Reductive coupling of CO with magnesium anthracene complexes: formation of magnesium enediolates.
Yuvaraj, K.; Jones, Cameron; Chemical communications (Cambridge, England) 57 (2021) 9224–9227; doi:10.1039/d1cc03890g

data_7128826
_publ_section_title
;
 Reductive coupling of CO with magnesium anthracene complexes: formation
 of magnesium enediolates.
;
_journal_issue                   73
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9224
_journal_page_last               9227
_journal_paper_doi               10.1039/d1cc03890g
_journal_volume                  57
_journal_year                    2021
_chemical_formula_sum            'C145 H160 Mg4 N8 O4'
_chemical_formula_weight         2176.04
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2021-07-17 deposited with the CCDC.	2021-08-16 downloaded from the CCDC.
;
_cell_angle_alpha                88.26(3)
_cell_angle_beta                 86.73(3)
_cell_angle_gamma                83.85(3)
_cell_formula_units_Z            2
_cell_length_a                   13.301(3)
_cell_length_b                   19.539(4)
_cell_length_c                   25.912(5)
_cell_measurement_reflns_used    24085
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.50
_cell_measurement_theta_min      3.00
_cell_volume                     6683(2)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'Blu-Ice (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CifTAB
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7109
_diffrn_reflns_av_R_equivalents  0.0880
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
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_diffrn_reflns_point_group_measured_fraction_full 0.970
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_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         3.001
_diffrn_source                   'Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  0.9948
_exptl_absorpt_correction_T_min  0.9911
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   XDS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.081
_exptl_crystal_description       block
_exptl_crystal_F_000             2332
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_exptl_crystal_size_mid          0.080
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_platon_squeeze_details
;
 After refinement of the main molecule, the residual electron density was 
 partially modelled as a mixture of disordered solvent (4 x PhMe 0.5 occupancy
disordered over two sites in the ASU). However, the refinement of the disordered
solvent models was unsatisfactory and consequently the resdiual electron density 
was accounted for using PLATON/SQUEEZE (Spek, A.L. (2015). Acta Cryst. C71, 9-18.).
One ordered molecule of toluene in the ASU was refined normally
;
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.070
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_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1358
_refine_ls_number_reflns         24085
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0912
_refine_ls_R_factor_gt           0.0788
_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^)+(0.1602P)^2^+1.1222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2350
_refine_ls_wR_factor_ref         0.2456
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18709
_reflns_number_total             24085
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03890g2.cif
_cod_data_source_block           Cj1501
_cod_depositor_comments
'Adding full bibliography for 7128823--7128826.cif.'
_cod_database_code               7128826
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.992
_shelx_estimated_absorpt_t_max   0.995
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              11400
_shelx_hkl_checksum              91471
_shelx_fab_checksum              28207