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_7716128
_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 F60 Gd2 N10 O26 Zn2'
_chemical_formula_sum            'C100 H72 F60 Gd2 N10 O26 Zn2'
_chemical_formula_weight         3414.91
_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                65.329(2)
_cell_angle_beta                 88.4220(10)
_cell_angle_gamma                75.8390(10)
_cell_formula_units_Z            1
_cell_length_a                   14.3666(2)
_cell_length_b                   15.3987(2)
_cell_length_c                   16.6493(3)
_cell_measurement_reflns_used    21621
_cell_measurement_temperature    113.15
_cell_measurement_theta_max      29.1790
_cell_measurement_theta_min      1.9290
_cell_volume                     3233.71(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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      113.15
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.902
_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   -110.00  70.00   0.50    2.00    --  -20.00   0.00   0.00  360
  2  \w   -110.00  55.00   0.50    2.00    --  -20.00   0.00  90.00  330
  3  \w   -110.00   7.00   0.50    2.00    --  -20.00 -70.00   0.00  234
  4  \w   -110.00   7.00   0.50    2.00    --  -20.00 -70.00 180.00  234
  5  \w   -110.00   7.00   0.50    2.00    --  -20.00 -70.00  90.00  234
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0474226000
_diffrn_orient_matrix_UB_12      -0.0316593000
_diffrn_orient_matrix_UB_13      0.0090500000
_diffrn_orient_matrix_UB_21      0.0135553000
_diffrn_orient_matrix_UB_22      0.0240231000
_diffrn_orient_matrix_UB_23      0.0245577000
_diffrn_orient_matrix_UB_31      -0.0138143000
_diffrn_orient_matrix_UB_32      -0.0338783000
_diffrn_orient_matrix_UB_33      0.0393267000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0879
_diffrn_reflns_av_unetI/netI     0.1095
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.902
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            84732
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.902
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.706
_diffrn_reflns_theta_min         1.813
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.535
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.16520
_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    1.754
_exptl_crystal_description       block
_exptl_crystal_F_000             1678
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.678
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     909
_refine_ls_number_reflns         25122
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.1417
_refine_ls_R_factor_gt           0.0838
_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^)+(0.0959P)^2^+7.3192P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1836
_refine_ls_wR_factor_ref         0.2188
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15261
_reflns_number_total             25122
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04360f2.cif
_cod_data_source_block           complex1-gdzn
_cod_depositor_comments
'Adding full bibliography for 7716128--7716130.cif.'
_cod_database_code               7716128
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.862
_shelx_estimated_absorpt_t_min   0.656
_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. Rigid bond restraints
 F4, C11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
3.a Aromatic/amide H refined with riding coordinates:
 C22(H22), C19(H19), C18(H18), C17(H17), C13(H13), C26(H26), C24(H24),
 C20(H20), C43(H43), C48(H48), C3(H3), C8(H8)
3.b Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C40(H40A,H40B,
 H40C), C29(H29A,H29B,H29C), C33(H33A,H33B,H33C), C32(H32A,H32B,H32C), C30(H30A,
 H30B,H30C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 3.270
_oxdiff_exptl_absorpt_empirical_full_min 0.547