A triangular Dy3 single-molecule toroic with high inversion energy barrier: magnetic properties and multiple-step assembly mechanism
Zhu, Zhong-Hong; Ma, Xiong-Feng; Wang, Hai-Ling; Zou, Hua-Hong; Mo, Kai-Qiang; Zhang, Yi-Quan; Yang, Qi-Zhen; Li, Bo; Liang, Fu-Pei; Inorganic Chemistry Frontiers 5 (2018) 3155–; doi:10.1039/C8QI01069B

data_4349943
_publ_section_title
;
 A triangular Dy3 single-molecule toroic with high inversion energy
 barrier: magnetic properties and multiple-step assembly mechanism
;
_journal_issue                   12
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              3155
_journal_paper_doi               10.1039/C8QI01069B
_journal_volume                  5
_journal_year                    2018
_chemical_formula_moiety         'C45 H45 Dy3 N14 O17, C O'
_chemical_formula_sum            'C46 H45 Dy3 N14 O18'
_chemical_formula_weight         1569.46
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-09-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-16 deposited with the CCDC.
2018-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                101.791(4)
_cell_angle_beta                 101.667(5)
_cell_angle_gamma                111.029(5)
_cell_formula_units_Z            2
_cell_length_a                   12.6762(9)
_cell_length_b                   13.0303(4)
_cell_length_c                   19.2205(10)
_cell_measurement_reflns_used    5184
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4230
_cell_measurement_theta_min      3.5380
_cell_volume                     2765.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9784
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -82.00  -7.00   1.00   26.00    --  -19.88 -57.00-180.00   75
  2  \w    -44.00   7.00   1.00   26.00    --  -19.88 -77.00  90.00   51
  3  \w    -69.00 -30.00   1.00   26.00    --  -19.88 112.00 -79.00   39
  4  \w    -96.00 -69.00   1.00   26.00    --  -19.88-178.00 -60.00   27
  5  \w    -34.00  43.00   1.00   26.00    --  -19.88  57.00  60.00   77
  6  \w    -22.00   5.00   1.00   26.00    --  -19.88 -77.00 150.00   27
  7  \w    -93.00  24.00   1.00   26.00    --  -19.88 -19.00-120.00  117
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0361610000
_diffrn_orient_matrix_UB_12      -0.0081819000
_diffrn_orient_matrix_UB_13      -0.0223996000
_diffrn_orient_matrix_UB_21      -0.0508450000
_diffrn_orient_matrix_UB_22      -0.0293240000
_diffrn_orient_matrix_UB_23      -0.0317730000
_diffrn_orient_matrix_UB_31      0.0077392000
_diffrn_orient_matrix_UB_32      0.0530807000
_diffrn_orient_matrix_UB_33      -0.0072042000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0697
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            21194
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.29
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.094
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63582
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.885
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1522
_refine_diff_density_max         1.082
_refine_diff_density_min         -1.153
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     725
_refine_ls_number_reflns         10837
_refine_ls_number_restraints     505
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0504
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0615P)^2^+10.3178P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1274
_refine_ls_wR_factor_ref         0.1426
_reflns_number_gt                7844
_reflns_number_total             10837
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8qi01069b2.cif
_cod_data_source_block           1
_cod_original_cell_volume        2765.7(2)
_cod_database_code               4349943
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 O9, N12
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
3. Uiso/Uaniso restraints and constraints
O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O8 \\sim O15 \\sim O13 \\sim O16
\\sim O12 \\sim O6 \\sim O7 \\sim O17 \\sim O14 \\sim O10 \\sim O9 \\sim O11
\\sim O18: within 6.1A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C(HA,HB), C6(H6A,H6B), C6BA(H6BA,H6BB), C9BA(H9BA,H9BB), C0EA(H0EA,H0EB)
4.b Aromatic/amide H refined with riding coordinates:
 C3CA(H3CA), C6CA(H6CA), C9CA(H9CA), C1DA(H1DA), C2DA(H2DA), C3DA(H3DA),
 C6DA(H6DA), C7DA(H7DA), C8DA(H8DA), C9DA(H9DA), C1EA(H1EA), C2EA(H2EA),
 C3EA(H3EA), C4EA(H4EA), C5EA(H5EA), C6EA(H6EA), C8EA(H8EA), C9EA(H9EA),
 C0FA(H0FA), C7FA(H7FA)
4.c Idealised Me refined as rotating group:
 C2CA(H2CA,H2CB,H2CC), C5CA(H5CA,H5CB,H5CC), C7CA(H7CA,H7CB,H7CC), C7EA(H7EA,
 H7EB,H7EC), C1FA(H1FA,H1FB,H1FC)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.362
_oxdiff_exptl_absorpt_empirical_full_min 0.756