Influence of ligand substitution and the solvent effect on the structures and magnetic properties of dinuclear Dy<sub>2</sub> supramolecular architectures constructed with the bis-β-diketonate-Dy<sub>2</sub> building block as a metalloligand.
Tang, Jiamin; Zhang, Sheng; Li, Linzhou; Yao, Linbin; Zhang, Ronghu; Yin, Bing; Zhang, Jiangwei; Dalton transactions (Cambridge, England : 2003) 52 (2023) 1366–1377; doi:10.1039/d2dt03468a

data_7712038
_publ_section_title
;
 Influence of ligand substitution and the solvent effect on the structures
 and magnetic properties of dinuclear Dy<sub>2</sub> supramolecular
 architectures constructed with the bis-&#x3b2;-diketonate-Dy<sub>2</sub>
 building block as a metalloligand.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1366
_journal_page_last               1377
_journal_paper_doi               10.1039/d2dt03468a
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         'C78 H38 Dy2 F18 N8 O12'
_chemical_formula_sum            'C78 H38 Dy2 F18 N8 O12'
_chemical_formula_weight         1946.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-11-22
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-12-07 deposited with the CCDC.	2023-01-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.167(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.7990(5)
_cell_length_b                   27.8502(8)
_cell_length_c                   11.8914(4)
_cell_measurement_reflns_used    7114
_cell_measurement_temperature    293.0(2)
_cell_measurement_theta_max      68.7120
_cell_measurement_theta_min      3.8490
_cell_volume                     3819.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1281
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -58.00  15.00   1.00    7.50    --    0.00 -37.00-150.00   73
  2  \w    -77.00 -52.00   1.00    7.50    --    0.00 178.00  60.00   25
  3  \w    -15.00  69.00   1.00    7.50    --    0.00  57.00   0.00   84
  4  \w     13.00  70.00   1.00   30.00    --   54.63 -57.00 -30.00   57
  5  \w     62.00 112.00   1.00   30.00    --   54.63-125.00 150.00   50
  6  \w    -11.00  73.00   1.00   30.00    --   54.63 -57.00 150.00   84
  7  \w     -2.00  76.00   1.00   30.00    --   54.63 -57.00  60.00   78
  8  \w     82.00 123.00   1.00   30.00    --   54.63  77.00 -90.00   41
  9  \w     14.00 125.00   1.00   30.00    --   54.63  19.00  60.00  111
 10  \w    -11.00  73.00   1.00   30.00    --   54.63 -57.00-120.00   84
 11  \w     89.00 176.00   1.00   30.00    --  109.26  63.00-150.00   87
 12  \w    124.00 151.00   1.00   30.00    --  109.26 111.00-150.00   27
 13  \w     39.00 111.00   1.00   30.00    --  109.26-111.00  90.00   72
 14  \w     46.00 130.00   1.00   30.00    --  109.26 -50.00-180.00   84
 15  \w     97.00 137.00   1.00   30.00    --  109.26 -77.00 -90.00   40
 16  \w     41.00 134.00   1.00   30.00    --  109.26 -37.00 -90.00   93
 17  \w     59.00 108.00   1.00   30.00    --  109.26-111.00   0.00   49
 18  \w     51.00 133.00   1.00   30.00    --  109.26 -37.00  60.00   82
 19  \w     67.00 112.00   1.00   30.00    --  109.26-111.00 -90.00   45
 20  \w    101.00 127.00   1.00   30.00    --  109.26 111.00 150.00   26
 21  \w     87.00 112.00   1.00   30.00    --  109.26-111.00-180.00   25
 22  \w    108.00 151.00   1.00   30.00    --  109.26 111.00-120.00   43
 23  \w     43.00 134.00   1.00   30.00    --  109.26 -77.00  90.00   91
 24  \w     55.00  87.00   1.00   30.00    --  109.26 -77.00 -90.00   32
 25  \w     50.00 177.00   1.00   30.00    --  109.26  12.00 -30.00  127
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1114060000
_diffrn_orient_matrix_UB_12      -0.0233791000
_diffrn_orient_matrix_UB_13      -0.0693730000
_diffrn_orient_matrix_UB_21      0.0734728000
_diffrn_orient_matrix_UB_22      -0.0382759000
_diffrn_orient_matrix_UB_23      -0.0450094000
_diffrn_orient_matrix_UB_31      -0.0065368000
_diffrn_orient_matrix_UB_32      -0.0323355000
_diffrn_orient_matrix_UB_33      0.1036090000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_unetI/netI     0.0749
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            25329
_diffrn_reflns_point_group_measured_fraction_full 0.823
_diffrn_reflns_point_group_measured_fraction_max 0.823
_diffrn_reflns_theta_full        67.249
_diffrn_reflns_theta_max         67.249
_diffrn_reflns_theta_min         3.174
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.332
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_description       block
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Flack x determined using 2544 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.010(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.881
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1144
_refine_ls_number_reflns         11240
_refine_ls_number_restraints     384
_refine_ls_restrained_S_all      0.894
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0386
_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^)+(0.0064P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0602
_refine_ls_wR_factor_ref         0.0664
_reflns_Friedel_coverage         0.609
_reflns_Friedel_fraction_full    0.637
_reflns_Friedel_fraction_max     0.637
_reflns_number_gt                8894
_reflns_number_total             11240
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03468a2.cif
_cod_data_source_block           exp_11728
_cod_depositor_comments
'Adding full bibliography for 7712034--7712040.cif.'
_cod_database_code               7712038
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.504
_shelx_estimated_absorpt_t_min   0.464
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C1-F1 = C1-F2 = C1-F3 = C14-F4 = C14-F5 = C14-F6
 1.32 with sigma of 0.01
 C1-F1' = C1-F2' = C1-F3'
 1.32 with sigma of 0.01
 C15-F7 = C15-F8 = C15-F9 = C28-F10 = C28-F11 = C28-F12
 1.32 with sigma of 0.01
 C28-F10' = C28-F11' = C28-F12' = C29-F13' = C29-F14' = C29-F15'
 1.32 with sigma of 0.01
 C29-F13 = C29-F14 = C29-F15 = C42-F16 = C42-F17 = C42-F18
 1.32 with sigma of 0.01
 F1-F2 = F2-F3 = F3-F1 = F4-F5 = F5-F6 = F6-F4
 2.1 with sigma of 0.01
 F1'-F2' = F2'-F3' = F3'-F1'
 2.1 with sigma of 0.01
 F7-F8 = F8-F9 = F9-F7 = F10-F11 = F11-F12 = F12-F10
 2.1 with sigma of 0.01
 F13-F14 = F14-F15 = F15-F13 = F16-F17 = F17-F18 = F18-F16
 2.1 with sigma of 0.01
 F10'-F11' = F11'-F12' = F12'-F10' = F13'-F14' = F14'-F15' = F15'-F13'
 2.1 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
F1 \\sim F2 \\sim F3 \\sim F2' \\sim F3' \\sim F1' \\sim F4 \\sim F5 \\sim F6
\\sim F7 \\sim F8 \\sim F9 \\sim F10 \\sim F11 \\sim F12 \\sim F13 \\sim F14
\\sim F15 \\sim F12' \\sim F10' \\sim F11' \\sim F13' \\sim F14' \\sim F15'
\\sim F16 \\sim F17 \\sim F18: within 3.8A with sigma of 0.02 and sigma for
terminal atoms of 0.04
4. Others
 Sof(F12')=Sof(F10')=Sof(F11')=1-FVAR(1)
 Sof(F10)=Sof(F11)=Sof(F12)=FVAR(1)
 Sof(F13')=Sof(F14')=Sof(F15')=1-FVAR(2)
 Sof(F13)=Sof(F14)=Sof(F15)=FVAR(2)
 Sof(F2')=Sof(F3')=Sof(F1')=1-FVAR(3)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(3)
 Fixed X: Dy2(0.80564)
 Fixed Y: Dy2(0.84202)
 Fixed Z: Dy2(0.510409)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C7(H7), C8(H8), C10(H10), C12(H12), C17(H17), C20(H20),
 C21(H21), C22(H22), C24(H24), C26(H26), C31(H31), C34(H34), C35(H35), C36(H36),
  C38(H38), C40(H40), C43(H43), C44(H44), C45(H45), C49(H49), C50(H50),
 C51(H51), C56(H56), C57(H57), C58(H58), C59(H59), C61(H61), C62(H62), C63(H63),
  C67(H67), C68(H68), C69(H69), C75(H75), C76(H76), C77(H77), C78(H78)
;
_shelx_res_checksum              58337
_shelx_hkl_checksum              81868
_shelx_fab_checksum              38992
_olex2_date_sample_data_collection 2020-12-11
_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 2.059
_oxdiff_exptl_absorpt_empirical_full_min 0.669