(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_7717095
_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         'C12 H13 Cl F N2 O S, C F3 O3 S'
_chemical_formula_sum            'C13 H13 Cl F4 N2 O4 S2'
_chemical_formula_weight         436.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-01
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2024-02-25 deposited with the CCDC.	2024-09-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.209(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.1258(3)
_cell_length_b                   25.4289(9)
_cell_length_c                   11.3897(4)
_cell_measurement_reflns_used    9233
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.8830
_cell_measurement_theta_min      3.4200
_cell_volume                     1771.42(12)
_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 0.963
_diffrn_measured_fraction_theta_max 0.916
_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      7.00  42.00   0.50   16.94    --   -9.32  76.00  20.00   70
  2  \w    -37.00 -12.00   0.50   16.94    --   -9.32 -76.00-106.00   50
  3  \w     -4.00  30.00   0.50   16.94    --    9.60  76.00  20.00   68
  4  \w    -28.00  -3.00   0.50   16.94    --    9.60 -76.00-106.00   50
  5  \w    -40.00   6.00   0.50   16.94    --   -9.32 -77.00-180.00   92
  6  \w    -53.00  -7.00   0.50   16.94    --   -9.32 125.00-180.00   92
  7  \w    -27.00  49.00   0.50   16.94    --   -9.32  57.00 -60.00  152
  8  \w    -56.00  -7.00   0.50   16.94    --   -9.32 125.00  30.00   98
  9  \w    -14.00  11.00   0.50   16.94    --    9.60 -99.00 150.00   50
 10  \w      8.00  46.00   0.50   16.94    --    9.60-125.00-150.00   76
 11  \w    -57.00  21.00   0.50   16.94    --    9.60 -19.00 -60.00  156
 12  \w    -13.00  20.00   0.50   16.94    --    9.60  77.00 150.00   66
;
_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      -0.0912654000
_diffrn_orient_matrix_UB_12      0.0171935000
_diffrn_orient_matrix_UB_13      -0.0005213000
_diffrn_orient_matrix_UB_21      -0.0547317000
_diffrn_orient_matrix_UB_22      -0.0157059000
_diffrn_orient_matrix_UB_23      -0.0438727000
_diffrn_orient_matrix_UB_31      -0.0461185000
_diffrn_orient_matrix_UB_32      -0.0153462000
_diffrn_orient_matrix_UB_33      0.0443374000
_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  0.0562
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.916
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16277
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.065
_diffrn_reflns_theta_min         3.204
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.514
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47143
_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    1.638
_exptl_crystal_description       block
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.011
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.008
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         3565
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0576
_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^)+(0.0966P)^2^+0.8275P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1622
_refine_ls_wR_factor_ref         0.1749
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2682
_reflns_number_total             3565
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02286f2.cif
_cod_data_source_block           ex-nipjmso2cl4f_autored
_cod_depositor_comments
'Adding full bibliography for 7717095--7717097.cif.'
_cod_database_code               7717095
_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:
 C8(H8), C3(H3), C2(H2), C11(H11), C9(H9)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              4349
_shelx_hkl_checksum              1260
_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 1.811
_oxdiff_exptl_absorpt_empirical_full_min 0.535