Straightforward synthesis of rubidium bis(trimethylsilyl)amide and complexes of the alkali metal bis(trimethylsilyl)amides with weakly coordinating 2,2,5,5-tetramethyltetrahydrofuran.
Krieck, Sven; Schüler, Philipp; Görls, Helmar; Westerhausen, Matthias; Dalton transactions (Cambridge, England : 2003) 47 (2018) 12562–12569; doi:10.1039/c8dt01539b

data_7046402
_publ_section_title
;
 Straightforward synthesis of rubidium bis(trimethylsilyl)amide and
 complexes of the alkali metal bis(trimethylsilyl)amides with weakly
 coordinating 2,2,5,5-tetramethyltetrahydrofuran.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12562
_journal_page_last               12569
_journal_paper_doi               10.1039/c8dt01539b
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C20 H52 N2 O2 Rb2 Si4'
_chemical_formula_sum            'C20 H52 N2 O2 Rb2 Si4'
_chemical_formula_weight         635.94
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2018-04-18 deposited with the CCDC.
2018-05-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.229(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.1879(2)
_cell_length_b                   12.3031(2)
_cell_length_c                   12.5560(2)
_cell_measurement_reflns_used    12950
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.37
_cell_measurement_theta_min      2.73
_cell_volume                     1667.59(5)
_computing_cell_refinement       DENZO
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_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  0.0274
_diffrn_reflns_av_sigmaI/netI    0.0225
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12950
_diffrn_reflns_theta_full        27.37
_diffrn_reflns_theta_max         27.37
_diffrn_reflns_theta_min         2.73
_exptl_absorpt_coefficient_mu    3.095
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.132
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.102
_refine_diff_density_max         0.847
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         3761
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0258
_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^)+(0.0129P)^2^+1.5434P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0524
_refine_ls_wR_factor_ref         0.0551
_reflns_number_gt                3386
_reflns_number_total             3761
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8dt01539b2.cif
_cod_data_source_block           FO6563
_cod_depositor_comments
'Adding full bibliography for 7046399--7046403.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7046402