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_4333077
_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            'C21 H63 K N2 Si8 Yb'
_chemical_formula_weight         780.59
_chemical_melting_point          493(3)
_chemical_name_systematic
; 
potassium-tris{bis(trimethylsilylamido)}ytterbate(II)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 115.260(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.048(5)
_cell_length_b                   12.557(2)
_cell_length_c                   17.440(4)
_cell_measurement_temperature    173(2)
_cell_volume                     4168.6(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Siemens P4'
_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  0.0491
_diffrn_reflns_av_sigmaI/netI    0.0591
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            10213
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.06
_diffrn_standards_interval_count 298
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.586
_exptl_absorpt_correction_T_max  0.742
_exptl_absorpt_correction_T_min  0.523
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_diff_density_max         1.518
_refine_diff_density_min         -1.481
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.881
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         9953
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.881
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0302
_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^)+(0.0247P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0677
_refine_ls_wR_factor_ref         0.0707
_reflns_number_gt                7135
_reflns_number_total             9953
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0613659sup1.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '195-245 \%C' was changed to '493(3)'
- it was converted from degrees Celsius(C) to Kelvins(K), the average
value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        4168.4(16)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4333077