Trends in trigonal prismatic Ln-[1]ferrocenophane complexes and discovery of a Ho3+ single-molecule magnet
Latendresse, Trevor P.; Vieru, Veacheslav; Upadhyay, Apoorva; Bhuvanesh, Nattamai S.; Chibotaru, Liviu F.; Nippe, Michael; Chemical Science 11 (2020) 3936–3951; doi:10.1039/D0SC01197E

data_1557650
_publ_section_title
;
 Trends in trigonal prismatic Ln-[1]ferrocenophane complexes and discovery
 of a Ho3+ single-molecule magnet
;
_journal_issue                   15
_journal_name_full               'Chemical Science'
_journal_page_first              3936
_journal_page_last               3951
_journal_paper_doi               10.1039/D0SC01197E
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C40 H44 Fe3 Ho Li2 O2, C20 H40 Li O4'
_chemical_formula_sum            'C60 H84 Fe3 Ho Li3 O6'
_chemical_formula_weight         1254.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-04-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-27 deposited with the CCDC.	2020-03-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.3440(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3389(4)
_cell_length_b                   13.7172(5)
_cell_length_c                   36.2329(12)
_cell_measurement_reflns_used    9452
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      28.618
_cell_measurement_theta_min      2.259
_cell_volume                     5611.1(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS, 2016)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      110.0
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker PHOTON-II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            187062
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.336
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.204
_exptl_absorpt_correction_T_max  0.2632
_exptl_absorpt_correction_T_min  0.1677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1402 before and 0.0590 after correction. The Ratio of minimum to maximum transmission is 0.6372. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_description       block
_exptl_crystal_F_000             2584
_exptl_crystal_size_max          0.124
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.073
_refine_diff_density_max         1.386
_refine_diff_density_min         -1.480
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.353
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     773
_refine_ls_number_reflns         9565
_refine_ls_number_restraints     825
_refine_ls_restrained_S_all      1.340
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.0931
_refine_ls_shift/su_max          0.293
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0483P)^2^+43.2222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1648
_refine_ls_wR_factor_ref         0.1666
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9096
_reflns_number_total             9565
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc01197e2.cif
_cod_data_source_block           tl080
_cod_depositor_comments
;Adding full bibliography for 1557647--1557656.cif.

 Adding full bibliography for 1557647--1557656.cif.
;
_cod_database_code               1557650
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.856
_shelx_estimated_absorpt_t_min   0.772
_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
2. Shared sites
{O1C, O1D}
3. Restrained distances
 C36-C40
 1.52 with sigma of 0.02
 C15C-C14C
 1.52 with sigma of 0.01
 C31-C32 \\sim C32-C33 \\sim C33-C34
 with sigma of 0.02
 O1-C31 \\sim O1-C34
 with sigma of 0.02
 O1-C32 \\sim O1-C33
 with sigma of 0.04
 C32-C34 \\sim C31-C33
 with sigma of 0.04
 C39-C38 \\sim C38-C37 \\sim C37-C36
 with sigma of 0.02
 O2-C39 \\sim O2-C36
 with sigma of 0.02
 O2-C38 \\sim O2-C37
 with sigma of 0.04
 C38-C36 \\sim C39-C37
 with sigma of 0.04
 O1-Li1 \\sim O1A-Li1
 with sigma of 0.005
 O2A-Li2 \\sim O2-Li2
 with sigma of 0.005
 O1C-Li1C \\sim O1D-Li1C
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
O1 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim O1A \\sim C31A \\sim C32A
\\sim C33A \\sim C34A \\sim C35A \\sim O2 \\sim C36 \\sim C37 \\sim C38 \\sim
C39 \\sim C40 \\sim O2A \\sim C36A \\sim C37A \\sim C38A \\sim C39A \\sim C40A:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Li1C \\sim O1C \\sim C1C \\sim C4C \\sim C2C \\sim C5C \\sim C3C \\sim O3C
\\sim O4C \\sim C11C \\sim C14C \\sim C16C \\sim C19C \\sim C12C \\sim C13C
\\sim C15C \\sim C17C \\sim C20C \\sim C18C: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(C3C) = Uanis(C3D)
Uanis(C5D) = Uanis(C5C)
Uanis(C2D) = Uanis(C2C)
Uanis(O1C) = Uanis(O1D)
Uanis(C1C) = Uanis(C1D)
Uanis(O1) = Uanis(O1A)
Uanis(C35) = Uanis(C35A)
Uanis(C4C) = Uanis(C4D)
5. Rigid body (RIGU) restrains
 O1, C31, C32, C33, C34, O1A, C31A, C32A, C33A, C34A, C35A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O2, C36, C37, C38, C39, C40, O2A, C36A, C37A, C38A, C39A, C40A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Li1C, O1C, C1C, C4C, C2C, C5C, C3C, O3C, O4C, C11C, C14C, C16C, C19C, C12C,
 C13C, C15C, C17C, C20C, C18C
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
6. Same fragment restrains
{O2, C36, C37, C38, C39, C40} sigma for 1-2: 0.005, 1-3: 0.04
as
{O2A, C36A, C37A, C38A, C39A, C40A}
7. Others
 Sof(O1A)=Sof(C31A)=Sof(H31A)=Sof(C32A)=Sof(H32C)=Sof(H32D)=Sof(C33A)=
 Sof(H33C)=Sof(H33D)=Sof(C34A)=Sof(H34C)=Sof(H34D)=Sof(C35A)=Sof(H35D)=
 Sof(H35E)=Sof(H35F)=1-FVAR(1)
 Sof(O1)=Sof(C31)=Sof(H31)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(C33)=Sof(H33A)=
 Sof(H33B)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=
 FVAR(1)
 Sof(O2A)=Sof(C36A)=Sof(H36A)=Sof(C37A)=Sof(H37C)=Sof(H37D)=Sof(C38A)=
 Sof(H38C)=Sof(H38D)=Sof(C39A)=Sof(H39C)=Sof(H39D)=Sof(C40A)=Sof(H40D)=
 Sof(H40E)=Sof(H40F)=1-FVAR(2)
 Sof(O2)=Sof(C36)=Sof(H36)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C38)=Sof(H38A)=
 Sof(H38B)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=
 FVAR(2)
 Sof(O1D)=Sof(C1D)=Sof(H1D)=Sof(C2D)=Sof(H2DA)=Sof(H2DB)=Sof(C3D)=Sof(H3DA)=
 Sof(H3DB)=Sof(C4D)=Sof(H4DA)=Sof(H4DB)=Sof(C5D)=Sof(H5DA)=Sof(H5DB)=Sof(H5DC)=
 1-FVAR(3)
 Sof(O1C)=Sof(C1C)=Sof(H1C)=Sof(C2C)=Sof(H2CA)=Sof(H2CB)=Sof(C3C)=Sof(H3CA)=
 Sof(H3CB)=Sof(C4C)=Sof(H4CA)=Sof(H4CB)=Sof(C5C)=Sof(H5CA)=Sof(H5CB)=Sof(H5CC)=
 FVAR(3)
8.a Ternary CH refined with riding coordinates:
 C5(H5), C31(H31), C31A(H31A), C36(H36), C36A(H36A), C1C(H1C), C1D(H1D),
 C14C(H14C), C16C(H16C), C6C(H6C)
8.b Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C32A(H32C,H32D), C33A(H33C,
 H33D), C34A(H34C,H34D), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B),
 C37A(H37C,H37D), C38A(H38C,H38D), C39A(H39C,H39D), C2C(H2CA,H2CB), C3C(H3CA,
 H3CB), C4C(H4CA,H4CB), C2D(H2DA,H2DB), C3D(H3DA,H3DB), C4D(H4DA,H4DB),
 C11C(H11A,H11B), C12C(H12A,H12B), C13C(H13A,H13B), C17C(H17A,H17B), C18C(H18A,
 H18B), C19C(H19A,H19B), C7C(H7CA,H7CB), C8C(H8CA,H8CB), C9C(H9CA,H9CB)
8.c Me refined with riding coordinates:
 C35(H35A,H35B,H35C), C35A(H35D,H35E,H35F), C40(H40A,H40B,H40C), C40A(H40D,
 H40E,H40F), C5C(H5CA,H5CB,H5CC), C5D(H5DA,H5DB,H5DC), C15C(H15A,H15B,H15C),
 C20C(H20A,H20B,H20C)
8.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13),
 C14(H14), C15(H15), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23),
  C24(H24), C25(H25), C27(H27), C28(H28), C29(H29), C30(H30)
8.e Idealised Me refined as rotating group:
 C10C(H10A,H10B,H10C)
;
_shelx_res_checksum              63246
_olex2_submission_special_instructions 'No special instructions were received'