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_7231971
_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 H52 Co2 Mo48 N8 O178 P4 Zn16)'
_chemical_formula_sum            'C48 H26 Co Mo24 N4 O89 P2 Zn8'
_chemical_formula_weight         5029.12
_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   mixed
_audit_block_doi                 10.5517/ccdc.csd.cc1zjbmg
_audit_creation_date             2018-03-30
_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                   17.386(4)
_cell_length_b                   23.565(6)
_cell_length_c                   45.325(11)
_cell_measurement_reflns_used    9951
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.011
_cell_measurement_theta_min      2.353
_cell_volume                     18570(8)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area Detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0665
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            65134
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         1.523
_exptl_absorpt_coefficient_mu    2.741
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4081
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1062 before and 0.0784 after correction. The Ratio of minimum to maximum transmission is 0.5475. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'dull light violet'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.799
_exptl_crystal_description       block
_exptl_crystal_F_000             9436
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
TITL mo_lan_0m in Fmmm #69
CELL   17.3860   23.5650   45.3250     90.00     90.00     90.00
SPGR Fmmm
C101 0.500 0.260 0.204 !       7.49 eA-3
Q102 0.750 0.250 0.227 !       5.11 eA-3
C103 0.250 0.251 0.203 !       3.84 eA-3
C104 0.835 0.226 0.187 !       3.80 eA-3
C105 0.173 0.502 0.352 !       2.95 eA-3
C106 0.679 0.460 0.136 !       2.45 eA-3
Q107 0.328 0.070 0.181 !       2.33 eA-3
Q108 0.401 0.364 0.235 !       2.31 eA-3
Q109 0.831 0.501 0.293 !       2.29 eA-3
Q110 0.500 0.428 0.224 !       2.08 eA-3
Q111 0.101 0.366 0.223 !       2.04 eA-3
Q112 0.904 0.500 0.176 !       2.01 eA-3
Q113 0.180 0.070 0.274 !       1.92 eA-3
Q114 0.601 0.365 0.259 !       1.84 eA-3
Q115 0.905 0.502 0.145 !       1.81 eA-3
Q116 1.000 0.433 0.321 !       1.77 eA-3
Q117 0.500 0.429 0.200 !       1.74 eA-3
Q118 0.165 0.502 0.254 !       1.67 eA-3
C119 0.687 0.502 0.121 !       1.59 eA-3
C120 1.000 0.500 0.000 !       1.58 eA-3
Q121 0.821 0.344 0.121 !       1.57 eA-3
Q122 0.823 0.422 0.205 !       1.57 eA-3
C123 1.000 0.376 0.047 !       1.51 eA-3
C124 0.771 0.345 0.125 !       1.51 eA-3
Q125 0.500 0.064 0.229 !       1.40 eA-3
C126 0.711 0.503 0.059 !       1.38 eA-3
C127 1.000 0.406 0.063 !       1.38 eA-3
C128 0.750 0.249 0.145 !       1.37 eA-3
C129 0.828 0.093 0.136 !       1.33 eA-3
C130 0.475 0.124 0.066 !       1.31 eA-3
C131 0.713 0.166 0.110 !       1.31 eA-3
Q132 0.162 0.118 0.149 !       1.29 eA-3
C133 0.852 0.196 0.168 !       1.29 eA-3
Q134 0.500 0.125 0.196 !       1.26 eA-3
C135 0.273 0.220 0.152 !       1.23 eA-3
C136 0.715 0.305 0.363 !       1.23 eA-3
Q137 0.500 0.195 0.288 !       1.22 eA-3
Q138 1.000 0.430 0.358 !       1.21 eA-3
Q139 1.000 0.177 0.180 !       1.21 eA-3
C140 1.000 0.444 0.057 !       1.21 eA-3
Q141 0.750 0.125 0.251 !       1.21 eA-3
Q142 0.737 0.499 0.031 !       1.20 eA-3
Q143 0.671 0.063 0.145 !       1.15 eA-3
Q144 0.446 0.500 0.426 !       1.15 eA-3
Q145 0.091 0.504 0.312 !       1.15 eA-3
C146 0.716 0.444 0.086 !       1.13 eA-3
Q147 0.359 0.500 0.109 !       1.13 eA-3
C148 0.310 0.164-0.002 !       1.11 eA-3
C149 0.700 0.133 0.105 !       1.11 eA-3
C150 0.268 0.245 0.085 !       1.10 eA-3
C151 0.289 0.194 0.122 !       1.10 eA-3
C152 0.689 0.445 0.109 !       1.08 eA-3
C153 0.281 0.178 0.067 !       1.07 eA-3
Q154 0.888 0.496 0.125 !       1.07 eA-3
Q155 0.179 0.501 0.063 !       1.07 eA-3
C156 0.784 0.100 0.015 !       1.07 eA-3
C157 0.283 0.298 0.398 !       1.07 eA-3
C158 0.801 0.498 0.402 !       1.06 eA-3
Q159 0.500 0.345 0.663 !       1.06 eA-3
Q160 1.000 0.345 0.163 !       1.06 eA-3
C161 0.253 0.278 0.085 !       1.06 eA-3
C162 0.094 0.267 0.301 !       1.06 eA-3
Q163 0.661 0.391 0.000 !       1.05 eA-3
C164 0.899 0.500 0.027 !       1.05 eA-3
Q165 0.563 0.230 0.318 !       1.05 eA-3
Q166 0.437 0.270 0.182 !       1.05 eA-3
Q167 0.063 0.230 0.818 !       1.05 eA-3
Q168 0.341 0.469 0.222 !       1.05 eA-3
C169 0.243 0.414 0.000 !       1.04 eA-3
C170 0.685 0.013 0.426 !       1.04 eA-3
Q171 1.000 0.383 0.139 !       1.04 eA-3
C172 0.903 0.226 0.185 !       1.04 eA-3
Q173 0.694 0.501 0.039 !       1.03 eA-3
Q174 1.000 0.497 0.254 !       1.03 eA-3
Q175 0.407 0.501 0.281 !       1.02 eA-3
Q176 0.582 0.501 0.238 !       1.02 eA-3
C177 0.282 0.016 0.414 !       1.02 eA-3
Q178 0.500 0.495 0.031 !       1.02 eA-3
Q179 0.500 0.077 0.194 !       1.01 eA-3
C180 0.260 0.204 0.359 !       1.01 eA-3
Q181 0.375 0.499 0.230 !       1.00 eA-3
C182 0.192 0.463 0.442 !       1.00 eA-3
C183 0.096 0.421 0.044 !       0.99 eA-3
C184 0.101 0.484 0.001 !       0.99 eA-3
Q185 0.376 0.360 0.195 !       0.98 eA-3
C186 0.685 0.414 0.118 !       0.98 eA-3
Q187 0.379 0.314 0.187 !       0.97 eA-3
Q188 0.950 0.498 0.105 !       0.97 eA-3
C189 0.941 0.370 0.047 !       0.97 eA-3
Q190 0.403 0.015 0.348 !       0.97 eA-3
Q191 0.141 0.337 0.233 !       0.97 eA-3
Q192 0.139 0.055 0.163 !       0.97 eA-3
C193 0.266 0.454 0.060 !       0.97 eA-3
Q194 0.419 0.498 0.223 !       0.97 eA-3
Q195 0.647 0.039 0.304 !       0.97 eA-3
C196 0.550 0.062 0.063 !       0.96 eA-3
C197 0.403 0.132 0.061 !       0.95 eA-3
Q198 0.907 0.363 0.187 !       0.95 eA-3
Q199 0.389 0.313 0.157 !       0.94 eA-3
;
_refine_diff_density_max         2.805
_refine_diff_density_min         -0.997
_refine_diff_density_rms         0.213
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         5702
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0495
_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^)+(0.0644P)^2^+559.6918P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1228
_refine_ls_wR_factor_ref         0.1398
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4624
_reflns_number_total             5702
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01827h2.cif
_cod_data_source_block           Co-PMOF
_cod_depositor_comments
'Adding full bibliography for 7231971--7231978.cif.'
_cod_original_cell_volume        18569(8)
_cod_database_code               7231971
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.811
_shelx_estimated_absorpt_t_min   0.684
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
C5 \\sim C2 \\sim C3 \\sim C4 \\sim O1 \\sim C1 \\sim N1 \\sim N2 \\sim C9
\\sim C7 \\sim C6 \\sim C8 \\sim C10: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: O1W(0.125) H1WA(0.125) H1WB(0.125)
4.a Riding coordinates:
 O1W(H1WA,H1WB)
4.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C6(H6), C4(H4), C3(H3)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'