Two novel lead(II) complexes of 2-(hydroxymethyl)pyridine: a threefold diamondoid supramolecular network based on Pb~4~O~4~ cores and a two-dimensional (4,4) network based on Pb~2~O~2~ units
Liu, Ting; Pan, Yu-Peng; Wang, Suna; Dou, Jian-Min; Acta Crystallographica Section C 69 (2013) 394–399; doi:10.1107/S0108270113006987

data_2018926
_publ_section_title
;
 Two novel lead(II) complexes of 2-(hydroxymethyl)pyridine: a threefold
 diamondoid supramolecular network based on Pb~4~O~4~ cores and a
 two-dimensional (4,4) network based on Pb~2~O~2~ units
;
_journal_coeditor_code           QS3024
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              394
_journal_page_last               399
_journal_paper_doi               10.1107/S0108270113006987
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Pb4 (C6 H6 N O)4 Cl4]'
_chemical_formula_moiety         'C24 H24 Cl4 N4 O4 Pb4'
_chemical_formula_sum            'C24 H24 Cl4 N4 O4 Pb4'
_chemical_formula_weight         1403.03
_chemical_name_systematic
Tetrakis[\m~3~-(pyridin-2-yl)methanolato]-<i>tetrahedro</i>-tetrakis[chloridolead(II)]
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.373(3)
_cell_length_b                   15.373(3)
_cell_length_c                   13.287(2)
_cell_measurement_reflns_used    2590
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.850
_cell_measurement_theta_min      2.650
_cell_volume                     3140.1(10)
_computing_cell_refinement       'SMART (Bruker, 2006)'
_computing_data_collection       'SMART (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0647
_diffrn_reflns_av_sigmaI/netI    0.0490
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5724
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    21.758
_exptl_absorpt_correction_T_max  0.1506
_exptl_absorpt_correction_T_min  0.0867
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Bruker, 2006)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.968
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2496
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.569
_refine_diff_density_min         -1.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         1374
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0260
_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^)+(0.0179P)^2^+15.1275P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0572
_refine_ls_wR_factor_ref         0.0609
_reflns_number_gt                1111
_reflns_number_total             1374
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            qs3024.cif
_cod_data_source_block           I
_cod_original_cell_volume        3140.2(9)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               2018926
_cod_database_fobs_code          2018926