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_1574467
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-05-30
_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                 111.587(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.7539(12)
_cell_length_b                   25.787(3)
_cell_length_c                   11.2182(14)
_cell_measurement_reflns_used    5368
_cell_measurement_temperature    298.00
_cell_measurement_theta_max      26.112
_cell_measurement_theta_min      2.372
_cell_volume                     2623.7(6)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      298.00
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.983
_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  0.0810
_diffrn_reflns_av_unetI/netI     0.0756
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            22763
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.564
_diffrn_reflns_theta_min         1.952
_diffrn_source_current           40.0
_diffrn_source_power             1.8
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.935
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6329
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1120 before and 0.0646 after correction.
The Ratio of minimum to maximum transmission is 0.8488.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_description       block
_exptl_crystal_F_000             1278
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.214
_refine_diff_density_min         -0.894
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         6106
_refine_ls_number_restraints     368
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.1165
_refine_ls_R_factor_gt           0.0680
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0850P)^2^+6.5300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1603
_refine_ls_wR_factor_ref         0.1927
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3909
_reflns_number_total             6106
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc01302j2.cif
_cod_data_source_block           y_a_CCDC3
_cod_depositor_comments
'Adding full bibliography for 1574464--1574468.cif.'
_cod_original_cell_volume        2623.8(5)
_cod_database_code               1574467
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.799
_shelx_estimated_absorpt_t_min   0.564
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O3-C16 \\sim O2-C18
 with sigma of 0.01
 C18-C19 \\sim C16-C17
 with sigma of 0.01
3. Rigid bond restraints
 O10, N5, O10, O9, O11
 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, C16, C17, C18, C19
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
 O7, C21, C22, C23, C24, C25, N4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O8, C26, C27, C28, C29, C30, N3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
O10 \\sim N5 \\sim O10 \\sim O9 \\sim O11: 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 C16 \\sim C17 \\sim C18 \\sim C19: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
O7 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim N4: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
O8 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim N3: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
5. Others
 Fixed Sof: C26(0.5) H26(0.5) C27(0.5) H27(0.5) C29(0.5) H29(0.5) C30(0.5)
 H30(0.5)
6.a Riding coordinates:
 C16(H16A,H16B), C26(H26), C27(H27), C29(H29), C30(H30), N3(H3), N4(H4A)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C18(H18A,H18B)
6.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C11(H11), C12(H12), C13(H13),
 C14(H14), C21(H21), C22(H22), C24(H24), C25(H25)
6.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              41094
_olex2_submission_special_instructions 'No special instructions were received'