#------------------------------------------------------------------------------ #$Date: 2009-11-16 01:43:51 +0000 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003164.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_2003164 _journal_name_full 'Acta Crystallographica, Section B' _journal_volume 54 _journal_year 1998 _journal_page_first 613 _journal_page_last 625 _chemical_formula_moiety 'Cs1,Cr1 N6 H18,2(Cl1 O4),2Br' _chemical_formula_sum 'Br2 Cl2 Cr1 Cs1 H18 N6 O8' _chemical_formula_iupac 'Cs[Cr(N H3)6],2(Cl O4),2Br' _chemical_formula_weight 645.83 _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 7.3690(10) _cell_length_b 7.3690(10) _cell_length_c 27.578(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1296.9(3) _cell_formula_units_Z 3 _cell_measurement_reflns_used 18 _cell_measurement_theta_min 16.0 _cell_measurement_theta_max 19.5 _cell_measurement_temperature 10(2) _exptl_crystal_description Plate _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.14 _exptl_crystal_density_diffrn 2.481 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 921 _exptl_absorpt_coefficient_mu 7.704 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.2088 _exptl_absorpt_correction_T_max 0.3836 _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 5118 _diffrn_reflns_av_R_equivalents 0.0228 _diffrn_reflns_av_sigmaI/netI 0.0105 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 30.06 _diffrn_reflns_theta_full 30.06 _diffrn_measured_fraction_theta_max 0.335 _diffrn_measured_fraction_theta_full 0.335 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.5 _reflns_number_total 861 _reflns_number_gt 858 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0098 _refine_ls_R_factor_gt 0.0098 _refine_ls_wR_factor_ref 0.0240 _refine_ls_goodness_of_fit_ref 1.156 _refine_ls_restrained_S_all 1.156 _refine_ls_number_reflns 861 _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^)+(0.0101P)^2^+1.4748P] 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 0.293 _refine_diff_density_min -0.468 _refine_ls_extinction_method 'SHELXTL (Sheldrick, 1983)' _refine_ls_extinction_coef 0.00373(12) 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' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cs' 'Cs' -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 '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 Cr 0.0000 0.0000 0.0000 0.00325(8) Uani d S 1 . . Cr N 0.1031(2) -0.1587(2) -0.04434(4) 0.0065(3) Uani d . 1 . . N H(1) 0.215(4) -0.164(4) -0.0303(7) 0.013(5) Uiso d . 1 . . H H(2) 0.147(5) -0.102(6) -0.0724(7) 0.022(6) Uiso d . 1 . . H H(3) -0.001(4) -0.294(4) -0.0469(9) 0.024(6) Uiso d . 1 . . H Cl 0.0000 0.0000 0.188776(14) 0.00427(8) Uani d S 1 . . Cl O(1) 0.0000 0.0000 0.13597(5) 0.0091(3) Uani d S 1 . . O O(2) 0.13238(18) -0.07939(19) 0.20639(3) 0.0080(3) Uani d . 1 . . O Br 0.0000 0.0000 0.371211(6) 0.00481(5) Uani d S 1 . . Br Cs 0.0000 0.0000 0.5000 0.00401(5) Uani d S 1 . . Cs 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 Cr 0.00355(11) 0.00355(11) 0.00266(16) 0.00178(5) 0.000 0.000 N 0.0068(7) 0.0073(7) 0.0054(5) 0.0036(6) 0.0005(4) -0.0005(4) Cl 0.00459(11) 0.00459(11) 0.00362(17) 0.00230(6) 0.000 0.000 O(1) 0.0122(4) 0.0122(4) 0.0028(6) 0.0061(2) 0.000 0.000 O(2) 0.0079(6) 0.0095(6) 0.0096(4) 0.0065(6) -0.0013(4) 0.0002(4) Br 0.00502(7) 0.00502(7) 0.00439(9) 0.00251(3) 0.000 0.000 Cs 0.00423(6) 0.00423(6) 0.00356(7) 0.00211(3) 0.000 0.000