#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2006158.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_2006158
loop_
_publ_author_name
'Boldyreva, E. V.'
'Kivikoski, J.'
'Howard, J. A. K.'
_publ_section_title
;
 Pentaamminenitrocobalt(III) Chloride Nitrate at 290K and 150K
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              526
_journal_page_last               528
_journal_volume                  53
_journal_year                    1997
_chemical_formula_iupac          '[Co (N O2)(N H3)5 ] Cl (N O3)'
_chemical_formula_moiety         'H15 O5 N7 Cl Co'
_chemical_formula_sum            'Cl Co H15 N7 O5'
_chemical_formula_weight         287.57
_chemical_name_systematic
;
nitro-pentaammine-Co(III)-chloride-nitrate
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2c 2n'
_symmetry_space_group_name_H-M   'P n a m'
_audit_creation_method           SHELXL-93
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.814(3)
_cell_length_b                   9.623(2)
_cell_length_c                   7.309(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    290
_cell_measurement_theta_max      23.615
_cell_measurement_theta_min      16.955
_cell_volume                     1041.9(4)
_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           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.02
_diffrn_reflns_av_sigmaI/netI    0.0301
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2762
_diffrn_reflns_theta_max         28.01
_diffrn_reflns_theta_min         3.47
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.92
_exptl_absorpt_correction_T_max  0.681
_exptl_absorpt_correction_T_min  0.553
_exptl_absorpt_correction_type
;
  'empirical, 36 \y scans of 6 reflections (North, Phillips & Mathews, 1968)'
;
_exptl_crystal_colour            ruby
_exptl_crystal_density_diffrn    1.833
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_description       'elongated prism'
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.290
_refine_ls_extinction_coef       0.0061(8)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.993
_refine_ls_goodness_of_fit_obs   1.051
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     83
_refine_ls_number_reflns         1353
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.993
_refine_ls_restrained_S_obs      1.051
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_obs          0.0240
_refine_ls_shift/esd_max         0.058
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc w = 1/[\s^2^(Fo^2^)+(0.0342P)^2^+0.3911P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_all         0.0674
_refine_ls_wR_factor_obs         0.0623
_reflns_number_observed          1050
_reflns_number_total             1353
_reflns_observed_criterion       >2.0\s(I)
_[local]_cod_data_source_file    sk1070.cif
_[local]_cod_data_source_block   at_290K
_[local]_cod_cif_authors_sg_Hall '-P 2c -2n'
_[local]_cod_chemical_formula_sum_orig 'H15 O5 N7 Cl Co'
_cod_original_cell_volume        1041.9(6)
_cod_database_code               2006158
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z'
'x, y, -z-1/2'
'-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 0.0181(2) 0.0206(2) 0.0230(2) -0.00071(13) 0.000 0.000
Cl1 0.0275(3) 0.0308(4) 0.0341(4) 0.0034(3) 0.000 0.000
N1 0.0240(11) 0.0247(12) 0.0345(12) -0.0005(9) 0.000 0.000
N2 0.0266(8) 0.0308(9) 0.0313(9) -0.0026(6) -0.0027(7) 0.0009(8)
N4 0.0211(11) 0.0337(13) 0.0237(11) -0.0014(9) 0.000 0.000
N3 0.0262(8) 0.0324(9) 0.0341(9) -0.0020(7) 0.0048(7) 0.0003(8)
O2 0.0401(13) 0.0317(12) 0.062(2) -0.0085(10) 0.000 0.000
O1 0.0338(12) 0.0315(12) 0.068(2) 0.0060(10) 0.000 0.000
N5 0.0221(11) 0.0330(13) 0.0349(13) 0.0023(9) 0.000 0.000
O4 0.071(2) 0.0345(14) 0.066(2) 0.0129(13) 0.000 0.000
O3 0.0468(9) 0.0538(10) 0.0383(9) -0.0051(8) -0.0009(7) -0.0102(8)
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 0.13299(2) 0.20415(4) -0.2500 0.02056(12) Uani d S 1 Co
Cl1 0.15198(5) -0.01892(8) 0.2500 0.0308(2) Uani d S 1 Cl
N1 0.12397(15) 0.4104(2) -0.2500 0.0277(5) Uani d S 1 N
H1A 0.083(2) 0.4384(7) -0.339(3) 0.042 Uiso calc PR 0.50 H
H1B 0.1802(12) 0.4484(9) -0.274(5) 0.042 Uiso calc PR 0.50 H
H1C 0.104(2) 0.4405(9) -0.137(4) 0.042 Uiso calc PR 0.50 H
N2 0.22559(10) 0.2183(2) -0.0576(2) 0.0296(4) Uani d . 1 N
H2A 0.2135(6) 0.2816(15) 0.0094(17) 0.044 Uiso calc R 1 H
H2B 0.2740(8) 0.2317(17) -0.1037(7) 0.044 Uiso calc R 1 H
H2C 0.2270(8) 0.1473(13) -0.0002(17) 0.044 Uiso calc R 1 H
N4 0.14679(15) 0.0016(3) -0.2500 0.0261(5) Uani d S 1 N
N3 0.03941(11) 0.1861(2) -0.0622(3) 0.0309(4) Uani d . 1 N
H3A 0.0264(8) 0.2617(12) -0.0241(18) 0.046 Uiso calc R 1 H
H3B 0.0580(5) 0.1391(16) 0.0203(17) 0.046 Uiso calc R 1 H
H3C -0.0045(8) 0.1502(17) -0.1058(9) 0.046 Uiso calc R 1 H
O2 0.0802(2) -0.0705(2) -0.2500 0.0447(6) Uani d S 1 O
O1 0.22340(15) -0.0456(2) -0.2500 0.0445(6) Uani d S 1 O
N5 0.4111(2) -0.0010(3) -0.2500 0.0300(5) Uani d S 1 N
O4 0.4122(2) -0.1289(3) -0.2500 0.0569(7) Uani d S 1 O
O3 0.41064(11) 0.0644(2) -0.1024(2) 0.0463(4) Uani d . 1 O
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
0 0 6
0 0 -6
5 11 0
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
N3 Co1 N3 7 . 88.99(11) ?
N3 Co1 N4 7 . 89.18(7) ?
N3 Co1 N4 . . 89.18(7) ?
N3 Co1 N2 7 . 178.50(7) ?
N3 Co1 N2 . . 89.92(8) ?
N4 Co1 N2 . . 89.77(7) ?
N3 Co1 N2 7 7 89.92(8) ?
N3 Co1 N2 . 7 178.50(7) ?
N4 Co1 N2 . 7 89.77(7) ?
N2 Co1 N2 . 7 91.15(10) ?
N3 Co1 N1 7 . 92.34(7) ?
N3 Co1 N1 . . 92.34(7) ?
N4 Co1 N1 . . 177.86(9) ?
N2 Co1 N1 . . 88.74(7) ?
N2 Co1 N1 7 . 88.74(7) ?
Co1 N1 H1A . . 109.47(4) ?
Co1 N1 H1B . . 109.47(7) ?
H1A N1 H1B . . 109.5 ?
Co1 N1 H1C . . 109.47(2) ?
H1A N1 H1C . . 109.5 ?
H1B N1 H1C . . 109.5 ?
Co1 N2 H2A . . 109.47(5) ?
Co1 N2 H2B . . 109.47(5) ?
H2A N2 H2B . . 109.5 ?
Co1 N2 H2C . . 109.47(5) ?
H2A N2 H2C . . 109.5 ?
H2B N2 H2C . . 109.5 ?
O2 N4 O1 . . 123.1(3) ?
O2 N4 Co1 . . 119.2(2) yes
O1 N4 Co1 . . 117.8(2) yes
Co1 N3 H3A . . 109.47(5) ?
Co1 N3 H3B . . 109.47(5) ?
H3A N3 H3B . . 109.5 ?
Co1 N3 H3C . . 109.47(6) ?
H3A N3 H3C . . 109.5 ?
H3B N3 H3C . . 109.5 ?
O4 N5 O3 . . 120.24(13) yes
O4 N5 O3 . 7 120.24(13) ?
O3 N5 O3 . 7 119.5(3) yes
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 N3 7 1.959(2) ?
Co1 N3 . 1.959(2) yes
Co1 N4 . 1.960(3) yes
Co1 N2 . 1.969(2) yes
Co1 N2 7 1.969(2) ?
Co1 N1 . 1.989(3) yes
N1 H1A . 0.93(2) ?
N1 H1B . 0.93(2) ?
N1 H1C . 0.93(2) ?
N2 H2A . 0.802(12) ?
N2 H2B . 0.802(12) ?
N2 H2C . 0.802(12) ?
N4 O2 . 1.206(3) yes
N4 O1 . 1.222(3) yes
N3 H3A . 0.802(12) ?
N3 H3B . 0.802(12) ?
N3 H3C . 0.802(12) ?
N5 O4 . 1.231(3) yes
N5 O3 . 1.249(2) yes
N5 O3 7 1.249(2) ?