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_7712039
_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           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                 116.872(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   36.8903(11)
_cell_length_b                   13.0524(2)
_cell_length_c                   17.0048(4)
_cell_measurement_reflns_used    2416
_cell_measurement_temperature    293.0(2)
_cell_measurement_theta_max      28.146
_cell_measurement_theta_min      2.156
_cell_volume                     7303.8(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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0295
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25083
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.232
_diffrn_reflns_theta_max         67.232
_diffrn_reflns_theta_min         4.270
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.756
_exptl_absorpt_correction_T_max  0.84230
_exptl_absorpt_correction_T_min  0.5426
_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    1.592
_exptl_crystal_description       block
_exptl_crystal_F_000             3424
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.755
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         6558
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0312
_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^)+(0.0494P)^2^+12.4872P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0812
_refine_ls_wR_factor_ref         0.0830
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6049
_reflns_number_total             6558
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03468a2.cif
_cod_data_source_block           11792
_cod_depositor_comments
'Adding full bibliography for 7712034--7712040.cif.'
_cod_original_cell_volume        7303.8(3)
_cod_database_code               7712039
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.493
_shelx_estimated_absorpt_t_min   0.453
_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. Restrained distances
 F7-C15 \\sim F7A-C15
 with sigma of 0.02
 F8-C15 \\sim F8A-C15
 with sigma of 0.02
 F9-C15 \\sim F9A-C15
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F1 \\sim F2 \\sim F3 \\sim F4 \\sim F5 \\sim F6 \\sim F7 \\sim F8 \\sim F9
\\sim F7A \\sim F9A \\sim F8A: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(F7) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F8) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(F7) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(C15) \\sim
Ueq, Uanis(F7A) \\sim Ueq, Uanis(F9A) \\sim Ueq, Uanis(F8A) \\sim Ueq: with
sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(F7A)=Sof(F9A)=Sof(F8A)=1-FVAR(1)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(1)
5.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), C26(H26), C29(H29), C31(H31), C32(H32)
5.b Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C)
;
_shelx_res_checksum              64627
_shelx_hkl_checksum              52104
_shelx_fab_checksum              79232
_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
;