# Copyright The Royal Society of Chemistry, 1999 # CCDC Number 186/1273 #SYNTHESIS AND STRUCTURES OF PHOTODECARBONYLATED RUTHENIUM(II) COMPLEXES data_A_TEXRAY.INF_file_is_not_p #------------------------------------------------------------------------------ _audit_creation_date 'Mon Sep 21 09:29:53 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 18.153(2) _cell_length_b 10.544(2) _cell_length_c 17.092(2) _cell_angle_alpha 90.00(1) _cell_angle_beta 115.66(1) _cell_angle_gamma 90.00(1) _cell_volume 2948.7(6) _cell_formula_units_Z 8 _cell_measurement_temperature 273.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' +x, +y, +z' ' -x, +y,1/2-z' ' -x, +y,1/2-z' ' -x, -y, -z' ' -x, -y, -z' ' +x, -y,1/2+z' ' +x, -y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'unknown' _exptl_crystal_colour 'unknown' _exptl_crystal_size_max 0.000 _exptl_crystal_size_mid 0.000 _exptl_crystal_size_min 0.000 _exptl_crystal_density_diffrn 2.004 _exptl_crystal_density_meas ? _chemical_formula_weight 444.81 _chemical_formula_analytical ? _chemical_formula_sum 'C11 H8 Cl4.50 N2 O Ru ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1732.00 _exptl_absorpt_coefficient_mu 1.870 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 273.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'unknown' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 6176 _reflns_number_total 3395 _reflns_number_observed 1247 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 8.62 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 28.64 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H 0 64 0.000 0.000 'International Tables' Ru 0 8 -1.259 0.836 'International Tables' C 0 88 0.003 0.002 'International Tables' O 0 8 0.011 0.006 'International Tables' Cl 0 36 0.148 0.159 'International Tables' N 0 16 0.006 0.003 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Ru(1) 0.17409(7) 0.1454(1) 0.51065(7) 0.0335(4) Uij ? ? Cl(1) 0.1839(2) 0.3656(4) 0.4759(2) 0.038(1) Uij ? ? Cl(2) 0.2230(3) 0.1972(5) 0.6618(3) 0.063(2) Uij ? ? Cl(3) -0.021(2) 0.410(3) 0.312(2) 0.122(9) Uij ? ? Cl(4) -0.081(2) 0.442(3) 0.277(2) 0.14(1) Uij ? ? Cl(5) -0.161(2) 0.517(3) 0.316(2) 0.15(1) Uij ? ? Cl(6) -0.077(2) 0.573(3) 0.398(2) 0.136(10) Uij ? ? Cl(7) -0.018(2) 0.509(4) 0.455(2) 0.19(2) Uij ? ? O(1) 0.0099(6) 0.164(1) 0.4954(6) 0.056(3) Uij ? ? N(1) 0.1738(6) -0.047(1) 0.5288(7) 0.031(3) Uij ? ? N(2) 0.1344(6) 0.082(1) 0.3844(6) 0.023(3) Uij ? ? C(1) 0.0631(7) 0.162(1) 0.4981(7) 0.020(3) Uij ? ? C(2) 0.1925(8) -0.109(1) 0.6026(8) 0.035(4) Uij ? ? C(3) 0.1865(9) -0.242(1) 0.6040(9) 0.041(4) Uij ? ? C(4) 0.1624(9) -0.308(2) 0.5305(9) 0.042(4) Uij ? ? C(5) 0.1434(9) -0.247(1) 0.4528(10) 0.039(4) Uij ? ? C(6) 0.1167(8) -0.309(1) 0.3704(9) 0.038(4) Uij ? ? C(7) 0.1011(9) -0.243(1) 0.297(1) 0.044(4) Uij ? ? C(8) 0.1058(8) -0.111(1) 0.2978(9) 0.033(4) Uij ? ? C(9) 0.0845(8) -0.033(1) 0.2231(9) 0.037(4) Uij ? ? C(10) 0.0860(8) 0.094(1) 0.2285(8) 0.032(4) Uij ? ? C(11) 0.1128(8) 0.148(2) 0.3112(9) 0.042(4) Uij ? ? C(12) 0.1306(8) -0.046(1) 0.3766(9) 0.032(4) Uij ? ? C(13) 0.1481(8) -0.115(1) 0.4539(8) 0.028(4) Uij ? ? H(1) 0.2104 -0.0624 0.6553 0.0420 Uij ? ? H(2) 0.1995 -0.2849 0.6574 0.0487 Uij ? ? H(3) 0.1583 -0.3982 0.5318 0.0509 Uij ? ? H(4) 0.1099 -0.3987 0.3671 0.0453 Uij ? ? H(5) 0.0866 -0.2874 0.2442 0.0526 Uij ? ? H(6) 0.0688 -0.0718 0.1681 0.0444 Uij ? ? H(7) 0.0694 0.1457 0.1782 0.0384 Uij ? ? H(8) 0.1159 0.2377 0.3155 0.0507 Uij ? ? Cl(1*) 0.3161(2) 0.1344(4) 0.5241(2) 0.038(1) Uij ? ? Ru(1*) 0.32591(7) 0.3546(1) 0.48935(7) 0.0335(4) Uij ? ? Cl(7*) 0.018(2) 0.491(4) 0.545(2) 0.19(2) Uij ? ? Cl(2*) 0.2770(3) 0.3028(5) 0.3382(3) 0.063(2) Uij ? ? N(1*) 0.3262(6) 0.547(1) 0.4712(7) 0.031(3) Uij ? ? N(2*) 0.3656(6) 0.418(1) 0.6156(6) 0.023(3) Uij ? ? C(1*) 0.4369(7) 0.338(1) 0.5019(7) 0.020(3) Uij ? ? Cl(6*) 0.077(2) 0.427(3) 0.602(2) 0.136(10) Uij ? ? C(2*) 0.3075(8) 0.609(1) 0.3974(8) 0.035(4) Uij ? ? C(13*) 0.3519(8) 0.615(1) 0.5461(8) 0.028(4) Uij ? ? C(11*) 0.3872(8) 0.352(2) 0.6888(9) 0.042(4) Uij ? ? C(12*) 0.3694(8) 0.546(1) 0.6234(9) 0.032(4) Uij ? ? O(1*) 0.4901(6) 0.336(1) 0.5046(6) 0.056(3) Uij ? ? Cl(5*) 0.161(2) 0.483(3) 0.684(2) 0.15(1) Uij ? ? C(3*) 0.3135(9) 0.742(1) 0.3960(9) 0.041(4) Uij ? ? H(1*) 0.2896 0.5624 0.3447 0.0420 Uij ? ? C(5*) 0.3566(9) 0.747(1) 0.5472(10) 0.039(4) Uij ? ? C(10*) 0.4140(8) 0.406(1) 0.7715(8) 0.032(4) Uij ? ? H(8*) 0.3841 0.2623 0.6845 0.0507 Uij ? ? C(8*) 0.3942(8) 0.611(1) 0.7022(9) 0.033(4) Uij ? ? Cl(4*) 0.081(2) 0.558(3) 0.723(2) 0.14(1) Uij ? ? C(4*) 0.3376(9) 0.808(2) 0.4695(9) 0.042(4) Uij ? ? H(2*) 0.3005 0.7849 0.3426 0.0487 Uij ? ? C(6*) 0.3833(8) 0.809(1) 0.6296(9) 0.038(4) Uij ? ? C(9*) 0.4155(8) 0.533(1) 0.7769(9) 0.037(4) Uij ? ? H(7*) 0.4306 0.3543 0.8218 0.0384 Uij ? ? C(7*) 0.3989(9) 0.743(1) 0.703(1) 0.044(4) Uij ? ? Cl(3*) 0.021(2) 0.590(3) 0.688(2) 0.122(9) Uij ? ? H(3*) 0.3417 0.8982 0.4682 0.0509 Uij ? ? H(4*) 0.3901 0.8987 0.6329 0.0453 Uij ? ? H(6*) 0.4312 0.5718 0.8319 0.0444 Uij ? ? H(5*) 0.4134 0.7874 0.7558 0.0526 Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru(1) 0.0239(7) 0.0415(8) 0.0375(7) 0.0012(8) 0.0156(5) -0.0026(8) Cl(1) 0.030(2) 0.039(3) 0.048(2) 0.001(2) 0.019(2) 0.000(2) Cl(2) 0.051(3) 0.076(4) 0.070(3) -0.008(3) 0.033(2) -0.003(3) Cl(1*) 0.030(2) 0.039(3) 0.048(2) 0.001(2) 0.019(2) 0.000(2) Ru(1*) 0.0239(7) 0.0415(8) 0.0375(7) 0.0012(8) 0.0156(5) -0.0026(8) Cl(2*) 0.051(3) 0.076(4) 0.070(3) -0.008(3) 0.033(2) -0.003(3) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1247 _refine_ls_number_parameters 112 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0829 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0687 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.246 _refine_ls_shift/esd_max 0.0010 _refine_ls_shift/esd_mean ? _refine_diff_density_min -1.24 _refine_diff_density_max 1.39 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru(1) Cl(1) 2.422(4) ? ? yes Ru(1) Cl(1) 2.489(3) ? ? yes Ru(1) Cl(2) 2.402(4) ? ? yes Ru(1) N(1) 2.05(1) ? ? yes Ru(1) N(2) 2.068(10) ? ? yes Ru(1) C(1) 1.94(1) ? ? yes Cl(3) Cl(4) 1.05(3) ? ? yes Cl(4) Cl(5) 2.00(4) ? ? yes Cl(5) Cl(6) 1.67(4) ? ? yes Cl(6) Cl(7) 1.28(4) ? ? yes Cl(7) Cl(7) 1.40(6) ? ? yes O(1) C(1) 0.95(1) ? ? yes N(1) C(2) 1.33(1) ? ? yes N(1) C(13) 1.36(1) ? ? yes N(2) C(11) 1.33(2) ? ? yes N(2) C(12) 1.36(2) ? ? yes C(2) C(3) 1.41(2) ? ? yes C(3) C(4) 1.33(2) ? ? yes C(4) C(5) 1.38(2) ? ? yes C(5) C(6) 1.43(2) ? ? yes C(5) C(13) 1.40(2) ? ? yes C(6) C(7) 1.35(2) ? ? yes C(7) C(8) 1.40(2) ? ? yes C(8) C(9) 1.42(2) ? ? yes C(8) C(12) 1.40(2) ? ? yes C(9) C(10) 1.34(2) ? ? yes C(10) C(11) 1.40(2) ? ? yes C(12) C(13) 1.42(2) ? ? yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(1) Ru(1) Cl(1) 83.4(1) ? ? ? yes Cl(1) Ru(1) Cl(2) 90.8(1) ? ? ? yes Cl(1) Ru(1) N(1) 171.8(3) ? ? ? yes Cl(1) Ru(1) N(2) 94.7(3) ? ? ? yes Cl(1) Ru(1) C(1) 94.1(4) ? ? ? yes Cl(1) Ru(1) Cl(2) 91.4(1) ? ? ? yes Cl(1) Ru(1) N(1) 90.6(3) ? ? ? yes Cl(1) Ru(1) N(2) 87.7(3) ? ? ? yes Cl(1) Ru(1) C(1) 177.4(4) ? ? ? yes Cl(2) Ru(1) N(1) 94.9(3) ? ? ? yes Cl(2) Ru(1) N(2) 174.3(3) ? ? ? yes Cl(2) Ru(1) C(1) 89.0(3) ? ? ? yes N(1) Ru(1) N(2) 79.4(4) ? ? ? yes N(1) Ru(1) C(1) 91.9(5) ? ? ? yes N(2) Ru(1) C(1) 92.1(4) ? ? ? yes Ru(1) Cl(1) Ru(1) 96.6(1) ? ? ? yes Cl(3) Cl(4) Cl(5) 130(3) ? ? ? yes Cl(4) Cl(5) Cl(6) 83(1) ? ? ? yes Cl(5) Cl(6) Cl(7) 127(3) ? ? ? yes Cl(6) Cl(7) Cl(7) 138(5) ? ? ? yes Ru(1) N(1) C(2) 127.9(9) ? ? ? yes Ru(1) N(1) C(13) 113.6(8) ? ? ? yes C(2) N(1) C(13) 118(1) ? ? ? yes Ru(1) N(2) C(11) 129(1) ? ? ? yes Ru(1) N(2) C(12) 113.8(8) ? ? ? yes C(11) N(2) C(12) 116(1) ? ? ? yes Ru(1) C(1) O(1) 175(1) ? ? ? yes N(1) C(2) C(3) 121(1) ? ? ? yes C(2) C(3) C(4) 120(1) ? ? ? yes C(3) C(4) C(5) 120(1) ? ? ? yes C(4) C(5) C(6) 124(1) ? ? ? yes C(4) C(5) C(13) 117(1) ? ? ? yes C(6) C(5) C(13) 117(1) ? ? ? yes C(5) C(6) C(7) 121(1) ? ? ? yes C(6) C(7) C(8) 121(1) ? ? ? yes C(7) C(8) C(9) 125(1) ? ? ? yes C(7) C(8) C(12) 119(1) ? ? ? yes C(9) C(8) C(12) 115(1) ? ? ? yes C(8) C(9) C(10) 121(1) ? ? ? yes C(9) C(10) C(11) 117(1) ? ? ? yes N(2) C(11) C(10) 124(1) ? ? ? yes N(2) C(12) C(8) 124(1) ? ? ? yes N(2) C(12) C(13) 115(1) ? ? ? yes C(8) C(12) C(13) 119(1) ? ? ? yes N(1) C(13) C(5) 122(1) ? ? ? yes N(1) C(13) C(12) 117(1) ? ? ? yes C(5) C(13) C(12) 120(1) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal ' RSC DALTON (COMM.)' _publ_contact_author ; CHRISTOPHER M. KEPERT DEPT. OF CHEMISTRY, MONASH UNI, CLAYTON 3168, AUSTRALIA ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #=END data_ru2pyk _audit_creation_date 97-07-07 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record ? _chemical_compound_source ? #ActaC _chemical_name_systematic ? #ActaC _chemical_name_common ? #ActaC _chemical_formula_analytical C26_H20_Cl8_N4_O4_Ru2 #ActaC _chemical_formula_moiety ? #ActaC _chemical_formula_structural [{C5H4N)2CO}Ru(CO)Cl2].2CH2Cl2 #ActaC _chemical_formula_sum C26_H20_Cl8_N4_O4_Ru2 #ActaC _chemical_formula_weight 938.23 #ActaC _chemical_melting_point ? #ActaC _computing_data_collection 'Enraf-Nonius Software' #ActaC _computing_cell_refinement 'Enraf-Nonius Software' #ActaC _computing_data_reduction xtal_ADDREF #ActaC _computing_structure_solution xtal #ActaC _computing_structure_refinement xtal_CRYLSQ #ActaC _computing_molecular_graphics xtal #ActaC _computing_publication_material xtal_BONDLA_CIFIO #ActaC _cell_length_a 9.8000(10) #ActaC _cell_length_b 12.192(3) #ActaC _cell_length_c 14.503(2) #ActaC _cell_angle_alpha 90.00000 #ActaC _cell_angle_beta 100.940(10) #ActaC _cell_angle_gamma 90.00000 #ActaC _cell_volume 1701.3(5) #ActaC _cell_formula_units_Z 2 #ActaC _cell_measurement_temperature 293 #ActaC _cell_measurement_reflns_used 14 #ActaC _cell_measurement_theta_min 13.2 #ActaC _cell_measurement_theta_max 26.3 #ActaC _cell_special_details #ActaC ; ? ; _symmetry_cell_setting monoclinic #ActaC _symmetry_space_group_name_H-M p_1_21/c_1 #ActaC _symmetry_space_group_name_Hall -p_2ybc #ActaC loop_ _symmetry_equiv_pos_as_xyz #ActaC +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _exptl_crystal_description ? #ActaC _exptl_crystal_preparation 'from CH2Cl2' _exptl_crystal_colour ? #ActaC _exptl_crystal_size_max 'not recorded' #ActaC _exptl_crystal_size_mid 'not recorded' #ActaC _exptl_crystal_size_min 'not recorded' #ActaC _exptl_crystal_density_diffrn 1.831 #ActaC _exptl_crystal_density_meas ? #ActaC _exptl_crystal_density_method ? #ActaC _exptl_crystal_F_000 920 #ActaC _exptl_absorpt_process_details ? _exptl_absorpt_coefficient_mu 1.55 #ActaC _exptl_absorpt_correction_type 'no correction' #ActaC _exptl_absorpt_correction_T_min 'not recorded' #ActaC _exptl_absorpt_correction_T_max 'not recorded' #ActaC _exptl_special_details #ActaC ; ? ; _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293 #ActaC _diffrn_radiation_wavelength 0.71073 #ActaC _diffrn_radiation_type MoK\a #ActaC _diffrn_radiation_source 'rotating anode' #ActaC _diffrn_radiation_monochromator graphite #ActaC _diffrn_radiation_detector 'single crystal' #ActaC _diffrn_measurement_device ? #ActaC _diffrn_measurement_method 2theta/theta #ActaC _diffrn_standards_number 6 #ActaC _diffrn_standards_interval_count ? #ActaC _diffrn_standards_interval_time 3600sec #ActaC _diffrn_standards_decay_% 0 #ActaC loop_ _diffrn_standard_refln_index_h #ActaC _diffrn_standard_refln_index_k #ActaC _diffrn_standard_refln_index_l #ActaC 4 0 0 -4 0 0 0 10 0 0 -10 0 0 0 12 0 0 -12 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale 1 19.14 _diffrn_reflns_number 4556 #ActaC _diffrn_reflns_av_R_equivalents 0.00 #ActaC _diffrn_reflns_av_sigmaI/netI 0.00 #ActaC _diffrn_reflns_limit_h_min 0 #ActaC _diffrn_reflns_limit_h_max 11 #ActaC _diffrn_reflns_limit_k_min 0 #ActaC _diffrn_reflns_limit_k_max 17 #ActaC _diffrn_reflns_limit_l_min -20 #ActaC _diffrn_reflns_limit_l_max 20 #ActaC _diffrn_reflns_theta_min 2.12 #ActaC _diffrn_reflns_theta_max 30.00 #ActaC _diffrn_reflns_reduction_process ? #ActaC loop_ _atom_type_symbol #ActaC _atom_type_description #ActaC _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real #ActaC _atom_type_scat_dispersion_imag #ActaC _atom_type_scat_source #ActaC C ? 0 52 .002 .002 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 Ru ? 0 4 -1.42 .836 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 Cl ? 0 16 .132 .159 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 O ? 0 8 .008 .006 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 N ? 0 8 .004 .003 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 H ? 0 40 0 0 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 loop_ _atom_site_label #ActaC _atom_site_fract_x #ActaC _atom_site_fract_y #ActaC _atom_site_fract_z #ActaC _atom_site_U_iso_or_equiv #ActaC _atom_site_thermal_displace_type #ActaC _atom_site_calc_flag #ActaC _atom_site_calc_attached_atom #ActaC Ru .33675(3) .05617(2) .012837(18) .02575(17) Uani ? ? Cl1 .50510(11) -.07367(8) .09489(7) .0363(4) Uani ? ? Cl2 .19411(12) .04387(9) .12791(8) .0451(5) Uani ? ? C1 .2416(5) -.0566(3) -.0576(3) .044(2) Uani ? ? O1 .1851(4) -.1255(3) -.1006(3) .076(2) Uani ? ? N11 .4475(3) .1861(3) .0919(2) .0330(14) Uani ? ? C12 .4788(4) .2787(3) .0497(3) .0366(18) Uani ? ? C13 .5633(5) .3585(4) .0982(4) .052(2) Uani ? ? C14 .6181(6) .3447(4) .1916(4) .055(3) Uani ? ? C15 .5845(5) .2505(4) .2356(3) .047(2) Uani ? ? C16 .5006(4) .1729(3) .1838(3) .040(2) Uani ? ? C .4106(5) .3031(3) -.0489(3) .040(2) Uani ? ? O .4664(4) .3662(3) -.0956(2) .0547(18) Uani ? ? N21 .2108(4) .1742(3) -.0573(2) .0380(16) Uani ? ? C22 .2636(5) .2683(3) -.0865(3) .040(2) Uani ? ? C23 .1802(6) .3411(4) -.1473(4) .058(3) Uani ? ? C24 .0414(7) .3194(5) -.1748(4) .075(3) Uani ? ? C25 -.0109(6) .2278(6) -.1443(4) .071(3) Uani ? ? C26 .0731(5) .1563(4) -.0857(4) .052(2) Uani ? ? Cl01 -.0429(5) .3849(3) .1055(4) .216(4) Uani ? ? Cl02 .2366(6) .4456(7) .1631(7) .407(10) Uani ? ? C0 .146(3) .3675(14) .1451(17) .35(2) Uani ? ? H13 .58590 .42270 .06610 .06400 Uiso ? ? H14 .67760 .39910 .22650 .06700 Uiso ? ? H15 .62140 .23870 .30070 .05600 Uiso ? ? H16 .48040 .10660 .21550 .04900 Uiso ? ? H23 .22280 .40500 -.16880 .07100 Uiso ? ? H24 -.01570 .36960 -.21760 .08400 Uiso ? ? H25 -.11030 .21120 -.16150 .08400 Uiso ? ? H26 .03500 .09060 -.06400 .06200 Uiso ? ? H0a .17451 .32447 .09807 .29000 Uiso ? ? H0b .15461 .32571 .20167 .29000 Uiso ? ? loop_ _atom_site_aniso_label #ActaC _atom_site_aniso_U_11 #ActaC _atom_site_aniso_U_22 #ActaC _atom_site_aniso_U_33 #ActaC _atom_site_aniso_U_12 #ActaC _atom_site_aniso_U_13 #ActaC _atom_site_aniso_U_23 #ActaC Ru .0273(2) .02170(16) .02675(16) -.00190(9) .00120(11) -.00022(9) Cl1 .0429(5) .0312(4) .0347(4) .0034(4) .0075(4) .0043(3) Cl2 .0412(6) .0509(6) .0446(6) -.0034(4) .0117(4) .0021(4) C1 .042(3) .038(2) .050(2) -.0028(17) .0040(19) -.0070(17) O1 .065(2) .060(2) .097(3) -.022(2) .001(2) -.032(2) N11 .0356(17) .0278(14) .0350(15) -.0041(12) .0050(13) -.0031(12) C12 .040(2) .0275(17) .043(2) -.0006(15) .0090(17) -.0023(15) C13 .059(3) .034(2) .060(3) -.013(2) .003(2) -.006(2) C14 .058(3) .045(2) .058(3) -.010(2) -.001(2) -.018(2) C15 .047(3) .050(2) .040(2) -.006(2) -.0016(18) -.0113(18) C16 .041(2) .042(2) .0341(19) -.0036(17) .0031(16) -.0046(16) C .052(3) .0255(17) .042(2) -.0013(16) .0081(18) -.0004(15) O .064(2) .0427(17) .056(2) -.0075(15) .0085(16) .0064(15) N21 .0381(19) .0331(16) .0402(17) .0017(14) .0010(14) .0003(13) C22 .047(2) .0324(19) .038(2) .0055(16) .0012(17) .0012(15) C23 .067(3) .045(3) .057(3) .009(2) -.002(2) .010(2) C24 .069(4) .069(4) .074(4) .025(3) -.021(3) .014(3) C25 .042(3) .081(4) .080(4) .005(3) -.014(2) .009(3) C26 .034(2) .057(3) .060(3) .004(2) -.005(2) .001(2) Cl01 .211(4) .129(3) .305(6) -.029(3) .045(4) -.026(3) Cl02 .156(4) .416(12) .579(14) .100(5) -.105(7) -.337(12) C0 .45(3) .226(17) .50(3) .26(2) .43(3) .29(2) _atom_sites_solution_primary Patterson _atom_sites_solution_secondary Fourier _atom_sites_solution_hydrogens 'difference map' _refine_special_details sfls__F_____calc_weight______full_matrix _refine_ls_structure_factor_coef F #ActaC _refine_ls_matrix_type full #ActaC _refine_ls_weighting_scheme calc #ActaC _refine_ls_hydrogen_treatment noref #ActaC _refine_ls_extinction_method Zachariasen #ActaC _refine_ls_extinction_coef 2114(487) #ActaC _refine_ls_extinction_expression Eq22_p292_"Cryst._Comp."_Munksgaard_1970 _refine_ls_abs_structure_details none #ActaC _refine_ls_abs_structure_Flack 0 #ActaC _refine_ls_number_reflns 3880 #ActaC _refine_ls_number_parameters 200 #ActaC _refine_ls_number_restraints 0 #ActaC _refine_ls_number_constraints 0 #ActaC _refine_ls_R_factor_all .048 #ActaC _refine_ls_R_factor_obs .041 #ActaC _refine_ls_wR_factor_all .066 #ActaC _refine_ls_wR_factor_obs .064 #ActaC _refine_ls_goodness_of_fit_all 2.089 #ActaC _refine_ls_goodness_of_fit_obs 2.209 #ActaC _refine_ls_shift/esd_max .051 #ActaC _refine_ls_shift/esd_mean .003 #ActaC _refine_diff_density_min -1.468 #ActaC _refine_diff_density_max 1.546 #ActaC _geom_special_details ? #ActaC loop_ _geom_bond_atom_site_label_1 #ActaC _geom_bond_atom_site_label_2 #ActaC _geom_bond_distance #ActaC _geom_bond_site_symmetry_1 #ActaC _geom_bond_site_symmetry_2 #ActaC _geom_bond_publ_flag #ActaC Ru Cl1 2.4287(10) . . ? Ru Cl2 2.3764(13) . . ? Ru C1 1.856(4) . . ? Ru N11 2.129(3) . . ? Ru N21 2.038(3) . . ? Ru Cl1 2.4100(12) . 3_655 ? C1 O1 1.127(6) . . ? N11 C12 1.347(5) . . ? N11 C16 1.345(5) . . ? C12 C13 1.381(6) . . ? C12 C 1.489(5) . . ? C13 C14 1.370(7) . . ? C13 H13 .957(5) . . ? C14 C15 1.383(7) . . ? C14 H14 .961(5) . . ? C15 C16 1.380(6) . . ? C15 H15 .955(4) . . ? C16 H16 .968(4) . . ? C O 1.220(6) . . ? C C22 1.502(6) . . ? N21 C22 1.359(5) . . ? N21 C26 1.352(6) . . ? C22 C23 1.400(6) . . ? C23 C24 1.369(8) . . ? C23 H23 .963(5) . . ? C24 C25 1.338(10) . . ? C24 H24 .971(6) . . ? C25 C26 1.376(8) . . ? C25 H25 .980(5) . . ? C26 H26 .962(5) . . ? Cl01 C0 1.84(2) . . ? Cl02 C0 1.30(2) . . ? C0 H0a .95(2) . . ? C0 H0b .96(2) . . ? loop_ _geom_contact_atom_site_label_1 #ActaC _geom_contact_atom_site_label_2 #ActaC _geom_contact_distance #ActaC _geom_contact_site_symmetry_1 #ActaC _geom_contact_site_symmetry_2 #ActaC _geom_contact_publ_flag #ActaC Ru Ru 3.5644(5) . 3_655 ? Ru O1 2.982(4) . . ? Ru N11 4.089(3) . 3_655 ? Ru C12 3.050(4) . . ? Ru C16 3.040(4) . . ? Ru C 3.261(4) . . ? Ru C22 2.981(4) . . ? Ru C26 2.968(5) . . ? Ru H16 3.0706(4) . . ? Ru H26 2.9853(4) . . ? Cl1 Cl1 3.2724(14) . 3_655 ? Cl1 Cl2 3.4821(17) . . ? Cl1 Cl2 4.7831(18) . 3_655 ? Cl1 C1 3.072(4) . . ? Cl1 C1 3.080(5) . 3_655 ? Cl1 O1 3.860(4) . . ? Cl1 O1 3.876(4) . 3_655 ? Cl1 N11 3.216(3) . . ? Cl1 N11 3.148(3) . 3_655 ? Cl1 C12 3.286(4) . 3_655 ? Cl1 C14 3.668(6) . 2_645 ? Cl1 C15 3.496(5) . 2_645 ? Cl1 C16 3.275(4) . . ? Cl1 C 3.027(4) . 3_655 ? Cl1 O 3.577(3) . 3_655 ? Cl1 N21 3.183(4) . 3_655 ? Cl1 N21 4.462(3) . . ? Cl1 C22 3.300(4) . 3_655 ? Cl1 Cl02 3.925(9) . 2_645 ? Cl1 H14 3.4331(12) . 2_645 ? Cl1 H15 3.1265(11) . 2_645 ? Cl1 H16 2.8477(11) . . ? Cl2 C1 3.071(5) . . ? Cl2 O1 3.795(4) . 3 ? Cl2 O1 3.892(5) . . ? Cl2 N11 3.153(4) . . ? Cl2 C14 3.782(5) . 2_645 ? Cl2 C16 3.351(4) . . ? Cl2 N21 3.152(4) . . ? Cl2 C23 3.575(6) . 4 ? Cl2 C24 3.852(7) . 4 ? Cl2 C25 3.796(7) . 3 ? Cl2 C26 3.390(5) . . ? Cl2 C26 3.547(5) . 3 ? Cl2 Cl01 4.803(6) . 2_545 ? Cl2 Cl01 4.744(4) . . ? Cl2 H14 2.8543(11) . 2_645 ? Cl2 H16 2.9525(11) . . ? Cl2 H23 2.9742(12) . 4 ? Cl2 H24 3.4799(13) . 4 ? Cl2 H25 3.2764(14) . 3 ? Cl2 H26 2.9758(11) . . ? Cl2 H26 2.7925(12) . 3 ? Cl2 H0a 3.4491(14) . . ? C1 N11 3.549(6) . 3_655 ? C1 N21 2.831(5) . . ? C1 H26 2.694(5) . . ? O1 N11 3.654(5) . 3_655 ? O1 Cl01 3.451(6) . 3 ? N11 C13 2.383(6) . . ? N11 C14 2.776(6) . . ? N11 C15 2.388(5) . . ? N11 C 2.462(5) . . ? N11 O 3.527(5) . . ? N11 N21 2.861(4) . . ? N11 C22 3.030(5) . . ? N11 Cl02 4.020(9) . . ? N11 H13 3.239(3) . . ? N11 H15 3.244(3) . . ? N11 H16 2.009(3) . . ? N11 H0a 3.179(3) . . ? C12 C14 2.384(6) . . ? C12 C15 2.721(6) . . ? C12 C16 2.310(6) . . ? C12 O 2.344(5) . . ? C12 N21 3.063(5) . . ? C12 C22 2.605(5) . . ? C12 Cl02 3.737(10) . . ? C12 H13 2.036(4) . . ? C13 C15 2.365(7) . . ? C13 C16 2.708(6) . . ? C13 C 2.457(6) . . ? C13 O 2.791(6) . . ? C13 Cl01 3.853(7) . 1_655 ? C13 Cl02 3.662(9) . . ? C13 H14 2.042(5) . . ? C14 C16 2.383(7) . . ? C14 Cl01 3.796(8) . 1_655 ? C14 Cl02 3.883(8) . . ? C14 H13 2.025(5) . . ? C14 H15 2.038(5) . . ? C15 H14 2.043(5) . . ? C15 H16 2.023(5) . . ? C16 H15 2.039(4) . . ? C N21 2.495(5) . . ? C C23 2.475(7) . . ? C H13 2.603(4) . . ? C H23 2.596(4) . . ? O N21 3.548(5) . . ? O C22 2.344(6) . . ? O C23 2.779(7) . . ? O H13 2.674(3) . 3_665 ? O H13 2.510(3) . . ? O H15 2.660(4) . 4_554 ? O H23 2.468(3) . . ? N21 C23 2.405(6) . . ? N21 C24 2.777(7) . . ? N21 C25 2.387(6) . . ? N21 Cl01 4.537(6) . . ? N21 Cl02 4.363(11) . 4_554 ? N21 Cl02 4.574(10) . . ? N21 H23 3.258(3) . . ? N21 H25 3.253(3) . . ? N21 H26 1.988(3) . . ? N21 H0a 2.977(4) . . ? C22 C24 2.389(7) . . ? C22 C25 2.707(7) . . ? C22 C26 2.315(7) . . ? C22 H23 2.044(4) . . ? C23 C25 2.334(8) . . ? C23 C26 2.708(8) . . ? C23 Cl01 3.694(7) . 3_565 ? C23 H24 2.026(5) . . ? C24 C26 2.359(8) . . ? C24 Cl01 3.742(8) . 3_565 ? C24 H23 2.049(7) . . ? C24 H25 2.023(7) . . ? C25 Cl01 3.836(9) . 4_554 ? C25 H24 2.025(7) . . ? C25 H26 2.039(7) . . ? C26 H25 2.034(4) . . ? Cl01 Cl01 4.351(7) . 3_565 ? Cl01 Cl02 4.499(11) . 3_565 ? Cl01 Cl02 2.807(7) . . ? Cl01 H13 3.603(5) . 1_455 ? Cl01 H14 3.526(6) . 1_455 ? Cl01 H23 3.335(5) . 3_565 ? Cl01 H24 3.402(4) . 3_565 ? Cl01 H0a 2.276(5) . . ? Cl01 H0b 2.278(5) . . ? Cl02 H16 3.576(7) . 2_655 ? Cl02 H24 3.322(8) . 3_565 ? Cl02 H0a 1.796(9) . . ? Cl02 H0b 1.808(9) . . ? H13 H14 2.3470(3) . . ? H14 H15 2.3475(4) . . ? H15 H16 2.3199(3) . . ? H23 H24 2.3500(2) . . ? H24 H25 2.3532(4) . . ? H25 H26 2.3291(3) . . ? H0a H0b 1.5515(2) . . ? loop_ _geom_angle_atom_site_label_1 #ActaC _geom_angle_atom_site_label_2 #ActaC _geom_angle_atom_site_label_3 #ActaC _geom_angle #ActaC _geom_angle_site_symmetry_1 #ActaC _geom_angle_site_symmetry_2 #ActaC _geom_angle_site_symmetry_3 #ActaC _geom_angle_publ_flag #ActaC Cl1 Ru Cl2 92.88(4) . . . ? Cl1 Ru C1 90.60(13) . . . ? Cl1 Ru N11 89.50(9) . . . ? Cl1 Ru N21 174.65(11) . . . ? Cl1 Ru Cl1 85.11(4) . . 3_655 ? Cl2 Ru C1 92.23(17) . . . ? Cl2 Ru N11 88.64(10) . . . ? Cl2 Ru N21 90.79(11) . . . ? Cl2 Ru Cl1 175.77(6) . . 3_655 ? C1 Ru N11 179.12(17) . . . ? C1 Ru N21 93.16(16) . . . ? C1 Ru Cl1 91.51(16) . . 3_655 ? N11 Ru N21 86.68(12) . . . ? N11 Ru Cl1 87.62(10) . . 3_655 ? N21 Ru Cl1 90.98(11) . . 3_655 ? Ru Cl1 Ru 94.89(4) . . 3_655 ? Ru C1 O1 179.3(5) . . . ? Ru N11 C12 121.0(2) . . . ? Ru N11 C16 120.4(3) . . . ? C12 N11 C16 118.2(3) . . . ? N11 C12 C13 121.7(4) . . . ? N11 C12 C 120.3(3) . . . ? C13 C12 C 117.7(4) . . . ? C12 C13 C14 120.1(4) . . . ? C12 C13 H13 120.0(5) . . . ? C14 C13 H13 119.9(5) . . . ? C13 C14 C15 118.4(4) . . . ? C13 C14 H14 121.4(5) . . . ? C15 C14 H14 120.2(5) . . . ? C14 C15 C16 119.2(4) . . . ? C14 C15 H15 120.2(4) . . . ? C16 C15 H15 120.6(5) . . . ? N11 C16 C15 122.4(4) . . . ? N11 C16 H16 119.6(4) . . . ? C15 C16 H16 118.0(4) . . . ? C12 C O 119.4(4) . . . ? C12 C C22 121.1(4) . . . ? O C C22 118.5(4) . . . ? Ru N21 C22 121.4(3) . . . ? Ru N21 C26 120.9(3) . . . ? C22 N21 C26 117.3(4) . . . ? C C22 N21 121.4(3) . . . ? C C22 C23 117.0(4) . . . ? N21 C22 C23 121.4(4) . . . ? C22 C23 C24 119.3(5) . . . ? C22 C23 H23 118.7(5) . . . ? C24 C23 H23 122.0(5) . . . ? C23 C24 C25 119.2(6) . . . ? C23 C24 H24 119.0(6) . . . ? C25 C24 H24 121.8(6) . . . ? C24 C25 C26 120.7(5) . . . ? C24 C25 H25 120.9(6) . . . ? C26 C25 H25 118.4(6) . . . ? N21 C26 C25 122.1(5) . . . ? N21 C26 H26 117.5(4) . . . ? C25 C26 H26 120.4(5) . . . ? Cl01 C0 Cl02 126.2(13) . . . ? Cl01 C0 H0a 105.1(17) . . . ? Cl01 C0 H0b 105(2) . . . ? Cl02 C0 H0a 105(2) . . . ? Cl02 C0 H0b 106(2) . . . ? H0a C0 H0b 109.3(18) . . . ? loop_ _geom_torsion_atom_site_label_1 #ActaC _geom_torsion_atom_site_label_2 #ActaC _geom_torsion_atom_site_label_3 #ActaC _geom_torsion_atom_site_label_4 #ActaC _geom_torsion #ActaC _geom_torsion_site_symmetry_1 #ActaC _geom_torsion_site_symmetry_2 #ActaC _geom_torsion_site_symmetry_3 #ActaC _geom_torsion_site_symmetry_4 #ActaC _geom_torsion_publ_flag #ActaC ? ? ? ? ? ? ? ? ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min -20 _reflns_limit_l_max 20 _reflns_number_total 4556 #ActaC _reflns_number_observed 3880 #ActaC _reflns_observed_criterion refl_observed_if_I____>3.000_sigma(I___) _reflns_d_resolution_high .711 _reflns_d_resolution_low 9.622 loop_ _reflns_scale_group_code _reflns_scale_meas_F 1 1.0595 _publ_requested_journal ? #ActaC _publ_requested_coeditor_name ? #ActaC _publ_contact_author #ActaC ; G.B.Deacon Monash University Chemistry Department Clayton Victoria Australia 3168 ; _publ_contact_letter #ActaC ; ? letter to co-editor ; _publ_contact_author_phone 61_3_9905_4568 #ActaC _publ_contact_author_fax 61_3_9905_4597 #ActaC _publ_contact_author_email ? #ActaC loop_ _publ_author_name #ActaC _publ_author_address #ActaC '? surname, initials' ; ? institute ? department ? address ? city ? country ; _publ_section_title #ActaC ; ? ; _publ_section_abstract #ActaC ; ? ; _publ_section_comment #ActaC ; ? ; _publ_section_experimental #ActaC ; ? ; _publ_section_references #ActaC ; ? ; _publ_section_figure_captions #ActaC ; ? ; _publ_section_acknowledgements #ActaC ; ? ; #============================================================================== # (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ?