Synthesis, spectroscopic findings and crystal engineering of Pb(ii)–Salen coordination polymers, and supramolecular architectures engineered by σ-hole/spodium/tetrel bonds: a combined experimental and theoretical investigation
Majumdar, Dhrubajyoti; Frontera, A.; Gomila, Rosa M.; Das, Sourav; Bankura, Kalipada; RSC Advances 12 (2022) 6352–6363; doi:10.1039/D1RA09346K

data_7244521
_publ_section_title
;
 Synthesis, spectroscopic findings and crystal engineering of
 Pb(ii)--Salen coordination polymers, and supramolecular architectures
 engineered by \s-hole/spodium/tetrel bonds: a combined experimental and
 theoretical investigation
;
_journal_issue                   10
_journal_name_full               'RSC Advances'
_journal_page_first              6352
_journal_page_last               6363
_journal_paper_doi               10.1039/D1RA09346K
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         'C21 H20 Cd N4 O5 Pb S2'
_chemical_formula_sum            'C21 H20 Cd N4 O5 Pb S2'
_chemical_formula_weight         792.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-02-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-05-19 deposited with the CCDC.	2022-01-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.022(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.813(7)
_cell_length_b                   16.798(12)
_cell_length_c                   15.066(11)
_cell_measurement_reflns_used    3299
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      17.41
_cell_measurement_theta_min      2.42
_cell_volume                     2465(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1269
_diffrn_reflns_av_unetI/netI     0.0565
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            59792
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         2.091
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.894
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4800
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.1403 before and 0.0746 after correction. The Ratio of minimum to maximum transmission is 0.6437. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.135
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.078
_exptl_crystal_size_mid          0.054
_exptl_crystal_size_min          0.033
_refine_diff_density_max         0.755
_refine_diff_density_min         -1.466
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         4584
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0538P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.1075
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3356
_reflns_number_total             4584
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra09346k4.cif
_cod_data_source_block           s1
_cod_database_code               7244521
_shelx_shelxl_version_number     2018/1
_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, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C10(H10)
2.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C9(H9A,H9B)
2.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C8(H8), C15(H15), C14(H14), C16(H16), C3(H3), C5(H5), C4(H4)
2.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C19(H19A,H19B,H19C)
2.e Idealised tetrahedral OH refined as rotating group:
 O00A(H00A)
;
_shelx_res_checksum              59794
_olex2_submission_special_instructions 'No special instructions were received'