# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'ProfD Peter Klufers' _publ_contact_author_email KLUEF@CUP.UNI-MUENCHEN.DE _publ_section_title ; Photoinduced Linkage Isomerism of {RuNO}6 Complexes with Bioligands and Related Chelators ; loop_ _publ_author_name P.Klufers 'Dominik Schaniel' 'Theo Woike' 'Anna Zangl' # Attachment 'zangl1.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 685117' #:---------------------------------------------------------------------------- #:---------------------------CRYSTAL DATA------------------------------------- #:---------------------------------------------------------------------------- _audit_author_name 'Zangl, A.' _audit_block_code Ru_NO_Cl_Cl_L-HisH-1_kn113_Zangl _audit_creation_method 'form98_non/compatible with shelxl97-2' _audit_creation_date 27-Mar-07 _chemical_name_systematic ? _chemical_compound_source ; K2[Ru(NO)Cl5] (658 mg, 1.70 mmol), L-histidine monohydrochloride monohydrate (358 mg, 1.71 mmol) and KCl (1.26 g, 16.9 mmol) are solved in 250 mL H2O. The pH value of the solution is adjusted to 4 with 0.1 M HCl. After refluxing for 2 hours the resulting light brown solution is evaporated to dryness on a rotary evaporator. The residue is suspended in a small amount of H2O and purified by centrifugation (3 times). Then the resulting brown solid is vacuum-dried. Crystals suitable for X-ray crystallography can be obtained from a diluted aqueous solution of the complex in H2O by slow evaporation of the solvent at room temperature. ; _chemical_name_common (Ru(NO)Cl2(L-HisH-1)) _chemical_formula_moiety 'C6 H8 Cl2 N4 O3 Ru' _chemical_formula_sum 'C6 H8 Cl2 N4 O3 Ru' _chemical_formula_weight 356.13 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 8.2032(2) _cell_length_b 10.7355(3) _cell_length_c 12.9656(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1141.82(5) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9230 _cell_measurement_theta_min 3.134 _cell_measurement_theta_max 27.485 _cell_special_details ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.07169(9) _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 1.838 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ; Sheldrick, G.M. SADABS. Version 2. Multi-Scan Absorption Correction Program. University of G\"ottingen, Germany, 2001. spherical correction included with mu*r = 0.073, leads to Tmin/Tmax = 0.6338 ; _exptl_special_details ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 4 2 0.060000 -1 -4 -2 0.050000 -2 -1 8 0.060000 2 1 -8 0.020000 -5 4 -3 0.020000 5 -4 3 0.010000 -1 2 13 0.053000 3 6 -5 0.036000 loop_ _diffrn_radiation_wavelength_id 0.71073 #?# _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'MONTEL, graded multilayered X-ray optics' _diffrn_radiation_collimation 0.20 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 9 _diffrn_special_details ? _diffrn_reflns_number 13632 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0302 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.50 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.400 _refine_diff_density_min -0.653 _refine_diff_density_rms 0.080 _reflns_number_total 2614 _reflns_number_gt 2485 _reflns_threshold_expression >2sigma(I) _reflns_special_details ? _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution ; A. Altomare, M. C. Burla, M. Camalli, G. L. Cascarano, C. Giacovazzo, A. Guagliardi, A. G. G. Moliterni, G. Polidori, R. Spagna: SIR97: a new tool for crystal structure determination and refinement; J. Appl. Crystallogr. 1999, 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)' _computing_molecular_graphics ? _computing_publication_material ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refall _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 -0.02(3) _refine_ls_number_reflns 2614 _refine_ls_number_parameters 177 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0243 _refine_ls_R_factor_gt 0.0215 _refine_ls_wR_factor_ref 0.0449 _refine_ls_wR_factor_gt 0.0437 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_special_details ? 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 Ru Ru 0.91268(3) 0.225533(19) 0.274796(15) 0.01527(6) Uani 1 1 d . . . Cl1 Cl 1.15444(9) 0.33807(7) 0.24014(6) 0.03268(18) Uani 1 1 d . . . Cl2 Cl 0.84433(10) 0.36471(7) 0.40996(5) 0.02663(17) Uani 1 1 d . . . O1 O 1.0744(3) 0.0605(2) 0.41631(17) 0.0354(5) Uani 1 1 d . . . O11 O 0.8005(2) 0.34025(17) 0.17488(14) 0.0203(4) Uani 1 1 d . . . O12 O 0.6799(3) 0.34993(19) 0.02285(16) 0.0297(5) Uani 1 1 d . . . N1 N 1.0100(3) 0.1247(2) 0.35823(18) 0.0208(5) Uani 1 1 d . . . N2 N 0.9452(3) 0.1266(2) 0.13885(18) 0.0200(5) Uani 1 1 d . . . H721 H 0.956(4) 0.041(3) 0.148(2) 0.023(8) Uiso 1 1 d . . . H722 H 1.024(4) 0.151(4) 0.110(3) 0.035(11) Uiso 1 1 d . . . N5 N 0.6887(3) 0.1374(2) 0.28588(17) 0.0191(5) Uani 1 1 d . . . N7 N 0.4734(3) 0.0512(3) 0.3513(2) 0.0321(7) Uani 1 1 d . . . H77 H 0.413(6) 0.032(4) 0.390(3) 0.047(13) Uiso 1 1 d . . . C1 C 0.7574(3) 0.2928(3) 0.0871(2) 0.0198(6) Uani 1 1 d . . . C2 C 0.8043(4) 0.1561(3) 0.0708(2) 0.0212(6) Uani 1 1 d . . . H2 H 0.824(3) 0.148(3) 0.000(2) 0.017(8) Uiso 1 1 d . . . C3 C 0.6605(4) 0.0727(3) 0.0970(2) 0.0248(7) Uani 1 1 d . . . H31 H 0.578(5) 0.094(3) 0.050(3) 0.034(9) Uiso 1 1 d . . . H32 H 0.690(4) -0.017(3) 0.082(2) 0.028(9) Uiso 1 1 d . . . C4 C 0.6044(3) 0.0794(2) 0.2070(2) 0.0202(6) Uani 1 1 d . . . C6 C 0.6049(4) 0.1185(3) 0.3721(2) 0.0250(6) Uani 1 1 d . . . H6 H 0.632(4) 0.151(3) 0.435(3) 0.035(10) Uiso 1 1 d . . . C8 C 0.4703(4) 0.0266(3) 0.2483(2) 0.0311(8) Uani 1 1 d . . . H8 H 0.393(5) -0.012(3) 0.221(3) 0.041(10) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.01655(10) 0.01315(10) 0.01610(10) -0.00016(9) -0.00154(9) -0.00014(9) Cl1 0.0240(3) 0.0290(4) 0.0451(5) -0.0004(3) 0.0019(3) -0.0101(3) Cl2 0.0351(4) 0.0246(4) 0.0202(3) -0.0079(3) -0.0022(3) 0.0015(3) O1 0.0441(13) 0.0304(12) 0.0317(11) 0.0059(9) -0.0106(12) 0.0085(12) O11 0.0246(10) 0.0174(9) 0.0189(9) -0.0025(8) -0.0021(8) 0.0026(8) O12 0.0398(13) 0.0274(11) 0.0220(10) 0.0020(9) -0.0096(10) 0.0061(10) N1 0.0229(12) 0.0186(12) 0.0208(12) -0.0018(10) -0.0026(10) -0.0020(11) N2 0.0228(14) 0.0171(13) 0.0200(12) -0.0007(10) 0.0042(11) 0.0024(10) N5 0.0180(11) 0.0201(11) 0.0191(11) -0.0010(10) 0.0015(10) -0.0008(9) N7 0.0229(14) 0.0415(17) 0.0319(15) 0.0036(13) 0.0068(13) -0.0081(13) C1 0.0195(13) 0.0231(16) 0.0167(12) 0.0015(11) 0.0017(11) -0.0014(12) C2 0.0263(15) 0.0226(15) 0.0146(13) -0.0037(12) 0.0003(12) 0.0022(12) C3 0.0275(16) 0.0235(16) 0.0233(15) -0.0045(13) -0.0033(14) -0.0049(14) C4 0.0191(13) 0.0198(13) 0.0218(14) -0.0017(11) -0.0022(12) -0.0002(12) C6 0.0231(15) 0.0303(16) 0.0217(14) 0.0004(12) 0.0031(14) -0.0043(14) C8 0.0261(17) 0.0329(17) 0.0344(18) -0.0007(13) -0.0025(14) -0.0103(14) 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 Ru N1 1.726(2) . ? Ru O11 2.0102(19) . ? Ru N5 2.072(2) . ? Ru N2 2.075(2) . ? Ru Cl1 2.3653(7) . ? Ru Cl2 2.3702(7) . ? O1 N1 1.149(3) . ? O11 C1 1.296(3) . ? O12 C1 1.214(3) . ? N2 C2 1.489(4) . ? N2 H721 0.93(3) . ? N2 H722 0.79(4) . ? N5 C6 1.327(4) . ? N5 C4 1.383(3) . ? N7 C6 1.326(4) . ? N7 C8 1.362(4) . ? N7 H77 0.73(4) . ? C1 C2 1.532(4) . ? C2 C3 1.519(4) . ? C2 H2 0.94(3) . ? C3 C4 1.500(4) . ? C3 H31 0.94(4) . ? C3 H32 1.01(3) . ? C4 C8 1.348(4) . ? C6 H6 0.91(4) . ? C8 H8 0.83(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 _geom_angle_publ_flag N1 Ru O11 178.66(10) . . ? N1 Ru N5 94.63(10) . . ? O11 Ru N5 85.32(8) . . ? N1 Ru N2 98.73(11) . . ? O11 Ru N2 79.92(8) . . ? N5 Ru N2 86.53(10) . . ? N1 Ru Cl1 92.95(8) . . ? O11 Ru Cl1 87.04(6) . . ? N5 Ru Cl1 171.92(7) . . ? N2 Ru Cl1 89.55(8) . . ? N1 Ru Cl2 92.37(8) . . ? O11 Ru Cl2 88.97(5) . . ? N5 Ru Cl2 91.53(7) . . ? N2 Ru Cl2 168.84(7) . . ? Cl1 Ru Cl2 90.96(3) . . ? C1 O11 Ru 116.76(17) . . ? O1 N1 Ru 177.7(2) . . ? C2 N2 Ru 107.13(17) . . ? C2 N2 H721 111(2) . . ? Ru N2 H721 114(2) . . ? C2 N2 H722 106(3) . . ? Ru N2 H722 110(3) . . ? H721 N2 H722 108(3) . . ? C6 N5 C4 107.1(2) . . ? C6 N5 Ru 126.0(2) . . ? C4 N5 Ru 126.73(18) . . ? C6 N7 C8 108.6(3) . . ? C6 N7 H77 125(3) . . ? C8 N7 H77 127(3) . . ? O12 C1 O11 123.2(3) . . ? O12 C1 C2 121.4(3) . . ? O11 C1 C2 115.4(2) . . ? N2 C2 C3 110.2(2) . . ? N2 C2 C1 108.5(2) . . ? C3 C2 C1 109.8(2) . . ? N2 C2 H2 115.4(17) . . ? C3 C2 H2 107.0(17) . . ? C1 C2 H2 105.7(18) . . ? C4 C3 C2 115.0(2) . . ? C4 C3 H31 113(2) . . ? C2 C3 H31 105(2) . . ? C4 C3 H32 107.3(18) . . ? C2 C3 H32 109.6(19) . . ? H31 C3 H32 106(3) . . ? C8 C4 N5 107.7(2) . . ? C8 C4 C3 127.4(3) . . ? N5 C4 C3 124.8(3) . . ? N7 C6 N5 109.5(3) . . ? N7 C6 H6 126(2) . . ? N5 C6 H6 124(2) . . ? C4 C8 N7 107.0(3) . . ? C4 C8 H8 131(3) . . ? N7 C8 H8 121(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag N2 H721 Cl2 0.93(3) 2.61(3) 3.359(2) 137(2) 4_745 ? N2 H721 Cl1 0.93(3) 2.77(3) 3.567(3) 144(3) 4_745 ? N2 H722 O12 0.79(4) 2.14(4) 2.857(3) 150(4) 3 ? N7 H77 O12 0.73(4) 2.38(4) 2.985(4) 141(4) 4_645 ? N7 H77 Cl2 0.73(4) 2.88(4) 3.393(3) 130(4) 3_456 ? _geom_special_details ;Puckering parameters (\%A, \%) according to D. Cremer, J. A. Pople, J. Am. Chem. Soc. 1975, 97, 1354--1358 Ru O11 C1 C2 N2 Q2 = 0.397(2) \f2 = 149.5(4) N5 C4 C8 N7 C6 No C & P - Puckering Analysis since = 0.4 < 5.0 Deg Ru N2 C2 C3 C4 N5 Q = 0.685(3) \q = 129.9(3) \f = 252.1(3) ; data_2 _database_code_depnum_ccdc_archive 'CCDC 685118' #:---------------------------------------------------------------------------- #:---------------------------CRYSTAL DATA------------------------------------- #:---------------------------------------------------------------------------- _audit_author_name 'Zangl, A.' _audit_block_code Ru_NO_Cl_Cl_DL-AmAlaH-1_ln069_Zangl _audit_creation_method 'form98_non/compatible with shelxl97-2' _audit_creation_date 09-Feb-07 _chemical_name_systematic ? _chemical_compound_source ; K2[Ru(NO)Cl5] (802 mg, 2.08 mmol), DL-2,3-Diaminopropionic acid monohydrochlorid (584 mg, 4.15 mmol) and KCl (1.55 g, 20.8 mmol) are solved in 250 mL H2O. The pH-value of the solution is adjusted to 4 with a concentrated solution of KOH in H2O. Then the mixture is refluxed for 2 hours and the resulting orange solution is evaporated to dryness on a rotary evaporator. The residue is suspended in a small amount of H2O and purified by centrifugation. This procedure is repeated three times, then the resulting orange solid is vacuum-dried. Crystals are obtained by heating the solid in little H2O until a clear solution results which is left standing to slowly cool down to room temperature. Within a day small orange crystals emerge from the solution. ; _chemical_name_common (Ru(NO)Cl2(DL-AmAlaH-1)) _chemical_formula_moiety 'C3 H7 Cl2 N3 O3 Ru' _chemical_formula_sum 'C3 H7 Cl2 N3 O3 Ru' _chemical_formula_weight 305.08 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_Int_Tables_number 14 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 6.5310(3) _cell_length_b 12.4611(5) _cell_length_c 10.2292(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.043(3) _cell_angle_gamma 90.00 _cell_volume 832.49(6) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 7698 _cell_measurement_theta_min 3.134 _cell_measurement_theta_max 27.485 _cell_special_details ? _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.055 _exptl_crystal_size_mid 0.045 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.43418(18) _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 592 _exptl_absorpt_coefficient_mu 2.494 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ; Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press (New York). ; _exptl_special_details ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 1 0.005000 0 0 -1 0.005000 -1 -6 0 0.040000 1 6 0 0.015000 2 0 1 0.020000 -2 0 -1 0.025000 loop_ _diffrn_radiation_wavelength_id 0.71073 #?# _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'MONTEL, graded multilayered X-ray optics' _diffrn_radiation_collimation 0.20 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 9 _diffrn_special_details ? _diffrn_reflns_number 3660 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0465 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.27 _diffrn_reflns_theta_max 27.54 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.975 _refine_diff_density_min -0.756 _refine_diff_density_rms 0.139 _reflns_number_total 1903 _reflns_number_gt 1563 _reflns_threshold_expression >2sigma(I) _reflns_special_details ? _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution ; A. Altomare, M. C. Burla, M. Camalli, G. L. Cascarano, C. Giacovazzo, A. Guagliardi, A. G. G. Moliterni, G. Polidori, R. Spagna: SIR97: a new tool for crystal structure determination and refinement; J. Appl. Crystallogr. 1999, 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)' _computing_molecular_graphics ? _computing_publication_material ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1903 _refine_ls_number_parameters 137 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0448 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0648 _refine_ls_wR_factor_gt 0.0591 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_special_details ; N-bonded H: DFIX 21 0.01 N2 H721 N2 H722 N3 H731 N3 H732 DFIX 21.60 0.02 H721 H722 H731 H732 FVAR 0.16778 0.82441 N-bonded H732: refall, riding with U(H)=1.2*U(C) ; 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 Ru Ru 0.89148(4) 0.18476(2) 0.30094(2) 0.01612(10) Uani 1 1 d . . . Cl1 Cl 0.79235(14) 0.03310(7) 0.17747(8) 0.0265(2) Uani 1 1 d . . . Cl2 Cl 1.20116(13) 0.19486(7) 0.17883(8) 0.0251(2) Uani 1 1 d . . . O1 O 1.1173(4) 0.0930(2) 0.5146(2) 0.0320(6) Uani 1 1 d . . . O11 O 0.7665(3) 0.27497(18) 0.1577(2) 0.0194(5) Uani 1 1 d . . . O12 O 0.6157(4) 0.43228(19) 0.1222(2) 0.0295(6) Uani 1 1 d . . . N1 N 1.0174(4) 0.1225(2) 0.4297(3) 0.0202(6) Uani 1 1 d . . . N2 N 0.9057(5) 0.3370(2) 0.3840(3) 0.0204(6) Uani 1 1 d D . . H721 H 0.997(4) 0.376(2) 0.357(3) 0.013(9) Uiso 1 1 d D . . H722 H 0.915(5) 0.332(2) 0.4642(18) 0.014(9) Uiso 1 1 d D . . N3 N 0.5975(4) 0.1940(2) 0.3803(3) 0.0196(6) Uani 1 1 d D . . H731 H 0.586(5) 0.157(2) 0.447(2) 0.020(10) Uiso 1 1 d D . . H732 H 0.521(5) 0.168(2) 0.325(3) 0.024 Uiso 1 1 d D . . C1 C 0.6908(5) 0.3665(3) 0.1965(3) 0.0218(7) Uani 1 1 d . . . C2 C 0.7022(5) 0.3809(3) 0.3450(3) 0.0215(7) Uani 1 1 d . . . H2 H 0.697(5) 0.454(3) 0.371(3) 0.013(8) Uiso 1 1 d . . . C3 C 0.5424(6) 0.3077(3) 0.4078(3) 0.0227(8) Uani 1 1 d . . . H31 H 0.409(6) 0.326(3) 0.378(3) 0.020(9) Uiso 1 1 d . . . H32 H 0.543(6) 0.322(3) 0.502(4) 0.030(11) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.01634(16) 0.01996(16) 0.01206(15) 0.00027(10) 0.00027(11) 0.00063(11) Cl1 0.0304(5) 0.0222(4) 0.0269(4) -0.0040(4) -0.0016(4) 0.0005(4) Cl2 0.0173(4) 0.0370(5) 0.0211(4) 0.0021(4) 0.0031(4) 0.0017(4) O1 0.0395(15) 0.0313(13) 0.0253(13) 0.0029(11) -0.0130(12) 0.0065(12) O11 0.0201(12) 0.0249(12) 0.0131(11) -0.0005(10) -0.0005(9) 0.0021(10) O12 0.0398(16) 0.0290(14) 0.0197(12) 0.0060(11) -0.0005(11) 0.0106(12) N1 0.0228(15) 0.0186(14) 0.0192(14) 0.0010(12) -0.0006(13) 0.0002(12) N2 0.0202(16) 0.0260(16) 0.0151(14) 0.0003(13) -0.0013(13) -0.0044(13) N3 0.0177(15) 0.0242(16) 0.0168(14) -0.0001(12) 0.0010(12) -0.0009(12) C1 0.0209(18) 0.0265(19) 0.0181(16) -0.0017(15) 0.0006(14) -0.0025(15) C2 0.0242(19) 0.0229(18) 0.0175(17) -0.0009(14) -0.0005(15) 0.0036(15) C3 0.0215(19) 0.029(2) 0.0178(18) -0.0020(14) -0.0005(15) 0.0064(15) 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 Ru N1 1.735(3) . ? Ru O11 2.019(2) . ? Ru N2 2.081(3) . ? Ru N3 2.088(3) . ? Ru Cl1 2.3632(8) . ? Ru Cl2 2.3813(9) . ? O1 N1 1.146(3) . ? O11 C1 1.305(4) . ? O12 C1 1.220(4) . ? N2 C2 1.492(4) . ? N2 H721 0.817(18) . ? N2 H722 0.825(18) . ? N3 C3 1.489(4) . ? N3 H731 0.830(18) . ? N3 H732 0.819(18) . ? C1 C2 1.531(4) . ? C2 C3 1.528(5) . ? C2 H2 0.95(3) . ? C3 H31 0.95(4) . ? C3 H32 0.98(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 _geom_angle_publ_flag N1 Ru O11 172.29(11) . . ? N1 Ru N2 94.39(12) . . ? O11 Ru N2 78.84(10) . . ? N1 Ru N3 99.50(12) . . ? O11 Ru N3 83.10(10) . . ? N2 Ru N3 80.31(12) . . ? N1 Ru Cl1 100.25(9) . . ? O11 Ru Cl1 86.96(7) . . ? N2 Ru Cl1 163.64(8) . . ? N3 Ru Cl1 90.02(8) . . ? N1 Ru Cl2 91.12(10) . . ? O11 Ru Cl2 86.16(7) . . ? N2 Ru Cl2 97.36(9) . . ? N3 Ru Cl2 169.26(8) . . ? Cl1 Ru Cl2 89.68(3) . . ? C1 O11 Ru 114.77(19) . . ? O1 N1 Ru 171.0(3) . . ? C2 N2 Ru 100.7(2) . . ? C2 N2 H721 110(2) . . ? Ru N2 H721 116(2) . . ? C2 N2 H722 111(2) . . ? Ru N2 H722 110(2) . . ? H721 N2 H722 109(2) . . ? C3 N3 Ru 110.4(2) . . ? C3 N3 H731 111(2) . . ? Ru N3 H731 112(2) . . ? C3 N3 H732 111(2) . . ? Ru N3 H732 106(3) . . ? H731 N3 H732 107(2) . . ? O12 C1 O11 123.4(3) . . ? O12 C1 C2 123.9(3) . . ? O11 C1 C2 112.7(3) . . ? N2 C2 C3 106.1(3) . . ? N2 C2 C1 105.3(3) . . ? C3 C2 C1 108.3(3) . . ? N2 C2 H2 108(2) . . ? C3 C2 H2 116(2) . . ? C1 C2 H2 112.8(19) . . ? N3 C3 C2 108.9(3) . . ? N3 C3 H31 113(2) . . ? C2 C3 H31 111(2) . . ? N3 C3 H32 111(2) . . ? C2 C3 H32 108(2) . . ? H31 C3 H32 106(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag N2 H721 Cl1 0.817(18) 2.42(2) 3.202(3) 162(3) 2_755 ? N2 H722 O11 0.825(18) 2.58(2) 3.259(4) 140(2) 4_566 ? N2 H722 Cl1 0.825(18) 2.87(3) 3.491(3) 134(3) 4_566 ? N2 H722 Cl2 0.825(18) 2.90(2) 3.601(3) 144(3) 4_566 ? N3 H731 O12 0.830(18) 2.116(19) 2.935(4) 169(3) 4_566 ? N3 H731 O11 0.830(18) 2.60(3) 3.068(4) 117(2) 4_566 ? N3 H732 Cl2 0.819(18) 2.59(3) 3.307(3) 147(3) 1_455 ? _geom_special_details ;Puckering parameters (\%A, \%) according to D. Cremer, J. A. Pople, J. Am. Chem. Soc. 1975, 97, 1354--1358 Ru O11 C1 C2 N2 Q2 = 0.579(3) \f2 = 324.1(3) Ru N2 C2 C3 N3 Q2 = 0.612(3) \f2 = 41.5(3) Ru O11 C1 C2 C3 N3 Q = 1.145(3) \q = 99.41(15) \f = 176.75(16) ; data_3 _database_code_depnum_ccdc_archive 'CCDC 685119' #:---------------------------------------------------------------------------- #:---------------------------CRYSTAL DATA------------------------------------- #:---------------------------------------------------------------------------- _audit_author_name 'Mayer, P.' _audit_block_code Ru_NO_Cl_Cl_Cl_KojH-1_K_ln031_Zangl _audit_creation_method 'form98_non/compatible with shelxl97-2' _audit_creation_date 16-Jan-07 _chemical_name_systematic ? _chemical_compound_source ; K2[Ru(NO)Cl5] (355 mg, 0.918 mmol) and kojic acid (130 mg, 0.915 mmol) are solved in 100 mL H2O. The pH value of the solution is adjusted to about 5 with a concentrated solution of KOH in H2O, then the mixture is refluxed for 1 hour. The resulting brown solution is filtered and evaporated to dryness on a rotary evaporator. The residue is solved in 2.5 mL H2O. Slow evaporation of the solvent yielded brown crystals which are filtered, washed with 2-3 mL H2O and 50 mL diethylether, and vacuum-dried. ; _chemical_name_common K(Ru(NO)Cl3(KojH-1)) _chemical_formula_moiety 'C6 H5 Cl3 N O5 Ru, K' _chemical_formula_sum 'C6 H5 Cl3 K N O5 Ru' _chemical_formula_weight 417.63 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.7023(2) _cell_length_b 9.6661(4) _cell_length_c 10.7942(5) _cell_angle_alpha 71.876(2) _cell_angle_beta 84.927(3) _cell_angle_gamma 73.877(2) _cell_volume 638.47(4) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9218 _cell_measurement_theta_min 3.134 _cell_measurement_theta_max 27.485 _cell_special_details ? _exptl_crystal_description platelet _exptl_crystal_colour brown _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.17241(14) _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 404 _exptl_absorpt_coefficient_mu 2.186 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ; Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press (New York). ; _exptl_special_details ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 -1 0 0.005000 0 1 0 0.005000 1 0 0 0.050000 -1 0 0 0.050000 0 0 1 0.030000 0 0 -1 0.010000 loop_ _diffrn_radiation_wavelength_id 0.71073 #?# _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'MONTEL, graded multilayered X-ray optics' _diffrn_radiation_collimation 0.20 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 9 _diffrn_special_details ? _diffrn_reflns_number 5473 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0410 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 27.47 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.847 _refine_diff_density_min -0.873 _refine_diff_density_rms 0.095 _reflns_number_total 2899 _reflns_number_gt 2467 _reflns_threshold_expression >2sigma(I) _reflns_special_details ? _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution ; A. Altomare, M. C. Burla, M. Camalli, G. L. Cascarano, C. Giacovazzo, A. Guagliardi, A. G. G. Moliterni, G. Polidori, R. Spagna: SIR97: a new tool for crystal structure determination and refinement; J. Appl. Crystallogr. 1999, 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)' _computing_molecular_graphics ? _computing_publication_material ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2899 _refine_ls_number_parameters 174 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0686 _refine_ls_wR_factor_gt 0.0644 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_special_details ? 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 Ru Ru 0.32156(3) 0.67978(2) 0.18606(2) 0.02385(9) Uani 1 1 d . . . K K 0.80094(10) 0.88616(7) -0.01339(7) 0.03052(16) Uani 1 1 d . . . Cl1 Cl 0.52888(12) 0.80842(9) 0.24883(8) 0.03324(18) Uani 1 1 d . . . Cl2 Cl 0.38380(12) 0.79380(9) -0.03491(7) 0.03238(18) Uani 1 1 d . . . Cl3 Cl 0.08100(12) 0.57116(8) 0.12688(9) 0.0378(2) Uani 1 1 d . . . O1 O 0.6617(4) 0.4131(3) 0.2211(3) 0.0565(8) Uani 1 1 d . . . O5 O 0.2241(3) 0.6128(2) 0.3766(2) 0.0308(5) Uani 1 1 d . . . O6 O 0.0837(3) 0.8630(2) 0.18125(19) 0.0252(4) Uani 1 1 d . . . O2 O -0.2171(3) 0.9584(2) 0.4520(2) 0.0301(5) Uani 1 1 d . . . O8 O -0.1303(4) 0.7772(3) 0.7800(2) 0.0376(6) Uani 1 1 d . . . H88 H -0.123(6) 0.694(4) 0.809(4) 0.041(12) Uiso 1 1 d . . . N1 N 0.5264(4) 0.5199(3) 0.2022(3) 0.0303(6) Uani 1 1 d . . . C5 C 0.0811(4) 0.7195(3) 0.4024(3) 0.0268(6) Uani 1 1 d . . . C6 C 0.0068(4) 0.8569(3) 0.3007(3) 0.0238(6) Uani 1 1 d . . . C7 C -0.1359(5) 0.9714(3) 0.3302(3) 0.0287(6) Uani 1 1 d . . . H7 H -0.192(5) 1.067(4) 0.275(3) 0.026(8) Uiso 1 1 d . . . C3 C -0.1556(5) 0.8277(3) 0.5472(3) 0.0291(7) Uani 1 1 d . . . C4 C -0.0107(5) 0.7079(4) 0.5278(3) 0.0316(7) Uani 1 1 d . . . H4 H 0.027(5) 0.617(4) 0.594(3) 0.026(8) Uiso 1 1 d . . . C8 C -0.2679(6) 0.8346(4) 0.6739(3) 0.0374(8) Uani 1 1 d . . . H81 H -0.337(5) 0.933(4) 0.677(3) 0.040(10) Uiso 1 1 d . . . H82 H -0.380(6) 0.776(4) 0.688(4) 0.049(11) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.02439(13) 0.01976(13) 0.02622(14) -0.00606(9) 0.00047(9) -0.00502(9) K 0.0343(4) 0.0271(3) 0.0299(4) -0.0068(3) -0.0010(3) -0.0092(3) Cl1 0.0322(4) 0.0379(4) 0.0363(4) -0.0167(3) 0.0013(3) -0.0140(3) Cl2 0.0409(4) 0.0309(4) 0.0255(4) -0.0085(3) 0.0029(3) -0.0106(3) Cl3 0.0356(4) 0.0229(4) 0.0554(5) -0.0087(4) -0.0098(4) -0.0090(3) O1 0.0371(14) 0.0390(14) 0.091(2) -0.0300(15) -0.0123(14) 0.0094(12) O5 0.0329(11) 0.0240(11) 0.0277(11) -0.0033(9) 0.0048(9) -0.0017(9) O6 0.0281(10) 0.0217(10) 0.0239(10) -0.0059(8) 0.0011(8) -0.0049(8) O2 0.0315(11) 0.0277(11) 0.0291(11) -0.0100(9) 0.0032(9) -0.0039(9) O8 0.0534(15) 0.0273(13) 0.0298(13) -0.0075(10) 0.0027(10) -0.0093(11) N1 0.0279(13) 0.0261(13) 0.0386(15) -0.0123(12) -0.0031(11) -0.0061(11) C5 0.0286(15) 0.0252(15) 0.0273(16) -0.0052(12) 0.0015(12) -0.0115(12) C6 0.0245(14) 0.0225(14) 0.0256(15) -0.0058(12) -0.0003(11) -0.0094(11) C7 0.0296(15) 0.0250(15) 0.0291(16) -0.0050(13) -0.0022(12) -0.0062(13) C3 0.0293(15) 0.0294(15) 0.0264(16) -0.0059(13) 0.0021(12) -0.0076(13) C4 0.0337(16) 0.0280(16) 0.0270(16) -0.0013(13) 0.0007(13) -0.0067(13) C8 0.0396(18) 0.0395(19) 0.0294(18) -0.0121(15) 0.0072(14) -0.0050(16) 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 Ru N1 1.732(3) . ? Ru O6 2.0174(19) . ? Ru O5 2.060(2) . ? Ru Cl2 2.3498(8) . ? Ru Cl1 2.3635(8) . ? Ru Cl3 2.3768(8) . ? Ru K 3.9043(7) 2_675 ? Ru K 3.9472(7) 1_455 ? K O8 2.703(3) 1_654 ? K O6 2.797(2) 2_675 ? K O6 2.869(2) 1_655 ? K Cl3 3.0899(10) 1_655 ? K Cl2 3.1838(11) 2_675 ? K Cl2 3.2090(10) . ? K Cl1 3.2289(10) . ? K Cl1 3.5724(10) 2_675 ? K Ru 3.9043(7) 2_675 ? K Ru 3.9472(7) 1_655 ? K K 3.9799(13) 2_775 ? K K 4.0569(13) 2_675 ? Cl1 K 3.5724(10) 2_675 ? Cl2 K 3.1838(11) 2_675 ? Cl3 K 3.0899(10) 1_455 ? O1 N1 1.146(3) . ? O5 C5 1.282(4) . ? O6 C6 1.335(3) . ? O6 K 2.797(2) 2_675 ? O6 K 2.869(2) 1_455 ? O2 C3 1.342(4) . ? O2 C7 1.359(4) . ? O8 C8 1.406(4) . ? O8 K 2.703(3) 1_456 ? O8 H88 0.76(4) . ? C5 C4 1.421(4) . ? C5 C6 1.429(4) . ? C6 C7 1.349(4) . ? C7 H7 0.92(3) . ? C3 C4 1.348(4) . ? C3 C8 1.513(4) . ? C4 H4 0.93(3) . ? C8 H81 0.95(4) . ? C8 H82 1.04(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 _geom_angle_publ_flag N1 Ru O6 175.87(11) . . ? N1 Ru O5 94.62(10) . . ? O6 Ru O5 81.57(8) . . ? N1 Ru Cl2 95.39(9) . . ? O6 Ru Cl2 88.42(6) . . ? O5 Ru Cl2 169.98(6) . . ? N1 Ru Cl1 92.40(9) . . ? O6 Ru Cl1 85.96(6) . . ? O5 Ru Cl1 89.08(6) . . ? Cl2 Ru Cl1 90.57(3) . . ? N1 Ru Cl3 93.67(9) . . ? O6 Ru Cl3 87.87(6) . . ? O5 Ru Cl3 88.83(7) . . ? Cl2 Ru Cl3 90.46(3) . . ? Cl1 Ru Cl3 173.71(3) . . ? N1 Ru K 138.95(9) . 2_675 ? O6 Ru K 43.15(6) . 2_675 ? O5 Ru K 116.66(6) . 2_675 ? Cl2 Ru K 54.60(2) . 2_675 ? Cl1 Ru K 64.08(2) . 2_675 ? Cl3 Ru K 111.78(2) . 2_675 ? N1 Ru K 139.06(9) . 1_455 ? O6 Ru K 44.19(6) . 1_455 ? O5 Ru K 104.06(6) . 1_455 ? Cl2 Ru K 67.97(2) . 1_455 ? Cl1 Ru K 123.49(2) . 1_455 ? Cl3 Ru K 51.49(2) . 1_455 ? K Ru K 60.912(17) 2_675 1_455 ? O8 K O6 85.35(7) 1_654 2_675 ? O8 K O6 129.96(7) 1_654 1_655 ? O6 K O6 90.76(6) 2_675 1_655 ? O8 K Cl3 82.68(6) 1_654 1_655 ? O6 K Cl3 128.71(5) 2_675 1_655 ? O6 K Cl3 61.66(4) 1_655 1_655 ? O8 K Cl2 136.91(6) 1_654 2_675 ? O6 K Cl2 61.02(5) 2_675 2_675 ? O6 K Cl2 79.89(4) 1_655 2_675 ? Cl3 K Cl2 138.88(3) 1_655 2_675 ? O8 K Cl2 75.92(6) 1_654 . ? O6 K Cl2 125.57(5) 2_675 . ? O6 K Cl2 139.57(5) 1_655 . ? Cl3 K Cl2 99.26(3) 1_655 . ? Cl2 K Cl2 101.22(3) 2_675 . ? O8 K Cl1 132.14(6) 1_654 . ? O6 K Cl1 137.95(5) 2_675 . ? O6 K Cl1 78.64(4) 1_655 . ? Cl3 K Cl1 81.40(3) 1_655 . ? Cl2 K Cl1 77.02(2) 2_675 . ? Cl2 K Cl1 62.70(2) . . ? O8 K Cl1 79.97(6) 1_654 2_675 ? O6 K Cl1 54.52(4) 2_675 2_675 ? O6 K Cl1 134.85(5) 1_655 2_675 ? Cl3 K Cl1 162.01(3) 1_655 2_675 ? Cl2 K Cl1 59.10(2) 2_675 2_675 ? Cl2 K Cl1 71.92(2) . 2_675 ? Cl1 K Cl1 106.96(2) . 2_675 ? O8 K Ru 101.35(5) 1_654 2_675 ? O6 K Ru 29.56(4) 2_675 2_675 ? O6 K Ru 98.97(4) 1_655 2_675 ? Cl3 K Ru 155.02(3) 1_655 2_675 ? Cl2 K Ru 36.986(15) 2_675 2_675 ? Cl2 K Ru 105.65(2) . 2_675 ? Cl1 K Ru 111.69(2) . 2_675 ? Cl1 K Ru 36.516(14) 2_675 2_675 ? O8 K Ru 102.39(6) 1_654 1_655 ? O6 K Ru 99.29(4) 2_675 1_655 ? O6 K Ru 29.35(4) 1_655 1_655 ? Cl3 K Ru 37.010(16) 1_655 1_655 ? Cl2 K Ru 108.62(2) 2_675 1_655 ? Cl2 K Ru 134.31(2) . 1_655 ? Cl1 K Ru 91.00(2) . 1_655 ? Cl1 K Ru 153.68(2) 2_675 1_655 ? Ru K Ru 119.088(17) 2_675 1_655 ? O8 K K 113.95(6) 1_654 2_775 ? O6 K K 46.12(4) 2_675 2_775 ? O6 K K 44.64(4) 1_655 2_775 ? Cl3 K K 95.58(3) 1_655 2_775 ? Cl2 K K 62.16(2) 2_675 2_775 ? Cl2 K K 163.22(3) . 2_775 ? Cl1 K K 112.32(3) . 2_775 ? Cl1 K K 95.77(3) 2_675 2_775 ? Ru K K 60.076(17) 2_675 2_775 ? Ru K K 59.012(17) 1_655 2_775 ? O8 K K 112.38(6) 1_654 2_675 ? O6 K K 94.58(5) 2_675 2_675 ? O6 K K 117.67(5) 1_655 2_675 ? Cl3 K K 135.93(3) 1_655 2_675 ? Cl2 K K 50.89(2) 2_675 2_675 ? Cl2 K K 50.33(2) . 2_675 ? Cl1 K K 57.38(2) . 2_675 ? Cl1 K K 49.578(19) 2_675 2_675 ? Ru K K 65.574(17) 2_675 2_675 ? Ru K K 143.43(3) 1_655 2_675 ? K K K 113.01(3) 2_775 2_675 ? Ru Cl1 K 99.77(3) . . ? Ru Cl1 K 79.41(2) . 2_675 ? K Cl1 K 73.04(2) . 2_675 ? Ru Cl2 K 88.41(3) . 2_675 ? Ru Cl2 K 100.63(3) . . ? K Cl2 K 78.78(3) 2_675 . ? Ru Cl3 K 91.50(3) . 1_455 ? C5 O5 Ru 110.65(17) . . ? C6 O6 Ru 110.76(17) . . ? C6 O6 K 123.48(17) . 2_675 ? Ru O6 K 107.29(8) . 2_675 ? C6 O6 K 116.98(16) . 1_455 ? Ru O6 K 106.46(8) . 1_455 ? K O6 K 89.24(6) 2_675 1_455 ? C3 O2 C7 119.7(2) . . ? C8 O8 K 121.9(2) . 1_456 ? C8 O8 H88 108(3) . . ? K O8 H88 105(3) 1_456 . ? O1 N1 Ru 175.7(3) . . ? O5 C5 C4 123.3(3) . . ? O5 C5 C6 119.0(3) . . ? C4 C5 C6 117.7(3) . . ? O6 C6 C7 124.1(3) . . ? O6 C6 C5 117.3(3) . . ? C7 C6 C5 118.6(3) . . ? C6 C7 O2 122.3(3) . . ? C6 C7 H7 127(2) . . ? O2 C7 H7 111(2) . . ? O2 C3 C4 122.3(3) . . ? O2 C3 C8 111.6(3) . . ? C4 C3 C8 126.1(3) . . ? C3 C4 C5 119.3(3) . . ? C3 C4 H4 122(2) . . ? C5 C4 H4 119(2) . . ? O8 C8 C3 111.8(3) . . ? O8 C8 H81 104(2) . . ? C3 C8 H81 115(2) . . ? O8 C8 H82 111(2) . . ? C3 C8 H82 109(2) . . ? H81 C8 H82 107(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 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 C5 C6 O6 3.7(4) . . . . ? O6 C6 C7 O2 177.0(3) . . . . ? O2 C3 C8 O8 -133.0(3) . . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O8 H88 Cl3 0.76(4) 2.38(4) 3.129(3) 173(4) 2_566 ? _geom_special_details ;Puckering parameters (\%A, \%) according to D. Cremer, J. A. Pople, J. Am. Chem. Soc. 1975, 97, 1354--1358 Ru O5 C5 C6 O6 Q2 = 0.098(2) \f2 = 344.8(17) O2 C3 C4 C5 C6 C7 No C & P - Puckering Analysis since = 2.2 < 5.0 Deg ; data_4 _database_code_depnum_ccdc_archive 'CCDC 685120' #:---------------------------------------------------------------------------- #:---------------------------CRYSTAL DATA------------------------------------- #:---------------------------------------------------------------------------- _audit_author_name 'Mayer, P.' _audit_block_code Ru_NO_Cl_Cl_MeImDiacH-2_K_0.5(H2O)_kn189_Zangl _audit_creation_method 'form98_non/compatible with shelxl97-2' _audit_creation_date 04-May-06 _chemical_name_systematic ? _chemical_compound_source ; K2[Ru(NO)Cl5] (523 mg, 1.35 mmol) is suspended in 100 mL Ethanol/H2O (3/1), then methyliminodiacetic acid (199 mg, 1.35 mmol) is solved in 5 mL H2O and added dropwise to the suspension. The pH value of the suspension is adjusted to 5 with a concentrated solution of KOH in H2O. Then the mixture is refluxed for 6 hours and the resulting brown solution is stored in a refrigerator. Within 2 weeks brown crystals are obtained which are filtered, washed with 40 mL Ethanol/H2O (3/1) and 100 mL diethylether, and vacuum-dried. ; _chemical_name_common 'K(Ru(NO)Cl2(MeImDiacH-2)) 0.5(H2O)' _chemical_formula_moiety 'C5 H7 Cl2 N2 O5 Ru, K, 0.5(H2 O)' _chemical_formula_sum 'C5 H8 Cl2 K N2 O5.50 Ru' _chemical_formula_weight 395.20 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.2438(5) _cell_length_b 6.43210(10) _cell_length_c 13.2528(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.9859(9) _cell_angle_gamma 90.00 _cell_volume 2355.11(7) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 4031 _cell_measurement_theta_min 3.134 _cell_measurement_theta_max 30.999 _cell_special_details ? _exptl_crystal_description platelet _exptl_crystal_colour orange _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.22922(7) _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1544 _exptl_absorpt_coefficient_mu 2.149 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ; Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press (New York). ; _exptl_special_details ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.010000 -1 0 0 0.025000 0 1 0 0.070000 0 -1 0 0.110000 0 0 1 0.015000 0 0 -1 0.035000 loop_ _diffrn_radiation_wavelength_id 0.71073 #?# _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'MONTEL, graded multilayered X-ray optics' _diffrn_radiation_collimation 0.20 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 9 _diffrn_special_details ? _diffrn_reflns_number 7185 _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_sigmaI/netI 0.0367 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 31.12 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 31.12 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.768 _refine_diff_density_min -0.809 _refine_diff_density_rms 0.106 _reflns_number_total 3764 _reflns_number_gt 3151 _reflns_threshold_expression >2sigma(I) _reflns_special_details ? _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution ; A. Altomare, M. C. Burla, M. Camalli, G. L. Cascarano, C. Giacovazzo, A. Guagliardi, A. G. G. Moliterni, G. Polidori, R. Spagna: SIR97: a new tool for crystal structure determination and refinement; J. Appl. Crystallogr. 1999, 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)' _computing_molecular_graphics ? _computing_publication_material ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _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 ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3764 _refine_ls_number_parameters 156 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0365 _refine_ls_R_factor_gt 0.0265 _refine_ls_wR_factor_ref 0.0670 _refine_ls_wR_factor_gt 0.0630 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_special_details ; C-bonded H: constr, one common U for all hydrogen atoms O-bonded H (H2O): refall, no DFIX ; 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 Ru Ru 0.144353(5) 0.80174(2) 0.047314(11) 0.01660(6) Uani 1 1 d . . . K K 0.029310(16) 0.59516(7) -0.10721(3) 0.02416(10) Uani 1 1 d . . . Cl1 Cl 0.200585(18) 0.59225(8) 0.15598(5) 0.03242(13) Uani 1 1 d . . . Cl2 Cl 0.13974(2) 0.55596(9) -0.08673(4) 0.03532(14) Uani 1 1 d . . . O1 O 0.22013(7) 1.0509(3) -0.00589(16) 0.0583(6) Uani 1 1 d . . . O11 O 0.09037(5) 0.6435(2) 0.09262(10) 0.0178(3) Uani 1 1 d . . . O12 O 0.04939(5) 0.6079(2) 0.21749(11) 0.0254(3) Uani 1 1 d . . . O51 O 0.08645(5) 0.9662(2) -0.03427(10) 0.0237(3) Uani 1 1 d . . . O52 O 0.03308(6) 1.2075(2) -0.01342(13) 0.0318(4) Uani 1 1 d . . . O91 O 0.0000 0.9510(5) -0.2500 0.0507(8) Uani 1 2 d S . . H911 H 0.0072(13) 1.016(5) -0.204(2) 0.054(11) Uiso 1 1 d . . . N1 N 0.18964(7) 0.9512(3) 0.01204(14) 0.0285(4) Uani 1 1 d . . . N3 N 0.13525(5) 0.9925(2) 0.16993(11) 0.0164(3) Uani 1 1 d . . . C1 C 0.08089(7) 0.6923(3) 0.18134(14) 0.0174(4) Uani 1 1 d . . . C2 C 0.11319(7) 0.8582(3) 0.23970(14) 0.0210(4) Uani 1 1 d . . . H21 H 0.0940 0.9460 0.2778 0.034(3) Uiso 1 1 calc R . . H22 H 0.1393 0.7913 0.2908 0.034(3) Uiso 1 1 calc R . . C4 C 0.10210(8) 1.1625(3) 0.12339(16) 0.0238(4) Uani 1 1 d . . . H41 H 0.1217 1.2868 0.1154 0.034(3) Uiso 1 1 calc R . . H42 H 0.0809 1.1991 0.1715 0.034(3) Uiso 1 1 calc R . . C5 C 0.07046(7) 1.1091(3) 0.01890(15) 0.0216(4) Uani 1 1 d . . . C6 C 0.18119(7) 1.0823(3) 0.23108(16) 0.0246(4) Uani 1 1 d . . . H61 H 0.1739 1.1678 0.2872 0.034(3) Uiso 1 1 calc R . . H62 H 0.1966 1.1686 0.1861 0.034(3) Uiso 1 1 calc R . . H63 H 0.2032 0.9695 0.2601 0.034(3) Uiso 1 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 Ru 0.01544(9) 0.01642(9) 0.01874(9) -0.00285(5) 0.00534(6) -0.00231(5) K 0.0225(2) 0.0268(2) 0.0220(2) -0.00231(17) 0.00193(16) -0.00161(17) Cl1 0.0206(2) 0.0244(3) 0.0496(3) 0.0032(2) 0.0012(2) 0.0057(2) Cl2 0.0338(3) 0.0394(3) 0.0367(3) -0.0213(3) 0.0165(2) -0.0089(2) O1 0.0557(12) 0.0666(13) 0.0635(13) -0.0160(11) 0.0378(11) -0.0354(11) O11 0.0176(6) 0.0169(6) 0.0190(6) -0.0015(5) 0.0041(5) -0.0031(5) O12 0.0201(7) 0.0324(8) 0.0241(7) 0.0045(6) 0.0056(6) -0.0071(6) O51 0.0249(7) 0.0257(7) 0.0183(6) 0.0028(6) -0.0007(5) -0.0013(6) O52 0.0229(8) 0.0267(8) 0.0417(9) 0.0111(7) -0.0025(7) 0.0031(6) O91 0.0340(15) 0.0278(15) 0.091(3) 0.000 0.0133(17) 0.000 N1 0.0301(9) 0.0314(10) 0.0271(9) -0.0065(8) 0.0131(8) -0.0090(8) N3 0.0169(7) 0.0150(7) 0.0166(7) -0.0014(6) 0.0019(6) -0.0004(6) C1 0.0148(8) 0.0171(9) 0.0189(9) 0.0035(7) 0.0006(7) 0.0011(7) C2 0.0233(10) 0.0247(10) 0.0154(9) 0.0003(8) 0.0052(7) -0.0033(8) C4 0.0254(10) 0.0164(9) 0.0277(10) -0.0002(8) 0.0012(8) 0.0044(8) C5 0.0189(9) 0.0195(10) 0.0254(10) 0.0092(8) 0.0021(8) -0.0030(8) C6 0.0229(10) 0.0231(10) 0.0255(10) -0.0034(8) 0.0000(8) -0.0060(8) 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 Ru N1 1.7399(18) . ? Ru O11 2.0252(13) . ? Ru O51 2.0561(14) . ? Ru N3 2.0943(15) . ? Ru Cl1 2.3371(5) . ? Ru Cl2 2.3613(5) . ? Ru K 3.7085(5) . ? K O12 2.7266(15) 5_565 ? K O52 2.7785(15) 1_545 ? K O12 2.8236(14) 6_565 ? K O11 2.8614(13) . ? K O52 2.9057(17) 5_575 ? K O51 2.9302(14) . ? K O91 2.975(2) . ? K Cl2 3.0844(7) . ? K K 3.7774(9) 5_565 ? K K 3.8030(9) 2_554 ? K H911 3.00(3) . ? O1 N1 1.138(2) . ? O11 C1 1.297(2) . ? O12 C1 1.221(2) . ? O12 K 2.7266(15) 5_565 ? O12 K 2.8236(14) 6_566 ? O51 C5 1.296(2) . ? O52 C5 1.229(2) . ? O52 K 2.7785(15) 1_565 ? O52 K 2.9057(17) 5_575 ? O91 K 2.975(2) 2_554 ? O91 H911 0.73(3) . ? N3 C4 1.488(2) . ? N3 C2 1.493(2) . ? N3 C6 1.496(2) . ? C1 C2 1.509(3) . ? C2 H21 0.9900 . ? C2 H22 0.9900 . ? C4 C5 1.523(3) . ? C4 H41 0.9900 . ? C4 H42 0.9900 . ? C6 H61 0.9800 . ? C6 H62 0.9800 . ? C6 H63 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ru O11 176.46(7) . . ? N1 Ru O51 97.08(8) . . ? O11 Ru O51 81.31(5) . . ? N1 Ru N3 95.75(7) . . ? O11 Ru N3 80.97(6) . . ? O51 Ru N3 83.93(6) . . ? N1 Ru Cl1 92.34(7) . . ? O11 Ru Cl1 89.12(4) . . ? O51 Ru Cl1 170.10(4) . . ? N3 Ru Cl1 92.11(4) . . ? N1 Ru Cl2 95.55(6) . . ? O11 Ru Cl2 87.67(4) . . ? O51 Ru Cl2 92.02(4) . . ? N3 Ru Cl2 168.38(4) . . ? Cl1 Ru Cl2 90.10(2) . . ? N1 Ru K 131.17(6) . . ? O11 Ru K 49.94(4) . . ? O51 Ru K 51.97(4) . . ? N3 Ru K 113.81(4) . . ? Cl1 Ru K 122.618(16) . . ? Cl2 Ru K 55.914(16) . . ? O12 K O52 76.17(5) 5_565 1_545 ? O12 K O12 67.54(5) 5_565 6_565 ? O52 K O12 87.55(5) 1_545 6_565 ? O12 K O11 144.66(4) 5_565 . ? O52 K O11 73.96(4) 1_545 . ? O12 K O11 128.78(4) 6_565 . ? O12 K O52 89.09(5) 5_565 5_575 ? O52 K O52 96.74(4) 1_545 5_575 ? O12 K O52 154.59(5) 6_565 5_575 ? O11 K O52 76.18(4) . 5_575 ? O12 K O51 154.01(4) 5_565 . ? O52 K O51 128.03(4) 1_545 . ? O12 K O51 117.21(4) 6_565 . ? O11 K O51 54.64(4) . . ? O52 K O51 79.52(4) 5_575 . ? O12 K O91 86.53(4) 5_565 . ? O52 K O91 162.67(5) 1_545 . ? O12 K O91 84.80(4) 6_565 . ? O11 K O91 122.66(5) . . ? O52 K O91 83.88(4) 5_575 . ? O51 K O91 69.20(4) . . ? O12 K Cl2 134.82(4) 5_565 . ? O52 K Cl2 86.74(4) 1_545 . ? O12 K Cl2 70.27(3) 6_565 . ? O11 K Cl2 61.54(3) . . ? O52 K Cl2 134.83(4) 5_575 . ? O51 K Cl2 63.89(3) . . ? O91 K Cl2 105.16(2) . . ? O12 K Ru 172.27(4) 5_565 . ? O52 K Ru 97.28(3) 1_545 . ? O12 K Ru 108.51(3) 6_565 . ? O11 K Ru 32.80(3) . . ? O52 K Ru 95.83(3) 5_575 . ? O51 K Ru 33.55(3) . . ? O91 K Ru 99.89(3) . . ? Cl2 K Ru 39.349(11) . . ? O12 K K 79.17(3) 5_565 5_565 ? O52 K K 49.81(4) 1_545 5_565 ? O12 K K 131.55(4) 6_565 5_565 ? O11 K K 67.23(3) . 5_565 ? O52 K K 46.93(3) 5_575 5_565 ? O51 K K 108.25(3) . 5_565 ? O91 K K 128.33(2) . 5_565 ? Cl2 K K 120.03(2) . 5_565 ? Ru K K 99.866(16) . 5_565 ? O12 K K 47.82(3) 5_565 2_554 ? O52 K K 114.43(4) 1_545 2_554 ? O12 K K 45.69(3) 6_565 2_554 ? O11 K K 167.22(3) . 2_554 ? O52 K K 111.05(4) 5_575 2_554 ? O51 K K 115.11(3) . 2_554 ? O91 K K 50.28(4) . 2_554 ? Cl2 K K 108.11(2) . 2_554 ? Ru K K 134.425(16) . 2_554 ? K K K 125.48(2) 5_565 2_554 ? O12 K H911 97.4(6) 5_565 . ? O52 K H911 170.0(7) 1_545 . ? O12 K H911 97.1(6) 6_565 . ? O11 K H911 109.3(6) . . ? O52 K H911 75.3(6) 5_575 . ? O51 K H911 57.3(6) . . ? O91 K H911 14.0(5) . . ? Cl2 K H911 103.1(7) . . ? Ru K H911 89.7(6) . . ? K K H911 122.0(7) 5_565 . ? K K H911 64.2(6) 2_554 . ? Ru Cl2 K 84.737(18) . . ? C1 O11 Ru 117.20(12) . . ? C1 O11 K 131.83(11) . . ? Ru O11 K 97.26(5) . . ? C1 O12 K 125.56(12) . 5_565 ? C1 O12 K 144.61(13) . 6_566 ? K O12 K 86.48(4) 5_565 6_566 ? C5 O51 Ru 114.09(12) . . ? C5 O51 K 121.81(12) . . ? Ru O51 K 94.47(5) . . ? C5 O52 K 124.63(13) . 1_565 ? C5 O52 K 127.47(14) . 5_575 ? K O52 K 83.26(4) 1_565 5_575 ? K O91 K 79.45(7) 2_554 . ? K O91 H911 164(3) 2_554 . ? K O91 H911 85(3) . . ? O1 N1 Ru 176.55(18) . . ? C4 N3 C2 111.98(15) . . ? C4 N3 C6 109.95(15) . . ? C2 N3 C6 108.34(14) . . ? C4 N3 Ru 106.08(11) . . ? C2 N3 Ru 106.01(11) . . ? C6 N3 Ru 114.47(12) . . ? O12 C1 O11 123.52(18) . . ? O12 C1 C2 121.68(17) . . ? O11 C1 C2 114.77(15) . . ? N3 C2 C1 112.18(15) . . ? N3 C2 H21 109.2 . . ? C1 C2 H21 109.2 . . ? N3 C2 H22 109.2 . . ? C1 C2 H22 109.2 . . ? H21 C2 H22 107.9 . . ? N3 C4 C5 114.29(16) . . ? N3 C4 H41 108.7 . . ? C5 C4 H41 108.7 . . ? N3 C4 H42 108.7 . . ? C5 C4 H42 108.7 . . ? H41 C4 H42 107.6 . . ? O52 C5 O51 123.17(19) . . ? O52 C5 C4 120.02(19) . . ? O51 C5 C4 116.70(16) . . ? N3 C6 H61 109.5 . . ? N3 C6 H62 109.5 . . ? H61 C6 H62 109.5 . . ? N3 C6 H63 109.5 . . ? H61 C6 H63 109.5 . . ? H62 C6 H63 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag ? ? ? ? ? ? ? ? ? _geom_special_details ;Puckering parameters (\%A, \%) according to D. Cremer, J. A. Pople, J. Am. Chem. Soc. 1975, 97, 1354--1358 Ru O11 C1 C2 N3 Q2 = 0.3302(15) \f2 = 324.8(3) Ru O51 C5 C4 N3 Q2 = 0.2161(18) \f2 = 121.3(4) ; data_5 _database_code_depnum_ccdc_archive 'CCDC 685121' #:---------------------------------------------------------------------------- #:---------------------------CRYSTAL DATA------------------------------------- #:---------------------------------------------------------------------------- _audit_author_name 'Mayer, P.' _audit_block_code Ru_NO_Cl_Cl_ThiodiglyH-2_K_H2O_kn144_Zangl _audit_creation_method 'form98_non/compatible with shelxl97-2' _audit_creation_date 28-Mar-07 _chemical_name_systematic ? _chemical_compound_source ; K2[Ru(NO)Cl5] (500 mg, 1.29 mmol) is suspended in 200 mL Ethanol/H2O (3/1), then a solution of thiodiglycolic acid (194 mg, 1.29 mmol) and KOH (145 mg, 2.58 mmol) in 7 mL H2O is added dropwise. The mixture is refluxed for 1 hour, filtered and evaporated to dryness an a rotary evaporator. The residue is solved in 2.5 mL H2O. Slow evaporation of the solvent yields brown crystals which are filtered, washed with 20 mL Ethanol/H2O (3/1) and 100 mL diethylether, and vacuum-dried. ; _chemical_name_common 'K(Ru(NO)Cl2(ThiodiglyH-2)) H2O' _chemical_formula_moiety 'C4 H4 Cl2 N O5 Ru S, K, H2 O' _chemical_formula_sum 'C4 H6 Cl2 K N O6 Ru S' _chemical_formula_weight 407.23 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c a 21' _symmetry_Int_Tables_number 29 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 13.2788(2) _cell_length_b 7.11970(10) _cell_length_c 24.9008(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2354.15(7) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 23628 _cell_measurement_theta_min 3.134 _cell_measurement_theta_max 27.485 _cell_special_details ? _exptl_crystal_description platelet _exptl_crystal_colour brown _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.29802(7) _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 2.325 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ; Sheldrick, G.M. SADABS. Version 2. Multi-Scan Absorption Correction Program. University of G\"ottingen, Germany, 2001. spherical correction included with mu*r = 0.060, leads to Tmin/Tmax = 0.0910 ; _exptl_special_details ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 1 0.020000 0 0 -1 0.020000 0 1 0 0.010000 0 -1 0 0.010000 1 0 0 0.050000 -1 0 0 0.040000 loop_ _diffrn_radiation_wavelength_id 0.71073 #?# _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'MONTEL, graded multilayered X-ray optics' _diffrn_radiation_collimation 0.20 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 9 _diffrn_special_details ? _diffrn_reflns_number 24872 _diffrn_reflns_av_R_equivalents 0.0392 _diffrn_reflns_av_sigmaI/netI 0.0383 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.459 _refine_diff_density_min -0.532 _refine_diff_density_rms 0.085 _reflns_number_total 5300 _reflns_number_gt 4702 _reflns_threshold_expression >2sigma(I) _reflns_special_details ? _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution ; A. Altomare, M. C. Burla, M. Camalli, G. L. Cascarano, C. Giacovazzo, A. Guagliardi, A. G. G. Moliterni, G. Polidori, R. Spagna: SIR97: a new tool for crystal structure determination and refinement; J. Appl. Crystallogr. 1999, 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)' _computing_molecular_graphics ? _computing_publication_material ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _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 -0.02(2) _refine_ls_number_reflns 5300 _refine_ls_number_parameters 306 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0326 _refine_ls_R_factor_gt 0.0248 _refine_ls_wR_factor_ref 0.0502 _refine_ls_wR_factor_gt 0.0478 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_special_details ; C-bonded H: constr, one common U for all hydrogen atoms O-bonded H (H2O): refall, 1 common O-H, which refined to 0.71934 \%A, H...H fixed to the 1.57fold of O-H (forcing H-O-H to 105\%) 1 of 4 H (H921) riding with U(H)=1.2*U(O) ; 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 -0.722711(19) -0.33551(4) 0.189591(10) 0.01751(7) Uani 1 1 d . . . Ru2 Ru -1.06750(2) -0.84063(4) -0.102467(10) 0.01774(7) Uani 1 1 d . . . K1 K -0.79221(7) -0.61426(13) 0.04868(4) 0.0370(2) Uani 1 1 d . . . K2 K -1.49569(7) -0.88126(12) 0.03792(4) 0.0349(2) Uani 1 1 d . . . Cl1 Cl -0.86575(7) -0.32381(14) 0.13210(4) 0.0300(2) Uani 1 1 d . . . Cl2 Cl -0.81044(7) -0.48190(13) 0.26165(4) 0.0255(2) Uani 1 1 d . . . Cl3 Cl -0.92437(7) -0.82071(14) -0.04502(4) 0.0282(2) Uani 1 1 d . . . Cl4 Cl -0.97754(6) -0.97873(14) -0.17512(4) 0.0268(2) Uani 1 1 d . . . S3 S -0.57331(7) -0.37849(14) 0.23657(4) 0.0214(2) Uani 1 1 d . . . S8 S -1.21748(6) -0.88966(14) -0.14863(4) 0.0206(2) Uani 1 1 d . . . O1 O -0.7720(2) 0.0324(4) 0.23002(12) 0.0412(7) Uani 1 1 d . . . O2 O -1.0189(2) -0.4756(4) -0.14442(11) 0.0339(6) Uani 1 1 d . . . O11 O -0.69792(19) -0.5945(3) 0.16001(10) 0.0226(6) Uani 1 1 d . . . O12 O -0.6051(2) -0.8536(4) 0.15719(12) 0.0336(7) Uani 1 1 d . . . O51 O -0.63455(18) -0.2597(3) 0.12663(9) 0.0225(6) Uani 1 1 d . . . O52 O -0.4812(2) -0.2180(4) 0.09407(11) 0.0363(7) Uani 1 1 d . . . O61 O -1.08871(19) -1.1018(3) -0.07326(10) 0.0224(6) Uani 1 1 d . . . O62 O -1.1819(2) -1.3596(4) -0.06796(12) 0.0346(7) Uani 1 1 d . . . O91 O -0.7093(3) -0.9513(6) 0.05814(17) 0.0478(9) Uani 1 1 d D . . H911 H -0.695(4) -0.949(8) 0.0856(11) 0.07(2) Uiso 1 1 d D . . H912 H -0.719(4) -1.048(4) 0.052(2) 0.08(2) Uiso 1 1 d D . . O92 O -1.5764(3) -0.5415(5) 0.03043(16) 0.0493(9) Uani 1 1 d D . . H921 H -1.602(4) -0.536(7) 0.0053(13) 0.059 Uiso 1 1 d D . . H922 H -1.579(4) -0.449(5) 0.042(2) 0.08(3) Uiso 1 1 d D . . O101 O -1.15584(19) -0.7676(4) -0.03914(9) 0.0233(6) Uani 1 1 d . . . O102 O -1.3078(2) -0.7256(4) -0.00609(11) 0.0345(7) Uani 1 1 d . . . N1 N -0.7491(2) -0.1116(5) 0.21386(13) 0.0230(7) Uani 1 1 d . . . N2 N -1.0431(2) -0.6172(4) -0.12715(12) 0.0214(7) Uani 1 1 d . . . C1 C -0.6233(3) -0.6992(5) 0.17651(15) 0.0248(10) Uani 1 1 d . . . C2 C -0.5600(3) -0.6258(5) 0.22287(18) 0.0242(9) Uani 1 1 d . . . H21 H -0.4883 -0.6522 0.2150 0.038(4) Uiso 1 1 calc R . . H22 H -0.5782 -0.6965 0.2557 0.038(4) Uiso 1 1 calc R . . C4 C -0.4926(3) -0.2640(5) 0.18787(17) 0.0252(8) Uani 1 1 d . . . H41 H -0.4764 -0.1364 0.2011 0.038(4) Uiso 1 1 calc R . . H42 H -0.4286 -0.3350 0.1855 0.038(4) Uiso 1 1 calc R . . C5 C -0.5367(3) -0.2477(5) 0.13253(16) 0.0250(9) Uani 1 1 d . . . C6 C -1.1637(3) -1.2067(5) -0.08806(14) 0.0217(8) Uani 1 1 d . . . C7 C -1.2287(3) -1.1390(5) -0.13348(18) 0.0239(9) Uani 1 1 d . . . H71 H -1.2999 -1.1666 -0.1247 0.038(4) Uiso 1 1 calc R . . H72 H -1.2113 -1.2113 -0.1661 0.038(4) Uiso 1 1 calc R . . C9 C -1.2977(3) -0.7749(5) -0.10008(17) 0.0278(8) Uani 1 1 d . . . H91 H -1.3147 -0.6481 -0.1136 0.038(4) Uiso 1 1 calc R . . H92 H -1.3613 -0.8468 -0.0972 0.038(4) Uiso 1 1 calc R . . C10 C -1.2521(3) -0.7553(5) -0.04415(15) 0.0233(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02131(15) 0.01488(15) 0.01634(14) -0.00015(15) -0.00018(11) 0.00125(11) Ru2 0.02134(15) 0.01495(15) 0.01692(14) 0.00094(15) 0.00048(11) -0.00078(11) K1 0.0473(6) 0.0272(5) 0.0366(5) -0.0009(4) 0.0028(4) 0.0040(4) K2 0.0437(5) 0.0264(5) 0.0345(5) -0.0006(4) 0.0039(4) 0.0001(4) Cl1 0.0278(5) 0.0362(6) 0.0260(5) 0.0009(4) -0.0061(4) 0.0033(4) Cl2 0.0289(5) 0.0255(5) 0.0221(5) 0.0029(4) 0.0028(3) -0.0032(4) Cl3 0.0259(5) 0.0351(6) 0.0235(5) -0.0010(4) -0.0032(4) -0.0011(4) Cl4 0.0305(6) 0.0279(5) 0.0221(5) -0.0017(4) 0.0033(3) 0.0040(4) S3 0.0247(5) 0.0195(5) 0.0199(5) -0.0001(4) -0.0036(4) -0.0023(4) S8 0.0241(5) 0.0181(5) 0.0197(5) 0.0005(4) -0.0013(4) -0.0002(4) O1 0.066(2) 0.0188(16) 0.0387(17) -0.0017(14) 0.0138(15) 0.0111(15) O2 0.0463(18) 0.0216(15) 0.0339(16) 0.0075(13) 0.0099(13) -0.0072(14) O11 0.0288(13) 0.0169(14) 0.0222(14) -0.0050(11) -0.0020(11) 0.0033(11) O12 0.0369(15) 0.0161(15) 0.0477(18) -0.0088(13) -0.0046(14) 0.0022(12) O51 0.0254(15) 0.0239(15) 0.0182(13) 0.0024(12) 0.0051(10) 0.0003(12) O52 0.0360(16) 0.0345(17) 0.0383(17) 0.0113(14) 0.0142(13) 0.0065(13) O61 0.0264(14) 0.0167(14) 0.0240(14) 0.0036(12) -0.0026(11) 0.0015(11) O62 0.0393(17) 0.0183(15) 0.0460(18) 0.0104(13) 0.0005(14) -0.0029(13) O91 0.076(3) 0.029(2) 0.038(2) 0.0034(17) -0.0132(18) 0.0041(17) O92 0.075(3) 0.030(2) 0.043(2) 0.0047(18) -0.0140(17) 0.0031(17) O101 0.0290(16) 0.0207(14) 0.0203(13) -0.0032(11) 0.0003(11) -0.0010(12) O102 0.0369(16) 0.0319(17) 0.0347(16) -0.0108(13) 0.0176(13) -0.0070(13) N1 0.0298(17) 0.0176(17) 0.0215(16) 0.0034(14) 0.0048(14) 0.0012(15) N2 0.0233(16) 0.0205(18) 0.0203(16) 0.0004(14) 0.0025(13) -0.0021(14) C1 0.027(2) 0.016(2) 0.032(2) 0.0064(17) -0.0001(17) -0.0035(16) C2 0.026(2) 0.018(2) 0.029(2) 0.0048(18) -0.0061(15) 0.0014(15) C4 0.0232(19) 0.020(2) 0.032(2) 0.0018(19) 0.0025(18) -0.0019(15) C5 0.033(2) 0.013(2) 0.029(2) 0.0064(18) 0.0084(18) 0.0032(17) C6 0.025(2) 0.0174(19) 0.022(2) 0.0009(16) 0.0051(15) 0.0016(16) C7 0.032(2) 0.014(2) 0.026(2) -0.0021(17) 0.0028(16) -0.0022(15) C9 0.0264(19) 0.020(2) 0.037(2) -0.0053(19) 0.0037(18) 0.0014(16) C10 0.032(2) 0.0079(18) 0.031(2) -0.0016(16) 0.0022(19) -0.0046(17) 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 N1 1.741(3) . ? Ru1 O11 2.013(2) . ? Ru1 O51 2.030(2) . ? Ru1 S3 2.3232(9) . ? Ru1 Cl2 2.3797(9) . ? Ru1 Cl1 2.3799(9) . ? Ru2 N2 1.736(3) . ? Ru2 O61 2.016(2) . ? Ru2 O101 2.033(2) . ? Ru2 S8 2.3258(9) . ? Ru2 Cl4 2.3804(9) . ? Ru2 Cl3 2.3831(10) . ? K1 O91 2.651(4) . ? K1 O102 2.785(3) 4_545 ? K1 O92 2.948(4) 1_655 ? K1 O52 3.000(3) 4_445 ? K1 O11 3.045(3) . ? K1 Cl1 3.0895(14) . ? K1 O62 3.258(3) 4_535 ? K1 Cl3 3.2685(13) . ? K1 K2 4.3805(11) 1_655 ? K1 K2 4.4518(13) 4_545 ? K1 K2 4.5026(13) 4_535 ? K1 H911 2.87(5) . ? K2 O92 2.652(4) . ? K2 O52 2.782(3) 1_445 ? K2 O91 2.924(4) 1_455 ? K2 O102 2.942(3) . ? K2 O61 3.034(3) 4_435 ? K2 Cl3 3.1088(13) 4_435 ? K2 Cl1 3.2571(13) 4_445 ? K2 O12 3.312(3) 1_455 ? K2 K1 4.3805(11) 1_455 ? K2 K1 4.4518(13) 4_445 ? K2 K1 4.5026(13) 4_435 ? K2 H921 2.95(4) . ? Cl1 K2 3.2571(13) 4_545 ? Cl3 K2 3.1087(13) 4_535 ? S3 C2 1.802(4) . ? S3 C4 1.812(4) . ? S8 C9 1.806(4) . ? S8 C7 1.821(4) . ? O1 N1 1.142(4) . ? O2 N2 1.142(4) . ? O11 C1 1.307(4) . ? O12 C1 1.224(4) . ? O12 K2 3.312(3) 1_655 ? O51 C5 1.310(4) . ? O52 C5 1.227(4) . ? O52 K2 2.782(3) 1_665 ? O52 K1 3.000(3) 4_545 ? O61 C6 1.298(4) . ? O61 K2 3.034(3) 4_535 ? O62 C6 1.223(4) . ? O62 K1 3.258(3) 4_435 ? O91 K2 2.924(4) 1_655 ? O91 H911 0.71(2) . ? O91 H912 0.72(2) . ? O92 K1 2.948(4) 1_455 ? O92 H921 0.71(2) . ? O92 H922 0.72(2) . ? O101 C10 1.288(4) . ? O102 C10 1.220(4) . ? O102 K1 2.785(3) 4_445 ? C1 C2 1.520(5) . ? C2 H21 0.9900 . ? C2 H22 0.9900 . ? C4 C5 1.502(6) . ? C4 H41 0.9900 . ? C4 H42 0.9900 . ? C6 C7 1.502(5) . ? C7 H71 0.9900 . ? C7 H72 0.9900 . ? C9 C10 1.524(6) . ? C9 H91 0.9900 . ? C9 H92 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ru1 O11 177.59(13) . . ? N1 Ru1 O51 98.09(12) . . ? O11 Ru1 O51 82.33(10) . . ? N1 Ru1 S3 96.75(11) . . ? O11 Ru1 S3 85.64(8) . . ? O51 Ru1 S3 86.07(7) . . ? N1 Ru1 Cl2 92.35(11) . . ? O11 Ru1 Cl2 87.41(8) . . ? O51 Ru1 Cl2 168.87(7) . . ? S3 Ru1 Cl2 88.89(3) . . ? N1 Ru1 Cl1 90.93(11) . . ? O11 Ru1 Cl1 86.70(8) . . ? O51 Ru1 Cl1 89.22(7) . . ? S3 Ru1 Cl1 171.48(4) . . ? Cl2 Ru1 Cl1 94.49(3) . . ? N2 Ru2 O61 177.28(13) . . ? N2 Ru2 O101 98.50(12) . . ? O61 Ru2 O101 82.85(10) . . ? N2 Ru2 S8 97.01(10) . . ? O61 Ru2 S8 85.43(8) . . ? O101 Ru2 S8 85.85(7) . . ? N2 Ru2 Cl4 90.91(10) . . ? O61 Ru2 Cl4 87.89(8) . . ? O101 Ru2 Cl4 169.96(8) . . ? S8 Ru2 Cl4 89.55(3) . . ? N2 Ru2 Cl3 90.54(10) . . ? O61 Ru2 Cl3 87.12(8) . . ? O101 Ru2 Cl3 88.82(7) . . ? S8 Ru2 Cl3 171.32(4) . . ? Cl4 Ru2 Cl3 94.62(3) . . ? O91 K1 O102 149.41(11) . 4_545 ? O91 K1 O92 76.64(11) . 1_655 ? O102 K1 O92 81.03(9) 4_545 1_655 ? O91 K1 O52 87.34(11) . 4_445 ? O102 K1 O52 117.91(9) 4_545 4_445 ? O92 K1 O52 160.26(10) 1_655 4_445 ? O91 K1 O11 77.89(11) . . ? O102 K1 O11 115.86(9) 4_545 . ? O92 K1 O11 74.48(9) 1_655 . ? O52 K1 O11 91.10(8) 4_445 . ? O91 K1 Cl1 132.65(10) . . ? O102 K1 Cl1 74.00(7) 4_545 . ? O92 K1 Cl1 107.06(9) 1_655 . ? O52 K1 Cl1 75.44(6) 4_445 . ? O11 K1 Cl1 59.13(5) . . ? O91 K1 O62 80.84(10) . 4_535 ? O102 K1 O62 69.29(7) 4_545 4_535 ? O92 K1 O62 55.63(10) 1_655 4_535 ? O52 K1 O62 133.56(8) 4_445 4_535 ? O11 K1 O62 129.00(7) . 4_535 ? Cl1 K1 O62 141.23(6) . 4_535 ? O91 K1 Cl3 83.07(10) . . ? O102 K1 Cl3 90.07(7) 4_545 . ? O92 K1 Cl3 119.41(9) 1_655 . ? O52 K1 Cl3 68.95(6) 4_445 . ? O11 K1 Cl3 153.04(6) . . ? Cl1 K1 Cl3 127.68(4) . . ? O62 K1 Cl3 65.13(5) 4_535 . ? O91 K1 K2 40.47(9) . 1_655 ? O102 K1 K2 114.44(6) 4_545 1_655 ? O92 K1 K2 36.18(7) 1_655 1_655 ? O52 K1 K2 127.02(6) 4_445 1_655 ? O11 K1 K2 72.91(5) . 1_655 ? Cl1 K1 K2 128.00(3) . 1_655 ? O62 K1 K2 61.10(5) 4_535 1_655 ? Cl3 K1 K2 104.11(3) . 1_655 ? O91 K1 K2 167.12(10) . 4_545 ? O102 K1 K2 40.27(5) 4_545 4_545 ? O92 K1 K2 116.21(8) 1_655 4_545 ? O52 K1 K2 80.24(6) 4_445 4_545 ? O11 K1 K2 105.53(5) . 4_545 ? Cl1 K1 K2 47.01(2) . 4_545 ? O62 K1 K2 105.33(5) 4_535 4_545 ? Cl3 K1 K2 89.29(3) . 4_545 ? K2 K1 K2 152.35(3) 1_655 4_545 ? O91 K1 K2 62.12(9) . 4_535 ? O102 K1 K2 128.27(7) 4_545 4_535 ? O92 K1 K2 135.60(9) 1_655 4_535 ? O52 K1 K2 37.15(5) 4_445 4_535 ? O11 K1 K2 109.74(5) . 4_535 ? Cl1 K1 K2 112.60(3) . 4_535 ? O62 K1 K2 99.86(5) 4_535 4_535 ? Cl3 K1 K2 43.66(2) . 4_535 ? K2 K1 K2 100.928(18) 1_655 4_535 ? K2 K1 K2 105.33(2) 4_545 4_535 ? O91 K1 H911 14.1(6) . . ? O102 K1 H911 156.1(11) 4_545 . ? O92 K1 H911 75.9(11) 1_655 . ? O52 K1 H911 85.7(11) 4_445 . ? O11 K1 H911 63.9(6) . . ? Cl1 K1 H911 118.9(7) . . ? O62 K1 H911 92.0(9) 4_535 . ? Cl3 K1 H911 95.6(7) . . ? K2 K1 H911 41.6(11) 1_655 . ? K2 K1 H911 162.4(9) 4_545 . ? K2 K1 H911 68.0(10) 4_535 . ? O92 K2 O52 148.13(11) . 1_445 ? O92 K2 O91 77.04(11) . 1_455 ? O52 K2 O91 80.42(9) 1_445 1_455 ? O92 K2 O102 88.44(11) . . ? O52 K2 O102 116.95(9) 1_445 . ? O91 K2 O102 162.03(10) 1_455 . ? O92 K2 O61 78.90(10) . 4_435 ? O52 K2 O61 116.91(8) 1_445 4_435 ? O91 K2 O61 75.84(10) 1_455 4_435 ? O102 K2 O61 91.16(8) . 4_435 ? O92 K2 Cl3 134.34(10) . 4_435 ? O52 K2 Cl3 74.01(6) 1_445 4_435 ? O91 K2 Cl3 107.06(10) 1_455 4_435 ? O102 K2 Cl3 75.60(6) . 4_435 ? O61 K2 Cl3 59.38(5) 4_435 4_435 ? O92 K2 Cl1 81.71(9) . 4_445 ? O52 K2 Cl1 89.30(7) 1_445 4_445 ? O91 K2 Cl1 117.81(10) 1_455 4_445 ? O102 K2 Cl1 69.52(6) . 4_445 ? O61 K2 Cl1 152.94(6) 4_435 4_445 ? Cl3 K2 Cl1 128.53(4) 4_435 4_445 ? O92 K2 O12 80.31(11) . 1_455 ? O52 K2 O12 68.34(7) 1_445 1_455 ? O91 K2 O12 55.27(10) 1_455 1_455 ? O102 K2 O12 133.13(8) . 1_455 ? O61 K2 O12 129.95(7) 4_435 1_455 ? Cl3 K2 O12 140.34(6) 4_435 1_455 ? Cl1 K2 O12 63.89(5) 4_445 1_455 ? O92 K2 K1 41.01(9) . 1_455 ? O52 K2 K1 113.92(6) 1_445 1_455 ? O91 K2 K1 36.05(8) 1_455 1_455 ? O102 K2 K1 128.43(6) . 1_455 ? O61 K2 K1 72.97(5) 4_435 1_455 ? Cl3 K2 K1 127.64(3) 4_435 1_455 ? Cl1 K2 K1 103.75(3) 4_445 1_455 ? O12 K2 K1 61.65(5) 1_455 1_455 ? O92 K2 K1 61.75(9) . 4_445 ? O52 K2 K1 127.64(7) 1_445 4_445 ? O91 K2 K1 135.54(9) 1_455 4_445 ? O102 K2 K1 37.73(5) . 4_445 ? O61 K2 K1 109.48(5) 4_435 4_445 ? Cl3 K2 K1 113.33(3) 4_435 4_445 ? Cl1 K2 K1 43.94(2) 4_445 4_445 ? O12 K2 K1 99.50(5) 1_455 4_445 ? K1 K2 K1 101.419(18) 1_455 4_445 ? O92 K2 K1 166.95(9) . 4_435 ? O52 K2 K1 40.64(5) 1_445 4_435 ? O91 K2 K1 115.84(8) 1_455 4_435 ? O102 K2 K1 79.27(6) . 4_435 ? O61 K2 K1 105.48(5) 4_435 4_435 ? Cl3 K2 K1 46.55(2) 4_435 4_435 ? Cl1 K2 K1 89.82(3) 4_445 4_435 ? O12 K2 K1 104.91(5) 1_455 4_435 ? K1 K2 K1 151.88(2) 1_455 4_435 ? K1 K2 K1 105.33(2) 4_445 4_435 ? O92 K2 H921 13.3(6) . . ? O52 K2 H921 152.9(11) 1_445 . ? O91 K2 H921 74.1(11) 1_455 . ? O102 K2 H921 89.4(11) . . ? O61 K2 H921 65.6(6) 4_435 . ? Cl3 K2 H921 122.1(7) 4_435 . ? Cl1 K2 H921 94.5(6) 4_445 . ? O12 K2 H921 89.3(9) 1_455 . ? K1 K2 H921 39.2(11) 1_455 . ? K1 K2 H921 69.3(10) 4_445 . ? K1 K2 H921 165.6(10) 4_435 . ? Ru1 Cl1 K1 97.40(4) . . ? Ru1 Cl1 K2 150.64(4) . 4_545 ? K1 Cl1 K2 89.05(4) . 4_545 ? Ru2 Cl3 K2 96.62(4) . 4_535 ? Ru2 Cl3 K1 152.06(4) . . ? K2 Cl3 K1 89.79(4) 4_535 . ? C2 S3 C4 104.75(19) . . ? C2 S3 Ru1 96.72(13) . . ? C4 S3 Ru1 96.26(13) . . ? C9 S8 C7 104.71(19) . . ? C9 S8 Ru2 96.08(13) . . ? C7 S8 Ru2 96.54(13) . . ? C1 O11 Ru1 122.1(2) . . ? C1 O11 K1 124.9(2) . . ? Ru1 O11 K1 107.96(10) . . ? C1 O12 K2 119.5(2) . 1_655 ? C5 O51 Ru1 120.2(2) . . ? C5 O52 K2 119.9(2) . 1_665 ? C5 O52 K1 136.7(2) . 4_545 ? K2 O52 K1 102.21(8) 1_665 4_545 ? C6 O61 Ru2 122.4(2) . . ? C6 O61 K2 123.3(2) . 4_535 ? Ru2 O61 K2 107.99(10) . 4_535 ? C6 O62 K1 120.3(2) . 4_435 ? K1 O91 K2 103.48(13) . 1_655 ? K1 O91 H911 100(5) . . ? K2 O91 H911 84(5) 1_655 . ? K1 O91 H912 141(5) . . ? K2 O91 H912 107(5) 1_655 . ? H911 O91 H912 106(3) . . ? K2 O92 K1 102.81(13) . 1_455 ? K2 O92 H921 108(4) . . ? K1 O92 H921 71(5) 1_455 . ? K2 O92 H922 146(4) . . ? K1 O92 H922 93(5) 1_455 . ? H921 O92 H922 106(3) . . ? C10 O101 Ru2 121.0(2) . . ? C10 O102 K1 119.1(2) . 4_445 ? C10 O102 K2 137.5(2) . . ? K1 O102 K2 102.00(8) 4_445 . ? O1 N1 Ru1 176.1(3) . . ? O2 N2 Ru2 174.1(3) . . ? O12 C1 O11 122.6(3) . . ? O12 C1 C2 119.9(3) . . ? O11 C1 C2 117.5(3) . . ? C1 C2 S3 115.2(3) . . ? C1 C2 H21 108.5 . . ? S3 C2 H21 108.5 . . ? C1 C2 H22 108.5 . . ? S3 C2 H22 108.5 . . ? H21 C2 H22 107.5 . . ? C5 C4 S3 114.7(3) . . ? C5 C4 H41 108.6 . . ? S3 C4 H41 108.6 . . ? C5 C4 H42 108.6 . . ? S3 C4 H42 108.6 . . ? H41 C4 H42 107.6 . . ? O52 C5 O51 121.3(4) . . ? O52 C5 C4 119.6(3) . . ? O51 C5 C4 119.0(3) . . ? O62 C6 O61 123.2(3) . . ? O62 C6 C7 118.7(3) . . ? O61 C6 C7 118.0(3) . . ? C6 C7 S8 115.0(3) . . ? C6 C7 H71 108.5 . . ? S8 C7 H71 108.5 . . ? C6 C7 H72 108.5 . . ? S8 C7 H72 108.5 . . ? H71 C7 H72 107.5 . . ? C10 C9 S8 114.8(3) . . ? C10 C9 H91 108.6 . . ? S8 C9 H91 108.6 . . ? C10 C9 H92 108.6 . . ? S8 C9 H92 108.6 . . ? H91 C9 H92 107.5 . . ? O102 C10 O101 122.5(3) . . ? O102 C10 C9 119.0(4) . . ? O101 C10 C9 118.4(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O91 H911 O12 0.71(2) 2.25(3) 2.913(5) 156(6) . ? O91 H911 O51 0.71(2) 2.56(5) 2.952(4) 117(5) 1_545 ? O91 H912 O102 0.72(2) 2.47(3) 3.092(5) 146(6) 4_535 ? O92 H921 O62 0.71(2) 2.24(3) 2.909(5) 157(5) 4_435 ? O92 H921 O101 0.71(2) 2.53(4) 2.993(4) 125(5) 4_445 ? O92 H922 O52 0.72(2) 2.46(4) 3.068(5) 142(5) 1_455 ? O92 H922 O51 0.72(2) 2.60(4) 3.219(5) 144(6) 1_455 ? _geom_special_details ; Puckering parameters (\%A, \%) according to D. Cremer, J. A. Pople, J. Am. Chem. Soc. 1975, 97, 1354--1358 Ru1 S3 C2 C1 O11 Q2 = 0.202(3) \f2 = 44.5(9) Ru1 S3 C4 C5 O51 Q2 = 0.226(3) \f2 = 228.8(7) Ru2 S8 C7 C6 O61 Q2 = 0.188(3) \f2 = 50.6(9) Ru2 S8 C9 C10 O101 Q2 = 0.234(3) \f2 = 225.4(7) ;