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_7010746
_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            'C354 H492 Li12 N24'
_chemical_formula_weight         5166.98
_chemical_name_common            '[NacNacLi]12*hexane'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 112.2750(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   32.8393(11)
_cell_length_b                   16.7836(6)
_cell_length_c                   33.3750(11)
_cell_measurement_reflns_used    5959
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      31.34
_cell_measurement_theta_min      2.63
_cell_volume                     17022.3(10)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    0.1053
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            31158
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.32
_diffrn_standards_decay_%        <0.01
_diffrn_standards_number         '50 frames remeasured'
_exptl_absorpt_coefficient_mu    0.057
_exptl_absorpt_correction_T_max  0.9864
_exptl_absorpt_correction_T_min  0.9725
_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    1.008
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5636
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.951
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       0.00166(18)
_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   0.945
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1775
_refine_ls_number_reflns         31158
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      0.948
_refine_ls_R_factor_all          0.1708
_refine_ls_R_factor_gt           0.0898
_refine_ls_shift/su_max          4.494
_refine_ls_shift/su_mean         0.091
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1780P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2448
_refine_ls_wR_factor_ref         0.2932
_reflns_number_gt                15015
_reflns_number_total             31158
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b103149j.txt
_cod_data_source_block           mas03n
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7010746