Regioselective magnesiation of N-heterocyclic molecules: securing insecure cyclic anions by a β-diketiminate-magnesium clamp.
Davin, Laia; McLellan, Ross; Hernán-Gómez, Alberto; Clegg, William; Kennedy, Alan R.; Mertens, Maria; Stepek, Iain A.; Hevia, Eva; Chemical communications (Cambridge, England) 53 (2017) 3653–3656; doi:10.1039/c6cc09675a

data_7119396
_publ_section_title
;
 Regioselective magnesiation of N-heterocyclic molecules: securing
 insecure cyclic anions by a \b-diketiminate-magnesium clamp.
;
_journal_issue                   26
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3653
_journal_page_last               3656
_journal_paper_doi               10.1039/c6cc09675a
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety         'C70 H94 Mg2 N6,C4 H8 O'
_chemical_formula_sum            'C74 H102 Mg2 N6 O'
_chemical_formula_weight         1140.23
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-11-28 deposited with the CCDC.
2017-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                101.488(3)
_cell_angle_beta                 92.550(3)
_cell_angle_gamma                93.804(3)
_cell_formula_units_Z            2
_cell_length_a                   12.3525(7)
_cell_length_b                   12.4080(8)
_cell_length_c                   22.7369(14)
_cell_measurement_reflns_used    9965
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.44
_cell_measurement_theta_min      2.28
_cell_volume                     3401.6(4)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Diamond GDA'
_computing_data_reduction        'Bruker APEX2'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXL-2014/7 and local programs'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.814
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type
'fixed-\c diffractometer with Pilatus 2M detector'
_diffrn_measurement_method       'narrow-frame \w and \f scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0635
_diffrn_reflns_av_unetI/netI     0.0974
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            42336
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         1.604
_diffrn_source                   'Diamond beamline I19'
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.113
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.432
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     768
_refine_ls_number_reflns         13767
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0561
_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^)+(0.0568P)^2^+0.3543P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1421
_refine_ls_wR_factor_ref         0.1595
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9222
_reflns_number_total             13767
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc09675a2.cif
_cod_data_source_block           ewc160007
_cod_depositor_comments
'Adding full bibliography for 7119393--7119397.cif.'
_cod_database_code               7119396
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.992
_shelx_estimated_absorpt_t_max   0.998
_shelx_res_checksum              728
_shelx_hkl_checksum              43485