Constructing layered structure amidine-based pentazolate salts with low sensitivity
Wang, Pengfei; Liu, Lile; Sun, Zebang; Qin, Feng; Shi, Lei; Gao, Chao; Du, Yang; Zhang, Chong; Hu, Bingcheng; Sun, Chengguo; CrystEngComm 26 (2024) 4114–4120; doi:10.1039/D4CE00521J

data_7248936
_publ_section_title
;
 Constructing layered structure amidine-based pentazolate salts with low
 sensitivity
;
_journal_issue                   30
_journal_name_full               CrystEngComm
_journal_page_first              4114
_journal_page_last               4120
_journal_paper_doi               10.1039/D4CE00521J
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'N5, C2 H7 N2'
_chemical_formula_sum            'C2 H7 N7'
_chemical_formula_weight         129.125
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_Int_Tables_number      62
_atom_sites_solution_primary     dual
_audit_creation_date             2024-05-08
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-05-08 deposited with the CCDC.	2024-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.629(1)
_cell_length_b                   6.5997(6)
_cell_length_c                   7.4672(5)
_cell_measurement_reflns_used    2345
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      25.52
_cell_measurement_theta_min      3.11
_cell_volume                     671.65(9)
_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  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.9955
_diffrn_measured_fraction_theta_max 0.9941
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_Laue_measured_fraction_full 0.9955
_diffrn_reflns_Laue_measured_fraction_max 0.9941
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            5669
_diffrn_reflns_point_group_measured_fraction_full 0.9955
_diffrn_reflns_point_group_measured_fraction_max 0.9941
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         3.11
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6764
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1032 before and 0.0485 after correction.
The Ratio of minimum to maximum transmission is 0.9072.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_description       plate
_exptl_crystal_F_000             272.210
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.2161
_refine_diff_density_min         -0.2229
_refine_diff_density_rms         0.0507
_refine_ls_d_res_high            0.7710
_refine_ls_d_res_low             6.5487
_refine_ls_goodness_of_fit_ref   1.0424
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    6
_refine_ls_number_parameters     62
_refine_ls_number_reflns         836
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0424
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0444
_refine_ls_shift/su_max          -0.0005
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0611P)^2^+0.0994P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1078
_refine_ls_wR_factor_ref         0.1230
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              17
_reflns_limit_h_min              0
_reflns_limit_k_max              8
_reflns_limit_k_min              0
_reflns_limit_l_max              9
_reflns_limit_l_min              0
_reflns_number_gt                594
_reflns_number_total             836
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4ce00521j2.cif
_cod_data_source_block           1_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7248931--7248937.cif.'
_cod_database_code               7248936
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
2.a X=CH2 refined with riding coordinates:
 N6(H6a,H6b), N7(H7a,H7b)
;
_olex2_submission_special_instructions 'No special instructions were received'