Highly Energetic Tetraazidoborate Anion and Boron Triazide Adducts
Wolfgang Fraenk; Tassilo Habereder; Anton Hammerl; Thomas M. Klapötke; Burkhard Krumm; Peter Mayer; Heinrich Nöth; Marcus Warchhold; Inorganic Chemistry 40 (2001) 1334–1340; doi:10.1021/ic001119b

data_4319421
_publ_contact_author
;
      Heinrich N\"oth
      Institut f\"ur anorganische Chemie
      Universit\"at M\"unchen
      Butenandtstr. 5-13 (Haus D)
      81377 M\"unchen
      Bundesrepublik Deutschland
;
_publ_contact_author_email       H.Noeth@lrz.uni-muenchen.de
_publ_contact_author_fax         '089 2180 7865'
_publ_contact_author_phone       '089 2180 7454'
_publ_section_title
;
 Highly Energetic Tetraazidoborate Anion and Boron Triazide Adducts
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1334
_journal_page_last               1340
_journal_paper_doi               10.1021/ic001119b
_journal_volume                  40
_journal_year                    2001
_chemical_compound_source        'provided by W. Fraenk'
_chemical_formula_moiety         '2(B N12, C9 H20 N)'
_chemical_formula_sum            'C18 H40 B2 N26'
_chemical_formula_weight         642.307
_chemical_name_common            BN3
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_author_name               'Mayer, P.'
_audit_block_code                B(N3)4_tmpH2_e021_klapoetke
_audit_creation_date             25-Jan-00
_audit_creation_method           'form98_1/compatible with shelxl97-2'
_cell_angle_alpha                90
_cell_angle_beta                 95.438(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.7179(3)
_cell_length_b                   14.8750(8)
_cell_length_c                   29.5527(15)
_cell_measurement_reflns_used    4719
_cell_measurement_temperature    200(3)
_cell_measurement_theta_max      24.0
_cell_measurement_theta_min      2.0
_cell_volume                     3377.5(3)
_computing_cell_refinement       'Stoe IPDS software (Darmstadt, Germany)'
_computing_data_collection       'Stoe IPDS software (Darmstadt, Germany)'
_computing_data_reduction        'Stoe IPDS software (Darmstadt, Germany)'
_computing_molecular_graphics
;ORTEP (M. N. Burnett, C. K. Johnson, ORTEP-III: Oak Ridge Thermal Ellipsoid
 Plot Program for Crystal Structure Illustrations, Oak Ridge National
 Laboratory Report ORNL-6895, 1996). Windows version (L. J. Farrugia, Univ.
 Glasgow) used --- SCHAKAL (E. Keller, University of  Freiburg (Breisgau),
 Germany, 1995).
;
_computing_publication_material
;PLATON (A. L. Spek, Acta Crystallogr, Sect. A, 1990, 46, C34, 1995 version).
--- T.B.Cohen, Pure Appl. Chem. 1996,68,2339-2359 (atomic masses).
;
_computing_structure_refinement
'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(3)
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device       'image-plate area detector'
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       'area detection'
_diffrn_radiation_collimation    '0.5 mm collimator'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_sigmaI/netI    0.0971
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            10762
_diffrn_reflns_theta_full        24.03
_diffrn_reflns_theta_max         24.03
_diffrn_reflns_theta_min         1.95
_diffrn_source_current           50_mA
_diffrn_source_power             2.75_kW
_diffrn_source_type              'Spellman DF4 Series'
_diffrn_source_voltage           55_kV
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  0.9956
_exptl_absorpt_correction_T_min  0.9915
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'XRed, rev. 1.09, Stoe (Darmstadt, Germany)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.26317(11)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.867
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         4970
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.884
_refine_ls_R_factor_all          0.1366
_refine_ls_R_factor_gt           0.0684
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1690
_refine_ls_wR_factor_ref         0.1968
_reflns_number_gt                2334
_reflns_number_total             4970
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001119b_2.cif
_cod_data_source_block           ar
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4319421
_kl_diffrn_detector_area_phi_start 0.0
_kl_diffrn_detector_area_phi_end 100.2
_kl_diffrn_detector_area_phi_incr 0.6
_kl_diffrn_detector_area_expos_time 12.00_min
_kl_diffrn_detector_area_plate_dist 80.0_mm
_kl_diffrn_detector_area_eff_mos_spread 0.005
_kl_diffrn_detector_area_profile_funct dynamic
_kl_diffrn_detector_area_profile_min 11
_kl_diffrn_detector_area_profile_max 15
_kl_archive_shelxl_comment       'release 97-2'
_kl_archive_shelxl_res
;
TITL e021 in P2(1)/n(14)
CELL  0.71073    7.7179   14.8750   29.5527    90.000    95.438    90.000
ZERR  4          0.0003    0.0008    0.0015     0.000     0.006     0.000
LATT  1
SYMM 0.5-X, 0.5+Y, 0.5-Z
SFAC C H B N
UNIT 72 160 8 104

TEMP  -73

L.S. 10
BOND $H
CONF
ACTA
FMAP 2
PLAN -50

DFIX 1.53  0.01 C12 C13A
DFIX 1.53  0.001 C17 C18A
DFIX -1.53 0.01  C12 C10A
DFIX 1.53  0.001 C12 C10B
DFIX -1.53 0.001  C17 C18B
DFIX -1.53 0.01  C12 C13B

WGHT    0.111800
REM Wichtung schwankt zwischen 0.1118 und 0.1122, bei letzterm schlechtere wR2
FVAR       0.43712   0.52068
MOLE   1
N26   4    0.778927    0.171201    0.112878    11.00000    0.04235    0.03844 =
         0.03186    0.00058    0.00631   -0.00498
AFIX  23
H26A  2    0.783041    0.205527    0.087106    11.00000   -1.20000
H26B  2    0.867742    0.129941    0.112917    11.00000   -1.20000
AFIX   0
C12   1    0.612532    0.119599    0.107260    11.00000    0.05061    0.05591 =
         0.07530   -0.02687    0.02226   -0.01720
C17   1    0.823461    0.233178    0.153274    11.00000    0.05429    0.03676 =
         0.02690   -0.00227    0.00571   -0.00362
C11   1    0.626807    0.064441    0.063804    11.00000    0.08147    0.13153 =
         0.14039   -0.09853    0.04638   -0.05788
AFIX  33
H11A  2    0.724636    0.022443    0.068656    11.00000   -1.20000
H11B  2    0.646095    0.105019    0.038642    11.00000   -1.20000
H11C  2    0.518792    0.030684    0.056399    11.00000   -1.20000
AFIX   0
C16   1    1.002067    0.270127    0.147203    11.00000    0.05303    0.05578 =
         0.03954    0.00054    0.00060   -0.01244
AFIX  33
H16A  2    1.086518    0.220774    0.148584    11.00000   -1.20000
H16B  2    1.035630    0.313437    0.171450    11.00000   -1.20000
H16C  2    0.999939    0.300145    0.117637    11.00000   -1.20000
AFIX   0
PART  1
C10A  1    0.442508    0.167899    0.105837   -21.00000    0.07264
AFIX  33
H10A  2    0.427305    0.205399    0.078484   -21.00000   -1.20000
H10B  2    0.441019    0.205982    0.132857   -21.00000   -1.20000
H10C  2    0.347607    0.124016    0.105236   -21.00000   -1.20000
AFIX   0
C18A  1    0.694430    0.310072    0.157542   -21.00000    0.06575
AFIX  33
H18A  2    0.579217    0.285253    0.161502   -21.00000   -1.20000
H18B  2    0.687737    0.346948    0.129951   -21.00000   -1.20000
H18C  2    0.733668    0.347281    0.183907   -21.00000   -1.20000
AFIX   0
C13A  1    0.637045    0.059380    0.153688   -21.00000    0.04225
AFIX  23
H13A  2    0.531278    0.022487    0.155683   -21.00000   -1.20000
H13B  2    0.736308    0.017834    0.151794   -21.00000   -1.20000
AFIX   0
C15A  1    0.846732    0.171264    0.196890   -21.00000    0.04991
AFIX  23
H15A  2    0.869884    0.208299    0.224638   -21.00000   -1.20000
H15B  2    0.945309    0.129294    0.194955   -21.00000   -1.20000
AFIX   0
C14A  1    0.670265    0.117277    0.198258   -21.00000    0.05844
AFIX  23
H14C  2    0.677585    0.077530    0.225241   -21.00000   -1.20000
H14D  2    0.572651    0.159739    0.200466   -21.00000   -1.20000
AFIX   0
PART 2
C10B  1    0.488697    0.199785    0.099857    21.00000    0.07711
AFIX  23
H10D  2    0.368100    0.176840    0.094458    21.00000   -1.20000
H10E  2    0.515650    0.232074    0.072082    21.00000   -1.20000
AFIX   0
C18B  1    0.683404    0.307076    0.146977    21.00000    0.03746
AFIX  23
H18D  2    0.704729    0.344324    0.120303    21.00000   -1.20000
H18E  2    0.692970    0.346551    0.174070    21.00000   -1.20000
AFIX   0
C13B  1    0.557839    0.053990    0.138725    21.00000    0.07056
AFIX  33
H13C  2    0.645392    0.006259    0.142976    21.00000   -1.20000
H13D  2    0.446189    0.028059    0.126648    21.00000   -1.20000
H13E  2    0.544677    0.082960    0.167986    21.00000   -1.20000
AFIX   0
C15B  1    0.812014    0.184886    0.196819    21.00000    0.04340
AFIX  33
H15C  2    0.692839    0.163169    0.198365    21.00000   -1.20000
H15D  2    0.843284    0.225874    0.222249    21.00000   -1.20000
H15E  2    0.892357    0.133718    0.198604    21.00000   -1.20000
AFIX   0
C14B  1    0.497377    0.267951    0.140047    21.00000    0.06230
AFIX  23
H14A  2    0.412086    0.316917    0.133130    21.00000   -1.20000
H14B  2    0.468661    0.237267    0.168110    21.00000   -1.20000
AFIX   0
PART 0
N25   4    0.567538    0.183566    0.372734    11.00000    0.05189    0.02943 =
         0.03165   -0.00360    0.00450    0.00593
AFIX  23
H25A  2    0.504277    0.210421    0.348454    11.00000   -1.20000
H25B  2    0.527569    0.206953    0.398626    11.00000   -1.20000
AFIX   0
C1    1    0.814824    0.204568    0.324553    11.00000    0.07296    0.05617 =
         0.05695    0.01056    0.02666    0.00307
AFIX  33
H1A   2    0.738954    0.240390    0.303041    11.00000   -1.20000
H1B   2    0.808903    0.141259    0.315359    11.00000   -1.20000
H1C   2    0.934954    0.226003    0.324728    11.00000   -1.20000
AFIX   0
C2    1    0.754561    0.313849    0.384649    11.00000    0.06782    0.03977 =
         0.07955   -0.00547    0.01465   -0.00879
AFIX  33
H2A   2    0.714932    0.320689    0.415000    11.00000   -1.20000
H2B   2    0.675768    0.346512    0.362457    11.00000   -1.20000
H2C   2    0.872517    0.338219    0.384606    11.00000   -1.20000
AFIX   0
C3    1    0.755292    0.213965    0.371959    11.00000    0.04585    0.03889 =
         0.05188   -0.00103    0.01203    0.00112
C4    1    0.863774    0.159437    0.407481    11.00000    0.04302    0.05458 =
         0.04686   -0.00332    0.00715    0.00103
AFIX  23
H4A   2    0.836486    0.179070    0.438018    11.00000   -1.20000
H4B   2    0.988388    0.172212    0.404973    11.00000   -1.20000
AFIX   0
C5    1    0.834125    0.058255    0.403253    11.00000    0.05750    0.04758 =
         0.04140    0.00264   -0.00039    0.01030
AFIX  23
H5A   2    0.868425    0.037000    0.373635    11.00000   -1.20000
H5B   2    0.907052    0.026746    0.427668    11.00000   -1.20000
AFIX   0
C6    1    0.644526    0.036907    0.406842    11.00000    0.05931    0.03401 =
         0.03608   -0.00192    0.00046    0.00264
AFIX  23
H6A   2    0.614143    0.054895    0.437361    11.00000   -1.20000
H6B   2    0.627756   -0.028910    0.404032    11.00000   -1.20000
AFIX   0
C7    1    0.521068    0.083101    0.371279    11.00000    0.04710    0.02810 =
         0.04155   -0.00573    0.00055    0.00145
C8    1    0.333438    0.078230    0.382085    11.00000    0.05772    0.05161 =
         0.06252   -0.00747    0.00585   -0.00951
AFIX  33
H8A   2    0.258983    0.109063    0.358239    11.00000   -1.20000
H8B   2    0.322019    0.107331    0.411405    11.00000   -1.20000
H8C   2    0.297852    0.015144    0.383606    11.00000   -1.20000
AFIX   0
C9    1    0.535282    0.044457    0.323809    11.00000    0.06949    0.04413 =
         0.03795   -0.01051   -0.00640    0.00754
AFIX  33
H9A   2    0.454230    0.076065    0.301740    11.00000   -1.20000
H9B   2    0.506280   -0.019689    0.323677    11.00000   -1.20000
H9C   2    0.654442    0.052237    0.315596    11.00000   -1.20000
AFIX   0
N1    4    0.692417    0.792892    0.470232    11.00000    0.07619    0.05354 =
         0.03683   -0.00927    0.00367   -0.02632
N2    4    0.771330    0.857590    0.487005    11.00000    0.08864    0.05961 =
         0.03282    0.01226   -0.00336   -0.01992
N3    4    0.847473    0.918612    0.500674    11.00000    0.14861    0.08647 =
         0.05696    0.00920   -0.01741   -0.07029
N4    4    0.396032    0.821317    0.500804    11.00000    0.10584    0.07053 =
         0.05135   -0.01524    0.02536    0.01759
N5    4    0.311217    0.851374    0.467335    11.00000    0.09171    0.04417 =
         0.07506   -0.00283    0.04271    0.00343
N6    4    0.224976    0.882182    0.438382    11.00000    0.12828    0.08305 =
         0.11447    0.02122    0.02316    0.03681
N7    4    0.487478    0.672832    0.465582    11.00000    0.06241    0.04991 =
         0.03273   -0.00694    0.00914   -0.01360
N8    4    0.398094    0.615672    0.480710    11.00000    0.06682    0.06302 =
         0.04047   -0.00121   -0.00080   -0.01654
N9    4    0.313983    0.559547    0.491880    11.00000    0.12180    0.10853 =
         0.07734    0.01950    0.00391   -0.06358
N10   4    0.598480    0.730351    0.545473    11.00000    0.09105    0.05669 =
         0.03199   -0.00589    0.00450   -0.00967
N11   4    0.718120    0.676892    0.552583    11.00000    0.10313    0.06202 =
         0.03550   -0.00325    0.00058   -0.02398
N12   4    0.827000    0.627620    0.561949    11.00000    0.12737    0.10017 =
         0.07655    0.00043   -0.02917    0.01298
N13   4    0.296542    0.388680    0.339052    11.00000    0.15242    0.07426 =
         0.06345    0.00667    0.00442   -0.02016
N14   4    0.371815    0.459100    0.353497    11.00000    0.08242    0.06506 =
         0.07793    0.00960   -0.01553    0.00140
N15   4    0.423078    0.520967    0.371056    11.00000    0.09158    0.07719 =
         0.11614   -0.01632   -0.00304   -0.02744
N16   4    0.162878    0.390553    0.256116    11.00000    0.11088    0.11958 =
         0.07404    0.02555   -0.00419    0.04008
N17   4    0.013603    0.399870    0.267540    11.00000    0.04412    0.06400 =
         0.07559   -0.00136    0.00735    0.00826
N18   4   -0.121169    0.408324    0.266657    11.00000    0.03938    0.19675 =
         0.10014    0.04904    0.01058    0.02506
N19   4    0.320430    0.257098    0.294945    11.00000    0.14541    0.07078 =
         0.04575    0.00383   -0.00832    0.03497
N20   4    0.294805    0.210505    0.261458    11.00000    0.07691    0.07847 =
         0.05655    0.01347   -0.00242    0.02347
N21   4    0.273670    0.161011    0.231890    11.00000    0.11044    0.09907 =
         0.07681    0.00024   -0.02283    0.01411
N22   4    0.479446    0.386802    0.273165    11.00000    0.09148    0.19164 =
         0.13704    0.09394    0.02190   -0.00367
N23   4    0.475852    0.442827    0.241594    11.00000    0.10586    0.07079 =
         0.06730    0.01260    0.03891   -0.01342
N24   4    0.507479    0.490161    0.216193    11.00000    0.10214    0.08689 =
         0.08790    0.03366    0.03726   -0.00085
B1    3    0.543215    0.753863    0.495831    11.00000    0.07362    0.04603 =
         0.03447   -0.00664    0.01487   -0.01065
B2    3    0.310677    0.358546    0.290801    11.00000    0.05154    0.06186 =
         0.04287    0.02256    0.00414    0.00053

HKLF 4

REM  e021 in P2(1)/n(14)
REM R1 =  0.0684 for   2334 Fo > 4sig(Fo)  and  0.1366 for all   4970 data
REM    411 parameters refined using      5 restraints

WGHT      0.1122      0.0000
REM Highest difference peak  0.619,  deepest hole -0.293,  1-sigma level  0.048
Q1    1   0.1285  0.3716  0.3070  11.00000  0.05    0.62
Q2    1   0.4585  0.4033  0.3291  11.00000  0.05    0.57
Q3    1   0.3267  0.4007  0.2413  11.00000  0.05    0.47
Q4    1   0.4542  0.2289  0.0914  11.00000  0.05    0.41
Q5    1  -0.0833  0.4777  0.2742  11.00000  0.05    0.32
;