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_1514442
_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_sum            'C42.5 H61.5 Mg N4'
_chemical_formula_weight         652.77
_chemical_name_systematic
;
?
;
_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                 96.842(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.0179(4)
_cell_length_b                   13.5976(3)
_cell_length_c                   21.7756(6)
_cell_measurement_reflns_used    7478
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      29.7144
_cell_measurement_theta_min      2.8207
_cell_volume                     4121.08(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0380
_diffrn_reflns_av_sigmaI/netI    0.0681
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            21699
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.74
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.052
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1426
_refine_diff_density_max         0.707
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         8074
_refine_ls_number_restraints     77
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.1027
_refine_ls_R_factor_gt           0.0640
_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^)+(0.1205P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1814
_refine_ls_wR_factor_ref         0.1953
_reflns_number_gt                5016
_reflns_number_total             8074
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c3sc22326d.txt
_cod_data_source_block           vb6
_cod_original_sg_symbol_H-M      P21/n
_cod_original_formula_sum        'C42.50 H61.50 Mg N4'
_cod_database_code               1514442