Substituents effect on Synthesis and Magnetic Properties of Carboxylic Acid Ligands Coordinated Dysprosium Complexes
Liu, Chen-Yang; Zhang, Qing-Yun; Zhan, CaiXia; Cao, Chen; Zhong, Fu-Hui; Zheng, Xiao-Yue; Peng, Yan; Liu, Sui-Jun; Hu, Zhao-Bo; Wen, He-Rui; CrystEngComm  (2026) –; doi:10.1039/D5CE01195G

data_7251667
_publ_section_title
;
 Substituent effect on the synthesis and magnetic properties of carboxylic
 acid ligand coordinated dysprosium complexes
;
_journal_issue                   14
_journal_name_full               CrystEngComm
_journal_page_first              2243
_journal_page_last               2249
_journal_paper_doi               10.1039/D5CE01195G
_journal_volume                  28
_journal_year                    2026
_chemical_formula_moiety         '2(C70 H46 Dy2 N8 O12), 4(C3 H7 N O)'
_chemical_formula_sum            'C152 H120 Dy4 N20 O28'
_chemical_formula_weight         3324.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc2px0tg
_audit_creation_date             2025-10-21
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2025-11-01 deposited with the CCDC.	2026-02-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.703(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.1367(13)
_cell_length_b                   13.3057(7)
_cell_length_c                   32.8861(15)
_cell_measurement_reflns_used    8591
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.2620
_cell_measurement_theta_min      2.0730
_cell_volume                     13618.5(11)
_computing_cell_refinement       'CrysAlisPro 1.171.42.92a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.92a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.92a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(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 0.788
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -6.00  37.00   0.50    1.50    --    4.91 -99.00 -60.00   86
  2  \w     -9.00  16.00   0.50    1.50    --   -5.92 -99.00  90.00   50
  3  \w    -79.00 -10.00   0.50    1.50    --   -5.92 -37.00 150.00  138
  4  \w     -7.00  61.00   0.50    1.50    --    4.91  37.00  60.00  136
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0045905000
_diffrn_orient_matrix_UB_12      0.0379294000
_diffrn_orient_matrix_UB_13      0.0146525000
_diffrn_orient_matrix_UB_21      -0.0031925000
_diffrn_orient_matrix_UB_22      0.0373626000
_diffrn_orient_matrix_UB_23      -0.0151605000
_diffrn_orient_matrix_UB_31      -0.0220948000
_diffrn_orient_matrix_UB_32      0.0024855000
_diffrn_orient_matrix_UB_33      0.0045919000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0695
_diffrn_reflns_av_unetI/netI     0.0965
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.788
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            47918
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.788
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.046
_diffrn_reflns_theta_min         2.063
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.254
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53229
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.92a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_description       block
_exptl_crystal_F_000             6640
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.051
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     923
_refine_ls_number_reflns         17183
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1146
_refine_ls_R_factor_gt           0.0600
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+69.6593P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1301
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10307
_reflns_number_total             17183
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce01195g2.cif
_cod_data_source_block           ha_py_auto
_cod_depositor_comments
'Adding full bibliography for 7251667--7251669.cif.'
_cod_database_code               7251667
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.806
_shelx_estimated_absorpt_t_min   0.806
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C71-O13
 1.2164 with sigma of 0.02
 O14-C76
 1.2164 with sigma of 0.02
 C72-C73
 2.4848 with sigma of 0.02
 C74-C75
 2.4848 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C72) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(N9) \\sim Ueq, Uanis(C73)
\\sim Ueq, Uanis(O13) \\sim Ueq: with sigma of 0.02 and sigma for terminal
atoms of 0.03
Uanis(O14) \\sim Ueq, Uanis(N10) \\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C74)
\\sim Ueq, Uanis(C76) \\sim Ueq: with sigma of 0.02 and sigma for terminal
atoms of 0.03
4.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C43(H43), C3(H3), C1(H1), C36(H36), C45(H45), C2(H2), C38(H38),
 C37(H37), C44(H44), C49(H49), C48(H48), C12(H12), C28(H28), C13(H13), C11(H11),
  C35(H35), C14(H14), C66(H66), C24(H24), C34(H34), C56(H56), C52(H52),
 C59(H59), C55(H55), C25(H25), C27(H27), C21(H21), C67(H67), C17(H17), C31(H31),
  C63(H63), C69(H69), C70(H70), C32(H32), C26(H26), C54(H54), C68(H68),
 C60(H60), C33(H33), C20(H20), C62(H62), C61(H61), C18(H18), C53(H53), C19(H19),
  C71(H71), C76(H76)
4.b Idealised Me refined as rotating group:
 C75(H75A,H75B,H75C), C74(H74A,H74B,H74C), C72(H72A,H72B,H72C), C73(H73A,H73B,
 H73C)
;
_shelx_res_checksum              37822
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.007
_oxdiff_exptl_absorpt_empirical_full_min 0.562