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_7712040
_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         'C90 H50 Dy2 F18 N4 O12'
_chemical_formula_sum            'C90 H50 Dy2 F18 N4 O12'
_chemical_formula_weight         2046.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                 93.385(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0834(6)
_cell_length_b                   21.4549(11)
_cell_length_c                   45.363(2)
_cell_measurement_reflns_used    3781
_cell_measurement_temperature    293.0(2)
_cell_measurement_theta_max      69.6340
_cell_measurement_theta_min      3.8780
_cell_volume                     9796.6(9)
_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    'SIR2004 (Burla et al.,  2007)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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      0.00  27.00   1.00   20.50    --    0.00   0.00  60.00   27
  2  \w    -72.00 -30.00   1.00   20.50    --    0.00   0.00  60.00   42
  3  \w     33.00  61.00   1.00   20.50    --    0.00   0.00  60.00   28
  4  \w    -77.00 -52.00   1.00   20.50    --    0.00 178.00 -90.00   25
  5  \w     40.00  74.00   1.00   82.50    --   54.63-125.00 150.00   34
  6  \w     29.00 118.00   1.00   82.50    --   54.63  77.00 -60.00   89
  7  \w    -14.00  82.00   1.00   82.50    --   54.63 -77.00-180.00   96
  8  \w     53.00 100.00   1.00   82.50    --   54.63  57.00  60.00   47
  9  \w     56.00 130.00   1.00   82.50    --  109.26 -50.00 -60.00   74
 10  \w    108.00 134.00   1.00   82.50    --  109.26 -37.00-150.00   26
 11  \w     87.00 158.00   1.00   82.50    --  109.26  77.00   0.00   71
 12  \w    113.00 139.00   1.00   82.50    --  109.26 111.00-150.00   26
 13  \w     41.00  91.00   1.00   82.50    --  109.26 -37.00-150.00   50
 14  \w     83.00 111.00   1.00   82.50    --  109.26-111.00-120.00   28
 15  \w    107.00 178.00   1.00   82.50    --  109.26  89.00 -40.00   71
 16  \w     67.00 128.00   1.00   82.50    --  109.26 178.00 -30.00   61
 17  \w     81.00 127.00   1.00   82.50    --  109.26 -63.00-150.00   46
 18  \w     94.00 169.00   1.00   82.50    --  109.26  50.00  60.00   75
;
_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      -0.1374224000
_diffrn_orient_matrix_UB_12      -0.0085649000
_diffrn_orient_matrix_UB_13      -0.0161968000
_diffrn_orient_matrix_UB_21      0.0423133000
_diffrn_orient_matrix_UB_22      -0.0647737000
_diffrn_orient_matrix_UB_23      -0.0107021000
_diffrn_orient_matrix_UB_31      -0.0524076000
_diffrn_orient_matrix_UB_32      -0.0298315000
_diffrn_orient_matrix_UB_33      0.0279278000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0849
_diffrn_reflns_av_unetI/netI     0.1211
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            36581
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.248
_diffrn_reflns_theta_max         67.247
_diffrn_reflns_theta_min         3.905
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.853
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48275
_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            gray
_exptl_crystal_colour_primary    gray
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_description       block
_exptl_crystal_F_000             4032
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.757
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1242
_refine_ls_number_reflns         17502
_refine_ls_number_restraints     4473
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.1359
_refine_ls_R_factor_gt           0.0657
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0649P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1419
_refine_ls_wR_factor_ref         0.1805
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9019
_reflns_number_total             17502
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03468a2.cif
_cod_data_source_block           exp_11654
_cod_depositor_comments
'Adding full bibliography for 7712034--7712040.cif.'
_cod_original_cell_volume        9796.7(9)
_cod_database_code               7712040
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.576
_shelx_estimated_absorpt_t_min   0.538
_reflns_odcompleteness_completeness 99.71
_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
 C85-C87 = C87-C89 = C89-C85 = C86-C88 = C88-C90 = C90-C86
 2.37 with sigma of 0.01
 C85-C86 = C86-C87 = C87-C88 = C88-C89 = C85-C90 = C89-C90
 1.38 with sigma of 0.01
 F13-F14 = F14-F15 = F15-F13 = F16-F17 = F17-F18 = F18-F16
 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
 F1-F2 = F2-F3 = F3-F1 = F4-F5 = F5-F6 = F6-F4
 2.1 with sigma of 0.01
 C29-F13 = C29-F14 = C29-F15 = C42-F16 = C42-F17 = C42-F18
 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
 C1-F1 = C1-F2 = C1-F3 = C14-F4 = C14-F5 = C14-F6
 1.32 with sigma of 0.01
 C1-C2 = C13-C14 = C15-C16 = C27-C28 = C29-C30 = C41-C42
 1.54 with sigma of 0.01
 C28-F11' = C28-F12' = C1-F1' = C1-F2' = C1-F3' = C28-F10'
 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' = 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
3. Restrained planarity
 C85, C86, C87, C88, C89, C90
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 3.8A with sigma of 0.02 and sigma
for terminal atoms of 0.04
5. Others
 Sof(F10')=Sof(F11')=Sof(F12')=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(F16')=Sof(F17')=Sof(F18')=1-FVAR(3)
 Sof(F16)=Sof(F17)=Sof(F18)=FVAR(3)
 Sof(F2')=Sof(F1')=Sof(F3')=1-FVAR(4)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(4)
6.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), C46(H46), C47(H47),
 C50(H50), C51(H51), C54(H54), C55(H55), C58(H58), C59(H59), C62(H62), C63(H63),
  C64(H64), C65(H65), C66(H66), C67(H67), C68(H68), C69(H69), C70(H70),
 C71(H71), C74(H74), C75(H75), C78(H78), C79(H79), C82(H82), C83(H83), C86(H86),
  C87(H87), C88(H88), C89(H89), C90(H90)
;
_shelx_res_checksum              12172
_shelx_hkl_checksum              84813
_shelx_fab_checksum              42402
_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 1.638
_oxdiff_exptl_absorpt_empirical_full_min 0.689