#------------------------------------------------------------------------------
#$Date: 2016-01-09 12:17:46 +0200 (Sat, 09 Jan 2016) $
#$Revision: 173735 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/30/7223049.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_7223049
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      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7595(5)
_cell_length_b                   7.4390(6)
_cell_length_c                   10.0890(4)
_cell_measurement_reflns_used    1696
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.5680
_cell_measurement_theta_min      2.7820
_cell_volume                     807.52(8)
_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)'
_computing_structure_solution    'SIR2004 (Burla et al., 2005)'
_diffrn_ambient_pressure         6850000
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 10.3457
_diffrn_measured_fraction_theta_full 0.736
_diffrn_measured_fraction_theta_max 0.716
_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  0.0624
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_laue_measured_fraction_full 0.736
_diffrn_reflns_laue_measured_fraction_max 0.716
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2137
_diffrn_reflns_point_group_measured_fraction_full 0.736
_diffrn_reflns_point_group_measured_fraction_max 0.716
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.366
_diffrn_reflns_theta_min         3.329
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    11.988
_exptl_absorpt_correction_T_max  0.265
_exptl_absorpt_correction_T_min  0.202
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'Absorb-7 (Angel, 2013)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.878
_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         0.641
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     36
_refine_ls_number_reflns         333
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0270
_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)+(0.0351P)²+2.0046P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0622
_refine_ls_wR_factor_ref         0.0637
_reflns_Friedel_coverage         0.000
_reflns_number_gt                310
_reflns_number_total             333
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5ce01820j3.cif
_cod_data_source_block           685GPa_HP_phase
_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               7223049
_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
;

    E:\_work_current\dif\_mypublications\2015_Co_dibromide\rerefine\new.res created by SHELXL-2014/7

TITL 6.85
CELL  0.71073 10.75950  7.43900 10.08900 90.00000 90.00000 90.00000
ZERR 4  0.00050  0.00060  0.00040  0.00000  0.00000  0.00000
LATT 7
SYMM -X, -Y, Z+ 0.50000
SYMM X, -Y, -Z
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
DELU
SIMU
ACTA
CONF
EQIV $1 -X,-Y,2-Z
EQIV $2 -0.5+X,0.5+Y,1.5-Z
HTAB N1 BR1
HTAB N2 BR1_$1
HTAB N3 BR1_$2
BOND
BOND $H
WGHT    0.035100    2.004600
FVAR       2.48679
BR1   1    0.289165    0.000000    1.000000    10.50000    0.01814    0.01206 =
         0.01517   -0.00084    0.00000    0.00000
CO1   2    0.000000    0.205590    0.750000    10.25000    0.00917    0.00647 =
         0.01098    0.00000    0.00000    0.00000
N3    4    0.000000    0.467569    0.750000    10.25000    0.01802    0.01155 =
         0.01339    0.00000    0.00000    0.00000
AFIX  33
H3A   3   -0.077987    0.507449    0.750000    10.25000   -1.50000
H3B   3    0.038993    0.507449    0.822027    10.25000   -1.50000
H3C   3    0.038993    0.507449    0.677973    10.25000   -1.50000
AFIX   0
N2    4    0.000000    0.198484    0.942395    10.50000    0.01177    0.01109 =
         0.01250    0.00262    0.00000    0.00000
AFIX  33
H2C   3    0.000000    0.310154    0.974053    10.50000   -1.50000
H2B   3   -0.067539    0.141021    0.970657    10.50000   -1.50000
H2A   3    0.067539    0.141021    0.970657    10.50000   -1.50000
AFIX   0
N4    4    0.000000   -0.050337    0.750000    10.25000    0.00820    0.01163 =
         0.00836    0.00000    0.00000    0.00000
N1    4    0.177656    0.209846    0.750000    10.50000    0.00973    0.01270 =
         0.01492    0.00000    0.00000   -0.00099
AFIX  33
H1C   3    0.203934    0.323288    0.750000    10.50000   -1.50000
H1B   3    0.205871    0.154116    0.822027    10.50000   -1.50000
H1A   3    0.205871    0.154115    0.677973    10.50000   -1.50000
AFIX   0
O1    5   -0.096499   -0.138865    0.750000    10.50000    0.01733    0.01115 =
         0.12502    0.00000    0.00000   -0.00628
HKLF      4

REM  6.85
REM R1 =  0.0270 for     310 Fo > 4sig(Fo)  and  0.0290 for all     333 data
REM     36 parameters refined using     42 restraints

END

WGHT      0.0351      2.0767

REM Highest difference peak  0.641,  deepest hole -0.522,  1-sigma level  0.128
Q1    1   0.1941  0.0929  0.7500  10.50000  0.05    0.64
Q2    1  -0.1822 -0.0928  0.7500  10.50000  0.05    0.53
Q3    1  -0.0616 -0.1669  0.6898  11.00000  0.05    0.52
Q4    1   0.0000  0.4167  1.0185  10.50000  0.05    0.45
Q5    1   0.0000  0.3053  0.6701  10.50000  0.05    0.44
Q6    1  -0.1669  0.5032  0.7500  10.50000  0.05    0.37
Q7    1   0.2015  0.2724  0.6793  11.00000  0.05    0.35
Q8    1   0.0000  0.0801  0.6679  10.50000  0.05    0.34
Q9    1   0.0909  0.2851  1.0168  11.00000  0.05    0.31
Q10   1   0.2587  0.4714  0.7500  10.50000  0.05    0.31
;
_shelx_res_checksum              62517
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, 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'
'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, y, z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -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 0.28917(5) 0.0000 1.0000 0.0151(3) Uani 1 2 d S T P
Co1 Co 0.0000 0.20559(15) 0.7500 0.0089(3) Uani 1 4 d S TU P
N3 N 0.0000 0.4676(10) 0.7500 0.0143(14) Uani 1 4 d S TU P
H3A H -0.0780 0.5074 0.7500 0.021 Uiso 0.5 2 calc R U P
H3B H 0.0390 0.5074 0.8220 0.021 Uiso 0.25 1 calc R U P
H3C H 0.0390 0.5074 0.6780 0.021 Uiso 0.25 1 calc R U P
N2 N 0.0000 0.1985(7) 0.9424(4) 0.0118(10) Uani 1 2 d S TU P
H2C H 0.0000 0.3102 0.9741 0.018 Uiso 1 2 calc R U P
H2B H -0.0675 0.1410 0.9707 0.018 Uiso 0.5 1 calc R U P
H2A H 0.0675 0.1410 0.9707 0.018 Uiso 0.5 1 calc R U P
N4 N 0.0000 -0.0503(10) 0.7500 0.0094(13) Uani 1 4 d S TU P
N1 N 0.1777(4) 0.2098(7) 0.7500 0.0125(10) Uani 1 2 d S TU P
H1C H 0.2039 0.3233 0.7500 0.019 Uiso 1 2 calc R U P
H1B H 0.2059 0.1541 0.8220 0.019 Uiso 0.5 1 calc R U P
H1A H 0.2059 0.1541 0.6780 0.019 Uiso 0.5 1 calc R U P
O1 O -0.0965(4) -0.1389(8) 0.7500 0.0512(16) Uani 1 2 d S TU P
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 0.0181(4) 0.0121(6) 0.0152(4) -0.00084(18) 0.000 0.000
Co1 0.0092(5) 0.0065(8) 0.0110(5) 0.000 0.000 0.000
N3 0.018(3) 0.012(4) 0.013(3) 0.000 0.000 0.000
N2 0.012(2) 0.011(3) 0.012(2) 0.0026(16) 0.000 0.000
N4 0.008(3) 0.012(4) 0.008(3) 0.000 0.000 0.000
N1 0.010(2) 0.013(3) 0.015(2) 0.000 0.000 -0.0010(17)
O1 0.017(2) 0.011(4) 0.125(5) 0.000 0.000 -0.0063(18)
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 90.95(16) . .
N4 Co1 N1 90.95(16) . 11
N1 Co1 N1 178.1(3) . 11
N4 Co1 N2 88.44(15) . .
N1 Co1 N2 90.026(5) . .
N1 Co1 N2 90.026(5) 11 .
N4 Co1 N2 88.44(15) . 10_557
N1 Co1 N2 90.026(5) . 10_557
N1 Co1 N2 90.026(5) 11 10_557
N2 Co1 N2 176.9(3) . 10_557
N4 Co1 N3 180.0 . .
N1 Co1 N3 89.05(16) . .
N1 Co1 N3 89.05(16) 11 .
N2 Co1 N3 91.56(15) . .
N2 Co1 N3 91.56(15) 10_557 .
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 . .
Co1 N2 H2C 109.5 . .
Co1 N2 H2B 109.5 . .
H2C N2 H2B 109.5 . .
Co1 N2 H2A 109.5 . .
H2C N2 H2A 109.5 . .
H2B N2 H2A 109.5 . .
O1 N4 O1 115.2(8) . 11
O1 N4 Co1 122.4(4) . .
O1 N4 Co1 122.4(4) 11 .
Co1 N1 H1C 109.5 . .
Co1 N1 H1B 109.5 . .
H1C N1 H1B 109.5 . .
Co1 N1 H1A 109.5 . .
H1C N1 H1A 109.5 . .
H1B N1 H1A 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N4 1.904(7) .
Co1 N1 1.912(4) .
Co1 N1 1.912(4) 11
Co1 N2 1.942(4) .
Co1 N2 1.942(4) 10_557
Co1 N3 1.949(7) .
N3 H3A 0.8900 .
N3 H3B 0.8900 .
N3 H3C 0.8900 .
N2 H2C 0.8900 .
N2 H2B 0.8900 .
N2 H2A 0.8900 .
N4 O1 1.230(6) .
N4 O1 1.230(6) 11
N1 H1C 0.8900 .
N1 H1B 0.8900 .
N1 H1A 0.8900 .
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 H1B Br1 0.89 2.31 3.200(3) 176.1 .
N2 H2B Br1 0.89 2.62 3.493(2) 166.2 9_557
N3 H3A Br1 0.89 2.90 3.4009(6) 117.3 14_457
