# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2014

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#                                CCDC 
# 
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#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
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#  fide research purposes only. It may contain copyright material
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data_2cp55m

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            
'C-methylpyrogallol[4]arene with 1-(2-pyridylazo)-2-napthol'
_chemical_formula_moiety         
'C32 H32 O12, 3(C15 H11 O1 N3), C1 H4 O1, H2 O1'
_chemical_formula_sum            'C78 H71 N9 O17'
_chemical_melting_point          ?

_exptl_crystal_description       prism
_exptl_crystal_colour            orange

_diffrn_ambient_temperature      173(2)
_chemical_formula_weight         1406.44

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   'C 2/c'
_symmetry_int_tables_number      15
_chemical_absolute_configuration ?

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

_cell_length_a                   22.950(4)
_cell_length_b                   34.573(5)
_cell_length_c                   17.549(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.677(2)
_cell_angle_gamma                90.00
_cell_volume                     13469(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3802
_cell_measurement_theta_min      2.2
_cell_measurement_theta_max      19.8
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5904
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_process_details   
;
 Data were corrected for decay and absorption using the program SADABS 
 (Sheldrick, G. M. (2003). SADABS. Version 2.10. University of
 Göttingen, Germany).
;

_exptl_special_details           
; 
 ? 
;
_diffrn_radiation_probe          ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 3802
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.0
_diffrn_reflns_number            79749
_diffrn_reflns_av_R_equivalents  0.1207
_diffrn_reflns_av_sigmaI/netI    0.1080
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.68
_diffrn_reflns_theta_max         27.64
_reflns_number_total             15605
_reflns_number_gt                7448
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2008)'
_computing_structure_solution    'SHELXS-1997 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-1997 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-SEED, Barbour, 2001'
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. There is a disordered oxygen
 atom that is water. The hydrogens were not modeled but were included in the 
 molecular formula.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0647P)²+0.0000P] where P=(Fo²+2Fc²)/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         15605
_refine_ls_number_parameters     956
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1572
_refine_ls_R_factor_gt           0.0619
_refine_ls_wR_factor_ref         0.1620
_refine_ls_wR_factor_gt          0.1255
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_restrained_S_all      0.990
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.14563(9) 0.42939(6) 0.19399(12) 0.0390(5) Uani 1 1 d . . .
H1 H 0.1596 0.4497 0.1791 0.047 Uiso 1 1 calc R . .
N1 N 0.42979(10) 0.34725(7) 0.18091(14) 0.0342(6) Uani 1 1 d . . .
C1 C 0.21631(11) 0.36696(8) 0.35930(16) 0.0265(6) Uani 1 1 d . . .
H13 H 0.2120 0.3414 0.3769 0.032 Uiso 1 1 calc R . .
O2 O 0.23612(10) 0.47705(6) 0.27998(14) 0.0476(6) Uani 1 1 d . . .
H2 H 0.2637 0.4887 0.3126 0.057 Uiso 1 1 calc R . .
N2 N 0.43150(11) 0.41338(7) 0.17446(15) 0.0382(6) Uani 1 1 d . . .
H2A H 0.4612 0.4113 0.1513 0.046 Uiso 1 1 calc R . .
C2 C 0.17702(12) 0.37921(8) 0.28885(16) 0.0262(6) Uani 1 1 d . . .
O3 O 0.31093(9) 0.45352(5) 0.41401(13) 0.0384(5) Uani 1 1 d . . .
H3 H 0.3442 0.4422 0.4302 0.046 Uiso 1 1 calc R . .
N3 N 0.41183(11) 0.44763(7) 0.18897(15) 0.0373(6) Uani 1 1 d . . .
C3 C 0.18380(12) 0.41677(8) 0.26379(17) 0.0317(7) Uani 1 1 d . . .
O4 O 0.40769(9) 0.40732(5) 0.44471(13) 0.0364(5) Uani 1 1 d . . .
H4 H 0.4370 0.4137 0.4269 0.044 Uiso 1 1 calc R . .
N4 N 0.65641(12) 0.01291(7) 0.59195(16) 0.0408(7) Uani 1 1 d . . .
C4 C 0.22914(13) 0.44034(8) 0.30765(19) 0.0331(7) Uani 1 1 d . . .
O5 O 0.49139(9) 0.36516(5) 0.40175(13) 0.0375(5) Uani 1 1 d . . .
H5 H 0.5099 0.3503 0.3780 0.045 Uiso 1 1 calc R . .
N5 N 0.56626(12) 0.03837(7) 0.52086(16) 0.0436(7) Uani 1 1 d . . .
H5A H 0.5671 0.0543 0.5602 0.052 Uiso 1 1 calc R . .
C5 C 0.26777(12) 0.42712(8) 0.37664(17) 0.0285(7) Uani 1 1 d . . .
O6 O 0.48623(8) 0.28641(5) 0.39449(11) 0.0315(5) Uani 1 1 d . . .
H6 H 0.5199 0.2946 0.4202 0.038 Uiso 1 1 calc R . .
N6 N 0.52171(12) 0.03991(8) 0.45622(16) 0.0420(7) Uani 1 1 d . . .
C6 C 0.26138(12) 0.39019(8) 0.40510(17) 0.0267(6) Uani 1 1 d . . .
O7 O 0.46957(8) 0.20963(6) 0.35518(12) 0.0363(5) Uani 1 1 d . . .
H7 H 0.4882 0.1986 0.3259 0.044 Uiso 1 1 calc R . .
N7 N 0.70775(11) 0.39380(7) 0.48208(15) 0.0376(6) Uani 1 1 d . . .
C7 C 0.30399(12) 0.37540(8) 0.48152(16) 0.0283(7) Uani 1 1 d . . .
H16 H 0.3242 0.3986 0.5106 0.034 Uiso 1 1 calc R . .
O8 O 0.42967(8) 0.18127(6) 0.20626(12) 0.0374(5) Uani 1 1 d . . .
H8 H 0.4121 0.1709 0.1633 0.045 Uiso 1 1 calc R . .
N8 N 0.64448(10) 0.34927(7) 0.51383(14) 0.0331(6) Uani 1 1 d . . .
H8A H 0.6617 0.3319 0.4900 0.040 Uiso 1 1 calc R . .
C8 C 0.35101(12) 0.30985(8) 0.46178(15) 0.0273(6) Uani 1 1 d . . .
H17 H 0.3182 0.2976 0.4758 0.033 Uiso 1 1 calc R . .
O9 O 0.30969(9) 0.17838(5) 0.13363(11) 0.0347(5) Uani 1 1 d . . .
H9 H 0.2896 0.1941 0.1007 0.042 Uiso 1 1 calc R . .
N9 N 0.60258(10) 0.33838(7) 0.54994(13) 0.0306(6) Uani 1 1 d . . .
C9 C 0.35342(11) 0.35031(8) 0.46305(15) 0.0249(6) Uani 1 1 d . . .
O10 O 0.25993(9) 0.24935(5) 0.08525(11) 0.0306(5) Uani 1 1 d . . .
H10 H 0.2824 0.2623 0.0639 0.037 Uiso 1 1 calc R . .
C10 C 0.40214(12) 0.36730(8) 0.44339(16) 0.0279(6) Uani 1 1 d . . .
O11 O 0.23987(9) 0.32358(5) 0.03480(11) 0.0334(5) Uani 1 1 d . . .
H11 H 0.2477 0.3473 0.0391 0.040 Uiso 1 1 calc R . .
C11 C 0.44549(11) 0.34543(8) 0.42078(16) 0.0259(6) Uani 1 1 d . . .
O12 O 0.17606(9) 0.37281(5) 0.10065(12) 0.0382(5) Uani 1 1 d . . .
H12 H 0.1621 0.3873 0.1302 0.046 Uiso 1 1 calc R . .
C12 C 0.44127(12) 0.30531(8) 0.41893(16) 0.0273(6) Uani 1 1 d . . .
O13 O 0.50585(10) 0.44872(6) 0.10921(15) 0.0552(7) Uani 1 1 d . . .
C13 C 0.39425(12) 0.28653(8) 0.44106(15) 0.0254(6) Uani 1 1 d . . .
O14 O 0.52178(11) 0.09977(7) 0.56898(15) 0.0584(7) Uani 1 1 d . . .
C14 C 0.39080(12) 0.24250(7) 0.44159(15) 0.0263(6) Uani 1 1 d . . .
H14 H 0.4327 0.2328 0.4638 0.032 Uiso 1 1 calc R . .
O15 O 0.64921(8) 0.28013(6) 0.46694(12) 0.0360(5) Uani 1 1 d . . .
C15 C 0.30834(12) 0.22746(7) 0.31886(16) 0.0250(6) Uani 1 1 d . . .
H15 H 0.2812 0.2395 0.3444 0.030 Uiso 1 1 calc R . .
C16 C 0.36929(12) 0.22591(7) 0.35855(15) 0.0247(6) Uani 1 1 d . . .
C17 C 0.40825(11) 0.20989(7) 0.31858(16) 0.0259(6) Uani 1 1 d . . .
C18 C 0.38734(12) 0.19526(8) 0.24296(16) 0.0263(6) Uani 1 1 d . . .
C19 C 0.32617(12) 0.19572(8) 0.20677(16) 0.0266(6) Uani 1 1 d . . .
C20 C 0.28548(11) 0.21236(7) 0.24423(16) 0.0242(6) Uani 1 1 d . . .
C21 C 0.21855(11) 0.21669(7) 0.20442(15) 0.0233(6) Uani 1 1 d . . .
H21 H 0.2102 0.2014 0.1545 0.028 Uiso 1 1 calc R . .
C22 C 0.17352(11) 0.28455(8) 0.21813(16) 0.0248(6) Uani 1 1 d . . .
H22 H 0.1584 0.2751 0.2602 0.030 Uiso 1 1 calc R . .
C23 C 0.20500(11) 0.25904(7) 0.18155(15) 0.0226(6) Uani 1 1 d . . .
C24 C 0.22815(11) 0.27387(8) 0.12122(15) 0.0242(6) Uani 1 1 d . . .
C25 C 0.21803(11) 0.31183(8) 0.09661(15) 0.0255(6) Uani 1 1 d . . .
C26 C 0.18523(12) 0.33618(8) 0.13318(16) 0.0257(6) Uani 1 1 d . . .
C27 C 0.16312(11) 0.32331(8) 0.19598(16) 0.0248(6) Uani 1 1 d . . .
C28 C 0.13097(12) 0.35157(8) 0.23823(16) 0.0268(6) Uani 1 1 d . . .
H28 H 0.1034 0.3675 0.1968 0.032 Uiso 1 1 calc R . .
C29 C 0.27012(13) 0.35545(8) 0.53521(17) 0.0364(7) Uani 1 1 d . . .
H29A H 0.2481 0.3331 0.5079 0.055 Uiso 1 1 calc R . .
H29B H 0.2416 0.3737 0.5487 0.055 Uiso 1 1 calc R . .
H29C H 0.2989 0.3468 0.5835 0.055 Uiso 1 1 calc R . .
C30 C 0.35205(12) 0.22710(8) 0.49498(17) 0.0332(7) Uani 1 1 d . . .
H30A H 0.3096 0.2331 0.4712 0.050 Uiso 1 1 calc R . .
H30B H 0.3647 0.2394 0.5469 0.050 Uiso 1 1 calc R . .
H30C H 0.3572 0.1990 0.5008 0.050 Uiso 1 1 calc R . .
C31 C 0.17941(12) 0.19987(8) 0.25502(16) 0.0307(7) Uani 1 1 d . . .
H31A H 0.1368 0.2024 0.2270 0.046 Uiso 1 1 calc R . .
H31B H 0.1870 0.2140 0.3050 0.046 Uiso 1 1 calc R . .
H31C H 0.1893 0.1725 0.2654 0.046 Uiso 1 1 calc R . .
C32 C 0.09215(12) 0.33201(8) 0.28589(17) 0.0308(7) Uani 1 1 d . . .
H32A H 0.1178 0.3166 0.3282 0.046 Uiso 1 1 calc R . .
H32B H 0.0627 0.3151 0.2513 0.046 Uiso 1 1 calc R . .
H32C H 0.0710 0.3518 0.3087 0.046 Uiso 1 1 calc R . .
C33 C 0.48255(14) 0.47959(9) 0.12519(19) 0.0412(8) Uani 1 1 d . . .
C34 C 0.50111(16) 0.51642(10) 0.1012(2) 0.0538(10) Uani 1 1 d . . .
H34 H 0.5313 0.5173 0.0729 0.065 Uiso 1 1 calc R . .
C35 C 0.47671(18) 0.54942(11) 0.1180(2) 0.0644(11) Uani 1 1 d . . .
H35 H 0.4898 0.5731 0.1003 0.077 Uiso 1 1 calc R . .
C36 C 0.43161(16) 0.55072(9) 0.1615(2) 0.0543(10) Uani 1 1 d . . .
C37 C 0.4077(2) 0.58541(11) 0.1802(3) 0.0861(15) Uani 1 1 d . . .
H37 H 0.4213 0.6091 0.1634 0.103 Uiso 1 1 calc R . .
C38 C 0.3655(2) 0.58609(13) 0.2217(3) 0.0956(16) Uani 1 1 d . . .
H38 H 0.3501 0.6102 0.2340 0.115 Uiso 1 1 calc R . .
C39 C 0.34440(18) 0.55201(11) 0.2465(3) 0.0739(13) Uani 1 1 d . . .
H39 H 0.3144 0.5527 0.2753 0.089 Uiso 1 1 calc R . .
C40 C 0.36707(16) 0.51728(10) 0.2294(2) 0.0558(10) Uani 1 1 d . . .
H40 H 0.3527 0.4939 0.2466 0.067 Uiso 1 1 calc R . .
C41 C 0.41096(14) 0.51576(9) 0.1872(2) 0.0424(8) Uani 1 1 d . . .
C42 C 0.43577(13) 0.47932(9) 0.16710(19) 0.0372(7) Uani 1 1 d . . .
C43 C 0.40447(12) 0.38016(8) 0.19653(17) 0.0310(7) Uani 1 1 d . . .
C44 C 0.35637(13) 0.38172(9) 0.23053(18) 0.0387(8) Uani 1 1 d . . .
H44 H 0.3400 0.4058 0.2410 0.046 Uiso 1 1 calc R . .
C45 C 0.33301(13) 0.34727(10) 0.24870(18) 0.0413(8) Uani 1 1 d . . .
H45 H 0.2995 0.3472 0.2713 0.050 Uiso 1 1 calc R . .
C46 C 0.35883(13) 0.31270(9) 0.23376(17) 0.0394(8) Uani 1 1 d . . .
H46 H 0.3437 0.2886 0.2465 0.047 Uiso 1 1 calc R . .
C47 C 0.40651(13) 0.31399(9) 0.20036(17) 0.0370(8) Uani 1 1 d . . .
H47 H 0.4241 0.2903 0.1904 0.044 Uiso 1 1 calc R . .
C48 C 0.61180(12) 0.27154(8) 0.50518(16) 0.0292(7) Uani 1 1 d . . .
C49 C 0.59274(12) 0.23214(8) 0.51002(16) 0.0307(7) Uani 1 1 d . . .
H49 H 0.6076 0.2126 0.4820 0.037 Uiso 1 1 calc R . .
C50 C 0.55459(12) 0.22256(8) 0.55309(16) 0.0312(7) Uani 1 1 d . . .
H50 H 0.5453 0.1960 0.5579 0.037 Uiso 1 1 calc R . .
C51 C 0.52697(12) 0.25129(8) 0.59275(16) 0.0281(6) Uani 1 1 d . . .
C52 C 0.48393(12) 0.24057(9) 0.63269(16) 0.0333(7) Uani 1 1 d . . .
H52 H 0.4754 0.2139 0.6378 0.040 Uiso 1 1 calc R . .
C53 C 0.45379(13) 0.26790(9) 0.66463(17) 0.0367(8) Uani 1 1 d . . .
H53 H 0.4246 0.2602 0.6915 0.044 Uiso 1 1 calc R . .
C54 C 0.46612(13) 0.30666(9) 0.65745(17) 0.0374(8) Uani 1 1 d . . .
H54 H 0.4444 0.3255 0.6785 0.045 Uiso 1 1 calc R . .
C55 C 0.50935(12) 0.31842(9) 0.62035(16) 0.0323(7) Uani 1 1 d . . .
H55 H 0.5178 0.3452 0.6169 0.039 Uiso 1 1 calc R . .
C56 C 0.54092(12) 0.29084(8) 0.58768(16) 0.0274(6) Uani 1 1 d . . .
C57 C 0.58692(12) 0.30140(8) 0.54676(16) 0.0281(6) Uani 1 1 d . . .
C58 C 0.66118(13) 0.38791(8) 0.51353(18) 0.0348(7) Uani 1 1 d . . .
C59 C 0.63153(15) 0.41751(9) 0.5418(2) 0.0519(10) Uani 1 1 d . . .
H59 H 0.5984 0.4124 0.5635 0.062 Uiso 1 1 calc R . .
C60 C 0.65206(16) 0.45450(10) 0.5371(2) 0.0625(11) Uani 1 1 d . . .
H60 H 0.6331 0.4755 0.5563 0.075 Uiso 1 1 calc R . .
C61 C 0.69998(16) 0.46149(10) 0.5048(2) 0.0541(10) Uani 1 1 d . . .
H61 H 0.7145 0.4870 0.5013 0.065 Uiso 1 1 calc R . .
C62 C 0.72618(15) 0.43008(9) 0.4777(2) 0.0459(9) Uani 1 1 d . . .
H62 H 0.7589 0.4346 0.4549 0.055 Uiso 1 1 calc R . .
C63 C 0.48186(16) 0.09869(10) 0.5051(2) 0.0476(9) Uani 1 1 d . . .
C64 C 0.43509(16) 0.12752(10) 0.4859(2) 0.0549(10) Uani 1 1 d . . .
H64 H 0.4350 0.1482 0.5215 0.066 Uiso 1 1 calc R . .
C65 C 0.39153(16) 0.12560(10) 0.4181(2) 0.0524(9) Uani 1 1 d . . .
H65 H 0.3616 0.1452 0.4075 0.063 Uiso 1 1 calc R . .
C66 C 0.38812(16) 0.09519(10) 0.3610(2) 0.0494(9) Uani 1 1 d . . .
C67 C 0.34075(17) 0.09375(12) 0.2928(2) 0.0628(11) Uani 1 1 d . . .
H67 H 0.3107 0.1133 0.2834 0.075 Uiso 1 1 calc R . .
C68 C 0.3374(2) 0.06447(14) 0.2395(3) 0.0723(12) Uani 1 1 d . . .
H68 H 0.3043 0.0631 0.1943 0.087 Uiso 1 1 calc R . .
C69 C 0.38230(19) 0.03691(13) 0.2517(2) 0.0673(11) Uani 1 1 d . . .
H69 H 0.3803 0.0170 0.2137 0.081 Uiso 1 1 calc R . .
C70 C 0.42993(17) 0.03761(11) 0.3177(2) 0.0580(10) Uani 1 1 d . . .
H70 H 0.4605 0.0185 0.3248 0.070 Uiso 1 1 calc R . .
C71 C 0.43319(15) 0.06662(10) 0.3745(2) 0.0450(8) Uani 1 1 d . . .
C72 C 0.48136(14) 0.06752(9) 0.44750(19) 0.0421(8) Uani 1 1 d . . .
C73 C 0.61208(14) 0.01099(9) 0.5258(2) 0.0397(8) Uani 1 1 d . . .
C74 C 0.61023(15) -0.01576(9) 0.4656(2) 0.0458(9) Uani 1 1 d . . .
H74 H 0.5777 -0.0162 0.4197 0.055 Uiso 1 1 calc R . .
C75 C 0.65764(16) -0.04150(9) 0.4755(2) 0.0500(9) Uani 1 1 d . . .
H75 H 0.6583 -0.0601 0.4359 0.060 Uiso 1 1 calc R . .
O16 O 0.59333(12) 0.13664(8) 0.43233(15) 0.0720(8) Uani 1 1 d . . .
H76 H 0.6135 0.1394 0.4792 0.086 Uiso 1 1 calc R . .
C76 C 0.70400(16) -0.04003(9) 0.5430(2) 0.0500(9) Uani 1 1 d . . .
H18 H 0.7370 -0.0575 0.5506 0.060 Uiso 1 1 calc R . .
C77 C 0.70143(15) -0.01268(9) 0.5994(2) 0.0461(9) Uani 1 1 d . . .
H77 H 0.7333 -0.0119 0.6460 0.055 Uiso 1 1 calc R . .
C78 C 0.6135(2) 0.10478(11) 0.4002(3) 0.0857(14) Uani 1 1 d . . .
H78A H 0.5837 0.0973 0.3519 0.129 Uiso 1 1 calc R . .
H78B H 0.6194 0.0834 0.4379 0.129 Uiso 1 1 calc R . .
H78C H 0.6518 0.1109 0.3878 0.129 Uiso 1 1 calc R . .
O17 O 0.5000 0.0683(3) 0.7500 0.161(3) Uiso 0.80 2 d SP A 1
O17A O 0.4603(5) 0.0461(3) 0.7390(7) 0.151(4) Uiso 0.45 1 d P . 2
O17B O 0.4778(13) 0.0591(8) 0.6836(18) 0.140(10) Uiso 0.15 1 d P B 3


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C3 1.384(3) . ?
N1 C43 1.337(3) . ?
N1 C47 1.348(3) . ?
C1 C6 1.393(4) . ?
C1 C2 1.399(4) . ?
O2 C4 1.383(3) . ?
N2 N3 1.315(3) . ?
N2 C43 1.405(3) . ?
C2 C3 1.392(4) . ?
C2 C28 1.531(4) . ?
O3 C5 1.384(3) . ?
N3 C42 1.325(4) . ?
C3 C4 1.390(4) . ?
O4 C10 1.389(3) . ?
N4 C73 1.337(4) . ?
N4 C77 1.341(4) . ?
C4 C5 1.384(4) . ?
O5 C11 1.366(3) . ?
N5 N6 1.322(3) . ?
N5 C73 1.401(4) . ?
C5 C6 1.392(4) . ?
O6 C12 1.378(3) . ?
N6 C72 1.312(4) . ?
C6 C7 1.533(4) . ?
O7 C17 1.391(3) . ?
N7 C62 1.332(4) . ?
N7 C58 1.337(4) . ?
C7 C9 1.527(4) . ?
C7 C29 1.529(4) . ?
O8 C18 1.382(3) . ?
N8 N9 1.333(3) . ?
N8 C58 1.390(3) . ?
C8 C13 1.396(4) . ?
C8 C9 1.400(4) . ?
O9 C19 1.380(3) . ?
N9 C57 1.326(3) . ?
C9 C10 1.382(4) . ?
O10 C24 1.372(3) . ?
C10 C11 1.385(4) . ?
O11 C25 1.367(3) . ?
C11 C12 1.390(4) . ?
O12 C26 1.383(3) . ?
C12 C13 1.396(4) . ?
O13 C33 1.257(3) . ?
C13 C14 1.524(4) . ?
O14 C63 1.256(4) . ?
C14 C16 1.527(4) . ?
C14 C30 1.541(4) . ?
O15 C48 1.252(3) . ?
C15 C20 1.384(4) . ?
C15 C16 1.397(3) . ?
C16 C17 1.384(4) . ?
C17 C18 1.387(4) . ?
C18 C19 1.386(4) . ?
C19 C20 1.395(4) . ?
C20 C21 1.525(4) . ?
C21 C31 1.529(4) . ?
C21 C23 1.529(3) . ?
C22 C23 1.395(4) . ?
C22 C27 1.399(4) . ?
C23 C24 1.397(4) . ?
C24 C25 1.383(4) . ?
C25 C26 1.390(4) . ?
C26 C27 1.398(4) . ?
C27 C28 1.525(4) . ?
C28 C32 1.526(4) . ?
C33 C34 1.439(4) . ?
C33 C42 1.447(4) . ?
C34 C35 1.336(5) . ?
C35 C36 1.434(5) . ?
C36 C37 1.392(5) . ?
C36 C41 1.413(4) . ?
C37 C38 1.353(6) . ?
C38 C39 1.385(6) . ?
C39 C40 1.372(5) . ?
C40 C41 1.395(4) . ?
C41 C42 1.462(4) . ?
C43 C44 1.383(4) . ?
C44 C45 1.376(4) . ?
C45 C46 1.388(4) . ?
C46 C47 1.367(4) . ?
C48 C49 1.440(4) . ?
C48 C57 1.461(4) . ?
C49 C50 1.335(4) . ?
C50 C51 1.448(4) . ?
C51 C52 1.398(4) . ?
C51 C56 1.412(4) . ?
C52 C53 1.372(4) . ?
C53 C54 1.382(4) . ?
C54 C55 1.379(4) . ?
C55 C56 1.405(4) . ?
C56 C57 1.466(4) . ?
C58 C59 1.388(4) . ?
C59 C60 1.373(4) . ?
C60 C61 1.380(4) . ?
C61 C62 1.382(4) . ?
C63 C64 1.441(5) . ?
C63 C72 1.476(4) . ?
C64 C65 1.347(5) . ?
C65 C66 1.441(5) . ?
C66 C67 1.400(5) . ?
C66 C71 1.406(5) . ?
C67 C68 1.367(5) . ?
C68 C69 1.380(5) . ?
C69 C70 1.377(5) . ?
C70 C71 1.403(5) . ?
C71 C72 1.465(4) . ?
C73 C74 1.397(4) . ?
C74 C75 1.382(4) . ?
C75 C76 1.379(5) . ?
O16 C78 1.370(4) . ?
C76 C77 1.380(4) . ?
O17A O17A 1.76(2) 2_656 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C43 N1 C47 117.0(2) . . ?
C6 C1 C2 123.6(3) . . ?
N3 N2 C43 119.0(2) . . ?
C3 C2 C1 117.6(3) . . ?
C3 C2 C28 121.0(2) . . ?
C1 C2 C28 121.3(2) . . ?
N2 N3 C42 120.0(3) . . ?
O1 C3 C4 121.5(2) . . ?
O1 C3 C2 118.5(3) . . ?
C4 C3 C2 120.0(3) . . ?
C73 N4 C77 116.7(3) . . ?
O2 C4 C5 120.3(3) . . ?
O2 C4 C3 118.7(3) . . ?
C5 C4 C3 120.9(3) . . ?
N6 N5 C73 119.1(3) . . ?
O3 C5 C4 114.8(2) . . ?
O3 C5 C6 124.2(3) . . ?
C4 C5 C6 120.9(3) . . ?
C72 N6 N5 119.9(3) . . ?
C5 C6 C1 116.9(3) . . ?
C5 C6 C7 121.2(2) . . ?
C1 C6 C7 121.9(2) . . ?
C62 N7 C58 117.8(3) . . ?
C9 C7 C29 113.3(2) . . ?
C9 C7 C6 110.3(2) . . ?
C29 C7 C6 112.2(2) . . ?
N9 N8 C58 120.4(2) . . ?
C13 C8 C9 123.6(3) . . ?
C57 N9 N8 118.2(2) . . ?
C10 C9 C8 116.9(2) . . ?
C10 C9 C7 120.2(2) . . ?
C8 C9 C7 122.9(2) . . ?
C9 C10 C11 121.6(2) . . ?
C9 C10 O4 119.7(2) . . ?
C11 C10 O4 118.6(2) . . ?
O5 C11 C10 116.9(2) . . ?
O5 C11 C12 123.1(2) . . ?
C10 C11 C12 120.0(2) . . ?
O6 C12 C11 115.3(2) . . ?
O6 C12 C13 123.9(2) . . ?
C11 C12 C13 120.8(2) . . ?
C12 C13 C8 117.0(2) . . ?
C12 C13 C14 120.7(2) . . ?
C8 C13 C14 122.3(2) . . ?
C13 C14 C16 112.0(2) . . ?
C13 C14 C30 112.8(2) . . ?
C16 C14 C30 110.7(2) . . ?
C20 C15 C16 123.3(3) . . ?
C17 C16 C15 117.2(2) . . ?
C17 C16 C14 122.7(2) . . ?
C15 C16 C14 120.1(2) . . ?
C16 C17 C18 121.3(2) . . ?
C16 C17 O7 118.5(2) . . ?
C18 C17 O7 120.2(2) . . ?
O8 C18 C19 122.7(2) . . ?
O8 C18 C17 117.4(2) . . ?
C19 C18 C17 119.9(2) . . ?
O9 C19 C18 115.3(2) . . ?
O9 C19 C20 124.0(2) . . ?
C18 C19 C20 120.7(2) . . ?
C15 C20 C19 117.6(2) . . ?
C15 C20 C21 119.5(2) . . ?
C19 C20 C21 122.8(2) . . ?
C20 C21 C31 111.6(2) . . ?
C20 C21 C23 109.2(2) . . ?
C31 C21 C23 114.0(2) . . ?
C23 C22 C27 123.3(2) . . ?
C22 C23 C24 117.2(2) . . ?
C22 C23 C21 125.4(2) . . ?
C24 C23 C21 117.3(2) . . ?
O10 C24 C25 120.6(2) . . ?
O10 C24 C23 118.1(2) . . ?
C25 C24 C23 121.3(2) . . ?
O11 C25 C24 117.6(2) . . ?
O11 C25 C26 122.5(2) . . ?
C24 C25 C26 119.9(2) . . ?
O12 C26 C25 114.1(2) . . ?
O12 C26 C27 124.7(2) . . ?
C25 C26 C27 121.2(2) . . ?
C26 C27 C22 117.0(2) . . ?
C26 C27 C28 119.8(2) . . ?
C22 C27 C28 123.2(2) . . ?
C27 C28 C32 113.8(2) . . ?
C27 C28 C2 109.5(2) . . ?
C32 C28 C2 111.8(2) . . ?
O13 C33 C34 120.8(3) . . ?
O13 C33 C42 121.3(3) . . ?
C34 C33 C42 117.9(3) . . ?
C35 C34 C33 121.3(3) . . ?
C34 C35 C36 122.9(3) . . ?
C37 C36 C41 118.6(4) . . ?
C37 C36 C35 122.2(3) . . ?
C41 C36 C35 119.2(3) . . ?
C38 C37 C36 121.4(4) . . ?
C37 C38 C39 120.6(4) . . ?
C40 C39 C38 119.6(4) . . ?
C39 C40 C41 121.0(4) . . ?
C40 C41 C36 118.9(3) . . ?
C40 C41 C42 122.6(3) . . ?
C36 C41 C42 118.6(3) . . ?
N3 C42 C33 124.6(3) . . ?
N3 C42 C41 115.3(3) . . ?
C33 C42 C41 120.1(3) . . ?
N1 C43 C44 123.9(3) . . ?
N1 C43 N2 113.2(2) . . ?
C44 C43 N2 122.9(3) . . ?
C45 C44 C43 117.8(3) . . ?
C44 C45 C46 119.4(3) . . ?
C47 C46 C45 118.6(3) . . ?
N1 C47 C46 123.2(3) . . ?
O15 C48 C49 121.1(3) . . ?
O15 C48 C57 120.5(3) . . ?
C49 C48 C57 118.4(3) . . ?
C50 C49 C48 121.4(3) . . ?
C49 C50 C51 122.1(3) . . ?
C52 C51 C56 119.2(3) . . ?
C52 C51 C50 120.7(3) . . ?
C56 C51 C50 120.0(3) . . ?
C53 C52 C51 121.0(3) . . ?
C52 C53 C54 119.7(3) . . ?
C55 C54 C53 121.2(3) . . ?
C54 C55 C56 120.0(3) . . ?
C55 C56 C51 118.9(3) . . ?
C55 C56 C57 122.8(3) . . ?
C51 C56 C57 118.3(2) . . ?
N9 C57 C48 124.5(3) . . ?
N9 C57 C56 116.2(2) . . ?
C48 C57 C56 119.3(2) . . ?
N7 C58 C59 123.4(3) . . ?
N7 C58 N8 113.5(2) . . ?
C59 C58 N8 123.1(3) . . ?
C60 C59 C58 117.3(3) . . ?
C59 C60 C61 120.6(3) . . ?
C60 C61 C62 117.7(3) . . ?
N7 C62 C61 123.2(3) . . ?
O14 C63 C64 121.4(3) . . ?
O14 C63 C72 120.7(3) . . ?
C64 C63 C72 117.9(3) . . ?
C65 C64 C63 121.0(3) . . ?
C64 C65 C66 123.2(3) . . ?
C67 C66 C71 119.8(4) . . ?
C67 C66 C65 121.0(4) . . ?
C71 C66 C65 119.2(3) . . ?
C68 C67 C66 120.6(4) . . ?
C67 C68 C69 119.6(4) . . ?
C70 C69 C68 121.4(4) . . ?
C69 C70 C71 119.9(4) . . ?
C70 C71 C66 118.6(3) . . ?
C70 C71 C72 121.9(3) . . ?
C66 C71 C72 119.5(3) . . ?
N6 C72 C71 116.1(3) . . ?
N6 C72 C63 124.7(3) . . ?
C71 C72 C63 119.2(3) . . ?
N4 C73 C74 124.0(3) . . ?
N4 C73 N5 114.5(3) . . ?
C74 C73 N5 121.5(3) . . ?
C75 C74 C73 117.4(3) . . ?
C76 C75 C74 119.7(3) . . ?
C75 C76 C77 118.5(3) . . ?
N4 C77 C76 123.7(3) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.64
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.594
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.057

_database_code_depnum_ccdc_archive 'CCDC 1002494'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2cp55n

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            
'C-methylpyrogallol[4]arene with 1-(2-pyridylazo)-2-napthol'
_chemical_formula_moiety         '2(C32 H32 O12), 3(C15 H11 O1 N3), 4(C2 H6 O1)'
_chemical_formula_sum            'C117 H121 N9 O31'
_chemical_melting_point          ?

_exptl_crystal_description       plate
_exptl_crystal_colour            orange

_diffrn_ambient_temperature      173(2)
_chemical_formula_weight         2149.23

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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
_chemical_absolute_configuration ?

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

_cell_length_a                   17.5240(4)
_cell_length_b                   17.9622(4)
_cell_length_c                   18.5524(4)
_cell_angle_alpha                99.3690(10)
_cell_angle_beta                 100.5790(10)
_cell_angle_gamma                110.0100(10)
_cell_volume                     5230.5(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9552
_cell_measurement_theta_min      3.9
_cell_measurement_theta_max      70.0
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2268
_exptl_absorpt_coefficient_mu    0.825
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_process_details   
;
 Data were corrected for decay and absorption using the program SADABS 
 (Sheldrick, G. M. (2003). SADABS. Version 2.10. University of
 Göttingen, Germany).
;

_exptl_special_details           
; 
 ? 
;
_diffrn_radiation_probe          ?
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.0
_diffrn_reflns_number            67161
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0364
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.50
_diffrn_reflns_theta_max         70.25
_reflns_number_total             18823
_reflns_number_gt                15375
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2008)'
_computing_structure_solution    'SHELXS-1997 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-1997 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-SEED, Barbour, 2001'
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. There are minor residual 
 electron densities that are near a disordered ethanol and a ethanol molecule
 that is minor disorder that is not included. The short hydrogen distances
 between H5D and H2G, H8B and H2I, and H3B and H2G are due to the molecules
 disordered over two positions.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1233P)²+3.0070P] where P=(Fo²+2Fc²)/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         18823
_refine_ls_number_parameters     1479
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0556
_refine_ls_wR_factor_ref         0.1896
_refine_ls_wR_factor_gt          0.1728
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.071
_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
O1A O 0.65781(10) 0.16105(10) 0.29210(9) 0.0225(3) Uani 1 1 d . . .
H1A H 0.6131 0.1695 0.2888 0.027 Uiso 1 1 calc R . .
O11A O 0.59925(10) -0.15113(9) 0.14228(9) 0.0227(3) Uani 1 1 d . . .
H11A H 0.5644 -0.1295 0.1476 0.027 Uiso 1 1 calc R . .
O9B O 0.58268(10) -0.12215(10) 0.69692(9) 0.0221(3) Uani 1 1 d . . .
H9B H 0.5302 -0.1469 0.6832 0.027 Uiso 1 1 calc R . .
O3A O 0.60476(10) 0.12814(10) 0.52983(9) 0.0202(3) Uani 1 1 d . . .
H3A H 0.6002 0.0904 0.5522 0.024 Uiso 1 1 calc R . .
O4A O 0.57874(10) -0.02895(9) 0.53814(9) 0.0204(3) Uani 1 1 d . . .
H4A H 0.5311 -0.0660 0.5176 0.024 Uiso 1 1 calc R . .
O2A O 0.57045(10) 0.17399(10) 0.39753(9) 0.0195(3) Uani 1 1 d . . .
H2A H 0.5475 0.1744 0.4335 0.023 Uiso 1 1 calc R . .
O5A O 0.52835(10) -0.19125(9) 0.51143(9) 0.0208(3) Uani 1 1 d . . .
H5A H 0.5172 -0.2379 0.4845 0.025 Uiso 1 1 calc R . .
O1B O 0.97982(11) 0.40525(9) 0.95897(9) 0.0250(4) Uani 1 1 d . . .
H1B H 0.9519 0.3822 0.9140 0.030 Uiso 1 1 calc R . .
O7B O 0.53592(10) -0.19774(10) 0.92845(9) 0.0236(3) Uani 1 1 d . . .
H7B H 0.4867 -0.2234 0.9010 0.028 Uiso 1 1 calc R . .
O6B O 0.57021(10) -0.04349(10) 1.01838(9) 0.0224(3) Uani 1 1 d . . .
H6B H 0.5664 -0.0917 1.0038 0.027 Uiso 1 1 calc R . .
O10B O 0.65265(10) 0.04873(9) 0.70916(9) 0.0216(3) Uani 1 1 d . . .
H10B H 0.6380 -0.0017 0.7053 0.026 Uiso 1 1 calc R . .
O2B O 0.94300(11) 0.45243(10) 1.09110(10) 0.0270(4) Uani 1 1 d . . .
H2B H 0.9521 0.4770 1.0568 0.032 Uiso 1 1 calc R . .
O5B O 0.59945(10) 0.10975(10) 1.08712(10) 0.0245(4) Uani 1 1 d . . .
H5B H 0.5542 0.0698 1.0654 0.029 Uiso 1 1 calc R . .
O6A O 0.63776(10) -0.26616(10) 0.51757(10) 0.0243(4) Uani 1 1 d . . .
H6A H 0.6740 -0.2851 0.5096 0.029 Uiso 1 1 calc R . .
O8B O 0.47381(10) -0.20394(10) 0.76885(9) 0.0222(3) Uani 1 1 d . . .
H8B H 0.4453 -0.2282 0.7959 0.027 Uiso 1 1 calc R . .
O3B O 0.90563(11) 0.34882(10) 1.18450(10) 0.0250(4) Uani 1 1 d . . .
H3B H 0.9171 0.3994 1.1941 0.030 Uiso 1 1 calc R . .
O12A O 0.63121(10) 0.00361(10) 0.21307(9) 0.0208(3) Uani 1 1 d . . .
H12A H 0.6501 0.0547 0.2287 0.025 Uiso 1 1 calc R . .
O11B O 0.71528(11) 0.21398(10) 0.74092(10) 0.0260(4) Uani 1 1 d . . .
H11B H 0.6643 0.1825 0.7264 0.031 Uiso 1 1 calc R . .
O10A O 0.71062(10) -0.22147(10) 0.17118(10) 0.0238(3) Uani 1 1 d . . .
H10A H 0.6581 -0.2445 0.1551 0.029 Uiso 1 1 calc R . .
O7A O 0.72818(11) -0.34756(10) 0.46695(10) 0.0249(4) Uani 1 1 d . . .
H7A H 0.6880 -0.3900 0.4400 0.030 Uiso 1 1 calc R . .
O4B O 0.75182(10) 0.22046(10) 1.15128(10) 0.0249(4) Uani 1 1 d . . .
H4B H 0.8022 0.2534 1.1634 0.030 Uiso 1 1 calc R . .
O12B O 0.86849(11) 0.30462(10) 0.83399(10) 0.0255(4) Uani 1 1 d . . .
H12B H 0.8286 0.3180 0.8171 0.031 Uiso 1 1 calc R . .
O9A O 0.77234(12) -0.32499(10) 0.22592(10) 0.0271(4) Uani 1 1 d . . .
H9A H 0.7563 -0.2993 0.1964 0.033 Uiso 1 1 calc R . .
O1I O 0.3718(3) 0.7225(3) 0.8514(4) 0.0239(10) Uani 0.769(10) 1 d PD A 1
H1I H 0.3452 0.7531 0.8574 0.029 Uiso 0.769(10) 1 calc PR A 1
O1E O 0.45166(11) 0.32542(11) 0.87057(11) 0.0314(4) Uani 1 1 d . . .
O8A O 0.70842(12) -0.41507(10) 0.31708(11) 0.0308(4) Uani 1 1 d . . .
H8A H 0.7057 -0.4272 0.2707 0.037 Uiso 1 1 calc R . .
N1E N 0.62193(13) 0.35793(12) 0.93984(12) 0.0251(4) Uani 1 1 d . . .
N2E N 0.57367(13) 0.28080(12) 0.91125(12) 0.0251(4) Uani 1 1 d . . .
H2E H 0.5195 0.2662 0.8913 0.030 Uiso 1 1 calc R . .
C12B C 0.80149(14) 0.04269(14) 1.08193(12) 0.0195(4) Uani 1 1 d . . .
H12C H 0.8484 0.0278 1.0809 0.023 Uiso 1 1 calc R . .
C3A C 0.65560(14) 0.12582(12) 0.48145(12) 0.0168(4) Uani 1 1 d . . .
C4A C 0.72401(14) 0.10259(12) 0.49743(12) 0.0174(4) Uani 1 1 d . . .
C5A C 0.76791(13) 0.09900(12) 0.44252(12) 0.0165(4) Uani 1 1 d . . .
H5A1 H 0.8138 0.0821 0.4523 0.020 Uiso 1 1 calc R . .
C23A C 0.67455(14) -0.10457(14) 0.19249(13) 0.0188(4) Uani 1 1 d . . .
C26B C 0.86529(14) 0.10027(14) 0.82920(13) 0.0193(4) Uani 1 1 d . . .
H26B H 0.9012 0.0749 0.8489 0.023 Uiso 1 1 calc R . .
N3E N 0.55326(13) 0.14548(12) 0.88272(12) 0.0236(4) Uani 1 1 d . . .
C12A C 0.78084(14) -0.05069(14) 0.55679(12) 0.0190(4) Uani 1 1 d . . .
H12D H 0.8388 -0.0176 0.5667 0.023 Uiso 1 1 calc R . .
C19B C 0.72536(14) -0.07790(13) 0.88055(13) 0.0184(4) Uani 1 1 d . . .
H19B H 0.7833 -0.0482 0.9051 0.022 Uiso 1 1 calc R . .
C16B C 0.55630(14) -0.16355(13) 0.80997(13) 0.0193(4) Uani 1 1 d . . .
C29A C 0.84223(14) 0.12977(14) 0.61153(13) 0.0213(5) Uani 1 1 d . . .
H29A H 0.8564 0.1146 0.6591 0.032 Uiso 1 1 calc R . .
H29B H 0.8527 0.1882 0.6221 0.032 Uiso 1 1 calc R . .
H29C H 0.8771 0.1183 0.5790 0.032 Uiso 1 1 calc R . .
C23B C 0.76207(14) 0.17345(14) 0.77023(13) 0.0198(4) Uani 1 1 d . . .
C25A C 0.77479(14) 0.02288(13) 0.27757(12) 0.0179(4) Uani 1 1 d . . .
C15B C 0.58685(14) -0.16010(13) 0.88596(13) 0.0191(4) Uani 1 1 d . . .
C14B C 0.70535(14) -0.10355(13) 1.00733(13) 0.0198(4) Uani 1 1 d . . .
H14B H 0.6601 -0.1416 1.0249 0.024 Uiso 1 1 calc R . .
C2B C 0.94479(14) 0.37673(14) 1.07057(14) 0.0220(5) Uani 1 1 d . . .
C2A C 0.63566(13) 0.14824(13) 0.41453(13) 0.0173(4) Uani 1 1 d . . .
C28A C 0.79658(14) 0.11234(13) 0.31470(13) 0.0185(4) Uani 1 1 d . . .
H28A H 0.7772 0.1375 0.2744 0.022 Uiso 1 1 calc R . .
C8B C 0.74660(15) 0.14398(14) 1.11779(13) 0.0201(4) Uani 1 1 d . . .
C27B C 0.78634(14) 0.05057(14) 0.78116(13) 0.0197(4) Uani 1 1 d . . .
C13B C 0.81650(14) 0.12306(14) 1.11748(12) 0.0195(4) Uani 1 1 d . . .
C13A C 0.72362(14) -0.01234(13) 0.55760(12) 0.0178(4) Uani 1 1 d . . .
C6B C 0.96155(13) 0.27114(14) 0.98268(13) 0.0197(4) Uani 1 1 d . . .
C1A C 0.68045(14) 0.14382(13) 0.36059(12) 0.0175(4) Uani 1 1 d . . .
C22A C 0.73204(15) -0.14110(13) 0.20764(13) 0.0198(4) Uani 1 1 d . . .
C10A C 0.67146(14) -0.18292(13) 0.52954(13) 0.0194(4) Uani 1 1 d . . .
C8A C 0.63924(14) -0.06237(13) 0.54156(12) 0.0172(4) Uani 1 1 d . . .
C3B C 0.92742(14) 0.32552(14) 1.11942(13) 0.0212(5) Uani 1 1 d . . .
C4B C 0.92647(14) 0.24673(14) 1.10069(13) 0.0199(4) Uani 1 1 d . . .
C24B C 0.84124(14) 0.22094(13) 0.81770(13) 0.0199(4) Uani 1 1 d . . .
C28B C 0.97711(14) 0.23879(14) 0.90752(13) 0.0211(5) Uani 1 1 d . . .
H28B H 1.0042 0.2871 0.8877 0.025 Uiso 1 1 calc R . .
C18B C 0.69736(14) -0.08217(13) 0.80419(13) 0.0183(4) Uani 1 1 d . . .
C9B C 0.66582(15) 0.08622(14) 1.08472(13) 0.0203(4) Uani 1 1 d . . .
C20B C 0.67197(14) -0.11530(13) 0.92241(13) 0.0186(4) Uani 1 1 d . . .
C1B C 0.96241(14) 0.34985(14) 1.00327(13) 0.0211(5) Uani 1 1 d . . .
C11B C 0.72125(14) -0.01664(13) 1.04800(12) 0.0190(4) Uani 1 1 d . . .
C21B C 0.75682(14) -0.04214(13) 0.75877(13) 0.0196(4) Uani 1 1 d . . .
H21B H 0.7239 -0.0605 0.7046 0.024 Uiso 1 1 calc R . .
C25B C 0.89401(14) 0.18511(14) 0.84959(12) 0.0194(4) Uani 1 1 d . . .
C5B C 0.94275(13) 0.22107(13) 1.03210(13) 0.0192(4) Uani 1 1 d . . .
H5B1 H 0.9409 0.1670 1.0185 0.023 Uiso 1 1 calc R . .
C19A C 0.83995(14) -0.16780(13) 0.40456(14) 0.0203(4) Uani 1 1 d . . .
H19A H 0.8694 -0.1106 0.4249 0.024 Uiso 1 1 calc R . .
C14A C 0.81807(14) -0.17768(14) 0.53530(13) 0.0212(5) Uani 1 1 d . . .
H14A H 0.8021 -0.2239 0.5605 0.025 Uiso 1 1 calc R . .
C24A C 0.69554(14) -0.02345(14) 0.22914(13) 0.0184(4) Uani 1 1 d . . .
C26A C 0.83118(14) -0.01612(14) 0.29141(13) 0.0193(4) Uani 1 1 d . . .
H26A H 0.8853 0.0145 0.3248 0.023 Uiso 1 1 calc R . .
C10B C 0.65289(14) 0.00663(14) 1.04969(12) 0.0197(4) Uani 1 1 d . . .
C7A C 0.74908(14) 0.07999(13) 0.57142(12) 0.0178(4) Uani 1 1 d . . .
H7A1 H 0.7158 0.0954 0.6052 0.021 Uiso 1 1 calc R . .
C29B C 0.97285(15) 0.15280(15) 1.16945(14) 0.0253(5) Uani 1 1 d . . .
H29D H 0.9571 0.1146 1.2014 0.038 Uiso 1 1 calc R . .
H29E H 1.0267 0.1974 1.1961 0.038 Uiso 1 1 calc R . .
H29F H 0.9781 0.1240 1.1222 0.038 Uiso 1 1 calc R . .
C32B C 1.03908(15) 0.19616(16) 0.91974(14) 0.0266(5) Uani 1 1 d . . .
H32A H 1.0128 0.1459 0.9354 0.040 Uiso 1 1 calc R . .
H32B H 1.0897 0.2327 0.9592 0.040 Uiso 1 1 calc R . .
H32C H 1.0543 0.1826 0.8725 0.040 Uiso 1 1 calc R . .
C22B C 0.73330(14) 0.08877(13) 0.75389(12) 0.0187(4) Uani 1 1 d . . .
C1E C 0.50251(16) 0.39705(14) 0.89840(14) 0.0245(5) Uani 1 1 d . . .
C10E C 0.58978(16) 0.41490(15) 0.93577(14) 0.0248(5) Uani 1 1 d . . .
C20A C 0.80747(14) -0.21536(14) 0.45205(13) 0.0207(5) Uani 1 1 d . . .
C6A C 0.74796(13) 0.11892(12) 0.37401(13) 0.0174(4) Uani 1 1 d . . .
C17B C 0.61186(14) -0.12312(13) 0.77071(13) 0.0187(4) Uani 1 1 d . . .
C15A C 0.76253(14) -0.29894(14) 0.42146(14) 0.0212(5) Uani 1 1 d . . .
C9A C 0.61274(14) -0.14659(14) 0.52770(12) 0.0185(4) Uani 1 1 d . . .
C17A C 0.78668(15) -0.28368(14) 0.29967(14) 0.0229(5) Uani 1 1 d . . .
C16A C 0.75292(15) -0.33259(14) 0.34593(14) 0.0234(5) Uani 1 1 d . . .
C11A C 0.75657(14) -0.13540(14) 0.54210(13) 0.0194(4) Uani 1 1 d . . .
C27A C 0.81065(14) -0.09810(14) 0.25791(13) 0.0191(4) Uani 1 1 d . . .
C7B C 0.90471(14) 0.18795(14) 1.15169(13) 0.0203(4) Uani 1 1 d . . .
H7B1 H 0.9043 0.2204 1.2007 0.024 Uiso 1 1 calc R . .
C2E C 0.47701(16) 0.46565(15) 0.89471(15) 0.0278(5) Uani 1 1 d . . .
H2E1 H 0.4213 0.4560 0.8685 0.033 Uiso 1 1 calc R . .
C32A C 0.89059(14) 0.16202(14) 0.34862(13) 0.0213(5) Uani 1 1 d . . .
H32D H 0.9104 0.1435 0.3926 0.032 Uiso 1 1 calc R . .
H32E H 0.9004 0.2200 0.3643 0.032 Uiso 1 1 calc R . .
H32F H 0.9212 0.1544 0.3107 0.032 Uiso 1 1 calc R . .
C15E C 0.58225(17) 0.08497(15) 0.88116(15) 0.0276(5) Uani 1 1 d . . .
H15E H 0.5434 0.0303 0.8597 0.033 Uiso 1 1 calc R . .
C30B C 0.78229(15) -0.12644(14) 1.02426(14) 0.0242(5) Uani 1 1 d . . .
H30A H 0.8278 -0.0903 1.0073 0.036 Uiso 1 1 calc R . .
H30B H 0.7673 -0.1832 0.9975 0.036 Uiso 1 1 calc R . .
H30C H 0.8009 -0.1204 1.0788 0.036 Uiso 1 1 calc R . .
C30A C 0.90963(15) -0.12313(15) 0.57497(15) 0.0260(5) Uani 1 1 d . . .
H30D H 0.9285 -0.0780 0.5506 0.039 Uiso 1 1 calc R . .
H30E H 0.9447 -0.1553 0.5715 0.039 Uiso 1 1 calc R . .
H30F H 0.9145 -0.1011 0.6283 0.039 Uiso 1 1 calc R . .
C11E C 0.60909(15) 0.22153(15) 0.91265(13) 0.0229(5) Uani 1 1 d . . .
C9E C 0.64777(16) 0.49948(15) 0.97125(14) 0.0260(5) Uani 1 1 d . . .
C4E C 0.61721(16) 0.56249(15) 0.96816(14) 0.0265(5) Uani 1 1 d . . .
C18A C 0.83143(14) -0.19989(14) 0.32816(14) 0.0213(5) Uani 1 1 d . . .
C21A C 0.86685(14) -0.14506(14) 0.27757(13) 0.0213(5) Uani 1 1 d . . .
H21A H 0.8627 -0.1819 0.2292 0.026 Uiso 1 1 calc R . .
C13E C 0.72234(16) 0.17830(18) 0.94041(15) 0.0306(6) Uani 1 1 d . . .
H13E H 0.7800 0.1891 0.9606 0.037 Uiso 1 1 calc R . .
C8E C 0.73167(17) 0.51979(16) 1.00936(16) 0.0325(6) Uani 1 1 d . . .
H8E H 0.7535 0.4782 1.0107 0.039 Uiso 1 1 calc R . .
C14E C 0.66526(17) 0.09858(17) 0.90912(15) 0.0296(5) Uani 1 1 d . . .
H14E H 0.6833 0.0542 0.9071 0.036 Uiso 1 1 calc R . .
C31B C 0.82929(15) -0.07257(15) 0.76372(15) 0.0257(5) Uani 1 1 d . . .
H31A H 0.8670 -0.0459 0.7345 0.038 Uiso 1 1 calc R . .
H31B H 0.8064 -0.1319 0.7431 0.038 Uiso 1 1 calc R . .
H31C H 0.8606 -0.0593 0.8167 0.038 Uiso 1 1 calc R . .
C3E C 0.53139(17) 0.54235(15) 0.92792(15) 0.0290(5) Uani 1 1 d . . .
H3E H 0.5124 0.5856 0.9248 0.035 Uiso 1 1 calc R . .
C31A C 0.95938(15) -0.09088(15) 0.31087(15) 0.0263(5) Uani 1 1 d . . .
H31D H 0.9666 -0.0554 0.3598 0.039 Uiso 1 1 calc R . .
H31E H 0.9792 -0.0572 0.2764 0.039 Uiso 1 1 calc R . .
H31F H 0.9920 -0.1251 0.3179 0.039 Uiso 1 1 calc R . .
C7E C 0.78297(18) 0.60032(17) 1.04504(17) 0.0360(6) Uani 1 1 d . . .
H7E H 0.8399 0.6137 1.0704 0.043 Uiso 1 1 calc R . .
C12E C 0.69471(16) 0.24200(16) 0.94210(15) 0.0286(5) Uani 1 1 d . . .
H12E H 0.7325 0.2973 0.9625 0.034 Uiso 1 1 calc R . .
C6E C 0.75176(18) 0.66175(16) 1.04407(16) 0.0339(6) Uani 1 1 d . . .
H6E H 0.7868 0.7165 1.0703 0.041 Uiso 1 1 calc R . .
C5E C 0.66996(17) 0.64331(16) 1.00511(15) 0.0311(6) Uani 1 1 d . . .
H5E H 0.6494 0.6857 1.0034 0.037 Uiso 1 1 calc R . .
C2I C 0.3488(3) 0.5813(2) 0.8214(3) 0.0563(15) Uani 0.769(10) 1 d PD A 1
H2I1 H 0.3123 0.5275 0.8250 0.084 Uiso 0.769(10) 1 calc PR A 1
H2I2 H 0.4070 0.5930 0.8479 0.084 Uiso 0.769(10) 1 calc PR A 1
H2I3 H 0.3453 0.5815 0.7681 0.084 Uiso 0.769(10) 1 calc PR A 1
C1I C 0.3222(3) 0.6427(2) 0.8556(3) 0.0433(13) Uani 0.769(10) 1 d PD A 1
H1I1 H 0.2628 0.6293 0.8299 0.052 Uiso 0.769(10) 1 calc PR A 1
H1I2 H 0.3257 0.6420 0.9093 0.052 Uiso 0.769(10) 1 calc PR A 1
O1D O 0.46084(11) 0.65757(10) 0.42642(10) 0.0274(4) Uani 1 1 d . . .
N2D N 0.47511(13) 0.51861(12) 0.41115(12) 0.0234(4) Uani 1 1 d . . .
H2D H 0.5021 0.5720 0.4228 0.028 Uiso 1 1 calc R . .
N1D N 0.39254(13) 0.48535(12) 0.39686(11) 0.0246(4) Uani 1 1 d . . .
N3D N 0.60104(14) 0.50183(12) 0.41673(12) 0.0261(4) Uani 1 1 d . . .
C1D C 0.38317(16) 0.61974(15) 0.40932(13) 0.0258(5) Uani 1 1 d . . .
C10D C 0.34720(16) 0.53036(15) 0.39519(13) 0.0251(5) Uani 1 1 d . . .
C11D C 0.51881(16) 0.46578(14) 0.40711(13) 0.0231(5) Uani 1 1 d . . .
C13D C 0.52158(18) 0.33363(15) 0.38851(15) 0.0301(5) Uani 1 1 d . . .
H13D H 0.4945 0.2760 0.3791 0.036 Uiso 1 1 calc R . .
C12D C 0.47558(17) 0.38184(15) 0.39350(15) 0.0282(5) Uani 1 1 d . . .
H12F H 0.4167 0.3588 0.3879 0.034 Uiso 1 1 calc R . .
C9D C 0.25570(17) 0.48607(17) 0.37613(15) 0.0318(6) Uani 1 1 d . . .
C8D C 0.21899(19) 0.40112(19) 0.36353(17) 0.0392(6) Uani 1 1 d . . .
H8D H 0.2535 0.3704 0.3681 0.047 Uiso 1 1 calc R . .
C15D C 0.64466(18) 0.45310(16) 0.41162(17) 0.0328(6) Uani 1 1 d . . .
H15D H 0.7037 0.4777 0.4182 0.039 Uiso 1 1 calc R . .
C14D C 0.60748(18) 0.36920(16) 0.39725(17) 0.0330(6) Uani 1 1 d . . .
H14D H 0.6400 0.3366 0.3934 0.040 Uiso 1 1 calc R . .
C4D C 0.20377(19) 0.5310(2) 0.36853(17) 0.0396(7) Uani 1 1 d . . .
C2D C 0.32536(19) 0.66144(18) 0.40150(17) 0.0358(6) Uani 1 1 d . . .
H2D1 H 0.3468 0.7193 0.4105 0.043 Uiso 1 1 calc R . .
C7D C 0.1321(2) 0.3615(2) 0.3443(2) 0.0500(8) Uani 1 1 d . . .
H7D H 0.1075 0.3039 0.3369 0.060 Uiso 1 1 calc R . .
C5D C 0.1162(2) 0.4894(2) 0.3480(2) 0.0529(9) Uani 1 1 d . . .
H5D H 0.0809 0.5192 0.3424 0.063 Uiso 1 1 calc R . .
C3D C 0.2415(2) 0.6187(2) 0.38160(19) 0.0430(7) Uani 1 1 d . . .
H3D H 0.2056 0.6479 0.3759 0.052 Uiso 1 1 calc R . .
C6D C 0.0807(2) 0.4055(3) 0.3358(2) 0.0576(9) Uani 1 1 d . . .
H6D H 0.0213 0.3779 0.3216 0.069 Uiso 1 1 calc R . .
O1C O 0.23451(12) 0.61652(11) 0.18730(14) 0.0423(5) Uani 1 1 d . . .
N2C N 0.39131(13) 0.67755(12) 0.24862(12) 0.0253(4) Uani 1 1 d . . .
H2C H 0.3444 0.6846 0.2326 0.030 Uiso 1 1 calc R . .
N1C N 0.39028(13) 0.60300(12) 0.23938(11) 0.0224(4) Uani 1 1 d . . .
N3C N 0.45371(14) 0.81590(13) 0.29494(12) 0.0273(4) Uani 1 1 d . . .
C11C C 0.46579(16) 0.74589(14) 0.28347(13) 0.0244(5) Uani 1 1 d . . .
C8C C 0.39607(16) 0.44659(16) 0.22247(14) 0.0254(5) Uani 1 1 d . . .
H8C H 0.4476 0.4925 0.2426 0.031 Uiso 1 1 calc R . .
C14C C 0.60201(17) 0.88549(16) 0.35030(14) 0.0316(6) Uani 1 1 d . . .
H14C H 0.6486 0.9354 0.3740 0.038 Uiso 1 1 calc R . .
C15C C 0.52212(17) 0.88468(16) 0.32765(15) 0.0307(6) Uani 1 1 d . . .
H15C H 0.5151 0.9353 0.3356 0.037 Uiso 1 1 calc R . .
C9C C 0.32054(16) 0.45813(14) 0.20126(13) 0.0225(5) Uani 1 1 d . . .
C10C C 0.31831(15) 0.53969(14) 0.20882(13) 0.0221(5) Uani 1 1 d . . .
C4C C 0.24491(16) 0.38905(15) 0.17199(14) 0.0265(5) Uani 1 1 d . . .
C12C C 0.54398(16) 0.74024(16) 0.30389(14) 0.0271(5) Uani 1 1 d . . .
H12G H 0.5495 0.6890 0.2948 0.032 Uiso 1 1 calc R . .
C7C C 0.39547(18) 0.36849(17) 0.21407(15) 0.0317(6) Uani 1 1 d . . .
H7C H 0.4470 0.3613 0.2277 0.038 Uiso 1 1 calc R . .
C5C C 0.24618(18) 0.31049(16) 0.16505(16) 0.0318(6) Uani 1 1 d . . .
H5C H 0.1950 0.2640 0.1457 0.038 Uiso 1 1 calc R . .
C13C C 0.61309(16) 0.81204(17) 0.33787(14) 0.0307(6) Uani 1 1 d . . .
H13C H 0.6675 0.8111 0.3525 0.037 Uiso 1 1 calc R . .
C6C C 0.32058(19) 0.30017(16) 0.18593(16) 0.0341(6) Uani 1 1 d . . .
H6C H 0.3209 0.2468 0.1812 0.041 Uiso 1 1 calc R . .
C1C C 0.23760(16) 0.54746(15) 0.18372(16) 0.0287(5) Uani 1 1 d . . .
C2C C 0.16277(17) 0.47378(16) 0.15536(18) 0.0349(6) Uani 1 1 d . . .
H2C1 H 0.1097 0.4777 0.1403 0.042 Uiso 1 1 calc R . .
C3C C 0.16676(17) 0.39969(15) 0.14989(16) 0.0316(6) Uani 1 1 d . . .
H3C H 0.1161 0.3525 0.1307 0.038 Uiso 1 1 calc R . .
O1F O 0.95535(15) 0.55305(14) 0.41648(13) 0.0477(5) Uani 1 1 d D B 1
H1F H 0.9473 0.5119 0.4351 0.057 Uiso 1 1 d . C 1
O1H O 0.9107(2) 0.41061(18) 0.4677(2) 0.0868(11) Uani 1 1 d DU . .
H1H H 0.9342 0.3940 0.5017 0.104 Uiso 1 1 d . . .
C1H C 0.8292(2) 0.3541(2) 0.4346(2) 0.0522(8) Uani 1 1 d D . .
H1H1 H 0.7892 0.3713 0.4575 0.063 Uiso 1 1 calc R . .
H1H2 H 0.8242 0.2999 0.4434 0.063 Uiso 1 1 calc R . .
C1F C 0.9091(3) 0.5986(3) 0.4441(2) 0.0660(11) Uani 1 1 d D B 1
H1F1 H 0.8940 0.5832 0.4900 0.079 Uiso 1 1 calc R B 1
H1F2 H 0.8565 0.5859 0.4052 0.079 Uiso 1 1 calc R B 1
C2H C 0.8084(3) 0.3487(3) 0.3506(2) 0.0682(11) Uani 1 1 d D . .
H2H1 H 0.8127 0.4023 0.3423 0.102 Uiso 1 1 calc R . .
H2H2 H 0.7511 0.3087 0.3267 0.102 Uiso 1 1 calc R . .
H2H3 H 0.8481 0.3316 0.3283 0.102 Uiso 1 1 calc R . .
C2F C 0.9622(4) 0.6886(3) 0.4625(4) 0.134(3) Uani 1 1 d DU B 1
H2F1 H 1.0179 0.6993 0.4943 0.201 Uiso 1 1 calc R B 1
H2F2 H 0.9352 0.7194 0.4895 0.201 Uiso 1 1 calc R B 1
H2F3 H 0.9682 0.7055 0.4155 0.201 Uiso 1 1 calc R B 1
O1G O 0.9111(4) 0.4935(3) 0.2550(2) 0.0445(10) Uani 0.803(10) 1 d PD D 1
H1G H 0.9262 0.5055 0.3025 0.053 Uiso 0.803(10) 1 calc PR D 1
C1G C 0.8962(3) 0.5586(3) 0.2301(2) 0.0484(13) Uani 0.803(10) 1 d PD D 1
H1G1 H 0.8714 0.5399 0.1748 0.058 Uiso 0.803(10) 1 calc PR D 1
H1G2 H 0.8531 0.5689 0.2533 0.058 Uiso 0.803(10) 1 calc PR D 1
C2G C 0.9626(5) 0.6321(5) 0.2441(5) 0.089(2) Uani 0.803(10) 1 d PDU D 1
H2G1 H 0.9427 0.6710 0.2236 0.134 Uiso 0.803(10) 1 calc PR D 1
H2G2 H 1.0055 0.6242 0.2200 0.134 Uiso 0.803(10) 1 calc PR D 1
H2G3 H 0.9869 0.6534 0.2988 0.134 Uiso 0.803(10) 1 calc PR D 1
C3I C 0.3332(9) 0.6314(8) 0.8095(8) 0.041(4) Uiso 0.231(10) 1 d PD A 2
H3I1 H 0.3725 0.6096 0.7904 0.049 Uiso 0.231(10) 1 calc PR A 2
H3I2 H 0.2846 0.6192 0.7663 0.049 Uiso 0.231(10) 1 calc PR A 2
C4I C 0.3038(11) 0.5895(11) 0.8657(10) 0.058(5) Uiso 0.231(10) 1 d PD A 2
H4I1 H 0.2779 0.5305 0.8435 0.087 Uiso 0.231(10) 1 calc PR A 2
H4I2 H 0.2623 0.6083 0.8828 0.087 Uiso 0.231(10) 1 calc PR A 2
H4I3 H 0.3515 0.6016 0.9089 0.087 Uiso 0.231(10) 1 calc PR A 2
O2I O 0.3739(15) 0.7165(11) 0.8370(12) 0.027(5) Uiso 0.231(10) 1 d PD A 2
H2I H 0.3642 0.7393 0.8023 0.033 Uiso 0.231(10) 1 calc PR A 2
C3G C 0.9938(17) 0.5846(13) 0.2534(18) 0.086(9) Uiso 0.197(10) 1 d PD D 2
H3G1 H 1.0518 0.5973 0.2828 0.103 Uiso 0.197(10) 1 calc PR D 2
H3G2 H 0.9945 0.5789 0.1996 0.103 Uiso 0.197(10) 1 calc PR D 2
O2G O 0.9407(12) 0.5064(11) 0.2615(13) 0.044(6) Uiso 0.197(10) 1 d PD D 2
H2G H 0.9701 0.4872 0.2877 0.053 Uiso 0.197(10) 1 calc PR D 2
C4G C 0.9723(16) 0.6540(12) 0.2765(15) 0.055(6) Uiso 0.197(10) 1 d PD D 2
H4G1 H 1.0098 0.7018 0.2637 0.083 Uiso 0.197(10) 1 calc PR D 2
H4G2 H 0.9787 0.6656 0.3312 0.083 Uiso 0.197(10) 1 calc PR D 2
H4G3 H 0.9140 0.6418 0.2502 0.083 Uiso 0.197(10) 1 calc PR D 2


_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
O1A C1A 1.376(3) . ?
O1A H1A 0.8400 . ?
O11A C23A 1.359(3) . ?
O11A H11A 0.8400 . ?
O9B C17B 1.376(3) . ?
O9B H9B 0.8400 . ?
O3A C3A 1.381(3) . ?
O3A H3A 0.8400 . ?
O4A C8A 1.383(3) . ?
O4A H4A 0.8400 . ?
O2A C2A 1.377(3) . ?
O2A H2A 0.8400 . ?
O5A C9A 1.366(3) . ?
O5A H5A 0.8400 . ?
O1B C1B 1.382(3) . ?
O1B H1B 0.8400 . ?
O7B C15B 1.376(3) . ?
O7B H7B 0.8400 . ?
O6B C10B 1.369(3) . ?
O6B H6B 0.8400 . ?
O10B C22B 1.372(3) . ?
O10B H10B 0.8400 . ?
O2B C2B 1.364(3) . ?
O2B H2B 0.8400 . ?
O5B C9B 1.372(3) . ?
O5B H5B 0.8400 . ?
O6A C10A 1.369(3) . ?
O6A H6A 0.8400 . ?
O8B C16B 1.377(3) . ?
O8B H8B 0.8400 . ?
O3B C3B 1.376(3) . ?
O3B H3B 0.8400 . ?
O12A C24A 1.377(3) . ?
O12A H12A 0.8400 . ?
O11B C23B 1.368(3) . ?
O11B H11B 0.8400 . ?
O10A C22A 1.379(3) . ?
O10A H10A 0.8400 . ?
O7A C15A 1.380(3) . ?
O7A H7A 0.8400 . ?
O4B C8B 1.377(3) . ?
O4B H4B 0.8400 . ?
O12B C24B 1.374(3) . ?
O12B H12B 0.8400 . ?
O9A C17A 1.379(3) . ?
O9A H9A 0.8400 . ?
O1I C1I 1.422(6) . ?
O1I H1I 0.8400 . ?
O1E C1E 1.243(3) . ?
O8A C16A 1.374(3) . ?
O8A H8A 0.8400 . ?
N1E N2E 1.308(3) . ?
N1E C10E 1.332(3) . ?
N2E C11E 1.405(3) . ?
N2E H2E 0.8800 . ?
C12B C11B 1.393(3) . ?
C12B C13B 1.398(3) . ?
C12B H12C 0.9500 . ?
C3A C2A 1.388(3) . ?
C3A C4A 1.397(3) . ?
C4A C5A 1.391(3) . ?
C4A C7A 1.524(3) . ?
C5A C6A 1.391(3) . ?
C5A H5A1 0.9500 . ?
C23A C22A 1.390(3) . ?
C23A C24A 1.393(3) . ?
C26B C25B 1.391(3) . ?
C26B C27B 1.396(3) . ?
C26B H26B 0.9500 . ?
N3E C11E 1.331(3) . ?
N3E C15E 1.346(3) . ?
C12A C11A 1.396(3) . ?
C12A C13A 1.398(3) . ?
C12A H12D 0.9500 . ?
C19B C20B 1.391(3) . ?
C19B C18B 1.392(3) . ?
C19B H19B 0.9500 . ?
C16B C15B 1.396(3) . ?
C16B C17B 1.398(3) . ?
C29A C7A 1.535(3) . ?
C29A H29A 0.9800 . ?
C29A H29B 0.9800 . ?
C29A H29C 0.9800 . ?
C23B C24B 1.387(3) . ?
C23B C22B 1.389(3) . ?
C25A C24A 1.391(3) . ?
C25A C26A 1.404(3) . ?
C25A C28A 1.525(3) . ?
C15B C20B 1.400(3) . ?
C14B C11B 1.525(3) . ?
C14B C20B 1.529(3) . ?
C14B C30B 1.534(3) . ?
C14B H14B 1.0000 . ?
C2B C1B 1.391(3) . ?
C2B C3B 1.393(3) . ?
C2A C1A 1.389(3) . ?
C28A C6A 1.524(3) . ?
C28A C32A 1.529(3) . ?
C28A H28A 1.0000 . ?
C8B C9B 1.388(3) . ?
C8B C13B 1.400(3) . ?
C27B C22B 1.403(3) . ?
C27B C21B 1.523(3) . ?
C13B C7B 1.522(3) . ?
C13A C8A 1.387(3) . ?
C13A C7A 1.526(3) . ?
C6B C5B 1.391(3) . ?
C6B C1B 1.397(3) . ?
C6B C28B 1.530(3) . ?
C1A C6A 1.397(3) . ?
C22A C27A 1.389(3) . ?
C10A C9A 1.393(3) . ?
C10A C11A 1.394(3) . ?
C8A C9A 1.385(3) . ?
C3B C4B 1.395(3) . ?
C4B C5B 1.395(3) . ?
C4B C7B 1.529(3) . ?
C24B C25B 1.396(3) . ?
C28B C25B 1.527(3) . ?
C28B C32B 1.534(3) . ?
C28B H28B 1.0000 . ?
C18B C17B 1.388(3) . ?
C18B C21B 1.523(3) . ?
C9B C10B 1.393(3) . ?
C11B C10B 1.401(3) . ?
C21B C31B 1.539(3) . ?
C21B H21B 1.0000 . ?
C5B H5B1 0.9500 . ?
C19A C20A 1.388(3) . ?
C19A C18A 1.400(3) . ?
C19A H19A 0.9500 . ?
C14A C30A 1.527(3) . ?
C14A C11A 1.527(3) . ?
C14A C20A 1.532(3) . ?
C14A H14A 1.0000 . ?
C26A C27A 1.393(3) . ?
C26A H26A 0.9500 . ?
C7A H7A1 1.0000 . ?
C29B C7B 1.540(3) . ?
C29B H29D 0.9800 . ?
C29B H29E 0.9800 . ?
C29B H29F 0.9800 . ?
C32B H32A 0.9800 . ?
C32B H32B 0.9800 . ?
C32B H32C 0.9800 . ?
C1E C2E 1.455(3) . ?
C1E C10E 1.458(4) . ?
C10E C9E 1.465(3) . ?
C20A C15A 1.395(3) . ?
C15A C16A 1.387(3) . ?
C17A C16A 1.391(4) . ?
C17A C18A 1.393(3) . ?
C27A C21A 1.533(3) . ?
C7B H7B1 1.0000 . ?
C2E C3E 1.340(4) . ?
C2E H2E1 0.9500 . ?
C32A H32D 0.9800 . ?
C32A H32E 0.9800 . ?
C32A H32F 0.9800 . ?
C15E C14E 1.372(4) . ?
C15E H15E 0.9500 . ?
C30B H30A 0.9800 . ?
C30B H30B 0.9800 . ?
C30B H30C 0.9800 . ?
C30A H30D 0.9800 . ?
C30A H30E 0.9800 . ?
C30A H30F 0.9800 . ?
C11E C12E 1.393(4) . ?
C9E C8E 1.401(4) . ?
C9E C4E 1.413(4) . ?
C4E C5E 1.399(4) . ?
C4E C3E 1.441(4) . ?
C18A C21A 1.527(3) . ?
C21A C31A 1.521(3) . ?
C21A H21A 1.0000 . ?
C13E C12E 1.385(4) . ?
C13E C14E 1.387(4) . ?
C13E H13E 0.9500 . ?
C8E C7E 1.385(4) . ?
C8E H8E 0.9500 . ?
C14E H14E 0.9500 . ?
C31B H31A 0.9800 . ?
C31B H31B 0.9800 . ?
C31B H31C 0.9800 . ?
C3E H3E 0.9500 . ?
C31A H31D 0.9800 . ?
C31A H31E 0.9800 . ?
C31A H31F 0.9800 . ?
C7E C6E 1.390(4) . ?
C7E H7E 0.9500 . ?
C12E H12E 0.9500 . ?
C6E C5E 1.380(4) . ?
C6E H6E 0.9500 . ?
C5E H5E 0.9500 . ?
C2I C1I 1.438(6) . ?
C2I H2I1 0.9800 . ?
C2I H2I2 0.9800 . ?
C2I H2I3 0.9800 . ?
C1I H1I1 0.9900 . ?
C1I H1I2 0.9900 . ?
O1D C1D 1.246(3) . ?
N2D N1D 1.318(3) . ?
N2D C11D 1.410(3) . ?
N2D H2D 0.8800 . ?
N1D C10D 1.313(3) . ?
N3D C11D 1.326(3) . ?
N3D C15D 1.348(3) . ?
C1D C2D 1.452(4) . ?
C1D C10D 1.467(3) . ?
C10D C9D 1.468(4) . ?
C11D C12D 1.391(3) . ?
C13D C12D 1.374(4) . ?
C13D C14D 1.385(4) . ?
C13D H13D 0.9500 . ?
C12D H12F 0.9500 . ?
C9D C8D 1.398(4) . ?
C9D C4D 1.412(4) . ?
C8D C7D 1.389(4) . ?
C8D H8D 0.9500 . ?
C15D C14D 1.378(4) . ?
C15D H15D 0.9500 . ?
C14D H14D 0.9500 . ?
C4D C5D 1.403(4) . ?
C4D C3D 1.443(5) . ?
C2D C3D 1.349(4) . ?
C2D H2D1 0.9500 . ?
C7D C6D 1.391(6) . ?
C7D H7D 0.9500 . ?
C5D C6D 1.379(6) . ?
C5D H5D 0.9500 . ?
C3D H3D 0.9500 . ?
C6D H6D 0.9500 . ?
O1C C1C 1.252(3) . ?
N2C N1C 1.316(3) . ?
N2C C11C 1.401(3) . ?
N2C H2C 0.8800 . ?
N1C C10C 1.323(3) . ?
N3C C11C 1.335(3) . ?
N3C C15C 1.344(3) . ?
C11C C12C 1.396(4) . ?
C8C C7C 1.382(4) . ?
C8C C9C 1.405(3) . ?
C8C H8C 0.9500 . ?
C14C C15C 1.380(4) . ?
C14C C13C 1.387(4) . ?
C14C H14C 0.9500 . ?
C15C H15C 0.9500 . ?
C9C C4C 1.408(4) . ?
C9C C10C 1.463(3) . ?
C10C C1C 1.467(3) . ?
C4C C5C 1.404(4) . ?
C4C C3C 1.442(4) . ?
C12C C13C 1.383(4) . ?
C12C H12G 0.9500 . ?
C7C C6C 1.392(4) . ?
C7C H7C 0.9500 . ?
C5C C6C 1.374(4) . ?
C5C H5C 0.9500 . ?
C13C H13C 0.9500 . ?
C6C H6C 0.9500 . ?
C1C C2C 1.442(4) . ?
C2C C3C 1.345(4) . ?
C2C H2C1 0.9500 . ?
C3C H3C 0.9500 . ?
O1F C1F 1.435(4) . ?
O1F H1F 0.8451 . ?
O1H C1H 1.390(4) . ?
O1H H1H 0.8409 . ?
C1H C2H 1.514(6) . ?
C1H H1H1 0.9900 . ?
C1H H1H2 0.9900 . ?
C1F C2F 1.507(7) . ?
C1F H1F1 0.9900 . ?
C1F H1F2 0.9900 . ?
C2H H2H1 0.9800 . ?
C2H H2H2 0.9800 . ?
C2H H2H3 0.9800 . ?
C2F H2F1 0.9800 . ?
C2F H2F2 0.9800 . ?
C2F H2F3 0.9800 . ?
O1G C1G 1.411(5) . ?
O1G H1G 0.8400 . ?
C1G C2G 1.375(9) . ?
C1G H1G1 0.9900 . ?
C1G H1G2 0.9900 . ?
C2G H2G1 0.9800 . ?
C2G H2G2 0.9800 . ?
C2G H2G3 0.9800 . ?
C3I O2I 1.40(2) . ?
C3I C4I 1.451(19) . ?
C3I H3I1 0.9900 . ?
C3I H3I2 0.9900 . ?
C4I H4I1 0.9800 . ?
C4I H4I2 0.9800 . ?
C4I H4I3 0.9800 . ?
O2I H2I 0.8400 . ?
C3G C4G 1.44(2) . ?
C3G O2G 1.44(2) . ?
C3G H3G1 0.9900 . ?
C3G H3G2 0.9900 . ?
O2G H2G 0.8400 . ?
C4G H4G1 0.9800 . ?
C4G H4G2 0.9800 . ?
C4G H4G3 0.9800 . ?

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
C1A O1A H1A 109.5 . . ?
C23A O11A H11A 109.5 . . ?
C17B O9B H9B 109.5 . . ?
C3A O3A H3A 109.5 . . ?
C8A O4A H4A 109.5 . . ?
C2A O2A H2A 109.5 . . ?
C9A O5A H5A 109.5 . . ?
C1B O1B H1B 109.5 . . ?
C15B O7B H7B 109.5 . . ?
C10B O6B H6B 109.5 . . ?
C22B O10B H10B 109.5 . . ?
C2B O2B H2B 109.5 . . ?
C9B O5B H5B 109.5 . . ?
C10A O6A H6A 109.5 . . ?
C16B O8B H8B 109.5 . . ?
C3B O3B H3B 109.5 . . ?
C24A O12A H12A 109.5 . . ?
C23B O11B H11B 109.5 . . ?
C22A O10A H10A 109.5 . . ?
C15A O7A H7A 109.5 . . ?
C8B O4B H4B 109.5 . . ?
C24B O12B H12B 109.5 . . ?
C17A O9A H9A 109.5 . . ?
C16A O8A H8A 109.5 . . ?
N2E N1E C10E 119.9(2) . . ?
N1E N2E C11E 119.4(2) . . ?
N1E N2E H2E 120.3 . . ?
C11E N2E H2E 120.3 . . ?
C11B C12B C13B 123.3(2) . . ?
C11B C12B H12C 118.3 . . ?
C13B C12B H12C 118.3 . . ?
O3A C3A C2A 116.48(19) . . ?
O3A C3A C4A 123.09(19) . . ?
C2A C3A C4A 120.4(2) . . ?
C5A C4A C3A 117.6(2) . . ?
C5A C4A C7A 120.69(19) . . ?
C3A C4A C7A 121.7(2) . . ?
C4A C5A C6A 123.3(2) . . ?
C4A C5A H5A1 118.4 . . ?
C6A C5A H5A1 118.4 . . ?
O11A C23A C22A 117.5(2) . . ?
O11A C23A C24A 123.1(2) . . ?
C22A C23A C24A 119.5(2) . . ?
C25B C26B C27B 123.2(2) . . ?
C25B C26B H26B 118.4 . . ?
C27B C26B H26B 118.4 . . ?
C11E N3E C15E 117.2(2) . . ?
C11A C12A C13A 123.0(2) . . ?
C11A C12A H12D 118.5 . . ?
C13A C12A H12D 118.5 . . ?
C20B C19B C18B 122.7(2) . . ?
C20B C19B H19B 118.7 . . ?
C18B C19B H19B 118.7 . . ?
O8B C16B C15B 125.2(2) . . ?
O8B C16B C17B 115.6(2) . . ?
C15B C16B C17B 119.3(2) . . ?
C7A C29A H29A 109.5 . . ?
C7A C29A H29B 109.5 . . ?
H29A C29A H29B 109.5 . . ?
C7A C29A H29C 109.5 . . ?
H29A C29A H29C 109.5 . . ?
H29B C29A H29C 109.5 . . ?
O11B C23B C24B 116.9(2) . . ?
O11B C23B C22B 122.6(2) . . ?
C24B C23B C22B 120.4(2) . . ?
C24A C25A C26A 117.8(2) . . ?
C24A C25A C28A 119.58(19) . . ?
C26A C25A C28A 122.6(2) . . ?
O7B C15B C16B 122.6(2) . . ?
O7B C15B C20B 117.4(2) . . ?
C16B C15B C20B 120.0(2) . . ?
C11B C14B C20B 109.05(17) . . ?
C11B C14B C30B 113.77(19) . . ?
C20B C14B C30B 111.32(19) . . ?
C11B C14B H14B 107.5 . . ?
C20B C14B H14B 107.5 . . ?
C30B C14B H14B 107.5 . . ?
O2B C2B C1B 122.3(2) . . ?
O2B C2B C3B 117.6(2) . . ?
C1B C2B C3B 120.1(2) . . ?
O2A C2A C3A 122.4(2) . . ?
O2A C2A C1A 116.95(19) . . ?
C3A C2A C1A 120.7(2) . . ?
C6A C28A C25A 110.27(17) . . ?
C6A C28A C32A 110.58(18) . . ?
C25A C28A C32A 114.23(18) . . ?
C6A C28A H28A 107.1 . . ?
C25A C28A H28A 107.1 . . ?
C32A C28A H28A 107.1 . . ?
O4B C8B C9B 115.6(2) . . ?
O4B C8B C13B 123.8(2) . . ?
C9B C8B C13B 120.6(2) . . ?
C26B C27B C22B 117.7(2) . . ?
C26B C27B C21B 122.2(2) . . ?
C22B C27B C21B 120.0(2) . . ?
C12B C13B C8B 117.4(2) . . ?
C12B C13B C7B 122.6(2) . . ?
C8B C13B C7B 119.9(2) . . ?
C8A C13A C12A 117.1(2) . . ?
C8A C13A C7A 119.37(19) . . ?
C12A C13A C7A 123.4(2) . . ?
C5B C6B C1B 117.5(2) . . ?
C5B C6B C28B 120.3(2) . . ?
C1B C6B C28B 122.1(2) . . ?
O1A C1A C2A 121.04(19) . . ?
O1A C1A C6A 118.6(2) . . ?
C2A C1A C6A 120.3(2) . . ?
O10A C22A C27A 119.5(2) . . ?
O10A C22A C23A 119.0(2) . . ?
C27A C22A C23A 121.4(2) . . ?
O6A C10A C9A 114.3(2) . . ?
O6A C10A C11A 125.2(2) . . ?
C9A C10A C11A 120.5(2) . . ?
O4A C8A C9A 118.0(2) . . ?
O4A C8A C13A 120.36(19) . . ?
C9A C8A C13A 121.6(2) . . ?
O3B C3B C2B 121.4(2) . . ?
O3B C3B C4B 118.2(2) . . ?
C2B C3B C4B 120.3(2) . . ?
C5B C4B C3B 118.2(2) . . ?
C5B C4B C7B 120.1(2) . . ?
C3B C4B C7B 121.6(2) . . ?
O12B C24B C23B 119.8(2) . . ?
O12B C24B C25B 119.1(2) . . ?
C23B C24B C25B 121.1(2) . . ?
C25B C28B C6B 110.61(18) . . ?
C25B C28B C32B 113.49(19) . . ?
C6B C28B C32B 110.62(19) . . ?
C25B C28B H28B 107.3 . . ?
C6B C28B H28B 107.3 . . ?
C32B C28B H28B 107.3 . . ?
C17B C18B C19B 117.3(2) . . ?
C17B C18B C21B 120.6(2) . . ?
C19B C18B C21B 122.1(2) . . ?
O5B C9B C8B 118.3(2) . . ?
O5B C9B C10B 121.1(2) . . ?
C8B C9B C10B 120.6(2) . . ?
C19B C20B C15B 118.7(2) . . ?
C19B C20B C14B 120.2(2) . . ?
C15B C20B C14B 121.1(2) . . ?
O1B C1B C2B 115.9(2) . . ?
O1B C1B C6B 123.1(2) . . ?
C2B C1B C6B 121.1(2) . . ?
C12B C11B C10B 117.5(2) . . ?
C12B C11B C14B 123.1(2) . . ?
C10B C11B C14B 119.4(2) . . ?
C27B C21B C18B 111.38(18) . . ?
C27B C21B C31B 113.53(19) . . ?
C18B C21B C31B 110.70(18) . . ?
C27B C21B H21B 106.9 . . ?
C18B C21B H21B 106.9 . . ?
C31B C21B H21B 106.9 . . ?
C26B C25B C24B 117.2(2) . . ?
C26B C25B C28B 123.0(2) . . ?
C24B C25B C28B 119.7(2) . . ?
C6B C5B C4B 122.9(2) . . ?
C6B C5B H5B1 118.6 . . ?
C4B C5B H5B1 118.6 . . ?
C20A C19A C18A 123.3(2) . . ?
C20A C19A H19A 118.4 . . ?
C18A C19A H19A 118.4 . . ?
C30A C14A C11A 114.05(19) . . ?
C30A C14A C20A 111.5(2) . . ?
C11A C14A C20A 110.16(18) . . ?
C30A C14A H14A 106.9 . . ?
C11A C14A H14A 106.9 . . ?
C20A C14A H14A 106.9 . . ?
O12A C24A C25A 125.3(2) . . ?
O12A C24A C23A 113.7(2) . . ?
C25A C24A C23A 121.0(2) . . ?
C27A C26A C25A 122.4(2) . . ?
C27A C26A H26A 118.8 . . ?
C25A C26A H26A 118.8 . . ?
O6B C10B C9B 114.4(2) . . ?
O6B C10B C11B 125.1(2) . . ?
C9B C10B C11B 120.5(2) . . ?
C4A C7A C13A 110.10(17) . . ?
C4A C7A C29A 111.19(18) . . ?
C13A C7A C29A 114.28(18) . . ?
C4A C7A H7A1 107.0 . . ?
C13A C7A H7A1 107.0 . . ?
C29A C7A H7A1 107.0 . . ?
C7B C29B H29D 109.5 . . ?
C7B C29B H29E 109.5 . . ?
H29D C29B H29E 109.5 . . ?
C7B C29B H29F 109.5 . . ?
H29D C29B H29F 109.5 . . ?
H29E C29B H29F 109.5 . . ?
C28B C32B H32A 109.5 . . ?
C28B C32B H32B 109.5 . . ?
H32A C32B H32B 109.5 . . ?
C28B C32B H32C 109.5 . . ?
H32A C32B H32C 109.5 . . ?
H32B C32B H32C 109.5 . . ?
O10B C22B C23B 114.89(19) . . ?
O10B C22B C27B 125.0(2) . . ?
C23B C22B C27B 120.1(2) . . ?
O1E C1E C2E 121.2(2) . . ?
O1E C1E C10E 120.9(2) . . ?
C2E C1E C10E 117.9(2) . . ?
N1E C10E C1E 123.7(2) . . ?
N1E C10E C9E 116.2(2) . . ?
C1E C10E C9E 120.1(2) . . ?
C19A C20A C15A 118.1(2) . . ?
C19A C20A C14A 121.5(2) . . ?
C15A C20A C14A 120.3(2) . . ?
C5A C6A C1A 117.7(2) . . ?
C5A C6A C28A 121.51(19) . . ?
C1A C6A C28A 120.8(2) . . ?
O9B C17B C18B 117.7(2) . . ?
O9B C17B C16B 120.4(2) . . ?
C18B C17B C16B 121.9(2) . . ?
O7A C15A C16A 120.6(2) . . ?
O7A C15A C20A 119.5(2) . . ?
C16A C15A C20A 120.0(2) . . ?
O5A C9A C8A 117.75(19) . . ?
O5A C9A C10A 122.32(19) . . ?
C8A C9A C10A 119.9(2) . . ?
O9A C17A C16A 114.7(2) . . ?
O9A C17A C18A 124.5(2) . . ?
C16A C17A C18A 120.8(2) . . ?
O8A C16A C15A 118.9(2) . . ?
O8A C16A C17A 120.3(2) . . ?
C15A C16A C17A 120.7(2) . . ?
C10A C11A C12A 117.8(2) . . ?
C10A C11A C14A 119.2(2) . . ?
C12A C11A C14A 123.0(2) . . ?
C22A C27A C26A 117.8(2) . . ?
C22A C27A C21A 118.1(2) . . ?
C26A C27A C21A 123.9(2) . . ?
C13B C7B C4B 110.20(18) . . ?
C13B C7B C29B 113.83(19) . . ?
C4B C7B C29B 110.94(19) . . ?
C13B C7B H7B1 107.2 . . ?
C4B C7B H7B1 107.2 . . ?
C29B C7B H7B1 107.2 . . ?
C3E C2E C1E 120.6(2) . . ?
C3E C2E H2E1 119.7 . . ?
C1E C2E H2E1 119.7 . . ?
C28A C32A H32D 109.5 . . ?
C28A C32A H32E 109.5 . . ?
H32D C32A H32E 109.5 . . ?
C28A C32A H32F 109.5 . . ?
H32D C32A H32F 109.5 . . ?
H32E C32A H32F 109.5 . . ?
N3E C15E C14E 123.1(2) . . ?
N3E C15E H15E 118.4 . . ?
C14E C15E H15E 118.4 . . ?
C14B C30B H30A 109.5 . . ?
C14B C30B H30B 109.5 . . ?
H30A C30B H30B 109.5 . . ?
C14B C30B H30C 109.5 . . ?
H30A C30B H30C 109.5 . . ?
H30B C30B H30C 109.5 . . ?
C14A C30A H30D 109.5 . . ?
C14A C30A H30E 109.5 . . ?
H30D C30A H30E 109.5 . . ?
C14A C30A H30F 109.5 . . ?
H30D C30A H30F 109.5 . . ?
H30E C30A H30F 109.5 . . ?
N3E C11E C12E 124.2(2) . . ?
N3E C11E N2E 113.4(2) . . ?
C12E C11E N2E 122.3(2) . . ?
C8E C9E C4E 119.0(2) . . ?
C8E C9E C10E 122.4(2) . . ?
C4E C9E C10E 118.6(2) . . ?
C5E C4E C9E 119.8(2) . . ?
C5E C4E C3E 120.8(2) . . ?
C9E C4E C3E 119.4(2) . . ?
C17A C18A C19A 117.0(2) . . ?
C17A C18A C21A 121.4(2) . . ?
C19A C18A C21A 121.5(2) . . ?
C31A C21A C18A 112.54(19) . . ?
C31A C21A C27A 113.98(19) . . ?
C18A C21A C27A 109.30(18) . . ?
C31A C21A H21A 106.9 . . ?
C18A C21A H21A 106.9 . . ?
C27A C21A H21A 106.9 . . ?
C12E C13E C14E 119.6(2) . . ?
C12E C13E H13E 120.2 . . ?
C14E C13E H13E 120.2 . . ?
C7E C8E C9E 120.2(3) . . ?
C7E C8E H8E 119.9 . . ?
C9E C8E H8E 119.9 . . ?
C15E C14E C13E 118.7(2) . . ?
C15E C14E H14E 120.6 . . ?
C13E C14E H14E 120.6 . . ?
C21B C31B H31A 109.5 . . ?
C21B C31B H31B 109.5 . . ?
H31A C31B H31B 109.5 . . ?
C21B C31B H31C 109.5 . . ?
H31A C31B H31C 109.5 . . ?
H31B C31B H31C 109.5 . . ?
C2E C3E C4E 123.3(2) . . ?
C2E C3E H3E 118.4 . . ?
C4E C3E H3E 118.4 . . ?
C21A C31A H31D 109.5 . . ?
C21A C31A H31E 109.5 . . ?
H31D C31A H31E 109.5 . . ?
C21A C31A H31F 109.5 . . ?
H31D C31A H31F 109.5 . . ?
H31E C31A H31F 109.5 . . ?
C8E C7E C6E 120.5(3) . . ?
C8E C7E H7E 119.7 . . ?
C6E C7E H7E 119.7 . . ?
C13E C12E C11E 117.1(2) . . ?
C13E C12E H12E 121.4 . . ?
C11E C12E H12E 121.4 . . ?
C5E C6E C7E 120.1(2) . . ?
C5E C6E H6E 119.9 . . ?
C7E C6E H6E 119.9 . . ?
C6E C5E C4E 120.3(3) . . ?
C6E C5E H5E 119.9 . . ?
C4E C5E H5E 119.9 . . ?
C1I C2I H2I1 109.5 . . ?
C1I C2I H2I2 109.5 . . ?
H2I1 C2I H2I2 109.5 . . ?
C1I C2I H2I3 109.5 . . ?
H2I1 C2I H2I3 109.5 . . ?
H2I2 C2I H2I3 109.5 . . ?
O1I C1I C2I 112.6(4) . . ?
O1I C1I H1I1 109.1 . . ?
C2I C1I H1I1 109.1 . . ?
O1I C1I H1I2 109.1 . . ?
C2I C1I H1I2 109.1 . . ?
H1I1 C1I H1I2 107.8 . . ?
N1D N2D C11D 117.75(19) . . ?
N1D N2D H2D 121.1 . . ?
C11D N2D H2D 121.1 . . ?
C10D N1D N2D 121.2(2) . . ?
C11D N3D C15D 117.2(2) . . ?
O1D C1D C2D 121.9(2) . . ?
O1D C1D C10D 120.3(2) . . ?
C2D C1D C10D 117.8(2) . . ?
N1D C10D C1D 123.6(2) . . ?
N1D C10D C9D 116.2(2) . . ?
C1D C10D C9D 120.2(2) . . ?
N3D C11D C12D 124.3(2) . . ?
N3D C11D N2D 115.5(2) . . ?
C12D C11D N2D 120.2(2) . . ?
C12D C13D C14D 119.9(2) . . ?
C12D C13D H13D 120.0 . . ?
C14D C13D H13D 120.0 . . ?
C13D C12D C11D 117.3(2) . . ?
C13D C12D H12F 121.4 . . ?
C11D C12D H12F 121.4 . . ?
C8D C9D C4D 119.5(3) . . ?
C8D C9D C10D 122.0(3) . . ?
C4D C9D C10D 118.5(3) . . ?
C7D C8D C9D 120.1(3) . . ?
C7D C8D H8D 119.9 . . ?
C9D C8D H8D 119.9 . . ?
N3D C15D C14D 122.9(3) . . ?
N3D C15D H15D 118.5 . . ?
C14D C15D H15D 118.5 . . ?
C15D C14D C13D 118.4(2) . . ?
C15D C14D H14D 120.8 . . ?
C13D C14D H14D 120.8 . . ?
C5D C4D C9D 119.2(3) . . ?
C5D C4D C3D 121.2(3) . . ?
C9D C4D C3D 119.6(3) . . ?
C3D C2D C1D 120.6(3) . . ?
C3D C2D H2D1 119.7 . . ?
C1D C2D H2D1 119.7 . . ?
C8D C7D C6D 120.5(3) . . ?
C8D C7D H7D 119.7 . . ?
C6D C7D H7D 119.7 . . ?
C6D C5D C4D 120.7(3) . . ?
C6D C5D H5D 119.6 . . ?
C4D C5D H5D 119.6 . . ?
C2D C3D C4D 123.3(3) . . ?
C2D C3D H3D 118.3 . . ?
C4D C3D H3D 118.3 . . ?
C5D C6D C7D 119.9(3) . . ?
C5D C6D H6D 120.1 . . ?
C7D C6D H6D 120.1 . . ?
N1C N2C C11C 121.2(2) . . ?
N1C N2C H2C 119.4 . . ?
C11C N2C H2C 119.4 . . ?
N2C N1C C10C 119.6(2) . . ?
C11C N3C C15C 116.9(2) . . ?
N3C C11C C12C 124.2(2) . . ?
N3C C11C N2C 113.0(2) . . ?
C12C C11C N2C 122.8(2) . . ?
C7C C8C C9C 120.1(2) . . ?
C7C C8C H8C 120.0 . . ?
C9C C8C H8C 120.0 . . ?
C15C C14C C13C 118.8(2) . . ?
C15C C14C H14C 120.6 . . ?
C13C C14C H14C 120.6 . . ?
N3C C15C C14C 123.3(3) . . ?
N3C C15C H15C 118.3 . . ?
C14C C15C H15C 118.3 . . ?
C8C C9C C4C 118.8(2) . . ?
C8C C9C C10C 121.9(2) . . ?
C4C C9C C10C 119.2(2) . . ?
N1C C10C C9C 117.4(2) . . ?
N1C C10C C1C 123.5(2) . . ?
C9C C10C C1C 119.2(2) . . ?
C5C C4C C9C 119.8(2) . . ?
C5C C4C C3C 120.6(2) . . ?
C9C C4C C3C 119.6(2) . . ?
C13C C12C C11C 117.5(2) . . ?
C13C C12C H12G 121.2 . . ?
C11C C12C H12G 121.2 . . ?
C8C C7C C6C 121.1(2) . . ?
C8C C7C H7C 119.5 . . ?
C6C C7C H7C 119.5 . . ?
C6C C5C C4C 120.7(3) . . ?
C6C C5C H5C 119.6 . . ?
C4C C5C H5C 119.6 . . ?
C12C C13C C14C 119.3(3) . . ?
C12C C13C H13C 120.4 . . ?
C14C C13C H13C 120.4 . . ?
C5C C6C C7C 119.5(2) . . ?
C5C C6C H6C 120.3 . . ?
C7C C6C H6C 120.3 . . ?
O1C C1C C2C 121.5(2) . . ?
O1C C1C C10C 120.3(2) . . ?
C2C C1C C10C 118.2(2) . . ?
C3C C2C C1C 121.2(2) . . ?
C3C C2C H2C1 119.4 . . ?
C1C C2C H2C1 119.4 . . ?
C2C C3C C4C 122.5(2) . . ?
C2C C3C H3C 118.7 . . ?
C4C C3C H3C 118.7 . . ?
C1F O1F H1F 109.1 . . ?
C1H O1H H1H 109.5 . . ?
O1H C1H C2H 108.9(3) . . ?
O1H C1H H1H1 109.9 . . ?
C2H C1H H1H1 109.9 . . ?
O1H C1H H1H2 109.9 . . ?
C2H C1H H1H2 109.9 . . ?
H1H1 C1H H1H2 108.3 . . ?
O1F C1F C2F 109.2(4) . . ?
O1F C1F H1F1 109.8 . . ?
C2F C1F H1F1 109.8 . . ?
O1F C1F H1F2 109.8 . . ?
C2F C1F H1F2 109.8 . . ?
H1F1 C1F H1F2 108.3 . . ?
C1H C2H H2H1 109.5 . . ?
C1H C2H H2H2 109.5 . . ?
H2H1 C2H H2H2 109.5 . . ?
C1H C2H H2H3 109.5 . . ?
H2H1 C2H H2H3 109.5 . . ?
H2H2 C2H H2H3 109.5 . . ?
C2G C1G O1G 118.8(5) . . ?
C2G C1G H1G1 107.6 . . ?
O1G C1G H1G1 107.6 . . ?
C2G C1G H1G2 107.6 . . ?
O1G C1G H1G2 107.6 . . ?
H1G1 C1G H1G2 107.1 . . ?
C1G C2G H2G1 109.5 . . ?
C1G C2G H2G2 109.5 . . ?
H2G1 C2G H2G2 109.5 . . ?
C1G C2G H2G3 109.5 . . ?
H2G1 C2G H2G3 109.5 . . ?
H2G2 C2G H2G3 109.5 . . ?
O2I C3I C4I 113.6(14) . . ?
O2I C3I H3I1 108.8 . . ?
C4I C3I H3I1 108.8 . . ?
O2I C3I H3I2 108.8 . . ?
C4I C3I H3I2 108.8 . . ?
H3I1 C3I H3I2 107.7 . . ?
C3I C4I H4I1 109.5 . . ?
C3I C4I H4I2 109.5 . . ?
H4I1 C4I H4I2 109.5 . . ?
C3I C4I H4I3 109.5 . . ?
H4I1 C4I H4I3 109.5 . . ?
H4I2 C4I H4I3 109.5 . . ?
C3I O2I H2I 109.5 . . ?
C4G C3G O2G 118(2) . . ?
C4G C3G H3G1 107.9 . . ?
O2G C3G H3G1 107.9 . . ?
C4G C3G H3G2 107.9 . . ?
O2G C3G H3G2 107.9 . . ?
H3G1 C3G H3G2 107.2 . . ?
C3G O2G H2G 109.5 . . ?
C3G C4G H4G1 109.5 . . ?
C3G C4G H4G2 109.5 . . ?
H4G1 C4G H4G2 109.5 . . ?
C3G C4G H4G3 109.5 . . ?
H4G1 C4G H4G3 109.5 . . ?
H4G2 C4G H4G3 109.5 . . ?

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
C10E N1E N2E C11E 177.0(2) . . . . ?
O3A C3A C4A C5A 177.00(19) . . . . ?
C2A C3A C4A C5A -3.1(3) . . . . ?
O3A C3A C4A C7A -1.6(3) . . . . ?
C2A C3A C4A C7A 178.22(19) . . . . ?
C3A C4A C5A C6A 1.4(3) . . . . ?
C7A C4A C5A C6A -179.97(19) . . . . ?
O8B C16B C15B O7B -0.1(3) . . . . ?
C17B C16B C15B O7B 179.45(19) . . . . ?
O8B C16B C15B C20B -178.43(19) . . . . ?
C17B C16B C15B C20B 1.1(3) . . . . ?
O3A C3A C2A O2A 2.0(3) . . . . ?
C4A C3A C2A O2A -177.92(19) . . . . ?
O3A C3A C2A C1A -176.67(19) . . . . ?
C4A C3A C2A C1A 3.5(3) . . . . ?
C24A C25A C28A C6A 70.4(3) . . . . ?
C26A C25A C28A C6A -108.1(2) . . . . ?
C24A C25A C28A C32A -164.3(2) . . . . ?
C26A C25A C28A C32A 17.2(3) . . . . ?
C25B C26B C27B C22B -1.5(3) . . . . ?
C25B C26B C27B C21B 179.1(2) . . . . ?
C11B C12B C13B C8B -0.6(3) . . . . ?
C11B C12B C13B C7B -177.6(2) . . . . ?
O4B C8B C13B C12B 179.3(2) . . . . ?
C9B C8B C13B C12B 0.8(3) . . . . ?
O4B C8B C13B C7B -3.5(3) . . . . ?
C9B C8B C13B C7B 177.9(2) . . . . ?
C11A C12A C13A C8A -1.2(3) . . . . ?
C11A C12A C13A C7A -178.3(2) . . . . ?
O2A C2A C1A O1A -2.8(3) . . . . ?
C3A C2A C1A O1A 175.92(19) . . . . ?
O2A C2A C1A C6A 179.43(19) . . . . ?
C3A C2A C1A C6A -1.9(3) . . . . ?
O11A C23A C22A O10A 0.5(3) . . . . ?
C24A C23A C22A O10A 179.9(2) . . . . ?
O11A C23A C22A C27A 179.7(2) . . . . ?
C24A C23A C22A C27A -0.9(3) . . . . ?
C12A C13A C8A O4A -177.23(19) . . . . ?
C7A C13A C8A O4A 0.0(3) . . . . ?
C12A C13A C8A C9A 2.0(3) . . . . ?
C7A C13A C8A C9A 179.2(2) . . . . ?
O2B C2B C3B O3B 2.8(3) . . . . ?
C1B C2B C3B O3B -176.7(2) . . . . ?
O2B C2B C3B C4B 178.6(2) . . . . ?
C1B C2B C3B C4B -0.9(3) . . . . ?
O3B C3B C4B C5B 175.54(19) . . . . ?
C2B C3B C4B C5B -0.4(3) . . . . ?
O3B C3B C4B C7B -1.9(3) . . . . ?
C2B C3B C4B C7B -177.9(2) . . . . ?
O11B C23B C24B O12B 0.9(3) . . . . ?
C22B C23B C24B O12B -179.3(2) . . . . ?
O11B C23B C24B C25B -179.2(2) . . . . ?
C22B C23B C24B C25B 0.5(3) . . . . ?
C5B C6B C28B C25B 78.3(3) . . . . ?
C1B C6B C28B C25B -99.3(2) . . . . ?
C5B C6B C28B C32B -48.4(3) . . . . ?
C1B C6B C28B C32B 134.0(2) . . . . ?
C20B C19B C18B C17B 2.5(3) . . . . ?
C20B C19B C18B C21B -178.92(19) . . . . ?
O4B C8B C9B O5B 0.8(3) . . . . ?
C13B C8B C9B O5B 179.5(2) . . . . ?
O4B C8B C9B C10B -179.5(2) . . . . ?
C13B C8B C9B C10B -0.9(3) . . . . ?
C18B C19B C20B C15B 1.0(3) . . . . ?
C18B C19B C20B C14B -175.8(2) . . . . ?
O7B C15B C20B C19B 178.75(19) . . . . ?
C16B C15B C20B C19B -2.9(3) . . . . ?
O7B C15B C20B C14B -4.5(3) . . . . ?
C16B C15B C20B C14B 173.9(2) . . . . ?
C11B C14B C20B C19B 72.1(3) . . . . ?
C30B C14B C20B C19B -54.2(3) . . . . ?
C11B C14B C20B C15B -104.6(2) . . . . ?
C30B C14B C20B C15B 129.0(2) . . . . ?
O2B C2B C1B O1B 1.3(3) . . . . ?
C3B C2B C1B O1B -179.3(2) . . . . ?
O2B C2B C1B C6B -178.2(2) . . . . ?
C3B C2B C1B C6B 1.2(3) . . . . ?
C5B C6B C1B O1B -179.7(2) . . . . ?
C28B C6B C1B O1B -2.1(3) . . . . ?
C5B C6B C1B C2B -0.2(3) . . . . ?
C28B C6B C1B C2B 177.4(2) . . . . ?
C13B C12B C11B C10B 0.4(3) . . . . ?
C13B C12B C11B C14B 178.2(2) . . . . ?
C20B C14B C11B C12B -109.9(2) . . . . ?
C30B C14B C11B C12B 15.0(3) . . . . ?
C20B C14B C11B C10B 67.8(3) . . . . ?
C30B C14B C11B C10B -167.3(2) . . . . ?
C26B C27B C21B C18B 101.1(2) . . . . ?
C22B C27B C21B C18B -78.3(3) . . . . ?
C26B C27B C21B C31B -24.7(3) . . . . ?
C22B C27B C21B C31B 155.9(2) . . . . ?
C17B C18B C21B C27B 106.8(2) . . . . ?
C19B C18B C21B C27B -71.7(3) . . . . ?
C17B C18B C21B C31B -125.9(2) . . . . ?
C19B C18B C21B C31B 55.6(3) . . . . ?
C27B C26B C25B C24B -2.2(3) . . . . ?
C27B C26B C25B C28B 174.4(2) . . . . ?
O12B C24B C25B C26B -177.5(2) . . . . ?
C23B C24B C25B C26B 2.7(3) . . . . ?
O12B C24B C25B C28B 5.8(3) . . . . ?
C23B C24B C25B C28B -174.1(2) . . . . ?
C6B C28B C25B C26B -104.5(2) . . . . ?
C32B C28B C25B C26B 20.5(3) . . . . ?
C6B C28B C25B C24B 72.1(3) . . . . ?
C32B C28B C25B C24B -162.9(2) . . . . ?
C1B C6B C5B C4B -1.1(3) . . . . ?
C28B C6B C5B C4B -178.8(2) . . . . ?
C3B C4B C5B C6B 1.4(3) . . . . ?
C7B C4B C5B C6B 178.9(2) . . . . ?
C26A C25A C24A O12A 175.8(2) . . . . ?
C28A C25A C24A O12A -2.8(3) . . . . ?
C26A C25A C24A C23A -3.4(3) . . . . ?
C28A C25A C24A C23A 178.0(2) . . . . ?
O11A C23A C24A O12A 3.5(3) . . . . ?
C22A C23A C24A O12A -175.84(19) . . . . ?
O11A C23A C24A C25A -177.1(2) . . . . ?
C22A C23A C24A C25A 3.5(3) . . . . ?
C24A C25A C26A C27A 0.8(3) . . . . ?
C28A C25A C26A C27A 179.4(2) . . . . ?
O5B C9B C10B O6B 0.7(3) . . . . ?
C8B C9B C10B O6B -178.97(19) . . . . ?
O5B C9B C10B C11B -179.7(2) . . . . ?
C8B C9B C10B C11B 0.7(3) . . . . ?
C12B C11B C10B O6B 179.2(2) . . . . ?
C14B C11B C10B O6B 1.3(3) . . . . ?
C12B C11B C10B C9B -0.5(3) . . . . ?
C14B C11B C10B C9B -178.3(2) . . . . ?
C5A C4A C7A C13A -73.1(3) . . . . ?
C3A C4A C7A C13A 105.5(2) . . . . ?
C5A C4A C7A C29A 54.6(3) . . . . ?
C3A C4A C7A C29A -126.8(2) . . . . ?
C8A C13A C7A C4A -71.7(3) . . . . ?
C12A C13A C7A C4A 105.3(2) . . . . ?
C8A C13A C7A C29A 162.3(2) . . . . ?
C12A C13A C7A C29A -20.7(3) . . . . ?
O11B C23B C22B O10B -3.2(3) . . . . ?
C24B C23B C22B O10B 177.1(2) . . . . ?
O11B C23B C22B C27B 175.4(2) . . . . ?
C24B C23B C22B C27B -4.4(3) . . . . ?
C26B C27B C22B O10B -176.9(2) . . . . ?
C21B C27B C22B O10B 2.6(3) . . . . ?
C26B C27B C22B C23B 4.7(3) . . . . ?
C21B C27B C22B C23B -175.8(2) . . . . ?
N2E N1E C10E C1E -2.1(4) . . . . ?
N2E N1E C10E C9E 178.2(2) . . . . ?
O1E C1E C10E N1E 3.2(4) . . . . ?
C2E C1E C10E N1E -176.8(2) . . . . ?
O1E C1E C10E C9E -177.2(2) . . . . ?
C2E C1E C10E C9E 2.9(3) . . . . ?
C18A C19A C20A C15A -1.5(3) . . . . ?
C18A C19A C20A C14A -179.9(2) . . . . ?
C30A C14A C20A C19A -50.5(3) . . . . ?
C11A C14A C20A C19A 77.1(3) . . . . ?
C30A C14A C20A C15A 131.2(2) . . . . ?
C11A C14A C20A C15A -101.2(2) . . . . ?
C4A C5A C6A C1A 0.1(3) . . . . ?
C4A C5A C6A C28A -178.65(19) . . . . ?
O1A C1A C6A C5A -177.76(18) . . . . ?
C2A C1A C6A C5A 0.1(3) . . . . ?
O1A C1A C6A C28A 1.0(3) . . . . ?
C2A C1A C6A C28A 178.89(19) . . . . ?
C25A C28A C6A C5A 72.1(3) . . . . ?
C32A C28A C6A C5A -55.2(3) . . . . ?
C25A C28A C6A C1A -106.6(2) . . . . ?
C32A C28A C6A C1A 126.1(2) . . . . ?
C19B C18B C17B O9B 175.00(19) . . . . ?
C21B C18B C17B O9B -3.6(3) . . . . ?
C19B C18B C17B C16B -4.3(3) . . . . ?
C21B C18B C17B C16B 177.10(19) . . . . ?
O8B C16B C17B O9B 2.9(3) . . . . ?
C15B C16B C17B O9B -176.75(19) . . . . ?
O8B C16B C17B C18B -177.80(19) . . . . ?
C15B C16B C17B C18B 2.6(3) . . . . ?
C19A C20A C15A O7A -178.82(19) . . . . ?
C14A C20A C15A O7A -0.5(3) . . . . ?
C19A C20A C15A C16A 1.4(3) . . . . ?
C14A C20A C15A C16A 179.8(2) . . . . ?
O4A C8A C9A O5A 0.1(3) . . . . ?
C13A C8A C9A O5A -179.19(19) . . . . ?
O4A C8A C9A C10A 179.12(19) . . . . ?
C13A C8A C9A C10A -0.1(3) . . . . ?
O6A C10A C9A O5A -3.2(3) . . . . ?
C11A C10A C9A O5A 176.3(2) . . . . ?
O6A C10A C9A C8A 177.83(19) . . . . ?
C11A C10A C9A C8A -2.7(3) . . . . ?
O7A C15A C16A O8A 0.2(3) . . . . ?
C20A C15A C16A O8A 180.0(2) . . . . ?
O7A C15A C16A C17A 179.3(2) . . . . ?
C20A C15A C16A C17A -0.9(3) . . . . ?
O9A C17A C16A O8A -0.8(3) . . . . ?
C18A C17A C16A O8A 179.6(2) . . . . ?
O9A C17A C16A C15A -179.9(2) . . . . ?
C18A C17A C16A C15A 0.4(3) . . . . ?
O6A C10A C11A C12A -177.1(2) . . . . ?
C9A C10A C11A C12A 3.5(3) . . . . ?
O6A C10A C11A C14A 6.0(3) . . . . ?
C9A C10A C11A C14A -173.4(2) . . . . ?
C13A C12A C11A C10A -1.5(3) . . . . ?
C13A C12A C11A C14A 175.2(2) . . . . ?
C30A C14A C11A C10A -160.4(2) . . . . ?
C20A C14A C11A C10A 73.3(3) . . . . ?
C30A C14A C11A C12A 22.8(3) . . . . ?
C20A C14A C11A C12A -103.4(2) . . . . ?
O10A C22A C27A C26A 177.6(2) . . . . ?
C23A C22A C27A C26A -1.7(3) . . . . ?
O10A C22A C27A C21A -6.8(3) . . . . ?
C23A C22A C27A C21A 173.9(2) . . . . ?
C25A C26A C27A C22A 1.7(3) . . . . ?
C25A C26A C27A C21A -173.6(2) . . . . ?
C12B C13B C7B C4B 104.7(2) . . . . ?
C8B C13B C7B C4B -72.3(3) . . . . ?
C12B C13B C7B C29B -20.7(3) . . . . ?
C8B C13B C7B C29B 162.3(2) . . . . ?
C5B C4B C7B C13B -72.3(3) . . . . ?
C3B C4B C7B C13B 105.1(2) . . . . ?
C5B C4B C7B C29B 54.7(3) . . . . ?
C3B C4B C7B C29B -127.9(2) . . . . ?
O1E C1E C2E C3E 176.9(2) . . . . ?
C10E C1E C2E C3E -3.1(4) . . . . ?
C11E N3E C15E C14E 0.4(4) . . . . ?
C15E N3E C11E C12E 0.0(4) . . . . ?
C15E N3E C11E N2E 179.4(2) . . . . ?
N1E N2E C11E N3E 179.2(2) . . . . ?
N1E N2E C11E C12E -1.4(4) . . . . ?
N1E C10E C9E C8E -1.8(4) . . . . ?
C1E C10E C9E C8E 178.5(2) . . . . ?
N1E C10E C9E C4E 179.5(2) . . . . ?
C1E C10E C9E C4E -0.1(3) . . . . ?
C8E C9E C4E C5E -2.2(4) . . . . ?
C10E C9E C4E C5E 176.5(2) . . . . ?
C8E C9E C4E C3E 178.9(2) . . . . ?
C10E C9E C4E C3E -2.4(3) . . . . ?
O9A C17A C18A C19A 179.9(2) . . . . ?
C16A C17A C18A C19A -0.5(3) . . . . ?
O9A C17A C18A C21A 2.1(3) . . . . ?
C16A C17A C18A C21A -178.3(2) . . . . ?
C20A C19A C18A C17A 1.1(3) . . . . ?
C20A C19A C18A C21A 178.9(2) . . . . ?
C17A C18A C21A C31A -129.5(2) . . . . ?
C19A C18A C21A C31A 52.8(3) . . . . ?
C17A C18A C21A C27A 102.8(2) . . . . ?
C19A C18A C21A C27A -74.9(3) . . . . ?
C22A C27A C21A C31A 161.0(2) . . . . ?
C26A C27A C21A C31A -23.7(3) . . . . ?
C22A C27A C21A C18A -72.1(3) . . . . ?
C26A C27A C21A C18A 103.2(2) . . . . ?
C4E C9E C8E C7E 1.7(4) . . . . ?
C10E C9E C8E C7E -177.0(3) . . . . ?
N3E C15E C14E C13E -0.1(4) . . . . ?
C12E C13E C14E C15E -0.6(4) . . . . ?
C1E C2E C3E C4E 0.6(4) . . . . ?
C5E C4E C3E C2E -176.6(3) . . . . ?
C9E C4E C3E C2E 2.3(4) . . . . ?
C9E C8E C7E C6E 0.6(4) . . . . ?
C14E C13E C12E C11E 1.0(4) . . . . ?
N3E C11E C12E C13E -0.7(4) . . . . ?
N2E C11E C12E C13E 180.0(2) . . . . ?
C8E C7E C6E C5E -2.3(4) . . . . ?
C7E C6E C5E C4E 1.8(4) . . . . ?
C9E C4E C5E C6E 0.4(4) . . . . ?
C3E C4E C5E C6E 179.4(2) . . . . ?
C11D N2D N1D C10D -176.0(2) . . . . ?
N2D N1D C10D C1D -0.5(4) . . . . ?
N2D N1D C10D C9D 178.0(2) . . . . ?
O1D C1D C10D N1D -2.4(4) . . . . ?
C2D C1D C10D N1D 176.6(2) . . . . ?
O1D C1D C10D C9D 179.1(2) . . . . ?
C2D C1D C10D C9D -1.8(3) . . . . ?
C15D N3D C11D C12D 1.1(4) . . . . ?
C15D N3D C11D N2D -178.6(2) . . . . ?
N1D N2D C11D N3D 175.5(2) . . . . ?
N1D N2D C11D C12D -4.2(3) . . . . ?
C14D C13D C12D C11D 0.2(4) . . . . ?
N3D C11D C12D C13D -1.2(4) . . . . ?
N2D C11D C12D C13D 178.5(2) . . . . ?
N1D C10D C9D C8D 2.6(4) . . . . ?
C1D C10D C9D C8D -178.9(2) . . . . ?
N1D C10D C9D C4D -175.8(2) . . . . ?
C1D C10D C9D C4D 2.8(4) . . . . ?
C4D C9D C8D C7D -0.5(4) . . . . ?
C10D C9D C8D C7D -178.9(3) . . . . ?
C11D N3D C15D C14D -0.1(4) . . . . ?
N3D C15D C14D C13D -0.7(4) . . . . ?
C12D C13D C14D C15D 0.6(4) . . . . ?
C8D C9D C4D C5D -0.4(4) . . . . ?
C10D C9D C4D C5D 178.0(3) . . . . ?
C8D C9D C4D C3D 179.9(3) . . . . ?
C10D C9D C4D C3D -1.7(4) . . . . ?
O1D C1D C2D C3D 178.8(3) . . . . ?
C10D C1D C2D C3D -0.2(4) . . . . ?
C9D C8D C7D C6D 1.4(5) . . . . ?
C9D C4D C5D C6D 0.5(5) . . . . ?
C3D C4D C5D C6D -179.8(3) . . . . ?
C1D C2D C3D C4D 1.4(5) . . . . ?
C5D C4D C3D C2D 179.9(3) . . . . ?
C9D C4D C3D C2D -0.4(5) . . . . ?
C4D C5D C6D C7D 0.4(6) . . . . ?
C8D C7D C6D C5D -1.3(6) . . . . ?
C11C N2C N1C C10C 177.5(2) . . . . ?
C15C N3C C11C C12C 0.7(4) . . . . ?
C15C N3C C11C N2C -179.5(2) . . . . ?
N1C N2C C11C N3C -173.6(2) . . . . ?
N1C N2C C11C C12C 6.2(4) . . . . ?
C11C N3C C15C C14C -1.0(4) . . . . ?
C13C C14C C15C N3C 1.0(4) . . . . ?
C7C C8C C9C C4C 0.4(4) . . . . ?
C7C C8C C9C C10C -179.7(2) . . . . ?
N2C N1C C10C C9C -178.8(2) . . . . ?
N2C N1C C10C C1C 0.2(4) . . . . ?
C8C C9C C10C N1C -2.6(3) . . . . ?
C4C C9C C10C N1C 177.3(2) . . . . ?
C8C C9C C10C C1C 178.4(2) . . . . ?
C4C C9C C10C C1C -1.7(3) . . . . ?
C8C C9C C4C C5C 0.4(4) . . . . ?
C10C C9C C4C C5C -179.5(2) . . . . ?
C8C C9C C4C C3C -180.0(2) . . . . ?
C10C C9C C4C C3C 0.1(4) . . . . ?
N3C C11C C12C C13C -0.3(4) . . . . ?
N2C C11C C12C C13C 179.9(2) . . . . ?
C9C C8C C7C C6C -1.1(4) . . . . ?
C9C C4C C5C C6C -0.5(4) . . . . ?
C3C C4C C5C C6C 179.9(3) . . . . ?
C11C C12C C13C C14C 0.2(4) . . . . ?
C15C C14C C13C C12C -0.6(4) . . . . ?
C4C C5C C6C C7C -0.2(4) . . . . ?
C8C C7C C6C C5C 1.0(4) . . . . ?
N1C C10C C1C O1C 3.4(4) . . . . ?
C9C C10C C1C O1C -177.6(3) . . . . ?
N1C C10C C1C C2C -176.4(2) . . . . ?
C9C C10C C1C C2C 2.6(4) . . . . ?
O1C C1C C2C C3C 178.3(3) . . . . ?
C10C C1C C2C C3C -1.9(4) . . . . ?
C1C C2C C3C C4C 0.3(5) . . . . ?
C5C C4C C3C C2C -179.8(3) . . . . ?
C9C C4C C3C C2C 0.7(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.944
_diffrn_reflns_theta_full        70.25
_diffrn_measured_fraction_theta_full 0.944
_refine_diff_density_max         0.602
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.085

_database_code_depnum_ccdc_archive 'CCDC 1002495'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2cp55o

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            
'C-methylpyrogallol[4]arene with 1-(2-pyridylazo)-2-napthol'
_chemical_formula_moiety         'C32 H32 O12, 2(C15 H11 O1 N3), 3(C3 H8 O1)'
_chemical_formula_sum            'C71 H78 N6 O17'
_chemical_melting_point          ?

_exptl_crystal_description       plate
_exptl_crystal_colour            orange

_diffrn_ambient_temperature      100(2)
_chemical_formula_weight         1287.39

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0020 0.0018 '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 -0.0030 0.0037 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O -0.0041 0.0068 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_int_tables_number      15
_chemical_absolute_configuration ?

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

_cell_length_a                   29.9239(11)
_cell_length_b                   19.7720(7)
_cell_length_c                   23.7677(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 116.033(2)
_cell_angle_gamma                90.00
_cell_volume                     12635.5(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9208
_cell_measurement_theta_min      2.2
_cell_measurement_theta_max      27.8
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5456
_exptl_absorpt_coefficient_mu    0.108
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_process_details   
;
 Data were corrected for decay and absorption using the program SADABS 
 (Sheldrick, G. M. (2003). SADABS. Version 2.10. University of
 Göttingen, Germany).
;

_exptl_special_details           
; 
 ? 
;
_diffrn_radiation_probe          ?
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_source                   'Advanced Light Source Station 11.3.1'
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker APEXII CCD diffractometer'
_diffrn_measurement_method       'ω/θ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.0
_diffrn_reflns_number            52259
_diffrn_reflns_av_R_equivalents  0.0691
_diffrn_reflns_av_sigmaI/netI    0.0643
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.94
_diffrn_reflns_theta_max         27.94
_reflns_number_total             11646
_reflns_number_gt                8730
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2008)'
_computing_structure_solution    'SHELXS-1997 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-1997 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-SEED, Barbour, 2001'
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0869P)²+9.7858P] where P=(Fo²+2Fc²)/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         11646
_refine_ls_number_parameters     859
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0774
_refine_ls_R_factor_gt           0.0570
_refine_ls_wR_factor_ref         0.1679
_refine_ls_wR_factor_gt          0.1556
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.34687(6) 0.29066(8) 1.02343(8) 0.0285(4) Uani 1 1 d . . .
H1 H 0.3518 0.2510 1.0376 0.034 Uiso 1 1 calc R . .
C1 C 0.25068(8) 0.40915(12) 1.01253(10) 0.0222(5) Uani 1 1 d . . .
H13 H 0.2382 0.4522 0.9949 0.027 Uiso 1 1 calc R . .
O1I O 0.47620(8) 0.27903(11) 0.60008(10) 0.0490(5) Uani 1 1 d . . .
H1I H 0.5071 0.2809 0.6116 0.059 Uiso 1 1 d . . .
C1I C 0.40287(13) 0.34537(19) 0.5620(2) 0.0691(11) Uani 1 1 d . . .
H1I1 H 0.3957 0.3333 0.5189 0.104 Uiso 1 1 calc R . .
H1I2 H 0.3894 0.3904 0.5626 0.104 Uiso 1 1 calc R . .
H1I3 H 0.3875 0.3122 0.5786 0.104 Uiso 1 1 calc R . .
O1P O 0.20268(6) 0.27920(8) 0.74383(8) 0.0291(4) Uani 1 1 d . . .
N1P N 0.12087(8) 0.45095(11) 0.65549(9) 0.0297(5) Uani 1 1 d . . .
C1P C 0.13469(9) 0.22170(12) 0.66491(11) 0.0255(5) Uani 1 1 d . . .
O2 O 0.30426(6) 0.22123(8) 1.08835(8) 0.0270(4) Uani 1 1 d . . .
H2 H 0.2809 0.1968 1.0876 0.032 Uiso 1 1 d . . .
C2 C 0.28990(8) 0.38157(12) 1.00355(10) 0.0231(5) Uani 1 1 d . . .
O2I O 0.42473(8) 0.28593(12) 0.85480(10) 0.0509(6) Uani 1 1 d . . .
H2I H 0.4164 0.2578 0.8254 0.061 Uiso 1 1 calc R . .
C2I C 0.45768(13) 0.34571(16) 0.60132(17) 0.0541(9) Uani 1 1 d . . .
H16 H 0.4735 0.3788 0.5838 0.065 Uiso 1 1 calc R . .
O2P O -0.02979(6) 0.26755(8) 0.63081(8) 0.0312(4) Uani 1 1 d . . .
N2P N 0.12548(7) 0.33593(10) 0.66091(9) 0.0264(4) Uani 1 1 d . . .
H2P1 H 0.1547 0.3402 0.6934 0.032 Uiso 1 1 calc R . .
C2P C 0.18311(9) 0.22380(12) 0.71934(11) 0.0253(5) Uani 1 1 d . . .
O3 O 0.22649(6) 0.28007(8) 1.10464(8) 0.0286(4) Uani 1 1 d . . .
H3 H 0.2478 0.2546 1.1311 0.034 Uiso 1 1 d . . .
C3 C 0.30752(8) 0.31811(12) 1.02985(11) 0.0236(5) Uani 1 1 d . . .
O3I O 0.27597(8) 0.29612(10) 0.70340(11) 0.0488(5) Uani 1 1 d . . .
H3I H 0.2566 0.2983 0.7204 0.059 Uiso 1 1 calc R . .
C3I C 0.46996(16) 0.36442(19) 0.66772(18) 0.0663(10) Uani 1 1 d . . .
H3I1 H 0.5061 0.3647 0.6927 0.099 Uiso 1 1 calc R . .
H3I2 H 0.4551 0.3313 0.6852 0.099 Uiso 1 1 calc R . .
H3I3 H 0.4567 0.4095 0.6687 0.099 Uiso 1 1 calc R . .
N3P N 0.10848(7) 0.27613(10) 0.63868(9) 0.0263(4) Uani 1 1 d . . .
C3P C 0.20795(9) 0.16046(13) 0.74264(12) 0.0282(5) Uani 1 1 d . . .
H3P H 0.2393 0.1602 0.7783 0.034 Uiso 1 1 calc R . .
O4 O 0.11393(6) 0.34593(8) 0.95769(8) 0.0257(4) Uani 1 1 d . . .
H4 H 0.0882 0.3324 0.9270 0.031 Uiso 1 1 calc R . .
C4 C 0.28531(8) 0.28399(11) 1.06204(11) 0.0243(5) Uani 1 1 d . . .
C4I C 0.42148(18) 0.1945(2) 0.9191(2) 0.0806(13) Uani 1 1 d . . .
H4I1 H 0.4085 0.1638 0.8831 0.121 Uiso 1 1 calc R . .
H4I2 H 0.4088 0.1808 0.9491 0.121 Uiso 1 1 calc R . .
H4I3 H 0.4579 0.1925 0.9394 0.121 Uiso 1 1 calc R . .
N4P N 0.04590(7) 0.44403(10) 0.72696(9) 0.0240(4) Uani 1 1 d . . .
C4P C 0.18776(9) 0.10196(13) 0.71512(12) 0.0284(5) Uani 1 1 d . . .
H4P H 0.2054 0.0613 0.7322 0.034 Uiso 1 1 calc R . .
O5 O 0.04048(6) 0.41257(8) 0.86641(8) 0.0270(4) Uani 1 1 d . . .
H5 H 0.0164 0.4373 0.8441 0.032 Uiso 1 1 calc R . .
C5 C 0.24706(8) 0.31287(12) 1.07102(10) 0.0240(5) Uani 1 1 d . . .
C5I C 0.40502(12) 0.26510(19) 0.89752(17) 0.0569(9) Uani 1 1 d . . .
H5I H 0.3679 0.2665 0.8755 0.068 Uiso 1 1 calc R . .
N5P N 0.04327(7) 0.32896(10) 0.71932(9) 0.0229(4) Uani 1 1 d . . .
H5P H 0.0148 0.3328 0.6856 0.028 Uiso 1 1 calc R . .
C5P C 0.14052(9) 0.09750(13) 0.66079(11) 0.0273(5) Uani 1 1 d . . .
O6 O 0.03344(6) 0.54834(8) 0.86370(8) 0.0269(4) Uani 1 1 d . . .
H6 H 0.0366 0.5906 0.8644 0.032 Uiso 1 1 calc R . .
C6 C 0.22883(8) 0.37650(12) 1.04615(10) 0.0231(5) Uani 1 1 d . . .
C6I C 0.42294(16) 0.3153(2) 0.9497(2) 0.0761(12) Uani 1 1 d . . .
H6I1 H 0.4109 0.3605 0.9329 0.114 Uiso 1 1 calc R . .
H6I2 H 0.4594 0.3154 0.9704 0.114 Uiso 1 1 calc R . .
H6I3 H 0.4103 0.3031 0.9801 0.114 Uiso 1 1 calc R . .
N6P N 0.06218(7) 0.26916(10) 0.74036(9) 0.0229(4) Uani 1 1 d . . .
C6P C 0.12137(10) 0.03505(14) 0.63278(12) 0.0331(6) Uani 1 1 d . . .
H6P H 0.1401 -0.0051 0.6491 0.040 Uiso 1 1 calc R . .
O7 O 0.03858(6) 0.68568(9) 0.83437(8) 0.0297(4) Uani 1 1 d . . .
H7 H 0.0362 0.7142 0.8591 0.036 Uiso 1 1 calc R . .
C7 C 0.19085(8) 0.41149(12) 1.06203(11) 0.0241(5) Uani 1 1 d . . .
H17 H 0.1735 0.3754 1.0744 0.029 Uiso 1 1 calc R . .
C7I C 0.32052(13) 0.39894(18) 0.74560(16) 0.0553(9) Uani 1 1 d . . .
H7I1 H 0.3059 0.4018 0.7753 0.083 Uiso 1 1 calc R . .
H7I2 H 0.3268 0.4446 0.7348 0.083 Uiso 1 1 calc R . .
H7I3 H 0.3519 0.3739 0.7648 0.083 Uiso 1 1 calc R . .
C7P C 0.07588(10) 0.03143(15) 0.58202(13) 0.0391(7) Uani 1 1 d . . .
H7P H 0.0628 -0.0111 0.5637 0.047 Uiso 1 1 calc R . .
O8 O 0.06457(7) 0.71471(10) 0.74070(8) 0.0363(4) Uani 1 1 d . . .
H8 H 0.0361 0.7085 0.7385 0.044 Uiso 1 1 calc R . .
C8 C 0.14928(8) 0.52052(12) 1.00683(11) 0.0225(5) Uani 1 1 d . . .
H18 H 0.1749 0.5450 1.0395 0.027 Uiso 1 1 calc R . .
C8I C 0.28517(11) 0.36297(15) 0.68742(15) 0.0434(7) Uani 1 1 d . . .
H8I H 0.2531 0.3884 0.6686 0.052 Uiso 1 1 calc R . .
C8P C 0.04886(10) 0.09029(15) 0.55736(14) 0.0404(7) Uani 1 1 d . . .
H8P H 0.0174 0.0876 0.5220 0.048 Uiso 1 1 calc R . .
O9 O 0.15709(7) 0.69640(10) 0.75351(8) 0.0333(4) Uani 1 1 d . . .
H9 H 0.1764 0.7297 0.7612 0.040 Uiso 1 1 calc R . .
C9 C 0.15122(8) 0.45014(12) 1.00844(10) 0.0218(5) Uani 1 1 d . . .
C9I C 0.30467(14) 0.35637(18) 0.63951(18) 0.0595(9) Uani 1 1 d . . .
H9I1 H 0.2803 0.3324 0.6028 0.089 Uiso 1 1 calc R . .
H9I2 H 0.3359 0.3309 0.6573 0.089 Uiso 1 1 calc R . .
H9I3 H 0.3106 0.4015 0.6270 0.089 Uiso 1 1 calc R . .
C9P C 0.06722(10) 0.15225(14) 0.58360(12) 0.0348(6) Uani 1 1 d . . .
H9P H 0.0484 0.1920 0.5662 0.042 Uiso 1 1 calc R . .
O10 O 0.19319(6) 0.56436(8) 0.75156(7) 0.0278(4) Uani 1 1 d . . .
H10 H 0.1899 0.6056 0.7574 0.033 Uiso 1 1 calc R . .
C10 C 0.11375(8) 0.41568(11) 0.95968(11) 0.0225(5) Uani 1 1 d . . .
C10P C 0.11364(9) 0.15694(13) 0.63606(11) 0.0270(5) Uani 1 1 d . . .
O11 O 0.21011(6) 0.42989(8) 0.74960(7) 0.0281(4) Uani 1 1 d . . .
H11 H 0.1838 0.4488 0.7244 0.034 Uiso 1 1 calc R . .
C11 C 0.07519(8) 0.45002(12) 0.91214(11) 0.0221(5) Uani 1 1 d . . .
C11P C 0.09716(9) 0.39320(13) 0.63295(11) 0.0279(5) Uani 1 1 d . . .
O12 O 0.26333(6) 0.36025(8) 0.85369(8) 0.0269(4) Uani 1 1 d . . .
H12 H 0.2424 0.3465 0.8185 0.032 Uiso 1 1 calc R . .
C12 C 0.07389(8) 0.52045(12) 0.91265(11) 0.0222(5) Uani 1 1 d . . .
C12P C 0.04871(10) 0.38877(14) 0.58714(12) 0.0326(6) Uani 1 1 d . . .
H12P H 0.0333 0.3463 0.5717 0.039 Uiso 1 1 calc R . .
C13 C 0.11135(8) 0.55673(11) 0.95938(11) 0.0216(5) Uani 1 1 d . . .
C13P C 0.02369(10) 0.44884(15) 0.56487(12) 0.0361(6) Uani 1 1 d . . .
H13P H -0.0098 0.4484 0.5337 0.043 Uiso 1 1 calc R . .
C14 C 0.11117(8) 0.63371(11) 0.95619(11) 0.0227(5) Uani 1 1 d . . .
H14 H 0.0763 0.6490 0.9444 0.027 Uiso 1 1 calc R . .
C14P C 0.04747(11) 0.50944(14) 0.58789(12) 0.0369(6) Uani 1 1 d . . .
H14P H 0.0305 0.5511 0.5730 0.044 Uiso 1 1 calc R . .
C15 C 0.17179(8) 0.64536(11) 0.90881(11) 0.0224(5) Uani 1 1 d . . .
H15 H 0.1968 0.6289 0.9474 0.027 Uiso 1 1 calc R . .
C15P C 0.09570(10) 0.50880(14) 0.63236(12) 0.0357(6) Uani 1 1 d . . .
H15P H 0.1121 0.5507 0.6476 0.043 Uiso 1 1 calc R . .
C16 C 0.12397(8) 0.65460(11) 0.90332(11) 0.0221(5) Uani 1 1 d . . .
C16P C -0.00912(9) 0.21354(12) 0.65610(11) 0.0256(5) Uani 1 1 d . . .
C17 C 0.08812(8) 0.67874(11) 0.84647(11) 0.0241(5) Uani 1 1 d . . .
C17P C 0.03868(8) 0.21406(12) 0.71224(11) 0.0226(5) Uani 1 1 d . . .
C18 C 0.09974(9) 0.69237(12) 0.79746(11) 0.0262(5) Uani 1 1 d . . .
C18P C 0.06297(8) 0.15020(12) 0.74056(11) 0.0240(5) Uani 1 1 d . . .
C19 C 0.14791(9) 0.68358(12) 0.80478(11) 0.0255(5) Uani 1 1 d . . .
C19P C 0.10875(9) 0.14876(13) 0.79384(11) 0.0261(5) Uani 1 1 d . . .
H19P H 0.1254 0.1898 0.8118 0.031 Uiso 1 1 calc R . .
C20 C 0.18471(8) 0.65901(11) 0.86068(11) 0.0232(5) Uani 1 1 d . . .
C20P C 0.12970(9) 0.08777(13) 0.82026(12) 0.0311(6) Uani 1 1 d . . .
H20P H 0.1609 0.0869 0.8563 0.037 Uiso 1 1 calc R . .
C21 C 0.23678(8) 0.64371(12) 0.86784(11) 0.0248(5) Uani 1 1 d . . .
H21 H 0.2390 0.6640 0.8306 0.030 Uiso 1 1 calc R . .
C21P C 0.10556(10) 0.02758(13) 0.79467(13) 0.0336(6) Uani 1 1 d . . .
H21P H 0.1199 -0.0142 0.8138 0.040 Uiso 1 1 calc R . .
C22 C 0.27448(8) 0.53007(12) 0.91754(11) 0.0229(5) Uani 1 1 d . . .
H22 H 0.2902 0.5526 0.9567 0.027 Uiso 1 1 calc R . .
C22P C 0.06114(10) 0.02813(13) 0.74182(13) 0.0317(6) Uani 1 1 d . . .
H22P H 0.0453 -0.0134 0.7240 0.038 Uiso 1 1 calc R . .
C23 C 0.24459(8) 0.56800(12) 0.86485(11) 0.0234(5) Uani 1 1 d . . .
C23P C 0.03898(9) 0.08928(12) 0.71381(12) 0.0275(5) Uani 1 1 d . . .
C24 C 0.22242(8) 0.53427(12) 0.80765(11) 0.0242(5) Uani 1 1 d . . .
C24P C -0.00826(9) 0.09105(13) 0.65955(12) 0.0295(6) Uani 1 1 d . . .
H24P H -0.0241 0.0493 0.6422 0.035 Uiso 1 1 calc R . .
C25 C 0.22983(8) 0.46505(12) 0.80449(11) 0.0247(5) Uani 1 1 d . . .
C25P C -0.03120(9) 0.14872(13) 0.63202(12) 0.0292(6) Uani 1 1 d . . .
H25P H -0.0624 0.1467 0.5961 0.035 Uiso 1 1 calc R . .
C26 C 0.25832(8) 0.42887(12) 0.85789(11) 0.0231(5) Uani 1 1 d . . .
C26P C 0.06902(8) 0.38626(12) 0.75128(11) 0.0223(5) Uani 1 1 d . . .
C27 C 0.28244(8) 0.46100(12) 0.91575(11) 0.0226(5) Uani 1 1 d . . .
C27P C 0.11460(9) 0.38222(12) 0.80378(11) 0.0254(5) Uani 1 1 d . . .
H27P H 0.1300 0.3398 0.8196 0.030 Uiso 1 1 calc R . .
C28 C 0.31660(8) 0.42058(12) 0.97235(11) 0.0235(5) Uani 1 1 d . . .
H28 H 0.3336 0.3865 0.9574 0.028 Uiso 1 1 calc R . .
C28P C 0.13659(8) 0.44184(13) 0.83199(11) 0.0270(5) Uani 1 1 d . . .
H28P H 0.1677 0.4414 0.8682 0.032 Uiso 1 1 calc R . .
C29 C 0.21906(9) 0.45540(13) 1.12014(11) 0.0308(6) Uani 1 1 d . . .
H29A H 0.1952 0.4784 1.1316 0.046 Uiso 1 1 calc R . .
H29B H 0.2390 0.4891 1.1110 0.046 Uiso 1 1 calc R . .
H29C H 0.2410 0.4267 1.1550 0.046 Uiso 1 1 calc R . .
C29P C 0.11319(9) 0.50270(12) 0.80735(11) 0.0263(5) Uani 1 1 d . . .
H29P H 0.1280 0.5444 0.8262 0.032 Uiso 1 1 calc R . .
C30 C 0.14439(9) 0.66798(12) 1.01764(11) 0.0281(5) Uani 1 1 d . . .
H30A H 0.1423 0.7171 1.0119 0.042 Uiso 1 1 calc R . .
H30B H 0.1788 0.6533 1.0312 0.042 Uiso 1 1 calc R . .
H30C H 0.1334 0.6556 1.0496 0.042 Uiso 1 1 calc R . .
C30P C 0.06821(9) 0.50160(12) 0.75530(11) 0.0259(5) Uani 1 1 d . . .
H30P H 0.0522 0.5434 0.7386 0.031 Uiso 1 1 calc R . .
C31 C 0.27662(9) 0.67826(13) 0.92530(12) 0.0311(6) Uani 1 1 d . . .
H31A H 0.2693 0.7267 0.9240 0.047 Uiso 1 1 calc R . .
H31B H 0.3092 0.6719 0.9256 0.047 Uiso 1 1 calc R . .
H31C H 0.2770 0.6584 0.9633 0.047 Uiso 1 1 calc R . .
C32 C 0.35746(9) 0.46385(13) 1.02178(12) 0.0301(6) Uani 1 1 d . . .
H32A H 0.3786 0.4353 1.0572 0.045 Uiso 1 1 calc R . .
H32B H 0.3422 0.4994 1.0364 0.045 Uiso 1 1 calc R . .
H32C H 0.3777 0.4846 1.0034 0.045 Uiso 1 1 calc R . .


_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 C3 1.365(3) . ?
O1 H1 0.8400 . ?
C1 C6 1.393(3) . ?
C1 C2 1.393(3) . ?
C1 H13 0.9500 . ?
O1I C2I 1.436(4) . ?
O1I H1I 0.8414 . ?
C1I C2I 1.489(5) . ?
C1I H1I1 0.9800 . ?
C1I H1I2 0.9800 . ?
C1I H1I3 0.9800 . ?
O1P C2P 1.258(3) . ?
N1P C11P 1.327(3) . ?
N1P C15P 1.347(3) . ?
C1P N3P 1.316(3) . ?
C1P C10P 1.458(3) . ?
C1P C2P 1.459(3) . ?
O2 C4 1.393(3) . ?
O2 H2 0.8437 . ?
C2 C3 1.398(3) . ?
C2 C28 1.517(3) . ?
O2I C5I 1.440(4) . ?
O2I H2I 0.8400 . ?
C2I C3I 1.501(5) . ?
C2I H16 1.0000 . ?
O2P C16P 1.248(3) . ?
N2P N3P 1.304(3) . ?
N2P C11P 1.396(3) . ?
N2P H2P1 0.8800 . ?
C2P C3P 1.437(3) . ?
O3 C5 1.367(3) . ?
O3 H3 0.8394 . ?
C3 C4 1.389(4) . ?
O3I C8I 1.435(4) . ?
O3I H3I 0.8400 . ?
C3I H3I1 0.9800 . ?
C3I H3I2 0.9800 . ?
C3I H3I3 0.9800 . ?
C3P C4P 1.336(4) . ?
C3P H3P 0.9500 . ?
O4 C10 1.380(3) . ?
O4 H4 0.8400 . ?
C4 C5 1.377(3) . ?
C4I C5I 1.495(6) . ?
C4I H4I1 0.9800 . ?
C4I H4I2 0.9800 . ?
C4I H4I3 0.9800 . ?
N4P C26P 1.329(3) . ?
N4P C30P 1.342(3) . ?
C4P C5P 1.439(3) . ?
C4P H4P 0.9500 . ?
O5 C11 1.348(3) . ?
O5 H5 0.8400 . ?
C5 C6 1.395(3) . ?
C5I C6I 1.493(5) . ?
C5I H5I 1.0000 . ?
N5P N6P 1.312(3) . ?
N5P C26P 1.393(3) . ?
N5P H5P 0.8800 . ?
C5P C10P 1.400(3) . ?
C5P C6P 1.400(4) . ?
O6 C12 1.374(3) . ?
O6 H6 0.8400 . ?
C6 C7 1.513(3) . ?
C6I H6I1 0.9800 . ?
C6I H6I2 0.9800 . ?
C6I H6I3 0.9800 . ?
N6P C17P 1.310(3) . ?
C6P C7P 1.368(4) . ?
C6P H6P 0.9500 . ?
O7 C17 1.388(3) . ?
O7 H7 0.8400 . ?
C7 C9 1.512(3) . ?
C7 C29 1.533(3) . ?
C7 H17 1.0000 . ?
C7I C8I 1.501(4) . ?
C7I H7I1 0.9800 . ?
C7I H7I2 0.9800 . ?
C7I H7I3 0.9800 . ?
C7P C8P 1.391(4) . ?
C7P H7P 0.9500 . ?
O8 C18 1.370(3) . ?
O8 H8 0.8400 . ?
C8 C9 1.393(3) . ?
C8 C13 1.396(3) . ?
C8 H18 0.9500 . ?
C8I C9I 1.496(5) . ?
C8I H8I 1.0000 . ?
C8P C9P 1.375(4) . ?
C8P H8P 0.9500 . ?
O9 C19 1.385(3) . ?
O9 H9 0.8400 . ?
C9 C10 1.387(3) . ?
C9I H9I1 0.9800 . ?
C9I H9I2 0.9800 . ?
C9I H9I3 0.9800 . ?
C9P C10P 1.404(3) . ?
C9P H9P 0.9500 . ?
O10 C24 1.368(3) . ?
O10 H10 0.8400 . ?
C10 C11 1.387(3) . ?
O11 C25 1.363(3) . ?
O11 H11 0.8400 . ?
C11 C12 1.393(3) . ?
C11P C12P 1.382(4) . ?
O12 C26 1.373(3) . ?
O12 H12 0.8400 . ?
C12 C13 1.383(3) . ?
C12P C13P 1.380(4) . ?
C12P H12P 0.9500 . ?
C13 C14 1.524(3) . ?
C13P C14P 1.378(4) . ?
C13P H13P 0.9500 . ?
C14 C30 1.518(3) . ?
C14 C16 1.523(3) . ?
C14 H14 1.0000 . ?
C14P C15P 1.364(4) . ?
C14P H14P 0.9500 . ?
C15 C20 1.385(3) . ?
C15 C16 1.391(3) . ?
C15 H15 0.9500 . ?
C15P H15P 0.9500 . ?
C16 C17 1.390(3) . ?
C16P C25P 1.440(3) . ?
C16P C17P 1.467(3) . ?
C17 C18 1.380(4) . ?
C17P C18P 1.465(3) . ?
C18 C19 1.385(3) . ?
C18P C19P 1.399(3) . ?
C18P C23P 1.404(3) . ?
C19 C20 1.389(3) . ?
C19P C20P 1.377(3) . ?
C19P H19P 0.9500 . ?
C20 C21 1.522(3) . ?
C20P C21P 1.387(4) . ?
C20P H20P 0.9500 . ?
C21 C23 1.521(3) . ?
C21 C31 1.524(3) . ?
C21 H21 1.0000 . ?
C21P C22P 1.371(4) . ?
C21P H21P 0.9500 . ?
C22 C27 1.390(3) . ?
C22 C23 1.396(3) . ?
C22 H22 0.9500 . ?
C22P C23P 1.399(3) . ?
C22P H22P 0.9500 . ?
C23 C24 1.393(3) . ?
C23P C24P 1.436(3) . ?
C24 C25 1.394(3) . ?
C24P C25P 1.344(4) . ?
C24P H24P 0.9500 . ?
C25 C26 1.378(3) . ?
C25P H25P 0.9500 . ?
C26 C27 1.395(3) . ?
C26P C27P 1.389(3) . ?
C27 C28 1.512(3) . ?
C27P C28P 1.373(3) . ?
C27P H27P 0.9500 . ?
C28 C32 1.532(3) . ?
C28 H28 1.0000 . ?
C28P C29P 1.386(3) . ?
C28P H28P 0.9500 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C29P C30P 1.372(3) . ?
C29P H29P 0.9500 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C30P H30P 0.9500 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?

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
C3 O1 H1 109.5 . . ?
C6 C1 C2 123.1(2) . . ?
C6 C1 H13 118.5 . . ?
C2 C1 H13 118.5 . . ?
C2I O1I H1I 109.4 . . ?
C2I C1I H1I1 109.5 . . ?
C2I C1I H1I2 109.5 . . ?
H1I1 C1I H1I2 109.5 . . ?
C2I C1I H1I3 109.5 . . ?
H1I1 C1I H1I3 109.5 . . ?
H1I2 C1I H1I3 109.5 . . ?
C11P N1P C15P 117.5(2) . . ?
N3P C1P C10P 116.8(2) . . ?
N3P C1P C2P 123.4(2) . . ?
C10P C1P C2P 119.9(2) . . ?
C4 O2 H2 109.2 . . ?
C1 C2 C3 117.4(2) . . ?
C1 C2 C28 122.4(2) . . ?
C3 C2 C28 119.9(2) . . ?
C5I O2I H2I 109.5 . . ?
O1I C2I C1I 108.2(3) . . ?
O1I C2I C3I 109.2(3) . . ?
C1I C2I C3I 110.8(3) . . ?
O1I C2I H16 109.5 . . ?
C1I C2I H16 109.5 . . ?
C3I C2I H16 109.5 . . ?
N3P N2P C11P 119.7(2) . . ?
N3P N2P H2P1 120.1 . . ?
C11P N2P H2P1 120.1 . . ?
O1P C2P C3P 121.6(2) . . ?
O1P C2P C1P 121.0(2) . . ?
C3P C2P C1P 117.5(2) . . ?
C5 O3 H3 109.5 . . ?
O1 C3 C4 120.9(2) . . ?
O1 C3 C2 118.8(2) . . ?
C4 C3 C2 120.3(2) . . ?
C8I O3I H3I 109.5 . . ?
C2I C3I H3I1 109.5 . . ?
C2I C3I H3I2 109.5 . . ?
H3I1 C3I H3I2 109.5 . . ?
C2I C3I H3I3 109.5 . . ?
H3I1 C3I H3I3 109.5 . . ?
H3I2 C3I H3I3 109.5 . . ?
N2P N3P C1P 120.3(2) . . ?
C4P C3P C2P 121.3(2) . . ?
C4P C3P H3P 119.4 . . ?
C2P C3P H3P 119.4 . . ?
C10 O4 H4 109.5 . . ?
C5 C4 C3 121.0(2) . . ?
C5 C4 O2 120.1(2) . . ?
C3 C4 O2 118.8(2) . . ?
C5I C4I H4I1 109.5 . . ?
C5I C4I H4I2 109.5 . . ?
H4I1 C4I H4I2 109.5 . . ?
C5I C4I H4I3 109.5 . . ?
H4I1 C4I H4I3 109.5 . . ?
H4I2 C4I H4I3 109.5 . . ?
C26P N4P C30P 117.48(19) . . ?
C3P C4P C5P 123.2(2) . . ?
C3P C4P H4P 118.4 . . ?
C5P C4P H4P 118.4 . . ?
C11 O5 H5 109.5 . . ?
O3 C5 C4 120.8(2) . . ?
O3 C5 C6 118.9(2) . . ?
C4 C5 C6 120.4(2) . . ?
O2I C5I C6I 106.6(3) . . ?
O2I C5I C4I 109.5(3) . . ?
C6I C5I C4I 113.1(3) . . ?
O2I C5I H5I 109.2 . . ?
C6I C5I H5I 109.2 . . ?
C4I C5I H5I 109.2 . . ?
N6P N5P C26P 118.84(18) . . ?
N6P N5P H5P 120.6 . . ?
C26P N5P H5P 120.6 . . ?
C10P C5P C6P 120.1(2) . . ?
C10P C5P C4P 118.9(2) . . ?
C6P C5P C4P 121.1(2) . . ?
C12 O6 H6 109.5 . . ?
C1 C6 C5 117.8(2) . . ?
C1 C6 C7 121.6(2) . . ?
C5 C6 C7 120.2(2) . . ?
C5I C6I H6I1 109.5 . . ?
C5I C6I H6I2 109.5 . . ?
H6I1 C6I H6I2 109.5 . . ?
C5I C6I H6I3 109.5 . . ?
H6I1 C6I H6I3 109.5 . . ?
H6I2 C6I H6I3 109.5 . . ?
C17P N6P N5P 120.66(19) . . ?
C7P C6P C5P 120.4(3) . . ?
C7P C6P H6P 119.8 . . ?
C5P C6P H6P 119.8 . . ?
C17 O7 H7 109.5 . . ?
C9 C7 C6 114.72(19) . . ?
C9 C7 C29 113.0(2) . . ?
C6 C7 C29 107.86(19) . . ?
C9 C7 H17 106.9 . . ?
C6 C7 H17 106.9 . . ?
C29 C7 H17 106.9 . . ?
C8I C7I H7I1 109.5 . . ?
C8I C7I H7I2 109.5 . . ?
H7I1 C7I H7I2 109.5 . . ?
C8I C7I H7I3 109.5 . . ?
H7I1 C7I H7I3 109.5 . . ?
H7I2 C7I H7I3 109.5 . . ?
C6P C7P C8P 119.8(3) . . ?
C6P C7P H7P 120.1 . . ?
C8P C7P H7P 120.1 . . ?
C18 O8 H8 109.5 . . ?
C9 C8 C13 123.0(2) . . ?
C9 C8 H18 118.5 . . ?
C13 C8 H18 118.5 . . ?
O3I C8I C9I 107.8(2) . . ?
O3I C8I C7I 109.4(3) . . ?
C9I C8I C7I 113.0(3) . . ?
O3I C8I H8I 108.9 . . ?
C9I C8I H8I 108.9 . . ?
C7I C8I H8I 108.9 . . ?
C9P C8P C7P 120.8(3) . . ?
C9P C8P H8P 119.6 . . ?
C7P C8P H8P 119.6 . . ?
C19 O9 H9 109.5 . . ?
C10 C9 C8 117.3(2) . . ?
C10 C9 C7 120.2(2) . . ?
C8 C9 C7 122.4(2) . . ?
C8I C9I H9I1 109.5 . . ?
C8I C9I H9I2 109.5 . . ?
H9I1 C9I H9I2 109.5 . . ?
C8I C9I H9I3 109.5 . . ?
H9I1 C9I H9I3 109.5 . . ?
H9I2 C9I H9I3 109.5 . . ?
C8P C9P C10P 120.3(3) . . ?
C8P C9P H9P 119.9 . . ?
C10P C9P H9P 119.9 . . ?
C24 O10 H10 109.5 . . ?
O4 C10 C11 118.4(2) . . ?
O4 C10 C9 120.4(2) . . ?
C11 C10 C9 121.2(2) . . ?
C5P C10P C9P 118.7(2) . . ?
C5P C10P C1P 119.3(2) . . ?
C9P C10P C1P 122.0(2) . . ?
C25 O11 H11 109.5 . . ?
O5 C11 C10 117.3(2) . . ?
O5 C11 C12 122.8(2) . . ?
C10 C11 C12 119.9(2) . . ?
N1P C11P C12P 124.2(2) . . ?
N1P C11P N2P 113.6(2) . . ?
C12P C11P N2P 122.1(2) . . ?
C26 O12 H12 109.5 . . ?
O6 C12 C13 125.1(2) . . ?
O6 C12 C11 114.30(19) . . ?
C13 C12 C11 120.6(2) . . ?
C13P C12P C11P 116.9(3) . . ?
C13P C12P H12P 121.5 . . ?
C11P C12P H12P 121.5 . . ?
C12 C13 C8 117.9(2) . . ?
C12 C13 C14 119.63(19) . . ?
C8 C13 C14 122.4(2) . . ?
C14P C13P C12P 119.8(2) . . ?
C14P C13P H13P 120.1 . . ?
C12P C13P H13P 120.1 . . ?
C30 C14 C16 112.16(19) . . ?
C30 C14 C13 114.28(19) . . ?
C16 C14 C13 108.38(19) . . ?
C30 C14 H14 107.2 . . ?
C16 C14 H14 107.2 . . ?
C13 C14 H14 107.2 . . ?
C15P C14P C13P 119.1(2) . . ?
C15P C14P H14P 120.5 . . ?
C13P C14P H14P 120.5 . . ?
C20 C15 C16 123.1(2) . . ?
C20 C15 H15 118.5 . . ?
C16 C15 H15 118.5 . . ?
N1P C15P C14P 122.4(3) . . ?
N1P C15P H15P 118.8 . . ?
C14P C15P H15P 118.8 . . ?
C17 C16 C15 117.4(2) . . ?
C17 C16 C14 121.9(2) . . ?
C15 C16 C14 120.5(2) . . ?
O2P C16P C25P 121.7(2) . . ?
O2P C16P C17P 120.8(2) . . ?
C25P C16P C17P 117.5(2) . . ?
C18 C17 O7 116.6(2) . . ?
C18 C17 C16 121.0(2) . . ?
O7 C17 C16 122.3(2) . . ?
N6P C17P C18P 115.8(2) . . ?
N6P C17P C16P 124.1(2) . . ?
C18P C17P C16P 120.1(2) . . ?
O8 C18 C17 121.7(2) . . ?
O8 C18 C19 118.1(2) . . ?
C17 C18 C19 120.2(2) . . ?
C19P C18P C23P 119.7(2) . . ?
C19P C18P C17P 121.6(2) . . ?
C23P C18P C17P 118.7(2) . . ?
C18 C19 O9 117.6(2) . . ?
C18 C19 C20 120.6(2) . . ?
O9 C19 C20 121.7(2) . . ?
C20P C19P C18P 120.0(2) . . ?
C20P C19P H19P 120.0 . . ?
C18P C19P H19P 120.0 . . ?
C15 C20 C19 117.8(2) . . ?
C15 C20 C21 120.8(2) . . ?
C19 C20 C21 121.3(2) . . ?
C19P C20P C21P 120.4(2) . . ?
C19P C20P H20P 119.8 . . ?
C21P C20P H20P 119.8 . . ?
C20 C21 C23 111.16(18) . . ?
C20 C21 C31 111.8(2) . . ?
C23 C21 C31 114.02(19) . . ?
C20 C21 H21 106.4 . . ?
C23 C21 H21 106.4 . . ?
C31 C21 H21 106.4 . . ?
C22P C21P C20P 120.3(2) . . ?
C22P C21P H21P 119.9 . . ?
C20P C21P H21P 119.9 . . ?
C27 C22 C23 123.5(2) . . ?
C27 C22 H22 118.3 . . ?
C23 C22 H22 118.3 . . ?
C21P C22P C23P 120.6(2) . . ?
C21P C22P H22P 119.7 . . ?
C23P C22P H22P 119.7 . . ?
C24 C23 C22 117.5(2) . . ?
C24 C23 C21 120.0(2) . . ?
C22 C23 C21 122.5(2) . . ?
C22P C23P C18P 119.0(2) . . ?
C22P C23P C24P 121.5(2) . . ?
C18P C23P C24P 119.5(2) . . ?
O10 C24 C25 115.0(2) . . ?
O10 C24 C23 124.7(2) . . ?
C25 C24 C23 120.2(2) . . ?
C25P C24P C23P 123.3(2) . . ?
C25P C24P H24P 118.3 . . ?
C23P C24P H24P 118.3 . . ?
O11 C25 C26 116.7(2) . . ?
O11 C25 C24 122.7(2) . . ?
C26 C25 C24 120.6(2) . . ?
C24P C25P C16P 121.0(2) . . ?
C24P C25P H25P 119.5 . . ?
C16P C25P H25P 119.5 . . ?
O12 C26 C25 119.3(2) . . ?
O12 C26 C27 119.7(2) . . ?
C25 C26 C27 121.0(2) . . ?
N4P C26P C27P 124.0(2) . . ?
N4P C26P N5P 113.83(19) . . ?
C27P C26P N5P 122.2(2) . . ?
C22 C27 C26 117.2(2) . . ?
C22 C27 C28 123.4(2) . . ?
C26 C27 C28 119.5(2) . . ?
C28P C27P C26P 117.4(2) . . ?
C28P C27P H27P 121.3 . . ?
C26P C27P H27P 121.3 . . ?
C27 C28 C2 114.09(18) . . ?
C27 C28 C32 112.8(2) . . ?
C2 C28 C32 108.87(19) . . ?
C27 C28 H28 106.9 . . ?
C2 C28 H28 106.9 . . ?
C32 C28 H28 106.9 . . ?
C27P C28P C29P 119.6(2) . . ?
C27P C28P H28P 120.2 . . ?
C29P C28P H28P 120.2 . . ?
C7 C29 H29A 109.5 . . ?
C7 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C7 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C30P C29P C28P 118.8(2) . . ?
C30P C29P H29P 120.6 . . ?
C28P C29P H29P 120.6 . . ?
C14 C30 H30A 109.5 . . ?
C14 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C14 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N4P C30P C29P 122.8(2) . . ?
N4P C30P H30P 118.6 . . ?
C29P C30P H30P 118.6 . . ?
C21 C31 H31A 109.5 . . ?
C21 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C21 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C28 C32 H32A 109.5 . . ?
C28 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C28 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?

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
C6 C1 C2 C3 0.1(3) . . . . ?
C6 C1 C2 C28 -173.9(2) . . . . ?
N3P C1P C2P O1P -0.8(4) . . . . ?
C10P C1P C2P O1P 177.8(2) . . . . ?
N3P C1P C2P C3P -179.2(2) . . . . ?
C10P C1P C2P C3P -0.6(3) . . . . ?
C1 C2 C3 O1 -178.10(19) . . . . ?
C28 C2 C3 O1 -4.0(3) . . . . ?
C1 C2 C3 C4 1.7(3) . . . . ?
C28 C2 C3 C4 175.8(2) . . . . ?
C11P N2P N3P C1P -179.5(2) . . . . ?
C10P C1P N3P N2P -178.3(2) . . . . ?
C2P C1P N3P N2P 0.3(4) . . . . ?
O1P C2P C3P C4P -177.7(2) . . . . ?
C1P C2P C3P C4P 0.7(4) . . . . ?
O1 C3 C4 C5 177.0(2) . . . . ?
C2 C3 C4 C5 -2.7(3) . . . . ?
O1 C3 C4 O2 0.6(3) . . . . ?
C2 C3 C4 O2 -179.17(19) . . . . ?
C2P C3P C4P C5P 0.3(4) . . . . ?
C3 C4 C5 O3 -177.7(2) . . . . ?
O2 C4 C5 O3 -1.3(3) . . . . ?
C3 C4 C5 C6 1.9(3) . . . . ?
O2 C4 C5 C6 178.3(2) . . . . ?
C3P C4P C5P C10P -1.5(4) . . . . ?
C3P C4P C5P C6P 178.6(2) . . . . ?
C2 C1 C6 C5 -0.9(3) . . . . ?
C2 C1 C6 C7 172.1(2) . . . . ?
O3 C5 C6 C1 179.48(19) . . . . ?
C4 C5 C6 C1 -0.2(3) . . . . ?
O3 C5 C6 C7 6.4(3) . . . . ?
C4 C5 C6 C7 -173.2(2) . . . . ?
C26P N5P N6P C17P 178.8(2) . . . . ?
C10P C5P C6P C7P -1.5(4) . . . . ?
C4P C5P C6P C7P 178.5(3) . . . . ?
C1 C6 C7 C9 45.3(3) . . . . ?
C5 C6 C7 C9 -142.0(2) . . . . ?
C1 C6 C7 C29 -81.6(3) . . . . ?
C5 C6 C7 C29 91.1(3) . . . . ?
C5P C6P C7P C8P 1.2(4) . . . . ?
C6P C7P C8P C9P -0.3(5) . . . . ?
C13 C8 C9 C10 1.0(3) . . . . ?
C13 C8 C9 C7 -176.4(2) . . . . ?
C6 C7 C9 C10 73.5(3) . . . . ?
C29 C7 C9 C10 -162.3(2) . . . . ?
C6 C7 C9 C8 -109.3(3) . . . . ?
C29 C7 C9 C8 14.9(3) . . . . ?
C7P C8P C9P C10P -0.3(4) . . . . ?
C8 C9 C10 O4 178.7(2) . . . . ?
C7 C9 C10 O4 -3.9(3) . . . . ?
C8 C9 C10 C11 -1.7(3) . . . . ?
C7 C9 C10 C11 175.7(2) . . . . ?
C6P C5P C10P C9P 0.9(4) . . . . ?
C4P C5P C10P C9P -179.1(2) . . . . ?
C6P C5P C10P C1P -178.5(2) . . . . ?
C4P C5P C10P C1P 1.6(4) . . . . ?
C8P C9P C10P C5P 0.0(4) . . . . ?
C8P C9P C10P C1P 179.3(3) . . . . ?
N3P C1P C10P C5P 178.1(2) . . . . ?
C2P C1P C10P C5P -0.6(3) . . . . ?
N3P C1P C10P C9P -1.2(4) . . . . ?
C2P C1P C10P C9P -179.9(2) . . . . ?
O4 C10 C11 O5 -0.7(3) . . . . ?
C9 C10 C11 O5 179.7(2) . . . . ?
O4 C10 C11 C12 -179.9(2) . . . . ?
C9 C10 C11 C12 0.5(4) . . . . ?
C15P N1P C11P C12P 0.6(4) . . . . ?
C15P N1P C11P N2P -178.1(2) . . . . ?
N3P N2P C11P N1P -173.0(2) . . . . ?
N3P N2P C11P C12P 8.3(4) . . . . ?
O5 C11 C12 O6 1.9(3) . . . . ?
C10 C11 C12 O6 -178.9(2) . . . . ?
O5 C11 C12 C13 -177.6(2) . . . . ?
C10 C11 C12 C13 1.5(4) . . . . ?
N1P C11P C12P C13P -1.3(4) . . . . ?
N2P C11P C12P C13P 177.3(2) . . . . ?
O6 C12 C13 C8 178.3(2) . . . . ?
C11 C12 C13 C8 -2.2(3) . . . . ?
O6 C12 C13 C14 -4.2(4) . . . . ?
C11 C12 C13 C14 175.3(2) . . . . ?
C9 C8 C13 C12 1.0(3) . . . . ?
C9 C8 C13 C14 -176.5(2) . . . . ?
C11P C12P C13P C14P 0.8(4) . . . . ?
C12 C13 C14 C30 163.2(2) . . . . ?
C8 C13 C14 C30 -19.4(3) . . . . ?
C12 C13 C14 C16 -70.9(3) . . . . ?
C8 C13 C14 C16 106.5(2) . . . . ?
C12P C13P C14P C15P 0.3(4) . . . . ?
C11P N1P C15P C14P 0.7(4) . . . . ?
C13P C14P C15P N1P -1.1(4) . . . . ?
C20 C15 C16 C17 0.0(3) . . . . ?
C20 C15 C16 C14 175.4(2) . . . . ?
C30 C14 C16 C17 -127.9(2) . . . . ?
C13 C14 C16 C17 105.0(2) . . . . ?
C30 C14 C16 C15 56.9(3) . . . . ?
C13 C14 C16 C15 -70.2(3) . . . . ?
C15 C16 C17 C18 0.5(3) . . . . ?
C14 C16 C17 C18 -174.9(2) . . . . ?
C15 C16 C17 O7 175.7(2) . . . . ?
C14 C16 C17 O7 0.3(3) . . . . ?
N5P N6P C17P C18P -179.0(2) . . . . ?
N5P N6P C17P C16P 0.6(4) . . . . ?
O2P C16P C17P N6P 1.7(4) . . . . ?
C25P C16P C17P N6P -177.7(2) . . . . ?
O2P C16P C17P C18P -178.7(2) . . . . ?
C25P C16P C17P C18P 1.9(3) . . . . ?
O7 C17 C18 O8 3.0(3) . . . . ?
C16 C17 C18 O8 178.5(2) . . . . ?
O7 C17 C18 C19 -177.0(2) . . . . ?
C16 C17 C18 C19 -1.5(4) . . . . ?
N6P C17P C18P C19P -0.8(3) . . . . ?
C16P C17P C18P C19P 179.5(2) . . . . ?
N6P C17P C18P C23P 178.1(2) . . . . ?
C16P C17P C18P C23P -1.6(3) . . . . ?
O8 C18 C19 O9 -1.6(3) . . . . ?
C17 C18 C19 O9 178.4(2) . . . . ?
O8 C18 C19 C20 -178.0(2) . . . . ?
C17 C18 C19 C20 2.0(4) . . . . ?
C23P C18P C19P C20P -0.9(4) . . . . ?
C17P C18P C19P C20P 178.0(2) . . . . ?
C16 C15 C20 C19 0.6(3) . . . . ?
C16 C15 C20 C21 -176.0(2) . . . . ?
C18 C19 C20 C15 -1.5(3) . . . . ?
O9 C19 C20 C15 -177.8(2) . . . . ?
C18 C19 C20 C21 175.1(2) . . . . ?
O9 C19 C20 C21 -1.2(3) . . . . ?
C18P C19P C20P C21P -0.4(4) . . . . ?
C15 C20 C21 C23 73.0(3) . . . . ?
C19 C20 C21 C23 -103.5(2) . . . . ?
C15 C20 C21 C31 -55.6(3) . . . . ?
C19 C20 C21 C31 127.9(2) . . . . ?
C19P C20P C21P C22P 1.7(4) . . . . ?
C20P C21P C22P C23P -1.5(4) . . . . ?
C27 C22 C23 C24 -1.0(3) . . . . ?
C27 C22 C23 C21 -179.4(2) . . . . ?
C20 C21 C23 C24 74.2(3) . . . . ?
C31 C21 C23 C24 -158.4(2) . . . . ?
C20 C21 C23 C22 -107.4(2) . . . . ?
C31 C21 C23 C22 20.1(3) . . . . ?
C21P C22P C23P C18P 0.1(4) . . . . ?
C21P C22P C23P C24P -178.1(2) . . . . ?
C19P C18P C23P C22P 1.0(4) . . . . ?
C17P C18P C23P C22P -177.9(2) . . . . ?
C19P C18P C23P C24P 179.3(2) . . . . ?
C17P C18P C23P C24P 0.4(4) . . . . ?
C22 C23 C24 O10 -178.3(2) . . . . ?
C21 C23 C24 O10 0.2(3) . . . . ?
C22 C23 C24 C25 0.9(3) . . . . ?
C21 C23 C24 C25 179.3(2) . . . . ?
C22P C23P C24P C25P 178.7(3) . . . . ?
C18P C23P C24P C25P 0.5(4) . . . . ?
O10 C24 C25 O11 0.9(3) . . . . ?
C23 C24 C25 O11 -178.3(2) . . . . ?
O10 C24 C25 C26 -179.6(2) . . . . ?
C23 C24 C25 C26 1.2(4) . . . . ?
C23P C24P C25P C16P -0.1(4) . . . . ?
O2P C16P C25P C24P 179.5(2) . . . . ?
C17P C16P C25P C24P -1.1(4) . . . . ?
O11 C25 C26 O12 -3.1(3) . . . . ?
C24 C25 C26 O12 177.4(2) . . . . ?
O11 C25 C26 C27 176.3(2) . . . . ?
C24 C25 C26 C27 -3.3(4) . . . . ?
C30P N4P C26P C27P -0.2(4) . . . . ?
C30P N4P C26P N5P 179.7(2) . . . . ?
N6P N5P C26P N4P -178.3(2) . . . . ?
N6P N5P C26P C27P 1.6(3) . . . . ?
C23 C22 C27 C26 -0.9(3) . . . . ?
C23 C22 C27 C28 177.3(2) . . . . ?
O12 C26 C27 C22 -177.6(2) . . . . ?
C25 C26 C27 C22 3.0(3) . . . . ?
O12 C26 C27 C28 4.1(3) . . . . ?
C25 C26 C27 C28 -175.2(2) . . . . ?
N4P C26P C27P C28P 0.3(4) . . . . ?
N5P C26P C27P C28P -179.5(2) . . . . ?
C22 C27 C28 C2 99.5(3) . . . . ?
C26 C27 C28 C2 -82.3(3) . . . . ?
C22 C27 C28 C32 -25.4(3) . . . . ?
C26 C27 C28 C32 152.8(2) . . . . ?
C1 C2 C28 C27 -41.7(3) . . . . ?
C3 C2 C28 C27 144.5(2) . . . . ?
C1 C2 C28 C32 85.2(3) . . . . ?
C3 C2 C28 C32 -88.6(3) . . . . ?
C26P C27P C28P C29P -0.4(4) . . . . ?
C27P C28P C29P C30P 0.4(4) . . . . ?
C26P N4P C30P C29P 0.1(4) . . . . ?
C28P C29P C30P N4P -0.3(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.94
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.059

_database_code_depnum_ccdc_archive 'CCDC 1002496'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2cp55p

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            
'C-ethyl-pyrogallol[4]arene with 1-(2-pyridylazo)-2-napthol'
_chemical_formula_moiety         'C32 H32 O12, 2(C15 H11 O1 N3), 2(C2 H3 N1)'
_chemical_formula_sum            'C66 H60 N8 O14'
_chemical_melting_point          ?

_exptl_crystal_description       plate
_exptl_crystal_colour            orange

_diffrn_ambient_temperature      173(2)
_chemical_formula_weight         1189.22

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'
O O 0.0106 0.0060 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?

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

_cell_length_a                   7.3273(8)
_cell_length_b                   16.7326(19)
_cell_length_c                   23.611(3)
_cell_angle_alpha                85.742(2)
_cell_angle_beta                 83.946(2)
_cell_angle_gamma                86.963(2)
_cell_volume                     2867.7(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    5520
_cell_measurement_theta_min      2.2
_cell_measurement_theta_max      27.0
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1248
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8658
_exptl_absorpt_correction_T_max  0.9990
_exptl_absorpt_process_details   
;
 Data were corrected for decay and absorption using the program SADABS 
 (Sheldrick, G. M. (2003). SADABS. Version 2.10. University of
 Göttingen, Germany).
;

_exptl_special_details           
; 
 ? 
;
_diffrn_radiation_probe          ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.0
_diffrn_reflns_number            33066
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_sigmaI/netI    0.0699
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.45
_diffrn_reflns_theta_max         27.27
_reflns_number_total             12730
_reflns_number_gt                7323
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2008)'
_computing_structure_solution    'SHELXS-1997 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-1997 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-SEED, Barbour, 2001'
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0505P)²+0.5612P] where P=(Fo²+2Fc²)/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         12730
_refine_ls_number_parameters     811
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1029
_refine_ls_R_factor_gt           0.0456
_refine_ls_wR_factor_ref         0.1225
_refine_ls_wR_factor_gt          0.0982
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_restrained_S_all      0.984
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.87148(19) 0.13930(8) 0.36240(6) 0.0257(3) Uani 1 1 d . . .
H1 H 0.9704 0.1260 0.3763 0.031 Uiso 1 1 calc R . .
O7 O 1.0219(2) 0.65521(9) 0.15140(6) 0.0292(4) Uani 1 1 d . . .
H7 H 1.1122 0.6571 0.1264 0.035 Uiso 1 1 calc R . .
O8 O 1.13092(19) 0.56065(9) 0.06557(6) 0.0300(4) Uani 1 1 d . . .
H8 H 1.1197 0.5509 0.0317 0.036 Uiso 1 1 calc R . .
O4 O 0.97932(19) 0.52639(9) 0.43811(6) 0.0269(3) Uani 1 1 d . . .
H4 H 1.0745 0.5511 0.4408 0.032 Uiso 1 1 calc R . .
O3 O 0.9505(2) 0.36307(9) 0.46767(6) 0.0283(4) Uani 1 1 d . . .
H3 H 0.9624 0.4125 0.4600 0.034 Uiso 1 1 calc R . .
O2 O 1.03835(19) 0.20894(8) 0.44056(6) 0.0279(3) Uani 1 1 d . . .
H2 H 1.0985 0.2387 0.4581 0.034 Uiso 1 1 calc R . .
O5 O 1.16533(19) 0.63204(9) 0.36406(6) 0.0291(4) Uani 1 1 d . . .
H5 H 1.2252 0.6530 0.3349 0.035 Uiso 1 1 calc R . .
O10 O 0.8846(2) 0.27662(9) 0.07615(6) 0.0328(4) Uani 1 1 d . . .
H10 H 0.9519 0.2367 0.0664 0.039 Uiso 1 1 calc R . .
O6 O 1.04330(19) 0.68411(9) 0.26379(6) 0.0277(3) Uani 1 1 d . . .
H6 H 1.0364 0.6769 0.2293 0.033 Uiso 1 1 calc R . .
O9 O 0.9368(2) 0.43195(9) 0.04608(6) 0.0290(4) Uani 1 1 d . . .
H9 H 0.9210 0.3831 0.0551 0.035 Uiso 1 1 calc R . .
O13 O 0.2045(2) 0.06484(9) 0.39233(7) 0.0350(4) Uani 1 1 d . . .
O12 O 0.8819(2) 0.11755(9) 0.25010(6) 0.0342(4) Uani 1 1 d . . .
H12 H 0.8782 0.1250 0.2850 0.041 Uiso 1 1 calc R . .
O11 O 1.0215(2) 0.15390(9) 0.14020(7) 0.0374(4) Uani 1 1 d . . .
H11 H 1.0258 0.1082 0.1575 0.045 Uiso 1 1 calc R . .
N2 N 0.4134(2) 0.12696(10) 0.45661(7) 0.0250(4) Uani 1 1 d . . .
H13 H 0.3059 0.1281 0.4430 0.030 Uiso 1 1 calc R . .
N3 N 0.3163(2) 0.24117(11) 0.50083(8) 0.0276(4) Uani 1 1 d . . .
N1 N 0.5374(2) 0.06971(10) 0.44395(7) 0.0234(4) Uani 1 1 d . . .
C6 C 0.6712(3) 0.25555(12) 0.34941(8) 0.0202(4) Uani 1 1 d . . .
C26 C 0.5992(3) 0.29795(12) 0.21123(8) 0.0207(4) Uani 1 1 d . . .
H26 H 0.5033 0.3324 0.2273 0.025 Uiso 1 1 calc R . .
C9 C 1.0024(3) 0.60524(12) 0.34916(9) 0.0212(5) Uani 1 1 d . . .
C13 C 0.7450(3) 0.52077(12) 0.37480(8) 0.0194(4) Uani 1 1 d . . .
C17 C 0.8715(3) 0.47675(12) 0.09185(8) 0.0228(5) Uani 1 1 d . . .
C11 C 0.7713(3) 0.60261(12) 0.28366(8) 0.0191(4) Uani 1 1 d . . .
C19 C 0.6580(3) 0.51149(12) 0.17056(8) 0.0213(5) Uani 1 1 d . . .
H19 H 0.5490 0.5012 0.1950 0.026 Uiso 1 1 calc R . .
C42 C 0.3360(3) 0.01595(13) 0.38048(9) 0.0263(5) Uani 1 1 d . . .
C16 C 0.9731(3) 0.54189(13) 0.09959(9) 0.0237(5) Uani 1 1 d . . .
C18 C 0.7102(3) 0.46038(12) 0.12698(8) 0.0210(5) Uani 1 1 d . . .
C28 C 0.5742(3) 0.21388(13) 0.30629(9) 0.0226(5) Uani 1 1 d . . .
H28 H 0.5938 0.1548 0.3150 0.027 Uiso 1 1 calc R . .
C3 C 0.8549(3) 0.33256(13) 0.42700(8) 0.0221(5) Uani 1 1 d . . .
C14 C 0.6973(3) 0.63260(12) 0.22754(9) 0.0226(5) Uani 1 1 d . . .
H14 H 0.7539 0.6851 0.2157 0.027 Uiso 1 1 calc R . .
C12 C 0.6803(3) 0.54740(12) 0.32294(8) 0.0198(4) Uani 1 1 d . . .
H17 H 0.5692 0.5272 0.3138 0.024 Uiso 1 1 calc R . .
C1 C 0.8173(3) 0.21682(12) 0.37524(9) 0.0213(5) Uani 1 1 d . . .
C24 C 0.8076(3) 0.18438(12) 0.22177(9) 0.0241(5) Uani 1 1 d . . .
C20 C 0.7583(3) 0.57696(12) 0.18002(8) 0.0207(4) Uani 1 1 d . . .
C7 C 0.6479(3) 0.45862(12) 0.41679(9) 0.0206(4) Uani 1 1 d . . .
H18 H 0.6890 0.4658 0.4551 0.025 Uiso 1 1 calc R . .
C22 C 0.8118(3) 0.26349(12) 0.13273(9) 0.0239(5) Uani 1 1 d . . .
C8 C 0.9087(3) 0.55122(12) 0.38722(8) 0.0205(4) Uani 1 1 d . . .
C23 C 0.8815(3) 0.19959(13) 0.16571(9) 0.0254(5) Uani 1 1 d . . .
C2 C 0.9062(3) 0.25415(12) 0.41448(9) 0.0216(5) Uani 1 1 d . . .
C5 C 0.6212(3) 0.33337(12) 0.36371(8) 0.0205(4) Uani 1 1 d . . .
H20 H 0.5221 0.3607 0.3464 0.025 Uiso 1 1 calc R . .
C27 C 0.6707(3) 0.31509(12) 0.15476(9) 0.0223(5) Uani 1 1 d . . .
C33 C 0.5042(3) 0.01592(13) 0.40844(9) 0.0241(5) Uani 1 1 d . . .
C10 C 0.9363(3) 0.63024(12) 0.29772(8) 0.0200(4) Uani 1 1 d . . .
C25 C 0.6620(3) 0.23249(12) 0.24531(9) 0.0205(4) Uani 1 1 d . . .
C21 C 0.6015(3) 0.38760(12) 0.11880(9) 0.0227(5) Uani 1 1 d . . .
H21 H 0.6291 0.3751 0.0779 0.027 Uiso 1 1 calc R . .
C4 C 0.7089(3) 0.37341(12) 0.40203(8) 0.0201(4) Uani 1 1 d . . .
C43 C 0.4531(3) 0.18601(12) 0.49181(9) 0.0230(5) Uani 1 1 d . . .
C40 C 0.4626(3) -0.09805(14) 0.32857(9) 0.0325(5) Uani 1 1 d . . .
H40 H 0.4489 -0.1363 0.3017 0.039 Uiso 1 1 calc R . .
C34 C 0.6519(3) -0.04515(12) 0.39609(9) 0.0244(5) Uani 1 1 d . . .
C41 C 0.3256(3) -0.04257(14) 0.33888(9) 0.0316(5) Uani 1 1 d . . .
H41 H 0.2203 -0.0418 0.3185 0.038 Uiso 1 1 calc R . .
C46 C 0.5016(3) 0.30280(13) 0.56146(10) 0.0317(5) Uani 1 1 d . . .
H46 H 0.5139 0.3436 0.5865 0.038 Uiso 1 1 calc R . .
C31 C 0.3931(3) 0.40324(13) 0.12929(9) 0.0287(5) Uani 1 1 d . . .
H31A H 0.3602 0.4162 0.1690 0.043 Uiso 1 1 calc R . .
H31B H 0.3308 0.3552 0.1220 0.043 Uiso 1 1 calc R . .
H31C H 0.3550 0.4483 0.1036 0.043 Uiso 1 1 calc R . .
C44 C 0.6199(3) 0.18622(13) 0.51466(9) 0.0260(5) Uani 1 1 d . . .
H44 H 0.7144 0.1464 0.5065 0.031 Uiso 1 1 calc R . .
C29 C 0.4381(3) 0.47146(13) 0.42286(9) 0.0257(5) Uani 1 1 d . . .
H29A H 0.3925 0.4691 0.3855 0.039 Uiso 1 1 calc R . .
H29B H 0.4042 0.5241 0.4375 0.039 Uiso 1 1 calc R . .
H29C H 0.3835 0.4294 0.4495 0.039 Uiso 1 1 calc R . .
C39 C 0.6293(3) -0.10206(13) 0.35644(9) 0.0278(5) Uani 1 1 d . . .
C15 C 0.9183(3) 0.59098(12) 0.14373(9) 0.0227(5) Uani 1 1 d . . .
C45 C 0.6430(3) 0.24636(13) 0.54970(9) 0.0300(5) Uani 1 1 d . . .
H45 H 0.7558 0.2491 0.5658 0.036 Uiso 1 1 calc R . .
C32 C 0.3652(3) 0.23198(13) 0.31234(9) 0.0276(5) Uani 1 1 d . . .
H32A H 0.3397 0.2894 0.3038 0.041 Uiso 1 1 calc R . .
H32B H 0.3144 0.2167 0.3515 0.041 Uiso 1 1 calc R . .
H32C H 0.3084 0.2013 0.2856 0.041 Uiso 1 1 calc R . .
C35 C 0.8137(3) -0.04964(13) 0.42318(10) 0.0288(5) Uani 1 1 d . . .
H35 H 0.8320 -0.0116 0.4497 0.035 Uiso 1 1 calc R . .
C30 C 0.4892(3) 0.64970(13) 0.23447(9) 0.0284(5) Uani 1 1 d . . .
H30A H 0.4279 0.6006 0.2490 0.043 Uiso 1 1 calc R . .
H30B H 0.4477 0.6682 0.1974 0.043 Uiso 1 1 calc R . .
H30C H 0.4587 0.6913 0.2615 0.043 Uiso 1 1 calc R . .
C65 C 0.4954(4) 0.68308(16) 0.05327(11) 0.0423(6) Uani 1 1 d . . .
C47 C 0.3427(3) 0.29798(14) 0.53573(10) 0.0310(5) Uani 1 1 d . . .
H47 H 0.2464 0.3372 0.5432 0.037 Uiso 1 1 calc R . .
C38 C 0.7669(3) -0.16143(14) 0.34500(10) 0.0340(6) Uani 1 1 d . . .
H38 H 0.7517 -0.1994 0.3181 0.041 Uiso 1 1 calc R . .
N8 N 0.3696(3) 0.69544(14) 0.08376(11) 0.0578(7) Uani 1 1 d . . .
C36 C 0.9467(3) -0.10959(14) 0.41121(10) 0.0351(6) Uani 1 1 d . . .
H36 H 1.0555 -0.1126 0.4300 0.042 Uiso 1 1 calc R . .
C37 C 0.9235(3) -0.16551(14) 0.37218(11) 0.0382(6) Uani 1 1 d . . .
H37 H 1.0159 -0.2064 0.3644 0.046 Uiso 1 1 calc R . .
C66 C 0.6585(4) 0.6653(2) 0.01501(12) 0.0651(9) Uani 1 1 d . . .
H66A H 0.7674 0.6647 0.0359 0.098 Uiso 1 1 calc R . .
H66B H 0.6688 0.7064 -0.0168 0.098 Uiso 1 1 calc R . .
H66C H 0.6493 0.6126 0.0001 0.098 Uiso 1 1 calc R . .
N6 N 0.0726(2) -0.00386(11) 0.16416(8) 0.0277(4) Uani 1 1 d . . .
N5 N 0.1655(2) 0.01506(11) 0.06853(8) 0.0288(4) Uani 1 1 d . . .
H5A H 0.1213 0.0649 0.0698 0.035 Uiso 1 1 calc R . .
N4 N 0.2403(2) -0.01179(11) 0.02017(8) 0.0294(4) Uani 1 1 d . . .
C58 C 0.1570(3) -0.03668(13) 0.11797(9) 0.0251(5) Uani 1 1 d . . .
O14 O 0.1084(2) 0.15208(10) 0.01226(7) 0.0441(4) Uani 1 1 d . . .
C59 C 0.2277(3) -0.11546(13) 0.11820(10) 0.0297(5) Uani 1 1 d . . .
H59 H 0.2871 -0.1367 0.0845 0.036 Uiso 1 1 calc R . .
C48 C 0.2498(3) 0.03523(14) -0.02735(9) 0.0297(5) Uani 1 1 d . . .
C57 C 0.1808(3) 0.11893(15) -0.03105(10) 0.0354(6) Uani 1 1 d . . .
C62 C 0.0536(3) -0.05039(14) 0.21295(10) 0.0319(5) Uani 1 1 d . . .
H62 H -0.0078 -0.0280 0.2460 0.038 Uiso 1 1 calc R . .
C60 C 0.2085(3) -0.16155(14) 0.16885(10) 0.0336(6) Uani 1 1 d . . .
H60 H 0.2562 -0.2155 0.1707 0.040 Uiso 1 1 calc R . .
C61 C 0.1192(3) -0.12918(14) 0.21744(10) 0.0355(6) Uani 1 1 d . . .
H61 H 0.1038 -0.1604 0.2527 0.043 Uiso 1 1 calc R . .
C49 C 0.3368(3) -0.00156(15) -0.07832(10) 0.0357(6) Uani 1 1 d . . .
C56 C 0.1991(3) 0.16167(17) -0.08684(11) 0.0435(7) Uani 1 1 d . . .
H56 H 0.1538 0.2158 -0.0910 0.052 Uiso 1 1 calc R . .
C51 C 0.4919(4) -0.11332(19) -0.12591(13) 0.0582(9) Uani 1 1 d . . .
H51 H 0.5409 -0.1671 -0.1244 0.070 Uiso 1 1 calc R . .
C55 C 0.2790(3) 0.12596(19) -0.13271(11) 0.0491(7) Uani 1 1 d . . .
H55 H 0.2885 0.1563 -0.1685 0.059 Uiso 1 1 calc R . .
C54 C 0.3507(3) 0.04467(18) -0.13078(11) 0.0429(7) Uani 1 1 d . . .
C53 C 0.4349(4) 0.0101(2) -0.17978(12) 0.0564(8) Uani 1 1 d . . .
H53 H 0.4429 0.0410 -0.2153 0.068 Uiso 1 1 calc R . .
C50 C 0.4075(3) -0.08151(17) -0.07685(12) 0.0457(7) Uani 1 1 d . . .
H50 H 0.3972 -0.1138 -0.0419 0.055 Uiso 1 1 calc R . .
C52 C 0.5053(4) -0.0669(2) -0.17760(13) 0.0643(10) Uani 1 1 d . . .
H52 H 0.5635 -0.0889 -0.2112 0.077 Uiso 1 1 calc R . .
C63 C 0.1361(3) 0.43068(14) 0.27015(10) 0.0301(5) Uani 1 1 d . . .
N7 N 0.2565(3) 0.46418(13) 0.28176(9) 0.0448(5) Uani 1 1 d . . .
C64 C -0.0154(3) 0.38696(16) 0.25444(11) 0.0428(6) Uani 1 1 d . . .
H64A H 0.0333 0.3397 0.2346 0.064 Uiso 1 1 calc R . .
H64B H -0.0878 0.4219 0.2292 0.064 Uiso 1 1 calc R . .
H64C H -0.0939 0.3698 0.2889 0.064 Uiso 1 1 calc R . .


_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 C1 1.382(2) . ?
O1 H1 0.8400 . ?
O7 C15 1.382(2) . ?
O7 H7 0.8400 . ?
O8 C16 1.373(2) . ?
O8 H8 0.8400 . ?
O4 C8 1.385(2) . ?
O4 H4 0.8400 . ?
O3 C3 1.388(2) . ?
O3 H3 0.8400 . ?
O2 C2 1.367(2) . ?
O2 H2 0.8400 . ?
O5 C9 1.385(2) . ?
O5 H5 0.8400 . ?
O10 C22 1.391(2) . ?
O10 H10 0.8400 . ?
O6 C10 1.380(2) . ?
O6 H6 0.8400 . ?
O9 C17 1.390(2) . ?
O9 H9 0.8400 . ?
O13 C42 1.253(2) . ?
O12 C24 1.377(2) . ?
O12 H12 0.8400 . ?
O11 C23 1.362(2) . ?
O11 H11 0.8400 . ?
N2 N1 1.313(2) . ?
N2 C43 1.398(3) . ?
N2 H13 0.8800 . ?
N3 C47 1.338(3) . ?
N3 C43 1.338(3) . ?
N1 C33 1.323(3) . ?
C6 C5 1.390(3) . ?
C6 C1 1.394(3) . ?
C6 C28 1.529(3) . ?
C26 C27 1.395(3) . ?
C26 C25 1.397(3) . ?
C26 H26 0.9500 . ?
C9 C8 1.382(3) . ?
C9 C10 1.382(3) . ?
C13 C12 1.393(3) . ?
C13 C8 1.395(3) . ?
C13 C7 1.532(3) . ?
C17 C16 1.386(3) . ?
C17 C18 1.398(3) . ?
C11 C10 1.397(3) . ?
C11 C12 1.402(3) . ?
C11 C14 1.525(3) . ?
C19 C20 1.395(3) . ?
C19 C18 1.396(3) . ?
C19 H19 0.9500 . ?
C42 C41 1.448(3) . ?
C42 C33 1.458(3) . ?
C16 C15 1.388(3) . ?
C18 C21 1.525(3) . ?
C28 C25 1.531(3) . ?
C28 C32 1.539(3) . ?
C28 H28 1.0000 . ?
C3 C2 1.390(3) . ?
C3 C4 1.398(3) . ?
C14 C20 1.527(3) . ?
C14 C30 1.530(3) . ?
C14 H14 1.0000 . ?
C12 H17 0.9500 . ?
C1 C2 1.389(3) . ?
C24 C23 1.387(3) . ?
C24 C25 1.395(3) . ?
C20 C15 1.397(3) . ?
C7 C4 1.526(3) . ?
C7 C29 1.534(3) . ?
C7 H18 1.0000 . ?
C22 C23 1.383(3) . ?
C22 C27 1.394(3) . ?
C5 C4 1.392(3) . ?
C5 H20 0.9500 . ?
C27 C21 1.524(3) . ?
C33 C34 1.470(3) . ?
C21 C31 1.533(3) . ?
C21 H21 1.0000 . ?
C43 C44 1.387(3) . ?
C40 C41 1.346(3) . ?
C40 C39 1.444(3) . ?
C40 H40 0.9500 . ?
C34 C35 1.401(3) . ?
C34 C39 1.412(3) . ?
C41 H41 0.9500 . ?
C46 C47 1.378(3) . ?
C46 C45 1.384(3) . ?
C46 H46 0.9500 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C44 C45 1.377(3) . ?
C44 H44 0.9500 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C39 C38 1.398(3) . ?
C45 H45 0.9500 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C35 C36 1.384(3) . ?
C35 H35 0.9500 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C65 N8 1.128(3) . ?
C65 C66 1.451(4) . ?
C47 H47 0.9500 . ?
C38 C37 1.369(3) . ?
C38 H38 0.9500 . ?
C36 C37 1.390(3) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
N6 C58 1.336(3) . ?
N6 C62 1.341(3) . ?
N5 N4 1.313(2) . ?
N5 C58 1.399(3) . ?
N5 H5A 0.8800 . ?
N4 C48 1.319(3) . ?
C58 C59 1.390(3) . ?
O14 C57 1.254(3) . ?
C59 C60 1.372(3) . ?
C59 H59 0.9500 . ?
C48 C49 1.463(3) . ?
C48 C57 1.463(3) . ?
C57 C56 1.448(3) . ?
C62 C61 1.379(3) . ?
C62 H62 0.9500 . ?
C60 C61 1.391(3) . ?
C60 H60 0.9500 . ?
C61 H61 0.9500 . ?
C49 C50 1.408(4) . ?
C49 C54 1.408(3) . ?
C56 C55 1.341(4) . ?
C56 H56 0.9500 . ?
C51 C50 1.383(4) . ?
C51 C52 1.395(4) . ?
C51 H51 0.9500 . ?
C55 C54 1.431(4) . ?
C55 H55 0.9500 . ?
C54 C53 1.402(4) . ?
C53 C52 1.360(4) . ?
C53 H53 0.9500 . ?
C50 H50 0.9500 . ?
C52 H52 0.9500 . ?
C63 N7 1.138(3) . ?
C63 C64 1.455(3) . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 O1 H1 109.5 . . ?
C15 O7 H7 109.5 . . ?
C16 O8 H8 109.5 . . ?
C8 O4 H4 109.5 . . ?
C3 O3 H3 109.5 . . ?
C2 O2 H2 109.5 . . ?
C9 O5 H5 109.5 . . ?
C22 O10 H10 109.5 . . ?
C10 O6 H6 109.5 . . ?
C17 O9 H9 109.5 . . ?
C24 O12 H12 109.5 . . ?
C23 O11 H11 109.5 . . ?
N1 N2 C43 119.65(17) . . ?
N1 N2 H13 120.2 . . ?
C43 N2 H13 120.2 . . ?
C47 N3 C43 116.78(18) . . ?
N2 N1 C33 119.95(17) . . ?
C5 C6 C1 117.22(18) . . ?
C5 C6 C28 122.07(18) . . ?
C1 C6 C28 120.69(18) . . ?
C27 C26 C25 123.08(19) . . ?
C27 C26 H26 118.5 . . ?
C25 C26 H26 118.5 . . ?
C8 C9 C10 120.78(18) . . ?
C8 C9 O5 117.62(18) . . ?
C10 C9 O5 121.59(18) . . ?
C12 C13 C8 117.28(18) . . ?
C12 C13 C7 122.97(17) . . ?
C8 C13 C7 119.72(18) . . ?
C16 C17 O9 115.64(18) . . ?
C16 C17 C18 121.10(19) . . ?
O9 C17 C18 123.21(18) . . ?
C10 C11 C12 117.24(18) . . ?
C10 C11 C14 120.01(17) . . ?
C12 C11 C14 122.75(18) . . ?
C20 C19 C18 123.16(19) . . ?
C20 C19 H19 118.4 . . ?
C18 C19 H19 118.4 . . ?
O13 C42 C41 121.15(19) . . ?
O13 C42 C33 120.99(19) . . ?
C41 C42 C33 117.87(19) . . ?
O8 C16 C17 122.92(19) . . ?
O8 C16 C15 116.95(18) . . ?
C17 C16 C15 120.12(19) . . ?
C19 C18 C17 117.24(18) . . ?
C19 C18 C21 122.08(18) . . ?
C17 C18 C21 120.64(18) . . ?
C6 C28 C25 111.20(16) . . ?
C6 C28 C32 112.49(17) . . ?
C25 C28 C32 112.41(17) . . ?
C6 C28 H28 106.8 . . ?
C25 C28 H28 106.8 . . ?
C32 C28 H28 106.8 . . ?
O3 C3 C2 115.08(17) . . ?
O3 C3 C4 124.37(18) . . ?
C2 C3 C4 120.43(18) . . ?
C11 C14 C20 111.87(16) . . ?
C11 C14 C30 112.33(17) . . ?
C20 C14 C30 112.56(17) . . ?
C11 C14 H14 106.5 . . ?
C20 C14 H14 106.5 . . ?
C30 C14 H14 106.5 . . ?
C13 C12 C11 123.20(18) . . ?
C13 C12 H17 118.4 . . ?
C11 C12 H17 118.4 . . ?
O1 C1 C2 119.63(17) . . ?
O1 C1 C6 119.23(18) . . ?
C2 C1 C6 121.13(18) . . ?
O12 C24 C23 115.28(18) . . ?
O12 C24 C25 123.94(18) . . ?
C23 C24 C25 120.70(19) . . ?
C19 C20 C15 117.49(19) . . ?
C19 C20 C14 122.23(18) . . ?
C15 C20 C14 120.28(18) . . ?
C4 C7 C13 111.15(16) . . ?
C4 C7 C29 112.08(16) . . ?
C13 C7 C29 113.10(17) . . ?
C4 C7 H18 106.7 . . ?
C13 C7 H18 106.7 . . ?
C29 C7 H18 106.7 . . ?
C23 C22 O10 119.13(18) . . ?
C23 C22 C27 121.68(19) . . ?
O10 C22 C27 119.20(18) . . ?
C9 C8 O4 119.58(18) . . ?
C9 C8 C13 120.87(18) . . ?
O4 C8 C13 119.55(18) . . ?
O11 C23 C22 116.79(18) . . ?
O11 C23 C24 123.26(19) . . ?
C22 C23 C24 119.94(19) . . ?
O2 C2 C1 116.54(18) . . ?
O2 C2 C3 123.30(18) . . ?
C1 C2 C3 120.12(18) . . ?
C6 C5 C4 123.42(19) . . ?
C6 C5 H20 118.3 . . ?
C4 C5 H20 118.3 . . ?
C22 C27 C26 116.89(19) . . ?
C22 C27 C21 121.12(18) . . ?
C26 C27 C21 121.97(18) . . ?
N1 C33 C42 124.11(19) . . ?
N1 C33 C34 116.13(18) . . ?
C42 C33 C34 119.73(19) . . ?
O6 C10 C9 114.76(17) . . ?
O6 C10 C11 124.62(18) . . ?
C9 C10 C11 120.61(18) . . ?
C24 C25 C26 117.64(18) . . ?
C24 C25 C28 120.99(18) . . ?
C26 C25 C28 121.37(18) . . ?
C27 C21 C18 109.77(16) . . ?
C27 C21 C31 112.82(17) . . ?
C18 C21 C31 113.24(17) . . ?
C27 C21 H21 106.9 . . ?
C18 C21 H21 106.9 . . ?
C31 C21 H21 106.9 . . ?
C5 C4 C3 117.63(19) . . ?
C5 C4 C7 121.51(17) . . ?
C3 C4 C7 120.86(18) . . ?
N3 C43 C44 124.10(19) . . ?
N3 C43 N2 113.65(18) . . ?
C44 C43 N2 122.25(19) . . ?
C41 C40 C39 123.0(2) . . ?
C41 C40 H40 118.5 . . ?
C39 C40 H40 118.5 . . ?
C35 C34 C39 118.8(2) . . ?
C35 C34 C33 122.11(19) . . ?
C39 C34 C33 119.12(19) . . ?
C40 C41 C42 121.1(2) . . ?
C40 C41 H41 119.4 . . ?
C42 C41 H41 119.4 . . ?
C47 C46 C45 118.0(2) . . ?
C47 C46 H46 121.0 . . ?
C45 C46 H46 121.0 . . ?
C21 C31 H31A 109.5 . . ?
C21 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C21 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C45 C44 C43 117.4(2) . . ?
C45 C44 H44 121.3 . . ?
C43 C44 H44 121.3 . . ?
C7 C29 H29A 109.5 . . ?
C7 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C7 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C38 C39 C34 119.9(2) . . ?
C38 C39 C40 121.1(2) . . ?
C34 C39 C40 119.1(2) . . ?
O7 C15 C16 119.58(18) . . ?
O7 C15 C20 119.55(18) . . ?
C16 C15 C20 120.86(19) . . ?
C44 C45 C46 119.9(2) . . ?
C44 C45 H45 120.0 . . ?
C46 C45 H45 120.0 . . ?
C28 C32 H32A 109.5 . . ?
C28 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C28 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C36 C35 C34 119.9(2) . . ?
C36 C35 H35 120.0 . . ?
C34 C35 H35 120.0 . . ?
C14 C30 H30A 109.5 . . ?
C14 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C14 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N8 C65 C66 178.5(3) . . ?
N3 C47 C46 123.7(2) . . ?
N3 C47 H47 118.1 . . ?
C46 C47 H47 118.1 . . ?
C37 C38 C39 120.7(2) . . ?
C37 C38 H38 119.6 . . ?
C39 C38 H38 119.6 . . ?
C35 C36 C37 121.1(2) . . ?
C35 C36 H36 119.5 . . ?
C37 C36 H36 119.5 . . ?
C38 C37 C36 119.7(2) . . ?
C38 C37 H37 120.2 . . ?
C36 C37 H37 120.2 . . ?
C65 C66 H66A 109.5 . . ?
C65 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C65 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C58 N6 C62 117.57(19) . . ?
N4 N5 C58 119.06(18) . . ?
N4 N5 H5A 120.5 . . ?
C58 N5 H5A 120.5 . . ?
N5 N4 C48 120.70(19) . . ?
N6 C58 C59 123.6(2) . . ?
N6 C58 N5 113.88(19) . . ?
C59 C58 N5 122.5(2) . . ?
C60 C59 C58 117.7(2) . . ?
C60 C59 H59 121.2 . . ?
C58 C59 H59 121.2 . . ?
N4 C48 C49 115.5(2) . . ?
N4 C48 C57 124.2(2) . . ?
C49 C48 C57 120.3(2) . . ?
O14 C57 C56 121.5(2) . . ?
O14 C57 C48 121.3(2) . . ?
C56 C57 C48 117.2(2) . . ?
N6 C62 C61 123.1(2) . . ?
N6 C62 H62 118.5 . . ?
C61 C62 H62 118.5 . . ?
C59 C60 C61 119.9(2) . . ?
C59 C60 H60 120.0 . . ?
C61 C60 H60 120.0 . . ?
C62 C61 C60 118.1(2) . . ?
C62 C61 H61 120.9 . . ?
C60 C61 H61 120.9 . . ?
C50 C49 C54 118.7(2) . . ?
C50 C49 C48 122.4(2) . . ?
C54 C49 C48 118.8(2) . . ?
C55 C56 C57 121.0(3) . . ?
C55 C56 H56 119.5 . . ?
C57 C56 H56 119.5 . . ?
C50 C51 C52 120.3(3) . . ?
C50 C51 H51 119.9 . . ?
C52 C51 H51 119.9 . . ?
C56 C55 C54 123.6(3) . . ?
C56 C55 H55 118.2 . . ?
C54 C55 H55 118.2 . . ?
C53 C54 C49 119.2(3) . . ?
C53 C54 C55 121.6(3) . . ?
C49 C54 C55 119.1(2) . . ?
C52 C53 C54 121.4(3) . . ?
C52 C53 H53 119.3 . . ?
C54 C53 H53 119.3 . . ?
C51 C50 C49 120.4(3) . . ?
C51 C50 H50 119.8 . . ?
C49 C50 H50 119.8 . . ?
C53 C52 C51 119.9(3) . . ?
C53 C52 H52 120.1 . . ?
C51 C52 H52 120.1 . . ?
N7 C63 C64 178.8(3) . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C43 N2 N1 C33 -176.69(18) . . . . ?
O9 C17 C16 O8 -1.6(3) . . . . ?
C18 C17 C16 O8 -179.13(19) . . . . ?
O9 C17 C16 C15 179.29(18) . . . . ?
C18 C17 C16 C15 1.7(3) . . . . ?
C20 C19 C18 C17 0.2(3) . . . . ?
C20 C19 C18 C21 177.96(18) . . . . ?
C16 C17 C18 C19 -1.0(3) . . . . ?
O9 C17 C18 C19 -178.39(18) . . . . ?
C16 C17 C18 C21 -178.81(18) . . . . ?
O9 C17 C18 C21 3.8(3) . . . . ?
C5 C6 C28 C25 87.3(2) . . . . ?
C1 C6 C28 C25 -91.3(2) . . . . ?
C5 C6 C28 C32 -39.8(3) . . . . ?
C1 C6 C28 C32 141.58(19) . . . . ?
C10 C11 C14 C20 93.4(2) . . . . ?
C12 C11 C14 C20 -86.6(2) . . . . ?
C10 C11 C14 C30 -138.84(19) . . . . ?
C12 C11 C14 C30 41.1(3) . . . . ?
C8 C13 C12 C11 -0.2(3) . . . . ?
C7 C13 C12 C11 -178.19(18) . . . . ?
C10 C11 C12 C13 1.2(3) . . . . ?
C14 C11 C12 C13 -178.75(18) . . . . ?
C5 C6 C1 O1 179.85(17) . . . . ?
C28 C6 C1 O1 -1.4(3) . . . . ?
C5 C6 C1 C2 1.3(3) . . . . ?
C28 C6 C1 C2 -179.98(18) . . . . ?
C18 C19 C20 C15 -0.1(3) . . . . ?
C18 C19 C20 C14 179.28(18) . . . . ?
C11 C14 C20 C19 88.2(2) . . . . ?
C30 C14 C20 C19 -39.4(3) . . . . ?
C11 C14 C20 C15 -92.4(2) . . . . ?
C30 C14 C20 C15 140.00(19) . . . . ?
C12 C13 C7 C4 85.8(2) . . . . ?
C8 C13 C7 C4 -92.1(2) . . . . ?
C12 C13 C7 C29 -41.3(3) . . . . ?
C8 C13 C7 C29 140.76(19) . . . . ?
C10 C9 C8 O4 179.15(18) . . . . ?
O5 C9 C8 O4 0.2(3) . . . . ?
C10 C9 C8 C13 -0.2(3) . . . . ?
O5 C9 C8 C13 -179.15(18) . . . . ?
C12 C13 C8 C9 -0.4(3) . . . . ?
C7 C13 C8 C9 177.73(18) . . . . ?
C12 C13 C8 O4 -179.71(17) . . . . ?
C7 C13 C8 O4 -1.6(3) . . . . ?
O10 C22 C23 O11 1.1(3) . . . . ?
C27 C22 C23 O11 -178.79(19) . . . . ?
O10 C22 C23 C24 -178.42(19) . . . . ?
C27 C22 C23 C24 1.7(3) . . . . ?
O12 C24 C23 O11 -2.0(3) . . . . ?
C25 C24 C23 O11 -178.89(19) . . . . ?
O12 C24 C23 C22 177.52(18) . . . . ?
C25 C24 C23 C22 0.6(3) . . . . ?
O1 C1 C2 O2 -3.4(3) . . . . ?
C6 C1 C2 O2 175.19(18) . . . . ?
O1 C1 C2 C3 178.92(18) . . . . ?
C6 C1 C2 C3 -2.5(3) . . . . ?
O3 C3 C2 O2 1.1(3) . . . . ?
C4 C3 C2 O2 -174.99(18) . . . . ?
O3 C3 C2 C1 178.69(18) . . . . ?
C4 C3 C2 C1 2.6(3) . . . . ?
C1 C6 C5 C4 -0.1(3) . . . . ?
C28 C6 C5 C4 -178.84(18) . . . . ?
C23 C22 C27 C26 -1.8(3) . . . . ?
O10 C22 C27 C26 178.27(17) . . . . ?
C23 C22 C27 C21 177.06(19) . . . . ?
O10 C22 C27 C21 -2.9(3) . . . . ?
C25 C26 C27 C22 -0.3(3) . . . . ?
C25 C26 C27 C21 -179.13(18) . . . . ?
N2 N1 C33 C42 1.1(3) . . . . ?
N2 N1 C33 C34 179.08(17) . . . . ?
O13 C42 C33 N1 -5.6(3) . . . . ?
C41 C42 C33 N1 174.7(2) . . . . ?
O13 C42 C33 C34 176.49(19) . . . . ?
C41 C42 C33 C34 -3.2(3) . . . . ?
C8 C9 C10 O6 -179.92(18) . . . . ?
O5 C9 C10 O6 -1.0(3) . . . . ?
C8 C9 C10 C11 1.3(3) . . . . ?
O5 C9 C10 C11 -179.80(18) . . . . ?
C12 C11 C10 O6 179.59(18) . . . . ?
C14 C11 C10 O6 -0.4(3) . . . . ?
C12 C11 C10 C9 -1.8(3) . . . . ?
C14 C11 C10 C9 178.21(18) . . . . ?
O12 C24 C25 C26 -179.19(18) . . . . ?
C23 C24 C25 C26 -2.6(3) . . . . ?
O12 C24 C25 C28 0.7(3) . . . . ?
C23 C24 C25 C28 177.28(19) . . . . ?
C27 C26 C25 C24 2.4(3) . . . . ?
C27 C26 C25 C28 -177.44(18) . . . . ?
C6 C28 C25 C24 89.3(2) . . . . ?
C32 C28 C25 C24 -143.56(19) . . . . ?
C6 C28 C25 C26 -90.8(2) . . . . ?
C32 C28 C25 C26 36.3(3) . . . . ?
C22 C27 C21 C18 -90.3(2) . . . . ?
C26 C27 C21 C18 88.5(2) . . . . ?
C22 C27 C21 C31 142.41(19) . . . . ?
C26 C27 C21 C31 -38.8(3) . . . . ?
C19 C18 C21 C27 -88.2(2) . . . . ?
C17 C18 C21 C27 89.5(2) . . . . ?
C19 C18 C21 C31 38.9(3) . . . . ?
C17 C18 C21 C31 -143.42(19) . . . . ?
C6 C5 C4 C3 0.2(3) . . . . ?
C6 C5 C4 C7 -179.42(18) . . . . ?
O3 C3 C4 C5 -177.14(18) . . . . ?
C2 C3 C4 C5 -1.4(3) . . . . ?
O3 C3 C4 C7 2.5(3) . . . . ?
C2 C3 C4 C7 178.21(18) . . . . ?
C13 C7 C4 C5 -87.8(2) . . . . ?
C29 C7 C4 C5 39.8(3) . . . . ?
C13 C7 C4 C3 92.6(2) . . . . ?
C29 C7 C4 C3 -139.80(19) . . . . ?
C47 N3 C43 C44 -2.3(3) . . . . ?
C47 N3 C43 N2 177.80(18) . . . . ?
N1 N2 C43 N3 179.30(17) . . . . ?
N1 N2 C43 C44 -0.6(3) . . . . ?
N1 C33 C34 C35 4.2(3) . . . . ?
C42 C33 C34 C35 -177.8(2) . . . . ?
N1 C33 C34 C39 -176.99(19) . . . . ?
C42 C33 C34 C39 1.1(3) . . . . ?
C39 C40 C41 C42 -1.7(3) . . . . ?
O13 C42 C41 C40 -176.1(2) . . . . ?
C33 C42 C41 C40 3.5(3) . . . . ?
N3 C43 C44 C45 1.4(3) . . . . ?
N2 C43 C44 C45 -178.75(19) . . . . ?
C35 C34 C39 C38 0.1(3) . . . . ?
C33 C34 C39 C38 -178.82(19) . . . . ?
C35 C34 C39 C40 179.7(2) . . . . ?
C33 C34 C39 C40 0.8(3) . . . . ?
C41 C40 C39 C38 179.1(2) . . . . ?
C41 C40 C39 C34 -0.5(3) . . . . ?
O8 C16 C15 O7 0.1(3) . . . . ?
C17 C16 C15 O7 179.28(18) . . . . ?
O8 C16 C15 C20 179.20(18) . . . . ?
C17 C16 C15 C20 -1.6(3) . . . . ?
C19 C20 C15 O7 179.90(17) . . . . ?
C14 C20 C15 O7 0.5(3) . . . . ?
C19 C20 C15 C16 0.8(3) . . . . ?
C14 C20 C15 C16 -178.59(19) . . . . ?
C43 C44 C45 C46 0.9(3) . . . . ?
C47 C46 C45 C44 -2.1(3) . . . . ?
C39 C34 C35 C36 -0.6(3) . . . . ?
C33 C34 C35 C36 178.3(2) . . . . ?
C43 N3 C47 C46 1.0(3) . . . . ?
C45 C46 C47 N3 1.1(3) . . . . ?
C34 C39 C38 C37 0.5(3) . . . . ?
C40 C39 C38 C37 -179.1(2) . . . . ?
C34 C35 C36 C37 0.5(3) . . . . ?
C39 C38 C37 C36 -0.6(4) . . . . ?
C35 C36 C37 C38 0.0(4) . . . . ?
C58 N5 N4 C48 179.68(18) . . . . ?
C62 N6 C58 C59 -0.9(3) . . . . ?
C62 N6 C58 N5 177.94(17) . . . . ?
N4 N5 C58 N6 -177.80(17) . . . . ?
N4 N5 C58 C59 1.1(3) . . . . ?
N6 C58 C59 C60 0.1(3) . . . . ?
N5 C58 C59 C60 -178.63(19) . . . . ?
N5 N4 C48 C49 179.77(18) . . . . ?
N5 N4 C48 C57 0.0(3) . . . . ?
N4 C48 C57 O14 0.9(3) . . . . ?
C49 C48 C57 O14 -178.9(2) . . . . ?
N4 C48 C57 C56 -178.9(2) . . . . ?
C49 C48 C57 C56 1.4(3) . . . . ?
C58 N6 C62 C61 0.9(3) . . . . ?
C58 C59 C60 C61 0.6(3) . . . . ?
N6 C62 C61 C60 -0.2(3) . . . . ?
C59 C60 C61 C62 -0.6(3) . . . . ?
N4 C48 C49 C50 -0.6(3) . . . . ?
C57 C48 C49 C50 179.1(2) . . . . ?
N4 C48 C49 C54 179.51(19) . . . . ?
C57 C48 C49 C54 -0.7(3) . . . . ?
O14 C57 C56 C55 179.1(2) . . . . ?
C48 C57 C56 C55 -1.2(3) . . . . ?
C57 C56 C55 C54 0.2(4) . . . . ?
C50 C49 C54 C53 -0.2(3) . . . . ?
C48 C49 C54 C53 179.6(2) . . . . ?
C50 C49 C54 C55 179.9(2) . . . . ?
C48 C49 C54 C55 -0.2(3) . . . . ?
C56 C55 C54 C53 -179.4(2) . . . . ?
C56 C55 C54 C49 0.5(4) . . . . ?
C49 C54 C53 C52 -0.8(4) . . . . ?
C55 C54 C53 C52 179.0(2) . . . . ?
C52 C51 C50 C49 -1.0(4) . . . . ?
C54 C49 C50 C51 1.1(3) . . . . ?
C48 C49 C50 C51 -178.7(2) . . . . ?
C54 C53 C52 C51 1.0(4) . . . . ?
C50 C51 C52 C53 -0.1(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        27.27
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.242
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.051

_database_code_depnum_ccdc_archive 'CCDC 1002497'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_3cp26a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            
'C-ethylpyrogallol[4]arene with 1-(2-pyridylazo)-2-napthol'
_chemical_formula_moiety         'C36 H40 O12, 2(C15 H11 O1 N3), C1 H4 O1'
_chemical_formula_sum            'C67 H66 N6 O15'
_chemical_melting_point          ?

_exptl_crystal_description       plate
_exptl_crystal_colour            orange

_diffrn_ambient_temperature      173(2)
_chemical_formula_weight         1195.26

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'
O O 0.0106 0.0060 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?

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

_cell_length_a                   12.6468(16)
_cell_length_b                   15.636(2)
_cell_length_c                   16.887(2)
_cell_angle_alpha                64.978(2)
_cell_angle_beta                 81.891(2)
_cell_angle_gamma                68.093(2)
_cell_volume                     2806.9(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    5885
_cell_measurement_theta_min      2.2
_cell_measurement_theta_max      25.7
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1260
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_process_details   
;
 Data were corrected for decay and absorption using the program SADABS 
 (Sheldrick, G. M. (2003). SADABS. Version 2.10. University of
 Göttingen, Germany).
;

_exptl_special_details           
; 
 ? 
;
_diffrn_radiation_probe          ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.0
_diffrn_reflns_number            29579
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0497
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.53
_diffrn_reflns_theta_max         25.91
_reflns_number_total             10865
_reflns_number_gt                7017
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2008)'
_computing_structure_solution    'SHELXS-1997 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-1997 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-SEED, Barbour, 2001'
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. There is minor residual electron
 density near the probe which is minor disorder that is not included. The 
 hydrogen on the pyrogallol[4]arene's hydroxyl groups are disordered and not
 included which accounts for the short distances.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0862P)²+2.1572P] where P=(Fo²+2Fc²)/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         10865
_refine_ls_number_parameters     809
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0975
_refine_ls_R_factor_gt           0.0577
_refine_ls_wR_factor_ref         0.1785
_refine_ls_wR_factor_gt          0.1506
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_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
O3 O 0.94861(15) 0.43060(14) 0.38925(12) 0.0260(4) Uani 1 1 d . . .
H3 H 0.8899 0.4540 0.3603 0.031 Uiso 1 1 calc R . .
O9 O 1.80544(15) 0.41365(15) 0.27381(13) 0.0308(5) Uani 1 1 d . . .
H9 H 1.8029 0.3567 0.2985 0.037 Uiso 1 1 calc R . .
O4 O 1.04070(17) 0.55831(16) 0.41174(13) 0.0320(5) Uani 1 1 d . . .
H4 H 1.0126 0.5280 0.3965 0.038 Uiso 1 1 calc R . .
O1 O 1.21794(17) 0.12372(14) 0.37824(12) 0.0288(5) Uani 1 1 d . . .
H1 H 1.2062 0.1005 0.4308 0.035 Uiso 1 1 calc R . .
O8 O 1.74493(16) 0.57486(16) 0.30750(13) 0.0330(5) Uani 1 1 d . . .
H8 H 1.7254 0.5653 0.3585 0.040 Uiso 1 1 d . . .
O2 O 1.02355(17) 0.22210(15) 0.44628(12) 0.0301(5) Uani 1 1 d . . .
H2 H 1.0283 0.2274 0.4918 0.036 Uiso 1 1 calc R . .
O7 O 1.52330(16) 0.71899(14) 0.26921(13) 0.0305(5) Uani 1 1 d . . .
H7 H 1.4951 0.7722 0.2248 0.037 Uiso 1 1 d . . .
O6 O 1.31588(17) 0.70843(16) 0.34749(13) 0.0333(5) Uani 1 1 d . . .
H6 H 1.3676 0.7197 0.3142 0.040 Uiso 1 1 calc R . .
O12 O 1.42898(17) 0.12141(15) 0.42417(12) 0.0298(5) Uani 1 1 d . . .
H12 H 1.3827 0.1120 0.4022 0.036 Uiso 1 1 calc R . .
O11 O 1.60173(17) 0.14950(16) 0.47457(12) 0.0327(5) Uani 1 1 d . . .
H11 H 1.5582 0.1208 0.5042 0.039 Uiso 1 1 calc R . .
O10 O 1.71299(17) 0.26767(17) 0.35932(13) 0.0361(5) Uani 1 1 d . . .
H10 H 1.7186 0.2385 0.4127 0.043 Uiso 1 1 calc R . .
C2 C 1.0791(2) 0.2782(2) 0.38119(17) 0.0227(6) Uani 1 1 d . . .
N2B N 1.6347(2) -0.01871(17) 0.32515(16) 0.0305(6) Uani 1 1 d . . .
H2B H 1.6470 -0.0430 0.3805 0.037 Uiso 1 1 calc R . .
O5 O 1.17354(18) 0.63122(17) 0.45552(13) 0.0345(5) Uani 1 1 d . . .
H5 H 1.1252 0.6074 0.4833 0.041 Uiso 1 1 calc R . .
O1B O 1.75340(19) -0.04392(15) 0.45028(13) 0.0377(5) Uani 1 1 d . . .
O1C O 1.91359(18) -0.22273(17) 0.40647(14) 0.0384(5) Uani 1 1 d . . .
C4C C 1.5958(2) -0.33948(19) 0.43483(16) 0.0184(5) Uani 1 1 d . . .
H4C H 1.5895 -0.3164 0.3745 0.022 Uiso 1 1 calc R . .
N3B N 1.6989(2) 0.02883(17) 0.26987(16) 0.0304(6) Uani 1 1 d . . .
N2C N 1.7492(2) -0.28250(18) 0.41814(15) 0.0297(6) Uani 1 1 d . . .
H2C H 1.7971 -0.2730 0.4421 0.036 Uiso 1 1 calc R . .
N3C N 1.7493(2) -0.25331(17) 0.33253(15) 0.0275(5) Uani 1 1 d . . .
C6 C 1.2328(2) 0.2808(2) 0.27707(16) 0.0214(6) Uani 1 1 d . . .
C23 C 1.5685(2) 0.1940(2) 0.38847(17) 0.0250(6) Uani 1 1 d . . .
C3 C 1.0391(2) 0.3826(2) 0.34832(17) 0.0223(6) Uani 1 1 d . . .
C24 C 1.4790(2) 0.1826(2) 0.35951(17) 0.0235(6) Uani 1 1 d . . .
C12 C 1.2004(2) 0.63352(19) 0.20836(17) 0.0229(6) Uani 1 1 d . . .
H12A H 1.2077 0.6339 0.1526 0.027 Uiso 1 1 calc R . .
C5C C 1.6736(2) -0.3284(2) 0.47132(18) 0.0272(6) Uani 1 1 d . . .
C9 C 1.1807(2) 0.6314(2) 0.37383(18) 0.0253(6) Uani 1 1 d . . .
C4 C 1.0922(2) 0.43875(19) 0.27781(17) 0.0212(6) Uani 1 1 d . . .
C19 C 1.5142(2) 0.5446(2) 0.18050(17) 0.0247(6) Uani 1 1 d . . .
H19 H 1.4632 0.5375 0.1510 0.030 Uiso 1 1 calc R . .
C25 C 1.4448(2) 0.2332(2) 0.27147(17) 0.0225(6) Uani 1 1 d . . .
C15 C 1.5561(2) 0.6386(2) 0.24502(17) 0.0252(6) Uani 1 1 d . . .
C26 C 1.5046(2) 0.2940(2) 0.21482(17) 0.0235(6) Uani 1 1 d . . .
H26 H 1.4832 0.3277 0.1560 0.028 Uiso 1 1 calc R . .
C16 C 1.6651(2) 0.5668(2) 0.26597(18) 0.0258(6) Uani 1 1 d . . .
C27 C 1.5947(2) 0.3066(2) 0.24204(17) 0.0240(6) Uani 1 1 d . . .
C17 C 1.6970(2) 0.4823(2) 0.24669(18) 0.0262(6) Uani 1 1 d . . .
C8 C 1.1129(2) 0.5940(2) 0.34838(17) 0.0233(6) Uani 1 1 d . . .
C7 C 1.0458(2) 0.5543(2) 0.23782(17) 0.0230(6) Uani 1 1 d . . .
H7A H 0.9711 0.5751 0.2635 0.028 Uiso 1 1 calc R . .
C1 C 1.1757(2) 0.2277(2) 0.34569(17) 0.0238(6) Uani 1 1 d . . .
C21 C 1.6549(2) 0.3780(2) 0.18129(17) 0.0259(6) Uani 1 1 d . . .
H21 H 1.7368 0.3421 0.1939 0.031 Uiso 1 1 calc R . .
C10 C 1.2570(2) 0.6705(2) 0.31620(18) 0.0246(6) Uani 1 1 d . . .
C20 C 1.4793(2) 0.6289(2) 0.20013(17) 0.0242(6) Uani 1 1 d . . .
N1C N 1.6856(3) -0.3595(2) 0.56127(19) 0.0480(7) Uani 1 1 d . . .
C22 C 1.6259(2) 0.2551(2) 0.33016(18) 0.0258(6) Uani 1 1 d . . .
C28 C 1.3417(2) 0.2255(2) 0.24093(17) 0.0239(6) Uani 1 1 d . . .
H28 H 1.3502 0.1541 0.2668 0.029 Uiso 1 1 calc R . .
C6B C 1.7789(3) 0.0437(2) 0.29956(18) 0.0290(6) Uani 1 1 d . . .
N1B N 1.4789(2) -0.06805(19) 0.35560(16) 0.0371(6) Uani 1 1 d . . .
C14 C 1.3596(2) 0.7088(2) 0.17322(18) 0.0268(6) Uani 1 1 d . . .
H14 H 1.3593 0.7657 0.1841 0.032 Uiso 1 1 calc R . .
C5B C 1.5463(3) -0.0296(2) 0.29343(18) 0.0301(7) Uani 1 1 d . . .
C6C C 1.8233(2) -0.2103(2) 0.28615(19) 0.0275(6) Uani 1 1 d . . .
C18 C 1.6219(2) 0.4702(2) 0.20305(17) 0.0242(6) Uani 1 1 d . . .
C5 C 1.1891(2) 0.3857(2) 0.24499(17) 0.0226(6) Uani 1 1 d . . .
H5A H 1.2266 0.4219 0.1995 0.027 Uiso 1 1 calc R . .
C11 C 1.2696(2) 0.6712(2) 0.23238(18) 0.0239(6) Uani 1 1 d . . .
C7C C 1.8159(2) -0.1744(2) 0.19122(19) 0.0296(7) Uani 1 1 d . . .
C13 C 1.1209(2) 0.59530(19) 0.26418(17) 0.0232(6) Uani 1 1 d . . .
C15C C 1.9087(3) -0.1959(2) 0.3249(2) 0.0304(7) Uani 1 1 d . . .
C15B C 1.8051(3) 0.0073(2) 0.3924(2) 0.0355(7) Uani 1 1 d . . .
C29 C 1.0257(2) 0.5968(2) 0.13886(18) 0.0282(6) Uani 1 1 d . . .
H29A H 0.9996 0.6698 0.1156 0.034 Uiso 1 1 calc R . .
H29B H 1.0973 0.5739 0.1116 0.034 Uiso 1 1 calc R . .
C7B C 1.8436(3) 0.1011(2) 0.23366(19) 0.0319(7) Uani 1 1 d . . .
C13C C 1.9791(3) -0.1199(2) 0.1809(2) 0.0403(8) Uani 1 1 d . . .
H13C H 2.0314 -0.0918 0.1459 0.048 Uiso 1 1 calc R . .
C14C C 1.9864(3) -0.1504(2) 0.2678(2) 0.0363(7) Uani 1 1 d . . .
H14C H 2.0421 -0.1420 0.2914 0.044 Uiso 1 1 calc R . .
C4B C 1.5320(3) -0.0032(2) 0.20495(19) 0.0353(7) Uani 1 1 d . . .
H4B H 1.5821 0.0217 0.1639 0.042 Uiso 1 1 calc R . .
C33 C 1.6367(3) 0.4074(2) 0.08424(18) 0.0308(7) Uani 1 1 d . . .
H33A H 1.6542 0.3469 0.0743 0.037 Uiso 1 1 calc R . .
H33B H 1.5571 0.4477 0.0684 0.037 Uiso 1 1 calc R . .
C3C C 1.5267(3) -0.3854(2) 0.4888(2) 0.0359(7) Uani 1 1 d . . .
H13 H 1.4719 -0.3941 0.4645 0.043 Uiso 1 1 calc R . .
C12C C 1.8939(3) -0.1288(2) 0.1394(2) 0.0354(7) Uani 1 1 d . . .
C8B C 1.8256(3) 0.1355(2) 0.14379(19) 0.0348(7) Uani 1 1 d . . .
H8B H 1.7714 0.1217 0.1239 0.042 Uiso 1 1 calc R . .
C31 C 1.3355(3) 0.7496(2) 0.07623(19) 0.0357(7) Uani 1 1 d . . .
H31A H 1.2584 0.7979 0.0628 0.043 Uiso 1 1 calc R . .
H31B H 1.3405 0.6948 0.0612 0.043 Uiso 1 1 calc R . .
C2C C 1.5330(3) -0.4203(2) 0.5782(2) 0.0344(7) Uani 1 1 d . . .
H15 H 1.4843 -0.4529 0.6134 0.041 Uiso 1 1 calc R . .
C35 C 1.3340(2) 0.2614(2) 0.14185(18) 0.0282(6) Uani 1 1 d . . .
H35A H 1.3265 0.3318 0.1144 0.034 Uiso 1 1 calc R . .
H35B H 1.4043 0.2236 0.1221 0.034 Uiso 1 1 calc R . .
C1C C 1.6126(2) -0.4063(2) 0.61480(19) 0.0318(7) Uani 1 1 d . . .
H18 H 1.6172 -0.4282 0.6751 0.038 Uiso 1 1 calc R . .
C8C C 1.7328(3) -0.1814(2) 0.1497(2) 0.0349(7) Uani 1 1 d . . .
H8C H 1.6810 -0.2111 0.1831 0.042 Uiso 1 1 calc R . .
C30 C 0.9383(3) 0.5653(3) 0.1151(2) 0.0400(8) Uani 1 1 d . . .
H30A H 0.9616 0.4931 0.1404 0.060 Uiso 1 1 calc R . .
H30B H 0.9330 0.5897 0.0526 0.060 Uiso 1 1 calc R . .
H30C H 0.8653 0.5932 0.1371 0.060 Uiso 1 1 calc R . .
C36 C 1.2348(3) 0.2491(3) 0.1125(2) 0.0375(7) Uani 1 1 d . . .
H36A H 1.2399 0.1800 0.1412 0.056 Uiso 1 1 calc R . .
H36B H 1.2370 0.2688 0.0504 0.056 Uiso 1 1 calc R . .
H36C H 1.1645 0.2909 0.1273 0.056 Uiso 1 1 calc R . .
C34 C 1.7104(3) 0.4668(3) 0.0258(2) 0.0437(8) Uani 1 1 d . . .
H34A H 1.6879 0.5302 0.0307 0.066 Uiso 1 1 calc R . .
H34B H 1.7010 0.4785 -0.0338 0.066 Uiso 1 1 calc R . .
H34C H 1.7890 0.4291 0.0436 0.066 Uiso 1 1 calc R . .
C2B C 1.3687(3) -0.0531(2) 0.2429(2) 0.0430(8) Uani 1 1 d . . .
H16 H 1.3062 -0.0607 0.2271 0.052 Uiso 1 1 calc R . .
C1B C 1.3915(3) -0.0791(3) 0.3291(2) 0.0459(9) Uani 1 1 d . . .
H20 H 1.3436 -0.1059 0.3714 0.055 Uiso 1 1 calc R . .
C3B C 1.4417(3) -0.0153(2) 0.1804(2) 0.0416(8) Uani 1 1 d . . .
H17 H 1.4292 0.0019 0.1217 0.050 Uiso 1 1 calc R . .
C9C C 1.7271(3) -0.1448(3) 0.0597(2) 0.0425(8) Uani 1 1 d . . .
H9C H 1.6716 -0.1500 0.0331 0.051 Uiso 1 1 calc R . .
C12B C 1.9270(3) 0.1222(2) 0.2619(2) 0.0415(8) Uani 1 1 d . . .
C10B C 1.9684(3) 0.2124(3) 0.1123(2) 0.0464(9) Uani 1 1 d . . .
H10B H 2.0090 0.2501 0.0717 0.056 Uiso 1 1 calc R . .
C11C C 1.8859(3) -0.0922(3) 0.0477(2) 0.0469(9) Uani 1 1 d . . .
H11C H 1.9370 -0.0624 0.0132 0.056 Uiso 1 1 calc R . .
C11B C 1.9880(3) 0.1788(3) 0.2001(2) 0.0489(9) Uani 1 1 d . . .
H11B H 2.0421 0.1937 0.2189 0.059 Uiso 1 1 calc R . .
C9B C 1.8883(3) 0.1900(3) 0.0844(2) 0.0419(8) Uani 1 1 d . . .
H9B H 1.8763 0.2119 0.0248 0.050 Uiso 1 1 calc R . .
C10C C 1.8038(3) -0.0999(3) 0.0084(2) 0.0502(9) Uani 1 1 d . . .
H10C H 1.7996 -0.0753 -0.0522 0.060 Uiso 1 1 calc R . .
C32 C 1.4192(3) 0.8005(3) 0.0207(2) 0.0539(10) Uani 1 1 d . . .
H32A H 1.4130 0.8560 0.0341 0.081 Uiso 1 1 calc R . .
H5C H 1.4014 0.8248 -0.0402 0.081 Uiso 1 1 calc R . .
H32C H 1.4955 0.7527 0.0332 0.081 Uiso 1 1 calc R . .
C14B C 1.8930(4) 0.0307(3) 0.4153(2) 0.0609(12) Uani 1 1 d . . .
H14B H 1.9118 0.0072 0.4739 0.073 Uiso 1 1 calc R . .
C13B C 1.9487(4) 0.0859(3) 0.3537(2) 0.0642(12) Uani 1 1 d . . .
H13B H 2.0034 0.1011 0.3713 0.077 Uiso 1 1 calc R . .
C1D C 0.1554(11) 0.8738(11) 0.4223(9) 0.270(7) Uani 1 1 d U . .
H1D1 H 0.0746 0.8940 0.4309 0.405 Uiso 1 1 calc R . .
H1D2 H 0.1719 0.8664 0.3678 0.405 Uiso 1 1 calc R . .
H1D3 H 0.1824 0.9242 0.4211 0.405 Uiso 1 1 calc R . .
O1D O 0.2035(3) 0.7930(2) 0.48246(17) 0.0567(7) Uani 1 1 d . . .
H1D H 0.2432 0.7521 0.4624 0.068 Uiso 1 1 calc R . .


_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
O3 C3 1.387(3) . ?
O3 H3 0.8200 . ?
O9 C17 1.380(3) . ?
O9 H9 0.8200 . ?
O4 C8 1.375(3) . ?
O4 H4 0.8200 . ?
O1 C1 1.382(3) . ?
O1 H1 0.8200 . ?
O8 C16 1.377(3) . ?
O8 H8 0.8272 . ?
O2 C2 1.377(3) . ?
O2 H2 0.8200 . ?
O7 C15 1.385(3) . ?
O7 H7 0.8415 . ?
O6 C10 1.375(3) . ?
O6 H6 0.8200 . ?
O12 C24 1.371(3) . ?
O12 H12 0.8200 . ?
O11 C23 1.369(3) . ?
O11 H11 0.8200 . ?
O10 C22 1.374(3) . ?
O10 H10 0.8200 . ?
C2 C3 1.388(4) . ?
C2 C1 1.397(4) . ?
N2B N3B 1.317(3) . ?
N2B C5B 1.397(4) . ?
N2B H2B 0.8600 . ?
O5 C9 1.369(3) . ?
O5 H5 0.8200 . ?
O1B C15B 1.255(4) . ?
O1C C15C 1.262(4) . ?
C4C C5C 1.330(4) . ?
C4C C3C 1.342(4) . ?
C4C H4C 0.9300 . ?
N3B C6B 1.321(4) . ?
N2C N3C 1.319(3) . ?
N2C C5C 1.400(3) . ?
N2C H2C 0.8600 . ?
N3C C6C 1.327(3) . ?
C6 C5 1.394(4) . ?
C6 C1 1.397(4) . ?
C6 C28 1.529(4) . ?
C23 C22 1.390(4) . ?
C23 C24 1.390(4) . ?
C3 C4 1.403(4) . ?
C24 C25 1.398(4) . ?
C12 C13 1.400(4) . ?
C12 C11 1.401(4) . ?
C12 H12A 0.9300 . ?
C5C N1C 1.397(4) . ?
C9 C10 1.387(4) . ?
C9 C8 1.396(4) . ?
C4 C5 1.392(4) . ?
C4 C7 1.534(4) . ?
C19 C20 1.393(4) . ?
C19 C18 1.394(4) . ?
C19 H19 0.9300 . ?
C25 C26 1.399(4) . ?
C25 C28 1.529(4) . ?
C15 C16 1.390(4) . ?
C15 C20 1.398(4) . ?
C26 C27 1.393(4) . ?
C26 H26 0.9300 . ?
C16 C17 1.394(4) . ?
C27 C22 1.391(4) . ?
C27 C21 1.524(4) . ?
C17 C18 1.390(4) . ?
C8 C13 1.404(4) . ?
C7 C13 1.525(4) . ?
C7 C29 1.534(4) . ?
C7 H7A 0.9800 . ?
C21 C33 1.530(4) . ?
C21 C18 1.530(4) . ?
C21 H21 0.9800 . ?
C10 C11 1.398(4) . ?
C20 C14 1.537(4) . ?
N1C C1C 1.383(4) . ?
C28 C35 1.528(4) . ?
C28 H28 0.9800 . ?
C6B C15B 1.464(4) . ?
C6B C7B 1.470(4) . ?
N1B C5B 1.337(4) . ?
N1B C1B 1.341(4) . ?
C14 C31 1.515(4) . ?
C14 C11 1.524(4) . ?
C14 H14 0.9800 . ?
C5B C4B 1.391(4) . ?
C6C C7C 1.461(4) . ?
C6C C15C 1.467(4) . ?
C5 H5A 0.9300 . ?
C7C C8C 1.403(4) . ?
C7C C12C 1.415(4) . ?
C15C C14C 1.441(4) . ?
C15B C14B 1.436(5) . ?
C29 C30 1.525(4) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C7B C8B 1.400(4) . ?
C7B C12B 1.408(4) . ?
C13C C14C 1.344(5) . ?
C13C C12C 1.442(5) . ?
C13C H13C 0.9300 . ?
C14C H14C 0.9300 . ?
C4B C3B 1.369(5) . ?
C4B H4B 0.9300 . ?
C33 C34 1.522(4) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C3C C2C 1.373(4) . ?
C3C H13 0.9300 . ?
C12C C11C 1.409(5) . ?
C8B C9B 1.384(4) . ?
C8B H8B 0.9300 . ?
C31 C32 1.534(4) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C2C C1C 1.379(4) . ?
C2C H15 0.9300 . ?
C35 C36 1.514(4) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C1C H18 0.9300 . ?
C8C C9C 1.381(4) . ?
C8C H8C 0.9300 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C2B C1B 1.378(4) . ?
C2B C3B 1.386(5) . ?
C2B H16 0.9300 . ?
C1B H20 0.9300 . ?
C3B H17 0.9300 . ?
C9C C10C 1.393(5) . ?
C9C H9C 0.9300 . ?
C12B C11B 1.402(5) . ?
C12B C13B 1.435(5) . ?
C10B C11B 1.373(5) . ?
C10B C9B 1.383(5) . ?
C10B H10B 0.9300 . ?
C11C C10C 1.374(5) . ?
C11C H11C 0.9300 . ?
C11B H11B 0.9300 . ?
C9B H9B 0.9300 . ?
C10C H10C 0.9300 . ?
C32 H32A 0.9600 . ?
C32 H5C 0.9600 . ?
C32 H32C 0.9600 . ?
C14B C13B 1.345(5) . ?
C14B H14B 0.9300 . ?
C13B H13B 0.9300 . ?
C1D O1D 1.231(13) . ?
C1D H1D1 0.9600 . ?
C1D H1D2 0.9600 . ?
C1D H1D3 0.9600 . ?
O1D H1D 0.8200 . ?

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
C3 O3 H3 109.5 . . ?
C17 O9 H9 109.5 . . ?
C8 O4 H4 109.5 . . ?
C1 O1 H1 109.5 . . ?
C16 O8 H8 108.9 . . ?
C2 O2 H2 109.5 . . ?
C15 O7 H7 107.9 . . ?
C10 O6 H6 109.5 . . ?
C24 O12 H12 109.5 . . ?
C23 O11 H11 109.5 . . ?
C22 O10 H10 109.5 . . ?
O2 C2 C3 121.8(2) . . ?
O2 C2 C1 118.4(2) . . ?
C3 C2 C1 119.7(2) . . ?
N3B N2B C5B 119.7(2) . . ?
N3B N2B H2B 120.2 . . ?
C5B N2B H2B 120.2 . . ?
C9 O5 H5 109.5 . . ?
C5C C4C C3C 117.1(3) . . ?
C5C C4C H4C 121.4 . . ?
C3C C4C H4C 121.4 . . ?
N2B N3B C6B 119.9(2) . . ?
N3C N2C C5C 122.2(2) . . ?
N3C N2C H2C 118.9 . . ?
C5C N2C H2C 118.9 . . ?
N2C N3C C6C 118.9(2) . . ?
C5 C6 C1 117.6(2) . . ?
C5 C6 C28 121.4(2) . . ?
C1 C6 C28 121.0(2) . . ?
O11 C23 C22 116.9(2) . . ?
O11 C23 C24 122.6(2) . . ?
C22 C23 C24 120.5(2) . . ?
O3 C3 C2 118.6(2) . . ?
O3 C3 C4 120.4(2) . . ?
C2 C3 C4 121.0(2) . . ?
O12 C24 C23 114.3(2) . . ?
O12 C24 C25 125.2(2) . . ?
C23 C24 C25 120.5(2) . . ?
C13 C12 C11 123.2(3) . . ?
C13 C12 H12A 118.4 . . ?
C11 C12 H12A 118.4 . . ?
C4C C5C N1C 124.1(3) . . ?
C4C C5C N2C 119.5(2) . . ?
N1C C5C N2C 116.4(3) . . ?
O5 C9 C10 118.1(2) . . ?
O5 C9 C8 121.4(2) . . ?
C10 C9 C8 120.5(3) . . ?
C5 C4 C3 117.5(2) . . ?
C5 C4 C7 120.8(2) . . ?
C3 C4 C7 121.7(2) . . ?
C20 C19 C18 123.0(3) . . ?
C20 C19 H19 118.5 . . ?
C18 C19 H19 118.5 . . ?
C24 C25 C26 117.4(2) . . ?
C24 C25 C28 120.3(2) . . ?
C26 C25 C28 122.3(2) . . ?
O7 C15 C16 120.1(2) . . ?
O7 C15 C20 120.0(2) . . ?
C16 C15 C20 119.9(3) . . ?
C27 C26 C25 123.3(2) . . ?
C27 C26 H26 118.3 . . ?
C25 C26 H26 118.3 . . ?
O8 C16 C15 122.0(3) . . ?
O8 C16 C17 117.4(2) . . ?
C15 C16 C17 120.7(3) . . ?
C22 C27 C26 117.5(2) . . ?
C22 C27 C21 119.2(2) . . ?
C26 C27 C21 123.2(2) . . ?
O9 C17 C18 123.5(3) . . ?
O9 C17 C16 115.9(2) . . ?
C18 C17 C16 120.6(2) . . ?
O4 C8 C9 114.3(2) . . ?
O4 C8 C13 125.1(2) . . ?
C9 C8 C13 120.6(2) . . ?
C13 C7 C4 110.8(2) . . ?
C13 C7 C29 114.0(2) . . ?
C4 C7 C29 111.4(2) . . ?
C13 C7 H7A 106.7 . . ?
C4 C7 H7A 106.7 . . ?
C29 C7 H7A 106.7 . . ?
O1 C1 C2 120.7(2) . . ?
O1 C1 C6 118.3(2) . . ?
C2 C1 C6 121.0(2) . . ?
C27 C21 C33 113.7(2) . . ?
C27 C21 C18 110.0(2) . . ?
C33 C21 C18 112.1(2) . . ?
C27 C21 H21 106.9 . . ?
C33 C21 H21 106.9 . . ?
C18 C21 H21 106.9 . . ?
O6 C10 C9 115.2(2) . . ?
O6 C10 C11 124.0(2) . . ?
C9 C10 C11 120.8(2) . . ?
C19 C20 C15 118.1(2) . . ?
C19 C20 C14 120.7(2) . . ?
C15 C20 C14 121.2(3) . . ?
C1C N1C C5C 117.1(3) . . ?
O10 C22 C23 120.3(2) . . ?
O10 C22 C27 118.9(2) . . ?
C23 C22 C27 120.8(3) . . ?
C35 C28 C25 113.5(2) . . ?
C35 C28 C6 111.9(2) . . ?
C25 C28 C6 109.6(2) . . ?
C35 C28 H28 107.2 . . ?
C25 C28 H28 107.2 . . ?
C6 C28 H28 107.2 . . ?
N3B C6B C15B 124.1(3) . . ?
N3B C6B C7B 116.6(3) . . ?
C15B C6B C7B 119.4(3) . . ?
C5B N1B C1B 116.8(3) . . ?
C31 C14 C11 114.9(2) . . ?
C31 C14 C20 112.3(2) . . ?
C11 C14 C20 111.0(2) . . ?
C31 C14 H14 106.0 . . ?
C11 C14 H14 106.0 . . ?
C20 C14 H14 106.0 . . ?
N1B C5B C4B 123.9(3) . . ?
N1B C5B N2B 113.9(3) . . ?
C4B C5B N2B 122.2(3) . . ?
N3C C6C C7C 116.8(3) . . ?
N3C C6C C15C 123.7(3) . . ?
C7C C6C C15C 119.5(3) . . ?
C17 C18 C19 117.6(3) . . ?
C17 C18 C21 121.6(2) . . ?
C19 C18 C21 120.8(2) . . ?
C4 C5 C6 123.1(2) . . ?
C4 C5 H5A 118.4 . . ?
C6 C5 H5A 118.4 . . ?
C10 C11 C12 117.6(2) . . ?
C10 C11 C14 119.1(2) . . ?
C12 C11 C14 123.3(2) . . ?
C8C C7C C12C 118.9(3) . . ?
C8C C7C C6C 122.5(3) . . ?
C12C C7C C6C 118.6(3) . . ?
C12 C13 C8 117.3(2) . . ?
C12 C13 C7 123.0(2) . . ?
C8 C13 C7 119.7(2) . . ?
O1C C15C C14C 120.9(3) . . ?
O1C C15C C6C 120.6(3) . . ?
C14C C15C C6C 118.5(3) . . ?
O1B C15B C14B 120.9(3) . . ?
O1B C15B C6B 121.0(3) . . ?
C14B C15B C6B 118.1(3) . . ?
C30 C29 C7 112.9(2) . . ?
C30 C29 H29A 109.0 . . ?
C7 C29 H29A 109.0 . . ?
C30 C29 H29B 109.0 . . ?
C7 C29 H29B 109.0 . . ?
H29A C29 H29B 107.8 . . ?
C8B C7B C12B 118.7(3) . . ?
C8B C7B C6B 122.5(3) . . ?
C12B C7B C6B 118.8(3) . . ?
C14C C13C C12C 122.9(3) . . ?
C14C C13C H13C 118.5 . . ?
C12C C13C H13C 118.5 . . ?
C13C C14C C15C 120.7(3) . . ?
C13C C14C H14C 119.7 . . ?
C15C C14C H14C 119.7 . . ?
C3B C4B C5B 117.7(3) . . ?
C3B C4B H4B 121.2 . . ?
C5B C4B H4B 121.2 . . ?
C34 C33 C21 112.5(3) . . ?
C34 C33 H33A 109.1 . . ?
C21 C33 H33A 109.1 . . ?
C34 C33 H33B 109.1 . . ?
C21 C33 H33B 109.1 . . ?
H33A C33 H33B 107.8 . . ?
C4C C3C C2C 123.2(3) . . ?
C4C C3C H13 118.4 . . ?
C2C C3C H13 118.4 . . ?
C11C C12C C7C 119.0(3) . . ?
C11C C12C C13C 121.4(3) . . ?
C7C C12C C13C 119.7(3) . . ?
C9B C8B C7B 120.2(3) . . ?
C9B C8B H8B 119.9 . . ?
C7B C8B H8B 119.9 . . ?
C14 C31 C32 112.1(3) . . ?
C14 C31 H31A 109.2 . . ?
C32 C31 H31A 109.2 . . ?
C14 C31 H31B 109.2 . . ?
C32 C31 H31B 109.2 . . ?
H31A C31 H31B 107.9 . . ?
C3C C2C C1C 118.9(3) . . ?
C3C C2C H15 120.6 . . ?
C1C C2C H15 120.6 . . ?
C36 C35 C28 113.2(2) . . ?
C36 C35 H35A 108.9 . . ?
C28 C35 H35A 108.9 . . ?
C36 C35 H35B 108.9 . . ?
C28 C35 H35B 108.9 . . ?
H35A C35 H35B 107.8 . . ?
C2C C1C N1C 119.6(3) . . ?
C2C C1C H18 120.2 . . ?
N1C C1C H18 120.2 . . ?
C9C C8C C7C 120.7(3) . . ?
C9C C8C H8C 119.6 . . ?
C7C C8C H8C 119.6 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C1B C2B C3B 118.0(3) . . ?
C1B C2B H16 121.0 . . ?
C3B C2B H16 121.0 . . ?
N1B C1B C2B 123.7(3) . . ?
N1B C1B H20 118.1 . . ?
C2B C1B H20 118.1 . . ?
C4B C3B C2B 120.0(3) . . ?
C4B C3B H17 120.0 . . ?
C2B C3B H17 120.0 . . ?
C8C C9C C10C 120.5(3) . . ?
C8C C9C H9C 119.7 . . ?
C10C C9C H9C 119.7 . . ?
C11B C12B C7B 119.8(3) . . ?
C11B C12B C13B 120.5(3) . . ?
C7B C12B C13B 119.7(3) . . ?
C11B C10B C9B 119.8(3) . . ?
C11B C10B H10B 120.1 . . ?
C9B C10B H10B 120.1 . . ?
C10C C11C C12C 121.2(3) . . ?
C10C C11C H11C 119.4 . . ?
C12C C11C H11C 119.4 . . ?
C10B C11B C12B 120.6(3) . . ?
C10B C11B H11B 119.7 . . ?
C12B C11B H11B 119.7 . . ?
C10B C9B C8B 120.9(3) . . ?
C10B C9B H9B 119.5 . . ?
C8B C9B H9B 119.5 . . ?
C11C C10C C9C 119.7(3) . . ?
C11C C10C H10C 120.2 . . ?
C9C C10C H10C 120.2 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H5C 109.5 . . ?
H32A C32 H5C 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H5C C32 H32C 109.5 . . ?
C13B C14B C15B 121.4(3) . . ?
C13B C14B H14B 119.3 . . ?
C15B C14B H14B 119.3 . . ?
C14B C13B C12B 122.6(3) . . ?
C14B C13B H13B 118.7 . . ?
C12B C13B H13B 118.7 . . ?
O1D C1D H1D1 109.5 . . ?
O1D C1D H1D2 109.5 . . ?
H1D1 C1D H1D2 109.5 . . ?
O1D C1D H1D3 109.5 . . ?
H1D1 C1D H1D3 109.5 . . ?
H1D2 C1D H1D3 109.5 . . ?
C1D O1D H1D 109.5 . . ?

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
C5B N2B N3B C6B 176.6(2) . . . . ?
C5C N2C N3C C6C 180.0(2) . . . . ?
O2 C2 C3 O3 7.6(4) . . . . ?
C1 C2 C3 O3 -174.9(2) . . . . ?
O2 C2 C3 C4 -175.4(2) . . . . ?
C1 C2 C3 C4 2.2(4) . . . . ?
O11 C23 C24 O12 -1.4(4) . . . . ?
C22 C23 C24 O12 -179.1(2) . . . . ?
O11 C23 C24 C25 177.1(2) . . . . ?
C22 C23 C24 C25 -0.6(4) . . . . ?
C3C C4C C5C N1C -1.4(4) . . . . ?
C3C C4C C5C N2C 178.9(3) . . . . ?
N3C N2C C5C C4C -2.9(4) . . . . ?
N3C N2C C5C N1C 177.4(2) . . . . ?
O3 C3 C4 C5 174.0(2) . . . . ?
C2 C3 C4 C5 -3.0(4) . . . . ?
O3 C3 C4 C7 -6.0(4) . . . . ?
C2 C3 C4 C7 177.1(2) . . . . ?
O12 C24 C25 C26 178.9(2) . . . . ?
C23 C24 C25 C26 0.5(4) . . . . ?
O12 C24 C25 C28 2.0(4) . . . . ?
C23 C24 C25 C28 -176.3(2) . . . . ?
C24 C25 C26 C27 -0.4(4) . . . . ?
C28 C25 C26 C27 176.3(2) . . . . ?
O7 C15 C16 O8 -2.8(4) . . . . ?
C20 C15 C16 O8 177.8(2) . . . . ?
O7 C15 C16 C17 176.1(2) . . . . ?
C20 C15 C16 C17 -3.3(4) . . . . ?
C25 C26 C27 C22 0.3(4) . . . . ?
C25 C26 C27 C21 -176.0(2) . . . . ?
O8 C16 C17 O9 1.7(4) . . . . ?
C15 C16 C17 O9 -177.2(2) . . . . ?
O8 C16 C17 C18 -178.5(2) . . . . ?
C15 C16 C17 C18 2.5(4) . . . . ?
O5 C9 C8 O4 0.0(4) . . . . ?
C10 C9 C8 O4 -179.5(2) . . . . ?
O5 C9 C8 C13 179.6(2) . . . . ?
C10 C9 C8 C13 0.2(4) . . . . ?
C5 C4 C7 C13 -74.1(3) . . . . ?
C3 C4 C7 C13 105.9(3) . . . . ?
C5 C4 C7 C29 54.0(3) . . . . ?
C3 C4 C7 C29 -126.0(3) . . . . ?
O2 C2 C1 O1 -3.3(4) . . . . ?
C3 C2 C1 O1 179.1(2) . . . . ?
O2 C2 C1 C6 177.3(2) . . . . ?
C3 C2 C1 C6 -0.3(4) . . . . ?
C5 C6 C1 O1 180.0(2) . . . . ?
C28 C6 C1 O1 -2.2(4) . . . . ?
C5 C6 C1 C2 -0.6(4) . . . . ?
C28 C6 C1 C2 177.2(2) . . . . ?
C22 C27 C21 C33 164.5(2) . . . . ?
C26 C27 C21 C33 -19.2(4) . . . . ?
C22 C27 C21 C18 -68.8(3) . . . . ?
C26 C27 C21 C18 107.5(3) . . . . ?
O5 C9 C10 O6 -1.9(4) . . . . ?
C8 C9 C10 O6 177.6(2) . . . . ?
O5 C9 C10 C11 178.9(2) . . . . ?
C8 C9 C10 C11 -1.6(4) . . . . ?
C18 C19 C20 C15 -0.5(4) . . . . ?
C18 C19 C20 C14 179.7(2) . . . . ?
O7 C15 C20 C19 -177.2(2) . . . . ?
C16 C15 C20 C19 2.3(4) . . . . ?
O7 C15 C20 C14 2.6(4) . . . . ?
C16 C15 C20 C14 -177.9(2) . . . . ?
C4C C5C N1C C1C 1.2(4) . . . . ?
N2C C5C N1C C1C -179.1(2) . . . . ?
O11 C23 C22 O10 1.0(4) . . . . ?
C24 C23 C22 O10 178.8(3) . . . . ?
O11 C23 C22 C27 -177.3(2) . . . . ?
C24 C23 C22 C27 0.4(4) . . . . ?
C26 C27 C22 O10 -178.7(2) . . . . ?
C21 C27 C22 O10 -2.2(4) . . . . ?
C26 C27 C22 C23 -0.3(4) . . . . ?
C21 C27 C22 C23 176.2(3) . . . . ?
C24 C25 C28 C35 -165.1(2) . . . . ?
C26 C25 C28 C35 18.2(4) . . . . ?
C24 C25 C28 C6 69.0(3) . . . . ?
C26 C25 C28 C6 -107.7(3) . . . . ?
C5 C6 C28 C35 -55.0(3) . . . . ?
C1 C6 C28 C35 127.3(3) . . . . ?
C5 C6 C28 C25 71.9(3) . . . . ?
C1 C6 C28 C25 -105.9(3) . . . . ?
N2B N3B C6B C15B 2.1(4) . . . . ?
N2B N3B C6B C7B -177.5(2) . . . . ?
C19 C20 C14 C31 -54.9(3) . . . . ?
C15 C20 C14 C31 125.3(3) . . . . ?
C19 C20 C14 C11 75.2(3) . . . . ?
C15 C20 C14 C11 -104.6(3) . . . . ?
C1B N1B C5B C4B -1.5(4) . . . . ?
C1B N1B C5B N2B 179.2(3) . . . . ?
N3B N2B C5B N1B -172.3(2) . . . . ?
N3B N2B C5B C4B 8.4(4) . . . . ?
N2C N3C C6C C7C -176.8(2) . . . . ?
N2C N3C C6C C15C 2.2(4) . . . . ?
O9 C17 C18 C19 179.0(2) . . . . ?
C16 C17 C18 C19 -0.7(4) . . . . ?
O9 C17 C18 C21 -0.2(4) . . . . ?
C16 C17 C18 C21 -179.9(2) . . . . ?
C20 C19 C18 C17 -0.3(4) . . . . ?
C20 C19 C18 C21 178.9(2) . . . . ?
C27 C21 C18 C17 105.6(3) . . . . ?
C33 C21 C18 C17 -126.8(3) . . . . ?
C27 C21 C18 C19 -73.6(3) . . . . ?
C33 C21 C18 C19 54.0(3) . . . . ?
C3 C4 C5 C6 2.0(4) . . . . ?
C7 C4 C5 C6 -178.0(2) . . . . ?
C1 C6 C5 C4 -0.3(4) . . . . ?
C28 C6 C5 C4 -178.1(2) . . . . ?
O6 C10 C11 C12 -177.5(2) . . . . ?
C9 C10 C11 C12 1.7(4) . . . . ?
O6 C10 C11 C14 4.7(4) . . . . ?
C9 C10 C11 C14 -176.2(2) . . . . ?
C13 C12 C11 C10 -0.3(4) . . . . ?
C13 C12 C11 C14 177.4(2) . . . . ?
C31 C14 C11 C10 -154.5(3) . . . . ?
C20 C14 C11 C10 76.8(3) . . . . ?
C31 C14 C11 C12 27.8(4) . . . . ?
C20 C14 C11 C12 -100.9(3) . . . . ?
N3C C6C C7C C8C 2.1(4) . . . . ?
C15C C6C C7C C8C -177.0(3) . . . . ?
N3C C6C C7C C12C -179.5(3) . . . . ?
C15C C6C C7C C12C 1.5(4) . . . . ?
C11 C12 C13 C8 -1.0(4) . . . . ?
C11 C12 C13 C7 -180.0(2) . . . . ?
O4 C8 C13 C12 -179.3(2) . . . . ?
C9 C8 C13 C12 1.1(4) . . . . ?
O4 C8 C13 C7 -0.3(4) . . . . ?
C9 C8 C13 C7 -179.9(2) . . . . ?
C4 C7 C13 C12 102.0(3) . . . . ?
C29 C7 C13 C12 -24.6(4) . . . . ?
C4 C7 C13 C8 -77.0(3) . . . . ?
C29 C7 C13 C8 156.4(2) . . . . ?
N3C C6C C15C O1C -1.8(4) . . . . ?
C7C C6C C15C O1C 177.2(3) . . . . ?
N3C C6C C15C C14C 178.5(3) . . . . ?
C7C C6C C15C C14C -2.6(4) . . . . ?
N3B C6B C15B O1B 2.1(5) . . . . ?
C7B C6B C15B O1B -178.3(3) . . . . ?
N3B C6B C15B C14B -178.8(3) . . . . ?
C7B C6B C15B C14B 0.7(4) . . . . ?
C13 C7 C29 C30 -172.5(2) . . . . ?
C4 C7 C29 C30 61.1(3) . . . . ?
N3B C6B C7B C8B -2.4(4) . . . . ?
C15B C6B C7B C8B 178.0(3) . . . . ?
N3B C6B C7B C12B 177.7(3) . . . . ?
C15B C6B C7B C12B -1.9(4) . . . . ?
C12C C13C C14C C15C 1.1(5) . . . . ?
O1C C15C C14C C13C -178.5(3) . . . . ?
C6C C15C C14C C13C 1.3(4) . . . . ?
N1B C5B C4B C3B 1.7(5) . . . . ?
N2B C5B C4B C3B -179.0(3) . . . . ?
C27 C21 C33 C34 -172.1(2) . . . . ?
C18 C21 C33 C34 62.3(3) . . . . ?
C5C C4C C3C C2C 0.2(5) . . . . ?
C8C C7C C12C C11C -0.2(4) . . . . ?
C6C C7C C12C C11C -178.8(3) . . . . ?
C8C C7C C12C C13C 179.3(3) . . . . ?
C6C C7C C12C C13C 0.8(4) . . . . ?
C14C C13C C12C C11C 177.4(3) . . . . ?
C14C C13C C12C C7C -2.2(5) . . . . ?
C12B C7B C8B C9B -0.6(5) . . . . ?
C6B C7B C8B C9B 179.5(3) . . . . ?
C11 C14 C31 C32 171.3(3) . . . . ?
C20 C14 C31 C32 -60.6(4) . . . . ?
C4C C3C C2C C1C 1.1(5) . . . . ?
C25 C28 C35 C36 177.4(2) . . . . ?
C6 C28 C35 C36 -57.8(3) . . . . ?
C3C C2C C1C N1C -1.3(4) . . . . ?
C5C N1C C1C C2C 0.2(4) . . . . ?
C12C C7C C8C C9C 0.2(4) . . . . ?
C6C C7C C8C C9C 178.6(3) . . . . ?
C5B N1B C1B C2B -0.1(5) . . . . ?
C3B C2B C1B N1B 1.4(5) . . . . ?
C5B C4B C3B C2B -0.4(5) . . . . ?
C1B C2B C3B C4B -1.1(5) . . . . ?
C7C C8C C9C C10C -0.1(5) . . . . ?
C8B C7B C12B C11B 1.5(5) . . . . ?
C6B C7B C12B C11B -178.6(3) . . . . ?
C8B C7B C12B C13B -178.7(3) . . . . ?
C6B C7B C12B C13B 1.2(5) . . . . ?
C7C C12C C11C C10C 0.2(5) . . . . ?
C13C C12C C11C C10C -179.3(3) . . . . ?
C9B C10B C11B C12B -0.3(6) . . . . ?
C7B C12B C11B C10B -1.1(5) . . . . ?
C13B C12B C11B C10B 179.1(4) . . . . ?
C11B C10B C9B C8B 1.2(5) . . . . ?
C7B C8B C9B C10B -0.7(5) . . . . ?
C12C C11C C10C C9C -0.1(5) . . . . ?
C8C C9C C10C C11C 0.0(5) . . . . ?
O1B C15B C14B C13B -179.8(4) . . . . ?
C6B C15B C14B C13B 1.2(6) . . . . ?
C15B C14B C13B C12B -2.0(7) . . . . ?
C11B C12B C13B C14B -179.5(4) . . . . ?
C7B C12B C13B C14B 0.8(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.91
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.700
_refine_diff_density_min         -0.612
_refine_diff_density_rms         0.061

_database_code_depnum_ccdc_archive 'CCDC 1002498'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_3cp26c

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            
'C-ethylpyrogallol[4]arene with 1-(2-pyridylazo)-2-napthol'
_chemical_formula_moiety         'C36 H40 O12, 2(C15 H11 O1 N3), H2 O'
_chemical_formula_sum            'C66 H64 N6 O15'
_chemical_melting_point          ?

_exptl_crystal_description       prism
_exptl_crystal_colour            orange

_diffrn_ambient_temperature      173(2)
_chemical_formula_weight         1181.23

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'
O O 0.0106 0.0060 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?

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

_cell_length_a                   12.5764(16)
_cell_length_b                   15.566(2)
_cell_length_c                   16.818(2)
_cell_angle_alpha                65.345(2)
_cell_angle_beta                 82.005(2)
_cell_angle_gamma                68.245(2)
_cell_volume                     2778.6(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3580
_cell_measurement_theta_min      2.2
_cell_measurement_theta_max      22.3
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1244
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_process_details   
;
 Data were corrected for decay and absorption using the program SADABS 
 (Sheldrick, G. M. (2003). SADABS. Version 2.10. University of
 Göttingen, Germany).
;

_exptl_special_details           
; 
 ? 
;
_diffrn_radiation_probe          ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.0
_diffrn_reflns_number            29131
_diffrn_reflns_av_R_equivalents  0.0539
_diffrn_reflns_av_sigmaI/netI    0.0712
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.58
_diffrn_reflns_theta_max         25.75
_reflns_number_total             10579
_reflns_number_gt                6392
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2008)'
_computing_structure_solution    'SHELXS-1997 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-1997 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-SEED, Barbour, 2001'
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. There is  no bond between  
 C15 and H7.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0747P)²+0.4946P] where P=(Fo²+2Fc²)/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         10579
_refine_ls_number_parameters     813
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1061
_refine_ls_R_factor_gt           0.0586
_refine_ls_wR_factor_ref         0.1638
_refine_ls_wR_factor_gt          0.1405
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_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
O3 O 0.44833(15) 0.93069(14) 0.38979(12) 0.0249(4) Uani 1 1 d . . .
H3 H 0.3883 0.9570 0.3592 0.030 Uiso 1 1 calc R . .
O7 O 1.02238(16) 1.22189(14) 0.26962(12) 0.0291(5) Uani 1 1 d . . .
H7 H 1.0462 1.2330 0.2178 0.035 Uiso 1 1 d . . .
O9 O 1.30543(15) 0.91534(14) 0.27470(13) 0.0295(5) Uani 1 1 d . . .
H9 H 1.3026 0.8569 0.2999 0.035 Uiso 1 1 calc R . .
O2 O 0.52306(16) 0.72199(14) 0.44584(12) 0.0264(5) Uani 1 1 d . . .
H2 H 0.5285 0.7271 0.4928 0.032 Uiso 1 1 calc R . .
O4 O 0.54039(18) 1.05900(16) 0.41196(13) 0.0335(5) Uani 1 1 d . . .
H4 H 0.5114 1.0277 0.3962 0.040 Uiso 1 1 calc R . .
O1 O 0.71801(17) 0.62392(14) 0.37682(12) 0.0282(5) Uani 1 1 d . . .
H1 H 0.7070 0.6003 0.4309 0.034 Uiso 1 1 calc R . .
O10 O 1.21511(16) 0.76762(15) 0.35865(13) 0.0317(5) Uani 1 1 d . . .
H10 H 1.2254 0.7329 0.4127 0.038 Uiso 1 1 calc R . .
O8 O 1.24487(16) 1.07561(14) 0.30916(13) 0.0322(5) Uani 1 1 d . . .
H8 H 1.2436 1.1339 0.2886 0.039 Uiso 1 1 d . . .
O11 O 1.10294(17) 0.65066(16) 0.47359(12) 0.0324(5) Uani 1 1 d . . .
H11 H 1.0568 0.6229 0.5042 0.039 Uiso 1 1 calc R . .
O6 O 0.81340(17) 1.21292(16) 0.34697(13) 0.0346(5) Uani 1 1 d . . .
H6 H 0.8776 1.2049 0.3259 0.041 Uiso 1 1 d . . .
O12 O 0.92916(17) 0.62239(15) 0.42315(12) 0.0313(5) Uani 1 1 d . . .
H12 H 0.8818 0.6120 0.4009 0.038 Uiso 1 1 calc R . .
C2 C 0.5790(2) 0.7784(2) 0.38048(17) 0.0223(6) Uani 1 1 d . . .
O5 O 0.67311(18) 1.13375(16) 0.45495(13) 0.0354(5) Uani 1 1 d . . .
H5 H 0.6191 1.1148 0.4820 0.042 Uiso 1 1 calc R . .
C6 C 0.7323(2) 0.7813(2) 0.27612(17) 0.0208(6) Uani 1 1 d . . .
C24 C 0.9794(2) 0.6832(2) 0.35821(18) 0.0231(6) Uani 1 1 d . . .
C25 C 0.9451(2) 0.7336(2) 0.27043(17) 0.0217(6) Uani 1 1 d . . .
C16 C 1.1648(2) 1.0690(2) 0.26571(18) 0.0255(7) Uani 1 1 d . . .
C23 C 1.0697(2) 0.6945(2) 0.38747(18) 0.0246(6) Uani 1 1 d . . .
C3 C 0.5390(2) 0.8828(2) 0.34778(17) 0.0211(6) Uani 1 1 d . . .
C7 C 0.5450(2) 1.0544(2) 0.23786(18) 0.0241(6) Uani 1 1 d . . .
H7A H 0.4683 1.0755 0.2641 0.029 Uiso 1 1 calc R . .
C12 C 0.6994(2) 1.1345(2) 0.20828(18) 0.0239(6) Uani 1 1 d . . .
H12A H 0.7067 1.1347 0.1512 0.029 Uiso 1 1 calc R . .
C18 C 1.1224(2) 0.9713(2) 0.20266(17) 0.0231(6) Uani 1 1 d . . .
C9 C 0.6794(2) 1.1334(2) 0.37394(18) 0.0246(6) Uani 1 1 d . . .
C27 C 1.0955(2) 0.8074(2) 0.24123(18) 0.0227(6) Uani 1 1 d . . .
C15 C 1.0554(2) 1.1401(2) 0.24485(18) 0.0252(7) Uani 1 1 d . . .
C26 C 1.0051(2) 0.7951(2) 0.21367(18) 0.0247(6) Uani 1 1 d . . .
H26 H 0.9828 0.8299 0.1536 0.030 Uiso 1 1 calc R . .
C13 C 0.6201(2) 1.09605(19) 0.26432(18) 0.0217(6) Uani 1 1 d . . .
C1 C 0.6758(2) 0.7278(2) 0.34439(17) 0.0223(6) Uani 1 1 d . . .
C17 C 1.1970(2) 0.9838(2) 0.24724(18) 0.0239(6) Uani 1 1 d . . .
C19 C 1.0142(2) 1.0459(2) 0.18007(17) 0.0241(6) Uani 1 1 d . . .
H19 H 0.9620 1.0381 0.1501 0.029 Uiso 1 1 calc R . .
C8 C 0.6126(2) 1.0950(2) 0.34845(18) 0.0241(6) Uani 1 1 d . . .
C5 C 0.6886(2) 0.8858(2) 0.24429(17) 0.0212(6) Uani 1 1 d . . .
H5A H 0.7269 0.9228 0.1977 0.025 Uiso 1 1 calc R . .
C28 C 0.8416(2) 0.7255(2) 0.23969(17) 0.0235(6) Uani 1 1 d . . .
H28 H 0.8501 0.6526 0.2659 0.028 Uiso 1 1 calc R . .
C22 C 1.1273(2) 0.7557(2) 0.32959(18) 0.0239(6) Uani 1 1 d . . .
C21 C 1.1560(2) 0.8788(2) 0.18074(17) 0.0251(6) Uani 1 1 d . . .
H21 H 1.2399 0.8424 0.1936 0.030 Uiso 1 1 calc R . .
C20 C 0.9789(2) 1.1310(2) 0.19918(17) 0.0235(6) Uani 1 1 d . B .
C10 C 0.7556(2) 1.1729(2) 0.31543(19) 0.0259(7) Uani 1 1 d . . .
C4 C 0.5916(2) 0.9388(2) 0.27727(17) 0.0216(6) Uani 1 1 d . . .
C29 C 0.5251(2) 1.0964(2) 0.13857(18) 0.0278(7) Uani 1 1 d . . .
H29A H 0.4981 1.1709 0.1148 0.033 Uiso 1 1 calc R . .
H29B H 0.5988 1.0732 0.1108 0.033 Uiso 1 1 calc R . .
C14 C 0.8592(2) 1.2099(2) 0.17286(19) 0.0295(7) Uani 1 1 d . . .
H14 H 0.8593 1.2678 0.1846 0.035 Uiso 1 1 calc R A 1
C33 C 1.1380(3) 0.9080(2) 0.08346(19) 0.0323(7) Uani 1 1 d . . .
H33A H 1.1552 0.8462 0.0730 0.039 Uiso 1 1 calc R . .
H33B H 1.0567 0.9497 0.0670 0.039 Uiso 1 1 calc R . .
C11 C 0.7687(2) 1.1726(2) 0.23256(18) 0.0239(6) Uani 1 1 d . B .
C35 C 0.8340(2) 0.7613(2) 0.14057(18) 0.0290(7) Uani 1 1 d . . .
H35A H 0.8266 0.8333 0.1128 0.035 Uiso 1 1 calc R . .
H35B H 0.9058 0.7226 0.1201 0.035 Uiso 1 1 calc R . .
C36 C 0.7341(3) 0.7492(2) 0.1114(2) 0.0371(8) Uani 1 1 d . . .
H36A H 0.7396 0.6784 0.1399 0.056 Uiso 1 1 calc R . .
H36B H 0.7356 0.7700 0.0478 0.056 Uiso 1 1 calc R . .
H36C H 0.6623 0.7913 0.1275 0.056 Uiso 1 1 calc R . .
C30 C 0.4382(3) 1.0639(3) 0.1147(2) 0.0404(8) Uani 1 1 d . . .
H30A H 0.4629 0.9902 0.1401 0.061 Uiso 1 1 calc R . .
H30B H 0.4325 1.0890 0.0509 0.061 Uiso 1 1 calc R . .
H30C H 0.3633 1.0917 0.1377 0.061 Uiso 1 1 calc R . .
C31 C 0.8352(3) 1.2514(3) 0.0768(2) 0.0308(10) Uani 0.875(6) 1 d P B 1
H31A H 0.7564 1.3012 0.0637 0.037 Uiso 0.875(6) 1 calc PR B 1
H31B H 0.8391 1.1960 0.0607 0.037 Uiso 0.875(6) 1 calc PR B 1
C34 C 1.2133(3) 0.9662(3) 0.0259(2) 0.0463(9) Uani 1 1 d . . .
H34A H 1.1939 1.0292 0.0338 0.069 Uiso 1 1 calc R . .
H34B H 1.2007 0.9816 -0.0355 0.069 Uiso 1 1 calc R . .
H34C H 1.2939 0.9255 0.0423 0.069 Uiso 1 1 calc R . .
C32 C 0.9189(4) 1.3018(4) 0.0213(3) 0.0466(12) Uani 0.875(6) 1 d P B 1
H32A H 0.8996 1.3274 -0.0408 0.070 Uiso 0.875(6) 1 calc PR B 1
H32B H 0.9970 1.2526 0.0331 0.070 Uiso 0.875(6) 1 calc PR B 1
H32C H 0.9140 1.3579 0.0358 0.070 Uiso 0.875(6) 1 calc PR B 1
O1C O 0.41260(18) 0.27642(16) 0.41086(14) 0.0377(5) Uani 1 1 d . . .
O1B O 0.25117(18) 0.45545(15) 0.45154(13) 0.0363(5) Uani 1 1 d . . .
N2B N 0.1304(2) 0.48048(17) 0.32702(16) 0.0302(6) Uani 1 1 d . . .
H2B H 0.1433 0.4557 0.3837 0.036 Uiso 1 1 calc R . .
N3B N 0.1956(2) 0.52734(17) 0.27098(16) 0.0295(6) Uani 1 1 d . . .
N3C N 0.2494(2) 0.24584(17) 0.33480(15) 0.0287(6) Uani 1 1 d . . .
C4C C 0.0931(2) 0.16095(19) 0.43578(16) 0.0167(6) Uani 1 1 d . . .
H4C H 0.0866 0.1850 0.3740 0.020 Uiso 1 1 calc R . .
N2C N 0.2483(2) 0.21683(18) 0.42035(15) 0.0310(6) Uani 1 1 d . . .
H2C H 0.2974 0.2264 0.4455 0.037 Uiso 1 1 calc R . .
C6C C 0.3242(2) 0.2890(2) 0.28910(19) 0.0275(7) Uani 1 1 d . . .
C6B C 0.2767(2) 0.5423(2) 0.30041(19) 0.0282(7) Uani 1 1 d . . .
N1B N -0.0290(2) 0.43531(19) 0.35700(16) 0.0335(6) Uani 1 1 d . . .
C5C C 0.1714(3) 0.1711(2) 0.47263(19) 0.0292(7) Uani 1 1 d . . .
C5B C 0.0407(2) 0.4710(2) 0.29466(19) 0.0284(7) Uani 1 1 d . . .
C15B C 0.3038(3) 0.5058(2) 0.39346(19) 0.0312(7) Uani 1 1 d . . .
C7B C 0.3415(3) 0.5988(2) 0.2343(2) 0.0312(7) Uani 1 1 d . . .
C7C C 0.3179(2) 0.3252(2) 0.19404(18) 0.0279(7) Uani 1 1 d . . .
C14C C 0.4874(3) 0.3490(2) 0.2729(2) 0.0330(7) Uani 1 1 d . . .
H14C H 0.5443 0.3574 0.2978 0.040 Uiso 1 1 calc R . .
N1C N 0.1848(3) 0.1388(2) 0.5630(2) 0.0534(8) Uani 1 1 d . . .
C15C C 0.4091(3) 0.3038(2) 0.3289(2) 0.0300(7) Uani 1 1 d . . .
C13C C 0.4813(3) 0.3798(2) 0.1855(2) 0.0365(8) Uani 1 1 d . . .
H13C H 0.5352 0.4087 0.1504 0.044 Uiso 1 1 calc R . .
C12C C 0.3967(3) 0.3708(2) 0.1429(2) 0.0339(7) Uani 1 1 d . . .
C3C C 0.0238(3) 0.1154(2) 0.4890(2) 0.0381(8) Uani 1 1 d . . .
H3C H -0.0332 0.1079 0.4634 0.046 Uiso 1 1 calc R . .
C8B C 0.3220(3) 0.6340(2) 0.1444(2) 0.0359(8) Uani 1 1 d . . .
H8B H 0.2650 0.6208 0.1244 0.043 Uiso 1 1 calc R . .
C4B C 0.0277(3) 0.4948(2) 0.2068(2) 0.0348(8) Uani 1 1 d . . .
H4B H 0.0810 0.5175 0.1652 0.042 Uiso 1 1 calc R . .
C8C C 0.2349(3) 0.3189(2) 0.1511(2) 0.0355(8) Uani 1 1 d . . .
H8C H 0.1810 0.2888 0.1844 0.043 Uiso 1 1 calc R . .
C1B C -0.1188(3) 0.4264(2) 0.3300(2) 0.0371(8) Uani 1 1 d . . .
H1B1 H -0.1701 0.4020 0.3728 0.044 Uiso 1 1 calc R . .
C2C C 0.0299(3) 0.0788(2) 0.5786(2) 0.0350(8) Uani 1 1 d . . .
H13 H -0.0205 0.0456 0.6139 0.042 Uiso 1 1 calc R . .
C1C C 0.1109(3) 0.0913(2) 0.6163(2) 0.0331(7) Uani 1 1 d . . .
H1C1 H 0.1162 0.0676 0.6781 0.040 Uiso 1 1 calc R . .
C14B C 0.3931(3) 0.5283(2) 0.4161(2) 0.0416(8) Uani 1 1 d . . .
H14B H 0.4124 0.5052 0.4760 0.050 Uiso 1 1 calc R . .
C12B C 0.4275(3) 0.6185(2) 0.2627(2) 0.0376(8) Uani 1 1 d . . .
C2B C -0.1405(3) 0.4508(2) 0.2441(2) 0.0385(8) Uani 1 1 d . . .
H15 H -0.2059 0.4447 0.2278 0.046 Uiso 1 1 calc R . .
C9C C 0.2304(3) 0.3558(2) 0.0613(2) 0.0420(8) Uani 1 1 d . . .
H9C H 0.1736 0.3509 0.0333 0.050 Uiso 1 1 calc R . .
C10B C 0.4675(3) 0.7083(3) 0.1126(2) 0.0498(10) Uani 1 1 d . . .
H10B H 0.5094 0.7464 0.0709 0.060 Uiso 1 1 calc R . .
C3B C -0.0649(3) 0.4844(2) 0.1819(2) 0.0403(8) Uani 1 1 d . . .
H3B H -0.0768 0.5003 0.1221 0.048 Uiso 1 1 calc R . .
C13B C 0.4502(3) 0.5820(3) 0.3536(2) 0.0438(9) Uani 1 1 d . . .
H13B H 0.5084 0.5960 0.3712 0.053 Uiso 1 1 calc R . .
C11B C 0.4891(3) 0.6741(3) 0.2004(2) 0.0453(9) Uani 1 1 d . . .
H11B H 0.5464 0.6882 0.2190 0.054 Uiso 1 1 calc R . .
C11C C 0.3897(3) 0.4070(3) 0.0515(2) 0.0440(9) Uani 1 1 d . . .
H11C H 0.4428 0.4371 0.0168 0.053 Uiso 1 1 calc R . .
C10C C 0.3079(3) 0.3999(3) 0.0113(2) 0.0490(9) Uani 1 1 d . . .
H10C H 0.3042 0.4252 -0.0508 0.059 Uiso 1 1 calc R . .
C9B C 0.3849(3) 0.6876(3) 0.0847(2) 0.0439(9) Uani 1 1 d . . .
H9B H 0.3715 0.7105 0.0238 0.053 Uiso 1 1 calc R . .
O1D O 0.6960(2) 0.3037(2) 0.47957(17) 0.0453(6) Uani 1 1 d . . .
H16 H 0.744(5) 0.258(4) 0.449(3) 0.121(19) Uiso 1 1 d . . .
H17 H 0.639(6) 0.288(5) 0.503(4) 0.16(3) Uiso 1 1 d . . .
C31A C 0.8352(16) 1.3136(14) 0.1160(12) 0.013(5) Uiso 0.125(6) 1 d P B 2
H31C H 0.8263 1.3515 0.1527 0.015 Uiso 0.125(6) 1 calc PR B 2
H31D H 0.7602 1.3383 0.0867 0.015 Uiso 0.125(6) 1 calc PR B 2
C32A C 0.923(2) 1.341(2) 0.0439(19) 0.033(7) Uiso 0.125(6) 1 d P B 2
H32D H 0.8954 1.4141 0.0096 0.050 Uiso 0.125(6) 1 calc PR B 2
H32E H 0.9313 1.3062 0.0053 0.050 Uiso 0.125(6) 1 calc PR B 2
H32F H 0.9970 1.3204 0.0713 0.050 Uiso 0.125(6) 1 calc PR B 2


_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
O3 C3 1.393(3) . ?
O3 H3 0.8400 . ?
O7 C15 1.404(3) . ?
O7 H7 0.8482 . ?
O9 C17 1.377(3) . ?
O9 H9 0.8400 . ?
O2 C2 1.382(3) . ?
O2 H2 0.8400 . ?
O4 C8 1.374(3) . ?
O4 H4 0.8400 . ?
O1 C1 1.380(3) . ?
O1 H1 0.8400 . ?
O10 C22 1.368(3) . ?
O10 H10 0.8400 . ?
O8 C16 1.380(3) . ?
O8 H8 0.8205 . ?
O11 C23 1.367(3) . ?
O11 H11 0.8400 . ?
O6 C10 1.385(3) . ?
O6 H6 0.8215 . ?
O12 C24 1.370(3) . ?
O12 H12 0.8400 . ?
C2 C3 1.386(4) . ?
C2 C1 1.398(4) . ?
O5 C9 1.356(3) . ?
O5 H5 0.8400 . ?
C6 C5 1.388(4) . ?
C6 C1 1.390(4) . ?
C6 C28 1.531(4) . ?
C24 C23 1.392(4) . ?
C24 C25 1.393(4) . ?
C25 C26 1.403(4) . ?
C25 C28 1.530(4) . ?
C16 C15 1.386(4) . ?
C16 C17 1.388(4) . ?
C23 C22 1.386(4) . ?
C3 C4 1.397(4) . ?
C7 C13 1.523(4) . ?
C7 C4 1.534(4) . ?
C7 C29 1.537(4) . ?
C7 H7A 1.0000 . ?
C12 C13 1.397(4) . ?
C12 C11 1.402(4) . ?
C12 H12A 0.9500 . ?
C18 C17 1.391(4) . ?
C18 C19 1.395(4) . ?
C18 C21 1.528(4) . ?
C9 C8 1.390(4) . ?
C9 C10 1.390(4) . ?
C27 C26 1.388(4) . ?
C27 C22 1.395(4) . ?
C27 C21 1.522(4) . ?
C15 C20 1.390(4) . ?
C15 H7 1.2864 . ?
C26 H26 0.9500 . ?
C13 C8 1.399(4) . ?
C19 C20 1.391(4) . ?
C19 H19 0.9500 . ?
C5 C4 1.387(4) . ?
C5 H5A 0.9500 . ?
C28 C35 1.526(4) . ?
C28 H28 1.0000 . ?
C21 C33 1.530(4) . ?
C21 H21 1.0000 . ?
C20 C14 1.527(4) . ?
C10 C11 1.382(4) . ?
C29 C30 1.521(4) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C14 C31A 1.428(18) . ?
C14 C31 1.496(4) . ?
C14 C11 1.526(4) . ?
C14 H14 1.0000 . ?
C33 C34 1.518(4) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C35 C36 1.509(4) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.525(5) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
O1C C15C 1.264(3) . ?
O1B C15B 1.254(3) . ?
N2B N3B 1.322(3) . ?
N2B C5B 1.397(4) . ?
N2B H2B 0.8800 . ?
N3B C6B 1.324(4) . ?
N3C N2C 1.316(3) . ?
N3C C6C 1.329(4) . ?
C4C C5C 1.321(4) . ?
C4C C3C 1.332(4) . ?
C4C H4C 0.9500 . ?
N2C C5C 1.402(4) . ?
N2C H2C 0.8800 . ?
C6C C7C 1.459(4) . ?
C6C C15C 1.465(4) . ?
C6B C7B 1.461(4) . ?
C6B C15B 1.466(4) . ?
N1B C5B 1.340(4) . ?
N1B C1B 1.347(4) . ?
C5C N1C 1.400(4) . ?
C5B C4B 1.382(4) . ?
C15B C14B 1.432(4) . ?
C7B C8B 1.400(4) . ?
C7B C12B 1.415(4) . ?
C7C C8C 1.403(4) . ?
C7C C12C 1.414(4) . ?
C14C C13C 1.347(4) . ?
C14C C15C 1.434(4) . ?
C14C H14C 0.9500 . ?
N1C C1C 1.393(4) . ?
C13C C12C 1.439(4) . ?
C13C H13C 0.9500 . ?
C12C C11C 1.403(4) . ?
C3C C2C 1.373(4) . ?
C3C H3C 0.9500 . ?
C8B C9B 1.379(4) . ?
C8B H8B 0.9500 . ?
C4B C3B 1.375(4) . ?
C4B H4B 0.9500 . ?
C8C C9C 1.374(4) . ?
C8C H8C 0.9500 . ?
C1B C2B 1.372(4) . ?
C1B H1B1 0.9500 . ?
C2C C1C 1.381(4) . ?
C2C H13 0.9500 . ?
C1C H1C1 0.9500 . ?
C14B C13B 1.350(4) . ?
C14B H14B 0.9500 . ?
C12B C11B 1.401(4) . ?
C12B C13B 1.420(4) . ?
C2B C3B 1.381(4) . ?
C2B H15 0.9500 . ?
C9C C10C 1.384(5) . ?
C9C H9C 0.9500 . ?
C10B C11B 1.373(5) . ?
C10B C9B 1.383(5) . ?
C10B H10B 0.9500 . ?
C3B H3B 0.9500 . ?
C13B H13B 0.9500 . ?
C11B H11B 0.9500 . ?
C11C C10C 1.367(5) . ?
C11C H11C 0.9500 . ?
C10C H10C 0.9500 . ?
C9B H9B 0.9500 . ?
O1D H16 1.01(6) . ?
O1D H17 0.84(6) . ?
C31A C32A 1.55(3) . ?
C31A H31C 0.9900 . ?
C31A H31D 0.9900 . ?
C32A H32D 0.9800 . ?
C32A H32E 0.9800 . ?
C32A H32F 0.9800 . ?

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
C3 O3 H3 109.5 . . ?
C15 O7 H7 64.2 . . ?
C17 O9 H9 109.5 . . ?
C2 O2 H2 109.5 . . ?
C8 O4 H4 109.5 . . ?
C1 O1 H1 109.5 . . ?
C22 O10 H10 109.5 . . ?
C16 O8 H8 109.4 . . ?
C23 O11 H11 109.5 . . ?
C10 O6 H6 109.4 . . ?
C24 O12 H12 109.5 . . ?
O2 C2 C3 122.0(2) . . ?
O2 C2 C1 118.3(2) . . ?
C3 C2 C1 119.7(2) . . ?
C9 O5 H5 109.5 . . ?
C5 C6 C1 118.0(2) . . ?
C5 C6 C28 121.6(2) . . ?
C1 C6 C28 120.4(2) . . ?
O12 C24 C23 113.8(2) . . ?
O12 C24 C25 125.6(2) . . ?
C23 C24 C25 120.6(2) . . ?
C24 C25 C26 117.5(3) . . ?
C24 C25 C28 120.3(2) . . ?
C26 C25 C28 122.2(2) . . ?
O8 C16 C15 122.7(3) . . ?
O8 C16 C17 116.5(2) . . ?
C15 C16 C17 120.7(3) . . ?
O11 C23 C22 116.7(2) . . ?
O11 C23 C24 122.8(2) . . ?
C22 C23 C24 120.5(3) . . ?
C2 C3 O3 118.3(2) . . ?
C2 C3 C4 121.1(2) . . ?
O3 C3 C4 120.5(2) . . ?
C13 C7 C4 111.0(2) . . ?
C13 C7 C29 114.0(2) . . ?
C4 C7 C29 111.0(2) . . ?
C13 C7 H7A 106.8 . . ?
C4 C7 H7A 106.8 . . ?
C29 C7 H7A 106.8 . . ?
C13 C12 C11 122.9(3) . . ?
C13 C12 H12A 118.6 . . ?
C11 C12 H12A 118.6 . . ?
C17 C18 C19 117.2(3) . . ?
C17 C18 C21 121.6(2) . . ?
C19 C18 C21 121.1(2) . . ?
O5 C9 C8 122.0(2) . . ?
O5 C9 C10 118.2(3) . . ?
C8 C9 C10 119.8(3) . . ?
C26 C27 C22 117.8(2) . . ?
C26 C27 C21 123.0(2) . . ?
C22 C27 C21 119.2(2) . . ?
C16 C15 C20 120.4(3) . . ?
C16 C15 O7 119.6(3) . . ?
C20 C15 O7 120.0(2) . . ?
C16 C15 H7 116.9 . . ?
C20 C15 H7 110.2 . . ?
O7 C15 H7 36.4 . . ?
C27 C26 C25 123.1(3) . . ?
C27 C26 H26 118.5 . . ?
C25 C26 H26 118.5 . . ?
C12 C13 C8 117.3(3) . . ?
C12 C13 C7 122.8(3) . . ?
C8 C13 C7 119.9(2) . . ?
O1 C1 C6 118.8(2) . . ?
O1 C1 C2 120.6(2) . . ?
C6 C1 C2 120.6(2) . . ?
O9 C17 C16 116.2(2) . . ?
O9 C17 C18 123.3(3) . . ?
C16 C17 C18 120.5(2) . . ?
C20 C19 C18 123.5(3) . . ?
C20 C19 H19 118.3 . . ?
C18 C19 H19 118.3 . . ?
O4 C8 C9 114.1(2) . . ?
O4 C8 C13 124.9(3) . . ?
C9 C8 C13 121.0(2) . . ?
C4 C5 C6 123.2(3) . . ?
C4 C5 H5A 118.4 . . ?
C6 C5 H5A 118.4 . . ?
C35 C28 C25 113.4(2) . . ?
C35 C28 C6 111.9(2) . . ?
C25 C28 C6 109.4(2) . . ?
C35 C28 H28 107.3 . . ?
C25 C28 H28 107.3 . . ?
C6 C28 H28 107.3 . . ?
O10 C22 C23 120.4(2) . . ?
O10 C22 C27 118.9(2) . . ?
C23 C22 C27 120.7(3) . . ?
C27 C21 C18 109.9(2) . . ?
C27 C21 C33 113.8(2) . . ?
C18 C21 C33 111.9(2) . . ?
C27 C21 H21 106.9 . . ?
C18 C21 H21 106.9 . . ?
C33 C21 H21 106.9 . . ?
C15 C20 C19 117.5(3) . . ?
C15 C20 C14 121.5(3) . . ?
C19 C20 C14 121.0(3) . . ?
C11 C10 O6 124.2(2) . . ?
C11 C10 C9 121.4(3) . . ?
O6 C10 C9 114.4(3) . . ?
C5 C4 C3 117.4(2) . . ?
C5 C4 C7 121.0(2) . . ?
C3 C4 C7 121.6(2) . . ?
C30 C29 C7 112.8(2) . . ?
C30 C29 H29A 109.0 . . ?
C7 C29 H29A 109.0 . . ?
C30 C29 H29B 109.0 . . ?
C7 C29 H29B 109.0 . . ?
H29A C29 H29B 107.8 . . ?
C31A C14 C31 56.2(8) . . ?
C31A C14 C11 121.9(8) . . ?
C31 C14 C11 115.5(3) . . ?
C31A C14 C20 125.1(8) . . ?
C31 C14 C20 112.5(2) . . ?
C11 C14 C20 111.2(2) . . ?
C31A C14 H14 49.4 . . ?
C31 C14 H14 105.5 . . ?
C11 C14 H14 105.5 . . ?
C20 C14 H14 105.5 . . ?
C34 C33 C21 112.2(3) . . ?
C34 C33 H33A 109.2 . . ?
C21 C33 H33A 109.2 . . ?
C34 C33 H33B 109.2 . . ?
C21 C33 H33B 109.2 . . ?
H33A C33 H33B 107.9 . . ?
C10 C11 C12 117.6(2) . . ?
C10 C11 C14 119.5(3) . . ?
C12 C11 C14 122.8(3) . . ?
C36 C35 C28 112.9(2) . . ?
C36 C35 H35A 109.0 . . ?
C28 C35 H35A 109.0 . . ?
C36 C35 H35B 109.0 . . ?
C28 C35 H35B 109.0 . . ?
H35A C35 H35B 107.8 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C14 C31 C32 112.8(3) . . ?
C14 C31 H31A 109.0 . . ?
C32 C31 H31A 109.0 . . ?
C14 C31 H31B 109.0 . . ?
C32 C31 H31B 109.0 . . ?
H31A C31 H31B 107.8 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N3B N2B C5B 118.9(2) . . ?
N3B N2B H2B 120.6 . . ?
C5B N2B H2B 120.6 . . ?
N2B N3B C6B 119.8(3) . . ?
N2C N3C C6C 118.9(2) . . ?
C5C C4C C3C 117.1(3) . . ?
C5C C4C H4C 121.4 . . ?
C3C C4C H4C 121.4 . . ?
N3C N2C C5C 121.9(2) . . ?
N3C N2C H2C 119.0 . . ?
C5C N2C H2C 119.0 . . ?
N3C C6C C7C 117.0(3) . . ?
N3C C6C C15C 123.6(3) . . ?
C7C C6C C15C 119.4(3) . . ?
N3B C6B C7B 116.4(3) . . ?
N3B C6B C15B 123.9(3) . . ?
C7B C6B C15B 119.7(3) . . ?
C5B N1B C1B 116.5(3) . . ?
C4C C5C N1C 124.5(3) . . ?
C4C C5C N2C 120.0(3) . . ?
N1C C5C N2C 115.5(3) . . ?
N1B C5B C4B 124.1(3) . . ?
N1B C5B N2B 113.4(3) . . ?
C4B C5B N2B 122.5(3) . . ?
O1B C15B C14B 120.9(3) . . ?
O1B C15B C6B 121.1(3) . . ?
C14B C15B C6B 118.0(3) . . ?
C8B C7B C12B 118.8(3) . . ?
C8B C7B C6B 122.7(3) . . ?
C12B C7B C6B 118.4(3) . . ?
C8C C7C C12C 118.5(3) . . ?
C8C C7C C6C 122.6(3) . . ?
C12C C7C C6C 118.9(3) . . ?
C13C C14C C15C 120.8(3) . . ?
C13C C14C H14C 119.6 . . ?
C15C C14C H14C 119.6 . . ?
C1C N1C C5C 116.6(3) . . ?
O1C C15C C14C 121.3(3) . . ?
O1C C15C C6C 120.1(3) . . ?
C14C C15C C6C 118.6(3) . . ?
C14C C13C C12C 122.8(3) . . ?
C14C C13C H13C 118.6 . . ?
C12C C13C H13C 118.6 . . ?
C11C C12C C7C 119.0(3) . . ?
C11C C12C C13C 121.5(3) . . ?
C7C C12C C13C 119.5(3) . . ?
C4C C3C C2C 123.8(3) . . ?
C4C C3C H3C 118.1 . . ?
C2C C3C H3C 118.1 . . ?
C9B C8B C7B 120.5(3) . . ?
C9B C8B H8B 119.8 . . ?
C7B C8B H8B 119.8 . . ?
C3B C4B C5B 117.7(3) . . ?
C3B C4B H4B 121.2 . . ?
C5B C4B H4B 121.2 . . ?
C9C C8C C7C 120.8(3) . . ?
C9C C8C H8C 119.6 . . ?
C7C C8C H8C 119.6 . . ?
N1B C1B C2B 123.6(3) . . ?
N1B C1B H1B1 118.2 . . ?
C2B C1B H1B1 118.2 . . ?
C3C C2C C1C 118.5(3) . . ?
C3C C2C H13 120.7 . . ?
C1C C2C H13 120.7 . . ?
C2C C1C N1C 119.4(3) . . ?
C2C C1C H1C1 120.3 . . ?
N1C C1C H1C1 120.3 . . ?
C13B C14B C15B 120.9(3) . . ?
C13B C14B H14B 119.5 . . ?
C15B C14B H14B 119.5 . . ?
C11B C12B C7B 119.3(3) . . ?
C11B C12B C13B 120.8(3) . . ?
C7B C12B C13B 119.8(3) . . ?
C1B C2B C3B 118.3(3) . . ?
C1B C2B H15 120.8 . . ?
C3B C2B H15 120.8 . . ?
C8C C9C C10C 120.7(3) . . ?
C8C C9C H9C 119.6 . . ?
C10C C9C H9C 119.6 . . ?
C11B C10B C9B 120.2(3) . . ?
C11B C10B H10B 119.9 . . ?
C9B C10B H10B 119.9 . . ?
C4B C3B C2B 119.8(3) . . ?
C4B C3B H3B 120.1 . . ?
C2B C3B H3B 120.1 . . ?
C14B C13B C12B 123.1(3) . . ?
C14B C13B H13B 118.5 . . ?
C12B C13B H13B 118.5 . . ?
C10B C11B C12B 120.5(3) . . ?
C10B C11B H11B 119.7 . . ?
C12B C11B H11B 119.7 . . ?
C10C C11C C12C 121.4(3) . . ?
C10C C11C H11C 119.3 . . ?
C12C C11C H11C 119.3 . . ?
C11C C10C C9C 119.7(3) . . ?
C11C C10C H10C 120.2 . . ?
C9C C10C H10C 120.2 . . ?
C8B C9B C10B 120.6(3) . . ?
C8B C9B H9B 119.7 . . ?
C10B C9B H9B 119.7 . . ?
H16 O1D H17 111(5) . . ?
C14 C31A C32A 118.1(16) . . ?
C14 C31A H31C 107.8 . . ?
C32A C31A H31C 107.8 . . ?
C14 C31A H31D 107.8 . . ?
C32A C31A H31D 107.8 . . ?
H31C C31A H31D 107.1 . . ?
C31A C32A H32D 109.5 . . ?
C31A C32A H32E 109.5 . . ?
H32D C32A H32E 109.5 . . ?
C31A C32A H32F 109.5 . . ?
H32D C32A H32F 109.5 . . ?
H32E C32A H32F 109.5 . . ?

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
O12 C24 C25 C26 178.2(2) . . . . ?
C23 C24 C25 C26 0.2(4) . . . . ?
O12 C24 C25 C28 1.4(4) . . . . ?
C23 C24 C25 C28 -176.6(2) . . . . ?
O12 C24 C23 O11 -1.6(4) . . . . ?
C25 C24 C23 O11 176.7(2) . . . . ?
O12 C24 C23 C22 -178.6(2) . . . . ?
C25 C24 C23 C22 -0.3(4) . . . . ?
O2 C2 C3 O3 8.1(4) . . . . ?
C1 C2 C3 O3 -174.7(2) . . . . ?
O2 C2 C3 C4 -175.1(2) . . . . ?
C1 C2 C3 C4 2.1(4) . . . . ?
O8 C16 C15 C20 178.5(2) . . . . ?
C17 C16 C15 C20 -4.8(4) . . . . ?
O8 C16 C15 O7 -1.1(4) . . . . ?
C17 C16 C15 O7 175.6(2) . . . . ?
C22 C27 C26 C25 0.1(4) . . . . ?
C21 C27 C26 C25 -176.3(2) . . . . ?
C24 C25 C26 C27 -0.1(4) . . . . ?
C28 C25 C26 C27 176.7(2) . . . . ?
C11 C12 C13 C8 -1.1(4) . . . . ?
C11 C12 C13 C7 -179.9(2) . . . . ?
C4 C7 C13 C12 101.9(3) . . . . ?
C29 C7 C13 C12 -24.3(4) . . . . ?
C4 C7 C13 C8 -76.9(3) . . . . ?
C29 C7 C13 C8 156.9(2) . . . . ?
C5 C6 C1 O1 180.0(2) . . . . ?
C28 C6 C1 O1 -1.9(4) . . . . ?
C5 C6 C1 C2 -1.1(4) . . . . ?
C28 C6 C1 C2 177.1(2) . . . . ?
O2 C2 C1 O1 -3.7(4) . . . . ?
C3 C2 C1 O1 179.0(2) . . . . ?
O2 C2 C1 C6 177.4(2) . . . . ?
C3 C2 C1 C6 0.1(4) . . . . ?
O8 C16 C17 O9 0.2(4) . . . . ?
C15 C16 C17 O9 -176.7(2) . . . . ?
O8 C16 C17 C18 -179.2(2) . . . . ?
C15 C16 C17 C18 3.9(4) . . . . ?
C19 C18 C17 O9 178.9(2) . . . . ?
C21 C18 C17 O9 0.1(4) . . . . ?
C19 C18 C17 C16 -1.7(4) . . . . ?
C21 C18 C17 C16 179.5(2) . . . . ?
C17 C18 C19 C20 0.6(4) . . . . ?
C21 C18 C19 C20 179.4(2) . . . . ?
O5 C9 C8 O4 0.6(4) . . . . ?
C10 C9 C8 O4 -179.6(2) . . . . ?
O5 C9 C8 C13 179.6(3) . . . . ?
C10 C9 C8 C13 -0.5(4) . . . . ?
C12 C13 C8 O4 -179.3(2) . . . . ?
C7 C13 C8 O4 -0.4(4) . . . . ?
C12 C13 C8 C9 1.8(4) . . . . ?
C7 C13 C8 C9 -179.4(2) . . . . ?
C1 C6 C5 C4 -0.1(4) . . . . ?
C28 C6 C5 C4 -178.2(2) . . . . ?
C24 C25 C28 C35 -165.0(2) . . . . ?
C26 C25 C28 C35 18.3(4) . . . . ?
C24 C25 C28 C6 69.3(3) . . . . ?
C26 C25 C28 C6 -107.4(3) . . . . ?
C5 C6 C28 C35 -54.5(3) . . . . ?
C1 C6 C28 C35 127.4(3) . . . . ?
C5 C6 C28 C25 72.0(3) . . . . ?
C1 C6 C28 C25 -106.0(3) . . . . ?
O11 C23 C22 O10 2.0(4) . . . . ?
C24 C23 C22 O10 179.2(3) . . . . ?
O11 C23 C22 C27 -176.8(2) . . . . ?
C24 C23 C22 C27 0.3(4) . . . . ?
C26 C27 C22 O10 -179.1(2) . . . . ?
C21 C27 C22 O10 -2.5(4) . . . . ?
C26 C27 C22 C23 -0.2(4) . . . . ?
C21 C27 C22 C23 176.3(2) . . . . ?
C26 C27 C21 C18 107.0(3) . . . . ?
C22 C27 C21 C18 -69.4(3) . . . . ?
C26 C27 C21 C33 -19.5(4) . . . . ?
C22 C27 C21 C33 164.1(3) . . . . ?
C17 C18 C21 C27 105.1(3) . . . . ?
C19 C18 C21 C27 -73.6(3) . . . . ?
C17 C18 C21 C33 -127.3(3) . . . . ?
C19 C18 C21 C33 53.9(3) . . . . ?
C16 C15 C20 C19 3.5(4) . . . . ?
O7 C15 C20 C19 -176.9(2) . . . . ?
C16 C15 C20 C14 -178.1(2) . . . . ?
O7 C15 C20 C14 1.5(4) . . . . ?
C18 C19 C20 C15 -1.4(4) . . . . ?
C18 C19 C20 C14 -179.9(2) . . . . ?
O5 C9 C10 C11 178.3(3) . . . . ?
C8 C9 C10 C11 -1.6(4) . . . . ?
O5 C9 C10 O6 -2.9(4) . . . . ?
C8 C9 C10 O6 177.2(2) . . . . ?
C6 C5 C4 C3 2.1(4) . . . . ?
C6 C5 C4 C7 -178.2(2) . . . . ?
C2 C3 C4 C5 -3.1(4) . . . . ?
O3 C3 C4 C5 173.6(2) . . . . ?
C2 C3 C4 C7 177.2(2) . . . . ?
O3 C3 C4 C7 -6.1(4) . . . . ?
C13 C7 C4 C5 -74.1(3) . . . . ?
C29 C7 C4 C5 53.8(3) . . . . ?
C13 C7 C4 C3 105.6(3) . . . . ?
C29 C7 C4 C3 -126.6(3) . . . . ?
C13 C7 C29 C30 -172.8(2) . . . . ?
C4 C7 C29 C30 61.0(3) . . . . ?
C15 C20 C14 C31A 61.7(10) . . . . ?
C19 C20 C14 C31A -119.9(10) . . . . ?
C15 C20 C14 C31 125.3(3) . . . . ?
C19 C20 C14 C31 -56.3(3) . . . . ?
C15 C20 C14 C11 -103.2(3) . . . . ?
C19 C20 C14 C11 75.1(3) . . . . ?
C27 C21 C33 C34 -171.5(2) . . . . ?
C18 C21 C33 C34 63.1(3) . . . . ?
O6 C10 C11 C12 -176.4(2) . . . . ?
C9 C10 C11 C12 2.2(4) . . . . ?
O6 C10 C11 C14 5.6(4) . . . . ?
C9 C10 C11 C14 -175.7(3) . . . . ?
C13 C12 C11 C10 -0.9(4) . . . . ?
C13 C12 C11 C14 177.0(2) . . . . ?
C31A C14 C11 C10 -88.6(10) . . . . ?
C31 C14 C11 C10 -153.2(3) . . . . ?
C20 C14 C11 C10 76.9(3) . . . . ?
C31A C14 C11 C12 93.6(10) . . . . ?
C31 C14 C11 C12 29.0(4) . . . . ?
C20 C14 C11 C12 -100.9(3) . . . . ?
C25 C28 C35 C36 177.8(2) . . . . ?
C6 C28 C35 C36 -57.9(3) . . . . ?
C31A C14 C31 C32 58.5(9) . . . . ?
C11 C14 C31 C32 171.2(3) . . . . ?
C20 C14 C31 C32 -59.6(4) . . . . ?
C5B N2B N3B C6B 176.0(2) . . . . ?
C6C N3C N2C C5C 179.8(3) . . . . ?
N2C N3C C6C C7C -176.6(2) . . . . ?
N2C N3C C6C C15C 1.9(4) . . . . ?
N2B N3B C6B C7B -177.2(2) . . . . ?
N2B N3B C6B C15B 2.9(4) . . . . ?
C3C C4C C5C N1C -1.0(4) . . . . ?
C3C C4C C5C N2C 178.9(3) . . . . ?
N3C N2C C5C C4C -3.6(4) . . . . ?
N3C N2C C5C N1C 176.3(2) . . . . ?
C1B N1B C5B C4B -2.6(4) . . . . ?
C1B N1B C5B N2B 178.6(2) . . . . ?
N3B N2B C5B N1B -171.1(2) . . . . ?
N3B N2B C5B C4B 10.1(4) . . . . ?
N3B C6B C15B O1B 1.3(4) . . . . ?
C7B C6B C15B O1B -178.6(3) . . . . ?
N3B C6B C15B C14B -179.4(3) . . . . ?
C7B C6B C15B C14B 0.8(4) . . . . ?
N3B C6B C7B C8B -1.3(4) . . . . ?
C15B C6B C7B C8B 178.6(3) . . . . ?
N3B C6B C7B C12B 178.6(3) . . . . ?
C15B C6B C7B C12B -1.5(4) . . . . ?
N3C C6C C7C C8C 2.2(4) . . . . ?
C15C C6C C7C C8C -176.3(3) . . . . ?
N3C C6C C7C C12C -179.4(3) . . . . ?
C15C C6C C7C C12C 2.0(4) . . . . ?
C4C C5C N1C C1C 1.2(4) . . . . ?
N2C C5C N1C C1C -178.7(3) . . . . ?
C13C C14C C15C O1C -178.6(3) . . . . ?
C13C C14C C15C C6C 1.7(4) . . . . ?
N3C C6C C15C O1C -1.3(4) . . . . ?
C7C C6C C15C O1C 177.2(3) . . . . ?
N3C C6C C15C C14C 178.4(3) . . . . ?
C7C C6C C15C C14C -3.1(4) . . . . ?
C15C C14C C13C C12C 0.8(5) . . . . ?
C8C C7C C12C C11C -0.6(4) . . . . ?
C6C C7C C12C C11C -179.0(3) . . . . ?
C8C C7C C12C C13C 178.9(3) . . . . ?
C6C C7C C12C C13C 0.4(4) . . . . ?
C14C C13C C12C C11C 177.5(3) . . . . ?
C14C C13C C12C C7C -1.9(5) . . . . ?
C5C C4C C3C C2C -0.3(5) . . . . ?
C12B C7B C8B C9B -0.5(5) . . . . ?
C6B C7B C8B C9B 179.5(3) . . . . ?
N1B C5B C4B C3B 2.5(5) . . . . ?
N2B C5B C4B C3B -178.8(3) . . . . ?
C12C C7C C8C C9C 0.3(4) . . . . ?
C6C C7C C8C C9C 178.7(3) . . . . ?
C5B N1B C1B C2B 0.6(5) . . . . ?
C4C C3C C2C C1C 1.3(5) . . . . ?
C3C C2C C1C N1C -1.0(4) . . . . ?
C5C N1C C1C C2C -0.2(4) . . . . ?
O1B C15B C14B C13B 179.6(3) . . . . ?
C6B C15B C14B C13B 0.3(5) . . . . ?
C8B C7B C12B C11B 1.1(5) . . . . ?
C6B C7B C12B C11B -178.9(3) . . . . ?
C8B C7B C12B C13B -178.8(3) . . . . ?
C6B C7B C12B C13B 1.2(4) . . . . ?
N1B C1B C2B C3B 1.3(5) . . . . ?
C7C C8C C9C C10C 0.0(5) . . . . ?
C5B C4B C3B C2B -0.3(5) . . . . ?
C1B C2B C3B C4B -1.5(5) . . . . ?
C15B C14B C13B C12B -0.6(5) . . . . ?
C11B C12B C13B C14B 179.9(3) . . . . ?
C7B C12B C13B C14B -0.2(5) . . . . ?
C9B C10B C11B C12B -0.5(6) . . . . ?
C7B C12B C11B C10B -0.6(5) . . . . ?
C13B C12B C11B C10B 179.3(3) . . . . ?
C7C C12C C11C C10C 0.6(5) . . . . ?
C13C C12C C11C C10C -178.8(3) . . . . ?
C12C C11C C10C C9C -0.3(5) . . . . ?
C8C C9C C10C C11C 0.0(5) . . . . ?
C7B C8B C9B C10B -0.6(5) . . . . ?
C11B C10B C9B C8B 1.1(6) . . . . ?
C31 C14 C31A C32A -65.9(17) . . . . ?
C11 C14 C31A C32A -167.1(15) . . . . ?
C20 C14 C31A C32A 29(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.75
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.058

_database_code_depnum_ccdc_archive 'CCDC 1002499'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_3cp26e

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            
'C-ethylpyrogallol[4]arene with 1-(2-pyridylazo)-2-napthol'
_chemical_formula_moiety         'C36 H40 O12, C15 H11 O1 N3'
_chemical_formula_sum            'C51 H51 N3 O13'
_chemical_melting_point          ?

_exptl_crystal_description       plate
_exptl_crystal_colour            orange

_diffrn_ambient_temperature      173(2)
_chemical_formula_weight         913.95

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'
O O 0.0106 0.0060 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_int_tables_number      14
_chemical_absolute_configuration ?

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                   15.986(3)
_cell_length_b                   13.950(3)
_cell_length_c                   19.675(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.924(3)
_cell_angle_gamma                90.00
_cell_volume                     4322.2(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    5454
_cell_measurement_theta_min      2.3
_cell_measurement_theta_max      22.9
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1928
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_process_details   
;
 Data were corrected for decay and absorption using the program SADABS 
 (Sheldrick, G. M. (2003). SADABS. Version 2.10. University of
 Göttingen, Germany).
;

_exptl_special_details           
; 
 ? 
;
_diffrn_radiation_probe          ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.0
_diffrn_reflns_number            37272
_diffrn_reflns_av_R_equivalents  0.0629
_diffrn_reflns_av_sigmaI/netI    0.0472
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.80
_diffrn_reflns_theta_max         23.92
_reflns_number_total             6713
_reflns_number_gt                4451
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2008)'
_computing_structure_solution    'SHELXS-1997 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-1997 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-SEED, Barbour, 2001'
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0484P)²+6.1345P] where P=(Fo²+2Fc²)/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         6713
_refine_ls_number_parameters     617
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0485
_refine_ls_wR_factor_ref         0.1349
_refine_ls_wR_factor_gt          0.1104
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.020
_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
O6 O 0.07196(13) 0.32441(16) 0.16695(10) 0.0277(5) Uani 1 1 d . . .
H6 H 0.0871 0.3711 0.1450 0.033 Uiso 1 1 calc R . .
O12 O 0.17208(14) 0.67956(16) 0.55403(10) 0.0302(5) Uani 1 1 d . . .
H12 H 0.1995 0.6393 0.5808 0.036 Uiso 1 1 calc R . .
O9 O 0.16130(13) 0.80040(15) 0.20001(11) 0.0292(5) Uani 1 1 d . . .
H9 H 0.1098 0.8075 0.1965 0.035 Uiso 1 1 d . . .
O10 O 0.12939(13) 0.79706(15) 0.33045(11) 0.0290(5) Uani 1 1 d . . .
H10 H 0.1541 0.8148 0.2982 0.035 Uiso 1 1 d . . .
O8 O 0.06448(13) 0.68101(16) 0.09979(10) 0.0292(5) Uani 1 1 d . . .
H8 H 0.0817 0.7100 0.0674 0.035 Uiso 1 1 calc R . .
O1 O 0.22584(14) 0.52873(15) 0.63733(10) 0.0289(5) Uani 1 1 d . . .
H1 H 0.2120 0.5003 0.6705 0.035 Uiso 1 1 d . . .
O7 O 0.10463(14) 0.48900(16) 0.09723(11) 0.0304(5) Uani 1 1 d . . .
H7 H 0.0577 0.5151 0.0824 0.036 Uiso 1 1 calc R . .
O2 O 0.14638(15) 0.35523(16) 0.63066(11) 0.0329(6) Uani 1 1 d . . .
H2 H 0.1215 0.3027 0.6209 0.039 Uiso 1 1 calc R . .
O3 O 0.16687(15) 0.22371(15) 0.53396(11) 0.0305(5) Uani 1 1 d . . .
H3 H 0.1450 0.2081 0.4936 0.037 Uiso 1 1 calc R . .
O4 O 0.10624(14) 0.20750(16) 0.39598(11) 0.0297(5) Uani 1 1 d . . .
H4 H 0.0537 0.2009 0.3830 0.036 Uiso 1 1 calc R . .
O5 O 0.00961(13) 0.23654(17) 0.27046(11) 0.0311(6) Uani 1 1 d . . .
H5 H -0.0148 0.2520 0.2307 0.037 Uiso 1 1 calc R . .
O11 O 0.08107(14) 0.77137(17) 0.45284(11) 0.0359(6) Uani 1 1 d . . .
H11 H 0.0582 0.8029 0.4182 0.043 Uiso 1 1 calc R . .
C48 C -0.04750(18) 0.4573(2) 0.34832(14) 0.0198(7) Uani 1 1 d . . .
H48 H -0.1049 0.4362 0.3397 0.024 Uiso 1 1 calc R . .
C12 C 0.2574(2) 0.3305(2) 0.30764(15) 0.0236(7) Uani 1 1 d . . .
H13 H 0.3147 0.3518 0.3167 0.028 Uiso 1 1 calc R . .
N2 N -0.06154(17) 0.5081(2) 0.23334(14) 0.0330(7) Uani 1 1 d D . .
H15 H -0.0364 0.5138 0.1971 0.040 Uiso 1 1 calc R . .
C23 C 0.1578(2) 0.7367(2) 0.44179(16) 0.0251(7) Uani 1 1 d . . .
C2 C 0.1981(2) 0.3744(2) 0.58367(15) 0.0247(7) Uani 1 1 d . . .
C13 C 0.2252(2) 0.2826(2) 0.35998(15) 0.0227(7) Uani 1 1 d . . .
C9 C 0.09182(19) 0.2690(2) 0.28077(15) 0.0236(7) Uani 1 1 d . . .
C10 C 0.12600(19) 0.3162(2) 0.23018(15) 0.0231(7) Uani 1 1 d . . .
C14 C 0.2443(2) 0.4046(2) 0.18666(16) 0.0262(7) Uani 1 1 d . . .
H14 H 0.2137 0.3800 0.1414 0.031 Uiso 1 1 calc R . .
C5 C 0.30196(19) 0.4208(2) 0.49081(15) 0.0231(7) Uani 1 1 d . . .
H16 H 0.3371 0.4374 0.4583 0.028 Uiso 1 1 calc R . .
C16 C 0.1339(2) 0.6458(2) 0.14582(15) 0.0255(7) Uani 1 1 d . . .
C17 C 0.1794(2) 0.7047(2) 0.19586(15) 0.0250(7) Uani 1 1 d . . .
C18 C 0.2452(2) 0.6679(2) 0.24451(15) 0.0248(7) Uani 1 1 d . . .
C27 C 0.2653(2) 0.7152(2) 0.36975(15) 0.0237(7) Uani 1 1 d . . .
C24 C 0.2072(2) 0.6869(2) 0.49493(15) 0.0246(7) Uani 1 1 d . . .
N1 N -0.14507(17) 0.50998(19) 0.22545(14) 0.0307(7) Uani 1 1 d D . .
C37 C -0.1889(2) 0.5085(2) 0.16131(17) 0.0310(8) Uani 1 1 d D . .
C6 C 0.29190(19) 0.4870(2) 0.54165(15) 0.0233(7) Uani 1 1 d . . .
C11 C 0.20935(19) 0.3487(2) 0.24282(15) 0.0225(7) Uani 1 1 d . . .
C7 C 0.2785(2) 0.2597(2) 0.43001(15) 0.0249(7) Uani 1 1 d . . .
H18 H 0.2581 0.1962 0.4442 0.030 Uiso 1 1 calc R . .
C8 C 0.1406(2) 0.2538(2) 0.34533(15) 0.0243(7) Uani 1 1 d . . .
C1 C 0.2390(2) 0.4625(2) 0.58807(15) 0.0238(7) Uani 1 1 d . . .
C26 C 0.31311(19) 0.6651(2) 0.42481(16) 0.0245(7) Uani 1 1 d . . .
H26 H 0.3671 0.6409 0.4193 0.029 Uiso 1 1 calc R . .
C20 C 0.2211(2) 0.5101(2) 0.19005(15) 0.0250(7) Uani 1 1 d . . .
C51 C 0.1211(2) 0.5148(2) 0.37285(17) 0.0311(8) Uani 1 1 d . . .
H51 H 0.1792 0.5328 0.3814 0.037 Uiso 1 1 calc R . .
C19 C 0.2649(2) 0.5714(2) 0.23973(16) 0.0260(7) Uani 1 1 d . . .
H19 H 0.3106 0.5459 0.2720 0.031 Uiso 1 1 calc R . .
O13 O -0.07134(17) 0.49516(18) 0.10222(12) 0.0441(7) Uani 1 1 d . . .
C21 C 0.2944(2) 0.7328(2) 0.30090(16) 0.0282(8) Uani 1 1 d . . .
H21 H 0.2773 0.8000 0.2873 0.034 Uiso 1 1 calc R . .
C28 C 0.33402(19) 0.5859(2) 0.54447(16) 0.0256(7) Uani 1 1 d . . .
H28 H 0.3258 0.6156 0.5891 0.031 Uiso 1 1 calc R . .
N3 N 0.0724(2) 0.5273(2) 0.30770(18) 0.0553(9) Uani 1 1 d D . .
C25 C 0.28564(19) 0.6488(2) 0.48729(15) 0.0232(7) Uani 1 1 d . . .
C22 C 0.1862(2) 0.7493(2) 0.37963(15) 0.0234(7) Uani 1 1 d . . .
C50 C 0.0842(2) 0.4760(2) 0.42486(18) 0.0355(9) Uani 1 1 d . . .
H50 H 0.1158 0.4688 0.4701 0.043 Uiso 1 1 calc R . .
C4 C 0.26294(19) 0.3314(2) 0.48554(15) 0.0221(7) Uani 1 1 d . . .
C29 C 0.3733(2) 0.2472(2) 0.42785(16) 0.0290(8) Uani 1 1 d . . .
H29A H 0.3800 0.2002 0.3915 0.035 Uiso 1 1 calc R . .
H29B H 0.3967 0.3091 0.4154 0.035 Uiso 1 1 calc R . .
C38 C -0.1504(3) 0.4933(2) 0.10013(17) 0.0364(9) Uani 1 1 d . . .
C31 C 0.3390(2) 0.3896(2) 0.18672(18) 0.0324(8) Uani 1 1 d . . .
H31A H 0.3562 0.4296 0.1499 0.039 Uiso 1 1 calc R . .
H31B H 0.3713 0.4119 0.2314 0.039 Uiso 1 1 calc R . .
C47 C -0.0125(2) 0.4970(2) 0.29947(17) 0.0317(8) Uani 1 1 d D . .
C41 C -0.3314(3) 0.4857(3) 0.0927(2) 0.0470(10) Uani 1 1 d . . .
C35 C 0.4289(2) 0.5807(2) 0.54622(17) 0.0321(8) Uani 1 1 d . . .
H35A H 0.4519 0.6466 0.5465 0.039 Uiso 1 1 calc R . .
H35B H 0.4400 0.5485 0.5038 0.039 Uiso 1 1 calc R . .
C15 C 0.1532(2) 0.5493(2) 0.14426(15) 0.0250(7) Uani 1 1 d . . .
C3 C 0.20955(19) 0.3093(2) 0.53257(15) 0.0238(7) Uani 1 1 d . . .
C30 C 0.4238(2) 0.2131(3) 0.49633(18) 0.0392(9) Uani 1 1 d . . .
H30A H 0.4229 0.2627 0.5314 0.059 Uiso 1 1 calc R . .
H30B H 0.4825 0.2003 0.4910 0.059 Uiso 1 1 calc R . .
H30C H 0.3983 0.1542 0.5107 0.059 Uiso 1 1 calc R . .
C36 C 0.4751(2) 0.5266(3) 0.60918(18) 0.0401(9) Uani 1 1 d . . .
H36A H 0.4628 0.5568 0.6513 0.060 Uiso 1 1 calc R . .
H36B H 0.5364 0.5283 0.6093 0.060 Uiso 1 1 calc R . .
H36C H 0.4557 0.4598 0.6073 0.060 Uiso 1 1 calc R . .
C32 C 0.3625(2) 0.2863(3) 0.17555(19) 0.0426(9) Uani 1 1 d . . .
H32A H 0.3517 0.2473 0.2145 0.064 Uiso 1 1 calc R . .
H32B H 0.4229 0.2825 0.1721 0.064 Uiso 1 1 calc R . .
H32C H 0.3282 0.2623 0.1328 0.064 Uiso 1 1 calc R . .
C39 C -0.2074(3) 0.4709(3) 0.03651(19) 0.0483(11) Uani 1 1 d . . .
H39 H -0.1847 0.4604 -0.0045 0.058 Uiso 1 1 calc R . .
C46 C -0.2806(2) 0.5119(3) 0.15555(18) 0.0369(9) Uani 1 1 d D . .
C49 C 0.0004(2) 0.4479(3) 0.40995(19) 0.0399(9) Uani 1 1 d . . .
H49 H -0.0244 0.4202 0.4459 0.048 Uiso 1 1 calc R . .
C33 C 0.3892(2) 0.7276(3) 0.30220(18) 0.0382(9) Uani 1 1 d . . .
H33A H 0.4087 0.6607 0.3110 0.046 Uiso 1 1 calc R . .
H33B H 0.4188 0.7681 0.3401 0.046 Uiso 1 1 calc R . .
C34 C 0.4115(2) 0.7619(3) 0.23306(19) 0.0536(11) Uani 1 1 d . . .
H34A H 0.3838 0.7203 0.1957 0.080 Uiso 1 1 calc R . .
H34B H 0.4732 0.7593 0.2353 0.080 Uiso 1 1 calc R . .
H34C H 0.3918 0.8280 0.2242 0.080 Uiso 1 1 calc R . .
C45 C -0.3206(2) 0.5400(3) 0.2106(2) 0.0513(11) Uani 1 1 d . . .
H45 H -0.2868 0.5599 0.2528 0.062 Uiso 1 1 calc R . .
C42 C -0.4200(3) 0.4833(3) 0.0880(3) 0.0665(14) Uani 1 1 d . . .
H42 H -0.4543 0.4632 0.0462 0.080 Uiso 1 1 calc R . .
C40 C -0.2913(3) 0.4647(3) 0.0345(2) 0.0530(11) Uani 1 1 d . . .
H40 H -0.3260 0.4454 -0.0074 0.064 Uiso 1 1 calc R . .
C43 C -0.4578(3) 0.5094(4) 0.1426(3) 0.0745(16) Uani 1 1 d . . .
H43 H -0.5179 0.5073 0.1385 0.089 Uiso 1 1 calc R . .
C44 C -0.4076(3) 0.5393(4) 0.2047(2) 0.0674(14) Uani 1 1 d . . .
H44 H -0.4335 0.5589 0.2424 0.081 Uiso 1 1 calc R . .


_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
O6 C10 1.392(4) . ?
O6 H6 0.8400 . ?
O12 C24 1.380(3) . ?
O12 H12 0.8400 . ?
O9 C17 1.371(4) . ?
O9 H9 0.8201 . ?
O10 C22 1.379(4) . ?
O10 H10 0.8401 . ?
O8 C16 1.395(4) . ?
O8 H8 0.8400 . ?
O1 C1 1.381(4) . ?
O1 H1 0.8248 . ?
O7 C15 1.385(4) . ?
O7 H7 0.8400 . ?
O2 C2 1.368(4) . ?
O2 H2 0.8400 . ?
O3 C3 1.378(4) . ?
O3 H3 0.8400 . ?
O4 C8 1.379(4) . ?
O4 H4 0.8400 . ?
O5 C9 1.372(4) . ?
O5 H5 0.8400 . ?
O11 C23 1.370(4) . ?
O11 H11 0.8400 . ?
C48 C47 1.315(4) . ?
C48 C49 1.324(4) . ?
C48 H48 0.9500 . ?
C12 C11 1.394(4) . ?
C12 C13 1.398(4) . ?
C12 H13 0.9500 . ?
N2 N1 1.318(4) . ?
N2 C47 1.407(4) . ?
N2 H15 0.8800 . ?
C23 C24 1.384(4) . ?
C23 C22 1.388(4) . ?
C2 C1 1.388(4) . ?
C2 C3 1.390(4) . ?
C13 C8 1.392(4) . ?
C13 C7 1.524(4) . ?
C9 C10 1.382(4) . ?
C9 C8 1.388(4) . ?
C10 C11 1.389(4) . ?
C14 C20 1.522(4) . ?
C14 C31 1.528(4) . ?
C14 C11 1.534(4) . ?
C14 H14 1.0000 . ?
C5 C4 1.390(4) . ?
C5 C6 1.391(4) . ?
C5 H16 0.9500 . ?
C16 C15 1.383(4) . ?
C16 C17 1.388(4) . ?
C17 C18 1.393(4) . ?
C18 C19 1.389(4) . ?
C18 C21 1.539(4) . ?
C27 C22 1.396(4) . ?
C27 C26 1.400(4) . ?
C27 C21 1.526(4) . ?
C24 C25 1.393(4) . ?
N1 C37 1.334(4) . ?
C37 C46 1.452(5) . ?
C37 C38 1.458(5) . ?
C6 C1 1.390(4) . ?
C6 C28 1.531(4) . ?
C7 C29 1.532(4) . ?
C7 C4 1.533(4) . ?
C7 H18 1.0000 . ?
C26 C25 1.394(4) . ?
C26 H26 0.9500 . ?
C20 C19 1.393(4) . ?
C20 C15 1.398(4) . ?
C51 C50 1.377(5) . ?
C51 N3 1.391(5) . ?
C51 H51 0.9500 . ?
C19 H19 0.9500 . ?
O13 C38 1.258(4) . ?
C21 C33 1.513(5) . ?
C21 H21 1.0000 . ?
C28 C35 1.513(4) . ?
C28 C25 1.528(4) . ?
C28 H28 1.0000 . ?
N3 C47 1.403(5) . ?
C50 C49 1.378(5) . ?
C50 H50 0.9500 . ?
C4 C3 1.397(4) . ?
C29 C30 1.522(5) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C38 C39 1.449(5) . ?
C31 C32 1.515(5) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C41 C42 1.403(6) . ?
C41 C46 1.405(5) . ?
C41 C40 1.436(6) . ?
C35 C36 1.528(5) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C39 C40 1.339(6) . ?
C39 H39 0.9500 . ?
C46 C45 1.405(5) . ?
C49 H49 0.9500 . ?
C33 C34 1.541(5) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C45 C44 1.376(5) . ?
C45 H45 0.9500 . ?
C42 C43 1.370(7) . ?
C42 H42 0.9500 . ?
C40 H40 0.9500 . ?
C43 C44 1.404(7) . ?
C43 H43 0.9500 . ?
C44 H44 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
C10 O6 H6 109.5 . . ?
C24 O12 H12 109.5 . . ?
C17 O9 H9 109.4 . . ?
C22 O10 H10 109.5 . . ?
C16 O8 H8 109.5 . . ?
C1 O1 H1 109.1 . . ?
C15 O7 H7 109.5 . . ?
C2 O2 H2 109.5 . . ?
C3 O3 H3 109.5 . . ?
C8 O4 H4 109.5 . . ?
C9 O5 H5 109.5 . . ?
C23 O11 H11 109.5 . . ?
C47 C48 C49 117.3(3) . . ?
C47 C48 H48 121.3 . . ?
C49 C48 H48 121.3 . . ?
C11 C12 C13 123.1(3) . . ?
C11 C12 H13 118.4 . . ?
C13 C12 H13 118.4 . . ?
N1 N2 C47 120.2(3) . . ?
N1 N2 H15 119.9 . . ?
C47 N2 H15 119.9 . . ?
O11 C23 C24 117.9(3) . . ?
O11 C23 C22 122.2(3) . . ?
C24 C23 C22 119.9(3) . . ?
O2 C2 C1 117.6(3) . . ?
O2 C2 C3 122.1(3) . . ?
C1 C2 C3 120.2(3) . . ?
C8 C13 C12 116.9(3) . . ?
C8 C13 C7 119.9(3) . . ?
C12 C13 C7 123.1(3) . . ?
O5 C9 C10 122.6(3) . . ?
O5 C9 C8 117.3(3) . . ?
C10 C9 C8 120.1(3) . . ?
C9 C10 C11 120.9(3) . . ?
C9 C10 O6 114.9(3) . . ?
C11 C10 O6 124.2(3) . . ?
C20 C14 C31 112.3(3) . . ?
C20 C14 C11 109.8(2) . . ?
C31 C14 C11 114.4(3) . . ?
C20 C14 H14 106.6 . . ?
C31 C14 H14 106.6 . . ?
C11 C14 H14 106.6 . . ?
C4 C5 C6 122.9(3) . . ?
C4 C5 H16 118.5 . . ?
C6 C5 H16 118.5 . . ?
C15 C16 C17 120.0(3) . . ?
C15 C16 O8 118.9(3) . . ?
C17 C16 O8 120.9(3) . . ?
O9 C17 C16 121.9(3) . . ?
O9 C17 C18 117.4(3) . . ?
C16 C17 C18 120.7(3) . . ?
C19 C18 C17 117.7(3) . . ?
C19 C18 C21 121.7(3) . . ?
C17 C18 C21 120.6(3) . . ?
C22 C27 C26 116.7(3) . . ?
C22 C27 C21 119.4(3) . . ?
C26 C27 C21 124.0(3) . . ?
O12 C24 C23 114.3(3) . . ?
O12 C24 C25 124.6(3) . . ?
C23 C24 C25 121.1(3) . . ?
N2 N1 C37 117.9(3) . . ?
N1 C37 C46 115.6(3) . . ?
N1 C37 C38 123.8(3) . . ?
C46 C37 C38 120.3(3) . . ?
C1 C6 C5 117.9(3) . . ?
C1 C6 C28 120.7(3) . . ?
C5 C6 C28 121.3(3) . . ?
C10 C11 C12 117.7(3) . . ?
C10 C11 C14 119.6(3) . . ?
C12 C11 C14 122.7(3) . . ?
C13 C7 C29 113.6(3) . . ?
C13 C7 C4 111.9(2) . . ?
C29 C7 C4 112.1(3) . . ?
C13 C7 H18 106.2 . . ?
C29 C7 H18 106.2 . . ?
C4 C7 H18 106.2 . . ?
O4 C8 C9 120.1(3) . . ?
O4 C8 C13 118.7(3) . . ?
C9 C8 C13 121.2(3) . . ?
O1 C1 C2 120.6(3) . . ?
O1 C1 C6 118.7(3) . . ?
C2 C1 C6 120.7(3) . . ?
C25 C26 C27 123.5(3) . . ?
C25 C26 H26 118.3 . . ?
C27 C26 H26 118.3 . . ?
C19 C20 C15 116.9(3) . . ?
C19 C20 C14 121.9(3) . . ?
C15 C20 C14 121.2(3) . . ?
C50 C51 N3 119.4(3) . . ?
C50 C51 H51 120.3 . . ?
N3 C51 H51 120.3 . . ?
C18 C19 C20 123.4(3) . . ?
C18 C19 H19 118.3 . . ?
C20 C19 H19 118.3 . . ?
C33 C21 C27 115.7(3) . . ?
C33 C21 C18 111.6(3) . . ?
C27 C21 C18 110.5(2) . . ?
C33 C21 H21 106.1 . . ?
C27 C21 H21 106.1 . . ?
C18 C21 H21 106.1 . . ?
C35 C28 C25 115.0(3) . . ?
C35 C28 C6 113.0(3) . . ?
C25 C28 C6 109.1(2) . . ?
C35 C28 H28 106.4 . . ?
C25 C28 H28 106.4 . . ?
C6 C28 H28 106.4 . . ?
C51 N3 C47 116.4(3) . . ?
C24 C25 C26 117.3(3) . . ?
C24 C25 C28 119.4(3) . . ?
C26 C25 C28 123.1(3) . . ?
O10 C22 C23 113.8(3) . . ?
O10 C22 C27 124.8(3) . . ?
C23 C22 C27 121.4(3) . . ?
C51 C50 C49 118.6(3) . . ?
C51 C50 H50 120.7 . . ?
C49 C50 H50 120.7 . . ?
C5 C4 C3 117.8(3) . . ?
C5 C4 C7 120.8(3) . . ?
C3 C4 C7 121.4(3) . . ?
C30 C29 C7 112.8(3) . . ?
C30 C29 H29A 109.0 . . ?
C7 C29 H29A 109.0 . . ?
C30 C29 H29B 109.0 . . ?
C7 C29 H29B 109.0 . . ?
H29A C29 H29B 107.8 . . ?
O13 C38 C39 120.7(3) . . ?
O13 C38 C37 122.3(3) . . ?
C39 C38 C37 116.9(3) . . ?
C32 C31 C14 113.6(3) . . ?
C32 C31 H31A 108.8 . . ?
C14 C31 H31A 108.8 . . ?
C32 C31 H31B 108.8 . . ?
C14 C31 H31B 108.8 . . ?
H31A C31 H31B 107.7 . . ?
C48 C47 N3 124.6(3) . . ?
C48 C47 N2 118.8(3) . . ?
N3 C47 N2 116.6(3) . . ?
C42 C41 C46 119.2(4) . . ?
C42 C41 C40 121.8(4) . . ?
C46 C41 C40 119.0(4) . . ?
C28 C35 C36 112.6(3) . . ?
C28 C35 H35A 109.1 . . ?
C36 C35 H35A 109.1 . . ?
C28 C35 H35B 109.1 . . ?
C36 C35 H35B 109.1 . . ?
H35A C35 H35B 107.8 . . ?
C16 C15 O7 120.3(3) . . ?
C16 C15 C20 121.2(3) . . ?
O7 C15 C20 118.5(3) . . ?
O3 C3 C2 115.1(3) . . ?
O3 C3 C4 124.4(3) . . ?
C2 C3 C4 120.5(3) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C40 C39 C38 121.1(4) . . ?
C40 C39 H39 119.5 . . ?
C38 C39 H39 119.5 . . ?
C45 C46 C41 118.7(4) . . ?
C45 C46 C37 122.4(3) . . ?
C41 C46 C37 118.8(3) . . ?
C48 C49 C50 123.6(3) . . ?
C48 C49 H49 118.2 . . ?
C50 C49 H49 118.2 . . ?
C21 C33 C34 110.7(3) . . ?
C21 C33 H33A 109.5 . . ?
C34 C33 H33A 109.5 . . ?
C21 C33 H33B 109.5 . . ?
C34 C33 H33B 109.5 . . ?
H33A C33 H33B 108.1 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C44 C45 C46 121.3(4) . . ?
C44 C45 H45 119.4 . . ?
C46 C45 H45 119.4 . . ?
C43 C42 C41 121.3(4) . . ?
C43 C42 H42 119.4 . . ?
C41 C42 H42 119.4 . . ?
C39 C40 C41 123.1(4) . . ?
C39 C40 H40 118.4 . . ?
C41 C40 H40 118.4 . . ?
C42 C43 C44 119.8(4) . . ?
C42 C43 H43 120.1 . . ?
C44 C43 H43 120.1 . . ?
C45 C44 C43 119.7(5) . . ?
C45 C44 H44 120.2 . . ?
C43 C44 H44 120.2 . . ?

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
C11 C12 C13 C8 -0.9(4) . . . . ?
C11 C12 C13 C7 177.8(3) . . . . ?
O5 C9 C10 C11 179.4(3) . . . . ?
C8 C9 C10 C11 0.3(5) . . . . ?
O5 C9 C10 O6 -2.9(4) . . . . ?
C8 C9 C10 O6 178.0(3) . . . . ?
C15 C16 C17 O9 -178.8(3) . . . . ?
O8 C16 C17 O9 -3.5(4) . . . . ?
C15 C16 C17 C18 0.6(4) . . . . ?
O8 C16 C17 C18 175.9(3) . . . . ?
O9 C17 C18 C19 -178.8(3) . . . . ?
C16 C17 C18 C19 1.8(4) . . . . ?
O9 C17 C18 C21 0.7(4) . . . . ?
C16 C17 C18 C21 -178.7(3) . . . . ?
O11 C23 C24 O12 -0.8(4) . . . . ?
C22 C23 C24 O12 179.8(3) . . . . ?
O11 C23 C24 C25 179.4(3) . . . . ?
C22 C23 C24 C25 0.0(5) . . . . ?
C47 N2 N1 C37 -171.8(3) . . . . ?
N2 N1 C37 C46 -179.2(3) . . . . ?
N2 N1 C37 C38 7.7(5) . . . . ?
C4 C5 C6 C1 -1.3(4) . . . . ?
C4 C5 C6 C28 -178.3(3) . . . . ?
C9 C10 C11 C12 1.1(4) . . . . ?
O6 C10 C11 C12 -176.4(3) . . . . ?
C9 C10 C11 C14 -177.4(3) . . . . ?
O6 C10 C11 C14 5.1(4) . . . . ?
C13 C12 C11 C10 -0.7(4) . . . . ?
C13 C12 C11 C14 177.7(3) . . . . ?
C20 C14 C11 C10 84.6(3) . . . . ?
C31 C14 C11 C10 -148.0(3) . . . . ?
C20 C14 C11 C12 -93.8(3) . . . . ?
C31 C14 C11 C12 33.6(4) . . . . ?
C8 C13 C7 C29 150.4(3) . . . . ?
C12 C13 C7 C29 -28.3(4) . . . . ?
C8 C13 C7 C4 -81.3(3) . . . . ?
C12 C13 C7 C4 100.0(3) . . . . ?
O5 C9 C8 O4 0.2(4) . . . . ?
C10 C9 C8 O4 179.4(3) . . . . ?
O5 C9 C8 C13 178.7(3) . . . . ?
C10 C9 C8 C13 -2.1(5) . . . . ?
C12 C13 C8 O4 -179.1(3) . . . . ?
C7 C13 C8 O4 2.1(4) . . . . ?
C12 C13 C8 C9 2.4(4) . . . . ?
C7 C13 C8 C9 -176.4(3) . . . . ?
O2 C2 C1 O1 -1.5(4) . . . . ?
C3 C2 C1 O1 177.9(3) . . . . ?
O2 C2 C1 C6 -179.4(3) . . . . ?
C3 C2 C1 C6 0.0(5) . . . . ?
C5 C6 C1 O1 -177.7(3) . . . . ?
C28 C6 C1 O1 -0.6(4) . . . . ?
C5 C6 C1 C2 0.3(4) . . . . ?
C28 C6 C1 C2 177.3(3) . . . . ?
C22 C27 C26 C25 -0.3(4) . . . . ?
C21 C27 C26 C25 -179.5(3) . . . . ?
C31 C14 C20 C19 -50.9(4) . . . . ?
C11 C14 C20 C19 77.6(4) . . . . ?
C31 C14 C20 C15 130.8(3) . . . . ?
C11 C14 C20 C15 -100.7(3) . . . . ?
C17 C18 C19 C20 -1.4(5) . . . . ?
C21 C18 C19 C20 179.1(3) . . . . ?
C15 C20 C19 C18 -1.3(4) . . . . ?
C14 C20 C19 C18 -179.7(3) . . . . ?
C22 C27 C21 C33 158.4(3) . . . . ?
C26 C27 C21 C33 -22.4(4) . . . . ?
C22 C27 C21 C18 -73.5(4) . . . . ?
C26 C27 C21 C18 105.7(3) . . . . ?
C19 C18 C21 C33 52.8(4) . . . . ?
C17 C18 C21 C33 -126.6(3) . . . . ?
C19 C18 C21 C27 -77.5(4) . . . . ?
C17 C18 C21 C27 103.1(3) . . . . ?
C1 C6 C28 C35 128.7(3) . . . . ?
C5 C6 C28 C35 -54.4(4) . . . . ?
C1 C6 C28 C25 -102.1(3) . . . . ?
C5 C6 C28 C25 74.8(4) . . . . ?
C50 C51 N3 C47 -1.1(5) . . . . ?
O12 C24 C25 C26 -178.1(3) . . . . ?
C23 C24 C25 C26 1.7(4) . . . . ?
O12 C24 C25 C28 6.3(5) . . . . ?
C23 C24 C25 C28 -173.9(3) . . . . ?
C27 C26 C25 C24 -1.5(5) . . . . ?
C27 C26 C25 C28 173.9(3) . . . . ?
C35 C28 C25 C24 -156.7(3) . . . . ?
C6 C28 C25 C24 75.2(3) . . . . ?
C35 C28 C25 C26 28.0(4) . . . . ?
C6 C28 C25 C26 -100.2(3) . . . . ?
O11 C23 C22 O10 -1.7(4) . . . . ?
C24 C23 C22 O10 177.7(3) . . . . ?
O11 C23 C22 C27 178.7(3) . . . . ?
C24 C23 C22 C27 -1.9(5) . . . . ?
C26 C27 C22 O10 -177.6(3) . . . . ?
C21 C27 C22 O10 1.7(5) . . . . ?
C26 C27 C22 C23 2.0(4) . . . . ?
C21 C27 C22 C23 -178.7(3) . . . . ?
N3 C51 C50 C49 2.1(5) . . . . ?
C6 C5 C4 C3 1.9(4) . . . . ?
C6 C5 C4 C7 -177.9(3) . . . . ?
C13 C7 C4 C5 -80.0(4) . . . . ?
C29 C7 C4 C5 49.0(4) . . . . ?
C13 C7 C4 C3 100.2(3) . . . . ?
C29 C7 C4 C3 -130.8(3) . . . . ?
C13 C7 C29 C30 -173.4(3) . . . . ?
C4 C7 C29 C30 58.5(4) . . . . ?
N1 C37 C38 O13 -11.3(5) . . . . ?
C46 C37 C38 O13 175.9(3) . . . . ?
N1 C37 C38 C39 165.7(3) . . . . ?
C46 C37 C38 C39 -7.1(5) . . . . ?
C20 C14 C31 C32 -173.7(3) . . . . ?
C11 C14 C31 C32 60.2(4) . . . . ?
C49 C48 C47 N3 2.0(5) . . . . ?
C49 C48 C47 N2 180.0(3) . . . . ?
C51 N3 C47 C48 -1.0(5) . . . . ?
C51 N3 C47 N2 -179.0(3) . . . . ?
N1 N2 C47 C48 22.7(5) . . . . ?
N1 N2 C47 N3 -159.2(3) . . . . ?
C25 C28 C35 C36 173.3(3) . . . . ?
C6 C28 C35 C36 -60.5(4) . . . . ?
C17 C16 C15 O7 175.9(3) . . . . ?
O8 C16 C15 O7 0.6(4) . . . . ?
C17 C16 C15 C20 -3.5(4) . . . . ?
O8 C16 C15 C20 -178.9(3) . . . . ?
C19 C20 C15 C16 3.8(4) . . . . ?
C14 C20 C15 C16 -177.8(3) . . . . ?
C19 C20 C15 O7 -175.7(3) . . . . ?
C14 C20 C15 O7 2.7(4) . . . . ?
O2 C2 C3 O3 -1.6(4) . . . . ?
C1 C2 C3 O3 179.0(3) . . . . ?
O2 C2 C3 C4 -179.9(3) . . . . ?
C1 C2 C3 C4 0.6(5) . . . . ?
C5 C4 C3 O3 -179.7(3) . . . . ?
C7 C4 C3 O3 0.1(5) . . . . ?
C5 C4 C3 C2 -1.5(4) . . . . ?
C7 C4 C3 C2 178.3(3) . . . . ?
O13 C38 C39 C40 177.1(4) . . . . ?
C37 C38 C39 C40 0.1(5) . . . . ?
C42 C41 C46 C45 -3.5(5) . . . . ?
C40 C41 C46 C45 174.9(4) . . . . ?
C42 C41 C46 C37 176.2(3) . . . . ?
C40 C41 C46 C37 -5.5(5) . . . . ?
N1 C37 C46 C45 16.1(5) . . . . ?
C38 C37 C46 C45 -170.6(3) . . . . ?
N1 C37 C46 C41 -163.5(3) . . . . ?
C38 C37 C46 C41 9.8(5) . . . . ?
C47 C48 C49 C50 -0.9(5) . . . . ?
C51 C50 C49 C48 -1.1(6) . . . . ?
C27 C21 C33 C34 -171.1(3) . . . . ?
C18 C21 C33 C34 61.4(4) . . . . ?
C41 C46 C45 C44 2.1(6) . . . . ?
C37 C46 C45 C44 -177.6(4) . . . . ?
C46 C41 C42 C43 2.5(6) . . . . ?
C40 C41 C42 C43 -175.8(4) . . . . ?
C38 C39 C40 C41 4.4(6) . . . . ?
C42 C41 C40 C39 176.7(4) . . . . ?
C46 C41 C40 C39 -1.6(6) . . . . ?
C41 C42 C43 C44 0.0(7) . . . . ?
C46 C45 C44 C43 0.4(7) . . . . ?
C42 C43 C44 C45 -1.5(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        23.92
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.056

_database_code_depnum_ccdc_archive 'CCDC 1002500'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2cp55e4

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            
'C-propylpyrogallol[4]arene with 1-(2-pyridylazo)-2-napthol'
_chemical_formula_moiety         
'C40 H48 O12, 2(C15 H11 O1 N3), 1.5(H2 O1), 1.5(C1 H4 O1)'
_chemical_formula_sum            'C71.50 H79 N6 O17'
_chemical_melting_point          ?

_exptl_crystal_description       plate
_exptl_crystal_colour            orange

_diffrn_ambient_temperature      173(2)
_chemical_formula_weight         1294.41

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'
O O 0.0106 0.0060 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?

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

_cell_length_a                   12.453(3)
_cell_length_b                   15.858(3)
_cell_length_c                   19.087(6)
_cell_angle_alpha                110.506(4)
_cell_angle_beta                 94.181(4)
_cell_angle_gamma                110.339(3)
_cell_volume                     3228.1(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    5824
_cell_measurement_theta_min      2.3
_cell_measurement_theta_max      22.2
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1372
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_process_details   
;
 Data were corrected for decay and absorption using the program SADABS 
 (Sheldrick, G. M. (2003). SADABS. Version 2.10. University of
 Göttingen, Germany).
;

_exptl_special_details           
; 
 ? 
;
_diffrn_radiation_probe          ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.0
_diffrn_reflns_number            37598
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_sigmaI/netI    0.0527
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.48
_diffrn_reflns_theta_max         27.20
_reflns_number_total             14230
_reflns_number_gt                8571
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2008)'
_computing_structure_solution    'SHELXS-1997 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-1997 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-SEED, Barbour, 2001'
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. There is minor residual
 electron denisty near a nitrogen on an aromatic group that is due to 
 delocalization. There are two partial lone oxygen atoms that are water 
 molecules that do not have calculated or modeled hydrogens but these 
 hydrogens are included in the molecular formula. O1M, O2M, and O3M are all
 partial occupancy atoms and do have acceptors, a partial occupancy water
 molecule. The hydroxyl groups of the pyrogallol[4]arene tail are disordered
 but not modeled. This along with the partial occupancy waters and methanols
 account for the short distances.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0951P)²+1.3324P] where P=(Fo²+2Fc²)/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         14230
_refine_ls_number_parameters     913
_refine_ls_number_restraints     49
_refine_ls_R_factor_all          0.1131
_refine_ls_R_factor_gt           0.0677
_refine_ls_wR_factor_ref         0.2070
_refine_ls_wR_factor_gt          0.1782
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.071
_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
O6 O 0.90331(15) 0.29165(13) 0.35466(10) 0.0346(4) Uani 1 1 d . . .
H6 H 0.9374 0.3320 0.3999 0.041 Uiso 1 1 calc R . .
O4 O 0.70448(16) 0.50514(13) 0.39842(10) 0.0336(4) Uani 1 1 d . . .
H4 H 0.6447 0.5104 0.3804 0.040 Uiso 1 1 calc R . .
O3 O 0.49200(16) 0.52328(12) 0.37379(10) 0.0341(4) Uani 1 1 d . . .
H3 H 0.4636 0.5581 0.4041 0.041 Uiso 1 1 calc R . .
O1W O 1.04858(18) 0.35788(15) 0.49051(13) 0.0374(5) Uani 1 1 d . . .
O5 O 0.86698(16) 0.44457(13) 0.44845(10) 0.0350(4) Uani 1 1 d . . .
H5 H 0.8810 0.5047 0.4643 0.042 Uiso 1 1 calc R . .
C7 C 0.5361(2) 0.38289(18) 0.24890(14) 0.0277(5) Uani 1 1 d . . .
H7 H 0.5643 0.4553 0.2635 0.033 Uiso 1 1 calc R . .
O7 O 0.92959(16) 0.11958(14) 0.29607(12) 0.0441(5) Uani 1 1 d . . .
H7A H 0.9468 0.1801 0.3185 0.053 Uiso 1 1 calc R . .
C9 C 0.8001(2) 0.39707(18) 0.37539(14) 0.0285(5) Uani 1 1 d . . .
O2 O 0.33494(17) 0.47351(14) 0.45638(11) 0.0401(5) Uani 1 1 d . . .
H2 H 0.3028 0.4518 0.4872 0.048 Uiso 1 1 calc R . .
O10 O 0.4559(2) -0.06241(15) 0.40269(11) 0.0488(5) Uani 1 1 d . . .
H10 H 0.4867 -0.0923 0.3705 0.059 Uiso 1 1 calc R . .
O1 O 0.19937(18) 0.27885(14) 0.42461(12) 0.0425(5) Uani 1 1 d . . .
H1 H 0.1851 0.2218 0.4217 0.051 Uiso 1 1 calc R . .
C12 C 0.6602(2) 0.28134(18) 0.23003(14) 0.0278(5) Uani 1 1 d . . .
H12 H 0.6111 0.2410 0.1803 0.033 Uiso 1 1 calc R . .
C10 C 0.8178(2) 0.31593(18) 0.32803(14) 0.0277(5) Uani 1 1 d . . .
O9 O 0.60826(19) -0.13007(15) 0.32267(11) 0.0467(5) Uani 1 1 d . . .
H9 H 0.6513 -0.1120 0.3657 0.056 Uiso 1 1 d . . .
C2 C 0.3427(2) 0.39819(19) 0.39656(14) 0.0300(6) Uani 1 1 d . . .
C8 C 0.7127(2) 0.42132(18) 0.34842(14) 0.0280(5) Uani 1 1 d . . .
C13 C 0.6400(2) 0.36283(18) 0.27560(14) 0.0269(5) Uani 1 1 d . . .
C11 C 0.7487(2) 0.25682(18) 0.25427(14) 0.0271(5) Uani 1 1 d . . .
C4 C 0.4399(2) 0.35446(18) 0.29236(14) 0.0268(5) Uani 1 1 d . . .
C14 C 0.7701(2) 0.16697(18) 0.20591(14) 0.0294(6) Uani 1 1 d . . .
H14 H 0.8569 0.1883 0.2110 0.035 Uiso 1 1 calc R . .
C19 C 0.6110(2) 0.03421(18) 0.22869(14) 0.0295(6) Uani 1 1 d . . .
H19 H 0.5561 0.0486 0.2029 0.035 Uiso 1 1 calc R . .
C3 C 0.4229(2) 0.42571(18) 0.35337(14) 0.0286(5) Uani 1 1 d . . .
C21 C 0.4370(2) -0.09842(19) 0.23978(15) 0.0328(6) Uani 1 1 d . . .
H21 H 0.4268 -0.1553 0.2539 0.039 Uiso 1 1 calc R . .
C1 C 0.2747(2) 0.29969(19) 0.37752(15) 0.0311(6) Uani 1 1 d . . .
C28 C 0.2034(2) 0.1185(2) 0.28771(16) 0.0380(6) Uani 1 1 d . . .
H28 H 0.1373 0.1168 0.3147 0.046 Uiso 1 1 calc R . .
C16 C 0.7697(3) -0.0044(2) 0.30631(16) 0.0384(7) Uani 1 1 d . . .
C5 C 0.3694(2) 0.25659(19) 0.27450(14) 0.0285(5) Uani 1 1 d . . .
H13 H 0.3800 0.2075 0.2331 0.034 Uiso 1 1 calc R . .
C26 C 0.3179(2) 0.00816(18) 0.26700(15) 0.0331(6) Uani 1 1 d . . .
H26 H 0.3115 0.0017 0.2153 0.040 Uiso 1 1 calc R . .
O8 O 0.8477(2) -0.02433(16) 0.34615(13) 0.0539(6) Uani 1 1 d . . .
H8 H 0.9137 0.0229 0.3613 0.065 Uiso 1 1 calc R . .
C29 C 0.4883(2) 0.3323(2) 0.16226(15) 0.0344(6) Uani 1 1 d . . .
H29A H 0.5546 0.3476 0.1367 0.041 Uiso 1 1 calc R . .
H29B H 0.4539 0.2604 0.1473 0.041 Uiso 1 1 calc R . .
C18 C 0.5683(2) -0.04029(18) 0.25442(14) 0.0312(6) Uani 1 1 d . . .
C20 C 0.7301(2) 0.08883(18) 0.23872(15) 0.0302(6) Uani 1 1 d . . .
C6 C 0.2842(2) 0.22678(19) 0.31408(15) 0.0309(6) Uani 1 1 d . . .
C32 C 0.7145(2) 0.1248(2) 0.12018(15) 0.0345(6) Uani 1 1 d . . .
H32A H 0.6280 0.0989 0.1131 0.041 Uiso 1 1 calc R . .
H32B H 0.7387 0.1784 0.1019 0.041 Uiso 1 1 calc R . .
C17 C 0.6502(3) -0.05889(19) 0.29427(15) 0.0367(6) Uani 1 1 d . . .
C15 C 0.8086(2) 0.06893(19) 0.27910(15) 0.0336(6) Uani 1 1 d . . .
C27 C 0.3808(2) -0.03781(18) 0.29214(15) 0.0326(6) Uani 1 1 d . . .
C35 C 0.3782(2) -0.14145(19) 0.15438(15) 0.0352(6) Uani 1 1 d . . .
H35A H 0.2924 -0.1755 0.1476 0.042 Uiso 1 1 calc R . .
H35B H 0.3919 -0.0872 0.1372 0.042 Uiso 1 1 calc R . .
O12 O 0.2202(3) 0.12071(19) 0.43668(15) 0.0698(8) Uani 1 1 d . . .
H12A H 0.2263 0.1144 0.4785 0.084 Uiso 1 1 calc R . .
C22 C 0.3924(3) -0.0258(2) 0.36852(16) 0.0397(7) Uani 1 1 d . . .
O11 O 0.3468(3) 0.03878(19) 0.49197(13) 0.0698(8) Uani 1 1 d . . .
H11 H 0.3906 0.0129 0.5026 0.084 Uiso 1 1 calc R . .
C25 C 0.2645(2) 0.06275(19) 0.31360(16) 0.0354(6) Uani 1 1 d . . .
C33 C 0.7486(3) 0.0429(2) 0.07120(17) 0.0458(7) Uani 1 1 d . . .
H33A H 0.8348 0.0693 0.0766 0.055 Uiso 1 1 calc R . .
H33B H 0.7271 -0.0098 0.0905 0.055 Uiso 1 1 calc R . .
C38 C 0.1479(2) 0.0738(2) 0.20145(17) 0.0432(7) Uani 1 1 d . . .
H38A H 0.1160 0.1181 0.1906 0.052 Uiso 1 1 calc R . .
H38B H 0.2104 0.0710 0.1726 0.052 Uiso 1 1 calc R . .
C36 C 0.4244(3) -0.2135(2) 0.10441(16) 0.0415(7) Uani 1 1 d . . .
H36A H 0.5105 -0.1800 0.1121 0.050 Uiso 1 1 calc R . .
H36B H 0.4089 -0.2686 0.1207 0.050 Uiso 1 1 calc R . .
C23 C 0.3383(3) 0.0266(2) 0.41612(17) 0.0492(8) Uani 1 1 d . . .
C30 C 0.3959(3) 0.3615(2) 0.13285(17) 0.0447(7) Uani 1 1 d . . .
H30A H 0.3364 0.3579 0.1646 0.054 Uiso 1 1 calc R . .
H30B H 0.4336 0.4304 0.1383 0.054 Uiso 1 1 calc R . .
C24 C 0.2742(3) 0.0688(2) 0.38871(18) 0.0483(8) Uani 1 1 d . . .
C39 C 0.0505(3) -0.0283(2) 0.1716(2) 0.0563(9) Uani 1 1 d . . .
H39A H -0.0112 -0.0269 0.2014 0.068 Uiso 1 1 calc R . .
H39B H 0.0827 -0.0741 0.1795 0.068 Uiso 1 1 calc R . .
C31 C 0.3353(3) 0.2961(3) 0.04965(19) 0.0656(10) Uani 1 1 d . . .
H31A H 0.3940 0.2985 0.0180 0.098 Uiso 1 1 calc R . .
H31B H 0.2789 0.3192 0.0327 0.098 Uiso 1 1 calc R . .
H31C H 0.2939 0.2285 0.0444 0.098 Uiso 1 1 calc R . .
C34 C 0.6895(4) -0.0005(3) -0.01278(19) 0.0682(11) Uani 1 1 d . . .
H34A H 0.6041 -0.0277 -0.0186 0.102 Uiso 1 1 calc R . .
H34B H 0.7138 -0.0529 -0.0414 0.102 Uiso 1 1 calc R . .
H34C H 0.7124 0.0508 -0.0327 0.102 Uiso 1 1 calc R . .
C40 C -0.0040(3) -0.0660(3) 0.0870(2) 0.0741(12) Uani 1 1 d . . .
H40A H -0.0304 -0.0184 0.0782 0.111 Uiso 1 1 calc R . .
H40B H -0.0713 -0.1290 0.0714 0.111 Uiso 1 1 calc R . .
H40C H 0.0545 -0.0751 0.0567 0.111 Uiso 1 1 calc R . .
O13 O 0.9616(2) 0.61881(16) 0.36098(12) 0.0532(6) Uani 1 1 d . . .
C50 C 0.9471(2) 0.4930(2) 0.24279(16) 0.0355(6) Uani 1 1 d . . .
N1 N 0.8694(2) 0.50406(18) 0.20040(14) 0.0404(6) Uani 1 1 d U . .
C49 C 0.9882(2) 0.4167(2) 0.20252(16) 0.0342(6) Uani 1 1 d . . .
N2 N 0.8272(2) 0.5704(2) 0.23230(16) 0.0510(7) Uani 1 1 d U . .
H17 H 0.8485 0.6053 0.2821 0.061 Uiso 1 1 calc R . .
C44 C 1.0704(2) 0.4002(2) 0.24472(16) 0.0376(6) Uani 1 1 d . . .
C41 C 0.9945(3) 0.5517(2) 0.32556(17) 0.0402(7) Uani 1 1 d . . .
C45 C 1.1087(3) 0.3266(2) 0.20684(19) 0.0467(8) Uani 1 1 d . . .
H45 H 1.1640 0.3149 0.2351 0.056 Uiso 1 1 calc R . .
C42 C 1.0777(3) 0.5298(2) 0.36437(17) 0.0438(7) Uani 1 1 d . . .
H42 H 1.1083 0.5660 0.4180 0.053 Uiso 1 1 calc R . .
C47 C 0.9871(3) 0.2876(2) 0.08783(18) 0.0468(7) Uani 1 1 d . . .
H47 H 0.9587 0.2490 0.0343 0.056 Uiso 1 1 calc R . .
C48 C 0.9476(3) 0.3599(2) 0.12376(17) 0.0413(7) Uani 1 1 d . . .
H48 H 0.8926 0.3709 0.0947 0.050 Uiso 1 1 calc R . .
C43 C 1.1129(2) 0.4590(2) 0.32601(18) 0.0426(7) Uani 1 1 d . . .
H43 H 1.1685 0.4470 0.3537 0.051 Uiso 1 1 calc R . .
C46 C 1.0675(3) 0.2710(2) 0.1294(2) 0.0500(8) Uani 1 1 d . . .
H46 H 1.0943 0.2213 0.1044 0.060 Uiso 1 1 calc R . .
C52 C 0.7116(3) 0.5319(3) 0.1090(2) 0.0603(9) Uani 1 1 d U . .
H52 H 0.7373 0.4817 0.0833 0.072 Uiso 1 1 calc R . .
C51 C 0.7488(3) 0.5846(3) 0.1865(2) 0.0593(9) Uani 1 1 d U . .
N3 N 0.7119(4) 0.6531(3) 0.2238(2) 0.0940(12) Uani 1 1 d U . .
C53 C 0.6359(4) 0.5537(4) 0.0694(3) 0.0803(13) Uani 1 1 d U . .
H53 H 0.6114 0.5200 0.0152 0.096 Uiso 1 1 calc R . .
C54 C 0.5958(5) 0.6226(4) 0.1066(3) 0.0983(16) Uani 1 1 d U . .
H54 H 0.5417 0.6367 0.0797 0.118 Uiso 1 1 calc R . .
C55 C 0.6355(5) 0.6703(4) 0.1830(4) 0.1108(19) Uani 1 1 d U . .
H55 H 0.6080 0.7189 0.2097 0.133 Uiso 1 1 calc R . .
N6 N 0.4356(2) 0.67930(17) 0.47008(14) 0.0421(6) Uani 1 1 d . . .
N4 N 0.2739(3) 0.69701(18) 0.32360(14) 0.0515(7) Uani 1 1 d . . .
C67 C 0.3267(3) 0.7813(2) 0.48400(17) 0.0431(7) Uani 1 1 d . . .
H67 H 0.2812 0.8052 0.4602 0.052 Uiso 1 1 calc R . .
C66 C 0.3710(3) 0.7155(2) 0.44112(16) 0.0382(7) Uani 1 1 d . . .
C70 C 0.4570(3) 0.7090(2) 0.54666(18) 0.0433(7) Uani 1 1 d . . .
H70 H 0.5017 0.6833 0.5690 0.052 Uiso 1 1 calc R . .
N5 N 0.3500(2) 0.67955(18) 0.36070(14) 0.0492(7) Uani 1 1 d . . .
H5A H 0.3879 0.6455 0.3356 0.059 Uiso 1 1 calc R . .
C69 C 0.4184(2) 0.7738(2) 0.59453(16) 0.0395(7) Uani 1 1 d . . .
H69 H 0.4371 0.7931 0.6485 0.047 Uiso 1 1 calc R . .
C68 C 0.3516(3) 0.8105(2) 0.56256(17) 0.0424(7) Uani 1 1 d . . .
H68 H 0.3232 0.8553 0.5944 0.051 Uiso 1 1 calc R . .
C65 C 0.2478(3) 0.6537(3) 0.24732(19) 0.0635(11) Uani 1 1 d . . .
C59 C 0.1255(5) 0.6267(4) 0.1273(3) 0.0938(18) Uani 1 1 d . . .
O14 O 0.3756(4) 0.5696(2) 0.23515(18) 0.0967(11) Uani 1 1 d . . .
C56 C 0.3002(5) 0.5863(3) 0.2037(2) 0.0713(13) Uani 1 1 d . . .
C64 C 0.1643(4) 0.6739(3) 0.2090(2) 0.0708(12) Uani 1 1 d . . .
C63 C 0.1144(4) 0.7380(3) 0.2472(3) 0.0810(15) Uani 1 1 d . . .
H63 H 0.1388 0.7700 0.3015 0.097 Uiso 1 1 calc R . .
C61 C -0.0047(5) 0.7096(5) 0.1294(4) 0.121(3) Uani 1 1 d . . .
H61 H -0.0614 0.7209 0.1020 0.145 Uiso 1 1 calc R . .
C57 C 0.2536(6) 0.5390(4) 0.1217(3) 0.105(2) Uani 1 1 d . . .
H57 H 0.2799 0.4916 0.0913 0.127 Uiso 1 1 calc R . .
C62 C 0.0313(4) 0.7582(4) 0.2113(3) 0.109(2) Uani 1 1 d . . .
H62 H -0.0005 0.8025 0.2398 0.131 Uiso 1 1 calc R . .
C60 C 0.0446(6) 0.6462(5) 0.0911(4) 0.132(3) Uani 1 1 d . . .
H60 H 0.0209 0.6144 0.0368 0.159 Uiso 1 1 calc R . .
C58 C 0.1764(6) 0.5592(4) 0.0878(3) 0.105(2) Uani 1 1 d . . .
H58 H 0.1521 0.5273 0.0335 0.126 Uiso 1 1 calc R . .
O1M O 0.6792(5) 0.7249(4) 0.3927(3) 0.0659(14) Uani 0.50 1 d PU A 1
H1M H 0.6165 0.6855 0.3600 0.079 Uiso 0.50 1 calc PR A 1
C37 C 0.3686(3) -0.2538(3) 0.02040(18) 0.0606(9) Uani 1 1 d . . .
H37A H 0.2831 -0.2853 0.0127 0.091 Uiso 1 1 calc R . .
H37B H 0.3978 -0.3022 -0.0091 0.091 Uiso 1 1 calc R . .
H37C H 0.3885 -0.2001 0.0030 0.091 Uiso 1 1 calc R . .
O1M2 O 0.7439(4) 0.8172(3) 0.4036(3) 0.0410(11) Uani 0.50 1 d P B 2
H1W H 1.097(3) 0.331(3) 0.472(2) 0.073(12) Uiso 1 1 d . . .
H2W H 1.036(4) 0.350(3) 0.532(3) 0.081(14) Uiso 1 1 d . . .
C1M2 C 0.7511(6) 0.7866(5) 0.3620(4) 0.0347(14) Uani 0.50 1 d P A 1
H1M1 H 0.7389 0.8477 0.3775 0.052 Uiso 0.50 1 calc PR A 1
H1M2 H 0.7311 0.7535 0.3059 0.052 Uiso 0.50 1 calc PR A 1
H1M3 H 0.8336 0.8014 0.3811 0.052 Uiso 0.50 1 calc PR A 1
C2M C 1.0503(15) 0.8784(12) 0.4574(9) 0.128(6) Uani 0.50 1 d PDU C 1
H2M1 H 1.1151 0.9200 0.5026 0.192 Uiso 0.50 1 calc PR C 1
H2M2 H 1.0780 0.8825 0.4115 0.192 Uiso 0.50 1 calc PR C 1
H2M3 H 1.0220 0.8102 0.4524 0.192 Uiso 0.50 1 calc PR C 1
C3M C 0.9952(19) 0.8772(17) 0.4171(11) 0.169(8) Uani 0.50 1 d PDU D 2
H3M1 H 0.9580 0.9240 0.4246 0.254 Uiso 0.50 1 calc PR D 2
H3M2 H 0.9413 0.8127 0.3786 0.254 Uiso 0.50 1 calc PR D 2
H3M3 H 1.0676 0.9002 0.3996 0.254 Uiso 0.50 1 calc PR D 2
O2M O 0.9505(9) 0.9134(7) 0.4663(6) 0.152(4) Uani 0.50 1 d PDU C 1
H2M H 0.8873 0.8674 0.4380 0.182 Uiso 0.50 1 calc PR C 1
O3M O 1.025(2) 0.8686(18) 0.4944(12) 0.278(10) Uani 0.50 1 d PDU D 2
H3M H 0.9901 0.8949 0.5257 0.334 Uiso 0.50 1 calc PR D 2


_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
O6 C10 1.373(3) . ?
O6 H6 0.8400 . ?
O4 C8 1.381(3) . ?
O4 H4 0.8400 . ?
O3 C3 1.375(3) . ?
O3 H3 0.8400 . ?
O1W H1W 0.88(4) . ?
O1W H2W 0.87(4) . ?
O5 C9 1.366(3) . ?
O5 H5 0.8400 . ?
C7 C29 1.526(4) . ?
C7 C13 1.529(3) . ?
C7 C4 1.536(3) . ?
C7 H7 1.0000 . ?
O7 C15 1.387(3) . ?
O7 H7A 0.8400 . ?
C9 C10 1.390(3) . ?
C9 C8 1.395(3) . ?
O2 C2 1.371(3) . ?
O2 H2 0.8400 . ?
O10 C22 1.378(4) . ?
O10 H10 0.8400 . ?
O1 C1 1.383(3) . ?
O1 H1 0.8400 . ?
C12 C11 1.389(3) . ?
C12 C13 1.400(3) . ?
C12 H12 0.9500 . ?
C10 C11 1.392(3) . ?
O9 C17 1.379(3) . ?
O9 H9 0.8413 . ?
C2 C1 1.388(4) . ?
C2 C3 1.392(4) . ?
C8 C13 1.393(4) . ?
C11 C14 1.527(3) . ?
C4 C5 1.391(4) . ?
C4 C3 1.399(3) . ?
C14 C20 1.528(4) . ?
C14 C32 1.533(4) . ?
C14 H14 1.0000 . ?
C19 C18 1.388(3) . ?
C19 C20 1.391(4) . ?
C19 H19 0.9500 . ?
C21 C18 1.519(4) . ?
C21 C27 1.519(4) . ?
C21 C35 1.536(4) . ?
C21 H21 1.0000 . ?
C1 C6 1.397(4) . ?
C28 C25 1.524(4) . ?
C28 C6 1.528(4) . ?
C28 C38 1.538(4) . ?
C28 H28 1.0000 . ?
C16 O8 1.376(3) . ?
C16 C15 1.387(4) . ?
C16 C17 1.391(4) . ?
C5 C6 1.392(3) . ?
C5 H13 0.9500 . ?
C26 C25 1.390(4) . ?
C26 C27 1.401(4) . ?
C26 H26 0.9500 . ?
O8 H8 0.8400 . ?
C29 C30 1.521(4) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C18 C17 1.399(4) . ?
C20 C15 1.388(4) . ?
C32 C33 1.527(4) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C27 C22 1.392(4) . ?
C35 C36 1.524(4) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
O12 C24 1.384(4) . ?
O12 H12A 0.8400 . ?
C22 C23 1.385(4) . ?
O11 C23 1.383(4) . ?
O11 H11 0.8400 . ?
C25 C24 1.396(4) . ?
C33 C34 1.512(5) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C38 C39 1.518(4) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C36 C37 1.508(4) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C23 C24 1.384(5) . ?
C30 C31 1.514(4) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C39 C40 1.520(5) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
O13 C41 1.264(3) . ?
C50 N1 1.314(4) . ?
C50 C49 1.466(4) . ?
C50 C41 1.471(4) . ?
N1 N2 1.317(3) . ?
C49 C48 1.397(4) . ?
C49 C44 1.407(4) . ?
N2 C51 1.392(4) . ?
N2 H17 0.8800 . ?
C44 C45 1.400(4) . ?
C44 C43 1.442(4) . ?
C41 C42 1.435(4) . ?
C45 C46 1.374(5) . ?
C45 H45 0.9500 . ?
C42 C43 1.343(4) . ?
C42 H42 0.9500 . ?
C47 C46 1.384(4) . ?
C47 C48 1.385(4) . ?
C47 H47 0.9500 . ?
C48 H48 0.9500 . ?
C43 H43 0.9500 . ?
C46 H46 0.9500 . ?
C52 C51 1.366(5) . ?
C52 C53 1.374(5) . ?
C52 H52 0.9500 . ?
C51 N3 1.323(5) . ?
N3 C55 1.345(6) . ?
C53 C54 1.355(6) . ?
C53 H53 0.9500 . ?
C54 C55 1.344(7) . ?
C54 H54 0.9500 . ?
C55 H55 0.9500 . ?
N6 C66 1.327(4) . ?
N6 C70 1.343(4) . ?
N4 N5 1.303(4) . ?
N4 C65 1.331(4) . ?
C67 C68 1.380(4) . ?
C67 C66 1.390(4) . ?
C67 H67 0.9500 . ?
C66 N5 1.405(4) . ?
C70 C69 1.367(4) . ?
C70 H70 0.9500 . ?
N5 H5A 0.8800 . ?
C69 C68 1.385(4) . ?
C69 H69 0.9500 . ?
C68 H68 0.9500 . ?
C65 C64 1.415(6) . ?
C65 C56 1.484(6) . ?
C59 C60 1.360(9) . ?
C59 C64 1.430(6) . ?
C59 C58 1.447(8) . ?
O14 C56 1.231(5) . ?
C56 C57 1.446(6) . ?
C64 C63 1.392(6) . ?
C63 C62 1.388(6) . ?
C63 H63 0.9500 . ?
C61 C60 1.380(9) . ?
C61 C62 1.433(8) . ?
C61 H61 0.9500 . ?
C57 C58 1.309(8) . ?
C57 H57 0.9500 . ?
C62 H62 0.9500 . ?
C60 H60 0.9500 . ?
C58 H58 0.9500 . ?
O1M C1M2 1.404(8) . ?
O1M H1M 0.8400 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C1M2 H1M1 0.9800 . ?
C1M2 H1M2 0.9800 . ?
C1M2 H1M3 0.9800 . ?
C2M O2M 1.525(19) . ?
C2M H2M1 0.9800 . ?
C2M H2M2 0.9800 . ?
C2M H2M3 0.9800 . ?
C3M O3M 1.557(19) . ?
C3M H3M1 0.9800 . ?
C3M H3M2 0.9800 . ?
C3M H3M3 0.9800 . ?
O2M H2M 0.8400 . ?
O3M H3M 0.8400 . ?

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
C10 O6 H6 109.5 . . ?
C8 O4 H4 109.5 . . ?
C3 O3 H3 109.5 . . ?
H1W O1W H2W 109(4) . . ?
C9 O5 H5 109.5 . . ?
C29 C7 C13 113.4(2) . . ?
C29 C7 C4 111.5(2) . . ?
C13 C7 C4 109.3(2) . . ?
C29 C7 H7 107.5 . . ?
C13 C7 H7 107.5 . . ?
C4 C7 H7 107.5 . . ?
C15 O7 H7A 109.5 . . ?
O5 C9 C10 116.0(2) . . ?
O5 C9 C8 124.2(2) . . ?
C10 C9 C8 119.7(2) . . ?
C2 O2 H2 109.5 . . ?
C22 O10 H10 109.5 . . ?
C1 O1 H1 109.5 . . ?
C11 C12 C13 123.0(2) . . ?
C11 C12 H12 118.5 . . ?
C13 C12 H12 118.5 . . ?
O6 C10 C9 119.7(2) . . ?
O6 C10 C11 118.8(2) . . ?
C9 C10 C11 121.5(2) . . ?
C17 O9 H9 109.4 . . ?
O2 C2 C1 123.6(2) . . ?
O2 C2 C3 116.0(2) . . ?
C1 C2 C3 120.4(2) . . ?
O4 C8 C13 123.8(2) . . ?
O4 C8 C9 115.5(2) . . ?
C13 C8 C9 120.6(2) . . ?
C8 C13 C12 117.8(2) . . ?
C8 C13 C7 120.8(2) . . ?
C12 C13 C7 121.2(2) . . ?
C12 C11 C10 117.4(2) . . ?
C12 C11 C14 123.6(2) . . ?
C10 C11 C14 119.0(2) . . ?
C5 C4 C3 117.5(2) . . ?
C5 C4 C7 121.2(2) . . ?
C3 C4 C7 121.3(2) . . ?
C11 C14 C20 109.8(2) . . ?
C11 C14 C32 114.0(2) . . ?
C20 C14 C32 111.4(2) . . ?
C11 C14 H14 107.1 . . ?
C20 C14 H14 107.1 . . ?
C32 C14 H14 107.1 . . ?
C18 C19 C20 123.5(2) . . ?
C18 C19 H19 118.3 . . ?
C20 C19 H19 118.3 . . ?
O3 C3 C2 120.0(2) . . ?
O3 C3 C4 119.4(2) . . ?
C2 C3 C4 120.5(2) . . ?
C18 C21 C27 110.9(2) . . ?
C18 C21 C35 111.6(2) . . ?
C27 C21 C35 113.7(2) . . ?
C18 C21 H21 106.8 . . ?
C27 C21 H21 106.8 . . ?
C35 C21 H21 106.8 . . ?
O1 C1 C2 116.6(2) . . ?
O1 C1 C6 122.8(2) . . ?
C2 C1 C6 120.6(2) . . ?
C25 C28 C6 111.5(2) . . ?
C25 C28 C38 115.5(2) . . ?
C6 C28 C38 110.4(2) . . ?
C25 C28 H28 106.3 . . ?
C6 C28 H28 106.3 . . ?
C38 C28 H28 106.3 . . ?
O8 C16 C15 121.2(3) . . ?
O8 C16 C17 118.6(3) . . ?
C15 C16 C17 120.2(2) . . ?
C4 C5 C6 123.4(2) . . ?
C4 C5 H13 118.3 . . ?
C6 C5 H13 118.3 . . ?
C25 C26 C27 123.5(3) . . ?
C25 C26 H26 118.2 . . ?
C27 C26 H26 118.2 . . ?
C16 O8 H8 109.5 . . ?
C30 C29 C7 114.6(2) . . ?
C30 C29 H29A 108.6 . . ?
C7 C29 H29A 108.6 . . ?
C30 C29 H29B 108.6 . . ?
C7 C29 H29B 108.6 . . ?
H29A C29 H29B 107.6 . . ?
C19 C18 C17 117.7(2) . . ?
C19 C18 C21 120.5(2) . . ?
C17 C18 C21 121.8(2) . . ?
C15 C20 C19 117.2(2) . . ?
C15 C20 C14 122.5(2) . . ?
C19 C20 C14 120.3(2) . . ?
C5 C6 C1 117.4(2) . . ?
C5 C6 C28 120.8(2) . . ?
C1 C6 C28 121.8(2) . . ?
C33 C32 C14 113.4(2) . . ?
C33 C32 H32A 108.9 . . ?
C14 C32 H32A 108.9 . . ?
C33 C32 H32B 108.9 . . ?
C14 C32 H32B 108.9 . . ?
H32A C32 H32B 107.7 . . ?
O9 C17 C16 121.8(2) . . ?
O9 C17 C18 118.0(3) . . ?
C16 C17 C18 120.2(2) . . ?
O7 C15 C16 114.9(2) . . ?
O7 C15 C20 123.9(2) . . ?
C16 C15 C20 121.2(2) . . ?
C22 C27 C26 117.8(3) . . ?
C22 C27 C21 119.6(2) . . ?
C26 C27 C21 122.6(2) . . ?
C36 C35 C21 112.5(2) . . ?
C36 C35 H35A 109.1 . . ?
C21 C35 H35A 109.1 . . ?
C36 C35 H35B 109.1 . . ?
C21 C35 H35B 109.1 . . ?
H35A C35 H35B 107.8 . . ?
C24 O12 H12A 109.5 . . ?
O10 C22 C23 115.2(3) . . ?
O10 C22 C27 124.7(3) . . ?
C23 C22 C27 120.1(3) . . ?
C23 O11 H11 109.5 . . ?
C26 C25 C24 116.3(3) . . ?
C26 C25 C28 123.4(2) . . ?
C24 C25 C28 120.2(2) . . ?
C34 C33 C32 112.8(3) . . ?
C34 C33 H33A 109.0 . . ?
C32 C33 H33A 109.0 . . ?
C34 C33 H33B 109.0 . . ?
C32 C33 H33B 109.0 . . ?
H33A C33 H33B 107.8 . . ?
C39 C38 C28 115.0(3) . . ?
C39 C38 H38A 108.5 . . ?
C28 C38 H38A 108.5 . . ?
C39 C38 H38B 108.5 . . ?
C28 C38 H38B 108.5 . . ?
H38A C38 H38B 107.5 . . ?
C37 C36 C35 112.3(3) . . ?
C37 C36 H36A 109.1 . . ?
C35 C36 H36A 109.1 . . ?
C37 C36 H36B 109.1 . . ?
C35 C36 H36B 109.1 . . ?
H36A C36 H36B 107.9 . . ?
O11 C23 C24 118.0(3) . . ?
O11 C23 C22 121.5(3) . . ?
C24 C23 C22 120.5(3) . . ?
C31 C30 C29 112.3(3) . . ?
C31 C30 H30A 109.1 . . ?
C29 C30 H30A 109.1 . . ?
C31 C30 H30B 109.1 . . ?
C29 C30 H30B 109.1 . . ?
H30A C30 H30B 107.9 . . ?
C23 C24 O12 120.0(3) . . ?
C23 C24 C25 121.7(3) . . ?
O12 C24 C25 118.3(3) . . ?
C38 C39 C40 112.2(3) . . ?
C38 C39 H39A 109.2 . . ?
C40 C39 H39A 109.2 . . ?
C38 C39 H39B 109.2 . . ?
C40 C39 H39B 109.2 . . ?
H39A C39 H39B 107.9 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
N1 C50 C49 115.9(3) . . ?
N1 C50 C41 124.5(3) . . ?
C49 C50 C41 119.5(2) . . ?
C50 N1 N2 119.8(3) . . ?
C48 C49 C44 119.2(3) . . ?
C48 C49 C50 121.9(3) . . ?
C44 C49 C50 118.8(3) . . ?
N1 N2 C51 119.4(3) . . ?
N1 N2 H17 120.3 . . ?
C51 N2 H17 120.3 . . ?
C45 C44 C49 119.2(3) . . ?
C45 C44 C43 121.4(3) . . ?
C49 C44 C43 119.4(3) . . ?
O13 C41 C42 121.5(3) . . ?
O13 C41 C50 120.4(3) . . ?
C42 C41 C50 118.1(3) . . ?
C46 C45 C44 120.9(3) . . ?
C46 C45 H45 119.6 . . ?
C44 C45 H45 119.6 . . ?
C43 C42 C41 121.0(3) . . ?
C43 C42 H42 119.5 . . ?
C41 C42 H42 119.5 . . ?
C46 C47 C48 120.5(3) . . ?
C46 C47 H47 119.8 . . ?
C48 C47 H47 119.8 . . ?
C47 C48 C49 120.3(3) . . ?
C47 C48 H48 119.8 . . ?
C49 C48 H48 119.8 . . ?
C42 C43 C44 123.1(3) . . ?
C42 C43 H43 118.5 . . ?
C44 C43 H43 118.5 . . ?
C45 C46 C47 120.0(3) . . ?
C45 C46 H46 120.0 . . ?
C47 C46 H46 120.0 . . ?
C51 C52 C53 117.9(4) . . ?
C51 C52 H52 121.1 . . ?
C53 C52 H52 121.1 . . ?
N3 C51 C52 122.2(3) . . ?
N3 C51 N2 114.9(4) . . ?
C52 C51 N2 123.0(3) . . ?
C51 N3 C55 117.9(4) . . ?
C54 C53 C52 120.9(5) . . ?
C54 C53 H53 119.6 . . ?
C52 C53 H53 119.6 . . ?
C55 C54 C53 117.5(4) . . ?
C55 C54 H54 121.2 . . ?
C53 C54 H54 121.2 . . ?
C54 C55 N3 123.6(4) . . ?
C54 C55 H55 118.2 . . ?
N3 C55 H55 118.2 . . ?
C66 N6 C70 116.0(2) . . ?
N5 N4 C65 117.7(3) . . ?
C68 C67 C66 117.2(3) . . ?
C68 C67 H67 121.4 . . ?
C66 C67 H67 121.4 . . ?
N6 C66 C67 124.9(3) . . ?
N6 C66 N5 112.8(3) . . ?
C67 C66 N5 122.3(3) . . ?
N6 C70 C69 124.2(3) . . ?
N6 C70 H70 117.9 . . ?
C69 C70 H70 117.9 . . ?
N4 N5 C66 119.5(3) . . ?
N4 N5 H5A 120.2 . . ?
C66 N5 H5A 120.2 . . ?
C70 C69 C68 118.5(3) . . ?
C70 C69 H69 120.8 . . ?
C68 C69 H69 120.8 . . ?
C67 C68 C69 119.3(3) . . ?
C67 C68 H68 120.4 . . ?
C69 C68 H68 120.4 . . ?
N4 C65 C64 116.2(4) . . ?
N4 C65 C56 122.9(4) . . ?
C64 C65 C56 120.9(4) . . ?
C60 C59 C64 120.0(6) . . ?
C60 C59 C58 123.7(6) . . ?
C64 C59 C58 116.3(5) . . ?
O14 C56 C57 122.3(5) . . ?
O14 C56 C65 122.5(4) . . ?
C57 C56 C65 115.2(5) . . ?
C63 C64 C65 123.1(4) . . ?
C63 C64 C59 116.4(5) . . ?
C65 C64 C59 120.5(5) . . ?
C62 C63 C64 124.4(5) . . ?
C62 C63 H63 117.8 . . ?
C64 C63 H63 117.8 . . ?
C60 C61 C62 118.6(6) . . ?
C60 C61 H61 120.7 . . ?
C62 C61 H61 120.7 . . ?
C58 C57 C56 122.3(6) . . ?
C58 C57 H57 118.8 . . ?
C56 C57 H57 118.8 . . ?
C63 C62 C61 117.3(6) . . ?
C63 C62 H62 121.4 . . ?
C61 C62 H62 121.4 . . ?
C59 C60 C61 123.3(6) . . ?
C59 C60 H60 118.4 . . ?
C61 C60 H60 118.4 . . ?
C57 C58 C59 124.6(5) . . ?
C57 C58 H58 117.7 . . ?
C59 C58 H58 117.7 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O3M C3M H3M1 109.5 . . ?
O3M C3M H3M2 109.5 . . ?
H3M1 C3M H3M2 109.5 . . ?
O3M C3M H3M3 109.5 . . ?
H3M1 C3M H3M3 109.5 . . ?
H3M2 C3M H3M3 109.5 . . ?
C3M O3M H3M 109.5 . . ?

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
O5 C9 C10 O6 -3.6(3) . . . . ?
C8 C9 C10 O6 -179.6(2) . . . . ?
O5 C9 C10 C11 174.9(2) . . . . ?
C8 C9 C10 C11 -1.1(4) . . . . ?
O5 C9 C8 O4 6.6(4) . . . . ?
C10 C9 C8 O4 -177.7(2) . . . . ?
O5 C9 C8 C13 -173.2(2) . . . . ?
C10 C9 C8 C13 2.5(4) . . . . ?
O4 C8 C13 C12 178.2(2) . . . . ?
C9 C8 C13 C12 -2.0(4) . . . . ?
O4 C8 C13 C7 -6.2(4) . . . . ?
C9 C8 C13 C7 173.6(2) . . . . ?
C11 C12 C13 C8 0.0(4) . . . . ?
C11 C12 C13 C7 -175.6(2) . . . . ?
C29 C7 C13 C8 163.6(2) . . . . ?
C4 C7 C13 C8 -71.3(3) . . . . ?
C29 C7 C13 C12 -20.9(3) . . . . ?
C4 C7 C13 C12 104.2(3) . . . . ?
C13 C12 C11 C10 1.3(4) . . . . ?
C13 C12 C11 C14 178.6(2) . . . . ?
O6 C10 C11 C12 177.7(2) . . . . ?
C9 C10 C11 C12 -0.8(4) . . . . ?
O6 C10 C11 C14 0.3(3) . . . . ?
C9 C10 C11 C14 -178.2(2) . . . . ?
C29 C7 C4 C5 51.4(3) . . . . ?
C13 C7 C4 C5 -74.7(3) . . . . ?
C29 C7 C4 C3 -131.2(2) . . . . ?
C13 C7 C4 C3 102.6(3) . . . . ?
C12 C11 C14 C20 -107.0(3) . . . . ?
C10 C11 C14 C20 70.3(3) . . . . ?
C12 C11 C14 C32 18.8(3) . . . . ?
C10 C11 C14 C32 -163.9(2) . . . . ?
O2 C2 C3 O3 2.8(3) . . . . ?
C1 C2 C3 O3 -178.4(2) . . . . ?
O2 C2 C3 C4 178.3(2) . . . . ?
C1 C2 C3 C4 -2.9(4) . . . . ?
C5 C4 C3 O3 178.9(2) . . . . ?
C7 C4 C3 O3 1.5(3) . . . . ?
C5 C4 C3 C2 3.4(4) . . . . ?
C7 C4 C3 C2 -174.0(2) . . . . ?
O2 C2 C1 O1 -2.8(4) . . . . ?
C3 C2 C1 O1 178.5(2) . . . . ?
O2 C2 C1 C6 177.7(2) . . . . ?
C3 C2 C1 C6 -1.0(4) . . . . ?
C3 C4 C5 C6 -0.1(4) . . . . ?
C7 C4 C5 C6 177.4(2) . . . . ?
C13 C7 C29 C30 -172.3(2) . . . . ?
C4 C7 C29 C30 63.8(3) . . . . ?
C20 C19 C18 C17 1.8(4) . . . . ?
C20 C19 C18 C21 -178.6(2) . . . . ?
C27 C21 C18 C19 -74.6(3) . . . . ?
C35 C21 C18 C19 53.2(3) . . . . ?
C27 C21 C18 C17 105.0(3) . . . . ?
C35 C21 C18 C17 -127.2(3) . . . . ?
C18 C19 C20 C15 -2.3(4) . . . . ?
C18 C19 C20 C14 177.6(2) . . . . ?
C11 C14 C20 C15 -105.9(3) . . . . ?
C32 C14 C20 C15 126.9(3) . . . . ?
C11 C14 C20 C19 74.2(3) . . . . ?
C32 C14 C20 C19 -53.0(3) . . . . ?
C4 C5 C6 C1 -3.6(4) . . . . ?
C4 C5 C6 C28 175.3(2) . . . . ?
O1 C1 C6 C5 -175.3(2) . . . . ?
C2 C1 C6 C5 4.2(4) . . . . ?
O1 C1 C6 C28 5.8(4) . . . . ?
C2 C1 C6 C28 -174.8(2) . . . . ?
C25 C28 C6 C5 79.7(3) . . . . ?
C38 C28 C6 C5 -50.1(3) . . . . ?
C25 C28 C6 C1 -101.4(3) . . . . ?
C38 C28 C6 C1 128.8(3) . . . . ?
C11 C14 C32 C33 173.1(2) . . . . ?
C20 C14 C32 C33 -62.0(3) . . . . ?
O8 C16 C17 O9 1.6(4) . . . . ?
C15 C16 C17 O9 -177.8(2) . . . . ?
O8 C16 C17 C18 179.6(2) . . . . ?
C15 C16 C17 C18 0.2(4) . . . . ?
C19 C18 C17 O9 177.4(2) . . . . ?
C21 C18 C17 O9 -2.2(4) . . . . ?
C19 C18 C17 C16 -0.6(4) . . . . ?
C21 C18 C17 C16 179.7(2) . . . . ?
O8 C16 C15 O7 -0.8(4) . . . . ?
C17 C16 C15 O7 178.7(2) . . . . ?
O8 C16 C15 C20 179.8(2) . . . . ?
C17 C16 C15 C20 -0.8(4) . . . . ?
C19 C20 C15 O7 -177.6(2) . . . . ?
C14 C20 C15 O7 2.5(4) . . . . ?
C19 C20 C15 C16 1.8(4) . . . . ?
C14 C20 C15 C16 -178.1(2) . . . . ?
C25 C26 C27 C22 -1.7(4) . . . . ?
C25 C26 C27 C21 179.1(2) . . . . ?
C18 C21 C27 C22 -77.5(3) . . . . ?
C35 C21 C27 C22 155.8(2) . . . . ?
C18 C21 C27 C26 101.7(3) . . . . ?
C35 C21 C27 C26 -24.9(3) . . . . ?
C18 C21 C35 C36 62.0(3) . . . . ?
C27 C21 C35 C36 -171.8(2) . . . . ?
C26 C27 C22 O10 -176.9(2) . . . . ?
C21 C27 C22 O10 2.4(4) . . . . ?
C26 C27 C22 C23 2.8(4) . . . . ?
C21 C27 C22 C23 -177.9(3) . . . . ?
C27 C26 C25 C24 -1.2(4) . . . . ?
C27 C26 C25 C28 175.6(2) . . . . ?
C6 C28 C25 C26 -97.0(3) . . . . ?
C38 C28 C25 C26 30.1(4) . . . . ?
C6 C28 C25 C24 79.7(3) . . . . ?
C38 C28 C25 C24 -153.2(3) . . . . ?
C14 C32 C33 C34 177.8(3) . . . . ?
C25 C28 C38 C39 62.2(3) . . . . ?
C6 C28 C38 C39 -170.1(2) . . . . ?
C21 C35 C36 C37 -178.7(3) . . . . ?
O10 C22 C23 O11 -1.1(4) . . . . ?
C27 C22 C23 O11 179.1(3) . . . . ?
O10 C22 C23 C24 178.6(3) . . . . ?
C27 C22 C23 C24 -1.2(5) . . . . ?
C7 C29 C30 C31 -169.3(3) . . . . ?
O11 C23 C24 O12 -0.5(5) . . . . ?
C22 C23 C24 O12 179.8(3) . . . . ?
O11 C23 C24 C25 177.8(3) . . . . ?
C22 C23 C24 C25 -1.9(5) . . . . ?
C26 C25 C24 C23 3.0(4) . . . . ?
C28 C25 C24 C23 -173.9(3) . . . . ?
C26 C25 C24 O12 -178.7(3) . . . . ?
C28 C25 C24 O12 4.4(4) . . . . ?
C28 C38 C39 C40 177.4(3) . . . . ?
C49 C50 N1 N2 179.4(2) . . . . ?
C41 C50 N1 N2 -1.3(4) . . . . ?
N1 C50 C49 C48 0.4(4) . . . . ?
C41 C50 C49 C48 -179.0(3) . . . . ?
N1 C50 C49 C44 -179.2(2) . . . . ?
C41 C50 C49 C44 1.4(4) . . . . ?
C50 N1 N2 C51 177.3(3) . . . . ?
C48 C49 C44 C45 -0.5(4) . . . . ?
C50 C49 C44 C45 179.1(2) . . . . ?
C48 C49 C44 C43 179.8(3) . . . . ?
C50 C49 C44 C43 -0.6(4) . . . . ?
N1 C50 C41 O13 -0.5(4) . . . . ?
C49 C50 C41 O13 178.8(2) . . . . ?
N1 C50 C41 C42 179.0(3) . . . . ?
C49 C50 C41 C42 -1.6(4) . . . . ?
C49 C44 C45 C46 0.3(4) . . . . ?
C43 C44 C45 C46 180.0(3) . . . . ?
O13 C41 C42 C43 -179.3(3) . . . . ?
C50 C41 C42 C43 1.1(4) . . . . ?
C46 C47 C48 C49 -0.3(5) . . . . ?
C44 C49 C48 C47 0.6(4) . . . . ?
C50 C49 C48 C47 -179.1(3) . . . . ?
C41 C42 C43 C44 -0.4(4) . . . . ?
C45 C44 C43 C42 -179.6(3) . . . . ?
C49 C44 C43 C42 0.1(4) . . . . ?
C44 C45 C46 C47 0.0(5) . . . . ?
C48 C47 C46 C45 0.0(5) . . . . ?
C53 C52 C51 N3 1.7(6) . . . . ?
C53 C52 C51 N2 -178.6(3) . . . . ?
N1 N2 C51 N3 -179.7(3) . . . . ?
N1 N2 C51 C52 0.7(5) . . . . ?
C52 C51 N3 C55 -0.1(7) . . . . ?
N2 C51 N3 C55 -179.7(4) . . . . ?
C51 C52 C53 C54 -2.6(6) . . . . ?
C52 C53 C54 C55 1.8(8) . . . . ?
C53 C54 C55 N3 -0.1(9) . . . . ?
C51 N3 C55 C54 -0.8(9) . . . . ?
C70 N6 C66 C67 0.8(4) . . . . ?
C70 N6 C66 N5 -178.6(2) . . . . ?
C68 C67 C66 N6 -0.3(4) . . . . ?
C68 C67 C66 N5 179.1(3) . . . . ?
C66 N6 C70 C69 -1.2(4) . . . . ?
C65 N4 N5 C66 -173.5(3) . . . . ?
N6 C66 N5 N4 169.8(2) . . . . ?
C67 C66 N5 N4 -9.6(4) . . . . ?
N6 C70 C69 C68 1.0(4) . . . . ?
C66 C67 C68 C69 0.1(4) . . . . ?
C70 C69 C68 C67 -0.4(4) . . . . ?
N5 N4 C65 C64 179.6(3) . . . . ?
N5 N4 C65 C56 0.8(4) . . . . ?
N4 C65 C56 O14 -3.5(6) . . . . ?
C64 C65 C56 O14 177.8(4) . . . . ?
N4 C65 C56 C57 174.5(3) . . . . ?
C64 C65 C56 C57 -4.3(5) . . . . ?
N4 C65 C64 C63 2.5(5) . . . . ?
C56 C65 C64 C63 -178.7(3) . . . . ?
N4 C65 C64 C59 -176.6(3) . . . . ?
C56 C65 C64 C59 2.3(5) . . . . ?
C60 C59 C64 C63 0.4(5) . . . . ?
C58 C59 C64 C63 -179.3(3) . . . . ?
C60 C59 C64 C65 179.5(4) . . . . ?
C58 C59 C64 C65 -0.2(5) . . . . ?
C65 C64 C63 C62 -179.1(3) . . . . ?
C59 C64 C63 C62 -0.1(5) . . . . ?
O14 C56 C57 C58 -177.6(4) . . . . ?
C65 C56 C57 C58 4.4(6) . . . . ?
C64 C63 C62 C61 -0.1(6) . . . . ?
C60 C61 C62 C63 0.0(7) . . . . ?
C64 C59 C60 C61 -0.6(7) . . . . ?
C58 C59 C60 C61 179.0(5) . . . . ?
C62 C61 C60 C59 0.4(8) . . . . ?
C56 C57 C58 C59 -2.6(7) . . . . ?
C60 C59 C58 C57 -179.4(5) . . . . ?
C64 C59 C58 C57 0.3(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        27.20
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.671
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.058

_database_code_depnum_ccdc_archive 'CCDC 1002506'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2cp55f

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            
'C-propylpyrogallol[4]arene with 1-(2-pyridylazo)-2-napthol'
_chemical_formula_moiety         
'C40 H48 O12, 2(C15 H11 O1 N3), C2 H6 O1, 2(H2 O1)'
_chemical_formula_sum            'C72 H80 N6 O17'
_chemical_melting_point          ?

_exptl_crystal_description       prism
_exptl_crystal_colour            orange

_diffrn_ambient_temperature      173(2)
_chemical_formula_weight         1301.42

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'
O O 0.0106 0.0060 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?

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

_cell_length_a                   12.6569(10)
_cell_length_b                   15.7620(13)
_cell_length_c                   18.771(2)
_cell_angle_alpha                109.6650(10)
_cell_angle_beta                 92.1130(10)
_cell_angle_gamma                111.9200(10)
_cell_volume                     3214.3(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9200
_cell_measurement_theta_min      2.3
_cell_measurement_theta_max      27.0
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1380
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_process_details   
;
 Data were corrected for decay and absorption using the program SADABS 
 (Sheldrick, G. M. (2003). SADABS. Version 2.10. University of
 Göttingen, Germany).
;

_exptl_special_details           
; 
 ? 
;
_diffrn_radiation_probe          ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.0
_diffrn_reflns_number            37001
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.52
_diffrn_reflns_theta_max         27.06
_reflns_number_total             13987
_reflns_number_gt                10343
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2008)'
_computing_structure_solution    'SHELXS-1997 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-1997 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-SEED, Barbour, 2001'
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. There is minor residual electron 
 density near a disordered ethanol that is minor disorder that is not included.
 There is a lone oxygen atom that is water and the hydrogen atoms are not modeled
 but they are included in the sum formula. The hydrogens on the pyrogallol[4]arene
 are disordered but not included which accounts for the short bond distances.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0637P)²+1.1943P] where P=(Fo²+2Fc²)/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         13987
_refine_ls_number_parameters     889
_refine_ls_number_restraints     46
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0479
_refine_ls_wR_factor_ref         0.1371
_refine_ls_wR_factor_gt          0.1234
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.056
_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
O1 O -0.39349(11) 0.71694(9) 0.14509(7) 0.0279(3) Uani 1 1 d . . .
H1 H -0.4237 0.6787 0.0992 0.034 Uiso 1 1 calc R . .
N1 N 0.22189(13) 0.31363(11) 0.18033(9) 0.0273(3) Uani 1 1 d . . .
C1 C -0.16072(14) 0.72484(12) 0.26938(10) 0.0221(4) Uani 1 1 d . . .
H13 H -0.1139 0.7649 0.3190 0.026 Uiso 1 1 calc R . .
O2 O -0.35867(11) 0.56251(9) 0.05182(7) 0.0288(3) Uani 1 1 d . . .
H2 H -0.3721 0.5022 0.0364 0.035 Uiso 1 1 calc R . .
N2 N 0.14627(13) 0.32774(11) 0.14229(9) 0.0280(3) Uani 1 1 d . . .
C2 C -0.24576(14) 0.75023(12) 0.24522(10) 0.0221(4) Uani 1 1 d . . .
O3 O -0.20436(11) 0.49989(9) 0.10286(7) 0.0267(3) Uani 1 1 d . . .
H3 H -0.1454 0.4952 0.1201 0.032 Uiso 1 1 calc R . .
N3 N 0.04790(13) 0.31075(11) 0.03082(9) 0.0277(3) Uani 1 1 d . . .
C3 C -0.31210(14) 0.69161(12) 0.17169(10) 0.0219(4) Uani 1 1 d . . .
O4 O -0.00047(10) 0.47619(9) 0.12817(7) 0.0256(3) Uani 1 1 d . . .
H4 H 0.0232 0.4402 0.0948 0.031 Uiso 1 1 calc R . .
N4 N 0.63154(13) 0.50208(11) 0.29524(9) 0.0259(3) Uani 1 1 d . . .
C4 C -0.29498(14) 0.60997(13) 0.12515(10) 0.0225(4) Uani 1 1 d . . .
O5 O 0.16140(12) 0.52039(9) 0.04420(7) 0.0314(3) Uani 1 1 d . . .
H5 H 0.1930 0.5396 0.0106 0.038 Uiso 1 1 calc R . .
N5 N 0.67263(14) 0.43651(11) 0.25997(9) 0.0278(3) Uani 1 1 d . . .
C5 C -0.21127(15) 0.58499(12) 0.15216(10) 0.0219(4) Uani 1 1 d . . .
O6 O 0.30284(12) 0.71455(9) 0.06853(8) 0.0317(3) Uani 1 1 d . . .
H6 H 0.3072 0.7652 0.0609 0.038 Uiso 1 1 calc R . .
N6 N 0.79139(15) 0.35655(13) 0.26036(9) 0.0355(4) Uani 1 1 d . . .
C6 C -0.14042(14) 0.64363(12) 0.22459(9) 0.0208(3) Uani 1 1 d . . .
O7 O 0.26676(11) 0.86572(10) 0.04660(7) 0.0287(3) Uani 1 1 d . . .
H7 H 0.2306 0.8473 0.0019 0.034 Uiso 1 1 calc R . .
C7 C -0.04059(14) 0.62227(12) 0.25186(9) 0.0214(3) Uani 1 1 d . . .
H16 H -0.0713 0.5496 0.2398 0.026 Uiso 1 1 calc R . .
O8 O 0.14434(12) 0.95077(10) -0.00339(7) 0.0312(3) Uani 1 1 d . . .
H8 H 0.0921 0.9677 -0.0140 0.037 Uiso 1 1 calc R . .
C8 C 0.13136(14) 0.74536(12) 0.22141(9) 0.0206(3) Uani 1 1 d . . .
H17 H 0.1222 0.7962 0.2621 0.025 Uiso 1 1 calc R . .
O9 O 0.05507(11) 1.06386(9) 0.09285(7) 0.0271(3) Uani 1 1 d . . .
H9 H 0.0297 1.0972 0.1270 0.033 Uiso 1 1 calc R . .
C9 C 0.05658(14) 0.64760(12) 0.20616(9) 0.0206(3) Uani 1 1 d . . .
O10 O -0.07397(11) 1.14965(9) 0.18047(7) 0.0293(3) Uani 1 1 d . . .
H10 H -0.1262 1.1513 0.1527 0.035 Uiso 1 1 calc R . .
C10 C 0.07199(14) 0.57410(12) 0.14644(9) 0.0210(3) Uani 1 1 d . . .
O11 O -0.30714(13) 1.05330(11) 0.15694(8) 0.0399(3) Uani 1 1 d . . .
H11 H -0.3715 1.0060 0.1347 0.048 Uiso 1 1 calc R . .
C11 C 0.15501(15) 0.59846(12) 0.10177(9) 0.0218(4) Uani 1 1 d . . .
O12 O -0.40891(11) 0.89682(10) 0.20321(9) 0.0362(3) Uani 1 1 d . . .
H12 H -0.4275 0.8358 0.1888 0.043 Uiso 1 1 calc R . .
C12 C 0.22650(15) 0.69657(13) 0.11774(10) 0.0223(4) Uani 1 1 d . . .
O13 O 0.12424(13) 0.44516(12) 0.26471(8) 0.0437(4) Uani 1 1 d . . .
C13 C 0.21885(14) 0.77245(12) 0.17999(9) 0.0208(3) Uani 1 1 d . . .
O14 O 0.53259(12) 0.38727(10) 0.13640(7) 0.0338(3) Uani 1 1 d . . .
C14 C 0.30207(15) 0.88048(12) 0.20111(10) 0.0223(4) Uani 1 1 d . . .
H14 H 0.3649 0.8803 0.1704 0.027 Uiso 1 1 calc R . .
O15A O 0.530(2) 0.9592(10) 0.0312(10) 0.191(7) Uani 0.298(11) 1 d PDU A 2
H15A H 0.5744 1.0131 0.0294 0.229 Uiso 0.298(11) 1 calc PR A 2
C15 C 0.19538(14) 0.99487(12) 0.22655(10) 0.0214(3) Uani 1 1 d . . .
H15 H 0.2071 1.0042 0.2794 0.026 Uiso 1 1 calc R . .
O16 O -0.54513(11) 0.63532(10) 0.01224(7) 0.0297(3) Uani 1 1 d . . .
C16 C 0.24084(14) 0.93563(12) 0.17607(10) 0.0214(3) Uani 1 1 d . . .
O17 O 0.16965(13) 0.75513(11) -0.10800(8) 0.0401(3) Uani 1 1 d . . .
C17 C 0.22291(15) 0.92385(13) 0.09922(10) 0.0230(4) Uani 1 1 d . . .
C18 C 0.16088(15) 0.96778(13) 0.07363(10) 0.0228(4) Uani 1 1 d . . .
C19 C 0.11644(15) 1.02582(12) 0.12549(10) 0.0216(3) Uani 1 1 d . . .
C20 C 0.13356(14) 1.04105(12) 0.20333(10) 0.0210(3) Uani 1 1 d . . .
C21 C 0.08260(15) 1.10443(12) 0.25857(9) 0.0211(3) Uani 1 1 d . . .
H21 H 0.0988 1.1640 0.2455 0.025 Uiso 1 1 calc R . .
C22 C -0.09895(15) 0.97268(12) 0.27004(9) 0.0219(4) Uani 1 1 d . . .
H22 H -0.0495 0.9543 0.2951 0.026 Uiso 1 1 calc R . .
C23 C -0.04876(15) 1.04972(12) 0.24503(9) 0.0215(3) Uani 1 1 d . . .
C24 C -0.12238(16) 1.07483(13) 0.20764(10) 0.0241(4) Uani 1 1 d . . .
C25 C -0.24222(16) 1.02345(14) 0.19477(10) 0.0271(4) Uani 1 1 d . . .
C26 C -0.28960(15) 0.94609(13) 0.22013(10) 0.0264(4) Uani 1 1 d . . .
C27 C -0.21843(15) 0.92115(12) 0.26007(10) 0.0228(4) Uani 1 1 d . . .
C28 C -0.26611(15) 0.84066(13) 0.29284(10) 0.0238(4) Uani 1 1 d . . .
H28 H -0.3518 0.8202 0.2872 0.029 Uiso 1 1 calc R . .
C29 C 0.00415(16) 0.67513(13) 0.33906(10) 0.0254(4) Uani 1 1 d . . .
H29A H 0.0382 0.7473 0.3520 0.030 Uiso 1 1 calc R . .
H29B H -0.0623 0.6595 0.3658 0.030 Uiso 1 1 calc R . .
C30 C 0.09439(17) 0.64742(15) 0.36931(11) 0.0323(4) Uani 1 1 d . . .
H30A H 0.0592 0.5761 0.3598 0.039 Uiso 1 1 calc R . .
H30B H 0.1591 0.6593 0.3407 0.039 Uiso 1 1 calc R . .
C31 C 0.1417(2) 0.70584(19) 0.45463(12) 0.0478(6) Uani 1 1 d . . .
H31A H 0.1996 0.6858 0.4715 0.072 Uiso 1 1 calc R . .
H31B H 0.0783 0.6930 0.4834 0.072 Uiso 1 1 calc R . .
H31C H 0.1779 0.7765 0.4642 0.072 Uiso 1 1 calc R . .
C32 C 0.36037(16) 0.92782(13) 0.28639(10) 0.0277(4) Uani 1 1 d . . .
H32A H 0.3003 0.9304 0.3183 0.033 Uiso 1 1 calc R . .
H32B H 0.3939 0.8849 0.2973 0.033 Uiso 1 1 calc R . .
C33 C 0.45551(17) 1.03146(14) 0.31062(12) 0.0384(5) Uani 1 1 d . . .
H33A H 0.5136 1.0303 0.2769 0.046 Uiso 1 1 calc R . .
H33B H 0.4215 1.0760 0.3036 0.046 Uiso 1 1 calc R . .
C34 C 0.5153(3) 1.0718(2) 0.39368(16) 0.0688(8) Uani 1 1 d . . .
H34A H 0.5759 1.1383 0.4066 0.103 Uiso 1 1 calc R . .
H34B H 0.5502 1.0285 0.4007 0.103 Uiso 1 1 calc R . .
H34C H 0.4585 1.0748 0.4275 0.103 Uiso 1 1 calc R . .
C35 C 0.13659(15) 1.14185(13) 0.34368(10) 0.0238(4) Uani 1 1 d . . .
H35A H 0.1186 1.0848 0.3595 0.029 Uiso 1 1 calc R . .
H35B H 0.2219 1.1752 0.3502 0.029 Uiso 1 1 calc R . .
C36 C 0.09202(17) 1.21358(14) 0.39566(10) 0.0303(4) Uani 1 1 d . . .
H36A H 0.1096 1.2705 0.3797 0.036 Uiso 1 1 calc R . .
H36B H 0.0068 1.1801 0.3894 0.036 Uiso 1 1 calc R . .
C37 C 0.1460(2) 1.25086(18) 0.47976(12) 0.0467(6) Uani 1 1 d . . .
H37A H 0.1156 1.2970 0.5111 0.070 Uiso 1 1 calc R . .
H37B H 0.2304 1.2848 0.4864 0.070 Uiso 1 1 calc R . .
H37C H 0.1270 1.1949 0.4962 0.070 Uiso 1 1 calc R . .
C38 C -0.21663(16) 0.88024(13) 0.37926(10) 0.0272(4) Uani 1 1 d . . .
H38A H -0.2437 0.8248 0.3973 0.033 Uiso 1 1 calc R . .
H38B H -0.1310 0.9067 0.3868 0.033 Uiso 1 1 calc R . .
C39 C -0.2515(2) 0.96090(15) 0.42817(11) 0.0386(5) Uani 1 1 d . . .
H39A H -0.2252 1.0162 0.4100 0.046 Uiso 1 1 calc R . .
H39B H -0.3371 0.9344 0.4214 0.046 Uiso 1 1 calc R . .
C40 C -0.2003(3) 0.9997(2) 0.51330(13) 0.0608(7) Uani 1 1 d . . .
H40A H -0.2245 1.0517 0.5423 0.091 Uiso 1 1 calc R . .
H40B H -0.1156 1.0268 0.5204 0.091 Uiso 1 1 calc R . .
H40C H -0.2280 0.9456 0.5320 0.091 Uiso 1 1 calc R . .
C41 C 0.19845(17) 0.42865(14) 0.29869(11) 0.0312(4) Uani 1 1 d . . .
C42 C 0.24792(16) 0.36125(13) 0.25718(10) 0.0266(4) Uani 1 1 d . . .
C43 C 0.33204(16) 0.34333(13) 0.29834(11) 0.0271(4) Uani 1 1 d . . .
C44 C 0.38365(17) 0.28006(14) 0.26061(11) 0.0314(4) Uani 1 1 d . . .
H44 H 0.3634 0.2469 0.2062 0.038 Uiso 1 1 calc R . .
C45 C 0.46357(18) 0.26548(15) 0.30162(12) 0.0359(5) Uani 1 1 d . . .
H45 H 0.4992 0.2236 0.2752 0.043 Uiso 1 1 calc R . .
C46 C 0.49245(18) 0.31200(16) 0.38190(13) 0.0390(5) Uani 1 1 d . . .
H46 H 0.5467 0.3010 0.4100 0.047 Uiso 1 1 calc R . .
C47 C 0.44218(18) 0.37352(15) 0.41990(12) 0.0365(5) Uani 1 1 d . . .
H47 H 0.4614 0.4044 0.4745 0.044 Uiso 1 1 calc R . .
C48 C 0.36278(17) 0.39141(14) 0.37926(11) 0.0307(4) Uani 1 1 d . . .
C49 C 0.31266(18) 0.45847(15) 0.41832(11) 0.0350(4) Uani 1 1 d . . .
H49 H 0.3342 0.4908 0.4727 0.042 Uiso 1 1 calc R . .
C50 C 0.23659(18) 0.47738(15) 0.38110(11) 0.0362(5) Uani 1 1 d . . .
H50 H 0.2075 0.5235 0.4095 0.043 Uiso 1 1 calc R . .
C51 C 0.12364(15) 0.28635(13) 0.06148(10) 0.0247(4) Uani 1 1 d . . .
C52 C 0.17631(17) 0.22805(14) 0.01928(11) 0.0299(4) Uani 1 1 d . . .
H52 H 0.2293 0.2124 0.0440 0.036 Uiso 1 1 calc R . .
C53 C 0.14883(17) 0.19352(14) -0.06017(11) 0.0313(4) Uani 1 1 d . . .
H53 H 0.1823 0.1528 -0.0914 0.038 Uiso 1 1 calc R . .
C54 C 0.07203(16) 0.21900(14) -0.09347(11) 0.0304(4) Uani 1 1 d . . .
H54 H 0.0525 0.1966 -0.1479 0.036 Uiso 1 1 calc R . .
C55 C 0.02447(17) 0.27731(14) -0.04645(11) 0.0310(4) Uani 1 1 d . . .
H55 H -0.0277 0.2949 -0.0698 0.037 Uiso 1 1 calc R . .
C56 C 0.50381(16) 0.45523(14) 0.17355(11) 0.0283(4) Uani 1 1 d . . .
C57 C 0.55273(15) 0.51329(13) 0.25601(10) 0.0252(4) Uani 1 1 d . . .
C58 C 0.51259(15) 0.58870(13) 0.29881(11) 0.0266(4) Uani 1 1 d . . .
C59 C 0.55339(17) 0.64419(14) 0.37767(11) 0.0311(4) Uani 1 1 d . . .
H59 H 0.6087 0.6333 0.4049 0.037 Uiso 1 1 calc R . .
C60 C 0.51377(18) 0.71473(15) 0.41634(12) 0.0375(5) Uani 1 1 d . . .
H60 H 0.5420 0.7518 0.4699 0.045 Uiso 1 1 calc R . .
C61 C 0.43307(19) 0.73196(16) 0.37758(13) 0.0398(5) Uani 1 1 d . . .
H61 H 0.4062 0.7805 0.4045 0.048 Uiso 1 1 calc R . .
C62 C 0.39242(18) 0.67819(16) 0.29993(13) 0.0375(5) Uani 1 1 d . . .
H62 H 0.3375 0.6901 0.2733 0.045 Uiso 1 1 calc R . .
C63 C 0.43099(16) 0.60629(14) 0.25966(11) 0.0300(4) Uani 1 1 d . . .
C64 C 0.38823(16) 0.54929(15) 0.17817(12) 0.0337(4) Uani 1 1 d . . .
H64 H 0.3340 0.5624 0.1521 0.040 Uiso 1 1 calc R . .
C65 C 0.42174(16) 0.47870(15) 0.13769(11) 0.0323(4) Uani 1 1 d . . .
H65 H 0.3906 0.4435 0.0842 0.039 Uiso 1 1 calc R . .
C66 C 0.75177(16) 0.42151(14) 0.30254(11) 0.0275(4) Uani 1 1 d . . .
C67 C 0.78431(17) 0.46944(14) 0.38200(11) 0.0312(4) Uani 1 1 d . . .
H67 H 0.7549 0.5158 0.4096 0.037 Uiso 1 1 calc R . .
C68 C 0.86011(18) 0.44801(16) 0.41955(12) 0.0375(5) Uani 1 1 d . . .
H68 H 0.8840 0.4794 0.4739 0.045 Uiso 1 1 calc R . .
C69 C 0.9015(2) 0.38038(17) 0.37773(12) 0.0416(5) Uani 1 1 d . . .
H69 H 0.9534 0.3640 0.4026 0.050 Uiso 1 1 calc R . .
C70 C 0.8656(2) 0.33750(17) 0.29904(13) 0.0419(5) Uani 1 1 d . . .
H70 H 0.8949 0.2917 0.2704 0.050 Uiso 1 1 calc R . .
C71 C 0.5549(3) 0.8759(3) -0.0230(2) 0.0895(10) Uani 0.702(11) 1 d PDU A 1
H71A H 0.6289 0.9317 -0.0179 0.107 Uiso 0.702(11) 1 calc PR A 1
H71B H 0.5739 0.8201 -0.0237 0.107 Uiso 0.702(11) 1 calc PR A 1
C72 C 0.4866(11) 0.8475(8) -0.0949(4) 0.111(3) Uani 0.702(11) 1 d PDU A 1
H72A H 0.5317 0.8355 -0.1356 0.166 Uiso 0.702(11) 1 calc PR A 1
H72B H 0.4633 0.9002 -0.0948 0.166 Uiso 0.702(11) 1 calc PR A 1
H72C H 0.4174 0.7869 -0.1044 0.166 Uiso 0.702(11) 1 calc PR A 1
O15 O 0.5070(3) 0.9048(6) 0.0447(2) 0.105(3) Uani 0.702(11) 1 d PDU A 1
H15B H 0.4347 0.8729 0.0343 0.126 Uiso 0.702(11) 1 calc PR A 1
C72A C 0.495(3) 0.876(3) -0.1000(13) 0.208(13) Uani 0.298(11) 1 d PDU A 2
H72D H 0.5099 0.8312 -0.1452 0.312 Uiso 0.298(11) 1 calc PR A 2
H72E H 0.5281 0.9432 -0.1001 0.312 Uiso 0.298(11) 1 calc PR A 2
H72F H 0.4116 0.8544 -0.1017 0.312 Uiso 0.298(11) 1 calc PR A 2
C71A C 0.5549(3) 0.8759(3) -0.0230(2) 0.0895(10) Uani 0.298(11) 1 d PU A 2
H71C H 0.5159 0.8129 -0.0156 0.107 Uiso 0.298(11) 1 calc PR A 2
H71D H 0.6390 0.8928 -0.0202 0.107 Uiso 0.298(11) 1 calc PR A 2
H2W H -0.5312 0.6499 -0.0336 0.050 Uiso 1 1 d . . .
H1W H -0.5909 0.6644 0.0252 0.077 Uiso 1 1 d . . .
H2N H 0.6534 0.4049 0.2068 0.050 Uiso 1 1 d . . .
H1N H 0.1199 0.3758 0.1709 0.050 Uiso 1 1 d . . .


_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 C3 1.369(2) . ?
O1 H1 0.8400 . ?
N1 N2 1.300(2) . ?
N1 C42 1.343(2) . ?
C1 C2 1.390(2) . ?
C1 C6 1.396(2) . ?
C1 H13 0.9500 . ?
O2 C4 1.371(2) . ?
O2 H2 0.8400 . ?
N2 C51 1.404(2) . ?
N2 H1N 0.9497 . ?
C2 C3 1.393(2) . ?
C2 C28 1.527(2) . ?
O3 C5 1.386(2) . ?
O3 H3 0.8400 . ?
N3 C51 1.335(2) . ?
N3 C55 1.344(2) . ?
C3 C4 1.390(2) . ?
O4 C10 1.380(2) . ?
O4 H4 0.8400 . ?
N4 C57 1.317(2) . ?
N4 N5 1.320(2) . ?
C4 C5 1.393(2) . ?
O5 C11 1.3689(19) . ?
O5 H5 0.8400 . ?
N5 C66 1.394(2) . ?
N5 H2N 0.9276 . ?
C5 C6 1.397(2) . ?
O6 C12 1.380(2) . ?
O6 H6 0.8400 . ?
N6 C66 1.339(2) . ?
N6 C70 1.344(3) . ?
C6 C7 1.536(2) . ?
O7 C17 1.391(2) . ?
O7 H7 0.8400 . ?
C7 C9 1.533(2) . ?
C7 C29 1.535(2) . ?
C7 H16 1.0000 . ?
O8 C18 1.371(2) . ?
O8 H8 0.8400 . ?
C8 C9 1.395(2) . ?
C8 C13 1.395(2) . ?
C8 H17 0.9500 . ?
O9 C19 1.378(2) . ?
O9 H9 0.8400 . ?
C9 C10 1.395(2) . ?
O10 C24 1.384(2) . ?
O10 H10 0.8400 . ?
C10 C11 1.391(2) . ?
O11 C25 1.368(2) . ?
O11 H11 0.8400 . ?
C11 C12 1.387(2) . ?
O12 C26 1.381(2) . ?
O12 H12 0.8400 . ?
C12 C13 1.400(2) . ?
O13 C41 1.268(2) . ?
C13 C14 1.530(2) . ?
O14 C56 1.255(2) . ?
C14 C16 1.526(2) . ?
C14 C32 1.537(2) . ?
C14 H14 1.0000 . ?
O15A H15A 0.8400 . ?
C15 C20 1.395(2) . ?
C15 C16 1.395(2) . ?
C15 H15 0.9500 . ?
O16 H2W 0.9681 . ?
O16 H1W 0.8600 . ?
C16 C17 1.390(2) . ?
C17 C18 1.389(2) . ?
C18 C19 1.388(2) . ?
C19 C20 1.393(2) . ?
C20 C21 1.524(2) . ?
C21 C23 1.524(2) . ?
C21 C35 1.534(2) . ?
C21 H21 1.0000 . ?
C22 C23 1.389(2) . ?
C22 C27 1.393(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.390(2) . ?
C24 C25 1.392(3) . ?
C25 C26 1.392(3) . ?
C26 C27 1.393(2) . ?
C27 C28 1.528(2) . ?
C28 C38 1.538(2) . ?
C28 H28 1.0000 . ?
C29 C30 1.520(2) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.515(3) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 C33 1.522(3) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.515(3) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 C36 1.524(2) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 C37 1.517(3) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C39 1.523(2) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.522(3) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 C50 1.444(3) . ?
C41 C42 1.450(3) . ?
C42 C43 1.456(3) . ?
C43 C44 1.403(3) . ?
C43 C48 1.412(3) . ?
C44 C45 1.380(3) . ?
C44 H44 0.9500 . ?
C45 C46 1.399(3) . ?
C45 H45 0.9500 . ?
C46 C47 1.372(3) . ?
C46 H46 0.9500 . ?
C47 C48 1.404(3) . ?
C47 H47 0.9500 . ?
C48 C49 1.439(3) . ?
C49 C50 1.345(3) . ?
C49 H49 0.9500 . ?
C50 H50 0.9500 . ?
C51 C52 1.387(3) . ?
C52 C53 1.384(3) . ?
C52 H52 0.9500 . ?
C53 C54 1.383(3) . ?
C53 H53 0.9500 . ?
C54 C55 1.376(3) . ?
C54 H54 0.9500 . ?
C55 H55 0.9500 . ?
C56 C65 1.439(3) . ?
C56 C57 1.473(3) . ?
C57 C58 1.468(3) . ?
C58 C59 1.399(3) . ?
C58 C63 1.407(3) . ?
C59 C60 1.384(3) . ?
C59 H59 0.9500 . ?
C60 C61 1.390(3) . ?
C60 H60 0.9500 . ?
C61 C62 1.377(3) . ?
C61 H61 0.9500 . ?
C62 C63 1.399(3) . ?
C62 H62 0.9500 . ?
C63 C64 1.446(3) . ?
C64 C65 1.343(3) . ?
C64 H64 0.9500 . ?
C65 H65 0.9500 . ?
C66 C67 1.389(3) . ?
C67 C68 1.372(3) . ?
C67 H67 0.9500 . ?
C68 C69 1.383(3) . ?
C68 H68 0.9500 . ?
C69 C70 1.376(3) . ?
C69 H69 0.9500 . ?
C70 H70 0.9500 . ?
C71 C72 1.410(8) . ?
C71 O15 1.437(5) . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
O15 H15B 0.8400 . ?
C72A H72D 0.9800 . ?
C72A H72E 0.9800 . ?
C72A H72F 0.9800 . ?

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
C3 O1 H1 109.5 . . ?
N2 N1 C42 117.47(16) . . ?
C2 C1 C6 123.53(16) . . ?
C2 C1 H13 118.2 . . ?
C6 C1 H13 118.2 . . ?
C4 O2 H2 109.5 . . ?
N1 N2 C51 119.49(15) . . ?
N1 N2 H1N 116.7 . . ?
C51 N2 H1N 122.8 . . ?
C1 C2 C3 117.37(15) . . ?
C1 C2 C28 123.84(15) . . ?
C3 C2 C28 118.72(15) . . ?
C5 O3 H3 109.5 . . ?
C51 N3 C55 116.41(16) . . ?
O1 C3 C4 120.17(15) . . ?
O1 C3 C2 118.76(15) . . ?
C4 C3 C2 121.05(15) . . ?
C10 O4 H4 109.5 . . ?
C57 N4 N5 119.66(15) . . ?
O2 C4 C3 115.92(15) . . ?
O2 C4 C5 123.92(15) . . ?
C3 C4 C5 120.00(15) . . ?
C11 O5 H5 109.5 . . ?
N4 N5 C66 119.39(15) . . ?
N4 N5 H2N 119.7 . . ?
C66 N5 H2N 120.7 . . ?
O3 C5 C4 115.65(15) . . ?
O3 C5 C6 123.63(15) . . ?
C4 C5 C6 120.71(15) . . ?
C12 O6 H6 109.5 . . ?
C66 N6 C70 116.48(17) . . ?
C1 C6 C5 117.27(15) . . ?
C1 C6 C7 121.53(15) . . ?
C5 C6 C7 121.13(15) . . ?
C17 O7 H7 109.5 . . ?
C9 C7 C29 111.91(14) . . ?
C9 C7 C6 109.80(13) . . ?
C29 C7 C6 112.61(14) . . ?
C9 C7 H16 107.4 . . ?
C29 C7 H16 107.4 . . ?
C6 C7 H16 107.4 . . ?
C18 O8 H8 109.5 . . ?
C9 C8 C13 123.45(15) . . ?
C9 C8 H17 118.3 . . ?
C13 C8 H17 118.3 . . ?
C19 O9 H9 109.5 . . ?
C8 C9 C10 117.35(15) . . ?
C8 C9 C7 121.22(14) . . ?
C10 C9 C7 121.41(15) . . ?
C24 O10 H10 109.5 . . ?
O4 C10 C11 119.25(15) . . ?
O4 C10 C9 119.83(15) . . ?
C11 C10 C9 120.80(16) . . ?
C25 O11 H11 109.5 . . ?
O5 C11 C12 124.05(15) . . ?
O5 C11 C10 115.73(15) . . ?
C12 C11 C10 120.21(15) . . ?
C26 O12 H12 109.5 . . ?
O6 C12 C11 116.51(15) . . ?
O6 C12 C13 122.56(16) . . ?
C11 C12 C13 120.92(15) . . ?
C8 C13 C12 117.09(16) . . ?
C8 C13 C14 121.51(15) . . ?
C12 C13 C14 121.39(15) . . ?
C16 C14 C13 110.33(13) . . ?
C16 C14 C32 114.99(14) . . ?
C13 C14 C32 110.67(14) . . ?
C16 C14 H14 106.8 . . ?
C13 C14 H14 106.8 . . ?
C32 C14 H14 106.8 . . ?
C20 C15 C16 123.32(15) . . ?
C20 C15 H15 118.3 . . ?
C16 C15 H15 118.3 . . ?
H2W O16 H1W 96.4 . . ?
C17 C16 C15 117.02(15) . . ?
C17 C16 C14 119.99(15) . . ?
C15 C16 C14 122.91(15) . . ?
C18 C17 C16 121.46(15) . . ?
C18 C17 O7 119.27(15) . . ?
C16 C17 O7 119.27(15) . . ?
O8 C18 C19 122.02(15) . . ?
O8 C18 C17 118.09(15) . . ?
C19 C18 C17 119.88(15) . . ?
O9 C19 C18 114.33(14) . . ?
O9 C19 C20 124.86(15) . . ?
C18 C19 C20 120.81(15) . . ?
C19 C20 C15 117.50(15) . . ?
C19 C20 C21 119.44(14) . . ?
C15 C20 C21 123.05(15) . . ?
C20 C21 C23 110.24(13) . . ?
C20 C21 C35 114.28(14) . . ?
C23 C21 C35 111.23(14) . . ?
C20 C21 H21 106.9 . . ?
C23 C21 H21 106.9 . . ?
C35 C21 H21 106.9 . . ?
C23 C22 C27 123.02(16) . . ?
C23 C22 H22 118.5 . . ?
C27 C22 H22 118.5 . . ?
C22 C23 C24 117.68(16) . . ?
C22 C23 C21 120.71(15) . . ?
C24 C23 C21 121.61(15) . . ?
O10 C24 C23 118.52(16) . . ?
O10 C24 C25 120.38(15) . . ?
C23 C24 C25 121.04(16) . . ?
O11 C25 C26 123.66(17) . . ?
O11 C25 C24 116.58(17) . . ?
C26 C25 C24 119.76(16) . . ?
O12 C26 C25 116.36(16) . . ?
O12 C26 C27 122.98(17) . . ?
C25 C26 C27 120.67(16) . . ?
C26 C27 C22 117.75(16) . . ?
C26 C27 C28 122.79(16) . . ?
C22 C27 C28 119.46(15) . . ?
C2 C28 C27 109.85(14) . . ?
C2 C28 C38 113.44(14) . . ?
C27 C28 C38 111.24(14) . . ?
C2 C28 H28 107.3 . . ?
C27 C28 H28 107.3 . . ?
C38 C28 H28 107.3 . . ?
C30 C29 C7 114.04(14) . . ?
C30 C29 H29A 108.7 . . ?
C7 C29 H29A 108.7 . . ?
C30 C29 H29B 108.7 . . ?
C7 C29 H29B 108.7 . . ?
H29A C29 H29B 107.6 . . ?
C31 C30 C29 112.36(16) . . ?
C31 C30 H30A 109.1 . . ?
C29 C30 H30A 109.1 . . ?
C31 C30 H30B 109.1 . . ?
C29 C30 H30B 109.1 . . ?
H30A C30 H30B 107.9 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C33 C32 C14 114.57(16) . . ?
C33 C32 H32A 108.6 . . ?
C14 C32 H32A 108.6 . . ?
C33 C32 H32B 108.6 . . ?
C14 C32 H32B 108.6 . . ?
H32A C32 H32B 107.6 . . ?
C34 C33 C32 112.3(2) . . ?
C34 C33 H33A 109.1 . . ?
C32 C33 H33A 109.1 . . ?
C34 C33 H33B 109.1 . . ?
C32 C33 H33B 109.1 . . ?
H33A C33 H33B 107.9 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C36 C35 C21 112.19(14) . . ?
C36 C35 H35A 109.2 . . ?
C21 C35 H35A 109.2 . . ?
C36 C35 H35B 109.2 . . ?
C21 C35 H35B 109.2 . . ?
H35A C35 H35B 107.9 . . ?
C37 C36 C35 112.06(16) . . ?
C37 C36 H36A 109.2 . . ?
C35 C36 H36A 109.2 . . ?
C37 C36 H36B 109.2 . . ?
C35 C36 H36B 109.2 . . ?
H36A C36 H36B 107.9 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C39 C38 C28 113.40(16) . . ?
C39 C38 H38A 108.9 . . ?
C28 C38 H38A 108.9 . . ?
C39 C38 H38B 108.9 . . ?
C28 C38 H38B 108.9 . . ?
H38A C38 H38B 107.7 . . ?
C40 C39 C38 112.40(18) . . ?
C40 C39 H39A 109.1 . . ?
C38 C39 H39A 109.1 . . ?
C40 C39 H39B 109.1 . . ?
C38 C39 H39B 109.1 . . ?
H39A C39 H39B 107.9 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
O13 C41 C50 120.31(18) . . ?
O13 C41 C42 121.96(17) . . ?
C50 C41 C42 117.74(17) . . ?
N1 C42 C41 123.35(17) . . ?
N1 C42 C43 116.26(16) . . ?
C41 C42 C43 120.37(16) . . ?
C44 C43 C48 118.77(17) . . ?
C44 C43 C42 122.45(17) . . ?
C48 C43 C42 118.77(17) . . ?
C45 C44 C43 120.72(19) . . ?
C45 C44 H44 119.6 . . ?
C43 C44 H44 119.6 . . ?
C44 C45 C46 120.4(2) . . ?
C44 C45 H45 119.8 . . ?
C46 C45 H45 119.8 . . ?
C47 C46 C45 119.77(19) . . ?
C47 C46 H46 120.1 . . ?
C45 C46 H46 120.1 . . ?
C46 C47 C48 120.90(19) . . ?
C46 C47 H47 119.6 . . ?
C48 C47 H47 119.6 . . ?
C47 C48 C43 119.45(19) . . ?
C47 C48 C49 121.34(18) . . ?
C43 C48 C49 119.21(18) . . ?
C50 C49 C48 122.81(18) . . ?
C50 C49 H49 118.6 . . ?
C48 C49 H49 118.6 . . ?
C49 C50 C41 121.06(19) . . ?
C49 C50 H50 119.5 . . ?
C41 C50 H50 119.5 . . ?
N3 C51 C52 124.58(17) . . ?
N3 C51 N2 112.42(16) . . ?
C52 C51 N2 123.00(16) . . ?
C53 C52 C51 117.49(17) . . ?
C53 C52 H52 121.3 . . ?
C51 C52 H52 121.3 . . ?
C54 C53 C52 119.15(18) . . ?
C54 C53 H53 120.4 . . ?
C52 C53 H53 120.4 . . ?
C55 C54 C53 118.85(17) . . ?
C55 C54 H54 120.6 . . ?
C53 C54 H54 120.6 . . ?
N3 C55 C54 123.50(18) . . ?
N3 C55 H55 118.3 . . ?
C54 C55 H55 118.3 . . ?
O14 C56 C65 121.53(17) . . ?
O14 C56 C57 120.69(17) . . ?
C65 C56 C57 117.78(17) . . ?
N4 C57 C58 116.55(16) . . ?
N4 C57 C56 124.10(17) . . ?
C58 C57 C56 119.35(16) . . ?
C59 C58 C63 118.74(17) . . ?
C59 C58 C57 121.96(17) . . ?
C63 C58 C57 119.30(17) . . ?
C60 C59 C58 120.52(19) . . ?
C60 C59 H59 119.7 . . ?
C58 C59 H59 119.7 . . ?
C59 C60 C61 120.7(2) . . ?
C59 C60 H60 119.7 . . ?
C61 C60 H60 119.7 . . ?
C62 C61 C60 119.49(19) . . ?
C62 C61 H61 120.3 . . ?
C60 C61 H61 120.3 . . ?
C61 C62 C63 120.87(19) . . ?
C61 C62 H62 119.6 . . ?
C63 C62 H62 119.6 . . ?
C62 C63 C58 119.72(18) . . ?
C62 C63 C64 121.11(18) . . ?
C58 C63 C64 119.17(18) . . ?
C65 C64 C63 122.96(18) . . ?
C65 C64 H64 118.5 . . ?
C63 C64 H64 118.5 . . ?
C64 C65 C56 121.40(18) . . ?
C64 C65 H65 119.3 . . ?
C56 C65 H65 119.3 . . ?
N6 C66 C67 123.70(17) . . ?
N6 C66 N5 114.21(16) . . ?
C67 C66 N5 122.08(17) . . ?
C68 C67 C66 118.16(18) . . ?
C68 C67 H67 120.9 . . ?
C66 C67 H67 120.9 . . ?
C67 C68 C69 119.53(19) . . ?
C67 C68 H68 120.2 . . ?
C69 C68 H68 120.2 . . ?
C70 C69 C68 118.20(19) . . ?
C70 C69 H69 120.9 . . ?
C68 C69 H69 120.9 . . ?
N6 C70 C69 123.92(19) . . ?
N6 C70 H70 118.0 . . ?
C69 C70 H70 118.0 . . ?
C72 C71 O15 117.7(5) . . ?
C72 C71 H71A 107.9 . . ?
O15 C71 H71A 107.9 . . ?
C72 C71 H71B 107.9 . . ?
O15 C71 H71B 107.9 . . ?
H71A C71 H71B 107.2 . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
H72D C72A H72E 109.5 . . ?
H72D C72A H72F 109.5 . . ?
H72E C72A H72F 109.5 . . ?

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
C42 N1 N2 C51 174.59(15) . . . . ?
C6 C1 C2 C3 -1.1(3) . . . . ?
C6 C1 C2 C28 -178.07(16) . . . . ?
C1 C2 C3 O1 -177.49(15) . . . . ?
C28 C2 C3 O1 -0.4(2) . . . . ?
C1 C2 C3 C4 1.2(2) . . . . ?
C28 C2 C3 C4 178.28(16) . . . . ?
O1 C3 C4 O2 3.7(2) . . . . ?
C2 C3 C4 O2 -174.96(15) . . . . ?
O1 C3 C4 C5 179.37(15) . . . . ?
C2 C3 C4 C5 0.7(3) . . . . ?
C57 N4 N5 C66 -176.85(16) . . . . ?
O2 C4 C5 O3 -7.5(2) . . . . ?
C3 C4 C5 O3 177.20(15) . . . . ?
O2 C4 C5 C6 172.55(16) . . . . ?
C3 C4 C5 C6 -2.8(3) . . . . ?
C2 C1 C6 C5 -0.8(3) . . . . ?
C2 C1 C6 C7 176.24(15) . . . . ?
O3 C5 C6 C1 -177.20(15) . . . . ?
C4 C5 C6 C1 2.8(2) . . . . ?
O3 C5 C6 C7 5.7(3) . . . . ?
C4 C5 C6 C7 -174.30(15) . . . . ?
C1 C6 C7 C9 -106.46(17) . . . . ?
C5 C6 C7 C9 70.5(2) . . . . ?
C1 C6 C7 C29 19.0(2) . . . . ?
C5 C6 C7 C29 -164.11(15) . . . . ?
C13 C8 C9 C10 0.4(2) . . . . ?
C13 C8 C9 C7 -178.01(15) . . . . ?
C29 C7 C9 C8 -50.1(2) . . . . ?
C6 C7 C9 C8 75.74(19) . . . . ?
C29 C7 C9 C10 131.54(16) . . . . ?
C6 C7 C9 C10 -102.64(17) . . . . ?
C8 C9 C10 O4 -179.15(14) . . . . ?
C7 C9 C10 O4 -0.7(2) . . . . ?
C8 C9 C10 C11 -3.2(2) . . . . ?
C7 C9 C10 C11 175.25(15) . . . . ?
O4 C10 C11 O5 -3.2(2) . . . . ?
C9 C10 C11 O5 -179.15(15) . . . . ?
O4 C10 C11 C12 178.13(15) . . . . ?
C9 C10 C11 C12 2.1(2) . . . . ?
O5 C11 C12 O6 4.3(2) . . . . ?
C10 C11 C12 O6 -177.13(15) . . . . ?
O5 C11 C12 C13 -176.81(15) . . . . ?
C10 C11 C12 C13 1.8(3) . . . . ?
C9 C8 C13 C12 3.3(2) . . . . ?
C9 C8 C13 C14 -177.35(15) . . . . ?
O6 C12 C13 C8 174.49(15) . . . . ?
C11 C12 C13 C8 -4.3(2) . . . . ?
O6 C12 C13 C14 -4.9(2) . . . . ?
C11 C12 C13 C14 176.27(15) . . . . ?
C8 C13 C14 C16 -74.60(19) . . . . ?
C12 C13 C14 C16 104.76(17) . . . . ?
C8 C13 C14 C32 53.8(2) . . . . ?
C12 C13 C14 C32 -126.83(17) . . . . ?
C20 C15 C16 C17 0.4(3) . . . . ?
C20 C15 C16 C14 -176.24(16) . . . . ?
C13 C14 C16 C17 -77.69(19) . . . . ?
C32 C14 C16 C17 156.30(16) . . . . ?
C13 C14 C16 C15 98.87(18) . . . . ?
C32 C14 C16 C15 -27.2(2) . . . . ?
C15 C16 C17 C18 -1.0(3) . . . . ?
C14 C16 C17 C18 175.73(16) . . . . ?
C15 C16 C17 O7 179.83(15) . . . . ?
C14 C16 C17 O7 -3.4(2) . . . . ?
C16 C17 C18 O8 -178.41(16) . . . . ?
O7 C17 C18 O8 0.7(2) . . . . ?
C16 C17 C18 C19 0.7(3) . . . . ?
O7 C17 C18 C19 179.88(15) . . . . ?
O8 C18 C19 O9 0.1(2) . . . . ?
C17 C18 C19 O9 -178.99(15) . . . . ?
O8 C18 C19 C20 179.34(16) . . . . ?
C17 C18 C19 C20 0.2(3) . . . . ?
O9 C19 C20 C15 178.32(16) . . . . ?
C18 C19 C20 C15 -0.8(2) . . . . ?
O9 C19 C20 C21 -0.3(3) . . . . ?
C18 C19 C20 C21 -179.44(15) . . . . ?
C16 C15 C20 C19 0.5(3) . . . . ?
C16 C15 C20 C21 179.07(15) . . . . ?
C19 C20 C21 C23 71.70(19) . . . . ?
C15 C20 C21 C23 -106.84(18) . . . . ?
C19 C20 C21 C35 -162.16(15) . . . . ?
C15 C20 C21 C35 19.3(2) . . . . ?
C27 C22 C23 C24 -0.8(2) . . . . ?
C27 C22 C23 C21 179.11(15) . . . . ?
C20 C21 C23 C22 74.90(19) . . . . ?
C35 C21 C23 C22 -52.9(2) . . . . ?
C20 C21 C23 C24 -105.22(17) . . . . ?
C35 C21 C23 C24 126.94(17) . . . . ?
C22 C23 C24 O10 -178.30(14) . . . . ?
C21 C23 C24 O10 1.8(2) . . . . ?
C22 C23 C24 C25 -0.9(2) . . . . ?
C21 C23 C24 C25 179.19(15) . . . . ?
O10 C24 C25 O11 -2.2(2) . . . . ?
C23 C24 C25 O11 -179.48(16) . . . . ?
O10 C24 C25 C26 177.80(15) . . . . ?
C23 C24 C25 C26 0.5(3) . . . . ?
O11 C25 C26 O12 1.8(3) . . . . ?
C24 C25 C26 O12 -178.13(15) . . . . ?
O11 C25 C26 C27 -178.36(16) . . . . ?
C24 C25 C26 C27 1.7(3) . . . . ?
O12 C26 C27 C22 176.54(15) . . . . ?
C25 C26 C27 C22 -3.3(2) . . . . ?
O12 C26 C27 C28 -3.5(3) . . . . ?
C25 C26 C27 C28 176.66(16) . . . . ?
C23 C22 C27 C26 2.8(2) . . . . ?
C23 C22 C27 C28 -177.08(15) . . . . ?
C1 C2 C28 C27 104.58(19) . . . . ?
C3 C2 C28 C27 -72.32(19) . . . . ?
C1 C2 C28 C38 -20.6(2) . . . . ?
C3 C2 C28 C38 162.49(15) . . . . ?
C26 C27 C28 C2 107.73(18) . . . . ?
C22 C27 C28 C2 -72.34(19) . . . . ?
C26 C27 C28 C38 -125.83(17) . . . . ?
C22 C27 C28 C38 54.1(2) . . . . ?
C9 C7 C29 C30 -61.7(2) . . . . ?
C6 C7 C29 C30 174.03(15) . . . . ?
C7 C29 C30 C31 176.43(17) . . . . ?
C16 C14 C32 C33 -61.2(2) . . . . ?
C13 C14 C32 C33 172.95(15) . . . . ?
C14 C32 C33 C34 -176.19(18) . . . . ?
C20 C21 C35 C36 173.88(14) . . . . ?
C23 C21 C35 C36 -60.51(19) . . . . ?
C21 C35 C36 C37 -179.71(16) . . . . ?
C2 C28 C38 C39 -171.81(16) . . . . ?
C27 C28 C38 C39 63.7(2) . . . . ?
C28 C38 C39 C40 -179.31(19) . . . . ?
N2 N1 C42 C41 -1.7(3) . . . . ?
N2 N1 C42 C43 179.44(15) . . . . ?
O13 C41 C42 N1 1.8(3) . . . . ?
C50 C41 C42 N1 -178.11(17) . . . . ?
O13 C41 C42 C43 -179.32(18) . . . . ?
C50 C41 C42 C43 0.7(3) . . . . ?
N1 C42 C43 C44 0.0(3) . . . . ?
C41 C42 C43 C44 -178.94(17) . . . . ?
N1 C42 C43 C48 180.00(16) . . . . ?
C41 C42 C43 C48 1.1(3) . . . . ?
C48 C43 C44 C45 -0.4(3) . . . . ?
C42 C43 C44 C45 179.59(17) . . . . ?
C43 C44 C45 C46 1.5(3) . . . . ?
C44 C45 C46 C47 -0.9(3) . . . . ?
C45 C46 C47 C48 -0.7(3) . . . . ?
C46 C47 C48 C43 1.7(3) . . . . ?
C46 C47 C48 C49 -177.80(19) . . . . ?
C44 C43 C48 C47 -1.1(3) . . . . ?
C42 C43 C48 C47 178.86(17) . . . . ?
C44 C43 C48 C49 178.37(17) . . . . ?
C42 C43 C48 C49 -1.6(3) . . . . ?
C47 C48 C49 C50 179.9(2) . . . . ?
C43 C48 C49 C50 0.4(3) . . . . ?
C48 C49 C50 C41 1.5(3) . . . . ?
O13 C41 C50 C49 178.0(2) . . . . ?
C42 C41 C50 C49 -2.0(3) . . . . ?
C55 N3 C51 C52 -1.5(3) . . . . ?
C55 N3 C51 N2 177.57(15) . . . . ?
N1 N2 C51 N3 -177.35(15) . . . . ?
N1 N2 C51 C52 1.8(3) . . . . ?
N3 C51 C52 C53 0.5(3) . . . . ?
N2 C51 C52 C53 -178.48(17) . . . . ?
C51 C52 C53 C54 0.6(3) . . . . ?
C52 C53 C54 C55 -0.6(3) . . . . ?
C51 N3 C55 C54 1.5(3) . . . . ?
C53 C54 C55 N3 -0.5(3) . . . . ?
N5 N4 C57 C58 -179.02(15) . . . . ?
N5 N4 C57 C56 1.2(3) . . . . ?
O14 C56 C57 N4 3.1(3) . . . . ?
C65 C56 C57 N4 -177.43(17) . . . . ?
O14 C56 C57 C58 -176.72(16) . . . . ?
C65 C56 C57 C58 2.8(2) . . . . ?
N4 C57 C58 C59 -1.7(3) . . . . ?
C56 C57 C58 C59 178.15(17) . . . . ?
N4 C57 C58 C63 178.12(16) . . . . ?
C56 C57 C58 C63 -2.1(2) . . . . ?
C63 C58 C59 C60 0.2(3) . . . . ?
C57 C58 C59 C60 -179.99(17) . . . . ?
C58 C59 C60 C61 -0.2(3) . . . . ?
C59 C60 C61 C62 0.0(3) . . . . ?
C60 C61 C62 C63 0.2(3) . . . . ?
C61 C62 C63 C58 -0.2(3) . . . . ?
C61 C62 C63 C64 179.73(19) . . . . ?
C59 C58 C63 C62 -0.1(3) . . . . ?
C57 C58 C63 C62 -179.85(17) . . . . ?
C59 C58 C63 C64 -179.96(17) . . . . ?
C57 C58 C63 C64 0.3(3) . . . . ?
C62 C63 C64 C65 -179.01(19) . . . . ?
C58 C63 C64 C65 0.9(3) . . . . ?
C63 C64 C65 C56 -0.1(3) . . . . ?
O14 C56 C65 C64 177.78(18) . . . . ?
C57 C56 C65 C64 -1.7(3) . . . . ?
C70 N6 C66 C67 0.8(3) . . . . ?
C70 N6 C66 N5 -178.24(18) . . . . ?
N4 N5 C66 N6 -177.23(16) . . . . ?
N4 N5 C66 C67 3.7(3) . . . . ?
N6 C66 C67 C68 -0.9(3) . . . . ?
N5 C66 C67 C68 178.06(18) . . . . ?
C66 C67 C68 C69 0.1(3) . . . . ?
C67 C68 C69 C70 0.7(3) . . . . ?
C66 N6 C70 C69 0.1(3) . . . . ?
C68 C69 C70 N6 -0.8(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.06
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.727
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.050

_database_code_depnum_ccdc_archive 'CCDC 1002507'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_3cp32d

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            
'C-propylpyrogallol[4]arene with 1-(2-pyridylazo)-2-napthol'
_chemical_formula_moiety         
'C40 H48 O12, 2(C15 H22 O1 N3), C3 H8 O12, 2(H2 O1)'
_chemical_formula_sum            'C73 H82 N6 O17'
_chemical_melting_point          ?

_exptl_crystal_description       plate
_exptl_crystal_colour            orange

_diffrn_ambient_temperature      100(2)
_chemical_formula_weight         1315.45

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0020 0.0018 '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 -0.0030 0.0037 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O -0.0041 0.0068 '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
_chemical_absolute_configuration ?

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

_cell_length_a                   12.618(3)
_cell_length_b                   15.758(3)
_cell_length_c                   18.702(4)
_cell_angle_alpha                109.763(3)
_cell_angle_beta                 92.291(3)
_cell_angle_gamma                112.029(3)
_cell_volume                     3184.1(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6022
_cell_measurement_theta_min      2.9
_cell_measurement_theta_max      28.9
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1396
_exptl_absorpt_coefficient_mu    0.109
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_process_details   
;
 Data were corrected for decay and absorption using the program SADABS 
 (Sheldrick, G. M. (2003). SADABS. Version 2.10. University of
 Göttingen, Germany).
;

_exptl_special_details           
; 
 ? 
;
_diffrn_radiation_probe          ?
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_source                   'Advanced Light Source Station 11.3.1'
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker APEXII CCD diffractometer'
_diffrn_measurement_method       'ω/θ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.0
_diffrn_reflns_number            36020
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_av_sigmaI/netI    0.0763
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.86
_diffrn_reflns_theta_max         29.01
_reflns_number_total             13007
_reflns_number_gt                9103
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2008)'
_computing_structure_solution    'SHELXS-1997 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-1997 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-SEED, Barbour, 2001'
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. The lone oxygen atoms are 
 disordered water molecules that do not have calculated or modeled hydrogens,
 but the hydrogens are included in the molecular formula.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0901P)²+1.4438P] where P=(Fo²+2Fc²)/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         13007
_refine_ls_number_parameters     887
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_gt           0.0615
_refine_ls_wR_factor_ref         0.1892
_refine_ls_wR_factor_gt          0.1671
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.048
_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
O1 O -0.00116(15) 0.52271(12) 0.37086(10) 0.0267(4) Uani 1 1 d . . .
H1 H -0.0248 0.5587 0.4045 0.032 Uiso 1 1 calc R . .
C1 C -0.1326(2) 0.25363(18) 0.27608(14) 0.0226(5) Uani 1 1 d . . .
H13 H -0.1230 0.2030 0.2353 0.027 Uiso 1 1 calc R . .
O1I O 0.4926(3) 0.0755(4) 0.4615(2) 0.142(2) Uani 1 1 d . . .
H1I H 0.5567 0.0718 0.4679 0.170 Uiso 1 1 calc R . .
C1I C 0.3812(5) 0.1504(5) 0.5062(4) 0.117(2) Uani 1 1 d D . .
H1I1 H 0.3744 0.1528 0.4547 0.175 Uiso 1 1 calc R . .
H1I2 H 0.3842 0.2120 0.5448 0.175 Uiso 1 1 calc R . .
H1I3 H 0.3135 0.0942 0.5074 0.175 Uiso 1 1 calc R . .
O1P O 0.12360(19) 0.44621(16) 0.76544(12) 0.0454(5) Uani 1 1 d . . .
N1P N 0.0453(2) 0.31503(16) 0.53017(13) 0.0326(5) Uani 1 1 d . . .
C1P C 0.1969(2) 0.4287(2) 0.79820(16) 0.0335(6) Uani 1 1 d . . .
O1W O 0.54811(15) 0.36644(13) 0.48703(10) 0.0282(4) Uani 1 1 d . . .
O2 O -0.16522(17) 0.47740(13) 0.45393(10) 0.0319(4) Uani 1 1 d . . .
H2 H -0.1967 0.4577 0.4874 0.038 Uiso 1 1 calc R . .
C2 C -0.0583(2) 0.35167(18) 0.29189(13) 0.0225(5) Uani 1 1 d . . .
C2I C 0.4847(6) 0.1390(4) 0.5235(3) 0.108(2) Uani 1 1 d D . .
H2I H 0.5470 0.2026 0.5259 0.129 Uiso 1 1 calc R . .
O2P O 0.46285(16) 0.61395(13) 0.36416(10) 0.0305(4) Uani 1 1 d . . .
N2P N 0.1413(2) 0.32766(17) 0.64126(13) 0.0319(5) Uani 1 1 d . . .
H2P H 0.1057 0.3636 0.6667 0.038 Uiso 1 1 calc R . .
C2P C 0.2450(2) 0.3602(2) 0.75594(16) 0.0337(6) Uani 1 1 d . . .
O2W O 0.8287(2) 0.2443(2) 0.60757(15) 0.0357(6) Uani 0.85 1 d P A 1
O3 O -0.30625(17) 0.28319(14) 0.42828(11) 0.0330(4) Uani 1 1 d . . .
H3 H -0.3106 0.2325 0.4359 0.040 Uiso 1 1 calc R . .
C3 C -0.0740(2) 0.42495(17) 0.35192(14) 0.0229(5) Uani 1 1 d . . .
C3I C 0.5154(6) 0.1376(5) 0.5976(4) 0.129(2) Uani 1 1 d . . .
H3I1 H 0.5891 0.1304 0.6007 0.194 Uiso 1 1 calc R . .
H3I2 H 0.4540 0.0818 0.6043 0.194 Uiso 1 1 calc R . .
H3I3 H 0.5240 0.1997 0.6385 0.194 Uiso 1 1 calc R . .
N3P N 0.2165(2) 0.31216(16) 0.67824(13) 0.0320(5) Uani 1 1 d . . .
C3P C 0.3300(2) 0.3413(2) 0.79540(16) 0.0337(6) Uani 1 1 d . . .
O4 O -0.26626(16) 0.13471(13) 0.45136(10) 0.0299(4) Uani 1 1 d . . .
H4 H -0.2322 0.1512 0.4966 0.036 Uiso 1 1 calc R . .
C4 C -0.1580(2) 0.39981(18) 0.39574(14) 0.0250(5) Uani 1 1 d . . .
N4P N 0.2054(2) 0.64400(17) 0.23887(13) 0.0343(5) Uani 1 1 d . . .
C4P C 0.3800(2) 0.2774(2) 0.75687(17) 0.0355(6) Uani 1 1 d . . .
H4P H 0.3581 0.2441 0.7022 0.043 Uiso 1 1 calc R . .
O5 O -0.14130(17) 0.05285(14) 0.50305(10) 0.0328(4) Uani 1 1 d . . .
H5 H -0.0914 0.0331 0.5132 0.039 Uiso 1 1 calc R . .
C5 C -0.2292(2) 0.30145(19) 0.37908(14) 0.0248(5) Uani 1 1 d . . .
N5P N 0.32487(18) 0.56476(15) 0.23908(12) 0.0260(5) Uani 1 1 d . . .
H5P H 0.3467 0.5984 0.2894 0.031 Uiso 1 1 calc R . .
C5P C 0.4598(3) 0.2618(2) 0.79635(18) 0.0405(7) Uani 1 1 d . . .
H16 H 0.4936 0.2188 0.7689 0.049 Uiso 1 1 calc R . .
O6 O -0.05321(17) -0.06172(13) 0.40698(10) 0.0292(4) Uani 1 1 d . . .
H6 H -0.0314 -0.0982 0.3724 0.035 Uiso 1 1 calc R . .
C6 C -0.2206(2) 0.22604(18) 0.31726(14) 0.0227(5) Uani 1 1 d . . .
N6P N 0.36679(18) 0.49998(15) 0.20412(12) 0.0250(4) Uani 1 1 d . . .
C6P C 0.4923(3) 0.3094(2) 0.87755(18) 0.0431(7) Uani 1 1 d . . .
H6P H 0.5480 0.2989 0.9051 0.052 Uiso 1 1 calc R . .
O7 O 0.07652(16) -0.14734(13) 0.32033(10) 0.0299(4) Uani 1 1 d . . .
H7 H 0.1294 -0.1482 0.3485 0.036 Uiso 1 1 calc R . .
C7 C -0.3030(2) 0.11788(18) 0.29584(15) 0.0263(5) Uani 1 1 d . . .
H17 H -0.3664 0.1176 0.3263 0.032 Uiso 1 1 calc R . .
C7P C 0.4425(3) 0.3712(2) 0.91628(18) 0.0412(7) Uani 1 1 d . . .
H7P H 0.4627 0.4017 0.9711 0.049 Uiso 1 1 calc R . .
O8 O 0.31047(18) -0.04937(15) 0.34402(12) 0.0398(5) Uani 1 1 d . . .
H8 H 0.3758 -0.0020 0.3651 0.048 Uiso 1 1 calc R . .
C8 C -0.1953(2) 0.00414(17) 0.27098(14) 0.0244(5) Uani 1 1 d . . .
H18 H -0.2071 -0.0059 0.2177 0.029 Uiso 1 1 calc R . .
C8P C 0.3634(2) 0.3904(2) 0.87732(16) 0.0371(6) Uani 1 1 d . . .
O9 O 0.41092(15) 0.10579(14) 0.29667(11) 0.0339(4) Uani 1 1 d . . .
H9 H 0.4296 0.1666 0.3088 0.041 Uiso 1 1 calc R . .
C9 C -0.2413(2) 0.06352(18) 0.32143(14) 0.0247(5) Uani 1 1 d . . .
C9P C 0.3146(3) 0.4578(2) 0.91697(17) 0.0402(7) Uani 1 1 d . . .
H9P H 0.3376 0.4900 0.9717 0.048 Uiso 1 1 calc R . .
O10 O 0.39322(15) 0.28396(13) 0.35483(10) 0.0263(4) Uani 1 1 d . . .
H10 H 0.4242 0.3229 0.4008 0.032 Uiso 1 1 calc R . .
C10 C -0.2224(2) 0.07685(18) 0.39920(15) 0.0264(5) Uani 1 1 d . . .
C10P C 0.2384(3) 0.4779(2) 0.88115(17) 0.0404(7) Uani 1 1 d . . .
H10P H 0.2112 0.5250 0.9105 0.048 Uiso 1 1 calc R . .
O11 O 0.35723(15) 0.43698(13) 0.44880(10) 0.0271(4) Uani 1 1 d . . .
H11 H 0.3766 0.4982 0.4632 0.033 Uiso 1 1 calc R . .
C11 C -0.1601(2) 0.03373(18) 0.42527(14) 0.0256(5) Uani 1 1 d . . .
C11P C 0.1172(2) 0.28652(18) 0.56019(15) 0.0286(5) Uani 1 1 d . . .
O12 O 0.20287(15) 0.49980(12) 0.39746(10) 0.0269(4) Uani 1 1 d . . .
H12 H 0.1479 0.5076 0.3778 0.032 Uiso 1 1 calc R . .
C12 C -0.1156(2) -0.02474(17) 0.37370(14) 0.0245(5) Uani 1 1 d . . .
C12P C 0.1652(3) 0.2247(2) 0.51699(16) 0.0347(6) Uani 1 1 d . . .
H12P H 0.2148 0.2055 0.5413 0.042 Uiso 1 1 calc R . .
C13 C -0.1332(2) -0.04087(17) 0.29524(14) 0.0241(5) Uani 1 1 d . . .
C13P C 0.1386(3) 0.1920(2) 0.43753(15) 0.0335(6) Uani 1 1 d . . .
H13P H 0.1695 0.1494 0.4058 0.040 Uiso 1 1 calc R . .
C14 C -0.0817(2) -0.10430(18) 0.24060(14) 0.0241(5) Uani 1 1 d . . .
H14 H -0.0975 -0.1634 0.2544 0.029 Uiso 1 1 calc R . .
C14P C 0.0666(2) 0.22205(19) 0.40467(15) 0.0306(6) Uani 1 1 d . . .
H14P H 0.0479 0.2012 0.3501 0.037 Uiso 1 1 calc R . .
C15 C 0.0994(2) 0.02770(17) 0.22912(13) 0.0231(5) Uani 1 1 d . . .
H15 H 0.0490 0.0454 0.2038 0.028 Uiso 1 1 calc R . .
C15P C 0.0223(2) 0.2827(2) 0.45243(16) 0.0337(6) Uani 1 1 d . . .
H15P H -0.0273 0.3030 0.4293 0.040 Uiso 1 1 calc R . .
C16 C 0.0501(2) -0.04884(17) 0.25447(13) 0.0231(5) Uani 1 1 d . . .
C16P C 0.4934(2) 0.54668(18) 0.32678(14) 0.0262(5) Uani 1 1 d . . .
C17 C 0.1244(2) -0.07279(18) 0.29248(14) 0.0260(5) Uani 1 1 d . . .
C17P C 0.4453(2) 0.48878(18) 0.24383(14) 0.0249(5) Uani 1 1 d . . .
C18 C 0.2445(2) -0.02086(19) 0.30551(14) 0.0289(6) Uani 1 1 d . . .
C18P C 0.4860(2) 0.41382(18) 0.20112(14) 0.0250(5) Uani 1 1 d . . .
C19 C 0.2914(2) 0.05613(19) 0.27960(15) 0.0277(5) Uani 1 1 d . . .
C19P C 0.4456(2) 0.35780(19) 0.12209(15) 0.0280(5) Uani 1 1 d . . .
H19P H 0.3898 0.3681 0.0944 0.034 Uiso 1 1 calc R . .
C20 C 0.2189(2) 0.08002(17) 0.23890(14) 0.0238(5) Uani 1 1 d . . .
C20P C 0.4856(2) 0.2877(2) 0.08360(16) 0.0331(6) Uani 1 1 d . . .
H20P H 0.4575 0.2505 0.0297 0.040 Uiso 1 1 calc R . .
C21 C 0.2659(2) 0.16027(18) 0.20585(14) 0.0251(5) Uani 1 1 d . . .
H21 H 0.3521 0.1813 0.2116 0.030 Uiso 1 1 calc R . .
C21P C 0.5668(2) 0.2711(2) 0.12320(16) 0.0337(6) Uani 1 1 d . . .
H21P H 0.5938 0.2226 0.0965 0.040 Uiso 1 1 calc R . .
C22 C 0.1599(2) 0.27520(17) 0.22904(14) 0.0230(5) Uani 1 1 d . . .
H22 H 0.1132 0.2350 0.1789 0.028 Uiso 1 1 calc R . .
C22P C 0.6076(2) 0.3254(2) 0.20122(16) 0.0320(6) Uani 1 1 d . . .
H22P H 0.6631 0.3140 0.2282 0.038 Uiso 1 1 calc R . .
C23 C 0.2451(2) 0.25021(17) 0.25386(14) 0.0232(5) Uani 1 1 d . . .
C23P C 0.5685(2) 0.39733(19) 0.24151(15) 0.0273(5) Uani 1 1 d . . .
C24 C 0.3116(2) 0.30895(18) 0.32777(14) 0.0236(5) Uani 1 1 d . . .
C24P C 0.6112(2) 0.4544(2) 0.32309(15) 0.0296(6) Uani 1 1 d . . .
H24P H 0.6661 0.4420 0.3495 0.036 Uiso 1 1 calc R . .
C25 C 0.2937(2) 0.39002(18) 0.37486(13) 0.0227(5) Uani 1 1 d . . .
C25P C 0.5765(2) 0.52444(19) 0.36339(15) 0.0283(5) Uani 1 1 d . . .
H25P H 0.6075 0.5601 0.4172 0.034 Uiso 1 1 calc R . .
C26 C 0.2103(2) 0.41529(17) 0.34748(14) 0.0230(5) Uani 1 1 d . . .
C26P C 0.2462(2) 0.57994(19) 0.19642(15) 0.0274(5) Uani 1 1 d . . .
C27 C 0.1394(2) 0.35664(18) 0.27419(14) 0.0228(5) Uani 1 1 d . . .
C27P C 0.2139(2) 0.5321(2) 0.11631(15) 0.0303(6) Uani 1 1 d . . .
H27P H 0.2442 0.4865 0.0884 0.036 Uiso 1 1 calc R . .
C28 C 0.0399(2) 0.37796(18) 0.24717(14) 0.0229(5) Uani 1 1 d . . .
H28 H 0.0707 0.4508 0.2596 0.027 Uiso 1 1 calc R . .
C28P C 0.1366(2) 0.5531(2) 0.07885(16) 0.0349(6) Uani 1 1 d . . .
H28P H 0.1123 0.5218 0.0242 0.042 Uiso 1 1 calc R . .
C29 C -0.3613(2) 0.0705(2) 0.21017(16) 0.0314(6) Uani 1 1 d . . .
H29A H -0.3946 0.1136 0.1992 0.038 Uiso 1 1 calc R . .
H29B H -0.3009 0.0679 0.1784 0.038 Uiso 1 1 calc R . .
C29P C 0.0947(3) 0.6200(2) 0.12119(17) 0.0390(7) Uani 1 1 d . . .
H29P H 0.0422 0.6362 0.0963 0.047 Uiso 1 1 calc R . .
C30 C -0.4574(3) -0.0334(2) 0.18525(18) 0.0408(7) Uani 1 1 d . . .
H30A H -0.4240 -0.0781 0.1928 0.049 Uiso 1 1 calc R . .
H30B H -0.5166 -0.0322 0.2183 0.049 Uiso 1 1 calc R . .
C30P C 0.1304(3) 0.6624(2) 0.19994(17) 0.0387(7) Uani 1 1 d . . .
H30P H 0.1003 0.7077 0.2288 0.046 Uiso 1 1 calc R . .
C31 C -0.5154(3) -0.0734(3) 0.1012(2) 0.0616(11) Uani 1 1 d . . .
H31A H -0.5769 -0.1400 0.0874 0.092 Uiso 1 1 calc R . .
H31B H -0.4574 -0.0763 0.0683 0.092 Uiso 1 1 calc R . .
H31C H -0.5494 -0.0297 0.0937 0.092 Uiso 1 1 calc R . .
C32 C -0.1361(2) -0.14320(18) 0.15540(14) 0.0256(5) Uani 1 1 d . . .
H32A H -0.1179 -0.0868 0.1387 0.031 Uiso 1 1 calc R . .
H32B H -0.2218 -0.1766 0.1488 0.031 Uiso 1 1 calc R . .
C33 C -0.0915(2) -0.2162(2) 0.10395(15) 0.0308(6) Uani 1 1 d . . .
H33A H -0.0059 -0.1826 0.1099 0.037 Uiso 1 1 calc R . .
H33B H -0.1086 -0.2721 0.1211 0.037 Uiso 1 1 calc R . .
C34 C -0.1469(3) -0.2558(2) 0.01972(16) 0.0420(7) Uani 1 1 d . . .
H34A H -0.1165 -0.3023 -0.0112 0.063 Uiso 1 1 calc R . .
H34B H -0.1285 -0.2007 0.0022 0.063 Uiso 1 1 calc R . .
H34C H -0.2315 -0.2899 0.0135 0.063 Uiso 1 1 calc R . .
C35 C 0.2158(2) 0.12021(19) 0.11942(14) 0.0279(5) Uani 1 1 d . . .
H35A H 0.1298 0.0933 0.1119 0.033 Uiso 1 1 calc R . .
H35B H 0.2425 0.1756 0.1013 0.033 Uiso 1 1 calc R . .
C36 C 0.2508(3) 0.0394(2) 0.07006(16) 0.0359(6) Uani 1 1 d . . .
H36A H 0.3368 0.0665 0.0768 0.043 Uiso 1 1 calc R . .
H36B H 0.2251 -0.0157 0.0885 0.043 Uiso 1 1 calc R . .
C37 C 0.1989(3) -0.0005(2) -0.01522(17) 0.0496(8) Uani 1 1 d . . .
H37A H 0.2243 -0.0518 -0.0442 0.074 Uiso 1 1 calc R . .
H37B H 0.2253 0.0535 -0.0342 0.074 Uiso 1 1 calc R . .
H37C H 0.1138 -0.0289 -0.0225 0.074 Uiso 1 1 calc R . .
C38 C -0.0055(2) 0.32480(18) 0.15934(14) 0.0252(5) Uani 1 1 d . . .
H38A H 0.0611 0.3404 0.1326 0.030 Uiso 1 1 calc R . .
H38B H -0.0402 0.2524 0.1462 0.030 Uiso 1 1 calc R . .
C39 C -0.0960(2) 0.3529(2) 0.12901(15) 0.0318(6) Uani 1 1 d . . .
H39A H -0.1600 0.3427 0.1585 0.038 Uiso 1 1 calc R . .
H39B H -0.0597 0.4239 0.1374 0.038 Uiso 1 1 calc R . .
C40 C -0.1457(3) 0.2920(2) 0.04362(17) 0.0435(7) Uani 1 1 d . . .
H40A H -0.2033 0.3122 0.0262 0.065 Uiso 1 1 calc R . .
H40B H -0.1832 0.2217 0.0353 0.065 Uiso 1 1 calc R . .
H40C H -0.0828 0.3028 0.0141 0.065 Uiso 1 1 calc R . .
H1W H 0.6043 0.3387 0.4684 0.061 Uiso 1 1 d . . .
H2W H 0.5344 0.3549 0.5345 0.088 Uiso 1 1 d . . .
O2WA O 0.7621(17) 0.2043(13) 0.6140(10) 0.050(4) Uani 0.15 1 d P B 2


_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 C3 1.373(3) . ?
O1 H1 0.8400 . ?
C1 C2 1.391(3) . ?
C1 C6 1.395(3) . ?
C1 H13 0.9500 . ?
O1I C2I 1.287(6) . ?
O1I H1I 0.8400 . ?
C1I C2I 1.423(6) . ?
C1I H1I1 0.9800 . ?
C1I H1I2 0.9800 . ?
C1I H1I3 0.9800 . ?
O1P C1P 1.252(3) . ?
N1P C11P 1.333(3) . ?
N1P C15P 1.346(3) . ?
C1P C10P 1.449(4) . ?
C1P C2P 1.452(4) . ?
O1W H1W 0.9826 . ?
O1W H2W 0.9747 . ?
O2 C4 1.371(3) . ?
O2 H2 0.8400 . ?
C2 C3 1.395(3) . ?
C2 C28 1.528(3) . ?
C2I C3I 1.434(8) . ?
C2I H2I 1.0000 . ?
O2P C16P 1.260(3) . ?
N2P N3P 1.294(3) . ?
N2P C11P 1.401(3) . ?
N2P H2P 0.8800 . ?
C2P N3P 1.351(3) . ?
C2P C3P 1.453(4) . ?
O3 C5 1.384(3) . ?
O3 H3 0.8400 . ?
C3 C4 1.388(3) . ?
C3I H3I1 0.9800 . ?
C3I H3I2 0.9800 . ?
C3I H3I3 0.9800 . ?
C3P C4P 1.398(4) . ?
C3P C8P 1.423(4) . ?
O4 C10 1.382(3) . ?
O4 H4 0.8400 . ?
C4 C5 1.383(4) . ?
N4P C26P 1.339(3) . ?
N4P C30P 1.344(4) . ?
C4P C5P 1.366(4) . ?
C4P H4P 0.9500 . ?
O5 C11 1.373(3) . ?
O5 H5 0.8400 . ?
C5 C6 1.392(3) . ?
N5P N6P 1.315(3) . ?
N5P C26P 1.387(3) . ?
N5P H5P 0.8800 . ?
C5P C6P 1.409(4) . ?
C5P H16 0.9500 . ?
O6 C12 1.377(3) . ?
O6 H6 0.8400 . ?
C6 C7 1.524(3) . ?
N6P C17P 1.314(3) . ?
C6P C7P 1.374(5) . ?
C6P H6P 0.9500 . ?
O7 C17 1.387(3) . ?
O7 H7 0.8400 . ?
C7 C9 1.522(3) . ?
C7 C29 1.533(4) . ?
C7 H17 1.0000 . ?
C7P C8P 1.392(4) . ?
C7P H7P 0.9500 . ?
O8 C18 1.366(3) . ?
O8 H8 0.8400 . ?
C8 C13 1.389(3) . ?
C8 C9 1.399(3) . ?
C8 H18 0.9500 . ?
C8P C9P 1.432(4) . ?
O9 C19 1.377(3) . ?
O9 H9 0.8400 . ?
C9 C10 1.394(3) . ?
C9P C10P 1.339(4) . ?
C9P H9P 0.9500 . ?
O10 C24 1.367(3) . ?
O10 H10 0.8400 . ?
C10 C11 1.383(3) . ?
C10P H10P 0.9500 . ?
O11 C25 1.370(3) . ?
O11 H11 0.8400 . ?
C11 C12 1.387(3) . ?
C11P C12P 1.384(4) . ?
O12 C26 1.384(3) . ?
O12 H12 0.8400 . ?
C12 C13 1.395(3) . ?
C12P C13P 1.378(4) . ?
C12P H12P 0.9500 . ?
C13 C14 1.522(3) . ?
C13P C14P 1.379(4) . ?
C13P H13P 0.9500 . ?
C14 C16 1.522(3) . ?
C14 C32 1.524(3) . ?
C14 H14 1.0000 . ?
C14P C15P 1.374(4) . ?
C14P H14P 0.9500 . ?
C15 C16 1.383(3) . ?
C15 C20 1.390(3) . ?
C15 H15 0.9500 . ?
C15P H15P 0.9500 . ?
C16 C17 1.386(3) . ?
C16P C25P 1.439(4) . ?
C16P C17P 1.470(3) . ?
C17 C18 1.389(4) . ?
C17P C18P 1.465(3) . ?
C18 C19 1.392(4) . ?
C18P C19P 1.394(4) . ?
C18P C23P 1.412(3) . ?
C19 C20 1.397(3) . ?
C19P C20P 1.379(4) . ?
C19P H19P 0.9500 . ?
C20 C21 1.526(4) . ?
C20P C21P 1.391(4) . ?
C20P H20P 0.9500 . ?
C21 C23 1.524(3) . ?
C21 C35 1.530(3) . ?
C21 H21 1.0000 . ?
C21P C22P 1.375(4) . ?
C21P H21P 0.9500 . ?
C22 C23 1.388(3) . ?
C22 C27 1.400(3) . ?
C22 H22 0.9500 . ?
C22P C23P 1.403(4) . ?
C22P H22P 0.9500 . ?
C23 C24 1.390(3) . ?
C23P C24P 1.438(4) . ?
C24 C25 1.389(3) . ?
C24P C25P 1.343(4) . ?
C24P H24P 0.9500 . ?
C25 C26 1.392(3) . ?
C25P H25P 0.9500 . ?
C26 C27 1.400(3) . ?
C26P C27P 1.391(4) . ?
C27 C28 1.525(3) . ?
C27P C28P 1.377(4) . ?
C27P H27P 0.9500 . ?
C28 C38 1.537(3) . ?
C28 H28 1.0000 . ?
C28P C29P 1.380(4) . ?
C28P H28P 0.9500 . ?
C29 C30 1.523(4) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29P C30P 1.369(4) . ?
C29P H29P 0.9500 . ?
C30 C31 1.515(5) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30P H30P 0.9500 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 C33 1.532(3) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.510(4) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 C36 1.525(3) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 C37 1.516(4) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C39 1.522(3) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.515(4) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?

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
C3 O1 H1 109.5 . . ?
C2 C1 C6 123.2(2) . . ?
C2 C1 H13 118.4 . . ?
C6 C1 H13 118.4 . . ?
C2I O1I H1I 109.5 . . ?
C2I C1I H1I1 109.5 . . ?
C2I C1I H1I2 109.5 . . ?
H1I1 C1I H1I2 109.5 . . ?
C2I C1I H1I3 109.5 . . ?
H1I1 C1I H1I3 109.5 . . ?
H1I2 C1I H1I3 109.5 . . ?
C11P N1P C15P 116.2(2) . . ?
O1P C1P C10P 120.5(3) . . ?
O1P C1P C2P 122.4(3) . . ?
C10P C1P C2P 117.1(3) . . ?
H1W O1W H2W 105.1 . . ?
C4 O2 H2 109.5 . . ?
C1 C2 C3 117.5(2) . . ?
C1 C2 C28 121.2(2) . . ?
C3 C2 C28 121.2(2) . . ?
O1I C2I C1I 106.8(5) . . ?
O1I C2I C3I 120.2(6) . . ?
C1I C2I C3I 119.4(7) . . ?
O1I C2I H2I 102.4 . . ?
C1I C2I H2I 102.4 . . ?
C3I C2I H2I 102.4 . . ?
N3P N2P C11P 119.2(2) . . ?
N3P N2P H2P 120.4 . . ?
C11P N2P H2P 120.4 . . ?
N3P C2P C1P 123.0(3) . . ?
N3P C2P C3P 115.7(3) . . ?
C1P C2P C3P 121.3(2) . . ?
C5 O3 H3 109.5 . . ?
O1 C3 C4 119.5(2) . . ?
O1 C3 C2 119.7(2) . . ?
C4 C3 C2 120.6(2) . . ?
C2I C3I H3I1 109.5 . . ?
C2I C3I H3I2 109.5 . . ?
H3I1 C3I H3I2 109.5 . . ?
C2I C3I H3I3 109.5 . . ?
H3I1 C3I H3I3 109.5 . . ?
H3I2 C3I H3I3 109.5 . . ?
N2P N3P C2P 117.3(2) . . ?
C4P C3P C8P 118.8(3) . . ?
C4P C3P C2P 123.2(3) . . ?
C8P C3P C2P 118.0(3) . . ?
C10 O4 H4 109.5 . . ?
O2 C4 C5 123.8(2) . . ?
O2 C4 C3 116.0(2) . . ?
C5 C4 C3 120.2(2) . . ?
C26P N4P C30P 116.5(2) . . ?
C5P C4P C3P 121.2(3) . . ?
C5P C4P H4P 119.4 . . ?
C3P C4P H4P 119.4 . . ?
C11 O5 H5 109.5 . . ?
C4 C5 O3 116.1(2) . . ?
C4 C5 C6 121.1(2) . . ?
O3 C5 C6 122.7(2) . . ?
N6P N5P C26P 119.8(2) . . ?
N6P N5P H5P 120.1 . . ?
C26P N5P H5P 120.1 . . ?
C4P C5P C6P 120.3(3) . . ?
C4P C5P H16 119.9 . . ?
C6P C5P H16 119.9 . . ?
C12 O6 H6 109.5 . . ?
C5 C6 C1 117.1(2) . . ?
C5 C6 C7 121.5(2) . . ?
C1 C6 C7 121.4(2) . . ?
C17P N6P N5P 119.9(2) . . ?
C7P C6P C5P 119.1(3) . . ?
C7P C6P H6P 120.4 . . ?
C5P C6P H6P 120.4 . . ?
C17 O7 H7 109.5 . . ?
C9 C7 C6 110.5(2) . . ?
C9 C7 C29 115.3(2) . . ?
C6 C7 C29 110.4(2) . . ?
C9 C7 H17 106.7 . . ?
C6 C7 H17 106.7 . . ?
C29 C7 H17 106.7 . . ?
C6P C7P C8P 121.8(3) . . ?
C6P C7P H7P 119.1 . . ?
C8P C7P H7P 119.1 . . ?
C18 O8 H8 109.5 . . ?
C13 C8 C9 122.9(2) . . ?
C13 C8 H18 118.5 . . ?
C9 C8 H18 118.5 . . ?
C7P C8P C3P 118.8(3) . . ?
C7P C8P C9P 122.1(3) . . ?
C3P C8P C9P 119.1(3) . . ?
C19 O9 H9 109.5 . . ?
C10 C9 C8 117.2(2) . . ?
C10 C9 C7 119.8(2) . . ?
C8 C9 C7 122.9(2) . . ?
C10P C9P C8P 123.6(3) . . ?
C10P C9P H9P 118.2 . . ?
C8P C9P H9P 118.2 . . ?
C24 O10 H10 109.5 . . ?
O4 C10 C11 119.3(2) . . ?
O4 C10 C9 119.4(2) . . ?
C11 C10 C9 121.3(2) . . ?
C9P C10P C1P 120.9(3) . . ?
C9P C10P H10P 119.5 . . ?
C1P C10P H10P 119.5 . . ?
C25 O11 H11 109.5 . . ?
O5 C11 C10 118.2(2) . . ?
O5 C11 C12 121.7(2) . . ?
C10 C11 C12 120.1(2) . . ?
N1P C11P C12P 124.5(2) . . ?
N1P C11P N2P 112.4(2) . . ?
C12P C11P N2P 123.1(2) . . ?
C26 O12 H12 109.5 . . ?
O6 C12 C11 114.5(2) . . ?
O6 C12 C13 124.8(2) . . ?
C11 C12 C13 120.6(2) . . ?
C13P C12P C11P 117.8(3) . . ?
C13P C12P H12P 121.1 . . ?
C11P C12P H12P 121.1 . . ?
C8 C13 C12 117.9(2) . . ?
C8 C13 C14 123.0(2) . . ?
C12 C13 C14 119.1(2) . . ?
C12P C13P C14P 119.2(3) . . ?
C12P C13P H13P 120.4 . . ?
C14P C13P H13P 120.4 . . ?
C13 C14 C16 110.29(19) . . ?
C13 C14 C32 114.2(2) . . ?
C16 C14 C32 111.4(2) . . ?
C13 C14 H14 106.9 . . ?
C16 C14 H14 106.9 . . ?
C32 C14 H14 106.9 . . ?
C15P C14P C13P 118.7(2) . . ?
C15P C14P H14P 120.6 . . ?
C13P C14P H14P 120.6 . . ?
C16 C15 C20 123.2(2) . . ?
C16 C15 H15 118.4 . . ?
C20 C15 H15 118.4 . . ?
N1P C15P C14P 123.6(3) . . ?
N1P C15P H15P 118.2 . . ?
C14P C15P H15P 118.2 . . ?
C15 C16 C17 117.9(2) . . ?
C15 C16 C14 120.5(2) . . ?
C17 C16 C14 121.7(2) . . ?
O2P C16P C25P 121.4(2) . . ?
O2P C16P C17P 120.6(2) . . ?
C25P C16P C17P 117.9(2) . . ?
C16 C17 O7 118.6(2) . . ?
C16 C17 C18 121.1(2) . . ?
O7 C17 C18 120.2(2) . . ?
N6P C17P C18P 116.6(2) . . ?
N6P C17P C16P 123.9(2) . . ?
C18P C17P C16P 119.5(2) . . ?
O8 C18 C17 116.8(2) . . ?
O8 C18 C19 123.5(2) . . ?
C17 C18 C19 119.7(2) . . ?
C19P C18P C23P 118.8(2) . . ?
C19P C18P C17P 122.3(2) . . ?
C23P C18P C17P 118.9(2) . . ?
O9 C19 C18 116.2(2) . . ?
O9 C19 C20 123.2(2) . . ?
C18 C19 C20 120.6(2) . . ?
C20P C19P C18P 120.9(2) . . ?
C20P C19P H19P 119.6 . . ?
C18P C19P H19P 119.6 . . ?
C15 C20 C19 117.5(2) . . ?
C15 C20 C21 119.7(2) . . ?
C19 C20 C21 122.8(2) . . ?
C19P C20P C21P 120.5(3) . . ?
C19P C20P H20P 119.8 . . ?
C21P C20P H20P 119.8 . . ?
C23 C21 C20 109.48(19) . . ?
C23 C21 C35 113.6(2) . . ?
C20 C21 C35 111.3(2) . . ?
C23 C21 H21 107.4 . . ?
C20 C21 H21 107.4 . . ?
C35 C21 H21 107.4 . . ?
C22P C21P C20P 119.7(2) . . ?
C22P C21P H21P 120.1 . . ?
C20P C21P H21P 120.1 . . ?
C23 C22 C27 123.3(2) . . ?
C23 C22 H22 118.3 . . ?
C27 C22 H22 118.3 . . ?
C21P C22P C23P 120.8(2) . . ?
C21P C22P H22P 119.6 . . ?
C23P C22P H22P 119.6 . . ?
C22 C23 C24 117.6(2) . . ?
C22 C23 C21 123.6(2) . . ?
C24 C23 C21 118.7(2) . . ?
C22P C23P C18P 119.3(2) . . ?
C22P C23P C24P 121.0(2) . . ?
C18P C23P C24P 119.6(2) . . ?
O10 C24 C25 120.0(2) . . ?
O10 C24 C23 118.9(2) . . ?
C25 C24 C23 121.1(2) . . ?
C25P C24P C23P 122.7(2) . . ?
C25P C24P H24P 118.6 . . ?
C23P C24P H24P 118.6 . . ?
O11 C25 C24 115.8(2) . . ?
O11 C25 C26 124.0(2) . . ?
C24 C25 C26 120.1(2) . . ?
C24P C25P C16P 121.4(2) . . ?
C24P C25P H25P 119.3 . . ?
C16P C25P H25P 119.3 . . ?
O12 C26 C25 115.6(2) . . ?
O12 C26 C27 123.7(2) . . ?
C25 C26 C27 120.7(2) . . ?
N4P C26P N5P 114.3(2) . . ?
N4P C26P C27P 123.8(2) . . ?
N5P C26P C27P 121.9(2) . . ?
C26 C27 C22 117.2(2) . . ?
C26 C27 C28 120.9(2) . . ?
C22 C27 C28 121.9(2) . . ?
C28P C27P C26P 117.7(2) . . ?
C28P C27P H27P 121.1 . . ?
C26P C27P H27P 121.1 . . ?
C27 C28 C2 110.21(19) . . ?
C27 C28 C38 112.45(19) . . ?
C2 C28 C38 111.2(2) . . ?
C27 C28 H28 107.6 . . ?
C2 C28 H28 107.6 . . ?
C38 C28 H28 107.6 . . ?
C27P C28P C29P 119.6(3) . . ?
C27P C28P H28P 120.2 . . ?
C29P C28P H28P 120.2 . . ?
C30 C29 C7 114.6(2) . . ?
C30 C29 H29A 108.6 . . ?
C7 C29 H29A 108.6 . . ?
C30 C29 H29B 108.6 . . ?
C7 C29 H29B 108.6 . . ?
H29A C29 H29B 107.6 . . ?
C30P C29P C28P 118.5(3) . . ?
C30P C29P H29P 120.8 . . ?
C28P C29P H29P 120.8 . . ?
C31 C30 C29 111.8(3) . . ?
C31 C30 H30A 109.3 . . ?
C29 C30 H30A 109.3 . . ?
C31 C30 H30B 109.3 . . ?
C29 C30 H30B 109.3 . . ?
H30A C30 H30B 107.9 . . ?
N4P C30P C29P 124.0(3) . . ?
N4P C30P H30P 118.0 . . ?
C29P C30P H30P 118.0 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C14 C32 C33 112.0(2) . . ?
C14 C32 H32A 109.2 . . ?
C33 C32 H32A 109.2 . . ?
C14 C32 H32B 109.2 . . ?
C33 C32 H32B 109.2 . . ?
H32A C32 H32B 107.9 . . ?
C34 C33 C32 111.9(2) . . ?
C34 C33 H33A 109.2 . . ?
C32 C33 H33A 109.2 . . ?
C34 C33 H33B 109.2 . . ?
C32 C33 H33B 109.2 . . ?
H33A C33 H33B 107.9 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C36 C35 C21 113.5(2) . . ?
C36 C35 H35A 108.9 . . ?
C21 C35 H35A 108.9 . . ?
C36 C35 H35B 108.9 . . ?
C21 C35 H35B 108.9 . . ?
H35A C35 H35B 107.7 . . ?
C37 C36 C35 112.8(2) . . ?
C37 C36 H36A 109.0 . . ?
C35 C36 H36A 109.0 . . ?
C37 C36 H36B 109.0 . . ?
C35 C36 H36B 109.0 . . ?
H36A C36 H36B 107.8 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C39 C38 C28 113.9(2) . . ?
C39 C38 H38A 108.8 . . ?
C28 C38 H38A 108.8 . . ?
C39 C38 H38B 108.8 . . ?
C28 C38 H38B 108.8 . . ?
H38A C38 H38B 107.7 . . ?
C40 C39 C38 111.9(2) . . ?
C40 C39 H39A 109.2 . . ?
C38 C39 H39A 109.2 . . ?
C40 C39 H39B 109.2 . . ?
C38 C39 H39B 109.2 . . ?
H39A C39 H39B 107.9 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?

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
C6 C1 C2 C3 -0.2(3) . . . . ?
C6 C1 C2 C28 177.6(2) . . . . ?
O1P C1P C2P N3P 1.5(4) . . . . ?
C10P C1P C2P N3P -177.7(3) . . . . ?
O1P C1P C2P C3P 180.0(3) . . . . ?
C10P C1P C2P C3P 0.7(4) . . . . ?
C1 C2 C3 O1 178.6(2) . . . . ?
C28 C2 C3 O1 0.8(3) . . . . ?
C1 C2 C3 C4 2.4(3) . . . . ?
C28 C2 C3 C4 -175.3(2) . . . . ?
C11P N2P N3P C2P 174.2(2) . . . . ?
C1P C2P N3P N2P -1.3(4) . . . . ?
C3P C2P N3P N2P -179.8(2) . . . . ?
N3P C2P C3P C4P -0.3(4) . . . . ?
C1P C2P C3P C4P -178.8(3) . . . . ?
N3P C2P C3P C8P 179.7(2) . . . . ?
C1P C2P C3P C8P 1.2(4) . . . . ?
O1 C3 C4 O2 3.1(3) . . . . ?
C2 C3 C4 O2 179.2(2) . . . . ?
O1 C3 C4 C5 -177.7(2) . . . . ?
C2 C3 C4 C5 -1.6(4) . . . . ?
C8P C3P C4P C5P -0.1(4) . . . . ?
C2P C3P C4P C5P 179.9(3) . . . . ?
O2 C4 C5 O3 -4.0(4) . . . . ?
C3 C4 C5 O3 176.8(2) . . . . ?
O2 C4 C5 C6 177.5(2) . . . . ?
C3 C4 C5 C6 -1.7(4) . . . . ?
C3P C4P C5P C6P 0.9(4) . . . . ?
C4 C5 C6 C1 3.8(3) . . . . ?
O3 C5 C6 C1 -174.5(2) . . . . ?
C4 C5 C6 C7 -176.7(2) . . . . ?
O3 C5 C6 C7 5.0(4) . . . . ?
C2 C1 C6 C5 -2.9(3) . . . . ?
C2 C1 C6 C7 177.6(2) . . . . ?
C26P N5P N6P C17P 176.9(2) . . . . ?
C4P C5P C6P C7P 0.1(4) . . . . ?
C5 C6 C7 C9 -104.9(3) . . . . ?
C1 C6 C7 C9 74.6(3) . . . . ?
C5 C6 C7 C29 126.3(2) . . . . ?
C1 C6 C7 C29 -54.2(3) . . . . ?
C5P C6P C7P C8P -1.9(4) . . . . ?
C6P C7P C8P C3P 2.6(4) . . . . ?
C6P C7P C8P C9P -177.4(3) . . . . ?
C4P C3P C8P C7P -1.5(4) . . . . ?
C2P C3P C8P C7P 178.4(3) . . . . ?
C4P C3P C8P C9P 178.5(3) . . . . ?
C2P C3P C8P C9P -1.5(4) . . . . ?
C13 C8 C9 C10 0.1(4) . . . . ?
C13 C8 C9 C7 176.2(2) . . . . ?
C6 C7 C9 C10 76.8(3) . . . . ?
C29 C7 C9 C10 -157.1(2) . . . . ?
C6 C7 C9 C8 -99.2(3) . . . . ?
C29 C7 C9 C8 26.9(3) . . . . ?
C7P C8P C9P C10P 179.9(3) . . . . ?
C3P C8P C9P C10P -0.1(4) . . . . ?
C8 C9 C10 O4 -179.9(2) . . . . ?
C7 C9 C10 O4 3.9(3) . . . . ?
C8 C9 C10 C11 0.5(4) . . . . ?
C7 C9 C10 C11 -175.8(2) . . . . ?
C8P C9P C10P C1P 2.1(5) . . . . ?
O1P C1P C10P C9P 178.3(3) . . . . ?
C2P C1P C10P C9P -2.4(4) . . . . ?
O4 C10 C11 O5 -1.9(4) . . . . ?
C9 C10 C11 O5 177.7(2) . . . . ?
O4 C10 C11 C12 179.9(2) . . . . ?
C9 C10 C11 C12 -0.5(4) . . . . ?
C15P N1P C11P C12P -2.1(4) . . . . ?
C15P N1P C11P N2P 176.8(2) . . . . ?
N3P N2P C11P N1P -175.1(2) . . . . ?
N3P N2P C11P C12P 3.9(4) . . . . ?
O5 C11 C12 O6 0.6(3) . . . . ?
C10 C11 C12 O6 178.7(2) . . . . ?
O5 C11 C12 C13 -178.2(2) . . . . ?
C10 C11 C12 C13 -0.1(4) . . . . ?
N1P C11P C12P C13P 1.4(4) . . . . ?
N2P C11P C12P C13P -177.4(2) . . . . ?
C9 C8 C13 C12 -0.6(4) . . . . ?
C9 C8 C13 C14 -179.1(2) . . . . ?
O6 C12 C13 C8 -178.1(2) . . . . ?
C11 C12 C13 C8 0.6(4) . . . . ?
O6 C12 C13 C14 0.5(4) . . . . ?
C11 C12 C13 C14 179.2(2) . . . . ?
C11P C12P C13P C14P 0.2(4) . . . . ?
C8 C13 C14 C16 106.7(3) . . . . ?
C12 C13 C14 C16 -71.8(3) . . . . ?
C8 C13 C14 C32 -19.6(3) . . . . ?
C12 C13 C14 C32 161.9(2) . . . . ?
C12P C13P C14P C15P -0.9(4) . . . . ?
C11P N1P C15P C14P 1.4(4) . . . . ?
C13P C14P C15P N1P 0.0(4) . . . . ?
C20 C15 C16 C17 1.1(3) . . . . ?
C20 C15 C16 C14 -178.9(2) . . . . ?
C13 C14 C16 C15 -74.5(3) . . . . ?
C32 C14 C16 C15 53.3(3) . . . . ?
C13 C14 C16 C17 105.5(3) . . . . ?
C32 C14 C16 C17 -126.7(2) . . . . ?
C15 C16 C17 O7 178.1(2) . . . . ?
C14 C16 C17 O7 -1.9(3) . . . . ?
C15 C16 C17 C18 0.7(3) . . . . ?
C14 C16 C17 C18 -179.3(2) . . . . ?
N5P N6P C17P C18P 178.8(2) . . . . ?
N5P N6P C17P C16P -1.5(4) . . . . ?
O2P C16P C17P N6P -2.2(4) . . . . ?
C25P C16P C17P N6P 178.2(2) . . . . ?
O2P C16P C17P C18P 177.5(2) . . . . ?
C25P C16P C17P C18P -2.1(3) . . . . ?
C16 C17 C18 O8 179.5(2) . . . . ?
O7 C17 C18 O8 2.1(3) . . . . ?
C16 C17 C18 C19 -0.4(4) . . . . ?
O7 C17 C18 C19 -177.8(2) . . . . ?
N6P C17P C18P C19P 1.0(4) . . . . ?
C16P C17P C18P C19P -178.7(2) . . . . ?
N6P C17P C18P C23P -178.6(2) . . . . ?
C16P C17P C18P C23P 1.7(3) . . . . ?
O8 C18 C19 O9 -1.7(4) . . . . ?
C17 C18 C19 O9 178.2(2) . . . . ?
O8 C18 C19 C20 178.5(2) . . . . ?
C17 C18 C19 C20 -1.6(4) . . . . ?
C23P C18P C19P C20P -0.3(4) . . . . ?
C17P C18P C19P C20P -179.9(2) . . . . ?
C16 C15 C20 C19 -3.1(3) . . . . ?
C16 C15 C20 C21 177.2(2) . . . . ?
O9 C19 C20 C15 -176.6(2) . . . . ?
C18 C19 C20 C15 3.3(3) . . . . ?
O9 C19 C20 C21 3.2(4) . . . . ?
C18 C19 C20 C21 -177.0(2) . . . . ?
C18P C19P C20P C21P 0.4(4) . . . . ?
C15 C20 C21 C23 72.4(3) . . . . ?
C19 C20 C21 C23 -107.4(3) . . . . ?
C15 C20 C21 C35 -54.1(3) . . . . ?
C19 C20 C21 C35 126.2(2) . . . . ?
C19P C20P C21P C22P -0.2(4) . . . . ?
C20P C21P C22P C23P 0.0(4) . . . . ?
C27 C22 C23 C24 0.9(4) . . . . ?
C27 C22 C23 C21 178.4(2) . . . . ?
C20 C21 C23 C22 -105.5(3) . . . . ?
C35 C21 C23 C22 19.6(3) . . . . ?
C20 C21 C23 C24 72.1(3) . . . . ?
C35 C21 C23 C24 -162.8(2) . . . . ?
C21P C22P C23P C18P 0.1(4) . . . . ?
C21P C22P C23P C24P -179.9(2) . . . . ?
C19P C18P C23P C22P 0.1(4) . . . . ?
C17P C18P C23P C22P 179.7(2) . . . . ?
C19P C18P C23P C24P -180.0(2) . . . . ?
C17P C18P C23P C24P -0.3(4) . . . . ?
C22 C23 C24 O10 177.6(2) . . . . ?
C21 C23 C24 O10 -0.1(3) . . . . ?
C22 C23 C24 C25 -0.3(4) . . . . ?
C21 C23 C24 C25 -178.0(2) . . . . ?
C22P C23P C24P C25P 179.4(3) . . . . ?
C18P C23P C24P C25P -0.6(4) . . . . ?
O10 C24 C25 O11 -3.5(3) . . . . ?
C23 C24 C25 O11 174.4(2) . . . . ?
O10 C24 C25 C26 -179.7(2) . . . . ?
C23 C24 C25 C26 -1.8(4) . . . . ?
C23P C24P C25P C16P 0.1(4) . . . . ?
O2P C16P C25P C24P -178.4(2) . . . . ?
C17P C16P C25P C24P 1.3(4) . . . . ?
O11 C25 C26 O12 7.0(3) . . . . ?
C24 C25 C26 O12 -177.2(2) . . . . ?
O11 C25 C26 C27 -172.4(2) . . . . ?
C24 C25 C26 C27 3.5(4) . . . . ?
C30P N4P C26P N5P 178.9(2) . . . . ?
C30P N4P C26P C27P -0.9(4) . . . . ?
N6P N5P C26P N4P 176.9(2) . . . . ?
N6P N5P C26P C27P -3.3(4) . . . . ?
O12 C26 C27 C22 177.8(2) . . . . ?
C25 C26 C27 C22 -2.9(4) . . . . ?
O12 C26 C27 C28 -5.5(4) . . . . ?
C25 C26 C27 C28 173.8(2) . . . . ?
C23 C22 C27 C26 0.7(4) . . . . ?
C23 C22 C27 C28 -175.9(2) . . . . ?
N4P C26P C27P C28P 0.8(4) . . . . ?
N5P C26P C27P C28P -179.0(2) . . . . ?
C26 C27 C28 C2 -70.7(3) . . . . ?
C22 C27 C28 C2 105.9(2) . . . . ?
C26 C27 C28 C38 164.6(2) . . . . ?
C22 C27 C28 C38 -18.9(3) . . . . ?
C1 C2 C28 C27 -74.8(3) . . . . ?
C3 C2 C28 C27 102.8(2) . . . . ?
C1 C2 C28 C38 50.6(3) . . . . ?
C3 C2 C28 C38 -131.7(2) . . . . ?
C26P C27P C28P C29P 0.2(4) . . . . ?
C9 C7 C29 C30 61.6(3) . . . . ?
C6 C7 C29 C30 -172.2(2) . . . . ?
C27P C28P C29P C30P -1.0(4) . . . . ?
C7 C29 C30 C31 176.9(2) . . . . ?
C26P N4P C30P C29P 0.0(4) . . . . ?
C28P C29P C30P N4P 0.9(5) . . . . ?
C13 C14 C32 C33 -173.3(2) . . . . ?
C16 C14 C32 C33 61.0(3) . . . . ?
C14 C32 C33 C34 179.1(2) . . . . ?
C23 C21 C35 C36 172.1(2) . . . . ?
C20 C21 C35 C36 -63.7(3) . . . . ?
C21 C35 C36 C37 179.1(2) . . . . ?
C27 C28 C38 C39 -173.9(2) . . . . ?
C2 C28 C38 C39 62.0(3) . . . . ?
C28 C38 C39 C40 -175.0(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        29.01
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.513
_refine_diff_density_min         -0.841
_refine_diff_density_rms         0.064

_database_code_depnum_ccdc_archive 'CCDC 1002508'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2cp81h

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            
'C-propylpyrogallol[4]arene with 1-(2-pyridylazo)-2-napthol'
_chemical_formula_moiety         'C40 H48 O16, C15 H11 O1 N3, C2 H6 O1'
_chemical_formula_sum            'C57 H65 N3 O18'
_chemical_melting_point          ?

_exptl_crystal_description       prism
_exptl_crystal_colour            orange

_diffrn_ambient_temperature      100(2)
_chemical_formula_weight         1080.12

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0020 0.0020 '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 -0.0031 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O -0.0041 0.0074 '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
_chemical_absolute_configuration ?

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

_cell_length_a                   11.8485(16)
_cell_length_b                   12.7498(17)
_cell_length_c                   18.287(2)
_cell_angle_alpha                84.294(2)
_cell_angle_beta                 85.839(2)
_cell_angle_gamma                63.720(2)
_cell_volume                     2463.5(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5271
_cell_measurement_theta_min      3.2
_cell_measurement_theta_max      31.2
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1144
_exptl_absorpt_coefficient_mu    0.131
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_process_details   
;
 Data were corrected for decay and absorption using the program SADABS 
 (Sheldrick, G. M. (2003). SADABS. Version 2.10. University of
 Göttingen, Germany).
;

_exptl_special_details           
; 
 ? 
;
_diffrn_radiation_probe          ?
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_source                   'Advanced Light Source Station 11.3.1'
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker APEXII CCD diffractometer'
_diffrn_measurement_method       'ω/θ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.0
_diffrn_reflns_number            33711
_diffrn_reflns_av_R_equivalents  0.0649
_diffrn_reflns_av_sigmaI/netI    0.0855
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         32.07
_reflns_number_total             13132
_reflns_number_gt                9453
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2008)'
_computing_structure_solution    'SHELXS-1997 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-1997 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-SEED, Barbour, 2001'
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. The short D-H, H-X distances
 and the D-H without acceptor are all due to disorder of the tail groups, 
 solvent, and tail hydroxyl groups. The tail hydroxyl groups are disordered
 but not modeled. There are no bonds between C1E and H3E1 or C2E and H1E'.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0791P)²+1.0413P] where P=(Fo²+2Fc²)/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         13132
_refine_ls_number_parameters     759
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0863
_refine_ls_R_factor_gt           0.0631
_refine_ls_wR_factor_ref         0.1850
_refine_ls_wR_factor_gt          0.1649
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.085
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.75495(14) 0.65675(12) 0.95194(7) 0.0198(3) Uani 1 1 d . . .
H1 H 0.7861 0.6928 0.9733 0.024 Uiso 1 1 calc R . .
O2 O 0.89718(14) 0.77745(13) 0.88958(8) 0.0220(3) Uani 1 1 d . . .
H2 H 0.8409 0.8152 0.9202 0.026 Uiso 1 1 calc R . .
O9 O 1.04527(14) -0.09328(13) 0.81164(8) 0.0236(3) Uani 1 1 d . . .
H9 H 1.1178 -0.1342 0.8277 0.028 Uiso 1 1 d . . .
O3 O 0.95087(15) 0.77880(13) 0.74310(8) 0.0236(3) Uani 1 1 d . . .
H3 H 0.9674 0.8104 0.7763 0.028 Uiso 1 1 calc R . .
O11 O 0.92762(15) 0.19914(13) 1.02560(8) 0.0246(3) Uani 1 1 d . . .
H11 H 0.9326 0.2525 1.0466 0.029 Uiso 1 1 calc R . .
O7 O 1.27247(13) 0.01751(13) 0.61616(9) 0.0251(3) Uani 1 1 d . . .
H7 H 1.3298 -0.0464 0.6325 0.030 Uiso 1 1 calc R . .
O12 O 0.80003(15) 0.43287(13) 1.00093(8) 0.0240(3) Uani 1 1 d . . .
H12 H 0.7779 0.5024 0.9837 0.029 Uiso 1 1 calc R . .
O6 O 1.30754(13) 0.21616(13) 0.60620(9) 0.0254(3) Uani 1 1 d . . .
H6 H 1.2887 0.1601 0.6052 0.030 Uiso 1 1 calc R . .
O10 O 0.93801(15) 0.05082(12) 0.92933(9) 0.0264(3) Uani 1 1 d . . .
H10 H 0.9643 0.0402 0.9721 0.032 Uiso 0.50 1 calc PR A 1
O8 O 1.26752(14) -0.13956(13) 0.72460(9) 0.0303(4) Uani 1 1 d . . .
H8 H 1.2530 -0.1858 0.7555 0.036 Uiso 1 1 d . . .
O15 O 0.56728(14) 0.23723(13) 0.60433(9) 0.0279(3) Uani 1 1 d . . .
H15 H 0.6266 0.2404 0.5777 0.033 Uiso 1 1 d . . .
O4 O 1.14503(15) 0.59959(14) 0.67449(9) 0.0291(3) Uani 1 1 d . . .
H4 H 1.0789 0.6540 0.6903 0.035 Uiso 1 1 calc R . .
O5 O 1.33575(15) 0.39748(15) 0.65276(10) 0.0331(4) Uani 1 1 d . . .
H5 H 1.3911 0.3344 0.6375 0.040 Uiso 1 1 calc R . .
O1P O 0.68548(18) 1.13650(14) 1.05727(9) 0.0349(4) Uani 1 1 d . . .
N3P N 0.85153(16) 0.70954(14) 1.05815(9) 0.0200(3) Uani 1 1 d . . .
N2P N 0.78081(17) 0.91291(15) 1.05592(9) 0.0218(3) Uani 1 1 d . . .
H2P H 0.7835 0.9737 1.0733 0.026 Uiso 1 1 calc R . .
N1P N 0.71619(16) 0.92729(15) 0.99646(9) 0.0212(3) Uani 1 1 d . . .
O14 O 0.71667(18) 0.2488(2) 0.48302(11) 0.0309(4) Uani 0.80 1 d P B 1
H14 H 0.6621 0.2753 0.4506 0.037 Uiso 0.80 1 calc PR B 1
O13 O 0.48307(18) 0.83011(19) 0.62576(13) 0.0602(7) Uani 1 1 d . . .
C20 C 0.94317(17) 0.09505(16) 0.74385(10) 0.0161(3) Uani 1 1 d . . .
C15 C 0.95145(17) 0.17284(16) 0.68708(10) 0.0165(3) Uani 1 1 d . . .
H18 H 0.8803 0.2462 0.6783 0.020 Uiso 1 1 calc R . .
C3 C 0.78468(18) 0.66021(16) 0.87811(10) 0.0176(4) Uani 1 1 d . . .
C2 C 0.74216(17) 0.60347(16) 0.83341(10) 0.0164(3) Uani 1 1 d . . .
C1 C 0.77519(18) 0.60394(16) 0.75890(10) 0.0183(4) Uani 1 1 d . . .
H19 H 0.7488 0.5635 0.7283 0.022 Uiso 1 1 calc R . .
C13 C 1.07899(18) 0.33328(16) 0.59991(10) 0.0172(4) Uani 1 1 d . . .
C8 C 0.97875(18) 0.44311(16) 0.60959(10) 0.0181(4) Uani 1 1 d . . .
H16 H 0.8963 0.4552 0.5992 0.022 Uiso 1 1 calc R . .
C9 C 0.99473(18) 0.53555(16) 0.63384(10) 0.0185(4) Uani 1 1 d . . .
C22 C 0.74144(17) 0.33284(16) 0.83172(10) 0.0168(4) Uani 1 1 d . . .
H22 H 0.6997 0.3627 0.7865 0.020 Uiso 1 1 calc R . .
C19 C 1.04954(18) -0.01148(16) 0.75710(10) 0.0175(4) Uani 1 1 d . . .
C17 C 1.16431(18) 0.04238(17) 0.65814(11) 0.0192(4) Uani 1 1 d . . .
C4 C 0.85278(18) 0.72008(16) 0.84796(11) 0.0185(4) Uani 1 1 d . . .
C21 C 0.82054(17) 0.12597(16) 0.78880(10) 0.0165(3) Uani 1 1 d . . .
H21 H 0.8267 0.0521 0.8167 0.020 Uiso 1 1 calc R . .
C6 C 0.84541(18) 0.66125(16) 0.72711(10) 0.0183(4) Uani 1 1 d . . .
C27 C 0.73352(17) 0.41260(16) 0.88108(10) 0.0168(4) Uani 1 1 d . . .
C16 C 1.05931(17) 0.14783(16) 0.64268(10) 0.0166(4) Uani 1 1 d . . .
C14 C 1.06080(18) 0.23062(16) 0.57619(10) 0.0179(4) Uani 0.80 1 d P B 1
H20 H 1.1366 0.1847 0.5450 0.022 Uiso 0.80 1 calc PR B 1
C23 C 0.80743(17) 0.21137(16) 0.84512(10) 0.0166(3) Uani 1 1 d . . .
C18 C 1.16060(18) -0.03776(16) 0.71497(11) 0.0202(4) Uani 1 1 d . . .
C38 C 0.54224(18) 0.58423(17) 0.82044(11) 0.0208(4) Uani 0.50 1 d P C 1
H38A H 0.5058 0.6702 0.8088 0.025 Uiso 0.50 1 calc PR C 1
H38B H 0.5671 0.5463 0.7734 0.025 Uiso 0.50 1 calc PR C 1
C12 C 1.19979(18) 0.31789(17) 0.61481(11) 0.0196(4) Uani 1 1 d . B .
C5 C 0.88159(18) 0.72108(16) 0.77302(11) 0.0195(4) Uani 1 1 d . B .
C24 C 0.86905(18) 0.16873(16) 0.91181(10) 0.0176(4) Uani 1 1 d . . .
C32 C 0.94577(19) 0.26632(18) 0.52882(11) 0.0209(4) Uani 0.80 1 d P B 1
H32A H 0.8679 0.3082 0.5585 0.025 Uiso 0.80 1 calc PR B 1
H32B H 0.9485 0.3206 0.4869 0.025 Uiso 0.80 1 calc PR B 1
C25 C 0.86388(18) 0.24564(17) 0.96195(10) 0.0186(4) Uani 1 1 d . . .
C11P C 0.84437(18) 0.80126(17) 1.09085(11) 0.0196(4) Uani 1 1 d . . .
C26 C 0.79705(18) 0.36647(17) 0.94681(10) 0.0184(4) Uani 1 1 d . . .
C7 C 0.88572(19) 0.65440(17) 0.64579(11) 0.0203(4) Uani 1 1 d . B .
H17 H 0.9185 0.7143 0.6334 0.024 Uiso 1 1 calc R . .
C28 C 0.65990(18) 0.54538(16) 0.86605(10) 0.0170(4) Uani 0.50 1 d P C 1
H28 H 0.6287 0.5773 0.9152 0.020 Uiso 0.50 1 calc PR C 1
C11 C 1.21872(19) 0.40904(18) 0.63800(11) 0.0216(4) Uani 1 1 d . . .
C35 C 0.70746(18) 0.16991(17) 0.73855(11) 0.0188(4) Uani 1 1 d . . .
H35A H 0.6299 0.1870 0.7693 0.023 Uiso 1 1 calc R C .
H35B H 0.6981 0.2440 0.7109 0.023 Uiso 1 1 calc R . .
C10 C 1.1165(2) 0.51605(18) 0.64923(11) 0.0212(4) Uani 1 1 d . B .
C15P C 0.90481(19) 0.60361(18) 1.09582(11) 0.0229(4) Uani 1 1 d . . .
H15P H 0.9117 0.5371 1.0731 0.027 Uiso 1 1 calc R . .
C12P C 0.89224(19) 0.79182(19) 1.15993(11) 0.0228(4) Uani 1 1 d . . .
H12P H 0.8887 0.8588 1.1806 0.027 Uiso 1 1 calc R . .
C29 C 0.7732(2) 0.68827(18) 0.59720(11) 0.0244(4) Uani 1 1 d . . .
H29A H 0.7245 0.6447 0.6163 0.029 Uiso 1 1 calc R B .
H29B H 0.8037 0.6663 0.5466 0.029 Uiso 1 1 calc R . .
C2P C 0.6394(2) 1.03413(17) 0.97073(11) 0.0234(4) Uani 1 1 d . . .
C13P C 0.94472(19) 0.6830(2) 1.19730(11) 0.0245(4) Uani 1 1 d . . .
H13P H 0.9773 0.6737 1.2447 0.029 Uiso 1 1 calc R . .
C39 C 0.4421(2) 0.5530(2) 0.86039(13) 0.0267(4) Uani 0.50 1 d P C 1
H39A H 0.4694 0.4683 0.8563 0.032 Uiso 0.50 1 calc PR C 1
H39B H 0.4432 0.5638 0.9132 0.032 Uiso 0.50 1 calc PR C 1
C36 C 0.72109(19) 0.08143(18) 0.68409(12) 0.0229(4) Uani 1 1 d . C .
H36A H 0.7956 0.0681 0.6512 0.027 Uiso 1 1 calc R . .
H36B H 0.7358 0.0058 0.7115 0.027 Uiso 1 1 calc R . .
C14P C 0.94974(19) 0.58690(19) 1.16547(11) 0.0233(4) Uani 1 1 d . . .
H14P H 0.9833 0.5114 1.1910 0.028 Uiso 1 1 calc R . .
C3P C 0.56330(19) 1.04270(19) 0.90884(12) 0.0248(4) Uani 1 1 d . . .
C37 C 0.6058(2) 0.12188(19) 0.63770(12) 0.0244(4) Uani 1 1 d . . .
H37A H 0.6246 0.0671 0.5989 0.029 Uiso 1 1 calc R C .
H37B H 0.5355 0.1189 0.6692 0.029 Uiso 1 1 calc R . .
C33 C 0.9425(2) 0.1591(2) 0.49977(13) 0.0295(5) Uani 0.80 1 d P B 1
H33A H 1.0232 0.1152 0.4730 0.035 Uiso 0.80 1 calc PR B 1
H33B H 0.9367 0.1071 0.5423 0.035 Uiso 0.80 1 calc PR B 1
C8P C 0.4792(2) 1.1553(2) 0.87866(13) 0.0312(5) Uani 1 1 d . . .
C4P C 0.5667(2) 0.9444(2) 0.87955(12) 0.0279(5) Uani 1 1 d . . .
H4P H 0.6190 0.8683 0.9008 0.033 Uiso 1 1 calc R . .
C1P C 0.6249(2) 1.14189(19) 1.00270(13) 0.0283(5) Uani 1 1 d . . .
C5P C 0.4950(2) 0.9557(2) 0.82007(13) 0.0339(5) Uani 1 1 d . . .
H5P H 0.4997 0.8877 0.8003 0.041 Uiso 1 1 calc R . .
C34 C 0.8371(2) 0.1852(2) 0.44983(14) 0.0339(5) Uani 0.80 1 d P B 1
H34A H 0.8467 0.2310 0.4049 0.041 Uiso 0.80 1 calc PR B 1
H34B H 0.8428 0.1104 0.4349 0.041 Uiso 0.80 1 calc PR B 1
C30 C 0.6878(2) 0.8203(2) 0.59577(13) 0.0372(6) Uani 1 1 d . B .
H30A H 0.6797 0.8456 0.6461 0.045 Uiso 1 1 calc R . .
H30B H 0.7287 0.8620 0.5640 0.045 Uiso 1 1 calc R . .
C6P C 0.4159(2) 1.0670(3) 0.78918(14) 0.0379(6) Uani 1 1 d . . .
H6P H 0.3680 1.0749 0.7478 0.046 Uiso 1 1 calc R . .
C7P C 0.4077(2) 1.1648(2) 0.81864(14) 0.0378(6) Uani 1 1 d . . .
H7P H 0.3526 1.2403 0.7980 0.045 Uiso 1 1 calc R . .
C10P C 0.5379(2) 1.2525(2) 0.96868(15) 0.0355(6) Uani 1 1 d . . .
H10P H 0.5284 1.3234 0.9868 0.043 Uiso 1 1 calc R . .
C9P C 0.4697(2) 1.2573(2) 0.91162(16) 0.0386(6) Uani 1 1 d . . .
H9P H 0.4118 1.3323 0.8918 0.046 Uiso 1 1 calc R . .
C31 C 0.5584(2) 0.8565(3) 0.56841(15) 0.0471(7) Uani 1 1 d . . .
H31A H 0.5187 0.9416 0.5537 0.056 Uiso 1 1 calc R B .
H31B H 0.5641 0.8139 0.5248 0.056 Uiso 1 1 calc R . .
O1E O 0.4680(3) 0.6299(3) 0.62472(18) 0.0580(8) Uani 0.70 1 d P D 1
H1E H 0.4036 0.6212 0.6392 0.070 Uiso 0.70 1 calc PR D 1
O16 O 0.2639(3) 0.7382(3) 0.84724(17) 0.0283(7) Uani 0.50 1 d P C 1
H16A H 0.2844 0.7473 0.8883 0.034 Uiso 0.50 1 calc PR C 1
O16A O 0.3185(3) 0.6206(3) 0.7471(2) 0.0244(8) Uani 0.40 1 d P C 2
H16B H 0.2799 0.6021 0.7180 0.029 Uiso 0.40 1 calc PR C 2
C1E C 0.5720(5) 0.5150(4) 0.6095(3) 0.0514(11) Uani 0.70 1 d P D 1
H1E1 H 0.5431 0.4527 0.6131 0.062 Uiso 0.70 1 calc PR D 1
H1E2 H 0.6423 0.4923 0.6431 0.062 Uiso 0.70 1 calc PR D 1
C2E C 0.6111(4) 0.5416(4) 0.5271(2) 0.0624(11) Uani 0.70 1 d P D 1
H2E1 H 0.6816 0.4710 0.5099 0.094 Uiso 0.70 1 calc PR D 1
H2E2 H 0.6364 0.6053 0.5253 0.094 Uiso 0.70 1 calc PR D 1
H2E3 H 0.5392 0.5648 0.4955 0.094 Uiso 0.70 1 calc PR D 1
C40 C 0.3111(4) 0.6148(4) 0.8383(2) 0.0266(9) Uani 0.50 1 d P C 1
H40A H 0.3057 0.6028 0.7862 0.032 Uiso 0.50 1 calc PR C 1
H40B H 0.2593 0.5829 0.8687 0.032 Uiso 0.50 1 calc PR C 1
C40A C 0.3627(4) 0.5344(5) 0.8038(3) 0.0332(10) Uani 0.40 1 d P C 2
H40C H 0.4146 0.4586 0.7824 0.040 Uiso 0.40 1 calc PR C 2
H40D H 0.2897 0.5282 0.8303 0.040 Uiso 0.40 1 calc PR C 2
O1E' O 0.5947(12) 0.4680(12) 0.4638(7) 0.111(4) Uiso 0.15 1 d P E -2
H1E' H 0.6501 0.4921 0.4520 0.133 Uiso 0.15 1 d P F -2
C3F C 0.4915(10) 0.6633(9) 0.5325(7) 0.022(3) Uiso 0.15 1 d PD G 3
H3F1 H 0.4967 0.6998 0.5762 0.033 Uiso 0.15 1 d P H 3
H3F2 H 0.4155 0.6510 0.5364 0.033 Uiso 0.15 1 d P I 3
H3F3 H 0.4890 0.7147 0.4885 0.033 Uiso 0.15 1 d P J 3
O14A O 0.7432(14) 0.3084(13) 0.4390(8) 0.079(4) Uiso 0.20 1 d P B 2
H14A H 0.6926 0.3251 0.4766 0.095 Uiso 0.20 1 d P K 2
O16B O 0.4166(14) 0.4975(13) 0.7358(8) 0.026(3) Uiso 0.10 1 d P C 3
H16C H 0.4063 0.5567 0.7065 0.032 Uiso 0.10 1 d P L 3
C3E' C 0.6274(13) 0.4356(13) 0.6154(7) 0.024(3) Uiso 0.15 1 d PD E -2
H3E1 H 0.5785 0.4286 0.6591 0.036 Uiso 0.15 1 d P M -2
H3E2 H 0.6759 0.4775 0.6249 0.036 Uiso 0.15 1 d P N -2
H3E3 H 0.6859 0.3562 0.6009 0.036 Uiso 0.15 1 d P O -2
C2E' C 0.5375(16) 0.5035(15) 0.5516(8) 0.039(4) Uiso 0.15 1 d PD E -2
H2E4 H 0.5118 0.5882 0.5543 0.047 Uiso 0.15 1 calc PR E -2
H2E5 H 0.4606 0.4911 0.5600 0.047 Uiso 0.15 1 calc PR E -2
C14A C 1.06080(18) 0.23062(16) 0.57619(10) 0.0179(4) Uani 0.20 1 d P B 2
H23 H 1.1366 0.1847 0.5450 0.022 Uiso 0.20 1 calc PR B 2
C32A C 0.94577(19) 0.26632(18) 0.52882(11) 0.0209(4) Uani 0.20 1 d P B 2
H32C H 0.8679 0.3082 0.5585 0.025 Uiso 0.20 1 calc PR B 2
H32D H 0.9485 0.3206 0.4869 0.025 Uiso 0.20 1 calc PR B 2
C33A C 0.9425(2) 0.1591(2) 0.49977(13) 0.0295(5) Uani 0.20 1 d P B 2
H33C H 1.0232 0.1152 0.4730 0.035 Uiso 0.20 1 calc PR B 2
H33D H 0.9367 0.1071 0.5423 0.035 Uiso 0.20 1 calc PR B 2
C34A C 0.8371(2) 0.1852(2) 0.44983(14) 0.0339(5) Uani 0.20 1 d P B 2
H34C H 0.8743 0.1577 0.4011 0.041 Uiso 0.20 1 calc PR B 2
H34D H 0.7923 0.1381 0.4694 0.041 Uiso 0.20 1 calc PR B 2
C38A C 0.54224(18) 0.58423(17) 0.82044(11) 0.0208(4) Uani 0.40 1 d P C 2
H38C H 0.5058 0.6702 0.8088 0.025 Uiso 0.40 1 calc PR C 2
H38D H 0.5671 0.5463 0.7734 0.025 Uiso 0.40 1 calc PR C 2
C28A C 0.65990(18) 0.54538(16) 0.86605(10) 0.0170(4) Uani 0.40 1 d P C 2
H28A H 0.6287 0.5773 0.9152 0.020 Uiso 0.40 1 calc PR C 2
C39A C 0.4421(2) 0.5530(2) 0.86039(13) 0.0267(4) Uani 0.40 1 d P C 2
H39C H 0.3866 0.6170 0.8913 0.032 Uiso 0.40 1 calc PR C 2
H39D H 0.4832 0.4805 0.8929 0.032 Uiso 0.40 1 calc PR C 2
C40B C 0.3627(4) 0.5344(5) 0.8038(3) 0.0332(10) Uani 0.10 1 d P C 3
H40E H 0.3340 0.4764 0.8270 0.040 Uiso 0.10 1 calc PR C 3
H40F H 0.2865 0.6094 0.7953 0.040 Uiso 0.10 1 calc PR C 3
C2F C 0.6111(4) 0.5416(4) 0.5271(2) 0.0624(11) Uani 0.15 1 d PD G 3
H2F1 H 0.6232 0.4954 0.5752 0.075 Uiso 0.15 1 calc PR G 3
H2F2 H 0.6867 0.5550 0.5152 0.075 Uiso 0.15 1 calc PR G 3
O1F' O 0.5947(12) 0.4680(12) 0.4638(7) 0.111(4) Uiso 0.15 1 d P G 3
H1F' H 0.6536 0.3990 0.4659 0.133 Uiso 0.15 1 d P P 3
C38B C 0.54224(18) 0.58423(17) 0.82044(11) 0.0208(4) Uani 0.10 1 d P C 3
H38E H 0.5058 0.6702 0.8088 0.025 Uiso 0.10 1 calc PR C 3
H38F H 0.5671 0.5463 0.7734 0.025 Uiso 0.10 1 calc PR C 3
C28B C 0.65990(18) 0.54538(16) 0.86605(10) 0.0170(4) Uani 0.10 1 d P C 3
H28B H 0.6287 0.5773 0.9152 0.020 Uiso 0.10 1 calc PR C 3
C39B C 0.4421(2) 0.5530(2) 0.86039(13) 0.0267(4) Uani 0.10 1 d P C 3
H39E H 0.3866 0.6170 0.8913 0.032 Uiso 0.10 1 calc PR C 3
H39F H 0.4832 0.4805 0.8929 0.032 Uiso 0.10 1 calc PR C 3
H10' H 0.9648 0.0138 0.8915 0.051 Uiso 0.50 1 d P Q 2
H13 H 0.4618 0.7887 0.6015 0.050 Uiso 1 1 d . . .


_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 C3 1.372(2) . ?
O1 H1 0.8400 . ?
O2 C4 1.379(2) . ?
O2 H2 0.8400 . ?
O9 C19 1.385(2) . ?
O9 H9 0.8401 . ?
O3 C5 1.380(2) . ?
O3 H3 0.8400 . ?
O11 C25 1.368(2) . ?
O11 H11 0.8400 . ?
O7 C17 1.370(2) . ?
O7 H7 0.8400 . ?
O12 C26 1.377(2) . ?
O12 H12 0.8400 . ?
O6 C12 1.372(2) . ?
O6 H6 0.8400 . ?
O10 C24 1.373(2) . ?
O10 H10 0.8400 . ?
O10 H10' 0.8377 . ?
O8 C18 1.361(2) . ?
O8 H8 0.8400 . ?
O15 C37 1.418(3) . ?
O15 H15 0.8400 . ?
O4 C10 1.379(2) . ?
O4 H4 0.8400 . ?
O5 C11 1.372(2) . ?
O5 H5 0.8400 . ?
O1P C1P 1.250(3) . ?
N3P C11P 1.333(2) . ?
N3P C15P 1.349(3) . ?
N2P N1P 1.326(2) . ?
N2P C11P 1.393(3) . ?
N2P H2P 0.8800 . ?
N1P C2P 1.320(3) . ?
O14 C34 1.417(3) . ?
O14 H14 0.8400 . ?
O14 H14A 0.8815 . ?
O13 C31 1.438(3) . ?
O13 H13 0.8484 . ?
C20 C15 1.392(3) . ?
C20 C19 1.398(3) . ?
C20 C21 1.525(2) . ?
C15 C16 1.391(3) . ?
C15 H18 0.9500 . ?
C3 C4 1.391(3) . ?
C3 C2 1.395(3) . ?
C2 C1 1.390(3) . ?
C2 C28 1.524(3) . ?
C1 C6 1.396(3) . ?
C1 H19 0.9500 . ?
C13 C8 1.396(3) . ?
C13 C12 1.400(3) . ?
C13 C14 1.524(3) . ?
C8 C9 1.391(3) . ?
C8 H16 0.9500 . ?
C9 C10 1.397(3) . ?
C9 C7 1.518(3) . ?
C22 C27 1.394(3) . ?
C22 C23 1.396(3) . ?
C22 H22 0.9500 . ?
C19 C18 1.397(3) . ?
C17 C16 1.389(3) . ?
C17 C18 1.396(3) . ?
C4 C5 1.388(3) . ?
C21 C23 1.523(3) . ?
C21 C35 1.538(3) . ?
C21 H21 1.0000 . ?
C6 C5 1.393(3) . ?
C6 C7 1.527(3) . ?
C27 C26 1.399(3) . ?
C27 C28 1.529(3) . ?
C16 C14 1.533(3) . ?
C14 C32 1.536(3) . ?
C14 H20 1.0000 . ?
C23 C24 1.401(3) . ?
C38 C39 1.528(3) . ?
C38 C28 1.536(3) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C12 C11 1.387(3) . ?
C24 C25 1.387(3) . ?
C32 C33 1.532(3) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C25 C26 1.394(3) . ?
C11P C12P 1.395(3) . ?
C7 C29 1.529(3) . ?
C7 H17 1.0000 . ?
C28 H28 1.0000 . ?
C11 C10 1.388(3) . ?
C35 C36 1.526(3) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C15P C14P 1.377(3) . ?
C15P H15P 0.9500 . ?
C12P C13P 1.374(3) . ?
C12P H12P 0.9500 . ?
C29 C30 1.531(3) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C2P C3P 1.463(3) . ?
C2P C1P 1.482(3) . ?
C13P C14P 1.384(3) . ?
C13P H13P 0.9500 . ?
C39 C40 1.462(5) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C36 C37 1.520(3) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C14P H14P 0.9500 . ?
C3P C4P 1.395(3) . ?
C3P C8P 1.419(3) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C33 C34 1.497(3) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C8P C7P 1.398(4) . ?
C8P C9P 1.444(4) . ?
C4P C5P 1.385(3) . ?
C4P H4P 0.9500 . ?
C1P C10P 1.439(3) . ?
C5P C6P 1.397(3) . ?
C5P H5P 0.9500 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C30 C31 1.501(4) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C6P C7P 1.368(4) . ?
C6P H6P 0.9500 . ?
C7P H7P 0.9500 . ?
C10P C9P 1.346(4) . ?
C10P H10P 0.9500 . ?
C9P H9P 0.9500 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
O1E C1E 1.475(6) . ?
O1E H1E 0.8400 . ?
O1E H3F1 1.3277 . ?
O16 C40 1.440(5) . ?
O16 H16A 0.8400 . ?
O16A C40A 1.378(6) . ?
O16A H16B 0.8400 . ?
O16A H16C 1.2469 . ?
C1E C2E 1.592(7) . ?
C1E H1E1 0.9900 . ?
C1E H1E2 0.9900 . ?
C1E H3E1 1.3335 . ?
C1E H3E2 1.1509 . ?
C2E H2E1 0.9800 . ?
C2E H2E2 0.9800 . ?
C2E H2E3 0.9800 . ?
C2E H1E' 1.5233 . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C40A H40C 0.9900 . ?
C40A H40D 0.9900 . ?
O1E' C2E' 1.72(2) . ?
O1E' H1E' 0.8456 . ?
O1E' H1F' 0.8458 . ?
C3F H3F1 0.9826 . ?
C3F H3F2 0.9758 . ?
C3F H3F3 0.9801 . ?
O14A H14A 0.8574 . ?
O14A H1F' 1.2862 . ?
O16B H16C 0.8489 . ?
C3E' C2E' 1.551(9) . ?
C3E' H3E1 0.9734 . ?
C3E' H3E2 0.9749 . ?
C3E' H3E3 0.9895 . ?
C2E' H2E4 0.9900 . ?
C2E' H2E5 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3 O1 H1 109.5 . . ?
C4 O2 H2 109.5 . . ?
C19 O9 H9 109.4 . . ?
C5 O3 H3 109.5 . . ?
C25 O11 H11 109.5 . . ?
C17 O7 H7 109.5 . . ?
C26 O12 H12 109.5 . . ?
C12 O6 H6 109.5 . . ?
C24 O10 H10 109.5 . . ?
C24 O10 H10' 111.4 . . ?
H10 O10 H10' 133.9 . . ?
C18 O8 H8 109.5 . . ?
C37 O15 H15 109.5 . . ?
C10 O4 H4 109.5 . . ?
C11 O5 H5 109.5 . . ?
C11P N3P C15P 117.16(17) . . ?
N1P N2P C11P 119.78(16) . . ?
N1P N2P H2P 120.1 . . ?
C11P N2P H2P 120.1 . . ?
C2P N1P N2P 119.61(18) . . ?
C34 O14 H14A 111.4 . . ?
H14 O14 H14A 72.9 . . ?
C31 O13 H13 97.2 . . ?
C15 C20 C19 117.86(17) . . ?
C15 C20 C21 120.27(16) . . ?
C19 C20 C21 121.86(16) . . ?
C20 C15 C16 122.85(17) . . ?
C20 C15 H18 118.6 . . ?
C16 C15 H18 118.6 . . ?
O1 C3 C4 121.57(17) . . ?
O1 C3 C2 117.84(16) . . ?
C4 C3 C2 120.58(17) . . ?
C1 C2 C3 117.97(17) . . ?
C1 C2 C28 121.80(17) . . ?
C3 C2 C28 120.21(16) . . ?
C2 C1 C6 122.87(18) . . ?
C2 C1 H19 118.6 . . ?
C6 C1 H19 118.6 . . ?
C8 C13 C12 117.65(18) . . ?
C8 C13 C14 122.64(17) . . ?
C12 C13 C14 119.69(16) . . ?
C9 C8 C13 122.67(18) . . ?
C9 C8 H16 118.7 . . ?
C13 C8 H16 118.7 . . ?
C8 C9 C10 117.92(17) . . ?
C8 C9 C7 122.84(18) . . ?
C10 C9 C7 119.23(18) . . ?
C27 C22 C23 123.53(17) . . ?
C27 C22 H22 118.2 . . ?
C23 C22 H22 118.2 . . ?
O9 C19 C18 119.11(17) . . ?
O9 C19 C20 120.18(17) . . ?
C18 C19 C20 120.70(17) . . ?
O7 C17 C16 118.78(17) . . ?
O7 C17 C18 120.11(17) . . ?
C16 C17 C18 121.10(17) . . ?
O2 C4 C5 117.13(17) . . ?
O2 C4 C3 122.97(17) . . ?
C5 C4 C3 119.88(17) . . ?
C23 C21 C20 109.76(15) . . ?
C23 C21 C35 113.78(15) . . ?
C20 C21 C35 111.11(15) . . ?
C23 C21 H21 107.3 . . ?
C20 C21 H21 107.3 . . ?
C35 C21 H21 107.3 . . ?
C5 C6 C1 117.43(17) . . ?
C5 C6 C7 121.22(17) . . ?
C1 C6 C7 121.31(17) . . ?
C22 C27 C26 117.14(17) . . ?
C22 C27 C28 123.02(17) . . ?
C26 C27 C28 119.85(17) . . ?
C17 C16 C15 117.93(17) . . ?
C17 C16 C14 120.70(16) . . ?
C15 C16 C14 121.29(16) . . ?
C13 C14 C16 111.01(15) . . ?
C13 C14 C32 114.47(15) . . ?
C16 C14 C32 111.14(16) . . ?
C13 C14 H20 106.6 . . ?
C16 C14 H20 106.6 . . ?
C32 C14 H20 106.6 . . ?
C22 C23 C24 117.53(17) . . ?
C22 C23 C21 122.67(17) . . ?
C24 C23 C21 119.70(16) . . ?
O8 C18 C17 116.54(17) . . ?
O8 C18 C19 123.96(17) . . ?
C17 C18 C19 119.49(17) . . ?
C39 C38 C28 112.54(17) . . ?
C39 C38 H38A 109.1 . . ?
C28 C38 H38A 109.1 . . ?
C39 C38 H38B 109.1 . . ?
C28 C38 H38B 109.1 . . ?
H38A C38 H38B 107.8 . . ?
O6 C12 C11 114.73(18) . . ?
O6 C12 C13 124.33(18) . . ?
C11 C12 C13 120.91(18) . . ?
O3 C5 C4 120.04(17) . . ?
O3 C5 C6 118.73(17) . . ?
C4 C5 C6 121.19(17) . . ?
O10 C24 C25 117.79(17) . . ?
O10 C24 C23 121.74(17) . . ?
C25 C24 C23 120.46(17) . . ?
C33 C32 C14 111.35(17) . . ?
C33 C32 H32A 109.4 . . ?
C14 C32 H32A 109.4 . . ?
C33 C32 H32B 109.4 . . ?
C14 C32 H32B 109.4 . . ?
H32A C32 H32B 108.0 . . ?
O11 C25 C24 117.92(17) . . ?
O11 C25 C26 121.56(17) . . ?
C24 C25 C26 120.51(17) . . ?
N3P C11P N2P 118.46(17) . . ?
N3P C11P C12P 123.32(19) . . ?
N2P C11P C12P 118.15(18) . . ?
O12 C26 C25 114.64(17) . . ?
O12 C26 C27 124.53(17) . . ?
C25 C26 C27 120.83(17) . . ?
C9 C7 C6 109.73(15) . . ?
C9 C7 C29 114.92(17) . . ?
C6 C7 C29 111.25(16) . . ?
C9 C7 H17 106.8 . . ?
C6 C7 H17 106.8 . . ?
C29 C7 H17 106.8 . . ?
C2 C28 C27 112.99(15) . . ?
C2 C28 C38 110.68(15) . . ?
C27 C28 C38 114.51(16) . . ?
C2 C28 H28 106.0 . . ?
C27 C28 H28 106.0 . . ?
C38 C28 H28 106.0 . . ?
O5 C11 C12 122.59(18) . . ?
O5 C11 C10 117.43(18) . . ?
C12 C11 C10 119.95(19) . . ?
C36 C35 C21 112.80(16) . . ?
C36 C35 H35A 109.0 . . ?
C21 C35 H35A 109.0 . . ?
C36 C35 H35B 109.0 . . ?
C21 C35 H35B 109.0 . . ?
H35A C35 H35B 107.8 . . ?
O4 C10 C11 115.41(18) . . ?
O4 C10 C9 123.74(18) . . ?
C11 C10 C9 120.83(18) . . ?
N3P C15P C14P 123.40(19) . . ?
N3P C15P H15P 118.3 . . ?
C14P C15P H15P 118.3 . . ?
C13P C12P C11P 118.14(19) . . ?
C13P C12P H12P 120.9 . . ?
C11P C12P H12P 120.9 . . ?
C7 C29 C30 110.76(19) . . ?
C7 C29 H29A 109.5 . . ?
C30 C29 H29A 109.5 . . ?
C7 C29 H29B 109.5 . . ?
C30 C29 H29B 109.5 . . ?
H29A C29 H29B 108.1 . . ?
N1P C2P C3P 116.49(19) . . ?
N1P C2P C1P 123.4(2) . . ?
C3P C2P C1P 120.05(19) . . ?
C12P C13P C14P 119.59(19) . . ?
C12P C13P H13P 120.2 . . ?
C14P C13P H13P 120.2 . . ?
C40 C39 C38 120.0(2) . . ?
C40 C39 H39A 107.3 . . ?
C38 C39 H39A 107.3 . . ?
C40 C39 H39B 107.3 . . ?
C38 C39 H39B 107.3 . . ?
H39A C39 H39B 106.9 . . ?
C37 C36 C35 112.69(17) . . ?
C37 C36 H36A 109.1 . . ?
C35 C36 H36A 109.1 . . ?
C37 C36 H36B 109.1 . . ?
C35 C36 H36B 109.1 . . ?
H36A C36 H36B 107.8 . . ?
C15P C14P C13P 118.30(19) . . ?
C15P C14P H14P 120.9 . . ?
C13P C14P H14P 120.9 . . ?
C4P C3P C8P 118.2(2) . . ?
C4P C3P C2P 122.69(19) . . ?
C8P C3P C2P 119.1(2) . . ?
O15 C37 C36 112.90(17) . . ?
O15 C37 H37A 109.0 . . ?
C36 C37 H37A 109.0 . . ?
O15 C37 H37B 109.0 . . ?
C36 C37 H37B 109.0 . . ?
H37A C37 H37B 107.8 . . ?
C34 C33 C32 115.48(19) . . ?
C34 C33 H33A 108.4 . . ?
C32 C33 H33A 108.4 . . ?
C34 C33 H33B 108.4 . . ?
C32 C33 H33B 108.4 . . ?
H33A C33 H33B 107.5 . . ?
C7P C8P C3P 119.7(2) . . ?
C7P C8P C9P 121.9(2) . . ?
C3P C8P C9P 118.5(2) . . ?
C5P C4P C3P 121.1(2) . . ?
C5P C4P H4P 119.4 . . ?
C3P C4P H4P 119.4 . . ?
O1P C1P C10P 121.5(2) . . ?
O1P C1P C2P 121.1(2) . . ?
C10P C1P C2P 117.3(2) . . ?
C4P C5P C6P 120.0(3) . . ?
C4P C5P H5P 120.0 . . ?
C6P C5P H5P 120.0 . . ?
O14 C34 C33 112.9(2) . . ?
O14 C34 H34A 109.0 . . ?
C33 C34 H34A 109.0 . . ?
O14 C34 H34B 109.0 . . ?
C33 C34 H34B 109.0 . . ?
H34A C34 H34B 107.8 . . ?
C31 C30 C29 114.3(2) . . ?
C31 C30 H30A 108.7 . . ?
C29 C30 H30A 108.7 . . ?
C31 C30 H30B 108.7 . . ?
C29 C30 H30B 108.7 . . ?
H30A C30 H30B 107.6 . . ?
C7P C6P C5P 119.8(2) . . ?
C7P C6P H6P 120.1 . . ?
C5P C6P H6P 120.1 . . ?
C6P C7P C8P 121.0(2) . . ?
C6P C7P H7P 119.5 . . ?
C8P C7P H7P 119.5 . . ?
C9P C10P C1P 121.1(2) . . ?
C9P C10P H10P 119.5 . . ?
C1P C10P H10P 119.5 . . ?
C10P C9P C8P 124.0(2) . . ?
C10P C9P H9P 118.0 . . ?
C8P C9P H9P 118.0 . . ?
O13 C31 C30 109.3(2) . . ?
O13 C31 H31A 109.8 . . ?
C30 C31 H31A 109.8 . . ?
O13 C31 H31B 109.8 . . ?
C30 C31 H31B 109.8 . . ?
H31A C31 H31B 108.3 . . ?
C1E O1E H3F1 100.4 . . ?
H1E O1E H3F1 137.5 . . ?
C40A O16A H16B 109.5 . . ?
C40A O16A H16C 89.3 . . ?
H16B O16A H16C 78.2 . . ?
O1E C1E C2E 100.9(3) . . ?
O1E C1E H1E1 111.6 . . ?
C2E C1E H1E1 111.6 . . ?
O1E C1E H1E2 111.6 . . ?
C2E C1E H1E2 111.6 . . ?
H1E1 C1E H1E2 109.4 . . ?
O1E C1E H3E1 113.5 . . ?
C2E C1E H3E1 143.2 . . ?
H1E1 C1E H3E1 44.2 . . ?
H1E2 C1E H3E1 68.2 . . ?
O1E C1E H3E2 128.3 . . ?
C2E C1E H3E2 89.2 . . ?
H1E1 C1E H3E2 111.0 . . ?
H1E2 C1E H3E2 24.5 . . ?
H3E1 C1E H3E2 79.8 . . ?
C1E C2E H2E1 109.5 . . ?
C1E C2E H2E2 109.5 . . ?
H2E1 C2E H2E2 109.5 . . ?
C1E C2E H2E3 109.5 . . ?
H2E1 C2E H2E3 109.5 . . ?
H2E2 C2E H2E3 109.5 . . ?
C1E C2E H1E' 144.0 . . ?
H2E1 C2E H1E' 47.0 . . ?
H2E2 C2E H1E' 104.9 . . ?
H2E3 C2E H1E' 67.4 . . ?
O16 C40 C39 109.7(3) . . ?
O16 C40 H40A 109.7 . . ?
C39 C40 H40A 109.7 . . ?
O16 C40 H40B 109.7 . . ?
C39 C40 H40B 109.7 . . ?
H40A C40 H40B 108.2 . . ?
O16A C40A H40C 108.4 . . ?
O16A C40A H40D 108.4 . . ?
H40C C40A H40D 107.4 . . ?
C2E' O1E' H1E' 109.6 . . ?
C2E' O1E' H1F' 108.7 . . ?
H1E' O1E' H1F' 87.7 . . ?
H3F1 C3F H3F2 109.6 . . ?
H3F1 C3F H3F3 109.3 . . ?
H3F2 C3F H3F3 109.8 . . ?
H14A O14A H1F' 41.2 . . ?
C2E' C3E' H3E1 109.6 . . ?
C2E' C3E' H3E2 109.1 . . ?
H3E1 C3E' H3E2 110.5 . . ?
C2E' C3E' H3E3 109.3 . . ?
H3E1 C3E' H3E3 109.2 . . ?
H3E2 C3E' H3E3 109.1 . . ?
C3E' C2E' O1E' 117.0(12) . . ?
C3E' C2E' H2E4 108.0 . . ?
O1E' C2E' H2E4 108.0 . . ?
C3E' C2E' H2E5 108.0 . . ?
O1E' C2E' H2E5 108.0 . . ?
H2E4 C2E' H2E5 107.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C11P N2P N1P C2P 168.68(18) . . . . ?
C19 C20 C15 C16 1.4(3) . . . . ?
C21 C20 C15 C16 -177.80(17) . . . . ?
O1 C3 C2 C1 -178.19(16) . . . . ?
C4 C3 C2 C1 3.1(3) . . . . ?
O1 C3 C2 C28 3.0(3) . . . . ?
C4 C3 C2 C28 -175.72(17) . . . . ?
C3 C2 C1 C6 -1.9(3) . . . . ?
C28 C2 C1 C6 176.89(17) . . . . ?
C12 C13 C8 C9 -0.7(3) . . . . ?
C14 C13 C8 C9 177.56(17) . . . . ?
C13 C8 C9 C10 -0.3(3) . . . . ?
C13 C8 C9 C7 -178.84(17) . . . . ?
C15 C20 C19 O9 -178.29(17) . . . . ?
C21 C20 C19 O9 0.9(3) . . . . ?
C15 C20 C19 C18 0.7(3) . . . . ?
C21 C20 C19 C18 179.81(17) . . . . ?
O1 C3 C4 O2 1.4(3) . . . . ?
C2 C3 C4 O2 -179.89(17) . . . . ?
O1 C3 C4 C5 179.68(17) . . . . ?
C2 C3 C4 C5 -1.6(3) . . . . ?
C15 C20 C21 C23 -78.5(2) . . . . ?
C19 C20 C21 C23 102.4(2) . . . . ?
C15 C20 C21 C35 48.2(2) . . . . ?
C19 C20 C21 C35 -130.88(19) . . . . ?
C2 C1 C6 C5 -0.8(3) . . . . ?
C2 C1 C6 C7 176.75(17) . . . . ?
C23 C22 C27 C26 0.8(3) . . . . ?
C23 C22 C27 C28 -179.39(17) . . . . ?
O7 C17 C16 C15 -178.38(17) . . . . ?
C18 C17 C16 C15 2.0(3) . . . . ?
O7 C17 C16 C14 4.7(3) . . . . ?
C18 C17 C16 C14 -174.86(18) . . . . ?
C20 C15 C16 C17 -2.7(3) . . . . ?
C20 C15 C16 C14 174.17(17) . . . . ?
C8 C13 C14 C16 -98.1(2) . . . . ?
C12 C13 C14 C16 80.1(2) . . . . ?
C8 C13 C14 C32 28.7(2) . . . . ?
C12 C13 C14 C32 -153.13(17) . . . . ?
C17 C16 C14 C13 -102.4(2) . . . . ?
C15 C16 C14 C13 80.8(2) . . . . ?
C17 C16 C14 C32 128.93(19) . . . . ?
C15 C16 C14 C32 -47.8(2) . . . . ?
C27 C22 C23 C24 -0.4(3) . . . . ?
C27 C22 C23 C21 -176.77(17) . . . . ?
C20 C21 C23 C22 94.1(2) . . . . ?
C35 C21 C23 C22 -31.1(2) . . . . ?
C20 C21 C23 C24 -82.3(2) . . . . ?
C35 C21 C23 C24 152.53(17) . . . . ?
O7 C17 C18 O8 -1.0(3) . . . . ?
C16 C17 C18 O8 178.58(19) . . . . ?
O7 C17 C18 C19 -179.71(18) . . . . ?
C16 C17 C18 C19 -0.1(3) . . . . ?
O9 C19 C18 O8 -0.9(3) . . . . ?
C20 C19 C18 O8 -179.86(19) . . . . ?
O9 C19 C18 C17 177.70(18) . . . . ?
C20 C19 C18 C17 -1.3(3) . . . . ?
C8 C13 C12 O6 -178.39(17) . . . . ?
C14 C13 C12 O6 3.3(3) . . . . ?
C8 C13 C12 C11 -0.3(3) . . . . ?
C14 C13 C12 C11 -178.61(17) . . . . ?
O2 C4 C5 O3 -0.6(3) . . . . ?
C3 C4 C5 O3 -178.96(17) . . . . ?
O2 C4 C5 C6 177.22(17) . . . . ?
C3 C4 C5 C6 -1.1(3) . . . . ?
C1 C6 C5 O3 -179.86(17) . . . . ?
C7 C6 C5 O3 2.6(3) . . . . ?
C1 C6 C5 C4 2.3(3) . . . . ?
C7 C6 C5 C4 -175.22(17) . . . . ?
C22 C23 C24 O10 -178.89(17) . . . . ?
C21 C23 C24 O10 -2.4(3) . . . . ?
C22 C23 C24 C25 -0.1(3) . . . . ?
C21 C23 C24 C25 176.40(17) . . . . ?
C13 C14 C32 C33 173.33(17) . . . . ?
C16 C14 C32 C33 -59.9(2) . . . . ?
O10 C24 C25 O11 -0.1(3) . . . . ?
C23 C24 C25 O11 -178.89(17) . . . . ?
O10 C24 C25 C26 178.98(17) . . . . ?
C23 C24 C25 C26 0.2(3) . . . . ?
C15P N3P C11P N2P -174.88(18) . . . . ?
C15P N3P C11P C12P 2.1(3) . . . . ?
N1P N2P C11P N3P 8.3(3) . . . . ?
N1P N2P C11P C12P -168.77(18) . . . . ?
O11 C25 C26 O12 -0.7(3) . . . . ?
C24 C25 C26 O12 -179.67(17) . . . . ?
O11 C25 C26 C27 179.29(17) . . . . ?
C24 C25 C26 C27 0.3(3) . . . . ?
C22 C27 C26 O12 179.23(17) . . . . ?
C28 C27 C26 O12 -0.6(3) . . . . ?
C22 C27 C26 C25 -0.7(3) . . . . ?
C28 C27 C26 C25 179.44(17) . . . . ?
C8 C9 C7 C6 97.7(2) . . . . ?
C10 C9 C7 C6 -80.8(2) . . . . ?
C8 C9 C7 C29 -28.6(3) . . . . ?
C10 C9 C7 C29 152.92(18) . . . . ?
C5 C6 C7 C9 101.5(2) . . . . ?
C1 C6 C7 C9 -76.0(2) . . . . ?
C5 C6 C7 C29 -130.2(2) . . . . ?
C1 C6 C7 C29 52.4(2) . . . . ?
C1 C2 C28 C27 81.2(2) . . . . ?
C3 C2 C28 C27 -100.0(2) . . . . ?
C1 C2 C28 C38 -48.7(2) . . . . ?
C3 C2 C28 C38 130.02(18) . . . . ?
C22 C27 C28 C2 -95.3(2) . . . . ?
C26 C27 C28 C2 84.5(2) . . . . ?
C22 C27 C28 C38 32.6(2) . . . . ?
C26 C27 C28 C38 -147.55(18) . . . . ?
C39 C38 C28 C2 -166.08(16) . . . . ?
C39 C38 C28 C27 64.8(2) . . . . ?
O6 C12 C11 O5 -1.4(3) . . . . ?
C13 C12 C11 O5 -179.65(19) . . . . ?
O6 C12 C11 C10 -179.45(18) . . . . ?
C13 C12 C11 C10 2.3(3) . . . . ?
C23 C21 C35 C36 -178.37(16) . . . . ?
C20 C21 C35 C36 57.2(2) . . . . ?
O5 C11 C10 O4 -0.1(3) . . . . ?
C12 C11 C10 O4 178.01(18) . . . . ?
O5 C11 C10 C9 178.51(18) . . . . ?
C12 C11 C10 C9 -3.3(3) . . . . ?
C8 C9 C10 O4 -179.14(18) . . . . ?
C7 C9 C10 O4 -0.6(3) . . . . ?
C8 C9 C10 C11 2.3(3) . . . . ?
C7 C9 C10 C11 -179.09(18) . . . . ?
C11P N3P C15P C14P 0.8(3) . . . . ?
N3P C11P C12P C13P -2.8(3) . . . . ?
N2P C11P C12P C13P 174.16(18) . . . . ?
C9 C7 C29 C30 -162.75(17) . . . . ?
C6 C7 C29 C30 71.8(2) . . . . ?
N2P N1P C2P C3P -174.95(17) . . . . ?
N2P N1P C2P C1P 3.1(3) . . . . ?
C11P C12P C13P C14P 0.7(3) . . . . ?
C28 C38 C39 C40 159.6(3) . . . . ?
C21 C35 C36 C37 176.49(17) . . . . ?
N3P C15P C14P C13P -2.7(3) . . . . ?
C12P C13P C14P C15P 1.9(3) . . . . ?
N1P C2P C3P C4P 2.4(3) . . . . ?
C1P C2P C3P C4P -175.66(19) . . . . ?
N1P C2P C3P C8P -179.81(18) . . . . ?
C1P C2P C3P C8P 2.1(3) . . . . ?
C35 C36 C37 O15 50.6(2) . . . . ?
C14 C32 C33 C34 -177.14(19) . . . . ?
C4P C3P C8P C7P -3.3(3) . . . . ?
C2P C3P C8P C7P 178.80(19) . . . . ?
C4P C3P C8P C9P 176.29(19) . . . . ?
C2P C3P C8P C9P -1.6(3) . . . . ?
C8P C3P C4P C5P 3.4(3) . . . . ?
C2P C3P C4P C5P -178.8(2) . . . . ?
N1P C2P C1P O1P -0.6(3) . . . . ?
C3P C2P C1P O1P 177.4(2) . . . . ?
N1P C2P C1P C10P 179.7(2) . . . . ?
C3P C2P C1P C10P -2.3(3) . . . . ?
C3P C4P C5P C6P -1.2(3) . . . . ?
C32 C33 C34 O14 -57.8(3) . . . . ?
C7 C29 C30 C31 -163.16(19) . . . . ?
C4P C5P C6P C7P -1.2(4) . . . . ?
C5P C6P C7P C8P 1.2(4) . . . . ?
C3P C8P C7P C6P 1.1(3) . . . . ?
C9P C8P C7P C6P -178.5(2) . . . . ?
O1P C1P C10P C9P -177.6(2) . . . . ?
C2P C1P C10P C9P 2.1(3) . . . . ?
C1P C10P C9P C8P -1.7(4) . . . . ?
C7P C8P C9P C10P -179.0(2) . . . . ?
C3P C8P C9P C10P 1.4(3) . . . . ?
C29 C30 C31 O13 77.7(3) . . . . ?
C38 C39 C40 O16 -60.6(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        32.07
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.803
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.072

_database_code_depnum_ccdc_archive 'CCDC 1002509'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2cp82a2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            
'C-propylpyrogallol[4]arene with 1-(2-pyridylazo)-2-napthol'
_chemical_formula_moiety         
'C40 H48 O12, C15 H11 O1 N3, C2 H3 N1, 2(H2 O1)'
_chemical_formula_sum            'C57 H66 N4 O15'
_chemical_melting_point          ?

_exptl_crystal_description       plate
_exptl_crystal_colour            orange

_diffrn_ambient_temperature      173(2)
_chemical_formula_weight         1047.14

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'
O O 0.0106 0.0060 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_int_tables_number      14
_chemical_absolute_configuration ?

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                   18.733(2)
_cell_length_b                   12.8486(13)
_cell_length_c                   22.432(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.8730(10)
_cell_angle_gamma                90.00
_cell_volume                     5166.7(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9937
_cell_measurement_theta_min      2.3
_cell_measurement_theta_max      24.9
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2224
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_process_details   
;
 Data were corrected for decay and absorption using the program SADABS 
 (Sheldrick, G. M. (2003). SADABS. Version 2.10. University of
 Göttingen, Germany).
;

_exptl_special_details           
; 
 ? 
;
_diffrn_radiation_probe          ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.0
_diffrn_reflns_number            42953
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_av_sigmaI/netI    0.0640
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.85
_diffrn_reflns_theta_max         27.39
_reflns_number_total             11637
_reflns_number_gt                6500
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2008)'
_computing_structure_solution    'SHELXS-1997 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-1997 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-SEED, Barbour, 2001'
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. There is minor residual electron
 density near a probe that is minor hydrogen disorder that is not included.
 There are two oxygen atoms that are water molecules that don't have hydrogens
 modeled, but the hydrogens are included in the sum formula. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0721P)²+6.7547P] where P=(Fo²+2Fc²)/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         11637
_refine_ls_number_parameters     700
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1318
_refine_ls_R_factor_gt           0.0599
_refine_ls_wR_factor_ref         0.1890
_refine_ls_wR_factor_gt          0.1468
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_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
O7 O 0.30586(12) 0.29914(15) 0.43949(9) 0.0276(5) Uani 1 1 d . . .
H7 H 0.3335 0.3002 0.4170 0.033 Uiso 1 1 calc R . .
O4 O 0.41229(11) 0.26316(17) 0.77267(8) 0.0274(5) Uani 1 1 d . . .
H4 H 0.4554 0.2732 0.7724 0.033 Uiso 1 1 calc R . .
O3 O 0.39527(12) 0.13404(16) 0.86811(8) 0.0248(5) Uani 1 1 d . . .
H3 H 0.4063 0.1826 0.8487 0.030 Uiso 1 1 calc R . .
O9 O 0.30616(12) -0.06596(16) 0.38879(9) 0.0302(5) Uani 1 1 d . . .
H9 H 0.2685 -0.0859 0.3609 0.036 Uiso 1 1 d . . .
O12 O 0.43302(11) -0.24112(17) 0.70380(9) 0.0304(5) Uani 1 1 d . . .
H12 H 0.4155 -0.2410 0.7333 0.037 Uiso 1 1 calc R . .
O1 O 0.39015(13) -0.22964(16) 0.82322(10) 0.0345(5) Uani 1 1 d . . .
H1 H 0.4240 -0.2274 0.8559 0.041 Uiso 1 1 calc R . .
O5 O 0.46005(11) 0.34699(18) 0.67808(9) 0.0312(5) Uani 1 1 d . . .
H5 H 0.4660 0.3742 0.6468 0.037 Uiso 1 1 calc R . .
O8 O 0.34754(12) 0.14709(17) 0.37431(9) 0.0305(5) Uani 1 1 d . . .
H8 H 0.3330 0.1151 0.3413 0.037 Uiso 1 1 d . . .
O10 O 0.38089(14) -0.1769(2) 0.49102(10) 0.0414(6) Uani 1 1 d . . .
H10 H 0.3489 -0.1583 0.4594 0.050 Uiso 1 1 calc R . .
O6 O 0.37265(12) 0.35136(17) 0.56094(9) 0.0308(5) Uani 1 1 d . . .
H6 H 0.3459 0.3395 0.5256 0.037 Uiso 1 1 calc R . .
O2 O 0.44934(13) -0.06719(18) 0.89731(10) 0.0377(6) Uani 1 1 d . . .
H2 H 0.4720 -0.0136 0.9108 0.045 Uiso 1 1 calc R . .
O11 O 0.47524(12) -0.2231(2) 0.60131(11) 0.0402(6) Uani 1 1 d . . .
H11 H 0.4797 -0.2794 0.5855 0.048 Uiso 1 1 calc R . .
N1 N 0.32909(15) 0.5062(2) 0.75033(12) 0.0300(6) Uani 1 1 d . . .
O13 O 0.35380(15) 0.54881(18) 0.63259(10) 0.0408(6) Uani 1 1 d . . .
C4 C 0.30805(15) 0.0700(2) 0.77236(12) 0.0198(6) Uani 1 1 d . . .
C12 C 0.24780(16) 0.2251(2) 0.63967(12) 0.0203(6) Uani 1 1 d . . .
H13 H 0.1999 0.1978 0.6316 0.024 Uiso 1 1 calc R . .
C16 C 0.30582(16) 0.1175(2) 0.41308(12) 0.0233(6) Uani 1 1 d . . .
C21 C 0.22369(17) -0.1195(2) 0.47415(13) 0.0250(6) Uani 1 1 d . . .
H21 H 0.2327 -0.1625 0.4410 0.030 Uiso 1 1 calc R . .
C29 C 0.18638(16) 0.1675(2) 0.74200(13) 0.0245(6) Uani 1 1 d . . .
H29A H 0.1636 0.2335 0.7259 0.029 Uiso 1 1 calc R . .
H29B H 0.1671 0.1149 0.7104 0.029 Uiso 1 1 calc R . .
C8 C 0.36578(16) 0.2643(2) 0.71240(12) 0.0215(6) Uani 1 1 d . . .
C14 C 0.21908(16) 0.2657(2) 0.52323(12) 0.0217(6) Uani 1 1 d . . .
H14 H 0.2274 0.3313 0.5040 0.026 Uiso 1 1 calc R . .
C3 C 0.36534(16) 0.0538(2) 0.82741(12) 0.0208(6) Uani 1 1 d . . .
C13 C 0.29459(16) 0.2228(2) 0.70059(12) 0.0197(6) Uani 1 1 d . . .
C24 C 0.37833(17) -0.2142(2) 0.65011(13) 0.0254(6) Uani 1 1 d . . .
N2 N 0.39823(15) 0.5243(2) 0.75060(12) 0.0323(6) Uani 1 1 d . . .
H2A H 0.4081 0.5324 0.7158 0.039 Uiso 1 1 calc R . .
C32 C 0.13604(16) 0.2604(2) 0.51809(12) 0.0254(6) Uani 1 1 d . . .
H32A H 0.1243 0.1911 0.5297 0.030 Uiso 1 1 calc R . .
H32B H 0.1254 0.3092 0.5473 0.030 Uiso 1 1 calc R . .
C9 C 0.38907(16) 0.3066(2) 0.66445(13) 0.0230(6) Uani 1 1 d . . .
C18 C 0.24442(16) -0.0075(2) 0.46247(12) 0.0225(6) Uani 1 1 d . . .
C28 C 0.27984(16) -0.2077(2) 0.70640(13) 0.0239(6) Uani 1 1 d . . .
H28 H 0.3036 -0.2707 0.7278 0.029 Uiso 1 1 calc R . .
C1 C 0.36437(16) -0.1300(2) 0.80609(13) 0.0241(6) Uani 1 1 d . . .
C6 C 0.31025(16) -0.1166(2) 0.74961(12) 0.0223(6) Uani 1 1 d . . .
C10 C 0.34176(17) 0.3068(2) 0.60372(13) 0.0236(6) Uani 1 1 d . . .
C20 C 0.24261(16) 0.1777(2) 0.48678(12) 0.0213(6) Uani 1 1 d . . .
C27 C 0.27638(17) -0.1584(2) 0.53541(13) 0.0241(6) Uani 1 1 d . . .
C26 C 0.25490(17) -0.1682(2) 0.58997(13) 0.0235(6) Uani 1 1 d . . .
H26 H 0.2055 -0.1549 0.5880 0.028 Uiso 1 1 calc R . .
C15 C 0.28437(16) 0.1977(2) 0.44590(12) 0.0219(6) Uani 1 1 d . . .
C11 C 0.26998(16) 0.2666(2) 0.59032(12) 0.0215(6) Uani 1 1 d . . .
C5 C 0.28343(16) -0.0162(2) 0.73362(12) 0.0226(6) Uani 1 1 d . . .
H15 H 0.2476 -0.0060 0.6955 0.027 Uiso 1 1 calc R . .
C7 C 0.27105(16) 0.1757(2) 0.75446(12) 0.0205(6) Uani 1 1 d . . .
H16 H 0.2897 0.2219 0.7904 0.025 Uiso 1 1 calc R . .
C19 C 0.22499(16) 0.0747(2) 0.49477(12) 0.0218(6) Uani 1 1 d . . .
H19 H 0.1988 0.0601 0.5232 0.026 Uiso 1 1 calc R . .
C52 C 0.43773(16) 0.5289(2) 0.85909(12) 0.0230(6) Uani 1 1 d . . .
H52 H 0.3885 0.5202 0.8594 0.028 Uiso 1 1 calc R . .
C51 C 0.45570(18) 0.5307(2) 0.80576(14) 0.0280(7) Uani 1 1 d . . .
C17 C 0.28527(17) 0.0155(2) 0.42065(12) 0.0232(6) Uani 1 1 d . . .
C25 C 0.30410(17) -0.1972(2) 0.64712(13) 0.0232(6) Uani 1 1 d . . .
C2 C 0.39391(16) -0.0455(2) 0.84427(12) 0.0240(6) Uani 1 1 d . . .
C35 C 0.14090(18) -0.1301(3) 0.46923(14) 0.0338(8) Uani 1 1 d . . .
H35A H 0.1307 -0.2018 0.4776 0.041 Uiso 1 1 calc R . .
H35B H 0.1299 -0.0871 0.5010 0.041 Uiso 1 1 calc R . .
C22 C 0.35045(18) -0.1804(2) 0.54020(13) 0.0282(7) Uani 1 1 d . . .
C38 C 0.19603(17) -0.2208(2) 0.69508(13) 0.0282(7) Uani 1 1 d . . .
H38A H 0.1707 -0.1586 0.6750 0.034 Uiso 1 1 calc R . .
H38B H 0.1787 -0.2790 0.6671 0.034 Uiso 1 1 calc R . .
N3 N 0.52837(19) 0.5416(3) 0.80313(16) 0.0522(8) Uani 1 1 d . . .
C23 C 0.40155(18) -0.2064(2) 0.59680(14) 0.0295(7) Uani 1 1 d . . .
C49 C 0.19997(19) 0.4825(2) 0.69788(15) 0.0338(8) Uani 1 1 d . . .
C50 C 0.27583(19) 0.5069(2) 0.69610(14) 0.0319(7) Uani 1 1 d . . .
C44 C 0.1410(2) 0.4854(3) 0.64151(16) 0.0399(8) Uani 1 1 d . . .
C33 C 0.08642(18) 0.2851(3) 0.45310(14) 0.0385(8) Uani 1 1 d . . .
H33A H 0.0966 0.3555 0.4422 0.046 Uiso 1 1 calc R . .
H33B H 0.0986 0.2382 0.4236 0.046 Uiso 1 1 calc R . .
C30 C 0.16463(18) 0.1396(3) 0.80029(14) 0.0349(8) Uani 1 1 d . . .
H30A H 0.1906 0.0766 0.8183 0.042 Uiso 1 1 calc R . .
H30B H 0.1804 0.1950 0.8306 0.042 Uiso 1 1 calc R . .
C55 C 0.58439(19) 0.5522(3) 0.85929(16) 0.0356(8) Uani 1 1 d . . .
H55 H 0.6339 0.5587 0.8594 0.043 Uiso 1 1 calc R . .
C39 C 0.17545(19) -0.2396(3) 0.75511(15) 0.0385(8) Uani 1 1 d . . .
H39A H 0.2018 -0.3006 0.7759 0.046 Uiso 1 1 calc R . .
H39B H 0.1913 -0.1805 0.7827 0.046 Uiso 1 1 calc R . .
C42 C 0.2256(2) 0.5395(3) 0.58251(16) 0.0437(9) Uani 1 1 d . . .
H42 H 0.2324 0.5602 0.5448 0.052 Uiso 1 1 calc R . .
C41 C 0.2889(2) 0.5322(3) 0.63635(15) 0.0364(8) Uani 1 1 d . . .
C48 C 0.1836(2) 0.4553(3) 0.75290(16) 0.0397(8) Uani 1 1 d . . .
H48 H 0.2216 0.4537 0.7903 0.048 Uiso 1 1 calc R . .
C53 C 0.4928(2) 0.5402(3) 0.91219(16) 0.0444(9) Uani 1 1 d . . .
H53 H 0.4805 0.5393 0.9495 0.053 Uiso 1 1 calc R . .
C54 C 0.5667(2) 0.5530(3) 0.91475(16) 0.0397(8) Uani 1 1 d . . .
H54 H 0.6033 0.5618 0.9526 0.048 Uiso 1 1 calc R . .
C40 C 0.0927(2) -0.2555(4) 0.74310(17) 0.0563(11) Uani 1 1 d . . .
H40A H 0.0663 -0.1979 0.7194 0.084 Uiso 1 1 calc R . .
H40B H 0.0814 -0.2599 0.7821 0.084 Uiso 1 1 calc R . .
H40C H 0.0779 -0.3188 0.7201 0.084 Uiso 1 1 calc R . .
C45 C 0.0690(2) 0.4592(3) 0.64255(19) 0.0485(10) Uani 1 1 d . . .
H45 H 0.0301 0.4610 0.6057 0.058 Uiso 1 1 calc R . .
C43 C 0.1568(2) 0.5172(3) 0.58512(17) 0.0466(10) Uani 1 1 d . . .
H43 H 0.1173 0.5225 0.5488 0.056 Uiso 1 1 calc R . .
C34 C 0.0043(2) 0.2753(4) 0.44746(18) 0.0598(12) Uani 1 1 d . . .
H34A H -0.0070 0.2042 0.4542 0.090 Uiso 1 1 calc R . .
H34B H -0.0245 0.2966 0.4066 0.090 Uiso 1 1 calc R . .
H34C H -0.0076 0.3187 0.4780 0.090 Uiso 1 1 calc R . .
C31 C 0.0821(2) 0.1230(4) 0.78713(17) 0.0524(11) Uani 1 1 d . . .
H31A H 0.0560 0.1846 0.7685 0.079 Uiso 1 1 calc R . .
H31B H 0.0707 0.1085 0.8254 0.079 Uiso 1 1 calc R . .
H31C H 0.0667 0.0654 0.7591 0.079 Uiso 1 1 calc R . .
C47 C 0.1119(2) 0.4309(3) 0.75224(18) 0.0456(9) Uani 1 1 d . . .
H47 H 0.1018 0.4142 0.7893 0.055 Uiso 1 1 calc R . .
C46 C 0.0546(2) 0.4308(3) 0.6969(2) 0.0512(10) Uani 1 1 d . . .
H46 H 0.0067 0.4117 0.6966 0.061 Uiso 1 1 calc R . .
C36 C 0.0892(2) -0.0987(4) 0.40574(17) 0.0566(12) Uani 1 1 d . . .
H36A H 0.0982 -0.0264 0.3978 0.068 Uiso 1 1 calc R . .
H36B H 0.1007 -0.1406 0.3737 0.068 Uiso 1 1 calc R . .
C37 C 0.0073(3) -0.1126(6) 0.4016(2) 0.099(2) Uani 1 1 d . . .
H37A H -0.0028 -0.1850 0.4063 0.148 Uiso 1 1 calc R . .
H37B H -0.0231 -0.0884 0.3618 0.148 Uiso 1 1 calc R . .
H37C H -0.0041 -0.0733 0.4341 0.148 Uiso 1 1 calc R . .
O14 O 0.44610(15) 0.9331(2) 0.05011(14) 0.0607(8) Uani 1 1 d . . .
C57 C 0.1877(3) 0.5917(4) 0.41903(18) 0.0551(11) Uani 1 1 d . . .
C56 C 0.2660(3) 0.5903(4) 0.4235(2) 0.0730(14) Uani 1 1 d . . .
H56A H 0.2935 0.6257 0.4608 0.109 Uiso 1 1 calc R . .
H56B H 0.2738 0.6247 0.3880 0.109 Uiso 1 1 calc R . .
H56C H 0.2829 0.5195 0.4249 0.109 Uiso 1 1 calc R . .
N4 N 0.1271(3) 0.5931(4) 0.4170(2) 0.0878(14) Uani 1 1 d . . .
O15 O 0.5100(4) -0.2607(5) 0.4813(4) 0.207(3) Uani 1 1 d . . .


_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
O7 C15 1.384(3) . ?
O7 H7 0.8200 . ?
O4 C8 1.380(3) . ?
O4 H4 0.8200 . ?
O3 C3 1.383(3) . ?
O3 H3 0.8200 . ?
O9 C17 1.386(3) . ?
O9 H9 0.8355 . ?
O12 C24 1.380(3) . ?
O12 H12 0.8200 . ?
O1 C1 1.382(3) . ?
O1 H1 0.8200 . ?
O5 C9 1.377(3) . ?
O5 H5 0.8200 . ?
O8 C16 1.381(3) . ?
O8 H8 0.8222 . ?
O10 C22 1.382(3) . ?
O10 H10 0.8200 . ?
O6 C10 1.381(3) . ?
O6 H6 0.8200 . ?
O2 C2 1.362(3) . ?
O2 H2 0.8200 . ?
O11 C23 1.371(4) . ?
O11 H11 0.8200 . ?
N1 N2 1.314(4) . ?
N1 C50 1.331(4) . ?
O13 C41 1.260(4) . ?
C4 C3 1.397(4) . ?
C4 C5 1.401(4) . ?
C4 C7 1.525(4) . ?
C12 C13 1.393(4) . ?
C12 C11 1.396(4) . ?
C12 H13 0.9300 . ?
C16 C17 1.390(4) . ?
C16 C15 1.392(4) . ?
C21 C27 1.525(4) . ?
C21 C35 1.529(4) . ?
C21 C18 1.533(4) . ?
C21 H21 0.9800 . ?
C29 C30 1.521(4) . ?
C29 C7 1.532(4) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C8 C9 1.384(4) . ?
C8 C13 1.388(4) . ?
C14 C32 1.527(4) . ?
C14 C11 1.530(4) . ?
C14 C20 1.532(4) . ?
C14 H14 0.9800 . ?
C3 C2 1.393(4) . ?
C13 C7 1.526(4) . ?
C24 C23 1.390(4) . ?
C24 C25 1.390(4) . ?
N2 C51 1.387(4) . ?
N2 H2A 0.8600 . ?
C32 C33 1.518(4) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C9 C10 1.393(4) . ?
C18 C19 1.388(4) . ?
C18 C17 1.403(4) . ?
C28 C6 1.521(4) . ?
C28 C38 1.525(4) . ?
C28 C25 1.531(4) . ?
C28 H28 0.9800 . ?
C1 C6 1.385(4) . ?
C1 C2 1.395(4) . ?
C6 C5 1.393(4) . ?
C10 C11 1.390(4) . ?
C20 C19 1.388(4) . ?
C20 C15 1.391(4) . ?
C27 C22 1.390(4) . ?
C27 C26 1.401(4) . ?
C26 C25 1.395(4) . ?
C26 H26 0.9300 . ?
C5 H15 0.9300 . ?
C7 H16 0.9800 . ?
C19 H19 0.9300 . ?
C52 C51 1.334(4) . ?
C52 C53 1.338(4) . ?
C52 H52 0.9300 . ?
C51 N3 1.387(4) . ?
C35 C36 1.526(5) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C22 C23 1.391(4) . ?
C38 C39 1.524(4) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
N3 C55 1.393(5) . ?
C49 C48 1.400(5) . ?
C49 C44 1.418(5) . ?
C49 C50 1.467(5) . ?
C50 C41 1.467(5) . ?
C44 C45 1.395(5) . ?
C44 C43 1.440(5) . ?
C33 C34 1.511(5) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C30 C31 1.503(5) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C55 C54 1.377(5) . ?
C55 H55 0.9300 . ?
C39 C40 1.508(5) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C42 C43 1.338(5) . ?
C42 C41 1.430(5) . ?
C42 H42 0.9300 . ?
C48 C47 1.374(5) . ?
C48 H48 0.9300 . ?
C53 C54 1.379(5) . ?
C53 H53 0.9300 . ?
C54 H54 0.9300 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C45 C46 1.372(6) . ?
C45 H45 0.9300 . ?
C43 H43 0.9300 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C47 C46 1.386(5) . ?
C47 H47 0.9300 . ?
C46 H46 0.9300 . ?
C36 C37 1.522(6) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C57 N4 1.122(6) . ?
C57 C56 1.442(7) . ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 0.9600 . ?

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
C15 O7 H7 109.5 . . ?
C8 O4 H4 109.5 . . ?
C3 O3 H3 109.5 . . ?
C17 O9 H9 108.3 . . ?
C24 O12 H12 109.5 . . ?
C1 O1 H1 109.5 . . ?
C9 O5 H5 109.5 . . ?
C16 O8 H8 109.3 . . ?
C22 O10 H10 109.5 . . ?
C10 O6 H6 109.5 . . ?
C2 O2 H2 109.5 . . ?
C23 O11 H11 109.5 . . ?
N2 N1 C50 118.7(3) . . ?
C3 C4 C5 117.4(3) . . ?
C3 C4 C7 122.6(2) . . ?
C5 C4 C7 119.9(2) . . ?
C13 C12 C11 122.6(3) . . ?
C13 C12 H13 118.7 . . ?
C11 C12 H13 118.7 . . ?
O8 C16 C17 124.3(3) . . ?
O8 C16 C15 115.6(3) . . ?
C17 C16 C15 120.0(3) . . ?
C27 C21 C35 114.4(2) . . ?
C27 C21 C18 109.4(2) . . ?
C35 C21 C18 111.9(3) . . ?
C27 C21 H21 106.9 . . ?
C35 C21 H21 106.9 . . ?
C18 C21 H21 106.9 . . ?
C30 C29 C7 112.4(2) . . ?
C30 C29 H29A 109.1 . . ?
C7 C29 H29A 109.1 . . ?
C30 C29 H29B 109.1 . . ?
C7 C29 H29B 109.1 . . ?
H29A C29 H29B 107.9 . . ?
O4 C8 C9 120.9(3) . . ?
O4 C8 C13 118.8(2) . . ?
C9 C8 C13 120.3(2) . . ?
C32 C14 C11 113.9(2) . . ?
C32 C14 C20 111.8(2) . . ?
C11 C14 C20 109.7(2) . . ?
C32 C14 H14 107.0 . . ?
C11 C14 H14 107.0 . . ?
C20 C14 H14 107.0 . . ?
O3 C3 C2 116.9(2) . . ?
O3 C3 C4 122.2(3) . . ?
C2 C3 C4 120.8(3) . . ?
C8 C13 C12 118.4(2) . . ?
C8 C13 C7 118.9(2) . . ?
C12 C13 C7 122.7(3) . . ?
O12 C24 C23 115.5(3) . . ?
O12 C24 C25 124.1(3) . . ?
C23 C24 C25 120.4(3) . . ?
N1 N2 C51 121.6(2) . . ?
N1 N2 H2A 119.2 . . ?
C51 N2 H2A 119.2 . . ?
C33 C32 C14 112.9(2) . . ?
C33 C32 H32A 109.0 . . ?
C14 C32 H32A 109.0 . . ?
C33 C32 H32B 109.0 . . ?
C14 C32 H32B 109.0 . . ?
H32A C32 H32B 107.8 . . ?
O5 C9 C8 118.5(2) . . ?
O5 C9 C10 121.1(2) . . ?
C8 C9 C10 120.4(3) . . ?
C19 C18 C17 117.7(3) . . ?
C19 C18 C21 120.5(2) . . ?
C17 C18 C21 121.8(3) . . ?
C6 C28 C38 111.6(2) . . ?
C6 C28 C25 109.6(2) . . ?
C38 C28 C25 114.6(2) . . ?
C6 C28 H28 106.9 . . ?
C38 C28 H28 106.9 . . ?
C25 C28 H28 106.9 . . ?
O1 C1 C6 118.3(3) . . ?
O1 C1 C2 120.4(3) . . ?
C6 C1 C2 121.3(3) . . ?
C1 C6 C5 117.7(3) . . ?
C1 C6 C28 121.8(3) . . ?
C5 C6 C28 120.5(2) . . ?
O6 C10 C11 125.3(3) . . ?
O6 C10 C9 113.9(3) . . ?
C11 C10 C9 120.8(2) . . ?
C19 C20 C15 117.4(3) . . ?
C19 C20 C14 121.2(2) . . ?
C15 C20 C14 121.3(3) . . ?
C22 C27 C26 116.6(3) . . ?
C22 C27 C21 120.5(2) . . ?
C26 C27 C21 122.8(3) . . ?
C25 C26 C27 123.1(3) . . ?
C25 C26 H26 118.4 . . ?
C27 C26 H26 118.4 . . ?
O7 C15 C20 118.6(2) . . ?
O7 C15 C16 120.3(2) . . ?
C20 C15 C16 121.1(3) . . ?
C10 C11 C12 117.5(2) . . ?
C10 C11 C14 120.2(2) . . ?
C12 C11 C14 122.2(3) . . ?
C6 C5 C4 122.9(3) . . ?
C6 C5 H15 118.5 . . ?
C4 C5 H15 118.5 . . ?
C4 C7 C13 110.3(2) . . ?
C4 C7 C29 110.7(2) . . ?
C13 C7 C29 113.9(2) . . ?
C4 C7 H16 107.2 . . ?
C13 C7 H16 107.2 . . ?
C29 C7 H16 107.2 . . ?
C20 C19 C18 123.4(3) . . ?
C20 C19 H19 118.3 . . ?
C18 C19 H19 118.3 . . ?
C51 C52 C53 117.8(3) . . ?
C51 C52 H52 121.1 . . ?
C53 C52 H52 121.1 . . ?
C52 C51 N3 123.1(3) . . ?
C52 C51 N2 117.8(3) . . ?
N3 C51 N2 119.0(3) . . ?
O9 C17 C16 121.3(2) . . ?
O9 C17 C18 118.4(3) . . ?
C16 C17 C18 120.3(3) . . ?
C24 C25 C26 118.1(3) . . ?
C24 C25 C28 119.3(3) . . ?
C26 C25 C28 122.6(3) . . ?
O2 C2 C3 124.1(3) . . ?
O2 C2 C1 116.3(3) . . ?
C3 C2 C1 119.6(3) . . ?
C36 C35 C21 113.6(3) . . ?
C36 C35 H35A 108.9 . . ?
C21 C35 H35A 108.9 . . ?
C36 C35 H35B 108.9 . . ?
C21 C35 H35B 108.9 . . ?
H35A C35 H35B 107.7 . . ?
O10 C22 C27 124.5(3) . . ?
O10 C22 C23 113.7(3) . . ?
C27 C22 C23 121.8(3) . . ?
C39 C38 C28 112.5(2) . . ?
C39 C38 H38A 109.1 . . ?
C28 C38 H38A 109.1 . . ?
C39 C38 H38B 109.1 . . ?
C28 C38 H38B 109.1 . . ?
H38A C38 H38B 107.8 . . ?
C51 N3 C55 117.6(3) . . ?
O11 C23 C24 119.0(3) . . ?
O11 C23 C22 121.1(3) . . ?
C24 C23 C22 119.9(3) . . ?
C48 C49 C44 118.6(3) . . ?
C48 C49 C50 122.6(3) . . ?
C44 C49 C50 118.7(3) . . ?
N1 C50 C49 116.7(3) . . ?
N1 C50 C41 123.8(3) . . ?
C49 C50 C41 119.5(3) . . ?
C45 C44 C49 119.0(3) . . ?
C45 C44 C43 121.9(3) . . ?
C49 C44 C43 119.0(4) . . ?
C34 C33 C32 112.8(3) . . ?
C34 C33 H33A 109.0 . . ?
C32 C33 H33A 109.0 . . ?
C34 C33 H33B 109.0 . . ?
C32 C33 H33B 109.0 . . ?
H33A C33 H33B 107.8 . . ?
C31 C30 C29 112.4(3) . . ?
C31 C30 H30A 109.1 . . ?
C29 C30 H30A 109.1 . . ?
C31 C30 H30B 109.1 . . ?
C29 C30 H30B 109.1 . . ?
H30A C30 H30B 107.8 . . ?
C54 C55 N3 120.1(3) . . ?
C54 C55 H55 119.9 . . ?
N3 C55 H55 119.9 . . ?
C40 C39 C38 112.0(3) . . ?
C40 C39 H39A 109.2 . . ?
C38 C39 H39A 109.2 . . ?
C40 C39 H39B 109.2 . . ?
C38 C39 H39B 109.2 . . ?
H39A C39 H39B 107.9 . . ?
C43 C42 C41 121.5(3) . . ?
C43 C42 H42 119.2 . . ?
C41 C42 H42 119.2 . . ?
O13 C41 C42 120.8(3) . . ?
O13 C41 C50 121.3(3) . . ?
C42 C41 C50 117.9(3) . . ?
C47 C48 C49 120.7(3) . . ?
C47 C48 H48 119.6 . . ?
C49 C48 H48 119.6 . . ?
C52 C53 C54 123.7(3) . . ?
C52 C53 H53 118.1 . . ?
C54 C53 H53 118.1 . . ?
C55 C54 C53 117.6(3) . . ?
C55 C54 H54 121.2 . . ?
C53 C54 H54 121.2 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C46 C45 C44 121.3(4) . . ?
C46 C45 H45 119.4 . . ?
C44 C45 H45 119.4 . . ?
C42 C43 C44 123.1(3) . . ?
C42 C43 H43 118.5 . . ?
C44 C43 H43 118.5 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C48 C47 C46 120.6(4) . . ?
C48 C47 H47 119.7 . . ?
C46 C47 H47 119.7 . . ?
C45 C46 C47 119.7(4) . . ?
C45 C46 H46 120.2 . . ?
C47 C46 H46 120.2 . . ?
C37 C36 C35 112.4(3) . . ?
C37 C36 H36A 109.1 . . ?
C35 C36 H36A 109.1 . . ?
C37 C36 H36B 109.1 . . ?
C35 C36 H36B 109.1 . . ?
H36A C36 H36B 107.8 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
N4 C57 C56 178.4(5) . . ?
C57 C56 H56A 109.5 . . ?
C57 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C57 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?

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
C5 C4 C3 O3 178.1(2) . . . . ?
C7 C4 C3 O3 -3.5(4) . . . . ?
C5 C4 C3 C2 -3.2(4) . . . . ?
C7 C4 C3 C2 175.2(3) . . . . ?
O4 C8 C13 C12 179.4(3) . . . . ?
C9 C8 C13 C12 0.0(4) . . . . ?
O4 C8 C13 C7 -1.1(4) . . . . ?
C9 C8 C13 C7 179.4(3) . . . . ?
C11 C12 C13 C8 0.5(4) . . . . ?
C11 C12 C13 C7 -178.9(3) . . . . ?
C50 N1 N2 C51 176.2(3) . . . . ?
C11 C14 C32 C33 166.4(3) . . . . ?
C20 C14 C32 C33 -68.6(3) . . . . ?
O4 C8 C9 O5 0.5(4) . . . . ?
C13 C8 C9 O5 180.0(3) . . . . ?
O4 C8 C9 C10 179.7(3) . . . . ?
C13 C8 C9 C10 -0.8(4) . . . . ?
C27 C21 C18 C19 -76.5(3) . . . . ?
C35 C21 C18 C19 51.4(3) . . . . ?
C27 C21 C18 C17 101.6(3) . . . . ?
C35 C21 C18 C17 -130.5(3) . . . . ?
O1 C1 C6 C5 178.4(3) . . . . ?
C2 C1 C6 C5 -3.3(4) . . . . ?
O1 C1 C6 C28 -0.8(4) . . . . ?
C2 C1 C6 C28 177.5(3) . . . . ?
C38 C28 C6 C1 119.6(3) . . . . ?
C25 C28 C6 C1 -112.5(3) . . . . ?
C38 C28 C6 C5 -59.6(3) . . . . ?
C25 C28 C6 C5 68.3(3) . . . . ?
O5 C9 C10 O6 -0.7(4) . . . . ?
C8 C9 C10 O6 -179.9(3) . . . . ?
O5 C9 C10 C11 -179.5(3) . . . . ?
C8 C9 C10 C11 1.3(4) . . . . ?
C32 C14 C20 C19 -51.0(3) . . . . ?
C11 C14 C20 C19 76.3(3) . . . . ?
C32 C14 C20 C15 131.0(3) . . . . ?
C11 C14 C20 C15 -101.7(3) . . . . ?
C35 C21 C27 C22 162.2(3) . . . . ?
C18 C21 C27 C22 -71.3(3) . . . . ?
C35 C21 C27 C26 -21.4(4) . . . . ?
C18 C21 C27 C26 105.1(3) . . . . ?
C22 C27 C26 C25 0.9(4) . . . . ?
C21 C27 C26 C25 -175.7(3) . . . . ?
C19 C20 C15 O7 -176.8(2) . . . . ?
C14 C20 C15 O7 1.3(4) . . . . ?
C19 C20 C15 C16 1.7(4) . . . . ?
C14 C20 C15 C16 179.8(3) . . . . ?
O8 C16 C15 O7 -1.1(4) . . . . ?
C17 C16 C15 O7 178.8(3) . . . . ?
O8 C16 C15 C20 -179.6(2) . . . . ?
C17 C16 C15 C20 0.3(4) . . . . ?
O6 C10 C11 C12 -179.5(3) . . . . ?
C9 C10 C11 C12 -0.8(4) . . . . ?
O6 C10 C11 C14 2.4(4) . . . . ?
C9 C10 C11 C14 -179.0(3) . . . . ?
C13 C12 C11 C10 0.0(4) . . . . ?
C13 C12 C11 C14 178.0(3) . . . . ?
C32 C14 C11 C10 -157.4(3) . . . . ?
C20 C14 C11 C10 76.5(3) . . . . ?
C32 C14 C11 C12 24.6(4) . . . . ?
C20 C14 C11 C12 -101.6(3) . . . . ?
C1 C6 C5 C4 -0.9(4) . . . . ?
C28 C6 C5 C4 178.3(3) . . . . ?
C3 C4 C5 C6 4.1(4) . . . . ?
C7 C4 C5 C6 -174.4(3) . . . . ?
C3 C4 C7 C13 108.2(3) . . . . ?
C5 C4 C7 C13 -73.4(3) . . . . ?
C3 C4 C7 C29 -124.8(3) . . . . ?
C5 C4 C7 C29 53.6(3) . . . . ?
C8 C13 C7 C4 -74.9(3) . . . . ?
C12 C13 C7 C4 104.5(3) . . . . ?
C8 C13 C7 C29 159.9(3) . . . . ?
C12 C13 C7 C29 -20.7(4) . . . . ?
C30 C29 C7 C4 65.6(3) . . . . ?
C30 C29 C7 C13 -169.4(3) . . . . ?
C15 C20 C19 C18 -2.5(4) . . . . ?
C14 C20 C19 C18 179.4(3) . . . . ?
C17 C18 C19 C20 1.3(4) . . . . ?
C21 C18 C19 C20 179.4(3) . . . . ?
C53 C52 C51 N3 1.3(5) . . . . ?
C53 C52 C51 N2 -176.8(3) . . . . ?
N1 N2 C51 C52 -7.0(4) . . . . ?
N1 N2 C51 N3 174.8(3) . . . . ?
O8 C16 C17 O9 0.2(4) . . . . ?
C15 C16 C17 O9 -179.7(3) . . . . ?
O8 C16 C17 C18 178.3(3) . . . . ?
C15 C16 C17 C18 -1.6(4) . . . . ?
C19 C18 C17 O9 179.0(2) . . . . ?
C21 C18 C17 O9 0.9(4) . . . . ?
C19 C18 C17 C16 0.8(4) . . . . ?
C21 C18 C17 C16 -177.3(3) . . . . ?
O12 C24 C25 C26 178.7(3) . . . . ?
C23 C24 C25 C26 -2.5(4) . . . . ?
O12 C24 C25 C28 0.4(4) . . . . ?
C23 C24 C25 C28 179.2(3) . . . . ?
C27 C26 C25 C24 1.8(4) . . . . ?
C27 C26 C25 C28 -180.0(3) . . . . ?
C6 C28 C25 C24 71.7(3) . . . . ?
C38 C28 C25 C24 -162.0(3) . . . . ?
C6 C28 C25 C26 -106.5(3) . . . . ?
C38 C28 C25 C26 19.7(4) . . . . ?
O3 C3 C2 O2 -0.8(4) . . . . ?
C4 C3 C2 O2 -179.6(3) . . . . ?
O3 C3 C2 C1 178.0(2) . . . . ?
C4 C3 C2 C1 -0.8(4) . . . . ?
O1 C1 C2 O2 1.3(4) . . . . ?
C6 C1 C2 O2 -177.0(3) . . . . ?
O1 C1 C2 C3 -177.6(3) . . . . ?
C6 C1 C2 C3 4.1(4) . . . . ?
C27 C21 C35 C36 -175.5(3) . . . . ?
C18 C21 C35 C36 59.4(4) . . . . ?
C26 C27 C22 O10 178.6(3) . . . . ?
C21 C27 C22 O10 -4.8(5) . . . . ?
C26 C27 C22 C23 -2.9(4) . . . . ?
C21 C27 C22 C23 173.8(3) . . . . ?
C6 C28 C38 C39 -59.4(3) . . . . ?
C25 C28 C38 C39 175.4(3) . . . . ?
C52 C51 N3 C55 -0.7(5) . . . . ?
N2 C51 N3 C55 177.4(3) . . . . ?
O12 C24 C23 O11 -1.4(4) . . . . ?
C25 C24 C23 O11 179.7(3) . . . . ?
O12 C24 C23 C22 179.5(3) . . . . ?
C25 C24 C23 C22 0.6(5) . . . . ?
O10 C22 C23 O11 1.8(4) . . . . ?
C27 C22 C23 O11 -176.9(3) . . . . ?
O10 C22 C23 C24 -179.1(3) . . . . ?
C27 C22 C23 C24 2.2(5) . . . . ?
N2 N1 C50 C49 177.8(3) . . . . ?
N2 N1 C50 C41 -3.3(5) . . . . ?
C48 C49 C50 N1 -2.6(5) . . . . ?
C44 C49 C50 N1 178.1(3) . . . . ?
C48 C49 C50 C41 178.4(3) . . . . ?
C44 C49 C50 C41 -0.9(5) . . . . ?
C48 C49 C44 C45 -1.2(5) . . . . ?
C50 C49 C44 C45 178.1(3) . . . . ?
C48 C49 C44 C43 177.6(3) . . . . ?
C50 C49 C44 C43 -3.0(5) . . . . ?
C14 C32 C33 C34 177.5(3) . . . . ?
C7 C29 C30 C31 -175.4(3) . . . . ?
C51 N3 C55 C54 -0.9(5) . . . . ?
C28 C38 C39 C40 -178.3(3) . . . . ?
C43 C42 C41 O13 176.7(3) . . . . ?
C43 C42 C41 C50 -4.5(5) . . . . ?
N1 C50 C41 O13 4.5(5) . . . . ?
C49 C50 C41 O13 -176.6(3) . . . . ?
N1 C50 C41 C42 -174.3(3) . . . . ?
C49 C50 C41 C42 4.6(5) . . . . ?
C44 C49 C48 C47 0.7(5) . . . . ?
C50 C49 C48 C47 -178.7(3) . . . . ?
C51 C52 C53 C54 -0.3(6) . . . . ?
N3 C55 C54 C53 1.7(5) . . . . ?
C52 C53 C54 C55 -1.2(6) . . . . ?
C49 C44 C45 C46 0.0(5) . . . . ?
C43 C44 C45 C46 -178.8(3) . . . . ?
C41 C42 C43 C44 0.5(6) . . . . ?
C45 C44 C43 C42 -177.8(3) . . . . ?
C49 C44 C43 C42 3.4(5) . . . . ?
C49 C48 C47 C46 1.2(6) . . . . ?
C44 C45 C46 C47 1.8(6) . . . . ?
C48 C47 C46 C45 -2.4(6) . . . . ?
C21 C35 C36 C37 178.5(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.39
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.856
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.068

_database_code_depnum_ccdc_archive 'CCDC 1002510'
