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_1557648
_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 Gd Li2 O2, C16 H32 Li O4'
_chemical_formula_sum            'C54 H72 Fe3 Gd Li3 O6'
_chemical_formula_weight         1162.73
_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             2018-01-25
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2020-02-26 deposited with the CCDC.	2020-03-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.491(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.3774(12)
_cell_length_b                   63.872(7)
_cell_length_c                   13.7293(15)
_cell_measurement_reflns_used    9984
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      27.417
_cell_measurement_theta_min      2.562
_cell_volume                     9967.6(19)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_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 0.894
_diffrn_measured_fraction_theta_max 0.894
_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  0.0560
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_Laue_measured_fraction_full 0.894
_diffrn_reflns_Laue_measured_fraction_max 0.894
_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            80125
_diffrn_reflns_point_group_measured_fraction_full 0.894
_diffrn_reflns_point_group_measured_fraction_max 0.894
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.179
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.218
_exptl_absorpt_correction_T_max  0.3335
_exptl_absorpt_correction_T_min  0.2368
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1326 before and 0.0742 after correction. The Ratio of minimum to maximum transmission is 0.7100. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_description       block
_exptl_crystal_F_000             4760
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.125
_refine_diff_density_max         1.107
_refine_diff_density_min         -0.984
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.274
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1248
_refine_ls_number_reflns         15704
_refine_ls_number_restraints     490
_refine_ls_restrained_S_all      1.256
_refine_ls_R_factor_all          0.0802
_refine_ls_R_factor_gt           0.0685
_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^)+113.9354P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1267
_refine_ls_wR_factor_ref         0.1323
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13660
_reflns_number_total             15704
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc01197e2.cif
_cod_data_source_block           mntpl042
_cod_depositor_comments
;Adding full bibliography for 1557647--1557656.cif.

 Adding full bibliography for 1557647--1557656.cif.
;
_cod_original_cell_volume        9967.6(18)
_cod_database_code               1557648
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.769
_shelx_estimated_absorpt_t_min   0.604
_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
 C52E-C51D \\sim C52D-C51D \\sim C54D-C53D \\sim C54D-C53E
 with sigma of 0.005
 C53D-C52D \\sim C53E-C52E
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
O6 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim O6A \\sim C51A \\sim C52A
\\sim C53A \\sim C54A: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
O6D \\sim C51D \\sim C52D \\sim C53D \\sim C54D \\sim C53E \\sim C52E: within
2A with sigma of 0.005 and sigma for terminal atoms of 0.01
C21 \\sim C25 \\sim C24 \\sim C23 \\sim C22: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C22 \\sim C23 \\sim C24 \\sim C25 \\sim C21: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C1D \\sim C2D \\sim C3D \\sim C4D \\sim C5D: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C53D) = Uanis(C53E)
Uanis(C52D) = Uanis(C52E)
Uanis(C1) = Uanis(C5) = Uanis(C2)
4. Rigid body (RIGU) restrains
 O6, C51, C52, C53, C54, O6A, C51A, C52A, C53A, C54A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 O6D, C51D, C52D, C53D, C54D, C53E, C52E
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C21, C25, C24, C23, C22
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C21, C22, C23, C24, C25
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1D, C2D, C3D, C4D, C5D
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Same fragment restrains
{O1, C31, C32, C33, C34} sigma for 1-2: 0.005, 1-3: 0.04
as
{O6, C51, C52, C53, C54}
{O1, C31, C32, C33, C34} sigma for 1-2: 0.005, 1-3: 0.04
as
{O6A, C51A, C52A, C53A, C54A}
6. Others
 Sof(O6A)=Sof(C51A)=Sof(H51C)=Sof(H51D)=Sof(C52A)=Sof(H52C)=Sof(H52D)=
 Sof(C53A)=Sof(H53C)=Sof(H53D)=Sof(C54A)=Sof(H54C)=Sof(H54D)=1-FVAR(1)
 Sof(O6)=Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(C53)=
 Sof(H53A)=Sof(H53B)=Sof(C54)=Sof(H54A)=Sof(H54B)=FVAR(1)
 Sof(H51G)=Sof(H51H)=Sof(H54G)=Sof(H54H)=Sof(C53E)=Sof(H53G)=Sof(H53H)=
 Sof(C52E)=Sof(H52G)=Sof(H52H)=1-FVAR(2)
 Sof(H51E)=Sof(H51F)=Sof(C52D)=Sof(H52E)=Sof(H52F)=Sof(C53D)=Sof(H53E)=
 Sof(H53F)=Sof(H54E)=Sof(H54F)=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), 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),
 C51A(H51C,H51D), C52A(H52C,H52D), C53A(H53C,H53D), C54A(H54C,H54D), C39D(H39C,
 H39D), C40D(H40C,H40D), C41D(H41C,H41D), C42D(H42C,H42D), C43D(H43C,H43D),
 C44D(H44C,H44D), C45D(H45C,H45D), C46D(H46C,H46D), C47D(H47C,H47D), C48D(H48C,
 H48D), C49D(H49C,H49D), C50D(H50C,H50D), C51D(H51E,H51F), C51D(H51G,H51H),
 C52D(H52E,H52F), C53D(H53E,H53F), C54D(H54E,H54F), C54D(H54G,H54H), C53E(H53G,
 H53H), C52E(H52G,H52H)
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              4142
_olex2_submission_special_instructions 'No special instructions were received'