# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry
# This journal is © The Royal Society of Chemistry 2012


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#
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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_dan001_01
_database_code_depnum_ccdc_archive 'CCDC 886234'
#TrackingRef '- Compound 25.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C19 H23 N O4'
_chemical_formula_sum            'C19 H23 N O4'
_chemical_absolute_configuration unk
_chemical_formula_weight         329.38

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   P21
_symmetry_space_group_name_Hall  P2yb

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

_cell_length_a                   9.7301(9)
_cell_length_b                   19.1540(19)
_cell_length_c                   18.7347(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.915(2)
_cell_angle_gamma                90.00
_cell_volume                     3491.1(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9925
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      26.75

_exptl_crystal_description       piece
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1408
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            41529
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.06
_diffrn_reflns_theta_max         27.00
_reflns_number_total             7856
_reflns_number_gt                6750
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
The crystal was twinned, and the twin contribution was accounted for in
the refinement by the twin matrix 1 0 0 0 -1 0 0 0 -1, because of the
monoclinic angle close to 90 deg., and the twin population parameter BASF
refined to 0.0418(8).
Because ofstructure determination of the light atom structure with
Mo-K(alpha) radiation the Friedel data were merged in the refinement.
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0544P)^2^+1.3958P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7856
_refine_ls_number_parameters     870
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0436
_refine_ls_wR_factor_ref         0.1145
_refine_ls_wR_factor_gt          0.1072
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_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 1.0456(2) 0.40636(13) -0.11919(12) 0.0286(5) Uani 1 1 d . . .
O2 O 1.0478(3) 0.37163(16) -0.23460(14) 0.0424(7) Uani 1 1 d . . .
O3 O 0.9232(3) 0.25154(13) -0.01696(14) 0.0370(6) Uani 1 1 d . . .
O4 O 1.3015(3) 0.26253(15) -0.06499(15) 0.0453(7) Uani 1 1 d . . .
N1 N 1.0158(3) 0.35119(14) 0.02647(14) 0.0258(6) Uani 1 1 d . . .
H1N H 1.0200 0.3969 0.0224 0.031 Uiso 1 1 calc R . .
C1 C 1.1082(4) 0.38971(19) -0.18205(18) 0.0313(8) Uani 1 1 d . . .
C2 C 1.2597(4) 0.3964(2) -0.1730(2) 0.0371(9) Uani 1 1 d . . .
H2A H 1.2978 0.3523 -0.1551 0.056 Uiso 1 1 calc R . .
H2B H 1.2807 0.4338 -0.1388 0.056 Uiso 1 1 calc R . .
H2C H 1.3005 0.4076 -0.2191 0.056 Uiso 1 1 calc R . .
C3 C 0.9013(3) 0.40333(19) -0.11732(17) 0.0267(7) Uani 1 1 d . . .
C4 C 0.8233(4) 0.4453(2) -0.16184(18) 0.0324(8) Uani 1 1 d . . .
H4 H 0.8661 0.4753 -0.1952 0.039 Uiso 1 1 calc R . .
C5 C 0.6817(4) 0.4429(2) -0.1571(2) 0.0394(9) Uani 1 1 d . . .
H5 H 0.6260 0.4716 -0.1871 0.047 Uiso 1 1 calc R . .
C6 C 0.6213(4) 0.3986(2) -0.1085(2) 0.0409(10) Uani 1 1 d . . .
H6 H 0.5239 0.3972 -0.1059 0.049 Uiso 1 1 calc R . .
C7 C 0.6984(4) 0.3564(2) -0.06366(19) 0.0340(8) Uani 1 1 d . . .
C8 C 0.8441(3) 0.35969(18) -0.06679(17) 0.0277(7) Uani 1 1 d . . .
C9 C 0.9324(4) 0.31625(18) -0.01705(17) 0.0277(7) Uani 1 1 d . . .
C10 C 0.6285(4) 0.3089(2) -0.0108(2) 0.0424(10) Uani 1 1 d . . .
H10A H 0.5288 0.3077 -0.0222 0.051 Uiso 1 1 calc R . .
H10B H 0.6647 0.2609 -0.0166 0.051 Uiso 1 1 calc R . .
C11 C 0.6484(4) 0.3308(2) 0.0660(2) 0.0377(9) Uani 1 1 d . . .
H11 H 0.6142 0.3752 0.0798 0.045 Uiso 1 1 calc R . .
C12 C 0.7103(4) 0.2922(2) 0.1152(2) 0.0422(10) Uani 1 1 d . . .
H12 H 0.7418 0.2475 0.1005 0.051 Uiso 1 1 calc R . .
C13 C 0.7361(5) 0.3115(2) 0.1918(2) 0.0460(10) Uani 1 1 d . . .
H13A H 0.6888 0.2776 0.2228 0.055 Uiso 1 1 calc R . .
H13B H 0.6966 0.3583 0.2008 0.055 Uiso 1 1 calc R . .
C14 C 0.8891(5) 0.3125(2) 0.2113(2) 0.0450(10) Uani 1 1 d . . .
H14A H 0.9321 0.2691 0.1936 0.054 Uiso 1 1 calc R . .
H14B H 0.8999 0.3132 0.2639 0.054 Uiso 1 1 calc R . .
C15 C 0.9646(4) 0.3754(2) 0.1800(2) 0.0380(9) Uani 1 1 d . . .
H15A H 0.9062 0.3957 0.1416 0.046 Uiso 1 1 calc R . .
H15B H 0.9749 0.4112 0.2179 0.046 Uiso 1 1 calc R . .
C16 C 1.1064(4) 0.36040(19) 0.14971(18) 0.0352(8) Uani 1 1 d . . .
H16A H 1.1620 0.3350 0.1860 0.042 Uiso 1 1 calc R . .
H16B H 1.1531 0.4053 0.1401 0.042 Uiso 1 1 calc R . .
C17 C 1.1009(4) 0.31735(18) 0.08085(18) 0.0293(7) Uani 1 1 d . . .
H17 H 1.0586 0.2711 0.0920 0.035 Uiso 1 1 calc R . .
C18 C 1.2459(4) 0.3039(2) 0.0518(2) 0.0344(8) Uani 1 1 d . . .
H18A H 1.2860 0.3487 0.0360 0.041 Uiso 1 1 calc R . .
H18B H 1.3053 0.2850 0.0905 0.041 Uiso 1 1 calc R . .
C19 C 1.2438(4) 0.2538(2) -0.0094(2) 0.0347(8) Uani 1 1 d . . .
H19 H 1.1930 0.2118 -0.0040 0.042 Uiso 1 1 calc R . .
O5 O 0.3891(2) 0.21571(14) 0.39338(12) 0.0319(6) Uani 1 1 d . . .
O6 O 0.3670(3) 0.24730(16) 0.27712(14) 0.0467(7) Uani 1 1 d . . .
O7 O 0.5052(3) 0.36716(13) 0.50238(13) 0.0313(5) Uani 1 1 d . . .
O8 O 0.1332(3) 0.35938(18) 0.45344(15) 0.0488(7) Uani 1 1 d . . .
N2 N 0.4212(3) 0.26387(14) 0.54052(13) 0.0227(5) Uani 1 1 d . . .
H2N H 0.4185 0.2184 0.5338 0.027 Uiso 1 1 calc R . .
C20 C 0.1667(4) 0.2202(3) 0.3457(2) 0.0504(11) Uani 1 1 d . . .
H20A H 0.1140 0.2269 0.3012 0.076 Uiso 1 1 calc R . .
H20B H 0.1374 0.2546 0.3811 0.076 Uiso 1 1 calc R . .
H20C H 0.1505 0.1730 0.3640 0.076 Uiso 1 1 calc R . .
C21 C 0.3162(4) 0.2295(2) 0.33178(19) 0.0369(9) Uani 1 1 d . . .
C22 C 0.5332(3) 0.22225(19) 0.39433(17) 0.0273(7) Uani 1 1 d . . .
C23 C 0.6111(4) 0.1863(2) 0.34554(18) 0.0354(8) Uani 1 1 d . . .
H23 H 0.5691 0.1587 0.3092 0.042 Uiso 1 1 calc R . .
C24 C 0.7529(4) 0.1920(2) 0.3516(2) 0.0433(10) Uani 1 1 d . . .
H24 H 0.8096 0.1678 0.3190 0.052 Uiso 1 1 calc R . .
C25 C 0.8123(4) 0.2327(2) 0.4046(2) 0.0415(10) Uani 1 1 d . . .
H25 H 0.9097 0.2359 0.4077 0.050 Uiso 1 1 calc R . .
C26 C 0.7344(4) 0.2691(2) 0.45344(19) 0.0337(8) Uani 1 1 d . . .
C27 C 0.5904(4) 0.26326(18) 0.44794(17) 0.0275(7) Uani 1 1 d . . .
C28 C 0.5013(3) 0.30274(18) 0.49901(17) 0.0244(6) Uani 1 1 d . . .
C29 C 0.8035(4) 0.3124(2) 0.5111(2) 0.0389(9) Uani 1 1 d . . .
H29A H 0.9028 0.3158 0.5008 0.047 Uiso 1 1 calc R . .
H29B H 0.7650 0.3602 0.5095 0.047 Uiso 1 1 calc R . .
C30 C 0.7870(4) 0.2835(2) 0.5853(2) 0.0353(8) Uani 1 1 d . . .
H30 H 0.8233 0.2384 0.5951 0.042 Uiso 1 1 calc R . .
C31 C 0.7249(4) 0.3169(2) 0.6379(2) 0.0368(9) Uani 1 1 d . . .
H31 H 0.6903 0.3622 0.6274 0.044 Uiso 1 1 calc R . .
C32 C 0.7042(4) 0.2904(2) 0.71179(19) 0.0375(9) Uani 1 1 d . . .
H32A H 0.7516 0.3218 0.7462 0.045 Uiso 1 1 calc R . .
H32B H 0.7460 0.2434 0.7164 0.045 Uiso 1 1 calc R . .
C33 C 0.5510(4) 0.2861(2) 0.73015(19) 0.0374(9) Uani 1 1 d . . .
H33A H 0.5424 0.2795 0.7823 0.045 Uiso 1 1 calc R . .
H33B H 0.5061 0.3308 0.7173 0.045 Uiso 1 1 calc R . .
C34 C 0.4764(4) 0.22668(19) 0.69159(18) 0.0319(8) Uani 1 1 d . . .
H34A H 0.4662 0.1873 0.7254 0.038 Uiso 1 1 calc R . .
H34B H 0.5346 0.2103 0.6521 0.038 Uiso 1 1 calc R . .
C35 C 0.3342(4) 0.24521(19) 0.66092(17) 0.0291(7) Uani 1 1 d . . .
H35A H 0.2797 0.2674 0.6988 0.035 Uiso 1 1 calc R . .
H35B H 0.2866 0.2016 0.6466 0.035 Uiso 1 1 calc R . .
C36 C 0.3382(3) 0.29433(18) 0.59646(17) 0.0264(7) Uani 1 1 d . . .
H36 H 0.3825 0.3390 0.6120 0.032 Uiso 1 1 calc R . .
C37 C 0.1921(4) 0.3111(2) 0.5685(2) 0.0336(8) Uani 1 1 d . . .
H37A H 0.1486 0.2677 0.5504 0.040 Uiso 1 1 calc R . .
H37B H 0.1363 0.3287 0.6084 0.040 Uiso 1 1 calc R . .
C38 C 0.1931(4) 0.3650(2) 0.5095(2) 0.0349(8) Uani 1 1 d . . .
H38 H 0.2450 0.4063 0.5175 0.042 Uiso 1 1 calc R . .
O9 O 0.3539(2) -0.00746(12) 0.39321(11) 0.0246(5) Uani 1 1 d . . .
O10 O 0.3229(3) 0.07066(15) 0.30469(14) 0.0435(7) Uani 1 1 d . . .
O11 O 0.4152(2) 0.11225(12) 0.54429(12) 0.0270(5) Uani 1 1 d . . .
O12 O 0.0821(3) 0.0866(2) 0.49868(16) 0.0556(8) Uani 1 1 d . . .
N3 N 0.3867(3) -0.00442(14) 0.55168(13) 0.0214(5) Uani 1 1 d . . .
H3N H 0.4025 -0.0452 0.5318 0.026 Uiso 1 1 calc R . .
C39 C 0.1309(4) 0.0022(2) 0.34547(19) 0.0397(9) Uani 1 1 d . . .
H39A H 0.0741 0.0306 0.3130 0.060 Uiso 1 1 calc R . .
H39B H 0.0966 0.0066 0.3942 0.060 Uiso 1 1 calc R . .
H39C H 0.1265 -0.0468 0.3306 0.060 Uiso 1 1 calc R . .
C40 C 0.2765(4) 0.0270(2) 0.34340(17) 0.0295(7) Uani 1 1 d . . .
C41 C 0.4946(3) 0.00898(17) 0.39966(16) 0.0220(6) Uani 1 1 d . . .
C42 C 0.5836(4) -0.00785(19) 0.34576(17) 0.0282(7) Uani 1 1 d . . .
H42 H 0.5504 -0.0285 0.3027 0.034 Uiso 1 1 calc R . .
C43 C 0.7217(4) 0.0060(2) 0.35554(18) 0.0322(8) Uani 1 1 d . . .
H43 H 0.7844 -0.0059 0.3191 0.039 Uiso 1 1 calc R . .
C44 C 0.7703(3) 0.03703(19) 0.41824(18) 0.0295(7) Uani 1 1 d . . .
H44 H 0.8656 0.0465 0.4240 0.035 Uiso 1 1 calc R . .
C45 C 0.6800(3) 0.05428(18) 0.47262(16) 0.0239(6) Uani 1 1 d . . .
C46 C 0.5394(3) 0.03896(17) 0.46328(15) 0.0211(6) Uani 1 1 d . . .
C47 C 0.4406(3) 0.05284(17) 0.52275(15) 0.0207(6) Uani 1 1 d . . .
C48 C 0.7350(3) 0.08597(19) 0.54174(17) 0.0283(7) Uani 1 1 d . . .
H48A H 0.8279 0.1051 0.5338 0.034 Uiso 1 1 calc R . .
H48B H 0.6746 0.1250 0.5560 0.034 Uiso 1 1 calc R . .
C49 C 0.7421(3) 0.03293(19) 0.60129(18) 0.0288(7) Uani 1 1 d . . .
H49 H 0.7935 -0.0085 0.5936 0.035 Uiso 1 1 calc R . .
C50 C 0.6810(4) 0.0405(2) 0.66392(17) 0.0326(8) Uani 1 1 d . . .
H50 H 0.6346 0.0834 0.6717 0.039 Uiso 1 1 calc R . .
C51 C 0.6780(4) -0.0117(2) 0.72320(19) 0.0370(8) Uani 1 1 d . . .
H51A H 0.7190 0.0093 0.7669 0.044 Uiso 1 1 calc R . .
H51B H 0.7340 -0.0528 0.7103 0.044 Uiso 1 1 calc R . .
C52 C 0.5311(4) -0.0351(2) 0.73829(19) 0.0390(9) Uani 1 1 d . . .
H52A H 0.4716 0.0066 0.7422 0.047 Uiso 1 1 calc R . .
H52B H 0.5300 -0.0598 0.7847 0.047 Uiso 1 1 calc R . .
C53 C 0.4716(4) -0.0835(2) 0.68006(18) 0.0327(8) Uani 1 1 d . . .
H53A H 0.5292 -0.0795 0.6372 0.039 Uiso 1 1 calc R . .
H53B H 0.4781 -0.1323 0.6972 0.039 Uiso 1 1 calc R . .
C54 C 0.3222(4) -0.06866(19) 0.65827(17) 0.0303(8) Uani 1 1 d . . .
H54A H 0.2664 -0.0656 0.7019 0.036 Uiso 1 1 calc R . .
H54B H 0.2869 -0.1084 0.6296 0.036 Uiso 1 1 calc R . .
C55 C 0.3027(3) -0.00139(19) 0.61512(17) 0.0263(7) Uani 1 1 d . . .
H55 H 0.3331 0.0391 0.6451 0.032 Uiso 1 1 calc R . .
C56 C 0.1491(4) 0.0089(2) 0.5933(2) 0.0355(8) Uani 1 1 d . . .
H56A H 0.1211 -0.0286 0.5596 0.043 Uiso 1 1 calc R . .
H56B H 0.0916 0.0048 0.6362 0.043 Uiso 1 1 calc R . .
C57 C 0.1237(4) 0.0781(2) 0.5590(2) 0.0401(9) Uani 1 1 d . . .
H57 H 0.1417 0.1186 0.5869 0.048 Uiso 1 1 calc R . .
O13 O 0.1092(2) 0.62118(12) -0.11048(11) 0.0264(5) Uani 1 1 d . . .
O14 O 0.1060(3) 0.54955(16) -0.20612(13) 0.0412(7) Uani 1 1 d . . .
O15 O 0.0449(2) 0.49678(12) 0.03816(12) 0.0270(5) Uani 1 1 d . . .
O16 O 0.3786(3) 0.50420(17) -0.01525(15) 0.0474(7) Uani 1 1 d . . .
N4 N 0.1056(3) 0.60945(13) 0.04703(12) 0.0194(5) Uani 1 1 d . . .
H4N H 0.0993 0.6514 0.0280 0.023 Uiso 1 1 calc R . .
C58 C 0.3198(4) 0.5992(2) -0.16560(18) 0.0347(8) Uani 1 1 d . . .
H58A H 0.3601 0.5763 -0.2070 0.052 Uiso 1 1 calc R . .
H58B H 0.3616 0.5804 -0.1217 0.052 Uiso 1 1 calc R . .
H58C H 0.3369 0.6496 -0.1681 0.052 Uiso 1 1 calc R . .
C59 C 0.1693(3) 0.58624(19) -0.16551(16) 0.0276(7) Uani 1 1 d . . .
C60 C -0.0329(3) 0.61078(17) -0.10038(16) 0.0235(6) Uani 1 1 d . . .
C61 C -0.1277(4) 0.63467(19) -0.15084(17) 0.0305(8) Uani 1 1 d . . .
H61 H -0.0979 0.6561 -0.1936 0.037 Uiso 1 1 calc R . .
C62 C -0.2663(4) 0.6268(2) -0.13774(18) 0.0343(8) Uani 1 1 d . . .
H62 H -0.3327 0.6441 -0.1710 0.041 Uiso 1 1 calc R . .
C63 C -0.3079(4) 0.5937(2) -0.07611(18) 0.0322(8) Uani 1 1 d . . .
H63 H -0.4033 0.5873 -0.0683 0.039 Uiso 1 1 calc R . .
C64 C -0.2135(3) 0.56935(17) -0.02537(16) 0.0256(7) Uani 1 1 d . . .
C65 C -0.0730(3) 0.57970(17) -0.03745(16) 0.0216(6) Uani 1 1 d . . .
C66 C 0.0319(3) 0.55795(16) 0.01864(15) 0.0194(6) Uani 1 1 d . . .
C67 C -0.2645(3) 0.5357(2) 0.04239(18) 0.0296(7) Uani 1 1 d . . .
H67A H -0.3619 0.5220 0.0356 0.035 Uiso 1 1 calc R . .
H67B H -0.2106 0.4928 0.0523 0.035 Uiso 1 1 calc R . .
C68 C -0.2517(3) 0.58434(19) 0.10514(17) 0.0277(7) Uani 1 1 d . . .
H68 H -0.2969 0.6282 0.1021 0.033 Uiso 1 1 calc R . .
C69 C -0.1812(4) 0.56965(19) 0.16463(17) 0.0300(7) Uani 1 1 d . . .
H69 H -0.1411 0.5246 0.1684 0.036 Uiso 1 1 calc R . .
C70 C -0.1600(4) 0.6187(2) 0.22630(18) 0.0345(8) Uani 1 1 d . . .
H70A H -0.1984 0.5976 0.2699 0.041 Uiso 1 1 calc R . .
H70B H -0.2100 0.6628 0.2166 0.041 Uiso 1 1 calc R . .
C71 C -0.0067(4) 0.6347(2) 0.23903(18) 0.0332(8) Uani 1 1 d . . .
H71A H 0.0055 0.6569 0.2864 0.040 Uiso 1 1 calc R . .
H71B H 0.0455 0.5903 0.2395 0.040 Uiso 1 1 calc R . .
C72 C 0.0517(3) 0.68287(19) 0.18189(17) 0.0287(7) Uani 1 1 d . . .
H72A H -0.0121 0.6829 0.1402 0.034 Uiso 1 1 calc R . .
H72B H 0.0546 0.7310 0.2011 0.034 Uiso 1 1 calc R . .
C73 C 0.1948(3) 0.66379(18) 0.15626(17) 0.0254(7) Uani 1 1 d . . .
H73A H 0.2555 0.6557 0.1983 0.031 Uiso 1 1 calc R . .
H73B H 0.2326 0.7037 0.1294 0.031 Uiso 1 1 calc R . .
C74 C 0.1966(3) 0.59896(17) 0.10875(15) 0.0221(6) Uani 1 1 d . . .
H74 H 0.1615 0.5585 0.1369 0.026 Uiso 1 1 calc R . .
C75 C 0.3437(3) 0.58163(19) 0.08400(18) 0.0283(7) Uani 1 1 d . . .
H75A H 0.3756 0.6187 0.0514 0.034 Uiso 1 1 calc R . .
H75B H 0.4068 0.5805 0.1260 0.034 Uiso 1 1 calc R . .
C76 C 0.3483(4) 0.5124(2) 0.0463(2) 0.0356(8) Uani 1 1 d . . .
H76 H 0.3254 0.4720 0.0731 0.043 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0228(12) 0.0395(14) 0.0235(11) -0.0014(10) -0.0005(9) -0.0054(10)
O2 0.0412(15) 0.0554(17) 0.0308(13) -0.0121(13) 0.0021(12) -0.0027(14)
O3 0.0488(16) 0.0243(13) 0.0380(14) -0.0063(11) 0.0073(12) -0.0062(11)
O4 0.0468(16) 0.0436(16) 0.0458(16) -0.0061(13) 0.0120(13) -0.0038(13)
N1 0.0314(15) 0.0210(14) 0.0251(13) -0.0038(11) 0.0041(11) -0.0006(11)
C1 0.0336(19) 0.0326(19) 0.0279(17) -0.0006(15) 0.0054(15) -0.0052(15)
C2 0.0296(19) 0.045(2) 0.0373(19) 0.0054(17) 0.0069(15) 0.0007(16)
C3 0.0208(16) 0.0344(18) 0.0249(15) -0.0102(14) -0.0006(13) -0.0056(14)
C4 0.0340(19) 0.040(2) 0.0231(16) -0.0107(14) -0.0060(14) -0.0030(16)
C5 0.033(2) 0.054(3) 0.0301(18) -0.0125(17) -0.0103(15) 0.0026(18)
C6 0.0237(18) 0.060(3) 0.039(2) -0.021(2) -0.0037(16) -0.0035(18)
C7 0.0273(18) 0.044(2) 0.0312(17) -0.0171(16) 0.0058(14) -0.0099(16)
C8 0.0279(17) 0.0294(17) 0.0259(16) -0.0099(14) 0.0033(13) -0.0054(14)
C9 0.0310(18) 0.0276(17) 0.0248(16) -0.0078(13) 0.0115(13) -0.0030(14)
C10 0.0318(19) 0.050(2) 0.045(2) -0.0134(19) 0.0090(16) -0.0137(18)
C11 0.036(2) 0.036(2) 0.042(2) -0.0073(17) 0.0155(17) -0.0077(16)
C12 0.051(2) 0.035(2) 0.042(2) -0.0031(18) 0.0220(18) -0.0029(18)
C13 0.066(3) 0.037(2) 0.036(2) 0.0048(17) 0.0164(19) 0.008(2)
C14 0.063(3) 0.039(2) 0.033(2) 0.0095(17) 0.0148(19) 0.016(2)
C15 0.056(2) 0.0312(19) 0.0270(17) -0.0006(15) 0.0039(16) 0.0098(18)
C16 0.052(2) 0.0279(18) 0.0260(17) 0.0021(14) -0.0043(16) 0.0032(17)
C17 0.0369(19) 0.0228(16) 0.0284(17) 0.0024(14) 0.0048(14) -0.0012(14)
C18 0.0318(19) 0.0306(19) 0.041(2) 0.0017(16) -0.0018(15) -0.0029(15)
C19 0.0301(18) 0.0304(19) 0.044(2) -0.0023(16) 0.0027(16) 0.0011(15)
O5 0.0279(12) 0.0475(15) 0.0201(11) -0.0039(11) -0.0027(9) -0.0010(11)
O6 0.0562(18) 0.0543(18) 0.0294(14) 0.0045(13) -0.0073(13) 0.0011(15)
O7 0.0386(13) 0.0268(13) 0.0284(11) 0.0055(10) -0.0024(10) -0.0072(11)
O8 0.0392(15) 0.065(2) 0.0415(15) 0.0082(14) -0.0112(13) -0.0075(14)
N2 0.0269(14) 0.0220(13) 0.0192(12) 0.0016(10) -0.0016(10) -0.0011(11)
C20 0.038(2) 0.074(3) 0.039(2) -0.018(2) -0.0111(18) 0.004(2)
C21 0.042(2) 0.041(2) 0.0273(19) -0.0060(16) -0.0093(16) 0.0013(17)
C22 0.0279(17) 0.0331(18) 0.0209(15) 0.0084(14) 0.0015(13) 0.0005(14)
C23 0.043(2) 0.040(2) 0.0229(16) 0.0060(16) 0.0061(15) 0.0025(18)
C24 0.041(2) 0.054(3) 0.035(2) 0.0152(19) 0.0157(17) 0.010(2)
C25 0.0238(18) 0.057(3) 0.043(2) 0.019(2) 0.0056(16) 0.0015(17)
C26 0.0294(18) 0.042(2) 0.0299(17) 0.0151(16) -0.0001(14) -0.0015(16)
C27 0.0294(17) 0.0300(18) 0.0231(15) 0.0087(13) -0.0021(13) -0.0041(14)
C28 0.0255(16) 0.0279(17) 0.0194(14) 0.0052(12) -0.0096(12) -0.0034(13)
C29 0.0270(18) 0.045(2) 0.045(2) 0.0165(18) -0.0096(16) -0.0077(17)
C30 0.0282(18) 0.035(2) 0.042(2) 0.0101(17) -0.0131(16) -0.0045(15)
C31 0.040(2) 0.0256(18) 0.044(2) 0.0053(16) -0.0206(17) -0.0004(16)
C32 0.046(2) 0.033(2) 0.0328(18) -0.0006(16) -0.0152(16) 0.0047(17)
C33 0.048(2) 0.035(2) 0.0284(17) -0.0021(16) -0.0117(16) 0.0077(18)
C34 0.042(2) 0.0309(18) 0.0225(16) 0.0020(14) -0.0031(14) 0.0037(16)
C35 0.0373(19) 0.0288(17) 0.0213(15) -0.0007(13) 0.0020(14) -0.0012(15)
C36 0.0297(17) 0.0267(17) 0.0227(15) -0.0005(13) -0.0026(13) -0.0018(14)
C37 0.0273(18) 0.039(2) 0.0339(18) 0.0011(16) -0.0022(14) 0.0016(16)
C38 0.0289(18) 0.037(2) 0.038(2) 0.0007(16) -0.0074(15) -0.0003(16)
O9 0.0223(11) 0.0317(12) 0.0197(10) -0.0022(9) -0.0043(8) -0.0023(10)
O10 0.0480(17) 0.0494(17) 0.0328(13) 0.0108(13) -0.0107(12) 0.0003(14)
O11 0.0284(12) 0.0269(12) 0.0258(11) -0.0030(10) 0.0014(9) 0.0007(10)
O12 0.0366(15) 0.086(2) 0.0442(16) -0.0092(17) -0.0121(13) 0.0093(16)
N3 0.0232(13) 0.0219(13) 0.0191(12) -0.0029(10) 0.0021(10) -0.0002(11)
C39 0.0300(19) 0.064(3) 0.0248(17) -0.0074(18) -0.0098(14) 0.0100(19)
C40 0.0331(18) 0.039(2) 0.0167(14) -0.0071(14) -0.0063(13) 0.0044(15)
C41 0.0199(15) 0.0271(16) 0.0190(14) 0.0038(12) -0.0022(12) 0.0001(12)
C42 0.0339(18) 0.0323(18) 0.0184(14) 0.0008(14) 0.0008(13) 0.0029(15)
C43 0.0296(18) 0.044(2) 0.0236(16) 0.0009(15) 0.0074(14) 0.0028(16)
C44 0.0220(16) 0.038(2) 0.0288(16) 0.0034(15) -0.0004(13) 0.0001(14)
C45 0.0213(15) 0.0283(16) 0.0220(14) 0.0036(13) -0.0017(12) -0.0002(13)
C46 0.0205(15) 0.0263(16) 0.0164(13) 0.0017(12) -0.0013(11) 0.0012(12)
C47 0.0199(15) 0.0237(15) 0.0181(13) -0.0027(12) -0.0064(11) 0.0000(12)
C48 0.0217(15) 0.0350(18) 0.0281(16) -0.0016(14) -0.0039(12) -0.0046(14)
C49 0.0199(15) 0.0359(19) 0.0300(17) -0.0046(15) -0.0109(13) 0.0027(14)
C50 0.0361(19) 0.036(2) 0.0251(16) -0.0076(15) -0.0086(14) -0.0021(16)
C51 0.040(2) 0.044(2) 0.0272(17) -0.0063(16) -0.0109(15) -0.0031(18)
C52 0.050(2) 0.047(2) 0.0204(16) -0.0020(16) -0.0054(16) -0.0056(19)
C53 0.042(2) 0.0345(19) 0.0218(16) 0.0005(14) 0.0007(14) -0.0047(16)
C54 0.038(2) 0.0336(19) 0.0195(15) -0.0024(14) 0.0063(14) -0.0047(15)
C55 0.0237(15) 0.0337(18) 0.0217(15) -0.0076(14) 0.0050(12) -0.0041(14)
C56 0.0235(17) 0.049(2) 0.0339(18) -0.0125(17) 0.0069(14) -0.0043(16)
C57 0.0224(17) 0.059(3) 0.039(2) -0.0135(19) -0.0037(15) 0.0044(17)
O13 0.0275(12) 0.0324(13) 0.0193(10) -0.0037(9) 0.0002(9) -0.0057(10)
O14 0.0388(15) 0.0568(17) 0.0283(12) -0.0150(13) 0.0053(11) -0.0077(13)
O15 0.0337(13) 0.0200(11) 0.0272(11) -0.0002(9) -0.0015(10) -0.0004(10)
O16 0.0359(15) 0.062(2) 0.0444(16) -0.0151(15) 0.0075(12) 0.0020(14)
N4 0.0228(13) 0.0197(12) 0.0157(11) 0.0004(10) -0.0043(10) 0.0009(10)
C58 0.0327(19) 0.044(2) 0.0276(17) -0.0025(16) 0.0052(14) -0.0067(16)
C59 0.0299(17) 0.0348(18) 0.0181(14) 0.0002(14) 0.0029(13) -0.0029(15)
C60 0.0234(16) 0.0287(17) 0.0184(14) -0.0053(13) -0.0022(12) -0.0030(13)
C61 0.040(2) 0.0351(19) 0.0165(15) -0.0002(14) -0.0055(14) 0.0010(16)
C62 0.0323(19) 0.044(2) 0.0259(16) -0.0065(16) -0.0134(14) 0.0042(17)
C63 0.0232(16) 0.042(2) 0.0312(17) -0.0078(16) -0.0060(13) 0.0011(15)
C64 0.0258(16) 0.0286(18) 0.0223(15) -0.0050(13) -0.0018(12) -0.0030(13)
C65 0.0254(16) 0.0202(15) 0.0192(14) -0.0059(12) -0.0036(12) -0.0002(12)
C66 0.0184(15) 0.0234(15) 0.0164(13) -0.0006(12) 0.0025(11) 0.0007(12)
C67 0.0206(15) 0.0374(19) 0.0306(17) -0.0030(15) -0.0004(13) -0.0072(14)
C68 0.0254(16) 0.0312(17) 0.0267(16) 0.0018(14) 0.0052(13) -0.0020(14)
C69 0.0318(18) 0.0291(19) 0.0291(16) 0.0002(14) 0.0050(14) -0.0033(15)
C70 0.038(2) 0.044(2) 0.0214(15) 0.0003(15) 0.0068(14) 0.0043(17)
C71 0.0334(19) 0.046(2) 0.0204(15) -0.0024(15) -0.0011(14) 0.0037(16)
C72 0.0295(17) 0.0335(18) 0.0229(15) -0.0053(14) -0.0042(13) 0.0003(15)
C73 0.0254(17) 0.0315(18) 0.0190(15) -0.0015(13) -0.0074(13) -0.0006(14)
C74 0.0235(15) 0.0241(16) 0.0185(13) 0.0013(12) -0.0050(12) -0.0009(13)
C75 0.0199(15) 0.0331(18) 0.0317(17) 0.0008(15) -0.0061(13) -0.0020(14)
C76 0.0233(17) 0.042(2) 0.042(2) 0.0018(17) -0.0010(15) 0.0038(15)

_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 1.372(4) . ?
O1 C3 1.407(4) . ?
O2 C1 1.190(4) . ?
O3 C9 1.243(4) . ?
O4 C19 1.202(4) . ?
N1 C9 1.323(4) . ?
N1 C17 1.455(4) . ?
N1 H1N 0.8800 . ?
C1 C2 1.487(5) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.377(5) . ?
C3 C8 1.386(5) . ?
C4 C5 1.384(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.382(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.379(6) . ?
C6 H6 0.9500 . ?
C7 C8 1.421(5) . ?
C7 C10 1.514(6) . ?
C8 C9 1.508(5) . ?
C10 C11 1.508(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.321(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.500(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.528(6) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.532(6) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.528(6) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.531(5) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.542(5) . ?
C17 H17 1.0000 . ?
C18 C19 1.495(5) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19 0.9500 . ?
O5 C21 1.371(4) . ?
O5 C22 1.407(4) . ?
O6 C21 1.194(5) . ?
O7 C28 1.236(4) . ?
O8 C38 1.197(4) . ?
N2 C28 1.337(4) . ?
N2 C36 1.455(4) . ?
N2 H2N 0.8800 . ?
C20 C21 1.493(6) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C22 C23 1.380(5) . ?
C22 C27 1.385(5) . ?
C23 C24 1.387(6) . ?
C23 H23 0.9500 . ?
C24 C25 1.383(6) . ?
C24 H24 0.9500 . ?
C25 C26 1.385(6) . ?
C25 H25 0.9500 . ?
C26 C27 1.408(5) . ?
C26 C29 1.512(6) . ?
C27 C28 1.505(5) . ?
C29 C30 1.507(5) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.328(6) . ?
C30 H30 0.9500 . ?
C31 C32 1.492(5) . ?
C31 H31 0.9500 . ?
C32 C33 1.537(6) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.526(5) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C35 1.531(5) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.532(5) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 C37 1.540(5) . ?
C36 H36 1.0000 . ?
C37 C38 1.514(5) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 H38 0.9500 . ?
O9 C40 1.360(4) . ?
O9 C41 1.408(4) . ?
O10 C40 1.201(5) . ?
O11 C47 1.234(4) . ?
O12 C57 1.205(5) . ?
N3 C47 1.334(4) . ?
N3 C55 1.455(4) . ?
N3 H3N 0.8800 . ?
C39 C40 1.495(5) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C41 C42 1.379(4) . ?
C41 C46 1.387(4) . ?
C42 C43 1.378(5) . ?
C42 H42 0.9500 . ?
C43 C44 1.393(5) . ?
C43 H43 0.9500 . ?
C44 C45 1.396(5) . ?
C44 H44 0.9500 . ?
C45 C46 1.407(4) . ?
C45 C48 1.520(4) . ?
C46 C47 1.507(4) . ?
C48 C49 1.510(5) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 C50 1.331(5) . ?
C49 H49 0.9500 . ?
C50 C51 1.494(5) . ?
C50 H50 0.9500 . ?
C51 C52 1.529(6) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 C53 1.537(5) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 C54 1.530(5) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 C55 1.531(5) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 C56 1.556(5) . ?
C55 H55 1.0000 . ?
C56 C57 1.492(6) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 H57 0.9500 . ?
O13 C59 1.368(4) . ?
O13 C60 1.412(4) . ?
O14 C59 1.199(4) . ?
O15 C66 1.233(4) . ?
O16 C76 1.206(5) . ?
N4 C66 1.326(4) . ?
N4 C74 1.459(4) . ?
N4 H4N 0.8800 . ?
C58 C59 1.485(5) . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C60 C65 1.383(4) . ?
C60 C61 1.388(5) . ?
C61 C62 1.383(5) . ?
C61 H61 0.9500 . ?
C62 C63 1.384(5) . ?
C62 H62 0.9500 . ?
C63 C64 1.391(5) . ?
C63 H63 0.9500 . ?
C64 C65 1.403(4) . ?
C64 C67 1.514(5) . ?
C65 C66 1.512(4) . ?
C67 C68 1.504(5) . ?
C67 H67A 0.9900 . ?
C67 H67B 0.9900 . ?
C68 C69 1.330(5) . ?
C68 H68 0.9500 . ?
C69 C70 1.500(5) . ?
C69 H69 0.9500 . ?
C70 C71 1.537(5) . ?
C70 H70A 0.9900 . ?
C70 H70B 0.9900 . ?
C71 C72 1.530(5) . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C72 C73 1.524(5) . ?
C72 H72A 0.9900 . ?
C72 H72B 0.9900 . ?
C73 C74 1.528(4) . ?
C73 H73A 0.9900 . ?
C73 H73B 0.9900 . ?
C74 C75 1.548(4) . ?
C74 H74 1.0000 . ?
C75 C76 1.503(5) . ?
C75 H75A 0.9900 . ?
C75 H75B 0.9900 . ?
C76 H76 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
C1 O1 C3 118.0(3) . . ?
C9 N1 C17 122.9(3) . . ?
C9 N1 H1N 118.6 . . ?
C17 N1 H1N 118.6 . . ?
O2 C1 O1 123.9(3) . . ?
O2 C1 C2 126.5(3) . . ?
O1 C1 C2 109.6(3) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 C8 122.9(3) . . ?
C4 C3 O1 120.1(3) . . ?
C8 C3 O1 117.0(3) . . ?
C3 C4 C5 118.8(4) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
C6 C5 C4 119.8(4) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C7 C6 C5 121.9(3) . . ?
C7 C6 H6 119.1 . . ?
C5 C6 H6 119.1 . . ?
C6 C7 C8 118.8(3) . . ?
C6 C7 C10 120.3(3) . . ?
C8 C7 C10 120.8(4) . . ?
C3 C8 C7 117.8(3) . . ?
C3 C8 C9 121.6(3) . . ?
C7 C8 C9 120.6(3) . . ?
O3 C9 N1 123.2(4) . . ?
O3 C9 C8 120.7(3) . . ?
N1 C9 C8 116.1(3) . . ?
C11 C10 C7 113.8(3) . . ?
C11 C10 H10A 108.8 . . ?
C7 C10 H10A 108.8 . . ?
C11 C10 H10B 108.8 . . ?
C7 C10 H10B 108.8 . . ?
H10A C10 H10B 107.7 . . ?
C12 C11 C10 124.0(4) . . ?
C12 C11 H11 118.0 . . ?
C10 C11 H11 118.0 . . ?
C11 C12 C13 126.7(4) . . ?
C11 C12 H12 116.7 . . ?
C13 C12 H12 116.7 . . ?
C12 C13 C14 112.3(3) . . ?
C12 C13 H13A 109.2 . . ?
C14 C13 H13A 109.2 . . ?
C12 C13 H13B 109.2 . . ?
C14 C13 H13B 109.2 . . ?
H13A C13 H13B 107.9 . . ?
C13 C14 C15 112.9(3) . . ?
C13 C14 H14A 109.0 . . ?
C15 C14 H14A 109.0 . . ?
C13 C14 H14B 109.0 . . ?
C15 C14 H14B 109.0 . . ?
H14A C14 H14B 107.8 . . ?
C16 C15 C14 115.8(3) . . ?
C16 C15 H15A 108.3 . . ?
C14 C15 H15A 108.3 . . ?
C16 C15 H15B 108.3 . . ?
C14 C15 H15B 108.3 . . ?
H15A C15 H15B 107.4 . . ?
C15 C16 C17 113.3(3) . . ?
C15 C16 H16A 108.9 . . ?
C17 C16 H16A 108.9 . . ?
C15 C16 H16B 108.9 . . ?
C17 C16 H16B 108.9 . . ?
H16A C16 H16B 107.7 . . ?
N1 C17 C16 111.2(3) . . ?
N1 C17 C18 109.9(3) . . ?
C16 C17 C18 111.6(3) . . ?
N1 C17 H17 108.0 . . ?
C16 C17 H17 108.0 . . ?
C18 C17 H17 108.0 . . ?
C19 C18 C17 112.1(3) . . ?
C19 C18 H18A 109.2 . . ?
C17 C18 H18A 109.2 . . ?
C19 C18 H18B 109.2 . . ?
C17 C18 H18B 109.2 . . ?
H18A C18 H18B 107.9 . . ?
O4 C19 C18 125.0(4) . . ?
O4 C19 H19 117.5 . . ?
C18 C19 H19 117.5 . . ?
C21 O5 C22 119.7(3) . . ?
C28 N2 C36 122.1(3) . . ?
C28 N2 H2N 119.0 . . ?
C36 N2 H2N 119.0 . . ?
C21 C20 H20A 109.5 . . ?
C21 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C21 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O6 C21 O5 124.2(4) . . ?
O6 C21 C20 127.0(4) . . ?
O5 C21 C20 108.8(3) . . ?
C23 C22 C27 123.0(3) . . ?
C23 C22 O5 120.3(3) . . ?
C27 C22 O5 116.6(3) . . ?
C22 C23 C24 117.6(4) . . ?
C22 C23 H23 121.2 . . ?
C24 C23 H23 121.2 . . ?
C25 C24 C23 120.5(4) . . ?
C25 C24 H24 119.8 . . ?
C23 C24 H24 119.8 . . ?
C24 C25 C26 122.0(4) . . ?
C24 C25 H25 119.0 . . ?
C26 C25 H25 119.0 . . ?
C25 C26 C27 117.8(4) . . ?
C25 C26 C29 120.3(3) . . ?
C27 C26 C29 121.8(3) . . ?
C22 C27 C26 119.1(3) . . ?
C22 C27 C28 121.2(3) . . ?
C26 C27 C28 119.7(3) . . ?
O7 C28 N2 123.0(3) . . ?
O7 C28 C27 121.1(3) . . ?
N2 C28 C27 115.9(3) . . ?
C30 C29 C26 113.8(3) . . ?
C30 C29 H29A 108.8 . . ?
C26 C29 H29A 108.8 . . ?
C30 C29 H29B 108.8 . . ?
C26 C29 H29B 108.8 . . ?
H29A C29 H29B 107.7 . . ?
C31 C30 C29 124.3(4) . . ?
C31 C30 H30 117.9 . . ?
C29 C30 H30 117.9 . . ?
C30 C31 C32 126.4(3) . . ?
C30 C31 H31 116.8 . . ?
C32 C31 H31 116.8 . . ?
C31 C32 C33 111.8(3) . . ?
C31 C32 H32A 109.3 . . ?
C33 C32 H32A 109.3 . . ?
C31 C32 H32B 109.3 . . ?
C33 C32 H32B 109.3 . . ?
H32A C32 H32B 107.9 . . ?
C34 C33 C32 112.9(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 . . ?
C33 C34 C35 115.2(3) . . ?
C33 C34 H34A 108.5 . . ?
C35 C34 H34A 108.5 . . ?
C33 C34 H34B 108.5 . . ?
C35 C34 H34B 108.5 . . ?
H34A C34 H34B 107.5 . . ?
C34 C35 C36 113.8(3) . . ?
C34 C35 H35A 108.8 . . ?
C36 C35 H35A 108.8 . . ?
C34 C35 H35B 108.8 . . ?
C36 C35 H35B 108.8 . . ?
H35A C35 H35B 107.7 . . ?
N2 C36 C35 110.1(3) . . ?
N2 C36 C37 111.0(3) . . ?
C35 C36 C37 111.1(3) . . ?
N2 C36 H36 108.2 . . ?
C35 C36 H36 108.2 . . ?
C37 C36 H36 108.2 . . ?
C38 C37 C36 112.0(3) . . ?
C38 C37 H37A 109.2 . . ?
C36 C37 H37A 109.2 . . ?
C38 C37 H37B 109.2 . . ?
C36 C37 H37B 109.2 . . ?
H37A C37 H37B 107.9 . . ?
O8 C38 C37 124.9(4) . . ?
O8 C38 H38 117.6 . . ?
C37 C38 H38 117.6 . . ?
C40 O9 C41 118.5(3) . . ?
C47 N3 C55 121.9(3) . . ?
C47 N3 H3N 119.0 . . ?
C55 N3 H3N 119.0 . . ?
C40 C39 H39A 109.5 . . ?
C40 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C40 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O10 C40 O9 122.9(3) . . ?
O10 C40 C39 127.1(3) . . ?
O9 C40 C39 110.1(3) . . ?
C42 C41 C46 122.3(3) . . ?
C42 C41 O9 120.4(3) . . ?
C46 C41 O9 117.3(3) . . ?
C43 C42 C41 118.7(3) . . ?
C43 C42 H42 120.7 . . ?
C41 C42 H42 120.7 . . ?
C42 C43 C44 120.7(3) . . ?
C42 C43 H43 119.6 . . ?
C44 C43 H43 119.6 . . ?
C43 C44 C45 120.5(3) . . ?
C43 C44 H44 119.8 . . ?
C45 C44 H44 119.8 . . ?
C44 C45 C46 118.8(3) . . ?
C44 C45 C48 120.0(3) . . ?
C46 C45 C48 121.2(3) . . ?
C41 C46 C45 119.0(3) . . ?
C41 C46 C47 120.8(3) . . ?
C45 C46 C47 120.1(3) . . ?
O11 C47 N3 122.9(3) . . ?
O11 C47 C46 122.5(3) . . ?
N3 C47 C46 114.5(3) . . ?
C49 C48 C45 111.9(3) . . ?
C49 C48 H48A 109.2 . . ?
C45 C48 H48A 109.2 . . ?
C49 C48 H48B 109.2 . . ?
C45 C48 H48B 109.2 . . ?
H48A C48 H48B 107.9 . . ?
C50 C49 C48 124.2(3) . . ?
C50 C49 H49 117.9 . . ?
C48 C49 H49 117.9 . . ?
C49 C50 C51 126.7(4) . . ?
C49 C50 H50 116.7 . . ?
C51 C50 H50 116.7 . . ?
C50 C51 C52 111.3(3) . . ?
C50 C51 H51A 109.4 . . ?
C52 C51 H51A 109.4 . . ?
C50 C51 H51B 109.4 . . ?
C52 C51 H51B 109.4 . . ?
H51A C51 H51B 108.0 . . ?
C51 C52 C53 112.9(3) . . ?
C51 C52 H52A 109.0 . . ?
C53 C52 H52A 109.0 . . ?
C51 C52 H52B 109.0 . . ?
C53 C52 H52B 109.0 . . ?
H52A C52 H52B 107.8 . . ?
C54 C53 C52 115.0(3) . . ?
C54 C53 H53A 108.5 . . ?
C52 C53 H53A 108.5 . . ?
C54 C53 H53B 108.5 . . ?
C52 C53 H53B 108.5 . . ?
H53A C53 H53B 107.5 . . ?
C53 C54 C55 113.9(3) . . ?
C53 C54 H54A 108.8 . . ?
C55 C54 H54A 108.8 . . ?
C53 C54 H54B 108.8 . . ?
C55 C54 H54B 108.8 . . ?
H54A C54 H54B 107.7 . . ?
N3 C55 C54 109.3(3) . . ?
N3 C55 C56 109.9(3) . . ?
C54 C55 C56 110.8(3) . . ?
N3 C55 H55 108.9 . . ?
C54 C55 H55 108.9 . . ?
C56 C55 H55 108.9 . . ?
C57 C56 C55 112.2(3) . . ?
C57 C56 H56A 109.2 . . ?
C55 C56 H56A 109.2 . . ?
C57 C56 H56B 109.2 . . ?
C55 C56 H56B 109.2 . . ?
H56A C56 H56B 107.9 . . ?
O12 C57 C56 125.1(4) . . ?
O12 C57 H57 117.5 . . ?
C56 C57 H57 117.5 . . ?
C59 O13 C60 117.6(2) . . ?
C66 N4 C74 122.2(3) . . ?
C66 N4 H4N 118.9 . . ?
C74 N4 H4N 118.9 . . ?
C59 C58 H58A 109.5 . . ?
C59 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C59 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
O14 C59 O13 122.9(3) . . ?
O14 C59 C58 126.4(3) . . ?
O13 C59 C58 110.6(3) . . ?
C65 C60 C61 121.9(3) . . ?
C65 C60 O13 117.7(3) . . ?
C61 C60 O13 120.2(3) . . ?
C62 C61 C60 118.9(3) . . ?
C62 C61 H61 120.6 . . ?
C60 C61 H61 120.6 . . ?
C61 C62 C63 119.8(3) . . ?
C61 C62 H62 120.1 . . ?
C63 C62 H62 120.1 . . ?
C62 C63 C64 121.6(3) . . ?
C62 C63 H63 119.2 . . ?
C64 C63 H63 119.2 . . ?
C63 C64 C65 118.5(3) . . ?
C63 C64 C67 119.6(3) . . ?
C65 C64 C67 121.9(3) . . ?
C60 C65 C64 119.2(3) . . ?
C60 C65 C66 121.0(3) . . ?
C64 C65 C66 119.8(3) . . ?
O15 C66 N4 122.4(3) . . ?
O15 C66 C65 122.2(3) . . ?
N4 C66 C65 115.4(3) . . ?
C68 C67 C64 111.6(3) . . ?
C68 C67 H67A 109.3 . . ?
C64 C67 H67A 109.3 . . ?
C68 C67 H67B 109.3 . . ?
C64 C67 H67B 109.3 . . ?
H67A C67 H67B 108.0 . . ?
C69 C68 C67 124.0(3) . . ?
C69 C68 H68 118.0 . . ?
C67 C68 H68 118.0 . . ?
C68 C69 C70 125.2(3) . . ?
C68 C69 H69 117.4 . . ?
C70 C69 H69 117.4 . . ?
C69 C70 C71 111.4(3) . . ?
C69 C70 H70A 109.3 . . ?
C71 C70 H70A 109.3 . . ?
C69 C70 H70B 109.3 . . ?
C71 C70 H70B 109.3 . . ?
H70A C70 H70B 108.0 . . ?
C72 C71 C70 112.5(3) . . ?
C72 C71 H71A 109.1 . . ?
C70 C71 H71A 109.1 . . ?
C72 C71 H71B 109.1 . . ?
C70 C71 H71B 109.1 . . ?
H71A C71 H71B 107.8 . . ?
C73 C72 C71 115.3(3) . . ?
C73 C72 H72A 108.5 . . ?
C71 C72 H72A 108.5 . . ?
C73 C72 H72B 108.5 . . ?
C71 C72 H72B 108.5 . . ?
H72A C72 H72B 107.5 . . ?
C72 C73 C74 113.4(3) . . ?
C72 C73 H73A 108.9 . . ?
C74 C73 H73A 108.9 . . ?
C72 C73 H73B 108.9 . . ?
C74 C73 H73B 108.9 . . ?
H73A C73 H73B 107.7 . . ?
N4 C74 C73 109.7(3) . . ?
N4 C74 C75 110.2(2) . . ?
C73 C74 C75 111.6(3) . . ?
N4 C74 H74 108.4 . . ?
C73 C74 H74 108.4 . . ?
C75 C74 H74 108.4 . . ?
C76 C75 C74 111.3(3) . . ?
C76 C75 H75A 109.4 . . ?
C74 C75 H75A 109.4 . . ?
C76 C75 H75B 109.4 . . ?
C74 C75 H75B 109.4 . . ?
H75A C75 H75B 108.0 . . ?
O16 C76 C75 125.0(4) . . ?
O16 C76 H76 117.5 . . ?
C75 C76 H76 117.5 . . ?

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
C3 O1 C1 O2 -1.5(5) . . . . ?
C3 O1 C1 C2 179.7(3) . . . . ?
C1 O1 C3 C4 -60.9(4) . . . . ?
C1 O1 C3 C8 122.4(3) . . . . ?
C8 C3 C4 C5 -1.4(5) . . . . ?
O1 C3 C4 C5 -177.8(3) . . . . ?
C3 C4 C5 C6 -0.3(5) . . . . ?
C4 C5 C6 C7 0.4(6) . . . . ?
C5 C6 C7 C8 1.2(5) . . . . ?
C5 C6 C7 C10 179.7(4) . . . . ?
C4 C3 C8 C7 2.9(5) . . . . ?
O1 C3 C8 C7 179.5(3) . . . . ?
C4 C3 C8 C9 -177.8(3) . . . . ?
O1 C3 C8 C9 -1.2(5) . . . . ?
C6 C7 C8 C3 -2.7(5) . . . . ?
C10 C7 C8 C3 178.8(3) . . . . ?
C6 C7 C8 C9 177.9(3) . . . . ?
C10 C7 C8 C9 -0.5(5) . . . . ?
C17 N1 C9 O3 -2.6(5) . . . . ?
C17 N1 C9 C8 175.8(3) . . . . ?
C3 C8 C9 O3 -119.9(4) . . . . ?
C7 C8 C9 O3 59.4(4) . . . . ?
C3 C8 C9 N1 61.6(4) . . . . ?
C7 C8 C9 N1 -119.1(3) . . . . ?
C6 C7 C10 C11 -110.3(4) . . . . ?
C8 C7 C10 C11 68.1(5) . . . . ?
C7 C10 C11 C12 -118.6(4) . . . . ?
C10 C11 C12 C13 178.5(4) . . . . ?
C11 C12 C13 C14 -119.6(5) . . . . ?
C12 C13 C14 C15 73.3(4) . . . . ?
C13 C14 C15 C16 -138.6(3) . . . . ?
C14 C15 C16 C17 69.9(4) . . . . ?
C9 N1 C17 C16 -141.0(3) . . . . ?
C9 N1 C17 C18 95.0(4) . . . . ?
C15 C16 C17 N1 56.4(4) . . . . ?
C15 C16 C17 C18 179.5(3) . . . . ?
N1 C17 C18 C19 -64.2(4) . . . . ?
C16 C17 C18 C19 172.0(3) . . . . ?
C17 C18 C19 O4 132.2(4) . . . . ?
C22 O5 C21 O6 -0.1(6) . . . . ?
C22 O5 C21 C20 -178.7(3) . . . . ?
C21 O5 C22 C23 -55.1(5) . . . . ?
C21 O5 C22 C27 127.8(3) . . . . ?
C27 C22 C23 C24 0.3(5) . . . . ?
O5 C22 C23 C24 -176.7(3) . . . . ?
C22 C23 C24 C25 -0.3(6) . . . . ?
C23 C24 C25 C26 0.1(6) . . . . ?
C24 C25 C26 C27 0.3(6) . . . . ?
C24 C25 C26 C29 179.4(4) . . . . ?
C23 C22 C27 C26 0.1(5) . . . . ?
O5 C22 C27 C26 177.1(3) . . . . ?
C23 C22 C27 C28 178.7(3) . . . . ?
O5 C22 C27 C28 -4.3(5) . . . . ?
C25 C26 C27 C22 -0.3(5) . . . . ?
C29 C26 C27 C22 -179.4(3) . . . . ?
C25 C26 C27 C28 -179.0(3) . . . . ?
C29 C26 C27 C28 2.0(5) . . . . ?
C36 N2 C28 O7 -4.0(5) . . . . ?
C36 N2 C28 C27 174.8(3) . . . . ?
C22 C27 C28 O7 -118.3(4) . . . . ?
C26 C27 C28 O7 60.3(4) . . . . ?
C22 C27 C28 N2 62.8(4) . . . . ?
C26 C27 C28 N2 -118.6(3) . . . . ?
C25 C26 C29 C30 -111.4(4) . . . . ?
C27 C26 C29 C30 67.7(5) . . . . ?
C26 C29 C30 C31 -118.8(4) . . . . ?
C29 C30 C31 C32 179.2(4) . . . . ?
C30 C31 C32 C33 -120.0(4) . . . . ?
C31 C32 C33 C34 72.3(4) . . . . ?
C32 C33 C34 C35 -137.2(3) . . . . ?
C33 C34 C35 C36 70.6(4) . . . . ?
C28 N2 C36 C35 -143.7(3) . . . . ?
C28 N2 C36 C37 92.9(4) . . . . ?
C34 C35 C36 N2 56.9(4) . . . . ?
C34 C35 C36 C37 -179.7(3) . . . . ?
N2 C36 C37 C38 -62.7(4) . . . . ?
C35 C36 C37 C38 174.5(3) . . . . ?
C36 C37 C38 O8 130.9(4) . . . . ?
C41 O9 C40 O10 0.1(5) . . . . ?
C41 O9 C40 C39 -179.7(3) . . . . ?
C40 O9 C41 C42 -68.0(4) . . . . ?
C40 O9 C41 C46 115.3(3) . . . . ?
C46 C41 C42 C43 -0.3(5) . . . . ?
O9 C41 C42 C43 -176.8(3) . . . . ?
C41 C42 C43 C44 -0.7(5) . . . . ?
C42 C43 C44 C45 0.5(6) . . . . ?
C43 C44 C45 C46 0.8(5) . . . . ?
C43 C44 C45 C48 178.0(3) . . . . ?
C42 C41 C46 C45 1.5(5) . . . . ?
O9 C41 C46 C45 178.2(3) . . . . ?
C42 C41 C46 C47 -176.4(3) . . . . ?
O9 C41 C46 C47 0.2(4) . . . . ?
C44 C45 C46 C41 -1.7(5) . . . . ?
C48 C45 C46 C41 -178.9(3) . . . . ?
C44 C45 C46 C47 176.2(3) . . . . ?
C48 C45 C46 C47 -1.0(5) . . . . ?
C55 N3 C47 O11 -5.3(5) . . . . ?
C55 N3 C47 C46 172.4(3) . . . . ?
C41 C46 C47 O11 -116.7(4) . . . . ?
C45 C46 C47 O11 65.4(4) . . . . ?
C41 C46 C47 N3 65.5(4) . . . . ?
C45 C46 C47 N3 -112.4(3) . . . . ?
C44 C45 C48 C49 -102.4(4) . . . . ?
C46 C45 C48 C49 74.8(4) . . . . ?
C45 C48 C49 C50 -124.0(4) . . . . ?
C48 C49 C50 C51 176.4(3) . . . . ?
C49 C50 C51 C52 -117.6(4) . . . . ?
C50 C51 C52 C53 72.8(4) . . . . ?
C51 C52 C53 C54 -137.9(3) . . . . ?
C52 C53 C54 C55 71.5(4) . . . . ?
C47 N3 C55 C54 -148.8(3) . . . . ?
C47 N3 C55 C56 89.3(4) . . . . ?
C53 C54 C55 N3 57.1(4) . . . . ?
C53 C54 C55 C56 178.4(3) . . . . ?
N3 C55 C56 C57 -66.1(4) . . . . ?
C54 C55 C56 C57 173.0(3) . . . . ?
C55 C56 C57 O12 117.8(4) . . . . ?
C60 O13 C59 O14 2.4(5) . . . . ?
C60 O13 C59 C58 -176.2(3) . . . . ?
C59 O13 C60 C65 116.2(3) . . . . ?
C59 O13 C60 C61 -67.1(4) . . . . ?
C65 C60 C61 C62 -0.3(5) . . . . ?
O13 C60 C61 C62 -176.8(3) . . . . ?
C60 C61 C62 C63 -1.9(5) . . . . ?
C61 C62 C63 C64 1.8(6) . . . . ?
C62 C63 C64 C65 0.6(5) . . . . ?
C62 C63 C64 C67 177.9(3) . . . . ?
C61 C60 C65 C64 2.7(5) . . . . ?
O13 C60 C65 C64 179.3(3) . . . . ?
C61 C60 C65 C66 -176.4(3) . . . . ?
O13 C60 C65 C66 0.3(4) . . . . ?
C63 C64 C65 C60 -2.8(5) . . . . ?
C67 C64 C65 C60 -180.0(3) . . . . ?
C63 C64 C65 C66 176.3(3) . . . . ?
C67 C64 C65 C66 -0.9(5) . . . . ?
C74 N4 C66 O15 -6.9(4) . . . . ?
C74 N4 C66 C65 170.9(2) . . . . ?
C60 C65 C66 O15 -119.6(3) . . . . ?
C64 C65 C66 O15 61.4(4) . . . . ?
C60 C65 C66 N4 62.6(4) . . . . ?
C64 C65 C66 N4 -116.4(3) . . . . ?
C63 C64 C67 C68 -103.6(4) . . . . ?
C65 C64 C67 C68 73.5(4) . . . . ?
C64 C67 C68 C69 -122.6(4) . . . . ?
C67 C68 C69 C70 176.3(3) . . . . ?
C68 C69 C70 C71 -118.6(4) . . . . ?
C69 C70 C71 C72 72.9(4) . . . . ?
C70 C71 C72 C73 -138.8(3) . . . . ?
C71 C72 C73 C74 72.8(4) . . . . ?
C66 N4 C74 C73 -144.4(3) . . . . ?
C66 N4 C74 C75 92.4(3) . . . . ?
C72 C73 C74 N4 57.6(3) . . . . ?
C72 C73 C74 C75 180.0(3) . . . . ?
N4 C74 C75 C76 -66.1(4) . . . . ?
C73 C74 C75 C76 171.8(3) . . . . ?
C74 C75 C76 O16 117.1(4) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.199
_refine_diff_density_rms         0.044




data_dan002_01
_database_code_depnum_ccdc_archive 'CCDC 886235'
#TrackingRef '- Compound 20.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H37 N O5'
_chemical_formula_sum            'C29 H37 N O5'
_chemical_absolute_configuration ad
_chemical_formula_weight         479.60

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'
N N 0.0311 0.0180 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21
_symmetry_space_group_name_Hall  P2yb

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

_cell_length_a                   17.1331(3)
_cell_length_b                   5.08920(10)
_cell_length_c                   17.6727(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 118.2340(10)
_cell_angle_gamma                90.00
_cell_volume                     1357.61(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    9957
_cell_measurement_theta_min      2.84
_cell_measurement_theta_max      66.00

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             516
_exptl_absorpt_coefficient_mu    0.637
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8173
_exptl_absorpt_correction_T_max  0.9390
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18755
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0240
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.84
_diffrn_reflns_theta_max         65.99
_reflns_number_total             4419
_reflns_number_gt                4194
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0794P)^2^+0.1856P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.1(2)
_refine_ls_number_reflns         4419
_refine_ls_number_parameters     351
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0429
_refine_ls_wR_factor_ref         0.1217
_refine_ls_wR_factor_gt          0.1184
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.037
_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 0.02111(9) 0.6065(10) 0.84936(8) 0.0513(3) Uani 1 1 d . A .
O2 O 0.11809(11) 0.9025(10) 0.93546(13) 0.0780(5) Uani 1 1 d . A .
O3 O -0.05825(10) 1.1911(10) 0.69048(9) 0.0497(3) Uani 1 1 d . A .
O4 O 0.21335(9) 0.8264(10) 0.73393(9) 0.0565(4) Uani 1 1 d . . .
N1 N -0.05987(10) 0.7526(10) 0.67087(9) 0.0401(3) Uani 1 1 d . A .
H1 H -0.0651(12) 0.602(6) 0.6889(12) 0.041(5) Uiso 1 1 d . . .
C1 C -0.09684(11) 0.9201(10) 0.77816(10) 0.0389(4) Uani 1 1 d . A .
C2 C -0.17073(12) 1.0537(10) 0.77356(12) 0.0463(4) Uani 1 1 d . . .
C3 C -0.19328(14) 1.0111(10) 0.83853(14) 0.0570(5) Uani 1 1 d . A .
H3 H -0.2429 1.1003 0.8366 0.068 Uiso 1 1 calc R . .
C4 C -0.14505(16) 0.8419(11) 0.90588(13) 0.0619(6) Uani 1 1 d . . .
H4 H -0.1618 0.8168 0.9495 0.074 Uiso 1 1 calc R A .
C5 C -0.07311(14) 0.7097(10) 0.91031(11) 0.0544(5) Uani 1 1 d . A .
H5 H -0.0403 0.5916 0.9562 0.065 Uiso 1 1 calc R . .
C6 C -0.04951(12) 0.7522(10) 0.84664(10) 0.0435(4) Uani 1 1 d . . .
C7 C -0.22545(14) 1.2392(11) 0.70018(14) 0.0589(5) Uani 0.872(4) 1 d PD A 1
H7A H -0.1984 1.4162 0.7154 0.071 Uiso 0.872(4) 1 calc PR A 1
H7B H -0.2215 1.1803 0.6487 0.071 Uiso 0.872(4) 1 calc PR A 1
C8 C -0.32073(18) 1.2625(11) 0.67694(19) 0.0671(7) Uani 0.872(4) 1 d PD A 1
H8 H -0.3551 1.1065 0.6581 0.081 Uiso 0.872(4) 1 calc PR A 1
C9 C -0.3618(3) 1.4741(13) 0.6797(3) 0.0936(13) Uani 0.872(4) 1 d PD A 1
H9A H -0.3305 1.6354 0.6980 0.112 Uiso 0.872(4) 1 calc PR A 1
H9B H -0.4232 1.4674 0.6633 0.112 Uiso 0.872(4) 1 calc PR A 1
C7A C -0.22545(14) 1.2392(11) 0.70018(14) 0.0589(5) Uani 0.128(4) 1 d PD A 2
H7C H -0.1837 1.3448 0.6886 0.071 Uiso 0.128(4) 1 calc PR A 2
H7D H -0.2602 1.1305 0.6485 0.071 Uiso 0.128(4) 1 calc PR A 2
C8A C -0.2879(10) 1.425(3) 0.7085(13) 0.0671(7) Uani 0.128(4) 1 d PD A 2
H8A H -0.2690 1.5451 0.7551 0.081 Uiso 0.128(4) 1 calc PR A 2
C9A C -0.3699(14) 1.414(8) 0.649(2) 0.0936(13) Uani 0.128(4) 1 d PD A 2
H9C H -0.3870 1.2924 0.6028 0.112 Uiso 0.128(4) 1 calc PR A 2
H9D H -0.4128 1.5286 0.6506 0.112 Uiso 0.128(4) 1 calc PR A 2
C10 C 0.10396(13) 0.7012(10) 0.89681(12) 0.0504(5) Uani 1 1 d . . .
C11 C 0.17094(16) 0.5225(11) 0.89317(16) 0.0659(6) Uani 1 1 d . A .
H11A H 0.2282 0.5478 0.9446 0.099 Uiso 1 1 calc R . .
H11B H 0.1769 0.5623 0.8419 0.099 Uiso 1 1 calc R . .
H11C H 0.1518 0.3398 0.8907 0.099 Uiso 1 1 calc R . .
C12 C -0.06926(11) 0.9666(10) 0.70976(10) 0.0382(4) Uani 1 1 d . . .
C13 C -0.4296(6) 0.562(2) 0.4405(8) 0.134(4) Uani 0.493(8) 1 d PD B 1
H13A H -0.4501 0.4787 0.3862 0.161 Uiso 0.493(8) 1 calc PR B 1
H13B H -0.4512 0.5061 0.4785 0.161 Uiso 0.493(8) 1 calc PR B 1
C14 C -0.3719(4) 0.752(2) 0.4628(5) 0.108(3) Uani 0.493(8) 1 d PD B 1
H14 H -0.3542 0.8263 0.5178 0.130 Uiso 0.493(8) 1 calc PR B 1
C15 C -0.3310(3) 0.865(3) 0.4140(8) 0.096(3) Uani 0.493(8) 1 d PD B 1
H15A H -0.3527 1.0473 0.3974 0.116 Uiso 0.493(8) 1 calc PR B 1
H15B H -0.3494 0.7624 0.3606 0.116 Uiso 0.493(8) 1 calc PR B 1
C16 C -0.22950(17) 0.8683(11) 0.46496(16) 0.0701(6) Uani 0.493(8) 1 d PD B 1
H16A H -0.2057 0.9444 0.4285 0.084 Uiso 0.493(8) 1 calc PR B 1
H16B H -0.2112 0.9838 0.5156 0.084 Uiso 0.493(8) 1 calc PR B 1
C13A C -0.4416(5) 0.546(2) 0.3811(9) 0.114(3) Uani 0.507(8) 1 d PD B 2
H13C H -0.4481 0.5313 0.4314 0.136 Uiso 0.507(8) 1 calc PR B 2
H13D H -0.4767 0.4399 0.3324 0.136 Uiso 0.507(8) 1 calc PR B 2
C14A C -0.3845(3) 0.7107(15) 0.3789(4) 0.080(2) Uani 0.507(8) 1 d PD B 2
H14A H -0.3805 0.7175 0.3271 0.096 Uiso 0.507(8) 1 calc PR B 2
C15A C -0.3258(3) 0.887(3) 0.4480(8) 0.096(3) Uani 0.507(8) 1 d PD B 2
H15C H -0.3285 0.8412 0.5012 0.116 Uiso 0.507(8) 1 calc PR B 2
H15D H -0.3469 1.0696 0.4325 0.116 Uiso 0.507(8) 1 calc PR B 2
C16A C -0.22950(17) 0.8683(11) 0.46496(16) 0.0701(6) Uani 0.507(8) 1 d PD B 2
H16C H -0.2272 0.9127 0.4115 0.084 Uiso 0.507(8) 1 calc PR B 2
H16D H -0.1935 0.9997 0.5091 0.084 Uiso 0.507(8) 1 calc PR B 2
C17 C -0.18931(16) 0.5990(11) 0.49501(14) 0.0615(5) Uani 1 1 d . . .
H17A H -0.2031 0.5400 0.5408 0.074 Uiso 1 1 calc R B 1
H17B H -0.2182 0.4747 0.4464 0.074 Uiso 1 1 calc R B 1
C18 C -0.09101(14) 0.5834(11) 0.52872(11) 0.0514(5) Uani 1 1 d . A .
H18A H -0.0784 0.6206 0.4806 0.062 Uiso 1 1 calc R . .
H18B H -0.0722 0.4003 0.5473 0.062 Uiso 1 1 calc R . .
C19 C -0.03327(12) 0.7661(10) 0.60337(10) 0.0409(4) Uani 1 1 d . . .
H19 H -0.0426 0.9503 0.5811 0.049 Uiso 1 1 calc R A .
C20 C 0.06441(13) 0.7002(10) 0.63974(11) 0.0455(4) Uani 1 1 d . A .
H20A H 0.0768 0.5330 0.6720 0.055 Uiso 1 1 calc R . .
H20B H 0.0781 0.6743 0.5917 0.055 Uiso 1 1 calc R . .
C21 C 0.12406(13) 0.9117(10) 0.69842(13) 0.0492(4) Uani 1 1 d . A .
H21A H 0.1160 1.0764 0.6657 0.059 Uiso 1 1 calc R . .
H21B H 0.1088 0.9468 0.7450 0.059 Uiso 1 1 calc R . .
C22 C 0.27228(17) 1.0216(11) 0.78788(18) 0.0726(7) Uani 0.872(4) 1 d PD A 1
H22A H 0.2592 1.0593 0.8357 0.087 Uiso 0.872(4) 1 calc PR A 1
H22B H 0.2636 1.1856 0.7547 0.087 Uiso 0.872(4) 1 calc PR A 1
C23 C 0.36656(9) 0.9329(11) 0.82361(14) 0.0646(6) Uani 0.872(4) 1 d PGD A 1
C24 C 0.39199(12) 0.7367(12) 0.78506(16) 0.0978(15) Uani 0.872(4) 1 d PG A 1
H24 H 0.3489 0.6527 0.7345 0.117 Uiso 0.872(4) 1 calc PR A 1
C25 C 0.48049(13) 0.6634(12) 0.82050(17) 0.1004(15) Uani 0.872(4) 1 d PG A 1
H25 H 0.4979 0.5293 0.7942 0.120 Uiso 0.872(4) 1 calc PR A 1
C26 C 0.54356(9) 0.7863(11) 0.89450(15) 0.0733(8) Uani 0.872(4) 1 d PGD A 1
C27 C 0.51813(12) 0.9825(11) 0.93305(14) 0.0930(12) Uani 0.872(4) 1 d PG A 1
H27 H 0.5612 1.0665 0.9836 0.112 Uiso 0.872(4) 1 calc PR A 1
C28 C 0.42963(14) 1.0558(11) 0.89760(15) 0.0884(11) Uani 0.872(4) 1 d PG A 1
H28 H 0.4122 1.1899 0.9239 0.106 Uiso 0.872(4) 1 calc PR A 1
C29 C 0.6609(10) 0.521(2) 0.9023(17) 0.124(3) Uani 0.872(4) 1 d PD A 1
H29A H 0.6487 0.5657 0.8438 0.186 Uiso 0.872(4) 1 calc PR A 1
H29B H 0.6297 0.3579 0.9011 0.186 Uiso 0.872(4) 1 calc PR A 1
H29C H 0.7248 0.4952 0.9384 0.186 Uiso 0.872(4) 1 calc PR A 1
O5 O 0.63214(14) 0.7214(17) 0.93550(16) 0.0919(10) Uani 0.872(4) 1 d PD A 1
C22A C 0.27228(17) 1.0216(11) 0.78788(18) 0.0726(7) Uani 0.128(4) 1 d PD A 2
H22C H 0.2609 1.0525 0.8371 0.087 Uiso 0.128(4) 1 calc PR A 2
H22D H 0.2610 1.1881 0.7554 0.087 Uiso 0.128(4) 1 calc PR A 2
C23A C 0.3673(4) 0.944(4) 0.8210(11) 0.0646(6) Uani 0.128(4) 1 d PGD A 2
C24A C 0.3897(6) 0.689(4) 0.8108(12) 0.0978(15) Uani 0.128(4) 1 d PG A 2
H24A H 0.3447 0.5612 0.7833 0.117 Uiso 0.128(4) 1 calc PR A 2
C25A C 0.4781(7) 0.621(4) 0.8409(13) 0.1004(15) Uani 0.128(4) 1 d PG A 2
H25A H 0.4934 0.4470 0.8339 0.120 Uiso 0.128(4) 1 calc PR A 2
C26A C 0.5441(4) 0.809(5) 0.8812(13) 0.0733(8) Uani 0.128(4) 1 d PGD A 2
C27A C 0.5216(6) 1.064(4) 0.8913(10) 0.0930(12) Uani 0.128(4) 1 d PG A 2
H27A H 0.5667 1.1921 0.9189 0.112 Uiso 0.128(4) 1 calc PR A 2
C28A C 0.4333(7) 1.132(4) 0.8612(9) 0.0884(11) Uani 0.128(4) 1 d PG A 2
H28A H 0.4180 1.3063 0.8682 0.106 Uiso 0.128(4) 1 calc PR A 2
C29A C 0.653(8) 0.471(12) 0.902(13) 0.124(3) Uani 0.128(4) 1 d PD A 2
H29D H 0.7163 0.4476 0.9183 0.186 Uiso 0.128(4) 1 d PR A 2
H29E H 0.6170 0.4058 0.8434 0.186 Uiso 0.128(4) 1 d PR A 2
H29F H 0.6395 0.3726 0.9417 0.186 Uiso 0.128(4) 1 d PR A 2
O5A O 0.6297(9) 0.726(7) 0.9080(16) 0.0919(10) Uani 0.128(4) 1 d PD A 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0605(8) 0.0418(8) 0.0470(6) -0.0031(6) 0.0218(5) 0.0069(6)
O2 0.0634(9) 0.0636(11) 0.1063(13) -0.0255(10) 0.0397(9) -0.0117(8)
O3 0.0772(9) 0.0254(7) 0.0632(7) -0.0002(6) 0.0470(7) -0.0014(6)
O4 0.0568(8) 0.0484(9) 0.0716(8) -0.0021(7) 0.0363(7) 0.0020(6)
N1 0.0597(9) 0.0233(8) 0.0474(8) 0.0032(6) 0.0337(7) 0.0014(6)
C1 0.0497(9) 0.0284(9) 0.0443(8) -0.0049(7) 0.0269(7) -0.0060(7)
C2 0.0504(9) 0.0393(11) 0.0546(10) -0.0047(8) 0.0293(8) -0.0029(8)
C3 0.0643(11) 0.0551(14) 0.0681(12) -0.0077(10) 0.0448(10) -0.0042(10)
C4 0.0793(14) 0.0682(15) 0.0551(11) -0.0025(10) 0.0458(10) -0.0076(12)
C5 0.0725(12) 0.0500(12) 0.0423(9) 0.0024(9) 0.0283(8) -0.0045(10)
C6 0.0533(9) 0.0360(10) 0.0415(8) -0.0052(7) 0.0227(7) -0.0029(8)
C7 0.0603(11) 0.0510(13) 0.0712(12) 0.0061(10) 0.0360(10) 0.0072(10)
C8 0.0574(14) 0.0505(17) 0.0851(17) 0.0004(13) 0.0270(13) 0.0024(12)
C9 0.0681(16) 0.074(3) 0.133(4) -0.007(2) 0.043(2) 0.0173(19)
C7A 0.0603(11) 0.0510(13) 0.0712(12) 0.0061(10) 0.0360(10) 0.0072(10)
C8A 0.0574(14) 0.0505(17) 0.0851(17) 0.0004(13) 0.0270(13) 0.0024(12)
C9A 0.0681(16) 0.074(3) 0.133(4) -0.007(2) 0.043(2) 0.0173(19)
C10 0.0606(11) 0.0456(12) 0.0509(9) 0.0086(9) 0.0313(8) 0.0028(9)
C11 0.0705(13) 0.0671(16) 0.0692(12) 0.0166(11) 0.0404(11) 0.0188(12)
C12 0.0487(8) 0.0264(9) 0.0427(8) -0.0013(7) 0.0244(7) -0.0007(7)
C13 0.082(5) 0.166(11) 0.153(8) 0.059(9) 0.055(6) 0.020(6)
C14 0.076(4) 0.140(8) 0.109(5) 0.007(5) 0.045(4) 0.014(5)
C15 0.081(2) 0.072(3) 0.116(9) 0.022(5) 0.030(3) 0.012(2)
C16 0.0780(15) 0.0476(14) 0.0770(14) 0.0066(11) 0.0304(12) 0.0016(12)
C13A 0.080(4) 0.092(6) 0.161(9) 0.007(6) 0.050(6) 0.003(4)
C14A 0.070(3) 0.065(4) 0.096(4) 0.009(3) 0.032(3) 0.014(3)
C15A 0.081(2) 0.072(3) 0.116(9) 0.022(5) 0.030(3) 0.012(2)
C16A 0.0780(15) 0.0476(14) 0.0770(14) 0.0066(11) 0.0304(12) 0.0016(12)
C17 0.0757(14) 0.0450(12) 0.0565(11) 0.0048(10) 0.0253(10) -0.0028(11)
C18 0.0761(12) 0.0371(10) 0.0450(9) 0.0008(8) 0.0319(9) 0.0030(10)
C19 0.0621(10) 0.0282(9) 0.0431(8) 0.0048(7) 0.0338(8) 0.0053(8)
C20 0.0655(11) 0.0327(10) 0.0514(9) 0.0041(8) 0.0384(8) 0.0071(9)
C21 0.0602(11) 0.0420(11) 0.0558(10) 0.0054(8) 0.0359(9) 0.0074(9)
C22 0.0690(14) 0.0556(16) 0.0941(17) -0.0111(12) 0.0392(13) -0.0012(11)
C23 0.0615(12) 0.0605(15) 0.0706(13) -0.0038(11) 0.0301(10) -0.0056(11)
C24 0.0585(14) 0.116(3) 0.099(3) -0.047(2) 0.0214(15) 0.0069(17)
C25 0.0610(14) 0.121(3) 0.105(3) -0.043(2) 0.0279(15) 0.0046(18)
C26 0.0574(12) 0.089(2) 0.0673(16) 0.0109(15) 0.0245(11) -0.0096(13)
C27 0.0786(18) 0.116(3) 0.0630(18) -0.013(2) 0.0160(15) 0.003(2)
C28 0.0851(19) 0.108(3) 0.0650(18) -0.0150(18) 0.0298(15) 0.0064(19)
C29 0.054(4) 0.133(5) 0.169(4) -0.009(6) 0.040(3) 0.005(4)
O5 0.0538(10) 0.126(2) 0.079(2) 0.010(2) 0.0180(11) -0.0038(12)
C22A 0.0690(14) 0.0556(16) 0.0941(17) -0.0111(12) 0.0392(13) -0.0012(11)
C23A 0.0615(12) 0.0605(15) 0.0706(13) -0.0038(11) 0.0301(10) -0.0056(11)
C24A 0.0585(14) 0.116(3) 0.099(3) -0.047(2) 0.0214(15) 0.0069(17)
C25A 0.0610(14) 0.121(3) 0.105(3) -0.043(2) 0.0279(15) 0.0046(18)
C26A 0.0574(12) 0.089(2) 0.0673(16) 0.0109(15) 0.0245(11) -0.0096(13)
C27A 0.0786(18) 0.116(3) 0.0630(18) -0.013(2) 0.0160(15) 0.003(2)
C28A 0.0851(19) 0.108(3) 0.0650(18) -0.0150(18) 0.0298(15) 0.0064(19)
C29A 0.054(4) 0.133(5) 0.169(4) -0.009(6) 0.040(3) 0.005(4)
O5A 0.0538(10) 0.126(2) 0.079(2) 0.010(2) 0.0180(11) -0.0038(12)

_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 C10 1.350(3) . ?
O1 C6 1.400(2) . ?
O2 C10 1.191(3) . ?
O3 C12 1.232(7) . ?
O4 C22 1.416(3) . ?
O4 C21 1.419(2) . ?
N1 C12 1.337(6) . ?
N1 C19 1.466(2) . ?
N1 H1 0.85(3) . ?
C1 C6 1.387(3) . ?
C1 C2 1.405(3) . ?
C1 C12 1.510(2) . ?
C2 C3 1.391(3) . ?
C2 C7 1.517(3) . ?
C3 C4 1.382(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.374(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.381(2) . ?
C5 H5 0.9500 . ?
C7 C8 1.488(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.300(5) . ?
C8 H8 0.9500 . ?
C9 H9A 0.9500 . ?
C9 H9B 0.9500 . ?
C8A C9A 1.300(5) . ?
C8A H8A 0.9500 . ?
C9A H9C 0.9500 . ?
C9A H9D 0.9500 . ?
C10 C11 1.489(3) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C13 C14 1.304(8) . ?
C13 H13A 0.9500 . ?
C13 H13B 0.9500 . ?
C14 C15 1.463(9) . ?
C14 H14 0.9500 . ?
C15 C16 1.534(5) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.513(4) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C13A C14A 1.304(7) . ?
C13A H13C 0.9500 . ?
C13A H13D 0.9500 . ?
C14A C15A 1.463(9) . ?
C14A H14A 0.9500 . ?
C15A H15C 0.9900 . ?
C15A H15D 0.9900 . ?
C17 C18 1.499(3) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.533(3) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.519(3) . ?
C19 H19 1.0000 . ?
C20 C21 1.508(3) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.499(3) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.3900 . ?
C23 C28 1.3900 . ?
C24 C25 1.3900 . ?
C24 H24 0.9500 . ?
C25 C26 1.3900 . ?
C25 H25 0.9500 . ?
C26 O5 1.377(2) . ?
C26 C27 1.3900 . ?
C27 C28 1.3900 . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 O5 1.381(12) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C29 H29D 0.9290 . ?
C29 H29E 1.1178 . ?
C29 H29F 1.1951 . ?
C23A C24A 1.3900 . ?
C23A C28A 1.3900 . ?
C24A C25A 1.3900 . ?
C24A H24A 0.9500 . ?
C25A C26A 1.3900 . ?
C25A H25A 0.9500 . ?
C26A O5A 1.377(3) . ?
C26A C27A 1.3900 . ?
C27A C28A 1.3900 . ?
C27A H27A 0.9500 . ?
C28A H28A 0.9500 . ?
C29A O5A 1.381(11) . ?
C29A H29D 0.9800 . ?
C29A H29E 0.9800 . ?
C29A H29F 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
C10 O1 C6 118.0(4) . . ?
C22 O4 C21 111.05(17) . . ?
C12 N1 C19 122.6(4) . . ?
C12 N1 H1 118.8(14) . . ?
C19 N1 H1 118.3(14) . . ?
C6 C1 C2 119.18(15) . . ?
C6 C1 C12 121.31(15) . . ?
C2 C1 C12 119.50(16) . . ?
C3 C2 C1 118.13(19) . . ?
C3 C2 C7 120.12(18) . . ?
C1 C2 C7 121.74(15) . . ?
C4 C3 C2 121.4(2) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C5 C4 C3 120.60(17) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
C4 C5 C6 118.52(19) . . ?
C4 C5 H5 120.7 . . ?
C6 C5 H5 120.7 . . ?
C5 C6 C1 122.12(17) . . ?
C5 C6 O1 118.06(17) . . ?
C1 C6 O1 119.69(14) . . ?
C8 C7 C2 116.05(19) . . ?
C8 C7 H7A 108.3 . . ?
C2 C7 H7A 108.3 . . ?
C8 C7 H7B 108.3 . . ?
C2 C7 H7B 108.3 . . ?
H7A C7 H7B 107.4 . . ?
C9 C8 C7 126.8(3) . . ?
C9 C8 H8 116.6 . . ?
C7 C8 H8 116.6 . . ?
C8 C9 H9A 120.0 . . ?
C8 C9 H9B 120.0 . . ?
H9A C9 H9B 120.0 . . ?
C9A C8A H8A 121.8 . . ?
C8A C9A H9C 120.0 . . ?
C8A C9A H9D 120.0 . . ?
H9C C9A H9D 120.0 . . ?
O2 C10 O1 122.12(19) . . ?
O2 C10 C11 126.7(2) . . ?
O1 C10 C11 111.1(2) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O3 C12 N1 122.79(14) . . ?
O3 C12 C1 120.9(4) . . ?
N1 C12 C1 116.3(4) . . ?
C14 C13 H13A 120.0 . . ?
C14 C13 H13B 120.0 . . ?
H13A C13 H13B 120.0 . . ?
C13 C14 C15 128.4(10) . . ?
C13 C14 H14 115.8 . . ?
C15 C14 H14 115.8 . . ?
C14 C15 C16 112.6(7) . . ?
C14 C15 H15A 109.1 . . ?
C16 C15 H15A 109.1 . . ?
C14 C15 H15B 109.1 . . ?
C16 C15 H15B 109.1 . . ?
H15A C15 H15B 107.8 . . ?
C17 C16 C15 113.5(6) . . ?
C17 C16 H16A 108.9 . . ?
C15 C16 H16A 108.9 . . ?
C17 C16 H16B 108.9 . . ?
C15 C16 H16B 108.9 . . ?
H16A C16 H16B 107.7 . . ?
C14A C13A H13C 120.0 . . ?
C14A C13A H13D 120.0 . . ?
H13C C13A H13D 120.0 . . ?
C13A C14A C15A 126.7(9) . . ?
C13A C14A H14A 116.6 . . ?
C15A C14A H14A 116.6 . . ?
C14A C15A H15C 109.2 . . ?
C14A C15A H15D 109.2 . . ?
H15C C15A H15D 107.9 . . ?
C18 C17 C16 115.3(2) . . ?
C18 C17 H17A 108.5 . . ?
C16 C17 H17A 108.5 . . ?
C18 C17 H17B 108.5 . . ?
C16 C17 H17B 108.5 . . ?
H17A C17 H17B 107.5 . . ?
C17 C18 C19 117.14(17) . . ?
C17 C18 H18A 108.0 . . ?
C19 C18 H18A 108.0 . . ?
C17 C18 H18B 108.0 . . ?
C19 C18 H18B 108.0 . . ?
H18A C18 H18B 107.3 . . ?
N1 C19 C20 110.46(13) . . ?
N1 C19 C18 110.46(15) . . ?
C20 C19 C18 111.33(15) . . ?
N1 C19 H19 108.2 . . ?
C20 C19 H19 108.2 . . ?
C18 C19 H19 108.2 . . ?
C21 C20 C19 112.7(4) . . ?
C21 C20 H20A 109.1 . . ?
C19 C20 H20A 109.1 . . ?
C21 C20 H20B 109.1 . . ?
C19 C20 H20B 109.1 . . ?
H20A C20 H20B 107.8 . . ?
O4 C21 C20 108.9(4) . . ?
O4 C21 H21A 109.9 . . ?
C20 C21 H21A 109.9 . . ?
O4 C21 H21B 109.9 . . ?
C20 C21 H21B 109.9 . . ?
H21A C21 H21B 108.3 . . ?
O4 C22 C23 110.8(2) . . ?
O4 C22 H22A 109.5 . . ?
C23 C22 H22A 109.5 . . ?
O4 C22 H22B 109.5 . . ?
C23 C22 H22B 109.5 . . ?
H22A C22 H22B 108.1 . . ?
C24 C23 C28 120.0 . . ?
C24 C23 C22 122.35(18) . . ?
C28 C23 C22 117.65(18) . . ?
C23 C24 C25 120.0 . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
C24 C25 C26 120.0 . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
O5 C26 C25 124.0(2) . . ?
O5 C26 C27 115.9(2) . . ?
C25 C26 C27 120.0 . . ?
C28 C27 C26 120.0 . . ?
C28 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
C27 C28 C23 120.0 . . ?
C27 C28 H28 120.0 . . ?
C23 C28 H28 120.0 . . ?
C26 O5 C29 118.7(8) . . ?
C24A C23A C28A 120.0 . . ?
C25A C24A C23A 120.00(5) . . ?
C25A C24A H24A 120.0 . . ?
C23A C24A H24A 120.0 . . ?
C24A C25A C26A 120.0 . . ?
C24A C25A H25A 120.0 . . ?
C26A C25A H25A 120.0 . . ?
O5A C26A C27A 124(2) . . ?
O5A C26A C25A 116(2) . . ?
C27A C26A C25A 120.0 . . ?
C28A C27A C26A 120.00(6) . . ?
C28A C27A H27A 120.0 . . ?
C26A C27A H27A 120.0 . . ?
C27A C28A C23A 120.0 . . ?
C27A C28A H28A 120.0 . . ?
C23A C28A H28A 120.0 . . ?
O5A C29A H29D 114.4 . . ?
O5A C29A H29E 109.6 . . ?
H29D C29A H29E 109.5 . . ?
O5A C29A H29F 104.2 . . ?
H29D C29A H29F 109.5 . . ?
H29E C29A H29F 109.5 . . ?
C26A O5A C29A 124(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 0.0(3) . . . . ?
C12 C1 C2 C3 -178.59(17) . . . . ?
C6 C1 C2 C7 -179.79(18) . . . . ?
C12 C1 C2 C7 1.6(3) . . . . ?
C1 C2 C3 C4 -0.2(3) . . . . ?
C7 C2 C3 C4 179.6(2) . . . . ?
C2 C3 C4 C5 -0.2(4) . . . . ?
C3 C4 C5 C6 0.8(3) . . . . ?
C4 C5 C6 C1 -1.1(3) . . . . ?
C4 C5 C6 O1 -176.81(19) . . . . ?
C2 C1 C6 C5 0.7(3) . . . . ?
C12 C1 C6 C5 179.21(17) . . . . ?
C2 C1 C6 O1 176.34(16) . . . . ?
C12 C1 C6 O1 -5.1(3) . . . . ?
C10 O1 C6 C5 -86.8(2) . . . . ?
C10 O1 C6 C1 97.38(19) . . . . ?
C3 C2 C7 C8 -29.4(3) . . . . ?
C1 C2 C7 C8 150.4(2) . . . . ?
C2 C7 C8 C9 118.9(4) . . . . ?
C6 O1 C10 O2 -0.2(3) . . . . ?
C6 O1 C10 C11 179.66(16) . . . . ?
C19 N1 C12 O3 1.7(3) . . . . ?
C19 N1 C12 C1 -179.87(15) . . . . ?
C6 C1 C12 O3 -127.2(2) . . . . ?
C2 C1 C12 O3 51.4(2) . . . . ?
C6 C1 C12 N1 54.4(2) . . . . ?
C2 C1 C12 N1 -127.06(18) . . . . ?
C13 C14 C15 C16 -126.8(11) . . . . ?
C14 C15 C16 C17 57.8(13) . . . . ?
C15 C16 C17 C18 167.8(6) . . . . ?
C16 C17 C18 C19 56.8(2) . . . . ?
C12 N1 C19 C20 100.94(19) . . . . ?
C12 N1 C19 C18 -135.45(18) . . . . ?
C17 C18 C19 N1 48.1(2) . . . . ?
C17 C18 C19 C20 171.21(16) . . . . ?
N1 C19 C20 C21 -70.35(18) . . . . ?
C18 C19 C20 C21 166.55(15) . . . . ?
C22 O4 C21 C20 178.44(17) . . . . ?
C19 C20 C21 O4 176.02(14) . . . . ?
C21 O4 C22 C23 -178.71(19) . . . . ?
O4 C22 C23 C24 21.4(3) . . . . ?
O4 C22 C23 C28 -159.1(2) . . . . ?
C28 C23 C24 C25 0.0 . . . . ?
C22 C23 C24 C25 179.5(3) . . . . ?
C23 C24 C25 C26 0.0 . . . . ?
C24 C25 C26 O5 178.0(3) . . . . ?
C24 C25 C26 C27 0.0 . . . . ?
O5 C26 C27 C28 -178.2(3) . . . . ?
C25 C26 C27 C28 0.0 . . . . ?
C26 C27 C28 C23 0.0 . . . . ?
C24 C23 C28 C27 0.0 . . . . ?
C22 C23 C28 C27 -179.5(3) . . . . ?
C25 C26 O5 C29 -0.7(11) . . . . ?
C27 C26 O5 C29 177.4(11) . . . . ?
C28A C23A C24A C25A 0.0 . . . . ?
C23A C24A C25A C26A 0.0 . . . . ?
C24A C25A C26A O5A -179(2) . . . . ?
C24A C25A C26A C27A 0.0 . . . . ?
O5A C26A C27A C28A 179(2) . . . . ?
C25A C26A C27A C28A 0.0 . . . . ?
C26A C27A C28A C23A 0.0 . . . . ?
C24A C23A C28A C27A 0.0 . . . . ?
C27A C26A O5A C29A 177(11) . . . . ?
C25A C26A O5A C29A -4(11) . . . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        65.99
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.233
_refine_diff_density_min         -0.169
_refine_diff_density_rms         0.035