#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003151.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_2003151 _journal_name_full 'Acta Crystallographica, Section B' _journal_volume 54 _journal_year 1998 _journal_page_first 613 _journal_page_last 625 _chemical_formula_moiety 'N1 H4,Co1 H18 N6,2(Cl1 O4),2Cl' _chemical_formula_sum 'Cl4 Co H22 N7 O8' _[local]_cod_chemical_formula_sum_orig 'Cl4 Co1 H22 N7 O8' _chemical_formula_iupac 'N H4[Co(N H3)6],2(Cl O4),Cl2' _chemical_formula_weight 448.98 _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 _[local]_cod_cif_authors_sg_Hall '-P 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 7.0250(10) _cell_length_b 7.0250(10) _cell_length_c 26.988(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1153.4(6) _cell_formula_units_Z 3 _cell_measurement_reflns_used 18 _cell_measurement_theta_min 16.6 _cell_measurement_theta_max 20.5 _cell_measurement_temperature 92(2) _exptl_crystal_description Plate _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.939 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 690 _exptl_absorpt_coefficient_mu 1.855 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.6300 _exptl_absorpt_correction_T_max 0.7000 _diffrn_ambient_temperature 92(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P3/P4' _diffrn_measurement_method '\w/2\q' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 1020 _diffrn_reflns_av_R_equivalents 0.0111 _diffrn_reflns_av_sigmaI/netI 0.0089 _diffrn_reflns_theta_min 6.26 _diffrn_reflns_theta_max 25.06 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_max 0.249 _diffrn_measured_fraction_theta_full 0.249 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min 6 _diffrn_reflns_limit_l_max 31 _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.1 _reflns_number_total 347 _reflns_number_gt 345 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0191 _refine_ls_R_factor_gt 0.0187 _refine_ls_wR_factor_ref 0.0533 _refine_ls_goodness_of_fit_ref 1.206 _refine_ls_restrained_S_all 1.175 _refine_ls_number_reflns 347 _refine_ls_number_parameters 40 _refine_ls_number_restraints 16 _refine_ls_hydrogen_treatment mixed _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0284P)^2^+1.8943P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 0.250 _refine_diff_density_min -0.219 _refine_ls_extinction_method 'SHELXTL (Sheldrick, 1983)' _refine_ls_extinction_coef 0.0026(10) 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' 'Co' 'Co' 0.3494 0.9721 '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 Co 0.0000 0.0000 0.0000 0.0046(3) Uani d S 1 . . Co N 0.1518(5) -0.1121(5) -0.04162(6) 0.0103(5) Uani d . 1 . . N H(1) 0.1784 -0.2058 -0.0236 0.033(6) Uiso calc R 1 . . H H(2) 0.2815 0.0023 -0.0524 0.033(6) Uiso calc R 1 . . H H(3) 0.0660 -0.1847 -0.0681 0.033(6) Uiso calc R 1 . . H Cl 0.0000 0.0000 0.18829(2) 0.0069(3) Uani d S 1 . . Cl O(1) 0.0000 0.0000 0.13485(8) 0.0157(7) Uani d S 1 . . O O(2) 0.0946(5) -0.1281(6) 0.20669(5) 0.0129(4) Uani d . 1 . . O Cl(1) 0.0000 0.0000 0.37559(3) 0.0092(3) Uani d S 1 . . Cl N(1) 0.0000 0.0000 0.5000 0.0097(10) Uani d SD 1 . . N H(4) 0.0000 0.0000 0.5340(7) 0.017(14) Uiso d SPD 0.50 . . H H5 0.096(9) -0.043(12) 0.4887(2) 0.017(14) Uiso d PD 0.50 . . H 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 Co 0.0051(3) 0.0051(3) 0.0036(4) 0.00256(16) 0.000 0.000 N 0.0137(18) 0.0114(13) 0.0083(8) 0.0081(12) -0.0019(10) -0.0022(9) Cl 0.0073(4) 0.0073(4) 0.0062(4) 0.00365(19) 0.000 0.000 O(1) 0.0203(12) 0.0203(12) 0.0065(12) 0.0101(6) 0.000 0.000 O(2) 0.0140(14) 0.0141(10) 0.0150(7) 0.0103(9) -0.0003(8) 0.0004(8) Cl(1) 0.0090(4) 0.0090(4) 0.0094(4) 0.00452(19) 0.000 0.000 N(1) 0.0106(18) 0.0106(18) 0.0079(18) 0.0053(9) 0.000 0.000 _cod_database_code 2003151