#------------------------------------------------------------------------------ #$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100941.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_1100941 _chemical_formula_moiety 'C28 H22 N7 O Ru.3(ClO4).2(H2O) ' _chemical_formula_sum 'C28 H26 Cl3 N7 O15 Ru' _chemical_formula_weight 907.98 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' 'Cl' 'Cl' 0.1484 0.1585 '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' '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' _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2829(14) _cell_length_b 10.4319(15) _cell_length_c 18.729(3) _cell_angle_alpha 104.955(2) _cell_angle_beta 92.655(2) _cell_angle_gamma 95.718(2) _cell_volume 1738.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used '5484' _cell_measurement_theta_min '2.39' _cell_measurement_theta_max '27.82' _exptl_crystal_description 'Plate' _exptl_crystal_colour 'Deep Brown' _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.734 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 916 _exptl_absorpt_coefficient_mu 0.763 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.6833 _exptl_absorpt_correction_T_max 0.9471 _exptl_absorpt_process_details 'Bruker SADABS' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ' CCD Area Detector' _diffrn_measurement_device ' Bruker Smart APEX' _diffrn_measurement_method 'Omega Scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16270 _diffrn_reflns_av_R_equivalents 0.0428 _diffrn_reflns_av_sigmaI/netI 0.0562 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6093 _reflns_number_gt 4668 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0768P)^2^+1.4544P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6093 _refine_ls_number_parameters 488 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0771 _refine_ls_R_factor_gt 0.0544 _refine_ls_wR_factor_ref 0.1428 _refine_ls_wR_factor_gt 0.1317 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.02173(4) 0.13102(4) 0.25891(2) 0.03238(16) Uani 1 1 d . . . O1 O -0.2326(5) -0.0622(4) 0.2196(2) 0.0629(12) Uani 1 1 d . . . N1 N -0.0360(5) 0.2489(4) 0.1906(2) 0.0371(10) Uani 1 1 d . . . N2 N 0.2047(5) 0.2737(4) 0.2731(2) 0.0369(10) Uani 1 1 d . . . N5 N -0.0476(5) 0.2438(4) 0.3566(2) 0.0366(10) Uani 1 1 d . . . N4 N 0.1154(4) 0.0495(4) 0.3315(2) 0.0344(9) Uani 1 1 d . . . N3 N 0.1481(5) 0.0049(4) 0.1899(2) 0.0401(10) Uani 1 1 d . . . N6 N -0.1332(5) 0.0135(4) 0.2370(2) 0.0414(11) Uani 1 1 d . . . N7 N 0.0195(6) 0.4173(4) 0.1419(2) 0.0465(12) Uani 1 1 d . . . C1 C -0.1236(7) 0.3711(6) 0.1211(3) 0.0491(15) Uani 1 1 d . . . C2 C -0.2295(9) 0.4168(7) 0.0804(3) 0.0650(19) Uani 1 1 d . . . H2 H -0.2067 0.4882 0.0602 0.078 Uiso 1 1 calc R . . C3 C -0.3628(10) 0.3540(8) 0.0722(4) 0.074(2) Uani 1 1 d . . . H3 H -0.4341 0.3826 0.0454 0.089 Uiso 1 1 calc R . . C4 C -0.4010(8) 0.2475(8) 0.1018(4) 0.0689(19) Uani 1 1 d . . . H4 H -0.4962 0.2068 0.0947 0.083 Uiso 1 1 calc R . . C5 C -0.2977(7) 0.2014(6) 0.1421(3) 0.0554(16) Uani 1 1 d . . . H5 H -0.3220 0.1296 0.1618 0.067 Uiso 1 1 calc R . . C6 C -0.1589(6) 0.2652(5) 0.1518(3) 0.0414(13) Uani 1 1 d . . . C7 C 0.0683(6) 0.3409(5) 0.1841(3) 0.0389(12) Uani 1 1 d . . . C8 C 0.2075(6) 0.3543(5) 0.2263(3) 0.0407(13) Uani 1 1 d . . . C9 C 0.3308(7) 0.4368(7) 0.2239(4) 0.0648(18) Uani 1 1 d . . . H9 H 0.3335 0.4890 0.1905 0.078 Uiso 1 1 calc R . . C10 C 0.4501(8) 0.4420(8) 0.2711(4) 0.076(2) Uani 1 1 d . . . H10 H 0.5340 0.4977 0.2697 0.091 Uiso 1 1 calc R . . C11 C 0.4452(7) 0.3651(7) 0.3201(4) 0.0685(19) Uani 1 1 d . . . H11 H 0.5241 0.3699 0.3535 0.082 Uiso 1 1 calc R . . C12 C 0.3231(6) 0.2819(6) 0.3190(3) 0.0518(15) Uani 1 1 d . . . H12 H 0.3209 0.2279 0.3515 0.062 Uiso 1 1 calc R . . C13 C 0.1620(7) -0.0073(6) 0.1176(3) 0.0486(14) Uani 1 1 d . . . H13 H 0.1045 0.0375 0.0924 0.058 Uiso 1 1 calc R . . C14 C 0.2597(7) -0.0850(7) 0.0802(3) 0.0620(17) Uani 1 1 d . . . H14 H 0.2695 -0.0919 0.0302 0.074 Uiso 1 1 calc R . . C15 C 0.3421(8) -0.1517(7) 0.1169(4) 0.0686(19) Uani 1 1 d . . . H15 H 0.4089 -0.2043 0.0920 0.082 Uiso 1 1 calc R . . C16 C 0.3268(7) -0.1413(6) 0.1915(3) 0.0554(16) Uani 1 1 d . . . H16 H 0.3831 -0.1864 0.2170 0.067 Uiso 1 1 calc R . . C17 C 0.2280(6) -0.0639(5) 0.2269(3) 0.0412(13) Uani 1 1 d . . . C18 C 0.2066(6) -0.0412(5) 0.3065(3) 0.0402(12) Uani 1 1 d . . . C19 C 0.2744(6) -0.0974(6) 0.3566(3) 0.0497(14) Uani 1 1 d . . . H19 H 0.3366 -0.1620 0.3409 0.060 Uiso 1 1 calc R . . C20 C 0.2471(6) -0.0550(6) 0.4303(3) 0.0508(15) Uani 1 1 d . . . H20 H 0.2911 -0.0924 0.4644 0.061 Uiso 1 1 calc R . . C21 C 0.1559(6) 0.0419(6) 0.4546(3) 0.0478(14) Uani 1 1 d . . . H21 H 0.1397 0.0708 0.5045 0.057 Uiso 1 1 calc R . . C22 C 0.0892(6) 0.0950(5) 0.4027(3) 0.0362(12) Uani 1 1 d . . . C23 C -0.0032(5) 0.2040(5) 0.4172(3) 0.0372(12) Uani 1 1 d . . . C24 C -0.0407(6) 0.2676(6) 0.4867(3) 0.0447(13) Uani 1 1 d . . . H24 H -0.0079 0.2422 0.5281 0.054 Uiso 1 1 calc R . . C25 C -0.1280(6) 0.3698(6) 0.4940(3) 0.0525(15) Uani 1 1 d . . . H25 H -0.1562 0.4126 0.5404 0.063 Uiso 1 1 calc R . . C26 C -0.1727(6) 0.4074(6) 0.4322(3) 0.0524(15) Uani 1 1 d . . . H26 H -0.2317 0.4756 0.4364 0.063 Uiso 1 1 calc R . . C27 C -0.1300(6) 0.3441(5) 0.3647(3) 0.0412(13) Uani 1 1 d . . . H27 H -0.1588 0.3713 0.3233 0.049 Uiso 1 1 calc R . . C28 C 0.1016(8) 0.5280(6) 0.1199(4) 0.070(2) Uani 1 1 d . . . H28A H 0.1375 0.5975 0.1633 0.104 Uiso 1 1 calc R . . H28B H 0.0389 0.5628 0.0891 0.104 Uiso 1 1 calc R . . H28C H 0.1818 0.4955 0.0928 0.104 Uiso 1 1 calc R . . Cl1 Cl 0.79285(19) 0.79029(16) 0.02695(8) 0.0591(4) Uani 1 1 d . . . O2 O 0.8162(10) 0.9264(6) 0.0585(4) 0.141(3) Uani 1 1 d . . . O3 O 0.9134(7) 0.7318(7) 0.0431(4) 0.136(3) Uani 1 1 d . . . O4 O 0.6761(8) 0.7274(9) 0.0535(4) 0.153(3) Uani 1 1 d . . . O5 O 0.7650(6) 0.7647(5) -0.0505(3) 0.0909(17) Uani 1 1 d . . . Cl2 Cl 0.92110(17) 0.68174(15) 0.29935(8) 0.0527(4) Uani 1 1 d . . . O6 O 0.9498(7) 0.7290(5) 0.2362(3) 0.0933(17) Uani 1 1 d . . . O7 O 0.9008(6) 0.7940(5) 0.3581(2) 0.0791(14) Uani 1 1 d . . . O8 O 1.0389(6) 0.6184(5) 0.3183(3) 0.0888(16) Uani 1 1 d . . . O9 O 0.7972(6) 0.5876(5) 0.2822(3) 0.0960(17) Uani 1 1 d . . . Cl3 Cl 0.46285(18) 0.27672(17) 0.52435(10) 0.0666(5) Uani 1 1 d . . . O10 O 0.5109(7) 0.2087(7) 0.4552(3) 0.109(2) Uani 1 1 d . . . O11 O 0.3291(6) 0.3222(6) 0.5115(4) 0.109(2) Uani 1 1 d . . . O12 O 0.5699(8) 0.3739(9) 0.5612(5) 0.182(4) Uani 1 1 d . . . O13 O 0.4383(7) 0.1778(8) 0.5656(4) 0.141(3) Uani 1 1 d . . . O14 O 0.5712(7) 0.6642(6) 0.1832(4) 0.123(2) Uani 1 1 d . . . O15 O 0.6792(9) 0.0317(6) 0.3656(4) 0.141(3) 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 Ru 0.0364(3) 0.0330(2) 0.0297(2) 0.01251(16) 0.00039(16) 0.00305(17) O1 0.060(3) 0.062(3) 0.060(3) 0.017(2) -0.005(2) -0.021(2) N1 0.043(3) 0.038(2) 0.034(2) 0.0150(19) 0.0029(19) 0.007(2) N2 0.040(3) 0.038(2) 0.035(2) 0.0145(19) 0.0029(19) 0.0021(19) N5 0.040(3) 0.034(2) 0.036(2) 0.0108(18) 0.0033(19) 0.0019(19) N4 0.039(3) 0.034(2) 0.031(2) 0.0123(18) -0.0023(18) 0.0010(19) N3 0.045(3) 0.037(2) 0.039(2) 0.0118(19) 0.007(2) 0.004(2) N6 0.046(3) 0.041(3) 0.040(3) 0.016(2) 0.007(2) 0.004(2) N7 0.067(4) 0.039(3) 0.040(3) 0.020(2) 0.009(2) 0.013(2) C1 0.071(4) 0.046(3) 0.035(3) 0.012(3) 0.007(3) 0.022(3) C2 0.097(6) 0.064(4) 0.043(4) 0.020(3) 0.000(4) 0.043(4) C3 0.088(6) 0.091(6) 0.048(4) 0.013(4) -0.012(4) 0.049(5) C4 0.063(5) 0.085(5) 0.052(4) 0.002(4) -0.011(3) 0.025(4) C5 0.056(4) 0.059(4) 0.052(4) 0.014(3) -0.002(3) 0.020(3) C6 0.050(4) 0.044(3) 0.031(3) 0.008(2) -0.003(2) 0.016(3) C7 0.052(3) 0.036(3) 0.032(3) 0.012(2) 0.007(2) 0.009(2) C8 0.052(4) 0.031(3) 0.035(3) 0.004(2) 0.008(2) 0.000(2) C9 0.062(4) 0.064(4) 0.072(5) 0.030(4) 0.012(4) -0.012(3) C10 0.054(5) 0.086(5) 0.083(5) 0.028(4) -0.005(4) -0.025(4) C11 0.053(4) 0.083(5) 0.063(4) 0.021(4) -0.013(3) -0.017(4) C12 0.049(4) 0.054(4) 0.051(4) 0.017(3) -0.006(3) -0.002(3) C13 0.059(4) 0.053(3) 0.036(3) 0.014(3) 0.007(3) 0.008(3) C14 0.076(5) 0.070(4) 0.042(3) 0.011(3) 0.018(3) 0.021(4) C15 0.074(5) 0.067(4) 0.068(5) 0.011(4) 0.025(4) 0.032(4) C16 0.063(4) 0.053(4) 0.052(4) 0.011(3) 0.006(3) 0.017(3) C17 0.040(3) 0.038(3) 0.048(3) 0.015(2) 0.004(2) 0.008(2) C18 0.046(3) 0.039(3) 0.037(3) 0.013(2) 0.000(2) 0.006(3) C19 0.050(4) 0.045(3) 0.057(4) 0.018(3) -0.005(3) 0.011(3) C20 0.055(4) 0.058(4) 0.049(4) 0.030(3) -0.007(3) 0.009(3) C21 0.051(4) 0.058(4) 0.036(3) 0.021(3) -0.001(3) -0.004(3) C22 0.039(3) 0.039(3) 0.033(3) 0.016(2) 0.000(2) 0.000(2) C23 0.035(3) 0.041(3) 0.037(3) 0.014(2) 0.000(2) -0.002(2) C24 0.046(3) 0.052(3) 0.032(3) 0.006(2) 0.003(2) 0.000(3) C25 0.045(4) 0.061(4) 0.042(3) -0.003(3) 0.010(3) 0.000(3) C26 0.043(4) 0.045(3) 0.062(4) 0.000(3) 0.003(3) 0.005(3) C27 0.037(3) 0.039(3) 0.045(3) 0.007(2) -0.002(2) 0.002(2) C28 0.099(6) 0.052(4) 0.072(5) 0.039(3) 0.016(4) 0.009(4) Cl1 0.0747(12) 0.0601(10) 0.0459(9) 0.0184(7) 0.0045(8) 0.0127(8) O2 0.242(9) 0.075(4) 0.098(5) 0.005(4) -0.013(5) 0.046(5) O3 0.111(5) 0.122(5) 0.185(7) 0.066(5) -0.048(5) 0.024(4) O4 0.099(5) 0.246(10) 0.138(6) 0.104(7) 0.020(4) -0.014(6) O5 0.123(5) 0.102(4) 0.048(3) 0.016(3) 0.010(3) 0.026(4) Cl2 0.0645(10) 0.0508(8) 0.0407(8) 0.0108(6) -0.0020(7) 0.0027(7) O6 0.141(5) 0.090(4) 0.061(3) 0.036(3) 0.024(3) 0.017(3) O7 0.100(4) 0.078(3) 0.049(3) -0.003(2) 0.005(2) 0.016(3) O8 0.090(4) 0.081(4) 0.094(4) 0.018(3) -0.014(3) 0.028(3) O9 0.083(4) 0.079(4) 0.117(5) 0.027(3) -0.015(3) -0.021(3) Cl3 0.0558(11) 0.0658(10) 0.0722(11) 0.0062(9) 0.0048(8) 0.0099(8) O10 0.102(4) 0.130(5) 0.086(4) 0.002(4) 0.022(3) 0.041(4) O11 0.090(4) 0.091(4) 0.159(6) 0.039(4) 0.022(4) 0.047(3) O12 0.114(6) 0.167(7) 0.183(8) -0.069(6) 0.024(5) -0.063(5) O13 0.116(5) 0.198(8) 0.155(7) 0.124(6) 0.010(5) 0.032(5) O14 0.099(5) 0.103(5) 0.186(7) 0.070(5) 0.008(4) 0.017(4) O15 0.195(7) 0.095(4) 0.119(5) 0.004(4) 0.076(5) -0.017(5) _cod_database_code 1100941