Dodecanuclear [NiII8Ln<sub>4</sub>] clusters and rings of corner-sharing {NiII2Ln<sub>2</sub>} cubanes (Ln = Dy, Gd, Y); magnetic and magnetothermal properties.
Tziotzi, Thomais G.; Agapaki, Eleftheria; Charkiolakis, Emmanouil K.; Gracia, David; Ubach I Cervera, Marc; Dalgarno, Scott J.; Evangelisti, Marco; Brechin, Euan K.; Milios, Constantinos J.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 4664–4671; doi:10.1039/d5dt00175g

data_7718029
_publ_section_title
;
 Dodecanuclear [NiII8Ln<sub>4</sub>] clusters and rings of corner-sharing
 {NiII2Ln<sub>2</sub>} cubanes (Ln = Dy, Gd, Y); magnetic and
 magnetothermal properties.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4664
_journal_page_last               4671
_journal_paper_doi               10.1039/d5dt00175g
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C80 H100 N8 Ni8 O36 Y4, 10[H2O]'
_chemical_formula_sum            'C80 H120 N8 Ni8 O46 Y4'
_chemical_formula_weight         2755.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-12-13
_audit_creation_method
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-12-13 deposited with the CCDC.	2025-02-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.3760(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.9054(7)
_cell_length_b                   19.9035(6)
_cell_length_c                   26.4714(8)
_cell_measurement_reflns_used    9962
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      25.93
_cell_measurement_theta_min      2.19
_cell_volume                     10798.1(6)
_computing_cell_refinement       'SAINT Bruker-AXS, Madison WI'
_computing_data_collection       'Bruker APEX2 Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT Bruker-AXS, Madison WI'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      220(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_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  0.0857
_diffrn_reflns_av_unetI/netI     0.0701
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            85906
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.757
_diffrn_reflns_theta_min         2.261
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.571
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6617
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1361 before and 0.0574 after correction.
The Ratio of minimum to maximum transmission is 0.8872.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_description       block
_exptl_crystal_F_000             5616
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.370
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     678
_refine_ls_number_reflns         13988
_refine_ls_number_restraints     140
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1236
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0456P)^2^+23.4091P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1107
_refine_ls_wR_factor_ref         0.1348
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7166
_reflns_number_total             13988
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00175g2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7718028--7718030.cif.'
_cod_database_code               7718029
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.435
_shelx_estimated_absorpt_t_min   0.344
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 C30-C31 = C29-C31
 1.54 with sigma of 0.02
 N3-C30 = N3-C29
 1.45 with sigma of 0.02
 C34-C32 = C33-C32 = C12-C10 = C11-C10
 1.54 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C1, C2, C3, C4, C5, C6
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C35, C36, C37, C38, C39, C40
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C32, O17, O19, C33, O16, O18, C34
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C29, C31, C30, O13, N3
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Fixed Sof: H31A(0.6) H31B(0.6) H31C(0.4) H31D(0.4) O5(0.5) O7(0.5) O17(0.5)
 O19(0.5) C12(0.5) H12A(0.5) H12B(0.5) H12C(0.5) C29(0.6) H29A(0.6) H29B(0.6)
 C33(0.5) H33A(0.5) H33B(0.5) H33C(0.5) O6(0.5) O8(0.5) O16(0.5) O18(0.5)
 C11(0.5) H11A(0.5) H11B(0.5) H11C(0.5) C30(0.4) H30A(0.4) H30B(0.4) C34(0.5)
 H34A(0.5) H34B(0.5) H34C(0.5)
5.a Rotating group:
 O3(H3A,H3B), O15(H15A,H15B)
5.b Ternary CH refined with riding coordinates:
 O4(H4), O11(H11), O14(H14), O20(H20)
5.c Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C20(H20A,H20B), C21(H21A,H21B), C31(H31A,H31B),
 C31(H31C,H31D), C42(H42A,H42B), C43(H43A,H43B), C29(H29A,H29B), C30(H30A,H30B)
5.d Me refined with riding coordinates:
 C12(H12A,H12B,H12C), C33(H33A,H33B,H33C), C11(H11A,H11B,H11C), C34(H34A,H34B,
 H34C)
5.e Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4A), C5(H5), C7(H7), C14(H14A), C15(H15), C16(H16),
 C17(H17), C19(H19), C23(H23), C24(H24), C25(H25), C26(H26), C28(H28), C36(H36),
  C37(H37), C38(H38), C39(H39), C41(H41)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              71031
_shelx_fab_checksum              80063
_olex2_submission_special_instructions 'No special instructions were received'