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_1557655
_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 Lu O2, C16 H32 Li O4, C4 H8 O'
_chemical_formula_sum            'C58 H80 Fe3 Li3 Lu O7'
_chemical_formula_weight         1252.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'I -2ya'
_space_group_name_H-M_alt        'I 1 a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-02-11
_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                 104.923(10)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   20.620(3)
_cell_length_b                   32.856(4)
_cell_length_c                   25.081(4)
_cell_measurement_reflns_used    9711
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      34.334
_cell_measurement_theta_min      2.479
_cell_volume                     16419(4)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_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  0.0802
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            330620
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.356
_diffrn_reflns_theta_min         2.041
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.618
_exptl_absorpt_correction_T_max  0.3414
_exptl_absorpt_correction_T_min  0.1287
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1166 before and 0.0721 after correction. The Ratio of minimum to maximum transmission is 0.3770. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_description       block
_exptl_crystal_F_000             7704
_exptl_crystal_size_max          0.464
_exptl_crystal_size_mid          0.386
_exptl_crystal_size_min          0.23
_refine_diff_density_max         5.611
_refine_diff_density_min         -7.484
_refine_diff_density_rms         0.341
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.045(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1945
_refine_ls_number_reflns         68250
_refine_ls_number_restraints     1196
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1014
_refine_ls_R_factor_gt           0.0876
_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^)+(0.1646P)^2^+123.1941P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2237
_refine_ls_wR_factor_ref         0.2475
_reflns_Friedel_coverage         0.987
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.984
_reflns_number_gt                57224
_reflns_number_total             68250
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc01197e2.cif
_cod_data_source_block           try
_cod_depositor_comments
;Adding full bibliography for 1557647--1557656.cif.

 Adding full bibliography for 1557647--1557656.cif.
;
_cod_database_code               1557655
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.584
_shelx_estimated_absorpt_t_min   0.376
_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
O1C \\sim O2C \\sim O3C \\sim O4C \\sim C1C \\sim C2C \\sim C2KA \\sim C3C
\\sim C4C \\sim C5C \\sim C6C \\sim C7C \\sim C8C \\sim C9C \\sim C10C \\sim
C11C \\sim C12C \\sim C13C \\sim C14C \\sim C15C \\sim Li1C \\sim O1S \\sim C2S
\\sim C3S \\sim C4S \\sim C5S \\sim O5C \\sim O6C \\sim O7C \\sim O8C \\sim
C16C \\sim C17C \\sim C18C \\sim C19C \\sim C20C \\sim C21C \\sim C22C \\sim
C23C \\sim C24C \\sim C25C \\sim C26C \\sim C27C \\sim C28C \\sim C29C \\sim
C30C \\sim C31C \\sim Li2C \\sim O6S \\sim C7S \\sim C8S \\sim C9S \\sim C10S
\\sim O9C \\sim O10C \\sim O11C \\sim O12C \\sim C32C \\sim C33C \\sim C34C
\\sim C35C \\sim C36C \\sim C37C \\sim C38C \\sim C39C \\sim C40C \\sim C41C
\\sim C42C \\sim C43C \\sim C44C \\sim C45C \\sim C46C \\sim C47C \\sim Li3C
\\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
O5 \\sim C107 \\sim C108 \\sim C109 \\sim C110: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 O1C, O2C, O3C, O4C, C1C, C2C, C2KA, C3C, C4C, C5C, C6C, C7C, C8C, C9C, C10C,
 C11C, C12C, C13C, C14C, C15C, Li1C, O1S, C2S, C3S, C4S, C5S, O5C, O6C, O7C,
 O8C, C16C, C17C, C18C, C19C, C20C, C21C, C22C, C23C, C24C, C25C, C26C, C27C,
 C28C, C29C, C30C, C31C, Li2C, O6S, C7S, C8S, C9S, C10S, O9C, O10C, O11C, O12C,
 C32C, C33C, C34C, C35C, C36C, C37C, C38C, C39C, C40C, C41C, C42C, C43C, C44C,
 C45C, C46C, C47C, Li3C, O11S, C12S, C13S, C14S, C15S
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C109, C108, C107, C110, O5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4.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), C107(H10A,H10B), C108(H10C,H10D), C109(H10E,
 H10F), C110(H11A,H11B), C111(H11C,H11D), C112(H11E,H11F), C113(H11G,H11H),
 C114(H11I,H11J), C1C(H1CA,H1CB), C2C(H2CA,H2CB), C2KA(H2KA,H2KB), C3C(H3CA,
 H3CB), C4C(H4CA,H4CB), C5C(H5CA,H5CB), C6C(H6CA,H6CB), C7C(H7CA,H7CB),
 C8C(H8CA,H8CB), C9C(H9CA,H9CB), C10C(H10G,H10H), C11C(H11K,H11L), C12C(H12A,
 H12B), C13C(H13A,H13B), C14C(H14A,H14B), C15C(H15A,H15B), C2S(H2SA,H2SB),
 C3S(H3SA,H3SB), C4S(H4SA,H4SB), C5S(H5SA,H5SB), C16C(H16A,H16B), 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), C7S(H7SA,H7SB), C8S(H8SA,H8SB), C9S(H9SA,H9SB), C10S(H10I,
 H10J), C32C(H32C,H32D), 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), C12S(H12C,H12D), C13S(H13C,
 H13D), C14S(H14C,H14D), C15S(H15C,H15D)
4.b Aromatic/amide H refined with riding coordinates:
 C0AA(H0AA), C2(H2), C3(H3), C4(H4), C4JA(H4JA), C7(H7), C8(H8), C9(H9),
 C10(H10), C12(H12), C13(H13), C14(H14), C15(H15), C17(H17), C18(H18), 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), 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),
 C103(H103), C104(H104), C105(H105), C106(H106)
;
_shelx_res_checksum              94112
_olex2_submission_special_instructions 'No special instructions were received'