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_7064180
_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         'C44 H57 N4 Nd O4, C H4 O'
_chemical_formula_sum            'C45 H61 N4 Nd O5'
_chemical_formula_weight         882.21
_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                   14.7750(10)
_cell_length_b                   12.4393(9)
_cell_length_c                   22.4001(16)
_cell_measurement_reflns_used    9105
_cell_measurement_temperature    99.99
_cell_measurement_theta_max      28.36
_cell_measurement_theta_min      2.33
_cell_volume                     4116.9(5)
_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  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXD  (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.99
_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 0.995
_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  0.1864
_diffrn_reflns_av_unetI/netI     0.1378
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_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       -28
_diffrn_reflns_number            55195
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.492
_diffrn_reflns_theta_min         2.140
_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    1.311
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5653
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.1593 before and 0.0790 after correction.
The Ratio of minimum to maximum transmission is 0.7581.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_description       Block
_exptl_crystal_F_000             1836
_exptl_crystal_size_max          0.154
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.044
_refine_diff_density_min         -1.666
_refine_diff_density_rms         0.150
_refine_ls_abs_structure_details
;
 Flack x determined using 2680 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.027(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         10189
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.0949
_refine_ls_R_factor_gt           0.0414
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0020P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0634
_refine_ls_wR_factor_ref         0.0765
_reflns_Friedel_coverage         0.916
_reflns_Friedel_fraction_full    0.986
_reflns_Friedel_fraction_max     0.960
_reflns_number_gt                6958
_reflns_number_total             10189
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj03826j2.cif
_cod_data_source_block           rf2304_pca21
_cod_database_code               7064180
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.925
_shelx_estimated_absorpt_t_min   0.824
_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:
 C1(H1A,H1B), C2(H2A,H2B), C4(H4A,H4B), C3(H3A,H3B), C5(H5A,H5B), C8(H8A,H8B),
 C7(H7A,H7B), C6(H6A,H6B), C9(H9A,H9B), C18(H18A,H18B), C27(H27A,H27B),
 C36(H36A,H36B)
2.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C15(H15), C24(H24), C22(H22), C31(H31), C33(H33), C40(H40), C42(H42)
2.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C26(H26A,H26B,H26C), C25(H25A,H25B,
 H25C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C43(H43A,H43B,H43C), C44(H44A,
 H44B,H44C), C45(H45A,H45B,H45C)
2.d Idealised tetrahedral OH refined as rotating group:
 O4(H4), O5(H5)
;
_shelx_res_checksum              40691
_olex2_submission_special_instructions 'No special instructions were received'