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_7036097
_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         'C32 H78 Mg2 N2 Si4'
_chemical_formula_sum            'C32 H78 Mg2 N2 Si4'
_chemical_formula_weight         651.94
_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 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_audit_update_record
;
2015-08-03 deposited with the CCDC.
2015-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                76.250(6)
_cell_angle_beta                 80.293(6)
_cell_angle_gamma                84.415(6)
_cell_formula_units_Z            1
_cell_length_a                   8.3413(7)
_cell_length_b                   9.1521(6)
_cell_length_c                   14.4572(10)
_cell_measurement_reflns_used    2539
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      28.1500
_cell_measurement_theta_min      3.7210
_cell_volume                     1054.80(14)
_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)
;
_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)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector_area_resol_mean 8.0714
_diffrn_measured_fraction_theta_full 0.9970
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -42.00   53.00   1.0000    1.8700
omega____ theta____ kappa____ phi______ frames
    -      -17.7663   37.0000  -90.0000 95

  2 omega  -29.00    5.00   1.0000    1.8700
omega____ theta____ kappa____ phi______ frames
    -      -17.7663  -37.0000   90.0000 34

  3 omega  -48.00   47.00   1.0000    1.8700
omega____ theta____ kappa____ phi______ frames
    -      -17.7663   77.0000  120.0000 95

  4 omega   32.00   61.00   1.0000    1.8700
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -99.0000  -90.0000 29

  5 omega  -86.00    7.00   1.0000    1.8700
omega____ theta____ kappa____ phi______ frames
    -      -17.7663  -77.0000    0.0000 93
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0859328000
_diffrn_orient_matrix_UB_12      0.0021803000
_diffrn_orient_matrix_UB_13      -0.0056622000
_diffrn_orient_matrix_UB_21      -0.0057276000
_diffrn_orient_matrix_UB_22      0.0767195000
_diffrn_orient_matrix_UB_23      -0.0247475000
_diffrn_orient_matrix_UB_31      -0.0072088000
_diffrn_orient_matrix_UB_32      0.0223235000
_diffrn_orient_matrix_UB_33      0.0443379000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0613
_diffrn_reflns_Laue_measured_fraction_full 0.9970
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6587
_diffrn_reflns_point_group_measured_fraction_full 0.9970
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         3.293
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.192
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.738
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
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
            a multifaceted crystal model
;
_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    1.026
_exptl_crystal_description       needle
_exptl_crystal_F_000             364
_exptl_crystal_size_max          0.4001
_exptl_crystal_size_mid          0.2104
_exptl_crystal_size_min          0.2072
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         3843
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0459
_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^)+(0.0433P)^2^+0.2740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1123
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3074
_reflns_number_total             3843
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02535d2.cif
_cod_data_source_block           08
_cod_depositor_comments
'Adding full bibliography for 7036089--7036100.cif.'
_cod_original_cell_volume        1054.79(14)
_cod_database_code               7036097
_manchester_internal_coll_name   adpm141
_manchester_internal_coll_client CAPG/AS
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 5s
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   CAPG/FO
_manchester_internal_coll_date   8/10/14
_manchester_internal_process_user CAPG
_manchester_internal_process_date 8/10/14
_manchester_internal_solution_user CAPG
_manchester_internal_solution_date 8/10/14
_manchester_internal_refinement_user CAPG
_manchester_internal_refinement_date 8/10/2014
_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         'C20 N Si2 Mg'
_reflns_odcompleteness_completeness 99.70
_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
2. Restrained distances
 C16-H16B = C16-H16C = C16-H16A
 0.96 with sigma of 0.02
 H16B-H16A
 1.56 with sigma of 0.02
 H16A-H16C
 1.56 with sigma of 0.02
 H16C-H16B
 1.56 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C13(H13)
3.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,
 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)
;
_shelx_res_checksum              54555
_olex2_submission_special_instructions 'No special instructions were received'