# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1568217'
_audit_update_record             
;
2017-08-10 deposited with the CCDC.
2018-04-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C4 H11 Cl N), Cl4 Co'
_chemical_formula_sum            'C8 H22 Cl6 Co N2'
_chemical_formula_weight         417.91

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

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

_cell_length_a                   8.979(4)
_cell_length_b                   12.077(5)
_cell_length_c                   16.673(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1808.0(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    5324
_cell_measurement_theta_min      2.0822
_cell_measurement_theta_max      27.4816

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_F_000             852
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.280
_exptl_absorpt_coefficient_mu    1.819
_shelx_estimated_absorpt_T_min   0.545
_shelx_estimated_absorpt_T_max   0.630
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.525
_exptl_absorpt_correction_T_max  0.601
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      223(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku, SCXmini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13385
_diffrn_reflns_av_unetI/netI     0.0642
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.082
_diffrn_reflns_theta_max         27.477
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4151
_reflns_number_gt                3794
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.754
_reflns_Friedel_fraction_max     0.997
_reflns_Friedel_fraction_full    1.000

_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       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2008)'
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0400P)²+1.8172P] 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     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0116(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.37(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4125
_refine_ls_number_parameters     162
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0500
_refine_ls_wR_factor_ref         0.1153
_refine_ls_wR_factor_gt          0.1065
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_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
Co1 Co 0.98869(9) 0.52204(6) 0.10825(4) 0.0313(2) Uani 1 1 d . . . . .
C1 C 0.8380(9) 0.6296(6) 0.3500(5) 0.0503(18) Uani 1 1 d . . . . .
H1A H 0.7537 0.5935 0.3753 0.076 Uiso 1 1 calc R U . . .
H1B H 0.8556 0.5968 0.2978 0.076 Uiso 1 1 calc R U . . .
H1C H 0.8170 0.7079 0.3438 0.076 Uiso 1 1 calc R U . . .
C2 C 1.0005(10) 0.4929(5) 0.4138(5) 0.059(2) Uani 1 1 d . . . . .
H2A H 1.0865 0.4824 0.4481 0.088 Uiso 1 1 calc R U . . .
H2B H 1.0183 0.4579 0.3623 0.088 Uiso 1 1 calc R U . . .
H2C H 0.9136 0.4599 0.4388 0.088 Uiso 1 1 calc R U . . .
C3 C 1.1063(9) 0.6651(7) 0.3600(5) 0.056(2) Uani 1 1 d . . . . .
H3A H 1.0947 0.7449 0.3576 0.083 Uiso 1 1 calc R U . . .
H3B H 1.1136 0.6356 0.3060 0.083 Uiso 1 1 calc R U . . .
H3C H 1.1961 0.6471 0.3896 0.083 Uiso 1 1 calc R U . . .
C4 C 0.9432(8) 0.6718(6) 0.4798(4) 0.0442(16) Uani 1 1 d . . . . .
H4A H 0.8512 0.6419 0.5028 0.053 Uiso 1 1 calc R U . . .
H4B H 0.9280 0.7510 0.4701 0.053 Uiso 1 1 calc R U . . .
C5 C 0.5736(11) 0.2404(8) 0.4326(4) 0.062(2) Uani 1 1 d . . . . .
H5A H 0.6769 0.2181 0.4380 0.094 Uiso 1 1 calc R U . . .
H5B H 0.5100 0.1855 0.4577 0.094 Uiso 1 1 calc R U . . .
H5C H 0.5590 0.3115 0.4584 0.094 Uiso 1 1 calc R U . . .
C6 C 0.6268(9) 0.3380(6) 0.3084(5) 0.0543(19) Uani 1 1 d . . . . .
H6A H 0.7313 0.3181 0.3119 0.081 Uiso 1 1 calc R U . . .
H6B H 0.6103 0.4073 0.3364 0.081 Uiso 1 1 calc R U . . .
H6C H 0.5987 0.3462 0.2526 0.081 Uiso 1 1 calc R U . . .
C7 C 0.3728(8) 0.2767(7) 0.3372(6) 0.059(2) Uani 1 1 d . . . . .
H7A H 0.3502 0.3431 0.3676 0.088 Uiso 1 1 calc R U . . .
H7B H 0.3136 0.2156 0.3573 0.088 Uiso 1 1 calc R U . . .
H7C H 0.3498 0.2890 0.2811 0.088 Uiso 1 1 calc R U . . .
C8 C 0.5703(8) 0.1383(6) 0.3115(4) 0.0417(15) Uani 1 1 d . . . . .
H8A H 0.5113 0.0821 0.3395 0.050 Uiso 1 1 calc R U . . .
H8B H 0.6757 0.1219 0.3209 0.050 Uiso 1 1 calc R U . . .
Cl1 Cl 1.0400(3) 0.47183(17) -0.02037(10) 0.0645(6) Uani 1 1 d . . . . .
Cl2 Cl 1.1396(2) 0.43112(14) 0.19531(11) 0.0487(5) Uani 1 1 d . . . . .
Cl3 Cl 0.7468(2) 0.47795(17) 0.13194(14) 0.0586(5) Uani 1 1 d . . . . .
Cl4 Cl 1.0197(2) 0.70701(12) 0.12968(10) 0.0444(4) Uani 1 1 d . . . . .
Cl5 Cl 1.0893(2) 0.6544(2) 0.54897(12) 0.0635(6) Uani 1 1 d . . . . .
Cl6 Cl 0.5339(2) 0.1297(2) 0.20846(11) 0.0635(6) Uani 1 1 d . . . . .
N1 N 0.9740(6) 0.6151(4) 0.4015(3) 0.0344(11) Uani 1 1 d . . . . .
N2 N 0.5351(6) 0.2496(4) 0.3459(3) 0.0371(12) Uani 1 1 d . . . . .


_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 Cl2 2.2691(19) . ?
Co1 Cl3 2.271(2) . ?
Co1 Cl1 2.2757(19) . ?
Co1 Cl4 2.2793(18) . ?
C1 N1 1.502(9) . ?
C2 N1 1.508(8) . ?
C3 N1 1.502(9) . ?
C4 N1 1.500(8) . ?
C4 Cl5 1.759(7) . ?
C5 N2 1.490(8) . ?
C6 N2 1.486(9) . ?
C7 N2 1.500(9) . ?
C8 N2 1.495(8) . ?
C8 Cl6 1.751(7) . ?

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
Cl2 Co1 Cl3 110.27(9) . . ?
Cl2 Co1 Cl1 110.67(8) . . ?
Cl3 Co1 Cl1 107.15(9) . . ?
Cl2 Co1 Cl4 107.52(7) . . ?
Cl3 Co1 Cl4 108.63(8) . . ?
Cl1 Co1 Cl4 112.59(8) . . ?
N1 C4 Cl5 112.3(4) . . ?
N2 C8 Cl6 113.0(5) . . ?
C4 N1 C3 111.3(5) . . ?
C4 N1 C1 107.1(5) . . ?
C3 N1 C1 109.4(5) . . ?
C4 N1 C2 111.0(5) . . ?
C3 N1 C2 109.3(6) . . ?
C1 N1 C2 108.7(6) . . ?
C6 N2 C5 109.4(6) . . ?
C6 N2 C8 111.5(5) . . ?
C5 N2 C8 104.8(5) . . ?
C6 N2 C7 109.9(6) . . ?
C5 N2 C7 109.6(6) . . ?
C8 N2 C7 111.4(5) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C8 H8B Cl2 0.98 2.85 3.613(7) 135.3 3_745
C8 H8A Cl3 0.98 2.68 3.571(7) 151.4 3_645
C7 H7C Cl2 0.97 2.92 3.669(9) 134.4 1_455
C7 H7B Cl3 0.97 2.93 3.800(9) 150.4 3_645
C6 H6C Cl3 0.97 2.89 3.561(8) 127.3 .
C6 H6A Cl4 0.97 2.78 3.693(8) 156.5 3_745
C5 H5C Cl4 0.97 2.95 3.451(7) 113.3 2_665
C5 H5C Cl1 0.97 2.79 3.706(9) 158.6 2_665
C5 H5A Cl4 0.97 2.95 3.817(10) 149.2 3_745
C4 H4B Cl1 0.98 2.81 3.689(8) 149.7 3_755
C4 H4A Cl3 0.98 2.74 3.552(8) 140.6 2_665
C3 H3C Cl6 0.97 2.93 3.453(8) 114.8 3_755
C1 H1C Cl2 0.97 2.80 3.724(8) 159.5 3_755
C1 H1A Cl6 0.97 2.97 3.479(8) 114.1 3_655
C8 H8B Cl2 0.98 2.85 3.613(7) 135.3 3_745
C8 H8A Cl3 0.98 2.68 3.571(7) 151.4 3_645
C7 H7C Cl2 0.97 2.92 3.669(9) 134.4 1_455
C7 H7B Cl3 0.97 2.93 3.800(9) 150.4 3_645
C6 H6C Cl3 0.97 2.89 3.561(8) 127.3 .
C6 H6A Cl4 0.97 2.78 3.693(8) 156.5 3_745
C5 H5C Cl4 0.97 2.95 3.451(7) 113.3 2_665
C5 H5C Cl1 0.97 2.79 3.706(9) 158.6 2_665
C5 H5A Cl4 0.97 2.95 3.817(10) 149.2 3_745
C4 H4B Cl1 0.98 2.81 3.689(8) 149.7 3_755
C4 H4A Cl3 0.98 2.74 3.552(8) 140.6 2_665
C3 H3C Cl6 0.97 2.93 3.453(8) 114.8 3_755
C1 H1C Cl2 0.97 2.80 3.724(8) 159.5 3_755
C1 H1A Cl6 0.97 2.97 3.479(8) 114.1 3_655

_refine_diff_density_max         0.397
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.089

####################################################################### 
# 
# 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_Cl-293K
_database_code_depnum_ccdc_archive 'CCDC 1568218'
_audit_update_record             
;
2018-04-01 deposited with the CCDC.
2018-04-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Cl4 Co, 2(C4 H11 Cl N)'
_chemical_formula_sum            'C8 H22 Cl6 Co N2'
_chemical_formula_weight         417.91

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   9.199(7)
_cell_length_b                   16.828(14)
_cell_length_c                   12.100(10)
_cell_angle_alpha                90
_cell_angle_beta                 93.47(2)
_cell_angle_gamma                90
_cell_volume                     1870(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4954
_cell_measurement_theta_min      1.6861
_cell_measurement_theta_max      27.5943

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_F_000             852
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_exptl_absorpt_coefficient_mu    1.759
_shelx_estimated_absorpt_T_min   0.559
_shelx_estimated_absorpt_T_max   0.703
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.559
_exptl_absorpt_correction_T_max  0.703
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_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  'Rigaku, SCXmini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11514
_diffrn_reflns_av_unetI/netI     0.0943
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.076
_diffrn_reflns_theta_max         25.248
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             3382
_reflns_number_gt                2692
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2008)'
_refine_special_details          
;
The twinning problem was solved through the correct form: firstly, TwinRotMat (through PLATON) finds this twin law: 
2-axis ( 0 0 1 ) [ 0 0 1 ], Angle () [] = 3.47 Deg, Freq = 33 
************* 
(-1.000 0.000 0.000) (h1) (h2) Nr Overlap = 538 
(0.000 -1.000 0.000) * (k1) = (k2) BASF = 0.25 
(0.159 0.000 1.000) (l1) (l2) DEL-R =-0.019
Then, refining against the generated HKLF 5 format hkl file yields indeed a refined BASF of 0.25 with a final R1 of 9.94% and wR1 of 19.88%. The high R1 value of the crystal structure may be due to the partial disordered of the structure.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0050P)²+20.4492P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0083(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         11514
_refine_ls_number_parameters     194
_refine_ls_number_restraints     94
_refine_ls_R_factor_all          0.1375
_refine_ls_R_factor_gt           0.0994
_refine_ls_wR_factor_ref         0.2168
_refine_ls_wR_factor_gt          0.1988
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.062
_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
Co1 Co 0.70045(17) 0.61376(9) 0.27716(12) 0.0478(5) Uani 1 1 d . U . . .
Cl1 Cl 0.484(4) 0.6760(19) 0.216(4) 0.086(6) Uani 0.5 1 d . U P . .
Cl2 Cl 0.686(3) 0.4872(18) 0.217(4) 0.084(6) Uani 0.5 1 d . U P . .
Cl3 Cl 0.722(4) 0.6096(13) 0.466(2) 0.086(6) Uani 0.5 1 d . U P . .
Cl4 Cl 0.887(3) 0.6790(19) 0.209(3) 0.077(6) Uani 0.5 1 d . U P . .
Cl5 Cl 0.7762(5) 0.2997(2) 0.0913(5) 0.1170(18) Uani 1 1 d . . . . .
Cl6 Cl 0.1326(6) 0.5406(3) 0.1362(4) 0.142(2) Uani 1 1 d . . . . .
Cl1' Cl 0.475(4) 0.6507(19) 0.223(4) 0.092(7) Uani 0.5 1 d . U P . .
Cl2' Cl 0.741(3) 0.4865(18) 0.214(4) 0.089(6) Uani 0.5 1 d . U P . .
Cl3' Cl 0.743(3) 0.6323(11) 0.4650(19) 0.060(3) Uani 0.5 1 d . U P . .
Cl4' Cl 0.866(4) 0.6953(18) 0.199(3) 0.069(5) Uani 0.5 1 d . U P . .
C1 C 0.6355(17) 0.1562(10) -0.0414(14) 0.103(5) Uani 1 1 d . U . . .
H1A H 0.6101 0.1959 -0.0848 0.154 Uiso 1 1 d . U . . .
H1B H 0.5769 0.1499 0.0235 0.154 Uiso 1 1 d . U . . .
H1C H 0.6194 0.1029 -0.0816 0.154 Uiso 1 1 d . U . . .
C2 C 0.8301(19) 0.0738(9) 0.0432(16) 0.136(6) Uani 1 1 d . U . . .
H2A H 0.7468 0.0506 0.0748 0.204 Uiso 1 1 calc R U . . .
H2B H 0.9079 0.0789 0.0993 0.204 Uiso 1 1 calc R U . . .
H2C H 0.8609 0.0403 -0.0152 0.204 Uiso 1 1 calc R U . . .
C3 C 0.8835(18) 0.1804(11) -0.0880(14) 0.132(6) Uani 1 1 d . U . . .
H3A H 0.8885 0.1389 -0.1422 0.198 Uiso 1 1 calc R U . . .
H3B H 0.9792 0.1908 -0.0553 0.198 Uiso 1 1 calc R U . . .
H3C H 0.8452 0.2278 -0.1231 0.198 Uiso 1 1 calc R U . . .
C4 C 0.8148(17) 0.1975(9) 0.1021(12) 0.096(4) Uani 1 1 d . U . . .
H4A H 0.9157 0.1905 0.1286 0.115 Uiso 1 1 calc R U . . .
H4B H 0.7540 0.1739 0.1560 0.115 Uiso 1 1 calc R U . . .
C5 C 0.3967(19) 0.3605(10) 0.0810(14) 0.106(6) Uani 1 1 d . . . . .
H5A H 0.4958 0.3742 0.1123 0.160 Uiso 1 1 d . U . . .
H5B H 0.4002 0.3625 0.0018 0.160 Uiso 1 1 d . U . . .
H5C H 0.3943 0.2997 0.0971 0.160 Uiso 1 1 d . U . . .
C6 C 0.1351(19) 0.3656(10) 0.1003(14) 0.113(6) Uani 1 1 d . . . . .
H6A H 0.1270 0.3148 0.1316 0.169 Uiso 1 1 d . U . . .
H6B H 0.1322 0.3559 0.0157 0.169 Uiso 1 1 d . U . . .
H6C H 0.0577 0.3991 0.1121 0.169 Uiso 1 1 d . U . . .
C7 C 0.2997(17) 0.4011(9) 0.2530(10) 0.091(5) Uani 1 1 d . . . . .
H7A H 0.3604 0.3482 0.2707 0.136 Uiso 1 1 d . U . . .
H7B H 0.2138 0.3928 0.2876 0.136 Uiso 1 1 d . U . . .
H7C H 0.3587 0.4411 0.2808 0.136 Uiso 1 1 d . U . . .
C8 C 0.2796(15) 0.4846(8) 0.0900(11) 0.078(4) Uani 1 1 d . . . . .
H8A H 0.2753 0.4852 0.0097 0.093 Uiso 1 1 calc R U . . .
H8B H 0.3703 0.5095 0.1162 0.093 Uiso 1 1 calc R U . . .
N1 N 0.7900(12) 0.1560(6) -0.0037(9) 0.068(3) Uani 1 1 d . U . . .
N2 N 0.2789(11) 0.4011(5) 0.1287(7) 0.051(2) Uani 1 1 d . . . . .


_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 Cl1' 2.23(3) . ?
Co1 Cl4 2.24(3) . ?
Co1 Cl2 2.25(3) . ?
Co1 Cl3 2.28(3) . ?
Co1 Cl4' 2.29(3) . ?
Co1 Cl3' 2.30(2) . ?
Co1 Cl2' 2.31(3) . ?
Co1 Cl1 2.33(3) . ?
Cl2 Cl2' 0.51(5) . ?
Cl5 C4 1.760(15) . ?
Cl6 C8 1.767(13) . ?
C1 N1 1.466(16) . ?
C1 H1A 0.8726 . ?
C1 H1B 0.9848 . ?
C1 H1C 1.0270 . ?
C2 N1 1.532(17) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 N1 1.434(16) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 N1 1.463(16) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N2 1.431(16) . ?
C5 H5A 0.9931 . ?
C5 H5B 0.9614 . ?
C5 H5C 1.0425 . ?
C6 N2 1.473(17) . ?
C6 H6A 0.9405 . ?
C6 H6B 1.0357 . ?
C6 H6C 0.9260 . ?
C7 N2 1.503(14) . ?
C7 H7A 1.0650 . ?
C7 H7B 0.9269 . ?
C7 H7C 0.9168 . ?
C8 N2 1.482(14) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?

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
Cl1' Co1 Cl4 118.5(14) . . ?
Cl1' Co1 Cl2 97.6(14) . . ?
Cl4 Co1 Cl2 112.3(11) . . ?
Cl1' Co1 Cl3 109.0(17) . . ?
Cl4 Co1 Cl3 111.2(11) . . ?
Cl2 Co1 Cl3 107.0(12) . . ?
Cl1' Co1 Cl4' 110.0(11) . . ?
Cl4 Co1 Cl4' 8.8(16) . . ?
Cl2 Co1 Cl4' 117.5(12) . . ?
Cl3 Co1 Cl4' 114.2(11) . . ?
Cl1' Co1 Cl3' 110.7(16) . . ?
Cl4 Co1 Cl3' 101.9(12) . . ?
Cl2 Co1 Cl3' 116.7(12) . . ?
Cl3 Co1 Cl3' 10.8(9) . . ?
Cl4' Co1 Cl3' 104.2(10) . . ?
Cl1' Co1 Cl2' 109.2(13) . . ?
Cl4 Co1 Cl2' 101.0(12) . . ?
Cl2 Co1 Cl2' 12.9(12) . . ?
Cl3 Co1 Cl2' 107.2(12) . . ?
Cl4' Co1 Cl2' 107.1(11) . . ?
Cl3' Co1 Cl2' 115.4(12) . . ?
Cl1' Co1 Cl1 10.9(17) . . ?
Cl4 Co1 Cl1 108.8(11) . . ?
Cl2 Co1 Cl1 106.9(12) . . ?
Cl3 Co1 Cl1 110.5(16) . . ?
Cl4' Co1 Cl1 100.2(13) . . ?
Cl3' Co1 Cl1 110.1(15) . . ?
Cl2' Co1 Cl1 117.7(15) . . ?
Cl2' Cl2 Co1 90(7) . . ?
Cl2 Cl2' Co1 77(7) . . ?
N1 C1 H1A 114.1 . . ?
N1 C1 H1B 108.6 . . ?
H1A C1 H1B 115.0 . . ?
N1 C1 H1C 104.7 . . ?
H1A C1 H1C 111.0 . . ?
H1B C1 H1C 102.4 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C4 Cl5 112.4(11) . . ?
N1 C4 H4A 109.1 . . ?
Cl5 C4 H4A 109.1 . . ?
N1 C4 H4B 109.1 . . ?
Cl5 C4 H4B 109.1 . . ?
H4A C4 H4B 107.8 . . ?
N2 C5 H5A 115.8 . . ?
N2 C5 H5B 117.3 . . ?
H5A C5 H5B 106.6 . . ?
N2 C5 H5C 111.6 . . ?
H5A C5 H5C 100.7 . . ?
H5B C5 H5C 102.9 . . ?
N2 C6 H6A 111.5 . . ?
N2 C6 H6B 105.3 . . ?
H6A C6 H6B 104.9 . . ?
N2 C6 H6C 113.9 . . ?
H6A C6 H6C 114.3 . . ?
H6B C6 H6C 106.0 . . ?
N2 C7 H7A 103.6 . . ?
N2 C7 H7B 113.1 . . ?
H7A C7 H7B 103.6 . . ?
N2 C7 H7C 113.8 . . ?
H7A C7 H7C 104.3 . . ?
H7B C7 H7C 116.5 . . ?
N2 C8 Cl6 112.8(9) . . ?
N2 C8 H8A 109.0 . . ?
Cl6 C8 H8A 109.0 . . ?
N2 C8 H8B 109.0 . . ?
Cl6 C8 H8B 109.0 . . ?
H8A C8 H8B 107.8 . . ?
C3 N1 C4 114.7(12) . . ?
C3 N1 C1 112.9(13) . . ?
C4 N1 C1 111.6(12) . . ?
C3 N1 C2 112.4(13) . . ?
C4 N1 C2 94.9(11) . . ?
C1 N1 C2 109.0(12) . . ?
C5 N2 C6 113.8(12) . . ?
C5 N2 C8 107.9(11) . . ?
C6 N2 C8 109.4(11) . . ?
C5 N2 C7 110.5(11) . . ?
C6 N2 C7 106.9(11) . . ?
C8 N2 C7 108.3(10) . . ?

_refine_diff_density_max         1.132
_refine_diff_density_min         -1.095
_refine_diff_density_rms         0.145

####################################################################### 
# 
# 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_Cl-353K
_database_code_depnum_ccdc_archive 'CCDC 1568219'
_audit_update_record             
;
2018-04-01 deposited with the CCDC.
2018-04-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C4 H11 Cl N), Cl4 Co'
_chemical_formula_sum            'C8 H22 Cl6 Co N2'
_chemical_formula_weight         417.91

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
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'

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

_cell_length_a                   12.156(13)
_cell_length_b                   9.164(10)
_cell_length_c                   16.939(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1887(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    353(2)
_cell_measurement_reflns_used    4999
_cell_measurement_theta_min      1.6752
_cell_measurement_theta_max      27.5126

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            BLUE
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_F_000             852
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_exptl_absorpt_coefficient_mu    1.743
_shelx_estimated_absorpt_T_min   0.562
_shelx_estimated_absorpt_T_max   0.706
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.562
_exptl_absorpt_correction_T_max  0.706
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_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  'Rigaku, SCXmini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11549
_diffrn_reflns_av_unetI/netI     0.0729
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.062
_diffrn_reflns_theta_max         25.494
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             1876
_reflns_number_gt                1787
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2008)'
_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)+(0.0100P)²+18.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11549
_refine_ls_number_parameters     128
_refine_ls_number_restraints     95
_refine_ls_R_factor_all          0.2006
_refine_ls_R_factor_gt           0.1375
_refine_ls_wR_factor_ref         0.2583
_refine_ls_wR_factor_gt          0.2217
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.067
_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
Co1 Co 0.22223(18) 0.7500 0.39325(15) 0.0974(9) Uani 1 2 d S T P . .
C1 C 0.2450(14) 0.2500 0.5981(13) 0.161(8) Uani 1 2 d S TU P B .
H1A H 0.2190 0.3338 0.5696 0.241 Uiso 0.5 1 d R U P . .
H1B H 0.2189 0.1628 0.5728 0.241 Uiso 0.5 1 d R U P . .
H1C H 0.2182 0.2500 0.6513 0.241 Uiso 1 2 d R U P . .
C3 C 0.425(2) 0.2500 0.5246(19) 0.200(8) Uani 1 2 d S TU P B .
H3A H 0.4203 0.3497 0.5075 0.240 Uiso 0.5 1 d R U P . .
H3B H 0.5025 0.2307 0.5311 0.240 Uiso 0.5 1 d R U P . .
C4 C 0.949(3) 0.7500 0.5761(17) 0.253(13) Uani 1 2 d S TU P C .
H4A H 0.9033 0.6651 0.5718 0.380 Uiso 0.5 1 d R U P . .
H4B H 0.9049 0.8362 0.5712 0.380 Uiso 0.5 1 d R U P . .
H4C H 1.0035 0.7500 0.5349 0.380 Uiso 1 2 d R U P . .
C6 C 0.902(2) 0.7500 0.6976(16) 0.198(8) Uani 1 2 d S TU P C .
H6A H 0.8608 0.8349 0.6824 0.238 Uiso 0.5 1 d R U P . .
H6B H 0.8608 0.6651 0.6824 0.238 Uiso 0.5 1 d R U P . .
Cl1 Cl 0.2782(7) 0.794(4) 0.5137(5) 0.228(14) Uani 0.5 1 d . . P A .
Cl3 Cl 0.0370(4) 0.7500 0.3799(4) 0.145(2) Uani 1 2 d S T P A .
Cl4 Cl 0.3813(13) 0.1635(14) 0.4529(8) 0.261(7) Uani 0.5 1 d . U P . .
Cl5 Cl 0.9016(10) 0.7500 0.7944(6) 0.280(5) Uani 1 2 d S TU P . .
N1 N 0.3733(13) 0.2500 0.6058(12) 0.142(5) Uani 1 2 d DS TU P . .
N2 N 0.9984(16) 0.7500 0.6574(12) 0.145(6) Uani 1 2 d S TU P . .
Cl2 Cl 0.2917(15) 0.9763(16) 0.3657(13) 0.252(10) Uani 0.5 1 d . . P A 1
C2 C 0.404(5) 0.134(5) 0.670(3) 0.186(15) Uani 0.5 1 d . U P B 1
H2A H 0.4834 0.1316 0.6714 0.279 Uiso 0.5 1 d R U P B 1
H2B H 0.3767 0.1381 0.7232 0.279 Uiso 0.5 1 d R U P B 1
H2C H 0.3774 0.0475 0.6447 0.279 Uiso 0.5 1 d R U P B 1
C5 C 1.088(3) 0.878(4) 0.698(2) 0.149(11) Uani 0.5 1 d . U P C 1
H5A H 1.1088 0.8466 0.7496 0.223 Uiso 0.5 1 d R U P C 1
H5B H 1.1517 0.8845 0.6647 0.223 Uiso 0.5 1 d R U P C 1
H5C H 1.0531 0.9721 0.7010 0.223 Uiso 0.5 1 d R U P C 1
Cl2' Cl 0.2899(10) 0.9178(14) 0.3132(6) 0.145(5) Uani 0.5 1 d . . P A 2
C2' C 0.407(4) 0.081(4) 0.6268(19) 0.175(14) Uani 0.5 1 d D U P B 2
H2'A H 0.4349 0.0023 0.6588 0.263 Uiso 0.5 1 d R U P B 2
H2'B H 0.3285 0.0770 0.6257 0.263 Uiso 0.5 1 d R U P B 2
H2'C H 0.4355 0.0710 0.5741 0.263 Uiso 0.5 1 d R U P B 2
C5' C 1.050(4) 0.888(4) 0.651(2) 0.157(12) Uani 0.5 1 d . U P C 2
H5'A H 1.0113 0.9317 0.6077 0.235 Uiso 0.5 1 d R U P C 2
H5'B H 1.0357 0.9424 0.6984 0.235 Uiso 0.5 1 d R U P C 2
H5'C H 1.1274 0.8878 0.6403 0.235 Uiso 0.5 1 d R U P C 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 Cl1 2.190(10) . ?
Co1 Cl1 2.190(10) 7_575 ?
Co1 Cl2' 2.210(10) . ?
Co1 Cl2' 2.210(10) 7_575 ?
Co1 Cl3 2.263(6) . ?
Co1 Cl2 2.287(16) . ?
Co1 Cl2 2.287(16) 7_575 ?
C1 N1 1.56(2) . ?
C3 N1 1.51(3) . ?
C3 Cl4 1.55(2) 7_565 ?
C3 Cl4 1.55(2) . ?
C4 N2 1.50(3) . ?
C6 N2 1.36(3) . ?
C6 Cl5 1.64(3) . ?
Cl1 Cl1 0.81(6) 7_575 ?
Cl4 Cl4 1.58(3) 7_565 ?
N1 C2 1.57(4) . ?
N1 C2 1.57(4) 7_565 ?
N1 C2' 1.65(3) . ?
N1 C2' 1.65(3) 7_565 ?
N2 C5' 1.41(4) . ?
N2 C5' 1.41(4) 7_575 ?
N2 C5 1.74(4) 7_575 ?
N2 C5 1.74(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Co1 Cl1 21.4(17) . 7_575 ?
Cl1 Co1 Cl2' 109.1(8) . . ?
Cl1 Co1 Cl2' 125.9(7) 7_575 . ?
Cl1 Co1 Cl2' 125.9(7) . 7_575 ?
Cl1 Co1 Cl2' 109.1(7) 7_575 7_575 ?
Cl2' Co1 Cl2' 88.2(7) . 7_575 ?
Cl1 Co1 Cl3 113.7(3) . . ?
Cl1 Co1 Cl3 113.7(3) 7_575 . ?
Cl2' Co1 Cl3 108.0(4) . . ?
Cl2' Co1 Cl3 108.0(4) 7_575 . ?
Cl1 Co1 Cl2 84.6(9) . . ?
Cl1 Co1 Cl2 104.1(9) 7_575 . ?
Cl3 Co1 Cl2 110.3(5) . . ?
Cl1 Co1 Cl2 104.1(9) . 7_575 ?
Cl1 Co1 Cl2 84.6(9) 7_575 7_575 ?
Cl3 Co1 Cl2 110.3(5) . 7_575 ?
Cl2 Co1 Cl2 130.1(10) . 7_575 ?
N1 C3 Cl4 124.6(19) . 7_565 ?
N1 C3 Cl4 124.6(19) . . ?
Cl4 C3 Cl4 61.6(16) 7_565 . ?
N2 C6 Cl5 120(2) . . ?
Cl1 Cl1 Co1 79.3(8) 7_575 . ?
C3 Cl4 Cl4 59.2(8) . 7_565 ?
C3 N1 C1 110.0(19) . . ?
C3 N1 C2 122(2) . . ?
C1 N1 C2 107(2) . . ?
C3 N1 C2 122(2) . 7_565 ?
C1 N1 C2 107(2) . 7_565 ?
C2 N1 C2 85(3) . 7_565 ?
C3 N1 C2' 95.2(15) . . ?
C1 N1 C2' 105.6(19) . . ?
C3 N1 C2' 95.2(16) . 7_565 ?
C1 N1 C2' 105.6(19) . 7_565 ?
C2' N1 C2' 141(4) . 7_565 ?
C6 N2 C5' 115(2) . . ?
C6 N2 C5' 115(2) . 7_575 ?
C5' N2 C5' 127(4) . 7_575 ?
C6 N2 C4 97(2) . . ?
C5' N2 C4 96.1(19) . . ?
C5' N2 C4 96.1(19) 7_575 . ?
C6 N2 C5 110(2) . 7_575 ?
C4 N2 C5 127.5(16) . 7_575 ?
C6 N2 C5 110(2) . . ?
C4 N2 C5 127.5(16) . . ?
C5 N2 C5 85(3) 7_575 . ?

_refine_diff_density_max         0.587
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.107

# start Validation Reply Form

_vrf_PLAT242_Cl-353K             
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Co1 Check 
RESPONSE: The chlorine atoms of the anion were extremely disordered.
;

# end Validation Reply Form

####################################################################### 
# 
# 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_Br-293K
_database_code_depnum_ccdc_archive 'CCDC 1568224'
_audit_update_record             
;
2017-08-10 deposited with the CCDC.
2018-04-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C4 H11 Br N), Br4 Co'
_chemical_formula_sum            'C8 H22 Br6 Co N2'
_chemical_formula_weight         684.61

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   9.4935(8)
_cell_length_b                   17.3888(13)
_cell_length_c                   12.4983(8)
_cell_angle_alpha                90
_cell_angle_beta                 93.438(7)
_cell_angle_gamma                90
_cell_volume                     2059.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5070
_cell_measurement_theta_min      1.6323
_cell_measurement_theta_max      27.4623

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            BLUE
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.208
_exptl_crystal_F_000             1284
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    12.460
_shelx_estimated_absorpt_T_min   0.021
_shelx_estimated_absorpt_T_max   0.083
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.021
_exptl_absorpt_correction_T_max  0.083
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_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  'Rigaku, SCXmini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12747
_diffrn_reflns_av_unetI/netI     0.1045
_diffrn_reflns_av_R_equivalents  0.1107
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.149
_diffrn_reflns_theta_max         25.250
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.985
_reflns_number_total             3733
_reflns_number_gt                2421
_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       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2008)'
_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)+(0.1312P)²+44.2641P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0086(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3677
_refine_ls_number_parameters     161
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.1615
_refine_ls_R_factor_gt           0.1135
_refine_ls_wR_factor_ref         0.3115
_refine_ls_wR_factor_gt          0.2783
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.005
_refine_ls_shift/su_max          0.002
_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
Co1 Co 0.3013(3) 0.11499(13) 0.22561(18) 0.0468(7) Uani 1 1 d . . . . .
Br1 Br 0.1187(2) 0.18810(14) 0.30400(19) 0.0737(8) Uani 1 1 d . . . . .
Br2 Br 0.2900(4) -0.01590(13) 0.2862(2) 0.1029(11) Uani 1 1 d . . . . .
Br3 Br 0.5274(2) 0.1664(2) 0.2863(2) 0.0981(11) Uani 1 1 d . . . . .
Br4 Br 0.2637(3) 0.12627(16) 0.03365(16) 0.0797(8) Uani 1 1 d . . . . .
Br5 Br 0.1263(4) -0.0408(2) 0.6381(3) 0.1191(12) Uani 1 1 d . . . . .
Br6 Br 0.2189(3) 0.80037(14) 0.4018(3) 0.0950(10) Uani 1 1 d . U . . .
C1 C 0.277(3) 0.0183(14) 0.589(2) 0.085(7) Uani 1 1 d . . . . .
H1A H 0.3654 -0.0071 0.6109 0.101 Uiso 1 1 calc R U . . .
H1B H 0.2693 0.0196 0.5116 0.101 Uiso 1 1 calc R U . . .
C2 C 0.312(3) 0.1013(16) 0.7484(16) 0.092(8) Uani 1 1 d . . . . .
H2A H 0.4047 0.0803 0.7650 0.137 Uiso 1 1 calc R U . . .
H2B H 0.2433 0.0704 0.7814 0.137 Uiso 1 1 calc R U . . .
H2C H 0.3086 0.1529 0.7752 0.137 Uiso 1 1 calc R U . . .
C3 C 0.140(3) 0.1375(18) 0.601(3) 0.116(10) Uani 1 1 d . . . . .
H3A H 0.0674 0.1084 0.6325 0.174 Uiso 1 1 calc R U . . .
H3B H 0.1245 0.1371 0.5244 0.174 Uiso 1 1 calc R U . . .
H3C H 0.1387 0.1895 0.6266 0.174 Uiso 1 1 calc R U . . .
C4 C 0.399(3) 0.1406(19) 0.582(3) 0.114(10) Uani 1 1 d . U . . .
H4A H 0.3958 0.1946 0.5977 0.172 Uiso 1 1 calc R U . . .
H4B H 0.3889 0.1333 0.5055 0.172 Uiso 1 1 calc R U . . .
H4C H 0.4870 0.1195 0.6091 0.172 Uiso 1 1 calc R U . . .
C5 C 0.180(3) 0.6964(12) 0.397(2) 0.078(4) Uani 1 1 d . U . . .
H5A H 0.0806 0.6900 0.3756 0.093 Uiso 1 1 calc R U . . .
H5B H 0.2336 0.6734 0.3422 0.093 Uiso 1 1 calc R U . . .
C6 C 0.359(2) 0.6547(16) 0.533(2) 0.092(6) Uani 1 1 d . U . . .
H6A H 0.3825 0.7047 0.5614 0.137 Uiso 1 1 calc R U . . .
H6B H 0.4138 0.6449 0.4719 0.137 Uiso 1 1 calc R U . . .
H6C H 0.3802 0.6164 0.5867 0.137 Uiso 1 1 calc R U . . .
C7 C 0.131(3) 0.6772(17) 0.586(2) 0.100(6) Uani 1 1 d . U . . .
H7A H 0.0966 0.6334 0.6236 0.149 Uiso 1 1 calc R U . . .
H7B H 0.0522 0.7076 0.5588 0.149 Uiso 1 1 calc R U . . .
H7C H 0.1898 0.7077 0.6347 0.149 Uiso 1 1 calc R U . . .
C8 C 0.171(3) 0.5718(13) 0.476(2) 0.098(6) Uani 1 1 d . U . . .
H8A H 0.1512 0.5458 0.5409 0.147 Uiso 1 1 calc R U . . .
H8B H 0.2480 0.5465 0.4436 0.147 Uiso 1 1 calc R U . . .
H8C H 0.0891 0.5707 0.4271 0.147 Uiso 1 1 calc R U . . .
N1 N 0.2828(16) 0.1017(9) 0.6317(12) 0.056(4) Uani 1 1 d . . . . .
N2 N 0.2100(18) 0.6520(9) 0.4999(15) 0.068(3) Uani 1 1 d . U . . .


_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 Br2 2.403(3) . ?
Co1 Br1 2.405(3) . ?
Co1 Br3 2.405(3) . ?
Co1 Br4 2.412(3) . ?
Br5 C1 1.89(3) . ?
Br6 C5 1.85(2) . ?
C1 N1 1.54(3) . ?
C2 N1 1.47(3) . ?
C3 N1 1.52(3) . ?
C4 N1 1.46(3) . ?
C5 N2 1.51(3) . ?
C6 N2 1.45(3) . ?
C7 N2 1.42(3) . ?
C8 N2 1.47(3) . ?

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
Br2 Co1 Br1 108.98(14) . . ?
Br2 Co1 Br3 107.97(15) . . ?
Br1 Co1 Br3 109.06(13) . . ?
Br2 Co1 Br4 112.57(13) . . ?
Br1 Co1 Br4 107.15(12) . . ?
Br3 Co1 Br4 111.07(13) . . ?
N1 C1 Br5 114.2(15) . . ?
N2 C5 Br6 116.7(16) . . ?
C2 N1 C4 108.8(19) . . ?
C2 N1 C3 112(2) . . ?
C4 N1 C3 113(2) . . ?
C2 N1 C1 109.7(17) . . ?
C4 N1 C1 107.4(19) . . ?
C3 N1 C1 106.6(19) . . ?
C7 N2 C6 109(2) . . ?
C7 N2 C8 108(2) . . ?
C6 N2 C8 108.5(18) . . ?
C7 N2 C5 113.8(18) . . ?
C6 N2 C5 110.8(19) . . ?
C8 N2 C5 106.2(18) . . ?

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
C3 H3C Br1 0.96 3.09 3.97(3) 153.1 4_566
C3 H3B Br1 0.96 2.89 3.81(3) 160.2 .
C3 H3A Br5 0.96 2.65 3.14(3) 111.7 .
C4 H4C Br2 0.96 3.02 3.95(3) 163.4 3_656
C4 H4C Br6 0.96 3.13 3.77(3) 125.2 3_666
C2 H2B Br5 0.96 2.82 3.29(3) 111.4 .
C1 H1B Br2 0.97 2.90 3.84(3) 164.0 .
C6 H6B Br4 0.96 3.08 3.76(2) 128.3 2_655
C6 H6A Br3 0.96 3.03 3.96(3) 162.4 3_666
C5 H5B Br3 0.97 2.86 3.75(3) 152.6 2_655
C5 H5A Br1 0.97 2.85 3.68(2) 144.1 2
C7 H7B Br1 0.96 3.03 3.66(3) 123.9 3_566

_refine_diff_density_max         3.129
_refine_diff_density_min         -1.556
_refine_diff_density_rms         0.204

