Control of the Stereochemical Impact of the Lone Pair in Lead(II) Tris(pyrazolyl)methane Complexes. Improved Preparation of Na{B[3,5-(CF3)2C6H3]4}
Daniel L. Reger; Terri D. Wright; Christine A. Little; Jaydeep J. S. Lamba; Mark D. Smith; Inorganic Chemistry 40 (2001) 3810–3814; doi:10.1021/ic0100121

data_4319980
_publ_section_title
;
 Control of the Stereochemical Impact of the Lone Pair in Lead(II)
 Tris(pyrazolyl)methane Complexes. Improved Preparation of
 Na{B[3,5-(CF3)2C6H3]4}
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3810
_journal_page_last               3814
_journal_paper_doi               10.1021/ic0100121
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C84.7 H45.4 B2 Cl1.4 F48 N12 Pb'
_chemical_formula_weight         2421.57
_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                71.7300(10)
_cell_angle_beta                 82.3630(10)
_cell_angle_gamma                70.5120(10)
_cell_formula_units_Z            2
_cell_length_a                   13.0133(6)
_cell_length_b                   17.2210(7)
_cell_length_c                   24.7634(11)
_cell_measurement_reflns_used    5950
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.5775
_cell_measurement_theta_min      2.452
_cell_volume                     4965.4(4)
_computing_cell_refinement       'SAINT+ NT V6.02a (Bruker, 1998)'
_computing_data_collection       'SMART NT V5.611 (Bruker, 2000)'
_computing_data_reduction        'SAINT+ NT V6.02a'
_computing_molecular_graphics    'SHELXTL V5.1 (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL V5.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega scans'
_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  0.0317
_diffrn_reflns_av_sigmaI/netI    0.0475
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            51219
_diffrn_reflns_theta_full        26.44
_diffrn_reflns_theta_max         26.44
_diffrn_reflns_theta_min         1.66
_diffrn_standards_decay_%        -0.45
_exptl_absorpt_coefficient_mu    1.876
_exptl_absorpt_correction_T_max  0.8644
_exptl_absorpt_correction_T_min  0.5680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelipiped
_exptl_crystal_F_000             2371
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.195
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1298
_refine_ls_number_reflns         20274
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0871
_refine_ls_R_factor_gt           0.0611
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc
  [0.00000+1.00000exp(0.85(sin\q/\l)^2^)]/
    [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.1111P)^2^+0.0000sin\q/\l]
  where P = 0.33333Fo^2^ + 0.66667Fc^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1631
_refine_ls_wR_factor_ref         0.1755
_reflns_number_gt                13186
_reflns_number_total             20274
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010012i_1.cif
_cod_data_source_block           cl209a1t
_cod_original_formula_sum        'C84.70 H45.40 B2 Cl1.40 F48 N12 Pb'
_cod_database_code               4319980