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_7036092
_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 N2 Na2 O2 Si4'
_chemical_formula_sum            'C32 H76 N2 Na2 O2 Si4'
_chemical_formula_weight         679.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-07-30
_audit_creation_method
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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                 93.418(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8330(8)
_cell_length_b                   11.7764(6)
_cell_length_c                   22.7974(10)
_cell_measurement_reflns_used    3364
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      25.8140
_cell_measurement_theta_min      3.7270
_cell_volume                     4243.1(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
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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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -48.00   51.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.3571   77.0000   30.0000 99

  2 omega   -4.00   22.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       19.4509   77.0000  150.0000 26

  3 omega   -6.00   81.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       19.4509   77.0000  -90.0000 87

  4 omega   17.00   46.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.3571   77.0000 -180.0000 29
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0014305000
_diffrn_orient_matrix_UB_12      -0.0601736000
_diffrn_orient_matrix_UB_13      -0.0008563000
_diffrn_orient_matrix_UB_21      -0.0410415000
_diffrn_orient_matrix_UB_22      -0.0024710000
_diffrn_orient_matrix_UB_23      0.0108219000
_diffrn_orient_matrix_UB_31      -0.0180888000
_diffrn_orient_matrix_UB_32      0.0008697000
_diffrn_orient_matrix_UB_33      -0.0292191000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_av_unetI/netI     0.0955
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17411
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         3.384
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.188
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.632
_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    1.063
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.4047
_exptl_crystal_size_mid          0.305
_exptl_crystal_size_min          0.2539
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         7758
_refine_ls_number_restraints     302
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1056
_refine_ls_R_factor_gt           0.0642
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0626P)^2^+1.7970P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1408
_refine_ls_wR_factor_ref         0.1656
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5150
_reflns_number_total             7758
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02535d2.cif
_cod_data_source_block           05a
_cod_depositor_comments
'Adding full bibliography for 7036089--7036100.cif.'
_cod_original_cell_volume        4243.2(4)
_cod_database_code               7036092
_manchester_internal_coll_name   adpm87
_manchester_internal_coll_client FO/CAPG
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 5.00
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   FO
_manchester_internal_coll_date   20/10/14
_manchester_internal_process_user CAPG
_manchester_internal_process_date 21/10/14
_manchester_internal_solution_user CAPG
_manchester_internal_solution_date 21/10/14
_manchester_internal_refinement_user FO
_manchester_internal_refinement_date 23/02/15
_manchester_internal_validation_user IVY
_manchester_internal_validation_date IVY
_manchester_internal_archive_date 30-07-15
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C20 H42 Si2 Na N O C4 H8'
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Restrained distances
 O1-C25 \\sim O1-C25A \\sim O1-C28A \\sim O1-C28 \\sim O2-C29 \\sim O2-C29A
\\sim O2-C32A \\sim O2-C32
 with sigma of 0.002
 C28A-C27A \\sim C28-C27 \\sim C26-C25A \\sim C26A-C25 \\sim C32-C31 \\sim
C32A-C31A \\sim C30A-C29A ~
 C30-C29
 with sigma of 0.02
 C31A-C30A \\sim C31-C30 \\sim C27A-C26 \\sim C27-C26A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C32 \\sim C32A \\sim O2 \\sim C29A \\sim C29 \\sim C30 \\sim C30A \\sim C31A
\\sim C31: within 2A with sigma of 0.004 and sigma for terminal atoms of 0.008
C25A \\sim C25 \\sim C26A \\sim C26 \\sim C27 \\sim C27A \\sim C28 \\sim C28A
\\sim O1: within 2A with sigma of 0.004 and sigma for terminal atoms of 0.008
4. Others
 Sof(C29A)=Sof(H29C)=Sof(H29D)=Sof(C30A)=Sof(H30C)=Sof(H30D)=Sof(C31A)=
 Sof(H31C)=Sof(H31D)=Sof(C32A)=Sof(H32C)=Sof(H32D)=1-FVAR(1)
 Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(C31)=Sof(H31A)=
 Sof(H31B)=Sof(C32)=Sof(H32A)=Sof(H32B)=FVAR(1)
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(C27A)=Sof(H27C)=Sof(H27D)=Sof(C28A)=
 Sof(H28C)=Sof(H28D)=Sof(C25A)=Sof(H25C)=Sof(H25D)=1-FVAR(2)
 Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(C28)=Sof(H28A)=
 Sof(H28B)=Sof(C26A)=Sof(H26C)=Sof(H26D)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,
 H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C29A(H29C,H29D),
 C30A(H30C,H30D), C31A(H31C,H31D), C32A(H32C,H32D), C27A(H27C,H27D), C26A(H26C,
 H26D), C28A(H28C,H28D), C25A(H25C,H25D)
5.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,
 H6B,H6C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,
 H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,
 H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C),
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C)
;
_shelx_res_checksum              1074
_olex2_submission_special_instructions 'No special instructions were received'