Slow Magnetic Relaxation in a Lanthanide-[1]Metallocenophane Complex.
Latendresse, Trevor Philip; Bhuvanesh, Nattamai S.; Nippe, Michael; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b01499

data_4126210
_publ_section_title
;
 Slow Magnetic Relaxation in a Lanthanide-[1]Metallocenophane Complex.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b01499
_journal_year                    2017
_chemical_formula_moiety         'C38 H40 Dy Fe3 Li2 O2, C16 H32 Li O4'
_chemical_formula_sum            'C54 H72 Dy Fe3 Li3 O6'
_chemical_formula_weight         1167.98
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-12-02
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.567(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.3810(9)
_cell_length_b                   63.671(5)
_cell_length_c                   13.7280(11)
_cell_measurement_reflns_used    9064
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.423
_cell_measurement_theta_min      2.297
_cell_volume                     9937.9(14)
_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      100.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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  0.0641
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       82
_diffrn_reflns_limit_k_min       -82
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            247289
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.471
_diffrn_reflns_theta_min         2.427
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.394
_exptl_absorpt_correction_T_max  0.9811
_exptl_absorpt_correction_T_min  0.5220
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1281 before and 0.0579 after correction.
The Ratio of minimum to maximum transmission is 0.5321.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_description       plate
_exptl_crystal_F_000             4776
_exptl_crystal_size_max          0.539
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.036
_refine_diff_density_max         1.040
_refine_diff_density_min         -2.475
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.334
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1223
_refine_ls_number_reflns         22555
_refine_ls_number_restraints     231
_refine_ls_restrained_S_all      1.331
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0589
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+57.2062P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.0979
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19808
_reflns_number_total             22555
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b01499_si_002.cif
_cod_data_source_block           Compound1
_cod_database_code               4126210
_shelx_estimated_absorpt_t_max   0.919
_shelx_estimated_absorpt_t_min   0.359
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C1C-C1B = C107-C106
 1.51 with sigma of 0.02
 O12A-Li6 \\sim O12-Li6
 with sigma of 0.02
 O12A-C1D \\sim O12-C105 \\sim O12A-C1A \\sim O12-C108
 with sigma of 0.02
 C1A-C1B \\sim C108-C107 \\sim C1D-C1C \\sim C106-C105
 with sigma of 0.02
 C1B-C1C \\sim C107-C106
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O12 \\sim C105 \\sim C106 \\sim C107 \\sim C108 \\sim O12A \\sim C1A \\sim C1B
\\sim C1C \\sim C1D \\sim C105 \\sim C106 \\sim C107 \\sim C108: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C60) = Uanis(C59) = Uanis(C63)
Uanis(O12) = Uanis(O12A)
Uanis(C68) = Uanis(C64) = Uanis(C65)
4. Rigid body (RIGU) restrains
 O12, O12A, C1A, C1B, C1C, C1D, C105, C106, C107, C108
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{O12, C105, C106, C107, C108} sigma for 1-2: 0.02, 1-3: 0.04
as
{O12A, C1A, C1B, C1C, C1D}
6. Others
 Sof(O12A)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(C1C)=
 Sof(H1CA)=Sof(H1CB)=Sof(C1D)=Sof(H1DA)=Sof(H1DB)=1-FVAR(1)
 Sof(O12)=Sof(C105)=Sof(H10K)=Sof(H10L)=Sof(C106)=Sof(H10M)=Sof(H10N)=
 Sof(C107)=Sof(H10O)=Sof(H10P)=Sof(C108)=Sof(H10Q)=Sof(H10R)=FVAR(1)
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), C69(H69A,H69B),
 C70(H70A,H70B), C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B), C74(H74A,H74B),
  C75(H75A,H75B), C76(H76A,H76B), C77(H77A,H77B), C78(H78A,H78B), C79(H79A,
 H79B), C80(H80A,H80B), C81(H81A,H81B), C82(H82A,H82B), C83(H83A,H83B),
 C84(H84A,H84B), C85(H85A,H85B), C86(H86A,H86B), C87(H87A,H87B), C88(H88A,H88B),
  C89(H89A,H89B), C90(H90A,H90B), C91(H91A,H91B), C92(H92A,H92B), C93(H93A,
 H93B), C94(H94A,H94B), C95(H95A,H95B), C96(H96A,H96B), C97(H97A,H97B),
 C98(H98A,H98B), C99(H99A,H99B), C100(H10A,H10B), C101(H10C,H10D), C102(H10E,
 H10F), C103(H10G,H10H), C104(H10I,H10J), C105(H10K,H10L), C106(H10M,H10N),
 C107(H10O,H10P), C108(H10Q,H10R), C1A(H1AA,H1AB), C1B(H1BA,H1BB), C1C(H1CA,
 H1CB), C1D(H1DA,H1DB)
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),
 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)
;
_shelx_res_checksum              56082
_shelx_hkl_checksum              76160
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'