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_7051664
_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 rubidium carbonate in water.
;
_chemical_formula_moiety         'C2 H2 N10 Rb2'
_chemical_formula_sum            'C2 H2 N10 Rb2'
_chemical_formula_weight         337.08
_chemical_name_common            'Rubidium hydrazinebistetrazolate'
_chemical_name_systematic
;
rubidium hydrazinebistetrazolate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                C2H2N10Rb2_dx037_Miro
_audit_creation_date             'Mon Jan 07 12:19:55 2008'
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_audit_update_record             'Tue Jan 15 16:28:14 2008'
_cell_angle_alpha                90.00
_cell_angle_beta                 111.490(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.5093(2)
_cell_length_b                   20.3928(6)
_cell_length_c                   6.7479(2)
_cell_measurement_reflns_used    6435
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.9994
_cell_measurement_theta_min      3.7119
_cell_volume                     833.47(5)
_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 0.933
_diffrn_measured_fraction_theta_max 0.933
_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  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            12036
_diffrn_reflns_theta_full        32.72
_diffrn_reflns_theta_max         32.72
_diffrn_reflns_theta_min         3.72
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_type              'Spellman generator'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    11.720
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37166
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction program,2005'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.686
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.634
_refine_diff_density_min         -0.823
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         2863
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0211
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0220P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0398
_refine_ls_wR_factor_ref         0.0452
_reflns_number_gt                2234
_reflns_number_total             2863
_reflns_threshold_expression     >2sigma(I
_cod_data_source_file            b818927g.txt
_cod_data_source_block           RbHBT
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        833.46(4)
_cod_original_sg_symbol_Hall     '-P 1'
_cod_original_sg_symbol_H-M      'P 2 1/n'
_cod_database_code               7051664
_kl_diffrn_measurement_detector_distance 50
_kl_archive_shelxl_comment       'release 97-2'
_kl_archive_shelxl_res
;
CELL 0.71073 6.5093 20.3928 6.7479 90.000 111.490 90.000
ZERR 4.00 0.0002 0.0006 0.0002 0.000 0.004 0.000
LATT 1
SYMM 1/2 - X, 1/2 + Y, 1/2 - Z
SFAC C H N RB
UNIT 8 8 40 8
MERG 2
FMAP 2
PLAN 25
ACTA
BOND $H
CONF
EQIV_$1 x-1/2, -y+1/2, z-1/2
EQIV_$2 x-1/2, -y+1/2, z+1/2
HTAB N6 N3_$1
HTAB N6 N4_$1
HTAB N5 N2_$2
L.S. 4
TEMP -173.00
WGHT 0.022000
FVAR 4.63197
RB2 4 0.739912 0.073993 0.325708 11.00000 0.01023
0.01009 =
0.00953 0.00063 0.00497 -0.00016
RB1 4 0.400815 0.132298 -0.285094 11.00000 0.01046
0.00821 =
0.01066 -0.00072 0.00482 0.00056
N10 3 0.221588 0.040493 -0.002811 11.00000 0.00935
0.00851 =
0.01036 -0.00082 0.00465 0.00035
N4 3 0.279065 0.285721 0.179064 11.00000 0.01464
0.00804 =
0.01309 -0.00163 0.00691 -0.00178
N2 3 0.565268 0.248344 0.117651 11.00000 0.01303
0.01187 =
0.01485 -0.00113 0.00599 -0.00170
C2 1 0.155747 0.071756 0.137380 11.00000 0.00720
0.00752 =
0.00933 -0.00130 0.00309 -0.00353
N6 3 0.032872 0.129625 0.091765 11.00000 0.01258
0.00748 =
0.01391 0.00115 0.00432 0.00030
N7 3 0.202965 0.039409 0.321072 11.00000 0.01170
0.00719 =
0.00975 0.00034 0.00428 -0.00027
N5 3 0.132749 0.182008 0.236901 11.00000 0.02131
0.00456 =
0.01957 -0.00220 0.01572 -0.00079
N9 3 0.312102 -0.015813 0.099280 11.00000 0.00776
0.01002 =
0.01121 0.00010 0.00291 -0.00023
N1 3 0.456844 0.195026 0.148536 11.00000 0.01374
0.00929 =
0.01151 -0.00130 0.00692 -0.00113
N8 3 0.302930 -0.016289 0.290497 11.00000 0.00930
0.00912 =
0.00969 -0.00053 0.00244 0.00013
N3 3 0.461421 0.302130 0.137068 11.00000 0.01377
0.01079 =
0.01372 -0.00200 0.00594 -0.00346
C1 1 0.284612 0.220176 0.184772 11.00000 0.01400
0.00713 =
0.00642 -0.00144 0.00478 -0.00205
H6 2 0.001733 0.141800 -0.023963 11.00000 0.01384
H5 2 0.030799 0.206554 0.250496 11.00000 0.02665
HKLF 4

REM rbhbt in P2(1)/n
REM R1 = 0.0211 for 2234 Fo > 4sig(Fo) and 0.0360 for all 2863 data
REM 135 parameters refined using 0 restraints

END

WGHT 0.0220 0.0000
REM Highest difference peak 0.634, deepest hole -0.823, 1-sigma level
0.145
Q1 1 0.5579 0.1357 -0.1273 11.00000 0.05 0.63
Q2 1 0.4724 0.1299 -0.3752 11.00000 0.05 0.62
Q3 1 0.6562 0.0459 0.2964 11.00000 0.05 0.62
Q4 1 0.4100 0.1208 -0.1411 11.00000 0.05 0.60
Q5 1 0.7093 0.0741 0.4057 11.00000 0.05 0.57
Q6 1 0.7473 0.1003 0.4718 11.00000 0.05 0.55
Q7 1 0.4908 0.0872 -0.3185 11.00000 0.05 0.55
Q8 1 0.6762 0.2566 0.1254 11.00000 0.05 0.52
Q9 1 0.5934 0.1299 -0.2718 11.00000 0.05 0.50
Q10 1 0.2769 0.2523 0.1687 11.00000 0.05 0.50
Q11 1 0.8231 0.0455 0.3553 11.00000 0.05 0.50
Q12 1 0.2998 -0.0198 0.1799 11.00000 0.05 0.49
Q13 1 0.5754 0.1531 0.0145 11.00000 0.05 0.48
Q14 1 0.3470 0.2038 0.1326 11.00000 0.05 0.48
Q15 1 0.5380 0.0898 -0.1871 11.00000 0.05 0.47
Q16 1 0.3247 0.0335 -0.0805 11.00000 0.05 0.47
Q17 1 0.3583 0.2348 0.2395 11.00000 0.05 0.47
Q18 1 0.2302 0.1344 -0.4178 11.00000 0.05 0.47
Q19 1 0.9448 0.0801 0.4125 11.00000 0.05 0.47
Q20 1 0.1815 0.3110 0.1228 11.00000 0.05 0.46
Q21 1 0.7561 0.0393 0.4693 11.00000 0.05 0.46
Q22 1 0.5958 0.0752 0.1844 11.00000 0.05 0.46
Q23 1 0.5085 0.1636 -0.2621 11.00000 0.05 0.46
Q24 1 0.1764 0.1421 0.2665 11.00000 0.05 0.46
Q25 1 0.5419 0.1036 -0.0017 11.00000 0.05 0.45
;