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_7251668
_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(C17.109 H16 Dy F4.664 N4 O7.555), 8(C14 H8 N4), 4(H2 O), C2 H F3 O2, C2 F3 O2, O, 0.891(C O), 2.672(F)'
_chemical_formula_sum            'C152 H104 Dy2 F18 N40 O25'
_chemical_formula_weight         3557.75
_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     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc2px0wj
_audit_creation_date             2025-10-27
_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                64.113(3)
_cell_angle_beta                 79.651(2)
_cell_angle_gamma                84.287(2)
_cell_formula_units_Z            1
_cell_length_a                   14.9545(3)
_cell_length_b                   16.3086(5)
_cell_length_c                   17.4443(5)
_cell_measurement_reflns_used    8600
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      29.3756
_cell_measurement_theta_min      2.1130
_cell_volume                     3764.2(2)
_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
;
Superflip  (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0648
_diffrn_reflns_av_unetI/netI     0.0570
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            52526
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.937
_exptl_absorpt_coefficient_mu    1.093
_exptl_absorpt_correction_type   none
_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    1.569
_exptl_crystal_description       block
_exptl_crystal_F_000             1790
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.411
_refine_diff_density_min         -1.177
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1188
_refine_ls_number_reflns         13273
_refine_ls_number_restraints     333
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0557
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0984P)^2^+2.1720P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1478
_refine_ls_wR_factor_ref         0.1577
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10557
_reflns_number_total             13273
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce01195g2.cif
_cod_data_source_block           a
_cod_depositor_comments
'Adding full bibliography for 7251667--7251669.cif.'
_cod_database_code               7251668
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.889
_shelx_estimated_absorpt_t_min   0.871
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 C2-C1
 1.548 with sigma of 0.011
 O5-C1
 1.255 with sigma of 0.01
 O8-C1
 1.225 with sigma of 0.01
 O13-H13B = O13-H13A
 0.85 with sigma of 0.002
 H13B-H13A
 1.34 with sigma of 0.002
 C01L-C01H
 1.32 with sigma of 0.01
 O12-C5
 1.255 with sigma of 0.01
 O11-C5
 1.225 with sigma of 0.01
 C6-C5
 1.548 with sigma of 0.011
 F9-C6 = F7-C6 = F8-C6
 1.32 with sigma of 0.01
 O9-C7
 1.225 with sigma of 0.01
 F10-C8 = F12-C8 = F11-C8
 1.32 with sigma of 0.01
 O10-C7
 1.255 with sigma of 0.01
 C8-C7
 1.548 with sigma of 0.011
 F12-C7
 2.282 with sigma of 0.01
 C7-F10
 2.282 with sigma of 0.01
 F11-C7
 2.282 with sigma of 0.01
 F4-F5 \\sim F5-F6 \\sim F6-F4
 with sigma of 0.02
 F7-F8 \\sim F8-F9 \\sim F9-F7
 with sigma of 0.02
 F10-F11 \\sim F11-F12 \\sim F12-F10
 with sigma of 0.02
 Dy1-H3A \\sim Dy1-H3B
 with sigma of 0.02
 Dy1-H2A \\sim Dy1-H2B
 with sigma of 0.02
 F10-C7 \\sim C7-F12
 with sigma of 0.02
 F12-C7 \\sim C7-F11
 with sigma of 0.02
 F11-C7 \\sim C7-F10
 with sigma of 0.02
 C2-F3A \\sim C2-F3B
 with sigma of 0.02
 F2B-F1B \\sim F2C-F1C
 with sigma of 0.02
 C2-F2B \\sim C2-F2C
 with sigma of 0.04
 C2-F1B \\sim C2-F1C
 with sigma of 0.04
 O6-C4A \\sim O6-C4B
 with sigma of 0.02
 O7-C4A \\sim O7A-C4B
 with sigma of 0.02
 O6-O7 \\sim O6-O7A
 with sigma of 0.04
 F4-F5 \\sim F4A-F5A
 with sigma of 0.04
 F4-F6 \\sim F4A-F6A
 with sigma of 0.04
 F4-C4A \\sim F4A-C4B
 with sigma of 0.04
 F5-F6 \\sim F5A-F6A
 with sigma of 0.04
 F5-C4A \\sim F5A-C4B
 with sigma of 0.04
 F6-C4A \\sim F6A-C4B
 with sigma of 0.04
3. Restrained planarity
 O5, C1, O8, C2
 with sigma of 0.1
 O9, C7, O10, C8
 with sigma of 0.1
4. Rigid bond restraints
 F2C, C2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C2, F3B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Uiso/Uaniso restraints and constraints
O6 \\sim O7 \\sim F4 \\sim C4 \\sim F5 \\sim F6: within 3A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 3A
O6 \\sim O7 \\sim F3A \\sim C4A \\sim F6 \\sim C4 \\sim F4 \\sim F5: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C1 \\sim C2 \\sim F3A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O12 \\sim C5 \\sim C6 \\sim F7 \\sim F9 \\sim F8: within 3A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 3A
O9 \\sim C7 \\sim O10: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C1 \\sim C2: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
F10 \\sim F11: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C2 \\sim F2B \\sim F1B \\sim F3A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
Uanis(O15) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O12) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6)
\\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F7) \\sim Ueq: with
sigma of 0.01 and sigma for terminal atoms of 0.02
6. Rigid body (RIGU) restrains
 F1B, F2B, C2, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C2, H14B, F3A, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
7. Others
 Sof(F3B)=Sof(F2C)=Sof(F1C)=1-FVAR(1)
 Sof(F3A)=Sof(F2B)=Sof(F1B)=FVAR(1)
 Sof(C4B)=Sof(O7A)=Sof(F6A)=Sof(F4A)=Sof(F5A)=1-FVAR(2)
 Sof(O7)=Sof(C4)=Sof(F4)=Sof(F5)=Sof(F6)=Sof(C4A)=FVAR(2)
 Fixed Sof: O12(0.5) H12(0.5) O11(0.5) F7(0.5) C5(0.5) F8(0.5) C6(0.5) F9(0.5)
 O9(0.5) C7(0.5) O10(0.5) F10(0.5) F11(0.5) C8(0.5) F12(0.5) O15(0.5)
 Fixed X: O7(0.476093)
 Fixed Y: O7(0.627316)
 Fixed Z: O7(0.223487)
8.a Riding coordinates:
 O1(H1A,H1B), O14(H14A,H14B), O13(H13A,H13B)
8.b Free rotating group:
 O3(H3A,H3B), O2(H2A,H2B)
8.c Rotating group:
 O4(H4A,H4B)
8.d Aromatic/amide H refined with riding coordinates:
 C011(H011), C017(H017), C01B(H01B), C01J(H01J), C01P(H01P), C01Q(H01Q),
 C01U(H01U), C01V(H01V), C01W(H01W), C01X(H01X), C01Y(H01Y), C020(H020),
 C021(H021), C022(H022), C023(H023), C024(H024), C025(H025), C026(H026),
 C027(H027), C028(H028), C029(H029), C02A(H02A), C02B(H02B), C02C(H02C),
 C02D(H02D), C02E(H02E), C02F(H02F), C02G(H02G), C02H(H02H), C02I(H02I),
 C02J(H02J), C02K(H02K), C02L(H02L), C02M(H02M), C02N(H02N), C02P(H02P),
 C02Q(H02Q), C02R(H02R), C02S(H02S), C02U(H02U)
8.e Tetrahedral OH refined with riding coordinates:
 O12(H12)
;
_shelx_res_checksum              95323
_olex2_submission_special_instructions 'No special instructions were received'