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_4334164
_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         'C48 H50 Br2 Pb2 S2, 0.5(C7 H8)'
_chemical_formula_sum            'C51.5 H54 Br2 Pb2 S2'
_chemical_formula_weight         1311.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 92.323(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8927(8)
_cell_length_b                   40.868(4)
_cell_length_c                   13.0063(12)
_cell_measurement_reflns_used    9786
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.50
_cell_volume                     4723.0(8)
_computing_cell_refinement       'SAINT (8.27b) (Bruker, 2012)'
_computing_data_collection       'Apex2 (2010-7) (Bruker, 2010)'
_computing_data_reduction        'SAINT (8.27b) (Bruker, 2012)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXT-2012 (Sheldrick, 2012)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            40295
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.500
_exptl_absorpt_coefficient_mu    8.934
_exptl_absorpt_correction_T_max  0.1191
_exptl_absorpt_correction_T_min  0.0745
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2012/1 (Sheldrick, 2012)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.844
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2516
_exptl_crystal_size_max          0.447
_exptl_crystal_size_mid          0.434
_exptl_crystal_size_min          0.301
_refine_diff_density_max         0.846
_refine_diff_density_min         -0.985
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       0.00016(2)
_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   1.176
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         10796
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.176
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0249
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0020P)^2^+12.6168P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0491
_refine_ls_wR_factor_ref         0.0500
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9881
_reflns_number_total             10796
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic302513c_si_002_3.cif
_cod_data_source_block           BDR102FMI
_cod_original_formula_sum        'C51.50 H54 Br2 Pb2 S2'
_cod_database_code               4334164
_shelx_estimated_absorpt_t_min   0.109
_shelx_estimated_absorpt_t_max   0.174
_shelxl_version_number           2012-6
_shelx_res_checksum              95575