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_7249842
_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 F30 Gd N8 O16'
_chemical_formula_sum            'C59 H47 Cu F30 Gd N8 O16'
_chemical_formula_weight         1914.83
_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                111.534(2)
_cell_angle_beta                 91.936(2)
_cell_angle_gamma                102.731(2)
_cell_formula_units_Z            2
_cell_length_a                   12.0459(9)
_cell_length_b                   16.7225(13)
_cell_length_c                   20.5508(15)
_cell_measurement_reflns_used    9322
_cell_measurement_temperature    192.80
_cell_measurement_theta_max      27.23
_cell_measurement_theta_min      2.34
_cell_volume                     3726.0(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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      192.80
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_unetI/netI     0.0718
_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       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23302
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.923
_exptl_absorpt_coefficient_mu    1.310
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0963 before and 0.0540 after correction.
The Ratio of minimum to maximum transmission is 0.8030.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_description       block
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.52
_exptl_crystal_size_min          0.45
_refine_diff_density_max         2.475
_refine_diff_density_min         -0.992
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1134
_refine_ls_number_reflns         13036
_refine_ls_number_restraints     256
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0949
_refine_ls_R_factor_gt           0.0653
_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^)+(0.0795P)^2^+13.3089P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1549
_refine_ls_wR_factor_ref         0.1779
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9736
_reflns_number_total             13036
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce01113a2.cif
_cod_data_source_block           cu-gd
_cod_depositor_comments
'Adding full bibliography for 7249842--7249844.cif.'
_cod_database_code               7249842
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.590
_shelx_estimated_absorpt_t_min   0.527
_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
 O5-C19 \\sim O5-C60
 with sigma of 0.02
 C21-C20 \\sim C61-C02Q
 with sigma of 0.02
 C21-C22 \\sim C61-C62
 with sigma of 0.02
 F2-C18 \\sim F02C-C0
 with sigma of 0.02
 C19-C20 \\sim C60-C02Q
 with sigma of 0.02
 C19-C18 \\sim C60-C0
 with sigma of 0.02
 F6-C22 \\sim F02N-C62
 with sigma of 0.02
 F5-C22 \\sim F02R-C62
 with sigma of 0.02
 F3-C18 \\sim F02W-C0
 with sigma of 0.02
 C22-F4 \\sim C62-F0
 with sigma of 0.02
 C18-F1 \\sim C0-F9A
 with sigma of 0.02
 O4-C20 \\sim O4-C02Q
 with sigma of 0.04
 O4-C22 \\sim O4-C62
 with sigma of 0.04
 O5-C20 \\sim O5-C02Q
 with sigma of 0.04
 O5-C18 \\sim O5-C0
 with sigma of 0.04
 C21-C19 \\sim C61-C60
 with sigma of 0.04
 C21-F6 \\sim C61-F02N
 with sigma of 0.04
 C21-F5 \\sim C61-F02R
 with sigma of 0.04
 C21-F4 \\sim C61-F0
 with sigma of 0.04
 F2-C19 \\sim F02C-C60
 with sigma of 0.04
 F2-F3 \\sim F02C-F02W
 with sigma of 0.04
 F2-F1 \\sim F02C-F9A
 with sigma of 0.04
 C19-F3 \\sim C60-F02W
 with sigma of 0.04
 C19-F1 \\sim C60-F9A
 with sigma of 0.04
 F6-F5 \\sim F02N-F02R
 with sigma of 0.04
 F6-F4 \\sim F02N-F0
 with sigma of 0.04
 C20-C22 \\sim C02Q-C62
 with sigma of 0.04
 C20-C18 \\sim C02Q-C0
 with sigma of 0.04
 F5-F4 \\sim F02R-F0
 with sigma of 0.04
 F3-F1 \\sim F02W-F9A
 with sigma of 0.04
 F02W-C0 \\sim F3-C18
 with sigma of 0.02
 F1-C18 \\sim F9A-C0
 with sigma of 0.02
 F02C-C0 \\sim F2-C18
 with sigma of 0.02
 C60-C0 \\sim C18-C19
 with sigma of 0.02
 O5-C60 \\sim O5-C19
 with sigma of 0.02
 C60-C02Q \\sim C20-C19
 with sigma of 0.02
 C02Q-C61 \\sim C20-C21
 with sigma of 0.02
 O4-C21 \\sim O4-C61
 with sigma of 0.02
 F0-C62 \\sim F4-C22
 with sigma of 0.02
 C62-C61 \\sim C22-C21
 with sigma of 0.02
 F02R-C62 \\sim F5-C22
 with sigma of 0.02
 F02N-C62 \\sim F6-C22
 with sigma of 0.02
 F9-C27 \\sim F39-C27
 with sigma of 0.02
 F39-C27 \\sim F9-C27
 with sigma of 0.02
 F7-C27 \\sim F33-C27
 with sigma of 0.02
 F8-C27 \\sim F32-C27
 with sigma of 0.02
 F9-F8 \\sim F9-F7 \\sim F8-F7
 with sigma of 0.02
 F39-F32 \\sim F39-F33 \\sim F32-F33
 with sigma of 0.02
 F5-F4 \\sim F5-F6 \\sim F4-F6
 with sigma of 0.02
 F1-F3 \\sim F1-F2 \\sim F3-F2
 with sigma of 0.02
 C54-F20 \\sim C54-F37
 with sigma of 0.02
 F21-C54 \\sim F36-C54
 with sigma of 0.02
 F19-C54 \\sim F38-C54
 with sigma of 0.02
 F20-C54 \\sim F37-C54
 with sigma of 0.02
 F21-F20 \\sim F21-F19 \\sim F20-F19
 with sigma of 0.02
 F36-F37 \\sim F36-F38 \\sim F37-F38
 with sigma of 0.02
 F10-C23 \\sim F31-C23
 with sigma of 0.02
 F12-C23 \\sim F34-C23
 with sigma of 0.02
 F11-C23 \\sim F35-C23
 with sigma of 0.02
 F31-C23 \\sim F10-C23
 with sigma of 0.02
 F34-C23 \\sim F12-C23
 with sigma of 0.02
 F11-F10 \\sim F10-F12 \\sim F11-F12
 with sigma of 0.02
 F31-F34 \\sim F31-F35 \\sim F34-F35
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F02W \\sim C0 \\sim F02C \\sim F9A \\sim C60 \\sim C02Q \\sim C61 \\sim F02R
\\sim F0 \\sim F02N \\sim C62: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C21 \\sim F2 \\sim C19 \\sim F6 \\sim C20 \\sim F5 \\sim F3 \\sim C22 \\sim F4
\\sim C18 \\sim F1: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
F9 \\sim F7 \\sim F8: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
F39 \\sim F32 \\sim F33: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
F21 \\sim F20 \\sim F19: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
F36 \\sim F38 \\sim F37: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
F11 \\sim F10 \\sim F12: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
F31 \\sim F35 \\sim F34: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
F36 \\sim F19 \\sim F38 \\sim F20 \\sim F37 \\sim F21: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
F4 \\sim F0 \\sim F6 \\sim F02N \\sim F02R \\sim F5: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C61) = Uanis(C21)
Uanis(C02Q) = Uanis(C20)
Uanis(C60) = Uanis(C19)
Uanis(C0) = Uanis(C18)
Uanis(F35) = Uanis(F12)
Uanis(F10) = Uanis(F34)
Uanis(F11) = Uanis(F31)
Uanis(F9) = Uanis(F39)
Uanis(F32) = Uanis(F8)
Uanis(F33) = Uanis(F7)
Uanis(F6) = Uanis(F02N)
Uanis(F0) = Uanis(F4)
Uanis(F5) = Uanis(F02R)
Uanis(F37) = Uanis(F21)
Uanis(F38) = Uanis(F20)
Uanis(F19) = Uanis(F36)
4. Others
 Sof(F02W)=Sof(C0)=Sof(F02C)=Sof(F9A)=Sof(C60)=Sof(C02Q)=Sof(H02Q)=Sof(C61)=
 Sof(F02R)=Sof(F0)=Sof(F02N)=Sof(C62)=1-FVAR(1)
 Sof(C21)=Sof(F2)=Sof(C19)=Sof(F6)=Sof(C20)=Sof(H20)=Sof(F5)=Sof(F3)=Sof(C22)=
 Sof(F4)=Sof(C18)=Sof(F1)=FVAR(1)
 Sof(F39)=Sof(F33)=Sof(F32)=1-FVAR(2)
 Sof(F9)=Sof(F8)=Sof(F7)=FVAR(2)
 Sof(F36)=Sof(F38)=Sof(F37)=1-FVAR(3)
 Sof(F19)=Sof(F21)=Sof(F20)=FVAR(3)
 Sof(F35)=Sof(F34)=Sof(F31)=1-FVAR(4)
 Sof(F11)=Sof(F10)=Sof(F12)=FVAR(4)
5.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C33(H33), C17(H17), C13(H13), C10(H10), C32(H32), C52(H52), C35(H35),
 C28(H28), C57(H57), C16(H16), C15(H15), C25(H25), C30(H30), C29(H29), C20(H20),
  C47(H47), C02Q(H02Q)
5.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C1(H1A,H1B,H1C), C41(H41A,H41B,H41C), C44(H44A,H44B,H44C),
 C37(H37A,H37B,H37C), C14(H14A,H14B,H14C), C6(H6A,H6B,H6C), C42(H42A,H42B,H42C),
  C40(H40A,H40B,H40C), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              84506
_olex2_submission_special_instructions 'No special instructions were received'