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_7712037
_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         'C66 H42 Dy2 F18 N4 O12'
_chemical_formula_sum            'C66 H42 Dy2 F18 N4 O12'
_chemical_formula_weight         1750.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/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                 118.708(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.5484(6)
_cell_length_b                   21.4427(6)
_cell_length_c                   18.8657(7)
_cell_measurement_reflns_used    7918
_cell_measurement_temperature    293.0(2)
_cell_measurement_theta_max      70.6350
_cell_measurement_theta_min      3.3080
_cell_volume                     6935.9(5)
_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(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1281
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.940
_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      1.00  36.00   1.00    2.03    --    0.00 -99.00  60.00   35
  2  \w    -70.00  -8.00   1.00    2.03    --    0.00 -77.00-180.00   62
  3  \w    -59.00 -34.00   1.00    2.03    --    0.00 178.00 -60.00   25
  4  \w     34.00 107.00   1.00   42.50    --   54.63-128.00 158.00   73
  5  \w     15.00  59.00   1.00   42.50    --   54.63 -57.00-180.00   44
  6  \w     91.00 118.00   1.00   42.50    --   54.63  57.00-150.00   27
  7  \w     41.00 112.00   1.00   42.50    --   54.63  57.00-180.00   71
  8  \w     48.00 120.00   1.00   42.50    --   54.63  57.00  90.00   72
  9  \w     39.00 105.00   1.00   42.50    --  109.26-111.00 -90.00   66
 10  \w    100.00 161.00   1.00   42.50    --  109.26  63.00 150.00   61
 11  \w     50.00 123.00   1.00   42.50    --  109.26 -63.00-120.00   73
 12  \w    133.00 174.00   1.00   42.50    --  109.26 111.00 150.00   41
 13  \w     37.00 133.00   1.00   42.50    --  109.26 -37.00-150.00   96
 14  \w     60.00  85.00   1.00   42.50    --  109.26-111.00   0.00   25
 15  \w     49.00 177.00   1.00   42.50    --  109.26   0.00 -60.00  128
;
_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      0.0864956000
_diffrn_orient_matrix_UB_12      0.0195856000
_diffrn_orient_matrix_UB_13      0.0418704000
_diffrn_orient_matrix_UB_21      0.0239175000
_diffrn_orient_matrix_UB_22      -0.0667342000
_diffrn_orient_matrix_UB_23      0.0332042000
_diffrn_orient_matrix_UB_31      0.0051217000
_diffrn_orient_matrix_UB_32      -0.0182984000
_diffrn_orient_matrix_UB_33      -0.0761581000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_Laue_measured_fraction_full 0.940
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24322
_diffrn_reflns_point_group_measured_fraction_full 0.940
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        64.998
_diffrn_reflns_theta_max         64.998
_diffrn_reflns_theta_min         3.300
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.380
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.11073
_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    1.676
_exptl_crystal_description       block
_exptl_crystal_F_000             3424
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.105
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     923
_refine_ls_number_reflns         11085
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0532
_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^)+(0.0899P)^2^+2.7876P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1374
_refine_ls_wR_factor_ref         0.1544
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8228
_reflns_number_total             11085
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03468a2.cif
_cod_data_source_block           exp_11817
_cod_depositor_comments
'Adding full bibliography for 7712034--7712040.cif.'
_cod_original_cell_volume        6935.9(4)
_cod_database_code               7712037
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.438
_shelx_estimated_absorpt_t_min   0.402
_reflns_odcompleteness_completeness 93.54
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Uiso/Uaniso restraints and constraints
F1 \\sim F2 \\sim F3 \\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 F16 \\sim F17
\\sim F18: within 3.8A with sigma of 0.02 and sigma for terminal atoms of 0.04
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C8(H8), C9(H9), 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), C45(H45), C46(H46), C49(H49), C50(H50),
 C52(H52), C55(H55), C57(H57), C58(H58), C61(H61), C62(H62), C64(H64)
3.b Idealised Me refined as rotating group:
 C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C65(H65A,H65B,H65C), C66(H66A,H66B,
 H66C)
;
_shelx_res_checksum              77297
_shelx_hkl_checksum              70960
_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 5.574
_oxdiff_exptl_absorpt_empirical_full_min 0.465