Pentafluoropyridine as a fluorinating reagent for preparing a hydrocarbon soluble ?-diketiminatolead(II) monofluoride
Anukul Jana; Sankaranarayana Pillai Sarish; Herbert W. Roesky; Dirk Leusser; Ina Objartel; Dietmar Stalke; Chem.Commun. 47 (2011) 5434–; doi:10.1039/c1cc11310k

data_7106384
_publ_section_title
;
 Pentafluoropyridine as a fluorinating reagent for preparing a hydrocarbon
 soluble ?-diketiminatolead(II) monofluoride
;
_journal_name_full               Chem.Commun.
_journal_page_first              5434
_journal_paper_doi               10.1039/c1cc11310k
_journal_volume                  47
_journal_year                    2011
_chemical_formula_sum            'C74 H92 F6 N4 O2 Pb'
_chemical_formula_weight         1390.71
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 107.0930(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.7060(15)
_cell_length_b                   18.9000(18)
_cell_length_c                   26.336(3)
_cell_measurement_reflns_used    9527
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.37
_cell_measurement_theta_min      2.547
_cell_volume                     7472.4(13)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       'APEX2 v2010.7-0'
_computing_data_reduction        'SAINT V7.68A'
_computing_molecular_graphics    'XSHELL vers. 4.01'
_computing_publication_material  'XSHELL vers. 4.01'
_computing_structure_refinement  'SHELXL in SHELXTL Version 2008/4'
_computing_structure_solution    'SHELXS in SHELXTL Version 2008/4'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart ApexII with D8-Goniometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'INCOAZEC quazer mirror optics'
_diffrn_radiation_source         'INCOTEC Mo micro source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_sigmaI/netI    0.0185
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            166483
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         1.35
_exptl_absorpt_coefficient_mu    2.316
_exptl_absorpt_correction_T_max  0.7921
_exptl_absorpt_correction_T_min  0.6482
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2864
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_platon_squeeze_details
'Highly disordered non-coordinating THF molecules'
_refine_diff_density_max         0.717
_refine_diff_density_min         -1.197
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     804
_refine_ls_number_reflns         14728
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0208
_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^)+(0.0280P)^2^+3.5678P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0522
_refine_ls_wR_factor_ref         0.0543
_reflns_number_gt                13062
_reflns_number_total             14728
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc11310k.txt
_cod_data_source_block           sq
_cod_original_cell_volume        7472.3(12)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7106384