#------------------------------------------------------------------------------
#$Date: 2016-01-09 11:17:46 +0100 (Sat 09 de Jan de 2016) $
#$Revision: 173735 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/30/7223037.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7223037
loop_
_publ_author_name
'Zakharov, B. A.'
'Marchuk, A. S.'
'Boldyreva, E. V.'
_publ_section_title
;
 A single-crystal to single-crystal phase transition in [Co(NH3)5NO2]Br2at
 high pressure: a step towards understanding linkage photo-isomerisation
;
_journal_issue                   46
_journal_name_full               CrystEngComm
_journal_page_first              8812
_journal_paper_doi               10.1039/C5CE01820J
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'Co H15 N6 O2, 2(Br)'
_chemical_formula_sum            'Br2 Co H15 N6 O2'
_chemical_formula_weight         349.93
_chemical_name_common            nitro-pentaammine-Co(III)-dibromide
_chemical_name_systematic        nitro-pentaammine-Co(III)-dibromide
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-09-10 deposited with the CCDC.
2015-10-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.604(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6807(6)
_cell_length_b                   8.8299(8)
_cell_length_c                   10.9759(5)
_cell_measurement_reflns_used    1571
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.4360
_cell_measurement_theta_min      2.7960
_cell_volume                     1031.79(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics    'Mercury (Macrae et al., 2006)'
_computing_publication_material  'enCIFer (Allen et al., 2004)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_pressure         100
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 10.3457
_diffrn_measured_fraction_theta_full 0.587
_diffrn_measured_fraction_theta_max 0.571
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       ω-scan
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_laue_measured_fraction_full 0.587
_diffrn_reflns_laue_measured_fraction_max 0.571
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2634
_diffrn_reflns_point_group_measured_fraction_full 0.587
_diffrn_reflns_point_group_measured_fraction_max 0.571
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         2.997
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    9.382
_exptl_absorpt_correction_T_max  0.302
_exptl_absorpt_correction_T_min  0.233
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'Absorb-7 (Angel, 2013)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.253
_exptl_crystal_description       block
_exptl_crystal_F_000             680
_exptl_crystal_preparation       'mounted in DAC'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     52
_refine_ls_number_reflns         605
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0286
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0233P)²+1.1579P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0621
_refine_ls_wR_factor_ref         0.0677
_reflns_Friedel_coverage         0.000
_reflns_number_gt                532
_reflns_number_total             605
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5ce01820j3.cif
_cod_data_source_block           000GPa
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Gaussian' changed to
'gaussian' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 7223037--7223049.cif.
;
_cod_database_code               7223037
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_res_file
;

    _0.00GPa.res created by SHELXL-2014/7

TITL 0.00
CELL  0.71073 10.68070  8.82990 10.97590 90.00000 94.60400 90.00000
ZERR 4  0.00060  0.00080  0.00050  0.00000  0.00500  0.00000
LATT 7
SYMM -X, Y, -Z+ 0.50000
SFAC BR CO H N O
UNIT 8 4 60 24 8
TEMP 22
L.S. 10
SHEL 50 0.8
FMAP 2
PLAN 10
ACTA
CONF
BOND
EQIV $1 1/2-X,-1/2+Y,1/2-Z
EQIV $2 X,1-Y,-1/2+Z
EQIV $3 1/2-X,1/2-Y,1-Z
EQIV $4 -1/2+X,-1/2+Y,Z
EQIV $5 -X,1-Y,1-Z
EQIV $6 -1/2+X,1/2-Y,-1/2+Z
HTAB N1 O1_$1
HTAB N1 BR1_$2
HTAB N1 BR1
HTAB N2 BR1_$3
HTAB N2 BR1_$4
HTAB N2 BR1
HTAB N2 BR1_$5
HTAB N3 BR1_$4
HTAB N3 BR1_$6
BOND $H
WGHT    0.023300    1.157900
FVAR       2.18121
BR1   1    0.292190    0.514935    0.489945    11.00000    0.03254    0.03497 =
         0.02946    0.00056    0.00341   -0.00269
CO1   2    0.000000    0.288097    0.250000    10.50000    0.02380    0.02122 =
         0.01766    0.00000    0.00145    0.00000
N1    4    0.182678    0.289256    0.250220    11.00000    0.02635    0.03463 =
         0.02884   -0.00439    0.00429    0.00028
AFIX  33
H1A   3    0.210868    0.194404    0.250254    11.00000   -1.50000
H1B   3    0.204855    0.336946    0.183832    11.00000   -1.50000
H1C   3    0.215645    0.336946    0.316675    11.00000   -1.50000
AFIX   0
N2    4    0.012656    0.293982    0.428891    11.00000    0.03613    0.02543 =
         0.02357   -0.00189    0.00197   -0.00346
AFIX  33
H2A   3    0.014718    0.199877    0.458032    11.00000   -1.50000
H2B   3    0.082597    0.342371    0.455740    11.00000   -1.50000
H2C   3   -0.053593    0.342371    0.454218    11.00000   -1.50000
AFIX   0
N3    4    0.000000    0.063739    0.250000    10.50000    0.03419    0.03646 =
         0.02343    0.00000    0.00019    0.00000
AFIX  33
H3A   3    0.078570    0.030141    0.250095    10.50000   -1.50000
H3B   3   -0.033891    0.030141    0.316374    10.50000   -1.50000
H3C   3   -0.044679    0.030141    0.183531    10.50000   -1.50000
AFIX   0
N4    4    0.000000    0.504972    0.250000    10.50000    0.03518    0.02330 =
         0.02564    0.00000    0.00306    0.00000
O1    5    0.071137    0.576552    0.188084    11.00000    0.06847    0.03460 =
         0.06192    0.00817    0.02481   -0.00562
HKLF 4

REM  0.00
REM R1 =  0.0286 for     532 Fo > 4sig(Fo)  and  0.0349 for all     605 data
REM     52 parameters refined using      0 restraints

END

WGHT      0.0234      1.1189

REM Highest difference peak  0.403,  deepest hole -0.363,  1-sigma level  0.089
Q1    1   0.0000  0.7480  0.2500  10.50000  0.05    0.40
Q2    1   0.0233  0.2935  0.3528  11.00000  0.05    0.38
Q3    1   0.2646  0.4360  0.5326  11.00000  0.05    0.36
Q4    1   0.2146  0.2659  0.3085  11.00000  0.05    0.35
Q5    1   0.3558  0.3553  0.4262  11.00000  0.05    0.35
Q6    1   0.2056  0.3506  0.5602  11.00000  0.05    0.33
Q7    1  -0.0667  0.2255  0.3919  11.00000  0.05    0.28
Q8    1  -0.1022  0.1834  0.4123  11.00000  0.05    0.28
Q9    1   0.1178  0.3453  0.2683  11.00000  0.05    0.27
Q10   1  -0.0384  0.1925  0.2995  11.00000  0.05    0.27
;
_shelx_res_checksum              14368
loop_
_space_group_symop_operation_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_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Br1 Br 0.29219(5) 0.51493(7) 0.48994(4) 0.0323(2) Uani 1 1 d . . .
Co1 Co 0.0000 0.28810(12) 0.2500 0.0209(3) Uani 1 2 d S T P
N1 N 0.1827(3) 0.2893(5) 0.2502(3) 0.0298(11) Uani 1 1 d . . .
H1A H 0.2109 0.1944 0.2503 0.045 Uiso 1 1 calc R U .
H1B H 0.2049 0.3369 0.1838 0.045 Uiso 1 1 calc R U .
H1C H 0.2156 0.3369 0.3167 0.045 Uiso 1 1 calc R U .
N2 N 0.0127(4) 0.2940(5) 0.4289(3) 0.0284(11) Uani 1 1 d . . .
H2A H 0.0147 0.1999 0.4580 0.043 Uiso 1 1 calc R U .
H2B H 0.0826 0.3424 0.4557 0.043 Uiso 1 1 calc R U .
H2C H -0.0536 0.3424 0.4542 0.043 Uiso 1 1 calc R U .
N3 N 0.0000 0.0637(8) 0.2500 0.0315(16) Uani 1 2 d S T P
H3A H 0.0786 0.0301 0.2501 0.047 Uiso 0.5 1 calc R U P
H3B H -0.0339 0.0301 0.3164 0.047 Uiso 0.5 1 calc R U P
H3C H -0.0447 0.0301 0.1835 0.047 Uiso 0.5 1 calc R U P
N4 N 0.0000 0.5050(9) 0.2500 0.0280(19) Uani 1 2 d S T P
O1 O 0.0711(4) 0.5766(6) 0.1881(4) 0.0539(15) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Br1 0.0325(4) 0.0350(7) 0.0295(3) 0.0006(2) 0.0034(3) -0.0027(2)
Co1 0.0238(6) 0.0212(10) 0.0177(5) 0.000 0.0014(4) 0.000
N1 0.026(3) 0.035(5) 0.029(2) -0.0044(18) 0.0043(19) 0.0003(19)
N2 0.036(3) 0.025(5) 0.024(2) -0.0019(16) 0.002(2) -0.0035(19)
N3 0.034(4) 0.036(7) 0.023(3) 0.000 0.000(3) 0.000
N4 0.035(5) 0.023(8) 0.026(4) 0.000 0.003(4) 0.000
O1 0.068(3) 0.035(5) 0.062(3) 0.008(2) 0.025(2) -0.006(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Br Br -0.2901 2.4595 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N4 Co1 N1 89.70(13) . 2
N4 Co1 N1 89.70(13) . .
N1 Co1 N1 179.4(3) 2 .
N4 Co1 N2 88.48(13) . .
N1 Co1 N2 89.41(16) 2 .
N1 Co1 N2 90.58(16) . .
N4 Co1 N2 88.48(13) . 2
N1 Co1 N2 90.58(16) 2 2
N1 Co1 N2 89.41(16) . 2
N2 Co1 N2 177.0(3) . 2
N4 Co1 N3 180.0 . .
N1 Co1 N3 90.30(13) 2 .
N1 Co1 N3 90.30(13) . .
N2 Co1 N3 91.52(13) . .
N2 Co1 N3 91.52(13) 2 .
Co1 N1 H1A 109.5 . .
Co1 N1 H1B 109.5 . .
H1A N1 H1B 109.5 . .
Co1 N1 H1C 109.5 . .
H1A N1 H1C 109.5 . .
H1B N1 H1C 109.5 . .
Co1 N2 H2A 109.5 . .
Co1 N2 H2B 109.5 . .
H2A N2 H2B 109.5 . .
Co1 N2 H2C 109.5 . .
H2A N2 H2C 109.5 . .
H2B N2 H2C 109.5 . .
Co1 N3 H3A 109.5 . .
Co1 N3 H3B 109.5 . .
H3A N3 H3B 109.5 . .
Co1 N3 H3C 109.5 . .
H3A N3 H3C 109.5 . .
H3B N3 H3C 109.5 . .
O1 N4 O1 118.4(10) . 2
O1 N4 Co1 120.8(5) . .
O1 N4 Co1 120.8(5) 2 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N4 1.915(8) .
Co1 N1 1.951(4) 2
Co1 N1 1.951(4) .
Co1 N2 1.958(3) .
Co1 N2 1.958(3) 2
Co1 N3 1.981(7) .
N1 H1A 0.8900 .
N1 H1B 0.8900 .
N1 H1C 0.8900 .
N2 H2A 0.8900 .
N2 H2B 0.8900 .
N2 H2C 0.8900 .
N3 H3A 0.8900 .
N3 H3B 0.8900 .
N3 H3C 0.8900 .
N4 O1 1.233(6) .
N4 O1 1.234(6) 2
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A O1 0.89 2.59 3.258(6) 132.5 4_545
N1 H1B Br1 0.89 2.73 3.613(4) 175.3 6_565
N1 H1C Br1 0.89 2.55 3.430(4) 170.0 .
N2 H2A Br1 0.89 2.83 3.504(4) 134.1 7_556
N2 H2A Br1 0.89 2.93 3.510(4) 124.5 3_445
N2 H2B Br1 0.89 2.71 3.584(4) 168.0 .
N2 H2C Br1 0.89 2.95 3.835(4) 172.5 5_566
N3 H3B Br1 0.89 2.77 3.6037(10) 156.7 3_445
N3 H3C Br1 0.89 2.67 3.5411(14) 167.3 8_455
