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_4333079
_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            'C36 H106 K2 N6 Si12 Yb2'
_chemical_formula_weight         1384.63
_chemical_melting_point          'dec. >150 \%C'
_chemical_name_systematic
; 
1-Trimethylsilyl-4-bis(bis(trimethylsilyl)amido-N)-2,2-dimethyl-3-
potassium-1-aza-2-sila-4-ytterba-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                67.365(13)
_cell_angle_beta                 80.343(14)
_cell_angle_gamma                77.379(14)
_cell_formula_units_Z            2
_cell_length_a                   11.715(2)
_cell_length_b                   16.888(3)
_cell_length_c                   19.192(3)
_cell_measurement_temperature    173(2)
_cell_volume                     3405.1(11)
_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  0.0468
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            16380
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.79
_diffrn_standards_interval_count 298
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    3.091
_exptl_absorpt_correction_T_max  0.4574
_exptl_absorpt_correction_T_min  0.3711
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1420
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.611
_refine_diff_density_min         -1.223
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.166
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     646
_refine_ls_number_reflns         15616
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0456P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.0957
_reflns_number_gt                12470
_reflns_number_total             15616
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0613659sup1.cif
_cod_data_source_block           4
_cod_original_cell_volume        3405.1(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4333079