#------------------------------------------------------------------------------ #$Date: 2016-02-20 02:53:41 +0200 (Sat, 20 Feb 2016) $ #$Revision: 176768 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/10/18/2101859.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2101859 loop_ _publ_author_name 'Boldyreva, E.' 'Kivikoski, J.' 'Howard, J. A. K.' _publ_section_title ; Distortion of Crystal Structures of Some Co^III^ Ammine Complexes. II. Distortion of Crystal Structures of [Co(NH~3~)~5~NO~2~]X~2~ (X = Cl, Br) on Cooling ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 405 _journal_page_last 414 _journal_paper_doi 10.1107/S0108768196014863 _journal_volume 53 _journal_year 1997 _chemical_formula_iupac '[Co (N O2) (N H3)5] Br2' _chemical_formula_moiety 'H15 Br2 Co N6 O2' _chemical_formula_sum 'Br2 Co H15 N6 O2' _chemical_formula_weight 349.93 _chemical_name_systematic 'nitropentaammine Co(III) bromide' _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 94.97(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 10.575(2) _cell_length_b 8.815(5) _cell_length_c 10.970(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 150 _cell_measurement_theta_max 24.9 _cell_measurement_theta_min 23.99 _cell_volume 1018.8(6) _computing_cell_refinement 'MSC/AFC Diffractometer Control Software' _computing_data_collection ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1988) ; _computing_data_reduction 'TEXSAN (Molecular Structure Corporation, 1989)' _computing_molecular_graphics 'SHELXTL-Plus (Sheldrick, 1989)' _computing_publication_material SHELXL93 _computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _diffrn_ambient_temperature 150 _diffrn_measurement_device 'Rigaku AFC6S 4-circle diffractometer' _diffrn_measurement_method '\w/2\q scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.02 _diffrn_reflns_av_sigmaI/netI 0.0315 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 2605 _diffrn_reflns_theta_max 28.01 _diffrn_reflns_theta_min 3.01 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 150 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 9.50 _exptl_absorpt_correction_T_max 0.1176 _exptl_absorpt_correction_T_min 0.0438 _exptl_absorpt_correction_type 'analytical (de Meulenauer & Tompa, 1965)' _exptl_crystal_colour ruby _exptl_crystal_density_diffrn 2.282 _exptl_crystal_density_meas ? _exptl_crystal_description 'distorted cuboctahedron' _exptl_crystal_F_000 680 _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.4 _refine_diff_density_max 0.522 _refine_diff_density_min -0.393 _refine_ls_extinction_coef 0.0075(3) _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_all 1.100 _refine_ls_goodness_of_fit_obs 1.156 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 59 _refine_ls_number_reflns 1230 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.100 _refine_ls_restrained_S_obs 1.156 _refine_ls_R_factor_all 0.0294 _refine_ls_R_factor_obs 0.0188 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0188P)^2^+0.6873P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.0485 _refine_ls_wR_factor_obs 0.0465 _reflns_number_observed 1034 _reflns_number_total 1230 _reflns_observed_criterion >2sigma(I) _cod_data_source_file hr0034.cif _cod_data_source_block cobr2lt _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w = 1/[\s^2^(Fo^2^)+(0.0188P)^2^+0.6873P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 1/[\s^2^(Fo^2^)+(0.0188P)^2^+0.6873P] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_database_code 2101859 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' 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 Co1 0.0134(2) 0.0151(2) 0.0113(2) 0.000 0.0010(2) 0.000 Br1 0.01738(14) 0.02281(15) 0.01754(14) 0.00162(10) 0.00176(9) -0.00060(9) N4 0.0179(14) 0.0203(15) 0.0161(14) 0.000 0.0014(12) 0.000 N3 0.0227(11) 0.0212(10) 0.0141(10) -0.0015(9) 0.0010(8) 0.0009(8) O1 0.0359(12) 0.0230(10) 0.0327(11) 0.0040(9) 0.0166(9) -0.0035(9) N2 0.0159(10) 0.0267(12) 0.0219(11) 0.0017(9) 0.0028(9) -0.0022(9) N1 0.029(2) 0.0176(14) 0.019(2) 0.000 0.0008(13) 0.000 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol Co1 0.0000 0.29000(5) 0.2500 0.01327(12) Uani d S 1 Co Br1 0.20719(2) 0.01728(3) 0.01109(2) 0.01923(10) Uani d . 1 Br N4 0.0000 0.5084(3) 0.2500 0.0181(6) Uani d S 1 N N3 0.0154(2) 0.2948(2) 0.4299(2) 0.0194(4) Uani d . 1 N H3A 0.0277(19) 0.2067(18) 0.4570(6) 0.029 Uiso calc R 1 H H3B -0.0515(15) 0.330(2) 0.4545(5) 0.029 Uiso calc R 1 H H3C 0.0767(18) 0.350(2) 0.4547(5) 0.029 Uiso calc R 1 H O1 -0.0727(2) 0.5786(2) 0.3126(2) 0.0298(5) Uani d . 1 O N2 0.1852(2) 0.2894(3) 0.2484(2) 0.0214(5) Uani d . 1 N H2A 0.2093(6) 0.2047(19) 0.2175(19) 0.032 Uiso calc R 1 H H2B 0.2200(7) 0.299(2) 0.3226(15) 0.032 Uiso calc R 1 H H2C 0.2084(5) 0.365(2) 0.2044(18) 0.032 Uiso calc R 1 H N1 0.0000 0.0643(4) 0.2500 0.0218(7) Uani d S 1 N H1A -0.085(3) 0.0277(12) 0.228(8) 0.033 Uiso calc PR 0.50 H H1B 0.029(8) 0.0277(12) 0.331(3) 0.033 Uiso calc PR 0.50 H H1C 0.056(7) 0.0277(12) 0.192(6) 0.033 Uiso calc PR 0.50 H 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' Co Co 0.3494 0.9721 '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_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -10 0 4 10 0 -4 4 -8 -1 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N4 Co1 N2 . . 90.16(7) ? N4 Co1 N2 . 2 90.16(7) ? N2 Co1 N2 . 2 179.67(14) ? N4 Co1 N3 . 2 88.77(7) ? N2 Co1 N3 . 2 89.25(9) ? N2 Co1 N3 2 2 90.75(9) ? N4 Co1 N3 . . 88.77(7) ? N2 Co1 N3 . . 90.75(9) ? N2 Co1 N3 2 . 89.25(9) ? N3 Co1 N3 2 . 177.54(13) ? N4 Co1 N1 . . 180.0 ? N2 Co1 N1 . . 89.84(7) ? N2 Co1 N1 2 . 89.84(7) ? N3 Co1 N1 2 . 91.23(7) ? N3 Co1 N1 . . 91.23(7) ? O1 N4 O1 2 . 120.1(3) yes O1 N4 Co1 2 . 120.0(2) yes O1 N4 Co1 . . 120.0(2) ? Co1 N3 H3A . . 109.47(7) ? Co1 N3 H3B . . 109.47(7) ? H3A N3 H3B . . 109.5 ? Co1 N3 H3C . . 109.47(7) ? H3A N3 H3C . . 109.5 ? H3B N3 H3C . . 109.5 ? Co1 N2 H2A . . 109.47(7) ? Co1 N2 H2B . . 109.47(7) ? H2A N2 H2B . . 109.5 ? Co1 N2 H2C . . 109.47(7) ? H2A N2 H2C . . 109.5 ? H2B N2 H2C . . 109.5 ? Co1 N1 H1A . . 109.471(11) ? Co1 N1 H1B . . 109.471(13) ? H1A N1 H1B . . 109.5 ? Co1 N1 H1C . . 109.47(2) ? H1A N1 H1C . . 109.5 ? H1B N1 H1C . . 109.5 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Co1 N4 . 1.925(3) yes Co1 N2 . 1.960(2) yes Co1 N2 2 1.960(2) ? Co1 N3 2 1.966(2) ? Co1 N3 . 1.966(2) yes Co1 N1 . 1.990(3) yes N4 O1 2 1.240(2) ? N4 O1 . 1.240(2) yes N3 H3A . 0.84(2) ? N3 H3B . 0.84(2) ? N3 H3C . 0.84(2) ? N2 H2A . 0.87(2) ? N2 H2B . 0.87(2) ? N2 H2C . 0.87(2) ? N1 H1A . 0.97(3) ? N1 H1B . 0.97(3) ? N1 H1C . 0.97(3) ?