# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2010

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Gale, Philip'
_publ_contact_author_email       philip.gale@soton.ac.uk

_publ_section_title              
;
Tripodal transmembrane transporters for bicarbonate
;
loop_
_publ_author_name
P.Gale
N.Busschaert
C.Haynes
S.Moore
C.Tong
J.Davis
W.Harrell
;
M.Light
;

# Attachment '- 0341_344_combined_rev1.cif'

data_2010sot0341
_database_code_depnum_ccdc_archive 'CCDC 781768'
#TrackingRef '- 0341_344_combined_rev1.cif'

_chemical_compound_source        'Stephen Moore'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
2(C27 H33 N7 S3), 2(C8 H20 N), C O3
;
_chemical_formula_sum            'C71 H106 N16 O3 S6'
_chemical_formula_weight         1424.08

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   Cc
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   24.1742(5)
_cell_length_b                   24.4456(7)
_cell_length_c                   12.7595(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.313(2)
_cell_angle_gamma                90.00
_cell_volume                     7527.7(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    36058
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.48

_exptl_crystal_description       Slab
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3056
_exptl_absorpt_coefficient_mu    0.238
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9720
_exptl_absorpt_correction_T_max  0.9905
_exptl_absorpt_process_details   
;
SADABS V2.10 (Sheldrick, G.M., 2003)
;

_exptl_special_details           
;
SADABS was used to perform the Absorption correction
Parameter refinement on 28324 reflections reduced R(int) from 0.2283 to 0.0773
Ratio of minimum to maximum apparent transmission: 0.790783
The given Tmin and Tmax were generated using the SHELX SIZE command
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker Nonius FR591 Rotating Anode'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_measurement_device_type  'Bruker-Nonius CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans to fill the asymmetric unit'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            33393
_diffrn_reflns_av_R_equivalents  0.0804
_diffrn_reflns_av_sigmaI/netI    0.1204
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.91
_diffrn_reflns_theta_max         27.48
_reflns_number_total             15112
_reflns_number_gt                10566
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement       
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    
;
Images generated using CrystalMaker: a crystal and molecular
structures program for Mac and Windows. CrystalMaker Software Ltd,
Oxford, England (www.crystalmaker.com)
;
_computing_publication_material  'WINGX (Farrugia, 1998)'
_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^ > 2\s(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.

The structure was refined as a racemic twin with the BASF value refining to
0.69(9)

To avoid several H...H close contacts and therefore discourage energetically
unfavourable side-chain conformations it was necessary to use the shelx
BUMP command. This was applied in its automatic mode which generated 10
distance restraints.
;

_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^)+(0.0000P)^2^+39.6654P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.69(9)
_refine_ls_number_reflns         15112
_refine_ls_number_parameters     874
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.1339
_refine_ls_R_factor_gt           0.0856
_refine_ls_wR_factor_ref         0.1767
_refine_ls_wR_factor_gt          0.1532
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.003
_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
S1 S -0.28231(7) 0.30650(7) -0.01147(14) 0.0373(4) Uani 1 1 d . . .
S2 S -0.17509(7) 0.03022(6) -0.05119(13) 0.0307(4) Uani 1 1 d . . .
S3 S -0.17469(8) 0.37110(7) -0.39158(14) 0.0367(4) Uani 1 1 d . . .
N1 N -0.1743(2) 0.2825(2) 0.0223(4) 0.0273(12) Uani 1 1 d . . .
H901 H -0.1442 0.2729 -0.0087 0.033 Uiso 1 1 calc R . .
N2 N -0.2167(2) 0.2438(2) -0.1214(4) 0.0313(12) Uani 1 1 d . . .
H902 H -0.1852 0.2262 -0.1265 0.038 Uiso 1 1 calc R . .
N3 N -0.11428(19) 0.12073(19) 0.0006(4) 0.0218(11) Uani 1 1 d . . .
H903 H -0.0946 0.1478 -0.0235 0.026 Uiso 1 1 calc R . .
N4 N -0.1401(2) 0.1104(2) -0.1705(4) 0.0258(11) Uani 1 1 d . . .
H904 H -0.1187 0.1389 -0.1792 0.031 Uiso 1 1 calc R . .
N5 N -0.1165(2) 0.36047(19) -0.2068(4) 0.0270(12) Uani 1 1 d . . .
H905 H -0.0983 0.3384 -0.1626 0.032 Uiso 1 1 calc R . .
N6 N -0.1217(2) 0.2847(2) -0.3081(4) 0.0288(12) Uani 1 1 d . . .
H906 H -0.1026 0.2696 -0.2549 0.035 Uiso 1 1 calc R . .
N7 N -0.1944(2) 0.18553(18) -0.3105(4) 0.0248(11) Uani 1 1 d . . .
C1 C -0.1647(2) 0.3020(2) 0.1265(5) 0.0212(13) Uani 1 1 d . . .
C2 C -0.2017(3) 0.2965(2) 0.2035(5) 0.0270(14) Uani 1 1 d . . .
H2 H -0.2378 0.2827 0.1866 0.032 Uiso 1 1 calc R . .
C3 C -0.1858(3) 0.3113(2) 0.3079(5) 0.0297(15) Uani 1 1 d . . .
H3 H -0.2111 0.3069 0.3615 0.036 Uiso 1 1 calc R . .
C4 C -0.1335(3) 0.3323(2) 0.3322(5) 0.0310(15) Uani 1 1 d . . .
H4 H -0.1231 0.3426 0.4024 0.037 Uiso 1 1 calc R . .
C5 C -0.0963(3) 0.3384(2) 0.2546(5) 0.0303(15) Uani 1 1 d . . .
H5 H -0.0604 0.3529 0.2714 0.036 Uiso 1 1 calc R . .
C6 C -0.1115(2) 0.3233(2) 0.1521(5) 0.0277(14) Uani 1 1 d . . .
H6 H -0.0859 0.3273 0.0989 0.033 Uiso 1 1 calc R . .
C7 C -0.2222(2) 0.2762(2) -0.0378(5) 0.0290(14) Uani 1 1 d . . .
C8 C -0.2601(3) 0.2361(3) -0.2045(5) 0.0397(17) Uani 1 1 d . . .
H8A H -0.2612 0.2682 -0.2519 0.048 Uiso 1 1 calc R . .
H8B H -0.2965 0.2331 -0.1732 0.048 Uiso 1 1 calc R . .
C9 C -0.2490(3) 0.1843(2) -0.2672(5) 0.0305(15) Uani 1 1 d . . .
H9A H -0.2516 0.1520 -0.2210 0.037 Uiso 1 1 calc R . .
H9B H -0.2778 0.1807 -0.3253 0.037 Uiso 1 1 calc R . .
C10 C -0.1126(2) 0.1158(2) 0.1122(5) 0.0246(13) Uani 1 1 d . . .
C11 C -0.1075(2) 0.0659(3) 0.1629(5) 0.0304(15) Uani 1 1 d . . .
H11 H -0.1031 0.0331 0.1244 0.036 Uiso 1 1 calc R . .
C12 C -0.1092(3) 0.0650(3) 0.2717(6) 0.0390(18) Uani 1 1 d . . .
H12 H -0.1058 0.0311 0.3078 0.047 Uiso 1 1 calc R . .
C13 C -0.1156(3) 0.1128(4) 0.3287(6) 0.048(2) Uani 1 1 d . . .
H13 H -0.1194 0.1116 0.4024 0.058 Uiso 1 1 calc R . .
C14 C -0.1164(3) 0.1627(3) 0.2750(6) 0.0411(18) Uani 1 1 d . . .
H14 H -0.1178 0.1960 0.3131 0.049 Uiso 1 1 calc R . .
C15 C -0.1152(3) 0.1639(3) 0.1685(5) 0.0318(15) Uani 1 1 d . . .
H15 H -0.1162 0.1980 0.1327 0.038 Uiso 1 1 calc R . .
C16 C -0.1417(2) 0.0898(2) -0.0737(5) 0.0224(13) Uani 1 1 d . . .
C17 C -0.1711(3) 0.0890(2) -0.2626(5) 0.0290(14) Uani 1 1 d . . .
H17A H -0.2084 0.0774 -0.2430 0.035 Uiso 1 1 calc R . .
H17B H -0.1519 0.0564 -0.2890 0.035 Uiso 1 1 calc R . .
C18 C -0.1767(3) 0.1314(2) -0.3475(5) 0.0269(14) Uani 1 1 d . . .
H18A H -0.1406 0.1353 -0.3797 0.032 Uiso 1 1 calc R . .
H18B H -0.2040 0.1184 -0.4028 0.032 Uiso 1 1 calc R . .
C19 C -0.1211(3) 0.4155(2) -0.1726(5) 0.0292(15) Uani 1 1 d . . .
C20 C -0.1323(3) 0.4250(3) -0.0687(5) 0.0353(16) Uani 1 1 d . . .
H20 H -0.1388 0.3949 -0.0239 0.042 Uiso 1 1 calc R . .
C21 C -0.1341(3) 0.4781(3) -0.0289(6) 0.0423(18) Uani 1 1 d . . .
H21 H -0.1413 0.4842 0.0425 0.051 Uiso 1 1 calc R . .
C22 C -0.1251(3) 0.5219(3) -0.0956(6) 0.0445(19) Uani 1 1 d . . .
H22 H -0.1255 0.5582 -0.0690 0.053 Uiso 1 1 calc R . .
C23 C -0.1156(3) 0.5131(3) -0.1990(7) 0.051(2) Uani 1 1 d . . .
H23 H -0.1112 0.5433 -0.2447 0.061 Uiso 1 1 calc R . .
C24 C -0.1125(3) 0.4594(3) -0.2375(6) 0.0374(17) Uani 1 1 d . . .
H24 H -0.1043 0.4533 -0.3086 0.045 Uiso 1 1 calc R . .
C25 C -0.1363(3) 0.3371(3) -0.2982(5) 0.0293(14) Uani 1 1 d . . .
C26 C -0.1347(3) 0.2510(3) -0.3994(5) 0.0333(16) Uani 1 1 d . . .
H26A H -0.1067 0.2216 -0.4025 0.040 Uiso 1 1 calc R . .
H26B H -0.1329 0.2736 -0.4635 0.040 Uiso 1 1 calc R . .
C27 C -0.1921(3) 0.2255(3) -0.3971(5) 0.0332(16) Uani 1 1 d . . .
H27A H -0.2199 0.2545 -0.3882 0.040 Uiso 1 1 calc R . .
H27B H -0.2013 0.2069 -0.4648 0.040 Uiso 1 1 calc R . .
S4 S 0.05039(7) 0.02232(6) -0.09602(13) 0.0289(4) Uani 1 1 d . . .
S5 S 0.18740(7) 0.26841(7) -0.12409(14) 0.0347(4) Uani 1 1 d . . .
S6 S 0.07823(7) 0.35920(7) 0.26355(13) 0.0358(4) Uani 1 1 d . . .
N8 N -0.00203(19) 0.11806(18) -0.1426(4) 0.0231(11) Uani 1 1 d . . .
H908 H -0.0169 0.1477 -0.1168 0.028 Uiso 1 1 calc R . .
N9 N 0.0200(2) 0.1030(2) 0.0293(4) 0.0253(11) Uani 1 1 d . . .
H909 H 0.0012 0.1333 0.0385 0.030 Uiso 1 1 calc R . .
N10 N 0.0759(2) 0.2670(2) -0.1527(4) 0.0340(13) Uani 1 1 d . . .
H910 H 0.0449 0.2644 -0.1202 0.041 Uiso 1 1 calc R . .
N11 N 0.1116(2) 0.2239(2) -0.0085(4) 0.0320(13) Uani 1 1 d . . .
H911 H 0.0776 0.2119 -0.0030 0.038 Uiso 1 1 calc R . .
N12 N 0.0260(2) 0.35338(19) 0.0716(4) 0.0282(12) Uani 1 1 d . . .
H912 H 0.0130 0.3314 0.0214 0.034 Uiso 1 1 calc R . .
N13 N 0.0223(2) 0.2768(2) 0.1711(4) 0.0268(12) Uani 1 1 d . . .
H913 H 0.0055 0.2625 0.1145 0.032 Uiso 1 1 calc R . .
N14 N 0.0802(2) 0.16937(19) 0.1804(4) 0.0240(11) Uani 1 1 d . . .
C28 C -0.0069(2) 0.1137(3) -0.2521(5) 0.0253(13) Uani 1 1 d . . .
C29 C -0.0209(2) 0.0654(3) -0.3060(5) 0.0298(15) Uani 1 1 d . . .
H29 H -0.0275 0.0329 -0.2677 0.036 Uiso 1 1 calc R . .
C30 C -0.0252(3) 0.0645(3) -0.4145(5) 0.0372(16) Uani 1 1 d . . .
H30 H -0.0337 0.0313 -0.4506 0.045 Uiso 1 1 calc R . .
C31 C -0.0173(3) 0.1119(4) -0.4701(6) 0.046(2) Uani 1 1 d . . .
H31 H -0.0204 0.1112 -0.5447 0.055 Uiso 1 1 calc R . .
C32 C -0.0049(3) 0.1602(3) -0.4187(6) 0.048(2) Uani 1 1 d . . .
H32 H 0.0007 0.1927 -0.4577 0.057 Uiso 1 1 calc R . .
C33 C -0.0005(3) 0.1615(3) -0.3098(5) 0.0369(17) Uani 1 1 d . . .
H33 H 0.0070 0.1951 -0.2744 0.044 Uiso 1 1 calc R . .
C34 C 0.0222(2) 0.0835(2) -0.0699(5) 0.0204(12) Uani 1 1 d . . .
C35 C 0.0467(3) 0.0772(2) 0.1212(5) 0.0258(14) Uani 1 1 d . . .
H35A H 0.0833 0.0628 0.1037 0.031 Uiso 1 1 calc R . .
H35B H 0.0239 0.0460 0.1431 0.031 Uiso 1 1 calc R . .
C36 C 0.0542(3) 0.1178(2) 0.2110(5) 0.0278(14) Uani 1 1 d . . .
H36A H 0.0175 0.1259 0.2380 0.033 Uiso 1 1 calc R . .
H36B H 0.0773 0.1008 0.2687 0.033 Uiso 1 1 calc R . .
C37 C 0.0698(2) 0.2863(2) -0.2577(5) 0.0272(14) Uani 1 1 d . . .
C38 C 0.0244(2) 0.3195(3) -0.2833(5) 0.0320(15) Uani 1 1 d . . .
H38 H 0.0013 0.3310 -0.2296 0.038 Uiso 1 1 calc R . .
C39 C 0.0120(3) 0.3360(3) -0.3861(5) 0.0335(15) Uani 1 1 d . . .
H39 H -0.0193 0.3584 -0.4028 0.040 Uiso 1 1 calc R . .
C40 C 0.0455(3) 0.3196(3) -0.4631(6) 0.0341(16) Uani 1 1 d . . .
H40 H 0.0377 0.3314 -0.5334 0.041 Uiso 1 1 calc R . .
C41 C 0.0903(3) 0.2863(3) -0.4399(5) 0.0332(15) Uani 1 1 d . . .
H41 H 0.1130 0.2749 -0.4943 0.040 Uiso 1 1 calc R . .
C42 C 0.1028(2) 0.2691(2) -0.3377(5) 0.0242(13) Uani 1 1 d . . .
H42 H 0.1335 0.2457 -0.3222 0.029 Uiso 1 1 calc R . .
C43 C 0.1229(3) 0.2516(3) -0.0939(5) 0.0289(14) Uani 1 1 d . . .
C44 C 0.1529(3) 0.2121(3) 0.0773(6) 0.0397(18) Uani 1 1 d . . .
H44A H 0.1570 0.2443 0.1241 0.048 Uiso 1 1 calc R . .
H44B H 0.1892 0.2047 0.0481 0.048 Uiso 1 1 calc R . .
C45 C 0.1352(3) 0.1628(3) 0.1401(5) 0.0313(15) Uani 1 1 d . . .
H45A H 0.1353 0.1299 0.0948 0.038 Uiso 1 1 calc R . .
H45B H 0.1626 0.1568 0.1998 0.038 Uiso 1 1 calc R . .
C46 C 0.0291(2) 0.4092(3) 0.0450(5) 0.0294(14) Uani 1 1 d . . .
C47 C 0.0430(3) 0.4228(3) -0.0544(6) 0.0375(16) Uani 1 1 d . . .
H47 H 0.0541 0.3950 -0.1008 0.045 Uiso 1 1 calc R . .
C48 C 0.0409(3) 0.4776(3) -0.0885(7) 0.047(2) Uani 1 1 d . . .
H48 H 0.0492 0.4864 -0.1584 0.057 Uiso 1 1 calc R . .
C49 C 0.0269(3) 0.5182(3) -0.0210(6) 0.0412(18) Uani 1 1 d . . .
H49 H 0.0264 0.5554 -0.0428 0.049 Uiso 1 1 calc R . .
C50 C 0.0135(3) 0.5041(3) 0.0796(6) 0.0381(17) Uani 1 1 d . . .
H50 H 0.0035 0.5321 0.1265 0.046 Uiso 1 1 calc R . .
C51 C 0.0144(3) 0.4505(3) 0.1134(6) 0.0349(16) Uani 1 1 d . . .
H51 H 0.0051 0.4417 0.1827 0.042 Uiso 1 1 calc R . .
C52 C 0.0407(2) 0.3292(2) 0.1652(5) 0.0267(14) Uani 1 1 d . . .
C53 C 0.0286(3) 0.2425(3) 0.2650(5) 0.0322(15) Uani 1 1 d . . .
H53A H -0.0037 0.2177 0.2672 0.039 Uiso 1 1 calc R . .
H53B H 0.0291 0.2661 0.3282 0.039 Uiso 1 1 calc R . .
C54 C 0.0805(3) 0.2094(2) 0.2670(5) 0.0292(14) Uani 1 1 d . . .
H54A H 0.1126 0.2342 0.2620 0.035 Uiso 1 1 calc R . .
H54B H 0.0850 0.1897 0.3348 0.035 Uiso 1 1 calc R . .
N15 N -0.3012(2) 0.07215(19) 0.1758(4) 0.0267(12) Uani 1 1 d . . .
C55 C -0.2817(3) 0.0128(2) 0.1772(5) 0.0296(14) Uani 1 1 d . . .
H55A H -0.2649 0.0048 0.1099 0.035 Uiso 1 1 calc R . .
H55B H -0.2523 0.0084 0.2340 0.035 Uiso 1 1 calc R . .
C56 C -0.3267(3) -0.0290(3) 0.1932(6) 0.0424(18) Uani 1 1 d . . .
H56A H -0.3435 -0.0219 0.2600 0.064 Uiso 1 1 calc R . .
H56B H -0.3106 -0.0658 0.1944 0.064 Uiso 1 1 calc R . .
H56C H -0.3552 -0.0264 0.1356 0.064 Uiso 1 1 calc R . .
C57 C -0.3476(2) 0.0806(3) 0.0925(5) 0.0298(15) Uani 1 1 d . . .
H57A H -0.3795 0.0579 0.1108 0.036 Uiso 1 1 calc R . .
H57B H -0.3593 0.1193 0.0944 0.036 Uiso 1 1 calc R . .
C58 C -0.3339(3) 0.0670(3) -0.0178(5) 0.0407(17) Uani 1 1 d . . .
H58A H -0.2997 0.0858 -0.0344 0.061 Uiso 1 1 calc R . .
H58B H -0.3643 0.0789 -0.0666 0.061 Uiso 1 1 calc R . .
H58C H -0.3288 0.0274 -0.0242 0.061 Uiso 1 1 calc R . .
C59 C -0.3240(3) 0.0888(3) 0.2779(5) 0.0306(14) Uani 1 1 d . . .
H59A H -0.3568 0.0659 0.2897 0.037 Uiso 1 1 calc R . .
H59B H -0.3368 0.1272 0.2716 0.037 Uiso 1 1 calc R . .
C60 C -0.2835(3) 0.0844(3) 0.3751(5) 0.0390(17) Uani 1 1 d . . .
H60A H -0.2706 0.0465 0.3830 0.058 Uiso 1 1 calc R . .
H60B H -0.3024 0.0953 0.4378 0.058 Uiso 1 1 calc R . .
H60C H -0.2517 0.1085 0.3665 0.058 Uiso 1 1 calc R . .
C61 C -0.2508(2) 0.1060(2) 0.1508(5) 0.0292(14) Uani 1 1 d . . .
H61A H -0.2230 0.1032 0.2107 0.035 Uiso 1 1 calc R . .
H61B H -0.2342 0.0898 0.0888 0.035 Uiso 1 1 calc R . .
C62 C -0.2619(3) 0.1653(2) 0.1289(6) 0.0355(16) Uani 1 1 d . . .
H62A H -0.2861 0.1689 0.0649 0.053 Uiso 1 1 calc R . .
H62B H -0.2268 0.1842 0.1192 0.053 Uiso 1 1 calc R . .
H62C H -0.2800 0.1816 0.1881 0.053 Uiso 1 1 calc R . .
N16 N -0.3098(2) 0.4631(2) 0.1906(5) 0.0461(16) Uani 1 1 d . . .
C63 C -0.3665(3) 0.4512(3) 0.1368(6) 0.0434(19) Uani 1 1 d . . .
H63A H -0.3925 0.4430 0.1919 0.052 Uiso 1 1 calc R . .
H63B H -0.3798 0.4850 0.1008 0.052 Uiso 1 1 calc R . .
C64 C -0.3701(3) 0.4050(3) 0.0576(8) 0.061(2) Uani 1 1 d . . .
H64A H -0.3429 0.4110 0.0047 0.092 Uiso 1 1 calc R . .
H64B H -0.4074 0.4040 0.0232 0.092 Uiso 1 1 calc R . .
H64C H -0.3624 0.3702 0.0935 0.092 Uiso 1 1 calc R . .
C65 C -0.2879(4) 0.4150(4) 0.2479(8) 0.063(3) Uani 1 1 d . . .
H65A H -0.2554 0.4265 0.2933 0.076 Uiso 1 1 calc R . .
H65B H -0.2746 0.3885 0.1963 0.076 Uiso 1 1 calc R . .
C66 C -0.3283(4) 0.3854(4) 0.3164(8) 0.070(3) Uani 1 1 d . . .
H66A H -0.3410 0.4106 0.3696 0.106 Uiso 1 1 calc R . .
H66B H -0.3097 0.3541 0.3510 0.106 Uiso 1 1 calc R . .
H66C H -0.3603 0.3724 0.2724 0.106 Uiso 1 1 calc R . .
C67 C -0.2675(3) 0.4775(3) 0.1119(7) 0.054(2) Uani 1 1 d . . .
H67A H -0.2632 0.4460 0.0643 0.065 Uiso 1 1 calc R . .
H67B H -0.2313 0.4841 0.1499 0.065 Uiso 1 1 calc R . .
C68 C -0.2835(3) 0.5285(3) 0.0455(6) 0.053(2) Uani 1 1 d . . .
H68A H -0.3165 0.5204 -0.0003 0.079 Uiso 1 1 calc R . .
H68B H -0.2528 0.5385 0.0025 0.079 Uiso 1 1 calc R . .
H68C H -0.2915 0.5590 0.0921 0.079 Uiso 1 1 calc R . .
C69 C -0.3180(3) 0.5119(3) 0.2627(5) 0.0381(16) Uani 1 1 d . . .
H69A H -0.3417 0.5389 0.2235 0.046 Uiso 1 1 calc R . .
H69B H -0.3388 0.4991 0.3227 0.046 Uiso 1 1 calc R . .
C70 C -0.2662(3) 0.5415(3) 0.3066(6) 0.054(2) Uani 1 1 d . . .
H70A H -0.2422 0.5156 0.3462 0.080 Uiso 1 1 calc R . .
H70B H -0.2769 0.5711 0.3531 0.080 Uiso 1 1 calc R . .
H70C H -0.2463 0.5568 0.2486 0.080 Uiso 1 1 calc R . .
C71 C -0.0515(2) 0.2443(2) -0.0668(5) 0.0186(11) Uani 1 1 d . . .
O1 O -0.09448(15) 0.22122(16) -0.1092(3) 0.0246(9) Uani 1 1 d . . .
O2 O -0.01266(16) 0.21578(16) -0.0204(4) 0.0296(11) Uani 1 1 d . . .
O3 O -0.0460(2) 0.29599(15) -0.0718(4) 0.0344(11) Uani 1 1 d . . .

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
S1 0.0270(9) 0.0390(9) 0.0462(11) -0.0069(8) 0.0047(7) 0.0138(7)
S2 0.0378(9) 0.0202(7) 0.0352(10) -0.0060(7) 0.0126(7) -0.0068(7)
S3 0.0517(11) 0.0320(9) 0.0258(10) 0.0039(7) -0.0029(8) 0.0145(8)
N1 0.023(3) 0.038(3) 0.022(3) -0.002(2) 0.005(2) 0.007(2)
N2 0.026(3) 0.034(3) 0.033(3) -0.005(2) 0.000(2) 0.009(2)
N3 0.026(3) 0.020(2) 0.019(3) 0.002(2) 0.001(2) -0.008(2)
N4 0.026(3) 0.024(3) 0.027(3) 0.005(2) -0.003(2) -0.005(2)
N5 0.039(3) 0.021(3) 0.020(3) 0.007(2) -0.003(2) 0.006(2)
N6 0.035(3) 0.024(3) 0.028(3) 0.008(2) 0.000(2) 0.004(2)
N7 0.033(3) 0.016(2) 0.024(3) -0.002(2) -0.003(2) 0.005(2)
C1 0.021(3) 0.018(3) 0.025(4) 0.004(2) 0.006(2) 0.004(2)
C2 0.031(3) 0.020(3) 0.031(4) 0.003(3) 0.008(3) 0.001(3)
C3 0.037(4) 0.015(3) 0.039(4) 0.005(3) 0.020(3) 0.004(3)
C4 0.044(4) 0.020(3) 0.030(4) 0.002(3) 0.005(3) 0.005(3)
C5 0.030(3) 0.026(3) 0.034(4) 0.005(3) 0.004(3) -0.003(3)
C6 0.024(3) 0.034(3) 0.025(4) 0.008(3) 0.006(3) 0.001(3)
C7 0.027(3) 0.024(3) 0.036(4) 0.003(3) 0.008(3) 0.007(3)
C8 0.036(4) 0.042(4) 0.039(4) -0.003(3) -0.015(3) 0.012(3)
C9 0.030(3) 0.025(3) 0.035(4) -0.005(3) -0.008(3) 0.001(3)
C10 0.018(3) 0.025(3) 0.031(4) 0.000(3) 0.000(2) 0.000(2)
C11 0.025(3) 0.033(4) 0.033(4) 0.014(3) 0.003(3) -0.002(3)
C12 0.030(4) 0.044(4) 0.041(5) 0.023(3) -0.004(3) -0.010(3)
C13 0.035(4) 0.085(6) 0.024(4) 0.007(4) 0.003(3) -0.005(4)
C14 0.032(4) 0.056(5) 0.035(5) -0.016(4) -0.007(3) 0.005(3)
C15 0.030(3) 0.038(4) 0.027(4) -0.003(3) -0.003(3) 0.007(3)
C16 0.015(3) 0.020(3) 0.033(4) 0.003(3) 0.007(2) -0.001(2)
C17 0.035(4) 0.027(3) 0.024(4) -0.003(3) -0.003(3) 0.004(3)
C18 0.032(3) 0.020(3) 0.028(4) -0.011(3) -0.002(3) 0.004(3)
C19 0.030(3) 0.019(3) 0.038(4) 0.004(3) -0.004(3) 0.003(3)
C20 0.049(4) 0.034(4) 0.022(4) -0.002(3) 0.000(3) 0.002(3)
C21 0.062(5) 0.030(4) 0.035(4) -0.012(3) 0.001(4) 0.009(3)
C22 0.065(5) 0.021(3) 0.046(5) -0.011(3) -0.012(4) -0.001(3)
C23 0.069(5) 0.033(4) 0.049(5) 0.004(4) -0.005(4) -0.011(4)
C24 0.053(5) 0.025(3) 0.034(4) -0.005(3) 0.003(3) 0.001(3)
C25 0.029(3) 0.036(4) 0.023(4) 0.005(3) 0.001(3) 0.006(3)
C26 0.046(4) 0.029(3) 0.027(4) 0.002(3) 0.011(3) 0.007(3)
C27 0.038(4) 0.036(4) 0.024(4) -0.007(3) -0.011(3) 0.004(3)
S4 0.0354(9) 0.0211(7) 0.0308(9) 0.0002(6) 0.0057(7) 0.0053(7)
S5 0.0256(8) 0.0401(9) 0.0387(10) 0.0105(8) 0.0041(7) -0.0050(7)
S6 0.0427(10) 0.0353(9) 0.0292(10) -0.0054(7) -0.0002(7) -0.0164(8)
N8 0.030(3) 0.015(2) 0.025(3) -0.010(2) 0.001(2) 0.005(2)
N9 0.025(3) 0.021(3) 0.030(3) 0.000(2) 0.003(2) 0.004(2)
N10 0.029(3) 0.048(3) 0.026(3) 0.002(3) 0.006(2) -0.015(3)
N11 0.031(3) 0.043(3) 0.023(3) 0.005(2) 0.003(2) -0.016(2)
N12 0.031(3) 0.022(3) 0.032(3) -0.011(2) 0.003(2) -0.010(2)
N13 0.024(3) 0.035(3) 0.021(3) -0.001(2) -0.004(2) -0.006(2)
N14 0.031(3) 0.021(3) 0.020(3) 0.001(2) -0.004(2) 0.003(2)
C28 0.018(3) 0.031(3) 0.026(4) 0.000(3) 0.000(2) 0.003(2)
C29 0.030(3) 0.027(3) 0.032(4) -0.006(3) -0.002(3) 0.002(3)
C30 0.028(4) 0.055(5) 0.029(4) -0.003(3) 0.000(3) 0.001(3)
C31 0.022(3) 0.078(6) 0.038(5) -0.003(4) 0.000(3) 0.011(4)
C32 0.037(4) 0.063(5) 0.043(5) 0.022(4) -0.003(3) -0.011(4)
C33 0.040(4) 0.041(4) 0.030(4) 0.007(3) -0.004(3) 0.001(3)
C34 0.021(3) 0.017(3) 0.023(3) -0.001(2) 0.004(2) -0.001(2)
C35 0.032(3) 0.020(3) 0.025(4) 0.005(2) -0.002(3) -0.007(3)
C36 0.033(3) 0.030(3) 0.019(3) 0.001(3) -0.004(3) 0.000(3)
C37 0.029(3) 0.029(3) 0.025(4) -0.007(3) 0.008(3) -0.016(3)
C38 0.022(3) 0.046(4) 0.028(4) -0.013(3) 0.001(3) 0.001(3)
C39 0.036(4) 0.033(4) 0.031(4) -0.005(3) -0.006(3) -0.003(3)
C40 0.042(4) 0.031(4) 0.029(4) 0.000(3) 0.001(3) -0.015(3)
C41 0.038(4) 0.036(4) 0.027(4) -0.009(3) 0.012(3) -0.011(3)
C42 0.024(3) 0.023(3) 0.026(3) 0.002(2) 0.007(3) -0.010(2)
C43 0.027(3) 0.030(3) 0.030(4) -0.002(3) 0.004(3) -0.011(3)
C44 0.040(4) 0.039(4) 0.038(4) 0.008(3) -0.006(3) -0.019(3)
C45 0.029(3) 0.030(3) 0.034(4) 0.003(3) 0.001(3) -0.005(3)
C46 0.028(3) 0.037(4) 0.023(4) -0.004(3) 0.001(3) -0.006(3)
C47 0.048(4) 0.025(3) 0.039(4) -0.003(3) 0.003(3) -0.008(3)
C48 0.052(5) 0.040(4) 0.049(5) 0.007(4) 0.001(4) -0.015(4)
C49 0.045(4) 0.023(3) 0.054(5) 0.002(3) -0.005(4) -0.004(3)
C50 0.037(4) 0.032(4) 0.045(5) -0.009(3) 0.004(3) -0.004(3)
C51 0.040(4) 0.030(3) 0.036(4) 0.003(3) 0.007(3) -0.001(3)
C52 0.024(3) 0.024(3) 0.032(4) 0.001(3) 0.003(3) 0.001(2)
C53 0.041(4) 0.032(4) 0.024(4) -0.003(3) 0.002(3) -0.008(3)
C54 0.040(4) 0.023(3) 0.023(4) 0.000(3) -0.007(3) -0.007(3)
N15 0.024(3) 0.024(3) 0.032(3) 0.000(2) -0.003(2) 0.003(2)
C55 0.034(4) 0.023(3) 0.032(4) -0.001(3) 0.001(3) 0.000(3)
C56 0.040(4) 0.019(3) 0.066(5) 0.001(3) -0.010(4) 0.004(3)
C57 0.023(3) 0.023(3) 0.042(4) 0.007(3) -0.009(3) 0.004(2)
C58 0.035(4) 0.053(4) 0.032(4) -0.006(3) -0.011(3) 0.001(3)
C59 0.031(3) 0.028(3) 0.034(4) 0.000(3) 0.009(3) 0.000(3)
C60 0.041(4) 0.042(4) 0.034(4) 0.005(3) 0.004(3) 0.008(3)
C61 0.022(3) 0.032(3) 0.034(4) 0.005(3) 0.004(3) 0.001(3)
C62 0.030(4) 0.029(3) 0.048(5) 0.003(3) 0.008(3) -0.001(3)
N16 0.037(3) 0.042(3) 0.061(5) 0.003(3) 0.016(3) 0.005(3)
C63 0.027(4) 0.031(4) 0.073(6) 0.001(3) 0.010(3) 0.007(3)
C64 0.037(4) 0.047(5) 0.101(8) -0.019(5) 0.013(4) 0.005(4)
C65 0.052(5) 0.063(6) 0.075(7) 0.016(5) 0.010(5) 0.011(4)
C66 0.075(6) 0.044(5) 0.094(8) 0.027(5) 0.015(5) 0.016(4)
C67 0.047(5) 0.055(5) 0.063(6) 0.000(4) 0.020(4) 0.000(4)
C68 0.043(4) 0.069(6) 0.048(5) 0.006(4) 0.017(4) -0.016(4)
C69 0.041(4) 0.043(4) 0.030(4) 0.005(3) 0.009(3) 0.004(3)
C70 0.044(5) 0.066(6) 0.052(5) 0.007(4) 0.008(4) -0.002(4)
C71 0.022(3) 0.022(3) 0.012(2) -0.005(2) 0.003(2) -0.009(2)
O1 0.020(2) 0.026(2) 0.028(3) 0.0023(18) 0.0013(17) -0.0022(17)
O2 0.026(2) 0.018(2) 0.043(3) -0.0071(19) -0.011(2) 0.0036(18)
O3 0.060(3) 0.014(2) 0.028(2) 0.0011(18) -0.015(2) -0.009(2)

_geom_special_details            
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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
S1 C7 1.682(6) . ?
S2 C16 1.697(6) . ?
S3 C25 1.686(6) . ?
N1 C7 1.361(8) . ?
N1 C1 1.418(8) . ?
N2 C7 1.341(8) . ?
N2 C8 1.459(8) . ?
N3 C16 1.356(7) . ?
N3 C10 1.427(8) . ?
N4 C16 1.337(8) . ?
N4 C17 1.454(7) . ?
N5 C25 1.361(8) . ?
N5 C19 1.421(7) . ?
N6 C25 1.335(8) . ?
N6 C26 1.447(8) . ?
N7 C9 1.461(8) . ?
N7 C27 1.478(8) . ?
N7 C18 1.478(7) . ?
C1 C2 1.374(8) . ?
C1 C6 1.407(8) . ?
C2 C3 1.412(9) . ?
C3 C4 1.383(9) . ?
C4 C5 1.385(9) . ?
C5 C6 1.388(9) . ?
C8 C9 1.529(9) . ?
C10 C15 1.380(9) . ?
C10 C11 1.383(8) . ?
C11 C12 1.392(10) . ?
C12 C13 1.389(11) . ?
C13 C14 1.398(11) . ?
C14 C15 1.362(9) . ?
C17 C18 1.500(8) . ?
C19 C24 1.379(9) . ?
C19 C20 1.388(9) . ?
C20 C21 1.395(9) . ?
C21 C22 1.393(10) . ?
C22 C23 1.369(11) . ?
C23 C24 1.408(10) . ?
C26 C27 1.522(9) . ?
S4 C34 1.685(6) . ?
S5 C43 1.679(6) . ?
S6 C52 1.675(6) . ?
N8 C34 1.362(7) . ?
N8 C28 1.400(8) . ?
N9 C34 1.357(7) . ?
N9 C35 1.450(7) . ?
N10 C43 1.376(8) . ?
N10 C37 1.420(8) . ?
N11 C43 1.325(8) . ?
N11 C44 1.467(8) . ?
N12 C52 1.361(8) . ?
N12 C46 1.409(8) . ?
N13 C52 1.358(7) . ?
N13 C53 1.463(8) . ?
N14 C45 1.464(8) . ?
N14 C36 1.472(7) . ?
N14 C54 1.476(8) . ?
C28 C33 1.395(9) . ?
C28 C29 1.398(8) . ?
C29 C30 1.383(9) . ?
C30 C31 1.377(11) . ?
C31 C32 1.376(11) . ?
C32 C33 1.388(10) . ?
C35 C36 1.518(8) . ?
C37 C38 1.388(9) . ?
C37 C42 1.397(8) . ?
C38 C39 1.389(9) . ?
C39 C40 1.368(9) . ?
C40 C41 1.375(9) . ?
C41 C42 1.386(9) . ?
C44 C45 1.521(8) . ?
C46 C47 1.371(9) . ?
C46 C51 1.393(9) . ?
C47 C48 1.409(9) . ?
C48 C49 1.369(11) . ?
C49 C50 1.385(10) . ?
C50 C51 1.381(9) . ?
C53 C54 1.493(9) . ?
N15 C59 1.501(8) . ?
N15 C57 1.514(7) . ?
N15 C61 1.521(7) . ?
N15 C55 1.525(7) . ?
C55 C56 1.516(9) . ?
C57 C58 1.500(9) . ?
C59 C60 1.539(9) . ?
C61 C62 1.498(8) . ?
N16 C65 1.468(10) . ?
N16 C67 1.515(9) . ?
N16 C63 1.526(9) . ?
N16 C69 1.528(9) . ?
C63 C64 1.514(10) . ?
C65 C66 1.530(12) . ?
C67 C68 1.544(11) . ?
C69 C70 1.523(10) . ?
C71 O3 1.272(6) . ?
C71 O1 1.276(6) . ?
C71 O2 1.286(7) . ?

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
C7 N1 C1 131.0(5) . . ?
C7 N2 C8 123.6(5) . . ?
C16 N3 C10 129.4(5) . . ?
C16 N4 C17 124.7(5) . . ?
C25 N5 C19 129.2(5) . . ?
C25 N6 C26 125.2(5) . . ?
C9 N7 C27 111.7(5) . . ?
C9 N7 C18 112.8(5) . . ?
C27 N7 C18 109.2(5) . . ?
C2 C1 C6 119.6(6) . . ?
C2 C1 N1 124.0(5) . . ?
C6 C1 N1 116.1(5) . . ?
C1 C2 C3 119.8(6) . . ?
C4 C3 C2 120.1(6) . . ?
C3 C4 C5 120.2(6) . . ?
C4 C5 C6 119.9(6) . . ?
C5 C6 C1 120.4(6) . . ?
N2 C7 N1 113.3(5) . . ?
N2 C7 S1 123.1(5) . . ?
N1 C7 S1 123.6(5) . . ?
N2 C8 C9 110.3(5) . . ?
N7 C9 C8 111.8(5) . . ?
C15 C10 C11 120.8(6) . . ?
C15 C10 N3 116.6(5) . . ?
C11 C10 N3 122.5(6) . . ?
C10 C11 C12 118.2(7) . . ?
C13 C12 C11 121.3(7) . . ?
C12 C13 C14 118.4(7) . . ?
C15 C14 C13 120.4(7) . . ?
C14 C15 C10 120.4(7) . . ?
N4 C16 N3 113.4(5) . . ?
N4 C16 S2 121.3(5) . . ?
N3 C16 S2 125.4(5) . . ?
N4 C17 C18 110.8(5) . . ?
N7 C18 C17 113.8(5) . . ?
C24 C19 C20 119.3(6) . . ?
C24 C19 N5 122.3(6) . . ?
C20 C19 N5 118.4(6) . . ?
C19 C20 C21 121.0(7) . . ?
C22 C21 C20 119.0(7) . . ?
C23 C22 C21 120.6(6) . . ?
C22 C23 C24 119.9(7) . . ?
C19 C24 C23 120.2(7) . . ?
N6 C25 N5 113.7(5) . . ?
N6 C25 S3 122.9(5) . . ?
N5 C25 S3 123.4(5) . . ?
N6 C26 C27 112.0(5) . . ?
N7 C27 C26 111.0(5) . . ?
C34 N8 C28 129.9(5) . . ?
C34 N9 C35 124.2(5) . . ?
C43 N10 C37 130.1(5) . . ?
C43 N11 C44 123.5(5) . . ?
C52 N12 C46 128.1(5) . . ?
C52 N13 C53 124.6(5) . . ?
C45 N14 C36 114.2(5) . . ?
C45 N14 C54 111.7(5) . . ?
C36 N14 C54 110.7(5) . . ?
C33 C28 C29 118.7(6) . . ?
C33 C28 N8 117.2(6) . . ?
C29 C28 N8 124.0(6) . . ?
C30 C29 C28 120.4(6) . . ?
C31 C30 C29 119.9(7) . . ?
C32 C31 C30 120.6(7) . . ?
C31 C32 C33 119.9(7) . . ?
C32 C33 C28 120.3(7) . . ?
N9 C34 N8 112.3(5) . . ?
N9 C34 S4 122.3(4) . . ?
N8 C34 S4 125.4(4) . . ?
N9 C35 C36 110.7(5) . . ?
N14 C36 C35 113.2(5) . . ?
C38 C37 C42 118.8(6) . . ?
C38 C37 N10 117.1(6) . . ?
C42 C37 N10 123.7(6) . . ?
C37 C38 C39 121.0(6) . . ?
C40 C39 C38 119.4(6) . . ?
C39 C40 C41 120.7(7) . . ?
C40 C41 C42 120.5(6) . . ?
C41 C42 C37 119.6(6) . . ?
N11 C43 N10 112.7(5) . . ?
N11 C43 S5 123.5(5) . . ?
N10 C43 S5 123.7(5) . . ?
N11 C44 C45 110.4(5) . . ?
N14 C45 C44 112.7(5) . . ?
C47 C46 C51 119.3(6) . . ?
C47 C46 N12 118.5(6) . . ?
C51 C46 N12 122.1(6) . . ?
C46 C47 C48 120.7(7) . . ?
C49 C48 C47 120.1(8) . . ?
C48 C49 C50 118.8(7) . . ?
C51 C50 C49 121.7(7) . . ?
C50 C51 C46 119.5(7) . . ?
N13 C52 N12 112.9(5) . . ?
N13 C52 S6 122.4(5) . . ?
N12 C52 S6 124.7(5) . . ?
N13 C53 C54 111.8(6) . . ?
N14 C54 C53 112.2(5) . . ?
C59 N15 C57 106.2(5) . . ?
C59 N15 C61 111.9(5) . . ?
C57 N15 C61 110.4(5) . . ?
C59 N15 C55 112.1(5) . . ?
C57 N15 C55 110.7(4) . . ?
C61 N15 C55 105.6(4) . . ?
C56 C55 N15 114.8(5) . . ?
C58 C57 N15 115.8(5) . . ?
N15 C59 C60 115.6(5) . . ?
C62 C61 N15 115.4(5) . . ?
C65 N16 C67 106.3(6) . . ?
C65 N16 C63 111.1(6) . . ?
C67 N16 C63 111.7(6) . . ?
C65 N16 C69 112.4(7) . . ?
C67 N16 C69 109.5(5) . . ?
C63 N16 C69 105.9(5) . . ?
C64 C63 N16 117.2(6) . . ?
N16 C65 C66 116.1(7) . . ?
N16 C67 C68 113.2(6) . . ?
C70 C69 N16 117.4(6) . . ?
O3 C71 O1 120.2(5) . . ?
O3 C71 O2 119.1(5) . . ?
O1 C71 O2 120.7(5) . . ?

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
N1 H901 O1 0.88 2.21 3.027(6) 155.1 .
N1 H901 O3 0.88 2.61 3.407(7) 150.6 .
N2 H902 O1 0.88 2.20 3.001(6) 152.0 .
N3 H903 O1 0.88 2.10 2.882(6) 147.2 .
N3 H903 O2 0.88 2.59 3.403(6) 155.0 .
N4 H904 O1 0.88 2.26 3.012(6) 142.8 .
N5 H905 O3 0.88 1.96 2.832(6) 169.8 .
N6 H906 O1 0.88 2.20 3.016(7) 153.5 .
N8 H908 O2 0.88 2.07 2.873(6) 151.3 .
N8 H908 O1 0.88 2.60 3.413(6) 153.1 .
N9 H909 O2 0.88 2.17 2.927(6) 143.7 .
N10 H910 O2 0.88 2.28 3.070(7) 150.0 .
N10 H910 O3 0.88 2.44 3.257(8) 154.3 .
N11 H911 O2 0.88 2.18 3.006(6) 155.7 .
N12 H912 O3 0.88 2.00 2.824(6) 155.4 .
N13 H913 O2 0.88 2.09 2.945(7) 163.2 .

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.460
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.091

#===END

data_2010sot0344
_database_code_depnum_ccdc_archive 'CCDC 781769'
#TrackingRef '- 0341_344_combined_rev1.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
2(C21 H45 N7 O3), 2(C16 H36 N), O4 S, 2(H2 O)
;
_chemical_formula_sum            'C74 H166 N16 O12 S'
_chemical_formula_weight         1504.29

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.3171(4)
_cell_length_b                   14.1510(6)
_cell_length_c                   24.6875(10)
_cell_angle_alpha                90.1722(16)
_cell_angle_beta                 103.847(3)
_cell_angle_gamma                90.899(2)
_cell_volume                     4516.5(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    86085
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      26.37

_exptl_crystal_description       Slab
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1668
_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9668
_exptl_absorpt_correction_T_max  0.9923
_exptl_absorpt_process_details   
;
SADABS V2.10 (Sheldrick, G.M., 2003)
;

_exptl_special_details           
;
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker Nonius FR591 Rotating Anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-Nonius CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans to fill the asymmetric unit'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            79090
_diffrn_reflns_av_R_equivalents  0.1410
_diffrn_reflns_av_sigmaI/netI    0.1374
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.92
_diffrn_reflns_theta_max         26.47
_reflns_number_total             18486
_reflns_number_gt                9385
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement       
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    
;
Images generated using CrystalMaker: a crystal and molecular
structures program for Mac and Windows. CrystalMaker Software Ltd,
Oxford, England (www.crystalmaker.com)
;
_computing_publication_material  'WINGX (Farrugia, 1998)'
_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^ > 2\s(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.

One arm of the first (N15) TBA molecule was modelled as disordered over
two conformations. The temperature factors of each equivalent pair of
atoms (A,B) was constrained to be equal and an additional isotropic
restraint (esd 0.02) was also applied. The geometry was restrained to be
the same as one of the un-disordered arms. An identical procedure was
used to treat one terminal butyl arm of each receptor molecule.

Whilst the positions of the water hydrogens was clear in the difference
map, it was necessary to restrain the O-H distances (0.84(3)) and the
H-O-H angle (H...H 1.4(3)). The temperature factors were freely refined.

In total 235 restraints were applied during the refinement.

;

_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^)+(0.0965P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0042(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         18486
_refine_ls_number_parameters     998
_refine_ls_number_restraints     235
_refine_ls_R_factor_all          0.1687
_refine_ls_R_factor_gt           0.0757
_refine_ls_wR_factor_ref         0.2075
_refine_ls_wR_factor_gt          0.1687
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_restrained_S_all      1.005
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O -0.07993(16) 0.00673(15) 0.19418(9) 0.0343(5) Uani 1 1 d . . .
O2 O 0.20815(19) 0.16712(18) 0.47045(10) 0.0472(7) Uani 1 1 d . A .
O3 O -0.02878(16) 0.50643(15) 0.25769(10) 0.0401(6) Uani 1 1 d . . .
N1 N -0.04625(19) 0.21925(17) 0.32577(10) 0.0263(6) Uani 1 1 d . . .
N2 N 0.04502(19) 0.06983(18) 0.26554(11) 0.0311(6) Uani 1 1 d . . .
H902 H 0.1077 0.0947 0.2757 0.037 Uiso 1 1 calc R . .
N3 N 0.0662(2) 0.0726(2) 0.17653(11) 0.0372(7) Uani 1 1 d . . .
H903 H 0.1285 0.0958 0.1911 0.045 Uiso 1 1 calc R . .
N4 N 0.16630(19) 0.26028(18) 0.39371(11) 0.0312(6) Uani 1 1 d . A .
H904 H 0.1859 0.2839 0.3649 0.037 Uiso 1 1 calc R . .
N6 N 0.00769(19) 0.35301(18) 0.24253(11) 0.0294(6) Uani 1 1 d . . .
H906 H 0.0533 0.3138 0.2351 0.035 Uiso 1 1 calc R . .
N7 N 0.1374(2) 0.46483(18) 0.26262(13) 0.0380(7) Uani 1 1 d . . .
H907 H 0.1788 0.4189 0.2584 0.046 Uiso 1 1 calc R . .
C1 C -0.0938(2) 0.1272(2) 0.30686(14) 0.0283(7) Uani 1 1 d . . .
H1A H -0.1377 0.1331 0.2686 0.034 Uiso 1 1 calc R . .
H1B H -0.1386 0.1069 0.3315 0.034 Uiso 1 1 calc R . .
C2 C -0.0125(2) 0.0529(2) 0.30729(14) 0.0298(7) Uani 1 1 d . . .
H2A H 0.0361 0.0523 0.3446 0.036 Uiso 1 1 calc R . .
H2B H -0.0467 -0.0101 0.3007 0.036 Uiso 1 1 calc R . .
C3 C 0.0047(2) 0.0483(2) 0.21108(14) 0.0302(8) Uani 1 1 d . . .
C4 C 0.0328(3) 0.0617(2) 0.11646(14) 0.0397(9) Uani 1 1 d . . .
H4A H -0.0100 0.0033 0.1076 0.048 Uiso 1 1 calc R . .
H4B H 0.0943 0.0547 0.1009 0.048 Uiso 1 1 calc R . .
C5 C -0.0283(3) 0.1437(3) 0.08933(16) 0.0451(9) Uani 1 1 d . . .
H5A H 0.0126 0.2026 0.1007 0.054 Uiso 1 1 calc R . .
H5B H -0.0923 0.1477 0.1029 0.054 Uiso 1 1 calc R . .
C6 C -0.0576(3) 0.1367(3) 0.02497(16) 0.0486(10) Uani 1 1 d . . .
H6A H -0.0839 0.0720 0.0137 0.058 Uiso 1 1 calc R . .
H6B H -0.1141 0.1812 0.0101 0.058 Uiso 1 1 calc R . .
C7 C 0.0313(3) 0.1588(3) -0.00019(18) 0.0616(12) Uani 1 1 d . . .
H7A H 0.0548 0.2242 0.0088 0.092 Uiso 1 1 calc R . .
H7B H 0.0094 0.1508 -0.0408 0.092 Uiso 1 1 calc R . .
H7C H 0.0881 0.1158 0.0149 0.092 Uiso 1 1 calc R . .
C8 C -0.0183(2) 0.2264(2) 0.38681(13) 0.0307(8) Uani 1 1 d . . .
H8A H -0.0009 0.1630 0.4028 0.037 Uiso 1 1 calc R . .
H8B H -0.0784 0.2493 0.3999 0.037 Uiso 1 1 calc R . .
C9 C 0.0731(2) 0.2933(2) 0.40729(14) 0.0329(8) Uani 1 1 d . . .
H9A H 0.0562 0.3561 0.3904 0.039 Uiso 1 1 calc R . .
H9B H 0.0856 0.3007 0.4483 0.039 Uiso 1 1 calc R . .
C10 C 0.2238(2) 0.1930(2) 0.42527(13) 0.0314(8) Uani 1 1 d . . .
N5A N 0.3008(2) 0.15824(19) 0.40438(11) 0.0366(7) Uani 0.566(4) 1 d PD A 5
H5A1 H 0.3010 0.1711 0.3696 0.044 Uiso 0.566(4) 1 calc PR A 5
C11A C 0.3834(8) 0.1007(6) 0.4365(6) 0.043(2) Uani 0.566(4) 1 d PDU A 5
H11A H 0.3965 0.1197 0.4762 0.051 Uiso 0.566(4) 1 calc PR A 5
H11B H 0.4473 0.1144 0.4239 0.051 Uiso 0.566(4) 1 calc PR A 5
C12A C 0.3621(6) -0.0043(5) 0.4321(3) 0.0498(16) Uani 0.566(4) 1 d PDU A 5
H12A H 0.2985 -0.0182 0.4450 0.060 Uiso 0.566(4) 1 calc PR A 5
H12B H 0.4199 -0.0368 0.4574 0.060 Uiso 0.566(4) 1 calc PR A 5
C13A C 0.3486(6) -0.0444(5) 0.3738(3) 0.0514(14) Uani 0.566(4) 1 d PDU A 5
H13A H 0.2828 -0.0220 0.3498 0.062 Uiso 0.566(4) 1 calc PR A 5
H13B H 0.4057 -0.0209 0.3578 0.062 Uiso 0.566(4) 1 calc PR A 5
C14A C 0.3478(12) -0.1505(6) 0.3736(5) 0.078(3) Uani 0.566(4) 1 d PDU A 5
H14A H 0.4160 -0.1729 0.3935 0.116 Uiso 0.566(4) 1 calc PR A 5
H14B H 0.3318 -0.1739 0.3350 0.116 Uiso 0.566(4) 1 calc PR A 5
H14C H 0.2953 -0.1740 0.3923 0.116 Uiso 0.566(4) 1 calc PR A 5
N5B N 0.3008(2) 0.15824(19) 0.40438(11) 0.0366(7) Uani 0.434(4) 1 d PD A 6
H5B1 H 0.3171 0.1851 0.3755 0.044 Uiso 0.434(4) 1 calc PR A 6
C11B C 0.3564(11) 0.0763(7) 0.4300(8) 0.043(2) Uani 0.434(4) 1 d PDU A 6
H11C H 0.3458 0.0683 0.4681 0.051 Uiso 0.434(4) 1 calc PR A 6
H11D H 0.4313 0.0860 0.4332 0.051 Uiso 0.434(4) 1 calc PR A 6
C12B C 0.3190(8) -0.0118(6) 0.3958(4) 0.0498(16) Uani 0.434(4) 1 d PDU A 6
H12C H 0.3332 -0.0057 0.3584 0.060 Uiso 0.434(4) 1 calc PR A 6
H12D H 0.2434 -0.0202 0.3910 0.060 Uiso 0.434(4) 1 calc PR A 6
C13B C 0.3757(7) -0.0986(6) 0.4260(4) 0.0514(14) Uani 0.434(4) 1 d PDU A 6
H13C H 0.4513 -0.0903 0.4307 0.062 Uiso 0.434(4) 1 calc PR A 6
H13D H 0.3618 -0.1045 0.4635 0.062 Uiso 0.434(4) 1 calc PR A 6
C14B C 0.3389(16) -0.1859(9) 0.3926(6) 0.078(3) Uani 0.434(4) 1 d PDU A 6
H14D H 0.2639 -0.1930 0.3874 0.116 Uiso 0.434(4) 1 calc PR A 6
H14E H 0.3731 -0.2410 0.4123 0.116 Uiso 0.434(4) 1 calc PR A 6
H14F H 0.3556 -0.1809 0.3561 0.116 Uiso 0.434(4) 1 calc PR A 6
C15 C -0.1104(2) 0.2979(2) 0.29977(13) 0.0292(7) Uani 1 1 d . . .
H15A H -0.0922 0.3550 0.3235 0.035 Uiso 1 1 calc R . .
H15B H -0.1841 0.2820 0.2972 0.035 Uiso 1 1 calc R . .
C16 C -0.0956(2) 0.3189(2) 0.24174(13) 0.0307(8) Uani 1 1 d . . .
H16A H -0.1101 0.2606 0.2187 0.037 Uiso 1 1 calc R . .
H16B H -0.1461 0.3669 0.2240 0.037 Uiso 1 1 calc R . .
C17 C 0.0349(2) 0.4451(2) 0.25470(14) 0.0320(8) Uani 1 1 d . . .
C18 C 0.1817(3) 0.5583(2) 0.27768(15) 0.0379(9) Uani 1 1 d . . .
H18A H 0.1253 0.6028 0.2782 0.045 Uiso 1 1 calc R . .
H18B H 0.2172 0.5800 0.2489 0.045 Uiso 1 1 calc R . .
C19 C 0.2587(3) 0.5606(3) 0.33449(18) 0.0549(11) Uani 1 1 d . . .
H19A H 0.3161 0.5178 0.3331 0.066 Uiso 1 1 calc R . .
H19B H 0.2882 0.6254 0.3414 0.066 Uiso 1 1 calc R . .
C20 C 0.2145(4) 0.5327(3) 0.38257(19) 0.0689(13) Uani 1 1 d . . .
H20A H 0.2708 0.5339 0.4170 0.083 Uiso 1 1 calc R . .
H20B H 0.1878 0.4668 0.3766 0.083 Uiso 1 1 calc R . .
C21 C 0.1286(4) 0.5950(4) 0.3912(2) 0.0912(17) Uani 1 1 d . . .
H21A H 0.1529 0.6609 0.3948 0.137 Uiso 1 1 calc R . .
H21B H 0.1081 0.5759 0.4251 0.137 Uiso 1 1 calc R . .
H21C H 0.0691 0.5885 0.3591 0.137 Uiso 1 1 calc R . .
O4 O 0.63406(16) 0.46244(16) 0.30348(9) 0.0360(6) Uani 1 1 d . . .
O5 O 0.55996(17) -0.03078(16) 0.22184(11) 0.0453(7) Uani 1 1 d . . .
O6 O 0.29113(18) 0.33330(18) 0.04052(9) 0.0436(6) Uani 1 1 d . B .
N8 N 0.55817(19) 0.26504(18) 0.16422(10) 0.0277(6) Uani 1 1 d . . .
N9 N 0.49165(19) 0.40579(18) 0.24048(11) 0.0307(6) Uani 1 1 d . . .
H909 H 0.4284 0.3826 0.2354 0.037 Uiso 1 1 calc R . .
N11 N 0.51950(19) 0.11701(19) 0.24595(11) 0.0331(7) Uani 1 1 d . . .
H911 H 0.4736 0.1524 0.2563 0.040 Uiso 1 1 calc R . .
N12 N 0.3970(2) -0.0006(2) 0.23050(14) 0.0481(9) Uani 1 1 d . . .
H912 H 0.3557 0.0416 0.2394 0.058 Uiso 1 1 calc R . .
N13 N 0.33781(19) 0.22047(19) 0.10686(11) 0.0321(6) Uani 1 1 d . B .
H913 H 0.3199 0.1881 0.1335 0.038 Uiso 1 1 calc R . .
C22 C 0.6086(2) 0.3558(2) 0.18275(13) 0.0286(7) Uani 1 1 d . . .
H22A H 0.6434 0.3799 0.1542 0.034 Uiso 1 1 calc R . .
H22B H 0.6621 0.3469 0.2178 0.034 Uiso 1 1 calc R . .
C23 C 0.5316(2) 0.4277(2) 0.19246(13) 0.0296(7) Uani 1 1 d . . .
H23A H 0.5656 0.4909 0.1978 0.035 Uiso 1 1 calc R . .
H23B H 0.4734 0.4302 0.1590 0.035 Uiso 1 1 calc R . .
C24 C 0.5489(2) 0.4200(2) 0.29275(14) 0.0300(8) Uani 1 1 d . . .
N10 N 0.5069(2) 0.3862(2) 0.33372(11) 0.0376(7) Uani 1 1 d D . .
H910 H 0.4447 0.3600 0.3249 0.045 Uiso 1 1 calc R . .
C25 C 0.5616(3) 0.3922(3) 0.39142(14) 0.0402(9) Uani 1 1 d D . .
H25A H 0.5889 0.4573 0.4002 0.048 Uiso 1 1 calc R . .
H25B H 0.6210 0.3490 0.3982 0.048 Uiso 1 1 calc R . .
C26 C 0.4917(3) 0.3661(3) 0.42929(14) 0.0437(9) Uani 1 1 d D . .
H26A H 0.4334 0.4105 0.4229 0.052 Uiso 1 1 calc R . .
H26B H 0.4625 0.3019 0.4192 0.052 Uiso 1 1 calc R . .
C27 C 0.5455(3) 0.3681(3) 0.48994(15) 0.0538(11) Uani 1 1 d D . .
H27A H 0.5779 0.4313 0.4998 0.065 Uiso 1 1 calc R . .
H27B H 0.6012 0.3209 0.4970 0.065 Uiso 1 1 calc R . .
C28 C 0.4706(4) 0.3466(3) 0.52705(18) 0.0670(13) Uani 1 1 d D . .
H28A H 0.4140 0.3918 0.5191 0.100 Uiso 1 1 calc R . .
H28B H 0.5076 0.3521 0.5664 0.100 Uiso 1 1 calc R . .
H28C H 0.4423 0.2823 0.5194 0.100 Uiso 1 1 calc R . .
C29 C 0.6248(2) 0.1850(2) 0.18590(13) 0.0301(8) Uani 1 1 d . . .
H29A H 0.6973 0.2018 0.1862 0.036 Uiso 1 1 calc R . .
H29B H 0.6039 0.1298 0.1608 0.036 Uiso 1 1 calc R . .
C30 C 0.6183(2) 0.1583(2) 0.24423(14) 0.0320(8) Uani 1 1 d . . .
H30A H 0.6733 0.1128 0.2596 0.038 Uiso 1 1 calc R . .
H30B H 0.6310 0.2155 0.2683 0.038 Uiso 1 1 calc R . .
C31 C 0.4953(3) 0.0260(2) 0.23224(15) 0.0368(9) Uani 1 1 d . . .
C32 C 0.3554(3) -0.0947(2) 0.21488(18) 0.0491(10) Uani 1 1 d . . .
H32A H 0.3228 -0.1188 0.2443 0.059 Uiso 1 1 calc R . .
H32B H 0.4130 -0.1370 0.2131 0.059 Uiso 1 1 calc R . .
C33 C 0.2760(3) -0.0989(3) 0.1592(2) 0.0592(12) Uani 1 1 d . . .
H33A H 0.2502 -0.1649 0.1524 0.071 Uiso 1 1 calc R . .
H33B H 0.2166 -0.0595 0.1620 0.071 Uiso 1 1 calc R . .
C34 C 0.3145(4) -0.0664(3) 0.1096(2) 0.0729(14) Uani 1 1 d . . .
H34A H 0.3391 0.0000 0.1159 0.087 Uiso 1 1 calc R . .
H34B H 0.2560 -0.0681 0.0762 0.087 Uiso 1 1 calc R . .
C35 C 0.4013(4) -0.1255(4) 0.0981(2) 0.0982(19) Uani 1 1 d . . .
H35A H 0.4619 -0.1200 0.1297 0.147 Uiso 1 1 calc R . .
H35B H 0.4196 -0.1028 0.0642 0.147 Uiso 1 1 calc R . .
H35C H 0.3786 -0.1918 0.0930 0.147 Uiso 1 1 calc R . .
C36 C 0.5181(2) 0.2606(2) 0.10439(13) 0.0317(8) Uani 1 1 d . . .
H36A H 0.5737 0.2404 0.0868 0.038 Uiso 1 1 calc R . .
H36B H 0.4969 0.3246 0.0905 0.038 Uiso 1 1 calc R . .
C37 C 0.4263(2) 0.1929(2) 0.08696(14) 0.0324(8) Uani 1 1 d . . .
H37A H 0.4062 0.1888 0.0457 0.039 Uiso 1 1 calc R . .
H37B H 0.4474 0.1291 0.1013 0.039 Uiso 1 1 calc R . .
C38 C 0.2817(3) 0.2967(2) 0.08448(13) 0.0340(8) Uani 1 1 d . . .
N14A N 0.2138(2) 0.3275(2) 0.11358(12) 0.0387(7) Uani 0.287(5) 1 d PD B 3
H14G H 0.2143 0.3027 0.1463 0.046 Uiso 0.287(5) 1 calc PR B 3
C39A C 0.1410(17) 0.4002(11) 0.0916(15) 0.0404(18) Uani 0.287(5) 1 d PDU B 3
H39A H 0.0800 0.3961 0.1079 0.048 Uiso 0.287(5) 1 calc PR B 3
H39B H 0.1175 0.3949 0.0505 0.048 Uiso 0.287(5) 1 calc PR B 3
C40A C 0.2008(14) 0.4920(10) 0.1085(7) 0.0380(15) Uani 0.287(5) 1 d PDU B 3
H40A H 0.2334 0.4915 0.1490 0.046 Uiso 0.287(5) 1 calc PR B 3
H40B H 0.2562 0.4987 0.0882 0.046 Uiso 0.287(5) 1 calc PR B 3
C41A C 0.1279(10) 0.5738(8) 0.0950(7) 0.0439(14) Uani 0.287(5) 1 d PDU B 3
H41A H 0.0927 0.5715 0.0548 0.053 Uiso 0.287(5) 1 calc PR B 3
H41B H 0.0743 0.5677 0.1165 0.053 Uiso 0.287(5) 1 calc PR B 3
C42A C 0.1834(11) 0.6677(9) 0.1083(6) 0.0536(15) Uani 0.287(5) 1 d PDU B 3
H42A H 0.2243 0.6677 0.1471 0.080 Uiso 0.287(5) 1 calc PR B 3
H42B H 0.1327 0.7183 0.1035 0.080 Uiso 0.287(5) 1 calc PR B 3
H42C H 0.2294 0.6780 0.0832 0.080 Uiso 0.287(5) 1 calc PR B 3
N14B N 0.2138(2) 0.3275(2) 0.11358(12) 0.0387(7) Uani 0.713(5) 1 d PD B 4
H14H H 0.2000 0.2920 0.1402 0.046 Uiso 0.713(5) 1 calc PR B 4
C39B C 0.1628(6) 0.4193(4) 0.1014(5) 0.0404(18) Uani 0.713(5) 1 d PDU B 4
H39C H 0.0960 0.4160 0.1123 0.048 Uiso 0.713(5) 1 calc PR B 4
H39D H 0.1472 0.4294 0.0606 0.048 Uiso 0.713(5) 1 calc PR B 4
C40B C 0.2237(5) 0.5042(4) 0.1300(2) 0.0380(15) Uani 0.713(5) 1 d PDU B 4
H40C H 0.2828 0.5162 0.1130 0.046 Uiso 0.713(5) 1 calc PR B 4
H40D H 0.2521 0.4889 0.1698 0.046 Uiso 0.713(5) 1 calc PR B 4
C41B C 0.1609(4) 0.5950(4) 0.1267(2) 0.0439(14) Uani 0.713(5) 1 d PDU B 4
H41C H 0.0985 0.5817 0.1407 0.053 Uiso 0.713(5) 1 calc PR B 4
H41D H 0.2030 0.6434 0.1515 0.053 Uiso 0.713(5) 1 calc PR B 4
C42B C 0.1277(5) 0.6350(4) 0.0679(2) 0.0536(15) Uani 0.713(5) 1 d PDU B 4
H42D H 0.1891 0.6497 0.0540 0.080 Uiso 0.713(5) 1 calc PR B 4
H42E H 0.0883 0.6926 0.0687 0.080 Uiso 0.713(5) 1 calc PR B 4
H42F H 0.0843 0.5882 0.0432 0.080 Uiso 0.713(5) 1 calc PR B 4
S1 S 0.27805(6) 0.23586(5) 0.25774(3) 0.0247(2) Uani 1 1 d . . .
O7 O 0.18637(15) 0.22850(15) 0.28105(9) 0.0299(5) Uani 1 1 d . . .
O8 O 0.37244(15) 0.21653(15) 0.30173(9) 0.0335(5) Uani 1 1 d . . .
O9 O 0.26912(16) 0.16693(15) 0.21192(9) 0.0331(5) Uani 1 1 d . . .
O10 O 0.28556(16) 0.33239(15) 0.23633(9) 0.0323(5) Uani 1 1 d . . .
N15 N 0.24915(18) 0.22211(18) 0.62429(10) 0.0271(6) Uani 1 1 d . . .
C43 C 0.3050(2) 0.1448(2) 0.60006(13) 0.0278(7) Uani 1 1 d . C .
H43A H 0.2719 0.1386 0.5598 0.033 Uiso 1 1 calc R . .
H43B H 0.3772 0.1666 0.6033 0.033 Uiso 1 1 calc R . .
C44 C 0.3079(3) 0.0485(2) 0.62542(15) 0.0417(9) Uani 1 1 d . . .
H44A H 0.2369 0.0272 0.6257 0.050 Uiso 1 1 calc R C .
H44B H 0.3495 0.0510 0.6645 0.050 Uiso 1 1 calc R . .
C45 C 0.3548(3) -0.0200(2) 0.59219(17) 0.0461(10) Uani 1 1 d . C .
H45A H 0.3181 -0.0139 0.5525 0.055 Uiso 1 1 calc R . .
H45B H 0.4275 0.0001 0.5954 0.055 Uiso 1 1 calc R . .
C46 C 0.3543(3) -0.1225(2) 0.60683(17) 0.0484(10) Uani 1 1 d . . .
H46A H 0.3987 -0.1318 0.6442 0.073 Uiso 1 1 calc R C .
H46B H 0.3804 -0.1595 0.5796 0.073 Uiso 1 1 calc R . .
H46C H 0.2835 -0.1434 0.6062 0.073 Uiso 1 1 calc R . .
C47 C 0.3045(2) 0.2472(2) 0.68369(13) 0.0296(7) Uani 1 1 d . C .
H47A H 0.3066 0.1897 0.7067 0.036 Uiso 1 1 calc R . .
H47B H 0.2628 0.2943 0.6979 0.036 Uiso 1 1 calc R . .
C48 C 0.4141(2) 0.2863(2) 0.69239(13) 0.0337(8) Uani 1 1 d . . .
H48A H 0.4574 0.2403 0.6784 0.040 Uiso 1 1 calc R C .
H48B H 0.4136 0.3457 0.6712 0.040 Uiso 1 1 calc R . .
C49 C 0.4590(2) 0.3053(2) 0.75407(13) 0.0317(8) Uani 1 1 d . C .
H49A H 0.4145 0.3504 0.7678 0.038 Uiso 1 1 calc R . .
H49B H 0.4590 0.2456 0.7749 0.038 Uiso 1 1 calc R . .
C50 C 0.5684(2) 0.3454(2) 0.76561(15) 0.0405(9) Uani 1 1 d . . .
H50A H 0.6121 0.3023 0.7506 0.061 Uiso 1 1 calc R C .
H50B H 0.5959 0.3525 0.8060 0.061 Uiso 1 1 calc R . .
H50C H 0.5679 0.4072 0.7478 0.061 Uiso 1 1 calc R . .
C51 C 0.2448(2) 0.3057(2) 0.58521(13) 0.0287(7) Uani 1 1 d D C .
H51A H 0.3165 0.3241 0.5847 0.034 Uiso 1 1 calc R . .
H51B H 0.2096 0.2844 0.5470 0.034 Uiso 1 1 calc R . .
C52 C 0.1907(3) 0.3927(2) 0.59883(14) 0.0338(8) Uani 1 1 d D . .
H52A H 0.2304 0.4210 0.6344 0.041 Uiso 1 1 calc R C .
H52B H 0.1209 0.3750 0.6032 0.041 Uiso 1 1 calc R . .
C53 C 0.1818(3) 0.4641(2) 0.55205(14) 0.0357(8) Uani 1 1 d D C .
H53A H 0.2513 0.4770 0.5457 0.043 Uiso 1 1 calc R . .
H53B H 0.1379 0.4367 0.5172 0.043 Uiso 1 1 calc R . .
C54 C 0.1356(3) 0.5563(3) 0.56509(16) 0.0493(10) Uani 1 1 d D . .
H54A H 0.0652 0.5445 0.5694 0.074 Uiso 1 1 calc R C .
H54B H 0.1336 0.6008 0.5345 0.074 Uiso 1 1 calc R . .
H54C H 0.1782 0.5833 0.5998 0.074 Uiso 1 1 calc R . .
C55A C 0.1406(2) 0.1892(2) 0.62573(13) 0.0311(8) Uani 0.458(14) 1 d PDU C 1
H55A H 0.1048 0.2432 0.6379 0.037 Uiso 0.458(14) 1 calc PR C 1
H55B H 0.1466 0.1398 0.6546 0.037 Uiso 0.458(14) 1 calc PR C 1
C56A C 0.0722(11) 0.1500(15) 0.5716(6) 0.036(3) Uani 0.458(14) 1 d PDU C 1
H56A H 0.0946 0.0857 0.5645 0.044 Uiso 0.458(14) 1 calc PR C 1
H56B H 0.0785 0.1908 0.5401 0.044 Uiso 0.458(14) 1 calc PR C 1
C57A C -0.0409(10) 0.1463(13) 0.5762(7) 0.046(3) Uani 0.458(14) 1 d PDU C 1
H57A H -0.0492 0.0976 0.6036 0.055 Uiso 0.458(14) 1 calc PR C 1
H57B H -0.0595 0.2081 0.5896 0.055 Uiso 0.458(14) 1 calc PR C 1
C58A C -0.1124(15) 0.1230(15) 0.5195(9) 0.067(4) Uani 0.458(14) 1 d PDU C 1
H58A H -0.1151 0.1774 0.4948 0.100 Uiso 0.458(14) 1 calc PR C 1
H58B H -0.1820 0.1083 0.5242 0.100 Uiso 0.458(14) 1 calc PR C 1
H58C H -0.0860 0.0682 0.5032 0.100 Uiso 0.458(14) 1 calc PR C 1
C55B C 0.1406(2) 0.1892(2) 0.62573(13) 0.0311(8) Uani 0.542(14) 1 d PDU C 2
H55C H 0.1100 0.2362 0.6466 0.037 Uiso 0.542(14) 1 calc PR C 2
H55D H 0.1447 0.1285 0.6459 0.037 Uiso 0.542(14) 1 calc PR C 2
C56B C 0.0698(10) 0.1761(11) 0.5671(5) 0.036(3) Uani 0.542(14) 1 d PDU C 2
H56C H 0.1088 0.1477 0.5419 0.044 Uiso 0.542(14) 1 calc PR C 2
H56D H 0.0439 0.2381 0.5518 0.044 Uiso 0.542(14) 1 calc PR C 2
C57B C -0.0220(9) 0.1106(10) 0.5712(5) 0.046(3) Uani 0.542(14) 1 d PDU C 2
H57C H 0.0063 0.0507 0.5886 0.055 Uiso 0.542(14) 1 calc PR C 2
H57D H -0.0593 0.1407 0.5968 0.055 Uiso 0.542(14) 1 calc PR C 2
C58B C -0.0993(12) 0.0869(13) 0.5176(7) 0.067(4) Uani 0.542(14) 1 d PDU C 2
H58D H -0.1459 0.1401 0.5067 0.100 Uiso 0.542(14) 1 calc PR C 2
H58E H -0.1396 0.0305 0.5229 0.100 Uiso 0.542(14) 1 calc PR C 2
H58F H -0.0628 0.0745 0.4883 0.100 Uiso 0.542(14) 1 calc PR C 2
N16 N 0.76991(18) 0.71414(18) 0.11560(10) 0.0267(6) Uani 1 1 d . . .
C59 C 0.8308(2) 0.7331(2) 0.17560(12) 0.0284(7) Uani 1 1 d . . .
H59A H 0.7944 0.7823 0.1918 0.034 Uiso 1 1 calc R . .
H59B H 0.8289 0.6746 0.1973 0.034 Uiso 1 1 calc R . .
C60 C 0.9425(2) 0.7643(2) 0.18376(13) 0.0314(8) Uani 1 1 d . . .
H60A H 0.9465 0.8245 0.1639 0.038 Uiso 1 1 calc R . .
H60B H 0.9810 0.7161 0.1682 0.038 Uiso 1 1 calc R . .
C61 C 0.9902(2) 0.7776(2) 0.24543(14) 0.0338(8) Uani 1 1 d . . .
H61A H 0.9486 0.8231 0.2609 0.041 Uiso 1 1 calc R . .
H61B H 0.9877 0.7165 0.2645 0.041 Uiso 1 1 calc R . .
C62 C 1.1011(3) 0.8132(2) 0.25743(15) 0.0402(9) Uani 1 1 d . . .
H62A H 1.1426 0.7688 0.2418 0.060 Uiso 1 1 calc R . .
H62B H 1.1288 0.8184 0.2979 0.060 Uiso 1 1 calc R . .
H62C H 1.1036 0.8753 0.2404 0.060 Uiso 1 1 calc R . .
C63 C 0.7687(2) 0.8000(2) 0.07890(13) 0.0289(7) Uani 1 1 d . . .
H63A H 0.8411 0.8164 0.0787 0.035 Uiso 1 1 calc R . .
H63B H 0.7328 0.7818 0.0403 0.035 Uiso 1 1 calc R . .
C64 C 0.7186(3) 0.8875(2) 0.09424(14) 0.0351(8) Uani 1 1 d . . .
H64A H 0.7531 0.9077 0.1327 0.042 Uiso 1 1 calc R . .
H64B H 0.6448 0.8742 0.0926 0.042 Uiso 1 1 calc R . .
C65 C 0.7283(3) 0.9660(2) 0.05323(15) 0.0388(9) Uani 1 1 d . . .
H65A H 0.8024 0.9767 0.0542 0.047 Uiso 1 1 calc R . .
H65B H 0.6931 0.9450 0.0150 0.047 Uiso 1 1 calc R . .
C66 C 0.6825(3) 1.0579(3) 0.06578(18) 0.0564(11) Uani 1 1 d . . .
H66A H 0.6086 1.0484 0.0636 0.085 Uiso 1 1 calc R . .
H66B H 0.6917 1.1055 0.0385 0.085 Uiso 1 1 calc R . .
H66C H 0.7175 1.0796 0.1034 0.085 Uiso 1 1 calc R . .
C67 C 0.6616(2) 0.6853(2) 0.11898(13) 0.0286(7) Uani 1 1 d . . .
H67A H 0.6663 0.6279 0.1422 0.034 Uiso 1 1 calc R . .
H67B H 0.6338 0.7361 0.1385 0.034 Uiso 1 1 calc R . .
C68 C 0.5853(2) 0.6656(2) 0.06406(14) 0.0346(8) Uani 1 1 d . . .
H68A H 0.6196 0.6297 0.0392 0.042 Uiso 1 1 calc R . .
H68B H 0.5617 0.7261 0.0457 0.042 Uiso 1 1 calc R . .
C69 C 0.4924(3) 0.6090(3) 0.07287(15) 0.0451(9) Uani 1 1 d . . .
H69A H 0.5156 0.5460 0.0876 0.054 Uiso 1 1 calc R . .
H69B H 0.4635 0.6416 0.1011 0.054 Uiso 1 1 calc R . .
C70 C 0.4079(3) 0.5964(3) 0.01964(16) 0.0595(12) Uani 1 1 d . . .
H70A H 0.3781 0.6579 0.0076 0.089 Uiso 1 1 calc R . .
H70B H 0.3538 0.5538 0.0266 0.089 Uiso 1 1 calc R . .
H70C H 0.4375 0.5694 -0.0096 0.089 Uiso 1 1 calc R . .
C71 C 0.8194(2) 0.6367(2) 0.08851(13) 0.0283(7) Uani 1 1 d . . .
H71A H 0.7834 0.6336 0.0485 0.034 Uiso 1 1 calc R . .
H71B H 0.8920 0.6561 0.0907 0.034 Uiso 1 1 calc R . .
C72 C 0.8199(3) 0.5388(2) 0.11181(14) 0.0368(8) Uani 1 1 d . . .
H72A H 0.7491 0.5195 0.1139 0.044 Uiso 1 1 calc R . .
H72B H 0.8654 0.5371 0.1499 0.044 Uiso 1 1 calc R . .
C73 C 0.8593(3) 0.4716(2) 0.07354(14) 0.0385(8) Uani 1 1 d . . .
H73A H 0.8160 0.4778 0.0351 0.046 Uiso 1 1 calc R . .
H73B H 0.9310 0.4906 0.0730 0.046 Uiso 1 1 calc R . .
C74 C 0.8582(3) 0.3694(3) 0.09083(17) 0.0550(11) Uani 1 1 d . . .
H74A H 0.9045 0.3619 0.1279 0.082 Uiso 1 1 calc R . .
H74B H 0.8817 0.3297 0.0638 0.082 Uiso 1 1 calc R . .
H74C H 0.7877 0.3503 0.0920 0.082 Uiso 1 1 calc R . .
O11 O 0.76630(18) 0.55491(16) 0.24809(10) 0.0375(6) Uani 1 1 d D . .
H101 H 0.727(2) 0.518(2) 0.2613(16) 0.060(13) Uiso 1 1 d D . .
H102 H 0.8250(16) 0.531(2) 0.2530(16) 0.060(13) Uiso 1 1 d D . .
O12 O 0.76902(18) 0.92945(16) 0.24447(10) 0.0351(6) Uani 1 1 d D . .
H103 H 0.7080(14) 0.947(2) 0.2355(13) 0.035(10) Uiso 1 1 d D . .
H104 H 0.807(2) 0.960(2) 0.2265(14) 0.049(11) Uiso 1 1 d D . .

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
O1 0.0274(12) 0.0373(14) 0.0367(14) -0.0048(11) 0.0057(11) -0.0086(10)
O2 0.0568(16) 0.0626(18) 0.0267(14) 0.0090(12) 0.0174(12) 0.0175(13)
O3 0.0247(12) 0.0327(14) 0.0648(17) 0.0050(12) 0.0139(12) 0.0066(10)
N1 0.0255(14) 0.0286(15) 0.0249(15) 0.0006(11) 0.0065(12) -0.0006(11)
N2 0.0215(14) 0.0366(16) 0.0350(17) -0.0036(13) 0.0063(12) -0.0036(11)
N3 0.0251(15) 0.0510(19) 0.0347(18) -0.0021(14) 0.0066(13) -0.0104(13)
N4 0.0275(15) 0.0385(17) 0.0271(16) 0.0043(12) 0.0049(12) 0.0037(12)
N6 0.0231(14) 0.0318(16) 0.0351(17) -0.0007(12) 0.0104(12) 0.0007(11)
N7 0.0252(15) 0.0263(16) 0.065(2) -0.0011(14) 0.0160(14) 0.0038(12)
C1 0.0247(16) 0.0298(18) 0.0303(19) -0.0012(14) 0.0071(14) -0.0058(13)
C2 0.0300(18) 0.0261(18) 0.0318(19) -0.0002(14) 0.0048(15) -0.0040(14)
C3 0.0266(18) 0.0294(19) 0.034(2) -0.0035(15) 0.0069(16) -0.0008(14)
C4 0.039(2) 0.043(2) 0.038(2) -0.0014(17) 0.0130(17) -0.0048(17)
C5 0.043(2) 0.045(2) 0.051(3) -0.0015(18) 0.0189(19) 0.0011(17)
C6 0.051(2) 0.045(2) 0.051(3) 0.0021(19) 0.015(2) -0.0023(18)
C7 0.060(3) 0.070(3) 0.060(3) -0.003(2) 0.025(2) 0.001(2)
C8 0.0327(18) 0.0356(19) 0.0254(19) -0.0017(14) 0.0100(15) 0.0010(15)
C9 0.0314(18) 0.037(2) 0.0299(19) -0.0074(15) 0.0062(15) 0.0040(15)
C10 0.0312(18) 0.038(2) 0.0229(19) -0.0070(15) 0.0024(15) -0.0035(15)
N5A 0.0357(16) 0.0440(18) 0.0323(17) 0.0100(13) 0.0118(13) 0.0102(13)
C11A 0.038(6) 0.051(5) 0.041(4) 0.004(4) 0.012(4) 0.008(4)
C12A 0.044(4) 0.053(3) 0.053(5) 0.005(4) 0.011(3) 0.007(3)
C13A 0.047(3) 0.061(4) 0.044(3) -0.004(3) 0.007(3) -0.004(3)
C14A 0.080(4) 0.070(7) 0.073(7) -0.005(5) -0.001(5) 0.002(6)
N5B 0.0357(16) 0.0440(18) 0.0323(17) 0.0100(13) 0.0118(13) 0.0102(13)
C11B 0.038(6) 0.051(5) 0.041(4) 0.004(4) 0.012(4) 0.008(4)
C12B 0.044(4) 0.053(3) 0.053(5) 0.005(4) 0.011(3) 0.007(3)
C13B 0.047(3) 0.061(4) 0.044(3) -0.004(3) 0.007(3) -0.004(3)
C14B 0.080(4) 0.070(7) 0.073(7) -0.005(5) -0.001(5) 0.002(6)
C15 0.0243(16) 0.0329(19) 0.0303(19) -0.0020(15) 0.0069(14) -0.0013(14)
C16 0.0238(17) 0.0310(19) 0.035(2) 0.0011(15) 0.0021(15) -0.0003(14)
C17 0.0262(18) 0.031(2) 0.040(2) 0.0030(15) 0.0101(15) 0.0006(15)
C18 0.0314(19) 0.031(2) 0.054(2) 0.0029(17) 0.0157(18) 0.0007(15)
C19 0.045(2) 0.042(2) 0.073(3) -0.004(2) 0.007(2) -0.0083(18)
C20 0.073(3) 0.062(3) 0.063(3) -0.001(2) 0.001(3) -0.025(3)
C21 0.091(4) 0.113(5) 0.079(4) -0.008(3) 0.040(3) -0.019(3)
O4 0.0321(13) 0.0444(15) 0.0318(14) -0.0068(11) 0.0096(11) -0.0149(11)
O5 0.0300(13) 0.0356(14) 0.0727(19) 0.0048(13) 0.0166(13) 0.0099(11)
O6 0.0453(15) 0.0633(17) 0.0219(14) 0.0068(12) 0.0064(11) 0.0158(12)
N8 0.0255(14) 0.0307(15) 0.0262(16) -0.0014(12) 0.0047(12) 0.0033(11)
N9 0.0225(14) 0.0366(17) 0.0338(17) -0.0044(13) 0.0085(13) -0.0073(12)
N11 0.0244(14) 0.0378(18) 0.0391(18) 0.0008(13) 0.0116(13) 0.0064(12)
N12 0.0295(16) 0.0306(17) 0.092(3) 0.0033(16) 0.0287(17) 0.0030(13)
N13 0.0277(15) 0.0407(17) 0.0267(16) 0.0049(13) 0.0044(12) 0.0003(12)
C22 0.0245(16) 0.0328(19) 0.0288(19) -0.0035(14) 0.0072(14) -0.0049(14)
C23 0.0298(17) 0.0299(19) 0.0288(19) -0.0006(14) 0.0070(15) -0.0037(14)
C24 0.0280(18) 0.0310(19) 0.032(2) -0.0049(15) 0.0097(16) -0.0020(14)
N10 0.0319(15) 0.0540(19) 0.0289(17) -0.0073(14) 0.0123(13) -0.0199(13)
C25 0.041(2) 0.047(2) 0.036(2) -0.0068(17) 0.0162(17) -0.0153(17)
C26 0.041(2) 0.056(3) 0.036(2) 0.0001(18) 0.0141(18) -0.0086(18)
C27 0.055(3) 0.071(3) 0.040(2) -0.002(2) 0.020(2) -0.015(2)
C28 0.084(3) 0.076(3) 0.053(3) 0.006(2) 0.041(3) -0.005(3)
C29 0.0233(16) 0.0344(19) 0.033(2) -0.0032(15) 0.0082(15) 0.0008(14)
C30 0.0242(17) 0.036(2) 0.034(2) -0.0004(15) 0.0020(15) 0.0048(14)
C31 0.0299(19) 0.037(2) 0.046(2) 0.0121(17) 0.0126(17) 0.0112(16)
C32 0.034(2) 0.032(2) 0.085(3) 0.011(2) 0.022(2) 0.0009(16)
C33 0.041(2) 0.043(2) 0.096(4) 0.010(2) 0.021(2) 0.0038(18)
C34 0.063(3) 0.063(3) 0.091(4) 0.010(3) 0.014(3) -0.004(2)
C35 0.064(3) 0.141(5) 0.096(4) -0.014(4) 0.032(3) 0.010(3)
C36 0.0326(18) 0.036(2) 0.0279(19) -0.0016(15) 0.0103(15) 0.0016(15)
C37 0.0315(18) 0.037(2) 0.0277(19) -0.0027(15) 0.0043(15) 0.0023(15)
C38 0.0360(19) 0.043(2) 0.0192(19) -0.0024(16) -0.0002(15) 0.0033(16)
N14A 0.0403(17) 0.0477(19) 0.0303(17) 0.0063(14) 0.0123(14) 0.0116(14)
C39A 0.032(4) 0.055(4) 0.034(5) 0.002(3) 0.005(3) 0.010(3)
C40A 0.037(4) 0.048(3) 0.029(4) 0.003(3) 0.008(3) 0.005(2)
C41A 0.047(3) 0.043(3) 0.040(4) 0.003(3) 0.005(3) 0.004(3)
C42A 0.057(4) 0.058(4) 0.047(3) 0.008(3) 0.012(3) 0.018(3)
N14B 0.0403(17) 0.0477(19) 0.0303(17) 0.0063(14) 0.0123(14) 0.0116(14)
C39B 0.032(4) 0.055(4) 0.034(5) 0.002(3) 0.005(3) 0.010(3)
C40B 0.037(4) 0.048(3) 0.029(4) 0.003(3) 0.008(3) 0.005(2)
C41B 0.047(3) 0.043(3) 0.040(4) 0.003(3) 0.005(3) 0.004(3)
C42B 0.057(4) 0.058(4) 0.047(3) 0.008(3) 0.012(3) 0.018(3)
S1 0.0200(4) 0.0296(5) 0.0254(5) -0.0002(3) 0.0074(3) 0.0000(3)
O7 0.0231(11) 0.0372(13) 0.0312(13) -0.0023(10) 0.0099(10) -0.0009(9)
O8 0.0243(12) 0.0402(14) 0.0341(14) 0.0017(11) 0.0036(10) 0.0000(10)
O9 0.0308(12) 0.0382(14) 0.0324(13) -0.0056(10) 0.0117(10) 0.0007(10)
O10 0.0285(12) 0.0314(13) 0.0389(14) 0.0057(10) 0.0115(10) 0.0008(10)
N15 0.0253(14) 0.0334(16) 0.0241(15) -0.0018(12) 0.0096(12) -0.0029(11)
C43 0.0290(17) 0.0311(19) 0.0263(18) -0.0040(14) 0.0128(14) 0.0004(14)
C44 0.051(2) 0.041(2) 0.038(2) 0.0052(17) 0.0203(18) 0.0097(17)
C45 0.052(2) 0.038(2) 0.054(3) -0.0036(18) 0.025(2) 0.0024(17)
C46 0.053(2) 0.043(2) 0.055(3) 0.0040(19) 0.023(2) 0.0071(18)
C47 0.0301(17) 0.037(2) 0.0238(18) -0.0054(14) 0.0115(14) -0.0001(14)
C48 0.0320(18) 0.040(2) 0.029(2) -0.0032(15) 0.0065(15) -0.0009(15)
C49 0.0309(18) 0.0289(19) 0.034(2) -0.0028(15) 0.0058(15) 0.0036(14)
C50 0.0332(19) 0.041(2) 0.043(2) -0.0058(17) -0.0009(17) -0.0005(16)
C51 0.0273(17) 0.0362(19) 0.0249(18) 0.0046(14) 0.0107(14) 0.0011(14)
C52 0.0319(18) 0.039(2) 0.033(2) -0.0027(15) 0.0122(15) 0.0047(15)
C53 0.0365(19) 0.036(2) 0.034(2) -0.0034(16) 0.0066(16) 0.0010(15)
C54 0.054(2) 0.044(2) 0.051(3) -0.0014(19) 0.015(2) 0.0140(19)
C55A 0.0244(17) 0.043(2) 0.0282(19) -0.0006(15) 0.0103(14) -0.0021(14)
C56A 0.033(2) 0.044(8) 0.035(3) 0.000(4) 0.0117(19) -0.013(3)
C57A 0.027(4) 0.082(8) 0.032(3) -0.003(5) 0.013(3) -0.009(4)
C58A 0.046(4) 0.081(11) 0.068(4) -0.005(6) 0.006(3) -0.023(6)
C55B 0.0244(17) 0.043(2) 0.0282(19) -0.0006(15) 0.0103(14) -0.0021(14)
C56B 0.033(2) 0.044(8) 0.035(3) 0.000(4) 0.0117(19) -0.013(3)
C57B 0.027(4) 0.082(8) 0.032(3) -0.003(5) 0.013(3) -0.009(4)
C58B 0.046(4) 0.081(11) 0.068(4) -0.005(6) 0.006(3) -0.023(6)
N16 0.0248(14) 0.0329(16) 0.0230(15) -0.0008(12) 0.0067(11) 0.0003(11)
C59 0.0330(18) 0.0320(19) 0.0195(17) -0.0011(14) 0.0049(14) 0.0039(14)
C60 0.0289(18) 0.036(2) 0.0284(19) -0.0038(15) 0.0057(15) -0.0036(14)
C61 0.0347(19) 0.033(2) 0.031(2) -0.0002(15) 0.0011(15) 0.0060(15)
C62 0.036(2) 0.035(2) 0.043(2) -0.0035(17) -0.0016(17) 0.0016(16)
C63 0.0274(17) 0.0322(19) 0.0282(19) 0.0016(14) 0.0089(14) -0.0037(14)
C64 0.037(2) 0.035(2) 0.034(2) -0.0004(15) 0.0106(16) 0.0006(15)
C65 0.045(2) 0.033(2) 0.038(2) -0.0030(16) 0.0106(17) -0.0041(16)
C66 0.072(3) 0.038(2) 0.064(3) 0.001(2) 0.025(2) 0.011(2)
C67 0.0263(17) 0.0343(19) 0.0263(19) 0.0014(14) 0.0088(14) -0.0022(14)
C68 0.0317(18) 0.044(2) 0.0284(19) 0.0025(16) 0.0080(15) -0.0042(15)
C69 0.0320(19) 0.066(3) 0.036(2) 0.0021(18) 0.0061(17) -0.0161(18)
C70 0.039(2) 0.096(4) 0.041(2) -0.001(2) 0.0066(19) -0.026(2)
C71 0.0267(17) 0.0361(19) 0.0234(18) -0.0053(14) 0.0089(14) 0.0024(14)
C72 0.043(2) 0.037(2) 0.032(2) 0.0023(16) 0.0114(16) 0.0076(16)
C73 0.044(2) 0.040(2) 0.031(2) -0.0019(16) 0.0087(17) 0.0076(16)
C74 0.072(3) 0.044(2) 0.051(3) -0.0011(19) 0.017(2) 0.021(2)
O11 0.0285(13) 0.0360(14) 0.0518(17) 0.0113(12) 0.0168(12) 0.0048(11)
O12 0.0258(13) 0.0383(15) 0.0433(15) 0.0062(11) 0.0121(12) 0.0036(11)

_geom_special_details            
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C3 1.243(4) . ?
O2 C10 1.238(4) . ?
O3 C17 1.238(4) . ?
N1 C1 1.464(4) . ?
N1 C8 1.466(4) . ?
N1 C15 1.467(4) . ?
N2 C3 1.355(4) . ?
N2 C2 1.442(4) . ?
N3 C3 1.358(4) . ?
N3 C4 1.450(4) . ?
N4 C10 1.356(4) . ?
N4 C9 1.445(4) . ?
N6 C17 1.360(4) . ?
N6 C16 1.446(4) . ?
N7 C17 1.356(4) . ?
N7 C18 1.450(4) . ?
C1 C2 1.519(4) . ?
C4 C5 1.493(5) . ?
C5 C6 1.545(5) . ?
C6 C7 1.492(5) . ?
C8 C9 1.517(4) . ?
C10 N5A 1.353(4) . ?
N5A C11A 1.454(9) . ?
C11A C12A 1.506(9) . ?
C12A C13A 1.514(9) . ?
C13A C14A 1.502(10) . ?
C11B C12B 1.514(12) . ?
C12B C13B 1.550(10) . ?
C13B C14B 1.493(12) . ?
C15 C16 1.522(4) . ?
C18 C19 1.526(5) . ?
C19 C20 1.497(6) . ?
C20 C21 1.508(6) . ?
O4 C24 1.245(4) . ?
O5 C31 1.257(4) . ?
O6 C38 1.237(4) . ?
N8 C36 1.446(4) . ?
N8 C22 1.460(4) . ?
N8 C29 1.471(4) . ?
N9 C24 1.345(4) . ?
N9 C23 1.444(4) . ?
N11 C31 1.345(4) . ?
N11 C30 1.441(4) . ?
N12 C31 1.347(4) . ?
N12 C32 1.449(4) . ?
N13 C38 1.363(4) . ?
N13 C37 1.439(4) . ?
C22 C23 1.514(4) . ?
C24 N10 1.353(4) . ?
N10 C25 1.438(4) . ?
C25 C26 1.511(4) . ?
C26 C27 1.497(5) . ?
C27 C28 1.535(5) . ?
C29 C30 1.512(4) . ?
C32 C33 1.520(6) . ?
C33 C34 1.507(6) . ?
C34 C35 1.518(6) . ?
C36 C37 1.520(4) . ?
C38 N14A 1.358(4) . ?
N14A C39A 1.441(13) . ?
C39A C40A 1.516(14) . ?
C40A C41A 1.509(13) . ?
C41A C42A 1.506(13) . ?
C39B C40B 1.514(7) . ?
C40B C41B 1.535(7) . ?
C41B C42B 1.527(7) . ?
S1 O7 1.472(2) . ?
S1 O9 1.473(2) . ?
S1 O10 1.477(2) . ?
S1 O8 1.481(2) . ?
N15 C47 1.513(4) . ?
N15 C55A 1.521(4) . ?
N15 C51 1.522(4) . ?
N15 C43 1.530(4) . ?
C43 C44 1.499(4) . ?
C44 C45 1.504(4) . ?
C45 C46 1.496(5) . ?
C47 C48 1.519(4) . ?
C48 C49 1.518(4) . ?
C49 C50 1.517(4) . ?
C51 C52 1.513(4) . ?
C52 C53 1.521(4) . ?
C53 C54 1.517(4) . ?
C55A C56A 1.523(11) . ?
C56A C57A 1.537(12) . ?
C57A C58A 1.525(12) . ?
C56B C57B 1.545(11) . ?
C57B C58B 1.503(10) . ?
N16 C67 1.514(4) . ?
N16 C63 1.515(4) . ?
N16 C71 1.520(4) . ?
N16 C59 1.529(4) . ?
C59 C60 1.512(4) . ?
C60 C61 1.513(4) . ?
C61 C62 1.512(4) . ?
C63 C64 1.506(4) . ?
C64 C65 1.529(4) . ?
C65 C66 1.507(5) . ?
C67 C68 1.510(4) . ?
C68 C69 1.522(4) . ?
C69 C70 1.519(5) . ?
C71 C72 1.502(4) . ?
C72 C73 1.523(4) . ?
C73 C74 1.510(5) . ?

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
C1 N1 C8 111.5(2) . . ?
C1 N1 C15 112.1(2) . . ?
C8 N1 C15 112.3(2) . . ?
C3 N2 C2 121.5(3) . . ?
C3 N3 C4 122.3(3) . . ?
C10 N4 C9 120.2(3) . . ?
C17 N6 C16 120.6(2) . . ?
C17 N7 C18 122.8(3) . . ?
N1 C1 C2 111.4(2) . . ?
N2 C2 C1 112.4(3) . . ?
O1 C3 N2 122.9(3) . . ?
O1 C3 N3 122.5(3) . . ?
N2 C3 N3 114.6(3) . . ?
N3 C4 C5 112.5(3) . . ?
C4 C5 C6 113.2(3) . . ?
C7 C6 C5 112.7(3) . . ?
N1 C8 C9 111.5(2) . . ?
N4 C9 C8 112.5(3) . . ?
O2 C10 N5A 122.6(3) . . ?
O2 C10 N4 122.4(3) . . ?
N5A C10 N4 115.0(3) . . ?
C10 N5A C11A 123.4(7) . . ?
N5A C11A C12A 114.8(7) . . ?
C11A C12A C13A 114.2(8) . . ?
C14A C13A C12A 111.8(6) . . ?
C11B C12B C13B 109.2(8) . . ?
C14B C13B C12B 109.5(9) . . ?
N1 C15 C16 111.7(2) . . ?
N6 C16 C15 112.7(3) . . ?
O3 C17 N7 122.4(3) . . ?
O3 C17 N6 122.8(3) . . ?
N7 C17 N6 114.8(3) . . ?
N7 C18 C19 112.7(3) . . ?
C20 C19 C18 114.9(3) . . ?
C19 C20 C21 114.3(4) . . ?
C36 N8 C22 112.3(2) . . ?
C36 N8 C29 112.8(2) . . ?
C22 N8 C29 112.0(2) . . ?
C24 N9 C23 121.5(3) . . ?
C31 N11 C30 122.1(3) . . ?
C31 N12 C32 123.8(3) . . ?
C38 N13 C37 120.2(3) . . ?
N8 C22 C23 111.5(2) . . ?
N9 C23 C22 112.5(3) . . ?
O4 C24 N9 123.1(3) . . ?
O4 C24 N10 121.5(3) . . ?
N9 C24 N10 115.3(3) . . ?
C24 N10 C25 121.5(3) . . ?
N10 C25 C26 111.1(3) . . ?
C27 C26 C25 113.5(3) . . ?
C26 C27 C28 111.8(3) . . ?
N8 C29 C30 112.1(2) . . ?
N11 C30 C29 112.8(3) . . ?
O5 C31 N11 122.4(3) . . ?
O5 C31 N12 122.0(3) . . ?
N11 C31 N12 115.6(3) . . ?
N12 C32 C33 113.7(3) . . ?
C34 C33 C32 115.4(3) . . ?
C33 C34 C35 113.9(4) . . ?
N8 C36 C37 112.7(3) . . ?
N13 C37 C36 113.4(3) . . ?
O6 C38 N14A 123.1(3) . . ?
O6 C38 N13 122.1(3) . . ?
N14A C38 N13 114.8(3) . . ?
C38 N14A C39A 120.9(17) . . ?
N14A C39A C40A 104.5(12) . . ?
C41A C40A C39A 109.3(12) . . ?
C42A C41A C40A 112.0(11) . . ?
C39B C40B C41B 114.5(5) . . ?
C42B C41B C40B 113.6(4) . . ?
O7 S1 O9 109.84(13) . . ?
O7 S1 O10 109.15(12) . . ?
O9 S1 O10 109.53(13) . . ?
O7 S1 O8 109.83(12) . . ?
O9 S1 O8 109.24(13) . . ?
O10 S1 O8 109.23(13) . . ?
C47 N15 C55A 106.7(2) . . ?
C47 N15 C51 112.1(2) . . ?
C55A N15 C51 110.5(2) . . ?
C47 N15 C43 111.8(2) . . ?
C55A N15 C43 110.7(2) . . ?
C51 N15 C43 105.2(2) . . ?
C44 C43 N15 117.4(2) . . ?
C43 C44 C45 109.7(3) . . ?
C46 C45 C44 118.2(3) . . ?
N15 C47 C48 116.3(2) . . ?
C49 C48 C47 109.5(2) . . ?
C50 C49 C48 112.2(3) . . ?
C52 C51 N15 116.6(2) . . ?
C51 C52 C53 109.5(2) . . ?
C54 C53 C52 112.3(3) . . ?
N15 C55A C56A 117.0(7) . . ?
C55A C56A C57A 109.4(12) . . ?
C58A C57A C56A 110.1(12) . . ?
C58B C57B C56B 116.8(11) . . ?
C67 N16 C63 111.3(2) . . ?
C67 N16 C71 111.0(2) . . ?
C63 N16 C71 105.3(2) . . ?
C67 N16 C59 106.2(2) . . ?
C63 N16 C59 112.0(2) . . ?
C71 N16 C59 111.1(2) . . ?
C60 C59 N16 116.8(2) . . ?
C59 C60 C61 109.2(2) . . ?
C62 C61 C60 112.8(3) . . ?
C64 C63 N16 117.3(2) . . ?
C63 C64 C65 108.9(3) . . ?
C66 C65 C64 113.1(3) . . ?
C68 C67 N16 116.1(2) . . ?
C67 C68 C69 110.8(3) . . ?
C70 C69 C68 112.8(3) . . ?
C72 C71 N16 117.7(2) . . ?
C71 C72 C73 108.2(3) . . ?
C74 C73 C72 113.4(3) . . ?

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
C8 N1 C1 C2 -83.2(3) . . . . ?
C15 N1 C1 C2 149.8(2) . . . . ?
C3 N2 C2 C1 -77.7(4) . . . . ?
N1 C1 C2 N2 -68.5(3) . . . . ?
C2 N2 C3 O1 -5.5(5) . . . . ?
C2 N2 C3 N3 177.0(3) . . . . ?
C4 N3 C3 O1 7.2(5) . . . . ?
C4 N3 C3 N2 -175.2(3) . . . . ?
C3 N3 C4 C5 84.5(4) . . . . ?
N3 C4 C5 C6 175.7(3) . . . . ?
C4 C5 C6 C7 -75.6(4) . . . . ?
C1 N1 C8 C9 151.6(2) . . . . ?
C15 N1 C8 C9 -81.6(3) . . . . ?
C10 N4 C9 C8 -80.0(4) . . . . ?
N1 C8 C9 N4 -63.8(3) . . . . ?
C9 N4 C10 O2 -10.4(5) . . . . ?
C9 N4 C10 N5A 171.2(3) . . . . ?
O2 C10 N5A C11A -11.3(6) . . . . ?
N4 C10 N5A C11A 167.1(5) . . . . ?
C10 N5A C11A C12A 91.3(10) . . . . ?
N5A C11A C12A C13A 62.7(12) . . . . ?
C11A C12A C13A C14A 169.1(9) . . . . ?
C11B C12B C13B C14B 179.8(12) . . . . ?
C1 N1 C15 C16 -81.8(3) . . . . ?
C8 N1 C15 C16 151.7(3) . . . . ?
C17 N6 C16 C15 -80.6(4) . . . . ?
N1 C15 C16 N6 -65.4(3) . . . . ?
C18 N7 C17 O3 2.9(5) . . . . ?
C18 N7 C17 N6 -178.0(3) . . . . ?
C16 N6 C17 O3 -10.6(5) . . . . ?
C16 N6 C17 N7 170.2(3) . . . . ?
C17 N7 C18 C19 117.3(4) . . . . ?
N7 C18 C19 C20 -60.8(4) . . . . ?
C18 C19 C20 C21 -60.7(5) . . . . ?
C36 N8 C22 C23 86.5(3) . . . . ?
C29 N8 C22 C23 -145.3(3) . . . . ?
C24 N9 C23 C22 75.0(4) . . . . ?
N8 C22 C23 N9 69.6(3) . . . . ?
C23 N9 C24 O4 8.6(5) . . . . ?
C23 N9 C24 N10 -172.5(3) . . . . ?
O4 C24 N10 C25 -4.2(5) . . . . ?
N9 C24 N10 C25 176.9(3) . . . . ?
C24 N10 C25 C26 169.7(3) . . . . ?
N10 C25 C26 C27 178.2(3) . . . . ?
C25 C26 C27 C28 176.8(3) . . . . ?
C36 N8 C29 C30 -148.4(3) . . . . ?
C22 N8 C29 C30 83.8(3) . . . . ?
C31 N11 C30 C29 79.6(4) . . . . ?
N8 C29 C30 N11 69.1(3) . . . . ?
C30 N11 C31 O5 6.4(5) . . . . ?
C30 N11 C31 N12 -173.8(3) . . . . ?
C32 N12 C31 O5 -2.2(6) . . . . ?
C32 N12 C31 N11 178.0(3) . . . . ?
C31 N12 C32 C33 -110.9(4) . . . . ?
N12 C32 C33 C34 59.9(4) . . . . ?
C32 C33 C34 C35 62.1(5) . . . . ?
C22 N8 C36 C37 -152.8(2) . . . . ?
C29 N8 C36 C37 79.5(3) . . . . ?
C38 N13 C37 C36 71.4(4) . . . . ?
N8 C36 C37 N13 63.4(4) . . . . ?
C37 N13 C38 O6 13.9(5) . . . . ?
C37 N13 C38 N14A -167.3(3) . . . . ?
O6 C38 N14A C39A 6.0(10) . . . . ?
N13 C38 N14A C39A -172.8(9) . . . . ?
C38 N14A C39A C40A -85(2) . . . . ?
N14A C39A C40A C41A -171.9(18) . . . . ?
C39A C40A C41A C42A -177(2) . . . . ?
C39B C40B C41B C42B -67.9(9) . . . . ?
C47 N15 C43 C44 66.5(4) . . . . ?
C55A N15 C43 C44 -52.3(4) . . . . ?
C51 N15 C43 C44 -171.6(3) . . . . ?
N15 C43 C44 C45 173.5(3) . . . . ?
C43 C44 C45 C46 -173.4(3) . . . . ?
C55A N15 C47 C48 -177.4(3) . . . . ?
C51 N15 C47 C48 -56.4(3) . . . . ?
C43 N15 C47 C48 61.5(3) . . . . ?
N15 C47 C48 C49 -178.6(3) . . . . ?
C47 C48 C49 C50 -179.5(3) . . . . ?
C47 N15 C51 C52 -59.6(3) . . . . ?
C55A N15 C51 C52 59.3(3) . . . . ?
C43 N15 C51 C52 178.8(3) . . . . ?
N15 C51 C52 C53 -173.1(3) . . . . ?
C51 C52 C53 C54 -175.6(3) . . . . ?
C47 N15 C55A C56A -173.8(9) . . . . ?
C51 N15 C55A C56A 64.1(10) . . . . ?
C43 N15 C55A C56A -52.0(10) . . . . ?
N15 C55A C56A C57A -164.6(11) . . . . ?
C55A C56A C57A C58A 170.6(13) . . . . ?
C67 N16 C59 C60 -179.4(3) . . . . ?
C63 N16 C59 C60 -57.7(3) . . . . ?
C71 N16 C59 C60 59.8(3) . . . . ?
N16 C59 C60 C61 -178.9(2) . . . . ?
C59 C60 C61 C62 -177.4(3) . . . . ?
C67 N16 C63 C64 56.8(4) . . . . ?
C71 N16 C63 C64 177.1(3) . . . . ?
C59 N16 C63 C64 -62.0(3) . . . . ?
N16 C63 C64 C65 178.4(3) . . . . ?
C63 C64 C65 C66 -178.7(3) . . . . ?
C63 N16 C67 C68 56.0(3) . . . . ?
C71 N16 C67 C68 -60.9(3) . . . . ?
C59 N16 C67 C68 178.2(3) . . . . ?
N16 C67 C68 C69 162.3(3) . . . . ?
C67 C68 C69 C70 173.8(3) . . . . ?
C67 N16 C71 C72 -52.2(4) . . . . ?
C63 N16 C71 C72 -172.8(3) . . . . ?
C59 N16 C71 C72 65.7(3) . . . . ?
N16 C71 C72 C73 172.3(3) . . . . ?
C71 C72 C73 C74 -176.9(3) . . . . ?

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
O12 H104 O1 0.855(17) 1.978(17) 2.814(3) 166(3) 1_665
O12 H103 O5 0.834(17) 1.948(17) 2.772(3) 170(3) 1_565
O11 H102 O3 0.840(17) 1.959(18) 2.779(3) 165(3) 1_655
O11 H101 O4 0.856(17) 1.952(19) 2.788(3) 165(4) .
N2 H902 O7 0.88 2.14 2.872(3) 140.6 .
N3 H903 O9 0.88 2.06 2.932(3) 168.9 .
N4 H904 O7 0.88 2.21 2.891(3) 133.8 .
N6 H906 O7 0.88 2.24 2.955(3) 138.7 .
N7 H907 O10 0.88 2.06 2.924(3) 167.1 .
N5A H5A1 O8 0.88 2.21 3.026(3) 154.7 .
N5A H5A1 O7 0.88 2.49 3.229(3) 141.5 .
N9 H909 O10 0.88 2.02 2.898(3) 171.4 .
N11 H911 O8 0.88 2.16 3.013(3) 164.5 .
N12 H912 O9 0.88 2.15 2.914(3) 144.5 .
N13 H913 O9 0.88 2.22 3.044(3) 156.4 .
N10 H910 O8 0.88 2.25 2.962(3) 138.4 .
N14A H14G O10 0.88 2.23 2.952(4) 138.5 .
N14A H14G O9 0.88 2.52 3.291(4) 146.7 .
N14B H14H O10 0.88 2.44 2.952(4) 117.8 .
N14B H14H O9 0.88 2.53 3.291(4) 145.0 .

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        26.47
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.076