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_7036098
_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 H90 Mg2 N2 Si4'
_chemical_formula_sum            'C38 H90 Mg2 N2 Si4'
_chemical_formula_weight         736.09
_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
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-08-03 deposited with the CCDC.
2015-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                104.507(7)
_cell_angle_beta                 94.560(8)
_cell_angle_gamma                114.542(8)
_cell_formula_units_Z            1
_cell_length_a                   9.0592(9)
_cell_length_b                   10.5786(9)
_cell_length_c                   14.0661(13)
_cell_measurement_reflns_used    1779
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      25.7640
_cell_measurement_theta_min      3.8620
_cell_volume                     1161.1(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9870
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
  1 omega  -40.00   49.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663   37.0000 -120.0000 89

  2 omega   33.00   61.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -99.0000 -120.0000 28

  3 omega  -87.00   12.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663  -77.0000  -30.0000 99

  4 omega  -90.00    5.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663  -37.0000   60.0000 95
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_diffrn_measurement_device       'four-circle diffractometer'
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_diffrn_orient_matrix_UB_11      -0.0486158000
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_diffrn_orient_matrix_UB_21      -0.0337050000
_diffrn_orient_matrix_UB_22      0.0129451000
_diffrn_orient_matrix_UB_23      -0.0417340000
_diffrn_orient_matrix_UB_31      -0.0651564000
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_diffrn_orient_matrix_UB_33      -0.0152935000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.1008
_diffrn_reflns_Laue_measured_fraction_full 0.9870
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6575
_diffrn_reflns_point_group_measured_fraction_full 0.9870
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         3.539
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.181
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_exptl_absorpt_correction_T_min  0.996
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
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Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_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    1.053
_exptl_crystal_description       block
_exptl_crystal_F_000             412
_exptl_crystal_size_max          0.1515
_exptl_crystal_size_mid          0.0999
_exptl_crystal_size_min          0.0861
_refine_diff_density_max         0.336
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         4197
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.023
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_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0406P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1048
_refine_ls_wR_factor_ref         0.1181
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2881
_reflns_number_total             4197
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02535d2.cif
_cod_data_source_block           09
_cod_depositor_comments
'Adding full bibliography for 7036089--7036100.cif.'
_cod_original_cell_volume        1161.05(19)
_cod_database_code               7036098
_manchester_internal_coll_name   adpm138
_manchester_internal_coll_client AF/DPM
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 12s
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   AF
_manchester_internal_coll_date   27/02/2015
_manchester_internal_process_user FO
_manchester_internal_process_date 10/03/2015
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_manchester_internal_solution_date 10/03/2015
_manchester_internal_refinement_user FO
_manchester_internal_refinement_date 10/03/2015
_manchester_internal_validation_user IVY
_manchester_internal_validation_date 24/04/2015
_manchester_internal_archive_date 24/04/2015
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         Mg1C19N1Si2
_reflns_odcompleteness_completeness 98.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 C19-H19A = C19-H19B = C19-H19C
 0.96 with sigma of 0.02
 H19C-H19B
 1.56 with sigma of 0.02
 H19B-H19A
 1.56 with sigma of 0.02
 H19A-H19C
 1.56 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C1(H1), C4(H4), C7(H7), C10(H10), C13(H13), C16(H16)
3.b 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)
;
_shelx_res_checksum              34968
_olex2_submission_special_instructions 'No special instructions were received'