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_7029003
_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         '2 C20 H40 Na O5 +,C88 H102 Mg2 N8 Si2 2-'
_chemical_formula_sum            'C128 H182 Mg2 N8 Na2 O10 Si2'
_chemical_formula_weight         2143.60
_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                 113.694(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   19.3321(10)
_cell_length_b                   17.1557(8)
_cell_length_c                   19.9580(11)
_cell_measurement_reflns_used    7295
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.43
_cell_measurement_theta_min      3.12
_cell_volume                     6061.2(6)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.838
_diffrn_measurement_device_type
'Oxford Diffraction Gemini A Ultra diffractomer'
_diffrn_measurement_method       'thin-slice \w scans'
_diffrn_radiation_monochromator  none
_diffrn_radiation_source         'sealed tube with Enhance optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0921
_diffrn_reflns_av_sigmaI/netI    0.2164
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            41345
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.47
_diffrn_reflns_theta_min         3.13
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_correction_T_min  0.956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2320
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.753
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     694
_refine_ls_number_reflns         12833
_refine_ls_number_restraints     1123
_refine_ls_restrained_S_all      0.767
_refine_ls_R_factor_all          0.1726
_refine_ls_R_factor_gt           0.0533
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0565P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1084
_refine_ls_wR_factor_ref         0.1275
_reflns_number_gt                4767
_reflns_number_total             12833
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c3dt52639a.txt
_cod_data_source_block           rem532
_cod_original_cell_volume        6061.2(5)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7029003