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_7036089
_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 H76 Cl2 Mg2 N2 O2 Si4'
_chemical_formula_sum            'C32 H76 Cl2 Mg2 N2 O2 Si4'
_chemical_formula_weight         752.82
_chemical_name_systematic
'bis(tertbutyldimethylsilyl)amido magnesium chloride'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-10-08
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2015-08-03 deposited with the CCDC.
2015-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.871(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.5683(7)
_cell_length_b                   11.3302(15)
_cell_length_c                   21.3284(19)
_cell_measurement_reflns_used    1402
_cell_measurement_temperature    150.03(10)
_cell_measurement_theta_max      24.2400
_cell_measurement_theta_min      3.6140
_cell_volume                     2278.0(4)
_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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
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      150.03(10)
_diffrn_detector_area_resol_mean 8.0714
_diffrn_measured_fraction_theta_full 0.9972
_diffrn_measured_fraction_theta_max 0.9972
_diffrn_measurement_details
;
  1 omega  -93.00   15.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.3597  -19.0000   30.0000 108

  2 omega  -29.00   47.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.3597   57.0000    0.0000 76

  3 omega   20.00   75.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4535 -118.0000  102.0000 55
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0138277000
_diffrn_orient_matrix_UB_12      0.0354680000
_diffrn_orient_matrix_UB_13      0.0277452000
_diffrn_orient_matrix_UB_21      -0.0199944000
_diffrn_orient_matrix_UB_22      0.0510727000
_diffrn_orient_matrix_UB_23      -0.0186744000
_diffrn_orient_matrix_UB_31      -0.0711945000
_diffrn_orient_matrix_UB_32      -0.0074324000
_diffrn_orient_matrix_UB_33      0.0045275000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0799
_diffrn_reflns_av_unetI/netI     0.1505
_diffrn_reflns_Laue_measured_fraction_full 0.9972
_diffrn_reflns_Laue_measured_fraction_max 0.9972
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8828
_diffrn_reflns_point_group_measured_fraction_full 0.9972
_diffrn_reflns_point_group_measured_fraction_max 0.9972
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         3.420
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.303
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.972
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.098
_exptl_crystal_description       plank
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.1558
_exptl_crystal_size_mid          0.0587
_exptl_crystal_size_min          0.0426
_refine_diff_density_max         0.736
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         4175
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1373
_refine_ls_R_factor_gt           0.0738
_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^)+(0.0621P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1504
_refine_ls_wR_factor_ref         0.1969
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2311
_reflns_number_total             4175
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02535d2.cif
_cod_data_source_block           01
_cod_depositor_comments
'Adding full bibliography for 7036089--7036100.cif.'
_cod_database_code               7036089
_manchester_internal_coll_name   adpm82
_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         MgNSi2ClC12H30OC4H8
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.82
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C13 \\sim C14 \\sim C15 \\sim C16: within 1.7A with sigma of 0.004 and sigma
for terminal atoms of 0.008
3.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C16(H16A,H16B), C15(H15A,H15B)
3.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C2(H2A,H2B,H2C), C12(H12A,H12B,H12C), C11(H11A,H11B,H11C),
 C3(H3A,H3B,H3C), C8(H8A,H8B,H8C), C4(H4A,H4B,H4C), C10(H10A,H10B,H10C), C9(H9A,
 H9B,H9C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              56124
_olex2_exptl_crystal_mounting_method 'Fomblin on microscope slide.'
_olex2_submission_special_instructions 'No special instructions were received'