# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2011
data_global
_journal_name_full               Chem.Commun.
_journal_coden_cambridge         0182
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
loop_
_publ_author_name
'Dongwhan Lee'
'Ho Lee'
JunyongJo
'Hyunsoo Park'
_publ_contact_author_email       dongwhan@indiana.edu
_publ_contact_author_name        'Lee, Dongwhan'

data_09024new
_database_code_depnum_ccdc_archive 'CCDC 814670'
#TrackingRef '- cmpd_3.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C26 H30 N2 O4'
_chemical_formula_sum            'C26 H30 N2 O4'
_chemical_melting_point          ?

_exptl_crystal_description       block
_exptl_crystal_colour            red

_diffrn_ambient_temperature      150(2)
_chemical_formula_weight         434.52

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_int_tables_number      2
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   15.452(3)
_cell_length_b                   17.781(3)
_cell_length_c                   17.792(3)
_cell_angle_alpha                84.536(5)
_cell_angle_beta                 88.272(4)
_cell_angle_gamma                88.275(5)
_cell_volume                     4862.1(15)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1933
_cell_measurement_theta_min      1.15
_cell_measurement_theta_max      28.28
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1856
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9881
_exptl_absorpt_correction_T_max  0.9905
_exptl_absorpt_process_details   'SADABS (Bruker-AXS, 2001)'

_exptl_special_details           
;
?
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker APEX II'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  kappa
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 83.33
_diffrn_reflns_number            64258
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0628
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.15
_diffrn_reflns_theta_max         28.28
_reflns_number_total             23666
_reflns_number_gt                14351
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker-AXS, 2009)'
_computing_cell_refinement       'APEX2 (Bruker-AXS, 2009)'
_computing_data_reduction        'APEX2 (Bruker-AXS, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Diamond 3.2 (Crystal Impact, 2009)'
_computing_publication_material  'WinGX 1.70.01 (2005)'

_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^)+(0.0758P)^2^+0.6354P] 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         23666
_refine_ls_number_parameters     1195
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.1111
_refine_ls_R_factor_gt           0.0583
_refine_ls_wR_factor_ref         0.1669
_refine_ls_wR_factor_gt          0.1387
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.041
_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
O1 O 0.85587(14) 0.35852(14) 1.11192(15) 0.0330(6) Uani 1 1 d . . .
H1 H 0.8962 0.3877 1.1181 0.049 Uiso 1 1 calc R . .
O2 O 1.12464(16) 0.78881(15) 0.90791(18) 0.0404(7) Uani 1 1 d . . .
H2 H 1.1324 0.7432 0.9002 0.061 Uiso 1 1 calc R . .
O3 O 0.96258(14) 0.48099(14) 1.09693(15) 0.0306(6) Uani 1 1 d . . .
H3 H 0.9261 0.5090 1.0730 0.046 Uiso 1 1 calc R . .
O4 O 1.24335(15) 0.48982(15) 1.18531(16) 0.0359(6) Uani 1 1 d . . .
H4 H 1.2843 0.5197 1.1860 0.054 Uiso 1 1 calc R . .
N1 N 0.90669(17) 0.59762(18) 1.02284(17) 0.0250(7) Uani 1 1 d . . .
N2 N 0.97733(17) 0.63394(17) 1.02923(17) 0.0243(7) Uani 1 1 d . . .
C1 C 0.6837(2) 0.6878(2) 0.9110(2) 0.0239(8) Uani 1 1 d . . .
C2 C 0.6849(2) 0.6211(2) 0.9590(2) 0.0242(8) Uani 1 1 d . . .
H2A H 0.6333 0.5934 0.9668 0.029 Uiso 1 1 calc R . .
C3 C 0.7586(2) 0.5942(2) 0.9957(2) 0.0243(8) Uani 1 1 d . . .
C4 C 0.8362(2) 0.6321(2) 0.9843(2) 0.0235(8) Uani 1 1 d . . .
C5 C 0.8382(2) 0.6986(2) 0.9345(2) 0.0253(8) Uani 1 1 d . . .
C6 C 0.7622(2) 0.7244(2) 0.8999(2) 0.0274(8) Uani 1 1 d . . .
H6A H 0.7638 0.7697 0.8669 0.033 Uiso 1 1 calc R . .
C7 C 0.5912(3) 0.6653(2) 0.8059(2) 0.0623(13) Uani 1 1 d . . .
H7A H 0.6426 0.6677 0.7724 0.093 Uiso 1 1 calc R . .
H7B H 0.5401 0.6829 0.7772 0.093 Uiso 1 1 calc R . .
H7C H 0.5833 0.6130 0.8273 0.093 Uiso 1 1 calc R . .
C8 C 0.6026(2) 0.7153(2) 0.8694(2) 0.0281(8) Uani 1 1 d . . .
C9 C 0.6095(2) 0.7973(2) 0.8354(2) 0.0464(10) Uani 1 1 d . . .
H9A H 0.6215 0.8296 0.8753 0.070 Uiso 1 1 calc R . .
H9B H 0.5548 0.8140 0.8118 0.070 Uiso 1 1 calc R . .
H9C H 0.6566 0.8009 0.7972 0.070 Uiso 1 1 calc R . .
C10 C 0.5249(2) 0.7129(2) 0.9228(2) 0.0505(11) Uani 1 1 d . . .
H10A H 0.5139 0.6604 0.9416 0.076 Uiso 1 1 calc R . .
H10B H 0.4741 0.7348 0.8961 0.076 Uiso 1 1 calc R . .
H10C H 0.5361 0.7421 0.9654 0.076 Uiso 1 1 calc R . .
C11 C 0.7585(2) 0.5241(2) 1.0445(2) 0.0263(8) Uani 1 1 d . . .
C12 C 0.7643(2) 0.4664(2) 1.0835(2) 0.0278(8) Uani 1 1 d . . .
C13 C 0.7745(2) 0.3939(2) 1.1310(2) 0.0287(8) Uani 1 1 d . . .
C14 C 0.7058(2) 0.3399(2) 1.1133(2) 0.0417(10) Uani 1 1 d . . .
H14A H 0.7096 0.3323 1.0594 0.063 Uiso 1 1 calc R . .
H14B H 0.6484 0.3610 1.1257 0.063 Uiso 1 1 calc R . .
H14C H 0.7150 0.2913 1.1433 0.063 Uiso 1 1 calc R . .
C15 C 0.7730(3) 0.4074(3) 1.2143(2) 0.0548(12) Uani 1 1 d . . .
H15A H 0.7840 0.3594 1.2448 0.082 Uiso 1 1 calc R . .
H15B H 0.7161 0.4283 1.2285 0.082 Uiso 1 1 calc R . .
H15C H 0.8178 0.4431 1.2231 0.082 Uiso 1 1 calc R . .
C16 C 0.9154(2) 0.7396(2) 0.9148(2) 0.0280(8) Uani 1 1 d . . .
C17 C 0.9741(2) 0.7772(2) 0.8915(2) 0.0358(10) Uani 1 1 d . . .
C18 C 1.0517(2) 0.8196(2) 0.8670(3) 0.0476(12) Uani 1 1 d . . .
C19 C 1.0702(3) 0.8147(3) 0.7828(3) 0.0830(19) Uani 1 1 d . . .
H19A H 1.1228 0.8421 0.7673 0.125 Uiso 1 1 calc R . .
H19B H 1.0213 0.8372 0.7540 0.125 Uiso 1 1 calc R . .
H19C H 1.0783 0.7616 0.7731 0.125 Uiso 1 1 calc R . .
C20 C 1.0409(3) 0.8998(2) 0.8863(4) 0.098(2) Uani 1 1 d . . .
H20A H 1.0386 0.9006 0.9413 0.147 Uiso 1 1 calc R . .
H20B H 0.9871 0.9221 0.8652 0.147 Uiso 1 1 calc R . .
H20C H 1.0901 0.9291 0.8650 0.147 Uiso 1 1 calc R . .
C21 C 1.0403(2) 0.5944(2) 1.0683(2) 0.0262(8) Uani 1 1 d . . .
C22 C 1.0339(2) 0.5178(2) 1.1020(2) 0.0237(8) Uani 1 1 d . . .
C23 C 1.1040(2) 0.4843(2) 1.1409(2) 0.0256(8) Uani 1 1 d . . .
H23 H 1.1012 0.4333 1.1621 0.031 Uiso 1 1 calc R . .
C24 C 1.1777(2) 0.5246(2) 1.1491(2) 0.0252(8) Uani 1 1 d . . .
C25 C 1.1844(2) 0.6001(2) 1.1157(2) 0.0281(8) Uani 1 1 d . . .
H25 H 1.2356 0.6272 1.1207 0.034 Uiso 1 1 calc R . .
C26 C 1.1164(2) 0.6336(2) 1.0761(2) 0.0271(8) Uani 1 1 d . . .
H26 H 1.1210 0.6840 1.0537 0.033 Uiso 1 1 calc R . .
O5 O 0.63847(16) 0.38738(16) 0.64466(15) 0.0359(6) Uani 1 1 d . . .
H5 H 0.5973 0.3794 0.6169 0.054 Uiso 1 1 calc R . .
O6 O 0.37248(15) 0.57750(16) 0.21104(15) 0.0362(7) Uani 1 1 d . . .
H6 H 0.3674 0.5962 0.2526 0.054 Uiso 1 1 calc R . .
O7 O 0.52859(15) 0.40082(15) 0.52001(14) 0.0287(6) Uani 1 1 d . . .
H7 H 0.5660 0.4244 0.4926 0.043 Uiso 1 1 calc R . .
O8 O 0.24747(16) 0.31395(16) 0.50963(16) 0.0384(7) Uani 1 1 d . . .
H8 H 0.2061 0.3133 0.4802 0.058 Uiso 1 1 calc R . .
N3 N 0.58829(17) 0.47113(17) 0.40157(17) 0.0238(7) Uani 1 1 d . . .
N4 N 0.51860(18) 0.46662(17) 0.36542(18) 0.0250(7) Uani 1 1 d . . .
C31 C 0.8086(2) 0.5863(2) 0.3141(2) 0.0253(8) Uani 1 1 d . . .
C32 C 0.8093(2) 0.5395(2) 0.3808(2) 0.0274(8) Uani 1 1 d . . .
H32 H 0.8612 0.5330 0.4082 0.033 Uiso 1 1 calc R . .
C33 C 0.7361(2) 0.5017(2) 0.4087(2) 0.0247(8) Uani 1 1 d . . .
C34 C 0.6569(2) 0.5588(2) 0.3005(2) 0.0233(8) Uani 1 1 d . . .
C35 C 0.6586(2) 0.5104(2) 0.3676(2) 0.0225(7) Uani 1 1 d . . .
C36 C 0.7327(2) 0.5955(2) 0.2754(2) 0.0271(8) Uani 1 1 d . . .
H36 H 0.7318 0.6281 0.2299 0.032 Uiso 1 1 calc R . .
C37 C 0.8902(2) 0.6289(2) 0.2858(2) 0.0275(8) Uani 1 1 d . . .
C38 C 0.8844(2) 0.6586(2) 0.20260(18) 0.0404(9) Uani 1 1 d . . .
H38A H 0.8721 0.6169 0.1727 0.061 Uiso 1 1 calc R . .
H38B H 0.9396 0.6808 0.1850 0.061 Uiso 1 1 calc R . .
H38C H 0.8379 0.6972 0.1967 0.061 Uiso 1 1 calc R . .
C39 C 0.8999(3) 0.6948(2) 0.3326(2) 0.0560(12) Uani 1 1 d . . .
H39A H 0.8487 0.7285 0.3271 0.084 Uiso 1 1 calc R . .
H39B H 0.9517 0.7226 0.3150 0.084 Uiso 1 1 calc R . .
H39C H 0.9057 0.6759 0.3858 0.084 Uiso 1 1 calc R . .
C40 C 0.9700(2) 0.5763(2) 0.2925(2) 0.0517(11) Uani 1 1 d . . .
H40A H 0.9823 0.5632 0.3459 0.078 Uiso 1 1 calc R . .
H40B H 1.0198 0.6017 0.2672 0.078 Uiso 1 1 calc R . .
H40C H 0.9592 0.5301 0.2686 0.078 Uiso 1 1 calc R . .
C41 C 0.7356(2) 0.4544(2) 0.4780(2) 0.0288(9) Uani 1 1 d . . .
C42 C 0.7291(2) 0.4156(2) 0.5364(2) 0.0329(9) Uani 1 1 d . . .
C43 C 0.7187(2) 0.3674(2) 0.6086(2) 0.0325(9) Uani 1 1 d . . .
C44 C 0.7896(2) 0.3847(3) 0.6614(2) 0.0481(11) Uani 1 1 d . . .
H44A H 0.7853 0.4382 0.6705 0.072 Uiso 1 1 calc R . .
H44B H 0.8464 0.3738 0.6382 0.072 Uiso 1 1 calc R . .
H44C H 0.7828 0.3533 0.7094 0.072 Uiso 1 1 calc R . .
C45 C 0.7182(3) 0.2852(2) 0.5939(3) 0.0550(12) Uani 1 1 d . . .
H45A H 0.7077 0.2540 0.6416 0.083 Uiso 1 1 calc R . .
H45B H 0.7744 0.2705 0.5718 0.083 Uiso 1 1 calc R . .
H45C H 0.6723 0.2776 0.5588 0.083 Uiso 1 1 calc R . .
C46 C 0.5814(2) 0.5740(2) 0.2560(2) 0.0296(8) Uani 1 1 d . . .
C47 C 0.5234(2) 0.5906(2) 0.2153(2) 0.0311(8) Uani 1 1 d . . .
C48 C 0.4461(2) 0.6089(2) 0.1690(2) 0.0380(9) Uani 1 1 d . . .
C49 C 0.4544(3) 0.5665(3) 0.0975(2) 0.0602(13) Uani 1 1 d . . .
H49A H 0.4614 0.5121 0.1120 0.090 Uiso 1 1 calc R . .
H49B H 0.5050 0.5843 0.0671 0.090 Uiso 1 1 calc R . .
H49C H 0.4021 0.5761 0.0679 0.090 Uiso 1 1 calc R . .
C50 C 0.4321(3) 0.6923(3) 0.1525(3) 0.0680(15) Uani 1 1 d . . .
H50A H 0.3817 0.7024 0.1206 0.102 Uiso 1 1 calc R . .
H50B H 0.4835 0.7139 0.1261 0.102 Uiso 1 1 calc R . .
H50C H 0.4220 0.7154 0.1999 0.102 Uiso 1 1 calc R . .
C51 C 0.4538(2) 0.4289(2) 0.4045(2) 0.0207(8) Uani 1 1 d . . .
C52 C 0.4585(2) 0.3959(2) 0.4818(2) 0.0245(8) Uani 1 1 d . . .
C53 C 0.3864(2) 0.3591(2) 0.5138(2) 0.0277(8) Uani 1 1 d . . .
H53 H 0.3879 0.3376 0.5647 0.033 Uiso 1 1 calc R . .
C54 C 0.3086(2) 0.3837(2) 0.3977(2) 0.0289(9) Uani 1 1 d . . .
H54 H 0.2581 0.3780 0.3699 0.035 Uiso 1 1 calc R . .
C55 C 0.3139(2) 0.3531(2) 0.4739(2) 0.0272(8) Uani 1 1 d . . .
C56 C 0.3766(2) 0.4209(2) 0.3655(2) 0.0245(8) Uani 1 1 d . . .
H56 H 0.3727 0.4426 0.3148 0.029 Uiso 1 1 calc R . .
O9 O 0.36960(17) 1.11657(16) -0.14433(15) 0.0389(7) Uani 1 1 d . . .
H9 H 0.4101 1.1214 -0.1149 0.058 Uiso 1 1 calc R . .
O10 O 0.61408(16) 0.90813(17) 0.29052(16) 0.0404(7) Uani 1 1 d . . .
H10 H 0.6218 0.8984 0.2455 0.061 Uiso 1 1 calc R . .
O11 O 0.47148(15) 1.09895(14) -0.01805(14) 0.0290(6) Uani 1 1 d . . .
H11 H 0.4333 1.0750 0.0080 0.043 Uiso 1 1 calc R . .
O12 O 0.75358(17) 1.18113(17) -0.00114(16) 0.0403(7) Uani 1 1 d . . .
H12 H 0.7944 1.1804 0.0291 0.060 Uiso 1 1 calc R . .
N5 N 0.40843(17) 1.02594(17) 0.09738(17) 0.0239(7) Uani 1 1 d . . .
N6 N 0.47769(18) 1.02857(17) 0.13555(18) 0.0257(7) Uani 1 1 d . . .
C61 C 0.1830(2) 0.9113(2) 0.1717(3) 0.0356(10) Uani 1 1 d . A .
C62 C 0.1859(2) 0.9626(2) 0.1085(3) 0.0338(9) Uani 1 1 d . . .
H62 H 0.1352 0.9721 0.0797 0.041 Uiso 1 1 calc R . .
C63 C 0.2606(2) 1.0006(2) 0.0856(2) 0.0262(8) Uani 1 1 d . . .
C64 C 0.3360(2) 0.9882(2) 0.1288(2) 0.0241(8) Uani 1 1 d . . .
C65 C 0.3338(2) 0.9377(2) 0.1939(2) 0.0272(8) Uani 1 1 d . . .
C66 C 0.2568(2) 0.9007(2) 0.2142(2) 0.0327(9) Uani 1 1 d . . .
H66 H 0.2550 0.8669 0.2589 0.039 Uiso 1 1 calc R . .
C67 C 0.1016(2) 0.8664(2) 0.1950(3) 0.0477(12) Uani 1 1 d D . .
C68A C 0.0417(3) 0.8652(3) 0.1203(3) 0.0454(13) Uani 0.646(4) 1 d PD A 1
H68A H 0.0768 0.8466 0.0788 0.068 Uiso 0.646(4) 1 calc PR A 1
H68B H 0.0195 0.9164 0.1051 0.068 Uiso 0.646(4) 1 calc PR A 1
H68C H -0.0070 0.8317 0.1326 0.068 Uiso 0.646(4) 1 calc PR A 1
C69A C 0.0513(4) 0.8994(4) 0.2520(4) 0.0566(16) Uani 0.646(4) 1 d PD A 1
H69A H 0.0003 0.8690 0.2652 0.085 Uiso 0.646(4) 1 calc PR A 1
H69B H 0.0328 0.9508 0.2333 0.085 Uiso 0.646(4) 1 calc PR A 1
H69C H 0.0863 0.9012 0.2969 0.085 Uiso 0.646(4) 1 calc PR A 1
C70A C 0.1283(3) 0.7841(3) 0.2110(4) 0.0528(16) Uani 0.646(4) 1 d PD A 1
H70A H 0.0766 0.7532 0.2152 0.079 Uiso 0.646(4) 1 calc PR A 1
H70B H 0.1594 0.7770 0.2585 0.079 Uiso 0.646(4) 1 calc PR A 1
H70C H 0.1662 0.7687 0.1697 0.079 Uiso 0.646(4) 1 calc PR A 1
C68B C 0.1089(6) 0.8405(6) 0.2918(4) 0.0454(13) Uani 0.354(4) 1 d PD A 2
H68D H 0.0533 0.8209 0.3118 0.068 Uiso 0.354(4) 1 calc PR A 2
H68E H 0.1231 0.8847 0.3175 0.068 Uiso 0.354(4) 1 calc PR A 2
H68F H 0.1543 0.8012 0.3005 0.068 Uiso 0.354(4) 1 calc PR A 2
C70B C 0.0225(5) 0.9211(5) 0.2023(7) 0.0528(16) Uani 0.354(4) 1 d PD A 2
H70D H 0.0009 0.9374 0.1520 0.079 Uiso 0.354(4) 1 calc PR A 2
H70E H 0.0398 0.9652 0.2266 0.079 Uiso 0.354(4) 1 calc PR A 2
H70F H -0.0233 0.8951 0.2329 0.079 Uiso 0.354(4) 1 calc PR A 2
C69B C 0.0947(7) 0.8007(6) 0.1639(6) 0.0566(16) Uani 0.354(4) 1 d PD A 2
H69D H 0.0469 0.7722 0.1889 0.085 Uiso 0.354(4) 1 calc PR A 2
H69E H 0.1489 0.7710 0.1703 0.085 Uiso 0.354(4) 1 calc PR A 2
H69F H 0.0835 0.8112 0.1100 0.085 Uiso 0.354(4) 1 calc PR A 2
C71 C 0.2643(2) 1.0502(2) 0.0176(3) 0.0317(9) Uani 1 1 d . . .
C72 C 0.2738(2) 1.0908(2) -0.0397(3) 0.0362(10) Uani 1 1 d . . .
C73 C 0.2896(3) 1.1398(2) -0.1103(2) 0.0362(9) Uani 1 1 d . . .
C74 C 0.2197(2) 1.1294(3) -0.1663(3) 0.0528(12) Uani 1 1 d . . .
H74A H 0.2311 1.1616 -0.2132 0.079 Uiso 1 1 calc R . .
H74B H 0.1631 1.1435 -0.1447 0.079 Uiso 1 1 calc R . .
H74C H 0.2197 1.0764 -0.1772 0.079 Uiso 1 1 calc R . .
C75 C 0.2953(3) 1.2211(3) -0.0929(3) 0.0503(11) Uani 1 1 d . . .
H75A H 0.3415 1.2252 -0.0570 0.075 Uiso 1 1 calc R . .
H75B H 0.2400 1.2378 -0.0708 0.075 Uiso 1 1 calc R . .
H75C H 0.3082 1.2531 -0.1396 0.075 Uiso 1 1 calc R . .
C76 C 0.4070(2) 0.9169(2) 0.2393(2) 0.0332(9) Uani 1 1 d . . .
C77 C 0.4646(2) 0.8945(3) 0.2793(2) 0.0393(10) Uani 1 1 d . . .
C78 C 0.5407(2) 0.8682(3) 0.3233(2) 0.0454(11) Uani 1 1 d . . .
C79 C 0.5573(3) 0.7835(3) 0.3182(3) 0.0766(16) Uani 1 1 d . . .
H79A H 0.5639 0.7736 0.2650 0.115 Uiso 1 1 calc R . .
H79B H 0.5083 0.7554 0.3416 0.115 Uiso 1 1 calc R . .
H79C H 0.6104 0.7672 0.3446 0.115 Uiso 1 1 calc R . .
C80 C 0.5294(3) 0.8880(3) 0.4033(2) 0.0854(19) Uani 1 1 d . . .
H80A H 0.5813 0.8718 0.4315 0.128 Uiso 1 1 calc R . .
H80B H 0.4790 0.8624 0.4272 0.128 Uiso 1 1 calc R . .
H80C H 0.5206 0.9428 0.4035 0.128 Uiso 1 1 calc R . .
C81 C 0.5438(2) 1.0668(2) 0.0978(2) 0.0197(7) Uani 1 1 d . . .
C82 C 0.5410(2) 1.1015(2) 0.0216(2) 0.0247(8) Uani 1 1 d . . .
C83 C 0.6139(2) 1.1383(2) -0.0087(2) 0.0275(8) Uani 1 1 d . . .
H83 H 0.6134 1.1611 -0.0592 0.033 Uiso 1 1 calc R . .
C84 C 0.6889(2) 1.1104(2) 0.1084(2) 0.0305(9) Uani 1 1 d . . .
H84 H 0.7386 1.1156 0.1374 0.037 Uiso 1 1 calc R . .
C85 C 0.6859(2) 1.1422(2) 0.0326(2) 0.0279(8) Uani 1 1 d . . .
C86 C 0.6201(2) 1.0729(2) 0.1388(2) 0.0263(8) Uani 1 1 d . . .
H86 H 0.6228 1.0498 0.1891 0.032 Uiso 1 1 calc R . .
O13 O 0.12387(15) 1.15113(14) 0.37981(15) 0.0350(6) Uani 1 1 d . . .
H13 H 0.0828 1.1215 0.3783 0.052 Uiso 1 1 calc R . .
O14 O -0.11591(16) 0.70680(16) 0.57743(18) 0.0423(7) Uani 1 1 d . . .
H14 H -0.1243 0.7449 0.6016 0.063 Uiso 1 1 calc R . .
O15 O 0.02088(15) 1.02199(14) 0.39671(16) 0.0335(6) Uani 1 1 d . . .
H15 H 0.0603 0.9957 0.4188 0.050 Uiso 1 1 calc R . .
O16 O -0.26213(15) 0.99970(15) 0.31775(16) 0.0364(6) Uani 1 1 d . . .
H16 H -0.3017 0.9682 0.3187 0.055 Uiso 1 1 calc R . .
N7 N 0.08688(17) 0.90667(18) 0.46747(17) 0.0264(7) Uani 1 1 d . . .
N8 N 0.01800(18) 0.86783(17) 0.46507(17) 0.0243(7) Uani 1 1 d . . .
C91 C 0.3117(2) 0.8333(2) 0.5846(2) 0.0318(9) Uani 1 1 d . . .
C92 C 0.3075(2) 0.8979(2) 0.5352(2) 0.0300(8) Uani 1 1 d . . .
H92 H 0.3567 0.9288 0.5281 0.036 Uiso 1 1 calc R . .
C93 C 0.2332(2) 0.9189(2) 0.4956(2) 0.0281(8) Uani 1 1 d . . .
C94 C 0.1590(2) 0.8754(2) 0.5056(2) 0.0254(8) Uani 1 1 d . . .
C95 C 0.1620(2) 0.8090(2) 0.5542(2) 0.0291(8) Uani 1 1 d . . .
C96 C 0.2385(2) 0.7891(2) 0.5918(2) 0.0305(8) Uani 1 1 d . . .
H96 H 0.2408 0.7432 0.6238 0.037 Uiso 1 1 calc R . .
C97 C 0.3909(2) 0.8114(2) 0.6314(2) 0.0370(9) Uani 1 1 d . . .
C98 C 0.4546(2) 0.8764(2) 0.6288(2) 0.0600(12) Uani 1 1 d . . .
H98A H 0.5010 0.8627 0.6643 0.090 Uiso 1 1 calc R . .
H98B H 0.4239 0.9222 0.6428 0.090 Uiso 1 1 calc R . .
H98C H 0.4796 0.8857 0.5776 0.090 Uiso 1 1 calc R . .
C99 C 0.3627(2) 0.7961(3) 0.7135(2) 0.0556(11) Uani 1 1 d . . .
H99A H 0.3282 0.7505 0.7200 0.083 Uiso 1 1 calc R . .
H99B H 0.3277 0.8392 0.7290 0.083 Uiso 1 1 calc R . .
H99C H 0.4140 0.7888 0.7448 0.083 Uiso 1 1 calc R . .
C100 C 0.4363(3) 0.7449(3) 0.6010(3) 0.0719(15) Uani 1 1 d . . .
H10D H 0.3997 0.7007 0.6099 0.108 Uiso 1 1 calc R . .
H10E H 0.4913 0.7346 0.6265 0.108 Uiso 1 1 calc R . .
H10F H 0.4476 0.7559 0.5466 0.108 Uiso 1 1 calc R . .
C101 C 0.2286(2) 0.9884(2) 0.4466(2) 0.0293(9) Uani 1 1 d . . .
C102 C 0.2194(2) 1.0448(2) 0.4069(2) 0.0302(8) Uani 1 1 d . . .
C103 C 0.2034(2) 1.1146(2) 0.3566(2) 0.0323(9) Uani 1 1 d . . .
C104 C 0.2731(2) 1.1709(2) 0.3655(2) 0.0432(10) Uani 1 1 d . . .
H10G H 0.2607 1.2176 0.3334 0.065 Uiso 1 1 calc R . .
H10H H 0.3295 1.1496 0.3506 0.065 Uiso 1 1 calc R . .
H10I H 0.2741 1.1820 0.4184 0.065 Uiso 1 1 calc R . .
C105 C 0.1959(3) 1.0960(2) 0.2749(2) 0.0428(10) Uani 1 1 d . . .
H10J H 0.1480 1.0616 0.2717 0.064 Uiso 1 1 calc R . .
H10K H 0.2501 1.0717 0.2584 0.064 Uiso 1 1 calc R . .
H10L H 0.1848 1.1426 0.2423 0.064 Uiso 1 1 calc R . .
C106 C 0.0901(2) 0.7598(2) 0.5694(2) 0.0296(8) Uani 1 1 d . . .
C107 C 0.0352(2) 0.7159(2) 0.5873(2) 0.0362(9) Uani 1 1 d . . .
C108 C -0.0390(2) 0.6670(2) 0.6027(2) 0.0392(9) Uani 1 1 d . . .
C109 C -0.0316(3) 0.5976(2) 0.5587(3) 0.0593(12) Uani 1 1 d . . .
H10M H -0.0832 0.5672 0.5692 0.089 Uiso 1 1 calc R . .
H10N H 0.0200 0.5674 0.5742 0.089 Uiso 1 1 calc R . .
H10O H -0.0269 0.6136 0.5045 0.089 Uiso 1 1 calc R . .
C110 C -0.0491(3) 0.6448(3) 0.6874(2) 0.0626(13) Uani 1 1 d . . .
H11A H -0.0589 0.6903 0.7138 0.094 Uiso 1 1 calc R . .
H11B H 0.0037 0.6180 0.7057 0.094 Uiso 1 1 calc R . .
H11C H -0.0986 0.6117 0.6972 0.094 Uiso 1 1 calc R . .
C111 C -0.0496(2) 0.9045(2) 0.4276(2) 0.0266(8) Uani 1 1 d . . .
C112 C -0.0484(2) 0.9814(2) 0.3945(2) 0.0256(8) Uani 1 1 d . . .
C113 C -0.1219(2) 1.0110(2) 0.3574(2) 0.0298(8) Uani 1 1 d . . .
H113 H -0.1227 1.0618 0.3352 0.036 Uiso 1 1 calc R . .
C115 C -0.1947(2) 0.8925(2) 0.3864(2) 0.0284(8) Uani 1 1 d . . .
H115 H -0.2447 0.8632 0.3836 0.034 Uiso 1 1 calc R . .
C114 C -0.1934(2) 0.9676(2) 0.3525(2) 0.0270(8) Uani 1 1 d . . .
C116 C -0.1236(2) 0.8623(2) 0.4232(2) 0.0293(9) Uani 1 1 d . . .
H116 H -0.1245 0.8118 0.4461 0.035 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0273(12) 0.0251(13) 0.0461(16) -0.0003(11) -0.0012(11) -0.0040(10)
O2 0.0266(12) 0.0259(14) 0.069(2) -0.0017(13) -0.0122(12) -0.0048(10)
O3 0.0228(11) 0.0269(14) 0.0416(16) 0.0026(11) -0.0084(11) -0.0029(10)
O4 0.0295(12) 0.0380(15) 0.0410(16) -0.0048(12) -0.0139(11) 0.0010(11)
N1 0.0217(13) 0.0309(18) 0.0232(17) -0.0047(13) -0.0035(12) -0.0018(12)
N2 0.0224(13) 0.0259(17) 0.0246(17) -0.0009(13) -0.0027(13) -0.0024(13)
C1 0.0228(15) 0.0259(17) 0.0233(18) -0.0041(13) -0.0009(13) -0.0004(13)
C2 0.0194(15) 0.0254(18) 0.0276(19) -0.0012(14) 0.0004(14) -0.0030(13)
C3 0.0265(17) 0.0236(18) 0.0225(19) 0.0001(14) -0.0012(14) 0.0000(14)
C4 0.0238(16) 0.0255(19) 0.0211(19) -0.0026(14) -0.0030(14) 0.0031(14)
C5 0.0190(15) 0.031(2) 0.026(2) -0.0028(15) 0.0020(14) -0.0057(14)
C6 0.0268(16) 0.0250(18) 0.029(2) 0.0048(14) -0.0005(15) 0.0012(14)
C7 0.080(3) 0.057(3) 0.054(3) -0.023(2) -0.045(2) 0.024(2)
C8 0.0230(15) 0.0343(19) 0.0262(18) 0.0023(14) -0.0035(14) -0.0009(14)
C9 0.0321(18) 0.037(2) 0.067(3) 0.0106(18) -0.0111(18) 0.0024(15)
C10 0.0189(15) 0.075(3) 0.053(3) 0.010(2) 0.0020(16) 0.0056(17)
C11 0.0198(15) 0.0265(19) 0.032(2) -0.0028(16) 0.0017(14) -0.0028(14)
C12 0.0261(17) 0.0231(19) 0.034(2) -0.0013(15) -0.0020(15) -0.0042(14)
C13 0.0339(18) 0.0215(18) 0.0294(19) 0.0040(14) 0.0017(15) -0.0021(14)
C14 0.0324(18) 0.029(2) 0.062(3) 0.0056(18) 0.0067(18) -0.0090(16)
C15 0.090(3) 0.038(2) 0.035(2) 0.0025(19) 0.006(2) -0.001(2)
C16 0.0207(16) 0.0270(19) 0.035(2) 0.0058(15) -0.0050(14) -0.0019(14)
C17 0.0239(16) 0.036(2) 0.045(2) 0.0111(17) -0.0029(15) -0.0002(15)
C18 0.0194(16) 0.0295(19) 0.089(4) 0.021(2) -0.0038(18) -0.0041(14)
C19 0.042(2) 0.131(5) 0.063(3) 0.058(3) 0.003(2) -0.018(3)
C20 0.035(2) 0.027(2) 0.227(8) 0.008(3) 0.008(3) -0.0009(17)
C21 0.0247(17) 0.032(2) 0.022(2) -0.0022(16) -0.0017(15) -0.0011(16)
C22 0.0230(16) 0.0272(19) 0.0219(19) -0.0048(15) -0.0032(14) -0.0053(14)
C23 0.0296(16) 0.0212(17) 0.026(2) -0.0013(14) -0.0044(14) -0.0028(14)
C24 0.0275(16) 0.0287(19) 0.0196(18) -0.0041(14) -0.0034(13) 0.0043(14)
C25 0.0224(15) 0.035(2) 0.029(2) -0.0076(16) -0.0029(14) -0.0066(15)
C26 0.0271(17) 0.029(2) 0.025(2) -0.0013(16) -0.0008(15) -0.0016(15)
O5 0.0339(13) 0.0498(16) 0.0236(14) -0.0008(11) -0.0048(11) 0.0010(11)
O6 0.0275(12) 0.0538(17) 0.0279(14) -0.0039(12) -0.0013(10) -0.0109(11)
O7 0.0267(11) 0.0357(15) 0.0234(14) 0.0032(10) -0.0073(10) -0.0069(10)
O8 0.0325(12) 0.0482(17) 0.0345(16) -0.0004(12) 0.0053(11) -0.0179(12)
N3 0.0225(13) 0.0273(16) 0.0212(16) 0.0014(12) -0.0025(12) -0.0035(12)
N4 0.0239(14) 0.0256(17) 0.0258(18) -0.0023(13) -0.0045(13) -0.0016(13)
C31 0.0180(14) 0.0226(17) 0.035(2) -0.0020(14) 0.0021(13) 0.0002(12)
C32 0.0226(16) 0.0269(19) 0.033(2) -0.0057(15) -0.0035(14) 0.0016(14)
C33 0.0210(15) 0.0281(19) 0.0249(19) -0.0033(14) -0.0025(13) 0.0040(14)
C34 0.0233(16) 0.0244(18) 0.0219(18) -0.0013(14) 0.0032(14) -0.0019(13)
C35 0.0200(15) 0.0216(17) 0.0263(19) -0.0037(14) -0.0024(14) 0.0012(13)
C36 0.0245(16) 0.0252(18) 0.031(2) 0.0011(14) -0.0011(14) -0.0012(14)
C37 0.0239(15) 0.0271(17) 0.031(2) -0.0011(14) 0.0010(14) -0.0060(13)
C38 0.0272(16) 0.054(2) 0.037(2) 0.0104(16) 0.0067(15) -0.0091(15)
C39 0.066(3) 0.051(2) 0.055(3) -0.016(2) 0.017(2) -0.029(2)
C40 0.0304(18) 0.050(2) 0.069(3) 0.025(2) 0.0053(18) -0.0044(16)
C41 0.0241(16) 0.0307(19) 0.032(2) -0.0016(16) -0.0038(15) -0.0004(14)
C42 0.0274(17) 0.038(2) 0.033(2) -0.0053(17) -0.0051(16) 0.0077(15)
C43 0.0357(18) 0.035(2) 0.027(2) -0.0039(15) -0.0050(15) 0.0077(15)
C44 0.035(2) 0.076(3) 0.033(2) -0.003(2) -0.0134(17) 0.0101(19)
C45 0.094(3) 0.036(2) 0.034(2) 0.0013(18) 0.000(2) 0.005(2)
C46 0.0268(17) 0.0301(19) 0.030(2) 0.0060(15) 0.0011(15) -0.0040(14)
C47 0.0277(16) 0.037(2) 0.0279(19) 0.0062(15) -0.0015(14) -0.0099(14)
C48 0.0281(16) 0.053(2) 0.0302(19) 0.0140(16) -0.0086(14) -0.0107(15)
C49 0.049(2) 0.102(4) 0.029(2) 0.001(2) -0.0032(17) -0.008(2)
C50 0.049(2) 0.053(3) 0.096(4) 0.031(2) -0.032(2) -0.0072(19)
C51 0.0239(16) 0.0188(18) 0.0200(19) -0.0034(14) -0.0026(14) -0.0048(13)
C52 0.0271(16) 0.0237(19) 0.0229(19) -0.0038(15) -0.0003(15) -0.0002(14)
C53 0.0321(17) 0.027(2) 0.0230(19) 0.0013(15) 0.0003(15) -0.0025(15)
C54 0.0298(17) 0.030(2) 0.027(2) -0.0043(16) -0.0042(15) -0.0071(15)
C55 0.0249(16) 0.029(2) 0.029(2) -0.0061(15) 0.0030(14) -0.0062(14)
C56 0.0268(17) 0.029(2) 0.0187(19) -0.0042(15) -0.0077(14) -0.0029(15)
O9 0.0357(13) 0.0535(17) 0.0279(14) -0.0061(12) -0.0092(11) 0.0113(12)
O10 0.0327(13) 0.0604(18) 0.0291(15) -0.0045(12) -0.0037(11) -0.0142(12)
O11 0.0261(11) 0.0354(15) 0.0249(14) 0.0032(10) -0.0061(10) -0.0074(10)
O12 0.0324(12) 0.0499(18) 0.0398(17) -0.0089(13) 0.0105(12) -0.0180(12)
N5 0.0202(13) 0.0286(17) 0.0228(16) -0.0016(12) -0.0014(12) -0.0016(12)
N6 0.0222(14) 0.0259(17) 0.0296(18) -0.0048(13) -0.0043(13) -0.0002(13)
C61 0.0217(16) 0.0240(19) 0.061(3) -0.0084(17) 0.0087(16) -0.0018(14)
C62 0.0216(16) 0.0262(19) 0.055(3) -0.0095(17) -0.0040(16) 0.0009(14)
C63 0.0207(15) 0.0276(19) 0.031(2) -0.0080(15) -0.0011(14) 0.0034(14)
C64 0.0191(15) 0.0243(18) 0.029(2) -0.0044(15) -0.0014(14) -0.0011(13)
C65 0.0269(16) 0.029(2) 0.025(2) -0.0008(15) 0.0026(15) -0.0025(15)
C66 0.0277(17) 0.0254(19) 0.044(2) 0.0008(16) 0.0066(16) -0.0028(15)
C67 0.0240(17) 0.027(2) 0.090(3) 0.007(2) 0.0074(19) -0.0053(15)
C68A 0.026(2) 0.065(3) 0.045(3) 0.004(2) -0.001(2) -0.020(2)
C69A 0.047(3) 0.061(4) 0.066(4) -0.026(3) 0.029(3) -0.027(3)
C70A 0.032(2) 0.038(3) 0.087(4) 0.012(3) -0.019(3) -0.013(2)
C68B 0.026(2) 0.065(3) 0.045(3) 0.004(2) -0.001(2) -0.020(2)
C70B 0.032(2) 0.038(3) 0.087(4) 0.012(3) -0.019(3) -0.013(2)
C69B 0.047(3) 0.061(4) 0.066(4) -0.026(3) 0.029(3) -0.027(3)
C71 0.0235(16) 0.031(2) 0.041(2) -0.0056(17) -0.0051(16) 0.0019(15)
C72 0.0297(18) 0.040(2) 0.039(2) -0.0074(18) -0.0094(17) 0.0097(16)
C73 0.0359(18) 0.042(2) 0.031(2) -0.0049(17) -0.0099(16) 0.0111(16)
C74 0.036(2) 0.082(3) 0.041(2) -0.011(2) -0.0144(18) 0.013(2)
C75 0.074(3) 0.037(2) 0.038(2) -0.0006(18) -0.004(2) 0.015(2)
C76 0.0293(18) 0.034(2) 0.035(2) 0.0030(16) 0.0041(16) -0.0090(15)
C77 0.0341(19) 0.052(2) 0.029(2) 0.0106(17) -0.0011(16) -0.0123(17)
C78 0.0394(19) 0.062(3) 0.032(2) 0.0183(19) -0.0104(16) -0.0138(18)
C79 0.061(3) 0.065(3) 0.097(4) 0.039(3) -0.035(3) -0.012(2)
C80 0.055(3) 0.172(6) 0.026(2) 0.013(3) -0.0038(19) -0.029(3)
C81 0.0173(14) 0.0187(17) 0.0231(19) -0.0013(14) -0.0036(14) -0.0018(13)
C82 0.0246(16) 0.0239(19) 0.026(2) -0.0044(15) -0.0003(14) 0.0010(14)
C83 0.0303(16) 0.0240(18) 0.028(2) -0.0016(15) 0.0001(15) -0.0019(14)
C84 0.0285(17) 0.034(2) 0.031(2) -0.0060(16) -0.0045(15) -0.0078(15)
C85 0.0244(15) 0.0238(18) 0.036(2) -0.0069(15) 0.0068(15) -0.0058(13)
C86 0.0270(17) 0.029(2) 0.024(2) -0.0040(15) -0.0081(15) -0.0047(15)
O13 0.0281(12) 0.0297(14) 0.0472(16) -0.0045(11) 0.0061(11) -0.0071(10)
O14 0.0318(13) 0.0308(15) 0.065(2) -0.0070(13) -0.0115(13) -0.0043(11)
O15 0.0292(12) 0.0264(14) 0.0439(17) 0.0026(11) -0.0026(11) -0.0038(11)
O16 0.0337(13) 0.0334(15) 0.0422(17) -0.0007(12) -0.0127(12) -0.0004(11)
N7 0.0210(13) 0.0326(18) 0.0263(17) -0.0054(13) -0.0024(12) -0.0021(12)
N8 0.0249(14) 0.0259(17) 0.0217(17) 0.0001(12) -0.0050(13) 0.0005(13)
C91 0.0207(15) 0.051(2) 0.0247(19) -0.0087(17) 0.0010(14) 0.0006(15)
C92 0.0228(15) 0.038(2) 0.030(2) -0.0054(15) 0.0012(14) -0.0029(14)
C93 0.0276(17) 0.035(2) 0.0219(19) -0.0050(15) -0.0022(14) 0.0023(15)
C94 0.0262(16) 0.0265(19) 0.0238(19) -0.0050(15) -0.0035(14) 0.0053(14)
C95 0.0262(17) 0.034(2) 0.027(2) -0.0059(16) 0.0021(15) -0.0030(15)
C96 0.0314(17) 0.034(2) 0.0250(19) 0.0006(15) -0.0017(15) 0.0047(15)
C97 0.0259(16) 0.050(2) 0.035(2) -0.0008(17) -0.0057(15) 0.0051(15)
C98 0.0348(19) 0.079(3) 0.063(3) 0.013(2) -0.0152(18) -0.0103(19)
C99 0.041(2) 0.093(3) 0.032(2) 0.003(2) -0.0138(16) -0.009(2)
C100 0.069(3) 0.079(3) 0.071(3) -0.030(3) -0.035(3) 0.047(3)
C101 0.0207(16) 0.033(2) 0.035(2) -0.0061(17) 0.0016(15) -0.0053(14)
C102 0.0244(16) 0.033(2) 0.033(2) -0.0046(16) 0.0028(15) -0.0074(15)
C103 0.0301(17) 0.0274(19) 0.039(2) -0.0027(16) 0.0085(15) -0.0078(15)
C104 0.0350(19) 0.036(2) 0.058(3) -0.0004(18) 0.0077(18) -0.0112(16)
C105 0.053(2) 0.038(2) 0.036(2) 0.0008(18) 0.0069(18) -0.0038(18)
C106 0.0293(17) 0.0283(19) 0.030(2) 0.0029(15) -0.0063(15) -0.0001(15)
C107 0.0318(18) 0.0294(19) 0.046(2) 0.0064(16) -0.0084(16) 0.0023(15)
C108 0.0363(18) 0.0328(19) 0.047(2) 0.0090(17) -0.0065(16) -0.0060(15)
C109 0.062(2) 0.030(2) 0.087(3) -0.004(2) -0.018(2) 0.0039(17)
C110 0.068(3) 0.066(3) 0.051(3) 0.017(2) -0.009(2) -0.033(2)
C111 0.0279(17) 0.027(2) 0.025(2) -0.0036(16) -0.0017(15) 0.0012(15)
C112 0.0288(17) 0.0257(19) 0.022(2) -0.0023(15) -0.0012(15) -0.0017(15)
C113 0.0337(18) 0.0229(19) 0.032(2) -0.0021(15) -0.0054(16) 0.0060(15)
C115 0.0240(16) 0.033(2) 0.029(2) -0.0047(16) -0.0029(15) -0.0061(15)
C114 0.0264(16) 0.032(2) 0.0238(19) -0.0088(15) -0.0095(14) 0.0048(14)
C116 0.0317(19) 0.030(2) 0.026(2) 0.0000(16) -0.0048(16) -0.0021(16)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C13 1.435(4) . ?
O1 H1 0.8400 . ?
O2 C18 1.428(4) . ?
O2 H2 0.8400 . ?
O3 C22 1.308(4) . ?
O3 H3 0.8400 . ?
O4 C24 1.323(4) . ?
O4 H4 0.8400 . ?
N1 N2 1.298(4) . ?
N1 C4 1.399(4) . ?
N2 C21 1.352(5) . ?
C1 C6 1.394(5) . ?
C1 C2 1.394(5) . ?
C1 C8 1.519(5) . ?
C2 C3 1.381(5) . ?
C2 H2A 0.9500 . ?
C3 C4 1.394(5) . ?
C3 C11 1.449(5) . ?
C4 C5 1.408(5) . ?
C5 C6 1.388(5) . ?
C5 C16 1.433(5) . ?
C6 H6A 0.9500 . ?
C7 C8 1.520(5) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C10 1.507(5) . ?
C8 C9 1.529(5) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.186(5) . ?
C12 C13 1.479(5) . ?
C13 C14 1.513(5) . ?
C13 C15 1.523(5) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.185(5) . ?
C17 C18 1.469(5) . ?
C18 C20 1.501(6) . ?
C18 C19 1.526(6) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C26 1.402(5) . ?
C21 C22 1.441(5) . ?
C22 C23 1.391(5) . ?
C23 C24 1.381(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.422(5) . ?
C25 C26 1.371(5) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
O5 C43 1.430(4) . ?
O5 H5 0.8400 . ?
O6 C48 1.439(4) . ?
O6 H6 0.8400 . ?
O7 C52 1.306(4) . ?
O7 H7 0.8400 . ?
O8 C55 1.365(4) . ?
O8 H8 0.8400 . ?
N3 N4 1.279(4) . ?
N3 C35 1.400(4) . ?
N4 C51 1.358(4) . ?
C31 C36 1.375(5) . ?
C31 C32 1.383(5) . ?
C31 C37 1.538(5) . ?
C32 C33 1.387(5) . ?
C32 H32 0.9500 . ?
C33 C35 1.420(5) . ?
C33 C41 1.424(5) . ?
C34 C36 1.399(5) . ?
C34 C35 1.404(5) . ?
C34 C46 1.434(5) . ?
C36 H36 0.9500 . ?
C37 C39 1.514(5) . ?
C37 C40 1.526(5) . ?
C37 C38 1.528(5) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 C42 1.194(6) . ?
C42 C43 1.482(6) . ?
C43 C45 1.510(6) . ?
C43 C44 1.521(5) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 C47 1.183(5) . ?
C47 C48 1.482(5) . ?
C48 C50 1.496(6) . ?
C48 C49 1.539(6) . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 C56 1.415(4) . ?
C51 C52 1.446(5) . ?
C52 C53 1.388(5) . ?
C53 C55 1.357(5) . ?
C53 H53 0.9500 . ?
C54 C56 1.342(5) . ?
C54 C55 1.415(6) . ?
C54 H54 0.9500 . ?
C56 H56 0.9500 . ?
O9 C73 1.427(5) . ?
O9 H9 0.8400 . ?
O10 C78 1.435(4) . ?
O10 H10 0.8400 . ?
O11 C82 1.308(4) . ?
O11 H11 0.8400 . ?
O12 C85 1.364(4) . ?
O12 H12 0.8400 . ?
N5 N6 1.289(4) . ?
N5 C64 1.397(4) . ?
N6 C81 1.367(4) . ?
C61 C62 1.380(6) . ?
C61 C66 1.385(5) . ?
C61 C67 1.535(5) . ?
C62 C63 1.386(5) . ?
C62 H62 0.9500 . ?
C63 C64 1.415(5) . ?
C63 C71 1.429(6) . ?
C64 C65 1.396(5) . ?
C65 C66 1.398(5) . ?
C65 C76 1.429(5) . ?
C66 H66 0.9500 . ?
C67 C69B 1.347(8) . ?
C67 C69A 1.419(6) . ?
C67 C70A 1.512(6) . ?
C67 C70B 1.548(8) . ?
C67 C68A 1.644(6) . ?
C67 C68B 1.747(8) . ?
C68A H68A 0.9800 . ?
C68A H68B 0.9800 . ?
C68A H68C 0.9800 . ?
C69A H69A 0.9800 . ?
C69A H69B 0.9800 . ?
C69A H69C 0.9800 . ?
C70A H70A 0.9800 . ?
C70A H70B 0.9800 . ?
C70A H70C 0.9800 . ?
C68B H68D 0.9800 . ?
C68B H68E 0.9800 . ?
C68B H68F 0.9800 . ?
C70B H70D 0.9800 . ?
C70B H70E 0.9800 . ?
C70B H70F 0.9800 . ?
C69B H69D 0.9800 . ?
C69B H69E 0.9800 . ?
C69B H69F 0.9800 . ?
C71 C72 1.198(6) . ?
C72 C73 1.478(6) . ?
C73 C75 1.514(6) . ?
C73 C74 1.519(5) . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 0.9800 . ?
C75 H75A 0.9800 . ?
C75 H75B 0.9800 . ?
C75 H75C 0.9800 . ?
C76 C77 1.192(5) . ?
C77 C78 1.472(5) . ?
C78 C80 1.503(6) . ?
C78 C79 1.531(6) . ?
C79 H79A 0.9800 . ?
C79 H79B 0.9800 . ?
C79 H79C 0.9800 . ?
C80 H80A 0.9800 . ?
C80 H80B 0.9800 . ?
C80 H80C 0.9800 . ?
C81 C86 1.418(4) . ?
C81 C82 1.437(5) . ?
C82 C83 1.388(5) . ?
C83 C85 1.359(5) . ?
C83 H83 0.9500 . ?
C84 C86 1.343(5) . ?
C84 C85 1.413(6) . ?
C84 H84 0.9500 . ?
C86 H86 0.9500 . ?
O13 C103 1.441(4) . ?
O13 H13 0.8400 . ?
O14 C108 1.426(4) . ?
O14 H14 0.8400 . ?
O15 C112 1.313(4) . ?
O15 H15 0.8400 . ?
O16 C114 1.331(4) . ?
O16 H16 0.8400 . ?
N7 N8 1.290(4) . ?
N7 C94 1.395(4) . ?
N8 C111 1.371(4) . ?
C91 C92 1.379(5) . ?
C91 C96 1.392(5) . ?
C91 C97 1.520(5) . ?
C92 C93 1.389(5) . ?
C92 H92 0.9500 . ?
C93 C94 1.399(5) . ?
C93 C101 1.444(5) . ?
C94 C95 1.397(5) . ?
C95 C96 1.396(5) . ?
C95 C106 1.438(5) . ?
C96 H96 0.9500 . ?
C97 C100 1.494(5) . ?
C97 C99 1.515(5) . ?
C97 C98 1.537(5) . ?
C98 H98A 0.9800 . ?
C98 H98B 0.9800 . ?
C98 H98C 0.9800 . ?
C99 H99A 0.9800 . ?
C99 H99B 0.9800 . ?
C99 H99C 0.9800 . ?
C100 H10D 0.9800 . ?
C100 H10E 0.9800 . ?
C100 H10F 0.9800 . ?
C101 C102 1.179(5) . ?
C102 C103 1.478(5) . ?
C103 C104 1.515(5) . ?
C103 C105 1.529(5) . ?
C104 H10G 0.9800 . ?
C104 H10H 0.9800 . ?
C104 H10I 0.9800 . ?
C105 H10J 0.9800 . ?
C105 H10K 0.9800 . ?
C105 H10L 0.9800 . ?
C106 C107 1.186(5) . ?
C107 C108 1.464(5) . ?
C108 C109 1.521(5) . ?
C108 C110 1.527(6) . ?
C109 H10M 0.9800 . ?
C109 H10N 0.9800 . ?
C109 H10O 0.9800 . ?
C110 H11A 0.9800 . ?
C110 H11B 0.9800 . ?
C110 H11C 0.9800 . ?
C111 C116 1.394(5) . ?
C111 C112 1.437(5) . ?
C112 C113 1.395(5) . ?
C113 C114 1.375(5) . ?
C113 H113 0.9500 . ?
C115 C116 1.366(5) . ?
C115 C114 1.412(6) . ?
C115 H115 0.9500 . ?
C116 H116 0.9500 . ?

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
C13 O1 H1 109.5 . . ?
C18 O2 H2 109.5 . . ?
C22 O3 H3 109.5 . . ?
C24 O4 H4 109.5 . . ?
N2 N1 C4 120.9(3) . . ?
N1 N2 C21 115.1(3) . . ?
C6 C1 C2 116.1(3) . . ?
C6 C1 C8 122.5(3) . . ?
C2 C1 C8 121.3(3) . . ?
C3 C2 C1 122.1(3) . . ?
C3 C2 H2A 119.0 . . ?
C1 C2 H2A 119.0 . . ?
C2 C3 C4 120.8(3) . . ?
C2 C3 C11 121.0(3) . . ?
C4 C3 C11 118.2(3) . . ?
C3 C4 N1 115.1(3) . . ?
C3 C4 C5 118.8(3) . . ?
N1 C4 C5 126.1(3) . . ?
C6 C5 C4 118.5(3) . . ?
C6 C5 C16 117.8(3) . . ?
C4 C5 C16 123.6(3) . . ?
C5 C6 C1 123.7(3) . . ?
C5 C6 H6A 118.1 . . ?
C1 C6 H6A 118.1 . . ?
C8 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C8 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C10 C8 C1 110.5(3) . . ?
C10 C8 C7 111.2(3) . . ?
C1 C8 C7 107.9(3) . . ?
C10 C8 C9 106.6(3) . . ?
C1 C8 C9 111.8(3) . . ?
C7 C8 C9 108.8(3) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C3 175.5(4) . . ?
C11 C12 C13 178.0(4) . . ?
O1 C13 C12 109.1(3) . . ?
O1 C13 C14 105.8(3) . . ?
C12 C13 C14 110.2(3) . . ?
O1 C13 C15 109.1(3) . . ?
C12 C13 C15 110.4(3) . . ?
C14 C13 C15 112.1(3) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 C5 172.4(4) . . ?
C16 C17 C18 175.1(4) . . ?
O2 C18 C17 109.8(3) . . ?
O2 C18 C20 105.6(4) . . ?
C17 C18 C20 110.0(4) . . ?
O2 C18 C19 108.7(3) . . ?
C17 C18 C19 110.1(4) . . ?
C20 C18 C19 112.3(4) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N2 C21 C26 115.4(3) . . ?
N2 C21 C22 125.3(3) . . ?
C26 C21 C22 119.3(3) . . ?
O3 C22 C23 120.8(3) . . ?
O3 C22 C21 120.2(3) . . ?
C23 C22 C21 119.0(3) . . ?
C24 C23 C22 120.6(3) . . ?
C24 C23 H23 119.7 . . ?
C22 C23 H23 119.7 . . ?
O4 C24 C23 118.4(4) . . ?
O4 C24 C25 120.9(3) . . ?
C23 C24 C25 120.6(3) . . ?
C26 C25 C24 119.5(3) . . ?
C26 C25 H25 120.2 . . ?
C24 C25 H25 120.2 . . ?
C25 C26 C21 121.0(4) . . ?
C25 C26 H26 119.5 . . ?
C21 C26 H26 119.5 . . ?
C43 O5 H5 109.5 . . ?
C48 O6 H6 109.5 . . ?
C52 O7 H7 109.5 . . ?
C55 O8 H8 109.5 . . ?
N4 N3 C35 120.2(3) . . ?
N3 N4 C51 115.3(3) . . ?
C36 C31 C32 118.5(3) . . ?
C36 C31 C37 121.1(3) . . ?
C32 C31 C37 120.4(3) . . ?
C31 C32 C33 121.8(3) . . ?
C31 C32 H32 119.1 . . ?
C33 C32 H32 119.1 . . ?
C32 C33 C35 119.3(3) . . ?
C32 C33 C41 122.3(3) . . ?
C35 C33 C41 118.3(3) . . ?
C36 C34 C35 118.7(3) . . ?
C36 C34 C46 117.4(3) . . ?
C35 C34 C46 124.0(3) . . ?
N3 C35 C34 126.0(3) . . ?
N3 C35 C33 114.7(3) . . ?
C34 C35 C33 119.2(3) . . ?
C31 C36 C34 122.5(3) . . ?
C31 C36 H36 118.8 . . ?
C34 C36 H36 118.8 . . ?
C39 C37 C40 110.3(3) . . ?
C39 C37 C38 109.1(3) . . ?
C40 C37 C38 106.8(3) . . ?
C39 C37 C31 108.5(3) . . ?
C40 C37 C31 110.4(3) . . ?
C38 C37 C31 111.6(3) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C37 C40 H40A 109.5 . . ?
C37 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C37 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C42 C41 C33 175.5(4) . . ?
C41 C42 C43 178.6(4) . . ?
O5 C43 C42 109.0(3) . . ?
O5 C43 C45 109.2(3) . . ?
C42 C43 C45 110.1(4) . . ?
O5 C43 C44 106.3(3) . . ?
C42 C43 C44 109.1(4) . . ?
C45 C43 C44 113.0(4) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C47 C46 C34 174.4(4) . . ?
C46 C47 C48 175.6(4) . . ?
O6 C48 C47 107.4(3) . . ?
O6 C48 C50 109.6(3) . . ?
C47 C48 C50 111.6(3) . . ?
O6 C48 C49 105.6(3) . . ?
C47 C48 C49 109.0(3) . . ?
C50 C48 C49 113.3(4) . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C48 C50 H50A 109.5 . . ?
C48 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C48 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
N4 C51 C56 116.8(3) . . ?
N4 C51 C52 125.0(3) . . ?
C56 C51 C52 118.2(3) . . ?
O7 C52 C53 121.3(3) . . ?
O7 C52 C51 120.7(3) . . ?
C53 C52 C51 118.0(3) . . ?
C55 C53 C52 121.4(4) . . ?
C55 C53 H53 119.3 . . ?
C52 C53 H53 119.3 . . ?
C56 C54 C55 118.6(3) . . ?
C56 C54 H54 120.7 . . ?
C55 C54 H54 120.7 . . ?
C53 C55 O8 117.0(4) . . ?
C53 C55 C54 121.5(3) . . ?
O8 C55 C54 121.5(3) . . ?
C54 C56 C51 122.3(3) . . ?
C54 C56 H56 118.8 . . ?
C51 C56 H56 118.8 . . ?
C73 O9 H9 109.5 . . ?
C78 O10 H10 109.5 . . ?
C82 O11 H11 109.5 . . ?
C85 O12 H12 109.5 . . ?
N6 N5 C64 120.6(3) . . ?
N5 N6 C81 114.6(3) . . ?
C62 C61 C66 117.8(4) . . ?
C62 C61 C67 121.9(4) . . ?
C66 C61 C67 120.2(4) . . ?
C61 C62 C63 121.9(4) . . ?
C61 C62 H62 119.0 . . ?
C63 C62 H62 119.0 . . ?
C62 C63 C64 119.6(4) . . ?
C62 C63 C71 121.4(3) . . ?
C64 C63 C71 119.0(3) . . ?
C65 C64 N5 126.4(3) . . ?
C65 C64 C63 119.3(3) . . ?
N5 C64 C63 114.2(3) . . ?
C64 C65 C66 118.7(4) . . ?
C64 C65 C76 124.4(3) . . ?
C66 C65 C76 116.8(4) . . ?
C61 C66 C65 122.6(4) . . ?
C61 C66 H66 118.7 . . ?
C65 C66 H66 118.7 . . ?
C69A C67 C70A 116.8(5) . . ?
C69B C67 C61 115.8(5) . . ?
C69A C67 C61 112.2(4) . . ?
C70A C67 C61 108.3(3) . . ?
C69B C67 C70B 121.3(6) . . ?
C61 C67 C70B 110.1(4) . . ?
C69A C67 C68A 108.3(4) . . ?
C70A C67 C68A 102.2(4) . . ?
C61 C67 C68A 108.4(3) . . ?
C69B C67 C68B 104.8(6) . . ?
C61 C67 C68B 106.0(4) . . ?
C70B C67 C68B 95.3(5) . . ?
C67 C68A H68A 109.5 . . ?
C67 C68A H68B 109.5 . . ?
C67 C68A H68C 109.5 . . ?
C67 C69A H69A 109.5 . . ?
C67 C69A H69B 109.5 . . ?
C67 C69A H69C 109.5 . . ?
C67 C70A H70A 109.5 . . ?
C67 C70A H70B 109.5 . . ?
C67 C70A H70C 109.5 . . ?
C67 C68B H68D 109.5 . . ?
C67 C68B H68E 109.5 . . ?
H68D C68B H68E 109.5 . . ?
C67 C68B H68F 109.5 . . ?
H68D C68B H68F 109.5 . . ?
H68E C68B H68F 109.5 . . ?
C67 C70B H70D 109.5 . . ?
C67 C70B H70E 109.5 . . ?
H70D C70B H70E 109.5 . . ?
C67 C70B H70F 109.5 . . ?
H70D C70B H70F 109.5 . . ?
H70E C70B H70F 109.5 . . ?
C67 C69B H69D 109.5 . . ?
C67 C69B H69E 109.5 . . ?
H69D C69B H69E 109.5 . . ?
C67 C69B H69F 109.5 . . ?
H69D C69B H69F 109.5 . . ?
H69E C69B H69F 109.5 . . ?
C72 C71 C63 175.2(4) . . ?
C71 C72 C73 177.5(4) . . ?
O9 C73 C72 108.8(3) . . ?
O9 C73 C75 109.1(3) . . ?
C72 C73 C75 109.8(4) . . ?
O9 C73 C74 106.5(3) . . ?
C72 C73 C74 110.1(4) . . ?
C75 C73 C74 112.3(4) . . ?
C73 C74 H74A 109.5 . . ?
C73 C74 H74B 109.5 . . ?
H74A C74 H74B 109.5 . . ?
C73 C74 H74C 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
C73 C75 H75A 109.5 . . ?
C73 C75 H75B 109.5 . . ?
H75A C75 H75B 109.5 . . ?
C73 C75 H75C 109.5 . . ?
H75A C75 H75C 109.5 . . ?
H75B C75 H75C 109.5 . . ?
C77 C76 C65 174.8(4) . . ?
C76 C77 C78 175.3(4) . . ?
O10 C78 C77 107.6(3) . . ?
O10 C78 C80 107.3(3) . . ?
C77 C78 C80 110.3(4) . . ?
O10 C78 C79 108.6(4) . . ?
C77 C78 C79 110.0(3) . . ?
C80 C78 C79 112.8(4) . . ?
C78 C79 H79A 109.5 . . ?
C78 C79 H79B 109.5 . . ?
H79A C79 H79B 109.5 . . ?
C78 C79 H79C 109.5 . . ?
H79A C79 H79C 109.5 . . ?
H79B C79 H79C 109.5 . . ?
C78 C80 H80A 109.5 . . ?
C78 C80 H80B 109.5 . . ?
H80A C80 H80B 109.5 . . ?
C78 C80 H80C 109.5 . . ?
H80A C80 H80C 109.5 . . ?
H80B C80 H80C 109.5 . . ?
N6 C81 C86 116.2(3) . . ?
N6 C81 C82 125.3(3) . . ?
C86 C81 C82 118.5(3) . . ?
O11 C82 C83 120.8(3) . . ?
O11 C82 C81 120.9(3) . . ?
C83 C82 C81 118.3(3) . . ?
C85 C83 C82 121.1(4) . . ?
C85 C83 H83 119.5 . . ?
C82 C83 H83 119.5 . . ?
C86 C84 C85 118.9(3) . . ?
C86 C84 H84 120.6 . . ?
C85 C84 H84 120.6 . . ?
C83 C85 O12 117.0(4) . . ?
C83 C85 C84 121.4(3) . . ?
O12 C85 C84 121.5(3) . . ?
C84 C86 C81 121.8(4) . . ?
C84 C86 H86 119.1 . . ?
C81 C86 H86 119.1 . . ?
C103 O13 H13 109.5 . . ?
C108 O14 H14 109.5 . . ?
C112 O15 H15 109.5 . . ?
C114 O16 H16 109.5 . . ?
N8 N7 C94 120.1(3) . . ?
N7 N8 C111 115.3(3) . . ?
C92 C91 C96 116.9(3) . . ?
C92 C91 C97 122.4(3) . . ?
C96 C91 C97 120.7(4) . . ?
C91 C92 C93 121.7(4) . . ?
C91 C92 H92 119.2 . . ?
C93 C92 H92 119.2 . . ?
C92 C93 C94 120.7(3) . . ?
C92 C93 C101 120.9(3) . . ?
C94 C93 C101 118.2(3) . . ?
N7 C94 C95 126.6(4) . . ?
N7 C94 C93 114.5(3) . . ?
C95 C94 C93 118.7(3) . . ?
C96 C95 C94 118.7(4) . . ?
C96 C95 C106 117.3(4) . . ?
C94 C95 C106 124.0(4) . . ?
C91 C96 C95 123.2(4) . . ?
C91 C96 H96 118.4 . . ?
C95 C96 H96 118.4 . . ?
C100 C97 C99 112.8(4) . . ?
C100 C97 C91 109.0(3) . . ?
C99 C97 C91 109.0(3) . . ?
C100 C97 C98 108.6(3) . . ?
C99 C97 C98 105.6(3) . . ?
C91 C97 C98 111.7(3) . . ?
C97 C98 H98A 109.5 . . ?
C97 C98 H98B 109.5 . . ?
H98A C98 H98B 109.5 . . ?
C97 C98 H98C 109.5 . . ?
H98A C98 H98C 109.5 . . ?
H98B C98 H98C 109.5 . . ?
C97 C99 H99A 109.5 . . ?
C97 C99 H99B 109.5 . . ?
H99A C99 H99B 109.5 . . ?
C97 C99 H99C 109.5 . . ?
H99A C99 H99C 109.5 . . ?
H99B C99 H99C 109.5 . . ?
C97 C100 H10D 109.5 . . ?
C97 C100 H10E 109.5 . . ?
H10D C100 H10E 109.5 . . ?
C97 C100 H10F 109.5 . . ?
H10D C100 H10F 109.5 . . ?
H10E C100 H10F 109.5 . . ?
C102 C101 C93 175.8(4) . . ?
C101 C102 C103 177.2(4) . . ?
O13 C103 C102 109.6(3) . . ?
O13 C103 C104 105.0(3) . . ?
C102 C103 C104 110.1(3) . . ?
O13 C103 C105 108.9(3) . . ?
C102 C103 C105 110.4(3) . . ?
C104 C103 C105 112.7(3) . . ?
C103 C104 H10G 109.5 . . ?
C103 C104 H10H 109.5 . . ?
H10G C104 H10H 109.5 . . ?
C103 C104 H10I 109.5 . . ?
H10G C104 H10I 109.5 . . ?
H10H C104 H10I 109.5 . . ?
C103 C105 H10J 109.5 . . ?
C103 C105 H10K 109.5 . . ?
H10J C105 H10K 109.5 . . ?
C103 C105 H10L 109.5 . . ?
H10J C105 H10L 109.5 . . ?
H10K C105 H10L 109.5 . . ?
C107 C106 C95 173.8(4) . . ?
C106 C107 C108 173.1(4) . . ?
O14 C108 C107 109.3(3) . . ?
O14 C108 C109 105.7(3) . . ?
C107 C108 C109 111.8(4) . . ?
O14 C108 C110 108.6(3) . . ?
C107 C108 C110 110.0(3) . . ?
C109 C108 C110 111.3(3) . . ?
C108 C109 H10M 109.5 . . ?
C108 C109 H10N 109.5 . . ?
H10M C109 H10N 109.5 . . ?
C108 C109 H10O 109.5 . . ?
H10M C109 H10O 109.5 . . ?
H10N C109 H10O 109.5 . . ?
C108 C110 H11A 109.5 . . ?
C108 C110 H11B 109.5 . . ?
H11A C110 H11B 109.5 . . ?
C108 C110 H11C 109.5 . . ?
H11A C110 H11C 109.5 . . ?
H11B C110 H11C 109.5 . . ?
N8 C111 C116 115.6(3) . . ?
N8 C111 C112 124.5(3) . . ?
C116 C111 C112 119.9(3) . . ?
O15 C112 C113 120.8(3) . . ?
O15 C112 C111 121.1(3) . . ?
C113 C112 C111 118.1(3) . . ?
C114 C113 C112 120.8(4) . . ?
C114 C113 H113 119.6 . . ?
C112 C113 H113 119.6 . . ?
C116 C115 C114 119.6(3) . . ?
C116 C115 H115 120.2 . . ?
C114 C115 H115 120.2 . . ?
O16 C114 C113 117.9(4) . . ?
O16 C114 C115 121.4(3) . . ?
C113 C114 C115 120.7(3) . . ?
C115 C116 C111 120.9(4) . . ?
C115 C116 H116 119.6 . . ?
C111 C116 H116 119.6 . . ?

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
C4 N1 N2 C21 179.5(3) . . . . ?
C6 C1 C2 C3 2.1(6) . . . . ?
C8 C1 C2 C3 178.2(3) . . . . ?
C1 C2 C3 C4 -1.7(6) . . . . ?
C1 C2 C3 C11 -179.0(4) . . . . ?
C2 C3 C4 N1 -178.0(3) . . . . ?
C11 C3 C4 N1 -0.6(5) . . . . ?
C2 C3 C4 C5 -0.1(6) . . . . ?
C11 C3 C4 C5 177.3(4) . . . . ?
N2 N1 C4 C3 -166.2(3) . . . . ?
N2 N1 C4 C5 16.1(6) . . . . ?
C3 C4 C5 C6 1.3(6) . . . . ?
N1 C4 C5 C6 179.0(3) . . . . ?
C3 C4 C5 C16 -176.0(4) . . . . ?
N1 C4 C5 C16 1.6(7) . . . . ?
C4 C5 C6 C1 -0.9(6) . . . . ?
C16 C5 C6 C1 176.6(4) . . . . ?
C2 C1 C6 C5 -0.9(6) . . . . ?
C8 C1 C6 C5 -176.9(4) . . . . ?
C6 C1 C8 C10 -136.2(4) . . . . ?
C2 C1 C8 C10 48.0(5) . . . . ?
C6 C1 C8 C7 102.0(4) . . . . ?
C2 C1 C8 C7 -73.9(5) . . . . ?
C6 C1 C8 C9 -17.6(5) . . . . ?
C2 C1 C8 C9 166.6(4) . . . . ?
N1 N2 C21 C26 -179.3(3) . . . . ?
N1 N2 C21 C22 -0.2(6) . . . . ?
N2 C21 C22 O3 -0.9(6) . . . . ?
C26 C21 C22 O3 178.3(3) . . . . ?
N2 C21 C22 C23 -179.7(4) . . . . ?
C26 C21 C22 C23 -0.6(6) . . . . ?
O3 C22 C23 C24 -177.0(3) . . . . ?
C21 C22 C23 C24 1.9(6) . . . . ?
C22 C23 C24 O4 -178.6(3) . . . . ?
C22 C23 C24 C25 -2.2(6) . . . . ?
O4 C24 C25 C26 177.5(3) . . . . ?
C23 C24 C25 C26 1.1(6) . . . . ?
C24 C25 C26 C21 0.1(6) . . . . ?
N2 C21 C26 C25 178.8(4) . . . . ?
C22 C21 C26 C25 -0.4(6) . . . . ?
C35 N3 N4 C51 -178.4(3) . . . . ?
C36 C31 C32 C33 0.5(6) . . . . ?
C37 C31 C32 C33 178.4(3) . . . . ?
C31 C32 C33 C35 0.7(6) . . . . ?
C31 C32 C33 C41 -178.8(4) . . . . ?
N4 N3 C35 C34 12.5(6) . . . . ?
N4 N3 C35 C33 -170.9(3) . . . . ?
C36 C34 C35 N3 178.1(3) . . . . ?
C46 C34 C35 N3 -1.0(7) . . . . ?
C36 C34 C35 C33 1.6(6) . . . . ?
C46 C34 C35 C33 -177.5(4) . . . . ?
C32 C33 C35 N3 -178.7(3) . . . . ?
C41 C33 C35 N3 0.9(5) . . . . ?
C32 C33 C35 C34 -1.8(6) . . . . ?
C41 C33 C35 C34 177.8(4) . . . . ?
C32 C31 C36 C34 -0.8(6) . . . . ?
C37 C31 C36 C34 -178.7(3) . . . . ?
C35 C34 C36 C31 -0.3(6) . . . . ?
C46 C34 C36 C31 178.8(4) . . . . ?
C36 C31 C37 C39 102.0(4) . . . . ?
C32 C31 C37 C39 -75.9(5) . . . . ?
C36 C31 C37 C40 -137.0(4) . . . . ?
C32 C31 C37 C40 45.2(5) . . . . ?
C36 C31 C37 C38 -18.3(5) . . . . ?
C32 C31 C37 C38 163.9(4) . . . . ?
N3 N4 C51 C56 -178.2(3) . . . . ?
N3 N4 C51 C52 0.9(6) . . . . ?
N4 C51 C52 O7 0.0(6) . . . . ?
C56 C51 C52 O7 179.2(3) . . . . ?
N4 C51 C52 C53 180.0(4) . . . . ?
C56 C51 C52 C53 -0.9(5) . . . . ?
O7 C52 C53 C55 -179.2(3) . . . . ?
C51 C52 C53 C55 0.8(6) . . . . ?
C52 C53 C55 O8 178.1(4) . . . . ?
C52 C53 C55 C54 0.4(6) . . . . ?
C56 C54 C55 C53 -1.7(6) . . . . ?
C56 C54 C55 O8 -179.3(3) . . . . ?
C55 C54 C56 C51 1.6(6) . . . . ?
N4 C51 C56 C54 178.9(4) . . . . ?
C52 C51 C56 C54 -0.3(6) . . . . ?
C64 N5 N6 C81 179.6(3) . . . . ?
C66 C61 C62 C63 2.4(7) . . . . ?
C67 C61 C62 C63 -177.0(4) . . . . ?
C61 C62 C63 C64 -1.4(7) . . . . ?
C61 C62 C63 C71 176.3(4) . . . . ?
N6 N5 C64 C65 -14.4(6) . . . . ?
N6 N5 C64 C63 170.1(3) . . . . ?
C62 C63 C64 C65 0.1(6) . . . . ?
C71 C63 C64 C65 -177.6(4) . . . . ?
C62 C63 C64 N5 176.0(3) . . . . ?
C71 C63 C64 N5 -1.8(6) . . . . ?
N5 C64 C65 C66 -175.3(4) . . . . ?
C63 C64 C65 C66 0.1(6) . . . . ?
N5 C64 C65 C76 0.5(7) . . . . ?
C63 C64 C65 C76 175.8(4) . . . . ?
C62 C61 C66 C65 -2.2(7) . . . . ?
C67 C61 C66 C65 177.2(4) . . . . ?
C64 C65 C66 C61 1.0(7) . . . . ?
C76 C65 C66 C61 -175.0(4) . . . . ?
C62 C61 C67 C69B 87.7(8) . . . . ?
C66 C61 C67 C69B -91.7(8) . . . . ?
C62 C61 C67 C69A -98.2(6) . . . . ?
C66 C61 C67 C69A 82.4(6) . . . . ?
C62 C61 C67 C70A 131.4(5) . . . . ?
C66 C61 C67 C70A -48.0(6) . . . . ?
C62 C61 C67 C70B -54.5(7) . . . . ?
C66 C61 C67 C70B 126.0(6) . . . . ?
C62 C61 C67 C68A 21.2(6) . . . . ?
C66 C61 C67 C68A -158.2(4) . . . . ?
C62 C61 C67 C68B -156.5(5) . . . . ?
C66 C61 C67 C68B 24.1(6) . . . . ?
N5 N6 C81 C86 178.2(3) . . . . ?
N5 N6 C81 C82 -0.9(6) . . . . ?
N6 C81 C82 O11 0.5(6) . . . . ?
C86 C81 C82 O11 -178.5(3) . . . . ?
N6 C81 C82 C83 -179.9(4) . . . . ?
C86 C81 C82 C83 1.0(5) . . . . ?
O11 C82 C83 C85 179.0(3) . . . . ?
C81 C82 C83 C85 -0.6(6) . . . . ?
C82 C83 C85 O12 -178.3(3) . . . . ?
C82 C83 C85 C84 -1.4(6) . . . . ?
C86 C84 C85 C83 3.0(6) . . . . ?
C86 C84 C85 O12 179.7(4) . . . . ?
C85 C84 C86 C81 -2.5(6) . . . . ?
N6 C81 C86 C84 -178.6(4) . . . . ?
C82 C81 C86 C84 0.5(6) . . . . ?
C94 N7 N8 C111 178.6(3) . . . . ?
C96 C91 C92 C93 1.3(6) . . . . ?
C97 C91 C92 C93 -177.0(4) . . . . ?
C91 C92 C93 C94 1.1(7) . . . . ?
C91 C92 C93 C101 177.3(4) . . . . ?
N8 N7 C94 C95 -11.7(6) . . . . ?
N8 N7 C94 C93 171.8(3) . . . . ?
C92 C93 C94 N7 174.5(3) . . . . ?
C101 C93 C94 N7 -1.8(5) . . . . ?
C92 C93 C94 C95 -2.3(6) . . . . ?
C101 C93 C94 C95 -178.5(4) . . . . ?
N7 C94 C95 C96 -175.4(4) . . . . ?
C93 C94 C95 C96 1.0(6) . . . . ?
N7 C94 C95 C106 3.3(7) . . . . ?
C93 C94 C95 C106 179.7(4) . . . . ?
C92 C91 C96 C95 -2.7(6) . . . . ?
C97 C91 C96 C95 175.6(4) . . . . ?
C94 C95 C96 C91 1.6(6) . . . . ?
C106 C95 C96 C91 -177.2(4) . . . . ?
C92 C91 C97 C100 -108.4(5) . . . . ?
C96 C91 C97 C100 73.4(5) . . . . ?
C92 C91 C97 C99 128.0(4) . . . . ?
C96 C91 C97 C99 -50.2(5) . . . . ?
C92 C91 C97 C98 11.7(6) . . . . ?
C96 C91 C97 C98 -166.6(4) . . . . ?
N7 N8 C111 C116 178.5(3) . . . . ?
N7 N8 C111 C112 -2.0(6) . . . . ?
N8 C111 C112 O15 1.8(6) . . . . ?
C116 C111 C112 O15 -178.8(3) . . . . ?
N8 C111 C112 C113 179.4(4) . . . . ?
C116 C111 C112 C113 -1.2(6) . . . . ?
O15 C112 C113 C114 177.4(3) . . . . ?
C111 C112 C113 C114 -0.2(6) . . . . ?
C112 C113 C114 O16 178.6(3) . . . . ?
C112 C113 C114 C115 1.4(6) . . . . ?
C116 C115 C114 O16 -178.3(4) . . . . ?
C116 C115 C114 C113 -1.3(6) . . . . ?
C114 C115 C116 C111 -0.1(6) . . . . ?
N8 C111 C116 C115 -179.2(4) . . . . ?
C112 C111 C116 C115 1.3(6) . . . . ?

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
O1 H1 O3 0.84 1.98 2.759(3) 154.8 .
O2 H2 O1 0.84 1.84 2.683(4) 176.3 2_767
O3 H3 N1 0.84 1.76 2.495(4) 145.5 .
O3 H3 N2 0.84 2.43 2.880(4) 114.4 .
O4 H4 O6 0.84 1.82 2.646(3) 166.6 1_656
O5 H5 O7 0.84 2.05 2.821(3) 152.2 .
O6 H6 O5 0.84 1.88 2.699(4) 165.4 2_666
O7 H7 N3 0.84 1.78 2.511(4) 144.7 .
O7 H7 N4 0.84 2.44 2.891(4) 114.3 .
O8 H8 O14 0.84 1.82 2.648(4) 169.2 2_566
O9 H9 O11 0.84 1.99 2.770(3) 153.5 .
O10 H10 O9 0.84 1.84 2.682(4) 174.7 2_675
O11 H11 N5 0.84 1.78 2.510(4) 144.7 .
O11 H11 N6 0.84 2.45 2.898(4) 114.2 .
O12 H12 O2 0.84 1.83 2.645(4) 161.6 2_776
O13 H13 O15 0.84 2.03 2.821(3) 156.4 .
O14 H14 O13 0.84 1.91 2.705(4) 157.4 2_576
O15 H15 N7 0.84 1.77 2.508(4) 144.8 .
O15 H15 N8 0.84 2.44 2.892(4) 114.2 .
O16 H16 O10 0.84 1.82 2.634(4) 162.9 1_455

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        28.28
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.051