A family of mono-, di-, and tetranuclear DyIII complexes bearing the ligand 2,6-diacetylpyridine bis(picolinoylhydrazone) and exhibiting slow relaxation of magnetization
Armenis, Alexandros; Bakali, Georgia; Brantley, ChristiAnna; Raptopoulou, Catherine; Psycharis, Vassilis; Cunha-Silva, Luis; Christou, George; Stamatatos, Theocharis; Dalton Transactions  (2022) –; doi:10.1039/D2DT02921A

data_7711670
_publ_section_title
;
 A family of mono-, di-, and tetranuclear DyIII complexes bearing the
 ligand 2,6-diacetylpyridine bis(picolinoylhydrazone) and exhibiting slow
 relaxation of magnetization
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02921A
_journal_year                    2022
_chemical_formula_moiety         'C44 H48 Dy2 N14 O8, 4(Cl O4), 2(C H4 O)'
_chemical_formula_sum            'C46 H56 Cl4 Dy2 N14 O26'
_chemical_formula_weight         1687.84
_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     dual
_audit_creation_date             2021-07-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-09-05 deposited with the CCDC.	2022-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                83.959(2)
_cell_angle_beta                 88.819(2)
_cell_angle_gamma                65.389(2)
_cell_formula_units_Z            1
_cell_length_a                   11.7041(3)
_cell_length_b                   11.8358(2)
_cell_length_c                   12.0835(2)
_cell_measurement_reflns_used    34749
_cell_measurement_temperature    173.00(2)
_cell_measurement_theta_max      76.2460
_cell_measurement_theta_min      3.6420
_cell_volume                     1512.88(6)
_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 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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173.00(2)
_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 0.999
_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    -96.00 -69.00   1.00    0.10    --  -48.45 141.00 113.00   27
  2  \w    -86.00 -59.00   1.00    0.10    --  -48.45 129.00 -58.00   27
  3  \w     26.00 120.00   1.00    0.10    --   48.45  77.00 -30.00   94
  4  \w    -27.00  26.00   1.00    0.10    --  -48.45  19.00  60.00   53
  5  \w    -89.00 -29.00   1.00    0.10    --  -86.25 129.00 -58.00   60
  6  \w    -26.00  25.00   1.00    0.10    --  -48.45  19.00 -30.00   51
  7  \w     90.00 168.00   1.00    0.10    --  106.49  77.00 -60.00   78
  8  \w     94.00 178.00   1.00    0.10    --  106.49  19.00  90.00   84
  9  \w    100.00 176.00   1.00    0.10    --  106.49 125.00-120.00   76
 10  \w    121.00 177.00   1.00    0.10    --  106.49 129.00 -58.00   56
 11  \w    119.00 145.00   1.00    0.10    --  106.49 141.00 113.00   26
 12  \w     84.00 117.00   1.00    0.10    --  106.49 141.00 113.00   33
 13  \w     34.00  66.00   1.00    0.10    --  106.49 -57.00  60.00   32
 14  \w     38.00  87.00   1.00    0.10    --   48.45-129.00-132.00   49
 15  \w     50.00  96.00   1.00    0.10    --   48.45-141.00  55.00   46
 16  \w     36.00  94.00   1.00    0.10    --  106.49 -77.00 -90.00   58
 17  \w     34.00  71.00   1.00    0.10    --  106.49 -99.00 -90.00   37
 18  \w     71.00 114.00   1.00    0.10    --  106.49-129.00-132.00   43
 19  \w     35.00 111.00   1.00    0.10    --  106.49-125.00-180.00   76
 20  \w     34.00 111.00   1.00    0.10    --  106.49-125.00 -90.00   77
 21  \w     74.00 104.00   1.00    0.10    --  106.49 -99.00 -90.00   30
 22  \w     96.00 122.00   1.00    0.10    --  106.49-141.00  55.00   26
 23  \w     35.00 109.00   1.00    0.10    --  106.49-125.00  60.00   74
 24  \w     35.00  96.00   1.00    0.10    --  106.49 -99.00  60.00   61
 25  \w   -159.00 -73.00   1.00    0.10    --  -86.25 -38.00 -90.00   86
 26  \w   -139.00-114.00   1.00    0.10    --  -86.25-129.00-132.00   25
 27  \w   -117.00 -73.00   1.00    0.10    --  -48.45-129.00-132.00   44
 28  \w   -109.00 -71.00   1.00    0.10    --  -48.45-141.00  55.00   38
 29  \w   -140.00 -77.00   1.00    0.10    --  -86.25-141.00  55.00   63
 30  \w   -159.00 -71.00   1.00    0.10    --  -86.25 -57.00  60.00   88
 31  \w     50.00  94.00   1.00    0.10    --   48.45  38.00-150.00   44
 32  \w    -11.00  32.00   1.00    0.10    --   18.00  91.00  97.50   43
 33  \w     -7.00  20.00   1.00    0.10    --   26.00  98.00 -94.50   27
 34  \w     10.00  35.00   1.00    0.10    --   38.00  89.00 117.29   25
 35  \w      7.00  32.00   1.00    0.10    --   38.00  94.00   8.86   25
 36  \w     17.00  42.00   1.00    0.10    --   46.00  90.00 176.84   25
 37  \w    -69.00 -40.00   1.00    0.10    --  -48.45 -19.00 -30.00   29
 38  \w   -123.00 -83.00   1.00    0.10    --  -48.45 -19.00 -30.00   40
 39  \w    -52.00 -26.00   1.00    0.10    --  -48.45 -77.00  90.00   26
 40  \w    -51.00 -26.00   1.00    0.10    --  -48.45 -77.00 150.00   25
 41  \w    -64.00 -36.00   1.00    0.10    --  -48.45 -19.00-150.00   28
 42  \w     36.00  62.00   1.00    0.10    --   48.45  38.00  30.00   26
 43  \w     69.00  97.00   1.00    0.10    --   48.45  38.00  30.00   28
 44  \w     27.00  53.00   1.00    0.10    --   50.00  77.00 -78.02   26
 45  \w     33.00  62.00   1.00    0.10    --   54.00  74.00 176.46   29
 46  \w     91.00 116.00   1.00    0.10    --   54.00  76.00 134.28   25
 47  \w     33.00  59.00   1.00    0.10    --   54.00  76.00 134.28   26
 48  \w     32.00  58.00   1.00    0.10    --   54.00  75.00 -66.57   26
 49  \w    -64.00 -38.00   1.00    0.10    --  -58.00 -74.00   5.10   26
 50  \w     38.00  64.00   1.00    0.10    --   58.00  74.00 -17.10   26
 51  \w     39.00  65.00   1.00    0.10    --   58.00  72.00 -38.17   26
 52  \w    -67.00 -42.00   1.00    0.10    --  -62.00 -69.00  49.88   25
 53  \w   -113.00 -88.00   1.00    0.10    --  -62.00 -69.00  49.88   25
 54  \w    -65.00 -39.00   1.00    0.10    --  -62.00 -76.00-153.27   26
 55  \w     40.00  65.00   1.00    0.10    --   62.00  75.00-140.58   25
 56  \w     41.00  66.00   1.00    0.10    --   62.00  74.00  79.85   25
 57  \w     40.00  65.00   1.00    0.10    --   62.00  76.00-122.57   25
 58  \w     41.00  67.00   1.00    0.10    --   62.00  73.00  27.25   26
 59  \w    -72.00 -46.00   1.00    0.10    --  -66.00 -69.00  36.23   26
 60  \w    -70.00 -45.00   1.00    0.10    --  -66.00 -72.00 -36.74   25
 61  \w    -71.00 -46.00   1.00    0.10    --  -66.00 -69.00-178.22   25
 62  \w    -72.00 -47.00   1.00    0.10    --  -66.00 -68.00 154.28   25
 63  \w     45.00  71.00   1.00    0.10    --   66.00  73.00 -88.90   26
 64  \w     44.00  70.00   1.00    0.10    --   66.00  76.00-119.01   26
 65  \w    -76.00 -50.00   1.00    0.10    --  -70.00 -69.00 131.58   26
 66  \w    -78.00 -53.00   1.00    0.10    --  -74.00 -72.00 136.73   25
 67  \w     52.00  78.00   1.00    0.10    --   74.00  76.00 117.60   26
 68  \w    -82.00 -56.00   1.00    0.10    --  -74.00 -66.00 171.35   26
 69  \w    -81.00 -55.00   1.00    0.10    --  -74.00 -69.00  -2.51   26
 70  \w    -86.00 -55.00   1.00    0.10    --  -74.00 -69.00  67.54   31
 71  \w    -79.00 -53.00   1.00    0.10    --  -74.00 -73.00 120.67   26
 72  \w    -78.00 -52.00   1.00    0.10    --  -74.00 -74.00 104.28   26
 73  \w    -83.00 -57.00   1.00    0.10    --  -74.00 -64.00 -88.83   26
 74  \w    -85.00 -60.00   1.00    0.10    --  -78.00 -68.00   7.77   25
 75  \w    -88.00 -62.00   1.00    0.10    --  -78.00 -64.00 160.58   26
 76  \w    -86.00 -60.00   1.00    0.10    --  -82.00 -74.00 100.82   26
 77  \w    -85.00 -60.00   1.00    0.10    --  -82.00 -74.00 -93.31   25
 78  \w   -152.00-127.00   1.00    0.10    --  -82.00 -74.00 -93.31   25
 79  \w   -149.00-122.00   1.00    0.10    --  -86.00 -69.00   4.69   27
 80  \w    -92.00 -66.00   1.00    0.10    --  -86.00 -69.00   4.69   26
 81  \w   -125.00-100.00   1.00    0.10    --  -86.25 -72.00 -18.05   25
 82  \w    -91.00 -63.00   1.00    0.10    --  -86.25 -77.00-180.00   28
 83  \w   -126.00 -64.00   1.00    0.10    --  -86.25 -77.00 -30.00   62
 84  \w    -93.00 -68.00   1.00    0.10    --  -86.25 -66.00 -92.49   25
 85  \w   -153.00-127.00   1.00    0.10    --  -86.25 -77.00-180.00   26
 86  \w   -144.00-118.00   1.00    0.10    --  -86.25 -66.00 -92.49   26
 87  \w   -155.00-130.00   1.00    0.10    --  -86.25 -57.00 120.00   25
 88  \w    -90.00 -64.00   1.00    0.10    --  -86.25 -76.00  79.74   26
 89  \w    -92.00 -67.00   1.00    0.10    --  -86.25 -72.00 -58.95   25
 90  \w    -93.00 -66.00   1.00    0.10    --  -86.25 -75.00  51.75   27
 91  \w   -115.00 -66.00   1.00    0.10    --  -86.25 -74.00 168.41   49
 92  \w    -91.00 -65.00   1.00    0.10    --  -86.25 -73.00-108.17   26
 93  \w    -89.00 -63.00   1.00    0.10    --  -86.25 -77.00 150.00   26
 94  \w    -99.00 -71.00   1.00    0.10    --  -86.25 -63.00  90.72   28
 95  \w   -100.00 -67.00   1.00    0.10    --  -86.25 -72.00 130.03   33
 96  \w   -127.00-101.00   1.00    0.10    --  -86.25 -75.00  51.75   26
 97  \w   -148.00-122.00   1.00    0.10    --  -86.25 -63.00  90.72   26
 98  \w   -155.00-130.00   1.00    0.10    --  -86.25 -72.00 130.03   25
 99  \w   -111.00 -65.00   1.00    0.10    --  -86.25 -77.00-150.00   46
100  \w    -92.00 -65.00   1.00    0.10    --  -86.25 -74.00  31.48   27
101  \w    -94.00 -69.00   1.00    0.10    --  -86.25 -66.00 -55.61   25
102  \w    -90.00 -65.00   1.00    0.10    --  -86.25 -73.00   1.21   25
103  \w    -92.00 -67.00   1.00    0.10    --  -86.25 -77.00 -90.00   25
104  \w    -92.00 -64.00   1.00    0.10    --  -86.25 -77.00-120.00   28
105  \w   -140.00-114.00   1.00    0.10    --  -86.25 -77.00-120.00   26
106  \w    -98.00 -66.00   1.00    0.10    --  -86.25 -72.00 -26.90   32
107  \w    -96.00 -71.00   1.00    0.10    --  -86.25 -73.00-159.83   25
108  \w   -131.00 -70.00   1.00    0.10    --  -86.25 -69.00-144.98   61
109  \w    -90.00 -65.00   1.00    0.10    --  -86.25 -72.00 -18.05   25
110  \w   -108.00 -65.00   1.00    0.10    --  -86.25 -76.00 -66.43   43
111  \w   -107.00 -81.00   1.00    0.10    --  -86.25 -57.00 120.00   26
112  \w    -90.00 -65.00   1.00    0.10    --  -86.25 -72.00  64.93   25
113  \w    146.00 172.00   1.00    0.10    --  106.49  38.00  30.00   26
114  \w     76.00 102.00   1.00    0.10    --  106.49-125.00   0.00   26
115  \w    100.00 144.00   1.00    0.10    --  106.49  38.00  30.00   44
116  \w     34.00  69.00   1.00    0.10    --  106.49-125.00   0.00   35
117  \w     93.00 147.00   1.00    0.10    --  106.49  77.00 -30.00   54
118  \w    146.00 177.00   1.00    0.10    --  106.49  38.00-180.00   31
119  \w    100.00 133.00   1.00    0.10    --  106.49  38.00-180.00   33
120  \w     86.00 123.00   1.00    0.10    --  106.49  77.00 150.00   37
121  \w    140.00 168.00   1.00    0.10    --  106.49  77.00-120.00   28
122  \w     90.00 132.00   1.00    0.10    --  106.49  77.00-120.00   42
123  \w     96.00 177.00   1.00    0.10    --  106.49  19.00 120.00   81
124  \w     36.00  64.00   1.00    0.10    --  106.49 -57.00 -90.00   28
125  \w     97.00 131.00   1.00    0.10    --  106.49  57.00-120.00   34
126  \w     36.00  62.00   1.00    0.10    --  106.49 -77.00 -30.00   26
127  \w     39.00  64.00   1.00    0.10    --  106.49 -57.00  30.00   25
128  \w     95.00 163.00   1.00    0.10    --  106.49 125.00-150.00   68
129  \w     34.00  60.00   1.00    0.10    --  106.49 -57.00-180.00   26
130  \w     71.00 105.00   1.00    0.10    --  106.49 -99.00-150.00   34
131  \w     82.00 107.00   1.00    0.10    --  106.49-125.00  90.00   25
132  \w     34.00  59.00   1.00    0.10    --  106.49-125.00  90.00   25
;
_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      -0.1427205000
_diffrn_orient_matrix_UB_12      0.0413395000
_diffrn_orient_matrix_UB_13      0.0115896000
_diffrn_orient_matrix_UB_21      0.0174924000
_diffrn_orient_matrix_UB_22      -0.0253379000
_diffrn_orient_matrix_UB_23      0.1275893000
_diffrn_orient_matrix_UB_31      -0.0173024000
_diffrn_orient_matrix_UB_32      0.1355732000
_diffrn_orient_matrix_UB_33      0.0058276000
_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  0.1439
_diffrn_reflns_av_unetI/netI     0.0575
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            45553
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.078
_diffrn_reflns_theta_max         67.078
_diffrn_reflns_theta_min         3.680
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.524
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.01116
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.853
_exptl_crystal_description       plate
_exptl_crystal_F_000             838
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.196
_refine_diff_density_min         -1.855
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         5388
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0955P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1270
_refine_ls_wR_factor_ref         0.1281
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5162
_reflns_number_total             5388
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02921a2.cif
_cod_data_source_block           210708h
_cod_database_code               7711670
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         DyCN
_shelx_estimated_absorpt_t_max   0.576
_shelx_estimated_absorpt_t_min   0.456
_reflns_odcompleteness_completeness 99.89
_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 N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O6-H6
 0.85 with sigma of 0.01
 Dy1-H6
 2.936308 with sigma of 0.02
 C17-H6
 1.900053 with sigma of 0.02
3.a Rotating group:
 O4(H4A,H4B)
3.b Aromatic/amide H refined with riding coordinates:
 N6(H6A), C1(H1), C3(H3), C4(H4), C5(H5), C6(H6B), C14(H14), C15(H15),
 C18(H18), C19(H19), C21(H21), C23(H23)
3.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C13(H13A,H13B,H13C), C17(H17A,H17B,H17C), C11(H11A,H11B,
 H11C)
3.d Idealised tetrahedral OH refined as rotating group:
 O3(H3A)
;
_shelx_res_checksum              27469
_shelx_hkl_checksum              13511
_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 51.253
_oxdiff_exptl_absorpt_empirical_full_min 0.428