Insensitive energetic compounds: alkaline earth metal salts of 5,5′-dinitramino-3,3′-methylene-1H-1,2,4-bistriazolate
Wang, Yanna; Yang, Xiaoming; Hu, Jie; Li, Haibo; Li, Zhimin; Zhang, Tonglai; New Journal of Chemistry 44 (2020) 19054–19060; doi:10.1039/D0NJ03773G

data_7060064
_publ_section_title
;
 Insensitive energetic compounds: alkaline earth metal salts of
 5,5&#x2032;-dinitramino-3,3&#x2032;-methylene-1H-1,2,4-bistriazolate
;
_journal_issue                   44
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              19054
_journal_page_last               19060
_journal_paper_doi               10.1039/D0NJ03773G
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'Ca2 H28 O14, 2(C5 H4 N10 O4), 4(H2 O)'
_chemical_formula_sum            'C10 H44 Ca2 N20 O26'
_chemical_formula_weight         940.81
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-11-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-06 deposited with the CCDC.	2020-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.83(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.691(4)
_cell_length_b                   8.2319(16)
_cell_length_c                   21.708(4)
_cell_measurement_reflns_used    9404
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.4855
_cell_measurement_theta_min      1.3384
_cell_volume                     3695.6(12)
_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      153.15
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            25998
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.473
_diffrn_reflns_theta_min         1.338
_exptl_absorpt_coefficient_mu    0.429
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7764
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_description       block
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.046
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.238
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         8280
_refine_ls_number_restraints     588
_refine_ls_restrained_S_all      1.224
_refine_ls_R_factor_all          0.1412
_refine_ls_R_factor_gt           0.1230
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0673P)^2^+41.0983P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2810
_refine_ls_wR_factor_ref         0.2933
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6822
_reflns_number_total             8280
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj03773g2.cif
_cod_data_source_block           bwn18377
_cod_depositor_comments
'Adding full bibliography for 7060062--7060064.cif.'
_cod_original_cell_volume        3695.6(13)
_cod_database_code               7060064
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.950
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, {H13A,H13B} of O13, {H10A,H10B} of O10, {H24A,H24B} of
  O24, {H25A,H25B} of O25, {H11A,H11B} of O11, {H16A,H16B} of O16, {H23A,H23B}
  of O23, {H14A,H14B} of O14, {H17A,H17B} of O17, {H12A,H12B} of O12, {H19A,
  H19B} of O19, {H9A,H9B} of O9, {H15A,H15B} of O15, {H22A,H22B} of O22, {H26A,
  H26B} of O26, All N(H) groups
 At 1.5 times of:
  {H18A,H18B} of O18, {H20A,H20B} of O20, {H21A,H21B} of O21
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.002 and sigma
for terminal atoms of 0.002
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.002 and
sigma for terminal atoms of 0.002
3.a Riding coordinates:
 O22(H22A,H22B), O14(H14A,H14B), O17(H17A,H17B), O12(H12A,H12B), O16(H16A,
 H16B), O23(H23A,H23B), N3(H3), N8(H8), O19(H19A,H19B), O21(H21A,H21B), O9(H9A,
 H9B), O15(H15A,H15B), O25(H25A,H25B), O24(H24A,H24B), O10(H10A,H10B), O20(H20A,
 H20B), O18(H18A,H18B), O13(H13A,H13B), O11(H11A,H11B), O26(H26A,H26B),
 N18(H18), N13(H13)
3.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C8(H8A,H8B)
;
_olex2_submission_special_instructions 'No special instructions were received'