# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _journal_coden_Cambridge 440 _publ_requested_journal 'New Journal of Chemistry' loop_ _publ_author_name 'Datta, Dipankar' 'Drew, M.' 'Pal, P. K.' _publ_contact_author_name 'Dr Dipankar Datta' _publ_contact_author_address ; Department of Inorganic Chemistry Indian Association for the Cultivation of Science Calcutta 700 032 INDIA ; _publ_contact_author_email 'ICDD@MAHENDRA.IACS.RES.IN' _publ_section_title ; Two simple precursor 2,2'-bisoxazline complexes of ruthenium ; _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands ; data_Ru(1a)2Cl2 _database_code_CSD 174511 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H32 Cl2 N4 O4 Ru' _chemical_formula_weight 564.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z' '-x, -y, -z' '-x-1/2, y-1/2, -z' _cell_length_a 15.42(2) _cell_length_b 9.832(14) _cell_length_c 16.076(19) _cell_angle_alpha 90.00 _cell_angle_beta 96.673(10) _cell_angle_gamma 90.00 _cell_volume 2421(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.549 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 0.901 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6185 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_sigmaI/netI 0.0490 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 25.98 _reflns_number_total 3926 _reflns_number_gt 2696 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0919P)^2^+0.0000P] 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 SHELXL _refine_ls_extinction_coef 0.0061(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3926 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0857 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1429 _refine_ls_wR_factor_gt 0.1207 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.80153(3) 0.50012(4) 0.75190(2) 0.02540(18) Uani 1 d . . . Cl2 Cl 0.73909(10) 0.27962(13) 0.71401(9) 0.0420(4) Uani 1 d . . . Cl3 Cl 0.66941(11) 0.58672(16) 0.79990(10) 0.0536(4) Uani 1 d . . . N10A N 0.9111(3) 0.4404(4) 0.6956(2) 0.0264(9) Uani 1 d . . . C9A C 0.9985(4) 0.3735(5) 0.7175(3) 0.0319(12) Uani 1 d . . . C8A C 1.0401(4) 0.3941(7) 0.6369(4) 0.0531(16) Uani 1 d . . . H8A1 H 1.0812 0.4690 0.6430 0.064 Uiso 1 calc R . . H8A2 H 1.0707 0.3125 0.6230 0.064 Uiso 1 calc R . . O7A O 0.9688(3) 0.4239(5) 0.5721(2) 0.0546(11) Uani 1 d . . . C6A C 0.9031(4) 0.4586(6) 0.6161(4) 0.0406(14) Uani 1 d . . . C5A C 0.8222(4) 0.5201(5) 0.5773(3) 0.0401(14) Uani 1 d . . . O4A O 0.8044(3) 0.5368(5) 0.4947(2) 0.0606(13) Uani 1 d . . . C3A C 0.7218(5) 0.6098(8) 0.4846(4) 0.069(2) Uani 1 d . . . H3A1 H 0.6816 0.5683 0.4411 0.083 Uiso 1 calc R . . H3A2 H 0.7307 0.7040 0.4697 0.083 Uiso 1 calc R . . C2A C 0.6859(4) 0.6008(6) 0.5697(4) 0.0455(15) Uani 1 d . . . N1A N 0.7669(3) 0.5566(4) 0.6266(3) 0.0329(10) Uani 1 d . . . C91A C 0.9812(5) 0.2222(6) 0.7310(5) 0.064(2) Uani 1 d . . . H91A H 1.0355 0.1766 0.7480 0.077 Uiso 1 calc R . . H91B H 0.9542 0.1830 0.6798 0.077 Uiso 1 calc R . . H91C H 0.9432 0.2121 0.7739 0.077 Uiso 1 calc R . . C92A C 1.0493(5) 0.4398(8) 0.7920(4) 0.068(2) Uani 1 d . . . H92A H 1.0566 0.5348 0.7808 0.081 Uiso 1 calc R . . H92B H 1.1056 0.3974 0.8029 0.081 Uiso 1 calc R . . H92C H 1.0182 0.4297 0.8401 0.081 Uiso 1 calc R . . C21A C 0.6190(5) 0.4893(8) 0.5715(5) 0.072(2) Uani 1 d . . . H21A H 0.6420 0.4060 0.5519 0.086 Uiso 1 calc R . . H21B H 0.5669 0.5137 0.5359 0.086 Uiso 1 calc R . . H21C H 0.6053 0.4773 0.6278 0.086 Uiso 1 calc R . . C22A C 0.6526(5) 0.7377(7) 0.5976(5) 0.068(2) Uani 1 d . . . H22A H 0.6031 0.7654 0.5596 0.082 Uiso 1 calc R . . H22B H 0.6980 0.8045 0.5977 0.082 Uiso 1 calc R . . H22C H 0.6357 0.7293 0.6530 0.082 Uiso 1 calc R . . N10B N 0.8645(3) 0.6760(4) 0.7991(3) 0.0311(10) Uani 1 d . . . C9B C 0.8839(4) 0.8172(5) 0.7717(4) 0.0421(14) Uani 1 d . . . C8B C 0.9505(5) 0.8643(6) 0.8438(4) 0.0564(17) Uani 1 d . . . H8B1 H 1.0095 0.8537 0.8294 0.068 Uiso 1 calc R . . H8B2 H 0.9412 0.9590 0.8571 0.068 Uiso 1 calc R . . O7B O 0.9360(3) 0.7764(4) 0.9149(2) 0.0487(11) Uani 1 d . . . C6B C 0.8929(4) 0.6694(5) 0.8772(3) 0.0372(13) Uani 1 d . . . C5B C 0.8765(4) 0.5458(5) 0.9222(3) 0.0364(13) Uani 1 d . . . O4B O 0.8946(3) 0.5322(4) 1.0051(2) 0.0513(12) Uani 1 d . . . C3B C 0.8656(5) 0.3974(6) 1.0224(4) 0.0600(19) Uani 1 d . . . H3B1 H 0.8253 0.4004 1.0644 0.072 Uiso 1 calc R . . H3B2 H 0.9149 0.3407 1.0431 0.072 Uiso 1 calc R . . C2B C 0.8197(4) 0.3394(5) 0.9395(3) 0.0422(15) Uani 1 d . . . N1B N 0.8392(3) 0.4481(4) 0.8777(2) 0.0310(10) Uani 1 d . . . C91B C 0.7993(5) 0.8992(6) 0.7660(5) 0.0622(19) Uani 1 d . . . H91D H 0.7545 0.8524 0.7305 0.075 Uiso 1 calc R . . H91E H 0.8086 0.9873 0.7430 0.075 Uiso 1 calc R . . H91F H 0.7814 0.9093 0.8209 0.075 Uiso 1 calc R . . C92B C 0.9222(5) 0.8163(7) 0.6886(4) 0.0624(19) Uani 1 d . . . H92D H 0.8807 0.7777 0.6460 0.075 Uiso 1 calc R . . H92E H 0.9747 0.7629 0.6940 0.075 Uiso 1 calc R . . H92F H 0.9355 0.9078 0.6734 0.075 Uiso 1 calc R . . C21B C 0.7208(5) 0.3296(9) 0.9400(5) 0.075(2) Uani 1 d . . . H21D H 0.6991 0.4138 0.9598 0.090 Uiso 1 calc R . . H21E H 0.7075 0.2569 0.9763 0.090 Uiso 1 calc R . . H21F H 0.6936 0.3121 0.8842 0.090 Uiso 1 calc R . . C22B C 0.8600(7) 0.2050(6) 0.9197(4) 0.077(3) Uani 1 d . . . H22D H 0.8321 0.1714 0.8673 0.093 Uiso 1 calc R . . H22E H 0.8522 0.1408 0.9633 0.093 Uiso 1 calc R . . H22F H 0.9212 0.2174 0.9162 0.093 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0209(3) 0.0235(2) 0.0325(3) 0.00019(15) 0.00652(16) -0.00093(16) Cl2 0.0436(9) 0.0333(7) 0.0482(8) -0.0022(5) 0.0010(6) -0.0138(6) Cl3 0.0328(9) 0.0584(9) 0.0734(10) 0.0047(7) 0.0225(7) 0.0099(7) N10A 0.027(3) 0.026(2) 0.026(2) -0.0008(15) 0.0011(17) -0.0025(17) C9A 0.024(3) 0.036(3) 0.036(3) -0.002(2) 0.005(2) 0.009(2) C8A 0.034(4) 0.071(4) 0.056(4) 0.005(3) 0.017(3) 0.012(3) O7A 0.047(3) 0.079(3) 0.040(2) 0.002(2) 0.0185(19) 0.016(2) C6A 0.039(4) 0.037(3) 0.048(3) -0.002(2) 0.013(3) 0.003(2) C5A 0.043(4) 0.045(3) 0.033(3) 0.007(2) 0.005(2) 0.002(3) O4A 0.064(4) 0.086(3) 0.032(2) 0.0116(19) 0.005(2) 0.018(3) C3A 0.060(5) 0.093(5) 0.053(4) 0.016(4) -0.002(4) 0.012(4) C2A 0.038(4) 0.051(3) 0.045(3) 0.012(3) -0.006(3) 0.009(3) N1A 0.026(3) 0.037(2) 0.035(2) 0.0039(18) 0.0023(19) 0.0008(19) C91A 0.054(5) 0.047(4) 0.094(5) 0.006(3) 0.019(4) 0.024(3) C92A 0.037(4) 0.096(5) 0.066(4) -0.030(4) -0.008(3) 0.017(4) C21A 0.036(5) 0.090(6) 0.084(5) 0.027(4) -0.019(4) -0.013(4) C22A 0.058(5) 0.071(5) 0.073(5) 0.023(4) -0.004(4) 0.019(4) N10B 0.029(3) 0.023(2) 0.042(3) -0.0041(17) 0.011(2) -0.0019(17) C9B 0.047(4) 0.026(3) 0.057(4) -0.001(2) 0.016(3) -0.001(2) C8B 0.056(5) 0.038(3) 0.077(4) -0.006(3) 0.016(3) -0.016(3) O7B 0.053(3) 0.039(2) 0.055(2) -0.0127(18) 0.010(2) -0.0178(19) C6B 0.034(4) 0.028(3) 0.052(4) -0.011(2) 0.013(3) -0.005(2) C5B 0.034(4) 0.037(3) 0.041(3) -0.004(2) 0.015(2) -0.001(2) O4B 0.071(4) 0.054(2) 0.028(2) -0.0073(16) 0.002(2) -0.009(2) C3B 0.083(6) 0.051(4) 0.044(3) 0.006(3) 0.000(3) -0.011(4) C2B 0.060(5) 0.036(3) 0.032(3) 0.005(2) 0.011(3) -0.002(3) N1B 0.029(3) 0.027(2) 0.037(2) -0.0019(17) 0.0077(19) -0.0008(19) C91B 0.058(5) 0.034(3) 0.095(5) 0.000(3) 0.011(4) 0.004(3) C92B 0.083(6) 0.042(3) 0.066(4) 0.003(3) 0.026(4) -0.012(3) C21B 0.069(6) 0.093(6) 0.065(5) 0.015(4) 0.020(4) -0.035(4) C22B 0.138(9) 0.039(4) 0.060(4) 0.015(3) 0.031(4) 0.014(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N10B 2.082(4) . ? Ru1 N10A 2.091(5) . ? Ru1 N1A 2.098(5) . ? Ru1 N1B 2.102(5) . ? Ru1 Cl3 2.416(3) . ? Ru1 Cl2 2.421(3) . ? N10A C6A 1.282(7) . ? N10A C9A 1.505(7) . ? C9A C92A 1.502(8) . ? C9A C8A 1.524(8) . ? C9A C91A 1.532(8) . ? C8A O7A 1.454(7) . ? O7A C6A 1.345(7) . ? C6A C5A 1.460(9) . ? C5A N1A 1.280(8) . ? C5A O4A 1.334(7) . ? O4A C3A 1.454(9) . ? C3A C2A 1.536(10) . ? C2A C21A 1.509(9) . ? C2A N1A 1.523(7) . ? C2A C22A 1.528(9) . ? N10B C6B 1.282(7) . ? N10B C9B 1.498(7) . ? C9B C92B 1.522(9) . ? C9B C91B 1.527(9) . ? C9B C8B 1.528(8) . ? C8B O7B 1.470(8) . ? O7B C6B 1.349(6) . ? C6B C5B 1.452(8) . ? C5B N1B 1.292(7) . ? C5B O4B 1.337(7) . ? O4B C3B 1.437(8) . ? C3B C2B 1.544(8) . ? C2B C22B 1.509(9) . ? C2B N1B 1.513(7) . ? C2B C21B 1.529(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 N10B Ru1 N10A 91.47(18) . . ? N10B Ru1 N1A 100.74(18) . . ? N10A Ru1 N1A 77.68(17) . . ? N10B Ru1 N1B 77.64(17) . . ? N10A Ru1 N1B 101.64(17) . . ? N1A Ru1 N1B 178.25(16) . . ? N10B Ru1 Cl3 88.02(16) . . ? N10A Ru1 Cl3 172.24(11) . . ? N1A Ru1 Cl3 94.80(15) . . ? N1B Ru1 Cl3 85.82(14) . . ? N10B Ru1 Cl2 171.91(12) . . ? N10A Ru1 Cl2 87.54(13) . . ? N1A Ru1 Cl2 86.90(13) . . ? N1B Ru1 Cl2 94.68(13) . . ? Cl3 Ru1 Cl2 94.04(10) . . ? C6A N10A C9A 105.9(4) . . ? C6A N10A Ru1 113.8(4) . . ? C9A N10A Ru1 140.2(3) . . ? C92A C9A N10A 111.6(4) . . ? C92A C9A C8A 112.9(6) . . ? N10A C9A C8A 101.4(4) . . ? C92A C9A C91A 113.0(5) . . ? N10A C9A C91A 106.9(5) . . ? C8A C9A C91A 110.3(5) . . ? O7A C8A C9A 106.2(5) . . ? C6A O7A C8A 103.1(4) . . ? N10A C6A O7A 119.9(5) . . ? N10A C6A C5A 117.5(6) . . ? O7A C6A C5A 122.6(5) . . ? N1A C5A O4A 120.4(5) . . ? N1A C5A C6A 116.7(5) . . ? O4A C5A C6A 122.8(6) . . ? C5A O4A C3A 104.3(5) . . ? O4A C3A C2A 105.9(5) . . ? C21A C2A N1A 107.3(5) . . ? C21A C2A C22A 112.3(7) . . ? N1A C2A C22A 110.8(5) . . ? C21A C2A C3A 112.2(6) . . ? N1A C2A C3A 101.3(5) . . ? C22A C2A C3A 112.3(5) . . ? C5A N1A C2A 105.5(5) . . ? C5A N1A Ru1 114.0(4) . . ? C2A N1A Ru1 138.7(4) . . ? C6B N10B C9B 106.1(4) . . ? C6B N10B Ru1 114.0(3) . . ? C9B N10B Ru1 139.7(4) . . ? N10B C9B C92B 111.4(4) . . ? N10B C9B C91B 107.9(5) . . ? C92B C9B C91B 111.5(6) . . ? N10B C9B C8B 101.4(4) . . ? C92B C9B C8B 111.8(6) . . ? C91B C9B C8B 112.3(5) . . ? O7B C8B C9B 105.2(5) . . ? C6B O7B C8B 102.7(4) . . ? N10B C6B O7B 119.7(5) . . ? N10B C6B C5B 118.0(5) . . ? O7B C6B C5B 122.3(5) . . ? N1B C5B O4B 120.4(5) . . ? N1B C5B C6B 116.1(5) . . ? O4B C5B C6B 123.5(5) . . ? C5B O4B C3B 104.6(4) . . ? O4B C3B C2B 107.2(4) . . ? C22B C2B N1B 111.3(5) . . ? C22B C2B C21B 112.4(7) . . ? N1B C2B C21B 108.8(5) . . ? C22B C2B C3B 110.3(6) . . ? N1B C2B C3B 101.5(4) . . ? C21B C2B C3B 112.1(6) . . ? C5B N1B C2B 105.8(4) . . ? C5B N1B Ru1 114.0(4) . . ? C2B N1B Ru1 138.6(3) . . ? _refine_diff_density_max 1.153 _refine_diff_density_min -0.638 _refine_diff_density_rms 0.167 data_Ru(1a)(dmf)Cl3 _database_code_CSD 174512 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H23 Cl3 N3 O3 Ru' _chemical_formula_weight 476.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x+1/2, -y, z+1/2' _cell_length_a 8.607(14) _cell_length_b 14.48(2) _cell_length_c 15.73(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1960(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.615 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 964 _exptl_absorpt_coefficient_mu 1.223 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2046 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0595 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 26.15 _reflns_number_total 2046 _reflns_number_gt 1462 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1565P)^2^+0.0000P] 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 SHELXL _refine_ls_extinction_coef 0.0013(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.17(12) _refine_ls_number_reflns 2046 _refine_ls_number_parameters 215 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0994 _refine_ls_R_factor_gt 0.0581 _refine_ls_wR_factor_ref 0.1835 _refine_ls_wR_factor_gt 0.1598 _refine_ls_goodness_of_fit_ref 0.910 _refine_ls_restrained_S_all 0.910 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.13663(11) 0.02006(7) 0.90168(6) 0.0385(3) Uani 1 d . . . Cl2 Cl -0.0897(4) 0.0153(3) 0.9871(2) 0.0587(8) Uani 1 d . . . Cl3 Cl 0.2948(4) 0.0306(3) 1.0215(2) 0.0564(9) Uani 1 d . . . Cl4 Cl -0.0116(4) 0.0047(2) 0.7768(2) 0.0543(8) Uani 1 d . . . N1 N 0.3319(11) 0.0326(8) 0.8266(7) 0.047(3) Uani 1 d . . . C2 C 0.4527(17) -0.0266(11) 0.7889(8) 0.058(3) Uani 1 d . . . C3 C 0.5533(19) 0.0378(12) 0.7360(14) 0.097(7) Uani 1 d . . . H3A H 0.6614 0.0344 0.7531 0.116 Uiso 1 calc R . . H3B H 0.5452 0.0236 0.6759 0.116 Uiso 1 calc R . . O4 O 0.4857(12) 0.1300(7) 0.7555(8) 0.074(3) Uani 1 d . . . C5 C 0.3647(17) 0.1182(9) 0.8024(9) 0.049(3) Uani 1 d . . . C6 C 0.2604(16) 0.1873(10) 0.8363(9) 0.052(3) Uani 1 d . . . O7 O 0.2724(14) 0.2754(7) 0.8160(8) 0.069(3) Uani 1 d . . . C8 C 0.1504(17) 0.3219(9) 0.8704(11) 0.062(4) Uani 1 d . . . H8A H 0.0872 0.3634 0.8366 0.074 Uiso 1 calc R . . H8B H 0.1985 0.3568 0.9160 0.074 Uiso 1 calc R . . C9 C 0.0520(15) 0.2432(8) 0.9062(10) 0.044(3) Uani 1 d . . . N10 N 0.1475(12) 0.1607(6) 0.8826(7) 0.042(2) Uani 1 d . . . C21 C 0.5473(18) -0.0755(14) 0.8591(11) 0.084(6) Uani 1 d . . . H21A H 0.6121 -0.0313 0.8875 0.101 Uiso 1 calc R . . H21B H 0.6110 -0.1226 0.8339 0.101 Uiso 1 calc R . . H21C H 0.4775 -0.1032 0.8993 0.101 Uiso 1 calc R . . C22 C 0.371(2) -0.1012(11) 0.7329(11) 0.079(5) Uani 1 d . . . H22A H 0.3033 -0.1378 0.7677 0.095 Uiso 1 calc R . . H22B H 0.4480 -0.1402 0.7072 0.095 Uiso 1 calc R . . H22C H 0.3113 -0.0713 0.6892 0.095 Uiso 1 calc R . . C91 C 0.0295(19) 0.2500(12) 1.0023(11) 0.070(4) Uani 1 d . . . H91A H -0.0130 0.1931 1.0233 0.084 Uiso 1 calc R . . H91B H -0.0405 0.2998 1.0149 0.084 Uiso 1 calc R . . H91C H 0.1279 0.2615 1.0290 0.084 Uiso 1 calc R . . C92 C -0.1025(17) 0.2331(11) 0.8592(10) 0.061(4) Uani 1 d . . . H92A H -0.0842 0.2335 0.7990 0.073 Uiso 1 calc R . . H92B H -0.1695 0.2836 0.8739 0.073 Uiso 1 calc R . . H92C H -0.1509 0.1759 0.8751 0.073 Uiso 1 calc R . . O31 O 0.1483(11) -0.1251(5) 0.9102(6) 0.050(2) Uani 1 d . . . C32 C 0.0242(19) -0.1715(9) 0.9026(11) 0.060(4) Uani 1 d . . . H32 H -0.0705 -0.1410 0.8977 0.073 Uiso 1 calc R . . N33 N 0.0280(18) -0.2627(7) 0.9015(10) 0.067(3) Uani 1 d . . . C34 C 0.171(3) -0.3148(12) 0.9111(17) 0.108(8) Uani 1 d . . . H34A H 0.2554 -0.2806 0.8870 0.129 Uiso 1 calc R . . H34B H 0.1609 -0.3730 0.8824 0.129 Uiso 1 calc R . . H34C H 0.1903 -0.3254 0.9704 0.129 Uiso 1 calc R . . C35 C -0.120(3) -0.3139(10) 0.8885(11) 0.080(5) Uani 1 d . . . H35A H -0.2058 -0.2723 0.8949 0.097 Uiso 1 calc R . . H35B H -0.1278 -0.3624 0.9299 0.097 Uiso 1 calc R . . H35C H -0.1211 -0.3400 0.8324 0.097 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0397(5) 0.0305(5) 0.0452(5) 0.0010(4) 0.0018(4) -0.0007(4) Cl2 0.0596(17) 0.0506(18) 0.0659(19) -0.0017(17) 0.0246(16) -0.0046(16) Cl3 0.0736(19) 0.0458(19) 0.0497(17) 0.0018(15) -0.0162(16) -0.0006(16) Cl4 0.0491(15) 0.058(2) 0.0563(17) -0.0031(15) -0.0112(14) -0.0041(14) N1 0.042(5) 0.050(7) 0.049(6) -0.005(5) 0.003(4) 0.004(5) C2 0.073(9) 0.057(8) 0.043(7) -0.002(7) -0.007(6) 0.003(8) C3 0.069(10) 0.090(15) 0.131(17) -0.013(12) 0.040(11) 0.020(9) O4 0.058(6) 0.071(7) 0.094(9) 0.001(6) 0.036(6) -0.015(5) C5 0.042(6) 0.051(7) 0.056(8) -0.001(6) 0.003(7) -0.002(6) C6 0.055(8) 0.053(8) 0.050(8) 0.011(6) 0.001(7) -0.008(6) O7 0.087(7) 0.043(6) 0.076(7) 0.020(5) 0.010(6) -0.015(5) C8 0.052(7) 0.040(7) 0.093(11) 0.013(7) -0.007(8) -0.004(6) C9 0.055(7) 0.027(6) 0.050(7) 0.004(5) 0.000(7) 0.002(5) N10 0.042(5) 0.026(5) 0.059(7) 0.006(4) -0.010(5) 0.002(4) C21 0.057(9) 0.125(16) 0.072(11) -0.038(10) -0.020(8) 0.048(10) C22 0.068(9) 0.083(11) 0.087(12) -0.037(9) -0.010(11) 0.002(9) C91 0.077(10) 0.066(9) 0.067(9) -0.019(7) -0.010(9) 0.028(8) C92 0.049(7) 0.068(10) 0.066(9) 0.008(8) -0.010(7) 0.009(7) O31 0.056(5) 0.030(4) 0.065(6) -0.005(4) 0.000(6) -0.002(4) C32 0.075(9) 0.037(7) 0.069(9) -0.004(7) 0.012(9) -0.001(6) N33 0.102(10) 0.034(6) 0.066(8) 0.009(6) 0.012(8) -0.004(6) C34 0.13(2) 0.046(10) 0.15(2) -0.004(12) -0.008(17) 0.016(10) C35 0.128(15) 0.042(8) 0.071(10) 0.000(7) 0.002(12) -0.024(10) _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 N10 2.061(9) . ? Ru1 N1 2.063(10) . ? Ru1 O31 2.109(8) . ? Ru1 Cl3 2.330(4) . ? Ru1 Cl4 2.353(4) . ? Ru1 Cl2 2.367(4) . ? N1 C5 1.326(16) . ? N1 C2 1.472(17) . ? C2 C3 1.52(2) . ? C2 C21 1.54(2) . ? C2 C22 1.561(19) . ? C3 O4 1.489(18) . ? O4 C5 1.288(18) . ? C5 C6 1.446(19) . ? C6 N10 1.274(17) . ? C6 O7 1.319(17) . ? O7 C8 1.513(18) . ? C8 C9 1.528(18) . ? C9 N10 1.496(15) . ? C9 C91 1.53(2) . ? C9 C92 1.53(2) . ? O31 C32 1.267(18) . ? C32 N33 1.321(17) . ? N33 C34 1.45(2) . ? N33 C35 1.49(2) . ? 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 N10 Ru1 N1 78.0(4) . . ? N10 Ru1 O31 172.9(4) . . ? N1 Ru1 O31 94.9(4) . . ? N10 Ru1 Cl3 91.5(3) . . ? N1 Ru1 Cl3 89.0(3) . . ? O31 Ru1 Cl3 89.2(3) . . ? N10 Ru1 Cl4 89.8(3) . . ? N1 Ru1 Cl4 88.4(3) . . ? O31 Ru1 Cl4 89.1(3) . . ? Cl3 Ru1 Cl4 176.73(13) . . ? N10 Ru1 Cl2 98.6(3) . . ? N1 Ru1 Cl2 176.6(3) . . ? O31 Ru1 Cl2 88.5(3) . . ? Cl3 Ru1 Cl2 91.34(18) . . ? Cl4 Ru1 Cl2 91.43(17) . . ? C5 N1 C2 106.2(12) . . ? C5 N1 Ru1 114.8(9) . . ? C2 N1 Ru1 139.0(9) . . ? N1 C2 C3 105.4(13) . . ? N1 C2 C21 110.6(11) . . ? C3 C2 C21 111.9(14) . . ? N1 C2 C22 108.1(12) . . ? C3 C2 C22 111.8(15) . . ? C21 C2 C22 108.9(14) . . ? O4 C3 C2 102.4(12) . . ? C5 O4 C3 108.4(12) . . ? O4 C5 N1 117.4(12) . . ? O4 C5 C6 128.4(12) . . ? N1 C5 C6 114.1(12) . . ? N10 C6 O7 119.3(13) . . ? N10 C6 C5 118.4(12) . . ? O7 C6 C5 122.1(13) . . ? C6 O7 C8 103.9(11) . . ? O7 C8 C9 105.1(10) . . ? N10 C9 C91 111.5(11) . . ? N10 C9 C92 106.4(11) . . ? C91 C9 C92 112.0(13) . . ? N10 C9 C8 101.5(11) . . ? C91 C9 C8 112.7(14) . . ? C92 C9 C8 112.1(12) . . ? C6 N10 C9 108.7(10) . . ? C6 N10 Ru1 114.6(9) . . ? C9 N10 Ru1 136.7(9) . . ? C32 O31 Ru1 118.8(9) . . ? O31 C32 N33 120.6(14) . . ? C32 N33 C34 122.7(15) . . ? C32 N33 C35 118.6(14) . . ? C34 N33 C35 118.7(13) . . ? _refine_diff_density_max 1.255 _refine_diff_density_min -0.929 _refine_diff_density_rms 0.132 data_[Ru(1a)2Cl2]PF6 _database_code_CSD 174513 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H32 Cl2 F6 N4 O4 P Ru ' _chemical_formula_weight 709.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P22121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' 'x, -y, -z' '-x, -y+1/2, z+1/2' _cell_length_a 8.545(12) _cell_length_b 12.001(16) _cell_length_c 14.002(20) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1435.9 _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.641 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 718 _exptl_absorpt_coefficient_mu 0.860 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5008 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 25.93 _reflns_number_total 2750 _reflns_number_gt 2397 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0463P)^2^+0.7078P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0(2) _refine_ls_number_reflns 2750 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0479 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.0832 _refine_ls_wR_factor_gt 0.0780 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.35463(4) 0.0000 0.0000 0.02554(12) Uani 1 d S . . N1 N 0.3518(4) 0.1651(3) 0.0524(2) 0.0295(7) Uani 1 d . . . C2 C 0.4560(6) 0.2675(4) 0.0480(4) 0.0435(12) Uani 1 d . . . C3 C 0.3737(7) 0.3438(4) 0.1212(4) 0.0591(14) Uani 1 d . . . H3A H 0.4490 0.3739 0.1661 0.071 Uiso 1 calc R . . H3B H 0.3222 0.4053 0.0890 0.071 Uiso 1 calc R . . O4 O 0.2583(5) 0.2742(3) 0.1710(3) 0.0515(9) Uani 1 d . . . C5 C 0.2572(6) 0.1796(3) 0.1212(3) 0.0360(10) Uani 1 d . . . C6 C 0.1551(5) 0.0866(3) 0.1450(3) 0.0326(9) Uani 1 d . . . O7 O 0.0421(4) 0.0959(3) 0.2097(2) 0.0473(8) Uani 1 d . . . C8 C -0.0424(5) -0.0104(5) 0.2039(3) 0.0482(11) Uani 1 d . . . H8A H -0.1419 -0.0008 0.1716 0.058 Uiso 1 calc R . . H8B H -0.0616 -0.0402 0.2672 0.058 Uiso 1 calc R . . C9 C 0.0653(6) -0.0888(4) 0.1465(3) 0.0387(11) Uani 1 d . . . N10 N 0.1742(3) -0.0043(4) 0.10190(18) 0.0263(6) Uani 1 d . . . C21 C 0.6209(6) 0.2344(5) 0.0796(5) 0.0587(15) Uani 1 d . . . H21A H 0.6632 0.1810 0.0355 0.070 Uiso 1 calc R . . H21B H 0.6165 0.2022 0.1423 0.070 Uiso 1 calc R . . H21C H 0.6866 0.2993 0.0809 0.070 Uiso 1 calc R . . C22 C 0.4569(8) 0.3194(4) -0.0504(4) 0.0615(16) Uani 1 d . . . H22A H 0.5028 0.2684 -0.0951 0.074 Uiso 1 calc R . . H22B H 0.5171 0.3870 -0.0490 0.074 Uiso 1 calc R . . H22C H 0.3516 0.3359 -0.0694 0.074 Uiso 1 calc R . . C91 C -0.0262(7) -0.1548(5) 0.0726(4) 0.0592(15) Uani 1 d . . . H91A H -0.0783 -0.1044 0.0299 0.071 Uiso 1 calc R . . H91B H -0.1023 -0.2007 0.1042 0.071 Uiso 1 calc R . . H91C H 0.0444 -0.2012 0.0370 0.071 Uiso 1 calc R . . C92 C 0.1605(8) -0.1624(5) 0.2125(4) 0.0632(16) Uani 1 d . . . H92A H 0.2395 -0.2006 0.1763 0.076 Uiso 1 calc R . . H92B H 0.0930 -0.2160 0.2424 0.076 Uiso 1 calc R . . H92C H 0.2095 -0.1174 0.2606 0.076 Uiso 1 calc R . . Cl1 Cl 0.53380(13) -0.03964(10) 0.12067(9) 0.0449(3) Uani 1 d . . . P1 P 0.03736(18) 0.0000 0.5000 0.0427(3) Uani 1 d S . . F11 F -0.0944(4) -0.0488(3) 0.5685(2) 0.0733(10) Uani 1 d . . . F12 F 0.1654(5) -0.0486(4) 0.5685(3) 0.1001(14) Uani 1 d . . . F13 F 0.0344(5) 0.1125(3) 0.5602(2) 0.0761(10) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01968(18) 0.02682(19) 0.0301(2) -0.0029(2) 0.000 0.000 N1 0.0215(16) 0.0264(16) 0.0406(19) -0.0039(14) -0.0040(17) -0.0034(15) C2 0.036(3) 0.034(3) 0.060(3) -0.004(2) -0.003(2) -0.009(2) C3 0.060(3) 0.036(2) 0.081(4) -0.016(3) 0.004(3) -0.009(3) O4 0.062(2) 0.0361(17) 0.057(2) -0.0217(15) 0.0073(19) -0.0024(18) C5 0.036(2) 0.033(2) 0.040(2) -0.008(2) -0.001(2) -0.0009(19) C6 0.031(2) 0.039(2) 0.029(2) 0.0001(17) -0.002(2) -0.008(2) O7 0.047(2) 0.0471(18) 0.048(2) -0.0118(15) 0.0184(17) 0.0011(17) C8 0.039(2) 0.061(3) 0.045(2) -0.004(3) 0.0109(19) -0.014(3) C9 0.040(3) 0.038(2) 0.038(3) -0.0001(19) 0.014(2) -0.009(2) N10 0.0222(14) 0.0330(15) 0.0237(13) 0.0041(18) 0.0006(10) -0.005(2) C21 0.037(3) 0.060(3) 0.079(4) -0.011(3) -0.010(3) -0.014(3) C22 0.067(4) 0.038(3) 0.080(4) 0.008(3) 0.004(3) -0.015(3) C91 0.046(3) 0.065(3) 0.066(4) -0.013(3) 0.016(3) -0.026(3) C92 0.068(4) 0.059(3) 0.062(3) 0.033(3) 0.013(3) -0.001(3) Cl1 0.0344(6) 0.0508(7) 0.0495(7) -0.0012(5) -0.0159(5) 0.0042(5) P1 0.0420(8) 0.0475(8) 0.0387(7) -0.0020(11) 0.000 0.000 F11 0.077(2) 0.079(2) 0.064(2) -0.0002(17) 0.0233(18) -0.0162(17) F12 0.082(3) 0.136(4) 0.082(3) 0.000(2) -0.030(2) 0.040(2) F13 0.103(3) 0.0604(19) 0.064(2) -0.0179(16) -0.006(2) -0.014(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 N10 2.101(3) 3 ? Ru1 N10 2.101(3) . ? Ru1 N1 2.113(4) . ? Ru1 N1 2.113(4) 3 ? Ru1 Cl1 2.329(3) 3 ? Ru1 Cl1 2.329(3) . ? N1 C5 1.269(6) . ? N1 C2 1.519(6) . ? C2 C22 1.511(7) . ? C2 C21 1.530(8) . ? C2 C3 1.544(7) . ? C3 O4 1.469(7) . ? O4 C5 1.332(5) . ? C5 C6 1.455(6) . ? C6 N10 1.257(6) . ? C6 O7 1.330(5) . ? O7 C8 1.469(6) . ? C8 C9 1.541(7) . ? C9 N10 1.511(6) . ? C9 C92 1.516(7) . ? C9 C91 1.520(7) . ? P1 F12 1.568(4) 3_556 ? P1 F12 1.568(4) . ? P1 F11 1.591(4) 3_556 ? P1 F11 1.591(4) . ? P1 F13 1.592(3) . ? P1 F13 1.592(3) 3_556 ? 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 N10 Ru1 N10 85.62(18) 3 . ? N10 Ru1 N1 101.79(16) 3 . ? N10 Ru1 N1 77.23(16) . . ? N10 Ru1 N1 77.23(16) 3 3 ? N10 Ru1 N1 101.78(16) . 3 ? N1 Ru1 N1 178.69(19) . 3 ? N10 Ru1 Cl1 89.12(14) 3 3 ? N10 Ru1 Cl1 168.49(12) . 3 ? N1 Ru1 Cl1 93.88(11) . 3 ? N1 Ru1 Cl1 86.98(11) 3 3 ? N10 Ru1 Cl1 168.49(12) 3 . ? N10 Ru1 Cl1 89.12(14) . . ? N1 Ru1 Cl1 86.97(11) . . ? N1 Ru1 Cl1 93.89(11) 3 . ? Cl1 Ru1 Cl1 97.81(13) 3 . ? C5 N1 C2 107.1(3) . . ? C5 N1 Ru1 113.5(3) . . ? C2 N1 Ru1 137.6(3) . . ? C22 C2 N1 112.0(4) . . ? C22 C2 C21 111.5(5) . . ? N1 C2 C21 108.5(4) . . ? C22 C2 C3 111.3(5) . . ? N1 C2 C3 100.7(4) . . ? C21 C2 C3 112.4(5) . . ? O4 C3 C2 106.5(4) . . ? C5 O4 C3 103.9(4) . . ? N1 C5 O4 120.6(4) . . ? N1 C5 C6 116.8(4) . . ? O4 C5 C6 122.5(4) . . ? N10 C6 O7 119.7(4) . . ? N10 C6 C5 118.5(4) . . ? O7 C6 C5 121.8(4) . . ? C6 O7 C8 104.2(3) . . ? O7 C8 C9 105.4(3) . . ? N10 C9 C92 108.2(4) . . ? N10 C9 C91 112.7(4) . . ? C92 C9 C91 112.8(5) . . ? N10 C9 C8 100.0(4) . . ? C92 C9 C8 111.0(4) . . ? C91 C9 C8 111.5(4) . . ? C6 N10 C9 107.7(3) . . ? C6 N10 Ru1 113.6(3) . . ? C9 N10 Ru1 138.5(3) . . ? F12 P1 F12 91.5(4) 3_556 . ? F12 P1 F11 89.3(2) 3_556 3_556 ? F12 P1 F11 179.2(2) . 3_556 ? F12 P1 F11 179.2(2) 3_556 . ? F12 P1 F11 89.3(2) . . ? F11 P1 F11 89.9(3) 3_556 . ? F12 P1 F13 91.2(2) 3_556 . ? F12 P1 F13 90.1(2) . . ? F11 P1 F13 89.8(2) 3_556 . ? F11 P1 F13 88.9(2) . . ? F12 P1 F13 90.1(2) 3_556 3_556 ? F12 P1 F13 91.2(2) . 3_556 ? F11 P1 F13 88.9(2) 3_556 3_556 ? F11 P1 F13 89.8(2) . 3_556 ? F13 P1 F13 178.2(3) . 3_556 ? _refine_diff_density_max 1.079 _refine_diff_density_min -0.382 _refine_diff_density_rms 0.082