# Supplementary Material (ESI) for Organic & Biomolecular Chemistry
# This journal is (c) The Royal Society of Chemistry 2009


data_global
_journal_name_full               Org.Biomol.Chem.
_journal_coden_cambridge         0177
#==============================================================================

# 1. SUBMISSION DETAILS

_publ_contact_author             
# Name and address of author for correspondence
;
Dr. Michael Bolte
Institut f\"ur Anorganische Chemie
J. W. Goethe-Universit\"at
Marie-Curie-Str. 11
60439 Frankfurt/Main
Germany
;
_publ_contact_author_phone       '49 69 798 29136'
_publ_contact_author_fax         '49 69 798 29239'
_publ_contact_author_email       bolte@chemie.uni-frankfurt.de
_publ_requested_coeditor_name    ' '

_publ_contact_letter             
;
Please consider this CIF submission as supplemenatry material for
a manucript
intended for publication in Org. Biomol. Chem.

;

#==============================================================================

_publ_section_title              
;
Sildenafil citrate monohydrate
;

# The loop structure below should contain the names and addresses of all
# authors, in the required order of publication. Repeat as necessary.

loop_
_publ_author_name
_publ_author_address

V.Bohmer
; Institut f\"ur Anorganische Chemie
J. W. Goethe-Universit\"at Frankfurt
Marie-Curie-Str. 11
60439 Frankfurt/Main
Germany
;
G.Podoprygorina
; Institut f\"ur Anorganische Chemie
J. W. Goethe-Universit\"at Frankfurt
Marie-Curie-Str. 11
60439 Frankfurt/Main
Germany
;
M.Bolte
; Institut f\"ur Anorganische Chemie
J. W. Goethe-Universit\"at Frankfurt
Marie-Curie-Str. 11
60439 Frankfurt/Main
Germany
;

#==============================================================================

_publ_section_references         
;
Allen, F. H. (2002). Acta Cryst., B58, 380-388.

Blessing, R.H. (1995). Acta Cryst. A51, 33-38.

Sheldrick, G.M. (1990). Acta Cryst. A46, 467 - 473.

Sheldrick, G.M. (1997). SHELXL-97. Program for the refinement of crystal
structures. Univ. of G\"ottingen, Federal Republic of Germany.

Stoe & Cie (2001). X-Area. Area-Detector Control and Integration
Software. Stoe & Cie, Darmstadt, Germany.

Spek, A.L. (2003). J. Appl. Cryst. 36, 7-13.

;
_publ_section_figure_captions    
;
Fig. 1. Perspective view of the title compound with the atom numbering;
displacement ellipsoids are at the 30% probability level.

Fig. 2. Least-squares fit sildenafil (open bonds) and iso-sildenafil
(closed bonds). The phenyl ring, the SO~2~ group and the piperazine
ring were fitted (rmsd = 0.122\%A).

;
_publ_section_acknowledgements   
;

;
#==============================================================================

# start Validation Reply Form
_vrf_PLAT213_boeh38              
;
PROBLEM: Atom C271 has ADP max/min Ratio ............. 5.50 prola
RESPONSE: This is a terminal methyl group.
;
_vrf_PLAT220_boeh38              
;
PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 10.00 Ratio
RESPONSE: This is a terminal methyl group.
;
_vrf_PLAT222_boeh38              
;
PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 10.00 Ratio
RESPONSE: This is a terminal methyl group.
;
_vrf_PLAT242_boeh38              
;
PROBLEM: Check Low Ueq as Compared to Neighbors for C27
RESPONSE: This is the central atom of t-butyl group.
;
_vrf_PLAT213_boeh63              
;
PROBLEM: Atom O251 has ADP max/min Ratio ............. 6.20 prola
RESPONSE: This is a terminal nitro group.
;
_vrf_PLAT220_boeh63              
;
PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 6.43 Ratio
RESPONSE: This is a terminal propyl group.
;
_vrf_PLAT222_boeh63              
;
PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 7.44 Ratio
RESPONSE: This is a terminal propyl group.
;
_vrf_PLAT773_boeh63              
;
PROBLEM: Suspect C-C Bond in CIF: C222 -- C223 .. 1.72 Ang.
RESPONSE: This is a terminal propyl group.
;
_publ_contact_author_name        'Dr. Michael Bolte'
# end Validation Reply Form

data_boeh38
_database_code_depnum_ccdc_archive 'CCDC 706486'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C65 H89 I N2 O8'
_chemical_formula_weight         1153.28

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'
I I -0.4742 1.8119 '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           Orthorhombic
_symmetry_space_group_name_H-M   'P 212121'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   11.2099(5)
_cell_length_b                   15.8759(6)
_cell_length_c                   35.5340(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6323.9(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    46189
_cell_measurement_theta_min      2.0
_cell_measurement_theta_max      25.4

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2440
_exptl_absorpt_coefficient_mu    0.559
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8285
_exptl_absorpt_correction_T_max  0.8730
_exptl_absorpt_process_details   'MULABS (Spek, 1990; Blessing, 1995)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            35791
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_sigmaI/netI    0.0342
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_theta_min         1.90
_diffrn_reflns_theta_max         25.02
_reflns_number_total             11121
_reflns_number_gt                10497
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 1991)'
_computing_publication_material  ?

_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^)+(0.0766P)^2^+1.4230P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.013(11)
_refine_ls_number_reflns         11121
_refine_ls_number_parameters     686
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0387
_refine_ls_wR_factor_ref         0.1082
_refine_ls_wR_factor_gt          0.1059
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.012
_refine_ls_shift/su_max          0.009
_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
C1 C 0.5211(3) 0.3375(2) 0.59319(8) 0.0349(6) Uani 1 1 d . . .
H1A H 0.4880 0.3948 0.5898 0.042 Uiso 1 1 calc R . .
H1B H 0.4606 0.2962 0.5847 0.042 Uiso 1 1 calc R . .
C11 C 0.6345(3) 0.32776(19) 0.56990(7) 0.0328(6) Uani 1 1 d . . .
C12 C 0.7214(3) 0.39044(19) 0.56935(7) 0.0329(6) Uani 1 1 d . . .
C13 C 0.8351(3) 0.37410(18) 0.55425(7) 0.0346(6) Uani 1 1 d . . .
C14 C 0.8544(3) 0.2970(2) 0.53643(8) 0.0384(6) Uani 1 1 d . . .
H14 H 0.9300 0.2864 0.5253 0.046 Uiso 1 1 calc R . .
C15 C 0.7672(3) 0.2351(2) 0.53434(9) 0.0397(7) Uani 1 1 d . . .
C16 C 0.6579(3) 0.25203(19) 0.55187(8) 0.0367(6) Uani 1 1 d . . .
H16 H 0.5975 0.2101 0.5514 0.044 Uiso 1 1 calc R . .
C17 C 0.7865(4) 0.1535(2) 0.51206(11) 0.0496(8) Uani 1 1 d . . .
C171 C 0.7038(4) 0.0822(2) 0.52465(12) 0.0615(10) Uani 1 1 d . . .
H17A H 0.6208 0.1014 0.5236 0.092 Uiso 1 1 calc R . .
H17B H 0.7236 0.0658 0.5505 0.092 Uiso 1 1 calc R . .
H17C H 0.7140 0.0336 0.5079 0.092 Uiso 1 1 calc R . .
C172 C 0.7573(5) 0.1716(3) 0.47000(11) 0.0703(12) Uani 1 1 d . . .
H17D H 0.6743 0.1904 0.4678 0.105 Uiso 1 1 calc R . .
H17E H 0.7685 0.1201 0.4552 0.105 Uiso 1 1 calc R . .
H17F H 0.8106 0.2157 0.4605 0.105 Uiso 1 1 calc R . .
C173 C 0.9160(5) 0.1241(3) 0.51457(17) 0.0769(14) Uani 1 1 d . . .
H17G H 0.9690 0.1698 0.5066 0.115 Uiso 1 1 calc R . .
H17H H 0.9276 0.0752 0.4981 0.115 Uiso 1 1 calc R . .
H17I H 0.9345 0.1084 0.5406 0.115 Uiso 1 1 calc R . .
O12 O 0.7012(2) 0.46731(14) 0.58618(5) 0.0359(4) Uani 1 1 d . . .
C121 C 0.6223(3) 0.5218(2) 0.56511(8) 0.0431(7) Uani 1 1 d . . .
H12A H 0.5964 0.5690 0.5814 0.052 Uiso 1 1 calc R . .
H12B H 0.5504 0.4897 0.5576 0.052 Uiso 1 1 calc R . .
C122 C 0.6824(4) 0.5572(2) 0.53001(9) 0.0513(9) Uani 1 1 d . . .
H12C H 0.7563 0.5871 0.5374 0.062 Uiso 1 1 calc R . .
H12D H 0.7052 0.5101 0.5132 0.062 Uiso 1 1 calc R . .
C123 C 0.6014(4) 0.6176(2) 0.50860(9) 0.0568(10) Uani 1 1 d . . .
H12E H 0.6391 0.6335 0.4844 0.068 Uiso 1 1 calc R . .
H12F H 0.5243 0.5899 0.5031 0.068 Uiso 1 1 calc R . .
N124 N 0.5812(3) 0.69301(18) 0.53145(7) 0.0440(6) Uani 1 1 d . . .
H124 H 0.6289 0.7019 0.5507 0.053 Uiso 1 1 calc R . .
C125 C 0.4950(3) 0.7492(2) 0.52485(8) 0.0373(6) Uani 1 1 d . . .
O125 O 0.4285(2) 0.74661(17) 0.49686(7) 0.0476(6) Uani 1 1 d . . .
C2 C 0.9351(3) 0.4373(2) 0.55987(8) 0.0386(6) Uani 1 1 d . . .
H2A H 0.9995 0.4263 0.5414 0.046 Uiso 1 1 calc R . .
H2B H 0.9045 0.4950 0.5554 0.046 Uiso 1 1 calc R . .
C21 C 0.9849(2) 0.4312(2) 0.59959(8) 0.0342(6) Uani 1 1 d . . .
C22 C 0.9822(2) 0.49774(19) 0.62521(8) 0.0318(6) Uani 1 1 d . . .
C23 C 1.0168(2) 0.48643(19) 0.66261(8) 0.0323(6) Uani 1 1 d . . .
C24 C 1.0617(3) 0.4080(2) 0.67324(8) 0.0371(6) Uani 1 1 d . . .
H24 H 1.0864 0.4003 0.6986 0.045 Uiso 1 1 calc R . .
C25 C 1.0718(3) 0.3409(2) 0.64860(9) 0.0414(7) Uani 1 1 d . . .
C26 C 1.0293(3) 0.3535(2) 0.61204(9) 0.0408(7) Uani 1 1 d . . .
H26 H 1.0306 0.3075 0.5949 0.049 Uiso 1 1 calc R . .
O22 O 0.94041(16) 0.57643(13) 0.61321(5) 0.0331(4) Uani 1 1 d . . .
C221 C 1.0342(3) 0.6360(2) 0.60541(9) 0.0376(7) Uani 1 1 d . . .
H22A H 1.0964 0.6307 0.6250 0.045 Uiso 1 1 calc R . .
H22B H 1.0011 0.6937 0.6070 0.045 Uiso 1 1 calc R . .
C222 C 1.0909(3) 0.6244(3) 0.56756(10) 0.0512(9) Uani 1 1 d . . .
H22C H 1.0287 0.6266 0.5478 0.061 Uiso 1 1 calc R . .
H22D H 1.1297 0.5684 0.5664 0.061 Uiso 1 1 calc R . .
C223 C 1.1846(4) 0.6937(4) 0.56016(13) 0.0774(15) Uani 1 1 d . . .
H22E H 1.2211 0.6846 0.5354 0.116 Uiso 1 1 calc R . .
H22F H 1.2463 0.6914 0.5797 0.116 Uiso 1 1 calc R . .
H22G H 1.1458 0.7490 0.5607 0.116 Uiso 1 1 calc R . .
C27 C 1.1140(4) 0.2529(2) 0.66170(11) 0.0572(10) Uani 1 1 d . . .
C271 C 1.0149(8) 0.2022(6) 0.6690(6) 0.317(12) Uani 1 1 d . . .
H27A H 0.9638 0.2297 0.6877 0.476 Uiso 1 1 calc R . .
H27B H 1.0415 0.1476 0.6787 0.476 Uiso 1 1 calc R . .
H27C H 0.9697 0.1937 0.6457 0.476 Uiso 1 1 calc R . .
C272 C 1.2001(8) 0.2169(4) 0.63439(18) 0.124(3) Uani 1 1 d . . .
H27D H 1.2682 0.2551 0.6317 0.186 Uiso 1 1 calc R . .
H27E H 1.1609 0.2098 0.6099 0.186 Uiso 1 1 calc R . .
H27F H 1.2279 0.1621 0.6435 0.186 Uiso 1 1 calc R . .
C273 C 1.1894(11) 0.2597(5) 0.6973(2) 0.183(6) Uani 1 1 d . . .
H27G H 1.2593 0.2951 0.6924 0.274 Uiso 1 1 calc R . .
H27H H 1.2157 0.2034 0.7050 0.274 Uiso 1 1 calc R . .
H27I H 1.1417 0.2850 0.7175 0.274 Uiso 1 1 calc R . .
C3 C 0.9978(3) 0.55238(19) 0.69313(8) 0.0344(6) Uani 1 1 d . . .
H3A H 1.0751 0.5668 0.7050 0.041 Uiso 1 1 calc R . .
H3B H 0.9640 0.6042 0.6820 0.041 Uiso 1 1 calc R . .
C31 C 0.9129(3) 0.51744(18) 0.72262(8) 0.0311(6) Uani 1 1 d . . .
C32 C 0.7917(2) 0.50934(18) 0.71459(7) 0.0291(6) Uani 1 1 d . . .
C33 C 0.7142(3) 0.46515(18) 0.73800(8) 0.0300(6) Uani 1 1 d . . .
C34 C 0.7604(3) 0.4325(2) 0.77141(8) 0.0344(6) Uani 1 1 d . . .
H34 H 0.7084 0.4033 0.7880 0.041 Uiso 1 1 calc R . .
C35 C 0.8805(3) 0.44115(19) 0.78139(8) 0.0349(6) Uani 1 1 d . . .
C36 C 0.9557(3) 0.48355(19) 0.75652(8) 0.0346(6) Uani 1 1 d . . .
H36 H 1.0377 0.4896 0.7627 0.042 Uiso 1 1 calc R . .
C37 C 0.9270(3) 0.3982(2) 0.81758(9) 0.0476(8) Uani 1 1 d . . .
C371 C 0.8510(5) 0.4254(5) 0.85110(11) 0.099(2) Uani 1 1 d . . .
H37A H 0.7672 0.4114 0.8463 0.148 Uiso 1 1 calc R . .
H37B H 0.8588 0.4863 0.8548 0.148 Uiso 1 1 calc R . .
H37C H 0.8781 0.3959 0.8738 0.148 Uiso 1 1 calc R . .
C372 C 1.0558(4) 0.4195(4) 0.82559(14) 0.0862(17) Uani 1 1 d . . .
H37D H 1.0634 0.4802 0.8299 0.129 Uiso 1 1 calc R . .
H37E H 1.1052 0.4032 0.8040 0.129 Uiso 1 1 calc R . .
H37F H 1.0825 0.3889 0.8480 0.129 Uiso 1 1 calc R . .
C373 C 0.9187(6) 0.3032(3) 0.81127(17) 0.0947(19) Uani 1 1 d . . .
H37G H 0.8356 0.2876 0.8062 0.142 Uiso 1 1 calc R . .
H37H H 0.9467 0.2736 0.8338 0.142 Uiso 1 1 calc R . .
H37I H 0.9684 0.2873 0.7897 0.142 Uiso 1 1 calc R . .
O32 O 0.75052(19) 0.54197(14) 0.68047(5) 0.0347(4) Uani 1 1 d . . .
C321 C 0.6801(3) 0.6166(2) 0.68434(9) 0.0420(7) Uani 1 1 d . . .
H32A H 0.6154 0.6057 0.7027 0.050 Uiso 1 1 calc R . .
H32B H 0.6426 0.6296 0.6598 0.050 Uiso 1 1 calc R . .
C322 C 0.7512(3) 0.6930(2) 0.69732(10) 0.0466(8) Uani 1 1 d . . .
H32C H 0.7885 0.6808 0.7220 0.056 Uiso 1 1 calc R . .
H32D H 0.8157 0.7048 0.6790 0.056 Uiso 1 1 calc R . .
C323 C 0.6715(4) 0.7697(2) 0.70086(9) 0.0476(8) Uani 1 1 d . . .
H32E H 0.6028 0.7567 0.7174 0.057 Uiso 1 1 calc R . .
H32F H 0.7167 0.8168 0.7122 0.057 Uiso 1 1 calc R . .
N324 N 0.6288(3) 0.79386(18) 0.66341(7) 0.0412(6) Uani 1 1 d . . .
H324 H 0.6635 0.7721 0.6434 0.049 Uiso 1 1 calc R . .
C325 C 0.5389(3) 0.8479(2) 0.65866(8) 0.0381(7) Uani 1 1 d . . .
O325 O 0.4894(3) 0.88434(19) 0.68465(6) 0.0594(7) Uani 1 1 d . . .
C4 C 0.5863(3) 0.44421(19) 0.72689(8) 0.0335(6) Uani 1 1 d . . .
H4A H 0.5410 0.4271 0.7496 0.040 Uiso 1 1 calc R . .
H4B H 0.5477 0.4950 0.7163 0.040 Uiso 1 1 calc R . .
C41 C 0.5824(2) 0.37364(19) 0.69806(8) 0.0310(6) Uani 1 1 d . . .
C42 C 0.5454(2) 0.38786(19) 0.66086(8) 0.0296(6) Uani 1 1 d . . .
C43 C 0.5499(2) 0.32282(19) 0.63457(8) 0.0317(6) Uani 1 1 d . . .
C44 C 0.5811(3) 0.2434(2) 0.64625(9) 0.0373(6) Uani 1 1 d . . .
H44 H 0.5814 0.1990 0.6283 0.045 Uiso 1 1 calc R . .
C45 C 0.6127(3) 0.2249(2) 0.68360(9) 0.0376(7) Uani 1 1 d . . .
C46 C 0.6141(3) 0.2927(2) 0.70848(8) 0.0351(6) Uani 1 1 d . . .
H46 H 0.6380 0.2830 0.7338 0.042 Uiso 1 1 calc R . .
C47 C 0.6282(4) 0.1331(2) 0.69607(10) 0.0512(9) Uani 1 1 d . . .
C471 C 0.6887(4) 0.0799(3) 0.66596(13) 0.0611(10) Uani 1 1 d . . .
H47A H 0.6977 0.0220 0.6751 0.092 Uiso 1 1 calc R . .
H47B H 0.7674 0.1035 0.6603 0.092 Uiso 1 1 calc R . .
H47C H 0.6398 0.0799 0.6431 0.092 Uiso 1 1 calc R . .
C472 C 0.5018(5) 0.0971(3) 0.70217(18) 0.0878(18) Uani 1 1 d . . .
H47D H 0.5076 0.0383 0.7104 0.132 Uiso 1 1 calc R . .
H47E H 0.4569 0.1001 0.6785 0.132 Uiso 1 1 calc R . .
H47F H 0.4606 0.1302 0.7215 0.132 Uiso 1 1 calc R . .
C473 C 0.7018(9) 0.1272(3) 0.73216(17) 0.127(3) Uani 1 1 d . . .
H47G H 0.7107 0.0679 0.7394 0.191 Uiso 1 1 calc R . .
H47H H 0.6611 0.1578 0.7524 0.191 Uiso 1 1 calc R . .
H47I H 0.7807 0.1519 0.7279 0.191 Uiso 1 1 calc R . .
O42 O 0.50250(17) 0.46665(13) 0.65032(5) 0.0315(4) Uani 1 1 d . . .
C421 C 0.3742(3) 0.4687(2) 0.65183(10) 0.0460(8) Uani 1 1 d . . .
H42A H 0.3473 0.4671 0.6784 0.055 Uiso 1 1 calc R . .
H42B H 0.3411 0.4189 0.6387 0.055 Uiso 1 1 calc R . .
C422 C 0.3303(3) 0.5485(3) 0.63314(11) 0.0530(9) Uani 1 1 d . . .
H42C H 0.3695 0.5541 0.6083 0.064 Uiso 1 1 calc R . .
H42D H 0.2434 0.5434 0.6287 0.064 Uiso 1 1 calc R . .
C423 C 0.3531(4) 0.6273(3) 0.65545(13) 0.0655(11) Uani 1 1 d . . .
H42E H 0.3226 0.6761 0.6416 0.098 Uiso 1 1 calc R . .
H42F H 0.4391 0.6338 0.6595 0.098 Uiso 1 1 calc R . .
H42G H 0.3125 0.6233 0.6798 0.098 Uiso 1 1 calc R . .
C51 C 0.4811(3) 0.81647(19) 0.55393(8) 0.0346(6) Uani 1 1 d . . .
C52 C 0.5137(3) 0.80111(19) 0.59121(8) 0.0352(6) Uani 1 1 d . . .
H52 H 0.5440 0.7474 0.5981 0.042 Uiso 1 1 calc R . .
C53 C 0.5020(3) 0.8637(2) 0.61826(8) 0.0338(6) Uani 1 1 d . . .
C54 C 0.4527(3) 0.9409(2) 0.60879(8) 0.0363(6) Uani 1 1 d . . .
H54 H 0.4421 0.9833 0.6273 0.044 Uiso 1 1 calc R . .
C55 C 0.4191(3) 0.9550(2) 0.57170(9) 0.0373(6) Uani 1 1 d . . .
C56 C 0.4325(3) 0.8936(2) 0.54395(8) 0.0353(6) Uani 1 1 d . . .
H56 H 0.4088 0.9044 0.5187 0.042 Uiso 1 1 calc R . .
I1 I 0.34508(2) 1.072676(14) 0.557078(6) 0.05257(9) Uani 1 1 d . . .
O1M O 0.3923(3) 0.6816(2) 0.42833(8) 0.0753(9) Uani 1 1 d . . .
H1M H 0.4035 0.7024 0.4501 0.090 Uiso 1 1 d R . .
C1M C 0.3256(6) 0.6069(3) 0.43229(14) 0.0852(16) Uani 1 1 d . . .
H1M1 H 0.3798 0.5594 0.4363 0.128 Uiso 1 1 calc R . .
H1M2 H 0.2787 0.5973 0.4094 0.128 Uiso 1 1 calc R . .
H1M3 H 0.2717 0.6122 0.4539 0.128 Uiso 1 1 calc R . .
O1W O 0.7492(2) 0.69664(19) 0.59938(8) 0.0601(7) Uani 1 1 d . . .
H1WA H 0.8170 0.7173 0.5938 0.072 Uiso 1 1 d R . .
H1WB H 0.7588 0.6459 0.6067 0.072 Uiso 1 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
C1 0.0360(15) 0.0398(16) 0.0288(14) -0.0006(12) -0.0048(12) 0.0026(13)
C11 0.0349(15) 0.0385(16) 0.0249(12) 0.0022(11) -0.0025(11) 0.0039(12)
C12 0.0437(16) 0.0334(14) 0.0217(12) 0.0016(10) -0.0001(11) 0.0056(13)
C13 0.0401(15) 0.0375(15) 0.0261(12) 0.0040(11) -0.0002(13) -0.0028(12)
C14 0.0422(16) 0.0415(16) 0.0315(13) 0.0047(11) 0.0078(13) 0.0032(14)
C15 0.0493(18) 0.0348(16) 0.0350(15) 0.0041(12) 0.0048(13) 0.0024(14)
C16 0.0433(15) 0.0352(14) 0.0318(13) -0.0020(11) 0.0046(13) -0.0002(13)
C17 0.058(2) 0.0376(18) 0.0533(19) -0.0013(15) 0.0168(17) 0.0014(16)
C171 0.076(3) 0.041(2) 0.067(2) -0.0089(18) 0.018(2) -0.0049(19)
C172 0.097(3) 0.065(3) 0.049(2) -0.020(2) 0.015(2) -0.007(2)
C173 0.069(3) 0.054(3) 0.108(4) -0.014(2) 0.011(3) 0.015(2)
O12 0.0448(11) 0.0335(11) 0.0295(9) -0.0015(8) 0.0001(8) 0.0006(9)
C121 0.0571(19) 0.0351(16) 0.0371(15) 0.0010(12) 0.0012(14) 0.0108(14)
C122 0.082(3) 0.0350(17) 0.0369(15) 0.0004(13) 0.0150(16) 0.0174(17)
C123 0.100(3) 0.0400(18) 0.0307(15) -0.0023(14) 0.0029(17) 0.017(2)
N124 0.0615(18) 0.0361(14) 0.0345(13) -0.0036(11) -0.0056(12) 0.0122(13)
C125 0.0454(17) 0.0356(15) 0.0307(14) 0.0018(12) 0.0016(13) -0.0001(13)
O125 0.0530(14) 0.0554(14) 0.0345(11) -0.0062(10) -0.0079(10) 0.0044(12)
C2 0.0438(15) 0.0392(16) 0.0329(14) 0.0061(13) 0.0052(13) -0.0034(13)
C21 0.0302(13) 0.0385(15) 0.0340(13) 0.0060(13) 0.0060(11) -0.0017(13)
C22 0.0246(12) 0.0314(15) 0.0394(14) 0.0071(12) 0.0033(11) -0.0005(11)
C23 0.0248(13) 0.0361(15) 0.0361(14) 0.0036(12) 0.0029(11) -0.0016(11)
C24 0.0359(15) 0.0416(17) 0.0339(14) 0.0087(12) 0.0040(12) 0.0042(12)
C25 0.0458(17) 0.0379(17) 0.0406(16) 0.0096(13) 0.0102(14) 0.0094(14)
C26 0.0460(18) 0.0364(16) 0.0401(16) 0.0037(13) 0.0089(14) 0.0047(14)
O22 0.0252(9) 0.0324(10) 0.0418(10) 0.0078(9) -0.0010(8) -0.0013(9)
C221 0.0311(15) 0.0331(15) 0.0486(17) 0.0120(13) -0.0052(12) -0.0065(12)
C222 0.0454(18) 0.065(2) 0.0435(17) 0.0170(16) -0.0039(14) -0.0143(17)
C223 0.052(2) 0.110(4) 0.070(3) 0.045(3) -0.006(2) -0.035(2)
C27 0.077(3) 0.0391(19) 0.055(2) 0.0144(16) 0.0125(19) 0.0231(18)
C271 0.090(5) 0.121(7) 0.74(3) 0.257(14) 0.039(11) 0.010(5)
C272 0.186(8) 0.093(4) 0.093(4) 0.026(3) 0.038(4) 0.092(5)
C273 0.349(16) 0.098(5) 0.100(5) -0.002(4) -0.081(7) 0.132(8)
C3 0.0277(14) 0.0385(16) 0.0369(14) 0.0029(12) 0.0011(11) -0.0037(11)
C31 0.0348(15) 0.0292(14) 0.0292(13) -0.0001(11) 0.0021(11) -0.0016(11)
C32 0.0309(13) 0.0317(14) 0.0248(12) 0.0018(11) -0.0015(10) 0.0012(12)
C33 0.0317(14) 0.0312(14) 0.0269(13) -0.0011(11) 0.0009(11) 0.0003(11)
C34 0.0365(14) 0.0355(15) 0.0310(13) 0.0039(12) 0.0026(11) 0.0016(13)
C35 0.0382(15) 0.0339(16) 0.0325(13) 0.0023(11) -0.0011(11) 0.0044(12)
C36 0.0293(14) 0.0380(16) 0.0366(15) 0.0022(12) -0.0054(12) 0.0031(12)
C37 0.0514(19) 0.054(2) 0.0373(16) 0.0124(14) -0.0060(14) 0.0032(16)
C371 0.093(4) 0.168(6) 0.0350(18) 0.019(3) 0.003(2) 0.039(5)
C372 0.062(3) 0.128(5) 0.068(3) 0.040(3) -0.024(2) -0.001(3)
C373 0.122(5) 0.064(3) 0.098(4) 0.036(3) -0.036(4) 0.007(3)
O32 0.0341(10) 0.0425(11) 0.0274(9) 0.0063(8) -0.0017(8) 0.0004(9)
C321 0.0405(17) 0.0433(17) 0.0422(16) 0.0110(13) -0.0088(13) -0.0007(14)
C322 0.0534(19) 0.0437(19) 0.0429(17) 0.0026(14) -0.0167(15) 0.0019(16)
C323 0.061(2) 0.0487(19) 0.0333(15) 0.0035(13) -0.0141(15) 0.0041(17)
N324 0.0493(16) 0.0454(15) 0.0289(12) 0.0027(10) -0.0030(11) 0.0148(13)
C325 0.0410(17) 0.0425(17) 0.0307(14) 0.0005(12) 0.0009(12) 0.0041(14)
O325 0.0713(17) 0.0756(19) 0.0313(11) -0.0044(11) 0.0020(11) 0.0284(15)
C4 0.0325(15) 0.0385(17) 0.0296(13) -0.0008(11) 0.0033(11) -0.0011(12)
C41 0.0273(13) 0.0366(16) 0.0292(13) 0.0006(11) 0.0023(10) -0.0014(11)
C42 0.0227(13) 0.0343(14) 0.0318(13) 0.0017(11) -0.0003(10) -0.0022(11)
C43 0.0274(14) 0.0380(16) 0.0298(13) 0.0021(11) -0.0003(11) -0.0004(11)
C44 0.0409(16) 0.0348(15) 0.0363(15) -0.0004(12) 0.0002(13) -0.0021(13)
C45 0.0416(16) 0.0341(16) 0.0372(15) 0.0058(12) 0.0022(12) 0.0002(13)
C46 0.0373(15) 0.0388(16) 0.0293(13) 0.0084(12) 0.0005(11) -0.0021(12)
C47 0.073(3) 0.0335(17) 0.0469(18) 0.0105(14) 0.0001(17) 0.0073(16)
C471 0.061(2) 0.0395(19) 0.082(3) 0.0091(19) 0.011(2) 0.0088(17)
C472 0.107(4) 0.043(2) 0.114(4) 0.021(2) 0.059(4) -0.001(2)
C473 0.246(10) 0.051(3) 0.084(4) 0.010(2) -0.076(5) 0.030(4)
O42 0.0230(9) 0.0352(10) 0.0363(10) 0.0045(8) -0.0002(8) 0.0030(8)
C421 0.0257(15) 0.053(2) 0.0594(19) 0.0068(16) -0.0007(13) 0.0046(13)
C422 0.0329(17) 0.065(2) 0.061(2) 0.0071(17) -0.0047(15) 0.0134(16)
C423 0.052(2) 0.061(2) 0.083(3) 0.002(2) -0.017(2) 0.014(2)
C51 0.0331(13) 0.0375(15) 0.0332(14) 0.0002(13) 0.0002(12) 0.0023(12)
C52 0.0358(15) 0.0339(16) 0.0358(15) 0.0067(12) 0.0024(12) 0.0062(13)
C53 0.0329(14) 0.0387(16) 0.0297(14) 0.0021(11) 0.0022(11) 0.0025(12)
C54 0.0382(15) 0.0361(17) 0.0346(14) -0.0033(12) 0.0021(12) 0.0083(13)
C55 0.0379(15) 0.0339(15) 0.0400(15) 0.0020(12) -0.0004(12) 0.0088(12)
C56 0.0363(15) 0.0376(15) 0.0321(13) 0.0056(12) 0.0000(12) 0.0056(13)
I1 0.06900(16) 0.03950(12) 0.04922(12) 0.00080(9) -0.00762(11) 0.01907(10)
O1M 0.113(3) 0.0664(19) 0.0464(14) 0.0036(13) -0.0045(16) -0.0217(18)
C1M 0.115(4) 0.073(3) 0.068(3) 0.011(2) -0.011(3) -0.034(3)
O1W 0.0497(14) 0.0605(17) 0.0701(17) 0.0048(14) 0.0015(13) 0.0107(13)

_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 C43 1.523(4) . ?
C1 C11 1.525(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C11 C16 1.387(4) . ?
C11 C12 1.393(4) . ?
C12 O12 1.378(4) . ?
C12 C13 1.406(4) . ?
C13 C14 1.395(4) . ?
C13 C2 1.518(4) . ?
C14 C15 1.388(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.401(5) . ?
C15 C17 1.533(5) . ?
C16 H16 0.9500 . ?
C17 C173 1.527(6) . ?
C17 C171 1.530(5) . ?
C17 C172 1.557(6) . ?
C171 H17A 0.9800 . ?
C171 H17B 0.9800 . ?
C171 H17C 0.9800 . ?
C172 H17D 0.9800 . ?
C172 H17E 0.9800 . ?
C172 H17F 0.9800 . ?
C173 H17G 0.9800 . ?
C173 H17H 0.9800 . ?
C173 H17I 0.9800 . ?
O12 C121 1.446(4) . ?
C121 C122 1.525(5) . ?
C121 H12A 0.9900 . ?
C121 H12B 0.9900 . ?
C122 C123 1.525(5) . ?
C122 H12C 0.9900 . ?
C122 H12D 0.9900 . ?
C123 N124 1.464(4) . ?
C123 H12E 0.9900 . ?
C123 H12F 0.9900 . ?
N124 C125 1.336(4) . ?
N124 H124 0.8800 . ?
C125 O125 1.244(4) . ?
C125 C51 1.494(4) . ?
C2 C21 1.521(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C21 C22 1.395(4) . ?
C21 C26 1.402(5) . ?
C22 C23 1.396(4) . ?
C22 O22 1.401(4) . ?
C23 C24 1.395(4) . ?
C23 C3 1.522(4) . ?
C24 C25 1.383(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.398(5) . ?
C25 C27 1.547(5) . ?
C26 H26 0.9500 . ?
O22 C221 1.441(4) . ?
C221 C222 1.499(5) . ?
C221 H22A 0.9900 . ?
C221 H22B 0.9900 . ?
C222 C223 1.543(5) . ?
C222 H22C 0.9900 . ?
C222 H22D 0.9900 . ?
C223 H22E 0.9800 . ?
C223 H22F 0.9800 . ?
C223 H22G 0.9800 . ?
C27 C271 1.397(9) . ?
C27 C272 1.483(7) . ?
C27 C273 1.526(9) . ?
C271 H27A 0.9800 . ?
C271 H27B 0.9800 . ?
C271 H27C 0.9800 . ?
C272 H27D 0.9800 . ?
C272 H27E 0.9800 . ?
C272 H27F 0.9800 . ?
C273 H27G 0.9800 . ?
C273 H27H 0.9800 . ?
C273 H27I 0.9800 . ?
C3 C31 1.521(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C31 C32 1.394(4) . ?
C31 C36 1.404(4) . ?
C32 C33 1.392(4) . ?
C32 O32 1.397(3) . ?
C33 C34 1.395(4) . ?
C33 C4 1.524(4) . ?
C34 C35 1.399(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.394(4) . ?
C35 C37 1.546(4) . ?
C36 H36 0.9500 . ?
C37 C372 1.511(6) . ?
C37 C371 1.527(6) . ?
C37 C373 1.528(7) . ?
C371 H37A 0.9800 . ?
C371 H37B 0.9800 . ?
C371 H37C 0.9800 . ?
C372 H37D 0.9800 . ?
C372 H37E 0.9800 . ?
C372 H37F 0.9800 . ?
C373 H37G 0.9800 . ?
C373 H37H 0.9800 . ?
C373 H37I 0.9800 . ?
O32 C321 1.430(4) . ?
C321 C322 1.523(5) . ?
C321 H32A 0.9900 . ?
C321 H32B 0.9900 . ?
C322 C323 1.515(5) . ?
C322 H32C 0.9900 . ?
C322 H32D 0.9900 . ?
C323 N324 1.465(4) . ?
C323 H32E 0.9900 . ?
C323 H32F 0.9900 . ?
N324 C325 1.334(4) . ?
N324 H324 0.8800 . ?
C325 O325 1.223(4) . ?
C325 C53 1.515(4) . ?
C4 C41 1.519(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C41 C46 1.383(4) . ?
C41 C42 1.404(4) . ?
C42 O42 1.391(4) . ?
C42 C43 1.393(4) . ?
C43 C44 1.373(4) . ?
C44 C45 1.404(4) . ?
C44 H44 0.9500 . ?
C45 C46 1.393(5) . ?
C45 C47 1.534(4) . ?
C46 H46 0.9500 . ?
C47 C471 1.522(6) . ?
C47 C473 1.528(6) . ?
C47 C472 1.543(7) . ?
C471 H47A 0.9800 . ?
C471 H47B 0.9800 . ?
C471 H47C 0.9800 . ?
C472 H47D 0.9800 . ?
C472 H47E 0.9800 . ?
C472 H47F 0.9800 . ?
C473 H47G 0.9800 . ?
C473 H47H 0.9800 . ?
C473 H47I 0.9800 . ?
O42 C421 1.439(3) . ?
C421 C422 1.514(5) . ?
C421 H42A 0.9900 . ?
C421 H42B 0.9900 . ?
C422 C423 1.502(6) . ?
C422 H42C 0.9900 . ?
C422 H42D 0.9900 . ?
C423 H42E 0.9800 . ?
C423 H42F 0.9800 . ?
C423 H42G 0.9800 . ?
C51 C56 1.386(4) . ?
C51 C52 1.396(4) . ?
C52 C53 1.389(4) . ?
C52 H52 0.9500 . ?
C53 C54 1.385(4) . ?
C54 C55 1.389(4) . ?
C54 H54 0.9500 . ?
C55 C56 1.395(5) . ?
C55 I1 2.109(3) . ?
C56 H56 0.9500 . ?
O1M C1M 1.408(6) . ?
O1M H1M 0.8513 . ?
C1M H1M1 0.9800 . ?
C1M H1M2 0.9800 . ?
C1M H1M3 0.9800 . ?
O1W H1WA 0.8513 . ?
O1W H1WB 0.8537 . ?

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
C43 C1 C11 109.4(2) . . ?
C43 C1 H1A 109.8 . . ?
C11 C1 H1A 109.8 . . ?
C43 C1 H1B 109.8 . . ?
C11 C1 H1B 109.8 . . ?
H1A C1 H1B 108.2 . . ?
C16 C11 C12 118.7(3) . . ?
C16 C11 C1 119.7(3) . . ?
C12 C11 C1 121.2(3) . . ?
O12 C12 C11 120.8(3) . . ?
O12 C12 C13 118.5(3) . . ?
C11 C12 C13 120.5(3) . . ?
C14 C13 C12 118.4(3) . . ?
C14 C13 C2 121.7(3) . . ?
C12 C13 C2 119.8(3) . . ?
C15 C14 C13 122.4(3) . . ?
C15 C14 H14 118.8 . . ?
C13 C14 H14 118.8 . . ?
C14 C15 C16 117.1(3) . . ?
C14 C15 C17 121.8(3) . . ?
C16 C15 C17 121.0(3) . . ?
C11 C16 C15 122.5(3) . . ?
C11 C16 H16 118.8 . . ?
C15 C16 H16 118.8 . . ?
C173 C17 C171 109.4(4) . . ?
C173 C17 C15 111.2(3) . . ?
C171 C17 C15 112.9(3) . . ?
C173 C17 C172 108.2(4) . . ?
C171 C17 C172 106.8(4) . . ?
C15 C17 C172 108.1(3) . . ?
C17 C171 H17A 109.5 . . ?
C17 C171 H17B 109.5 . . ?
H17A C171 H17B 109.5 . . ?
C17 C171 H17C 109.5 . . ?
H17A C171 H17C 109.5 . . ?
H17B C171 H17C 109.5 . . ?
C17 C172 H17D 109.5 . . ?
C17 C172 H17E 109.5 . . ?
H17D C172 H17E 109.5 . . ?
C17 C172 H17F 109.5 . . ?
H17D C172 H17F 109.5 . . ?
H17E C172 H17F 109.5 . . ?
C17 C173 H17G 109.5 . . ?
C17 C173 H17H 109.5 . . ?
H17G C173 H17H 109.5 . . ?
C17 C173 H17I 109.5 . . ?
H17G C173 H17I 109.5 . . ?
H17H C173 H17I 109.5 . . ?
C12 O12 C121 113.9(2) . . ?
O12 C121 C122 111.9(3) . . ?
O12 C121 H12A 109.2 . . ?
C122 C121 H12A 109.2 . . ?
O12 C121 H12B 109.2 . . ?
C122 C121 H12B 109.2 . . ?
H12A C121 H12B 107.9 . . ?
C123 C122 C121 112.1(3) . . ?
C123 C122 H12C 109.2 . . ?
C121 C122 H12C 109.2 . . ?
C123 C122 H12D 109.2 . . ?
C121 C122 H12D 109.2 . . ?
H12C C122 H12D 107.9 . . ?
N124 C123 C122 109.3(3) . . ?
N124 C123 H12E 109.8 . . ?
C122 C123 H12E 109.8 . . ?
N124 C123 H12F 109.8 . . ?
C122 C123 H12F 109.8 . . ?
H12E C123 H12F 108.3 . . ?
C125 N124 C123 124.1(3) . . ?
C125 N124 H124 118.0 . . ?
C123 N124 H124 118.0 . . ?
O125 C125 N124 123.5(3) . . ?
O125 C125 C51 121.0(3) . . ?
N124 C125 C51 115.5(3) . . ?
C21 C2 C13 110.5(2) . . ?
C21 C2 H2A 109.5 . . ?
C13 C2 H2A 109.5 . . ?
C21 C2 H2B 109.5 . . ?
C13 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
C22 C21 C26 117.9(3) . . ?
C22 C21 C2 123.3(3) . . ?
C26 C21 C2 118.7(3) . . ?
C23 C22 C21 121.2(3) . . ?
C23 C22 O22 119.8(3) . . ?
C21 C22 O22 118.9(3) . . ?
C24 C23 C22 118.2(3) . . ?
C24 C23 C3 118.1(3) . . ?
C22 C23 C3 123.4(3) . . ?
C25 C24 C23 123.0(3) . . ?
C25 C24 H24 118.5 . . ?
C23 C24 H24 118.5 . . ?
C24 C25 C26 116.8(3) . . ?
C24 C25 C27 122.0(3) . . ?
C26 C25 C27 120.9(3) . . ?
C25 C26 C21 122.7(3) . . ?
C25 C26 H26 118.7 . . ?
C21 C26 H26 118.7 . . ?
C22 O22 C221 113.6(2) . . ?
O22 C221 C222 113.6(3) . . ?
O22 C221 H22A 108.8 . . ?
C222 C221 H22A 108.8 . . ?
O22 C221 H22B 108.8 . . ?
C222 C221 H22B 108.8 . . ?
H22A C221 H22B 107.7 . . ?
C221 C222 C223 110.7(4) . . ?
C221 C222 H22C 109.5 . . ?
C223 C222 H22C 109.5 . . ?
C221 C222 H22D 109.5 . . ?
C223 C222 H22D 109.5 . . ?
H22C C222 H22D 108.1 . . ?
C222 C223 H22E 109.5 . . ?
C222 C223 H22F 109.5 . . ?
H22E C223 H22F 109.5 . . ?
C222 C223 H22G 109.5 . . ?
H22E C223 H22G 109.5 . . ?
H22F C223 H22G 109.5 . . ?
C271 C27 C272 114.6(9) . . ?
C271 C27 C273 109.1(9) . . ?
C272 C27 C273 102.1(6) . . ?
C271 C27 C25 109.4(4) . . ?
C272 C27 C25 110.5(3) . . ?
C273 C27 C25 110.8(4) . . ?
C27 C271 H27A 109.5 . . ?
C27 C271 H27B 109.5 . . ?
H27A C271 H27B 109.5 . . ?
C27 C271 H27C 109.5 . . ?
H27A C271 H27C 109.5 . . ?
H27B C271 H27C 109.5 . . ?
C27 C272 H27D 109.5 . . ?
C27 C272 H27E 109.5 . . ?
H27D C272 H27E 109.5 . . ?
C27 C272 H27F 109.5 . . ?
H27D C272 H27F 109.5 . . ?
H27E C272 H27F 109.5 . . ?
C27 C273 H27G 109.5 . . ?
C27 C273 H27H 109.5 . . ?
H27G C273 H27H 109.5 . . ?
C27 C273 H27I 109.5 . . ?
H27G C273 H27I 109.5 . . ?
H27H C273 H27I 109.5 . . ?
C31 C3 C23 109.1(2) . . ?
C31 C3 H3A 109.9 . . ?
C23 C3 H3A 109.9 . . ?
C31 C3 H3B 109.9 . . ?
C23 C3 H3B 109.9 . . ?
H3A C3 H3B 108.3 . . ?
C32 C31 C36 118.2(3) . . ?
C32 C31 C3 120.2(2) . . ?
C36 C31 C3 121.1(3) . . ?
C31 C32 C33 122.2(3) . . ?
C31 C32 O32 117.7(2) . . ?
C33 C32 O32 119.9(2) . . ?
C32 C33 C34 117.6(3) . . ?
C32 C33 C4 122.9(3) . . ?
C34 C33 C4 119.3(3) . . ?
C35 C34 C33 122.5(3) . . ?
C35 C34 H34 118.8 . . ?
C33 C34 H34 118.8 . . ?
C36 C35 C34 117.9(3) . . ?
C36 C35 C37 122.4(3) . . ?
C34 C35 C37 119.5(3) . . ?
C35 C36 C31 121.5(3) . . ?
C35 C36 H36 119.3 . . ?
C31 C36 H36 119.3 . . ?
C372 C37 C371 108.8(4) . . ?
C372 C37 C373 107.9(4) . . ?
C371 C37 C373 111.1(5) . . ?
C372 C37 C35 112.3(3) . . ?
C371 C37 C35 109.6(3) . . ?
C373 C37 C35 107.1(3) . . ?
C37 C371 H37A 109.5 . . ?
C37 C371 H37B 109.5 . . ?
H37A C371 H37B 109.5 . . ?
C37 C371 H37C 109.5 . . ?
H37A C371 H37C 109.5 . . ?
H37B C371 H37C 109.5 . . ?
C37 C372 H37D 109.5 . . ?
C37 C372 H37E 109.5 . . ?
H37D C372 H37E 109.5 . . ?
C37 C372 H37F 109.5 . . ?
H37D C372 H37F 109.5 . . ?
H37E C372 H37F 109.5 . . ?
C37 C373 H37G 109.5 . . ?
C37 C373 H37H 109.5 . . ?
H37G C373 H37H 109.5 . . ?
C37 C373 H37I 109.5 . . ?
H37G C373 H37I 109.5 . . ?
H37H C373 H37I 109.5 . . ?
C32 O32 C321 114.0(2) . . ?
O32 C321 C322 113.6(3) . . ?
O32 C321 H32A 108.8 . . ?
C322 C321 H32A 108.8 . . ?
O32 C321 H32B 108.8 . . ?
C322 C321 H32B 108.8 . . ?
H32A C321 H32B 107.7 . . ?
C323 C322 C321 110.9(3) . . ?
C323 C322 H32C 109.5 . . ?
C321 C322 H32C 109.5 . . ?
C323 C322 H32D 109.5 . . ?
C321 C322 H32D 109.5 . . ?
H32C C322 H32D 108.0 . . ?
N324 C323 C322 109.1(3) . . ?
N324 C323 H32E 109.9 . . ?
C322 C323 H32E 109.9 . . ?
N324 C323 H32F 109.9 . . ?
C322 C323 H32F 109.9 . . ?
H32E C323 H32F 108.3 . . ?
C325 N324 C323 122.0(3) . . ?
C325 N324 H324 119.0 . . ?
C323 N324 H324 119.0 . . ?
O325 C325 N324 123.5(3) . . ?
O325 C325 C53 120.9(3) . . ?
N324 C325 C53 115.6(3) . . ?
C41 C4 C33 111.3(2) . . ?
C41 C4 H4A 109.4 . . ?
C33 C4 H4A 109.4 . . ?
C41 C4 H4B 109.4 . . ?
C33 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
C46 C41 C42 118.5(3) . . ?
C46 C41 C4 119.8(3) . . ?
C42 C41 C4 121.7(3) . . ?
O42 C42 C43 119.9(2) . . ?
O42 C42 C41 120.0(3) . . ?
C43 C42 C41 120.1(3) . . ?
C44 C43 C42 119.2(3) . . ?
C44 C43 C1 119.1(3) . . ?
C42 C43 C1 121.8(3) . . ?
C43 C44 C45 122.8(3) . . ?
C43 C44 H44 118.6 . . ?
C45 C44 H44 118.6 . . ?
C46 C45 C44 116.2(3) . . ?
C46 C45 C47 123.4(3) . . ?
C44 C45 C47 120.0(3) . . ?
C41 C46 C45 123.0(3) . . ?
C41 C46 H46 118.5 . . ?
C45 C46 H46 118.5 . . ?
C471 C47 C473 108.4(4) . . ?
C471 C47 C45 112.0(3) . . ?
C473 C47 C45 111.3(3) . . ?
C471 C47 C472 107.6(4) . . ?
C473 C47 C472 110.8(5) . . ?
C45 C47 C472 106.7(3) . . ?
C47 C471 H47A 109.5 . . ?
C47 C471 H47B 109.5 . . ?
H47A C471 H47B 109.5 . . ?
C47 C471 H47C 109.5 . . ?
H47A C471 H47C 109.5 . . ?
H47B C471 H47C 109.5 . . ?
C47 C472 H47D 109.5 . . ?
C47 C472 H47E 109.5 . . ?
H47D C472 H47E 109.5 . . ?
C47 C472 H47F 109.5 . . ?
H47D C472 H47F 109.5 . . ?
H47E C472 H47F 109.5 . . ?
C47 C473 H47G 109.5 . . ?
C47 C473 H47H 109.5 . . ?
H47G C473 H47H 109.5 . . ?
C47 C473 H47I 109.5 . . ?
H47G C473 H47I 109.5 . . ?
H47H C473 H47I 109.5 . . ?
C42 O42 C421 110.8(2) . . ?
O42 C421 C422 109.1(3) . . ?
O42 C421 H42A 109.9 . . ?
C422 C421 H42A 109.9 . . ?
O42 C421 H42B 109.9 . . ?
C422 C421 H42B 109.9 . . ?
H42A C421 H42B 108.3 . . ?
C423 C422 C421 114.2(3) . . ?
C423 C422 H42C 108.7 . . ?
C421 C422 H42C 108.7 . . ?
C423 C422 H42D 108.7 . . ?
C421 C422 H42D 108.7 . . ?
H42C C422 H42D 107.6 . . ?
C422 C423 H42E 109.5 . . ?
C422 C423 H42F 109.5 . . ?
H42E C423 H42F 109.5 . . ?
C422 C423 H42G 109.5 . . ?
H42E C423 H42G 109.5 . . ?
H42F C423 H42G 109.5 . . ?
C56 C51 C52 120.0(3) . . ?
C56 C51 C125 119.7(3) . . ?
C52 C51 C125 120.3(3) . . ?
C53 C52 C51 120.5(3) . . ?
C53 C52 H52 119.8 . . ?
C51 C52 H52 119.8 . . ?
C54 C53 C52 120.1(3) . . ?
C54 C53 C325 119.0(3) . . ?
C52 C53 C325 120.8(3) . . ?
C53 C54 C55 118.8(3) . . ?
C53 C54 H54 120.6 . . ?
C55 C54 H54 120.6 . . ?
C54 C55 C56 121.9(3) . . ?
C54 C55 I1 118.9(2) . . ?
C56 C55 I1 119.2(2) . . ?
C51 C56 C55 118.6(3) . . ?
C51 C56 H56 120.7 . . ?
C55 C56 H56 120.7 . . ?
C1M O1M H1M 108.3 . . ?
O1M C1M H1M1 109.5 . . ?
O1M C1M H1M2 109.5 . . ?
H1M1 C1M H1M2 109.5 . . ?
O1M C1M H1M3 109.5 . . ?
H1M1 C1M H1M3 109.5 . . ?
H1M2 C1M H1M3 109.5 . . ?
H1WA O1W H1WB 108.8 . . ?

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
C43 C1 C11 C16 97.6(3) . . . . ?
C43 C1 C11 C12 -75.8(3) . . . . ?
C16 C11 C12 O12 178.6(2) . . . . ?
C1 C11 C12 O12 -7.9(4) . . . . ?
C16 C11 C12 C13 -6.5(4) . . . . ?
C1 C11 C12 C13 167.0(3) . . . . ?
O12 C12 C13 C14 -178.5(2) . . . . ?
C11 C12 C13 C14 6.5(4) . . . . ?
O12 C12 C13 C2 5.5(4) . . . . ?
C11 C12 C13 C2 -169.4(2) . . . . ?
C12 C13 C14 C15 -2.4(4) . . . . ?
C2 C13 C14 C15 173.5(3) . . . . ?
C13 C14 C15 C16 -1.6(4) . . . . ?
C13 C14 C15 C17 175.2(3) . . . . ?
C12 C11 C16 C15 2.4(4) . . . . ?
C1 C11 C16 C15 -171.2(3) . . . . ?
C14 C15 C16 C11 1.6(4) . . . . ?
C17 C15 C16 C11 -175.2(3) . . . . ?
C14 C15 C17 C173 35.3(5) . . . . ?
C16 C15 C17 C173 -148.0(4) . . . . ?
C14 C15 C17 C171 158.8(3) . . . . ?
C16 C15 C17 C171 -24.6(5) . . . . ?
C14 C15 C17 C172 -83.3(4) . . . . ?
C16 C15 C17 C172 93.4(4) . . . . ?
C11 C12 O12 C121 -75.2(3) . . . . ?
C13 C12 O12 C121 109.9(3) . . . . ?
C12 O12 C121 C122 -72.6(3) . . . . ?
O12 C121 C122 C123 -177.5(3) . . . . ?
C121 C122 C123 N124 66.7(4) . . . . ?
C122 C123 N124 C125 -164.6(3) . . . . ?
C123 N124 C125 O125 -5.6(5) . . . . ?
C123 N124 C125 C51 173.5(3) . . . . ?
C14 C13 C2 C21 -98.9(3) . . . . ?
C12 C13 C2 C21 76.9(3) . . . . ?
C13 C2 C21 C22 -118.9(3) . . . . ?
C13 C2 C21 C26 57.1(3) . . . . ?
C26 C21 C22 C23 -3.2(4) . . . . ?
C2 C21 C22 C23 172.8(3) . . . . ?
C26 C21 C22 O22 178.8(2) . . . . ?
C2 C21 C22 O22 -5.2(4) . . . . ?
C21 C22 C23 C24 4.1(4) . . . . ?
O22 C22 C23 C24 -177.9(2) . . . . ?
C21 C22 C23 C3 -170.2(3) . . . . ?
O22 C22 C23 C3 7.8(4) . . . . ?
C22 C23 C24 C25 -0.9(5) . . . . ?
C3 C23 C24 C25 173.7(3) . . . . ?
C23 C24 C25 C26 -2.9(5) . . . . ?
C23 C24 C25 C27 -175.9(3) . . . . ?
C24 C25 C26 C21 3.8(5) . . . . ?
C27 C25 C26 C21 176.9(3) . . . . ?
C22 C21 C26 C25 -0.8(5) . . . . ?
C2 C21 C26 C25 -177.0(3) . . . . ?
C23 C22 O22 C221 80.3(3) . . . . ?
C21 C22 O22 C221 -101.7(3) . . . . ?
C22 O22 C221 C222 80.5(3) . . . . ?
O22 C221 C222 C223 176.4(3) . . . . ?
C24 C25 C27 C271 96.1(10) . . . . ?
C26 C25 C27 C271 -76.6(10) . . . . ?
C24 C25 C27 C272 -136.8(5) . . . . ?
C26 C25 C27 C272 50.5(6) . . . . ?
C24 C25 C27 C273 -24.3(7) . . . . ?
C26 C25 C27 C273 163.0(6) . . . . ?
C24 C23 C3 C31 -58.1(3) . . . . ?
C22 C23 C3 C31 116.2(3) . . . . ?
C23 C3 C31 C32 -73.1(3) . . . . ?
C23 C3 C31 C36 99.3(3) . . . . ?
C36 C31 C32 C33 -3.5(4) . . . . ?
C3 C31 C32 C33 169.1(3) . . . . ?
C36 C31 C32 O32 -178.9(3) . . . . ?
C3 C31 C32 O32 -6.3(4) . . . . ?
C31 C32 C33 C34 3.5(4) . . . . ?
O32 C32 C33 C34 178.8(3) . . . . ?
C31 C32 C33 C4 -170.4(3) . . . . ?
O32 C32 C33 C4 4.8(4) . . . . ?
C32 C33 C34 C35 -1.4(5) . . . . ?
C4 C33 C34 C35 172.8(3) . . . . ?
C33 C34 C35 C36 -0.6(5) . . . . ?
C33 C34 C35 C37 -175.9(3) . . . . ?
C34 C35 C36 C31 0.6(4) . . . . ?
C37 C35 C36 C31 175.8(3) . . . . ?
C32 C31 C36 C35 1.4(4) . . . . ?
C3 C31 C36 C35 -171.1(3) . . . . ?
C36 C35 C37 C372 9.2(5) . . . . ?
C34 C35 C37 C372 -175.6(4) . . . . ?
C36 C35 C37 C371 130.4(4) . . . . ?
C34 C35 C37 C371 -54.5(5) . . . . ?
C36 C35 C37 C373 -109.0(4) . . . . ?
C34 C35 C37 C373 66.1(5) . . . . ?
C31 C32 O32 C321 -108.2(3) . . . . ?
C33 C32 O32 C321 76.3(3) . . . . ?
C32 O32 C321 C322 68.8(3) . . . . ?
O32 C321 C322 C323 -180.0(3) . . . . ?
C321 C322 C323 N324 -66.3(4) . . . . ?
C322 C323 N324 C325 166.1(3) . . . . ?
C323 N324 C325 O325 3.7(5) . . . . ?
C323 N324 C325 C53 -177.6(3) . . . . ?
C32 C33 C4 C41 74.4(4) . . . . ?
C34 C33 C4 C41 -99.4(3) . . . . ?
C33 C4 C41 C46 69.1(3) . . . . ?
C33 C4 C41 C42 -111.9(3) . . . . ?
C46 C41 C42 O42 174.1(2) . . . . ?
C4 C41 C42 O42 -4.9(4) . . . . ?
C46 C41 C42 C43 -4.9(4) . . . . ?
C4 C41 C42 C43 176.1(3) . . . . ?
O42 C42 C43 C44 -173.5(3) . . . . ?
C41 C42 C43 C44 5.4(4) . . . . ?
O42 C42 C43 C1 6.5(4) . . . . ?
C41 C42 C43 C1 -174.5(3) . . . . ?
C11 C1 C43 C44 -68.5(4) . . . . ?
C11 C1 C43 C42 111.5(3) . . . . ?
C42 C43 C44 C45 -2.0(5) . . . . ?
C1 C43 C44 C45 177.9(3) . . . . ?
C43 C44 C45 C46 -1.8(5) . . . . ?
C43 C44 C45 C47 170.8(3) . . . . ?
C42 C41 C46 C45 0.9(5) . . . . ?
C4 C41 C46 C45 180.0(3) . . . . ?
C44 C45 C46 C41 2.4(5) . . . . ?
C47 C45 C46 C41 -169.9(3) . . . . ?
C46 C45 C47 C471 -149.0(3) . . . . ?
C44 C45 C47 C471 39.0(5) . . . . ?
C46 C45 C47 C473 -27.4(6) . . . . ?
C44 C45 C47 C473 160.5(5) . . . . ?
C46 C45 C47 C472 93.5(4) . . . . ?
C44 C45 C47 C472 -78.5(4) . . . . ?
C43 C42 O42 C421 82.9(3) . . . . ?
C41 C42 O42 C421 -96.1(3) . . . . ?
C42 O42 C421 C422 -169.1(3) . . . . ?
O42 C421 C422 C423 -72.0(4) . . . . ?
O125 C125 C51 C56 -26.7(5) . . . . ?
N124 C125 C51 C56 154.2(3) . . . . ?
O125 C125 C51 C52 151.4(3) . . . . ?
N124 C125 C51 C52 -27.7(4) . . . . ?
C56 C51 C52 C53 -2.5(5) . . . . ?
C125 C51 C52 C53 179.4(3) . . . . ?
C51 C52 C53 C54 3.0(5) . . . . ?
C51 C52 C53 C325 -179.0(3) . . . . ?
O325 C325 C53 C54 27.6(5) . . . . ?
N324 C325 C53 C54 -151.2(3) . . . . ?
O325 C325 C53 C52 -150.4(3) . . . . ?
N324 C325 C53 C52 30.8(4) . . . . ?
C52 C53 C54 C55 -2.0(5) . . . . ?
C325 C53 C54 C55 180.0(3) . . . . ?
C53 C54 C55 C56 0.6(5) . . . . ?
C53 C54 C55 I1 -179.6(2) . . . . ?
C52 C51 C56 C55 1.1(5) . . . . ?
C125 C51 C56 C55 179.2(3) . . . . ?
C54 C55 C56 C51 -0.1(5) . . . . ?
I1 C55 C56 C51 -179.9(2) . . . . ?

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
N124 H124 O1W 0.88 2.19 3.062(4) 168.6 .
N324 H324 O1W 0.88 2.19 3.063(4) 169.8 .
O1M H1M O125 0.85 1.82 2.676(4) 179.7 .
O1W H1WA O1M 0.85 1.98 2.698(5) 141.9 4_566
O1W H1WB O22 0.85 2.33 2.911(3) 126.0 .

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.929
_refine_diff_density_min         -0.740
_refine_diff_density_rms         0.061

data_boeh63
_database_code_depnum_ccdc_archive 'CCDC 706487'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C56 H65 I N6 O17'
_chemical_formula_weight         1221.04

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'
I I -0.4742 1.8119 '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           Monoclinic
_symmetry_space_group_name_H-M   'P 21/n'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   13.2687(5)
_cell_length_b                   13.5843(4)
_cell_length_c                   31.5174(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.788(3)
_cell_angle_gamma                90.00
_cell_volume                     5661.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    55356
_cell_measurement_theta_min      2.2
_cell_measurement_theta_max      25.8

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2528
_exptl_absorpt_coefficient_mu    0.642
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8878
_exptl_absorpt_correction_T_max  0.9327
_exptl_absorpt_process_details   'MULABS (Spek, 2003; Blessing, 1995)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            58800
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         2.15
_diffrn_reflns_theta_max         25.44
_reflns_number_total             10402
_reflns_number_gt                8887
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990) '
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997) '
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 1991)'
_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^)+(0.0557P)^2^+3.0722P] 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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10402
_refine_ls_number_parameters     812
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0352
_refine_ls_wR_factor_ref         0.0952
_refine_ls_wR_factor_gt          0.0918
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.002
_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
I1 I 0.826801(14) 0.124854(13) 0.586234(6) 0.04052(7) Uani 1 1 d . . .
C1 C 0.32920(17) 0.78126(16) 0.52226(7) 0.0267(5) Uani 1 1 d . . .
H1A H 0.3703 0.7218 0.5294 0.032 Uiso 1 1 calc R . .
H1B H 0.3204 0.7875 0.4909 0.032 Uiso 1 1 calc R . .
C11 C 0.38288(17) 0.87161(16) 0.54132(7) 0.0258(5) Uani 1 1 d . . .
C12 C 0.42849(16) 0.86973(15) 0.58314(7) 0.0248(4) Uani 1 1 d . . .
C13 C 0.45518(17) 0.95598(17) 0.60571(8) 0.0273(5) Uani 1 1 d . . .
C14 C 0.44859(17) 1.04543(16) 0.58355(8) 0.0302(5) Uani 1 1 d . . .
H14 H 0.4679 1.1053 0.5975 0.036 Uiso 1 1 calc R . .
C15 C 0.41364(18) 1.04523(17) 0.54114(8) 0.0308(5) Uani 1 1 d . . .
C16 C 0.37755(18) 0.96148(17) 0.51969(8) 0.0296(5) Uani 1 1 d . . .
H16 H 0.3498 0.9652 0.4910 0.035 Uiso 1 1 calc R . .
O12 O 0.44079(12) 0.78077(11) 0.60407(5) 0.0267(3) Uani 1 1 d . . .
C121 C 0.52683(17) 0.72504(16) 0.59129(8) 0.0283(5) Uani 1 1 d . . .
H12A H 0.5284 0.7292 0.5600 0.034 Uiso 1 1 calc R . .
H12B H 0.5185 0.6549 0.5988 0.034 Uiso 1 1 calc R . .
C122 C 0.62692(17) 0.76269(17) 0.61248(8) 0.0299(5) Uani 1 1 d . . .
H12C H 0.6247 0.7601 0.6438 0.036 Uiso 1 1 calc R . .
H12D H 0.6360 0.8323 0.6043 0.036 Uiso 1 1 calc R . .
C123 C 0.71741(19) 0.70276(18) 0.60001(8) 0.0329(5) Uani 1 1 d . . .
H12E H 0.7228 0.7081 0.5690 0.039 Uiso 1 1 calc R . .
H12F H 0.7805 0.7289 0.6149 0.039 Uiso 1 1 calc R . .
N124 N 0.70417(17) 0.60007(15) 0.61166(7) 0.0319(4) Uani 1 1 d . . .
H124 H 0.667(2) 0.590(2) 0.6309(10) 0.033(7) Uiso 1 1 d . . .
C125 C 0.75311(17) 0.52552(18) 0.59411(7) 0.0290(5) Uani 1 1 d . . .
O125 O 0.82083(13) 0.53944(14) 0.57030(6) 0.0385(4) Uani 1 1 d . . .
N15 N 0.41032(18) 1.13909(15) 0.51738(8) 0.0412(5) Uani 1 1 d . . .
O151 O 0.36358(18) 1.14157(15) 0.48230(8) 0.0550(6) Uani 1 1 d . . .
O152 O 0.4565(2) 1.20952(14) 0.53373(8) 0.0609(6) Uani 1 1 d . . .
C2 C 0.48036(18) 0.95191(18) 0.65358(8) 0.0310(5) Uani 1 1 d . . .
H2A H 0.5075 1.0162 0.6640 0.037 Uiso 1 1 calc R . .
H2B H 0.5323 0.9009 0.6607 0.037 Uiso 1 1 calc R . .
C21 C 0.38426(18) 0.92751(17) 0.67475(7) 0.0279(5) Uani 1 1 d . . .
C22 C 0.36979(17) 0.83995(17) 0.69699(7) 0.0265(5) Uani 1 1 d . A .
C23 C 0.27488(18) 0.81280(17) 0.71012(7) 0.0279(5) Uani 1 1 d . . .
C24 C 0.1947(2) 0.87813(19) 0.70173(9) 0.0384(6) Uani 1 1 d . . .
H24 H 0.1287 0.8612 0.7089 0.046 Uiso 1 1 calc R . .
C25 C 0.2121(2) 0.9676(2) 0.68296(9) 0.0419(7) Uani 1 1 d . . .
C26 C 0.3041(2) 0.99381(18) 0.66922(8) 0.0344(5) Uani 1 1 d . . .
H26 H 0.3128 1.0560 0.6562 0.041 Uiso 1 1 calc R . .
O22 O 0.45056(12) 0.77608(12) 0.70548(5) 0.0303(4) Uani 1 1 d . . .
C221 C 0.5266(5) 0.8118(5) 0.7384(2) 0.0456(19) Uani 0.536(11) 1 d P A 1
H22A H 0.5890 0.7721 0.7377 0.055 Uiso 0.536(11) 1 calc PR A 1
H22B H 0.5437 0.8810 0.7322 0.055 Uiso 0.536(11) 1 calc PR A 1
C222 C 0.4914(6) 0.8062(7) 0.7803(2) 0.076(3) Uani 0.536(11) 1 d P A 1
H22C H 0.4644 0.7402 0.7863 0.091 Uiso 0.536(11) 1 calc PR A 1
H22D H 0.4398 0.8570 0.7847 0.091 Uiso 0.536(11) 1 calc PR A 1
C223 C 0.604(3) 0.829(2) 0.8097(10) 0.159(13) Uani 0.536(11) 1 d P A 1
H22E H 0.5918 0.8324 0.8400 0.238 Uiso 0.536(11) 1 calc PR A 1
H22F H 0.6310 0.8925 0.8009 0.238 Uiso 0.536(11) 1 calc PR A 1
H22G H 0.6519 0.7767 0.8051 0.238 Uiso 0.536(11) 1 calc PR A 1
C224 C 0.4903(5) 0.7722(6) 0.7509(2) 0.0363(19) Uani 0.464(11) 1 d P A 2
H22H H 0.5255 0.7088 0.7567 0.044 Uiso 0.464(11) 1 calc PR A 2
H22I H 0.4335 0.7763 0.7693 0.044 Uiso 0.464(11) 1 calc PR A 2
C225 C 0.5616(8) 0.8548(7) 0.7609(3) 0.078(3) Uani 0.464(11) 1 d P A 2
H22J H 0.5293 0.9189 0.7533 0.093 Uiso 0.464(11) 1 calc PR A 2
H22K H 0.6232 0.8476 0.7455 0.093 Uiso 0.464(11) 1 calc PR A 2
C226 C 0.588(2) 0.8465(18) 0.8109(9) 0.085(6) Uani 0.464(11) 1 d P A 2
H22L H 0.6345 0.8995 0.8205 0.128 Uiso 0.464(11) 1 calc PR A 2
H22M H 0.6198 0.7827 0.8176 0.128 Uiso 0.464(11) 1 calc PR A 2
H22N H 0.5257 0.8521 0.8254 0.128 Uiso 0.464(11) 1 calc PR A 2
N25 N 0.1274(3) 1.0369(3) 0.67619(12) 0.0869(13) Uani 1 1 d . . .
O251 O 0.0453(3) 1.0057(4) 0.6772(3) 0.292(5) Uani 1 1 d . . .
O252 O 0.1446(2) 1.12295(18) 0.66906(9) 0.0760(8) Uani 1 1 d . . .
C3 C 0.25634(18) 0.71431(17) 0.73170(7) 0.0289(5) Uani 1 1 d . . .
H3A H 0.3149 0.6702 0.7290 0.035 Uiso 1 1 calc R . .
H3B H 0.2495 0.7252 0.7624 0.035 Uiso 1 1 calc R . .
C31 C 0.16134(17) 0.66606(17) 0.71148(7) 0.0276(5) Uani 1 1 d . . .
C32 C 0.16136(17) 0.62852(16) 0.67013(8) 0.0264(5) Uani 1 1 d . . .
C33 C 0.07246(18) 0.59999(17) 0.64579(8) 0.0281(5) Uani 1 1 d . . .
C34 C -0.01689(19) 0.60039(18) 0.66578(8) 0.0333(5) Uani 1 1 d . . .
H34 H -0.0786 0.5811 0.6506 0.040 Uiso 1 1 calc R . .
C35 C -0.01526(19) 0.62923(19) 0.70805(8) 0.0350(5) Uani 1 1 d . . .
C36 C 0.07092(18) 0.66336(18) 0.73131(8) 0.0315(5) Uani 1 1 d . . .
H36 H 0.0687 0.6844 0.7600 0.038 Uiso 1 1 calc R . .
O32 O 0.25297(12) 0.62668(11) 0.65253(5) 0.0283(3) Uani 1 1 d . . .
C321 C 0.29433(19) 0.52836(19) 0.64838(8) 0.0338(5) Uani 1 1 d . . .
H32A H 0.3589 0.5332 0.6348 0.041 Uiso 1 1 calc R . .
H32B H 0.2468 0.4890 0.6293 0.041 Uiso 1 1 calc R . .
C322 C 0.3132(2) 0.47502(19) 0.69069(8) 0.0359(6) Uani 1 1 d . . .
H32C H 0.2494 0.4710 0.7047 0.043 Uiso 1 1 calc R . .
H32D H 0.3628 0.5125 0.7096 0.043 Uiso 1 1 calc R . .
C323 C 0.3536(2) 0.37159(18) 0.68400(9) 0.0365(6) Uani 1 1 d . . .
H32E H 0.3612 0.3363 0.7116 0.044 Uiso 1 1 calc R . .
H32F H 0.3051 0.3345 0.6645 0.044 Uiso 1 1 calc R . .
N324 N 0.45118(16) 0.37702(16) 0.66599(7) 0.0315(4) Uani 1 1 d . . .
H324 H 0.479(2) 0.431(2) 0.6672(9) 0.032(7) Uiso 1 1 d . . .
C325 C 0.49622(18) 0.29666(17) 0.65169(8) 0.0308(5) Uani 1 1 d . . .
O325 O 0.45916(15) 0.21413(13) 0.65406(6) 0.0417(4) Uani 1 1 d . . .
N35 N -0.11096(18) 0.6274(2) 0.72888(8) 0.0502(6) Uani 1 1 d . . .
O351 O -0.10955(18) 0.6544(2) 0.76583(8) 0.0775(9) Uani 1 1 d . . .
O352 O -0.18758(17) 0.5999(3) 0.70806(8) 0.0810(9) Uani 1 1 d . . .
C4 C 0.07233(18) 0.58034(17) 0.59821(7) 0.0293(5) Uani 1 1 d . . .
H4A H 0.1204 0.5266 0.5932 0.035 Uiso 1 1 calc R . .
H4B H 0.0040 0.5595 0.5866 0.035 Uiso 1 1 calc R . .
C41 C 0.10295(17) 0.67357(17) 0.57578(7) 0.0271(5) Uani 1 1 d . . .
C42 C 0.19529(17) 0.68226(16) 0.55708(7) 0.0251(5) Uani 1 1 d . B .
C43 C 0.22607(17) 0.77161(16) 0.54007(7) 0.0253(4) Uani 1 1 d . . .
C44 C 0.16193(19) 0.85265(18) 0.54072(8) 0.0323(5) Uani 1 1 d . . .
H44 H 0.1808 0.9140 0.5293 0.039 Uiso 1 1 calc R . .
C45 C 0.07013(19) 0.84233(19) 0.55830(9) 0.0355(6) Uani 1 1 d . . .
C46 C 0.04002(18) 0.75523(19) 0.57567(8) 0.0332(5) Uani 1 1 d . . .
H46 H -0.0234 0.7510 0.5875 0.040 Uiso 1 1 calc R . .
O42 O 0.25963(12) 0.60253(11) 0.55763(5) 0.0268(3) Uani 1 1 d . . .
C421 C 0.2510(16) 0.5357(16) 0.5212(5) 0.052(6) Uani 0.41(2) 1 d P B 1
H42A H 0.1984 0.4861 0.5259 0.062 Uiso 0.41(2) 1 calc PR B 1
H42B H 0.2277 0.5738 0.4955 0.062 Uiso 0.41(2) 1 calc PR B 1
C422 C 0.3425(9) 0.4853(11) 0.5134(3) 0.046(3) Uani 0.41(2) 1 d P B 1
H42C H 0.3180 0.4210 0.5019 0.056 Uiso 0.41(2) 1 calc PR B 1
H42D H 0.3660 0.5211 0.4887 0.056 Uiso 0.41(2) 1 calc PR B 1
C423 C 0.4150(15) 0.4658(15) 0.5325(11) 0.114(9) Uani 0.41(2) 1 d P B 1
H42E H 0.4496 0.4136 0.5180 0.172 Uiso 0.41(2) 1 calc PR B 1
H42F H 0.3999 0.4427 0.5608 0.172 Uiso 0.41(2) 1 calc PR B 1
H42G H 0.4586 0.5240 0.5356 0.172 Uiso 0.41(2) 1 calc PR B 1
C424 C 0.2385(12) 0.5414(10) 0.5205(4) 0.042(3) Uani 0.59(2) 1 d P B 2
H42H H 0.2530 0.5774 0.4944 0.051 Uiso 0.59(2) 1 calc PR B 2
H42I H 0.1667 0.5207 0.5178 0.051 Uiso 0.59(2) 1 calc PR B 2
C425 C 0.3074(8) 0.4526(5) 0.5272(3) 0.050(2) Uani 0.59(2) 1 d P B 2
H42J H 0.2699 0.4035 0.5429 0.060 Uiso 0.59(2) 1 calc PR B 2
H42K H 0.3144 0.4244 0.4986 0.060 Uiso 0.59(2) 1 calc PR B 2
C426 C 0.4096(10) 0.4571(10) 0.5486(3) 0.084(4) Uani 0.59(2) 1 d P B 2
H42L H 0.4366 0.3902 0.5524 0.126 Uiso 0.59(2) 1 calc PR B 2
H42M H 0.4072 0.4886 0.5764 0.126 Uiso 0.59(2) 1 calc PR B 2
H42N H 0.4534 0.4953 0.5312 0.126 Uiso 0.59(2) 1 calc PR B 2
N45 N 0.00323(19) 0.92874(19) 0.55908(9) 0.0533(7) Uani 1 1 d . . .
O451 O 0.0353(2) 1.00848(18) 0.54913(13) 0.0961(11) Uani 1 1 d . . .
O452 O -0.08200(18) 0.91673(18) 0.56994(10) 0.0707(7) Uani 1 1 d . . .
C51 C 0.71763(17) 0.42350(17) 0.60411(7) 0.0279(5) Uani 1 1 d . . .
C52 C 0.62671(18) 0.40798(17) 0.62239(8) 0.0297(5) Uani 1 1 d . . .
H52 H 0.5860 0.4630 0.6284 0.036 Uiso 1 1 calc R . .
C53 C 0.59446(18) 0.31390(17) 0.63200(8) 0.0294(5) Uani 1 1 d . . .
C54 C 0.65327(19) 0.23290(18) 0.62230(8) 0.0317(5) Uani 1 1 d . . .
H54 H 0.6330 0.1681 0.6291 0.038 Uiso 1 1 calc R . .
C55 C 0.74190(19) 0.24837(18) 0.60254(8) 0.0318(5) Uani 1 1 d . . .
C56 C 0.77501(18) 0.34220(18) 0.59362(7) 0.0307(5) Uani 1 1 d . . .
H56 H 0.8362 0.3512 0.5805 0.037 Uiso 1 1 calc R . .
O1W O 0.54641(17) 0.58633(15) 0.67978(7) 0.0404(4) Uani 1 1 d . . .
H1WA H 0.568(3) 0.565(3) 0.7029(13) 0.061(11) Uiso 1 1 d . . .
H1WB H 0.513(3) 0.634(3) 0.6835(12) 0.057(11) Uiso 1 1 d . . .
O61 O 0.6103(2) 0.5018(2) 0.75526(8) 0.0805(8) Uani 1 1 d . . .
C62 C 0.6667(3) 0.5474(3) 0.79090(11) 0.0631(9) Uani 1 1 d . . .
H62A H 0.6207 0.5729 0.8115 0.076 Uiso 1 1 calc R . .
H62B H 0.7080 0.6025 0.7813 0.076 Uiso 1 1 calc R . .
C63 C 0.7321(3) 0.4687(4) 0.81038(16) 0.0950(16) Uani 1 1 d . . .
H63A H 0.7436 0.4779 0.8416 0.114 Uiso 1 1 calc R . .
H63B H 0.7983 0.4675 0.7980 0.114 Uiso 1 1 calc R . .
C64 C 0.6740(4) 0.3756(4) 0.79996(15) 0.0879(14) Uani 1 1 d . . .
H64A H 0.7200 0.3186 0.7983 0.105 Uiso 1 1 calc R . .
H64B H 0.6253 0.3619 0.8214 0.105 Uiso 1 1 calc R . .
C65 C 0.6205(3) 0.3983(3) 0.75727(13) 0.0722(11) Uani 1 1 d . . .
H65A H 0.6603 0.3743 0.7342 0.087 Uiso 1 1 calc R . .
H65B H 0.5532 0.3664 0.7543 0.087 Uiso 1 1 calc R . .
O71 O 0.0754(10) 0.3491(6) 0.5662(3) 0.069(3) Uani 0.382(18) 1 d P C 1
O71' O 0.0639(7) 0.3105(11) 0.5858(4) 0.137(6) Uani 0.618(18) 1 d P C 2
C72 C 0.0544(4) 0.2990(5) 0.53311(19) 0.1094(18) Uani 1 1 d . . .
H72A H 0.0423 0.3425 0.5080 0.131 Uiso 0.382(18) 1 calc PR C 1
H72B H -0.0071 0.2590 0.5359 0.131 Uiso 0.382(18) 1 calc PR C 1
H72C H -0.0099 0.2671 0.5224 0.131 Uiso 0.618(18) 1 calc PR C 2
H72D H 0.0610 0.3631 0.5187 0.131 Uiso 0.618(18) 1 calc PR C 2
C73 C 0.1441(5) 0.2334(4) 0.52828(18) 0.1042(17) Uani 1 1 d . C .
H73A H 0.1901 0.2633 0.5088 0.125 Uiso 1 1 calc R . .
H73B H 0.1220 0.1682 0.5169 0.125 Uiso 1 1 calc R . .
C74 C 0.1958(5) 0.2236(4) 0.57243(18) 0.1113(19) Uani 1 1 d . . .
H74A H 0.2044 0.1539 0.5812 0.134 Uiso 0.382(18) 1 calc PR C 1
H74B H 0.2622 0.2572 0.5752 0.134 Uiso 0.382(18) 1 calc PR C 1
H74C H 0.2700 0.2191 0.5712 0.134 Uiso 0.618(18) 1 calc PR C 2
H74D H 0.1723 0.1635 0.5864 0.134 Uiso 0.618(18) 1 calc PR C 2
C75 C 0.1211(13) 0.2743(11) 0.5963(3) 0.054(4) Uani 0.382(18) 1 d P C 1
H75A H 0.1540 0.3061 0.6221 0.065 Uiso 0.382(18) 1 calc PR C 1
H75B H 0.0691 0.2277 0.6048 0.065 Uiso 0.382(18) 1 calc PR C 1
C75' C 0.1690(6) 0.3145(6) 0.59715(19) 0.0536(19) Uani 0.618(18) 1 d P C 2
H75C H 0.1859 0.3072 0.6282 0.064 Uiso 0.618(18) 1 calc PR C 2
H75D H 0.2004 0.3750 0.5868 0.064 Uiso 0.618(18) 1 calc PR C 2

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
I1 0.04273(11) 0.03796(10) 0.04028(11) -0.00556(7) -0.00016(7) 0.02266(7)
C1 0.0274(11) 0.0258(11) 0.0269(11) -0.0015(9) 0.0017(9) 0.0013(9)
C11 0.0250(11) 0.0244(11) 0.0284(11) 0.0006(9) 0.0049(9) 0.0016(9)
C12 0.0218(10) 0.0222(10) 0.0310(12) 0.0015(9) 0.0049(9) 0.0008(8)
C13 0.0230(11) 0.0265(11) 0.0327(12) -0.0017(9) 0.0051(9) -0.0015(9)
C14 0.0284(12) 0.0215(11) 0.0418(14) -0.0029(10) 0.0101(10) -0.0019(9)
C15 0.0302(12) 0.0227(11) 0.0408(14) 0.0069(10) 0.0111(10) 0.0028(9)
C16 0.0273(12) 0.0314(12) 0.0303(12) 0.0035(9) 0.0047(9) 0.0037(9)
O12 0.0282(8) 0.0222(7) 0.0298(8) 0.0030(6) 0.0022(7) 0.0008(6)
C121 0.0309(12) 0.0201(10) 0.0332(12) 0.0000(9) -0.0013(10) 0.0030(9)
C122 0.0295(12) 0.0247(11) 0.0350(13) 0.0005(9) -0.0007(10) 0.0003(9)
C123 0.0318(13) 0.0290(12) 0.0379(14) 0.0033(10) 0.0026(10) 0.0002(10)
N124 0.0360(11) 0.0284(10) 0.0320(11) 0.0027(8) 0.0076(9) 0.0061(8)
C125 0.0236(11) 0.0345(12) 0.0279(12) -0.0018(9) -0.0038(9) 0.0054(9)
O125 0.0275(9) 0.0441(10) 0.0446(10) -0.0064(8) 0.0070(8) -0.0011(7)
N15 0.0462(13) 0.0271(11) 0.0525(15) 0.0080(10) 0.0167(11) 0.0038(10)
O151 0.0651(14) 0.0440(12) 0.0555(14) 0.0228(10) 0.0021(11) 0.0038(10)
O152 0.0869(17) 0.0261(10) 0.0713(15) 0.0052(10) 0.0151(13) -0.0100(10)
C2 0.0293(12) 0.0279(11) 0.0356(13) -0.0059(10) 0.0003(10) -0.0043(9)
C21 0.0333(12) 0.0262(11) 0.0237(11) -0.0072(9) -0.0002(9) -0.0011(9)
C22 0.0276(11) 0.0268(11) 0.0242(11) -0.0080(9) -0.0023(9) 0.0020(9)
C23 0.0320(12) 0.0293(12) 0.0223(11) -0.0052(9) 0.0016(9) 0.0029(9)
C24 0.0350(14) 0.0419(14) 0.0403(14) 0.0062(11) 0.0151(11) 0.0114(11)
C25 0.0441(15) 0.0387(14) 0.0451(15) 0.0087(12) 0.0169(12) 0.0218(12)
C26 0.0450(15) 0.0282(12) 0.0309(13) -0.0020(10) 0.0092(11) 0.0068(10)
O22 0.0253(8) 0.0316(8) 0.0324(9) -0.0022(7) -0.0063(7) 0.0036(7)
C221 0.041(3) 0.044(3) 0.047(4) 0.006(3) -0.022(3) -0.008(3)
C222 0.066(5) 0.115(7) 0.045(5) 0.006(4) -0.008(3) -0.034(4)
C223 0.23(3) 0.15(2) 0.081(15) 0.008(13) -0.105(19) -0.052(16)
C224 0.034(3) 0.044(4) 0.029(4) 0.003(3) -0.008(3) -0.004(3)
C225 0.086(6) 0.093(6) 0.047(5) 0.011(4) -0.033(4) -0.048(5)
C226 0.123(12) 0.064(7) 0.057(9) -0.022(6) -0.064(8) 0.042(8)
N25 0.075(2) 0.078(2) 0.117(3) 0.058(2) 0.064(2) 0.0528(18)
O251 0.082(3) 0.195(5) 0.625(14) 0.284(7) 0.182(5) 0.102(3)
O252 0.102(2) 0.0529(15) 0.0746(17) 0.0133(12) 0.0187(15) 0.0440(14)
C3 0.0278(12) 0.0308(12) 0.0282(12) -0.0017(9) 0.0019(9) 0.0032(9)
C31 0.0277(12) 0.0253(11) 0.0299(12) 0.0003(9) 0.0028(9) 0.0030(9)
C32 0.0241(11) 0.0241(11) 0.0316(12) 0.0018(9) 0.0061(9) 0.0024(9)
C33 0.0287(12) 0.0255(11) 0.0306(12) -0.0004(9) 0.0042(9) -0.0011(9)
C34 0.0289(12) 0.0346(12) 0.0365(13) -0.0017(10) 0.0035(10) -0.0042(10)
C35 0.0285(12) 0.0398(14) 0.0383(14) 0.0000(11) 0.0111(10) -0.0024(10)
C36 0.0334(13) 0.0329(12) 0.0288(12) -0.0014(10) 0.0067(10) -0.0003(10)
O32 0.0243(8) 0.0300(8) 0.0313(8) -0.0006(7) 0.0068(7) 0.0036(6)
C321 0.0317(13) 0.0371(13) 0.0333(13) 0.0015(10) 0.0079(10) 0.0121(10)
C322 0.0369(13) 0.0364(13) 0.0359(14) 0.0040(11) 0.0124(11) 0.0092(11)
C323 0.0352(13) 0.0324(13) 0.0433(14) 0.0044(11) 0.0112(11) 0.0045(10)
N324 0.0281(10) 0.0252(10) 0.0416(12) -0.0023(9) 0.0062(9) 0.0029(9)
C325 0.0329(13) 0.0284(12) 0.0303(12) -0.0030(9) -0.0024(10) 0.0059(10)
O325 0.0462(11) 0.0264(9) 0.0537(12) -0.0051(8) 0.0116(9) -0.0010(8)
N35 0.0340(13) 0.0721(18) 0.0465(14) -0.0077(12) 0.0160(11) -0.0122(12)
O351 0.0502(14) 0.134(2) 0.0516(14) -0.0325(15) 0.0274(11) -0.0287(15)
O352 0.0354(12) 0.153(3) 0.0569(15) -0.0239(16) 0.0148(11) -0.0288(15)
C4 0.0277(12) 0.0300(12) 0.0300(12) -0.0039(9) 0.0015(9) -0.0039(9)
C41 0.0259(11) 0.0300(12) 0.0249(11) -0.0027(9) -0.0017(9) 0.0001(9)
C42 0.0250(11) 0.0260(11) 0.0233(11) -0.0041(9) -0.0033(9) 0.0035(9)
C43 0.0249(11) 0.0261(11) 0.0240(11) -0.0032(9) -0.0027(9) 0.0027(9)
C44 0.0340(13) 0.0262(11) 0.0362(13) 0.0009(10) 0.0009(10) 0.0032(10)
C45 0.0319(13) 0.0301(12) 0.0443(15) -0.0028(11) 0.0022(11) 0.0125(10)
C46 0.0267(12) 0.0379(13) 0.0350(13) -0.0044(10) 0.0030(10) 0.0039(10)
O42 0.0307(8) 0.0229(8) 0.0264(8) -0.0029(6) 0.0006(6) 0.0058(6)
C421 0.053(8) 0.057(9) 0.040(8) -0.041(6) -0.033(6) 0.027(6)
C422 0.042(6) 0.056(6) 0.041(5) -0.010(4) 0.007(4) 0.017(5)
C423 0.059(10) 0.100(11) 0.19(2) -0.079(13) 0.054(14) -0.023(9)
C424 0.050(5) 0.033(5) 0.046(6) -0.006(4) 0.017(5) 0.009(4)
C425 0.070(5) 0.030(3) 0.050(4) -0.012(3) 0.008(4) 0.012(3)
C426 0.075(7) 0.119(8) 0.055(5) -0.040(4) -0.014(4) 0.070(6)
N45 0.0445(15) 0.0428(15) 0.0738(19) -0.0014(13) 0.0120(13) 0.0195(11)
O451 0.0807(19) 0.0375(13) 0.177(3) 0.0236(16) 0.053(2) 0.0282(13)
O452 0.0451(13) 0.0565(14) 0.114(2) -0.0039(14) 0.0261(13) 0.0229(11)
C51 0.0265(11) 0.0309(12) 0.0253(11) -0.0026(9) -0.0037(9) 0.0071(9)
C52 0.0298(12) 0.0268(11) 0.0321(12) -0.0055(9) 0.0001(10) 0.0095(9)
C53 0.0287(12) 0.0290(12) 0.0299(12) -0.0041(9) -0.0023(9) 0.0069(9)
C54 0.0344(13) 0.0263(11) 0.0333(13) -0.0048(9) -0.0047(10) 0.0071(10)
C55 0.0348(13) 0.0313(12) 0.0280(12) -0.0060(9) -0.0047(10) 0.0156(10)
C56 0.0288(12) 0.0369(13) 0.0257(12) -0.0033(10) -0.0017(9) 0.0119(10)
O1W 0.0505(12) 0.0339(10) 0.0373(11) -0.0039(9) 0.0059(9) 0.0068(9)
O61 0.115(2) 0.0736(17) 0.0484(14) 0.0156(12) -0.0206(14) -0.0137(16)
C62 0.0512(19) 0.087(3) 0.0518(19) -0.0042(18) 0.0070(15) -0.0143(18)
C63 0.069(3) 0.120(4) 0.090(3) -0.043(3) -0.030(2) 0.028(3)
C64 0.082(3) 0.102(4) 0.075(3) 0.026(2) -0.018(2) 0.016(3)
C65 0.078(3) 0.070(2) 0.065(2) 0.0090(19) -0.022(2) -0.001(2)
O71 0.102(8) 0.045(4) 0.061(6) 0.010(4) 0.009(5) 0.011(4)
O71' 0.093(5) 0.180(14) 0.142(11) -0.089(10) 0.032(7) -0.056(7)
C72 0.085(3) 0.129(5) 0.110(4) -0.029(4) -0.016(3) -0.026(3)
C73 0.133(5) 0.083(3) 0.101(4) -0.017(3) 0.036(3) -0.017(3)
C74 0.133(5) 0.108(4) 0.097(4) 0.013(3) 0.033(3) 0.049(4)
C75 0.053(9) 0.061(8) 0.048(5) 0.004(4) -0.006(5) 0.004(7)
C75' 0.043(4) 0.056(4) 0.063(4) -0.012(3) 0.006(3) -0.024(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
I1 C55 2.108(2) . ?
C1 C11 1.518(3) . ?
C1 C43 1.527(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C11 C16 1.397(3) . ?
C11 C12 1.404(3) . ?
C12 O12 1.380(3) . ?
C12 C13 1.401(3) . ?
C13 C14 1.401(3) . ?
C13 C2 1.519(3) . ?
C14 C15 1.378(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.388(4) . ?
C15 N15 1.478(3) . ?
C16 H16 0.9500 . ?
O12 C121 1.454(3) . ?
C121 C122 1.524(3) . ?
C121 H12A 0.9900 . ?
C121 H12B 0.9900 . ?
C122 C123 1.529(3) . ?
C122 H12C 0.9900 . ?
C122 H12D 0.9900 . ?
C123 N124 1.457(3) . ?
C123 H12E 0.9900 . ?
C123 H12F 0.9900 . ?
N124 C125 1.347(3) . ?
N124 H124 0.83(3) . ?
C125 O125 1.232(3) . ?
C125 C51 1.506(3) . ?
N15 O151 1.222(3) . ?
N15 O152 1.226(3) . ?
C2 C21 1.524(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C21 C26 1.394(3) . ?
C21 C22 1.402(3) . ?
C22 O22 1.388(3) . ?
C22 C23 1.407(3) . ?
C23 C24 1.394(3) . ?
C23 C3 1.530(3) . ?
C24 C25 1.380(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.375(4) . ?
C25 N25 1.469(4) . ?
C26 H26 0.9500 . ?
O22 C221 1.469(6) . ?
O22 C224 1.484(7) . ?
C221 C222 1.437(12) . ?
C221 H22A 0.9900 . ?
C221 H22B 0.9900 . ?
C222 C223 1.72(3) . ?
C222 H22C 0.9900 . ?
C222 H22D 0.9900 . ?
C223 H22E 0.9800 . ?
C223 H22F 0.9800 . ?
C223 H22G 0.9800 . ?
C224 C225 1.485(12) . ?
C224 H22H 0.9900 . ?
C224 H22I 0.9900 . ?
C225 C226 1.59(3) . ?
C225 H22J 0.9900 . ?
C225 H22K 0.9900 . ?
C226 H22L 0.9800 . ?
C226 H22M 0.9800 . ?
C226 H22N 0.9800 . ?
N25 O251 1.172(6) . ?
N25 O252 1.216(4) . ?
C3 C31 1.513(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C31 C36 1.399(3) . ?
C31 C32 1.399(3) . ?
C32 O32 1.378(3) . ?
C32 C33 1.407(3) . ?
C33 C34 1.388(3) . ?
C33 C4 1.523(3) . ?
C34 C35 1.387(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.386(4) . ?
C35 N35 1.478(3) . ?
C36 H36 0.9500 . ?
O32 C321 1.454(3) . ?
C321 C322 1.520(4) . ?
C321 H32A 0.9900 . ?
C321 H32B 0.9900 . ?
C322 C323 1.525(3) . ?
C322 H32C 0.9900 . ?
C322 H32D 0.9900 . ?
C323 N324 1.458(3) . ?
C323 H32E 0.9900 . ?
C323 H32F 0.9900 . ?
N324 C325 1.340(3) . ?
N324 H324 0.82(3) . ?
C325 O325 1.229(3) . ?
C325 C53 1.508(3) . ?
N35 O351 1.219(3) . ?
N35 O352 1.222(3) . ?
C4 C41 1.522(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C41 C46 1.388(3) . ?
C41 C42 1.408(3) . ?
C42 O42 1.378(3) . ?
C42 C43 1.401(3) . ?
C43 C44 1.393(3) . ?
C44 C45 1.387(4) . ?
C44 H44 0.9500 . ?
C45 C46 1.377(4) . ?
C45 N45 1.473(3) . ?
C46 H46 0.9500 . ?
O42 C424 1.443(14) . ?
O42 C421 1.460(16) . ?
C421 C422 1.43(2) . ?
C421 H42A 0.9900 . ?
C421 H42B 0.9900 . ?
C422 C423 1.12(3) . ?
C422 H42C 0.9900 . ?
C422 H42D 0.9900 . ?
C423 H42E 0.9800 . ?
C423 H42F 0.9800 . ?
C423 H42G 0.9800 . ?
C424 C425 1.517(17) . ?
C424 H42H 0.9900 . ?
C424 H42I 0.9900 . ?
C425 C426 1.464(14) . ?
C425 H42J 0.9900 . ?
C425 H42K 0.9900 . ?
C426 H42L 0.9800 . ?
C426 H42M 0.9800 . ?
C426 H42N 0.9800 . ?
N45 O451 1.215(4) . ?
N45 O452 1.220(3) . ?
C51 C52 1.396(3) . ?
C51 C56 1.397(3) . ?
C52 C53 1.389(4) . ?
C52 H52 0.9500 . ?
C53 C54 1.397(3) . ?
C54 C55 1.392(4) . ?
C54 H54 0.9500 . ?
C55 C56 1.385(4) . ?
C56 H56 0.9500 . ?
O1W H1WA 0.82(4) . ?
O1W H1WB 0.81(4) . ?
O61 C65 1.413(5) . ?
O61 C62 1.438(4) . ?
C62 C63 1.478(6) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C63 C64 1.503(7) . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C64 C65 1.500(5) . ?
C64 H64A 0.9900 . ?
C64 H64B 0.9900 . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
O71 C72 1.257(11) . ?
O71 C75 1.483(16) . ?
O71' C75' 1.412(11) . ?
O71' C72 1.663(14) . ?
C72 C73 1.505(8) . ?
C72 H72A 0.9900 . ?
C72 H72B 0.9900 . ?
C72 H72C 0.9900 . ?
C72 H72D 0.9900 . ?
C73 C74 1.505(8) . ?
C73 H73A 0.9900 . ?
C73 H73B 0.9900 . ?
C74 C75 1.465(13) . ?
C74 C75' 1.518(8) . ?
C74 H74A 0.9900 . ?
C74 H74B 0.9900 . ?
C74 H74C 0.9900 . ?
C74 H74D 0.9900 . ?
C75 H75A 0.9900 . ?
C75 H75B 0.9900 . ?
C75' H75C 0.9900 . ?
C75' H75D 0.9900 . ?

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
C11 C1 C43 109.23(18) . . ?
C11 C1 H1A 109.8 . . ?
C43 C1 H1A 109.8 . . ?
C11 C1 H1B 109.8 . . ?
C43 C1 H1B 109.8 . . ?
H1A C1 H1B 108.3 . . ?
C16 C11 C12 118.3(2) . . ?
C16 C11 C1 120.7(2) . . ?
C12 C11 C1 120.54(19) . . ?
O12 C12 C13 118.4(2) . . ?
O12 C12 C11 119.29(19) . . ?
C13 C12 C11 122.2(2) . . ?
C14 C13 C12 118.0(2) . . ?
C14 C13 C2 121.8(2) . . ?
C12 C13 C2 119.9(2) . . ?
C15 C14 C13 118.9(2) . . ?
C15 C14 H14 120.5 . . ?
C13 C14 H14 120.5 . . ?
C14 C15 C16 123.3(2) . . ?
C14 C15 N15 118.9(2) . . ?
C16 C15 N15 117.8(2) . . ?
C15 C16 C11 118.5(2) . . ?
C15 C16 H16 120.7 . . ?
C11 C16 H16 120.7 . . ?
C12 O12 C121 112.81(16) . . ?
O12 C121 C122 112.29(18) . . ?
O12 C121 H12A 109.1 . . ?
C122 C121 H12A 109.1 . . ?
O12 C121 H12B 109.1 . . ?
C122 C121 H12B 109.1 . . ?
H12A C121 H12B 107.9 . . ?
C121 C122 C123 112.5(2) . . ?
C121 C122 H12C 109.1 . . ?
C123 C122 H12C 109.1 . . ?
C121 C122 H12D 109.1 . . ?
C123 C122 H12D 109.1 . . ?
H12C C122 H12D 107.8 . . ?
N124 C123 C122 109.3(2) . . ?
N124 C123 H12E 109.8 . . ?
C122 C123 H12E 109.8 . . ?
N124 C123 H12F 109.8 . . ?
C122 C123 H12F 109.8 . . ?
H12E C123 H12F 108.3 . . ?
C125 N124 C123 123.0(2) . . ?
C125 N124 H124 121(2) . . ?
C123 N124 H124 116(2) . . ?
O125 C125 N124 122.4(2) . . ?
O125 C125 C51 121.7(2) . . ?
N124 C125 C51 115.9(2) . . ?
O151 N15 O152 123.8(2) . . ?
O151 N15 C15 118.3(2) . . ?
O152 N15 C15 117.9(3) . . ?
C13 C2 C21 108.67(19) . . ?
C13 C2 H2A 110.0 . . ?
C21 C2 H2A 110.0 . . ?
C13 C2 H2B 110.0 . . ?
C21 C2 H2B 110.0 . . ?
H2A C2 H2B 108.3 . . ?
C26 C21 C22 118.4(2) . . ?
C26 C21 C2 117.6(2) . . ?
C22 C21 C2 123.9(2) . . ?
O22 C22 C21 119.4(2) . . ?
O22 C22 C23 118.4(2) . . ?
C21 C22 C23 122.2(2) . . ?
C24 C23 C22 117.7(2) . . ?
C24 C23 C3 119.5(2) . . ?
C22 C23 C3 122.7(2) . . ?
C25 C24 C23 119.3(2) . . ?
C25 C24 H24 120.4 . . ?
C23 C24 H24 120.4 . . ?
C26 C25 C24 123.3(2) . . ?
C26 C25 N25 118.5(2) . . ?
C24 C25 N25 118.2(3) . . ?
C25 C26 C21 118.8(2) . . ?
C25 C26 H26 120.6 . . ?
C21 C26 H26 120.6 . . ?
C22 O22 C221 113.8(3) . . ?
C22 O22 C224 114.5(3) . . ?
C221 O22 C224 33.1(3) . . ?
C222 C221 O22 112.0(6) . . ?
C222 C221 H22A 109.2 . . ?
O22 C221 H22A 109.2 . . ?
C222 C221 H22B 109.2 . . ?
O22 C221 H22B 109.2 . . ?
H22A C221 H22B 107.9 . . ?
C221 C222 C223 98.8(14) . . ?
C221 C222 H22C 112.0 . . ?
C223 C222 H22C 112.0 . . ?
C221 C222 H22D 112.0 . . ?
C223 C222 H22D 112.0 . . ?
H22C C222 H22D 109.7 . . ?
C222 C223 H22E 109.5 . . ?
C222 C223 H22F 109.5 . . ?
H22E C223 H22F 109.5 . . ?
C222 C223 H22G 109.5 . . ?
H22E C223 H22G 109.5 . . ?
H22F C223 H22G 109.5 . . ?
O22 C224 C225 110.3(6) . . ?
O22 C224 H22H 109.6 . . ?
C225 C224 H22H 109.6 . . ?
O22 C224 H22I 109.6 . . ?
C225 C224 H22I 109.6 . . ?
H22H C224 H22I 108.1 . . ?
C224 C225 C226 103.9(14) . . ?
C224 C225 H22J 111.0 . . ?
C226 C225 H22J 111.0 . . ?
C224 C225 H22K 111.0 . . ?
C226 C225 H22K 111.0 . . ?
H22J C225 H22K 109.0 . . ?
C225 C226 H22L 109.5 . . ?
C225 C226 H22M 109.5 . . ?
H22L C226 H22M 109.5 . . ?
C225 C226 H22N 109.5 . . ?
H22L C226 H22N 109.5 . . ?
H22M C226 H22N 109.5 . . ?
O251 N25 O252 122.9(3) . . ?
O251 N25 C25 117.8(3) . . ?
O252 N25 C25 119.3(3) . . ?
C31 C3 C23 110.53(19) . . ?
C31 C3 H3A 109.5 . . ?
C23 C3 H3A 109.5 . . ?
C31 C3 H3B 109.5 . . ?
C23 C3 H3B 109.5 . . ?
H3A C3 H3B 108.1 . . ?
C36 C31 C32 118.3(2) . . ?
C36 C31 C3 122.6(2) . . ?
C32 C31 C3 119.0(2) . . ?
O32 C32 C31 116.8(2) . . ?
O32 C32 C33 120.2(2) . . ?
C31 C32 C33 122.9(2) . . ?
C34 C33 C32 117.4(2) . . ?
C34 C33 C4 121.1(2) . . ?
C32 C33 C4 121.2(2) . . ?
C35 C34 C33 119.4(2) . . ?
C35 C34 H34 120.3 . . ?
C33 C34 H34 120.3 . . ?
C36 C35 C34 123.3(2) . . ?
C36 C35 N35 118.2(2) . . ?
C34 C35 N35 118.5(2) . . ?
C35 C36 C31 118.2(2) . . ?
C35 C36 H36 120.9 . . ?
C31 C36 H36 120.9 . . ?
C32 O32 C321 113.90(17) . . ?
O32 C321 C322 113.3(2) . . ?
O32 C321 H32A 108.9 . . ?
C322 C321 H32A 108.9 . . ?
O32 C321 H32B 108.9 . . ?
C322 C321 H32B 108.9 . . ?
H32A C321 H32B 107.7 . . ?
C321 C322 C323 110.6(2) . . ?
C321 C322 H32C 109.5 . . ?
C323 C322 H32C 109.5 . . ?
C321 C322 H32D 109.5 . . ?
C323 C322 H32D 109.5 . . ?
H32C C322 H32D 108.1 . . ?
N324 C323 C322 109.9(2) . . ?
N324 C323 H32E 109.7 . . ?
C322 C323 H32E 109.7 . . ?
N324 C323 H32F 109.7 . . ?
C322 C323 H32F 109.7 . . ?
H32E C323 H32F 108.2 . . ?
C325 N324 C323 121.7(2) . . ?
C325 N324 H324 122(2) . . ?
C323 N324 H324 116(2) . . ?
O325 C325 N324 122.0(2) . . ?
O325 C325 C53 122.0(2) . . ?
N324 C325 C53 115.9(2) . . ?
O351 N35 O352 123.4(2) . . ?
O351 N35 C35 118.3(2) . . ?
O352 N35 C35 118.3(2) . . ?
C41 C4 C33 109.46(19) . . ?
C41 C4 H4A 109.8 . . ?
C33 C4 H4A 109.8 . . ?
C41 C4 H4B 109.8 . . ?
C33 C4 H4B 109.8 . . ?
H4A C4 H4B 108.2 . . ?
C46 C41 C42 118.4(2) . . ?
C46 C41 C4 118.8(2) . . ?
C42 C41 C4 122.6(2) . . ?
O42 C42 C43 119.0(2) . . ?
O42 C42 C41 119.2(2) . . ?
C43 C42 C41 121.6(2) . . ?
C44 C43 C42 118.8(2) . . ?
C44 C43 C1 120.3(2) . . ?
C42 C43 C1 120.90(19) . . ?
C45 C44 C43 119.0(2) . . ?
C45 C44 H44 120.5 . . ?
C43 C44 H44 120.5 . . ?
C46 C45 C44 122.6(2) . . ?
C46 C45 N45 118.9(2) . . ?
C44 C45 N45 118.5(2) . . ?
C45 C46 C41 119.6(2) . . ?
C45 C46 H46 120.2 . . ?
C41 C46 H46 120.2 . . ?
C42 O42 C424 111.4(7) . . ?
C42 O42 C421 118.1(9) . . ?
C424 O42 C421 7.2(14) . . ?
C422 C421 O42 114.8(13) . . ?
C422 C421 H42A 108.6 . . ?
O42 C421 H42A 108.6 . . ?
C422 C421 H42B 108.6 . . ?
O42 C421 H42B 108.6 . . ?
H42A C421 H42B 107.5 . . ?
C423 C422 C421 136.0(15) . . ?
C423 C422 H42C 103.2 . . ?
C421 C422 H42C 103.2 . . ?
C423 C422 H42D 103.2 . . ?
C421 C422 H42D 103.2 . . ?
H42C C422 H42D 105.1 . . ?
C422 C423 H42E 109.5 . . ?
C422 C423 H42F 109.5 . . ?
H42E C423 H42F 109.5 . . ?
C422 C423 H42G 109.5 . . ?
H42E C423 H42G 109.5 . . ?
H42F C423 H42G 109.5 . . ?
O42 C424 C425 105.8(9) . . ?
O42 C424 H42H 110.6 . . ?
C425 C424 H42H 110.6 . . ?
O42 C424 H42I 110.6 . . ?
C425 C424 H42I 110.6 . . ?
H42H C424 H42I 108.7 . . ?
C426 C425 C424 123.7(8) . . ?
C426 C425 H42J 106.4 . . ?
C424 C425 H42J 106.4 . . ?
C426 C425 H42K 106.4 . . ?
C424 C425 H42K 106.4 . . ?
H42J C425 H42K 106.5 . . ?
C425 C426 H42L 109.5 . . ?
C425 C426 H42M 109.5 . . ?
H42L C426 H42M 109.5 . . ?
C425 C426 H42N 109.5 . . ?
H42L C426 H42N 109.5 . . ?
H42M C426 H42N 109.5 . . ?
O451 N45 O452 123.0(3) . . ?
O451 N45 C45 118.8(2) . . ?
O452 N45 C45 118.2(3) . . ?
C52 C51 C56 119.0(2) . . ?
C52 C51 C125 121.4(2) . . ?
C56 C51 C125 119.5(2) . . ?
C53 C52 C51 121.4(2) . . ?
C53 C52 H52 119.3 . . ?
C51 C52 H52 119.3 . . ?
C52 C53 C54 119.3(2) . . ?
C52 C53 C325 121.7(2) . . ?
C54 C53 C325 119.0(2) . . ?
C55 C54 C53 119.1(2) . . ?
C55 C54 H54 120.4 . . ?
C53 C54 H54 120.4 . . ?
C56 C55 C54 121.6(2) . . ?
C56 C55 I1 119.87(18) . . ?
C54 C55 I1 118.52(18) . . ?
C55 C56 C51 119.4(2) . . ?
C55 C56 H56 120.3 . . ?
C51 C56 H56 120.3 . . ?
H1WA O1W H1WB 109(4) . . ?
C65 O61 C62 110.6(3) . . ?
O61 C62 C63 105.2(3) . . ?
O61 C62 H62A 110.7 . . ?
C63 C62 H62A 110.7 . . ?
O61 C62 H62B 110.7 . . ?
C63 C62 H62B 110.7 . . ?
H62A C62 H62B 108.8 . . ?
C62 C63 C64 104.2(3) . . ?
C62 C63 H63A 110.9 . . ?
C64 C63 H63A 110.9 . . ?
C62 C63 H63B 110.9 . . ?
C64 C63 H63B 110.9 . . ?
H63A C63 H63B 108.9 . . ?
C65 C64 C63 102.6(4) . . ?
C65 C64 H64A 111.2 . . ?
C63 C64 H64A 111.2 . . ?
C65 C64 H64B 111.2 . . ?
C63 C64 H64B 111.2 . . ?
H64A C64 H64B 109.2 . . ?
O61 C65 C64 106.3(3) . . ?
O61 C65 H65A 110.5 . . ?
C64 C65 H65A 110.5 . . ?
O61 C65 H65B 110.5 . . ?
C64 C65 H65B 110.5 . . ?
H65A C65 H65B 108.7 . . ?
C72 O71 C75 102.1(8) . . ?
C75' O71' C72 104.3(7) . . ?
O71 C72 C73 106.4(7) . . ?
O71 C72 O71' 29.2(5) . . ?
C73 C72 O71' 99.3(6) . . ?
O71 C72 H72A 110.5 . . ?
C73 C72 H72A 110.5 . . ?
O71' C72 H72A 137.4 . . ?
O71 C72 H72B 110.5 . . ?
C73 C72 H72B 110.5 . . ?
O71' C72 H72B 87.5 . . ?
H72A C72 H72B 108.6 . . ?
O71 C72 H72C 130.1 . . ?
C73 C72 H72C 111.9 . . ?
O71' C72 H72C 111.9 . . ?
H72A C72 H72C 84.9 . . ?
H72B C72 H72C 25.6 . . ?
O71 C72 H72D 83.2 . . ?
C73 C72 H72D 111.9 . . ?
O71' C72 H72D 111.9 . . ?
H72A C72 H72D 28.6 . . ?
H72B C72 H72D 129.0 . . ?
H72C C72 H72D 109.6 . . ?
C72 C73 C74 105.2(4) . . ?
C72 C73 H73A 110.7 . . ?
C74 C73 H73A 110.7 . . ?
C72 C73 H73B 110.7 . . ?
C74 C73 H73B 110.7 . . ?
H73A C73 H73B 108.8 . . ?
C75 C74 C73 99.0(6) . . ?
C75 C74 C75' 32.5(6) . . ?
C73 C74 C75' 107.1(5) . . ?
C75 C74 H74A 112.0 . . ?
C73 C74 H74A 112.0 . . ?
C75' C74 H74A 131.4 . . ?
C75 C74 H74B 112.0 . . ?
C73 C74 H74B 112.0 . . ?
C75' C74 H74B 79.9 . . ?
H74A C74 H74B 109.6 . . ?
C75 C74 H74C 140.1 . . ?
C73 C74 H74C 110.3 . . ?
C75' C74 H74C 110.3 . . ?
H74A C74 H74C 82.0 . . ?
H74B C74 H74C 31.9 . . ?
C75 C74 H74D 84.7 . . ?
C73 C74 H74D 110.3 . . ?
C75' C74 H74D 110.3 . . ?
H74A C74 H74D 28.5 . . ?
H74B C74 H74D 130.8 . . ?
H74C C74 H74D 108.5 . . ?
C74 C75 O71 104.6(10) . . ?
C74 C75 H75A 110.8 . . ?
O71 C75 H75A 110.8 . . ?
C74 C75 H75B 110.8 . . ?
O71 C75 H75B 110.8 . . ?
H75A C75 H75B 108.9 . . ?
O71' C75' C74 96.2(7) . . ?
O71' C75' H75C 112.5 . . ?
C74 C75' H75C 112.5 . . ?
O71' C75' H75D 112.5 . . ?
C74 C75' H75D 112.5 . . ?
H75C C75' H75D 110.0 . . ?

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
C43 C1 C11 C16 -95.3(2) . . . . ?
C43 C1 C11 C12 76.9(3) . . . . ?
C16 C11 C12 O12 -175.61(19) . . . . ?
C1 C11 C12 O12 12.0(3) . . . . ?
C16 C11 C12 C13 9.4(3) . . . . ?
C1 C11 C12 C13 -163.0(2) . . . . ?
O12 C12 C13 C14 176.01(19) . . . . ?
C11 C12 C13 C14 -8.9(3) . . . . ?
O12 C12 C13 C2 -9.8(3) . . . . ?
C11 C12 C13 C2 165.3(2) . . . . ?
C12 C13 C14 C15 1.9(3) . . . . ?
C2 C13 C14 C15 -172.2(2) . . . . ?
C13 C14 C15 C16 4.7(3) . . . . ?
C13 C14 C15 N15 -177.7(2) . . . . ?
C14 C15 C16 C11 -4.3(3) . . . . ?
N15 C15 C16 C11 178.1(2) . . . . ?
C12 C11 C16 C15 -2.7(3) . . . . ?
C1 C11 C16 C15 169.7(2) . . . . ?
C13 C12 O12 C121 -105.8(2) . . . . ?
C11 C12 O12 C121 79.0(2) . . . . ?
C12 O12 C121 C122 78.7(2) . . . . ?
O12 C121 C122 C123 178.58(18) . . . . ?
C121 C122 C123 N124 -58.4(3) . . . . ?
C122 C123 N124 C125 159.6(2) . . . . ?
C123 N124 C125 O125 8.1(4) . . . . ?
C123 N124 C125 C51 -169.9(2) . . . . ?
C14 C15 N15 O151 -167.6(2) . . . . ?
C16 C15 N15 O151 10.1(3) . . . . ?
C14 C15 N15 O152 13.9(3) . . . . ?
C16 C15 N15 O152 -168.4(2) . . . . ?
C14 C13 C2 C21 105.8(2) . . . . ?
C12 C13 C2 C21 -68.2(3) . . . . ?
C13 C2 C21 C26 -61.7(3) . . . . ?
C13 C2 C21 C22 114.1(2) . . . . ?
C26 C21 C22 O22 -175.5(2) . . . . ?
C2 C21 C22 O22 8.7(3) . . . . ?
C26 C21 C22 C23 6.3(3) . . . . ?
C2 C21 C22 C23 -169.5(2) . . . . ?
O22 C22 C23 C24 179.4(2) . . . . ?
C21 C22 C23 C24 -2.4(3) . . . . ?
O22 C22 C23 C3 -2.5(3) . . . . ?
C21 C22 C23 C3 175.7(2) . . . . ?
C22 C23 C24 C25 -3.0(4) . . . . ?
C3 C23 C24 C25 178.9(2) . . . . ?
C23 C24 C25 C26 4.6(4) . . . . ?
C23 C24 C25 N25 -177.3(3) . . . . ?
C24 C25 C26 C21 -0.6(4) . . . . ?
N25 C25 C26 C21 -178.7(3) . . . . ?
C22 C21 C26 C25 -4.8(4) . . . . ?
C2 C21 C26 C25 171.3(2) . . . . ?
C21 C22 O22 C221 72.5(5) . . . . ?
C23 C22 O22 C221 -109.3(4) . . . . ?
C21 C22 O22 C224 108.8(4) . . . . ?
C23 C22 O22 C224 -72.9(5) . . . . ?
C22 O22 C221 C222 73.2(7) . . . . ?
C224 O22 C221 C222 -25.7(7) . . . . ?
O22 C221 C222 C223 169.0(10) . . . . ?
C22 O22 C224 C225 -82.8(7) . . . . ?
C221 O22 C224 C225 13.7(7) . . . . ?
O22 C224 C225 C226 174.4(9) . . . . ?
C26 C25 N25 O251 160.2(6) . . . . ?
C24 C25 N25 O251 -18.0(7) . . . . ?
C26 C25 N25 O252 -18.6(5) . . . . ?
C24 C25 N25 O252 163.2(3) . . . . ?
C24 C23 C3 C31 45.4(3) . . . . ?
C22 C23 C3 C31 -132.7(2) . . . . ?
C23 C3 C31 C36 -105.3(3) . . . . ?
C23 C3 C31 C32 70.2(3) . . . . ?
C36 C31 C32 O32 -176.1(2) . . . . ?
C3 C31 C32 O32 8.2(3) . . . . ?
C36 C31 C32 C33 8.3(3) . . . . ?
C3 C31 C32 C33 -167.4(2) . . . . ?
O32 C32 C33 C34 177.9(2) . . . . ?
C31 C32 C33 C34 -6.6(3) . . . . ?
O32 C32 C33 C4 -8.6(3) . . . . ?
C31 C32 C33 C4 166.8(2) . . . . ?
C32 C33 C34 C35 0.6(4) . . . . ?
C4 C33 C34 C35 -172.9(2) . . . . ?
C33 C34 C35 C36 3.6(4) . . . . ?
C33 C34 C35 N35 -178.9(2) . . . . ?
C34 C35 C36 C31 -1.9(4) . . . . ?
N35 C35 C36 C31 -179.4(2) . . . . ?
C32 C31 C36 C35 -3.9(3) . . . . ?
C3 C31 C36 C35 171.6(2) . . . . ?
C31 C32 O32 C321 109.0(2) . . . . ?
C33 C32 O32 C321 -75.3(3) . . . . ?
C32 O32 C321 C322 -60.1(3) . . . . ?
O32 C321 C322 C323 178.4(2) . . . . ?
C321 C322 C323 N324 63.1(3) . . . . ?
C322 C323 N324 C325 -170.7(2) . . . . ?
C323 N324 C325 O325 -2.0(4) . . . . ?
C323 N324 C325 C53 177.2(2) . . . . ?
C36 C35 N35 O351 -1.2(4) . . . . ?
C34 C35 N35 O351 -178.8(3) . . . . ?
C36 C35 N35 O352 178.1(3) . . . . ?
C34 C35 N35 O352 0.5(4) . . . . ?
C34 C33 C4 C41 112.3(2) . . . . ?
C32 C33 C4 C41 -60.9(3) . . . . ?
C33 C4 C41 C46 -65.2(3) . . . . ?
C33 C4 C41 C42 111.3(2) . . . . ?
C46 C41 C42 O42 178.7(2) . . . . ?
C4 C41 C42 O42 2.3(3) . . . . ?
C46 C41 C42 C43 2.4(3) . . . . ?
C4 C41 C42 C43 -174.0(2) . . . . ?
O42 C42 C43 C44 -178.2(2) . . . . ?
C41 C42 C43 C44 -1.9(3) . . . . ?
O42 C42 C43 C1 0.1(3) . . . . ?
C41 C42 C43 C1 176.4(2) . . . . ?
C11 C1 C43 C44 48.1(3) . . . . ?
C11 C1 C43 C42 -130.1(2) . . . . ?
C42 C43 C44 C45 0.2(4) . . . . ?
C1 C43 C44 C45 -178.0(2) . . . . ?
C43 C44 C45 C46 0.8(4) . . . . ?
C43 C44 C45 N45 179.6(2) . . . . ?
C44 C45 C46 C41 -0.2(4) . . . . ?
N45 C45 C46 C41 -179.0(2) . . . . ?
C42 C41 C46 C45 -1.4(4) . . . . ?
C4 C41 C46 C45 175.2(2) . . . . ?
C43 C42 O42 C424 -93.9(5) . . . . ?
C41 C42 O42 C424 89.8(5) . . . . ?
C43 C42 O42 C421 -91.2(10) . . . . ?
C41 C42 O42 C421 92.4(10) . . . . ?
C42 O42 C421 C422 152.2(13) . . . . ?
C424 O42 C421 C422 173(11) . . . . ?
O42 C421 C422 C423 22(3) . . . . ?
C42 O42 C424 C425 -174.9(6) . . . . ?
C421 O42 C424 C425 24(9) . . . . ?
O42 C424 C425 C426 -34.8(13) . . . . ?
C46 C45 N45 O451 170.1(3) . . . . ?
C44 C45 N45 O451 -8.7(5) . . . . ?
C46 C45 N45 O452 -9.6(4) . . . . ?
C44 C45 N45 O452 171.6(3) . . . . ?
O125 C125 C51 C52 -164.6(2) . . . . ?
N124 C125 C51 C52 13.4(3) . . . . ?
O125 C125 C51 C56 13.2(3) . . . . ?
N124 C125 C51 C56 -168.8(2) . . . . ?
C56 C51 C52 C53 2.8(4) . . . . ?
C125 C51 C52 C53 -179.4(2) . . . . ?
C51 C52 C53 C54 -1.4(4) . . . . ?
C51 C52 C53 C325 -179.9(2) . . . . ?
O325 C325 C53 C52 168.1(2) . . . . ?
N324 C325 C53 C52 -11.1(3) . . . . ?
O325 C325 C53 C54 -10.4(4) . . . . ?
N324 C325 C53 C54 170.4(2) . . . . ?
C52 C53 C54 C55 -1.1(4) . . . . ?
C325 C53 C54 C55 177.4(2) . . . . ?
C53 C54 C55 C56 2.3(4) . . . . ?
C53 C54 C55 I1 -177.88(17) . . . . ?
C54 C55 C56 C51 -0.9(4) . . . . ?
I1 C55 C56 C51 179.28(17) . . . . ?
C52 C51 C56 C55 -1.6(3) . . . . ?
C125 C51 C56 C55 -179.5(2) . . . . ?
C65 O61 C62 C63 12.6(5) . . . . ?
O61 C62 C63 C64 -28.5(5) . . . . ?
C62 C63 C64 C65 33.1(5) . . . . ?
C62 O61 C65 C64 8.6(5) . . . . ?
C63 C64 C65 O61 -25.8(5) . . . . ?
C75 O71 C72 C73 -43.1(13) . . . . ?
C75 O71 C72 O71' 36.5(12) . . . . ?
C75' O71' C72 O71 -70.1(14) . . . . ?
C75' O71' C72 C73 36.8(11) . . . . ?
O71 C72 C73 C74 24.0(8) . . . . ?
O71' C72 C73 C74 -5.1(7) . . . . ?
C72 C73 C74 C75 6.8(9) . . . . ?
C72 C73 C74 C75' -25.6(7) . . . . ?
C73 C74 C75 O71 -30.8(14) . . . . ?
C75' C74 C75 O71 77.0(13) . . . . ?
C72 O71 C75 C74 49.1(17) . . . . ?
C72 O71' C75' C74 -50.4(11) . . . . ?
C75 C74 C75' O71' -31.0(12) . . . . ?
C73 C74 C75' O71' 48.7(11) . . . . ?

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
O1W H1WB O22 0.81(4) 2.23(4) 3.015(3) 166(4) .
O1W H1WA O61 0.82(4) 1.90(4) 2.713(3) 174(4) .
N124 H124 O1W 0.83(3) 2.31(3) 3.127(3) 170(3) .
N324 H324 O1W 0.82(3) 2.32(3) 3.127(3) 171(3) .

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.136
_refine_diff_density_min         -0.998
_refine_diff_density_rms         0.059

#END