Co(NCS)2 Chain Compound with Alternating 5- and 6-Fold Coordination: Influence of Metal Coordination on the Magnetic Properties
Michael Böhme; Michał Rams; Christoph Krebs; Sebastian Mangelsen; Inke Jess; Winfried Plass; Christian Näther; Inorganic Chemistry 61 (2022) 16841–16855; doi:10.1021/acs.inorgchem.2c02813

data_4350830
_publ_contact_author             'Christian N\"ather'
_publ_contact_author_email       cnaether@ac.uni-kiel.de
_publ_section_title
;
 Co(NCS)2 Chain Compound with Alternating 5- and 6-Fold Coordination:
 Influence of Metal Coordination on the Magnetic Properties
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   42
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              16841
_journal_page_last               16855
_journal_paper_doi               10.1021/acs.inorgchem.2c02813
_journal_volume                  61
_journal_year                    2022
_chemical_formula_moiety         'C19 H12 Br3 Co2 N7 S4'
_chemical_formula_sum            'C19 H12 Br3 Co2 N7 S4'
_chemical_formula_weight         824.19
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_contact_author_name
;
;
_audit_creation_date             2021-12-25
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_cell_angle_alpha                87.0930(10)
_cell_angle_beta                 86.9440(10)
_cell_angle_gamma                68.012(2)
_cell_formula_units_Z            2
_cell_length_a                   7.10020(10)
_cell_length_b                   8.8255(2)
_cell_length_c                   22.2445(4)
_cell_measurement_reflns_used    13819
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.7830
_cell_measurement_theta_min      3.9700
_cell_volume                     1289.96(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w   -119.00 -73.00   0.50   13.00    --  -47.64-125.00 -60.00   92
  2  \w    -70.00  25.00   0.50   13.00    --  -47.64  77.00 -30.00  190
  3  \w   -119.00 -25.00   0.50   13.00    --  -47.64 -77.00-150.00  188
  4  \w     34.00  95.00   0.50   13.00    --   47.64-125.00 -30.00  122
  5  \w     34.00  95.00   0.50   13.00    --   47.64-125.00  60.00  122
  6  \w    -27.00  26.00   0.50   13.00    --   47.64 -19.00 -30.00  106
  7  \w   -160.00 -71.00   0.50   45.00    --  -87.75 -61.00 -30.00  178
  8  \w    -71.00 -15.00   0.50   45.00    --  -87.75  61.00 -30.00  112
  9  \w     38.00  70.00   0.50   45.00    --  109.25 -60.00 118.00   64
 10  \w     37.00 106.00   0.50   45.00    --  109.25 -95.00 -90.00  138
 11  \w     97.00 178.00   0.50   45.00    --  109.25  30.00   0.00  162
 12  \w     37.00  71.00   0.50   45.00    --  109.25 -61.00-120.00   68
 13  \w     96.00 178.00   0.50   45.00    --  109.25  15.00 150.00  164
 14  \w     97.00 178.00   0.50   45.00    --  109.25  45.00  30.00  162
 15  \w     37.00 107.00   0.50   45.00    --  109.25-104.00  96.17  140
 16  \w     37.00 106.00   0.50   45.00    --  109.25 -95.00 -30.00  138
 17  \w     37.00 106.00   0.50   45.00    --  109.25 -95.00 120.00  138
 18  \w     37.00 106.00   0.50   45.00    --  109.25 -95.00 -60.00  138
 19  \w    149.00 178.00   0.50   45.00    --  109.25 125.00 -60.00   58
 20  \w     97.00 176.00   0.50   45.00    --  109.25  30.00-120.00  158
 21  \w     53.00 111.00   0.50   45.00    --  109.25-125.00-150.00  116
 22  \w     45.00  71.00   0.50   45.00    --  109.25 -61.00 -30.00   52
 23  \w     80.00 111.00   0.50   45.00    --  109.25-125.00 -30.00   62
 24  \w     95.00 124.00   0.50   45.00    --  109.25 125.00 -60.00   58
 25  \w     54.00 105.00   0.50   45.00    --  109.25 -77.00 -30.00  102
 26  \w     38.00  71.00   0.50   45.00    --  109.25 -77.00  90.00   66
 27  \w    111.00 170.00   0.50   45.00    --  109.25  30.00 -60.00  118
 28  \w    112.00 173.00   0.50   45.00    --  109.25  15.00  90.00  122
 29  \w     42.00  68.00   0.50   45.00    --  109.25 -61.00 -90.00   52
 30  \w     40.00  75.00   0.50   45.00    --  109.25-125.00 -30.00   70
 31  \w     37.00  78.00   0.50   45.00    --  109.25 -95.00  60.00   82
 32  \w     58.00  96.00   0.50   45.00    --  109.25 -77.00-180.00   76
 33  \w    104.00 170.00   0.50   45.00    --  109.25  45.00-180.00  132
 34  \w     46.00  71.00   0.50   45.00    --  109.25 -61.00  90.00   50
 35  \w     59.00  98.00   0.50   45.00    --  109.25 -95.00  30.00   78
 36  \w     37.00  66.00   0.50   45.00    --  109.25 -61.00 150.00   58
 37  \w     62.00 116.00   0.50   45.00    --  109.25-130.00 105.98  108
 38  \w     80.00 108.00   0.50   45.00    --  109.25-112.00-117.48   56
 39  \w     50.00  76.00   0.50   45.00    --  109.25-112.00-117.48   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1022956000
_diffrn_orient_matrix_UB_12      0.0768261000
_diffrn_orient_matrix_UB_13      -0.0487473000
_diffrn_orient_matrix_UB_21      0.1763312000
_diffrn_orient_matrix_UB_22      -0.1663351000
_diffrn_orient_matrix_UB_23      -0.0070689000
_diffrn_orient_matrix_UB_31      -0.1152026000
_diffrn_orient_matrix_UB_32      -0.0436835000
_diffrn_orient_matrix_UB_33      -0.0488783000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0200
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            18839
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.136
_diffrn_reflns_theta_min         3.982
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    18.761
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45364
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.121a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light red'
_exptl_crystal_density_diffrn    2.122
_exptl_crystal_description       plate
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.860
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       0.00021(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         5397
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0226
_refine_ls_R_factor_gt           0.0221
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0228P)^2^+2.1406P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0544
_refine_ls_wR_factor_ref         0.0546
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5314
_reflns_number_total             5397
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ck767_ck768.cif
_cod_data_source_block           ck767
_cod_original_cell_volume        1289.96(4)
_cod_database_code               4350830
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C19 H12Br3Co2N7S4'
_chemical_oxdiff_usercomment     ck767
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C13(H13), C14(H14), C15(H15), C21(H21), C23(H23), C24(H24),
 C25(H25), C31(H31), C33(H33), C34(H34), C35(H35)
;
_shelx_res_checksum              38426
_shelx_hkl_checksum              38626
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.965
_oxdiff_exptl_absorpt_empirical_full_min 0.421