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_7102147
_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            'C38 H66 N3 Pb Si2'
_chemical_formula_weight         828.31
_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                76.037(2)
_cell_angle_beta                 89.319(2)
_cell_angle_gamma                65.115(2)
_cell_formula_units_Z            2
_cell_length_a                   11.9877(7)
_cell_length_b                   12.6789(8)
_cell_length_c                   15.1520(10)
_cell_measurement_temperature    173(2)
_cell_volume                     2016.9(2)
_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  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0662
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            12160
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.88
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.270
_exptl_absorpt_correction_T_max  0.2800
_exptl_absorpt_correction_T_min  0.2800
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             850
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         2.837
_refine_diff_density_min         -2.401
_refine_diff_density_rms         0.223
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         6989
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0586
_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^)+(0.1345P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1674
_refine_ls_wR_factor_ref         0.1809
_reflns_number_gt                5838
_reflns_number_total             6989
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b710888e.txt
_cod_data_source_block           Pb-NTMS2
_cod_database_code               7102147