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_7010745
_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 H42 N2'
_chemical_formula_weight         418.65
_chemical_name_common            NacNacH
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 97.40(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.053(5)
_cell_length_b                   17.944(6)
_cell_length_c                   20.034(5)
_cell_measurement_reflns_used    29
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.89
_cell_measurement_theta_min      4.91
_cell_volume                     5366(3)
_computing_cell_refinement       'Siemens P3'
_computing_data_collection       'Siemens P3'
_computing_data_reduction        'Siemens XDISK'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       2\q-\w
_diffrn_radiation_monochromator  'nickel filter'
_diffrn_radiation_source         'Siemens Cu rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0204
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7786
_diffrn_reflns_theta_full        56.44
_diffrn_reflns_theta_max         56.44
_diffrn_reflns_theta_min         3.32
_diffrn_standards_decay_%        <0.01
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.444
_exptl_absorpt_correction_T_max  0.9653
_exptl_absorpt_correction_T_min  0.8932
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
XABS2: an empirical absorption correction program.  Parkin, S.; 
Moezzi, B.; Hope, H. J. Appl. Cryst. 1995, 28, 53-56.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.036
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.215
_refine_diff_density_min         -0.200
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         7091
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.0628
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0653P)^2^+4.6853P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1489
_refine_ls_wR_factor_ref         0.1659
_reflns_number_gt                5195
_reflns_number_total             7091
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b103149j.txt
_cod_data_source_block           be49
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7010745