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_7036095
_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         'C26 H66 Mg2 N2 Si4'
_chemical_formula_sum            'C26 H66 Mg2 N2 Si4'
_chemical_formula_weight         567.78
_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   mixed
_audit_creation_date             2015-04-24
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Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
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_audit_update_record
;
2015-08-03 deposited with the CCDC.
2015-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                94.746(7)
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_cell_formula_units_Z            1
_cell_length_a                   7.7791(8)
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_cell_measurement_reflns_used    1262
_cell_measurement_temperature    150.01(11)
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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)
(compiled Aug  2 2013,16:46:58)
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_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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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_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_diffrn_ambient_temperature      150.01(11)
_diffrn_detector_area_resol_mean 8.0714
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_diffrn_measurement_details
;
  1 omega  -11.00   81.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       18.8601   77.0000  -30.0000 92

  2 omega   23.00   61.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -99.0000 -150.0000 38

  3 omega   35.00   75.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       18.8601 -178.0000 -150.0000 40

  4 omega  -10.00   57.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -99.0000   90.0000 67

  5 omega  -51.00   15.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -77.0000 -150.0000 66

  6 omega  -91.00    2.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663  -19.0000   30.0000 93
;
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_diffrn_orient_matrix_UB_32      0.0367863000
_diffrn_orient_matrix_UB_33      0.0055796000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_av_unetI/netI     0.1173
_diffrn_reflns_Laue_measured_fraction_full 0.9979
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_diffrn_reflns_limit_h_max       9
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_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6732
_diffrn_reflns_point_group_measured_fraction_full 0.9979
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_diffrn_reflns_theta_full        26.000
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_diffrn_reflns_theta_min         3.294
_diffrn_source                   'SuperNova (Mo) X-ray Source'
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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            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.999
_exptl_crystal_description       needle
_exptl_crystal_F_000             316
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_exptl_crystal_size_min          0.0932
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_refine_ls_number_reflns         3448
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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^)+(0.0451P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_number_gt                2157
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_cod_depositor_comments
'Adding full bibliography for 7036089--7036100.cif.'
_cod_original_cell_volume        943.75(16)
_cod_database_code               7036095
_manchester_internal_coll_name   adpm142
_manchester_internal_coll_client FO/DPM
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_manchester_internal_coll_user   FO
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_manchester_internal_refinement_date 07/03/2015
_manchester_internal_validation_user IVY
_manchester_internal_validation_date 25/04/2015
_manchester_internal_archive_date 25/04/2015
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C20 N Si2 Mg'
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H13B-H13A
 1.56 with sigma of 0.02
 H13A-H13C
 1.56 with sigma of 0.02
 C13-H13B = C13-H13A = C13-H13C
 0.96 with sigma of 0.02
 H13C-H13B
 1.56 with sigma of 0.02
3.a Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,
 H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,
 H11C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              96321
_olex2_submission_special_instructions 'No special instructions were received'