#------------------------------------------------------------------------------ #$Date: 2016-02-20 02:53:41 +0200 (Sat, 20 Feb 2016) $ #$Revision: 176768 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/10/18/2101857.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_2101857 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] Cl2' _chemical_formula_moiety 'H15 Cl2 Co N6 O2' _chemical_formula_sum 'Cl2 Co H15 N6 O2' _chemical_formula_weight 261.01 _chemical_name_systematic 'nitropentaammine Co(III) chloride' _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 95.41(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 10.215(3) _cell_length_b 8.697(4) _cell_length_c 10.748(3) _cell_measurement_reflns_used 25 _cell_measurement_temperature 150 _cell_measurement_theta_max 24.99 _cell_measurement_theta_min 24.775 _cell_volume 950.6(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 0.0201 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 2446 _diffrn_reflns_theta_max 28.00 _diffrn_reflns_theta_min 3.08 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 150 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 2.34 _exptl_absorpt_correction_T_max 0.5342 _exptl_absorpt_correction_T_min 0.3874 _exptl_absorpt_correction_type 'analytical (de Meulenauer & Tompa, 1965)' _exptl_crystal_colour ruby _exptl_crystal_density_diffrn 1.824 _exptl_crystal_density_meas ? _exptl_crystal_description 'distorted cuboctahedron' _exptl_crystal_F_000 536 _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.4 _refine_diff_density_max 0.251 _refine_diff_density_min -0.286 _refine_ls_extinction_coef 0.0579(12) _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_all 1.106 _refine_ls_goodness_of_fit_obs 1.124 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 59 _refine_ls_number_reflns 1152 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.106 _refine_ls_restrained_S_obs 1.124 _refine_ls_R_factor_all 0.0174 _refine_ls_R_factor_obs 0.0152 _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^)+(0.0126P)^2^+0.6359P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.0379 _refine_ls_wR_factor_obs 0.0372 _reflns_number_observed 1077 _reflns_number_total 1152 _reflns_observed_criterion >2sigma(I) _cod_data_source_file hr0034.cif _cod_data_source_block cocl2lt _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w = 1/[\s^2^(Fo^2^)+(0.0126P)^2^+0.6359P] 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^)+(0.0126P)^2^+0.6359P] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 950.7(6) _cod_database_code 2101857 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 0.01256(13) 0.01219(13) 0.00943(12) 0.000 0.00025(7) 0.000 Cl1 0.0193(2) 0.0203(2) 0.01674(15) 0.00227(10) 0.00153(10) -0.00054(10) O1 0.0314(5) 0.0204(4) 0.0242(5) 0.0059(4) 0.0088(4) -0.0036(4) N3 0.0218(5) 0.0187(5) 0.0126(5) -0.0013(4) -0.0001(4) 0.0006(4) N4 0.0178(7) 0.0170(7) 0.0113(6) 0.000 -0.0005(5) 0.000 N2 0.0169(5) 0.0242(6) 0.0212(5) -0.0031(4) 0.0019(4) 0.0016(4) N1 0.0345(9) 0.0162(7) 0.0191(7) 0.000 -0.0020(6) 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 0.28784(2) 0.2500 0.01144(9) Uani d S 1 Co Cl1 0.20713(3) 0.01902(3) 0.01504(3) 0.01878(9) Uani d . 1 Cl O1 -0.07355(10) 0.57980(11) 0.31472(9) 0.0250(2) Uani d . 1 O N3 0.02304(11) 0.28945(12) 0.43304(9) 0.0178(2) Uani d . 1 N H3A 0.0544(10) 0.2037(11) 0.4593(3) 0.027 Uiso calc R 1 H H3B -0.0509(9) 0.3041(12) 0.4613(4) 0.027 Uiso calc R 1 H H3C 0.0755(10) 0.3613(12) 0.4579(3) 0.027 Uiso calc R 1 H N4 0.0000 0.5085(2) 0.2500 0.0155(3) Uani d S 1 N N2 -0.19115(11) 0.29091(13) 0.25606(11) 0.0208(2) Uani d . 1 N H2A -0.2174(4) 0.2029(11) 0.2698(11) 0.031 Uiso calc R 1 H H2B -0.2270(4) 0.3219(13) 0.1882(9) 0.031 Uiso calc R 1 H H2C -0.2100(3) 0.3493(13) 0.3127(10) 0.031 Uiso calc R 1 H N1 0.0000 0.0596(2) 0.2500 0.0236(3) Uani d S 1 N H1A 0.007(7) 0.0277(7) 0.3232(14) 0.035 Uiso calc PR 0.50 H H1B 0.063(4) 0.0277(7) 0.214(6) 0.035 Uiso calc PR 0.50 H H1C -0.070(3) 0.0277(7) 0.213(5) 0.035 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' 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_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 9 -6 -10 -2 -6 1 -9 -6 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 N3 . . 89.59(3) ? N4 Co1 N3 . 2 89.59(3) ? N3 Co1 N3 . 2 179.18(6) ? N4 Co1 N2 . . 89.22(3) ? N3 Co1 N2 . . 89.55(5) ? N3 Co1 N2 2 . 90.43(5) ? N4 Co1 N2 . 2 89.22(3) ? N3 Co1 N2 . 2 90.43(5) ? N3 Co1 N2 2 2 89.55(5) ? N2 Co1 N2 . 2 178.44(7) ? N4 Co1 N1 . . 180.0 ? N3 Co1 N1 . . 90.41(3) ? N3 Co1 N1 2 . 90.41(3) ? N2 Co1 N1 . . 90.78(3) ? N2 Co1 N1 2 . 90.78(3) ? Co1 N3 H3A . . 109.47(3) ? Co1 N3 H3B . . 109.47(4) ? H3A N3 H3B . . 109.5 ? Co1 N3 H3C . . 109.47(3) ? H3A N3 H3C . . 109.5 ? H3B N3 H3C . . 109.5 ? O1 N4 O1 . 2 119.8(2) yes O1 N4 Co1 . . 120.08(8) yes O1 N4 Co1 2 . 120.08(8) ? Co1 N2 H2A . . 109.47(3) ? Co1 N2 H2B . . 109.47(4) ? H2A N2 H2B . . 109.5 ? Co1 N2 H2C . . 109.47(4) ? H2A N2 H2C . . 109.5 ? H2B N2 H2C . . 109.5 ? Co1 N1 H1A . . 109.471(12) ? Co1 N1 H1B . . 109.471(14) ? H1A N1 H1B . . 109.5 ? Co1 N1 H1C . . 109.471(10) ? 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 . 1.919(2) yes Co1 N3 . 1.9592(11) yes Co1 N3 2 1.9592(11) ? Co1 N2 . 1.9600(12) yes Co1 N2 2 1.9600(12) ? Co1 N1 . 1.985(2) yes O1 N4 . 1.2376(12) yes N3 H3A . 0.850(10) ? N3 H3B . 0.850(10) ? N3 H3C . 0.850(10) ? N4 O1 2 1.2376(12) ? N2 H2A . 0.829(10) ? N2 H2B . 0.829(10) ? N2 H2C . 0.829(10) ? N1 H1A . 0.83(2) ? N1 H1B . 0.83(2) ? N1 H1C . 0.83(2) ?