Synthesis of Dianionic β-Diketiminate Lanthanide Amides L′LnN(SiMe3)2(THF) by Deprotonation of the β-Diketiminate Ligand L (L = {[(2,6-iPr2C6H3)NC(CH3)]2CH}−) and the Transformation with [HNEt3][BPh4] to the Cationic Samarium Amide [LSmN(SiMe3)2][BPh4]
Liu, Peng; Zhang, Yong; Yao, Yingming; Shen, Qi; Organometallics 31 (2012) 1017–; doi:10.1021/om2010904

data_4068105
_publ_section_title
;
 Synthesis of Dianionic \b-Diketiminate Lanthanide Amides
 L&#x2032;LnN(SiMe3)2(THF) by Deprotonation of the \b-Diketiminate Ligand
 L (L = {[(2,6-iPr2C6H3)NC(CH3)]2CH}&#x2212;) and the Transformation with
 [HNEt3][BPh4] to the Cationic Samarium Amide [LSmN(SiMe3)2][BPh4]
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              1017
_journal_paper_doi               10.1021/om2010904
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C41 H77 N4 Nd Si4, 0.5(C7 H8)'
_chemical_formula_sum            'C44.5 H81 N4 Nd Si4'
_chemical_formula_weight         928.73
_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_creation_method           SHELXL-97
_cell_angle_alpha                75.163(3)
_cell_angle_beta                 79.407(3)
_cell_angle_gamma                68.293(3)
_cell_formula_units_Z            2
_cell_length_a                   11.7324(3)
_cell_length_b                   11.7814(2)
_cell_length_c                   20.5952(6)
_cell_measurement_reflns_used    12138
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     2544.08(12)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0433
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            21712
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    1.146
_exptl_absorpt_correction_T_max  0.565
_exptl_absorpt_correction_T_min  0.392
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.50
_refine_diff_density_max         1.266
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         9384
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+0.6725P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0793
_reflns_number_gt                8630
_reflns_number_total             9384
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om2010904_si_001.cif
_cod_data_source_block           complex5
_cod_original_cell_volume        2544.08(11)
_cod_original_formula_sum        'C44.50 H81 N4 Nd Si4'
_cod_database_code               4068105