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_7128825
_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_moiety         '2(C132 H152 Mg4 N8 O4), 6(C6 H14), 3(C7 H8)'
_chemical_formula_sum            'C321 H412 Mg8 N16 O8'
_chemical_formula_weight         4817.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-07-17 deposited with the CCDC.	2021-08-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.114(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
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_cell_length_b                   18.8553(3)
_cell_length_c                   23.5022(5)
_cell_measurement_reflns_used    16784
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      68.3950
_cell_measurement_theta_min      3.7120
_cell_volume                     13878.0(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1360
_diffrn_reflns_av_unetI/netI     0.0870
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            153548
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.527
_diffrn_reflns_theta_min         3.669
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.680
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63667
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.153
_exptl_crystal_description       block
_exptl_crystal_F_000             5220
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.090
_platon_squeeze_details
;
 After refinement of the main molecule, the residual electron density was 
 partially modelled as a mixture of disordered solvent (3 x C6H14 and 
 1.5 x PhMe in the ASU). However, the refinement of the 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.).
;
_refine_diff_density_max         0.332
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1379
_refine_ls_number_reflns         28946
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1262
_refine_ls_R_factor_gt           0.0756
_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^)+(0.0738P)^2^+3.9876P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1620
_refine_ls_wR_factor_ref         0.1832
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16999
_reflns_number_total             28946
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03890g2.cif
_cod_data_source_block           cj1500
_cod_depositor_comments
'Adding full bibliography for 7128823--7128826.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7128825
_shelx_shelxl_version_number     2018/3
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              58202
_shelx_hkl_checksum              63043
_shelx_fab_checksum              40091