Reversible on-off switching of Dy(III) single-molecule magnets via single-crystal-to-single-crystal transformation
Xi, Jing; Cen, Peipei; Guo, Yan; Li, Yuzhu; Qin, Yuanyuan; Zhang, Yi-Quan; Song, Weiming; Liu, Xiangyu; Dalton Transactions  (2022) –; doi:10.1039/D2DT00501H

data_7709925
_publ_section_title
;
 Reversible on-off switching of Dy(III) single-molecule magnets via
 single-crystal-to-single-crystal transformation
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00501H
_journal_year                    2022
_chemical_formula_moiety         'C32 H18 Cl8 Dy N7 O9'
_chemical_formula_sum            'C32 H18 Cl8 Dy N7 O9'
_chemical_formula_weight         1090.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-01-14 deposited with the CCDC.	2022-04-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.797(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0086(5)
_cell_length_b                   16.5773(7)
_cell_length_c                   20.2262(10)
_cell_measurement_reflns_used    4736
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      73.5950
_cell_measurement_theta_min      3.4120
_cell_volume                     4005.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.963
_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     19.00  64.00   1.00    1.00    --   39.98 -99.00-120.00   45
  2  \w     26.00  53.00   1.00    1.00    --   39.98-125.00   0.00   27
  3  \w     57.00 134.00   1.00    2.00    --  108.20 -45.00  60.00   77
  4  \w     80.00 172.00   1.00    2.00    --  108.20  30.00 -60.00   92
  5  \w    127.00 178.00   1.00    2.00    --  108.20  61.00-120.00   51
  6  \w    124.00 177.00   1.00    2.00    --  108.20  45.00  30.00   53
  7  \w    104.00 178.00   1.00    3.00    --  108.20 125.00 150.00   74
  8  \w     96.00 127.00   1.00    3.00    --  108.20 125.00 120.00   31
  9  \w     79.00 112.00   1.00    3.00    --  108.20  61.00-120.00   33
 10  \w     44.00 101.00   1.00    3.00    --  108.20 -94.00  90.00   57
 11  \w    -66.00  29.00   1.00    1.80    --  -39.98  57.00-150.00   95
 12  \w   -106.00 -16.00   1.00    1.80    --  -39.98 -37.00  30.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0469825000
_diffrn_orient_matrix_UB_12      0.0090720000
_diffrn_orient_matrix_UB_13      -0.0733392000
_diffrn_orient_matrix_UB_21      -0.0700029000
_diffrn_orient_matrix_UB_22      -0.0772006000
_diffrn_orient_matrix_UB_23      0.0052542000
_diffrn_orient_matrix_UB_31      -0.0975986000
_diffrn_orient_matrix_UB_32      0.0508965000
_diffrn_orient_matrix_UB_33      0.0213349000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0654
_diffrn_reflns_av_unetI/netI     0.0948
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15315
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.402
_diffrn_reflns_theta_min         3.454
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.423
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.808
_exptl_crystal_description       block
_exptl_crystal_F_000             2132
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.531
_refine_diff_density_min         -1.123
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     736
_refine_ls_number_reflns         7881
_refine_ls_number_restraints     927
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.1127
_refine_ls_R_factor_gt           0.0905
_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^)+(0.0068P)^2^+76.1494P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1821
_refine_ls_wR_factor_ref         0.1925
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6143
_reflns_number_total             7881
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00501h2.cif
_cod_data_source_block           exp_1963
_cod_database_code               7709925
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.337
_shelx_estimated_absorpt_t_min   0.239
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
C12 \\sim C12A \\sim C13 \\sim C13A \\sim C14 \\sim C14A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
C21 \\sim C21A \\sim C22 \\sim C22A \\sim C23A \\sim C24 \\sim C25 \\sim C25A
\\sim C26 \\sim C26A \\sim C24A \\sim C23 \\sim O5 \\sim O5A \\sim O6 \\sim O6A
\\sim N6 \\sim N6A: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02
C27 \\sim C27A \\sim C28 \\sim C28A \\sim C29 \\sim C30 \\sim C30A \\sim C31
\\sim C31A \\sim C32A \\sim C32 \\sim Cl7 \\sim Cl7A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O6) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Cl7A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Cl2A) = Uanis(Cl2)
Uanis(C11) = Uanis(C11A)
Uanis(C14) = Uanis(C14A)
Uanis(C28) = Uanis(C28A)
3. Rigid body (RIGU) restrains
 Cl7, Cl8, O7, O8, O9, N7, C27, C28, C29, C30, C31, C32
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl5, Cl6, O4, O5, O6, N6, C21, C22, C23, C24, C25, C26
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl5A, Cl6A, O4, O5A, O6A, N6A, C21A, C22A, C23A, C24A, C25A, C26A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl7A, Cl8A, O7, O8A, O9A, N7A, C27A, C28A, C29A, C30A, C31A, C32A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl2A, N4, C10, C11, C12, C13, C14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl2, N4, C10, C11A, C12A, C13A, C14A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(Cl2A)=Sof(Cl5A)=Sof(Cl6A)=Sof(O5A)=Sof(O6A)=Sof(N6A)=Sof(C21A)=Sof(C22A)=
 Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(C25A)=Sof(H25A)=Sof(C26A)=1-FVAR(1)
 Sof(Cl2)=Sof(Cl5)=Sof(Cl6)=Sof(O5)=Sof(O6)=Sof(N6)=Sof(C21)=Sof(C22)=Sof(C23)=
 Sof(H23)=Sof(C24)=Sof(C25)=Sof(H25)=Sof(C26)=FVAR(1)
 Sof(Cl7A)=Sof(Cl8A)=Sof(O8A)=Sof(O9A)=Sof(N7A)=Sof(C27A)=Sof(C28A)=Sof(C29A)=
 Sof(H29A)=Sof(C30A)=Sof(C31A)=Sof(H31A)=Sof(C32A)=1-FVAR(2)
 Sof(Cl7)=Sof(Cl8)=Sof(O8)=Sof(O9)=Sof(N7)=Sof(C27)=Sof(C28)=Sof(C29)=Sof(H29)=
 Sof(C30)=Sof(C31)=Sof(H31)=Sof(C32)=FVAR(2)
 Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(C13A)=Sof(H13A)=Sof(C14A)=Sof(H14A)=1-FVAR(3)
 Sof(C11)=Sof(H11)=Sof(C12)=Sof(C13)=Sof(H13)=Sof(C14)=Sof(H14)=FVAR(3)
5.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C6(H6), C9(H9), C11(H11), C11A(H11A), C13(H13),
 C13A(H13A), C14(H14), C14A(H14A), C17(H17), C19(H19), C23(H23), C23A(H23A),
 C25(H25), C25A(H25A), C29(H29), C29A(H29A), C31(H31), C31A(H31A)
;
_shelx_res_checksum              33921
_shelx_hkl_checksum              72100
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.036
_oxdiff_exptl_absorpt_empirical_full_min 0.644