#------------------------------------------------------------------------------ #$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003162.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_2003162 _journal_name_full 'Acta Crystallographica, Section B' _journal_year 1998 _journal_volume B54 _journal_page_first 613 _journal_page_last 625 _chemical_formula_moiety 'Cs1,Cr1 N6 H18,2(Cl1 O4),2Cl' _chemical_formula_sum 'Cl4 Cr1 Cs1 H18 N6 O8' _chemical_formula_iupac 'Cs[Cr(N H3)6],2(Cl O4),2Cl' _chemical_formula_weight 556.91 _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'R-3' _symmetry_space_group_name_Hall '-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 7.2940(10) _cell_length_b 7.2940(10) _cell_length_c 27.311(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1258.3(4) _cell_formula_units_Z 3 _cell_measurement_reflns_used 18 _cell_measurement_theta_min 16.1 _cell_measurement_theta_max 19.7 _cell_measurement_temperature 10(2) _exptl_crystal_description Plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 2.205 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 813 _exptl_absorpt_coefficient_mu 3.495 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.6732 _exptl_absorpt_correction_T_max 0.8214 _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 4930 _diffrn_reflns_av_R_equivalents 0.0223 _diffrn_reflns_av_sigmaI/netI 0.0119 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 30.07 _diffrn_reflns_theta_full 30.07 _diffrn_measured_fraction_theta_max 0.333 _diffrn_measured_fraction_theta_full 0.333 _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 831 _reflns_number_gt 812 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0160 _refine_ls_R_factor_gt 0.0146 _refine_ls_wR_factor_ref 0.0436 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.112 _refine_ls_number_reflns 831 _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^)+(0.0246P)^2^+3.8280P] 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 0.963 _refine_diff_density_min -0.795 _refine_ls_extinction_method 'SHELXTL (Sheldrick, 1983)' _refine_ls_extinction_coef 0.0028(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' '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' 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 0.00417(13) Uani d S 1 . . Cr N 0.0895(3) -0.1759(3) -0.04356(7) 0.0080(4) Uani d . 1 . . N H(1) 0.174(11) -0.194(11) -0.0289(11) 0.019(8) Uiso d . 1 . . H H(2) 0.152(10) -0.124(10) -0.0702(12) 0.023(9) Uiso d . 1 . . H H(3) -0.008(7) -0.310(8) -0.0509(18) 0.040(13) Uiso d . 1 . . H Cl 0.0000 0.0000 0.18851(2) 0.00521(14) Uani d S 1 . . Cl O(1) 0.0000 0.0000 0.13523(8) 0.0100(4) Uani d S 1 . . O O(2) 0.1419(2) -0.0708(2) 0.20632(6) 0.0093(4) Uani d . 1 . . O Cl(1) 0.0000 0.0000 0.37047(2) 0.00476(13) Uani d S 1 . . Cl Cs 0.0000 0.0000 0.5000 0.00540(9) 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 0.00455(17) 0.00455(17) 0.0034(3) 0.00228(9) 0.000 0.000 N 0.0086(10) 0.0089(9) 0.0072(7) 0.0049(9) 0.0003(6) 0.0002(6) Cl 0.00548(19) 0.00548(19) 0.0047(3) 0.00274(9) 0.000 0.000 O(1) 0.0134(6) 0.0134(6) 0.0032(9) 0.0067(3) 0.000 0.000 O(2) 0.0104(9) 0.0120(10) 0.0096(6) 0.0086(9) -0.0019(5) -0.0006(5) Cl(1) 0.00490(17) 0.00490(17) 0.0045(3) 0.00245(8) 0.000 0.000 Cs 0.00539(10) 0.00539(10) 0.00544(13) 0.00269(5) 0.000 0.000