Slow magnetic relaxation in a Dy<sub>3</sub> triangle and a bistriangular Dy<sub>6</sub> cluster.
Wang, Wen; Shang, Tao; Wang, Juan; Yao, Bin-Ling; Li, Li-Cun; Ma, Yue; Wang, Qing-Lun; Zhang, Yuan-Zhu; Zhang, Yi-Quan; Zhao, Bin; Dalton transactions (Cambridge, England : 2003) 51 (2022) 9404–9411; doi:10.1039/d1dt03414f

data_7710382
_publ_section_title
;
 Slow magnetic relaxation in a Dy<sub>3</sub> triangle and a bistriangular
 Dy<sub>6</sub> cluster.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9404
_journal_page_last               9411
_journal_paper_doi               10.1039/d1dt03414f
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety         'C39 H43 Dy3 N6 O13, 2(N O3), 2.295(H2 O)'
_chemical_formula_sum            'C39 H47.59 Dy3 N8 O21.3'
_chemical_formula_weight         1456.66
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-11-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-02-13 deposited with the CCDC.	2022-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                72.659(4)
_cell_angle_beta                 88.383(3)
_cell_angle_gamma                82.404(4)
_cell_formula_units_Z            2
_cell_length_a                   10.8894(5)
_cell_length_b                   13.6662(7)
_cell_length_c                   16.7262(6)
_cell_measurement_reflns_used    15443
_cell_measurement_temperature    150
_cell_measurement_theta_max      32.8020
_cell_measurement_theta_min      1.9660
_cell_volume                     2354.99(19)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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   -115.00  65.00   0.50    3.00    --  -25.00  45.00   0.00  360
  2  \w   -115.00  65.00   0.50    3.00    --  -25.00  45.00  90.00  360
  3  \w   -115.00  65.00   0.50    3.00    --  -25.00  45.00 180.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0434497000
_diffrn_orient_matrix_UB_12      -0.0154974000
_diffrn_orient_matrix_UB_13      -0.0277055000
_diffrn_orient_matrix_UB_21      0.0333606000
_diffrn_orient_matrix_UB_22      0.0414350000
_diffrn_orient_matrix_UB_23      -0.0006714000
_diffrn_orient_matrix_UB_31      0.0363050000
_diffrn_orient_matrix_UB_32      -0.0324040000
_diffrn_orient_matrix_UB_33      0.0347258000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25031
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_min         2.265
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.801
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.054
_exptl_crystal_description       prism
_exptl_crystal_F_000             1412
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.253
_refine_diff_density_min         -2.138
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     689
_refine_ls_number_reflns         9757
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0324
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0330P)^2^+3.2695P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0699
_refine_ls_wR_factor_ref         0.0738
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8363
_reflns_number_total             9757
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03414f2.cif
_cod_data_source_block           r20211101d
_cod_depositor_comments
'Adding full bibliography for 7710382--7710383.cif.'
_cod_original_formula_sum        'C39 H47.59 Dy3 N8 O21.30'
_cod_database_code               7710382
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C20H20N4O4Dy
_reflns_odcompleteness_completeness 89.38
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.90
_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 O(H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N8A) \\sim Ueq, Uanis(O17) \\sim Ueq, Uanis(N8) \\sim Ueq, Uanis(O18)
\\sim Ueq, Uanis(O19) \\sim Ueq, Uanis(O17A) \\sim Ueq, Uanis(O18A) \\sim Ueq,
Uanis(O19A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 N8A, O17, N8, O18, O19, O17A, O18A, O19A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(O17A)=Sof(O18A)=Sof(N8A)=Sof(O19A)=Sof(O22)=Sof(H22a)=Sof(H22b)=1-FVAR(1)
 Sof(O17)=Sof(O18)=Sof(O19)=Sof(N8)=FVAR(1)
5.a Riding coordinates:
 O1(H1), O5(H5), O9(H9), O11(H11a,H11b), O12(H12a,H12b), O13(H13a,H13b),
 O20(H20a,H20b), O21(H21a,H21b), O22(H22a,H22b)
5.b Ternary CH refined with riding coordinates:
 C12(H12), C25(H25), C38(H38)
5.c Secondary CH2 refined with riding coordinates:
 C11(H11c,H11d), C13(H13c,H13d), C24(H24a,H24b), C26(H26a,H26b), C37(H37a,
 H37b), C39(H39a,H39b)
5.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C7(H7a), C8(H8), C10(H10), C15(H15), C16(H16),
 C17(H17), C20(H20), C21(H21), C23(H23), C27(H27), C28(H28), C29(H29), C33(H33),
  C34(H34), C36(H36)
;
_shelx_res_checksum              72359
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.354
_oxdiff_exptl_absorpt_empirical_full_min 0.787