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_7036100
_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         '0.5(C84 H188 Mg4 N4 Si8)'
_chemical_formula_sum            'C42 H94 Mg2 N2 Si4'
_chemical_formula_weight         788.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-07-30
_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                90
_cell_angle_beta                 117.029(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.268(3)
_cell_length_b                   16.935(4)
_cell_length_c                   13.2403(17)
_cell_measurement_reflns_used    648
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      20.6420
_cell_measurement_theta_min      3.6990
_cell_volume                     5046.9(16)
_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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_computing_data_reduction
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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)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (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 0.392
_diffrn_measured_fraction_theta_max 0.851
_diffrn_measurement_details
;
  1 omega  -11.00   39.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       -3.1874  -99.0000 -120.0000 50

  2 omega  -61.00   60.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       -3.1874    0.0000  -90.0000 121
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0370442000
_diffrn_orient_matrix_UB_12      -0.0193861000
_diffrn_orient_matrix_UB_13      0.0191002000
_diffrn_orient_matrix_UB_21      -0.0256117000
_diffrn_orient_matrix_UB_22      -0.0363517000
_diffrn_orient_matrix_UB_23      -0.0052857000
_diffrn_orient_matrix_UB_31      0.0292106000
_diffrn_orient_matrix_UB_32      -0.0072987000
_diffrn_orient_matrix_UB_33      -0.0244674000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
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_diffrn_reflns_av_R_equivalents  0.1610
_diffrn_reflns_av_unetI/netI     0.1225
_diffrn_reflns_Laue_measured_fraction_full 0.392
_diffrn_reflns_Laue_measured_fraction_max 0.851
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10631
_diffrn_reflns_point_group_measured_fraction_full 0.392
_diffrn_reflns_point_group_measured_fraction_max 0.851
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         19.778
_diffrn_reflns_theta_min         3.370
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.170
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63978
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_exptl_absorpt_process_details
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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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.037
_exptl_crystal_description       needle
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.2319
_exptl_crystal_size_mid          0.1414
_exptl_crystal_size_min          0.1166
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         1949
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.1424
_refine_ls_R_factor_gt           0.1003
_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^)+81.6204P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1918
_refine_ls_wR_factor_ref         0.2060
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1378
_reflns_number_total             1949
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02535d2.cif
_cod_data_source_block           04
_cod_depositor_comments
'Adding full bibliography for 7036089--7036100.cif.'
_cod_original_cell_volume        5047.1(15)
_cod_database_code               7036100
_manchester_internal_coll_name   adpm92
_manchester_internal_coll_client CAPG/AS/FO/DPM
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 4s
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   FO
_manchester_internal_coll_date   27/10/2014
_manchester_internal_process_user FO
_manchester_internal_process_date 17/06/2015
_manchester_internal_solution_user FO
_manchester_internal_solution_date 17/06/2015
_manchester_internal_refinement_user FO
_manchester_internal_refinement_date 18/06/2015
_manchester_internal_validation_user 18/06/2015
_manchester_internal_validation_date 18/06/2015
_manchester_internal_archive_date IVY
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         C42H84Mg2N2Si4
_reflns_odcompleteness_completeness 67.94
_reflns_odcompleteness_iscentric 1
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_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. Restrained distances
 C24-C23 \\sim C22-C23 \\sim C20-C19 \\sim C21-C20
 with sigma of 0.004
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.004 and sigma
for terminal atoms of 0.008
5. Others
 Fixed Sof: C19(0.5) H19A(0.5) H19B(0.5) C20(0.5) H20(0.5) C21(0.5) H21A(0.5)
 H21B(0.5) C22(0.5) H22A(0.5) H22B(0.5) C23(0.5) H23(0.5) C24(0.5) H24A(0.5)
 H24B(0.5)
6.a Ternary CH refined with riding coordinates:
 C1(H1), C4(H4), C7(H7), C10(H10), C13(H13), C16(H16)
6.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C21(H21A,H21B), C22(H22A,H22B), C24(H24A,H24B)
6.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C23(H23)
6.d 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              8605
_olex2_submission_special_instructions 'No special instructions were received'