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_7036090
_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         'C38 H88 Cl2 Mg2 N2 O2 Si4'
_chemical_formula_sum            'C38 H88 Cl2 Mg2 N2 O2 Si4'
_chemical_formula_weight         836.98
_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
_audit_creation_date             2015-07-30
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Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
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2015-08-03 deposited with the CCDC.
2015-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                86.179(8)
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_cell_formula_units_Z            1
_cell_length_a                   9.7845(8)
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_cell_length_c                   12.2422(12)
_cell_measurement_reflns_used    2123
_cell_measurement_temperature    108(2)
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_computing_cell_refinement
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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   -6.00  104.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       22.3246   77.0000  120.0000 110

  2 omega   -5.00  104.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       22.3246   77.0000 -120.0000 109

  3 omega   -6.00  104.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       22.3246   77.0000    0.0000 110

  4 omega   34.00   96.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       22.3246  179.0000 -120.0000 62
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_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
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_diffrn_radiation_monochromator  graphite
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_diffrn_reflns_av_unetI/netI     0.0859
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_diffrn_reflns_limit_l_max       14
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_diffrn_reflns_number            7601
_diffrn_reflns_point_group_measured_fraction_full 0.993
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_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.972
_diffrn_source                   'Enhance (Mo) X-ray Source'
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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)
Numerical absorption correction based on gaussian integration over
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_exptl_crystal_density_diffrn    1.145
_exptl_crystal_F_000             460
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_refine_ls_extinction_method     none
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_refine_ls_structure_factor_coef Fsqd
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'w=1/[\s^2^(Fo^2^)+(0.0401P)^2^] where P=(Fo^2^+2Fc^2^)/3'
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'Adding full bibliography for 7036089--7036100.cif.'
_cod_database_code               7036090
_manchester_internal_coll_name   odpm31
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_manchester_internal_coll_user   CAPG
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_manchester_internal_validation_user IVY
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_manchester_internal_archive_date 2015-07-30
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         MgClNSi2C6H15C9H21
_reflns_odcompleteness_completeness 99.06
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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)
2.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B)
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), C13(H13A,
 H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              10475
_olex2_submission_special_instructions 'No special instructions were received'