Effects of strong coordination bonds at the axial or equatorial positions on magnetic relaxation for pentagonal bipyramidal dysprosium(III) single-ion magnets.
Li, Min; Han, Jiayi; Wu, Haipeng; Du, Yi-En; Liu, Yufang; Chen, Yongqiang; Chen, Sanping; Dalton transactions (Cambridge, England : 2003) 51 (2022) 16964–16972; doi:10.1039/d2dt02402k

data_7711802
_publ_section_title
;
 Effects of strong coordination bonds at the axial or equatorial positions
 on magnetic relaxation for pentagonal bipyramidal dysprosium(III)
 single-ion magnets.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16964
_journal_page_last               16972
_journal_paper_doi               10.1039/d2dt02402k
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety         'C20 H22 Cl2 Dy N6 O3'
_chemical_formula_sum            'C21 H21 Cl2 Dy N5 O3'
_chemical_formula_weight         624.83
_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             2021-08-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-09-06 deposited with the CCDC.	2022-10-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.146(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6018(2)
_cell_length_b                   21.7017(5)
_cell_length_c                   13.7591(3)
_cell_measurement_reflns_used    8600
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.7370
_cell_measurement_theta_min      3.8920
_cell_volume                     2739.64(11)
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_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    -93.00 -66.00   1.00    0.10    --  -48.45-138.00  23.00   27
  2  \w    -94.00 -46.00   1.00    0.10    --  -48.45 138.00  85.00   48
  3  \w   -119.00 -70.00   1.00    0.10    --  -48.45-131.00-160.00   49
  4  \w     48.00  73.00   1.00    0.10    --   48.45-138.00  23.00   25
  5  \w     44.00  69.00   1.00    0.10    --   48.45-131.00-160.00   25
  6  \w    -27.00  27.00   1.00    0.10    --  -48.45  19.00-180.00   54
  7  \w   -120.00 -73.00   1.00    0.10    --  -48.45-125.00 -30.00   47
  8  \w    -25.00  27.00   1.00    0.10    --  -48.45  19.00 -60.00   52
  9  \w   -133.00-107.00   1.00    0.80    --  -86.25-138.00  23.00   26
 10  \w   -159.00 -83.00   1.00    0.80    --  -86.25-131.00-160.00   76
 11  \w   -111.00 -73.00   1.00    0.80    --  -86.25 -19.00  30.00   38
 12  \w   -162.00-115.00   1.00    0.80    --  -86.25 -19.00  30.00   47
 13  \w     83.00 116.00   1.00    0.80    --  106.49-131.00-160.00   33
 14  \w    107.00 132.00   1.00    0.80    --  106.49 138.00  85.00   25
 15  \w     92.00 125.00   1.00    0.80    --  106.49 131.00 -90.00   33
 16  \w     89.00 121.00   1.00    0.80    --  106.49-138.00  23.00   32
 17  \w     95.00 178.00   1.00    0.80    --  106.49 125.00 120.00   83
 18  \w     94.00 124.00   1.00    0.80    --  106.49  19.00  30.00   30
 19  \w     36.00  66.00   1.00    0.80    --  106.49 -57.00  90.00   30
 20  \w     35.00 105.00   1.00    0.80    --  106.49 -99.00  30.00   70
 21  \w     35.00  65.00   1.00    0.80    --  106.49 -57.00-150.00   30
 22  \w     40.00  66.00   1.00    0.80    --  106.49 -57.00-180.00   26
 23  \w     36.00 105.00   1.00    0.80    --  106.49 -99.00-180.00   69
 24  \w    135.00 162.00   1.00    0.80    --  106.49  19.00  30.00   27
 25  \w     34.00  66.00   1.00    0.80    --  106.49 -57.00  60.00   32
;
_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      -0.0423476000
_diffrn_orient_matrix_UB_12      0.0412952000
_diffrn_orient_matrix_UB_13      -0.0952444000
_diffrn_orient_matrix_UB_21      0.0256360000
_diffrn_orient_matrix_UB_22      0.0576653000
_diffrn_orient_matrix_UB_23      0.0683559000
_diffrn_orient_matrix_UB_31      0.1604141000
_diffrn_orient_matrix_UB_32      0.0016710000
_diffrn_orient_matrix_UB_33      0.0000051000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0801
_diffrn_reflns_av_unetI/netI     0.0623
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18089
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.065
_diffrn_reflns_theta_max         67.065
_diffrn_reflns_theta_min         3.931
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.624
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41475
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_description       block
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.595
_refine_diff_density_min         -1.003
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4852
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0610
_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^)+(0.0428P)^2^+16.4759P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1512
_refine_ls_wR_factor_ref         0.1560
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4125
_reflns_number_total             4852
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02402k2.cif
_cod_data_source_block           2
_cod_original_cell_volume        2739.63(11)
_cod_database_code               7711802
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         DyCNO
_shelx_estimated_absorpt_t_max   0.635
_shelx_estimated_absorpt_t_min   0.490
_diffrn_oxdiff_digest_frames
;
016a623beb5eda8022af02b70f3ead9e8f000277c8b
;
_diffrn_oxdiff_digest_hkl
;
0191901c74152f18676069b7e5132920b09600
;
_reflns_odcompleteness_completeness 99.15
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
2.a Rotating group:
 N5(H5A,H5B)
2.b Ternary CH refined with riding coordinates:
 N2(H2), N3(H3)
2.c Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C6(H6A,H6B), C8(H8A,H8B)
2.d Aromatic/amide H refined with riding coordinates:
 C19(H19), C12(H12), C3(H3A), C16(H16), C4(H4), C11(H11), C17(H17), C13(H13),
 C1(H1), C9(H9), C14(H14), C2(H2A)
;
_shelx_res_checksum              54203
_shelx_fab_checksum              1365
_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 1.645
_oxdiff_exptl_absorpt_empirical_full_min 0.658