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_7031974
_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         'C46 H68 N4 O1 Pb1'
_chemical_formula_sum            'C46 H68 N4 O Pb'
_chemical_formula_weight         900.23
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2n 2ac'
_symmetry_space_group_name_H-M   'P c m n'
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_atom_sites_solution_secondary   difmap
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_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_b                   19.5694(3)
_cell_length_c                   27.4022(4)
_cell_measurement_reflns_used    88724
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_measurement_wavelength     0.71073
_cell_volume                     4990.19(12)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_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
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_diffrn_measured_fraction_theta_max 0.997
_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 Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.68507E-1
_diffrn_orient_matrix_UB_12      -0.232202E-1
_diffrn_orient_matrix_UB_13      0.227051E-1
_diffrn_orient_matrix_UB_21      -0.753614E-1
_diffrn_orient_matrix_UB_22      0.4036E-3
_diffrn_orient_matrix_UB_23      -0.260134E-1
_diffrn_orient_matrix_UB_31      0.342794E-1
_diffrn_orient_matrix_UB_32      -0.45518E-1
_diffrn_orient_matrix_UB_33      -0.118132E-1
_diffrn_radiation_monochromator  graphite
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_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0689
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
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_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            64880
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_diffrn_reflns_theta_max         27.5
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_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    3.413
_exptl_absorpt_correction_T_max  0.8032
_exptl_absorpt_correction_T_min  0.7084
_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    1.198
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rod
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.075
_refine_diff_density_min         -1.758
_refine_diff_density_rms         0.364
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.338
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         5878
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.336
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0588
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0781P)^2^+54.6317P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1951
_refine_ls_wR_factor_ref         0.2115
_reflns_number_gt                5009
_reflns_number_total             5878
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt01714e2.cif
_cod_data_source_block           mpc_lh602
_cod_depositor_comments
'Adding full bibliography for 7031968--7031975.cif.'
_cod_database_code               7031974