Can cage-like cations function as antagonistic ions towards pentazolate anions?
Jiang, Tianyu; Xia, Honglei; Zhang, Wenquan; Cai, Ziwu; Song, Siwei; Liu, Tianlin; CrystEngComm 26 (2024) 977–984; doi:10.1039/D3CE01168B

data_7247947
_publ_section_title
;
 Can cage-like cations function as antagonistic ions towards pentazolate
 anions?
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              977
_journal_page_last               984
_journal_paper_doi               10.1039/D3CE01168B
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'H2 O, C10 H18 N, N5'
_chemical_formula_sum            'C10 H20 N6 O'
_chemical_formula_weight         240.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-10-20
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2023-10-20 deposited with the CCDC.	2024-01-02 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 103.185(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.515(3)
_cell_length_b                   12.609(4)
_cell_length_c                   11.115(4)
_cell_measurement_reflns_used    544
_cell_measurement_temperature    296.25
_cell_measurement_theta_max      17.88
_cell_measurement_theta_min      2.48
_cell_volume                     1298.4(7)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0948
_diffrn_reflns_av_unetI/netI     0.0927
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7429
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.48
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6399
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0961 before and 0.0518 after correction. The Ratio of minimum to maximum transmission is 0.8585. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.193
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         2208
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1561
_refine_ls_R_factor_gt           0.0596
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0968P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1493
_refine_ls_wR_factor_ref         0.2125
_reflns_number_gt                989
_reflns_number_total             2208
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d3ce01168b2.cif
_cod_data_source_block           mo_1207-1202-1_0m
_cod_depositor_comments
'Adding full bibliography for 7247947--7247948.cif.'
_cod_original_cell_volume        1298.3(7)
_cod_database_code               7247947
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O1-H1c
 0.84 with sigma of 0.02
3.a Free rotating group:
 O1(H1c,H1d)
3.b Ternary CH refined with riding coordinates:
 C10(H10), C8(H8), C6(H6)
3.c Secondary CH2 refined with riding coordinates:
 C3(H3a,H3b), C1(H1a,H1b), C4(H4a,H4b), C9(H9a,H9b), C5(H5a,H5b), C7(H7a,H7b)
3.d Idealised Me refined as rotating group:
 N6(H6a,H6b,H6c)
;
_olex2_submission_special_instructions 'No special instructions were received'