#------------------------------------------------------------------------------
#$Date: 2024-08-05 21:29:33 +0300 (Mon, 05 Aug 2024) $
#$Revision: 293801 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/89/7248931.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7248931
loop_
_publ_author_name
'Wang, Pengfei'
'Liu, Lile'
'Sun, Zebang'
'Qin, Feng'
'Shi, Lei'
'Gao, Chao'
'Du, Yang'
'Zhang, Chong'
'Hu, Bingcheng'
'Sun, Chengguo'
_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, C H5 N2'
_chemical_formula_sum            'C H5 N7'
_chemical_formula_weight         115.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-04-29 deposited with the CCDC.	2024-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.756(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.9752(6)
_cell_length_b                   15.7038(18)
_cell_length_c                   7.0385(10)
_cell_measurement_reflns_used    1361
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      4.00
_cell_volume                     523.72(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2019/3 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker D8 QUEST PHOTON 100'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2234
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.431
_diffrn_reflns_theta_min         2.594
_diffrn_source.source            'Ius 2.0'
_diffrn_source.type              microfocus
_exptl_absorpt_coefficient_mu    0.116
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6511
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_description       block
_exptl_crystal_F_000             240
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.157
_refine_diff_density_min         -0.130
_refine_diff_density_rms         0.032
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     38
_refine_ls_number_reflns         596
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0341
_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/[σ²(Fo²)+(0.0426P)²+0.0880P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0855
_reflns_Friedel_coverage         0.000
_reflns_number_gt                487
_reflns_number_total             596
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ce00521j2.cif
_cod_data_source_block           WPF240415_1_a
_cod_depositor_comments
'Adding full bibliography for 7248931--7248937.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7248931
_shelx_shelxl_version_number     2019/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.979
_shelx_estimated_absorpt_t_max   0.982
_shelx_res_file
;
TITL WPF240415_1_a.res in C2/c
    WPF240415_1_a.res
    created by SHELXL-2019/3 at 21:11:11 on 16-Apr-2024
CELL 0.71073 4.9752 15.7038 7.0385 90.000 107.756 90.000
ZERR 4.00 0.0006 0.0018 0.0010 0.000 0.004 0.000
LATT 7
SYMM -x, y, -z+1/2
SFAC C  H    N
UNIT 4  20   28
L.S. 10
ACTA
BOND $H
FMAP 2
PLAN -5
omit 3   3   0
size 0.18 0.17 0.16
HTAB N4 N3
EQIV $2 -x, -y+1, -z+1
HTAB N4 N2_$2
CONF
TEMP 23.000
WGHT    0.042600    0.088000
FVAR       1.60072
N4    3    0.271599    0.384096    0.648478    11.00000    0.02739    0.03762 =
         0.04662   -0.00416   -0.00082   -0.00409
AFIX  93
H4A   2    0.264457    0.438812    0.645305    11.00000   -1.20000
H4B   2    0.126481    0.354767    0.583973    11.00000   -1.20000
AFIX   0
C1    1    0.500000    0.346013    0.750000    10.50000    0.03337    0.03025 =
         0.04666    0.00000    0.01058    0.00000
AFIX  43
H1    2    0.499999    0.286791    0.749998    10.50000   -1.20000
AFIX   0
N1    3    0.500000    0.701095    0.750000    10.50000    0.03769    0.03312 =
         0.05019    0.00000   -0.00036    0.00000
N2    3    0.289825    0.652066    0.652574    11.00000    0.03092    0.03795 =
         0.04579    0.00068   -0.00161    0.00003
N3    3    0.369646    0.573006    0.689636    11.00000    0.03966    0.03502 =
         0.05227   -0.00276    0.00225   -0.00454

HKLF 4 1 1 0 0 0 1 0 0 0 1




REM  WPF240415_1_a.res in C2/c
REM wR2 = 0.0855, GooF = S = 1.090, Restrained GooF = 1.090 for all data
REM R1 = 0.0341 for 487 Fo > 4sig(Fo) and 0.0453 for all 596 data
REM 38 parameters refined using 0 restraints

END

WGHT      0.0423      0.0831

REM Highest difference peak  0.157,  deepest hole -0.130,  1-sigma level  0.032
Q1    1  -0.1458  0.3417  0.4023  11.00000  0.05    0.16
Q2    1  -0.2716  0.3842  0.2610  11.00000  0.05    0.11
Q3    1  -0.2917  0.4579  0.2593  11.00000  0.05    0.10
Q4    1   0.2920  0.4320  0.5490  11.00000  0.05    0.10
Q5    1   0.2295  0.4230  0.7117  11.00000  0.05    0.10
;
_shelx_res_checksum              28871
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N4 N 0.27160(18) 0.38410(5) 0.64848(14) 0.0399(3) Uani 1 1 d . . . . .
H4A H 0.264457 0.438812 0.645305 0.048 Uiso 1 1 calc R U . . .
H4B H 0.126481 0.354767 0.583973 0.048 Uiso 1 1 calc R U . . .
C1 C 0.500000 0.34601(9) 0.750000 0.0371(4) Uani 1 2 d S T P . .
H1 H 0.499999 0.286791 0.749998 0.045 Uiso 1 2 calc R U P . .
N1 N 0.500000 0.70110(8) 0.750000 0.0434(4) Uani 1 2 d S T P . .
N2 N 0.28982(19) 0.65207(5) 0.65257(14) 0.0412(3) Uani 1 1 d . . . . .
N3 N 0.3696(2) 0.57301(5) 0.68964(15) 0.0450(3) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N4 0.0274(5) 0.0376(5) 0.0466(6) -0.0042(4) -0.0008(4) -0.0041(4)
C1 0.0334(8) 0.0302(7) 0.0467(9) 0.000 0.0106(7) 0.000
N1 0.0377(7) 0.0331(7) 0.0502(8) 0.000 -0.0004(6) 0.000
N2 0.0309(5) 0.0379(5) 0.0458(6) 0.0007(4) -0.0016(4) 0.0000(4)
N3 0.0397(6) 0.0350(5) 0.0523(6) -0.0028(4) 0.0023(4) -0.0045(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N4 H4A 120.0 . . ?
C1 N4 H4B 120.0 . . ?
H4A N4 H4B 120.0 . . ?
N4 C1 N4 124.76(14) 2_656 . ?
N4 C1 H1 117.6 2_656 . ?
N4 C1 H1 117.6 . . ?
N2 N1 N2 108.08(12) 2_656 . ?
N3 N2 N1 107.97(9) . . ?
N2 N3 N3 107.99(6) . 2_656 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N4 C1 1.2901(11) . ?
N4 H4A 0.8600 . ?
N4 H4B 0.8600 . ?
C1 H1 0.9300 . ?
N1 N2 1.3111(11) 2_656 ?
N1 N2 1.3111(12) . ?
N2 N3 1.3054(12) . ?
N3 N3 1.3161(19) 2_656 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N4 H4A N3 0.86 2.17 3.0061(12) 163.7 . yes
N4 H4B N2 0.86 2.23 3.0007(13) 149.2 5_566 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 N1 N2 N3 0.02(5) 2_656 . . . ?
N1 N2 N3 N3 -0.05(14) . . . 2_656 ?
