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_7712035
_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           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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                 117.146(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.5237(5)
_cell_length_b                   20.9359(4)
_cell_length_c                   21.2684(10)
_cell_measurement_reflns_used    10274
_cell_measurement_temperature    293.0(2)
_cell_measurement_theta_max      71.1300
_cell_measurement_theta_min      3.2840
_cell_volume                     7735.8(6)
_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 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    -29.00  70.00   1.00    4.00    --    0.00  77.00-180.00   99
  2  \w      5.00  42.00   1.00    4.00    --    0.00 -99.00  30.00   37
  3  \w    -67.00 -36.00   1.00    4.00    --    0.00 178.00 -30.00   31
  4  \w     31.00  66.00   1.00    4.00    --    0.00  57.00 -90.00   35
  5  \w    -20.00   8.00   1.00    4.00    --    0.00  57.00 -90.00   28
  6  \w     -3.00  75.00   1.00   14.00    --   54.63 -57.00-180.00   78
  7  \w    -16.00  99.00   1.00   14.00    --   54.63 -19.00 -30.00  115
  8  \w    -16.00  58.00   1.00   14.00    --   54.63 -77.00 -60.00   74
  9  \w    -13.00  20.00   1.00   14.00    --   54.63 -57.00 -60.00   33
 10  \w     16.00  80.00   1.00   14.00    --   54.63 -37.00  60.00   64
 11  \w     37.00 109.00   1.00   14.00    --   54.63-125.00 120.00   72
 12  \w     90.00 123.00   1.00   14.00    --   54.63  57.00 150.00   33
 13  \w     32.00  71.00   1.00   14.00    --   54.63 -57.00 -60.00   39
 14  \w     41.00 130.00   1.00   14.00    --  109.26 -50.00 150.00   89
 15  \w     87.00 178.00   1.00   14.00    --  109.26  50.00-180.00   91
 16  \w     38.00 109.00   1.00   14.00    --  109.26-111.00  60.00   71
 17  \w     38.00  66.00   1.00   14.00    --  109.26 -91.00  60.00   28
 18  \w     37.00 129.00   1.00   14.00    --  109.26 -37.00-120.00   92
 19  \w     88.00 113.00   1.00   14.00    --  109.26-111.00 -30.00   25
 20  \w     57.00 113.00   1.00   14.00    --  109.26-111.00-120.00   56
 21  \w     53.00 138.00   1.00   14.00    --  109.26 -77.00-120.00   85
 22  \w     48.00 171.00   1.00   14.00    --  109.26  12.00 150.00  123
 23  \w     39.00 127.00   1.00   14.00    --  109.26 -50.00  30.00   88
 24  \w     68.00 141.00   1.00   14.00    --  109.26 -91.00  60.00   73
 25  \w    153.00 178.00   1.00   14.00    --  109.26  12.00 -60.00   25
 26  \w     43.00 128.00   1.00   14.00    --  109.26  12.00 -60.00   85
;
_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      0.0820004000
_diffrn_orient_matrix_UB_12      0.0081865000
_diffrn_orient_matrix_UB_13      0.0078874000
_diffrn_orient_matrix_UB_21      0.0319996000
_diffrn_orient_matrix_UB_22      0.0035470000
_diffrn_orient_matrix_UB_23      0.0808710000
_diffrn_orient_matrix_UB_31      0.0107366000
_diffrn_orient_matrix_UB_32      -0.0729841000
_diffrn_orient_matrix_UB_33      0.0047360000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            25535
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.238
_diffrn_reflns_theta_max         67.238
_diffrn_reflns_theta_min         3.306
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.191
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22709
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_description       block
_exptl_crystal_F_000             3808
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.355
_refine_diff_density_min         -2.228
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         6936
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0464
_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^)+(0.0855P)^2^+11.1086P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1240
_refine_ls_wR_factor_ref         0.1325
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5803
_reflns_number_total             6936
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03468a2.cif
_cod_data_source_block           exp_11720
_cod_depositor_comments
'Adding full bibliography for 7712034--7712040.cif.'
_cod_original_cell_volume        7735.7(5)
_cod_database_code               7712035
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.553
_shelx_estimated_absorpt_t_min   0.468
_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. Uiso/Uaniso restraints and constraints
F7 \\sim F8 \\sim F9 \\sim F7' \\sim F8' \\sim F9' \\sim C33: within 3.8A with
sigma of 0.02 and sigma for terminal atoms of 0.04
3. Others
 Sof(F7')=Sof(F9')=Sof(F8')=1-FVAR(1)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C8(H8), C9(H9), C10(H10), C14(H14), C15(H15),
 C16(H16), C17(H17), C21(H21), C24(H24), C25(H25), C26(H26), C28(H28), C30(H30),
  C35(H35), C38(H38), C39(H39), C40(H40)
;
_shelx_res_checksum              57223
_shelx_hkl_checksum              84156
_shelx_fab_checksum              35921
_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 2.901
_oxdiff_exptl_absorpt_empirical_full_min 0.583