#------------------------------------------------------------------------------
#$Date: 2019-11-24 16:03:40 +0200 (Sun, 24 Nov 2019) $
#$Revision: 238465 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/76/7237644.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_7237644
loop_
_publ_author_name
'Xu, Yuangang'
'Tian, Lili'
'Li, Dongxue'
'Wang, Pengcheng'
'Lu, Ming'
_publ_section_title
;
 A series of energetic cyclo-pentazolate salts: rapid synthesis,
 characterization, and promising performance
;
_journal_issue                   20
_journal_name_full               'Journal of Materials Chemistry A'
_journal_page_first              12468
_journal_paper_doi               10.1039/C9TA01077G
_journal_volume                  7
_journal_year                    2019
_chemical_formula_moiety         'H4 N, N5'
_chemical_formula_sum            'H4 N6'
_chemical_formula_weight         88.09
_space_group_crystal_system      orthorhombic
_space_group_IT_number           54
_space_group_name_Hall           '-P 2a 2ac'
_space_group_name_H-M_alt        'P c c a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-23 deposited with the CCDC.	2019-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.399(4)
_cell_length_b                   3.9543(19)
_cell_length_c                   10.362(5)
_cell_measurement_reflns_used    343
_cell_measurement_temperature    150
_cell_measurement_theta_max      24.10
_cell_measurement_theta_min      3.93
_cell_volume                     385.1(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0746
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            1871
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.280
_diffrn_reflns_theta_min         3.933
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.125
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5253
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0710 before and 0.0246 after correction. The Ratio of minimum to maximum transmission is 0.7047. The λ/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_description       block
_exptl_crystal_F_000             184
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.223
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     37
_refine_ls_number_reflns         392
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0497
_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)+(0.0912P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1243
_refine_ls_wR_factor_ref         0.1354
_reflns_Friedel_coverage         0.000
_reflns_number_gt                322
_reflns_number_total             392
_reflns_threshold_expression     'I > 2σ(I)'
_iucr_refine_instructions_details
;
TITL 327_a.res in Pcca
    327.res
    created by SHELXL-2018/3 at 15:23:17 on 23-Dec-2018
REM Old TITL 327 in Pcca #54
REM SHELXT solution in Pcca
REM R1 0.171, Rweak 0.001, Alpha 0.008, Orientation as input
REM Formula found by SHELXT: N O
CELL 0.71073 9.3994 3.9543 10.3615 90 90 90
ZERR 4 0.0043 0.0019 0.0048 0 0 0
LATT 1
SYMM 0.5-X,-Y,+Z
SYMM -X,+Y,0.5-Z
SYMM 0.5+X,-Y,0.5-Z
SFAC H N
UNIT 16 24
SADI N4 H4a N4 H4b

L.S. 4 0 31
PLAN  20
SIZE 0.19 0.12 0.08
TEMP -123.15
BOND $H
list 4
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\327.hkl">
REM </olex2.extras>

WGHT    0.091200
FVAR       1.25319
N4    2    0.500000    0.054682    0.250000    10.50000    0.03110    0.04098 =
         0.02059    0.00000   -0.00158    0.00000
N3    2    0.308273    0.407873    0.432180    11.00000    0.03768    0.05464 =
         0.02277    0.00009    0.00076    0.00459
N2    2    0.344004    0.351527    0.553112    11.00000    0.04202    0.05783 =
         0.02706    0.00666   -0.00440   -0.00069
N1    2    0.250000    0.500000    0.627175    10.50000    0.04849    0.06376 =
         0.02226    0.00000    0.00000   -0.01078
H4A   1    0.563487    0.177788    0.210909    11.00000    0.05804
H4B   1    0.455692   -0.070134    0.193043    11.00000    0.03895
HKLF 4




REM  327_a.res in Pcca
REM wR2 = 0.1354, GooF = S = 1.072, Restrained GooF = 1.071 for all data
REM R1 = 0.0497 for 322 Fo > 4sig(Fo) and 0.0587 for all 392 data
REM 37 parameters refined using 1 restraints

END  
     
WGHT      0.0723      0.0000 

REM Highest difference peak  0.342,  deepest hole -0.223,  1-sigma level  0.075
Q1    1   0.4273  0.1591  0.5621  11.00000  0.05    0.34
Q2    1   0.4971  0.0098  0.0611  11.00000  0.05    0.30
Q3    1   0.4030  0.1613  0.4402  11.00000  0.05    0.22
Q4    1   0.2500  0.5000  0.4319  10.50000  0.05    0.20
Q5    1   0.2049  0.2711  0.4254  11.00000  0.05    0.18
Q6    1   0.4149  0.6328  0.5623  11.00000  0.05    0.16
Q7    1   0.2500  0.5000  0.5608  10.50000  0.05    0.14
Q8    1   0.3288 -0.0620  0.4379  11.00000  0.05    0.13
Q9    1   0.4506  0.6483  0.4401  11.00000  0.05    0.13
Q10   1   0.4081  0.5687  0.4489  11.00000  0.05    0.12
Q11   1   0.1947  0.4549  0.7547  11.00000  0.05    0.12
Q12   1   0.1918  0.2544  0.5851  11.00000  0.05    0.11
Q13   1   0.4289 -0.1282  0.2548  11.00000  0.05    0.10
Q14   1   0.3186  0.3489  0.5818  11.00000  0.05    0.09
Q15   1   0.1777  0.6268  0.7424  11.00000  0.05    0.08
Q16   1   0.4034  0.1297  0.1129  11.00000  0.05    0.07
Q17   1   0.2500  0.0000  0.5696  10.50000  0.05    0.06
Q18   1   0.5000  0.5398  0.2500  10.50000  0.05    0.02

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0497 for 322 Fo > 4sig(Fo) and 0.0587 for all 2193 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.34, deepest hole -0.22
  REM Mean Shift 0, Max Shift -0.001.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0587
  REM R1_gt = 0.0497
  REM wR_ref = 0.1354
  REM GOOF = 1.072
  REM Shift_max = -0.001
  REM Shift_mean = 0
  REM Reflections_all = 2193
  REM Reflections_gt = 322
  REM Parameters = n/a
  REM Hole = -0.22
  REM Peak = 0.34
  REM Flack = n/a

  
;
_cod_data_source_file            c9ta01077g2.cif
_cod_data_source_block           327
_cod_database_code               7237644
_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   0.990
_shelx_estimated_absorpt_t_min   0.977
_olex2_refinement_description
;
1. Restrained distances
 N4-H4A \\sim N4-H4B
 with sigma of 0.02
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x, -y, z-1/2'
'-x-1/2, y, 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
N4 N 0.500000 0.0547(5) 0.250000 0.0309(6) Uani 1 2 d DS T P
N3 N 0.30827(15) 0.4079(4) 0.43218(14) 0.0384(6) Uani 1 1 d . . .
N2 N 0.34400(17) 0.3515(5) 0.55311(16) 0.0423(6) Uani 1 1 d . . .
N1 N 0.250000 0.500000 0.62718(19) 0.0448(8) Uani 1 2 d S T P
H4A H 0.563(2) 0.178(5) 0.211(2) 0.058(7) Uiso 1 1 d D . .
H4B H 0.456(2) -0.070(5) 0.1930(19) 0.039(5) Uiso 1 1 d 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 0.0311(13) 0.0410(13) 0.0206(10) 0.000 -0.0016(8) 0.000
N3 0.0377(10) 0.0546(11) 0.0228(9) 0.0001(6) 0.0008(6) 0.0046(7)
N2 0.0420(11) 0.0578(12) 0.0271(9) 0.0067(7) -0.0044(6) -0.0007(8)
N1 0.0485(15) 0.0638(15) 0.0223(12) 0.000 0.000 -0.0108(12)
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'
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
H4A N4 H4A 112(3) . 3_655
H4A N4 H4B 109(2) 3_655 3_655
H4A N4 H4B 108(2) . 3_655
H4A N4 H4B 109(2) . .
H4B N4 H4A 108(2) . 3_655
H4B N4 H4B 111(3) . 3_655
N3 N3 N2 107.83(10) 2_565 .
N1 N2 N3 108.05(15) . .
N2 N1 N2 108.2(2) 2_565 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N4 H4A 0.870(16) .
N4 H4A 0.870(16) 3_655
N4 H4B 0.875(15) .
N4 H4B 0.875(15) 3_655
N3 N3 1.316(3) 2_565
N3 N2 1.316(2) .
N2 N1 1.309(2) .
