Alkali metal salts of 3,6-dinitramino-1,2,4,5-tetrazine: promising nitrogen-rich energetic materials
Zhang, Tianhe; Du, Jiang; Li, Zhimin; Lin, Xinyu; Wang, Lin; Yang, Li; Zhang, Tonglai; CrystEngComm 21 (2019) 765–; doi:10.1039/C8CE01827H

data_7231978
_publ_section_title
;
 Alkali metal salts of 3,6-dinitramino-1,2,4,5-tetrazine: promising
 nitrogen-rich energetic materials
;
_journal_issue                   4
_journal_name_full               CrystEngComm
_journal_page_first              765
_journal_paper_doi               10.1039/C8CE01827H
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         '0.5(C96 H48 Mo48 N8 Ni2 O176 P4 Zn16)'
_chemical_formula_sum            'C48 H24 Mo24 N4 Ni O88 P2 Zn8'
_chemical_formula_weight         5010.88
_space_group_crystal_system      orthorhombic
_space_group_IT_number           69
_space_group_name_Hall           '-F 2 2'
_space_group_name_H-M_alt        'F m m m'
_symmetry_space_group_name_Hall  '-F 2 2'
_symmetry_space_group_name_H-M   'F m m m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_block_doi                 10.5517/ccdc.csd.cc1zjbpj
_audit_creation_date             2018-04-14
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5370)
;
_audit_update_record
;
2018-09-06 deposited with the CCDC.
2018-12-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.352(5)
_cell_length_b                   23.578(7)
_cell_length_c                   45.260(13)
_cell_measurement_reflns_used    9989
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.905
_cell_measurement_theta_min      2.348
_cell_volume                     18517(9)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0599
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            29915
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        23.967
_diffrn_reflns_theta_max         23.967
_diffrn_reflns_theta_min         1.525
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.760
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.3766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1167 before and 0.0876 after correction. The Ratio of minimum to maximum transmission is 0.5055. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'dull dark violet'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.797
_exptl_crystal_description       plate
_exptl_crystal_F_000             9400
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
TITL mo_hq80-4b_0m_a.res in Fmmm
CELL   17.3520   23.5780   45.2600     90.00     90.00     90.00
SPGR Fmmm
C101 0.500 0.233 0.204 !       7.89 eA-3
Q102 0.750 0.253 0.227 !       5.65 eA-3
Q103 0.762 0.248 0.207 !       4.59 eA-3
Q104 0.500 0.063 0.223 !       4.43 eA-3
C105 0.333 0.233 0.194 !       3.84 eA-3
C106 0.828 0.500 0.148 !       3.72 eA-3
C107 1.000 0.403 0.440 !       3.70 eA-3
Q108 0.500 0.197 0.204 !       3.68 eA-3
C109 0.500 0.389 0.081 !       3.44 eA-3
Q110 0.159 0.499 0.250 !       3.36 eA-3
Q111 0.684 0.430 0.179 !       3.28 eA-3
Q112 0.500 0.499 0.246 !       3.28 eA-3
Q113 0.900 0.367 0.281 !       3.25 eA-3
C114 0.765 0.235 0.318 !       3.24 eA-3
C115 1.000 0.052 0.052 !       3.16 eA-3
Q116 0.178 0.420 0.274 !       3.15 eA-3
C117 0.217 0.475 0.050 !       3.07 eA-3
Q118 0.172 0.499 0.203 !       3.05 eA-3
Q119 0.107 0.372 0.234 !       3.04 eA-3
C120 0.500 0.297-0.001 !       2.98 eA-3
C121 0.295 0.500 0.012 !       2.98 eA-3
C122 0.219 0.211 0.152 !       2.98 eA-3
C123 1.000 0.139 0.042 !       2.83 eA-3
C124 0.838 0.070 0.033 !       2.81 eA-3
C125 1.000 0.104 0.034 !       2.81 eA-3
C126 1.000 0.023 0.035 !       2.79 eA-3
C127 0.719 0.312 0.113 !       2.79 eA-3
C128 0.238 0.094 0.000 !       2.78 eA-3
C129 0.836 0.498 0.012 !       2.76 eA-3
C130 0.742 0.148 0.375 !       2.76 eA-3
C131 0.173 0.405 0.137 !       2.75 eA-3
C132 0.704 0.143 0.446 !       2.72 eA-3
C133 0.774 0.164 0.133 !       2.72 eA-3
C134 0.799 0.062 0.378 !       2.69 eA-3
C135 0.962 0.088 0.069 !       2.68 eA-3
Q136 0.853 0.352-0.001 !       2.65 eA-3
Q137 0.275 0.111 0.379 !       2.65 eA-3
C138 0.159 0.453 0.130 !       2.64 eA-3
Q139 0.413 0.498 0.168 !       2.59 eA-3
C140 0.834 0.479 0.141 !       2.58 eA-3
C141 0.718 0.062 0.083 !       2.57 eA-3
Q142 1.000 0.086 0.206 !       2.56 eA-3
Q143 0.813 0.376 0.154 !       2.55 eA-3
Q144 0.186 0.288 0.187 !       2.55 eA-3
C145 0.707 0.148-0.001 !       2.53 eA-3
Q146 0.563 0.048 0.436 !       2.51 eA-3
C147 0.764 0.429 0.036 !       2.50 eA-3
C148 0.194 0.181 0.089 !       2.49 eA-3
C149 0.183 0.498 0.070 !       2.48 eA-3
C150 0.903 0.219-0.001 !       2.48 eA-3
C151 0.770 0.497 0.090 !       2.48 eA-3
Q152 0.247 0.132 0.144 !       2.46 eA-3
Q153 0.401 0.496 0.187 !       2.46 eA-3
C154 0.729 0.080 0.058 !       2.45 eA-3
C155 0.429 0.124 0.465 !       2.45 eA-3
Q156 0.190 0.147 0.121 !       2.45 eA-3
C157 0.231 0.239 0.164 !       2.41 eA-3
Q158 0.500 0.345 0.344 !       2.40 eA-3
C159 0.871 0.498 0.133 !       2.39 eA-3
Q160 0.279 0.498 0.348 !       2.38 eA-3
C161 0.248 0.413 0.025 !       2.38 eA-3
C162 0.720 0.500 0.434 !       2.36 eA-3
Q163 0.729 0.499 0.227 !       2.36 eA-3
C164 0.251 0.424 0.107 !       2.35 eA-3
Q165 1.000 0.228 0.248 !       2.35 eA-3
C166 0.809 0.453 0.146 !       2.34 eA-3
Q167 0.597 0.242 0.449 !       2.33 eA-3
Q168 0.261 0.335 0.155 !       2.31 eA-3
C169 0.250 0.253 0.422 !       2.29 eA-3
C170 0.130 0.125 0.000 !       2.29 eA-3
Q171 0.949 0.258 0.237 !       2.29 eA-3
C172 0.691 0.167 0.144 !       2.28 eA-3
C173 1.000 0.087 0.012 !       2.27 eA-3
Q174 0.500 0.141 0.202 !       2.26 eA-3
C175 0.455 0.500 0.000 !       2.26 eA-3
C176 0.936 0.029 0.043 !       2.24 eA-3
C177 0.286 0.228 0.489 !       2.23 eA-3
C178 0.975 0.368 0.437 !       2.22 eA-3
Q179 1.000 0.466 0.156 !       2.22 eA-3
C180 0.283 0.023 0.001 !       2.21 eA-3
Q181 0.500 0.060 0.176 !       2.20 eA-3
C182 0.229 0.141 0.012 !       2.19 eA-3
Q183 0.500 0.369 0.322 !       2.19 eA-3
Q184 0.866 0.501 0.109 !       2.19 eA-3
C185 0.184 0.500 0.121 !       2.19 eA-3
Q186 0.500 0.079 0.138 !       2.19 eA-3
Q187 0.534 0.318 0.097 !       2.18 eA-3
C188 0.728 0.471 0.032 !       2.18 eA-3
Q189 0.305 0.468 0.243 !       2.18 eA-3
C190 0.054 0.424 0.454 !       2.17 eA-3
C191 0.909 0.420 0.456 !       2.17 eA-3
Q192 0.248 0.190 0.173 !       2.16 eA-3
Q193 0.500 0.163 0.291 !       2.14 eA-3
C194 0.634 0.374 0.065 !       2.13 eA-3
Q195 0.500 0.391 0.340 !       2.13 eA-3
C196 0.246 0.108 0.043 !       2.12 eA-3
C197 0.780 0.402 0.020 !       2.12 eA-3
Q198 0.246 0.219 0.196 !       2.12 eA-3
Q199 0.891 0.187 0.336 !       2.12 eA-3
;
_refine_diff_density_max         4.175
_refine_diff_density_min         -3.018
_refine_diff_density_rms         0.414
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3893
_refine_ls_number_restraints     279
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.1517
_refine_ls_R_factor_gt           0.1238
_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/[\s^2^(Fo^2^)+(0.0558P)^2^+9992.3027P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2686
_refine_ls_wR_factor_ref         0.2888
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3170
_reflns_number_total             3893
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01827h2.cif
_cod_data_source_block           Ni-PMOF
_cod_depositor_comments
'Adding full bibliography for 7231971--7231978.cif.'
_cod_original_cell_volume        18518(9)
_cod_database_code               7231978
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.789
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained planarity
 C4_$1, C3_$1, C2, C4, C3, C5
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
N1 \\sim N2 \\sim C7 \\sim C6 \\sim C8 \\sim C9 \\sim C5 \\sim O1 \\sim C1
\\sim C2 \\sim C4 \\sim C3 \\sim C10: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02
O15 \\sim O4 \\sim O5 \\sim O13 \\sim O6 \\sim O3 \\sim P1 \\sim O2 \\sim O7
\\sim O12 \\sim O11 \\sim O8 \\sim O10 \\sim O9 \\sim O14: within 3.2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(P1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O7) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O2) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C4(H4), C3(H3), C10(H10)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'