Different mechanisms for lanthanide(III) sensitization and Yb-field-induced single-molecule magnet behaviour in a series of pentagonal bipyramidal and octahedral lanthanide complexes with axial phosphine oxide ligands.
Allia, Hadjer; Rodríguez Expósito, Ana; Palacios, Maria A.; Jiménez, Juan Ramón; Carneiro Neto, Albano; Moura Jr., Renaldo T.; Piccinelli, Fabio; Navarro, Amparo; Quesada-Moreno, María Mar; Colacio, Enrique; Physical Chemistry Chemical Physics  (2025) –; doi:10.1039/D4CP04862H

data_7250340
_publ_section_title
;
 Different mechanisms for lanthanide(III) sensitization and
 Yb-field-induced single-molecule magnet behaviour in a series of
 pentagonal bipyramidal and octahedral lanthanide complexes with axial
 phosphine oxide ligands.
;
_journal_name_full               'Physical Chemistry Chemical Physics'
_journal_paper_doi               10.1039/D4CP04862H
_journal_year                    2025
_chemical_formula_moiety         'C27 H37 Cl0.5 O3 P Yb0.5, Cl, C4 H8 O'
_chemical_formula_sum            'C31 H49 Cl1.5 O4 P Yb0.5'
_chemical_formula_weight         656.36
_space_group_crystal_system      tetragonal
_space_group_IT_number           80
_space_group_name_Hall           'I 4bw'
_space_group_name_H-M_alt        'I 41'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-12-19
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-12-19 deposited with the CCDC.	2025-04-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.1565(11)
_cell_length_b                   24.1565(11)
_cell_length_c                   12.1744(8)
_cell_measurement_reflns_used    9128
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      30.530
_cell_measurement_theta_min      2.385
_cell_volume                     7104.2(7)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'four-circle diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0635
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            64202
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.537
_diffrn_reflns_theta_min         2.385
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.520
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5597
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1083 before and 0.0733 after correction.
The Ratio of minimum to maximum transmission is 0.7502.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2740
_refine_diff_density_max         1.865
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.138
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.029(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         10751
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0386
_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^)+(0.0644P)^2^+5.9490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1109
_reflns_Friedel_coverage         0.898
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.978
_reflns_number_gt                9282
_reflns_number_total             10751
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cp04862h2.cif
_cod_data_source_block           compound_1
_cod_original_cell_volume        7104.2(8)
_cod_original_formula_sum        'C31 H49 Cl1.50 O4 P Yb0.50'
_cod_database_code               7250340
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.971(12)
 0.029(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(Cl2) = Uanis(Cl2A)
4. Others
 Fixed Sof: Cl2(0.5) Cl2A(0.5)
5.a Ternary CH refined with riding coordinates:
 C12(H12), C16(H16), C4(H4), C2(H2), C8(H8), C14(H14)
5.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C13(H13A,H13B), C11(H11A,H11B), C5(H5A,H5B), C3(H3A,H3B),
 C9(H9A,H9B), C20(H20A,H20B), C1(H1A,H1B), C10(H10A,H10B), C21(H21A,H21B),
 C15(H15A,H15B), C7(H7A,H7B), C17(H17A,H17B), C31(H31A,H31B), C30(H30A,H30B),
 C28(H28A,H28B), C29(H29A,H29B)
5.c Aromatic/amide H refined with riding coordinates:
 C24(H24), C26(H26), C27(H27), C23(H23), C25(H25)
;
_shelx_res_checksum              23488
_olex2_submission_special_instructions 'No special instructions were received'