#------------------------------------------------------------------------------
#$Date: 2016-01-09 12:17:46 +0200 (Sat, 09 Jan 2016) $
#$Revision: 173735 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/30/7223045.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_7223045
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                 93.508(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6148(4)
_cell_length_b                   7.5680(7)
_cell_length_c                   10.6476(4)
_cell_measurement_reflns_used    1712
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.1830
_cell_measurement_theta_min      2.6350
_cell_volume                     853.75(9)
_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         4400000
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 10.3457
_diffrn_measured_fraction_theta_full 0.570
_diffrn_measured_fraction_theta_max 0.557
_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  0.0547
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_laue_measured_fraction_full 0.570
_diffrn_reflns_laue_measured_fraction_max 0.557
_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       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2262
_diffrn_reflns_point_group_measured_fraction_full 0.570
_diffrn_reflns_point_group_measured_fraction_max 0.557
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         3.308
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    11.339
_exptl_absorpt_correction_T_max  0.274
_exptl_absorpt_correction_T_min  0.208
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'Absorb-7 (Angel, 2013)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.722
_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         0.330
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     52
_refine_ls_number_reflns         488
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0240
_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)+(0.0246P)²+1.7508P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0557
_refine_ls_wR_factor_ref         0.0575
_reflns_Friedel_coverage         0.000
_reflns_number_gt                455
_reflns_number_total             488
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5ce01820j3.cif
_cod_data_source_block           440GPa
_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               7223045
_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
;

    _4.40GPa.res created by SHELXL-2014/7

TITL 4.40
CELL  0.71073 10.61480  7.56800 10.64760 90.00000 93.50800 90.00000
ZERR 4  0.00040  0.00070  0.00040  0.00000  0.00300  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    0.024600    1.750800
FVAR       2.39359
BR1   1    0.289038    0.510485    0.496043    11.00000    0.01786    0.01461 =
         0.01636    0.00130    0.00261   -0.00067
CO1   2    0.000000    0.291793    0.250000    10.50000    0.01098    0.00735 =
         0.01107    0.00000    0.00034    0.00000
N1    4    0.181912    0.289171    0.251769    11.00000    0.01625    0.01197 =
         0.01356   -0.00064    0.00025    0.00313
AFIX  33
H1A   3    0.209060    0.177899    0.252033    11.00000   -1.50000
H1B   3    0.206751    0.344202    0.183672    11.00000   -1.50000
H1C   3    0.213810    0.344202    0.320418    11.00000   -1.50000
AFIX   0
N2    4    0.005548    0.300632    0.432082    11.00000    0.01495    0.01064 =
         0.01422   -0.00063    0.00160   -0.00239
AFIX  33
H2A   3    0.006481    0.191177    0.462691    11.00000   -1.50000
H2B   3    0.074913    0.357390    0.460714    11.00000   -1.50000
H2C   3   -0.062200    0.357390    0.456494    11.00000   -1.50000
AFIX   0
N3    4    0.000000    0.032291    0.250000    10.50000    0.02262    0.00588 =
         0.01905    0.00000   -0.00031    0.00000
AFIX  33
H3A   3   -0.079093   -0.006909    0.249231    10.50000   -1.50000
H3B   3    0.036017   -0.006909    0.182011    10.50000   -1.50000
H3C   3    0.043076   -0.006909    0.318758    10.50000   -1.50000
AFIX   0
N4    4    0.000000    0.544194    0.250000    10.50000    0.01291    0.00493 =
         0.01258    0.00000   -0.00099    0.00000
O1    5    0.080101    0.628497    0.195039    11.00000    0.02658    0.02729 =
         0.03711    0.00031    0.01982   -0.00647
HKLF 4

REM  4.40
REM R1 =  0.0240 for     455 Fo > 4sig(Fo)  and  0.0265 for all     488 data
REM     52 parameters refined using      0 restraints

END

WGHT      0.0246      1.7509

REM Highest difference peak  0.330,  deepest hole -0.304,  1-sigma level  0.090
Q1    1   0.3584  0.4961  0.5609  11.00000  0.05    0.33
Q2    1   0.1439  0.4865  0.3120  11.00000  0.05    0.32
Q3    1   0.2027  0.4158  0.2580  11.00000  0.05    0.32
Q4    1   0.0601  0.2814  0.3101  11.00000  0.05    0.32
Q5    1   0.3527  0.3115  0.4340  11.00000  0.05    0.31
Q6    1   0.0000  0.5000  0.5000  10.50000  0.05    0.31
Q7    1   0.2605  0.3353  0.2487  11.00000  0.05    0.31
Q8    1   0.2800  0.2232  0.4341  11.00000  0.05    0.30
Q9    1   0.1952  0.1954  0.1896  11.00000  0.05    0.28
Q10   1   0.2226  0.5106  0.4341  11.00000  0.05    0.27
;
_shelx_res_checksum              73952
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 0.28904(4) 0.51049(6) 0.49604(3) 0.0162(2) Uani 1 1 d . . .
Co1 Co 0.0000 0.29179(13) 0.2500 0.0098(3) Uani 1 2 d S T P
N1 N 0.1819(3) 0.2892(6) 0.2518(3) 0.0140(10) Uani 1 1 d . . .
H1A H 0.2091 0.1779 0.2520 0.021 Uiso 1 1 calc R U .
H1B H 0.2068 0.3442 0.1837 0.021 Uiso 1 1 calc R U .
H1C H 0.2138 0.3442 0.3204 0.021 Uiso 1 1 calc R U .
N2 N 0.0055(3) 0.3006(5) 0.4321(3) 0.0132(9) Uani 1 1 d . . .
H2A H 0.0065 0.1912 0.4627 0.020 Uiso 1 1 calc R U .
H2B H 0.0749 0.3574 0.4607 0.020 Uiso 1 1 calc R U .
H2C H -0.0622 0.3574 0.4565 0.020 Uiso 1 1 calc R U .
N3 N 0.0000 0.0323(8) 0.2500 0.0159(14) Uani 1 2 d S T P
H3A H -0.0791 -0.0069 0.2492 0.024 Uiso 0.5 1 calc R U P
H3B H 0.0360 -0.0069 0.1820 0.024 Uiso 0.5 1 calc R U P
H3C H 0.0431 -0.0069 0.3188 0.024 Uiso 0.5 1 calc R U P
N4 N 0.0000 0.5442(9) 0.2500 0.0102(15) Uani 1 2 d S T P
O1 O 0.0801(3) 0.6285(6) 0.1950(3) 0.0296(12) 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 0.0179(3) 0.0146(6) 0.0164(3) 0.00130(15) 0.0026(2) -0.00067(16)
Co1 0.0110(5) 0.0073(9) 0.0111(4) 0.000 0.0003(3) 0.000
N1 0.016(2) 0.012(4) 0.0136(17) -0.0006(13) 0.0003(14) 0.0031(15)
N2 0.015(2) 0.011(4) 0.0142(17) -0.0006(14) 0.0016(14) -0.0024(15)
N3 0.023(3) 0.006(6) 0.019(3) 0.000 0.000(2) 0.000
N4 0.013(3) 0.005(7) 0.013(2) 0.000 -0.001(3) 0.000
O1 0.027(2) 0.027(4) 0.037(2) 0.0003(17) 0.0198(16) -0.0065(17)
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 90.59(13) . .
N4 Co1 N1 90.59(13) . 2
N1 Co1 N1 178.8(3) . 2
N4 Co1 N2 88.02(12) . .
N1 Co1 N2 91.23(14) . .
N1 Co1 N2 88.81(14) 2 .
N4 Co1 N2 88.02(12) . 2
N1 Co1 N2 88.81(14) . 2
N1 Co1 N2 91.23(14) 2 2
N2 Co1 N2 176.0(2) . 2
N4 Co1 N3 180.0 . .
N1 Co1 N3 89.41(13) . .
N1 Co1 N3 89.41(13) 2 .
N2 Co1 N3 91.98(12) . .
N2 Co1 N3 91.98(12) 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 118.0(7) 2 .
O1 N4 Co1 121.0(3) 2 .
O1 N4 Co1 121.0(3) . .
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 1.930(3) .
Co1 N1 1.930(3) 2
Co1 N2 1.937(3) .
Co1 N2 1.937(3) 2
Co1 N3 1.964(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 1.238(5) 2
N4 O1 1.238(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 2.30 2.829(5) 117.6 4_545
N1 H1B Br1 0.89 2.49 3.374(4) 176.5 6_565
N1 H1C Br1 0.89 2.35 3.241(3) 175.3 .
N2 H2A Br1 0.89 2.67 3.268(4) 125.7 7_556
N2 H2A Br1 0.89 2.72 3.280(4) 121.6 3_445
N2 H2B Br1 0.89 2.56 3.434(3) 167.9 .
N2 H2C Br1 0.89 2.68 3.564(4) 170.1 5_566
N3 H3A Br1 0.89 3.05 3.5529(5) 117.3 3_445
N3 H3A Br1 0.89 2.96 3.4191(7) 113.9 8_455
