Stable Plumbylene Dichalcogenolate Monomers with Large Differences in Their Interligand Angles and the Synthesis and Characterization of a Monothiolato Pb(II) Bromide and Lithium Trithiolato Plumbate
Brian D. Rekken; Thomas M. Brown; Marilyn M. Olmstead; James C. Fettinger; Philip P. Power; Inorganic Chemistry 52 (2013) 3054–3062; doi:10.1021/ic302513c

data_4334162
_publ_section_title
;
 Stable Plumbylene Dichalcogenolate Monomers with Large Differences in
 Their Interligand Angles and the Synthesis and Characterization of a
 Monothiolato Pb(II) Bromide and Lithium Trithiolato Plumbate
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3054
_journal_page_last               3062
_journal_paper_doi               10.1021/ic302513c
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C60 H74 Pb S2, 3(C4 H8 O)'
_chemical_formula_sum            'C72 H98 O3 Pb S2'
_chemical_formula_weight         1282.81
_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                 100.779(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.531(4)
_cell_length_b                   16.631(2)
_cell_length_c                   16.071(2)
_cell_measurement_reflns_used    1540
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.82
_cell_volume                     6440.9(15)
_computing_cell_refinement       'SAINT (7.68A) (Bruker, 2009)'
_computing_data_collection       'Apex2 (2010-7) (Bruker, 2010)'
_computing_data_reduction        'SAINT (7.68A) (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD'
_diffrn_measurement_method       '\w and \f'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0645
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7395
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.58
_exptl_absorpt_coefficient_mu    2.730
_exptl_absorpt_correction_T_max  0.6692
_exptl_absorpt_correction_T_min  0.3529
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS V2008/4 (Sheldrick, 2008)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_description       'Oval Plate'
_exptl_crystal_F_000             2672
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.634
_refine_diff_density_min         -0.882
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         7395
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0131P)^2^+6.9927P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0759
_refine_ls_wR_factor_ref         0.0775
_reflns_number_gt                6398
_reflns_number_total             7395
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302513c_si_002_1.cif
_cod_data_source_block           bdr69tw42
_cod_original_cell_volume        6440.8(16)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4334162