Synthesis, structures, and magnetic properties of butterfly-shaped hexanuclear [FeIII4LnIII2] single-molecule magnets
Liu, Shujing; Zou, Chen; Wang, Hanjie; Chen, Sihuai; Yuan, Jun; Jia, Lihui; CrystEngComm 25 (2023) 5893–5899; doi:10.1039/D3CE00824J

data_7247426
_publ_section_title
;
 Synthesis, structures, and magnetic properties of butterfly-shaped
 hexanuclear [FeIII4LnIII2] single-molecule magnets
;
_journal_issue                   42
_journal_name_full               CrystEngComm
_journal_page_first              5893
_journal_page_last               5899
_journal_paper_doi               10.1039/D3CE00824J
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C30 H72 Dy2 Fe4 N10 O28, 4(C H4 O)'
_chemical_formula_sum            'C34 H88 Dy2 Fe4 N10 O32'
_chemical_formula_weight         1697.54
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-09
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-07-03 deposited with the CCDC.	2023-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                80.21(3)
_cell_angle_beta                 80.56(3)
_cell_angle_gamma                75.51(3)
_cell_formula_units_Z            1
_cell_length_a                   11.053(12)
_cell_length_b                   11.220(12)
_cell_length_c                   13.170(14)
_cell_measurement_reflns_used    5919
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      23.54
_cell_measurement_theta_min      2.33
_cell_volume                     1546(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0623
_diffrn_reflns_av_unetI/netI     0.0461
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            41831
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        24.956
_diffrn_reflns_theta_max         24.956
_diffrn_reflns_theta_min         2.554
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    3.393
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5833
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0985 before and 0.0672 after correction.
The Ratio of minimum to maximum transmission is 0.7827.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.824
_exptl_crystal_description       block
_exptl_crystal_F_000             854
_refine_diff_density_max         0.890
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         5371
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0354
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0090P)^2^+4.3226P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0569
_refine_ls_wR_factor_ref         0.0632
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4472
_reflns_number_total             5371
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00824j2.cif
_cod_data_source_block           0904lsj12_0m
_cod_depositor_comments
'Adding full bibliography for 7247426--7247427.cif.'
_cod_database_code               7247426
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  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. Restrained distances
 Dy1-H8A \\sim Dy1-H8B
 with sigma of 0.02
3.a Free rotating group:
 O8(H8A,H8B)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C13(H13A,H13B), C4(H4A,H4B), C2(H2A,H2B), C6(H6A,H6B), C5(H5A,
 H5B), C9(H9A,H9B), C18(H18A,H18B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,
 H12B), C14(H14A,H14B)
3.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C8(H8C,H8D,H8E), C16(H16A,H16B,H16C), C15(H15A,H15B,H15C),
 C17(H17A,H17B,H17C)
3.d Idealised tetrahedral OH refined as rotating group:
 O16(H16), O15(H15)
;
_shelx_res_checksum              41129
_olex2_submission_special_instructions 'No special instructions were received'