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_7718028
_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 Dy4 N8 Ni8 O36, 6[H2O]'
_chemical_formula_sum            'C80 H112 Dy4 N8 Ni8 O42'
_chemical_formula_weight         2977.45
_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                 101.165(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.9513(16)
_cell_length_b                   19.9583(16)
_cell_length_c                   25.322(2)
_cell_measurement_reflns_used    9041
_cell_measurement_temperature    195(2)
_cell_measurement_theta_max      27.94
_cell_measurement_theta_min      2.62
_cell_volume                     10388.1(14)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      195(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  0.0578
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            126728
_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         28.334
_diffrn_reflns_theta_min         2.311
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.338
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6348
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1262 before and 0.0522 after correction.
The Ratio of minimum to maximum transmission is 0.8513.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.904
_exptl_crystal_description       Needle
_exptl_crystal_F_000             5888
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.822
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     626
_refine_ls_number_reflns         12917
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0402
_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^)+(0.0502P)^2^+62.0498P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.1076
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9989
_reflns_number_total             12917
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00175g2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7718028--7718030.cif.'
_cod_database_code               7718028
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.846
_shelx_estimated_absorpt_t_min   0.493
_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
 C29-C28 = C29-C28A
 1.54 with sigma of 0.02
 N3-C28 = N3-C28A
 1.45 with sigma of 0.02
3. Rigid body (RIGU) restrains
 N3, C29, C28, C28A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Fixed Sof: H29A(0.65) H29B(0.65) H29C(0.35) H29D(0.35) C28(0.65) H28A(0.65)
 H28B(0.65) C28A(0.35) H28C(0.35) H28D(0.35)
5.a Rotating group:
 O8(H8A,H8B), O13(H13A,H13B)
5.b Ternary CH refined with riding coordinates:
 O3(H3), O9(H9), O12(H12), O14(H14)
5.c Secondary CH2 refined with riding coordinates:
 C8(H8C,H8D), C9(H9A,H9B), C19(H19A,H19B), C20(H20A,H20B), C29(H29A,H29B),
 C29(H29C,H29D), C37(H37A,H37B), C38(H38A,H38B), C28(H28A,H28B), C28A(H28C,H28D)
5.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3A), C4(H4), C5(H5), C7(H7), C13(H13), C14(H14A), C15(H15),
 C16(H16), C18(H18), C22(H22), C23(H23), C24(H24), C25(H25), C27(H27), C31(H31),
  C32(H32), C33(H33), C34(H34), C36(H36)
5.e Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C40(H40A,H40B,H40C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              49128
_shelx_fab_checksum              46095
_olex2_submission_special_instructions 'No special instructions were received'