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_7113243
_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            'C63 H99 N2 P Pb Si2'
_chemical_formula_weight         1178.78
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET)
(compiled Apr 13 2006,12:24:59)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 109.2604(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.4953(2)
_cell_length_b                   18.9054(3)
_cell_length_c                   14.3412(2)
_cell_measurement_reflns_used    14147
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.1715
_cell_measurement_theta_min      3.1155
_cell_volume                     3198.18(9)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET)
(compiled Apr 13 2006,12:24:59)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET)
(compiled Apr 13 2006,12:24:59)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET)
(compiled Apr 13 2006,12:24:59)
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur S Sapphire'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_av_sigmaI/netI    0.0294
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17579
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.13
_exptl_absorpt_coefficient_mu    2.736
_exptl_absorpt_correction_T_max  0.5146
_exptl_absorpt_correction_T_min  0.3303
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
(compiled Aug 28 2006,13:05:05)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       drop
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         5751
_refine_ls_number_restraints     188
_refine_ls_restrained_S_all      1.282
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0219
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0331P)^2^+0.5054P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0558
_refine_ls_wR_factor_ref         0.0616
_reflns_number_gt                5002
_reflns_number_total             5751
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7102149
_cod_data_source_file            b710888e.txt
_cod_data_source_block           block33
_cod_original_cell_volume        3198.18(8)
_cod_original_sg_symbol_H-M      P21/m
_cod_database_code               7113243