Hard Single-Molecule Magnet Behavior By a Linear Trinuclear Lanthanide-[1]Metallocenophane Complex.
Latendresse, Trevor P.; Bhuvanesh, Nattamai S.; Nippe, Michael; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b08690

data_4126598
_publ_section_title
;
 Hard Single-Molecule Magnet Behavior By a Linear Trinuclear
 Lanthanide-[1]Metallocenophane Complex.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b08690
_journal_year                    2017
_chemical_formula_moiety
'C68 H64 Dy3 Fe6 Li2 O2, C24 H48 I Li2 O6, 2(C4 H8 O)'
_chemical_formula_sum            'C100 H128 Dy3 Fe6 I Li4 O10'
_chemical_formula_weight         2467.28
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-08-11
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_cell_angle_alpha                101.096(6)
_cell_angle_beta                 105.259(5)
_cell_angle_gamma                104.987(6)
_cell_formula_units_Z            1
_cell_length_a                   10.9826(18)
_cell_length_b                   13.462(2)
_cell_length_c                   17.649(3)
_cell_measurement_reflns_used    9590
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.764
_cell_measurement_theta_min      2.313
_cell_volume                     2334.8(7)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_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 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0506
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            52991
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        22.496
_diffrn_reflns_theta_max         22.496
_diffrn_reflns_theta_min         2.492
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.659
_exptl_absorpt_correction_T_max  0.2594
_exptl_absorpt_correction_T_min  0.1482
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1302 before and 0.0794 after correction. The Ratio of minimum to maximum transmission is 0.5713. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_description       block
_exptl_crystal_F_000             1227
_exptl_crystal_size_max          0.241
_exptl_crystal_size_mid          0.179
_exptl_crystal_size_min          0.098
_refine_diff_density_max         1.549
_refine_diff_density_min         -1.162
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     610
_refine_ls_number_reflns         5988
_refine_ls_number_restraints     517
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0545
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+48.7776P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1190
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5224
_reflns_number_total             5988
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b08690_si_001.cif
_cod_data_source_block           mntl036
_cod_original_cell_volume        2334.7(7)
_cod_database_code               4126598
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.716
_shelx_estimated_absorpt_t_min   0.473
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O2A-Li2 \\sim O2-Li2
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
I1 \\sim O3 \\sim O4 \\sim O2 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim O2A
\\sim C35A \\sim C36A \\sim C37A \\sim C38A \\sim C39 \\sim C40 \\sim C41 \\sim
C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim Li2: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.01
O2 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim O2A \\sim C35A \\sim C36A
\\sim C37A \\sim C38A: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
O1 \\sim Li1 \\sim C21 \\sim C11: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 I1, O2, O3, O4, C35, C36, C37, C38, C39, C40, C41, C42, C43, C44, C45, C46, Li2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O2, C35, C36, C37, C38, O2A, C35A, C36A, C37A, C38A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 O1, Li1, C21, C11
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C1, C2, C3, C4, C5
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
5. Same fragment restrains
{O1, C31, C32, C33, C34} sigma for 1-2: 0.005, 1-3: 0.04
as
{O2, C35, C36, C37, C38}
{O1, C31, C32, C33, C34} sigma for 1-2: 0.005, 1-3: 0.04
as
{O2A, C35A, C36A, C37A, C38A}
6. Others
 Fixed Sof: I1(0.5) O2(0.5) C35(0.5) H35A(0.5) H35B(0.5) C36(0.5) H36A(0.5)
 H36B(0.5) C37(0.5) H37A(0.5) H37B(0.5) C38(0.5) H38A(0.5) H38B(0.5) O2A(0.5)
 C35A(0.5) H35C(0.5) H35D(0.5) C36A(0.5) H36C(0.5) H36D(0.5) C37A(0.5)
 H37C(0.5) H37D(0.5) C38A(0.5) H38C(0.5) H38D(0.5)
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), C35A(H35C,H35D),
 C36A(H36C,H36D), C37A(H37C,H37D), C38A(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)
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)
;
_shelx_res_checksum              94386
_shelx_hkl_checksum              70996
_olex2_submission_special_instructions 'No special instructions were received'