Electrosynthesis of a <i>cyclo</i>-N<sub>5</sub><sup>-</sup> anion <i>via</i> TEMPO-mediated selective C-N bond cleavage in aryl-pentazole.
Zhao, Feng; Gu, Ziyan; Song, Bin; Ju, Xuehai; Hu, Bingcheng; Zhang, Chong; Chemical communications (Cambridge, England) 61 (2025) 12725–12728; doi:10.1039/d5cc02899j

data_7134843
_publ_section_title
;
 Electrosynthesis of a <i>cyclo</i>-N<sub>5</sub><sup>-</sup> anion
 <i>via</i> TEMPO-mediated selective C-N bond cleavage in aryl-pentazole.
;
_journal_issue                   68
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              12725
_journal_page_last               12728
_journal_paper_doi               10.1039/d5cc02899j
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'Co H8 N10 O4, 2(H4 O2)'
_chemical_formula_sum            'Co H16 N10 O8'
_chemical_formula_weight         343.16
_space_group_crystal_system      orthorhombic
_space_group_IT_number           69
_space_group_name_Hall           '-F 2 2'
_space_group_name_H-M_alt        'F m m m'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2024-12-11
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-04-22 deposited with the CCDC.	2025-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.4648(3)
_cell_length_b                   12.1663(5)
_cell_length_c                   17.1617(7)
_cell_measurement_reflns_used    3187
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      68.07
_cell_measurement_theta_min      7.28
_cell_volume                     1349.81(10)
_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      193.00
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            3725
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.059
_diffrn_reflns_theta_min         7.280
_diffrn_source_current           1.1
_diffrn_source_power             0.05500000000000001
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.541
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.4187
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1312 before and 0.0533 after correction.
The Ratio of minimum to maximum transmission is 0.5560.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic light colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.689
_exptl_crystal_description       block
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     32
_refine_ls_number_reflns         370
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.173
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0270
_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^)+(0.0430P)^2^+2.6243P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0739
_reflns_Friedel_coverage         0.000
_reflns_number_gt                370
_reflns_number_total             370
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc02899j2.cif
_cod_data_source_block           cu_nlg_zf_0m
_cod_depositor_comments          'Adding full bibliography for 7134843.cif.'
_cod_database_code               7134843
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: H1A(0.5) H1B(0.5) H2A(0.5) H2B(0.5)
3.a Riding coordinates:
 O1(H1A,H1B), O2(H2A,H2B)
;
_shelx_res_checksum              80947
_shelx_hkl_checksum              40966
_olex2_submission_special_instructions 'No special instructions were received'