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_1557653
_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 Tm, C16 H32 Li O4'
_chemical_formula_sum            'C54 H72 Fe3 Li3 O6 Tm'
_chemical_formula_weight         1174.41
_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             2018-12-19
_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                 92.280(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.4199(15)
_cell_length_b                   63.606(8)
_cell_length_c                   13.7467(19)
_cell_measurement_reflns_used    9944
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      27.555
_cell_measurement_theta_min      3.194
_cell_volume                     9977(2)
_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      120.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker PHOTON2'
_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  0.0336
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_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            103328
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.182
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.665
_exptl_absorpt_correction_T_max  0.2949
_exptl_absorpt_correction_T_min  0.1998
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1080 before and 0.0536 after correction. The Ratio of minimum to maximum transmission is 0.6775. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_description       block
_exptl_crystal_F_000             4800
_exptl_crystal_size_max          0.451
_exptl_crystal_size_mid          0.283
_exptl_crystal_size_min          0.106
_refine_diff_density_max         1.231
_refine_diff_density_min         -1.186
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.409
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1245
_refine_ls_number_reflns         17342
_refine_ls_number_restraints     247
_refine_ls_restrained_S_all      1.402
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+49.0562P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0919
_refine_ls_wR_factor_ref         0.0920
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17226
_reflns_number_total             17342
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc01197e2.cif
_cod_data_source_block           mntl072
_cod_depositor_comments
;Adding full bibliography for 1557647--1557656.cif.

 Adding full bibliography for 1557647--1557656.cif.
;
_cod_database_code               1557653
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.765
_shelx_estimated_absorpt_t_min   0.379
_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
 C52A-C51 \\sim C52-C51 \\sim C53A-C52A \\sim C53-C52 \\sim C54-C53 \\sim
C54-C53A
 with sigma of 0.01
 O6B-C54B \\sim O6B-C54C \\sim O6B-C51C \\sim O6B-C51B
 with sigma of 0.01
 C54B-C53B \\sim C54C-C53B \\sim C52B-C51C \\sim C52B-C51B
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Tm1B \\sim O1B \\sim Li1B: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.04
C51 \\sim C52 \\sim C53 \\sim C54 \\sim C52A \\sim C53A: within 2A with sigma
of 0.02 and sigma for terminal atoms of 0.04
O6B \\sim C51B \\sim C52B \\sim C53B \\sim C54B \\sim C51C \\sim C54C: within
2A with sigma of 0.02 and sigma for terminal atoms of 0.04
4. Rigid body (RIGU) restrains
 Tm1B, O1B, Li1B
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C51, C52, C53, C54, C52A, C53A
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 O6B, C51B, C52B, C53B, C54B, C51C, C54C
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
5. Others
 Sof(H51C)=Sof(H51D)=Sof(H54C)=Sof(H54D)=Sof(C52A)=Sof(H52C)=Sof(H52D)=
 Sof(C53A)=Sof(H53C)=Sof(H53D)=1-FVAR(1)
 Sof(H51A)=Sof(H51B)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(C53)=Sof(H53A)=Sof(H53B)=
 Sof(H54A)=Sof(H54B)=FVAR(1)
 Sof(H52G)=Sof(H52H)=Sof(H53G)=Sof(H53H)=Sof(C51C)=Sof(H51G)=Sof(H51H)=
 Sof(C54C)=Sof(H54G)=Sof(H54H)=1-FVAR(2)
 Sof(C51B)=Sof(H51E)=Sof(H51F)=Sof(H52E)=Sof(H52F)=Sof(H53E)=Sof(H53F)=
 Sof(C54B)=Sof(H54E)=Sof(H54F)=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), 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), C51(H51C,H51D), C52(H52A,H52B), C53(H53A,H53B),
 C54(H54A,H54B), C54(H54C,H54D), 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(H51E,H51F), C52B(H52E,H52F), C52B(H52G,H52H), C53B(H53E,H53F),
 C53B(H53G,H53H), C54B(H54E,H54F), C52A(H52C,H52D), C53A(H53C,H53D), C51C(H51G,
 H51H), C54C(H54G,H54H)
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),
 C2B(H2B), 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              94704
_olex2_submission_special_instructions 'No special instructions were received'