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_4068106
_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         'C35 H59 Cl N3 Si2 Yb'
_chemical_formula_sum            'C35 H59 Cl N3 Si2 Yb'
_chemical_formula_weight         786.52
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 104.166(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.156(5)
_cell_length_b                   18.248(5)
_cell_length_c                   13.096(4)
_cell_measurement_reflns_used    15796
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     3975(2)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0766
_diffrn_reflns_av_sigmaI/netI    0.1106
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17901
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.14
_exptl_absorpt_coefficient_mu    2.505
_exptl_absorpt_correction_T_max  0.857
_exptl_absorpt_correction_T_min  0.682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            blue-green
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1620
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.913
_refine_diff_density_min         -1.068
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         7373
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.1072
_refine_ls_R_factor_gt           0.0767
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0075P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0967
_refine_ls_wR_factor_ref         0.1046
_reflns_number_gt                5652
_reflns_number_total             7373
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om2010904_si_001.cif
_cod_data_source_block           complex6
_cod_original_cell_volume        3975.3(18)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4068106