Energetic π-conjugated vinyl bridged triazoles: a thermally stable and insensitive heterocyclic cation
Ma, Qing; Chen, Ya; Liao, Longyu; Lu, Huanchang; Fan, Guijuan; Huang, Jinglun; Dalton Trans.  (2017) –; doi:10.1039/C7DT01261F

data_7042965
_publ_section_title
;
 Energetic \p-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         '2(C6 H2 N3 O9), C6 H12 N10'
_chemical_formula_sum            'C18 H16 N16 O18'
_chemical_formula_weight         744.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2016-10-25
_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                 101.493(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.2505(7)
_cell_length_b                   5.1854(3)
_cell_length_c                   23.7693(12)
_cell_measurement_reflns_used    540
_cell_measurement_temperature    296
_cell_measurement_theta_max      52.76
_cell_measurement_theta_min      7.61
_cell_volume                     1358.86(14)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            5230
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        65.988
_diffrn_reflns_theta_max         65.988
_diffrn_reflns_theta_min         4.080
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.452
_exptl_absorpt_correction_T_max  0.7527
_exptl_absorpt_correction_T_min  0.6183
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0892 before and 0.0433 after correction.
The Ratio of minimum to maximum transmission is 0.8214.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.819
_exptl_crystal_description       prism
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.933
_refine_diff_density_min         -0.848
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         2292
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.1256
_refine_ls_R_factor_gt           0.0846
_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/[\s^2^(Fo^2^)+(0.1532P)^2^+2.0226P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2307
_refine_ls_wR_factor_ref         0.2706
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1433
_reflns_number_total             2292
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01261f2.cif
_cod_data_source_block           cu_dm16685_0m
_cod_database_code               7042965
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.868
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H) groups
2. Uiso/Uaniso restraints and constraints
O8 \\sim O9 \\sim N3: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(O9) \\sim Ueq, Uanis(O8) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
3.a Tetrahedral OH refined with riding coordinates:
 O1(H1)
;
_shelx_res_checksum              80731
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'