(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_7717097
_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 O2 S'
_chemical_formula_sum            'C13 H13 Cl F4 N2 O5 S2'
_chemical_formula_weight         452.82
_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             2024-03-06
_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                90
_cell_angle_beta                 92.262(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.7355(4)
_cell_length_b                   10.8997(5)
_cell_length_c                   21.2900(10)
_cell_measurement_reflns_used    6785
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.8210
_cell_measurement_theta_min      3.4190
_cell_volume                     1793.66(15)
_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 2014/5 (Sheldrick, 2014)'
_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 0.977
_diffrn_measured_fraction_theta_max 0.922
_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    -53.00 -11.00   0.50   17.99    --   -9.32 -23.00  20.00   84
  2  \w     -4.00  22.00   0.50   17.99    --   -9.32  23.00-174.00   52
  3  \w      6.00  76.00   0.50   17.99    --    9.60  23.00-174.00  140
  4  \w    -44.00 -19.00   0.50   17.99    --    9.60 -23.00  20.00   50
  5  \w    -55.00 -11.00   0.50   17.99    --   -9.32 125.00 120.00   88
  6  \w    -13.00  12.00   0.50   17.99    --    9.60 -99.00 -90.00   50
  7  \w    -39.00  -9.00   0.50   17.99    --    9.60 -77.00 -90.00   60
  8  \w     -9.00  39.00   0.50   17.99    --    9.60  77.00   0.00   96
  9  \w    -38.00  20.00   0.50   17.99    --    9.60 -77.00 -60.00  116
 10  \w      9.00  34.00   0.50   17.99    --    9.60-125.00  90.00   50
 11  \w     -6.00  39.00   0.50   17.99    --    9.60  77.00  60.00   90
 12  \w     25.00  56.00   0.50   17.99    --    9.60-125.00-180.00   62
 13  \w     18.00  56.00   0.50   17.99    --    9.60-125.00 -30.00   76
 14  \w      7.00  32.00   0.50   17.99    --    9.60-125.00  60.00   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      -0.0852093000
_diffrn_orient_matrix_UB_12      -0.0236347000
_diffrn_orient_matrix_UB_13      0.0014377000
_diffrn_orient_matrix_UB_21      0.0299447000
_diffrn_orient_matrix_UB_22      -0.0584584000
_diffrn_orient_matrix_UB_23      -0.0093327000
_diffrn_orient_matrix_UB_31      0.0163495000
_diffrn_orient_matrix_UB_32      -0.0160298000
_diffrn_orient_matrix_UB_33      0.0319769000
_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  0.0597
_diffrn_reflns_av_unetI/netI     0.0607
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.922
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            17191
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.124
_diffrn_reflns_theta_min         3.231
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.515
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58054
_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    1.677
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.011
_exptl_crystal_size_mid          0.008
_exptl_crystal_size_min          0.006
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         3648
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0903
_refine_ls_R_factor_gt           0.0505
_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^)+(0.0490P)^2^+0.4144P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1094
_refine_ls_wR_factor_ref         0.1256
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2303
_reflns_number_total             3648
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02286f2.cif
_cod_data_source_block           ex-jmso2
_cod_depositor_comments
;
Adding full bibliography for 7717095--7717097.cif.

2025-04-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C52 H52 Cl4 F16 N8 O20 S8'
_cod_original_formula_weight         1811.29
_cod_original_formula_moiety         '4(C F3 O3 S), 4(C12 H13 Cl F N2 O2 S)'
_cod_original_formula_units_Z            1
_cod_database_code               7717097
_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), C2(H2), C12(H12), C9(H9), C11(H11)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              99779
_shelx_hkl_checksum              3527
_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 1.646
_oxdiff_exptl_absorpt_empirical_full_min 0.373