A Heterotopically Chelated Low-Valent Lead Amide1
Murso, Alexander; Straka, Michal; Kaupp, Martin; Bertermann, Rüdiger; Stalke, Dietmar; Organometallics 24 (2005) 3576–; doi:10.1021/om0501677

data_4075833
_publ_contact_author             'Prof. Dr. D. Stalke'
_publ_section_title
;
 A Heterotopically Chelated Low-Valent Lead Amide1
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3576
_journal_paper_doi               10.1021/om0501677
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C24 H33 N2 P Pb Si2'
_chemical_formula_weight         643.86
_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                102.425(3)
_cell_angle_beta                 96.536(3)
_cell_angle_gamma                95.131(3)
_cell_formula_units_Z            4
_cell_length_a                   8.5944(15)
_cell_length_b                   17.482(3)
_cell_length_c                   18.411(3)
_cell_measurement_reflns_used    9594
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.50
_cell_measurement_theta_min      2.40
_cell_volume                     2665.3(8)
_computing_cell_refinement       'SAINT-NT V5/6.28'
_computing_data_collection       'SMART-NT V5.6'
_computing_data_reduction        'SAINT-NT V5/6.28'
_computing_molecular_graphics    'XP in SHELXTL-97'
_computing_publication_material  'XP in SHELXTL-97'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_method       omega-scans
_diffrn_radiation_monochromator  'Bruker APEX CCD'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0159
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            73736
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    6.493
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.648136
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS 2.01'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.226
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         13238
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0206
_refine_ls_R_factor_gt           0.0179
_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^)+(0.0185P)^2^+2.1865P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0405
_refine_ls_wR_factor_ref         0.0412
_reflns_number_gt                12281
_reflns_number_total             13243
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0501677si20050309_030025.cif
_cod_data_source_block           compound_zweigelt
_cod_original_cell_volume        2665.2(8)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4075833