Structural and magnetic properties of lanthanide–tetraphenol–cyclen complexes: slow magnetic relaxation of the Nd(iii) complex
Massoud, Salah S.; Louka, Febee R.; Guizouarn, Thierry; Fischer, Roland C.; Torvisco, Ana; Mautner, Franz A.; Smith, Asia M.; Salem, Nahed M. H.; Velmurugan, Gunasekaran; Comba, Peter; Pointillart, Fabrice; New Journal of Chemistry  (2026) –; doi:10.1039/D5NJ03826J

data_7064183
_publ_section_title
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 Structural and magnetic properties of lanthanide--tetraphenol--cyclen
 complexes: slow magnetic relaxation of the Nd(iii) complex
;
_journal_name_full               'New Journal of Chemistry'
_journal_paper_doi               10.1039/D5NJ03826J
_journal_year                    2026
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C44 H57 Gd N4 O4, C H4 O'
_chemical_formula_sum            'C45 H61 Gd N4 O5'
_chemical_formula_weight         895.22
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-09-18
_audit_creation_method
;
Olex2 1.5-ac7-018
(compiled 2025.08.06 svn.rb7424aed for Rigaku Oxford Diffraction, GUI svn.r7314)
;
_audit_update_record
;
2025-09-19 deposited with the CCDC.	2025-11-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.8229(4)
_cell_length_b                   12.4491(4)
_cell_length_c                   22.4326(8)
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    99.98
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.44
_cell_volume                     4139.5(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5-ac7-018 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac7-018 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXD  (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.98
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1025
_diffrn_reflns_av_unetI/netI     0.0641
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            112309
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.328
_diffrn_reflns_theta_min         2.136
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           0.89
_diffrn_source_power             0.0445
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.652
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4773
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1532 before and 0.1005 after correction.
The Ratio of minimum to maximum transmission is 0.6401.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_description       Block
_exptl_crystal_F_000             1852
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.461
_refine_diff_density_min         -3.673
_refine_diff_density_rms         0.119
_refine_ls_abs_structure_details
;
 Flack x determined using 3596 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.011(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         10167
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0409
_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^)+8.9716P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.0734
_reflns_Friedel_coverage         0.924
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.971
_reflns_number_gt                8798
_reflns_number_total             10167
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj03826j2.cif
_cod_data_source_block           rf2302a_d
_cod_database_code               7064183
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.879
_shelx_estimated_absorpt_t_min   0.790
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C21(H21a,H21b), C12(H12a,H12b), C1(H1a,H1b), C34(H34a,H34b), C22(H22a,H22b),
 C11(H11a,H11b), C10(H10a,H10b), C44(H44a,H44b), C43(H43a,H43b), C33(H33a,H33b),
  C32(H32a,H32b), C23(H23a,H23b)
2.b Aromatic/amide H refined with riding coordinates:
 C27(H27), C29(H29), C16(H16), C18(H18), C5(H5), C7(H7), C38(H38), C40(H40)
2.c Idealised Me refined as rotating group:
 C30(H30a,H30b,H30c), C31(H31a,H31b,H31c), C19(H19a,H19b,H19c), C20(H20a,H20b,
 H20c), C8(H8a,H8b,H8c), C9(H9a,H9b,H9c), C41(H41a,H41b,H41c), C42(H42a,H42b,
 H42c), C45(H45a,H45b,H45c)
2.d Idealised tetrahedral OH refined as rotating group:
 O4(H4), O5(H5a)
;
_shelx_res_checksum              45369
_olex2_submission_special_instructions 'No special instructions were received'