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_7134778
_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            'C19 H24 N2 O'
_chemical_formula_weight         296.40
_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
_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                90
_cell_angle_beta                 117.172(2)
_cell_angle_gamma                90
_cell_formula_units_Z            16
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_cell_length_b                   26.1026(3)
_cell_length_c                   17.6208(3)
_cell_measurement_reflns_used    24044
_cell_measurement_temperature    122.9(2)
_cell_measurement_theta_max      79.9130
_cell_measurement_theta_min      4.5180
_cell_volume                     6719.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
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_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      122.9(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            54341
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.128
_diffrn_reflns_theta_min         3.490
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.565
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38281
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.70a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_description       plate
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.979
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     949
_refine_ls_number_reflns         14255
_refine_ls_number_restraints     338
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0670
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1151P)^2^+3.7984P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1877
_refine_ls_wR_factor_ref         0.1989
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11911
_reflns_number_total             14255
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc03202d2.cif
_cod_data_source_block           cj1742
_cod_depositor_comments
'Adding full bibliography for 7134774--7134781.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7134778
_shelx_shelxl_version_number     2018/3
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_smtbx_masks_special_details
;
The unit cell contains 4 water 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              94968
_shelx_hkl_checksum              27770
_shelx_fab_checksum              6110