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_4133832
_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 O2 Pb3 S6'
_chemical_formula_weight         1002.05
_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-2018/1
_cell_angle_alpha                90
_cell_angle_beta                 128.277(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.652(3)
_cell_length_b                   8.2402(12)
_cell_length_c                   13.876(2)
_cell_measurement_reflns_used    17097
_cell_measurement_temperature    80(2)
_cell_measurement_theta_max      15.601
_cell_measurement_theta_min      1.621
_cell_volume                     1674.2(5)
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_diffrn_ambient_temperature      80(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'PILATUS3 X CdTe 1M'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.4142
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_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            17097
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        14.390
_diffrn_reflns_theta_max         15.601
_diffrn_reflns_theta_min         1.621
_exptl_absorpt_coefficient_mu    7.627
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    3.976
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.0200
_exptl_crystal_size_mid          0.0200
_exptl_crystal_size_min          0.0100
_refine_diff_density_max         1.299
_refine_diff_density_min         -1.880
_refine_diff_density_rms         0.190
_refine_ls_extinction_coef       0.00060(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         1911
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0158
_refine_ls_R_factor_gt           0.0158
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0113P)^2^+19.0819P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0416
_refine_ls_wR_factor_ref         0.0416
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1911
_reflns_number_total             1911
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b10436_si_001.cif
_cod_data_source_block           Pb3ttc22H2O
_cod_original_cell_volume        1674.1(5)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4133832
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.516
_shelx_estimated_absorpt_t_max   0.516
_shelx_res_checksum              20919
_shelx_hkl_checksum              802