#------------------------------------------------------------------------------
#$Date: 2016-02-20 01:53:41 +0100 (Sat 20 de Feb de 2016) $
#$Revision: 176768 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/18/2101858.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 CoIII Ammine Complexes. II.
 Distortion of Crystal Structures of [Co(NH₃)₅NO₂]X₂
 (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                 94.70(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       'ω/2θ 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_%        0
_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      ?
_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_details
'w = 1/[σ²(Fo²)+(0.0229P)²+0.0603P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_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)
_cod_data_source_file            hr0034.cif
_cod_data_source_block           cobr2rt
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0229P)^2^+0.0603P] 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^)+(0.0229P)^2^+0.0603P] 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               2101858
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 0.0215(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_
_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_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
0 -4 0
-5 -3 0
0 -2 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 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 ?
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) ?
