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_7064181
_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 Ho N4 O4, C H4 O'
_chemical_formula_sum            'C45 H61 Ho N4 O5'
_chemical_formula_weight         902.90
_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                   14.9515(7)
_cell_length_b                   12.4578(6)
_cell_length_c                   22.3763(11)
_cell_measurement_reflns_used    9729
_cell_measurement_temperature    99.97
_cell_measurement_theta_max      27.85
_cell_measurement_theta_min      2.31
_cell_volume                     4167.9(3)
_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      99.97
_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 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.1010
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            235200
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.712
_diffrn_reflns_theta_min         2.128
_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    1.948
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5424
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1507 before and 0.1080 after correction.
The Ratio of minimum to maximum transmission is 0.7273.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_description       block
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.851
_refine_diff_density_min         -1.054
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
 Flack x determined using 4252 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.028(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         10760
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0274
_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^)+(0.0240P)^2^+3.0210P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0572
_refine_ls_wR_factor_ref         0.0614
_reflns_Friedel_coverage         0.947
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                9522
_reflns_number_total             10760
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj03826j2.cif
_cod_data_source_block           rf2298a_0m_d
_cod_database_code               7064181
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.844
_shelx_estimated_absorpt_t_min   0.733
_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:
 C33(H33A,H33B), C43(H43A,H43B), C23(H23A,H23B), C22(H22A,H22B), C11(H11A,
 H11B), C32(H32A,H32B), C1(H1A,H1B), C44(H44A,H44B), C34(H34A,H34B), C21(H21A,
 H21B), C10(H10A,H10B), C12(H12A,H12B)
2.b Aromatic/amide H refined with riding coordinates:
 C40(H40), C38(H38), C29(H29), C7(H7), C18(H18), C5(H5), C27(H27), C16(H16)
2.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C41(H41A,H41B,H41C), C8(H8A,H8B,H8C), C42(H42A,H42B,
 H42C), C31(H31A,H31B,H31C), C19(H19A,H19B,H19C), C9(H9A,H9B,H9C), C45(H45A,
 H45B,H45C), C20(H20A,H20B,H20C)
2.d Idealised tetrahedral OH refined as rotating group:
 O4(H4), O5(H5A)
;
_shelx_res_checksum              98599
_olex2_submission_special_instructions 'No special instructions were received'