Isomeric and chemical consequences of the direct magnesiation of 1,3-benzoazoles using β-diketiminate-stabilized magnesium bases
Baillie, Sharon E.; Blair, Victoria L.; Bradley, Tyne D.; Clegg, William; Cowan, Jemma; Harrington, Ross W.; Hernán-Gómez, Alberto; Kennedy, Alan R.; Livingstone, Zoe; Hevia, Eva; Chemical Science 4 (2013) 1895–; doi:10.1039/c3sc22326d

data_1514440
_publ_section_title
;
 Isomeric and chemical consequences of the direct magnesiation of
 1,3-benzoazoles using \b-diketiminate-stabilized magnesium bases
;
_journal_issue                   4
_journal_name_full               'Chemical Science'
_journal_page_first              1895
_journal_paper_doi               10.1039/c3sc22326d
_journal_volume                  4
_journal_year                    2013
_chemical_formula_moiety         'C43 H50 Mg N4 S2, 1.25 C4 H8 O'
_chemical_formula_sum            'C48 H60 Mg N4 O1.25 S2'
_chemical_formula_weight         801.43
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.385(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.964(5)
_cell_length_b                   12.505(3)
_cell_length_c                   38.624(10)
_cell_measurement_reflns_used    9746
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.63
_cell_measurement_theta_min      2.36
_cell_volume                     9103(4)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Rigaku CrystalClear'
_computing_data_reduction        'Bruker APEX2'
_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      120(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Crystal Logic diffractometer and Rigaku Saturn 724+ CCD'
_diffrn_measurement_method       'thick-slice \w scans'
_diffrn_radiation_monochromator  'silicon double crystal'
_diffrn_radiation_source         'Diamond beamline I19'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0683
_diffrn_reflns_av_sigmaI/netI    0.0577
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            69167
_diffrn_reflns_theta_full        24.21
_diffrn_reflns_theta_max         24.21
_diffrn_reflns_theta_min         1.11
_exptl_absorpt_coefficient_mu    0.159
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3440
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.969
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       0.0020(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1037
_refine_ls_number_reflns         16016
_refine_ls_number_restraints     186
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1026
_refine_ls_R_factor_gt           0.0746
_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^)+(0.0672P)^2^+17.1363P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1793
_refine_ls_wR_factor_ref         0.1956
_reflns_number_gt                11598
_reflns_number_total             16016
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c3sc22326d.txt
_cod_data_source_block           eh3
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1514440