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_1557647
_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         'C38 H40 Fe3 Ho Li2 O2, C16 H32 Li O4'
_chemical_formula_sum            'C54 H72 Fe3 Ho Li3 O6'
_chemical_formula_weight         1170.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-02-22
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2020-02-26 deposited with the CCDC.	2020-03-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.383(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.3991(7)
_cell_length_b                   63.596(3)
_cell_length_c                   13.7285(8)
_cell_measurement_reflns_used    9680
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      24.072
_cell_measurement_theta_min      2.299
_cell_volume                     9943.7(10)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      110.0
_diffrn_measured_fraction_theta_full 0.900
_diffrn_measured_fraction_theta_max 0.900
_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  0.0638
_diffrn_reflns_av_unetI/netI     0.0679
_diffrn_reflns_Laue_measured_fraction_full 0.900
_diffrn_reflns_Laue_measured_fraction_max 0.900
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       68
_diffrn_reflns_limit_k_min       -68
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            50971
_diffrn_reflns_point_group_measured_fraction_full 0.900
_diffrn_reflns_point_group_measured_fraction_max 0.900
_diffrn_reflns_theta_full        22.500
_diffrn_reflns_theta_max         22.500
_diffrn_reflns_theta_min         2.184
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.481
_exptl_absorpt_correction_T_max  0.3299
_exptl_absorpt_correction_T_min  0.2395
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1232 before and 0.0752 after correction. The Ratio of minimum to maximum transmission is 0.7260. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_description       block
_exptl_crystal_F_000             4784
_exptl_crystal_size_max          0.184
_exptl_crystal_size_mid          0.176
_exptl_crystal_size_min          0.152
_refine_diff_density_max         1.194
_refine_diff_density_min         -1.027
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.224
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1143
_refine_ls_number_reflns         11711
_refine_ls_number_restraints     438
_refine_ls_restrained_S_all      1.201
_refine_ls_R_factor_all          0.1061
_refine_ls_R_factor_gt           0.0848
_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^)+217.6344P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1426
_refine_ls_wR_factor_ref         0.1511
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9407
_reflns_number_total             11711
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc01197e2.cif
_cod_data_source_block           mntpl045
_cod_depositor_comments
;Adding full bibliography for 1557647--1557656.cif.

 Adding full bibliography for 1557647--1557656.cif.
;
_cod_original_cell_volume        9943.8(10)
_cod_database_code               1557647
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.704
_shelx_estimated_absorpt_t_min   0.658
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 O4E-Li3D \\sim O4D-Li3D
 with sigma of 0.01
 O4E-C46E \\sim O4D-C46D \\sim O4E-C43E \\sim O4D-C43D
 with sigma of 0.01
 C44E-C43E \\sim C44D-C43D \\sim C46D-C45D \\sim C46E-C45E
 with sigma of 0.01
 C45E-C44E \\sim C45D-C44D
 with sigma of 0.01
 C46-C45 \\sim C46-C45A \\sim C44-C43
 with sigma of 0.01
 C45-C44 \\sim C45A-C44
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O4D \\sim C43D \\sim C44D \\sim C45D \\sim C46D \\sim O4E \\sim C43E \\sim C44E
\\sim C45E \\sim C46E: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
O5D \\sim C47D \\sim C48D \\sim C49D \\sim C50D: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
Uanis(C22) = Uanis(C21) = Uanis(C25)
Uanis(C27) = Uanis(C26) = Uanis(C30)
Uanis(C15) = Uanis(C11) = Uanis(C12)
Uanis(C5) = Uanis(C1) = Uanis(C2)
Uanis(C20) = Uanis(C16) = Uanis(C17)
Uanis(C17D) = Uanis(C16D) = Uanis(C20D)
Uanis(C10D) = Uanis(C6D) = Uanis(C7D)
Uanis(C3D) = Uanis(C2D) = Uanis(C1D)
Uanis(C29D) = Uanis(C28D) = Uanis(C27D)
Uanis(O2) = Uanis(Li2)
Uanis(C45) = Uanis(C45A)
4. Rigid body (RIGU) restrains
 O4D, C43D, C44D, C45D, C46D, O4E, C43E, C44E, C45E, C46E
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C47D, C48D, C49D, C50D, O5D
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C22, C21, C25, C24, C23
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C30, C26, C27, C28, C29
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C2, C1, C5, C4, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C6, C7, C10, C9, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C16, C17, C18, C19, C20
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Sof(O4E)=Sof(C43E)=Sof(H43E)=Sof(H43F)=Sof(C44E)=Sof(H44G)=Sof(H44H)=
 Sof(C45E)=Sof(H45G)=Sof(H45H)=Sof(C46E)=Sof(H46G)=Sof(H46H)=1-FVAR(1)
 Sof(O4D)=Sof(C43D)=Sof(H43A)=Sof(H43B)=Sof(C44D)=Sof(H44A)=Sof(H44B)=
 Sof(C45D)=Sof(H45A)=Sof(H45B)=Sof(C46D)=Sof(H46A)=Sof(H46B)=FVAR(1)
 Sof(H44C)=Sof(H44D)=Sof(H46C)=Sof(H46D)=Sof(C45A)=Sof(H45C)=Sof(H45D)=1-FVAR(2)
 Sof(H44E)=Sof(H44F)=Sof(C45)=Sof(H45E)=Sof(H45F)=Sof(H46E)=Sof(H46F)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,
 H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C31D(H31C,H31D),
 C32D(H32C,H32D), C33D(H33C,H33D), C34D(H34C,H34D), C35D(H35C,H35D), C36D(H36C,
 H36D), C37D(H37C,H37D), C38D(H38C,H38D), C39(H39A,H39B), C40(H40A,H40B),
 C41(H41A,H41B), C42(H42A,H42B), C43(H43C,H43D), C44(H44E,H44F), C44(H44C,H44D),
  C45(H45E,H45F), C46(H46E,H46F), C46(H46C,H46D), C47(H47A,H47B), C48(H48A,
 H48B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B),
 C53(H53A,H53B), C54(H54A,H54B), C39D(H39C,H39D), C40D(H40C,H40D), C41D(H41C,
 H41D), C42D(H42C,H42D), C43D(H43A,H43B), C44D(H44A,H44B), C45D(H45A,H45B),
 C46D(H46A,H46B), C43E(H43E,H43F), C44E(H44G,H44H), C45E(H45G,H45H), C46E(H46G,
 H46H), C47D(H47C,H47D), C48D(H48C,H48D), C49D(H49C,H49D), C50D(H50C,H50D),
 C51D(H51C,H51D), C52D(H52C,H52D), C53D(H53C,H53D), C54D(H54C,H54D), C45A(H45C,
 H45D)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), 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),
 C2D(H2D), C3D(H3D), C4D(H4D), C5D(H5D), C7D(H7D), C8D(H8D), C9D(H9D),
 C10D(H10D), C12D(H12D), C13D(H13D), C14D(H14D), C15D(H15D), C17D(H17D),
 C18D(H18D), C19D(H19D), C20D(H20D), C22D(H22D), C23D(H23D), C24D(H24D),
 C25D(H25D), C27D(H27D), C28D(H28D), C29D(H29D), C30D(H30D)
;
_shelx_res_checksum              84207
_olex2_submission_special_instructions 'No special instructions were received'