#------------------------------------------------------------------------------
#$Date: 2016-01-09 12:17:46 +0200 (Sat, 09 Jan 2016) $
#$Revision: 173735 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/30/7223046.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_7223046
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                 93.439(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6023(5)
_cell_length_b                   7.5308(7)
_cell_length_c                   10.6049(4)
_cell_measurement_reflns_used    1704
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.8020
_cell_measurement_theta_min      2.6420
_cell_volume                     845.21(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         4800000
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 10.3457
_diffrn_measured_fraction_theta_full 0.576
_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  0.0546
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_laue_measured_fraction_full 0.576
_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       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2236
_diffrn_reflns_point_group_measured_fraction_full 0.576
_diffrn_reflns_point_group_measured_fraction_max 0.560
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.354
_diffrn_reflns_theta_min         3.320
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    11.454
_exptl_absorpt_correction_T_max  0.272
_exptl_absorpt_correction_T_min  0.207
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'Absorb-7 (Angel, 2013)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.750
_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         0.386
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     52
_refine_ls_number_reflns         482
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0252
_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)+(0.0275P)²+2.5892P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0603
_reflns_Friedel_coverage         0.000
_reflns_number_gt                451
_reflns_number_total             482
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5ce01820j3.cif
_cod_data_source_block           480GPa
_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               7223046
_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
;

    _4.80GPa.res created by SHELXL-2014/7

TITL 4.80
CELL  0.71073 10.60230  7.53080 10.60490 90.00000 93.43900 90.00000
ZERR 4  0.00050  0.00070  0.00040  0.00000  0.00400  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    0.027500    2.589200
FVAR       2.41200
BR1   1    0.288969    0.510177    0.496233    11.00000    0.01750    0.01396 =
         0.01622    0.00148    0.00223   -0.00039
CO1   2    0.000000    0.291958    0.250000    10.50000    0.01054    0.00704 =
         0.01129    0.00000    0.00031    0.00000
N1    4    0.181763    0.289700    0.251837    11.00000    0.01586    0.01286 =
         0.01365    0.00069   -0.00036    0.00149
AFIX  33
H1A   3    0.209060    0.177934    0.252113    11.00000   -1.50000
H1B   3    0.206682    0.345061    0.183480    11.00000   -1.50000
H1C   3    0.213535    0.345062    0.320767    11.00000   -1.50000
AFIX   0
N2    4    0.005284    0.301338    0.432559    11.00000    0.01363    0.01123 =
         0.01405   -0.00182    0.00173   -0.00189
AFIX  33
H2A   3    0.006178    0.191428    0.463444    11.00000   -1.50000
H2B   3    0.074687    0.358450    0.461239    11.00000   -1.50000
H2C   3   -0.062583    0.358450    0.456971    11.00000   -1.50000
AFIX   0
N3    4    0.000000    0.030545    0.250000    10.50000    0.02416    0.00925 =
         0.01554    0.00000   -0.00040    0.00000
AFIX  33
H3A   3    0.079187   -0.008849    0.250801    10.50000   -1.50000
H3B   3   -0.036168   -0.008849    0.318243    10.50000   -1.50000
H3C   3   -0.043020   -0.008849    0.180956    10.50000   -1.50000
AFIX   0
N4    4    0.000000    0.545425    0.250000    10.50000    0.01207    0.00959 =
         0.01132    0.00000    0.00012    0.00000
O1    5    0.080533    0.629895    0.195514    11.00000    0.02478    0.02706 =
         0.03633   -0.00135    0.01865   -0.00616
HKLF 4

REM  4.80
REM R1 =  0.0252 for     451 Fo > 4sig(Fo)  and  0.0273 for all     482 data
REM     52 parameters refined using      0 restraints

END

WGHT      0.0274      2.5908

REM Highest difference peak  0.386,  deepest hole -0.376,  1-sigma level  0.098
Q1    1   0.1410  0.5294  0.2543  11.00000  0.05    0.39
Q2    1   0.2013  0.1973  0.1950  11.00000  0.05    0.34
Q3    1   0.0061  0.2779  0.3612  11.00000  0.05    0.33
Q4    1   0.2557  0.3484  0.2420  11.00000  0.05    0.30
Q5    1   0.0951  0.2278  0.3442  11.00000  0.05    0.30
Q6    1   0.1543  0.4897  0.3100  11.00000  0.05    0.29
Q7    1  -0.0961 -0.1266  0.4188  11.00000  0.05    0.28
Q8    1   0.1360  0.6053  0.1710  11.00000  0.05    0.28
Q9    1   0.2202  0.2322  0.3136  11.00000  0.05    0.27
Q10   1  -0.0861 -0.0315  0.3335  11.00000  0.05    0.27
;
_shelx_res_checksum              20634
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 0.28897(4) 0.51018(7) 0.49623(4) 0.0158(2) Uani 1 1 d . . .
Co1 Co 0.0000 0.29196(13) 0.2500 0.0096(3) Uani 1 2 d S T P
N1 N 0.1818(3) 0.2897(6) 0.2518(3) 0.0142(10) Uani 1 1 d . . .
H1A H 0.2091 0.1779 0.2521 0.021 Uiso 1 1 calc R U .
H1B H 0.2067 0.3451 0.1835 0.021 Uiso 1 1 calc R U .
H1C H 0.2135 0.3451 0.3208 0.021 Uiso 1 1 calc R U .
N2 N 0.0053(3) 0.3013(6) 0.4326(3) 0.0129(10) Uani 1 1 d . . .
H2A H 0.0062 0.1914 0.4634 0.019 Uiso 1 1 calc R U .
H2B H 0.0747 0.3585 0.4612 0.019 Uiso 1 1 calc R U .
H2C H -0.0626 0.3584 0.4570 0.019 Uiso 1 1 calc R U .
N3 N 0.0000 0.0305(8) 0.2500 0.0164(15) Uani 1 2 d S T P
H3A H 0.0792 -0.0088 0.2508 0.025 Uiso 0.5 1 calc R U P
H3B H -0.0362 -0.0088 0.3182 0.025 Uiso 0.5 1 calc R U P
H3C H -0.0430 -0.0088 0.1810 0.025 Uiso 0.5 1 calc R U P
N4 N 0.0000 0.5454(9) 0.2500 0.0110(16) Uani 1 2 d S T P
O1 O 0.0805(3) 0.6299(6) 0.1955(3) 0.0287(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 0.0175(3) 0.0140(6) 0.0162(3) 0.00148(16) 0.0022(2) -0.00039(17)
Co1 0.0105(5) 0.0070(10) 0.0113(4) 0.000 0.0003(3) 0.000
N1 0.016(2) 0.013(4) 0.0136(18) 0.0007(14) -0.0004(15) 0.0015(15)
N2 0.014(2) 0.011(4) 0.0140(18) -0.0018(15) 0.0017(15) -0.0019(15)
N3 0.024(3) 0.009(6) 0.016(3) 0.000 0.000(2) 0.000
N4 0.012(3) 0.010(7) 0.011(3) 0.000 0.000(3) 0.000
O1 0.025(2) 0.027(5) 0.036(2) -0.0013(17) 0.0187(17) -0.0062(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 90.51(14) . 2
N4 Co1 N1 90.51(14) . .
N1 Co1 N1 179.0(3) 2 .
N4 Co1 N2 87.91(13) . 2
N1 Co1 N2 91.22(14) 2 2
N1 Co1 N2 88.82(14) . 2
N4 Co1 N2 87.91(13) . .
N1 Co1 N2 88.82(14) 2 .
N1 Co1 N2 91.22(14) . .
N2 Co1 N2 175.8(3) 2 .
N4 Co1 N3 180.0 . .
N1 Co1 N3 89.49(14) 2 .
N1 Co1 N3 89.49(13) . .
N2 Co1 N3 92.09(13) 2 .
N2 Co1 N3 92.09(13) . .
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(4) . .
O1 N4 Co1 121.0(4) 2 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N4 1.909(7) .
Co1 N1 1.926(3) 2
Co1 N1 1.926(3) .
Co1 N2 1.935(3) 2
Co1 N2 1.935(3) .
Co1 N3 1.969(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 1.236(5) .
N4 O1 1.236(5) 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 2.30 2.818(5) 117.5 4_545
N1 H1B Br1 0.89 2.47 3.359(4) 176.4 6_565
N1 H1C Br1 0.89 2.34 3.227(4) 175.6 .
N2 H2A Br1 0.89 2.66 3.261(4) 125.4 7_556
N2 H2A Br1 0.89 2.72 3.273(4) 121.6 3_445
N2 H2B Br1 0.89 2.55 3.425(4) 167.8 .
N2 H2C Br1 0.89 2.67 3.550(4) 169.9 5_566
N3 H3B Br1 0.89 2.73 3.5425(5) 152.8 3_445
N3 H3C Br1 0.89 2.57 3.4088(7) 158.0 8_455
