A thermally and photoresponsive luminescent single-molecule magnet based on dysprosium–anthracene: effect of temperature on anthracene photocycloaddition
Ma, Xiu-Fang; Hou, Xin-Lan; Qin, Ye-Hui; Teng, Qian; Bao, Song-Song; Tian, Yu-Xi; Zheng, Li-Min; Chemical Science 16 (2025) 10340–10348; doi:10.1039/D5SC01302J

data_1574468
_publ_section_title
;
 A thermally and photoresponsive luminescent single-molecule magnet based
 on dysprosium--anthracene: effect of temperature on anthracene
 photocycloaddition
;
_journal_issue                   23
_journal_name_full               'Chemical Science'
_journal_page_first              10340
_journal_page_last               10348
_journal_paper_doi               10.1039/D5SC01302J
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C50 H52 Dy N5 O11 P2 Se2'
_chemical_formula_sum            'C50 H52 Dy N5 O11 P2 Se2'
_chemical_formula_weight         1281.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2024-11-28
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2025-02-05 deposited with the CCDC.	2025-04-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.946(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.5847(12)
_cell_length_b                   25.809(3)
_cell_length_c                   11.2751(13)
_cell_measurement_reflns_used    4531
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      25.579
_cell_measurement_theta_min      2.308
_cell_volume                     2568.4(5)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      300(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_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  0.0894
_diffrn_reflns_av_unetI/netI     0.0920
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            21742
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.524
_diffrn_reflns_theta_min         1.961
_exptl_absorpt_coefficient_mu    2.998
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5487
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0993 before and 0.0766 after correction.
The Ratio of minimum to maximum transmission is 0.7359.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_description       bloc
_exptl_crystal_F_000             1278
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.012
_refine_diff_density_max         1.410
_refine_diff_density_min         -1.580
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         6016
_refine_ls_number_restraints     390
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1493
_refine_ls_R_factor_gt           0.0858
_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^)+(0.0674P)^2^+22.2273P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1817
_refine_ls_wR_factor_ref         0.2206
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3615
_reflns_number_total             6016
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc01302j2.cif
_cod_data_source_block           y_a_CCDC4
_cod_depositor_comments
'Adding full bibliography for 1574464--1574468.cif.'
_cod_original_cell_volume        2568.4(6)
_cod_database_code               1574468
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.558
_olex2_refinement_description
;
1. Restrained distances
 C28-C29 \\sim C29-C25 \\sim C25-C26 \\sim C26-C27 \\sim C23-C24
 with sigma of 0.01
 C28-C25 \\sim C25-C27 \\sim C23-C20
 with sigma of 0.02
 N4-C25 \\sim N3-C20
 with sigma of 0.02
 N4-C29 \\sim N3-C24 \\sim N3-C21
 with sigma of 0.02
 N4-C28 \\sim N3-C23 \\sim N3-C22
 with sigma of 0.02
 C16-C17 \\sim C18-C19
 with sigma of 0.01
 O3-C18 \\sim O2-C16
 with sigma of 0.01
2. Rigid bond restraints
 O7, C23, C24, C20, C21, C22, N3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O8, C28, C29, C25, C26, C27, N4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 P1, O1, O3, O2, C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13, C14,
 C15, C18, C19, C16, C17
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 N2, O10, O9, O11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
O7 \\sim C23 \\sim C24 \\sim C20 \\sim C21 \\sim C22 \\sim N3: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
O8 \\sim C28 \\sim C29 \\sim C25 \\sim C26 \\sim C27 \\sim N4: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
P1 \\sim O1 \\sim O3 \\sim O2 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5
\\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13
\\sim C14 \\sim C15 \\sim C18 \\sim C19 \\sim C16 \\sim C17: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
N2 \\sim O10 \\sim O9 \\sim O11: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
4. Others
 Fixed Sof: C28(0.5) H28(0.5) C29(0.5) H29(0.5) C26(0.5) H26(0.5) C27(0.5)
 H27(0.5) N4(0.5) H4A(0.5)
5.a Riding coordinates:
 C28(H28), C29(H29), C26(H26), C27(H27), N4(H4A)
5.b Ternary CH refined with riding coordinates:
 C9(H9)
5.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C18(H18A,H18B), C16(H16A,H16B)
5.d Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C11(H11), C12(H12), C13(H13), C14(H14),
 C23(H23), C24(H24), C21(H21), C22(H22), N3(H3)
5.e Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              29057
_olex2_submission_special_instructions 'No special instructions were received'