Lead and tin β-diketiminato amido/anilido complexes: competitive nucleophilic reactivity at the β-diketiminato γ-carbon.
Harris, Lisa A.-M.; Tam, Eric C. Y.; Coles, Martyn P.; Fulton, J. Robin; Dalton transactions (Cambridge, England : 2003) 43 (2014) 13803–13814; doi:10.1039/c4dt01714e

data_7032366
_publ_section_title
;
 Lead and tin \b-diketiminato amido/anilido complexes: competitive
 nucleophilic reactivity at the \b-diketiminato \g-carbon.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13803
_journal_page_last               13814
_journal_paper_doi               10.1039/c4dt01714e
_journal_volume                  43
_journal_year                    2014
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C41 H59 N3 Pb1'
_chemical_formula_sum            'C41 H59 N3 Pb'
_chemical_formula_weight         801.1
_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
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_audit_creation_date             2014-03-12T07:59:48-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                100.7430(10)
_cell_angle_beta                 102.6090(10)
_cell_angle_gamma                99.0180(10)
_cell_formula_units_Z            2
_cell_length_a                   9.22380(10)
_cell_length_b                   11.4878(2)
_cell_length_c                   19.2046(3)
_cell_measurement_reflns_used    22842
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     1909.24(5)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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      0.276721E-1
_diffrn_orient_matrix_UB_12      0.280618E-1
_diffrn_orient_matrix_UB_13      0.546023E-1
_diffrn_orient_matrix_UB_21      -0.108929
_diffrn_orient_matrix_UB_22      -0.244568E-1
_diffrn_orient_matrix_UB_23      0.61E-5
_diffrn_orient_matrix_UB_31      0.160407E-1
_diffrn_orient_matrix_UB_32      -0.825364E-1
_diffrn_orient_matrix_UB_33      0.47994E-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  0.0524
_diffrn_reflns_av_unetI/netI     0.0397
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_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
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_diffrn_reflns_limit_l_min       -24
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_diffrn_reflns_theta_max         27.48
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_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    4.449
_exptl_absorpt_correction_T_max  0.6211
_exptl_absorpt_correction_T_min  0.4868
_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    1.393
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needles
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.792
_refine_diff_density_min         -0.915
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         8691
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0248
_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^)+(0.0112P)^2^+2.2486P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0478
_refine_ls_wR_factor_ref         0.0494
_reflns_number_gt                7920
_reflns_number_total             8691
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7031971
_cod_data_source_file            c4dt01714e2.cif
_cod_data_source_block           (5)-jun309
_cod_database_code               7032366