#------------------------------------------------------------------------------
#$Date: 2024-08-05 21:29:33 +0300 (Mon, 05 Aug 2024) $
#$Revision: 293801 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/89/7248937.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_7248937
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, C4 H9 N2'
_chemical_formula_sum            'C4 H9 N7'
_chemical_formula_weight         155.163
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_Int_Tables_number      11
_audit_creation_date             2024-04-29
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-04-29 deposited with the CCDC.	2024-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.937(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.0037(15)
_cell_length_b                   7.0175(15)
_cell_length_c                   7.7191(16)
_cell_measurement_reflns_used    1649
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      24.69
_cell_measurement_theta_min      2.93
_cell_volume                     376.60(14)
_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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.9932
_diffrn_measured_fraction_theta_max 0.9932
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1434
_diffrn_reflns_av_unetI/netI     0.0714
_diffrn_reflns_Laue_measured_fraction_full 0.9932
_diffrn_reflns_Laue_measured_fraction_max 0.9932
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_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            5041
_diffrn_reflns_point_group_measured_fraction_full 0.9932
_diffrn_reflns_point_group_measured_fraction_max 0.9932
_diffrn_reflns_theta_full        25.0612
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         2.66
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_description       block
_exptl_crystal_F_000             164.119
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.3529
_refine_diff_density_min         -0.3679
_refine_diff_density_rms         0.0911
_refine_ls_d_res_high            0.8389
_refine_ls_d_res_low             7.6626
_refine_ls_goodness_of_fit_ref   1.0564
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     87
_refine_ls_number_reflns         727
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.0556
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0580
_refine_ls_shift/su_max          -0.0008
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0536P)²+0.2293P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1406
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              8
_reflns_limit_h_min              -8
_reflns_limit_k_max              8
_reflns_limit_k_min              0
_reflns_limit_l_max              9
_reflns_limit_l_min              0
_reflns_number_gt                534
_reflns_number_total             727
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4ce00521j2.cif
_cod_data_source_block           1_CCDC4
_cod_depositor_comments
'Adding full bibliography for 7248931--7248937.cif.'
_cod_database_code               7248937
_olex2_refinement_description
;
1. Restrained distances
 N6-H6b
 0.88 with sigma of 0.01
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y+1/2,-z
3 -x,-y,-z
4 x,-y-1/2,z
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_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
N1 N 0.4481(4) 0.25 0.7729(5) 0.0495(9) Uani 1.000000 2 S T P
N2 N 0.5808(5) 0.25 0.9079(4) 0.0483(9) Uani 1.000000 2 S T P
N3 N 0.7484(4) 0.25 0.8511(4) 0.0437(9) Uani 1.000000 2 S T P
N4 N 0.7229(5) 0.25 0.6811(4) 0.0493(9) Uani 1.000000 2 S T P
N5 N 0.5366(5) 0.25 0.6323(4) 0.0490(9) Uani 1.000000 2 S T P
H7a H 0.234(5) 0.25 -0.062(5) 0.046(10) Uiso 1.000000 2 S T P
N6 N 0.3977(4) 0.25 0.2465(4) 0.0410(9) Uani 1.000000 2 DS T P
N7 N 0.1486(5) 0.25 0.0282(4) 0.0361(8) Uani 1.000000 2 S T P
H7b H 0.030(6) 0.25 0.006(5) 0.034(11) Uiso 1.000000 2 S T P
C1 C 0.2124(5) 0.25 0.1959(4) 0.0279(8) Uani 1.000000 2 S T P
C2 C 0.0808(5) 0.25 0.3279(5) 0.0339(9) Uani 1.000000 2 S T P
H2 H 0.139(5) 0.25 0.435(5) 0.038(10) Uiso 1.000000 2 S T P
C3 C -0.1081(4) 0.1455(4) 0.2966(4) 0.0390(7) Uani 1.000000 1 . . .
H3a H -0.155(3) 0.083(4) 0.399(3) 0.043(7) Uiso 1.000000 1 . . .
H3b H -0.125(3) 0.075(4) 0.189(4) 0.049(8) Uiso 1.000000 1 . . .
H6a H 0.481(5) 0.25 0.164(5) 0.044(11) Uiso 1.000000 2 S T P
H6b H 0.438(5) 0.25 0.3584(17) 0.061(13) Uiso 1.000000 2 DS T P
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
C 0.00313 0.00162 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.21560 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.00304 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
N 0.00612 0.00332 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.52900 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
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
N5 N1 N2 107.3(3) . . ?
N3 N2 N1 108.3(3) . . ?
N4 N3 N2 108.6(3) . . ?
N5 N4 N3 107.4(3) . . ?
N4 N5 N1 108.3(3) . . ?
H6a N6 C1 119(2) . . ?
H6b N6 C1 119(3) . . ?
H6b N6 H6a 122(4) . . ?
H7b N7 H7a 123(3) . . ?
C1 N7 H7a 123(2) . . ?
C1 N7 H7b 115(3) . . ?
N7 C1 N6 120.0(3) . . ?
C2 C1 N6 118.7(3) . . ?
C2 C1 N7 121.3(3) . . ?
H2 C2 C1 114(2) . . ?
C3 C2 C1 120.4(3) . . ?
C3 C2 C1 120.4(3) 4_565 . ?
C3 C2 H2 116.8(19) . . ?
C3 C2 H2 116.8(19) 4_565 . ?
C3 C2 C3 58.3(2) 4_565 . ?
C3 C3 C2 60.86(12) 4_565 . ?
H3a C3 C2 117.1(14) . . ?
H3b C3 C2 113.7(15) . . ?
H3b C3 H3a 116(2) . . ?
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
N1 N2 1.310(4) . ?
N1 N5 1.313(4) . ?
N2 N3 1.302(4) . ?
N3 N4 1.303(4) . ?
N4 N5 1.314(4) . ?
H7a N7 0.97(4) . ?
N6 C1 1.309(4) . ?
N6 H6a 0.92(4) . ?
N6 H6b 0.876(10) . ?
N7 H7b 0.83(4) . ?
N7 C1 1.317(4) . ?
C1 C2 1.454(5) . ?
C2 H2 0.88(4) . ?
C2 C3 1.507(4) 4_565 ?
C2 C3 1.507(4) . ?
C3 C3 1.467(6) 4_565 ?
C3 H3a 1.00(3) . ?
C3 H3b 0.96(3) . ?
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
N1 N2 N3 N4 -0.0 . . . . ?
N1 N5 N4 N3 -0.0 . . . . ?
N2 N3 N4 N5 0.0 . . . . ?
N6 C1 C2 C3 -145.62(13) . . . . ?
N6 C1 C2 C3 145.62(13) . . . 4_565 ?
N7 C1 C2 C3 34.38(13) . . . . ?
N7 C1 C2 C3 -34.38(13) . . . 4_565 ?
C1 C2 C3 C3 -109.1(2) . . . 4_565 ?
C1 C2 C3 C3 109.1(2) . . 4_565 . ?
loop_
_restr_distance_atom_site_label_1
_restr_distance_atom_site_label_2
_restr_distance_site_symmetry_2
_restr_distance_target
_restr_distance_target_weight_param
_restr_distance_diff
N6 H6b 1 0.8800 0.0100 0.0037
