Versatility of the methyl-bipyrimidine-<i>N</i>-oxide ligand for the design of lanthanide single-molecule magnets.
Douib, Haiet; Lefeuvre, Bertrand; Flores Gonzalez, Jessica; Dorcet, Vincent; Pointillart, Fabrice; CrystEngComm 27 (2025) 7677–7688; doi:10.1039/d5ce00831j

data_7251011
_publ_section_title
;
 Versatility of the methyl-bipyrimidine-<i>N</i>-oxide ligand for the
 design of lanthanide single-molecule magnets.
;
_journal_issue                   47
_journal_name_full               CrystEngComm
_journal_page_first              7677
_journal_page_last               7688
_journal_paper_doi               10.1039/d5ce00831j
_journal_volume                  27
_journal_year                    2025
_chemical_absolute_configuration rm/ad/rmad/syn/unk/.
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C93 H92 Dy2 F42 N4 O13'
_chemical_formula_sum            'C93 H92 Dy2 F42 N4 O13'
_chemical_formula_weight         2596.70
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2025-08-22 deposited with the CCDC.	2025-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.3763(6)
_cell_length_b                   21.8829(6)
_cell_length_c                   23.9653(8)
_cell_measurement_reflns_used    9963
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.4844
_cell_measurement_theta_min      2.1721
_cell_measurement_wavelength     0.710730
_cell_volume                     10685.9(6)
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_collection       'Bruker APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics
;
   'SXGRAPH (L. Farrugia, 1999), Mercury (CSD, 2020)'
;
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2020)'
_computing_structure_refinement  'SHELXL-2018_3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 CCD-LDI-APEX2
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'APEXII Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_orient_matrix_UB_11      0.0223971
_diffrn_orient_matrix_UB_12      0.0196056
_diffrn_orient_matrix_UB_13      -0.0325273
_diffrn_orient_matrix_UB_21      0.0413870
_diffrn_orient_matrix_UB_22      0.0032394
_diffrn_orient_matrix_UB_23      0.0222291
_diffrn_orient_matrix_UB_31      0.0139287
_diffrn_orient_matrix_UB_32      -0.0411512
_diffrn_orient_matrix_UB_33      -0.0137471
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            73824
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.519
_diffrn_reflns_theta_min         2.363
_diffrn_source_current           1.0
_diffrn_source_power             50.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.519
_exptl_absorpt_correction_T_max  0.772
_exptl_absorpt_correction_T_min  0.644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_description       prism
_exptl_crystal_F_000             5168
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.170
_refine_diff_density_max         0.979
_refine_diff_density_min         -0.812
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details
;
Flack x determined using 7883 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.033(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1404
_refine_ls_number_reflns         24497
_refine_ls_number_restraints     123
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+6.3658P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0900
_reflns_Friedel_coverage         0.856
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                19822
_reflns_number_total             24497
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d5ce00831j2.cif
_cod_data_source_block           HD396p
_cod_depositor_comments
'Adding full bibliography for 7251008--7251017.cif.'
_cod_database_code               7251011
_shelx_res_checksum              45820
_shelx_fab_checksum              57963