An insight into triel bonds in O,O′-diarylphosphorodithioates of thallium(i): experimental and theoretical investigations
Firdoos, Tahira; Kumar, Pretam; Radha, Anu; Gomila, Rosa M.; Frontera, Antonio; Sood, Puneet; Pandey, Sushil K.; New Journal of Chemistry 46 (2022) 832–843; doi:10.1039/D1NJ04852J

data_7061092
_publ_section_title
;
 An insight into triel bonds in O,O&#x2032;-diarylphosphorodithioates of
 thallium(i): experimental and theoretical investigations
;
_journal_issue                   2
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              832
_journal_page_last               843
_journal_paper_doi               10.1039/D1NJ04852J
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C18 H22 O2 P S2 Tl'
_chemical_formula_sum            'C18 H22 O2 P S2 Tl'
_chemical_formula_weight         569.82
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-07-02
_audit_creation_method
;
Olex2 1.2-ac21
(compiled 2015.09.16 svn.r134, GUI svn.r4998)
;
_audit_update_record
;
2021-09-13 deposited with the CCDC.	2021-11-29 downloaded from the CCDC.
;
_cell_angle_alpha                107.092(11)
_cell_angle_beta                 95.785(10)
_cell_angle_gamma                90.443(8)
_cell_formula_units_Z            2
_cell_length_a                   8.4373(8)
_cell_length_b                   9.6672(9)
_cell_length_c                   12.6725(19)
_cell_measurement_reflns_used    2393
_cell_measurement_temperature    150.0(3)
_cell_measurement_theta_max      28.1060
_cell_measurement_theta_min      2.2170
_cell_volume                     982.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9974
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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     35.00 120.00   1.00    4.46    --   26.84 178.00  90.00   85
  2  \w     28.00 107.00   1.00    4.46    --   26.84  37.00 -60.00   79
  3  \w    -54.00  67.00   1.00    4.46    --   26.84 -77.00  60.00  121
  4  \w    -47.00  65.00   1.00    4.46    --   26.84 -57.00 150.00  112
;
_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      -0.0193326000
_diffrn_orient_matrix_UB_12      0.0131258000
_diffrn_orient_matrix_UB_13      0.0552004000
_diffrn_orient_matrix_UB_21      0.0784940000
_diffrn_orient_matrix_UB_22      -0.0168244000
_diffrn_orient_matrix_UB_23      0.0165883000
_diffrn_orient_matrix_UB_31      0.0247899000
_diffrn_orient_matrix_UB_32      0.0737984000
_diffrn_orient_matrix_UB_33      0.0121225000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1080
_diffrn_reflns_av_unetI/netI     0.1221
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5647
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         2.21
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    8.524
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49556
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.927
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       triclinic
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.176
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.064
_refine_diff_density_max         4.812
_refine_diff_density_min         -3.106
_refine_diff_density_rms         0.338
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         4026
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1039
_refine_ls_R_factor_gt           0.0893
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0897P)^2^+26.2224P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2072
_refine_ls_wR_factor_ref         0.2222
_reflns_number_gt                3316
_reflns_number_total             4026
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d1nj04852j2.cif
_cod_data_source_block           tl_4iso_lt_mo
_cod_depositor_comments
'Adding full bibliography for 7061091--7061092.cif.'
_cod_database_code               7061092
_chemical_oxdiff_formula         'C36 H42 O4 P2 S4 Tl2'
_reflns_odcompleteness_completeness 98.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 Ternary CH refined with riding coordinates:
 C5(H5), C4(H4)
2.b Aromatic/amide H refined with riding coordinates:
 C1AA(H1AA), C9(H9), C15(H15), C17(H17), C20(H20), C22(H22), C26(H26), C30(H30)
2.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C8(H8A,H8B,H8C), C1(H1A,H1B,H1C), C2AA(H2AA,H2AB,H2AC)
;
_olex2_date_sample_data_collection 2021-05-03
_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 1.940
_oxdiff_exptl_absorpt_empirical_full_min 0.674