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_4333078
_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            'C30 H65 K N3 Si6 Y'
_chemical_formula_weight         764.40
_chemical_name_systematic
; 
1-Trimethylsilyl-4-bis(bis(trimethylsilyl)amido-N)-2,2-dimethyl-3-
(bis(\h^6^benzene)-potassium)-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                82.05(3)
_cell_angle_beta                 84.44(3)
_cell_angle_gamma                82.38(3)
_cell_formula_units_Z            2
_cell_length_a                   9.950(4)
_cell_length_b                   11.856(5)
_cell_length_c                   19.285(6)
_cell_measurement_temperature    173(2)
_cell_volume                     2226.1(15)
_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  0.0461
_diffrn_reflns_av_sigmaI/netI    0.0574
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            9287
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        2.5
_diffrn_standards_interval_count 298
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.586
_exptl_absorpt_correction_T_max  0.854
_exptl_absorpt_correction_T_min  0.652
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.140
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         8750
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.181
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0507
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0498P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1047
_refine_ls_wR_factor_ref         0.1188
_reflns_number_gt                6378
_reflns_number_total             8750
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0613659sup1.cif
_cod_data_source_block           3a
_cod_original_cell_volume        2226.1(14)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4333078