#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:23:40 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180391 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/60/7206027.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7206027
loop_
_publ_author_name
'Gelmboldt, Vladimir O.'
'Ganin, Eduard V.'
'Basok, Stepan S.'
'Kulygina, Ekaterina Yu.'
'Botoshansky, Mark M.'
'Kravtsov, Victor Ch.'
'Fonari, Marina S.'
_publ_section_title
;
 Tetrabenzylcyclen as a receptor for fluoride
;
_journal_issue                   11
_journal_name_full               CrystEngComm
_journal_page_first              3682
_journal_paper_doi               10.1039/c1ce05279a
_journal_volume                  13
_journal_year                    2011
_chemical_formula_moiety         'C36 H47 N4, F, Si F6, 4(H2 O)'
_chemical_formula_sum            'C36 H55 F7 N4 O4 Si'
_chemical_formula_weight         768.93
_chemical_name_common
;
1,4,7,10-tetrabenzyl-1,4,7,-triazonia-10-azacyclododecane
fluoride hexafluorosilicate tetrahydrate
;
_chemical_name_systematic
;
1,4,7,10-tetrabenzyl-1,4,7,-triazonia-10-azacyclododecane
fluoride hexafluorosilicate tetrahydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.044(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   37.0414(14)
_cell_length_b                   11.1521(4)
_cell_length_c                   19.2636(7)
_cell_measurement_reflns_used    4313
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.8608
_cell_measurement_theta_min      2.9340
_cell_volume                     7835.6(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0715
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            13831
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    0.136
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83007
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3264
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.223
_refine_diff_density_rms         0.034
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.841
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     519
_refine_ls_number_reflns         7297
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      0.867
_refine_ls_R_factor_all          0.0950
_refine_ls_R_factor_gt           0.0399
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0405P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0809
_refine_ls_wR_factor_ref         0.0896
_reflns_number_gt                3577
_reflns_number_total             7297
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1ce05279a.txt
_cod_data_source_block           vo9n
_cod_database_code               7206027
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
Si1 Si 0.461613(15) 0.75363(5) 0.52728(3) 0.03597(15) Uani 1 1 d . . .
F1 F 0.48635(3) 0.63849(10) 0.50589(8) 0.0688(4) Uani 1 1 d . . .
F2 F 0.43688(3) 0.86853(11) 0.54869(7) 0.0671(4) Uani 1 1 d . . .
F3 F 0.43581(3) 0.75067(10) 0.44637(6) 0.0597(4) Uani 1 1 d . . .
F4 F 0.48776(3) 0.75919(10) 0.60756(6) 0.0581(4) Uani 1 1 d . . .
F5 F 0.49045(3) 0.85005(10) 0.49849(7) 0.0608(4) Uani 1 1 d . . .
F6 F 0.43336(3) 0.65648(11) 0.55626(7) 0.0650(4) Uani 1 1 d . . .
F7 F 0.63427(3) 0.74541(9) 0.67006(6) 0.0448(3) Uani 1 1 d . . .
N1 N 0.58368(4) 0.91671(14) 0.74083(9) 0.0422(5) Uani 1 1 d . . .
N2 N 0.59902(5) 0.91825(15) 0.59361(10) 0.0397(5) Uani 1 1 d . . .
H2N H 0.6111(5) 0.8640(16) 0.6306(11) 0.049(6) Uiso 1 1 d . . .
N3 N 0.59409(5) 0.63333(15) 0.57331(10) 0.0395(5) Uani 1 1 d . . .
H3N H 0.6126(5) 0.6723(16) 0.6080(11) 0.043(6) Uiso 1 1 d . . .
N4 N 0.58450(5) 0.64536(16) 0.73487(10) 0.0419(5) Uani 1 1 d . . .
H1N H 0.6013(6) 0.6922(16) 0.7175(11) 0.048(7) Uiso 1 1 d . . .
C1 C 0.57083(6) 1.01127(18) 0.68980(12) 0.0488(6) Uani 1 1 d . . .
H1A H 0.5887 1.0756 0.6950 0.059 Uiso 1 1 calc R . .
H1B H 0.5480 1.0438 0.6999 0.059 Uiso 1 1 calc R . .
C2 C 0.56476(5) 0.96670(18) 0.61467(12) 0.0442(6) Uani 1 1 d . . .
H2A H 0.5463 0.9042 0.6091 0.053 Uiso 1 1 calc R . .
H2B H 0.5555 1.0321 0.5834 0.053 Uiso 1 1 calc R . .
C3 C 0.59034(6) 0.84480(18) 0.52716(11) 0.0451(6) Uani 1 1 d . . .
H3A H 0.5758 0.8934 0.4909 0.054 Uiso 1 1 calc R . .
H3B H 0.6131 0.8258 0.5113 0.054 Uiso 1 1 calc R . .
C4 C 0.57008(6) 0.72968(17) 0.53421(12) 0.0453(6) Uani 1 1 d . . .
H4A H 0.5598 0.7004 0.4875 0.054 Uiso 1 1 calc R . .
H4B H 0.5499 0.7458 0.5589 0.054 Uiso 1 1 calc R . .
C5 C 0.57318(6) 0.54884(18) 0.61211(12) 0.0471(6) Uani 1 1 d . . .
H5A H 0.5893 0.4834 0.6304 0.057 Uiso 1 1 calc R . .
H5B H 0.5532 0.5149 0.5786 0.057 Uiso 1 1 calc R . .
C6 C 0.55745(6) 0.60265(19) 0.67251(12) 0.0470(6) Uani 1 1 d . . .
H6A H 0.5420 0.6699 0.6544 0.056 Uiso 1 1 calc R . .
H6B H 0.5418 0.5432 0.6889 0.056 Uiso 1 1 calc R . .
C7 C 0.56524(6) 0.71947(18) 0.78279(12) 0.0513(6) Uani 1 1 d . . .
H7A H 0.5439 0.6756 0.7920 0.062 Uiso 1 1 calc R . .
H7B H 0.5816 0.7303 0.8275 0.062 Uiso 1 1 calc R . .
C8 C 0.55309(6) 0.84058(18) 0.75337(12) 0.0464(6) Uani 1 1 d . . .
H8A H 0.5362 0.8299 0.7093 0.056 Uiso 1 1 calc R . .
H8B H 0.5400 0.8811 0.7860 0.056 Uiso 1 1 calc R . .
C9 C 0.60256(6) 0.9686(2) 0.80816(12) 0.0606(7) Uani 1 1 d . . .
H9A H 0.6083 0.9047 0.8425 0.073 Uiso 1 1 calc R . .
H9B H 0.5860 1.0237 0.8258 0.073 Uiso 1 1 calc R . .
C10 C 0.63714(7) 1.0337(2) 0.80149(13) 0.0569(7) Uani 1 1 d . . .
C11 C 0.66600(7) 0.9736(3) 0.77967(13) 0.0708(8) Uani 1 1 d . . .
H11 H 0.6638 0.8923 0.7691 0.085 Uiso 1 1 calc R . .
C12 C 0.69770(8) 1.0330(3) 0.77348(15) 0.0873(9) Uani 1 1 d . . .
H12 H 0.7168 0.9913 0.7589 0.105 Uiso 1 1 calc R . .
C13 C 0.70156(10) 1.1504(4) 0.78822(19) 0.1017(11) Uani 1 1 d . . .
H13 H 0.7232 1.1894 0.7833 0.122 Uiso 1 1 calc R . .
C14 C 0.67399(11) 1.2129(3) 0.8105(2) 0.1031(12) Uani 1 1 d . . .
H14 H 0.6769 1.2940 0.8214 0.124 Uiso 1 1 calc R . .
C15 C 0.64134(8) 1.1536(3) 0.81662(16) 0.0866(9) Uani 1 1 d . . .
H15 H 0.6223 1.1960 0.8311 0.104 Uiso 1 1 calc R . .
C16 C 0.62481(6) 1.02023(18) 0.58504(13) 0.0539(6) Uani 1 1 d . . .
H16A H 0.6118 1.0776 0.5519 0.065 Uiso 1 1 calc R . .
H16B H 0.6314 1.0606 0.6301 0.065 Uiso 1 1 calc R . .
C17 C 0.65937(6) 0.98413(19) 0.55987(13) 0.0487(6) Uani 1 1 d . . .
C18 C 0.66713(8) 1.0300(3) 0.49761(14) 0.0787(8) Uani 1 1 d . . .
H18 H 0.6503 1.0799 0.4701 0.094 Uiso 1 1 calc R . .
C19 C 0.69975(10) 1.0023(3) 0.47580(17) 0.1003(11) Uani 1 1 d . . .
H19 H 0.7046 1.0335 0.4336 0.120 Uiso 1 1 calc R . .
C20 C 0.72487(9) 0.9299(3) 0.51537(19) 0.0934(10) Uani 1 1 d . . .
H20 H 0.7468 0.9122 0.5005 0.112 Uiso 1 1 calc R . .
C21 C 0.71768(7) 0.8838(2) 0.57652(18) 0.0773(8) Uani 1 1 d . . .
H21 H 0.7347 0.8336 0.6034 0.093 Uiso 1 1 calc R . .
C22 C 0.68539(6) 0.9106(2) 0.59937(14) 0.0608(7) Uani 1 1 d . . .
H22 H 0.6810 0.8790 0.6418 0.073 Uiso 1 1 calc R . .
C23 C 0.61397(6) 0.56408(19) 0.52389(12) 0.0482(6) Uani 1 1 d . . .
H23A H 0.5974 0.5056 0.4983 0.058 Uiso 1 1 calc R . .
H23B H 0.6213 0.6189 0.4898 0.058 Uiso 1 1 calc R . .
C24 C 0.64739(6) 0.50048(19) 0.56228(12) 0.0433(6) Uani 1 1 d . . .
C25 C 0.68023(6) 0.5610(2) 0.57852(13) 0.0553(7) Uani 1 1 d . . .
H25 H 0.6815 0.6412 0.5658 0.066 Uiso 1 1 calc R . .
C26 C 0.71111(7) 0.5045(3) 0.61316(14) 0.0666(7) Uani 1 1 d . . .
H26 H 0.7331 0.5463 0.6236 0.080 Uiso 1 1 calc R . .
C27 C 0.70953(7) 0.3870(3) 0.63220(14) 0.0727(8) Uani 1 1 d . . .
H27 H 0.7304 0.3488 0.6559 0.087 Uiso 1 1 calc R . .
C28 C 0.67716(8) 0.3257(2) 0.61637(15) 0.0691(8) Uani 1 1 d . . .
H28 H 0.6761 0.2456 0.6295 0.083 Uiso 1 1 calc R . .
C29 C 0.64611(6) 0.3816(2) 0.58115(13) 0.0562(7) Uani 1 1 d . . .
H29 H 0.6243 0.3391 0.5701 0.067 Uiso 1 1 calc R . .
C30 C 0.60481(6) 0.54244(18) 0.77568(13) 0.0577(7) Uani 1 1 d . . .
H30A H 0.5903 0.5124 0.8093 0.069 Uiso 1 1 calc R . .
H30B H 0.6076 0.4779 0.7432 0.069 Uiso 1 1 calc R . .
C31 C 0.64189(6) 0.57802(19) 0.81426(13) 0.0497(6) Uani 1 1 d . . .
C32 C 0.67172(7) 0.5679(2) 0.78061(14) 0.0711(8) Uani 1 1 d . . .
H32 H 0.6686 0.5395 0.7346 0.085 Uiso 1 1 calc R . .
C33 C 0.70606(8) 0.5999(3) 0.81524(19) 0.0919(10) Uani 1 1 d . . .
H33 H 0.7259 0.5943 0.7919 0.110 Uiso 1 1 calc R . .
C34 C 0.71144(8) 0.6396(3) 0.88289(19) 0.0870(9) Uani 1 1 d . . .
H34 H 0.7348 0.6600 0.9060 0.104 Uiso 1 1 calc R . .
C35 C 0.68198(8) 0.6492(2) 0.91673(15) 0.0806(8) Uani 1 1 d . . .
H35 H 0.6853 0.6770 0.9629 0.097 Uiso 1 1 calc R . .
C36 C 0.64757(7) 0.6177(2) 0.88254(14) 0.0643(7) Uani 1 1 d . . .
H36 H 0.6278 0.6236 0.9062 0.077 Uiso 1 1 calc R . .
O1W O 0.52101(5) 0.93348(15) 0.38736(9) 0.0655(5) Uani 1 1 d D . .
H1W1 H 0.5115(7) 0.902(2) 0.4222(12) 0.098 Uiso 1 1 d D . .
H2W1 H 0.5316(7) 0.9982(17) 0.4022(14) 0.098 Uiso 1 1 d D . .
O2W O 0.52253(7) 0.55511(19) 0.39164(15) 0.1282(9) Uani 1 1 d D . .
H1W2 H 0.5293(10) 0.494(3) 0.4185(17) 0.192 Uiso 1 1 d D . .
H2W2 H 0.5358(11) 0.553(4) 0.3553(16) 0.192 Uiso 1 1 d D . .
O3W O 0.55351(12) 0.7414(2) 0.3289(2) 0.194(2) Uani 0.918(5) 1 d PU . .
O3W' O 0.5085(7) 0.7976(19) 0.2711(12) 0.092(11) Uani 0.082(5) 1 d PU . 2
O4W O 0.4304(4) 0.6888(5) 0.3053(3) 0.133(4) Uani 0.638(17) 1 d PD A 1
H1W4 H 0.440(2) 0.723(6) 0.3465(17) 0.199 Uiso 0.638(17) 1 d PD A 1
H2W4 H 0.4423(18) 0.718(6) 0.272(2) 0.199 Uiso 0.638(17) 1 d PD A 1
O4W' O 0.4636(6) 0.6713(6) 0.3297(8) 0.118(5) Uani 0.362(17) 1 d P A 2
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'
O O 0.0106 0.0060 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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 Si1 F6 90.72(7) . . ?
F2 Si1 F1 179.94(10) . . ?
F6 Si1 F1 89.22(7) . . ?
F2 Si1 F4 89.84(7) . . ?
F6 Si1 F4 90.60(7) . . ?
F1 Si1 F4 90.15(7) . . ?
F2 Si1 F5 89.89(7) . . ?
F6 Si1 F5 179.27(8) . . ?
F1 Si1 F5 90.17(7) . . ?
F4 Si1 F5 89.00(7) . . ?
F2 Si1 F3 89.79(7) . . ?
F6 Si1 F3 90.52(7) . . ?
F1 Si1 F3 90.22(7) . . ?
F4 Si1 F3 178.82(7) . . ?
F5 Si1 F3 89.88(7) . . ?
C1 N1 C8 110.91(16) . . ?
C1 N1 C9 110.84(16) . . ?
C8 N1 C9 109.99(17) . . ?
C2 N2 C3 111.16(16) . . ?
C2 N2 C16 109.82(16) . . ?
C3 N2 C16 111.18(17) . . ?
C2 N2 H2N 109.1(12) . . ?
C3 N2 H2N 106.5(11) . . ?
C16 N2 H2N 109.0(11) . . ?
C5 N3 C4 112.66(16) . . ?
C5 N3 C23 110.07(15) . . ?
C4 N3 C23 111.01(17) . . ?
C5 N3 H3N 107.5(11) . . ?
C4 N3 H3N 107.9(10) . . ?
C23 N3 H3N 107.4(11) . . ?
C6 N4 C7 110.04(16) . . ?
C6 N4 C30 112.12(16) . . ?
C7 N4 C30 110.04(17) . . ?
C6 N4 H1N 106.7(13) . . ?
C7 N4 H1N 109.5(12) . . ?
C30 N4 H1N 108.3(12) . . ?
N1 C1 C2 112.54(16) . . ?
N1 C1 H1A 109.1 . . ?
C2 C1 H1A 109.1 . . ?
N1 C1 H1B 109.1 . . ?
C2 C1 H1B 109.1 . . ?
H1A C1 H1B 107.8 . . ?
N2 C2 C1 112.75(17) . . ?
N2 C2 H2A 109.0 . . ?
C1 C2 H2A 109.0 . . ?
N2 C2 H2B 109.0 . . ?
C1 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
C4 C3 N2 115.02(18) . . ?
C4 C3 H3A 108.5 . . ?
N2 C3 H3A 108.5 . . ?
C4 C3 H3B 108.5 . . ?
N2 C3 H3B 108.5 . . ?
H3A C3 H3B 107.5 . . ?
C3 C4 N3 113.11(16) . . ?
C3 C4 H4A 109.0 . . ?
N3 C4 H4A 109.0 . . ?
C3 C4 H4B 109.0 . . ?
N3 C4 H4B 109.0 . . ?
H4A C4 H4B 107.8 . . ?
N3 C5 C6 115.83(17) . . ?
N3 C5 H5A 108.3 . . ?
C6 C5 H5A 108.3 . . ?
N3 C5 H5B 108.3 . . ?
C6 C5 H5B 108.3 . . ?
H5A C5 H5B 107.4 . . ?
N4 C6 C5 116.64(17) . . ?
N4 C6 H6A 108.1 . . ?
C5 C6 H6A 108.1 . . ?
N4 C6 H6B 108.1 . . ?
C5 C6 H6B 108.1 . . ?
H6A C6 H6B 107.3 . . ?
C8 C7 N4 113.84(18) . . ?
C8 C7 H7A 108.8 . . ?
N4 C7 H7A 108.8 . . ?
C8 C7 H7B 108.8 . . ?
N4 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
N1 C8 C7 113.11(17) . . ?
N1 C8 H8A 109.0 . . ?
C7 C8 H8A 109.0 . . ?
N1 C8 H8B 109.0 . . ?
C7 C8 H8B 109.0 . . ?
H8A C8 H8B 107.8 . . ?
N1 C9 C10 113.26(19) . . ?
N1 C9 H9A 108.9 . . ?
C10 C9 H9A 108.9 . . ?
N1 C9 H9B 108.9 . . ?
C10 C9 H9B 108.9 . . ?
H9A C9 H9B 107.7 . . ?
C15 C10 C11 118.0(3) . . ?
C15 C10 C9 121.5(3) . . ?
C11 C10 C9 120.5(2) . . ?
C12 C11 C10 120.6(3) . . ?
C12 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
C13 C12 C11 120.9(3) . . ?
C13 C12 H12 119.5 . . ?
C11 C12 H12 119.5 . . ?
C12 C13 C14 120.4(3) . . ?
C12 C13 H13 119.8 . . ?
C14 C13 H13 119.8 . . ?
C13 C14 C15 119.3(3) . . ?
C13 C14 H14 120.4 . . ?
C15 C14 H14 120.4 . . ?
C10 C15 C14 120.6(3) . . ?
C10 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
C17 C16 N2 115.10(17) . . ?
C17 C16 H16A 108.5 . . ?
N2 C16 H16A 108.5 . . ?
C17 C16 H16B 108.5 . . ?
N2 C16 H16B 108.5 . . ?
H16A C16 H16B 107.5 . . ?
C18 C17 C22 117.8(2) . . ?
C18 C17 C16 120.0(2) . . ?
C22 C17 C16 122.1(2) . . ?
C17 C18 C19 120.5(3) . . ?
C17 C18 H18 119.8 . . ?
C19 C18 H18 119.8 . . ?
C20 C19 C18 120.7(3) . . ?
C20 C19 H19 119.6 . . ?
C18 C19 H19 119.6 . . ?
C21 C20 C19 119.6(3) . . ?
C21 C20 H20 120.2 . . ?
C19 C20 H20 120.2 . . ?
C20 C21 C22 120.6(3) . . ?
C20 C21 H21 119.7 . . ?
C22 C21 H21 119.7 . . ?
C21 C22 C17 120.8(3) . . ?
C21 C22 H22 119.6 . . ?
C17 C22 H22 119.6 . . ?
C24 C23 N3 112.36(17) . . ?
C24 C23 H23A 109.1 . . ?
N3 C23 H23A 109.1 . . ?
C24 C23 H23B 109.1 . . ?
N3 C23 H23B 109.1 . . ?
H23A C23 H23B 107.9 . . ?
C29 C24 C25 118.7(2) . . ?
C29 C24 C23 121.3(2) . . ?
C25 C24 C23 119.9(2) . . ?
C26 C25 C24 120.9(2) . . ?
C26 C25 H25 119.6 . . ?
C24 C25 H25 119.6 . . ?
C27 C26 C25 120.0(2) . . ?
C27 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C26 C27 C28 119.9(2) . . ?
C26 C27 H27 120.1 . . ?
C28 C27 H27 120.1 . . ?
C27 C28 C29 120.4(2) . . ?
C27 C28 H28 119.8 . . ?
C29 C28 H28 119.8 . . ?
C24 C29 C28 120.1(2) . . ?
C24 C29 H29 119.9 . . ?
C28 C29 H29 119.9 . . ?
C31 C30 N4 112.73(17) . . ?
C31 C30 H30A 109.0 . . ?
N4 C30 H30A 109.0 . . ?
C31 C30 H30B 109.0 . . ?
N4 C30 H30B 109.0 . . ?
H30A C30 H30B 107.8 . . ?
C36 C31 C32 118.5(2) . . ?
C36 C31 C30 122.5(2) . . ?
C32 C31 C30 119.1(2) . . ?
C33 C32 C31 119.9(3) . . ?
C33 C32 H32 120.0 . . ?
C31 C32 H32 120.0 . . ?
C34 C33 C32 121.2(3) . . ?
C34 C33 H33 119.4 . . ?
C32 C33 H33 119.4 . . ?
C33 C34 C35 119.1(3) . . ?
C33 C34 H34 120.4 . . ?
C35 C34 H34 120.4 . . ?
C34 C35 C36 120.1(3) . . ?
C34 C35 H35 119.9 . . ?
C36 C35 H35 119.9 . . ?
C31 C36 C35 121.1(3) . . ?
C31 C36 H36 119.4 . . ?
C35 C36 H36 119.4 . . ?
H1W1 O1W H2W1 108(2) . . ?
H1W2 O2W H2W2 107(3) . . ?
H1W4 O4W H2W4 108(3) . . ?
H1W4 O4W' H2W4 71(3) . . ?
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
Si1 F2 1.6682(13) . ?
Si1 F6 1.6686(13) . ?
Si1 F1 1.6703(13) . ?
Si1 F4 1.6766(13) . ?
Si1 F5 1.6767(12) . ?
Si1 F3 1.6806(13) . ?
N1 C1 1.464(2) . ?
N1 C8 1.469(2) . ?
N1 C9 1.480(3) . ?
N2 C2 1.499(2) . ?
N2 C3 1.506(2) . ?
N2 C16 1.513(2) . ?
N2 H2N 0.98(2) . ?
N3 C5 1.500(3) . ?
N3 C4 1.510(2) . ?
N3 C23 1.513(2) . ?
N3 H3N 0.97(2) . ?
N4 C6 1.501(3) . ?
N4 C7 1.508(2) . ?
N4 C30 1.515(3) . ?
N4 H1N 0.92(2) . ?
C1 C2 1.509(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.505(3) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.513(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.503(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.497(3) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C15 1.372(3) . ?
C10 C11 1.388(3) . ?
C11 C12 1.371(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.341(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.366(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.402(4) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.501(3) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.379(3) . ?
C17 C22 1.387(3) . ?
C18 C19 1.382(4) . ?
C18 H18 0.9300 . ?
C19 C20 1.361(4) . ?
C19 H19 0.9300 . ?
C20 C21 1.354(4) . ?
C20 H20 0.9300 . ?
C21 C22 1.378(3) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 C24 1.504(3) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 C29 1.377(3) . ?
C24 C25 1.379(3) . ?
C25 C26 1.373(3) . ?
C25 H25 0.9300 . ?
C26 C27 1.364(3) . ?
C26 H26 0.9300 . ?
C27 C28 1.368(3) . ?
C27 H27 0.9300 . ?
C28 C29 1.379(3) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C30 C31 1.497(3) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 C36 1.369(3) . ?
C31 C32 1.380(3) . ?
C32 C33 1.376(4) . ?
C32 H32 0.9300 . ?
C33 C34 1.358(4) . ?
C33 H33 0.9300 . ?
C34 C35 1.369(4) . ?
C34 H34 0.9300 . ?
C35 C36 1.374(3) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
O1W H1W1 0.885(16) . ?
O1W H2W1 0.847(16) . ?
O2W H1W2 0.866(18) . ?
O2W H2W2 0.924(18) . ?
O3W' O3W' 0.94(5) 2_655 ?
O4W H1W4 0.90(2) . ?
O4W H2W4 0.90(2) . ?
O4W' H1W4 1.14(8) . ?
O4W' H2W4 1.35(7) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2N F7 0.98(2) 1.68(2) 2.630(2) 160.8(18) .
N3 H3N F7 0.97(2) 1.55(2) 2.507(2) 166.7(17) .
N4 H1N F7 0.92(2) 1.75(2) 2.647(2) 163.8(18) .
O1W H1W1 F5 0.885(16) 1.870(17) 2.753(2) 174(2) .
O1W H2W1 F2 0.847(16) 2.020(17) 2.856(2) 169(3) 5_676
O2W H1W2 F6 0.866(18) 2.17(3) 2.945(3) 148(3) 5_666
O2W H1W2 F1 0.866(18) 2.22(2) 2.982(3) 146(3) 5_666
O2W H2W2 O3W 0.924(18) 2.28(4) 2.753(4) 111(3) .
O4W H1W4 F3 0.90(2) 1.98(4) 2.777(5) 147(6) .
O4W H2W4 O3W 0.90(2) 2.00(3) 2.814(6) 151(6) 2_655
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 N2 C3 164.36(17) . . . . ?
C2 N2 C3 C4 -67.1(2) . . . . ?
N2 C3 C4 N3 -74.5(2) . . . . ?
C3 C4 N3 C5 150.52(18) . . . . ?
C4 N3 C5 C6 -65.9(2) . . . . ?
N3 C5 C6 N4 -66.0(3) . . . . ?
C5 C6 N4 C7 167.91(18) . . . . ?
C6 N4 C7 C8 -71.7(2) . . . . ?
N4 C7 C8 N1 -61.3(2) . . . . ?
C7 C8 N1 C1 158.91(18) . . . . ?
C8 N1 C1 C2 -79.3(2) . . . . ?
N1 C1 C2 N2 -60.6(2) . . . . ?
