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_7064182
_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_formula_moiety         'C40 H45 Cl4 Ho N4 O4, 2[H2O]'
_chemical_formula_sum            'C40 H49 Cl4 Ho N4 O6'
_chemical_formula_weight         988.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_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                 102.217(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1871(6)
_cell_length_b                   18.6904(8)
_cell_length_c                   17.0530(6)
_cell_measurement_reflns_used    9959
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.87
_cell_measurement_theta_min      2.44
_cell_volume                     4107.9(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      99.99
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0795
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_Laue_measured_fraction_full 0.999
_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       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            81536
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.036
_diffrn_reflns_theta_min         2.088
_diffrn_source_current           0.89
_diffrn_source_power             0.0445
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.237
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6155
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.1022 before and 0.0602 after correction.
The Ratio of minimum to maximum transmission is 0.8255.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_description       block
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.742
_refine_diff_density_min         -1.143
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         9945
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0327
_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^)+(0.0149P)^2^+5.1612P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0550
_refine_ls_wR_factor_ref         0.0590
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8019
_reflns_number_total             9945
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj03826j2.cif
_cod_data_source_block           rf2290_0m_c
_cod_database_code               7064182
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.841
_shelx_estimated_absorpt_t_min   0.702
_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, All O(H,H) groups
2. Others
 Sof(O6)=Sof(H6A)=Sof(H6B)=1-FVAR(1)
 Sof(O5)=Sof(H5A)=Sof(H5B)=FVAR(1)
 Sof(O9)=Sof(H9C)=Sof(H9D)=1-FVAR(2)
 Sof(O7)=Sof(H7A)=Sof(H7B)=FVAR(2)
3.a Free rotating group:
 O6(H6A,H6B), O9(H9C,H9D), O5(H5A,H5B), O7(H7A,H7B)
3.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C19(H19A,H19B), C20(H20A,H20B), C29(H29A,H29B),
 C39(H39A,H39B), C30(H30A,H30B), C1(H1A,H1B), C40(H40A,H40B), C11(H11A,H11B),
 C21(H21A,H21B), C31(H31A,H31B)
3.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C15(H15), C17(H17), C25(H25), C27(H27), C35(H35), C37(H37)
3.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C18(H18A,H18B,H18C), C28(H28A,H28B,H28C), C38(H38A,H38B,H38C)
3.e Idealised tetrahedral OH refined as rotating group:
 O4(H4)
;
_shelx_res_checksum              99239
_olex2_submission_special_instructions 'No special instructions were received'