Syntheses and structures of [(Me3N)3SiNHLi]4, (C4H8O)Al[NHSi(NMe2)3]3, ((Me2N)3SiNH)3Al and Li(THF)2+[((Me2N)3SiNH)4Al]–
Bradley, John S.; Cheng, Fei; Archibald, Stephen J.; Supplit, Ralf; Rovai, Riccardo; Lehmann, Christian W.; Krüger, Carl; Lefebvre, Frédéric; Dalton Transactions  (2003) 1846–; doi:10.1039/b209605f

data_7012283
_publ_section_title
;
 Syntheses and structures of [(Me3N)3SiNHLi]4, (C4H8O)Al[NHSi(NMe2)3]3,
 ((Me2N)3SiNH)3Al and Li(THF)2+[((Me2N)3SiNH)4Al]--
;
_journal_issue                   9
_journal_name_full               'Dalton Transactions'
_journal_page_first              1846
_journal_paper_doi               10.1039/b209605f
_journal_year                    2003
_chemical_compound_source        'see paper'
_chemical_formula_sum            'C32 H92 Al Li N16 O2 Si4'
_chemical_formula_weight         879.50
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 105.3130(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.2318(4)
_cell_length_b                   21.7844(9)
_cell_length_c                   20.2211(6)
_cell_measurement_reflns_used    7460
_cell_measurement_temperature    173
_cell_volume                     5196.9(3)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'XPREP (Siemens, 1995)'
_computing_molecular_graphics    'XP (Siemens, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.871
_diffrn_measured_fraction_theta_max 0.871
_diffrn_measurement_device_type  SMART-CCD
_diffrn_measurement_method       \w-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  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0324
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            27683
_diffrn_reflns_theta_full        33.79
_diffrn_reflns_theta_max         33.79
_diffrn_reflns_theta_min         1.87
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.175
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.53
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS, Sheldrick, G.W. (1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.124
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.648
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         9089
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0407
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0656P)^2^+2.0013P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1083
_refine_ls_wR_factor_ref         0.1175
_reflns_number_gt                7103
_reflns_number_total             9089
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b209605f.txt
_cod_data_source_block           3160
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C32 H92 Al1 Li1 N16 O2 Si4'
_cod_database_code               7012283