Agostic-Type B−H···Pb Interactions Stabilize a Dialkylplumbylene. Structure of and Bonding in [{nPr2P(BH3)}(Me3Si)C(CH2)]2Pb
Izod, Keith; McFarlane, William; Wills, Corinne; Clegg, William; Harrington, Ross W.; Organometallics 27 (2008) 4386–; doi:10.1021/om800598b

data_4072117
_publ_section_title
;
 Agostic-Type B&#x2212;H&#x00B7;&#x00B7;&#x00B7;Pb Interactions Stabilize
 a Dialkylplumbylene. Structure of and Bonding in
 [{nPr2P(BH3)}(Me3Si)C(CH2)]2Pb
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4386
_journal_paper_doi               10.1021/om800598b
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C22 H56 B2 P2 Pb Si2'
_chemical_formula_sum            'C22 H56 B2 P2 Pb Si2'
_chemical_formula_weight         667.60
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.796(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.4175(8)
_cell_length_b                   17.6207(13)
_cell_length_c                   16.6197(12)
_cell_measurement_reflns_used    8991
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.70
_cell_measurement_theta_min      2.50
_cell_volume                     3201.0(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker APEX2 CCD diffractometer'
_diffrn_measurement_method       'thin-slice \w scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6895
_diffrn_reflns_av_R_equivalents  0.0601
_diffrn_reflns_av_sigmaI/netI    0.0590
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33323
_diffrn_reflns_theta_full        29.50
_diffrn_reflns_theta_max         29.50
_diffrn_reflns_theta_min         2.47
_diffrn_standards_decay_%        5
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.453
_exptl_absorpt_correction_T_max  0.811
_exptl_absorpt_correction_T_min  0.612
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.559
_refine_diff_density_min         -1.430
_refine_diff_density_rms         0.166
_refine_ls_extinction_coef       0.00040(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         9462
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0437
_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^)+(0.0001P)^2^+15.4942P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.0929
_reflns_number_gt                8084
_reflns_number_total             9462
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om800598b_si_002.cif
_cod_data_source_block           ki297_rac-10
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4072117