#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:14:55 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180383 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/52/7205281.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_7205281
loop_
_publ_author_name
'Dey, Sandeep Kumar'
'Ojha, Bimlesh'
'Das, Gopal'
_publ_section_title
;
 A subtle interplay of C--H hydrogen bonds in complexation of anions of
 varied dimensionality by a nitro functionalized tripodal podand
;
_journal_issue                   1
_journal_name_full               CrystEngComm
_journal_page_first              269
_journal_paper_doi               10.1039/c0ce00316f
_journal_volume                  13
_journal_year                    2011
_chemical_formula_sum            'C48 H50 F6 N8 O20 Si'
_chemical_formula_weight         1201.05
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                116.352(3)
_cell_angle_beta                 94.269(5)
_cell_angle_gamma                106.342(3)
_cell_formula_units_Z            3
_cell_length_a                   15.4544(9)
_cell_length_b                   17.9320(9)
_cell_length_c                   18.6070(10)
_cell_measurement_reflns_used    5889
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      21.45
_cell_measurement_theta_min      3.12
_cell_volume                     4313.2(5)
_computing_cell_refinement       'Bruker Smart'
_computing_data_collection       'Bruker Smart'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and onega scans'
_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  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0936
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            45963
_diffrn_reflns_theta_full        30.07
_diffrn_reflns_theta_max         30.07
_diffrn_reflns_theta_min         1.26
_exptl_absorpt_coefficient_mu    0.140
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.941
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1866
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.906
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1121
_refine_ls_number_reflns         24200
_refine_ls_number_restraints     1779
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.1594
_refine_ls_R_factor_gt           0.0935
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1238P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2127
_refine_ls_wR_factor_ref         0.2440
_reflns_number_gt                19542
_reflns_number_total             24200
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CE00316F.TXT
_cod_data_source_block           nitro-SiF6
_cod_original_cell_volume        4313.2(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7205281
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.67054(7) 0.67049(6) 0.66660(6) 0.0481(3) Uani 1 1 d U . .
F1 F 0.64387(17) 0.59204(15) 0.69461(15) 0.0751(7) Uani 1 1 d U . .
F4 F 0.69748(15) 0.74910(14) 0.63831(14) 0.0647(6) Uani 1 1 d U . .
F2 F 0.74144(18) 0.74266(14) 0.76141(13) 0.0829(8) Uani 1 1 d U . .
F6 F 0.59982(16) 0.59857(14) 0.57149(13) 0.0683(7) Uani 1 1 d U . .
F3 F 0.75772(17) 0.63960(17) 0.63410(15) 0.0778(7) Uani 1 1 d U . .
F5 F 0.58235(18) 0.70157(17) 0.69884(15) 0.0785(7) Uani 1 1 d U . .
N1 N 0.8314(2) 0.6612(2) 0.81937(18) 0.0425(7) Uani 1 1 d U . .
C3 C 0.8975(2) 0.4614(2) 0.86203(19) 0.0369(8) Uani 1 1 d U . .
C1 C 0.8209(3) 0.5689(2) 0.75392(19) 0.0460(9) Uani 1 1 d U . .
H1A H 0.7568 0.5308 0.7402 0.055 Uiso 1 1 calc R . .
H1B H 0.8339 0.5715 0.7047 0.055 Uiso 1 1 calc R . .
C8 C 0.8652(3) 0.4405(2) 0.9211(2) 0.0453(9) Uani 1 1 d U . .
H8 H 0.8157 0.4555 0.9411 0.054 Uiso 1 1 calc R . .
C6 C 0.9814(3) 0.3772(2) 0.9200(2) 0.0481(9) Uani 1 1 d U . .
C2 C 0.8817(3) 0.5264(2) 0.7764(2) 0.0471(9) Uani 1 1 d U . .
H2A H 0.8808 0.4743 0.7274 0.057 Uiso 1 1 calc R . .
H2B H 0.9450 0.5679 0.7994 0.057 Uiso 1 1 calc R . .
C4 C 0.9711(2) 0.4407(2) 0.8334(2) 0.0417(8) Uani 1 1 d U . .
H4 H 0.9927 0.4547 0.7940 0.050 Uiso 1 1 calc R . .
C7 C 0.9072(3) 0.3976(2) 0.9497(2) 0.0485(9) Uani 1 1 d U . .
H7 H 0.8858 0.3825 0.9886 0.058 Uiso 1 1 calc R . .
C5 C 1.0128(3) 0.3988(2) 0.8639(2) 0.0480(9) Uani 1 1 d U . .
H5 H 1.0636 0.3853 0.8453 0.058 Uiso 1 1 calc R . .
O1 O 0.84925(16) 0.50148(15) 0.83542(13) 0.0442(6) Uani 1 1 d U . .
O3 O 0.9926(3) 0.3099(2) 0.9994(2) 0.0919(11) Uani 1 1 d U . .
O2 O 1.0997(3) 0.3261(3) 0.9334(2) 0.1128(14) Uani 1 1 d U . .
N2 N 1.0272(3) 0.3341(2) 0.9529(2) 0.0692(11) Uani 1 1 d U . .
C9 C 0.9272(3) 0.7278(2) 0.8509(2) 0.0481(9) Uani 1 1 d U . .
H9A H 0.9255 0.7848 0.8907 0.058 Uiso 1 1 calc R . .
H9B H 0.9654 0.7102 0.8796 0.058 Uiso 1 1 calc R . .
C16 C 1.0551(3) 0.5811(3) 0.6340(2) 0.0606(11) Uani 1 1 d U . .
H16 H 1.0342 0.5352 0.6464 0.073 Uiso 1 1 calc R . .
C15 C 1.0964(3) 0.5688(3) 0.5678(2) 0.0652(12) Uani 1 1 d U . .
H15 H 1.1032 0.5147 0.5351 0.078 Uiso 1 1 calc R . .
C10 C 0.9723(3) 0.7392(3) 0.7863(2) 0.0602(11) Uani 1 1 d U . .
H10A H 0.9282 0.7402 0.7471 0.072 Uiso 1 1 calc R . .
H10B H 1.0242 0.7951 0.8116 0.072 Uiso 1 1 calc R . .
C11 C 1.0452(3) 0.6617(3) 0.6813(2) 0.0558(10) Uani 1 1 d U . .
C14 C 1.1270(3) 0.6386(4) 0.5519(2) 0.0677(13) Uani 1 1 d U . .
C13 C 1.1203(3) 0.7198(4) 0.6001(3) 0.0737(13) Uani 1 1 d U . .
H13 H 1.1433 0.7663 0.5888 0.088 Uiso 1 1 calc R . .
C12 C 1.0793(3) 0.7316(3) 0.6649(3) 0.0673(12) Uani 1 1 d U . .
H12 H 1.0742 0.7864 0.6981 0.081 Uiso 1 1 calc R . .
O4 O 1.00411(19) 0.66696(18) 0.74495(16) 0.0608(8) Uani 1 1 d U . .
O6 O 1.1743(2) 0.5526(3) 0.4391(2) 0.1149(15) Uani 1 1 d U . .
O5 O 1.1986(3) 0.6880(4) 0.4680(3) 0.1349(17) Uani 1 1 d U . .
N3 N 1.1687(3) 0.6242(4) 0.4804(3) 0.0899(15) Uani 1 1 d U . .
C17 C 0.7865(3) 0.6587(2) 0.8875(2) 0.0483(9) Uani 1 1 d U . .
H17A H 0.8160 0.6320 0.9124 0.058 Uiso 1 1 calc R . .
H17B H 0.7219 0.6208 0.8639 0.058 Uiso 1 1 calc R . .
C18 C 0.7918(3) 0.7486(2) 0.9540(2) 0.0552(10) Uani 1 1 d U . .
H18A H 0.8540 0.7829 0.9886 0.066 Uiso 1 1 calc R . .
H18B H 0.7734 0.7819 0.9303 0.066 Uiso 1 1 calc R . .
C19 C 0.7317(3) 0.7924(3) 1.0749(3) 0.0687(12) Uani 1 1 d U . .
O7 O 0.7284(2) 0.72769(19) 0.99928(17) 0.0719(9) Uani 1 1 d U . .
C21 C 0.7842(4) 0.9383(5) 1.1870(3) 0.138(3) Uani 1 1 d U . .
H21 H 0.8228 0.9976 1.2118 0.166 Uiso 1 1 calc R . .
C20 C 0.7899(3) 0.8788(4) 1.1106(3) 0.0915(17) Uani 1 1 d U . .
H20 H 0.8326 0.8970 1.0837 0.110 Uiso 1 1 calc R . .
C22 C 0.7231(4) 0.9115(6) 1.2263(3) 0.128(3) Uani 1 1 d U . .
C24 C 0.6689(4) 0.7637(4) 1.1147(3) 0.0991(17) Uani 1 1 d U . .
H24 H 0.6301 0.7046 1.0905 0.119 Uiso 1 1 calc R . .
C23 C 0.6653(5) 0.8267(5) 1.1930(4) 0.123(2) Uani 1 1 d U . .
H23 H 0.6236 0.8098 1.2212 0.147 Uiso 1 1 calc R . .
O8 O 0.7517(4) 1.0517(6) 1.3297(4) 0.269(4) Uani 1 1 d U . .
O9 O 0.6741(5) 0.9457(6) 1.3479(3) 0.257(4) Uani 1 1 d U . .
N4 N 0.7155(5) 0.9736(7) 1.3070(4) 0.203(4) Uani 1 1 d U . .
Si2 Si 1.0000 1.0000 1.0000 0.0414(4) Uani 1 2 d SU . .
F9 F 0.97951(15) 0.92947(15) 1.03794(14) 0.0692(7) Uani 1 1 d U . .
F8 F 0.9158(2) 0.92412(15) 0.91523(16) 0.0949(9) Uani 1 1 d U . .
F7 F 1.0779(2) 0.9588(2) 0.95914(18) 0.0970(9) Uani 1 1 d U . .
N5 N 0.1641(2) 0.99399(18) 0.15003(17) 0.0383(7) Uani 1 1 d U . .
C25 C 0.2604(2) 1.0607(2) 0.1844(2) 0.0433(9) Uani 1 1 d U . .
H25A H 0.2592 1.1158 0.2283 0.052 Uiso 1 1 calc R . .
H25B H 0.2989 1.0393 0.2084 0.052 Uiso 1 1 calc R . .
C26 C 0.3038(3) 1.0794(3) 0.1224(2) 0.0535(10) Uani 1 1 d U . .
H26A H 0.2595 1.0855 0.0875 0.064 Uiso 1 1 calc R . .
H26B H 0.3568 1.1345 0.1501 0.064 Uiso 1 1 calc R . .
C27 C 0.3652(3) 1.0027(3) 0.0054(2) 0.0520(10) Uani 1 1 d U . .
C32 C 0.3818(3) 0.9262(3) -0.0424(2) 0.0611(11) Uani 1 1 d U . .
H32 H 0.3691 0.8808 -0.0289 0.073 Uiso 1 1 calc R . .
C31 C 0.4175(3) 0.9168(3) -0.1109(2) 0.0729(13) Uani 1 1 d U . .
H31 H 0.4307 0.8661 -0.1429 0.088 Uiso 1 1 calc R . .
C28 C 0.3833(3) 1.0712(3) -0.0138(3) 0.0681(12) Uani 1 1 d U . .
H28 H 0.3727 1.1231 0.0194 0.082 Uiso 1 1 calc R . .
C30 C 0.4330(3) 0.9850(4) -0.1304(3) 0.0760(14) Uani 1 1 d U . .
C29 C 0.4170(3) 1.0613(4) -0.0826(3) 0.0818(14) Uani 1 1 d U . .
H29 H 0.4290 1.1063 -0.0966 0.098 Uiso 1 1 calc R . .
C35 C 0.2372(2) 0.7968(2) 0.1915(2) 0.0399(8) Uani 1 1 d U . .
C34 C 0.2181(2) 0.8610(2) 0.1054(2) 0.0437(9) Uani 1 1 d U . .
H34A H 0.2151 0.8076 0.0566 0.052 Uiso 1 1 calc R . .
H34B H 0.2815 0.9024 0.1254 0.052 Uiso 1 1 calc R . .
C33 C 0.1550(2) 0.9017(2) 0.08439(19) 0.0420(8) Uani 1 1 d U . .
H33A H 0.0916 0.8625 0.0716 0.050 Uiso 1 1 calc R . .
H33B H 0.1660 0.9043 0.0348 0.050 Uiso 1 1 calc R . .
C39 C 0.2454(3) 0.7309(2) 0.2777(2) 0.0495(9) Uani 1 1 d U . .
H39 H 0.2242 0.7162 0.3169 0.059 Uiso 1 1 calc R . .
C40 C 0.2054(3) 0.7749(2) 0.2508(2) 0.0441(9) Uani 1 1 d U . .
H40 H 0.1567 0.7908 0.2717 0.053 Uiso 1 1 calc R . .
C38 C 0.3172(3) 0.7084(2) 0.2467(2) 0.0547(10) Uani 1 1 d U . .
C36 C 0.3100(3) 0.7753(2) 0.1615(2) 0.0505(9) Uani 1 1 d U . .
H36 H 0.3319 0.7906 0.1229 0.061 Uiso 1 1 calc R . .
C37 C 0.3508(3) 0.7302(3) 0.1897(2) 0.0572(10) Uani 1 1 d U . .
H37 H 0.4004 0.7151 0.1701 0.069 Uiso 1 1 calc R . .
O10 O 0.33302(18) 1.00583(17) 0.07298(15) 0.0552(7) Uani 1 1 d U . .
O11 O 0.4824(4) 1.0362(4) -0.2197(3) 0.159(2) Uani 1 1 d U . .
O12 O 0.4852(4) 0.9061(3) -0.2443(2) 0.150(2) Uani 1 1 d U . .
N6 N 0.4692(4) 0.9741(5) -0.2036(3) 0.1115(18) Uani 1 1 d U . .
O13 O 0.19053(17) 0.83936(16) 0.16774(14) 0.0480(6) Uani 1 1 d U . .
O15 O 0.3303(2) 0.6409(2) 0.3256(2) 0.0908(11) Uani 1 1 d U . .
O14 O 0.4253(4) 0.6450(4) 0.2504(3) 0.149(2) Uani 1 1 d U . .
N7 N 0.3592(3) 0.6608(3) 0.2760(3) 0.0773(12) Uani 1 1 d U . .
C41 C 0.1155(3) 0.9917(2) 0.2164(2) 0.0453(9) Uani 1 1 d U . .
H41A H 0.0523 0.9501 0.1911 0.054 Uiso 1 1 calc R . .
H41B H 0.1466 0.9706 0.2466 0.054 Uiso 1 1 calc R . .
C42 C 0.1139(3) 1.0816(3) 0.2757(2) 0.0594(11) Uani 1 1 d U . .
H42A H 0.1715 1.1167 0.3175 0.071 Uiso 1 1 calc R . .
H42B H 0.1050 1.1135 0.2469 0.071 Uiso 1 1 calc R . .
C45 C 0.0861(3) 1.2790(3) 0.4956(2) 0.0625(11) Uani 1 1 d U . .
H45 H 0.1250 1.3382 0.5209 0.075 Uiso 1 1 calc R . .
C44 C 0.0961(3) 1.2173(3) 0.4217(2) 0.0563(10) Uani 1 1 d U . .
H44 H 0.1430 1.2340 0.3974 0.068 Uiso 1 1 calc R . .
C43 C 0.0355(3) 1.1307(3) 0.3847(2) 0.0530(10) Uani 1 1 d U . .
C46 C 0.0174(3) 1.2514(3) 0.5312(2) 0.0622(11) Uani 1 1 d U . .
C48 C -0.0329(3) 1.1056(3) 0.4203(2) 0.0619(11) Uani 1 1 d U . .
H48 H -0.0732 1.0469 0.3941 0.074 Uiso 1 1 calc R . .
C47 C -0.0433(3) 1.1653(3) 0.4940(3) 0.0674(12) Uani 1 1 d U . .
H47 H -0.0901 1.1480 0.5181 0.081 Uiso 1 1 calc R . .
O16 O 0.03797(18) 1.06428(18) 0.31191(15) 0.0638(8) Uani 1 1 d U . .
O17 O 0.0536(3) 1.3938(3) 0.6377(2) 0.1282(16) Uani 1 1 d U . .
O18 O -0.0447(3) 1.2867(3) 0.6457(2) 0.1278(16) Uani 1 1 d U . .
N8 N 0.0095(3) 1.3163(3) 0.6107(2) 0.0821(12) Uani 1 1 d U . .
N9 N 0.5017(2) 0.66760(18) 0.50984(17) 0.0402(7) Uani 1 1 d U . .
C51 C 0.4344(2) 0.8654(2) 0.46464(19) 0.0372(8) Uani 1 1 d U . .
C54 C 0.3610(2) 0.9571(2) 0.4076(2) 0.0398(8) Uani 1 1 d U . .
C56 C 0.4714(2) 0.8885(2) 0.40854(19) 0.0402(8) Uani 1 1 d U . .
H56 H 0.5210 0.8724 0.3900 0.048 Uiso 1 1 calc R . .
C52 C 0.3598(2) 0.8883(2) 0.4920(2) 0.0414(8) Uani 1 1 d U . .
H52 H 0.3350 0.8730 0.5296 0.050 Uiso 1 1 calc R . .
C49 C 0.5087(2) 0.7601(2) 0.5743(2) 0.0434(8) Uani 1 1 d U . .
H49A H 0.4963 0.7580 0.6238 0.052 Uiso 1 1 calc R . .
H49B H 0.5720 0.8000 0.5881 0.052 Uiso 1 1 calc R . .
C50 C 0.4452(2) 0.7991(2) 0.5502(2) 0.0419(8) Uani 1 1 d U . .
H50A H 0.3826 0.7559 0.5266 0.050 Uiso 1 1 calc R . .
H50B H 0.4442 0.8511 0.5983 0.050 Uiso 1 1 calc R . .
C55 C 0.4350(2) 0.9352(2) 0.38010(19) 0.0432(9) Uani 1 1 d U . .
H55 H 0.4602 0.9515 0.3431 0.052 Uiso 1 1 calc R . .
C53 C 0.3229(2) 0.9339(2) 0.4628(2) 0.0444(9) Uani 1 1 d U . .
H53 H 0.2725 0.9491 0.4802 0.053 Uiso 1 1 calc R . .
O19 O 0.47810(16) 0.82304(15) 0.49118(14) 0.0433(6) Uani 1 1 d U . .
O20 O 0.3545(2) 1.0219(2) 0.3263(2) 0.0796(9) Uani 1 1 d U . .
O21 O 0.2616(3) 1.0307(2) 0.4053(2) 0.0939(11) Uani 1 1 d U . .
N10 N 0.3233(3) 1.0063(2) 0.3779(2) 0.0573(9) Uani 1 1 d U . .
C57 C 0.4068(2) 0.5982(2) 0.4807(2) 0.0465(9) Uani 1 1 d U . .
H57A H 0.3630 0.6197 0.4632 0.056 Uiso 1 1 calc R . .
H57B H 0.4064 0.5452 0.4328 0.056 Uiso 1 1 calc R . .
C58 C 0.3742(3) 0.5730(3) 0.5431(2) 0.0555(10) Uani 1 1 d U . .
H58A H 0.3222 0.5172 0.5160 0.067 Uiso 1 1 calc R . .
H58B H 0.4237 0.5655 0.5714 0.067 Uiso 1 1 calc R . .
O22 O 0.34637(17) 0.64240(17) 0.60181(15) 0.0541(7) Uani 1 1 d U . .
C59 C 0.3151(3) 0.6303(3) 0.6641(3) 0.0624(11) Uani 1 1 d U . .
C63 C 0.2588(3) 0.6934(5) 0.7856(3) 0.103(2) Uani 1 1 d U . .
H63 H 0.2447 0.7402 0.8247 0.124 Uiso 1 1 calc R . .
C62 C 0.2458(4) 0.6185(6) 0.7899(4) 0.114(2) Uani 1 1 d U . .
C60 C 0.2994(3) 0.5533(4) 0.6693(3) 0.0913(16) Uani 1 1 d U . .
H60 H 0.3110 0.5052 0.6294 0.110 Uiso 1 1 calc R . .
C61 C 0.2657(4) 0.5490(5) 0.7353(4) 0.111(2) Uani 1 1 d U . .
H61 H 0.2571 0.4990 0.7416 0.133 Uiso 1 1 calc R . .
C65 C 0.5365(3) 0.6625(3) 0.4353(2) 0.0509(10) Uani 1 1 d U . .
H65A H 0.5362 0.6027 0.4019 0.061 Uiso 1 1 calc R . .
H65B H 0.4934 0.6724 0.4029 0.061 Uiso 1 1 calc R . .
C66 C 0.6311(3) 0.7264(3) 0.4523(2) 0.0603(11) Uani 1 1 d U . .
H66A H 0.6304 0.7862 0.4720 0.072 Uiso 1 1 calc R . .
H66B H 0.6741 0.7266 0.4931 0.072 Uiso 1 1 calc R . .
O25 O 0.6556(2) 0.6948(2) 0.37522(16) 0.0771(9) Uani 1 1 d U . .
C69 C 0.8765(3) 0.8695(3) 0.4171(3) 0.0780(13) Uani 1 1 d U . .
H69 H 0.9181 0.9236 0.4590 0.094 Uiso 1 1 calc R . .
C68 C 0.7945(3) 0.8264(3) 0.4290(3) 0.0673(12) Uani 1 1 d U . .
H68 H 0.7789 0.8526 0.4794 0.081 Uiso 1 1 calc R . .
C70 C 0.8944(3) 0.8282(4) 0.3393(3) 0.0781(13) Uani 1 1 d U . .
C71 C 0.8354(4) 0.7479(4) 0.2763(3) 0.0820(14) Uani 1 1 d U . .
H71 H 0.8493 0.7223 0.2250 0.098 Uiso 1 1 calc R . .
N12 N 0.9862(4) 0.8713(4) 0.3267(4) 0.1029(16) Uani 1 1 d U . .
C72 C 0.7557(3) 0.7066(3) 0.2913(3) 0.0812(14) Uani 1 1 d U . .
H72 H 0.7148 0.6519 0.2498 0.097 Uiso 1 1 calc R . .
C67 C 0.7351(3) 0.7448(3) 0.3668(3) 0.0650(11) Uani 1 1 d U . .
O26 O 0.9990(3) 0.8349(3) 0.2567(3) 0.1446(18) Uani 1 1 d U . .
O27 O 1.0412(3) 0.9374(3) 0.3860(3) 0.1346(18) Uani 1 1 d U . .
C64 C 0.2938(3) 0.6992(3) 0.7210(3) 0.0786(14) Uani 1 1 d U . .
H64 H 0.3028 0.7502 0.7162 0.094 Uiso 1 1 calc R . .
N11 N 0.2066(6) 0.6140(7) 0.8598(5) 0.172(3) Uani 1 1 d U . .
O24 O 0.1862(6) 0.6734(7) 0.9048(4) 0.253(4) Uani 1 1 d U . .
O23 O 0.2032(5) 0.5474(5) 0.8659(4) 0.215(3) Uani 1 1 d U . .
H1N H 0.796(3) 0.677(3) 0.799(2) 0.068(15) Uiso 1 1 d . . .
H2N H 0.136(2) 1.011(2) 0.119(2) 0.049(11) Uiso 1 1 d . . .
H3N H 0.553(3) 0.642(2) 0.535(2) 0.068(11) Uiso 1 1 d . . .
O28 O 0.4823(10) 0.3136(11) 0.1503(8) 0.500 Uiso 1 1 d P . .
O29 O 0.5705(9) 0.2861(9) 0.0319(8) 0.500 Uiso 1 1 d P . .
O30 O 0.4881(10) 0.5717(11) 0.8438(8) 0.500 Uiso 1 1 d P . .
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'
P P 0.1023 0.0942 '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
F3 Si1 F5 179.66(13) . . ?
F3 Si1 F1 88.80(14) . . ?
F5 Si1 F1 91.39(14) . . ?
F3 Si1 F4 91.05(13) . . ?
F5 Si1 F4 88.76(13) . . ?
F1 Si1 F4 179.85(15) . . ?
F3 Si1 F2 89.46(14) . . ?
F5 Si1 F2 90.82(14) . . ?
F1 Si1 F2 89.09(12) . . ?
F4 Si1 F2 90.96(12) . . ?
F3 Si1 F6 90.46(13) . . ?
F5 Si1 F6 89.26(13) . . ?
F1 Si1 F6 91.18(12) . . ?
F4 Si1 F6 88.77(12) . . ?
F2 Si1 F6 179.72(15) . . ?
C9 N1 C17 112.5(3) . . ?
C9 N1 C1 115.5(3) . . ?
C17 N1 C1 111.2(3) . . ?
O1 C3 C4 124.4(3) . . ?
O1 C3 C8 115.1(3) . . ?
C4 C3 C8 120.5(3) . . ?
C2 C1 N1 115.8(3) . . ?
C7 C8 C3 119.4(4) . . ?
C5 C6 C7 120.9(4) . . ?
C5 C6 N2 120.4(4) . . ?
C7 C6 N2 118.6(4) . . ?
O1 C2 C1 109.9(3) . . ?
C3 C4 C5 119.0(3) . . ?
C8 C7 C6 119.2(3) . . ?
C6 C5 C4 120.9(4) . . ?
C3 O1 C2 117.0(3) . . ?
O3 N2 O2 123.9(4) . . ?
O3 N2 C6 118.3(4) . . ?
O2 N2 C6 117.8(4) . . ?
C10 C9 N1 115.0(3) . . ?
C11 C16 C15 119.7(4) . . ?
C14 C15 C16 118.3(4) . . ?
O4 C10 C9 108.8(3) . . ?
O4 C11 C16 115.0(4) . . ?
O4 C11 C12 124.6(4) . . ?
C16 C11 C12 120.4(4) . . ?
C13 C14 C15 122.4(4) . . ?
C13 C14 N3 119.6(5) . . ?
C15 C14 N3 118.0(5) . . ?
C12 C13 C14 119.1(5) . . ?
C13 C12 C11 120.0(4) . . ?
C11 O4 C10 119.4(3) . . ?
O6 N3 O5 123.8(5) . . ?
O6 N3 C14 118.6(6) . . ?
O5 N3 C14 117.5(5) . . ?
N1 C17 C18 114.2(3) . . ?
O7 C18 C17 103.5(3) . . ?
O7 C19 C20 124.8(4) . . ?
O7 C19 C24 113.9(5) . . ?
C20 C19 C24 121.3(4) . . ?
C19 O7 C18 118.8(3) . . ?
C22 C21 C20 120.6(6) . . ?
C19 C20 C21 118.7(5) . . ?
C21 C22 C23 122.0(6) . . ?
C21 C22 N4 121.3(8) . . ?
C23 C22 N4 116.6(8) . . ?
C19 C24 C23 118.2(6) . . ?
C22 C23 C24 119.2(6) . . ?
O9 N4 O8 123.0(8) . . ?
O9 N4 C22 119.8(10) . . ?
O8 N4 C22 117.1(9) . . ?
F7 Si2 F7 180.0(2) . 2_777 ?
F7 Si2 F9 87.87(13) . . ?
F7 Si2 F9 92.13(13) 2_777 . ?
F7 Si2 F9 92.13(13) . 2_777 ?
F7 Si2 F9 87.87(13) 2_777 2_777 ?
F9 Si2 F9 180.00(8) . 2_777 ?
F7 Si2 F8 88.32(16) . 2_777 ?
F7 Si2 F8 91.68(16) 2_777 2_777 ?
F9 Si2 F8 90.15(11) . 2_777 ?
F9 Si2 F8 89.85(12) 2_777 2_777 ?
F7 Si2 F8 91.68(16) . . ?
F7 Si2 F8 88.32(16) 2_777 . ?
F9 Si2 F8 89.85(12) . . ?
F9 Si2 F8 90.15(11) 2_777 . ?
F8 Si2 F8 180.000(1) 2_777 . ?
C25 N5 C41 112.3(3) . . ?
C25 N5 C33 115.3(3) . . ?
C41 N5 C33 112.1(3) . . ?
C26 C25 N5 114.1(3) . . ?
O10 C26 C25 108.1(3) . . ?
O10 C27 C32 114.8(4) . . ?
O10 C27 C28 124.2(4) . . ?
C32 C27 C28 121.0(4) . . ?
C27 C32 C31 119.9(4) . . ?
C30 C31 C32 118.3(4) . . ?
C27 C28 C29 119.1(4) . . ?
C29 C30 C31 121.8(4) . . ?
C29 C30 N6 120.0(5) . . ?
C31 C30 N6 118.1(5) . . ?
C30 C29 C28 119.8(5) . . ?
O13 C35 C36 124.6(3) . . ?
O13 C35 C40 115.2(3) . . ?
C36 C35 C40 120.2(4) . . ?
O13 C34 C33 109.4(3) . . ?
C34 C33 N5 116.3(3) . . ?
C40 C39 C38 119.2(4) . . ?
C39 C40 C35 120.3(4) . . ?
C39 C38 C37 121.7(4) . . ?
C39 C38 N7 118.6(4) . . ?
C37 C38 N7 119.7(4) . . ?
C35 C36 C37 119.0(4) . . ?
C38 C37 C36 119.4(4) . . ?
C27 O10 C26 118.9(3) . . ?
O12 N6 O11 124.3(5) . . ?
O12 N6 C30 118.9(6) . . ?
O11 N6 C30 116.8(6) . . ?
C35 O13 C34 117.7(3) . . ?
O15 N7 O14 122.1(5) . . ?
O15 N7 C38 120.4(5) . . ?
O14 N7 C38 117.4(5) . . ?
C42 C41 N5 112.3(3) . . ?
O16 C42 C41 105.4(3) . . ?
C46 C45 C44 119.0(4) . . ?
C45 C44 C43 118.9(4) . . ?
O16 C43 C48 114.9(4) . . ?
O16 C43 C44 124.3(4) . . ?
C48 C43 C44 120.8(4) . . ?
C47 C46 C45 122.0(4) . . ?
C47 C46 N8 119.4(4) . . ?
C45 C46 N8 118.6(4) . . ?
C43 C48 C47 121.3(4) . . ?
C46 C47 C48 117.9(4) . . ?
C43 O16 C42 118.6(3) . . ?
O17 N8 O18 124.0(4) . . ?
O17 N8 C46 119.3(5) . . ?
O18 N8 C46 116.7(5) . . ?
C65 N9 C57 107.9(3) . . ?
C65 N9 C49 115.2(3) . . ?
C57 N9 C49 114.7(3) . . ?
O19 C51 C52 124.3(3) . . ?
O19 C51 C56 115.5(3) . . ?
C52 C51 C56 120.2(3) . . ?
C55 C54 C53 121.6(3) . . ?
C55 C54 N10 118.5(3) . . ?
C53 C54 N10 119.9(4) . . ?
C55 C56 C51 120.5(3) . . ?
C53 C52 C51 119.3(3) . . ?
C50 C49 N9 116.0(3) . . ?
O19 C50 C49 108.4(3) . . ?
C54 C55 C56 118.7(3) . . ?
C52 C53 C54 119.8(3) . . ?
C51 O19 C50 118.6(3) . . ?
O20 N10 O21 121.9(4) . . ?
O20 N10 C54 118.8(4) . . ?
O21 N10 C54 119.3(4) . . ?
C58 C57 N9 115.0(3) . . ?
O22 C58 C57 108.9(3) . . ?
C59 O22 C58 116.7(3) . . ?
C64 C59 O22 115.2(4) . . ?
C64 C59 C60 120.2(5) . . ?
O22 C59 C60 124.5(5) . . ?
C62 C63 C64 118.1(6) . . ?
C63 C62 C61 123.5(7) . . ?
C63 C62 N11 116.7(8) . . ?
C61 C62 N11 119.8(8) . . ?
C61 C60 C59 118.7(6) . . ?
C62 C61 C60 119.0(7) . . ?
C66 C65 N9 115.6(3) . . ?
O25 C66 C65 104.2(3) . . ?
C67 O25 C66 119.4(3) . . ?
C68 C69 C70 116.9(5) . . ?
C67 C68 C69 120.7(4) . . ?
C71 C70 C69 123.2(4) . . ?
C71 C70 N12 119.0(5) . . ?
C69 C70 N12 117.6(5) . . ?
C72 C71 C70 117.9(5) . . ?
O27 N12 O26 126.0(5) . . ?
O27 N12 C70 117.7(5) . . ?
O26 N12 C70 116.2(6) . . ?
C67 C72 C71 120.9(5) . . ?
C72 C67 O25 115.2(4) . . ?
C72 C67 C68 120.4(4) . . ?
O25 C67 C68 124.4(4) . . ?
C59 C64 C63 120.4(6) . . ?
O24 N11 O23 126.2(10) . . ?
O24 N11 C62 119.0(10) . . ?
O23 N11 C62 114.7(9) . . ?
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 F3 1.653(3) . ?
Si1 F5 1.667(3) . ?
Si1 F1 1.667(2) . ?
Si1 F4 1.673(2) . ?
Si1 F2 1.696(2) . ?
Si1 F6 1.698(2) . ?
N1 C9 1.489(5) . ?
N1 C17 1.501(4) . ?
N1 C1 1.510(4) . ?
C3 O1 1.371(4) . ?
C3 C4 1.367(5) . ?
C3 C8 1.393(4) . ?
C1 C2 1.505(5) . ?
C8 C7 1.373(5) . ?
C6 C5 1.343(5) . ?
C6 C7 1.380(5) . ?
C6 N2 1.463(5) . ?
C2 O1 1.431(4) . ?
C4 C5 1.377(5) . ?
O3 N2 1.223(5) . ?
O2 N2 1.229(5) . ?
C9 C10 1.495(5) . ?
C16 C11 1.379(5) . ?
C16 C15 1.389(5) . ?
C15 C14 1.377(6) . ?
C10 O4 1.429(4) . ?
C11 O4 1.364(4) . ?
C11 C12 1.390(6) . ?
C14 C13 1.370(6) . ?
C14 N3 1.472(6) . ?
C13 C12 1.365(5) . ?
O6 N3 1.202(6) . ?
O5 N3 1.236(6) . ?
C17 C18 1.509(5) . ?
C18 O7 1.416(4) . ?
C19 O7 1.355(5) . ?
C19 C20 1.365(6) . ?
C19 C24 1.386(6) . ?
C21 C22 1.348(9) . ?
C21 C20 1.377(6) . ?
C22 C23 1.345(9) . ?
C22 N4 1.456(8) . ?
C24 C23 1.408(7) . ?
O8 N4 1.204(13) . ?
O9 N4 1.214(11) . ?
Si2 F7 1.647(2) . ?
Si2 F7 1.647(2) 2_777 ?
Si2 F9 1.673(2) . ?
Si2 F9 1.673(2) 2_777 ?
Si2 F8 1.681(2) 2_777 ?
Si2 F8 1.681(2) . ?
N5 C25 1.495(4) . ?
N5 C41 1.502(4) . ?
N5 C33 1.517(4) . ?
C25 C26 1.491(5) . ?
C26 O10 1.453(4) . ?
C27 O10 1.370(4) . ?
C27 C32 1.374(5) . ?
C27 C28 1.388(5) . ?
C32 C31 1.386(5) . ?
C31 C30 1.386(6) . ?
C28 C29 1.376(5) . ?
C30 C29 1.366(7) . ?
C30 N6 1.466(6) . ?
C35 O13 1.363(4) . ?
C35 C36 1.368(5) . ?
C35 C40 1.404(5) . ?
C34 O13 1.433(4) . ?
C34 C33 1.495(4) . ?
C39 C40 1.355(5) . ?
C39 C38 1.367(5) . ?
C38 C37 1.372(5) . ?
C38 N7 1.456(5) . ?
C36 C37 1.393(5) . ?
O11 N6 1.245(7) . ?
O12 N6 1.224(7) . ?
O15 N7 1.201(5) . ?
O14 N7 1.210(5) . ?
C41 C42 1.504(5) . ?
C42 O16 1.423(4) . ?
C45 C46 1.383(6) . ?
C45 C44 1.384(5) . ?
C44 C43 1.379(5) . ?
C43 O16 1.362(4) . ?
C43 C48 1.363(5) . ?
C46 C47 1.371(6) . ?
C46 N8 1.461(5) . ?
C48 C47 1.371(5) . ?
O17 N8 1.202(5) . ?
O18 N8 1.243(5) . ?
N9 C65 1.499(4) . ?
N9 C57 1.500(4) . ?
N9 C49 1.522(4) . ?
C51 O19 1.360(4) . ?
C51 C52 1.387(5) . ?
C51 C56 1.388(4) . ?
C54 C55 1.373(5) . ?
C54 C53 1.380(5) . ?
C54 N10 1.448(5) . ?
C56 C55 1.383(5) . ?
C52 C53 1.380(5) . ?
C49 C50 1.500(5) . ?
C50 O19 1.424(4) . ?
O20 N10 1.210(4) . ?
O21 N10 1.212(4) . ?
C57 C58 1.494(5) . ?
C58 O22 1.446(4) . ?
O22 C59 1.368(5) . ?
C59 C64 1.370(6) . ?
C59 C60 1.380(6) . ?
C63 C62 1.341(9) . ?
C63 C64 1.387(6) . ?
C62 C61 1.348(9) . ?
C62 N11 1.500(9) . ?
C60 C61 1.393(7) . ?
C65 C66 1.488(5) . ?
C66 O25 1.416(4) . ?
O25 C67 1.368(5) . ?
C69 C68 1.377(6) . ?
C69 C70 1.394(6) . ?
C68 C67 1.381(6) . ?
C70 C71 1.372(6) . ?
C70 N12 1.503(6) . ?
C71 C72 1.367(6) . ?
N12 O27 1.214(6) . ?
N12 O26 1.232(6) . ?
C72 C67 1.370(5) . ?
N11 O24 1.170(11) . ?
N11 O23 1.236(11) . ?
