Mono-, Di-, and Trianionic β-Diketiminato Ligands: A Computational Study and the Synthesis and Structure of [(YbL)3(THF)], L = [{N(SiMe3)C(Ph)}2CH]
Odile Eisenstein; Peter B. Hitchcock; Alexei V. Khvostov; Michael F. Lappert; Laurent Maron; Lionel Perrin; Andrey V. Protchenko; Journal of the American Chemical Society 125 (2003) 10790–10791; doi:10.1021/ja036902s

data_4114149
_publ_section_title
;
 Mono-, Di-, and Trianionic \b-Diketiminato Ligands: A Computational Study
 and the Synthesis and Structure of [(YbL)3(THF)], L =
 [{N(SiMe3)C(Ph)}2CH]
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10790
_journal_page_last               10791
_journal_paper_doi               10.1021/ja036902s
_journal_volume                  125
_journal_year                    2003
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C67 H95 N6 O Si6 Yb3'
_chemical_formula_sum            'C67 H95 N6 O Si6 Yb3'
_chemical_formula_weight         1688.15
_chemical_name_common            '[Yb3(thf){Me3SiNCPhCHCPhNSiMe3}3]'
_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             2002-02-14T08:17:59-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                65.993(2)
_cell_angle_beta                 84.086(2)
_cell_angle_gamma                86.355(2)
_cell_formula_units_Z            2
_cell_length_a                   13.4823(4)
_cell_length_b                   16.3546(5)
_cell_length_c                   20.0818(6)
_cell_measurement_reflns_used    13654
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      4
_cell_measurement_wavelength     0.71073
_cell_volume                     4022.3(2)
_computing_cell_refinement       'HKL Scalepack'
_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_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_unetI/netI     0.0558
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29430
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         3.73
_exptl_absorpt_coefficient_mu    3.587
_exptl_absorpt_correction_T_max  0.358
_exptl_absorpt_correction_T_min  0.323
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_description       needle
_exptl_crystal_F_000             1682
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.419
_refine_diff_density_min         -0.999
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    'riding mode'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     748
_refine_ls_number_reflns         14142
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0388
_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^)+(0.0465P)^2^+13.9786P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1
_refine_ls_wR_factor_ref         0.1091
_reflns_number_gt                11516
_reflns_number_total             14142
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja036902ssi20030625_055612.cif
_cod_data_source_block           feb602
_cod_database_code               4114149