Modulating magnetic dynamics through tailoring the terminal ligands in Dy<sub>2</sub> single-molecule magnets.
Cen, Peipei; Liu, Xiangyu; Zhang, Yi-Quan; Ferrando-Soria, Jesús; Xie, Gang; Chen, Sanping; Pardo, Emilio; Dalton transactions (Cambridge, England : 2003) 49 (2020) 808–816; doi:10.1039/c9dt03993g

data_7702954
_publ_section_title
;
 Modulating magnetic dynamics through tailoring the terminal ligands in
 Dy<sub>2</sub> single-molecule magnets.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              808
_journal_page_last               816
_journal_paper_doi               10.1039/c9dt03993g
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C56 H34 Dy2 F12 N8 O10 S4'
_chemical_formula_sum            'C56 H34 Dy2 F12 N8 O10 S4'
_chemical_formula_weight         1660.19
_space_group_crystal_system      trigonal
_space_group_IT_number           144
_space_group_name_Hall           'P 31'
_space_group_name_H-M_alt        'P 31'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-07-24
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-10-26 deposited with the CCDC.	2019-12-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   13.6044(4)
_cell_length_b                   13.6044(4)
_cell_length_c                   28.6443(8)
_cell_measurement_reflns_used    3385
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.5970
_cell_measurement_theta_min      4.0270
_cell_volume                     4591.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6525
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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    -82.00  21.00   1.00    1.00    --  -41.14  19.00  60.00  103
  2  \w     33.00 121.00   1.00    1.24    --  106.40-125.00 150.00   88
  3  \w     33.00  84.00   1.00    1.24    --  106.40 -45.00-120.00   51
  4  \w    106.00 132.00   1.00    1.24    --  106.40 -45.00-120.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1283225000
_diffrn_orient_matrix_UB_12      -0.0716441000
_diffrn_orient_matrix_UB_13      -0.0096208000
_diffrn_orient_matrix_UB_21      -0.0202952000
_diffrn_orient_matrix_UB_22      0.0830413000
_diffrn_orient_matrix_UB_23      0.0293699000
_diffrn_orient_matrix_UB_31      0.0146001000
_diffrn_orient_matrix_UB_32      0.0712268000
_diffrn_orient_matrix_UB_33      -0.0440188000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0611
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            9825
_diffrn_reflns_point_group_measured_fraction_full 0.564
_diffrn_reflns_point_group_measured_fraction_max 0.564
_diffrn_reflns_theta_full        65.929
_diffrn_reflns_theta_max         65.929
_diffrn_reflns_theta_min         3.752
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.077
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58308
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.801
_exptl_crystal_description       block
_exptl_crystal_F_000             2430
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.742
_refine_diff_density_min         -0.719
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.001(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     844
_refine_ls_number_reflns         6012
_refine_ls_number_restraints     119
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0417
_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^)+(0.0595P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1058
_reflns_Friedel_coverage         0.133
_reflns_Friedel_fraction_full    0.133
_reflns_Friedel_fraction_max     0.133
_reflns_number_gt                5658
_reflns_number_total             6012
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03993g2.cif
_cod_data_source_block           ww
_cod_depositor_comments
'Adding full bibliography for 7702953--7702954.cif.'
_cod_original_cell_volume        4591.2(3)
_cod_database_code               7702954
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.184
_shelx_estimated_absorpt_t_min   0.162
_reflns_odcompleteness_completeness 88.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 S1-C1 = S1-C4 = S1A-C2 = S1A-C4
 1.68 with sigma of 0.01
 C1-C2 = C2-C3 = C3-C4 = C3A-C4 = C3A-C1
 1.4 with sigma of 0.01
 C1-C3 = C2-C4 = C2-C3A
 2.25 with sigma of 0.02
 C25-S4 = C28-S4 = C26-S4A
 1.68 with sigma of 0.02
 C25-C26 = C26-C27 = C27-C28 = C25-C27A = C27A-C28
 1.4 with sigma of 0.02
 C25-C27 = C26-C28 = C26-C27A
 2.25 with sigma of 0.02
 S2-C9 = S2-C12 = S2A-C10
 1.68 with sigma of 0.01
 C9-C10 = C10-C11 = C11-C12 = C9-C11A = C11A-C12
 1.4 with sigma of 0.01
 C9-C11 = C10-C12 = C11A-C10
 2.25 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(S1A) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(S1) \\sim
Ueq, Uanis(C3) \\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(C11A) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C27A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C3) \\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26)
\\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C9) \\sim Ueq,
Uanis(C10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C27A) = Uanis(C27)
Uanis(C11A) = Uanis(C11)
Uanis(S2A) = Uanis(C11) = Uanis(C11A) = Uanis(S2)
Uanis(S2A) = Uanis(S2)
Uanis(S1) = Uanis(C3A) = Uanis(C3) = Uanis(S1A)
4. Others
 Sof(C3A)=Sof(H3A)=Sof(S1A)=Sof(H2B)=Sof(H1B)=1-FVAR(1)
 Sof(S1)=Sof(C3)=Sof(H3)=Sof(H2A)=Sof(H1A)=FVAR(1)
 Sof(S4A)=Sof(C27A)=Sof(H27A)=Sof(H25A)=Sof(H26A)=1-FVAR(2)
 Sof(S4)=Sof(C27)=Sof(H27)=Sof(H25)=Sof(H26)=FVAR(2)
 Sof(S2A)=Sof(C11A)=Sof(H11A)=Sof(H10A)=Sof(H9B)=1-FVAR(3)
 Sof(S2)=Sof(C11)=Sof(H11)=Sof(H10)=Sof(H9A)=FVAR(3)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C3A(H3A), C11(H11), C11A(H11A), C27(H27), C27A(H27A), C2(H2A),
 C2(H2B), C1(H1A), C1(H1B), C6(H6), C10(H10), C10(H10A), C9(H9A), C9(H9B),
 C14(H14), C17(H17), C18(H18), C19(H19), C22(H22), C45(H45), C44(H44), C43(H43),
  C42(H42), C40(H40), C36(H36), C35(H35), C34(H34), C33(H33), C58(H58),
 C57(H57), C56(H56), C55(H55), C51(H51), C49(H49), C48(H48), C47(H47), C46(H46),
  C25(H25), C25(H25A), C26(H26), C26(H26A), C30(H30)
;
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.383
_oxdiff_exptl_absorpt_empirical_full_min 0.753