Semiconductive Nature of Lead-Based Metal‒Organic Frameworks with Three-Dimensionally Extended Sulfur Secondary Building Units
Kamakura, Yoshinobu; Chinapang, Pondchanok; Masaoka, Shigeyuki; Saeki, Akinori; Ogasawara, Kazuyoshi; Nishitani, Shigeto R.; Yoshikawa, Hirofumi; Katayama, Tetsuro; Tamai, Naoto; Sugimoto, Kunihisa; Tanaka, Daisuke; Journal of the American Chemical Society  (2019) –; doi:10.1021/jacs.9b10436

data_4133831
_publ_section_title
;
 Semiconductive Nature of Lead-Based Metal--Organic Frameworks with
 Three-Dimensionally Extended Sulfur Secondary Building Units
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b10436
_journal_year                    2019
_chemical_formula_sum            'C6 N6 Pb3 S6'
_chemical_formula_weight         970.05
_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'
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 127.187(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.162(16)
_cell_length_b                   8.278(7)
_cell_length_c                   13.734(13)
_cell_measurement_reflns_used    2851
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.4932
_cell_measurement_theta_min      3.0198
_cell_volume                     1645(3)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0650
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9418
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.549
_diffrn_reflns_theta_min         3.020
_exptl_absorpt_coefficient_mu    31.386
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.7065
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    3.917
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.336
_refine_diff_density_min         -1.792
_refine_diff_density_rms         0.287
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     96
_refine_ls_number_reflns         1878
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0274
_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^)+(0.0311P)^2^+21.2133P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0658
_refine_ls_wR_factor_ref         0.0666
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1822
_reflns_number_total             1878
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b10436_si_001.cif
_cod_data_source_block           Pb3ttc2
_cod_original_cell_volume        1645(2)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4133831
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              43751
_shelx_hkl_checksum              70695