Crystal structure of poly[tetra-(μ4-naphthalene-1,8-dicarboxylato-κ4 O:O,O′: O′′:O′′,O′′′)-(μ4-oxo-κ4 O:O:O:O) penta-lead(II)], C48H24O17Pb5
Zhou, Fang-Xia; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 575–577; doi:10.1515/ncrs-2019-0824

data_8105223
_publ_section_title
;
 Crystal structure of poly[tetra-(\m4-naphthalene-1,8-dicarboxylato-\k4
 O:O,O&#x2032;:
 O&#x2032;&#x2032;:O&#x2032;&#x2032;,O&#x2032;&#x2032;&#x2032;)-(\m4-oxo-\k4
 O:O:O:O) penta-lead(II)], C48H24O17Pb5
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              575
_journal_page_last               577
_journal_paper_doi               10.1515/ncrs-2019-0824
_journal_volume                  235
_journal_year                    2020
_chemical_absolute_configuration .
_chemical_formula_sum            'C48 H24 O17 Pb5'
_chemical_formula_weight         1908.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     SHELXT
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 115.7300(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.8455(6)
_cell_length_b                   9.4617(2)
_cell_length_c                   21.0940(5)
_cell_measurement_reflns_used    852
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.01
_cell_measurement_theta_min      2.47
_cell_volume                     4287.33(18)
_computing_cell_refinement       'SMART Apex2 [8]'
_computing_data_collection       'SMART Apex2 [8]'
_computing_data_reduction        'SMART Apex2 [8]'
_computing_molecular_graphics    'SHELXL-2017/1 [9]'
_computing_publication_material  'SHELXL-2017/1 [9]'
_computing_structure_refinement  'SHELXL-2017/1 [9]'
_computing_structure_solution    'SHELXT  [9]'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker Smart Apex2 CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13438
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.201
_diffrn_reflns_theta_min         1.896
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    19.650
_exptl_absorpt_correction_T_max  0.619
_exptl_absorpt_correction_T_min  0.287
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.957
_exptl_crystal_description       block
_exptl_crystal_F_000             3432
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.389
_refine_diff_density_min         -1.483
_refine_diff_density_rms         0.227
_refine_ls_abs_structure_details
;
.
;
_refine_ls_abs_structure_Flack   .
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         5147
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0290
_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^)+(0.0216P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0541
_refine_ls_wR_factor_ref         0.0580
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4118
_reflns_number_total             5147
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2019-0824_suppl.cif
_cod_data_source_block           C48H24O17Pb5
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               8105223
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.111
_shelx_estimated_absorpt_t_max   0.440