[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_7109789
_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_formula_moiety         'C28 H34 N4 Pb S2, 2(F6 P), 2(C2 H3 N)'
_chemical_formula_sum            'C32 H40 F12 N6 P2 Pb S2'
_chemical_formula_weight         1069.95
_chemical_name_systematic        ?
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 105.692(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   41.814(8)
_cell_length_b                   8.9420(16)
_cell_length_c                   22.936(5)
_cell_measurement_reflns_used    17463
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      3.1
_cell_volume                     8256(3)
_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0551
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -54
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            43828
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.02
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.352
_exptl_absorpt_correction_T_max  0.3370
_exptl_absorpt_correction_T_min  0.1708
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4208
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.196
_refine_diff_density_min         -0.827
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.174
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         9366
_refine_ls_number_restraints     189
_refine_ls_restrained_S_all      11.349
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+63.4080P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1004
_reflns_number_gt                8847
_reflns_number_total             9366
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc45066j.txt
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7109789