Unsymmetrical bis(anilido)xanthene ligands: development and use in the preparation of magnesium diamide complexes.
Evans, Matthew J.; Jones, Cameron; Chemical communications (Cambridge, England) 61 (2025) 11814–11817; doi:10.1039/d5cc03202d

data_7134776
_publ_section_title
;
 Unsymmetrical bis(anilido)xanthene ligands: development and use in the
 preparation of magnesium diamide complexes.
;
_journal_issue                   63
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              11814
_journal_page_last               11817
_journal_paper_doi               10.1039/d5cc03202d
_journal_volume                  61
_journal_year                    2025
_chemical_formula_sum            'C80 H110 Mg N2 O3'
_chemical_formula_weight         1172.00
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2025-06-05 deposited with the CCDC.	2025-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.86(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.500(4)
_cell_length_b                   17.780(4)
_cell_length_c                   22.860(5)
_cell_measurement_reflns_used    28099
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.372
_cell_measurement_theta_min      0.922
_cell_volume                     6875(3)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'AS QEGUI'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 13.3000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  MX1
_diffrn_measurement_method       'Omega Scan'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            188359
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         0.922
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  'Value not reported by XDS'
_exptl_absorpt_correction_T_min  'Value not reported by XDS'
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 2010)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.132
_exptl_crystal_description       plate
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.544
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details
;
 Flack x determined using 12852 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.49(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1573
_refine_ls_number_reflns         28099
_refine_ls_number_restraints     174
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0367
_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^)+(0.0637P)^2^+1.0741P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0960
_refine_ls_wR_factor_ref         0.0969
_reflns_Friedel_coverage         0.933
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                27361
_reflns_number_total             28099
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc03202d2.cif
_cod_data_source_block           cj1748
_cod_depositor_comments
'Adding full bibliography for 7134774--7134781.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7134776
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.991
_shelx_estimated_absorpt_t_max   0.998
_shelx_res_checksum              63180
_shelx_hkl_checksum              15901