The synthesis of monomeric terminal lead aryloxides: dependence on reagents and conditions.
Fulton, J. Robin; Hitchcock, Peter B.; Johnstone, Nick C.; Tam, Eric C. Y.; Dalton transactions (Cambridge, England : 2003)  (2007) 3360–3362; doi:10.1039/b707984b

data_7005990
_publ_section_title
;
 The synthesis of monomeric terminal lead aryloxides: dependence on
 reagents and conditions.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3360
_journal_page_last               3362
_journal_paper_doi               10.1039/b707984b
_journal_year                    2007
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C88 H128 Cl2 Li2 N4 O2 Pb2, 6(C6 D6)'
_chemical_formula_sum            'C124 H128 Cl2 D36 Li2 N4 O2 Pb2'
_chemical_formula_weight         2277.8
_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      2.3
_audit_creation_date             2006-07-26T09:52:11-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                99.340(1)
_cell_angle_beta                 102.769(1)
_cell_angle_gamma                105.893(1)
_cell_formula_units_Z            1
_cell_length_a                   12.2848(2)
_cell_length_b                   14.8940(4)
_cell_length_c                   17.3448(4)
_cell_measurement_reflns_used    47522
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     2891.57(12)
_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-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_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      0.383046E-1
_diffrn_orient_matrix_UB_12      0.638724E-1
_diffrn_orient_matrix_UB_13      0.397306E-1
_diffrn_orient_matrix_UB_21      0.789552E-1
_diffrn_orient_matrix_UB_22      -0.85409E-2
_diffrn_orient_matrix_UB_23      0.46033E-2
_diffrn_orient_matrix_UB_31      0.83847E-2
_diffrn_orient_matrix_UB_32      0.318157E-1
_diffrn_orient_matrix_UB_33      -0.458695E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            40829
_diffrn_reflns_theta_full        26.34
_diffrn_reflns_theta_max         26.34
_diffrn_reflns_theta_min         3.59
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    3.00
_exptl_absorpt_correction_T_max  0.7711
_exptl_absorpt_correction_T_min  0.572
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1156
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.223
_refine_diff_density_min         -0.905
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         11385
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.042
_refine_ls_R_factor_gt           0.0348
_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^)+(0.0290P)^2^+5.4675P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0845
_reflns_number_gt                10266
_reflns_number_total             11385
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b707984b.txt
_cod_data_source_block           (2)-jul1006
_cod_original_cell_volume        2891.57(11)
_cod_database_code               7005990