Anion driven tetrel bonding dictated supramolecular architectures of lead(ii) with a zwitterionic form of polydentate N′-(piperidine-1-carbonothioyl)picolinohydrazonamide
Mahmoudi, Ghodrat; Garcia-Santos, Isabel; Castiñeiras, Alfonso; Fernández-Vazquez, Roi; Servati Gargari, Masoumeh; Gomila, Rosa M.; Frontera, Antonio; Safin, Damir A.; CrystEngComm 26 (2024) 4357–4366; doi:10.1039/D4CE00582A

data_7249063
_publ_section_title
;
 Anion driven tetrel bonding dictated supramolecular architectures of
 lead(ii) with a zwitterionic form of polydentate
 N&#x2032;-(piperidine-1-carbonothioyl)picolinohydrazonamide
;
_journal_issue                   32
_journal_name_full               CrystEngComm
_journal_page_first              4357
_journal_page_last               4366
_journal_paper_doi               10.1039/D4CE00582A
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety
'C36 H48 Cl N15 O4 Pb3 S3, 2(Cl O4), 3(H2 O), O0.25'
_chemical_formula_sum            'C36 H54 Cl3 N15 O15.25 Pb3 S3'
_chemical_formula_weight         1765.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2019/2
_audit_update_record
;
2024-06-03 deposited with the CCDC.	2024-07-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.1890(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.1389(10)
_cell_length_b                   11.3401(5)
_cell_length_c                   38.3204(19)
_cell_measurement_reflns_used    9864
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      2.16
_cell_volume                     10678.0(8)
_computing_cell_refinement       'APEX4 Software (Bruker, 2021)'
_computing_data_collection       'APEX4 Software (Bruker, 2021)'
_computing_data_reduction        'APEX4 Software (Bruker, 2021)'
_computing_molecular_graphics    'DIAMOND, (Brandenburg, 1999)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON III-14'
_diffrn_measurement_method       'omega and phi'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1140
_diffrn_reflns_av_unetI/netI     0.0632
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            123133
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.166
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    9.782
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    2.196
_exptl_crystal_description       needle
_exptl_crystal_F_000             6736
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.313
_refine_diff_density_min         -1.482
_refine_diff_density_rms         0.218
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     691
_refine_ls_number_reflns         13253
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0060P)^2^+58.5600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0518
_refine_ls_wR_factor_ref         0.0593
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9834
_reflns_number_total             13253
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00582a1.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7249062--7249063.cif.'
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               7249063
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_min   0.640
_shelx_estimated_absorpt_t_max   0.828
_shelx_res_checksum              95540