# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2012


data_global
#TrackingRef '- SI--100oC.cif'

_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

loop_
_publ_author_name
_publ_author_address
'Fei Xu'
;
Graduate School of Energy Science, Kyoto University
Yoshida, Sakyo-ku, Kyoto 606-8501, Japan
;
'Kazuhiko Matsumoto'
;
Graduate School of Energy Science, Kyoto University
Yoshida, Sakyo-ku, Kyoto 606-8501, Japan
;
'Rika Hagiwara'
;
Graduate School of Energy Science, Kyoto University
Yoshida, Sakyo-ku, Kyoto 606-8501, Japan
;

_publ_contact_author_name        'Kazuhiko Matsumoto'

_publ_contact_author_address     
;
Graduate School of Energy Science, Kyoto University
Yoshida, Sakyo-ku, Kyoto 606-8501, Japan
;
_publ_contact_author_phone       81-75-753-4817
_publ_contact_author_fax         81-75-753-4817
_publ_contact_author_email       k-matsumoto@energy.kyoto-u.ac.jp

_publ_section_title              
;
Effects of Alkyl Chain Length and Anion Size on Thermal
and Structural Properties for 1-Alkyl-3-methylimidazolium
Hexafluorocomplex Salts (CxMImAF6, x = 14, 16, and 18; A = P, As, Sb, Nb,
and Ta)
;

#============================================================

data_C18MImPF6-25oC
#TrackingRef '- SI-25oC.cif'

_database_code_depnum_ccdc_archive 'CCDC 843137'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            C18MImPF6
_chemical_melting_point          352.9
_chemical_formula_moiety         
;
(C22 N2 H43 +), (P F6 -)
;
_chemical_formula_sum            'C22 H43 F6 N2 P'
_chemical_formula_weight         480.55

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/a

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x-1/2, -y-1/2, z'

_cell_length_a                   9.6506(16)
_cell_length_b                   9.5436(17)
_cell_length_c                   29.633(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.169(4)
_cell_angle_gamma                90.00
_cell_volume                     2727.3(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    298
_cell_measurement_reflns_used    5692
_cell_measurement_theta_min      6.01
_cell_measurement_theta_max      55.41

_exptl_crystal_description       platelet
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1032
_exptl_absorpt_coefficient_mu    0.152
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4817
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'RAPID AUTO 2.40 (Rigaku 2006)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      298
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS RapidII'
_diffrn_measurement_method       'imaging plate'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18736
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         3.00
_diffrn_reflns_theta_max         24.00
_reflns_number_total             4276
_reflns_number_gt                1328
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Rigaku R-AXIS Rapid-II'
_computing_cell_refinement       'RAPID AUTO 2.40 (Rigaku 2006)'
_computing_data_reduction        'RAPID AUTO 2.40 (Rigaku 2006)'
_computing_structure_solution    'SIR92 (Altmare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
This structure was solved based on the data at 25 deg C and the octadecyl chain
in this structure has a large conformational flexibility, which results in large
thermal motions of the atoms. Hence, the following restraints were applied.
The N-C and C-C bond lengths in the octadecyl chain were restrained using
the DFIX (1,2 C(N)-C distance: 1.54 A) and DANG (1,3 C(N)-C distance: 2.52 A)
commands in SHELXL. The N-C-C-C part of the trans structure was
weakly fixed using the FLAT command. Atomic displacement factors of the
disordered part and some carbon atoms in the octadecyl chain were restrained
using DELU and SIMU in SHELXL. The large R_factor_gt value is caused by the large
thermal motions of the atoms and the highly disordered structure.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4276
_refine_ls_number_parameters     301
_refine_ls_number_restraints     145
_refine_ls_R_factor_all          0.2122
_refine_ls_R_factor_gt           0.1039
_refine_ls_wR_factor_ref         0.3894
_refine_ls_wR_factor_gt          0.3062
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.142
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P -0.1641(2) 0.0270(3) 0.10122(9) 0.1360(11) Uani 1 1 d . . .
F4 F -0.2466(7) -0.0375(8) 0.1406(2) 0.239(3) Uani 1 1 d . . .
F3 F -0.2875(7) 0.1242(7) 0.0937(3) 0.279(4) Uani 1 1 d . . .
F2 F -0.0894(8) 0.0767(11) 0.0607(2) 0.288(4) Uani 1 1 d . . .
F5 F -0.0470(6) -0.0796(6) 0.1110(2) 0.218(3) Uani 1 1 d . . .
N1 N 0.3713(9) -0.0218(9) 0.1069(2) 0.134(2) Uani 1 1 d D A .
F6 F -0.0828(7) 0.1277(7) 0.1320(3) 0.251(3) Uani 1 1 d . . .
F1 F -0.2442(5) -0.0805(7) 0.0695(2) 0.199(2) Uani 1 1 d . . .
C21 C -0.618(2) -0.1505(18) 0.6759(7) 0.274(8) Uani 1 1 d D . .
H21A H -0.7039 -0.1312 0.6591 0.329 Uiso 1 1 calc R . .
H21B H -0.6093 -0.2513 0.6792 0.329 Uiso 1 1 calc R . .
C9 C 0.1357(11) -0.1442(15) 0.2392(4) 0.271(7) Uani 1 1 d DU . .
H9AA H 0.0739 -0.0785 0.2236 0.326 Uiso 0.561(16) 1 calc PR A 1
H9BA H 0.0927 -0.2357 0.2363 0.326 Uiso 0.561(16) 1 calc PR A 1
H9AB H 0.0526 -0.1287 0.2186 0.326 Uiso 0.439(16) 1 d PR A 2
H9BB H 0.1640 -0.2370 0.2379 0.326 Uiso 0.439(16) 1 d PR A 2
C18 C -0.3700(15) -0.1005(14) 0.5768(6) 0.231(6) Uani 1 1 d D . .
H18A H -0.2846 -0.1214 0.5938 0.277 Uiso 1 1 calc R . .
H18B H -0.3779 0.0007 0.5752 0.277 Uiso 1 1 calc R . .
C17 C -0.3550(17) -0.1548(13) 0.5291(5) 0.224(5) Uani 1 1 d D . .
H17A H -0.3481 -0.2561 0.5305 0.269 Uiso 1 1 calc R . .
H17B H -0.4396 -0.1326 0.5118 0.269 Uiso 1 1 calc R . .
C13 C -0.0976(14) -0.1601(14) 0.3838(4) 0.232(5) Uani 1 1 d DU . .
H13A H -0.1840 -0.1388 0.3675 0.279 Uiso 1 1 calc R . .
H13B H -0.0892 -0.2613 0.3854 0.279 Uiso 1 1 calc R . .
N3 N 0.4011(8) -0.1215(7) 0.0446(3) 0.126(2) Uani 1 1 d . . .
C22 C -0.6230(19) -0.086(2) 0.7212(9) 0.300(10) Uani 1 1 d D . .
H22A H -0.6306 0.0153 0.7180 0.360 Uiso 1 1 calc R . .
H22B H -0.5375 -0.1058 0.7382 0.360 Uiso 1 1 calc R . .
C12 C 0.0211(13) -0.1033(14) 0.3573(5) 0.230(5) Uani 1 1 d DU A .
H12A H 0.0143 -0.0021 0.3554 0.276 Uiso 1 1 calc R . .
H12B H 0.1085 -0.1265 0.3727 0.276 Uiso 1 1 calc R . .
C10 C 0.1368(13) -0.1073(15) 0.2872(4) 0.272(6) Uani 1 1 d DU A .
H10A H 0.1373 -0.0060 0.2900 0.326 Uiso 1 1 calc R . .
H10B H 0.2217 -0.1422 0.3017 0.326 Uiso 1 1 calc R . .
C15 C -0.2263(14) -0.1584(14) 0.4564(5) 0.228(5) Uani 1 1 d DU . .
H15A H -0.3113 -0.1355 0.4395 0.274 Uiso 1 1 calc R . .
H15B H -0.2196 -0.2597 0.4581 0.274 Uiso 1 1 calc R . .
C24 C 0.4636(9) -0.2115(9) 0.0101(3) 0.161(3) Uani 1 1 d . . .
H24A H 0.4318 -0.1816 -0.0195 0.242 Uiso 1 1 calc R . .
H24B H 0.4367 -0.3072 0.0147 0.242 Uiso 1 1 calc R . .
H24C H 0.5628 -0.2041 0.0126 0.242 Uiso 1 1 calc R . .
C5 C 0.2647(11) 0.0239(10) 0.0807(5) 0.150(3) Uani 1 1 d . . .
H5 H 0.1932 0.0837 0.0883 0.180 Uiso 1 1 calc R . .
C20 C -0.4984(17) -0.0963(17) 0.6499(7) 0.258(8) Uani 1 1 d D . .
H20A H -0.5060 0.0049 0.6479 0.309 Uiso 1 1 calc R . .
H20B H -0.4129 -0.1174 0.6669 0.309 Uiso 1 1 calc R . .
C14 C -0.1050(13) -0.1031(14) 0.4312(5) 0.226(5) Uani 1 1 d DU . .
H14A H -0.0199 -0.1268 0.4480 0.271 Uiso 1 1 calc R . .
H14B H -0.1112 -0.0018 0.4298 0.271 Uiso 1 1 calc R . .
C11 C 0.0179(13) -0.1635(14) 0.3111(5) 0.237(5) Uani 1 1 d DU . .
H11A H 0.0236 -0.2649 0.3127 0.284 Uiso 1 1 calc R A .
H11B H -0.0681 -0.1384 0.2951 0.284 Uiso 1 1 calc R . .
C2 C 0.4479(9) -0.1101(10) 0.0859(5) 0.140(3) Uani 1 1 d . . .
H2 H 0.5242 -0.1575 0.0986 0.168 Uiso 1 1 calc R . .
C19 C -0.4881(17) -0.1538(15) 0.6035(6) 0.232(6) Uani 1 1 d D . .
H19A H -0.5740 -0.1333 0.5868 0.278 Uiso 1 1 calc R . .
H19B H -0.4802 -0.2549 0.6057 0.278 Uiso 1 1 calc R . .
C23 C -0.744(3) -0.139(2) 0.7469(6) 0.332(11) Uani 1 1 d D . .
H23A H -0.8233 -0.1503 0.7266 0.498 Uiso 1 1 calc R . .
H23B H -0.7657 -0.0739 0.7702 0.498 Uiso 1 1 calc R . .
H23C H -0.7207 -0.2283 0.7603 0.498 Uiso 1 1 calc R . .
C16 C -0.2347(14) -0.1012(14) 0.5033(6) 0.224(5) Uani 1 1 d D . .
H16A H -0.2410 0.0001 0.5016 0.269 Uiso 1 1 calc R . .
H16B H -0.1495 -0.1240 0.5201 0.269 Uiso 1 1 calc R . .
C4 C 0.2855(10) -0.0369(11) 0.0412(4) 0.145(3) Uani 1 1 d . . .
H4 H 0.2303 -0.0242 0.0151 0.174 Uiso 1 1 calc R . .
C7A C 0.2558(16) -0.024(2) 0.1831(5) 0.213(8) Uani 0.561(16) 1 d PDU A 1
H7A1 H 0.2335 0.0561 0.2017 0.256 Uiso 0.561(16) 1 calc PR A 1
H7A2 H 0.1776 -0.0380 0.1621 0.256 Uiso 0.561(16) 1 calc PR A 1
C8A C 0.265(2) -0.149(2) 0.2133(6) 0.281(9) Uani 0.561(16) 1 d PDU A 1
H8A1 H 0.2694 -0.2349 0.1957 0.337 Uiso 0.561(16) 1 calc PR A 1
H8A2 H 0.3467 -0.1442 0.2334 0.337 Uiso 0.561(16) 1 calc PR A 1
C7B C 0.294(2) -0.1060(17) 0.1766(5) 0.236(9) Uani 0.439(16) 1 d PDU A 2
H7B1 H 0.2120 -0.1272 0.1577 0.283 Uiso 0.439(16) 1 calc PR A 2
H7B2 H 0.3495 -0.1901 0.1801 0.283 Uiso 0.439(16) 1 calc PR A 2
C8B C 0.2546(19) -0.0507(19) 0.2210(5) 0.235(9) Uani 0.439(16) 1 d PDU A 2
H8B1 H 0.2232 0.0455 0.2179 0.282 Uiso 0.439(16) 1 calc PR A 2
H8B2 H 0.3342 -0.0525 0.2420 0.282 Uiso 0.439(16) 1 calc PR A 2
C6 C 0.3798(9) 0.0167(11) 0.1557(3) 0.186(4) Uani 1 1 d DU . .
H6AA H 0.3925 0.1173 0.1580 0.224 Uiso 0.561(16) 1 calc PR A 1
H6BA H 0.4618 -0.0272 0.1694 0.224 Uiso 0.561(16) 1 calc PR A 1
H6AB H 0.3517 0.1075 0.1618 0.224 Uiso 0.439(16) 1 d PR A 2
H6BB H 0.4753 0.0032 0.1680 0.224 Uiso 0.439(16) 1 d PR A 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1 0.1313(17) 0.1268(17) 0.151(2) 0.0010(17) 0.0282(15) -0.0009(17)
F4 0.250(6) 0.287(8) 0.183(5) 0.029(5) 0.051(5) -0.037(6)
F3 0.178(5) 0.180(6) 0.478(12) 0.015(7) -0.018(7) 0.059(4)
F2 0.247(6) 0.419(11) 0.199(6) 0.096(7) 0.023(5) -0.138(8)
F5 0.166(4) 0.177(5) 0.308(7) -0.031(5) -0.032(5) 0.038(4)
N1 0.132(5) 0.134(6) 0.136(6) 0.026(5) 0.015(5) -0.016(5)
F6 0.220(6) 0.198(6) 0.332(8) -0.106(6) -0.041(6) -0.014(5)
F1 0.145(4) 0.220(5) 0.234(5) -0.080(4) 0.027(4) -0.021(4)
C21 0.35(2) 0.219(15) 0.252(18) -0.004(13) -0.030(16) -0.077(15)
C9 0.178(9) 0.276(13) 0.364(14) 0.155(12) 0.067(11) -0.021(9)
C18 0.237(14) 0.198(13) 0.255(16) -0.064(12) -0.030(12) 0.000(11)
C17 0.274(16) 0.174(11) 0.221(14) 0.002(10) -0.036(12) -0.044(11)
C13 0.239(12) 0.193(10) 0.262(11) 0.020(9) -0.026(9) -0.072(9)
N3 0.129(6) 0.115(5) 0.136(6) 0.011(5) 0.016(5) -0.021(5)
C22 0.29(2) 0.29(2) 0.32(2) -0.11(2) -0.021(18) -0.011(16)
C12 0.188(10) 0.189(11) 0.311(12) 0.010(10) -0.015(9) -0.043(8)
C10 0.214(11) 0.242(13) 0.362(14) 0.101(14) 0.025(11) -0.029(10)
C15 0.282(14) 0.186(10) 0.213(11) 0.009(9) -0.039(9) -0.063(10)
C24 0.183(8) 0.131(7) 0.174(8) -0.020(6) 0.053(6) -0.010(6)
C5 0.154(8) 0.148(8) 0.149(8) 0.004(7) 0.029(8) 0.021(6)
C20 0.258(17) 0.217(15) 0.293(19) -0.107(15) -0.052(15) 0.006(13)
C14 0.213(11) 0.183(11) 0.280(12) -0.008(10) -0.021(9) -0.035(9)
C11 0.211(10) 0.209(11) 0.288(11) 0.052(10) 0.001(10) -0.077(9)
C2 0.111(6) 0.125(7) 0.186(11) 0.013(7) 0.034(7) 0.009(5)
C19 0.258(16) 0.189(12) 0.245(15) -0.013(11) -0.023(12) -0.049(11)
C23 0.45(3) 0.31(2) 0.237(16) 0.006(14) -0.012(18) -0.08(2)
C16 0.219(13) 0.183(11) 0.267(15) -0.018(11) -0.031(12) -0.030(9)
C4 0.119(6) 0.133(7) 0.182(10) 0.037(7) -0.004(6) 0.010(6)
C7A 0.194(13) 0.312(19) 0.140(12) 0.066(12) 0.084(10) 0.091(13)
C8A 0.231(15) 0.24(2) 0.38(2) 0.112(15) 0.094(14) 0.035(15)
C7B 0.213(18) 0.239(19) 0.259(17) 0.106(17) 0.057(13) 0.066(14)
C8B 0.189(15) 0.23(2) 0.296(17) 0.141(17) 0.095(14) 0.045(14)
C6 0.164(8) 0.217(10) 0.181(9) 0.014(7) 0.037(6) 0.012(7)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 F2 1.500(6) . ?
P1 F3 1.519(6) . ?
P1 F6 1.523(6) . ?
P1 F5 1.541(6) . ?
P1 F4 1.565(6) . ?
P1 F1 1.575(6) . ?
N1 C2 1.295(9) . ?
N1 C5 1.338(10) . ?
N1 C6 1.492(9) . ?
C21 C22 1.482(13) . ?
C21 C20 1.503(13) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C9 C10 1.467(10) . ?
C9 C8A 1.493(10) . ?
C9 C8B 1.565(6) . ?
C9 H9AA 0.9700 . ?
C9 H9BA 0.9700 . ?
C9 H9AB 0.9992 . ?
C9 H9BB 0.9281 . ?
C18 C19 1.501(12) . ?
C18 C17 1.519(11) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C17 C16 1.503(11) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C13 C14 1.511(11) . ?
C13 C12 1.514(11) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
N3 C2 1.295(10) . ?
N3 C4 1.378(9) . ?
N3 C24 1.482(9) . ?
C22 C23 1.510(10) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C12 C11 1.483(11) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C10 C11 1.472(9) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C15 C16 1.498(11) . ?
C15 C14 1.507(11) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C5 C4 1.328(11) . ?
C5 H5 0.9300 . ?
C20 C19 1.487(12) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C2 H2 0.9300 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C4 H4 0.9300 . ?
C7A C8A 1.496(11) . ?
C7A C6 1.522(10) . ?
C7A H7A1 0.9700 . ?
C7A H7A2 0.9700 . ?
C8A H9BB 1.4981 . ?
C8A H8A1 0.9700 . ?
C8A H8A2 0.9700 . ?
C7B C8B 1.481(8) . ?
C7B C6 1.575(7) . ?
C7B H7B1 0.9700 . ?
C7B H7B2 0.9700 . ?
C8B H8B1 0.9700 . ?
C8B H8B2 0.9700 . ?
C6 H6AA 0.9700 . ?
C6 H6BA 0.9700 . ?
C6 H6AB 0.9285 . ?
C6 H6BB 0.9862 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F2 P1 F3 95.0(5) . . ?
F2 P1 F6 91.6(5) . . ?
F3 P1 F6 94.9(4) . . ?
F2 P1 F5 89.4(5) . . ?
F3 P1 F5 175.2(4) . . ?
F6 P1 F5 86.9(4) . . ?
F2 P1 F4 174.4(5) . . ?
F3 P1 F4 86.1(4) . . ?
F6 P1 F4 93.8(4) . . ?
F5 P1 F4 89.4(4) . . ?
F2 P1 F1 88.2(4) . . ?
F3 P1 F1 86.9(4) . . ?
F6 P1 F1 178.2(4) . . ?
F5 P1 F1 91.3(3) . . ?
F4 P1 F1 86.4(4) . . ?
C2 N1 C5 112.0(9) . . ?
C2 N1 C6 127.8(11) . . ?
C5 N1 C6 119.7(10) . . ?
C22 C21 C20 111.9(17) . . ?
C22 C21 H21A 109.2 . . ?
C20 C21 H21A 109.2 . . ?
C22 C21 H21B 109.2 . . ?
C20 C21 H21B 109.2 . . ?
H21A C21 H21B 107.9 . . ?
C10 C9 C8A 122.2(11) . . ?
C10 C9 C8B 102.6(8) . . ?
C8A C9 C8B 37.2(9) . . ?
C10 C9 H9AA 106.8 . . ?
C8A C9 H9AA 106.8 . . ?
C8B C9 H9AA 85.0 . . ?
C10 C9 H9BA 106.8 . . ?
C8A C9 H9BA 106.8 . . ?
C8B C9 H9BA 143.2 . . ?
H9AA C9 H9BA 106.6 . . ?
C10 C9 H9AB 122.1 . . ?
C8A C9 H9AB 111.1 . . ?
C8B C9 H9AB 106.8 . . ?
H9AA C9 H9AB 31.8 . . ?
H9BA C9 H9AB 75.4 . . ?
C10 C9 H9BB 106.0 . . ?
C8A C9 H9BB 72.2 . . ?
C8B C9 H9BB 108.1 . . ?
H9AA C9 H9BB 140.7 . . ?
H9BA C9 H9BB 42.4 . . ?
H9AB C9 H9BB 110.3 . . ?
C19 C18 C17 118.5(13) . . ?
C19 C18 H18A 107.7 . . ?
C17 C18 H18A 107.7 . . ?
C19 C18 H18B 107.7 . . ?
C17 C18 H18B 107.7 . . ?
H18A C18 H18B 107.1 . . ?
C16 C17 C18 117.4(13) . . ?
C16 C17 H17A 108.0 . . ?
C18 C17 H17A 108.0 . . ?
C16 C17 H17B 108.0 . . ?
C18 C17 H17B 108.0 . . ?
H17A C17 H17B 107.2 . . ?
C14 C13 C12 114.7(12) . . ?
C14 C13 H13A 108.6 . . ?
C12 C13 H13A 108.6 . . ?
C14 C13 H13B 108.6 . . ?
C12 C13 H13B 108.6 . . ?
H13A C13 H13B 107.6 . . ?
C2 N3 C4 105.8(8) . . ?
C2 N3 C24 124.5(10) . . ?
C4 N3 C24 129.7(11) . . ?
C21 C22 C23 111.6(19) . . ?
C21 C22 H22A 109.3 . . ?
C23 C22 H22A 109.3 . . ?
C21 C22 H22B 109.3 . . ?
C23 C22 H22B 109.3 . . ?
H22A C22 H22B 108.0 . . ?
C11 C12 C13 110.5(11) . . ?
C11 C12 H12A 109.5 . . ?
C13 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C13 C12 H12B 109.5 . . ?
H12A C12 H12B 108.1 . . ?
C9 C10 C11 113.7(12) . . ?
C9 C10 H10A 108.8 . . ?
C11 C10 H10A 108.8 . . ?
C9 C10 H10B 108.8 . . ?
C11 C10 H10B 108.8 . . ?
H10A C10 H10B 107.7 . . ?
C16 C15 C14 113.7(13) . . ?
C16 C15 H15A 108.8 . . ?
C14 C15 H15A 108.8 . . ?
C16 C15 H15B 108.8 . . ?
C14 C15 H15B 108.8 . . ?
H15A C15 H15B 107.7 . . ?
N3 C24 H24A 109.5 . . ?
N3 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N3 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C4 C5 N1 103.3(9) . . ?
C4 C5 H5 128.3 . . ?
N1 C5 H5 128.3 . . ?
C19 C20 C21 115.2(16) . . ?
C19 C20 H20A 108.5 . . ?
C21 C20 H20A 108.5 . . ?
C19 C20 H20B 108.5 . . ?
C21 C20 H20B 108.5 . . ?
H20A C20 H20B 107.5 . . ?
C15 C14 C13 113.6(12) . . ?
C15 C14 H14A 108.9 . . ?
C13 C14 H14A 108.9 . . ?
C15 C14 H14B 108.9 . . ?
C13 C14 H14B 108.9 . . ?
H14A C14 H14B 107.7 . . ?
C10 C11 C12 108.2(11) . . ?
C10 C11 H11A 110.0 . . ?
C12 C11 H11A 110.1 . . ?
C10 C11 H11B 110.0 . . ?
C12 C11 H11B 110.0 . . ?
H11A C11 H11B 108.4 . . ?
N3 C2 N1 108.9(9) . . ?
N3 C2 H2 125.6 . . ?
N1 C2 H2 125.6 . . ?
C20 C19 C18 116.1(15) . . ?
C20 C19 H19A 108.3 . . ?
C18 C19 H19A 108.3 . . ?
C20 C19 H19B 108.3 . . ?
C18 C19 H19B 108.3 . . ?
H19A C19 H19B 107.4 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C15 C16 C17 114.6(12) . . ?
C15 C16 H16A 108.6 . . ?
C17 C16 H16A 108.6 . . ?
C15 C16 H16B 108.6 . . ?
C17 C16 H16B 108.6 . . ?
H16A C16 H16B 107.6 . . ?
C5 C4 N3 109.9(9) . . ?
C5 C4 H4 125.0 . . ?
N3 C4 H4 125.0 . . ?
C8A C7A C6 119.3(12) . . ?
C8A C7A H7A1 107.5 . . ?
C6 C7A H7A1 107.5 . . ?
C8A C7A H7A2 107.5 . . ?
C6 C7A H7A2 107.5 . . ?
H7A1 C7A H7A2 107.0 . . ?
C9 C8A C7A 104.3(11) . . ?
C9 C8A H9BB 36.2 . . ?
C7A C8A H9BB 135.4 . . ?
C9 C8A H8A1 110.9 . . ?
C7A C8A H8A1 110.9 . . ?
H9BB C8A H8A1 80.4 . . ?
C9 C8A H8A2 110.9 . . ?
C7A C8A H8A2 110.9 . . ?
H9BB C8A H8A2 104.9 . . ?
H8A1 C8A H8A2 108.9 . . ?
C8B C7B C6 103.9(9) . . ?
C8B C7B H7B1 111.0 . . ?
C6 C7B H7B1 111.0 . . ?
C8B C7B H7B2 111.0 . . ?
C6 C7B H7B2 111.0 . . ?
H7B1 C7B H7B2 109.0 . . ?
C7B C8B C9 108.5(8) . . ?
C7B C8B H8B1 110.0 . . ?
C9 C8B H8B1 110.0 . . ?
C7B C8B H8B2 110.0 . . ?
C9 C8B H8B2 110.0 . . ?
H8B1 C8B H8B2 108.4 . . ?
N1 C6 C7A 116.1(10) . . ?
N1 C6 C7B 100.8(7) . . ?
C7A C6 C7B 33.4(9) . . ?
N1 C6 H6AA 108.3 . . ?
C7A C6 H6AA 108.3 . . ?
C7B C6 H6AA 140.8 . . ?
N1 C6 H6BA 108.3 . . ?
C7A C6 H6BA 108.3 . . ?
C7B C6 H6BA 87.1 . . ?
H6AA C6 H6BA 107.4 . . ?
N1 C6 H6AB 114.4 . . ?
C7A C6 H6AB 83.7 . . ?
C7B C6 H6AB 117.1 . . ?
H6AA C6 H6AB 25.7 . . ?
H6BA C6 H6AB 124.1 . . ?
N1 C6 H6BB 110.1 . . ?
C7A C6 H6BB 120.9 . . ?
C7B C6 H6BB 104.9 . . ?
H6AA C6 H6BB 89.4 . . ?
H6BA C6 H6BB 18.9 . . ?
H6AB C6 H6BB 108.9 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        24.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.048

#=END

data_C18MImAsF6-25oC
#TrackingRef '- SI-25oC.cif'

_database_code_depnum_ccdc_archive 'CCDC 843138'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            C18MImAsF6
_chemical_melting_point          351.1
_chemical_formula_moiety         
;
(C22 N2 H43 +), (As F6 -)
;
_chemical_formula_sum            'C22 H43 As F6 N2'
_chemical_formula_weight         524.50

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/a

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x-1/2, -y-1/2, z'

_cell_length_a                   9.5645(13)
_cell_length_b                   9.8620(15)
_cell_length_c                   28.969(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.400(3)
_cell_angle_gamma                90.00
_cell_volume                     2724.5(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    298
_cell_measurement_reflns_used    7481
_cell_measurement_theta_min      6.03
_cell_measurement_theta_max      54.90

_exptl_crystal_description       platelet
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1104
_exptl_absorpt_coefficient_mu    1.299
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4746
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'RAPID AUTO 2.40 (Rigaku 2006)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      298
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS RapidII'
_diffrn_measurement_method       'imaging plate'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20574
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_sigmaI/netI    0.0761
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4779
_reflns_number_gt                2370
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Rigaku R-AXIS Rapid-II'
_computing_cell_refinement       'RAPID AUTO 2.40 (Rigaku 2006)'
_computing_data_reduction        'RAPID AUTO 2.40 (Rigaku 2006)'
_computing_structure_solution    'SIR92 (Altmare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
This structure was solved based on the data at 25 deg C and the octadecyl chain
in this structure has a large conformational flexibility, which results in large
thermal motions of the atoms. Hence, the following restraints were applied.
The N-C and C-C bond lengths in the octadecyl chain were restrained using
the DFIX (1,2 C(N)-C distance: 1.54 A) and DANG (1,3 C(N)-C distance: 2.52 A)
commands in SHELXL. The N-C-C-C part of the trans structure was
weakly fixed using the FLAT command. Atomic displacement factors of the
disordered part and some carbon atoms in the octadecyl chain were restrained
using DELU and SIMU in SHELXL.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4779
_refine_ls_number_parameters     301
_refine_ls_number_restraints     99
_refine_ls_R_factor_all          0.1466
_refine_ls_R_factor_gt           0.0886
_refine_ls_wR_factor_ref         0.3324
_refine_ls_wR_factor_gt          0.2720
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.269
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As -0.15333(10) 0.02491(11) 0.10466(3) 0.1046(6) Uani 1 1 d . . .
F4 F -0.2335(10) -0.0440(9) 0.1486(3) 0.172(3) Uani 1 1 d . . .
F3 F -0.2872(8) 0.1313(8) 0.0964(4) 0.219(5) Uani 1 1 d . . .
F2 F -0.0776(9) 0.0855(14) 0.0586(3) 0.231(5) Uani 1 1 d . . .
F5 F -0.0221(7) -0.0887(8) 0.1131(3) 0.173(3) Uani 1 1 d . . .
N1 N 0.3891(9) -0.0108(8) 0.1097(3) 0.108(2) Uani 1 1 d D A .
F6 F -0.0584(9) 0.1300(8) 0.1400(3) 0.186(3) Uani 1 1 d . . .
F1 F -0.2444(6) -0.0871(9) 0.0685(2) 0.154(3) Uani 1 1 d . . .
C21 C -0.6413(14) -0.1503(11) 0.6696(4) 0.136(4) Uani 1 1 d D . .
H21A H -0.7278 -0.1356 0.6506 0.163 Uiso 1 1 calc R . .
H21B H -0.6280 -0.2475 0.6729 0.163 Uiso 1 1 calc R . .
C9 C 0.1525(11) -0.1392(13) 0.2406(5) 0.213(8) Uani 1 1 d DU . .
H9AA H 0.0879 -0.0735 0.2260 0.256 Uiso 0.733(17) 1 calc PR A 1
H9BA H 0.1083 -0.2272 0.2359 0.256 Uiso 0.733(17) 1 calc PR A 1
H9AB H 0.0694 -0.1238 0.2201 0.256 Uiso 0.267(17) 1 d PR A 2
H9BB H 0.1808 -0.2321 0.2394 0.256 Uiso 0.267(17) 1 d PR A 2
C18 C -0.3841(12) -0.0942(11) 0.5740(4) 0.124(3) Uani 1 1 d D . .
H18A H -0.2987 -0.1077 0.5938 0.149 Uiso 1 1 calc R . .
H18B H -0.3984 0.0028 0.5708 0.149 Uiso 1 1 calc R . .
C17 C -0.3619(12) -0.1527(10) 0.5261(3) 0.120(3) Uani 1 1 d D . .
H17A H -0.3487 -0.2498 0.5294 0.145 Uiso 1 1 calc R . .
H17B H -0.4475 -0.1387 0.5065 0.145 Uiso 1 1 calc R . .
C13 C -0.0921(11) -0.1603(10) 0.3831(3) 0.116(3) Uani 1 1 d D . .
H13A H -0.1790 -0.1459 0.3642 0.140 Uiso 1 1 calc R . .
H13B H -0.0788 -0.2574 0.3866 0.140 Uiso 1 1 calc R . .
N3 N 0.4041(9) -0.1185(8) 0.0487(3) 0.111(2) Uani 1 1 d . . .
C22 C -0.6560(17) -0.0913(19) 0.7160(5) 0.181(6) Uani 1 1 d D . .
H22A H -0.6651 0.0062 0.7128 0.217 Uiso 1 1 calc R . .
H22B H -0.5706 -0.1091 0.7353 0.217 Uiso 1 1 calc R . .
C12 C 0.0287(11) -0.1022(12) 0.3579(4) 0.123(3) Uani 1 1 d D A .
H12A H 0.0192 -0.0045 0.3555 0.148 Uiso 1 1 calc R . .
H12B H 0.1170 -0.1222 0.3753 0.148 Uiso 1 1 calc R . .
C10 C 0.1556(11) -0.1127(13) 0.2903(4) 0.173(6) Uani 1 1 d D A .
H10A H 0.1641 -0.0159 0.2957 0.208 Uiso 1 1 calc R . .
H10B H 0.2372 -0.1564 0.3058 0.208 Uiso 1 1 calc R . .
C15 C -0.2261(11) -0.1566(10) 0.4545(3) 0.116(3) Uani 1 1 d D . .
H15A H -0.3122 -0.1419 0.4352 0.139 Uiso 1 1 calc R . .
H15B H -0.2128 -0.2538 0.4577 0.139 Uiso 1 1 calc R . .
C24 C 0.4556(14) -0.2094(13) 0.0148(4) 0.144(4) Uani 1 1 d . . .
H24A H 0.4006 -0.1988 -0.0141 0.216 Uiso 1 1 calc R . .
H24B H 0.4485 -0.3013 0.0253 0.216 Uiso 1 1 calc R . .
H24C H 0.5519 -0.1887 0.0106 0.216 Uiso 1 1 calc R . .
C5 C 0.2805(13) 0.0340(12) 0.0818(5) 0.127(4) Uani 1 1 d . . .
H5 H 0.2116 0.0961 0.0883 0.152 Uiso 1 1 calc R . .
C20 C -0.5212(13) -0.0923(13) 0.6450(4) 0.136(4) Uani 1 1 d D . .
H20A H -0.5351 0.0047 0.6416 0.163 Uiso 1 1 calc R . .
H20B H -0.4349 -0.1062 0.6643 0.163 Uiso 1 1 calc R . .
C14 C -0.1053(11) -0.0986(11) 0.4301(4) 0.117(3) Uani 1 1 d D . .
H14A H -0.1183 -0.0015 0.4266 0.141 Uiso 1 1 calc R . .
H14B H -0.0188 -0.1135 0.4491 0.141 Uiso 1 1 calc R . .
C11 C 0.0284(11) -0.1629(11) 0.3100(4) 0.139(4) Uani 1 1 d D . .
H11A H 0.0297 -0.2612 0.3118 0.166 Uiso 1 1 calc R A .
H11B H -0.0546 -0.1349 0.2911 0.166 Uiso 1 1 calc R . .
C2 C 0.4569(9) -0.1100(9) 0.0921(4) 0.098(2) Uani 1 1 d D . .
H2 H 0.5270 -0.1634 0.1069 0.118 Uiso 1 1 calc R . .
C19 C -0.5043(12) -0.1520(11) 0.5983(3) 0.127(4) Uani 1 1 d D . .
H19A H -0.5904 -0.1378 0.5789 0.152 Uiso 1 1 calc R . .
H19B H -0.4907 -0.2491 0.6017 0.152 Uiso 1 1 calc R . .
C23 C -0.779(2) -0.1435(17) 0.7407(6) 0.209(7) Uani 1 1 d D . .
H23A H -0.8640 -0.1292 0.7216 0.314 Uiso 1 1 calc R . .
H23B H -0.7835 -0.0958 0.7695 0.314 Uiso 1 1 calc R . .
H23C H -0.7668 -0.2387 0.7468 0.314 Uiso 1 1 calc R . .
C16 C -0.2430(11) -0.0976(11) 0.5016(3) 0.118(3) Uani 1 1 d D . .
H16A H -0.1568 -0.1127 0.5208 0.142 Uiso 1 1 calc R . .
H16B H -0.2553 -0.0003 0.4983 0.142 Uiso 1 1 calc R . .
C4 C 0.2952(13) -0.0320(12) 0.0424(5) 0.126(4) Uani 1 1 d . . .
H4 H 0.2393 -0.0205 0.0149 0.151 Uiso 1 1 calc R . .
C7A C 0.2846(15) 0.0016(15) 0.1921(4) 0.124(5) Uani 0.733(17) 1 d PDU A 1
H7A1 H 0.1948 0.0238 0.1760 0.149 Uiso 0.733(17) 1 calc PR A 1
H7A2 H 0.3012 0.0658 0.2172 0.149 Uiso 0.733(17) 1 calc PR A 1
C8A C 0.2750(19) -0.1404(16) 0.2126(6) 0.175(7) Uani 0.733(17) 1 d PDU A 1
H8A1 H 0.2628 -0.2076 0.1882 0.209 Uiso 0.733(17) 1 calc PR A 1
H8A2 H 0.3596 -0.1616 0.2319 0.209 Uiso 0.733(17) 1 calc PR A 1
C7B C 0.294(3) -0.096(2) 0.1769(5) 0.145(9) Uani 0.267(17) 1 d PDU A 2
H7B1 H 0.2009 -0.0883 0.1616 0.174 Uiso 0.267(17) 1 calc PR A 2
H7B2 H 0.3314 -0.1853 0.1707 0.174 Uiso 0.267(17) 1 calc PR A 2
C8B C 0.293(2) -0.073(3) 0.2268(6) 0.168(10) Uani 0.267(17) 1 d PDU A 2
H8B1 H 0.2941 0.0236 0.2337 0.202 Uiso 0.267(17) 1 calc PR A 2
H8B2 H 0.3733 -0.1150 0.2435 0.202 Uiso 0.267(17) 1 calc PR A 2
C6 C 0.3940(11) 0.0192(12) 0.1599(4) 0.141(4) Uani 1 1 d DU . .
H6AA H 0.4737 -0.0316 0.1734 0.169 Uiso 0.733(17) 1 calc PR A 1
H6BA H 0.4205 0.1140 0.1625 0.169 Uiso 0.733(17) 1 calc PR A 1
H6AB H 0.3659 0.1101 0.1660 0.169 Uiso 0.267(17) 1 d PR A 2
H6BB H 0.4894 0.0058 0.1722 0.169 Uiso 0.267(17) 1 d PR A 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
As1 0.0994(8) 0.1003(9) 0.1155(9) 0.0038(5) 0.0165(6) -0.0001(5)
F4 0.194(7) 0.204(8) 0.123(5) 0.020(5) 0.041(5) -0.029(6)
F3 0.143(5) 0.139(6) 0.372(14) 0.023(8) 0.000(7) 0.050(5)
F2 0.169(7) 0.337(13) 0.187(8) 0.111(9) 0.019(6) -0.080(9)
F5 0.135(5) 0.146(6) 0.231(8) -0.040(6) -0.023(5) 0.040(5)
N1 0.104(5) 0.101(6) 0.118(6) 0.016(5) 0.008(5) -0.017(4)
F6 0.182(7) 0.131(6) 0.240(9) -0.063(6) -0.010(6) -0.022(5)
F1 0.117(4) 0.201(7) 0.146(5) -0.057(5) 0.022(4) -0.026(5)
C21 0.182(11) 0.106(8) 0.119(8) -0.011(6) 0.002(8) 0.012(8)
C9 0.105(8) 0.205(14) 0.332(19) 0.148(14) 0.042(10) -0.013(9)
C18 0.137(8) 0.100(7) 0.134(8) -0.014(6) 0.003(7) -0.010(7)
C17 0.149(9) 0.087(7) 0.122(7) -0.018(5) -0.014(7) 0.010(6)
C13 0.126(7) 0.086(7) 0.136(8) 0.002(6) 0.006(6) -0.006(5)
N3 0.108(6) 0.094(6) 0.133(7) 0.017(5) 0.017(5) -0.025(5)
C22 0.202(15) 0.180(14) 0.162(13) -0.050(11) 0.025(12) -0.018(13)
C12 0.117(7) 0.110(8) 0.142(9) 0.017(7) 0.007(7) -0.010(6)
C10 0.138(10) 0.170(13) 0.211(15) 0.075(12) 0.010(10) -0.020(9)
C15 0.138(8) 0.093(7) 0.117(7) -0.011(5) 0.014(6) 0.007(6)
C24 0.177(11) 0.115(9) 0.148(9) -0.015(8) 0.054(8) -0.021(8)
C5 0.119(8) 0.123(9) 0.138(10) 0.019(8) 0.012(8) 0.017(7)
C20 0.161(10) 0.108(8) 0.136(9) -0.018(7) 0.007(8) 0.003(8)
C14 0.122(7) 0.096(7) 0.133(8) 0.014(6) 0.005(6) -0.011(6)
C11 0.117(8) 0.107(8) 0.194(13) 0.023(8) 0.023(8) -0.024(6)
C2 0.099(6) 0.089(7) 0.108(7) 0.012(5) 0.015(5) 0.000(5)
C19 0.155(9) 0.097(7) 0.124(8) -0.013(6) -0.014(7) 0.009(7)
C23 0.28(2) 0.167(15) 0.192(15) 0.005(12) 0.076(16) 0.000(14)
C16 0.123(7) 0.087(7) 0.145(9) 0.002(6) 0.003(7) -0.011(6)
C4 0.121(8) 0.116(9) 0.139(10) 0.028(7) -0.003(7) 0.005(7)
C7A 0.124(10) 0.142(12) 0.111(10) 0.025(8) 0.030(7) -0.003(8)
C8A 0.154(12) 0.134(13) 0.237(17) 0.032(11) 0.031(11) -0.020(11)
C7B 0.123(18) 0.086(18) 0.232(19) -0.017(18) 0.040(16) 0.023(14)
C8B 0.148(17) 0.15(2) 0.215(17) 0.091(18) 0.046(18) -0.045(18)
C6 0.135(9) 0.145(10) 0.148(10) 0.014(7) 0.056(7) 0.014(7)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
As1 F3 1.658(7) . ?
As1 F6 1.675(7) . ?
As1 F2 1.676(8) . ?
As1 F4 1.681(7) . ?
As1 F5 1.686(7) . ?
As1 F1 1.713(6) . ?
N1 C2 1.298(5) . ?
N1 C5 1.341(14) . ?
N1 C6 1.482(11) . ?
C21 C22 1.481(12) . ?
C21 C20 1.511(12) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C9 C10 1.461(10) . ?
C9 C8A 1.474(10) . ?
C9 C8B 1.572(5) . ?
C9 H9AA 0.9700 . ?
C9 H9BA 0.9700 . ?
C9 H9AB 0.9677 . ?
C9 H9BB 0.9560 . ?
C18 C19 1.505(11) . ?
C18 C17 1.533(11) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C17 C16 1.490(11) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C13 C14 1.505(11) . ?
C13 C12 1.525(11) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
N3 C2 1.323(12) . ?
N3 C4 1.348(13) . ?
N3 C24 1.444(14) . ?
C22 C23 1.512(10) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C12 C11 1.510(12) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C10 C11 1.469(9) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C15 C16 1.503(11) . ?
C15 C14 1.513(11) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C5 C4 1.331(16) . ?
C5 H5 0.9300 . ?
C20 C19 1.496(11) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C2 H2 0.9300 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C4 H4 0.9300 . ?
C7A C6 1.465(9) . ?
C7A C8A 1.527(11) . ?
C7A H7A1 0.9700 . ?
C7A H7A2 0.9700 . ?
C7A H6AB 1.5527 . ?
C8A H9BB 1.5282 . ?
C8A H8A1 0.9700 . ?
C8A H8A2 0.9700 . ?
C7B C8B 1.467(8) . ?
C7B C6 1.585(6) . ?
C7B H7B1 0.9700 . ?
C7B H7B2 0.9700 . ?
C8B H8B1 0.9700 . ?
C8B H8B2 0.9700 . ?
C6 H6AA 0.9700 . ?
C6 H6BA 0.9700 . ?
C6 H6AB 0.9560 . ?
C6 H6BB 0.9635 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F3 As1 F6 94.2(5) . . ?
F3 As1 F2 92.0(6) . . ?
F6 As1 F2 91.0(5) . . ?
F3 As1 F4 88.5(5) . . ?
F6 As1 F4 92.6(5) . . ?
F2 As1 F4 176.3(5) . . ?
F3 As1 F5 177.6(4) . . ?
F6 As1 F5 87.7(4) . . ?
F2 As1 F5 89.5(5) . . ?
F4 As1 F5 89.9(5) . . ?
F3 As1 F1 88.2(4) . . ?
F6 As1 F1 177.6(4) . . ?
F2 As1 F1 88.5(5) . . ?
F4 As1 F1 87.9(4) . . ?
F5 As1 F1 89.9(4) . . ?
C2 N1 C5 113.6(9) . . ?
C2 N1 C6 123.7(9) . . ?
C5 N1 C6 119.4(9) . . ?
C22 C21 C20 114.1(11) . . ?
C22 C21 H21A 108.7 . . ?
C20 C21 H21A 108.7 . . ?
C22 C21 H21B 108.7 . . ?
C20 C21 H21B 108.7 . . ?
H21A C21 H21B 107.6 . . ?
C10 C9 C8A 125.8(11) . . ?
C10 C9 C8B 102.8(7) . . ?
C8A C9 C8B 30.1(9) . . ?
C10 C9 H9AA 105.9 . . ?
C8A C9 H9AA 105.9 . . ?
C8B C9 H9AA 98.0 . . ?
C10 C9 H9BA 105.9 . . ?
C8A C9 H9BA 105.9 . . ?
C8B C9 H9BA 135.2 . . ?
H9AA C9 H9BA 106.2 . . ?
C10 C9 H9AB 122.1 . . ?
C8A C9 H9AB 108.3 . . ?
C8B C9 H9AB 117.1 . . ?
H9AA C9 H9AB 32.9 . . ?
H9BA C9 H9AB 74.1 . . ?
C10 C9 H9BB 102.9 . . ?
C8A C9 H9BB 74.6 . . ?
C8B C9 H9BB 98.1 . . ?
H9AA C9 H9BB 142.7 . . ?
H9BA C9 H9BB 42.3 . . ?
H9AB C9 H9BB 110.4 . . ?
C19 C18 C17 116.4(9) . . ?
C19 C18 H18A 108.2 . . ?
C17 C18 H18A 108.2 . . ?
C19 C18 H18B 108.2 . . ?
C17 C18 H18B 108.2 . . ?
H18A C18 H18B 107.3 . . ?
C16 C17 C18 117.3(9) . . ?
C16 C17 H17A 108.0 . . ?
C18 C17 H17A 108.0 . . ?
C16 C17 H17B 108.0 . . ?
C18 C17 H17B 108.0 . . ?
H17A C17 H17B 107.2 . . ?
C14 C13 C12 113.6(9) . . ?
C14 C13 H13A 108.8 . . ?
C12 C13 H13A 108.8 . . ?
C14 C13 H13B 108.8 . . ?
C12 C13 H13B 108.8 . . ?
H13A C13 H13B 107.7 . . ?
C2 N3 C4 108.9(10) . . ?
C2 N3 C24 124.2(10) . . ?
C4 N3 C24 126.9(11) . . ?
C21 C22 C23 115.3(13) . . ?
C21 C22 H22A 108.4 . . ?
C23 C22 H22A 108.4 . . ?
C21 C22 H22B 108.4 . . ?
C23 C22 H22B 108.4 . . ?
H22A C22 H22B 107.5 . . ?
C11 C12 C13 110.1(9) . . ?
C11 C12 H12A 109.6 . . ?
C13 C12 H12A 109.6 . . ?
C11 C12 H12B 109.6 . . ?
C13 C12 H12B 109.6 . . ?
H12A C12 H12B 108.2 . . ?
C9 C10 C11 111.6(10) . . ?
C9 C10 H10A 109.3 . . ?
C11 C10 H10A 109.3 . . ?
C9 C10 H10B 109.3 . . ?
C11 C10 H10B 109.3 . . ?
H10A C10 H10B 108.0 . . ?
C16 C15 C14 114.6(9) . . ?
C16 C15 H15A 108.6 . . ?
C14 C15 H15A 108.6 . . ?
C16 C15 H15B 108.6 . . ?
C14 C15 H15B 108.6 . . ?
H15A C15 H15B 107.6 . . ?
N3 C24 H24A 109.5 . . ?
N3 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N3 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C4 C5 N1 103.2(11) . . ?
C4 C5 H5 128.4 . . ?
N1 C5 H5 128.4 . . ?
C19 C20 C21 114.6(10) . . ?
C19 C20 H20A 108.6 . . ?
C21 C20 H20A 108.6 . . ?
C19 C20 H20B 108.6 . . ?
C21 C20 H20B 108.6 . . ?
H20A C20 H20B 107.6 . . ?
C13 C14 C15 113.0(8) . . ?
C13 C14 H14A 109.0 . . ?
C15 C14 H14A 109.0 . . ?
C13 C14 H14B 109.0 . . ?
C15 C14 H14B 109.0 . . ?
H14A C14 H14B 107.8 . . ?
C10 C11 C12 106.3(9) . . ?
C10 C11 H11A 110.5 . . ?
C12 C11 H11A 110.5 . . ?
C10 C11 H11B 110.5 . . ?
C12 C11 H11B 110.5 . . ?
H11A C11 H11B 108.7 . . ?
N1 C2 N3 104.7(8) . . ?
N1 C2 H2 127.6 . . ?
N3 C2 H2 127.6 . . ?
C20 C19 C18 114.4(9) . . ?
C20 C19 H19A 108.7 . . ?
C18 C19 H19A 108.7 . . ?
C20 C19 H19B 108.7 . . ?
C18 C19 H19B 108.7 . . ?
H19A C19 H19B 107.6 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C17 C16 C15 115.5(8) . . ?
C17 C16 H16A 108.4 . . ?
C15 C16 H16A 108.4 . . ?
C17 C16 H16B 108.4 . . ?
C15 C16 H16B 108.4 . . ?
H16A C16 H16B 107.5 . . ?
C5 C4 N3 109.0(11) . . ?
C5 C4 H4 125.5 . . ?
N3 C4 H4 125.5 . . ?
C6 C7A C8A 115.1(10) . . ?
C6 C7A H7A1 108.5 . . ?
C8A C7A H7A1 108.5 . . ?
C6 C7A H7A2 108.5 . . ?
C8A C7A H7A2 108.5 . . ?
H7A1 C7A H7A2 107.5 . . ?
C6 C7A H6AB 36.8 . . ?
C8A C7A H6AB 150.4 . . ?
H7A1 C7A H6AB 93.9 . . ?
H7A2 C7A H6AB 81.7 . . ?
C9 C8A C7A 106.3(10) . . ?
C9 C8A H9BB 37.1 . . ?
C7A C8A H9BB 142.7 . . ?
C9 C8A H8A1 110.5 . . ?
C7A C8A H8A1 110.5 . . ?
H9BB C8A H8A1 85.5 . . ?
C9 C8A H8A2 110.5 . . ?
C7A C8A H8A2 110.5 . . ?
H9BB C8A H8A2 94.6 . . ?
H8A1 C8A H8A2 108.7 . . ?
C8B C7B C6 104.2(11) . . ?
C8B C7B H7B1 110.9 . . ?
C6 C7B H7B1 110.9 . . ?
C8B C7B H7B2 110.9 . . ?
C6 C7B H7B2 110.9 . . ?
H7B1 C7B H7B2 108.9 . . ?
C7B C8B C9 105.0(8) . . ?
C7B C8B H8B1 110.8 . . ?
C9 C8B H8B1 110.8 . . ?
C7B C8B H8B2 110.8 . . ?
C9 C8B H8B2 110.8 . . ?
H8B1 C8B H8B2 108.8 . . ?
C7A C6 N1 129.2(10) . . ?
C7A C6 C7B 40.7(10) . . ?
N1 C6 C7B 100.8(7) . . ?
C7A C6 H6AA 105.0 . . ?
N1 C6 H6AA 105.0 . . ?
C7B C6 H6AA 88.6 . . ?
C7A C6 H6BA 105.0 . . ?
N1 C6 H6BA 105.0 . . ?
C7B C6 H6BA 145.7 . . ?
H6AA C6 H6BA 105.9 . . ?
C7A C6 H6AB 76.6 . . ?
N1 C6 H6AB 112.4 . . ?
C7B C6 H6AB 115.5 . . ?
H6AA C6 H6AB 129.2 . . ?
H6BA C6 H6AB 32.6 . . ?
C7A C6 H6BB 116.8 . . ?
N1 C6 H6BB 107.1 . . ?
C7B C6 H6BB 111.2 . . ?
H6AA C6 H6BB 23.9 . . ?
H6BA C6 H6BB 82.4 . . ?
H6AB C6 H6BB 109.4 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.867
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.087

#=END

data_C18MImSbF6-25oC
#TrackingRef '- SI-25oC.cif'

_database_code_depnum_ccdc_archive 'CCDC 843139'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            C18MImSbF6
_chemical_melting_point          347.5
_chemical_formula_moiety         
;
(C22 N2 H43 +), (Sb F6 -)
;
_chemical_formula_sum            'C22 H43 F6 N2 Sb'
_chemical_formula_weight         571.33

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/a

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x-1/2, -y-1/2, z'

_cell_length_a                   9.6973(7)
_cell_length_b                   9.9933(7)
_cell_length_c                   28.991(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.2424(16)
_cell_angle_gamma                90.00
_cell_volume                     2797.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    298
_cell_measurement_reflns_used    12905
_cell_measurement_theta_min      6.12
_cell_measurement_theta_max      54.95

_exptl_crystal_description       platelet
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1176
_exptl_absorpt_coefficient_mu    1.036
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4337
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'RAPID AUTO 2.40 (Rigaku 2006)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      298
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS RapidII'
_diffrn_measurement_method       'imaging plate'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21577
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0258
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         3.06
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4925
_reflns_number_gt                2763
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Rigaku R-AXIS Rapid-II'
_computing_cell_refinement       'RAPID AUTO 2.40 (Rigaku 2006)'
_computing_data_reduction        'RAPID AUTO 2.40 (Rigaku 2006)'
_computing_structure_solution    'SIR92 (Altmare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
This structure was solved based on the data at 25 deg C and the octadecyl chain
in this structure has a large conformational flexibility, which results in large
thermal motions of the atoms. Hence, the following restraints were applied.
The N-C and C-C bond lengths in the octadecyl chain were restrained using
the DFIX (1,2 C(N)-C distance: 1.54 A) and DANG (1,3 C(N)-C distance: 2.52 A)
commands in SHELXL. The N-C-C-C part of the trans structure was
weakly fixed using the FLAT command. Atomic displacement factors of the
disordered part and some carbon atoms in the octadecyl chain were restrained
using DELU and SIMU in SHELXL.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0990P)^2^+0.2202P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4925
_refine_ls_number_parameters     301
_refine_ls_number_restraints     99
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0500
_refine_ls_wR_factor_ref         0.1770
_refine_ls_wR_factor_gt          0.1514
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.229
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sb1 Sb -0.15393(5) 0.02913(5) 0.107611(17) 0.1124(3) Uani 1 1 d . . .
F4 F -0.2408(8) -0.0475(7) 0.1547(2) 0.192(3) Uani 1 1 d . . .
F3 F -0.2998(7) 0.1417(6) 0.0977(3) 0.233(3) Uani 1 1 d . . .
F2 F -0.0748(7) 0.0975(11) 0.0580(2) 0.247(4) Uani 1 1 d . . .
F5 F -0.0129(6) -0.0929(6) 0.1170(3) 0.192(3) Uani 1 1 d . . .
N1 N 0.3837(7) -0.0186(7) 0.1138(2) 0.1149(18) Uani 1 1 d D A .
F6 F -0.0520(7) 0.1429(6) 0.1463(2) 0.198(2) Uani 1 1 d . . .
F1 F -0.2513(5) -0.0909(7) 0.0682(2) 0.1695(19) Uani 1 1 d . . .
C21 C -0.6461(11) -0.1513(9) 0.6669(3) 0.153(3) Uani 1 1 d D . .
H21A H -0.6301 -0.2466 0.6708 0.184 Uiso 1 1 calc R . .
H21B H -0.7309 -0.1402 0.6468 0.184 Uiso 1 1 calc R . .
C9 C 0.1641(9) -0.1483(10) 0.2450(4) 0.209(6) Uani 1 1 d DU . .
H9AA H 0.1373 -0.2418 0.2441 0.251 Uiso 0.572(14) 1 calc PR A 1
H9BA H 0.0907 -0.1005 0.2269 0.251 Uiso 0.572(14) 1 calc PR A 1
H9AB H 0.0810 -0.1328 0.2244 0.251 Uiso 0.428(14) 1 d PR A 2
H9BB H 0.1924 -0.2411 0.2437 0.251 Uiso 0.428(14) 1 d PR A 2
C18 C -0.3897(9) -0.0942(8) 0.5738(3) 0.135(3) Uani 1 1 d D . .
H18A H -0.3052 -0.1043 0.5941 0.163 Uiso 1 1 calc R . .
H18B H -0.4068 0.0009 0.5697 0.163 Uiso 1 1 calc R . .
C17 C -0.3671(9) -0.1542(7) 0.5271(3) 0.134(3) Uani 1 1 d D . .
H17A H -0.3508 -0.2494 0.5313 0.161 Uiso 1 1 calc R . .
H17B H -0.4518 -0.1438 0.5069 0.161 Uiso 1 1 calc R . .
C13 C -0.0894(8) -0.1599(7) 0.3871(3) 0.136(3) Uani 1 1 d D . .
H13A H -0.1746 -0.1472 0.3674 0.163 Uiso 1 1 calc R . .
H13B H -0.0755 -0.2555 0.3910 0.163 Uiso 1 1 calc R . .
N3 N 0.4026(7) -0.1193(6) 0.0510(2) 0.1213(18) Uani 1 1 d . . .
C22 C -0.6673(15) -0.0924(13) 0.7131(4) 0.198(5) Uani 1 1 d D . .
H22A H -0.6816 0.0031 0.7092 0.238 Uiso 1 1 calc R . .
H22B H -0.5829 -0.1048 0.7333 0.238 Uiso 1 1 calc R . .
C12 C 0.0287(9) -0.1040(9) 0.3626(4) 0.146(3) Uani 1 1 d D A .
H12A H 0.0175 -0.0078 0.3597 0.175 Uiso 1 1 calc R . .
H12B H 0.1149 -0.1207 0.3814 0.175 Uiso 1 1 calc R . .
C10 C 0.1573(9) -0.1047(11) 0.2934(3) 0.185(5) Uani 1 1 d D A .
H10A H 0.1511 -0.0079 0.2941 0.222 Uiso 1 1 calc R . .
H10B H 0.2425 -0.1303 0.3113 0.222 Uiso 1 1 calc R . .
C15 C -0.2264(8) -0.1568(7) 0.4571(3) 0.132(2) Uani 1 1 d D . .
H15A H -0.3103 -0.1459 0.4366 0.158 Uiso 1 1 calc R . .
H15B H -0.2111 -0.2520 0.4615 0.158 Uiso 1 1 calc R . .
C24 C 0.4571(10) -0.2085(9) 0.0161(3) 0.155(3) Uani 1 1 d . . .
H24A H 0.4491 -0.1648 -0.0135 0.232 Uiso 1 1 calc R . .
H24B H 0.4047 -0.2901 0.0141 0.232 Uiso 1 1 calc R . .
H24C H 0.5526 -0.2282 0.0251 0.232 Uiso 1 1 calc R . .
C5 C 0.2851(11) 0.0321(9) 0.0850(4) 0.140(3) Uani 1 1 d . . .
H5 H 0.2212 0.0975 0.0913 0.168 Uiso 1 1 calc R . .
C20 C -0.5299(10) -0.0933(10) 0.6435(3) 0.147(3) Uani 1 1 d D . .
H20A H -0.4455 -0.1030 0.6639 0.176 Uiso 1 1 calc R . .
H20B H -0.5468 0.0018 0.6392 0.176 Uiso 1 1 calc R . .
C14 C -0.1078(9) -0.1001(7) 0.4337(3) 0.129(2) Uani 1 1 d D . .
H14A H -0.0232 -0.1135 0.4537 0.154 Uiso 1 1 calc R . .
H14B H -0.1215 -0.0045 0.4300 0.154 Uiso 1 1 calc R . .
C11 C 0.0386(8) -0.1618(9) 0.3157(4) 0.147(3) Uani 1 1 d D . .
H11A H 0.0494 -0.2581 0.3183 0.177 Uiso 1 1 calc R A .
H11B H -0.0465 -0.1438 0.2965 0.177 Uiso 1 1 calc R . .
C2 C 0.4534(7) -0.1110(7) 0.0953(3) 0.113(2) Uani 1 1 d D . .
H2 H 0.5249 -0.1618 0.1100 0.136 Uiso 1 1 calc R . .
C19 C -0.5064(9) -0.1537(8) 0.5970(3) 0.138(3) Uani 1 1 d D . .
H19A H -0.4889 -0.2487 0.6013 0.166 Uiso 1 1 calc R . .
H19B H -0.5907 -0.1442 0.5766 0.166 Uiso 1 1 calc R . .
C23 C -0.7858(15) -0.1484(14) 0.7369(4) 0.225(6) Uani 1 1 d D . .
H23A H -0.8655 -0.1575 0.7149 0.338 Uiso 1 1 calc R . .
H23B H -0.8071 -0.0890 0.7613 0.338 Uiso 1 1 calc R . .
H23C H -0.7605 -0.2345 0.7497 0.338 Uiso 1 1 calc R . .
C16 C -0.2496(8) -0.0963(8) 0.5030(3) 0.128(2) Uani 1 1 d D . .
H16A H -0.2664 -0.0013 0.4986 0.154 Uiso 1 1 calc R . .
H16B H -0.1651 -0.1058 0.5234 0.154 Uiso 1 1 calc R . .
C4 C 0.2953(11) -0.0285(10) 0.0455(4) 0.143(3) Uani 1 1 d . . .
H4 H 0.2395 -0.0130 0.0182 0.171 Uiso 1 1 calc R . .
C7A C 0.2919(14) -0.0037(14) 0.1953(4) 0.123(5) Uani 0.572(14) 1 d PDU A 1
H7A1 H 0.2034 0.0128 0.1779 0.148 Uiso 0.572(14) 1 calc PR A 1
H7A2 H 0.3043 0.0641 0.2193 0.148 Uiso 0.572(14) 1 calc PR A 1
C8A C 0.2860(17) -0.1392(14) 0.2184(6) 0.174(6) Uani 0.572(14) 1 d PDU A 1
H8A1 H 0.2815 -0.2089 0.1950 0.208 Uiso 0.572(14) 1 calc PR A 1
H8A2 H 0.3694 -0.1528 0.2390 0.208 Uiso 0.572(14) 1 calc PR A 1
C7B C 0.3131(18) -0.1026(13) 0.1839(4) 0.137(6) Uani 0.428(14) 1 d PDU A 2
H7B1 H 0.2307 -0.1207 0.1633 0.165 Uiso 0.428(14) 1 calc PR A 2
H7B2 H 0.3668 -0.1842 0.1883 0.165 Uiso 0.428(14) 1 calc PR A 2
C8B C 0.2764(18) -0.0503(14) 0.2284(5) 0.144(6) Uani 0.428(14) 1 d PDU A 2
H8B1 H 0.2393 0.0396 0.2248 0.173 Uiso 0.428(14) 1 calc PR A 2
H8B2 H 0.3572 -0.0481 0.2508 0.173 Uiso 0.428(14) 1 calc PR A 2
C6 C 0.4018(10) 0.0126(9) 0.1640(3) 0.147(3) Uani 1 1 d DU . .
H6AA H 0.4796 -0.0406 0.1769 0.176 Uiso 0.572(14) 1 calc PR A 1
H6BA H 0.4310 0.1054 0.1665 0.176 Uiso 0.572(14) 1 calc PR A 1
H6AB H 0.3737 0.1035 0.1701 0.176 Uiso 0.428(14) 1 d PR A 2
H6BB H 0.4973 -0.0008 0.1763 0.176 Uiso 0.428(14) 1 d PR A 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Sb1 0.1090(4) 0.1098(4) 0.1202(4) 0.0054(2) 0.0203(3) -0.0004(2)
F4 0.217(7) 0.212(6) 0.147(4) 0.024(4) 0.027(4) -0.044(5)
F3 0.165(5) 0.156(5) 0.380(11) 0.037(6) 0.028(6) 0.044(4)
F2 0.194(6) 0.376(11) 0.177(5) 0.072(7) 0.045(4) -0.086(7)
F5 0.158(4) 0.157(4) 0.252(7) -0.035(5) -0.035(4) 0.029(4)
N1 0.108(4) 0.114(4) 0.125(5) 0.022(4) 0.026(4) -0.012(3)
F6 0.211(6) 0.148(4) 0.233(6) -0.047(4) 0.004(5) -0.032(4)
F1 0.124(3) 0.210(5) 0.175(4) -0.053(4) 0.016(3) -0.012(4)
C21 0.197(10) 0.116(6) 0.143(7) -0.009(5) -0.008(6) -0.005(6)
C9 0.136(7) 0.195(10) 0.306(13) 0.134(11) 0.072(8) 0.001(7)
C18 0.153(7) 0.096(5) 0.151(7) -0.011(5) -0.021(5) -0.006(5)
C17 0.159(7) 0.089(4) 0.150(6) -0.007(4) -0.016(5) 0.002(5)
C13 0.135(6) 0.087(4) 0.181(8) 0.002(5) -0.007(5) -0.009(4)
N3 0.121(5) 0.108(4) 0.136(5) 0.018(4) 0.016(4) -0.030(4)
C22 0.257(15) 0.174(10) 0.159(9) -0.035(8) 0.000(9) -0.025(11)
C12 0.128(6) 0.104(6) 0.202(9) 0.024(6) -0.007(6) -0.017(5)
C10 0.121(7) 0.181(9) 0.252(12) 0.104(10) 0.015(7) -0.026(7)
C15 0.149(7) 0.088(4) 0.151(6) -0.012(4) -0.020(5) 0.000(5)
C24 0.193(8) 0.128(6) 0.146(6) -0.014(6) 0.026(6) -0.037(6)
C5 0.128(7) 0.130(7) 0.162(9) 0.033(7) 0.008(7) 0.014(5)
C20 0.170(8) 0.118(6) 0.147(7) -0.011(6) -0.023(6) -0.010(6)
C14 0.141(6) 0.089(4) 0.151(6) 0.004(5) -0.015(5) -0.015(4)
C11 0.123(6) 0.113(6) 0.206(9) 0.029(6) 0.018(6) -0.013(5)
C2 0.103(5) 0.107(5) 0.130(6) 0.017(4) 0.013(4) -0.007(4)
C19 0.167(8) 0.101(5) 0.142(6) -0.014(5) -0.015(5) 0.000(5)
C23 0.272(16) 0.219(14) 0.189(11) 0.006(10) 0.045(11) -0.020(12)
C16 0.140(6) 0.091(4) 0.148(6) 0.002(4) -0.019(5) -0.010(4)
C4 0.139(8) 0.138(7) 0.147(8) 0.035(6) -0.005(6) -0.009(6)
C7A 0.124(9) 0.139(10) 0.113(9) 0.027(7) 0.041(7) 0.012(8)
C8A 0.145(11) 0.116(10) 0.268(17) 0.044(11) 0.064(10) 0.003(10)
C7B 0.152(13) 0.092(11) 0.173(13) -0.036(10) 0.040(10) 0.003(9)
C8B 0.170(14) 0.090(12) 0.182(13) 0.022(10) 0.065(12) -0.003(10)
C6 0.141(7) 0.157(7) 0.149(7) 0.020(5) 0.049(6) 0.006(5)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sb1 F3 1.810(6) . ?
Sb1 F6 1.823(6) . ?
Sb1 F2 1.823(6) . ?
Sb1 F5 1.834(6) . ?
Sb1 F4 1.837(6) . ?
Sb1 F1 1.854(5) . ?
N1 C2 1.290(7) . ?
N1 C5 1.312(12) . ?
N1 C6 1.484(10) . ?
C21 C20 1.486(10) . ?
C21 C22 1.494(10) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C9 C8A 1.471(9) . ?
C9 C10 1.478(8) . ?
C9 C8B 1.571(5) . ?
C9 H9AA 0.9700 . ?
C9 H9BA 0.9700 . ?
C9 H9AB 0.9696 . ?
C9 H9BB 0.9689 . ?
C18 C19 1.492(9) . ?
C18 C17 1.513(9) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C17 C16 1.505(9) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C13 C14 1.501(9) . ?
C13 C12 1.511(10) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
N3 C2 1.335(9) . ?
N3 C4 1.379(11) . ?
N3 C24 1.481(10) . ?
C22 C23 1.501(10) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C12 C11 1.488(10) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C10 C11 1.484(8) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C15 C16 1.497(9) . ?
C15 C14 1.499(9) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C5 C4 1.307(13) . ?
C5 H5 0.9300 . ?
C20 C19 1.512(10) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C2 H2 0.9300 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C4 H4 0.9300 . ?
C7A C6 1.470(9) . ?
C7A C8A 1.514(11) . ?
C7A H7A1 0.9700 . ?
C7A H7A2 0.9700 . ?
C7A H6AB 1.5540 . ?
C8A H9BB 1.5884 . ?
C8A H8A1 0.9700 . ?
C8A H8A2 0.9700 . ?
C7B C8B 1.465(8) . ?
C7B C6 1.578(6) . ?
C7B H7B1 0.9700 . ?
C7B H7B2 0.9700 . ?
C8B H8B1 0.9700 . ?
C8B H8B2 0.9700 . ?
C6 H6AA 0.9700 . ?
C6 H6BA 0.9700 . ?
C6 H6AB 0.9690 . ?
C6 H6BB 0.9705 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F3 Sb1 F6 94.7(4) . . ?
F3 Sb1 F2 91.2(4) . . ?
F6 Sb1 F2 90.4(4) . . ?
F3 Sb1 F5 176.8(3) . . ?
F6 Sb1 F5 88.2(3) . . ?
F2 Sb1 F5 90.2(4) . . ?
F3 Sb1 F4 88.4(4) . . ?
F6 Sb1 F4 93.6(3) . . ?
F2 Sb1 F4 176.0(3) . . ?
F5 Sb1 F4 89.9(4) . . ?
F3 Sb1 F1 87.6(3) . . ?
F6 Sb1 F1 177.7(3) . . ?
F2 Sb1 F1 89.1(3) . . ?
F5 Sb1 F1 89.6(3) . . ?
F4 Sb1 F1 86.9(3) . . ?
C2 N1 C5 113.1(8) . . ?
C2 N1 C6 122.5(8) . . ?
C5 N1 C6 123.9(9) . . ?
C20 C21 C22 115.4(9) . . ?
C20 C21 H21A 108.4 . . ?
C22 C21 H21A 108.4 . . ?
C20 C21 H21B 108.4 . . ?
C22 C21 H21B 108.4 . . ?
H21A C21 H21B 107.5 . . ?
C8A C9 C10 126.0(9) . . ?
C8A C9 C8B 35.9(6) . . ?
C10 C9 C8B 101.5(6) . . ?
C8A C9 H9AA 105.8 . . ?
C10 C9 H9AA 105.8 . . ?
C8B C9 H9AA 141.7 . . ?
C8A C9 H9BA 105.8 . . ?
C10 C9 H9BA 105.8 . . ?
C8B C9 H9BA 91.4 . . ?
H9AA C9 H9BA 106.2 . . ?
C8A C9 H9AB 109.3 . . ?
C10 C9 H9AB 115.4 . . ?
C8B C9 H9AB 105.9 . . ?
H9AA C9 H9AB 86.1 . . ?
H9BA C9 H9AB 20.4 . . ?
C8A C9 H9BB 78.3 . . ?
C10 C9 H9BB 110.8 . . ?
C8B C9 H9BB 112.3 . . ?
H9AA C9 H9BB 32.0 . . ?
H9BA C9 H9BB 130.4 . . ?
H9AB C9 H9BB 110.6 . . ?
C19 C18 C17 115.1(7) . . ?
C19 C18 H18A 108.5 . . ?
C17 C18 H18A 108.5 . . ?
C19 C18 H18B 108.5 . . ?
C17 C18 H18B 108.5 . . ?
H18A C18 H18B 107.5 . . ?
C16 C17 C18 116.1(7) . . ?
C16 C17 H17A 108.3 . . ?
C18 C17 H17A 108.3 . . ?
C16 C17 H17B 108.3 . . ?
C18 C17 H17B 108.3 . . ?
H17A C17 H17B 107.4 . . ?
C14 C13 C12 115.7(7) . . ?
C14 C13 H13A 108.3 . . ?
C12 C13 H13A 108.3 . . ?
C14 C13 H13B 108.3 . . ?
C12 C13 H13B 108.3 . . ?
H13A C13 H13B 107.4 . . ?
C2 N3 C4 106.2(8) . . ?
C2 N3 C24 124.8(8) . . ?
C4 N3 C24 128.9(9) . . ?
C21 C22 C23 116.0(10) . . ?
C21 C22 H22A 108.3 . . ?
C23 C22 H22A 108.3 . . ?
C21 C22 H22B 108.3 . . ?
C23 C22 H22B 108.3 . . ?
H22A C22 H22B 107.4 . . ?
C11 C12 C13 113.7(7) . . ?
C11 C12 H12A 108.8 . . ?
C13 C12 H12A 108.8 . . ?
C11 C12 H12B 108.8 . . ?
C13 C12 H12B 108.8 . . ?
H12A C12 H12B 107.7 . . ?
C9 C10 C11 113.9(8) . . ?
C9 C10 H10A 108.8 . . ?
C11 C10 H10A 108.8 . . ?
C9 C10 H10B 108.8 . . ?
C11 C10 H10B 108.8 . . ?
H10A C10 H10B 107.7 . . ?
C16 C15 C14 115.8(7) . . ?
C16 C15 H15A 108.3 . . ?
C14 C15 H15A 108.3 . . ?
C16 C15 H15B 108.3 . . ?
C14 C15 H15B 108.3 . . ?
H15A C15 H15B 107.4 . . ?
N3 C24 H24A 109.5 . . ?
N3 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N3 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C4 C5 N1 105.6(9) . . ?
C4 C5 H5 127.2 . . ?
N1 C5 H5 127.2 . . ?
C21 C20 C19 115.7(8) . . ?
C21 C20 H20A 108.3 . . ?
C19 C20 H20A 108.3 . . ?
C21 C20 H20B 108.3 . . ?
C19 C20 H20B 108.3 . . ?
H20A C20 H20B 107.4 . . ?
C15 C14 C13 114.6(6) . . ?
C15 C14 H14A 108.6 . . ?
C13 C14 H14A 108.6 . . ?
C15 C14 H14B 108.6 . . ?
C13 C14 H14B 108.6 . . ?
H14A C14 H14B 107.6 . . ?
C10 C11 C12 111.4(8) . . ?
C10 C11 H11A 109.3 . . ?
C12 C11 H11A 109.3 . . ?
C10 C11 H11B 109.3 . . ?
C12 C11 H11B 109.3 . . ?
H11A C11 H11B 108.0 . . ?
N1 C2 N3 106.4(7) . . ?
N1 C2 H2 126.8 . . ?
N3 C2 H2 126.8 . . ?
C18 C19 C20 115.2(7) . . ?
C18 C19 H19A 108.5 . . ?
C20 C19 H19A 108.5 . . ?
C18 C19 H19B 108.5 . . ?
C20 C19 H19B 108.5 . . ?
H19A C19 H19B 107.5 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C15 C16 C17 116.1(7) . . ?
C15 C16 H16A 108.3 . . ?
C17 C16 H16A 108.3 . . ?
C15 C16 H16B 108.3 . . ?
C17 C16 H16B 108.3 . . ?
H16A C16 H16B 107.4 . . ?
C5 C4 N3 108.7(9) . . ?
C5 C4 H4 125.7 . . ?
N3 C4 H4 125.7 . . ?
C6 C7A C8A 115.5(9) . . ?
C6 C7A H7A1 108.4 . . ?
C8A C7A H7A1 108.4 . . ?
C6 C7A H7A2 108.4 . . ?
C8A C7A H7A2 108.4 . . ?
H7A1 C7A H7A2 107.5 . . ?
C6 C7A H6AB 37.2 . . ?
C8A C7A H6AB 150.0 . . ?
H7A1 C7A H6AB 95.9 . . ?
H7A2 C7A H6AB 79.6 . . ?
C9 C8A C7A 110.6(9) . . ?
C9 C8A H9BB 36.7 . . ?
C7A C8A H9BB 145.5 . . ?
C9 C8A H8A1 109.5 . . ?
C7A C8A H8A1 109.5 . . ?
H9BB C8A H8A1 82.6 . . ?
C9 C8A H8A2 109.5 . . ?
C7A C8A H8A2 109.5 . . ?
H9BB C8A H8A2 96.1 . . ?
H8A1 C8A H8A2 108.1 . . ?
C8B C7B C6 104.3(7) . . ?
C8B C7B H7B1 110.9 . . ?
C6 C7B H7B1 110.9 . . ?
C8B C7B H7B2 110.9 . . ?
C6 C7B H7B2 110.9 . . ?
H7B1 C7B H7B2 108.9 . . ?
C7B C8B C9 106.1(7) . . ?
C7B C8B H8B1 110.5 . . ?
C9 C8B H8B1 110.5 . . ?
C7B C8B H8B2 110.5 . . ?
C9 C8B H8B2 110.5 . . ?
H8B1 C8B H8B2 108.7 . . ?
C7A C6 N1 123.7(9) . . ?
C7A C6 C7B 40.8(7) . . ?
N1 C6 C7B 100.8(6) . . ?
C7A C6 H6AA 106.4 . . ?
N1 C6 H6AA 106.4 . . ?
C7B C6 H6AA 83.6 . . ?
C7A C6 H6BA 106.4 . . ?
N1 C6 H6BA 106.4 . . ?
C7B C6 H6BA 146.6 . . ?
H6AA C6 H6BA 106.5 . . ?
C7A C6 H6AB 76.1 . . ?
N1 C6 H6AB 111.5 . . ?
C7B C6 H6AB 116.4 . . ?
H6AA C6 H6AB 131.7 . . ?
H6BA C6 H6AB 34.5 . . ?
C7A C6 H6BB 118.6 . . ?
N1 C6 H6BB 110.8 . . ?
C7B C6 H6BB 107.4 . . ?
H6AA C6 H6BB 25.9 . . ?
H6BA C6 H6BB 80.9 . . ?
H6AB C6 H6BB 109.7 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.056

#=END

data_C18MImNbF6-25oC
#TrackingRef '- SI-25oC.cif'

_database_code_depnum_ccdc_archive 'CCDC 843140'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            C18MImNbF6
_chemical_melting_point          347.2
_chemical_formula_moiety         
;
(C22 N2 H43 +), (Nb F6 -)
;
_chemical_formula_sum            'C22 H43 F6 N2 Nb'
_chemical_formula_weight         542.49

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/a

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x-1/2, -y-1/2, z'

_cell_length_a                   9.5882(11)
_cell_length_b                   10.0041(14)
_cell_length_c                   28.871(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.094(3)
_cell_angle_gamma                90.00
_cell_volume                     2758.4(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    298
_cell_measurement_reflns_used    10535
_cell_measurement_theta_min      5.98
_cell_measurement_theta_max      55.07

_exptl_crystal_description       platelet
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1136
_exptl_absorpt_coefficient_mu    0.487
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7628
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'RAPID AUTO 2.40 (Rigaku 2006)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      298
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS RapidII'
_diffrn_measurement_method       'imaging plate'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21340
_diffrn_reflns_av_R_equivalents  0.0551
_diffrn_reflns_av_sigmaI/netI    0.0459
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         2.99
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4855
_reflns_number_gt                2336
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Rigaku R-AXIS Rapid-II'
_computing_cell_refinement       'RAPID AUTO 2.40 (Rigaku 2006)'
_computing_data_reduction        'RAPID AUTO 2.40 (Rigaku 2006)'
_computing_structure_solution    'SIR92 (Altmare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
This structure was solved based on the data at 25 deg C and the octadecyl chain
in this structure has a large conformational flexibility, which results in large
thermal motions of the atoms. Hence, the following restraints were applied.
The N-C and C-C bond lengths in the octadecyl chain were restrained using
the DFIX (1,2 C(N)-C distance: 1.54 A) and DANG (1,3 C(N)-C distance: 2.52 A)
commands in SHELXL. The N-C-C-C part of the trans structure was
weakly fixed using the FLAT command. Atomic displacement factors of the
disordered part and some carbon atoms in the octadecyl chain were restrained
using DELU and SIMU in SHELXL.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4855
_refine_ls_number_parameters     301
_refine_ls_number_restraints     108
_refine_ls_R_factor_all          0.1582
_refine_ls_R_factor_gt           0.0885
_refine_ls_wR_factor_ref         0.3264
_refine_ls_wR_factor_gt          0.2576
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.143
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.003

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb -0.15256(10) 0.02625(11) 0.10806(3) 0.1015(5) Uani 1 1 d . . .
F4 F -0.2419(10) -0.0529(9) 0.1550(3) 0.162(3) Uani 1 1 d . . .
F3 F -0.2992(9) 0.1431(8) 0.1005(4) 0.188(4) Uani 1 1 d . . .
F2 F -0.0754(9) 0.0997(13) 0.0571(3) 0.206(5) Uani 1 1 d . . .
F5 F -0.0098(8) -0.0986(8) 0.1150(3) 0.157(3) Uani 1 1 d . . .
N1 N 0.3908(10) -0.0127(9) 0.1122(3) 0.108(3) Uani 1 1 d D A .
F6 F -0.0485(9) 0.1374(8) 0.1477(3) 0.169(3) Uani 1 1 d . . .
F1 F -0.2524(7) -0.0924(9) 0.0671(3) 0.157(3) Uani 1 1 d . . .
C21 C -0.6468(15) -0.1519(13) 0.6678(4) 0.137(4) Uani 1 1 d D . .
H21A H -0.7324 -0.1424 0.6475 0.165 Uiso 1 1 calc R . .
H21B H -0.6292 -0.2468 0.6720 0.165 Uiso 1 1 calc R . .
C9 C 0.1587(11) -0.1406(12) 0.2445(4) 0.193(7) Uani 1 1 d DU . .
H9AA H 0.1155 -0.2279 0.2402 0.231 Uiso 0.682(19) 1 calc PR A 1
H9BA H 0.0940 -0.0766 0.2291 0.231 Uiso 0.682(19) 1 calc PR A 1
H9AB H 0.0755 -0.1251 0.2239 0.231 Uiso 0.318(19) 1 d PR A 2
H9BB H 0.1869 -0.2334 0.2432 0.231 Uiso 0.318(19) 1 d PR A 2
C18 C -0.3874(13) -0.0946(12) 0.5737(4) 0.124(4) Uani 1 1 d D . .
H18A H -0.4039 0.0006 0.5699 0.149 Uiso 1 1 calc R . .
H18B H -0.3015 -0.1058 0.5938 0.149 Uiso 1 1 calc R . .
C17 C -0.3672(13) -0.1547(11) 0.5266(4) 0.122(4) Uani 1 1 d D . .
H17A H -0.3514 -0.2500 0.5304 0.146 Uiso 1 1 calc R . .
H17B H -0.4530 -0.1430 0.5065 0.146 Uiso 1 1 calc R . .
C13 C -0.0904(12) -0.1613(11) 0.3852(4) 0.119(4) Uani 1 1 d D . .
H13A H -0.1761 -0.1466 0.3654 0.143 Uiso 1 1 calc R . .
H13B H -0.0779 -0.2570 0.3890 0.143 Uiso 1 1 calc R . .
N3 N 0.3948(10) -0.1137(10) 0.0502(3) 0.108(3) Uani 1 1 d . . .
C22 C -0.669(2) -0.0918(19) 0.7140(6) 0.185(7) Uani 1 1 d D . .
H22A H -0.6847 0.0034 0.7097 0.221 Uiso 1 1 calc R . .
H22B H -0.5839 -0.1028 0.7343 0.221 Uiso 1 1 calc R . .
C12 C 0.0320(12) -0.1048(13) 0.3615(5) 0.130(4) Uani 1 1 d D A .
H12A H 0.0234 -0.0083 0.3593 0.156 Uiso 1 1 calc R . .
H12B H 0.1189 -0.1253 0.3799 0.156 Uiso 1 1 calc R . .
C10 C 0.1672(12) -0.1100(13) 0.2963(4) 0.197(7) Uani 1 1 d DU A .
H10A H 0.2483 -0.1530 0.3124 0.236 Uiso 1 1 calc R . .
H10B H 0.1742 -0.0144 0.3017 0.236 Uiso 1 1 calc R . .
C15 C -0.2261(11) -0.1582(11) 0.4563(4) 0.116(3) Uani 1 1 d D . .
H15A H -0.3116 -0.1480 0.4360 0.139 Uiso 1 1 calc R . .
H15B H -0.2097 -0.2531 0.4608 0.139 Uiso 1 1 calc R . .
C24 C 0.4489(14) -0.2060(14) 0.0157(4) 0.132(4) Uani 1 1 d . . .
H24A H 0.5260 -0.1647 0.0022 0.198 Uiso 1 1 calc R . .
H24B H 0.3758 -0.2254 -0.0083 0.198 Uiso 1 1 calc R . .
H24C H 0.4798 -0.2875 0.0309 0.198 Uiso 1 1 calc R . .
C5 C 0.2835(15) 0.0399(14) 0.0863(6) 0.130(4) Uani 1 1 d . . .
H5 H 0.2191 0.1034 0.0945 0.156 Uiso 1 1 calc R . .
C20 C -0.5283(15) -0.0921(14) 0.6440(4) 0.137(4) Uani 1 1 d D . .
H20A H -0.4424 -0.1014 0.6642 0.165 Uiso 1 1 calc R . .
H20B H -0.5459 0.0026 0.6394 0.165 Uiso 1 1 calc R . .
C14 C -0.1058(12) -0.0995(12) 0.4324(4) 0.118(3) Uani 1 1 d D . .
H14A H -0.1204 -0.0040 0.4286 0.142 Uiso 1 1 calc R . .
H14B H -0.0195 -0.1125 0.4520 0.142 Uiso 1 1 calc R . .
C11 C 0.0352(12) -0.1637(13) 0.3132(5) 0.142(5) Uani 1 1 d D . .
H11A H 0.0372 -0.2605 0.3144 0.170 Uiso 1 1 calc R A .
H11B H -0.0458 -0.1354 0.2931 0.170 Uiso 1 1 calc R . .
C2 C 0.4522(11) -0.1116(9) 0.0936(4) 0.097(3) Uani 1 1 d D . .
H2 H 0.5207 -0.1681 0.1074 0.117 Uiso 1 1 calc R . .
C19 C -0.5075(13) -0.1551(12) 0.5976(4) 0.121(4) Uani 1 1 d D . .
H19A H -0.5932 -0.1456 0.5774 0.145 Uiso 1 1 calc R . .
H19B H -0.4901 -0.2499 0.6022 0.145 Uiso 1 1 calc R . .
C23 C -0.789(2) -0.1484(18) 0.7383(6) 0.202(8) Uani 1 1 d D . .
H23A H -0.8714 -0.1537 0.7168 0.303 Uiso 1 1 calc R . .
H23B H -0.8079 -0.0913 0.7638 0.303 Uiso 1 1 calc R . .
H23C H -0.7652 -0.2361 0.7499 0.303 Uiso 1 1 calc R . .
C16 C -0.2471(11) -0.0957(12) 0.5025(4) 0.116(3) Uani 1 1 d D . .
H16A H -0.2638 -0.0008 0.4980 0.139 Uiso 1 1 calc R . .
H16B H -0.1615 -0.1056 0.5228 0.139 Uiso 1 1 calc R . .
C4 C 0.2915(16) -0.0215(15) 0.0456(6) 0.132(4) Uani 1 1 d . . .
H4 H 0.2350 -0.0037 0.0185 0.159 Uiso 1 1 calc R . .
C7A C 0.2884(18) -0.0054(17) 0.1939(5) 0.127(6) Uani 0.682(19) 1 d PDU A 1
H7A1 H 0.1984 0.0067 0.1762 0.153 Uiso 0.682(19) 1 calc PR A 1
H7A2 H 0.2965 0.0635 0.2177 0.153 Uiso 0.682(19) 1 calc PR A 1
C8A C 0.286(2) -0.1411(18) 0.2185(7) 0.186(8) Uani 0.682(19) 1 d PDU A 1
H8A1 H 0.2817 -0.2133 0.1960 0.223 Uiso 0.682(19) 1 calc PR A 1
H8A2 H 0.3697 -0.1525 0.2397 0.223 Uiso 0.682(19) 1 calc PR A 1
C7B C 0.294(2) -0.090(2) 0.1793(5) 0.150(9) Uani 0.318(19) 1 d PDU A 2
H7B1 H 0.2007 -0.0792 0.1636 0.180 Uiso 0.318(19) 1 calc PR A 2
H7B2 H 0.3267 -0.1798 0.1732 0.180 Uiso 0.318(19) 1 calc PR A 2
C8B C 0.292(2) -0.067(2) 0.2300(6) 0.164(10) Uani 0.318(19) 1 d PDU A 2
H8B1 H 0.2870 0.0277 0.2366 0.196 Uiso 0.318(19) 1 calc PR A 2
H8B2 H 0.3758 -0.1034 0.2467 0.196 Uiso 0.318(19) 1 calc PR A 2
C6 C 0.3971(12) 0.0180(13) 0.1627(4) 0.141(5) Uani 1 1 d DU . .
H6AA H 0.4793 -0.0284 0.1766 0.170 Uiso 0.682(19) 1 calc PR A 1
H6BA H 0.4186 0.1126 0.1653 0.170 Uiso 0.682(19) 1 calc PR A 1
H6AB H 0.3691 0.1089 0.1688 0.170 Uiso 0.318(19) 1 d PR A 2
H6BB H 0.4926 0.0046 0.1750 0.170 Uiso 0.318(19) 1 d PR A 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Nb1 0.0996(7) 0.0966(8) 0.1092(8) 0.0047(5) 0.0151(5) -0.0010(5)
F4 0.193(8) 0.158(7) 0.139(6) 0.029(5) 0.031(5) -0.034(6)
F3 0.138(6) 0.142(7) 0.287(11) 0.035(7) 0.030(6) 0.046(5)
F2 0.167(7) 0.295(13) 0.160(7) 0.076(8) 0.039(6) -0.054(8)
F5 0.131(5) 0.128(6) 0.206(8) -0.031(6) -0.021(5) 0.034(5)
N1 0.109(6) 0.099(7) 0.117(7) 0.024(5) 0.008(6) -0.017(5)
F6 0.172(7) 0.124(6) 0.206(8) -0.053(5) -0.007(6) -0.022(5)
F1 0.122(5) 0.196(7) 0.151(6) -0.058(6) 0.009(4) -0.016(5)
C21 0.179(12) 0.102(9) 0.125(10) -0.006(8) -0.015(9) 0.000(9)
C9 0.109(8) 0.174(13) 0.297(15) 0.137(12) 0.029(10) -0.021(8)
C18 0.147(10) 0.092(8) 0.129(9) -0.019(7) -0.013(8) -0.009(8)
C17 0.145(9) 0.079(7) 0.135(9) -0.013(7) -0.019(7) -0.006(7)
C13 0.136(9) 0.082(8) 0.136(10) -0.005(7) -0.009(7) -0.011(6)
N3 0.116(7) 0.100(7) 0.106(7) 0.014(5) 0.003(5) -0.033(6)
C22 0.23(2) 0.150(14) 0.168(15) -0.029(13) -0.006(14) -0.012(15)
C12 0.113(8) 0.102(9) 0.171(12) 0.024(9) -0.005(8) -0.009(7)
C10 0.132(10) 0.182(15) 0.280(15) 0.123(14) 0.040(12) -0.019(10)
C15 0.134(9) 0.090(8) 0.120(8) -0.009(6) -0.011(7) 0.005(7)
C24 0.156(10) 0.136(11) 0.105(8) -0.011(8) 0.015(8) -0.033(9)
C5 0.123(9) 0.129(11) 0.134(11) 0.029(9) -0.014(9) 0.002(8)
C20 0.174(12) 0.102(9) 0.132(10) -0.007(8) -0.012(9) -0.006(9)
C14 0.115(8) 0.089(8) 0.147(10) 0.016(7) -0.009(7) -0.009(6)
C11 0.122(9) 0.099(9) 0.203(15) 0.019(9) 0.008(9) -0.018(7)
C2 0.099(6) 0.076(7) 0.120(9) 0.010(6) 0.021(6) -0.005(5)
C19 0.148(10) 0.092(8) 0.117(8) -0.013(6) -0.020(7) 0.004(7)
C23 0.28(2) 0.155(16) 0.175(15) 0.011(12) 0.035(16) -0.029(16)
C16 0.117(8) 0.088(8) 0.137(9) 0.002(7) -0.019(7) -0.016(6)
C4 0.127(10) 0.129(11) 0.140(12) 0.048(9) 0.006(9) 0.005(9)
C7A 0.122(11) 0.135(14) 0.132(13) 0.032(10) 0.048(9) 0.014(10)
C8A 0.162(13) 0.113(15) 0.288(17) 0.048(12) 0.045(12) -0.018(12)
C7B 0.117(16) 0.094(18) 0.249(18) -0.008(18) 0.062(15) 0.033(14)
C8B 0.146(17) 0.12(2) 0.225(16) 0.111(17) 0.026(15) -0.026(16)
C6 0.135(10) 0.144(11) 0.154(11) 0.015(8) 0.061(8) 0.015(8)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 F6 1.826(7) . ?
Nb1 F3 1.827(7) . ?
Nb1 F4 1.845(7) . ?
Nb1 F5 1.851(7) . ?
Nb1 F2 1.857(7) . ?
Nb1 F1 1.876(7) . ?
N1 C2 1.293(7) . ?
N1 C5 1.326(15) . ?
N1 C6 1.486(12) . ?
C21 C22 1.496(13) . ?
C21 C20 1.504(12) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C9 C8A 1.491(10) . ?
C9 C10 1.524(6) . ?
C9 C8B 1.563(5) . ?
C9 H9AA 0.9700 . ?
C9 H9BA 0.9700 . ?
C9 H9AB 0.9626 . ?
C9 H9BB 0.9690 . ?
C18 C17 1.516(11) . ?
C18 C19 1.520(12) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C17 C16 1.515(12) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C13 C14 1.513(11) . ?
C13 C12 1.520(12) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
N3 C2 1.322(13) . ?
N3 C4 1.351(15) . ?
N3 C24 1.486(15) . ?
C22 C23 1.512(10) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C12 C11 1.517(12) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C10 C11 1.495(9) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C15 C16 1.504(11) . ?
C15 C14 1.515(11) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C5 C4 1.334(19) . ?
C5 H5 0.9300 . ?
C20 C19 1.508(12) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C2 H2 0.9300 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C4 H4 0.9300 . ?
C7A C6 1.457(10) . ?
C7A C8A 1.533(11) . ?
C7A H7A1 0.9700 . ?
C7A H7A2 0.9700 . ?
C8A H9BB 1.5465 . ?
C8A H8A1 0.9700 . ?
C8A H8A2 0.9700 . ?
C7B C8B 1.483(8) . ?
C7B C6 1.574(6) . ?
C7B H7B1 0.9700 . ?
C7B H7B2 0.9700 . ?
C8B H8B1 0.9700 . ?
C8B H8B2 0.9700 . ?
C6 H6AA 0.9700 . ?
C6 H6BA 0.9700 . ?
C6 H6AB 0.9688 . ?
C6 H6BB 0.9614 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F6 Nb1 F3 93.2(4) . . ?
F6 Nb1 F4 93.7(4) . . ?
F3 Nb1 F4 87.7(4) . . ?
F6 Nb1 F5 89.2(4) . . ?
F3 Nb1 F5 177.3(4) . . ?
F4 Nb1 F5 91.0(4) . . ?
F6 Nb1 F2 91.2(5) . . ?
F3 Nb1 F2 90.5(5) . . ?
F4 Nb1 F2 174.8(4) . . ?
F5 Nb1 F2 90.6(5) . . ?
F6 Nb1 F1 177.5(3) . . ?
F3 Nb1 F1 89.2(4) . . ?
F4 Nb1 F1 87.0(4) . . ?
F5 Nb1 F1 88.4(4) . . ?
F2 Nb1 F1 88.1(4) . . ?
C2 N1 C5 115.4(12) . . ?
C2 N1 C6 125.9(10) . . ?
C5 N1 C6 115.7(11) . . ?
C22 C21 C20 115.0(12) . . ?
C22 C21 H21A 108.5 . . ?
C20 C21 H21A 108.5 . . ?
C22 C21 H21B 108.5 . . ?
C20 C21 H21B 108.5 . . ?
H21A C21 H21B 107.5 . . ?
C8A C9 C10 121.4(10) . . ?
C8A C9 C8B 30.7(10) . . ?
C10 C9 C8B 101.2(6) . . ?
C8A C9 H9AA 107.0 . . ?
C10 C9 H9AA 107.0 . . ?
C8B C9 H9AA 137.6 . . ?
C8A C9 H9BA 107.0 . . ?
C10 C9 H9BA 107.0 . . ?
C8B C9 H9BA 94.2 . . ?
H9AA C9 H9BA 106.7 . . ?
C8A C9 H9AB 111.2 . . ?
C10 C9 H9AB 122.8 . . ?
C8B C9 H9AB 114.3 . . ?
H9AA C9 H9AB 75.2 . . ?
H9BA C9 H9AB 32.1 . . ?
C8A C9 H9BB 74.6 . . ?
C10 C9 H9BB 103.8 . . ?
C8B C9 H9BB 101.7 . . ?
H9AA C9 H9BB 41.3 . . ?
H9BA C9 H9BB 141.7 . . ?
H9AB C9 H9BB 110.5 . . ?
C17 C18 C19 114.3(9) . . ?
C17 C18 H18A 108.7 . . ?
C19 C18 H18A 108.7 . . ?
C17 C18 H18B 108.7 . . ?
C19 C18 H18B 108.7 . . ?
H18A C18 H18B 107.6 . . ?
C16 C17 C18 114.8(9) . . ?
C16 C17 H17A 108.6 . . ?
C18 C17 H17A 108.6 . . ?
C16 C17 H17B 108.6 . . ?
C18 C17 H17B 108.6 . . ?
H17A C17 H17B 107.5 . . ?
C14 C13 C12 113.2(10) . . ?
C14 C13 H13A 108.9 . . ?
C12 C13 H13A 108.9 . . ?
C14 C13 H13B 108.9 . . ?
C12 C13 H13B 108.9 . . ?
H13A C13 H13B 107.8 . . ?
C2 N3 C4 108.8(11) . . ?
C2 N3 C24 120.3(11) . . ?
C4 N3 C24 130.9(13) . . ?
C21 C22 C23 116.1(15) . . ?
C21 C22 H22A 108.3 . . ?
C23 C22 H22A 108.3 . . ?
C21 C22 H22B 108.3 . . ?
C23 C22 H22B 108.3 . . ?
H22A C22 H22B 107.4 . . ?
C11 C12 C13 110.5(10) . . ?
C11 C12 H12A 109.6 . . ?
C13 C12 H12A 109.6 . . ?
C11 C12 H12B 109.6 . . ?
C13 C12 H12B 109.6 . . ?
H12A C12 H12B 108.1 . . ?
C11 C10 C9 105.9(10) . . ?
C11 C10 H10A 110.6 . . ?
C9 C10 H10A 110.6 . . ?
C11 C10 H10B 110.5 . . ?
C9 C10 H10B 110.5 . . ?
H10A C10 H10B 108.7 . . ?
C16 C15 C14 114.3(9) . . ?
C16 C15 H15A 108.7 . . ?
C14 C15 H15A 108.7 . . ?
C16 C15 H15B 108.7 . . ?
C14 C15 H15B 108.7 . . ?
H15A C15 H15B 107.6 . . ?
N3 C24 H24A 109.5 . . ?
N3 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N3 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N1 C5 C4 102.2(14) . . ?
N1 C5 H5 128.9 . . ?
C4 C5 H5 128.9 . . ?
C21 C20 C19 113.9(11) . . ?
C21 C20 H20A 108.8 . . ?
C19 C20 H20A 108.8 . . ?
C21 C20 H20B 108.8 . . ?
C19 C20 H20B 108.8 . . ?
H20A C20 H20B 107.7 . . ?
C13 C14 C15 113.0(9) . . ?
C13 C14 H14A 109.0 . . ?
C15 C14 H14A 109.0 . . ?
C13 C14 H14B 109.0 . . ?
C15 C14 H14B 109.0 . . ?
H14A C14 H14B 107.8 . . ?
C10 C11 C12 104.3(10) . . ?
C10 C11 H11A 110.9 . . ?
C12 C11 H11A 110.9 . . ?
C10 C11 H11B 110.9 . . ?
C12 C11 H11B 110.9 . . ?
H11A C11 H11B 108.9 . . ?
N1 C2 N3 103.9(10) . . ?
N1 C2 H2 128.1 . . ?
N3 C2 H2 128.1 . . ?
C20 C19 C18 113.7(10) . . ?
C20 C19 H19A 108.8 . . ?
C18 C19 H19A 108.8 . . ?
C20 C19 H19B 108.8 . . ?
C18 C19 H19B 108.8 . . ?
H19A C19 H19B 107.7 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C15 C16 C17 114.3(9) . . ?
C15 C16 H16A 108.7 . . ?
C17 C16 H16A 108.7 . . ?
C15 C16 H16B 108.7 . . ?
C17 C16 H16B 108.7 . . ?
H16A C16 H16B 107.6 . . ?
C5 C4 N3 109.1(14) . . ?
C5 C4 H4 125.5 . . ?
N3 C4 H4 125.5 . . ?
C6 C7A C8A 117.9(11) . . ?
C6 C7A H7A1 107.8 . . ?
C8A C7A H7A1 107.8 . . ?
C6 C7A H7A2 107.8 . . ?
C8A C7A H7A2 107.8 . . ?
H7A1 C7A H7A2 107.2 . . ?
C9 C8A C7A 106.0(11) . . ?
C9 C8A H9BB 37.2 . . ?
C7A C8A H9BB 141.0 . . ?
C9 C8A H8A1 110.5 . . ?
C7A C8A H8A1 110.5 . . ?
H9BB C8A H8A1 82.7 . . ?
C9 C8A H8A2 110.5 . . ?
C7A C8A H8A2 110.5 . . ?
H9BB C8A H8A2 98.4 . . ?
H8A1 C8A H8A2 108.7 . . ?
C8B C7B C6 104.7(10) . . ?
C8B C7B H7B1 110.8 . . ?
C6 C7B H7B1 110.8 . . ?
C8B C7B H7B2 110.8 . . ?
C6 C7B H7B2 110.8 . . ?
H7B1 C7B H7B2 108.9 . . ?
C7B C8B C9 105.7(7) . . ?
C7B C8B H8B1 110.6 . . ?
C9 C8B H8B1 110.6 . . ?
C7B C8B H8B2 110.6 . . ?
C9 C8B H8B2 110.6 . . ?
H8B1 C8B H8B2 108.7 . . ?
C7A C6 N1 127.2(12) . . ?
C7A C6 C7B 36.4(10) . . ?
N1 C6 C7B 100.6(7) . . ?
C7A C6 H6AA 105.5 . . ?
N1 C6 H6AA 105.5 . . ?
C7B C6 H6AA 93.2 . . ?
C7A C6 H6BA 105.5 . . ?
N1 C6 H6BA 105.5 . . ?
C7B C6 H6BA 141.6 . . ?
H6AA C6 H6BA 106.1 . . ?
C7A C6 H6AB 79.2 . . ?
N1 C6 H6AB 112.7 . . ?
C7B C6 H6AB 113.5 . . ?
H6AA C6 H6AB 127.0 . . ?
H6BA C6 H6AB 29.6 . . ?
C7A C6 H6BB 117.4 . . ?
N1 C6 H6BB 106.7 . . ?
C7B C6 H6BB 113.4 . . ?
H6AA C6 H6BB 21.4 . . ?
H6BA C6 H6BB 85.4 . . ?
H6AB C6 H6BB 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.897
_refine_diff_density_min         -0.664
_refine_diff_density_rms         0.095

#=END

data_C18MImTaF6-25oC
#TrackingRef '- SI-25oC.cif'

_database_code_depnum_ccdc_archive 'CCDC 843141'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            C18MImTaF6
_chemical_melting_point          347.0
_chemical_formula_moiety         
;
(C22 N2 H43 +), (Ta F6 -)
;
_chemical_formula_sum            'C22 H43 F6 N2 Ta'
_chemical_formula_weight         630.53

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/a

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x-1/2, -y-1/2, z'

_cell_length_a                   9.6813(8)
_cell_length_b                   10.0074(9)
_cell_length_c                   29.014(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.112(2)
_cell_angle_gamma                90.00
_cell_volume                     2799.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    298
_cell_measurement_reflns_used    10816
_cell_measurement_theta_min      6.12
_cell_measurement_theta_max      54.80

_exptl_crystal_description       platelet
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1264
_exptl_absorpt_coefficient_mu    3.976
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1945
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'RAPID AUTO 2.40 (Rigaku 2006)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      298
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS RapidII'
_diffrn_measurement_method       'imaging plate'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20501
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_sigmaI/netI    0.0538
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         3.06
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4902
_reflns_number_gt                2514
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Rigaku R-AXIS Rapid-II'
_computing_cell_refinement       'RAPID AUTO 2.40 (Rigaku 2006)'
_computing_data_reduction        'RAPID AUTO 2.40 (Rigaku 2006)'
_computing_structure_solution    'SIR92 (Altmare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
This structure was solved based on the data at 25 deg C and the octadecyl chain
in this structure has a large conformational flexibility, which results in large
thermal motions of the atoms. Hence, the following restraints were applied.
The N-C and C-C bond lengths in the octadecyl chain were restrained using
the DFIX (1,2 C(N)-C distance: 1.54 A) and DANG (1,3 C(N)-C distance: 2.52 A)
commands in SHELXL. The N-C-C-C part of the trans structure was
weakly fixed using the FLAT command. Atomic displacement factors of the
disordered part and some carbon atoms in the octadecyl chain were restrained
using DELU and SIMU in SHELXL.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0676P)^2^+0.9149P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4902
_refine_ls_number_parameters     301
_refine_ls_number_restraints     98
_refine_ls_R_factor_all          0.0976
_refine_ls_R_factor_gt           0.0469
_refine_ls_wR_factor_ref         0.1406
_refine_ls_wR_factor_gt          0.1136
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ta1 Ta -0.15451(4) 0.02938(5) 0.108425(15) 0.1173(3) Uani 1 1 d . . .
F4 F -0.2441(10) -0.0492(8) 0.1548(3) 0.199(3) Uani 1 1 d . . .
F3 F -0.2974(8) 0.1434(8) 0.0992(4) 0.230(4) Uani 1 1 d . . .
F2 F -0.0743(9) 0.0995(12) 0.0587(3) 0.239(4) Uani 1 1 d . . .
F5 F -0.0142(7) -0.0954(8) 0.1172(3) 0.194(3) Uani 1 1 d . . .
N1 N 0.3863(10) -0.0203(11) 0.1129(3) 0.121(3) Uani 1 1 d D A .
F6 F -0.0533(8) 0.1418(7) 0.1475(3) 0.201(3) Uani 1 1 d . . .
F1 F -0.2542(6) -0.0887(8) 0.0683(3) 0.179(3) Uani 1 1 d . . .
C21 C -0.6446(15) -0.1533(13) 0.6673(5) 0.168(5) Uani 1 1 d D . .
H21A H -0.6264 -0.2481 0.6713 0.201 Uiso 1 1 calc R . .
H21B H -0.7298 -0.1437 0.6473 0.201 Uiso 1 1 calc R . .
C9 C 0.1618(11) -0.1450(13) 0.2468(5) 0.207(7) Uani 1 1 d DU . .
H9AA H 0.0912 -0.0946 0.2284 0.249 Uiso 0.525(17) 1 calc PR A 1
H9BA H 0.1323 -0.2376 0.2454 0.249 Uiso 0.525(17) 1 calc PR A 1
H9AB H 0.0787 -0.1295 0.2262 0.249 Uiso 0.475(17) 1 d PR A 2
H9BB H 0.1900 -0.2378 0.2455 0.249 Uiso 0.475(17) 1 d PR A 2
C18 C -0.3881(12) -0.0941(11) 0.5739(4) 0.150(4) Uani 1 1 d D . .
H18A H -0.4056 0.0008 0.5698 0.180 Uiso 1 1 calc R . .
H18B H -0.3029 -0.1038 0.5939 0.180 Uiso 1 1 calc R . .
C17 C -0.3670(12) -0.1547(10) 0.5274(4) 0.139(4) Uani 1 1 d D . .
H17A H -0.4516 -0.1435 0.5073 0.167 Uiso 1 1 calc R . .
H17B H -0.3513 -0.2499 0.5315 0.167 Uiso 1 1 calc R . .
C13 C -0.0910(12) -0.1611(11) 0.3870(4) 0.144(4) Uani 1 1 d D . .
H13A H -0.1766 -0.1479 0.3675 0.173 Uiso 1 1 calc R . .
H13B H -0.0767 -0.2565 0.3907 0.173 Uiso 1 1 calc R . .
N3 N 0.3989(10) -0.1172(9) 0.0503(4) 0.122(3) Uani 1 1 d . . .
C22 C -0.6650(18) -0.0929(18) 0.7137(6) 0.209(7) Uani 1 1 d D . .
H22A H -0.6787 0.0026 0.7098 0.251 Uiso 1 1 calc R . .
H22B H -0.5810 -0.1060 0.7340 0.251 Uiso 1 1 calc R . .
C12 C 0.0277(12) -0.1029(12) 0.3631(5) 0.154(4) Uani 1 1 d D A .
H12A H 0.0149 -0.0071 0.3598 0.185 Uiso 1 1 calc R . .
H12B H 0.1140 -0.1181 0.3820 0.185 Uiso 1 1 calc R . .
C10 C 0.1552(12) -0.1022(15) 0.2946(4) 0.205(7) Uani 1 1 d D A .
H10A H 0.1462 -0.0057 0.2954 0.246 Uiso 1 1 calc R . .
H10B H 0.2413 -0.1259 0.3124 0.246 Uiso 1 1 calc R . .
C15 C -0.2262(10) -0.1581(9) 0.4573(4) 0.134(4) Uani 1 1 d D . .
H15A H -0.3106 -0.1469 0.4369 0.161 Uiso 1 1 calc R . .
H15B H -0.2109 -0.2532 0.4616 0.161 Uiso 1 1 calc R . .
C24 C 0.4515(13) -0.2075(12) 0.0153(4) 0.162(4) Uani 1 1 d . . .
H24A H 0.4367 -0.1672 -0.0148 0.243 Uiso 1 1 calc R . .
H24B H 0.4031 -0.2912 0.0153 0.243 Uiso 1 1 calc R . .
H24C H 0.5489 -0.2226 0.0227 0.243 Uiso 1 1 calc R . .
C5 C 0.2827(16) 0.0322(14) 0.0855(7) 0.154(4) Uani 1 1 d . . .
H5 H 0.2183 0.0959 0.0929 0.185 Uiso 1 1 calc R . .
C20 C -0.5278(15) -0.0911(14) 0.6440(4) 0.164(5) Uani 1 1 d D . .
H20A H -0.4430 -0.0987 0.6643 0.196 Uiso 1 1 calc R . .
H20B H -0.5471 0.0033 0.6393 0.196 Uiso 1 1 calc R . .
C14 C -0.1063(11) -0.1001(11) 0.4337(4) 0.137(4) Uani 1 1 d D . .
H14A H -0.1198 -0.0045 0.4301 0.164 Uiso 1 1 calc R . .
H14B H -0.0212 -0.1141 0.4534 0.164 Uiso 1 1 calc R . .
C11 C 0.0371(11) -0.1635(12) 0.3166(5) 0.155(4) Uani 1 1 d D . .
H11A H -0.0487 -0.1483 0.2974 0.186 Uiso 1 1 calc R A .
H11B H 0.0511 -0.2592 0.3197 0.186 Uiso 1 1 calc R . .
C2 C 0.4511(11) -0.1134(11) 0.0934(5) 0.121(3) Uani 1 1 d . . .
H2 H 0.5213 -0.1675 0.1072 0.146 Uiso 1 1 calc R . .
C19 C -0.5056(12) -0.1548(10) 0.5978(4) 0.143(4) Uani 1 1 d D . .
H19A H -0.4872 -0.2492 0.6027 0.171 Uiso 1 1 calc R . .
H19B H -0.5906 -0.1468 0.5776 0.171 Uiso 1 1 calc R . .
C23 C -0.786(2) -0.1496(17) 0.7369(6) 0.245(8) Uani 1 1 d D . .
H23A H -0.8640 -0.1600 0.7144 0.367 Uiso 1 1 calc R . .
H23B H -0.8096 -0.0899 0.7608 0.367 Uiso 1 1 calc R . .
H23C H -0.7605 -0.2350 0.7501 0.367 Uiso 1 1 calc R . .
C16 C -0.2474(12) -0.0959(12) 0.5036(4) 0.141(4) Uani 1 1 d D . .
H16A H -0.2635 -0.0009 0.4993 0.169 Uiso 1 1 calc R . .
H16B H -0.1628 -0.1064 0.5239 0.169 Uiso 1 1 calc R . .
C4 C 0.2928(14) -0.0275(15) 0.0452(6) 0.148(4) Uani 1 1 d . . .
H4 H 0.2369 -0.0109 0.0181 0.177 Uiso 1 1 calc R . .
C7A C 0.2833(18) -0.009(2) 0.1933(6) 0.147(7) Uani 0.525(17) 1 d PDU A 1
H7A1 H 0.1964 -0.0085 0.1738 0.176 Uiso 0.525(17) 1 calc PR A 1
H7A2 H 0.2820 0.0661 0.2142 0.176 Uiso 0.525(17) 1 calc PR A 1
C8A C 0.290(2) -0.137(2) 0.2218(7) 0.200(9) Uani 0.525(17) 1 d PDU A 1
H8A1 H 0.2956 -0.2144 0.2017 0.240 Uiso 0.525(17) 1 calc PR A 1
H8A2 H 0.3715 -0.1366 0.2438 0.240 Uiso 0.525(17) 1 calc PR A 1
C7B C 0.3051(18) -0.1033(16) 0.1821(5) 0.158(7) Uani 0.475(17) 1 d PDU A 2
H7B1 H 0.2196 -0.1141 0.1623 0.189 Uiso 0.475(17) 1 calc PR A 2
H7B2 H 0.3539 -0.1880 0.1842 0.189 Uiso 0.475(17) 1 calc PR A 2
C8B C 0.2769(19) -0.0536(18) 0.2287(5) 0.176(8) Uani 0.475(17) 1 d PDU A 2
H8B1 H 0.2456 0.0385 0.2268 0.211 Uiso 0.475(17) 1 calc PR A 2
H8B2 H 0.3607 -0.0577 0.2497 0.211 Uiso 0.475(17) 1 calc PR A 2
C6 C 0.3988(12) 0.0106(12) 0.1632(4) 0.157(4) Uani 1 1 d DU . .
H6AA H 0.4256 0.1038 0.1662 0.189 Uiso 0.525(17) 1 calc PR A 1
H6BA H 0.4767 -0.0411 0.1769 0.189 Uiso 0.525(17) 1 calc PR A 1
H6AB H 0.3707 0.1015 0.1693 0.189 Uiso 0.475(17) 1 d PR A 2
H6BB H 0.4943 -0.0028 0.1755 0.189 Uiso 0.475(17) 1 d PR A 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ta1 0.1151(3) 0.1165(4) 0.1220(4) 0.0061(3) 0.0193(2) -0.0007(3)
F4 0.228(8) 0.211(8) 0.159(6) 0.035(5) 0.021(6) -0.027(6)
F3 0.179(6) 0.158(6) 0.352(12) 0.039(7) 0.027(7) 0.050(5)
F2 0.201(7) 0.334(11) 0.188(7) 0.089(8) 0.050(6) -0.062(8)
F5 0.155(5) 0.152(5) 0.266(9) -0.035(6) -0.036(6) 0.033(5)
N1 0.116(6) 0.121(7) 0.126(8) 0.021(6) 0.009(6) -0.023(5)
F6 0.214(7) 0.146(6) 0.240(8) -0.056(5) 0.007(6) -0.036(5)
F1 0.130(4) 0.222(7) 0.184(6) -0.061(5) 0.007(4) -0.031(5)
C21 0.205(13) 0.131(10) 0.161(12) -0.020(9) -0.016(10) -0.005(10)
C9 0.134(9) 0.199(13) 0.296(16) 0.140(13) 0.055(10) 0.010(9)
C18 0.157(9) 0.107(7) 0.178(12) -0.014(8) -0.031(9) -0.007(8)
C17 0.167(10) 0.102(7) 0.144(10) -0.012(7) -0.016(8) -0.002(7)
C13 0.151(9) 0.108(8) 0.169(11) -0.001(7) -0.007(8) -0.011(7)
N3 0.128(7) 0.117(7) 0.122(8) 0.013(6) 0.007(6) -0.030(6)
C22 0.263(19) 0.182(14) 0.178(16) -0.042(13) -0.008(13) -0.018(14)
C12 0.145(9) 0.106(8) 0.204(14) 0.015(9) -0.023(9) -0.019(8)
C10 0.163(11) 0.200(14) 0.248(18) 0.107(15) -0.011(12) -0.033(11)
C15 0.139(8) 0.086(6) 0.171(10) -0.007(7) -0.025(7) -0.007(6)
C24 0.188(10) 0.144(10) 0.157(10) -0.018(9) 0.034(9) -0.058(9)
C5 0.151(11) 0.155(12) 0.158(12) 0.028(10) 0.017(11) 0.006(9)
C20 0.202(13) 0.129(9) 0.150(11) -0.009(9) -0.036(10) -0.015(10)
C14 0.136(8) 0.099(7) 0.168(11) 0.016(8) -0.025(8) -0.017(7)
C11 0.135(8) 0.116(9) 0.217(14) 0.033(9) 0.026(9) -0.012(7)
C2 0.113(7) 0.104(8) 0.149(11) 0.007(7) 0.017(7) -0.006(6)
C19 0.171(10) 0.103(7) 0.148(10) -0.009(7) -0.022(8) -0.011(7)
C23 0.33(2) 0.199(17) 0.216(18) -0.009(13) 0.058(17) -0.027(17)
C16 0.159(9) 0.112(7) 0.144(10) -0.004(7) -0.025(8) 0.002(8)
C4 0.132(9) 0.145(10) 0.163(13) 0.039(10) -0.002(9) 0.000(8)
C7A 0.125(12) 0.172(16) 0.151(16) 0.062(12) 0.052(10) 0.040(12)
C8A 0.164(14) 0.167(17) 0.27(2) 0.097(14) 0.057(13) 0.026(14)
C7B 0.127(13) 0.135(16) 0.216(16) 0.055(15) 0.040(12) 0.057(11)
C8B 0.158(14) 0.170(19) 0.206(15) 0.107(15) 0.058(13) 0.029(13)
C6 0.153(9) 0.165(10) 0.162(11) 0.022(8) 0.061(8) 0.011(7)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ta1 F3 1.795(7) . ?
Ta1 F6 1.821(7) . ?
Ta1 F2 1.837(7) . ?
Ta1 F4 1.842(8) . ?
Ta1 F5 1.846(7) . ?
Ta1 F1 1.867(6) . ?
N1 C2 1.283(12) . ?
N1 C5 1.331(16) . ?
N1 C6 1.486(11) . ?
C21 C20 1.503(12) . ?
C21 C22 1.505(12) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C9 C10 1.459(12) . ?
C9 C8A 1.494(10) . ?
C9 C8B 1.568(5) . ?
C9 H9AA 0.9700 . ?
C9 H9BA 0.9700 . ?
C9 H9AB 0.9700 . ?
C9 H9BB 0.9700 . ?
C18 C17 1.509(11) . ?
C18 C19 1.512(11) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C17 C16 1.518(11) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C13 C14 1.505(11) . ?
C13 C12 1.512(11) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
N3 C2 1.307(12) . ?
N3 C4 1.363(14) . ?
N3 C24 1.483(14) . ?
C22 C23 1.510(10) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C12 C11 1.488(11) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C10 C11 1.491(9) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C15 C16 1.513(11) . ?
C15 C14 1.514(10) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C5 C4 1.324(18) . ?
C5 H5 0.9300 . ?
C20 C19 1.516(11) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C2 H2 0.9300 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C4 H4 0.9300 . ?
C7A C6 1.492(10) . ?
C7A C8A 1.525(11) . ?
C7A H7A1 0.9700 . ?
C7A H7A2 0.9700 . ?
C8A H8A1 0.9700 . ?
C8A H8A2 0.9700 . ?
C7B C8B 1.491(8) . ?
C7B C6 1.585(7) . ?
C7B H7B1 0.9700 . ?
C7B H7B2 0.9700 . ?
C8B H8B1 0.9700 . ?
C8B H8B2 0.9700 . ?
C6 H6AA 0.9700 . ?
C6 H6BA 0.9700 . ?
C6 H6AB 0.9700 . ?
C6 H6BB 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F3 Ta1 F6 93.7(4) . . ?
F3 Ta1 F2 90.8(5) . . ?
F6 Ta1 F2 90.6(4) . . ?
F3 Ta1 F4 88.5(4) . . ?
F6 Ta1 F4 94.0(4) . . ?
F2 Ta1 F4 175.3(4) . . ?
F3 Ta1 F5 176.9(3) . . ?
F6 Ta1 F5 89.1(3) . . ?
F2 Ta1 F5 90.5(5) . . ?
F4 Ta1 F5 90.0(4) . . ?
F3 Ta1 F1 87.7(4) . . ?
F6 Ta1 F1 178.5(3) . . ?
F2 Ta1 F1 89.0(4) . . ?
F4 Ta1 F1 86.3(4) . . ?
F5 Ta1 F1 89.5(3) . . ?
C2 N1 C5 113.3(12) . . ?
C2 N1 C6 125.8(12) . . ?
C5 N1 C6 119.7(13) . . ?
C20 C21 C22 113.6(12) . . ?
C20 C21 H21A 108.9 . . ?
C22 C21 H21A 108.9 . . ?
C20 C21 H21B 108.9 . . ?
C22 C21 H21B 108.9 . . ?
H21A C21 H21B 107.7 . . ?
C10 C9 C8A 123.7(13) . . ?
C10 C9 C8B 103.8(8) . . ?
C8A C9 C8B 33.1(9) . . ?
C10 C9 H9AA 106.4 . . ?
C8A C9 H9AA 106.4 . . ?
C8B C9 H9AA 90.0 . . ?
C10 C9 H9BA 106.4 . . ?
C8A C9 H9BA 106.4 . . ?
C8B C9 H9BA 139.4 . . ?
H9AA C9 H9BA 106.5 . . ?
C10 C9 H9AB 115.7 . . ?
C8A C9 H9AB 112.0 . . ?
C8B C9 H9AB 106.1 . . ?
H9AA C9 H9AB 22.2 . . ?
H9BA C9 H9AB 84.4 . . ?
C10 C9 H9BB 110.6 . . ?
C8A C9 H9BB 77.4 . . ?
C8B C9 H9BB 109.6 . . ?
H9AA C9 H9BB 131.6 . . ?
H9BA C9 H9BB 33.4 . . ?
H9AB C9 H9BB 110.6 . . ?
C17 C18 C19 114.6(10) . . ?
C17 C18 H18A 108.6 . . ?
C19 C18 H18A 108.6 . . ?
C17 C18 H18B 108.6 . . ?
C19 C18 H18B 108.6 . . ?
H18A C18 H18B 107.6 . . ?
C18 C17 C16 114.8(10) . . ?
C18 C17 H17A 108.6 . . ?
C16 C17 H17A 108.6 . . ?
C18 C17 H17B 108.6 . . ?
C16 C17 H17B 108.6 . . ?
H17A C17 H17B 107.5 . . ?
C14 C13 C12 113.4(11) . . ?
C14 C13 H13A 108.9 . . ?
C12 C13 H13A 108.9 . . ?
C14 C13 H13B 108.9 . . ?
C12 C13 H13B 108.9 . . ?
H13A C13 H13B 107.7 . . ?
C2 N3 C4 107.9(11) . . ?
C2 N3 C24 123.1(12) . . ?
C4 N3 C24 129.0(13) . . ?
C21 C22 C23 114.6(15) . . ?
C21 C22 H22A 108.6 . . ?
C23 C22 H22A 108.6 . . ?
C21 C22 H22B 108.6 . . ?
C23 C22 H22B 108.6 . . ?
H22A C22 H22B 107.6 . . ?
C11 C12 C13 111.7(10) . . ?
C11 C12 H12A 109.3 . . ?
C13 C12 H12A 109.3 . . ?
C11 C12 H12B 109.3 . . ?
C13 C12 H12B 109.3 . . ?
H12A C12 H12B 107.9 . . ?
C9 C10 C11 112.8(12) . . ?
C9 C10 H10A 109.0 . . ?
C11 C10 H10A 109.0 . . ?
C9 C10 H10B 109.0 . . ?
C11 C10 H10B 109.0 . . ?
H10A C10 H10B 107.8 . . ?
C16 C15 C14 114.5(9) . . ?
C16 C15 H15A 108.6 . . ?
C14 C15 H15A 108.6 . . ?
C16 C15 H15B 108.6 . . ?
C14 C15 H15B 108.6 . . ?
H15A C15 H15B 107.6 . . ?
N3 C24 H24A 109.5 . . ?
N3 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N3 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C4 C5 N1 103.8(13) . . ?
C4 C5 H5 128.1 . . ?
N1 C5 H5 128.1 . . ?
C21 C20 C19 113.2(11) . . ?
C21 C20 H20A 108.9 . . ?
C19 C20 H20A 108.9 . . ?
C21 C20 H20B 108.9 . . ?
C19 C20 H20B 108.9 . . ?
H20A C20 H20B 107.7 . . ?
C13 C14 C15 113.1(10) . . ?
C13 C14 H14A 109.0 . . ?
C15 C14 H14A 109.0 . . ?
C13 C14 H14B 109.0 . . ?
C15 C14 H14B 109.0 . . ?
H14A C14 H14B 107.8 . . ?
C12 C11 C10 109.4(11) . . ?
C12 C11 H11A 109.8 . . ?
C10 C11 H11A 109.8 . . ?
C12 C11 H11B 109.8 . . ?
C10 C11 H11B 109.8 . . ?
H11A C11 H11B 108.3 . . ?
N1 C2 N3 106.3(10) . . ?
N1 C2 H2 126.9 . . ?
N3 C2 H2 126.9 . . ?
C18 C19 C20 114.1(10) . . ?
C18 C19 H19A 108.7 . . ?
C20 C19 H19A 108.7 . . ?
C18 C19 H19B 108.7 . . ?
C20 C19 H19B 108.7 . . ?
H19A C19 H19B 107.6 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C15 C16 C17 114.5(10) . . ?
C15 C16 H16A 108.6 . . ?
C17 C16 H16A 108.6 . . ?
C15 C16 H16B 108.6 . . ?
C17 C16 H16B 108.6 . . ?
H16A C16 H16B 107.6 . . ?
C5 C4 N3 108.4(13) . . ?
C5 C4 H4 125.8 . . ?
N3 C4 H4 125.8 . . ?
C6 C7A C8A 115.6(12) . . ?
C6 C7A H7A1 108.4 . . ?
C8A C7A H7A1 108.4 . . ?
C6 C7A H7A2 108.4 . . ?
C8A C7A H7A2 108.4 . . ?
H7A1 C7A H7A2 107.5 . . ?
C9 C8A C7A 108.0(11) . . ?
C9 C8A H8A1 110.1 . . ?
C7A C8A H8A1 110.1 . . ?
C9 C8A H8A2 110.1 . . ?
C7A C8A H8A2 110.1 . . ?
H8A1 C8A H8A2 108.4 . . ?
C8B C7B C6 103.3(10) . . ?
C8B C7B H7B1 111.1 . . ?
C6 C7B H7B1 111.1 . . ?
C8B C7B H7B2 111.1 . . ?
C6 C7B H7B2 111.1 . . ?
H7B1 C7B H7B2 109.1 . . ?
C7B C8B C9 107.5(7) . . ?
C7B C8B H8B1 110.2 . . ?
C9 C8B H8B1 110.2 . . ?
C7B C8B H8B2 110.2 . . ?
C9 C8B H8B2 110.2 . . ?
H8B1 C8B H8B2 108.5 . . ?
N1 C6 C7A 123.1(12) . . ?
N1 C6 C7B 101.0(8) . . ?
C7A C6 C7B 38.7(9) . . ?
N1 C6 H6AA 106.5 . . ?
C7A C6 H6AA 106.5 . . ?
C7B C6 H6AA 144.9 . . ?
N1 C6 H6BA 106.5 . . ?
C7A C6 H6BA 106.5 . . ?
C7B C6 H6BA 85.6 . . ?
H6AA C6 H6BA 106.5 . . ?
N1 C6 H6AB 112.0 . . ?
C7A C6 H6AB 77.3 . . ?
C7B C6 H6AB 115.6 . . ?
H6AA C6 H6AB 32.8 . . ?
H6BA C6 H6AB 130.1 . . ?
N1 C6 H6BB 108.9 . . ?
C7A C6 H6BB 120.4 . . ?
C7B C6 H6BB 109.3 . . ?
H6AA C6 H6BB 82.1 . . ?
H6BA C6 H6BB 25.2 . . ?
H6AB C6 H6BB 109.6 . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.068

#============================================================

data_C18MImPF6-55oC
#TrackingRef '- SI-55oC.cif'

_database_code_depnum_ccdc_archive 'CCDC 843142'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            C18MImPF6
_chemical_melting_point          352.9
_chemical_formula_moiety         
;
(C22 N2 H43 +), (P F6 -)
;
_chemical_formula_sum            'C22 H43 F6 N2 P'
_chemical_formula_weight         480.55

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/a

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x-1/2, -y-1/2, z'

_cell_length_a                   9.740(2)
_cell_length_b                   9.526(2)
_cell_length_c                   29.916(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.578(5)
_cell_angle_gamma                90.00
_cell_volume                     2775.5(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    328
_cell_measurement_reflns_used    5094
_cell_measurement_theta_min      5.91
_cell_measurement_theta_max      55.47

_exptl_crystal_description       platelet
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.150
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1032
_exptl_absorpt_coefficient_mu    0.150
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4432
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'RAPID AUTO 2.40 (Rigaku 2006)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      328
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS RapidII'
_diffrn_measurement_method       'imaging plate'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17469
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         2.96
_diffrn_reflns_theta_max         23.25
_reflns_number_total             3979
_reflns_number_gt                1210
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Rigaku R-AXIS Rapid-II'
_computing_cell_refinement       'RAPID AUTO 2.40 (Rigaku 2006)'
_computing_data_reduction        'RAPID AUTO 2.40 (Rigaku 2006)'
_computing_structure_solution    'SIR92 (Altmare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
This structure was solved based on the data at 55 deg C and the octadecyl chain
in this structure has a large conformational flexibility, which results in large
thermal motions of the atoms. Hence, the following restraints were applied.
The N-C and C-C bond lengths in the octadecyl chain were restrained using
the DFIX (1,2 C(N)-C distance: 1.54 A) and DANG (1,3 C(N)-C distance: 2.52 A)
commands in SHELXL. Atomic displacement factors of the disordered part and
some carbon atoms in the octadecyl chain were restrained using DELU and SIMU
in SHELXL. The large R_factor_gt value is caused by the large thermal motions of
the atoms.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3979
_refine_ls_number_parameters     282
_refine_ls_number_restraints     98
_refine_ls_R_factor_all          0.2395
_refine_ls_R_factor_gt           0.1341
_refine_ls_wR_factor_ref         0.4298
_refine_ls_wR_factor_gt          0.3577
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_restrained_S_all      1.193
_refine_ls_shift/su_max          0.042
_refine_ls_shift/su_mean         0.003

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P -0.1702(3) 0.0279(3) 0.10034(11) 0.1494(13) Uani 1 1 d . . .
F4 F -0.2551(8) -0.0356(10) 0.1390(2) 0.278(4) Uani 1 1 d . . .
F3 F -0.2898(8) 0.1261(8) 0.0923(4) 0.314(5) Uani 1 1 d . . .
F2 F -0.0939(9) 0.0734(13) 0.0601(3) 0.330(6) Uani 1 1 d . . .
F5 F -0.0562(6) -0.0798(7) 0.1111(3) 0.243(3) Uani 1 1 d . . .
N1 N 0.3654(11) -0.0272(11) 0.1063(3) 0.147(3) Uani 1 1 d D . .
F6 F -0.0903(9) 0.1300(8) 0.1296(3) 0.294(4) Uani 1 1 d . . .
F1 F -0.2483(5) -0.0809(8) 0.0697(2) 0.220(3) Uani 1 1 d . . .
C21 C -0.622(2) -0.147(2) 0.6779(6) 0.335(9) Uani 1 1 d DU . .
H21A H -0.6996 -0.1002 0.6635 0.402 Uiso 1 1 calc R . .
H21B H -0.6373 -0.2473 0.6766 0.402 Uiso 1 1 calc R . .
C9 C 0.1279(15) -0.1409(19) 0.2411(5) 0.325(9) Uani 1 1 d DU . .
H9A H 0.0487 -0.0968 0.2271 0.390 Uiso 1 1 calc R . .
H9B H 0.1241 -0.2414 0.2362 0.390 Uiso 1 1 calc R . .
C18 C -0.3672(19) -0.1061(19) 0.5790(9) 0.290(9) Uani 1 1 d D . .
H18A H -0.2850 -0.1377 0.5946 0.348 Uiso 1 1 calc R . .
H18B H -0.3647 -0.0043 0.5791 0.348 Uiso 1 1 calc R . .
C17 C -0.354(2) -0.1518(17) 0.5311(7) 0.274(8) Uani 1 1 d D . .
H17A H -0.3575 -0.2536 0.5304 0.329 Uiso 1 1 calc R . .
H17B H -0.4345 -0.1182 0.5149 0.329 Uiso 1 1 calc R . .
C13 C -0.1027(17) -0.1550(18) 0.3880(7) 0.288(8) Uani 1 1 d D . .
H13A H -0.1842 -0.1173 0.3735 0.346 Uiso 1 1 calc R . .
H13B H -0.1092 -0.2566 0.3870 0.346 Uiso 1 1 calc R . .
N3 N 0.3964(11) -0.1227(9) 0.0430(4) 0.142(3) Uani 1 1 d D . .
C22 C -0.608(2) -0.099(3) 0.7256(7) 0.357(10) Uani 1 1 d DU . .
H22A H -0.5939 0.0016 0.7270 0.428 Uiso 1 1 calc R . .
H22B H -0.5310 -0.1454 0.7401 0.428 Uiso 1 1 calc R . .
C12 C 0.0228(19) -0.1092(19) 0.3619(6) 0.289(8) Uani 1 1 d DU . .
H12A H 0.0322 -0.0080 0.3637 0.347 Uiso 1 1 calc R . .
H12B H 0.1044 -0.1511 0.3751 0.347 Uiso 1 1 calc R . .
C10 C 0.1380(18) -0.106(2) 0.2902(6) 0.329(9) Uani 1 1 d DU . .
H10A H 0.2175 -0.1523 0.3032 0.394 Uiso 1 1 calc R . .
H10B H 0.1499 -0.0055 0.2939 0.394 Uiso 1 1 calc R . .
C15 C -0.2315(19) -0.1543(18) 0.4579(5) 0.281(8) Uani 1 1 d DU . .
H15A H -0.3100 -0.1138 0.4424 0.337 Uiso 1 1 calc R . .
H15B H -0.2400 -0.2557 0.4568 0.337 Uiso 1 1 calc R . .
C24 C 0.4599(11) -0.2132(11) 0.0089(3) 0.179(4) Uani 1 1 d . . .
H24A H 0.4323 -0.1820 -0.0204 0.268 Uiso 1 1 calc R . .
H24B H 0.4307 -0.3085 0.0131 0.268 Uiso 1 1 calc R . .
H24C H 0.5580 -0.2080 0.0117 0.268 Uiso 1 1 calc R . .
C5 C 0.2622(14) 0.0183(11) 0.0822(6) 0.162(5) Uani 1 1 d . . .
H5 H 0.1912 0.0771 0.0910 0.195 Uiso 1 1 calc R . .
C20 C -0.4905(18) -0.108(2) 0.6551(7) 0.316(9) Uani 1 1 d DU . .
H20A H -0.4770 -0.0078 0.6574 0.380 Uiso 1 1 calc R . .
H20B H -0.4148 -0.1537 0.6707 0.380 Uiso 1 1 calc R . .
C14 C -0.1008(16) -0.1095(18) 0.4353(7) 0.264(7) Uani 1 1 d DU . .
H14A H -0.0919 -0.0081 0.4369 0.317 Uiso 1 1 calc R . .
H14B H -0.0225 -0.1507 0.4507 0.317 Uiso 1 1 calc R . .
C11 C 0.0116(16) -0.1518(17) 0.3141(5) 0.281(8) Uani 1 1 d DU . .
H11A H -0.0688 -0.1087 0.3004 0.337 Uiso 1 1 calc R . .
H11B H 0.0017 -0.2529 0.3120 0.337 Uiso 1 1 calc R . .
C2 C 0.4450(10) -0.1123(11) 0.0832(5) 0.159(4) Uani 1 1 d D . .
H2 H 0.5232 -0.1573 0.0941 0.190 Uiso 1 1 calc R . .
C19 C -0.487(2) -0.1493(19) 0.6071(7) 0.287(9) Uani 1 1 d D . .
H19A H -0.5696 -0.1121 0.5930 0.345 Uiso 1 1 calc R . .
H19B H -0.4938 -0.2508 0.6057 0.345 Uiso 1 1 calc R . .
C23 C -0.741(3) -0.138(3) 0.7481(7) 0.389(12) Uani 1 1 d DU . .
H23A H -0.7305 -0.2284 0.7622 0.583 Uiso 1 1 calc R . .
H23B H -0.8132 -0.1428 0.7262 0.583 Uiso 1 1 calc R . .
H23C H -0.7626 -0.0691 0.7702 0.583 Uiso 1 1 calc R . .
C16 C -0.2296(18) -0.1065(19) 0.5056(6) 0.276(7) Uani 1 1 d DU . .
H16A H -0.2235 -0.0049 0.5063 0.331 Uiso 1 1 calc R . .
H16B H -0.1482 -0.1437 0.5204 0.331 Uiso 1 1 calc R . .
C4 C 0.2813(12) -0.0375(13) 0.0426(6) 0.169(4) Uani 1 1 d . . .
H4 H 0.2253 -0.0220 0.0177 0.203 Uiso 1 1 calc R . .
C7 C 0.2504(15) -0.064(2) 0.1756(5) 0.329(8) Uani 1 1 d DU . .
H7A H 0.1661 -0.0140 0.1685 0.395 Uiso 1 1 calc R . .
H7B H 0.2446 -0.1568 0.1624 0.395 Uiso 1 1 calc R . .
C8 C 0.2666(15) -0.076(3) 0.2238(5) 0.372(9) Uani 1 1 d DU . .
H8A H 0.2826 0.0155 0.2371 0.447 Uiso 1 1 calc R . .
H8B H 0.3434 -0.1367 0.2313 0.447 Uiso 1 1 calc R . .
C6 C 0.3768(11) 0.0177(13) 0.1557(4) 0.223(5) Uani 1 1 d DU . .
H6A H 0.3671 0.1184 0.1591 0.267 Uiso 1 1 calc R . .
H6B H 0.4628 -0.0125 0.1692 0.267 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1 0.141(2) 0.136(2) 0.171(3) 0.003(2) 0.0155(19) 0.003(2)
F4 0.269(8) 0.358(10) 0.207(6) 0.047(6) 0.045(6) -0.027(8)
F3 0.214(7) 0.197(6) 0.530(14) 0.008(8) -0.061(8) 0.083(5)
F2 0.262(8) 0.518(15) 0.211(7) 0.102(8) 0.021(6) -0.161(10)
F5 0.190(5) 0.191(5) 0.346(9) -0.022(5) -0.050(6) 0.043(5)
N1 0.127(6) 0.149(7) 0.166(8) 0.043(7) -0.025(7) -0.022(6)
F6 0.262(8) 0.211(6) 0.408(11) -0.115(7) -0.072(8) -0.019(6)
F1 0.156(4) 0.239(6) 0.264(6) -0.095(5) 0.014(4) -0.030(4)
C21 0.339(19) 0.306(18) 0.358(17) -0.046(16) -0.097(16) -0.018(19)
C9 0.217(13) 0.309(18) 0.45(2) 0.169(19) 0.002(16) -0.044(13)
C18 0.28(2) 0.240(18) 0.35(3) -0.066(19) -0.11(2) -0.003(15)
C17 0.34(2) 0.220(15) 0.263(18) 0.022(13) -0.051(16) -0.077(14)
C13 0.257(18) 0.261(17) 0.34(2) 0.086(17) -0.083(16) -0.102(14)
N3 0.146(8) 0.120(6) 0.159(7) 0.014(6) -0.007(6) -0.033(6)
C22 0.31(2) 0.35(2) 0.41(2) -0.13(2) -0.108(15) -0.026(19)
C12 0.238(14) 0.223(14) 0.40(2) -0.015(16) -0.026(15) -0.043(12)
C10 0.274(18) 0.275(17) 0.44(2) 0.061(19) 0.012(17) -0.056(14)
C15 0.306(16) 0.266(15) 0.270(16) 0.042(12) -0.076(15) -0.082(13)
C24 0.211(10) 0.143(8) 0.183(9) -0.023(7) 0.033(8) -0.011(7)
C5 0.167(11) 0.152(9) 0.169(10) -0.008(8) 0.041(10) 0.006(8)
C20 0.260(17) 0.288(19) 0.40(2) -0.132(18) -0.123(14) 0.038(16)
C14 0.249(15) 0.234(15) 0.308(15) -0.022(14) -0.062(13) -0.029(12)
C11 0.239(13) 0.224(14) 0.38(2) 0.066(13) -0.042(15) -0.093(11)
C2 0.115(7) 0.125(8) 0.236(15) 0.012(8) 0.032(9) 0.020(6)
C19 0.29(2) 0.239(17) 0.34(2) 0.024(16) -0.070(18) -0.061(15)
C23 0.43(3) 0.36(3) 0.37(2) -0.024(19) -0.046(19) -0.03(3)
C16 0.278(17) 0.243(16) 0.306(16) -0.001(14) -0.060(13) -0.040(13)
C4 0.129(8) 0.144(8) 0.233(15) 0.051(9) -0.032(9) 0.012(7)
C7 0.218(12) 0.461(18) 0.308(16) -0.034(17) 0.030(14) 0.024(14)
C8 0.248(14) 0.489(19) 0.381(17) 0.108(19) 0.022(16) -0.064(14)
C6 0.155(9) 0.260(13) 0.252(13) -0.043(10) -0.031(9) -0.014(9)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 F2 1.486(7) . ?
P1 F3 1.512(7) . ?
P1 F6 1.518(7) . ?
P1 F5 1.543(6) . ?
P1 F4 1.551(7) . ?
P1 F1 1.576(6) . ?
N1 C5 1.305(13) . ?
N1 C2 1.321(11) . ?
N1 C6 1.540(10) . ?
C21 C22 1.503(14) . ?
C21 C20 1.506(14) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C9 C10 1.507(13) . ?
C9 C8 1.578(12) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C18 C19 1.504(13) . ?
C18 C17 1.505(12) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C17 C16 1.503(13) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C13 C14 1.481(12) . ?
C13 C12 1.522(12) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
N3 C2 1.293(8) . ?
N3 C4 1.383(12) . ?
N3 C24 1.477(11) . ?
C22 C23 1.508(10) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C12 C11 1.489(12) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C10 C11 1.495(12) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C15 C16 1.497(13) . ?
C15 C14 1.509(12) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C5 C4 1.315(13) . ?
C5 H5 0.9300 . ?
C20 C19 1.489(13) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C2 H2 0.9300 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C4 H4 0.9300 . ?
C7 C8 1.454(9) . ?
C7 C6 1.578(9) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F2 P1 F3 94.6(6) . . ?
F2 P1 F6 91.3(5) . . ?
F3 P1 F6 94.9(5) . . ?
F2 P1 F5 89.9(5) . . ?
F3 P1 F5 175.1(5) . . ?
F6 P1 F5 86.7(4) . . ?
F2 P1 F4 172.9(5) . . ?
F3 P1 F4 86.8(5) . . ?
F6 P1 F4 95.4(5) . . ?
F5 P1 F4 88.4(4) . . ?
F2 P1 F1 87.8(5) . . ?
F3 P1 F1 86.9(5) . . ?
F6 P1 F1 178.0(4) . . ?
F5 P1 F1 91.5(4) . . ?
F4 P1 F1 85.4(4) . . ?
C5 N1 C2 111.5(10) . . ?
C5 N1 C6 119.1(13) . . ?
C2 N1 C6 129.4(13) . . ?
C22 C21 C20 106.6(19) . . ?
C22 C21 H21A 110.4 . . ?
C20 C21 H21A 110.4 . . ?
C22 C21 H21B 110.4 . . ?
C20 C21 H21B 110.4 . . ?
H21A C21 H21B 108.6 . . ?
C10 C9 C8 100.8(11) . . ?
C10 C9 H9A 111.6 . . ?
C8 C9 H9A 111.6 . . ?
C10 C9 H9B 111.6 . . ?
C8 C9 H9B 111.6 . . ?
H9A C9 H9B 109.4 . . ?
C19 C18 C17 121.8(17) . . ?
C19 C18 H18A 106.9 . . ?
C17 C18 H18A 106.9 . . ?
C19 C18 H18B 106.9 . . ?
C17 C18 H18B 106.9 . . ?
H18A C18 H18B 106.7 . . ?
C16 C17 C18 118.4(17) . . ?
C16 C17 H17A 107.7 . . ?
C18 C17 H17A 107.7 . . ?
C16 C17 H17B 107.7 . . ?
C18 C17 H17B 107.7 . . ?
H17A C17 H17B 107.1 . . ?
C14 C13 C12 113.9(15) . . ?
C14 C13 H13A 108.8 . . ?
C12 C13 H13A 108.8 . . ?
C14 C13 H13B 108.8 . . ?
C12 C13 H13B 108.8 . . ?
H13A C13 H13B 107.7 . . ?
C2 N3 C4 104.6(11) . . ?
C2 N3 C24 122.4(12) . . ?
C4 N3 C24 132.9(14) . . ?
C21 C22 C23 106.1(17) . . ?
C21 C22 H22A 110.5 . . ?
C23 C22 H22A 110.5 . . ?
C21 C22 H22B 110.5 . . ?
C23 C22 H22B 110.5 . . ?
H22A C22 H22B 108.7 . . ?
C11 C12 C13 111.3(16) . . ?
C11 C12 H12A 109.4 . . ?
C13 C12 H12A 109.4 . . ?
C11 C12 H12B 109.4 . . ?
C13 C12 H12B 109.4 . . ?
H12A C12 H12B 108.0 . . ?
C11 C10 C9 110.8(13) . . ?
C11 C10 H10A 109.5 . . ?
C9 C10 H10A 109.5 . . ?
C11 C10 H10B 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?
C16 C15 C14 109.7(18) . . ?
C16 C15 H15A 109.7 . . ?
C14 C15 H15A 109.7 . . ?
C16 C15 H15B 109.7 . . ?
C14 C15 H15B 109.7 . . ?
H15A C15 H15B 108.2 . . ?
N3 C24 H24A 109.5 . . ?
N3 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N3 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N1 C5 C4 104.4(11) . . ?
N1 C5 H5 127.8 . . ?
C4 C5 H5 127.8 . . ?
C19 C20 C21 113.6(18) . . ?
C19 C20 H20A 108.8 . . ?
C21 C20 H20A 108.8 . . ?
C19 C20 H20B 108.8 . . ?
C21 C20 H20B 108.8 . . ?
H20A C20 H20B 107.7 . . ?
C13 C14 C15 110.0(15) . . ?
C13 C14 H14A 109.7 . . ?
C15 C14 H14A 109.7 . . ?
C13 C14 H14B 109.7 . . ?
C15 C14 H14B 109.7 . . ?
H14A C14 H14B 108.2 . . ?
C12 C11 C10 109.0(15) . . ?
C12 C11 H11A 109.9 . . ?
C10 C11 H11A 109.9 . . ?
C12 C11 H11B 109.9 . . ?
C10 C11 H11B 109.9 . . ?
H11A C11 H11B 108.3 . . ?
N3 C2 N1 108.8(10) . . ?
N3 C2 H2 125.6 . . ?
N1 C2 H2 125.6 . . ?
C20 C19 C18 119.5(19) . . ?
C20 C19 H19A 107.5 . . ?
C18 C19 H19A 107.5 . . ?
C20 C19 H19B 107.5 . . ?
C18 C19 H19B 107.5 . . ?
H19A C19 H19B 107.0 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C15 C16 C17 113.1(18) . . ?
C15 C16 H16A 109.0 . . ?
C17 C16 H16A 109.0 . . ?
C15 C16 H16B 109.0 . . ?
C17 C16 H16B 109.0 . . ?
H16A C16 H16B 107.8 . . ?
C5 C4 N3 110.5(11) . . ?
C5 C4 H4 124.7 . . ?
N3 C4 H4 124.7 . . ?
C8 C7 C6 109.6(11) . . ?
C8 C7 H7A 109.8 . . ?
C6 C7 H7A 109.8 . . ?
C8 C7 H7B 109.7 . . ?
C6 C7 H7B 109.7 . . ?
H7A C7 H7B 108.2 . . ?
C7 C8 C9 105.8(11) . . ?
C7 C8 H8A 110.5 . . ?
C9 C8 H8A 110.5 . . ?
C7 C8 H8B 110.6 . . ?
C9 C8 H8B 110.6 . . ?
H8A C8 H8B 108.7 . . ?
N1 C6 C7 100.1(8) . . ?
N1 C6 H6A 111.7 . . ?
C7 C6 H6A 111.7 . . ?
N1 C6 H6B 111.7 . . ?
C7 C6 H6B 111.8 . . ?
H6A C6 H6B 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        23.25
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.070

#=END

data_C18MImAsF6-55oC
#TrackingRef '- SI-55oC.cif'

_database_code_depnum_ccdc_archive 'CCDC 843143'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            C18MImAsF6
_chemical_melting_point          351.1
_chemical_formula_moiety         
;
(C22 N2 H43 +), (As F6 -)
;
_chemical_formula_sum            'C22 H43 As F6 N2'
_chemical_formula_weight         524.50

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/a

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x-1/2, -y-1/2, z'

_cell_length_a                   9.7983(11)
_cell_length_b                   9.6239(13)
_cell_length_c                   29.575(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.6869(18)
_cell_angle_gamma                90.00
_cell_volume                     2787.6(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    328
_cell_measurement_reflns_used    6466
_cell_measurement_theta_min      6.07
_cell_measurement_theta_max      54.88

_exptl_crystal_description       platelet
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1104
_exptl_absorpt_coefficient_mu    1.270
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1884
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'RAPID AUTO 2.40 (Rigaku 2006)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      328
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS RapidII'
_diffrn_measurement_method       'imaging plate'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21446
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_sigmaI/netI    0.0539
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         3.03
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4899
_reflns_number_gt                1690
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Rigaku R-AXIS Rapid-II'
_computing_cell_refinement       'RAPID AUTO 2.40 (Rigaku 2006)'
_computing_data_reduction        'RAPID AUTO 2.40 (Rigaku 2006)'
_computing_structure_solution    'SIR92 (Altmare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
This structure was solved based on the data at 55 deg C and the octadecyl chain
in this structure has a large conformational flexibility, which results in large
thermal motions of the atoms. Hence, the following restraints were applied.
The N-C and C-C bond lengths in the octadecyl chain were restrained using
the DFIX (1,2 C(N)-C distance: 1.54 A) and DANG (1,3 C(N)-C distance: 2.52 A)
commands in SHELXL. Atomic displacement factors of the disordered part and
some carbon atoms in the octadecyl chain were restrained using DELU and SIMU
in SHELXL. The large R_factor_gt value is caused by the large thermal motions of
the atoms.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1959P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4899
_refine_ls_number_parameters     282
_refine_ls_number_restraints     77
_refine_ls_R_factor_all          0.1810
_refine_ls_R_factor_gt           0.0853
_refine_ls_wR_factor_ref         0.3303
_refine_ls_wR_factor_gt          0.2410
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_restrained_S_all      0.977
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As -0.16670(9) 0.02836(11) 0.10309(4) 0.1464(7) Uani 1 1 d . . .
F4 F -0.2565(11) -0.0391(12) 0.1445(3) 0.292(5) Uani 1 1 d . . .
F3 F -0.2938(8) 0.1317(8) 0.0942(4) 0.319(5) Uani 1 1 d . . .
F2 F -0.0855(9) 0.0802(16) 0.0580(3) 0.339(6) Uani 1 1 d . . .
F5 F -0.0410(7) -0.0864(9) 0.1132(3) 0.249(3) Uani 1 1 d . . .
N1 N 0.3669(10) -0.0246(10) 0.1083(3) 0.146(2) Uani 1 1 d D . .
F6 F -0.0778(9) 0.1349(9) 0.1358(4) 0.301(5) Uani 1 1 d . . .
F1 F -0.2529(6) -0.0875(8) 0.0698(3) 0.225(3) Uani 1 1 d . . .
C21 C -0.615(2) -0.151(3) 0.6753(7) 0.316(9) Uani 1 1 d DU . .
H21A H -0.6219 -0.2510 0.6731 0.379 Uiso 1 1 calc R . .
H21B H -0.6954 -0.1120 0.6600 0.379 Uiso 1 1 calc R . .
C9 C 0.1400(16) -0.1436(19) 0.2433(6) 0.317(9) Uani 1 1 d DU . .
H9A H 0.0521 -0.1344 0.2275 0.381 Uiso 1 1 calc R . .
H9B H 0.1727 -0.2383 0.2407 0.381 Uiso 1 1 calc R . .
C18 C -0.3674(19) -0.100(2) 0.5778(9) 0.279(9) Uani 1 1 d D . .
H18A H -0.2847 -0.1238 0.5950 0.335 Uiso 1 1 calc R . .
H18B H -0.3731 0.0005 0.5767 0.335 Uiso 1 1 calc R . .
C17 C -0.354(2) -0.1530(19) 0.5304(7) 0.263(8) Uani 1 1 d D . .
H17A H -0.3495 -0.2536 0.5316 0.316 Uiso 1 1 calc R . .
H17B H -0.4363 -0.1285 0.5133 0.316 Uiso 1 1 calc R . .
C13 C -0.0928(19) -0.1631(19) 0.3864(7) 0.271(8) Uani 1 1 d D . .
H13A H -0.0809 -0.2626 0.3897 0.325 Uiso 1 1 calc R . .
H13B H -0.1775 -0.1469 0.3694 0.325 Uiso 1 1 calc R . .
N3 N 0.3993(9) -0.1223(8) 0.0459(4) 0.138(2) Uani 1 1 d . . .
C22 C -0.619(2) -0.111(3) 0.7243(8) 0.373(11) Uani 1 1 d DU . .
H22A H -0.5989 -0.0131 0.7271 0.448 Uiso 1 1 calc R . .
H22B H -0.5477 -0.1618 0.7406 0.448 Uiso 1 1 calc R . .
C12 C 0.0240(17) -0.1042(19) 0.3609(7) 0.262(7) Uani 1 1 d DU . .
H12A H 0.0165 -0.0037 0.3595 0.314 Uiso 1 1 calc R . .
H12B H 0.1097 -0.1275 0.3763 0.314 Uiso 1 1 calc R . .
C10 C 0.1357(17) -0.096(2) 0.2918(6) 0.303(8) Uani 1 1 d DU . .
H10A H 0.2209 -0.1192 0.3075 0.363 Uiso 1 1 calc R . .
H10B H 0.1249 0.0045 0.2928 0.363 Uiso 1 1 calc R . .
C15 C -0.2154(19) -0.1550(18) 0.4576(7) 0.267(9) Uani 1 1 d D . .
H15A H -0.2036 -0.2550 0.4591 0.321 Uiso 1 1 calc R . .
H15B H -0.2989 -0.1373 0.4401 0.321 Uiso 1 1 calc R . .
C24 C 0.4596(11) -0.2090(12) 0.0114(4) 0.190(4) Uani 1 1 d . . .
H24A H 0.4594 -0.1595 -0.0168 0.285 Uiso 1 1 calc R . .
H24B H 0.4075 -0.2929 0.0078 0.285 Uiso 1 1 calc R . .
H24C H 0.5519 -0.2317 0.0205 0.285 Uiso 1 1 calc R . .
C5 C 0.2678(13) 0.0171(12) 0.0808(6) 0.167(4) Uani 1 1 d . . .
H5 H 0.1976 0.0772 0.0882 0.201 Uiso 1 1 calc R . .
C20 C -0.4937(19) -0.106(3) 0.6506(7) 0.305(8) Uani 1 1 d DU . .
H20A H -0.4130 -0.1391 0.6671 0.366 Uiso 1 1 calc R . .
H20B H -0.4904 -0.0051 0.6510 0.366 Uiso 1 1 calc R . .
C14 C -0.1009(17) -0.097(2) 0.4326(8) 0.254(8) Uani 1 1 d D . .
H14A H -0.0161 -0.1128 0.4495 0.305 Uiso 1 1 calc R . .
H14B H -0.1130 0.0028 0.4292 0.305 Uiso 1 1 calc R . .
C11 C 0.0206(17) -0.1629(19) 0.3145(6) 0.285(8) Uani 1 1 d DU . .
H11A H 0.0324 -0.2630 0.3154 0.342 Uiso 1 1 calc R . .
H11B H -0.0654 -0.1417 0.2990 0.342 Uiso 1 1 calc R . .
C2 C 0.4443(9) -0.1108(10) 0.0874(5) 0.145(3) Uani 1 1 d D . .
H2 H 0.5197 -0.1569 0.1000 0.174 Uiso 1 1 calc R . .
C19 C -0.486(2) -0.153(2) 0.6027(7) 0.263(8) Uani 1 1 d D . .
H19A H -0.4830 -0.2536 0.6023 0.316 Uiso 1 1 calc R . .
H19B H -0.5686 -0.1244 0.5865 0.316 Uiso 1 1 calc R . .
C23 C -0.753(3) -0.140(4) 0.7464(8) 0.427(15) Uani 1 1 d DU . .
H23A H -0.8222 -0.0802 0.7335 0.641 Uiso 1 1 calc R . .
H23B H -0.7431 -0.1216 0.7783 0.641 Uiso 1 1 calc R . .
H23C H -0.7781 -0.2350 0.7417 0.641 Uiso 1 1 calc R . .
C16 C -0.2355(17) -0.1028(19) 0.5051(8) 0.251(8) Uani 1 1 d D . .
H16A H -0.1536 -0.1253 0.5228 0.302 Uiso 1 1 calc R . .
H16B H -0.2413 -0.0023 0.5037 0.302 Uiso 1 1 calc R . .
C4 C 0.2844(12) -0.0398(13) 0.0413(5) 0.157(3) Uani 1 1 d . . .
H4 H 0.2300 -0.0274 0.0153 0.188 Uiso 1 1 calc R . .
C7 C 0.2770(16) -0.0820(19) 0.1810(4) 0.307(8) Uani 1 1 d DU . .
H7A H 0.1929 -0.0857 0.1629 0.368 Uiso 1 1 calc R . .
H7B H 0.3148 -0.1751 0.1827 0.368 Uiso 1 1 calc R . .
C8 C 0.2480(19) -0.033(2) 0.2263(5) 0.312(9) Uani 1 1 d DU . .
H8A H 0.2097 0.0595 0.2255 0.374 Uiso 1 1 calc R . .
H8B H 0.3299 -0.0335 0.2456 0.374 Uiso 1 1 calc R . .
C6 C 0.3811(14) 0.0177(13) 0.1581(4) 0.206(5) Uani 1 1 d D . .
H6A H 0.3565 0.1144 0.1623 0.247 Uiso 1 1 calc R . .
H6B H 0.4733 0.0026 0.1699 0.247 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
As1 0.1351(9) 0.1349(10) 0.1701(11) 0.0009(6) 0.0206(6) 0.0015(6)
F4 0.291(10) 0.353(13) 0.232(8) 0.048(8) 0.027(8) -0.053(9)
F3 0.201(6) 0.181(7) 0.572(18) 0.016(9) -0.016(8) 0.063(5)
F2 0.270(9) 0.519(18) 0.231(8) 0.105(10) 0.044(7) -0.148(11)
F5 0.200(6) 0.197(6) 0.345(10) -0.030(7) -0.052(6) 0.052(5)
N1 0.127(6) 0.152(7) 0.158(7) 0.015(5) 0.011(6) -0.011(5)
F6 0.266(8) 0.222(8) 0.410(12) -0.128(8) -0.054(8) -0.023(7)
F1 0.154(4) 0.245(7) 0.277(7) -0.087(6) 0.027(5) -0.028(5)
C21 0.32(2) 0.30(2) 0.323(17) -0.071(17) -0.058(15) -0.045(18)
C9 0.226(14) 0.31(2) 0.42(2) 0.15(2) 0.041(15) -0.002(13)
C18 0.257(19) 0.202(16) 0.37(3) -0.050(19) -0.07(2) -0.016(15)
C17 0.33(2) 0.191(15) 0.263(18) 0.010(14) -0.077(17) -0.055(15)
C13 0.32(2) 0.212(16) 0.274(18) 0.030(15) -0.054(16) -0.089(15)
N3 0.133(6) 0.111(6) 0.171(7) 0.020(5) 0.019(5) -0.018(5)
C22 0.38(2) 0.36(2) 0.37(2) -0.16(2) -0.046(17) -0.05(2)
C12 0.216(12) 0.188(14) 0.381(19) 0.004(15) -0.020(14) -0.042(12)
C10 0.220(14) 0.30(2) 0.39(2) 0.09(2) -0.013(15) -0.049(14)
C15 0.35(2) 0.197(15) 0.254(16) -0.028(14) -0.071(17) -0.041(16)
C24 0.200(9) 0.166(10) 0.206(9) -0.007(8) 0.049(8) 0.000(8)
C5 0.147(9) 0.168(10) 0.188(11) 0.021(9) 0.017(9) 0.017(7)
C20 0.274(19) 0.27(2) 0.36(2) -0.077(19) -0.087(14) -0.020(17)
C14 0.231(15) 0.238(18) 0.29(2) 0.042(17) 0.004(14) -0.071(14)
C11 0.252(13) 0.231(16) 0.37(2) 0.028(15) -0.001(15) -0.096(12)
C2 0.108(6) 0.133(8) 0.196(10) 0.021(7) 0.019(7) 0.003(6)
C19 0.30(2) 0.215(17) 0.278(19) -0.049(14) -0.045(16) -0.040(15)
C23 0.51(4) 0.45(4) 0.33(2) 0.02(3) 0.03(2) -0.06(4)
C16 0.235(15) 0.172(13) 0.34(3) -0.016(15) -0.050(15) -0.034(12)
C4 0.144(8) 0.157(9) 0.169(10) 0.029(8) -0.001(7) -0.003(7)
C7 0.258(16) 0.43(3) 0.229(14) -0.013(16) 0.019(12) 0.055(17)
C8 0.260(16) 0.39(2) 0.291(16) 0.017(16) 0.080(15) -0.053(14)
C6 0.196(12) 0.189(12) 0.233(15) 0.003(10) 0.003(11) -0.016(9)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
As1 F3 1.609(7) . ?
As1 F6 1.641(7) . ?
As1 F2 1.649(7) . ?
As1 F4 1.661(10) . ?
As1 F5 1.675(7) . ?
As1 F1 1.695(6) . ?
N1 C2 1.295(5) . ?
N1 C5 1.311(14) . ?
N1 C6 1.528(11) . ?
C21 C20 1.479(13) . ?
C21 C22 1.498(14) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C9 C10 1.510(13) . ?
C9 C8 1.589(13) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C18 C19 1.481(13) . ?
C18 C17 1.501(13) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C17 C16 1.480(13) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C13 C12 1.499(13) . ?
C13 C14 1.513(13) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
N3 C2 1.295(11) . ?
N3 C4 1.380(12) . ?
N3 C24 1.457(12) . ?
C22 C23 1.505(10) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C12 C11 1.483(12) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C10 C11 1.479(12) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C15 C14 1.473(12) . ?
C15 C16 1.509(13) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C5 C4 1.306(14) . ?
C5 H5 0.9300 . ?
C20 C19 1.493(13) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C2 H2 0.9300 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C4 H4 0.9300 . ?
C7 C8 1.454(9) . ?
C7 C6 1.570(9) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F3 As1 F6 96.0(5) . . ?
F3 As1 F2 94.1(6) . . ?
F6 As1 F2 91.5(6) . . ?
F3 As1 F4 86.4(5) . . ?
F6 As1 F4 95.4(6) . . ?
F2 As1 F4 173.0(5) . . ?
F3 As1 F5 176.6(4) . . ?
F6 As1 F5 86.1(4) . . ?
F2 As1 F5 88.5(6) . . ?
F4 As1 F5 90.8(5) . . ?
F3 As1 F1 86.7(5) . . ?
F6 As1 F1 177.3(4) . . ?
F2 As1 F1 88.5(5) . . ?
F4 As1 F1 84.5(5) . . ?
F5 As1 F1 91.2(4) . . ?
C2 N1 C5 109.4(10) . . ?
C2 N1 C6 126.4(12) . . ?
C5 N1 C6 124.1(12) . . ?
C20 C21 C22 117(2) . . ?
C20 C21 H21A 108.1 . . ?
C22 C21 H21A 108.1 . . ?
C20 C21 H21B 108.1 . . ?
C22 C21 H21B 108.1 . . ?
H21A C21 H21B 107.3 . . ?
C10 C9 C8 97.7(12) . . ?
C10 C9 H9A 112.2 . . ?
C8 C9 H9A 112.2 . . ?
C10 C9 H9B 112.2 . . ?
C8 C9 H9B 112.2 . . ?
H9A C9 H9B 109.8 . . ?
C19 C18 C17 116.1(17) . . ?
C19 C18 H18A 108.3 . . ?
C17 C18 H18A 108.3 . . ?
C19 C18 H18B 108.3 . . ?
C17 C18 H18B 108.3 . . ?
H18A C18 H18B 107.4 . . ?
C16 C17 C18 117.1(18) . . ?
C16 C17 H17A 108.0 . . ?
C18 C17 H17A 108.0 . . ?
C16 C17 H17B 108.0 . . ?
C18 C17 H17B 108.0 . . ?
H17A C17 H17B 107.3 . . ?
C12 C13 C14 110.8(16) . . ?
C12 C13 H13A 109.5 . . ?
C14 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 108.1 . . ?
C2 N3 C4 107.4(9) . . ?
C2 N3 C24 125.3(10) . . ?
C4 N3 C24 127.3(12) . . ?
C21 C22 C23 115(2) . . ?
C21 C22 H22A 108.5 . . ?
C23 C22 H22A 108.5 . . ?
C21 C22 H22B 108.5 . . ?
C23 C22 H22B 108.5 . . ?
H22A C22 H22B 107.5 . . ?
C11 C12 C13 108.9(16) . . ?
C11 C12 H12A 109.9 . . ?
C13 C12 H12A 109.9 . . ?
C11 C12 H12B 109.9 . . ?
C13 C12 H12B 109.9 . . ?
H12A C12 H12B 108.3 . . ?
C11 C10 C9 110.0(13) . . ?
C11 C10 H10A 109.7 . . ?
C9 C10 H10A 109.7 . . ?
C11 C10 H10B 109.7 . . ?
C9 C10 H10B 109.7 . . ?
H10A C10 H10B 108.2 . . ?
C14 C15 C16 117.6(18) . . ?
C14 C15 H15A 107.9 . . ?
C16 C15 H15A 107.9 . . ?
C14 C15 H15B 107.9 . . ?
C16 C15 H15B 107.9 . . ?
H15A C15 H15B 107.2 . . ?
N3 C24 H24A 109.5 . . ?
N3 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N3 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C4 C5 N1 108.5(11) . . ?
C4 C5 H5 125.7 . . ?
N1 C5 H5 125.7 . . ?
C21 C20 C19 116.5(19) . . ?
C21 C20 H20A 108.2 . . ?
C19 C20 H20A 108.2 . . ?
C21 C20 H20B 108.2 . . ?
C19 C20 H20B 108.2 . . ?
H20A C20 H20B 107.3 . . ?
C15 C14 C13 110.7(17) . . ?
C15 C14 H14A 109.5 . . ?
C13 C14 H14A 109.5 . . ?
C15 C14 H14B 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 108.1 . . ?
C10 C11 C12 104.9(15) . . ?
C10 C11 H11A 110.8 . . ?
C12 C11 H11A 110.8 . . ?
C10 C11 H11B 110.8 . . ?
C12 C11 H11B 110.8 . . ?
H11A C11 H11B 108.8 . . ?
N1 C2 N3 108.6(9) . . ?
N1 C2 H2 125.7 . . ?
N3 C2 H2 125.7 . . ?
C18 C19 C20 115.5(18) . . ?
C18 C19 H19A 108.4 . . ?
C20 C19 H19A 108.4 . . ?
C18 C19 H19B 108.4 . . ?
C20 C19 H19B 108.4 . . ?
H19A C19 H19B 107.5 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C17 C16 C15 119.2(18) . . ?
C17 C16 H16A 107.5 . . ?
C15 C16 H16A 107.5 . . ?
C17 C16 H16B 107.5 . . ?
C15 C16 H16B 107.5 . . ?
H16A C16 H16B 107.0 . . ?
C5 C4 N3 106.0(11) . . ?
C5 C4 H4 127.0 . . ?
N3 C4 H4 127.0 . . ?
C8 C7 C6 110.4(11) . . ?
C8 C7 H7A 109.6 . . ?
C6 C7 H7A 109.6 . . ?
C8 C7 H7B 109.6 . . ?
C6 C7 H7B 109.6 . . ?
H7A C7 H7B 108.1 . . ?
C7 C8 C9 103.1(11) . . ?
C7 C8 H8A 111.2 . . ?
C9 C8 H8A 111.2 . . ?
C7 C8 H8B 111.2 . . ?
C9 C8 H8B 111.2 . . ?
H8A C8 H8B 109.1 . . ?
N1 C6 C7 102.2(9) . . ?
N1 C6 H6A 111.3 . . ?
C7 C6 H6A 111.3 . . ?
N1 C6 H6B 111.3 . . ?
C7 C6 H6B 111.3 . . ?
H6A C6 H6B 109.2 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.067

#=END

data_C18MImSbF6-55oC
#TrackingRef '- SI-55oC.cif'

_database_code_depnum_ccdc_archive 'CCDC 843144'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            C18MImSbF6
_chemical_melting_point          347.5
_chemical_formula_moiety         
;
(C22 N2 H43 +), (Sb F6 -)
;
_chemical_formula_sum            'C22 H43 F6 N2 Sb'
_chemical_formula_weight         571.33

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/a

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x-1/2, -y-1/2, z'

_cell_length_a                   9.9860(13)
_cell_length_b                   9.8314(14)
_cell_length_c                   29.360(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.795(2)
_cell_angle_gamma                90.00
_cell_volume                     2879.0(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    328
_cell_measurement_reflns_used    9368
_cell_measurement_theta_min      6.03
_cell_measurement_theta_max      54.86

_exptl_crystal_description       platelet
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1176
_exptl_absorpt_coefficient_mu    1.007
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2423
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'RAPID AUTO 2.40 (Rigaku 2006)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      328
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS RapidII'
_diffrn_measurement_method       'imaging plate'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22176
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_sigmaI/netI    0.0451
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5061
_reflns_number_gt                2149
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Rigaku R-AXIS Rapid-II'
_computing_cell_refinement       'RAPID AUTO 2.40 (Rigaku 2006)'
_computing_data_reduction        'RAPID AUTO 2.40 (Rigaku 2006)'
_computing_structure_solution    'SIR92 (Altmare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
This structure was solved based on the data at 55 deg C and the octadecyl chain
in this structure has a large conformational flexibility, which results in large
thermal motions of the atoms. Hence, the following restraints were applied.
The N-C and C-C bond lengths in the octadecyl chain were restrained using
the DFIX (1,2 C-C distance: 1.54 A) and DANG (1,3 C-C distance: 2.52 A)
commands in SHELXL. Atomic displacement factors of the disordered part and
some carbon atoms in the octadecyl chain were restrained using DELU and SIMU
in SHELXL.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1517P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5061
_refine_ls_number_parameters     282
_refine_ls_number_restraints     69
_refine_ls_R_factor_all          0.1207
_refine_ls_R_factor_gt           0.0691
_refine_ls_wR_factor_ref         0.2652
_refine_ls_wR_factor_gt          0.2048
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sb1 Sb -0.16386(6) 0.03251(8) 0.10680(2) 0.1596(5) Uani 1 1 d . . .
F4 F -0.2636(15) -0.0413(14) 0.1523(4) 0.328(6) Uani 1 1 d . . .
F3 F -0.3006(9) 0.1439(9) 0.0965(5) 0.355(6) Uani 1 1 d . . .
F2 F -0.0776(12) 0.0891(18) 0.0570(4) 0.391(9) Uani 1 1 d . . .
F5 F -0.0336(8) -0.0926(10) 0.1209(4) 0.277(4) Uani 1 1 d . . .
N1 N 0.3724(10) -0.0311(10) 0.1115(3) 0.165(3) Uani 1 1 d D . .
F6 F -0.0687(10) 0.1455(9) 0.1438(4) 0.318(5) Uani 1 1 d . . .
F1 F -0.2527(6) -0.0943(10) 0.0702(3) 0.257(4) Uani 1 1 d . . .
C21 C -0.619(2) -0.164(2) 0.6743(7) 0.343(9) Uani 1 1 d DU . .
H21A H -0.5946 -0.2582 0.6798 0.412 Uiso 1 1 calc R . .
H21B H -0.7037 -0.1619 0.6566 0.412 Uiso 1 1 calc R . .
C9 C 0.1507(15) -0.1456(19) 0.2492(5) 0.293(8) Uani 1 1 d DU . .
H9A H 0.0659 -0.1311 0.2324 0.352 Uiso 1 1 calc R . .
H9B H 0.1749 -0.2410 0.2476 0.352 Uiso 1 1 calc R . .
C18 C -0.3780(19) -0.092(2) 0.5773(8) 0.292(9) Uani 1 1 d D . .
H18A H -0.4017 0.0028 0.5720 0.351 Uiso 1 1 calc R . .
H18B H -0.2964 -0.0931 0.5966 0.351 Uiso 1 1 calc R . .
C17 C -0.348(2) -0.1553(19) 0.5318(6) 0.280(8) Uani 1 1 d D . .
H17A H -0.3252 -0.2500 0.5373 0.336 Uiso 1 1 calc R . .
H17B H -0.4301 -0.1541 0.5128 0.336 Uiso 1 1 calc R . .
C13 C -0.0897(18) -0.1581(18) 0.3952(8) 0.296(11) Uani 1 1 d D . .
H13A H -0.0744 -0.2542 0.4010 0.355 Uiso 1 1 calc R . .
H13B H -0.1734 -0.1497 0.3773 0.355 Uiso 1 1 calc R . .
N3 N 0.4002(9) -0.1233(8) 0.0478(3) 0.157(2) Uani 1 1 d . . .
C22 C -0.633(3) -0.092(3) 0.7188(8) 0.375(11) Uani 1 1 d DU . .
H22A H -0.6473 0.0051 0.7138 0.450 Uiso 1 1 calc R . .
H22B H -0.5533 -0.1038 0.7385 0.450 Uiso 1 1 calc R . .
C12 C 0.0213(18) -0.105(2) 0.3678(7) 0.289(10) Uani 1 1 d D . .
H12A H 0.0117 -0.0070 0.3657 0.347 Uiso 1 1 calc R . .
H12B H 0.1055 -0.1231 0.3846 0.347 Uiso 1 1 calc R . .
C10 C 0.1454(17) -0.097(2) 0.2985(6) 0.309(9) Uani 1 1 d D . .
H10A H 0.2283 -0.1213 0.3151 0.371 Uiso 1 1 calc R . .
H10B H 0.1365 0.0009 0.2990 0.371 Uiso 1 1 calc R . .
C15 C -0.2176(19) -0.1607(18) 0.4584(7) 0.257(6) Uani 1 1 d D . .
H15A H -0.1969 -0.2566 0.4621 0.308 Uiso 1 1 calc R . .
H15B H -0.2971 -0.1515 0.4383 0.308 Uiso 1 1 calc R . .
C24 C 0.4650(11) -0.2108(12) 0.0129(4) 0.202(4) Uani 1 1 d . . .
H24A H 0.4617 -0.1648 -0.0160 0.303 Uiso 1 1 calc R . .
H24B H 0.4179 -0.2957 0.0099 0.303 Uiso 1 1 calc R . .
H24C H 0.5568 -0.2276 0.0226 0.303 Uiso 1 1 calc R . .
C5 C 0.2771(16) 0.0156(13) 0.0841(7) 0.194(4) Uani 1 1 d . . .
H5 H 0.2114 0.0776 0.0916 0.232 Uiso 1 1 calc R . .
C20 C -0.513(2) -0.093(2) 0.6490(6) 0.308(8) Uani 1 1 d DU . .
H20A H -0.4297 -0.0945 0.6676 0.370 Uiso 1 1 calc R . .
H20B H -0.5385 0.0009 0.6443 0.370 Uiso 1 1 calc R . .
C14 C -0.1040(19) -0.087(2) 0.4400(7) 0.266(8) Uani 1 1 d D . .
H14A H -0.0236 -0.0966 0.4597 0.320 Uiso 1 1 calc R . .
H14B H -0.1242 0.0086 0.4358 0.320 Uiso 1 1 calc R . .
C11 C 0.0310(15) -0.1599(18) 0.3208(6) 0.281(8) Uani 1 1 d D . .
H11A H 0.0429 -0.2578 0.3221 0.337 Uiso 1 1 calc R . .
H11B H -0.0514 -0.1410 0.3031 0.337 Uiso 1 1 calc R . .
C2 C 0.4460(10) -0.1140(11) 0.0896(5) 0.168(3) Uani 1 1 d . . .
H2 H 0.5205 -0.1601 0.1020 0.202 Uiso 1 1 calc R . .
C19 C -0.489(2) -0.1579(19) 0.6034(6) 0.296(8) Uani 1 1 d DU . .
H19A H -0.5715 -0.1541 0.5847 0.356 Uiso 1 1 calc R . .
H19B H -0.4666 -0.2530 0.6082 0.356 Uiso 1 1 calc R . .
C23 C -0.753(3) -0.155(3) 0.7396(8) 0.431(15) Uani 1 1 d DU . .
H23A H -0.8229 -0.1673 0.7165 0.646 Uiso 1 1 calc R . .
H23B H -0.7838 -0.0957 0.7630 0.646 Uiso 1 1 calc R . .
H23C H -0.7279 -0.2409 0.7527 0.646 Uiso 1 1 calc R . .
C16 C -0.2392(18) -0.095(2) 0.5044(7) 0.264(7) Uani 1 1 d D . .
H16A H -0.1555 -0.0994 0.5226 0.317 Uiso 1 1 calc R . .
H16B H -0.2596 0.0006 0.4993 0.317 Uiso 1 1 calc R . .
C4 C 0.2896(14) -0.0405(13) 0.0434(6) 0.184(4) Uani 1 1 d . . .
H4 H 0.2348 -0.0265 0.0173 0.221 Uiso 1 1 calc R . .
C7 C 0.2801(17) -0.091(2) 0.1830(5) 0.306(8) Uani 1 1 d DU . .
H7A H 0.1953 -0.0821 0.1657 0.367 Uiso 1 1 calc R . .
H7B H 0.3091 -0.1846 0.1813 0.367 Uiso 1 1 calc R . .
C8 C 0.262(2) -0.054(2) 0.2313(5) 0.320(8) Uani 1 1 d DU . .
H8A H 0.2364 0.0413 0.2335 0.384 Uiso 1 1 calc R . .
H8B H 0.3450 -0.0672 0.2493 0.384 Uiso 1 1 calc R . .
C6 C 0.3869(15) 0.0042(15) 0.1620(4) 0.223(5) Uani 1 1 d D . .
H6A H 0.3670 0.0993 0.1672 0.267 Uiso 1 1 calc R . .
H6B H 0.4765 -0.0159 0.1744 0.267 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Sb1 0.1519(6) 0.1444(7) 0.1844(7) 0.0024(4) 0.0256(4) -0.0003(3)
F4 0.340(14) 0.401(16) 0.246(9) 0.045(9) 0.031(9) -0.050(11)
F3 0.260(8) 0.214(8) 0.59(2) 0.041(10) -0.015(9) 0.085(7)
F2 0.333(13) 0.58(2) 0.265(9) 0.100(13) 0.056(8) -0.192(16)
F5 0.228(7) 0.228(7) 0.365(11) -0.025(8) -0.075(7) 0.040(6)
N1 0.154(6) 0.162(7) 0.182(8) 0.032(6) 0.019(6) -0.008(5)
F6 0.323(10) 0.214(8) 0.410(13) -0.092(8) -0.055(9) -0.031(7)
F1 0.172(5) 0.259(7) 0.339(9) -0.100(7) 0.003(5) -0.018(5)
C21 0.43(2) 0.254(17) 0.343(17) -0.053(14) -0.050(14) -0.094(16)
C9 0.236(13) 0.29(2) 0.353(17) 0.093(17) 0.044(14) -0.029(12)
C18 0.32(2) 0.231(17) 0.32(2) -0.073(18) -0.050(17) -0.001(16)
C17 0.35(2) 0.226(16) 0.257(16) 0.001(15) -0.063(15) -0.056(16)
C13 0.247(16) 0.236(19) 0.40(3) 0.100(19) -0.031(17) -0.081(13)
N3 0.158(6) 0.139(6) 0.175(7) 0.025(5) 0.012(5) -0.031(5)
C22 0.47(3) 0.30(2) 0.34(2) -0.067(18) -0.041(17) -0.10(2)
C12 0.273(19) 0.194(14) 0.39(3) -0.038(19) -0.09(2) 0.015(15)
C10 0.254(17) 0.33(2) 0.33(2) 0.07(2) -0.024(18) -0.038(18)
C15 0.295(19) 0.222(15) 0.250(16) -0.015(13) -0.013(13) 0.002(14)
C24 0.223(9) 0.179(9) 0.208(8) -0.011(8) 0.054(8) -0.037(8)
C5 0.192(11) 0.174(10) 0.219(13) 0.025(10) 0.051(11) 0.011(8)
C20 0.37(2) 0.248(16) 0.299(15) -0.016(13) -0.108(13) -0.053(15)
C14 0.249(17) 0.34(2) 0.208(13) -0.008(15) 0.004(12) 0.001(18)
C11 0.211(13) 0.219(16) 0.41(3) 0.049(17) 0.014(15) -0.078(12)
C2 0.135(6) 0.139(8) 0.234(12) 0.011(8) 0.048(8) 0.002(5)
C19 0.37(2) 0.214(15) 0.292(14) -0.004(12) -0.100(13) -0.044(15)
C23 0.56(4) 0.34(3) 0.39(2) -0.04(2) 0.03(2) -0.11(3)
C16 0.259(17) 0.251(17) 0.279(19) -0.019(16) -0.028(14) -0.018(14)
C4 0.174(10) 0.174(10) 0.204(12) 0.023(8) 0.003(8) 0.000(8)
C7 0.253(15) 0.40(2) 0.268(14) -0.025(17) 0.055(13) 0.025(17)
C8 0.279(16) 0.40(2) 0.286(15) -0.012(16) 0.043(14) -0.099(14)
C6 0.200(12) 0.253(14) 0.218(14) -0.019(10) 0.045(10) -0.015(9)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sb1 F3 1.765(8) . ?
Sb1 F6 1.792(8) . ?
Sb1 F2 1.820(9) . ?
Sb1 F5 1.823(8) . ?
Sb1 F1 1.845(7) . ?
Sb1 F4 1.853(12) . ?
N1 C2 1.290(12) . ?
N1 C5 1.301(18) . ?
N1 C6 1.522(11) . ?
C21 C20 1.497(13) . ?
C21 C22 1.499(14) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C9 C10 1.527(13) . ?
C9 C8 1.544(12) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C18 C17 1.518(13) . ?
C18 C19 1.521(13) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C17 C16 1.504(13) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C13 C12 1.495(13) . ?
C13 C14 1.502(13) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
N3 C2 1.293(12) . ?
N3 C4 1.373(13) . ?
N3 C24 1.507(13) . ?
C22 C23 1.502(10) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C12 C11 1.491(12) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C10 C11 1.479(12) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C15 C14 1.470(13) . ?
C15 C16 1.522(12) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C5 C4 1.327(17) . ?
C5 H5 0.9300 . ?
C20 C19 1.513(13) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C2 H2 0.9300 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C4 H4 0.9300 . ?
C7 C8 1.483(9) . ?
C7 C6 1.566(9) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F3 Sb1 F6 95.9(6) . . ?
F3 Sb1 F2 93.7(7) . . ?
F6 Sb1 F2 92.2(6) . . ?
F3 Sb1 F5 174.3(5) . . ?
F6 Sb1 F5 85.9(5) . . ?
F2 Sb1 F5 91.6(7) . . ?
F3 Sb1 F1 88.5(5) . . ?
F6 Sb1 F1 175.6(4) . . ?
F2 Sb1 F1 88.3(5) . . ?
F5 Sb1 F1 89.7(5) . . ?
F3 Sb1 F4 85.9(6) . . ?
F6 Sb1 F4 95.4(6) . . ?
F2 Sb1 F4 172.4(5) . . ?
F5 Sb1 F4 88.5(6) . . ?
F1 Sb1 F4 84.0(5) . . ?
C2 N1 C5 109.3(11) . . ?
C2 N1 C6 126.9(13) . . ?
C5 N1 C6 123.7(14) . . ?
C20 C21 C22 108.0(17) . . ?
C20 C21 H21A 110.1 . . ?
C22 C21 H21A 110.1 . . ?
C20 C21 H21B 110.1 . . ?
C22 C21 H21B 110.1 . . ?
H21A C21 H21B 108.4 . . ?
C10 C9 C8 101.4(11) . . ?
C10 C9 H9A 111.5 . . ?
C8 C9 H9A 111.5 . . ?
C10 C9 H9B 111.5 . . ?
C8 C9 H9B 111.5 . . ?
H9A C9 H9B 109.3 . . ?
C17 C18 C19 116.6(16) . . ?
C17 C18 H18A 108.1 . . ?
C19 C18 H18A 108.1 . . ?
C17 C18 H18B 108.1 . . ?
C19 C18 H18B 108.1 . . ?
H18A C18 H18B 107.3 . . ?
C16 C17 C18 119.2(17) . . ?
C16 C17 H17A 107.5 . . ?
C18 C17 H17A 107.5 . . ?
C16 C17 H17B 107.5 . . ?
C18 C17 H17B 107.5 . . ?
H17A C17 H17B 107.0 . . ?
C12 C13 C14 114.4(17) . . ?
C12 C13 H13A 108.7 . . ?
C14 C13 H13A 108.7 . . ?
C12 C13 H13B 108.7 . . ?
C14 C13 H13B 108.7 . . ?
H13A C13 H13B 107.6 . . ?
C2 N3 C4 107.0(10) . . ?
C2 N3 C24 122.8(10) . . ?
C4 N3 C24 130.2(12) . . ?
C21 C22 C23 105.5(19) . . ?
C21 C22 H22A 110.6 . . ?
C23 C22 H22A 110.6 . . ?
C21 C22 H22B 110.6 . . ?
C23 C22 H22B 110.6 . . ?
H22A C22 H22B 108.8 . . ?
C11 C12 C13 117.1(17) . . ?
C11 C12 H12A 108.0 . . ?
C13 C12 H12A 108.0 . . ?
C11 C12 H12B 108.0 . . ?
C13 C12 H12B 108.0 . . ?
H12A C12 H12B 107.3 . . ?
C11 C10 C9 110.7(13) . . ?
C11 C10 H10A 109.5 . . ?
C9 C10 H10A 109.5 . . ?
C11 C10 H10B 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?
C14 C15 C16 105.2(16) . . ?
C14 C15 H15A 110.7 . . ?
C16 C15 H15A 110.7 . . ?
C14 C15 H15B 110.7 . . ?
C16 C15 H15B 110.7 . . ?
H15A C15 H15B 108.8 . . ?
N3 C24 H24A 109.5 . . ?
N3 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N3 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N1 C5 C4 108.2(13) . . ?
N1 C5 H5 125.9 . . ?
C4 C5 H5 125.9 . . ?
C21 C20 C19 113.1(18) . . ?
C21 C20 H20A 109.0 . . ?
C19 C20 H20A 109.0 . . ?
C21 C20 H20B 109.0 . . ?
C19 C20 H20B 109.0 . . ?
H20A C20 H20B 107.8 . . ?
C15 C14 C13 101.6(18) . . ?
C15 C14 H14A 111.4 . . ?
C13 C14 H14A 111.4 . . ?
C15 C14 H14B 111.4 . . ?
C13 C14 H14B 111.4 . . ?
H14A C14 H14B 109.3 . . ?
C10 C11 C12 110.3(15) . . ?
C10 C11 H11A 109.6 . . ?
C12 C11 H11A 109.6 . . ?
C10 C11 H11B 109.6 . . ?
C12 C11 H11B 109.6 . . ?
H11A C11 H11B 108.1 . . ?
N1 C2 N3 109.6(10) . . ?
N1 C2 H2 125.2 . . ?
N3 C2 H2 125.2 . . ?
C20 C19 C18 114.7(17) . . ?
C20 C19 H19A 108.6 . . ?
C18 C19 H19A 108.6 . . ?
C20 C19 H19B 108.6 . . ?
C18 C19 H19B 108.6 . . ?
H19A C19 H19B 107.6 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C17 C16 C15 116.3(18) . . ?
C17 C16 H16A 108.2 . . ?
C15 C16 H16A 108.2 . . ?
C17 C16 H16B 108.2 . . ?
C15 C16 H16B 108.2 . . ?
H16A C16 H16B 107.4 . . ?
C5 C4 N3 105.8(12) . . ?
C5 C4 H4 127.1 . . ?
N3 C4 H4 127.1 . . ?
C8 C7 C6 110.4(11) . . ?
C8 C7 H7A 109.6 . . ?
C6 C7 H7A 109.6 . . ?
C8 C7 H7B 109.6 . . ?
C6 C7 H7B 109.6 . . ?
H7A C7 H7B 108.1 . . ?
C7 C8 C9 107.7(11) . . ?
C7 C8 H8A 110.2 . . ?
C9 C8 H8A 110.2 . . ?
C7 C8 H8B 110.2 . . ?
C9 C8 H8B 110.2 . . ?
H8A C8 H8B 108.5 . . ?
N1 C6 C7 102.4(9) . . ?
N1 C6 H6A 111.3 . . ?
C7 C6 H6A 111.3 . . ?
N1 C6 H6B 111.3 . . ?
C7 C6 H6B 111.3 . . ?
H6A C6 H6B 109.2 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.408
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.067

#=END

data_C18MImNbF6-55oC
#TrackingRef '- SI-55oC.cif'

_database_code_depnum_ccdc_archive 'CCDC 843145'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            C18MImNbF6
_chemical_melting_point          347.2
_chemical_formula_moiety         
;
(C22 N2 H43 +), (Nb F6 -)
;
_chemical_formula_sum            'C22 H43 F6 N2 Nb'
_chemical_formula_weight         542.49

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/a

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x-1/2, -y-1/2, z'

_cell_length_a                   9.838(3)
_cell_length_b                   9.772(3)
_cell_length_c                   29.126(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.286(6)
_cell_angle_gamma                90.00
_cell_volume                     2795.5(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    328
_cell_measurement_reflns_used    6232
_cell_measurement_theta_min      5.99
_cell_measurement_theta_max      54.93

_exptl_crystal_description       platelet
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1136
_exptl_absorpt_coefficient_mu    0.480
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2062
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'RAPID AUTO 2.40 (Rigaku 2006)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      328
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS RapidII'
_diffrn_measurement_method       'imaging plate'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18406
_diffrn_reflns_av_R_equivalents  0.0639
_diffrn_reflns_av_sigmaI/netI    0.0745
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         3.00
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4671
_reflns_number_gt                1479
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Rigaku R-AXIS Rapid-II'
_computing_cell_refinement       'RAPID AUTO 2.40 (Rigaku 2006)'
_computing_data_reduction        'RAPID AUTO 2.40 (Rigaku 2006)'
_computing_structure_solution    'SIR92 (Altmare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
This structure was solved based on the data at 55 deg C and the octadecyl chain
in this structure has a large conformational flexibility, which results in large
thermal motions of the atoms. Hence, the following restraints were applied.
The N-C and C-C bond lengths in the octadecyl chain were restrained using
the DFIX (1,2 C-C distance: 1.54 A) and DANG (1,3 C-C distance: 2.52 A)
commands in SHELXL. Atomic displacement factors of the disordered part and
some carbon atoms in the octadecyl chain were restrained using DELU and SIMU
in SHELXL.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1502P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4671
_refine_ls_number_parameters     282
_refine_ls_number_restraints     61
_refine_ls_R_factor_all          0.1995
_refine_ls_R_factor_gt           0.0832
_refine_ls_wR_factor_ref         0.2955
_refine_ls_wR_factor_gt          0.2090
_refine_ls_goodness_of_fit_ref   0.951
_refine_ls_restrained_S_all      0.983
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb -0.16367(9) 0.03298(11) 0.10793(4) 0.1498(7) Uani 1 1 d . . .
F4 F -0.2629(11) -0.0454(11) 0.1523(3) 0.285(5) Uani 1 1 d . . .
F3 F -0.3020(8) 0.1469(8) 0.0961(5) 0.327(6) Uani 1 1 d . . .
F2 F -0.0785(11) 0.0943(15) 0.0596(3) 0.346(7) Uani 1 1 d . . .
F5 F -0.0300(7) -0.0934(9) 0.1196(4) 0.259(4) Uani 1 1 d . . .
N1 N 0.3702(13) -0.0286(14) 0.1107(4) 0.157(3) Uani 1 1 d D . .
F6 F -0.0673(9) 0.1486(8) 0.1463(4) 0.285(4) Uani 1 1 d . . .
F1 F -0.2552(6) -0.0925(9) 0.0683(3) 0.231(3) Uani 1 1 d . . .
C21 C -0.6294(19) -0.1546(18) 0.6715(6) 0.279(8) Uani 1 1 d DU . .
H21A H -0.6240 -0.2536 0.6726 0.335 Uiso 1 1 calc R . .
H21B H -0.7118 -0.1297 0.6536 0.335 Uiso 1 1 calc R . .
C9 C 0.1505(15) -0.1450(16) 0.2483(6) 0.265(8) Uani 1 1 d DU . .
H9A H 0.0650 -0.1283 0.2310 0.318 Uiso 1 1 calc R . .
H9B H 0.1738 -0.2411 0.2460 0.318 Uiso 1 1 calc R . .
C18 C -0.378(2) -0.0960(18) 0.5793(8) 0.242(8) Uani 1 1 d D . .
H18A H -0.2957 -0.1142 0.5985 0.291 Uiso 1 1 calc R . .
H18B H -0.3888 0.0024 0.5772 0.291 Uiso 1 1 calc R . .
C17 C -0.360(2) -0.1527(16) 0.5322(8) 0.249(8) Uani 1 1 d D . .
H17A H -0.4435 -0.1348 0.5136 0.299 Uiso 1 1 calc R . .
H17B H -0.3512 -0.2512 0.5349 0.299 Uiso 1 1 calc R . .
C13 C -0.092(2) -0.1622(17) 0.3890(8) 0.242(8) Uani 1 1 d D . .
H13A H -0.0807 -0.2605 0.3916 0.290 Uiso 1 1 calc R . .
H13B H -0.1750 -0.1443 0.3702 0.290 Uiso 1 1 calc R . .
N3 N 0.4043(13) -0.1263(10) 0.0479(5) 0.143(3) Uani 1 1 d . . .
C22 C -0.636(2) -0.100(2) 0.7194(7) 0.328(9) Uani 1 1 d DU . .
H22A H -0.6368 -0.0005 0.7186 0.393 Uiso 1 1 calc R . .
H22B H -0.5556 -0.1285 0.7379 0.393 Uiso 1 1 calc R . .
C12 C 0.026(2) -0.1010(19) 0.3675(8) 0.264(10) Uani 1 1 d D . .
H12A H 0.1098 -0.1244 0.3848 0.316 Uiso 1 1 calc R . .
H12B H 0.0175 -0.0022 0.3663 0.316 Uiso 1 1 calc R . .
C10 C 0.1427(18) -0.102(2) 0.2980(6) 0.297(10) Uani 1 1 d D . .
H10A H 0.2252 -0.1312 0.3151 0.357 Uiso 1 1 calc R . .
H10B H 0.1385 -0.0032 0.2995 0.357 Uiso 1 1 calc R . .
C15 C -0.2222(18) -0.1540(15) 0.4592(7) 0.225(6) Uani 1 1 d D . .
H15A H -0.2140 -0.2527 0.4613 0.270 Uiso 1 1 calc R . .
H15B H -0.3036 -0.1340 0.4400 0.270 Uiso 1 1 calc R . .
C24 C 0.4624(13) -0.2119(13) 0.0128(5) 0.195(5) Uani 1 1 d . . .
H24A H 0.4418 -0.1728 -0.0170 0.292 Uiso 1 1 calc R . .
H24B H 0.4243 -0.3022 0.0139 0.292 Uiso 1 1 calc R . .
H24C H 0.5594 -0.2170 0.0185 0.292 Uiso 1 1 calc R . .
C5 C 0.2713(17) 0.0177(16) 0.0822(9) 0.192(6) Uani 1 1 d . . .
H5 H 0.2027 0.0790 0.0886 0.230 Uiso 1 1 calc R . .
C20 C -0.5086(17) -0.099(2) 0.6489(7) 0.251(7) Uani 1 1 d DU . .
H20A H -0.5158 -0.0002 0.6471 0.301 Uiso 1 1 calc R . .
H20B H -0.4267 -0.1210 0.6675 0.301 Uiso 1 1 calc R . .
C14 C -0.1035(16) -0.1009(17) 0.4359(7) 0.208(6) Uani 1 1 d D . .
H14A H -0.0210 -0.1208 0.4546 0.250 Uiso 1 1 calc R . .
H14B H -0.1112 -0.0022 0.4330 0.250 Uiso 1 1 calc R . .
C11 C 0.0256(15) -0.1590(16) 0.3199(7) 0.245(8) Uani 1 1 d D . .
H11A H 0.0319 -0.2580 0.3212 0.294 Uiso 1 1 calc R . .
H11B H -0.0580 -0.1344 0.3025 0.294 Uiso 1 1 calc R . .
C2 C 0.4450(12) -0.1157(14) 0.0910(7) 0.145(4) Uani 1 1 d . . .
H2 H 0.5172 -0.1638 0.1053 0.174 Uiso 1 1 calc R . .
C19 C -0.497(2) -0.1556(18) 0.6018(7) 0.263(10) Uani 1 1 d D . .
H19A H -0.5796 -0.1354 0.5832 0.316 Uiso 1 1 calc R . .
H19B H -0.4871 -0.2542 0.6035 0.316 Uiso 1 1 calc R . .
C23 C -0.761(2) -0.151(3) 0.7407(8) 0.388(13) Uani 1 1 d DU . .
H23A H -0.8377 -0.1441 0.7187 0.582 Uiso 1 1 calc R . .
H23B H -0.7782 -0.0969 0.7672 0.582 Uiso 1 1 calc R . .
H23C H -0.7486 -0.2449 0.7496 0.582 Uiso 1 1 calc R . .
C16 C -0.2419(19) -0.0998(18) 0.5063(7) 0.233(7) Uani 1 1 d D . .
H16A H -0.2512 -0.0012 0.5039 0.279 Uiso 1 1 calc R . .
H16B H -0.1591 -0.1177 0.5250 0.279 Uiso 1 1 calc R . .
C4 C 0.2918(19) -0.043(2) 0.0422(7) 0.183(5) Uani 1 1 d . . .
H4 H 0.2389 -0.0308 0.0150 0.220 Uiso 1 1 calc R . .
C7 C 0.2843(17) -0.0913(19) 0.1830(5) 0.297(8) Uani 1 1 d DU . .
H7A H 0.1979 -0.0859 0.1654 0.356 Uiso 1 1 calc R . .
H7B H 0.3168 -0.1848 0.1818 0.356 Uiso 1 1 calc R . .
C8 C 0.2652(19) -0.053(2) 0.2312(5) 0.311(8) Uani 1 1 d DU . .
H8A H 0.2398 0.0427 0.2331 0.374 Uiso 1 1 calc R . .
H8B H 0.3488 -0.0671 0.2499 0.374 Uiso 1 1 calc R . .
C6 C 0.3893(14) 0.0067(13) 0.1618(5) 0.205(5) Uani 1 1 d D . .
H6A H 0.3680 0.1019 0.1674 0.246 Uiso 1 1 calc R . .
H6B H 0.4815 -0.0124 0.1737 0.246 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Nb1 0.1473(9) 0.1446(9) 0.1594(11) 0.0050(7) 0.0271(7) -0.0022(6)
F4 0.308(10) 0.337(12) 0.215(8) 0.048(8) 0.061(8) -0.070(9)
F3 0.220(7) 0.215(8) 0.541(18) 0.034(9) -0.018(9) 0.100(6)
F2 0.337(12) 0.493(17) 0.213(8) 0.079(11) 0.059(8) -0.172(13)
F5 0.193(6) 0.214(6) 0.361(11) -0.043(8) -0.068(7) 0.058(6)
N1 0.155(8) 0.150(8) 0.169(11) 0.004(8) 0.039(9) -0.005(7)
F6 0.289(8) 0.223(8) 0.336(11) -0.084(7) -0.029(8) -0.057(7)
F1 0.176(5) 0.258(7) 0.259(8) -0.089(7) 0.011(5) -0.029(5)
C21 0.318(18) 0.234(16) 0.277(16) -0.043(13) -0.041(14) -0.068(14)
C9 0.224(14) 0.232(17) 0.34(2) 0.087(16) 0.014(15) -0.033(11)
C18 0.27(2) 0.186(13) 0.26(2) -0.059(16) -0.076(18) 0.012(15)
C17 0.28(2) 0.181(14) 0.28(2) -0.007(15) -0.044(17) -0.044(13)
C13 0.266(19) 0.186(14) 0.27(2) 0.004(14) -0.033(16) -0.054(12)
N3 0.141(8) 0.133(8) 0.157(11) 0.022(7) 0.022(8) -0.028(6)
C22 0.35(2) 0.309(19) 0.320(19) -0.107(18) -0.014(15) -0.098(17)
C12 0.28(2) 0.180(13) 0.32(3) -0.032(17) -0.08(2) -0.037(15)
C10 0.28(2) 0.270(19) 0.33(3) 0.01(2) -0.06(2) -0.052(18)
C15 0.265(18) 0.163(12) 0.242(19) -0.010(12) -0.021(15) -0.030(12)
C24 0.240(13) 0.183(10) 0.167(11) -0.022(10) 0.054(10) -0.027(10)
C5 0.162(12) 0.178(12) 0.235(19) 0.042(14) 0.007(14) 0.025(9)
C20 0.252(17) 0.207(14) 0.285(17) -0.051(14) -0.068(12) -0.021(13)
C14 0.204(14) 0.193(12) 0.225(17) 0.006(14) -0.011(13) -0.028(11)
C11 0.184(12) 0.187(13) 0.37(3) 0.020(15) 0.029(15) -0.068(11)
C2 0.146(9) 0.130(9) 0.160(13) 0.021(9) 0.019(10) -0.002(7)
C19 0.29(2) 0.196(15) 0.30(2) -0.038(15) -0.061(18) -0.065(15)
C23 0.48(3) 0.38(3) 0.30(2) -0.03(2) 0.041(19) -0.14(3)
C16 0.27(2) 0.176(13) 0.25(2) -0.031(14) -0.054(16) -0.002(13)
C4 0.173(14) 0.182(14) 0.193(16) 0.024(12) -0.003(12) -0.018(11)
C7 0.243(15) 0.40(2) 0.243(16) -0.024(19) 0.015(14) 0.012(17)
C8 0.293(17) 0.37(2) 0.279(17) 0.014(17) 0.080(17) -0.075(14)
C6 0.193(12) 0.207(12) 0.221(17) -0.015(11) 0.055(12) -0.037(10)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 F3 1.777(7) . ?
Nb1 F2 1.782(8) . ?
Nb1 F6 1.817(7) . ?
Nb1 F5 1.822(7) . ?
Nb1 F4 1.832(9) . ?
Nb1 F1 1.878(7) . ?
N1 C2 1.282(13) . ?
N1 C5 1.322(17) . ?
N1 C6 1.528(11) . ?
C21 C20 1.494(13) . ?
C21 C22 1.498(13) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C9 C10 1.512(13) . ?
C9 C8 1.548(12) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C18 C19 1.494(13) . ?
C18 C17 1.499(13) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C17 C16 1.516(12) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C13 C12 1.480(13) . ?
C13 C14 1.500(12) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
N3 C2 1.300(13) . ?
N3 C4 1.376(16) . ?
N3 C24 1.461(14) . ?
C22 C23 1.500(10) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C12 C11 1.497(12) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C10 C11 1.458(12) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C15 C14 1.479(12) . ?
C15 C16 1.491(12) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C5 C4 1.331(17) . ?
C5 H5 0.9300 . ?
C20 C19 1.490(13) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C2 H2 0.9300 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C4 H4 0.9300 . ?
C7 C8 1.475(9) . ?
C7 C6 1.562(9) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F3 Nb1 F2 91.5(6) . . ?
F3 Nb1 F6 95.5(5) . . ?
F2 Nb1 F6 91.4(5) . . ?
F3 Nb1 F5 176.1(4) . . ?
F2 Nb1 F5 90.5(6) . . ?
F6 Nb1 F5 87.8(4) . . ?
F3 Nb1 F4 88.0(5) . . ?
F2 Nb1 F4 172.5(4) . . ?
F6 Nb1 F4 96.1(5) . . ?
F5 Nb1 F4 89.6(5) . . ?
F3 Nb1 F1 87.4(4) . . ?
F2 Nb1 F1 88.0(5) . . ?
F6 Nb1 F1 177.0(4) . . ?
F5 Nb1 F1 89.3(4) . . ?
F4 Nb1 F1 84.5(4) . . ?
C2 N1 C5 111.5(14) . . ?
C2 N1 C6 123.0(17) . . ?
C5 N1 C6 125.4(18) . . ?
C20 C21 C22 110.9(17) . . ?
C20 C21 H21A 109.4 . . ?
C22 C21 H21A 109.4 . . ?
C20 C21 H21B 109.4 . . ?
C22 C21 H21B 109.4 . . ?
H21A C21 H21B 108.0 . . ?
C10 C9 C8 103.0(12) . . ?
C10 C9 H9A 111.2 . . ?
C8 C9 H9A 111.2 . . ?
C10 C9 H9B 111.2 . . ?
C8 C9 H9B 111.2 . . ?
H9A C9 H9B 109.1 . . ?
C19 C18 C17 112.9(17) . . ?
C19 C18 H18A 109.0 . . ?
C17 C18 H18A 109.0 . . ?
C19 C18 H18B 109.0 . . ?
C17 C18 H18B 109.0 . . ?
H18A C18 H18B 107.8 . . ?
C18 C17 C16 117.5(18) . . ?
C18 C17 H17A 107.9 . . ?
C16 C17 H17A 107.9 . . ?
C18 C17 H17B 107.9 . . ?
C16 C17 H17B 107.9 . . ?
H17A C17 H17B 107.2 . . ?
C12 C13 C14 108.9(17) . . ?
C12 C13 H13A 109.9 . . ?
C14 C13 H13A 109.9 . . ?
C12 C13 H13B 109.9 . . ?
C14 C13 H13B 109.9 . . ?
H13A C13 H13B 108.3 . . ?
C2 N3 C4 105.6(13) . . ?
C2 N3 C24 127.5(16) . . ?
C4 N3 C24 126.9(17) . . ?
C21 C22 C23 110.1(18) . . ?
C21 C22 H22A 109.6 . . ?
C23 C22 H22A 109.6 . . ?
C21 C22 H22B 109.6 . . ?
C23 C22 H22B 109.6 . . ?
H22A C22 H22B 108.2 . . ?
C13 C12 C11 106.3(17) . . ?
C13 C12 H12A 110.5 . . ?
C11 C12 H12A 110.5 . . ?
C13 C12 H12B 110.5 . . ?
C11 C12 H12B 110.5 . . ?
H12A C12 H12B 108.7 . . ?
C11 C10 C9 113.4(14) . . ?
C11 C10 H10A 108.9 . . ?
C9 C10 H10A 108.9 . . ?
C11 C10 H10B 108.9 . . ?
C9 C10 H10B 108.9 . . ?
H10A C10 H10B 107.7 . . ?
C14 C15 C16 116.4(18) . . ?
C14 C15 H15A 108.2 . . ?
C16 C15 H15A 108.2 . . ?
C14 C15 H15B 108.2 . . ?
C16 C15 H15B 108.2 . . ?
H15A C15 H15B 107.3 . . ?
N3 C24 H24A 109.5 . . ?
N3 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N3 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N1 C5 C4 104.8(16) . . ?
N1 C5 H5 127.6 . . ?
C4 C5 H5 127.6 . . ?
C19 C20 C21 112.2(18) . . ?
C19 C20 H20A 109.2 . . ?
C21 C20 H20A 109.2 . . ?
C19 C20 H20B 109.2 . . ?
C21 C20 H20B 109.2 . . ?
H20A C20 H20B 107.9 . . ?
C15 C14 C13 112.3(18) . . ?
C15 C14 H14A 109.2 . . ?
C13 C14 H14A 109.2 . . ?
C15 C14 H14B 109.2 . . ?
C13 C14 H14B 109.2 . . ?
H14A C14 H14B 107.9 . . ?
C10 C11 C12 107.5(17) . . ?
C10 C11 H11A 110.2 . . ?
C12 C11 H11A 110.2 . . ?
C10 C11 H11B 110.2 . . ?
C12 C11 H11B 110.2 . . ?
H11A C11 H11B 108.5 . . ?
N1 C2 N3 109.4(12) . . ?
N1 C2 H2 125.3 . . ?
N3 C2 H2 125.3 . . ?
C20 C19 C18 111.2(17) . . ?
C20 C19 H19A 109.4 . . ?
C18 C19 H19A 109.4 . . ?
C20 C19 H19B 109.4 . . ?
C18 C19 H19B 109.4 . . ?
H19A C19 H19B 108.0 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C15 C16 C17 118.7(18) . . ?
C15 C16 H16A 107.6 . . ?
C17 C16 H16A 107.6 . . ?
C15 C16 H16B 107.6 . . ?
C17 C16 H16B 107.6 . . ?
H16A C16 H16B 107.1 . . ?
C5 C4 N3 108.7(15) . . ?
C5 C4 H4 125.7 . . ?
N3 C4 H4 125.7 . . ?
C8 C7 C6 110.2(11) . . ?
C8 C7 H7A 109.6 . . ?
C6 C7 H7A 109.6 . . ?
C8 C7 H7B 109.6 . . ?
C6 C7 H7B 109.6 . . ?
H7A C7 H7B 108.1 . . ?
C7 C8 C9 107.1(11) . . ?
C7 C8 H8A 110.3 . . ?
C9 C8 H8A 110.3 . . ?
C7 C8 H8B 110.3 . . ?
C9 C8 H8B 110.3 . . ?
H8A C8 H8B 108.5 . . ?
N1 C6 C7 101.6(9) . . ?
N1 C6 H6A 111.5 . . ?
C7 C6 H6A 111.5 . . ?
N1 C6 H6B 111.5 . . ?
C7 C6 H6B 111.5 . . ?
H6A C6 H6B 109.3 . . ?

_diffrn_measured_fraction_theta_max 0.950
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.950
_refine_diff_density_max         0.519
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.074

#=END

data_C18MImTaF6-55oC
#TrackingRef '- SI-55oC.cif'

_database_code_depnum_ccdc_archive 'CCDC 843146'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            C18MImTaF6
_chemical_melting_point          347.0
_chemical_formula_moiety         
;
(C22 N2 H43 +), (Ta F6 -)
;
_chemical_formula_sum            'C22 H43 F6 N2 Ta'
_chemical_formula_weight         630.53

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/a

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x-1/2, -y-1/2, z'

_cell_length_a                   9.9490(10)
_cell_length_b                   9.7952(10)
_cell_length_c                   29.289(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.810(2)
_cell_angle_gamma                90.00
_cell_volume                     2850.9(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    328
_cell_measurement_reflns_used    8156
_cell_measurement_theta_min      6.05
_cell_measurement_theta_max      54.96

_exptl_crystal_description       platelet
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1264
_exptl_absorpt_coefficient_mu    3.905
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2479
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'RAPID AUTO 2.40 (Rigaku 2006)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      328
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS RapidII'
_diffrn_measurement_method       'imaging plate'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22069
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         3.03
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5006
_reflns_number_gt                1685
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Rigaku R-AXIS Rapid-II'
_computing_cell_refinement       'RAPID AUTO 2.40 (Rigaku 2006)'
_computing_data_reduction        'RAPID AUTO 2.40 (Rigaku 2006)'
_computing_structure_solution    'SIR92 (Altmare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
This structure was solved based on the data at 55 deg C and the octadecyl chain
in this structure has a large conformational flexibility, which results in large
thermal motions of the atoms. Hence, the following restraints were applied.
The N-C and C-C bond lengths in the octadecyl chain were restrained using
the DFIX (1,2 C-C distance: 1.54 A) and DANG (1,3 C-C distance: 2.52 A)
commands in SHELXL. Atomic displacement factors of the disordered part and
some carbon atoms in the octadecyl chain were restrained using DELU and SIMU
in SHELXL.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0846P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5006
_refine_ls_number_parameters     282
_refine_ls_number_restraints     84
_refine_ls_R_factor_all          0.1414
_refine_ls_R_factor_gt           0.0495
_refine_ls_wR_factor_ref         0.1673
_refine_ls_wR_factor_gt          0.1190
_refine_ls_goodness_of_fit_ref   0.880
_refine_ls_restrained_S_all      0.903
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ta1 Ta -0.16553(5) 0.03407(6) 0.107771(18) 0.1704(4) Uani 1 1 d . . .
F4 F -0.2671(15) -0.0407(13) 0.1504(4) 0.337(6) Uani 1 1 d . . .
F3 F -0.3009(9) 0.1472(10) 0.0982(5) 0.366(7) Uani 1 1 d . . .
F2 F -0.0852(15) 0.0998(18) 0.0604(4) 0.394(8) Uani 1 1 d . . .
F5 F -0.0341(9) -0.0924(11) 0.1196(4) 0.295(5) Uani 1 1 d . . .
N1 N 0.3657(16) -0.0280(16) 0.1107(5) 0.176(4) Uani 1 1 d D . .
F6 F -0.0736(11) 0.1481(10) 0.1454(4) 0.326(5) Uani 1 1 d . . .
F1 F -0.2542(8) -0.0902(10) 0.0683(4) 0.272(4) Uani 1 1 d . . .
C21 C -0.629(2) -0.156(3) 0.6740(7) 0.348(10) Uani 1 1 d DU . .
H21A H -0.6295 -0.2548 0.6733 0.418 Uiso 1 1 calc R . .
H21B H -0.7104 -0.1229 0.6583 0.418 Uiso 1 1 calc R . .
C9 C 0.1466(18) -0.143(2) 0.2475(6) 0.313(9) Uani 1 1 d DU . .
H9A H 0.0618 -0.1247 0.2309 0.376 Uiso 1 1 calc R . .
H9B H 0.1677 -0.2397 0.2447 0.376 Uiso 1 1 calc R . .
C18 C -0.376(2) -0.098(2) 0.5790(11) 0.298(12) Uani 1 1 d D . .
H18A H -0.3915 -0.0008 0.5763 0.358 Uiso 1 1 calc R . .
H18B H -0.2944 -0.1107 0.5981 0.358 Uiso 1 1 calc R . .
C17 C -0.351(3) -0.153(2) 0.5323(9) 0.293(10) Uani 1 1 d D . .
H17A H -0.4327 -0.1396 0.5135 0.352 Uiso 1 1 calc R . .
H17B H -0.3373 -0.2505 0.5353 0.352 Uiso 1 1 calc R . .
C13 C -0.0928(17) -0.158(2) 0.3906(6) 0.277(8) Uani 1 1 d DU . .
H13A H -0.0877 -0.2570 0.3924 0.332 Uiso 1 1 calc R . .
H13B H -0.1742 -0.1344 0.3728 0.332 Uiso 1 1 calc R . .
N3 N 0.4073(15) -0.1274(13) 0.0490(7) 0.175(4) Uani 1 1 d D . .
C22 C -0.622(2) -0.107(3) 0.7226(8) 0.392(11) Uani 1 1 d DU . .
H22A H -0.6102 -0.0085 0.7240 0.470 Uiso 1 1 calc R . .
H22B H -0.5485 -0.1501 0.7401 0.470 Uiso 1 1 calc R . .
C12 C 0.0266(19) -0.105(2) 0.3671(7) 0.293(8) Uani 1 1 d DU . .
H12A H 0.1086 -0.1340 0.3837 0.351 Uiso 1 1 calc R . .
H12B H 0.0247 -0.0061 0.3668 0.351 Uiso 1 1 calc R . .
C10 C 0.1417(17) -0.101(2) 0.2974(6) 0.314(9) Uani 1 1 d DU . .
H10A H 0.2232 -0.1314 0.3139 0.377 Uiso 1 1 calc R . .
H10B H 0.1385 -0.0022 0.2993 0.377 Uiso 1 1 calc R . .
C15 C -0.219(2) -0.162(2) 0.4597(8) 0.303(10) Uani 1 1 d D . .
H15A H -0.2068 -0.2597 0.4632 0.364 Uiso 1 1 calc R . .
H15B H -0.2999 -0.1468 0.4403 0.364 Uiso 1 1 calc R . .
C24 C 0.4669(14) -0.2154(15) 0.0125(5) 0.229(6) Uani 1 1 d . . .
H24A H 0.4596 -0.1686 -0.0163 0.343 Uiso 1 1 calc R . .
H24B H 0.4189 -0.3003 0.0102 0.343 Uiso 1 1 calc R . .
H24C H 0.5600 -0.2329 0.0206 0.343 Uiso 1 1 calc R . .
C5 C 0.2730(19) 0.0125(18) 0.0809(11) 0.218(8) Uani 1 1 d . . .
H5 H 0.2028 0.0728 0.0856 0.262 Uiso 1 1 calc R . .
C20 C -0.509(2) -0.103(3) 0.6511(8) 0.314(9) Uani 1 1 d DU . .
H20A H -0.4292 -0.1247 0.6701 0.377 Uiso 1 1 calc R . .
H20B H -0.5157 -0.0046 0.6492 0.377 Uiso 1 1 calc R . .
C14 C -0.099(2) -0.100(2) 0.4379(7) 0.279(7) Uani 1 1 d DU . .
H14A H -0.1085 -0.0019 0.4365 0.334 Uiso 1 1 calc R . .
H14B H -0.0178 -0.1222 0.4559 0.334 Uiso 1 1 calc R . .
C11 C 0.0256(15) -0.1578(19) 0.3190(6) 0.272(7) Uani 1 1 d DU . .
H11A H 0.0303 -0.2568 0.3190 0.326 Uiso 1 1 calc R . .
H11B H -0.0566 -0.1304 0.3023 0.326 Uiso 1 1 calc R . .
C2 C 0.4444(16) -0.1147(18) 0.0922(9) 0.176(5) Uani 1 1 d . . .
H2 H 0.5157 -0.1605 0.1072 0.211 Uiso 1 1 calc R . .
C19 C -0.491(3) -0.159(2) 0.6038(8) 0.299(11) Uani 1 1 d D . .
H19A H -0.4774 -0.2569 0.6061 0.359 Uiso 1 1 calc R . .
H19B H -0.5736 -0.1440 0.5855 0.359 Uiso 1 1 calc R . .
C23 C -0.756(3) -0.148(3) 0.7402(8) 0.468(17) Uani 1 1 d DU . .
H23A H -0.8220 -0.1515 0.7153 0.701 Uiso 1 1 calc R . .
H23B H -0.7829 -0.0824 0.7623 0.701 Uiso 1 1 calc R . .
H23C H -0.7479 -0.2364 0.7543 0.701 Uiso 1 1 calc R . .
C16 C -0.235(2) -0.097(2) 0.5057(9) 0.272(9) Uani 1 1 d D . .
H16A H -0.2489 0.0003 0.5014 0.326 Uiso 1 1 calc R . .
H16B H -0.1524 -0.1092 0.5240 0.326 Uiso 1 1 calc R . .
C4 C 0.301(2) -0.052(2) 0.0417(8) 0.217(8) Uani 1 1 d D . .
H4 H 0.2520 -0.0442 0.0139 0.260 Uiso 1 1 calc R . .
C7 C 0.2799(18) -0.0943(19) 0.1824(5) 0.309(8) Uani 1 1 d DU . .
H7A H 0.1949 -0.0894 0.1648 0.371 Uiso 1 1 calc R . .
H7B H 0.3121 -0.1877 0.1815 0.371 Uiso 1 1 calc R . .
C8 C 0.260(2) -0.054(2) 0.2303(5) 0.321(9) Uani 1 1 d DU . .
H8A H 0.2356 0.0419 0.2318 0.385 Uiso 1 1 calc R . .
H8B H 0.3422 -0.0679 0.2489 0.385 Uiso 1 1 calc R . .
C6 C 0.3846(16) 0.0034(16) 0.1612(6) 0.238(7) Uani 1 1 d D . .
H6A H 0.3647 0.0983 0.1675 0.285 Uiso 1 1 calc R . .
H6B H 0.4755 -0.0171 0.1726 0.285 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ta1 0.1642(5) 0.1554(5) 0.1931(6) 0.0028(4) 0.0225(4) -0.0009(4)
F4 0.363(14) 0.381(16) 0.270(11) 0.045(9) 0.046(10) -0.076(11)
F3 0.262(8) 0.226(9) 0.60(2) -0.006(11) -0.029(10) 0.095(7)
F2 0.431(16) 0.503(19) 0.253(10) 0.088(12) 0.065(10) -0.194(16)
F5 0.222(7) 0.246(8) 0.412(14) -0.040(10) -0.045(8) 0.045(7)
N1 0.183(11) 0.149(9) 0.198(13) 0.016(9) 0.033(11) -0.005(8)
F6 0.351(11) 0.231(9) 0.391(13) -0.075(9) -0.050(10) -0.047(9)
F1 0.198(6) 0.279(8) 0.337(10) -0.103(8) 0.002(6) -0.020(6)
C21 0.38(2) 0.30(2) 0.355(19) -0.058(18) -0.080(16) -0.105(18)
C9 0.304(19) 0.26(2) 0.37(2) 0.074(19) 0.006(17) -0.052(14)
C18 0.29(2) 0.214(19) 0.37(3) -0.09(2) -0.11(2) -0.002(17)
C17 0.36(3) 0.204(18) 0.30(3) -0.013(18) -0.10(2) -0.054(18)
C13 0.287(15) 0.219(15) 0.31(2) 0.008(12) -0.077(16) -0.077(12)
N3 0.143(8) 0.149(10) 0.233(15) 0.045(11) 0.009(11) -0.028(7)
C22 0.44(3) 0.35(2) 0.39(2) -0.11(2) -0.056(19) -0.14(2)
C12 0.292(19) 0.231(16) 0.35(2) -0.013(17) -0.055(15) -0.072(14)
C10 0.215(14) 0.31(2) 0.41(3) 0.06(2) -0.048(16) -0.072(14)
C15 0.39(3) 0.213(18) 0.30(2) -0.022(17) -0.05(2) -0.095(18)
C24 0.265(14) 0.188(12) 0.240(14) -0.027(11) 0.079(12) -0.024(11)
C5 0.179(12) 0.183(15) 0.29(2) 0.077(16) -0.017(17) 0.032(10)
C20 0.32(2) 0.247(19) 0.37(2) -0.080(19) -0.098(16) -0.047(17)
C14 0.307(18) 0.202(15) 0.319(19) 0.006(14) -0.065(15) -0.053(15)
C11 0.207(13) 0.235(17) 0.37(2) 0.017(16) -0.023(14) -0.054(12)
C2 0.163(12) 0.162(13) 0.200(16) 0.023(12) -0.029(11) -0.020(10)
C19 0.35(3) 0.218(19) 0.32(3) -0.032(17) -0.10(2) -0.061(19)
C23 0.56(4) 0.47(4) 0.37(3) -0.07(3) 0.01(2) -0.22(4)
C16 0.252(18) 0.213(18) 0.34(3) -0.02(2) -0.042(19) 0.002(15)
C4 0.23(2) 0.22(2) 0.198(17) 0.026(14) -0.020(16) -0.063(18)
C7 0.277(16) 0.36(2) 0.293(19) -0.057(19) 0.004(15) 0.015(17)
C8 0.304(18) 0.36(2) 0.302(19) -0.003(17) 0.021(17) -0.083(14)
C6 0.215(15) 0.259(17) 0.24(2) -0.006(14) 0.043(14) -0.037(11)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ta1 F3 1.756(8) . ?
Ta1 F2 1.756(9) . ?
Ta1 F6 1.789(9) . ?
Ta1 F4 1.801(12) . ?
Ta1 F5 1.822(9) . ?
Ta1 F1 1.871(8) . ?
N1 C2 1.292(17) . ?
N1 C5 1.30(2) . ?
N1 C6 1.514(12) . ?
C21 C20 1.486(13) . ?
C21 C22 1.500(14) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C9 C10 1.523(13) . ?
C9 C8 1.535(13) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C18 C17 1.502(13) . ?
C18 C19 1.507(13) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C17 C16 1.518(13) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C13 C12 1.495(13) . ?
C13 C14 1.502(12) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
N3 C4 1.298(10) . ?
N3 C2 1.307(15) . ?
N3 C24 1.515(17) . ?
C22 C23 1.507(10) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C12 C11 1.502(12) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C10 C11 1.453(12) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C15 C14 1.506(13) . ?
C15 C16 1.506(13) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C5 C4 1.35(2) . ?
C5 H5 0.9300 . ?
C20 C19 1.508(13) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C2 H2 0.9300 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C4 H4 0.9300 . ?
C7 C8 1.479(9) . ?
C7 C6 1.566(9) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F3 Ta1 F2 91.0(7) . . ?
F3 Ta1 F6 94.0(6) . . ?
F2 Ta1 F6 91.1(6) . . ?
F3 Ta1 F4 85.1(6) . . ?
F2 Ta1 F4 171.7(5) . . ?
F6 Ta1 F4 96.5(6) . . ?
F3 Ta1 F5 175.6(5) . . ?
F2 Ta1 F5 92.8(7) . . ?
F6 Ta1 F5 88.1(5) . . ?
F4 Ta1 F5 90.8(6) . . ?
F3 Ta1 F1 88.7(5) . . ?
F2 Ta1 F1 88.2(6) . . ?
F6 Ta1 F1 177.3(4) . . ?
F4 Ta1 F1 84.3(5) . . ?
F5 Ta1 F1 89.2(5) . . ?
C2 N1 C5 110.2(17) . . ?
C2 N1 C6 120(2) . . ?
C5 N1 C6 130(2) . . ?
C20 C21 C22 108.6(18) . . ?
C20 C21 H21A 110.0 . . ?
C22 C21 H21A 110.0 . . ?
C20 C21 H21B 110.0 . . ?
C22 C21 H21B 110.0 . . ?
H21A C21 H21B 108.4 . . ?
C10 C9 C8 102.6(12) . . ?
C10 C9 H9A 111.3 . . ?
C8 C9 H9A 111.3 . . ?
C10 C9 H9B 111.3 . . ?
C8 C9 H9B 111.3 . . ?
H9A C9 H9B 109.2 . . ?
C17 C18 C19 118(2) . . ?
C17 C18 H18A 107.9 . . ?
C19 C18 H18A 107.9 . . ?
C17 C18 H18B 107.9 . . ?
C19 C18 H18B 107.9 . . ?
H18A C18 H18B 107.2 . . ?
C18 C17 C16 120(2) . . ?
C18 C17 H17A 107.3 . . ?
C16 C17 H17A 107.3 . . ?
C18 C17 H17B 107.3 . . ?
C16 C17 H17B 107.3 . . ?
H17A C17 H17B 106.9 . . ?
C12 C13 C14 111.5(18) . . ?
C12 C13 H13A 109.3 . . ?
C14 C13 H13A 109.3 . . ?
C12 C13 H13B 109.3 . . ?
C14 C13 H13B 109.3 . . ?
H13A C13 H13B 108.0 . . ?
C4 N3 C2 107.2(19) . . ?
C4 N3 C24 123(2) . . ?
C2 N3 C24 129(2) . . ?
C21 C22 C23 103.9(18) . . ?
C21 C22 H22A 111.0 . . ?
C23 C22 H22A 111.0 . . ?
C21 C22 H22B 111.0 . . ?
C23 C22 H22B 111.0 . . ?
H22A C22 H22B 109.0 . . ?
C13 C12 C11 110.1(15) . . ?
C13 C12 H12A 109.6 . . ?
C11 C12 H12A 109.6 . . ?
C13 C12 H12B 109.6 . . ?
C11 C12 H12B 109.6 . . ?
H12A C12 H12B 108.2 . . ?
C11 C10 C9 112.1(13) . . ?
C11 C10 H10A 109.2 . . ?
C9 C10 H10A 109.2 . . ?
C11 C10 H10B 109.2 . . ?
C9 C10 H10B 109.2 . . ?
H10A C10 H10B 107.9 . . ?
C14 C15 C16 109.3(18) . . ?
C14 C15 H15A 109.8 . . ?
C16 C15 H15A 109.8 . . ?
C14 C15 H15B 109.8 . . ?
C16 C15 H15B 109.8 . . ?
H15A C15 H15B 108.3 . . ?
N3 C24 H24A 109.5 . . ?
N3 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N3 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N1 C5 C4 104.9(17) . . ?
N1 C5 H5 127.6 . . ?
C4 C5 H5 127.6 . . ?
C21 C20 C19 115(2) . . ?
C21 C20 H20A 108.5 . . ?
C19 C20 H20A 108.5 . . ?
C21 C20 H20B 108.5 . . ?
C19 C20 H20B 108.5 . . ?
H20A C20 H20B 107.5 . . ?
C13 C14 C15 108.1(18) . . ?
C13 C14 H14A 110.1 . . ?
C15 C14 H14A 110.1 . . ?
C13 C14 H14B 110.1 . . ?
C15 C14 H14B 110.1 . . ?
H14A C14 H14B 108.4 . . ?
C10 C11 C12 107.9(14) . . ?
C10 C11 H11A 110.1 . . ?
C12 C11 H11A 110.1 . . ?
C10 C11 H11B 110.1 . . ?
C12 C11 H11B 110.1 . . ?
H11A C11 H11B 108.4 . . ?
N1 C2 N3 108.7(15) . . ?
N1 C2 H2 125.7 . . ?
N3 C2 H2 125.7 . . ?
C18 C19 C20 115(2) . . ?
C18 C19 H19A 108.4 . . ?
C20 C19 H19A 108.4 . . ?
C18 C19 H19B 108.4 . . ?
C20 C19 H19B 108.4 . . ?
H19A C19 H19B 107.5 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C15 C16 C17 115(2) . . ?
C15 C16 H16A 108.5 . . ?
C17 C16 H16A 108.5 . . ?
C15 C16 H16B 108.5 . . ?
C17 C16 H16B 108.5 . . ?
H16A C16 H16B 107.5 . . ?
N3 C4 C5 109.0(19) . . ?
N3 C4 H4 125.5 . . ?
C5 C4 H4 125.5 . . ?
C8 C7 C6 109.5(11) . . ?
C8 C7 H7A 109.8 . . ?
C6 C7 H7A 109.8 . . ?
C8 C7 H7B 109.8 . . ?
C6 C7 H7B 109.8 . . ?
H7A C7 H7B 108.2 . . ?
C7 C8 C9 107.0(12) . . ?
C7 C8 H8A 110.3 . . ?
C9 C8 H8A 110.3 . . ?
C7 C8 H8B 110.3 . . ?
C9 C8 H8B 110.3 . . ?
H8A C8 H8B 108.6 . . ?
N1 C6 C7 102.2(10) . . ?
N1 C6 H6A 111.3 . . ?
C7 C6 H6A 111.3 . . ?
N1 C6 H6B 111.3 . . ?
C7 C6 H6B 111.3 . . ?
H6A C6 H6B 109.2 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.072

#=END


#============================================================

data_C18MImPF6--100oC
#TrackingRef '- SI--100oC.cif'

_database_code_depnum_ccdc_archive 'CCDC 843147'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            C18MImPF6
_chemical_melting_point          352.9
_chemical_formula_moiety         
;
(C22 N2 H43 +), (P F6 -)
;
_chemical_formula_sum            'C22 H43 F6 N2 P'
_chemical_formula_weight         480.55

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/a

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x-1/2, -y-1/2, z'

_cell_length_a                   9.1715(7)
_cell_length_b                   9.8807(8)
_cell_length_c                   28.520(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.707(2)
_cell_angle_gamma                90.00
_cell_volume                     2571.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173
_cell_measurement_reflns_used    11398
_cell_measurement_theta_min      6.08
_cell_measurement_theta_max      54.98

_exptl_crystal_description       platelet
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1032
_exptl_absorpt_coefficient_mu    0.161
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6296
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'RAPID AUTO 2.40 (Rigaku 2006)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS RapidII'
_diffrn_measurement_method       'imaging plate'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22634
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_sigmaI/netI    0.0511
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         3.04
_diffrn_reflns_theta_max         27.48
_reflns_number_total             5864
_reflns_number_gt                3373
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Rigaku R-AXIS Rapid-II'
_computing_cell_refinement       'RAPID AUTO 2.40 (Rigaku 2006)'
_computing_data_reduction        'RAPID AUTO 2.40 (Rigaku 2006)'
_computing_structure_solution    'SIR92 (Altmare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0519P)^2^+0.9719P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5864
_refine_ls_number_parameters     282
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1000
_refine_ls_R_factor_gt           0.0465
_refine_ls_wR_factor_ref         0.1532
_refine_ls_wR_factor_gt          0.1059
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_restrained_S_all      1.117
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P -0.14396(7) 0.01931(7) 0.10347(2) 0.03969(19) Uani 1 1 d . . .
F4 F -0.21504(18) -0.04596(18) 0.14665(5) 0.0548(4) Uani 1 1 d . . .
F3 F -0.27856(19) 0.12091(19) 0.09605(8) 0.0758(6) Uani 1 1 d . . .
F2 F -0.0751(2) 0.0821(2) 0.05916(7) 0.0803(7) Uani 1 1 d . . .
F5 F -0.01153(17) -0.08469(16) 0.11068(6) 0.0542(4) Uani 1 1 d . . .
N1 N 0.3932(2) -0.0033(2) 0.11362(7) 0.0338(5) Uani 1 1 d . . .
F6 F -0.0544(2) 0.12276(18) 0.13735(7) 0.0692(5) Uani 1 1 d . . .
F1 F -0.23375(18) -0.0867(2) 0.06906(6) 0.0606(5) Uani 1 1 d . . .
C21 C -0.6528(3) -0.1495(3) 0.67100(8) 0.0371(6) Uani 1 1 d . . .
H21A H -0.7434 -0.1365 0.6509 0.044 Uiso 1 1 calc R . .
H21B H -0.6383 -0.2461 0.6753 0.044 Uiso 1 1 calc R . .
C9 C 0.1511(3) -0.1701(3) 0.22743(8) 0.0388(6) Uani 1 1 d . . .
H9A H 0.1443 -0.2678 0.2298 0.047 Uiso 1 1 calc R . .
H9B H 0.0624 -0.1385 0.2094 0.047 Uiso 1 1 calc R . .
C18 C -0.3868(3) -0.0961(3) 0.57350(8) 0.0365(5) Uani 1 1 d . . .
H18A H -0.2958 -0.1107 0.5933 0.044 Uiso 1 1 calc R . .
H18B H -0.4010 0.0009 0.5702 0.044 Uiso 1 1 calc R . .
C17 C -0.3725(3) -0.1566(3) 0.52490(8) 0.0349(5) Uani 1 1 d . . .
H17A H -0.3583 -0.2536 0.5282 0.042 Uiso 1 1 calc R . .
H17B H -0.4634 -0.1419 0.5051 0.042 Uiso 1 1 calc R . .
C6 C 0.4261(3) 0.0456(3) 0.16249(8) 0.0393(6) Uani 1 1 d . . .
H6A H 0.4421 0.1426 0.1622 0.047 Uiso 1 1 calc R . .
H6B H 0.5155 0.0032 0.1764 0.047 Uiso 1 1 calc R . .
C13 C -0.0953(3) -0.1594(3) 0.37862(8) 0.0354(5) Uani 1 1 d . . .
H13A H -0.0817 -0.2564 0.3820 0.043 Uiso 1 1 calc R . .
H13B H -0.1870 -0.1445 0.3593 0.043 Uiso 1 1 calc R . .
N3 N 0.4035(2) -0.1170(2) 0.04942(7) 0.0396(5) Uani 1 1 d . . .
C22 C -0.6680(3) -0.0852(3) 0.71850(9) 0.0508(7) Uani 1 1 d . . .
H22A H -0.6811 0.0116 0.7143 0.061 Uiso 1 1 calc R . .
H22B H -0.5780 -0.0995 0.7388 0.061 Uiso 1 1 calc R . .
C12 C 0.0288(3) -0.1023(3) 0.35303(8) 0.0359(5) Uani 1 1 d . . .
H12A H 0.1212 -0.1197 0.3717 0.043 Uiso 1 1 calc R . .
H12B H 0.0171 -0.0050 0.3502 0.043 Uiso 1 1 calc R . .
C10 C 0.1576(3) -0.1102(3) 0.27703(8) 0.0362(5) Uani 1 1 d . . .
H10A H 0.2511 -0.1326 0.2942 0.043 Uiso 1 1 calc R . .
H10B H 0.1510 -0.0124 0.2748 0.043 Uiso 1 1 calc R . .
C15 C -0.2328(3) -0.1576(2) 0.45193(8) 0.0339(5) Uani 1 1 d . . .
H15A H -0.2186 -0.2545 0.4551 0.041 Uiso 1 1 calc R . .
H15B H -0.3239 -0.1428 0.4323 0.041 Uiso 1 1 calc R . .
C8 C 0.2816(3) -0.1355(2) 0.20026(9) 0.0392(6) Uani 1 1 d . . .
H8A H 0.3700 -0.1710 0.2174 0.047 Uiso 1 1 calc R . .
H8B H 0.2692 -0.1807 0.1699 0.047 Uiso 1 1 calc R . .
C24 C 0.4537(4) -0.2122(3) 0.01482(10) 0.0543(8) Uani 1 1 d . . .
H24A H 0.3704 -0.2528 -0.0028 0.081 Uiso 1 1 calc R . .
H24B H 0.5125 -0.2815 0.0309 0.081 Uiso 1 1 calc R . .
H24C H 0.5110 -0.1646 -0.0062 0.081 Uiso 1 1 calc R . .
C5 C 0.2868(3) 0.0466(3) 0.08107(9) 0.0466(7) Uani 1 1 d . . .
H5 H 0.2220 0.1165 0.0858 0.056 Uiso 1 1 calc R . .
C20 C -0.5269(3) -0.0926(3) 0.64613(8) 0.0388(6) Uani 1 1 d . . .
H20A H -0.4361 -0.1069 0.6660 0.047 Uiso 1 1 calc R . .
H20B H -0.5405 0.0042 0.6423 0.047 Uiso 1 1 calc R . .
C14 C -0.1077(3) -0.0987(3) 0.42726(8) 0.0348(5) Uani 1 1 d . . .
H14A H -0.0164 -0.1138 0.4468 0.042 Uiso 1 1 calc R . .
H14B H -0.1216 -0.0017 0.4240 0.042 Uiso 1 1 calc R . .
C11 C 0.0343(3) -0.1630(3) 0.30404(8) 0.0358(5) Uani 1 1 d . . .
H11A H 0.0444 -0.2604 0.3072 0.043 Uiso 1 1 calc R . .
H11B H -0.0583 -0.1451 0.2856 0.043 Uiso 1 1 calc R . .
C2 C 0.4617(3) -0.1026(3) 0.09352(9) 0.0374(6) Uani 1 1 d . . .
H2 H 0.5384 -0.1538 0.1081 0.045 Uiso 1 1 calc R . .
C7 C 0.3022(3) 0.0139(2) 0.19221(9) 0.0357(5) Uani 1 1 d . . .
H7A H 0.3215 0.0585 0.2225 0.043 Uiso 1 1 calc R . .
H7B H 0.2118 0.0508 0.1768 0.043 Uiso 1 1 calc R . .
C19 C -0.5123(3) -0.1551(3) 0.59801(8) 0.0356(5) Uani 1 1 d . . .
H19A H -0.4975 -0.2518 0.6018 0.043 Uiso 1 1 calc R . .
H19B H -0.6032 -0.1415 0.5781 0.043 Uiso 1 1 calc R . .
C23 C -0.7956(4) -0.1411(3) 0.74277(11) 0.0621(9) Uani 1 1 d . . .
H23A H -0.8857 -0.1237 0.7236 0.093 Uiso 1 1 calc R . .
H23B H -0.7982 -0.0979 0.7728 0.093 Uiso 1 1 calc R . .
H23C H -0.7834 -0.2369 0.7472 0.093 Uiso 1 1 calc R . .
C16 C -0.2468(3) -0.0975(3) 0.50052(8) 0.0345(5) Uani 1 1 d . . .
H16A H -0.1559 -0.1125 0.5203 0.041 Uiso 1 1 calc R . .
H16B H -0.2608 -0.0005 0.4974 0.041 Uiso 1 1 calc R . .
C4 C 0.2930(3) -0.0237(3) 0.04117(9) 0.0487(7) Uani 1 1 d . . .
H4 H 0.2335 -0.0115 0.0131 0.058 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1 0.0409(4) 0.0395(4) 0.0388(4) 0.0044(3) 0.0049(3) 0.0007(3)
F4 0.0614(10) 0.0653(11) 0.0398(9) 0.0043(8) 0.0156(8) -0.0037(9)
F3 0.0522(11) 0.0548(11) 0.1192(17) 0.0221(11) 0.0033(11) 0.0156(9)
F2 0.0562(11) 0.1209(18) 0.0638(12) 0.0452(12) 0.0061(9) -0.0203(12)
F5 0.0480(9) 0.0488(9) 0.0658(11) -0.0037(8) 0.0050(8) 0.0108(8)
N1 0.0358(10) 0.0347(11) 0.0323(10) 0.0033(8) 0.0101(9) -0.0022(9)
F6 0.0656(12) 0.0485(10) 0.0912(14) -0.0227(10) -0.0034(10) -0.0072(9)
F1 0.0492(9) 0.0857(13) 0.0472(10) -0.0198(9) 0.0069(8) -0.0141(9)
C21 0.0465(14) 0.0352(13) 0.0301(12) 0.0005(10) 0.0068(11) -0.0004(11)
C9 0.0488(14) 0.0365(13) 0.0330(13) -0.0015(11) 0.0137(11) -0.0063(12)
C18 0.0417(13) 0.0387(13) 0.0301(12) -0.0021(10) 0.0093(11) -0.0035(11)
C17 0.0408(13) 0.0361(12) 0.0286(12) -0.0013(10) 0.0071(10) -0.0018(11)
C6 0.0441(14) 0.0403(14) 0.0346(13) -0.0040(11) 0.0096(11) -0.0083(12)
C13 0.0410(13) 0.0357(12) 0.0305(12) 0.0004(10) 0.0087(10) -0.0006(11)
N3 0.0496(13) 0.0387(11) 0.0317(11) -0.0015(9) 0.0095(10) -0.0093(10)
C22 0.0516(16) 0.069(2) 0.0329(14) -0.0071(13) 0.0114(13) -0.0049(15)
C12 0.0393(13) 0.0400(13) 0.0292(12) 0.0027(10) 0.0074(10) -0.0026(11)
C10 0.0378(13) 0.0382(13) 0.0340(13) 0.0019(11) 0.0104(11) -0.0020(11)
C15 0.0388(13) 0.0353(12) 0.0284(12) -0.0004(10) 0.0064(10) -0.0035(11)
C8 0.0465(14) 0.0367(13) 0.0365(13) 0.0010(11) 0.0152(12) 0.0006(12)
C24 0.076(2) 0.0473(16) 0.0419(16) -0.0114(13) 0.0194(15) -0.0155(15)
C5 0.0500(15) 0.0496(16) 0.0407(15) 0.0111(13) 0.0067(12) 0.0092(14)
C20 0.0429(14) 0.0442(14) 0.0302(13) -0.0048(11) 0.0089(11) -0.0031(12)
C14 0.0395(13) 0.0363(13) 0.0294(12) 0.0012(10) 0.0067(10) -0.0018(11)
C11 0.0406(13) 0.0358(13) 0.0325(13) 0.0015(10) 0.0113(11) -0.0004(11)
C2 0.0383(13) 0.0381(13) 0.0370(13) 0.0002(11) 0.0094(11) -0.0014(11)
C7 0.0392(13) 0.0341(12) 0.0348(12) -0.0021(10) 0.0095(11) -0.0021(11)
C19 0.0411(13) 0.0360(13) 0.0302(12) -0.0018(10) 0.0065(10) -0.0001(11)
C23 0.089(2) 0.0561(19) 0.0462(17) 0.0032(14) 0.0326(17) -0.0004(18)
C16 0.0396(13) 0.0357(12) 0.0291(11) -0.0007(10) 0.0075(10) -0.0026(11)
C4 0.0532(16) 0.0572(17) 0.0349(14) 0.0105(13) 0.0005(12) 0.0016(14)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 F6 1.5798(18) . ?
P1 F4 1.5866(16) . ?
P1 F3 1.5890(18) . ?
P1 F5 1.5886(16) . ?
P1 F2 1.5935(18) . ?
P1 F1 1.6055(18) . ?
N1 C2 1.326(3) . ?
N1 C5 1.370(3) . ?
N1 C6 1.478(3) . ?
C21 C22 1.515(3) . ?
C21 C20 1.521(3) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C9 C8 1.528(3) . ?
C9 C10 1.529(3) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C18 C19 1.522(3) . ?
C18 C17 1.527(3) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C17 C16 1.521(3) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C6 C7 1.517(3) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C13 C12 1.521(3) . ?
C13 C14 1.526(3) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
N3 C2 1.324(3) . ?
N3 C4 1.374(3) . ?
N3 C24 1.470(3) . ?
C22 C23 1.521(4) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C12 C11 1.526(3) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C10 C11 1.523(3) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C15 C14 1.520(3) . ?
C15 C16 1.525(3) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C8 C7 1.508(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C5 C4 1.339(4) . ?
C5 H5 0.9300 . ?
C20 C19 1.523(3) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C2 H2 0.9300 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C4 H4 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F6 P1 F4 90.98(10) . . ?
F6 P1 F3 91.30(11) . . ?
F4 P1 F3 89.22(10) . . ?
F6 P1 F5 89.71(10) . . ?
F4 P1 F5 90.26(9) . . ?
F3 P1 F5 178.88(11) . . ?
F6 P1 F2 90.58(12) . . ?
F4 P1 F2 178.44(12) . . ?
F3 P1 F2 90.73(11) . . ?
F5 P1 F2 89.77(10) . . ?
F6 P1 F1 179.49(11) . . ?
F4 P1 F1 89.07(10) . . ?
F3 P1 F1 89.22(11) . . ?
F5 P1 F1 89.78(10) . . ?
F2 P1 F1 89.36(11) . . ?
C2 N1 C5 108.0(2) . . ?
C2 N1 C6 126.0(2) . . ?
C5 N1 C6 125.9(2) . . ?
C22 C21 C20 113.8(2) . . ?
C22 C21 H21A 108.8 . . ?
C20 C21 H21A 108.8 . . ?
C22 C21 H21B 108.8 . . ?
C20 C21 H21B 108.8 . . ?
H21A C21 H21B 107.7 . . ?
C8 C9 C10 114.9(2) . . ?
C8 C9 H9A 108.5 . . ?
C10 C9 H9A 108.5 . . ?
C8 C9 H9B 108.5 . . ?
C10 C9 H9B 108.5 . . ?
H9A C9 H9B 107.5 . . ?
C19 C18 C17 113.8(2) . . ?
C19 C18 H18A 108.8 . . ?
C17 C18 H18A 108.8 . . ?
C19 C18 H18B 108.8 . . ?
C17 C18 H18B 108.8 . . ?
H18A C18 H18B 107.7 . . ?
C16 C17 C18 113.7(2) . . ?
C16 C17 H17A 108.8 . . ?
C18 C17 H17A 108.8 . . ?
C16 C17 H17B 108.8 . . ?
C18 C17 H17B 108.8 . . ?
H17A C17 H17B 107.7 . . ?
N1 C6 C7 111.4(2) . . ?
N1 C6 H6A 109.3 . . ?
C7 C6 H6A 109.3 . . ?
N1 C6 H6B 109.3 . . ?
C7 C6 H6B 109.3 . . ?
H6A C6 H6B 108.0 . . ?
C12 C13 C14 114.7(2) . . ?
C12 C13 H13A 108.6 . . ?
C14 C13 H13A 108.6 . . ?
C12 C13 H13B 108.6 . . ?
C14 C13 H13B 108.6 . . ?
H13A C13 H13B 107.6 . . ?
C2 N3 C4 108.1(2) . . ?
C2 N3 C24 125.7(2) . . ?
C4 N3 C24 126.1(2) . . ?
C21 C22 C23 113.5(2) . . ?
C21 C22 H22A 108.9 . . ?
C23 C22 H22A 108.9 . . ?
C21 C22 H22B 108.9 . . ?
C23 C22 H22B 108.9 . . ?
H22A C22 H22B 107.7 . . ?
C13 C12 C11 112.8(2) . . ?
C13 C12 H12A 109.0 . . ?
C11 C12 H12A 109.0 . . ?
C13 C12 H12B 109.0 . . ?
C11 C12 H12B 109.0 . . ?
H12A C12 H12B 107.8 . . ?
C11 C10 C9 111.9(2) . . ?
C11 C10 H10A 109.2 . . ?
C9 C10 H10A 109.2 . . ?
C11 C10 H10B 109.2 . . ?
C9 C10 H10B 109.2 . . ?
H10A C10 H10B 107.9 . . ?
C14 C15 C16 114.0(2) . . ?
C14 C15 H15A 108.7 . . ?
C16 C15 H15A 108.7 . . ?
C14 C15 H15B 108.7 . . ?
C16 C15 H15B 108.7 . . ?
H15A C15 H15B 107.6 . . ?
C7 C8 C9 114.4(2) . . ?
C7 C8 H8A 108.7 . . ?
C9 C8 H8A 108.7 . . ?
C7 C8 H8B 108.7 . . ?
C9 C8 H8B 108.7 . . ?
H8A C8 H8B 107.6 . . ?
N3 C24 H24A 109.5 . . ?
N3 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N3 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C4 C5 N1 107.6(2) . . ?
C4 C5 H5 126.2 . . ?
N1 C5 H5 126.2 . . ?
C21 C20 C19 114.1(2) . . ?
C21 C20 H20A 108.7 . . ?
C19 C20 H20A 108.7 . . ?
C21 C20 H20B 108.7 . . ?
C19 C20 H20B 108.7 . . ?
H20A C20 H20B 107.6 . . ?
C15 C14 C13 113.5(2) . . ?
C15 C14 H14A 108.9 . . ?
C13 C14 H14A 108.9 . . ?
C15 C14 H14B 108.9 . . ?
C13 C14 H14B 108.9 . . ?
H14A C14 H14B 107.7 . . ?
C10 C11 C12 114.9(2) . . ?
C10 C11 H11A 108.5 . . ?
C12 C11 H11A 108.5 . . ?
C10 C11 H11B 108.5 . . ?
C12 C11 H11B 108.5 . . ?
H11A C11 H11B 107.5 . . ?
N3 C2 N1 109.1(2) . . ?
N3 C2 H2 125.5 . . ?
N1 C2 H2 125.5 . . ?
C8 C7 C6 113.5(2) . . ?
C8 C7 H7A 108.9 . . ?
C6 C7 H7A 108.9 . . ?
C8 C7 H7B 108.9 . . ?
C6 C7 H7B 108.9 . . ?
H7A C7 H7B 107.7 . . ?
C18 C19 C20 113.4(2) . . ?
C18 C19 H19A 108.9 . . ?
C20 C19 H19A 108.9 . . ?
C18 C19 H19B 108.9 . . ?
C20 C19 H19B 108.9 . . ?
H19A C19 H19B 107.7 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C17 C16 C15 113.7(2) . . ?
C17 C16 H16A 108.8 . . ?
C15 C16 H16A 108.8 . . ?
C17 C16 H16B 108.8 . . ?
C15 C16 H16B 108.8 . . ?
H16A C16 H16B 107.7 . . ?
C5 C4 N3 107.2(2) . . ?
C5 C4 H4 126.4 . . ?
N3 C4 H4 126.4 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.072

#=END

data_C18MImAsF6--100oC
#TrackingRef '- SI--100oC.cif'

_database_code_depnum_ccdc_archive 'CCDC 843148'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            C18MImAsF6
_chemical_melting_point          351.1
_chemical_formula_moiety         
;
(C22 N2 H43 +), (As F6 -)
;
_chemical_formula_sum            'C22 H43 As F6 N2'
_chemical_formula_weight         524.50

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/a

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x-1/2, -y-1/2, z'

_cell_length_a                   9.1894(2)
_cell_length_b                   9.9779(3)
_cell_length_c                   28.5321(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.0148(7)
_cell_angle_gamma                90.00
_cell_volume                     2601.74(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    173
_cell_measurement_reflns_used    16988
_cell_measurement_theta_min      6.05
_cell_measurement_theta_max      54.94

_exptl_crystal_description       platelet
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1104
_exptl_absorpt_coefficient_mu    1.360
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7140
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'RAPID AUTO 2.40 (Rigaku 2006)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS RapidII'
_diffrn_measurement_method       'imaging plate'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24782
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_sigmaI/netI    0.0403
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         27.47
_reflns_number_total             5884
_reflns_number_gt                4153
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Rigaku R-AXIS Rapid-II'
_computing_cell_refinement       'RAPID AUTO 2.40 (Rigaku 2006)'
_computing_data_reduction        'RAPID AUTO 2.40 (Rigaku 2006)'
_computing_structure_solution    'SIR92 (Altmare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+1.1046P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5884
_refine_ls_number_parameters     282
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0418
_refine_ls_wR_factor_ref         0.1190
_refine_ls_wR_factor_gt          0.0981
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_restrained_S_all      1.126
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As -0.14483(3) 0.01897(3) 0.104696(11) 0.03872(11) Uani 1 1 d . . .
F4 F -0.2185(2) -0.0533(2) 0.15093(6) 0.0538(5) Uani 1 1 d . . .
F3 F -0.2902(2) 0.1271(2) 0.09796(9) 0.0696(6) Uani 1 1 d . . .
F2 F -0.0745(2) 0.0895(3) 0.05707(7) 0.0750(7) Uani 1 1 d . . .
F5 F -0.0020(2) -0.09151(18) 0.11097(7) 0.0542(5) Uani 1 1 d . . .
N1 N 0.3922(3) -0.0016(2) 0.11593(8) 0.0349(5) Uani 1 1 d . . .
F6 F -0.0470(2) 0.1284(2) 0.14138(8) 0.0640(6) Uani 1 1 d . . .
F1 F -0.2422(2) -0.0917(2) 0.06732(7) 0.0603(5) Uani 1 1 d . . .
C21 C -0.6566(3) -0.1487(3) 0.66964(10) 0.0395(7) Uani 1 1 d . . .
H21A H -0.7467 -0.1349 0.6493 0.047 Uiso 1 1 calc R . .
H21B H -0.6429 -0.2445 0.6737 0.047 Uiso 1 1 calc R . .
C9 C 0.1525(3) -0.1696(3) 0.22956(10) 0.0403(7) Uani 1 1 d . . .
H9A H 0.0640 -0.1377 0.2115 0.048 Uiso 1 1 calc R . .
H9B H 0.1451 -0.2664 0.2318 0.048 Uiso 1 1 calc R . .
C18 C -0.3884(3) -0.0960(3) 0.57353(10) 0.0379(6) Uani 1 1 d . . .
H18A H -0.2979 -0.1106 0.5936 0.046 Uiso 1 1 calc R . .
H18B H -0.4024 0.0000 0.5702 0.046 Uiso 1 1 calc R . .
C17 C -0.3734(3) -0.1560(3) 0.52522(10) 0.0368(6) Uani 1 1 d . . .
H17A H -0.4639 -0.1415 0.5051 0.044 Uiso 1 1 calc R . .
H17B H -0.3592 -0.2520 0.5286 0.044 Uiso 1 1 calc R . .
C6 C 0.4276(3) 0.0436(3) 0.16468(10) 0.0389(7) Uani 1 1 d . . .
H6A H 0.4455 0.1394 0.1649 0.047 Uiso 1 1 calc R . .
H6B H 0.5165 -0.0004 0.1781 0.047 Uiso 1 1 calc R . .
C13 C -0.0944(3) -0.1598(3) 0.38013(10) 0.0371(6) Uani 1 1 d . . .
H13A H -0.1859 -0.1450 0.3606 0.045 Uiso 1 1 calc R . .
H13B H -0.0810 -0.2558 0.3836 0.045 Uiso 1 1 calc R . .
N3 N 0.3972(3) -0.1117(2) 0.05097(8) 0.0393(6) Uani 1 1 d . . .
C22 C -0.6731(4) -0.0867(4) 0.71723(11) 0.0540(9) Uani 1 1 d . . .
H22A H -0.6850 0.0094 0.7133 0.065 Uiso 1 1 calc R . .
H22B H -0.5838 -0.1020 0.7378 0.065 Uiso 1 1 calc R . .
C12 C 0.0306(3) -0.1032(3) 0.35467(10) 0.0373(6) Uani 1 1 d . . .
H12A H 0.0192 -0.0068 0.3518 0.045 Uiso 1 1 calc R . .
H12B H 0.1228 -0.1208 0.3735 0.045 Uiso 1 1 calc R . .
C10 C 0.1592(3) -0.1109(3) 0.27913(10) 0.0374(6) Uani 1 1 d . . .
H10A H 0.1529 -0.0140 0.2770 0.045 Uiso 1 1 calc R . .
H10B H 0.2525 -0.1336 0.2964 0.045 Uiso 1 1 calc R . .
C15 C -0.2326(3) -0.1570(3) 0.45286(10) 0.0360(6) Uani 1 1 d . . .
H15A H -0.3232 -0.1423 0.4329 0.043 Uiso 1 1 calc R . .
H15B H -0.2187 -0.2531 0.4562 0.043 Uiso 1 1 calc R . .
C8 C 0.2832(3) -0.1358(3) 0.20250(10) 0.0390(7) Uani 1 1 d . . .
H8A H 0.3713 -0.1718 0.2196 0.047 Uiso 1 1 calc R . .
H8B H 0.2701 -0.1798 0.1720 0.047 Uiso 1 1 calc R . .
C24 C 0.4435(4) -0.2047(3) 0.01565(11) 0.0527(8) Uani 1 1 d . . .
H24A H 0.3589 -0.2463 -0.0009 0.079 Uiso 1 1 calc R . .
H24B H 0.5057 -0.2723 0.0310 0.079 Uiso 1 1 calc R . .
H24C H 0.4961 -0.1564 -0.0063 0.079 Uiso 1 1 calc R . .
C5 C 0.2871(4) 0.0518(3) 0.08370(11) 0.0470(8) Uani 1 1 d . . .
H5 H 0.2251 0.1227 0.0889 0.056 Uiso 1 1 calc R . .
C20 C -0.5301(3) -0.0926(3) 0.64544(10) 0.0406(7) Uani 1 1 d . . .
H20A H -0.5435 0.0034 0.6416 0.049 Uiso 1 1 calc R . .
H20B H -0.4399 -0.1069 0.6657 0.049 Uiso 1 1 calc R . .
C14 C -0.1064(3) -0.0989(3) 0.42862(9) 0.0363(6) Uani 1 1 d . . .
H14A H -0.0155 -0.1142 0.4484 0.044 Uiso 1 1 calc R . .
H14B H -0.1199 -0.0028 0.4253 0.044 Uiso 1 1 calc R . .
C11 C 0.0355(3) -0.1632(3) 0.30602(10) 0.0385(6) Uani 1 1 d . . .
H11A H -0.0570 -0.1453 0.2875 0.046 Uiso 1 1 calc R . .
H11B H 0.0454 -0.2597 0.3092 0.046 Uiso 1 1 calc R . .
C2 C 0.4574(3) -0.1009(3) 0.09525(10) 0.0365(6) Uani 1 1 d . . .
H2 H 0.5327 -0.1541 0.1094 0.044 Uiso 1 1 calc R . .
C7 C 0.3041(3) 0.0129(3) 0.19499(10) 0.0352(6) Uani 1 1 d . . .
H7A H 0.3253 0.0561 0.2254 0.042 Uiso 1 1 calc R . .
H7B H 0.2136 0.0504 0.1800 0.042 Uiso 1 1 calc R . .
C19 C -0.5143(3) -0.1541(3) 0.59770(10) 0.0374(6) Uani 1 1 d . . .
H19A H -0.6047 -0.1407 0.5775 0.045 Uiso 1 1 calc R . .
H19B H -0.4995 -0.2499 0.6016 0.045 Uiso 1 1 calc R . .
C23 C -0.8011(4) -0.1411(4) 0.74084(13) 0.0630(10) Uani 1 1 d . . .
H23A H -0.8900 -0.1280 0.7205 0.095 Uiso 1 1 calc R . .
H23B H -0.8075 -0.0946 0.7700 0.095 Uiso 1 1 calc R . .
H23C H -0.7869 -0.2350 0.7470 0.095 Uiso 1 1 calc R . .
C16 C -0.2473(3) -0.0972(3) 0.50126(9) 0.0363(6) Uani 1 1 d . . .
H16A H -0.1567 -0.1120 0.5213 0.044 Uiso 1 1 calc R . .
H16B H -0.2614 -0.0012 0.4980 0.044 Uiso 1 1 calc R . .
C4 C 0.2897(4) -0.0163(3) 0.04353(12) 0.0498(8) Uani 1 1 d . . .
H4 H 0.2298 -0.0017 0.0157 0.060 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
As1 0.04210(18) 0.03486(17) 0.03947(19) 0.00395(13) 0.00548(14) 0.00009(13)
F4 0.0628(12) 0.0584(12) 0.0418(10) 0.0069(8) 0.0127(9) -0.0042(9)
F3 0.0536(11) 0.0536(13) 0.1020(17) 0.0207(12) 0.0102(12) 0.0111(10)
F2 0.0584(12) 0.1080(19) 0.0594(13) 0.0356(13) 0.0095(11) -0.0150(12)
F5 0.0511(10) 0.0444(11) 0.0672(12) -0.0056(9) 0.0066(9) 0.0064(8)
N1 0.0381(12) 0.0317(13) 0.0361(12) 0.0028(9) 0.0092(11) -0.0055(9)
F6 0.0650(12) 0.0468(12) 0.0791(15) -0.0170(10) 0.0018(11) -0.0069(10)
F1 0.0507(11) 0.0823(15) 0.0483(11) -0.0176(10) 0.0065(9) -0.0107(10)
C21 0.0503(17) 0.0355(16) 0.0334(15) 0.0002(12) 0.0078(13) 0.0007(13)
C9 0.0468(16) 0.0361(16) 0.0393(16) 0.0005(12) 0.0110(14) -0.0060(13)
C18 0.0444(16) 0.0363(16) 0.0340(15) -0.0026(12) 0.0081(13) -0.0022(12)
C17 0.0424(15) 0.0355(15) 0.0330(15) -0.0026(11) 0.0067(13) -0.0007(12)
C6 0.0428(15) 0.0375(17) 0.0373(15) -0.0033(12) 0.0084(13) -0.0091(12)
C13 0.0414(15) 0.0352(15) 0.0357(15) 0.0010(11) 0.0088(13) -0.0006(12)
N3 0.0486(14) 0.0347(13) 0.0354(13) 0.0017(10) 0.0076(12) -0.0102(11)
C22 0.058(2) 0.067(2) 0.0382(17) -0.0144(16) 0.0100(16) -0.0043(17)
C12 0.0407(15) 0.0379(16) 0.0341(15) 0.0008(12) 0.0071(13) -0.0030(12)
C10 0.0372(14) 0.0380(16) 0.0381(15) 0.0012(12) 0.0092(13) -0.0032(12)
C15 0.0406(15) 0.0355(15) 0.0325(14) -0.0019(11) 0.0069(13) -0.0026(12)
C8 0.0449(16) 0.0330(16) 0.0409(16) 0.0011(12) 0.0135(14) 0.0009(12)
C24 0.070(2) 0.048(2) 0.0423(18) -0.0081(14) 0.0149(17) -0.0138(17)
C5 0.0523(18) 0.0443(19) 0.0448(18) 0.0099(14) 0.0069(16) 0.0078(14)
C20 0.0450(16) 0.0426(18) 0.0347(15) -0.0041(12) 0.0060(13) -0.0010(13)
C14 0.0402(15) 0.0376(16) 0.0315(14) 0.0004(11) 0.0057(12) -0.0010(12)
C11 0.0423(15) 0.0358(16) 0.0390(16) 0.0022(12) 0.0123(13) -0.0015(12)
C2 0.0367(14) 0.0327(15) 0.0411(16) 0.0016(12) 0.0079(13) -0.0028(11)
C7 0.0372(14) 0.0329(15) 0.0364(15) -0.0034(11) 0.0078(13) 0.0006(11)
C19 0.0420(15) 0.0365(16) 0.0341(15) -0.0025(11) 0.0059(13) -0.0005(12)
C23 0.089(3) 0.055(2) 0.051(2) 0.0001(16) 0.034(2) -0.003(2)
C16 0.0413(14) 0.0364(16) 0.0313(14) -0.0009(11) 0.0041(12) -0.0007(12)
C4 0.0528(19) 0.056(2) 0.0397(17) 0.0114(14) -0.0001(15) -0.0010(16)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
As1 F6 1.703(2) . ?
As1 F4 1.7043(17) . ?
As1 F5 1.7088(18) . ?
As1 F3 1.7119(19) . ?
As1 F2 1.7158(18) . ?
As1 F1 1.7198(19) . ?
N1 C2 1.327(3) . ?
N1 C5 1.370(4) . ?
N1 C6 1.466(4) . ?
C21 C22 1.514(4) . ?
C21 C20 1.520(4) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C9 C10 1.526(4) . ?
C9 C8 1.532(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C18 C19 1.522(4) . ?
C18 C17 1.522(4) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C17 C16 1.523(4) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C6 C7 1.528(4) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C13 C14 1.526(4) . ?
C13 C12 1.529(4) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
N3 C2 1.329(4) . ?
N3 C4 1.373(4) . ?
N3 C24 1.465(4) . ?
C22 C23 1.516(5) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C12 C11 1.517(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C10 C11 1.528(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C15 C16 1.523(4) . ?
C15 C14 1.525(4) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C8 C7 1.514(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C5 C4 1.335(5) . ?
C5 H5 0.9300 . ?
C20 C19 1.515(4) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C2 H2 0.9300 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C4 H4 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F6 As1 F4 91.29(10) . . ?
F6 As1 F5 89.95(10) . . ?
F4 As1 F5 90.51(9) . . ?
F6 As1 F3 91.17(11) . . ?
F4 As1 F3 89.14(10) . . ?
F5 As1 F3 178.83(10) . . ?
F6 As1 F2 90.29(11) . . ?
F4 As1 F2 178.36(10) . . ?
F5 As1 F2 89.91(11) . . ?
F3 As1 F2 90.41(11) . . ?
F6 As1 F1 179.42(9) . . ?
F4 As1 F1 89.16(9) . . ?
F5 As1 F1 89.69(10) . . ?
F3 As1 F1 89.19(11) . . ?
F2 As1 F1 89.26(11) . . ?
C2 N1 C5 108.1(3) . . ?
C2 N1 C6 125.9(3) . . ?
C5 N1 C6 126.0(3) . . ?
C22 C21 C20 114.2(3) . . ?
C22 C21 H21A 108.7 . . ?
C20 C21 H21A 108.7 . . ?
C22 C21 H21B 108.7 . . ?
C20 C21 H21B 108.7 . . ?
H21A C21 H21B 107.6 . . ?
C10 C9 C8 115.2(2) . . ?
C10 C9 H9A 108.5 . . ?
C8 C9 H9A 108.5 . . ?
C10 C9 H9B 108.5 . . ?
C8 C9 H9B 108.5 . . ?
H9A C9 H9B 107.5 . . ?
C19 C18 C17 114.0(2) . . ?
C19 C18 H18A 108.8 . . ?
C17 C18 H18A 108.8 . . ?
C19 C18 H18B 108.8 . . ?
C17 C18 H18B 108.8 . . ?
H18A C18 H18B 107.7 . . ?
C18 C17 C16 113.6(2) . . ?
C18 C17 H17A 108.8 . . ?
C16 C17 H17A 108.8 . . ?
C18 C17 H17B 108.8 . . ?
C16 C17 H17B 108.8 . . ?
H17A C17 H17B 107.7 . . ?
N1 C6 C7 111.8(2) . . ?
N1 C6 H6A 109.3 . . ?
C7 C6 H6A 109.3 . . ?
N1 C6 H6B 109.3 . . ?
C7 C6 H6B 109.3 . . ?
H6A C6 H6B 107.9 . . ?
C14 C13 C12 114.4(2) . . ?
C14 C13 H13A 108.7 . . ?
C12 C13 H13A 108.7 . . ?
C14 C13 H13B 108.7 . . ?
C12 C13 H13B 108.7 . . ?
H13A C13 H13B 107.6 . . ?
C2 N3 C4 108.2(3) . . ?
C2 N3 C24 125.7(3) . . ?
C4 N3 C24 126.1(3) . . ?
C21 C22 C23 114.0(3) . . ?
C21 C22 H22A 108.7 . . ?
C23 C22 H22A 108.7 . . ?
C21 C22 H22B 108.7 . . ?
C23 C22 H22B 108.7 . . ?
H22A C22 H22B 107.6 . . ?
C11 C12 C13 112.7(2) . . ?
C11 C12 H12A 109.1 . . ?
C13 C12 H12A 109.1 . . ?
C11 C12 H12B 109.1 . . ?
C13 C12 H12B 109.1 . . ?
H12A C12 H12B 107.8 . . ?
C9 C10 C11 112.0(2) . . ?
C9 C10 H10A 109.2 . . ?
C11 C10 H10A 109.2 . . ?
C9 C10 H10B 109.2 . . ?
C11 C10 H10B 109.2 . . ?
H10A C10 H10B 107.9 . . ?
C16 C15 C14 113.9(2) . . ?
C16 C15 H15A 108.8 . . ?
C14 C15 H15A 108.8 . . ?
C16 C15 H15B 108.8 . . ?
C14 C15 H15B 108.8 . . ?
H15A C15 H15B 107.7 . . ?
C7 C8 C9 113.9(2) . . ?
C7 C8 H8A 108.8 . . ?
C9 C8 H8A 108.8 . . ?
C7 C8 H8B 108.8 . . ?
C9 C8 H8B 108.8 . . ?
H8A C8 H8B 107.7 . . ?
N3 C24 H24A 109.5 . . ?
N3 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N3 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C4 C5 N1 107.7(3) . . ?
C4 C5 H5 126.2 . . ?
N1 C5 H5 126.2 . . ?
C19 C20 C21 114.2(2) . . ?
C19 C20 H20A 108.7 . . ?
C21 C20 H20A 108.7 . . ?
C19 C20 H20B 108.7 . . ?
C21 C20 H20B 108.7 . . ?
H20A C20 H20B 107.6 . . ?
C15 C14 C13 113.0(2) . . ?
C15 C14 H14A 109.0 . . ?
C13 C14 H14A 109.0 . . ?
C15 C14 H14B 109.0 . . ?
C13 C14 H14B 109.0 . . ?
H14A C14 H14B 107.8 . . ?
C12 C11 C10 114.8(2) . . ?
C12 C11 H11A 108.6 . . ?
C10 C11 H11A 108.6 . . ?
C12 C11 H11B 108.6 . . ?
C10 C11 H11B 108.6 . . ?
H11A C11 H11B 107.5 . . ?
N1 C2 N3 108.7(3) . . ?
N1 C2 H2 125.6 . . ?
N3 C2 H2 125.6 . . ?
C8 C7 C6 112.9(2) . . ?
C8 C7 H7A 109.0 . . ?
C6 C7 H7A 109.0 . . ?
C8 C7 H7B 109.0 . . ?
C6 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
C20 C19 C18 113.7(2) . . ?
C20 C19 H19A 108.8 . . ?
C18 C19 H19A 108.8 . . ?
C20 C19 H19B 108.8 . . ?
C18 C19 H19B 108.8 . . ?
H19A C19 H19B 107.7 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C17 C16 C15 113.6(2) . . ?
C17 C16 H16A 108.9 . . ?
C15 C16 H16A 108.9 . . ?
C17 C16 H16B 108.9 . . ?
C15 C16 H16B 108.9 . . ?
H16A C16 H16B 107.7 . . ?
C5 C4 N3 107.3(3) . . ?
C5 C4 H4 126.3 . . ?
N3 C4 H4 126.3 . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.838
_refine_diff_density_min         -0.657
_refine_diff_density_rms         0.080

#=END

data_C18MImSbF6--100oC
#TrackingRef '- SI--100oC.cif'

_database_code_depnum_ccdc_archive 'CCDC 843149'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            C18MImSbF6
_chemical_melting_point          347.5
_chemical_formula_moiety         
;
(C22 N2 H43 +), (Sb F6 -)
;
_chemical_formula_sum            'C22 H43 F6 N2 Sb'
_chemical_formula_weight         571.33

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/a
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x-1/2, -y-1/2, z'

_cell_length_a                   9.2091(3)
_cell_length_b                   10.1539(5)
_cell_length_c                   28.5250(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.2477(10)
_cell_angle_gamma                90.00
_cell_volume                     2651.47(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    173
_cell_measurement_reflns_used    22679
_cell_measurement_theta_min      5.99
_cell_measurement_theta_max      54.99

_exptl_crystal_description       platelet
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1176
_exptl_absorpt_coefficient_mu    1.093
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7247
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'RAPID AUTO 2.40 (Rigaku 2006)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS RapidII'
_diffrn_measurement_method       'imaging plate'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            25221
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         3.00
_diffrn_reflns_theta_max         27.48
_reflns_number_total             6035
_reflns_number_gt                5442
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Rigaku R-AXIS Rapid-II'
_computing_cell_refinement       'RAPID AUTO 2.40 (Rigaku 2006)'
_computing_data_reduction        'RAPID AUTO 2.40 (Rigaku 2006)'
_computing_structure_solution    'SIR92 (Altmare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0392P)^2^+0.6381P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6035
_refine_ls_number_parameters     282
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0262
_refine_ls_wR_factor_ref         0.0676
_refine_ls_wR_factor_gt          0.0656
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sb1 Sb -0.142547(12) 0.016685(12) 0.106039(4) 0.03108(5) Uani 1 1 d . . .
F4 F -0.22005(14) -0.06319(13) 0.15688(4) 0.0486(3) Uani 1 1 d . . .
F3 F -0.30077(13) 0.13320(13) 0.10018(5) 0.0546(3) Uani 1 1 d . . .
F2 F -0.07123(14) 0.09414(16) 0.05337(5) 0.0599(4) Uani 1 1 d . . .
F5 F 0.01234(13) -0.10361(12) 0.11142(5) 0.0472(3) Uani 1 1 d . . .
N1 N 0.39256(18) 0.00198(14) 0.11947(6) 0.0298(3) Uani 1 1 d . . .
F6 F -0.03278(14) 0.13301(13) 0.14596(5) 0.0529(3) Uani 1 1 d . . .
F1 F -0.25248(13) -0.09963(14) 0.06481(5) 0.0538(3) Uani 1 1 d . . .
C21 C -0.6669(2) -0.14816(19) 0.66823(6) 0.0345(4) Uani 1 1 d . . .
H21A H -0.7557 -0.1344 0.6472 0.041 Uiso 1 1 calc R . .
H21B H -0.6534 -0.2424 0.6723 0.041 Uiso 1 1 calc R . .
C9 C 0.1589(2) -0.16881(19) 0.23298(6) 0.0352(4) Uani 1 1 d . . .
H9A H 0.0705 -0.1372 0.2149 0.042 Uiso 1 1 calc R . .
H9B H 0.1516 -0.2639 0.2349 0.042 Uiso 1 1 calc R . .
C18 C -0.3930(2) -0.09514(19) 0.57425(6) 0.0342(4) Uani 1 1 d . . .
H18A H -0.3037 -0.1092 0.5950 0.041 Uiso 1 1 calc R . .
H18B H -0.4070 -0.0008 0.5707 0.041 Uiso 1 1 calc R . .
C17 C -0.37519(19) -0.15473(18) 0.52611(6) 0.0325(4) Uani 1 1 d . . .
H17A H -0.3609 -0.2490 0.5297 0.039 Uiso 1 1 calc R . .
H17B H -0.4646 -0.1409 0.5054 0.039 Uiso 1 1 calc R . .
C6 C 0.4326(2) 0.04208(19) 0.16905(7) 0.0341(4) Uani 1 1 d . . .
H6A H 0.4529 0.1358 0.1702 0.041 Uiso 1 1 calc R . .
H6B H 0.5209 -0.0038 0.1815 0.041 Uiso 1 1 calc R . .
C13 C -0.09039(19) -0.15979(18) 0.38288(6) 0.0325(4) Uani 1 1 d . . .
H13A H -0.1811 -0.1455 0.3629 0.039 Uiso 1 1 calc R . .
H13B H -0.0770 -0.2541 0.3866 0.039 Uiso 1 1 calc R . .
N3 N 0.38906(17) -0.10182(16) 0.05318(5) 0.0348(3) Uani 1 1 d . . .
C22 C -0.6859(2) -0.0871(3) 0.71575(7) 0.0487(5) Uani 1 1 d . . .
H22A H -0.5979 -0.1024 0.7370 0.058 Uiso 1 1 calc R . .
H22B H -0.6975 0.0073 0.7119 0.058 Uiso 1 1 calc R . .
C12 C 0.03513(19) -0.10439(19) 0.35816(6) 0.0330(4) Uani 1 1 d . . .
H12A H 0.0239 -0.0097 0.3552 0.040 Uiso 1 1 calc R . .
H12B H 0.1266 -0.1216 0.3774 0.040 Uiso 1 1 calc R . .
C10 C 0.16581(19) -0.11220(19) 0.28278(6) 0.0330(4) Uani 1 1 d . . .
H10A H 0.1601 -0.0169 0.2810 0.040 Uiso 1 1 calc R . .
H10B H 0.2588 -0.1353 0.3001 0.040 Uiso 1 1 calc R . .
C15 C -0.23126(19) -0.15646(18) 0.45476(6) 0.0320(4) Uani 1 1 d . . .
H15A H -0.3211 -0.1422 0.4343 0.038 Uiso 1 1 calc R . .
H15B H -0.2175 -0.2508 0.4583 0.038 Uiso 1 1 calc R . .
C8 C 0.2889(2) -0.13481(18) 0.20615(6) 0.0334(4) Uani 1 1 d . . .
H8A H 0.3769 -0.1714 0.2230 0.040 Uiso 1 1 calc R . .
H8B H 0.2751 -0.1764 0.1754 0.040 Uiso 1 1 calc R . .
C24 C 0.4283(3) -0.1920(2) 0.01652(7) 0.0456(5) Uani 1 1 d . . .
H24A H 0.3422 -0.2365 0.0026 0.068 Uiso 1 1 calc R . .
H24B H 0.4974 -0.2557 0.0303 0.068 Uiso 1 1 calc R . .
H24C H 0.4710 -0.1431 -0.0073 0.068 Uiso 1 1 calc R . .
C5 C 0.2884(2) 0.0614(2) 0.08801(7) 0.0407(4) Uani 1 1 d . . .
H5 H 0.2305 0.1330 0.0942 0.049 Uiso 1 1 calc R . .
C20 C -0.5383(2) -0.0925(2) 0.64516(6) 0.0364(4) Uani 1 1 d . . .
H20A H -0.5512 0.0019 0.6415 0.044 Uiso 1 1 calc R . .
H20B H -0.4494 -0.1071 0.6660 0.044 Uiso 1 1 calc R . .
C14 C -0.10421(19) -0.09966(18) 0.43109(6) 0.0323(4) Uani 1 1 d . . .
H14A H -0.1175 -0.0053 0.4276 0.039 Uiso 1 1 calc R . .
H14B H -0.0141 -0.1145 0.4513 0.039 Uiso 1 1 calc R . .
C11 C 0.04199(19) -0.16369(18) 0.30933(6) 0.0331(4) Uani 1 1 d . . .
H11A H -0.0501 -0.1466 0.2904 0.040 Uiso 1 1 calc R . .
H11B H 0.0522 -0.2584 0.3126 0.040 Uiso 1 1 calc R . .
C2 C 0.45096(19) -0.09675(17) 0.09752(6) 0.0311(3) Uani 1 1 d . . .
H2 H 0.5234 -0.1532 0.1109 0.037 Uiso 1 1 calc R . .
C7 C 0.3110(2) 0.01146(17) 0.19960(7) 0.0309(4) Uani 1 1 d . . .
H7A H 0.3341 0.0522 0.2303 0.037 Uiso 1 1 calc R . .
H7B H 0.2205 0.0498 0.1852 0.037 Uiso 1 1 calc R . .
C19 C -0.5204(2) -0.15235(19) 0.59733(6) 0.0335(4) Uani 1 1 d . . .
H19A H -0.6097 -0.1386 0.5766 0.040 Uiso 1 1 calc R . .
H19B H -0.5062 -0.2466 0.6011 0.040 Uiso 1 1 calc R . .
C23 C -0.8156(3) -0.1411(2) 0.73801(8) 0.0576(6) Uani 1 1 d . . .
H23A H -0.9033 -0.1257 0.7173 0.086 Uiso 1 1 calc R . .
H23B H -0.8225 -0.0977 0.7676 0.086 Uiso 1 1 calc R . .
H23C H -0.8031 -0.2340 0.7432 0.086 Uiso 1 1 calc R . .
C16 C -0.2478(2) -0.09705(19) 0.50297(6) 0.0325(4) Uani 1 1 d . . .
H16A H -0.1582 -0.1114 0.5235 0.039 Uiso 1 1 calc R . .
H16B H -0.2618 -0.0027 0.4995 0.039 Uiso 1 1 calc R . .
C4 C 0.2860(3) -0.0034(2) 0.04688(8) 0.0436(5) Uani 1 1 d . . .
H4 H 0.2260 0.0149 0.0193 0.052 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Sb1 0.03323(8) 0.03021(8) 0.03051(8) 0.00217(4) 0.00665(5) 0.00044(4)
F4 0.0586(7) 0.0481(7) 0.0413(6) 0.0097(5) 0.0161(6) -0.0017(6)
F3 0.0417(6) 0.0439(7) 0.0799(9) 0.0154(6) 0.0137(6) 0.0114(5)
F2 0.0497(7) 0.0839(11) 0.0482(7) 0.0243(7) 0.0144(6) -0.0047(7)
F5 0.0407(6) 0.0389(6) 0.0622(8) -0.0029(5) 0.0064(6) 0.0080(5)
N1 0.0307(7) 0.0288(8) 0.0308(8) 0.0033(5) 0.0083(7) -0.0050(5)
F6 0.0546(7) 0.0417(7) 0.0620(8) -0.0149(6) 0.0034(6) -0.0078(6)
F1 0.0424(6) 0.0701(9) 0.0494(7) -0.0206(6) 0.0067(6) -0.0101(6)
C21 0.0402(9) 0.0367(10) 0.0274(8) -0.0018(7) 0.0078(8) -0.0008(7)
C9 0.0398(9) 0.0334(9) 0.0341(9) -0.0009(7) 0.0125(8) -0.0065(7)
C18 0.0378(9) 0.0360(10) 0.0297(8) -0.0019(7) 0.0077(7) -0.0017(7)
C17 0.0343(9) 0.0353(9) 0.0287(8) -0.0022(7) 0.0071(7) -0.0014(7)
C6 0.0365(9) 0.0339(9) 0.0330(9) -0.0047(7) 0.0091(8) -0.0096(7)
C13 0.0337(9) 0.0340(9) 0.0308(8) 0.0005(7) 0.0086(7) -0.0018(7)
N3 0.0403(8) 0.0344(8) 0.0309(7) 0.0021(6) 0.0094(7) -0.0081(6)
C22 0.0514(12) 0.0636(15) 0.0328(10) -0.0111(9) 0.0122(9) -0.0084(10)
C12 0.0345(9) 0.0356(9) 0.0300(8) 0.0008(7) 0.0084(7) -0.0032(7)
C10 0.0308(8) 0.0372(10) 0.0322(9) 0.0012(7) 0.0089(7) -0.0017(7)
C15 0.0337(9) 0.0349(9) 0.0284(8) -0.0008(7) 0.0078(7) -0.0012(7)
C8 0.0396(9) 0.0292(9) 0.0337(9) 0.0006(7) 0.0147(8) 0.0013(7)
C24 0.0623(13) 0.0430(11) 0.0340(9) -0.0058(8) 0.0159(9) -0.0127(10)
C5 0.0430(10) 0.0387(10) 0.0411(10) 0.0090(8) 0.0074(9) 0.0069(8)
C20 0.0386(9) 0.0402(10) 0.0308(9) -0.0053(7) 0.0061(8) -0.0037(8)
C14 0.0334(8) 0.0353(9) 0.0288(8) 0.0001(7) 0.0061(7) -0.0023(7)
C11 0.0338(9) 0.0332(9) 0.0337(9) 0.0011(7) 0.0108(7) -0.0025(7)
C2 0.0331(8) 0.0298(9) 0.0314(8) 0.0024(7) 0.0080(7) -0.0030(7)
C7 0.0337(9) 0.0293(9) 0.0312(9) -0.0033(6) 0.0094(8) -0.0014(6)
C19 0.0369(9) 0.0363(10) 0.0280(8) -0.0027(7) 0.0071(7) -0.0004(7)
C23 0.0789(16) 0.0550(14) 0.0445(11) 0.0012(10) 0.0320(12) -0.0036(12)
C16 0.0341(8) 0.0343(9) 0.0294(8) -0.0012(7) 0.0054(7) -0.0015(7)
C4 0.0466(12) 0.0489(12) 0.0350(10) 0.0102(8) 0.0034(9) -0.0003(9)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sb1 F6 1.8610(12) . ?
Sb1 F4 1.8696(11) . ?
Sb1 F3 1.8702(12) . ?
Sb1 F5 1.8715(11) . ?
Sb1 F2 1.8766(12) . ?
Sb1 F1 1.8825(12) . ?
N1 C2 1.326(2) . ?
N1 C5 1.379(3) . ?
N1 C6 1.480(2) . ?
C21 C22 1.518(2) . ?
C21 C20 1.525(2) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C9 C10 1.527(2) . ?
C9 C8 1.529(2) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C18 C19 1.521(2) . ?
C18 C17 1.525(2) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C17 C16 1.524(2) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C6 C7 1.524(2) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C13 C14 1.523(2) . ?
C13 C12 1.526(2) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
N3 C2 1.331(2) . ?
N3 C4 1.377(3) . ?
N3 C24 1.465(2) . ?
C22 C23 1.515(3) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C12 C11 1.525(2) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C10 C11 1.528(2) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C15 C16 1.524(2) . ?
C15 C14 1.526(2) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C8 C7 1.513(2) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C5 C4 1.343(3) . ?
C5 H5 0.9300 . ?
C20 C19 1.519(2) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C2 H2 0.9300 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C4 H4 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F6 Sb1 F4 91.63(6) . . ?
F6 Sb1 F3 91.10(6) . . ?
F4 Sb1 F3 89.09(6) . . ?
F6 Sb1 F5 90.33(6) . . ?
F4 Sb1 F5 90.30(6) . . ?
F3 Sb1 F5 178.46(6) . . ?
F6 Sb1 F2 90.56(6) . . ?
F4 Sb1 F2 177.66(6) . . ?
F3 Sb1 F2 90.03(6) . . ?
F5 Sb1 F2 90.52(6) . . ?
F6 Sb1 F1 179.07(6) . . ?
F4 Sb1 F1 89.30(6) . . ?
F3 Sb1 F1 88.87(6) . . ?
F5 Sb1 F1 89.71(6) . . ?
F2 Sb1 F1 88.51(6) . . ?
C2 N1 C5 108.21(17) . . ?
C2 N1 C6 125.97(17) . . ?
C5 N1 C6 125.81(16) . . ?
C22 C21 C20 113.86(16) . . ?
C22 C21 H21A 108.8 . . ?
C20 C21 H21A 108.8 . . ?
C22 C21 H21B 108.8 . . ?
C20 C21 H21B 108.8 . . ?
H21A C21 H21B 107.7 . . ?
C10 C9 C8 115.16(15) . . ?
C10 C9 H9A 108.5 . . ?
C8 C9 H9A 108.5 . . ?
C10 C9 H9B 108.5 . . ?
C8 C9 H9B 108.5 . . ?
H9A C9 H9B 107.5 . . ?
C19 C18 C17 113.68(15) . . ?
C19 C18 H18A 108.8 . . ?
C17 C18 H18A 108.8 . . ?
C19 C18 H18B 108.8 . . ?
C17 C18 H18B 108.8 . . ?
H18A C18 H18B 107.7 . . ?
C16 C17 C18 113.62(15) . . ?
C16 C17 H17A 108.8 . . ?
C18 C17 H17A 108.8 . . ?
C16 C17 H17B 108.8 . . ?
C18 C17 H17B 108.8 . . ?
H17A C17 H17B 107.7 . . ?
N1 C6 C7 111.59(15) . . ?
N1 C6 H6A 109.3 . . ?
C7 C6 H6A 109.3 . . ?
N1 C6 H6B 109.3 . . ?
C7 C6 H6B 109.3 . . ?
H6A C6 H6B 108.0 . . ?
C14 C13 C12 114.31(15) . . ?
C14 C13 H13A 108.7 . . ?
C12 C13 H13A 108.7 . . ?
C14 C13 H13B 108.7 . . ?
C12 C13 H13B 108.7 . . ?
H13A C13 H13B 107.6 . . ?
C2 N3 C4 108.30(17) . . ?
C2 N3 C24 126.12(17) . . ?
C4 N3 C24 125.52(18) . . ?
C23 C22 C21 113.55(19) . . ?
C23 C22 H22A 108.9 . . ?
C21 C22 H22A 108.9 . . ?
C23 C22 H22B 108.9 . . ?
C21 C22 H22B 108.9 . . ?
H22A C22 H22B 107.7 . . ?
C11 C12 C13 112.67(15) . . ?
C11 C12 H12A 109.1 . . ?
C13 C12 H12A 109.1 . . ?
C11 C12 H12B 109.1 . . ?
C13 C12 H12B 109.1 . . ?
H12A C12 H12B 107.8 . . ?
C9 C10 C11 111.99(15) . . ?
C9 C10 H10A 109.2 . . ?
C11 C10 H10A 109.2 . . ?
C9 C10 H10B 109.2 . . ?
C11 C10 H10B 109.2 . . ?
H10A C10 H10B 107.9 . . ?
C16 C15 C14 113.98(15) . . ?
C16 C15 H15A 108.8 . . ?
C14 C15 H15A 108.8 . . ?
C16 C15 H15B 108.8 . . ?
C14 C15 H15B 108.8 . . ?
H15A C15 H15B 107.7 . . ?
C7 C8 C9 113.98(15) . . ?
C7 C8 H8A 108.8 . . ?
C9 C8 H8A 108.8 . . ?
C7 C8 H8B 108.8 . . ?
C9 C8 H8B 108.8 . . ?
H8A C8 H8B 107.7 . . ?
N3 C24 H24A 109.5 . . ?
N3 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N3 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C4 C5 N1 107.37(19) . . ?
C4 C5 H5 126.3 . . ?
N1 C5 H5 126.3 . . ?
C19 C20 C21 113.88(16) . . ?
C19 C20 H20A 108.8 . . ?
C21 C20 H20A 108.8 . . ?
C19 C20 H20B 108.8 . . ?
C21 C20 H20B 108.8 . . ?
H20A C20 H20B 107.7 . . ?
C13 C14 C15 113.05(15) . . ?
C13 C14 H14A 109.0 . . ?
C15 C14 H14A 109.0 . . ?
C13 C14 H14B 109.0 . . ?
C15 C14 H14B 109.0 . . ?
H14A C14 H14B 107.8 . . ?
C12 C11 C10 115.14(15) . . ?
C12 C11 H11A 108.5 . . ?
C10 C11 H11A 108.5 . . ?
C12 C11 H11B 108.5 . . ?
C10 C11 H11B 108.5 . . ?
H11A C11 H11B 107.5 . . ?
N1 C2 N3 108.91(17) . . ?
N1 C2 H2 125.5 . . ?
N3 C2 H2 125.5 . . ?
C8 C7 C6 112.82(15) . . ?
C8 C7 H7A 109.0 . . ?
C6 C7 H7A 109.0 . . ?
C8 C7 H7B 109.0 . . ?
C6 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
C20 C19 C18 113.60(15) . . ?
C20 C19 H19A 108.8 . . ?
C18 C19 H19A 108.8 . . ?
C20 C19 H19B 108.8 . . ?
C18 C19 H19B 108.8 . . ?
H19A C19 H19B 107.7 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C17 C16 C15 113.33(15) . . ?
C17 C16 H16A 108.9 . . ?
C15 C16 H16A 108.9 . . ?
C17 C16 H16B 108.9 . . ?
C15 C16 H16B 108.9 . . ?
H16A C16 H16B 107.7 . . ?
C5 C4 N3 107.21(19) . . ?
C5 C4 H4 126.4 . . ?
N3 C4 H4 126.4 . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.931
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.069

#=END

data_C18MImNbF6--100oC
#TrackingRef '- SI--100oC.cif'

_database_code_depnum_ccdc_archive 'CCDC 843150'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            C18MImNbF6
_chemical_melting_point          347.2
_chemical_formula_moiety         
;
(C22 N2 H43 +), (Nb F6 -)
;
_chemical_formula_sum            'C22 H43 F6 N2 Nb'
_chemical_formula_weight         542.49

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/a

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x-1/2, -y-1/2, z'

_cell_length_a                   9.1865(5)
_cell_length_b                   10.1457(7)
_cell_length_c                   28.4689(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.1335(16)
_cell_angle_gamma                90.00
_cell_volume                     2638.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173
_cell_measurement_reflns_used    11043
_cell_measurement_theta_min      6.00
_cell_measurement_theta_max      54.97

_exptl_crystal_description       platelet
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1136
_exptl_absorpt_coefficient_mu    0.509
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6281
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'RAPID AUTO 2.40 (Rigaku 2006)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS RapidII'
_diffrn_measurement_method       'imaging plate'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15005
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_sigmaI/netI    0.0743
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         3.00
_diffrn_reflns_theta_max         27.48
_reflns_number_total             5954
_reflns_number_gt                4284
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Rigaku R-AXIS Rapid-II'
_computing_cell_refinement       'RAPID AUTO 2.40 (Rigaku 2006)'
_computing_data_reduction        'RAPID AUTO 2.40 (Rigaku 2006)'
_computing_structure_solution    'SIR92 (Altmare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0458P)^2^+4.1931P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5954
_refine_ls_number_parameters     282
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0470
_refine_ls_wR_factor_ref         0.1454
_refine_ls_wR_factor_gt          0.1125
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb -0.14172(4) 0.01661(4) 0.106348(12) 0.03317(13) Uani 1 1 d . . .
F4 F -0.2233(3) -0.0646(3) 0.15662(9) 0.0502(7) Uani 1 1 d . . .
F3 F -0.2997(3) 0.1347(3) 0.10124(11) 0.0574(8) Uani 1 1 d . . .
F2 F -0.0698(3) 0.0948(4) 0.05340(10) 0.0603(8) Uani 1 1 d . . .
F5 F 0.0123(3) -0.1063(3) 0.11137(10) 0.0483(6) Uani 1 1 d . . .
N1 N 0.3924(3) 0.0018(3) 0.11877(11) 0.0312(7) Uani 1 1 d . . .
F6 F -0.0298(3) 0.1320(3) 0.14654(10) 0.0541(7) Uani 1 1 d . . .
F1 F -0.2529(3) -0.0987(3) 0.06442(10) 0.0558(8) Uani 1 1 d . . .
C21 C -0.6676(5) -0.1472(5) 0.66860(14) 0.0385(9) Uani 1 1 d . . .
H21A H -0.6547 -0.2416 0.6725 0.046 Uiso 1 1 calc R . .
H21B H -0.7566 -0.1328 0.6477 0.046 Uiso 1 1 calc R . .
C9 C 0.1593(4) -0.1685(5) 0.23251(14) 0.0363(9) Uani 1 1 d . . .
H9A H 0.0707 -0.1371 0.2144 0.044 Uiso 1 1 calc R . .
H9B H 0.1522 -0.2637 0.2345 0.044 Uiso 1 1 calc R . .
C18 C -0.3933(5) -0.0953(4) 0.57430(14) 0.0366(9) Uani 1 1 d . . .
H18A H -0.3031 -0.1090 0.5947 0.044 Uiso 1 1 calc R . .
H18B H -0.4080 -0.0010 0.5707 0.044 Uiso 1 1 calc R . .
C17 C -0.3772(5) -0.1553(4) 0.52592(14) 0.0360(9) Uani 1 1 d . . .
H17A H -0.4667 -0.1405 0.5053 0.043 Uiso 1 1 calc R . .
H17B H -0.3635 -0.2497 0.5293 0.043 Uiso 1 1 calc R . .
C6 C 0.4329(4) 0.0432(4) 0.16833(14) 0.0355(9) Uani 1 1 d . . .
H6A H 0.4523 0.1371 0.1692 0.043 Uiso 1 1 calc R . .
H6B H 0.5221 -0.0018 0.1807 0.043 Uiso 1 1 calc R . .
C13 C -0.0906(4) -0.1607(4) 0.38279(14) 0.0354(9) Uani 1 1 d . . .
H13A H -0.1817 -0.1468 0.3629 0.043 Uiso 1 1 calc R . .
H13B H -0.0767 -0.2550 0.3866 0.043 Uiso 1 1 calc R . .
N3 N 0.3863(4) -0.1012(4) 0.05235(11) 0.0362(8) Uani 1 1 d . . .
C22 C -0.6859(6) -0.0865(6) 0.71642(16) 0.0512(12) Uani 1 1 d . . .
H22A H -0.6973 0.0081 0.7126 0.061 Uiso 1 1 calc R . .
H22B H -0.5975 -0.1021 0.7375 0.061 Uiso 1 1 calc R . .
C12 C 0.0357(4) -0.1043(4) 0.35781(13) 0.0333(8) Uani 1 1 d . . .
H12A H 0.0236 -0.0096 0.3547 0.040 Uiso 1 1 calc R . .
H12B H 0.1274 -0.1208 0.3771 0.040 Uiso 1 1 calc R . .
C10 C 0.1653(4) -0.1121(5) 0.28219(14) 0.0360(9) Uani 1 1 d . . .
H10A H 0.2589 -0.1341 0.2995 0.043 Uiso 1 1 calc R . .
H10B H 0.1584 -0.0168 0.2803 0.043 Uiso 1 1 calc R . .
C15 C -0.2314(4) -0.1572(4) 0.45476(14) 0.0356(9) Uani 1 1 d . . .
H15A H -0.3214 -0.1434 0.4342 0.043 Uiso 1 1 calc R . .
H15B H -0.2171 -0.2515 0.4585 0.043 Uiso 1 1 calc R . .
C8 C 0.2901(5) -0.1342(4) 0.20564(15) 0.0360(9) Uani 1 1 d . . .
H8A H 0.3780 -0.1714 0.2225 0.043 Uiso 1 1 calc R . .
H8B H 0.2762 -0.1752 0.1747 0.043 Uiso 1 1 calc R . .
C24 C 0.4238(6) -0.1913(5) 0.01538(16) 0.0486(12) Uani 1 1 d . . .
H24A H 0.3463 -0.2541 0.0086 0.073 Uiso 1 1 calc R . .
H24B H 0.5129 -0.2368 0.0259 0.073 Uiso 1 1 calc R . .
H24C H 0.4367 -0.1420 -0.0127 0.073 Uiso 1 1 calc R . .
C5 C 0.2877(5) 0.0614(5) 0.08755(15) 0.0409(10) Uani 1 1 d . . .
H5 H 0.2295 0.1328 0.0939 0.049 Uiso 1 1 calc R . .
C20 C -0.5392(5) -0.0923(5) 0.64546(14) 0.0380(9) Uani 1 1 d . . .
H20A H -0.4503 -0.1061 0.6665 0.046 Uiso 1 1 calc R . .
H20B H -0.5525 0.0021 0.6414 0.046 Uiso 1 1 calc R . .
C14 C -0.1036(5) -0.0994(4) 0.43113(14) 0.0365(9) Uani 1 1 d . . .
H14A H -0.1172 -0.0050 0.4275 0.044 Uiso 1 1 calc R . .
H14B H -0.0132 -0.1141 0.4513 0.044 Uiso 1 1 calc R . .
C11 C 0.0433(4) -0.1638(4) 0.30918(14) 0.0353(9) Uani 1 1 d . . .
H11A H 0.0549 -0.2585 0.3127 0.042 Uiso 1 1 calc R . .
H11B H -0.0494 -0.1481 0.2903 0.042 Uiso 1 1 calc R . .
C2 C 0.4508(4) -0.0955(4) 0.09676(14) 0.0327(8) Uani 1 1 d . . .
H2 H 0.5247 -0.1512 0.1099 0.039 Uiso 1 1 calc R . .
C7 C 0.3130(4) 0.0125(4) 0.19940(13) 0.0322(8) Uani 1 1 d . . .
H7A H 0.3378 0.0524 0.2302 0.039 Uiso 1 1 calc R . .
H7B H 0.2221 0.0517 0.1855 0.039 Uiso 1 1 calc R . .
C19 C -0.5193(4) -0.1530(5) 0.59776(13) 0.0351(9) Uani 1 1 d . . .
H19A H -0.5034 -0.2470 0.6019 0.042 Uiso 1 1 calc R . .
H19B H -0.6090 -0.1412 0.5769 0.042 Uiso 1 1 calc R . .
C23 C -0.8162(6) -0.1404(6) 0.73911(18) 0.0576(14) Uani 1 1 d . . .
H23A H -0.9037 -0.1293 0.7178 0.086 Uiso 1 1 calc R . .
H23B H -0.8258 -0.0937 0.7679 0.086 Uiso 1 1 calc R . .
H23C H -0.8013 -0.2324 0.7459 0.086 Uiso 1 1 calc R . .
C16 C -0.2478(4) -0.0966(4) 0.50310(14) 0.0343(8) Uani 1 1 d . . .
H16A H -0.2618 -0.0022 0.4995 0.041 Uiso 1 1 calc R . .
H16B H -0.1584 -0.1111 0.5238 0.041 Uiso 1 1 calc R . .
C4 C 0.2855(5) -0.0024(5) 0.04677(16) 0.0442(10) Uani 1 1 d . . .
H4 H 0.2255 0.0169 0.0192 0.053 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Nb1 0.0359(2) 0.0322(2) 0.03234(19) 0.00229(15) 0.00814(14) 0.00051(15)
F4 0.0579(16) 0.0492(17) 0.0457(14) 0.0111(12) 0.0164(13) -0.0001(13)
F3 0.0465(15) 0.0464(18) 0.082(2) 0.0161(14) 0.0171(15) 0.0124(13)
F2 0.0520(16) 0.083(2) 0.0488(16) 0.0236(15) 0.0168(13) -0.0021(16)
F5 0.0448(14) 0.0386(16) 0.0619(16) -0.0020(12) 0.0068(13) 0.0054(12)
N1 0.0329(16) 0.0296(18) 0.0323(15) 0.0016(13) 0.0090(13) -0.0054(13)
F6 0.0558(16) 0.0425(17) 0.0637(17) -0.0108(13) 0.0054(14) -0.0051(13)
F1 0.0482(15) 0.070(2) 0.0502(15) -0.0173(14) 0.0119(13) -0.0098(14)
C21 0.049(2) 0.037(2) 0.032(2) 0.0004(16) 0.0112(18) 0.0004(19)
C9 0.037(2) 0.038(2) 0.035(2) 0.0002(17) 0.0098(17) -0.0051(17)
C18 0.044(2) 0.038(2) 0.0294(19) 0.0008(16) 0.0105(17) -0.0020(18)
C17 0.041(2) 0.038(2) 0.0317(19) -0.0022(16) 0.0135(17) -0.0026(17)
C6 0.036(2) 0.039(2) 0.0326(19) -0.0041(16) 0.0088(17) -0.0079(17)
C13 0.040(2) 0.034(2) 0.034(2) 0.0025(16) 0.0122(17) 0.0008(17)
N3 0.0421(19) 0.038(2) 0.0294(16) 0.0006(14) 0.0099(15) -0.0078(15)
C22 0.063(3) 0.058(3) 0.036(2) -0.010(2) 0.018(2) -0.007(2)
C12 0.0296(18) 0.040(2) 0.0304(19) 0.0015(16) 0.0028(15) -0.0028(16)
C10 0.036(2) 0.039(2) 0.035(2) 0.0017(17) 0.0121(17) -0.0022(17)
C15 0.038(2) 0.037(2) 0.0335(19) -0.0013(16) 0.0112(17) 0.0004(17)
C8 0.046(2) 0.028(2) 0.037(2) -0.0020(16) 0.0202(18) 0.0005(17)
C24 0.068(3) 0.042(3) 0.039(2) -0.0049(19) 0.019(2) -0.010(2)
C5 0.040(2) 0.043(3) 0.041(2) 0.0078(18) 0.0069(19) 0.0056(19)
C20 0.036(2) 0.046(3) 0.0318(19) -0.0048(17) 0.0035(17) -0.0024(18)
C14 0.042(2) 0.037(2) 0.0318(19) -0.0010(16) 0.0105(17) -0.0028(18)
C11 0.036(2) 0.037(2) 0.034(2) 0.0035(16) 0.0118(17) 0.0005(17)
C2 0.0304(19) 0.035(2) 0.0336(19) 0.0042(16) 0.0070(16) -0.0010(16)
C7 0.0363(19) 0.030(2) 0.0315(18) -0.0027(15) 0.0102(16) 0.0015(16)
C19 0.035(2) 0.041(2) 0.0296(19) 0.0008(16) 0.0049(16) -0.0002(17)
C23 0.071(3) 0.062(4) 0.044(3) -0.001(2) 0.027(3) -0.002(3)
C16 0.0336(19) 0.038(2) 0.0321(19) -0.0009(16) 0.0067(16) -0.0023(16)
C4 0.045(2) 0.051(3) 0.037(2) 0.0100(19) 0.0035(19) 0.002(2)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 F6 1.867(3) . ?
Nb1 F4 1.876(2) . ?
Nb1 F3 1.875(3) . ?
Nb1 F5 1.880(3) . ?
Nb1 F2 1.884(2) . ?
Nb1 F1 1.891(3) . ?
N1 C2 1.314(5) . ?
N1 C5 1.377(5) . ?
N1 C6 1.481(5) . ?
C21 C20 1.517(5) . ?
C21 C22 1.520(6) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C9 C10 1.521(6) . ?
C9 C8 1.532(5) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C18 C19 1.515(5) . ?
C18 C17 1.528(5) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C17 C16 1.534(5) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C6 C7 1.517(5) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C13 C14 1.526(5) . ?
C13 C12 1.535(5) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
N3 C2 1.339(5) . ?
N3 C4 1.363(6) . ?
N3 C24 1.462(5) . ?
C22 C23 1.521(6) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C12 C11 1.519(5) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C10 C11 1.518(5) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C15 C16 1.530(5) . ?
C15 C14 1.531(5) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C8 C7 1.516(6) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C5 C4 1.328(7) . ?
C5 H5 0.9300 . ?
C20 C19 1.520(5) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C2 H2 0.9300 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C4 H4 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F6 Nb1 F4 92.68(13) . . ?
F6 Nb1 F3 91.01(14) . . ?
F4 Nb1 F3 88.34(12) . . ?
F6 Nb1 F5 90.51(13) . . ?
F4 Nb1 F5 90.52(12) . . ?
F3 Nb1 F5 178.15(12) . . ?
F6 Nb1 F2 90.51(14) . . ?
F4 Nb1 F2 176.51(13) . . ?
F3 Nb1 F2 90.19(13) . . ?
F5 Nb1 F2 90.86(13) . . ?
F6 Nb1 F1 178.64(12) . . ?
F4 Nb1 F1 88.68(13) . . ?
F3 Nb1 F1 89.13(14) . . ?
F5 Nb1 F1 89.38(13) . . ?
F2 Nb1 F1 88.13(14) . . ?
C2 N1 C5 108.3(4) . . ?
C2 N1 C6 126.4(4) . . ?
C5 N1 C6 125.3(4) . . ?
C20 C21 C22 113.9(4) . . ?
C20 C21 H21A 108.8 . . ?
C22 C21 H21A 108.8 . . ?
C20 C21 H21B 108.8 . . ?
C22 C21 H21B 108.8 . . ?
H21A C21 H21B 107.7 . . ?
C10 C9 C8 115.2(4) . . ?
C10 C9 H9A 108.5 . . ?
C8 C9 H9A 108.5 . . ?
C10 C9 H9B 108.5 . . ?
C8 C9 H9B 108.5 . . ?
H9A C9 H9B 107.5 . . ?
C19 C18 C17 113.3(4) . . ?
C19 C18 H18A 108.9 . . ?
C17 C18 H18A 108.9 . . ?
C19 C18 H18B 108.9 . . ?
C17 C18 H18B 108.9 . . ?
H18A C18 H18B 107.7 . . ?
C18 C17 C16 112.4(4) . . ?
C18 C17 H17A 109.1 . . ?
C16 C17 H17A 109.1 . . ?
C18 C17 H17B 109.1 . . ?
C16 C17 H17B 109.1 . . ?
H17A C17 H17B 107.9 . . ?
N1 C6 C7 111.9(3) . . ?
N1 C6 H6A 109.2 . . ?
C7 C6 H6A 109.2 . . ?
N1 C6 H6B 109.2 . . ?
C7 C6 H6B 109.2 . . ?
H6A C6 H6B 107.9 . . ?
C14 C13 C12 113.7(4) . . ?
C14 C13 H13A 108.8 . . ?
C12 C13 H13A 108.8 . . ?
C14 C13 H13B 108.8 . . ?
C12 C13 H13B 108.8 . . ?
H13A C13 H13B 107.7 . . ?
C2 N3 C4 107.8(4) . . ?
C2 N3 C24 126.3(4) . . ?
C4 N3 C24 125.8(4) . . ?
C21 C22 C23 113.7(4) . . ?
C21 C22 H22A 108.8 . . ?
C23 C22 H22A 108.8 . . ?
C21 C22 H22B 108.8 . . ?
C23 C22 H22B 108.8 . . ?
H22A C22 H22B 107.7 . . ?
C11 C12 C13 112.6(3) . . ?
C11 C12 H12A 109.1 . . ?
C13 C12 H12A 109.1 . . ?
C11 C12 H12B 109.1 . . ?
C13 C12 H12B 109.1 . . ?
H12A C12 H12B 107.8 . . ?
C11 C10 C9 112.7(4) . . ?
C11 C10 H10A 109.1 . . ?
C9 C10 H10A 109.1 . . ?
C11 C10 H10B 109.1 . . ?
C9 C10 H10B 109.1 . . ?
H10A C10 H10B 107.8 . . ?
C16 C15 C14 113.3(4) . . ?
C16 C15 H15A 108.9 . . ?
C14 C15 H15A 108.9 . . ?
C16 C15 H15B 108.9 . . ?
C14 C15 H15B 108.9 . . ?
H15A C15 H15B 107.7 . . ?
C7 C8 C9 114.1(3) . . ?
C7 C8 H8A 108.7 . . ?
C9 C8 H8A 108.7 . . ?
C7 C8 H8B 108.7 . . ?
C9 C8 H8B 108.7 . . ?
H8A C8 H8B 107.6 . . ?
N3 C24 H24A 109.5 . . ?
N3 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N3 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C4 C5 N1 107.2(4) . . ?
C4 C5 H5 126.4 . . ?
N1 C5 H5 126.4 . . ?
C21 C20 C19 114.3(4) . . ?
C21 C20 H20A 108.7 . . ?
C19 C20 H20A 108.7 . . ?
C21 C20 H20B 108.7 . . ?
C19 C20 H20B 108.7 . . ?
H20A C20 H20B 107.6 . . ?
C13 C14 C15 112.2(4) . . ?
C13 C14 H14A 109.2 . . ?
C15 C14 H14A 109.2 . . ?
C13 C14 H14B 109.2 . . ?
C15 C14 H14B 109.2 . . ?
H14A C14 H14B 107.9 . . ?
C10 C11 C12 115.6(4) . . ?
C10 C11 H11A 108.4 . . ?
C12 C11 H11A 108.4 . . ?
C10 C11 H11B 108.4 . . ?
C12 C11 H11B 108.4 . . ?
H11A C11 H11B 107.4 . . ?
N1 C2 N3 108.7(4) . . ?
N1 C2 H2 125.6 . . ?
N3 C2 H2 125.6 . . ?
C8 C7 C6 112.8(3) . . ?
C8 C7 H7A 109.0 . . ?
C6 C7 H7A 109.0 . . ?
C8 C7 H7B 109.0 . . ?
C6 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
C18 C19 C20 114.0(4) . . ?
C18 C19 H19A 108.7 . . ?
C20 C19 H19A 108.7 . . ?
C18 C19 H19B 108.7 . . ?
C20 C19 H19B 108.7 . . ?
H19A C19 H19B 107.6 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C15 C16 C17 112.3(4) . . ?
C15 C16 H16A 109.1 . . ?
C17 C16 H16A 109.1 . . ?
C15 C16 H16B 109.1 . . ?
C17 C16 H16B 109.1 . . ?
H16A C16 H16B 107.9 . . ?
C5 C4 N3 108.0(4) . . ?
C5 C4 H4 126.0 . . ?
N3 C4 H4 126.0 . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.118

#=END

data_C18MImTaF6--100oC
#TrackingRef '- SI--100oC.cif'

_database_code_depnum_ccdc_archive 'CCDC 843151'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            C18MImTaF6
_chemical_melting_point          347.0
_chemical_formula_moiety         
;
(C22 N2 H43 +), (Ta F6 -)
;
_chemical_formula_sum            'C22 H43 F6 N2 Ta'
_chemical_formula_weight         630.53

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/a

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x-1/2, -y-1/2, z'

_cell_length_a                   9.2100(3)
_cell_length_b                   10.1744(3)
_cell_length_c                   28.4495(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.1688(11)
_cell_angle_gamma                90.00
_cell_volume                     2650.46(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    173
_cell_measurement_reflns_used    20105
_cell_measurement_theta_min      6.04
_cell_measurement_theta_max      54.96

_exptl_crystal_description       platelet
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1264
_exptl_absorpt_coefficient_mu    4.188
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5857
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'RAPID AUTO 2.40 (Rigaku 2006)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS RapidII'
_diffrn_measurement_method       'imaging plate'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11776
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         24.00
_reflns_number_total             3944
_reflns_number_gt                3478
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Rigaku R-AXIS Rapid-II'
_computing_cell_refinement       'RAPID AUTO 2.40 (Rigaku 2006)'
_computing_data_reduction        'RAPID AUTO 2.40 (Rigaku 2006)'
_computing_structure_solution    'SIR92 (Altmare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1044P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3944
_refine_ls_number_parameters     282
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0349
_refine_ls_wR_factor_ref         0.1380
_refine_ls_wR_factor_gt          0.1100
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ta1 Ta -0.14132(3) 0.01638(3) 0.106412(9) 0.03321(17) Uani 1 1 d . . .
F4 F -0.2201(5) -0.0652(4) 0.15738(15) 0.0496(10) Uani 1 1 d . . .
F3 F -0.2994(5) 0.1345(4) 0.10099(18) 0.0564(12) Uani 1 1 d . . .
F2 F -0.0699(5) 0.0947(5) 0.05308(16) 0.0614(13) Uani 1 1 d . . .
F5 F 0.0126(5) -0.1075(4) 0.11135(17) 0.0523(11) Uani 1 1 d . . .
N1 N 0.3928(7) 0.0030(5) 0.1194(2) 0.0323(14) Uani 1 1 d . . .
F6 F -0.0292(5) 0.1323(4) 0.14675(17) 0.0521(11) Uani 1 1 d . . .
F1 F -0.2527(4) -0.0994(5) 0.06445(16) 0.0551(12) Uani 1 1 d . . .
C21 C -0.6693(7) -0.1479(6) 0.6685(2) 0.0334(14) Uani 1 1 d . . .
H21A H -0.7582 -0.1338 0.6476 0.040 Uiso 1 1 calc R . .
H21B H -0.6558 -0.2420 0.6723 0.040 Uiso 1 1 calc R . .
C9 C 0.1610(7) -0.1683(7) 0.2332(2) 0.0395(16) Uani 1 1 d . . .
H9A H 0.0721 -0.1371 0.2153 0.047 Uiso 1 1 calc R . .
H9B H 0.1541 -0.2632 0.2351 0.047 Uiso 1 1 calc R . .
C18 C -0.3944(7) -0.0955(7) 0.5743(2) 0.0362(14) Uani 1 1 d . . .
H18A H -0.3047 -0.1084 0.5950 0.043 Uiso 1 1 calc R . .
H18B H -0.4096 -0.0016 0.5705 0.043 Uiso 1 1 calc R . .
C17 C -0.3761(7) -0.1548(7) 0.5264(2) 0.0373(15) Uani 1 1 d . . .
H17A H -0.3630 -0.2489 0.5301 0.045 Uiso 1 1 calc R . .
H17B H -0.4651 -0.1403 0.5056 0.045 Uiso 1 1 calc R . .
C6 C 0.4314(9) 0.0422(8) 0.1690(3) 0.0414(17) Uani 1 1 d . . .
H6A H 0.4518 0.1358 0.1701 0.050 Uiso 1 1 calc R . .
H6B H 0.5200 -0.0033 0.1813 0.050 Uiso 1 1 calc R . .
C13 C -0.0890(7) -0.1595(7) 0.3829(2) 0.0375(15) Uani 1 1 d . . .
H13A H -0.0752 -0.2536 0.3867 0.045 Uiso 1 1 calc R . .
H13B H -0.1794 -0.1458 0.3627 0.045 Uiso 1 1 calc R . .
N3 N 0.3855(6) -0.1015(6) 0.05272(19) 0.0381(13) Uani 1 1 d . . .
C22 C -0.6880(8) -0.0883(9) 0.7162(3) 0.051(2) Uani 1 1 d . . .
H22A H -0.6983 0.0062 0.7126 0.061 Uiso 1 1 calc R . .
H22B H -0.6004 -0.1049 0.7375 0.061 Uiso 1 1 calc R . .
C12 C 0.0358(7) -0.1044(8) 0.3584(2) 0.0392(16) Uani 1 1 d . . .
H12A H 0.1273 -0.1220 0.3776 0.047 Uiso 1 1 calc R . .
H12B H 0.0249 -0.0098 0.3555 0.047 Uiso 1 1 calc R . .
C10 C 0.1668(7) -0.1132(7) 0.2829(2) 0.0370(15) Uani 1 1 d . . .
H10A H 0.1623 -0.0180 0.2813 0.044 Uiso 1 1 calc R . .
H10B H 0.2591 -0.1372 0.3005 0.044 Uiso 1 1 calc R . .
C15 C -0.2299(7) -0.1554(6) 0.4552(2) 0.0330(14) Uani 1 1 d . . .
H15A H -0.3197 -0.1411 0.4347 0.040 Uiso 1 1 calc R . .
H15B H -0.2163 -0.2496 0.4584 0.040 Uiso 1 1 calc R . .
C8 C 0.2894(7) -0.1342(7) 0.2058(2) 0.0368(15) Uani 1 1 d . . .
H8A H 0.2730 -0.1741 0.1747 0.044 Uiso 1 1 calc R . .
H8B H 0.3772 -0.1730 0.2219 0.044 Uiso 1 1 calc R . .
C24 C 0.4268(9) -0.1901(7) 0.0162(3) 0.0448(18) Uani 1 1 d . . .
H24A H 0.3431 -0.2399 0.0035 0.067 Uiso 1 1 calc R . .
H24B H 0.5016 -0.2489 0.0297 0.067 Uiso 1 1 calc R . .
H24C H 0.4631 -0.1399 -0.0086 0.067 Uiso 1 1 calc R . .
C5 C 0.2907(8) 0.0637(8) 0.0884(3) 0.0431(17) Uani 1 1 d . . .
H5 H 0.2353 0.1370 0.0945 0.052 Uiso 1 1 calc R . .
C20 C -0.5405(7) -0.0915(7) 0.6454(2) 0.0380(15) Uani 1 1 d . . .
H20A H -0.5548 0.0023 0.6411 0.046 Uiso 1 1 calc R . .
H20B H -0.4518 -0.1043 0.6665 0.046 Uiso 1 1 calc R . .
C14 C -0.1049(7) -0.1002(6) 0.4310(2) 0.0353(14) Uani 1 1 d . . .
H14A H -0.0147 -0.1142 0.4513 0.042 Uiso 1 1 calc R . .
H14B H -0.1186 -0.0061 0.4273 0.042 Uiso 1 1 calc R . .
C11 C 0.0415(7) -0.1636(7) 0.3094(2) 0.0368(15) Uani 1 1 d . . .
H11A H -0.0502 -0.1452 0.2905 0.044 Uiso 1 1 calc R . .
H11B H 0.0503 -0.2582 0.3126 0.044 Uiso 1 1 calc R . .
C2 C 0.4508(7) -0.0956(7) 0.0971(2) 0.0346(14) Uani 1 1 d . . .
H2 H 0.5245 -0.1512 0.1101 0.041 Uiso 1 1 calc R . .
C7 C 0.3160(8) 0.0136(6) 0.1997(3) 0.0322(15) Uani 1 1 d . . .
H7A H 0.2258 0.0545 0.1863 0.039 Uiso 1 1 calc R . .
H7B H 0.3428 0.0524 0.2305 0.039 Uiso 1 1 calc R . .
C19 C -0.5202(7) -0.1532(7) 0.5977(2) 0.0363(15) Uani 1 1 d . . .
H19A H -0.5039 -0.2468 0.6021 0.044 Uiso 1 1 calc R . .
H19B H -0.6095 -0.1420 0.5767 0.044 Uiso 1 1 calc R . .
C23 C -0.8186(10) -0.1412(9) 0.7384(3) 0.060(2) Uani 1 1 d . . .
H23A H -0.9056 -0.1277 0.7172 0.090 Uiso 1 1 calc R . .
H23B H -0.8273 -0.0961 0.7676 0.090 Uiso 1 1 calc R . .
H23C H -0.8056 -0.2335 0.7445 0.090 Uiso 1 1 calc R . .
C16 C -0.2489(7) -0.0996(7) 0.5032(2) 0.0370(15) Uani 1 1 d . . .
H16A H -0.2613 -0.0052 0.5002 0.044 Uiso 1 1 calc R . .
H16B H -0.1600 -0.1153 0.5239 0.044 Uiso 1 1 calc R . .
C4 C 0.2855(10) -0.0032(7) 0.0472(3) 0.044(2) Uani 1 1 d . . .
H4 H 0.2241 0.0151 0.0198 0.053 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ta1 0.0360(2) 0.0340(2) 0.0304(2) 0.00222(10) 0.00657(15) 0.00052(10)
F4 0.063(3) 0.045(2) 0.043(2) 0.010(2) 0.016(2) 0.004(2)
F3 0.049(2) 0.047(3) 0.075(3) 0.014(2) 0.013(2) 0.006(2)
F2 0.054(2) 0.089(4) 0.044(3) 0.023(3) 0.0154(19) -0.008(3)
F5 0.051(2) 0.046(3) 0.060(3) -0.001(2) 0.006(2) 0.004(2)
N1 0.033(3) 0.036(3) 0.029(3) 0.003(2) 0.007(3) -0.010(2)
F6 0.054(2) 0.041(2) 0.061(3) -0.014(2) 0.005(2) -0.018(2)
F1 0.044(2) 0.069(3) 0.054(3) -0.020(2) 0.0132(19) -0.015(2)
C21 0.034(3) 0.028(3) 0.039(4) -0.003(3) 0.009(3) -0.001(3)
C9 0.046(4) 0.041(4) 0.034(4) -0.001(3) 0.016(3) -0.008(3)
C18 0.043(3) 0.031(3) 0.035(4) -0.001(3) 0.005(3) -0.003(3)
C17 0.035(3) 0.047(4) 0.031(4) -0.002(3) 0.006(3) -0.004(3)
C6 0.045(4) 0.050(4) 0.030(4) -0.003(3) 0.009(3) -0.002(4)
C13 0.037(3) 0.046(4) 0.031(4) 0.002(3) 0.012(3) 0.001(3)
N3 0.045(3) 0.041(3) 0.029(3) 0.002(3) 0.009(2) -0.011(3)
C22 0.047(4) 0.075(6) 0.031(4) -0.005(4) 0.013(3) -0.009(4)
C12 0.039(3) 0.048(4) 0.031(4) 0.004(3) 0.008(3) 0.002(3)
C10 0.035(3) 0.041(4) 0.035(4) 0.003(3) 0.008(3) 0.002(3)
C15 0.035(3) 0.030(3) 0.035(4) 0.000(3) 0.010(3) 0.000(3)
C8 0.044(4) 0.036(4) 0.032(4) 0.004(3) 0.013(3) 0.009(3)
C24 0.058(4) 0.041(4) 0.036(4) -0.002(3) 0.011(3) -0.004(4)
C5 0.052(4) 0.042(4) 0.037(4) 0.004(3) 0.008(3) -0.003(4)
C20 0.040(3) 0.041(4) 0.032(4) -0.002(3) 0.000(3) -0.003(3)
C14 0.039(3) 0.030(3) 0.036(4) 0.006(3) 0.005(3) 0.000(3)
C11 0.037(3) 0.040(4) 0.036(4) 0.000(3) 0.012(3) -0.009(3)
C2 0.039(3) 0.040(4) 0.026(3) 0.000(3) 0.008(3) -0.006(3)
C7 0.037(4) 0.029(3) 0.031(4) -0.007(3) 0.005(3) -0.004(3)
C19 0.039(3) 0.045(4) 0.027(3) 0.000(3) 0.008(3) 0.001(3)
C23 0.081(6) 0.058(5) 0.047(5) 0.004(4) 0.032(4) -0.001(5)
C16 0.038(3) 0.043(4) 0.032(4) 0.002(3) 0.010(3) -0.004(3)
C4 0.043(5) 0.046(4) 0.041(5) 0.016(3) -0.002(4) 0.012(3)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ta1 F6 1.876(4) . ?
Ta1 F3 1.882(4) . ?
Ta1 F4 1.882(4) . ?
Ta1 F5 1.891(4) . ?
Ta1 F2 1.893(4) . ?
Ta1 F1 1.898(4) . ?
N1 C2 1.330(9) . ?
N1 C5 1.366(10) . ?
N1 C6 1.473(10) . ?
C21 C22 1.512(10) . ?
C21 C20 1.530(9) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C9 C10 1.517(9) . ?
C9 C8 1.526(9) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C18 C19 1.516(9) . ?
C18 C17 1.516(9) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C17 C16 1.512(9) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C6 C7 1.475(11) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C13 C12 1.515(9) . ?
C13 C14 1.516(9) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
N3 C2 1.339(8) . ?
N3 C4 1.358(10) . ?
N3 C24 1.456(9) . ?
C22 C23 1.517(11) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C12 C11 1.523(9) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C10 C11 1.533(9) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C15 C16 1.506(9) . ?
C15 C14 1.512(9) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C8 C7 1.536(9) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C5 C4 1.352(12) . ?
C5 H5 0.9300 . ?
C20 C19 1.524(9) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C2 H2 0.9300 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C4 H4 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F6 Ta1 F3 91.1(2) . . ?
F6 Ta1 F4 92.2(2) . . ?
F3 Ta1 F4 89.2(2) . . ?
F6 Ta1 F5 90.9(2) . . ?
F3 Ta1 F5 177.87(19) . . ?
F4 Ta1 F5 89.8(2) . . ?
F6 Ta1 F2 90.6(2) . . ?
F3 Ta1 F2 89.9(2) . . ?
F4 Ta1 F2 177.10(19) . . ?
F5 Ta1 F2 91.0(2) . . ?
F6 Ta1 F1 178.73(19) . . ?
F3 Ta1 F1 89.1(2) . . ?
F4 Ta1 F1 89.1(2) . . ?
F5 Ta1 F1 89.03(19) . . ?
F2 Ta1 F1 88.2(2) . . ?
C2 N1 C5 108.4(7) . . ?
C2 N1 C6 126.5(7) . . ?
C5 N1 C6 125.1(7) . . ?
C22 C21 C20 113.9(6) . . ?
C22 C21 H21A 108.8 . . ?
C20 C21 H21A 108.8 . . ?
C22 C21 H21B 108.8 . . ?
C20 C21 H21B 108.8 . . ?
H21A C21 H21B 107.7 . . ?
C10 C9 C8 116.2(6) . . ?
C10 C9 H9A 108.2 . . ?
C8 C9 H9A 108.2 . . ?
C10 C9 H9B 108.2 . . ?
C8 C9 H9B 108.2 . . ?
H9A C9 H9B 107.4 . . ?
C19 C18 C17 113.9(5) . . ?
C19 C18 H18A 108.8 . . ?
C17 C18 H18A 108.8 . . ?
C19 C18 H18B 108.8 . . ?
C17 C18 H18B 108.8 . . ?
H18A C18 H18B 107.7 . . ?
C16 C17 C18 114.2(6) . . ?
C16 C17 H17A 108.7 . . ?
C18 C17 H17A 108.7 . . ?
C16 C17 H17B 108.7 . . ?
C18 C17 H17B 108.7 . . ?
H17A C17 H17B 107.6 . . ?
N1 C6 C7 113.4(7) . . ?
N1 C6 H6A 108.9 . . ?
C7 C6 H6A 108.9 . . ?
N1 C6 H6B 108.9 . . ?
C7 C6 H6B 108.9 . . ?
H6A C6 H6B 107.7 . . ?
C12 C13 C14 114.8(6) . . ?
C12 C13 H13A 108.6 . . ?
C14 C13 H13A 108.6 . . ?
C12 C13 H13B 108.6 . . ?
C14 C13 H13B 108.6 . . ?
H13A C13 H13B 107.5 . . ?
C2 N3 C4 107.9(6) . . ?
C2 N3 C24 125.0(6) . . ?
C4 N3 C24 126.8(6) . . ?
C21 C22 C23 113.7(7) . . ?
C21 C22 H22A 108.8 . . ?
C23 C22 H22A 108.8 . . ?
C21 C22 H22B 108.8 . . ?
C23 C22 H22B 108.8 . . ?
H22A C22 H22B 107.7 . . ?
C13 C12 C11 112.2(6) . . ?
C13 C12 H12A 109.2 . . ?
C11 C12 H12A 109.2 . . ?
C13 C12 H12B 109.2 . . ?
C11 C12 H12B 109.2 . . ?
H12A C12 H12B 107.9 . . ?
C9 C10 C11 112.5(6) . . ?
C9 C10 H10A 109.1 . . ?
C11 C10 H10A 109.1 . . ?
C9 C10 H10B 109.1 . . ?
C11 C10 H10B 109.1 . . ?
H10A C10 H10B 107.8 . . ?
C16 C15 C14 116.2(5) . . ?
C16 C15 H15A 108.2 . . ?
C14 C15 H15A 108.2 . . ?
C16 C15 H15B 108.2 . . ?
C14 C15 H15B 108.2 . . ?
H15A C15 H15B 107.4 . . ?
C9 C8 C7 115.0(6) . . ?
C9 C8 H8A 108.5 . . ?
C7 C8 H8A 108.5 . . ?
C9 C8 H8B 108.5 . . ?
C7 C8 H8B 108.5 . . ?
H8A C8 H8B 107.5 . . ?
N3 C24 H24A 109.5 . . ?
N3 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N3 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C4 C5 N1 106.9(7) . . ?
C4 C5 H5 126.5 . . ?
N1 C5 H5 126.5 . . ?
C19 C20 C21 113.8(6) . . ?
C19 C20 H20A 108.8 . . ?
C21 C20 H20A 108.8 . . ?
C19 C20 H20B 108.8 . . ?
C21 C20 H20B 108.8 . . ?
H20A C20 H20B 107.7 . . ?
C15 C14 C13 114.5(5) . . ?
C15 C14 H14A 108.6 . . ?
C13 C14 H14A 108.6 . . ?
C15 C14 H14B 108.6 . . ?
C13 C14 H14B 108.6 . . ?
H14A C14 H14B 107.6 . . ?
C12 C11 C10 114.8(5) . . ?
C12 C11 H11A 108.6 . . ?
C10 C11 H11A 108.6 . . ?
C12 C11 H11B 108.6 . . ?
C10 C11 H11B 108.6 . . ?
H11A C11 H11B 107.5 . . ?
N1 C2 N3 108.8(6) . . ?
N1 C2 H2 125.6 . . ?
N3 C2 H2 125.6 . . ?
C6 C7 C8 113.2(6) . . ?
C6 C7 H7A 108.9 . . ?
C8 C7 H7A 108.9 . . ?
C6 C7 H7B 108.9 . . ?
C8 C7 H7B 108.9 . . ?
H7A C7 H7B 107.7 . . ?
C18 C19 C20 113.8(6) . . ?
C18 C19 H19A 108.8 . . ?
C20 C19 H19A 108.8 . . ?
C18 C19 H19B 108.8 . . ?
C20 C19 H19B 108.8 . . ?
H19A C19 H19B 107.7 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C15 C16 C17 115.2(6) . . ?
C15 C16 H16A 108.5 . . ?
C17 C16 H16A 108.5 . . ?
C15 C16 H16B 108.5 . . ?
C17 C16 H16B 108.5 . . ?
H16A C16 H16B 107.5 . . ?
C5 C4 N3 108.0(7) . . ?
C5 C4 H4 126.0 . . ?
N3 C4 H4 126.0 . . ?

_diffrn_measured_fraction_theta_max 0.945
_diffrn_reflns_theta_full        24.00
_diffrn_measured_fraction_theta_full 0.945
_refine_diff_density_max         1.629
_refine_diff_density_min         -1.412
_refine_diff_density_rms         0.215