# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_000GPa
_database_code_depnum_ccdc_archive 'CCDC 1423454'
_audit_update_record             
;
2015-09-10 deposited with the CCDC.
2015-10-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        nitro-pentaammine-Co(III)-dibromide
_chemical_name_common            nitro-pentaammine-Co(III)-dibromide
_chemical_melting_point          ?
_chemical_formula_moiety         'Co H15 N6 O2, 2(Br)'
_chemical_formula_sum            'Br2 Co H15 N6 O2'
_chemical_formula_weight         349.93

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

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'

_cell_length_a                   10.6807(6)
_cell_length_b                   8.8299(8)
_cell_length_c                   10.9759(5)
_cell_angle_alpha                90
_cell_angle_beta                 94.604(5)
_cell_angle_gamma                90
_cell_volume                     1031.79(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1571
_cell_measurement_theta_min      2.7960
_cell_measurement_theta_max      27.4360

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_preparation       'mounted in DAC'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.253
_exptl_crystal_F_000             680
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?

_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    9.382
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?

_exptl_absorpt_correction_type   Gaussian
_exptl_absorpt_correction_T_min  0.233
_exptl_absorpt_correction_T_max  0.302
_exptl_absorpt_process_details   'Absorb-7 (Angel, 2013)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      295(2)
_diffrn_ambient_pressure         100
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a

_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 10.3457
_diffrn_reflns_number            2634
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.997
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.571
_diffrn_measured_fraction_theta_full 0.587
_diffrn_reflns_Laue_measured_fraction_max 0.571
_diffrn_reflns_Laue_measured_fraction_full 0.587
_diffrn_reflns_point_group_measured_fraction_max 0.571
_diffrn_reflns_point_group_measured_fraction_full 0.587
_reflns_number_total             605
_reflns_number_gt                532
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_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_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_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'

_computing_molecular_graphics    'Mercury (Macrae et al., 2006)'
_computing_publication_material  'enCIFer (Allen et al., 2004)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0233P)²+1.1579P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         605
_refine_ls_number_parameters     52
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0286
_refine_ls_wR_factor_ref         0.0677
_refine_ls_wR_factor_gt          0.0621
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_restrained_S_all      1.114
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.29219(5) 0.51493(7) 0.48994(4) 0.0323(2) Uani 1 1 d . . . . .
Co1 Co 0.0000 0.28810(12) 0.2500 0.0209(3) Uani 1 2 d S T P . .
N1 N 0.1827(3) 0.2893(5) 0.2502(3) 0.0298(11) Uani 1 1 d . . . . .
H1A H 0.2109 0.1944 0.2503 0.045 Uiso 1 1 calc R U . . .
H1B H 0.2049 0.3369 0.1838 0.045 Uiso 1 1 calc R U . . .
H1C H 0.2156 0.3369 0.3167 0.045 Uiso 1 1 calc R U . . .
N2 N 0.0127(4) 0.2940(5) 0.4289(3) 0.0284(11) Uani 1 1 d . . . . .
H2A H 0.0147 0.1999 0.4580 0.043 Uiso 1 1 calc R U . . .
H2B H 0.0826 0.3424 0.4557 0.043 Uiso 1 1 calc R U . . .
H2C H -0.0536 0.3424 0.4542 0.043 Uiso 1 1 calc R U . . .
N3 N 0.0000 0.0637(8) 0.2500 0.0315(16) Uani 1 2 d S T P . .
H3A H 0.0786 0.0301 0.2501 0.047 Uiso 0.5 1 calc R U P . .
H3B H -0.0339 0.0301 0.3164 0.047 Uiso 0.5 1 calc R U P . .
H3C H -0.0447 0.0301 0.1835 0.047 Uiso 0.5 1 calc R U P . .
N4 N 0.0000 0.5050(9) 0.2500 0.0280(19) Uani 1 2 d S T P . .
O1 O 0.0711(4) 0.5766(6) 0.1881(4) 0.0539(15) 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 0.0325(4) 0.0350(7) 0.0295(3) 0.0006(2) 0.0034(3) -0.0027(2)
Co1 0.0238(6) 0.0212(10) 0.0177(5) 0.000 0.0014(4) 0.000
N1 0.026(3) 0.035(5) 0.029(2) -0.0044(18) 0.0043(19) 0.0003(19)
N2 0.036(3) 0.025(5) 0.024(2) -0.0019(16) 0.002(2) -0.0035(19)
N3 0.034(4) 0.036(7) 0.023(3) 0.000 0.000(3) 0.000
N4 0.035(5) 0.023(8) 0.026(4) 0.000 0.003(4) 0.000
O1 0.068(3) 0.035(5) 0.062(3) 0.008(2) 0.025(2) -0.006(3)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 N4 1.915(8) . ?
Co1 N1 1.951(4) 2 ?
Co1 N1 1.951(4) . ?
Co1 N2 1.958(3) . ?
Co1 N2 1.958(3) 2 ?
Co1 N3 1.981(7) . ?
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 1.233(6) . ?
N4 O1 1.234(6) 2 ?

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
_geom_angle_publ_flag
N4 Co1 N1 89.70(13) . 2 ?
N4 Co1 N1 89.70(13) . . ?
N1 Co1 N1 179.4(3) 2 . ?
N4 Co1 N2 88.48(13) . . ?
N1 Co1 N2 89.41(16) 2 . ?
N1 Co1 N2 90.58(16) . . ?
N4 Co1 N2 88.48(13) . 2 ?
N1 Co1 N2 90.58(16) 2 2 ?
N1 Co1 N2 89.41(16) . 2 ?
N2 Co1 N2 177.0(3) . 2 ?
N4 Co1 N3 180.0 . . ?
N1 Co1 N3 90.30(13) 2 . ?
N1 Co1 N3 90.30(13) . . ?
N2 Co1 N3 91.52(13) . . ?
N2 Co1 N3 91.52(13) 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 118.4(10) . 2 ?
O1 N4 Co1 120.8(5) . . ?
O1 N4 Co1 120.8(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 2.59 3.258(6) 132.5 4_545
N1 H1B Br1 0.89 2.73 3.613(4) 175.3 6_565
N1 H1C Br1 0.89 2.55 3.430(4) 170.0 .
N2 H2A Br1 0.89 2.83 3.504(4) 134.1 7_556
N2 H2A Br1 0.89 2.93 3.510(4) 124.5 3_445
N2 H2B Br1 0.89 2.71 3.584(4) 168.0 .
N2 H2C Br1 0.89 2.95 3.835(4) 172.5 5_566
N3 H3B Br1 0.89 2.77 3.6037(10) 156.7 3_445
N3 H3C Br1 0.89 2.67 3.5411(14) 167.3 8_455

_refine_diff_density_max         0.403
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.089

_shelx_res_file                  
;

    _0.00GPa.res created by SHELXL-2014/7

TITL 0.00
CELL  0.71073 10.68070  8.82990 10.97590 90.00000 94.60400 90.00000
ZERR 4  0.00060  0.00080  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    0.023300    1.157900
FVAR       2.18121
BR1   1    0.292190    0.514935    0.489945    11.00000    0.03254    0.03497 =
         0.02946    0.00056    0.00341   -0.00269
CO1   2    0.000000    0.288097    0.250000    10.50000    0.02380    0.02122 =
         0.01766    0.00000    0.00145    0.00000
N1    4    0.182678    0.289256    0.250220    11.00000    0.02635    0.03463 =
         0.02884   -0.00439    0.00429    0.00028
AFIX  33
H1A   3    0.210868    0.194404    0.250254    11.00000   -1.50000
H1B   3    0.204855    0.336946    0.183832    11.00000   -1.50000
H1C   3    0.215645    0.336946    0.316675    11.00000   -1.50000
AFIX   0
N2    4    0.012656    0.293982    0.428891    11.00000    0.03613    0.02543 =
         0.02357   -0.00189    0.00197   -0.00346
AFIX  33
H2A   3    0.014718    0.199877    0.458032    11.00000   -1.50000
H2B   3    0.082597    0.342371    0.455740    11.00000   -1.50000
H2C   3   -0.053593    0.342371    0.454218    11.00000   -1.50000
AFIX   0
N3    4    0.000000    0.063739    0.250000    10.50000    0.03419    0.03646 =
         0.02343    0.00000    0.00019    0.00000
AFIX  33
H3A   3    0.078570    0.030141    0.250095    10.50000   -1.50000
H3B   3   -0.033891    0.030141    0.316374    10.50000   -1.50000
H3C   3   -0.044679    0.030141    0.183531    10.50000   -1.50000
AFIX   0
N4    4    0.000000    0.504972    0.250000    10.50000    0.03518    0.02330 =
         0.02564    0.00000    0.00306    0.00000
O1    5    0.071137    0.576552    0.188084    11.00000    0.06847    0.03460 =
         0.06192    0.00817    0.02481   -0.00562
HKLF 4

REM  0.00
REM R1 =  0.0286 for     532 Fo > 4sig(Fo)  and  0.0349 for all     605 data
REM     52 parameters refined using      0 restraints

END

WGHT      0.0234      1.1189

REM Highest difference peak  0.403,  deepest hole -0.363,  1-sigma level  0.089
Q1    1   0.0000  0.7480  0.2500  10.50000  0.05    0.40
Q2    1   0.0233  0.2935  0.3528  11.00000  0.05    0.38
Q3    1   0.2646  0.4360  0.5326  11.00000  0.05    0.36
Q4    1   0.2146  0.2659  0.3085  11.00000  0.05    0.35
Q5    1   0.3558  0.3553  0.4262  11.00000  0.05    0.35
Q6    1   0.2056  0.3506  0.5602  11.00000  0.05    0.33
Q7    1  -0.0667  0.2255  0.3919  11.00000  0.05    0.28
Q8    1  -0.1022  0.1834  0.4123  11.00000  0.05    0.28
Q9    1   0.1178  0.3453  0.2683  11.00000  0.05    0.27
Q10   1  -0.0384  0.1925  0.2995  11.00000  0.05    0.27
;
_shelx_res_checksum              14368
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_015GPa
_database_code_depnum_ccdc_archive 'CCDC 1423455'
_audit_update_record             
;
2015-09-10 deposited with the CCDC.
2015-10-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        nitro-pentaammine-Co(III)-dibromide
_chemical_name_common            nitro-pentaammine-Co(III)-dibromide
_chemical_melting_point          ?
_chemical_formula_moiety         'Co H15 N6 O2, 2(Br)'
_chemical_formula_sum            'Br2 Co H15 N6 O2'
_chemical_formula_weight         349.93

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

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'

_cell_length_a                   10.6575(5)
_cell_length_b                   8.7649(9)
_cell_length_c                   10.9567(5)
_cell_angle_alpha                90
_cell_angle_beta                 94.589(5)
_cell_angle_gamma                90
_cell_volume                     1020.21(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1795
_cell_measurement_theta_min      2.7820
_cell_measurement_theta_max      27.7820

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_preparation       'mounted in DAC'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.278
_exptl_crystal_F_000             680
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?

_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    9.489
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?

_exptl_absorpt_correction_type   Gaussian
_exptl_absorpt_correction_T_min  0.231
_exptl_absorpt_correction_T_max  0.300
_exptl_absorpt_process_details   'Absorb-7 (Angel, 2013)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      295(2)
_diffrn_ambient_pressure         150000
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a

_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 10.3457
_diffrn_reflns_number            2719
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.013
_diffrn_reflns_theta_max         26.357
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.560
_diffrn_measured_fraction_theta_full 0.577
_diffrn_reflns_Laue_measured_fraction_max 0.560
_diffrn_reflns_Laue_measured_fraction_full 0.577
_diffrn_reflns_point_group_measured_fraction_max 0.560
_diffrn_reflns_point_group_measured_fraction_full 0.577
_reflns_number_total             588
_reflns_number_gt                541
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_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_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_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'

_computing_molecular_graphics    'Mercury (Macrae et al., 2006)'
_computing_publication_material  'enCIFer (Allen et al., 2004)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0190P)²+1.1318P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         588
_refine_ls_number_parameters     52
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0271
_refine_ls_wR_factor_ref         0.0578
_refine_ls_wR_factor_gt          0.0557
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      1.084
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
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)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
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_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
_geom_angle_publ_flag
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_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

_refine_diff_density_max         0.498
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.083

_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
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_058GPa
_database_code_depnum_ccdc_archive 'CCDC 1423456'
_audit_update_record             
;
2015-09-10 deposited with the CCDC.
2015-10-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        nitro-pentaammine-Co(III)-dibromide
_chemical_name_common            nitro-pentaammine-Co(III)-dibromide
_chemical_melting_point          ?
_chemical_formula_moiety         'Co H15 N6 O2, 2(Br)'
_chemical_formula_sum            'Br2 Co H15 N6 O2'
_chemical_formula_weight         349.93

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

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'

_cell_length_a                   10.6184(4)
_cell_length_b                   8.6082(8)
_cell_length_c                   10.9307(4)
_cell_angle_alpha                90
_cell_angle_beta                 94.591(4)
_cell_angle_gamma                90
_cell_volume                     995.92(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1799
_cell_measurement_theta_min      2.8070
_cell_measurement_theta_max      28.1060

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_preparation       'mounted in DAC'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.334
_exptl_crystal_F_000             680
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?

_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    9.720
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?

_exptl_absorpt_correction_type   Gaussian
_exptl_absorpt_correction_T_min  0.228
_exptl_absorpt_correction_T_max  0.297
_exptl_absorpt_process_details   'Absorb-7 (Angel, 2013)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      295(2)
_diffrn_ambient_pressure         580000
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a

_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 10.3457
_diffrn_reflns_number            2610
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.050
_diffrn_reflns_theta_max         26.350
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.555
_diffrn_measured_fraction_theta_full 0.567
_diffrn_reflns_Laue_measured_fraction_max 0.555
_diffrn_reflns_Laue_measured_fraction_full 0.567
_diffrn_reflns_point_group_measured_fraction_max 0.555
_diffrn_reflns_point_group_measured_fraction_full 0.567
_reflns_number_total             569
_reflns_number_gt                518
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_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_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_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'

_computing_molecular_graphics    'Mercury (Macrae et al., 2006)'
_computing_publication_material  'enCIFer (Allen et al., 2004)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0284P)²+1.2770P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         569
_refine_ls_number_parameters     52
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0266
_refine_ls_wR_factor_ref         0.0634
_refine_ls_wR_factor_gt          0.0614
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.29156(4) 0.51579(6) 0.49120(4) 0.0285(2) Uani 1 1 d . . . . .
Co1 Co 0.0000 0.28883(10) 0.2500 0.0185(3) Uani 1 2 d S T P . .
N1 N 0.1841(3) 0.2889(5) 0.2507(3) 0.0267(10) Uani 1 1 d . . . . .
H1A H 0.2121 0.1914 0.2508 0.040 Uiso 1 1 calc R U . . .
H1B H 0.2068 0.3376 0.1841 0.040 Uiso 1 1 calc R U . . .
H1C H 0.2173 0.3376 0.3175 0.040 Uiso 1 1 calc R U . . .
N2 N 0.0108(3) 0.2961(5) 0.4299(3) 0.0252(9) Uani 1 1 d . . . . .
H2A H 0.0126 0.1998 0.4595 0.038 Uiso 1 1 calc R U . . .
H2B H 0.0809 0.3460 0.4573 0.038 Uiso 1 1 calc R U . . .
H2C H -0.0562 0.3460 0.4544 0.038 Uiso 1 1 calc R U . . .
N3 N 0.0000 0.0583(7) 0.2500 0.0292(13) Uani 1 2 d S T P . .
H3A H 0.0790 0.0238 0.2503 0.044 Uiso 0.5 1 calc R U P . .
H3B H -0.0343 0.0238 0.3166 0.044 Uiso 0.5 1 calc R U P . .
H3C H -0.0448 0.0238 0.1832 0.044 Uiso 0.5 1 calc R U P . .
N4 N 0.0000 0.5108(8) 0.2500 0.0275(17) Uani 1 2 d S T P . .
O1 O 0.0737(3) 0.5856(6) 0.1900(3) 0.0458(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 0.0292(3) 0.0300(6) 0.0263(3) 0.00070(18) 0.0026(2) -0.00217(18)
Co1 0.0198(5) 0.0198(8) 0.0158(4) 0.000 0.0015(4) 0.000
N1 0.024(2) 0.031(4) 0.025(2) -0.0045(15) 0.0022(18) -0.0026(15)
N2 0.028(2) 0.031(4) 0.018(2) 0.0014(14) 0.0061(17) -0.0012(15)
N3 0.042(4) 0.019(6) 0.026(3) 0.000 0.001(3) 0.000
N4 0.027(4) 0.028(7) 0.028(4) 0.000 0.000(3) 0.000
O1 0.066(3) 0.017(4) 0.056(2) 0.0054(19) 0.016(2) -0.008(2)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 N4 1.911(7) . ?
Co1 N1 1.955(3) 2 ?
Co1 N1 1.955(3) . ?
Co1 N2 1.961(3) 2 ?
Co1 N2 1.961(3) . ?
Co1 N3 1.985(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 1.240(5) . ?
N4 O1 1.240(5) 2 ?

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
_geom_angle_publ_flag
N4 Co1 N1 89.99(12) . 2 ?
N4 Co1 N1 89.99(12) . . ?
N1 Co1 N1 180.0(2) 2 . ?
N4 Co1 N2 88.16(12) . 2 ?
N1 Co1 N2 91.03(14) 2 2 ?
N1 Co1 N2 88.97(14) . 2 ?
N4 Co1 N2 88.16(12) . . ?
N1 Co1 N2 88.97(14) 2 . ?
N1 Co1 N2 91.03(14) . . ?
N2 Co1 N2 176.3(2) 2 . ?
N4 Co1 N3 180.0 . . ?
N1 Co1 N3 90.01(12) 2 . ?
N1 Co1 N3 90.01(12) . . ?
N2 Co1 N3 91.84(12) 2 . ?
N2 Co1 N3 91.84(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 117.5(9) . 2 ?
O1 N4 Co1 121.3(4) . . ?
O1 N4 Co1 121.3(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 2.49 3.135(5) 130.1 4_545
N1 H1B Br1 0.89 2.67 3.562(4) 176.0 6_565
N1 H1C Br1 0.89 2.52 3.398(3) 170.2 .
N2 H2A Br1 0.89 2.81 3.474(4) 132.8 7_556
N2 H2A Br1 0.89 2.88 3.456(4) 124.3 3_445
N2 H2B Br1 0.89 2.67 3.548(4) 168.0 .
N2 H2C Br1 0.89 2.87 3.757(4) 172.4 5_566
N3 H3B Br1 0.89 2.76 3.5941(8) 155.9 3_445
N3 H3C Br1 0.89 2.64 3.5079(12) 166.1 8_455

_refine_diff_density_max         0.310
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.083

_shelx_res_file                  
;

    _0.58GPa.res created by SHELXL-2014/7

TITL 0.58
CELL  0.71073 10.61840  8.60820 10.93070 90.00000 94.59100 90.00000
ZERR 4  0.00040  0.00080  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    0.028400    1.277000
FVAR       2.20834
BR1   1    0.291555    0.515789    0.491200    11.00000    0.02916    0.02997 =
         0.02635    0.00070    0.00265   -0.00217
CO1   2    0.000000    0.288828    0.250000    10.50000    0.01978    0.01984 =
         0.01580    0.00000    0.00145    0.00000
N1    4    0.184137    0.288886    0.250659    11.00000    0.02402    0.03096 =
         0.02510   -0.00446    0.00220   -0.00259
AFIX  33
H1A   3    0.212105    0.191418    0.250759    11.00000   -1.50000
H1B   3    0.206830    0.337633    0.184064    11.00000   -1.50000
H1C   3    0.217319    0.337633    0.317453    11.00000   -1.50000
AFIX   0
N2    4    0.010822    0.296144    0.429856    11.00000    0.02764    0.03089 =
         0.01765    0.00136    0.00609   -0.00119
AFIX  33
H2A   3    0.012608    0.199824    0.459536    11.00000   -1.50000
H2B   3    0.080924    0.345964    0.457272    11.00000   -1.50000
H2C   3   -0.056154    0.345964    0.454383    11.00000   -1.50000
AFIX   0
N3    4    0.000000    0.058253    0.250000    10.50000    0.04181    0.01937 =
         0.02608    0.00000    0.00096    0.00000
AFIX  33
H3A   3    0.079046    0.023790    0.250282    10.50000   -1.50000
H3B   3   -0.034278    0.023790    0.316554    10.50000   -1.50000
H3C   3   -0.044768    0.023790    0.183165    10.50000   -1.50000
AFIX   0
N4    4    0.000000    0.510803    0.250000    10.50000    0.02708    0.02756 =
         0.02761    0.00000    0.00036    0.00000
O1    5    0.073670    0.585569    0.189990    11.00000    0.06613    0.01717 =
         0.05601    0.00542    0.01617   -0.00833
HKLF 4

REM  0.58
REM R1 =  0.0266 for     518 Fo > 4sig(Fo)  and  0.0303 for all     569 data
REM     52 parameters refined using      0 restraints

END

WGHT      0.0284      1.2770

REM Highest difference peak  0.310,  deepest hole -0.339,  1-sigma level  0.083
Q1    1   0.0993  0.6203  0.2897  11.00000  0.05    0.31
Q2    1   0.2222  0.2452  0.3104  11.00000  0.05    0.31
Q3    1   0.4054  0.6125  0.5408  11.00000  0.05    0.31
Q4    1   0.0820  0.4018  0.2728  11.00000  0.05    0.28
Q5    1   0.4056  0.5496  0.4551  11.00000  0.05    0.27
Q6    1   0.3109  0.4127  0.5875  11.00000  0.05    0.26
Q7    1   0.0033  0.3244  0.4855  11.00000  0.05    0.25
Q8    1   0.0666  0.1922  0.5205  11.00000  0.05    0.25
Q9    1   0.1424  0.3029  0.3169  11.00000  0.05    0.25
Q10   1  -0.0657  0.3063  0.3263  11.00000  0.05    0.25
;
_shelx_res_checksum              3722
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_097GPa
_database_code_depnum_ccdc_archive 'CCDC 1423457'
_audit_update_record             
;
2015-09-10 deposited with the CCDC.
2015-10-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        nitro-pentaammine-Co(III)-dibromide
_chemical_name_common            nitro-pentaammine-Co(III)-dibromide
_chemical_melting_point          ?
_chemical_formula_moiety         'Co H15 N6 O2, 2(Br)'
_chemical_formula_sum            'Br2 Co H15 N6 O2'
_chemical_formula_weight         349.93

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

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'

_cell_length_a                   10.6243(5)
_cell_length_b                   8.4030(8)
_cell_length_c                   10.9113(5)
_cell_angle_alpha                90
_cell_angle_beta                 94.483(4)
_cell_angle_gamma                90
_cell_volume                     971.14(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1835
_cell_measurement_theta_min      2.7930
_cell_measurement_theta_max      27.5720

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_preparation       'mounted in DAC'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.393
_exptl_crystal_F_000             680
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?

_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    9.969
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?

_exptl_absorpt_correction_type   Gaussian
_exptl_absorpt_correction_T_min  0.225
_exptl_absorpt_correction_T_max  0.293
_exptl_absorpt_process_details   'Absorb-7 (Angel, 2013)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      295(2)
_diffrn_ambient_pressure         970000
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a

_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 10.3457
_diffrn_reflns_number            2651
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_av_R_equivalents  0.0511
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.094
_diffrn_reflns_theta_max         26.312
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.565
_diffrn_measured_fraction_theta_full 0.579
_diffrn_reflns_Laue_measured_fraction_max 0.565
_diffrn_reflns_Laue_measured_fraction_full 0.579
_diffrn_reflns_point_group_measured_fraction_max 0.565
_diffrn_reflns_point_group_measured_fraction_full 0.579
_reflns_number_total             562
_reflns_number_gt                522
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_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_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_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'

_computing_molecular_graphics    'Mercury (Macrae et al., 2006)'
_computing_publication_material  'enCIFer (Allen et al., 2004)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0224P)²+0.5934P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         562
_refine_ls_number_parameters     52
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0240
_refine_ls_wR_factor_ref         0.0559
_refine_ls_wR_factor_gt          0.0531
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_restrained_S_all      1.118
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.29103(4) 0.51555(6) 0.49217(3) 0.02659(19) Uani 1 1 d . . . . .
Co1 Co 0.0000 0.28959(10) 0.2500 0.0174(2) Uani 1 2 d S T P . .
N1 N 0.1835(3) 0.2891(5) 0.2517(3) 0.0240(9) Uani 1 1 d . . . . .
H1A H 0.2112 0.1891 0.2519 0.036 Uiso 1 1 calc R U . . .
H1B H 0.2068 0.3389 0.1851 0.036 Uiso 1 1 calc R U . . .
H1C H 0.2162 0.3389 0.3187 0.036 Uiso 1 1 calc R U . . .
N2 N 0.0103(3) 0.2969(4) 0.4293(3) 0.0231(9) Uani 1 1 d . . . . .
H2A H 0.0120 0.1982 0.4590 0.035 Uiso 1 1 calc R U . . .
H2B H 0.0803 0.3479 0.4568 0.035 Uiso 1 1 calc R U . . .
H2C H -0.0567 0.3479 0.4539 0.035 Uiso 1 1 calc R U . . .
N3 N 0.0000 0.0518(7) 0.2500 0.0281(13) Uani 1 2 d S T P . .
H3A H 0.0790 0.0165 0.2507 0.042 Uiso 0.5 1 calc R U P . .
H3B H -0.0348 0.0165 0.3164 0.042 Uiso 0.5 1 calc R U P . .
H3C H -0.0442 0.0165 0.1828 0.042 Uiso 0.5 1 calc R U P . .
N4 N 0.0000 0.5162(7) 0.2500 0.0221(15) Uani 1 2 d S T P . .
O1 O 0.0747(3) 0.5929(5) 0.1897(3) 0.0439(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 0.0264(3) 0.0297(6) 0.0239(3) 0.00105(16) 0.0029(2) -0.00182(16)
Co1 0.0174(4) 0.0206(8) 0.0142(4) 0.000 0.0012(3) 0.000
N1 0.0236(19) 0.025(4) 0.023(2) -0.0026(14) 0.0004(16) -0.0001(14)
N2 0.0265(19) 0.024(4) 0.0188(19) 0.0012(13) 0.0032(16) -0.0027(14)
N3 0.033(3) 0.025(5) 0.026(3) 0.000 0.000(2) 0.000
N4 0.026(3) 0.016(6) 0.023(3) 0.000 -0.002(3) 0.000
O1 0.051(2) 0.035(4) 0.049(2) 0.0055(18) 0.0231(18) -0.0090(19)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 N4 1.904(6) . ?
Co1 N1 1.948(3) 2 ?
Co1 N1 1.948(3) . ?
Co1 N2 1.952(3) . ?
Co1 N2 1.952(3) 2 ?
Co1 N3 1.998(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 1.248(5) 2 ?
N4 O1 1.248(5) . ?

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
_geom_angle_publ_flag
N4 Co1 N1 90.13(12) . 2 ?
N4 Co1 N1 90.13(12) . . ?
N1 Co1 N1 179.7(2) 2 . ?
N4 Co1 N2 88.20(11) . . ?
N1 Co1 N2 89.27(13) 2 . ?
N1 Co1 N2 90.74(13) . . ?
N4 Co1 N2 88.20(11) . 2 ?
N1 Co1 N2 90.74(13) 2 2 ?
N1 Co1 N2 89.27(13) . 2 ?
N2 Co1 N2 176.4(2) . 2 ?
N4 Co1 N3 180.0 . . ?
N1 Co1 N3 89.87(12) 2 . ?
N1 Co1 N3 89.87(12) . . ?
N2 Co1 N3 91.80(11) . . ?
N2 Co1 N3 91.80(11) 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 117.8(7) 2 . ?
O1 N4 Co1 121.1(4) 2 . ?
O1 N4 Co1 121.1(4) . . ?


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 2.45 3.078(4) 127.8 4_545
N1 H1B Br1 0.89 2.65 3.539(3) 176.4 6_565
N1 H1C Br1 0.89 2.49 3.368(3) 171.1 .
N2 H2A Br1 0.89 2.78 3.435(3) 131.8 7_556
N2 H2A Br1 0.89 2.85 3.426(3) 123.6 3_445
N2 H2B Br1 0.89 2.65 3.524(3) 168.6 .
N2 H2C Br1 0.89 2.84 3.728(3) 172.0 5_566
N3 H3B Br1 0.89 2.77 3.5946(7) 155.3 3_445
N3 H3C Br1 0.89 2.63 3.4910(10) 164.4 8_455

_refine_diff_density_max         0.325
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.078

_shelx_res_file                  
;

    _0.97GPa.res created by SHELXL-2014/7

TITL 0.97
CELL  0.71073 10.62430  8.40300 10.91130 90.00000 94.48300 90.00000
ZERR 4  0.00050  0.00080  0.00050  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    0.022400    0.593400
FVAR       2.22518
BR1   1    0.291034    0.515548    0.492174    11.00000    0.02638    0.02967 =
         0.02386    0.00105    0.00287   -0.00182
CO1   2    0.000000    0.289588    0.250000    10.50000    0.01737    0.02055 =
         0.01424    0.00000    0.00116    0.00000
N1    4    0.183466    0.289072    0.251671    11.00000    0.02356    0.02524 =
         0.02310   -0.00256    0.00036   -0.00010
AFIX  33
H1A   3    0.211232    0.189137    0.251924    11.00000   -1.50000
H1B   3    0.206773    0.338922    0.185126    11.00000   -1.50000
H1C   3    0.216220    0.338922    0.318727    11.00000   -1.50000
AFIX   0
N2    4    0.010324    0.296866    0.429319    11.00000    0.02650    0.02410 =
         0.01885    0.00115    0.00321   -0.00269
AFIX  33
H2A   3    0.012032    0.198164    0.458987    11.00000   -1.50000
H2B   3    0.080324    0.347876    0.456844    11.00000   -1.50000
H2C   3   -0.056677    0.347876    0.453882    11.00000   -1.50000
AFIX   0
N3    4    0.000000    0.051827    0.250000    10.50000    0.03338    0.02454 =
         0.02591    0.00000   -0.00038    0.00000
AFIX  33
H3A   3    0.079034    0.016522    0.250720    10.50000   -1.50000
H3B   3   -0.034793    0.016522    0.316440    10.50000   -1.50000
H3C   3   -0.044241    0.016522    0.182839    10.50000   -1.50000
AFIX   0
N4    4    0.000000    0.516157    0.250000    10.50000    0.02645    0.01590 =
         0.02348    0.00000   -0.00160    0.00000
O1    5    0.074656    0.592864    0.189735    11.00000    0.05052    0.03509 =
         0.04911    0.00553    0.02309   -0.00897
HKLF 4

REM  0.97
REM R1 =  0.0240 for     522 Fo > 4sig(Fo)  and  0.0273 for all     562 data
REM     52 parameters refined using      0 restraints

END

WGHT      0.0224      0.5934

REM Highest difference peak  0.325,  deepest hole -0.318,  1-sigma level  0.078
Q1    1   0.2234  0.2132  0.3167  11.00000  0.05    0.32
Q2    1   0.0954  0.1500  0.4482  11.00000  0.05    0.29
Q3    1   0.0937  0.3554  0.3389  11.00000  0.05    0.27
Q4    1   0.1247  0.6919  0.1748  11.00000  0.05    0.24
Q5    1   0.1179 -0.0890  0.1934  11.00000  0.05    0.23
Q6    1   0.0995  0.1991  0.3462  11.00000  0.05    0.23
Q7    1   0.1850  0.1905  0.1811  11.00000  0.05    0.23
Q8    1   0.1171  0.4436  0.2586  11.00000  0.05    0.23
Q9    1   0.0999  0.2962  0.1705  11.00000  0.05    0.22
Q10   1   0.2141  0.6059  0.3914  11.00000  0.05    0.22
;
_shelx_res_checksum              65192
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_161GPa
_database_code_depnum_ccdc_archive 'CCDC 1423458'
_audit_update_record             
;
2015-09-10 deposited with the CCDC.
2015-10-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        nitro-pentaammine-Co(III)-dibromide
_chemical_name_common            nitro-pentaammine-Co(III)-dibromide
_chemical_melting_point          ?
_chemical_formula_moiety         'Co H15 N6 O2, 2(Br)'
_chemical_formula_sum            'Br2 Co H15 N6 O2'
_chemical_formula_weight         349.93

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

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'

_cell_length_a                   10.6792(4)
_cell_length_b                   8.0977(7)
_cell_length_c                   10.9004(4)
_cell_angle_alpha                90
_cell_angle_beta                 94.192(4)
_cell_angle_gamma                90
_cell_volume                     940.11(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1813
_cell_measurement_theta_min      3.1630
_cell_measurement_theta_max      27.7470

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_preparation       'mounted in DAC'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.472
_exptl_crystal_F_000             680
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?

_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    10.297
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?

_exptl_absorpt_correction_type   Gaussian
_exptl_absorpt_correction_T_min  0.219
_exptl_absorpt_correction_T_max  0.288
_exptl_absorpt_process_details   'Absorb-7 (Angel, 2013)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      295(2)
_diffrn_ambient_pressure         1610000
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a

_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 10.3457
_diffrn_reflns_number            2485
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_av_R_equivalents  0.0550
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.160
_diffrn_reflns_theta_max         26.346
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.548
_diffrn_measured_fraction_theta_full 0.561
_diffrn_reflns_Laue_measured_fraction_max 0.548
_diffrn_reflns_Laue_measured_fraction_full 0.561
_diffrn_reflns_point_group_measured_fraction_max 0.548
_diffrn_reflns_point_group_measured_fraction_full 0.561
_reflns_number_total             528
_reflns_number_gt                490
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_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_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_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'

_computing_molecular_graphics    'Mercury (Macrae et al., 2006)'
_computing_publication_material  'enCIFer (Allen et al., 2004)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0134P)²+3.2923P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         528
_refine_ls_number_parameters     52
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0239
_refine_ls_wR_factor_ref         0.0525
_refine_ls_wR_factor_gt          0.0507
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.29041(4) 0.51403(6) 0.49349(4) 0.02305(19) Uani 1 1 d . . . . .
Co1 Co 0.0000 0.29045(11) 0.2500 0.0148(2) Uani 1 2 d S T P . .
N1 N 0.1818(3) 0.2897(6) 0.2515(3) 0.0229(10) Uani 1 1 d . . . . .
H1A H 0.2094 0.1860 0.2517 0.034 Uiso 1 1 calc R U . . .
H1B H 0.2053 0.3414 0.1848 0.034 Uiso 1 1 calc R U . . .
H1C H 0.2142 0.3414 0.3185 0.034 Uiso 1 1 calc R U . . .
N2 N 0.0085(3) 0.2993(5) 0.4295(3) 0.0197(9) Uani 1 1 d . . . . .
H2A H 0.0099 0.1971 0.4596 0.029 Uiso 1 1 calc R U . . .
H2B H 0.0778 0.3524 0.4572 0.029 Uiso 1 1 calc R U . . .
H2C H -0.0585 0.3524 0.4536 0.029 Uiso 1 1 calc R U . . .
N3 N 0.0000 0.0454(8) 0.2500 0.0247(14) Uani 1 2 d S T P . .
H3A H -0.0786 0.0088 0.2494 0.037 Uiso 0.5 1 calc R U P . .
H3B H 0.0349 0.0088 0.1835 0.037 Uiso 0.5 1 calc R U P . .
H3C H 0.0437 0.0088 0.3172 0.037 Uiso 0.5 1 calc R U P . .
N4 N 0.0000 0.5256(8) 0.2500 0.0204(16) Uani 1 2 d S T P . .
O1 O 0.0757(3) 0.6063(6) 0.1918(3) 0.0375(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 0.0238(3) 0.0242(5) 0.0214(3) 0.00104(17) 0.0028(2) -0.00169(18)
Co1 0.0143(4) 0.0172(9) 0.0130(4) 0.000 0.0015(3) 0.000
N1 0.017(2) 0.032(4) 0.020(2) -0.0017(15) 0.0040(16) 0.0052(16)
N2 0.020(2) 0.023(4) 0.0169(19) 0.0015(14) 0.0042(16) -0.0045(15)
N3 0.032(3) 0.019(6) 0.023(3) 0.000 -0.001(3) 0.000
N4 0.020(3) 0.023(7) 0.019(3) 0.000 0.001(3) 0.000
O1 0.042(2) 0.029(5) 0.044(2) 0.0065(18) 0.0203(19) -0.0072(19)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 N4 1.904(7) . ?
Co1 N1 1.940(3) . ?
Co1 N1 1.940(3) 2 ?
Co1 N2 1.954(3) . ?
Co1 N2 1.954(3) 2 ?
Co1 N3 1.984(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 1.248(5) 2 ?
N4 O1 1.248(5) . ?

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
_geom_angle_publ_flag
N4 Co1 N1 90.18(14) . . ?
N4 Co1 N1 90.18(14) . 2 ?
N1 Co1 N1 179.6(3) . 2 ?
N4 Co1 N2 87.90(13) . . ?
N1 Co1 N2 91.09(14) . . ?
N1 Co1 N2 88.93(14) 2 . ?
N4 Co1 N2 87.90(13) . 2 ?
N1 Co1 N2 88.93(14) . 2 ?
N1 Co1 N2 91.08(14) 2 2 ?
N2 Co1 N2 175.8(3) . 2 ?
N4 Co1 N3 180.0 . . ?
N1 Co1 N3 89.82(14) . . ?
N1 Co1 N3 89.82(14) 2 . ?
N2 Co1 N3 92.10(13) . . ?
N2 Co1 N3 92.10(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 116.8(8) 2 . ?
O1 N4 Co1 121.6(4) 2 . ?
O1 N4 Co1 121.6(4) . . ?


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 2.42 3.010(5) 124.0 4_545
N1 H1B Br1 0.89 2.61 3.501(4) 176.0 6_565
N1 H1C Br1 0.89 2.46 3.340(4) 173.1 .
N2 H2A Br1 0.89 2.75 3.390(4) 129.7 7_556
N2 H2A Br1 0.89 2.82 3.388(4) 123.0 3_445
N2 H2B Br1 0.89 2.63 3.503(3) 168.9 .
N2 H2C Br1 0.89 2.80 3.683(4) 171.3 5_566
N3 H3A Br1 0.89 3.10 3.6038(6) 118.3 3_445
N3 H3A Br1 0.89 3.03 3.4849(10) 113.5 8_455

_refine_diff_density_max         0.311
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.080

_shelx_res_file                  
;

    _1.61GPa.res created by SHELXL-2014/7

TITL 1.61
CELL  0.71073 10.67920  8.09770 10.90040 90.00000 94.19200 90.00000
ZERR 4  0.00040  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    0.013400    3.292300
FVAR       2.25566
BR1   1    0.290410    0.514032    0.493490    11.00000    0.02379    0.02417 =
         0.02137    0.00104    0.00279   -0.00169
CO1   2    0.000000    0.290452    0.250000    10.50000    0.01431    0.01718 =
         0.01304    0.00000    0.00148    0.00000
N1    4    0.181806    0.289690    0.251461    11.00000    0.01724    0.03208 =
         0.01971   -0.00173    0.00401    0.00524
AFIX  33
H1A   3    0.209351    0.185952    0.251683    11.00000   -1.50000
H1B   3    0.205296    0.341384    0.184843    11.00000   -1.50000
H1C   3    0.214157    0.341384    0.318528    11.00000   -1.50000
AFIX   0
N2    4    0.008456    0.299287    0.429531    11.00000    0.01965    0.02279 =
         0.01694    0.00149    0.00425   -0.00449
AFIX  33
H2A   3    0.009873    0.197076    0.459617    11.00000   -1.50000
H2B   3    0.077829    0.352404    0.457185    11.00000   -1.50000
H2C   3   -0.058483    0.352404    0.453573    11.00000   -1.50000
AFIX   0
N3    4    0.000000    0.045408    0.250000    10.50000    0.03194    0.01932 =
         0.02260    0.00000   -0.00052    0.00000
AFIX  33
H3A   3   -0.078618    0.008772    0.249368    10.50000   -1.50000
H3B   3    0.034879    0.008772    0.183474    10.50000   -1.50000
H3C   3    0.043739    0.008772    0.317158    10.50000   -1.50000
AFIX   0
N4    4    0.000000    0.525554    0.250000    10.50000    0.01969    0.02270 =
         0.01874    0.00000    0.00149    0.00000
O1    5    0.075670    0.606292    0.191755    11.00000    0.04195    0.02853 =
         0.04450    0.00647    0.02032   -0.00718
HKLF 4

REM  1.61
REM R1 =  0.0239 for     490 Fo > 4sig(Fo)  and  0.0270 for all     528 data
REM     52 parameters refined using      0 restraints

END

WGHT      0.0134      3.2923

REM Highest difference peak  0.311,  deepest hole -0.454,  1-sigma level  0.080
Q1    1   0.1914  0.1995  0.1798  11.00000  0.05    0.31
Q2    1   0.2540  0.2337  0.3326  11.00000  0.05    0.24
Q3    1   0.1075  0.5777  0.2629  11.00000  0.05    0.23
Q4    1  -0.1029  0.4148  0.5099  11.00000  0.05    0.23
Q5    1   0.1193  0.1076  0.3182  11.00000  0.05    0.23
Q6    1  -0.1154  0.4740  0.4916  11.00000  0.05    0.23
Q7    1  -0.0795  0.4079  0.2976  11.00000  0.05    0.22
Q8    1   0.0624  0.3306  0.3685  11.00000  0.05    0.22
Q9    1  -0.0678  0.1656  0.4495  11.00000  0.05    0.22
Q10   1   0.1334  0.4521  0.2451  11.00000  0.05    0.22
;
_shelx_res_checksum              33492
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_260GPa
_database_code_depnum_ccdc_archive 'CCDC 1423459'
_audit_update_record             
;
2015-09-10 deposited with the CCDC.
2015-10-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        nitro-pentaammine-Co(III)-dibromide
_chemical_name_common            nitro-pentaammine-Co(III)-dibromide
_chemical_melting_point          ?
_chemical_formula_moiety         'Co H15 N6 O2, 2(Br)'
_chemical_formula_sum            'Br2 Co H15 N6 O2'
_chemical_formula_weight         349.93

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

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'

_cell_length_a                   10.6750(5)
_cell_length_b                   7.8148(8)
_cell_length_c                   10.8204(4)
_cell_angle_alpha                90
_cell_angle_beta                 93.829(4)
_cell_angle_gamma                90
_cell_volume                     900.66(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1806
_cell_measurement_theta_min      2.7960
_cell_measurement_theta_max      27.7170

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_preparation       'mounted in DAC'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.581
_exptl_crystal_F_000             680
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?

_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    10.749
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?

_exptl_absorpt_correction_type   Gaussian
_exptl_absorpt_correction_T_min  0.215
_exptl_absorpt_correction_T_max  0.282
_exptl_absorpt_process_details   'Absorb-7 (Angel, 2013)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      295(2)
_diffrn_ambient_pressure         2600000
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a

_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 10.3457
_diffrn_reflns_number            2359
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_av_R_equivalents  0.0560
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.233
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.541
_diffrn_measured_fraction_theta_full 0.554
_diffrn_reflns_Laue_measured_fraction_max 0.541
_diffrn_reflns_Laue_measured_fraction_full 0.554
_diffrn_reflns_point_group_measured_fraction_max 0.541
_diffrn_reflns_point_group_measured_fraction_full 0.554
_reflns_number_total             502
_reflns_number_gt                457
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_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_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_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'

_computing_molecular_graphics    'Mercury (Macrae et al., 2006)'
_computing_publication_material  'enCIFer (Allen et al., 2004)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0211P)²+0.8807P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         502
_refine_ls_number_parameters     52
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0231
_refine_ls_wR_factor_ref         0.0551
_refine_ls_wR_factor_gt          0.0525
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_restrained_S_all      1.108
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.28966(4) 0.51218(6) 0.49484(3) 0.0194(2) Uani 1 1 d . . . . .
Co1 Co 0.0000 0.29134(11) 0.2500 0.0120(3) Uani 1 2 d S T P . .
N1 N 0.1818(3) 0.2904(5) 0.2515(3) 0.0180(9) Uani 1 1 d . . . . .
H1A H 0.2093 0.1829 0.2518 0.027 Uiso 1 1 calc R U . . .
H1B H 0.2058 0.3439 0.1845 0.027 Uiso 1 1 calc R U . . .
H1C H 0.2137 0.3439 0.3191 0.027 Uiso 1 1 calc R U . . .
N2 N 0.0072(3) 0.3006(5) 0.4297(3) 0.0163(9) Uani 1 1 d . . . . .
H2A H 0.0084 0.1947 0.4600 0.024 Uiso 1 1 calc R U . . .
H2B H 0.0764 0.3557 0.4575 0.024 Uiso 1 1 calc R U . . .
H2C H -0.0600 0.3557 0.4538 0.024 Uiso 1 1 calc R U . . .
N3 N 0.0000 0.0394(7) 0.2500 0.0190(13) Uani 1 2 d S T P . .
H3A H -0.0786 0.0014 0.2493 0.029 Uiso 0.5 1 calc R U P . .
H3B H 0.0354 0.0014 0.1830 0.029 Uiso 0.5 1 calc R U P . .
H3C H 0.0433 0.0014 0.3176 0.029 Uiso 0.5 1 calc R U P . .
N4 N 0.0000 0.5363(8) 0.2500 0.0171(16) Uani 1 2 d S T P . .
O1 O 0.0772(3) 0.6186(6) 0.1930(3) 0.0325(11) 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 0.0208(3) 0.0185(6) 0.0191(3) 0.00108(15) 0.0026(2) -0.00103(16)
Co1 0.0124(4) 0.0118(9) 0.0119(4) 0.000 0.0005(3) 0.000
N1 0.0187(19) 0.017(4) 0.0182(18) 0.0006(14) -0.0018(15) 0.0056(14)
N2 0.0165(19) 0.016(4) 0.0161(18) 0.0003(14) 0.0023(15) -0.0008(14)
N3 0.027(3) 0.010(6) 0.020(3) 0.000 0.002(2) 0.000
N4 0.013(3) 0.026(7) 0.012(3) 0.000 -0.001(3) 0.000
O1 0.036(2) 0.025(4) 0.039(2) 0.0030(16) 0.0175(16) -0.0070(17)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 N4 1.914(6) . ?
Co1 N1 1.939(3) . ?
Co1 N1 1.939(3) 2 ?
Co1 N2 1.942(3) . ?
Co1 N2 1.942(3) 2 ?
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 1.242(5) 2 ?
N4 O1 1.242(5) . ?

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
_geom_angle_publ_flag
N4 Co1 N1 90.22(12) . . ?
N4 Co1 N1 90.22(12) . 2 ?
N1 Co1 N1 179.6(2) . 2 ?
N4 Co1 N2 87.87(11) . . ?
N1 Co1 N2 91.09(13) . . ?
N1 Co1 N2 88.93(13) 2 . ?
N4 Co1 N2 87.87(11) . 2 ?
N1 Co1 N2 88.92(13) . 2 ?
N1 Co1 N2 91.09(13) 2 2 ?
N2 Co1 N2 175.7(2) . 2 ?
N4 Co1 N3 180.0 . . ?
N1 Co1 N3 89.78(12) . . ?
N1 Co1 N3 89.78(12) 2 . ?
N2 Co1 N3 92.13(11) . . ?
N2 Co1 N3 92.13(11) 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 117.6(7) 2 . ?
O1 N4 Co1 121.2(3) 2 . ?
O1 N4 Co1 121.2(3) . . ?


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 2.37 2.928(5) 120.8 4_545
N1 H1B Br1 0.89 2.55 3.442(4) 176.0 6_565
N1 H1C Br1 0.89 2.41 3.295(3) 174.7 .
N2 H2A Br1 0.89 2.71 3.333(3) 127.8 7_556
N2 H2A Br1 0.89 2.78 3.345(3) 122.3 3_445
N2 H2B Br1 0.89 2.59 3.470(3) 168.9 .
N2 H2C Br1 0.89 2.75 3.632(3) 170.7 5_566
N3 H3A Br1 0.89 3.09 3.5917(5) 117.9 3_445
N3 H3A Br1 0.89 3.01 3.4640(8) 113.7 8_455

_refine_diff_density_max         0.301
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.080

_shelx_res_file                  
;

    _2.60GPa.res created by SHELXL-2014/7

TITL 2.60
CELL  0.71073 10.67500  7.81480 10.82040 90.00000 93.82900 90.00000
ZERR 4  0.00050  0.00080  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    0.021100    0.880700
FVAR       2.32726
BR1   1    0.289655    0.512180    0.494837    11.00000    0.02082    0.01851 =
         0.01915    0.00108    0.00264   -0.00103
CO1   2    0.000000    0.291339    0.250000    10.50000    0.01239    0.01183 =
         0.01187    0.00000    0.00047    0.00000
N1    4    0.181774    0.290380    0.251539    11.00000    0.01870    0.01680 =
         0.01815    0.00064   -0.00178    0.00563
AFIX  33
H1A   3    0.209276    0.182861    0.251772    11.00000   -1.50000
H1B   3    0.205759    0.343919    0.184470    11.00000   -1.50000
H1C   3    0.213704    0.343919    0.319082    11.00000   -1.50000
AFIX   0
N2    4    0.007164    0.300588    0.429670    11.00000    0.01653    0.01633 =
         0.01613    0.00035    0.00235   -0.00077
AFIX  33
H2A   3    0.008373    0.194702    0.460011    11.00000   -1.50000
H2B   3    0.076373    0.355651    0.457524    11.00000   -1.50000
H2C   3   -0.059972    0.355650    0.453823    11.00000   -1.50000
AFIX   0
N3    4    0.000000    0.039393    0.250000    10.50000    0.02724    0.00995 =
         0.01983    0.00000    0.00166    0.00000
AFIX  33
H3A   3   -0.078646    0.001431    0.249334    10.50000   -1.50000
H3B   3    0.035351    0.001431    0.183027    10.50000   -1.50000
H3C   3    0.043296    0.001431    0.317639    10.50000   -1.50000
AFIX   0
N4    4    0.000000    0.536311    0.250000    10.50000    0.01269    0.02584 =
         0.01248    0.00000   -0.00082    0.00000
O1    5    0.077228    0.618552    0.192972    11.00000    0.03556    0.02465 =
         0.03932    0.00297    0.01745   -0.00697
HKLF 4

REM  2.60
REM R1 =  0.0231 for     457 Fo > 4sig(Fo)  and  0.0266 for all     502 data
REM     52 parameters refined using      0 restraints

END

WGHT      0.0211      0.8807

REM Highest difference peak  0.301,  deepest hole -0.350,  1-sigma level  0.080
Q1    1   0.2009  0.2250  0.3038  11.00000  0.05    0.30
Q2    1   0.0000 -0.0201  0.2500  10.50000  0.05    0.30
Q3    1   0.2782  0.0696  0.1626  11.00000  0.05    0.27
Q4    1   0.3075  0.3066  0.2278  11.00000  0.05    0.26
Q5    1   0.1999  0.2323  0.1823  11.00000  0.05    0.26
Q6    1   0.1775  0.5468  0.2223  11.00000  0.05    0.25
Q7    1   0.1345  0.3392  0.2487  11.00000  0.05    0.24
Q8    1   0.0868  0.4048  0.2688  11.00000  0.05    0.24
Q9    1   0.1935  0.6673  0.4018  11.00000  0.05    0.23
Q10   1   0.0851  0.6793  0.3348  11.00000  0.05    0.23
;
_shelx_res_checksum              15214
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_330GPa
_database_code_depnum_ccdc_archive 'CCDC 1423460'
_audit_update_record             
;
2015-09-10 deposited with the CCDC.
2015-10-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        nitro-pentaammine-Co(III)-dibromide
_chemical_name_common            nitro-pentaammine-Co(III)-dibromide
_chemical_melting_point          ?
_chemical_formula_moiety         'Co H15 N6 O2, 2(Br)'
_chemical_formula_sum            'Br2 Co H15 N6 O2'
_chemical_formula_weight         349.93

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

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'

_cell_length_a                   10.6557(4)
_cell_length_b                   7.7006(7)
_cell_length_c                   10.7594(4)
_cell_angle_alpha                90
_cell_angle_beta                 93.693(4)
_cell_angle_gamma                90
_cell_volume                     881.03(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1745
_cell_measurement_theta_min      2.7930
_cell_measurement_theta_max      28.0120

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_preparation       'mounted in DAC'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.638
_exptl_crystal_F_000             680
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?

_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    10.988
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?

_exptl_absorpt_correction_type   Gaussian
_exptl_absorpt_correction_T_min  0.212
_exptl_absorpt_correction_T_max  0.279
_exptl_absorpt_process_details   'Absorb-7 (Angel, 2013)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      295(2)
_diffrn_ambient_pressure         3300000
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a

_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 10.3457
_diffrn_reflns_number            1398
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.716
_diffrn_reflns_theta_max         26.326
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.535
_diffrn_measured_fraction_theta_full 0.546
_diffrn_reflns_Laue_measured_fraction_max 0.535
_diffrn_reflns_Laue_measured_fraction_full 0.546
_diffrn_reflns_point_group_measured_fraction_max 0.535
_diffrn_reflns_point_group_measured_fraction_full 0.546
_reflns_number_total             484
_reflns_number_gt                439
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_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_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_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'

_computing_molecular_graphics    'Mercury (Macrae et al., 2006)'
_computing_publication_material  'enCIFer (Allen et al., 2004)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0104P)²+2.0207P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         484
_refine_ls_number_parameters     52
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0249
_refine_ls_wR_factor_ref         0.0512
_refine_ls_wR_factor_gt          0.0492
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_restrained_S_all      1.118
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.28944(4) 0.51148(7) 0.49537(4) 0.01797(19) Uani 1 1 d . . . . .
Co1 Co 0.0000 0.29157(13) 0.2500 0.0110(3) Uani 1 2 d S T P . .
N1 N 0.1815(3) 0.2896(6) 0.2522(3) 0.0161(10) Uani 1 1 d . . . . .
H1A H 0.2087 0.1804 0.2525 0.024 Uiso 1 1 calc R U . . .
H1B H 0.2061 0.3438 0.1848 0.024 Uiso 1 1 calc R U . . .
H1C H 0.2132 0.3438 0.3202 0.024 Uiso 1 1 calc R U . . .
N2 N 0.0066(3) 0.3012(6) 0.4305(3) 0.0136(9) Uani 1 1 d . . . . .
H2A H 0.0077 0.1938 0.4611 0.020 Uiso 1 1 calc R U . . .
H2B H 0.0758 0.3572 0.4585 0.020 Uiso 1 1 calc R U . . .
H2C H -0.0607 0.3572 0.4546 0.020 Uiso 1 1 calc R U . . .
N3 N 0.0000 0.0368(8) 0.2500 0.0174(14) Uani 1 2 d S T P . .
H3A H -0.0788 -0.0018 0.2491 0.026 Uiso 0.5 1 calc R U P . .
H3B H 0.0358 -0.0018 0.1828 0.026 Uiso 0.5 1 calc R U P . .
H3C H 0.0430 -0.0018 0.3181 0.026 Uiso 0.5 1 calc R U P . .
N4 N 0.0000 0.5393(9) 0.2500 0.0140(16) Uani 1 2 d S T P . .
O1 O 0.0781(3) 0.6232(6) 0.1933(3) 0.0317(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 0.0187(3) 0.0177(5) 0.0177(3) 0.00115(19) 0.0029(2) -0.00070(19)
Co1 0.0115(5) 0.0099(9) 0.0116(5) 0.000 0.0006(4) 0.000
N1 0.019(2) 0.012(4) 0.017(2) -0.0032(15) -0.0032(17) -0.0012(16)
N2 0.015(2) 0.009(4) 0.016(2) 0.0013(15) 0.0006(17) 0.0004(15)
N3 0.022(4) 0.010(6) 0.020(3) 0.000 -0.001(3) 0.000
N4 0.015(4) 0.012(7) 0.015(3) 0.000 0.003(3) 0.000
O1 0.026(2) 0.036(5) 0.036(2) 0.0027(18) 0.0214(18) -0.0075(18)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 N4 1.908(7) . ?
Co1 N1 1.932(3) . ?
Co1 N1 1.932(3) 2 ?
Co1 N2 1.940(3) 2 ?
Co1 N2 1.940(3) . ?
Co1 N3 1.962(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 1.244(5) 2 ?
N4 O1 1.244(5) . ?

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
_geom_angle_publ_flag
N4 Co1 N1 90.44(14) . . ?
N4 Co1 N1 90.44(14) . 2 ?
N1 Co1 N1 179.1(3) . 2 ?
N4 Co1 N2 87.80(13) . 2 ?
N1 Co1 N2 89.09(15) . 2 ?
N1 Co1 N2 90.95(15) 2 2 ?
N4 Co1 N2 87.80(13) . . ?
N1 Co1 N2 90.95(15) . . ?
N1 Co1 N2 89.09(15) 2 . ?
N2 Co1 N2 175.6(3) 2 . ?
N4 Co1 N3 180.0 . . ?
N1 Co1 N3 89.56(14) . . ?
N1 Co1 N3 89.56(14) 2 . ?
N2 Co1 N3 92.20(13) 2 . ?
N2 Co1 N3 92.20(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 117.5(7) 2 . ?
O1 N4 Co1 121.3(4) 2 . ?
O1 N4 Co1 121.3(4) . . ?


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 2.35 2.890(5) 119.2 4_545
N1 H1B Br1 0.89 2.53 3.422(4) 176.4 6_565
N1 H1C Br1 0.89 2.38 3.271(4) 175.0 .
N2 H2A Br1 0.89 2.69 3.307(4) 126.9 7_556
N2 H2A Br1 0.89 2.76 3.321(4) 122.0 3_445
N2 H2B Br1 0.89 2.58 3.453(4) 168.7 .
N2 H2C Br1 0.89 2.72 3.604(4) 170.3 5_566
N3 H3A Br1 0.89 3.08 3.5784(6) 117.5 3_445
N3 H3A Br1 0.89 2.99 3.4476(8) 114.0 8_455

_refine_diff_density_max         0.318
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.085

_shelx_res_file                  
;

    _3.30GPa.res created by SHELXL-2014/7

TITL 3.30
CELL  0.71073 10.65570  7.70060 10.75940 90.00000 93.69300 90.00000
ZERR 4  0.00040  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    0.010400    2.020700
FVAR       2.35642
BR1   1    0.289437    0.511485    0.495368    11.00000    0.01871    0.01773 =
         0.01770    0.00115    0.00291   -0.00070
CO1   2    0.000000    0.291568    0.250000    10.50000    0.01150    0.00986 =
         0.01156    0.00000    0.00061    0.00000
N1    4    0.181471    0.289637    0.252166    11.00000    0.01889    0.01182 =
         0.01702   -0.00321   -0.00316   -0.00115
AFIX  33
H1A   3    0.208725    0.180378    0.252491    11.00000   -1.50000
H1B   3    0.206053    0.343822    0.184827    11.00000   -1.50000
H1C   3    0.213215    0.343822    0.320177    11.00000   -1.50000
AFIX   0
N2    4    0.006592    0.301235    0.430459    11.00000    0.01550    0.00932 =
         0.01587    0.00133    0.00056    0.00035
AFIX  33
H2A   3    0.007710    0.193828    0.461055    11.00000   -1.50000
H2B   3    0.075840    0.357156    0.458472    11.00000   -1.50000
H2C   3   -0.060748    0.357156    0.454644    11.00000   -1.50000
AFIX   0
N3    4    0.000000    0.036770    0.250000    10.50000    0.02199    0.00960 =
         0.02021    0.00000   -0.00088    0.00000
AFIX  33
H3A   3   -0.078802   -0.001755    0.249059    10.50000   -1.50000
H3B   3    0.035820   -0.001755    0.182795    10.50000   -1.50000
H3C   3    0.042982   -0.001755    0.318145    10.50000   -1.50000
AFIX   0
N4    4    0.000000    0.539291    0.250000    10.50000    0.01476    0.01210 =
         0.01549    0.00000    0.00258    0.00000
O1    5    0.078150    0.623161    0.193329    11.00000    0.02562    0.03611 =
         0.03598    0.00266    0.02142   -0.00746
HKLF 4

REM  3.30
REM R1 =  0.0249 for     439 Fo > 4sig(Fo)  and  0.0292 for all     484 data
REM     52 parameters refined using      0 restraints

END

WGHT      0.0104      2.0207

REM Highest difference peak  0.318,  deepest hole -0.322,  1-sigma level  0.085
Q1    1   0.1988  0.2265  0.3012  11.00000  0.05    0.32
Q2    1   0.1814  0.2163  0.1903  11.00000  0.05    0.31
Q3    1   0.2035  0.2746  0.0773  11.00000  0.05    0.30
Q4    1   0.0447  0.7207  0.1111  11.00000  0.05    0.27
Q5    1  -0.0228  0.4995  0.4920  11.00000  0.05    0.27
Q6    1   0.2009  0.4352  0.4288  11.00000  0.05    0.24
Q7    1   0.2443  0.5934  0.4172  11.00000  0.05    0.24
Q8    1   0.1463  0.4685  0.3128  11.00000  0.05    0.24
Q9    1   0.1801  0.2764  0.5729  11.00000  0.05    0.24
Q10   1   0.2379  0.3672  0.2613  11.00000  0.05    0.24
;
_shelx_res_checksum              98258
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_380GPa
_database_code_depnum_ccdc_archive 'CCDC 1423461'
_audit_update_record             
;
2015-09-10 deposited with the CCDC.
2015-10-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        nitro-pentaammine-Co(III)-dibromide
_chemical_name_common            nitro-pentaammine-Co(III)-dibromide
_chemical_melting_point          ?
_chemical_formula_moiety         'Co H15 N6 O2, 2(Br)'
_chemical_formula_sum            'Br2 Co H15 N6 O2'
_chemical_formula_weight         349.93

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

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'

_cell_length_a                   10.6379(4)
_cell_length_b                   7.6361(6)
_cell_length_c                   10.7112(3)
_cell_angle_alpha                90
_cell_angle_beta                 93.601(3)
_cell_angle_gamma                90
_cell_volume                     868.38(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1743
_cell_measurement_theta_min      2.8030
_cell_measurement_theta_max      28.1760

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_preparation       'mounted in DAC'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.677
_exptl_crystal_F_000             680
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?

_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    11.148
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?

_exptl_absorpt_correction_type   Gaussian
_exptl_absorpt_correction_T_min  0.210
_exptl_absorpt_correction_T_max  0.277
_exptl_absorpt_process_details   'Absorb-7 (Angel, 2013)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      295(2)
_diffrn_ambient_pressure         3800000
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a

_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 10.3457
_diffrn_reflns_number            1833
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.286
_diffrn_reflns_theta_max         26.365
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.533
_diffrn_measured_fraction_theta_full 0.541
_diffrn_reflns_Laue_measured_fraction_max 0.533
_diffrn_reflns_Laue_measured_fraction_full 0.541
_diffrn_reflns_point_group_measured_fraction_max 0.533
_diffrn_reflns_point_group_measured_fraction_full 0.541
_reflns_number_total             478
_reflns_number_gt                443
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_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_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_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'

_computing_molecular_graphics    'Mercury (Macrae et al., 2006)'
_computing_publication_material  'enCIFer (Allen et al., 2004)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0210P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         478
_refine_ls_number_parameters     52
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0224
_refine_ls_wR_factor_ref         0.0498
_refine_ls_wR_factor_gt          0.0487
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
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)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
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_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
_geom_angle_publ_flag
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_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

_refine_diff_density_max         0.329
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.082

_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
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_440GPa
_database_code_depnum_ccdc_archive 'CCDC 1423462'
_audit_update_record             
;
2015-09-10 deposited with the CCDC.
2015-10-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        nitro-pentaammine-Co(III)-dibromide
_chemical_name_common            nitro-pentaammine-Co(III)-dibromide
_chemical_melting_point          ?
_chemical_formula_moiety         'Co H15 N6 O2, 2(Br)'
_chemical_formula_sum            'Br2 Co H15 N6 O2'
_chemical_formula_weight         349.93

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

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'

_cell_length_a                   10.6148(4)
_cell_length_b                   7.5680(7)
_cell_length_c                   10.6476(4)
_cell_angle_alpha                90
_cell_angle_beta                 93.508(3)
_cell_angle_gamma                90
_cell_volume                     853.75(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1712
_cell_measurement_theta_min      2.6350
_cell_measurement_theta_max      28.1830

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_preparation       'mounted in DAC'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.722
_exptl_crystal_F_000             680
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?

_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    11.339
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?

_exptl_absorpt_correction_type   Gaussian
_exptl_absorpt_correction_T_min  0.208
_exptl_absorpt_correction_T_max  0.274
_exptl_absorpt_process_details   'Absorb-7 (Angel, 2013)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      295(2)
_diffrn_ambient_pressure         4400000
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a

_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 10.3457
_diffrn_reflns_number            2262
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.308
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.557
_diffrn_measured_fraction_theta_full 0.570
_diffrn_reflns_Laue_measured_fraction_max 0.557
_diffrn_reflns_Laue_measured_fraction_full 0.570
_diffrn_reflns_point_group_measured_fraction_max 0.557
_diffrn_reflns_point_group_measured_fraction_full 0.570
_reflns_number_total             488
_reflns_number_gt                455
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_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_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_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'

_computing_molecular_graphics    'Mercury (Macrae et al., 2006)'
_computing_publication_material  'enCIFer (Allen et al., 2004)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0246P)²+1.7508P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         488
_refine_ls_number_parameters     52
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0240
_refine_ls_wR_factor_ref         0.0575
_refine_ls_wR_factor_gt          0.0557
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.083
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
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)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
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_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
_geom_angle_publ_flag
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_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

_refine_diff_density_max         0.330
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.090

_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
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_480GPa
_database_code_depnum_ccdc_archive 'CCDC 1423463'
_audit_update_record             
;
2015-09-10 deposited with the CCDC.
2015-10-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        nitro-pentaammine-Co(III)-dibromide
_chemical_name_common            nitro-pentaammine-Co(III)-dibromide
_chemical_melting_point          ?
_chemical_formula_moiety         'Co H15 N6 O2, 2(Br)'
_chemical_formula_sum            'Br2 Co H15 N6 O2'
_chemical_formula_weight         349.93

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

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'

_cell_length_a                   10.6023(5)
_cell_length_b                   7.5308(7)
_cell_length_c                   10.6049(4)
_cell_angle_alpha                90
_cell_angle_beta                 93.439(4)
_cell_angle_gamma                90
_cell_volume                     845.21(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1704
_cell_measurement_theta_min      2.6420
_cell_measurement_theta_max      27.8020

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_preparation       'mounted in DAC'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.750
_exptl_crystal_F_000             680
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?

_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    11.454
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?

_exptl_absorpt_correction_type   Gaussian
_exptl_absorpt_correction_T_min  0.207
_exptl_absorpt_correction_T_max  0.272
_exptl_absorpt_process_details   'Absorb-7 (Angel, 2013)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      295(2)
_diffrn_ambient_pressure         4800000
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a

_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 10.3457
_diffrn_reflns_number            2236
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.320
_diffrn_reflns_theta_max         26.354
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.560
_diffrn_measured_fraction_theta_full 0.576
_diffrn_reflns_Laue_measured_fraction_max 0.560
_diffrn_reflns_Laue_measured_fraction_full 0.576
_diffrn_reflns_point_group_measured_fraction_max 0.560
_diffrn_reflns_point_group_measured_fraction_full 0.576
_reflns_number_total             482
_reflns_number_gt                451
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_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_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_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'

_computing_molecular_graphics    'Mercury (Macrae et al., 2006)'
_computing_publication_material  'enCIFer (Allen et al., 2004)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0275P)²+2.5892P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         482
_refine_ls_number_parameters     52
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0252
_refine_ls_wR_factor_ref         0.0603
_refine_ls_wR_factor_gt          0.0586
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.070
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
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)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
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_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
_geom_angle_publ_flag
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_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

_refine_diff_density_max         0.386
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.098

_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
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_550GPa
_database_code_depnum_ccdc_archive 'CCDC 1423464'
_audit_update_record             
;
2015-09-10 deposited with the CCDC.
2015-10-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        nitro-pentaammine-Co(III)-dibromide
_chemical_name_common            nitro-pentaammine-Co(III)-dibromide
_chemical_melting_point          ?
_chemical_formula_moiety         'Co H15 N6 O2, 2(Br)'
_chemical_formula_sum            'Br2 Co H15 N6 O2'
_chemical_formula_weight         349.93

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

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'

_cell_length_a                   10.5931(4)
_cell_length_b                   7.4783(7)
_cell_length_c                   10.5357(4)
_cell_angle_alpha                90
_cell_angle_beta                 93.300(4)
_cell_angle_gamma                90
_cell_volume                     833.24(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1697
_cell_measurement_theta_min      2.8230
_cell_measurement_theta_max      27.8890

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_preparation       'mounted in DAC'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.789
_exptl_crystal_F_000             680
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?

_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    11.618
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?

_exptl_absorpt_correction_type   Gaussian
_exptl_absorpt_correction_T_min  0.205
_exptl_absorpt_correction_T_max  0.270
_exptl_absorpt_process_details   'Absorb-7 (Angel, 2013)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      295(2)
_diffrn_ambient_pressure         5500000
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a

_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 10.3457
_diffrn_reflns_number            2182
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.336
_diffrn_reflns_theta_max         26.359
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.557
_diffrn_measured_fraction_theta_full 0.576
_diffrn_reflns_Laue_measured_fraction_max 0.557
_diffrn_reflns_Laue_measured_fraction_full 0.576
_diffrn_reflns_point_group_measured_fraction_max 0.557
_diffrn_reflns_point_group_measured_fraction_full 0.576
_reflns_number_total             475
_reflns_number_gt                441
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_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_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_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'

_computing_molecular_graphics    'Mercury (Macrae et al., 2006)'
_computing_publication_material  'enCIFer (Allen et al., 2004)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0200P)²+3.2405P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         475
_refine_ls_number_parameters     52
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0232
_refine_ls_wR_factor_ref         0.0564
_refine_ls_wR_factor_gt          0.0536
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_restrained_S_all      1.098
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.28881(4) 0.50966(7) 0.49659(4) 0.0153(2) Uani 1 1 d . . . . .
Co1 Co 0.0000 0.29206(13) 0.2500 0.0093(3) Uani 1 2 d S T P . .
N1 N 0.1819(3) 0.2894(6) 0.2520(3) 0.0125(10) Uani 1 1 d . . . . .
H1A H 0.2091 0.1768 0.2523 0.019 Uiso 1 1 calc R U . . .
H1B H 0.2071 0.3451 0.1832 0.019 Uiso 1 1 calc R U . . .
H1C H 0.2135 0.3451 0.3214 0.019 Uiso 1 1 calc R U . . .
N2 N 0.0052(3) 0.3006(6) 0.4337(3) 0.0130(10) Uani 1 1 d . . . . .
H2A H 0.0061 0.1898 0.4645 0.020 Uiso 1 1 calc R U . . .
H2B H 0.0747 0.3580 0.4626 0.020 Uiso 1 1 calc R U . . .
H2C H -0.0627 0.3580 0.4586 0.020 Uiso 1 1 calc R U . . .
N3 N 0.0000 0.0291(9) 0.2500 0.0171(15) Uani 1 2 d S T P . .
H3A H 0.0793 -0.0106 0.2509 0.026 Uiso 0.5 1 calc R U P . .
H3B H -0.0364 -0.0106 0.3187 0.026 Uiso 0.5 1 calc R U P . .
H3C H -0.0428 -0.0106 0.1805 0.026 Uiso 0.5 1 calc R U P . .
N4 N 0.0000 0.5458(9) 0.2500 0.0098(15) Uani 1 2 d S T P . .
O1 O 0.0822(3) 0.6320(7) 0.1961(3) 0.0289(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 0.0172(3) 0.0127(6) 0.0162(3) 0.00112(17) 0.0022(2) -0.00047(17)
Co1 0.0097(5) 0.0070(10) 0.0112(4) 0.000 -0.0001(3) 0.000
N1 0.015(2) 0.007(4) 0.0151(18) 0.0015(15) -0.0008(15) 0.0024(15)
N2 0.015(2) 0.010(4) 0.0141(18) -0.0007(15) 0.0002(15) -0.0010(15)
N3 0.024(4) 0.009(6) 0.018(3) 0.000 0.001(3) 0.000
N4 0.009(3) 0.008(7) 0.012(3) 0.000 0.001(3) 0.000
O1 0.027(2) 0.027(5) 0.035(2) -0.0007(18) 0.0183(17) -0.0058(18)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 N4 1.897(7) . ?
Co1 N1 1.926(3) 2 ?
Co1 N1 1.926(3) . ?
Co1 N2 1.934(3) . ?
Co1 N2 1.934(3) 2 ?
Co1 N3 1.967(7) . ?
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 1.246(5) . ?
N4 O1 1.246(5) 2 ?

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
_geom_angle_publ_flag
N4 Co1 N1 90.59(13) . 2 ?
N4 Co1 N1 90.59(13) . . ?
N1 Co1 N1 178.8(3) 2 . ?
N4 Co1 N2 88.11(13) . . ?
N1 Co1 N2 88.97(15) 2 . ?
N1 Co1 N2 91.07(15) . . ?
N4 Co1 N2 88.11(13) . 2 ?
N1 Co1 N2 91.07(15) 2 2 ?
N1 Co1 N2 88.97(15) . 2 ?
N2 Co1 N2 176.2(3) . 2 ?
N4 Co1 N3 180.0 . . ?
N1 Co1 N3 89.41(13) 2 . ?
N1 Co1 N3 89.41(13) . . ?
N2 Co1 N3 91.89(13) . . ?
N2 Co1 N3 91.89(13) 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 117.7(7) . 2 ?
O1 N4 Co1 121.1(4) . . ?
O1 N4 Co1 121.1(4) 2 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Co1 N4 O1 -147.3(2) 2 . . . ?
N1 Co1 N4 O1 32.7(2) . . . . ?
N2 Co1 N4 O1 123.8(2) . . . . ?
N2 Co1 N4 O1 -56.2(2) 2 . . . ?
N1 Co1 N4 O1 32.7(2) 2 . . 2 ?
N1 Co1 N4 O1 -147.3(2) . . . 2 ?
N2 Co1 N4 O1 -56.2(2) . . . 2 ?
N2 Co1 N4 O1 123.8(2) 2 . . 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 2.27 2.788(5) 116.8 4_545
N1 H1B Br1 0.89 2.45 3.336(4) 176.6 6_565
N1 H1C Br1 0.89 2.32 3.210(4) 175.7 .
N2 H2A Br1 0.89 2.65 3.240(4) 124.9 7_556
N2 H2A Br1 0.89 2.70 3.256(4) 121.2 3_445
N2 H2B Br1 0.89 2.54 3.417(4) 167.5 .
N2 H2C Br1 0.89 2.66 3.538(4) 169.6 5_566
N3 H3B Br1 0.89 2.71 3.5277(5) 152.6 3_445
N3 H3C Br1 0.89 2.56 3.3955(7) 157.4 8_455

_refine_diff_density_max         0.440
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.090

_shelx_res_file                  
;

    _5.50GPa.res created by SHELXL-2014/7

TITL 5.50
CELL  0.71073 10.59310  7.47830 10.53570 90.00000 93.30000 90.00000
ZERR 4  0.00040  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    0.020000    3.240500
FVAR       2.42725
BR1   1    0.288810    0.509659    0.496592    11.00000    0.01724    0.01273 =
         0.01617    0.00112    0.00220   -0.00047
CO1   2    0.000000    0.292060    0.250000    10.50000    0.00972    0.00696 =
         0.01123    0.00000   -0.00014    0.00000
N1    4    0.181885    0.289391    0.251965    11.00000    0.01504    0.00724 =
         0.01509    0.00155   -0.00078    0.00241
AFIX  33
H1A   3    0.209083    0.176781    0.252259    11.00000   -1.50000
H1B   3    0.207096    0.345079    0.183189    11.00000   -1.50000
H1C   3    0.213534    0.345080    0.321356    11.00000   -1.50000
AFIX   0
N2    4    0.005213    0.300592    0.433731    11.00000    0.01458    0.01025 =
         0.01412   -0.00068    0.00022   -0.00098
AFIX  33
H2A   3    0.006088    0.189757    0.464539    11.00000   -1.50000
H2B   3    0.074661    0.357972    0.462602    11.00000   -1.50000
H2C   3   -0.062710    0.357972    0.458585    11.00000   -1.50000
AFIX   0
N3    4    0.000000    0.029073    0.250000    10.50000    0.02419    0.00919 =
         0.01794    0.00000    0.00099    0.00000
AFIX  33
H3A   3    0.079256   -0.010597    0.250858    10.50000   -1.50000
H3B   3   -0.036411   -0.010597    0.318655    10.50000   -1.50000
H3C   3   -0.042846   -0.010598    0.180487    10.50000   -1.50000
AFIX   0
N4    4    0.000000    0.545793    0.250000    10.50000    0.00923    0.00802 =
         0.01220    0.00000    0.00142    0.00000
O1    5    0.082215    0.631960    0.196140    11.00000    0.02699    0.02694 =
         0.03476   -0.00068    0.01833   -0.00582
HKLF 4

REM  5.50
REM R1 =  0.0232 for     441 Fo > 4sig(Fo)  and  0.0261 for all     475 data
REM     52 parameters refined using      0 restraints

END

WGHT      0.0200      3.2404

REM Highest difference peak  0.440,  deepest hole -0.362,  1-sigma level  0.090
Q1    1   0.2109  0.1846  0.1811  11.00000  0.05    0.44
Q2    1   0.2237  0.2190  0.3201  11.00000  0.05    0.38
Q3    1   0.1616  0.4930  0.2940  11.00000  0.05    0.34
Q4    1   0.1341  0.1721  0.5574  11.00000  0.05    0.31
Q5    1   0.2029  0.4206  0.2477  11.00000  0.05    0.30
Q6    1   0.1328  0.3963  0.3919  11.00000  0.05    0.30
Q7    1   0.1114  0.5303  0.4375  11.00000  0.05    0.29
Q8    1   0.2055  0.1675  0.3429  11.00000  0.05    0.29
Q9    1   0.0000  0.5000  0.5000  10.50000  0.05    0.28
Q10   1   0.2876  0.2823  0.3976  11.00000  0.05    0.27
;
_shelx_res_checksum              51532
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_601GPa
_database_code_depnum_ccdc_archive 'CCDC 1423465'
_audit_update_record             
;
2015-09-10 deposited with the CCDC.
2015-10-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        nitro-pentaammine-Co(III)-dibromide
_chemical_name_common            nitro-pentaammine-Co(III)-dibromide
_chemical_melting_point          ?
_chemical_formula_moiety         'Co H15 N6 O2, 2(Br)'
_chemical_formula_sum            'Br2 Co H15 N6 O2'
_chemical_formula_weight         349.93

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

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'

_cell_length_a                   10.5914(5)
_cell_length_b                   7.4435(7)
_cell_length_c                   10.4601(4)
_cell_angle_alpha                90
_cell_angle_beta                 93.121(4)
_cell_angle_gamma                90
_cell_volume                     823.42(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1683
_cell_measurement_theta_min      2.8280
_cell_measurement_theta_max      27.9710

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_preparation       'mounted in DAC'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.823
_exptl_crystal_F_000             680
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?

_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    11.757
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?

_exptl_absorpt_correction_type   Gaussian
_exptl_absorpt_correction_T_min  0.205
_exptl_absorpt_correction_T_max  0.268
_exptl_absorpt_process_details   'Absorb-7 (Angel, 2013)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      295(2)
_diffrn_ambient_pressure         6010000
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a

_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 10.3457
_diffrn_reflns_number            2170
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.347
_diffrn_reflns_theta_max         26.357
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.560
_diffrn_measured_fraction_theta_full 0.579
_diffrn_reflns_Laue_measured_fraction_max 0.560
_diffrn_reflns_Laue_measured_fraction_full 0.579
_diffrn_reflns_point_group_measured_fraction_max 0.560
_diffrn_reflns_point_group_measured_fraction_full 0.579
_reflns_number_total             469
_reflns_number_gt                438
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_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_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_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'

_computing_molecular_graphics    'Mercury (Macrae et al., 2006)'
_computing_publication_material  'enCIFer (Allen et al., 2004)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0238P)²+4.0477P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         469
_refine_ls_number_parameters     52
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0256
_refine_ls_wR_factor_ref         0.0618
_refine_ls_wR_factor_gt          0.0603
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.089
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.28874(4) 0.50916(7) 0.49694(4) 0.0154(2) Uani 1 1 d . . . . .
Co1 Co 0.0000 0.29213(14) 0.2500 0.0093(3) Uani 1 2 d S T P . .
N1 N 0.1813(3) 0.2900(6) 0.2518(3) 0.0126(10) Uani 1 1 d . . . . .
H1A H 0.2087 0.1770 0.2520 0.019 Uiso 1 1 calc R U . . .
H1B H 0.2066 0.3461 0.1825 0.019 Uiso 1 1 calc R U . . .
H1C H 0.2128 0.3461 0.3216 0.019 Uiso 1 1 calc R U . . .
N2 N 0.0046(4) 0.3008(6) 0.4350(3) 0.0136(10) Uani 1 1 d . . . . .
H2A H 0.0054 0.1894 0.4661 0.020 Uiso 1 1 calc R U . . .
H2B H 0.0740 0.3584 0.4641 0.020 Uiso 1 1 calc R U . . .
H2C H -0.0634 0.3584 0.4600 0.020 Uiso 1 1 calc R U . . .
N3 N 0.0000 0.0283(9) 0.2500 0.0164(16) Uani 1 2 d S T P . .
H3A H 0.0793 -0.0116 0.2508 0.025 Uiso 0.5 1 calc R U P . .
H3B H -0.0365 -0.0116 0.3192 0.025 Uiso 0.5 1 calc R U P . .
H3C H -0.0427 -0.0116 0.1800 0.025 Uiso 0.5 1 calc R U P . .
N4 N 0.0000 0.5481(10) 0.2500 0.0107(16) Uani 1 2 d S T P . .
O1 O 0.0840(4) 0.6336(7) 0.1985(4) 0.0295(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 0.0169(4) 0.0133(6) 0.0160(3) 0.00108(18) 0.0020(2) -0.00047(19)
Co1 0.0100(5) 0.0060(10) 0.0117(5) 0.000 0.0003(4) 0.000
N1 0.015(2) 0.008(4) 0.015(2) -0.0005(16) -0.0010(17) 0.0009(17)
N2 0.013(2) 0.015(4) 0.012(2) -0.0001(16) 0.0025(17) 0.0007(17)
N3 0.023(4) 0.009(7) 0.017(3) 0.000 -0.001(3) 0.000
N4 0.011(4) 0.008(7) 0.013(3) 0.000 -0.001(3) 0.000
O1 0.025(2) 0.026(5) 0.039(2) 0.0007(19) 0.0179(19) -0.0043(19)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 N4 1.905(7) . ?
Co1 N1 1.920(4) 2 ?
Co1 N1 1.920(4) . ?
Co1 N2 1.934(4) . ?
Co1 N2 1.935(4) 2 ?
Co1 N3 1.964(7) . ?
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(6) . ?
N4 O1 1.241(6) 2 ?

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
_geom_angle_publ_flag
N4 Co1 N1 90.47(14) . 2 ?
N4 Co1 N1 90.47(14) . . ?
N1 Co1 N1 179.1(3) 2 . ?
N4 Co1 N2 88.09(14) . . ?
N1 Co1 N2 88.89(16) 2 . ?
N1 Co1 N2 91.14(16) . . ?
N4 Co1 N2 88.09(14) . 2 ?
N1 Co1 N2 91.14(16) 2 2 ?
N1 Co1 N2 88.89(16) . 2 ?
N2 Co1 N2 176.2(3) . 2 ?
N4 Co1 N3 180.0 . . ?
N1 Co1 N3 89.53(14) 2 . ?
N1 Co1 N3 89.53(14) . . ?
N2 Co1 N3 91.91(14) . . ?
N2 Co1 N3 91.91(14) 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 118.3(8) . 2 ?
O1 N4 Co1 120.9(4) . . ?
O1 N4 Co1 120.9(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 2.25 2.768(5) 116.7 4_545
N1 H1B Br1 0.89 2.42 3.311(4) 176.3 6_565
N1 H1C Br1 0.89 2.31 3.196(4) 176.1 .
N2 H2A Br1 0.89 2.65 3.233(4) 124.4 7_556
N2 H2A Br1 0.89 2.69 3.243(4) 121.1 3_445
N2 H2B Br1 0.89 2.54 3.416(4) 167.1 .
N2 H2C Br1 0.89 2.64 3.522(4) 169.3 5_566
N3 H3B Br1 0.89 2.70 3.5111(6) 152.4 3_445
N3 H3C Br1 0.89 2.55 3.3832(7) 157.0 8_455

_refine_diff_density_max         0.460
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.100

_shelx_res_file                  
;

    _6.01GPa.res created by SHELXL-2014/7

TITL 6.01
CELL  0.71073 10.59140  7.44350 10.46010 90.00000 93.12100 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    0.023800    4.047700
FVAR       2.44422
BR1   1    0.288740    0.509163    0.496936    11.00000    0.01686    0.01328 =
         0.01603    0.00108    0.00196   -0.00047
CO1   2    0.000000    0.292131    0.250000    10.50000    0.01004    0.00599 =
         0.01170    0.00000    0.00030    0.00000
N1    4    0.181323    0.290030    0.251760    11.00000    0.01525    0.00771 =
         0.01453   -0.00048   -0.00097    0.00089
AFIX  33
H1A   3    0.208700    0.176980    0.252026    11.00000   -1.50000
H1B   3    0.206585    0.346068    0.182463    11.00000   -1.50000
H1C   3    0.212753    0.346068    0.321607    11.00000   -1.50000
AFIX   0
N2    4    0.004604    0.300783    0.435033    11.00000    0.01333    0.01521 =
         0.01241   -0.00006    0.00251    0.00072
AFIX  33
H2A   3    0.005377    0.189443    0.466082    11.00000   -1.50000
H2B   3    0.073968    0.358443    0.464109    11.00000   -1.50000
H2C   3   -0.063413    0.358443    0.460035    11.00000   -1.50000
AFIX   0
N3    4    0.000000    0.028288    0.250000    10.50000    0.02320    0.00855 =
         0.01728    0.00000   -0.00057    0.00000
AFIX  33
H3A   3    0.079262   -0.011567    0.250770    10.50000   -1.50000
H3B   3   -0.036548   -0.011567    0.319187    10.50000   -1.50000
H3C   3   -0.042714   -0.011568    0.180043    10.50000   -1.50000
AFIX   0
N4    4    0.000000    0.548076    0.250000    10.50000    0.01106    0.00763 =
         0.01309    0.00000   -0.00134    0.00000
O1    5    0.084044    0.633612    0.198459    11.00000    0.02450    0.02633 =
         0.03944    0.00073    0.01793   -0.00433
HKLF 4

REM  6.01
REM R1 =  0.0256 for     438 Fo > 4sig(Fo)  and  0.0281 for all     469 data
REM     52 parameters refined using      0 restraints

END

WGHT      0.0238      4.0477

REM Highest difference peak  0.460,  deepest hole -0.391,  1-sigma level  0.100
Q1    1   0.2250  0.2179  0.3243  11.00000  0.05    0.46
Q2    1   0.1030  0.6260  0.2817  11.00000  0.05    0.38
Q3    1   0.1975  0.2197  0.1827  11.00000  0.05    0.37
Q4    1   0.1978  0.3997  0.5403  11.00000  0.05    0.33
Q5    1  -0.1039  0.1976  0.4301  11.00000  0.05    0.33
Q6    1   0.2763  0.4942  0.1812  11.00000  0.05    0.31
Q7    1   0.2651  0.1002  0.2587  11.00000  0.05    0.31
Q8    1   0.3139  0.3941  0.5967  11.00000  0.05    0.30
Q9    1   0.2681  0.3235  0.2619  11.00000  0.05    0.29
Q10   1   0.3001  0.4730  0.1641  11.00000  0.05    0.28
;
_shelx_res_checksum              50166
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_685GPa_HP_phase
_database_code_depnum_ccdc_archive 'CCDC 1423466'
_audit_update_record             
;
2015-09-10 deposited with the CCDC.
2015-10-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        nitro-pentaammine-Co(III)-dibromide
_chemical_name_common            nitro-pentaammine-Co(III)-dibromide
_chemical_melting_point          ?
_chemical_formula_moiety         'Co H15 N6 O2, 2(Br)'
_chemical_formula_sum            'Br2 Co H15 N6 O2'
_chemical_formula_weight         349.93

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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_H-M_alt        'C m c m'
_space_group_name_Hall           '-C 2c 2'

_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.
;

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'

_cell_length_a                   10.7595(5)
_cell_length_b                   7.4390(6)
_cell_length_c                   10.0890(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     807.52(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1696
_cell_measurement_theta_min      2.7820
_cell_measurement_theta_max      27.5680

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_preparation       'mounted in DAC'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.878
_exptl_crystal_F_000             680
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?

_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    11.988
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Gaussian
_exptl_absorpt_correction_T_min  0.202
_exptl_absorpt_correction_T_max  0.265
_exptl_absorpt_process_details   'Absorb-7 (Angel, 2013)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      295(2)
_diffrn_ambient_pressure         6850000
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 10.3457
_diffrn_reflns_number            2137
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_av_R_equivalents  0.0624
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.329
_diffrn_reflns_theta_max         26.366
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.716
_diffrn_measured_fraction_theta_full 0.736
_diffrn_reflns_Laue_measured_fraction_max 0.716
_diffrn_reflns_Laue_measured_fraction_full 0.736
_diffrn_reflns_point_group_measured_fraction_max 0.716
_diffrn_reflns_point_group_measured_fraction_full 0.736
_reflns_number_total             333
_reflns_number_gt                310
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_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_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_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_structure_solution    'SIR2004 (Burla et al., 2005)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'

_computing_molecular_graphics    'Mercury (Macrae et al., 2006)'
_computing_publication_material  'enCIFer (Allen et al., 2004)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0351P)²+2.0046P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         333
_refine_ls_number_parameters     36
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0270
_refine_ls_wR_factor_ref         0.0637
_refine_ls_wR_factor_gt          0.0622
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      0.991
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
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)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
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_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
_geom_angle_publ_flag
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_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

_refine_diff_density_max         0.641
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.128

_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
