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_1557649
_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 O2 Yb, C16 H32 Li O4'
_chemical_formula_sum            'C54 H72 Fe3 Li3 O6 Yb'
_chemical_formula_weight         1178.52
_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
_audit_creation_date             2018-10-05
_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                 92.170(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.4155(6)
_cell_length_b                   63.489(3)
_cell_length_c                   13.7300(7)
_cell_measurement_reflns_used    9211
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      27.466
_cell_measurement_theta_min      2.400
_cell_volume                     9943.8(9)
_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)'
_diffrn_ambient_temperature      110.0
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_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  0.0526
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       61
_diffrn_reflns_limit_k_min       -60
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            60904
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        20.000
_diffrn_reflns_theta_max         20.000
_diffrn_reflns_theta_min         2.199
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.771
_exptl_absorpt_correction_T_max  0.2617
_exptl_absorpt_correction_T_min  0.1609
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1421 before and 0.0789 after correction. The Ratio of minimum to maximum transmission is 0.6148. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_description       plate
_exptl_crystal_F_000             4808
_exptl_crystal_size_max          0.396
_exptl_crystal_size_mid          0.363
_exptl_crystal_size_min          0.045
_refine_diff_density_max         0.891
_refine_diff_density_min         -1.125
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.294
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1165
_refine_ls_number_reflns         8938
_refine_ls_number_restraints     2722
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0774
_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^)+(0.0001P)^2^+342.0445P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1571
_refine_ls_wR_factor_ref         0.1617
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8128
_reflns_number_total             8938
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc01197e2.cif
_cod_data_source_block           tl059
_cod_depositor_comments
;Adding full bibliography for 1557647--1557656.cif.

 Adding full bibliography for 1557647--1557656.cif.
;
_cod_original_cell_volume        9943.9(9)
_cod_database_code               1557649
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.885
_shelx_estimated_absorpt_t_min   0.407
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C15) = Uanis(C14) = Uanis(C11)
Uanis(C5B) = Uanis(C1B) = Uanis(C2B)
Uanis(C5) = Uanis(C1) = Uanis(C2)
Uanis(O1) = Uanis(Li1)
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4.a Ternary CH refined with riding coordinates:
 C10(H10), C2B(H2B)
4.b 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), C31B(H31C,H31D),
 C32B(H32C,H32D), C33B(H33C,H33D), C34B(H34C,H34D), C35B(H35C,H35D), C36B(H36C,
 H36D), C37B(H37C,H37D), C38B(H38C,H38D), 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),
 C39B(H39C,H39D), C40B(H40C,H40D), C41B(H41C,H41D), C42B(H42C,H42D), C43B(H43C,
 H43D), C44B(H44C,H44D), C45B(H45C,H45D), C46B(H46C,H46D), C47B(H47C,H47D),
 C48B(H48C,H48D), C49B(H49C,H49D), C50B(H50C,H50D), C51B(H51C,H51D), C52B(H52C,
 H52D), C53B(H53C,H53D), C54B(H54C,H54D)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), 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), C3B(H3B),
 C4B(H4B), C5B(H5B), C7B(H7B), C8B(H8B), C9B(H9B), C10B(H10B), C12B(H12B),
 C13B(H13B), C14B(H14B), C15B(H15B), C17B(H17B), C18B(H18B), C19B(H19B),
 C20B(H20B), C22B(H22B), C23B(H23B), C24B(H24B), C25B(H25B), C27B(H27B),
 C28B(H28B), C29B(H29B), C30B(H30B)
;
_shelx_res_checksum              13895
_olex2_submission_special_instructions 'No special instructions were received'