data_global
_journal_name_full               CrystEngComm
_journal_coden_cambridge         1350
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
loop_
_publ_author_name
_publ_author_address
F.Luciawati
;School of Chemistry and Centre for Green Chemistry,
Monash University, Wellington Road, Clayton, Victoria,
3800, Australia
;
L.T.Higham
;School of Chemistry and Centre for Green Chemistry,
Monash University, Wellington Road, Clayton, Victoria,
3800, Australia
;
J.L.Scott
;School of Chemistry and Centre for Green Chemistry,
Monash University, Wellington Road, Clayton, Victoria,
3800, Australia
;
C.R.Strauss
;QUILL Centre, The Queen?s University of Belfast,
David Keir Building, Stranmillis Rd, Belfast BT9 5AG,
Northern Ireland, UK
;
_publ_contact_author_address     
;School of Chemistry and Centre for Green Chemistry,
Monash University, Wellington Road, Clayton, Victoria,
3800, Australia
;
_publ_contact_author_email       
'Janet.Scott@sci.monash.edu.au janetsco@tiscali.co.uk'
_publ_contact_author_name        'Janet L. Scott'

# Attachment '2b.cif'

data_2b
_database_code_depnum_ccdc_archive 'CCDC 641524'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
(3,4:10,11:19,20:26,27-tetrabenzo-5,9,21,25-tetraoxa-tricyclo[27.3.1.113,17]
tetratriaconta-1(32),3,10,13,15,17(34),19,26,29(33),30-decaene-33,34-diol)
propylenediamine hemi-salt
;
_chemical_name_common            
;
(3,4:10,11:19,20:26,27-tetrabenzo-5,9,21,25-tetraoxa-
tricyclo(27.3.1.113,17) tetratriaconta-
1(32),3,10,13,15,17(34),19,26,29(33),30-decaene-33,34-diol)
propylenediamine hemi-salt
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H43 O6, C3 H11 N2'
_chemical_formula_sum            'C49 H54 N2 O6'
_chemical_formula_weight         766.94

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

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_space_group_name_Hall           '-P 1'
_space_group_id                  2

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

_cell_length_a                   12.6886(3)
_cell_length_b                   14.0567(4)
_cell_length_c                   14.1856(6)
_cell_angle_alpha                96.182(1)
_cell_angle_beta                 110.043(1)
_cell_angle_gamma                116.463(2)
_cell_volume                     2023.28(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)

_exptl_crystal_description       needles
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             820
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_type   none

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(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  'Enraf Nonius Kappa CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_number            7520
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1131
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.61
_diffrn_reflns_theta_max         25.71
_reflns_number_total             7520
_reflns_number_gt                4156
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Nonius collect'
_computing_cell_refinement       'Nonius collect'
_computing_data_reduction        'Nonius collect'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-seed
_computing_publication_material  ciftab

_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.
Most hydrogen atoms were refined using a riding mode,but the positions of
hydrogen atoms of NH2/NH3+ and OH/O- groups were located in electron density
difference maps and these atoms were refined without restraints.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0471P)^2^+3.4172P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7520
_refine_ls_number_parameters     538
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1494
_refine_ls_R_factor_gt           0.0685
_refine_ls_wR_factor_ref         0.1820
_refine_ls_wR_factor_gt          0.1529
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_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 0.9162(2) 0.0438(2) 0.0638(2) 0.0299(6) Uani 1 1 d . . .
C1 C 0.8738(3) 0.0808(3) 0.1244(3) 0.0246(9) Uani 1 1 d . . .
O2 O 0.9694(2) 0.2823(2) -0.1174(2) 0.0302(6) Uani 1 1 d . . .
C2 C 0.8794(3) 0.1840(3) 0.1291(3) 0.0249(9) Uani 1 1 d . . .
O3 O 0.7607(2) -0.3070(2) 0.1001(2) 0.0305(6) Uani 1 1 d . . .
C3 C 0.9173(3) 0.2434(3) 0.0530(3) 0.0272(9) Uani 1 1 d . . .
H3A H 1.0007 0.2512 0.0580 0.033 Uiso 1 1 calc R . .
H3B H 0.9317 0.3193 0.0732 0.033 Uiso 1 1 calc R . .
O4 O 1.8558(2) 0.7487(2) 0.4323(2) 0.0321(7) Uani 1 1 d . . .
C4 C 0.8128(4) 0.1808(3) -0.0599(3) 0.0270(9) Uani 1 1 d . . .
C5 C 0.8424(4) 0.2008(3) -0.1440(3) 0.0298(9) Uani 1 1 d . . .
C6 C 1.0032(4) 0.3066(3) -0.2017(3) 0.0313(9) Uani 1 1 d . . .
H6A H 0.9381 0.3185 -0.2531 0.038 Uiso 1 1 calc R . .
H6B H 1.0043 0.2434 -0.2387 0.038 Uiso 1 1 calc R . .
C7 C 1.1373(4) 0.4109(3) -0.1551(3) 0.0335(10) Uani 1 1 d . . .
H7A H 1.1665 0.4234 -0.2113 0.040 Uiso 1 1 calc R . .
H7B H 1.1305 0.4756 -0.1301 0.040 Uiso 1 1 calc R . .
C8 C 0.7604(4) -0.4069(3) 0.0648(3) 0.0306(9) Uani 1 1 d . . .
H8A H 0.7809 -0.4060 0.0035 0.037 Uiso 1 1 calc R . .
H8B H 0.6731 -0.4736 0.0433 0.037 Uiso 1 1 calc R . .
C9 C 0.6676(3) -0.2904(3) 0.0324(3) 0.0266(9) Uani 1 1 d . . .
C10 C 0.6823(3) -0.1862(3) 0.0660(3) 0.0242(9) Uani 1 1 d . . .
C11 C 0.7984(4) -0.0993(3) 0.1686(3) 0.0280(9) Uani 1 1 d . . .
H11A H 0.7854 -0.1238 0.2287 0.034 Uiso 1 1 calc R . .
H11B H 0.8790 -0.0958 0.1709 0.034 Uiso 1 1 calc R . .
C12 C 0.8180(3) 0.0153(3) 0.1822(3) 0.0227(8) Uani 1 1 d . . .
C16 C 0.6827(4) 0.1054(3) -0.0822(3) 0.0338(10) Uani 1 1 d . . .
H16 H 0.6598 0.0915 -0.0259 0.041 Uiso 1 1 calc R . .
C17 C 0.5863(4) 0.0504(3) -0.1863(3) 0.0408(11) Uani 1 1 d . . .
H17 H 0.4978 0.0011 -0.2005 0.049 Uiso 1 1 calc R . .
C18 C 0.6194(4) 0.0673(3) -0.2678(4) 0.0404(11) Uani 1 1 d . . .
H18 H 0.5540 0.0273 -0.3385 0.049 Uiso 1 1 calc R . .
C19 C 0.7472(4) 0.1422(3) -0.2485(3) 0.0349(10) Uani 1 1 d . . .
H19 H 0.7698 0.1536 -0.3054 0.042 Uiso 1 1 calc R . .
C20 C 0.5664(4) -0.3698(3) -0.0638(3) 0.0332(10) Uani 1 1 d . . .
H20 H 0.5601 -0.4390 -0.0870 0.040 Uiso 1 1 calc R . .
C21 C 0.4755(4) -0.3458(4) -0.1249(3) 0.0404(11) Uani 1 1 d . . .
H21 H 0.4060 -0.3992 -0.1903 0.048 Uiso 1 1 calc R . .
C22 C 0.4844(4) -0.2453(4) -0.0918(3) 0.0383(11) Uani 1 1 d . . .
H22 H 0.4201 -0.2304 -0.1330 0.046 Uiso 1 1 calc R . .
C23 C 0.5884(4) -0.1665(3) 0.0021(3) 0.0308(9) Uani 1 1 d . . .
H23 H 0.5956 -0.0965 0.0236 0.037 Uiso 1 1 calc R . .
C24 C 0.7734(3) 0.0562(3) 0.2437(3) 0.0296(9) Uani 1 1 d . . .
H24 H 0.7354 0.0122 0.2823 0.036 Uiso 1 1 calc R . .
C25 C 0.7822(4) 0.1582(4) 0.2506(3) 0.0338(10) Uani 1 1 d . . .
H25 H 0.7527 0.1849 0.2945 0.041 Uiso 1 1 calc R . .
C26 C 0.8352(3) 0.2212(3) 0.1921(3) 0.0305(10) Uani 1 1 d . . .
H26 H 0.8410 0.2914 0.1957 0.037 Uiso 1 1 calc R . .
O1' O 1.4381(2) 0.5503(2) 0.3676(2) 0.0290(6) Uani 1 1 d . . .
H1'O H 1.389(5) 0.491(5) 0.389(4) 0.084(19) Uiso 1 1 d . . .
C1' C 1.3805(3) 0.5717(3) 0.2789(3) 0.0228(8) Uani 1 1 d . . .
O2' O 1.1256(2) 0.4596(2) 0.47800(19) 0.0289(6) Uani 1 1 d . . .
C2' C 1.2496(3) 0.5450(3) 0.2401(3) 0.0232(8) Uani 1 1 d . . .
C3' C 1.1744(3) 0.5076(3) 0.3045(3) 0.0244(9) Uani 1 1 d . . .
H3'1 H 1.1678 0.4373 0.3160 0.029 Uiso 1 1 calc R . .
H3'2 H 1.0845 0.4924 0.2651 0.029 Uiso 1 1 calc R . .
C4' C 1.2408(3) 0.5958(3) 0.4107(3) 0.0234(8) Uani 1 1 d . . .
C5' C 1.2186(3) 0.5688(3) 0.4978(3) 0.0250(9) Uani 1 1 d . . .
C6' C 1.0990(4) 0.4312(3) 0.5651(3) 0.0296(9) Uani 1 1 d . . .
H6'1 H 1.0717 0.4796 0.5927 0.035 Uiso 1 1 calc R . .
H6'2 H 1.1789 0.4427 0.6228 0.035 Uiso 1 1 calc R . .
C7' C 0.9911(4) 0.3106(3) 0.5267(3) 0.0312(10) Uani 1 1 d . . .
H7'1 H 0.9121 0.3011 0.4697 0.037 Uiso 1 1 calc R . .
H7'2 H 0.9692 0.2919 0.5854 0.037 Uiso 1 1 calc R . .
C8' C 1.9760(3) 0.7710(3) 0.5139(3) 0.0307(9) Uani 1 1 d . . .
H8'1 H 1.9656 0.7609 0.5789 0.037 Uiso 1 1 calc R . .
H8'2 H 2.0467 0.8487 0.5306 0.037 Uiso 1 1 calc R . .
C9' C 1.8081(4) 0.8159(3) 0.4511(3) 0.0259(9) Uani 1 1 d . . .
C10' C 1.6818(3) 0.7811(3) 0.3770(3) 0.0234(8) Uani 1 1 d . . .
C11' C 1.6044(3) 0.6727(3) 0.2855(3) 0.0262(9) Uani 1 1 d . . .
H11C H 1.6399 0.6856 0.2328 0.031 Uiso 1 1 calc R . .
H11D H 1.6177 0.6149 0.3125 0.031 Uiso 1 1 calc R . .
C12' C 1.4608(3) 0.6297(3) 0.2321(3) 0.0233(8) Uani 1 1 d . . .
C13' C 1.4049(4) 0.6524(3) 0.1418(3) 0.0272(9) Uani 1 1 d . . .
H13' H 1.4572 0.6903 0.1084 0.033 Uiso 1 1 calc R . .
C14' C 1.2741(4) 0.6210(3) 0.0993(3) 0.0279(9) Uani 1 1 d . . .
H14' H 1.2365 0.6353 0.0361 0.033 Uiso 1 1 calc R . .
C15' C 1.1990(4) 0.5692(3) 0.1488(3) 0.0255(9) Uani 1 1 d . . .
H15' H 1.1098 0.5493 0.1198 0.031 Uiso 1 1 calc R . .
C16' C 1.3281(4) 0.7064(3) 0.4270(3) 0.0315(10) Uani 1 1 d . . .
H16' H 1.3409 0.7277 0.3686 0.038 Uiso 1 1 calc R . .
C17' C 1.3976(4) 0.7876(3) 0.5240(3) 0.0362(10) Uani 1 1 d . . .
H17' H 1.4572 0.8626 0.5320 0.043 Uiso 1 1 calc R . .
C18' C 1.3794(4) 0.7580(3) 0.6093(3) 0.0337(10) Uani 1 1 d . . .
H18' H 1.4288 0.8123 0.6770 0.040 Uiso 1 1 calc R . .
C19' C 1.2892(4) 0.6491(3) 0.5962(3) 0.0302(9) Uani 1 1 d . . .
H19' H 1.2756 0.6294 0.6548 0.036 Uiso 1 1 calc R . .
C20' C 1.8780(4) 0.9116(3) 0.5373(3) 0.0336(10) Uani 1 1 d . . .
H20' H 1.9628 0.9328 0.5882 0.040 Uiso 1 1 calc R . .
C21' C 1.8236(4) 0.9766(3) 0.5491(3) 0.0353(10) Uani 1 1 d . . .
H21' H 1.8708 1.0417 0.6083 0.042 Uiso 1 1 calc R . .
C22' C 1.7007(4) 0.9457(3) 0.4744(3) 0.0335(10) Uani 1 1 d . . .
H22' H 1.6642 0.9907 0.4808 0.040 Uiso 1 1 calc R . .
C23' C 1.6304(4) 0.8479(3) 0.3895(3) 0.0299(9) Uani 1 1 d . . .
H23' H 1.5454 0.8267 0.3391 0.036 Uiso 1 1 calc R . .
N1 N 1.3295(4) 0.3774(3) 0.4315(3) 0.0410(9) Uani 1 1 d . . .
H1NA H 1.246(5) 0.351(4) 0.430(4) 0.065(16) Uiso 1 1 d . . .
H1NB H 1.384(6) 0.393(5) 0.504(5) 0.09(2) Uiso 1 1 d . . .
C1G C 1.3408(5) 0.2927(4) 0.3707(4) 0.0557(14) Uani 1 1 d . . .
H1G1 H 1.3232 0.2290 0.3994 0.067 Uiso 1 1 calc R . .
H1G2 H 1.4302 0.3258 0.3754 0.067 Uiso 1 1 calc R . .
C2G C 1.2431(5) 0.2544(4) 0.2595(4) 0.0538(14) Uani 1 1 d . . .
H2G1 H 1.2628 0.3185 0.2314 0.065 Uiso 1 1 calc R . .
H2G2 H 1.1546 0.2247 0.2562 0.065 Uiso 1 1 calc R . .
C3G C 1.2452(5) 0.1617(4) 0.1903(4) 0.0621(16) Uani 1 1 d . . .
H3G1 H 1.3346 0.1892 0.1964 0.074 Uiso 1 1 calc R . .
H3G2 H 1.2188 0.0948 0.2144 0.074 Uiso 1 1 calc R . .
N2 N 1.1535(4) 0.1332(4) 0.0806(4) 0.0501(11) Uani 1 1 d . . .
H2NA H 1.179(5) 0.196(4) 0.054(4) 0.055(15) Uiso 1 1 d . . .
H2NB H 1.060(7) 0.111(5) 0.084(5) 0.11(2) Uiso 1 1 d . . .
H2NC H 1.150(6) 0.069(6) 0.030(5) 0.11(2) Uiso 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0342(15) 0.0308(16) 0.0337(16) 0.0090(13) 0.0230(13) 0.0181(13)
C1 0.0167(18) 0.029(2) 0.022(2) 0.0040(17) 0.0056(17) 0.0099(16)
O2 0.0256(14) 0.0325(16) 0.0283(15) 0.0080(12) 0.0120(12) 0.0120(12)
C2 0.0185(18) 0.025(2) 0.025(2) 0.0050(17) 0.0061(17) 0.0097(16)
O3 0.0302(14) 0.0305(16) 0.0314(16) 0.0063(12) 0.0117(13) 0.0182(13)
C3 0.0221(19) 0.022(2) 0.031(2) 0.0096(17) 0.0070(18) 0.0094(17)
O4 0.0263(14) 0.0356(16) 0.0307(16) 0.0064(13) 0.0056(13) 0.0190(13)
C4 0.027(2) 0.018(2) 0.031(2) 0.0049(17) 0.0083(18) 0.0110(17)
C5 0.024(2) 0.025(2) 0.033(2) 0.0035(18) 0.0042(19) 0.0138(18)
C6 0.037(2) 0.037(2) 0.025(2) 0.0110(19) 0.0140(19) 0.022(2)
C7 0.040(2) 0.033(2) 0.033(2) 0.0130(19) 0.021(2) 0.020(2)
C8 0.032(2) 0.028(2) 0.035(2) 0.0097(19) 0.0171(19) 0.0166(19)
C9 0.0233(19) 0.032(2) 0.024(2) 0.0115(18) 0.0108(18) 0.0129(17)
C10 0.0229(19) 0.025(2) 0.025(2) 0.0102(17) 0.0127(17) 0.0109(17)
C11 0.025(2) 0.027(2) 0.025(2) 0.0082(17) 0.0079(17) 0.0100(17)
C12 0.0197(18) 0.029(2) 0.0166(19) 0.0043(16) 0.0062(16) 0.0123(17)
C16 0.030(2) 0.026(2) 0.036(2) 0.0091(19) 0.011(2) 0.0106(18)
C17 0.025(2) 0.030(2) 0.044(3) 0.006(2) 0.001(2) 0.0086(19)
C18 0.036(2) 0.027(2) 0.036(3) -0.001(2) -0.001(2) 0.013(2)
C19 0.037(2) 0.032(2) 0.031(2) 0.0043(19) 0.008(2) 0.021(2)
C20 0.035(2) 0.028(2) 0.025(2) 0.0070(18) 0.0081(19) 0.0115(19)
C21 0.030(2) 0.033(3) 0.030(2) 0.007(2) -0.001(2) 0.007(2)
C22 0.031(2) 0.036(3) 0.032(2) 0.013(2) 0.002(2) 0.013(2)
C23 0.031(2) 0.029(2) 0.034(2) 0.0125(19) 0.016(2) 0.0154(19)
C24 0.022(2) 0.037(2) 0.023(2) 0.0046(18) 0.0099(17) 0.0114(18)
C25 0.024(2) 0.042(3) 0.030(2) -0.001(2) 0.0107(19) 0.0163(19)
C26 0.023(2) 0.025(2) 0.036(2) -0.0002(18) 0.0068(19) 0.0135(18)
O1' 0.0260(14) 0.0350(17) 0.0274(15) 0.0166(13) 0.0096(12) 0.0169(13)
C1' 0.027(2) 0.022(2) 0.0195(19) 0.0065(16) 0.0089(17) 0.0143(17)
O2' 0.0309(14) 0.0301(16) 0.0235(14) 0.0095(12) 0.0135(12) 0.0126(13)
C2' 0.0236(19) 0.021(2) 0.022(2) 0.0041(16) 0.0079(17) 0.0118(16)
C3' 0.0213(19) 0.026(2) 0.024(2) 0.0054(17) 0.0085(17) 0.0122(16)
C4' 0.0203(18) 0.029(2) 0.025(2) 0.0096(17) 0.0092(17) 0.0158(17)
C5' 0.0232(19) 0.026(2) 0.030(2) 0.0096(18) 0.0141(18) 0.0145(17)
C6' 0.030(2) 0.043(3) 0.027(2) 0.0182(19) 0.0189(19) 0.021(2)
C7' 0.025(2) 0.042(3) 0.033(2) 0.015(2) 0.0157(19) 0.0198(19)
C8' 0.022(2) 0.034(2) 0.031(2) 0.0121(19) 0.0077(18) 0.0139(18)
C9' 0.027(2) 0.029(2) 0.028(2) 0.0118(18) 0.0155(19) 0.0168(18)
C10' 0.0239(19) 0.022(2) 0.026(2) 0.0107(17) 0.0144(17) 0.0093(16)
C11' 0.027(2) 0.026(2) 0.030(2) 0.0108(17) 0.0149(18) 0.0138(17)
C12' 0.027(2) 0.023(2) 0.020(2) 0.0049(16) 0.0083(17) 0.0136(17)
C13' 0.035(2) 0.024(2) 0.025(2) 0.0074(17) 0.0156(19) 0.0148(18)
C14' 0.035(2) 0.028(2) 0.022(2) 0.0088(17) 0.0091(18) 0.0197(19)
C15' 0.028(2) 0.024(2) 0.022(2) 0.0032(17) 0.0083(18) 0.0152(17)
C16' 0.037(2) 0.030(2) 0.035(2) 0.0128(19) 0.023(2) 0.017(2)
C17' 0.037(2) 0.027(2) 0.040(3) 0.002(2) 0.021(2) 0.0118(19)
C18' 0.032(2) 0.033(2) 0.031(2) -0.0020(19) 0.0138(19) 0.015(2)
C19' 0.032(2) 0.038(3) 0.027(2) 0.0076(19) 0.0158(19) 0.021(2)
C20' 0.025(2) 0.036(2) 0.032(2) 0.010(2) 0.0104(19) 0.0116(19)
C21' 0.036(2) 0.025(2) 0.034(2) 0.0052(19) 0.015(2) 0.0077(19)
C22' 0.035(2) 0.025(2) 0.041(3) 0.0100(19) 0.018(2) 0.0142(19)
C23' 0.028(2) 0.026(2) 0.035(2) 0.0137(19) 0.0143(19) 0.0128(18)
N1 0.049(2) 0.040(2) 0.045(3) 0.0164(19) 0.029(2) 0.024(2)
C1G 0.043(3) 0.052(3) 0.078(4) 0.035(3) 0.028(3) 0.025(3)
C2G 0.041(3) 0.035(3) 0.068(4) 0.004(2) 0.012(3) 0.018(2)
C3G 0.037(3) 0.054(3) 0.073(4) -0.008(3) 0.030(3) 0.010(2)
N2 0.052(3) 0.031(2) 0.069(3) 0.001(2) 0.046(3) 0.010(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 C1 1.330(4) . ?
C1 C2 1.412(5) . ?
C1 C12 1.415(5) . ?
O2 C5 1.377(4) . ?
O2 C6 1.428(4) . ?
C2 C26 1.376(5) . ?
C2 C3 1.512(5) . ?
O3 C9 1.374(4) . ?
O3 C8 1.438(4) . ?
C3 C4 1.516(5) . ?
O4 C9' 1.377(4) . ?
O4 C8' 1.432(4) . ?
C4 C5 1.388(6) . ?
C4 C16 1.400(5) . ?
C5 C19 1.400(5) . ?
C6 C7 1.509(5) . ?
C7 C8 1.506(5) 2_755 ?
C8 C7 1.506(5) 2_755 ?
C9 C20 1.396(5) . ?
C9 C10 1.397(5) . ?
C10 C23 1.389(5) . ?
C10 C11 1.524(5) . ?
C11 C12 1.496(5) . ?
C12 C24 1.390(5) . ?
C16 C17 1.395(6) . ?
C17 C18 1.369(6) . ?
C18 C19 1.388(6) . ?
C20 C21 1.386(6) . ?
C21 C22 1.381(6) . ?
C22 C23 1.385(5) . ?
C24 C25 1.377(6) . ?
C25 C26 1.393(6) . ?
O1' C1' 1.362(4) . ?
C1' C2' 1.406(5) . ?
C1' C12' 1.408(5) . ?
O2' C5' 1.375(4) . ?
O2' C6' 1.440(4) . ?
C2' C15' 1.388(5) . ?
C2' C3' 1.508(5) . ?
C3' C4' 1.520(5) . ?
C4' C16' 1.382(5) . ?
C4' C5' 1.413(5) . ?
C5' C19' 1.389(5) . ?
C6' C7' 1.506(5) . ?
C7' C8' 1.506(5) 2_866 ?
C8' C7' 1.506(5) 2_866 ?
C9' C20' 1.390(5) . ?
C9' C10' 1.396(5) . ?
C10' C23' 1.388(5) . ?
C10' C11' 1.529(5) . ?
C11' C12' 1.495(5) . ?
C12' C13' 1.383(5) . ?
C13' C14' 1.384(5) . ?
C14' C15' 1.373(5) . ?
C16' C17' 1.381(6) . ?
C17' C18' 1.380(6) . ?
C18' C19' 1.385(6) . ?
C20' C21' 1.396(6) . ?
C21' C22' 1.381(6) . ?
C22' C23' 1.396(5) . ?
N1 C1G 1.481(6) . ?
C1G C2G 1.482(7) . ?
C2G C3G 1.561(7) . ?
C3G N2 1.464(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 120.7(3) . . ?
O1 C1 C12 120.3(3) . . ?
C2 C1 C12 119.0(3) . . ?
C5 O2 C6 117.5(3) . . ?
C26 C2 C1 120.0(4) . . ?
C26 C2 C3 121.1(3) . . ?
C1 C2 C3 118.3(3) . . ?
C9 O3 C8 117.7(3) . . ?
C2 C3 C4 111.9(3) . . ?
C9' O4 C8' 117.2(3) . . ?
C5 C4 C16 118.1(4) . . ?
C5 C4 C3 120.8(3) . . ?
C16 C4 C3 121.0(4) . . ?
O2 C5 C4 115.7(3) . . ?
O2 C5 C19 123.0(4) . . ?
C4 C5 C19 121.3(4) . . ?
O2 C6 C7 108.0(3) . . ?
C8 C7 C6 114.1(3) 2_755 . ?
O3 C8 C7 107.8(3) . 2_755 ?
O3 C9 C20 123.4(4) . . ?
O3 C9 C10 114.9(3) . . ?
C20 C9 C10 121.7(3) . . ?
C23 C10 C9 117.2(3) . . ?
C23 C10 C11 122.6(3) . . ?
C9 C10 C11 120.1(3) . . ?
C12 C11 C10 113.8(3) . . ?
C24 C12 C1 118.6(4) . . ?
C24 C12 C11 121.8(3) . . ?
C1 C12 C11 119.3(3) . . ?
C17 C16 C4 120.7(4) . . ?
C18 C17 C16 120.0(4) . . ?
C17 C18 C19 120.8(4) . . ?
C18 C19 C5 118.9(4) . . ?
C21 C20 C9 118.7(4) . . ?
C22 C21 C20 121.0(4) . . ?
C21 C22 C23 119.1(4) . . ?
C22 C23 C10 122.2(4) . . ?
C25 C24 C12 122.4(4) . . ?
C24 C25 C26 118.6(4) . . ?
C2 C26 C25 121.3(4) . . ?
O1' C1' C2' 121.7(3) . . ?
O1' C1' C12' 117.0(3) . . ?
C2' C1' C12' 121.1(3) . . ?
C5' O2' C6' 116.5(3) . . ?
C15' C2' C1' 117.6(3) . . ?
C15' C2' C3' 121.2(3) . . ?
C1' C2' C3' 120.5(3) . . ?
C2' C3' C4' 111.4(3) . . ?
C16' C4' C5' 116.8(4) . . ?
C16' C4' C3' 121.3(3) . . ?
C5' C4' C3' 121.9(3) . . ?
O2' C5' C19' 123.7(3) . . ?
O2' C5' C4' 115.7(3) . . ?
C19' C5' C4' 120.6(4) . . ?
O2' C6' C7' 108.5(3) . . ?
C6' C7' C8' 114.4(3) . 2_866 ?
O4 C8' C7' 106.9(3) . 2_866 ?
O4 C9' C20' 123.6(3) . . ?
O4 C9' C10' 115.3(3) . . ?
C20' C9' C10' 121.1(4) . . ?
C23' C10' C9' 117.9(4) . . ?
C23' C10' C11' 122.0(3) . . ?
C9' C10' C11' 120.2(3) . . ?
C12' C11' C10' 113.7(3) . . ?
C13' C12' C1' 118.3(3) . . ?
C13' C12' C11' 122.1(3) . . ?
C1' C12' C11' 119.5(3) . . ?
C12' C13' C14' 121.1(4) . . ?
C15' C14' C13' 119.7(3) . . ?
C14' C15' C2' 121.9(3) . . ?
C17' C16' C4' 123.1(4) . . ?
C18' C17' C16' 119.0(4) . . ?
C17' C18' C19' 120.1(4) . . ?
C18' C19' C5' 120.2(4) . . ?
C9' C20' C21' 119.9(4) . . ?
C22' C21' C20' 119.7(4) . . ?
C21' C22' C23' 119.7(4) . . ?
C10' C23' C22' 121.6(4) . . ?
N1 C1G C2G 107.5(4) . . ?
C1G C2G C3G 110.9(4) . . ?
N2 C3G C2G 108.1(4) . . ?

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
O1 C1 C2 C26 -180.0(3) . . . . ?
C12 C1 C2 C26 2.2(5) . . . . ?
O1 C1 C2 C3 8.2(5) . . . . ?
C12 C1 C2 C3 -169.6(3) . . . . ?
C26 C2 C3 C4 -103.4(4) . . . . ?
C1 C2 C3 C4 68.4(4) . . . . ?
C2 C3 C4 C5 -160.5(3) . . . . ?
C2 C3 C4 C16 22.5(5) . . . . ?
C6 O2 C5 C4 -179.0(3) . . . . ?
C6 O2 C5 C19 -0.1(5) . . . . ?
C16 C4 C5 O2 174.9(3) . . . . ?
C3 C4 C5 O2 -2.1(5) . . . . ?
C16 C4 C5 C19 -4.1(6) . . . . ?
C3 C4 C5 C19 178.9(3) . . . . ?
C5 O2 C6 C7 169.8(3) . . . . ?
O2 C6 C7 C8 51.5(4) . . . 2_755 ?
C9 O3 C8 C7 -175.3(3) . . . 2_755 ?
C8 O3 C9 C20 6.1(5) . . . . ?
C8 O3 C9 C10 -172.9(3) . . . . ?
O3 C9 C10 C23 -178.0(3) . . . . ?
C20 C9 C10 C23 3.0(6) . . . . ?
O3 C9 C10 C11 2.5(5) . . . . ?
C20 C9 C10 C11 -176.6(4) . . . . ?
C23 C10 C11 C12 -12.5(5) . . . . ?
C9 C10 C11 C12 167.0(3) . . . . ?
O1 C1 C12 C24 -179.3(3) . . . . ?
C2 C1 C12 C24 -1.5(5) . . . . ?
O1 C1 C12 C11 -4.3(5) . . . . ?
C2 C1 C12 C11 173.5(3) . . . . ?
C10 C11 C12 C24 98.9(4) . . . . ?
C10 C11 C12 C1 -75.9(4) . . . . ?
C5 C4 C16 C17 1.3(6) . . . . ?
C3 C4 C16 C17 178.3(4) . . . . ?
C4 C16 C17 C18 2.0(6) . . . . ?
C16 C17 C18 C19 -2.6(6) . . . . ?
C17 C18 C19 C5 -0.2(6) . . . . ?
O2 C5 C19 C18 -175.4(4) . . . . ?
C4 C5 C19 C18 3.6(6) . . . . ?
O3 C9 C20 C21 178.2(4) . . . . ?
C10 C9 C20 C21 -2.8(6) . . . . ?
C9 C20 C21 C22 0.2(6) . . . . ?
C20 C21 C22 C23 2.0(7) . . . . ?
C21 C22 C23 C10 -1.8(6) . . . . ?
C9 C10 C23 C22 -0.7(6) . . . . ?
C11 C10 C23 C22 178.9(4) . . . . ?
C1 C12 C24 C25 -0.3(5) . . . . ?
C11 C12 C24 C25 -175.2(3) . . . . ?
C12 C24 C25 C26 1.4(5) . . . . ?
C1 C2 C26 C25 -1.2(5) . . . . ?
C3 C2 C26 C25 170.5(3) . . . . ?
C24 C25 C26 C2 -0.6(5) . . . . ?
O1' C1' C2' C15' -179.6(3) . . . . ?
C12' C1' C2' C15' 5.4(5) . . . . ?
O1' C1' C2' C3' 9.3(5) . . . . ?
C12' C1' C2' C3' -165.7(3) . . . . ?
C15' C2' C3' C4' -111.7(4) . . . . ?
C1' C2' C3' C4' 59.2(4) . . . . ?
C2' C3' C4' C16' 20.9(5) . . . . ?
C2' C3' C4' C5' -157.7(3) . . . . ?
C6' O2' C5' C19' 2.4(5) . . . . ?
C6' O2' C5' C4' -178.3(3) . . . . ?
C16' C4' C5' O2' 176.3(3) . . . . ?
C3' C4' C5' O2' -5.0(5) . . . . ?
C16' C4' C5' C19' -4.5(5) . . . . ?
C3' C4' C5' C19' 174.3(3) . . . . ?
C5' O2' C6' C7' 177.5(3) . . . . ?
O2' C6' C7' C8' 61.5(4) . . . 2_866 ?
C9' O4 C8' C7' -178.3(3) . . . 2_866 ?
C8' O4 C9' C20' 8.9(5) . . . . ?
C8' O4 C9' C10' -170.7(3) . . . . ?
O4 C9' C10' C23' -177.5(3) . . . . ?
C20' C9' C10' C23' 2.8(5) . . . . ?
O4 C9' C10' C11' 2.4(5) . . . . ?
C20' C9' C10' C11' -177.3(4) . . . . ?
C23' C10' C11' C12' -16.9(5) . . . . ?
C9' C10' C11' C12' 163.2(3) . . . . ?
O1' C1' C12' C13' 179.9(3) . . . . ?
C2' C1' C12' C13' -4.9(5) . . . . ?
O1' C1' C12' C11' -5.1(5) . . . . ?
C2' C1' C12' C11' 170.1(3) . . . . ?
C10' C11' C12' C13' 95.8(4) . . . . ?
C10' C11' C12' C1' -79.0(4) . . . . ?
C1' C12' C13' C14' 1.2(5) . . . . ?
C11' C12' C13' C14' -173.7(3) . . . . ?
C12' C13' C14' C15' 1.9(6) . . . . ?
C13' C14' C15' C2' -1.3(6) . . . . ?
C1' C2' C15' C14' -2.3(5) . . . . ?
C3' C2' C15' C14' 168.7(3) . . . . ?
C5' C4' C16' C17' 3.6(6) . . . . ?
C3' C4' C16' C17' -175.1(4) . . . . ?
C4' C16' C17' C18' -0.4(6) . . . . ?
C16' C17' C18' C19' -2.2(6) . . . . ?
C17' C18' C19' C5' 1.3(6) . . . . ?
O2' C5' C19' C18' -178.7(3) . . . . ?
C4' C5' C19' C18' 2.1(6) . . . . ?
O4 C9' C20' C21' 178.5(4) . . . . ?
C10' C9' C20' C21' -1.9(6) . . . . ?
C9' C20' C21' C22' -0.5(6) . . . . ?
C20' C21' C22' C23' 2.0(6) . . . . ?
C9' C10' C23' C22' -1.4(6) . . . . ?
C11' C10' C23' C22' 178.7(4) . . . . ?
C21' C22' C23' C10' -1.0(6) . . . . ?
N1 C1G C2G C3G -178.1(4) . . . . ?
C1G C2G C3G N2 -176.1(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2NB O1 1.11(7) 1.53(7) 2.603(5) 160(5) .
O1' H1'O N1 0.95(6) 1.70(6) 2.640(5) 166(5) .
N1 H1NB O1' 0.96(6) 2.07(6) 2.966(5) 154(5) 2_866
N2 H2NC O1 1.06(7) 1.61(7) 2.621(5) 157(5) 2_755

_diffrn_measured_fraction_theta_max 0.976
_diffrn_reflns_theta_full        25.71
_diffrn_measured_fraction_theta_full 0.976
_refine_diff_density_max         0.658
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.062

# Attachment '2d.cif'

data_2d
_database_code_depnum_ccdc_archive 'CCDC 641525'
#TrackingRef '2d.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
(3,4:10,11:19,20:26,27-tetrabenzo-5,9,21,25-tetraoxa-tricyclo[27.3.1.113,17]
tetratriaconta-1(32),3,10,13,15,17(34),19,26,29(33),30-decaene-33,34-diol)
di-ethylenediamine salt
;
_chemical_name_common            
;
(3,4:10,11:19,20:26,27-tetrabenzo-5,9,21,25-tetraoxa-
tricyclo(27.3.1.113,17) tetratriaconta-
1(32),3,10,13,15,17(34),19,26,29(33),30-decaene-33,34-diol) di-
ethylenediamine salt
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H42 O6,C2 H9 N2,C2 H9 N2'
_chemical_formula_sum            'C50 H60 N4 O6'
_chemical_formula_weight         813.02

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

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_space_group_name_Hall           '-P 1'
_space_group_id                  2

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

_cell_length_a                   11.610(2)
_cell_length_b                   11.669(2)
_cell_length_c                   18.732(4)
_cell_angle_alpha                78.05(3)
_cell_angle_beta                 82.69(3)
_cell_angle_gamma                60.57(3)
_cell_volume                     2161.5(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)

_exptl_crystal_description       needles
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
__exptl_crystal_density_diffrn   1.249
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             872
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_type   none

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(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  'Enraf Nonius Kappa CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_number            35285
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_sigmaI/netI    0.0471
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.15
_diffrn_reflns_theta_max         29.05
_reflns_number_total             11323
_reflns_number_gt                10149
_reflns_threshold_expression     >2sigma(I)

_computing_cell_refinement       'Nonius collect'
_computing_data_reduction        'Nonius collect'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-seed
_computing_publication_material  ciftab

_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.
One ethylenediamine molecule exhibited disorder of the non-hydrogen bonded
amine group and associated methylene group, which was modeled over two
positions with sofs refined as x and 1-x; x refined to 0.62 over many cycles.
The CH2 group beta to the disordered amine group was similarly refined over
two positions to allow for rotational disorder, but a common carbon atom
position was maintained by use of appropriate EADP and EXYZ cards. All
non-hydrogen atoms were refined anisotropically and most hydrogen atoms were
refined using a riding model. The positions of hydrogen atoms of hydrogen
bonded NH2/NH3+ and OH/O- groups were located in electron density difference
maps and these atoms were refined without restraints. Similarly, non-
hydrogen bonded amine group hydrogen atoms were located and refined without
restraint, except those of disordered N1, which were generated geometrically
using HFIX 137 with the vacant position assigned an sof of zero (as
kindly suggested by a referee).
;

_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^)+(0.0353P)^2^+2.3624P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11323
_refine_ls_number_parameters     588
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0980
_refine_ls_R_factor_gt           0.0881
_refine_ls_wR_factor_ref         0.1704
_refine_ls_wR_factor_gt          0.1657
_refine_ls_goodness_of_fit_ref   1.252
_refine_ls_restrained_S_all      1.252
_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 0.08475(15) 0.56921(15) 0.04315(8) 0.0187(3) Uani 1 1 d . . .
C1 C 0.1255(2) 0.6480(2) 0.06026(11) 0.0151(4) Uani 1 1 d . . .
O2 O 0.12862(17) 0.68774(17) -0.20858(9) 0.0251(4) Uani 1 1 d . . .
C2 C 0.1419(2) 0.7442(2) 0.00637(12) 0.0179(4) Uani 1 1 d . . .
O3 O 0.15303(17) 0.28357(16) 0.24577(9) 0.0244(4) Uani 1 1 d . . .
C3 C 0.1312(2) 0.7436(2) -0.07292(12) 0.0215(5) Uani 1 1 d . . .
H3A H 0.1324 0.8236 -0.1028 0.026 Uiso 1 1 calc R . .
H3B H 0.0453 0.7493 -0.0798 0.026 Uiso 1 1 calc R . .
C4 C 0.2423(2) 0.6195(2) -0.10005(12) 0.0197(4) Uani 1 1 d . . .
C5 C 0.2335(2) 0.5910(2) -0.16792(12) 0.0220(5) Uani 1 1 d . . .
C6 C 0.1129(2) 0.6608(3) -0.27747(12) 0.0239(5) Uani 1 1 d . . .
H6A H 0.0963 0.5836 -0.2695 0.029 Uiso 1 1 calc R . .
H6B H 0.1940 0.6401 -0.3086 0.029 Uiso 1 1 calc R . .
C7 C 0.0033(3) 0.2156(3) 0.31374(13) 0.0263(5) Uani 1 1 d . . .
H7A H -0.0192 0.1420 0.3254 0.032 Uiso 1 1 calc R . .
H7B H 0.0180 0.2329 0.3604 0.032 Uiso 1 1 calc R . .
H4NB H 0.1364 0.4652 -0.0080 0.055(10) Uiso 1 1 d R . .
C8 C 0.1305(3) 0.1705(2) 0.26850(13) 0.0253(5) Uani 1 1 d . . .
H8A H 0.2049 0.0970 0.2978 0.030 Uiso 1 1 calc R . .
H8B H 0.1232 0.1380 0.2254 0.030 Uiso 1 1 calc R . .
C9 C 0.2655(2) 0.2660(2) 0.20468(12) 0.0211(5) Uani 1 1 d . . .
C10 C 0.2728(2) 0.3833(2) 0.17538(11) 0.0184(4) Uani 1 1 d . . .
C11 C 0.1587(2) 0.5184(2) 0.18823(12) 0.0193(4) Uani 1 1 d . . .
H11C H 0.0741 0.5180 0.1862 0.023 Uiso 1 1 calc R . .
H11D H 0.1646 0.5319 0.2378 0.023 Uiso 1 1 calc R . .
C12 C 0.1575(2) 0.6339(2) 0.13336(11) 0.0163(4) Uani 1 1 d . . .
C13 C 0.1918(2) 0.7227(2) 0.15137(12) 0.0196(4) Uani 1 1 d . . .
H13 H 0.2114 0.7142 0.2005 0.024 Uiso 1 1 calc R . .
C14 C 0.1985(2) 0.8236(2) 0.09961(13) 0.0237(5) Uani 1 1 d . . .
H14 H 0.2183 0.8857 0.1135 0.028 Uiso 1 1 calc R . .
C15 C 0.1755(2) 0.8321(2) 0.02725(13) 0.0219(5) Uani 1 1 d . . .
H15 H 0.1828 0.8988 -0.0088 0.026 Uiso 1 1 calc R . .
C16 C 0.3518(2) 0.5278(2) -0.05838(12) 0.0214(5) Uani 1 1 d . . .
H16 H 0.3612 0.5464 -0.0131 0.026 Uiso 1 1 calc R . .
C17 C 0.4481(2) 0.4096(3) -0.08108(13) 0.0269(5) Uani 1 1 d . . .
H17 H 0.5224 0.3494 -0.0519 0.032 Uiso 1 1 calc R . .
C18 C 0.4343(3) 0.3809(3) -0.14639(14) 0.0286(5) Uani 1 1 d . . .
H18 H 0.4980 0.2991 -0.1615 0.034 Uiso 1 1 calc R . .
C19 C 0.3274(3) 0.4713(3) -0.19037(13) 0.0272(5) Uani 1 1 d . . .
H19 H 0.3186 0.4515 -0.2354 0.033 Uiso 1 1 calc R . .
C20 C 0.3679(3) 0.1414(2) 0.19297(14) 0.0268(5) Uani 1 1 d . . .
H20 H 0.3610 0.0630 0.2124 0.032 Uiso 1 1 calc R . .
C21 C 0.4806(2) 0.1327(3) 0.15259(14) 0.0278(5) Uani 1 1 d . . .
H21 H 0.5507 0.0480 0.1445 0.033 Uiso 1 1 calc R . .
C22 C 0.4909(2) 0.2466(3) 0.12424(13) 0.0255(5) Uani 1 1 d . . .
H22 H 0.5681 0.2404 0.0971 0.031 Uiso 1 1 calc R . .
C23 C 0.3869(2) 0.3708(2) 0.13584(12) 0.0212(5) Uani 1 1 d . . .
H23 H 0.3944 0.4488 0.1162 0.025 Uiso 1 1 calc R . .
O1' O 0.44839(16) 0.88665(17) 0.45956(9) 0.0215(3) Uani 1 1 d . . .
C1' C 0.3786(2) 0.8610(2) 0.42151(11) 0.0158(4) Uani 1 1 d . . .
O2' O 0.79660(16) 0.81160(17) 0.29002(9) 0.0255(4) Uani 1 1 d . . .
C2' C 0.4203(2) 0.8340(2) 0.34893(11) 0.0157(4) Uani 1 1 d . . .
O3' O 0.24177(16) 0.90484(18) 0.67212(9) 0.0248(4) Uani 1 1 d . . .
C3' C 0.5498(2) 0.8281(2) 0.31786(12) 0.0173(4) Uani 1 1 d . . .
H3'1 H 0.5485 0.9117 0.3227 0.021 Uiso 1 1 calc R . .
H3'2 H 0.5561 0.8243 0.2651 0.021 Uiso 1 1 calc R . .
C4' C 0.6730(2) 0.7105(2) 0.35386(12) 0.0170(4) Uani 1 1 d . . .
C5' C 0.7971(2) 0.7047(2) 0.33847(12) 0.0199(4) Uani 1 1 d . . .
C6' C 0.9112(2) 0.8287(2) 0.28867(13) 0.0232(5) Uani 1 1 d . . .
H6'1 H 0.9900 0.7524 0.2713 0.028 Uiso 1 1 calc R . .
H6'2 H 0.9276 0.8333 0.3383 0.028 Uiso 1 1 calc R . .
C7' C 0.1147(2) 1.0430(2) 0.76235(12) 0.0212(5) Uani 1 1 d . . .
H7'1 H 0.1165 1.0553 0.8129 0.025 Uiso 1 1 calc R . .
H7'2 H 0.0400 1.0257 0.7601 0.025 Uiso 1 1 calc R . .
C8' C 0.2417(2) 0.9220(2) 0.74630(12) 0.0216(5) Uani 1 1 d . . .
H8'1 H 0.3183 0.9339 0.7528 0.026 Uiso 1 1 calc R . .
H8'2 H 0.2493 0.8418 0.7806 0.026 Uiso 1 1 calc R . .
C9' C 0.3385(2) 0.7843(2) 0.65385(12) 0.0212(5) Uani 1 1 d . . .
C10' C 0.3334(2) 0.7619(2) 0.58399(12) 0.0189(4) Uani 1 1 d . . .
C11' C 0.2262(2) 0.8666(2) 0.53167(12) 0.0200(4) Uani 1 1 d . . .
H11A H 0.1446 0.8586 0.5440 0.024 Uiso 1 1 calc R . .
H11B H 0.2061 0.9563 0.5389 0.024 Uiso 1 1 calc R . .
C12' C 0.2630(2) 0.8550(2) 0.45243(11) 0.0172(4) Uani 1 1 d . . .
C13' C 0.1884(2) 0.8330(2) 0.40974(12) 0.0197(4) Uani 1 1 d . . .
H13' H 0.1100 0.8312 0.4303 0.024 Uiso 1 1 calc R . .
C14' C 0.2253(2) 0.8137(2) 0.33803(13) 0.0220(5) Uani 1 1 d . . .
H14' H 0.1714 0.8019 0.3092 0.026 Uiso 1 1 calc R . .
C15' C 0.3421(2) 0.8120(2) 0.30895(12) 0.0194(4) Uani 1 1 d . . .
H15' H 0.3693 0.7953 0.2605 0.023 Uiso 1 1 calc R . .
C16' C 0.6683(2) 0.6064(2) 0.40344(13) 0.0236(5) Uani 1 1 d . . .
H16' H 0.5857 0.6075 0.4148 0.028 Uiso 1 1 calc R . .
C17' C 0.7812(3) 0.5006(2) 0.43709(14) 0.0280(5) Uani 1 1 d . . .
H17' H 0.7750 0.4310 0.4711 0.034 Uiso 1 1 calc R . .
C18' C 0.9014(2) 0.4971(2) 0.42095(13) 0.0258(5) Uani 1 1 d . . .
H18' H 0.9784 0.4253 0.4442 0.031 Uiso 1 1 calc R . .
C19' C 0.9108(2) 0.5978(3) 0.37095(13) 0.0259(5) Uani 1 1 d . . .
H19' H 0.9945 0.5940 0.3588 0.031 Uiso 1 1 calc R . .
C20' C 0.4367(2) 0.6886(3) 0.70144(13) 0.0285(5) Uani 1 1 d . . .
H20' H 0.4408 0.7061 0.7481 0.034 Uiso 1 1 calc R . .
C21' C 0.5292(2) 0.5668(3) 0.68059(14) 0.0269(5) Uani 1 1 d . . .
H21' H 0.5945 0.5005 0.7137 0.032 Uiso 1 1 calc R . .
C22' C 0.5259(3) 0.5427(2) 0.61192(14) 0.0257(5) Uani 1 1 d . . .
H22' H 0.5893 0.4605 0.5972 0.031 Uiso 1 1 calc R . .
C23' C 0.4287(3) 0.6402(2) 0.56469(13) 0.0232(5) Uani 1 1 d . . .
H23' H 0.4271 0.6233 0.5174 0.028 Uiso 1 1 calc R . .
N4 N 0.1633(2) 0.3819(2) -0.03576(11) 0.0218(4) Uani 1 1 d . . .
H4NA H 0.207(3) 0.391(3) -0.0776(17) 0.032(8) Uiso 1 1 d . . .
H4NC H 0.079(3) 0.396(3) -0.0473(17) 0.041(9) Uiso 1 1 d . . .
C1G C 0.2389(3) 0.2486(3) 0.00868(14) 0.0295(5) Uani 1 1 d . . .
H1GB H 0.1801 0.2328 0.0478 0.035 Uiso 1 1 calc R . .
H1GA H 0.3118 0.2467 0.0321 0.035 Uiso 1 1 calc R . .
C2G C 0.2966(3) 0.1372(3) -0.03703(17) 0.0367(6) Uani 1 1 d . . .
H2GB H 0.3641 0.1477 -0.0716 0.044 Uiso 1 1 calc R . .
H2GA H 0.3427 0.0509 -0.0040 0.044 Uiso 1 1 calc R . .
N5 N 0.2030(3) 0.1300(3) -0.07867(17) 0.0410(6) Uani 1 1 d . . .
H5NB H 0.126(5) 0.140(4) -0.049(2) 0.085(15) Uiso 1 1 d . . .
H5NA H 0.180(4) 0.212(4) -0.126(2) 0.082(14) Uiso 1 1 d . . .
N1 N 0.6073(6) 0.8336(7) 0.6162(4) 0.0390(19) Uani 0.385(7) 1 d P A 2
H1A H 0.6486 0.8631 0.6401 0.058 Uiso 0.385(7) 1 calc PR A 2
H1B H 0.5714 0.7902 0.6492 0.058 Uiso 0.385(7) 1 calc PR A 2
H1C H 0.5423 0.9045 0.5887 0.058 Uiso 0.00 1 calc PR A 2
C3GA C 0.7027(12) 0.7430(12) 0.5691(7) 0.042(3) Uiso 0.385(7) 1 d P A 2
H3GB H 0.7772 0.6710 0.5989 0.051 Uiso 0.385(7) 1 calc PR A 2
H3GD H 0.6601 0.7012 0.5493 0.051 Uiso 0.385(7) 1 calc PR A 2
C4GA C 0.7549(2) 0.8046(3) 0.50924(14) 0.0272(5) Uani 0.385(7) 1 d P A 2
H4GC H 0.8151 0.7357 0.4795 0.033 Uiso 0.385(7) 1 calc PR A 2
H4GD H 0.8090 0.8338 0.5295 0.033 Uiso 0.385(7) 1 calc PR A 2
N2 N 0.7735(3) 0.6449(4) 0.6199(2) 0.0274(10) Uani 0.615(7) 1 d P A 1
H2NA H 0.802(6) 0.665(6) 0.654(4) 0.061(19) Uiso 0.615(7) 1 d P A 1
H2NB H 0.729(6) 0.594(6) 0.650(3) 0.053(17) Uiso 0.615(7) 1 d P A 1
C3G C 0.6822(6) 0.7673(6) 0.5766(3) 0.0265(14) Uiso 0.615(7) 1 d P A 1
H3GA H 0.6420 0.8397 0.6062 0.032 Uiso 0.615(7) 1 calc PR A 1
H3GC H 0.6104 0.7563 0.5610 0.032 Uiso 0.615(7) 1 calc PR A 1
C4G C 0.7549(2) 0.8046(3) 0.50924(14) 0.0272(5) Uani 0.615(7) 1 d P A 1
H4GA H 0.8188 0.8271 0.5247 0.033 Uiso 0.615(7) 1 calc PR A 1
H4GB H 0.8047 0.7277 0.4831 0.033 Uiso 0.615(7) 1 calc PR A 1
N3 N 0.6576(2) 0.9211(2) 0.45965(12) 0.0265(4) Uani 1 1 d . . .
H3NC H 0.564(4) 0.920(4) 0.446(2) 0.075(13) Uiso 1 1 d . . .
H3NB H 0.697(4) 0.954(4) 0.406(2) 0.081(13) Uiso 1 1 d . . .
H3NA H 0.604(5) 1.028(6) 0.488(3) 0.127(19) Uiso 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0198(8) 0.0206(8) 0.0198(8) -0.0075(6) -0.0007(6) -0.0112(6)
C1 0.0141(9) 0.0137(9) 0.0160(9) -0.0049(7) -0.0004(7) -0.0047(8)
O2 0.0298(9) 0.0295(9) 0.0163(8) -0.0055(7) -0.0043(7) -0.0131(8)
C2 0.0179(10) 0.0176(10) 0.0173(10) -0.0037(8) -0.0003(8) -0.0076(8)
O3 0.0272(9) 0.0194(8) 0.0270(9) -0.0023(7) 0.0012(7) -0.0125(7)
C3 0.0250(12) 0.0214(11) 0.0158(10) -0.0023(8) -0.0015(8) -0.0094(9)
C4 0.0228(11) 0.0247(11) 0.0165(10) -0.0039(8) 0.0026(8) -0.0155(9)
C5 0.0240(11) 0.0289(12) 0.0180(10) -0.0038(9) 0.0000(9) -0.0166(10)
C6 0.0303(13) 0.0329(13) 0.0144(10) -0.0046(9) -0.0020(9) -0.0190(11)
C7 0.0386(14) 0.0310(13) 0.0172(11) 0.0009(9) -0.0051(10) -0.0236(12)
C8 0.0325(13) 0.0204(11) 0.0244(12) 0.0023(9) -0.0089(10) -0.0142(10)
C9 0.0230(11) 0.0215(11) 0.0171(10) -0.0018(8) -0.0058(8) -0.0087(9)
C10 0.0185(10) 0.0199(10) 0.0135(9) -0.0028(8) -0.0029(8) -0.0063(9)
C11 0.0212(11) 0.0177(10) 0.0149(10) -0.0024(8) 0.0012(8) -0.0067(9)
C12 0.0141(10) 0.0165(10) 0.0161(10) -0.0046(8) 0.0010(8) -0.0054(8)
C13 0.0194(11) 0.0226(11) 0.0173(10) -0.0101(8) -0.0007(8) -0.0079(9)
C14 0.0248(12) 0.0245(12) 0.0278(12) -0.0109(9) 0.0010(9) -0.0142(10)
C15 0.0244(11) 0.0179(11) 0.0239(11) -0.0035(9) 0.0026(9) -0.0111(9)
C16 0.0206(11) 0.0302(12) 0.0171(10) -0.0064(9) 0.0006(8) -0.0144(10)
C17 0.0162(11) 0.0362(14) 0.0242(12) -0.0074(10) 0.0009(9) -0.0089(10)
C18 0.0244(12) 0.0338(14) 0.0263(12) -0.0136(10) 0.0065(10) -0.0114(11)
C19 0.0310(13) 0.0354(14) 0.0187(11) -0.0107(10) 0.0035(9) -0.0171(11)
C20 0.0278(13) 0.0191(11) 0.0288(12) -0.0027(9) -0.0083(10) -0.0064(10)
C21 0.0218(12) 0.0250(12) 0.0278(12) -0.0102(10) -0.0080(9) -0.0008(10)
C22 0.0179(11) 0.0322(13) 0.0208(11) -0.0068(9) -0.0033(9) -0.0063(10)
C23 0.0196(11) 0.0254(12) 0.0165(10) -0.0032(8) -0.0028(8) -0.0089(9)
O1' 0.0242(8) 0.0303(9) 0.0200(8) -0.0093(7) 0.0000(6) -0.0189(7)
C1' 0.0185(10) 0.0155(10) 0.0153(9) -0.0022(7) -0.0022(8) -0.0094(8)
O2' 0.0187(8) 0.0301(9) 0.0281(9) 0.0066(7) -0.0035(7) -0.0157(7)
C2' 0.0156(10) 0.0145(9) 0.0162(10) -0.0028(7) -0.0013(8) -0.0064(8)
O3' 0.0192(8) 0.0350(10) 0.0182(8) -0.0127(7) -0.0008(6) -0.0084(7)
C3' 0.0162(10) 0.0170(10) 0.0178(10) -0.0029(8) 0.0002(8) -0.0074(8)
C4' 0.0168(10) 0.0164(10) 0.0188(10) -0.0073(8) 0.0009(8) -0.0075(8)
C5' 0.0192(11) 0.0213(11) 0.0179(10) -0.0022(8) 0.0015(8) -0.0095(9)
C6' 0.0166(11) 0.0315(13) 0.0243(11) -0.0057(9) 0.0024(9) -0.0139(10)
C7' 0.0221(11) 0.0289(12) 0.0194(10) -0.0098(9) 0.0057(8) -0.0167(10)
C8' 0.0240(11) 0.0304(12) 0.0153(10) -0.0089(9) 0.0016(8) -0.0153(10)
C9' 0.0167(10) 0.0278(12) 0.0217(11) -0.0097(9) 0.0017(8) -0.0110(9)
C10' 0.0223(11) 0.0257(11) 0.0177(10) -0.0053(8) 0.0011(8) -0.0179(10)
C11' 0.0217(11) 0.0256(11) 0.0176(10) -0.0079(9) 0.0026(8) -0.0143(9)
C12' 0.0186(10) 0.0192(10) 0.0164(10) -0.0054(8) 0.0005(8) -0.0103(9)
C13' 0.0152(10) 0.0233(11) 0.0230(11) -0.0064(9) 0.0010(8) -0.0105(9)
C14' 0.0184(11) 0.0292(12) 0.0230(11) -0.0096(9) -0.0042(9) -0.0121(9)
C15' 0.0187(10) 0.0211(11) 0.0169(10) -0.0068(8) -0.0020(8) -0.0069(9)
C16' 0.0195(11) 0.0204(11) 0.0304(12) -0.0019(9) -0.0009(9) -0.0100(9)
C17' 0.0289(13) 0.0186(11) 0.0332(13) 0.0003(10) -0.0023(10) -0.0104(10)
C18' 0.0208(11) 0.0185(11) 0.0282(12) -0.0011(9) -0.0045(9) -0.0022(9)
C19' 0.0168(11) 0.0302(13) 0.0278(12) -0.0049(10) 0.0006(9) -0.0094(10)
C20' 0.0244(12) 0.0379(14) 0.0211(11) -0.0098(10) -0.0020(9) -0.0113(11)
C21' 0.0240(12) 0.0295(13) 0.0256(12) -0.0004(10) -0.0043(9) -0.0123(10)
C22' 0.0302(13) 0.0186(11) 0.0292(12) -0.0059(9) 0.0017(10) -0.0122(10)
C23' 0.0343(13) 0.0217(11) 0.0198(11) -0.0058(9) 0.0015(9) -0.0176(10)
N4 0.0207(10) 0.0243(10) 0.0250(10) -0.0100(8) 0.0020(8) -0.0128(8)
C1G 0.0280(13) 0.0280(13) 0.0299(13) -0.0038(10) -0.0073(10) -0.0105(11)
C2G 0.0301(14) 0.0260(13) 0.0483(17) -0.0104(12) -0.0085(12) -0.0059(11)
N5 0.0383(14) 0.0303(13) 0.0584(17) -0.0184(12) -0.0064(13) -0.0141(11)
N1 0.035(4) 0.044(4) 0.042(4) -0.007(3) 0.002(3) -0.024(3)
C4GA 0.0224(12) 0.0256(12) 0.0260(12) -0.0024(10) -0.0019(9) -0.0063(10)
N2 0.0213(18) 0.0299(19) 0.0267(19) 0.0036(14) -0.0089(14) -0.0101(15)
C4G 0.0224(12) 0.0256(12) 0.0260(12) -0.0024(10) -0.0019(9) -0.0063(10)
N3 0.0233(10) 0.0290(11) 0.0274(11) -0.0034(9) -0.0023(8) -0.0129(9)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.327(3) . ?
C1 C2 1.417(3) . ?
C1 C12 1.420(3) . ?
O2 C5 1.366(3) . ?
O2 C6 1.442(3) . ?
C2 C15 1.398(3) . ?
C2 C3 1.508(3) . ?
O3 C9 1.373(3) . ?
O3 C8 1.438(3) . ?
C3 C4 1.524(3) . ?
C4 C16 1.393(3) . ?
C4 C5 1.406(3) . ?
C5 C19 1.395(3) . ?
C6 C7 1.509(4) 2_565 ?
C7 C6 1.509(4) 2_565 ?
C7 C8 1.509(4) . ?
C9 C20 1.394(3) . ?
C9 C10 1.405(3) . ?
C10 C23 1.390(3) . ?
C10 C11 1.524(3) . ?
C11 C12 1.511(3) . ?
C12 C13 1.390(3) . ?
C13 C14 1.389(3) . ?
C14 C15 1.389(3) . ?
C16 C17 1.392(3) . ?
C17 C18 1.381(3) . ?
C18 C19 1.395(4) . ?
C20 C21 1.393(4) . ?
C21 C22 1.383(4) . ?
C22 C23 1.396(3) . ?
O1' C1' 1.314(3) . ?
C1' C12' 1.422(3) . ?
C1' C2' 1.429(3) . ?
O2' C5' 1.381(3) . ?
O2' C6' 1.436(3) . ?
C2' C15' 1.391(3) . ?
C2' C3' 1.516(3) . ?
O3' C9' 1.381(3) . ?
O3' C8' 1.444(3) . ?
C3' C4' 1.522(3) . ?
C4' C16' 1.387(3) . ?
C4' C5' 1.404(3) . ?
C5' C19' 1.393(3) . ?
C6' C7' 1.511(3) 2_676 ?
C7' C8' 1.509(3) . ?
C7' C6' 1.511(3) 2_676 ?
C9' C20' 1.392(3) . ?
C9' C10' 1.400(3) . ?
C10' C23' 1.392(3) . ?
C10' C11' 1.524(3) . ?
C11' C12' 1.506(3) . ?
C12' C13' 1.391(3) . ?
C13' C14' 1.386(3) . ?
C14' C15' 1.388(3) . ?
C16' C17' 1.392(3) . ?
C17' C18' 1.372(4) . ?
C18' C19' 1.384(4) . ?
C20' C21' 1.395(4) . ?
C21' C22' 1.382(3) . ?
C22' C23' 1.388(3) . ?
N4 C1G 1.480(3) . ?
C1G C2G 1.527(4) . ?
C2G N5 1.460(4) . ?
N1 C3GA 1.452(13) . ?
C3GA C4GA 1.435(12) . ?
C4GA N3 1.491(3) . ?
N2 C3G 1.439(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 121.24(19) . . ?
O1 C1 C12 119.93(19) . . ?
C2 C1 C12 118.79(19) . . ?
C5 O2 C6 117.28(19) . . ?
C15 C2 C1 119.6(2) . . ?
C15 C2 C3 121.3(2) . . ?
C1 C2 C3 119.0(2) . . ?
C9 O3 C8 118.08(19) . . ?
C2 C3 C4 113.03(19) . . ?
C16 C4 C5 117.6(2) . . ?
C16 C4 C3 122.3(2) . . ?
C5 C4 C3 120.0(2) . . ?
O2 C5 C19 123.8(2) . . ?
O2 C5 C4 115.3(2) . . ?
C19 C5 C4 120.8(2) . . ?
O2 C6 C7 107.2(2) . 2_565 ?
C6 C7 C8 114.4(2) 2_565 . ?
O3 C8 C7 107.4(2) . . ?
O3 C9 C20 123.5(2) . . ?
O3 C9 C10 115.4(2) . . ?
C20 C9 C10 121.1(2) . . ?
C23 C10 C9 117.8(2) . . ?
C23 C10 C11 122.1(2) . . ?
C9 C10 C11 120.1(2) . . ?
C12 C11 C10 113.33(18) . . ?
C13 C12 C1 119.2(2) . . ?
C13 C12 C11 122.28(19) . . ?
C1 C12 C11 118.44(19) . . ?
C14 C13 C12 122.0(2) . . ?
C15 C14 C13 118.8(2) . . ?
C14 C15 C2 121.3(2) . . ?
C17 C16 C4 122.1(2) . . ?
C18 C17 C16 119.3(2) . . ?
C17 C18 C19 120.4(2) . . ?
C18 C19 C5 119.7(2) . . ?
C21 C20 C9 119.5(2) . . ?
C22 C21 C20 120.4(2) . . ?
C21 C22 C23 119.5(2) . . ?
C10 C23 C22 121.7(2) . . ?
O1' C1' C12' 120.82(19) . . ?
O1' C1' C2' 120.50(19) . . ?
C12' C1' C2' 118.64(19) . . ?
C5' O2' C6' 116.41(18) . . ?
C15' C2' C1' 119.3(2) . . ?
C15' C2' C3' 121.66(19) . . ?
C1' C2' C3' 119.07(19) . . ?
C9' O3' C8' 115.77(18) . . ?
C2' C3' C4' 114.81(18) . . ?
C16' C4' C5' 117.2(2) . . ?
C16' C4' C3' 122.4(2) . . ?
C5' C4' C3' 120.46(19) . . ?
O2' C5' C19' 123.6(2) . . ?
O2' C5' C4' 115.2(2) . . ?
C19' C5' C4' 121.2(2) . . ?
O2' C6' C7' 107.81(19) . 2_676 ?
C8' C7' C6' 114.86(19) . 2_676 ?
O3' C8' C7' 109.12(19) . . ?
O3' C9' C20' 122.8(2) . . ?
O3' C9' C10' 116.4(2) . . ?
C20' C9' C10' 120.8(2) . . ?
C23' C10' C9' 117.5(2) . . ?
C23' C10' C11' 121.5(2) . . ?
C9' C10' C11' 121.0(2) . . ?
C12' C11' C10' 113.93(19) . . ?
C13' C12' C1' 119.39(19) . . ?
C13' C12' C11' 120.9(2) . . ?
C1' C12' C11' 119.67(19) . . ?
C14' C13' C12' 121.8(2) . . ?
C13' C14' C15' 119.0(2) . . ?
C14' C15' C2' 121.7(2) . . ?
C4' C16' C17' 121.9(2) . . ?
C18' C17' C16' 119.8(2) . . ?
C17' C18' C19' 120.2(2) . . ?
C18' C19' C5' 119.7(2) . . ?
C9' C20' C21' 120.0(2) . . ?
C22' C21' C20' 120.1(2) . . ?
C21' C22' C23' 119.1(2) . . ?
C22' C23' C10' 122.4(2) . . ?
N4 C1G C2G 112.1(2) . . ?
N5 C2G C1G 116.4(2) . . ?
C4GA C3GA N1 114.5(8) . . ?
C3GA C4GA N3 117.1(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
O1 C1 C2 C15 175.3(2) . . . . ?
C12 C1 C2 C15 -6.7(3) . . . . ?
O1 C1 C2 C3 -8.6(3) . . . . ?
C12 C1 C2 C3 169.41(19) . . . . ?
C15 C2 C3 C4 109.5(2) . . . . ?
C1 C2 C3 C4 -66.5(3) . . . . ?
C2 C3 C4 C16 -9.1(3) . . . . ?
C2 C3 C4 C5 167.9(2) . . . . ?
C6 O2 C5 C19 2.2(3) . . . . ?
C6 O2 C5 C4 -177.8(2) . . . . ?
C16 C4 C5 O2 -176.2(2) . . . . ?
C3 C4 C5 O2 6.6(3) . . . . ?
C16 C4 C5 C19 3.7(3) . . . . ?
C3 C4 C5 C19 -173.4(2) . . . . ?
C5 O2 C6 C7 -176.56(19) . . . 2_565 ?
C9 O3 C8 C7 178.77(19) . . . . ?
C6 C7 C8 O3 52.2(3) 2_565 . . . ?
C8 O3 C9 C20 -9.8(3) . . . . ?
C8 O3 C9 C10 171.22(19) . . . . ?
O3 C9 C10 C23 177.40(19) . . . . ?
C20 C9 C10 C23 -1.6(3) . . . . ?
O3 C9 C10 C11 -1.8(3) . . . . ?
C20 C9 C10 C11 179.3(2) . . . . ?
C23 C10 C11 C12 21.5(3) . . . . ?
C9 C10 C11 C12 -159.3(2) . . . . ?
O1 C1 C12 C13 -175.90(19) . . . . ?
C2 C1 C12 C13 6.1(3) . . . . ?
O1 C1 C12 C11 6.7(3) . . . . ?
C2 C1 C12 C11 -171.33(19) . . . . ?
C10 C11 C12 C13 -107.4(2) . . . . ?
C10 C11 C12 C1 69.9(3) . . . . ?
C1 C12 C13 C14 -1.4(3) . . . . ?
C11 C12 C13 C14 175.9(2) . . . . ?
C12 C13 C14 C15 -2.8(3) . . . . ?
C13 C14 C15 C2 2.2(4) . . . . ?
C1 C2 C15 C14 2.6(3) . . . . ?
C3 C2 C15 C14 -173.4(2) . . . . ?
C5 C4 C16 C17 -2.0(3) . . . . ?
C3 C4 C16 C17 175.1(2) . . . . ?
C4 C16 C17 C18 -0.9(4) . . . . ?
C16 C17 C18 C19 2.1(4) . . . . ?
C17 C18 C19 C5 -0.4(4) . . . . ?
O2 C5 C19 C18 177.3(2) . . . . ?
C4 C5 C19 C18 -2.6(4) . . . . ?
O3 C9 C20 C21 -177.8(2) . . . . ?
C10 C9 C20 C21 1.1(3) . . . . ?
C9 C20 C21 C22 0.0(4) . . . . ?
C20 C21 C22 C23 -0.6(4) . . . . ?
C9 C10 C23 C22 1.0(3) . . . . ?
C11 C10 C23 C22 -179.9(2) . . . . ?
C21 C22 C23 C10 0.1(3) . . . . ?
O1' C1' C2' C15' -177.7(2) . . . . ?
C12' C1' C2' C15' 4.5(3) . . . . ?
O1' C1' C2' C3' 3.2(3) . . . . ?
C12' C1' C2' C3' -174.68(19) . . . . ?
C15' C2' C3' C4' -111.2(2) . . . . ?
C1' C2' C3' C4' 68.0(3) . . . . ?
C2' C3' C4' C16' 9.2(3) . . . . ?
C2' C3' C4' C5' -169.82(19) . . . . ?
C6' O2' C5' C19' -16.6(3) . . . . ?
C6' O2' C5' C4' 163.0(2) . . . . ?
C16' C4' C5' O2' -178.7(2) . . . . ?
C3' C4' C5' O2' 0.4(3) . . . . ?
C16' C4' C5' C19' 0.9(3) . . . . ?
C3' C4' C5' C19' 180.0(2) . . . . ?
C5' O2' C6' C7' -174.94(19) . . . 2_676 ?
C9' O3' C8' C7' -167.61(19) . . . . ?
C6' C7' C8' O3' -56.9(3) 2_676 . . . ?
C8' O3' C9' C20' -4.8(3) . . . . ?
C8' O3' C9' C10' 175.1(2) . . . . ?
O3' C9' C10' C23' -179.0(2) . . . . ?
C20' C9' C10' C23' 0.8(3) . . . . ?
O3' C9' C10' C11' 0.2(3) . . . . ?
C20' C9' C10' C11' -179.9(2) . . . . ?
C23' C10' C11' C12' -24.1(3) . . . . ?
C9' C10' C11' C12' 156.6(2) . . . . ?
O1' C1' C12' C13' 177.4(2) . . . . ?
C2' C1' C12' C13' -4.7(3) . . . . ?
O1' C1' C12' C11' -5.2(3) . . . . ?
C2' C1' C12' C11' 172.61(19) . . . . ?
C10' C11' C12' C13' 119.9(2) . . . . ?
C10' C11' C12' C1' -57.4(3) . . . . ?
C1' C12' C13' C14' 1.5(3) . . . . ?
C11' C12' C13' C14' -175.9(2) . . . . ?
C12' C13' C14' C15' 2.2(4) . . . . ?
C13' C14' C15' C2' -2.4(4) . . . . ?
C1' C2' C15' C14' -0.9(3) . . . . ?
C3' C2' C15' C14' 178.2(2) . . . . ?
C5' C4' C16' C17' 0.3(3) . . . . ?
C3' C4' C16' C17' -178.8(2) . . . . ?
C4' C16' C17' C18' -0.5(4) . . . . ?
C16' C17' C18' C19' -0.5(4) . . . . ?
C17' C18' C19' C5' 1.7(4) . . . . ?
O2' C5' C19' C18' 177.7(2) . . . . ?
C4' C5' C19' C18' -1.9(4) . . . . ?
O3' C9' C20' C21' 177.9(2) . . . . ?
C10' C9' C20' C21' -2.0(4) . . . . ?
C9' C20' C21' C22' 2.0(4) . . . . ?
C20' C21' C22' C23' -0.8(4) . . . . ?
C21' C22' C23' C10' -0.3(4) . . . . ?
C9' C10' C23' C22' 0.3(3) . . . . ?
C11' C10' C23' C22' -179.0(2) . . . . ?
N4 C1G C2G N5 -55.8(4) . . . . ?
N1 C3GA C4GA N3 -55.2(10) . . . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        29.05
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         1.337
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.057


# Attachment '2c.cif'

data_2c
_database_code_depnum_ccdc_archive 'CCDC 641526'
#TrackingRef '2c.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
(3,4:10,11:19,20:26,27-tetrabenzo-5,9,21,25-tetraoxa-tricyclo[27.3.1.113,17]
tetratriaconta-1(32),3,10,13,15,17(34),19,26,29(33),30-decaene-33,34-diol)
butylenediamine hemi-salt
;
_chemical_name_common            
;
(3,4:10,11:19,20:26,27-tetrabenzo-5,9,21,25-tetraoxa-
tricyclo(27.3.1.113,17) tetratriaconta-
1(32),3,10,13,15,17(34),19,26,29(33),30-decaene-33,34-diol)
butylenediamine hemi-salt
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H43 O6, C4 H13 N2'
_chemical_formula_sum            'C50 H56 N2 O6'
_chemical_formula_weight         780.97

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

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_space_group_name_Hall           '-P 1'
_space_group_id                  2

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

_cell_length_a                   12.7812(5)
_cell_length_b                   14.0559(5)
_cell_length_c                   14.2325(5)
_cell_angle_alpha                64.129(2)
_cell_angle_beta                 69.975(2)
_cell_angle_gamma                64.398(2)
_cell_volume                     2037.10(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)

_exptl_crystal_description       needles
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             836
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_type   none

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(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  'Enraf Nonius Kappa CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_number            26266
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_av_sigmaI/netI    0.0837
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.93
_diffrn_reflns_theta_max         30.09
_reflns_number_total             11755
_reflns_number_gt                6989
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Nonius collect'
_computing_cell_refinement       'Nonius collect'
_computing_data_reduction        'Nonius collect'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-seed
_computing_publication_material  ciftab

_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.
The butylenediamine molecule exhibits partial disorder of the alkyl chain
and C3G and C4G were modelled over two positions with sofs 0.65 and 0.35 for
the major and minor components respectively. Hydrogen atom positions for
the methylene group C2G were located in electron density difference maps and
were refined with strong bond length restraints. All non-hydrogen atoms were
refined anisotropically, most hydrogen atoms were refined using a riding
model, but the positions of hydrogen atoms of NH2/NH3+ and OH/O- groups were
located in electron density difference maps and these atoms were refined
without restraints.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0536P)^2^+0.2651P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11755
_refine_ls_number_parameters     547
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1132
_refine_ls_R_factor_gt           0.0579
_refine_ls_wR_factor_ref         0.1420
_refine_ls_wR_factor_gt          0.1182
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.016
_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 0.62765(11) 0.96161(10) 0.06426(9) 0.0251(3) Uani 1 1 d . . .
C1 C 0.70831(15) 0.91891(14) 0.12323(13) 0.0199(4) Uani 1 1 d . . .
O2 O 0.43985(11) 1.29158(10) 0.10142(9) 0.0258(3) Uani 1 1 d . . .
C2 C 0.70509(15) 0.97641(13) 0.18463(13) 0.0197(3) Uani 1 1 d . . .
O3 O 0.81208(11) 0.72165(10) -0.12282(9) 0.0272(3) Uani 1 1 d . . .
C3 C 0.61382(16) 1.09127(14) 0.17594(13) 0.0222(4) Uani 1 1 d . . .
H3A H 0.6113 1.1128 0.2345 0.027 Uiso 1 1 calc R . .
H3B H 0.5351 1.0879 0.1846 0.027 Uiso 1 1 calc R . .
C4 C 0.63881(16) 1.18073(14) 0.07045(13) 0.0213(4) Uani 1 1 d . . .
C5 C 0.54775(16) 1.28118(14) 0.03450(13) 0.0225(4) Uani 1 1 d . . .
C6 C 0.34537(16) 1.39362(14) 0.06695(14) 0.0253(4) Uani 1 1 d . . .
H6A H 0.3217 1.3954 0.0067 0.030 Uiso 1 1 calc R . .
H6B H 0.3713 1.4589 0.0429 0.030 Uiso 1 1 calc R . .
C7 C 0.75711(17) 0.60112(15) -0.15871(15) 0.0278(4) Uani 1 1 d . . .
H7A H 0.7339 0.5949 -0.2149 0.033 Uiso 1 1 calc R . .
H7B H 0.8236 0.5320 -0.1343 0.033 Uiso 1 1 calc R . .
C8 C 0.80022(17) 0.69989(15) -0.20702(14) 0.0268(4) Uani 1 1 d . . .
H8A H 0.8774 0.6829 -0.2555 0.032 Uiso 1 1 calc R . .
H8B H 0.7431 0.7666 -0.2485 0.032 Uiso 1 1 calc R . .
C9 C 0.86979(15) 0.79539(14) -0.14930(14) 0.0233(4) Uani 1 1 d . . .
C10 C 0.87351(15) 0.81696(14) -0.06368(14) 0.0231(4) Uani 1 1 d . . .
C11 C 0.81505(16) 0.76158(14) 0.04871(13) 0.0233(4) Uani 1 1 d . . .
H11A H 0.7362 0.7659 0.0473 0.028 Uiso 1 1 calc R . .
H11B H 0.8632 0.6813 0.0746 0.028 Uiso 1 1 calc R . .
C12 C 0.80151(15) 0.81610(14) 0.12436(13) 0.0209(4) Uani 1 1 d . . .
C13 C 0.88452(16) 0.77392(15) 0.18697(14) 0.0252(4) Uani 1 1 d . . .
H13 H 0.9457 0.7042 0.1885 0.030 Uiso 1 1 calc R . .
C14 C 0.88077(16) 0.83048(15) 0.24726(14) 0.0280(4) Uani 1 1 d . . .
H14 H 0.9389 0.8006 0.2893 0.034 Uiso 1 1 calc R . .
C15 C 0.79047(16) 0.93179(15) 0.24541(14) 0.0246(4) Uani 1 1 d . . .
H15 H 0.7873 0.9712 0.2867 0.030 Uiso 1 1 calc R . .
C16 C 0.75111(17) 1.16762(15) 0.00744(14) 0.0256(4) Uani 1 1 d . . .
H16 H 0.8141 1.1003 0.0304 0.031 Uiso 1 1 calc R . .
C17 C 0.77364(18) 1.25041(16) -0.08813(15) 0.0317(4) Uani 1 1 d . . .
H17 H 0.8513 1.2402 -0.1294 0.038 Uiso 1 1 calc R . .
C18 C 0.68204(19) 1.34776(16) -0.12253(15) 0.0330(5) Uani 1 1 d . . .
H18 H 0.6968 1.4044 -0.1882 0.040 Uiso 1 1 calc R . .
C19 C 0.56887(17) 1.36360(15) -0.06232(14) 0.0279(4) Uani 1 1 d . . .
H19 H 0.5060 1.4303 -0.0869 0.033 Uiso 1 1 calc R . .
C20 C 0.92006(16) 0.84671(15) -0.25260(15) 0.0287(4) Uani 1 1 d . . .
H20 H 0.9136 0.8339 -0.3103 0.034 Uiso 1 1 calc R . .
C21 C 0.97974(17) 0.91671(15) -0.27063(16) 0.0326(5) Uani 1 1 d . . .
H21 H 1.0159 0.9509 -0.3410 0.039 Uiso 1 1 calc R . .
C22 C 0.98737(17) 0.93740(16) -0.18782(17) 0.0344(5) Uani 1 1 d . . .
H22 H 1.0295 0.9847 -0.2006 0.041 Uiso 1 1 calc R . .
C23 C 0.93299(16) 0.88854(15) -0.08525(15) 0.0281(4) Uani 1 1 d . . .
H23 H 0.9367 0.9046 -0.0284 0.034 Uiso 1 1 calc R . .
O1' O 0.61317(11) 0.44318(11) 0.37085(10) 0.0252(3) Uani 1 1 d . . .
H1'O H 0.611(2) 0.498(2) 0.3860(18) 0.053(7) Uiso 1 1 d . . .
C1' C 0.69049(16) 0.42737(13) 0.28130(13) 0.0214(4) Uani 1 1 d . . .
O2' O 0.38029(11) 0.26431(10) 0.42877(10) 0.0285(3) Uani 1 1 d . . .
C2' C 0.66430(15) 0.37742(13) 0.22981(13) 0.0209(4) Uani 1 1 d . . .
O3' O 0.83988(11) 0.52760(10) 0.48425(9) 0.0252(3) Uani 1 1 d . . .
C3' C 0.56034(16) 0.33598(14) 0.27995(14) 0.0232(4) Uani 1 1 d . . .
H3'1 H 0.5394 0.3248 0.2255 0.028 Uiso 1 1 calc R . .
H3'2 H 0.4916 0.3940 0.3047 0.028 Uiso 1 1 calc R . .
C4' C 0.58473(16) 0.22640(14) 0.37357(14) 0.0223(4) Uani 1 1 d . . .
C5' C 0.49134(16) 0.19404(14) 0.44877(14) 0.0248(4) Uani 1 1 d . . .
C6' C 0.28229(16) 0.24233(15) 0.51065(14) 0.0270(4) Uani 1 1 d . . .
H6'1 H 0.2840 0.2515 0.5752 0.032 Uiso 1 1 calc R . .
H6'2 H 0.2860 0.1645 0.5293 0.032 Uiso 1 1 calc R . .
C7' C 0.82898(16) 0.67592(15) 0.53037(15) 0.0267(4) Uani 1 1 d . . .
H7'1 H 0.8337 0.6934 0.5888 0.032 Uiso 1 1 calc R . .
H7'2 H 0.8975 0.6870 0.4726 0.032 Uiso 1 1 calc R . .
C8' C 0.83904(16) 0.55436(15) 0.57069(14) 0.0256(4) Uani 1 1 d . . .
H8'1 H 0.9128 0.5061 0.5990 0.031 Uiso 1 1 calc R . .
H8'2 H 0.7713 0.5413 0.6287 0.031 Uiso 1 1 calc R . .
C9' C 0.85050(15) 0.41864(14) 0.50613(14) 0.0220(4) Uani 1 1 d . . .
C10' C 0.85162(15) 0.39321(14) 0.42136(13) 0.0221(4) Uani 1 1 d . . .
C11' C 0.83497(17) 0.48386(14) 0.31289(14) 0.0250(4) Uani 1 1 d . . .
H11C H 0.7752 0.5543 0.3231 0.030 Uiso 1 1 calc R . .
H11D H 0.9104 0.4983 0.2747 0.030 Uiso 1 1 calc R . .
C12' C 0.79587(16) 0.45106(13) 0.24590(13) 0.0216(4) Uani 1 1 d . . .
C13' C 0.86991(16) 0.43164(14) 0.15332(13) 0.0230(4) Uani 1 1 d . . .
H13' H 0.9406 0.4496 0.1269 0.028 Uiso 1 1 calc R . .
C14' C 0.84277(16) 0.38683(14) 0.09916(13) 0.0234(4) Uani 1 1 d . . .
H14' H 0.8934 0.3758 0.0353 0.028 Uiso 1 1 calc R . .
C15' C 0.74149(16) 0.35822(14) 0.13838(14) 0.0237(4) Uani 1 1 d . . .
H15' H 0.7243 0.3250 0.1024 0.028 Uiso 1 1 calc R . .
C16' C 0.69884(17) 0.15566(15) 0.38734(15) 0.0263(4) Uani 1 1 d . . .
H16' H 0.7639 0.1753 0.3366 0.032 Uiso 1 1 calc R . .
C17' C 0.71990(17) 0.05656(15) 0.47391(15) 0.0296(4) Uani 1 1 d . . .
H17' H 0.7986 0.0090 0.4819 0.036 Uiso 1 1 calc R . .
C18' C 0.62641(18) 0.02787(15) 0.54766(16) 0.0326(5) Uani 1 1 d . . .
H18' H 0.6406 -0.0395 0.6071 0.039 Uiso 1 1 calc R . .
C19' C 0.51181(18) 0.09608(15) 0.53619(15) 0.0313(4) Uani 1 1 d . . .
H19' H 0.4473 0.0761 0.5878 0.038 Uiso 1 1 calc R . .
C20' C 0.85971(16) 0.33669(15) 0.60619(14) 0.0262(4) Uani 1 1 d . . .
H20' H 0.8570 0.3554 0.6638 0.031 Uiso 1 1 calc R . .
C21' C 0.87280(16) 0.22813(16) 0.62221(15) 0.0296(4) Uani 1 1 d . . .
H21' H 0.8790 0.1724 0.6907 0.036 Uiso 1 1 calc R . .
C22' C 0.87687(18) 0.20103(15) 0.53901(15) 0.0319(5) Uani 1 1 d . . .
H22' H 0.8872 0.1262 0.5494 0.038 Uiso 1 1 calc R . .
C23' C 0.86588(16) 0.28324(15) 0.43990(15) 0.0270(4) Uani 1 1 d . . .
H23' H 0.8682 0.2638 0.3830 0.032 Uiso 1 1 calc R . .
N1 N 0.39411(15) 1.02497(14) 0.11759(13) 0.0289(4) Uani 1 1 d . . .
H1NA H 0.489(2) 1.003(2) 0.1057(18) 0.056(7) Uiso 1 1 d . . .
H1NB H 0.377(2) 1.039(2) 0.046(2) 0.063(7) Uiso 1 1 d . . .
H1NC H 0.3567(19) 1.0946(19) 0.1335(16) 0.040(6) Uiso 1 1 d . . .
C1G C 0.3508(2) 0.93617(17) 0.20607(17) 0.0514(7) Uani 1 1 d . B .
H1G1 H 0.2651 0.9567 0.2108 0.062 Uiso 1 1 calc R . .
H1G2 H 0.3624 0.9302 0.2740 0.062 Uiso 1 1 calc R . .
C2G C 0.4162(2) 0.82340(17) 0.18918(16) 0.0426(6) Uani 1 1 d D . .
H2G2 H 0.3579 0.7869 0.2057 0.121(14) Uiso 1 1 calc RD A 1
H2G1 H 0.4533 0.8369 0.1131 0.090(10) Uiso 1 1 calc RD A 1
C3G C 0.5075(3) 0.7461(2) 0.2530(2) 0.0292(6) Uiso 0.65 1 d P B 1
H3G1 H 0.5610 0.7855 0.2421 0.035 Uiso 0.65 1 calc PR B 1
H3G2 H 0.5548 0.6826 0.2261 0.035 Uiso 0.65 1 calc PR B 1
C4G C 0.4625(3) 0.6989(3) 0.3717(2) 0.0317(7) Uiso 0.65 1 d P B 1
H4G1 H 0.4201 0.7609 0.4009 0.038 Uiso 0.65 1 calc PR B 1
H4G2 H 0.4062 0.6619 0.3839 0.038 Uiso 0.65 1 calc PR B 1
C3G' C 0.4493(5) 0.7275(4) 0.2886(4) 0.0264(11) Uiso 0.35 1 d P B 2
H3G3 H 0.4701 0.6574 0.2753 0.032 Uiso 0.35 1 calc PR B 2
H3G4 H 0.3775 0.7326 0.3450 0.032 Uiso 0.35 1 calc PR B 2
C4G' C 0.5489(5) 0.7143(4) 0.3338(4) 0.0242(11) Uiso 0.35 1 d P B 2
H4G3 H 0.6232 0.7067 0.2805 0.029 Uiso 0.35 1 calc PR B 2
H4G4 H 0.5296 0.7814 0.3517 0.029 Uiso 0.35 1 calc PR B 2
N2 N 0.56348(17) 0.61539(14) 0.42845(14) 0.0327(4) Uani 1 1 d . . .
H2NA H 0.628(4) 0.643(3) 0.431(3) 0.142(15) Uiso 1 1 d . . .
H2NB H 0.507(3) 0.594(3) 0.507(3) 0.116(12) Uiso 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0210(7) 0.0279(6) 0.0291(7) -0.0146(5) -0.0106(5) -0.0010(5)
C1 0.0172(8) 0.0206(8) 0.0226(8) -0.0067(7) -0.0049(7) -0.0065(7)
O2 0.0215(7) 0.0231(6) 0.0256(6) -0.0067(5) -0.0027(5) -0.0041(5)
C2 0.0193(9) 0.0200(8) 0.0194(8) -0.0070(6) -0.0020(7) -0.0072(7)
O3 0.0300(7) 0.0298(7) 0.0262(7) -0.0124(5) -0.0007(6) -0.0143(6)
C3 0.0232(9) 0.0228(8) 0.0221(9) -0.0099(7) -0.0031(7) -0.0076(7)
C4 0.0233(9) 0.0206(8) 0.0228(8) -0.0102(7) -0.0028(7) -0.0080(7)
C5 0.0232(9) 0.0235(8) 0.0228(9) -0.0120(7) -0.0012(7) -0.0078(7)
C6 0.0262(10) 0.0189(8) 0.0291(9) -0.0092(7) -0.0076(8) -0.0033(7)
C7 0.0260(10) 0.0253(9) 0.0324(10) -0.0158(8) -0.0058(8) -0.0024(8)
C8 0.0262(10) 0.0283(9) 0.0262(9) -0.0139(8) -0.0047(8) -0.0050(8)
C9 0.0157(9) 0.0195(8) 0.0304(9) -0.0093(7) -0.0014(7) -0.0037(7)
C10 0.0153(9) 0.0175(8) 0.0316(9) -0.0089(7) -0.0029(7) -0.0019(7)
C11 0.0212(9) 0.0187(8) 0.0283(9) -0.0096(7) -0.0027(7) -0.0051(7)
C12 0.0191(9) 0.0184(8) 0.0240(8) -0.0058(7) -0.0030(7) -0.0073(7)
C13 0.0191(9) 0.0219(8) 0.0289(9) -0.0053(7) -0.0063(7) -0.0040(7)
C14 0.0246(10) 0.0320(10) 0.0258(9) -0.0041(8) -0.0099(8) -0.0102(8)
C15 0.0261(10) 0.0289(9) 0.0223(9) -0.0078(7) -0.0055(7) -0.0125(8)
C16 0.0251(10) 0.0248(9) 0.0291(9) -0.0134(7) -0.0028(8) -0.0077(8)
C17 0.0297(11) 0.0330(10) 0.0313(10) -0.0148(8) 0.0056(8) -0.0143(9)
C18 0.0401(12) 0.0277(9) 0.0255(10) -0.0078(8) 0.0036(9) -0.0150(9)
C19 0.0329(11) 0.0216(8) 0.0251(9) -0.0066(7) -0.0044(8) -0.0077(8)
C20 0.0216(10) 0.0258(9) 0.0302(10) -0.0092(8) -0.0026(8) -0.0024(8)
C21 0.0226(10) 0.0255(9) 0.0328(10) -0.0036(8) 0.0017(8) -0.0052(8)
C22 0.0246(10) 0.0267(9) 0.0471(12) -0.0090(9) -0.0022(9) -0.0115(8)
C23 0.0232(10) 0.0235(9) 0.0365(10) -0.0108(8) -0.0039(8) -0.0075(8)
O1' 0.0258(7) 0.0264(6) 0.0247(7) -0.0139(5) 0.0023(5) -0.0100(6)
C1' 0.0220(9) 0.0170(7) 0.0208(8) -0.0069(6) -0.0051(7) -0.0015(7)
O2' 0.0199(7) 0.0292(7) 0.0302(7) -0.0099(6) 0.0013(5) -0.0075(5)
C2' 0.0206(9) 0.0182(8) 0.0225(8) -0.0067(7) -0.0060(7) -0.0039(7)
O3' 0.0290(7) 0.0249(6) 0.0241(6) -0.0119(5) -0.0058(5) -0.0069(5)
C3' 0.0214(9) 0.0232(8) 0.0268(9) -0.0105(7) -0.0059(7) -0.0059(7)
C4' 0.0250(10) 0.0204(8) 0.0253(9) -0.0128(7) -0.0037(7) -0.0066(7)
C5' 0.0237(10) 0.0235(8) 0.0294(9) -0.0144(7) -0.0025(8) -0.0063(7)
C6' 0.0246(10) 0.0272(9) 0.0297(10) -0.0129(8) 0.0030(8) -0.0120(8)
C7' 0.0229(10) 0.0359(10) 0.0287(10) -0.0181(8) 0.0008(8) -0.0134(8)
C8' 0.0224(9) 0.0317(9) 0.0256(9) -0.0143(8) -0.0042(7) -0.0073(8)
C9' 0.0153(8) 0.0228(8) 0.0263(9) -0.0108(7) -0.0030(7) -0.0032(7)
C10' 0.0171(9) 0.0243(8) 0.0230(9) -0.0085(7) -0.0035(7) -0.0050(7)
C11' 0.0267(10) 0.0217(8) 0.0261(9) -0.0070(7) -0.0059(8) -0.0080(7)
C12' 0.0233(9) 0.0174(8) 0.0223(8) -0.0057(7) -0.0075(7) -0.0040(7)
C13' 0.0208(9) 0.0203(8) 0.0228(9) -0.0047(7) -0.0048(7) -0.0045(7)
C14' 0.0226(9) 0.0235(8) 0.0189(8) -0.0081(7) -0.0032(7) -0.0028(7)
C15' 0.0272(10) 0.0211(8) 0.0230(9) -0.0088(7) -0.0076(8) -0.0046(7)
C16' 0.0236(10) 0.0237(9) 0.0314(10) -0.0121(8) -0.0024(8) -0.0072(8)
C17' 0.0276(10) 0.0226(9) 0.0360(10) -0.0104(8) -0.0081(9) -0.0040(8)
C18' 0.0385(12) 0.0217(9) 0.0332(10) -0.0066(8) -0.0084(9) -0.0080(8)
C19' 0.0313(11) 0.0244(9) 0.0334(10) -0.0098(8) 0.0015(9) -0.0109(8)
C20' 0.0191(9) 0.0302(9) 0.0267(9) -0.0105(8) -0.0052(7) -0.0044(8)
C21' 0.0235(10) 0.0285(9) 0.0300(10) -0.0028(8) -0.0090(8) -0.0072(8)
C22' 0.0345(11) 0.0216(9) 0.0376(11) -0.0059(8) -0.0151(9) -0.0055(8)
C23' 0.0279(10) 0.0237(9) 0.0314(10) -0.0117(8) -0.0106(8) -0.0042(8)
N1 0.0221(9) 0.0327(9) 0.0313(9) -0.0185(7) -0.0087(7) 0.0019(7)
C1G 0.0586(16) 0.0304(11) 0.0296(11) -0.0068(9) 0.0023(10) 0.0046(11)
C2G 0.0518(15) 0.0316(10) 0.0306(11) -0.0132(9) -0.0097(10) 0.0022(10)
N2 0.0349(10) 0.0312(9) 0.0320(9) -0.0145(7) -0.0044(8) -0.0087(8)

_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 1.3213(19) . ?
C1 C2 1.408(2) . ?
C1 C12 1.419(2) . ?
O2 C5 1.370(2) . ?
O2 C6 1.432(2) . ?
C2 C15 1.384(2) . ?
C2 C3 1.510(2) . ?
O3 C9 1.375(2) . ?
O3 C8 1.427(2) . ?
C3 C4 1.519(2) . ?
C4 C16 1.390(2) . ?
C4 C5 1.402(2) . ?
C5 C19 1.391(2) . ?
C6 C7 1.502(3) 2_675 ?
C7 C6 1.502(3) 2_675 ?
C7 C8 1.507(3) . ?
C9 C20 1.387(3) . ?
C9 C10 1.398(2) . ?
C10 C23 1.384(3) . ?
C10 C11 1.523(2) . ?
C11 C12 1.501(2) . ?
C12 C13 1.383(2) . ?
C13 C14 1.380(3) . ?
C14 C15 1.389(3) . ?
C16 C17 1.388(3) . ?
C17 C18 1.381(3) . ?
C18 C19 1.384(3) . ?
C20 C21 1.382(3) . ?
C21 C22 1.373(3) . ?
C22 C23 1.389(3) . ?
O1' C1' 1.358(2) . ?
C1' C12' 1.398(3) . ?
C1' C2' 1.401(2) . ?
O2' C5' 1.375(2) . ?
O2' C6' 1.429(2) . ?
C2' C15' 1.392(2) . ?
C2' C3' 1.507(2) . ?
O3' C9' 1.376(2) . ?
O3' C8' 1.431(2) . ?
C3' C4' 1.524(2) . ?
C4' C16' 1.388(2) . ?
C4' C5' 1.395(3) . ?
C5' C19' 1.389(2) . ?
C6' C7' 1.501(3) 2_666 ?
C7' C6' 1.501(3) 2_666 ?
C7' C8' 1.507(3) . ?
C9' C20' 1.391(2) . ?
C9' C10' 1.394(2) . ?
C10' C23' 1.388(2) . ?
C10' C11' 1.525(2) . ?
C11' C12' 1.510(2) . ?
C12' C13' 1.394(2) . ?
C13' C14' 1.381(2) . ?
C14' C15' 1.381(3) . ?
C16' C17' 1.391(2) . ?
C17' C18' 1.371(3) . ?
C18' C19' 1.380(3) . ?
C20' C21' 1.382(3) . ?
C21' C22' 1.373(3) . ?
C22' C23' 1.385(2) . ?
N1 C1G 1.483(3) . ?
C1G C2G 1.523(3) . ?
C2G C3G 1.461(3) . ?
C2G C3G' 1.500(5) . ?
C3G C4G 1.521(4) . ?
C4G N2 1.507(3) . ?
C3G' C4G' 1.524(7) . ?
C4G' N2 1.448(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 120.38(15) . . ?
O1 C1 C12 121.18(15) . . ?
C2 C1 C12 118.42(15) . . ?
C5 O2 C6 116.62(13) . . ?
C15 C2 C1 120.10(15) . . ?
C15 C2 C3 120.61(16) . . ?
C1 C2 C3 119.09(14) . . ?
C9 O3 C8 117.88(14) . . ?
C2 C3 C4 112.91(14) . . ?
C16 C4 C5 117.79(16) . . ?
C16 C4 C3 122.03(15) . . ?
C5 C4 C3 120.18(16) . . ?
O2 C5 C19 123.64(16) . . ?
O2 C5 C4 115.43(15) . . ?
C19 C5 C4 120.93(17) . . ?
O2 C6 C7 108.38(14) . 2_675 ?
C6 C7 C8 115.13(15) 2_675 . ?
O3 C8 C7 108.22(14) . . ?
O3 C9 C20 123.62(17) . . ?
O3 C9 C10 114.96(15) . . ?
C20 C9 C10 121.41(17) . . ?
C23 C10 C9 117.52(17) . . ?
C23 C10 C11 122.12(17) . . ?
C9 C10 C11 120.36(16) . . ?
C12 C11 C10 112.22(14) . . ?
C13 C12 C1 119.63(16) . . ?
C13 C12 C11 121.16(15) . . ?
C1 C12 C11 118.89(14) . . ?
C14 C13 C12 121.70(16) . . ?
C13 C14 C15 118.83(16) . . ?
C2 C15 C14 121.30(17) . . ?
C17 C16 C4 121.71(17) . . ?
C18 C17 C16 119.34(18) . . ?
C17 C18 C19 120.63(17) . . ?
C18 C19 C5 119.57(17) . . ?
C21 C20 C9 119.22(19) . . ?
C22 C21 C20 120.68(18) . . ?
C21 C22 C23 119.43(19) . . ?
C10 C23 C22 121.67(19) . . ?
O1' C1' C12' 122.38(16) . . ?
O1' C1' C2' 116.58(16) . . ?
C12' C1' C2' 120.86(16) . . ?
C5' O2' C6' 117.00(14) . . ?
C15' C2' C1' 118.79(16) . . ?
C15' C2' C3' 121.51(16) . . ?
C1' C2' C3' 119.44(15) . . ?
C9' O3' C8' 116.56(13) . . ?
C2' C3' C4' 112.83(14) . . ?
C16' C4' C5' 117.74(16) . . ?
C16' C4' C3' 121.94(16) . . ?
C5' C4' C3' 120.33(15) . . ?
O2' C5' C19' 123.43(17) . . ?
O2' C5' C4' 115.42(15) . . ?
C19' C5' C4' 121.13(17) . . ?
O2' C6' C7' 107.91(14) . 2_666 ?
C6' C7' C8' 114.82(15) 2_666 . ?
O3' C8' C7' 108.40(14) . . ?
O3' C9' C20' 123.22(16) . . ?
O3' C9' C10' 116.18(15) . . ?
C20' C9' C10' 120.60(16) . . ?
C23' C10' C9' 117.64(16) . . ?
C23' C10' C11' 121.34(16) . . ?
C9' C10' C11' 121.00(15) . . ?
C12' C11' C10' 112.25(14) . . ?
C13' C12' C1' 118.24(16) . . ?
C13' C12' C11' 120.71(16) . . ?
C1' C12' C11' 120.68(15) . . ?
C14' C13' C12' 121.42(17) . . ?
C13' C14' C15' 119.58(16) . . ?
C14' C15' C2' 120.92(17) . . ?
C4' C16' C17' 121.37(18) . . ?
C18' C17' C16' 119.64(18) . . ?
C17' C18' C19' 120.50(18) . . ?
C18' C19' C5' 119.60(18) . . ?
C21' C20' C9' 120.28(17) . . ?
C22' C21' C20' 119.86(17) . . ?
C21' C22' C23' 119.68(18) . . ?
C22' C23' C10' 121.90(18) . . ?
N1 C1G C2G 110.94(18) . . ?
C3G C2G C3G' 32.1(2) . . ?
C3G C2G C1G 114.9(2) . . ?
C3G' C2G C1G 113.4(3) . . ?
C2G C3G C4G 115.4(3) . . ?
N2 C4G C3G 110.7(2) . . ?
C2G C3G' C4G' 119.9(4) . . ?
N2 C4G' C3G' 108.8(4) . . ?
C4G' N2 C4G 44.5(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
O1 C1 C2 C15 -179.37(16) . . . . ?
C12 C1 C2 C15 -0.9(2) . . . . ?
O1 C1 C2 C3 -4.5(2) . . . . ?
C12 C1 C2 C3 173.97(15) . . . . ?
C15 C2 C3 C4 103.78(19) . . . . ?
C1 C2 C3 C4 -71.1(2) . . . . ?
C2 C3 C4 C16 -21.6(2) . . . . ?
C2 C3 C4 C5 159.51(16) . . . . ?
C6 O2 C5 C19 0.5(2) . . . . ?
C6 O2 C5 C4 179.67(15) . . . . ?
C16 C4 C5 O2 -177.65(15) . . . . ?
C3 C4 C5 O2 1.3(2) . . . . ?
C16 C4 C5 C19 1.6(3) . . . . ?
C3 C4 C5 C19 -179.47(16) . . . . ?
C5 O2 C6 C7 -168.90(15) . . . 2_675 ?
C9 O3 C8 C7 168.80(14) . . . . ?
C6 C7 C8 O3 47.4(2) 2_675 . . . ?
C8 O3 C9 C20 -2.1(2) . . . . ?
C8 O3 C9 C10 177.15(14) . . . . ?
O3 C9 C10 C23 178.48(15) . . . . ?
C20 C9 C10 C23 -2.2(2) . . . . ?
O3 C9 C10 C11 -0.7(2) . . . . ?
C20 C9 C10 C11 178.55(15) . . . . ?
C23 C10 C11 C12 15.3(2) . . . . ?
C9 C10 C11 C12 -165.55(15) . . . . ?
O1 C1 C12 C13 179.93(16) . . . . ?
C2 C1 C12 C13 1.5(2) . . . . ?
O1 C1 C12 C11 6.3(2) . . . . ?
C2 C1 C12 C11 -172.17(15) . . . . ?
C10 C11 C12 C13 -95.26(19) . . . . ?
C10 C11 C12 C1 78.3(2) . . . . ?
C1 C12 C13 C14 -1.4(3) . . . . ?
C11 C12 C13 C14 172.15(17) . . . . ?
C12 C13 C14 C15 0.6(3) . . . . ?
C1 C2 C15 C14 0.2(3) . . . . ?
C3 C2 C15 C14 -174.63(16) . . . . ?
C13 C14 C15 C2 0.0(3) . . . . ?
C5 C4 C16 C17 -0.1(3) . . . . ?
C3 C4 C16 C17 -179.05(17) . . . . ?
C4 C16 C17 C18 -0.9(3) . . . . ?
C16 C17 C18 C19 0.5(3) . . . . ?
C17 C18 C19 C5 0.9(3) . . . . ?
O2 C5 C19 C18 177.18(17) . . . . ?
C4 C5 C19 C18 -2.0(3) . . . . ?
O3 C9 C20 C21 -177.80(16) . . . . ?
C10 C9 C20 C21 3.0(3) . . . . ?
C9 C20 C21 C22 -1.4(3) . . . . ?
C20 C21 C22 C23 -0.9(3) . . . . ?
C9 C10 C23 C22 -0.1(3) . . . . ?
C11 C10 C23 C22 179.11(16) . . . . ?
C21 C22 C23 C10 1.7(3) . . . . ?
O1' C1' C2' C15' -179.27(14) . . . . ?
C12' C1' C2' C15' -4.1(2) . . . . ?
O1' C1' C2' C3' -5.0(2) . . . . ?
C12' C1' C2' C3' 170.14(15) . . . . ?
C15' C2' C3' C4' 98.44(18) . . . . ?
C1' C2' C3' C4' -75.64(19) . . . . ?
C2' C3' C4' C16' -20.1(2) . . . . ?
C2' C3' C4' C5' 160.03(16) . . . . ?
C6' O2' C5' C19' 9.2(2) . . . . ?
C6' O2' C5' C4' -171.91(15) . . . . ?
C16' C4' C5' O2' -177.04(15) . . . . ?
C3' C4' C5' O2' 2.9(2) . . . . ?
C16' C4' C5' C19' 1.9(3) . . . . ?
C3' C4' C5' C19' -178.18(17) . . . . ?
C5' O2' C6' C7' -176.72(14) . . . 2_666 ?
C9' O3' C8' C7' 179.03(14) . . . . ?
C6' C7' C8' O3' 62.0(2) 2_666 . . . ?
C8' O3' C9' C20' 0.2(2) . . . . ?
C8' O3' C9' C10' -179.80(15) . . . . ?
O3' C9' C10' C23' 178.06(16) . . . . ?
C20' C9' C10' C23' -2.0(3) . . . . ?
O3' C9' C10' C11' -3.3(2) . . . . ?
C20' C9' C10' C11' 176.70(16) . . . . ?
C23' C10' C11' C12' 19.1(2) . . . . ?
C9' C10' C11' C12' -159.55(16) . . . . ?
O1' C1' C12' C13' 179.72(14) . . . . ?
C2' C1' C12' C13' 4.8(2) . . . . ?
O1' C1' C12' C11' 6.7(2) . . . . ?
C2' C1' C12' C11' -168.19(14) . . . . ?
C10' C11' C12' C13' -113.23(17) . . . . ?
C10' C11' C12' C1' 59.6(2) . . . . ?
C1' C12' C13' C14' -2.1(2) . . . . ?
C11' C12' C13' C14' 170.96(15) . . . . ?
C12' C13' C14' C15' -1.4(2) . . . . ?
C13' C14' C15' C2' 2.2(2) . . . . ?
C1' C2' C15' C14' 0.5(2) . . . . ?
C3' C2' C15' C14' -173.59(15) . . . . ?
C5' C4' C16' C17' -0.9(3) . . . . ?
C3' C4' C16' C17' 179.15(17) . . . . ?
C4' C16' C17' C18' -0.2(3) . . . . ?
C16' C17' C18' C19' 0.5(3) . . . . ?
C17' C18' C19' C5' 0.5(3) . . . . ?
O2' C5' C19' C18' 177.17(17) . . . . ?
C4' C5' C19' C18' -1.7(3) . . . . ?
O3' C9' C20' C21' -178.56(17) . . . . ?
C10' C9' C20' C21' 1.5(3) . . . . ?
C9' C20' C21' C22' 0.1(3) . . . . ?
C20' C21' C22' C23' -1.0(3) . . . . ?
C21' C22' C23' C10' 0.5(3) . . . . ?
C9' C10' C23' C22' 1.0(3) . . . . ?
C11' C10' C23' C22' -177.66(17) . . . . ?
N1 C1G C2G C3G 102.5(3) . . . . ?
N1 C1G C2G C3G' 137.8(3) . . . . ?
C3G' C2G C3G C4G -25.3(4) . . . . ?
C1G C2G C3G C4G 69.4(3) . . . . ?
C2G C3G C4G N2 176.7(2) . . . . ?
C3G C2G C3G' C4G' 27.2(4) . . . . ?
C1G C2G C3G' C4G' -73.0(5) . . . . ?
C2G C3G' C4G' N2 -179.4(4) . . . . ?
C3G' C4G' N2 C4G -28.1(3) . . . . ?
C3G C4G N2 C4G' 29.6(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        30.09
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         0.972
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.055

# Attachment '1e checkcif.pdf'

# Attachment '1e.cif'

data_1e
_database_code_depnum_ccdc_archive 'CCDC 641527'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
(3,4:9,10:18,19:24,25-tetrabenzo-5,8,20,23-tetraoxa-tricyclo
[25.3.1.112,16]dotriaconta-1(30),3,9,12,14,16(32),18, 24,27(31),
28-decaene-31,32-diol) propylenediamine inclusion complex
;
_chemical_name_common            
;
(3,4:9,10:18,19:24,25-tetrabenzo-5,8,20,23-tetraoxa-tricyclo
(25.3.1.112,16)dotriaconta-1(30),3,9,12,14,16(32),18, 24,27(31), 28-
decaene-31,32-diol) propylenediamine inclusion complex
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H38 O6, C3 H12 N2, C3 H10 N2'
_chemical_formula_sum            'C50 H60 N4 O6'
_chemical_formula_weight         813.02

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

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_space_group_name_Hall           '-P 1'
_space_group_id                  2

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

_cell_length_a                   12.6048(7)
_cell_length_b                   13.1155(8)
_cell_length_c                   15.0029(7)
_cell_angle_alpha                82.348(3)
_cell_angle_beta                 75.666(3)
_cell_angle_gamma                63.130(3)
_cell_volume                     2142.9(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)

_exptl_crystal_description       needles
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             872
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_type   none

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(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  'Enraf Nonius Kappa CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_number            30823
_diffrn_reflns_av_R_equivalents  0.0648
_diffrn_reflns_av_sigmaI/netI    0.0976
_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       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.07
_diffrn_reflns_theta_max         27.94
_reflns_number_total             10212
_reflns_number_gt                7001
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Nonius collect'
_computing_cell_refinement       'Nonius collect'
_computing_data_reduction        'Nonius collect'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-seed
_computing_publication_material  ciftab

_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.
Most hydrogen atoms were refined usinga riding model, but the positions of
hydrogen atoms of NH2/NH3+ and OH/O- groups were located in electron density
difference maps and these atoms were refined without restraints.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0163P)^2^+2.2086P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0057(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         10212
_refine_ls_number_parameters     582
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1266
_refine_ls_R_factor_gt           0.0846
_refine_ls_wR_factor_ref         0.1581
_refine_ls_wR_factor_gt          0.1399
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_restrained_S_all      1.113
_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 0.17572(16) 0.89902(17) 0.46652(13) 0.0232(4) Uani 1 1 d . . .
C1 C 0.2901(2) 0.8622(2) 0.41893(18) 0.0188(6) Uani 1 1 d . . .
O2 O 0.09545(17) 0.64195(16) 0.35412(13) 0.0245(4) Uani 1 1 d . . .
C2 C 0.3433(2) 0.7654(2) 0.36239(18) 0.0211(6) Uani 1 1 d . . .
O3 O 0.15696(16) 1.18346(16) 0.61639(13) 0.0235(4) Uani 1 1 d . . .
C3 C 0.2665(2) 0.7117(2) 0.3463(2) 0.0231(6) Uani 1 1 d . . .
H3A H 0.2798 0.7058 0.2790 0.028 Uiso 1 1 calc R . .
H3B H 0.1802 0.7657 0.3679 0.028 Uiso 1 1 calc R . .
C4 C 0.2835(2) 0.5956(2) 0.38919(19) 0.0223(6) Uani 1 1 d . . .
C5 C 0.1932(2) 0.5612(2) 0.38906(19) 0.0232(6) Uani 1 1 d . . .
C6 C -0.0092(2) 0.6210(2) 0.3666(2) 0.0242(6) Uani 1 1 d . . .
H6A H -0.0417 0.6130 0.4330 0.029 Uiso 1 1 calc R . .
H6B H 0.0129 0.5494 0.3364 0.029 Uiso 1 1 calc R . .
C7 C 0.1029(2) 1.2798(2) 0.67532(19) 0.0230(6) Uani 1 1 d . . .
H7A H 0.1665 1.3005 0.6831 0.028 Uiso 1 1 calc R . .
H7B H 0.0645 1.2600 0.7367 0.028 Uiso 1 1 calc R . .
C8 C 0.2459(2) 1.0841(2) 0.64559(19) 0.0220(6) Uani 1 1 d . . .
C9 C 0.3193(2) 1.0013(2) 0.57819(18) 0.0198(6) Uani 1 1 d . . .
C10 C 0.3074(2) 1.0247(2) 0.47776(18) 0.0206(6) Uani 1 1 d . . .
H10A H 0.2201 1.0680 0.4760 0.025 Uiso 1 1 calc R . .
H10B H 0.3481 1.0738 0.4487 0.025 Uiso 1 1 calc R . .
C11 C 0.3605(2) 0.9196(2) 0.42184(18) 0.0201(6) Uani 1 1 d . . .
C12 C 0.4800(2) 0.8782(2) 0.37330(19) 0.0227(6) Uani 1 1 d . . .
H12 H 0.5268 0.9171 0.3764 0.027 Uiso 1 1 calc R . .
C13 C 0.5333(3) 0.7817(3) 0.3202(2) 0.0268(7) Uani 1 1 d . . .
H13 H 0.6160 0.7534 0.2885 0.032 Uiso 1 1 calc R . .
C14 C 0.4634(2) 0.7279(2) 0.31469(19) 0.0252(6) Uani 1 1 d . . .
H14 H 0.4984 0.6631 0.2770 0.030 Uiso 1 1 calc R . .
C15 C 0.3824(3) 0.5210(3) 0.4257(2) 0.0272(7) Uani 1 1 d . . .
H15 H 0.4442 0.5431 0.4267 0.033 Uiso 1 1 calc R . .
C16 C 0.3934(3) 0.4136(3) 0.4613(2) 0.0333(7) Uani 1 1 d . . .
H16 H 0.4615 0.3637 0.4870 0.040 Uiso 1 1 calc R . .
C17 C 0.3049(3) 0.3805(3) 0.4590(2) 0.0336(7) Uani 1 1 d . . .
H17 H 0.3129 0.3069 0.4821 0.040 Uiso 1 1 calc R . .
C18 C 0.2031(3) 0.4546(2) 0.4228(2) 0.0280(7) Uani 1 1 d . . .
H18 H 0.1419 0.4319 0.4214 0.034 Uiso 1 1 calc R . .
C19 C 0.2629(2) 1.0645(2) 0.73529(19) 0.0233(6) Uani 1 1 d . . .
H19 H 0.2116 1.1207 0.7803 0.028 Uiso 1 1 calc R . .
C20 C 0.3543(3) 0.9633(3) 0.7594(2) 0.0283(7) Uani 1 1 d . . .
H20 H 0.3663 0.9507 0.8208 0.034 Uiso 1 1 calc R . .
C21 C 0.4282(3) 0.8807(3) 0.6945(2) 0.0283(7) Uani 1 1 d . . .
H21 H 0.4916 0.8115 0.7106 0.034 Uiso 1 1 calc R . .
C22 C 0.4084(2) 0.9005(2) 0.6050(2) 0.0249(6) Uani 1 1 d . . .
H22 H 0.4579 0.8427 0.5610 0.030 Uiso 1 1 calc R . .
O1' O -0.00917(17) 0.86094(16) 0.04566(13) 0.0236(4) Uani 1 1 d . . .
C1' C -0.0141(2) 0.7622(2) 0.06990(18) 0.0195(6) Uani 1 1 d . . .
O2' O -0.37846(18) 1.04142(17) -0.03338(14) 0.0276(5) Uani 1 1 d . . .
C2' C -0.1219(2) 0.7505(2) 0.07415(18) 0.0213(6) Uani 1 1 d . . .
O3' O 0.39119(17) 0.73424(17) 0.02156(14) 0.0284(5) Uani 1 1 d . . .
C3' C -0.2292(2) 0.8507(2) 0.04651(19) 0.0241(6) Uani 1 1 d . . .
H3'1 H -0.2196 0.9210 0.0495 0.029 Uiso 1 1 calc R . .
H3'2 H -0.3034 0.8573 0.0924 0.029 Uiso 1 1 calc R . .
C4' C -0.2494(2) 0.8468(2) -0.04882(19) 0.0233(6) Uani 1 1 d . . .
C5' C -0.3283(2) 0.9475(2) -0.0873(2) 0.0246(6) Uani 1 1 d . . .
C6' C -0.4605(3) 1.1473(3) -0.0675(2) 0.0285(7) Uani 1 1 d . . .
H6'1 H -0.5349 1.1424 -0.0724 0.034 Uiso 1 1 calc R . .
H6'2 H -0.4217 1.1659 -0.1293 0.034 Uiso 1 1 calc R . .
C7' C 0.4917(3) 0.7628(3) 0.0015(2) 0.0293(7) Uani 1 1 d . . .
H7'1 H 0.5037 0.7922 -0.0627 0.035 Uiso 1 1 calc R . .
H7'2 H 0.5673 0.6948 0.0096 0.035 Uiso 1 1 calc R . .
C8' C 0.3939(2) 0.6556(2) -0.03166(19) 0.0245(6) Uani 1 1 d . . .
C9' C 0.2964(2) 0.6259(2) -0.00300(19) 0.0231(6) Uani 1 1 d . . .
C10' C 0.2045(2) 0.6739(3) 0.08598(19) 0.0242(6) Uani 1 1 d . . .
H10C H 0.2414 0.6319 0.1387 0.029 Uiso 1 1 calc R . .
H10D H 0.1865 0.7551 0.0896 0.029 Uiso 1 1 calc R . .
C11' C 0.0873(2) 0.6659(2) 0.09428(18) 0.0208(6) Uani 1 1 d . . .
C12' C 0.0770(3) 0.5654(2) 0.1260(2) 0.0260(6) Uani 1 1 d . . .
H12' H 0.1446 0.5019 0.1438 0.031 Uiso 1 1 calc R . .
C13' C -0.0295(3) 0.5558(3) 0.1322(2) 0.0304(7) Uani 1 1 d . . .
H13' H -0.0351 0.4867 0.1541 0.036 Uiso 1 1 calc R . .
C14' C -0.1277(3) 0.6485(3) 0.1061(2) 0.0268(6) Uani 1 1 d . . .
H14' H -0.2009 0.6421 0.1101 0.032 Uiso 1 1 calc R . .
C15' C -0.1925(3) 0.7487(3) -0.1001(2) 0.0285(7) Uani 1 1 d . . .
H15' H -0.1386 0.6793 -0.0755 0.034 Uiso 1 1 calc R . .
C16' C -0.2135(3) 0.7505(3) -0.1871(2) 0.0345(7) Uani 1 1 d . . .
H16' H -0.1739 0.6824 -0.2213 0.041 Uiso 1 1 calc R . .
C17' C -0.2908(3) 0.8499(3) -0.2240(2) 0.0360(8) Uani 1 1 d . . .
H17' H -0.3041 0.8504 -0.2837 0.043 Uiso 1 1 calc R . .
C18' C -0.3499(3) 0.9503(3) -0.1742(2) 0.0307(7) Uani 1 1 d . . .
H18' H -0.4040 1.0192 -0.1992 0.037 Uiso 1 1 calc R . .
C19' C 0.4844(3) 0.6072(3) -0.1087(2) 0.0297(7) Uani 1 1 d . . .
H19' H 0.5501 0.6276 -0.1271 0.036 Uiso 1 1 calc R . .
C20' C 0.4786(3) 0.5288(3) -0.1586(2) 0.0321(7) Uani 1 1 d . . .
H20' H 0.5409 0.4949 -0.2109 0.039 Uiso 1 1 calc R . .
C21' C 0.3828(3) 0.5002(3) -0.1324(2) 0.0331(7) Uani 1 1 d . . .
H21' H 0.3782 0.4473 -0.1671 0.040 Uiso 1 1 calc R . .
C22' C 0.2925(3) 0.5489(2) -0.0551(2) 0.0267(6) Uani 1 1 d . . .
H22' H 0.2265 0.5288 -0.0377 0.032 Uiso 1 1 calc R . .
N1 N -0.0236(2) 0.9492(2) 0.40668(16) 0.0239(5) Uani 1 1 d . . .
H1NA H -0.096(3) 1.012(3) 0.454(2) 0.051(10) Uiso 1 1 d . . .
H1NB H 0.069(4) 0.919(3) 0.427(3) 0.062(12) Uiso 1 1 d . . .
H1NC H -0.037(3) 0.880(3) 0.404(3) 0.063(12) Uiso 1 1 d . . .
C1G C -0.0234(3) 1.0157(2) 0.31842(19) 0.0264(6) Uani 1 1 d . . .
H1G1 H -0.0079 1.0813 0.3258 0.032 Uiso 1 1 calc R . .
H1G2 H -0.1049 1.0466 0.3036 0.032 Uiso 1 1 calc R . .
C2G C 0.0715(3) 0.9450(2) 0.23885(19) 0.0261(6) Uani 1 1 d . . .
H2G1 H 0.1530 0.9129 0.2538 0.031 Uiso 1 1 calc R . .
H2G2 H 0.0551 0.8803 0.2302 0.031 Uiso 1 1 calc R . .
C3G C 0.0714(3) 1.0148(3) 0.1509(2) 0.0286(7) Uani 1 1 d . . .
H3G1 H 0.0846 1.0810 0.1608 0.034 Uiso 1 1 calc R . .
H3G2 H 0.1404 0.9677 0.1029 0.034 Uiso 1 1 calc R . .
N2 N -0.0419(2) 1.0571(2) 0.11727(18) 0.0265(6) Uani 1 1 d . . .
H2NA H -0.048(3) 0.994(3) 0.107(2) 0.029(9) Uiso 1 1 d . . .
H2NB H -0.033(3) 1.101(3) 0.050(3) 0.059(11) Uiso 1 1 d . . .
H2NC H -0.114(3) 1.111(3) 0.157(2) 0.030(8) Uiso 1 1 d . . .
N3 N -0.0418(4) 1.2669(3) 0.4260(3) 0.0619(10) Uani 1 1 d . . .
H3NA H -0.113(6) 1.224(5) 0.459(4) 0.16(3) Uiso 1 1 d . . .
H3NB H 0.043(9) 1.259(9) 0.391(7) 0.31(5) Uiso 1 1 d . . .
C4G C -0.1037(4) 1.3679(4) 0.3666(3) 0.0515(10) Uani 1 1 d . . .
H4G1 H -0.0496 1.4057 0.3418 0.062 Uiso 1 1 calc R . .
H4G2 H -0.1791 1.4237 0.4049 0.062 Uiso 1 1 calc R . .
C5G C -0.1363(3) 1.3342(3) 0.2858(2) 0.0440(9) Uani 1 1 d . . .
H5G1 H -0.1616 1.4007 0.2427 0.053 Uiso 1 1 calc R . .
H5G2 H -0.0625 1.2718 0.2522 0.053 Uiso 1 1 calc R . .
C6G C -0.2350(3) 1.2962(3) 0.3142(2) 0.0385(8) Uani 1 1 d . . .
H6G1 H -0.2192 1.2410 0.3667 0.046 Uiso 1 1 calc R . .
H6G2 H -0.3140 1.3628 0.3342 0.046 Uiso 1 1 calc R . .
N4 N -0.2403(3) 1.2419(2) 0.2364(2) 0.0356(7) Uani 1 1 d . . .
H4NA H -0.310(4) 1.220(4) 0.253(3) 0.090(16) Uiso 1 1 d . . .
H4NB H -0.256(4) 1.293(4) 0.188(3) 0.073(15) Uiso 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0172(9) 0.0301(11) 0.0220(10) -0.0070(8) 0.0000(8) -0.0106(8)
C1 0.0179(13) 0.0207(14) 0.0178(13) 0.0004(11) -0.0047(10) -0.0083(11)
O2 0.0212(10) 0.0249(11) 0.0292(11) 0.0039(9) -0.0096(8) -0.0107(9)
C2 0.0241(14) 0.0223(14) 0.0197(14) -0.0018(11) -0.0066(11) -0.0113(12)
O3 0.0217(10) 0.0227(10) 0.0228(10) -0.0056(8) -0.0072(8) -0.0042(8)
C3 0.0224(14) 0.0212(14) 0.0261(15) -0.0030(12) -0.0071(12) -0.0082(12)
C4 0.0219(14) 0.0217(14) 0.0216(14) -0.0045(11) -0.0036(11) -0.0077(12)
C5 0.0203(14) 0.0225(14) 0.0244(15) -0.0037(12) -0.0059(11) -0.0059(12)
C6 0.0216(14) 0.0243(15) 0.0297(16) -0.0042(12) -0.0043(12) -0.0122(12)
C7 0.0204(14) 0.0237(14) 0.0246(15) -0.0065(12) -0.0050(11) -0.0077(12)
C8 0.0147(13) 0.0250(15) 0.0265(15) -0.0026(12) -0.0026(11) -0.0093(11)
C9 0.0169(13) 0.0243(14) 0.0218(14) -0.0026(11) -0.0023(11) -0.0124(11)
C10 0.0211(13) 0.0189(14) 0.0224(14) -0.0019(11) -0.0050(11) -0.0087(11)
C11 0.0184(13) 0.0218(14) 0.0190(14) -0.0033(11) -0.0034(11) -0.0075(11)
C12 0.0207(14) 0.0268(15) 0.0225(14) -0.0033(12) -0.0016(11) -0.0128(12)
C13 0.0199(14) 0.0315(16) 0.0250(15) -0.0070(13) 0.0011(12) -0.0090(13)
C14 0.0227(14) 0.0241(15) 0.0257(15) -0.0083(12) -0.0040(12) -0.0060(12)
C15 0.0202(14) 0.0275(16) 0.0324(17) -0.0024(13) -0.0077(12) -0.0077(12)
C16 0.0285(16) 0.0250(16) 0.0404(19) 0.0025(14) -0.0150(14) -0.0037(13)
C17 0.0339(17) 0.0230(16) 0.0413(19) 0.0052(14) -0.0093(15) -0.0110(14)
C18 0.0245(15) 0.0233(15) 0.0343(17) 0.0011(13) -0.0053(13) -0.0098(12)
C19 0.0229(14) 0.0274(15) 0.0197(14) -0.0048(12) -0.0045(11) -0.0099(12)
C20 0.0300(16) 0.0292(16) 0.0252(16) 0.0006(13) -0.0096(13) -0.0109(13)
C21 0.0273(15) 0.0241(15) 0.0303(16) 0.0005(13) -0.0091(13) -0.0072(13)
C22 0.0208(14) 0.0264(15) 0.0271(15) -0.0049(12) -0.0046(12) -0.0091(12)
O1' 0.0290(11) 0.0226(10) 0.0212(10) 0.0006(8) -0.0059(8) -0.0130(9)
C1' 0.0228(14) 0.0190(13) 0.0153(13) -0.0017(11) -0.0019(11) -0.0085(11)
O2' 0.0287(11) 0.0229(11) 0.0294(11) -0.0003(9) -0.0124(9) -0.0066(9)
C2' 0.0220(14) 0.0221(14) 0.0183(14) -0.0045(11) -0.0032(11) -0.0078(12)
O3' 0.0222(10) 0.0315(12) 0.0317(12) -0.0070(9) -0.0001(9) -0.0131(9)
C3' 0.0212(14) 0.0287(16) 0.0248(15) -0.0052(12) -0.0057(11) -0.0113(12)
C4' 0.0206(14) 0.0259(15) 0.0250(15) -0.0016(12) -0.0057(11) -0.0107(12)
C5' 0.0227(14) 0.0270(15) 0.0276(16) -0.0014(12) -0.0038(12) -0.0144(12)
C6' 0.0213(14) 0.0292(16) 0.0353(17) 0.0030(13) -0.0106(13) -0.0098(13)
C7' 0.0200(14) 0.0294(16) 0.0361(18) 0.0011(14) -0.0040(13) -0.0103(13)
C8' 0.0224(14) 0.0207(14) 0.0252(15) -0.0027(12) -0.0059(12) -0.0039(12)
C9' 0.0230(14) 0.0208(14) 0.0212(14) -0.0013(11) -0.0048(11) -0.0055(12)
C10' 0.0193(14) 0.0300(16) 0.0215(14) -0.0058(12) -0.0031(11) -0.0085(12)
C11' 0.0207(13) 0.0242(14) 0.0153(13) -0.0027(11) -0.0022(11) -0.0080(12)
C12' 0.0276(15) 0.0189(14) 0.0271(16) -0.0020(12) -0.0052(12) -0.0064(12)
C13' 0.0376(17) 0.0202(15) 0.0353(17) 0.0017(13) -0.0048(14) -0.0163(14)
C14' 0.0279(15) 0.0286(16) 0.0275(16) -0.0038(13) -0.0016(12) -0.0167(13)
C15' 0.0301(16) 0.0287(16) 0.0263(16) -0.0012(13) -0.0071(13) -0.0118(13)
C16' 0.0432(19) 0.0346(18) 0.0263(17) -0.0060(14) -0.0072(14) -0.0161(16)
C17' 0.046(2) 0.043(2) 0.0256(17) 0.0016(15) -0.0144(15) -0.0225(17)
C18' 0.0334(17) 0.0363(18) 0.0279(16) 0.0049(14) -0.0122(13) -0.0186(15)
C19' 0.0202(14) 0.0291(16) 0.0310(17) 0.0011(13) -0.0028(12) -0.0049(13)
C20' 0.0270(16) 0.0320(17) 0.0259(16) -0.0081(13) -0.0009(13) -0.0036(13)
C21' 0.0373(18) 0.0280(17) 0.0285(17) -0.0098(13) -0.0052(14) -0.0080(14)
C22' 0.0280(15) 0.0231(15) 0.0255(15) -0.0049(12) -0.0059(12) -0.0068(13)
N1 0.0241(13) 0.0258(13) 0.0211(13) -0.0014(10) -0.0038(10) -0.0105(11)
C1G 0.0284(15) 0.0263(15) 0.0213(15) 0.0020(12) -0.0061(12) -0.0093(13)
C2G 0.0224(14) 0.0258(15) 0.0265(16) -0.0018(12) -0.0041(12) -0.0076(12)
C3G 0.0278(15) 0.0328(17) 0.0249(16) -0.0011(13) -0.0045(12) -0.0132(14)
N2 0.0312(14) 0.0275(14) 0.0233(14) 0.0007(11) -0.0048(11) -0.0158(12)
N3 0.053(2) 0.072(3) 0.051(2) -0.0102(19) -0.0198(18) -0.012(2)
C4G 0.064(3) 0.060(3) 0.039(2) -0.0098(19) -0.0005(19) -0.038(2)
C5G 0.050(2) 0.042(2) 0.043(2) -0.0008(17) -0.0041(17) -0.0253(18)
C6G 0.0375(19) 0.0322(18) 0.041(2) -0.0022(15) -0.0034(15) -0.0130(15)
N4 0.0351(16) 0.0292(15) 0.0445(18) 0.0038(13) -0.0130(13) -0.0147(13)

_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 1.332(3) . ?
C1 C11 1.409(4) . ?
C1 C2 1.421(4) . ?
O2 C5 1.381(3) . ?
O2 C6 1.428(3) . ?
C2 C14 1.389(4) . ?
C2 C3 1.506(4) . ?
O3 C8 1.385(3) . ?
O3 C7 1.437(3) . ?
C3 C4 1.513(4) . ?
C4 C15 1.380(4) . ?
C4 C5 1.403(4) . ?
C5 C18 1.382(4) . ?
C6 C7 1.498(4) 2_576 ?
C7 C6 1.498(4) 2_576 ?
C8 C19 1.387(4) . ?
C8 C9 1.407(4) . ?
C9 C22 1.382(4) . ?
C9 C10 1.528(4) . ?
C10 C11 1.500(4) . ?
C11 C12 1.385(4) . ?
C12 C13 1.387(4) . ?
C13 C14 1.377(4) . ?
C15 C16 1.395(4) . ?
C16 C17 1.377(4) . ?
C17 C18 1.401(4) . ?
C19 C20 1.384(4) . ?
C20 C21 1.382(4) . ?
C21 C22 1.396(4) . ?
O1' C1' 1.323(3) . ?
C1' C11' 1.418(4) . ?
C1' C2' 1.420(4) . ?
O2' C5' 1.371(3) . ?
O2' C6' 1.426(3) . ?
C2' C14' 1.387(4) . ?
C2' C3' 1.502(4) . ?
O3' C8' 1.370(3) . ?
O3' C7' 1.430(3) . ?
C3' C4' 1.524(4) . ?
C4' C15' 1.385(4) . ?
C4' C5' 1.400(4) . ?
C5' C18' 1.389(4) . ?
C6' C7' 1.491(4) 2_575 ?
C7' C6' 1.491(4) 2_575 ?
C8' C19' 1.389(4) . ?
C8' C9' 1.405(4) . ?
C9' C22' 1.381(4) . ?
C9' C10' 1.523(4) . ?
C10' C11' 1.502(4) . ?
C11' C12' 1.392(4) . ?
C12' C13' 1.382(4) . ?
C13' C14' 1.385(4) . ?
C15' C16' 1.390(4) . ?
C16' C17' 1.372(4) . ?
C17' C18' 1.395(4) . ?
C19' C20' 1.386(4) . ?
C20' C21' 1.374(4) . ?
C21' C22' 1.391(4) . ?
N1 C1G 1.486(4) . ?
C1G C2G 1.517(4) . ?
C2G C3G 1.503(4) . ?
C3G N2 1.473(4) . ?
N3 C4G 1.502(5) . ?
C4G C5G 1.545(5) . ?
C5G C6G 1.489(5) . ?
C6G N4 1.476(4) . ?

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
O1 C1 C11 121.0(2) . . ?
O1 C1 C2 120.7(2) . . ?
C11 C1 C2 118.3(2) . . ?
C5 O2 C6 117.7(2) . . ?
C14 C2 C1 119.4(2) . . ?
C14 C2 C3 120.1(2) . . ?
C1 C2 C3 120.2(2) . . ?
C8 O3 C7 116.6(2) . . ?
C2 C3 C4 119.7(2) . . ?
C15 C4 C5 118.2(3) . . ?
C15 C4 C3 124.8(3) . . ?
C5 C4 C3 117.0(2) . . ?
O2 C5 C18 123.9(3) . . ?
O2 C5 C4 114.8(2) . . ?
C18 C5 C4 121.3(3) . . ?
O2 C6 C7 108.0(2) . 2_576 ?
O3 C7 C6 109.3(2) . 2_576 ?
O3 C8 C19 123.4(2) . . ?
O3 C8 C9 115.7(2) . . ?
C19 C8 C9 120.9(3) . . ?
C22 C9 C8 117.4(3) . . ?
C22 C9 C10 121.0(2) . . ?
C8 C9 C10 121.5(2) . . ?
C11 C10 C9 114.5(2) . . ?
C12 C11 C1 119.9(2) . . ?
C12 C11 C10 119.6(2) . . ?
C1 C11 C10 120.5(2) . . ?
C11 C12 C13 121.9(3) . . ?
C14 C13 C12 118.3(3) . . ?
C13 C14 C2 122.1(3) . . ?
C4 C15 C16 121.4(3) . . ?
C17 C16 C15 119.5(3) . . ?
C16 C17 C18 120.5(3) . . ?
C5 C18 C17 119.0(3) . . ?
C20 C19 C8 120.2(3) . . ?
C21 C20 C19 120.1(3) . . ?
C20 C21 C22 119.1(3) . . ?
C9 C22 C21 122.3(3) . . ?
O1' C1' C11' 120.9(2) . . ?
O1' C1' C2' 120.8(2) . . ?
C11' C1' C2' 118.3(2) . . ?
C5' O2' C6' 118.0(2) . . ?
C14' C2' C1' 119.7(3) . . ?
C14' C2' C3' 121.2(3) . . ?
C1' C2' C3' 119.1(2) . . ?
C8' O3' C7' 118.6(2) . . ?
C2' C3' C4' 116.1(2) . . ?
C15' C4' C5' 118.1(3) . . ?
C15' C4' C3' 123.3(3) . . ?
C5' C4' C3' 118.6(3) . . ?
O2' C5' C18' 123.8(3) . . ?
O2' C5' C4' 114.5(3) . . ?
C18' C5' C4' 121.6(3) . . ?
O2' C6' C7' 107.5(2) . 2_575 ?
O3' C7' C6' 106.2(2) . 2_575 ?
O3' C8' C19' 124.1(3) . . ?
O3' C8' C9' 115.0(2) . . ?
C19' C8' C9' 120.9(3) . . ?
C22' C9' C8' 117.7(3) . . ?
C22' C9' C10' 122.9(3) . . ?
C8' C9' C10' 119.2(2) . . ?
C11' C10' C9' 113.6(2) . . ?
C12' C11' C1' 119.8(2) . . ?
C12' C11' C10' 120.8(3) . . ?
C1' C11' C10' 119.5(2) . . ?
C13' C12' C11' 121.5(3) . . ?
C12' C13' C14' 119.0(3) . . ?
C13' C14' C2' 121.6(3) . . ?
C4' C15' C16' 120.8(3) . . ?
C17' C16' C15' 120.5(3) . . ?
C16' C17' C18' 120.2(3) . . ?
C5' C18' C17' 118.8(3) . . ?
C20' C19' C8' 119.8(3) . . ?
C21' C20' C19' 120.0(3) . . ?
C20' C21' C22' 119.9(3) . . ?
C9' C22' C21' 121.6(3) . . ?
N1 C1G C2G 112.9(2) . . ?
C3G C2G C1G 111.8(2) . . ?
N2 C3G C2G 113.7(2) . . ?
N3 C4G C5G 112.5(3) . . ?
C6G C5G C4G 114.2(3) . . ?
N4 C6G C5G 109.9(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
O1 C1 C2 C14 -179.0(3) . . . . ?
C11 C1 C2 C14 2.3(4) . . . . ?
O1 C1 C2 C3 7.5(4) . . . . ?
C11 C1 C2 C3 -171.2(3) . . . . ?
C14 C2 C3 C4 77.1(4) . . . . ?
C1 C2 C3 C4 -109.4(3) . . . . ?
C2 C3 C4 C15 -15.4(4) . . . . ?
C2 C3 C4 C5 166.4(2) . . . . ?
C6 O2 C5 C18 10.0(4) . . . . ?
C6 O2 C5 C4 -169.2(2) . . . . ?
C15 C4 C5 O2 178.0(2) . . . . ?
C3 C4 C5 O2 -3.7(4) . . . . ?
C15 C4 C5 C18 -1.3(4) . . . . ?
C3 C4 C5 C18 177.0(3) . . . . ?
C5 O2 C6 C7 179.1(2) . . . 2_576 ?
C8 O3 C7 C6 -179.9(2) . . . 2_576 ?
C7 O3 C8 C19 16.5(4) . . . . ?
C7 O3 C8 C9 -164.2(2) . . . . ?
O3 C8 C9 C22 -179.5(2) . . . . ?
C19 C8 C9 C22 -0.1(4) . . . . ?
O3 C8 C9 C10 4.9(4) . . . . ?
C19 C8 C9 C10 -175.8(2) . . . . ?
C22 C9 C10 C11 23.2(4) . . . . ?
C8 C9 C10 C11 -161.3(2) . . . . ?
O1 C1 C11 C12 178.6(3) . . . . ?
C2 C1 C11 C12 -2.6(4) . . . . ?
O1 C1 C11 C10 -0.9(4) . . . . ?
C2 C1 C11 C10 177.8(2) . . . . ?
C9 C10 C11 C12 -92.2(3) . . . . ?
C9 C10 C11 C1 87.4(3) . . . . ?
C1 C11 C12 C13 0.8(4) . . . . ?
C10 C11 C12 C13 -179.7(3) . . . . ?
C11 C12 C13 C14 1.5(4) . . . . ?
C12 C13 C14 C2 -1.9(5) . . . . ?
C1 C2 C14 C13 0.0(4) . . . . ?
C3 C2 C14 C13 173.5(3) . . . . ?
C5 C4 C15 C16 0.3(4) . . . . ?
C3 C4 C15 C16 -177.8(3) . . . . ?
C4 C15 C16 C17 0.9(5) . . . . ?
C15 C16 C17 C18 -1.2(5) . . . . ?
O2 C5 C18 C17 -178.2(3) . . . . ?
C4 C5 C18 C17 1.0(4) . . . . ?
C16 C17 C18 C5 0.3(5) . . . . ?
O3 C8 C19 C20 -179.6(3) . . . . ?
C9 C8 C19 C20 1.2(4) . . . . ?
C8 C19 C20 C21 -0.8(4) . . . . ?
C19 C20 C21 C22 -0.7(4) . . . . ?
C8 C9 C22 C21 -1.3(4) . . . . ?
C10 C9 C22 C21 174.4(3) . . . . ?
C20 C21 C22 C9 1.7(4) . . . . ?
O1' C1' C2' C14' -175.4(2) . . . . ?
C11' C1' C2' C14' 3.2(4) . . . . ?
O1' C1' C2' C3' 2.8(4) . . . . ?
C11' C1' C2' C3' -178.6(2) . . . . ?
C14' C2' C3' C4' -79.9(3) . . . . ?
C1' C2' C3' C4' 102.0(3) . . . . ?
C2' C3' C4' C15' 14.4(4) . . . . ?
C2' C3' C4' C5' -165.0(2) . . . . ?
C6' O2' C5' C18' 2.0(4) . . . . ?
C6' O2' C5' C4' -179.7(2) . . . . ?
C15' C4' C5' O2' -178.4(2) . . . . ?
C3' C4' C5' O2' 1.0(4) . . . . ?
C15' C4' C5' C18' 0.0(4) . . . . ?
C3' C4' C5' C18' 179.4(3) . . . . ?
C5' O2' C6' C7' -174.3(2) . . . 2_575 ?
C8' O3' C7' C6' 177.7(2) . . . 2_575 ?
C7' O3' C8' C19' -4.8(4) . . . . ?
C7' O3' C8' C9' 175.3(2) . . . . ?
O3' C8' C9' C22' 178.6(3) . . . . ?
C19' C8' C9' C22' -1.3(4) . . . . ?
O3' C8' C9' C10' -4.9(4) . . . . ?
C19' C8' C9' C10' 175.2(3) . . . . ?
C22' C9' C10' C11' -21.1(4) . . . . ?
C8' C9' C10' C11' 162.5(3) . . . . ?
O1' C1' C11' C12' 175.3(2) . . . . ?
C2' C1' C11' C12' -3.3(4) . . . . ?
O1' C1' C11' C10' -4.4(4) . . . . ?
C2' C1' C11' C10' 177.0(2) . . . . ?
C9' C10' C11' C12' 83.2(3) . . . . ?
C9' C10' C11' C1' -97.1(3) . . . . ?
C1' C11' C12' C13' 1.7(4) . . . . ?
C10' C11' C12' C13' -178.6(3) . . . . ?
C11' C12' C13' C14' 0.1(4) . . . . ?
C12' C13' C14' C2' -0.2(5) . . . . ?
C1' C2' C14' C13' -1.5(4) . . . . ?
C3' C2' C14' C13' -179.6(3) . . . . ?
C5' C4' C15' C16' 0.0(4) . . . . ?
C3' C4' C15' C16' -179.3(3) . . . . ?
C4' C15' C16' C17' 0.2(5) . . . . ?
C15' C16' C17' C18' -0.4(5) . . . . ?
O2' C5' C18' C17' 178.0(3) . . . . ?
C4' C5' C18' C17' -0.2(4) . . . . ?
C16' C17' C18' C5' 0.4(5) . . . . ?
O3' C8' C19' C20' -179.5(3) . . . . ?
C9' C8' C19' C20' 0.4(5) . . . . ?
C8' C19' C20' C21' 0.7(5) . . . . ?
C19' C20' C21' C22' -0.8(5) . . . . ?
C8' C9' C22' C21' 1.3(4) . . . . ?
C10' C9' C22' C21' -175.2(3) . . . . ?
C20' C21' C22' C9' -0.2(5) . . . . ?
N1 C1G C2G C3G -178.9(2) . . . . ?
C1G C2G C3G N2 -64.8(3) . . . . ?
N3 C4G C5G C6G 69.5(4) . . . . ?
C4G C5G C6G N4 -167.3(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1NB O1 1.15(4) 1.51(4) 2.649(3) 169(3) .
N1 H1NA O1 1.08(4) 1.58(4) 2.648(3) 167(3) 2_576
N2 H2NA O1' 0.90(3) 1.89(3) 2.739(3) 157(3) .
N2 H2NB O1' 1.09(4) 1.51(4) 2.587(3) 167(3) 2_575
N2 H2NC N4 0.97(3) 2.01(3) 2.964(4) 167(3) .
N1 H1NC O3 1.01(4) 2.12(4) 3.010(3) 147(3) 2_576

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        27.94
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.560
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.061

data_1b
_database_code_depnum_ccdc_archive 'CCDC 767013'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
(3,4:9,10:18,19:24,25-tetrabenzo-5,8,20,23-tetraoxa-tricyclo
[25.3.1.112,16]dotriaconta-1(30),3,9,12,14,16(32),18, 24,27(31),
28-decaene-31,32-diol) propylenediamine inclusion complex
;
_chemical_name_common            
;
(3,4:9,10:18,19:24,25-tetrabenzo-5,8,20,23-tetraoxa-tricyclo
(25.3.1.112,16)dotriaconta-1(30),3,9,12,14,16(32),18, 24,27(31), 28-
decaene-31,32-diol) propylenediamine inclusion complex
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H40 O6,C3 H10 N2,C1 H Cl3'
_chemical_formula_sum            'C48 H51 Cl3 N2 O6'
_chemical_formula_weight         858.26

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'
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'
Cl Cl 0.1484 0.1585 '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'
_space_group_name_Hall           '-P 1'
_space_group_id                  2

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

_cell_length_a                   12.6805(2)
_cell_length_b                   13.8085(3)
_cell_length_c                   14.8731(3)
_cell_angle_alpha                113.964(1)
_cell_angle_beta                 93.672(1)
_cell_angle_gamma                108.788(1)
_cell_volume                     2195.08(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)

_exptl_crystal_description       needles
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             904
_exptl_absorpt_coefficient_mu    0.260
_exptl_absorpt_correction_type   none

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(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  'Enraf Nonius Kappa CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_number            10317
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1075
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.94
_diffrn_reflns_theta_max         27.92
_reflns_number_total             10317
_reflns_number_gt                5653
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Nonius collect'
_computing_cell_refinement       'Nonius collect'
_computing_data_reduction        'Nonius collect'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-seed
_computing_publication_material  ciftab

_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.
The positions of hydrogen atoms of NH2 and OH groups were located in electron
density difference maps and these atoms were refined without restraints.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0586P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10317
_refine_ls_number_parameters     556
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1350
_refine_ls_R_factor_gt           0.0555
_refine_ls_wR_factor_ref         0.1340
_refine_ls_wR_factor_gt          0.1105
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_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 0.33850(13) 0.93906(14) 0.42153(11) 0.0238(4) Uani 1 1 d . . .
H1O H 0.396(2) 0.953(2) 0.3955(18) 0.037(8) Uiso 1 1 d . . .
C1 C 0.24728(18) 0.84173(19) 0.36042(15) 0.0177(5) Uani 1 1 d . . .
O2 O 0.56923(13) 0.76987(14) 0.20049(11) 0.0255(4) Uani 1 1 d . . .
C2 C 0.25468(18) 0.7517(2) 0.27531(15) 0.0195(5) Uani 1 1 d . . .
O3 O 0.23190(13) 1.14442(13) 0.64628(10) 0.0235(4) Uani 1 1 d . . .
C3 C 0.36722(19) 0.7531(2) 0.24839(16) 0.0225(5) Uani 1 1 d . . .
H3A H 0.3640 0.6735 0.2189 0.027 Uiso 1 1 calc R . .
H3B H 0.4275 0.7980 0.3115 0.027 Uiso 1 1 calc R . .
C4 C 0.40301(18) 0.80210(19) 0.17507(15) 0.0188(5) Uani 1 1 d . . .
C5 C 0.50895(18) 0.80672(19) 0.15021(15) 0.0192(5) Uani 1 1 d . . .
C6 C 0.67868(18) 0.7708(2) 0.18234(15) 0.0237(6) Uani 1 1 d . . .
H6A H 0.7268 0.8457 0.1867 0.028 Uiso 1 1 calc R . .
H6B H 0.6705 0.7098 0.1144 0.028 Uiso 1 1 calc R . .
C7 C 0.26909(19) 1.2498(2) 0.73767(15) 0.0238(6) Uani 1 1 d . . .
H7A H 0.2034 1.2715 0.7559 0.029 Uiso 1 1 calc R . .
H7B H 0.3260 1.3123 0.7292 0.029 Uiso 1 1 calc R . .
C8 C 0.18929(17) 1.14310(19) 0.55839(15) 0.0177(5) Uani 1 1 d . . .
C9 C 0.14259(18) 1.03443(19) 0.47462(15) 0.0174(5) Uani 1 1 d . . .
C10 C 0.13972(18) 0.92961(19) 0.48502(15) 0.0186(5) Uani 1 1 d . . .
H10A H 0.0694 0.9003 0.5071 0.022 Uiso 1 1 calc R . .
H10B H 0.2058 0.9524 0.5387 0.022 Uiso 1 1 calc R . .
C11 C 0.14276(18) 0.83365(19) 0.38969(15) 0.0169(5) Uani 1 1 d . . .
C12 C 0.04525(18) 0.7376(2) 0.32941(15) 0.0204(5) Uani 1 1 d . . .
H12 H -0.0260 0.7317 0.3480 0.024 Uiso 1 1 calc R . .
C13 C 0.05013(19) 0.6500(2) 0.24263(15) 0.0229(5) Uani 1 1 d . . .
H13 H -0.0176 0.5857 0.2011 0.027 Uiso 1 1 calc R . .
C14 C 0.15436(19) 0.65709(19) 0.21694(15) 0.0222(5) Uani 1 1 d . . .
H14 H 0.1577 0.5961 0.1583 0.027 Uiso 1 1 calc R . .
C15 C 0.33766(19) 0.8400(2) 0.13042(15) 0.0239(6) Uani 1 1 d . . .
H15 H 0.2663 0.8387 0.1471 0.029 Uiso 1 1 calc R . .
C16 C 0.3739(2) 0.8800(2) 0.06149(17) 0.0310(6) Uani 1 1 d . . .
H16 H 0.3281 0.9068 0.0321 0.037 Uiso 1 1 calc R . .
C17 C 0.4770(2) 0.8807(2) 0.03585(17) 0.0292(6) Uani 1 1 d . . .
H17 H 0.5010 0.9061 -0.0127 0.035 Uiso 1 1 calc R . .
C18 C 0.54530(19) 0.8446(2) 0.08049(15) 0.0239(6) Uani 1 1 d . . .
H18 H 0.6165 0.8458 0.0634 0.029 Uiso 1 1 calc R . .
C19 C 0.19030(18) 1.2403(2) 0.55029(16) 0.0217(5) Uani 1 1 d . . .
H19 H 0.2233 1.3135 0.6074 0.026 Uiso 1 1 calc R . .
C20 C 0.1430(2) 1.2299(2) 0.45860(17) 0.0259(6) Uani 1 1 d . . .
H20 H 0.1430 1.2960 0.4530 0.031 Uiso 1 1 calc R . .
C21 C 0.0958(2) 1.1238(2) 0.37550(17) 0.0294(6) Uani 1 1 d . . .
H21 H 0.0625 1.1163 0.3128 0.035 Uiso 1 1 calc R . .
C22 C 0.0975(2) 1.0281(2) 0.38440(16) 0.0269(6) Uani 1 1 d . . .
H22 H 0.0665 0.9556 0.3264 0.032 Uiso 1 1 calc R . .
O1' O 0.42442(14) 0.54669(15) 0.63229(11) 0.0251(4) Uani 1 1 d . . .
H1'O H 0.495(3) 0.587(3) 0.625(2) 0.067(10) Uiso 1 1 d . . .
C1' C 0.42121(18) 0.55068(19) 0.72507(15) 0.0183(5) Uani 1 1 d . . .
O2' O 0.15241(13) 0.56009(13) 0.51595(10) 0.0234(4) Uani 1 1 d . . .
C2' C 0.31805(17) 0.54776(18) 0.75581(15) 0.0173(5) Uani 1 1 d . . .
O3' O 0.81718(11) 0.56219(13) 0.68785(10) 0.0223(4) Uani 1 1 d . . .
C3' C 0.22014(18) 0.53978(19) 0.68611(16) 0.0197(5) Uani 1 1 d . . .
H3'1 H 0.1477 0.5020 0.7012 0.024 Uiso 1 1 calc R . .
H3'2 H 0.2196 0.4897 0.6158 0.024 Uiso 1 1 calc R . .
C4' C 0.22255(17) 0.65289(19) 0.69223(15) 0.0180(5) Uani 1 1 d . . .
C5' C 0.18408(18) 0.6594(2) 0.60515(15) 0.0193(5) Uani 1 1 d . . .
C6' C 0.10680(19) 0.5617(2) 0.42589(15) 0.0220(5) Uani 1 1 d . . .
H6'1 H 0.1637 0.6208 0.4135 0.026 Uiso 1 1 calc R . .
H6'2 H 0.0371 0.5793 0.4325 0.026 Uiso 1 1 calc R . .
C7' C 0.92108(18) 0.5553(2) 0.65937(15) 0.0213(5) Uani 1 1 d . . .
H7'1 H 0.9756 0.5678 0.7175 0.026 Uiso 1 1 calc R . .
H7'2 H 0.9567 0.6149 0.6377 0.026 Uiso 1 1 calc R . .
C8' C 0.82207(18) 0.66491(19) 0.76000(14) 0.0181(5) Uani 1 1 d . . .
C9' C 0.71939(18) 0.66269(19) 0.79217(15) 0.0188(5) Uani 1 1 d . . .
C10' C 0.61976(18) 0.5484(2) 0.75080(16) 0.0226(5) Uani 1 1 d . . .
H10C H 0.6026 0.5143 0.6761 0.027 Uiso 1 1 calc R . .
H10D H 0.6437 0.4967 0.7701 0.027 Uiso 1 1 calc R . .
C11' C 0.51122(18) 0.55184(19) 0.78521(15) 0.0195(5) Uani 1 1 d . . .
C12' C 0.49776(19) 0.55393(19) 0.87852(16) 0.0228(5) Uani 1 1 d . . .
H12' H 0.5584 0.5549 0.9202 0.027 Uiso 1 1 calc R . .
C13' C 0.39905(19) 0.5546(2) 0.91146(16) 0.0230(5) Uani 1 1 d . . .
H13' H 0.3924 0.5578 0.9758 0.028 Uiso 1 1 calc R . .
C14' C 0.30894(18) 0.55061(19) 0.84980(16) 0.0209(5) Uani 1 1 d . . .
H14' H 0.2402 0.5498 0.8720 0.025 Uiso 1 1 calc R . .
C15' C 0.25575(19) 0.7505(2) 0.78371(17) 0.0255(6) Uani 1 1 d . . .
H15' H 0.2828 0.7481 0.8435 0.031 Uiso 1 1 calc R . .
C16' C 0.2505(2) 0.8518(2) 0.79003(17) 0.0312(6) Uani 1 1 d . . .
H16' H 0.2747 0.9180 0.8535 0.037 Uiso 1 1 calc R . .
C17' C 0.2099(2) 0.8561(2) 0.70394(17) 0.0288(6) Uani 1 1 d . . .
H17' H 0.2045 0.9248 0.7083 0.035 Uiso 1 1 calc R . .
C18' C 0.17691(19) 0.7598(2) 0.61084(17) 0.0233(5) Uani 1 1 d . . .
H18' H 0.1496 0.7627 0.5514 0.028 Uiso 1 1 calc R . .
C19' C 0.91898(19) 0.7657(2) 0.80110(15) 0.0232(5) Uani 1 1 d . . .
H19' H 0.9887 0.7660 0.7811 0.028 Uiso 1 1 calc R . .
C20' C 0.9128(2) 0.8661(2) 0.87167(16) 0.0276(6) Uani 1 1 d . . .
H20' H 0.9787 0.9353 0.8997 0.033 Uiso 1 1 calc R . .
C21' C 0.8129(2) 0.8668(2) 0.90139(17) 0.0303(6) Uani 1 1 d . . .
H21' H 0.8090 0.9362 0.9486 0.036 Uiso 1 1 calc R . .
C22' C 0.7169(2) 0.7645(2) 0.86171(16) 0.0263(6) Uani 1 1 d . . .
H22' H 0.6481 0.7651 0.8832 0.032 Uiso 1 1 calc R . .
N1 N 0.53504(18) 0.03903(19) 0.38533(17) 0.0305(5) Uani 1 1 d . . .
H1NA H 0.549(2) 0.032(2) 0.330(2) 0.036(8) Uiso 1 1 d . . .
H1NB H 0.590(3) 0.020(3) 0.415(2) 0.056(9) Uiso 1 1 d . . .
C1G C 0.5433(2) 0.1564(2) 0.45051(17) 0.0291(6) Uani 1 1 d . . .
H1G1 H 0.6239 0.2102 0.4690 0.035 Uiso 1 1 calc R . .
H1G2 H 0.5198 0.1596 0.5135 0.035 Uiso 1 1 calc R . .
C2G C 0.4692(2) 0.1937(2) 0.39901(17) 0.0311(6) Uani 1 1 d . . .
H2G1 H 0.3915 0.1329 0.3692 0.037 Uiso 1 1 calc R . .
H2G2 H 0.5016 0.2053 0.3437 0.037 Uiso 1 1 calc R . .
C3G C 0.4618(2) 0.3042(2) 0.47359(17) 0.0309(6) Uani 1 1 d . . .
H3G1 H 0.4210 0.2900 0.5243 0.037 Uiso 1 1 calc R . .
H3G2 H 0.5399 0.3619 0.5096 0.037 Uiso 1 1 calc R . .
N2 N 0.40172(19) 0.3499(2) 0.42321(17) 0.0306(5) Uani 1 1 d . . .
H2NB H 0.385(2) 0.404(2) 0.4675(18) 0.031(8) Uiso 1 1 d . . .
H2NA H 0.333(2) 0.294(3) 0.382(2) 0.049(9) Uiso 1 1 d . . .
C1Z C -0.0605(2) 0.7088(2) 0.00399(17) 0.0360(7) Uani 1 1 d . . .
H1Z H -0.0959 0.7246 -0.0479 0.043 Uiso 1 1 calc R . .
Cl1 Cl -0.16684(6) 0.60346(6) 0.01969(5) 0.0415(2) Uani 1 1 d . . .
Cl2 Cl 0.04811(6) 0.66075(7) -0.04021(5) 0.0526(2) Uani 1 1 d . . .
Cl3 Cl -0.00202(8) 0.83648(7) 0.11634(5) 0.0643(3) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0176(9) 0.0215(10) 0.0248(8) 0.0076(7) 0.0046(7) 0.0019(7)
C1 0.0197(12) 0.0156(12) 0.0202(11) 0.0103(10) 0.0023(9) 0.0070(10)
O2 0.0231(8) 0.0371(11) 0.0282(8) 0.0194(8) 0.0116(7) 0.0187(8)
C2 0.0221(12) 0.0229(13) 0.0196(11) 0.0121(10) 0.0073(9) 0.0123(11)
O3 0.0329(9) 0.0169(9) 0.0158(7) 0.0035(7) -0.0018(7) 0.0101(7)
C3 0.0277(13) 0.0256(14) 0.0227(11) 0.0133(10) 0.0107(10) 0.0163(11)
C4 0.0222(12) 0.0164(12) 0.0155(10) 0.0047(9) 0.0038(9) 0.0082(10)
C5 0.0223(12) 0.0179(13) 0.0136(10) 0.0038(9) 0.0007(9) 0.0079(10)
C6 0.0231(13) 0.0274(14) 0.0208(11) 0.0076(10) 0.0079(10) 0.0135(11)
C7 0.0224(12) 0.0217(13) 0.0227(11) 0.0033(10) 0.0042(10) 0.0117(11)
C8 0.0167(11) 0.0210(13) 0.0196(11) 0.0106(10) 0.0063(9) 0.0098(10)
C9 0.0195(11) 0.0178(13) 0.0196(11) 0.0105(10) 0.0081(9) 0.0093(10)
C10 0.0216(12) 0.0185(13) 0.0174(10) 0.0086(9) 0.0055(9) 0.0087(10)
C11 0.0205(12) 0.0164(12) 0.0170(10) 0.0090(9) 0.0043(9) 0.0089(10)
C12 0.0185(12) 0.0251(14) 0.0226(11) 0.0145(10) 0.0060(9) 0.0093(11)
C13 0.0228(13) 0.0176(13) 0.0208(11) 0.0077(10) 0.0013(9) 0.0010(10)
C14 0.0332(14) 0.0168(13) 0.0168(11) 0.0062(9) 0.0078(10) 0.0111(11)
C15 0.0217(12) 0.0305(15) 0.0209(11) 0.0117(11) 0.0036(9) 0.0116(11)
C16 0.0322(14) 0.0392(17) 0.0304(13) 0.0216(12) 0.0041(11) 0.0173(13)
C17 0.0342(14) 0.0334(16) 0.0239(12) 0.0177(11) 0.0079(11) 0.0112(12)
C18 0.0230(13) 0.0236(14) 0.0203(11) 0.0077(10) 0.0053(10) 0.0059(11)
C19 0.0216(12) 0.0204(13) 0.0248(12) 0.0102(10) 0.0072(9) 0.0097(11)
C20 0.0312(14) 0.0239(14) 0.0365(13) 0.0212(11) 0.0157(11) 0.0161(12)
C21 0.0455(16) 0.0300(16) 0.0224(12) 0.0170(11) 0.0076(11) 0.0192(13)
C22 0.0382(14) 0.0264(15) 0.0184(11) 0.0093(10) 0.0067(10) 0.0161(12)
O1' 0.0257(9) 0.0312(10) 0.0209(8) 0.0152(7) 0.0078(7) 0.0086(8)
C1' 0.0209(12) 0.0134(12) 0.0186(11) 0.0072(9) 0.0036(9) 0.0042(10)
O2' 0.0328(9) 0.0219(9) 0.0176(7) 0.0085(7) 0.0041(7) 0.0139(8)
C2' 0.0165(11) 0.0120(12) 0.0208(11) 0.0065(9) 0.0022(9) 0.0037(9)
O3' 0.0158(8) 0.0225(9) 0.0247(8) 0.0067(7) 0.0057(6) 0.0074(7)
C3' 0.0153(11) 0.0194(13) 0.0248(11) 0.0121(10) 0.0020(9) 0.0048(10)
C4' 0.0142(11) 0.0178(13) 0.0231(11) 0.0104(10) 0.0047(9) 0.0058(10)
C5' 0.0180(11) 0.0194(13) 0.0231(11) 0.0106(10) 0.0081(9) 0.0081(10)
C6' 0.0207(12) 0.0301(14) 0.0204(11) 0.0149(10) 0.0045(9) 0.0117(11)
C7' 0.0177(12) 0.0269(14) 0.0225(11) 0.0137(10) 0.0051(9) 0.0090(11)
C8' 0.0220(12) 0.0187(13) 0.0142(10) 0.0083(9) 0.0018(9) 0.0077(10)
C9' 0.0187(12) 0.0187(13) 0.0165(10) 0.0075(9) -0.0002(9) 0.0054(10)
C10' 0.0182(12) 0.0181(13) 0.0279(12) 0.0074(10) 0.0030(9) 0.0071(10)
C11' 0.0174(12) 0.0117(12) 0.0238(11) 0.0050(9) -0.0001(9) 0.0037(10)
C12' 0.0231(12) 0.0173(13) 0.0246(12) 0.0089(10) -0.0019(10) 0.0056(10)
C13' 0.0279(13) 0.0198(13) 0.0180(11) 0.0088(10) 0.0027(10) 0.0049(11)
C14' 0.0203(12) 0.0187(13) 0.0243(11) 0.0103(10) 0.0083(9) 0.0071(10)
C15' 0.0296(13) 0.0229(14) 0.0230(12) 0.0101(10) 0.0035(10) 0.0097(11)
C16' 0.0431(16) 0.0203(14) 0.0266(13) 0.0052(11) 0.0079(11) 0.0146(12)
C17' 0.0353(14) 0.0219(14) 0.0363(14) 0.0157(11) 0.0118(11) 0.0155(12)
C18' 0.0261(13) 0.0235(14) 0.0265(12) 0.0159(11) 0.0090(10) 0.0103(11)
C19' 0.0226(12) 0.0265(14) 0.0189(11) 0.0122(10) 0.0025(9) 0.0053(11)
C20' 0.0292(14) 0.0198(14) 0.0241(12) 0.0108(10) -0.0011(10) -0.0022(11)
C21' 0.0357(15) 0.0210(14) 0.0249(12) 0.0038(11) 0.0057(11) 0.0083(12)
C22' 0.0260(13) 0.0267(15) 0.0263(12) 0.0111(11) 0.0083(10) 0.0109(12)
N1 0.0287(13) 0.0302(13) 0.0274(12) 0.0138(10) 0.0061(10) 0.0041(10)
C1G 0.0237(13) 0.0278(15) 0.0265(12) 0.0103(11) 0.0035(10) 0.0015(11)
C2G 0.0321(14) 0.0283(15) 0.0251(12) 0.0120(11) 0.0029(11) 0.0027(12)
C3G 0.0339(15) 0.0328(16) 0.0245(12) 0.0148(12) 0.0098(11) 0.0079(12)
N2 0.0303(13) 0.0288(14) 0.0306(12) 0.0143(11) 0.0116(10) 0.0067(11)
C1Z 0.0495(17) 0.0305(16) 0.0218(12) 0.0096(11) 0.0070(12) 0.0108(13)
Cl1 0.0445(4) 0.0402(4) 0.0420(4) 0.0185(3) 0.0186(3) 0.0173(3)
Cl2 0.0360(4) 0.0638(6) 0.0437(4) 0.0148(4) 0.0102(3) 0.0139(4)
Cl3 0.1049(7) 0.0302(4) 0.0319(4) 0.0008(3) -0.0075(4) 0.0162(5)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.357(3) . ?
C1 C2 1.403(3) . ?
C1 C11 1.406(3) . ?
O2 C5 1.375(3) . ?
O2 C6 1.428(2) . ?
C2 C14 1.395(3) . ?
C2 C3 1.503(3) . ?
O3 C8 1.373(3) . ?
O3 C7 1.434(2) . ?
C3 C4 1.522(3) . ?
C4 C15 1.375(3) . ?
C4 C5 1.405(3) . ?
C5 C18 1.381(3) . ?
C6 C7 1.494(3) 2_676 ?
C7 C6 1.494(3) 2_676 ?
C8 C19 1.392(3) . ?
C8 C9 1.403(3) . ?
C9 C22 1.382(3) . ?
C9 C10 1.506(3) . ?
C10 C11 1.510(3) . ?
C11 C12 1.388(3) . ?
C12 C13 1.386(3) . ?
C13 C14 1.384(3) . ?
C15 C16 1.387(3) . ?
C16 C17 1.384(3) . ?
C17 C18 1.383(3) . ?
C19 C20 1.386(3) . ?
C20 C21 1.379(3) . ?
C21 C22 1.387(3) . ?
O1' C1' 1.362(2) . ?
C1' C11' 1.396(3) . ?
C1' C2' 1.407(3) . ?
O2' C5' 1.378(3) . ?
O2' C6' 1.436(3) . ?
C2' C14' 1.396(3) . ?
C2' C3' 1.511(3) . ?
O3' C8' 1.366(2) . ?
O3' C7' 1.430(2) . ?
C3' C4' 1.517(3) . ?
C4' C15' 1.385(3) . ?
C4' C5' 1.402(3) . ?
C5' C18' 1.388(3) . ?
C6' C7' 1.501(3) 2_666 ?
C7' C6' 1.501(3) 2_666 ?
C8' C19' 1.390(3) . ?
C8' C9' 1.411(3) . ?
C9' C22' 1.378(3) . ?
C9' C10' 1.514(3) . ?
C10' C11' 1.507(3) . ?
C11' C12' 1.399(3) . ?
C12' C13' 1.375(3) . ?
C13' C14' 1.390(3) . ?
C15' C16' 1.386(4) . ?
C16' C17' 1.380(3) . ?
C17' C18' 1.390(3) . ?
C19' C20' 1.388(3) . ?
C20' C21' 1.370(3) . ?
C21' C22' 1.395(3) . ?
N1 C1G 1.476(3) . ?
C1G C2G 1.509(3) . ?
C2G C3G 1.516(3) . ?
C3G N2 1.469(3) . ?
C1Z Cl1 1.744(3) . ?
C1Z Cl3 1.748(2) . ?
C1Z Cl2 1.766(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 123.52(19) . . ?
O1 C1 C11 115.58(18) . . ?
C2 C1 C11 120.86(19) . . ?
C5 O2 C6 119.41(17) . . ?
C14 C2 C1 118.23(19) . . ?
C14 C2 C3 119.85(19) . . ?
C1 C2 C3 121.9(2) . . ?
C8 O3 C7 118.28(18) . . ?
C2 C3 C4 116.3(2) . . ?
C15 C4 C5 118.1(2) . . ?
C15 C4 C3 124.35(19) . . ?
C5 C4 C3 117.5(2) . . ?
O2 C5 C18 124.9(2) . . ?
O2 C5 C4 113.84(19) . . ?
C18 C5 C4 121.2(2) . . ?
O2 C6 C7 105.98(17) . 2_676 ?
O3 C7 C6 106.49(19) . 2_676 ?
O3 C8 C19 124.00(19) . . ?
O3 C8 C9 115.0(2) . . ?
C19 C8 C9 121.0(2) . . ?
C22 C9 C8 117.3(2) . . ?
C22 C9 C10 122.17(19) . . ?
C8 C9 C10 120.47(19) . . ?
C9 C10 C11 114.56(17) . . ?
C12 C11 C1 118.73(18) . . ?
C12 C11 C10 122.07(19) . . ?
C1 C11 C10 119.20(19) . . ?
C13 C12 C11 121.1(2) . . ?
C14 C13 C12 119.5(2) . . ?
C13 C14 C2 121.44(19) . . ?
C4 C15 C16 121.3(2) . . ?
C17 C16 C15 119.6(2) . . ?
C18 C17 C16 120.4(2) . . ?
C17 C18 C5 119.3(2) . . ?
C20 C19 C8 119.7(2) . . ?
C21 C20 C19 120.2(2) . . ?
C20 C21 C22 119.4(2) . . ?
C9 C22 C21 122.3(2) . . ?
O1' C1' C11' 123.19(18) . . ?
O1' C1' C2' 115.79(19) . . ?
C11' C1' C2' 120.94(19) . . ?
C5' O2' C6' 117.35(17) . . ?
C14' C2' C1' 118.6(2) . . ?
C14' C2' C3' 121.96(18) . . ?
C1' C2' C3' 119.45(18) . . ?
C8' O3' C7' 117.83(16) . . ?
C2' C3' C4' 115.65(18) . . ?
C15' C4' C5' 118.0(2) . . ?
C15' C4' C3' 121.6(2) . . ?
C5' C4' C3' 120.36(19) . . ?
O2' C5' C18' 123.2(2) . . ?
O2' C5' C4' 115.8(2) . . ?
C18' C5' C4' 121.0(2) . . ?
O2' C6' C7' 106.86(19) . 2_666 ?
O3' C7' C6' 108.21(17) . 2_666 ?
O3' C8' C19' 124.38(19) . . ?
O3' C8' C9' 114.84(18) . . ?
C19' C8' C9' 120.78(19) . . ?
C22' C9' C8' 117.9(2) . . ?
C22' C9' C10' 123.87(19) . . ?
C8' C9' C10' 118.25(19) . . ?
C11' C10' C9' 115.89(18) . . ?
C1' C11' C12' 118.31(19) . . ?
C1' C11' C10' 121.58(19) . . ?
C12' C11' C10' 120.1(2) . . ?
C13' C12' C11' 121.7(2) . . ?
C12' C13' C14' 119.4(2) . . ?
C13' C14' C2' 120.96(19) . . ?
C4' C15' C16' 121.5(2) . . ?
C17' C16' C15' 119.9(2) . . ?
C16' C17' C18' 120.0(2) . . ?
C5' C18' C17' 119.7(2) . . ?
C20' C19' C8' 119.3(2) . . ?
C21' C20' C19' 120.9(2) . . ?
C20' C21' C22' 119.4(2) . . ?
C9' C22' C21' 121.7(2) . . ?
N1 C1G C2G 111.93(19) . . ?
C1G C2G C3G 110.67(19) . . ?
N2 C3G C2G 111.77(19) . . ?
Cl1 C1Z Cl3 111.31(13) . . ?
Cl1 C1Z Cl2 110.76(16) . . ?
Cl3 C1Z Cl2 110.19(14) . . ?

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
O1 C1 C2 C14 -178.5(2) . . . . ?
C11 C1 C2 C14 3.9(3) . . . . ?
O1 C1 C2 C3 3.8(3) . . . . ?
C11 C1 C2 C3 -173.8(2) . . . . ?
C14 C2 C3 C4 89.4(3) . . . . ?
C1 C2 C3 C4 -93.0(3) . . . . ?
C2 C3 C4 C15 -2.6(3) . . . . ?
C2 C3 C4 C5 178.68(19) . . . . ?
C6 O2 C5 C18 0.8(3) . . . . ?
C6 O2 C5 C4 -179.69(18) . . . . ?
C15 C4 C5 O2 178.41(19) . . . . ?
C3 C4 C5 O2 -2.8(3) . . . . ?
C15 C4 C5 C18 -2.1(3) . . . . ?
C3 C4 C5 C18 176.7(2) . . . . ?
C5 O2 C6 C7 168.47(18) . . . 2_676 ?
C8 O3 C7 C6 -174.45(17) . . . 2_676 ?
C7 O3 C8 C19 6.7(3) . . . . ?
C7 O3 C8 C9 -172.98(17) . . . . ?
O3 C8 C9 C22 179.40(19) . . . . ?
C19 C8 C9 C22 -0.3(3) . . . . ?
O3 C8 C9 C10 1.0(3) . . . . ?
C19 C8 C9 C10 -178.64(19) . . . . ?
C22 C9 C10 C11 29.8(3) . . . . ?
C8 C9 C10 C11 -151.91(19) . . . . ?
O1 C1 C11 C12 178.5(2) . . . . ?
C2 C1 C11 C12 -3.7(3) . . . . ?
O1 C1 C11 C10 -1.1(3) . . . . ?
C2 C1 C11 C10 176.6(2) . . . . ?
C9 C10 C11 C12 -102.2(2) . . . . ?
C9 C10 C11 C1 77.5(3) . . . . ?
C1 C11 C12 C13 0.9(3) . . . . ?
C10 C11 C12 C13 -179.5(2) . . . . ?
C11 C12 C13 C14 1.7(4) . . . . ?
C12 C13 C14 C2 -1.4(4) . . . . ?
C1 C2 C14 C13 -1.3(3) . . . . ?
C3 C2 C14 C13 176.4(2) . . . . ?
C5 C4 C15 C16 1.0(3) . . . . ?
C3 C4 C15 C16 -177.7(2) . . . . ?
C4 C15 C16 C17 0.9(4) . . . . ?
C15 C16 C17 C18 -1.7(4) . . . . ?
C16 C17 C18 C5 0.7(3) . . . . ?
O2 C5 C18 C17 -179.3(2) . . . . ?
C4 C5 C18 C17 1.3(3) . . . . ?
O3 C8 C19 C20 -178.62(19) . . . . ?
C9 C8 C19 C20 1.0(3) . . . . ?
C8 C19 C20 C21 -0.5(3) . . . . ?
C19 C20 C21 C22 -0.7(3) . . . . ?
C8 C9 C22 C21 -1.0(3) . . . . ?
C10 C9 C22 C21 177.3(2) . . . . ?
C20 C21 C22 C9 1.5(4) . . . . ?
O1' C1' C2' C14' 179.47(19) . . . . ?
C11' C1' C2' C14' 2.5(3) . . . . ?
O1' C1' C2' C3' 0.4(3) . . . . ?
C11' C1' C2' C3' -176.5(2) . . . . ?
C14' C2' C3' C4' 95.8(2) . . . . ?
C1' C2' C3' C4' -85.2(2) . . . . ?
C2' C3' C4' C15' -39.7(3) . . . . ?
C2' C3' C4' C5' 144.32(19) . . . . ?
C6' O2' C5' C18' -1.9(3) . . . . ?
C6' O2' C5' C4' 176.76(18) . . . . ?
C15' C4' C5' O2' 179.78(18) . . . . ?
C3' C4' C5' O2' -4.1(3) . . . . ?
C15' C4' C5' C18' -1.5(3) . . . . ?
C3' C4' C5' C18' 174.62(19) . . . . ?
C5' O2' C6' C7' -179.75(16) . . . 2_666 ?
C8' O3' C7' C6' -175.52(18) . . . 2_666 ?
C7' O3' C8' C19' 6.0(3) . . . . ?
C7' O3' C8' C9' -173.58(19) . . . . ?
O3' C8' C9' C22' -177.26(19) . . . . ?
C19' C8' C9' C22' 3.1(3) . . . . ?
O3' C8' C9' C10' 4.5(3) . . . . ?
C19' C8' C9' C10' -175.1(2) . . . . ?
C22' C9' C10' C11' 3.8(3) . . . . ?
C8' C9' C10' C11' -178.1(2) . . . . ?
O1' C1' C11' C12' -178.9(2) . . . . ?
C2' C1' C11' C12' -2.1(3) . . . . ?
O1' C1' C11' C10' -0.1(3) . . . . ?
C2' C1' C11' C10' 176.6(2) . . . . ?
C9' C10' C11' C1' 99.0(2) . . . . ?
C9' C10' C11' C12' -82.3(3) . . . . ?
C1' C11' C12' C13' 0.1(3) . . . . ?
C10' C11' C12' C13' -178.6(2) . . . . ?
C11' C12' C13' C14' 1.4(3) . . . . ?
C12' C13' C14' C2' -1.0(3) . . . . ?
C1' C2' C14' C13' -0.9(3) . . . . ?
C3' C2' C14' C13' 178.1(2) . . . . ?
C5' C4' C15' C16' 0.6(3) . . . . ?
C3' C4' C15' C16' -175.5(2) . . . . ?
C4' C15' C16' C17' 0.9(4) . . . . ?
C15' C16' C17' C18' -1.5(4) . . . . ?
O2' C5' C18' C17' 179.57(19) . . . . ?
C4' C5' C18' C17' 1.0(3) . . . . ?
C16' C17' C18' C5' 0.6(3) . . . . ?
O3' C8' C19' C20' 177.8(2) . . . . ?
C9' C8' C19' C20' -2.6(3) . . . . ?
C8' C19' C20' C21' 0.3(4) . . . . ?
C19' C20' C21' C22' 1.4(4) . . . . ?
C8' C9' C22' C21' -1.4(3) . . . . ?
C10' C9' C22' C21' 176.7(2) . . . . ?
C20' C21' C22' C9' -0.8(4) . . . . ?
N1 C1G C2G C3G 169.30(19) . . . . ?
C1G C2G C3G N2 173.09(19) . . . . ?

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        27.92
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.063

# Attachment '1c checkcif.pdf'

# Attachment '1c.cif'

data_1c
_database_code_depnum_ccdc_archive 'CCDC 767014'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
(3,4:9,10:18,19:24,25-tetrabenzo-5,8,20,23-tetraoxa-tricyclo
[25.3.1.112,16]dotriaconta-1(30),3,9,12,14,16(32),18, 24,27(31),
28-decaene-31,32-diol) butylenediamine hemi-salt
;
_chemical_name_common            
;
(3,4:9,10:18,19:24,25-tetrabenzo-5,8,20,23-tetraoxa-tricyclo
(25.3.1.112,16)dotriaconta-1(30),3,9,12,14,16(32),18, 24,27(31), 28-
decaene-31,32-diol) butylenediamine hemi-salt
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H39 O6,C4 H13 N2,C1 H1 Cl3'
_chemical_formula_sum            'C49 H53 Cl3 N2 O6'
_chemical_formula_weight         872.28

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'
Cl Cl 0.1484 0.1585 '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'
_space_group_name_Hall           '-P 1'
_space_group_id                  2

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

_cell_length_a                   12.8654(2)
_cell_length_b                   14.0595(2)
_cell_length_c                   14.5748(3)
_cell_angle_alpha                114.863(1)
_cell_angle_beta                 91.742(1)
_cell_angle_gamma                109.327(1)
_cell_volume                     2212.46(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)

_exptl_crystal_description       needles
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             920
_exptl_absorpt_coefficient_mu    0.259
_exptl_absorpt_correction_type   none

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(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  'Enraf Nonius Kappa CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_number            36591
_diffrn_reflns_av_R_equivalents  0.1196
_diffrn_reflns_av_sigmaI/netI    0.1693
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.54
_diffrn_reflns_theta_max         27.95
_reflns_number_total             10438
_reflns_number_gt                4440
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Nonius collect'
_computing_cell_refinement       'Nonius collect'
_computing_data_reduction        'Nonius collect'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-seed
_computing_publication_material  ciftab

_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.
Both the butylenediamine and chloroform molecules exhibited disorder.
For the former the alkyl chain was modeled over two positions with site
occupancy factors (sofs) of 0.8 and 0.2 for the major and minor components.
The non-hydrogen atoms of the major component were refined anisotropically
while those of the minor component were refined treated isotropically
throughout. All non-hydrogen atoms of the HCs were refined anisotropically,
the positions of hydrogen atoms of NH2/NH3+ and OH/O- groups were located
in electron density difference maps and these atoms were refined without
restraints. The chloroform molecule was refined with carbon, hydrogen and
one chlorine atom split over two positions with sofs of 0.5 each, while the
remaining chlorine atoms were refined over three positions with sofs of 0.5,
0.35 and 0.15. Bond length restraints and SADI cards were applied.
;

_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^)+(0.0952P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10438
_refine_ls_number_parameters     585
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.2151
_refine_ls_R_factor_gt           0.0772
_refine_ls_wR_factor_ref         0.2137
_refine_ls_wR_factor_gt          0.1640
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.050
_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 0.0655(2) 0.4695(2) 0.37051(18) 0.0368(7) Uani 1 1 d . . .
H1O H -0.019(4) 0.423(4) 0.373(4) 0.083(16) Uiso 1 1 d . . .
C1 C 0.0805(3) 0.4598(3) 0.2752(3) 0.0264(8) Uani 1 1 d . . .
O2 O 0.34929(19) 0.44672(19) 0.49263(18) 0.0295(6) Uani 1 1 d . . .
C2 C 0.1846(3) 0.4594(3) 0.2500(3) 0.0255(8) Uani 1 1 d . . .
O3 O -0.31370(18) 0.4401(2) 0.29542(19) 0.0309(6) Uani 1 1 d . . .
C3 C 0.2735(3) 0.4681(3) 0.3267(3) 0.0297(9) Uani 1 1 d . . .
H3A H 0.2602 0.5081 0.3968 0.036 Uiso 1 1 calc R . .
H3B H 0.3475 0.5161 0.3224 0.036 Uiso 1 1 calc R . .
C4 C 0.2804(3) 0.3571(3) 0.3144(3) 0.0260(8) Uani 1 1 d . . .
C5 C 0.3237(3) 0.3517(3) 0.4008(3) 0.0254(8) Uani 1 1 d . . .
C6 C 0.3958(3) 0.4462(3) 0.5834(3) 0.0295(9) Uani 1 1 d . . .
H6A H 0.4667 0.4330 0.5751 0.035 Uiso 1 1 calc R . .
H6B H 0.3423 0.3852 0.5953 0.035 Uiso 1 1 calc R . .
C7 C -0.4175(3) 0.4407(3) 0.3276(3) 0.0303(9) Uani 1 1 d . . .
H7A H -0.4489 0.3801 0.3485 0.036 Uiso 1 1 calc R . .
H7B H -0.4726 0.4267 0.2699 0.036 Uiso 1 1 calc R . .
C8 C -0.3121(3) 0.3388(3) 0.2250(3) 0.0269(8) Uani 1 1 d . . .
C9 C -0.2083(3) 0.3434(3) 0.1951(3) 0.0271(9) Uani 1 1 d . . .
C10 C -0.1132(3) 0.4585(3) 0.2342(3) 0.0306(9) Uani 1 1 d . . .
H10C H -0.1359 0.5031 0.2060 0.037 Uiso 1 1 calc R . .
H10D H -0.1031 0.4987 0.3103 0.037 Uiso 1 1 calc R . .
C11 C -0.0018(3) 0.4560(3) 0.2075(3) 0.0262(8) Uani 1 1 d . . .
C12 C 0.0224(3) 0.4509(3) 0.1131(3) 0.0300(9) Uani 1 1 d . . .
H12 H -0.0329 0.4478 0.0659 0.036 Uiso 1 1 calc R . .
C13 C 0.1244(3) 0.4503(3) 0.0864(3) 0.0328(9) Uani 1 1 d . . .
H13 H 0.1392 0.4465 0.0218 0.039 Uiso 1 1 calc R . .
C14 C 0.2043(3) 0.4554(3) 0.1554(3) 0.0303(9) Uani 1 1 d . . .
H14 H 0.2750 0.4563 0.1378 0.036 Uiso 1 1 calc R . .
C15 C 0.2518(3) 0.2627(3) 0.2194(3) 0.0342(9) Uani 1 1 d . . .
H15 H 0.2203 0.2643 0.1605 0.041 Uiso 1 1 calc R . .
C16 C 0.2679(3) 0.1657(3) 0.2082(3) 0.0373(10) Uani 1 1 d . . .
H16 H 0.2482 0.1019 0.1423 0.045 Uiso 1 1 calc R . .
C17 C 0.3130(3) 0.1632(3) 0.2939(3) 0.0347(10) Uani 1 1 d . . .
H17 H 0.3251 0.0975 0.2867 0.042 Uiso 1 1 calc R . .
C18 C 0.3406(3) 0.2550(3) 0.3897(3) 0.0308(9) Uani 1 1 d . . .
H18 H 0.3711 0.2523 0.4484 0.037 Uiso 1 1 calc R . .
C19 C -0.4034(3) 0.2365(3) 0.1860(3) 0.0315(9) Uani 1 1 d . . .
H19 H -0.4739 0.2341 0.2051 0.038 Uiso 1 1 calc R . .
C20 C -0.3911(3) 0.1379(3) 0.1192(3) 0.0392(10) Uani 1 1 d . . .
H20 H -0.4534 0.0677 0.0926 0.047 Uiso 1 1 calc R . .
C21 C -0.2894(3) 0.1403(3) 0.0907(3) 0.0399(10) Uani 1 1 d . . .
H21 H -0.2813 0.0722 0.0454 0.048 Uiso 1 1 calc R . .
C22 C -0.1991(3) 0.2430(3) 0.1288(3) 0.0341(10) Uani 1 1 d . . .
H22 H -0.1291 0.2444 0.1089 0.041 Uiso 1 1 calc R . .
O1' O -0.15355(18) -0.08457(19) 0.41390(18) 0.0309(6) Uani 1 1 d . . .
C1' C -0.2488(3) -0.1704(3) 0.3586(3) 0.0249(8) Uani 1 1 d . . .
O2' O -0.2602(2) 0.1460(2) 0.64509(18) 0.0342(6) Uani 1 1 d . . .
C2' C -0.3519(3) -0.1703(3) 0.3894(3) 0.0246(8) Uani 1 1 d . . .
O3' O 0.06879(19) -0.2355(2) 0.19874(19) 0.0347(6) Uani 1 1 d . . .
C3' C -0.3523(3) -0.0706(3) 0.4858(3) 0.0251(8) Uani 1 1 d . . .
H3'1 H -0.2856 -0.0455 0.5384 0.030 Uiso 1 1 calc R . .
H3'2 H -0.4197 -0.0965 0.5132 0.030 Uiso 1 1 calc R . .
C4' C -0.3515(3) 0.0306(3) 0.4717(3) 0.0245(8) Uani 1 1 d . . .
C5' C -0.3074(3) 0.1390(3) 0.5550(3) 0.0258(8) Uani 1 1 d . . .
C6' C -0.2285(3) 0.2500(3) 0.7372(3) 0.0330(9) Uani 1 1 d . . .
H6'1 H -0.2951 0.2689 0.7554 0.040 Uiso 1 1 calc R . .
H6'2 H -0.1736 0.3124 0.7281 0.040 Uiso 1 1 calc R . .
C7' C 0.1768(3) -0.2331(3) 0.1798(3) 0.0321(9) Uani 1 1 d . . .
H7'1 H 0.2232 -0.1594 0.1829 0.039 Uiso 1 1 calc R . .
H7'2 H 0.1707 -0.2942 0.1108 0.039 Uiso 1 1 calc R . .
C8' C 0.0114(3) -0.1971(3) 0.1511(3) 0.0286(9) Uani 1 1 d . . .
C9' C -0.0971(3) -0.2081(3) 0.1729(3) 0.0260(8) Uani 1 1 d . . .
C10' C -0.1420(3) -0.2705(3) 0.2356(3) 0.0295(9) Uani 1 1 d . . .
H10A H -0.1531 -0.3510 0.1942 0.035 Uiso 1 1 calc R . .
H10B H -0.0839 -0.2390 0.2979 0.035 Uiso 1 1 calc R . .
C11' C -0.2498(3) -0.2654(3) 0.2692(3) 0.0251(8) Uani 1 1 d . . .
C12' C -0.3513(3) -0.3555(3) 0.2133(3) 0.0289(9) Uani 1 1 d . . .
H12' H -0.3513 -0.4192 0.1536 0.035 Uiso 1 1 calc R . .
C13' C -0.4522(3) -0.3536(3) 0.2433(3) 0.0305(9) Uani 1 1 d . . .
H13' H -0.5210 -0.4149 0.2043 0.037 Uiso 1 1 calc R . .
C14' C -0.4509(3) -0.2605(3) 0.3312(3) 0.0287(9) Uani 1 1 d . . .
H14' H -0.5198 -0.2589 0.3520 0.034 Uiso 1 1 calc R . .
C15' C -0.3995(3) 0.0196(3) 0.3795(3) 0.0325(9) Uani 1 1 d . . .
H15' H -0.4293 -0.0532 0.3215 0.039 Uiso 1 1 calc R . .
C16' C -0.4055(3) 0.1118(3) 0.3694(3) 0.0375(10) Uani 1 1 d . . .
H16' H -0.4392 0.1016 0.3053 0.045 Uiso 1 1 calc R . .
C17' C -0.3624(3) 0.2180(3) 0.4528(3) 0.0345(10) Uani 1 1 d . . .
H17' H -0.3674 0.2811 0.4466 0.041 Uiso 1 1 calc R . .
C18' C -0.3114(3) 0.2328(3) 0.5459(3) 0.0297(9) Uani 1 1 d . . .
H18' H -0.2795 0.3062 0.6030 0.036 Uiso 1 1 calc R . .
C19' C 0.0539(3) -0.1484(3) 0.0883(3) 0.0323(9) Uani 1 1 d . . .
H19' H 0.1268 -0.1414 0.0739 0.039 Uiso 1 1 calc R . .
C20' C -0.0115(3) -0.1100(3) 0.0471(3) 0.0424(11) Uani 1 1 d . . .
H20' H 0.0163 -0.0782 0.0025 0.051 Uiso 1 1 calc R . .
C21' C -0.1159(3) -0.1168(3) 0.0693(3) 0.0427(11) Uani 1 1 d . . .
H21' H -0.1593 -0.0885 0.0414 0.051 Uiso 1 1 calc R . .
C22' C -0.1577(3) -0.1655(3) 0.1328(3) 0.0337(9) Uani 1 1 d . . .
H22' H -0.2295 -0.1693 0.1488 0.040 Uiso 1 1 calc R . .
Cl1A Cl -0.4318(3) -0.3230(3) -0.0482(2) 0.0594(10) Uiso 0.50 1 d PD A 5
Cl2A Cl -0.4641(4) -0.1395(3) 0.1014(3) 0.0473(10) Uiso 0.35 1 d PD A 5
Cl3A Cl -0.6450(3) -0.3630(5) 0.0176(3) 0.0422(11) Uiso 0.35 1 d PD A 5
Cl2B Cl -0.5197(8) -0.1574(5) 0.1098(6) 0.066(3) Uiso 0.15 1 d PD B 6
Cl3B Cl -0.6418(6) -0.3906(6) 0.0309(7) 0.053(3) Uiso 0.15 1 d PD C 6
Cl1C Cl -0.4334(2) -0.3524(2) -0.0418(2) 0.0418(8) Uiso 0.50 1 d PD D 2
Cl2C Cl -0.4239(2) -0.1237(2) 0.08901(19) 0.0507(8) Uiso 0.50 1 d PD D 2
Cl3C Cl -0.6261(3) -0.3199(3) 0.0332(3) 0.0629(10) Uiso 0.50 1 d P D 2
N1 N -0.1144(3) 0.3570(3) 0.4072(3) 0.0421(9) Uani 1 1 d . . .
H1NA H -0.116(3) 0.400(3) 0.476(3) 0.037(11) Uiso 1 1 d . . .
H1NB H -0.185(5) 0.330(4) 0.364(4) 0.10(2) Uiso 1 1 d . . .
N2 N 0.0503(3) 0.0053(4) 0.3898(3) 0.0423(10) Uani 1 1 d . . .
H2NC H -0.037(4) -0.043(4) 0.394(4) 0.086(16) Uiso 1 1 d . . .
H2NB H 0.069(3) -0.037(3) 0.346(3) 0.034(13) Uiso 1 1 d . . .
H2NA H 0.104(4) 0.037(3) 0.454(4) 0.053(13) Uiso 1 1 d . . .
C1G C -0.0973(4) 0.2533(5) 0.3920(4) 0.0363(13) Uani 0.80 1 d P E 3
H1G1 H -0.0879 0.2130 0.3204 0.044 Uiso 0.80 1 calc PR E 3
H1G2 H -0.1635 0.2021 0.4038 0.044 Uiso 0.80 1 calc PR E 3
C2G C 0.0075(5) 0.2863(5) 0.4681(4) 0.0439(14) Uani 0.80 1 d P E 3
H2G1 H 0.0744 0.3258 0.4474 0.053 Uiso 0.80 1 calc PR E 3
H2G2 H 0.0038 0.3402 0.5374 0.053 Uiso 0.80 1 calc PR E 3
C3G C 0.0213(5) 0.1870(5) 0.4742(5) 0.0411(17) Uani 0.80 1 d P E 3
H3G1 H -0.0467 0.1463 0.4928 0.049 Uiso 0.80 1 calc PR E 3
H3G2 H 0.0859 0.2156 0.5302 0.049 Uiso 0.80 1 calc PR E 3
C4G C 0.0400(6) 0.1046(8) 0.3756(7) 0.0372(18) Uani 0.80 1 d P E 3
H4G1 H 0.1096 0.1434 0.3575 0.045 Uiso 0.80 1 calc PR E 3
H4G2 H -0.0237 0.0757 0.3187 0.045 Uiso 0.80 1 calc PR E 3
C5G C -0.5025(6) -0.2863(5) 0.0539(8) 0.069(5) Uiso 0.50 1 d PD A 5
H5G H -0.4718 -0.3005 0.1087 0.083 Uiso 0.50 1 calc PR A 5
C1G' C -0.055(3) 0.306(2) 0.463(2) 0.055(7) Uiso 0.20 1 d P E 4
H1G3 H 0.0119 0.3674 0.5152 0.066 Uiso 0.20 1 calc PR E 4
H1G4 H -0.1078 0.2709 0.4980 0.066 Uiso 0.20 1 calc PR E 4
C2G' C -0.022(2) 0.223(2) 0.385(2) 0.064(7) Uiso 0.20 1 d P E 4
H2G3 H 0.0416 0.2612 0.3609 0.077 Uiso 0.20 1 calc PR E 4
H2G4 H -0.0856 0.1722 0.3257 0.077 Uiso 0.20 1 calc PR E 4
C3G' C 0.014(3) 0.147(3) 0.428(3) 0.047(9) Uiso 0.20 1 d P E 4
H3G3 H 0.0769 0.1976 0.4883 0.056 Uiso 0.20 1 calc PR E 4
H3G4 H -0.0500 0.1073 0.4513 0.056 Uiso 0.20 1 calc PR E 4
C4G' C 0.047(4) 0.068(4) 0.351(4) 0.064(15) Uiso 0.20 1 d P E 4
H4G3 H -0.0085 0.0265 0.2857 0.077 Uiso 0.20 1 calc PR E 4
H4G4 H 0.1217 0.1053 0.3392 0.077 Uiso 0.20 1 calc PR E 4
C5G' C -0.4794(9) -0.2668(5) 0.0608(6) 0.036(3) Uiso 0.50 1 d PD D 2
H5G' H -0.4553 -0.2726 0.1235 0.043 Uiso 0.50 1 calc PR D 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 0.0323(15) 0.0498(17) 0.0328(16) 0.0249(14) 0.0097(12) 0.0125(13)
C1 0.027(2) 0.0233(19) 0.030(2) 0.0131(17) 0.0055(16) 0.0093(16)
O2 0.0322(14) 0.0304(14) 0.0269(14) 0.0124(13) 0.0011(11) 0.0144(11)
C2 0.029(2) 0.0196(18) 0.027(2) 0.0102(17) 0.0010(16) 0.0093(15)
O3 0.0232(13) 0.0286(14) 0.0354(15) 0.0091(12) 0.0061(11) 0.0104(11)
C3 0.0272(19) 0.025(2) 0.037(2) 0.0140(18) 0.0021(16) 0.0115(16)
C4 0.0214(18) 0.025(2) 0.030(2) 0.0108(18) 0.0036(15) 0.0097(15)
C5 0.0197(17) 0.027(2) 0.028(2) 0.0097(18) 0.0061(15) 0.0099(15)
C6 0.0256(19) 0.040(2) 0.031(2) 0.0199(19) 0.0071(16) 0.0169(17)
C7 0.0221(19) 0.037(2) 0.034(2) 0.0164(19) 0.0055(16) 0.0129(16)
C8 0.0263(19) 0.029(2) 0.025(2) 0.0114(18) 0.0013(15) 0.0120(16)
C9 0.027(2) 0.031(2) 0.025(2) 0.0139(18) 0.0011(15) 0.0109(16)
C10 0.0250(19) 0.029(2) 0.039(2) 0.0143(18) 0.0042(16) 0.0130(16)
C11 0.0248(19) 0.0232(19) 0.029(2) 0.0105(17) 0.0031(16) 0.0094(15)
C12 0.031(2) 0.027(2) 0.027(2) 0.0116(17) -0.0026(16) 0.0072(16)
C13 0.037(2) 0.034(2) 0.021(2) 0.0104(18) 0.0072(17) 0.0092(18)
C14 0.0241(19) 0.028(2) 0.034(2) 0.0089(18) 0.0102(17) 0.0100(16)
C15 0.036(2) 0.035(2) 0.034(2) 0.016(2) 0.0049(17) 0.0151(18)
C16 0.044(2) 0.030(2) 0.033(2) 0.0071(19) 0.0061(18) 0.0179(18)
C17 0.041(2) 0.028(2) 0.044(3) 0.017(2) 0.0129(19) 0.0215(18)
C18 0.030(2) 0.033(2) 0.036(2) 0.019(2) 0.0110(17) 0.0158(17)
C19 0.0250(19) 0.032(2) 0.033(2) 0.0140(19) 0.0030(16) 0.0066(17)
C20 0.038(2) 0.032(2) 0.035(2) 0.010(2) 0.0033(18) 0.0050(19)
C21 0.048(3) 0.031(2) 0.032(2) 0.0064(19) 0.0059(19) 0.015(2)
C22 0.032(2) 0.031(2) 0.039(2) 0.014(2) 0.0109(18) 0.0126(17)
O1' 0.0215(13) 0.0309(14) 0.0282(14) 0.0067(12) 0.0024(11) 0.0049(11)
C1' 0.0237(19) 0.026(2) 0.025(2) 0.0132(17) 0.0018(15) 0.0078(16)
O2' 0.0426(15) 0.0280(14) 0.0278(15) 0.0072(12) 0.0007(12) 0.0163(12)
C2' 0.0250(19) 0.0268(19) 0.029(2) 0.0156(17) 0.0069(16) 0.0135(16)
O3' 0.0286(14) 0.0534(17) 0.0397(16) 0.0291(14) 0.0140(12) 0.0250(12)
C3' 0.0241(18) 0.0264(19) 0.027(2) 0.0119(17) 0.0071(15) 0.0129(15)
C4' 0.0186(17) 0.028(2) 0.031(2) 0.0148(18) 0.0113(15) 0.0119(15)
C5' 0.0215(18) 0.032(2) 0.026(2) 0.0136(18) 0.0064(15) 0.0120(16)
C6' 0.030(2) 0.034(2) 0.032(2) 0.0089(19) 0.0085(17) 0.0177(17)
C7' 0.030(2) 0.038(2) 0.030(2) 0.0111(19) 0.0108(17) 0.0190(17)
C8' 0.033(2) 0.027(2) 0.024(2) 0.0073(17) 0.0026(16) 0.0145(17)
C9' 0.029(2) 0.026(2) 0.0213(19) 0.0083(17) 0.0039(15) 0.0111(16)
C10' 0.031(2) 0.031(2) 0.031(2) 0.0152(18) 0.0086(16) 0.0153(17)
C11' 0.0278(19) 0.029(2) 0.027(2) 0.0174(18) 0.0054(15) 0.0137(16)
C12' 0.037(2) 0.024(2) 0.023(2) 0.0090(17) 0.0025(16) 0.0110(17)
C13' 0.0223(19) 0.032(2) 0.032(2) 0.0142(19) -0.0004(16) 0.0039(16)
C14' 0.0222(18) 0.035(2) 0.033(2) 0.0182(19) 0.0091(16) 0.0112(16)
C15' 0.037(2) 0.028(2) 0.027(2) 0.0103(18) 0.0044(17) 0.0096(17)
C16' 0.044(2) 0.041(2) 0.033(2) 0.020(2) 0.0084(18) 0.0176(19)
C17' 0.035(2) 0.037(2) 0.044(3) 0.027(2) 0.0121(19) 0.0171(18)
C18' 0.028(2) 0.026(2) 0.034(2) 0.0119(18) 0.0103(17) 0.0119(16)
C19' 0.035(2) 0.036(2) 0.027(2) 0.0159(19) 0.0089(17) 0.0125(18)
C20' 0.046(3) 0.050(3) 0.042(3) 0.030(2) 0.015(2) 0.019(2)
C21' 0.047(3) 0.054(3) 0.042(3) 0.032(2) 0.007(2) 0.022(2)
C22' 0.032(2) 0.039(2) 0.036(2) 0.020(2) 0.0068(17) 0.0168(18)
N1 0.042(2) 0.053(2) 0.040(2) 0.028(2) 0.0112(19) 0.0180(19)
N2 0.030(2) 0.049(2) 0.026(2) 0.004(2) 0.0062(17) 0.0074(18)
C1G 0.031(3) 0.042(3) 0.032(3) 0.019(3) 0.004(2) 0.007(2)
C2G 0.052(4) 0.034(3) 0.034(3) 0.013(3) -0.006(3) 0.007(3)
C3G 0.058(4) 0.028(3) 0.031(4) 0.010(3) 0.000(3) 0.013(3)
C4G 0.028(3) 0.044(5) 0.034(5) 0.022(4) 0.006(3) 0.003(4)

_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 1.363(4) . ?
C1 C11 1.398(5) . ?
C1 C2 1.400(5) . ?
O2 C5 1.365(4) . ?
O2 C6 1.439(4) . ?
C2 C14 1.390(5) . ?
C2 C3 1.512(5) . ?
O3 C8 1.368(4) . ?
O3 C7 1.431(4) . ?
C3 C4 1.529(5) . ?
C4 C15 1.383(5) . ?
C4 C5 1.401(5) . ?
C5 C18 1.392(5) . ?
C6 C7 1.496(5) 2_566 ?
C7 C6 1.496(5) 2_566 ?
C8 C19 1.389(5) . ?
C8 C9 1.406(5) . ?
C9 C22 1.384(5) . ?
C9 C10 1.520(5) . ?
C10 C11 1.504(5) . ?
C11 C12 1.398(5) . ?
C12 C13 1.381(5) . ?
C13 C14 1.380(5) . ?
C15 C16 1.391(5) . ?
C16 C17 1.380(5) . ?
C17 C18 1.376(5) . ?
C19 C20 1.384(5) . ?
C20 C21 1.379(5) . ?
C21 C22 1.385(5) . ?
O1' C1' 1.323(4) . ?
C1' C2' 1.414(5) . ?
C1' C11' 1.417(5) . ?
O2' C5' 1.380(4) . ?
O2' C6' 1.424(4) . ?
C2' C14' 1.382(5) . ?
C2' C3' 1.512(5) . ?
O3' C8' 1.366(4) . ?
O3' C7' 1.417(4) . ?
C3' C4' 1.517(5) . ?
C4' C15' 1.387(5) . ?
C4' C5' 1.396(5) . ?
C5' C18' 1.397(5) . ?
C6' C7' 1.503(5) 2_556 ?
C7' C6' 1.503(5) 2_556 ?
C8' C19' 1.384(5) . ?
C8' C9' 1.414(5) . ?
C9' C22' 1.372(5) . ?
C9' C10' 1.520(5) . ?
C10' C11' 1.499(5) . ?
C11' C12' 1.395(5) . ?
C12' C13' 1.387(5) . ?
C13' C14' 1.389(5) . ?
C15' C16' 1.391(5) . ?
C16' C17' 1.378(5) . ?
C17' C18' 1.391(5) . ?
C19' C20' 1.379(5) . ?
C20' C21' 1.374(6) . ?
C21' C22' 1.391(5) . ?
Cl1A C5G 1.748(6) . ?
Cl2A C5G 1.757(6) . ?
Cl3A C5G 1.719(7) . ?
Cl1C C5G' 1.746(6) . ?
Cl2C C5G' 1.750(6) . ?
Cl3C C5G' 1.746(11) . ?
N1 C1G 1.471(6) . ?
N1 C1G' 1.60(3) . ?
N2 C4G' 1.24(5) . ?
N2 C4G 1.541(10) . ?
C1G C2G 1.525(7) . ?
C2G C3G 1.503(8) . ?
C3G C4G 1.507(11) . ?
C1G' C2G' 1.44(4) . ?
C2G' C3G' 1.61(4) . ?
C3G' C4G' 1.40(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C11 121.7(3) . . ?
O1 C1 C2 117.0(3) . . ?
C11 C1 C2 121.2(3) . . ?
C5 O2 C6 117.9(3) . . ?
C14 C2 C1 118.2(3) . . ?
C14 C2 C3 121.9(3) . . ?
C1 C2 C3 119.9(3) . . ?
C8 O3 C7 117.6(2) . . ?
C2 C3 C4 116.8(3) . . ?
C15 C4 C5 118.3(3) . . ?
C15 C4 C3 122.2(3) . . ?
C5 C4 C3 119.4(3) . . ?
O2 C5 C18 123.9(3) . . ?
O2 C5 C4 115.8(3) . . ?
C18 C5 C4 120.4(3) . . ?
O2 C6 C7 107.4(3) . 2_566 ?
O3 C7 C6 108.5(3) . 2_566 ?
O3 C8 C19 124.2(3) . . ?
O3 C8 C9 115.2(3) . . ?
C19 C8 C9 120.6(3) . . ?
C22 C9 C8 118.2(3) . . ?
C22 C9 C10 123.2(3) . . ?
C8 C9 C10 118.6(3) . . ?
C11 C10 C9 115.6(3) . . ?
C12 C11 C1 118.0(3) . . ?
C12 C11 C10 120.1(3) . . ?
C1 C11 C10 121.9(3) . . ?
C13 C12 C11 121.8(3) . . ?
C14 C13 C12 118.8(3) . . ?
C13 C14 C2 122.0(3) . . ?
C4 C15 C16 121.5(4) . . ?
C17 C16 C15 119.3(4) . . ?
C18 C17 C16 120.6(4) . . ?
C17 C18 C5 120.0(4) . . ?
C20 C19 C8 119.5(3) . . ?
C21 C20 C19 120.8(3) . . ?
C20 C21 C22 119.4(4) . . ?
C9 C22 C21 121.5(4) . . ?
O1' C1' C2' 120.4(3) . . ?
O1' C1' C11' 121.1(3) . . ?
C2' C1' C11' 118.5(3) . . ?
C5' O2' C6' 118.7(3) . . ?
C14' C2' C1' 119.9(3) . . ?
C14' C2' C3' 120.9(3) . . ?
C1' C2' C3' 119.3(3) . . ?
C8' O3' C7' 119.7(3) . . ?
C2' C3' C4' 115.4(3) . . ?
C15' C4' C5' 117.4(3) . . ?
C15' C4' C3' 122.4(3) . . ?
C5' C4' C3' 120.1(3) . . ?
O2' C5' C4' 115.4(3) . . ?
O2' C5' C18' 123.2(3) . . ?
C4' C5' C18' 121.4(3) . . ?
O2' C6' C7' 106.5(3) . 2_556 ?
O3' C7' C6' 106.2(3) . 2_556 ?
O3' C8' C19' 124.5(3) . . ?
O3' C8' C9' 114.4(3) . . ?
C19' C8' C9' 121.0(4) . . ?
C22' C9' C8' 118.1(3) . . ?
C22' C9' C10' 123.6(3) . . ?
C8' C9' C10' 118.3(3) . . ?
C11' C10' C9' 116.0(3) . . ?
C12' C11' C1' 119.9(3) . . ?
C12' C11' C10' 119.9(3) . . ?
C1' C11' C10' 120.2(3) . . ?
C13' C12' C11' 121.1(3) . . ?
C12' C13' C14' 118.9(3) . . ?
C2' C14' C13' 121.7(3) . . ?
C4' C15' C16' 122.1(3) . . ?
C17' C16' C15' 119.7(4) . . ?
C16' C17' C18' 119.9(4) . . ?
C17' C18' C5' 119.6(3) . . ?
C20' C19' C8' 118.9(4) . . ?
C21' C20' C19' 121.3(4) . . ?
C20' C21' C22' 119.4(4) . . ?
C9' C22' C21' 121.3(4) . . ?
C1G N1 C1G' 37.1(10) . . ?
C4G' N2 C4G 18(2) . . ?
N1 C1G C2G 108.6(5) . . ?
C3G C2G C1G 113.4(4) . . ?
C2G C3G C4G 113.9(6) . . ?
C3G C4G N2 109.5(5) . . ?
Cl3A C5G Cl1A 112.9(5) . . ?
Cl3A C5G Cl2A 114.4(5) . . ?
Cl1A C5G Cl2A 103.9(4) . . ?
C2G' C1G' N1 108(2) . . ?
C1G' C2G' C3G' 112(3) . . ?
C4G' C3G' C2G' 111(4) . . ?
N2 C4G' C3G' 102(4) . . ?
Cl1C C5G' Cl3C 108.6(5) . . ?
Cl1C C5G' Cl2C 113.7(5) . . ?
Cl3C C5G' Cl2C 110.7(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
O1 C1 C2 C14 -176.7(3) . . . . ?
C11 C1 C2 C14 0.2(5) . . . . ?
O1 C1 C2 C3 0.7(5) . . . . ?
C11 C1 C2 C3 177.6(3) . . . . ?
C14 C2 C3 C4 -86.8(4) . . . . ?
C1 C2 C3 C4 95.9(4) . . . . ?
C2 C3 C4 C15 30.3(5) . . . . ?
C2 C3 C4 C5 -153.8(3) . . . . ?
C6 O2 C5 C18 -0.5(4) . . . . ?
C6 O2 C5 C4 -179.0(3) . . . . ?
C15 C4 C5 O2 -179.3(3) . . . . ?
C3 C4 C5 O2 4.6(4) . . . . ?
C15 C4 C5 C18 2.1(5) . . . . ?
C3 C4 C5 C18 -174.0(3) . . . . ?
C5 O2 C6 C7 179.3(3) . . . 2_566 ?
C8 O3 C7 C6 170.4(3) . . . 2_566 ?
C7 O3 C8 C19 -2.5(5) . . . . ?
C7 O3 C8 C9 179.1(3) . . . . ?
O3 C8 C9 C22 176.3(3) . . . . ?
C19 C8 C9 C22 -2.2(5) . . . . ?
O3 C8 C9 C10 -5.6(5) . . . . ?
C19 C8 C9 C10 175.9(3) . . . . ?
C22 C9 C10 C11 -7.6(5) . . . . ?
C8 C9 C10 C11 174.4(3) . . . . ?
O1 C1 C11 C12 177.3(3) . . . . ?
C2 C1 C11 C12 0.5(5) . . . . ?
O1 C1 C11 C10 -2.2(5) . . . . ?
C2 C1 C11 C10 -178.9(3) . . . . ?
C9 C10 C11 C12 85.9(4) . . . . ?
C9 C10 C11 C1 -94.7(4) . . . . ?
C1 C11 C12 C13 -0.5(5) . . . . ?
C10 C11 C12 C13 179.0(3) . . . . ?
C11 C12 C13 C14 -0.3(5) . . . . ?
C12 C13 C14 C2 1.0(5) . . . . ?
C1 C2 C14 C13 -0.9(5) . . . . ?
C3 C2 C14 C13 -178.3(3) . . . . ?
C5 C4 C15 C16 -1.8(5) . . . . ?
C3 C4 C15 C16 174.2(3) . . . . ?
C4 C15 C16 C17 0.4(5) . . . . ?
C15 C16 C17 C18 0.7(5) . . . . ?
C16 C17 C18 C5 -0.4(5) . . . . ?
O2 C5 C18 C17 -179.5(3) . . . . ?
C4 C5 C18 C17 -1.1(5) . . . . ?
O3 C8 C19 C20 -176.6(3) . . . . ?
C9 C8 C19 C20 1.7(5) . . . . ?
C8 C19 C20 C21 -0.2(6) . . . . ?
C19 C20 C21 C22 -0.7(6) . . . . ?
C8 C9 C22 C21 1.2(6) . . . . ?
C10 C9 C22 C21 -176.8(3) . . . . ?
C20 C21 C22 C9 0.2(6) . . . . ?
O1' C1' C2' C14' -179.8(3) . . . . ?
C11' C1' C2' C14' -1.4(5) . . . . ?
O1' C1' C2' C3' 0.4(5) . . . . ?
C11' C1' C2' C3' 178.8(3) . . . . ?
C14' C2' C3' C4' -96.7(4) . . . . ?
C1' C2' C3' C4' 83.1(4) . . . . ?
C2' C3' C4' C15' 29.8(5) . . . . ?
C2' C3' C4' C5' -154.1(3) . . . . ?
C6' O2' C5' C4' -170.8(3) . . . . ?
C6' O2' C5' C18' 9.3(5) . . . . ?
C15' C4' C5' O2' -179.9(3) . . . . ?
C3' C4' C5' O2' 3.8(4) . . . . ?
C15' C4' C5' C18' 0.0(5) . . . . ?
C3' C4' C5' C18' -176.3(3) . . . . ?
C5' O2' C6' C7' -178.1(3) . . . 2_556 ?
C8' O3' C7' C6' 165.1(3) . . . 2_556 ?
C7' O3' C8' C19' -4.0(5) . . . . ?
C7' O3' C8' C9' 177.6(3) . . . . ?
O3' C8' C9' C22' 176.3(3) . . . . ?
C19' C8' C9' C22' -2.2(5) . . . . ?
O3' C8' C9' C10' -6.1(4) . . . . ?
C19' C8' C9' C10' 175.4(3) . . . . ?
C22' C9' C10' C11' -10.9(5) . . . . ?
C8' C9' C10' C11' 171.6(3) . . . . ?
O1' C1' C11' C12' 179.0(3) . . . . ?
C2' C1' C11' C12' 0.7(5) . . . . ?
O1' C1' C11' C10' 0.1(5) . . . . ?
C2' C1' C11' C10' -178.2(3) . . . . ?
C9' C10' C11' C12' 98.5(4) . . . . ?
C9' C10' C11' C1' -82.7(4) . . . . ?
C1' C11' C12' C13' 0.4(5) . . . . ?
C10' C11' C12' C13' 179.3(3) . . . . ?
C11' C12' C13' C14' -0.7(5) . . . . ?
C1' C2' C14' C13' 1.2(5) . . . . ?
C3' C2' C14' C13' -179.1(3) . . . . ?
C12' C13' C14' C2' -0.1(5) . . . . ?
C5' C4' C15' C16' -0.8(5) . . . . ?
C3' C4' C15' C16' 175.4(3) . . . . ?
C4' C15' C16' C17' 0.3(6) . . . . ?
C15' C16' C17' C18' 1.1(5) . . . . ?
C16' C17' C18' C5' -1.9(5) . . . . ?
O2' C5' C18' C17' -178.8(3) . . . . ?
C4' C5' C18' C17' 1.3(5) . . . . ?
O3' C8' C19' C20' -178.1(3) . . . . ?
C9' C8' C19' C20' 0.2(5) . . . . ?
C8' C19' C20' C21' 1.6(6) . . . . ?
C19' C20' C21' C22' -1.3(6) . . . . ?
C8' C9' C22' C21' 2.5(5) . . . . ?
C10' C9' C22' C21' -175.0(3) . . . . ?
C20' C21' C22' C9' -0.8(6) . . . . ?
C1G' N1 C1G C2G -21.8(16) . . . . ?
N1 C1G C2G C3G 168.9(4) . . . . ?
C1G C2G C3G C4G 64.7(7) . . . . ?
C2G C3G C4G N2 -178.7(5) . . . . ?
C4G' N2 C4G C3G -179(8) . . . . ?
C1G N1 C1G' C2G' 32.4(15) . . . . ?
N1 C1G' C2G' C3G' -167.7(19) . . . . ?
C1G' C2G' C3G' C4G' -179(3) . . . . ?
C4G N2 C4G' C3G' -7(5) . . . . ?
C2G' C3G' C4G' N2 -168(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        27.95
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.809
_refine_diff_density_rms         0.071