Unusual alkali metal α- or β-phenyl(trimethylsilyl)amides
Antolini, Floria; Hitchcock, Peter B.; Lappert, Michael F.; Merle, Philippe; Chemical Communications  (2000) 1301–; doi:10.1039/b003169k

data_7110982
_publ_section_title
;
 Unusual alkali metal \a- or \b-phenyl(trimethylsilyl)amides
;
_journal_issue                   14
_journal_name_full               'Chemical Communications'
_journal_page_first              1301
_journal_paper_doi               10.1039/b003169k
_journal_year                    2000
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C9 H14 Li1 N1 Si1'
_chemical_formula_structural     'C9 H14 N LI SI'
_chemical_formula_sum            'C36 H56 Li4 N4 Si4'
_chemical_formula_weight         684.97
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_conform_dict_location     ftp://ftp.iucr.org/cifdics/cif_core2.1beta.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1beta3
_audit_creation_date             1999-05-09T13:50:08-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                99.82(3)
_cell_angle_beta                 91.76(3)
_cell_angle_gamma                113.16(3)
_cell_formula_units_Z            2
_cell_length_a                   10.103(4)
_cell_length_b                   10.873(5)
_cell_length_c                   20.223(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      7.6
_cell_measurement_wavelength     0.71073
_cell_volume                     2000.8(15)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_orient_matrix_type
;
  x-axis points to radiation source
  the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      0.37083E-1
_diffrn_orient_matrix_UB_12      -0.45033E-1
_diffrn_orient_matrix_UB_13      -0.37876E-1
_diffrn_orient_matrix_UB_21      -0.36436E-1
_diffrn_orient_matrix_UB_22      0.42772E-1
_diffrn_orient_matrix_UB_23      -0.32282E-1
_diffrn_orient_matrix_UB_31      0.95027E-1
_diffrn_orient_matrix_UB_32      0.81098E-1
_diffrn_orient_matrix_UB_33      0.8641E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_av_sigmaI/netI    0.1182
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            7003
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.06
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        3
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.178
_exptl_absorpt_correction_T_max  0.9653
_exptl_absorpt_correction_T_min  0.9487
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.404
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         7003
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1398
_refine_ls_R_factor_gt           0.0729
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1604
_refine_ls_wR_factor_ref         0.1944
_reflns_number_gt                4136
_reflns_number_total             7003
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b003169ksup1.cif
_cod_data_source_block           B003169K-4
_cod_original_cell_volume        2000.7(14)
_cod_database_code               7110982
_diffrn_standards_decay_corr_max 1.244
_diffrn_standards_decay_corr_min 0.972