Synthesis and theoretical studies on rare three-coordinate lead complexes.
Chen, Matthew; Fulton, J. Robin; Hitchcock, Peter B.; Johnstone, Nick C.; Lappert, Michael F.; Protchenko, Andrey V.; Dalton transactions (Cambridge, England : 2003)  (2007) 2770–2778; doi:10.1039/b702994b

data_7005554
_publ_section_title
;
 Synthesis and theoretical studies on rare three-coordinate lead
 complexes.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2770
_journal_page_last               2778
_journal_paper_doi               10.1039/b702994b
_journal_year                    2007
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C35 H59 N3 Pb1 Si2, 0.5(C6 H6)'
_chemical_formula_sum            'C38 H62 N3 Pb Si2'
_chemical_formula_weight         824.28
_chemical_name_systematic
;
?
;
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2003-10-06T14:21:17-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                97.37
_cell_angle_beta                 100.251(1)
_cell_angle_gamma                115.650(1)
_cell_formula_units_Z            2
_cell_length_a                   11.9346(1)
_cell_length_b                   13.3033(1)
_cell_length_c                   14.6879(2)
_cell_measurement_reflns_used    12023
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     2012.46(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.335227E-1
_diffrn_orient_matrix_UB_12      0.322713E-1
_diffrn_orient_matrix_UB_13      0.702573E-1
_diffrn_orient_matrix_UB_21      0.892339E-1
_diffrn_orient_matrix_UB_22      0.193091E-1
_diffrn_orient_matrix_UB_23      -0.48403E-2
_diffrn_orient_matrix_UB_31      0.136182E-1
_diffrn_orient_matrix_UB_32      0.770218E-1
_diffrn_orient_matrix_UB_33      -0.99108E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21146
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         3.71
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    4.279
_exptl_absorpt_correction_T_max  0.619
_exptl_absorpt_correction_T_min  0.407
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.36
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             842
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.598
_refine_diff_density_min         -1.119
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         6985
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.025
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0224P)^2^+2.6530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0562
_refine_ls_wR_factor_ref         0.0578
_reflns_number_gt                6494
_reflns_number_total             6985
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b702994b.txt
_cod_data_source_block           (5)-oct603
_cod_original_cell_volume        2012.49(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7005554