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_4334163
_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         'C72 H75 Pb S3 Li, 2(C7 H8)'
_chemical_formula_sum            'C86 H91 Li Pb S3'
_chemical_formula_weight         1434.89
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 108.5190(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.2474(5)
_cell_length_b                   20.2689(7)
_cell_length_c                   13.9860(5)
_cell_measurement_reflns_used    9720
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.53
_cell_volume                     3560.9(2)
_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    '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 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  0.0182
_diffrn_reflns_av_unetI/netI     0.0144
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            31827
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         2.529
_exptl_absorpt_coefficient_mu    2.502
_exptl_absorpt_correction_T_max  0.7920
_exptl_absorpt_correction_T_min  0.4491
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS 2012/1 (Sheldrick, 2012)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_description       Block
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.434
_exptl_crystal_size_mid          0.271
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         8385
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0243
_refine_ls_R_factor_gt           0.0217
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0181P)^2^+2.1401P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0494
_refine_ls_wR_factor_ref         0.0504
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7859
_reflns_number_total             8385
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic302513c_si_002_2.cif
_cod_data_source_block           BDR88FMI
_cod_database_code               4334163
_shelx_estimated_absorpt_t_min   0.410
_shelx_estimated_absorpt_t_max   0.705
_shelxl_version_number           2012-6
_shelx_res_checksum              30134