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_7712036
_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 H34 Dy2 F18 N4 O12'
_chemical_formula_sum            'C66 H34 Dy2 F18 N4 O12'
_chemical_formula_weight         1741.97
_space_group_crystal_system      orthorhombic
_space_group_IT_number           45
_space_group_name_Hall           'I 2 -2c'
_space_group_name_H-M_alt        'I b a 2'
_atom_sites_solution_hydrogens   geom
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.5572(5)
_cell_length_b                   18.9503(6)
_cell_length_c                   21.1019(7)
_cell_measurement_reflns_used    1854
_cell_measurement_temperature    293.0(2)
_cell_measurement_theta_max      26.482
_cell_measurement_theta_min      2.156
_cell_volume                     7020.9(4)
_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_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            12424
_diffrn_reflns_point_group_measured_fraction_full 0.752
_diffrn_reflns_point_group_measured_fraction_max 0.752
_diffrn_reflns_theta_full        67.177
_diffrn_reflns_theta_max         67.177
_diffrn_reflns_theta_min         3.432
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.230
_exptl_absorpt_correction_T_max  0.84230
_exptl_absorpt_correction_T_min  0.68197
_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            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_description       block
_exptl_crystal_F_000             3392
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_platon_squeeze_details
;

;
_refine_diff_density_max         0.644
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.014(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         4712
_refine_ls_number_restraints     174
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0926P)^2^+3.8417P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1383
_reflns_Friedel_coverage         0.459
_reflns_Friedel_fraction_full    0.489
_reflns_Friedel_fraction_max     0.489
_reflns_number_gt                3927
_reflns_number_total             4712
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03468a2.cif
_cod_data_source_block           11490
_cod_depositor_comments
'Adding full bibliography for 7712034--7712040.cif.'
_cod_database_code               7712036
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.346
_shelx_estimated_absorpt_t_min   0.322
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.986(8)
 0.014(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 C15-F7 = C15-F8 = C15-F9
 1.32 with sigma of 0.01
 F7-F8 = F8-F9 = F9-F7
 2.28 with sigma of 0.01
 C14-F4 = C14-F5 = C14-F6
 1.32 with sigma of 0.01
 F4-F5 = F5-F6 = F6-F4
 2.28 with sigma of 0.01
 C1-F1 = C1-F2 = C1-F3
 1.32 with sigma of 0.01
 F1-F2 = F2-F3 = F3-F1
 2.28 with sigma of 0.01
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Fixed X: Dy1(0.075089)
 Fixed Y: Dy1(0.20322)
 Fixed Z: Dy1(-0.003851)
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), C23(H23), C24(H24), C25(H25), C27(H27), C28(H28), C30(H30),
  C31(H31), C32(H32)
;
_shelx_res_checksum              79932
_shelx_hkl_checksum              33844
_shelx_fab_checksum              43802
_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
;