Assessing the reactivity of sodium alkyl-magnesiates towards quinoxaline: single electron transfer (SET) vs. nucleophilic alkylation processes.
Livingstone, Zoe; Hernán-Gómez, Alberto; Baillie, Sharon E.; Armstrong, David R.; Carrella, Luca M.; Clegg, William; Harrington, Ross W.; Kennedy, Alan R.; Rentschler, Eva; Hevia, Eva; Dalton transactions (Cambridge, England : 2003) 45 (2016) 6175–6182; doi:10.1039/c5dt04044b

data_7037359
_publ_section_title
;
 Assessing the reactivity of sodium alkyl-magnesiates towards quinoxaline:
 single electron transfer (SET) vs. nucleophilic alkylation processes.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6175
_journal_page_last               6182
_journal_paper_doi               10.1039/c5dt04044b
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety
'2 C24 H48 Na O6 +,C 88 H100 Mg2 N8 Si2 2-,2 C4 H8 O'
_chemical_formula_sum            'C144 H212 Mg2 N8 Na2 O14 Si2'
_chemical_formula_weight         2429.98
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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-2014/7
_audit_update_record
;
2015-10-14 deposited with the CCDC.
2015-11-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.851(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.601(7)
_cell_length_b                   15.449(8)
_cell_length_c                   34.612(19)
_cell_measurement_reflns_used    3662
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      24.28
_cell_measurement_theta_min      2.22
_cell_volume                     6730(6)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Rigaku CrystalClear'
_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
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type
'Crystal Logic diffractometer and Rigaku Saturn 724+ detector'
_diffrn_measurement_method       'thick-slice \w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.1625
_diffrn_reflns_av_unetI/netI     0.1489
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            29380
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        21.314
_diffrn_reflns_theta_max         21.314
_diffrn_reflns_theta_min         1.714
_diffrn_source                   'Diamond Light Source beamline I19'
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
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_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2636
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.451
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       0.027(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014)'
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1061
_refine_ls_number_reflns         8121
_refine_ls_number_restraints     3054
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.1908
_refine_ls_R_factor_gt           0.0973
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1966P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2634
_refine_ls_wR_factor_ref         0.3319
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3861
_reflns_number_total             8121
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04044b2.cif
_cod_data_source_block           rem560dls
_cod_depositor_comments
'Adding full bibliography for 7037359--7037362.cif.'
_cod_database_code               7037359
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.994
_shelx_estimated_absorpt_t_max   0.999
_shelx_res_checksum              78905