Structure, magnetic properties and fluorescence selectivity of 1D chain complexes based on the pyrazolyl nitronyl nitroxide radical
Chu, Jiamin; Liu, Yi; Li, Jing; Zhu, Mei; CrystEngComm 27 (2025) 1583–1590; doi:10.1039/D4CE01113A

data_7249843
_publ_section_title
;
 Structure, magnetic properties and fluorescence selectivity of 1D chain
 complexes based on the pyrazolyl nitronyl nitroxide radical
;
_journal_issue                   11
_journal_name_full               CrystEngComm
_journal_page_first              1583
_journal_page_last               1590
_journal_paper_doi               10.1039/D4CE01113A
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C59 H47 Cu Dy F30 N8 O16'
_chemical_formula_sum            'C59 H47 Cu Dy F30 N8 O16'
_chemical_formula_weight         1920.08
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-11-25
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-11-26 deposited with the CCDC.	2025-01-27 downloaded from the CCDC.
;
_cell_angle_alpha                111.440(3)
_cell_angle_beta                 92.035(4)
_cell_angle_gamma                102.735(4)
_cell_formula_units_Z            2
_cell_length_a                   12.0447(7)
_cell_length_b                   16.7040(10)
_cell_length_c                   20.5482(13)
_cell_measurement_reflns_used    9941
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      78.72
_cell_measurement_theta_min      3.79
_cell_volume                     3722.6(4)
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      193.00
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0757
_diffrn_reflns_av_unetI/netI     0.0851
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            45969
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        66.601
_diffrn_reflns_theta_max         66.601
_diffrn_reflns_theta_min         2.329
_exptl_absorpt_coefficient_mu    6.968
_exptl_absorpt_correction_T_max  0.7543
_exptl_absorpt_correction_T_min  0.3117
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1432 before and 0.0887 after correction.
The Ratio of minimum to maximum transmission is 0.4132.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_description       block
_exptl_crystal_F_000             1900
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.33
_refine_diff_density_max         4.287
_refine_diff_density_min         -1.806
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1133
_refine_ls_number_reflns         13021
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.1170
_refine_ls_R_factor_gt           0.1011
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2526
_refine_ls_wR_factor_ref         0.2738
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9895
_reflns_number_total             13021
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce01113a2.cif
_cod_data_source_block           cu-dy
_cod_depositor_comments
'Adding full bibliography for 7249842--7249844.cif.'
_cod_database_code               7249843
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.207
_shelx_estimated_absorpt_t_min   0.107
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C19-C18 \\sim C19-C0
 with sigma of 0.02
 F1-C18 \\sim F39-C0
 with sigma of 0.02
 F2-C18 \\sim F38-C0
 with sigma of 0.02
 C18-F3 \\sim C0-F37
 with sigma of 0.02
 C19-F1 \\sim C19-F39
 with sigma of 0.04
 C19-F2 \\sim C19-F38
 with sigma of 0.04
 C19-F3 \\sim C19-F37
 with sigma of 0.04
 F1-F2 \\sim F39-F38
 with sigma of 0.04
 F1-F3 \\sim F39-F37
 with sigma of 0.04
 F2-F3 \\sim F38-F37
 with sigma of 0.04
 C18-C19 \\sim C19-C0
 with sigma of 0.02
 F38-C0 \\sim F2-C18
 with sigma of 0.02
 F3-C18 \\sim F37-C0
 with sigma of 0.02
 F39-C0 \\sim F1-C18
 with sigma of 0.02
 F3-F1 \\sim F1-F2 \\sim F3-F2
 with sigma of 0.02
 F37-F38 \\sim F37-F39 \\sim F38-F39
 with sigma of 0.02
 F27-C55 \\sim F31-C55
 with sigma of 0.02
 F31-C55 \\sim F27-C55
 with sigma of 0.02
 F26-C55 \\sim F33-C55
 with sigma of 0.02
 F25-C55 \\sim F32-C55
 with sigma of 0.02
 F27-F25 \\sim F27-F26 \\sim F25-F26
 with sigma of 0.02
 F31-F32 \\sim F32-F33 \\sim F31-F33
 with sigma of 0.02
 F4-C22 \\sim F35-C22
 with sigma of 0.02
 F6-C22 \\sim F36-C22
 with sigma of 0.02
 F5-C22 \\sim F34-C22
 with sigma of 0.02
 F34-F35 \\sim F34-F36 \\sim F35-F36
 with sigma of 0.02
 F4-F5 \\sim F4-F6 \\sim F5-F6
 with sigma of 0.02
 F1-F2 \\sim F1-F3 \\sim F2-F3
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F1 \\sim F2 \\sim C18 \\sim F3: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
F37 \\sim F39 \\sim C0 \\sim F38: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
F27 \\sim F26 \\sim F25: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
F32 \\sim F31 \\sim F33: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
F5 \\sim F4 \\sim F6: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
F34 \\sim F35 \\sim F36: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
F32 \\sim F25: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
F33 \\sim F26: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
F31 \\sim F27: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
Uanis(C18) = Uanis(C0)
4. Others
 Sof(F37)=Sof(F39)=Sof(C0)=Sof(F38)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(C18)=Sof(F3)=FVAR(1)
 Sof(F31)=Sof(F32)=Sof(F33)=1-FVAR(2)
 Sof(F25)=Sof(F26)=Sof(F27)=FVAR(2)
 Sof(F35)=Sof(F36)=Sof(F34)=1-FVAR(3)
 Sof(F5)=Sof(F4)=Sof(F6)=FVAR(3)
5.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C9(H9), C47(H47), C57(H57), C25(H25), C35(H35), C33(H33), C10(H10),
 C17(H17), C32(H32), C15(H15), C16(H16), C28(H28), C29(H29), C30(H30), C20(H20),
  C52(H52)
5.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C4(H4A,H4B,H4C), C3(H3A,H3B,H3C), C6(H6A,H6B,H6C),
 C37(H37A,H37B,H37C), C44(H44A,H44B,H44C), C41(H41A,H41B,H41C), C40(H40A,H40B,
 H40C), C43(H43A,H43B,H43C), C1(H1A,H1B,H1C)
;
_shelx_res_checksum              79543
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'