A nested spin structure and single molecule magnet behaviour in an Fe<sub>8</sub>Dy<sub>12</sub> heterometallic cyclic coordination cluster.
Peng, Yan; Braun, Jonas; Schulze, Michael; Kaemmerer, Hagen; Schneider, Yannik F.; Anson, Christopher E.; Wernsdorfer, Wolfgang; Powell, Annie K.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 894–897; doi:10.1039/d3dt04141g

data_7714769
_publ_section_title
;
 A nested spin structure and single molecule magnet behaviour in an
 Fe<sub>8</sub>Dy<sub>12</sub> heterometallic cyclic coordination cluster.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              894
_journal_page_last               897
_journal_paper_doi               10.1039/d3dt04141g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'C120 H252 Dy12 Fe8 N32 O96, 8(C2 H3 N), 6(C H4 O)'
_chemical_formula_sum            'C142 H300 Dy12 Fe8 N40 O102'
_chemical_formula_weight         6597.00
_space_group_crystal_system      tetragonal
_space_group_IT_number           142
_space_group_name_Hall           '-I 4bd 2c'
_space_group_name_H-M_alt        'I 41/a c d :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     'intrinsic phasing'
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-11-06
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-11-08 deposited with the CCDC.	2023-12-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   37.7905(13)
_cell_length_b                   37.7905(13)
_cell_length_c                   61.582(2)
_cell_measurement_reflns_used    9236
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.502
_cell_measurement_theta_min      2.678
_cell_volume                     87947(5)
_computing_cell_refinement       'Apex2 (Bruker AXS Inc., 2005)'
_computing_data_collection       'Apex2 (Bruker AXS Inc., 2005)'
_computing_data_reduction        'Apex2 (Bruker AXS Inc., 2005)'
_computing_molecular_graphics    'Diamond 2.1 (Crystal Impact, 1998)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker SMART Apex'
_diffrn_measurement_method       'CCD area detector, \w-scans'
_diffrn_radiation_monochromator  silicon
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.79942
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       74
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            139306
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        28.663
_diffrn_reflns_theta_max         30.395
_diffrn_reflns_theta_min         1.756
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    6.326
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.6221
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 (Bruker AXS Inc., 2005)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.993
_exptl_crystal_description       block
_exptl_crystal_F_000             51968
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         4.352
_refine_diff_density_min         -2.649
_refine_diff_density_rms         0.227
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.576
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1298
_refine_ls_number_reflns         22903
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.576
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0575
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0970P)^2^+87.4253P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1763
_refine_ls_wR_factor_ref         0.1996
_reflns_number_gt                18273
_reflns_number_total             22903
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04141g3.cif
_cod_data_source_block           p60302_sq
_cod_depositor_comments          'Adding full bibliography for 7714769.cif.'
_cod_original_cell_volume        87947(7)
_cod_original_sg_symbol_H-M      'I 41/a c d'
_cod_database_code               7714769
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.786
_shelx_estimated_absorpt_t_min   0.666
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, H12 of O12, H9 of O9, H18 of O18, H24 of O24, H27 of O27,
   H3 of O3, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H81 of O81
2. Restrained distances
 O3-H3 = O9-H9 = O18-H18 = O24-H24
 0.96 with sigma of 0.04
 O12-H12 = O27-H27
 0.88 with sigma of 0.04
 H3-O30_$1 = H9-O6 = H18-O15 = H24-O21
 1.6 with sigma of 0.04
 H12-O43_$2 = H27-O44
 2.08 with sigma of 0.04
 H81C-O34
 2.68 with sigma of 0.04
 N6-C31A \\sim N6-C31B \\sim N6-C33A \\sim N6-C33B \\sim N6-C35A \\sim N6-C35B
 with sigma of 0.02
 C31A-C32 \\sim C31B-C32 \\sim C33A-C34 \\sim C33B-C34 \\sim C35A-C36 \\sim
C35B-C36
 with sigma of 0.02
3. Others
 Fixed Sof: C31A(0.5) H31A(0.5) H31B(0.5) C31B(0.5) H31C(0.5) H31D(0.5)
 H32A(0.5) H32B(0.5) H32C(0.5) H32D(0.5) C33A(0.5) H33A(0.5) H33B(0.5)
 C33B(0.5) H33C(0.5) H33D(0.5) H34A(0.5) H34B(0.5) H34C(0.5) H34D(0.5)
 C35A(0.5) H35A(0.5) H35B(0.5) C35B(0.5) H35C(0.5) H35D(0.5) H36A(0.5)
 H36B(0.5) H36C(0.5) H36D(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B),
  C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,
 H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B),
 C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B),
  C31A(H31A,H31B), C31B(H31C,H31D), C32(H32A,H32B), C32(H32C,H32D), C33A(H33A,
 H33B), C33B(H33C,H33D), C34(H34A,H34B), C34(H34C,H34D), C35A(H35A,H35B),
 C35B(H35C,H35D), C36(H36A,H36B), C36(H36C,H36D), C37(H37A,H37B), C38(H38A,
 H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B),
 C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B),
  C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,
 H52B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B),
 C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B)
4.b Idealised Me refined as rotating group:
 C72(H72A,H72B,H72C), C74(H74A,H74B,H74C), C81(H81A,H81B,H81C)
4.c Idealised tetrahedral OH refined as rotating group:
 O81(H81)
;
_shelx_res_checksum              73247
_shelx_fab_checksum              9524
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'