 
data_99src152 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C48 H52 F6 N2 O11' 
_chemical_formula_weight          946.92 
 
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' 
 
_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                    11.352(2) 
_cell_length_b                    12.894(3) 
_cell_length_c                    17.223(3) 
_cell_angle_alpha                 68.61(3) 
_cell_angle_beta                  83.13(3) 
_cell_angle_gamma                 80.13(3) 
_cell_volume                      2308.1(8) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     75107 
_cell_measurement_theta_min       2.16 
_cell_measurement_theta_max       27.47 
 
_exptl_crystal_description        block 
_exptl_crystal_colour             yellow 
_exptl_crystal_size_max           0.20 
_exptl_crystal_size_mid           0.15 
_exptl_crystal_size_min          0.10 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.362 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              992 
_exptl_absorpt_coefficient_mu     0.112 
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
_exptl_absorpt_process_details    'SORTAV Blessing (1997)'
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'Bruker-Nonius FR591 rotating anode' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Bruker-Nonius KappaCCD' 
_diffrn_measurement_method        'Φ & ω scans' 
_diffrn_detector_area_resol_mean  9.091 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             75107 
_diffrn_reflns_av_R_equivalents   0.0630 
_diffrn_reflns_av_sigmaI/netI     0.0379 
_diffrn_reflns_limit_h_min        -14 
_diffrn_reflns_limit_h_max        14 
_diffrn_reflns_limit_k_min        -16 
_diffrn_reflns_limit_k_max        16 
_diffrn_reflns_limit_l_min        -22 
_diffrn_reflns_limit_l_max        22 
_diffrn_reflns_theta_min          2.16 
_diffrn_reflns_theta_max          27.47 
_reflns_number_total              10538 
_reflns_number_gt                 7412 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'COLLECT (Hooft, 1998)'
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)'
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme 
 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          10538 
_refine_ls_number_parameters      622 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0884 
_refine_ls_R_factor_gt            0.0595 
_refine_ls_wR_factor_ref          0.1843 
_refine_ls_wR_factor_gt           0.1684 
_refine_ls_goodness_of_fit_ref    1.246 
_refine_ls_restrained_S_all       1.246 
_refine_ls_shift/su_max           0.048 
_refine_ls_shift/su_mean          0.003 
 
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
O1 O 0.33356(13) 0.19134(11) 0.01881(8) 0.0359(3) Uani 1 d . . . 
O2 O 0.07446(12) 0.33072(12) -0.10202(8) 0.0400(3) Uani 1 d . . . 
O3 O -0.12758(12) 0.38829(11) -0.00986(9) 0.0385(3) Uani 1 d . . . 
O4 O 0.23186(11) 0.20922(10) 0.55338(8) 0.0292(3) Uani 1 d . . . 
O5 O 0.37945(11) -0.08620(10) 0.45490(8) 0.0305(3) Uani 1 d . . . 
O6 O 0.49665(11) 0.02825(10) 0.30501(8) 0.0291(3) Uani 1 d . . . 
N1 N 0.26511(17) 0.44281(14) -0.07671(10) 0.0343(4) Uani 1 d . . . 
H1 H 0.2246(19) -0.1165(17) 0.6385(13) 0.039(6) Uiso 1 d . . . 
N2 N 0.30865(13) -0.09806(12) 0.63800(9) 0.0246(3) Uani 1 d . . . 
H2 H 0.332(2) 0.453(2) -0.0735(16) 0.049(7) Uiso 1 d . . . 
C1 C 0.32363(19) 0.27898(16) 0.05355(12) 0.0356(4) Uani 1 d . . . 
H1A H 0.4002 0.3063 0.0458 0.043 Uiso 1 calc R . . 
H1B H 0.3026 0.2488 0.1131 0.043 Uiso 1 calc R . . 
C2 C 0.22925(18) 0.37493(16) 0.01168(12) 0.0348(4) Uani 1 d . . . 
H2A H 0.1564 0.3448 0.0121 0.042 Uiso 1 calc R . . 
H2B H 0.2115 0.4243 0.0439 0.042 Uiso 1 calc R . . 
C3 C 0.27186(18) 0.38210(18) -0.13787(12) 0.0383(5) Uani 1 d . . . 
H3A H 0.3249 0.4167 -0.1855 0.046 Uiso 1 calc R . . 
H3B H 0.3075 0.3048 -0.1112 0.046 Uiso 1 calc R . . 
C4 C 0.15438(18) 0.38177(18) -0.16918(12) 0.0404(5) Uani 1 d . . . 
H4A H 0.1198 0.4584 -0.1991 0.049 Uiso 1 calc R . . 
H4B H 0.1672 0.3410 -0.2077 0.049 Uiso 1 calc R . . 
C5 C -0.04399(19) 0.34533(19) -0.12758(14) 0.0431(5) Uani 1 d . . . 
H5A H -0.0471 0.2994 -0.1609 0.052 Uiso 1 calc R . . 
H5B H -0.0679 0.4234 -0.1612 0.052 Uiso 1 calc R . . 
C6 C -0.12602(19) 0.31116(17) -0.05134(15) 0.0426(5) Uani 1 d . . . 
H6A H -0.2060 0.3126 -0.0665 0.051 Uiso 1 calc R . . 
H6B H -0.0979 0.2355 -0.0151 0.051 Uiso 1 calc R . . 
C7 C -0.20471(19) 0.36697(18) 0.06326(14) 0.0445(5) Uani 1 d . . . 
H7A H -0.1859 0.2895 0.0999 0.053 Uiso 1 calc R . . 
H7B H -0.2872 0.3788 0.0488 0.053 Uiso 1 calc R . . 
C8 C -0.18896(19) 0.44530(17) 0.10710(13) 0.0409(5) Uani 1 d . . . 
H8A H -0.2078 0.4096 0.1665 0.049 Uiso 1 calc R . . 
H8B H -0.1055 0.4569 0.0997 0.049 Uiso 1 calc R . . 
C9 C 0.35874(18) 0.08365(15) 0.07489(11) 0.0313(4) Uani 1 d . . . 
C10 C 0.47828(17) 0.03688(16) 0.09008(12) 0.0325(4) Uani 1 d . . . 
C11 C 0.57697(19) 0.09558(18) 0.04884(13) 0.0400(5) Uani 1 d . . . 
H11 H 0.5630 0.1679 0.0098 0.048 Uiso 1 calc R . . 
C12 C 0.6908(2) 0.0464(2) 0.06640(16) 0.0512(6) Uani 1 d . . . 
H12 H 0.7546 0.0847 0.0385 0.061 Uiso 1 calc R . . 
C13 C 0.7140(2) -0.0639(2) 0.12742(17) 0.0555(6) Uani 1 d . . . 
H13 H 0.7925 -0.0961 0.1397 0.067 Uiso 1 calc R . . 
C14 C 0.6233(2) -0.1215(2) 0.16714(15) 0.0484(6) Uani 1 d . . . 
H14 H 0.6401 -0.1927 0.2072 0.058 Uiso 1 calc R . . 
C15 C 0.50142(19) -0.07590(16) 0.14936(12) 0.0363(5) Uani 1 d . . . 
C16 C 0.4069(2) -0.13515(16) 0.18677(12) 0.0384(5) Uani 1 d . . . 
H16 H 0.4229 -0.2083 0.2243 0.046 Uiso 1 calc R . . 
C17 C 0.28860(19) -0.08915(16) 0.17025(12) 0.0367(5) Uani 1 d . . . 
C18 C 0.1894(2) -0.1482(2) 0.21060(15) 0.0502(6) Uani 1 d . . . 
H18 H 0.2038 -0.2215 0.2480 0.060 Uiso 1 calc R . . 
C19 C 0.0752(2) -0.0991(2) 0.19523(18) 0.0601(7) Uani 1 d . . . 
H19 H 0.0122 -0.1384 0.2233 0.072 Uiso 1 calc R . . 
C20 C 0.0509(2) 0.0109(2) 0.13709(18) 0.0578(6) Uani 1 d . . . 
H20 H -0.0281 0.0431 0.1266 0.069 Uiso 1 calc R . . 
C21 C 0.1410(2) 0.07031(19) 0.09645(15) 0.0441(5) Uani 1 d . . . 
H21 H 0.1234 0.1422 0.0574 0.053 Uiso 1 calc R . . 
C22 C 0.26295(18) 0.02370(16) 0.11282(12) 0.0340(4) Uani 1 d . . . 
C23 C 0.24422(17) 0.10364(14) 0.62148(11) 0.0287(4) Uani 1 d . . . 
H23A H 0.1664 0.0820 0.6453 0.034 Uiso 1 calc R . . 
H23B H 0.2885 0.1075 0.6649 0.034 Uiso 1 calc R . . 
C24 C 0.31257(16) 0.02139(14) 0.58237(11) 0.0260(4) Uani 1 d . . . 
H24A H 0.2787 0.0341 0.5300 0.031 Uiso 1 calc R . . 
H24B H 0.3954 0.0350 0.5701 0.031 Uiso 1 calc R . . 
C25 C 0.38441(16) -0.18024(14) 0.60211(11) 0.0262(4) Uani 1 d . . . 
H25A H 0.4660 -0.1630 0.5911 0.031 Uiso 1 calc R . . 
H25B H 0.3857 -0.2556 0.6431 0.031 Uiso 1 calc R . . 
C26 C 0.33918(16) -0.17740(15) 0.52258(11) 0.0285(4) Uani 1 d . . . 
H26A H 0.3688 -0.2475 0.5134 0.034 Uiso 1 calc R . . 
H26B H 0.2523 -0.1686 0.5268 0.034 Uiso 1 calc R . . 
C27 C 0.33682(16) -0.07278(16) 0.37700(11) 0.0300(4) Uani 1 d . . . 
H27A H 0.2506 -0.0712 0.3822 0.036 Uiso 1 calc R . . 
H27B H 0.3730 -0.1351 0.3594 0.036 Uiso 1 calc R . . 
C28 C 0.36954(16) 0.03518(15) 0.31450(12) 0.0306(4) Uani 1 d . . . 
H28A H 0.3377 0.0488 0.2613 0.037 Uiso 1 calc R . . 
H28B H 0.3357 0.0970 0.3333 0.037 Uiso 1 calc R . . 
C29 C 0.53551(18) 0.13321(15) 0.25832(12) 0.0319(4) Uani 1 d . . . 
H29A H 0.4878 0.1917 0.2759 0.038 Uiso 1 calc R . . 
H29B H 0.5255 0.1516 0.1994 0.038 Uiso 1 calc R . . 
C30 C 0.33510(16) -0.12711(15) 0.72811(11) 0.0288(4) Uani 1 d . . . 
H30A H 0.2884 -0.0711 0.7488 0.035 Uiso 1 calc R . . 
H30B H 0.3090 -0.1991 0.7609 0.035 Uiso 1 calc R . . 
C31 C 0.19248(16) 0.30054(14) 0.57886(11) 0.0260(4) Uani 1 d . . . 
C32 C 0.06992(16) 0.33703(14) 0.58457(11) 0.0259(4) Uani 1 d . . . 
C33 C -0.01797(17) 0.28307(15) 0.56672(12) 0.0315(4) Uani 1 d . . . 
H33 H 0.0055 0.2202 0.5513 0.038 Uiso 1 calc R . . 
C34 C -0.13599(18) 0.32388(17) 0.57235(13) 0.0364(5) Uani 1 d . . . 
H34 H -0.1925 0.2883 0.5604 0.044 Uiso 1 calc R . . 
C35 C -0.17493(17) 0.41848(17) 0.59574(12) 0.0353(4) Uani 1 d . . . 
H35 H -0.2564 0.4444 0.5992 0.042 Uiso 1 calc R . . 
C36 C -0.09479(16) 0.47220(16) 0.61325(11) 0.0307(4) Uani 1 d . . . 
H36 H -0.1219 0.5343 0.6291 0.037 Uiso 1 calc R . . 
C37 C 0.03112(15) 0.43462(14) 0.60774(11) 0.0266(4) Uani 1 d . . . 
C38 C 0.11550(16) 0.49023(14) 0.62299(11) 0.0265(4) Uani 1 d . . . 
H38 H 0.0899 0.5534 0.6377 0.032 Uiso 1 calc R . . 
C39 C 0.23808(15) 0.45288(14) 0.61662(11) 0.0247(4) Uani 1 d . . . 
C40 C 0.32548(16) 0.50947(15) 0.63222(12) 0.0301(4) Uani 1 d . . . 
H40 H 0.3006 0.5719 0.6480 0.036 Uiso 1 calc R . . 
C41 C 0.44441(17) 0.47325(17) 0.62437(13) 0.0350(4) Uani 1 d . . . 
H41 H 0.5002 0.5109 0.6347 0.042 Uiso 1 calc R . . 
C42 C 0.48372(17) 0.37805(16) 0.60044(13) 0.0349(4) Uani 1 d . . . 
H42 H 0.5653 0.3544 0.5946 0.042 Uiso 1 calc R . . 
C43 C 0.40383(16) 0.32088(15) 0.58598(12) 0.0312(4) Uani 1 d . . . 
H43 H 0.4313 0.2582 0.5710 0.037 Uiso 1 calc R . . 
C44 C 0.27819(15) 0.35617(14) 0.59358(11) 0.0252(4) Uani 1 d . . . 
C45 C 1.0603(2) 0.2476(2) 0.2848(2) 0.0622(8) Uani 1 d . . . 
C46 C 0.93480(18) 0.21725(16) 0.31312(12) 0.0349(4) Uani 1 d . . . 
C47 C 0.36452(18) 0.46455(18) 0.21248(14) 0.0394(5) Uani 1 d . . . 
C48 C 0.48809(19) 0.46469(16) 0.17046(13) 0.0366(5) Uani 1 d . . . 
F1 F 1.12680(15) 0.1867(2) 0.25001(17) 0.1118(8) Uani 1 d . . . 
F2 F 1.06340(19) 0.35414(19) 0.2551(3) 0.1512(14) Uani 1 d . . . 
F3 F 1.12497(18) 0.2292(3) 0.35110(19) 0.1135(14) Uani 0.780(5) d P . . 
F3' F 1.0548(5) 0.3011(8) 0.1907(5) 0.088(4) Uani 0.220(5) d P . . 
F4 F 0.31651(13) 0.56600(13) 0.21553(11) 0.0706(4) Uani 1 d . . . 
F5 F 0.28808(13) 0.43969(17) 0.17092(11) 0.0824(6) Uani 1 d . . . 
F6 F 0.35610(12) 0.39455(13) 0.29150(9) 0.0643(4) Uani 1 d . . . 
O7 O 0.85211(12) 0.29581(12) 0.29873(10) 0.0463(4) Uani 1 d . . . 
O8 O 0.92754(14) 0.11501(13) 0.34928(11) 0.0536(4) Uani 1 d . . . 
O9 O 0.49871(14) 0.53648(15) 0.10043(10) 0.0553(4) Uani 1 d . . . 
O10 O 0.56843(13) 0.39512(12) 0.21291(11) 0.0505(4) Uani 1 d . . . 
O11 O 0.9340(4) 0.0411(5) 0.5211(3) 0.146(2) Uani 0.60 d P . . 
 
 
_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 
O1 C9 1.376(2) . ? 
O1 C1 1.443(2) . ? 
O2 C4 1.412(3) . ? 
O2 C5 1.425(2) . ? 
O3 C7 1.412(3) . ? 
O3 C6 1.417(2) . ? 
O4 C31 1.389(2) . ? 
O4 C23 1.435(2) . ? 
O5 C26 1.417(2) . ? 
O5 C27 1.422(2) . ? 
O6 C29 1.414(2) . ? 
O6 C28 1.424(2) . ? 
N1 C8 1.494(2) 2_565 ? 
N1 C2 1.500(2) . ? 
N1 C3 1.513(3) . ? 
N2 C24 1.493(2) . ? 
N2 C25 1.511(2) . ? 
N2 C30 1.513(2) . ? 
C1 C2 1.509(3) . ? 
C3 C4 1.498(3) . ? 
C5 C6 1.487(3) . ? 
C7 C8 1.508(3) . ? 
C8 N1 1.494(2) 2_565 ? 
C9 C22 1.399(3) . ? 
C9 C10 1.401(3) . ? 
C10 C11 1.429(3) . ? 
C10 C15 1.441(3) . ? 
C11 C12 1.356(3) . ? 
C12 C13 1.430(4) . ? 
C13 C14 1.342(4) . ? 
C14 C15 1.430(3) . ? 
C15 C16 1.381(3) . ? 
C16 C17 1.390(3) . ? 
C17 C18 1.432(3) . ? 
C17 C22 1.433(3) . ? 
C18 C19 1.352(4) . ? 
C19 C20 1.410(4) . ? 
C20 C21 1.352(3) . ? 
C21 C22 1.429(3) . ? 
C23 C24 1.515(2) . ? 
C25 C26 1.505(2) . ? 
C27 C28 1.491(3) . ? 
C29 C30 1.499(3) 2_656 ? 
C30 C29 1.499(3) 2_656 ? 
C31 C32 1.394(3) . ? 
C31 C44 1.399(2) . ? 
C32 C33 1.429(2) . ? 
C32 C37 1.439(2) . ? 
C33 C34 1.359(3) . ? 
C34 C35 1.406(3) . ? 
C35 C36 1.353(3) . ? 
C36 C37 1.432(3) . ? 
C37 C38 1.391(2) . ? 
C38 C39 1.397(2) . ? 
C39 C44 1.429(2) . ? 
C39 C40 1.430(2) . ? 
C40 C41 1.358(3) . ? 
C41 C42 1.419(3) . ? 
C42 C43 1.358(3) . ? 
C43 C44 1.426(2) . ? 
C45 F1 1.256(3) . ? 
C45 F2 1.284(3) . ? 
C45 F3 1.358(4) . ? 
C45 F3' 1.517(8) . ? 
C45 C46 1.519(3) . ? 
C46 O7 1.231(2) . ? 
C46 O8 1.248(2) . ? 
C47 F6 1.334(3) . ? 
C47 F5 1.334(2) . ? 
C47 F4 1.345(3) . ? 
C47 C48 1.500(3) . ? 
C48 O9 1.231(3) . ? 
C48 O10 1.254(2) . ? 
F1 F3' 1.605(7) . ? 
F2 F3' 1.520(11) . ? 
 
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 
C9 O1 C1 114.98(13) . . ? 
C4 O2 C5 112.07(15) . . ? 
C7 O3 C6 113.59(16) . . ? 
C31 O4 C23 113.29(13) . . ? 
C26 O5 C27 113.62(13) . . ? 
C29 O6 C28 112.59(14) . . ? 
C8 N1 C2 112.07(15) 2_565 . ? 
C8 N1 C3 110.99(16) 2_565 . ? 
C2 N1 C3 114.45(16) . . ? 
C24 N2 C25 112.45(14) . . ? 
C24 N2 C30 116.21(13) . . ? 
C25 N2 C30 110.27(13) . . ? 
O1 C1 C2 110.48(15) . . ? 
N1 C2 C1 113.77(16) . . ? 
C4 C3 N1 115.23(17) . . ? 
O2 C4 C3 110.53(16) . . ? 
O2 C5 C6 108.19(17) . . ? 
O3 C6 C5 107.62(16) . . ? 
O3 C7 C8 108.99(17) . . ? 
N1 C8 C7 114.03(18) 2_565 . ? 
O1 C9 C22 118.15(17) . . ? 
O1 C9 C10 119.38(18) . . ? 
C22 C9 C10 122.44(17) . . ? 
C9 C10 C11 122.88(18) . . ? 
C9 C10 C15 117.94(19) . . ? 
C11 C10 C15 119.18(18) . . ? 
C12 C11 C10 120.3(2) . . ? 
C11 C12 C13 120.6(2) . . ? 
C14 C13 C12 120.5(2) . . ? 
C13 C14 C15 121.6(2) . . ? 
C16 C15 C14 122.7(2) . . ? 
C16 C15 C10 119.61(18) . . ? 
C14 C15 C10 117.7(2) . . ? 
C15 C16 C17 122.22(18) . . ? 
C16 C17 C18 122.87(19) . . ? 
C16 C17 C22 119.29(19) . . ? 
C18 C17 C22 117.8(2) . . ? 
C19 C18 C17 121.2(2) . . ? 
C18 C19 C20 120.6(2) . . ? 
C21 C20 C19 120.8(2) . . ? 
C20 C21 C22 120.7(2) . . ? 
C9 C22 C21 122.67(18) . . ? 
C9 C22 C17 118.47(18) . . ? 
C21 C22 C17 118.85(19) . . ? 
O4 C23 C24 104.23(14) . . ? 
N2 C24 C23 112.27(15) . . ? 
C26 C25 N2 112.85(14) . . ? 
O5 C26 C25 109.10(14) . . ? 
O5 C27 C28 107.98(14) . . ? 
O6 C28 C27 108.83(14) . . ? 
O6 C29 C30 109.22(14) . 2_656 ? 
C29 C30 N2 114.47(15) 2_656 . ? 
O4 C31 C32 119.10(15) . . ? 
O4 C31 C44 118.39(15) . . ? 
C32 C31 C44 122.42(16) . . ? 
C31 C32 C33 122.76(16) . . ? 
C31 C32 C37 118.28(15) . . ? 
C33 C32 C37 118.95(16) . . ? 
C34 C33 C32 119.80(18) . . ? 
C33 C34 C35 121.71(17) . . ? 
C36 C35 C34 120.50(18) . . ? 
C35 C36 C37 120.87(18) . . ? 
C38 C37 C36 122.03(17) . . ? 
C38 C37 C32 119.80(16) . . ? 
C36 C37 C32 118.17(16) . . ? 
C37 C38 C39 121.22(16) . . ? 
C38 C39 C44 119.72(16) . . ? 
C38 C39 C40 121.61(16) . . ? 
C44 C39 C40 118.66(16) . . ? 
C41 C40 C39 120.91(17) . . ? 
C40 C41 C42 120.17(17) . . ? 
C43 C42 C41 120.94(17) . . ? 
C42 C43 C44 120.62(17) . . ? 
C31 C44 C43 122.75(16) . . ? 
C31 C44 C39 118.55(16) . . ? 
C43 C44 C39 118.69(16) . . ? 
F1 C45 F2 118.7(3) . . ? 
F1 C45 F3 100.1(2) . . ? 
F2 C45 F3 94.5(3) . . ? 
F1 C45 F3' 70.0(4) . . ? 
F2 C45 F3' 65.1(4) . . ? 
F3 C45 F3' 145.4(4) . . ? 
F1 C45 C46 115.7(2) . . ? 
F2 C45 C46 113.2(2) . . ? 
F3 C45 C46 111.1(2) . . ? 
F3' C45 C46 102.8(3) . . ? 
O7 C46 O8 127.4(2) . . ? 
O7 C46 C45 116.65(18) . . ? 
O8 C46 C45 115.97(18) . . ? 
F6 C47 F5 106.96(18) . . ? 
F6 C47 F4 104.58(18) . . ? 
F5 C47 F4 104.69(18) . . ? 
F6 C47 C48 115.53(17) . . ? 
F5 C47 C48 111.65(18) . . ? 
F4 C47 C48 112.60(18) . . ? 
O9 C48 O10 128.3(2) . . ? 
O9 C48 C47 115.97(19) . . ? 
O10 C48 C47 115.66(18) . . ? 
C45 F1 F3' 62.6(4) . . ? 
C45 F2 F3' 64.9(3) . . ? 
C45 F3' F2 50.0(3) . . ? 
C45 F3' F1 47.3(2) . . ? 
F2 F3' F1 88.7(4) . . ? 
 
_diffrn_measured_fraction_theta_max    0.996 
_diffrn_reflns_theta_full              27.47 
_diffrn_measured_fraction_theta_full   0.996 
_refine_diff_density_max    0.561 
_refine_diff_density_min   -0.719 
_refine_diff_density_rms    0.059 
