Thallium(i)phosphorodithioates containing intra- and intermolecular π-hole triel bonds
Firdoos, Tahira; Kumar, Pretam; Sharma, Nipunn; Gomila, Rosa M.; Frontera, Antonio; Sood, Puneet; Pandey, Sushil K.; CrystEngComm 25 (2023) 3777–3789; doi:10.1039/D3CE00396E

data_7246901
_publ_section_title
;
 Thallium(i)phosphorodithioates containing intra- and intermolecular
 \p-hole triel bonds
;
_journal_issue                   26
_journal_name_full               CrystEngComm
_journal_page_first              3777
_journal_page_last               3789
_journal_paper_doi               10.1039/D3CE00396E
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C16 H18 O2 P S2 Tl'
_chemical_formula_sum            'C16 H18 O2 P S2 Tl'
_chemical_formula_weight         541.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-03
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2023-04-11 deposited with the CCDC.	2023-06-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.128(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.7730(19)
_cell_length_b                   7.5700(3)
_cell_length_c                   19.9962(11)
_cell_measurement_reflns_used    2686
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      27.8700
_cell_measurement_theta_min      2.1600
_cell_volume                     3639.0(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_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 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9974
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  26.00   1.00   25.00    --  -27.88 -99.00 150.00   46
  2  \w     40.00 116.00   1.00   25.00    --   28.04 178.00 120.00   76
  3  \w    -23.00  96.00   1.00   25.00    --   28.04  38.00-180.00  119
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0293656000
_diffrn_orient_matrix_UB_12      -0.0007440000
_diffrn_orient_matrix_UB_13      0.0167665000
_diffrn_orient_matrix_UB_21      0.0005656000
_diffrn_orient_matrix_UB_22      0.0927715000
_diffrn_orient_matrix_UB_23      -0.0046564000
_diffrn_orient_matrix_UB_31      -0.0024981000
_diffrn_orient_matrix_UB_32      0.0130387000
_diffrn_orient_matrix_UB_33      0.0338676000
_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  0.0274
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.891
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            6074
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.132
_diffrn_reflns_theta_min         2.184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    9.197
_exptl_absorpt_correction_T_max  0.239
_exptl_absorpt_correction_T_min  0.051
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
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_density_diffrn    1.978
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       monoclinic
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.418
_exptl_crystal_size_mid          0.349
_exptl_crystal_size_min          0.237
_refine_diff_density_max         2.196
_refine_diff_density_min         -2.681
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.828
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         3965
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.828
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0914P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1096
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3373
_reflns_number_total             3965
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00396e2.cif
_cod_data_source_block           tl_2_5_lt_mo
_cod_depositor_comments
'Adding full bibliography for 7246901--7246902.cif.'
_cod_database_code               7246901
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C128  H144  O16  P8  S16  Tl8  '
_shelx_estimated_absorpt_t_max   0.219
_shelx_estimated_absorpt_t_min   0.114
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C10(H10), C12(H12), C2(H2), C5(H5), C4(H4)
2.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              66225
_shelx_hkl_checksum              77124
_olex2_date_sample_data_collection 2022-11-02
_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 3.836
_oxdiff_exptl_absorpt_empirical_full_min 0.358