#------------------------------------------------------------------------------ #$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $ #$Revision: 176467 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/11/49/4114999.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4114999 loop_ _publ_author_name 'Andrey Yu. Kovalevsky' 'Kimberly A. Bagley' 'Philip Coppens' _publ_section_title ; The First Photocrystallographic Evidence for Light-Induced Metastable Linkage Isomers of Ruthenium Sulfur Dioxide Complexes ; _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 9241 _journal_page_last 9248 _journal_paper_doi 10.1021/ja026045c _journal_volume 124 _journal_year 2002 _chemical_formula_sum 'Cl2 H12 N4 O2 Ru S' _chemical_formula_weight 304.17 _chemical_name_common trans-[Ru(II)(NH3)4Cl(SO2)]Cl _chemical_name_systematic ; trans-Tetraamminechloro(sulfur dioxide)ruthenium(II) chloride ; _space_group_IT_number 62 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_space_group_name_H-M 'P n m a' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 13.8859(17) _cell_length_b 7.2451(9) _cell_length_c 9.2462(11) _cell_measurement_reflns_used 745 _cell_measurement_temperature 90(1) _cell_measurement_theta_max 30 _cell_measurement_theta_min 4 _cell_volume 930.2(2) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 90(1) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'rotating anode' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0984 _diffrn_reflns_av_sigmaI/netI 0.0507 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 13678 _diffrn_reflns_theta_full 30.07 _diffrn_reflns_theta_max 30.07 _diffrn_reflns_theta_min 2.65 _exptl_absorpt_coefficient_mu 2.442 _exptl_absorpt_correction_T_max 0.9086 _exptl_absorpt_correction_T_min 0.8381 _exptl_absorpt_correction_type 'face-indexed non-empirical' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 2.172 _exptl_crystal_description parallelepiped _exptl_crystal_F_000 600 _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _refine_diff_density_max 1.024 _refine_diff_density_min -2.872 _refine_diff_density_rms 0.274 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.278 _refine_ls_hydrogen_treatment 'ideal NH3 groups' _refine_ls_matrix_type full _refine_ls_number_parameters 57 _refine_ls_number_reflns 1467 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.278 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_gt 0.0353 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean <0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0682 _refine_ls_wR_factor_ref 0.0734 _reflns_number_gt 1180 _reflns_number_total 1467 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ja026045c_s2_1.cif _cod_data_source_block RuSO2Cl_dark _cod_original_formula_sum 'H12 Cl2 N4 O2 Ru S' _cod_database_code 4114999 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' 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 Ru1 Ru 0.08542(2) 0.7500 0.78014(4) 0.00632(10) Uani 1 2 d S Cl1 Cl 0.00313(8) 0.7500 1.00925(12) 0.0124(2) Uani 1 2 d S Cl2 Cl 0.15101(7) 0.2500 0.56661(12) 0.0137(2) Uani 1 2 d S S1 S 0.16650(8) 0.7500 0.59102(13) 0.0122(2) Uani 1 2 d S N1 N 0.17384(17) 0.9579(4) 0.8692(3) 0.0128(5) Uani 1 1 d . H1A H 0.2236 0.9049 0.9178 0.019 Uiso 1 1 calc R H1B H 0.1386 1.0283 0.9312 0.019 Uiso 1 1 calc R H1C H 0.1974 1.0302 0.7969 0.019 Uiso 1 1 calc R N2 N -0.01260(18) 0.9538(4) 0.7091(3) 0.0116(5) Uani 1 1 d . H2A H -0.0536 0.9038 0.6431 0.017 Uiso 1 1 calc R H2B H 0.0204 1.0485 0.6676 0.017 Uiso 1 1 calc R H2C H -0.0468 0.9969 0.7859 0.017 Uiso 1 1 calc R O1 O 0.2708(2) 0.7500 0.6022(4) 0.0197(7) Uani 1 2 d S O2 O 0.1302(3) 0.7500 0.4467(4) 0.0199(7) 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 Ru1 0.00760(15) 0.00563(15) 0.00574(16) 0.000 -0.00036(12) 0.000 Cl1 0.0154(5) 0.0116(5) 0.0102(5) 0.000 0.0022(4) 0.000 Cl2 0.0129(4) 0.0156(5) 0.0128(5) 0.000 0.0029(4) 0.000 S1 0.0130(5) 0.0101(5) 0.0135(5) 0.000 0.0039(4) 0.000 N1 0.0111(11) 0.0104(12) 0.0170(14) -0.0003(10) -0.0019(10) -0.0007(9) N2 0.0124(11) 0.0112(11) 0.0113(13) 0.0000(10) -0.0019(10) 0.0028(9) O1 0.0171(16) 0.0274(18) 0.0145(17) 0.000 0.0047(13) 0.000 O2 0.0239(18) 0.0175(17) 0.0182(18) 0.000 0.0050(14) 0.000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source N N 0.0061 0.0033 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 S1 Ru1 N1 90.75(8) . . S1 Ru1 N1 90.75(8) . 7_575 N1 Ru1 N1 91.08(14) . 7_575 S1 Ru1 N2 95.00(8) . 7_575 N1 Ru1 N2 174.16(10) . 7_575 N1 Ru1 N2 89.84(10) 7_575 7_575 S1 Ru1 N2 95.00(8) . . N1 Ru1 N2 89.84(10) . . N1 Ru1 N2 174.16(10) 7_575 . N2 Ru1 N2 88.67(14) 7_575 . S1 Ru1 Cl1 175.57(4) . . N1 Ru1 Cl1 86.15(8) . . N1 Ru1 Cl1 86.15(8) 7_575 . N2 Ru1 Cl1 88.16(7) 7_575 . N2 Ru1 Cl1 88.16(8) . . O2 S1 O1 114.8(2) . . O2 S1 Ru1 126.54(16) . . O1 S1 Ru1 118.67(15) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Ru1 S1 2.0797(12) . Ru1 N1 2.110(2) . Ru1 N1 2.110(2) 7_575 Ru1 N2 2.113(2) 7_575 Ru1 N2 2.113(2) . Ru1 Cl1 2.4069(12) . S1 O2 1.426(4) . S1 O1 1.451(3) . 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 N1 Ru1 S1 O2 -134.45(7) . N1 Ru1 S1 O2 134.45(7) 7_575 N2 Ru1 S1 O2 44.55(7) 7_575 N2 Ru1 S1 O2 -44.55(7) . Cl1 Ru1 S1 O2 180.000(2) . N1 Ru1 S1 O1 45.55(7) . N1 Ru1 S1 O1 -45.55(7) 7_575 N2 Ru1 S1 O1 -135.45(7) 7_575 N2 Ru1 S1 O1 135.45(7) . Cl1 Ru1 S1 O1 0.000(3) .