Bis[<i>O</i>,<i>O</i>'-bis(4-<i>tert</i>-butylphenyl) dithiophosphato-κ^2^<i>S</i>,<i>S</i>']bis(pyridine-κ<i>N</i>)lead(II)
Zhang, Xiulan; Xie, Bin; He, Linxin; Lu, Lu; Chen, Neng; Acta Crystallographica Section E 69 (2013) m524–; doi:10.1107/S1600536813023945

data_2238496
_publ_section_title
;
 Bis[<i>O</i>,<i>O</i>'-bis(4-<i>tert</i>-butylphenyl)
 dithiophosphato-\k^2^<i>S</i>,<i>S</i>']bis(pyridine-\k<i>N</i>)lead(II)
;
_journal_coeditor_code           HB7129
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m524
_journal_paper_doi               10.1107/S1600536813023945
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Pb (C20 H26 O2 P S2)2 (C5 H5 N)2]'
_chemical_formula_moiety         'C50 H62 N2 O4 P2 Pb S4'
_chemical_formula_sum            'C50 H62 N2 O4 P2 Pb S4'
_chemical_formula_weight         1152.39
_chemical_name_systematic
'Bis[<i>O</i>,<i>O</i>'-bis(4-<i>tert</i>-butylphenyl) dithiophosphato-\k^2^<i>S</i>,<i>S</i>']bis(pyridine-\k<i>N</i>)lead(II)'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.7528(18)
_cell_angle_beta                 79.4467(19)
_cell_angle_gamma                71.298(2)
_cell_formula_units_Z            2
_cell_length_a                   12.4260(3)
_cell_length_b                   12.9136(3)
_cell_length_c                   17.9749(4)
_cell_measurement_reflns_used    10707
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.21
_cell_measurement_theta_min      2.86
_cell_volume                     2681.23(11)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_sigmaI/netI    0.0516
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22556
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.86
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.404
_exptl_absorpt_correction_T_max  0.5493
_exptl_absorpt_correction_T_min  0.4833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.801
_refine_diff_density_min         -0.688
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     663
_refine_ls_number_reflns         10953
_refine_ls_number_restraints     572
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0328
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+0.8500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0619
_refine_ls_wR_factor_ref         0.0675
_reflns_number_gt                9252
_reflns_number_total             10953
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb7129.cif
_cod_data_source_block           I
_cod_original_cell_volume        2681.22(10)
_cod_database_code               2238496
_cod_database_fobs_code          2238496