Regulating the solution structural integrity and slow magnetic relaxation behavior of two Dy6 clusters with a pyridine‒triazole ligand
Li, Hai-Ye; Pang, Xu-Hong; Tao, Ye; Huang, Fu-Ping; Zou, Hua-Hong; Liang, Fu-Pei; New Journal of Chemistry 45 (2021) 7096–7102; doi:10.1039/D1NJ00140J

data_7060466
_publ_section_title
;
 Regulating the solution structural integrity and slow magnetic relaxation
 behavior of two Dy6 clusters with a pyridine--triazole ligand
;
_journal_issue                   16
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              7096
_journal_page_last               7102
_journal_paper_doi               10.1039/D1NJ00140J
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C78 H72 Dy6 N36 O20, 2(N2.5 O)'
_chemical_formula_sum            'C78 H72 Dy6 N41 O22'
_chemical_formula_weight         2910.76
_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     dual
_audit_creation_date             2021-03-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2021-03-16 deposited with the CCDC.	2021-03-19 downloaded from the CCDC.
;
_cell_angle_alpha                83.784(2)
_cell_angle_beta                 75.381(2)
_cell_angle_gamma                88.137(2)
_cell_formula_units_Z            1
_cell_length_a                   12.4747(3)
_cell_length_b                   13.3828(3)
_cell_length_c                   15.3803(4)
_cell_measurement_reflns_used    24447
_cell_measurement_temperature    294.32(19)
_cell_measurement_theta_max      31.4370
_cell_measurement_theta_min      2.2560
_cell_volume                     2469.92(11)
_computing_cell_refinement       'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      294.32(19)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.850
_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     51.00  85.00   0.50   50.00    --   13.79  77.00  60.00   68
  2  \w     -1.00  39.00   0.50   50.00    --   13.79  77.00  60.00   80
  3  \w    -67.00   5.00   0.50   50.00    --   13.79 -19.00 120.00  144
  4  \w    -23.00  27.00   0.50   50.00    --  -12.86 -99.00   0.00  100
  5  \w     -2.00  57.00   0.50   50.00    --   13.79-106.00 -79.00  118
  6  \w    -23.00  27.00   0.50   50.00    --  -12.86 -99.00-120.00  100
  7  \w    -22.00  53.00   0.50   50.00    --   13.79 -99.00-120.00  150
  8  \w    -64.00  21.00   0.50   50.00    --   13.79 -37.00 -30.00  170
  9  \w    -67.00   5.00   0.50   50.00    --   13.79 -19.00-150.00  144
 10  \w    -87.00  10.00   0.50   50.00    --  -12.86 -57.00  60.00  194
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0240214000
_diffrn_orient_matrix_UB_12      0.0225063000
_diffrn_orient_matrix_UB_13      0.0401644000
_diffrn_orient_matrix_UB_21      0.0145680000
_diffrn_orient_matrix_UB_22      0.0482080000
_diffrn_orient_matrix_UB_23      -0.0234003000
_diffrn_orient_matrix_UB_31      -0.0516116000
_diffrn_orient_matrix_UB_32      0.0034588000
_diffrn_orient_matrix_UB_33      -0.0116337000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.850
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            46607
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.850
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.940
_diffrn_reflns_theta_min         2.272
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.569
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74096
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.80a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic light yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.957
_exptl_crystal_description       block
_exptl_crystal_F_000             1399
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.664
_refine_diff_density_min         -1.042
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     689
_refine_ls_number_reflns         14501
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+0.9922P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0865
_refine_ls_wR_factor_ref         0.0948
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10898
_reflns_number_total             14501
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj00140j2.cif
_cod_data_source_block           20210315-dy6-1
_cod_depositor_comments
'Adding full bibliography for 7060465--7060467.cif.'
_cod_database_code               7060466
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N Dy'
_shelx_estimated_absorpt_t_max   0.875
_shelx_estimated_absorpt_t_min   0.804
_reflns_odcompleteness_completeness 99.95
_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. Restrained distances
 O7-N19
 1.39 with sigma of 0.02
 N1A-O12
 1.5 with sigma of 0.02
 N20-N1A
 1.3 with sigma of 0.02
 O9A-N19
 1.39 with sigma of 0.02
3. Rigid bond restraints
 O10, C38
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(O11) \\sim Ueq, Uanis(N1B) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(N1A)
\\sim Ueq, Uanis(N20) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(N17) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C40) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(N18) = Uanis(N19)
Uanis(O9) = Uanis(O9A)
Uanis(C39) = Uanis(C39A)
Uanis(N17) = Uanis(N17A)
Uanis(C40) = Uanis(C40A)
5. Others
 Sof(O9A)=Sof(N19)=1-FVAR(1)
 Sof(O9)=Sof(N18)=FVAR(1)
 Sof(H38A)=Sof(N17A)=Sof(C39A)=Sof(H39D)=Sof(H39E)=Sof(H39F)=1-FVAR(2)
 Sof(H38)=Sof(N17)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=FVAR(2)
 Sof(C40A)=Sof(H40D)=Sof(H40E)=Sof(H40F)=1-FVAR(3)
 Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=FVAR(3)
 Fixed Sof: O11(0.5) O12(0.5) N1B(0.5)
 Fixed X: O11(0.00586) O12(-0.013261) N1B(-0.08372)
 Fixed Y: O11(0.34792) O12(0.128821) N1B(0.234579)
 Fixed Z: O11(0.10476) O12(0.095181) N1B(0.119781)
6.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C23(H23A,H23B)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C12(H12), C13(H13), C14(H14), C15(H15),
 C16(H16), C17(H17), C18(H18), C19(H19), C27(H27), C28(H28), C29(H29), C30(H30),
  C38(H38), C38(H38A)
6.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C39(H39A,H39B,
 H39C), C40(H40A,H40B,H40C), C39A(H39D,H39E,H39F), C40A(H40D,H40E,H40F)
;
_shelx_res_checksum              46716
_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 1.495
_oxdiff_exptl_absorpt_empirical_full_min 0.674