Salt metathesis versus protonolysis routes for the synthesis of silylamide Hauser base (R2NMgX; X = halogen) and amido-Grignard (R2NMgR) complexes.
Goodwin, Conrad A. P.; Smith, Alex; Ortu, Fabrizio; Vitorica-Yrezabal, Iñigo J; Mills, David P.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 6004–6014; doi:10.1039/c5dt02535d

data_7036094
_publ_section_title
;
 Salt metathesis versus protonolysis routes for the synthesis of
 silylamide Hauser base (R2NMgX; X = halogen) and amido-Grignard (R2NMgR)
 complexes.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6004
_journal_page_last               6014
_journal_paper_doi               10.1039/c5dt02535d
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C24 H60 K2 N2 Si4'
_chemical_formula_sum            'C24 H60 K2 N2 Si4'
_chemical_formula_weight         567.30
_chemical_name_systematic        'bis(tertbutyldimethylsilyl)amido potassium'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
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Olex2 1.2
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;
2015-08-03 deposited with the CCDC.
2015-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                90.787(7)
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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_diffrn_measurement_details
;
  1 omega  -41.00   50.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -18.9307   57.0000  -60.0000 91

  2 omega   -8.00   91.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       19.9464   37.0000   90.0000 99

  3 omega  -20.00   24.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -18.9307  -99.0000   60.0000 44

  4 omega  -88.00    3.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -18.9307  -57.0000  150.0000 91
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_diffrn_radiation_monochromator  mirror
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_diffrn_reflns_av_unetI/netI     0.1179
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_diffrn_reflns_number            5521
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.104
_exptl_crystal_description       needle
_exptl_crystal_F_000             312
_exptl_crystal_size_max          0.419
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.095
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_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0411P)^2^] where P=(Fo^2^+2Fc^2^)/3'
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_cod_depositor_comments
'Adding full bibliography for 7036089--7036100.cif.'
_cod_original_cell_volume        853.36(13)
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_manchester_internal_coll_name   adpm123
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_chemical_oxdiff_formula         K(N(SiC6H15)2)
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_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,
 H6B,H6C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,
 H11C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              83964
_olex2_exptl_crystal_mounting_method 'From fomblin on microscope slide.'
_olex2_submission_special_instructions 'No special instructions were received'