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_7036096
_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         'C17 H43 Mg N O2 Si2'
_chemical_formula_sum            'C17 H43 Mg N O2 Si2'
_chemical_formula_weight         374.01
_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
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
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2015-08-03 deposited with the CCDC.
2015-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                87.573(4)
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_cell_formula_units_Z            2
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_cell_measurement_reflns_used    3964
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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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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  -47.00   17.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -57.0000  -30.0000 64

  2 omega  -20.00   57.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -99.0000   60.0000 77

  3 omega  -50.00   37.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -57.0000   90.0000 87

  4 omega   39.00   65.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
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  5 omega   -9.00   34.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
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  6 omega  -11.00   84.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601   77.0000 -150.0000 95
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_diffrn_orient_matrix_UB_33      0.0023446000
_diffrn_radiation_monochromator  mirror
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_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
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Numerical absorption correction based on gaussian integration over
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_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.031
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_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0392P)^2^+0.3726P] where P=(Fo^2^+2Fc^2^)/3'
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'Adding full bibliography for 7036089--7036100.cif.'
_cod_original_cell_volume        1205.13(11)
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_chemical_oxdiff_formula         'C20 N Si2 Mg'
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_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,
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 H17B,H17C)
;
_olex2_submission_special_instructions 'No special instructions were received'