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_7119397
_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_compound_source        'synthesis as described'
_chemical_formula_moiety         'C73 H96 Mg2 N8'
_chemical_formula_sum            'C73 H96 Mg2 N8'
_chemical_formula_weight         1134.2
_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'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
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_audit_creation_date             2013-03-22T11:29:21-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2016-11-28 deposited with the CCDC.
2017-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                96.729(7)
_cell_angle_beta                 109.851(8)
_cell_angle_gamma                103.994(7)
_cell_formula_units_Z            1
_cell_length_a                   10.7648(8)
_cell_length_b                   12.8654(11)
_cell_length_c                   13.4034(12)
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_cell_measurement_temperature    123(2)
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_cell_measurement_wavelength     0.71073
_cell_volume                     1653.3(3)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_collection
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_reduction
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
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_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 16.0727
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0264562000
_diffrn_orient_matrix_UB_12      0.0580875000
_diffrn_orient_matrix_UB_13      0.0152468000
_diffrn_orient_matrix_UB_21      -0.0333240000
_diffrn_orient_matrix_UB_22      0.0032249000
_diffrn_orient_matrix_UB_23      -0.0546674000
_diffrn_orient_matrix_UB_31      -0.0598969000
_diffrn_orient_matrix_UB_32      0.0023320000
_diffrn_orient_matrix_UB_33      0.0101485000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0772
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
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_diffrn_reflns_number            13766
_diffrn_reflns_theta_full        27
_diffrn_reflns_theta_max         27
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94809
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
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Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light brown'
_exptl_crystal_density_diffrn    1.139
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             614
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         13766
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.1062
_refine_ls_R_factor_gt           0.0776
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1074P)^2^+1.4283P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2137
_refine_ls_wR_factor_ref         0.24
_reflns_number_gt                9992
_reflns_number_total             13766
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c6cc09675a2.cif
_cod_data_source_block           iain2
_cod_depositor_comments
'Adding full bibliography for 7119393--7119397.cif.'
_cod_original_cell_volume        1653.3(2)
_cod_database_code               7119397