#------------------------------------------------------------------------------
#$Date: 2016-01-09 12:17:46 +0200 (Sat, 09 Jan 2016) $
#$Revision: 173735 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/30/7223038.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_7223038
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                 94.589(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6575(5)
_cell_length_b                   8.7649(9)
_cell_length_c                   10.9567(5)
_cell_measurement_reflns_used    1795
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.7820
_cell_measurement_theta_min      2.7820
_cell_volume                     1020.21(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         150000
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 10.3457
_diffrn_measured_fraction_theta_full 0.577
_diffrn_measured_fraction_theta_max 0.560
_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  0.0562
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_laue_measured_fraction_full 0.577
_diffrn_reflns_laue_measured_fraction_max 0.560
_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            2719
_diffrn_reflns_point_group_measured_fraction_full 0.577
_diffrn_reflns_point_group_measured_fraction_max 0.560
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.357
_diffrn_reflns_theta_min         3.013
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    9.489
_exptl_absorpt_correction_T_max  0.300
_exptl_absorpt_correction_T_min  0.231
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'Absorb-7 (Angel, 2013)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.278
_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         0.498
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     52
_refine_ls_number_reflns         588
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0271
_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)+(0.0190P)²+1.1318P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0557
_refine_ls_wR_factor_ref         0.0578
_reflns_Friedel_coverage         0.000
_reflns_number_gt                541
_reflns_number_total             588
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5ce01820j3.cif
_cod_data_source_block           015GPa
_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               7223038
_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
;

    _0.15GPa.res created by SHELXL-2014/7

TITL 0.15
CELL  0.71073 10.65750  8.76490 10.95670 90.00000 94.58900 90.00000
ZERR 4  0.00050  0.00090  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    0.019000    1.131800
FVAR       2.14680
BR1   1    0.291890    0.515204    0.490497    11.00000    0.03167    0.03249 =
         0.02820    0.00058    0.00224   -0.00252
CO1   2    0.000000    0.288248    0.250000    10.50000    0.02218    0.01982 =
         0.01675    0.00000    0.00111    0.00000
N1    4    0.183317    0.288711    0.250560    11.00000    0.02623    0.02507 =
         0.03177   -0.00580    0.00019   -0.00054
AFIX  33
H1A   3    0.211323    0.193047    0.250645    11.00000   -1.50000
H1B   3    0.205819    0.336648    0.184108    11.00000   -1.50000
H1C   3    0.216338    0.336648    0.317180    11.00000   -1.50000
AFIX   0
N2    4    0.011724    0.294147    0.429293    11.00000    0.03192    0.03072 =
         0.01760    0.00072    0.00669   -0.00039
AFIX  33
H2A   3    0.013632    0.199340    0.458470    11.00000   -1.50000
H2B   3    0.081699    0.342891    0.456524    11.00000   -1.50000
H2C   3   -0.054833    0.342891    0.454334    11.00000   -1.50000
AFIX   0
N3    4    0.000000    0.061458    0.250000    10.50000    0.04038    0.02769 =
         0.02512    0.00000   -0.00068    0.00000
AFIX  33
H3A   3   -0.078753    0.027611    0.249760    10.50000   -1.50000
H3B   3    0.034117    0.027611    0.183584    10.50000   -1.50000
H3C   3    0.044636    0.027611    0.316656    10.50000   -1.50000
AFIX   0
N4    4    0.000000    0.506149    0.250000    10.50000    0.03237    0.02592 =
         0.02591    0.00000    0.00160    0.00000
O1    5    0.071766    0.579506    0.188167    11.00000    0.06426    0.02870 =
         0.06340    0.00746    0.02100   -0.00725
HKLF 4

REM  0.15
REM R1 =  0.0271 for     541 Fo > 4sig(Fo)  and  0.0312 for all     588 data
REM     52 parameters refined using      0 restraints

END

WGHT      0.0190      1.1318

REM Highest difference peak  0.498,  deepest hole -0.301,  1-sigma level  0.083
Q1    1   0.0000  0.7451  0.2500  10.50000  0.05    0.50
Q2    1   0.1260  0.2924  0.2092  11.00000  0.05    0.27
Q3    1   0.1978  0.6416  0.5033  11.00000  0.05    0.27
Q4    1  -0.1862  0.0132  0.2766  11.00000  0.05    0.27
Q5    1  -0.0378  0.2538  0.3638  11.00000  0.05    0.26
Q6    1   0.2686  0.4678  0.2018  11.00000  0.05    0.25
Q7    1   0.0961  0.1415  0.6055  11.00000  0.05    0.25
Q8    1   0.2917  0.4028  0.1141  11.00000  0.05    0.25
Q9    1   0.1631  0.5090  0.3491  11.00000  0.05    0.24
Q10   1   0.1118  0.2442  0.1404  11.00000  0.05    0.23
;
_shelx_res_checksum              39520
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 0.29189(4) 0.51520(6) 0.49050(4) 0.0308(2) Uani 1 1 d . . .
Co1 Co 0.0000 0.28825(10) 0.2500 0.0196(2) Uani 1 2 d S T P
N1 N 0.1833(3) 0.2887(5) 0.2506(3) 0.0278(9) Uani 1 1 d . . .
H1A H 0.2113 0.1930 0.2506 0.042 Uiso 1 1 calc R U .
H1B H 0.2058 0.3366 0.1841 0.042 Uiso 1 1 calc R U .
H1C H 0.2163 0.3366 0.3172 0.042 Uiso 1 1 calc R U .
N2 N 0.0117(3) 0.2941(4) 0.4293(3) 0.0265(9) Uani 1 1 d . . .
H2A H 0.0136 0.1993 0.4585 0.040 Uiso 1 1 calc R U .
H2B H 0.0817 0.3429 0.4565 0.040 Uiso 1 1 calc R U .
H2C H -0.0548 0.3429 0.4543 0.040 Uiso 1 1 calc R U .
N3 N 0.0000 0.0615(7) 0.2500 0.0312(14) Uani 1 2 d S T P
H3A H -0.0788 0.0276 0.2498 0.047 Uiso 0.5 1 calc R U P
H3B H 0.0341 0.0276 0.1836 0.047 Uiso 0.5 1 calc R U P
H3C H 0.0446 0.0276 0.3167 0.047 Uiso 0.5 1 calc R U P
N4 N 0.0000 0.5061(8) 0.2500 0.0281(16) Uani 1 2 d S T P
O1 O 0.0718(3) 0.5795(6) 0.1882(3) 0.0513(13) 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 0.0317(3) 0.0325(6) 0.0282(3) 0.00058(18) 0.0022(2) -0.00252(19)
Co1 0.0222(5) 0.0198(8) 0.0168(4) 0.000 0.0011(4) 0.000
N1 0.026(2) 0.025(4) 0.032(2) -0.0058(16) 0.0002(17) -0.0005(16)
N2 0.032(2) 0.031(4) 0.018(2) 0.0007(14) 0.0067(17) -0.0004(16)
N3 0.040(4) 0.028(6) 0.025(3) 0.000 -0.001(3) 0.000
N4 0.032(4) 0.026(7) 0.026(4) 0.000 0.002(3) 0.000
O1 0.064(3) 0.029(5) 0.063(3) 0.007(2) 0.021(2) -0.007(2)
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 89.88(12) . .
N4 Co1 N1 89.88(12) . 2
N1 Co1 N1 179.8(2) . 2
N4 Co1 N2 88.49(12) . 2
N1 Co1 N2 89.23(14) . 2
N1 Co1 N2 90.76(14) 2 2
N4 Co1 N2 88.49(12) . .
N1 Co1 N2 90.76(14) . .
N1 Co1 N2 89.23(14) 2 .
N2 Co1 N2 177.0(2) 2 .
N4 Co1 N3 180.0 . .
N1 Co1 N3 90.12(12) . .
N1 Co1 N3 90.12(12) 2 .
N2 Co1 N3 91.51(12) 2 .
N2 Co1 N3 91.51(12) . .
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 117.6(9) 2 .
O1 N4 Co1 121.2(4) 2 .
O1 N4 Co1 121.2(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N4 1.910(7) .
Co1 N1 1.953(3) .
Co1 N1 1.953(3) 2
Co1 N2 1.959(3) 2
Co1 N2 1.959(3) .
Co1 N3 1.988(6) .
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 1.241(5) 2
N4 O1 1.241(5) .
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 2.56 3.216(5) 131.5 4_545
N1 H1B Br1 0.89 2.71 3.597(4) 175.7 6_565
N1 H1C Br1 0.89 2.54 3.421(3) 169.9 .
N2 H2A Br1 0.89 2.82 3.494(4) 133.5 7_556
N2 H2A Br1 0.89 2.91 3.488(4) 124.5 3_445
N2 H2B Br1 0.89 2.70 3.578(3) 167.8 .
N2 H2C Br1 0.89 2.92 3.807(4) 172.6 5_566
N3 H3A Br1 0.89 3.07 3.6003(9) 119.8 3_445
N3 H3A Br1 0.89 3.08 3.5279(12) 113.3 8_455
