#------------------------------------------------------------------------------ #$Date: 2008-04-05 11:13:02 +0300 (Sat, 05 Apr 2008) $ #$Revision: 340 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2101858.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_2101858 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_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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 94.70(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 10.680(3) _cell_length_b 8.838(4) _cell_length_c 10.990(3) _cell_measurement_reflns_used 25 _cell_measurement_temperature 290 _cell_measurement_theta_max 23.925 _cell_measurement_theta_min 21.145 _cell_volume 1033.9(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 290 _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 0.0375 _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 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 2648 _diffrn_reflns_theta_max 28.02 _diffrn_reflns_theta_min 3.44 _diffrn_standards_decay_% none _diffrn_standards_interval_count 150 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 9.36 _exptl_absorpt_correction_T_max 0.1197 _exptl_absorpt_correction_T_min 0.0450 _exptl_absorpt_correction_type 'analytical (de Meulenauer & Tompa, 1965)' _exptl_crystal_colour ruby _exptl_crystal_density_diffrn 2.248 _exptl_crystal_density_meas 'not measured' _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 0.375 _refine_diff_density_min -0.454 _refine_ls_extinction_coef 0.0095(4) _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_all 1.036 _refine_ls_goodness_of_fit_obs 1.104 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 59 _refine_ls_number_reflns 1249 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.036 _refine_ls_restrained_S_obs 1.104 _refine_ls_R_factor_all 0.0395 _refine_ls_R_factor_obs 0.0214 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w = 1/[\s^2^(Fo^2^)+(0.0229P)^2^+0.0603P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_all 0.0522 _refine_ls_wR_factor_obs 0.0490 _reflns_number_observed 981 _reflns_number_total 1249 _reflns_observed_criterion >2sigma(I) _[local]_cod_data_source_file hr0034.cif 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_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 -4 0 -5 -3 0 0 -2 6 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_ _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 0.28837(5) 0.2500 0.02081(14) Uani d S 1 Co Br1 0.20769(3) 0.01538(3) 0.01036(3) 0.03177(11) Uani d . 1 Br N4 0.0000 0.5067(4) 0.2500 0.0271(7) Uani d S 1 N N3 0.0134(2) 0.2930(3) 0.4295(2) 0.0299(5) Uani d . 1 N H3A 0.014(2) 0.2012(18) 0.4574(6) 0.045 Uiso calc R 1 H H3B -0.0503(16) 0.342(2) 0.4545(5) 0.045 Uiso calc R 1 H H3C 0.0825(17) 0.338(2) 0.4558(6) 0.045 Uiso calc R 1 H N2 0.1841(2) 0.2880(3) 0.2501(2) 0.0318(5) Uani d . 1 N H2A 0.2098(6) 0.1972(19) 0.227(2) 0.048 Uiso calc R 1 H H2B 0.2182(7) 0.309(2) 0.3249(16) 0.048 Uiso calc R 1 H H2C 0.2076(5) 0.358(2) 0.1981(17) 0.048 Uiso calc R 1 H O1 -0.0715(2) 0.5759(3) 0.3125(2) 0.0490(6) Uani d . 1 O N1 0.0000 0.0632(4) 0.2500 0.0323(8) Uani d S 1 N H1A -0.081(5) 0.0251(12) 0.207(8) 0.049 Uiso calc PR 0.50 H H1B 0.008(9) 0.0251(12) 0.337(3) 0.049 Uiso calc PR 0.50 H H1C 0.073(6) 0.0251(12) 0.206(8) 0.049 Uiso calc PR 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 Co1 0.0215(2) 0.0231(3) 0.0179(2) 0.000 0.0021(2) 0.000 Br1 0.0306(2) 0.0353(2) 0.0295(2) 0.00255(12) 0.00310(11) -0.00065(12) N4 0.029(2) 0.028(2) 0.024(2) 0.000 0.0032(13) 0.000 N3 0.0378(13) 0.0306(12) 0.0213(11) -0.0014(10) 0.0013(9) 0.0000(9) N2 0.0255(11) 0.0374(14) 0.0325(13) 0.0013(10) 0.0031(10) -0.0051(11) O1 0.059(2) 0.0332(11) 0.059(2) 0.0055(11) 0.0281(12) -0.0061(11) N1 0.043(2) 0.027(2) 0.027(2) 0.000 0.0009(15) 0.000 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 . 1.930(3) yes Co1 N2 . 1.966(2) yes Co1 N2 2 1.966(2) ? Co1 N3 2 1.967(2) yes Co1 N3 . 1.967(2) ? Co1 N1 . 1.990(4) yes N4 O1 2 1.231(3) yes N4 O1 . 1.231(3) ? N3 H3A . 0.87(2) ? N3 H3B . 0.87(2) ? N3 H3C . 0.87(2) ? N2 H2A . 0.89(2) ? N2 H2B . 0.89(2) ? N2 H2C . 0.89(2) ? N1 H1A . 1.01(3) ? N1 H1B . 1.01(3) ? N1 H1C . 1.01(3) ? 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 . . 90.10(7) ? N4 Co1 N2 . 2 90.10(7) ? N2 Co1 N2 . 2 179.80(15) ? N4 Co1 N3 . 2 88.80(7) ? N2 Co1 N3 . 2 89.47(10) ? N2 Co1 N3 2 2 90.53(10) ? N4 Co1 N3 . . 88.80(7) ? N2 Co1 N3 . . 90.53(10) ? N2 Co1 N3 2 . 89.47(10) ? N3 Co1 N3 2 . 177.61(14) ? N4 Co1 N1 . . 180.0 ? N2 Co1 N1 . . 89.90(7) ? N2 Co1 N1 2 . 89.90(7) ? N3 Co1 N1 2 . 91.20(7) ? N3 Co1 N1 . . 91.20(7) ? O1 N4 O1 2 . 120.4(3) yes O1 N4 Co1 2 . 119.8(2) ? O1 N4 Co1 . . 119.8(2) yes 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(8) ? H2A N2 H2C . . 109.5 ? H2B N2 H2C . . 109.5 ? Co1 N1 H1A . . 109.471(10) ? Co1 N1 H1B . . 109.471(12) ? H1A N1 H1B . . 109.5 ? Co1 N1 H1C . . 109.47(2) ? H1A N1 H1C . . 109.5 ? H1B N1 H1C . . 109.5 ?