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_7036091
_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         'C44 H100 Cl2 Mg2 N2 O2 Si4'
_chemical_formula_sum            'C44 H100 Cl2 Mg2 N2 O2 Si4'
_chemical_formula_weight         921.13
_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
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_atom_sites_solution_hydrogens   geom
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Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
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2015-08-03 deposited with the CCDC.
2015-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
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_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.7375(3)
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_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
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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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_computing_data_reduction
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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)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_diffrn_measurement_details
;
  1 omega  111.71  248.71   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   73.8669  109.2094 137

  2 phi    -25.79  333.43   1.0006   10.0000
omega____ theta____ kappa____ phi______ frames
 106.1694   95.0000   73.8669     -     359

  3 phi     -6.71  171.40   1.0006   10.0000
omega____ theta____ kappa____ phi______ frames
 154.7097   15.0000   73.8669     -     178

  4 phi     24.86  220.98   1.0006   10.0000
omega____ theta____ kappa____ phi______ frames
 204.2097  111.0000   73.8669     -     196

  5 phi   -203.07   15.06   1.0006   10.0000
omega____ theta____ kappa____ phi______ frames
 124.9794  100.5000   73.8669     -     218

  6 omega  260.75  333.75   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -70.0000   73.8669    4.2094 73

  7 phi    185.71  332.80   1.0006   10.0000
omega____ theta____ kappa____ phi______ frames
  45.0897  -70.0000   73.8669     -     147

  8 phi    -25.79  123.30   1.0006   10.0000
omega____ theta____ kappa____ phi______ frames
 239.2097  113.0000   73.8669     -     149

  9 phi     95.07  316.21   1.0006   10.0000
omega____ theta____ kappa____ phi______ frames
 136.8394   95.0000   73.8669     -     221

 10 phi   -205.79   -3.66   1.0006   10.0000
omega____ theta____ kappa____ phi______ frames
  91.3697   93.0000   73.8669     -     202
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'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
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_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
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_diffrn_reflns_av_unetI/netI     0.0230
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_diffrn_reflns_limit_l_max       24
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_diffrn_reflns_number            7000
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_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         4.157
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.394
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71550
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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.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.125
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0692P)^2^+3.9641P] where P=(Fo^2^+2Fc^2^)/3'
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_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02535d2.cif
_cod_data_source_block           03
_cod_depositor_comments
'Adding full bibliography for 7036089--7036100.cif.'
_cod_original_cell_volume        2719.68(14)
_cod_database_code               7036091
_manchester_internal_coll_name   xdpm23
_manchester_internal_coll_client FO/DPM
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_manchester_internal_coll_user   FO
_manchester_internal_coll_date   15/10/2014
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_manchester_internal_process_date 16/10/2014
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_manchester_internal_solution_date 16/10/2014
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_manchester_internal_validation_user IVY
_manchester_internal_validation_date 24/04/2015
_manchester_internal_archive_date 24/04/2015
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         '"C44 H100 Cl2 Mg2 N2 O2 Si4'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C4(H4), C7(H7), C10(H10), C13(H13), C16(H16)
2.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B)
2.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,
 H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,
 H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
;
_olex2_submission_special_instructions 'No special instructions were received'