#------------------------------------------------------------------------------ #$Date: 2009-11-16 01:43:51 +0000 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003158.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_2003158 _journal_name_full 'Acta Crystallographica, Section B' _journal_volume 54 _journal_year 1998 _journal_page_first 613 _journal_page_last 625 _chemical_formula_moiety 'Rb1,N6 H18 Ru1,2(ClO4),2Cl' _chemical_formula_sum 'Cl4 H18 N6 O8 Rb1 Ru1' _chemical_formula_iupac 'Rb[Ru(N H3)6],2(Cl O4),2Cl' _chemical_formula_weight 558.54 _symmetry_cell_setting Trigonal _space_group_IT_number 148 _symmetry_space_group_name_Hall '-R 3' _symmetry_space_group_name_H-M 'R -3 :H' _[local]_cod_cif_authors_sg_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 7.0900(10) _cell_length_b 7.0900(10) _cell_length_c 27.351(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1190.7(3) _cell_formula_units_Z 3 _cell_measurement_reflns_used 18 _cell_measurement_theta_min 16.5 _cell_measurement_theta_max 20.3 _cell_measurement_temperature 9.5(3) _exptl_crystal_description 'Trigonal antiprism' _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.14 _exptl_crystal_density_diffrn 2.337 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 819 _exptl_absorpt_coefficient_mu 4.747 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.3558 _exptl_absorpt_correction_T_max 0.5425 _diffrn_ambient_temperature 10(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator none _diffrn_measurement_device_type 'Huber 512' _diffrn_measurement_method '\w/2\q' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16066 _diffrn_reflns_av_R_equivalents 0.0201 _diffrn_reflns_av_sigmaI/netI 0.0119 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 50.16 _diffrn_reflns_theta_full 50.16 _diffrn_measured_fraction_theta_max 0.335 _diffrn_measured_fraction_theta_full 0.335 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -58 _diffrn_reflns_limit_l_max 58 _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.3 _reflns_number_total 2827 _reflns_number_gt 2589 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0268 _refine_ls_R_factor_gt 0.0198 _refine_ls_wR_factor_ref 0.0511 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_number_reflns 2827 _refine_ls_number_parameters 46 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment mixed _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0293P)^2^+1.4386P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.914 _refine_diff_density_min -1.075 _refine_ls_extinction_method 'SHELXTL (Sheldrick, 1983)' _refine_ls_extinction_coef 0.0033(2) 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' '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' 'Rb' 'Rb' -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Ru 0.0000 0.0000 0.0000 0.00513(2) Uani d S 1 . . Ru N 0.16788(13) -0.11250(13) -0.04367(3) 0.00935(12) Uani d . 1 . . N H(1) 0.220(4) -0.189(5) -0.0282(7) 0.011(4) Uiso d . 1 . . H H(2) 0.304(4) -0.006(4) -0.0505(9) 0.017(5) Uiso d . 1 . . H H(3) 0.100(6) -0.176(6) -0.0704(9) 0.038(9) Uiso d . 1 . . H Cl 0.0000 0.0000 0.185561(10) 0.00644(4) Uani d S 1 . . Cl O(1) 0.0000 0.0000 0.13282(4) 0.01150(15) Uani d S 1 . . O O(2) 0.08546(12) -0.13461(12) 0.20351(3) 0.01010(12) Uani d . 1 . . O Cl(1) 0.0000 0.0000 0.376444(12) 0.00866(4) Uani d S 1 . . Cl Rb 0.0000 0.0000 0.5000 0.00632(3) Uani d S 1 . . Rb loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru 0.00554(3) 0.00554(3) 0.00429(4) 0.002770(10) 0.000 0.000 N 0.0102(3) 0.0107(3) 0.0081(2) 0.0059(3) 0.00022(17) -0.00084(18) Cl 0.00680(6) 0.00680(6) 0.00573(8) 0.00340(3) 0.000 0.000 O(1) 0.0147(2) 0.0147(2) 0.0051(2) 0.00735(12) 0.000 0.000 O(2) 0.0112(3) 0.0103(3) 0.0113(2) 0.0073(3) 0.00015(17) 0.00121(17) Cl(1) 0.00886(6) 0.00886(6) 0.00826(8) 0.00443(3) 0.000 0.000 Rb 0.00641(4) 0.00641(4) 0.00613(5) 0.00321(2) 0.000 0.000