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_1557652
_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 Li2 Lu O2, C16 H32 Li O4'
_chemical_formula_sum            'C54 H72 Fe3 Li3 Lu O6'
_chemical_formula_weight         1180.45
_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     direct
_audit_creation_date             2018-10-24
_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                 92.282(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.4149(16)
_cell_length_b                   63.246(9)
_cell_length_c                   13.7430(19)
_cell_measurement_reflns_used    9833
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      30.276
_cell_measurement_theta_min      2.405
_cell_volume                     9914(2)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      110.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.906
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0624
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_Laue_measured_fraction_full 0.906
_diffrn_reflns_Laue_measured_fraction_max 0.906
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       75
_diffrn_reflns_limit_k_min       -75
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            99358
_diffrn_reflns_point_group_measured_fraction_full 0.906
_diffrn_reflns_point_group_measured_fraction_max 0.906
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.189
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.884
_exptl_absorpt_correction_T_max  0.2986
_exptl_absorpt_correction_T_min  0.1648
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1336 before and 0.0891 after correction. The Ratio of minimum to maximum transmission is 0.5519. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_description       block
_exptl_crystal_F_000             4816
_exptl_crystal_size_max          0.341
_exptl_crystal_size_mid          0.267
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.330
_refine_diff_density_min         -1.671
_refine_diff_density_rms         0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1221
_refine_ls_number_reflns         15843
_refine_ls_number_restraints     661
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0666
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+306.4883P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1537
_refine_ls_wR_factor_ref         0.1603
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14209
_reflns_number_total             15843
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc01197e2.cif
_cod_data_source_block           tl061
_cod_depositor_comments
;Adding full bibliography for 1557647--1557656.cif.

 Adding full bibliography for 1557647--1557656.cif.
;
_cod_database_code               1557652
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.723
_shelx_estimated_absorpt_t_min   0.440
_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
 O8-C92 \\sim O8-C92A \\sim O8-C89A \\sim O8-C89
 with sigma of 0.01
 C92A-C91 \\sim C92-C91 \\sim C90-C89A \\sim C90-C89
 with sigma of 0.01
 C108-C107 \\sim C108-C1A \\sim C106-C105 \\sim C105-C1B
 with sigma of 0.01
 C107-C106 \\sim C1B-C1A
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
O1 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8
\\sim C9 \\sim C10 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim Li1
\\sim O3 \\sim O4 \\sim Li3 \\sim Li4 \\sim O8 \\sim Li5: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
C54 \\sim C55 \\sim C56 \\sim C57 \\sim C58 \\sim C64 \\sim C65 \\sim C66 \\sim
C67 \\sim C68: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.02
C54 \\sim C55 \\sim C56 \\sim C57 \\sim C58: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01
O8 \\sim C89 \\sim C90 \\sim C91 \\sim C92 \\sim C92A \\sim C89A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02
O12 \\sim C105 \\sim C106 \\sim C107 \\sim C108 \\sim C1A \\sim C1B: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02
C88 \\sim C87 \\sim C86: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C81 \\sim C82 \\sim C83 \\sim C84: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C15) = Uanis(C14)
Uanis(C20) = Uanis(C16)
Uanis(C55) = Uanis(C54)
Uanis(C7) = Uanis(C6)
4. Rigid body (RIGU) restrains
 C54, C55, C56, C57, C58
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 O1, C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C21, C22, C23, C24, C25, Li1, O3,
  O4, Li3, Li4, O8, Li5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C54, C55, C56, C57, C58, C64, C65, C66, C67, C68
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O8, C89, C90, C91, C92, C92A, C89A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C105, C106, C107, C108, C1A, C1B, O12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C88, C87, C86
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C83, C82, C84, C81
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Sof(H90C)=Sof(H90D)=Sof(H91C)=Sof(H91D)=Sof(C92A)=Sof(H92C)=Sof(H92D)=
 Sof(C89A)=Sof(H89C)=Sof(H89D)=1-FVAR(1)
 Sof(C89)=Sof(H89A)=Sof(H89B)=Sof(H90A)=Sof(H90B)=Sof(H91A)=Sof(H91B)=Sof(C92)=
 Sof(H92A)=Sof(H92B)=FVAR(1)
 Sof(H10M)=Sof(H10N)=Sof(H10U)=Sof(H10V)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(C1B)=
 Sof(H1BA)=Sof(H1BB)=1-FVAR(2)
 Sof(H10K)=Sof(H10L)=Sof(C106)=Sof(H10O)=Sof(H10P)=Sof(C107)=Sof(H10Q)=
 Sof(H10R)=Sof(H10S)=Sof(H10T)=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), C69(H69A,H69B),
 C70(H70A,H70B), C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B), C74(H74A,H74B),
  C75(H75A,H75B), C76(H76A,H76B), C77(H77A,H77B), C78(H78A,H78B), C79(H79A,
 H79B), C80(H80A,H80B), C81(H81A,H81B), C82(H82A,H82B), C83(H83A,H83B),
 C84(H84A,H84B), C85(H85A,H85B), C86(H86A,H86B), C87(H87A,H87B), C88(H88A,H88B),
  C89(H89A,H89B), C90(H90A,H90B), C90(H90C,H90D), C91(H91A,H91B), C91(H91C,
 H91D), C92(H92A,H92B), C93(H93A,H93B), C94(H94A,H94B), C95(H95A,H95B),
 C96(H96A,H96B), C97(H97A,H97B), C98(H98A,H98B), C99(H99A,H99B), C100(H10A,
 H10B), C101(H10C,H10D), C102(H10E,H10F), C103(H10G,H10H), C104(H10I,H10J),
 C105(H10K,H10L), C105(H10M,H10N), C106(H10O,H10P), C107(H10Q,H10R), C108(H10S,
 H10T), C108(H10U,H10V), C92A(H92C,H92D), C89A(H89C,H89D), C1A(H1AA,H1AB),
 C1B(H1BA,H1BB)
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),
 C40(H40), C41(H41), C42(H42), C43(H43), C45(H45), C46(H46), C47(H47), C48(H48),
  C50(H50), C51(H51), C52(H52), C53(H53), C55(H55), C56(H56), C57(H57),
 C58(H58), C60(H60), C61(H61), C62(H62), C63(H63), C65(H65), C66(H66), C67(H67),
  C68(H68)
;
_shelx_res_checksum              27155
_olex2_submission_special_instructions 'No special instructions were received'