Superior thermally robust energetic materials featuring Z-E isomeric bis(3,4-diamino-1,2,4-triazol-5-yl)-1H-pyrazole: self-assembly nitrogen-rich tubes and templates with Hofmeister anions capture architecture
Geng, Wenjing; Jia, Yunfei; Chen, Ya; Ma, Qing; Fan, Guijuan; Liao, Longyu; CrystEngComm  (2020) –; doi:10.1039/D0CE00278J

data_7240274
_publ_section_title
;
 Superior thermally robust energetic materials featuring Z-E isomeric
 bis(3,4-diamino-1,2,4-triazol-5-yl)-1H-pyrazole: self-assembly
 nitrogen-rich tubes and templates with Hofmeister anions capture
 architecture
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00278J
_journal_year                    2020
_chemical_formula_moiety         'O4 S, 3(H2 O), C7 H12 N12'
_chemical_formula_sum            'C7 H18 N12 O7 S'
_chemical_formula_weight         414.39
_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             2018-01-24
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2020-04-04 deposited with the CCDC.	2020-04-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.193(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.6062(7)
_cell_length_b                   10.0221(11)
_cell_length_c                   24.619(3)
_cell_measurement_reflns_used    1385
_cell_measurement_temperature    173
_cell_measurement_theta_max      23.087
_cell_measurement_theta_min      2.625
_cell_volume                     1623.3(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      173
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0870
_diffrn_reflns_av_unetI/netI     0.1042
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9494
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.395
_diffrn_reflns_theta_min         1.661
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.268
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6209
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0877 before and 0.0675 after correction. The Ratio of minimum to maximum transmission is 0.8330. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_description       needle
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         3227
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.1197
_refine_ls_R_factor_gt           0.0574
_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^)+(0.0720P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1298
_refine_ls_wR_factor_ref         0.1587
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1891
_reflns_number_total             3227
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00278j2.cif
_cod_data_source_block           mo_20180085-ma-32_0m
_cod_database_code               7240274
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.961
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 O7-H7B
 0.85 with sigma of 0.02
 O5-H5B \\sim O5-H5A
 with sigma of 0.02
3.a Free rotating group:
 O5(H5A), O6(H6A,H6B), O7(H7A)
3.b Rotating group:
 N2(H2A,H2B), N10(H10A,H10B)
3.c Aromatic/amide H refined with riding coordinates:
 N6(H6), N4(H4), N9(H9), C4(H4A)
3.d X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N11(H11A,H11B)
;
_olex2_submission_special_instructions 'No special instructions were received'