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_7709928
_publ_section_title
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 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, 0.5(C2 H3 N)'
_chemical_formula_sum            'C33 H19.5 Cl8 Dy N7.5 O9'
_chemical_formula_weight         1111.16
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-27
_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                81.914(7)
_cell_angle_beta                 68.257(6)
_cell_angle_gamma                72.685(6)
_cell_formula_units_Z            2
_cell_length_a                   11.511(2)
_cell_length_b                   13.220(3)
_cell_length_c                   15.127(3)
_cell_measurement_reflns_used    9242
_cell_measurement_temperature    296.0
_cell_measurement_theta_max      27.38
_cell_measurement_theta_min      2.89
_cell_volume                     2040.1(7)
_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_temperature      296.0
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            70045
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.450
_diffrn_reflns_theta_min         2.182
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.417
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.809
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.808
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     617
_refine_ls_number_reflns         9194
_refine_ls_number_restraints     555
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0256
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0244P)^2^+2.1123P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0594
_refine_ls_wR_factor_ref         0.0619
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8504
_reflns_number_total             9194
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00501h2.cif
_cod_data_source_block           xj44
_cod_original_cell_volume        2040.2(8)
_cod_original_formula_sum        'C33 H19.50 Cl8 Dy N7.50 O9'
_cod_database_code               7709928
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.794
_shelx_estimated_absorpt_t_min   0.760
_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. Restrained distances
 C33-N8
 1.137 with sigma of 0.01
 C33-C34
 1.456 with sigma of 0.01
 C34-N8
 2.593 with sigma of 0.02
 N7-C30 \\sim N7A-C30A
 with sigma of 0.02
 O7-C27 \\sim O7-C27A
 with sigma of 0.02
 O7-C27A \\sim O7-C27
 with sigma of 0.02
 Cl8A-C32A \\sim Cl8-C32
 with sigma of 0.02
 Cl7-C28 \\sim Cl7A-C28A
 with sigma of 0.02
 O8A-N7A \\sim O8-N7
 with sigma of 0.02
 O9A-N7A \\sim O9-N7
 with sigma of 0.02
 O9-O8 \\sim O9A-O8A
 with sigma of 0.02
 O9-C30 \\sim O9A-C30A
 with sigma of 0.02
 O8-C30 \\sim O8A-C30A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl7 \\sim Cl8 \\sim O8 \\sim O9 \\sim N7 \\sim C27 \\sim C28 \\sim C29 \\sim
C30 \\sim C31 \\sim C32 \\sim C27A \\sim C32A \\sim C31A \\sim C30A \\sim C29A
\\sim C28A \\sim Cl7A \\sim N7A \\sim O8A \\sim O9A \\sim Cl8A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
N8 \\sim C33 \\sim C34: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C33 \\sim N8 \\sim C34: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C27A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N8) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 O7, C27, C28, C29, C30, C31, C32, Cl8, N7, O8, O9, Cl7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C27A, C32A, C31A, C30A, C29A, C28A, Cl7A, N7A, O8A, O9A, Cl8A, O7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 N8, C33, C34
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C33, N8, C34
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Others
 Sof(C27A)=Sof(C32A)=Sof(C31A)=Sof(H31A)=Sof(C30A)=Sof(C29A)=Sof(H29A)=
 Sof(C28A)=Sof(Cl7A)=Sof(N7A)=Sof(O8A)=Sof(O9A)=Sof(Cl8A)=1-FVAR(1)
 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(1)
 Fixed Sof: N8(0.5) C33(0.5) C34(0.5) H34A(0.5) H34B(0.5) H34C(0.5)
6.a Riding coordinates:
 C34(H34A,H34B,H34C)
6.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C6(H6), C9(H9), C11(H11), C13(H13), C14(H14),
 C17(H17), C19(H19), C23(H23), C25(H25), C29(H29), C31(H31), C31A(H31A),
 C29A(H29A)
6.d Fitted hexagon refined as free rotating group:
 C27(C28,C29,C30,C31,C32), C27A(C32A,C31A,C30A,C29A,C28A)
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_shelx_res_checksum              35636
_shelx_hkl_checksum              47536
_olex2_submission_special_instructions 'No special instructions were received'