Nitrogen-rich alkali metal 5,5′-hydrazinebistetrazolate salts: environmentally friendly compounds in pyrotechnic mixtures
Ebespächer, Moritz; Klapötke, Thomas M.; Miró Sabaté, Carles; New Journal of Chemistry 33 (2009) 517–; doi:10.1039/b818927g

data_7051663
_publ_section_title
;
 Nitrogen-rich alkali metal 5,5&#x2032;-hydrazinebistetrazolate salts:
 environmentally friendly compounds in pyrotechnic mixtures
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              517
_journal_paper_doi               10.1039/b818927g
_journal_volume                  33
_journal_year                    2009
_chemical_compound_source
;
5,5-hidrazinebistetrazole was treated with lithium hydroxide in water.
;
_chemical_formula_moiety         'C2 H8 Li2 N10 O3'
_chemical_formula_sum            'C2 H8 Li2 N10 O3'
_chemical_formula_weight         234.06
_chemical_name_common            'Lithium hydrazinebistetrazolate trihydrate'
_chemical_name_systematic
;
lithium hydrazinebistetrazolate trihydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                C2H8Li2N10O3_dx034_Miro
_audit_creation_date             'Wed Jan 09 14:46:18 2008'
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_audit_update_record             'Tue Jan 15 15:21:21 2008'
_cell_angle_alpha                83.827(3)
_cell_angle_beta                 75.925(4)
_cell_angle_gamma                66.539(4)
_cell_formula_units_Z            2
_cell_length_a                   6.7522(4)
_cell_length_b                   7.7880(3)
_cell_length_c                   10.0091(4)
_cell_measurement_reflns_used    7271
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.11
_cell_measurement_theta_min      4.20
_cell_volume                     468.30(4)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET)
(compiled Apr 1 2005,17:53:34)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET)
(compiled Apr 1 2005,17:53:34)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET)
(compiled Apr 1 2005,17:53:34)
;
_computing_structure_refinement
'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)'
_computing_structure_solution
;
A. Altomare, M. C. Burla, M. Camalli, G. L. Cascarano, C. Giacovazzo, A.
Guagliardi, A. G. G. Moliterni, G. Polidori, R. Spagna: SIR97: a new tool for
crystal structure determination and refinement; J. Appl. Crystallogr. 1999,
32, 115-119.
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 15.9809
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Oxford Xcalibur3 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_collimation    '0.5 mm collimator'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0241
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13435
_diffrn_reflns_theta_full        30.11
_diffrn_reflns_theta_max         30.11
_diffrn_reflns_theta_min         4.20
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_type              'Spellman generator'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.139
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.954
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction program, 2005'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             240
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         2743
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0479P)^2^+0.7103P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0898
_refine_ls_wR_factor_ref         0.0933
_reflns_number_gt                2152
_reflns_number_total             2743
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b818927g.txt
_cod_data_source_block           LiHBTx3H2O
_cod_database_code               7051663
_kl_diffrn_measurement_detector_distance 50
_kl_archive_shelxl_comment       'release 97-2'
_kl_archive_shelxl_res
;
CELL 0.71073 6.7522 7.7880 10.0091 83.827 75.925 66.539
ZERR 2.00 0.0004 0.0003 0.0004 0.003 0.004 0.004
LATT 1
SFAC C H C N O LI
UNIT 0 16 4 20 6 4
MERG 2
FMAP 2
PLAN 25
ACTA
BOND $H
CONF
EQIV $1 -x, -y+1, -z+1
EQIV $2 -x, -y+1, -z+2
EQIV $3 -x+1, -y+1, -z+1
EQIV $4 -x+1, -y, -z+2
EQIV $5 x, y+1, z
EQIV $6 x, y-1, z
HTAB N5 N9_$1
HTAB N6 N2_$2
HTAB O3 N9_$3
HTAB O3 N10_$3
HTAB O2 N10_$1
HTAB O1 N1_$2
HTAB O3 N2_$4
HTAB O1 N1_$5
HTAB O2 O1_$6
L.S. 14
TEMP -173.00
WGHT 0.057200 0.013400
FVAR 0.35346
C2 3 0.186326 0.548868 0.560055 11.00000 0.01072 0.01112 =
0.01050 0.00054 -0.00326 -0.00588
N5 4 0.133585 0.385452 0.766997 11.00000 0.01674 0.01266 =
0.01121 0.00458 -0.00630 -0.00883
N7 4 0.344004 0.399139 0.492517 11.00000 0.01202 0.01266 =
0.00953 0.00023 -0.00201 -0.00518
O2 5 0.281762 0.012562 0.577371 11.00000 0.01479 0.01275 =
0.01192 0.00160 -0.00377 -0.00355
O1 5 0.185498 0.881993 0.854207 11.00000 0.01467 0.01337 =
0.01404 -0.00144 -0.00134 -0.00644
N8 4 0.362997 0.454062 0.358649 11.00000 0.01240 0.01311 =
0.01017 0.00120 -0.00271 -0.00571
N6 4 0.118052 0.559678 0.703106 11.00000 0.01394 0.00940 =
0.00869 0.00142 -0.00142 -0.00316
N2 4 0.293743 0.209107 1.072216 11.00000 0.01430 0.01367 =
0.01164 0.00095 -0.00414 -0.00661
N10 4 0.106184 0.692800 0.476740 11.00000 0.01240 0.01263 =
0.00952 0.00075 -0.00204 -0.00507
N3 4 0.373558 0.339413 1.044534 11.00000 0.01436 0.01277 =
0.00944 0.00157 -0.00226 -0.00573
N1 4 0.184964 0.209585 0.974304 11.00000 0.01307 0.01295 =
0.01004 0.00161 -0.00332 -0.00601
N9 4 0.223007 0.627736 0.349148 11.00000 0.01219 0.01377 =
0.01124 0.00030 -0.00232 -0.00527
N4 4 0.322543 0.431684 0.926616 11.00000 0.01214 0.01192 =
0.00888 0.00013 -0.00324 -0.00492
C1 3 0.207906 0.347601 0.887455 11.00000 0.00955 0.01046 =
0.00868 -0.00083 -0.00078 -0.00304
LI1 6 0.431245 0.632219 0.832594 11.00000 0.01743 0.01446 =
0.01452 0.00075 -0.00209 -0.00745
LI2 6 0.485354 0.141929 0.575560 11.00000 0.01900 0.01420 =
0.01693 0.00129 -0.00561 -0.00604
O3 5 0.641782 0.065486 0.720594 11.00000 0.02394 0.01735 =
0.01586 0.00566 -0.00856 -0.01088
H5 2 0.021263 0.356251 0.768669 11.00000 0.01985
H6 2 -0.010358 0.641146 0.729558 11.00000 0.02171
H3B 2 0.688553 0.151536 0.732048 11.00000 0.05024
H2B 2 0.166063 0.085655 0.553381 11.00000 0.04040
H1A 2 0.083968 0.855711 0.904422 11.00000 0.04995
H3A 2 0.651826 -0.013763 0.790507 11.00000 0.03648
H1B 2 0.199296 0.969091 0.894744 11.00000 0.04056
H2A 2 0.238428 -0.036225 0.652935 11.00000 0.03700
HKLF 4

REM dx034 in P-1
REM R1 = 0.0316 for 2152 Fo > 4sig(Fo) and 0.0410 for all 2743 data
REM 186 parameters refined using 0 restraints

END

WGHT 0.0572 0.0134
REM Highest difference peak 0.287, deepest hole -0.245, 1-sigma level 0.051
Q1 1 0.2811 0.3756 0.8956 11.00000 0.05 0.29
Q2 1 0.2160 0.2687 0.9213 11.00000 0.05 0.26
Q3 1 0.1240 0.6137 0.5278 11.00000 0.05 0.25
Q4 1 0.2327 0.2033 1.0233 11.00000 0.05 0.23
Q5 1 0.1621 0.5530 0.6244 11.00000 0.05 0.22
Q6 1 0.1516 0.3797 0.8356 11.00000 0.05 0.22
Q7 1 0.4441 0.3556 1.0916 11.00000 0.05 0.21
Q8 1 0.4160 0.3808 0.2985 11.00000 0.05 0.21
Q9 1 0.4346 0.3048 0.5237 11.00000 0.05 0.20
Q10 1 0.2874 0.1322 1.1385 11.00000 0.05 0.20
Q11 1 0.3518 0.2696 1.0625 11.00000 0.05 0.20
Q12 1 0.2804 0.4541 0.5371 11.00000 0.05 0.20
Q13 1 0.3507 0.4085 0.4496 11.00000 0.05 0.20
Q14 1 -0.0267 0.7607 0.4924 11.00000 0.05 0.20
Q15 1 0.3948 0.5059 0.8832 11.00000 0.05 0.20
Q16 1 0.3686 0.3819 0.9829 11.00000 0.05 0.19
Q17 1 0.1280 0.4723 0.7370 11.00000 0.05 0.19
Q18 1 0.2842 0.5529 0.9114 11.00000 0.05 0.18
Q19 1 0.3843 -0.0006 0.5227 11.00000 0.05 0.18
Q20 1 0.2043 0.5755 0.7394 11.00000 0.05 0.17
Q21 1 0.1037 0.1477 1.0001 11.00000 0.05 0.17
Q22 1 0.1387 0.6801 0.4430 11.00000 0.05 0.17
Q23 1 0.2858 0.7680 0.8910 11.00000 0.05 0.17
Q24 1 0.2774 0.5339 0.3521 11.00000 0.05 0.16
Q25 1 0.0909 0.3215 0.7409 11.00000 0.05 0.16
;