Os1 Cl1 90.0 . . ? Cl1 Os1 Cl1 180.0 9_665 . ? Os1 P1 H1 119.9(8) . . ? Os1 P1 H2 119.9(8) . . ? H1 P1 H2 97.4(10) . . ? Os1 P1 H2Z 119.9(8) . . ? H1 P1 H2Z 51.4(4) . . ? H2 P1 H2Z 51.4(4) . . ? Os1 P1 H1Z 119.9(8) . . ? H1 P1 H1Z 120.3(15) . . ? H2 P1 H1Z 51.4(4) . . ? H2Z P1 H1Z 97.4(10) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.173 _refine_diff_density_min -0.544 _refine_diff_density_rms 0.122 # Attachment 'trans-RuCl2-PH3-4.CIF.txt' data_trans-RuCl2(PH3)4 _database_code_depnum_ccdc_archive 'CCDC 775885' _publ_section_abstract ;The air stable tetraphosphine complexes trans-MCl2(PH3)4 (M = Ru, Os) are formed in high yield from the reaction of MCl3 * 3 H2O with PH3 in methanol at 70 \%C. ; _publ_section_comment none _publ_section_references ; Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (2008). SHELXL-97. Acat Cryst., A64, 112-122. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _audit_creation_method SHELXL-97 _chemical_name_systematic trans-dichloridotetraphosphaneruthenium _chemical_name_common . _chemical_formula_moiety 'Cl2 H12 P4 Ru' _chemical_formula_sum 'Cl2 H12 P4 Ru' _exptl_crystal_recrystallization_method 'crystallized from methanol at -50 \%C' _chemical_melting_point . _exptl_crystal_description 'clear tetragonal crystals' _exptl_crystal_colour 'intense yellow' _diffrn_ambient_temperature 153(1) _chemical_formula_weight 307.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 42/m n m' _symmetry_space_group_name_Hall '-P 4n 2n' _symmetry_int_tables_number 136 _chemical_absolute_configuration . loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+1/2, x+1/2, z+1/2' '-x, -y, z' 'y+1/2, -x+1/2, z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y, x, -z' '-x+1/2, y+1/2, -z+1/2' '-y, -x, -z' '-x, -y, -z' 'y-1/2, -x-1/2, -z-1/2' 'x, y, -z' '-y-1/2, x-1/2, -z-1/2' '-x-1/2, y-1/2, z-1/2' '-y, -x, z' 'x-1/2, -y-1/2, z-1/2' 'y, x, z' _cell_length_a 6.5817(9) _cell_length_b 6.5817(9) _cell_length_c 11.726(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 507.96(13) _cell_formula_units_Z 2 _cell_measurement_temperature 153(1) _cell_measurement_reflns_used 593 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 2.013 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 300 _exptl_absorpt_coefficient_mu 2.616 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.783 _exptl_absorpt_correction_T_max 0.880 _exptl_absorpt_process_details 'Scalepack (Otwinoski and Minor, 1997)' _exptl_special_details . _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f-scans and \w-scans to fill asymmetric unit' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 996 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0313 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 27.48 _reflns_number_total 339 _reflns_number_gt 313 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction 'Denzo (Otwinoski and Minor, 1997)' _computing_structure_solution 'XS SHELXTL/PC v5.1, Bruker AXS' _computing_structure_refinement 'XL SHELXTL/PC v5.1, Bruker AXS' _computing_molecular_graphics 'XP SHELXTL/PC v5.1, Bruker AXS' _computing_publication_material . _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Rotational disorder of the hydrogen positions due to rotation of phosphine about the Ru-P bond was refined by assignment of two rotationally antiparallel groups, whose site occupancy factors were refined subject to restraint of the sum to unity. The P-H bond lengths, H-H distances, and Ru-H distances were restrained to be equal and the distances refined. A single isotropic displacement parameter was assigned for all of the hydrogens and refined. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.1820P] 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 339 _refine_ls_number_parameters 26 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.0190 _refine_ls_R_factor_gt 0.0160 _refine_ls_wR_factor_ref 0.0373 _refine_ls_wR_factor_gt 0.0364 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.069 _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 0.5000 0.5000 0.0000 0.02161(14) Uani 1 8 d SD . . Cl1 Cl 0.23920(9) 0.23920(9) 0.0000 0.0365(2) Uani 1 4 d S . . P1 P 0.67916(7) 0.32084(7) 0.13618(5) 0.03079(19) Uani 1 2 d SD . . H1 H 0.6471(15) 0.3529(15) 0.2405(9) 0.053(8) Uiso 0.77(3) 2 d SPD A 1 H2 H 0.8699(16) 0.3328(13) 0.1398(9) 0.053(8) Uiso 0.77(3) 1 d PD A 1 H1Z H 0.8090(11) 0.1910(11) 0.1063(12) 0.053(8) Uiso 0.23(3) 2 d SPD A 2 H2Z H 0.7890(10) 0.414(2) 0.2069(7) 0.053(8) Uiso 0.23(3) 1 d PD A 2 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 0.02218(16) 0.02218(16) 0.0205(2) 0.000 0.000 0.00075(13) Cl1 0.0340(3) 0.0340(3) 0.0414(5) 0.000 0.000 -0.0105(4) P1 0.0324(2) 0.0324(2) 0.0276(3) 0.00396(19) -0.00396(19) 0.0028(2) _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 P1 2.3088(7) . ? Ru1 P1 2.3088(7) 3_665 ? Ru1 P1 2.3088(7) 9_665 ? Ru1 P1 2.3088(7) 11 ? Ru1 Cl1 2.4275(9) . ? Ru1 Cl1 2.4275(9) 9_665 ? P1 H1 1.259(10) . ? P1 H2 1.259(10) . ? P1 H1Z 1.259(10) . ? P1 H2Z 1.259(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 P1 Ru1 P1 92.48(3) . 3_665 ? P1 Ru1 P1 180.0 . 9_665 ? P1 Ru1 P1 87.52(3) 3_665 9_665 ? P1 Ru1 P1 87.52(3) . 11 ? P1 Ru1 P1 180.0 3_665 11 ? P1 Ru1 P1 92.48(3) 9_665 11 ? P1 Ru1 Cl1 90.0 . . ? P1 Ru1 Cl1 90.0 3_665 . ? P1 Ru1 Cl1 90.0 9_665 . ? P1 Ru1 Cl1 90.0 11 . ? P1 Ru1 Cl1 90.0 . 9_665 ? P1 Ru1 Cl1 90.0 3_665 9_665 ? P1 Ru1 Cl1 90.0 9_665 9_665 ? P1 Ru1 Cl1 90.0 11 9_665 ? Cl1 Ru1 Cl1 180.0 . 9_665 ? Ru1 P1 H1 120.1(6) . . ? Ru1 P1 H2 120.1(6) . . ? H1 P1 H2 97.1(8) . . ? Ru1 P1 H1Z 120.1(6) . . ? H1 P1 H1Z 119.9(12) . . ? H2 P1 H1Z 51.3(3) . . ? Ru1 P1 H2Z 120.1(6) . . ? H1 P1 H2Z 51.3(3) . . ? H2 P1 H2Z 51.3(4) . . ? H1Z P1 H2Z 97.1(8) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.225 _refine_diff_density_min -0.484 _refine_diff_density_rms 0.066