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#$Date: 2025-10-06 11:27:30 +0300 (Mon, 06 Oct 2025) $
#$Revision: 302575 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/25/06/7250683.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_7250683
loop_
_publ_author_name
'Chen, Lei'
'Shen, Zhili'
'Kong, Deren'
'Zhang, Chong'
'Hu, Bingcheng'
'Gao, Chao'
_publ_section_title
;
 Improving the anti-hygroscopicity and safety of hydroxylamine pentazolate
 salt (NH3OH+N5−) by cocrystallization
;
_journal_issue                   31
_journal_name_full               CrystEngComm
_journal_page_first              5312
_journal_page_last               5318
_journal_paper_doi               10.1039/D5CE00437C
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'H4 N O, N5'
_chemical_formula_sum            'H4 N6 O'
_chemical_formula_weight         104.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2025-04-08
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-04-23 deposited with the CCDC.	2025-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.582(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   3.7631(2)
_cell_length_b                   14.7655(7)
_cell_length_c                   7.6847(4)
_cell_measurement_reflns_used    2755
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      27.34
_cell_measurement_theta_min      3.00
_cell_volume                     424.18(4)
_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 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            10009
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.508
_diffrn_reflns_theta_min         2.759
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.144
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7048
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1189 before and 0.0600 after correction.
The Ratio of minimum to maximum transmission is 0.9453.
The λ/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_description       block
_exptl_crystal_F_000             216
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.158
_refine_diff_density_min         -0.195
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     70
_refine_ls_number_reflns         968
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0293
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0412P)²+0.0754P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0813
_reflns_Friedel_coverage         0.000
_reflns_number_gt                821
_reflns_number_total             968
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5ce00437c1.cif
_cod_data_source_block           mo_20250407_ys_nlg_qa_aeo_0m
_cod_depositor_comments
'Adding full bibliography for 7250682--7250683.cif.'
_cod_database_code               7250683
_shelx_shelxl_version_number     2018/3
_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_max   0.984
_shelx_estimated_absorpt_t_min   0.979
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups, All O(H) groups
2.a Rotating group:
 O1(H1), N6(H6A,H6B)
;
_shelx_res_file
;
TITL mo_20250407_ys_nlg_qa_aeo_0m_a.res in P2(1)/c
    mo_20250407_ys_nlg_qa_aeo_0m.res
    created by SHELXL-2018/3 at 15:37:36 on 08-Apr-2025
REM Old TITL mo_20250407_YS_NLG_QA_AEO_0m in P2(1)/c
REM SHELXT solution in P2(1)/c: R1 0.098, Rweak 0.006, Alpha 0.014
REM <I/s> 1.157 for 44 systematic absences, Orientation as input
REM Formula found by SHELXT: C6 N
CELL 0.71073 3.7631 14.7655 7.6847 90 96.582 90
ZERR 4 0.0002 0.0007 0.0004 0 0.002 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC H N O
UNIT 16 24 4

L.S. 4 0 0
PLAN  5
SIZE 0.11 0.14 0.15
TEMP -80.15
CONF
list 4
fmap 2 53
ACTA
MORE -1
BOND $H
REM <olex2.extras>
REM <HklSrc "%.\\mo_20250407_YS_NLG_QA_AEO_0m.hkl">
REM </olex2.extras>

WGHT    0.041200    0.075400
FVAR       2.12642
O1    3   -0.090610    0.601075    0.388398    11.00000    0.02676    0.04073 =
         0.02089   -0.00297   -0.00048   -0.00482
AFIX   7
H1    1    0.032908    0.611800    0.490780    11.00000   -1.20000
AFIX   0
N6    2    0.135696    0.608103    0.255189    11.00000    0.02375    0.02183 =
         0.02204   -0.00099   -0.00231    0.00112
AFIX   7
H6A   1    0.304988    0.566130    0.269507    11.00000   -1.20000
H6B   1    0.010872    0.600480    0.151197    11.00000   -1.20000
AFIX   0
N5    2    0.347782    0.705412    0.794262    11.00000    0.03745    0.02412 =
         0.02576    0.00073    0.00359    0.00460
N1    2    0.338794    0.632665    0.694619    11.00000    0.02885    0.02622 =
         0.02163    0.00066   -0.00012    0.00115
N2    2    0.521668    0.568468    0.782836    11.00000    0.03121    0.02222 =
         0.02677   -0.00078   -0.00344    0.00097
N4    2    0.535957    0.686473    0.944346    11.00000    0.04297    0.02672 =
         0.02271   -0.00274    0.00129   -0.00088
N3    2    0.643500    0.601864    0.937151    11.00000    0.03261    0.02504 =
         0.02475    0.00228   -0.00406   -0.00156
H6C   1    0.222308    0.667487    0.253518    11.00000    0.04141
HKLF 4




REM  mo_20250407_ys_nlg_qa_aeo_0m_a.res in P2(1)/c
REM wR2 = 0.0813, GooF = S = 1.077, Restrained GooF = 1.077 for all data
REM R1 = 0.0293 for 821 Fo > 4sig(Fo) and 0.0355 for all 968 data
REM 70 parameters refined using 0 restraints

END

WGHT      0.0412      0.0754

REM Highest difference peak  0.158,  deepest hole -0.195,  1-sigma level  0.043
Q1    1   0.4114  0.6202  0.5732  11.00000  0.05    0.16
Q2    1   0.2470  0.6260  0.6072  11.00000  0.05    0.15
Q3    1   0.8311  0.6010  1.0125  11.00000  0.05    0.15
Q4    1   0.6607  0.5752  1.0391  11.00000  0.05    0.13
Q5    1   0.5393  0.6419  0.9556  11.00000  0.05    0.12
;
_shelx_res_checksum              68032
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
O1 O -0.0906(2) 0.60107(6) 0.38840(10) 0.0297(2) Uani 1 1 d . . . . .
H1 H 0.032908 0.611800 0.490780 0.036 Uiso 1 1 d R U . . .
N6 N 0.1357(2) 0.60810(6) 0.25519(12) 0.0229(2) Uani 1 1 d . . . . .
H6A H 0.304988 0.566130 0.269507 0.028 Uiso 1 1 d R U . . .
H6B H 0.010872 0.600480 0.151197 0.028 Uiso 1 1 d R U . . .
N5 N 0.3478(3) 0.70541(6) 0.79426(13) 0.0291(2) Uani 1 1 d . . . . .
N1 N 0.3388(2) 0.63266(6) 0.69462(12) 0.0258(2) Uani 1 1 d . . . . .
N2 N 0.5217(2) 0.56847(6) 0.78284(12) 0.0273(2) Uani 1 1 d . . . . .
N4 N 0.5360(3) 0.68647(7) 0.94435(12) 0.0310(3) Uani 1 1 d . . . . .
N3 N 0.6435(3) 0.60186(6) 0.93715(13) 0.0280(2) Uani 1 1 d . . . . .
H6C H 0.222(4) 0.6675(11) 0.254(2) 0.041(4) Uiso 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
O1 0.0268(4) 0.0407(5) 0.0209(4) -0.0030(3) -0.0005(3) -0.0048(3)
N6 0.0238(5) 0.0218(5) 0.0220(5) -0.0010(4) -0.0023(3) 0.0011(3)
N5 0.0375(5) 0.0241(5) 0.0258(5) 0.0007(4) 0.0036(4) 0.0046(4)
N1 0.0288(5) 0.0262(5) 0.0216(5) 0.0007(4) -0.0001(4) 0.0012(4)
N2 0.0312(5) 0.0222(5) 0.0268(5) -0.0008(4) -0.0034(4) 0.0010(4)
N4 0.0430(6) 0.0267(5) 0.0227(5) -0.0027(4) 0.0013(4) -0.0009(4)
N3 0.0326(5) 0.0250(5) 0.0247(5) 0.0023(4) -0.0041(4) -0.0016(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
O O 0.0106 0.0060 '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
N6 O1 H1 109.6 . . ?
O1 N6 H6A 110.1 . . ?
O1 N6 H6B 110.1 . . ?
O1 N6 H6C 108.6(10) . . ?
H6A N6 H6B 108.8 . . ?
H6A N6 H6C 114.2 . . ?
H6B N6 H6C 104.8 . . ?
N4 N5 N1 108.20(9) . . ?
N2 N1 N5 108.15(9) . . ?
N1 N2 N3 107.59(9) . . ?
N5 N4 N3 107.63(9) . . ?
N4 N3 N2 108.43(9) . . ?
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
O1 H1 0.8811 . ?
O1 N6 1.4085(12) . ?
N6 H6A 0.8866 . ?
N6 H6B 0.8865 . ?
N6 H6C 0.936(16) . ?
N5 N1 1.3173(13) . ?
N5 N4 1.3125(14) . ?
N1 N2 1.3133(13) . ?
N2 N3 1.3172(13) . ?
N4 N3 1.3163(14) . ?
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
N5 N1 N2 N3 -0.01(12) . . . . ?
N5 N4 N3 N2 -0.06(13) . . . . ?
N1 N5 N4 N3 0.05(13) . . . . ?
N1 N2 N3 N4 0.05(12) . . . . ?
N4 N5 N1 N2 -0.02(12) . . . . ?
