Establishing σ-hole tetrel bonds by hemidirected lead(ii) phosphonodithioates
Kumar, Pretam; Gomila, Rosa M.; Frontera, Antonio; Pandey, Sushil K.; CrystEngComm 27 (2025) 6386–6396; doi:10.1039/D5CE00611B

data_7250820
_publ_section_title
;
 Establishing \s-hole tetrel bonds by hemidirected lead(ii)
 phosphonodithioates
;
_journal_issue                   38
_journal_name_full               CrystEngComm
_journal_page_first              6386
_journal_page_last               6396
_journal_paper_doi               10.1039/D5CE00611B
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C56 H56 O8 P4 Pb2 S8'
_chemical_formula_sum            'C56 H56 O8 P4 Pb2 S8'
_chemical_formula_weight         1651.74
_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     iterative
_audit_creation_date             2023-01-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-01-13 deposited with the CCDC.	2025-08-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.996(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.3663(5)
_cell_length_b                   23.2716(12)
_cell_length_c                   13.8240(6)
_cell_measurement_reflns_used    4019
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      27.5550
_cell_measurement_theta_min      2.1720
_cell_volume                     3235.9(3)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 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 0.882
_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    -22.00  37.00   1.00   49.87    --  -27.72 -19.00 -30.00   59
  2  \w     39.00 116.00   1.00   49.87    --   28.04 178.00-120.00   77
  3  \w      2.00 105.00   1.00   49.87    --   28.04  57.00 -60.00  103
;
_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      0.0290957000
_diffrn_orient_matrix_UB_12      -0.0273233000
_diffrn_orient_matrix_UB_13      0.0138560000
_diffrn_orient_matrix_UB_21      0.0496668000
_diffrn_orient_matrix_UB_22      0.0131157000
_diffrn_orient_matrix_UB_23      0.0379514000
_diffrn_orient_matrix_UB_31      -0.0406604000
_diffrn_orient_matrix_UB_32      -0.0034107000
_diffrn_orient_matrix_UB_33      0.0341114000
_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  0.0479
_diffrn_reflns_av_unetI/netI     0.0901
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.882
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11231
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.882
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.194
_diffrn_reflns_theta_min         1.750
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.602
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.16997
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_description       block
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.678
_refine_diff_density_min         -1.875
_refine_diff_density_rms         0.238
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.299
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         7020
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.299
_refine_ls_R_factor_all          0.1234
_refine_ls_R_factor_gt           0.0899
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2264
_refine_ls_wR_factor_ref         0.2502
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4936
_reflns_number_total             7020
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00611b2.cif
_cod_data_source_block           pblrpc_lt_mo
_cod_depositor_comments
'Adding full bibliography for 7250819--7250820.cif.'
_cod_database_code               7250820
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'c h n o Pb'
_shelx_estimated_absorpt_t_max   0.604
_shelx_estimated_absorpt_t_min   0.284
_reflns_odcompleteness_completeness 99.50
_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 Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C12(H12), C27(H27), C20(H20), C23(H23), C19(H19), C13(H13),
 C24(H24), C10(H10), C26(H26), C16(H16), C9(H9), C3(H3), C17(H17), C2(H2)
2.b Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C7(H7A,H7B,H7C), C21(H21A,H21B,H21C), C14(H14A,H14B,H14C)
;
_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 5.476
_oxdiff_exptl_absorpt_empirical_full_min 0.466