[Pb(Tab)2(4,4'-bipy)](PF6)2: two-step ambient temperature quantitative solid-state synthesis, structure and dielectric properties
Wang, Fan; Ni, Chun-Yan; Liu, Quan; Li, Fu-Ling; Shi, Jing; Li, Hong-Xi; Lang, Jian-Ping; Chemical Communications (Cambridge, United Kingdom) 49 (2013) 9248–9250; doi:10.1039/c3cc45066j

data_7116512
_publ_section_title
;
 [Pb(Tab)2(4,4'-bipy)](PF6)2: two-step ambient temperature quantitative
 solid-state synthesis, structure and dielectric properties
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   81
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              9248
_journal_page_last               9250
_journal_paper_doi               10.1039/c3cc45066j
_journal_volume                  49
_journal_year                    2013
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C39 H59 N5 O Pb2 S4, 4(F6 P), 2(C2 H3 N)'
_chemical_formula_sum            'C43 H65 F24 N7 O P4 Pb2 S4'
_chemical_formula_weight         1818.52
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.194(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   37.896(6)
_cell_length_b                   12.929(2)
_cell_length_c                   12.973(2)
_cell_measurement_reflns_used    7242
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      3.1
_cell_volume                     6330.1(17)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       /w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0847
_diffrn_reflns_av_sigmaI/netI    0.0840
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            26276
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.12
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.656
_exptl_absorpt_correction_T_max  0.3230
_exptl_absorpt_correction_T_min  0.1325
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.908
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3536
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.782
_refine_diff_density_min         -1.030
_refine_diff_density_rms         0.293
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881, with 5122 Friedel pairs'
_refine_ls_abs_structure_Flack   0.384(13)
_refine_ls_extinction_coef       0.00134(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         11005
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.1003
_refine_ls_R_factor_gt           0.0962
_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^)+(0.1020P)^2^+368.5409P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2331
_refine_ls_wR_factor_ref         0.2359
_reflns_number_gt                10436
_reflns_number_total             11005
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            7109789alt.cif
_cod_data_source_block           1
_cod_original_cell_volume        6330.3(18)
_cod_original_sg_symbol_H-M      C2
_cod_database_code               7116512