# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_-173C
_database_code_depnum_ccdc_archive 'CCDC 1470414'
_audit_update_record             
;
2016-03-25 deposited with the CCDC.
2016-05-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_name_common            nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_melting_point          ?
_chemical_formula_moiety         'Co H15 N6 O2, N O3, Cl'
_chemical_formula_sum            'Cl Co H15 N7 O5'
_chemical_formula_weight         287.57

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1484 0.1585 '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           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   14.7021(11)
_cell_length_b                   7.1057(8)
_cell_length_c                   9.6760(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1010.84(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    11727
_cell_measurement_theta_min      1.47
_cell_measurement_theta_max      29.50

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.890
_exptl_crystal_F_000             592
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    1.977
_shelx_estimated_absorpt_T_min   0.588
_shelx_estimated_absorpt_T_max   0.756
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6507
_exptl_absorpt_correction_T_max  0.7709
_exptl_absorpt_process_details   X-RED
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 6.67
_diffrn_reflns_number            6811
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.520
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             1119
_reflns_number_gt                960
_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       'X-AREA (Stoe & Cie, 2006)'
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2006)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2006)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0303P)²+0.0271P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1119
_refine_ls_number_parameters     79
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0189
_refine_ls_wR_factor_ref         0.0475
_refine_ls_wR_factor_gt          0.0464
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.001
_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
Cl1 Cl 0.34895(3) 0.2500 0.52552(5) 0.01188(12) Uani 1 2 d S T P . .
Co1 Co 0.13416(2) 0.2500 0.79765(3) 0.00831(10) Uani 1 2 d S T P . .
N1 N 0.12459(11) 0.2500 0.59339(18) 0.0123(4) Uani 1 2 d S T P . .
H1A H 0.1804 0.2715 0.5559 0.018 Uiso 0.5 1 calc R U P . .
H1B H 0.0855 0.3421 0.5662 0.018 Uiso 0.5 1 calc R U P . .
H1C H 0.1035 0.1363 0.5642 0.018 Uiso 0.5 1 calc R U P . .
N2 N 0.22650(8) 0.05013(18) 0.78294(13) 0.0124(3) Uani 1 1 d . . . . .
H2A H 0.2204 -0.0100 0.7004 0.019 Uiso 1 1 calc R U . . .
H2B H 0.2188 -0.0339 0.8530 0.019 Uiso 1 1 calc R U . . .
H2C H 0.2830 0.1019 0.7886 0.019 Uiso 1 1 calc R U . . .
N3 N 0.04077(8) 0.05600(19) 0.81636(13) 0.0133(3) Uani 1 1 d . . . . .
H3A H 0.0328 -0.0028 0.7337 0.020 Uiso 1 1 calc R U . . .
H3B H -0.0125 0.1100 0.8432 0.020 Uiso 1 1 calc R U . . .
H3C H 0.0586 -0.0296 0.8809 0.020 Uiso 1 1 calc R U . . .
N4 N 0.14915(11) 0.2500 0.99453(18) 0.0105(4) Uani 1 2 d S T P . .
N5 N 0.41352(11) 0.2500 0.99174(18) 0.0128(4) Uani 1 2 d S T P . .
O1 O 0.22709(10) 0.2500 1.04393(15) 0.0151(3) Uani 1 2 d S T P . .
O2 O 0.08212(10) 0.2500 1.07189(16) 0.0154(3) Uani 1 2 d S T P . .
O3 O 0.41178(7) 0.09745(15) 0.92670(12) 0.0177(2) Uani 1 1 d . . . . .
O4 O 0.41740(11) 0.2500 1.12037(17) 0.0225(4) Uani 1 2 d S T P . .


_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 1.9177(18) . ?
Co1 N3 1.9540(13) 8_565 ?
Co1 N3 1.9540(13) . ?
Co1 N2 1.9699(12) . ?
Co1 N2 1.9699(12) 8_565 ?
Co1 N1 1.9814(18) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
N2 H2C 0.9100 . ?
N3 H3A 0.9100 . ?
N3 H3B 0.9100 . ?
N3 H3C 0.9100 . ?
N4 O2 1.238(2) . ?
N4 O1 1.241(2) . ?
N5 O4 1.246(2) . ?
N5 O3 1.2536(14) 8_565 ?
N5 O3 1.2537(14) . ?

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 N3 89.35(5) . 8_565 ?
N4 Co1 N3 89.35(5) . . ?
N3 Co1 N3 89.74(8) 8_565 . ?
N4 Co1 N2 89.57(5) . . ?
N3 Co1 N2 178.34(5) 8_565 . ?
N3 Co1 N2 88.99(6) . . ?
N4 Co1 N2 89.57(5) . 8_565 ?
N3 Co1 N2 88.99(6) 8_565 8_565 ?
N3 Co1 N2 178.34(5) . 8_565 ?
N2 Co1 N2 92.27(7) . 8_565 ?
N4 Co1 N1 177.47(7) . . ?
N3 Co1 N1 92.44(5) 8_565 . ?
N3 Co1 N1 92.44(5) . . ?
N2 Co1 N1 88.67(5) . . ?
N2 Co1 N1 88.67(5) 8_565 . ?
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 . . ?
O2 N4 O1 120.14(17) . . ?
O2 N4 Co1 120.61(13) . . ?
O1 N4 Co1 119.25(13) . . ?
O4 N5 O3 120.15(9) . 8_565 ?
O4 N5 O3 120.16(9) . . ?
O3 N5 O3 119.69(17) 8_565 . ?


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 H1C O3 0.91 2.83 3.3170(19) 114.6 6_557
N1 H1C O3 0.91 2.14 2.9971(15) 156.5 2_554
N1 H1B O3 0.91 2.26 2.9971(15) 137.6 7_665
N1 H1A Cl1 0.91 2.50 3.3632(17) 158.5 .
N2 H2C Cl1 0.91 2.92 3.3855(13) 113.3 .
N2 H2B Cl1 0.91 2.48 3.3598(13) 163.4 2
N2 H2A O1 0.91 2.41 3.2190(17) 148.5 2_554
N2 H2C O3 0.91 2.32 3.0770(16) 140.8 .
N3 H3C Cl1 0.91 2.50 3.3841(13) 163.4 2
N3 H3B Cl1 0.91 2.60 3.4921(13) 167.3 3_456
N3 H3A O3 0.91 2.47 3.0356(16) 120.9 6_557
N3 H3C O2 0.91 2.63 3.0267(16) 106.9 4_547
N3 H3A O4 0.91 2.20 2.9500(17) 139.7 2_554

_refine_diff_density_max         0.232
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.058

####################################################################### 
# 
# 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_-160C
_database_code_depnum_ccdc_archive 'CCDC 1470415'
_audit_update_record             
;
2016-03-25 deposited with the CCDC.
2016-05-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_name_common            nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_melting_point          ?
_chemical_formula_moiety         'Co H15 N6 O2, N O3, Cl'
_chemical_formula_sum            'Cl Co H15 N7 O5'
_chemical_formula_weight         287.57

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1484 0.1585 '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           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   14.7044(11)
_cell_length_b                   7.1209(8)
_cell_length_c                   9.6716(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1012.70(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    113(2)
_cell_measurement_reflns_used    11607
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      29.50

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.886
_exptl_crystal_F_000             592
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    1.974
_shelx_estimated_absorpt_T_min   0.589
_shelx_estimated_absorpt_T_max   0.756
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6463
_exptl_absorpt_correction_T_max  0.7778
_exptl_absorpt_process_details   X-RED
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      113(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 6.67
_diffrn_reflns_number            6815
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.521
_diffrn_reflns_theta_max         26.359
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1121
_reflns_number_gt                970
_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       'X-AREA (Stoe & Cie, 2006)'
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2006)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2006)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0302P)²+0.1062P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1121
_refine_ls_number_parameters     79
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0245
_refine_ls_R_factor_gt           0.0198
_refine_ls_wR_factor_ref         0.0491
_refine_ls_wR_factor_gt          0.0481
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.001
_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
Cl1 Cl 0.34886(3) 0.2500 0.52472(5) 0.01266(13) Uani 1 2 d S T P . .
Co1 Co 0.13404(2) 0.2500 0.79741(3) 0.00877(10) Uani 1 2 d S T P . .
N1 N 0.12469(12) 0.2500 0.59300(19) 0.0132(4) Uani 1 2 d S T P . .
H1A H 0.1806 0.2708 0.5556 0.020 Uiso 0.5 1 calc R U P . .
H1B H 0.0859 0.3424 0.5657 0.020 Uiso 0.5 1 calc R U P . .
H1C H 0.1033 0.1368 0.5638 0.020 Uiso 0.5 1 calc R U P . .
N2 N 0.22653(8) 0.05092(18) 0.78263(13) 0.0129(3) Uani 1 1 d . . . . .
H2A H 0.2205 -0.0089 0.7000 0.019 Uiso 1 1 calc R U . . .
H2B H 0.2189 -0.0330 0.8526 0.019 Uiso 1 1 calc R U . . .
H2C H 0.2830 0.1027 0.7885 0.019 Uiso 1 1 calc R U . . .
N3 N 0.04059(8) 0.0566(2) 0.81606(14) 0.0142(3) Uani 1 1 d . . . . .
H3A H 0.0314 0.0003 0.7328 0.021 Uiso 1 1 calc R U . . .
H3B H -0.0122 0.1102 0.8453 0.021 Uiso 1 1 calc R U . . .
H3C H 0.0590 -0.0307 0.8788 0.021 Uiso 1 1 calc R U . . .
N4 N 0.14892(12) 0.2500 0.99453(19) 0.0113(4) Uani 1 2 d S T P . .
N5 N 0.41333(12) 0.2500 0.99249(19) 0.0137(4) Uani 1 2 d S T P . .
O1 O 0.22681(10) 0.2500 1.04394(16) 0.0162(3) Uani 1 2 d S T P . .
O2 O 0.08187(10) 0.2500 1.07160(17) 0.0162(3) Uani 1 2 d S T P . .
O3 O 0.41169(7) 0.09775(16) 0.92741(12) 0.0189(3) Uani 1 1 d . . . . .
O4 O 0.41705(12) 0.2500 1.12109(18) 0.0240(4) Uani 1 2 d S T P . .


_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 1.9190(19) . ?
Co1 N3 1.9535(13) . ?
Co1 N3 1.9536(13) 8_565 ?
Co1 N2 1.9697(13) 8_565 ?
Co1 N2 1.9697(13) . ?
Co1 N1 1.9818(19) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
N2 H2C 0.9100 . ?
N3 H3A 0.9100 . ?
N3 H3B 0.9100 . ?
N3 H3C 0.9100 . ?
N4 O2 1.236(2) . ?
N4 O1 1.241(2) . ?
N5 O4 1.245(3) . ?
N5 O3 1.2539(15) . ?
N5 O3 1.2539(15) 8_565 ?

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 N3 89.34(5) . . ?
N4 Co1 N3 89.34(5) . 8_565 ?
N3 Co1 N3 89.62(8) . 8_565 ?
N4 Co1 N2 89.62(5) . 8_565 ?
N3 Co1 N2 178.40(6) . 8_565 ?
N3 Co1 N2 89.15(6) 8_565 8_565 ?
N4 Co1 N2 89.62(5) . . ?
N3 Co1 N2 89.15(6) . . ?
N3 Co1 N2 178.40(5) 8_565 . ?
N2 Co1 N2 92.06(8) 8_565 . ?
N4 Co1 N1 177.43(7) . . ?
N3 Co1 N1 92.48(5) . . ?
N3 Co1 N1 92.48(5) 8_565 . ?
N2 Co1 N1 88.59(5) 8_565 . ?
N2 Co1 N1 88.59(5) . . ?
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 . . ?
O2 N4 O1 120.27(18) . . ?
O2 N4 Co1 120.54(14) . . ?
O1 N4 Co1 119.19(14) . . ?
O4 N5 O3 120.16(9) . . ?
O4 N5 O3 120.16(9) . 8_565 ?
O3 N5 O3 119.68(18) . 8_565 ?


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 H1C O3 0.91 2.83 3.320(2) 114.9 6_557
N1 H1C O3 0.91 2.14 2.9972(16) 156.6 2_554
N1 H1B O3 0.91 2.26 2.9972(16) 138.1 7_665
N1 H1A Cl1 0.91 2.50 3.3618(18) 158.9 .
N2 H2C Cl1 0.91 2.92 3.3864(14) 113.2 .
N2 H2B Cl1 0.91 2.48 3.3620(14) 163.4 2
N2 H2A O1 0.91 2.41 3.2236(17) 148.3 2_554
N2 H2C O3 0.91 2.32 3.0798(17) 140.6 .
N3 H3C Cl1 0.91 2.50 3.3887(14) 164.5 2
N3 H3B Cl1 0.91 2.60 3.4950(14) 169.2 3_456
N3 H3A O3 0.91 2.45 3.0370(17) 122.9 6_557
N3 H3C O2 0.91 2.64 3.0317(17) 106.9 4_547
N3 H3A O4 0.91 2.22 2.9516(18) 137.3 2_554

_refine_diff_density_max         0.275
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.059

####################################################################### 
# 
# 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_-140C
_database_code_depnum_ccdc_archive 'CCDC 1470416'
_audit_update_record             
;
2016-03-25 deposited with the CCDC.
2016-05-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_name_common            nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_melting_point          ?
_chemical_formula_moiety         'Co H15 N6 O2, N O3, Cl'
_chemical_formula_sum            'Cl Co H15 N7 O5'
_chemical_formula_weight         287.57

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1484 0.1585 '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           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   14.7115(11)
_cell_length_b                   7.1415(8)
_cell_length_c                   9.6639(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1015.31(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    11513
_cell_measurement_theta_min      2.09
_cell_measurement_theta_max      29.50

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.881
_exptl_crystal_F_000             592
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    1.969
_shelx_estimated_absorpt_T_min   0.590
_shelx_estimated_absorpt_T_max   0.757
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6516
_exptl_absorpt_correction_T_max  0.7714
_exptl_absorpt_process_details   X-RED
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 6.67
_diffrn_reflns_number            6849
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.522
_diffrn_reflns_theta_max         26.362
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1123
_reflns_number_gt                966
_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       'X-AREA (Stoe & Cie, 2006)'
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2006)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2006)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0341P)²+0.0173P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1123
_refine_ls_number_parameters     79
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0253
_refine_ls_R_factor_gt           0.0203
_refine_ls_wR_factor_ref         0.0519
_refine_ls_wR_factor_gt          0.0508
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_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
Cl1 Cl 0.34872(3) 0.2500 0.52360(6) 0.01414(13) Uani 1 2 d S T P . .
Co1 Co 0.13391(2) 0.2500 0.79711(3) 0.00973(11) Uani 1 2 d S T P . .
N1 N 0.12453(12) 0.2500 0.5926(2) 0.0145(4) Uani 1 2 d S T P . .
H1A H 0.1803 0.2715 0.5552 0.022 Uiso 0.5 1 calc R U P . .
H1B H 0.0855 0.3416 0.5653 0.022 Uiso 0.5 1 calc R U P . .
H1C H 0.1035 0.1369 0.5634 0.022 Uiso 0.5 1 calc R U P . .
N2 N 0.22639(9) 0.05171(19) 0.78230(14) 0.0145(3) Uani 1 1 d . . . . .
H2A H 0.2213 -0.0061 0.6987 0.022 Uiso 1 1 calc R U . . .
H2B H 0.2179 -0.0335 0.8511 0.022 Uiso 1 1 calc R U . . .
H2C H 0.2827 0.1031 0.7902 0.022 Uiso 1 1 calc R U . . .
N3 N 0.04030(8) 0.0575(2) 0.81580(14) 0.0156(3) Uani 1 1 d . . . . .
H3A H 0.0309 0.0017 0.7324 0.023 Uiso 1 1 calc R U . . .
H3B H -0.0124 0.1111 0.8454 0.023 Uiso 1 1 calc R U . . .
H3C H 0.0588 -0.0298 0.8783 0.023 Uiso 1 1 calc R U . . .
N4 N 0.14866(12) 0.2500 0.9944(2) 0.0123(4) Uani 1 2 d S T P . .
N5 N 0.41311(12) 0.2500 0.9936(2) 0.0150(4) Uani 1 2 d S T P . .
O1 O 0.22641(11) 0.2500 1.04417(17) 0.0182(4) Uani 1 2 d S T P . .
O2 O 0.08156(11) 0.2500 1.07155(17) 0.0183(4) Uani 1 2 d S T P . .
O3 O 0.41161(8) 0.09830(17) 0.92841(13) 0.0210(3) Uani 1 1 d . . . . .
O4 O 0.41653(12) 0.2500 1.12213(19) 0.0270(4) Uani 1 2 d S T P . .


_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 1.919(2) . ?
Co1 N3 1.9541(14) 8_565 ?
Co1 N3 1.9541(14) . ?
Co1 N2 1.9689(13) 8_565 ?
Co1 N2 1.9689(13) . ?
Co1 N1 1.9813(19) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
N2 H2C 0.9100 . ?
N3 H3A 0.9100 . ?
N3 H3B 0.9100 . ?
N3 H3C 0.9100 . ?
N4 O2 1.237(2) . ?
N4 O1 1.241(2) . ?
N5 O4 1.243(3) . ?
N5 O3 1.2535(15) . ?
N5 O3 1.2535(15) 8_565 ?

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 N3 89.30(6) . 8_565 ?
N4 Co1 N3 89.30(6) . . ?
N3 Co1 N3 89.41(8) 8_565 . ?
N4 Co1 N2 89.66(5) . 8_565 ?
N3 Co1 N2 89.30(6) 8_565 8_565 ?
N3 Co1 N2 178.35(6) . 8_565 ?
N4 Co1 N2 89.66(5) . . ?
N3 Co1 N2 178.35(6) 8_565 . ?
N3 Co1 N2 89.30(6) . . ?
N2 Co1 N2 91.98(8) 8_565 . ?
N4 Co1 N1 177.50(8) . . ?
N3 Co1 N1 92.47(6) 8_565 . ?
N3 Co1 N1 92.47(6) . . ?
N2 Co1 N1 88.60(5) 8_565 . ?
N2 Co1 N1 88.60(5) . . ?
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 . . ?
O2 N4 O1 120.16(19) . . ?
O2 N4 Co1 120.56(15) . . ?
O1 N4 Co1 119.28(14) . . ?
O4 N5 O3 120.19(9) . . ?
O4 N5 O3 120.20(9) . 8_565 ?
O3 N5 O3 119.61(19) . 8_565 ?


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 H1C O3 0.91 2.84 3.321(2) 114.6 6_557
N1 H1C O3 0.91 2.14 2.9979(16) 157.2 2_554
N1 H1B O3 0.91 2.26 2.9979(16) 137.8 7_665
N1 H1A Cl1 0.91 2.50 3.3648(19) 158.7 .
N2 H2C Cl1 0.91 2.95 3.3904(14) 111.7 .
N2 H2B Cl1 0.91 2.48 3.3617(14) 164.6 2
N2 H2A O1 0.91 2.42 3.2281(18) 148.0 2_554
N2 H2C O3 0.91 2.32 3.0870(17) 141.9 .
N3 H3C Cl1 0.91 2.51 3.3943(15) 164.4 2
N3 H3B Cl1 0.91 2.60 3.4989(14) 169.2 3_456
N3 H3A O3 0.91 2.44 3.0395(18) 123.3 6_557
N3 H3C O2 0.91 2.64 3.0368(18) 107.3 4_547
N3 H3A O4 0.91 2.23 2.9545(19) 136.4 2_554

_refine_diff_density_max         0.270
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.060

####################################################################### 
# 
# 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_-120C
_database_code_depnum_ccdc_archive 'CCDC 1470417'
_audit_update_record             
;
2016-03-25 deposited with the CCDC.
2016-05-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_name_common            nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_melting_point          ?
_chemical_formula_moiety         'Co H15 N6 O2, N O3, Cl'
_chemical_formula_sum            'Cl Co H15 N7 O5'
_chemical_formula_weight         287.57

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1484 0.1585 '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           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   14.7211(11)
_cell_length_b                   7.1625(8)
_cell_length_c                   9.6562(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1018.15(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    11391
_cell_measurement_theta_min      2.54
_cell_measurement_theta_max      29.51

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.876
_exptl_crystal_F_000             592
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    1.963
_shelx_estimated_absorpt_T_min   0.590
_shelx_estimated_absorpt_T_max   0.757
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6526
_exptl_absorpt_correction_T_max  0.7726
_exptl_absorpt_process_details   X-RED
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 6.67
_diffrn_reflns_number            6847
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.523
_diffrn_reflns_theta_max         26.327
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             1123
_reflns_number_gt                962
_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       'X-AREA (Stoe & Cie, 2006)'
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2006)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2006)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0316P)²+0.1529P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1123
_refine_ls_number_parameters     79
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0209
_refine_ls_wR_factor_ref         0.0523
_refine_ls_wR_factor_gt          0.0510
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.001
_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
Cl1 Cl 0.34862(4) 0.2500 0.52268(6) 0.01584(14) Uani 1 2 d S T P . .
Co1 Co 0.13378(2) 0.2500 0.79688(3) 0.01082(11) Uani 1 2 d S T P . .
N1 N 0.12430(13) 0.2500 0.5923(2) 0.0158(4) Uani 1 2 d S T P . .
H1A H 0.1802 0.2702 0.5548 0.024 Uiso 0.5 1 calc R U P . .
H1B H 0.0857 0.3421 0.5650 0.024 Uiso 0.5 1 calc R U P . .
H1C H 0.1027 0.1376 0.5631 0.024 Uiso 0.5 1 calc R U P . .
N2 N 0.22627(9) 0.0526(2) 0.78201(14) 0.0158(3) Uani 1 1 d . . . . .
H2A H 0.2197 -0.0081 0.6998 0.024 Uiso 1 1 calc R U . . .
H2B H 0.2193 -0.0299 0.8529 0.024 Uiso 1 1 calc R U . . .
H2C H 0.2826 0.1046 0.7865 0.024 Uiso 1 1 calc R U . . .
N3 N 0.04024(9) 0.0581(2) 0.81552(15) 0.0170(3) Uani 1 1 d . . . . .
H3A H 0.0302 0.0039 0.7317 0.025 Uiso 1 1 calc R U . . .
H3B H -0.0121 0.1112 0.8466 0.025 Uiso 1 1 calc R U . . .
H3C H 0.0591 -0.0301 0.8770 0.025 Uiso 1 1 calc R U . . .
N4 N 0.14835(13) 0.2500 0.9943(2) 0.0138(4) Uani 1 2 d S T P . .
N5 N 0.41292(13) 0.2500 0.9947(2) 0.0171(4) Uani 1 2 d S T P . .
O1 O 0.22605(11) 0.2500 1.04432(18) 0.0205(4) Uani 1 2 d S T P . .
O2 O 0.08139(11) 0.2500 1.07136(19) 0.0206(4) Uani 1 2 d S T P . .
O3 O 0.41148(8) 0.09889(17) 0.92934(14) 0.0235(3) Uani 1 1 d . . . . .
O4 O 0.41592(14) 0.2500 1.1231(2) 0.0298(5) Uani 1 2 d S T P . .


_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 1.919(2) . ?
Co1 N3 1.9538(14) 8_565 ?
Co1 N3 1.9538(14) . ?
Co1 N2 1.9679(14) . ?
Co1 N2 1.9680(14) 8_565 ?
Co1 N1 1.980(2) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
N2 H2C 0.9100 . ?
N3 H3A 0.9100 . ?
N3 H3B 0.9100 . ?
N3 H3C 0.9100 . ?
N4 O2 1.235(3) . ?
N4 O1 1.241(3) . ?
N5 O4 1.241(3) . ?
N5 O3 1.2531(16) . ?
N5 O3 1.2531(16) 8_565 ?

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 N3 89.27(6) . 8_565 ?
N4 Co1 N3 89.27(6) . . ?
N3 Co1 N3 89.41(9) 8_565 . ?
N4 Co1 N2 89.72(6) . . ?
N3 Co1 N2 178.43(6) 8_565 . ?
N3 Co1 N2 89.37(6) . . ?
N4 Co1 N2 89.72(6) . 8_565 ?
N3 Co1 N2 89.37(6) 8_565 8_565 ?
N3 Co1 N2 178.43(6) . 8_565 ?
N2 Co1 N2 91.83(8) . 8_565 ?
N4 Co1 N1 177.62(8) . . ?
N3 Co1 N1 92.42(6) 8_565 . ?
N3 Co1 N1 92.42(6) . . ?
N2 Co1 N1 88.62(6) . . ?
N2 Co1 N1 88.62(6) 8_565 . ?
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 . . ?
O2 N4 O1 120.1(2) . . ?
O2 N4 Co1 120.61(15) . . ?
O1 N4 Co1 119.29(15) . . ?
O4 N5 O3 120.26(10) . . ?
O4 N5 O3 120.26(10) . 8_565 ?
O3 N5 O3 119.5(2) . 8_565 ?


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 H1C O3 0.91 2.83 3.321(2) 115.2 6_557
N1 H1C O3 0.91 2.14 2.9997(17) 157.0 2_554
N1 H1B O3 0.91 2.26 2.9997(17) 138.4 7_665
N1 H1A Cl1 0.91 2.50 3.370(2) 159.2 .
N2 H2C Cl1 0.91 2.92 3.3931(15) 114.1 .
N2 H2B Cl1 0.91 2.48 3.3638(15) 162.5 2
N2 H2A O1 0.91 2.43 3.2341(19) 147.7 2_554
N2 H2C O3 0.91 2.35 3.0931(19) 139.2 .
N3 H3C Cl1 0.91 2.51 3.3984(15) 165.0 2
N3 H3B Cl1 0.91 2.61 3.5053(15) 170.2 3_456
N3 H3A O3 0.91 2.44 3.0444(19) 124.4 6_557
N3 H3C O2 0.91 2.65 3.0445(18) 107.3 4_547
N3 H3A O4 0.91 2.24 2.956(2) 134.7 2_554

_refine_diff_density_max         0.283
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.061

####################################################################### 
# 
# 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_-100C
_database_code_depnum_ccdc_archive 'CCDC 1470418'
_audit_update_record             
;
2016-03-25 deposited with the CCDC.
2016-05-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_name_common            nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_melting_point          ?
_chemical_formula_moiety         'Co H15 N6 O2, N O3, Cl'
_chemical_formula_sum            'Cl Co H15 N7 O5'
_chemical_formula_weight         287.57

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1484 0.1585 '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           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   14.7279(11)
_cell_length_b                   7.1809(8)
_cell_length_c                   9.6504(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1020.62(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    11203
_cell_measurement_theta_min      1.45
_cell_measurement_theta_max      29.51

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.871
_exptl_crystal_F_000             592
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    1.958
_shelx_estimated_absorpt_T_min   0.591
_shelx_estimated_absorpt_T_max   0.758
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6532
_exptl_absorpt_correction_T_max  0.7723
_exptl_absorpt_process_details   X-RED
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 6.67
_diffrn_reflns_number            6877
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.523
_diffrn_reflns_theta_max         26.352
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             1124
_reflns_number_gt                958
_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       'X-AREA (Stoe & Cie, 2006)'
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2006)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2006)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0326P)²+0.0879P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1124
_refine_ls_number_parameters     79
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0211
_refine_ls_wR_factor_ref         0.0530
_refine_ls_wR_factor_gt          0.0519
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_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
Cl1 Cl 0.34852(4) 0.2500 0.52188(6) 0.01754(14) Uani 1 2 d S T P . .
Co1 Co 0.13365(2) 0.2500 0.79664(3) 0.01187(11) Uani 1 2 d S T P . .
N1 N 0.12440(13) 0.2500 0.5919(2) 0.0170(4) Uani 1 2 d S T P . .
H1A H 0.1801 0.2726 0.5545 0.025 Uiso 0.5 1 calc R U P . .
H1B H 0.0849 0.3403 0.5645 0.025 Uiso 0.5 1 calc R U P . .
H1C H 0.1040 0.1371 0.5625 0.025 Uiso 0.5 1 calc R U P . .
N2 N 0.22622(9) 0.0534(2) 0.78180(15) 0.0172(3) Uani 1 1 d . . . . .
H2A H 0.2208 -0.0049 0.6985 0.026 Uiso 1 1 calc R U . . .
H2B H 0.2182 -0.0308 0.8512 0.026 Uiso 1 1 calc R U . . .
H2C H 0.2825 0.1050 0.7888 0.026 Uiso 1 1 calc R U . . .
N3 N 0.04003(9) 0.0590(2) 0.81509(15) 0.0185(3) Uani 1 1 d . . . . .
H3A H 0.0286 0.0076 0.7307 0.028 Uiso 1 1 calc R U . . .
H3B H -0.0117 0.1114 0.8488 0.028 Uiso 1 1 calc R U . . .
H3C H 0.0595 -0.0311 0.8744 0.028 Uiso 1 1 calc R U . . .
N4 N 0.14808(13) 0.2500 0.9944(2) 0.0151(4) Uani 1 2 d S T P . .
N5 N 0.41264(13) 0.2500 0.9956(2) 0.0183(4) Uani 1 2 d S T P . .
O1 O 0.22563(11) 0.2500 1.04431(18) 0.0227(4) Uani 1 2 d S T P . .
O2 O 0.08112(11) 0.2500 1.07129(19) 0.0226(4) Uani 1 2 d S T P . .
O3 O 0.41138(9) 0.09938(18) 0.93036(14) 0.0260(3) Uani 1 1 d . . . . .
O4 O 0.41540(14) 0.2500 1.1240(2) 0.0327(5) Uani 1 2 d S T P . .


_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 1.920(2) . ?
Co1 N3 1.9531(14) 8_565 ?
Co1 N3 1.9532(14) . ?
Co1 N2 1.9678(14) . ?
Co1 N2 1.9679(14) 8_565 ?
Co1 N1 1.981(2) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
N2 H2C 0.9100 . ?
N3 H3A 0.9100 . ?
N3 H3B 0.9100 . ?
N3 H3C 0.9100 . ?
N4 O2 1.234(3) . ?
N4 O1 1.240(3) . ?
N5 O4 1.240(3) . ?
N5 O3 1.2514(16) 8_565 ?
N5 O3 1.2514(16) . ?

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 N3 89.29(6) . 8_565 ?
N4 Co1 N3 89.29(6) . . ?
N3 Co1 N3 89.23(9) 8_565 . ?
N4 Co1 N2 89.75(6) . . ?
N3 Co1 N2 178.44(6) 8_565 . ?
N3 Co1 N2 89.53(7) . . ?
N4 Co1 N2 89.75(6) . 8_565 ?
N3 Co1 N2 89.53(7) 8_565 8_565 ?
N3 Co1 N2 178.44(6) . 8_565 ?
N2 Co1 N2 91.68(8) . 8_565 ?
N4 Co1 N1 177.59(8) . . ?
N3 Co1 N1 92.43(6) 8_565 . ?
N3 Co1 N1 92.43(6) . . ?
N2 Co1 N1 88.57(6) . . ?
N2 Co1 N1 88.57(6) 8_565 . ?
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 . . ?
O2 N4 O1 120.1(2) . . ?
O2 N4 Co1 120.62(15) . . ?
O1 N4 Co1 119.24(15) . . ?
O4 N5 O3 120.20(10) . 8_565 ?
O4 N5 O3 120.20(10) . . ?
O3 N5 O3 119.6(2) 8_565 . ?


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 H1C O3 0.91 2.85 3.325(2) 114.0 6_557
N1 H1C O3 0.91 2.14 3.0003(17) 158.3 2_554
N1 H1B O3 0.91 2.27 3.0003(17) 137.3 7_665
N1 H1A Cl1 0.91 2.51 3.369(2) 158.4 .
N2 H2C Cl1 0.91 2.94 3.3954(15) 112.3 .
N2 H2B Cl1 0.91 2.48 3.3655(15) 164.0 2
N2 H2A O1 0.91 2.44 3.2407(19) 147.5 2_554
N2 H2C O3 0.91 2.34 3.0985(19) 140.8 .
N3 H3C Cl1 0.91 2.52 3.4058(16) 165.8 2
N3 H3B Cl1 0.91 2.60 3.5089(15) 172.3 3_456
N3 H3A O3 0.91 2.41 3.0470(19) 126.7 6_557
N3 H3C O2 0.91 2.65 3.0510(19) 107.4 4_547
N3 H3A O4 0.91 2.27 2.959(2) 132.0 2_554

_refine_diff_density_max         0.300
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.061

####################################################################### 
# 
# 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_-80C
_database_code_depnum_ccdc_archive 'CCDC 1470419'
_audit_update_record             
;
2016-03-25 deposited with the CCDC.
2016-05-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_name_common            nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_melting_point          ?
_chemical_formula_moiety         'Co H15 N6 O2, N O3, Cl'
_chemical_formula_sum            'Cl Co H15 N7 O5'
_chemical_formula_weight         287.57

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1484 0.1585 '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           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   14.7390(11)
_cell_length_b                   7.2001(8)
_cell_length_c                   9.6461(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1023.67(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    11388
_cell_measurement_theta_min      1.45
_cell_measurement_theta_max      29.50

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.866
_exptl_crystal_F_000             592
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    1.953
_shelx_estimated_absorpt_T_min   0.592
_shelx_estimated_absorpt_T_max   0.758
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6552
_exptl_absorpt_correction_T_max  0.7733
_exptl_absorpt_process_details   X-RED
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 6.67
_diffrn_reflns_number            6889
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.523
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             1129
_reflns_number_gt                971
_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       'X-AREA (Stoe & Cie, 2006)'
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2006)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2006)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0288P)²+0.2795P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1129
_refine_ls_number_parameters     79
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0218
_refine_ls_wR_factor_ref         0.0536
_refine_ls_wR_factor_gt          0.0522
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.001
_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
Cl1 Cl 0.34840(4) 0.2500 0.52124(6) 0.01923(15) Uani 1 2 d S T P . .
Co1 Co 0.13351(2) 0.2500 0.79643(3) 0.01292(11) Uani 1 2 d S T P . .
N1 N 0.12417(14) 0.2500 0.5914(2) 0.0187(4) Uani 1 2 d S T P . .
H1A H 0.1800 0.2699 0.5539 0.028 Uiso 0.5 1 calc R U P . .
H1B H 0.0857 0.3418 0.5639 0.028 Uiso 0.5 1 calc R U P . .
H1C H 0.1025 0.1383 0.5622 0.028 Uiso 0.5 1 calc R U P . .
N2 N 0.22609(9) 0.0540(2) 0.78164(15) 0.0189(3) Uani 1 1 d . . . . .
H2A H 0.2169 -0.0123 0.7026 0.028 Uiso 1 1 calc R U . . .
H2B H 0.2220 -0.0230 0.8562 0.028 Uiso 1 1 calc R U . . .
H2C H 0.2822 0.1066 0.7793 0.028 Uiso 1 1 calc R U . . .
N3 N 0.03993(9) 0.0594(2) 0.81484(16) 0.0201(3) Uani 1 1 d . . . . .
H3A H 0.0285 0.0083 0.7303 0.030 Uiso 1 1 calc R U . . .
H3B H -0.0117 0.1116 0.8487 0.030 Uiso 1 1 calc R U . . .
H3C H 0.0595 -0.0305 0.8741 0.030 Uiso 1 1 calc R U . . .
N4 N 0.14783(13) 0.2500 0.9942(2) 0.0161(4) Uani 1 2 d S T P . .
N5 N 0.41249(14) 0.2500 0.9965(2) 0.0202(5) Uani 1 2 d S T P . .
O1 O 0.22513(12) 0.2500 1.04460(19) 0.0251(4) Uani 1 2 d S T P . .
O2 O 0.08082(12) 0.2500 1.0711(2) 0.0255(4) Uani 1 2 d S T P . .
O3 O 0.41125(9) 0.09976(19) 0.93114(15) 0.0285(3) Uani 1 1 d . . . . .
O4 O 0.41500(15) 0.2500 1.1249(2) 0.0354(5) Uani 1 2 d S T P . .


_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 1.919(2) . ?
Co1 N3 1.9539(15) 8_565 ?
Co1 N3 1.9539(15) . ?
Co1 N2 1.9684(14) 8_565 ?
Co1 N2 1.9684(14) . ?
Co1 N1 1.983(2) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
N2 H2C 0.9100 . ?
N3 H3A 0.9100 . ?
N3 H3B 0.9100 . ?
N3 H3C 0.9100 . ?
N4 O2 1.235(3) . ?
N4 O1 1.239(3) . ?
N5 O4 1.239(3) . ?
N5 O3 1.2521(17) 8_565 ?
N5 O3 1.2521(17) . ?

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 N3 89.27(6) . 8_565 ?
N4 Co1 N3 89.27(6) . . ?
N3 Co1 N3 89.24(9) 8_565 . ?
N4 Co1 N2 89.76(6) . 8_565 ?
N3 Co1 N2 89.56(7) 8_565 8_565 ?
N3 Co1 N2 178.46(6) . 8_565 ?
N4 Co1 N2 89.76(6) . . ?
N3 Co1 N2 178.46(6) 8_565 . ?
N3 Co1 N2 89.56(7) . . ?
N2 Co1 N2 91.63(9) 8_565 . ?
N4 Co1 N1 177.67(8) . . ?
N3 Co1 N1 92.39(6) 8_565 . ?
N3 Co1 N1 92.39(6) . . ?
N2 Co1 N1 88.62(6) 8_565 . ?
N2 Co1 N1 88.62(6) . . ?
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 . . ?
O2 N4 O1 120.0(2) . . ?
O2 N4 Co1 120.60(16) . . ?
O1 N4 Co1 119.43(16) . . ?
O4 N5 O3 120.24(11) . 8_565 ?
O4 N5 O3 120.24(11) . . ?
O3 N5 O3 119.5(2) 8_565 . ?


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 H1C O3 0.91 2.83 3.327(2) 115.4 6_557
N1 H1C O3 0.91 2.14 3.0006(18) 157.5 2_554
N1 H1B O3 0.91 2.26 3.0006(18) 138.7 7_665
N1 H1A Cl1 0.91 2.51 3.373(2) 159.5 .
N2 H2C Cl1 0.91 2.87 3.3987(16) 118.8 .
N2 H2B Cl1 0.91 2.51 3.3671(16) 157.9 2
N2 H2A O1 0.91 2.45 3.246(2) 146.8 2_554
N2 H2C O3 0.91 2.40 3.104(2) 134.1 .
N3 H3C Cl1 0.91 2.52 3.4111(16) 165.8 2
N3 H3B Cl1 0.91 2.61 3.5146(16) 172.3 3_456
N3 H3A O3 0.91 2.42 3.051(2) 126.8 6_557
N3 H3C O2 0.91 2.66 3.0562(19) 107.6 4_547
N3 H3A O4 0.91 2.28 2.960(2) 131.5 2_554

_refine_diff_density_max         0.308
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.063

####################################################################### 
# 
# 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_-60C
_database_code_depnum_ccdc_archive 'CCDC 1470420'
_audit_update_record             
;
2016-03-25 deposited with the CCDC.
2016-05-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_name_common            nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_melting_point          ?
_chemical_formula_moiety         'Co H15 N6 O2, N O3, Cl'
_chemical_formula_sum            'Cl Co H15 N7 O5'
_chemical_formula_weight         287.57

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1484 0.1585 '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           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   14.736(2)
_cell_length_b                   7.2220(11)
_cell_length_c                   9.6239(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1024.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    213(2)
_cell_measurement_reflns_used    11072
_cell_measurement_theta_min      1.46
_cell_measurement_theta_max      29.50

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.865
_exptl_crystal_F_000             592
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    1.952
_shelx_estimated_absorpt_T_min   0.592
_shelx_estimated_absorpt_T_max   0.758
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6668
_exptl_absorpt_correction_T_max  0.7731
_exptl_absorpt_process_details   X-RED
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      213(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 6.67
_diffrn_reflns_number            6888
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_av_R_equivalents  0.0663
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.528
_diffrn_reflns_theta_max         26.344
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             1126
_reflns_number_gt                981
_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       'X-AREA (Stoe & Cie, 2006)'
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2006)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2006)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0268P)²+0.6944P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1126
_refine_ls_number_parameters     79
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0262
_refine_ls_wR_factor_ref         0.0625
_refine_ls_wR_factor_gt          0.0603
_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
Cl1 Cl 0.34832(4) 0.2500 0.52060(7) 0.01935(18) Uani 1 2 d S T P . .
Co1 Co 0.13341(2) 0.2500 0.79626(4) 0.01223(14) Uani 1 2 d S T P . .
N1 N 0.12433(15) 0.2500 0.5911(2) 0.0176(5) Uani 1 2 d S T P . .
H1A H 0.1800 0.2635 0.5541 0.026 Uiso 0.5 1 calc R U P . .
H1B H 0.0887 0.3443 0.5636 0.026 Uiso 0.5 1 calc R U P . .
H1C H 0.1002 0.1422 0.5624 0.026 Uiso 0.5 1 calc R U P . .
N2 N 0.22591(11) 0.0550(2) 0.78152(17) 0.0193(4) Uani 1 1 d . . . . .
H2A H 0.2175 -0.0090 0.7023 0.029 Uiso 1 1 calc R U . . .
H2B H 0.2212 -0.0222 0.8546 0.029 Uiso 1 1 calc R U . . .
H2C H 0.2815 0.1068 0.7809 0.029 Uiso 1 1 calc R U . . .
N3 N 0.03970(11) 0.0602(3) 0.81436(17) 0.0203(4) Uani 1 1 d . . . . .
H3A H 0.0279 0.0110 0.7303 0.030 Uiso 1 1 calc R U . . .
H3B H -0.0112 0.1114 0.8489 0.030 Uiso 1 1 calc R U . . .
H3C H 0.0592 -0.0293 0.8721 0.030 Uiso 1 1 calc R U . . .
N4 N 0.14761(15) 0.2500 0.9943(2) 0.0162(5) Uani 1 2 d S T P . .
N5 N 0.41222(15) 0.2500 0.9974(3) 0.0198(5) Uani 1 2 d S T P . .
O1 O 0.22463(13) 0.2500 1.0449(2) 0.0260(5) Uani 1 2 d S T P . .
O2 O 0.08068(13) 0.2500 1.0711(2) 0.0259(5) Uani 1 2 d S T P . .
O3 O 0.41106(10) 0.1003(2) 0.93203(17) 0.0292(4) Uani 1 1 d . . . . .
O4 O 0.41432(17) 0.2500 1.1258(2) 0.0371(6) Uani 1 2 d S T P . .


_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 1.918(2) . ?
Co1 N3 1.9535(17) . ?
Co1 N3 1.9535(17) 8_565 ?
Co1 N2 1.9652(16) . ?
Co1 N2 1.9652(16) 8_565 ?
Co1 N1 1.979(2) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N1 H1C 0.9000 . ?
N2 H2A 0.9000 . ?
N2 H2B 0.9000 . ?
N2 H2C 0.9000 . ?
N3 H3A 0.9000 . ?
N3 H3B 0.9000 . ?
N3 H3C 0.9000 . ?
N4 O2 1.232(3) . ?
N4 O1 1.235(3) . ?
N5 O4 1.237(3) . ?
N5 O3 1.2506(19) 8_565 ?
N5 O3 1.2506(19) . ?

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 N3 89.34(7) . . ?
N4 Co1 N3 89.34(7) . 8_565 ?
N3 Co1 N3 89.13(11) . 8_565 ?
N4 Co1 N2 89.78(7) . . ?
N3 Co1 N2 89.64(8) . . ?
N3 Co1 N2 178.50(7) 8_565 . ?
N4 Co1 N2 89.78(7) . 8_565 ?
N3 Co1 N2 178.50(7) . 8_565 ?
N3 Co1 N2 89.64(8) 8_565 8_565 ?
N2 Co1 N2 91.57(10) . 8_565 ?
N4 Co1 N1 177.61(9) . . ?
N3 Co1 N1 92.36(7) . . ?
N3 Co1 N1 92.36(7) 8_565 . ?
N2 Co1 N1 88.56(7) . . ?
N2 Co1 N1 88.56(7) 8_565 . ?
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 . . ?
O2 N4 O1 120.0(2) . . ?
O2 N4 Co1 120.57(18) . . ?
O1 N4 Co1 119.46(18) . . ?
O4 N5 O3 120.20(12) . 8_565 ?
O4 N5 O3 120.20(12) . . ?
O3 N5 O3 119.6(2) 8_565 . ?


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 H1C O3 0.90 2.80 3.331(3) 118.7 6_557
N1 H1C O3 0.90 2.16 3.003(2) 155.5 2_554
N1 H1B O3 0.90 2.24 3.003(2) 142.2 7_665
N1 H1A Cl1 0.90 2.50 3.370(2) 161.9 .
N2 H2C Cl1 0.90 2.88 3.3976(18) 117.8 .
N2 H2B Cl1 0.90 2.51 3.3677(18) 159.1 2
N2 H2A O1 0.90 2.46 3.251(2) 146.8 2_554
N2 H2C O3 0.90 2.40 3.106(2) 135.3 .
N3 H3C Cl1 0.90 2.54 3.4177(18) 166.1 2
N3 H3B Cl1 0.90 2.62 3.5151(18) 173.1 3_456
N3 H3A O3 0.90 2.41 3.050(2) 127.9 6_557
N3 H3C O2 0.90 2.66 3.063(2) 108.0 4_547
N3 H3A O4 0.90 2.30 2.961(2) 130.1 2_554

_refine_diff_density_max         0.363
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.078

####################################################################### 
# 
# 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_-40C
_database_code_depnum_ccdc_archive 'CCDC 1470421'
_audit_update_record             
;
2016-03-25 deposited with the CCDC.
2016-05-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_name_common            nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_melting_point          ?
_chemical_formula_moiety         'Co H15 N6 O2, N O3, Cl'
_chemical_formula_sum            'Cl Co H15 N7 O5'
_chemical_formula_weight         287.57

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1484 0.1585 '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           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   14.755(2)
_cell_length_b                   7.2394(11)
_cell_length_c                   9.6181(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1027.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    233(2)
_cell_measurement_reflns_used    10761
_cell_measurement_theta_min      1.45
_cell_measurement_theta_max      29.50

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.859
_exptl_crystal_F_000             592
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    1.946
_shelx_estimated_absorpt_T_min   0.593
_shelx_estimated_absorpt_T_max   0.759
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6603
_exptl_absorpt_correction_T_max  0.7820
_exptl_absorpt_process_details   X-RED
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      233(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 6.67
_diffrn_reflns_number            6950
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.528
_diffrn_reflns_theta_max         26.361
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1133
_reflns_number_gt                983
_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       'X-AREA (Stoe & Cie, 2006)'
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2006)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2006)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0308P)²+0.7001P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1133
_refine_ls_number_parameters     79
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0268
_refine_ls_wR_factor_ref         0.0638
_refine_ls_wR_factor_gt          0.0613
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_restrained_S_all      1.099
_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
Cl1 Cl 0.34822(5) 0.2500 0.52015(8) 0.02150(18) Uani 1 2 d S T P . .
Co1 Co 0.13330(2) 0.2500 0.79615(4) 0.01346(14) Uani 1 2 d S T P . .
N1 N 0.12417(15) 0.2500 0.5908(3) 0.0194(5) Uani 1 2 d S T P . .
H1A H 0.1794 0.2685 0.5538 0.029 Uiso 0.5 1 calc R U P . .
H1B H 0.0866 0.3410 0.5635 0.029 Uiso 0.5 1 calc R U P . .
H1C H 0.1023 0.1405 0.5619 0.029 Uiso 0.5 1 calc R U P . .
N2 N 0.22577(11) 0.0555(2) 0.78139(17) 0.0209(4) Uani 1 1 d . . . . .
H2A H 0.2169 -0.0094 0.7027 0.031 Uiso 1 1 calc R U . . .
H2B H 0.2216 -0.0206 0.8551 0.031 Uiso 1 1 calc R U . . .
H2C H 0.2812 0.1073 0.7795 0.031 Uiso 1 1 calc R U . . .
N3 N 0.03972(11) 0.0606(3) 0.81424(18) 0.0220(4) Uani 1 1 d . . . . .
H3A H 0.0276 0.0122 0.7301 0.033 Uiso 1 1 calc R U . . .
H3B H -0.0110 0.1115 0.8494 0.033 Uiso 1 1 calc R U . . .
H3C H 0.0594 -0.0292 0.8715 0.033 Uiso 1 1 calc R U . . .
N4 N 0.14729(15) 0.2500 0.9942(3) 0.0179(5) Uani 1 2 d S T P . .
N5 N 0.41208(16) 0.2500 0.9980(3) 0.0212(6) Uani 1 2 d S T P . .
O1 O 0.22424(14) 0.2500 1.0452(2) 0.0288(5) Uani 1 2 d S T P . .
O2 O 0.08052(14) 0.2500 1.0710(2) 0.0285(5) Uani 1 2 d S T P . .
O3 O 0.41093(10) 0.1009(2) 0.93271(18) 0.0326(4) Uani 1 1 d . . . . .
O4 O 0.41386(18) 0.2500 1.1265(3) 0.0406(6) Uani 1 2 d S T P . .


_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 1.916(2) . ?
Co1 N3 1.9538(17) 8_565 ?
Co1 N3 1.9538(17) . ?
Co1 N2 1.9659(17) 8_565 ?
Co1 N2 1.9659(17) . ?
Co1 N1 1.979(2) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N1 H1C 0.9000 . ?
N2 H2A 0.9000 . ?
N2 H2B 0.9000 . ?
N2 H2C 0.9000 . ?
N3 H3A 0.9000 . ?
N3 H3B 0.9000 . ?
N3 H3C 0.9000 . ?
N4 O2 1.231(3) . ?
N4 O1 1.237(3) . ?
N5 O4 1.236(3) . ?
N5 O3 1.249(2) . ?
N5 O3 1.249(2) 8_565 ?

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 N3 89.29(7) . 8_565 ?
N4 Co1 N3 89.29(7) . . ?
N3 Co1 N3 89.15(11) 8_565 . ?
N4 Co1 N2 89.83(7) . 8_565 ?
N3 Co1 N2 89.66(8) 8_565 8_565 ?
N3 Co1 N2 178.53(7) . 8_565 ?
N4 Co1 N2 89.83(7) . . ?
N3 Co1 N2 178.53(7) 8_565 . ?
N3 Co1 N2 89.66(8) . . ?
N2 Co1 N2 91.51(10) 8_565 . ?
N4 Co1 N1 177.72(10) . . ?
N3 Co1 N1 92.34(7) 8_565 . ?
N3 Co1 N1 92.34(7) . . ?
N2 Co1 N1 88.58(7) 8_565 . ?
N2 Co1 N1 88.58(7) . . ?
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 . . ?
O2 N4 O1 119.8(2) . . ?
O2 N4 Co1 120.68(19) . . ?
O1 N4 Co1 119.56(19) . . ?
O4 N5 O3 120.19(13) . . ?
O4 N5 O3 120.19(13) . 8_565 ?
O3 N5 O3 119.6(3) . 8_565 ?


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 H1C O3 0.90 2.84 3.334(3) 116.1 6_557
N1 H1C O3 0.90 2.15 3.006(2) 157.8 2_554
N1 H1B O3 0.90 2.26 3.006(2) 139.6 7_665
N1 H1A Cl1 0.90 2.51 3.375(2) 160.1 .
N2 H2C Cl1 0.90 2.88 3.4002(18) 118.7 .
N2 H2B Cl1 0.90 2.52 3.3698(18) 158.2 2
N2 H2A O1 0.90 2.47 3.255(2) 146.5 2_554
N2 H2C O3 0.90 2.42 3.113(2) 134.4 .
N3 H3C Cl1 0.90 2.54 3.4222(19) 166.3 2
N3 H3B Cl1 0.90 2.63 3.5215(18) 173.6 3_456
N3 H3A O3 0.90 2.41 3.056(2) 128.4 6_557
N3 H3C O2 0.90 2.67 3.069(2) 108.0 4_547
N3 H3A O4 0.90 2.31 2.964(2) 129.3 2_554

_refine_diff_density_max         0.269
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.087

####################################################################### 
# 
# 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_-20C
_database_code_depnum_ccdc_archive 'CCDC 1470422'
_audit_update_record             
;
2016-03-25 deposited with the CCDC.
2016-05-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_name_common            nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_melting_point          ?
_chemical_formula_moiety         'Co H15 N6 O2, N O3, Cl'
_chemical_formula_sum            'Cl Co H15 N7 O5'
_chemical_formula_weight         287.57

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1484 0.1585 '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           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   14.770(2)
_cell_length_b                   7.2540(11)
_cell_length_c                   9.6152(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1030.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    253(2)
_cell_measurement_reflns_used    10678
_cell_measurement_theta_min      1.45
_cell_measurement_theta_max      29.50

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.854
_exptl_crystal_F_000             592
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    1.940
_shelx_estimated_absorpt_T_min   0.594
_shelx_estimated_absorpt_T_max   0.760
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6603
_exptl_absorpt_correction_T_max  0.7819
_exptl_absorpt_process_details   X-RED
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      253(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 6.67
_diffrn_reflns_number            6969
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.528
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1139
_reflns_number_gt                978
_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       'X-AREA (Stoe & Cie, 2006)'
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2006)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2006)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0340P)²+0.6438P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1139
_refine_ls_number_parameters     79
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0273
_refine_ls_wR_factor_ref         0.0658
_refine_ls_wR_factor_gt          0.0632
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.001
_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
Cl1 Cl 0.34813(5) 0.2500 0.51986(8) 0.02349(19) Uani 1 2 d S T P . .
Co1 Co 0.13322(2) 0.2500 0.79602(4) 0.01483(14) Uani 1 2 d S T P . .
N1 N 0.12402(16) 0.2500 0.5907(3) 0.0217(5) Uani 1 2 d S T P . .
H1A H 0.1784 0.2702 0.5540 0.033 Uiso 0.5 1 calc R U P . .
H1B H 0.0862 0.3385 0.5638 0.033 Uiso 0.5 1 calc R U P . .
H1C H 0.1033 0.1413 0.5620 0.033 Uiso 0.5 1 calc R U P . .
N2 N 0.22563(11) 0.0562(3) 0.78150(17) 0.0227(4) Uani 1 1 d . . . . .
H2A H 0.2162 -0.0094 0.7047 0.034 Uiso 1 1 calc R U . . .
H2B H 0.2223 -0.0173 0.8554 0.034 Uiso 1 1 calc R U . . .
H2C H 0.2803 0.1077 0.7778 0.034 Uiso 1 1 calc R U . . .
N3 N 0.03974(11) 0.0611(3) 0.81404(18) 0.0238(4) Uani 1 1 d . . . . .
H3A H 0.0281 0.0127 0.7309 0.036 Uiso 1 1 calc R U . . .
H3B H -0.0105 0.1115 0.8482 0.036 Uiso 1 1 calc R U . . .
H3C H 0.0590 -0.0271 0.8712 0.036 Uiso 1 1 calc R U . . .
N4 N 0.14704(15) 0.2500 0.9942(3) 0.0196(5) Uani 1 2 d S T P . .
N5 N 0.41185(16) 0.2500 0.9988(3) 0.0233(6) Uani 1 2 d S T P . .
O1 O 0.22389(14) 0.2500 1.0453(2) 0.0316(5) Uani 1 2 d S T P . .
O2 O 0.08028(14) 0.2500 1.0709(2) 0.0312(5) Uani 1 2 d S T P . .
O3 O 0.41079(11) 0.1015(2) 0.93342(18) 0.0357(4) Uani 1 1 d . . . . .
O4 O 0.41348(19) 0.2500 1.1270(3) 0.0443(7) Uani 1 2 d S T P . .


_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 1.917(2) . ?
Co1 N3 1.9531(18) . ?
Co1 N3 1.9531(17) 8_565 ?
Co1 N2 1.9641(17) . ?
Co1 N2 1.9641(17) 8_565 ?
Co1 N1 1.979(3) . ?
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 O2 1.231(3) . ?
N4 O1 1.237(3) . ?
N5 O4 1.233(4) . ?
N5 O3 1.247(2) . ?
N5 O3 1.247(2) 8_565 ?

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 N3 89.26(7) . . ?
N4 Co1 N3 89.26(7) . 8_565 ?
N3 Co1 N3 89.13(11) . 8_565 ?
N4 Co1 N2 89.81(7) . . ?
N3 Co1 N2 89.73(8) . . ?
N3 Co1 N2 178.54(7) 8_565 . ?
N4 Co1 N2 89.81(7) . 8_565 ?
N3 Co1 N2 178.54(7) . 8_565 ?
N3 Co1 N2 89.74(8) 8_565 8_565 ?
N2 Co1 N2 91.38(10) . 8_565 ?
N4 Co1 N1 177.83(10) . . ?
N3 Co1 N1 92.29(7) . . ?
N3 Co1 N1 92.29(7) 8_565 . ?
N2 Co1 N1 88.67(7) . . ?
N2 Co1 N1 88.67(7) 8_565 . ?
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 . . ?
O2 N4 O1 119.8(2) . . ?
O2 N4 Co1 120.68(19) . . ?
O1 N4 Co1 119.49(19) . . ?
O4 N5 O3 120.26(13) . . ?
O4 N5 O3 120.26(13) . 8_565 ?
O3 N5 O3 119.5(3) . 8_565 ?


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 H1C O3 0.89 2.86 3.337(3) 115.2 6_557
N1 H1C O3 0.89 2.16 3.009(2) 158.9 2_554
N1 H1B O3 0.89 2.28 3.009(2) 138.6 7_665
N1 H1A Cl1 0.89 2.53 3.380(2) 159.4 .
N2 H2C Cl1 0.89 2.87 3.4027(18) 120.1 .
N2 H2B Cl1 0.89 2.54 3.3726(18) 156.9 2
N2 H2A O1 0.89 2.49 3.264(2) 146.3 2_554
N2 H2C O3 0.89 2.44 3.118(2) 133.2 .
N3 H3C Cl1 0.89 2.56 3.4279(19) 166.2 2
N3 H3B Cl1 0.89 2.64 3.5268(19) 173.0 3_456
N3 H3A O3 0.89 2.43 3.062(2) 128.1 6_557
N3 H3C O2 0.89 2.67 3.075(2) 108.5 4_547
N3 H3A O4 0.89 2.32 2.967(2) 129.8 2_554

_refine_diff_density_max         0.292
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.088

####################################################################### 
# 
# 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_0C
_database_code_depnum_ccdc_archive 'CCDC 1470423'
_audit_update_record             
;
2016-03-25 deposited with the CCDC.
2016-05-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_name_common            nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_melting_point          ?
_chemical_formula_moiety         'Co H15 N6 O2, N O3, Cl'
_chemical_formula_sum            'Cl Co H15 N7 O5'
_chemical_formula_weight         287.57

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1484 0.1585 '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           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   14.787(2)
_cell_length_b                   7.2696(11)
_cell_length_c                   9.6113(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1033.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    10361
_cell_measurement_theta_min      1.45
_cell_measurement_theta_max      29.51

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.849
_exptl_crystal_F_000             592
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    1.935
_shelx_estimated_absorpt_T_min   0.594
_shelx_estimated_absorpt_T_max   0.760
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6615
_exptl_absorpt_correction_T_max  0.7829
_exptl_absorpt_process_details   X-RED
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 6.67
_diffrn_reflns_number            6985
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.527
_diffrn_reflns_theta_max         26.367
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1141
_reflns_number_gt                961
_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       'X-AREA (Stoe & Cie, 2006)'
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2006)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2006)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0336P)²+0.6640P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1141
_refine_ls_number_parameters     79
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0272
_refine_ls_wR_factor_ref         0.0663
_refine_ls_wR_factor_gt          0.0638
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.081
_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
Cl1 Cl 0.34810(5) 0.2500 0.51950(8) 0.02556(19) Uani 1 2 d S T P . .
Co1 Co 0.13314(2) 0.2500 0.79590(4) 0.01619(14) Uani 1 2 d S T P . .
N1 N 0.12402(16) 0.2500 0.5905(3) 0.0231(5) Uani 1 2 d S T P . .
H1A H 0.1785 0.2695 0.5538 0.035 Uiso 0.5 1 calc R U P . .
H1B H 0.0865 0.3388 0.5635 0.035 Uiso 0.5 1 calc R U P . .
H1C H 0.1030 0.1417 0.5617 0.035 Uiso 0.5 1 calc R U P . .
N2 N 0.22550(11) 0.0565(3) 0.78152(18) 0.0247(4) Uani 1 1 d . . . . .
H2A H 0.2144 -0.0127 0.7071 0.037 Uiso 1 1 calc R U . . .
H2B H 0.2240 -0.0133 0.8576 0.037 Uiso 1 1 calc R U . . .
H2C H 0.2799 0.1079 0.7734 0.037 Uiso 1 1 calc R U . . .
N3 N 0.03981(11) 0.0615(3) 0.81384(19) 0.0258(4) Uani 1 1 d . . . . .
H3A H 0.0281 0.0134 0.7306 0.039 Uiso 1 1 calc R U . . .
H3B H -0.0103 0.1118 0.8482 0.039 Uiso 1 1 calc R U . . .
H3C H 0.0591 -0.0266 0.8709 0.039 Uiso 1 1 calc R U . . .
N4 N 0.14681(16) 0.2500 0.9941(3) 0.0216(6) Uani 1 2 d S T P . .
N5 N 0.41166(16) 0.2500 0.9992(3) 0.0254(6) Uani 1 2 d S T P . .
O1 O 0.22352(14) 0.2500 1.0456(2) 0.0342(6) Uani 1 2 d S T P . .
O2 O 0.08023(15) 0.2500 1.0709(2) 0.0340(6) Uani 1 2 d S T P . .
O3 O 0.41060(11) 0.1019(2) 0.93400(19) 0.0394(4) Uani 1 1 d . . . . .
O4 O 0.4131(2) 0.2500 1.1277(3) 0.0479(7) Uani 1 2 d S T P . .


_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 1.916(3) . ?
Co1 N3 1.9522(18) . ?
Co1 N3 1.9522(18) 8_565 ?
Co1 N2 1.9655(18) 8_565 ?
Co1 N2 1.9655(18) . ?
Co1 N1 1.979(3) . ?
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 O2 1.230(3) . ?
N4 O1 1.238(3) . ?
N5 O4 1.236(4) . ?
N5 O3 1.246(2) . ?
N5 O3 1.246(2) 8_565 ?

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 N3 89.24(7) . . ?
N4 Co1 N3 89.24(7) . 8_565 ?
N3 Co1 N3 89.14(11) . 8_565 ?
N4 Co1 N2 89.81(7) . 8_565 ?
N3 Co1 N2 178.52(8) . 8_565 ?
N3 Co1 N2 89.72(8) 8_565 8_565 ?
N4 Co1 N2 89.81(7) . . ?
N3 Co1 N2 89.72(8) . . ?
N3 Co1 N2 178.52(8) 8_565 . ?
N2 Co1 N2 91.41(11) 8_565 . ?
N4 Co1 N1 177.85(10) . . ?
N3 Co1 N1 92.29(7) . . ?
N3 Co1 N1 92.29(7) 8_565 . ?
N2 Co1 N1 88.69(7) 8_565 . ?
N2 Co1 N1 88.69(7) . . ?
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 . . ?
O2 N4 O1 119.6(3) . . ?
O2 N4 Co1 120.8(2) . . ?
O1 N4 Co1 119.63(19) . . ?
O4 N5 O3 120.20(14) . . ?
O4 N5 O3 120.20(14) . 8_565 ?
O3 N5 O3 119.6(3) . 8_565 ?


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 H1C O3 0.89 2.86 3.343(3) 115.6 6_557
N1 H1C O3 0.89 2.16 3.011(2) 158.8 2_554
N1 H1B O3 0.89 2.28 3.011(2) 139.0 7_665
N1 H1A Cl1 0.89 2.53 3.383(3) 159.7 .
N2 H2C Cl1 0.89 2.84 3.4070(19) 123.3 .
N2 H2B Cl1 0.89 2.55 3.3734(19) 153.5 2
N2 H2A O1 0.89 2.50 3.267(2) 145.4 2_554
N2 H2C O3 0.89 2.47 3.122(3) 130.1 .
N3 H3C Cl1 0.89 2.56 3.433(2) 166.2 2
N3 H3B Cl1 0.89 2.65 3.5325(19) 173.0 3_456
N3 H3A O3 0.89 2.44 3.068(3) 128.2 6_557
N3 H3C O2 0.89 2.68 3.083(2) 108.6 4_547
N3 H3A O4 0.89 2.32 2.969(3) 129.3 2_554

_refine_diff_density_max         0.298
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.090

####################################################################### 
# 
# 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_20C
_database_code_depnum_ccdc_archive 'CCDC 1470424'
_audit_update_record             
;
2016-03-25 deposited with the CCDC.
2016-05-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_name_common            nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_melting_point          ?
_chemical_formula_moiety         'Co H15 N6 O2, N O3, Cl'
_chemical_formula_sum            'Cl Co H15 N7 O5'
_chemical_formula_weight         287.57

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1484 0.1585 '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           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   14.804(2)
_cell_length_b                   7.2851(11)
_cell_length_c                   9.6112(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1036.6(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    10181
_cell_measurement_theta_min      1.45
_cell_measurement_theta_max      29.50

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.843
_exptl_crystal_F_000             592
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    1.928
_shelx_estimated_absorpt_T_min   0.595
_shelx_estimated_absorpt_T_max   0.761
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6630
_exptl_absorpt_correction_T_max  0.7839
_exptl_absorpt_process_details   X-RED
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 6.67
_diffrn_reflns_number            6968
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.527
_diffrn_reflns_theta_max         26.347
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             1141
_reflns_number_gt                966
_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       'X-AREA (Stoe & Cie, 2006)'
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2006)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2006)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0301P)²+0.7386P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1141
_refine_ls_number_parameters     79
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0268
_refine_ls_wR_factor_ref         0.0647
_refine_ls_wR_factor_gt          0.0619
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      1.084
_refine_ls_shift/su_max          0.001
_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
Cl1 Cl 0.34803(5) 0.2500 0.51928(8) 0.0278(2) Uani 1 2 d S T P . .
Co1 Co 0.13306(2) 0.2500 0.79581(4) 0.01755(14) Uani 1 2 d S T P . .
N1 N 0.12398(17) 0.2500 0.5903(3) 0.0258(6) Uani 1 2 d S T P . .
H1A H 0.1780 0.2734 0.5537 0.039 Uiso 0.5 1 calc R U P . .
H1B H 0.0850 0.3360 0.5634 0.039 Uiso 0.5 1 calc R U P . .
H1C H 0.1049 0.1406 0.5613 0.039 Uiso 0.5 1 calc R U P . .
N2 N 0.22540(11) 0.0571(3) 0.78155(19) 0.0264(4) Uani 1 1 d . . . . .
H2A H 0.2129 -0.0152 0.7094 0.040 Uiso 1 1 calc R U . . .
H2B H 0.2257 -0.0093 0.8593 0.040 Uiso 1 1 calc R U . . .
H2C H 0.2794 0.1084 0.7695 0.040 Uiso 1 1 calc R U . . .
N3 N 0.03973(11) 0.0617(3) 0.81365(19) 0.0277(4) Uani 1 1 d . . . . .
H3A H 0.0266 0.0167 0.7300 0.042 Uiso 1 1 calc R U . . .
H3B H -0.0097 0.1109 0.8510 0.042 Uiso 1 1 calc R U . . .
H3C H 0.0597 -0.0283 0.8682 0.042 Uiso 1 1 calc R U . . .
N4 N 0.14647(16) 0.2500 0.9943(3) 0.0235(6) Uani 1 2 d S T P . .
N5 N 0.41148(17) 0.2500 0.9999(3) 0.0277(6) Uani 1 2 d S T P . .
O1 O 0.22310(15) 0.2500 1.0457(2) 0.0379(6) Uani 1 2 d S T P . .
O2 O 0.08008(15) 0.2500 1.0707(2) 0.0373(6) Uani 1 2 d S T P . .
O3 O 0.41045(12) 0.1024(2) 0.9348(2) 0.0427(4) Uani 1 1 d . . . . .
O4 O 0.4127(2) 0.2500 1.1281(3) 0.0516(7) Uani 1 2 d S T P . .


_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 1.918(3) . ?
Co1 N3 1.9545(18) . ?
Co1 N3 1.9545(18) 8_565 ?
Co1 N2 1.9653(18) 8_565 ?
Co1 N2 1.9653(18) . ?
Co1 N1 1.980(3) . ?
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 O2 1.227(3) . ?
N4 O1 1.237(3) . ?
N5 O4 1.233(4) . ?
N5 O3 1.244(2) 8_565 ?
N5 O3 1.244(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 N3 89.19(8) . . ?
N4 Co1 N3 89.19(8) . 8_565 ?
N3 Co1 N3 89.15(11) . 8_565 ?
N4 Co1 N2 89.85(7) . 8_565 ?
N3 Co1 N2 178.56(8) . 8_565 ?
N3 Co1 N2 89.77(8) 8_565 8_565 ?
N4 Co1 N2 89.85(7) . . ?
N3 Co1 N2 89.77(8) . . ?
N3 Co1 N2 178.56(8) 8_565 . ?
N2 Co1 N2 91.30(11) 8_565 . ?
N4 Co1 N1 177.95(10) . . ?
N3 Co1 N1 92.27(7) . . ?
N3 Co1 N1 92.27(7) 8_565 . ?
N2 Co1 N1 88.72(7) 8_565 . ?
N2 Co1 N1 88.72(7) . . ?
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 . . ?
O2 N4 O1 119.7(3) . . ?
O2 N4 Co1 120.8(2) . . ?
O1 N4 Co1 119.5(2) . . ?
O4 N5 O3 120.20(14) . 8_565 ?
O4 N5 O3 120.20(14) . . ?
O3 N5 O3 119.6(3) 8_565 . ?


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 H1C O3 0.89 2.89 3.348(3) 113.5 6_557
N1 H1C O3 0.89 2.16 3.014(2) 160.6 2_554
N1 H1B O3 0.89 2.30 3.014(2) 136.9 7_665
N1 H1A Cl1 0.89 2.54 3.386(3) 158.0 .
N2 H2C Cl1 0.89 2.81 3.4095(19) 126.2 .
N2 H2B Cl1 0.89 2.57 3.3775(19) 150.4 2
N2 H2A O1 0.89 2.51 3.275(2) 144.4 2_554
N2 H2C O3 0.89 2.51 3.128(3) 127.2 .
N3 H3C Cl1 0.89 2.57 3.439(2) 166.9 2
N3 H3B Cl1 0.89 2.65 3.5376(19) 175.7 3_456
N3 H3A O3 0.89 2.42 3.074(3) 130.7 6_557
N3 H3C O2 0.89 2.69 3.088(2) 108.3 4_547
N3 H3A O4 0.89 2.35 2.972(3) 126.6 2_554

_refine_diff_density_max         0.323
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.079

####################################################################### 
# 
# 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_30C
_database_code_depnum_ccdc_archive 'CCDC 1470425'
_audit_update_record             
;
2016-03-25 deposited with the CCDC.
2016-05-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_name_common            nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_melting_point          ?
_chemical_formula_moiety         'Co H15 N6 O2, N O3, Cl'
_chemical_formula_sum            'Cl Co H15 N7 O5'
_chemical_formula_weight         287.57

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1484 0.1585 '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           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   14.815(2)
_cell_length_b                   7.2951(11)
_cell_length_c                   9.6129(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1039.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    303(2)
_cell_measurement_reflns_used    10379
_cell_measurement_theta_min      1.45
_cell_measurement_theta_max      29.49

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.838
_exptl_crystal_F_000             592
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    1.924
_shelx_estimated_absorpt_T_min   0.596
_shelx_estimated_absorpt_T_max   0.761
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6619
_exptl_absorpt_correction_T_max  0.7842
_exptl_absorpt_process_details   X-RED
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      303(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 6.67
_diffrn_reflns_number            6985
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.526
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             1143
_reflns_number_gt                964
_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       'X-AREA (Stoe & Cie, 2006)'
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2006)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2006)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0285P)²+0.6148P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1143
_refine_ls_number_parameters     79
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0266
_refine_ls_wR_factor_ref         0.0631
_refine_ls_wR_factor_gt          0.0608
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_restrained_S_all      1.123
_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
Cl1 Cl 0.34802(5) 0.2500 0.51915(8) 0.0292(2) Uani 1 2 d S T P . .
Co1 Co 0.13304(2) 0.2500 0.79573(4) 0.01856(14) Uani 1 2 d S T P . .
N1 N 0.12412(16) 0.2500 0.5900(3) 0.0270(6) Uani 1 2 d S T P . .
H1A H 0.1783 0.2715 0.5535 0.040 Uiso 0.5 1 calc R U P . .
H1B H 0.0859 0.3371 0.5630 0.040 Uiso 0.5 1 calc R U P . .
H1C H 0.1042 0.1414 0.5611 0.040 Uiso 0.5 1 calc R U P . .
N2 N 0.22536(11) 0.0573(3) 0.78141(18) 0.0278(4) Uani 1 1 d . . . . .
H2A H 0.2119 -0.0171 0.7110 0.042 Uiso 1 1 calc R U . . .
H2B H 0.2269 -0.0066 0.8602 0.042 Uiso 1 1 calc R U . . .
H2C H 0.2790 0.1085 0.7665 0.042 Uiso 1 1 calc R U . . .
N3 N 0.03976(11) 0.0622(3) 0.81346(19) 0.0293(4) Uani 1 1 d . . . . .
H3A H 0.0282 0.0142 0.7302 0.044 Uiso 1 1 calc R U . . .
H3B H -0.0103 0.1123 0.8476 0.044 Uiso 1 1 calc R U . . .
H3C H 0.0589 -0.0256 0.8706 0.044 Uiso 1 1 calc R U . . .
N4 N 0.14656(16) 0.2500 0.9942(3) 0.0246(6) Uani 1 2 d S T P . .
N5 N 0.41140(16) 0.2500 1.0001(3) 0.0289(6) Uani 1 2 d S T P . .
O1 O 0.22300(14) 0.2500 1.0458(2) 0.0398(6) Uani 1 2 d S T P . .
O2 O 0.07992(15) 0.2500 1.0707(2) 0.0395(6) Uani 1 2 d S T P . .
O3 O 0.41045(12) 0.1026(2) 0.9350(2) 0.0453(4) Uani 1 1 d . . . . .
O4 O 0.4124(2) 0.2500 1.1286(3) 0.0550(7) Uani 1 2 d S T P . .


_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 1.919(3) . ?
Co1 N3 1.9535(18) 8_565 ?
Co1 N3 1.9535(18) . ?
Co1 N2 1.9659(17) . ?
Co1 N2 1.9659(17) 8_565 ?
Co1 N1 1.982(3) . ?
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 O2 1.231(3) . ?
N4 O1 1.236(3) . ?
N5 O4 1.235(4) . ?
N5 O3 1.244(2) 8_565 ?
N5 O3 1.244(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 N3 89.26(7) . 8_565 ?
N4 Co1 N3 89.26(7) . . ?
N3 Co1 N3 89.08(11) 8_565 . ?
N4 Co1 N2 89.83(7) . . ?
N3 Co1 N2 178.58(7) 8_565 . ?
N3 Co1 N2 89.82(8) . . ?
N4 Co1 N2 89.83(7) . 8_565 ?
N3 Co1 N2 89.82(8) 8_565 8_565 ?
N3 Co1 N2 178.58(7) . 8_565 ?
N2 Co1 N2 91.27(11) . 8_565 ?
N4 Co1 N1 177.83(10) . . ?
N3 Co1 N1 92.28(7) 8_565 . ?
N3 Co1 N1 92.28(7) . . ?
N2 Co1 N1 88.65(7) . . ?
N2 Co1 N1 88.65(7) 8_565 . ?
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 . . ?
O2 N4 O1 119.7(3) . . ?
O2 N4 Co1 120.7(2) . . ?
O1 N4 Co1 119.63(19) . . ?
O4 N5 O3 120.22(14) . 8_565 ?
O4 N5 O3 120.22(14) . . ?
O3 N5 O3 119.6(3) 8_565 . ?


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 H1C O3 0.89 2.88 3.352(3) 114.5 6_557
N1 H1C O3 0.89 2.16 3.016(2) 160.0 2_554
N1 H1B O3 0.89 2.30 3.016(2) 138.1 7_665
N1 H1A Cl1 0.89 2.54 3.386(3) 158.9 .
N2 H2C Cl1 0.89 2.79 3.4109(19) 128.4 .
N2 H2B Cl1 0.89 2.59 3.3811(19) 148.1 2
N2 H2A O1 0.89 2.52 3.277(2) 143.6 2_554
N2 H2C O3 0.89 2.53 3.132(3) 125.2 .
N3 H3C Cl1 0.89 2.57 3.444(2) 166.1 2
N3 H3B Cl1 0.89 2.66 3.5407(19) 172.8 3_456
N3 H3A O3 0.89 2.45 3.076(3) 128.1 6_557
N3 H3C O2 0.89 2.69 3.093(2) 108.9 4_547
N3 H3A O4 0.89 2.33 2.974(3) 129.0 2_554

_refine_diff_density_max         0.307
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.074

####################################################################### 
# 
# 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_40C
_database_code_depnum_ccdc_archive 'CCDC 1470426'
_audit_update_record             
;
2016-03-25 deposited with the CCDC.
2016-05-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_name_common            nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_melting_point          ?
_chemical_formula_moiety         'Co H15 N6 O2, N O3, Cl'
_chemical_formula_sum            'Cl Co H15 N7 O5'
_chemical_formula_weight         287.57

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1484 0.1585 '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           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   14.825(2)
_cell_length_b                   7.3004(11)
_cell_length_c                   9.6126(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1040.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    313(2)
_cell_measurement_reflns_used    10213
_cell_measurement_theta_min      1.47
_cell_measurement_theta_max      29.50

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.836
_exptl_crystal_F_000             592
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    1.921
_shelx_estimated_absorpt_T_min   0.596
_shelx_estimated_absorpt_T_max   0.761
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6618
_exptl_absorpt_correction_T_max  0.7842
_exptl_absorpt_process_details   X-RED
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      313(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 6.67
_diffrn_reflns_number            6992
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.525
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             1144
_reflns_number_gt                960
_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       'X-AREA (Stoe & Cie, 2006)'
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2006)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2006)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0327P)²+0.3978P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1144
_refine_ls_number_parameters     79
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0268
_refine_ls_wR_factor_ref         0.0647
_refine_ls_wR_factor_gt          0.0624
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_restrained_S_all      1.125
_refine_ls_shift/su_max          0.001
_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
Cl1 Cl 0.34797(5) 0.2500 0.51906(8) 0.0305(2) Uani 1 2 d S T P . .
Co1 Co 0.13300(2) 0.2500 0.79569(4) 0.01953(14) Uani 1 2 d S T P . .
N1 N 0.12414(16) 0.2500 0.5899(3) 0.0279(5) Uani 1 2 d S T P . .
H1A H 0.1779 0.2751 0.5535 0.042 Uiso 0.5 1 calc R U P . .
H1B H 0.0846 0.3346 0.5630 0.042 Uiso 0.5 1 calc R U P . .
H1C H 0.1059 0.1403 0.5608 0.042 Uiso 0.5 1 calc R U P . .
N2 N 0.22524(11) 0.0575(3) 0.78134(18) 0.0292(4) Uani 1 1 d . . . . .
H2A H 0.2148 -0.0103 0.7061 0.044 Uiso 1 1 calc R U . . .
H2B H 0.2232 -0.0132 0.8567 0.044 Uiso 1 1 calc R U . . .
H2C H 0.2795 0.1088 0.7747 0.044 Uiso 1 1 calc R U . . .
N3 N 0.03967(11) 0.0622(3) 0.81332(19) 0.0310(4) Uani 1 1 d . . . . .
H3A H 0.0292 0.0123 0.7304 0.046 Uiso 1 1 calc R U . . .
H3B H -0.0108 0.1129 0.8454 0.046 Uiso 1 1 calc R U . . .
H3C H 0.0582 -0.0241 0.8722 0.046 Uiso 1 1 calc R U . . .
N4 N 0.14634(15) 0.2500 0.9946(3) 0.0255(5) Uani 1 2 d S T P . .
N5 N 0.41121(16) 0.2500 1.0006(3) 0.0301(6) Uani 1 2 d S T P . .
O1 O 0.22276(14) 0.2500 1.0459(2) 0.0419(6) Uani 1 2 d S T P . .
O2 O 0.07982(15) 0.2500 1.0706(2) 0.0408(6) Uani 1 2 d S T P . .
O3 O 0.41041(12) 0.1029(2) 0.9353(2) 0.0475(4) Uani 1 1 d . . . . .
O4 O 0.4121(2) 0.2500 1.1285(3) 0.0571(7) Uani 1 2 d S T P . .


_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 1.922(2) . ?
Co1 N3 1.9550(18) . ?
Co1 N3 1.9550(18) 8_565 ?
Co1 N2 1.9658(17) . ?
Co1 N2 1.9658(17) 8_565 ?
Co1 N1 1.983(3) . ?
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 O2 1.228(3) . ?
N4 O1 1.236(3) . ?
N5 O4 1.230(4) . ?
N5 O3 1.244(2) 8_565 ?
N5 O3 1.244(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 N3 89.23(7) . . ?
N4 Co1 N3 89.23(7) . 8_565 ?
N3 Co1 N3 89.05(11) . 8_565 ?
N4 Co1 N2 89.90(7) . . ?
N3 Co1 N2 89.83(8) . . ?
N3 Co1 N2 178.59(7) 8_565 . ?
N4 Co1 N2 89.90(7) . 8_565 ?
N3 Co1 N2 178.59(7) . 8_565 ?
N3 Co1 N2 89.83(8) 8_565 8_565 ?
N2 Co1 N2 91.28(11) . 8_565 ?
N4 Co1 N1 177.89(10) . . ?
N3 Co1 N1 92.27(7) . . ?
N3 Co1 N1 92.27(7) 8_565 . ?
N2 Co1 N1 88.63(7) . . ?
N2 Co1 N1 88.62(7) 8_565 . ?
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 . . ?
O2 N4 O1 119.9(3) . . ?
O2 N4 Co1 120.64(19) . . ?
O1 N4 Co1 119.44(19) . . ?
O4 N5 O3 120.28(14) . 8_565 ?
O4 N5 O3 120.28(14) . . ?
O3 N5 O3 119.4(3) 8_565 . ?


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 H1C O3 0.89 2.91 3.354(3) 112.5 6_557
N1 H1C O3 0.89 2.16 3.018(2) 161.6 2_554
N1 H1B O3 0.89 2.31 3.018(2) 136.1 7_665
N1 H1A Cl1 0.89 2.55 3.387(2) 157.3 .
N2 H2C Cl1 0.89 2.85 3.4121(18) 122.4 .
N2 H2B Cl1 0.89 2.56 3.3821(19) 154.6 2
N2 H2A O1 0.89 2.51 3.279(2) 145.3 2_554
N2 H2C O3 0.89 2.48 3.136(3) 131.0 .
N3 H3C Cl1 0.89 2.58 3.447(2) 165.3 2
N3 H3B Cl1 0.89 2.66 3.5428(19) 170.9 3_456
N3 H3A O3 0.89 2.46 3.078(3) 126.5 6_557
N3 H3C O2 0.89 2.68 3.095(2) 109.3 4_547
N3 H3A O4 0.89 2.32 2.977(3) 130.6 2_554

_refine_diff_density_max         0.309
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.075

####################################################################### 
# 
# 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_50C
_database_code_depnum_ccdc_archive 'CCDC 1470427'
_audit_update_record             
;
2016-03-25 deposited with the CCDC.
2016-05-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_name_common            nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_melting_point          ?
_chemical_formula_moiety         'Co H15 N6 O2, N O3, Cl'
_chemical_formula_sum            'Cl Co H15 N7 O5'
_chemical_formula_weight         287.57

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1484 0.1585 '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           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   14.832(2)
_cell_length_b                   7.3084(11)
_cell_length_c                   9.6102(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1041.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    323(2)
_cell_measurement_reflns_used    10087
_cell_measurement_theta_min      1.46
_cell_measurement_theta_max      29.51

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.834
_exptl_crystal_F_000             592
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    1.919
_shelx_estimated_absorpt_T_min   0.597
_shelx_estimated_absorpt_T_max   0.762
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6618
_exptl_absorpt_correction_T_max  0.7842
_exptl_absorpt_process_details   X-RED
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      323(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 6.67
_diffrn_reflns_number            7004
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.525
_diffrn_reflns_theta_max         26.367
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             1146
_reflns_number_gt                961
_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       'X-AREA (Stoe & Cie, 2006)'
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2006)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2006)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0331P)²+0.4917P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1146
_refine_ls_number_parameters     79
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0273
_refine_ls_wR_factor_ref         0.0661
_refine_ls_wR_factor_gt          0.0635
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_restrained_S_all      1.106
_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
Cl1 Cl 0.34795(5) 0.2500 0.51892(8) 0.0316(2) Uani 1 2 d S T P . .
Co1 Co 0.13296(2) 0.2500 0.79567(4) 0.02023(14) Uani 1 2 d S T P . .
N1 N 0.12413(16) 0.2500 0.5898(3) 0.0293(6) Uani 1 2 d S T P . .
H1A H 0.1780 0.2738 0.5534 0.044 Uiso 0.5 1 calc R U P . .
H1B H 0.0850 0.3353 0.5629 0.044 Uiso 0.5 1 calc R U P . .
H1C H 0.1053 0.1408 0.5608 0.044 Uiso 0.5 1 calc R U P . .
N2 N 0.22525(11) 0.0577(3) 0.78133(18) 0.0302(4) Uani 1 1 d . . . . .
H2A H 0.2121 -0.0160 0.7105 0.045 Uiso 1 1 calc R U . . .
H2B H 0.2265 -0.0067 0.8599 0.045 Uiso 1 1 calc R U . . .
H2C H 0.2789 0.1089 0.7671 0.045 Uiso 1 1 calc R U . . .
N3 N 0.03974(11) 0.0624(3) 0.81322(19) 0.0318(4) Uani 1 1 d . . . . .
H3A H 0.0287 0.0137 0.7301 0.048 Uiso 1 1 calc R U . . .
H3B H -0.0105 0.1128 0.8464 0.048 Uiso 1 1 calc R U . . .
H3C H 0.0586 -0.0246 0.8711 0.048 Uiso 1 1 calc R U . . .
N4 N 0.14633(16) 0.2500 0.9943(3) 0.0266(6) Uani 1 2 d S T P . .
N5 N 0.41129(17) 0.2500 1.0005(3) 0.0315(6) Uani 1 2 d S T P . .
O1 O 0.22259(15) 0.2500 1.0459(2) 0.0433(6) Uani 1 2 d S T P . .
O2 O 0.07975(15) 0.2500 1.0707(2) 0.0426(6) Uani 1 2 d S T P . .
O3 O 0.41028(12) 0.1032(2) 0.9356(2) 0.0493(5) Uani 1 1 d . . . . .
O4 O 0.4121(2) 0.2500 1.1288(3) 0.0591(8) Uani 1 2 d S T P . .


_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 1.920(3) . ?
Co1 N3 1.9542(18) 8_565 ?
Co1 N3 1.9542(19) . ?
Co1 N2 1.9665(18) 8_565 ?
Co1 N2 1.9665(18) . ?
Co1 N1 1.982(3) . ?
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 O2 1.230(3) . ?
N4 O1 1.235(3) . ?
N5 O4 1.233(4) . ?
N5 O3 1.241(2) . ?
N5 O3 1.241(2) 8_565 ?

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 N3 89.27(8) . 8_565 ?
N4 Co1 N3 89.27(8) . . ?
N3 Co1 N3 89.08(12) 8_565 . ?
N4 Co1 N2 89.87(7) . 8_565 ?
N3 Co1 N2 89.85(9) 8_565 8_565 ?
N3 Co1 N2 178.64(8) . 8_565 ?
N4 Co1 N2 89.87(7) . . ?
N3 Co1 N2 178.64(8) 8_565 . ?
N3 Co1 N2 89.85(9) . . ?
N2 Co1 N2 91.21(11) 8_565 . ?
N4 Co1 N1 177.86(10) . . ?
N3 Co1 N1 92.26(7) 8_565 . ?
N3 Co1 N1 92.26(7) . . ?
N2 Co1 N1 88.63(7) 8_565 . ?
N2 Co1 N1 88.63(7) . . ?
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 . . ?
O2 N4 O1 119.7(3) . . ?
O2 N4 Co1 120.7(2) . . ?
O1 N4 Co1 119.6(2) . . ?
O4 N5 O3 120.15(14) . . ?
O4 N5 O3 120.15(14) . 8_565 ?
O3 N5 O3 119.7(3) . 8_565 ?


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 H1C O3 0.89 2.91 3.357(3) 113.1 6_557
N1 H1C O3 0.89 2.16 3.020(2) 161.2 2_554
N1 H1B O3 0.89 2.31 3.020(2) 136.8 7_665
N1 H1A Cl1 0.89 2.55 3.389(3) 157.9 .
N2 H2C Cl1 0.89 2.79 3.4126(19) 127.9 .
N2 H2B Cl1 0.89 2.59 3.3839(19) 148.7 2
N2 H2A O1 0.89 2.52 3.283(2) 143.7 2_554
N2 H2C O3 0.89 2.53 3.137(3) 125.7 .
N3 H3C Cl1 0.89 2.58 3.449(2) 165.7 2
N3 H3B Cl1 0.89 2.66 3.546(2) 171.9 3_456
N3 H3A O3 0.89 2.46 3.081(3) 127.3 6_557
N3 H3C O2 0.89 2.69 3.098(2) 109.2 4_547
N3 H3A O4 0.89 2.33 2.978(3) 129.5 2_554

_refine_diff_density_max         0.320
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.075

####################################################################### 
# 
# 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_60C
_database_code_depnum_ccdc_archive 'CCDC 1470428'
_audit_update_record             
;
2016-03-25 deposited with the CCDC.
2016-05-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_name_common            nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_melting_point          ?
_chemical_formula_moiety         'Co H15 N6 O2, N O3, Cl'
_chemical_formula_sum            'Cl Co H15 N7 O5'
_chemical_formula_weight         287.57

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1484 0.1585 '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           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   14.841(2)
_cell_length_b                   7.3153(11)
_cell_length_c                   9.6100(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1043.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    333(2)
_cell_measurement_reflns_used    9978
_cell_measurement_theta_min      1.45
_cell_measurement_theta_max      29.50

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.831
_exptl_crystal_F_000             592
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    1.916
_shelx_estimated_absorpt_T_min   0.597
_shelx_estimated_absorpt_T_max   0.762
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6632
_exptl_absorpt_correction_T_max  0.7851
_exptl_absorpt_process_details   X-RED
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      333(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 6.67
_diffrn_reflns_number            7017
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.525
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             1148
_reflns_number_gt                974
_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       'X-AREA (Stoe & Cie, 2006)'
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2006)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2006)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0361P)²+0.3459P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1148
_refine_ls_number_parameters     79
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0282
_refine_ls_wR_factor_ref         0.0673
_refine_ls_wR_factor_gt          0.0651
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_restrained_S_all      1.106
_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
Cl1 Cl 0.34789(5) 0.2500 0.51895(8) 0.0329(2) Uani 1 2 d S T P . .
Co1 Co 0.13293(2) 0.2500 0.79563(4) 0.02107(14) Uani 1 2 d S T P . .
N1 N 0.12412(16) 0.2500 0.5897(3) 0.0307(6) Uani 1 2 d S T P . .
H1A H 0.1777 0.2764 0.5533 0.046 Uiso 0.5 1 calc R U P . .
H1B H 0.0841 0.3334 0.5628 0.046 Uiso 0.5 1 calc R U P . .
H1C H 0.1066 0.1401 0.5605 0.046 Uiso 0.5 1 calc R U P . .
N2 N 0.22513(11) 0.0579(3) 0.78131(18) 0.0311(4) Uani 1 1 d . . . . .
H2A H 0.2138 -0.0117 0.7074 0.047 Uiso 1 1 calc R U . . .
H2B H 0.2241 -0.0107 0.8578 0.047 Uiso 1 1 calc R U . . .
H2C H 0.2792 0.1092 0.7722 0.047 Uiso 1 1 calc R U . . .
N3 N 0.03975(11) 0.0628(3) 0.81309(19) 0.0330(4) Uani 1 1 d . . . . .
H3A H 0.0302 0.0113 0.7305 0.050 Uiso 1 1 calc R U . . .
H3B H -0.0110 0.1139 0.8433 0.050 Uiso 1 1 calc R U . . .
H3C H 0.0577 -0.0221 0.8734 0.050 Uiso 1 1 calc R U . . .
N4 N 0.14618(16) 0.2500 0.9945(3) 0.0272(6) Uani 1 2 d S T P . .
N5 N 0.41114(17) 0.2500 1.0011(3) 0.0327(6) Uani 1 2 d S T P . .
O1 O 0.22230(15) 0.2500 1.0461(2) 0.0452(6) Uani 1 2 d S T P . .
O2 O 0.07971(15) 0.2500 1.0705(2) 0.0444(6) Uani 1 2 d S T P . .
O3 O 0.41021(12) 0.1036(2) 0.9359(2) 0.0517(5) Uani 1 1 d . . . . .
O4 O 0.4118(2) 0.2500 1.1292(3) 0.0621(8) Uani 1 2 d S T P . .


_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 1.921(3) . ?
Co1 N3 1.9535(18) 8_565 ?
Co1 N3 1.9535(18) . ?
Co1 N2 1.9662(17) . ?
Co1 N2 1.9662(18) 8_565 ?
Co1 N1 1.983(3) . ?
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 O2 1.228(3) . ?
N4 O1 1.234(3) . ?
N5 O4 1.230(4) . ?
N5 O3 1.241(2) . ?
N5 O3 1.241(2) 8_565 ?

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 N3 89.26(7) . 8_565 ?
N4 Co1 N3 89.26(7) . . ?
N3 Co1 N3 89.02(12) 8_565 . ?
N4 Co1 N2 89.91(7) . . ?
N3 Co1 N2 178.62(7) 8_565 . ?
N3 Co1 N2 89.86(8) . . ?
N4 Co1 N2 89.91(7) . 8_565 ?
N3 Co1 N2 89.86(8) 8_565 8_565 ?
N3 Co1 N2 178.62(7) . 8_565 ?
N2 Co1 N2 91.24(11) . 8_565 ?
N4 Co1 N1 177.91(10) . . ?
N3 Co1 N1 92.24(7) 8_565 . ?
N3 Co1 N1 92.24(7) . . ?
N2 Co1 N1 88.62(7) . . ?
N2 Co1 N1 88.62(7) 8_565 . ?
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 . . ?
O2 N4 O1 119.8(3) . . ?
O2 N4 Co1 120.6(2) . . ?
O1 N4 Co1 119.6(2) . . ?
O4 N5 O3 120.34(14) . . ?
O4 N5 O3 120.34(14) . 8_565 ?
O3 N5 O3 119.3(3) . 8_565 ?


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 H1C O3 0.89 2.93 3.360(3) 111.7 6_557
N1 H1C O3 0.89 2.16 3.022(2) 162.3 2_554
N1 H1B O3 0.89 2.32 3.022(2) 135.3 7_665
N1 H1A Cl1 0.89 2.55 3.390(3) 156.6 .
N2 H2C Cl1 0.89 2.83 3.4134(19) 124.2 .
N2 H2B Cl1 0.89 2.57 3.3857(19) 152.7 2
N2 H2A O1 0.89 2.52 3.285(2) 144.7 2_554
N2 H2C O3 0.89 2.50 3.141(3) 129.2 .
N3 H3C Cl1 0.89 2.59 3.454(2) 164.4 2
N3 H3B Cl1 0.89 2.67 3.5480(19) 169.3 3_456
N3 H3A O3 0.89 2.49 3.084(3) 125.0 6_557
N3 H3C O2 0.89 2.69 3.103(2) 109.7 4_547
N3 H3A O4 0.89 2.31 2.980(3) 131.8 2_554

_refine_diff_density_max         0.298
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.075

####################################################################### 
# 
# 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_70C
_database_code_depnum_ccdc_archive 'CCDC 1470429'
_audit_update_record             
;
2016-03-25 deposited with the CCDC.
2016-05-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_name_common            nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_melting_point          ?
_chemical_formula_moiety         'Co H15 N6 O2, N O3, Cl'
_chemical_formula_sum            'Cl Co H15 N7 O5'
_chemical_formula_weight         287.57

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1484 0.1585 '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           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   14.851(2)
_cell_length_b                   7.3236(11)
_cell_length_c                   9.6090(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1045.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    343(2)
_cell_measurement_reflns_used    9936
_cell_measurement_theta_min      1.47
_cell_measurement_theta_max      29.50

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.828
_exptl_crystal_F_000             592
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    1.913
_shelx_estimated_absorpt_T_min   0.598
_shelx_estimated_absorpt_T_max   0.762
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6632
_exptl_absorpt_correction_T_max  0.7851
_exptl_absorpt_process_details   X-RED
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      343(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 6.67
_diffrn_reflns_number            7027
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.525
_diffrn_reflns_theta_max         26.367
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             1150
_reflns_number_gt                956
_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       'X-AREA (Stoe & Cie, 2006)'
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2006)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2006)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0336P)²+0.4885P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1150
_refine_ls_number_parameters     79
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0282
_refine_ls_wR_factor_ref         0.0671
_refine_ls_wR_factor_gt          0.0643
_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
Cl1 Cl 0.34787(5) 0.2500 0.51876(8) 0.0341(2) Uani 1 2 d S T P . .
Co1 Co 0.13288(2) 0.2500 0.79562(4) 0.02169(14) Uani 1 2 d S T P . .
N1 N 0.12411(17) 0.2500 0.5897(3) 0.0317(6) Uani 1 2 d S T P . .
H1A H 0.1778 0.2755 0.5533 0.047 Uiso 0.5 1 calc R U P . .
H1B H 0.0845 0.3340 0.5628 0.047 Uiso 0.5 1 calc R U P . .
H1C H 0.1062 0.1405 0.5606 0.047 Uiso 0.5 1 calc R U P . .
N2 N 0.22516(12) 0.0583(3) 0.78138(19) 0.0321(4) Uani 1 1 d . . . . .
H2A H 0.2120 -0.0155 0.7106 0.048 Uiso 1 1 calc R U . . .
H2B H 0.2265 -0.0059 0.8600 0.048 Uiso 1 1 calc R U . . .
H2C H 0.2787 0.1094 0.7670 0.048 Uiso 1 1 calc R U . . .
N3 N 0.03970(12) 0.0627(3) 0.8130(2) 0.0337(4) Uani 1 1 d . . . . .
H3A H 0.0281 0.0155 0.7296 0.051 Uiso 1 1 calc R U . . .
H3B H -0.0102 0.1126 0.8475 0.051 Uiso 1 1 calc R U . . .
H3C H 0.0588 -0.0251 0.8698 0.051 Uiso 1 1 calc R U . . .
N4 N 0.14600(16) 0.2500 0.9945(3) 0.0288(6) Uani 1 2 d S T P . .
N5 N 0.41096(17) 0.2500 1.0012(3) 0.0336(6) Uani 1 2 d S T P . .
O1 O 0.22208(15) 0.2500 1.0462(3) 0.0466(6) Uani 1 2 d S T P . .
O2 O 0.07970(16) 0.2500 1.0705(3) 0.0460(6) Uani 1 2 d S T P . .
O3 O 0.41008(13) 0.1035(3) 0.9361(2) 0.0536(5) Uani 1 1 d . . . . .
O4 O 0.4117(2) 0.2500 1.1293(3) 0.0634(8) Uani 1 2 d S T P . .


_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 1.921(3) . ?
Co1 N3 1.9554(19) . ?
Co1 N3 1.9555(19) 8_565 ?
Co1 N2 1.9669(18) . ?
Co1 N2 1.9670(18) 8_565 ?
Co1 N1 1.983(3) . ?
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 O2 1.226(3) . ?
N4 O1 1.234(3) . ?
N5 O4 1.231(4) . ?
N5 O3 1.242(2) 8_565 ?
N5 O3 1.242(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 N3 89.25(8) . . ?
N4 Co1 N3 89.25(8) . 8_565 ?
N3 Co1 N3 89.07(12) . 8_565 ?
N4 Co1 N2 89.92(7) . . ?
N3 Co1 N2 89.90(9) . . ?
N3 Co1 N2 178.69(8) 8_565 . ?
N4 Co1 N2 89.92(7) . 8_565 ?
N3 Co1 N2 178.69(8) . 8_565 ?
N3 Co1 N2 89.90(9) 8_565 8_565 ?
N2 Co1 N2 91.11(11) . 8_565 ?
N4 Co1 N1 177.95(10) . . ?
N3 Co1 N1 92.21(8) . . ?
N3 Co1 N1 92.21(8) 8_565 . ?
N2 Co1 N1 88.64(7) . . ?
N2 Co1 N1 88.64(7) 8_565 . ?
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 . . ?
O2 N4 O1 119.8(3) . . ?
O2 N4 Co1 120.7(2) . . ?
O1 N4 Co1 119.5(2) . . ?
O4 N5 O3 120.23(15) . 8_565 ?
O4 N5 O3 120.23(15) . . ?
O3 N5 O3 119.5(3) 8_565 . ?


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 H1C O3 0.89 2.92 3.364(3) 112.2 6_557
N1 H1C O3 0.89 2.16 3.023(2) 162.0 2_554
N1 H1B O3 0.89 2.32 3.023(2) 135.8 7_665
N1 H1A Cl1 0.89 2.55 3.392(3) 157.1 .
N2 H2C Cl1 0.89 2.79 3.415(2) 128.0 .
N2 H2B Cl1 0.89 2.60 3.388(2) 148.5 2
N2 H2A O1 0.89 2.53 3.289(3) 143.5 2_554
N2 H2C O3 0.89 2.54 3.140(3) 125.5 .
N3 H3C Cl1 0.89 2.59 3.456(2) 166.2 2
N3 H3B Cl1 0.89 2.67 3.551(2) 173.0 3_456
N3 H3A O3 0.89 2.45 3.086(3) 128.4 6_557
N3 H3C O2 0.89 2.70 3.105(2) 109.2 4_547
N3 H3A O4 0.89 2.35 2.980(3) 128.2 2_554

_refine_diff_density_max         0.358
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.075

####################################################################### 
# 
# 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_80C
_database_code_depnum_ccdc_archive 'CCDC 1470430'
_audit_update_record             
;
2016-03-25 deposited with the CCDC.
2016-05-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_name_common            nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_melting_point          ?
_chemical_formula_moiety         'Co H15 N6 O2, N O3, Cl'
_chemical_formula_sum            'Cl Co H15 N7 O5'
_chemical_formula_weight         287.57

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1484 0.1585 '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           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   14.860(2)
_cell_length_b                   7.3294(11)
_cell_length_c                   9.6098(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1046.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    353(2)
_cell_measurement_reflns_used    9592
_cell_measurement_theta_min      1.45
_cell_measurement_theta_max      29.51

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.825
_exptl_crystal_F_000             592
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    1.910
_shelx_estimated_absorpt_T_min   0.598
_shelx_estimated_absorpt_T_max   0.763
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6633
_exptl_absorpt_correction_T_max  0.7850
_exptl_absorpt_process_details   X-RED
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      353(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 6.67
_diffrn_reflns_number            7018
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.524
_diffrn_reflns_theta_max         26.344
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             1150
_reflns_number_gt                963
_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       'X-AREA (Stoe & Cie, 2006)'
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2006)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2006)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0337P)²+0.4816P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1150
_refine_ls_number_parameters     79
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0290
_refine_ls_wR_factor_ref         0.0670
_refine_ls_wR_factor_gt          0.0645
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_restrained_S_all      1.094
_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
Cl1 Cl 0.34785(5) 0.2500 0.51872(9) 0.0354(2) Uani 1 2 d S T P . .
Co1 Co 0.13287(2) 0.2500 0.79558(4) 0.02252(14) Uani 1 2 d S T P . .
N1 N 0.12397(17) 0.2500 0.5896(3) 0.0325(6) Uani 1 2 d S T P . .
H1A H 0.1776 0.2749 0.5532 0.049 Uiso 0.5 1 calc R U P . .
H1B H 0.0845 0.3343 0.5628 0.049 Uiso 0.5 1 calc R U P . .
H1C H 0.1058 0.1408 0.5606 0.049 Uiso 0.5 1 calc R U P . .
N2 N 0.22501(12) 0.0584(3) 0.78141(19) 0.0335(4) Uani 1 1 d . . . . .
H2A H 0.2128 -0.0131 0.7090 0.050 Uiso 1 1 calc R U . . .
H2B H 0.2251 -0.0079 0.8590 0.050 Uiso 1 1 calc R U . . .
H2C H 0.2788 0.1096 0.7698 0.050 Uiso 1 1 calc R U . . .
N3 N 0.03975(12) 0.0631(3) 0.8129(2) 0.0354(5) Uani 1 1 d . . . . .
H3A H 0.0282 0.0158 0.7295 0.053 Uiso 1 1 calc R U . . .
H3B H -0.0101 0.1129 0.8473 0.053 Uiso 1 1 calc R U . . .
H3C H 0.0588 -0.0246 0.8697 0.053 Uiso 1 1 calc R U . . .
N4 N 0.14608(16) 0.2500 0.9945(3) 0.0297(6) Uani 1 2 d S T P . .
N5 N 0.41086(17) 0.2500 1.0014(3) 0.0346(6) Uani 1 2 d S T P . .
O1 O 0.22200(15) 0.2500 1.0463(3) 0.0490(7) Uani 1 2 d S T P . .
O2 O 0.07963(16) 0.2500 1.0705(3) 0.0479(6) Uani 1 2 d S T P . .
O3 O 0.41000(13) 0.1039(3) 0.9364(2) 0.0559(5) Uani 1 1 d . . . . .
O4 O 0.4114(2) 0.2500 1.1295(3) 0.0659(9) Uani 1 2 d S T P . .


_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 1.921(3) . ?
Co1 N3 1.9542(19) . ?
Co1 N3 1.9542(19) 8_565 ?
Co1 N2 1.9658(18) 8_565 ?
Co1 N2 1.9658(18) . ?
Co1 N1 1.983(3) . ?
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 O2 1.228(3) . ?
N4 O1 1.233(3) . ?
N5 O4 1.230(4) . ?
N5 O3 1.239(2) 8_565 ?
N5 O3 1.239(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 N3 89.30(8) . . ?
N4 Co1 N3 89.30(8) . 8_565 ?
N3 Co1 N3 89.02(12) . 8_565 ?
N4 Co1 N2 89.87(7) . 8_565 ?
N3 Co1 N2 178.65(8) . 8_565 ?
N3 Co1 N2 89.91(9) 8_565 8_565 ?
N4 Co1 N2 89.87(7) . . ?
N3 Co1 N2 89.91(9) . . ?
N3 Co1 N2 178.65(8) 8_565 . ?
N2 Co1 N2 91.15(11) 8_565 . ?
N4 Co1 N1 177.95(10) . . ?
N3 Co1 N1 92.16(8) . . ?
N3 Co1 N1 92.16(8) 8_565 . ?
N2 Co1 N1 88.70(7) 8_565 . ?
N2 Co1 N1 88.70(7) . . ?
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 . . ?
O2 N4 O1 119.7(3) . . ?
O2 N4 Co1 120.6(2) . . ?
O1 N4 Co1 119.7(2) . . ?
O4 N5 O3 120.26(15) . 8_565 ?
O4 N5 O3 120.26(15) . . ?
O3 N5 O3 119.5(3) 8_565 . ?


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 H1C O3 0.89 2.92 3.364(3) 112.5 6_557
N1 H1C O3 0.89 2.17 3.025(2) 161.8 2_554
N1 H1B O3 0.89 2.32 3.025(2) 136.1 7_665
N1 H1A Cl1 0.89 2.56 3.396(3) 157.3 .
N2 H2C Cl1 0.89 2.82 3.417(2) 126.1 .
N2 H2B Cl1 0.89 2.58 3.389(2) 150.6 2
N2 H2A O1 0.89 2.53 3.292(3) 144.1 2_554
N2 H2C O3 0.89 2.52 3.145(3) 127.4 .
N3 H3C Cl1 0.89 2.59 3.460(2) 166.2 2
N3 H3B Cl1 0.89 2.67 3.554(2) 173.0 3_456
N3 H3A O3 0.89 2.46 3.090(3) 128.3 6_557
N3 H3C O2 0.89 2.70 3.110(2) 109.3 4_547
N3 H3A O4 0.89 2.35 2.983(3) 128.1 2_554

_refine_diff_density_max         0.295
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.073

####################################################################### 
# 
# 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_90C
_database_code_depnum_ccdc_archive 'CCDC 1470431'
_audit_update_record             
;
2016-03-25 deposited with the CCDC.
2016-05-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_name_common            nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_melting_point          ?
_chemical_formula_moiety         'Co H15 N6 O2, N O3, Cl'
_chemical_formula_sum            'Cl Co H15 N7 O5'
_chemical_formula_weight         287.57

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1484 0.1585 '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           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   14.872(2)
_cell_length_b                   7.3394(11)
_cell_length_c                   9.6071(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1048.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    363(2)
_cell_measurement_reflns_used    9567
_cell_measurement_theta_min      1.45
_cell_measurement_theta_max      29.49

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.821
_exptl_crystal_F_000             592
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    1.906
_shelx_estimated_absorpt_T_min   0.599
_shelx_estimated_absorpt_T_max   0.763
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6648
_exptl_absorpt_correction_T_max  0.7860
_exptl_absorpt_process_details   X-RED
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      363(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 6.67
_diffrn_reflns_number            7031
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.524
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             1152
_reflns_number_gt                958
_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       'X-AREA (Stoe & Cie, 2006)'
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2006)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2006)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0354P)²+0.4323P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1152
_refine_ls_number_parameters     79
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0280
_refine_ls_wR_factor_ref         0.0663
_refine_ls_wR_factor_gt          0.0631
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.001
_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
Cl1 Cl 0.34783(5) 0.2500 0.51864(8) 0.0365(2) Uani 1 2 d S T P . .
Co1 Co 0.13283(2) 0.2500 0.79558(4) 0.02336(14) Uani 1 2 d S T P . .
N1 N 0.12398(17) 0.2500 0.5897(3) 0.0337(6) Uani 1 2 d S T P . .
H1A H 0.1777 0.2741 0.5532 0.051 Uiso 0.5 1 calc R U P . .
H1B H 0.0849 0.3347 0.5627 0.051 Uiso 0.5 1 calc R U P . .
H1C H 0.1054 0.1412 0.5606 0.051 Uiso 0.5 1 calc R U P . .
N2 N 0.22496(12) 0.0585(3) 0.78156(19) 0.0344(4) Uani 1 1 d . . . . .
H2A H 0.2103 -0.0184 0.7136 0.052 Uiso 1 1 calc R U . . .
H2B H 0.2282 -0.0017 0.8618 0.052 Uiso 1 1 calc R U . . .
H2C H 0.2780 0.1091 0.7629 0.052 Uiso 1 1 calc R U . . .
N3 N 0.03979(12) 0.0631(3) 0.8130(2) 0.0362(4) Uani 1 1 d . . . . .
H3A H 0.0284 0.0156 0.7296 0.054 Uiso 1 1 calc R U . . .
H3B H -0.0101 0.1129 0.8471 0.054 Uiso 1 1 calc R U . . .
H3C H 0.0588 -0.0243 0.8701 0.054 Uiso 1 1 calc R U . . .
N4 N 0.14590(16) 0.2500 0.9944(3) 0.0307(6) Uani 1 2 d S T P . .
N5 N 0.41084(17) 0.2500 1.0018(3) 0.0361(6) Uani 1 2 d S T P . .
O1 O 0.22171(15) 0.2500 1.0463(3) 0.0512(7) Uani 1 2 d S T P . .
O2 O 0.07963(16) 0.2500 1.0705(3) 0.0501(6) Uani 1 2 d S T P . .
O3 O 0.40990(13) 0.1042(3) 0.9368(2) 0.0584(5) Uani 1 1 d . . . . .
O4 O 0.4113(2) 0.2500 1.1297(3) 0.0679(9) Uani 1 2 d S T P . .


_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 1.920(3) . ?
Co1 N3 1.9556(18) 8_565 ?
Co1 N3 1.9557(19) . ?
Co1 N2 1.9674(18) 8_565 ?
Co1 N2 1.9674(18) . ?
Co1 N1 1.983(3) . ?
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 O2 1.227(3) . ?
N4 O1 1.233(3) . ?
N5 O4 1.229(4) . ?
N5 O3 1.239(2) 8_565 ?
N5 O3 1.239(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 N3 89.24(8) . 8_565 ?
N4 Co1 N3 89.24(8) . . ?
N3 Co1 N3 89.10(12) 8_565 . ?
N4 Co1 N2 89.86(7) . 8_565 ?
N3 Co1 N2 89.85(9) 8_565 8_565 ?
N3 Co1 N2 178.63(8) . 8_565 ?
N4 Co1 N2 89.86(7) . . ?
N3 Co1 N2 178.63(8) 8_565 . ?
N3 Co1 N2 89.85(9) . . ?
N2 Co1 N2 91.18(11) 8_565 . ?
N4 Co1 N1 177.99(10) . . ?
N3 Co1 N1 92.19(8) 8_565 . ?
N3 Co1 N1 92.19(8) . . ?
N2 Co1 N1 88.73(7) 8_565 . ?
N2 Co1 N1 88.73(7) . . ?
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 . . ?
O2 N4 O1 119.6(3) . . ?
O2 N4 Co1 120.8(2) . . ?
O1 N4 Co1 119.7(2) . . ?
O4 N5 O3 120.27(15) . 8_565 ?
O4 N5 O3 120.27(15) . . ?
O3 N5 O3 119.4(3) 8_565 . ?


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 H1C O3 0.89 2.92 3.369(3) 112.9 6_557
N1 H1C O3 0.89 2.17 3.028(2) 161.7 2_554
N1 H1B O3 0.89 2.32 3.028(2) 136.5 7_665
N1 H1A Cl1 0.89 2.56 3.398(3) 157.7 .
N2 H2C Cl1 0.89 2.77 3.4197(19) 131.2 .
N2 H2B Cl1 0.89 2.62 3.3892(19) 145.1 2
N2 H2A O1 0.89 2.55 3.296(3) 142.1 2_554
N2 H2C O3 0.89 2.58 3.147(3) 122.6 .
N3 H3C Cl1 0.89 2.59 3.461(2) 166.1 2
N3 H3B Cl1 0.89 2.67 3.557(2) 172.7 3_456
N3 H3A O3 0.89 2.47 3.096(3) 128.1 6_557
N3 H3C O2 0.89 2.70 3.112(2) 109.3 4_547
N3 H3A O4 0.89 2.35 2.984(3) 128.3 2_554

_refine_diff_density_max         0.265
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.071

####################################################################### 
# 
# 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_100C
_database_code_depnum_ccdc_archive 'CCDC 1470432'
_audit_update_record             
;
2016-03-25 deposited with the CCDC.
2016-05-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_name_common            nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_melting_point          ?
_chemical_formula_moiety         'Co H15 N6 O2, N O3, Cl'
_chemical_formula_sum            'Cl Co H15 N7 O5'
_chemical_formula_weight         287.57

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1484 0.1585 '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           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   14.877(2)
_cell_length_b                   7.3463(12)
_cell_length_c                   9.6072(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1050.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    373(2)
_cell_measurement_reflns_used    9262
_cell_measurement_theta_min      1.45
_cell_measurement_theta_max      29.51

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.819
_exptl_crystal_F_000             592
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    1.904
_shelx_estimated_absorpt_T_min   0.599
_shelx_estimated_absorpt_T_max   0.763
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6649
_exptl_absorpt_correction_T_max  0.7860
_exptl_absorpt_process_details   X-RED
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      373(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 6.67
_diffrn_reflns_number            7048
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.524
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             1154
_reflns_number_gt                949
_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       'X-AREA (Stoe & Cie, 2006)'
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2006)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2006)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0344P)²+0.5520P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1154
_refine_ls_number_parameters     79
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0288
_refine_ls_wR_factor_ref         0.0679
_refine_ls_wR_factor_gt          0.0643
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.001
_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
Cl1 Cl 0.34777(5) 0.2500 0.51859(9) 0.0379(2) Uani 1 2 d S T P . .
Co1 Co 0.13278(2) 0.2500 0.79558(4) 0.02414(14) Uani 1 2 d S T P . .
N1 N 0.12401(18) 0.2500 0.5896(3) 0.0350(6) Uani 1 2 d S T P . .
H1A H 0.1776 0.2749 0.5532 0.052 Uiso 0.5 1 calc R U P . .
H1B H 0.0846 0.3341 0.5627 0.052 Uiso 0.5 1 calc R U P . .
H1C H 0.1058 0.1410 0.5605 0.052 Uiso 0.5 1 calc R U P . .
N2 N 0.22496(12) 0.0589(3) 0.7817(2) 0.0354(4) Uani 1 1 d . . . . .
H2A H 0.2089 -0.0213 0.7168 0.053 Uiso 1 1 calc R U . . .
H2B H 0.2303 0.0026 0.8633 0.053 Uiso 1 1 calc R U . . .
H2C H 0.2774 0.1088 0.7586 0.053 Uiso 1 1 calc R U . . .
N3 N 0.03983(12) 0.0633(3) 0.8129(2) 0.0374(5) Uani 1 1 d . . . . .
H3A H 0.0284 0.0159 0.7295 0.056 Uiso 1 1 calc R U . . .
H3B H -0.0101 0.1130 0.8471 0.056 Uiso 1 1 calc R U . . .
H3C H 0.0588 -0.0241 0.8699 0.056 Uiso 1 1 calc R U . . .
N4 N 0.14582(17) 0.2500 0.9945(3) 0.0324(6) Uani 1 2 d S T P . .
N5 N 0.41078(18) 0.2500 1.0020(3) 0.0374(7) Uani 1 2 d S T P . .
O1 O 0.22152(16) 0.2500 1.0465(3) 0.0529(7) Uani 1 2 d S T P . .
O2 O 0.07949(17) 0.2500 1.0705(3) 0.0518(7) Uani 1 2 d S T P . .
O3 O 0.40981(14) 0.1044(3) 0.9370(2) 0.0606(5) Uani 1 1 d . . . . .
O4 O 0.4112(2) 0.2500 1.1301(3) 0.0709(9) Uani 1 2 d S T P . .


_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 1.921(3) . ?
Co1 N3 1.9548(19) 8_565 ?
Co1 N3 1.9548(19) . ?
Co1 N2 1.9672(19) . ?
Co1 N2 1.9673(19) 8_565 ?
Co1 N1 1.983(3) . ?
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 O2 1.227(4) . ?
N4 O1 1.232(3) . ?
N5 O4 1.230(4) . ?
N5 O3 1.239(2) 8_565 ?
N5 O3 1.239(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 N3 89.25(8) . 8_565 ?
N4 Co1 N3 89.25(8) . . ?
N3 Co1 N3 89.12(13) 8_565 . ?
N4 Co1 N2 89.83(8) . . ?
N3 Co1 N2 178.66(8) 8_565 . ?
N3 Co1 N2 89.89(9) . . ?
N4 Co1 N2 89.83(8) . 8_565 ?
N3 Co1 N2 89.89(9) 8_565 8_565 ?
N3 Co1 N2 178.66(8) . 8_565 ?
N2 Co1 N2 91.09(12) . 8_565 ?
N4 Co1 N1 177.98(11) . . ?
N3 Co1 N1 92.19(8) 8_565 . ?
N3 Co1 N1 92.19(8) . . ?
N2 Co1 N1 88.75(8) . . ?
N2 Co1 N1 88.75(8) 8_565 . ?
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 . . ?
O2 N4 O1 119.6(3) . . ?
O2 N4 Co1 120.7(2) . . ?
O1 N4 Co1 119.7(2) . . ?
O4 N5 O3 120.30(16) . 8_565 ?
O4 N5 O3 120.30(16) . . ?
O3 N5 O3 119.4(3) 8_565 . ?


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 H1C O3 0.89 2.93 3.371(3) 112.5 6_557
N1 H1C O3 0.89 2.17 3.030(3) 162.0 2_554
N1 H1B O3 0.89 2.33 3.030(3) 136.1 7_665
N1 H1A Cl1 0.89 2.56 3.398(3) 157.3 .
N2 H2C Cl1 0.89 2.74 3.420(2) 134.5 .
N2 H2B Cl1 0.89 2.65 3.391(2) 141.5 2
N2 H2A O1 0.89 2.56 3.300(3) 140.6 2_554
N2 H2C O3 0.89 2.61 3.146(3) 119.5 .
N3 H3C Cl1 0.89 2.59 3.464(2) 166.1 2
N3 H3B Cl1 0.89 2.67 3.559(2) 172.8 3_456
N3 H3A O3 0.89 2.47 3.097(3) 128.1 6_557
N3 H3C O2 0.89 2.71 3.115(3) 109.3 4_547
N3 H3A O4 0.89 2.35 2.985(3) 128.1 2_554

_refine_diff_density_max         0.267
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.072

####################################################################### 
# 
# 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_110C
_database_code_depnum_ccdc_archive 'CCDC 1470433'
_audit_update_record             
;
2016-03-25 deposited with the CCDC.
2016-05-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_name_common            nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_melting_point          ?
_chemical_formula_moiety         'Co H15 N6 O2, N O3, Cl'
_chemical_formula_sum            'Cl Co H15 N7 O5'
_chemical_formula_weight         287.57

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1484 0.1585 '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           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   14.881(2)
_cell_length_b                   7.3506(12)
_cell_length_c                   9.6096(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1051.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    383(2)
_cell_measurement_reflns_used    9175
_cell_measurement_theta_min      1.45
_cell_measurement_theta_max      29.51

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.817
_exptl_crystal_F_000             592
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    1.902
_shelx_estimated_absorpt_T_min   0.599
_shelx_estimated_absorpt_T_max   0.764
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6649
_exptl_absorpt_correction_T_max  0.7860
_exptl_absorpt_process_details   X-RED
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      383(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 6.67
_diffrn_reflns_number            7066
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.523
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             1157
_reflns_number_gt                948
_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       'X-AREA (Stoe & Cie, 2006)'
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2006)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2006)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0368P)²+0.4453P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1157
_refine_ls_number_parameters     79
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0288
_refine_ls_wR_factor_ref         0.0689
_refine_ls_wR_factor_gt          0.0658
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.053
_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
Cl1 Cl 0.34777(5) 0.2500 0.51857(9) 0.0388(2) Uani 1 2 d S T P . .
Co1 Co 0.13277(2) 0.2500 0.79555(4) 0.02477(15) Uani 1 2 d S T P . .
N1 N 0.12406(18) 0.2500 0.5898(3) 0.0361(6) Uani 1 2 d S T P . .
H1A H 0.1775 0.2763 0.5535 0.054 Uiso 0.5 1 calc R U P . .
H1B H 0.0841 0.3330 0.5629 0.054 Uiso 0.5 1 calc R U P . .
H1C H 0.1066 0.1406 0.5606 0.054 Uiso 0.5 1 calc R U P . .
N2 N 0.22482(12) 0.0590(3) 0.7816(2) 0.0362(4) Uani 1 1 d . . . . .
H2A H 0.2126 -0.0126 0.7093 0.054 Uiso 1 1 calc R U . . .
H2B H 0.2250 -0.0068 0.8593 0.054 Uiso 1 1 calc R U . . .
H2C H 0.2785 0.1101 0.7697 0.054 Uiso 1 1 calc R U . . .
N3 N 0.03977(12) 0.0634(3) 0.8128(2) 0.0384(5) Uani 1 1 d . . . . .
H3A H 0.0288 0.0151 0.7295 0.058 Uiso 1 1 calc R U . . .
H3B H -0.0103 0.1133 0.8460 0.058 Uiso 1 1 calc R U . . .
H3C H 0.0585 -0.0233 0.8706 0.058 Uiso 1 1 calc R U . . .
N4 N 0.14574(17) 0.2500 0.9946(3) 0.0333(6) Uani 1 2 d S T P . .
N5 N 0.41064(18) 0.2500 1.0024(3) 0.0389(7) Uani 1 2 d S T P . .
O1 O 0.22142(16) 0.2500 1.0466(3) 0.0548(7) Uani 1 2 d S T P . .
O2 O 0.07958(17) 0.2500 1.0703(3) 0.0529(7) Uani 1 2 d S T P . .
O3 O 0.40990(14) 0.1045(3) 0.9375(2) 0.0625(6) Uani 1 1 d . . . . .
O4 O 0.4109(2) 0.2500 1.1302(3) 0.0728(9) Uani 1 2 d S T P . .


_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 1.922(3) . ?
Co1 N3 1.9556(19) 8_565 ?
Co1 N3 1.9557(19) . ?
Co1 N2 1.9660(19) 8_565 ?
Co1 N2 1.9660(19) . ?
Co1 N1 1.981(3) . ?
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 O2 1.224(4) . ?
N4 O1 1.232(4) . ?
N5 O4 1.228(4) . ?
N5 O3 1.238(2) 8_565 ?
N5 O3 1.238(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 N3 89.25(8) . 8_565 ?
N4 Co1 N3 89.25(8) . . ?
N3 Co1 N3 89.09(12) 8_565 . ?
N4 Co1 N2 89.89(8) . 8_565 ?
N3 Co1 N2 89.89(9) 8_565 8_565 ?
N3 Co1 N2 178.67(8) . 8_565 ?
N4 Co1 N2 89.89(8) . . ?
N3 Co1 N2 178.67(8) 8_565 . ?
N3 Co1 N2 89.89(9) . . ?
N2 Co1 N2 91.12(12) 8_565 . ?
N4 Co1 N1 177.99(11) . . ?
N3 Co1 N1 92.19(8) 8_565 . ?
N3 Co1 N1 92.18(8) . . ?
N2 Co1 N1 88.70(8) 8_565 . ?
N2 Co1 N1 88.70(8) . . ?
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 . . ?
O2 N4 O1 119.6(3) . . ?
O2 N4 Co1 120.7(2) . . ?
O1 N4 Co1 119.7(2) . . ?
O4 N5 O3 120.28(16) . 8_565 ?
O4 N5 O3 120.28(16) . . ?
O3 N5 O3 119.4(3) 8_565 . ?


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 H1C O3 0.89 2.94 3.372(3) 111.7 6_557
N1 H1C O3 0.89 2.17 3.031(3) 162.7 2_554
N1 H1B O3 0.89 2.33 3.031(3) 135.3 7_665
N1 H1A Cl1 0.89 2.56 3.399(3) 156.7 .
N2 H2C Cl1 0.89 2.82 3.421(2) 126.3 .
N2 H2B Cl1 0.89 2.59 3.393(2) 150.4 2
N2 H2A O1 0.89 2.54 3.301(3) 143.8 2_554
N2 H2C O3 0.89 2.53 3.153(3) 127.2 .
N3 H3C Cl1 0.89 2.60 3.467(2) 165.7 2
N3 H3B Cl1 0.89 2.68 3.560(2) 171.9 3_456
N3 H3A O3 0.89 2.48 3.100(3) 127.4 6_557
N3 H3C O2 0.89 2.71 3.118(3) 109.5 4_547
N3 H3A O4 0.89 2.35 2.987(3) 128.8 2_554

_refine_diff_density_max         0.258
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.073

####################################################################### 
# 
# 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_120C
_database_code_depnum_ccdc_archive 'CCDC 1470434'
_audit_update_record             
;
2016-03-25 deposited with the CCDC.
2016-05-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_name_common            nitro-pentaammine-Co(III)-chloride-nitrate
_chemical_melting_point          ?
_chemical_formula_moiety         'Co H15 N6 O2, N O3, Cl'
_chemical_formula_sum            'Cl Co H15 N7 O5'
_chemical_formula_weight         287.57

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1484 0.1585 '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           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   14.896(3)
_cell_length_b                   7.3587(15)
_cell_length_c                   9.6062(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1053.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    393(2)
_cell_measurement_reflns_used    5887
_cell_measurement_theta_min      1.45
_cell_measurement_theta_max      29.49

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.814
_exptl_crystal_F_000             592
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    1.898
_shelx_estimated_absorpt_T_min   0.600
_shelx_estimated_absorpt_T_max   0.764
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6644
_exptl_absorpt_correction_T_max  0.7859
_exptl_absorpt_process_details   X-RED
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      393(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 6.67
_diffrn_reflns_number            7074
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.523
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             1159
_reflns_number_gt                953
_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       'X-AREA (Stoe & Cie, 2006)'
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2006)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2006)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0319P)²+0.5577P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1159
_refine_ls_number_parameters     79
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0287
_refine_ls_wR_factor_ref         0.0670
_refine_ls_wR_factor_gt          0.0637
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.074
_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
Cl1 Cl 0.34773(5) 0.2500 0.51852(9) 0.0399(2) Uani 1 2 d S T P . .
Co1 Co 0.13274(2) 0.2500 0.79557(4) 0.02528(14) Uani 1 2 d S T P . .
N1 N 0.12388(18) 0.2500 0.5894(3) 0.0364(6) Uani 1 2 d S T P . .
H1A H 0.1775 0.2738 0.5529 0.055 Uiso 0.5 1 calc R U P . .
H1B H 0.0849 0.3347 0.5625 0.055 Uiso 0.5 1 calc R U P . .
H1C H 0.1052 0.1415 0.5604 0.055 Uiso 0.5 1 calc R U P . .
N2 N 0.22485(12) 0.0594(3) 0.7816(2) 0.0373(5) Uani 1 1 d . . . . .
H2A H 0.2102 -0.0176 0.7138 0.056 Uiso 1 1 calc R U . . .
H2B H 0.2283 -0.0004 0.8620 0.056 Uiso 1 1 calc R U . . .
H2C H 0.2777 0.1099 0.7627 0.056 Uiso 1 1 calc R U . . .
N3 N 0.03979(12) 0.0635(3) 0.8127(2) 0.0393(5) Uani 1 1 d . . . . .
H3A H 0.0273 0.0184 0.7289 0.059 Uiso 1 1 calc R U . . .
H3B H -0.0096 0.1125 0.8490 0.059 Uiso 1 1 calc R U . . .
H3C H 0.0593 -0.0252 0.8679 0.059 Uiso 1 1 calc R U . . .
N4 N 0.14567(17) 0.2500 0.9946(3) 0.0346(6) Uani 1 2 d S T P . .
N5 N 0.41053(18) 0.2500 1.0025(3) 0.0392(7) Uani 1 2 d S T P . .
O1 O 0.22104(17) 0.2500 1.0466(3) 0.0560(8) Uani 1 2 d S T P . .
O2 O 0.07955(18) 0.2500 1.0704(3) 0.0547(7) Uani 1 2 d S T P . .
O3 O 0.40966(14) 0.1049(3) 0.9376(2) 0.0641(6) Uani 1 1 d . . . . .
O4 O 0.4107(3) 0.2500 1.1304(3) 0.0744(10) Uani 1 2 d S T P . .


_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 1.922(3) . ?
Co1 N3 1.956(2) 8_565 ?
Co1 N3 1.956(2) . ?
Co1 N2 1.9666(19) 8_565 ?
Co1 N2 1.9666(19) . ?
Co1 N1 1.985(3) . ?
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 O2 1.225(4) . ?
N4 O1 1.229(4) . ?
N5 O4 1.228(4) . ?
N5 O3 1.236(2) 8_565 ?
N5 O3 1.236(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 N3 89.28(8) . 8_565 ?
N4 Co1 N3 89.28(8) . . ?
N3 Co1 N3 89.10(13) 8_565 . ?
N4 Co1 N2 89.88(8) . 8_565 ?
N3 Co1 N2 89.95(9) 8_565 8_565 ?
N3 Co1 N2 178.74(8) . 8_565 ?
N4 Co1 N2 89.88(8) . . ?
N3 Co1 N2 178.74(8) 8_565 . ?
N3 Co1 N2 89.95(9) . . ?
N2 Co1 N2 90.99(12) 8_565 . ?
N4 Co1 N1 178.06(11) . . ?
N3 Co1 N1 92.10(8) 8_565 . ?
N3 Co1 N1 92.10(8) . . ?
N2 Co1 N1 88.76(8) 8_565 . ?
N2 Co1 N1 88.76(8) . . ?
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 . . ?
O2 N4 O1 119.6(3) . . ?
O2 N4 Co1 120.7(2) . . ?
O1 N4 Co1 119.7(2) . . ?
O4 N5 O3 120.27(17) . 8_565 ?
O4 N5 O3 120.27(17) . . ?
O3 N5 O3 119.4(3) 8_565 . ?


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 H1C O3 0.89 2.93 3.375(3) 113.1 6_557
N1 H1C O3 0.89 2.17 3.033(3) 161.7 2_554
N1 H1B O3 0.89 2.32 3.033(3) 136.6 7_665
N1 H1A Cl1 0.89 2.56 3.403(3) 157.8 .
N2 H2C Cl1 0.89 2.77 3.421(2) 131.5 .
N2 H2B Cl1 0.89 2.63 3.396(2) 144.8 2
N2 H2A O1 0.89 2.56 3.306(3) 141.9 2_554
N2 H2C O3 0.89 2.59 3.152(3) 122.3 .
N3 H3C Cl1 0.89 2.60 3.470(2) 166.7 2
N3 H3B Cl1 0.89 2.68 3.563(2) 174.6 3_456
N3 H3A O3 0.89 2.46 3.103(3) 129.8 6_557
N3 H3C O2 0.89 2.71 3.121(3) 109.2 4_547
N3 H3A O4 0.89 2.38 2.989(3) 126.1 2_554

_refine_diff_density_max         0.248
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.071

