#------------------------------------------------------------------------------
#$Date: 2019-11-24 16:03:40 +0200 (Sun, 24 Nov 2019) $
#$Revision: 238465 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/76/7237642.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_7237642
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         'H5 N2, N5'
_chemical_formula_sum            'H5 N7'
_chemical_formula_weight         103.11
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-04 deposited with the CCDC.	2019-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.766(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.4527(16)
_cell_length_b                   12.247(3)
_cell_length_c                   5.4073(14)
_cell_measurement_reflns_used    784
_cell_measurement_temperature    150
_cell_measurement_theta_max      25.732
_cell_measurement_theta_min      3.186
_cell_volume                     423.40(18)
_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      150.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.993
_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  0.0444
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            3281
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.669
_diffrn_reflns_theta_min         3.186
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.133
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6572
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1062 before and 0.0565 after correction. The Ratio of minimum to maximum transmission is 0.8817. The λ/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_description       block
_exptl_crystal_F_000             216
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.209
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     73
_refine_ls_number_reflns         890
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0406
_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)+(0.0501P)²+0.0059P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.1008
_reflns_Friedel_coverage         0.000
_reflns_number_gt                745
_reflns_number_total             890
_reflns_threshold_expression     'I > 2σ(I)'
_iucr_refine_instructions_details
;

    mo_20181166-nlgx-300_0m.res created by SHELXL-2014/7

TITL mo_20181166-nlgx-300_0m_a.res in P2(1)/c
REM Old TITL mo_20181166-NLGX-300_0m in P21/a #14
REM SHELXT solution in P2(1)/c
REM R1 0.095, Rweak 0.009, Alpha 0.009, Orientation a'=c, b'=-b, c'=a
REM Formula found by SHELXT: C7
CELL 0.71073 6.4527 12.2471 5.4073 90 97.766 90
ZERR 4 0.0016 0.0031 0.0014 0 0.006 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC H N
UNIT 20 28
 
L.S. 10
PLAN  20
SIZE 0.19 0.12 0.08
TEMP -123.15
BOND $H
list 4
fmap 2
acta
OMIT 1 1 0
OMIT 0 2 0
REM <olex2.extras>
REM <HklSrc "%.\\mo_20181166-NLGX-300_0m.hkl">
REM </olex2.extras>
 
WGHT    0.050100    0.005900
FVAR       1.19978
N2    2    0.095204    0.659727    0.115492    11.00000    0.01370    0.02121 =
         0.01245    0.00121    0.00415    0.00034
N3    2    0.555381    0.608755    0.337867    11.00000    0.01589    0.01823 =
         0.01765    0.00136    0.00125    0.00149
N1    2    0.228244    0.646145   -0.077890    11.00000    0.01504    0.01840 =
         0.01170   -0.00219    0.00198   -0.00076
AFIX 137
H1A   1    0.205807    0.702079   -0.189063    11.00000   -1.20000
H1B   1    0.197815    0.581647   -0.158213    11.00000   -1.20000
H1C   1    0.364642    0.646179   -0.007809    11.00000   -1.20000
AFIX   0
N4    2    0.530868    0.659933    0.547640    11.00000    0.01801    0.02073 =
         0.01790   -0.00085    0.00281    0.00381
N7    2    0.735884    0.557306    0.370988    11.00000    0.01544    0.02059 =
         0.01885   -0.00232    0.00315    0.00103
N6    2    0.824170    0.575829    0.603471    11.00000    0.01741    0.02617 =
         0.01961   -0.00434   -0.00220    0.00368
N5    2    0.698002    0.639412    0.712176    11.00000    0.02170    0.02560 =
         0.01833   -0.00411   -0.00107    0.00510
H2A   1    0.110282    0.599237    0.207221    11.00000    0.03043
H2B   1   -0.028288    0.660306    0.042323    11.00000    0.02790
HKLF 4
 
REM  mo_20181166-nlgx-300_0m_a.res in P2(1)/c
REM R1 =  0.0406 for     745 Fo > 4sig(Fo)  and  0.0490 for all     890 data
REM     73 parameters refined using      0 restraints
 
END  
     
WGHT      0.0501      0.0059 

REM Highest difference peak  0.209,  deepest hole -0.281,  1-sigma level  0.070
Q1    1   0.9589  0.6816  0.6687  11.00000  0.05    0.21
Q2    1   0.6999  0.4641  0.5366  11.00000  0.05    0.19
Q3    1   0.5676  0.6864  0.2212  11.00000  0.05    0.18
Q4    1   0.4082  0.6584  0.2383  11.00000  0.05    0.18
Q5    1   0.7541  0.5586  0.9564  11.00000  0.05    0.17
Q6    1   0.0788  0.6980 -0.1977  11.00000  0.05    0.17
Q7    1   0.9418  0.5016  0.7191  11.00000  0.05    0.17
Q8    1   0.4752  0.7051  0.0940  11.00000  0.05    0.17
Q9    1   0.1050  0.7229 -0.4383  11.00000  0.05    0.16
Q10   1   0.4190  0.7078  0.5003  11.00000  0.05    0.16
Q11   1   0.7499  0.5481  0.1714  11.00000  0.05    0.16
Q12   1  -0.0901  0.5905 -0.0003  11.00000  0.05    0.16
Q13   1   0.1847  0.7134  0.1618  11.00000  0.05    0.16
Q14   1   0.3283  0.5778  0.3800  11.00000  0.05    0.15
Q15   1  -0.0712  0.5461  0.1540  11.00000  0.05    0.15
Q16   1   0.8477  0.7167  0.7182  11.00000  0.05    0.15
Q17   1   0.1095  0.5410  0.4215  11.00000  0.05    0.15
Q18   1   0.0044  0.5792  0.2349  11.00000  0.05    0.15
Q19   1   0.0859  0.4834  0.0382  11.00000  0.05    0.14
Q20   1   0.5667  0.5314  0.7992  11.00000  0.05    0.14

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0406 for 745 Fo > 4sig(Fo) and 0.0490 for all 3404 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.21, deepest hole -0.28
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0490
  REM R1_gt = 0.0406
  REM wR_ref = 0.1008
  REM GOOF = 1.116
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 3404
  REM Reflections_gt = 745
  REM Parameters = n/a
  REM Hole = -0.28
  REM Peak = 0.21
  REM Flack = n/a

  
;
_cod_data_source_file            c9ta01077g2.cif
_cod_data_source_block           mo_20181166-nlgx-300_0m
_cod_original_cell_volume        423.40(19)
_cod_database_code               7237642
_shelx_shelxl_version_number     2014/7
_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   0.989
_shelx_estimated_absorpt_t_min   0.975
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H) groups
2.a Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_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
N2 N 0.0952(2) 0.65973(11) 0.1155(3) 0.0156(3) Uani 1 1 d .
N3 N 0.55538(19) 0.60876(10) 0.3379(2) 0.0173(3) Uani 1 1 d .
N1 N 0.22824(18) 0.64614(10) -0.0779(2) 0.0150(3) Uani 1 1 d .
H1A H 0.2058 0.7021 -0.1891 0.018 Uiso 1 1 calc GR
H1B H 0.1978 0.5816 -0.1582 0.018 Uiso 1 1 calc GR
H1C H 0.3646 0.6462 -0.0078 0.018 Uiso 1 1 calc GR
N4 N 0.53087(19) 0.65993(11) 0.5476(2) 0.0188(4) Uani 1 1 d .
N7 N 0.73588(18) 0.55731(11) 0.3710(2) 0.0182(3) Uani 1 1 d .
N6 N 0.82417(19) 0.57583(11) 0.6035(3) 0.0215(4) Uani 1 1 d .
N5 N 0.6980(2) 0.63941(11) 0.7122(3) 0.0222(4) Uani 1 1 d .
H2A H 0.110(3) 0.5992(17) 0.207(4) 0.030(5) Uiso 1 1 d .
H2B H -0.028(3) 0.6603(14) 0.042(4) 0.028(5) 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
N2 0.0137(7) 0.0212(7) 0.0125(7) 0.0012(5) 0.0041(5) 0.0003(5)
N3 0.0159(6) 0.0182(7) 0.0176(7) 0.0014(5) 0.0013(5) 0.0015(5)
N1 0.0150(6) 0.0184(7) 0.0117(7) -0.0022(5) 0.0020(5) -0.0008(5)
N4 0.0180(7) 0.0207(7) 0.0179(8) -0.0009(6) 0.0028(5) 0.0038(5)
N7 0.0154(6) 0.0206(7) 0.0189(8) -0.0023(5) 0.0031(5) 0.0010(5)
N6 0.0174(6) 0.0262(8) 0.0196(8) -0.0043(6) -0.0022(5) 0.0037(6)
N5 0.0217(7) 0.0256(8) 0.0183(8) -0.0041(6) -0.0011(5) 0.0051(6)
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
N1 N2 H2A 106.0(12)
N1 N2 H2B 106.1(13)
H2A N2 H2B 107.1(17)
N7 N3 N4 108.44(12)
N2 N1 H1A 109.5
N2 N1 H1B 109.5
N2 N1 H1C 109.5
H1A N1 H1B 109.5
H1A N1 H1C 109.5
H1B N1 H1C 109.5
N3 N4 N5 107.73(12)
N3 N7 N6 107.81(12)
N5 N6 N7 108.10(12)
N6 N5 N4 107.91(13)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
N2 N1 1.4494(17)
N2 H2A 0.89(2)
N2 H2B 0.84(2)
N3 N4 1.3240(18)
N3 N7 1.3150(17)
N1 H1A 0.9100
N1 H1B 0.9100
N1 H1C 0.9100
N4 N5 1.3261(18)
N7 N6 1.3277(19)
N6 N5 1.3206(19)
