Formation and Structure of the Oxygen-Centered Lead Thiolate Cluster Pb5O(SRF)8.2C7H8 [RF= 2,4,6-Tris(trifluoromethyl)phenyl]
Frank T. Edelmann; Jan-Karel F. Buijink; Sally A. Brooker; Regine Herbst-Irmer; Ulrike Kilimann; Frank M. Bohnen; Inorganic Chemistry 39 (2000) 6134–6135; doi:10.1021/ic000219e

data_4321676
_publ_section_title
;
 Formation and Structure of the Oxygen-Centered Lead Thiolate Cluster
 Pb5O(SRF)8.2C7H8 [RF= 2,4,6-Tris(trifluoromethyl)phenyl]
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6134
_journal_page_last               6135
_journal_paper_doi               10.1021/ic000219e
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C86 H32 F72 O Pb5 S8'
_chemical_formula_weight         3741.55
_chemical_name_systematic
;
 ?
;
_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                68.200(10)
_cell_angle_beta                 78.210(10)
_cell_angle_gamma                70.810(10)
_cell_formula_units_Z            2
_cell_length_a                   17.385(4)
_cell_length_b                   18.104(5)
_cell_length_c                   20.073(5)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10
_cell_volume                     5516(2)
_computing_cell_refinement       'Stoe DIF4'
_computing_data_collection       'Stoe DIF4'
_computing_data_reduction        'Stoe REDU4'
_computing_molecular_graphics    'Bruker AXS SHELXTL-Plus'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'Stoe-Siemens-AED four-circle-diffractometer'
_diffrn_measurement_method       'Profile data from 2theta/omega'
_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  0.0824
_diffrn_reflns_av_sigmaI/netI    0.0677
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15505
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         4.01
_diffrn_standards_interval_time  90
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.923
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.703
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.253
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismn
_exptl_crystal_F_000             3484
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.287
_refine_diff_density_min         -1.152
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1761
_refine_ls_number_reflns         14311
_refine_ls_number_restraints     13927
_refine_ls_restrained_S_all      0.944
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+44.7634P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0957
_reflns_number_gt                10074
_reflns_number_total             14311
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000219e.cif
_cod_data_source_block           pbs
_cod_database_code               4321676