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_1557654
_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 Er Fe3 Li2 O2, C16 H32 Li O4'
_chemical_formula_sum            'C54 H72 Er Fe3 Li3 O6'
_chemical_formula_weight         1172.74
_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             2018-01-17
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2020-02-27 deposited with the CCDC.	2020-03-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.262(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.4007(11)
_cell_length_b                   63.598(6)
_cell_length_c                   13.7293(14)
_cell_measurement_reflns_used    9382
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      24.713
_cell_measurement_theta_min      2.400
_cell_volume                     9946.8(17)
_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 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.0544
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       61
_diffrn_reflns_limit_k_min       -61
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            54860
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        19.999
_diffrn_reflns_theta_max         19.999
_diffrn_reflns_theta_min         2.183
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.577
_exptl_absorpt_correction_T_max  0.2582
_exptl_absorpt_correction_T_min  0.1697
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1390 before and 0.0768 after correction. The Ratio of minimum to maximum transmission is 0.6572. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_description       block
_exptl_crystal_F_000             4792
_exptl_crystal_size_max          0.298
_exptl_crystal_size_mid          0.231
_exptl_crystal_size_min          0.158
_refine_diff_density_max         0.680
_refine_diff_density_min         -0.819
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.265
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1203
_refine_ls_number_reflns         9065
_refine_ls_number_restraints     465
_refine_ls_restrained_S_all      1.235
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+95.9735P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0938
_refine_ls_wR_factor_ref         0.0967
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8060
_reflns_number_total             9065
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc01197e2.cif
_cod_data_source_block           mntpl041
_cod_depositor_comments
;Adding full bibliography for 1557647--1557656.cif.

 Adding full bibliography for 1557647--1557656.cif.
;
_cod_original_cell_volume        9946.9(17)
_cod_database_code               1557654
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.686
_shelx_estimated_absorpt_t_min   0.514
_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
 C42-C41A \\sim C42-C41 \\sim C41A-C40 \\sim C41-C40
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
O3D \\sim C39D \\sim C40D \\sim C41D \\sim C42D \\sim O3E \\sim C39E \\sim C40E
\\sim C41E \\sim C42E: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
C40 \\sim C41 \\sim C42 \\sim C41A: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01
C29 \\sim C30 \\sim C26 \\sim C27 \\sim C28: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01
C20 \\sim C19 \\sim C18 \\sim C17: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01
C11 \\sim C12 \\sim C13 \\sim C14: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01
C1 \\sim C2 \\sim C3 \\sim C4: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01
Er1D \\sim Li2D \\sim O2D: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(O3D) = Uanis(O3E)
Uanis(C41) = Uanis(C41A)
Uanis(C22D) = Uanis(C23D) = Uanis(C24D)
Uanis(C12D) = Uanis(C11D) = Uanis(C15D) = Uanis(C14D) = Uanis(C13D)
Uanis(C5D) = Uanis(C4D) = Uanis(C3D)
4. Rigid body (RIGU) restrains
 O3D, C39D, C40D, C41D, C42D, O3E, C39E, C40E, C41E, C42E
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C40, C41, C42, C41A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C26, C27, C28, C29, C30
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C20, C19, C18, C17
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C11, C12, C13, C14
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C1, C2, C3, C4
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 Er1D, Li2D, O2D
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
5. Same fragment restrains
{O4, C43, C44, C45, C46} sigma for 1-2: 0.005, 1-3: 0.04
as
{O3D, C39D, C40D, C41D, C42D}
{O4, C43, C44, C45, C46} sigma for 1-2: 0.005, 1-3: 0.04
as
{O3E, C39E, C40E, C41E, C42E}
6. Others
 Sof(O3E)=Sof(C39E)=Sof(H39C)=Sof(H39D)=Sof(C40E)=Sof(H40C)=Sof(H40D)=
 Sof(C41E)=Sof(H41C)=Sof(H41D)=Sof(C42E)=Sof(H42C)=Sof(H42D)=1-FVAR(1)
 Sof(O3D)=Sof(C39D)=Sof(H39A)=Sof(H39B)=Sof(C40D)=Sof(H40A)=Sof(H40B)=
 Sof(C41D)=Sof(H41A)=Sof(H41B)=Sof(C42D)=Sof(H42A)=Sof(H42B)=FVAR(1)
 Sof(H40G)=Sof(H40H)=Sof(H42G)=Sof(H42H)=Sof(C41A)=Sof(H41G)=Sof(H41H)=1-FVAR(2)
 Sof(H40E)=Sof(H40F)=Sof(C41)=Sof(H41E)=Sof(H41F)=Sof(H42E)=Sof(H42F)=FVAR(2)
7.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), C43(H43C,H43D), C44(H44C,H44D),
 C45(H45C,H45D), C46(H46C,H46D), C39(H39E,H39F), C40(H40E,H40F), C40(H40G,H40H),
  C41(H41E,H41F), C42(H42E,H42F), C42(H42G,H42H), C47(H47C,H47D), C48(H48C,
 H48D), C49(H49C,H49D), C50(H50C,H50D), C51(H51C,H51D), C52(H52C,H52D),
 C53(H53C,H53D), C54(H54C,H54D), C39D(H39A,H39B), C40D(H40A,H40B), C41D(H41A,
 H41B), C42D(H42A,H42B), C39E(H39C,H39D), C40E(H40C,H40D), C41E(H41C,H41D),
 C42E(H42C,H42D), C43D(H43A,H43B), C44D(H44A,H44B), C45D(H45A,H45B), C46D(H46A,
 H46B), C47D(H47A,H47B), C48D(H48A,H48B), C49D(H49A,H49B), C50D(H50A,H50B),
 C51D(H51A,H51B), C52D(H52A,H52B), C53D(H53A,H53B), C54D(H54A,H54B), C41A(H41G,
 H41H)
7.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              25732
_olex2_submission_special_instructions 'No special instructions were received'