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_7010744
_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            'C29 H39.5 Li N2'
_chemical_formula_weight         423.07
_chemical_name_common            (NacNacLi)2
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.765(3)
_cell_angle_beta                 91.189(3)
_cell_angle_gamma                102.979(3)
_cell_formula_units_Z            4
_cell_length_a                   12.4708(14)
_cell_length_b                   14.0455(16)
_cell_length_c                   15.1235(17)
_cell_measurement_reflns_used    2313
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.19
_cell_measurement_theta_min      2.38
_cell_volume                     2580.3(5)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0872
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9315
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.49
_diffrn_standards_decay_%        <0.01
_diffrn_standards_number         '50 frames remeasured'
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_T_max  0.9895
_exptl_absorpt_correction_T_min  0.9865
_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    1.089
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             922
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       0.0118(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     591
_refine_ls_number_reflns         9315
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1546
_refine_ls_R_factor_gt           0.0769
_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^)+(0.1223P)^2^+0.1214P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1956
_refine_ls_wR_factor_ref         0.2406
_reflns_number_gt                4630
_reflns_number_total             9315
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b103149j.txt
_cod_data_source_block           be46
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C29 H39.50 Li N2'
_cod_database_code               7010744