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_1557651
_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
'1(C40 H34 Fe3 Ho Li2 N2), C20 H20 Li N4, 0.88(C5 H5 N)'
_chemical_formula_sum            'C64.38 H58.38 Fe3 Ho Li3 N6.88'
_chemical_formula_weight         1281.60
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-26 deposited with the CCDC.	2020-03-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.2060(9)
_cell_length_b                   22.6446(10)
_cell_length_c                   23.1321(11)
_cell_measurement_reflns_used    9899
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      24.758
_cell_measurement_theta_min      2.197
_cell_volume                     11108.1(9)
_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 0.999
_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  0.0837
_diffrn_reflns_av_unetI/netI     0.0930
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            67434
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.303
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.225
_exptl_absorpt_correction_T_max  0.3334
_exptl_absorpt_correction_T_min  0.2269
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0908 before and 0.0601 after correction. The Ratio of minimum to maximum transmission is 0.6806. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_description       plate
_exptl_crystal_F_000             5174
_exptl_crystal_size_max          0.082
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.021
_refine_diff_density_max         0.922
_refine_diff_density_min         -1.197
_refine_diff_density_rms         0.136
_refine_ls_abs_structure_details
;
 Flack x determined using 4904 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.019(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1371
_refine_ls_number_reflns         19541
_refine_ls_number_restraints     876
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0246P)^2^+38.0492P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0932
_refine_ls_wR_factor_ref         0.1135
_reflns_Friedel_coverage         0.846
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                13766
_reflns_number_total             19541
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc01197e2.cif
_cod_data_source_block           mntpl058
_cod_depositor_comments
;Adding full bibliography for 1557647--1557656.cif.

 Adding full bibliography for 1557647--1557656.cif.
;
_cod_database_code               1557651
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.955
_shelx_estimated_absorpt_t_min   0.839
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{N3, N3A}
{C73, C73A}
3. Uiso/Uaniso restraints and constraints
N5 \\sim N6 \\sim N7 \\sim N8 \\sim C81 \\sim C82 \\sim C83 \\sim C84 \\sim C85
\\sim C86 \\sim C87 \\sim C88 \\sim C89 \\sim C90 \\sim C91 \\sim C92 \\sim C93
\\sim C94 \\sim C95 \\sim C96 \\sim C97 \\sim C98 \\sim C99 \\sim C100 \\sim
Li5: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
N3 \\sim C71 \\sim C72 \\sim C73 \\sim C74 \\sim C75 \\sim N3A \\sim C71A \\sim
C72A \\sim C73A \\sim C74A \\sim C75A: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C122 \\sim C121 \\sim N13 \\sim C123 \\sim C125 \\sim C124 \\sim N12 \\sim C120
\\sim C119 \\sim C118 \\sim C117 \\sim C116 \\sim Li6: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
C127 \\sim C126 \\sim N14 \\sim C128 \\sim C129 \\sim C130: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01
C22 \\sim C21 \\sim C25 \\sim Li1: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(N3) = Uanis(N3A)
Uanis(C73) = Uanis(C73A)
Uanis(Li3) = Uanis(Ho2)
Uanis(Ho1) = Uanis(Li1)
4. Rigid body (RIGU) restrains
 N5, N6, N7, N8, C81, C82, C83, C84, C85, C86, C87, C88, C89, C90, C91, C92,
 C93, C94, C95, C96, C97, C98, C99, C100, Li5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N3, C71, C72, C73, C74, C75, N3A, C71A, C72A, C73A, C74A, C75A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C122, C121, N13, C123, C125, C124, N12, C120, C119, C118, C117, C116, Li6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C127, C126, N14, C128, C129, C130
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C21, Li1, C22, C25
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
5. Same fragment restrains
{N3, C71, C72, C73, C74, C75, N3A, C71A, C72A, C73A, C74A, C75A} sigma for 1-2:
0.005, 1-3: 0.04
as
{N3A, C71A, C72A, C73A, C74A, C75A, N4, C80, C79, C78, C77, C76}
6. Others
 Sof(N3A)=Sof(C71A)=Sof(H71A)=Sof(C72A)=Sof(H72A)=Sof(C73A)=Sof(H73A)=
 Sof(C74A)=Sof(H74A)=Sof(C75A)=Sof(H75A)=1-FVAR(1)
 Sof(N3)=Sof(C71)=Sof(H71)=Sof(C72)=Sof(H72)=Sof(C73)=Sof(H73)=Sof(C74)=
 Sof(H74)=Sof(C75)=Sof(H75)=FVAR(1)
 Fixed Sof: C121(0.75) H121(0.75) C122(0.75) H122(0.75) C123(0.75) H123(0.75)
 C124(0.75) H124(0.75) C125(0.75) H125(0.75) N13(0.75)
7.a Aromatic/amide H refined with riding coordinates:
 C35(H35), C34(H34), C33(H33), C32(H32), C31(H31), C1(H1), 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), C36(H36), C37(H37),
 C38(H38), C39(H39), C40(H40), C42(H42), C43(H43), C44(H44), C45(H45), C47(H47),
  C48(H48), C49(H49), C50(H50), C52(H52), C53(H53), C54(H54), C55(H55),
 C57(H57), C58(H58), C59(H59), C60(H60), C62(H62), C63(H63), C64(H64), C65(H65),
  C67(H67), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72), C73(H73),
 C74(H74), C75(H75), C71A(H71A), C72A(H72A), C73A(H73A), C74A(H74A), C75A(H75A),
  C80(H80), C79(H79), C78(H78), C77(H77), C76(H76), C81(H81), C82(H82),
 C83(H83), C84(H84), C85(H85), C86(H86), C87(H87), C88(H88), C89(H89), C90(H90),
  C91(H91), C92(H92), C93(H93), C94(H94), C95(H95), C96(H96), C97(H97),
 C98(H98), C99(H99), C100(H100), C120(H120), C119(H119), C118(H118), C117(H117),
  C116(H116), C101(H101), C102(H102), C103(H103), C104(H104), C105(H105),
 C106(H106), C107(H107), C108(H108), C109(H109), C110(H110), C111(H111),
 C112(H112), C113(H113), C114(H114), C115(H115), C121(H121), C122(H122),
 C123(H123), C124(H124), C125(H125), C127(H127), C126(H126), C128(H128),
 C129(H129), C130(H130)
7.b Fitted hexagon refined as free rotating group:
 N1(C35,C34,C33,C32,C31), N3(C71,C72,C73,C74,C75), N4(C80,C79,C78,C77,C76),
 N12(C120,C119,C118,C117,C116), C121(C122,C123,C124,C125,N13), C127(C126,N14,
 C128,C129,C130)
;
_shelx_res_checksum              8275
_olex2_submission_special_instructions 'No special instructions were received'