The synthesis and structure of lithium derivatives of the sterically encumbered β-diketiminate ligand [{(2,6-Pri2H3C6)N(CH3)C}2CH]–, and a modified synthesis of the aminoimine precursor
Stender, Matthias; Wright, Robert J.; Eichler, Barrett E.; Prust, Jörg; Olmstead, Marilyn M.; Roesky, Herbert W.; Power, Philip P.; Journal of the Chemical Society, Dalton Transactions  (2001) 3465–; doi:10.1039/b103149j

data_7010743
_publ_section_title
;
 The synthesis and structure of lithium derivatives of the sterically
 encumbered \b-diketiminate ligand [{(2,6-Pri2H3C6)N(CH3)C}2CH]--, and
 a modified synthesis of the aminoimine precursor
;
_journal_issue                   23
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3465
_journal_paper_doi               10.1039/b103149j
_journal_year                    2001
_chemical_formula_sum            'C33 H49 Li N2 O'
_chemical_formula_weight         496.68
_chemical_name_common            NacNacLi.THF
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.499(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.936(5)
_cell_length_b                   14.757(5)
_cell_length_c                   15.720(5)
_cell_measurement_reflns_used    415
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      23.39
_cell_measurement_theta_min      2.21
_cell_volume                     3099.8(18)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL v. 5.10'
_computing_molecular_graphics    'XP, Bruker SHELXTL v. 5.10'
_computing_publication_material  'XCIF, Bruker SHELXTL v. 5.10'
_computing_structure_refinement  'XL, Bruker SHELXTL v. 5.10'
_computing_structure_solution    'XS, Bruker SHELXTL v. 5.10'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       /w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0872
_diffrn_reflns_av_sigmaI/netI    0.0739
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            20948
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.06
_diffrn_standards_decay_%        <0.01
_diffrn_standards_number         '50 frames remeasured'
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_T_max  0.9858
_exptl_absorpt_correction_T_min  0.9779
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS: an empirical absorption program by G. M. Sheldrick
using the method described by Blessing, R. H.; Acta Cryst.
A51, 1995, 33.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.064
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.889
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         4513
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1356
_refine_ls_R_factor_gt           0.0750
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0894P)^2^+6.0603P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1772
_refine_ls_wR_factor_ref         0.2159
_reflns_number_gt                2707
_reflns_number_total             4513
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b103149j.txt
_cod_data_source_block           be45
_cod_original_cell_volume        3099.7(19)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7010743