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_7718030
_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 Gd4 N8 Ni8 O36, 24[H2O]'
_chemical_formula_sum            'C80 H148 Gd4 N8 Ni8 O60'
_chemical_formula_weight         3280.74
_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                 101.119(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.9663(10)
_cell_length_b                   20.0465(9)
_cell_length_c                   26.2609(13)
_cell_measurement_reflns_used    9097
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      28.87
_cell_measurement_theta_min      2.28
_cell_volume                     10830.3(9)
_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      210(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0573
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            314922
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.153
_diffrn_reflns_theta_min         2.180
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.874
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1281 before and 0.0599 after correction.
The Ratio of minimum to maximum transmission is 0.9241.
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    2.012
_exptl_crystal_description       block
_exptl_crystal_F_000             6576
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.377
_refine_diff_density_min         -1.710
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     673
_refine_ls_number_reflns         14593
_refine_ls_number_restraints     192
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0514
_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^)+(0.0400P)^2^+116.8280P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1170
_refine_ls_wR_factor_ref         0.1225
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12456
_reflns_number_total             14593
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00175g2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7718028--7718030.cif.'
_cod_database_code               7718030
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.542
_shelx_estimated_absorpt_t_min   0.389
_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, All O(H,H) groups
2. Rigid body (RIGU) restrains
 C37, O9, O13, C39, O12, O14, C38
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N4, C28, C29, C30, C31, C32, C33, C34, C35, C36, O8, O7
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N3, C19, C20, C21, C22, C23, C24, C25, C26, C27, O6, O5
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3. Others
 Fixed Sof: O9(0.4) O13(0.4) O16(0.5) O20(0.5) C39(0.4) H39A(0.4) H39B(0.4)
 H39C(0.4) C42(0.5) H42A(0.5) H42B(0.5) H42C(0.5) O12(0.6) O14(0.6) O15(0.5)
 O19(0.5) C38(0.6) H38A(0.6) H38B(0.6) H38C(0.6) C41(0.5) H41A(0.5) H41B(0.5)
 H41C(0.5)
4.a Rotating group:
 O22(H22A,H22B), O25(H25A,H25B)
4.b Ternary CH refined with riding coordinates:
 O21(H21), O23(H23), O24(H24), O26(H26)
4.c Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C17(H17A,H17B), C18(H18A,H18B), C26(H26A,H26B),
 C27(H27A,H27B), C35(H35A,H35B), C36(H36A,H36B)
4.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C11(H11), C12(H12), C13(H13),
 C14(H14), C16(H16), C20(H20), C21(H21A), C22(H22), C23(H23A), C25(H25),
 C29(H29), C30(H30), C31(H31), C32(H32), C34(H34)
4.e Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C42(H42A,H42B,H42C), C38(H38A,H38B,H38C), C41(H41A,H41B,
 H41C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              55561
_shelx_fab_checksum              37306
_olex2_submission_special_instructions 'No special instructions were received'