Crystal structure evolution of the high energetic compound carbonic dihydrazidinium bis[3-(5-nitroimino-1,2,4-triazolate)] induced by solvents
Ren, Jianrong; Chen, Dong; Liu, Guangrui; Wang, Kangcai; Fan, Guijuan; Yu, Yanwu; Zhang, Chaoyang; Li, Hongzhen; CrystEngComm 22 (2020) 593–601; doi:10.1039/C9CE01329F

data_7239680
_publ_section_title
;
 Crystal structure evolution of the high energetic compound carbonic
 dihydrazidinium bis[3-(5-nitroimino-1,2,4-triazolate)] induced by
 solvents
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              593
_journal_page_last               601
_journal_paper_doi               10.1039/C9CE01329F
_journal_volume                  22
_journal_year                    2020
_chemical_formula_moiety         'C4 H2 N10 O4, C H8 N4 O, 2(H2 O)'
_chemical_formula_sum            'C5 H14 N14 O7'
_chemical_formula_weight         382.30
_chemical_name_common            CBNT
_chemical_name_systematic
'carbohydrazide bis[3-(5-nitroimino-1,2,4-triazolate)]'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-06-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-06-25 deposited with the CCDC.	2019-12-03 downloaded from the CCDC.
;
_cell_angle_alpha                97.740(10)
_cell_angle_beta                 99.840(11)
_cell_angle_gamma                90.131(10)
_cell_formula_units_Z            2
_cell_length_a                   6.5011(8)
_cell_length_b                   10.2497(12)
_cell_length_c                   11.0964(13)
_cell_measurement_reflns_used    1139
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.7250
_cell_measurement_theta_min      3.7390
_cell_volume                     721.64(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0874
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.833
_diffrn_measurement_details
;
  1 omega  -83.00   11.40   0.8000   75.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.9669  -77.0000  -60.0000 118

  2 omega  -42.00   52.40   0.8000   75.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.9669   77.0000   60.0000 118

  3 omega  -87.00  -35.00   0.8000   75.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.9669 -178.0000   90.0000 65

  4 omega  -15.00   19.40   0.8000   75.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.9669  -99.0000 -180.0000 43

  5 omega    1.00   61.00   0.8000   75.0000
omega____ theta____ kappa____ phi______ frames
    -       16.6856   38.0000 -150.0000 75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0470816000
_diffrn_orient_matrix_UB_12      0.0637561000
_diffrn_orient_matrix_UB_13      0.0175623000
_diffrn_orient_matrix_UB_21      -0.0421779000
_diffrn_orient_matrix_UB_22      0.0171350000
_diffrn_orient_matrix_UB_23      -0.0588989000
_diffrn_orient_matrix_UB_31      -0.0909627000
_diffrn_orient_matrix_UB_32      0.0228484000
_diffrn_orient_matrix_UB_33      0.0226231000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0817
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.833
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5609
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.833
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.323
_diffrn_reflns_theta_min         2.932
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.157
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29988
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.759
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         3290
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1036
_refine_ls_R_factor_gt           0.0597
_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^)+(0.0658P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1394
_refine_ls_wR_factor_ref         0.1664
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2023
_reflns_number_total             3290
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01329f2.cif
_cod_data_source_block           180606_s2_cd_180530-1
_cod_depositor_comments
;Adding full bibliography for 7239680--7239683.cif.

 Adding full bibliography for 7239680--7239683.cif.
;
_cod_original_cell_volume        721.65(15)
_cod_database_code               7239680
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         c12h12n2o3
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.947
_reflns_odcompleteness_completeness 98.51
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O6(H6A,H6B), O7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 N12(H12), N13(H13)
;
_shelx_res_checksum              6105
_olex2_submission_special_instructions 'No special instructions were received'