# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2005

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Francois Diederich'
_publ_contact_author_address     
;
Laboratorium fur Organische Chemie
ETH-Hoenggerberg / HCI G 313
Wolfgang-Pauli-Strasse 10
Zurich
CH 8093
SWITZERLAND
;

_publ_contact_author_email       DIEDERICH@ORG.CHEM.ETHZ.CH

_publ_section_title              
;
Selective Steroid Recognition by a Partially Bridged
Resorcin[4]arene Cavitand
;
loop_
_publ_author_name
'Francois Diederich'
'Vladimir A. Azov'
'Martina Cacciarini'
'Hermann Kunzer'
'Paul Seiler'

data_martina_ca1_D_04
_database_code_depnum_ccdc_archive 'CCDC 277163'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C88 H116 N4 O8, 2(C3 H6 O)'
_chemical_formula_sum            'C94 H128 N4 O10'
_chemical_formula_weight         1474.00

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'

_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                   11.8400(2)
_cell_length_b                   13.8058(2)
_cell_length_c                   28.6689(4)
_cell_angle_alpha                78.641(1)
_cell_angle_beta                 80.066(1)
_cell_angle_gamma                72.126(1)
_cell_volume                     4341.04(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    220(2)
_cell_measurement_reflns_used    9922
_cell_measurement_theta_min      2.82
_cell_measurement_theta_max      22.99

_exptl_crystal_description       'Cut fragment'
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.128
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1600
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      220(2)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Kappa CCD'
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_reflns_number            18839
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0490
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.82
_diffrn_reflns_theta_max         22.99
_reflns_number_total             11913
_reflns_number_gt                8241
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Kappa CCD'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        'Denzo + Scalepak (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR97 (Altomare et Al., 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP (Johnson,1976)'
_computing_publication_material  SHELXL97

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness 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 threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1172P)^2^+3.1564P] 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    'H-atoms riding'
_refine_ls_extinction_method     SHELXL97
_refine_ls_extinction_coef       0.0073(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         11913
_refine_ls_number_parameters     954
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1158
_refine_ls_R_factor_gt           0.0816
_refine_ls_wR_factor_ref         0.2394
_refine_ls_wR_factor_gt          0.2120
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001

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
C1 C 0.2087(3) 0.0001(3) 0.25587(13) 0.0722(12) Uani 1 d . . .
H1A H 0.2710 -0.0663 0.2537 0.104 Uiso 1 calc R . .
C2 C 0.2278(3) 0.0383(3) 0.29901(14) 0.0720(12) Uani 1 d . . .
C3 C 0.1917(3) 0.1426(3) 0.30295(14) 0.0721(12) Uani 1 d . . .
H3A H 0.1529 0.1890 0.2781 0.052 Uiso 1 calc R . .
C4 C 0.2090(3) 0.1829(3) 0.34100(14) 0.0706(11) Uani 1 d . . .
C5 C 0.2672(3) 0.1104(4) 0.37651(14) 0.0773(13) Uani 1 d . . .
C6 C 0.3037(3) 0.0058(4) 0.37460(16) 0.0812(13) Uani 1 d . . .
H6A H 0.3428 -0.0407 0.3994 0.104 Uiso 1 calc R . .
C7 C 0.2829(4) -0.0299(4) 0.33671(15) 0.0800(13) Uani 1 d . . .
O8 O 0.3213(3) -0.1348(2) 0.33809(10) 0.0999(11) Uani 1 d . . .
H8A H 0.2781 -0.1525 0.3235 0.139 Uiso 1 calc R . .
C9 C 0.1684(4) 0.2967(3) 0.34389(15) 0.0819(13) Uani 1 d . . .
H9A H 0.2170 0.3072 0.3663 0.136 Uiso 1 calc R . .
C10 C 0.0379(4) 0.3302(3) 0.36653(14) 0.0688(11) Uani 1 d . . .
C11 C -0.0602(4) 0.3617(3) 0.34006(13) 0.0628(10) Uani 1 d . . .
H11A H -0.0450 0.3617 0.3068 0.076 Uiso 1 calc R . .
C12 C -0.1784(4) 0.3929(2) 0.36037(12) 0.0573(9) Uani 1 d . . .
C13 C -0.1982(4) 0.3940(3) 0.40955(13) 0.0673(11) Uani 1 d . . .
C14 C -0.1045(5) 0.3632(3) 0.43678(14) 0.0787(13) Uani 1 d . . .
H14A H -0.1193 0.3650 0.4699 0.062 Uiso 1 calc R . .
C15 C 0.0110(5) 0.3299(3) 0.41524(16) 0.0751(12) Uani 1 d . . .
O16 O -0.3158(3) 0.4283(2) 0.42934(9) 0.0833(9) Uani 1 d . . .
H16A H -0.3180 0.4300 0.4583 0.093 Uiso 1 calc R . .
O17 O 0.1033(3) 0.3021(2) 0.44463(10) 0.0898(10) Uani 1 d . . .
C18 C 0.1228(4) 0.2064(3) 0.47275(15) 0.0729(12) Uani 1 d . . .
C19 C 0.2221(4) 0.1265(3) 0.45858(14) 0.0715(11) Uani 1 d . . .
O20 O 0.2903(2) 0.1472(2) 0.41550(10) 0.0885(9) Uani 1 d . . .
N21 N 0.2527(3) 0.0368(3) 0.48394(11) 0.0766(10) Uani 1 d . . .
C22 C 0.1800(4) 0.0220(3) 0.52646(12) 0.0647(10) Uani 1 d . . .
C23 C 0.0809(4) 0.0995(3) 0.54006(14) 0.0792(12) Uani 1 d . . .
N24 N 0.0527(4) 0.1955(3) 0.51214(13) 0.0915(12) Uani 1 d . . .
C25 C 0.0101(5) 0.0805(4) 0.58320(16) 0.123(2) Uani 1 d . . .
H25A H -0.0564 0.1331 0.5933 0.122 Uiso 1 calc R . .
C26 C 0.0374(5) -0.0145(4) 0.61080(16) 0.1090(19) Uani 1 d . . .
H26A H -0.0123 -0.0278 0.6392 0.162 Uiso 1 calc R . .
C27 C 0.1372(4) -0.0909(3) 0.59729(14) 0.0817(13) Uani 1 d . . .
H27A H 0.1558 -0.1556 0.6168 0.056 Uiso 1 calc R . .
C28 C 0.2088(4) -0.0736(3) 0.55610(14) 0.0787(12) Uani 1 d . . .
H28A H 0.2777 -0.1257 0.5475 0.077 Uiso 1 calc R . .
C29 C -0.2821(3) 0.4226(2) 0.33072(11) 0.0540(9) Uani 1 d . . .
H29A H -0.3508 0.4666 0.3490 0.035 Uiso 1 calc R . .
C30 C -0.3184(3) 0.3268(2) 0.32758(10) 0.0481(8) Uani 1 d . . .
C31 C -0.2663(3) 0.2688(2) 0.29084(11) 0.0467(8) Uani 1 d . . .
H31A H -0.2086 0.2905 0.2678 0.034 Uiso 1 calc R . .
C32 C -0.2942(3) 0.1810(2) 0.28603(10) 0.0443(8) Uani 1 d . . .
C33 C -0.3782(3) 0.1513(2) 0.32136(11) 0.0477(8) Uani 1 d . . .
C34 C -0.4342(3) 0.2053(3) 0.35791(12) 0.0544(9) Uani 1 d . . .
H34A H -0.4924 0.1834 0.3805 0.098 Uiso 1 calc R . .
C35 C -0.4043(3) 0.2932(2) 0.36141(11) 0.0553(9) Uani 1 d . . .
O36 O -0.4646(3) 0.34441(19) 0.39876(9) 0.0796(8) Uani 1 d . . .
H36A H -0.4311 0.3872 0.4017 0.181 Uiso 1 calc R . .
C37 C -0.2375(3) 0.1195(2) 0.24505(11) 0.0495(8) Uani 1 d . . .
H37A H -0.2966 0.0860 0.2402 0.060 Uiso 1 calc R . .
C38 C -0.1268(3) 0.0330(2) 0.25869(10) 0.0489(8) Uani 1 d . . .
C39 C -0.0155(3) 0.0512(3) 0.25322(11) 0.0539(9) Uani 1 d . . .
H39A H -0.0112 0.1188 0.2419 0.031 Uiso 1 calc R . .
C40 C 0.0894(3) -0.0244(3) 0.26348(12) 0.0609(10) Uani 1 d . . .
C41 C 0.0798(4) -0.1236(3) 0.28136(14) 0.0720(11) Uani 1 d . . .
C42 C -0.0277(4) -0.1446(3) 0.28834(13) 0.0706(11) Uani 1 d . . .
H42A H -0.0327 -0.2115 0.3010 0.086 Uiso 1 calc R . .
C43 C -0.1296(3) -0.0669(3) 0.27676(12) 0.0576(9) Uani 1 d . . .
O44 O -0.2373(2) -0.09309(17) 0.28214(8) 0.0632(7) Uani 1 d . . .
O45 O 0.1840(3) -0.1996(2) 0.29075(12) 0.1036(11) Uani 1 d . . .
H45A H 0.1679 -0.2476 0.3105 0.054 Uiso 1 calc R . .
C46 C -0.2878(3) -0.1096(3) 0.32906(12) 0.0578(9) Uani 1 d . . .
C47 C -0.3727(3) -0.0253(2) 0.34821(12) 0.0523(9) Uani 1 d . . .
O48 O -0.4103(2) 0.06360(16) 0.31653(8) 0.0558(6) Uani 1 d . . .
N49 N -0.4184(3) -0.0309(2) 0.39261(11) 0.0621(8) Uani 1 d . . .
C50 C -0.3846(4) -0.1267(3) 0.42023(13) 0.0644(10) Uani 1 d . . .
C51 C -0.3077(4) -0.2116(3) 0.40032(14) 0.0708(11) Uani 1 d . . .
N52 N -0.2562(3) -0.2008(2) 0.35335(12) 0.0750(9) Uani 1 d . . .
C53 C -0.4319(4) -0.1397(4) 0.46865(15) 0.0859(13) Uani 1 d . . .
H53A H -0.4828 -0.0830 0.4825 0.099 Uiso 1 calc R . .
C54 C -0.4034(5) -0.2357(4) 0.49572(16) 0.0970(16) Uani 1 d . . .
H54A H -0.4338 -0.2443 0.5283 0.081 Uiso 1 calc R . .
C55 C -0.3308(5) -0.3194(4) 0.47556(19) 0.1043(17) Uani 1 d . . .
H55A H -0.3148 -0.3849 0.4944 0.124 Uiso 1 calc R . .
C56 C -0.2816(5) -0.3098(3) 0.42895(18) 0.0994(15) Uani 1 d . . .
H56A H -0.2309 -0.3677 0.4160 0.206 Uiso 1 calc R . .
C57 C 0.2267(3) 0.0698(3) 0.20784(13) 0.0711(11) Uani 1 d . . .
H57A H 0.1606 0.1334 0.2066 0.076 Uiso 1 calc R . .
H57B H 0.3010 0.0884 0.2059 0.095 Uiso 1 calc R . .
C58 C 0.2322(4) 0.0186(3) 0.16555(13) 0.0745(12) Uani 1 d . . .
H58A H 0.1574 0.0007 0.1675 0.090 Uiso 1 calc R . .
H58B H 0.2973 -0.0457 0.1674 0.092 Uiso 1 calc R . .
C59 C 0.2514(4) 0.0840(3) 0.11747(13) 0.0728(11) Uani 1 d . . .
H59A H 0.1815 0.1442 0.1141 0.098 Uiso 1 calc R . .
H59B H 0.3208 0.1089 0.1170 0.102 Uiso 1 calc R . .
C60 C 0.2714(4) 0.0286(3) 0.07491(13) 0.0714(11) Uani 1 d . . .
H60A H 0.3401 -0.0326 0.0787 0.109 Uiso 1 calc R . .
H60B H 0.2012 0.0052 0.0750 0.066 Uiso 1 calc R . .
C61 C 0.2935(4) 0.0921(3) 0.02723(13) 0.0685(10) Uani 1 d . . .
H61A H 0.3604 0.1192 0.0280 0.071 Uiso 1 calc R . .
H61B H 0.2226 0.1510 0.0225 0.089 Uiso 1 calc R . .
C62 C 0.3211(4) 0.0354(3) -0.01525(13) 0.0688(10) Uani 1 d . . .
H62A H 0.3904 -0.0248 -0.0102 0.136 Uiso 1 calc R . .
H62B H 0.2530 0.0104 -0.0168 0.090 Uiso 1 calc R . .
C63 C 0.3469(4) 0.0999(3) -0.06258(13) 0.0698(11) Uani 1 d . . .
H63A H 0.4151 0.1246 -0.0608 0.171 Uiso 1 calc R . .
H63B H 0.2777 0.1603 -0.0672 0.087 Uiso 1 calc R . .
C64 C 0.3743(4) 0.0458(3) -0.10595(14) 0.0714(11) Uani 1 d . . .
H64A H 0.4429 -0.0152 -0.1014 0.093 Uiso 1 calc R . .
H64B H 0.3056 0.0224 -0.1084 0.114 Uiso 1 calc R . .
C65 C 0.4017(4) 0.1126(3) -0.15234(13) 0.0734(11) Uani 1 d . . .
H65A H 0.4718 0.1343 -0.1500 0.085 Uiso 1 calc R . .
H65B H 0.3341 0.1748 -0.1561 0.086 Uiso 1 calc R . .
C66 C 0.4256(4) 0.0624(4) -0.19676(15) 0.0863(13) Uani 1 d . . .
H66A H 0.4926 -0.0003 -0.1930 0.105 Uiso 1 calc R . .
H66B H 0.3551 0.0419 -0.1996 0.116 Uiso 1 calc R . .
C67 C 0.4545(4) 0.1308(4) -0.24247(15) 0.0991(15) Uani 1 d . . .
H67A H 0.4683 0.0941 -0.2694 0.208 Uiso 1 calc R . .
H67B H 0.5257 0.1498 -0.2405 0.098 Uiso 1 calc R . .
H67C H 0.3881 0.1925 -0.2469 0.148 Uiso 1 calc R . .
C68 C -0.2135(3) 0.1885(2) 0.19727(11) 0.0517(8) Uani 1 d . . .
H68A H -0.2866 0.2442 0.1914 0.049 Uiso 1 calc R . .
H68B H -0.1517 0.2199 0.2002 0.057 Uiso 1 calc R . .
C69 C -0.1735(4) 0.1314(3) 0.15455(11) 0.0597(9) Uani 1 d . . .
H69A H -0.2363 0.1018 0.1509 0.071 Uiso 1 calc R . .
H69B H -0.1017 0.0743 0.1608 0.063 Uiso 1 calc R . .
C70 C -0.1464(4) 0.1992(3) 0.10806(11) 0.0616(10) Uani 1 d . . .
H70A H -0.2176 0.2572 0.1024 0.058 Uiso 1 calc R . .
H70B H -0.0824 0.2274 0.1116 0.086 Uiso 1 calc R . .
C71 C -0.1091(4) 0.1445(3) 0.06450(12) 0.0639(10) Uani 1 d . . .
H71A H -0.0372 0.0871 0.0700 0.101 Uiso 1 calc R . .
H71B H -0.1727 0.1153 0.0613 0.105 Uiso 1 calc R . .
C72 C -0.0838(4) 0.2120(3) 0.01778(12) 0.0639(10) Uani 1 d . . .
H72A H -0.0188 0.2398 0.0206 0.110 Uiso 1 calc R . .
H72B H -0.1550 0.2704 0.0126 0.090 Uiso 1 calc R . .
C73 C -0.0496(4) 0.1568(3) -0.02552(12) 0.0662(10) Uani 1 d . . .
H73A H 0.0218 0.0987 -0.0203 0.114 Uiso 1 calc R . .
H73B H -0.1145 0.1287 -0.0281 0.120 Uiso 1 calc R . .
C74 C -0.0247(4) 0.2237(3) -0.07239(13) 0.0744(11) Uani 1 d . . .
H74A H 0.0398 0.2524 -0.0698 0.153 Uiso 1 calc R . .
H74B H -0.0963 0.2814 -0.0779 0.072 Uiso 1 calc R . .
C75 C 0.0107(5) 0.1664(4) -0.11516(14) 0.0934(15) Uani 1 d . . .
H75A H -0.0582 0.1463 -0.1202 0.148 Uiso 1 calc R . .
H75B H 0.0745 0.1030 -0.1073 0.183 Uiso 1 calc R . .
C76 C 0.0535(6) 0.2260(5) -0.16177(18) 0.127(2) Uani 1 d . . .
H76A H 0.1163 0.2524 -0.1554 0.218 Uiso 1 calc R . .
H76B H 0.0905 0.1772 -0.1844 0.204 Uiso 1 calc R . .
C77 C -0.0296(7) 0.3073(5) -0.1841(2) 0.139(2) Uani 1 d . . .
H77A H -0.0711 0.3537 -0.1608 0.181 Uiso 1 calc R . .
H77B H -0.0892 0.2802 -0.1929 0.230 Uiso 1 calc R . .
C78 C 0.0166(7) 0.3707(5) -0.2288(2) 0.157(3) Uani 1 d . . .
H78A H -0.0494 0.4266 -0.2407 0.214 Uiso 1 calc R . .
H78B H 0.0533 0.3272 -0.2532 0.150 Uiso 1 calc R . .
H78C H 0.0754 0.3988 -0.2209 0.214 Uiso 1 calc R . .
C79 C -0.2613(3) 0.4878(3) 0.28199(12) 0.0600(9) Uani 1 d . . .
H79A H -0.2316 0.5438 0.2865 0.073 Uiso 1 calc R . .
H79B H -0.1995 0.4448 0.2613 0.053 Uiso 1 calc R . .
C80 C -0.3738(3) 0.5335(3) 0.25705(12) 0.0672(10) Uani 1 d . . .
H80A H -0.4335 0.5803 0.2767 0.077 Uiso 1 calc R . .
H80B H -0.4067 0.4778 0.2548 0.082 Uiso 1 calc R . .
C81 C -0.3532(4) 0.5924(3) 0.20687(13) 0.0695(11) Uani 1 d . . .
H81A H -0.4301 0.6387 0.1980 0.110 Uiso 1 calc R . .
H81B H -0.3013 0.6351 0.2078 0.090 Uiso 1 calc R . .
C82 C -0.2975(4) 0.5255(3) 0.16828(13) 0.0683(10) Uani 1 d . . .
H82A H -0.3515 0.4859 0.1658 0.085 Uiso 1 calc R . .
H82B H -0.2226 0.4765 0.1778 0.066 Uiso 1 calc R . .
C83 C -0.2718(4) 0.5866(3) 0.11943(12) 0.0674(10) Uani 1 d . . .
H83A H -0.3441 0.6425 0.1125 0.083 Uiso 1 calc R . .
H83B H -0.2093 0.6183 0.1212 0.102 Uiso 1 calc R . .
C84 C -0.2325(4) 0.5264(3) 0.07794(13) 0.0681(10) Uani 1 d . . .
H84A H -0.1608 0.4698 0.0848 0.090 Uiso 1 calc R . .
H84B H -0.2955 0.4960 0.0754 0.067 Uiso 1 calc R . .
C85 C -0.2057(4) 0.5896(3) 0.03037(12) 0.0653(10) Uani 1 d . . .
H85A H -0.1413 0.6183 0.0329 0.088 Uiso 1 calc R . .
H85B H -0.2768 0.6476 0.0244 0.096 Uiso 1 calc R . .
C86 C -0.1699(4) 0.5338(3) -0.01252(13) 0.0669(10) Uani 1 d . . .
H86A H -0.2352 0.5072 -0.0159 0.071 Uiso 1 calc R . .
H86B H -0.1000 0.4747 -0.0064 0.078 Uiso 1 calc R . .
C87 C -0.1401(4) 0.5992(3) -0.05934(13) 0.0667(10) Uani 1 d . . .
H87A H -0.2100 0.6584 -0.0653 0.096 Uiso 1 calc R . .
H87B H -0.0748 0.6258 -0.0558 0.093 Uiso 1 calc R . .
C88 C -0.1044(4) 0.5449(3) -0.10254(14) 0.0763(11) Uani 1 d . . .
H88A H -0.1704 0.5199 -0.1069 0.152 Uiso 1 calc R . .
H88B H -0.0354 0.4848 -0.0966 0.078 Uiso 1 calc R . .
C89 C -0.0726(5) 0.6127(4) -0.14834(14) 0.0925(14) Uani 1 d . . .
H89A H -0.0506 0.5735 -0.1747 0.069 Uiso 1 calc R . .
H89B H -0.0060 0.6363 -0.1446 0.186 Uiso 1 calc R . .
H89C H -0.1411 0.6716 -0.1549 0.145 Uiso 1 calc R . .
C90 C 0.1950(4) 0.3626(4) 0.29576(16) 0.1003(16) Uani 1 d . . .
H90A H 0.1567 0.4356 0.2980 0.078 Uiso 1 calc R . .
H90B H 0.1619 0.3447 0.2706 0.139 Uiso 1 calc R . .
C91 C 0.3317(5) 0.3443(6) 0.2823(2) 0.163(3) Uani 1 d . . .
H91A H 0.3700 0.2699 0.2852 0.180 Uiso 1 calc R . .
H91B H 0.3618 0.3705 0.3057 0.181 Uiso 1 calc R . .
C92 C 0.3704(9) 0.3956(9) 0.2311(4) 0.215(5) Uani 1 d . . .
H92A H 0.4379 0.4219 0.2320 0.250 Uiso 1 calc R . .
H92B H 0.3040 0.4540 0.2202 0.260 Uiso 1 calc R . .
C93 C 0.4073(8) 0.3167(7) 0.1951(4) 0.209(5) Uani 1 d . . .
H93A H 0.4728 0.2584 0.2066 0.130 Uiso 1 calc R . .
H93B H 0.3394 0.2903 0.1949 0.150 Uiso 1 calc R . .
C94 C 0.4470(7) 0.3597(7) 0.1434(4) 0.178(4) Uani 1 d . . .
H94A H 0.3823 0.4200 0.1330 0.154 Uiso 1 calc R . .
H94B H 0.5159 0.3844 0.1441 0.217 Uiso 1 calc R . .
C95 C 0.4794(7) 0.2935(6) 0.1069(4) 0.172(4) Uani 1 d . . .
H95A H 0.4124 0.2662 0.1065 0.200 Uiso 1 calc R . .
H95B H 0.5477 0.2350 0.1157 0.200 Uiso 1 calc R . .
C96 C 0.5121(7) 0.3463(6) 0.0558(4) 0.171(4) Uani 1 d . . .
H96A H 0.4438 0.4045 0.0467 0.205 Uiso 1 calc R . .
H96B H 0.5790 0.3739 0.0560 0.205 Uiso 1 calc R . .
C97 C 0.5441(8) 0.2804(6) 0.0208(5) 0.201(5) Uani 1 d . . .
H97A H 0.4781 0.2514 0.0209 0.231 Uiso 1 calc R . .
H97B H 0.6139 0.2231 0.0293 0.209 Uiso 1 calc R . .
C98 C 0.5736(6) 0.3353(5) -0.0305(4) 0.155(3) Uani 1 d . . .
H98A H 0.5040 0.3933 -0.0385 0.123 Uiso 1 calc R . .
H98B H 0.6399 0.3637 -0.0304 0.190 Uiso 1 calc R . .
C99 C 0.6054(8) 0.2710(6) -0.0677(5) 0.201(5) Uani 1 d . . .
H99A H 0.5396 0.2419 -0.0676 0.241 Uiso 1 calc R . .
H99B H 0.6759 0.2137 -0.0601 0.241 Uiso 1 calc R . .
C100 C 0.6316(7) 0.3258(7) -0.1168(4) 0.194(4) Uani 1 d . . .
H1AA H 0.6540 0.2776 -0.1395 0.200 Uiso 1 calc R . .
H1AB H 0.6968 0.3549 -0.1173 0.160 Uiso 1 calc R . .
H1AC H 0.5611 0.3806 -0.1254 0.150 Uiso 1 calc R . .
O101 O -0.3654(4) 0.4258(2) 0.52379(10) 0.1200(14) Uani 1 d . . .
C102 C -0.3721(5) 0.3492(4) 0.55243(15) 0.0855(13) Uani 1 d . . .
C103 C -0.3091(6) 0.2456(4) 0.54116(18) 0.1154(19) Uani 1 d . . .
H10A H -0.2662 0.2507 0.5091 0.173 Uiso 1 calc R . .
H10B H -0.3665 0.2074 0.5427 0.173 Uiso 1 calc R . .
H10C H -0.2529 0.2100 0.5641 0.173 Uiso 1 calc R . .
C104 C -0.4423(5) 0.3581(4) 0.59995(17) 0.120(2) Uani 1 d . . .
H10D H -0.4792 0.4303 0.6027 0.179 Uiso 1 calc R . .
H10E H -0.3901 0.3265 0.6247 0.179 Uiso 1 calc R . .
H10F H -0.5040 0.3235 0.6037 0.179 Uiso 1 calc R . .
O201 O -0.1806(7) 0.3789(6) 0.6536(3) 0.225(3) Uiso 1 d . . .
C202 C -0.1371(6) 0.4108(5) 0.6102(3) 0.1271(19) Uiso 1 d . . .
C203 C -0.2360(11) 0.5059(9) 0.5984(4) 0.253(5) Uiso 1 d . . .
H20B H -0.3109 0.4908 0.6097 0.379 Uiso 1 calc R . .
H20C H -0.2308 0.5597 0.6140 0.379 Uiso 1 calc R . .
H20D H -0.2309 0.5279 0.5644 0.379 Uiso 1 calc R . .
C204 C -0.0160(13) 0.3850(10) 0.6028(5) 0.280(6) Uiso 1 d . . .
H20E H 0.0175 0.3141 0.6156 0.419 Uiso 1 calc R . .
H20F H 0.0101 0.3962 0.5691 0.419 Uiso 1 calc R . .
H20G H 0.0102 0.4281 0.6186 0.419 Uiso 1 calc 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
C1 0.056(2) 0.078(3) 0.058(2) 0.023(2) 0.0029(18) -0.0101(19)
C2 0.053(2) 0.087(3) 0.058(2) 0.030(2) -0.0035(18) -0.019(2)
C3 0.054(2) 0.091(3) 0.065(3) 0.039(2) -0.0203(18) -0.034(2)
C4 0.062(2) 0.090(3) 0.062(2) 0.033(2) -0.0202(19) -0.044(2)
C5 0.060(2) 0.116(4) 0.056(2) 0.035(2) -0.0194(19) -0.048(2)
C6 0.061(3) 0.095(3) 0.065(3) 0.040(3) -0.012(2) -0.020(2)
C7 0.063(3) 0.098(3) 0.055(3) 0.029(2) -0.002(2) -0.016(2)
O8 0.100(2) 0.088(2) 0.0691(18) 0.0281(16) -0.0065(15) 0.0082(17)
C9 0.098(3) 0.088(3) 0.075(3) 0.040(2) -0.044(2) -0.064(3)
C10 0.103(3) 0.056(2) 0.062(3) 0.0248(18) -0.041(2) -0.049(2)
C11 0.097(3) 0.057(2) 0.049(2) 0.0147(17) -0.026(2) -0.046(2)
C12 0.093(3) 0.0413(18) 0.045(2) 0.0087(15) -0.0202(19) -0.0326(18)
C13 0.113(4) 0.044(2) 0.046(2) 0.0042(17) -0.020(2) -0.025(2)
C14 0.150(5) 0.050(2) 0.048(2) 0.0089(18) -0.046(3) -0.037(3)
C15 0.122(4) 0.053(2) 0.067(3) 0.017(2) -0.049(3) -0.045(2)
O16 0.132(3) 0.0677(17) 0.0454(15) -0.0045(13) -0.0178(16) -0.0205(17)
O17 0.145(3) 0.0684(17) 0.0802(19) 0.0213(15) -0.0697(19) -0.0547(17)
C18 0.113(4) 0.064(3) 0.055(3) 0.021(2) -0.044(2) -0.045(3)
C19 0.073(3) 0.087(3) 0.062(2) 0.027(2) -0.030(2) -0.045(2)
O20 0.0764(19) 0.122(2) 0.0727(19) 0.0396(17) -0.0297(15) -0.0579(17)
N21 0.072(2) 0.088(2) 0.062(2) 0.0269(18) -0.0197(17) -0.0300(18)
C22 0.072(3) 0.076(3) 0.047(2) 0.0122(19) -0.0188(18) -0.029(2)
C23 0.100(3) 0.077(3) 0.050(2) 0.008(2) -0.025(2) -0.012(3)
N24 0.132(3) 0.074(2) 0.056(2) 0.0108(19) -0.035(2) -0.011(2)
C25 0.123(4) 0.121(4) 0.061(3) 0.021(3) 0.004(3) 0.027(3)
C26 0.100(4) 0.122(4) 0.060(3) 0.038(3) -0.004(2) -0.001(3)
C27 0.090(3) 0.079(3) 0.061(3) 0.023(2) -0.014(2) -0.020(3)
C28 0.090(3) 0.073(3) 0.056(2) 0.016(2) -0.010(2) -0.014(2)
C29 0.078(2) 0.0415(18) 0.0418(18) 0.0052(15) -0.0114(16) -0.0201(16)
C30 0.062(2) 0.0430(17) 0.0365(17) 0.0051(15) -0.0098(15) -0.0153(15)
C31 0.054(2) 0.0468(18) 0.0370(17) 0.0093(15) -0.0084(14) -0.0194(15)
C32 0.0484(19) 0.0429(17) 0.0390(17) 0.0056(14) -0.0098(14) -0.0142(15)
C33 0.052(2) 0.0422(18) 0.0495(19) 0.0055(15) -0.0115(16) -0.0189(15)
C34 0.051(2) 0.052(2) 0.054(2) 0.0006(17) 0.0023(16) -0.0165(16)
C35 0.064(2) 0.049(2) 0.045(2) -0.0008(16) 0.0014(16) -0.0134(17)
O36 0.104(2) 0.0645(16) 0.0640(16) -0.0146(13) 0.0252(15) -0.0314(15)
C37 0.061(2) 0.0481(18) 0.0402(18) 0.0043(15) -0.0070(15) -0.0236(16)
C38 0.062(2) 0.0441(18) 0.0336(17) 0.0038(14) -0.0024(14) -0.0134(16)
C39 0.068(2) 0.0461(19) 0.0382(18) 0.0088(15) -0.0004(16) -0.0159(18)
C40 0.063(2) 0.057(2) 0.0437(19) 0.0152(16) 0.0028(16) -0.0099(18)
C41 0.069(3) 0.056(2) 0.067(2) 0.0129(19) 0.0029(19) -0.003(2)
C42 0.082(3) 0.043(2) 0.069(3) 0.0118(18) 0.004(2) -0.012(2)
C43 0.073(3) 0.050(2) 0.047(2) -0.0007(16) 0.0006(17) -0.0228(19)
O44 0.0811(18) 0.0533(14) 0.0558(15) 0.0021(11) -0.0048(12) -0.0280(13)
O45 0.081(2) 0.0647(17) 0.124(3) 0.0363(17) 0.0014(17) 0.0001(15)
C46 0.072(2) 0.054(2) 0.052(2) 0.0042(18) -0.0083(18) -0.0313(19)
C47 0.061(2) 0.049(2) 0.053(2) 0.0065(17) -0.0100(17) -0.0315(17)
O48 0.0625(15) 0.0531(14) 0.0563(14) 0.0051(11) -0.0119(11) -0.0284(11)
N49 0.072(2) 0.0614(19) 0.0578(19) 0.0043(15) -0.0016(15) -0.0372(15)
C50 0.079(3) 0.069(2) 0.056(2) 0.011(2) -0.0114(19) -0.048(2)
C51 0.082(3) 0.064(2) 0.066(3) 0.013(2) -0.007(2) -0.036(2)
N52 0.093(2) 0.0555(19) 0.070(2) 0.0123(17) -0.0022(18) -0.0295(17)
C53 0.119(4) 0.087(3) 0.062(3) 0.005(2) -0.001(2) -0.060(3)
C54 0.143(5) 0.106(4) 0.058(3) 0.018(3) -0.010(3) -0.080(4)
C55 0.140(5) 0.086(3) 0.087(4) 0.031(3) -0.020(3) -0.057(3)
C56 0.122(4) 0.073(3) 0.090(3) 0.029(3) -0.005(3) -0.038(3)
C57 0.061(2) 0.076(3) 0.057(2) 0.017(2) 0.0041(18) -0.0147(19)
C58 0.075(3) 0.073(3) 0.059(2) 0.011(2) 0.0072(19) -0.019(2)
C59 0.079(3) 0.071(2) 0.057(2) 0.009(2) 0.0046(19) -0.024(2)
C60 0.080(3) 0.070(2) 0.065(2) 0.002(2) 0.001(2) -0.034(2)
C61 0.080(3) 0.066(2) 0.058(2) -0.0011(19) -0.0005(19) -0.029(2)
C62 0.079(3) 0.064(2) 0.064(2) -0.0031(19) -0.0032(19) -0.028(2)
C63 0.082(3) 0.065(2) 0.060(2) -0.0054(19) 0.0008(19) -0.024(2)
C64 0.079(3) 0.072(2) 0.069(3) -0.015(2) -0.006(2) -0.027(2)
C65 0.074(3) 0.088(3) 0.062(2) -0.022(2) 0.0006(19) -0.028(2)
C66 0.079(3) 0.108(3) 0.077(3) -0.034(3) -0.005(2) -0.023(3)
C67 0.086(3) 0.161(5) 0.062(3) -0.030(3) 0.008(2) -0.053(3)
C68 0.068(2) 0.0478(18) 0.0389(18) 0.0032(15) -0.0125(15) -0.0189(16)
C69 0.086(3) 0.0504(19) 0.0426(19) 0.0021(16) -0.0093(17) -0.0234(18)
C70 0.087(3) 0.056(2) 0.0421(19) -0.0019(16) -0.0081(17) -0.0230(19)
C71 0.094(3) 0.054(2) 0.045(2) 0.0028(17) -0.0118(18) -0.0268(19)
C72 0.088(3) 0.058(2) 0.044(2) 0.0010(17) -0.0065(18) -0.0242(19)
C73 0.091(3) 0.059(2) 0.045(2) 0.0005(17) -0.0078(18) -0.023(2)
C74 0.095(3) 0.072(2) 0.050(2) -0.0002(19) -0.001(2) -0.024(2)
C75 0.138(4) 0.093(3) 0.046(2) -0.006(2) 0.002(2) -0.037(3)
C76 0.162(6) 0.143(5) 0.070(3) -0.014(3) 0.002(3) -0.047(4)
C77 0.192(7) 0.105(4) 0.097(4) 0.026(3) -0.020(4) -0.030(4)
C78 0.252(9) 0.110(4) 0.102(4) 0.025(4) -0.002(5) -0.075(5)
C79 0.086(3) 0.0483(19) 0.047(2) 0.0112(16) -0.0149(18) -0.0273(18)
C80 0.081(3) 0.063(2) 0.049(2) 0.0127(18) -0.0134(18) -0.017(2)
C81 0.086(3) 0.058(2) 0.056(2) 0.0146(19) -0.0189(19) -0.018(2)
C82 0.082(3) 0.062(2) 0.058(2) 0.0160(19) -0.0210(19) -0.026(2)
C83 0.084(3) 0.060(2) 0.056(2) 0.0100(19) -0.0181(19) -0.025(2)
C84 0.080(3) 0.063(2) 0.064(2) 0.0075(19) -0.0220(19) -0.026(2)
C85 0.079(3) 0.059(2) 0.056(2) 0.0062(18) -0.0143(18) -0.0218(19)
C86 0.082(3) 0.059(2) 0.063(2) -0.0001(19) -0.0222(19) -0.024(2)
C87 0.082(3) 0.057(2) 0.058(2) -0.0012(18) -0.0161(19) -0.0166(19)
C88 0.093(3) 0.071(2) 0.064(3) -0.011(2) -0.019(2) -0.016(2)
C89 0.119(4) 0.096(3) 0.056(3) -0.014(2) -0.009(2) -0.020(3)
C90 0.111(4) 0.107(3) 0.097(3) 0.057(3) -0.048(3) -0.076(3)
C91 0.121(5) 0.211(7) 0.161(6) 0.104(5) -0.051(4) -0.116(5)
C92 0.192(8) 0.244(11) 0.228(10) 0.095(9) -0.032(7) -0.169(9)
C93 0.188(8) 0.169(7) 0.282(12) 0.146(8) -0.136(8) -0.121(7)
C94 0.119(6) 0.126(6) 0.279(11) 0.078(7) -0.074(6) -0.063(5)
C95 0.138(6) 0.098(5) 0.291(12) 0.006(7) -0.099(7) -0.032(5)
C96 0.121(5) 0.082(4) 0.307(12) 0.040(7) -0.078(6) -0.039(4)
C97 0.142(7) 0.068(4) 0.403(17) 0.013(8) -0.122(9) -0.027(4)
C98 0.088(4) 0.077(4) 0.301(11) 0.006(6) -0.070(5) -0.022(3)
C99 0.149(7) 0.083(5) 0.378(17) 0.002(8) -0.098(9) -0.033(5)
C100 0.124(6) 0.132(6) 0.321(13) 0.014(8) -0.061(7) -0.042(5)
O101 0.233(4) 0.071(2) 0.0518(17) 0.0014(16) -0.015(2) -0.045(2)
C102 0.129(4) 0.078(3) 0.057(3) 0.003(2) -0.029(2) -0.039(3)
C103 0.184(6) 0.079(3) 0.090(4) 0.001(3) -0.018(3) -0.056(4)
C104 0.122(4) 0.117(4) 0.081(3) 0.023(3) -0.001(3) -0.008(3)

_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
C1 C2 1.512(6) . ?
C1 C40 1.522(5) . ?
C1 C57 1.539(5) . ?
C2 C3 1.392(6) . ?
C2 C7 1.395(5) . ?
C3 C4 1.388(6) . ?
C4 C5 1.390(5) . ?
C4 C9 1.511(6) . ?
C5 C6 1.384(6) . ?
C5 O20 1.414(5) . ?
C6 C7 1.364(6) . ?
C7 O8 1.372(5) . ?
C9 C10 1.535(6) . ?
C9 C90 1.537(5) . ?
C10 C15 1.377(6) . ?
C10 C11 1.407(5) . ?
C11 C12 1.389(5) . ?
C12 C13 1.391(5) . ?
C12 C29 1.521(5) . ?
C13 C14 1.378(6) . ?
C13 O16 1.383(5) . ?
C14 C15 1.377(6) . ?
C15 O17 1.409(5) . ?
O17 C18 1.380(4) . ?
C18 N24 1.293(5) . ?
C18 C19 1.407(6) . ?
C19 N21 1.287(5) . ?
C19 O20 1.385(5) . ?
N21 C22 1.384(5) . ?
C22 C23 1.382(6) . ?
C22 C28 1.401(5) . ?
C23 N24 1.383(5) . ?
C23 C25 1.397(6) . ?
C25 C26 1.368(7) . ?
C26 C27 1.377(6) . ?
C27 C28 1.356(5) . ?
C29 C79 1.531(4) . ?
C29 C30 1.534(5) . ?
C30 C31 1.391(4) . ?
C30 C35 1.401(4) . ?
C31 C32 1.388(4) . ?
C32 C33 1.386(4) . ?
C32 C37 1.524(4) . ?
C33 C34 1.363(5) . ?
C33 O48 1.413(4) . ?
C34 C35 1.389(5) . ?
C35 O36 1.372(4) . ?
C37 C38 1.526(4) . ?
C37 C68 1.544(4) . ?
C38 C43 1.383(4) . ?
C38 C39 1.392(5) . ?
C39 C40 1.389(5) . ?
C40 C41 1.398(5) . ?
C41 C42 1.363(6) . ?
C41 O45 1.380(4) . ?
C42 C43 1.385(5) . ?
C43 O44 1.405(4) . ?
O44 C46 1.380(4) . ?
C46 N52 1.290(4) . ?
C46 C47 1.418(5) . ?
C47 N49 1.292(4) . ?
C47 O48 1.377(4) . ?
N49 C50 1.381(5) . ?
C50 C51 1.399(6) . ?
C50 C53 1.403(5) . ?
C51 N52 1.379(5) . ?
C51 C56 1.414(6) . ?
C53 C54 1.373(6) . ?
C54 C55 1.375(7) . ?
C55 C56 1.361(7) . ?
C57 C58 1.502(6) . ?
C58 C59 1.515(5) . ?
C59 C60 1.512(5) . ?
C60 C61 1.500(5) . ?
C61 C62 1.511(5) . ?
C62 C63 1.508(5) . ?
C63 C64 1.512(5) . ?
C64 C65 1.509(5) . ?
C65 C66 1.512(5) . ?
C66 C67 1.511(6) . ?
C68 C69 1.516(5) . ?
C69 C70 1.517(5) . ?
C70 C71 1.517(5) . ?
C71 C72 1.515(5) . ?
C72 C73 1.515(5) . ?
C73 C74 1.512(5) . ?
C74 C75 1.519(5) . ?
C75 C76 1.519(7) . ?
C76 C77 1.377(8) . ?
C77 C78 1.522(7) . ?
C79 C80 1.523(5) . ?
C80 C81 1.526(5) . ?
C81 C82 1.512(5) . ?
C82 C83 1.520(5) . ?
C83 C84 1.511(5) . ?
C84 C85 1.508(5) . ?
C85 C86 1.509(5) . ?
C86 C87 1.514(5) . ?
C87 C88 1.505(5) . ?
C88 C89 1.517(6) . ?
C90 C91 1.550(7) . ?
C91 C92 1.558(10) . ?
C92 C93 1.562(14) . ?
C93 C94 1.533(12) . ?
C94 C95 1.450(11) . ?
C95 C96 1.543(12) . ?
C96 C97 1.413(13) . ?
C97 C98 1.550(13) . ?
C98 C99 1.449(12) . ?
C99 C100 1.490(13) . ?
O101 C102 1.219(5) . ?
C102 C103 1.467(6) . ?
C102 C104 1.475(6) . ?
O201 C202 1.307(8) . ?
C202 C204 1.356(13) . ?
C202 C203 1.492(12) . ?

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
C2 C1 C40 111.2(3) . . ?
C2 C1 C57 114.5(4) . . ?
C40 C1 C57 112.3(3) . . ?
C3 C2 C7 117.0(4) . . ?
C3 C2 C1 121.8(3) . . ?
C7 C2 C1 121.2(4) . . ?
C4 C3 C2 124.7(4) . . ?
C3 C4 C5 114.9(4) . . ?
C3 C4 C9 123.0(3) . . ?
C5 C4 C9 122.1(4) . . ?
C6 C5 C4 122.7(5) . . ?
C6 C5 O20 119.9(4) . . ?
C4 C5 O20 117.4(4) . . ?
C7 C6 C5 120.0(4) . . ?
C6 C7 O8 115.9(4) . . ?
C6 C7 C2 120.6(5) . . ?
O8 C7 C2 123.5(5) . . ?
C4 C9 C10 111.3(3) . . ?
C4 C9 C90 112.5(4) . . ?
C10 C9 C90 113.9(3) . . ?
C15 C10 C11 116.0(4) . . ?
C15 C10 C9 120.5(4) . . ?
C11 C10 C9 123.5(4) . . ?
C12 C11 C10 123.6(4) . . ?
C11 C12 C13 116.9(4) . . ?
C11 C12 C29 122.0(3) . . ?
C13 C12 C29 121.1(4) . . ?
C14 C13 O16 122.1(4) . . ?
C14 C13 C12 121.2(4) . . ?
O16 C13 C12 116.7(4) . . ?
C15 C14 C13 119.7(4) . . ?
C14 C15 C10 122.4(4) . . ?
C14 C15 O17 117.2(4) . . ?
C10 C15 O17 120.2(5) . . ?
C18 O17 C15 116.7(3) . . ?
N24 C18 O17 118.7(4) . . ?
N24 C18 C19 122.9(3) . . ?
O17 C18 C19 118.4(4) . . ?
N21 C19 O20 119.2(4) . . ?
N21 C19 C18 123.2(4) . . ?
O20 C19 C18 117.6(4) . . ?
C19 O20 C5 115.0(3) . . ?
C19 N21 C22 115.7(4) . . ?
C23 C22 N21 121.3(3) . . ?
C23 C22 C28 119.9(4) . . ?
N21 C22 C28 118.8(4) . . ?
C22 C23 N24 121.0(4) . . ?
C22 C23 C25 119.1(4) . . ?
N24 C23 C25 119.9(4) . . ?
C18 N24 C23 115.9(4) . . ?
C26 C25 C23 120.1(5) . . ?
C25 C26 C27 120.4(4) . . ?
C28 C27 C26 120.5(4) . . ?
C27 C28 C22 119.9(4) . . ?
C12 C29 C79 113.9(3) . . ?
C12 C29 C30 110.1(2) . . ?
C79 C29 C30 113.6(3) . . ?
C31 C30 C35 117.0(3) . . ?
C31 C30 C29 121.1(3) . . ?
C35 C30 C29 122.0(3) . . ?
C32 C31 C30 124.1(3) . . ?
C33 C32 C31 115.6(3) . . ?
C33 C32 C37 121.1(3) . . ?
C31 C32 C37 123.3(3) . . ?
C34 C33 C32 123.3(3) . . ?
C34 C33 O48 119.9(3) . . ?
C32 C33 O48 116.7(3) . . ?
C33 C34 C35 119.3(3) . . ?
O36 C35 C34 116.3(3) . . ?
O36 C35 C30 123.0(3) . . ?
C34 C35 C30 120.6(3) . . ?
C32 C37 C38 111.1(2) . . ?
C32 C37 C68 112.6(2) . . ?
C38 C37 C68 112.9(3) . . ?
C43 C38 C39 116.0(3) . . ?
C43 C38 C37 123.0(3) . . ?
C39 C38 C37 121.0(3) . . ?
C40 C39 C38 124.0(3) . . ?
C39 C40 C41 116.7(4) . . ?
C39 C40 C1 121.5(3) . . ?
C41 C40 C1 121.8(3) . . ?
C42 C41 O45 121.6(3) . . ?
C42 C41 C40 121.3(3) . . ?
O45 C41 C40 117.0(4) . . ?
C41 C42 C43 119.8(3) . . ?
C38 C43 C42 122.1(4) . . ?
C38 C43 O44 120.0(3) . . ?
C42 C43 O44 117.8(3) . . ?
C46 O44 C43 114.2(3) . . ?
N52 C46 O44 118.7(3) . . ?
N52 C46 C47 123.1(3) . . ?
O44 C46 C47 118.2(3) . . ?
N49 C47 O48 120.2(3) . . ?
N49 C47 C46 122.9(3) . . ?
O48 C47 C46 116.8(3) . . ?
C47 O48 C33 118.1(2) . . ?
C47 N49 C50 115.7(3) . . ?
N49 C50 C51 121.1(3) . . ?
N49 C50 C53 119.3(4) . . ?
C51 C50 C53 119.5(4) . . ?
N52 C51 C50 121.0(3) . . ?
N52 C51 C56 119.5(4) . . ?
C50 C51 C56 119.5(4) . . ?
C46 N52 C51 115.8(3) . . ?
C54 C53 C50 119.6(5) . . ?
C53 C54 C55 120.6(4) . . ?
C56 C55 C54 121.6(4) . . ?
C55 C56 C51 119.2(5) . . ?
C58 C57 C1 112.3(3) . . ?
C57 C58 C59 114.1(3) . . ?
C60 C59 C58 114.4(3) . . ?
C61 C60 C59 114.7(3) . . ?
C60 C61 C62 115.0(3) . . ?
C63 C62 C61 114.0(3) . . ?
C62 C63 C64 115.5(3) . . ?
C65 C64 C63 113.6(3) . . ?
C64 C65 C66 115.2(4) . . ?
C67 C66 C65 113.8(4) . . ?
C69 C68 C37 113.7(3) . . ?
C68 C69 C70 113.3(3) . . ?
C71 C70 C69 114.3(3) . . ?
C72 C71 C70 114.7(3) . . ?
C71 C72 C73 114.0(3) . . ?
C74 C73 C72 114.5(3) . . ?
C73 C74 C75 113.5(3) . . ?
C74 C75 C76 115.4(4) . . ?
C77 C76 C75 118.0(6) . . ?
C76 C77 C78 117.0(6) . . ?
C80 C79 C29 113.0(3) . . ?
C79 C80 C81 113.8(3) . . ?
C82 C81 C80 114.9(3) . . ?
C81 C82 C83 113.3(3) . . ?
C84 C83 C82 116.0(3) . . ?
C85 C84 C83 114.1(3) . . ?
C84 C85 C86 116.3(3) . . ?
C85 C86 C87 114.6(3) . . ?
C88 C87 C86 115.4(3) . . ?
C87 C88 C89 113.4(3) . . ?
C9 C90 C91 110.4(4) . . ?
C90 C91 C92 115.0(5) . . ?
C91 C92 C93 110.9(8) . . ?
C94 C93 C92 115.0(7) . . ?
C95 C94 C93 119.3(8) . . ?
C94 C95 C96 114.9(8) . . ?
C97 C96 C95 113.9(8) . . ?
C96 C97 C98 113.2(7) . . ?
C99 C98 C97 115.2(8) . . ?
C98 C99 C100 114.3(8) . . ?
O101 C102 C103 121.2(4) . . ?
O101 C102 C104 120.8(4) . . ?
C103 C102 C104 117.9(4) . . ?
O201 C202 C204 114.2(9) . . ?
O201 C202 C203 99.3(7) . . ?
C204 C202 C203 135.4(9) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C40 C1 C2 C3 -90.8(4) . . . . ?
C57 C1 C2 C3 37.8(5) . . . . ?
C40 C1 C2 C7 89.3(4) . . . . ?
C57 C1 C2 C7 -142.1(4) . . . . ?
C7 C2 C3 C4 1.5(6) . . . . ?
C1 C2 C3 C4 -178.4(3) . . . . ?
C2 C3 C4 C5 0.2(5) . . . . ?
C2 C3 C4 C9 -180.0(3) . . . . ?
C3 C4 C5 C6 -0.9(5) . . . . ?
C9 C4 C5 C6 179.2(4) . . . . ?
C3 C4 C5 O20 178.2(3) . . . . ?
C9 C4 C5 O20 -1.6(5) . . . . ?
C4 C5 C6 C7 0.0(6) . . . . ?
O20 C5 C6 C7 -179.1(3) . . . . ?
C5 C6 C7 O8 -179.5(3) . . . . ?
C5 C6 C7 C2 1.7(6) . . . . ?
C3 C2 C7 C6 -2.4(6) . . . . ?
C1 C2 C7 C6 177.5(4) . . . . ?
C3 C2 C7 O8 178.9(3) . . . . ?
C1 C2 C7 O8 -1.2(6) . . . . ?
C3 C4 C9 C10 86.4(4) . . . . ?
C5 C4 C9 C10 -93.8(4) . . . . ?
C3 C4 C9 C90 -42.8(5) . . . . ?
C5 C4 C9 C90 137.0(4) . . . . ?
C4 C9 C10 C15 91.3(4) . . . . ?
C90 C9 C10 C15 -140.3(4) . . . . ?
C4 C9 C10 C11 -88.2(4) . . . . ?
C90 C9 C10 C11 40.2(5) . . . . ?
C15 C10 C11 C12 1.1(5) . . . . ?
C9 C10 C11 C12 -179.4(3) . . . . ?
C10 C11 C12 C13 1.1(5) . . . . ?
C10 C11 C12 C29 -177.7(3) . . . . ?
C11 C12 C13 C14 -1.4(5) . . . . ?
C29 C12 C13 C14 177.5(3) . . . . ?
C11 C12 C13 O16 178.0(3) . . . . ?
C29 C12 C13 O16 -3.2(5) . . . . ?
O16 C13 C14 C15 -179.9(3) . . . . ?
C12 C13 C14 C15 -0.6(5) . . . . ?
C13 C14 C15 C10 3.0(6) . . . . ?
C13 C14 C15 O17 178.3(3) . . . . ?
C11 C10 C15 C14 -3.2(5) . . . . ?
C9 C10 C15 C14 177.3(3) . . . . ?
C11 C10 C15 O17 -178.3(3) . . . . ?
C9 C10 C15 O17 2.1(5) . . . . ?
C14 C15 O17 C18 78.6(5) . . . . ?
C10 C15 O17 C18 -106.0(4) . . . . ?
C15 O17 C18 N24 -79.5(5) . . . . ?
C15 O17 C18 C19 104.0(5) . . . . ?
N24 C18 C19 N21 -1.3(6) . . . . ?
O17 C18 C19 N21 175.1(3) . . . . ?
N24 C18 C19 O20 179.7(4) . . . . ?
O17 C18 C19 O20 -3.9(5) . . . . ?
N21 C19 O20 C5 80.5(4) . . . . ?
C18 C19 O20 C5 -100.4(4) . . . . ?
C6 C5 O20 C19 -71.8(5) . . . . ?
C4 C5 O20 C19 109.0(4) . . . . ?
O20 C19 N21 C22 -179.9(3) . . . . ?
C18 C19 N21 C22 1.1(6) . . . . ?
C19 N21 C22 C23 0.4(6) . . . . ?
C19 N21 C22 C28 -179.3(4) . . . . ?
N21 C22 C23 N24 -1.7(6) . . . . ?
C28 C22 C23 N24 178.0(4) . . . . ?
N21 C22 C23 C25 179.6(5) . . . . ?
C28 C22 C23 C25 -0.6(7) . . . . ?
O17 C18 N24 C23 -176.5(3) . . . . ?
C19 C18 N24 C23 -0.1(6) . . . . ?
C22 C23 N24 C18 1.5(6) . . . . ?
C25 C23 N24 C18 -179.9(5) . . . . ?
C22 C23 C25 C26 -1.6(9) . . . . ?
N24 C23 C25 C26 179.7(5) . . . . ?
C23 C25 C26 C27 2.5(9) . . . . ?
C25 C26 C27 C28 -1.0(9) . . . . ?
C26 C27 C28 C22 -1.3(7) . . . . ?
C23 C22 C28 C27 2.1(7) . . . . ?
N21 C22 C28 C27 -178.1(4) . . . . ?
C11 C12 C29 C79 -41.6(4) . . . . ?
C13 C12 C29 C79 139.6(3) . . . . ?
C11 C12 C29 C30 87.4(4) . . . . ?
C13 C12 C29 C30 -91.4(4) . . . . ?
C12 C29 C30 C31 -89.8(4) . . . . ?
C79 C29 C30 C31 39.3(4) . . . . ?
C12 C29 C30 C35 89.7(4) . . . . ?
C79 C29 C30 C35 -141.1(3) . . . . ?
C35 C30 C31 C32 -0.1(5) . . . . ?
C29 C30 C31 C32 179.5(3) . . . . ?
C30 C31 C32 C33 -1.1(4) . . . . ?
C30 C31 C32 C37 179.0(3) . . . . ?
C31 C32 C33 C34 2.2(5) . . . . ?
C37 C32 C33 C34 -177.9(3) . . . . ?
C31 C32 C33 O48 178.4(3) . . . . ?
C37 C32 C33 O48 -1.8(4) . . . . ?
C32 C33 C34 C35 -2.0(5) . . . . ?
O48 C33 C34 C35 -178.1(3) . . . . ?
C33 C34 C35 O36 179.4(3) . . . . ?
C33 C34 C35 C30 0.6(5) . . . . ?
C31 C30 C35 O36 -178.4(3) . . . . ?
C29 C30 C35 O36 2.0(5) . . . . ?
C31 C30 C35 C34 0.4(5) . . . . ?
C29 C30 C35 C34 -179.2(3) . . . . ?
C33 C32 C37 C38 -87.7(4) . . . . ?
C31 C32 C37 C38 92.1(3) . . . . ?
C33 C32 C37 C68 144.5(3) . . . . ?
C31 C32 C37 C68 -35.7(4) . . . . ?
C32 C37 C38 C43 95.3(4) . . . . ?
C68 C37 C38 C43 -137.1(3) . . . . ?
C32 C37 C38 C39 -85.0(3) . . . . ?
C68 C37 C38 C39 42.6(4) . . . . ?
C43 C38 C39 C40 1.8(5) . . . . ?
C37 C38 C39 C40 -177.9(3) . . . . ?
C38 C39 C40 C41 -1.5(5) . . . . ?
C38 C39 C40 C1 178.9(3) . . . . ?
C2 C1 C40 C39 85.8(4) . . . . ?
C57 C1 C40 C39 -43.9(5) . . . . ?
C2 C1 C40 C41 -93.8(4) . . . . ?
C57 C1 C40 C41 136.5(4) . . . . ?
C39 C40 C41 C42 -0.1(6) . . . . ?
C1 C40 C41 C42 179.6(4) . . . . ?
C39 C40 C41 O45 178.8(3) . . . . ?
C1 C40 C41 O45 -1.6(6) . . . . ?
O45 C41 C42 C43 -177.6(4) . . . . ?
C40 C41 C42 C43 1.2(6) . . . . ?
C39 C38 C43 C42 -0.6(5) . . . . ?
C37 C38 C43 C42 179.1(3) . . . . ?
C39 C38 C43 O44 -178.1(3) . . . . ?
C37 C38 C43 O44 1.6(5) . . . . ?
C41 C42 C43 C38 -0.9(6) . . . . ?
C41 C42 C43 O44 176.7(3) . . . . ?
C38 C43 O44 C46 -107.2(3) . . . . ?
C42 C43 O44 C46 75.2(4) . . . . ?
C43 O44 C46 N52 -88.0(4) . . . . ?
C43 O44 C46 C47 92.3(4) . . . . ?
N52 C46 C47 N49 5.6(6) . . . . ?
O44 C46 C47 N49 -174.8(3) . . . . ?
N52 C46 C47 O48 -171.1(3) . . . . ?
O44 C46 C47 O48 8.5(5) . . . . ?
N49 C47 O48 C33 70.3(4) . . . . ?
C46 C47 O48 C33 -112.9(3) . . . . ?
C34 C33 O48 C47 -74.3(4) . . . . ?
C32 C33 O48 C47 109.4(3) . . . . ?
O48 C47 N49 C50 173.0(3) . . . . ?
C46 C47 N49 C50 -3.6(5) . . . . ?
C47 N49 C50 C51 -1.3(5) . . . . ?
C47 N49 C50 C53 -179.0(3) . . . . ?
N49 C50 C51 N52 4.7(6) . . . . ?
C53 C50 C51 N52 -177.6(4) . . . . ?
N49 C50 C51 C56 -175.7(4) . . . . ?
C53 C50 C51 C56 1.9(6) . . . . ?
O44 C46 N52 C51 178.4(3) . . . . ?
C47 C46 N52 C51 -1.9(5) . . . . ?
C50 C51 N52 C46 -2.9(6) . . . . ?
C56 C51 N52 C46 177.6(4) . . . . ?
N49 C50 C53 C54 176.8(4) . . . . ?
C51 C50 C53 C54 -0.9(6) . . . . ?
C50 C53 C54 C55 -1.2(7) . . . . ?
C53 C54 C55 C56 2.3(8) . . . . ?
C54 C55 C56 C51 -1.2(8) . . . . ?
N52 C51 C56 C55 178.7(5) . . . . ?
C50 C51 C56 C55 -0.9(7) . . . . ?
C2 C1 C57 C58 168.0(3) . . . . ?
C40 C1 C57 C58 -63.9(4) . . . . ?
C1 C57 C58 C59 -179.2(3) . . . . ?
C57 C58 C59 C60 173.2(4) . . . . ?
C58 C59 C60 C61 -178.6(4) . . . . ?
C59 C60 C61 C62 176.4(4) . . . . ?
C60 C61 C62 C63 -178.1(4) . . . . ?
C61 C62 C63 C64 -179.7(4) . . . . ?
C62 C63 C64 C65 -179.0(4) . . . . ?
C63 C64 C65 C66 -178.1(4) . . . . ?
C64 C65 C66 C67 -179.1(4) . . . . ?
C32 C37 C68 C69 -171.8(3) . . . . ?
C38 C37 C68 C69 61.3(4) . . . . ?
C37 C68 C69 C70 -178.2(3) . . . . ?
C68 C69 C70 C71 -178.6(3) . . . . ?
C69 C70 C71 C72 179.1(3) . . . . ?
C70 C71 C72 C73 -178.6(3) . . . . ?
C71 C72 C73 C74 179.7(4) . . . . ?
C72 C73 C74 C75 179.4(4) . . . . ?
C73 C74 C75 C76 -171.8(5) . . . . ?
C74 C75 C76 C77 -70.4(7) . . . . ?
C75 C76 C77 C78 175.7(5) . . . . ?
C12 C29 C79 C80 -169.1(3) . . . . ?
C30 C29 C79 C80 63.7(4) . . . . ?
C29 C79 C80 C81 -175.9(3) . . . . ?
C79 C80 C81 C82 78.2(4) . . . . ?
C80 C81 C82 C83 -176.6(3) . . . . ?
C81 C82 C83 C84 -171.7(3) . . . . ?
C82 C83 C84 C85 -178.9(3) . . . . ?
C83 C84 C85 C86 -178.2(3) . . . . ?
C84 C85 C86 C87 -178.3(3) . . . . ?
C85 C86 C87 C88 -179.9(3) . . . . ?
C86 C87 C88 C89 -178.6(4) . . . . ?
C4 C9 C90 C91 -67.7(6) . . . . ?
C10 C9 C90 C91 164.5(5) . . . . ?
C9 C90 C91 C92 172.1(7) . . . . ?
C90 C91 C92 C93 -97.2(9) . . . . ?
C91 C92 C93 C94 180.0(6) . . . . ?
C92 C93 C94 C95 -178.0(8) . . . . ?
C93 C94 C95 C96 177.2(6) . . . . ?
C94 C95 C96 C97 179.6(7) . . . . ?
C95 C96 C97 C98 178.6(6) . . . . ?
C96 C97 C98 C99 -179.2(6) . . . . ?
C97 C98 C99 C100 179.1(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        22.99
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.609
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.041