Magnetic relaxation in two chain-like Zn2Dy2 Schiff base coordination polymers bridged by tetraoxolene and its one-electron reduced radical
Liu, Cai-Ming; Hao, Xiang; New Journal of Chemistry 45 (2021) 19868–19875; doi:10.1039/D1NJ04299H

data_7060986
_publ_section_title
;
 Magnetic relaxation in two chain-like Zn2Dy2 Schiff base coordination
 polymers bridged by tetraoxolene and its one-electron reduced radical
;
_journal_issue                   42
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              19868
_journal_page_last               19875
_journal_paper_doi               10.1039/D1NJ04299H
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C53 H52 Cl4 Dy2 N5 O22 Zn2, 0.5(Cl O4)'
_chemical_formula_sum            'C53 H52 Cl4.5 Dy2 N5 O24 Zn2'
_chemical_formula_weight         1758.26
_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             2021-09-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-09-03 deposited with the CCDC.	2021-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                90.1020(10)
_cell_angle_beta                 100.5900(10)
_cell_angle_gamma                99.6450(10)
_cell_formula_units_Z            2
_cell_length_a                   11.58000(10)
_cell_length_b                   14.76280(10)
_cell_length_c                   19.97170(10)
_cell_measurement_reflns_used    56739
_cell_measurement_temperature    219.99(16)
_cell_measurement_theta_max      74.6320
_cell_measurement_theta_min      2.2470
_cell_volume                     3306.77(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      219.99(16)
_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 0.956
_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     36.00 106.00   0.50    0.50    --   47.57  28.00  81.00  140
  2  \w     94.00 120.00   0.50    2.00    --  103.25  28.00  81.00   52
  3  \w     37.00 118.00   0.50    0.50    --   47.57  38.00 150.00  162
  4  \w     48.00  74.00   0.50    0.50    --   70.00  76.00  89.18   52
  5  \w     44.00  69.00   0.50    0.50    --   66.00  78.00  48.06   50
  6  \w     38.00  65.00   0.50    0.50    --   62.00  80.00  -2.67   54
  7  \w     44.00  69.00   0.50    0.50    --   66.00  78.00 -39.18   50
  8  \w     43.00  69.00   0.50    0.50    --   66.00  78.00  21.78   52
  9  \w     44.00  69.00   0.50    0.50    --   66.00  78.00  64.67   50
 10  \w     31.00  56.00   0.50    0.50    --   54.00  80.00 106.77   50
 11  \w     34.00  60.00   0.50    0.50    --   58.00  79.00 132.45   52
 12  \w     39.00  72.00   0.50    0.50    --   62.00  79.00 154.57   66
 13  \w     15.00  40.00   0.50    0.50    --   42.00  87.00  46.01   50
 14  \w      8.00  33.00   0.50    0.50    --   38.00  92.00  91.85   50
 15  \w    -24.00   4.00   0.50    0.50    --   10.00 103.00 -23.98   56
 16  \w     -8.00  27.00   0.50    0.50    --   22.00  97.00 -85.86   70
 17  \w     15.00  40.00   0.50    0.50    --   42.00  87.00 -43.84   50
 18  \w     31.00  56.00   0.50    0.50    --   54.00  79.00 -43.65   50
 19  \w     26.00  89.00   0.50    0.50    --   50.00  80.00 -84.56  126
 20  \w     88.00 138.00   0.50    0.50    --   66.00  79.00-118.20  100
 21  \w     90.00 115.00   0.50    0.50    --   66.00  79.00-153.44   50
 22  \w     61.00  88.00   0.50    2.00    --   82.00  73.00-106.20   54
 23  \w     38.00  78.00   0.50    0.50    --   62.00  80.00-171.54   80
 24  \w     42.00  80.00   0.50    0.50    --   66.00  79.00-118.20   76
 25  \w     42.00  68.00   0.50    0.50    --   66.00  79.00-153.44   52
 26  \w     13.00  38.00   0.50    0.50    --   42.00  91.00-163.26   50
 27  \w     -8.00  25.00   0.50    0.50    --   22.00  98.00-169.27   66
 28  \w    -19.00   6.00   0.50    0.50    --   47.57 -28.00 -80.00   50
 29  \w     34.00  60.00   0.50    2.00    --  103.25 -94.00-150.00   52
 30  \w     80.00 106.00   0.50    2.00    --  103.25 -94.00-150.00   52
 31  \w     76.00 105.00   0.50    2.00    --  103.25 -94.00 -90.00   58
 32  \w     68.00  99.00   0.50    2.00    --  103.25 -94.00   0.00   62
 33  \w     47.00  73.00   0.50    2.00    --  103.25 -94.00 -90.00   52
 34  \w     45.00  72.00   0.50    2.00    --  103.25 -61.00-120.00   54
 35  \w     33.00  98.00   0.50    2.00    --  103.25 -94.00 -30.00  130
 36  \w     56.00 111.00   0.50    2.00    --  103.25-125.00  90.00  110
 37  \w     32.00 103.00   0.50    2.00    --  103.25-125.00 120.00  142
 38  \w     38.00  73.00   0.50    2.00    --  103.25 -61.00 150.00   70
 39  \w     32.00 109.00   0.50    2.00    --  103.25 -77.00  90.00  154
 40  \w     32.00  77.00   0.50    2.00    --  103.25 -77.00   0.00   90
 41  \w     33.00  59.00   0.50    2.00    --  103.25 -94.00   0.00   52
 42  \w     33.00  66.00   0.50    2.00    --  103.25 -61.00  30.00   66
 43  \w     20.00  92.00   0.50    0.50    --   47.57-125.00   0.00  144
 44  \w    -24.00  25.00   0.50    0.50    --  -47.57  28.00  81.00   98
 45  \w    -52.00 -25.00   0.50    0.50    --  -47.57 -77.00  60.00   54
 46  \w    -56.00 -30.00   0.50    0.50    --  -54.00 -79.00  18.61   52
 47  \w    -64.00 -30.00   0.50    0.50    --  -54.00 -79.00 -10.63   68
 48  \w    -80.00 -51.00   0.50    0.50    --  -47.57 -28.00 -80.00   58
 49  \w    -61.00  24.00   0.50    0.50    --  -47.57  57.00-120.00  170
 50  \w    -68.00 -42.00   0.50    2.00    --  -99.00  61.00-180.00   52
 51  \w   -112.00 -76.00   0.50    2.00    --  -99.00 125.00 -60.00   72
 52  \w    -93.00 -57.00   0.50    2.00    --  -99.00  77.00 -30.00   72
 53  \w   -125.00 -91.00   0.50    2.00    --  -99.00 144.00  51.21   68
 54  \w    -68.00 -26.00   0.50    2.00    --  -99.00 125.00 120.00   84
 55  \w    -68.00 -41.00   0.50    2.00    --  -99.00 153.00 160.36   54
 56  \w   -108.00 -45.00   0.50    2.00    --  -99.00 120.00 179.06  126
 57  \w   -112.00 -79.00   0.50    2.00    --  -99.00 125.00 120.00   66
 58  \w   -131.00 -73.00   0.50    2.00    --  -99.00 153.00 160.36  116
 59  \w    -69.00 -44.00   0.50    0.50    --    6.00 167.00 122.35   50
 60  \w   -118.00 -82.00   0.50    0.50    --  -47.57 -28.00 -80.00   72
 61  \w    -89.00 -53.00   0.50    2.00    --  -74.00 -72.00 -80.44   72
 62  \w    -60.00 -35.00   0.50    0.50    --  -58.00 -77.00-102.89   50
 63  \w    -55.00 -30.00   0.50    0.50    --  -54.00 -80.00-116.52   50
 64  \w    -61.00 -34.00   0.50    0.50    --  -58.00 -80.00-153.76   54
 65  \w    -81.00 -47.00   0.50    0.50    --  -70.00 -76.00-134.96   68
 66  \w    -83.00 -48.00   0.50    0.50    --  -70.00 -75.00 -96.42   70
 67  \w    -79.00 -52.00   0.50    2.00    --  -74.00 -74.00 -50.12   54
 68  \w    -78.00 -52.00   0.50    2.00    --  -74.00 -74.00 -25.01   52
 69  \w    -78.00 -52.00   0.50    2.00    --  -74.00 -74.00  25.20   52
 70  \w    -76.00 -50.00   0.50    2.00    --  -74.00 -80.00  15.46   52
 71  \w    -83.00 -57.00   0.50    2.00    --  -78.00 -73.00  68.63   52
 72  \w    -73.00 -47.00   0.50    0.50    --  -70.00 -76.00 130.37   52
 73  \w    -81.00 -54.00   0.50    2.00    --  -78.00 -79.00 135.43   54
 74  \w    -86.00 -60.00   0.50    2.00    --  -82.00 -75.00 167.35   52
 75  \w    -88.00 -58.00   0.50    2.00    --  -82.00 -79.00 120.80   60
 76  \w    -91.00 -65.00   0.50    2.00    --  -86.00 -72.00  70.95   52
 77  \w    -90.00 -64.00   0.50    2.00    --  -86.00 -75.00  19.19   52
 78  \w    -87.00 -61.00   0.50    2.00    --  -82.00 -73.00  -3.78   52
 79  \w    -90.00 -64.00   0.50    2.00    --  -86.00 -75.00 -16.99   52
 80  \w    -93.00 -67.00   0.50    2.00    --  -90.00 -77.00 -21.87   52
 81  \w    -86.00 -57.00   0.50    2.00    --  -78.00 -72.00 -96.74   58
 82  \w    -82.00 -56.00   0.50    2.00    --  -78.00 -74.00-150.67   52
 83  \w    -83.00 -56.00   0.50    2.00    --  -78.00 -74.00-160.99   54
 84  \w    -85.00 -60.00   0.50    2.00    --  -82.00 -75.00-178.26   50
 85  \w    -89.00 -56.00   0.50    2.00    --  -78.00 -74.00-138.94   66
 86  \w    -89.00 -60.00   0.50    2.00    --  -82.00 -74.00-103.21   58
 87  \w   -100.00 -75.00   0.50    2.00    --  -94.00 -67.00-123.44   50
 88  \w   -112.00 -76.00   0.50    2.00    --  -94.00 -65.00-139.49   72
 89  \w   -140.00 -70.00   0.50    2.00    --  -94.00 -80.00 -46.45  140
 90  \w   -103.00 -67.00   0.50    2.00    --  -90.00 -76.00   2.57   72
 91  \w    -90.00 -64.00   0.50    2.00    --  -86.00 -74.00  61.32   52
 92  \w    -93.00 -65.00   0.50    2.00    --  -86.00 -74.00 100.84   56
 93  \w    -97.00 -66.00   0.50    2.00    --  -86.00 -73.00 179.24   62
 94  \w    -96.00 -71.00   0.50    2.00    --  -94.00 -76.00 179.85   50
 95  \w   -120.00 -68.00   0.50    2.00    --  -90.00 -74.00  41.69  104
 96  \w   -120.00 -73.00   0.50    2.00    --  -94.00 -72.00 -16.13   94
 97  \w   -139.00-101.00   0.50    2.00    --  -86.00 -75.00  19.19   76
 98  \w   -158.00-110.00   0.50    2.00    --  -86.00 -74.00  61.32   96
 99  \w   -150.00-125.00   0.50    2.00    --  -90.00 -74.00  41.69   50
100  \w   -155.00-114.00   0.50    2.00    --  -90.00 -76.00   2.57   82
101  \w   -148.00 -66.00   0.50    2.00    --  -90.00 -80.00 -37.25  164
102  \w   -147.00 -71.00   0.50    2.00    --  -94.00 -77.00 -83.25  152
103  \w   -162.00-127.00   0.50    2.00    --  -99.00 -28.00 -80.00   70
104  \w   -162.00 -75.00   0.50    2.00    --  -90.00 -66.00-111.86  174
105  \w   -162.00-114.00   0.50    2.00    --  -90.00 -77.00 -21.87   96
106  \w   -158.00 -67.00   0.50    2.00    --  -90.00 -77.00  55.75  182
107  \w   -143.00-117.00   0.50    2.00    --  -94.00 -76.00 179.85   52
108  \w   -152.00 -71.00   0.50    2.00    --  -94.00 -77.00 139.35  162
109  \w   -160.00 -68.00   0.50    2.00    --  -90.00 -74.00  14.69  184
110  \w   -164.00-128.00   0.50    2.00    --  -94.00 -72.00 -16.13   72
111  \w   -168.00 -75.00   0.50    2.00    --  -99.00 -80.00 -91.10  186
112  \w   -166.00-127.00   0.50    2.00    --  -94.00 -67.00-123.44   78
113  \w   -166.00 -74.00   0.50    2.00    --  -94.00 -70.00-156.61  184
114  \w   -167.00 -71.00   0.50    2.00    --  -94.00 -77.00-135.00  192
115  \w   -168.00 -75.00   0.50    2.00    --  -99.00 -79.00 103.53  186
116  \w   -166.00 -79.00   0.50    2.00    --  -99.00 -75.00 171.75  174
117  \w   -165.00 -75.00   0.50    2.00    --  -99.00 -79.00 113.13  180
118  \w   -167.00 -79.00   0.50    2.00    --  -99.00 -70.00 157.25  176
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0681494000
_diffrn_orient_matrix_UB_12      -0.0768923000
_diffrn_orient_matrix_UB_13      0.0285357000
_diffrn_orient_matrix_UB_21      -0.1192603000
_diffrn_orient_matrix_UB_22      -0.0646169000
_diffrn_orient_matrix_UB_23      -0.0002418000
_diffrn_orient_matrix_UB_31      -0.0005495000
_diffrn_orient_matrix_UB_32      -0.0336036000
_diffrn_orient_matrix_UB_33      -0.0731489000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0880
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            112669
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.338
_diffrn_reflns_theta_min         2.252
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.061
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_description       block
_exptl_crystal_F_000             1731
_exptl_crystal_preparation       'Magnetic properties'
_refine_diff_density_max         2.447
_refine_diff_density_min         -1.589
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     837
_refine_ls_number_reflns         13098
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0611
_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^)+(0.1031P)^2^+7.9475P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1666
_refine_ls_wR_factor_ref         0.1720
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11192
_reflns_number_total             13098
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj04299h2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7060986--7060987.cif.'
_cod_original_cell_volume        3306.76(4)
_cod_original_formula_sum        'C53 H52 Cl4.50 Dy2 N5 O24 Zn2'
_cod_database_code               7060986
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H22 of O22, H8 of O8, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H21 of O21
2. Restrained distances
 O21-H21
 0.85 with sigma of 0.01
 O8-C32
 1.43 with sigma of 0.01
 C53-H21
 1.950919 with sigma of 0.02
 Dy2-H21
 3.11378 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O27) \\sim Ueq, Uanis(O26) \\sim Ueq, Uanis(O25) \\sim Ueq, Uanis(Cl5)
\\sim Ueq, Uanis(O24) \\sim Ueq, Uanis(C32) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: Cl5(0.5) O24(0.5) O25(0.5) O26(0.5) O27(0.5)
5.a Riding coordinates:
 O8(H8), O21(H21), O22(H22)
5.b :
 Cl5(O24,O25,O26,O27)
5.c Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C41(H41A,H41B), C42(H42A,H42B),
 C43(H43A,H43B)
5.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8A), C12(H12), C14(H14), C15(H15), C16(H16),
 C35(H35), C36(H36), C37(H37), C40(H40), C44(H44), C46(H46), C47(H47), C48(H48)
5.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C19(H19A,H19B,H19C), C32(H32A,H32B,H32C), C33(H33A,H33B,
 H33C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              24660
_shelx_fab_checksum              42657
_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 2.456
_oxdiff_exptl_absorpt_empirical_full_min 0.489