#------------------------------------------------------------------------------
#$Date: 2016-01-09 11:17:46 +0100 (Sat 09 de Jan de 2016) $
#$Revision: 173735 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/30/7223044.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_7223044
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                 93.601(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6379(4)
_cell_length_b                   7.6361(6)
_cell_length_c                   10.7112(3)
_cell_measurement_reflns_used    1743
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.1760
_cell_measurement_theta_min      2.8030
_cell_volume                     868.38(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)'
_diffrn_ambient_pressure         3800000
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 10.3457
_diffrn_measured_fraction_theta_full 0.541
_diffrn_measured_fraction_theta_max 0.533
_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  0.0490
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_laue_measured_fraction_full 0.541
_diffrn_reflns_laue_measured_fraction_max 0.533
_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            1833
_diffrn_reflns_point_group_measured_fraction_full 0.541
_diffrn_reflns_point_group_measured_fraction_max 0.533
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.365
_diffrn_reflns_theta_min         3.286
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    11.148
_exptl_absorpt_correction_T_max  0.277
_exptl_absorpt_correction_T_min  0.210
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'Absorb-7 (Angel, 2013)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.677
_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         0.329
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     52
_refine_ls_number_reflns         478
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0224
_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)+(0.0210P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0487
_refine_ls_wR_factor_ref         0.0498
_reflns_Friedel_coverage         0.000
_reflns_number_gt                443
_reflns_number_total             478
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5ce01820j3.cif
_cod_data_source_block           380GPa
_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               7223044
_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
;

    _3.80GPa.res created by SHELXL-2014/7

TITL 3.80
CELL  0.71073 10.63790  7.63610 10.71120 90.00000 93.60100 90.00000
ZERR 4  0.00040  0.00060  0.00030  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
DELU
SIMU
BOND $H
WGHT    0.021000
FVAR       2.35600
BR1   1    0.289215    0.510993    0.495720    11.00000    0.01812    0.01531 =
         0.01692    0.00133    0.00227   -0.00057
CO1   2    0.000000    0.291732    0.250000    10.50000    0.01170    0.00612 =
         0.01150    0.00000   -0.00019    0.00000
N1    4    0.181578    0.287633    0.251516    11.00000    0.01757    0.00898 =
         0.01674    0.00044    0.00102    0.00141
REM 0
AFIX  33
H1A   3    0.208197    0.177132    0.251738    11.00000   -1.50000
H1B   3    0.206390    0.341939    0.183779    11.00000   -1.50000
H1C   3    0.213841    0.341939    0.319729    11.00000   -1.50000
AFIX   0
N2    4    0.006529    0.300825    0.431169    11.00000    0.01556    0.01311 =
         0.01312    0.00106    0.00296   -0.00109
REM 0
AFIX  33
H2A   3    0.007630    0.192400    0.461703    11.00000   -1.50000
H2B   3    0.075880    0.357124    0.459327    11.00000   -1.50000
H2C   3   -0.060924    0.357124    0.455648    11.00000   -1.50000
AFIX   0
N3    4    0.000000    0.032960    0.250000    10.50000    0.02345    0.00205 =
         0.02031    0.00000    0.00367    0.00000
REM 0
AFIX  33
H3A   3   -0.078917   -0.005891    0.249341    10.50000   -1.50000
H3B   3    0.035733   -0.005891    0.182354    10.50000   -1.50000
H3C   3    0.043184   -0.005890    0.318304    10.50000   -1.50000
AFIX   0
N4    4    0.000000    0.540564    0.250000    10.50000    0.01034    0.00883 =
         0.01460    0.00000    0.00015    0.00000
O1    5    0.078503    0.625593    0.192830    11.00000    0.02445    0.03360 =
         0.03470    0.00156    0.02075   -0.00856
HKLF 4

REM  3.80
REM R1 =  0.0224 for     443 Fo > 4sig(Fo)  and  0.0247 for all     478 data
REM     52 parameters refined using     42 restraints

END

WGHT      0.0210      0.0000

REM Highest difference peak  0.329,  deepest hole -0.259,  1-sigma level  0.082
Q1    1   0.2137  0.2116  0.1904  11.00000  0.05    0.33
Q2    1   0.3567  0.5067  0.5454  11.00000  0.05    0.33
Q3    1   0.0000 -0.1501  0.2500  10.50000  0.05    0.28
Q4    1   0.2177  0.2802  0.0628  11.00000  0.05    0.28
Q5    1   0.1453  0.4907  0.3127  11.00000  0.05    0.27
Q6    1   0.1085  0.6254  0.2594  11.00000  0.05    0.26
Q7    1  -0.0370  0.2082  0.2853  11.00000  0.05    0.25
Q8    1   0.1192  0.1952  0.5778  11.00000  0.05    0.25
Q9    1   0.0816  0.2171  0.3185  11.00000  0.05    0.25
Q10   1   0.0198  0.4171  0.5068  11.00000  0.05    0.24
;
_shelx_res_checksum              3424
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 0.28921(3) 0.51099(6) 0.49572(3) 0.01674(19) Uani 1 1 d . . .
Co1 Co 0.0000 0.29173(11) 0.2500 0.0098(2) Uani 1 2 d S TU P
N1 N 0.1816(3) 0.2876(5) 0.2515(3) 0.0144(9) Uani 1 1 d . U .
H1A H 0.2082 0.1771 0.2517 0.022 Uiso 1 1 calc R U .
H1B H 0.2064 0.3419 0.1838 0.022 Uiso 1 1 calc R U .
H1C H 0.2138 0.3419 0.3197 0.022 Uiso 1 1 calc R U .
N2 N 0.0065(3) 0.3008(5) 0.4312(2) 0.0138(8) Uani 1 1 d . U .
H2A H 0.0076 0.1924 0.4617 0.021 Uiso 1 1 calc R U .
H2B H 0.0759 0.3571 0.4593 0.021 Uiso 1 1 calc R U .
H2C H -0.0609 0.3571 0.4556 0.021 Uiso 1 1 calc R U .
N3 N 0.0000 0.0330(7) 0.2500 0.0152(11) Uani 1 2 d S TU P
H3A H -0.0789 -0.0059 0.2493 0.023 Uiso 0.5 1 calc R U P
H3B H 0.0357 -0.0059 0.1824 0.023 Uiso 0.5 1 calc R U P
H3C H 0.0432 -0.0059 0.3183 0.023 Uiso 0.5 1 calc R U P
N4 N 0.0000 0.5406(8) 0.2500 0.0113(12) Uani 1 2 d S TU P
O1 O 0.0785(3) 0.6256(5) 0.1928(3) 0.0301(10) Uani 1 1 d . U .
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(3) 0.0153(5) 0.0169(3) 0.00133(15) 0.0023(2) -0.00057(15)
Co1 0.0117(4) 0.0061(8) 0.0115(4) 0.000 -0.0002(3) 0.000
N1 0.0176(19) 0.009(3) 0.0167(16) 0.0004(13) 0.0010(13) 0.0014(13)
N2 0.0156(18) 0.013(3) 0.0131(15) 0.0011(13) 0.0030(13) -0.0011(13)
N3 0.023(3) 0.002(4) 0.020(2) 0.000 0.004(2) 0.000
N4 0.010(3) 0.009(5) 0.015(2) 0.000 0.000(2) 0.000
O1 0.0245(19) 0.034(4) 0.0347(18) 0.0016(15) 0.0208(15) -0.0086(15)
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 90.93(12) . .
N4 Co1 N1 90.93(12) . 2
N1 Co1 N1 178.1(2) . 2
N4 Co1 N2 87.95(11) . 2
N1 Co1 N2 88.97(12) . 2
N1 Co1 N2 91.10(12) 2 2
N4 Co1 N2 87.95(11) . .
N1 Co1 N2 91.10(12) . .
N1 Co1 N2 88.97(12) 2 .
N2 Co1 N2 175.9(2) 2 .
N4 Co1 N3 180.0 . .
N1 Co1 N3 89.07(12) . .
N1 Co1 N3 89.07(12) 2 .
N2 Co1 N3 92.05(11) 2 .
N2 Co1 N3 92.05(11) . .
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 117.3(6) . 2
O1 N4 Co1 121.3(3) . .
O1 N4 Co1 121.3(3) 2 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N4 1.900(6) .
Co1 N1 1.931(3) .
Co1 N1 1.931(3) 2
Co1 N2 1.939(3) 2
Co1 N2 1.939(3) .
Co1 N3 1.976(5) .
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 1.248(4) .
N4 O1 1.248(4) 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 2.34 2.865(4) 117.6 4_545
N1 H1B Br1 0.89 2.51 3.402(3) 176.7 6_565
N1 H1C Br1 0.89 2.38 3.269(3) 174.6 .
N2 H2A Br1 0.89 2.68 3.285(3) 126.5 7_556
N2 H2A Br1 0.89 2.75 3.305(3) 121.7 3_445
N2 H2B Br1 0.89 2.56 3.440(3) 168.5 .
N2 H2C Br1 0.89 2.71 3.590(3) 170.1 5_566
N3 H3A Br1 0.89 3.07 3.5672(5) 117.5 3_445
N3 H3A Br1 0.89 2.98 3.4339(6) 113.7 8_455
