Two phenoxo-O bridged dinuclear Dy(III) complexes exhibiting distinct slow magnetic relaxation induced by different β-diketonate ligands
Chang, Yi-Xin; Gao, Ning; Wang, Mei-Ying; Wang, Wan-Ting; Fan, Zi-Wei; Ren, Duo-Duo; Wu, Zhi-Lei; Wang, Wen-Min; Inorganica Chimica Acta 505 (2020) 119499–; doi:10.1016/j.ica.2020.119499

data_1565216
_publ_section_title
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 Two phenoxo-O bridged dinuclear Dy(III) complexes exhibiting distinct
 slow magnetic relaxation induced by different \b-diketonate ligands
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119499
_journal_paper_doi               10.1016/j.ica.2020.119499
_journal_volume                  505
_journal_year                    2020
_chemical_formula_moiety         'C68 H46 Dy2 F12 N4 O10 S4'
_chemical_formula_sum            'C68 H46 Dy2 F12 N4 O10 S4'
_chemical_formula_weight         1760.33
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_cell_angle_alpha                69.802(5)
_cell_angle_beta                 69.742(6)
_cell_angle_gamma                78.280(5)
_cell_formula_units_Z            1
_cell_length_a                   10.8475(12)
_cell_length_b                   13.0262(13)
_cell_length_c                   13.4316(17)
_cell_measurement_reflns_used    2678
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.369
_cell_measurement_theta_min      2.205
_cell_volume                     1663.5(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1141
_diffrn_reflns_av_unetI/netI     0.1046
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21502
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.004
_diffrn_reflns_theta_max         25.004
_diffrn_reflns_theta_min         2.206
_exptl_absorpt_coefficient_mu    2.450
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0800 before and 0.0670 after correction.
The Ratio of minimum to maximum transmission is 0.7574.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.757
_exptl_crystal_description       block
_exptl_crystal_F_000             866
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.090
_refine_diff_density_min         -1.210
_refine_diff_density_rms         0.210
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         5849
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1406
_refine_ls_R_factor_gt           0.0859
_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^)+(0.1300P)^2^+25.5360P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2062
_refine_ls_wR_factor_ref         0.2532
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4163
_reflns_number_total             5849
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            2.cif
_cod_data_source_block           2
_cod_database_code               1565216
_shelx_estimated_absorpt_t_max   0.758
_shelx_estimated_absorpt_t_min   0.603
_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. Uiso/Uaniso restraints and constraints
Uanis(C30) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C22) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C26) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C29B) = Uanis(C27B) = Uanis(S1A) = Uanis(C27A) = Uanis(S1B) = Uanis(C28B)
= Uanis(C29A) = Uanis(C28A)
Uanis(S2A) = Uanis(C21B) = Uanis(C19B) = Uanis(C19A) = Uanis(C20B) =
Uanis(C20A) = Uanis(S2B) = Uanis(C21A)
Uanis(F5A) = Uanis(F4B) = Uanis(F4A) = Uanis(F6B) = Uanis(F6A) = Uanis(F5B)
3. Others
 Sof(S1B)=Sof(C29B)=Sof(H29B)=Sof(C28B)=Sof(H28B)=Sof(C27B)=Sof(H27B)=1-FVAR(1)
 Sof(C29A)=Sof(H29A)=Sof(C28A)=Sof(H28A)=Sof(C27A)=Sof(H27A)=Sof(S1A)=FVAR(1)
 Sof(S2B)=Sof(C20B)=Sof(H20B)=Sof(C19B)=Sof(H19B)=Sof(C21B)=Sof(H21B)=1-FVAR(2)
 Sof(S2A)=Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(H20A)=Sof(C21A)=Sof(H21A)=FVAR(2)
 Sof(F5A)=Sof(F6A)=Sof(F4A)=1-FVAR(3)
 Sof(F4B)=Sof(F6B)=Sof(F5B)=FVAR(3)
4.a :
 C22(S2B,C20B,C19B,C21B), C29A(C28A,C27A,S1A,C30)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
4.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C17(H17), C9(H9), C4(H4), C8(H8), C7(H7), C24(H24),
 C16(H16), C5(H5), C32(H32), C18(H18), C20B(H20B), C19B(H19B), C21B(H21B),
 C29B(H29B), C28B(H28B), C27B(H27B), C29A(H29A), C28A(H28A), C27A(H27A),
 C19A(H19A), C20A(H20A), C21A(H21A)
4.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_shelx_res_checksum              93807
_shelx_hkl_checksum              11396
_olex2_submission_special_instructions 'No special instructions were received'