Synthesis of molecular lead-pnictogen compounds including [Pb4(SbSiiPr3)6], the first structurally characterised compound with a lead-antimony bond.
Traut, Stephan; von Hänisch, Carsten; Chemical communications (Cambridge, England) 46 (2010) 1538–1540; doi:10.1039/b921473a

data_7105321
_publ_section_title
;
 Synthesis of molecular lead-pnictogen compounds including
 [Pb4(SbSiiPr3)6], the first structurally characterised compound with a
 lead-antimony bond.
;
_journal_issue                   9
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1538
_journal_page_last               1540
_journal_paper_doi               10.1039/b921473a
_journal_volume                  46
_journal_year                    2010
_chemical_formula_sum            'C64 H108 As4 O2 Pb4 Si4'
_chemical_formula_weight         2150.30
_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                66.81(3)
_cell_angle_beta                 71.53(3)
_cell_angle_gamma                81.69(3)
_cell_formula_units_Z            2
_cell_length_a                   14.324(3)
_cell_length_b                   16.404(3)
_cell_length_c                   18.630(4)
_cell_measurement_reflns_used    758
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      26.08
_cell_measurement_theta_min      1.32
_cell_volume                     3815.5(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.930
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_sigmaI/netI    0.0517
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22737
_diffrn_reflns_theta_full        25.64
_diffrn_reflns_theta_max         25.64
_diffrn_reflns_theta_min         1.24
_exptl_absorpt_coefficient_mu    10.619
_exptl_absorpt_correction_T_max  0.6000
_exptl_absorpt_correction_T_min  0.0810
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.872
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.283
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.386
_refine_diff_density_min         -2.817
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.869
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         13420
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.869
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0430
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1208
_reflns_number_gt                11090
_reflns_number_total             13420
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b921473a.txt
_cod_data_source_block           e:\traut\crystal\st128\p-1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7105321