Probing the metallating ability of a polybasic sodium alkylmagnesiate supported by a bulky bis(amido) ligand: deprotomagnesiation reactions of nitrogen-based aromatic substrates.
Armstrong, David R.; Clegg, William; Hernán-Gómez, Alberto; Kennedy, Alan R.; Livingstone, Zoe; Robertson, Stuart D.; Russo, Luca; Hevia, Eva; Dalton transactions (Cambridge, England : 2003) 43 (2014) 4361–4369; doi:10.1039/c3dt52639a

data_7029004
_publ_section_title
;
 Probing the metallating ability of a polybasic sodium alkylmagnesiate
 supported by a bulky bis(amido) ligand: deprotomagnesiation reactions of
 nitrogen-based aromatic substrates.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4361
_journal_page_last               4369
_journal_paper_doi               10.1039/c3dt52639a
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C56 H77 Mg N4 Na O3 Si'
_chemical_formula_sum            'C56 H77 Mg N4 Na O3 Si'
_chemical_formula_weight         929.61
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.314(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4287(6)
_cell_length_b                   38.3533(18)
_cell_length_c                   14.3444(7)
_cell_measurement_reflns_used    8228
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.8298
_cell_measurement_theta_min      2.7642
_cell_volume                     5559.3(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_device_type  'Oxford Diffraction, Gemini S'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_sigmaI/netI    0.0566
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            39077
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.89
_diffrn_reflns_theta_min         3.16
_exptl_absorpt_coefficient_mu    0.105
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99170
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.111
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.604
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     638
_refine_ls_number_reflns         13477
_refine_ls_number_restraints     128
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0968
_refine_ls_R_factor_gt           0.0665
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0715P)^2^+3.3172P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1553
_refine_ls_wR_factor_ref         0.1707
_reflns_number_gt                9627
_reflns_number_total             13477
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            c3dt52639a.txt
_cod_data_source_block           srzl1106
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7029004