# Supplementary Material (ESI) for New Journal of Chemistry
# This journal is (c) The Royal Society of Chemistry and 
# The Centre National de la Recherche Scientifique, 2008

data_global

_journal_coden_Cambridge         440

loop_
_publ_author_name
'Lluisa Perez-Garcia'
'Ermitas Alcalde'
'Susana Ramos'
'J Stoddart'
'A J.P. White'
'David J Williams'

_publ_contact_author_name        'Lluisa Perez-Garcia'
_publ_contact_author_email       MLPEREZ@UB.EDU

_publ_section_title              
;
Proton Ionizable 1H-1,2,4-Triazole ?-Electron
Deficient Cyclophanes as Hosts and in [2]Catenanes
;

# Attachment 'NJC_09-08_new_B815355H.cif copy'

data_10_4PF6
_database_code_depnum_ccdc_archive 'CCDC 708196'

_audit_creation_method           SHELXL
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_formula_moiety         'C28 H40 O10, C32 H29 N7, 4(F6 P), 4(C2 H3 N)'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_sum            'C68 H81 F24 N11 O10 P4'
_chemical_formula_weight         1792.32
_chemical_melting_point          ?
_chemical_compound_source        ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.5888(7)
_cell_length_b                   14.7300(10)
_cell_length_c                   22.343(2)
_cell_angle_alpha                71.118(5)
_cell_angle_beta                 74.753(5)
_cell_angle_gamma                78.274(5)
_cell_volume                     4048.3(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    203(2)
_cell_measurement_reflns_used    22
_cell_measurement_theta_min      11.03
_cell_measurement_theta_max      27.99

_exptl_crystal_description       rhombs
_exptl_crystal_colour            Red
_exptl_crystal_size_max          0.67
_exptl_crystal_size_mid          0.57
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1844
_exptl_absorpt_coefficient_mu    1.906
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      203(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_standards_number         3
_diffrn_standards_interval_count 97
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12374
_diffrn_reflns_av_R_equivalents  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0378
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.14
_diffrn_reflns_theta_max         60.00
_reflns_number_total             11798
_reflns_number_observed          8887
_reflns_observed_criterion       >2sigma(I)

_computing_data_collection       'Siemens XSCANS'
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'

_refine_special_details          
;
Refinement on F^2^ for ALL reflections except for 845 with very negative F^2^
or flagged by the user for potential systematic errors. Weighted R-factors
wR and all goodnesses 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 observed criterion
of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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.

A distance constraint of 0.90 A was used for the N37-H37 bond.
Spherical thermal parameter restraints were used for F22, F23, F41, F43 F45,
F46 and C91 to prevent the thermal parameters of these atoms from going
wildly anisotropic.

;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      
'calc w=1/[\s^2^(Fo^2^)+(0.1090P)^2^+4.0511P] 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    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00026(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         10953
_refine_ls_number_parameters     1123
_refine_ls_number_restraints     43
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_obs          0.0709
_refine_ls_wR_factor_all         0.2082
_refine_ls_wR_factor_obs         0.1836
_refine_ls_goodness_of_fit_all   1.049
_refine_ls_goodness_of_fit_obs   1.105
_refine_ls_restrained_S_all      1.092
_refine_ls_restrained_S_obs      1.129
_refine_ls_shift/esd_max         0.159
_refine_ls_shift/esd_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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
N1 N 0.3375(2) 0.4440(2) 0.3591(2) 0.0365(7) Uani 1 d . .
C2 C 0.3586(3) 0.4172(3) 0.3043(2) 0.0401(9) Uani 1 d . .
H2A H 0.3680 0.3512 0.3066 0.048 Uiso 1 calc R .
C3 C 0.3662(3) 0.4857(3) 0.2453(2) 0.0383(9) Uani 1 d . .
H3A H 0.3814 0.4665 0.2073 0.046 Uiso 1 calc R .
C4 C 0.3515(3) 0.5844(3) 0.2414(2) 0.0330(8) Uani 1 d . .
C5 C 0.3335(3) 0.6087(3) 0.2987(2) 0.0373(9) Uani 1 d . .
H5A H 0.3260 0.6740 0.2978 0.045 Uiso 1 calc R .
C6 C 0.3267(3) 0.5376(3) 0.3568(2) 0.0373(8) Uani 1 d . .
H6A H 0.3144 0.5547 0.3954 0.045 Uiso 1 calc R .
C7 C 0.3473(3) 0.6599(3) 0.1790(2) 0.0337(8) Uani 1 d . .
C8 C 0.3717(3) 0.6367(3) 0.1206(2) 0.0473(10) Uani 1 d . .
H8A H 0.4015 0.5737 0.1194 0.057 Uiso 1 calc R .
C9 C 0.3527(4) 0.7049(3) 0.0653(2) 0.0500(11) Uani 1 d . .
H9A H 0.3684 0.6880 0.0264 0.060 Uiso 1 calc R .
N10 N 0.3120(2) 0.7956(2) 0.0658(2) 0.0411(8) Uani 1 d . .
C11 C 0.2949(3) 0.8235(3) 0.1200(2) 0.0425(9) Uani 1 d . .
H11A H 0.2711 0.8884 0.1189 0.051 Uiso 1 calc R .
C12 C 0.3124(3) 0.7567(3) 0.1767(2) 0.0392(9) Uani 1 d . .
H12A H 0.3007 0.7763 0.2143 0.047 Uiso 1 calc R .
C13 C 0.2738(3) 0.8633(3) 0.0084(2) 0.0445(10) Uani 1 d . .
H13A H 0.3123 0.8458 -0.0309 0.053 Uiso 1 calc R .
H13B H 0.2839 0.9296 0.0035 0.053 Uiso 1 calc R .
C14 C 0.1611(3) 0.8574(3) 0.0178(2) 0.0402(9) Uani 1 d . .
C15 C 0.1288(4) 0.7929(3) -0.0043(2) 0.0465(10) Uani 1 d . .
H15A H 0.1771 0.7566 -0.0292 0.056 Uiso 1 calc R .
C16 C 0.0256(4) 0.7817(3) 0.0103(2) 0.0478(10) Uani 1 d . .
H16A H 0.0041 0.7375 -0.0045 0.057 Uiso 1 calc R .
C17 C -0.0453(3) 0.8351(3) 0.0461(2) 0.0415(9) Uani 1 d . .
C18 C -0.0140(3) 0.9018(3) 0.0666(2) 0.0419(9) Uani 1 d . .
H18A H -0.0627 0.9398 0.0901 0.050 Uiso 1 calc R .
C19 C 0.0890(3) 0.9124(3) 0.0525(2) 0.0405(9) Uani 1 d . .
H19A H 0.1101 0.9574 0.0666 0.049 Uiso 1 calc R .
C20 C -0.1563(3) 0.8164(3) 0.0676(2) 0.0501(11) Uani 1 d . .
H20A H -0.2017 0.8769 0.0691 0.060 Uiso 1 calc R .
H20B H -0.1738 0.7907 0.0370 0.060 Uiso 1 calc R .
N21 N -0.1703(3) 0.7446(3) 0.1338(2) 0.0441(8) Uani 1 d . .
C22 C -0.1927(4) 0.7757(3) 0.1864(2) 0.0518(11) Uani 1 d . .
H22A H -0.2087 0.8424 0.1820 0.062 Uiso 1 calc R .
C23 C -0.1928(4) 0.7121(3) 0.2459(2) 0.0514(11) Uani 1 d . .
H23A H -0.2091 0.7352 0.2824 0.062 Uiso 1 calc R .
C24 C -0.1690(3) 0.6133(3) 0.2536(2) 0.0379(9) Uani 1 d . .
C25 C -0.1508(3) 0.5834(3) 0.1987(2) 0.0457(10) Uani 1 d . .
H25A H -0.1378 0.5170 0.2020 0.055 Uiso 1 calc R .
C26 C -0.1514(4) 0.6501(3) 0.1390(2) 0.0491(10) Uani 1 d . .
H26A H -0.1385 0.6290 0.1019 0.059 Uiso 1 calc R .
C27 C -0.1552(3) 0.5429(3) 0.3170(2) 0.0389(9) Uani 1 d . .
C28 C -0.1596(3) 0.5747(3) 0.3698(2) 0.0484(10) Uani 1 d . .
H28A H -0.1832 0.6398 0.3683 0.058 Uiso 1 calc R .
C29 C -0.1298(3) 0.5114(3) 0.4242(2) 0.0493(11) Uani 1 d . .
H29A H -0.1322 0.5337 0.4595 0.059 Uiso 1 calc R .
N30 N -0.0973(3) 0.4181(3) 0.4274(2) 0.0450(8) Uani 1 d . .
C31 C -0.0985(4) 0.3837(3) 0.3790(2) 0.0496(10) Uani 1 d . .
H31A H -0.0797 0.3173 0.3832 0.060 Uiso 1 calc R .
C32 C -0.1268(3) 0.4441(3) 0.3237(2) 0.0464(10) Uani 1 d . .
H32A H -0.1270 0.4191 0.2900 0.056 Uiso 1 calc R .
C33 C -0.0544(4) 0.3515(4) 0.4836(2) 0.0543(11) Uani 1 d . .
H33A H -0.0707 0.3820 0.5186 0.065 Uiso 1 calc R .
H33B H -0.0861 0.2916 0.4998 0.065 Uiso 1 calc R .
C34 C 0.0595(3) 0.3283(3) 0.4639(2) 0.0441(10) Uani 1 d . .
N35 N 0.1282(3) 0.3866(2) 0.4597(2) 0.0401(8) Uani 1 d . .
C36 C 0.2176(3) 0.3385(3) 0.4382(2) 0.0359(8) Uani 1 d . .
N37 N 0.2013(3) 0.2565(2) 0.4310(2) 0.0443(8) Uani 1 d D .
H37 H 0.2518(25) 0.2104(24) 0.4210(22) 0.047(13) Uiso 1 d D .
N38 N 0.1001(3) 0.2482(3) 0.4473(2) 0.0506(9) Uani 1 d . .
C39 C 0.3212(3) 0.3685(3) 0.4229(2) 0.0418(9) Uani 1 d . .
H39A H 0.3738 0.3124 0.4214 0.050 Uiso 1 calc R .
H39B H 0.3279 0.3942 0.4568 0.050 Uiso 1 calc R .
O41 O 0.1355(2) 0.4093(2) 0.28681(15) 0.0479(7) Uani 1 d . .
C42 C 0.1551(4) 0.3574(3) 0.2395(3) 0.0581(12) Uani 1 d . .
H42A H 0.2157 0.3777 0.2059 0.070 Uiso 1 calc R .
H42B H 0.0961 0.3717 0.2190 0.070 Uiso 1 calc R .
C43 C 0.1734(4) 0.2512(4) 0.2720(3) 0.0632(13) Uani 1 d . .
H43A H 0.1176 0.2326 0.3098 0.076 Uiso 1 calc R .
H43B H 0.1749 0.2147 0.2420 0.076 Uiso 1 calc R .
O44 O 0.2689(3) 0.2297(2) 0.2917(2) 0.0520(8) Uani 1 d . .
C45 C 0.3028(5) 0.1289(3) 0.3081(3) 0.0662(14) Uani 1 d . .
H45A H 0.3154 0.1057 0.2699 0.079 Uiso 1 calc R .
H45B H 0.2499 0.0942 0.3417 0.079 Uiso 1 calc R .
C46 C 0.3995(4) 0.1108(3) 0.3321(3) 0.0604(13) Uani 1 d . .
H46A H 0.4256 0.0417 0.3422 0.072 Uiso 1 calc R .
H46B H 0.4520 0.1466 0.2989 0.072 Uiso 1 calc R .
O47 O 0.3770(3) 0.1421(2) 0.3889(2) 0.0553(8) Uani 1 d . .
C48 C 0.4481(4) 0.1016(4) 0.4308(2) 0.0621(13) Uani 1 d . .
H48A H 0.4514 0.0310 0.4444 0.075 Uiso 1 calc R .
H48B H 0.4222 0.1236 0.4698 0.075 Uiso 1 calc R .
C49 C 0.5532(4) 0.1274(3) 0.4012(3) 0.0622(13) Uani 1 d . .
H49A H 0.5960 0.1024 0.4336 0.075 Uiso 1 calc R .
H49B H 0.5840 0.0979 0.3659 0.075 Uiso 1 calc R .
O50 O 0.5500(3) 0.2303(2) 0.3766(2) 0.0592(9) Uani 1 d . .
C51 C 0.6504(4) 0.2569(4) 0.3463(3) 0.0641(13) Uani 1 d . .
H51A H 0.6921 0.2070 0.3268 0.077 Uiso 1 calc R .
H51B H 0.6839 0.2619 0.3788 0.077 Uiso 1 calc R .
C52 C 0.6436(4) 0.3512(4) 0.2956(3) 0.0574(12) Uani 1 d . .
H52A H 0.7119 0.3620 0.2681 0.069 Uiso 1 calc R .
H52B H 0.5980 0.3508 0.2682 0.069 Uiso 1 calc R .
O53 O 0.6043(3) 0.4268(2) 0.3258(2) 0.0540(8) Uani 1 d . .
C54 C 0.5950(3) 0.5199(3) 0.2860(2) 0.0451(10) Uani 1 d . .
C55 C 0.6095(3) 0.5434(3) 0.2185(2) 0.0461(10) Uani 1 d . .
H55A H 0.6284 0.4944 0.1976 0.055 Uiso 1 calc R .
C56 C 0.5957(3) 0.6392(4) 0.1832(2) 0.0487(11) Uani 1 d . .
H56A H 0.6056 0.6551 0.1379 0.058 Uiso 1 calc R .
C57 C 0.5676(3) 0.7126(3) 0.2129(2) 0.0470(10) Uani 1 d . .
C58 C 0.5531(3) 0.6887(3) 0.2802(2) 0.0499(11) Uani 1 d . .
H58A H 0.5337 0.7376 0.3012 0.060 Uiso 1 calc R .
C59 C 0.5675(3) 0.5930(3) 0.3153(2) 0.0462(10) Uani 1 d . .
H59A H 0.5583 0.5772 0.3606 0.055 Uiso 1 calc R .
O60 O 0.5582(3) 0.8048(2) 0.1722(2) 0.0586(8) Uani 1 d . .
C61 C 0.5176(4) 0.8825(4) 0.2004(3) 0.0606(13) Uani 1 d . .
H61A H 0.5590 0.8819 0.2305 0.073 Uiso 1 calc R .
H61B H 0.4468 0.8751 0.2247 0.073 Uiso 1 calc R .
C62 C 0.5194(4) 0.9757(4) 0.1479(3) 0.0628(13) Uani 1 d . .
H62A H 0.5019 1.0297 0.1670 0.075 Uiso 1 calc R .
H62B H 0.5889 0.9793 0.1207 0.075 Uiso 1 calc R .
O63 O 0.4484(2) 0.9841(2) 0.1091(2) 0.0553(8) Uani 1 d . .
C64 C 0.4380(4) 1.0792(3) 0.0659(3) 0.0567(12) Uani 1 d . .
H64A H 0.5045 1.0928 0.0368 0.068 Uiso 1 calc R .
H64B H 0.4163 1.1265 0.0907 0.068 Uiso 1 calc R .
C65 C 0.3603(3) 1.0881(3) 0.0272(2) 0.0524(11) Uani 1 d . .
H65A H 0.3507 1.1553 0.0003 0.063 Uiso 1 calc R .
H65B H 0.3878 1.0473 -0.0020 0.063 Uiso 1 calc R .
O66 O 0.2619(2) 1.0618(2) 0.06454(15) 0.0463(7) Uani 1 d . .
C67 C 0.2168(4) 1.1139(3) 0.1113(3) 0.0552(12) Uani 1 d . .
H67A H 0.2145 1.1836 0.0899 0.066 Uiso 1 calc R .
H67B H 0.2587 1.0967 0.1439 0.066 Uiso 1 calc R .
C68 C 0.1113(4) 1.0897(3) 0.1428(2) 0.0551(12) Uani 1 d . .
H68A H 0.0780 1.1292 0.1723 0.066 Uiso 1 calc R .
H68B H 0.0704 1.1035 0.1100 0.066 Uiso 1 calc R .
O69 O 0.1168(2) 0.9903(2) 0.17779(15) 0.0487(7) Uani 1 d . .
C70 C 0.0220(4) 0.9668(3) 0.2191(2) 0.0549(11) Uani 1 d . .
H70A H -0.0309 0.9803 0.1937 0.066 Uiso 1 calc R .
H70B H 0.0003 1.0059 0.2495 0.066 Uiso 1 calc R .
C71 C 0.0344(4) 0.8618(3) 0.2554(2) 0.0517(11) Uani 1 d . .
H71A H 0.0946 0.8458 0.2750 0.062 Uiso 1 calc R .
H71B H -0.0265 0.8461 0.2899 0.062 Uiso 1 calc R .
O72 O 0.0475(2) 0.8080(2) 0.21006(15) 0.0502(7) Uani 1 d . .
C73 C 0.0694(3) 0.7093(3) 0.2314(2) 0.0401(9) Uani 1 d . .
C74 C 0.0747(3) 0.6570(3) 0.2952(2) 0.0418(9) Uani 1 d . .
H74A H 0.0631 0.6890 0.3271 0.050 Uiso 1 calc R .
C75 C 0.0973(3) 0.5573(3) 0.3108(2) 0.0411(9) Uani 1 d . .
H75A H 0.1016 0.5220 0.3536 0.049 Uiso 1 calc R .
C76 C 0.1138(3) 0.5081(3) 0.2652(2) 0.0394(9) Uani 1 d . .
C77 C 0.1085(3) 0.5607(3) 0.2014(2) 0.0445(10) Uani 1 d . .
H77A H 0.1198 0.5285 0.1696 0.053 Uiso 1 calc R .
C78 C 0.0867(3) 0.6602(3) 0.1853(2) 0.0440(10) Uani 1 d . .
H78A H 0.0835 0.6954 0.1423 0.053 Uiso 1 calc R .
P10 P -0.05303(12) 1.37128(10) 0.12163(7) 0.0620(4) Uani 1 d . .
F11 F -0.1616(3) 1.4347(3) 0.1219(3) 0.118(2) Uani 1 d . .
F12 F -0.0046(3) 1.4652(2) 0.1156(2) 0.0834(10) Uani 1 d . .
F13 F -0.0305(5) 1.3970(3) 0.0456(2) 0.133(2) Uani 1 d . .
F14 F -0.0979(4) 1.2768(3) 0.1286(2) 0.1017(13) Uani 1 d . .
F15 F -0.0763(3) 1.3505(3) 0.1976(2) 0.0842(10) Uani 1 d . .
F16 F 0.0567(3) 1.3120(3) 0.1219(2) 0.1098(15) Uani 1 d . .
P20 P 0.68745(11) 0.85085(9) 0.38477(6) 0.0545(3) Uani 1 d . .
F21 F 0.6507(5) 0.7711(6) 0.3619(4) 0.078(2) Uani 0.60 d P 1
F22 F 0.5798(7) 0.9025(6) 0.3959(6) 0.118(3) Uani 0.60 d PU 1
F23 F 0.7056(11) 0.8902(8) 0.3098(4) 0.167(4) Uani 0.60 d PU 1
F24 F 0.8083(4) 0.7975(5) 0.3746(5) 0.087(2) Uani 0.60 d P 1
F25 F 0.6785(7) 0.7761(6) 0.4530(3) 0.115(3) Uani 0.60 d P 1
F26 F 0.7117(5) 0.9290(5) 0.4088(5) 0.106(3) Uani 0.60 d P 1
F21' F 0.6627(10) 0.7545(10) 0.3865(6) 0.082(4) Uiso 0.40 d P 2
F22' F 0.5674(10) 0.8707(8) 0.4232(5) 0.074(3) Uiso 0.40 d P 2
F23' F 0.6435(13) 0.9295(12) 0.3273(9) 0.137(5) Uiso 0.40 d P 2
F24' F 0.7909(9) 0.8308(8) 0.3468(5) 0.080(3) Uiso 0.40 d P 2
F25' F 0.7142(14) 0.8241(14) 0.4506(9) 0.152(6) Uiso 0.40 d P 2
F26' F 0.7361(12) 0.9522(11) 0.3644(7) 0.121(5) Uiso 0.40 d P 2
P30 P 0.76074(12) 0.16751(10) 0.61799(7) 0.0623(4) Uani 1 d . .
F31 F 0.7854(4) 0.1910(5) 0.5421(2) 0.135(2) Uani 1 d . .
F32 F 0.6824(13) 0.1124(12) 0.6157(9) 0.184(8) Uani 0.60 d P 1
F33 F 0.8283(6) 0.0628(5) 0.6360(4) 0.109(2) Uani 0.60 d P 1
F34 F 0.8671(6) 0.2055(6) 0.6142(3) 0.098(2) Uani 0.60 d P 1
F35 F 0.7089(10) 0.2697(5) 0.6030(4) 0.124(4) Uani 0.60 d P 1
F36 F 0.7342(3) 0.1537(3) 0.6944(2) 0.0986(12) Uani 1 d . .
F32' F 0.6718(13) 0.1038(12) 0.6285(9) 0.090(4) Uiso 0.40 d P 2
F33' F 0.8585(13) 0.1117(13) 0.6068(8) 0.141(5) Uiso 0.40 d P 2
F34' F 0.8108(8) 0.2574(8) 0.6159(5) 0.081(3) Uiso 0.40 d P 2
F35' F 0.6500(8) 0.2433(9) 0.6227(6) 0.084(3) Uiso 0.40 d P 2
P40 P 0.51136(12) 0.32744(11) 0.11624(7) 0.0666(4) Uani 1 d . .
F41 F 0.3938(5) 0.3543(9) 0.1439(4) 0.110(3) Uani 0.60 d PU 1
F42 F 0.4784(4) 0.3124(5) 0.0557(3) 0.081(2) Uani 0.60 d P 1
F43 F 0.4942(12) 0.2190(6) 0.1516(6) 0.186(5) Uani 0.60 d PU 1
F44 F 0.5379(8) 0.3332(9) 0.1788(5) 0.121(4) Uani 0.60 d P 1
F45 F 0.5215(11) 0.4300(7) 0.0809(7) 0.178(5) Uani 0.60 d PU 1
F46 F 0.6240(9) 0.2768(9) 0.0983(5) 0.150(4) Uani 0.60 d PU 1
F41' F 0.4101(9) 0.3986(8) 0.1228(6) 0.075(3) Uiso 0.40 d P 2
F42' F 0.5075(19) 0.2428(18) 0.1055(12) 0.192(8) Uiso 0.40 d P 2
F43' F 0.5131(12) 0.2969(10) 0.1874(8) 0.090(4) Uiso 0.40 d P 2
F44' F 0.5483(10) 0.4332(9) 0.1187(6) 0.104(3) Uiso 0.40 d P 2
F45' F 0.5235(10) 0.3907(10) 0.0405(6) 0.114(4) Uiso 0.40 d P 2
F46' F 0.6297(10) 0.3170(8) 0.0847(6) 0.078(3) Uiso 0.40 d P 2
N80 N 0.7582(3) 0.0195(3) 0.1423(2) 0.0618(11) Uani 1 d . .
C81 C 0.7474(4) 0.0677(4) 0.1744(2) 0.0539(11) Uani 1 d . .
C82 C 0.7329(6) 0.1287(5) 0.2154(3) 0.084(2) Uani 1 d . .
H82A H 0.7413 0.0893 0.2583 0.125 Uiso 1 d R .
H82B H 0.6644 0.1646 0.2181 0.125 Uiso 1 d R .
H82C H 0.7836 0.1737 0.1975 0.125 Uiso 1 d R .
N83 N 0.2660(5) 0.3381(4) -0.0246(2) 0.0798(14) Uani 1 d . .
C84 C 0.2580(5) 0.4013(4) -0.0049(2) 0.0634(13) Uani 1 d . .
C85 C 0.2458(6) 0.4825(5) 0.0210(3) 0.082(2) Uani 1 d . .
H85A H 0.2234 0.5418 -0.0097 0.123 Uiso 1 d R .
H85B H 0.3109 0.4877 0.0290 0.123 Uiso 1 d R .
H85C H 0.1947 0.4719 0.0613 0.123 Uiso 1 d R .
N86 N 0.3550(4) 0.5297(4) 0.5041(2) 0.0681(12) Uani 1 d . .
C87 C 0.3942(4) 0.5917(4) 0.5019(2) 0.0578(12) Uani 1 d . .
C88 C 0.4468(5) 0.6709(5) 0.4981(3) 0.080(2) Uani 1 d . .
H88A H 0.4624 0.6622 0.5397 0.120 Uiso 1 d R .
H88B H 0.4033 0.7319 0.4861 0.120 Uiso 1 d R .
H88C H 0.5103 0.6712 0.4656 0.120 Uiso 1 d R .
N89 N 0.9031(8) 0.1580(6) 0.3794(6) 0.162(4) Uani 1 d . .
C90 C 0.9036(8) 0.0847(6) 0.4101(6) 0.130(4) Uani 1 d . .
C91 C 0.8997(10) -0.0104(7) 0.4537(7) 0.169(5) Uani 1 d U .
H91A H 0.9503 -0.0237 0.4800 0.253 Uiso 1 d R .
H91B H 0.9148 -0.0570 0.4292 0.253 Uiso 1 d R .
H91C H 0.8316 -0.0150 0.4814 0.253 Uiso 1 d 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
N1 0.030(2) 0.034(2) 0.042(2) -0.0065(14) -0.0103(13) -0.0032(13)
C2 0.037(2) 0.032(2) 0.051(2) -0.016(2) -0.009(2) -0.001(2)
C3 0.037(2) 0.038(2) 0.041(2) -0.015(2) -0.007(2) -0.002(2)
C4 0.020(2) 0.034(2) 0.043(2) -0.010(2) -0.0057(15) -0.0039(14)
C5 0.037(2) 0.033(2) 0.046(2) -0.013(2) -0.012(2) -0.006(2)
C6 0.036(2) 0.039(2) 0.040(2) -0.014(2) -0.010(2) -0.006(2)
C7 0.023(2) 0.038(2) 0.041(2) -0.012(2) -0.0083(15) -0.0048(15)
C8 0.046(2) 0.045(2) 0.045(2) -0.014(2) -0.007(2) 0.008(2)
C9 0.052(3) 0.050(3) 0.038(2) -0.014(2) -0.002(2) 0.006(2)
N10 0.033(2) 0.042(2) 0.043(2) -0.0057(15) -0.0053(14) -0.0077(14)
C11 0.043(2) 0.035(2) 0.051(2) -0.011(2) -0.014(2) -0.005(2)
C12 0.039(2) 0.039(2) 0.043(2) -0.012(2) -0.011(2) -0.007(2)
C13 0.046(2) 0.043(2) 0.038(2) -0.001(2) -0.007(2) -0.011(2)
C14 0.045(2) 0.037(2) 0.034(2) -0.001(2) -0.011(2) -0.006(2)
C15 0.054(3) 0.046(2) 0.038(2) -0.015(2) -0.007(2) -0.003(2)
C16 0.056(3) 0.050(2) 0.042(2) -0.013(2) -0.016(2) -0.011(2)
C17 0.048(2) 0.040(2) 0.034(2) 0.000(2) -0.018(2) -0.005(2)
C18 0.044(2) 0.036(2) 0.041(2) -0.007(2) -0.012(2) 0.001(2)
C19 0.046(2) 0.032(2) 0.042(2) -0.005(2) -0.014(2) -0.004(2)
C20 0.048(2) 0.050(3) 0.051(3) 0.001(2) -0.024(2) -0.011(2)
N21 0.033(2) 0.042(2) 0.056(2) -0.007(2) -0.015(2) -0.0067(14)
C22 0.052(3) 0.041(2) 0.054(3) -0.014(2) -0.001(2) 0.000(2)
C23 0.052(3) 0.043(2) 0.051(3) -0.017(2) 0.004(2) -0.003(2)
C24 0.026(2) 0.041(2) 0.046(2) -0.012(2) -0.003(2) -0.008(2)
C25 0.050(2) 0.035(2) 0.055(3) -0.009(2) -0.018(2) -0.008(2)
C26 0.055(3) 0.048(3) 0.053(3) -0.015(2) -0.022(2) -0.009(2)
C27 0.026(2) 0.039(2) 0.049(2) -0.011(2) -0.004(2) -0.006(2)
C28 0.041(2) 0.051(3) 0.052(3) -0.021(2) -0.005(2) 0.002(2)
C29 0.041(2) 0.059(3) 0.048(2) -0.023(2) -0.002(2) -0.004(2)
N30 0.036(2) 0.050(2) 0.043(2) -0.008(2) -0.0019(15) -0.011(2)
C31 0.052(3) 0.039(2) 0.056(3) -0.008(2) -0.010(2) -0.012(2)
C32 0.049(2) 0.044(2) 0.050(2) -0.014(2) -0.010(2) -0.013(2)
C33 0.051(3) 0.059(3) 0.040(2) 0.002(2) -0.002(2) -0.014(2)
C34 0.049(2) 0.043(2) 0.031(2) 0.001(2) -0.006(2) -0.009(2)
N35 0.048(2) 0.037(2) 0.031(2) -0.0046(14) -0.0085(14) -0.0043(15)
C36 0.044(2) 0.030(2) 0.030(2) -0.0025(15) -0.011(2) 0.000(2)
N37 0.048(2) 0.032(2) 0.048(2) -0.0074(15) -0.011(2) -0.003(2)
N38 0.054(2) 0.045(2) 0.048(2) -0.003(2) -0.009(2) -0.016(2)
C39 0.044(2) 0.036(2) 0.045(2) -0.007(2) -0.017(2) -0.001(2)
O41 0.046(2) 0.044(2) 0.051(2) -0.0073(13) -0.0126(13) -0.0075(13)
C42 0.063(3) 0.052(3) 0.067(3) -0.017(2) -0.029(2) -0.004(2)
C43 0.067(3) 0.053(3) 0.081(4) -0.023(3) -0.027(3) -0.011(2)
O44 0.062(2) 0.035(2) 0.061(2) -0.0115(14) -0.019(2) -0.0070(14)
C45 0.092(4) 0.036(2) 0.077(4) -0.020(2) -0.025(3) -0.006(2)
C46 0.076(3) 0.039(2) 0.060(3) -0.018(2) -0.011(3) 0.008(2)
O47 0.061(2) 0.043(2) 0.056(2) -0.0149(14) -0.011(2) 0.0059(14)
C48 0.078(4) 0.046(3) 0.052(3) -0.007(2) -0.015(2) 0.005(2)
C49 0.076(4) 0.038(2) 0.065(3) -0.005(2) -0.026(3) 0.007(2)
O50 0.061(2) 0.039(2) 0.075(2) -0.014(2) -0.020(2) 0.0045(14)
C51 0.055(3) 0.059(3) 0.084(4) -0.031(3) -0.025(3) 0.011(2)
C52 0.050(3) 0.060(3) 0.065(3) -0.027(2) -0.008(2) -0.003(2)
O53 0.062(2) 0.049(2) 0.054(2) -0.0171(14) -0.0161(15) -0.0034(15)
C54 0.034(2) 0.053(3) 0.049(2) -0.011(2) -0.012(2) -0.008(2)
C55 0.035(2) 0.058(3) 0.050(2) -0.021(2) -0.009(2) -0.007(2)
C56 0.033(2) 0.068(3) 0.045(2) -0.013(2) -0.008(2) -0.010(2)
C57 0.032(2) 0.054(3) 0.053(3) -0.008(2) -0.013(2) -0.010(2)
C58 0.042(2) 0.053(3) 0.059(3) -0.020(2) -0.010(2) -0.011(2)
C59 0.039(2) 0.055(3) 0.047(2) -0.014(2) -0.012(2) -0.008(2)
O60 0.057(2) 0.053(2) 0.060(2) -0.006(2) -0.015(2) -0.0072(15)
C61 0.055(3) 0.058(3) 0.073(3) -0.016(3) -0.022(2) -0.011(2)
C62 0.057(3) 0.052(3) 0.083(4) -0.009(3) -0.027(3) -0.017(2)
O63 0.050(2) 0.037(2) 0.081(2) -0.0065(15) -0.027(2) -0.0092(13)
C64 0.051(3) 0.033(2) 0.082(3) -0.007(2) -0.017(2) -0.009(2)
C65 0.045(2) 0.040(2) 0.063(3) -0.006(2) -0.009(2) -0.006(2)
O66 0.045(2) 0.0376(15) 0.055(2) -0.0114(13) -0.0102(13) -0.0057(12)
C67 0.059(3) 0.036(2) 0.066(3) -0.015(2) -0.007(2) -0.005(2)
C68 0.061(3) 0.034(2) 0.060(3) -0.011(2) -0.006(2) 0.003(2)
O69 0.047(2) 0.0364(15) 0.054(2) -0.0062(13) -0.0072(14) -0.0022(12)
C70 0.046(3) 0.049(3) 0.061(3) -0.014(2) -0.004(2) -0.001(2)
C71 0.049(3) 0.051(3) 0.049(3) -0.010(2) -0.003(2) -0.009(2)
O72 0.057(2) 0.042(2) 0.048(2) -0.0023(13) -0.0168(14) -0.0075(14)
C73 0.031(2) 0.042(2) 0.045(2) -0.002(2) -0.012(2) -0.010(2)
C74 0.036(2) 0.044(2) 0.042(2) -0.006(2) -0.007(2) -0.009(2)
C75 0.032(2) 0.048(2) 0.038(2) 0.000(2) -0.008(2) -0.010(2)
C76 0.028(2) 0.042(2) 0.043(2) -0.004(2) -0.007(2) -0.007(2)
C77 0.034(2) 0.056(3) 0.046(2) -0.014(2) -0.010(2) -0.009(2)
C78 0.038(2) 0.050(2) 0.040(2) -0.002(2) -0.012(2) -0.012(2)
P10 0.0778(9) 0.0540(7) 0.0624(8) -0.0300(6) -0.0188(7) 0.0002(6)
F11 0.100(3) 0.121(3) 0.172(5) -0.081(3) -0.078(3) 0.028(3)
F12 0.096(2) 0.067(2) 0.094(2) -0.040(2) -0.005(2) -0.016(2)
F13 0.255(7) 0.084(3) 0.067(2) -0.033(2) -0.031(3) -0.021(3)
F14 0.130(3) 0.090(3) 0.106(3) -0.051(2) -0.015(2) -0.037(2)
F15 0.111(3) 0.084(2) 0.062(2) -0.024(2) -0.016(2) -0.021(2)
F16 0.087(3) 0.069(2) 0.154(4) -0.040(2) -0.001(3) 0.012(2)
P20 0.0712(8) 0.0410(6) 0.0486(7) -0.0152(5) -0.0150(6) 0.0051(6)
F21 0.068(4) 0.115(5) 0.083(5) -0.074(4) -0.016(3) -0.009(3)
F22 0.096(5) 0.082(5) 0.158(9) -0.044(6) -0.032(6) 0.050(5)
F23 0.274(12) 0.135(7) 0.048(4) 0.011(4) -0.018(6) -0.013(8)
F24 0.053(3) 0.076(4) 0.149(7) -0.058(5) -0.030(4) 0.011(3)
F25 0.171(8) 0.098(5) 0.060(4) 0.031(3) -0.055(4) -0.033(5)
F26 0.088(4) 0.087(5) 0.179(8) -0.105(5) 0.006(5) -0.023(4)
P30 0.0727(9) 0.0534(7) 0.0604(8) -0.0145(6) -0.0046(6) -0.0228(6)
F31 0.153(4) 0.217(6) 0.067(2) -0.058(3) 0.013(3) -0.112(4)
F32 0.195(12) 0.187(11) 0.190(15) 0.009(9) -0.052(9) -0.162(10)
F33 0.105(5) 0.054(4) 0.145(7) -0.024(4) -0.006(5) 0.003(3)
F34 0.119(6) 0.120(6) 0.057(3) 0.022(3) -0.035(4) -0.078(5)
F35 0.229(12) 0.058(4) 0.095(5) -0.025(4) -0.093(7) 0.042(6)
F36 0.090(3) 0.122(3) 0.061(2) -0.004(2) -0.008(2) -0.011(2)
P40 0.0752(9) 0.0676(9) 0.0553(8) -0.0327(7) -0.0114(7) 0.0158(7)
F41 0.048(3) 0.201(10) 0.085(5) -0.065(6) 0.006(3) -0.013(5)
F42 0.074(3) 0.127(5) 0.057(3) -0.053(3) -0.015(3) 0.004(3)
F43 0.365(15) 0.090(5) 0.127(7) 0.004(5) -0.075(9) -0.110(8)
F44 0.112(7) 0.192(11) 0.110(7) -0.109(8) -0.054(6) 0.016(7)
F45 0.249(14) 0.094(6) 0.210(12) 0.003(7) -0.110(11) -0.061(7)
F46 0.129(6) 0.176(8) 0.109(6) -0.060(6) -0.028(5) 0.094(6)
N80 0.056(3) 0.056(2) 0.067(3) -0.015(2) -0.013(2) 0.001(2)
C81 0.050(3) 0.048(3) 0.052(3) -0.004(2) -0.010(2) 0.003(2)
C82 0.100(5) 0.073(4) 0.078(4) -0.029(3) -0.016(4) -0.003(3)
N83 0.117(4) 0.064(3) 0.066(3) -0.019(2) -0.031(3) -0.011(3)
C84 0.078(4) 0.060(3) 0.049(3) -0.004(2) -0.020(2) -0.012(3)
C85 0.102(5) 0.077(4) 0.081(4) -0.035(3) -0.028(4) -0.009(3)
N86 0.070(3) 0.079(3) 0.061(3) -0.016(2) -0.018(2) -0.024(3)
C87 0.058(3) 0.071(3) 0.047(3) -0.015(2) -0.018(2) -0.009(3)
C88 0.090(4) 0.083(4) 0.086(4) -0.025(3) -0.033(3) -0.032(3)
N89 0.166(9) 0.084(5) 0.244(12) -0.031(6) -0.073(8) -0.023(5)
C90 0.136(8) 0.058(4) 0.210(11) -0.025(6) -0.075(8) -0.015(5)
C91 0.180(10) 0.110(7) 0.227(12) -0.004(7) -0.108(9) -0.030(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
N1 C6 1.342(5) . ?
N1 C2 1.351(5) . ?
N1 C39 1.491(5) . ?
C2 C3 1.370(6) . ?
C3 C4 1.404(5) . ?
C4 C5 1.388(6) . ?
C4 C7 1.481(5) . ?
C5 C6 1.373(6) . ?
C7 C8 1.395(6) . ?
C7 C12 1.396(6) . ?
C8 C9 1.365(6) . ?
C9 N10 1.341(6) . ?
N10 C11 1.350(6) . ?
N10 C13 1.491(5) . ?
C11 C12 1.372(6) . ?
C13 C14 1.507(6) . ?
C14 C19 1.379(6) . ?
C14 C15 1.388(6) . ?
C15 C16 1.385(7) . ?
C16 C17 1.372(6) . ?
C17 C18 1.387(6) . ?
C17 C20 1.511(6) . ?
C18 C19 1.380(6) . ?
C20 N21 1.504(5) . ?
N21 C26 1.334(6) . ?
N21 C22 1.337(6) . ?
C22 C23 1.357(7) . ?
C23 C24 1.390(6) . ?
C24 C25 1.381(6) . ?
C24 C27 1.492(6) . ?
C25 C26 1.377(6) . ?
C27 C28 1.387(6) . ?
C27 C32 1.396(6) . ?
C28 C29 1.372(7) . ?
C29 N30 1.340(6) . ?
N30 C31 1.339(6) . ?
N30 C33 1.494(6) . ?
C31 C32 1.366(6) . ?
C33 C34 1.493(6) . ?
C34 N38 1.321(6) . ?
C34 N35 1.359(6) . ?
N35 C36 1.331(5) . ?
C36 N37 1.338(5) . ?
C36 C39 1.483(6) . ?
N37 N38 1.346(5) . ?
O41 C76 1.373(5) . ?
O41 C42 1.436(6) . ?
C42 C43 1.496(7) . ?
C43 O44 1.422(6) . ?
O44 C45 1.418(6) . ?
C45 C46 1.490(8) . ?
C46 O47 1.426(6) . ?
O47 C48 1.431(6) . ?
C48 C49 1.477(8) . ?
C49 O50 1.431(6) . ?
O50 C51 1.426(6) . ?
C51 C52 1.486(7) . ?
C52 O53 1.427(6) . ?
O53 C54 1.374(5) . ?
C54 C59 1.377(6) . ?
C54 C55 1.402(6) . ?
C55 C56 1.378(7) . ?
C56 C57 1.384(7) . ?
C57 O60 1.371(6) . ?
C57 C58 1.397(7) . ?
C58 C59 1.377(7) . ?
O60 C61 1.429(6) . ?
C61 C62 1.490(7) . ?
C62 O63 1.422(6) . ?
O63 C64 1.424(5) . ?
C64 C65 1.495(7) . ?
C65 O66 1.431(5) . ?
O66 C67 1.430(6) . ?
C67 C68 1.481(7) . ?
C68 O69 1.416(5) . ?
O69 C70 1.408(5) . ?
C70 C71 1.494(6) . ?
C71 O72 1.432(6) . ?
O72 C73 1.371(5) . ?
C73 C78 1.387(6) . ?
C73 C74 1.397(6) . ?
C74 C75 1.384(6) . ?
C75 C76 1.380(6) . ?
C76 C77 1.397(6) . ?
C77 C78 1.379(6) . ?
P10 F16 1.567(4) . ?
P10 F13 1.574(4) . ?
P10 F14 1.578(4) . ?
P10 F11 1.577(4) . ?
P10 F15 1.581(4) . ?
P10 F12 1.603(4) . ?
P20 F24' 1.465(12) . ?
P20 F22 1.503(8) . ?
P20 F21' 1.510(14) . ?
P20 F25' 1.52(2) . ?
P20 F26 1.539(5) . ?
P20 F23 1.555(7) . ?
P20 F25 1.557(6) . ?
P20 F23' 1.58(2) . ?
P20 F21 1.629(6) . ?
P20 F26' 1.636(15) . ?
P20 F22' 1.648(12) . ?
P20 F24 1.662(6) . ?
P30 F33' 1.42(2) . ?
P30 F32 1.485(12) . ?
P30 F35 1.497(6) . ?
P30 F31 1.574(4) . ?
P30 F34' 1.590(10) . ?
P30 F32' 1.60(2) . ?
P30 F36 1.602(4) . ?
P30 F33 1.613(7) . ?
P30 F34 1.626(6) . ?
P30 F35' 1.682(12) . ?
P40 F42' 1.36(2) . ?
P40 F45 1.476(9) . ?
P40 F43' 1.51(2) . ?
P40 F41' 1.555(12) . ?
P40 F44 1.564(7) . ?
P40 F46 1.570(9) . ?
P40 F43 1.570(8) . ?
P40 F41 1.573(7) . ?
P40 F46' 1.575(13) . ?
P40 F42 1.621(5) . ?
P40 F45' 1.629(13) . ?
P40 F44' 1.751(13) . ?
N80 C81 1.129(7) . ?
C81 C82 1.432(8) . ?
N83 C84 1.128(7) . ?
C84 C85 1.451(8) . ?
N86 C87 1.130(7) . ?
C87 C88 1.457(8) . ?
N89 C90 1.076(11) . ?
C90 C91 1.425(13) . ?

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
C6 N1 C2 120.8(3) . . ?
C6 N1 C39 120.0(3) . . ?
C2 N1 C39 119.1(3) . . ?
N1 C2 C3 120.3(4) . . ?
C2 C3 C4 120.3(4) . . ?
C5 C4 C3 117.6(4) . . ?
C5 C4 C7 121.1(3) . . ?
C3 C4 C7 121.1(3) . . ?
C6 C5 C4 120.2(4) . . ?
N1 C6 C5 120.8(4) . . ?
C8 C7 C12 117.0(4) . . ?
C8 C7 C4 121.5(4) . . ?
C12 C7 C4 121.3(3) . . ?
C9 C8 C7 120.4(4) . . ?
N10 C9 C8 120.7(4) . . ?
C9 N10 C11 120.9(4) . . ?
C9 N10 C13 119.6(4) . . ?
C11 N10 C13 119.1(3) . . ?
N10 C11 C12 119.8(4) . . ?
C11 C12 C7 120.7(4) . . ?
N10 C13 C14 108.9(3) . . ?
C19 C14 C15 119.3(4) . . ?
C19 C14 C13 119.5(4) . . ?
C15 C14 C13 121.1(4) . . ?
C16 C15 C14 120.2(4) . . ?
C17 C16 C15 120.1(4) . . ?
C16 C17 C18 119.9(4) . . ?
C16 C17 C20 120.4(4) . . ?
C18 C17 C20 119.6(4) . . ?
C19 C18 C17 119.9(4) . . ?
C14 C19 C18 120.5(4) . . ?
N21 C20 C17 108.4(3) . . ?
C26 N21 C22 120.7(4) . . ?
C26 N21 C20 119.4(4) . . ?
C22 N21 C20 119.7(4) . . ?
N21 C22 C23 120.7(4) . . ?
C22 C23 C24 120.8(4) . . ?
C25 C24 C23 116.9(4) . . ?
C25 C24 C27 121.1(4) . . ?
C23 C24 C27 121.8(4) . . ?
C26 C25 C24 120.6(4) . . ?
N21 C26 C25 120.2(4) . . ?
C28 C27 C32 117.3(4) . . ?
C28 C27 C24 120.8(4) . . ?
C32 C27 C24 121.5(4) . . ?
C29 C28 C27 120.2(4) . . ?
N30 C29 C28 120.7(4) . . ?
C31 N30 C29 120.5(4) . . ?
C31 N30 C33 118.7(4) . . ?
C29 N30 C33 120.7(4) . . ?
N30 C31 C32 120.7(4) . . ?
C31 C32 C27 120.2(4) . . ?
C34 C33 N30 110.5(3) . . ?
N38 C34 N35 115.1(4) . . ?
N38 C34 C33 120.6(4) . . ?
N35 C34 C33 124.2(4) . . ?
C36 N35 C34 102.4(3) . . ?
N35 C36 N37 109.6(4) . . ?
N35 C36 C39 127.2(4) . . ?
N37 C36 C39 123.2(4) . . ?
C36 N37 N38 110.7(3) . . ?
C34 N38 N37 102.1(4) . . ?
C36 C39 N1 110.0(3) . . ?
C76 O41 C42 116.7(3) . . ?
O41 C42 C43 109.3(4) . . ?
O44 C43 C42 108.8(4) . . ?
C45 O44 C43 111.4(4) . . ?
O44 C45 C46 108.7(4) . . ?
O47 C46 C45 108.2(4) . . ?
C46 O47 C48 115.8(4) . . ?
O47 C48 C49 114.0(4) . . ?
O50 C49 C48 110.0(4) . . ?
C51 O50 C49 111.0(4) . . ?
O50 C51 C52 110.0(4) . . ?
O53 C52 C51 109.2(4) . . ?
C54 O53 C52 117.2(4) . . ?
O53 C54 C59 116.9(4) . . ?
O53 C54 C55 123.8(4) . . ?
C59 C54 C55 119.2(4) . . ?
C56 C55 C54 119.1(4) . . ?
C55 C56 C57 121.5(4) . . ?
O60 C57 C56 115.7(4) . . ?
O60 C57 C58 125.2(4) . . ?
C56 C57 C58 119.1(4) . . ?
C59 C58 C57 119.3(4) . . ?
C58 C59 C54 121.7(4) . . ?
C57 O60 C61 118.0(4) . . ?
O60 C61 C62 108.9(5) . . ?
O63 C62 C61 110.8(4) . . ?
C62 O63 C64 110.6(3) . . ?
O63 C64 C65 110.1(4) . . ?
O66 C65 C64 114.9(4) . . ?
C67 O66 C65 113.3(3) . . ?
O66 C67 C68 109.6(4) . . ?
O69 C68 C67 109.0(4) . . ?
C70 O69 C68 111.8(3) . . ?
O69 C70 C71 108.7(4) . . ?
O72 C71 C70 107.5(4) . . ?
C73 O72 C71 117.9(3) . . ?
O72 C73 C78 116.2(4) . . ?
O72 C73 C74 124.5(4) . . ?
C78 C73 C74 119.4(4) . . ?
C75 C74 C73 119.0(4) . . ?
C76 C75 C74 121.8(4) . . ?
O41 C76 C75 116.1(4) . . ?
O41 C76 C77 124.9(4) . . ?
C75 C76 C77 119.0(4) . . ?
C78 C77 C76 119.6(4) . . ?
C77 C78 C73 121.2(4) . . ?
F16 P10 F13 90.2(3) . . ?
F16 P10 F14 89.8(2) . . ?
F13 P10 F14 91.0(2) . . ?
F16 P10 F11 177.4(2) . . ?
F13 P10 F11 90.4(3) . . ?
F14 P10 F11 92.7(3) . . ?
F16 P10 F15 91.1(2) . . ?
F13 P10 F15 177.4(2) . . ?
F14 P10 F15 91.2(2) . . ?
F11 P10 F15 88.2(3) . . ?
F16 P10 F12 88.6(2) . . ?
F13 P10 F12 89.8(2) . . ?
F14 P10 F12 178.2(3) . . ?
F11 P10 F12 88.9(2) . . ?
F15 P10 F12 88.0(2) . . ?
F24' P20 F21' 89.9(7) . . ?
F24' P20 F25' 98.4(8) . . ?
F21' P20 F25' 99.9(9) . . ?
F22 P20 F26 83.2(5) . . ?
F22 P20 F23 94.3(7) . . ?
F26 P20 F23 106.8(6) . . ?
F22 P20 F25 96.9(6) . . ?
F26 P20 F25 92.4(5) . . ?
F23 P20 F25 158.9(6) . . ?
F24' P20 F23' 96.5(8) . . ?
F21' P20 F23' 106.7(8) . . ?
F25' P20 F23' 149.5(10) . . ?
F22 P20 F21 91.7(5) . . ?
F26 P20 F21 174.8(4) . . ?
F23 P20 F21 74.8(5) . . ?
F25 P20 F21 87.0(5) . . ?
F24' P20 F26' 76.0(7) . . ?
F21' P20 F26' 164.2(7) . . ?
F25' P20 F26' 89.5(9) . . ?
F23' P20 F26' 68.5(8) . . ?
F24' P20 F22' 175.2(6) . . ?
F21' P20 F22' 86.9(7) . . ?
F25' P20 F22' 85.7(8) . . ?
F23' P20 F22' 81.0(7) . . ?
F26' P20 F22' 106.6(7) . . ?
F22 P20 F24 176.8(5) . . ?
F26 P20 F24 93.7(3) . . ?
F23 P20 F24 87.1(6) . . ?
F25 P20 F24 82.7(5) . . ?
F21 P20 F24 91.4(3) . . ?
F32 P30 F35 103.0(9) . . ?
F33' P30 F31 78.9(7) . . ?
F32 P30 F31 84.3(7) . . ?
F35 P30 F31 82.1(4) . . ?
F33' P30 F34' 92.1(8) . . ?
F31 P30 F34' 93.1(4) . . ?
F33' P30 F32' 109.8(9) . . ?
F31 P30 F32' 94.0(7) . . ?
F34' P30 F32' 157.9(7) . . ?
F33' P30 F36 104.0(7) . . ?
F32 P30 F36 98.5(7) . . ?
F35 P30 F36 93.2(4) . . ?
F31 P30 F36 175.0(3) . . ?
F34' P30 F36 82.7(4) . . ?
F32' P30 F36 88.9(7) . . ?
F32 P30 F33 84.5(8) . . ?
F35 P30 F33 172.5(5) . . ?
F31 P30 F33 99.8(4) . . ?
F36 P30 F33 84.7(4) . . ?
F32 P30 F34 165.1(9) . . ?
F35 P30 F34 90.0(6) . . ?
F31 P30 F34 90.2(3) . . ?
F36 P30 F34 88.0(3) . . ?
F33 P30 F34 82.8(4) . . ?
F33' P30 F35' 173.1(8) . . ?
F31 P30 F35' 95.3(5) . . ?
F34' P30 F35' 84.3(5) . . ?
F32' P30 F35' 74.2(7) . . ?
F36 P30 F35' 81.5(4) . . ?
F42' P40 F43' 102.7(12) . . ?
F42' P40 F41' 117.9(12) . . ?
F43' P40 F41' 94.8(7) . . ?
F45 P40 F44 94.3(7) . . ?
F45 P40 F46 102.2(8) . . ?
F44 P40 F46 88.2(6) . . ?
F45 P40 F43 176.0(7) . . ?
F44 P40 F43 88.8(7) . . ?
F46 P40 F43 80.3(8) . . ?
F45 P40 F41 90.8(7) . . ?
F44 P40 F41 90.2(5) . . ?
F46 P40 F41 167.0(7) . . ?
F43 P40 F41 86.7(7) . . ?
F42' P40 F46' 87.9(11) . . ?
F43' P40 F46' 101.4(8) . . ?
F41' P40 F46' 145.6(6) . . ?
F45 P40 F42 90.8(6) . . ?
F44 P40 F42 174.5(6) . . ?
F46 P40 F42 92.7(5) . . ?
F43 P40 F42 86.0(5) . . ?
F41 P40 F42 87.6(4) . . ?
F42' P40 F45' 95.0(12) . . ?
F43' P40 F45' 161.3(7) . . ?
F41' P40 F45' 81.7(6) . . ?
F46' P40 F45' 73.2(7) . . ?
F42' P40 F44' 165.4(11) . . ?
F43' P40 F44' 82.1(6) . . ?
F41' P40 F44' 74.8(6) . . ?
F46' P40 F44' 77.6(6) . . ?
F45' P40 F44' 79.2(7) . . ?
N80 C81 C82 179.6(6) . . ?
N83 C84 C85 179.0(7) . . ?
N86 C87 C88 178.7(6) . . ?
N89 C90 C91 176.5(15) . . ?

_refine_diff_density_max         0.940
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.063

#===END

data_11_4PF6
_database_code_depnum_ccdc_archive 'CCDC 708197'

_audit_creation_method           SHELXL
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_formula_moiety         'C28 H40 O10, C28 H26 N10, 4(F6 P), 5(C2 H3 N)'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_sum            'C66 H81 F24 N15 O10 P4'
_chemical_formula_weight         1824.34
_chemical_melting_point          ?
_chemical_compound_source        ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.5062(6)
_cell_length_b                   16.4849(15)
_cell_length_c                   18.6366(12)
_cell_angle_alpha                98.186(7)
_cell_angle_beta                 92.115(4)
_cell_angle_gamma                104.056(7)
_cell_volume                     3973.1(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    183(2)
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      11.15
_cell_measurement_theta_max      24.03

_exptl_crystal_description       'prismatic blocks'
_exptl_crystal_colour            Red
_exptl_crystal_size_max          0.77
_exptl_crystal_size_mid          0.70
_exptl_crystal_size_min          0.47
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1876
_exptl_absorpt_coefficient_mu    1.968
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      183(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_standards_number         3
_diffrn_standards_interval_count 97
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13790
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.40
_diffrn_reflns_theta_max         63.99
_reflns_number_total             13163
_reflns_number_observed          10254
_reflns_observed_criterion       >2sigma(I)

_computing_data_collection       'Siemens XSCANS'
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'

_refine_special_details          
;
Refinement on F^2^ for ALL reflections except for 784 with very negative F^2^
or flagged by the user for potential systematic errors. Weighted R-factors
wR and all goodnesses 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 observed criterion
of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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.

A distance constraint of 0.90 A was used for the N18-H18 and N36-H36 bonds.

Similar distance restraints were used for all 10 P-F bonds and 4 of the
F-P-F angles in the disordered P40 PF6 anion.

;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      
'calc w=1/[\s^2^(Fo^2^)+(0.0865P)^2^+3.6850P] 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    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00126(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         12379
_refine_ls_number_parameters     1097
_refine_ls_number_restraints     53
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_obs          0.0597
_refine_ls_wR_factor_all         0.1673
_refine_ls_wR_factor_obs         0.1489
_refine_ls_goodness_of_fit_all   1.044
_refine_ls_goodness_of_fit_obs   1.092
_refine_ls_restrained_S_all      1.091
_refine_ls_restrained_S_obs      1.115
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
N1 N 0.0848(2) 0.2958(2) 0.10995(14) 0.0274(5) Uani 1 d . .
C2 C 0.1783(2) 0.3500(2) 0.1283(2) 0.0307(7) Uani 1 d . .
H2A H 0.2145 0.3781 0.0925 0.037 Uiso 1 calc R .
C3 C 0.2205(2) 0.3641(2) 0.1979(2) 0.0309(7) Uani 1 d . .
H3A H 0.2857 0.4025 0.2104 0.037 Uiso 1 calc R .
C4 C 0.1687(2) 0.3224(2) 0.2512(2) 0.0265(6) Uani 1 d . .
C5 C 0.0709(2) 0.2707(2) 0.2312(2) 0.0289(7) Uani 1 d . .
H5A H 0.0316 0.2442 0.2666 0.035 Uiso 1 calc R .
C6 C 0.0310(2) 0.2579(2) 0.1604(2) 0.0285(7) Uani 1 d . .
H6A H -0.0354 0.2218 0.1471 0.034 Uiso 1 calc R .
C7 C 0.2194(2) 0.3280(2) 0.3246(2) 0.0278(6) Uani 1 d . .
C8 C 0.3121(3) 0.3855(2) 0.3472(2) 0.0360(7) Uani 1 d . .
H8A H 0.3385 0.4286 0.3191 0.043 Uiso 1 calc R .
C9 C 0.3661(3) 0.3811(2) 0.4093(2) 0.0379(8) Uani 1 d . .
H9A H 0.4299 0.4208 0.4240 0.045 Uiso 1 calc R .
N10 N 0.3290(2) 0.3205(2) 0.45007(15) 0.0320(6) Uani 1 d . .
C11 C 0.2355(2) 0.2685(2) 0.4334(2) 0.0326(7) Uani 1 d . .
H11A H 0.2081 0.2297 0.4650 0.039 Uiso 1 calc R .
C12 C 0.1789(2) 0.2707(2) 0.3714(2) 0.0294(7) Uani 1 d . .
H12A H 0.1126 0.2336 0.3601 0.035 Uiso 1 calc R .
C13 C 0.3932(3) 0.3100(2) 0.5126(2) 0.0388(8) Uani 1 d . .
H13A H 0.3528 0.3065 0.5558 0.047 Uiso 1 calc R .
H13B H 0.4527 0.3597 0.5240 0.047 Uiso 1 calc R .
C14 C 0.4298(3) 0.2312(2) 0.4951(2) 0.0349(7) Uani 1 d . .
N15 N 0.4953(2) 0.2169(2) 0.4465(2) 0.0374(7) Uani 1 d . .
C16 C 0.5015(3) 0.1368(2) 0.4533(2) 0.0401(8) Uani 1 d . .
N17 N 0.4442(3) 0.1021(2) 0.5022(2) 0.0561(9) Uani 1 d . .
N18 N 0.3989(3) 0.1644(2) 0.5280(2) 0.0531(9) Uani 1 d D .
H18 H 0.3625(44) 0.1499(42) 0.5658(24) 0.121(25) Uiso 1 d D .
C19 C 0.5674(3) 0.0907(3) 0.4095(2) 0.0464(9) Uani 1 d . .
H19A H 0.6364 0.1287 0.4090 0.056 Uiso 1 calc R .
H19B H 0.5747 0.0414 0.4321 0.056 Uiso 1 calc R .
N20 N 0.5211(2) 0.0609(2) 0.3332(2) 0.0382(7) Uani 1 d . .
C21 C 0.4309(3) 0.0032(2) 0.3223(2) 0.0392(8) Uani 1 d . .
H21A H 0.4010 -0.0213 0.3620 0.047 Uiso 1 calc R .
C22 C 0.3815(3) -0.0208(2) 0.2540(2) 0.0345(7) Uani 1 d . .
H22A H 0.3177 -0.0619 0.2469 0.041 Uiso 1 calc R .
C23 C 0.4238(2) 0.0143(2) 0.1948(2) 0.0309(7) Uani 1 d . .
C24 C 0.5220(3) 0.0684(2) 0.2073(2) 0.0378(8) Uani 1 d . .
H24A H 0.5569 0.0898 0.1679 0.045 Uiso 1 calc R .
C25 C 0.5680(3) 0.0906(2) 0.2766(2) 0.0410(8) Uani 1 d . .
H25A H 0.6345 0.1278 0.2847 0.049 Uiso 1 calc R .
C26 C 0.3621(2) 0.0021(2) 0.1241(2) 0.0289(7) Uani 1 d . .
C27 C 0.2609(3) -0.0456(2) 0.1155(2) 0.0342(7) Uani 1 d . .
H27A H 0.2355 -0.0805 0.1505 0.041 Uiso 1 calc R .
C28 C 0.1975(3) -0.0428(2) 0.0575(2) 0.0332(7) Uani 1 d . .
H28A H 0.1283 -0.0749 0.0531 0.040 Uiso 1 calc R .
N29 N 0.2324(2) 0.0048(2) 0.00681(14) 0.0304(6) Uani 1 d . .
C30 C 0.3315(3) 0.0459(2) 0.0100(2) 0.0361(8) Uani 1 d . .
H30A H 0.3562 0.0759 -0.0282 0.043 Uiso 1 calc R .
C31 C 0.3980(3) 0.0455(2) 0.0675(2) 0.0359(8) Uani 1 d . .
H31A H 0.4680 0.0748 0.0687 0.043 Uiso 1 calc R .
C32 C 0.1605(3) 0.0147(2) -0.0522(2) 0.0350(7) Uani 1 d . .
H32A H 0.0933 -0.0259 -0.0516 0.042 Uiso 1 calc R .
H32B H 0.1877 0.0020 -0.1000 0.042 Uiso 1 calc R .
C33 C 0.1472(2) 0.1033(2) -0.0420(2) 0.0290(7) Uani 1 d . .
N34 N 0.0756(2) 0.1290(2) -0.00072(14) 0.0287(6) Uani 1 d . .
C35 C 0.0956(2) 0.2110(2) -0.0058(2) 0.0274(6) Uani 1 d . .
N36 N 0.1728(2) 0.2319(2) -0.0472(2) 0.0337(6) Uani 1 d D .
H36 H 0.2007 0.2834 -0.0587 0.057(13) Uiso 1 d D .
N37 N 0.2071(2) 0.1629(2) -0.0718(2) 0.0367(6) Uani 1 d . .
C38 C 0.0454(2) 0.2747(2) 0.0324(2) 0.0313(7) Uani 1 d . .
H38A H 0.0604 0.3264 0.0094 0.038 Uiso 1 calc R .
H38B H -0.0297 0.2512 0.0287 0.038 Uiso 1 calc R .
O41 O 0.3343(2) 0.2359(2) 0.09813(13) 0.0409(6) Uani 1 d . .
C42 C 0.4357(3) 0.2904(3) 0.0943(2) 0.0513(10) Uani 1 d . .
H42A H 0.4885 0.2608 0.1056 0.062 Uiso 1 calc R .
H42B H 0.4461 0.3425 0.1304 0.062 Uiso 1 calc R .
C43 C 0.4453(3) 0.3125(3) 0.0212(2) 0.0520(10) Uani 1 d . .
H43A H 0.5179 0.3381 0.0144 0.062 Uiso 1 calc R .
H43B H 0.4214 0.2608 -0.0154 0.062 Uiso 1 calc R .
O44 O 0.3856(2) 0.3708(2) 0.01128(15) 0.0458(6) Uani 1 d . .
C45 C 0.4035(3) 0.3994(3) -0.0557(2) 0.0504(10) Uani 1 d . .
H45A H 0.3929 0.3506 -0.0953 0.060 Uiso 1 calc R .
H45B H 0.4749 0.4336 -0.0548 0.060 Uiso 1 calc R .
C46 C 0.3309(3) 0.4518(2) -0.0685(2) 0.0451(9) Uani 1 d . .
H46A H 0.3365 0.4974 -0.0266 0.054 Uiso 1 calc R .
H46B H 0.3465 0.4782 -0.1126 0.054 Uiso 1 calc R .
O47 O 0.2305(2) 0.39710(15) -0.07732(14) 0.0417(6) Uani 1 d . .
C48 C 0.1540(3) 0.4354(2) -0.1025(2) 0.0442(9) Uani 1 d . .
H48A H 0.0866 0.3938 -0.1073 0.053 Uiso 1 calc R .
H48B H 0.1693 0.4501 -0.1513 0.053 Uiso 1 calc R .
C49 C 0.1476(3) 0.5135(2) -0.0529(2) 0.0421(9) Uani 1 d . .
H49A H 0.2105 0.5589 -0.0540 0.051 Uiso 1 calc R .
H49B H 0.0886 0.5334 -0.0698 0.051 Uiso 1 calc R .
O50 O 0.1360(2) 0.49626(14) 0.01935(13) 0.0391(6) Uani 1 d . .
C51 C 0.1303(3) 0.5704(2) 0.0665(2) 0.0460(9) Uani 1 d . .
H51A H 0.0625 0.5817 0.0578 0.055 Uiso 1 calc R .
H51B H 0.1833 0.6193 0.0557 0.055 Uiso 1 calc R .
C52 C 0.1457(3) 0.5609(2) 0.1441(2) 0.0441(9) Uani 1 d . .
H52A H 0.2074 0.5398 0.1513 0.053 Uiso 1 calc R .
H52B H 0.1559 0.6166 0.1754 0.053 Uiso 1 calc R .
O53 O 0.0580(2) 0.5026(2) 0.16408(14) 0.0436(6) Uani 1 d . .
C54 C 0.0590(3) 0.4888(2) 0.2349(2) 0.0387(8) Uani 1 d . .
C55 C 0.1384(3) 0.5258(2) 0.2868(2) 0.0398(8) Uani 1 d . .
H55A H 0.1954 0.5670 0.2752 0.048 Uiso 1 calc R .
C56 C 0.1358(3) 0.5034(2) 0.3560(2) 0.0390(8) Uani 1 d . .
H56A H 0.1913 0.5293 0.3911 0.047 Uiso 1 calc R .
C57 C 0.0534(3) 0.4440(2) 0.3740(2) 0.0369(8) Uani 1 d . .
C58 C -0.0287(3) 0.4080(2) 0.3222(2) 0.0406(8) Uani 1 d . .
H58A H -0.0864 0.3678 0.3342 0.049 Uiso 1 calc R .
C59 C -0.0265(3) 0.4304(2) 0.2538(2) 0.0390(8) Uani 1 d . .
H59A H -0.0832 0.4063 0.2192 0.047 Uiso 1 calc R .
O60 O 0.0468(2) 0.4155(2) 0.44002(14) 0.0441(6) Uani 1 d . .
C61 C 0.1232(3) 0.4615(2) 0.4966(2) 0.0453(9) Uani 1 d . .
H61A H 0.1230 0.5221 0.5040 0.054 Uiso 1 calc R .
H61B H 0.1918 0.4568 0.4823 0.054 Uiso 1 calc R .
C62 C 0.1014(3) 0.4263(2) 0.5656(2) 0.0478(9) Uani 1 d . .
H62A H 0.1298 0.4711 0.6076 0.057 Uiso 1 calc R .
H62B H 0.0265 0.4077 0.5686 0.057 Uiso 1 calc R .
O63 O 0.1451(2) 0.3565(2) 0.56911(13) 0.0434(6) Uani 1 d . .
C64 C 0.1241(3) 0.3239(3) 0.6351(2) 0.0484(9) Uani 1 d . .
H64A H 0.0547 0.2852 0.6300 0.058 Uiso 1 calc R .
H64B H 0.1260 0.3710 0.6750 0.058 Uiso 1 calc R .
C65 C 0.2015(3) 0.2771(3) 0.6532(2) 0.0466(9) Uani 1 d . .
H65A H 0.2699 0.3174 0.6604 0.056 Uiso 1 calc R .
H65B H 0.1862 0.2564 0.6999 0.056 Uiso 1 calc R .
O66 O 0.2058(2) 0.2065(2) 0.59967(13) 0.0397(6) Uani 1 d . .
C67 C 0.1186(3) 0.1365(2) 0.5968(2) 0.0395(8) Uani 1 d . .
H67A H 0.0570 0.1511 0.5774 0.047 Uiso 1 calc R .
H67B H 0.1066 0.1229 0.6463 0.047 Uiso 1 calc R .
C68 C 0.1371(3) 0.0622(2) 0.5492(2) 0.0398(8) Uani 1 d . .
H68A H 0.2024 0.0511 0.5656 0.048 Uiso 1 calc R .
H68B H 0.0812 0.0114 0.5514 0.048 Uiso 1 calc R .
O69 O 0.1412(2) 0.08051(15) 0.47698(12) 0.0365(5) Uani 1 d . .
C70 C 0.1614(3) 0.0125(2) 0.4279(2) 0.0408(8) Uani 1 d . .
H70A H 0.1077 -0.0401 0.4290 0.049 Uiso 1 calc R .
H70B H 0.2283 0.0029 0.4425 0.049 Uiso 1 calc R .
C71 C 0.1626(3) 0.0350(2) 0.3536(2) 0.0407(8) Uani 1 d . .
H71A H 0.1609 -0.0154 0.3173 0.049 Uiso 1 calc R .
H71B H 0.1020 0.0562 0.3428 0.049 Uiso 1 calc R .
O72 O 0.2548(2) 0.09966(15) 0.35030(12) 0.0350(5) Uani 1 d . .
C73 C 0.2697(2) 0.1313(2) 0.2863(2) 0.0310(7) Uani 1 d . .
C74 C 0.1986(2) 0.1109(2) 0.2261(2) 0.0320(7) Uani 1 d . .
H74A H 0.1341 0.0722 0.2274 0.038 Uiso 1 calc R .
C75 C 0.2232(3) 0.1474(2) 0.1649(2) 0.0327(7) Uani 1 d . .
H75A H 0.1749 0.1336 0.1239 0.039 Uiso 1 calc R .
C76 C 0.3168(3) 0.2038(2) 0.1620(2) 0.0328(7) Uani 1 d . .
C77 C 0.3866(3) 0.2250(2) 0.2225(2) 0.0348(7) Uani 1 d . .
H77A H 0.4506 0.2645 0.2216 0.042 Uiso 1 calc R .
C78 C 0.3626(2) 0.1887(2) 0.2837(2) 0.0321(7) Uani 1 d . .
H78A H 0.4106 0.2033 0.3249 0.039 Uiso 1 calc R .
P10 P 0.73073(6) 0.22610(6) 0.07882(5) 0.0360(2) Uani 1 d . .
F11 F 0.7773(2) 0.2219(2) 0.00146(14) 0.0670(7) Uani 1 d . .
F12 F 0.6710(2) 0.2915(2) 0.0569(2) 0.0701(8) Uani 1 d . .
F13 F 0.8261(2) 0.30162(14) 0.11023(15) 0.0587(7) Uani 1 d . .
F14 F 0.7926(2) 0.16002(14) 0.09787(15) 0.0603(7) Uani 1 d . .
F15 F 0.6369(2) 0.1493(2) 0.0469(2) 0.0742(8) Uani 1 d . .
F16 F 0.6843(3) 0.2283(2) 0.1551(2) 0.0846(9) Uani 1 d . .
P20 P 0.85754(7) 0.07958(6) 0.27790(5) 0.0368(2) Uani 1 d . .
F21 F 0.9285(2) 0.08788(15) 0.21093(12) 0.0513(6) Uani 1 d . .
F22 F 0.8361(2) 0.16864(15) 0.27096(14) 0.0610(6) Uani 1 d . .
F23 F 0.9559(2) 0.1273(2) 0.33270(12) 0.0562(6) Uani 1 d . .
F24 F 0.8809(2) -0.0079(2) 0.2860(2) 0.0673(7) Uani 1 d . .
F25 F 0.7607(2) 0.0330(2) 0.22318(12) 0.0519(6) Uani 1 d . .
F26 F 0.7876(2) 0.0729(2) 0.34541(13) 0.0609(7) Uani 1 d . .
P30 P 0.05111(7) 0.78970(6) 0.20956(5) 0.0391(2) Uani 1 d . .
F31 F 0.0569(2) 0.7502(2) 0.12713(13) 0.0712(8) Uani 1 d . .
F32 F 0.0602(2) 0.8792(2) 0.1845(2) 0.0735(8) Uani 1 d . .
F33 F 0.1733(2) 0.8113(2) 0.22030(15) 0.0632(7) Uani 1 d . .
F34 F 0.0431(2) 0.7003(2) 0.2337(2) 0.0692(8) Uani 1 d . .
F35 F -0.0694(2) 0.7685(2) 0.1977(2) 0.0719(8) Uani 1 d . .
F36 F 0.0467(2) 0.8296(2) 0.29150(13) 0.0659(7) Uani 1 d . .
P40 P 0.50045(8) 0.57451(7) 0.26498(7) 0.0516(3) Uani 1 d D .
F41 F 0.6127(2) 0.5815(2) 0.2428(2) 0.1110(14) Uani 1 d D .
F42 F 0.4820(5) 0.6210(5) 0.2024(3) 0.140(2) Uani 0.75 d PD 1
F43 F 0.5381(3) 0.6669(2) 0.3172(2) 0.0691(10) Uani 0.75 d PD 1
F44 F 0.5252(4) 0.5383(4) 0.3363(2) 0.096(2) Uani 0.75 d PD 1
F45 F 0.4670(3) 0.4808(3) 0.2264(4) 0.093(2) Uani 0.75 d PD 1
F42' F 0.5152(13) 0.6669(8) 0.2661(11) 0.095(4) Uiso 0.25 d PD 2
F43' F 0.5296(15) 0.5906(13) 0.3397(8) 0.111(6) Uiso 0.25 d PD 2
F44' F 0.4917(17) 0.4789(11) 0.2705(12) 0.125(7) Uiso 0.25 d PD 2
F45' F 0.4645(15) 0.5365(15) 0.1788(9) 0.126(6) Uiso 0.25 d PD 2
F46 F 0.3866(2) 0.5657(2) 0.2843(2) 0.0924(11) Uani 1 d D .
N80 N 0.5110(3) 0.8681(3) 0.1026(2) 0.0618(10) Uani 1 d . .
C81 C 0.4488(3) 0.8173(3) 0.1193(2) 0.0477(9) Uani 1 d . .
C82 C 0.3693(4) 0.7531(4) 0.1412(3) 0.081(2) Uani 1 d . .
H82A H 0.3750 0.6973 0.1183 0.121 Uiso 1 d R .
H82B H 0.3026 0.7614 0.1262 0.121 Uiso 1 d R .
H82C H 0.3758 0.7568 0.1942 0.121 Uiso 1 d R .
N83 N -0.2183(4) 0.2930(4) 0.4444(4) 0.126(2) Uani 1 d . .
C84 C -0.1600(4) 0.2601(4) 0.4645(3) 0.0753(15) Uani 1 d . .
C85 C -0.0866(4) 0.2188(3) 0.4893(3) 0.0680(13) Uani 1 d . .
H85A H -0.0947 0.1640 0.4583 0.102 Uiso 1 d R .
H85B H -0.0972 0.2101 0.5396 0.102 Uiso 1 d R .
H85C H -0.0174 0.2541 0.4868 0.102 Uiso 1 d R .
N86 N 0.5804(5) 0.8843(3) 0.3219(3) 0.093(2) Uani 1 d . .
C87 C 0.6268(4) 0.8597(3) 0.2785(2) 0.0569(11) Uani 1 d . .
C88 C 0.6846(3) 0.8283(3) 0.2235(2) 0.0564(11) Uani 1 d . .
H88A H 0.7578 0.8513 0.2375 0.085 Uiso 1 d R .
H88B H 0.6677 0.8457 0.1773 0.085 Uiso 1 d R .
H88C H 0.6680 0.7664 0.2178 0.085 Uiso 1 d R .
N89 N 0.3010(4) 0.8691(3) 0.4218(3) 0.099(2) Uani 1 d . .
C90 C 0.3128(4) 0.8065(3) 0.3990(3) 0.0660(12) Uani 1 d . .
C91 C 0.3349(7) 0.7274(5) 0.3749(5) 0.148(4) Uani 1 d . .
H91A H 0.2873 0.6969 0.3333 0.222 Uiso 1 d R .
H91B H 0.3273 0.6936 0.4145 0.222 Uiso 1 d R .
H91C H 0.4052 0.7371 0.3602 0.222 Uiso 1 d R .
N92 N 0.6209(4) 0.4559(4) 0.4685(3) 0.105(2) Uani 1 d . .
C93 C 0.6356(4) 0.4237(4) 0.4133(4) 0.080(2) Uani 1 d . .
C94 C 0.6519(5) 0.3819(5) 0.3412(4) 0.106(2) Uani 1 d . .
H94A H 0.6434 0.3213 0.3418 0.158 Uiso 1 d R .
H94B H 0.7213 0.4070 0.3286 0.158 Uiso 1 d R .
H94C H 0.6020 0.3899 0.3050 0.158 Uiso 1 d 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
N1 0.0256(13) 0.0249(13) 0.0346(14) 0.0037(11) 0.0028(11) 0.0120(10)
C2 0.030(2) 0.027(2) 0.036(2) 0.0067(13) 0.0045(13) 0.0088(13)
C3 0.028(2) 0.025(2) 0.038(2) 0.0027(13) 0.0028(13) 0.0051(13)
C4 0.0264(15) 0.0202(14) 0.035(2) 0.0015(12) 0.0042(13) 0.0121(12)
C5 0.026(2) 0.029(2) 0.033(2) 0.0039(13) 0.0025(13) 0.0109(13)
C6 0.0184(14) 0.027(2) 0.040(2) 0.0054(13) 0.0025(12) 0.0066(12)
C7 0.0251(15) 0.0244(15) 0.034(2) -0.0018(12) 0.0017(13) 0.0099(12)
C8 0.035(2) 0.031(2) 0.039(2) 0.0060(14) -0.0011(14) 0.0030(14)
C9 0.031(2) 0.034(2) 0.042(2) 0.0011(15) -0.0014(15) -0.0010(14)
N10 0.0282(14) 0.0348(15) 0.0318(14) 0.0003(11) 0.0003(11) 0.0086(11)
C11 0.030(2) 0.034(2) 0.033(2) 0.0037(14) 0.0056(13) 0.0073(14)
C12 0.0246(15) 0.030(2) 0.034(2) 0.0027(13) 0.0041(13) 0.0079(13)
C13 0.035(2) 0.048(2) 0.028(2) -0.0036(15) -0.0046(14) 0.008(2)
C14 0.031(2) 0.046(2) 0.026(2) 0.0062(14) -0.0057(13) 0.0063(15)
N15 0.0276(14) 0.046(2) 0.040(2) 0.0092(13) -0.0014(12) 0.0111(13)
C16 0.038(2) 0.045(2) 0.036(2) 0.003(2) -0.0107(15) 0.013(2)
N17 0.085(3) 0.045(2) 0.040(2) 0.0088(15) 0.005(2) 0.018(2)
N18 0.071(2) 0.050(2) 0.038(2) 0.011(2) 0.013(2) 0.012(2)
C19 0.041(2) 0.054(2) 0.046(2) 0.004(2) -0.012(2) 0.021(2)
N20 0.033(2) 0.041(2) 0.043(2) 0.0035(13) -0.0041(13) 0.0191(13)
C21 0.038(2) 0.039(2) 0.043(2) 0.009(2) 0.001(2) 0.014(2)
C22 0.033(2) 0.033(2) 0.038(2) 0.0054(14) 0.0035(14) 0.0096(14)
C23 0.027(2) 0.028(2) 0.041(2) 0.0031(14) 0.0059(13) 0.0150(13)
C24 0.028(2) 0.042(2) 0.047(2) 0.008(2) 0.0063(15) 0.0139(15)
C25 0.023(2) 0.044(2) 0.058(2) 0.007(2) 0.003(2) 0.0120(15)
C26 0.030(2) 0.026(2) 0.035(2) 0.0036(13) 0.0079(13) 0.0154(13)
C27 0.034(2) 0.030(2) 0.039(2) 0.0096(14) 0.0053(14) 0.0065(14)
C28 0.032(2) 0.029(2) 0.037(2) 0.0042(14) 0.0026(14) 0.0062(13)
N29 0.0321(14) 0.0292(13) 0.0324(14) 0.0031(11) 0.0047(11) 0.0131(11)
C30 0.038(2) 0.040(2) 0.034(2) 0.0108(15) 0.0134(14) 0.014(2)
C31 0.026(2) 0.038(2) 0.046(2) 0.011(2) 0.0103(14) 0.0108(14)
C32 0.044(2) 0.034(2) 0.028(2) -0.0003(13) -0.0026(14) 0.0144(15)
C33 0.031(2) 0.034(2) 0.0229(15) 0.0028(13) -0.0024(12) 0.0115(13)
N34 0.0292(13) 0.0307(14) 0.0265(13) 0.0040(11) 0.0002(10) 0.0086(11)
C35 0.0243(15) 0.032(2) 0.026(2) 0.0066(13) -0.0028(12) 0.0082(13)
N36 0.0329(15) 0.0310(15) 0.040(2) 0.0116(12) 0.0051(12) 0.0095(12)
N37 0.036(2) 0.039(2) 0.038(2) 0.0086(13) 0.0083(12) 0.0137(13)
C38 0.029(2) 0.033(2) 0.035(2) 0.0072(14) -0.0012(13) 0.0130(13)
O41 0.0416(14) 0.0517(15) 0.0381(13) 0.0147(11) 0.0073(11) 0.0232(12)
C42 0.034(2) 0.074(3) 0.057(2) 0.025(2) 0.010(2) 0.027(2)
C43 0.044(2) 0.067(3) 0.057(2) 0.017(2) 0.014(2) 0.030(2)
O44 0.0391(14) 0.052(2) 0.055(2) 0.0177(13) 0.0071(12) 0.0227(12)
C45 0.042(2) 0.056(2) 0.055(2) 0.011(2) 0.014(2) 0.014(2)
C46 0.042(2) 0.042(2) 0.051(2) 0.015(2) 0.005(2) 0.004(2)
O47 0.0421(14) 0.0348(13) 0.0474(15) 0.0110(11) -0.0005(11) 0.0060(11)
C48 0.048(2) 0.043(2) 0.041(2) 0.015(2) -0.010(2) 0.008(2)
C49 0.043(2) 0.039(2) 0.047(2) 0.018(2) -0.009(2) 0.011(2)
O50 0.0434(14) 0.0314(12) 0.0434(14) 0.0098(10) -0.0053(11) 0.0100(10)
C51 0.050(2) 0.032(2) 0.059(2) 0.008(2) -0.005(2) 0.017(2)
C52 0.043(2) 0.032(2) 0.055(2) 0.002(2) -0.008(2) 0.010(2)
O53 0.0377(13) 0.0434(14) 0.050(2) 0.0088(12) -0.0098(11) 0.0117(11)
C54 0.037(2) 0.032(2) 0.050(2) 0.000(2) -0.007(2) 0.0201(15)
C55 0.036(2) 0.033(2) 0.049(2) 0.004(2) -0.007(2) 0.0099(15)
C56 0.034(2) 0.033(2) 0.048(2) -0.002(2) -0.009(2) 0.0113(15)
C57 0.037(2) 0.033(2) 0.043(2) -0.0029(15) 0.0002(15) 0.0181(15)
C58 0.030(2) 0.037(2) 0.055(2) -0.002(2) 0.004(2) 0.0141(15)
C59 0.027(2) 0.037(2) 0.053(2) -0.004(2) -0.0075(15) 0.0159(14)
O60 0.0382(14) 0.0430(14) 0.049(2) 0.0016(12) -0.0003(11) 0.0096(11)
C61 0.046(2) 0.040(2) 0.049(2) -0.001(2) -0.004(2) 0.016(2)
C62 0.051(2) 0.045(2) 0.049(2) -0.003(2) 0.007(2) 0.021(2)
O63 0.054(2) 0.0441(14) 0.0363(13) 0.0053(11) 0.0113(11) 0.0202(12)
C64 0.058(2) 0.054(2) 0.034(2) 0.004(2) 0.016(2) 0.017(2)
C65 0.046(2) 0.060(2) 0.031(2) 0.004(2) 0.003(2) 0.010(2)
O66 0.0340(13) 0.0510(15) 0.0362(13) 0.0096(11) 0.0063(10) 0.0125(11)
C67 0.034(2) 0.050(2) 0.038(2) 0.017(2) 0.0060(15) 0.012(2)
C68 0.040(2) 0.045(2) 0.041(2) 0.019(2) 0.007(2) 0.017(2)
O69 0.0432(14) 0.0377(13) 0.0344(12) 0.0122(10) 0.0058(10) 0.0168(11)
C70 0.041(2) 0.033(2) 0.050(2) 0.007(2) 0.009(2) 0.012(2)
C71 0.038(2) 0.037(2) 0.045(2) 0.001(2) 0.005(2) 0.007(2)
O72 0.0333(12) 0.0400(13) 0.0326(12) 0.0057(10) 0.0020(9) 0.0109(10)
C73 0.035(2) 0.032(2) 0.032(2) 0.0028(13) 0.0047(13) 0.0192(14)
C74 0.029(2) 0.035(2) 0.033(2) -0.0009(14) 0.0019(13) 0.0125(14)
C75 0.033(2) 0.039(2) 0.030(2) -0.0024(14) -0.0018(13) 0.0218(15)
C76 0.038(2) 0.037(2) 0.031(2) 0.0040(14) 0.0042(14) 0.0246(15)
C77 0.028(2) 0.036(2) 0.043(2) 0.0061(15) 0.0034(14) 0.0126(14)
C78 0.029(2) 0.036(2) 0.034(2) 0.0030(14) -0.0014(13) 0.0145(14)
P10 0.0245(4) 0.0362(5) 0.0492(5) 0.0133(4) -0.0026(4) 0.0084(4)
F11 0.067(2) 0.083(2) 0.0543(15) 0.0156(13) 0.0138(12) 0.0198(14)
F12 0.0399(13) 0.068(2) 0.118(2) 0.041(2) 0.0023(13) 0.0298(12)
F13 0.0413(12) 0.0372(12) 0.092(2) 0.0002(12) -0.0181(12) 0.0079(10)
F14 0.0602(15) 0.0420(12) 0.081(2) 0.0091(12) -0.0218(13) 0.0224(11)
F15 0.0395(13) 0.063(2) 0.109(2) 0.021(2) -0.0177(14) -0.0105(12)
F16 0.108(2) 0.086(2) 0.070(2) 0.023(2) 0.039(2) 0.033(2)
P20 0.0286(4) 0.0432(5) 0.0382(5) 0.0136(4) -0.0033(4) 0.0048(4)
F21 0.0406(12) 0.0608(14) 0.0484(13) 0.0117(11) 0.0087(10) 0.0025(10)
F22 0.068(2) 0.0481(13) 0.072(2) 0.0124(12) -0.0048(13) 0.0239(12)
F23 0.0347(12) 0.076(2) 0.0500(13) 0.0126(12) -0.0128(10) -0.0002(11)
F24 0.066(2) 0.0541(15) 0.089(2) 0.0286(14) -0.0021(14) 0.0198(13)
F25 0.0340(11) 0.0659(15) 0.0479(13) 0.0068(11) -0.0086(9) 0.0004(10)
F26 0.0407(12) 0.092(2) 0.0460(13) 0.0180(13) 0.0076(10) 0.0040(12)
P30 0.0371(5) 0.0370(5) 0.0408(5) 0.0026(4) 0.0122(4) 0.0054(4)
F31 0.078(2) 0.085(2) 0.0440(14) -0.0045(13) 0.0185(13) 0.0140(15)
F32 0.072(2) 0.058(2) 0.108(2) 0.039(2) 0.040(2) 0.0285(13)
F33 0.0356(12) 0.085(2) 0.072(2) 0.0255(14) 0.0118(11) 0.0116(12)
F34 0.086(2) 0.0446(13) 0.084(2) 0.0225(13) 0.034(2) 0.0197(13)
F35 0.0385(13) 0.096(2) 0.076(2) 0.017(2) 0.0124(12) 0.0052(13)
F36 0.071(2) 0.062(2) 0.0519(14) -0.0131(12) 0.0227(12) 0.0012(13)
P40 0.0349(5) 0.0524(6) 0.0636(7) 0.0163(5) 0.0057(5) -0.0011(4)
F41 0.052(2) 0.112(3) 0.136(3) -0.034(2) 0.041(2) -0.016(2)
F42 0.156(6) 0.187(7) 0.095(4) 0.096(5) 0.004(4) 0.040(5)
F43 0.050(2) 0.061(2) 0.085(3) -0.004(2) 0.004(2) 0.001(2)
F44 0.128(4) 0.097(4) 0.074(3) 0.027(3) -0.015(3) 0.045(3)
F45 0.051(2) 0.071(3) 0.125(4) -0.051(3) 0.011(3) -0.010(2)
F46 0.0391(14) 0.068(2) 0.172(3) 0.021(2) 0.027(2) 0.0119(13)
N80 0.053(2) 0.066(2) 0.071(3) 0.011(2) 0.019(2) 0.022(2)
C81 0.044(2) 0.058(2) 0.047(2) 0.001(2) 0.004(2) 0.027(2)
C82 0.058(3) 0.082(4) 0.106(4) 0.032(3) 0.014(3) 0.012(3)
N83 0.074(4) 0.132(5) 0.196(7) 0.090(5) 0.010(4) 0.037(4)
C84 0.054(3) 0.074(3) 0.100(4) 0.028(3) 0.005(3) 0.011(3)
C85 0.059(3) 0.070(3) 0.075(3) 0.007(3) -0.003(2) 0.020(2)
N86 0.150(5) 0.089(3) 0.066(3) 0.030(3) 0.045(3) 0.062(3)
C87 0.081(3) 0.051(2) 0.044(2) 0.016(2) 0.006(2) 0.023(2)
C88 0.054(2) 0.062(3) 0.053(2) 0.006(2) -0.003(2) 0.015(2)
N89 0.098(4) 0.076(3) 0.139(5) 0.034(3) 0.035(3) 0.041(3)
C90 0.062(3) 0.062(3) 0.073(3) 0.007(2) 0.009(2) 0.013(2)
C91 0.139(7) 0.084(5) 0.195(9) -0.052(5) 0.025(7) 0.020(5)
N92 0.052(3) 0.119(4) 0.116(4) -0.032(4) -0.004(3) -0.003(3)
C93 0.041(3) 0.091(4) 0.096(4) -0.002(3) -0.014(3) 0.009(3)
C94 0.088(5) 0.131(6) 0.100(5) 0.006(4) -0.012(4) 0.041(4)

_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
N1 C6 1.342(4) . ?
N1 C2 1.358(4) . ?
N1 C38 1.484(4) . ?
C2 C3 1.363(5) . ?
C3 C4 1.399(4) . ?
C4 C5 1.392(4) . ?
C4 C7 1.488(4) . ?
C5 C6 1.374(4) . ?
C7 C8 1.384(4) . ?
C7 C12 1.403(4) . ?
C8 C9 1.366(5) . ?
C9 N10 1.352(4) . ?
N10 C11 1.339(4) . ?
N10 C13 1.482(4) . ?
C11 C12 1.372(5) . ?
C13 C14 1.496(5) . ?
C14 N18 1.324(5) . ?
C14 N15 1.327(4) . ?
N15 C16 1.366(5) . ?
C16 N17 1.320(5) . ?
C16 C19 1.498(5) . ?
N17 N18 1.359(5) . ?
C19 N20 1.497(5) . ?
N20 C21 1.339(5) . ?
N20 C25 1.340(5) . ?
C21 C22 1.375(5) . ?
C22 C23 1.394(5) . ?
C23 C24 1.398(5) . ?
C23 C26 1.494(5) . ?
C24 C25 1.374(5) . ?
C26 C27 1.392(5) . ?
C26 C31 1.395(5) . ?
C27 C28 1.367(5) . ?
C28 N29 1.340(4) . ?
N29 C30 1.339(4) . ?
N29 C32 1.493(4) . ?
C30 C31 1.374(5) . ?
C32 C33 1.500(4) . ?
C33 N37 1.316(4) . ?
C33 N34 1.368(4) . ?
N34 C35 1.331(4) . ?
C35 N36 1.327(4) . ?
C35 C38 1.496(4) . ?
N36 N37 1.357(4) . ?
O41 C76 1.375(4) . ?
O41 C42 1.454(5) . ?
C42 C43 1.462(6) . ?
C43 O44 1.422(4) . ?
O44 C45 1.406(5) . ?
C45 C46 1.489(5) . ?
C46 O47 1.424(4) . ?
O47 C48 1.433(4) . ?
C48 C49 1.497(5) . ?
C49 O50 1.422(4) . ?
O50 C51 1.420(4) . ?
C51 C52 1.490(5) . ?
C52 O53 1.430(5) . ?
O53 C54 1.371(5) . ?
C54 C55 1.376(5) . ?
C54 C59 1.404(5) . ?
C55 C56 1.390(5) . ?
C56 C57 1.380(5) . ?
C57 O60 1.375(4) . ?
C57 C58 1.397(5) . ?
C58 C59 1.376(5) . ?
O60 C61 1.436(4) . ?
C61 C62 1.495(6) . ?
C62 O63 1.423(4) . ?
O63 C64 1.422(4) . ?
C64 C65 1.498(6) . ?
C65 O66 1.434(5) . ?
O66 C67 1.429(4) . ?
C67 C68 1.484(5) . ?
C68 O69 1.421(4) . ?
O69 C70 1.428(4) . ?
C70 C71 1.483(5) . ?
C71 O72 1.439(4) . ?
O72 C73 1.370(4) . ?
C73 C78 1.383(5) . ?
C73 C74 1.396(5) . ?
C74 C75 1.380(5) . ?
C75 C76 1.384(5) . ?
C76 C77 1.389(5) . ?
C77 C78 1.376(5) . ?
P10 F16 1.574(3) . ?
P10 F12 1.582(2) . ?
P10 F13 1.584(2) . ?
P10 F15 1.585(2) . ?
P10 F11 1.593(3) . ?
P10 F14 1.595(2) . ?
P20 F24 1.576(3) . ?
P20 F22 1.586(2) . ?
P20 F25 1.591(2) . ?
P20 F26 1.601(2) . ?
P20 F21 1.603(2) . ?
P20 F23 1.609(2) . ?
P30 F35 1.580(3) . ?
P30 F34 1.581(3) . ?
P30 F36 1.583(2) . ?
P30 F32 1.589(3) . ?
P30 F31 1.593(2) . ?
P30 F33 1.600(2) . ?
P40 F43' 1.40(2) . ?
P40 F42' 1.485(13) . ?
P40 F42 1.528(4) . ?
P40 F45 1.558(4) . ?
P40 F41 1.568(3) . ?
P40 F44' 1.57(2) . ?
P40 F46 1.570(3) . ?
P40 F44 1.589(4) . ?
P40 F43 1.641(4) . ?
P40 F45' 1.65(2) . ?
N80 C81 1.120(5) . ?
C81 C82 1.429(7) . ?
N83 C84 1.138(7) . ?
C84 C85 1.430(7) . ?
N86 C87 1.131(6) . ?
C87 C88 1.426(6) . ?
N89 C90 1.111(7) . ?
C90 C91 1.421(8) . ?
N92 C93 1.136(7) . ?
C93 C94 1.470(9) . ?

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
C6 N1 C2 120.6(3) . . ?
C6 N1 C38 120.1(3) . . ?
C2 N1 C38 119.1(3) . . ?
N1 C2 C3 120.2(3) . . ?
C2 C3 C4 120.6(3) . . ?
C5 C4 C3 117.5(3) . . ?
C5 C4 C7 121.2(3) . . ?
C3 C4 C7 121.1(3) . . ?
C6 C5 C4 120.2(3) . . ?
N1 C6 C5 120.7(3) . . ?
C8 C7 C12 117.4(3) . . ?
C8 C7 C4 121.3(3) . . ?
C12 C7 C4 121.1(3) . . ?
C9 C8 C7 120.8(3) . . ?
N10 C9 C8 120.2(3) . . ?
C11 N10 C9 120.6(3) . . ?
C11 N10 C13 119.7(3) . . ?
C9 N10 C13 119.8(3) . . ?
N10 C11 C12 120.9(3) . . ?
C11 C12 C7 119.6(3) . . ?
N10 C13 C14 110.2(3) . . ?
N18 C14 N15 110.2(3) . . ?
N18 C14 C13 122.8(3) . . ?
N15 C14 C13 127.0(3) . . ?
C14 N15 C16 102.5(3) . . ?
N17 C16 N15 114.7(3) . . ?
N17 C16 C19 121.6(4) . . ?
N15 C16 C19 123.7(3) . . ?
C16 N17 N18 102.0(3) . . ?
C14 N18 N17 110.6(3) . . ?
N20 C19 C16 110.5(3) . . ?
C21 N20 C25 120.2(3) . . ?
C21 N20 C19 118.3(3) . . ?
C25 N20 C19 121.5(3) . . ?
N20 C21 C22 120.3(3) . . ?
C21 C22 C23 120.9(3) . . ?
C22 C23 C24 116.8(3) . . ?
C22 C23 C26 121.1(3) . . ?
C24 C23 C26 121.8(3) . . ?
C25 C24 C23 119.7(3) . . ?
N20 C25 C24 121.5(3) . . ?
C27 C26 C31 116.9(3) . . ?
C27 C26 C23 120.6(3) . . ?
C31 C26 C23 122.1(3) . . ?
C28 C27 C26 121.0(3) . . ?
N29 C28 C27 120.4(3) . . ?
C30 N29 C28 120.2(3) . . ?
C30 N29 C32 119.6(3) . . ?
C28 N29 C32 120.2(3) . . ?
N29 C30 C31 121.4(3) . . ?
C30 C31 C26 119.7(3) . . ?
N29 C32 C33 110.4(3) . . ?
N37 C33 N34 115.0(3) . . ?
N37 C33 C32 121.2(3) . . ?
N34 C33 C32 123.8(3) . . ?
C35 N34 C33 101.9(3) . . ?
N36 C35 N34 110.6(3) . . ?
N36 C35 C38 122.6(3) . . ?
N34 C35 C38 126.7(3) . . ?
C35 N36 N37 110.2(3) . . ?
C33 N37 N36 102.3(3) . . ?
N1 C38 C35 109.1(2) . . ?
C76 O41 C42 116.0(3) . . ?
O41 C42 C43 109.2(3) . . ?
O44 C43 C42 109.5(3) . . ?
C45 O44 C43 109.7(3) . . ?
O44 C45 C46 108.3(3) . . ?
O47 C46 C45 107.3(3) . . ?
C46 O47 C48 113.6(3) . . ?
O47 C48 C49 113.1(3) . . ?
O50 C49 C48 110.2(3) . . ?
C51 O50 C49 110.3(3) . . ?
O50 C51 C52 111.2(3) . . ?
O53 C52 C51 109.5(3) . . ?
C54 O53 C52 116.7(3) . . ?
O53 C54 C55 124.7(3) . . ?
O53 C54 C59 116.4(3) . . ?
C55 C54 C59 118.9(4) . . ?
C54 C55 C56 120.7(4) . . ?
C57 C56 C55 120.6(3) . . ?
O60 C57 C56 124.3(3) . . ?
O60 C57 C58 116.7(3) . . ?
C56 C57 C58 118.9(3) . . ?
C59 C58 C57 120.5(3) . . ?
C58 C59 C54 120.3(3) . . ?
C57 O60 C61 116.4(3) . . ?
O60 C61 C62 109.7(3) . . ?
O63 C62 C61 111.1(3) . . ?
C64 O63 C62 110.5(3) . . ?
O63 C64 C65 110.1(3) . . ?
O66 C65 C64 115.2(3) . . ?
C67 O66 C65 112.8(3) . . ?
O66 C67 C68 109.0(3) . . ?
O69 C68 C67 108.1(3) . . ?
C68 O69 C70 111.5(3) . . ?
O69 C70 C71 108.6(3) . . ?
O72 C71 C70 108.1(3) . . ?
C73 O72 C71 117.5(3) . . ?
O72 C73 C78 115.6(3) . . ?
O72 C73 C74 125.1(3) . . ?
C78 C73 C74 119.3(3) . . ?
C75 C74 C73 119.3(3) . . ?
C74 C75 C76 121.3(3) . . ?
O41 C76 C75 116.8(3) . . ?
O41 C76 C77 124.0(3) . . ?
C75 C76 C77 119.2(3) . . ?
C78 C77 C76 119.8(3) . . ?
C77 C78 C73 121.1(3) . . ?
F16 P10 F12 91.0(2) . . ?
F16 P10 F13 91.4(2) . . ?
F12 P10 F13 90.23(14) . . ?
F16 P10 F15 89.2(2) . . ?
F12 P10 F15 90.78(15) . . ?
F13 P10 F15 178.78(15) . . ?
F16 P10 F11 178.9(2) . . ?
F12 P10 F11 89.7(2) . . ?
F13 P10 F11 89.4(2) . . ?
F15 P10 F11 89.9(2) . . ?
F16 P10 F14 91.2(2) . . ?
F12 P10 F14 177.8(2) . . ?
F13 P10 F14 89.77(13) . . ?
F15 P10 F14 89.20(14) . . ?
F11 P10 F14 88.0(2) . . ?
F24 P20 F22 178.8(2) . . ?
F24 P20 F25 90.75(14) . . ?
F22 P20 F25 90.50(14) . . ?
F24 P20 F26 90.4(2) . . ?
F22 P20 F26 89.52(15) . . ?
F25 P20 F26 90.60(13) . . ?
F24 P20 F21 90.20(15) . . ?
F22 P20 F21 89.84(14) . . ?
F25 P20 F21 90.11(13) . . ?
F26 P20 F21 179.05(15) . . ?
F24 P20 F23 89.63(14) . . ?
F22 P20 F23 89.13(14) . . ?
F25 P20 F23 179.45(14) . . ?
F26 P20 F23 89.81(13) . . ?
F21 P20 F23 89.48(13) . . ?
F35 P30 F34 89.9(2) . . ?
F35 P30 F36 90.6(2) . . ?
F34 P30 F36 89.9(2) . . ?
F35 P30 F32 90.5(2) . . ?
F34 P30 F32 179.18(15) . . ?
F36 P30 F32 90.8(2) . . ?
F35 P30 F31 90.0(2) . . ?
F34 P30 F31 90.4(2) . . ?
F36 P30 F31 179.3(2) . . ?
F32 P30 F31 88.9(2) . . ?
F35 P30 F33 179.2(2) . . ?
F34 P30 F33 90.5(2) . . ?
F36 P30 F33 90.12(15) . . ?
F32 P30 F33 89.06(15) . . ?
F31 P30 F33 89.27(15) . . ?
F43' P40 F42' 88.9(11) . . ?
F42 P40 F45 100.8(4) . . ?
F43' P40 F41 93.5(8) . . ?
F42' P40 F41 90.1(6) . . ?
F42 P40 F41 89.0(3) . . ?
F45 P40 F41 90.7(2) . . ?
F43' P40 F44' 86.1(11) . . ?
F42' P40 F44' 174.6(11) . . ?
F41 P40 F44' 88.2(8) . . ?
F43' P40 F46 88.4(8) . . ?
F42' P40 F46 90.6(6) . . ?
F42 P40 F46 89.9(3) . . ?
F45 P40 F46 87.7(2) . . ?
F41 P40 F46 177.9(2) . . ?
F44' P40 F46 91.3(8) . . ?
F42 P40 F44 172.4(4) . . ?
F45 P40 F44 86.7(3) . . ?
F41 P40 F44 90.6(3) . . ?
F46 P40 F44 90.8(3) . . ?
F42 P40 F43 88.2(3) . . ?
F45 P40 F43 171.0(3) . . ?
F41 P40 F43 90.1(2) . . ?
F46 P40 F43 91.6(2) . . ?
F44 P40 F43 84.2(3) . . ?
F43' P40 F45' 169.0(12) . . ?
F42' P40 F45' 102.1(11) . . ?
F41 P40 F45' 86.2(7) . . ?
F44' P40 F45' 82.9(11) . . ?
F46 P40 F45' 91.7(7) . . ?
N80 C81 C82 179.4(4) . . ?
N83 C84 C85 179.6(7) . . ?
N86 C87 C88 179.5(6) . . ?
N89 C90 C91 174.8(7) . . ?
N92 C93 C94 178.5(6) . . ?

_refine_diff_density_max         0.573
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.069

#===END