Polylithiated Tetraaminosilanes: Synthesis and Characterization of (Et2O.Li)4[Si(Nnaph)4] and X-ray Structure of {THF.Li3[Si(NiPr)3(NHiPr)]}2
Justin K. Brask; Tristram Chivers; Masood Parvez; Inorganic Chemistry 39 (2000) 2505–2508; doi:10.1021/ic991238v

data_4321028
_publ_section_title
;
 Polylithiated Tetraaminosilanes: Synthesis and Characterization of
 (Et2O.Li)4[Si(Nnaph)4] and X-ray Structure of
 {THF.Li3[Si(NiPr)3(NHiPr)]}2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2505
_journal_page_last               2508
_journal_paper_doi               10.1021/ic991238v
_journal_volume                  39
_journal_year                    2000
_chemical_compound_source        'synthesized by authors'
_chemical_formula_moiety         'C16 H37 Li3 N4 O Si '
_chemical_formula_sum            'C16 H37 Li3 N4 O Si'
_chemical_formula_weight         350.40
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_date             1999-10-12
_audit_creation_method           'by teXsan v1.7'
_cell_angle_alpha                90
_cell_angle_beta                 93.22(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.661(7)
_cell_length_b                   16.964(5)
_cell_length_c                   12.405(4)
_cell_measurement_reflns_used    16
_cell_measurement_temperature    170(1)
_cell_measurement_theta_max      13.3
_cell_measurement_theta_min      10.2
_cell_volume                     2239.9(18)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1995)'
_computing_publication_material  'teXsan (MSC, 1995)'
_computing_structure_refinement  'teXsan (MSC, 1995)'
_computing_structure_solution    'Direcdt methods'
_diffrn_ambient_temperature      170(1)
_diffrn_measurement_device       'Rigaku AFC6S'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.01357
_diffrn_orient_matrix_UB_12      -0.00910
_diffrn_orient_matrix_UB_13      0.07945
_diffrn_orient_matrix_UB_21      0.05968
_diffrn_orient_matrix_UB_22      0.04548
_diffrn_orient_matrix_UB_23      0.00515
_diffrn_orient_matrix_UB_31      -0.07128
_diffrn_orient_matrix_UB_32      0.03639
_diffrn_orient_matrix_UB_33      0.01345
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
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_diffrn_reflns_av_sigmaI/netI    0.170
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_diffrn_reflns_limit_k_min       0
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_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5618
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         2.59
_diffrn_standards_decay_%        0.93
_diffrn_standards_interval_count 200
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_exptl_absorpt_correction_type   '\y scans (North,Phillips & Matthews, 1968)'
_exptl_crystal_colour            colorless
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_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
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_refine_diff_density_min         -0.19
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_refine_ls_goodness_of_fit_all   2.319
_refine_ls_goodness_of_fit_obs   2.319
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_refine_ls_number_restraints     0
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_refine_ls_R_factor_obs          0.0614
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_refine_ls_shift/esd_mean        0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00010|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0611
_refine_ls_wR_factor_obs         0.0611
_reflns_number_observed          1351
_reflns_number_total             5340
_reflns_observed_criterion       >3.00\s(I)
_cod_data_source_file            ic991238v.cif
_cod_data_source_block           Justin-10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(Fo) +
0.00010|Fo|^2^]' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w = 1/[\s^2^(Fo) + 0.00010|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2239.9(15)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C16 H37 Li3 N4 O Si '
_cod_database_code               4321028