A new type of heteroleptic complex of divalent lead and synthesis of the P-plumbyleniophosphasilene, R2Si=P‒Pb(L): (L = β-diketiminate)
Yao, Shenglai; Block, Stefan; Brym, Markus; Driess, Matthias; Chemical Communications (Cambridge, United Kingdom)  (2007) 3844–3846; doi:10.1039/b710888e

data_7102148
_publ_section_title
;
 A new type of heteroleptic complex of divalent lead and synthesis of the
 P-plumbyleniophosphasilene, R2Si=P--Pb(L): (L = \b-diketiminate)
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   37
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              3844
_journal_page_last               3846
_journal_paper_doi               10.1039/b710888e
_journal_year                    2007
_chemical_formula_sum            'C35 H59 N2 P Pb Si2'
_chemical_formula_weight         802.18
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                90.1280(10)
_cell_angle_beta                 90.4550(10)
_cell_angle_gamma                109.5890(10)
_cell_formula_units_Z            2
_cell_length_a                   9.5295(3)
_cell_length_b                   10.2387(3)
_cell_length_c                   21.1917(6)
_cell_measurement_temperature    173(2)
_cell_volume                     1947.91(10)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11779
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.96
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.457
_exptl_absorpt_correction_T_max  0.5742
_exptl_absorpt_correction_T_min  0.2336
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.713
_refine_diff_density_min         -1.206
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         6757
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0895P)^2^+3.6958P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1274
_refine_ls_wR_factor_ref         0.1361
_reflns_number_gt                5862
_reflns_number_total             6757
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b710888e.txt
_cod_data_source_block           Pb-PTMS2
_cod_database_code               7102148