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_1565215
_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         'C76 H54 Dy2 F12 N4 O10'
_chemical_formula_sum            'C76 H54 Dy2 F12 N4 O10'
_chemical_formula_weight         1736.23
_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                101.120(3)
_cell_angle_beta                 112.968(3)
_cell_angle_gamma                100.847(3)
_cell_formula_units_Z            1
_cell_length_a                   10.9464(7)
_cell_length_b                   12.8805(8)
_cell_length_c                   13.9048(9)
_cell_measurement_reflns_used    4615
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.468
_cell_measurement_theta_min      2.286
_cell_volume                     1694.2(2)
_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      150.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1104
_diffrn_reflns_av_unetI/netI     0.0846
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            27153
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         2.112
_exptl_absorpt_coefficient_mu    2.286
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6542
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0741 before and 0.0655 after correction.
The Ratio of minimum to maximum transmission is 0.8779.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_description       block
_exptl_crystal_F_000             858
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.768
_refine_diff_density_min         -0.992
_refine_diff_density_rms         0.189
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         5970
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0630P)^2^+0.2346P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1018
_refine_ls_wR_factor_ref         0.1199
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4585
_reflns_number_total             5970
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1.cif
_cod_data_source_block           1
_cod_original_cell_volume        1694.22(19)
_cod_database_code               1565215
_shelx_estimated_absorpt_t_max   0.787
_shelx_estimated_absorpt_t_min   0.493
_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. Rigid bond restraints
 F4, C38, F5, F6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C38, F5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
3. Uiso/Uaniso restraints and constraints
F5 \\sim F4 \\sim F6: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(F5) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F4) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(F5) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(F5') = Uanis(F5) = Uanis(F4') = Uanis(F4) = Uanis(F6') = Uanis(F6)
4. Others
 Sof(F4')=Sof(F5')=Sof(F6')=1-FVAR(1)
 Sof(F6)=Sof(F5)=Sof(F4)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B)
5.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C28(H28), C8(H8), C29(H29), C2(H2), C36(H36), C30(H30), C24(H24),
 C3(H3), C13(H13), C27(H27), C15(H15), C32(H32), C10(H10), C4(H4), C21(H21),
 C33(H33), C16(H16), C26(H26), C31(H31), C25(H25), C12(H12)
5.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C)
;
_shelx_res_checksum              90460
_shelx_hkl_checksum              52186
_olex2_submission_special_instructions 'No special instructions were received'