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_7106383
_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            'C29 H41 F N2 Pb'
_chemical_formula_weight         643.83
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 95.906(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.7697(16)
_cell_length_b                   20.465(3)
_cell_length_c                   11.7727(16)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.54
_cell_measurement_theta_min      2.33
_cell_volume                     2820.6(7)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       'Apex2 v2010.11-0'
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker TXS-Mo rotating anode'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'INCOATEC Helios Mirror optics'
_diffrn_radiation_source         'Bruker TXS-Mo rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_sigmaI/netI    0.0183
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            90262
_diffrn_reflns_theta_full        30.62
_diffrn_reflns_theta_max         30.62
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    6.006
_exptl_absorpt_correction_T_max  0.7589
_exptl_absorpt_correction_T_min  0.5022
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SADABS-2008/2
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.121
_refine_diff_density_min         -1.411
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         8667
_refine_ls_number_restraints     715
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0256
_refine_ls_R_factor_gt           0.0210
_refine_ls_shift/su_max          0.147
_refine_ls_shift/su_mean         0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0180P)^2^+3.7248P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0491
_refine_ls_wR_factor_ref         0.0503
_reflns_number_gt                7652
_reflns_number_total             8667
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc11310k.txt
_cod_data_source_block           PbF
_cod_original_cell_volume        2820.7(7)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7106383