Pb⋯X (X = N, S, I) tetrel bonding interactions in Pb(ii) complexes: X-ray characterization, Hirshfeld surfaces and DFT calculations
Mahmoudi, Ghodrat; Seth, Saikat Kumar; Bauzá, Antonio; Zubkov, Fedor I.; Gurbanov, Atash V.; White, Jonathan; Stilinović, Vladimir; Doert, Thomas; Frontera, Antonio; CrystEngComm 20 (2018) 2812–; doi:10.1039/C8CE00110C

data_1549180
_publ_section_title
;
 Pb&#x22EF;X (X = N, S, I) tetrel bonding interactions in Pb(ii)
 complexes: X-ray characterization, Hirshfeld surfaces and DFT
 calculations
;
_journal_issue                   20
_journal_name_full               CrystEngComm
_journal_page_first              2812
_journal_paper_doi               10.1039/C8CE00110C
_journal_volume                  20
_journal_year                    2018
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C28 H24 N8 O6 Pb2'
_chemical_formula_sum            'C28 H24 N8 O6 Pb2'
_chemical_formula_weight         982.95
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-02-23 deposited with the CCDC.
2018-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.218(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.4785(2)
_cell_length_b                   21.4405(5)
_cell_length_c                   9.0220(2)
_cell_measurement_reflns_used    17979
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.4958
_cell_measurement_theta_min      2.8444
_cell_measurement_wavelength     0.71073
_cell_volume                     1442.69(6)
_computing_cell_refinement
'CrysAlis Pro (Oxford Diffraction Ltd., 2010)'
_computing_data_collection
'CrysAlis Pro (Oxford Diffraction Ltd., 2010)'
_computing_data_reduction
'CrysAlis Pro (Oxford Diffraction Ltd., 2010)'
_computing_molecular_graphics    'Diamond v.3.2f (Crystal Impact GbR, 2008)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare et al, 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.3504
_diffrn_detector_type            'Sapphire2 (large Be window)'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega -109.00    3.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.9916  -77.0000  -90.0000 112

  2 omega -113.00  -40.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.9916  -77.0000  150.0000 73

  3 omega   -8.00   66.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       30.9291  -77.0000   30.0000 74

  4 omega    4.00   30.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.9916   77.0000   60.0000 26

  5 omega  -69.00  -44.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.9916   77.0000   60.0000 25

  6 omega  -29.00   34.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.9916   77.0000  -30.0000 63

  7 omega  -20.00    6.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.9916  -77.0000 -180.0000 26

  8 omega   -9.00  107.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       30.9291   77.0000 -180.0000 116

  9 omega  -23.00   63.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.9916   77.0000 -120.0000 86

 10 omega -115.00    9.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.9916  -77.0000   30.0000 124

 11 omega  -44.00  -19.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       30.9291  -77.0000 -120.0000 25

 12 omega   12.00   68.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       30.9291  -77.0000 -120.0000 56

 13 omega  -46.00   72.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       30.9291  -84.0000  156.0000 118

;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur 2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0476067
_diffrn_orient_matrix_UB_12      -0.0264773
_diffrn_orient_matrix_UB_13      -0.0228325
_diffrn_orient_matrix_UB_21      -0.0725015
_diffrn_orient_matrix_UB_22      -0.019463
_diffrn_orient_matrix_UB_23      0.0169869
_diffrn_orient_matrix_UB_31      -0.0390462
_diffrn_orient_matrix_UB_32      0.0037259
_diffrn_orient_matrix_UB_33      -0.0735308
_diffrn_radiation_collimation    '0.5 mm'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Enhance (Mo) X-ray Source, sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            29921
_diffrn_reflns_theta_full        31
_diffrn_reflns_theta_max         31
_diffrn_reflns_theta_min         2.89
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    11.713
_exptl_absorpt_correction_T_max  0.364
_exptl_absorpt_correction_T_min  0.09
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
        (compiled Apr 28 2010,14:27:37)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'Light yellow'
_exptl_crystal_density_diffrn    2.263
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.719
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         4582
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0226
_refine_ls_R_factor_gt           0.0180
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0263P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0423
_refine_ls_wR_factor_ref         0.0430
_reflns_number_gt                3991
_reflns_number_total             4582
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c8ce00110c2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 1549180--1549183.cif.'
_cod_database_code               1549180
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              34769