Carbon Dioxide Activation by "Non-nucleophilic" Lead Alkoxides
Eric C. Y. Tam; Nick C. Johnstone; Lorenzo Ferro; Peter B. Hitchcock; J. Robin Fulton; Inorganic Chemistry 48 (2009) 8971–8976; doi:10.1021/ic900134f

data_4303124
_publ_section_title
;
Carbon Dioxide Activation by "Non-nucleophilic" Lead Alkoxides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8971
_journal_page_last               8976
_journal_paper_doi               10.1021/ic900134f
_journal_volume                  48
_journal_year                    2009
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C33 H50 N2 O Pb'
_chemical_formula_sum            'C33 H50 N2 O Pb'
_chemical_formula_weight         697.94
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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             2006-08-14T15:24:02-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 108.168(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3743(1)
_cell_length_b                   16.8363(2)
_cell_length_c                   15.2434(2)
_cell_measurement_reflns_used    43662
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.682
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     3261.29(7)
_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 0.99
_diffrn_measured_fraction_theta_max 0.99
_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      0.163709E-1
_diffrn_orient_matrix_UB_12      -0.192764E-1
_diffrn_orient_matrix_UB_13      0.650103E-1
_diffrn_orient_matrix_UB_21      0.758656E-1
_diffrn_orient_matrix_UB_22      -0.54234E-2
_diffrn_orient_matrix_UB_23      0.43882E-2
_diffrn_orient_matrix_UB_31      0.130016E-1
_diffrn_orient_matrix_UB_32      0.559181E-1
_diffrn_orient_matrix_UB_33      0.228364E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0606
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            41847
_diffrn_reflns_theta_full        25.82
_diffrn_reflns_theta_max         25.82
_diffrn_reflns_theta_min         3.43
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    5.198
_exptl_absorpt_correction_T_max  0.5941
_exptl_absorpt_correction_T_min  0.4510
_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    1.421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.365
_refine_diff_density_min         -1.395
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         6251
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.033
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+4.2984P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0637
_refine_ls_wR_factor_ref         0.0668
_reflns_number_gt                5497
_reflns_number_total             6251
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900134f_si_002_2.cif
_cod_data_source_block           (3)-aug1006
_cod_original_cell_volume        3261.29(6)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4303124