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_7711804
_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
'2(C32 H30 Cl3 Dy N10 O9), C32 H29 Cl3 Dy N10 O9, H2 O'
_chemical_formula_sum            'C96 H92 Cl9 Dy3 N30 O28'
_chemical_formula_weight         2920.54
_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
_audit_creation_date             2021-08-03
_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                73.820(2)
_cell_angle_beta                 82.393(2)
_cell_angle_gamma                82.882(2)
_cell_formula_units_Z            2
_cell_length_a                   11.2799(3)
_cell_length_b                   21.7618(6)
_cell_length_c                   25.8284(7)
_cell_measurement_reflns_used    17848
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      74.9920
_cell_measurement_theta_min      3.0960
_cell_volume                     6010.1(3)
_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)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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   -111.00 -37.00   1.00    2.20    --  -48.20 -66.00-169.00   74
  2  \w    -63.00  23.00   1.00    2.20    --  -48.20  66.00 -34.00   86
  3  \w    -21.00  63.00   1.00    2.20    --   48.20 -66.00-169.00   84
  4  \w     36.00 115.00   1.00    2.20    --   48.20  66.00 -34.00   79
  5  \w    -26.00  26.00   1.00    2.20    --  -48.20  19.00 -90.00   52
  6  \w     34.00  95.00   1.00    2.20    --   48.20-125.00  60.00   61
  7  \w    -64.00 -24.00   1.00   25.00    --  -86.25  66.00 -34.00   40
  8  \w   -158.00 -86.00   1.00   25.00    --  -86.25 -66.00-169.00   72
  9  \w    -63.00 -14.00   1.00   25.00    --  -86.25  57.00 150.00   49
 10  \w   -155.00 -86.00   1.00   25.00    --  -86.25 -99.00 -90.00   69
 11  \w     93.00 164.00   1.00   25.00    --  106.49  66.00 -34.00   71
 12  \w     36.00  79.00   1.00   25.00    --  106.49 -66.00-169.00   43
 13  \w     35.00 106.00   1.00   25.00    --  106.49 -99.00 -90.00   71
 14  \w     39.00 174.00   1.00   25.00    --  106.49   0.00 -60.00  135
 15  \w     35.00 106.00   1.00   25.00    --  106.49 -99.00  30.00   71
 16  \w     94.00 178.00   1.00   25.00    --  106.49  19.00  60.00   84
 17  \w     74.00 101.00   1.00   25.00    --  106.49 -99.00-180.00   27
 18  \w     94.00 123.00   1.00   25.00    --  106.49  19.00 150.00   29
 19  \w    127.00 173.00   1.00   25.00    --  106.49  19.00 150.00   46
 20  \w     34.00 105.00   1.00   25.00    --  106.49 -77.00 -60.00   71
 21  \w     34.00 106.00   1.00   25.00    --  106.49 -99.00-150.00   72
 22  \w     36.00 106.00   1.00   25.00    --  106.49 -99.00 -60.00   70
 23  \w     35.00  66.00   1.00   25.00    --  106.49 -57.00  60.00   31
 24  \w     36.00  69.00   1.00   25.00    --  106.49 -99.00-180.00   33
 25  \w     34.00 105.00   1.00   25.00    --  106.49 -99.00 150.00   71
 26  \w     34.00 106.00   1.00   25.00    --  106.49 -99.00  90.00   72
 27  \w     38.00  65.00   1.00   25.00    --  106.49 -57.00 -30.00   27
;
_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      0.0277684000
_diffrn_orient_matrix_UB_12      -0.0669770000
_diffrn_orient_matrix_UB_13      -0.0102736000
_diffrn_orient_matrix_UB_21      -0.0808901000
_diffrn_orient_matrix_UB_22      0.0206260000
_diffrn_orient_matrix_UB_23      -0.0466400000
_diffrn_orient_matrix_UB_31      0.1087718000
_diffrn_orient_matrix_UB_32      0.0238295000
_diffrn_orient_matrix_UB_33      -0.0402172000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0783
_diffrn_reflns_av_unetI/netI     0.0653
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            65718
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.078
_diffrn_reflns_theta_max         67.078
_diffrn_reflns_theta_min         3.122
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.368
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86250
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_description       block
_exptl_crystal_F_000             2906
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.612
_refine_diff_density_min         -1.375
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1595
_refine_ls_number_reflns         21242
_refine_ls_number_restraints     409
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0977
_refine_ls_R_factor_gt           0.0625
_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^)+(0.1154P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1670
_refine_ls_wR_factor_ref         0.1887
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13481
_reflns_number_total             21242
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02402k2.cif
_cod_data_source_block           3
_cod_database_code               7711804
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         DyClCN
_shelx_estimated_absorpt_t_max   0.708
_shelx_estimated_absorpt_t_min   0.638
_diffrn_oxdiff_digest_frames
;
0107003068e8566a22556a1b5dded2fc2d01690c43c
;
_diffrn_oxdiff_digest_hkl
;
0164e6e9d005edcecc53c30df249fedc19a399
;
_reflns_odcompleteness_completeness 98.92
_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
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O5-N6 = O3-N6 = O4-N5 = O2-N5
 1.22 with sigma of 0.01
 O10-N8 = O9-N9 = O8-N8 = O7-N9
 1.22 with sigma of 0.01
 N6-C18 = N5-C18
 1.45 with sigma of 0.01
 O24-N33 = O25-N34 = O26-N33 = O27-N34
 1.22 with sigma of 0.01
 N33-C94 = N34-C94
 1.45 with sigma of 0.01
 Cl4-C16 = Cl3-C16
 1.75 with sigma of 0.01
3. Rigid bond restraints
 Cl2, C25
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
O1 \\sim N7 \\sim C15 \\sim N6 \\sim C18 \\sim O5 \\sim C20 \\sim O3 \\sim C16
\\sim C17 \\sim C19 \\sim O4 \\sim O2 \\sim N5 \\sim Cl4 \\sim Cl3: within 1.7A
with sigma of 0.004 and sigma for terminal atoms of 0.008
C23 \\sim C22 \\sim C21 \\sim C26 \\sim C25 \\sim C24 \\sim Cl2 \\sim O6 \\sim
N10 \\sim N8 \\sim O8 \\sim O9 \\sim O7 \\sim N9 \\sim O10: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.008
Cl9 \\sim Cl10 \\sim C86 \\sim O28 \\sim C85 \\sim C90 \\sim N29 \\sim N30
\\sim C89 \\sim C88 \\sim C87 \\sim N31 \\sim O30 \\sim O29: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.008
C66 \\sim C65 \\sim N26 \\sim C69 \\sim C68 \\sim C67: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.008
Uanis(Cl3) \\sim Ueq, Uanis(O26) \\sim Ueq, Uanis(N33) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.01
5. Others
 Fixed Sof: O10(0.5) N8(0.5) O8(0.5) N6(0.5) O5(0.5) O3(0.5) O24(0.5) O26(0.5)
 N33(0.5) O4(0.5) O2(0.5) N5(0.5) O9(0.5) O7(0.5) N9(0.5) N34(0.5) O25(0.5)
 O27(0.5) N29(0.5) N30(0.5) H29A(0.5) H29B(0.5) Cl9(0.5) Cl10(0.5) Cl4(0.5)
 Cl3(0.5)
6.a Riding coordinates:
 O36(H36A,H36B)
6.b Rotating group:
 N17(H17A,H17B), N32(H32A,H32B), N27(H27A,H27B), N21(H21A,H21B)
6.c Ternary CH refined with riding coordinates:
 N24(H24A), N3(H3), N14(H14A), N2(H2), N15(H15), N25(H25)
6.d Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C72(H72A,H72B), C9(H9A,H9B), C7(H7C,H7D), C8(H8A,H8B), C6(H6A,
 H6B), C71(H71A,H71B), C39(H39A,H39B), C73(H73A,H73B), C41(H41A,H41B), C38(H38A,
 H38B), C70(H70A,H70B), N30(H29A,H29B)
6.e Aromatic/amide H refined with riding coordinates:
 C29(H29), C31(H31), C46(H46), C57(H57), C1(H1), C14(H14), C60(H60), C55(H55),
 C4(H4), C13(H13), C83(H83), C62(H62), C2(H2A), C81(H81), C52(H52), C3(H3A),
 C76(H76), C77(H77), C75(H75), C45(H45), C11(H11), C43(H43), C50(H50), C78(H78),
  C95(H95), C93(H93), C36(H36), C12(H12), C24(H24), C33(H33), C87(H87),
 C89(H89), C44(H44), C22(H22), C35(H35), C68(H68), C67(H67), C17(H17), C19(H19),
  C66(H66), C34(H34), C65(H65)
6.f Fitted hexagon refined as free rotating group:
 C95(C96,C91,C92,C93,C94)
6.g X=CH2 refined with riding coordinates:
 N12(H12A,H12B), N19(H19A,H19B), N7(H7A,H7B), N10(H10A,H10B)
;
_shelx_res_checksum              38121
_shelx_fab_checksum              38134
_platon_squeeze_void_probe_radius 1.20
_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 2.734
_oxdiff_exptl_absorpt_empirical_full_min 0.534