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_7710383
_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         'C60 H51 Dy3 N8 O18'
_chemical_formula_sum            'C60 H51 Dy3 N8 O18'
_chemical_formula_weight         1659.58
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-05-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-05-08 deposited with the CCDC.	2022-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.893(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.0115(11)
_cell_length_b                   17.9550(4)
_cell_length_c                   26.5020(9)
_cell_measurement_reflns_used    7750
_cell_measurement_temperature    116(7)
_cell_measurement_theta_max      28.2410
_cell_measurement_theta_min      3.2470
_cell_volume                     8319.9(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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_environment      N~2~
_diffrn_ambient_temperature      116(7)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2116
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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    -36.00  38.00   1.00   40.00    --   18.94 -57.00  90.00   74
  2  \w    -50.00 -24.00   1.00   40.00    --   18.94 -57.00   0.00   26
  3  \w    -56.00  53.00   1.00   40.00    --  -19.25  19.00 -60.00  109
  4  \w     55.00  86.00   1.00   40.00    --   18.94 178.00  30.00   31
  5  \w    -88.00 -61.00   1.00   40.00    --  -19.25 -57.00   0.00   27
;
_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      -0.0321143000
_diffrn_orient_matrix_UB_12      -0.0071388000
_diffrn_orient_matrix_UB_13      0.0104114000
_diffrn_orient_matrix_UB_21      -0.0117334000
_diffrn_orient_matrix_UB_22      -0.0288596000
_diffrn_orient_matrix_UB_23      -0.0184954000
_diffrn_orient_matrix_UB_31      0.0218042000
_diffrn_orient_matrix_UB_32      -0.0259930000
_diffrn_orient_matrix_UB_33      0.0176111000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_unetI/netI     0.0786
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            36342
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.752
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.724
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77103
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_description       block
_exptl_crystal_F_000             3236
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.701
_refine_diff_density_min         -0.817
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     926
_refine_ls_number_reflns         14526
_refine_ls_number_restraints     559
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_gt           0.0560
_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^)+(0.0599P)^2^+12.5949P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1230
_refine_ls_wR_factor_ref         0.1386
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9910
_reflns_number_total             14526
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03414f2.cif
_cod_data_source_block           p151221a
_cod_depositor_comments
'Adding full bibliography for 7710382--7710383.cif.'
_cod_database_code               7710383
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H O N Dy Na'
_chemical_oxdiff_usercomment     2015102103
_shelx_estimated_absorpt_t_max   0.685
_shelx_estimated_absorpt_t_min   0.612
_reflns_odcompleteness_completeness 99.78
_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 N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C59-C53
 2.4 with sigma of 0.02
 H15A-N8A
 1.8 with sigma of 0.02
 C54-C53
 1.4 with sigma of 0.01
 N8A-C52A
 1.3 with sigma of 0.02
 C36-C37
 1.4 with sigma of 0.02
 O15A-C50A
 1.4 with sigma of 0.02
 H9-H4
 2.2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O15) \\sim Ueq, Uanis(N8) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C51)
\\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C48) \\sim Ueq,
Uanis(C47) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C59A) \\sim Ueq, Uanis(C58A)
\\sim Ueq, Uanis(C57A) \\sim Ueq, Uanis(C56A) \\sim Ueq, Uanis(C55A) \\sim Ueq,
Uanis(C54A) \\sim Ueq, Uanis(C60A) \\sim Ueq, Uanis(C53A) \\sim Ueq,
Uanis(O17A) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C58)
\\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C55) \\sim Ueq,
Uanis(C54) \\sim Ueq, Uanis(N8A) \\sim Ueq, Uanis(C52A) \\sim Ueq, Uanis(C51A)
\\sim Ueq, Uanis(C50A) \\sim Ueq, Uanis(C49A) \\sim Ueq, Uanis(O15A) \\sim Ueq,
Uanis(O17) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C48A) \\sim Ueq, Uanis(C47A)
\\sim Ueq, Uanis(C46A) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C11) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C44) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 Dy3, O14, O15, O15A, O17, O17A, N7, N8, N8A, C46, C46A, C47, C47A, C48, C48A,
 C49, C49A, C50, C50A, C51, C51A, C52, C52A, C53, C53A, C54, C54A, C55, C55A,
 C56, C56A, C57, C57A, C58, C58A, C59, C59A, C60, C60A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O15A)=Sof(H15A)=Sof(O17A)=Sof(N8A)=Sof(C51A)=Sof(C50A)=Sof(C49A)=
 Sof(H49A)=Sof(C48A)=Sof(H48A)=Sof(C47A)=Sof(H47A)=Sof(C46A)=Sof(H46A)=
 Sof(C52A)=Sof(C53A)=Sof(H53A)=Sof(C59A)=Sof(C58A)=Sof(C57A)=Sof(H57A)=
 Sof(C56A)=Sof(H56A)=Sof(C55A)=Sof(H55A)=Sof(C54A)=Sof(C60A)=Sof(H60D)=
 Sof(H60E)=Sof(H60F)=1-FVAR(1)
 Sof(O15)=Sof(H15)=Sof(O17)=Sof(N8)=Sof(C51)=Sof(C50)=Sof(C49)=Sof(H49)=
 Sof(C48)=Sof(H48)=Sof(C47)=Sof(H47)=Sof(C46)=Sof(H46)=Sof(C52)=Sof(C53)=
 Sof(H53)=Sof(C59)=Sof(C58)=Sof(C57)=Sof(H57)=Sof(C56)=Sof(H56)=Sof(C55)=
 Sof(H55)=Sof(C54)=Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(H60C)=FVAR(1)
6.a Riding coordinates:
 O1(H1), O2(H2)
6.b Aromatic/amide H refined with riding coordinates:
 N4(H4), N5(H5), C3(H3), C4(H4A), C5(H5A), C8(H8), C12(H12), C13(H13),
 C14(H14), C15(H15B), C18(H18), C19(H19), C20(H20), C23(H23), C27(H27),
 C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C38(H38),
  C40(H40), C41(H41), C42(H42), C49(H49), C48(H48), C47(H47), C46(H46),
 C49A(H49A), C48A(H48A), C47A(H47A), C46A(H46A), C53(H53), C53A(H53A), C57(H57),
  C56(H56), C55(H55), C57A(H57A), C56A(H56A), C55A(H55A)
6.c Fitted hexagon refined as free rotating group:
 C51(C50,C49,C48,C47,C46), C51A(C50A,C49A,C48A,C47A,C46A), C59(C58,C57,C56,C55,
 C54), C59A(C58A,C57A,C56A,C55A,C54A)
6.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C16(H16A,H16B,H16C), C45(H45A,H45B,H45C), C60(H60A,H60B,
 H60C), C60A(H60D,H60E,H60F)
6.e Idealised tetrahedral OH refined as rotating group:
 O9(H9), O11(H11), O15(H15), O15A(H15A)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 336 electrons were 
found in a volume of 3304\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
8.5[H2O] per Asymmetric Unit 
which account for 340 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              64869
_shelx_fab_checksum              58862
_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 1.462
_oxdiff_exptl_absorpt_empirical_full_min 0.825