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_7128824
_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            'C94 H108 Mg4 O12.5'
_chemical_formula_weight         1535.04
_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   mixed
_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                90
_cell_angle_beta                 100.0110(10)
_cell_angle_gamma                90
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_cell_length_b                   14.5347(2)
_cell_length_c                   26.9566(3)
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_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      69.00
_cell_measurement_theta_min      6.33
_cell_volume                     8222.03(17)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    xseed
_computing_publication_material  Ciftab
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
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_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.000
_diffrn_reflns_theta_min         6.327
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.913
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87351
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_description       block
_exptl_crystal_F_000             3280
_exptl_crystal_size_max          0.140
_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 (2.5 x THF, each
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.).
;
_refine_diff_density_max         0.458
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     973
_refine_ls_number_reflns         15238
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0467
_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^)+(0.0566P)^2^+3.2026P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1148
_refine_ls_wR_factor_ref         0.1210
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12315
_reflns_number_total             15238
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03890g2.cif
_cod_data_source_block           Cj1502
_cod_depositor_comments
'Adding full bibliography for 7128823--7128826.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C94 H108 Mg4 O12.50'
_cod_database_code               7128824
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.883
_shelx_estimated_absorpt_t_max   0.922
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              96832
_shelx_hkl_checksum              1336
_shelx_fab_checksum              50230