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_4350831
_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      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_contact_author_name
;
;
_audit_creation_date             2021-05-10
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.4026(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.05905(8)
_cell_length_b                   16.33462(16)
_cell_length_c                   11.25627(10)
_cell_measurement_reflns_used    21672
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.2450
_cell_measurement_theta_min      3.9030
_cell_volume                     1295.64(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.105a (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  (Sheldrick, 2015)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.992
_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 -25.00   0.50   14.69    --  -47.54 -77.00  90.00  188
  2  \w    -70.00  25.00   0.50   14.69    --  -47.54  77.00-150.00  190
  3  \w    -25.00  43.00   0.50   14.69    --   47.54 -38.00  30.00  136
  4  \w     35.00 121.00   0.50   14.69    --   47.54  38.00 -60.00  172
  5  \w     34.00  95.00   0.50   14.69    --   47.54-125.00  90.00  122
  6  \w     35.00 121.00   0.50   14.69    --   47.54  38.00-150.00  172
  7  \w   -166.00 -78.00   0.50   58.74    --  -91.75 -15.00  90.00  176
  8  \w   -166.00 -78.00   0.50   58.74    --  -91.75 -15.00-180.00  176
  9  \w     42.00 105.00   0.50   58.74    --  113.25 -77.00 -60.00  126
 10  \w     97.00 178.00   0.50   58.74    --  113.25  61.00  90.00  162
 11  \w     42.00  71.00   0.50   58.74    --  113.25 -61.00-180.00   58
 12  \w     42.00 106.00   0.50   58.74    --  113.25 -95.00  60.00  128
 13  \w     97.00 178.00   0.50   58.74    --  113.25  61.00 -90.00  162
 14  \w    101.00 178.00   0.50   58.74    --  113.25  45.00  60.00  154
 15  \w     42.00 108.00   0.50   58.74    --  113.25-111.00  58.44  132
 16  \w    101.00 178.00   0.50   58.74    --  113.25  45.00 -60.00  154
 17  \w    101.00 178.00   0.50   58.74    --  113.25  30.00-150.00  154
 18  \w    101.00 178.00   0.50   58.74    --  113.25  30.00  30.00  154
 19  \w     42.00 106.00   0.50   58.74    --  113.25 -95.00-177.49  128
 20  \w     42.00 105.00   0.50   58.74    --  113.25 -77.00-120.00  126
 21  \w     42.00 106.00   0.50   58.74    --  113.25 -95.00  90.00  128
 22  \w     97.00 178.00   0.50   58.74    --  113.25  61.00 150.00  162
 23  \w     42.00 111.00   0.50   58.74    --  113.25-125.00-180.00  138
 24  \w     42.00 105.00   0.50   58.74    --  113.25 -77.00-150.00  126
 25  \w     42.00 105.00   0.50   58.74    --  113.25 -77.00 120.00  126
 26  \w     42.00 106.00   0.50   58.74    --  113.25 -95.00   0.00  128
 27  \w    101.00 178.00   0.50   58.74    --  113.25  45.00  30.00  154
 28  \w     42.00 107.00   0.50   58.74    --  113.25-103.00-170.84  130
 29  \w     42.00 106.00   0.50   58.74    --  113.25 -97.00-107.59  128
 30  \w     42.00 111.00   0.50   58.74    --  113.25-125.00 -90.00  138
 31  \w     42.00 111.00   0.50   58.74    --  113.25-125.00   0.00  138
 32  \w     42.00  71.00   0.50   58.74    --  113.25 -61.00 -30.00   58
 33  \w     42.00 106.00   0.50   58.74    --  113.25 -95.00 120.00  128
 34  \w     42.00 111.00   0.50   58.74    --  113.25-125.00-120.00  138
 35  \w     42.00 111.00   0.50   58.74    --  113.25-125.00 120.00  138
 36  \w     48.00 130.00   0.50   58.74    --  113.25-151.00  46.51  164
 37  \w   -119.00 -33.00   0.50   14.69    --  -47.54 -57.00-150.00  172
 38  \w   -119.00 -25.00   0.50   14.69    --  -47.54 -77.00  30.00  188
 39  \w   -119.00 -25.00   0.50   14.69    --  -47.54 -77.00-180.00  188
 40  \w   -119.00 -65.00   0.50   14.69    --  -47.54 -77.00 -30.00  108
 41  \w   -119.00 -25.00   0.50   14.69    --  -47.54 -77.00 150.00  188
 42  \w     34.00  95.00   0.50   14.69    --   47.54-125.00 -60.00  122
 43  \w     25.00 119.00   0.50   14.69    --   47.54  77.00 -90.00  188
 44  \w     33.00 119.00   0.50   14.69    --   47.54  57.00   0.00  172
;
_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      -0.0964300000
_diffrn_orient_matrix_UB_12      0.0654662000
_diffrn_orient_matrix_UB_13      -0.0814870000
_diffrn_orient_matrix_UB_21      -0.1958329000
_diffrn_orient_matrix_UB_22      -0.0279819000
_diffrn_orient_matrix_UB_23      0.0380758000
_diffrn_orient_matrix_UB_31      0.0134846000
_diffrn_orient_matrix_UB_32      0.0618445000
_diffrn_orient_matrix_UB_33      0.1034325000
_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  0.0348
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            26884
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.930
_diffrn_reflns_theta_min         3.934
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    18.679
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.105a (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    2.113
_exptl_crystal_description       needle
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.781
_refine_diff_density_min         -0.757
_refine_diff_density_rms         0.205
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.496(8)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         5212
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0473
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0857P)^2^+6.6239P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1325
_refine_ls_wR_factor_ref         0.1326
_reflns_Friedel_coverage         0.931
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                5169
_reflns_number_total             5212
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ck767_ck768.cif
_cod_data_source_block           ck768
_cod_database_code               4350831
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C36H22Br6Mn4N16S8
_chemical_oxdiff_usercomment     'Christoph Kerbs  ck768  co-3Brompy'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.504(8)
 0.496(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Rigid body (RIGU) restrains
 C21, C22, C23, C24, C25
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
4.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              71584
_shelx_hkl_checksum              14720
_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 2.817
_oxdiff_exptl_absorpt_empirical_full_min 0.729