Cubane lanthanoid complexes with tridentate [O, PO, O] coordination using tris(5-<i>tert</i>-butyl-2-hydroxyphenyl)-phosphine oxide ligands: synthesis, characterisation, and magnetic behaviour.
Mangundu, Patrick; Ho, Curtis C.; Mole, Richard A.; Korb, Marcus; Fuller, Rebecca O.; Dalton transactions (Cambridge, England : 2003) 55 (2026) 5408–5415; doi:10.1039/d5dt02969d

data_7720582
_publ_section_title
;
 Cubane lanthanoid complexes with tridentate [O, P&#xe001;O, O]
 coordination using tris(5-<i>tert</i>-butyl-2-hydroxyphenyl)-phosphine
 oxide ligands: synthesis, characterisation, and magnetic behaviour.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5408
_journal_page_last               5415
_journal_paper_doi               10.1039/d5dt02969d
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety
'C126.40 H172.80 O24 P4 Tb4, 4.8(C2 H6 O) [+ solvent]'
_chemical_formula_sum            'C136 H201.6 O28.8 P4 Tb4'
_chemical_formula_weight         3056.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2025-09-27 deposited with the CCDC.	2026-02-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.7870(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.39750(10)
_cell_length_b                   35.3854(3)
_cell_length_c                   28.9254(2)
_cell_measurement_reflns_used    74728
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.1840
_cell_measurement_theta_min      2.8870
_cell_volume                     15574.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.43.129a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.129a 64-bit (release 29-06-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.129a (Rigaku OD, 2024)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0897
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            223575
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.499
_diffrn_reflns_theta_max         66.499
_diffrn_reflns_theta_min         2.904
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    9.642
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.661
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.129a (Rigaku Oxford Diffraction, 2024)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_description       plate
_exptl_crystal_F_000             6272
_exptl_crystal_size_max          0.214
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.028
_refine_diff_density_max         2.605
_refine_diff_density_min         -1.256
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1607
_refine_ls_number_reflns         27407
_refine_ls_number_restraints     1782
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0572
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0636P)^2^+90.3870P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1476
_refine_ls_wR_factor_ref         0.1519
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23479
_reflns_number_total             27407
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02969d5.cif
_cod_data_source_block           MK-B-74-Tb
_cod_depositor_comments
'Adding full bibliography for 7720582--7720584.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C136 H201.60 O28.80 P4 Tb4'
_cod_database_code               7720582
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.237
_shelx_estimated_absorpt_t_max   0.761
_oxdiff_exptl_absorpt_empirical_full_min 0.623
_oxdiff_exptl_absorpt_empirical_full_max 2.572
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              61636
_shelx_fab_checksum              37239