#------------------------------------------------------------------------------
#$Date: 2017-05-18 05:24:41 +0300 (Thu, 18 May 2017) $
#$Revision: 196724 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/29/7042961.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_7042961
loop_
_publ_author_name
'Ma, Qing'
'Chen, Ya'
'Liao, Longyu'
'Lu, Huanchang'
'Fan, Guijuan'
'Huang, Jinglun'
_publ_section_title
;
 Energetic π-conjugated vinyl bridged triazoles: a thermally stable and
 insensitive heterocyclic cation
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01261F
_journal_year                    2017
_chemical_formula_moiety         'C6 H12 N10, 2(Cl O4)'
_chemical_formula_sum            'C6 H12 Cl2 N10 O8'
_chemical_formula_weight         423.16
_space_group_crystal_system      tetragonal
_space_group_IT_number           142
_space_group_name_Hall           '-I 4bd 2c'
_space_group_name_H-M_alt        'I 41/a c d'
_symmetry_space_group_name_Hall  '-I 4bd 2c'
_symmetry_space_group_name_H-M   'I 41/a c d :2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2016-11-02
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2016-12-28 deposited with the CCDC.
2017-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   12.2856(7)
_cell_length_b                   12.2856(7)
_cell_length_c                   40.490(4)
_cell_measurement_reflns_used    5027
_cell_measurement_temperature    130
_cell_measurement_theta_max      30.358
_cell_measurement_theta_min      2.55
_cell_volume                     6111.4(8)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      130
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            28870
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.660
_diffrn_reflns_theta_min         2.012
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.494
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6882
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0516 before and 0.0464 after correction.
The Ratio of minimum to maximum transmission is 0.9224.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.840
_exptl_crystal_description       block
_exptl_crystal_F_000             3456
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         2368
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0338
_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)+(0.0462P)²+7.1737P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0923
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1920
_reflns_number_total             2368
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt01261f2.cif
_cod_data_source_block           dm16712
_cod_original_cell_volume        6111.4(9)
_cod_database_code               7042961
_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   0.943
_shelx_estimated_absorpt_t_min   0.908
_olex2_refinement_description
;
;
_shelx_shelxl_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+1/4, x+3/4, z+1/4'
'-x, -y+1/2, z'
'y+1/4, -x+1/4, z+3/4'
'x, -y, -z+1/2'
'-x+1/2, y, -z'
'y+3/4, x+1/4, -z+1/4'
'-y+1/4, -x+1/4, -z+1/4'
'x+1/2, y+1/2, z+1/2'
'-y+3/4, x+5/4, z+3/4'
'-x+1/2, -y+1, z+1/2'
'y+3/4, -x+3/4, z+5/4'
'x+1/2, -y+1/2, -z+1'
'-x+1, y+1/2, -z+1/2'
'y+5/4, x+3/4, -z+3/4'
'-y+3/4, -x+3/4, -z+3/4'
'-x, -y, -z'
'y-1/4, -x-3/4, -z-1/4'
'x, y-1/2, -z'
'-y-1/4, x-1/4, -z-3/4'
'-x, y, z-1/2'
'x-1/2, -y, z'
'-y-3/4, -x-1/4, z-1/4'
'y-1/4, x-1/4, z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/4, -x-1/4, -z+1/4'
'x+1/2, y, -z+1/2'
'-y+1/4, x+1/4, -z-1/4'
'-x+1/2, y+1/2, z'
'x, -y+1/2, z+1/2'
'-y-1/4, -x+1/4, z+1/4'
'y+1/4, x+1/4, z+1/4'
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
N1 N -0.12818(10) 0.70822(10) 0.08843(3) 0.0128(2) Uani 1 1 d
H1 H -0.0824(18) 0.6654(18) 0.0940(5) 0.028(6) Uiso 1 1 d
N2 N -0.18611(10) 0.76460(10) 0.11232(3) 0.0138(2) Uani 1 1 d
N3 N -0.24937(10) 0.79883(10) 0.06229(3) 0.0112(2) Uani 1 1 d
N4 N -0.31164(10) 0.83496(10) 0.03549(3) 0.0132(2) Uani 1 1 d
H4A H -0.2942(16) 0.9037(17) 0.0310(5) 0.023(5) Uiso 1 1 d
H4B H -0.3812(19) 0.8268(17) 0.0405(5) 0.028(6) Uiso 1 1 d
N5 N -0.13132(12) 0.69309(12) 0.02927(3) 0.0174(3) Uani 1 1 d
H5A H -0.1545(18) 0.7225(18) 0.0121(5) 0.031(6) Uiso 1 1 d
H5B H -0.0864(19) 0.6451(19) 0.0289(6) 0.032(6) Uiso 1 1 d
C1 C -0.16618(11) 0.72847(11) 0.05814(3) 0.0118(3) Uani 1 1 d
C2 C -0.25878(12) 0.81989(11) 0.09588(3) 0.0124(3) Uani 1 1 d
C3 C -0.33911(12) 0.89544(12) 0.10888(3) 0.0139(3) Uani 1 1 d
H3 H -0.3794(17) 0.9371(17) 0.0932(5) 0.021(5) Uiso 1 1 d
Cl1 Cl 0.09442(3) 0.46682(3) 0.04750(2) 0.01536(10) Uani 1 1 d
O1 O 0.01164(11) 0.53892(10) 0.06025(3) 0.0253(3) Uani 1 1 d
O2 O 0.12943(13) 0.50754(13) 0.01602(3) 0.0371(4) Uani 1 1 d
O3 O 0.04920(10) 0.35946(10) 0.04353(4) 0.0299(3) Uani 1 1 d
O4 O 0.18461(11) 0.46301(11) 0.06991(4) 0.0339(3) Uani 1 1 d
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'
Cl Cl 0.1484 0.1585 '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
N2 N1 H1 119.5(16) .
C1 N1 H1 128.6(16) .
C1 N1 N2 111.61(12) .
C2 N2 N1 104.79(12) .
C1 N3 N4 121.38(11) .
C1 N3 C2 107.72(11) .
C2 N3 N4 130.86(12) .
N3 N4 H4A 109.2(13) .
N3 N4 H4B 108.3(14) .
H4A N4 H4B 112.8(18) .
H5A N5 H5B 122(2) .
C1 N5 H5A 119.0(15) .
C1 N5 H5B 118.6(17) .
N1 C1 N3 105.65(12) .
N5 C1 N1 129.73(14) .
N5 C1 N3 124.59(13) .
N2 C2 N3 110.23(12) .
N2 C2 C3 127.74(13) .
N3 C2 C3 122.02(12) .
C2 C3 H3 117.0(12) .
C3 C3 C2 122.86(17) 7_365
C3 C3 H3 120.1(12) 7_365
O2 Cl1 O1 108.34(9) .
O2 Cl1 O3 109.62(9) .
O3 Cl1 O1 109.27(8) .
O4 Cl1 O1 109.77(8) .
O4 Cl1 O2 110.00(9) .
O4 Cl1 O3 109.82(8) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N1 H1 0.80(2) .
N1 N2 1.3864(16) .
N1 C1 1.3359(18) .
N2 C2 1.3047(18) .
N3 N4 1.3998(16) .
N3 C1 1.3491(18) .
N3 C2 1.3892(17) .
N4 H4A 0.89(2) .
N4 H4B 0.88(2) .
N5 H5A 0.83(2) .
N5 H5B 0.81(2) .
N5 C1 1.3184(18) .
C2 C3 1.4536(19) .
C3 C3 1.332(3) 7_365
C3 H3 0.95(2) .
Cl1 O1 1.4441(12) .
Cl1 O2 1.4350(13) .
Cl1 O3 1.4402(12) .
Cl1 O4 1.4329(13) .
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_4
N1 N2 C2 N3 0.83(15) .
N1 N2 C2 C3 -178.10(14) .
N2 N1 C1 N3 0.15(16) .
N2 N1 C1 N5 177.96(15) .
N2 C2 C3 C3 -6.08(19) 7_365
N3 C2 C3 C3 175.10(9) 7_365
N4 N3 C1 N1 -177.52(12) .
N4 N3 C1 N5 4.5(2) .
N4 N3 C2 N2 176.82(13) .
N4 N3 C2 C3 -4.2(2) .
C1 N1 N2 C2 -0.63(16) .
C1 N3 C2 N2 -0.78(16) .
C1 N3 C2 C3 178.23(13) .
C2 N3 C1 N1 0.36(15) .
C2 N3 C1 N5 -177.59(14) .
