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_4334165
_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         '4(C60 H74 O2 Pb), 2(C4 H10 O)'
_chemical_formula_sum            'C248 H316 O10 Pb4'
_chemical_formula_weight         4285.75
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                96.326(4)
_cell_angle_beta                 92.024(5)
_cell_angle_gamma                91.391(5)
_cell_formula_units_Z            2
_cell_length_a                   16.8740(14)
_cell_length_b                   19.5017(17)
_cell_length_c                   33.268(3)
_cell_measurement_reflns_used    9632
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.46
_cell_volume                     10869.7(16)
_computing_cell_refinement       'SAINT (8.18C) (Bruker, 2012)'
_computing_data_collection       'Apex2 (2010-11.3) (Bruker, 2010)'
_computing_data_reduction        'SAINT (8.18C) (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 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Duo 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  0.0221
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            97776
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         1.528
_exptl_absorpt_coefficient_mu    3.146
_exptl_absorpt_correction_T_max  0.5397
_exptl_absorpt_correction_T_min  0.4348
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1 (Sheldrick, 2008)'
_exptl_crystal_colour            'Pale Yellow'
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_description       Block
_exptl_crystal_F_000             4424
_exptl_crystal_size_max          0.366
_exptl_crystal_size_mid          0.255
_exptl_crystal_size_min          0.197
_refine_diff_density_max         1.318
_refine_diff_density_min         -1.426
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2479
_refine_ls_number_reflns         49485
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0247
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0267P)^2^+7.9670P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0567
_refine_ls_wR_factor_ref         0.0596
_reflns_Friedel_coverage         0.000
_reflns_number_gt                42395
_reflns_number_total             49485
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic302513c_si_002_4.cif
_cod_data_source_block           BDR162FMI
_cod_original_cell_volume        10869.6(16)
_cod_database_code               4334165
_shelx_estimated_absorpt_t_min   0.392
_shelx_estimated_absorpt_t_max   0.576
_shelxl_version_number           2012-6
_shelx_res_checksum              27787