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_7712034
_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         'C56 H24 Dy2 F24 O16, 2(C6 H15 N)'
_chemical_formula_sum            'C68 H54 Dy2 F24 N2 O16'
_chemical_formula_weight         1936.13
_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
_audit_creation_date             2022-11-22
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-12-07 deposited with the CCDC.	2023-01-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.772(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.4037(11)
_cell_length_b                   20.0870(8)
_cell_length_c                   21.2918(11)
_cell_measurement_reflns_used    2922
_cell_measurement_temperature    293.0(1)
_cell_measurement_theta_max      61.1860
_cell_measurement_theta_min      3.3260
_cell_volume                     7535.1(7)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/1 (Sheldrick, 2015)'
_diffrn_ambient_temperature      293.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1281
_diffrn_detector_type            Eos
_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     14.00  50.00   1.00    2.00    --    0.00  57.00 -90.00   36
  2  \w      1.00  42.00   1.00    2.00    --    0.00 -99.00  60.00   41
  3  \w    -77.00 -32.00   1.00    2.00    --    0.00 178.00 120.00   45
  4  \w    -76.00 -50.00   1.00    2.00    --    0.00 178.00 -90.00   26
  5  \w     42.00  88.00   1.00    6.00    --   54.63-125.00  90.00   46
  6  \w    -18.00  52.00   1.00    6.00    --   54.63 -37.00 150.00   70
  7  \w     34.00 123.00   1.00    6.00    --   54.63  37.00  60.00   89
  8  \w      2.00  68.00   1.00    6.00    --   54.63 -57.00  60.00   66
  9  \w     57.00 129.00   1.00    6.00    --  109.26 -50.00 120.00   72
 10  \w     63.00 126.00   1.00    6.00    --  109.26 178.00  30.00   63
 11  \w     91.00 176.00   1.00    6.00    --  109.26  50.00 -90.00   85
 12  \w     46.00 113.00   1.00    6.00    --  109.26-111.00   0.00   67
 13  \w     41.00 147.00   1.00    6.00    --  109.26 -91.00  30.00  106
 14  \w     51.00  76.00   1.00    6.00    --  109.26-111.00 150.00   25
 15  \w     55.00 106.00   1.00    6.00    --  109.26-111.00 -90.00   51
 16  \w    129.00 172.00   1.00    6.00    --  109.26  50.00 -30.00   43
;
_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      -0.0093249000
_diffrn_orient_matrix_UB_12      -0.0476362000
_diffrn_orient_matrix_UB_13      0.0526095000
_diffrn_orient_matrix_UB_21      -0.0869529000
_diffrn_orient_matrix_UB_22      0.0050769000
_diffrn_orient_matrix_UB_23      -0.0392280000
_diffrn_orient_matrix_UB_31      0.0000613000
_diffrn_orient_matrix_UB_32      -0.0598763000
_diffrn_orient_matrix_UB_33      -0.0451907000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0845
_diffrn_reflns_av_unetI/netI     0.1234
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            28168
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.245
_diffrn_reflns_theta_max         67.245
_diffrn_reflns_theta_min         3.173
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.610
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69197
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_description       block
_exptl_crystal_F_000             3808
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.186
_refine_diff_density_min         -0.988
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1015
_refine_ls_number_reflns         13494
_refine_ls_number_restraints     3181
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.1507
_refine_ls_R_factor_gt           0.0770
_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^)+(0.0878P)^2^+5.0809P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1766
_refine_ls_wR_factor_ref         0.2294
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7071
_reflns_number_total             13494
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03468a2.cif
_cod_data_source_block           exp_11493
_cod_depositor_comments
'Adding full bibliography for 7712034--7712040.cif.'
_cod_database_code               7712034
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.457
_shelx_estimated_absorpt_t_min   0.421
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1-F1 = C1-F2 = C1-F3
 1.32 with sigma of 0.01
 F1-F2 = F2-F3 = F3-F1
 2.1 with sigma of 0.01
 C1-C2
 1.52 with sigma of 0.01
3. 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 within 3.8A
4.a Secondary CH2 refined with riding coordinates:
 C57(H57A,H57B), C59(H59A,H59B), C61(H61A,H61B), C63(H63A,H63B), C65(H65A,
 H65B), C67(H67A,H67B)
4.b 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), C45(H45), C48(H48), C49(H49), C50(H50), C52(H52), C54(H54)
4.c Idealised Me refined as rotating group:
 C58(H58A,H58B,H58C), C60(H60A,H60B,H60C), C62(H62A,H62B,H62C), C64(H64A,H64B,
 H64C), C66(H66A,H66B,H66C), C68(H68A,H68B,H68C)
;
_shelx_res_checksum              53200
_shelx_hkl_checksum              68973
_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 1.394
_oxdiff_exptl_absorpt_empirical_full_min 0.839