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_1557656
_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_absolute_configuration ad
_chemical_formula_moiety
'C38 H40 Fe3 Li2 O2 Yb, C16 H32 Li O4, C4 H8 O'
_chemical_formula_sum            'C58 H80 Fe3 Li3 O7 Yb'
_chemical_formula_weight         1250.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-12
_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                 120.475(2)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   28.077(3)
_cell_length_b                   32.756(4)
_cell_length_c                   20.619(2)
_cell_measurement_reflns_used    9857
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      33.128
_cell_measurement_theta_min      3.220
_cell_volume                     16343(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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      110.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_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  0.0699
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            397333
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.093
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.535
_exptl_absorpt_correction_T_max  0.2851
_exptl_absorpt_correction_T_min  0.1042
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1624 before and 0.1066 after correction. The Ratio of minimum to maximum transmission is 0.3655. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_description       block
_exptl_crystal_F_000             7692
_exptl_crystal_size_max          0.416
_exptl_crystal_size_mid          0.342
_exptl_crystal_size_min          0.258
_refine_diff_density_max         1.659
_refine_diff_density_min         -1.819
_refine_diff_density_rms         0.123
_refine_ls_abs_structure_details
;
 Flack x determined using 15532 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.064(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1945
_refine_ls_number_reflns         37402
_refine_ls_number_restraints     662
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0414
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0334P)^2^+131.7620P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0963
_refine_ls_wR_factor_ref         0.1054
_reflns_Friedel_coverage         0.994
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                34214
_reflns_number_total             37402
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc01197e2.cif
_cod_data_source_block           tl078
_cod_depositor_comments
;Adding full bibliography for 1557647--1557656.cif.

 Adding full bibliography for 1557647--1557656.cif.
;
_cod_original_cell_volume        16344(3)
_cod_database_code               1557656
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.561
_shelx_estimated_absorpt_t_min   0.419
_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
O1 \\sim O2 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim
C37 \\sim C38 \\sim O5 \\sim O6 \\sim C107 \\sim C108 \\sim C109 \\sim C110
\\sim C111 \\sim C112 \\sim C113 \\sim C114 \\sim O2C \\sim O4C \\sim C5C \\sim
C6C \\sim C7C \\sim C8C \\sim C13C \\sim C14C \\sim C15C \\sim C16C \\sim O8C
\\sim C29C \\sim C30C \\sim C31C \\sim C32C \\sim O6S \\sim C7S \\sim C8S \\sim
C9S \\sim C10S \\sim O10C \\sim O11C \\sim C37C \\sim C38C \\sim C39C \\sim
C40C \\sim C41C \\sim C42C \\sim C43C \\sim C44C \\sim O11S \\sim C12S \\sim
C13S \\sim C14S \\sim C15S: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
3. Rigid body (RIGU) restrains
 O1, O2, C31, C32, C33, C34, C35, C36, C37, C38, O5, O6, C107, C108, C109,
 C110, C111, C112, C113, C114, O2C, O4C, C5C, C6C, C7C, C8C, C13C, C14C, C15C,
 C16C, O8C, C29C, C30C, C31C, C32C, O6S, C7S, C8S, C9S, C10S, O10C, O11C, C37C,
 C38C, C39C, C40C, C41C, C42C, C43C, C44C, O11S, C12S, C13S, C14S, C15S
 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:
 C7(H7), C68(H68), C103(H103), C104(H104)
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), C69(H69A,H69B),
 C70(H70A,H70B), C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B), C74(H74A,H74B),
  C75(H75A,H75B), C76(H76A,H76B), C105(H10A,H10B), C107(H10C,H10D), C108(H10E,
 H10F), C109(H10G,H10H), C110(H11A,H11B), C111(H11C,H11D), C112(H11E,H11F),
 C113(H11G,H11H), C114(H11I,H11J), C1C(H1CA,H1CB), C2C(H2CA,H2CB), C3C(H3CA,
 H3CB), C4C(H4CA,H4CB), C5C(H5CA,H5CB), C6C(H6CA,H6CB), C7C(H7CA,H7CB),
 C8C(H8CA,H8CB), C9C(H9CA,H9CB), C10C(H10I,H10J), C11C(H11K,H11L), C12C(H12A,
 H12B), C13C(H13A,H13B), C14C(H14A,H14B), C15C(H15A,H15B), C16C(H16A,H16B),
 C2S(H2SA,H2SB), C3S(H3SA,H3SB), C4S(H4SA,H4SB), C5S(H5SA,H5SB), C17C(H17A,
 H17B), C18C(H18A,H18B), C19C(H19A,H19B), C20C(H20A,H20B), C21C(H21A,H21B),
 C22C(H22A,H22B), C23C(H23A,H23B), C24C(H24A,H24B), C25C(H25A,H25B), C26C(H26A,
 H26B), C27C(H27A,H27B), C28C(H28A,H28B), C29C(H29A,H29B), C30C(H30A,H30B),
 C31C(H31C,H31D), C32C(H32C,H32D), C7S(H7SA,H7SB), C8S(H8SA,H8SB), C9S(H9SA,
 H9SB), C10S(H10K,H10L), C33C(H33C,H33D), C34C(H34C,H34D), C35C(H35C,H35D),
 C36C(H36C,H36D), C37C(H37C,H37D), C38C(H38C,H38D), C39C(H39A,H39B), C40C(H40A,
 H40B), C41C(H41A,H41B), C42C(H42A,H42B), C43C(H43A,H43B), C44C(H44A,H44B),
 C45C(H45A,H45B), C46C(H46A,H46B), C47C(H47A,H47B), C48C(H48A,H48B), C12S(H12C,
 H12D), C13S(H13C,H13D), C14S(H14C,H14D), C15S(H15C,H15D)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), 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), C78(H78),
  C79(H79), C80(H80), C81(H81), C83(H83), C84(H84), C85(H85), C86(H86),
 C88(H88), C89(H89), C90(H90), C91(H91), C93(H93), C94(H94), C95(H95), C96(H96),
  C98(H98), C99(H99), C100(H100), C101(H101)
;
_shelx_res_checksum              40252
_olex2_submission_special_instructions 'No special instructions were received'