Tuning spin dynamics of binuclear Dy complexes using different nitroxide biradical derivatives.
Song, Hongwei; Jin, Chaoyi; Wang, Xiaotong; Xie, Junfang; Ma, Yue; Tang, Jinkui; Li, Licun; Dalton transactions (Cambridge, England : 2003) 53 (2024) 10007–10017; doi:10.1039/d3dt04360f

data_7716129
_publ_section_title
;
 Tuning spin dynamics of binuclear Dy complexes using different nitroxide
 biradical derivatives.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10007
_journal_page_last               10017
_journal_paper_doi               10.1039/d3dt04360f
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C100 H72 Dy2 F60 N10 O30 Zn2'
_chemical_formula_sum            'C100 H72 Dy2 F60 N10 O30 Zn2'
_chemical_formula_weight         3489.41
_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
_audit_creation_date             2023-12-25
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2023-12-25 deposited with the CCDC.	2024-05-21 downloaded from the CCDC.
;
_cell_angle_alpha                113.099(2)
_cell_angle_beta                 90.6130(10)
_cell_angle_gamma                105.1620(10)
_cell_formula_units_Z            1
_cell_length_a                   14.2934(2)
_cell_length_b                   15.4505(2)
_cell_length_c                   16.4647(3)
_cell_measurement_reflns_used    23216
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      73.3180
_cell_measurement_theta_min      2.9410
_cell_volume                     3201.73(10)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.958
_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     33.00 112.00   0.50    0.08    --   73.49   0.00-150.00  158
  2  \w     76.00 127.00   0.50    0.08    --   75.16  30.00 -90.00  102
  3  \w     89.00 115.00   0.50    0.08    --   73.49  30.00 -60.00   52
  4  \w     61.00  86.00   0.50    0.08    --   73.49 155.00  62.00   50
  5  \w     62.00  87.00   0.50    0.08    --   75.16 155.00  62.00   50
  6  \w     84.00 117.00   0.50    0.08    --   73.49 125.00 120.00   66
  7  \w     81.00 106.00   0.50    0.08    --   75.16 125.00  60.00   50
  8  \w     29.00 106.00   0.50    0.08    --   75.16-120.00-177.00  154
  9  \w     28.00  53.00   0.50    0.05    --   59.62-120.00-177.00   50
 10  \w     18.00  54.00   0.50    0.05    --   59.62 -95.00-180.00   72
 11  \w     79.00 124.00   0.50    0.08    --   73.49-155.00  24.00   90
 12  \w     56.00  81.00   0.50    0.08    --   75.16-155.00  24.00   50
 13  \w     52.00  77.00   0.50    0.05    --   59.62-155.00  24.00   50
 14  \w     18.00  43.00   0.50    0.05    --   59.62 -95.00  60.00   50
 15  \w     34.00  75.00   0.50    0.08    --   73.49 -95.00  30.00   82
 16  \w     31.00  86.00   0.50    0.08    --   73.49 -95.00  90.00  110
 17  \w     19.00  69.00   0.50    0.05    --   59.62 -95.00   0.00  100
 18  \w     36.00  80.00   0.50    0.08    --   73.49 -95.00 -90.00   88
 19  \w     34.00  61.00   0.50    0.08    --   75.16 -95.00-150.00   54
 20  \w     34.00  86.00   0.50    0.08    --   73.49 -95.00-180.00  104
 21  \w    -37.00  -9.00   0.50    0.05    --  -60.23  30.00  30.00   56
 22  \w    -38.00 -12.00   0.50    0.05    --  -60.23  30.00 -30.00   52
 23  \w    -37.00 -12.00   0.50    0.05    --  -60.23  30.00-120.00   50
 24  \w    -75.00 -50.00   0.50    0.05    --  -60.23 155.00  62.00   50
 25  \w   -106.00 -81.00   0.50    0.08    --  -74.38 155.00  62.00   50
 26  \w    -87.00 -62.00   0.50    0.08    --  -82.00 155.00  62.00   50
 27  \w   -111.00 -49.00   0.50    0.08    --  -82.00 125.00  60.00  124
 28  \w   -123.00 -50.00   0.50    0.08    --  -81.26 141.00 -13.87  146
 29  \w   -110.00 -39.00   0.50    0.08    --  -82.00 125.00 -60.00  142
 30  \w    -80.00 -55.00   0.50    0.05    --  -60.23 120.00 -94.00   50
 31  \w   -109.00 -81.00   0.50    0.08    --  -81.26 114.00-128.23   56
 32  \w   -109.00 -38.00   0.50    0.08    --  -81.26 114.00-165.41  142
 33  \w    -64.00 -39.00   0.50    0.08    --  -81.26 114.00-128.23   50
 34  \w    -84.00 -47.00   0.50    0.08    --  -82.00 120.00 -94.00   74
 35  \w   -112.00 -79.00   0.50    0.05    --  -60.23 -30.00-150.00   66
 36  \w   -131.00 -83.00   0.50    0.08    --  -82.00 -30.00-180.00   96
 37  \w   -129.00 -81.00   0.50    0.08    --  -82.00 -30.00-120.00   96
 38  \w   -126.00 -80.00   0.50    0.08    --  -82.00 -30.00 -60.00   92
 39  \w   -124.00 -68.00   0.50    0.08    --  -74.38 -15.00   0.00  112
 40  \w   -120.00 -72.00   0.50    0.08    --  -74.38 -30.00  60.00   96
 41  \w   -128.00 -84.00   0.50    0.08    --  -82.00-125.00  60.00   88
 42  \w    -96.00 -71.00   0.50    0.08    --  -82.00-155.00  24.00   50
 43  \w   -113.00 -88.00   0.50    0.08    --  -74.38-155.00  24.00   50
 44  \w   -129.00 -82.00   0.50    0.08    --  -82.00-125.00 -30.00   94
 45  \w   -123.00 -96.00   0.50    0.08    --  -82.00-125.00 -90.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0630519000
_diffrn_orient_matrix_UB_12      0.0384285000
_diffrn_orient_matrix_UB_13      0.0736425000
_diffrn_orient_matrix_UB_21      0.0782455000
_diffrn_orient_matrix_UB_22      0.0091768000
_diffrn_orient_matrix_UB_23      0.0703591000
_diffrn_orient_matrix_UB_31      0.0507793000
_diffrn_orient_matrix_UB_32      0.1061128000
_diffrn_orient_matrix_UB_33      0.0120494000
_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  0.0539
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            47869
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.492
_diffrn_reflns_theta_min         2.942
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.050
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic light colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.810
_exptl_crystal_description       block
_exptl_crystal_F_000             1714
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
TITL exp_312_autored_a.res in P-1
CELL   14.2934   15.4505   16.4647    113.10     90.61    105.16
SPGR P-1
Q101 0.811 0.684 0.341 !       5.61 eA-3
Q102 0.546 0.954 0.049 !       4.68 eA-3
Q103 0.816 0.627 0.299 !       2.69 eA-3
Q104 0.299 0.907 0.221 !       1.86 eA-3
Q105 0.519 0.098 0.059 !       1.78 eA-3
Q106 0.608 0.995 0.110 !       1.59 eA-3
Q107 0.641 0.055 0.218 !       1.57 eA-3
Q108 0.265 0.822 0.142 !       1.52 eA-3
Q109 0.643 0.699 0.439 !       1.51 eA-3
Q110 0.560 0.794 0.022 !       1.49 eA-3
Q111 0.574 0.347 0.284 !       1.46 eA-3
Q112 0.395 0.041 0.002 !       1.44 eA-3
Q113 0.277 0.765 0.176 !       1.44 eA-3
Q114 0.596 0.515 0.364 !       1.43 eA-3
Q115 0.593 0.441 0.360 !       1.43 eA-3
Q116 0.838 0.531 0.328 !       1.43 eA-3
Q117 0.465 0.918 0.128 !       1.40 eA-3
Q118 0.438 0.860 0.139 !       1.37 eA-3
Q119 0.406 0.060 0.481 !       1.36 eA-3
Q120 0.636 0.608 0.443 !       1.35 eA-3
Q121 0.611 0.013 0.050 !       1.33 eA-3
Q122 0.369 0.983 0.245 !       1.33 eA-3
Q123 0.863 0.727 0.424 !       1.33 eA-3
Q124 0.014 0.216 0.364 !       1.30 eA-3
Q125 0.651 0.198 0.375 !       1.28 eA-3
Q126 0.700 0.062 0.365 !       1.28 eA-3
Q127 0.358 0.492 0.465 !       1.27 eA-3
Q128 0.609 0.435 0.447 !       1.27 eA-3
Q129 0.678 0.732 0.374 !       1.26 eA-3
Q130 0.797 0.361 0.346 !       1.25 eA-3
Q131 0.131 0.479 0.282 !       1.25 eA-3
Q132 0.485 0.182 0.217 !       1.24 eA-3
Q133 0.541 0.179 0.129 !       1.24 eA-3
Q134 0.754 0.594 0.197 !       1.24 eA-3
Q135 0.133 0.811 0.281 !       1.23 eA-3
Q136 0.940 0.841 0.097 !       1.21 eA-3
Q137 0.988 0.141 0.434 !       1.21 eA-3
Q138 0.878 0.432 0.480 !       1.20 eA-3
Q139 0.731 0.111 0.077 !       1.20 eA-3
Q140 0.329 0.486 0.391 !       1.20 eA-3
Q141 0.940 0.698 0.273 !       1.19 eA-3
Q142 0.298 0.627 0.272 !       1.18 eA-3
Q143 0.953 0.411 0.363 !       1.17 eA-3
Q144 0.510 0.263 0.280 !       1.16 eA-3
Q145 0.627 0.357 0.213 !       1.13 eA-3
Q146 0.316 0.053 0.080 !       1.11 eA-3
Q147 0.687 0.830 0.372 !       1.11 eA-3
Q148 0.397 0.512 0.217 !       1.10 eA-3
Q149 0.656 0.100 0.402 !       1.05 eA-3
Q150 0.360 0.210 0.488 !       1.05 eA-3
Q151 0.125 0.157 0.378 !       1.04 eA-3
Q152 0.127 0.723 0.199 !       1.04 eA-3
Q153 0.343 0.398 0.468 !       1.04 eA-3
Q154 0.394 0.206 0.429 !       1.03 eA-3
Q155 0.695 0.032 0.049 !       1.03 eA-3
Q156 0.902 0.620 0.487 !       1.03 eA-3
Q157 0.232 0.367 0.176 !       1.01 eA-3
Q158 0.078 0.823 0.187 !       1.00 eA-3
Q159 0.518 0.753 0.045 !       0.99 eA-3
Q160 0.797 0.890 0.370 !       0.99 eA-3
Q161 0.706 0.144 0.357 !       0.98 eA-3
Q162 0.786 0.524 0.176 !       0.98 eA-3
Q163 0.869 0.547 0.408 !       0.97 eA-3
Q164 0.278 0.139 0.232 !       0.97 eA-3
Q165 0.453 0.770 0.110 !       0.96 eA-3
Q166 0.343 0.822 0.266 !       0.96 eA-3
Q167 0.767 0.159 0.343 !       0.96 eA-3
Q168 0.315 0.036 0.458 !       0.95 eA-3
Q169 0.090 0.844 0.248 !       0.95 eA-3
Q170 0.469 0.258 0.466 !       0.95 eA-3
Q171 0.502 0.407 0.062 !       0.94 eA-3
Q172 0.128 0.128 0.150 !       0.92 eA-3
Q173 0.162 0.980 0.142 !       0.92 eA-3
Q174 0.740 0.934 0.110 !       0.92 eA-3
Q175 0.234 0.088 0.081 !       0.90 eA-3
Q176 0.357 0.558 0.374 !       0.89 eA-3
Q177 0.752 0.374 0.014 !       0.89 eA-3
Q178 0.831 0.544 0.107 !       0.89 eA-3
Q179 0.274 0.426 0.236 !       0.89 eA-3
Q180 0.935 0.939 0.092 !       0.89 eA-3
Q181 0.850 0.849 0.156 !       0.89 eA-3
Q182 0.919 0.233 0.187 !       0.89 eA-3
Q183 0.848 0.436 0.013 !       0.89 eA-3
Q184 0.323 0.110 0.501 !       0.89 eA-3
Q185 0.440 0.374 0.027 !       0.89 eA-3
Q186 0.388 0.869 0.276 !       0.88 eA-3
Q187 0.216 0.468 0.273 !       0.86 eA-3
Q188 0.579 0.748 0.461 !       0.86 eA-3
Q189 0.263 0.403 0.331 !       0.85 eA-3
Q190 0.691 0.675 0.292 !       0.85 eA-3
Q191 0.692 0.483-0.007 !       0.85 eA-3
Q192 0.597 0.262 0.137 !       0.84 eA-3
Q193 0.840 0.308 0.134 !       0.84 eA-3
Q194 0.055 0.907 0.294 !       0.83 eA-3
Q195 0.745 0.435 0.019 !       0.83 eA-3
Q196 0.068 0.770 0.104 !       0.81 eA-3
Q197 0.122 0.725 0.140 !       0.77 eA-3
Q198 0.530 0.622 0.099 !       0.76 eA-3
Q199 0.969 0.252 0.064 !       0.76 eA-3
;
_refine_diff_density_max         4.048
_refine_diff_density_min         -1.774
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     927
_refine_ls_number_reflns         12551
_refine_ls_number_restraints     843
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0797
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1671P)^2^+5.7673P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2314
_refine_ls_wR_factor_ref         0.2384
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11043
_reflns_number_total             12551
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04360f2.cif
_cod_data_source_block           complex3-dyzn
_cod_depositor_comments
'Adding full bibliography for 7716128--7716130.cif.'
_cod_database_code               7716129
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F29-C38
 1.5 with sigma of 0.02
3. Rigid bond restraints
 F20, C39
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F29, 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
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C1A \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32
\\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40
\\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48
\\sim C49: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 3.8A
Uanis(F29) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C6(H6), C10(H10), C11(H11), C13(H13), C15(H15),
 C20(H20), C28(H28), C31(H31), C36(H36)
5.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C1A(H1AA,H1AB,H1AC), C42(H42A,H42B,H42C), C44(H44A,H44B,
 H44C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,
 H49B,H49C)
;
_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 3.292
_oxdiff_exptl_absorpt_empirical_full_min 0.336