#------------------------------------------------------------------------------ #$Date: 2008-04-05 11:13:02 +0300 (Sat, 05 Apr 2008) $ #$Revision: 340 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2101856.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_2101856 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] 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' _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 95.050(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 10.338(2) _cell_length_b 8.687(2) _cell_length_c 10.756(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 290 _cell_measurement_theta_max 24.995 _cell_measurement_theta_min 24.695 _cell_volume 962.2(3) _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 0.0266 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _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 2469 _diffrn_reflns_theta_max 27.97 _diffrn_reflns_theta_min 3.07 _diffrn_standards_decay_% none _diffrn_standards_interval_count 150 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 2.31 _exptl_absorpt_correction_T_max 0.5383 _exptl_absorpt_correction_T_min 0.3908 _exptl_absorpt_correction_type 'analytical (de Meulenauer, & Tompa, 1965)' _exptl_crystal_colour ruby _exptl_crystal_density_diffrn 1.802 _exptl_crystal_density_meas 'not measured' _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 0.223 _refine_diff_density_min -0.264 _refine_ls_extinction_coef 0.0635(17) _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_all 0.984 _refine_ls_goodness_of_fit_obs 0.994 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 59 _refine_ls_number_reflns 1163 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.984 _refine_ls_restrained_S_obs 0.994 _refine_ls_R_factor_all 0.0208 _refine_ls_R_factor_obs 0.0175 _refine_ls_shift/esd_max -0.005 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w = 1/[\s^2^(Fo^2^)+(0.0220P)^2^+0.8015P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_all 0.0479 _refine_ls_wR_factor_obs 0.0464 _reflns_number_observed 1074 _reflns_number_total 1163 _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 -2 0 -2 -2 2 -2 0 2 -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' 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_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol Co1 0.0000 0.28552(3) 0.2500 0.01892(11) Uani d S 1 Co Cl1 0.20751(4) 0.01613(5) 0.01368(3) 0.03235(12) Uani d . 1 Cl N3 0.01826(14) 0.2880(2) 0.43265(11) 0.0302(3) Uani d . 1 N H3A 0.0455(13) 0.2041(13) 0.4588(4) 0.045 Uiso calc R 1 H H3B -0.0528(11) 0.3051(15) 0.4587(4) 0.045 Uiso calc R 1 H H3C 0.0697(12) 0.3560(15) 0.4572(4) 0.045 Uiso calc R 1 H N4 0.0000 0.5071(2) 0.2500 0.0247(3) Uani d S 1 N N2 0.18915(13) 0.2874(2) 0.24672(14) 0.0340(3) Uani d . 1 N H2A 0.2148(4) 0.2001(13) 0.2346(15) 0.051 Uiso calc R 1 H H2B 0.2227(5) 0.3190(18) 0.3136(11) 0.051 Uiso calc R 1 H H2C 0.2089(3) 0.3440(17) 0.1906(12) 0.051 Uiso calc R 1 H N1 0.0000 0.0566(2) 0.2500 0.0351(4) Uani d S 1 N H1A 0.043(8) 0.0253(8) 0.312(5) 0.053 Uiso calc PR 0.50 H H1B 0.032(9) 0.0253(8) 0.188(5) 0.053 Uiso calc PR 0.50 H H1C -0.0744(19) 0.0253(8) 0.250(10) 0.053 Uiso calc PR 0.50 H O1 -0.07315(13) 0.57829(15) 0.31376(12) 0.0429(3) Uani d . 1 O 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 0.02051(15) 0.0203(2) 0.01572(14) 0.000 0.00055(8) 0.000 Cl1 0.0330(2) 0.0349(2) 0.0293(2) 0.00328(14) 0.00295(14) -0.00120(14) N3 0.0391(7) 0.0315(7) 0.0196(5) -0.0019(5) 0.0002(5) 0.0008(5) N4 0.0277(8) 0.0258(8) 0.0202(8) 0.000 0.0009(6) 0.000 N2 0.0255(6) 0.0392(8) 0.0373(7) 0.0037(5) 0.0024(5) -0.0056(6) N1 0.0490(11) 0.0256(9) 0.0299(9) 0.000 -0.0019(8) 0.000 O1 0.0535(7) 0.0333(6) 0.0445(7) 0.0094(6) 0.0181(6) -0.0052(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(2) yes Co1 N3 . 1.9571(12) yes Co1 N3 2 1.9571(12) ? Co1 N2 2 1.9590(14) yes Co1 N2 . 1.9590(14) ? Co1 N1 . 1.989(2) yes N3 H3A . 0.822(12) ? N3 H3B . 0.822(12) ? N3 H3C . 0.822(12) ? N4 O1 . 1.2312(15) yes N4 O1 2 1.2312(15) ? N2 H2A . 0.818(12) ? N2 H2B . 0.818(12) ? N2 H2C . 0.818(12) ? N1 H1A . 0.82(2) ? N1 H1B . 0.82(2) ? N1 H1C . 0.82(2) ? 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 . . 89.36(4) ? N4 Co1 N3 . 2 89.36(4) ? N3 Co1 N3 . 2 178.72(8) ? N4 Co1 N2 . 2 89.52(4) ? N3 Co1 N2 . 2 89.43(6) ? N3 Co1 N2 2 2 90.56(6) ? N4 Co1 N2 . . 89.52(4) ? N3 Co1 N2 . . 90.56(6) ? N3 Co1 N2 2 . 89.43(6) ? N2 Co1 N2 2 . 179.03(8) ? N4 Co1 N1 . . 180.0 ? N3 Co1 N1 . . 90.64(4) ? N3 Co1 N1 2 . 90.64(4) ? N2 Co1 N1 2 . 90.48(4) ? N2 Co1 N1 . . 90.48(4) ? Co1 N3 H3A . . 109.47(4) ? Co1 N3 H3B . . 109.47(4) ? H3A N3 H3B . . 109.5 ? Co1 N3 H3C . . 109.47(4) ? H3A N3 H3C . . 109.5 ? H3B N3 H3C . . 109.5 ? O1 N4 O1 . 2 119.7(2) yes O1 N4 Co1 . . 120.15(9) yes O1 N4 Co1 2 . 120.15(9) ? Co1 N2 H2A . . 109.47(4) ? 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(8) ? Co1 N1 H1B . . 109.471(12) ? H1A N1 H1B . . 109.5 ? Co1 N1 H1C . . 109.471(7) ? H1A N1 H1C . . 109.5 ? H1B N1 H1C . . 109.5 ?