Structures and magnetic properties of novel Ln(iii)-based pentanuclear clusters: magnetic refrigeration and single-molecule magnet behavior
Wang, Wen-Min; Zhang, Tian-Tian; Wang, Dan; Cui, Jian-Zhong; New Journal of Chemistry 44 (2020) 19351–19359; doi:10.1039/D0NJ04469E

data_7060045
_publ_section_title
;
 Structures and magnetic properties of novel Ln(iii)-based pentanuclear
 clusters: magnetic refrigeration and single-molecule magnet behavior
;
_journal_issue                   44
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              19351
_journal_page_last               19359
_journal_paper_doi               10.1039/D0NJ04469E
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C71 H85 Ho5 N12 O30, 3[CH4O]'
_chemical_formula_sum            'C74 H97 Ho5 N12 O33'
_chemical_formula_weight         2507.30
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-10-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-10-08 deposited with the CCDC.	2020-10-13 downloaded from the CCDC.
;
_cell_angle_alpha                77.620(3)
_cell_angle_beta                 76.363(3)
_cell_angle_gamma                89.378(3)
_cell_formula_units_Z            2
_cell_length_a                   14.2798(10)
_cell_length_b                   15.9898(10)
_cell_length_c                   20.7864(14)
_cell_measurement_reflns_used    9287
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.47
_cell_measurement_theta_min      2.21
_cell_volume                     4501.2(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      149.99
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.976
_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  0.0778
_diffrn_reflns_av_unetI/netI     0.0541
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            93364
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.152
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.425
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5620
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1021 before and 0.0665 after correction.
The Ratio of minimum to maximum transmission is 0.7540.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.850
_exptl_crystal_description       block
_exptl_crystal_F_000             2340
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.963
_refine_diff_density_min         -0.681
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1085
_refine_ls_number_reflns         17923
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.0547
_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^)+(0.0675P)^2^+18.8896P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1352
_refine_ls_wR_factor_ref         0.1629
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10861
_reflns_number_total             17923
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj04469e2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7060044--7060049.cif.'
_cod_database_code               7060045
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.642
_shelx_estimated_absorpt_t_min   0.404
_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
2. Restrained distances
 H8-O19
 2.2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C40) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C39) \\sim Ueq, Uanis(C41) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C28(H28A,H28B), C19(H19A,H19B), C1(H1A,H1B)
4.b Aromatic/amide H refined with riding coordinates:
 C22(H22), C24(H24), C13(H13), C4(H4A), C12(H12A), C15(H15), C21(H21),
 C59(H59), C33(H33), C49(H49), C6(H6), C3(H3), C31(H31), C64(H64), C30(H30),
 C44(H44), C54(H54), C69(H69), C39(H39)
4.c Idealised Me refined as rotating group:
 C51(H51A,H51B,H51C), C36(H36A,H36B,H36C), C27(H27A,H27B,H27C), C62(H62A,H62B,
 H62C), C47(H47A,H47B,H47C), C56(H56A,H56B,H56C), C66(H66A,H66B,H66C), C18(H18A,
 H18B,H18C), C61(H61A,H61B,H61C), C9(H9A,H9B,H9C), C52(H52A,H52B,H52C),
 C67(H67A,H67B,H67C), C71(H71A,H71B,H71C), C41(H41A,H41B,H41C), C42(H42A,H42B,
 H42C), C46(H46A,H46B,H46C), C57(H57A,H57B,H57C), C37(H37A,H37B,H37C)
4.d Idealised tetrahedral OH refined as rotating group:
 O16(H16), O12(H12), O4(H4), O8(H8)
;
_shelx_res_checksum              391
_shelx_fab_checksum              20845
_olex2_submission_special_instructions 'No special instructions were received'