 
data_02sot043 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
Phil Gale 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C62 H90 F N9 O10' 
_chemical_formula_weight          1140.43 
 
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                    13.408(5) 
_cell_length_b                    15.847(5) 
_cell_length_c                    17.023(5) 
_cell_angle_alpha                 73.042(5) 
_cell_angle_beta                  74.733(5) 
_cell_angle_gamma                 68.046(5) 
_cell_volume                      3159.9(18) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     120(2) 
_cell_measurement_reflns_used     8376
_cell_measurement_theta_min       1.02
_cell_measurement_theta_max       26.02
 
_exptl_crystal_description        block
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.06 
_exptl_crystal_size_mid           0.04 
_exptl_crystal_size_min           0.01 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.199 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1228 
_exptl_absorpt_coefficient_mu     0.084 
_exptl_absorpt_correction_type    multiscans 
_exptl_absorpt_correction_T_min   0.9950 
_exptl_absorpt_correction_T_max   0.9992 
_exptl_absorpt_process_details    'SORTAV (Blessing, 1997)'
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       120(2) 
_diffrn_radiation_wavelength      0.71069 
_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             19191 
_diffrn_reflns_av_R_equivalents   0.2915 
_diffrn_reflns_av_sigmaI/netI     0.7011 
_diffrn_reflns_limit_h_min        -15 
_diffrn_reflns_limit_h_max        15 
_diffrn_reflns_limit_k_min        -18 
_diffrn_reflns_limit_k_max        18 
_diffrn_reflns_limit_l_min        -17 
_diffrn_reflns_limit_l_max        18 
_diffrn_reflns_theta_min          3.07 
_diffrn_reflns_theta_max          25.02 
_reflns_number_total              8690 
_reflns_number_gt                 1664 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)'
_computing_cell_refinement        'DENZO & COLLECT'
_computing_data_reduction         'DENZO & COLLECT'
_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  
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.1447P)²+0.0000P] where P=(Fo²+2Fc²)/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        0.0101(18) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_number_reflns          8690 
_refine_ls_number_parameters      700 
_refine_ls_number_restraints      378 
_refine_ls_R_factor_all           0.4882 
_refine_ls_R_factor_gt            0.1467 
_refine_ls_wR_factor_ref          0.4036 
_refine_ls_wR_factor_gt           0.2700 
_refine_ls_goodness_of_fit_ref    0.812 
_refine_ls_restrained_S_all       0.797 
_refine_ls_shift/su_max           0.001 
_refine_ls_shift/su_mean          0.000 
 
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
F1 F 0.4148(4) 0.6483(3) 0.1885(3) 0.0009(14) Uani 1 1 d U . . 
O1 O 0.0534(11) 0.3354(11) 0.2163(10) 0.106(5) Uani 1 1 d . . . 
O2 O -0.0675(11) 0.4582(10) 0.1568(9) 0.089(4) Uani 1 1 d . . . 
O3 O -0.0121(13) 0.7550(10) 0.0819(10) 0.105(5) Uani 1 1 d . . . 
O4 O 0.1319(13) 0.7687(10) 0.1068(10) 0.099(5) Uani 1 1 d . . . 
O5 O 0.3589(9) 0.2978(8) 0.2796(7) 0.069(4) Uani 1 1 d . . . 
O6 O 0.7710(8) 0.4187(7) 0.3440(7) 0.060(3) Uani 1 1 d . . . 
O7 O 0.5357(12) 0.8643(8) 0.1166(9) 0.084(5) Uani 1 1 d . . . 
O8 O 0.6364(11) 0.9281(10) 0.1467(10) 0.108(5) Uani 1 1 d . . . 
O9 O 0.9376(11) 0.7350(10) 0.2852(9) 0.090(5) Uani 1 1 d . . . 
O10 O 0.9487(10) 0.5923(10) 0.3515(9) 0.083(4) Uani 1 1 d . . . 
N1 N 0.0152(14) 0.4197(12) 0.1887(11) 0.074(5) Uani 1 1 d . . . 
N2 N 0.0768(19) 0.7231(13) 0.1079(12) 0.100(6) Uani 1 1 d . . . 
N3 N 0.3396(9) 0.4538(8) 0.2390(9) 0.058(4) Uani 1 1 d . . . 
H3 H 0.3733 0.4931 0.2358 0.069 Uiso 1 1 calc R . . 
N4 N 0.5299(10) 0.4188(9) 0.2927(8) 0.054(4) Uani 1 1 d . . . 
N5 N 0.6448(10) 0.5353(8) 0.2724(8) 0.050(4) Uani 1 1 d . . . 
H5 H 0.5842 0.5482 0.2541 0.060 Uiso 1 1 calc R . . 
N6 N 0.6060(14) 0.8600(11) 0.1500(10) 0.072(5) Uani 1 1 d . . . 
N7 N 0.9067(12) 0.6653(13) 0.3070(11) 0.066(4) Uani 1 1 d . . . 
C1 C 0.1808(9) 0.4354(5) 0.2159(7) 0.067(5) Uani 1 1 d GU . . 
H1 H 0.2055 0.3706 0.2400 0.080 Uiso 1 1 calc R . . 
C2 C 0.0831(8) 0.4744(7) 0.1855(7) 0.058(5) Uani 1 1 d GU . . 
C3 C 0.0470(7) 0.5692(7) 0.1502(7) 0.060(5) Uani 1 1 d GU . . 
H3A H -0.0198 0.5959 0.1293 0.072 Uiso 1 1 calc R . . 
C4 C 0.1085(9) 0.6248(5) 0.1454(7) 0.062(5) Uani 1 1 d GU . . 
C5 C 0.2062(8) 0.5858(7) 0.1759(7) 0.050(4) Uani 1 1 d GU . . 
H5A H 0.2482 0.6238 0.1726 0.061 Uiso 1 1 calc R . . 
C6 C 0.2423(7) 0.4910(7) 0.2112(7) 0.059(5) Uani 1 1 d GU . . 
C7 C 0.3902(14) 0.3625(14) 0.2711(11) 0.061(5) Uani 1 1 d U . . 
C8 C 0.4985(14) 0.3433(12) 0.2986(11) 0.061(5) Uani 1 1 d U . . 
C9 C 0.5810(12) 0.2596(10) 0.3207(10) 0.049(4) Uani 1 1 d U . . 
C10 C 0.6655(12) 0.2836(11) 0.3351(10) 0.051(4) Uani 1 1 d U . . 
C11 C 0.6309(14) 0.3816(11) 0.3116(10) 0.053(5) Uani 1 1 d U . . 
C12 C 0.6917(14) 0.4432(12) 0.3125(11) 0.053(5) Uani 1 1 d U . . 
C13 C 0.6851(9) 0.6092(6) 0.2586(7) 0.053(5) Uani 1 1 d GU . . 
C14 C 0.6300(7) 0.6950(8) 0.2129(7) 0.064(5) Uani 1 1 d GU . . 
H14 H 0.5681 0.7016 0.1917 0.077 Uiso 1 1 calc R . . 
C15 C 0.6655(8) 0.7710(6) 0.1984(6) 0.058(5) Uani 1 1 d GU . . 
C16 C 0.7561(9) 0.7613(6) 0.2295(7) 0.062(5) Uani 1 1 d GU . . 
H16 H 0.7804 0.8132 0.2196 0.075 Uiso 1 1 calc R . . 
C17 C 0.8112(7) 0.6755(8) 0.2752(7) 0.053(5) Uani 1 1 d GU . . 
C18 C 0.7757(8) 0.5995(6) 0.2898(6) 0.061(5) Uani 1 1 d GU . . 
H18 H 0.8133 0.5409 0.3210 0.073 Uiso 1 1 calc R . . 
C19 C 0.5865(9) 0.1610(5) 0.3275(7) 0.055(5) Uani 1 1 d GU . . 
C20 C 0.5052(7) 0.1261(7) 0.3792(7) 0.055(5) Uani 1 1 d GU . . 
H20 H 0.4436 0.1653 0.4088 0.066 Uiso 1 1 calc R . . 
C21 C 0.5141(8) 0.0337(7) 0.3877(6) 0.064(5) Uani 1 1 d GU . . 
H21 H 0.4585 0.0099 0.4231 0.077 Uiso 1 1 calc R . . 
C22 C 0.6042(9) -0.0237(6) 0.3445(7) 0.070(5) Uani 1 1 d GU . . 
H22 H 0.6103 -0.0868 0.3503 0.084 Uiso 1 1 calc R . . 
C23 C 0.6856(8) 0.0112(7) 0.2927(7) 0.078(6) Uani 1 1 d GU . . 
H23 H 0.7472 -0.0281 0.2631 0.094 Uiso 1 1 calc R . . 
C24 C 0.6767(8) 0.1035(7) 0.2842(6) 0.056(5) Uani 1 1 d GU . . 
H24 H 0.7323 0.1274 0.2488 0.067 Uiso 1 1 calc R . . 
C25 C 0.7695(7) 0.2157(6) 0.3560(7) 0.043(4) Uani 1 1 d GU . . 
C26 C 0.7702(7) 0.1374(7) 0.4199(6) 0.057(5) Uani 1 1 d GU . . 
H26 H 0.7032 0.1293 0.4514 0.069 Uiso 1 1 calc R . . 
C27 C 0.8688(9) 0.0710(6) 0.4377(6) 0.070(5) Uani 1 1 d GU . . 
H27 H 0.8693 0.0175 0.4814 0.084 Uiso 1 1 calc R . . 
C28 C 0.9667(7) 0.0829(7) 0.3916(7) 0.076(6) Uani 1 1 d GU . . 
H28 H 1.0341 0.0375 0.4038 0.091 Uiso 1 1 calc R . . 
C29 C 0.9661(7) 0.1612(8) 0.3278(7) 0.074(6) Uani 1 1 d GU . . 
H29 H 1.0330 0.1693 0.2963 0.089 Uiso 1 1 calc R . . 
C30 C 0.8675(9) 0.2276(6) 0.3100(6) 0.062(5) Uani 1 1 d GU . . 
H30 H 0.8670 0.2811 0.2663 0.075 Uiso 1 1 calc R . . 
N8 N 0.5208(11) 0.2181(10) 0.0658(9) 0.067(4) Uani 1 1 d . . . 
C31 C 0.4719(13) 0.1605(11) 0.1411(11) 0.057(5) Uani 1 1 d U . . 
H31A H 0.4203 0.2034 0.1770 0.069 Uiso 1 1 calc R . . 
H31B H 0.5314 0.1187 0.1723 0.069 Uiso 1 1 calc R . . 
C32 C 0.4121(13) 0.1010(10) 0.1316(10) 0.055(5) Uani 1 1 d U . . 
H32A H 0.3471 0.1419 0.1062 0.066 Uiso 1 1 calc R . . 
H32B H 0.4604 0.0599 0.0933 0.066 Uiso 1 1 calc R . . 
C33 C 0.3766(14) 0.0424(11) 0.2131(11) 0.069(5) Uani 1 1 d U . . 
H33A H 0.4408 0.0053 0.2406 0.083 Uiso 1 1 calc R . . 
H33B H 0.3480 -0.0017 0.2022 0.083 Uiso 1 1 calc R . . 
C34 C 0.2873(15) 0.1009(13) 0.2731(12) 0.088(6) Uani 1 1 d U . . 
H34A H 0.2194 0.1300 0.2502 0.132 Uiso 1 1 calc R . . 
H34B H 0.3117 0.1493 0.2792 0.132 Uiso 1 1 calc R . . 
H34C H 0.2744 0.0602 0.3278 0.132 Uiso 1 1 calc R . . 
C35 C 0.6099(14) 0.1570(12) 0.0097(12) 0.071(5) Uani 1 1 d U . . 
H35A H 0.6288 0.1968 -0.0449 0.085 Uiso 1 1 calc R . . 
H35B H 0.5815 0.1123 -0.0001 0.085 Uiso 1 1 calc R . . 
C36 C 0.7142(13) 0.1025(11) 0.0490(11) 0.067(5) Uani 1 1 d U . . 
H36A H 0.7444 0.1470 0.0571 0.080 Uiso 1 1 calc R . . 
H36B H 0.6954 0.0637 0.1042 0.080 Uiso 1 1 calc R . . 
C37 C 0.7996(15) 0.0406(13) -0.0068(13) 0.082(6) Uani 1 1 d U . . 
H37A H 0.8650 0.0076 0.0200 0.098 Uiso 1 1 calc R . . 
H37B H 0.8213 0.0810 -0.0601 0.098 Uiso 1 1 calc R . . 
C38 C 0.765(3) -0.032(3) -0.026(2) 0.253(19) Uani 1 1 d U . . 
H38A H 0.7720 -0.0860 0.0204 0.380 Uiso 1 1 calc R . . 
H38B H 0.8127 -0.0515 -0.0770 0.380 Uiso 1 1 calc R . . 
H38C H 0.6894 -0.0045 -0.0353 0.380 Uiso 1 1 calc R . . 
C39 C 0.5602(14) 0.2815(11) 0.0933(11) 0.063(5) Uani 1 1 d U . . 
H39A H 0.6154 0.2423 0.1292 0.076 Uiso 1 1 calc R . . 
H39B H 0.4978 0.3197 0.1277 0.076 Uiso 1 1 calc R . . 
C40 C 0.6098(14) 0.3464(11) 0.0224(11) 0.063(5) Uani 1 1 d U . . 
H40A H 0.5541 0.3897 -0.0118 0.076 Uiso 1 1 calc R . . 
H40B H 0.6710 0.3097 -0.0139 0.076 Uiso 1 1 calc R . . 
C41 C 0.6512(15) 0.4017(12) 0.0598(12) 0.076(6) Uani 1 1 d U . . 
H41A H 0.6689 0.4527 0.0150 0.091 Uiso 1 1 calc R . . 
H41B H 0.5914 0.4307 0.1019 0.091 Uiso 1 1 calc R . . 
C42 C 0.7506(14) 0.3450(12) 0.1005(12) 0.083(6) Uani 1 1 d U . . 
H42A H 0.7291 0.3059 0.1539 0.125 Uiso 1 1 calc R . . 
H42B H 0.7822 0.3870 0.1101 0.125 Uiso 1 1 calc R . . 
H42C H 0.8048 0.3053 0.0639 0.125 Uiso 1 1 calc R . . 
C43 C 0.4362(14) 0.2755(12) 0.0115(12) 0.074(6) Uani 1 1 d U . . 
H43A H 0.4145 0.2328 -0.0079 0.089 Uiso 1 1 calc R . . 
H43B H 0.4698 0.3129 -0.0384 0.089 Uiso 1 1 calc R . . 
C44 C 0.3327(13) 0.3417(11) 0.0538(11) 0.065(5) Uani 1 1 d U . . 
H44A H 0.3513 0.3909 0.0659 0.078 Uiso 1 1 calc R . . 
H44B H 0.3026 0.3065 0.1072 0.078 Uiso 1 1 calc R . . 
C45 C 0.2460(15) 0.3869(13) -0.0042(13) 0.084(6) Uani 1 1 d U . . 
H45A H 0.2825 0.4037 -0.0624 0.101 Uiso 1 1 calc R . . 
H45B H 0.1934 0.4449 0.0121 0.101 Uiso 1 1 calc R . . 
N9 N 0.7979(10) 0.3036(9) 0.5770(9) 0.057(4) Uani 1 1 d . . . 
C46 C 0.1831(17) 0.3203(14) 0.0003(14) 0.108(8) Uani 1 1 d U . . 
H46A H 0.2348 0.2629 -0.0160 0.162 Uiso 1 1 calc R . . 
H46B H 0.1301 0.3508 -0.0378 0.162 Uiso 1 1 calc R . . 
H46C H 0.1446 0.3053 0.0574 0.162 Uiso 1 1 calc R . . 
C47 C 0.8958(12) 0.2689(11) 0.5146(10) 0.053(5) Uani 1 1 d U . . 
H47A H 0.8922 0.3171 0.4622 0.064 Uiso 1 1 calc R . . 
H47B H 0.8916 0.2129 0.5026 0.064 Uiso 1 1 calc R . . 
C48 C 1.0111(12) 0.2429(11) 0.5398(10) 0.061(5) Uani 1 1 d U . . 
H48A H 1.0194 0.2991 0.5481 0.073 Uiso 1 1 calc R . . 
H48B H 1.0159 0.1959 0.5930 0.073 Uiso 1 1 calc R . . 
C49 C 1.1020(12) 0.2043(11) 0.4719(11) 0.060(5) Uani 1 1 d U . . 
H49A H 1.1040 0.2543 0.4211 0.072 Uiso 1 1 calc R . . 
H49B H 1.0877 0.1541 0.4577 0.072 Uiso 1 1 calc R . . 
C50 C 1.2119(14) 0.1660(12) 0.5011(12) 0.082(6) Uani 1 1 d U . . 
H50A H 1.2257 0.2157 0.5155 0.122 Uiso 1 1 calc R . . 
H50B H 1.2699 0.1426 0.4564 0.122 Uiso 1 1 calc R . . 
H50C H 1.2106 0.1151 0.5503 0.122 Uiso 1 1 calc R . . 
C51 C 0.7898(13) 0.3965(10) 0.5896(10) 0.055(5) Uani 1 1 d U . . 
H51A H 0.8534 0.3883 0.6136 0.066 Uiso 1 1 calc R . . 
H51B H 0.7231 0.4175 0.6306 0.066 Uiso 1 1 calc R . . 
C52 C 0.7859(13) 0.4719(10) 0.5096(10) 0.061(5) Uani 1 1 d U . . 
H52A H 0.8575 0.4575 0.4721 0.073 Uiso 1 1 calc R . . 
H52B H 0.7299 0.4741 0.4803 0.073 Uiso 1 1 calc R . . 
C53 C 0.7582(13) 0.5658(11) 0.5312(11) 0.064(5) Uani 1 1 d U . . 
H53A H 0.6895 0.5763 0.5723 0.077 Uiso 1 1 calc R . . 
H53B H 0.7443 0.6151 0.4802 0.077 Uiso 1 1 calc R . . 
C54 C 0.8450(13) 0.5770(11) 0.5666(11) 0.069(5) Uani 1 1 d U . . 
H54A H 0.8606 0.5280 0.6167 0.104 Uiso 1 1 calc R . . 
H54B H 0.8181 0.6382 0.5810 0.104 Uiso 1 1 calc R . . 
H54C H 0.9119 0.5720 0.5248 0.104 Uiso 1 1 calc R . . 
C55 C 0.7059(12) 0.3064(11) 0.5438(10) 0.058(5) Uani 1 1 d U . . 
H55A H 0.7105 0.2414 0.5479 0.070 Uiso 1 1 calc R . . 
H55B H 0.7146 0.3368 0.4839 0.070 Uiso 1 1 calc R . . 
C56 C 0.5902(13) 0.3572(12) 0.5866(12) 0.070(5) Uani 1 1 d U . . 
H56A H 0.5812 0.3298 0.6472 0.085 Uiso 1 1 calc R . . 
H56B H 0.5817 0.4238 0.5788 0.085 Uiso 1 1 calc R . . 
C57 C 0.5026(13) 0.3494(11) 0.5507(11) 0.065(5) Uani 1 1 d U . . 
H57A H 0.4312 0.3919 0.5720 0.078 Uiso 1 1 calc R . . 
H57B H 0.5171 0.3710 0.4894 0.078 Uiso 1 1 calc R . . 
C58 C 0.4941(14) 0.2535(12) 0.5701(12) 0.078(6) Uani 1 1 d U . . 
H58A H 0.5636 0.2108 0.5481 0.117 Uiso 1 1 calc R . . 
H58B H 0.4359 0.2552 0.5443 0.117 Uiso 1 1 calc R . . 
H58C H 0.4771 0.2320 0.6307 0.117 Uiso 1 1 calc R . . 
C59 C 0.8046(15) 0.2374(12) 0.6620(12) 0.073(6) Uani 1 1 d U . . 
H59A H 0.8666 0.2383 0.6826 0.087 Uiso 1 1 calc R . . 
H59B H 0.7373 0.2624 0.7008 0.087 Uiso 1 1 calc R . . 
C60 C 0.8183(14) 0.1370(11) 0.6670(11) 0.065(5) Uani 1 1 d U . . 
H60A H 0.8784 0.1130 0.6228 0.078 Uiso 1 1 calc R . . 
H60B H 0.7503 0.1327 0.6583 0.078 Uiso 1 1 calc R . . 
C61 C 0.8438(14) 0.0790(12) 0.7518(12) 0.075(6) Uani 1 1 d U . . 
H61A H 0.7893 0.1094 0.7955 0.090 Uiso 1 1 calc R . . 
H61B H 0.8370 0.0170 0.7592 0.090 Uiso 1 1 calc R . . 
C62 C 0.9560(14) 0.0664(12) 0.7635(12) 0.080(6) Uani 1 1 d U . . 
H62A H 1.0106 0.0358 0.7208 0.119 Uiso 1 1 calc R . . 
H62B H 0.9681 0.0277 0.8189 0.119 Uiso 1 1 calc R . . 
H62C H 0.9626 0.1273 0.7585 0.119 Uiso 1 1 calc R . . 
 
 
_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 N1 1.231(16) . ? 
O2 N1 1.232(17) . ? 
O3 N2 1.25(2) . ? 
O4 N2 1.20(2) . ? 
O5 C7 1.206(18) . ? 
O6 C12 1.199(17) . ? 
O7 N6 1.194(17) . ? 
O8 N6 1.270(17) . ? 
O9 N7 1.245(16) . ? 
O10 N7 1.206(17) . ? 
N1 C2 1.456(16) . ? 
N2 C4 1.443(19) . ? 
N3 C7 1.360(19) . ? 
N3 C6 1.364(13) . ? 
N4 C11 1.345(18) . ? 
N4 C8 1.380(19) . ? 
N5 C12 1.396(18) . ? 
N5 C13 1.401(13) . ? 
N6 C15 1.460(16) . ? 
N7 C17 1.455(16) . ? 
C1 C2 1.3900 . ? 
C1 C6 1.3900 . ? 
C2 C3 1.3900 . ? 
C3 C4 1.3900 . ? 
C4 C5 1.3900 . ? 
C5 C6 1.3900 . ? 
C7 C8 1.54(2) . ? 
C8 C9 1.40(2) . ? 
C9 C10 1.419(19) . ? 
C9 C19 1.508(16) . ? 
C10 C11 1.408(19) . ? 
C10 C25 1.465(16) . ? 
C11 C12 1.49(2) . ? 
C13 C14 1.3900 . ? 
C13 C18 1.3900 . ? 
C14 C15 1.3900 . ? 
C15 C16 1.3900 . ? 
C16 C17 1.3900 . ? 
C17 C18 1.3900 . ? 
C19 C20 1.3900 . ? 
C19 C24 1.3900 . ? 
C20 C21 1.3900 . ? 
C21 C22 1.3900 . ? 
C22 C23 1.3900 . ? 
C23 C24 1.3900 . ? 
C25 C26 1.3900 . ? 
C25 C30 1.3900 . ? 
C26 C27 1.3900 . ? 
C27 C28 1.3900 . ? 
C28 C29 1.3900 . ? 
C29 C30 1.3900 . ? 
N8 C31 1.493(19) . ? 
N8 C43 1.50(2) . ? 
N8 C39 1.519(19) . ? 
N8 C35 1.53(2) . ? 
C31 C32 1.510(19) . ? 
C32 C33 1.50(2) . ? 
C33 C34 1.55(2) . ? 
C35 C36 1.55(2) . ? 
C36 C37 1.52(2) . ? 
C37 C38 1.53(4) . ? 
C39 C40 1.52(2) . ? 
C40 C41 1.54(2) . ? 
C41 C42 1.51(2) . ? 
C43 C44 1.54(2) . ? 
C44 C45 1.55(2) . ? 
C45 C46 1.55(2) . ? 
N9 C55 1.468(18) . ? 
N9 C47 1.489(19) . ? 
N9 C51 1.509(17) . ? 
N9 C59 1.52(2) . ? 
C47 C48 1.59(2) . ? 
C48 C49 1.52(2) . ? 
C49 C50 1.53(2) . ? 
C51 C52 1.53(2) . ? 
C52 C53 1.52(2) . ? 
C53 C54 1.53(2) . ? 
C55 C56 1.55(2) . ? 
C56 C57 1.52(2) . ? 
C57 C58 1.50(2) . ? 
C59 C60 1.51(2) . ? 
C60 C61 1.52(2) . ? 
C61 C62 1.50(2) . ? 
 
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 
O1 N1 O2 125.6(16) . . ? 
O1 N1 C2 115.2(15) . . ? 
O2 N1 C2 118.8(15) . . ? 
O4 N2 O3 125(2) . . ? 
O4 N2 C4 120.1(19) . . ? 
O3 N2 C4 115(2) . . ? 
C7 N3 C6 127.2(13) . . ? 
C11 N4 C8 104.8(13) . . ? 
C12 N5 C13 126.3(13) . . ? 
O7 N6 O8 125.1(16) . . ? 
O7 N6 C15 120.1(16) . . ? 
O8 N6 C15 114.8(16) . . ? 
O10 N7 O9 125.6(16) . . ? 
O10 N7 C17 118.8(15) . . ? 
O9 N7 C17 115.6(16) . . ? 
C2 C1 C6 120.0 . . ? 
C1 C2 C3 120.0 . . ? 
C1 C2 N1 122.5(10) . . ? 
C3 C2 N1 117.5(10) . . ? 
C2 C3 C4 120.0 . . ? 
C5 C4 C3 120.0 . . ? 
C5 C4 N2 117.3(12) . . ? 
C3 C4 N2 122.7(12) . . ? 
C4 C5 C6 120.0 . . ? 
N3 C6 C5 119.0(9) . . ? 
N3 C6 C1 121.0(9) . . ? 
C5 C6 C1 120.0 . . ? 
O5 C7 N3 126.9(17) . . ? 
O5 C7 C8 118.6(17) . . ? 
N3 C7 C8 114.5(16) . . ? 
N4 C8 C9 111.0(14) . . ? 
N4 C8 C7 117.7(16) . . ? 
C9 C8 C7 130.8(16) . . ? 
C8 C9 C10 106.6(14) . . ? 
C8 C9 C19 129.4(14) . . ? 
C10 C9 C19 124.0(13) . . ? 
C11 C10 C9 103.8(13) . . ? 
C11 C10 C25 131.5(14) . . ? 
C9 C10 C25 123.9(13) . . ? 
N4 C11 C10 113.4(14) . . ? 
N4 C11 C12 120.3(15) . . ? 
C10 C11 C12 126.2(15) . . ? 
O6 C12 N5 122.7(15) . . ? 
O6 C12 C11 125.3(16) . . ? 
N5 C12 C11 112.0(15) . . ? 
C14 C13 C18 120.0 . . ? 
C14 C13 N5 117.6(9) . . ? 
C18 C13 N5 122.4(9) . . ? 
C13 C14 C15 120.0 . . ? 
C16 C15 C14 120.0 . . ? 
C16 C15 N6 121.4(11) . . ? 
C14 C15 N6 118.6(11) . . ? 
C15 C16 C17 120.0 . . ? 
C16 C17 C18 120.0 . . ? 
C16 C17 N7 119.9(11) . . ? 
C18 C17 N7 120.1(11) . . ? 
C17 C18 C13 120.0 . . ? 
C20 C19 C24 120.0 . . ? 
C20 C19 C9 120.7(9) . . ? 
C24 C19 C9 119.2(9) . . ? 
C19 C20 C21 120.0 . . ? 
C20 C21 C22 120.0 . . ? 
C21 C22 C23 120.0 . . ? 
C24 C23 C22 120.0 . . ? 
C23 C24 C19 120.0 . . ? 
C26 C25 C30 120.0 . . ? 
C26 C25 C10 119.9(10) . . ? 
C30 C25 C10 120.0(10) . . ? 
C27 C26 C25 120.0 . . ? 
C26 C27 C28 120.0 . . ? 
C27 C28 C29 120.0 . . ? 
C30 C29 C28 120.0 . . ? 
C29 C30 C25 120.0 . . ? 
C31 N8 C43 109.3(13) . . ? 
C31 N8 C39 109.1(13) . . ? 
C43 N8 C39 110.0(13) . . ? 
C31 N8 C35 111.4(13) . . ? 
C43 N8 C35 103.4(14) . . ? 
C39 N8 C35 113.5(13) . . ? 
N8 C31 C32 120.1(14) . . ? 
C33 C32 C31 112.6(15) . . ? 
C32 C33 C34 113.0(14) . . ? 
N8 C35 C36 111.9(15) . . ? 
C37 C36 C35 110.7(16) . . ? 
C36 C37 C38 116(2) . . ? 
N8 C39 C40 114.9(14) . . ? 
C39 C40 C41 108.8(15) . . ? 
C42 C41 C40 114.9(15) . . ? 
N8 C43 C44 115.0(16) . . ? 
C43 C44 C45 110.0(15) . . ? 
C44 C45 C46 111.9(15) . . ? 
C55 N9 C47 104.4(12) . . ? 
C55 N9 C51 113.9(12) . . ? 
C47 N9 C51 111.5(12) . . ? 
C55 N9 C59 110.4(13) . . ? 
C47 N9 C59 110.9(12) . . ? 
C51 N9 C59 106.0(12) . . ? 
N9 C47 C48 116.5(13) . . ? 
C49 C48 C47 110.1(14) . . ? 
C48 C49 C50 110.3(15) . . ? 
N9 C51 C52 113.6(14) . . ? 
C53 C52 C51 109.3(14) . . ? 
C52 C53 C54 115.7(14) . . ? 
N9 C55 C56 116.5(14) . . ? 
C57 C56 C55 111.2(14) . . ? 
C58 C57 C56 115.2(14) . . ? 
C60 C59 N9 117.4(15) . . ? 
C59 C60 C61 109.5(15) . . ? 
C62 C61 C60 113.2(15) . . ? 
 
loop_ 
 _geom_hbond_atom_site_label_D 
 _geom_hbond_atom_site_label_H 
 _geom_hbond_atom_site_label_A 
 _geom_hbond_distance_DH 
 _geom_hbond_distance_HA 
 _geom_hbond_distance_DA 
 _geom_hbond_angle_DHA 
 _geom_hbond_site_symmetry_A 
N3 H3 F1  0.88 2.58 3.403(12) 156.8 . 
N5 H5 F1  0.88 2.55 3.385(13) 157.7 . 
 
_diffrn_measured_fraction_theta_max    0.780 
_diffrn_reflns_theta_full              25.02 
_diffrn_measured_fraction_theta_full   0.780 
_refine_diff_density_max    0.720 
_refine_diff_density_min   -0.328 
_refine_diff_density_rms    0.099 
