A single carbon atom controls the geometry and reactivity of Co<sup>II</sup>(N<sub>2</sub>S<sub>2</sub>) complexes.
Jana, Manish; Quiroz, Manuel; Darensbourg, Marcetta Y.; Chemical communications (Cambridge, England) 60 (2024) 1128–1131; doi:10.1039/d3cc05394f

data_7132483
_publ_section_title
;
 A single carbon atom controls the geometry and reactivity of
 Co<sup>II</sup>(N<sub>2</sub>S<sub>2</sub>) complexes.
;
_journal_issue                   9
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1128
_journal_page_last               1131
_journal_paper_doi               10.1039/d3cc05394f
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C40 H52 Co2 N4 S4'
_chemical_formula_sum            'C40 H52 Co2 N4 S4'
_chemical_formula_weight         834.95
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Hygroscopic,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-12
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-10-19 deposited with the CCDC.	2023-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.083(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.8761(3)
_cell_length_b                   13.6323(3)
_cell_length_c                   15.8821(3)
_cell_measurement_reflns_used    12290
_cell_measurement_temperature    100.01(12)
_cell_measurement_theta_max      76.2960
_cell_measurement_theta_min      3.3560
_cell_volume                     3784.60(13)
_computing_cell_refinement       'CrysAlisPro 1.171.42.101a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.101a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.101a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(12)
_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 0.999
_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    -79.00  23.00   1.00   10.00    --  -47.69  98.00   6.00  102
  2  \w     -5.00  79.00   1.00   10.00    --   47.69 -98.00-100.00   84
  3  \w    -80.00 -21.00   1.00   20.00    --  -91.75  98.00   6.00   59
  4  \w   -162.00 -86.00   1.00   20.00    --  -91.75 -98.00-100.00   76
  5  \w     36.00 106.00   1.00   20.00    --  106.12 -98.00-100.00   70
  6  \w    106.00 177.00   1.00   20.00    --  106.12  98.00   6.00   71
  7  \w    -43.00  25.00   1.00   10.00    --  -47.69  38.00 -30.00   68
  8  \w    -26.00  28.00   1.00   10.00    --  -47.69  19.00 -90.00   54
  9  \w   -118.00 -73.00   1.00   10.00    --  -47.69-126.00  60.00   45
 10  \w    -27.00  26.00   1.00   10.00    --   47.69 -19.00   0.00   53
 11  \w    -27.00  26.00   1.00   10.00    --   47.69 -19.00-120.00   53
 12  \w     25.00 120.00   1.00   10.00    --   47.69  77.00   0.00   95
 13  \w    -50.00 -20.00   1.00   20.00    --  -91.75  45.00 -60.00   30
 14  \w   -163.00 -78.00   1.00   20.00    --  -91.75 -51.00 -50.65   85
 15  \w    -87.00 -21.00   1.00   20.00    --  -91.75 126.00-120.00   66
 16  \w    -50.00 -20.00   1.00   20.00    --  -91.75  45.00 150.00   30
 17  \w    -50.00 -20.00   1.00   20.00    --  -91.75  45.00-120.00   30
 18  \w   -163.00 -77.00   1.00   20.00    --  -91.75 -57.00 168.24   86
 19  \w    -50.00 -20.00   1.00   20.00    --  -91.75  45.00   0.00   30
 20  \w   -163.00 -79.00   1.00   20.00    --  -91.75 -45.00-150.00   84
 21  \w    -50.00 -20.00   1.00   20.00    --  -91.75  45.00  30.00   30
 22  \w    -50.00 -20.00   1.00   20.00    --  -91.75  45.00-150.00   30
 23  \w    -50.00 -20.00   1.00   20.00    --  -91.75  45.00 -30.00   30
 24  \w    -71.00 -19.00   1.00   20.00    --  -91.75  61.00  60.00   52
 25  \w   -163.00 -70.00   1.00   20.00    --  -91.75 -74.00 -51.13   93
 26  \w    -71.00 -19.00   1.00   20.00    --  -91.75  61.00   0.00   52
 27  \w   -166.00 -79.00   1.00   20.00    --  -91.75 -30.00-180.00   87
 28  \w     34.00 105.00   1.00   20.00    --  106.12 -95.00  30.00   71
 29  \w     95.00 177.00   1.00   20.00    --  106.12 126.00-180.00   82
 30  \w     34.00 105.00   1.00   20.00    --  106.12 -77.00  90.00   71
 31  \w     94.00 178.00   1.00   20.00    --  106.12  30.00 150.00   84
 32  \w     34.00 105.00   1.00   20.00    --  106.12 -95.00   0.00   71
 33  \w     34.00 105.00   1.00   20.00    --  106.12 -95.00-150.00   71
 34  \w     34.00  71.00   1.00   20.00    --  106.12 -61.00-180.00   37
 35  \w     34.00  71.00   1.00   20.00    --  106.12 -61.00  30.00   37
 36  \w     94.00 178.00   1.00   20.00    --  106.12  45.00-180.00   84
 37  \w     36.00 112.00   1.00   20.00    --  106.12-126.00 120.00   76
 38  \w     34.00  71.00   1.00   20.00    --  106.12 -61.00 -90.00   37
 39  \w     37.00 108.00   1.00   20.00    --  106.12-108.00   7.09   71
 40  \w     34.00 105.00   1.00   20.00    --  106.12 -95.00 -60.00   71
 41  \w     34.00 105.00   1.00   20.00    --  106.12 -95.00 -90.00   71
 42  \w     37.00 108.00   1.00   20.00    --  106.12-108.00-169.38   71
 43  \w     39.00  70.00   1.00   20.00    --  106.12 -61.00  90.00   31
;
_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      0.0034239000
_diffrn_orient_matrix_UB_12      -0.0727658000
_diffrn_orient_matrix_UB_13      -0.0733237000
_diffrn_orient_matrix_UB_21      -0.0363025000
_diffrn_orient_matrix_UB_22      0.0775936000
_diffrn_orient_matrix_UB_23      -0.0665751000
_diffrn_orient_matrix_UB_31      0.0802392000
_diffrn_orient_matrix_UB_32      0.0382005000
_diffrn_orient_matrix_UB_33      -0.0044100000
_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  0.0821
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            31776
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.075
_diffrn_reflns_theta_min         4.113
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.195
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.923
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.101a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic greenish green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_description       needle
_exptl_crystal_F_000             1752
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DMF ETHER'
_exptl_crystal_size_max          0.081
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3587
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0378P)^2^+10.8230P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.0988
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3177
_reflns_number_total             3587
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05394f2.cif
_cod_data_source_block           mj_co_dabz
_cod_depositor_comments
'Adding full bibliography for 7132482--7132485.cif.'
_cod_database_code               7132483
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Co C H N S'
_shelx_estimated_absorpt_t_max   0.803
_shelx_estimated_absorpt_t_min   0.523
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C14(H14A,H14B)
2.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C16(H16), C17(H17), C18(H18),
 C19(H19), C20(H20)
;
_shelx_res_checksum              88274
_shelx_hkl_checksum              72304
_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 3.030
_oxdiff_exptl_absorpt_empirical_full_min 0.446