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

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Dr C Aakeroy'
_publ_contact_author_address     
;
Department of Chemistry
Kansas State University
Manhattan
Kansas
66506-3701
UNITED STATES OF AMERICA
;

_publ_contact_author_email       AAKEROY@KSU.EDU

_publ_section_title              
;
Supramolecular Reagents: Versatile Tools for
Non-covalent Synthesis
;
loop_
_publ_author_name
'C. Aakeroy'
'John Desper'
'Joaquin F. Urbina'

data_1
_database_code_depnum_ccdc_archive 'CCDC 259793'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
N-[(3-pyridyl)methyl]benzimidazole, 4-NO2-PhCOOH, 3,5-di(NO2)-PhCOOH
;
_chemical_name_common            
;N-((3-pyridyl)methyl)benzimidazole, 4-NO2-PhCOOH, 3,5-di(NO2)-
PhCOOH
;
_chemical_melting_point          ?
_chemical_formula_moiety         
;
(C13 H11 N3) (C7 H5 N O4) (C7 H4 N2 O6)
;
_chemical_formula_sum            'C27 H20 N6 O10'
_chemical_formula_weight         588.49

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

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   7.7602(11)
_cell_length_b                   15.269(2)
_cell_length_c                   22.456(3)
_cell_angle_alpha                82.064(3)
_cell_angle_beta                 81.610(3)
_cell_angle_gamma                78.915(3)
_cell_volume                     2566.7(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5297
_cell_measurement_theta_min      2.15
_cell_measurement_theta_max      28.50

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1216
_exptl_absorpt_coefficient_mu    0.119
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            30029
_diffrn_reflns_av_R_equivalents  0.0932
_diffrn_reflns_av_sigmaI/netI    0.1166
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.56
_diffrn_reflns_theta_max         30.14
_reflns_number_total             14779
_reflns_number_gt                9331
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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^)+(0.0010P)^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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         14779
_refine_ls_number_parameters     796
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_gt           0.0544
_refine_ls_wR_factor_ref         0.1090
_refine_ls_wR_factor_gt          0.0980
_refine_ls_goodness_of_fit_ref   0.886
_refine_ls_restrained_S_all      0.886
_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
N11 N 0.15874(18) 0.69848(9) 0.29160(6) 0.0166(3) Uani 1 1 d . . .
C12 C 0.1339(2) 0.78792(11) 0.29557(7) 0.0192(4) Uani 1 1 d . . .
H12 H 0.0788 0.8322 0.2670 0.023 Uiso 1 1 calc R . .
N13 N 0.19430(18) 0.80695(9) 0.34333(6) 0.0191(3) Uani 1 1 d . . .
C14 C 0.2624(2) 0.72459(11) 0.37331(7) 0.0174(3) Uani 1 1 d . . .
C15 C 0.3407(2) 0.70486(12) 0.42664(7) 0.0217(4) Uani 1 1 d . . .
H15 H 0.3559 0.7511 0.4486 0.026 Uiso 1 1 calc R . .
C16 C 0.3952(2) 0.61581(12) 0.44622(8) 0.0236(4) Uani 1 1 d . . .
H16 H 0.4493 0.6004 0.4825 0.028 Uiso 1 1 calc R . .
C17 C 0.3730(2) 0.54717(12) 0.41410(7) 0.0232(4) Uani 1 1 d . . .
H17 H 0.4122 0.4864 0.4292 0.028 Uiso 1 1 calc R . .
C18 C 0.2957(2) 0.56545(11) 0.36109(7) 0.0186(4) Uani 1 1 d . . .
H18 H 0.2805 0.5189 0.3393 0.022 Uiso 1 1 calc R . .
C19 C 0.2414(2) 0.65565(11) 0.34130(7) 0.0158(3) Uani 1 1 d . . .
N21 N 0.34158(19) 0.56704(9) 0.10278(6) 0.0211(3) Uani 1 1 d . . .
C22 C 0.2497(2) 0.57482(11) 0.15769(7) 0.0182(3) Uani 1 1 d . . .
H22 H 0.2034 0.5242 0.1785 0.022 Uiso 1 1 calc R . .
C23 C 0.2183(2) 0.65268(11) 0.18597(7) 0.0163(3) Uani 1 1 d . . .
C24 C 0.2873(2) 0.72609(11) 0.15526(7) 0.0200(4) Uani 1 1 d . . .
H24 H 0.2709 0.7804 0.1732 0.024 Uiso 1 1 calc R . .
C25 C 0.3806(2) 0.71901(12) 0.09792(7) 0.0222(4) Uani 1 1 d . . .
H25 H 0.4279 0.7686 0.0759 0.027 Uiso 1 1 calc R . .
C26 C 0.4035(2) 0.63890(11) 0.07334(8) 0.0223(4) Uani 1 1 d . . .
H26 H 0.4660 0.6348 0.0339 0.027 Uiso 1 1 calc R . .
C27 C 0.0996(2) 0.65551(11) 0.24566(7) 0.0174(3) Uani 1 1 d . . .
H27A H -0.0197 0.6877 0.2377 0.021 Uiso 1 1 calc R . .
H27B H 0.0884 0.5932 0.2625 0.021 Uiso 1 1 calc R . .
C31 C 0.2370(2) 1.11412(11) 0.33734(7) 0.0161(3) Uani 1 1 d . . .
C32 C 0.1951(2) 1.18993(11) 0.29672(7) 0.0171(3) Uani 1 1 d . . .
H32 H 0.1372 1.1870 0.2628 0.020 Uiso 1 1 calc R . .
C33 C 0.2391(2) 1.26955(11) 0.30652(7) 0.0162(3) Uani 1 1 d . . .
N33 N 0.19005(18) 1.35094(9) 0.26479(6) 0.0198(3) Uani 1 1 d . . .
O33 O 0.10634(16) 1.34565(8) 0.22359(5) 0.0261(3) Uani 1 1 d . . .
O34 O 0.23390(17) 1.42069(8) 0.27415(5) 0.0269(3) Uani 1 1 d . . .
C34 C 0.3248(2) 1.27719(11) 0.35481(7) 0.0182(3) Uani 1 1 d . . .
H34 H 0.3546 1.3326 0.3607 0.022 Uiso 1 1 calc R . .
C35 C 0.3649(2) 1.20083(11) 0.39399(7) 0.0171(3) Uani 1 1 d . . .
N35 N 0.45960(19) 1.20707(10) 0.44525(6) 0.0220(3) Uani 1 1 d . . .
O35 O 0.50262(17) 1.27911(9) 0.44864(5) 0.0308(3) Uani 1 1 d . . .
O36 O 0.48976(16) 1.13983(9) 0.48154(5) 0.0275(3) Uani 1 1 d . . .
C36 C 0.3215(2) 1.11937(11) 0.38716(7) 0.0172(3) Uani 1 1 d . . .
H36 H 0.3486 1.0682 0.4157 0.021 Uiso 1 1 calc R . .
C37 C 0.1920(2) 1.02689(11) 0.32583(7) 0.0182(3) Uani 1 1 d . . .
O31 O 0.23222(16) 0.96137(8) 0.36821(5) 0.0222(3) Uani 1 1 d . . .
H31 H 0.205(2) 0.9025(13) 0.3579(8) 0.027 Uiso 1 1 d . . .
O32 O 0.12585(16) 1.02120(8) 0.28095(5) 0.0241(3) Uani 1 1 d . . .
C41 C 0.4166(2) 0.25012(11) 0.10827(7) 0.0178(3) Uani 1 1 d . A .
C42 C 0.3579(2) 0.23152(11) 0.05640(7) 0.0207(4) Uani 1 1 d . . .
H42 H 0.3238 0.2791 0.0261 0.025 Uiso 1 1 calc R . .
C43 C 0.3491(2) 0.14389(11) 0.04877(8) 0.0216(4) Uani 1 1 d . A .
H43 H 0.3111 0.1304 0.0133 0.026 Uiso 1 1 calc R . .
C44 C 0.3971(2) 0.07715(11) 0.09416(7) 0.0194(4) Uani 1 1 d . . .
N44A N 0.3910(2) -0.01651(10) 0.08674(7) 0.0262(3) Uani 0.635(13) 1 d PD A 1
O43A O 0.4178(17) -0.0731(3) 0.1284(2) 0.096(3) Uani 0.635(13) 1 d PD A 1
O44A O 0.3514(10) -0.03285(18) 0.0392(2) 0.0375(13) Uani 0.635(13) 1 d PD A 1
N44B N 0.3910(2) -0.01651(10) 0.08674(7) 0.0262(3) Uani 0.365(13) 1 d PD A 2
O43B O 0.4954(5) -0.0762(4) 0.1120(3) 0.0199(15) Uiso 0.365(13) 1 d PD A 2
O44B O 0.2889(8) -0.0313(4) 0.0562(3) 0.0263(14) Uiso 0.365(13) 1 d PD A 2
C45 C 0.4528(2) 0.09374(12) 0.14658(7) 0.0248(4) Uani 1 1 d . A .
H45 H 0.4830 0.0462 0.1774 0.030 Uiso 1 1 calc R . .
C46 C 0.4635(2) 0.18106(12) 0.15306(7) 0.0214(4) Uani 1 1 d . . .
H46 H 0.5032 0.1939 0.1884 0.026 Uiso 1 1 calc R A .
C47 C 0.4289(2) 0.34427(11) 0.11703(8) 0.0197(4) Uani 1 1 d . . .
O41 O 0.37473(16) 0.40486(8) 0.07314(5) 0.0246(3) Uani 1 1 d . A .
H41 H 0.371(2) 0.4678(13) 0.0840(8) 0.030 Uiso 1 1 d . . .
O42 O 0.48513(16) 0.36116(8) 0.16156(5) 0.0250(3) Uani 1 1 d . A .
N51 N 0.30604(18) 0.55384(9) 0.72141(6) 0.0177(3) Uani 1 1 d . . .
C52 C 0.3009(2) 0.64317(11) 0.71973(7) 0.0193(4) Uani 1 1 d . . .
H52 H 0.3467 0.6693 0.7487 0.023 Uiso 1 1 calc R . .
N53 N 0.22564(18) 0.69000(9) 0.67360(6) 0.0188(3) Uani 1 1 d . . .
C54 C 0.1771(2) 0.62742(11) 0.64251(7) 0.0177(3) Uani 1 1 d . . .
C55 C 0.0974(2) 0.63942(12) 0.58959(7) 0.0220(4) Uani 1 1 d . . .
H55 H 0.0650 0.6975 0.5687 0.026 Uiso 1 1 calc R . .
C56 C 0.0676(2) 0.56371(12) 0.56887(8) 0.0243(4) Uani 1 1 d . . .
H56 H 0.0115 0.5699 0.5333 0.029 Uiso 1 1 calc R . .
C57 C 0.1177(2) 0.47765(12) 0.59883(8) 0.0242(4) Uani 1 1 d . . .
H57 H 0.0954 0.4271 0.5828 0.029 Uiso 1 1 calc R . .
C58 C 0.1984(2) 0.46438(11) 0.65096(7) 0.0208(4) Uani 1 1 d . . .
H58 H 0.2332 0.4061 0.6711 0.025 Uiso 1 1 calc R . .
C59 C 0.2261(2) 0.54162(11) 0.67241(7) 0.0177(3) Uani 1 1 d . . .
N61 N 0.15695(19) 0.33963(9) 0.88801(6) 0.0211(3) Uani 1 1 d . . .
C62 C 0.2515(2) 0.36815(11) 0.83643(7) 0.0192(4) Uani 1 1 d . . .
H62 H 0.3083 0.3253 0.8098 0.023 Uiso 1 1 calc R . .
C63 C 0.2703(2) 0.45681(11) 0.82028(7) 0.0171(3) Uani 1 1 d . . .
C64 C 0.1845(2) 0.51906(11) 0.85942(7) 0.0225(4) Uani 1 1 d . . .
H64 H 0.1935 0.5807 0.8498 0.027 Uiso 1 1 calc R . .
C65 C 0.0862(2) 0.49055(12) 0.91233(8) 0.0250(4) Uani 1 1 d . . .
H65 H 0.0261 0.5322 0.9394 0.030 Uiso 1 1 calc R . .
C66 C 0.0765(2) 0.40037(12) 0.92518(8) 0.0235(4) Uani 1 1 d . . .
H66 H 0.0101 0.3808 0.9619 0.028 Uiso 1 1 calc R . .
C67 C 0.3903(2) 0.48364(11) 0.76445(7) 0.0198(4) Uani 1 1 d . . .
H67A H 0.4908 0.5047 0.7772 0.024 Uiso 1 1 calc R . .
H67B H 0.4393 0.4297 0.7434 0.024 Uiso 1 1 calc R . .
C71 C 0.2707(2) 0.99404(11) 0.66017(7) 0.0179(3) Uani 1 1 d . . .
C72 C 0.3425(2) 1.04030(11) 0.69694(7) 0.0192(4) Uani 1 1 d . . .
H72 H 0.3903 1.0099 0.7323 0.023 Uiso 1 1 calc R . .
C73 C 0.3436(2) 1.13059(11) 0.68145(7) 0.0188(4) Uani 1 1 d . . .
N73 N 0.41971(19) 1.17846(10) 0.72098(6) 0.0228(3) Uani 1 1 d . . .
O73 O 0.50807(17) 1.13393(9) 0.75881(6) 0.0302(3) Uani 1 1 d . . .
O74 O 0.38992(17) 1.26145(8) 0.71345(5) 0.0293(3) Uani 1 1 d . . .
C74 C 0.2758(2) 1.17862(11) 0.63075(7) 0.0194(4) Uani 1 1 d . . .
H74 H 0.2783 1.2409 0.6206 0.023 Uiso 1 1 calc R . .
C75 C 0.2041(2) 1.13064(11) 0.59547(7) 0.0198(4) Uani 1 1 d . . .
N75 N 0.12509(19) 1.18027(10) 0.54204(6) 0.0248(3) Uani 1 1 d . . .
O75 O 0.13133(17) 1.26094(8) 0.53107(6) 0.0331(3) Uani 1 1 d . . .
O76 O 0.05646(18) 1.13889(9) 0.51176(6) 0.0329(3) Uani 1 1 d . . .
C76 C 0.2012(2) 1.03982(11) 0.60833(7) 0.0187(4) Uani 1 1 d . . .
H76 H 0.1529 1.0092 0.5825 0.022 Uiso 1 1 calc R . .
C77 C 0.2698(2) 0.89574(11) 0.67833(7) 0.0184(3) Uani 1 1 d . . .
O71 O 0.20500(16) 0.85754(8) 0.64024(5) 0.0216(3) Uani 1 1 d . . .
H71 H 0.213(2) 0.7892(12) 0.6551(8) 0.026 Uiso 1 1 d . . .
O72 O 0.32849(16) 0.85755(8) 0.72455(5) 0.0233(3) Uani 1 1 d . . .
C81 C 0.1076(2) 0.03455(11) 0.87846(7) 0.0200(4) Uani 1 1 d . . .
C82 C 0.1410(2) -0.01225(11) 0.93428(7) 0.0219(4) Uani 1 1 d . . .
H82 H 0.1664 0.0186 0.9650 0.026 Uiso 1 1 calc R . .
C83 C 0.1375(2) -0.10335(11) 0.94563(7) 0.0231(4) Uani 1 1 d . . .
H83 H 0.1628 -0.1360 0.9835 0.028 Uiso 1 1 calc R . .
C84 C 0.0963(2) -0.14549(11) 0.90021(8) 0.0212(4) Uani 1 1 d . . .
N84 N 0.0936(2) -0.24220(10) 0.91127(7) 0.0274(4) Uani 1 1 d . . .
O83 O 0.03522(18) -0.27635(9) 0.87375(7) 0.0405(4) Uani 1 1 d . . .
O84 O 0.1486(2) -0.28460(9) 0.95726(6) 0.0413(4) Uani 1 1 d . . .
C85 C 0.0589(2) -0.10045(12) 0.84468(8) 0.0230(4) Uani 1 1 d . . .
H85 H 0.0296 -0.1312 0.8146 0.028 Uiso 1 1 calc R . .
C86 C 0.0650(2) -0.00999(12) 0.83385(8) 0.0225(4) Uani 1 1 d . . .
H86 H 0.0400 0.0222 0.7959 0.027 Uiso 1 1 calc R . .
C87 C 0.1195(2) 0.13184(11) 0.86498(8) 0.0204(4) Uani 1 1 d . . .
O81 O 0.13001(19) 0.17062(9) 0.91267(5) 0.0317(3) Uani 1 1 d . . .
H81 H 0.143(2) 0.2384(14) 0.8999(8) 0.038 Uiso 1 1 d . . .
O82 O 0.11685(16) 0.17056(8) 0.81384(5) 0.0246(3) 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
N11 0.0203(7) 0.0165(7) 0.0140(7) -0.0036(5) -0.0036(6) -0.0036(6)
C12 0.0201(9) 0.0186(9) 0.0170(8) -0.0003(7) -0.0018(7) -0.0004(7)
N13 0.0221(8) 0.0175(7) 0.0179(7) -0.0042(6) -0.0009(6) -0.0033(6)
C14 0.0158(8) 0.0184(8) 0.0174(8) -0.0034(7) 0.0011(7) -0.0027(7)
C15 0.0235(9) 0.0274(10) 0.0163(8) -0.0059(7) -0.0032(7) -0.0066(7)
C16 0.0249(10) 0.0298(10) 0.0164(9) -0.0005(7) -0.0063(7) -0.0045(8)
C17 0.0266(10) 0.0203(9) 0.0209(9) 0.0014(7) -0.0047(8) -0.0010(7)
C18 0.0213(9) 0.0172(8) 0.0174(8) -0.0039(7) -0.0008(7) -0.0031(7)
C19 0.0140(8) 0.0204(9) 0.0129(8) -0.0023(6) -0.0005(6) -0.0033(6)
N21 0.0250(8) 0.0198(8) 0.0180(7) -0.0031(6) -0.0034(6) -0.0017(6)
C22 0.0206(9) 0.0174(8) 0.0173(8) -0.0014(6) -0.0056(7) -0.0025(7)
C23 0.0159(8) 0.0182(8) 0.0154(8) -0.0022(6) -0.0053(7) -0.0016(6)
C24 0.0213(9) 0.0180(8) 0.0212(9) -0.0046(7) -0.0036(7) -0.0020(7)
C25 0.0258(10) 0.0208(9) 0.0198(9) 0.0015(7) -0.0017(7) -0.0071(7)
C26 0.0243(9) 0.0239(9) 0.0173(9) -0.0020(7) -0.0010(7) -0.0022(7)
C27 0.0193(8) 0.0179(8) 0.0169(8) -0.0052(6) -0.0054(7) -0.0033(7)
C31 0.0144(8) 0.0164(8) 0.0174(8) -0.0043(6) 0.0009(6) -0.0029(6)
C32 0.0140(8) 0.0218(9) 0.0158(8) -0.0042(7) -0.0006(7) -0.0037(7)
C33 0.0162(8) 0.0155(8) 0.0157(8) -0.0017(6) -0.0003(6) -0.0016(6)
N33 0.0202(8) 0.0198(8) 0.0188(7) -0.0029(6) 0.0007(6) -0.0035(6)
O33 0.0278(7) 0.0274(7) 0.0239(7) 0.0031(5) -0.0089(6) -0.0070(6)
O34 0.0414(8) 0.0171(6) 0.0237(7) -0.0033(5) -0.0019(6) -0.0098(6)
C34 0.0196(9) 0.0183(8) 0.0177(8) -0.0067(7) 0.0017(7) -0.0054(7)
C35 0.0144(8) 0.0246(9) 0.0128(8) -0.0056(7) 0.0001(6) -0.0035(7)
N35 0.0236(8) 0.0283(9) 0.0159(7) -0.0059(6) -0.0024(6) -0.0066(7)
O35 0.0423(8) 0.0330(8) 0.0248(7) -0.0086(6) -0.0075(6) -0.0187(6)
O36 0.0306(7) 0.0337(8) 0.0192(6) 0.0005(5) -0.0082(6) -0.0063(6)
C36 0.0176(8) 0.0179(8) 0.0159(8) -0.0029(6) -0.0009(7) -0.0025(7)
C37 0.0148(8) 0.0186(8) 0.0207(9) -0.0050(7) 0.0002(7) -0.0013(7)
O31 0.0310(7) 0.0141(6) 0.0233(6) -0.0017(5) -0.0073(5) -0.0060(5)
O32 0.0296(7) 0.0229(7) 0.0225(6) -0.0058(5) -0.0089(6) -0.0049(5)
C41 0.0173(8) 0.0199(9) 0.0166(8) -0.0065(7) 0.0006(7) -0.0028(7)
C42 0.0219(9) 0.0219(9) 0.0177(9) -0.0006(7) -0.0038(7) -0.0025(7)
C43 0.0237(9) 0.0229(9) 0.0199(9) -0.0048(7) -0.0072(7) -0.0031(7)
C44 0.0208(9) 0.0174(9) 0.0214(9) -0.0047(7) -0.0034(7) -0.0041(7)
N44A 0.0329(9) 0.0229(8) 0.0240(8) -0.0012(7) -0.0088(7) -0.0052(7)
O43A 0.236(8) 0.0283(17) 0.037(2) 0.0150(16) -0.053(3) -0.046(3)
O44A 0.063(3) 0.0256(13) 0.0314(19) -0.0090(12) -0.026(2) -0.0066(15)
N44B 0.0329(9) 0.0229(8) 0.0240(8) -0.0012(7) -0.0088(7) -0.0052(7)
C45 0.0332(11) 0.0234(9) 0.0172(9) 0.0010(7) -0.0078(8) -0.0026(8)
C46 0.0241(9) 0.0256(9) 0.0157(8) -0.0059(7) -0.0039(7) -0.0036(7)
C47 0.0162(8) 0.0230(9) 0.0193(9) -0.0054(7) 0.0023(7) -0.0030(7)
O41 0.0358(8) 0.0175(6) 0.0211(6) -0.0057(5) -0.0048(6) -0.0023(6)
O42 0.0287(7) 0.0260(7) 0.0233(7) -0.0080(5) -0.0062(6) -0.0062(5)
N51 0.0181(7) 0.0186(7) 0.0169(7) -0.0013(6) -0.0033(6) -0.0041(6)
C52 0.0206(9) 0.0192(9) 0.0189(8) -0.0037(7) -0.0015(7) -0.0053(7)
N53 0.0196(7) 0.0189(7) 0.0177(7) -0.0015(6) -0.0006(6) -0.0046(6)
C54 0.0151(8) 0.0197(9) 0.0172(8) -0.0025(7) 0.0021(7) -0.0029(7)
C55 0.0217(9) 0.0235(9) 0.0185(9) 0.0020(7) -0.0026(7) -0.0013(7)
C56 0.0217(9) 0.0340(11) 0.0183(9) -0.0045(8) -0.0024(7) -0.0064(8)
C57 0.0235(10) 0.0272(10) 0.0243(9) -0.0093(8) 0.0002(8) -0.0085(8)
C58 0.0195(9) 0.0197(9) 0.0215(9) -0.0015(7) 0.0016(7) -0.0032(7)
C59 0.0135(8) 0.0231(9) 0.0164(8) -0.0036(7) -0.0003(7) -0.0033(7)
N61 0.0245(8) 0.0194(7) 0.0206(7) -0.0006(6) -0.0062(6) -0.0057(6)
C62 0.0214(9) 0.0188(9) 0.0187(8) -0.0040(7) -0.0067(7) -0.0018(7)
C63 0.0179(8) 0.0173(8) 0.0167(8) -0.0020(6) -0.0071(7) -0.0010(7)
C64 0.0283(10) 0.0163(8) 0.0233(9) -0.0028(7) -0.0053(8) -0.0027(7)
C65 0.0305(10) 0.0242(10) 0.0205(9) -0.0075(7) -0.0012(8) -0.0027(8)
C66 0.0244(10) 0.0275(10) 0.0182(9) -0.0013(7) -0.0034(7) -0.0041(8)
C67 0.0197(9) 0.0189(9) 0.0206(9) -0.0007(7) -0.0065(7) -0.0006(7)
C71 0.0162(8) 0.0188(8) 0.0169(8) -0.0018(7) 0.0006(7) -0.0009(7)
C72 0.0183(9) 0.0227(9) 0.0146(8) -0.0015(7) -0.0002(7) -0.0003(7)
C73 0.0171(8) 0.0201(9) 0.0195(9) -0.0066(7) 0.0008(7) -0.0030(7)
N73 0.0225(8) 0.0252(8) 0.0209(8) -0.0050(6) 0.0026(6) -0.0067(6)
O73 0.0321(8) 0.0336(8) 0.0274(7) -0.0024(6) -0.0095(6) -0.0081(6)
O74 0.0394(8) 0.0203(7) 0.0283(7) -0.0068(5) 0.0033(6) -0.0083(6)
C74 0.0185(9) 0.0166(8) 0.0214(9) -0.0024(7) 0.0032(7) -0.0023(7)
C75 0.0181(9) 0.0226(9) 0.0150(8) 0.0018(7) 0.0006(7) 0.0008(7)
N75 0.0248(8) 0.0251(9) 0.0209(8) 0.0018(6) -0.0008(7) -0.0002(7)
O75 0.0402(8) 0.0221(7) 0.0328(7) 0.0057(6) -0.0063(6) 0.0003(6)
O76 0.0397(8) 0.0367(8) 0.0242(7) 0.0020(6) -0.0135(6) -0.0081(6)
C76 0.0178(8) 0.0206(9) 0.0164(8) -0.0022(7) 0.0003(7) -0.0013(7)
C77 0.0163(8) 0.0187(8) 0.0185(8) -0.0030(7) 0.0020(7) -0.0014(7)
O71 0.0275(7) 0.0171(6) 0.0207(6) -0.0010(5) -0.0060(5) -0.0041(5)
O72 0.0292(7) 0.0214(6) 0.0181(6) 0.0010(5) -0.0051(5) -0.0021(5)
C81 0.0209(9) 0.0217(9) 0.0166(8) -0.0023(7) -0.0028(7) -0.0015(7)
C82 0.0292(10) 0.0209(9) 0.0169(8) -0.0040(7) -0.0039(7) -0.0059(7)
C83 0.0313(10) 0.0215(9) 0.0157(9) -0.0004(7) -0.0034(8) -0.0036(8)
C84 0.0217(9) 0.0175(9) 0.0241(9) -0.0048(7) 0.0028(7) -0.0048(7)
N84 0.0262(9) 0.0217(8) 0.0336(9) -0.0073(7) 0.0023(7) -0.0039(7)
O83 0.0428(9) 0.0267(8) 0.0581(10) -0.0195(7) -0.0123(8) -0.0060(7)
O84 0.0616(10) 0.0244(8) 0.0369(8) 0.0040(6) -0.0042(7) -0.0117(7)
C85 0.0227(9) 0.0266(10) 0.0218(9) -0.0092(7) -0.0024(8) -0.0051(8)
C86 0.0226(9) 0.0269(10) 0.0177(9) -0.0022(7) -0.0039(7) -0.0031(7)
C87 0.0208(9) 0.0200(9) 0.0194(9) -0.0010(7) -0.0034(7) -0.0013(7)
O81 0.0576(10) 0.0187(7) 0.0210(7) 0.0001(5) -0.0085(6) -0.0110(6)
O82 0.0280(7) 0.0243(7) 0.0190(6) 0.0023(5) -0.0032(5) -0.0020(5)

_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
N11 C12 1.356(2) . ?
N11 C19 1.3895(19) . ?
N11 C27 1.4650(19) . ?
C12 N13 1.319(2) . ?
C12 H12 0.9500 . ?
N13 C14 1.389(2) . ?
C14 C15 1.392(2) . ?
C14 C19 1.400(2) . ?
C15 C16 1.374(2) . ?
C15 H15 0.9500 . ?
C16 C17 1.401(2) . ?
C16 H16 0.9500 . ?
C17 C18 1.381(2) . ?
C17 H17 0.9500 . ?
C18 C19 1.391(2) . ?
C18 H18 0.9500 . ?
N21 C26 1.335(2) . ?
N21 C22 1.340(2) . ?
C22 C23 1.389(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.389(2) . ?
C23 C27 1.512(2) . ?
C24 C25 1.389(2) . ?
C24 H24 0.9500 . ?
C25 C26 1.381(2) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C31 C32 1.388(2) . ?
C31 C36 1.396(2) . ?
C31 C37 1.504(2) . ?
C32 C33 1.378(2) . ?
C32 H32 0.9500 . ?
C33 C34 1.381(2) . ?
C33 N33 1.472(2) . ?
N33 O33 1.2250(17) . ?
N33 O34 1.2314(17) . ?
C34 C35 1.374(2) . ?
C34 H34 0.9500 . ?
C35 C36 1.383(2) . ?
C35 N35 1.476(2) . ?
N35 O35 1.2244(18) . ?
N35 O36 1.2269(18) . ?
C36 H36 0.9500 . ?
C37 O32 1.2161(18) . ?
C37 O31 1.307(2) . ?
O31 H31 1.024(18) . ?
C41 C46 1.386(2) . ?
C41 C42 1.393(2) . ?
C41 C47 1.500(2) . ?
C42 C43 1.388(2) . ?
C42 H42 0.9500 . ?
C43 C44 1.376(2) . ?
C43 H43 0.9500 . ?
C44 C45 1.382(2) . ?
C44 N44A 1.473(2) . ?
N44A O43A 1.196(3) . ?
N44A O44A 1.222(3) . ?
C45 C46 1.380(2) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C47 O42 1.2244(18) . ?
C47 O41 1.313(2) . ?
O41 H41 1.018(18) . ?
N51 C52 1.352(2) . ?
N51 C59 1.389(2) . ?
N51 C67 1.463(2) . ?
C52 N53 1.318(2) . ?
C52 H52 0.9500 . ?
N53 C54 1.393(2) . ?
N53 H71 1.502(19) . ?
C54 C55 1.393(2) . ?
C54 C59 1.397(2) . ?
C55 C56 1.375(2) . ?
C55 H55 0.9500 . ?
C56 C57 1.402(3) . ?
C56 H56 0.9500 . ?
C57 C58 1.380(2) . ?
C57 H57 0.9500 . ?
C58 C59 1.398(2) . ?
C58 H58 0.9500 . ?
N61 C66 1.336(2) . ?
N61 C62 1.344(2) . ?
C62 C63 1.382(2) . ?
C62 H62 0.9500 . ?
C63 C64 1.391(2) . ?
C63 C67 1.507(2) . ?
C64 C65 1.380(2) . ?
C64 H64 0.9500 . ?
C65 C66 1.381(2) . ?
C65 H65 0.9500 . ?
C66 H66 0.9500 . ?
C67 H67A 0.9900 . ?
C67 H67B 0.9900 . ?
C71 C72 1.392(2) . ?
C71 C76 1.396(2) . ?
C71 C77 1.501(2) . ?
C72 C73 1.376(2) . ?
C72 H72 0.9500 . ?
C73 C74 1.381(2) . ?
C73 N73 1.473(2) . ?
N73 O73 1.2188(18) . ?
N73 O74 1.2359(18) . ?
C74 C75 1.386(2) . ?
C74 H74 0.9500 . ?
C75 C76 1.381(2) . ?
C75 N75 1.475(2) . ?
N75 O76 1.2243(18) . ?
N75 O75 1.2314(18) . ?
C76 H76 0.9500 . ?
C77 O72 1.2222(19) . ?
C77 O71 1.3041(19) . ?
O71 H71 1.044(19) . ?
C81 C82 1.388(2) . ?
C81 C86 1.395(2) . ?
C81 C87 1.492(2) . ?
C82 C83 1.384(2) . ?
C82 H82 0.9500 . ?
C83 C84 1.383(2) . ?
C83 H83 0.9500 . ?
C84 C85 1.380(2) . ?
C84 N84 1.467(2) . ?
N84 O84 1.2269(19) . ?
N84 O83 1.2292(18) . ?
C85 C86 1.378(2) . ?
C85 H85 0.9500 . ?
C86 H86 0.9500 . ?
C87 O82 1.2181(19) . ?
C87 O81 1.3129(19) . ?
O81 H81 1.06(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C12 N11 C19 106.82(13) . . ?
C12 N11 C27 126.30(13) . . ?
C19 N11 C27 126.78(13) . . ?
N13 C12 N11 112.93(14) . . ?
N13 C12 H12 123.5 . . ?
N11 C12 H12 123.5 . . ?
C12 N13 C14 105.52(13) . . ?
N13 C14 C15 130.10(15) . . ?
N13 C14 C19 109.26(14) . . ?
C15 C14 C19 120.63(16) . . ?
C16 C15 C14 117.38(16) . . ?
C16 C15 H15 121.3 . . ?
C14 C15 H15 121.3 . . ?
C15 C16 C17 121.68(16) . . ?
C15 C16 H16 119.2 . . ?
C17 C16 H16 119.2 . . ?
C18 C17 C16 121.77(16) . . ?
C18 C17 H17 119.1 . . ?
C16 C17 H17 119.1 . . ?
C17 C18 C19 116.38(15) . . ?
C17 C18 H18 121.8 . . ?
C19 C18 H18 121.8 . . ?
N11 C19 C18 132.36(15) . . ?
N11 C19 C14 105.47(14) . . ?
C18 C19 C14 122.16(15) . . ?
C26 N21 C22 117.87(14) . . ?
N21 C22 C23 123.70(16) . . ?
N21 C22 H22 118.1 . . ?
C23 C22 H22 118.1 . . ?
C22 C23 C24 117.61(15) . . ?
C22 C23 C27 118.59(15) . . ?
C24 C23 C27 123.61(14) . . ?
C23 C24 C25 119.06(15) . . ?
C23 C24 H24 120.5 . . ?
C25 C24 H24 120.5 . . ?
C26 C25 C24 119.06(16) . . ?
C26 C25 H25 120.5 . . ?
C24 C25 H25 120.5 . . ?
N21 C26 C25 122.67(16) . . ?
N21 C26 H26 118.7 . . ?
C25 C26 H26 118.7 . . ?
N11 C27 C23 115.52(13) . . ?
N11 C27 H27A 108.4 . . ?
C23 C27 H27A 108.4 . . ?
N11 C27 H27B 108.4 . . ?
C23 C27 H27B 108.4 . . ?
H27A C27 H27B 107.5 . . ?
C32 C31 C36 120.10(15) . . ?
C32 C31 C37 118.66(14) . . ?
C36 C31 C37 121.24(15) . . ?
C33 C32 C31 118.80(15) . . ?
C33 C32 H32 120.6 . . ?
C31 C32 H32 120.6 . . ?
C32 C33 C34 122.83(15) . . ?
C32 C33 N33 119.18(14) . . ?
C34 C33 N33 117.98(14) . . ?
O33 N33 O34 124.03(14) . . ?
O33 N33 C33 118.34(13) . . ?
O34 N33 C33 117.62(14) . . ?
C35 C34 C33 116.86(15) . . ?
C35 C34 H34 121.6 . . ?
C33 C34 H34 121.6 . . ?
C34 C35 C36 123.00(15) . . ?
C34 C35 N35 117.76(15) . . ?
C36 C35 N35 119.23(15) . . ?
O35 N35 O36 124.47(14) . . ?
O35 N35 C35 117.68(14) . . ?
O36 N35 C35 117.85(14) . . ?
C35 C36 C31 118.38(15) . . ?
C35 C36 H36 120.8 . . ?
C31 C36 H36 120.8 . . ?
O32 C37 O31 125.75(15) . . ?
O32 C37 C31 121.35(15) . . ?
O31 C37 C31 112.90(14) . . ?
C37 O31 H31 110.7(10) . . ?
C46 C41 C42 119.94(15) . . ?
C46 C41 C47 118.95(15) . . ?
C42 C41 C47 121.11(15) . . ?
C43 C42 C41 120.33(16) . . ?
C43 C42 H42 119.8 . . ?
C41 C42 H42 119.8 . . ?
C44 C43 C42 118.02(15) . . ?
C44 C43 H43 121.0 . . ?
C42 C43 H43 121.0 . . ?
C43 C44 C45 122.95(15) . . ?
C43 C44 N44A 119.00(15) . . ?
C45 C44 N44A 118.05(15) . . ?
O43A N44A O44A 122.5(2) . . ?
O43A N44A C44 118.6(2) . . ?
O44A N44A C44 118.80(19) . . ?
C46 C45 C44 118.32(16) . . ?
C46 C45 H45 120.8 . . ?
C44 C45 H45 120.8 . . ?
C45 C46 C41 120.42(16) . . ?
C45 C46 H46 119.8 . . ?
C41 C46 H46 119.8 . . ?
O42 C47 O41 124.27(16) . . ?
O42 C47 C41 121.75(15) . . ?
O41 C47 C41 113.99(14) . . ?
C47 O41 H41 110.5(10) . . ?
C52 N51 C59 106.90(13) . . ?
C52 N51 C67 126.12(14) . . ?
C59 N51 C67 126.87(14) . . ?
N53 C52 N51 112.74(15) . . ?
N53 C52 H52 123.6 . . ?
N51 C52 H52 123.6 . . ?
C52 N53 C54 105.79(14) . . ?
C52 N53 H71 126.6(6) . . ?
C54 N53 H71 127.4(6) . . ?
C55 C54 N53 130.30(15) . . ?
C55 C54 C59 120.89(15) . . ?
N53 C54 C59 108.79(14) . . ?
C56 C55 C54 117.15(16) . . ?
C56 C55 H55 121.4 . . ?
C54 C55 H55 121.4 . . ?
C55 C56 C57 121.82(16) . . ?
C55 C56 H56 119.1 . . ?
C57 C56 H56 119.1 . . ?
C58 C57 C56 121.83(16) . . ?
C58 C57 H57 119.1 . . ?
C56 C57 H57 119.1 . . ?
C57 C58 C59 116.20(16) . . ?
C57 C58 H58 121.9 . . ?
C59 C58 H58 121.9 . . ?
N51 C59 C54 105.77(14) . . ?
N51 C59 C58 132.08(16) . . ?
C54 C59 C58 122.11(15) . . ?
C66 N61 C62 118.09(15) . . ?
N61 C62 C63 123.24(15) . . ?
N61 C62 H62 118.4 . . ?
C63 C62 H62 118.4 . . ?
C62 C63 C64 117.74(15) . . ?
C62 C63 C67 120.85(14) . . ?
C64 C63 C67 121.27(15) . . ?
C65 C64 C63 119.47(16) . . ?
C65 C64 H64 120.3 . . ?
C63 C64 H64 120.3 . . ?
C64 C65 C66 118.84(16) . . ?
C64 C65 H65 120.6 . . ?
C66 C65 H65 120.6 . . ?
N61 C66 C65 122.61(16) . . ?
N61 C66 H66 118.7 . . ?
C65 C66 H66 118.7 . . ?
N51 C67 C63 114.95(13) . . ?
N51 C67 H67A 108.5 . . ?
C63 C67 H67A 108.5 . . ?
N51 C67 H67B 108.5 . . ?
C63 C67 H67B 108.5 . . ?
H67A C67 H67B 107.5 . . ?
C72 C71 C76 119.61(16) . . ?
C72 C71 C77 118.23(14) . . ?
C76 C71 C77 122.16(15) . . ?
C73 C72 C71 119.25(15) . . ?
C73 C72 H72 120.4 . . ?
C71 C72 H72 120.4 . . ?
C72 C73 C74 123.14(16) . . ?
C72 C73 N73 118.47(15) . . ?
C74 C73 N73 118.38(15) . . ?
O73 N73 O74 124.24(15) . . ?
O73 N73 C73 118.11(15) . . ?
O74 N73 C73 117.64(14) . . ?
C73 C74 C75 116.07(16) . . ?
C73 C74 H74 122.0 . . ?
C75 C74 H74 122.0 . . ?
C76 C75 C74 123.40(15) . . ?
C76 C75 N75 118.94(15) . . ?
C74 C75 N75 117.66(15) . . ?
O76 N75 O75 124.25(15) . . ?
O76 N75 C75 118.02(15) . . ?
O75 N75 C75 117.73(15) . . ?
C75 C76 C71 118.53(16) . . ?
C75 C76 H76 120.7 . . ?
C71 C76 H76 120.7 . . ?
O72 C77 O71 125.22(16) . . ?
O72 C77 C71 120.92(15) . . ?
O71 C77 C71 113.85(14) . . ?
C77 O71 H71 109.3(9) . . ?
C82 C81 C86 119.76(16) . . ?
C82 C81 C87 120.90(15) . . ?
C86 C81 C87 119.33(15) . . ?
C83 C82 C81 120.69(16) . . ?
C83 C82 H82 119.7 . . ?
C81 C82 H82 119.7 . . ?
C84 C83 C82 117.98(16) . . ?
C84 C83 H83 121.0 . . ?
C82 C83 H83 121.0 . . ?
C85 C84 C83 122.70(16) . . ?
C85 C84 N84 118.59(15) . . ?
C83 C84 N84 118.70(15) . . ?
O84 N84 O83 123.47(16) . . ?
O84 N84 C84 118.73(15) . . ?
O83 N84 C84 117.80(15) . . ?
C86 C85 C84 118.59(16) . . ?
C86 C85 H85 120.7 . . ?
C84 C85 H85 120.7 . . ?
C85 C86 C81 120.26(16) . . ?
C85 C86 H86 119.9 . . ?
C81 C86 H86 119.9 . . ?
O82 C87 O81 124.16(16) . . ?
O82 C87 C81 121.65(16) . . ?
O81 C87 C81 114.18(14) . . ?
C87 O81 H81 110.4(10) . . ?

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
C19 N11 C12 N13 0.42(19) . . . . ?
C27 N11 C12 N13 177.00(14) . . . . ?
N11 C12 N13 C14 -0.50(18) . . . . ?
C12 N13 C14 C15 -179.20(17) . . . . ?
C12 N13 C14 C19 0.39(18) . . . . ?
N13 C14 C15 C16 179.39(17) . . . . ?
C19 C14 C15 C16 -0.2(2) . . . . ?
C14 C15 C16 C17 -0.1(3) . . . . ?
C15 C16 C17 C18 0.1(3) . . . . ?
C16 C17 C18 C19 0.1(2) . . . . ?
C12 N11 C19 C18 178.79(17) . . . . ?
C27 N11 C19 C18 2.2(3) . . . . ?
C12 N11 C19 C14 -0.15(17) . . . . ?
C27 N11 C19 C14 -176.71(14) . . . . ?
C17 C18 C19 N11 -179.16(16) . . . . ?
C17 C18 C19 C14 -0.4(2) . . . . ?
N13 C14 C19 N11 -0.14(17) . . . . ?
C15 C14 C19 N11 179.49(14) . . . . ?
N13 C14 C19 C18 -179.22(15) . . . . ?
C15 C14 C19 C18 0.4(2) . . . . ?
C26 N21 C22 C23 -1.2(2) . . . . ?
N21 C22 C23 C24 -0.3(2) . . . . ?
N21 C22 C23 C27 174.88(15) . . . . ?
C22 C23 C24 C25 1.2(2) . . . . ?
C27 C23 C24 C25 -173.71(15) . . . . ?
C23 C24 C25 C26 -0.6(2) . . . . ?
C22 N21 C26 C25 1.8(3) . . . . ?
C24 C25 C26 N21 -0.9(3) . . . . ?
C12 N11 C27 C23 82.03(19) . . . . ?
C19 N11 C27 C23 -102.05(18) . . . . ?
C22 C23 C27 N11 138.70(15) . . . . ?
C24 C23 C27 N11 -46.5(2) . . . . ?
C36 C31 C32 C33 0.2(2) . . . . ?
C37 C31 C32 C33 -178.81(14) . . . . ?
C31 C32 C33 C34 0.6(2) . . . . ?
C31 C32 C33 N33 -178.04(14) . . . . ?
C32 C33 N33 O33 2.3(2) . . . . ?
C34 C33 N33 O33 -176.46(14) . . . . ?
C32 C33 N33 O34 -178.77(14) . . . . ?
C34 C33 N33 O34 2.5(2) . . . . ?
C32 C33 C34 C35 -0.4(2) . . . . ?
N33 C33 C34 C35 178.32(14) . . . . ?
C33 C34 C35 C36 -0.8(2) . . . . ?
C33 C34 C35 N35 178.82(13) . . . . ?
C34 C35 N35 O35 -2.6(2) . . . . ?
C36 C35 N35 O35 177.03(15) . . . . ?
C34 C35 N35 O36 177.36(15) . . . . ?
C36 C35 N35 O36 -3.0(2) . . . . ?
C34 C35 C36 C31 1.6(2) . . . . ?
N35 C35 C36 C31 -178.00(13) . . . . ?
C32 C31 C36 C35 -1.3(2) . . . . ?
C37 C31 C36 C35 177.72(14) . . . . ?
C32 C31 C37 O32 2.5(2) . . . . ?
C36 C31 C37 O32 -176.51(15) . . . . ?
C32 C31 C37 O31 -177.77(14) . . . . ?
C36 C31 C37 O31 3.2(2) . . . . ?
C46 C41 C42 C43 -1.2(2) . . . . ?
C47 C41 C42 C43 179.34(15) . . . . ?
C41 C42 C43 C44 1.0(2) . . . . ?
C42 C43 C44 C45 0.1(3) . . . . ?
C42 C43 C44 N44A -179.23(15) . . . . ?
C43 C44 N44A O43A -173.5(7) . . . . ?
C45 C44 N44A O43A 7.1(8) . . . . ?
C43 C44 N44A O44A 3.4(5) . . . . ?
C45 C44 N44A O44A -176.0(5) . . . . ?
C43 C44 C45 C46 -1.1(3) . . . . ?
N44A C44 C45 C46 178.25(16) . . . . ?
C44 C45 C46 C41 1.0(3) . . . . ?
C42 C41 C46 C45 0.2(3) . . . . ?
C47 C41 C46 C45 179.66(15) . . . . ?
C46 C41 C47 O42 2.7(2) . . . . ?
C42 C41 C47 O42 -177.82(15) . . . . ?
C46 C41 C47 O41 -177.39(15) . . . . ?
C42 C41 C47 O41 2.1(2) . . . . ?
C59 N51 C52 N53 -0.44(19) . . . . ?
C67 N51 C52 N53 175.92(14) . . . . ?
N51 C52 N53 C54 0.08(18) . . . . ?
C52 N53 C54 C55 -178.08(17) . . . . ?
C52 N53 C54 C59 0.30(18) . . . . ?
N53 C54 C55 C56 178.99(16) . . . . ?
C59 C54 C55 C56 0.8(2) . . . . ?
C54 C55 C56 C57 -1.1(3) . . . . ?
C55 C56 C57 C58 0.5(3) . . . . ?
C56 C57 C58 C59 0.5(2) . . . . ?
C52 N51 C59 C54 0.59(17) . . . . ?
C67 N51 C59 C54 -175.73(14) . . . . ?
C52 N51 C59 C58 178.13(17) . . . . ?
C67 N51 C59 C58 1.8(3) . . . . ?
C55 C54 C59 N51 178.01(14) . . . . ?
N53 C54 C59 N51 -0.55(17) . . . . ?
C55 C54 C59 C58 0.2(2) . . . . ?
N53 C54 C59 C58 -178.40(14) . . . . ?
C57 C58 C59 N51 -178.00(16) . . . . ?
C57 C58 C59 C54 -0.8(2) . . . . ?
C66 N61 C62 C63 0.4(2) . . . . ?
N61 C62 C63 C64 -0.8(2) . . . . ?
N61 C62 C63 C67 174.83(15) . . . . ?
C62 C63 C64 C65 0.4(2) . . . . ?
C67 C63 C64 C65 -175.23(16) . . . . ?
C63 C64 C65 C66 0.4(3) . . . . ?
C62 N61 C66 C65 0.5(2) . . . . ?
C64 C65 C66 N61 -0.9(3) . . . . ?
C52 N51 C67 C63 92.59(19) . . . . ?
C59 N51 C67 C63 -91.77(19) . . . . ?
C62 C63 C67 N51 125.27(16) . . . . ?
C64 C63 C67 N51 -59.2(2) . . . . ?
C76 C71 C72 C73 0.0(2) . . . . ?
C77 C71 C72 C73 -179.48(15) . . . . ?
C71 C72 C73 C74 0.2(3) . . . . ?
C71 C72 C73 N73 179.85(14) . . . . ?
C72 C73 N73 O73 13.7(2) . . . . ?
C74 C73 N73 O73 -166.58(15) . . . . ?
C72 C73 N73 O74 -166.44(15) . . . . ?
C74 C73 N73 O74 13.3(2) . . . . ?
C72 C73 C74 C75 0.4(2) . . . . ?
N73 C73 C74 C75 -179.33(14) . . . . ?
C73 C74 C75 C76 -1.1(2) . . . . ?
C73 C74 C75 N75 178.02(14) . . . . ?
C76 C75 N75 O76 1.5(2) . . . . ?
C74 C75 N75 O76 -177.73(14) . . . . ?
C76 C75 N75 O75 -179.09(15) . . . . ?
C74 C75 N75 O75 1.7(2) . . . . ?
C74 C75 C76 C71 1.3(2) . . . . ?
N75 C75 C76 C71 -177.80(14) . . . . ?
C72 C71 C76 C75 -0.7(2) . . . . ?
C77 C71 C76 C75 178.75(15) . . . . ?
C72 C71 C77 O72 0.9(2) . . . . ?
C76 C71 C77 O72 -178.62(15) . . . . ?
C72 C71 C77 O71 -178.00(14) . . . . ?
C76 C71 C77 O71 2.5(2) . . . . ?
C86 C81 C82 C83 1.9(3) . . . . ?
C87 C81 C82 C83 -177.11(16) . . . . ?
C81 C82 C83 C84 -1.4(3) . . . . ?
C82 C83 C84 C85 0.0(3) . . . . ?
C82 C83 C84 N84 179.43(16) . . . . ?
C85 C84 N84 O84 170.75(16) . . . . ?
C83 C84 N84 O84 -8.7(2) . . . . ?
C85 C84 N84 O83 -9.6(2) . . . . ?
C83 C84 N84 O83 170.95(15) . . . . ?
C83 C84 C85 C86 0.7(3) . . . . ?
N84 C84 C85 C86 -178.67(15) . . . . ?
C84 C85 C86 C81 -0.2(3) . . . . ?
C82 C81 C86 C85 -1.1(3) . . . . ?
C87 C81 C86 C85 177.91(16) . . . . ?
C82 C81 C87 O82 168.86(17) . . . . ?
C86 C81 C87 O82 -10.2(3) . . . . ?
C82 C81 C87 O81 -12.1(2) . . . . ?
C86 C81 C87 O81 168.87(15) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O31 H31 N13 1.024(18) 1.559(18) 2.5762(17) 171.0(16) .
O71 H71 N53 1.044(19) 1.502(19) 2.5455(18) 177.4(15) .
O41 H41 N21 1.018(18) 1.594(19) 2.6081(18) 173.6(16) .
O81 H81 N61 1.06(2) 1.55(2) 2.6057(19) 174.2(16) .

_diffrn_measured_fraction_theta_max 0.977
_diffrn_reflns_theta_full        30.14
_diffrn_measured_fraction_theta_full 0.977
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.076

#END

data_2
_database_code_depnum_ccdc_archive 'CCDC 259794'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
1-(3-pyridylmethyl)benzimidazole, 3,5-diNO2PhCOOH, 3-Me2NPhCOOH
;
_chemical_name_common            
;1-(3-pyridylmethyl)benzimidazole, 3,5-diNO2PhCOOH, 3-
Me2NPhCOOH
;
_chemical_melting_point          ?
_chemical_formula_moiety         
;
(C13 H11 N3) (C7 H4 N2 O6) (C9 H11 N O2)
;
_chemical_formula_sum            'C29 H26 N6 O8'
_chemical_formula_weight         586.56

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

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   8.1324(7)
_cell_length_b                   10.8110(9)
_cell_length_c                   15.3761(13)
_cell_angle_alpha                95.489(4)
_cell_angle_beta                 90.318(5)
_cell_angle_gamma                91.503(5)
_cell_volume                     1345.2(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    203(2)
_cell_measurement_reflns_used    2689
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      27.00

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             612
_exptl_absorpt_coefficient_mu    0.108
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      203(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9845
_diffrn_reflns_av_R_equivalents  0.0691
_diffrn_reflns_av_sigmaI/netI    0.0823
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.33
_diffrn_reflns_theta_max         27.51
_reflns_number_total             5871
_reflns_number_gt                3561
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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^)+(0.1000P)^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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5871
_refine_ls_number_parameters     394
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1044
_refine_ls_R_factor_gt           0.0628
_refine_ls_wR_factor_ref         0.1840
_refine_ls_wR_factor_gt          0.1587
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_restrained_S_all      0.974
_refine_ls_shift/su_max          0.000
_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
N11 N 0.0740(2) 0.82722(18) 0.67499(13) 0.0347(5) Uani 1 1 d . . .
C12 C 0.0624(3) 0.8212(2) 0.76176(15) 0.0352(6) Uani 1 1 d . . .
H12 H 0.0003 0.7593 0.7867 0.042 Uiso 1 1 calc R . .
N13 N 0.1459(2) 0.91000(19) 0.80816(13) 0.0354(5) Uani 1 1 d . . .
C14 C 0.2182(3) 0.9814(2) 0.74722(15) 0.0334(5) Uani 1 1 d . . .
C15 C 0.3169(3) 1.0883(2) 0.75795(17) 0.0385(6) Uani 1 1 d . . .
H15 H 0.3453 1.1254 0.8140 0.046 Uiso 1 1 calc R . .
C16 C 0.3716(3) 1.1383(2) 0.68461(18) 0.0453(7) Uani 1 1 d . . .
H16 H 0.4387 1.2108 0.6906 0.054 Uiso 1 1 calc R . .
C17 C 0.3301(4) 1.0840(3) 0.60120(19) 0.0502(7) Uani 1 1 d . . .
H17 H 0.3706 1.1204 0.5522 0.060 Uiso 1 1 calc R . .
C18 C 0.2315(4) 0.9786(3) 0.58881(17) 0.0477(7) Uani 1 1 d . . .
H18 H 0.2035 0.9419 0.5326 0.057 Uiso 1 1 calc R . .
C19 C 0.1753(3) 0.9292(2) 0.66359(16) 0.0356(6) Uani 1 1 d . . .
N21 N 0.2727(3) 0.5395(2) 0.46241(14) 0.0427(5) Uani 1 1 d . . .
C22 C 0.1759(3) 0.6308(2) 0.49327(16) 0.0398(6) Uani 1 1 d . . .
H22 H 0.1544 0.6943 0.4574 0.048 Uiso 1 1 calc R . .
C23 C 0.1057(3) 0.6373(2) 0.57464(15) 0.0319(5) Uani 1 1 d . . .
C24 C 0.1368(3) 0.5429(2) 0.62564(17) 0.0411(6) Uani 1 1 d . . .
H24 H 0.0900 0.5431 0.6814 0.049 Uiso 1 1 calc R . .
C25 C 0.2365(3) 0.4484(3) 0.59489(18) 0.0453(7) Uani 1 1 d . . .
H25 H 0.2593 0.3836 0.6293 0.054 Uiso 1 1 calc R . .
C26 C 0.3028(3) 0.4500(3) 0.51302(18) 0.0435(6) Uani 1 1 d . . .
H26 H 0.3717 0.3854 0.4922 0.052 Uiso 1 1 calc R . .
C27 C -0.0029(3) 0.7422(2) 0.60640(16) 0.0358(6) Uani 1 1 d . . .
H27A H -0.0314 0.7887 0.5570 0.043 Uiso 1 1 calc R . .
H27B H -0.1052 0.7077 0.6287 0.043 Uiso 1 1 calc R . .
C31 C 0.3034(3) 0.5339(2) 0.14840(15) 0.0322(5) Uani 1 1 d . . .
C32 C 0.2349(3) 0.4568(2) 0.08075(16) 0.0333(5) Uani 1 1 d . . .
H32 H 0.1783 0.3835 0.0928 0.040 Uiso 1 1 calc R . .
C33 C 0.2482(3) 0.4856(2) -0.00579(16) 0.0365(6) Uani 1 1 d . . .
N33 N 0.1829(3) 0.4093(2) -0.07393(14) 0.0510(6) Uani 1 1 d . . .
C38 C 0.0855(3) 0.3012(3) -0.05884(19) 0.0494(7) Uani 1 1 d . . .
H38A H -0.0128 0.3262 -0.0271 0.074 Uiso 1 1 calc R . .
H38B H 0.1488 0.2479 -0.0249 0.074 Uiso 1 1 calc R . .
H38C H 0.0544 0.2563 -0.1144 0.074 Uiso 1 1 calc R . .
C39 C 0.1840(4) 0.4476(3) -0.16079(17) 0.0545(8) Uani 1 1 d . . .
H39A H 0.2945 0.4742 -0.1751 0.082 Uiso 1 1 calc R . .
H39B H 0.1100 0.5160 -0.1640 0.082 Uiso 1 1 calc R . .
H39C H 0.1481 0.3784 -0.2020 0.082 Uiso 1 1 calc R . .
C34 C 0.3333(3) 0.5972(3) -0.01983(17) 0.0407(6) Uani 1 1 d . . .
H34 H 0.3439 0.6202 -0.0770 0.049 Uiso 1 1 calc R . .
C35 C 0.4005(3) 0.6723(3) 0.04832(18) 0.0421(6) Uani 1 1 d . . .
H35 H 0.4575 0.7458 0.0370 0.050 Uiso 1 1 calc R . .
C36 C 0.3869(3) 0.6430(2) 0.13323(17) 0.0392(6) Uani 1 1 d . . .
H36 H 0.4331 0.6956 0.1797 0.047 Uiso 1 1 calc R . .
C37 C 0.2838(3) 0.4978(2) 0.23854(16) 0.0357(6) Uani 1 1 d . . .
O37 O 0.3574(2) 0.57366(18) 0.29904(12) 0.0463(5) Uani 1 1 d . . .
H37 H 0.327(3) 0.549(3) 0.351(2) 0.056 Uiso 1 1 d . . .
O38 O 0.2051(2) 0.40488(17) 0.25508(11) 0.0436(5) Uani 1 1 d . . .
C41 C 0.2920(3) 1.0265(2) 1.10876(15) 0.0334(5) Uani 1 1 d . . .
C42 C 0.2150(3) 0.9419(2) 1.15915(15) 0.0349(6) Uani 1 1 d . . .
H42 H 0.1533 0.8735 1.1328 0.042 Uiso 1 1 calc R . .
C43 C 0.2319(3) 0.9609(2) 1.24877(15) 0.0346(6) Uani 1 1 d . . .
N43 N 0.1524(3) 0.8720(2) 1.30234(14) 0.0441(6) Uani 1 1 d . . .
O43 O 0.0761(3) 0.78418(19) 1.26673(13) 0.0551(5) Uani 1 1 d . . .
O44 O 0.1672(3) 0.8915(2) 1.38115(13) 0.0750(7) Uani 1 1 d . . .
C44 C 0.3200(3) 1.0601(2) 1.29016(16) 0.0374(6) Uani 1 1 d . . .
H44 H 0.3288 1.0719 1.3514 0.045 Uiso 1 1 calc R . .
C45 C 0.3942(3) 1.1406(2) 1.23854(16) 0.0343(5) Uani 1 1 d . . .
N45 N 0.4936(3) 1.2456(2) 1.28107(15) 0.0417(5) Uani 1 1 d . . .
O45 O 0.4886(2) 1.26286(19) 1.36087(13) 0.0546(5) Uani 1 1 d . . .
O46 O 0.5754(2) 1.30836(18) 1.23519(13) 0.0518(5) Uani 1 1 d . . .
C46 C 0.3834(3) 1.1260(2) 1.14889(16) 0.0352(5) Uani 1 1 d . . .
H46 H 0.4373 1.1828 1.1153 0.042 Uiso 1 1 calc R . .
C47 C 0.2801(3) 1.0122(2) 1.01169(16) 0.0350(6) Uani 1 1 d . . .
O48 O 0.3575(2) 1.07907(18) 0.96780(12) 0.0500(5) Uani 1 1 d . . .
O47 O 0.1791(2) 0.92322(17) 0.98053(12) 0.0439(5) Uani 1 1 d . . .
H47 H 0.174(3) 0.919(3) 0.919(2) 0.053 Uiso 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
N11 0.0449(11) 0.0316(11) 0.0268(11) -0.0016(9) -0.0033(8) 0.0029(9)
C12 0.0414(12) 0.0370(14) 0.0267(13) 0.0005(11) -0.0006(10) 0.0038(11)
N13 0.0421(11) 0.0360(12) 0.0272(11) -0.0009(9) -0.0016(8) 0.0012(9)
C14 0.0400(12) 0.0316(13) 0.0282(13) -0.0003(10) -0.0016(10) 0.0063(10)
C15 0.0455(13) 0.0341(14) 0.0349(14) -0.0012(11) -0.0054(11) 0.0018(11)
C16 0.0593(16) 0.0315(14) 0.0452(17) 0.0048(13) -0.0064(13) 0.0011(12)
C17 0.0753(18) 0.0401(16) 0.0357(15) 0.0086(13) -0.0002(13) -0.0073(14)
C18 0.0732(18) 0.0432(16) 0.0267(14) 0.0035(12) -0.0026(12) -0.0032(14)
C19 0.0417(13) 0.0299(13) 0.0345(14) -0.0012(11) -0.0030(10) 0.0028(10)
N21 0.0492(12) 0.0482(14) 0.0289(12) -0.0039(10) 0.0005(9) -0.0034(11)
C22 0.0527(14) 0.0368(14) 0.0299(13) 0.0043(11) -0.0014(11) -0.0053(12)
C23 0.0373(12) 0.0325(13) 0.0249(12) -0.0005(10) -0.0066(9) -0.0054(10)
C24 0.0502(14) 0.0433(16) 0.0304(13) 0.0061(12) 0.0020(11) 0.0040(12)
C25 0.0591(16) 0.0419(16) 0.0355(15) 0.0056(12) -0.0062(12) 0.0087(13)
C26 0.0420(13) 0.0450(16) 0.0413(16) -0.0075(13) -0.0072(11) 0.0055(12)
C27 0.0452(13) 0.0342(14) 0.0274(13) 0.0004(10) -0.0084(10) -0.0009(11)
C31 0.0327(11) 0.0344(13) 0.0299(13) 0.0039(11) 0.0036(9) 0.0030(10)
C32 0.0334(11) 0.0323(13) 0.0350(14) 0.0066(11) 0.0027(10) 0.0004(10)
C33 0.0345(12) 0.0430(15) 0.0321(13) 0.0039(11) -0.0018(10) 0.0012(11)
N33 0.0535(13) 0.0669(17) 0.0323(12) 0.0095(12) -0.0072(10) -0.0189(12)
C38 0.0540(15) 0.0496(18) 0.0433(16) 0.0008(14) -0.0067(12) -0.0056(13)
C39 0.0604(17) 0.074(2) 0.0288(14) 0.0069(14) -0.0052(12) -0.0063(15)
C34 0.0416(13) 0.0470(16) 0.0351(14) 0.0113(12) 0.0042(11) 0.0023(12)
C35 0.0459(14) 0.0354(14) 0.0459(16) 0.0088(12) 0.0050(12) -0.0012(11)
C36 0.0441(13) 0.0336(14) 0.0398(15) 0.0028(12) 0.0041(11) 0.0018(11)
C37 0.0353(12) 0.0381(14) 0.0330(14) -0.0011(11) 0.0038(10) 0.0028(11)
O37 0.0586(11) 0.0501(12) 0.0285(10) -0.0012(9) 0.0017(8) -0.0095(9)
O38 0.0509(10) 0.0447(11) 0.0355(10) 0.0074(8) 0.0027(8) -0.0076(9)
C41 0.0402(12) 0.0297(13) 0.0304(13) 0.0024(10) 0.0002(10) 0.0079(10)
C42 0.0418(13) 0.0343(14) 0.0284(13) 0.0007(11) -0.0021(10) 0.0061(10)
C43 0.0393(12) 0.0354(14) 0.0299(13) 0.0060(11) 0.0000(10) 0.0078(10)
N43 0.0589(13) 0.0446(14) 0.0297(12) 0.0074(11) -0.0017(10) 0.0031(11)
O43 0.0715(13) 0.0524(13) 0.0418(12) 0.0107(10) -0.0030(10) -0.0135(11)
O44 0.1222(19) 0.0737(16) 0.0293(12) 0.0107(11) -0.0046(12) -0.0183(14)
C44 0.0457(13) 0.0384(14) 0.0269(13) -0.0048(11) -0.0016(10) 0.0093(11)
C45 0.0390(12) 0.0301(13) 0.0327(14) -0.0040(11) -0.0046(10) 0.0059(10)
N45 0.0445(12) 0.0414(13) 0.0373(13) -0.0076(11) -0.0063(10) 0.0071(10)
O45 0.0695(13) 0.0552(13) 0.0361(11) -0.0112(9) -0.0076(9) 0.0004(10)
O46 0.0542(11) 0.0495(12) 0.0494(12) -0.0038(10) 0.0016(9) -0.0113(9)
C46 0.0407(12) 0.0331(14) 0.0313(13) -0.0010(11) -0.0001(10) 0.0063(10)
C47 0.0418(12) 0.0316(13) 0.0314(13) 0.0019(11) 0.0001(10) 0.0041(11)
O48 0.0671(12) 0.0501(12) 0.0328(10) 0.0090(9) -0.0036(9) -0.0151(10)
O47 0.0591(11) 0.0444(11) 0.0271(9) 0.0023(8) -0.0038(8) -0.0115(9)

_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
N11 C12 1.346(3) . ?
N11 C19 1.384(3) . ?
N11 C27 1.458(3) . ?
C12 N13 1.312(3) . ?
C12 H12 0.9400 . ?
N13 C14 1.393(3) . ?
C14 C15 1.386(3) . ?
C14 C19 1.393(3) . ?
C15 C16 1.368(3) . ?
C15 H15 0.9400 . ?
C16 C17 1.394(4) . ?
C16 H16 0.9400 . ?
C17 C18 1.373(4) . ?
C17 H17 0.9400 . ?
C18 C19 1.388(4) . ?
C18 H18 0.9400 . ?
N21 C26 1.325(3) . ?
N21 C22 1.333(3) . ?
C22 C23 1.375(3) . ?
C22 H22 0.9400 . ?
C23 C24 1.372(3) . ?
C23 C27 1.502(3) . ?
C24 C25 1.371(4) . ?
C24 H24 0.9400 . ?
C25 C26 1.373(4) . ?
C25 H25 0.9400 . ?
C26 H26 0.9400 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C31 C32 1.375(3) . ?
C31 C36 1.385(3) . ?
C31 C37 1.484(3) . ?
C32 C33 1.400(3) . ?
C32 H32 0.9400 . ?
C33 N33 1.366(3) . ?
C33 C34 1.410(4) . ?
N33 C38 1.433(3) . ?
N33 C39 1.436(3) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C38 H38C 0.9700 . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C39 H39C 0.9700 . ?
C34 C35 1.365(4) . ?
C34 H34 0.9400 . ?
C35 C36 1.377(4) . ?
C35 H35 0.9400 . ?
C36 H36 0.9400 . ?
C37 O38 1.225(3) . ?
C37 O37 1.311(3) . ?
O37 H37 0.90(3) . ?
C41 C46 1.385(3) . ?
C41 C42 1.393(3) . ?
C41 C47 1.488(3) . ?
C42 C43 1.379(3) . ?
C42 H42 0.9400 . ?
C43 C44 1.376(4) . ?
C43 N43 1.464(3) . ?
N43 O43 1.205(3) . ?
N43 O44 1.215(3) . ?
C44 C45 1.364(3) . ?
C44 H44 0.9400 . ?
C45 C46 1.374(3) . ?
C45 N45 1.474(3) . ?
N45 O46 1.214(3) . ?
N45 O45 1.224(3) . ?
C46 H46 0.9400 . ?
C47 O48 1.204(3) . ?
C47 O47 1.302(3) . ?
O47 H47 0.94(3) . ?

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
C12 N11 C19 106.5(2) . . ?
C12 N11 C27 126.8(2) . . ?
C19 N11 C27 126.7(2) . . ?
N13 C12 N11 113.5(2) . . ?
N13 C12 H12 123.2 . . ?
N11 C12 H12 123.2 . . ?
C12 N13 C14 105.2(2) . . ?
C15 C14 C19 120.0(2) . . ?
C15 C14 N13 131.2(2) . . ?
C19 C14 N13 108.8(2) . . ?
C16 C15 C14 118.1(2) . . ?
C16 C15 H15 121.0 . . ?
C14 C15 H15 121.0 . . ?
C15 C16 C17 121.4(3) . . ?
C15 C16 H16 119.3 . . ?
C17 C16 H16 119.3 . . ?
C18 C17 C16 121.7(3) . . ?
C18 C17 H17 119.2 . . ?
C16 C17 H17 119.2 . . ?
C17 C18 C19 116.5(3) . . ?
C17 C18 H18 121.7 . . ?
C19 C18 H18 121.7 . . ?
N11 C19 C18 131.7(2) . . ?
N11 C19 C14 106.0(2) . . ?
C18 C19 C14 122.3(2) . . ?
C26 N21 C22 118.1(2) . . ?
N21 C22 C23 123.6(2) . . ?
N21 C22 H22 118.2 . . ?
C23 C22 H22 118.2 . . ?
C24 C23 C22 117.4(2) . . ?
C24 C23 C27 121.0(2) . . ?
C22 C23 C27 121.6(2) . . ?
C25 C24 C23 119.7(2) . . ?
C25 C24 H24 120.1 . . ?
C23 C24 H24 120.1 . . ?
C24 C25 C26 119.0(3) . . ?
C24 C25 H25 120.5 . . ?
C26 C25 H25 120.5 . . ?
N21 C26 C25 122.2(2) . . ?
N21 C26 H26 118.9 . . ?
C25 C26 H26 118.9 . . ?
N11 C27 C23 112.96(19) . . ?
N11 C27 H27A 109.0 . . ?
C23 C27 H27A 109.0 . . ?
N11 C27 H27B 109.0 . . ?
C23 C27 H27B 109.0 . . ?
H27A C27 H27B 107.8 . . ?
C32 C31 C36 121.1(2) . . ?
C32 C31 C37 118.1(2) . . ?
C36 C31 C37 120.7(2) . . ?
C31 C32 C33 121.0(2) . . ?
C31 C32 H32 119.5 . . ?
C33 C32 H32 119.5 . . ?
N33 C33 C32 121.8(2) . . ?
N33 C33 C34 121.2(2) . . ?
C32 C33 C34 117.0(2) . . ?
C33 N33 C38 120.9(2) . . ?
C33 N33 C39 120.3(2) . . ?
C38 N33 C39 117.7(2) . . ?
N33 C38 H38A 109.5 . . ?
N33 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
N33 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
N33 C39 H39A 109.5 . . ?
N33 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
N33 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C35 C34 C33 121.0(2) . . ?
C35 C34 H34 119.5 . . ?
C33 C34 H34 119.5 . . ?
C34 C35 C36 121.6(2) . . ?
C34 C35 H35 119.2 . . ?
C36 C35 H35 119.2 . . ?
C35 C36 C31 118.3(3) . . ?
C35 C36 H36 120.9 . . ?
C31 C36 H36 120.9 . . ?
O38 C37 O37 122.8(2) . . ?
O38 C37 C31 122.8(2) . . ?
O37 C37 C31 114.5(2) . . ?
C37 O37 H37 106.9(19) . . ?
C46 C41 C42 120.0(2) . . ?
C46 C41 C47 118.5(2) . . ?
C42 C41 C47 121.5(2) . . ?
C43 C42 C41 118.3(2) . . ?
C43 C42 H42 120.9 . . ?
C41 C42 H42 120.9 . . ?
C44 C43 C42 122.8(2) . . ?
C44 C43 N43 118.5(2) . . ?
C42 C43 N43 118.7(2) . . ?
O43 N43 O44 123.4(2) . . ?
O43 N43 C43 119.0(2) . . ?
O44 N43 C43 117.6(2) . . ?
C45 C44 C43 117.2(2) . . ?
C45 C44 H44 121.4 . . ?
C43 C44 H44 121.4 . . ?
C44 C45 C46 122.8(2) . . ?
C44 C45 N45 118.3(2) . . ?
C46 C45 N45 118.9(2) . . ?
O46 N45 O45 124.5(2) . . ?
O46 N45 C45 118.2(2) . . ?
O45 N45 C45 117.3(2) . . ?
C45 C46 C41 119.0(2) . . ?
C45 C46 H46 120.5 . . ?
C41 C46 H46 120.5 . . ?
O48 C47 O47 124.5(2) . . ?
O48 C47 C41 121.5(2) . . ?
O47 C47 C41 113.9(2) . . ?
C47 O47 H47 110.6(18) . . ?

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
C19 N11 C12 N13 0.3(3) . . . . ?
C27 N11 C12 N13 179.5(2) . . . . ?
N11 C12 N13 C14 0.4(3) . . . . ?
C12 N13 C14 C15 178.4(3) . . . . ?
C12 N13 C14 C19 -0.9(3) . . . . ?
C19 C14 C15 C16 -1.1(4) . . . . ?
N13 C14 C15 C16 179.6(2) . . . . ?
C14 C15 C16 C17 0.0(4) . . . . ?
C15 C16 C17 C18 0.5(5) . . . . ?
C16 C17 C18 C19 0.1(4) . . . . ?
C12 N11 C19 C18 179.0(3) . . . . ?
C27 N11 C19 C18 -0.2(4) . . . . ?
C12 N11 C19 C14 -0.9(3) . . . . ?
C27 N11 C19 C14 179.9(2) . . . . ?
C17 C18 C19 N11 178.9(3) . . . . ?
C17 C18 C19 C14 -1.2(4) . . . . ?
C15 C14 C19 N11 -178.3(2) . . . . ?
N13 C14 C19 N11 1.1(3) . . . . ?
C15 C14 C19 C18 1.8(4) . . . . ?
N13 C14 C19 C18 -178.8(2) . . . . ?
C26 N21 C22 C23 0.0(4) . . . . ?
N21 C22 C23 C24 -0.8(4) . . . . ?
N21 C22 C23 C27 -179.9(2) . . . . ?
C22 C23 C24 C25 0.9(4) . . . . ?
C27 C23 C24 C25 -180.0(2) . . . . ?
C23 C24 C25 C26 -0.3(4) . . . . ?
C22 N21 C26 C25 0.6(4) . . . . ?
C24 C25 C26 N21 -0.4(4) . . . . ?
C12 N11 C27 C23 -92.1(3) . . . . ?
C19 N11 C27 C23 87.0(3) . . . . ?
C24 C23 C27 N11 71.9(3) . . . . ?
C22 C23 C27 N11 -109.0(2) . . . . ?
C36 C31 C32 C33 0.4(4) . . . . ?
C37 C31 C32 C33 179.7(2) . . . . ?
C31 C32 C33 N33 179.1(2) . . . . ?
C31 C32 C33 C34 -0.5(3) . . . . ?
C32 C33 N33 C38 5.4(4) . . . . ?
C34 C33 N33 C38 -175.0(2) . . . . ?
C32 C33 N33 C39 173.6(2) . . . . ?
C34 C33 N33 C39 -6.8(4) . . . . ?
N33 C33 C34 C35 -179.0(2) . . . . ?
C32 C33 C34 C35 0.6(4) . . . . ?
C33 C34 C35 C36 -0.6(4) . . . . ?
C34 C35 C36 C31 0.4(4) . . . . ?
C32 C31 C36 C35 -0.3(4) . . . . ?
C37 C31 C36 C35 -179.6(2) . . . . ?
C32 C31 C37 O38 -2.4(4) . . . . ?
C36 C31 C37 O38 176.9(2) . . . . ?
C32 C31 C37 O37 177.7(2) . . . . ?
C36 C31 C37 O37 -3.0(3) . . . . ?
C46 C41 C42 C43 0.5(3) . . . . ?
C47 C41 C42 C43 179.8(2) . . . . ?
C41 C42 C43 C44 0.5(4) . . . . ?
C41 C42 C43 N43 -179.6(2) . . . . ?
C44 C43 N43 O43 -179.3(2) . . . . ?
C42 C43 N43 O43 0.7(3) . . . . ?
C44 C43 N43 O44 0.8(4) . . . . ?
C42 C43 N43 O44 -179.1(2) . . . . ?
C42 C43 C44 C45 -0.8(4) . . . . ?
N43 C43 C44 C45 179.3(2) . . . . ?
C43 C44 C45 C46 0.1(4) . . . . ?
C43 C44 C45 N45 -178.2(2) . . . . ?
C44 C45 N45 O46 171.3(2) . . . . ?
C46 C45 N45 O46 -7.1(3) . . . . ?
C44 C45 N45 O45 -8.2(3) . . . . ?
C46 C45 N45 O45 173.4(2) . . . . ?
C44 C45 C46 C41 0.8(4) . . . . ?
N45 C45 C46 C41 179.1(2) . . . . ?
C42 C41 C46 C45 -1.1(3) . . . . ?
C47 C41 C46 C45 179.5(2) . . . . ?
C46 C41 C47 O48 5.7(4) . . . . ?
C42 C41 C47 O48 -173.7(2) . . . . ?
C46 C41 C47 O47 -173.8(2) . . . . ?
C42 C41 C47 O47 6.8(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
O47 H47 N13 0.94(3) 1.71(3) 2.652(3) 175(3) .
O37 H37 N21 0.90(3) 1.78(3) 2.665(3) 166(3) .

_diffrn_measured_fraction_theta_max 0.948
_diffrn_reflns_theta_full        27.51
_diffrn_measured_fraction_theta_full 0.948
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.071

#END

data_3
_database_code_depnum_ccdc_archive 'CCDC 259795'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
1-(3-pyridylmethyl)-2-methyl-BzIm, 3,5-diNO2PhCOOH, 4-NO2PhCOOH
;
_chemical_name_common            
;1-(3-pyridylmethyl)-2-methyl-BzIm, 3,5-diNO2PhCOOH, 4-
NO2PhCOOH
;
_chemical_melting_point          ?
_chemical_formula_moiety         
;
(C14 H13 N3) (C7 H4 N2 O6) (C7 H5 N O4)
;
_chemical_formula_sum            'C28 H22 N6 O10'
_chemical_formula_weight         602.52

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           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   7.7318(8)
_cell_length_b                   7.0062(7)
_cell_length_c                   49.395(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.012(6)
_cell_angle_gamma                90.00
_cell_volume                     2675.3(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3473
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      25.50

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1248
_exptl_absorpt_coefficient_mu    0.116
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18644
_diffrn_reflns_av_R_equivalents  0.1180
_diffrn_reflns_av_sigmaI/netI    0.1172
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -65
_diffrn_reflns_limit_l_max       64
_diffrn_reflns_theta_min         1.65
_diffrn_reflns_theta_max         28.26
_reflns_number_total             6183
_reflns_number_gt                3208
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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^)+(0.0700P)^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       0.0202(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         6183
_refine_ls_number_parameters     404
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1162
_refine_ls_R_factor_gt           0.0613
_refine_ls_wR_factor_ref         0.1511
_refine_ls_wR_factor_gt          0.1298
_refine_ls_goodness_of_fit_ref   0.891
_refine_ls_restrained_S_all      0.891
_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
N11 N -0.0320(2) 0.6078(3) 0.36744(4) 0.0304(5) Uani 1 1 d . . .
C12 C -0.1101(3) 0.4346(3) 0.36862(5) 0.0309(6) Uani 1 1 d . . .
N13 N -0.1003(2) 0.3420(3) 0.34568(4) 0.0317(5) Uani 1 1 d . . .
C14 C -0.0130(3) 0.4608(3) 0.32804(5) 0.0295(5) Uani 1 1 d . . .
C15 C 0.0282(3) 0.4368(4) 0.30113(5) 0.0391(6) Uani 1 1 d . . .
H15 H 0.0028 0.3213 0.2918 0.047 Uiso 1 1 calc R . .
C16 C 0.1074(3) 0.5868(4) 0.28850(6) 0.0443(7) Uani 1 1 d . . .
H16 H 0.1361 0.5752 0.2700 0.053 Uiso 1 1 calc R . .
C17 C 0.1469(3) 0.7554(4) 0.30210(6) 0.0452(7) Uani 1 1 d . . .
H17 H 0.2015 0.8559 0.2926 0.054 Uiso 1 1 calc R . .
C18 C 0.1094(3) 0.7802(4) 0.32878(6) 0.0376(6) Uani 1 1 d . . .
H18 H 0.1372 0.8950 0.3381 0.045 Uiso 1 1 calc R . .
C19 C 0.0287(3) 0.6295(3) 0.34154(5) 0.0280(5) Uani 1 1 d . . .
C20 C -0.1993(3) 0.3636(4) 0.39293(5) 0.0416(7) Uani 1 1 d . . .
H20A H -0.2950 0.4495 0.3972 0.062 Uiso 1 1 calc R . .
H20B H -0.1173 0.3589 0.4083 0.062 Uiso 1 1 calc R . .
H20C H -0.2448 0.2352 0.3894 0.062 Uiso 1 1 calc R . .
N21 N 0.4014(2) 0.6264(3) 0.42514(4) 0.0356(5) Uani 1 1 d . . .
C22 C 0.2461(3) 0.6143(3) 0.41289(5) 0.0315(6) Uani 1 1 d . . .
H22 H 0.1883 0.4947 0.4129 0.038 Uiso 1 1 calc R . .
C23 C 0.1657(3) 0.7671(3) 0.40026(5) 0.0304(6) Uani 1 1 d . . .
C24 C 0.2528(3) 0.9382(4) 0.39984(5) 0.0363(6) Uani 1 1 d . . .
H24 H 0.2029 1.0460 0.3910 0.044 Uiso 1 1 calc R . .
C25 C 0.4136(3) 0.9518(4) 0.41235(5) 0.0401(7) Uani 1 1 d . . .
H25 H 0.4757 1.0687 0.4122 0.048 Uiso 1 1 calc R . .
C26 C 0.4818(3) 0.7947(4) 0.42487(5) 0.0376(6) Uani 1 1 d . . .
H26 H 0.5912 0.8057 0.4338 0.045 Uiso 1 1 calc R . .
C27 C -0.0150(3) 0.7494(4) 0.38883(5) 0.0370(6) Uani 1 1 d . . .
H27A H -0.0938 0.7152 0.4036 0.044 Uiso 1 1 calc R . .
H27B H -0.0520 0.8750 0.3816 0.044 Uiso 1 1 calc R . .
C31 C 0.7225(3) 0.2867(3) 0.49259(5) 0.0313(6) Uani 1 1 d . . .
C32 C 0.8359(3) 0.3572(4) 0.51209(5) 0.0356(6) Uani 1 1 d . . .
H32 H 0.8567 0.4907 0.5132 0.043 Uiso 1 1 calc R . .
C33 C 0.9187(3) 0.2363(3) 0.52994(5) 0.0324(6) Uani 1 1 d . . .
H33 H 1.0009 0.2833 0.5428 0.039 Uiso 1 1 calc R . .
C34 C 0.8791(3) 0.0454(3) 0.52863(5) 0.0291(5) Uani 1 1 d . . .
N34 N 0.9666(3) -0.0837(3) 0.54784(4) 0.0369(5) Uani 1 1 d . . .
O34 O 1.0815(2) -0.0186(3) 0.56244(4) 0.0435(5) Uani 1 1 d . . .
O35 O 0.9213(3) -0.2509(3) 0.54840(4) 0.0519(5) Uani 1 1 d . . .
C35 C 0.7645(3) -0.0292(4) 0.50997(5) 0.0333(6) Uani 1 1 d . . .
H35 H 0.7384 -0.1617 0.5098 0.040 Uiso 1 1 calc R . .
C36 C 0.6885(3) 0.0930(3) 0.49152(5) 0.0328(6) Uani 1 1 d . . .
H36 H 0.6120 0.0440 0.4779 0.039 Uiso 1 1 calc R . .
C37 C 0.6433(3) 0.4250(4) 0.47311(5) 0.0377(6) Uani 1 1 d . . .
O37 O 0.5323(2) 0.3505(3) 0.45562(4) 0.0437(5) Uani 1 1 d . . .
H37 H 0.479(3) 0.462(4) 0.4430(6) 0.052 Uiso 1 1 d . . .
O38 O 0.6800(3) 0.5931(3) 0.47352(4) 0.0616(6) Uani 1 1 d . . .
C41 C 0.6157(3) 0.7561(3) 0.32564(5) 0.0284(5) Uani 1 1 d . . .
C42 C 0.6539(3) 0.7219(3) 0.29885(5) 0.0299(6) Uani 1 1 d . . .
H42 H 0.7146 0.8140 0.2886 0.036 Uiso 1 1 calc R . .
C43 C 0.6025(3) 0.5526(4) 0.28731(5) 0.0337(6) Uani 1 1 d . . .
N43 N 0.6469(3) 0.5146(4) 0.25913(5) 0.0497(6) Uani 1 1 d . . .
O43 O 0.7285(3) 0.6335(3) 0.24688(4) 0.0559(6) Uani 1 1 d . . .
O44 O 0.6030(4) 0.3621(4) 0.24961(5) 0.1044(11) Uani 1 1 d . . .
C44 C 0.5131(3) 0.4153(4) 0.30112(5) 0.0334(6) Uani 1 1 d . . .
H44 H 0.4785 0.2991 0.2927 0.040 Uiso 1 1 calc R . .
C45 C 0.4758(3) 0.4542(3) 0.32769(5) 0.0290(5) Uani 1 1 d . . .
N45 N 0.3813(3) 0.3105(3) 0.34311(5) 0.0375(5) Uani 1 1 d . . .
O45 O 0.3364(2) 0.1652(2) 0.33149(4) 0.0484(5) Uani 1 1 d . . .
O46 O 0.3520(3) 0.3453(3) 0.36680(4) 0.0524(5) Uani 1 1 d . . .
C46 C 0.5254(3) 0.6209(3) 0.34011(5) 0.0302(6) Uani 1 1 d . . .
H46 H 0.4980 0.6433 0.3585 0.036 Uiso 1 1 calc R . .
C47 C 0.6761(3) 0.9324(3) 0.33957(5) 0.0315(6) Uani 1 1 d . . .
O47 O 0.7492(2) 1.0554(3) 0.32372(4) 0.0392(5) Uani 1 1 d . . .
H47 H 0.804(3) 1.164(4) 0.3343(5) 0.047 Uiso 1 1 d . . .
O48 O 0.6600(2) 0.9527(3) 0.36375(4) 0.0422(5) 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
N11 0.0347(10) 0.0256(11) 0.0308(12) -0.0028(9) -0.0035(9) -0.0003(9)
C12 0.0297(11) 0.0275(13) 0.0352(15) 0.0012(12) -0.0043(11) 0.0016(10)
N13 0.0312(10) 0.0280(11) 0.0361(13) -0.0030(10) -0.0013(9) -0.0028(9)
C14 0.0280(11) 0.0305(13) 0.0299(14) -0.0024(11) -0.0040(10) 0.0010(10)
C15 0.0340(12) 0.0447(16) 0.0384(16) -0.0049(13) -0.0044(12) 0.0007(12)
C16 0.0398(14) 0.061(2) 0.0318(16) 0.0046(14) 0.0014(12) 0.0026(14)
C17 0.0377(14) 0.0502(18) 0.0476(19) 0.0111(15) -0.0001(13) -0.0039(13)
C18 0.0352(13) 0.0325(15) 0.0449(18) 0.0047(13) -0.0047(12) -0.0037(11)
C19 0.0253(11) 0.0276(13) 0.0308(14) 0.0009(11) -0.0040(10) 0.0005(10)
C20 0.0465(14) 0.0410(16) 0.0374(16) 0.0018(13) 0.0014(13) -0.0062(12)
N21 0.0378(11) 0.0364(13) 0.0325(13) -0.0049(10) -0.0028(9) -0.0027(9)
C22 0.0362(12) 0.0263(13) 0.0321(15) -0.0034(11) 0.0013(11) -0.0029(10)
C23 0.0368(12) 0.0301(14) 0.0243(13) -0.0053(11) -0.0015(10) -0.0013(11)
C24 0.0454(14) 0.0326(14) 0.0308(15) -0.0028(12) -0.0004(12) -0.0025(12)
C25 0.0442(14) 0.0365(15) 0.0397(17) -0.0015(13) 0.0066(12) -0.0137(12)
C26 0.0347(13) 0.0449(17) 0.0331(15) -0.0060(13) -0.0005(11) -0.0105(12)
C27 0.0391(13) 0.0330(15) 0.0387(16) -0.0105(12) -0.0054(12) 0.0025(11)
C31 0.0327(12) 0.0303(14) 0.0311(14) -0.0044(11) 0.0034(11) -0.0031(10)
C32 0.0430(13) 0.0297(14) 0.0342(15) -0.0048(12) -0.0006(12) -0.0074(11)
C33 0.0382(13) 0.0303(14) 0.0286(14) -0.0038(11) -0.0015(11) -0.0042(11)
C34 0.0322(11) 0.0305(13) 0.0248(13) -0.0027(11) 0.0053(10) 0.0013(10)
N34 0.0460(12) 0.0297(13) 0.0351(13) -0.0013(10) 0.0070(10) 0.0022(10)
O34 0.0495(10) 0.0441(12) 0.0366(11) -0.0029(9) -0.0101(9) -0.0007(9)
O35 0.0691(13) 0.0315(11) 0.0549(14) 0.0060(10) -0.0044(10) -0.0046(10)
C35 0.0357(12) 0.0276(13) 0.0368(15) -0.0047(12) 0.0068(11) -0.0046(11)
C36 0.0323(12) 0.0333(14) 0.0330(15) -0.0058(12) 0.0019(11) -0.0050(11)
C37 0.0370(13) 0.0346(16) 0.0414(17) -0.0055(13) -0.0003(12) -0.0032(11)
O37 0.0479(10) 0.0357(11) 0.0467(12) -0.0016(9) -0.0163(9) -0.0057(9)
O38 0.0773(14) 0.0339(12) 0.0723(16) 0.0064(10) -0.0363(12) -0.0111(10)
C41 0.0303(11) 0.0254(13) 0.0292(14) -0.0016(11) -0.0044(10) 0.0025(10)
C42 0.0263(11) 0.0320(14) 0.0311(14) 0.0011(11) -0.0042(10) -0.0006(10)
C43 0.0321(12) 0.0362(15) 0.0329(15) -0.0061(12) -0.0007(11) -0.0017(11)
N43 0.0463(13) 0.0642(18) 0.0386(15) -0.0167(14) 0.0028(11) -0.0124(12)
O43 0.0649(13) 0.0674(15) 0.0355(12) -0.0022(11) 0.0099(10) -0.0044(11)
O44 0.126(2) 0.115(2) 0.0737(18) -0.0657(17) 0.0462(16) -0.0716(19)
C44 0.0311(12) 0.0286(14) 0.0404(16) -0.0078(12) -0.0057(11) -0.0001(10)
C45 0.0298(11) 0.0240(13) 0.0330(15) 0.0022(11) -0.0033(10) 0.0017(10)
N45 0.0390(11) 0.0280(12) 0.0454(15) 0.0021(11) -0.0033(11) 0.0006(9)
O45 0.0510(11) 0.0290(10) 0.0650(14) -0.0042(10) -0.0046(10) -0.0104(9)
O46 0.0742(13) 0.0419(12) 0.0415(13) 0.0034(10) 0.0120(10) -0.0079(10)
C46 0.0324(12) 0.0301(13) 0.0281(14) -0.0016(11) -0.0030(11) 0.0026(10)
C47 0.0315(12) 0.0279(14) 0.0350(16) -0.0030(12) -0.0045(11) 0.0029(10)
O47 0.0482(10) 0.0300(10) 0.0394(11) -0.0037(9) -0.0012(9) -0.0093(8)
O48 0.0523(11) 0.0386(11) 0.0356(12) -0.0093(9) 0.0004(9) -0.0061(9)

_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
N11 C12 1.357(3) . ?
N11 C19 1.379(3) . ?
N11 C27 1.454(3) . ?
C12 N13 1.309(3) . ?
C12 C20 1.482(4) . ?
N13 C14 1.388(3) . ?
C14 C15 1.383(3) . ?
C14 C19 1.392(3) . ?
C15 C16 1.373(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.390(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.366(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.384(3) . ?
C18 H18 0.9500 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
N21 C26 1.333(3) . ?
N21 C22 1.338(3) . ?
C22 C23 1.381(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.375(3) . ?
C23 C27 1.503(3) . ?
C24 C25 1.381(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.364(4) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C31 C32 1.382(3) . ?
C31 C36 1.384(3) . ?
C31 C37 1.490(4) . ?
C32 C33 1.373(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.373(3) . ?
C33 H33 0.9500 . ?
C34 C35 1.371(3) . ?
C34 N34 1.468(3) . ?
N34 O34 1.222(2) . ?
N34 O35 1.223(3) . ?
C35 C36 1.375(3) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 O38 1.211(3) . ?
C37 O37 1.315(3) . ?
O37 H37 1.08(3) . ?
C41 C42 1.382(3) . ?
C41 C46 1.383(3) . ?
C41 C47 1.485(3) . ?
C42 C43 1.371(3) . ?
C42 H42 0.9500 . ?
C43 C44 1.373(3) . ?
C43 N43 1.464(3) . ?
N43 O43 1.213(3) . ?
N43 O44 1.213(3) . ?
C44 C45 1.376(3) . ?
C44 H44 0.9500 . ?
C45 C46 1.370(3) . ?
C45 N45 1.466(3) . ?
N45 O45 1.216(3) . ?
N45 O46 1.220(3) . ?
C46 H46 0.9500 . ?
C47 O48 1.212(3) . ?
C47 O47 1.300(3) . ?
O47 H47 1.01(3) . ?

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
C12 N11 C19 107.29(19) . . ?
C12 N11 C27 127.9(2) . . ?
C19 N11 C27 124.8(2) . . ?
N13 C12 N11 111.9(2) . . ?
N13 C12 C20 124.7(2) . . ?
N11 C12 C20 123.3(2) . . ?
C12 N13 C14 106.4(2) . . ?
C15 C14 N13 130.8(2) . . ?
C15 C14 C19 120.6(2) . . ?
N13 C14 C19 108.6(2) . . ?
C16 C15 C14 117.1(3) . . ?
C16 C15 H15 121.4 . . ?
C14 C15 H15 121.4 . . ?
C15 C16 C17 121.8(3) . . ?
C15 C16 H16 119.1 . . ?
C17 C16 H16 119.1 . . ?
C18 C17 C16 121.7(3) . . ?
C18 C17 H17 119.1 . . ?
C16 C17 H17 119.1 . . ?
C17 C18 C19 116.6(3) . . ?
C17 C18 H18 121.7 . . ?
C19 C18 H18 121.7 . . ?
N11 C19 C18 132.1(2) . . ?
N11 C19 C14 105.7(2) . . ?
C18 C19 C14 122.2(2) . . ?
C12 C20 H20A 109.5 . . ?
C12 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C12 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C26 N21 C22 117.8(2) . . ?
N21 C22 C23 123.3(2) . . ?
N21 C22 H22 118.4 . . ?
C23 C22 H22 118.4 . . ?
C24 C23 C22 117.7(2) . . ?
C24 C23 C27 121.2(2) . . ?
C22 C23 C27 120.9(2) . . ?
C23 C24 C25 119.4(2) . . ?
C23 C24 H24 120.3 . . ?
C25 C24 H24 120.3 . . ?
C26 C25 C24 119.0(2) . . ?
C26 C25 H25 120.5 . . ?
C24 C25 H25 120.5 . . ?
N21 C26 C25 122.8(2) . . ?
N21 C26 H26 118.6 . . ?
C25 C26 H26 118.6 . . ?
N11 C27 C23 113.6(2) . . ?
N11 C27 H27A 108.8 . . ?
C23 C27 H27A 108.8 . . ?
N11 C27 H27B 108.8 . . ?
C23 C27 H27B 108.8 . . ?
H27A C27 H27B 107.7 . . ?
C32 C31 C36 119.7(2) . . ?
C32 C31 C37 117.8(2) . . ?
C36 C31 C37 122.5(2) . . ?
C33 C32 C31 120.6(2) . . ?
C33 C32 H32 119.7 . . ?
C31 C32 H32 119.7 . . ?
C32 C33 C34 118.0(2) . . ?
C32 C33 H33 121.0 . . ?
C34 C33 H33 121.0 . . ?
C35 C34 C33 122.9(2) . . ?
C35 C34 N34 119.0(2) . . ?
C33 C34 N34 118.0(2) . . ?
O34 N34 O35 123.3(2) . . ?
O34 N34 C34 118.3(2) . . ?
O35 N34 C34 118.4(2) . . ?
C34 C35 C36 118.2(2) . . ?
C34 C35 H35 120.9 . . ?
C36 C35 H35 120.9 . . ?
C35 C36 C31 120.4(2) . . ?
C35 C36 H36 119.8 . . ?
C31 C36 H36 119.8 . . ?
O38 C37 O37 123.2(2) . . ?
O38 C37 C31 121.9(2) . . ?
O37 C37 C31 115.0(2) . . ?
C37 O37 H37 109.4(15) . . ?
C42 C41 C46 119.6(2) . . ?
C42 C41 C47 121.2(2) . . ?
C46 C41 C47 119.2(2) . . ?
C43 C42 C41 118.9(2) . . ?
C43 C42 H42 120.6 . . ?
C41 C42 H42 120.6 . . ?
C42 C43 C44 122.9(2) . . ?
C42 C43 N43 118.8(2) . . ?
C44 C43 N43 118.3(2) . . ?
O43 N43 O44 123.8(3) . . ?
O43 N43 C43 118.8(2) . . ?
O44 N43 C43 117.4(3) . . ?
C43 C44 C45 116.8(2) . . ?
C43 C44 H44 121.6 . . ?
C45 C44 H44 121.6 . . ?
C46 C45 C44 122.3(2) . . ?
C46 C45 N45 119.4(2) . . ?
C44 C45 N45 118.3(2) . . ?
O45 N45 O46 124.3(2) . . ?
O45 N45 C45 118.1(2) . . ?
O46 N45 C45 117.7(2) . . ?
C45 C46 C41 119.5(2) . . ?
C45 C46 H46 120.3 . . ?
C41 C46 H46 120.3 . . ?
O48 C47 O47 124.7(2) . . ?
O48 C47 C41 121.2(2) . . ?
O47 C47 C41 114.1(2) . . ?
C47 O47 H47 111.7(15) . . ?

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
C19 N11 C12 N13 1.6(3) . . . . ?
C27 N11 C12 N13 -179.3(2) . . . . ?
C19 N11 C12 C20 -176.9(2) . . . . ?
C27 N11 C12 C20 2.2(4) . . . . ?
N11 C12 N13 C14 -0.9(3) . . . . ?
C20 C12 N13 C14 177.5(2) . . . . ?
C12 N13 C14 C15 -177.9(2) . . . . ?
C12 N13 C14 C19 -0.1(2) . . . . ?
N13 C14 C15 C16 176.1(2) . . . . ?
C19 C14 C15 C16 -1.4(3) . . . . ?
C14 C15 C16 C17 0.7(4) . . . . ?
C15 C16 C17 C18 0.2(4) . . . . ?
C16 C17 C18 C19 -0.5(4) . . . . ?
C12 N11 C19 C18 176.1(2) . . . . ?
C27 N11 C19 C18 -3.0(4) . . . . ?
C12 N11 C19 C14 -1.6(2) . . . . ?
C27 N11 C19 C14 179.33(19) . . . . ?
C17 C18 C19 N11 -177.5(2) . . . . ?
C17 C18 C19 C14 -0.1(3) . . . . ?
C15 C14 C19 N11 179.1(2) . . . . ?
N13 C14 C19 N11 1.1(2) . . . . ?
C15 C14 C19 C18 1.1(3) . . . . ?
N13 C14 C19 C18 -176.9(2) . . . . ?
C26 N21 C22 C23 -0.4(4) . . . . ?
N21 C22 C23 C24 1.6(4) . . . . ?
N21 C22 C23 C27 -174.9(2) . . . . ?
C22 C23 C24 C25 -1.3(4) . . . . ?
C27 C23 C24 C25 175.2(2) . . . . ?
C23 C24 C25 C26 -0.1(4) . . . . ?
C22 N21 C26 C25 -1.1(4) . . . . ?
C24 C25 C26 N21 1.4(4) . . . . ?
C12 N11 C27 C23 108.0(3) . . . . ?
C19 N11 C27 C23 -73.1(3) . . . . ?
C24 C23 C27 N11 121.9(3) . . . . ?
C22 C23 C27 N11 -61.7(3) . . . . ?
C36 C31 C32 C33 1.8(4) . . . . ?
C37 C31 C32 C33 -177.3(2) . . . . ?
C31 C32 C33 C34 -3.1(4) . . . . ?
C32 C33 C34 C35 1.6(4) . . . . ?
C32 C33 C34 N34 -179.6(2) . . . . ?
C35 C34 N34 O34 172.4(2) . . . . ?
C33 C34 N34 O34 -6.4(3) . . . . ?
C35 C34 N34 O35 -7.4(3) . . . . ?
C33 C34 N34 O35 173.7(2) . . . . ?
C33 C34 C35 C36 1.1(4) . . . . ?
N34 C34 C35 C36 -177.7(2) . . . . ?
C34 C35 C36 C31 -2.4(4) . . . . ?
C32 C31 C36 C35 1.0(4) . . . . ?
C37 C31 C36 C35 -179.9(2) . . . . ?
C32 C31 C37 O38 2.4(4) . . . . ?
C36 C31 C37 O38 -176.7(3) . . . . ?
C32 C31 C37 O37 -177.8(2) . . . . ?
C36 C31 C37 O37 3.1(4) . . . . ?
C46 C41 C42 C43 -0.7(3) . . . . ?
C47 C41 C42 C43 176.8(2) . . . . ?
C41 C42 C43 C44 0.6(4) . . . . ?
C41 C42 C43 N43 -178.5(2) . . . . ?
C42 C43 N43 O43 0.4(3) . . . . ?
C44 C43 N43 O43 -178.7(2) . . . . ?
C42 C43 N43 O44 178.5(3) . . . . ?
C44 C43 N43 O44 -0.6(4) . . . . ?
C42 C43 C44 C45 -0.1(3) . . . . ?
N43 C43 C44 C45 179.0(2) . . . . ?
C43 C44 C45 C46 -0.3(3) . . . . ?
C43 C44 C45 N45 -179.7(2) . . . . ?
C46 C45 N45 O45 178.9(2) . . . . ?
C44 C45 N45 O45 -1.8(3) . . . . ?
C46 C45 N45 O46 -0.8(3) . . . . ?
C44 C45 N45 O46 178.6(2) . . . . ?
C44 C45 C46 C41 0.2(3) . . . . ?
N45 C45 C46 C41 179.56(19) . . . . ?
C42 C41 C46 C45 0.3(3) . . . . ?
C47 C41 C46 C45 -177.19(19) . . . . ?
C42 C41 C47 O48 -171.5(2) . . . . ?
C46 C41 C47 O48 6.0(3) . . . . ?
C42 C41 C47 O47 6.9(3) . . . . ?
C46 C41 C47 O47 -175.62(19) . . . . ?

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
O47 H47 N13 1.01(3) 1.55(3) 2.553(3) 170(2) 1_665
O37 H37 N21 1.08(3) 1.56(3) 2.641(3) 179(2) .

_diffrn_measured_fraction_theta_max 0.932
_diffrn_reflns_theta_full        28.26
_diffrn_measured_fraction_theta_full 0.932
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.090

#END