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_7250819
_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_absolute_configuration ad
_chemical_formula_moiety         'C15 H16 O2 P S2, C6 H16 N'
_chemical_formula_sum            'C21 H32 N O2 P S2'
_chemical_formula_weight         425.56
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-03-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-10-09 deposited with the CCDC.	2025-08-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7130(5)
_cell_length_b                   12.9300(4)
_cell_length_c                   14.0951(5)
_cell_measurement_reflns_used    2372
_cell_measurement_temperature    298
_cell_measurement_theta_max      66.8770
_cell_measurement_theta_min      4.8710
_cell_volume                     2316.94(14)
_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 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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      298
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9974
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_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    -47.00  56.00   1.00    1.00    --   25.57 -57.00  30.00  103
  2  \w    111.00 137.00   1.00    1.50    --   66.78 111.00-120.00   26
  3  \w     62.00 136.00   1.00    1.50    --   66.78  61.00   0.00   74
  4  \w    100.00 136.00   1.00    1.50    --   66.78 111.00  90.00   36
  5  \w     66.00 149.00   1.00    1.50    --   66.78 178.00 -60.00   83
  6  \w    114.00 148.00   1.00    3.50    --  108.00 -54.00  90.00   34
  7  \w     33.00  65.00   1.00    3.50    --  108.00 -54.00  90.00   32
  8  \w     77.00 126.00   1.00    3.50    --  108.00 -65.00-150.00   49
  9  \w     93.00 140.00   1.00    3.50    --  108.00 138.00 150.00   47
 10  \w     39.00  65.00   1.00    3.50    --  108.00 -65.00-150.00   26
 11  \w    102.00 162.00   1.00    3.50    --  108.00 104.00 -60.00   60
 12  \w     91.00 117.00   1.00    3.50    --  108.00  65.00 -30.00   26
 13  \w    130.00 174.00   1.00    3.50    --  108.00  65.00 -30.00   44
 14  \w     88.00 170.00   1.00    3.50    --  108.00  65.00 120.00   82
;
_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      0.0773392000
_diffrn_orient_matrix_UB_12      0.0458199000
_diffrn_orient_matrix_UB_13      0.0728739000
_diffrn_orient_matrix_UB_21      -0.0448101000
_diffrn_orient_matrix_UB_22      -0.0722916000
_diffrn_orient_matrix_UB_23      0.0769886000
_diffrn_orient_matrix_UB_31      0.0817576000
_diffrn_orient_matrix_UB_32      -0.0829029000
_diffrn_orient_matrix_UB_33      -0.0267398000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4832
_diffrn_reflns_point_group_measured_fraction_full 0.825
_diffrn_reflns_point_group_measured_fraction_max 0.825
_diffrn_reflns_theta_full        66.995
_diffrn_reflns_theta_max         66.995
_diffrn_reflns_theta_min         4.878
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.850
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84932
_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_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.211
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details
;
 Flack x determined using 1029 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3408
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0586P)^2^+0.3577P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0956
_refine_ls_wR_factor_ref         0.0988
_reflns_Friedel_coverage         0.493
_reflns_Friedel_fraction_full    0.630
_reflns_Friedel_fraction_max     0.630
_reflns_number_gt                3236
_reflns_number_total             3408
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00611b2.cif
_cod_data_source_block           lr4e_rt_cu
_cod_depositor_comments
'Adding full bibliography for 7250819--7250820.cif.'
_cod_database_code               7250819
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'c h n o p s'
_reflns_odcompleteness_completeness 96.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C16(H16A,H16B), C14(H14A,H14B), C18(H18A,H18B), C20(H20A,H20B)
2.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C4(H4), C9(H9), C6(H6), C3(H3), C7(H7), C13(H13), C12(H12)
2.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C1(H1A,H1B,H1C), C15(H15A,H15B,H15C), C19(H19A,H19B,
 H19C), C21(H21A,H21B,H21C)
;
_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 1.325
_oxdiff_exptl_absorpt_empirical_full_min 0.731