Thiazetidin-2-ylidenes as four membered N-heterocyclic carbenes: theoretical studies and the generation of complexes with N<sup>+</sup> center.
Dubey, Gurudutt; Mahawar, Nutan; Singh, Tejender; Saha, Nirjhar; Sahoo, Subash C.; Bharatam, Prasad V.; Physical chemistry chemical physics : PCCP 24 (2022) 629–633; doi:10.1039/d1cp04732a

data_7244100
_publ_section_title
;
 Thiazetidin-2-ylidenes as four membered N-heterocyclic carbenes:
 theoretical studies and the generation of complexes with N<sup>+</sup>
 center.
;
_journal_issue                   2
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              629
_journal_page_last               633
_journal_paper_doi               10.1039/d1cp04732a
_journal_volume                  24
_journal_year                    2022
_chemical_formula_moiety         'C17 H16 N3 S2, C F3 O3 S'
_chemical_formula_sum            'C18 H16 F3 N3 O3 S3'
_chemical_formula_weight         475.52
_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
_audit_creation_date             2021-07-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-12 deposited with the CCDC.	2021-12-13 downloaded from the CCDC.
;
_cell_angle_alpha                107.755(2)
_cell_angle_beta                 96.663(2)
_cell_angle_gamma                92.537(2)
_cell_formula_units_Z            4
_cell_length_a                   10.4325(2)
_cell_length_b                   11.4030(3)
_cell_length_c                   18.4984(4)
_cell_measurement_reflns_used    13406
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.7190
_cell_measurement_theta_min      3.3680
_cell_volume                     2074.24(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (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_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_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     20.00  57.00   0.50   12.00    --   -9.79  25.00 107.00   74
  2  \w    -64.00 -39.00   0.50   12.00    --   -9.79 -25.00 -55.00   50
  3  \w    -58.00  19.00   0.50   12.00    --   10.07 -25.00 -55.00  154
  4  \w      3.00  49.00   0.50   12.00    --   10.07  25.00 107.00   92
  5  \w    -17.00   9.00   0.50   12.00    --   -9.79  57.00 -90.00   52
  6  \w    -58.00  -3.00   0.50   12.00    --   -9.79 125.00-180.00  110
  7  \w    -58.00  -4.00   0.50   12.00    --   -9.79 125.00   0.00  108
  8  \w    -19.00  61.00   0.50   12.00    --   -9.79  19.00-150.00  160
  9  \w    -57.00  -3.00   0.50   12.00    --   -9.79 125.00  90.00  108
 10  \w      4.00  35.00   0.50   12.00    --   10.07 -99.00-150.00   62
 11  \w     14.00  40.00   0.50   12.00    --   10.07-125.00   0.00   52
 12  \w    -17.00   8.00   0.50   12.00    --   10.07 -99.00-120.00   50
 13  \w    -19.00  43.00   0.50   12.00    --   10.07 -99.00 -60.00  124
 14  \w     17.00  42.00   0.50   12.00    --   10.07-125.00 120.00   50
 15  \w    -54.00  23.00   0.50   12.00    --   10.07 -38.00  60.00  154
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.910
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28811
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.569
_diffrn_reflns_theta_min         3.255
_exptl_absorpt_coefficient_mu    0.410
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_description       rod
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     633
_refine_ls_number_reflns         8561
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0516
_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^)+(0.0455P)^2^+0.7585P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1120
_refine_ls_wR_factor_ref         0.1287
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5517
_reflns_number_total             8561
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cp04732a2.cif
_cod_data_source_block           dn6
_cod_depositor_comments          'Adding full bibliography for 7244100.cif.'
_cod_original_cell_volume        2074.24(8)
_cod_database_code               7244100
_shelx_shelxl_version_number     2017/1
_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. Rigid body (RIGU) restrains
 F4, F4A, F5, F5A, F6, F6A
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 C17B, C16B, C15B, C14B, C13A, C12A
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 C17A, C16A, C15A, C14A, C13A, C12A
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
3. Others
 Fixed Sof: F6A(0.4) C17A(0.6) H17A(0.6) F4A(0.7) O4A(0.5) O6(0.5) C16A(0.6)
 H16A(0.6) F5A(0.6) C14A(0.6) H14A(0.6) C15A(0.6) H15A(0.6) C14B(0.4) H14B(0.4)
 C15B(0.4) H15B(0.4) C16B(0.4) H16B(0.4) C17B(0.4) H17B(0.4) F4(0.3) F5(0.4)
 F6(0.6) O6A(0.5) O5A(0.3) O5(0.7) O4(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C11(H11C,H11D), C2(H2A,H2B), C2A(H2AA,H2AB), C11A(H11A,H11B)
4.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C5A(H5A), C13(H13), C5(H5), C8A(H8A), C8(H8), C15(H15), C16(H16),
 C6A(H6A), C14(H14), C7(H7), C13A(H13A), C7A(H7A), C6(H6), C17A(H17A),
 C16A(H16A), C14A(H14A), C15A(H15A), C14B(H14B), C15B(H15B), C16B(H16B),
 C17B(H17B)
4.c Idealised Me refined as rotating group:
 C10(H10D,H10E,H10F), C10A(H10A,H10B,H10C)
;
_shelx_res_checksum              7055
_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
;