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_7134780
_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            'C164 H202 K6 Mg2 N4 O2'
_chemical_formula_weight         2544.50
_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   mixed
_atom_sites_solution_primary     fmap
_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                103.86(3)
_cell_angle_beta                 104.61(3)
_cell_angle_gamma                93.90(3)
_cell_formula_units_Z            1
_cell_length_a                   13.650(3)
_cell_length_b                   16.680(3)
_cell_length_c                   24.090(5)
_cell_measurement_reflns_used    97564
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.372
_cell_measurement_theta_min      0.906
_cell_volume                     5105(2)
_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 0.990
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  MX1
_diffrn_measurement_method       'Omega Scan'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            97564
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         0.906
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.172
_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            'dark red'
_exptl_crystal_density_diffrn    0.828
_exptl_crystal_description       block
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.759
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     816
_refine_ls_number_reflns         20409
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1092
_refine_ls_R_factor_gt           0.0890
_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^)+(0.1794P)^2^+2.5081P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2691
_refine_ls_wR_factor_ref         0.2946
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14278
_reflns_number_total             20409
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc03202d2.cif
_cod_data_source_block           cj1747
_cod_depositor_comments
'Adding full bibliography for 7134774--7134781.cif.'
_cod_database_code               7134780
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.981
_shelx_estimated_absorpt_t_max   0.991
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_smtbx_masks_special_details
;
The unit cell contains 12 benzene solvates that were poorly ordered, such 
that a suitable crystallographic model could not be derived. Consequently,
these solvates were treated as a diffuse contribution to the overall 
scattering without specific atom positions using the Olex2 implementation of
SQUEEZE (Acta Cryst. (2015). C71, 9-18), also known as Solvent Mask. 
(Acta Cryst. A 1990, A46, 194., J. Appl. Cryst., 42: 339-341. & J. Molec. 
Biol. 1994, 243, 100).
;
_shelx_res_checksum              37051
_shelx_hkl_checksum              80205
_shelx_fab_checksum              4004