(Imidazol-2-ylidene) → S coordination interactions and its modulation upon <i>S</i>-oxidation.
Mukhopadhyay, Joy; Sahoo, Subash C.; Bharatam, Prasad V.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 17050–17058; doi:10.1039/d4dt02286f

data_7717096
_publ_section_title
;
 (Imidazol-2-ylidene) &#x2192; S coordination interactions and its
 modulation upon <i>S</i>-oxidation.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17050
_journal_page_last               17058
_journal_paper_doi               10.1039/d4dt02286f
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C F3 O3 S, C12 H13 Cl F N2 S'
_chemical_formula_sum            'C13 H13 Cl F4 N2 O3 S2'
_chemical_formula_weight         420.82
_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_creation_date             2024-03-06
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2024-03-13 deposited with the CCDC.	2024-09-23 downloaded from the CCDC.
;
_cell_angle_alpha                82.544(6)
_cell_angle_beta                 81.102(6)
_cell_angle_gamma                67.567(9)
_cell_formula_units_Z            2
_cell_length_a                   7.7328(7)
_cell_length_b                   7.9098(7)
_cell_length_c                   15.8738(9)
_cell_measurement_reflns_used    5183
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0070
_cell_measurement_theta_min      3.3080
_cell_volume                     883.98(14)
_computing_cell_refinement       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.924
_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    -44.00   1.00   0.50   10.40    --   -9.32 106.00 131.00   90
  2  \w     -9.00  16.00   0.50   10.40    --    9.60-106.00  31.00   50
  3  \w    -33.00  16.00   0.50   10.40    --   -9.32 -77.00 -60.00   98
  4  \w    -20.00  14.00   0.50   10.40    --    9.60  99.00 121.48   68
  5  \w    -35.00  -8.00   0.50   10.40    --    9.60 125.00-130.13   54
  6  \w     -4.00  74.00   0.50   10.40    --    9.60  38.00 150.00  156
  7  \w    -37.00   6.00   0.50   10.40    --    9.60 -77.00 -30.00   86
  8  \w    -14.00  28.00   0.50   10.40    --    9.60 -99.00  60.00   84
  9  \w    -20.00  13.00   0.50   10.40    --    9.60  98.00 -27.12   66
 10  \w    -40.00 -14.00   0.50   10.40    --    9.60 -77.00-120.00   52
 11  \w     -9.00  35.00   0.50   10.40    --    9.60 -77.00-120.00   88
 12  \w    -61.00  20.00   0.50   10.40    --    9.60 -19.00 150.00  162
 13  \w     15.00  54.00   0.50   10.40    --    9.60-125.00 120.00   78
 14  \w    -10.00  40.00   0.50   10.40    --    9.60 -99.00-150.00  100
 15  \w    -25.00   1.00   0.50   10.40    --    9.60 -38.00 -90.00   52
 16  \w    -45.00 -20.00   0.50   10.40    --    9.60 -38.00-120.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0763975000
_diffrn_orient_matrix_UB_12      0.0844281000
_diffrn_orient_matrix_UB_13      0.0063568000
_diffrn_orient_matrix_UB_21      0.0158349000
_diffrn_orient_matrix_UB_22      -0.0075062000
_diffrn_orient_matrix_UB_23      0.0434018000
_diffrn_orient_matrix_UB_31      0.0623838000
_diffrn_orient_matrix_UB_32      0.0477941000
_diffrn_orient_matrix_UB_33      -0.0115673000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_unetI/netI     0.0476
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10987
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.095
_diffrn_reflns_theta_min         3.174
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.507
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97599
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_description       block
_exptl_crystal_F_000             428
_exptl_crystal_size_max          0.008
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.004
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         3596
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0497P)^2^+0.1474P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1094
_refine_ls_wR_factor_ref         0.1258
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2339
_reflns_number_total             3596
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02286f2.cif
_cod_data_source_block           ex-jmso2a2_auto
_cod_depositor_comments
'Adding full bibliography for 7717095--7717097.cif.'
_cod_database_code               7717096
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C H N O Cl F S'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C9(H9), C2(H2), C12(H12), C11(H11)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              26367
_shelx_hkl_checksum              92773
_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 1.176
_oxdiff_exptl_absorpt_empirical_full_min 0.849