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_7709926
_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, 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   geom
_audit_creation_date             2019-11-29
_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                85.319(5)
_cell_angle_beta                 68.224(6)
_cell_angle_gamma                73.146(6)
_cell_formula_units_Z            2
_cell_length_a                   11.2759(7)
_cell_length_b                   13.1435(9)
_cell_length_c                   15.0492(9)
_cell_measurement_reflns_used    6293
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.0840
_cell_measurement_theta_min      2.8750
_cell_volume                     1981.4(2)
_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_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.839
_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  0.0430
_diffrn_reflns_av_unetI/netI     0.0789
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.839
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18723
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.839
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.512
_diffrn_reflns_theta_min         2.020
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.489
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90560
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.862
_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         1.008
_refine_diff_density_min         -0.793
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         9276
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0475
_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^)+(0.0208P)^2^+3.5413P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0842
_refine_ls_wR_factor_ref         0.0915
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7780
_reflns_number_total             9276
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00501h2.cif
_cod_data_source_block           lxy191125b
_cod_original_formula_sum        'C33 H19.50 Cl8 Dy N7.50 O9'
_cod_database_code               7709926
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.789
_shelx_estimated_absorpt_t_min   0.754
_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
 C1A-N8
 1.137 with sigma of 0.01
 C1A-C1B
 1.456 with sigma of 0.01
 C1B-N8
 2.593 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N8 \\sim C1A \\sim C1B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
4. Rigid body (RIGU) restrains
 N8, C1A, C1B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: N8(0.5) C1A(0.5) C1B(0.5) H1BA(0.5) H1BB(0.5) H1BC(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B)
6.b 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)
6.c Idealised Me refined as rotating group:
 C1B(H1BA,H1BB,H1BC)
;
_shelx_res_checksum              31995
_shelx_hkl_checksum              54549
_olex2_submission_special_instructions 'No special instructions were received'