Homoleptic Tetranuclear Complexes of Divalent Tin and Lead Tetraolates
Zheng Wei; Jen-Hsien Yang; Volodimir D. Vreshch; Alexander V. Zabula; Alexander S. Filatov; Evgeny V. Dikarev; Inorganic Chemistry 50 (2011) 7295–7300; doi:10.1021/ic200890h

data_4325825
_publ_contact_author_address
;
Department of Chemistry
University at Albany
1400 Washington ave
Albany NY 12222
USA
;
_publ_contact_author_email       dikarev@albany.edu
_publ_contact_author_fax         518-442-3462
_publ_contact_author_name
;
Dikarev, Evgeny V. 
;
_publ_contact_author_phone       518-442-4401
_publ_section_title
;
 Homoleptic Tetranuclear Complexes of Divalent Tin and Lead Tetraolates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7295
_journal_page_last               7300
_journal_paper_doi               10.1021/ic200890h
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C10 H4 F12 O8 Pb4, 0.5(C6 H5 Cl)'
_chemical_formula_sum            'C13 H6.5 Cl0.5 F12 O8 Pb4'
_chemical_formula_weight         1365.17
_chemical_name_systematic
; 
 Bis(1,1,1,5,5,5-hexafluoropentane-2,2,4,4-tetraolate)-
 tetralead(II), chlorobenzene adduct
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 93.3870(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.8813(6)
_cell_length_b                   27.3449(16)
_cell_length_c                   15.7652(9)
_cell_measurement_reflns_used    9568
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.34
_cell_volume                     4682.7(5)
_computing_cell_refinement       'SAINT Ver. 6.22  (Bruker-AXS, 2003)'
_computing_data_collection       'SMART Ver. 5.622 (Bruker-AXS, 2003)'
_computing_data_reduction        'SAINT Ver. 6.22'
_computing_molecular_graphics    'SHELXTL Ver. 6.14'
_computing_publication_material  'SHELXTL Ver. 6.14'
_computing_structure_refinement  'SHELXTL Ver. 6.14'
_computing_structure_solution    'SHELXTL Ver. 6.14 (Bruker-AXS, 2003)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       '0.30\% \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_sigmaI/netI    0.0412
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            40393
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.49
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    28.867
_exptl_absorpt_correction_T_max  0.1604
_exptl_absorpt_correction_T_min  0.0521
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS  (Bruker-AXS, 2003)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.873
_exptl_crystal_description       plate
_exptl_crystal_F_000             4744
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.891
_refine_diff_density_min         -1.981
_refine_diff_density_rms         0.294
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     676
_refine_ls_number_reflns         10973
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0331P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0670
_refine_ls_wR_factor_ref         0.0706
_reflns_number_gt                9126
_reflns_number_total             10973
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic200890h_si_001_1.cif
_cod_data_source_block           Pb4(hfpt)2,0.5(C6H5Cl)_(2,0.5(C6H5Cl))
_cod_original_sg_symbol_Hall     '-P 2yn      '
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4325825