#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/61/2006159.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_2006159
loop_
_publ_author_name
'Boldyreva, Elena V.'
'Kivikoski, Jussi'
'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_paper_doi               10.1107/S0108270196014217
_journal_volume                  53
_journal_year                    1997
_chemical_formula_iupac          '[Co (N H3)5 N O2] (N O3) Cl'
_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'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.726(5)
_cell_length_b                   9.646(7)
_cell_length_c                   7.219(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    150
_cell_measurement_theta_max      23.945
_cell_measurement_theta_min      20.42
_cell_volume                     1025.4(9)
_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       'ω/2θ 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    0.0297
_diffrn_reflns_limit_h_max       19
_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            2723
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         3.48
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.95
_exptl_absorpt_correction_T_max  0.677
_exptl_absorpt_correction_T_min  0.544
_exptl_absorpt_correction_type
;
 'empirical, 36 psi scans of 6 reflections (North, Phillips & Mathews, 1968)'
;
_exptl_crystal_colour            ruby
_exptl_crystal_density_diffrn    1.863
_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         0.425
_refine_diff_density_min         -0.350
_refine_ls_extinction_coef       0.0060(7)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.042
_refine_ls_goodness_of_fit_obs   1.089
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     83
_refine_ls_number_reflns         1333
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_restrained_S_obs      1.089
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_obs          .0233
_refine_ls_shift/esd_max         0.007
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0260P)²+0.5638P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0619
_refine_ls_wR_factor_obs         .0570
_reflns_number_observed          1091
_reflns_number_total             1335
_reflns_observed_criterion       >2.0\s(I)
_cod_data_source_file            sk1070.cif
_cod_data_source_block           at_150K
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0260P)^2^+0.5638P] 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^)+(0.0260P)^2^+0.5638P] 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        1025.4(8)
_cod_original_formula_sum        'H15 O5 N7 Cl Co'
_cod_database_code               2006159
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 .0111(2) .0132(2) .0155(2) -.00014(11) .000 .000
Cl1 .0161(3) .0195(3) .0230(3) .0017(2) .000 .000
N1 .0154(10) .0163(10) .0234(11) .0004(8) .000 .000
N4 .0120(10) .0248(11) .0121(10) -.0003(8) .000 .000
N2 .0174(7) .0199(7) .0205(8) -.0021(5) -.0005(6) .0003(6)
O1 .0208(10) .0223(10) .0395(12) .0039(8) .000 .000
N3 .0171(7) .0198(7) .0240(8) -.0007(6) .0035(6) .0005(7)
O2 .0258(10) .0208(10) .0386(12) -.0058(8) .000 .000
N5 .0121(10) .0219(11) .0237(11) .0028(8) .000 .000
O4 .0441(13) .0218(10) .0435(13) .0080(9) .000 .000
O3 .0254(7) .0330(7) .0245(7) -.0032(6) -.0004(6) -.0062(6)
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_disorder_group
_atom_site_type_symbol
Co1 .13352(2) .20341(3) -.2500 .01327(11) Uani d S 1 . Co
Cl1 .15142(4) -.02121(6) .2500 .0195(2) Uani d S 1 . Cl
N1 .12440(14) .4092(2) -.2500 .0184(4) Uani d S 1 . N
H1A .1039(19) .4396(8) -.366(3) .028 Uiso calc PR .50 . H
H1B .1818(11) .4476(8) -.226(4) .028 Uiso calc PR .50 . H
H1C .083(2) .4374(6) -.158(3) .028 Uiso calc PR .50 . H
N4 .14829(14) .0015(2) -.2500 .0163(4) Uani d S 1 . N
N2 .22605(10) .21811(15) -.0541(2) .0192(3) Uani d . 1 . N
H2A .2188(6) .2891(12) .0022(15) .029 Uiso calc R 1 . H
H2B .2758(7) .2177(15) -.1000(7) .029 Uiso calc R 1 . H
H2C .2213(6) .1535(12) .0156(15) .029 Uiso calc R 1 . H
O1 .22563(13) -.0450(2) -.2500 .0276(5) Uani d S 1 . O
N3 .03976(10) .1849(2) -.0592(2) .0203(3) Uani d . 1 . N
H3A .0278(7) .2626(11) -.0157(15) .030 Uiso calc R 1 . H
H3B .0585(4) .1334(14) .0249(15) .030 Uiso calc R 1 . H
H3C -.0068(7) .1509(14) -.1058(8) .030 Uiso calc R 1 . H
O2 .08081(13) -.0713(2) -.2500 .0284(5) Uani d S 1 . O
N5 .41219(14) .0025(2) -.2500 .0193(5) Uani d S 1 . N
O4 .4150(2) -.1255(2) -.2500 .0365(5) Uani d S 1 . O
O3 .41137(9) .06827(15) -.0999(2) .0276(3) 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 89.37(10) ?
N3 Co1 N4 . . 89.30(6) ?
N3 Co1 N4 7 . 89.30(6) ?
N3 Co1 N2 . . 89.39(7) ?
N3 Co1 N2 7 . 178.42(6) ?
N4 Co1 N2 . . 89.70(6) ?
N3 Co1 N2 . 7 178.42(6) ?
N3 Co1 N2 7 7 89.39(7) ?
N4 Co1 N2 . 7 89.70(6) ?
N2 Co1 N2 . 7 91.84(9) ?
N3 Co1 N1 . . 92.48(6) ?
N3 Co1 N1 7 . 92.48(6) ?
N4 Co1 N1 . . 177.50(9) ?
N2 Co1 N1 . . 88.56(6) ?
N2 Co1 N1 7 . 88.56(6) ?
Co1 N1 H1A . . 109.47(2) ?
Co1 N1 H1B . . 109.47(6) ?
H1A N1 H1B . . 109.5 ?
Co1 N1 H1C . . 109.47(4) ?
H1A N1 H1C . . 109.5 ?
H1B N1 H1C . . 109.5 ?
O2 N4 O1 . . 123.3(2) yes
O2 N4 Co1 . . 118.9(2) yes
O1 N4 Co1 . . 117.8(2) yes
Co1 N2 H2A . . 109.47(4) ?
Co1 N2 H2B . . 109.47(5) ?
H2A N2 H2B . . 109.5 ?
Co1 N2 H2C . . 109.47(4) ?
H2A N2 H2C . . 109.5 ?
H2B N2 H2C . . 109.5 ?
Co1 N3 H3A . . 109.47(4) ?
Co1 N3 H3B . . 109.47(5) ?
H3A N3 H3B . . 109.5 ?
Co1 N3 H3C . . 109.47(5) ?
H3A N3 H3C . . 109.5 ?
H3B N3 H3C . . 109.5 ?
O4 N5 O3 . . 120.35(11) yes
O4 N5 O3 . 7 120.35(11) ?
O3 N5 O3 . yes 119.3(2) ?
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 . 1.958(2) yes
Co1 N3 7 1.958(2) ?
Co1 N4 . 1.960(2) yes
Co1 N2 . 1.9691(15) yes
Co1 N2 7 1.9691(15) ?
Co1 N1 . 1.989(2) yes
N1 H1A . .94(2) ?
N1 H1B . .94(2) ?
N1 H1C . .94(2) ?
N4 O2 . 1.217(3) yes
N4 O1 . 1.224(3) yes
N2 H2A . .804(11) ?
N2 H2B . .804(11) ?
N2 H2C . .804(11) ?
N3 H3A . .832(11) ?
N3 H3B . .832(11) ?
N3 H3C . .832(11) ?
N5 O4 . 1.235(3) yes
N5 O3 . 1.256(2) yes
N5 O3 7 1.256(2) ?
