Reactions of Hypersilyl Potassium with Rare-Earth Metal Bis(Trimethylsilylamides): Addition versus Peripheral Deprotonation
Niemeyer, Mark; Inorganic Chemistry 45 (2006) 9085–9095; doi:10.1021/ic0613659

data_4333080
_publ_section_title
;
 Reactions of Hypersilyl Potassium with Rare-Earth Metal
 Bis(Trimethylsilylamides):&#x00A0; Addition versus Peripheral
 Deprotonation
;
_journal_issue                   22
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9085
_journal_page_last               9095
_journal_paper_doi               10.1021/ic0613659
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C24 H69 Li N5 Si6 Y'
_chemical_formula_weight         692.23
_chemical_melting_point          '295-297 \%C (dec.) '
_chemical_name_systematic
; 
1-Trimethylsilyl-4-bis(bis(trimethylsilyl)amido-N)-2,2-dimethyl-3-
(bis(tetramethylethylenediamine-N,N'-lithium)-1-aza-2-sila-4-
yttra-cyclobutane
;
_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                93.53(2)
_cell_angle_beta                 99.65(2)
_cell_angle_gamma                100.15(2)
_cell_formula_units_Z            2
_cell_length_a                   12.265(4)
_cell_length_b                   13.418(5)
_cell_length_c                   13.450(5)
_cell_measurement_temperature    173(2)
_cell_volume                     2138.5(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Siemens P3'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_av_sigmaI/netI    0.0573
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9764
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         1.55
_diffrn_standards_interval_count 298
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.551
_exptl_absorpt_correction_T_max  0.5421
_exptl_absorpt_correction_T_min  0.3893
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.075
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.70
_exptl_crystal_size_min          0.45
_refine_diff_density_max         0.675
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         9324
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.198
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0532
_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^)+(0.0521P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1257
_reflns_number_gt                6926
_reflns_number_total             9324
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0613659sup1.cif
_cod_data_source_block           6
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4333080