# Supplementary Material (ESI) for Organic & Biomolecular Chemistry
# This journal is © The Royal Society of Chemistry 2004



data_global
_journal_name_full               Org.Biomol.Chem.

_journal_coden_Cambridge         0177

_publ_contact_author_name        'Prof. Francois Diederich'
_publ_contact_author_address     
;
Department of Chemistry
ETH Zuerich
ETH Hoenggerberg
HCI G313
Zuerich
CH-8093
SWITZERLAND
;
_publ_contact_author_email       DIEDERICH@ORG.CHEM.ETHZ.CH

_publ_section_title              
;
New Rebek imide-type receptors for adenine featuring acetylene-linked
pi-stacking platforms
;

_publ_section_references         
;
Mackay, S., Gilmore, C. J.,Edwards, C., Stewart, N. & Shankland, K.
(1999). maXus  Computer Program for the Solution and Refinement of
Crystal Structures. Bruker Nonius, The Netherlands, MacScience, Japan
& The University of Glasgow.

Johnson, C. K. (1976). ORTEP-II. A Fortran Thermal-Ellipsoid Plot
Program. Report ORNL-5138. Oak Ridge National Laboratory, Oak Ridge,
Tennessee, USA.

Otwinowski, Z. and Minor, W, (1997). In Methods in Enzymology, 276,
edited by C.W. Carter, Jr. & R.M. Sweet pp. 307-326,
New York:Academic Press.

Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L.,
Giacovazzo, C., Guagliardi, A., Moliterni, A.G.G & Spagna, R.
(1999). J. Appl. Cryst. 32, 115-119.

Sheldrick, G. M. (1997).  SHELXL97.  Program for the Refinement of Crystal
Structures.  University of Gottingen, Germany.

;
loop_
_publ_author_name
'Raffaella Faraoni'
'Muriel Blanzat'
'Stefan Kubicek'
'Christophe Braun'
'Bernd Schweizer'
'Volker Gramlich'
;
F.Diedrich
;

data_compound_6
_database_code_depnum_ccdc_archive 'CCDC 234432'

_audit_creation_method           maXus

_chemical_compound_source        'Diederich Group'
_exptl_crystal_description       Cube
_exptl_crystal_size_max          .3
_exptl_crystal_size_mid          .2
_exptl_crystal_size_min          .2
_exptl_crystal_colour            Colourless
_cell_measurement_temperature    172
_refine_ls_hydrogen_treatment    refall

_diffrn_measurement_device       KappaCCD
_computing_data_collection       KappaCCD
_computing_data_reduction        'Denzo and Scalepak (Otwinowski & Minor, 1997)'

_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26

loop_
_diffrn_radiation_wavelength
0.71073
_diffrn_radiation_wavelength_id  all

_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.03694
_diffrn_orient_matrix_UB_12      0.00705
_diffrn_orient_matrix_UB_13      0.05949
_diffrn_orient_matrix_UB_21      -0.03468
_diffrn_orient_matrix_UB_22      0.06763
_diffrn_orient_matrix_UB_23      0.01352
_diffrn_orient_matrix_UB_31      -0.02787
_diffrn_orient_matrix_UB_32      -0.02207
_diffrn_orient_matrix_UB_33      0.03892

_cell_formula_units_Z            8
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_density_method    'not measured'
_exptl_special_details           
;
?
;
_chemical_formula_weight         346.430
_diffrn_radiation_type           ' MoK\a'

loop_
_symmetry_equiv_pos_as_xyz
+X,+Y,+Z
-X,-Y,-Z
'-X+ 1/2,+Y+ 1/2,-Z'
'+X+ 1/2,-Y+ 1/2,+Z'

_symmetry_space_group_name_H-M   'P 21/a        '
_symmetry_cell_setting           Monoclinic
_chemical_formula_moiety         'C22 H22 N2 O2 '
_chemical_formula_sum            'C22 H22 N2 O2 '
_chemical_name_systematic        
;
?
;
_cell_length_a                   14.9171(2)
_cell_length_b                   12.9531(2)
_cell_length_c                   19.9159(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.7345(8)
_cell_angle_gamma                90.00
_cell_volume                     3665.33(9)
_diffrn_reflns_number            17878
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         2.04
_diffrn_reflns_theta_full        28.70
_cell_measurement_reflns_used    9267
_cell_measurement_theta_min      0.998
_cell_measurement_theta_max      28.700
_diffrn_measurement_method       CCD
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_diffrn_reflns_av_R_equivalents  0.030
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?

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'

_exptl_absorpt_coefficient_mu    0.081
_reflns_number_total             9409
_reflns_number_gt                7284
_reflns_threshold_expression     >2sigma(I)

_computing_structure_solution    'SIR97 (Altomare, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+ (0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9409
_refine_ls_number_parameters     645
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0485
_refine_ls_wR_factor_ref         0.1541
_refine_ls_wR_factor_gt          0.1391
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.352
_refine_ls_shift/su_mean         0.035

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
O25 O 0.61111(8) 0.26923(8) 0.33812(5) 0.0393(2) Uani 1 1 d . . .
O26 O 0.55871(8) 0.26621(8) 0.10355(5) 0.0433(3) Uani 1 1 d . . .
O51 O 0.39686(8) 0.84691(7) 0.31260(5) 0.0399(2) Uani 1 1 d . . .
O52 O 0.34755(7) 0.52852(7) 0.37969(5) 0.0352(2) Uani 1 1 d . . .
N23 N 0.33753(8) 0.60099(9) 0.20959(5) 0.0321(3) Uani 1 1 d . . .
N24 N 0.59486(8) 0.26072(9) 0.22195(5) 0.0283(2) Uani 1 1 d . . .
N49 N 0.59353(7) 0.49004(8) 0.23567(5) 0.0278(2) Uani 1 1 d . . .
N50 N 0.35261(7) 0.69328(8) 0.34519(5) 0.0270(2) Uani 1 1 d . . .
C1 C 0.59392(9) 0.21653(10) 0.28489(6) 0.0279(3) Uani 1 1 d . . .
C2 C 0.56972(9) 0.10254(10) 0.28369(6) 0.0279(3) Uani 1 1 d . . .
C3 C 0.46290(9) 0.09030(11) 0.27074(7) 0.0300(3) Uani 1 1 d . . .
C4 C 0.39790(9) 0.12131(10) 0.19704(7) 0.0305(3) Uani 1 1 d . . .
C5 C 0.43855(10) 0.08103(11) 0.13925(7) 0.0316(3) Uani 1 1 d . . .
C6 C 0.54508(9) 0.09913(10) 0.15325(6) 0.0299(3) Uani 1 1 d . . .
C7 C 0.56605(9) 0.21478(10) 0.15598(7) 0.0300(3) Uani 1 1 d . . .
C8 C 0.59805(10) 0.05070(11) 0.22421(7) 0.0311(3) Uani 1 1 d . . .
C9 C 0.62161(11) 0.05350(12) 0.35486(7) 0.0375(3) Uani 1 1 d . . .
C10 C 0.30036(11) 0.07282(14) 0.18755(10) 0.0439(4) Uani 1 1 d . . .
C11 C 0.57574(13) 0.05158(13) 0.09320(8) 0.0417(4) Uani 1 1 d . . .
C12 C 0.38417(9) 0.23452(11) 0.18894(7) 0.0307(3) Uani 1 1 d . . .
C13 C 0.36869(9) 0.32436(11) 0.17709(7) 0.0309(3) Uani 1 1 d . . .
C14 C 0.35332(9) 0.43216(10) 0.16289(7) 0.0285(3) Uani 1 1 d . . .
C15 C 0.33917(9) 0.47323(11) 0.09651(7) 0.0308(3) Uani 1 1 d . . .
C16 C 0.32354(9) 0.57997(11) 0.08532(6) 0.0306(3) Uani 1 1 d . . .
C17 C 0.30927(11) 0.62778(13) 0.01874(7) 0.0410(3) Uani 1 1 d . . .
C18 C 0.29511(12) 0.73131(14) 0.01078(8) 0.0466(4) Uani 1 1 d . . .
C19 C 0.29469(12) 0.79316(13) 0.06917(9) 0.0456(4) Uani 1 1 d . . .
C20 C 0.30885(11) 0.75019(12) 0.13429(8) 0.0400(3) Uani 1 1 d . . .
C21 C 0.32329(9) 0.64253(11) 0.14360(7) 0.0306(3) Uani 1 1 d . . .
C22 C 0.35187(9) 0.50133(11) 0.21796(7) 0.0304(3) Uani 1 1 d . . .
C27 C 0.38098(9) 0.79482(10) 0.35864(6) 0.0278(3) Uani 1 1 d . . .
C28 C 0.38927(9) 0.83638(9) 0.43208(6) 0.0267(3) Uani 1 1 d . . .
C29 C 0.49227(9) 0.83121(10) 0.48023(7) 0.0271(3) Uani 1 1 d . . .
C30 C 0.53396(8) 0.72172(10) 0.49901(6) 0.0258(3) Uani 1 1 d . . .
C31 C 0.46220(9) 0.65145(10) 0.51859(6) 0.0258(3) Uani 1 1 d . . .
C32 C 0.36008(8) 0.65819(10) 0.46937(6) 0.0252(3) Uani 1 1 d . . .
C33 C 0.35357(9) 0.61946(10) 0.39552(6) 0.0255(3) Uani 1 1 d . . .
C34 C 0.32789(9) 0.77040(10) 0.46400(7) 0.0274(3) Uani 1 1 d . . .
C35 C 0.35709(11) 0.94924(11) 0.42424(8) 0.0359(3) Uani 1 1 d . . .
C36 C 0.62437(10) 0.72753(12) 0.56239(7) 0.0347(3) Uani 1 1 d . . .
C37 C 0.29755(10) 0.58993(12) 0.49918(7) 0.0322(3) Uani 1 1 d . . .
C38 C 0.55831(8) 0.67958(10) 0.43768(6) 0.0271(3) Uani 1 1 d . . .
C39 C 0.57410(9) 0.65057(10) 0.38533(7) 0.0286(3) Uani 1 1 d . . .
C40 C 0.58140(9) 0.62371(10) 0.31708(6) 0.0276(3) Uani 1 1 d . . .
C41 C 0.57088(10) 0.69795(11) 0.26619(7) 0.0347(3) Uani 1 1 d . . .
C42 C 0.57014(10) 0.66973(10) 0.19757(7) 0.0320(3) Uani 1 1 d . . .
C43 C 0.55502(13) 0.74156(12) 0.14148(8) 0.0438(4) Uani 1 1 d . . .
C44 C 0.54977(12) 0.70908(13) 0.07536(8) 0.0444(4) Uani 1 1 d . . .
C45 C 0.55924(10) 0.60371(12) 0.06189(7) 0.0365(3) Uani 1 1 d . . .
C46 C 0.57505(9) 0.53195(11) 0.11464(7) 0.0310(3) Uani 1 1 d . . .
C47 C 0.58051(8) 0.56382(10) 0.18403(6) 0.0269(3) Uani 1 1 d . . .
C48 C 0.59350(9) 0.51970(11) 0.29900(7) 0.0279(3) Uani 1 1 d . . .
H3A H 0.4461(10) 0.1305(12) 0.3071(8) 0.032(4) Uiso 1 1 d . . .
H8A H 0.5844(11) -0.0267(13) 0.2222(8) 0.036(4) Uiso 1 1 d . . .
H34A H 0.3327(11) 0.7968(13) 0.5125(9) 0.037(4) Uiso 1 1 d . . .
H36A H 0.6094(12) 0.7587(14) 0.6039(9) 0.047(5) Uiso 1 1 d . . .
H31A H 0.4597(10) 0.6714(11) 0.5641(8) 0.027(3) Uiso 1 1 d . . .
H31B H 0.4828(10) 0.5775(12) 0.5217(7) 0.031(4) Uiso 1 1 d . . .
H5A H 0.4295(11) 0.0047(14) 0.1338(8) 0.041(4) Uiso 1 1 d . . .
H3B H 0.4520(10) 0.0156(13) 0.2777(8) 0.033(4) Uiso 1 1 d . . .
H35A H 0.3607(11) 0.9786(13) 0.4733(9) 0.041(4) Uiso 1 1 d . . .
H8B H 0.6687(12) 0.0590(12) 0.2325(8) 0.038(4) Uiso 1 1 d . . .
H29A H 0.5325(11) 0.8719(13) 0.4585(8) 0.034(4) Uiso 1 1 d . . .
H29B H 0.4927(10) 0.8672(12) 0.5247(8) 0.029(3) Uiso 1 1 d . . .
H36B H 0.6728(12) 0.7755(13) 0.5504(9) 0.044(4) Uiso 1 1 d . . .
H48 H 0.6029(10) 0.4656(12) 0.3336(8) 0.029(4) Uiso 1 1 d . . .
H11 H 0.5607(13) -0.0239(17) 0.0878(10) 0.058(5) Uiso 1 1 d . . .
H34B H 0.2601(12) 0.7767(12) 0.4344(8) 0.039(4) Uiso 1 1 d . . .
H9 H 0.6052(12) -0.0230(15) 0.3530(9) 0.048(5) Uiso 1 1 d . . .
H5B H 0.4033(11) 0.1125(12) 0.0904(8) 0.035(4) Uiso 1 1 d . . .
H35B H 0.3998(12) 0.9909(14) 0.4045(9) 0.046(5) Uiso 1 1 d . . .
H36C H 0.6512(12) 0.6577(14) 0.5755(9) 0.043(4) Uiso 1 1 d . . .
H9B H 0.6006(12) 0.0847(13) 0.3942(9) 0.041(4) Uiso 1 1 d . . .
H46 H 0.5786(10) 0.4563(12) 0.1054(8) 0.031(4) Uiso 1 1 d . . .
H43 H 0.5471(12) 0.8164(15) 0.1519(9) 0.053(5) Uiso 1 1 d . . .
H37A H 0.3011(11) 0.6115(13) 0.5476(9) 0.038(4) Uiso 1 1 d . . .
H15 H 0.3377(11) 0.4298(14) 0.0567(9) 0.043(4) Uiso 1 1 d . . .
H37B H 0.3194(12) 0.5159(15) 0.5029(9) 0.045(5) Uiso 1 1 d . . .
H37C H 0.2313(12) 0.5931(13) 0.4680(9) 0.041(4) Uiso 1 1 d . . .
H11B H 0.5378(14) 0.0868(16) 0.0474(11) 0.062(6) Uiso 1 1 d . . .
H41 H 0.5643(12) 0.7711(14) 0.2771(9) 0.050(5) Uiso 1 1 d . . .
H9C H 0.6918(14) 0.0607(15) 0.3670(10) 0.056(5) Uiso 1 1 d . . .
H19 H 0.2842(14) 0.8672(17) 0.0614(11) 0.063(6) Uiso 1 1 d . . .
H22 H 0.3631(11) 0.4732(13) 0.2658(9) 0.040(4) Uiso 1 1 d . . .
H24 H 0.6000(11) 0.3294(14) 0.2216(8) 0.036(4) Uiso 1 1 d . . .
H35C H 0.2914(13) 0.9556(14) 0.3928(9) 0.048(5) Uiso 1 1 d . . .
H50 H 0.3521(12) 0.6682(14) 0.3010(10) 0.050(5) Uiso 1 1 d . . .
H45 H 0.5520(13) 0.5811(14) 0.0129(10) 0.049(5) Uiso 1 1 d . . .
H10A H 0.2746(13) 0.0936(15) 0.2255(10) 0.050(5) Uiso 1 1 d . . .
H10B H 0.3065(13) -0.0064(16) 0.1881(10) 0.059(5) Uiso 1 1 d . . .
H44 H 0.5382(15) 0.7595(16) 0.0358(11) 0.066(6) Uiso 1 1 d . . .
H20 H 0.3117(12) 0.7923(14) 0.1773(10) 0.050(5) Uiso 1 1 d . . .
H17 H 0.3103(14) 0.5844(16) -0.0203(10) 0.059(5) Uiso 1 1 d . . .
H10C H 0.2538(14) 0.0942(15) 0.1411(10) 0.060(5) Uiso 1 1 d . . .
H11C H 0.6462(15) 0.0645(17) 0.0993(11) 0.069(6) Uiso 1 1 d . . .
H18 H 0.2853(15) 0.7602(17) -0.0351(12) 0.069(6) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O25 C1 1.2206(15) . ?
O26 C7 1.2150(16) . ?
O51 C27 1.2184(15) . ?
O52 C33 1.2156(15) . ?
N23 C22 1.3109(18) . ?
N23 C21 1.3753(16) . ?
N24 C1 1.3819(16) . ?
N24 C7 1.3860(16) . ?
N49 C48 1.3188(16) . ?
N49 C47 1.3737(17) . ?
N50 C33 1.3823(16) . ?
N50 C27 1.3827(16) . ?
C1 C2 1.5185(18) . ?
C2 C8 1.5289(18) . ?
C2 C9 1.5308(18) . ?
C2 C3 1.5429(18) . ?
C3 C4 1.5456(18) . ?
C4 C12 1.4827(19) . ?
C4 C10 1.543(2) . ?
C4 C5 1.5458(19) . ?
C5 C6 1.5453(19) . ?
C6 C7 1.5280(18) . ?
C6 C8 1.5280(18) . ?
C6 C11 1.5336(18) . ?
C12 C13 1.196(2) . ?
C13 C14 1.4292(19) . ?
C14 C15 1.3803(18) . ?
C14 C22 1.4216(18) . ?
C15 C16 1.409(2) . ?
C16 C21 1.4165(18) . ?
C16 C17 1.4197(19) . ?
C17 C18 1.359(2) . ?
C18 C19 1.414(2) . ?
C19 C20 1.367(2) . ?
C20 C21 1.415(2) . ?
C27 C28 1.5277(17) . ?
C28 C34 1.5256(18) . ?
C28 C35 1.5318(18) . ?
C28 C29 1.5450(17) . ?
C29 C30 1.5481(18) . ?
C30 C38 1.4806(16) . ?
C30 C36 1.5429(18) . ?
C30 C31 1.5429(17) . ?
C31 C32 1.5426(17) . ?
C32 C34 1.5242(18) . ?
C32 C37 1.5304(18) . ?
C32 C33 1.5288(16) . ?
C38 C39 1.1971(18) . ?
C39 C40 1.4390(17) . ?
C40 C41 1.3711(19) . ?
C40 C48 1.4201(18) . ?
C41 C42 1.4113(18) . ?
C42 C47 1.4157(19) . ?
C42 C43 1.418(2) . ?
C43 C44 1.362(2) . ?
C44 C45 1.406(2) . ?
C45 C46 1.368(2) . ?
C46 C47 1.4207(17) . ?
N24 H24 0.894(18) . ?
N50 H50 0.936(19) . ?
C3 H3A 0.985(16) . ?
C3 H3B 0.997(16) . ?
C5 H5A 0.999(18) . ?
C5 H5B 1.038(16) . ?
C8 H8A 1.021(17) . ?
C8 H8B 1.022(16) . ?
C9 H9 1.019(19) . ?
C9 H9B 1.013(17) . ?
C9 H9C 1.004(19) . ?
C10 H10A 0.984(19) . ?
C10 H10B 1.03(2) . ?
C10 H10C 1.01(2) . ?
C11 H11 1.00(2) . ?
C11 H11B 1.02(2) . ?
C11 H11C 1.03(2) . ?
C15 H15 0.967(18) . ?
C17 H17 0.96(2) . ?
C18 H18 0.96(2) . ?
C19 H19 0.98(2) . ?
C20 H20 1.005(19) . ?
C22 H22 0.986(16) . ?
C29 H29A 0.992(17) . ?
C29 H29B 1.000(15) . ?
C31 H31A 0.955(15) . ?
C31 H31B 1.002(16) . ?
C34 H34A 1.007(16) . ?
C34 H34B 1.006(17) . ?
C35 H35A 1.035(17) . ?
C35 H35B 1.002(18) . ?
C35 H35C 0.992(18) . ?
C36 H36A 1.005(17) . ?
C36 H36B 1.035(17) . ?
C36 H36C 0.992(18) . ?
C37 H37A 0.989(16) . ?
C37 H37B 1.009(18) . ?
C37 H37C 0.994(17) . ?
C41 H41 0.984(19) . ?
C43 H43 1.01(2) . ?
C44 H44 1.00(2) . ?
C45 H45 0.993(18) . ?
C46 H46 1.002(16) . ?
C48 H48 0.963(16) . ?

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
C22 N23 C21 118.59(11) . . ?
C1 N24 C7 126.60(11) . . ?
C48 N49 C47 118.18(11) . . ?
C33 N50 C27 125.63(10) . . ?
O25 C1 N24 119.91(12) . . ?
O25 C1 C2 122.92(11) . . ?
N24 C1 C2 117.16(10) . . ?
C1 C2 C8 108.58(10) . . ?
C1 C2 C9 109.77(11) . . ?
C8 C2 C9 110.73(11) . . ?
C1 C2 C3 109.33(10) . . ?
C8 C2 C3 109.91(10) . . ?
C9 C2 C3 108.50(11) . . ?
C2 C3 C4 116.70(10) . . ?
C12 C4 C10 107.19(12) . . ?
C12 C4 C3 112.72(11) . . ?
C10 C4 C3 107.82(12) . . ?
C12 C4 C5 108.98(11) . . ?
C10 C4 C5 109.91(12) . . ?
C3 C4 C5 110.15(11) . . ?
C6 C5 C4 115.43(10) . . ?
C7 C6 C8 109.09(11) . . ?
C7 C6 C11 108.35(11) . . ?
C8 C6 C11 111.30(12) . . ?
C7 C6 C5 110.08(11) . . ?
C8 C6 C5 108.56(11) . . ?
C11 C6 C5 109.44(11) . . ?
O26 C7 N24 120.00(12) . . ?
O26 C7 C6 122.90(12) . . ?
N24 C7 C6 117.10(11) . . ?
C2 C8 C6 110.43(11) . . ?
C13 C12 C4 174.83(14) . . ?
C12 C13 C14 178.10(14) . . ?
C15 C14 C22 117.54(12) . . ?
C15 C14 C13 122.32(12) . . ?
C22 C14 C13 120.15(11) . . ?
C14 C15 C16 119.96(12) . . ?
C15 C16 C21 118.26(12) . . ?
C15 C16 C17 123.12(13) . . ?
C21 C16 C17 118.61(13) . . ?
C18 C17 C16 120.86(14) . . ?
C17 C18 C19 120.18(14) . . ?
C20 C19 C18 120.76(15) . . ?
C19 C20 C21 119.94(14) . . ?
N23 C21 C20 118.95(12) . . ?
N23 C21 C16 121.40(12) . . ?
C20 C21 C16 119.65(12) . . ?
N23 C22 C14 124.24(12) . . ?
O51 C27 N50 119.94(11) . . ?
O51 C27 C28 123.21(11) . . ?
N50 C27 C28 116.84(10) . . ?
C34 C28 C27 108.52(10) . . ?
C34 C28 C35 111.58(11) . . ?
C27 C28 C35 107.90(11) . . ?
C34 C28 C29 109.06(10) . . ?
C27 C28 C29 110.74(10) . . ?
C35 C28 C29 109.04(11) . . ?
C28 C29 C30 116.11(10) . . ?
C38 C30 C36 108.66(10) . . ?
C38 C30 C31 110.76(10) . . ?
C36 C30 C31 108.83(10) . . ?
C38 C30 C29 108.66(10) . . ?
C36 C30 C29 109.86(10) . . ?
C31 C30 C29 110.06(10) . . ?
C32 C31 C30 115.65(10) . . ?
C34 C32 C37 111.22(11) . . ?
C34 C32 C33 108.61(10) . . ?
C37 C32 C33 108.42(10) . . ?
C34 C32 C31 109.12(10) . . ?
C37 C32 C31 108.75(10) . . ?
C33 C32 C31 110.72(10) . . ?
O52 C33 N50 119.91(11) . . ?
O52 C33 C32 123.06(11) . . ?
N50 C33 C32 117.02(10) . . ?
C32 C34 C28 110.32(10) . . ?
C39 C38 C30 175.52(13) . . ?
C38 C39 C40 171.91(13) . . ?
C41 C40 C48 118.21(11) . . ?
C41 C40 C39 120.28(12) . . ?
C48 C40 C39 121.39(12) . . ?
C40 C41 C42 119.97(13) . . ?
C41 C42 C47 117.80(12) . . ?
C41 C42 C43 123.05(13) . . ?
C47 C42 C43 119.08(12) . . ?
C44 C43 C42 120.51(14) . . ?
C43 C44 C45 120.31(14) . . ?
C46 C45 C44 121.11(13) . . ?
C45 C46 C47 119.66(13) . . ?
N49 C47 C42 122.02(11) . . ?
N49 C47 C46 118.63(12) . . ?
C42 C47 C46 119.33(12) . . ?
N49 C48 C40 123.78(12) . . ?
C1 N24 H24 116.4(10) . . ?
C7 N24 H24 115.0(10) . . ?
C33 N50 H50 115.9(11) . . ?
C27 N50 H50 115.3(11) . . ?
C2 C3 H3A 107.7(9) . . ?
C4 C3 H3A 109.5(9) . . ?
C2 C3 H3B 106.2(9) . . ?
C4 C3 H3B 107.6(9) . . ?
H3A C3 H3B 108.8(12) . . ?
C6 C5 H5A 105.5(9) . . ?
C4 C5 H5A 110.1(9) . . ?
C6 C5 H5B 108.0(9) . . ?
C4 C5 H5B 111.3(8) . . ?
H5A C5 H5B 105.9(12) . . ?
C2 C8 H8A 111.2(8) . . ?
C6 C8 H8A 109.0(9) . . ?
C2 C8 H8B 110.1(9) . . ?
C6 C8 H8B 108.9(9) . . ?
H8A C8 H8B 107.1(12) . . ?
C2 C9 H9 108.8(10) . . ?
C2 C9 H9B 111.2(9) . . ?
H9 C9 H9B 106.8(14) . . ?
C2 C9 H9C 112.4(11) . . ?
H9 C9 H9C 108.7(15) . . ?
H9B C9 H9C 108.8(14) . . ?
C4 C10 H10A 111.7(11) . . ?
C4 C10 H10B 109.1(11) . . ?
H10A C10 H10B 108.6(15) . . ?
C4 C10 H10C 111.1(11) . . ?
H10A C10 H10C 107.8(15) . . ?
H10B C10 H10C 108.5(16) . . ?
C6 C11 H11 111.4(11) . . ?
C6 C11 H11B 107.5(11) . . ?
H11 C11 H11B 107.2(16) . . ?
C6 C11 H11C 112.1(12) . . ?
H11 C11 H11C 110.9(16) . . ?
H11B C11 H11C 107.4(16) . . ?
C14 C15 H15 121.4(10) . . ?
C16 C15 H15 118.7(10) . . ?
C18 C17 H17 121.4(12) . . ?
C16 C17 H17 117.7(12) . . ?
C17 C18 H18 118.0(13) . . ?
C19 C18 H18 121.8(13) . . ?
C20 C19 H19 121.4(12) . . ?
C18 C19 H19 117.8(12) . . ?
C19 C20 H20 122.7(10) . . ?
C21 C20 H20 117.3(10) . . ?
N23 C22 H22 117.4(10) . . ?
C14 C22 H22 118.3(10) . . ?
C28 C29 H29A 109.0(9) . . ?
C30 C29 H29A 109.9(9) . . ?
C28 C29 H29B 105.5(8) . . ?
C30 C29 H29B 108.6(9) . . ?
H29A C29 H29B 107.4(12) . . ?
C32 C31 H31A 105.8(9) . . ?
C30 C31 H31A 108.1(9) . . ?
C32 C31 H31B 108.5(8) . . ?
C30 C31 H31B 110.9(8) . . ?
H31A C31 H31B 107.5(12) . . ?
C32 C34 H34A 109.1(9) . . ?
C28 C34 H34A 109.5(9) . . ?
C32 C34 H34B 110.9(9) . . ?
C28 C34 H34B 109.6(9) . . ?
H34A C34 H34B 107.4(13) . . ?
C28 C35 H35A 109.3(9) . . ?
C28 C35 H35B 109.7(10) . . ?
H35A C35 H35B 108.5(13) . . ?
C28 C35 H35C 111.2(11) . . ?
H35A C35 H35C 108.8(13) . . ?
H35B C35 H35C 109.4(14) . . ?
C30 C36 H36A 109.6(10) . . ?
C30 C36 H36B 109.8(9) . . ?
H36A C36 H36B 107.2(14) . . ?
C30 C36 H36C 110.7(10) . . ?
H36A C36 H36C 108.7(14) . . ?
H36B C36 H36C 110.8(14) . . ?
C32 C37 H37A 110.9(10) . . ?
C32 C37 H37B 110.8(9) . . ?
H37A C37 H37B 106.2(13) . . ?
C32 C37 H37C 109.9(10) . . ?
H37A C37 H37C 110.2(13) . . ?
H37B C37 H37C 108.8(14) . . ?
C40 C41 H41 120.6(10) . . ?
C42 C41 H41 119.4(10) . . ?
C44 C43 H43 121.5(10) . . ?
C42 C43 H43 118.0(10) . . ?
C43 C44 H44 120.4(12) . . ?
C45 C44 H44 119.2(12) . . ?
C46 C45 H45 119.8(11) . . ?
C44 C45 H45 119.1(11) . . ?
C45 C46 H46 122.0(8) . . ?
C47 C46 H46 118.2(8) . . ?
N49 C48 H48 115.5(9) . . ?
C40 C48 H48 120.8(9) . . ?

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
C7 N24 C1 O25 -171.66(12) . . . . ?
C7 N24 C1 C2 7.58(19) . . . . ?
O25 C1 C2 C8 -153.28(13) . . . . ?
N24 C1 C2 C8 27.51(15) . . . . ?
O25 C1 C2 C9 -32.10(17) . . . . ?
N24 C1 C2 C9 148.69(12) . . . . ?
O25 C1 C2 C3 86.81(14) . . . . ?
N24 C1 C2 C3 -92.40(13) . . . . ?
C1 C2 C3 C4 68.49(14) . . . . ?
C8 C2 C3 C4 -50.60(15) . . . . ?
C9 C2 C3 C4 -171.82(11) . . . . ?
C2 C3 C4 C12 -79.12(14) . . . . ?
C2 C3 C4 C10 162.78(12) . . . . ?
C2 C3 C4 C5 42.84(15) . . . . ?
C12 C4 C5 C6 78.54(14) . . . . ?
C10 C4 C5 C6 -164.27(12) . . . . ?
C3 C4 C5 C6 -45.61(15) . . . . ?
C4 C5 C6 C7 -63.22(14) . . . . ?
C4 C5 C6 C8 56.13(15) . . . . ?
C4 C5 C6 C11 177.80(12) . . . . ?
C1 N24 C7 O26 170.27(13) . . . . ?
C1 N24 C7 C6 -9.93(19) . . . . ?
C8 C6 C7 O26 156.58(13) . . . . ?
C11 C6 C7 O26 35.26(18) . . . . ?
C5 C6 C7 O26 -84.40(15) . . . . ?
C8 C6 C7 N24 -23.22(16) . . . . ?
C11 C6 C7 N24 -144.54(13) . . . . ?
C5 C6 C7 N24 95.81(13) . . . . ?
C1 C2 C8 C6 -60.12(14) . . . . ?
C9 C2 C8 C6 179.29(11) . . . . ?
C3 C2 C8 C6 59.42(14) . . . . ?
C7 C6 C8 C2 57.92(14) . . . . ?
C11 C6 C8 C2 177.43(12) . . . . ?
C5 C6 C8 C2 -62.04(14) . . . . ?
C10 C4 C12 C13 -61.9(16) . . . . ?
C3 C4 C12 C13 18E1(10) . . . . ?
C5 C4 C12 C13 57.0(16) . . . . ?
C4 C12 C13 C14 -108(4) . . . . ?
C12 C13 C14 C15 77(4) . . . . ?
C12 C13 C14 C22 -103(4) . . . . ?
C22 C14 C15 C16 -0.35(18) . . . . ?
C13 C14 C15 C16 179.45(12) . . . . ?
C14 C15 C16 C21 0.29(19) . . . . ?
C14 C15 C16 C17 179.45(13) . . . . ?
C15 C16 C17 C18 -179.53(15) . . . . ?
C21 C16 C17 C18 -0.4(2) . . . . ?
C16 C17 C18 C19 0.2(3) . . . . ?
C17 C18 C19 C20 0.3(3) . . . . ?
C18 C19 C20 C21 -0.6(3) . . . . ?
C22 N23 C21 C20 -179.28(13) . . . . ?
C22 N23 C21 C16 0.23(19) . . . . ?
C19 C20 C21 N23 179.90(14) . . . . ?
C19 C20 C21 C16 0.4(2) . . . . ?
C15 C16 C21 N23 -0.22(19) . . . . ?
C17 C16 C21 N23 -179.42(12) . . . . ?
C15 C16 C21 C20 179.28(13) . . . . ?
C17 C16 C21 C20 0.1(2) . . . . ?
C21 N23 C22 C14 -0.3(2) . . . . ?
C15 C14 C22 N23 0.4(2) . . . . ?
C13 C14 C22 N23 -179.43(13) . . . . ?
C33 N50 C27 O51 163.89(12) . . . . ?
C33 N50 C27 C28 -17.03(18) . . . . ?
O51 C27 C28 C34 156.73(13) . . . . ?
N50 C27 C28 C34 -22.32(15) . . . . ?
O51 C27 C28 C35 35.68(17) . . . . ?
N50 C27 C28 C35 -143.37(12) . . . . ?
O51 C27 C28 C29 -83.59(16) . . . . ?
N50 C27 C28 C29 97.37(13) . . . . ?
C34 C28 C29 C30 53.09(13) . . . . ?
C27 C28 C29 C30 -66.27(13) . . . . ?
C35 C28 C29 C30 175.16(11) . . . . ?
C28 C29 C30 C38 77.14(13) . . . . ?
C28 C29 C30 C36 -164.11(11) . . . . ?
C28 C29 C30 C31 -44.30(14) . . . . ?
C38 C30 C31 C32 -75.30(13) . . . . ?
C36 C30 C31 C32 165.30(10) . . . . ?
C29 C30 C31 C32 44.87(14) . . . . ?
C30 C31 C32 C34 -54.54(13) . . . . ?
C30 C31 C32 C37 -176.03(11) . . . . ?
C30 C31 C32 C33 64.95(13) . . . . ?
C27 N50 C33 O52 -163.53(12) . . . . ?
C27 N50 C33 C32 17.86(18) . . . . ?
C34 C32 C33 O52 -157.70(12) . . . . ?
C37 C32 C33 O52 -36.73(17) . . . . ?
C31 C32 C33 O52 82.50(15) . . . . ?
C34 C32 C33 N50 20.86(14) . . . . ?
C37 C32 C33 N50 141.84(11) . . . . ?
C31 C32 C33 N50 -98.94(12) . . . . ?
C37 C32 C34 C28 -178.25(10) . . . . ?
C33 C32 C34 C28 -59.02(13) . . . . ?
C31 C32 C34 C28 61.78(12) . . . . ?
C27 C28 C34 C32 59.80(13) . . . . ?
C35 C28 C34 C32 178.56(10) . . . . ?
C29 C28 C34 C32 -60.93(13) . . . . ?
C36 C30 C38 C39 -136.8(17) . . . . ?
C31 C30 C38 C39 103.7(17) . . . . ?
C29 C30 C38 C39 -17.3(18) . . . . ?
C30 C38 C39 C40 -18(3) . . . . ?
C38 C39 C40 C41 46.2(11) . . . . ?
C38 C39 C40 C48 -129.8(10) . . . . ?
C48 C40 C41 C42 1.4(2) . . . . ?
C39 C40 C41 C42 -174.62(12) . . . . ?
C40 C41 C42 C47 0.0(2) . . . . ?
C40 C41 C42 C43 176.85(14) . . . . ?
C41 C42 C43 C44 -176.28(15) . . . . ?
C47 C42 C43 C44 0.5(2) . . . . ?
C42 C43 C44 C45 0.0(3) . . . . ?
C43 C44 C45 C46 -0.8(2) . . . . ?
C44 C45 C46 C47 1.0(2) . . . . ?
C48 N49 C47 C42 1.97(18) . . . . ?
C48 N49 C47 C46 -176.46(11) . . . . ?
C41 C42 C47 N49 -1.76(19) . . . . ?
C43 C42 C47 N49 -178.74(13) . . . . ?
C41 C42 C47 C46 176.66(12) . . . . ?
C43 C42 C47 C46 -0.32(19) . . . . ?
C45 C46 C47 N49 178.02(12) . . . . ?
C45 C46 C47 C42 -0.45(19) . . . . ?
C47 N49 C48 C40 -0.43(18) . . . . ?
C41 C40 C48 N49 -1.27(19) . . . . ?
C39 C40 C48 N49 174.74(11) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.315
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.054
#==END

data_compound_7
_database_code_depnum_ccdc_archive 'CCDC 234433'

_audit_creation_method           maXus

_exptl_crystal_description       plate
_exptl_crystal_size_max          .3
_exptl_crystal_size_mid          .2
_exptl_crystal_size_min          .02
_exptl_crystal_colour            Colourless
_cell_measurement_temperature    100
_refine_ls_hydrogen_treatment    refall

# Submission details

_diffrn_measurement_device       KappaCCD
_computing_data_collection       KappaCCD
_computing_data_reduction        'Denzo and Scalepak (Otwinowski & Minor, 1997)'

_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20

loop_
_diffrn_radiation_wavelength
0.71073
_diffrn_radiation_wavelength_id  all

_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      -0.08571
_diffrn_orient_matrix_UB_12      -0.10464
_diffrn_orient_matrix_UB_13      0.01343
_diffrn_orient_matrix_UB_21      0.03517
_diffrn_orient_matrix_UB_22      -0.00585
_diffrn_orient_matrix_UB_23      0.04913
_diffrn_orient_matrix_UB_31      -0.03074
_diffrn_orient_matrix_UB_32      0.03966
_diffrn_orient_matrix_UB_33      0.02668

_cell_formula_units_Z            2
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_density_method    'not measured'
_exptl_special_details           
;
?
;
_chemical_formula_weight         848.13
_diffrn_radiation_type           ' MoK\a'

loop_
_symmetry_equiv_pos_as_xyz
+X,+Y,+Z
-X,-Y,-Z

_symmetry_space_group_name_H-M   'P -1          '
_symmetry_cell_setting           Triclinic
_chemical_formula_analytical     'C42 H52 N12 O4, C H Cl3 '
_chemical_formula_moiety         'C42 H52 N12 O4, 0.5(C1 Cl3) '
_chemical_formula_sum            'C42 H52 N12 O4, 0.5(C1 Cl3) '
_chemical_name_systematic        
;
?
;
_cell_length_a                   7.6166(3)
_cell_length_b                   16.8616(8)
_cell_length_c                   17.8082(7)
_cell_angle_alpha                88.088(3)
_cell_angle_beta                 81.177(3)
_cell_angle_gamma                77.664(2)
_cell_volume                     2207.8(2)
_diffrn_reflns_number            11693
_diffrn_reflns_theta_max         24.11
_diffrn_reflns_theta_min         3.33
_diffrn_reflns_theta_full        24.11
_cell_measurement_reflns_used    5917
_cell_measurement_theta_min      0.998
_cell_measurement_theta_max      24.108
_diffrn_measurement_method       CCD
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?

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'
Cl Cl 0.1484 0.1585 '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'

_exptl_absorpt_coefficient_mu    0.170
_reflns_number_total             6757
_reflns_number_gt                5307
_reflns_threshold_expression     >2sigma(I)

_computing_structure_solution    'SIR97 (Altomare, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². Chloroform molecule disordered.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+ (0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6757
_refine_ls_number_parameters     753
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1056
_refine_ls_R_factor_gt           0.0843
_refine_ls_wR_factor_ref         0.2353
_refine_ls_wR_factor_gt          0.2208
_refine_ls_goodness_of_fit_ref   1.622
_refine_ls_restrained_S_all      1.622
_refine_ls_shift/su_max          0.244
_refine_ls_shift/su_mean         0.011

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
O22 O 0.5988(3) 0.44463(16) 0.81189(13) 0.0386(6) Uani 1 1 d . . .
O23 O 0.6610(4) 0.23537(16) 0.65388(14) 0.0391(6) Uani 1 1 d . . .
O51 O 1.1051(4) 0.30273(18) 0.04471(14) 0.0504(8) Uani 1 1 d . . .
O52 O 0.6253(3) 0.23892(16) 0.19383(14) 0.0392(6) Uani 1 1 d . . .
N24 N 0.6449(4) 0.33378(19) 0.73804(17) 0.0318(7) Uani 1 1 d . . .
N25 N 0.1976(4) 0.39375(17) 0.54375(15) 0.0287(6) Uani 1 1 d . . .
N26 N 0.1766(4) 0.43403(17) 0.41202(15) 0.0296(6) Uani 1 1 d . . .
N27 N 0.2472(4) 0.56593(17) 0.38576(15) 0.0301(7) Uani 1 1 d . . .
N28 N 0.2836(4) 0.50373(17) 0.58440(15) 0.0293(6) Uani 1 1 d . . .
N29 N 0.3260(4) 0.6437(2) 0.47497(19) 0.0333(7) Uani 1 1 d . . .
N53 N 0.8504(4) 0.28240(19) 0.11809(17) 0.0347(7) Uani 1 1 d . . .
N54 N 0.9923(4) 0.01804(18) 0.14772(16) 0.0347(7) Uani 1 1 d . . .
N55 N 0.9125(5) -0.09320(18) 0.08768(16) 0.0386(8) Uani 1 1 d . . .
N56 N 1.1468(5) -0.15187(19) -0.01377(16) 0.0389(8) Uani 1 1 d . . .
N57 N 1.2659(4) 0.01942(18) 0.07921(15) 0.0344(7) Uani 1 1 d . . .
N58 N 1.4178(6) -0.1107(2) -0.04861(18) 0.0432(8) Uani 1 1 d . . .
C1 C 0.5841(5) 0.3749(2) 0.80691(19) 0.0330(8) Uani 1 1 d . . .
C2 C 0.4998(5) 0.3281(2) 0.87212(19) 0.0358(8) Uani 1 1 d . . .
C3 C 0.2918(5) 0.3443(3) 0.8713(2) 0.0385(9) Uani 1 1 d . . .
C4 C 0.2284(5) 0.3079(2) 0.8044(2) 0.0382(9) Uani 1 1 d . . .
C5 C 0.3368(5) 0.2210(2) 0.7864(2) 0.0392(9) Uani 1 1 d . . .
C6 C 0.5435(5) 0.2082(2) 0.7848(2) 0.0354(8) Uani 1 1 d . . .
C7 C 0.6216(5) 0.2593(2) 0.7199(2) 0.0325(8) Uani 1 1 d . . .
C8 C 0.5795(6) 0.2369(2) 0.8601(2) 0.0372(8) Uani 1 1 d . . .
C9 C 0.5357(6) 0.3571(3) 0.9475(2) 0.0435(10) Uani 1 1 d . . .
C10 C 0.6314(6) 0.1186(3) 0.7697(3) 0.0450(10) Uani 1 1 d . . .
C11 C 0.0256(6) 0.3068(3) 0.8266(3) 0.0489(11) Uani 1 1 d . . .
C12 C 0.2423(5) 0.3578(2) 0.7346(2) 0.0342(8) Uani 1 1 d . . .
C13 C 0.2424(5) 0.3949(2) 0.67574(19) 0.0315(8) Uani 1 1 d . . .
C14 C 0.2435(4) 0.4324(2) 0.60320(19) 0.0299(8) Uani 1 1 d . . .
C15 C 0.2106(4) 0.4452(2) 0.48239(18) 0.0282(7) Uani 1 1 d . . .
C16 C 0.1983(4) 0.4974(2) 0.36815(18) 0.0304(8) Uani 1 1 d . . .
C17 C 0.2797(4) 0.5752(2) 0.45665(17) 0.0280(7) Uani 1 1 d . . .
C18 C 0.2630(4) 0.5118(2) 0.50897(17) 0.0275(7) Uani 1 1 d . . .
C19 C 0.1490(5) 0.3145(2) 0.5451(2) 0.0331(8) Uani 1 1 d . . .
C20 C 0.3141(6) 0.2454(2) 0.5338(3) 0.0411(9) Uani 1 1 d . . .
C21 C 0.2598(9) 0.1634(3) 0.5402(3) 0.0615(13) Uani 1 1 d . . .
C30 C 1.0014(5) 0.3174(2) 0.1038(2) 0.0368(9) Uani 1 1 d . . .
C31 C 1.0260(5) 0.3738(2) 0.16428(19) 0.0338(8) Uani 1 1 d . . .
C32 C 1.1611(5) 0.3262(2) 0.2151(2) 0.0320(8) Uani 1 1 d . . .
C33 C 1.0971(5) 0.2563(2) 0.26199(18) 0.0330(8) Uani 1 1 d . . .
C34 C 0.8961(5) 0.2854(2) 0.2999(2) 0.0336(8) Uani 1 1 d . . .
C35 C 0.7639(5) 0.3344(2) 0.2492(2) 0.0354(8) Uani 1 1 d . . .
C67 C 0.7385(5) 0.2813(2) 0.1865(2) 0.0339(8) Uani 1 1 d . . .
C37 C 0.8432(5) 0.4060(2) 0.2135(2) 0.0368(9) Uani 1 1 d . . .
C38 C 1.1055(7) 0.4437(3) 0.1254(2) 0.0440(10) Uani 1 1 d . . .
C39 C 0.5802(6) 0.3655(3) 0.2977(3) 0.0479(11) Uani 1 1 d . . .
C40 C 1.2178(6) 0.2305(3) 0.3246(2) 0.0405(9) Uani 1 1 d . . .
C41 C 1.1183(5) 0.1846(2) 0.21443(18) 0.0314(8) Uani 1 1 d . . .
C42 C 1.1425(5) 0.1240(2) 0.17665(19) 0.0339(8) Uani 1 1 d . . .
C43 C 1.1395(5) 0.0543(2) 0.13450(18) 0.0320(8) Uani 1 1 d . . .
C44 C 1.0254(5) -0.0435(2) 0.09646(19) 0.0354(8) Uani 1 1 d . . .
C45 C 0.9858(6) -0.1437(2) 0.0306(2) 0.0401(10) Uani 1 1 d . . .
C46 C 1.2581(6) -0.1015(2) -0.00383(19) 0.0368(9) Uani 1 1 d . . .
C47 C 1.1948(5) -0.0428(2) 0.05393(18) 0.0345(8) Uani 1 1 d . . .
C48 C 0.8229(5) 0.0432(2) 0.2013(2) 0.0394(9) Uani 1 1 d . . .
C49 C 0.8326(7) 0.0049(3) 0.2791(2) 0.0533(11) Uani 1 1 d . . .
C50 C 0.6526(8) 0.0337(4) 0.3310(3) 0.0671(14) Uani 1 1 d . . .
Cl59 Cl 1.0004(18) 0.0739(8) 0.4170(7) 0.180(4) Uiso 0.30 1 d P . .
Cl60 Cl 0.8142(7) 0.1420(4) 0.4775(3) 0.1563(16) Uiso 0.60 1 d P . .
Cl61 Cl 0.8162(17) 0.0787(8) 0.5344(7) 0.174(4) Uiso 0.30 1 d P . .
C62 C 1.0000 0.0000 0.5000 0.167(8) Uani 1 2 d S . .
Cl63 Cl 0.7449(10) 0.0098(5) 0.5747(4) 0.113(2) Uiso 0.30 1 d P . .
H34A H 0.894(5) 0.316(2) 0.347(2) 0.036(9) Uiso 1 1 d . . .
H19A H 0.090(6) 0.316(3) 0.503(2) 0.047(11) Uiso 1 1 d . . .
H16 H 0.173(4) 0.494(2) 0.3132(18) 0.020(8) Uiso 1 1 d . . .
H5A H 0.317(6) 0.201(3) 0.742(3) 0.044(11) Uiso 1 1 d . . .
H20 H 0.396(5) 0.250(2) 0.573(2) 0.032(9) Uiso 1 1 d . . .
H37 H 0.852(4) 0.439(2) 0.2562(18) 0.016(7) Uiso 1 1 d . . .
H32A H 1.162(5) 0.365(2) 0.2565(19) 0.027(8) Uiso 1 1 d . . .
H38A H 1.025(6) 0.475(3) 0.091(2) 0.042(11) Uiso 1 1 d . . .
H32B H 1.272(6) 0.307(2) 0.184(2) 0.034(9) Uiso 1 1 d . . .
H38B H 1.224(7) 0.424(3) 0.098(3) 0.056(13) Uiso 1 1 d . . .
H21 H 0.179(7) 0.159(3) 0.510(3) 0.046(12) Uiso 1 1 d . . .
H34B H 0.849(5) 0.241(2) 0.3224(19) 0.025(8) Uiso 1 1 d . . .
H8 H 0.700(6) 0.225(3) 0.862(2) 0.042(11) Uiso 1 1 d . . .
H39 H 0.599(5) 0.401(2) 0.333(2) 0.029(9) Uiso 1 1 d . . .
H19B H 0.079(5) 0.309(2) 0.597(2) 0.038(10) Uiso 1 1 d . . .
H3 H 0.243(5) 0.410(3) 0.875(2) 0.037(10) Uiso 1 1 d . . .
H5B H 0.295(6) 0.185(3) 0.826(2) 0.043(10) Uiso 1 1 d . . .
H10 H 0.772(6) 0.111(3) 0.769(2) 0.042(10) Uiso 1 1 d . . .
H49A H 0.937(8) 0.020(4) 0.305(3) 0.077(16) Uiso 1 1 d . . .
H40A H 1.349(6) 0.211(3) 0.303(2) 0.041(10) Uiso 1 1 d . . .
H3B H 0.247(6) 0.321(3) 0.927(3) 0.054(12) Uiso 1 1 d . . .
H38C H 1.130(6) 0.478(3) 0.165(2) 0.045(11) Uiso 1 1 d . . .
H53 H 0.835(6) 0.251(3) 0.081(3) 0.052(12) Uiso 1 1 d . . .
H40B H 1.216(7) 0.281(3) 0.358(3) 0.063(13) Uiso 1 1 d . . .
H11A H -0.049(6) 0.359(3) 0.835(2) 0.034(10) Uiso 1 1 d . . .
H20B H 0.382(5) 0.244(2) 0.483(2) 0.036(10) Uiso 1 1 d . . .
H29 H 0.349(6) 0.650(3) 0.525(3) 0.044(11) Uiso 1 1 d . . .
H37B H 0.742(6) 0.443(3) 0.182(2) 0.048(11) Uiso 1 1 d . . .
H49B H 0.863(6) -0.056(3) 0.271(2) 0.046(11) Uiso 1 1 d . . .
H48 H 0.788(6) 0.107(3) 0.205(2) 0.047(11) Uiso 1 1 d . . .
H9 H 0.478(6) 0.334(3) 0.994(3) 0.047(11) Uiso 1 1 d . . .
H21B H 0.356(9) 0.117(4) 0.524(3) 0.081(17) Uiso 1 1 d . . .
H11B H -0.018(7) 0.287(3) 0.787(3) 0.054(13) Uiso 1 1 d . . .
H39B H 0.520(7) 0.389(3) 0.266(3) 0.051(15) Uiso 1 1 d . . .
H10B H 0.607(6) 0.100(3) 0.724(3) 0.051(12) Uiso 1 1 d . . .
H39C H 0.523(7) 0.312(3) 0.320(3) 0.066(14) Uiso 1 1 d . . .
H10C H 0.573(5) 0.092(3) 0.810(2) 0.037(10) Uiso 1 1 d . . .
H48B H 0.730(6) 0.025(3) 0.174(2) 0.042(10) Uiso 1 1 d . . .
H8B H 0.523(5) 0.206(3) 0.905(2) 0.038(10) Uiso 1 1 d . . .
H21C H 0.188(7) 0.153(3) 0.596(3) 0.065(14) Uiso 1 1 d . . .
H11C H 0.016(5) 0.271(2) 0.874(2) 0.035(10) Uiso 1 1 d . . .
H24 H 0.674(5) 0.364(3) 0.704(2) 0.030(10) Uiso 1 1 d . . .
H45 H 0.928(6) -0.175(3) 0.024(2) 0.039(12) Uiso 1 1 d . . .
H50A H 0.618(8) 0.093(4) 0.339(3) 0.076(16) Uiso 1 1 d . . .
H58A H 1.446(5) -0.150(2) -0.085(2) 0.029(9) Uiso 1 1 d . . .
H40C H 1.184(6) 0.181(3) 0.360(2) 0.052(12) Uiso 1 1 d . . .
H29B H 0.332(6) 0.680(3) 0.443(2) 0.037(11) Uiso 1 1 d . . .
H9B H 0.499(7) 0.418(4) 0.951(3) 0.068(15) Uiso 1 1 d . . .
H58B H 1.485(8) -0.081(4) -0.049(3) 0.075(19) Uiso 1 1 d . . .
H50B H 0.550(10) 0.018(4) 0.305(4) 0.10(2) Uiso 1 1 d . . .
H9C H 0.662(7) 0.347(3) 0.956(2) 0.053(12) Uiso 1 1 d . . .
H50C H 0.687(11) 0.021(5) 0.386(5) 0.13(3) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O22 C1 1.212(4) . ?
O23 C7 1.227(4) . ?
O51 C30 1.214(4) . ?
O52 C67 1.223(4) . ?
N24 C7 1.362(5) . ?
N24 C1 1.395(5) . ?
N25 C15 1.377(4) . ?
N25 C14 1.387(4) . ?
N25 C19 1.460(4) . ?
N26 C16 1.327(4) . ?
N26 C15 1.345(4) . ?
N27 C17 1.343(4) . ?
N27 C16 1.347(5) . ?
N28 C14 1.324(4) . ?
N28 C18 1.375(4) . ?
N29 C17 1.342(5) . ?
N53 C67 1.377(5) . ?
N53 C30 1.388(5) . ?
N54 C44 1.361(5) . ?
N54 C43 1.374(5) . ?
N54 C48 1.473(5) . ?
N55 C45 1.323(5) . ?
N55 C44 1.352(5) . ?
N56 C45 1.336(5) . ?
N56 C46 1.355(5) . ?
N57 C43 1.322(5) . ?
N57 C47 1.395(5) . ?
N58 C46 1.330(5) . ?
C1 C2 1.521(5) . ?
C2 C9 1.526(5) . ?
C2 C8 1.537(6) . ?
C2 C3 1.551(5) . ?
C3 C4 1.543(6) . ?
C4 C12 1.481(5) . ?
C4 C11 1.539(5) . ?
C4 C5 1.537(6) . ?
C5 C6 1.538(5) . ?
C6 C8 1.524(5) . ?
C6 C10 1.530(6) . ?
C6 C7 1.541(5) . ?
C12 C13 1.202(5) . ?
C13 C14 1.419(5) . ?
C15 C18 1.389(5) . ?
C17 C18 1.408(5) . ?
C19 C20 1.513(5) . ?
C20 C21 1.521(6) . ?
C30 C31 1.518(5) . ?
C31 C37 1.529(5) . ?
C31 C38 1.536(5) . ?
C31 C32 1.551(5) . ?
C32 C33 1.542(5) . ?
C33 C41 1.465(5) . ?
C33 C40 1.546(5) . ?
C33 C34 1.557(5) . ?
C34 C35 1.544(5) . ?
C35 C67 1.515(5) . ?
C35 C39 1.524(5) . ?
C35 C37 1.539(5) . ?
C41 C42 1.207(5) . ?
C42 C43 1.422(5) . ?
C44 C47 1.394(5) . ?
C46 C47 1.407(5) . ?
C48 C49 1.515(6) . ?
C49 C50 1.525(7) . ?
Cl59 Cl60 1.846(14) . ?
Cl59 C62 1.901(13) . ?
Cl59 Cl63 2.163(16) 2_756 ?
Cl59 Cl61 2.325(17) . ?
Cl60 Cl61 1.446(13) . ?
Cl61 Cl63 1.501(14) . ?
Cl61 C62 1.758(13) . ?
C62 Cl61 1.758(13) 2_756 ?
C62 Cl59 1.901(13) 2_756 ?
C62 Cl63 2.158(7) . ?
C62 Cl63 2.158(7) 2_756 ?
Cl63 Cl59 2.163(16) 2_756 ?
N24 H24 0.82(4) . ?
N29 H29 0.94(4) . ?
N29 H29B 0.83(5) . ?
N53 H53 0.89(5) . ?
N58 H58A 0.91(4) . ?
N58 H58B 0.78(7) . ?
C3 H3 1.09(4) . ?
C3 H3B 1.08(5) . ?
C5 H5A 0.91(4) . ?
C5 H5B 0.98(4) . ?
C8 H8 0.90(5) . ?
C8 H8B 1.02(4) . ?
C9 H9 0.99(5) . ?
C9 H9B 1.01(6) . ?
C9 H9C 0.97(5) . ?
C10 H10 1.05(4) . ?
C10 H10B 0.95(5) . ?
C10 H10C 0.93(4) . ?
C11 H11A 0.95(5) . ?
C11 H11B 0.92(5) . ?
C11 H11C 1.03(4) . ?
C16 H16 1.03(3) . ?
C19 H19A 0.93(5) . ?
C19 H19B 1.00(4) . ?
C20 H20 1.03(4) . ?
C20 H20B 0.97(4) . ?
C21 H21 0.89(5) . ?
C21 H21B 0.97(7) . ?
C21 H21C 1.09(5) . ?
C32 H32A 1.01(4) . ?
C32 H32B 0.94(4) . ?
C34 H34A 0.99(4) . ?
C34 H34B 0.95(4) . ?
C37 H37 0.97(3) . ?
C37 H37B 1.10(5) . ?
C38 H38A 0.99(5) . ?
C38 H38B 0.95(5) . ?
C38 H38C 0.99(4) . ?
C39 H39 0.93(4) . ?
C39 H39B 0.82(5) . ?
C39 H39C 1.12(6) . ?
C40 H40A 1.00(4) . ?
C40 H40B 1.04(5) . ?
C40 H40C 1.09(5) . ?
C45 H45 0.77(5) . ?
C48 H48 1.05(5) . ?
C48 H48B 1.02(4) . ?
C49 H49A 1.06(6) . ?
C49 H49B 1.01(5) . ?
C50 H50A 0.99(7) . ?
C50 H50B 1.05(7) . ?
C50 H50C 1.05(9) . ?

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
C7 N24 C1 127.6(3) . . ?
C15 N25 C14 105.6(3) . . ?
C15 N25 C19 126.9(3) . . ?
C14 N25 C19 127.5(3) . . ?
C16 N26 C15 110.6(3) . . ?
C17 N27 C16 118.9(3) . . ?
C14 N28 C18 103.4(3) . . ?
C67 N53 C30 126.6(3) . . ?
C44 N54 C43 106.4(3) . . ?
C44 N54 C48 125.2(3) . . ?
C43 N54 C48 128.2(3) . . ?
C45 N55 C44 109.7(3) . . ?
C45 N56 C46 119.4(3) . . ?
C43 N57 C47 104.1(3) . . ?
O22 C1 N24 119.7(3) . . ?
O22 C1 C2 123.7(3) . . ?
N24 C1 C2 116.5(3) . . ?
C1 C2 C9 109.7(3) . . ?
C1 C2 C8 109.0(3) . . ?
C9 C2 C8 111.4(3) . . ?
C1 C2 C3 108.4(3) . . ?
C9 C2 C3 109.4(3) . . ?
C8 C2 C3 108.9(3) . . ?
C4 C3 C2 116.7(3) . . ?
C12 C4 C11 106.2(3) . . ?
C12 C4 C5 109.1(3) . . ?
C11 C4 C5 109.4(3) . . ?
C12 C4 C3 112.6(3) . . ?
C11 C4 C3 108.0(3) . . ?
C5 C4 C3 111.3(3) . . ?
C6 C5 C4 115.5(3) . . ?
C8 C6 C10 111.9(3) . . ?
C8 C6 C5 108.7(3) . . ?
C10 C6 C5 109.5(3) . . ?
C8 C6 C7 109.0(3) . . ?
C10 C6 C7 108.6(3) . . ?
C5 C6 C7 109.1(3) . . ?
O23 C7 N24 120.2(3) . . ?
O23 C7 C6 122.4(3) . . ?
N24 C7 C6 117.4(3) . . ?
C6 C8 C2 111.2(3) . . ?
C13 C12 C4 174.1(4) . . ?
C12 C13 C14 175.2(4) . . ?
N28 C14 N25 113.6(3) . . ?
N28 C14 C13 126.6(3) . . ?
N25 C14 C13 119.8(3) . . ?
N26 C15 N25 127.4(3) . . ?
N26 C15 C18 127.3(3) . . ?
N25 C15 C18 105.4(3) . . ?
N26 C16 N27 128.9(3) . . ?
N29 C17 N27 119.3(3) . . ?
N29 C17 C18 122.7(3) . . ?
N27 C17 C18 118.0(3) . . ?
N28 C18 C15 112.0(3) . . ?
N28 C18 C17 131.7(3) . . ?
C15 C18 C17 116.3(3) . . ?
N25 C19 C20 112.5(3) . . ?
C19 C20 C21 111.3(4) . . ?
O51 C30 N53 119.7(3) . . ?
O51 C30 C31 123.3(3) . . ?
N53 C30 C31 117.0(3) . . ?
C30 C31 C37 109.6(3) . . ?
C30 C31 C38 109.0(3) . . ?
C37 C31 C38 111.0(3) . . ?
C30 C31 C32 109.3(3) . . ?
C37 C31 C32 109.2(3) . . ?
C38 C31 C32 108.8(3) . . ?
C33 C32 C31 115.5(3) . . ?
C41 C33 C32 110.9(3) . . ?
C41 C33 C40 106.6(3) . . ?
C32 C33 C40 109.3(3) . . ?
C41 C33 C34 111.2(3) . . ?
C32 C33 C34 109.6(3) . . ?
C40 C33 C34 109.1(3) . . ?
C35 C34 C33 116.5(3) . . ?
C67 C35 C39 108.9(3) . . ?
C67 C35 C37 109.1(3) . . ?
C39 C35 C37 110.3(3) . . ?
C67 C35 C34 110.5(3) . . ?
C39 C35 C34 109.1(3) . . ?
C37 C35 C34 108.9(3) . . ?
O52 C67 N53 119.7(3) . . ?
O52 C67 C35 123.5(3) . . ?
N53 C67 C35 116.8(3) . . ?
C31 C37 C35 109.7(3) . . ?
C42 C41 C33 177.1(4) . . ?
C41 C42 C43 170.6(4) . . ?
N57 C43 N54 113.2(3) . . ?
N57 C43 C42 126.4(3) . . ?
N54 C43 C42 120.3(3) . . ?
N55 C44 N54 126.2(3) . . ?
N55 C44 C47 127.4(3) . . ?
N54 C44 C47 106.4(3) . . ?
N55 C45 N56 129.9(4) . . ?
N58 C46 N56 118.4(3) . . ?
N58 C46 C47 124.8(4) . . ?
N56 C46 C47 116.8(3) . . ?
C44 C47 N57 109.8(3) . . ?
C44 C47 C46 116.8(3) . . ?
N57 C47 C46 133.4(4) . . ?
N54 C48 C49 113.0(3) . . ?
C48 C49 C50 109.9(4) . . ?
Cl60 Cl59 C62 86.2(5) . . ?
Cl60 Cl59 Cl63 140.2(7) . 2_756 ?
C62 Cl59 Cl63 63.8(5) . 2_756 ?
Cl60 Cl59 Cl61 38.5(4) . . ?
C62 Cl59 Cl61 47.9(4) . . ?
Cl63 Cl59 Cl61 108.3(7) 2_756 . ?
Cl61 Cl60 Cl59 89.0(7) . . ?
Cl60 Cl61 Cl63 152.9(10) . . ?
Cl60 Cl61 C62 105.7(7) . . ?
Cl63 Cl61 C62 82.5(7) . . ?
Cl60 Cl61 Cl59 52.6(6) . . ?
Cl63 Cl61 Cl59 127.0(8) . . ?
C62 Cl61 Cl59 53.3(5) . . ?
Cl61 C62 Cl61 180.0(7) . 2_756 ?
Cl61 C62 Cl59 78.8(6) . . ?
Cl61 C62 Cl59 101.2(6) 2_756 . ?
Cl61 C62 Cl59 101.2(6) . 2_756 ?
Cl61 C62 Cl59 78.8(6) 2_756 2_756 ?
Cl59 C62 Cl59 179.997(3) . 2_756 ?
Cl61 C62 Cl63 43.6(4) . . ?
Cl61 C62 Cl63 136.4(4) 2_756 . ?
Cl59 C62 Cl63 116.0(4) . . ?
Cl59 C62 Cl63 64.0(4) 2_756 . ?
Cl61 C62 Cl63 136.4(4) . 2_756 ?
Cl61 C62 Cl63 43.6(4) 2_756 2_756 ?
Cl59 C62 Cl63 64.0(4) . 2_756 ?
Cl59 C62 Cl63 116.0(4) 2_756 2_756 ?
Cl63 C62 Cl63 180.0 . 2_756 ?
Cl61 Cl63 C62 53.9(5) . . ?
Cl61 Cl63 Cl59 99.5(7) . 2_756 ?
C62 Cl63 Cl59 52.2(4) . 2_756 ?
C7 N24 H24 119(3) . . ?
C1 N24 H24 112(3) . . ?
C17 N29 H29 119(3) . . ?
C17 N29 H29B 120(3) . . ?
H29 N29 H29B 121(4) . . ?
C67 N53 H53 116(3) . . ?
C30 N53 H53 116(3) . . ?
C46 N58 H58A 118(2) . . ?
C46 N58 H58B 124(4) . . ?
H58A N58 H58B 117(5) . . ?
C4 C3 H3 112(2) . . ?
C2 C3 H3 106(2) . . ?
C4 C3 H3B 115(2) . . ?
C2 C3 H3B 100(2) . . ?
H3 C3 H3B 106(3) . . ?
C6 C5 H5A 108(3) . . ?
C4 C5 H5A 113(3) . . ?
C6 C5 H5B 106(2) . . ?
C4 C5 H5B 108(2) . . ?
H5A C5 H5B 105(4) . . ?
C6 C8 H8 110(2) . . ?
C2 C8 H8 111(3) . . ?
C6 C8 H8B 111(2) . . ?
C2 C8 H8B 108(2) . . ?
H8 C8 H8B 105(4) . . ?
C2 C9 H9 116(2) . . ?
C2 C9 H9B 110(3) . . ?
H9 C9 H9B 109(4) . . ?
C2 C9 H9C 117(3) . . ?
H9 C9 H9C 102(4) . . ?
H9B C9 H9C 102(4) . . ?
C6 C10 H10 108(2) . . ?
C6 C10 H10B 113(3) . . ?
H10 C10 H10B 110(4) . . ?
C6 C10 H10C 103(2) . . ?
H10 C10 H10C 114(3) . . ?
H10B C10 H10C 108(4) . . ?
C4 C11 H11A 113(2) . . ?
C4 C11 H11B 110(3) . . ?
H11A C11 H11B 103(4) . . ?
C4 C11 H11C 107(2) . . ?
H11A C11 H11C 112(3) . . ?
H11B C11 H11C 112(4) . . ?
N26 C16 H16 115.4(18) . . ?
N27 C16 H16 115.7(18) . . ?
N25 C19 H19A 104(3) . . ?
C20 C19 H19A 107(3) . . ?
N25 C19 H19B 106(2) . . ?
C20 C19 H19B 109(2) . . ?
H19A C19 H19B 119(4) . . ?
C19 C20 H20 109(2) . . ?
C21 C20 H20 111(2) . . ?
C19 C20 H20B 113(2) . . ?
C21 C20 H20B 103(2) . . ?
H20 C20 H20B 110(3) . . ?
C20 C21 H21 113(3) . . ?
C20 C21 H21B 116(4) . . ?
H21 C21 H21B 102(4) . . ?
C20 C21 H21C 112(3) . . ?
H21 C21 H21C 102(4) . . ?
H21B C21 H21C 111(5) . . ?
C33 C32 H32A 101(2) . . ?
C31 C32 H32A 105(2) . . ?
C33 C32 H32B 111(2) . . ?
C31 C32 H32B 108(2) . . ?
H32A C32 H32B 116(3) . . ?
C35 C34 H34A 111(2) . . ?
C33 C34 H34A 109(2) . . ?
C35 C34 H34B 110(2) . . ?
C33 C34 H34B 111(2) . . ?
H34A C34 H34B 98(3) . . ?
C31 C37 H37 113.6(19) . . ?
C35 C37 H37 105.2(18) . . ?
C31 C37 H37B 113(2) . . ?
C35 C37 H37B 108(2) . . ?
H37 C37 H37B 107(3) . . ?
C31 C38 H38A 111(2) . . ?
C31 C38 H38B 111(3) . . ?
H38A C38 H38B 110(4) . . ?
C31 C38 H38C 109(2) . . ?
H38A C38 H38C 113(4) . . ?
H38B C38 H38C 102(4) . . ?
C35 C39 H39 107(2) . . ?
C35 C39 H39B 102(3) . . ?
H39 C39 H39B 112(4) . . ?
C35 C39 H39C 108(3) . . ?
H39 C39 H39C 117(3) . . ?
H39B C39 H39C 109(4) . . ?
C33 C40 H40A 112(2) . . ?
C33 C40 H40B 110(3) . . ?
H40A C40 H40B 104(4) . . ?
C33 C40 H40C 114(2) . . ?
H40A C40 H40C 105(3) . . ?
H40B C40 H40C 111(3) . . ?
N55 C45 H45 114(3) . . ?
N56 C45 H45 116(3) . . ?
N54 C48 H48 110(2) . . ?
C49 C48 H48 111(2) . . ?
N54 C48 H48B 102(2) . . ?
C49 C48 H48B 113(2) . . ?
H48 C48 H48B 108(3) . . ?
C48 C49 H49A 113(3) . . ?
C50 C49 H49A 108(3) . . ?
C48 C49 H49B 106(2) . . ?
C50 C49 H49B 113(2) . . ?
H49A C49 H49B 107(4) . . ?
C49 C50 H50A 115(3) . . ?
C49 C50 H50B 108(4) . . ?
H50A C50 H50B 107(5) . . ?
C49 C50 H50C 103(4) . . ?
H50A C50 H50C 94(5) . . ?
H50B C50 H50C 130(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 N24 C1 O22 -172.2(3) . . . . ?
C7 N24 C1 C2 7.1(5) . . . . ?
O22 C1 C2 C9 -31.6(5) . . . . ?
N24 C1 C2 C9 149.0(3) . . . . ?
O22 C1 C2 C8 -153.8(3) . . . . ?
N24 C1 C2 C8 26.8(4) . . . . ?
O22 C1 C2 C3 87.7(4) . . . . ?
N24 C1 C2 C3 -91.6(4) . . . . ?
C1 C2 C3 C4 68.9(4) . . . . ?
C9 C2 C3 C4 -171.6(3) . . . . ?
C8 C2 C3 C4 -49.6(4) . . . . ?
C2 C3 C4 C12 -80.8(4) . . . . ?
C2 C3 C4 C11 162.2(3) . . . . ?
C2 C3 C4 C5 42.0(4) . . . . ?
C12 C4 C5 C6 80.3(4) . . . . ?
C11 C4 C5 C6 -163.9(3) . . . . ?
C3 C4 C5 C6 -44.5(4) . . . . ?
C4 C5 C6 C8 55.0(4) . . . . ?
C4 C5 C6 C10 177.6(3) . . . . ?
C4 C5 C6 C7 -63.7(4) . . . . ?
C1 N24 C7 O23 170.1(3) . . . . ?
C1 N24 C7 C6 -9.4(5) . . . . ?
C8 C6 C7 O23 157.7(3) . . . . ?
C10 C6 C7 O23 35.4(5) . . . . ?
C5 C6 C7 O23 -83.8(4) . . . . ?
C8 C6 C7 N24 -22.9(4) . . . . ?
C10 C6 C7 N24 -145.1(3) . . . . ?
C5 C6 C7 N24 95.6(4) . . . . ?
C10 C6 C8 C2 176.7(3) . . . . ?
C5 C6 C8 C2 -62.3(4) . . . . ?
C7 C6 C8 C2 56.5(4) . . . . ?
C1 C2 C8 C6 -58.7(4) . . . . ?
C9 C2 C8 C6 -179.9(3) . . . . ?
C3 C2 C8 C6 59.3(4) . . . . ?
C11 C4 C12 C13 -42(4) . . . . ?
C5 C4 C12 C13 76(4) . . . . ?
C3 C4 C12 C13 -160(4) . . . . ?
C4 C12 C13 C14 -45(7) . . . . ?
C18 N28 C14 N25 -0.1(4) . . . . ?
C18 N28 C14 C13 -179.5(3) . . . . ?
C15 N25 C14 N28 0.2(4) . . . . ?
C19 N25 C14 N28 179.1(3) . . . . ?
C15 N25 C14 C13 179.6(3) . . . . ?
C19 N25 C14 C13 -1.5(5) . . . . ?
C12 C13 C14 N28 -161(4) . . . . ?
C12 C13 C14 N25 20(4) . . . . ?
C16 N26 C15 N25 178.2(3) . . . . ?
C16 N26 C15 C18 -0.5(5) . . . . ?
C14 N25 C15 N26 -179.1(3) . . . . ?
C19 N25 C15 N26 2.0(5) . . . . ?
C14 N25 C15 C18 -0.2(3) . . . . ?
C19 N25 C15 C18 -179.1(3) . . . . ?
C15 N26 C16 N27 0.1(5) . . . . ?
C17 N27 C16 N26 -0.2(5) . . . . ?
C16 N27 C17 N29 -179.1(3) . . . . ?
C16 N27 C17 C18 0.7(4) . . . . ?
C14 N28 C18 C15 0.0(4) . . . . ?
C14 N28 C18 C17 177.6(3) . . . . ?
N26 C15 C18 N28 179.1(3) . . . . ?
N25 C15 C18 N28 0.2(4) . . . . ?
N26 C15 C18 C17 1.0(5) . . . . ?
N25 C15 C18 C17 -177.9(3) . . . . ?
N29 C17 C18 N28 1.1(6) . . . . ?
N27 C17 C18 N28 -178.7(3) . . . . ?
N29 C17 C18 C15 178.7(3) . . . . ?
N27 C17 C18 C15 -1.1(4) . . . . ?
C15 N25 C19 C20 95.9(4) . . . . ?
C14 N25 C19 C20 -82.8(4) . . . . ?
N25 C19 C20 C21 176.5(4) . . . . ?
C67 N53 C30 O51 168.0(4) . . . . ?
C67 N53 C30 C31 -12.7(5) . . . . ?
O51 C30 C31 C37 157.2(4) . . . . ?
N53 C30 C31 C37 -22.2(4) . . . . ?
O51 C30 C31 C38 35.5(5) . . . . ?
N53 C30 C31 C38 -143.9(4) . . . . ?
O51 C30 C31 C32 -83.3(4) . . . . ?
N53 C30 C31 C32 97.4(4) . . . . ?
C30 C31 C32 C33 -64.3(4) . . . . ?
C37 C31 C32 C33 55.6(4) . . . . ?
C38 C31 C32 C33 176.8(3) . . . . ?
C31 C32 C33 C41 78.0(4) . . . . ?
C31 C32 C33 C40 -164.8(3) . . . . ?
C31 C32 C33 C34 -45.2(4) . . . . ?
C41 C33 C34 C35 -78.4(4) . . . . ?
C32 C33 C34 C35 44.6(4) . . . . ?
C40 C33 C34 C35 164.2(3) . . . . ?
C33 C34 C35 C67 66.5(4) . . . . ?
C33 C34 C35 C39 -173.8(3) . . . . ?
C33 C34 C35 C37 -53.3(4) . . . . ?
C30 N53 C67 O52 -170.0(3) . . . . ?
C30 N53 C67 C35 10.2(5) . . . . ?
C39 C35 C67 O52 -32.9(5) . . . . ?
C37 C35 C67 O52 -153.4(3) . . . . ?
C34 C35 C67 O52 86.9(4) . . . . ?
C39 C35 C67 N53 146.9(4) . . . . ?
C37 C35 C67 N53 26.4(4) . . . . ?
C34 C35 C67 N53 -93.3(4) . . . . ?
C30 C31 C37 C35 57.4(4) . . . . ?
C38 C31 C37 C35 177.9(3) . . . . ?
C32 C31 C37 C35 -62.3(4) . . . . ?
C67 C35 C37 C31 -59.6(4) . . . . ?
C39 C35 C37 C31 -179.3(3) . . . . ?
C34 C35 C37 C31 61.0(4) . . . . ?
C32 C33 C41 C42 103(7) . . . . ?
C40 C33 C41 C42 -16(7) . . . . ?
C34 C33 C41 C42 -135(7) . . . . ?
C33 C41 C42 C43 141(6) . . . . ?
C47 N57 C43 N54 1.0(4) . . . . ?
C47 N57 C43 C42 -176.7(3) . . . . ?
C44 N54 C43 N57 -1.1(4) . . . . ?
C48 N54 C43 N57 -176.1(3) . . . . ?
C44 N54 C43 C42 176.8(3) . . . . ?
C48 N54 C43 C42 1.8(5) . . . . ?
C41 C42 C43 N57 157(2) . . . . ?
C41 C42 C43 N54 -21(2) . . . . ?
C45 N55 C44 N54 177.5(3) . . . . ?
C45 N55 C44 C47 -0.2(5) . . . . ?
C43 N54 C44 N55 -177.5(3) . . . . ?
C48 N54 C44 N55 -2.4(5) . . . . ?
C43 N54 C44 C47 0.6(4) . . . . ?
C48 N54 C44 C47 175.8(3) . . . . ?
C44 N55 C45 N56 2.1(5) . . . . ?
C46 N56 C45 N55 -2.1(6) . . . . ?
C45 N56 C46 N58 179.9(3) . . . . ?
C45 N56 C46 C47 0.1(5) . . . . ?
N55 C44 C47 N57 178.1(3) . . . . ?
N54 C44 C47 N57 0.0(4) . . . . ?
N55 C44 C47 C46 -1.4(5) . . . . ?
N54 C44 C47 C46 -179.5(3) . . . . ?
C43 N57 C47 C44 -0.6(4) . . . . ?
C43 N57 C47 C46 178.8(4) . . . . ?
N58 C46 C47 C44 -178.5(3) . . . . ?
N56 C46 C47 C44 1.4(5) . . . . ?
N58 C46 C47 N57 2.2(6) . . . . ?
N56 C46 C47 N57 -177.9(3) . . . . ?
C44 N54 C48 C49 95.5(4) . . . . ?
C43 N54 C48 C49 -90.4(5) . . . . ?
N54 C48 C49 C50 -179.9(4) . . . . ?
C62 Cl59 Cl60 Cl61 -4.3(6) . . . . ?
Cl63 Cl59 Cl60 Cl61 -43.9(12) 2_756 . . . ?
Cl59 Cl60 Cl61 Cl63 -100(2) . . . . ?
Cl59 Cl60 Cl61 C62 4.8(7) . . . . ?
C62 Cl59 Cl61 Cl60 174.2(9) . . . . ?
Cl63 Cl59 Cl61 Cl60 152.1(8) 2_756 . . . ?
Cl60 Cl59 Cl61 Cl63 145.7(13) . . . . ?
C62 Cl59 Cl61 Cl63 -40.1(9) . . . . ?
Cl63 Cl59 Cl61 Cl63 -62.1(12) 2_756 . . . ?
Cl60 Cl59 Cl61 C62 -174.2(9) . . . . ?
Cl63 Cl59 Cl61 C62 -22.1(5) 2_756 . . . ?
Cl60 Cl61 C62 Cl61 -18E1(3) . . . 2_756 ?
Cl63 Cl61 C62 Cl61 -2E1(3) . . . 2_756 ?
Cl59 Cl61 C62 Cl61 -17E1(3) . . . 2_756 ?
Cl60 Cl61 C62 Cl59 -4.8(7) . . . . ?
Cl63 Cl61 C62 Cl59 148.8(7) . . . . ?
Cl60 Cl61 C62 Cl59 175.2(7) . . . 2_756 ?
Cl63 Cl61 C62 Cl59 -31.2(7) . . . 2_756 ?
Cl59 Cl61 C62 Cl59 179.998(3) . . . 2_756 ?
Cl60 Cl61 C62 Cl63 -153.6(11) . . . . ?
Cl59 Cl61 C62 Cl63 -148.8(7) . . . . ?
Cl60 Cl61 C62 Cl63 26.4(11) . . . 2_756 ?
Cl63 Cl61 C62 Cl63 179.9980(10) . . . 2_756 ?
Cl59 Cl61 C62 Cl63 31.2(7) . . . 2_756 ?
Cl60 Cl59 C62 Cl61 3.6(5) . . . . ?
Cl63 Cl59 C62 Cl61 156.6(5) 2_756 . . . ?
Cl60 Cl59 C62 Cl61 -176.4(5) . . . 2_756 ?
Cl63 Cl59 C62 Cl61 -23.4(5) 2_756 . . 2_756 ?
Cl61 Cl59 C62 Cl61 180.000(2) . . . 2_756 ?
Cl60 Cl59 C62 Cl59 -6E1(2) . . . 2_756 ?
Cl63 Cl59 C62 Cl59 9E1(2) 2_756 . . 2_756 ?
Cl61 Cl59 C62 Cl59 -7E1(2) . . . 2_756 ?
Cl60 Cl59 C62 Cl63 27.0(6) . . . . ?
Cl63 Cl59 C62 Cl63 180.001(2) 2_756 . . . ?
Cl61 Cl59 C62 Cl63 23.4(5) . . . . ?
Cl60 Cl59 C62 Cl63 -153.0(6) . . . 2_756 ?
Cl61 Cl59 C62 Cl63 -156.6(5) . . . 2_756 ?
Cl60 Cl61 Cl63 C62 110(2) . . . . ?
Cl59 Cl61 Cl63 C62 31.4(7) . . . . ?
Cl60 Cl61 Cl63 Cl59 137(2) . . . 2_756 ?
C62 Cl61 Cl63 Cl59 26.9(6) . . . 2_756 ?
Cl59 Cl61 Cl63 Cl59 58.3(11) . . . 2_756 ?
Cl61 C62 Cl63 Cl61 179.999(3) 2_756 . . . ?
Cl59 C62 Cl63 Cl61 -34.4(8) . . . . ?
Cl59 C62 Cl63 Cl61 145.6(8) 2_756 . . . ?
Cl63 C62 Cl63 Cl61 -109(8) 2_756 . . . ?
Cl61 C62 Cl63 Cl59 -145.6(8) . . . 2_756 ?
Cl61 C62 Cl63 Cl59 34.4(8) 2_756 . . 2_756 ?
Cl59 C62 Cl63 Cl59 180.003(2) . . . 2_756 ?
Cl63 C62 Cl63 Cl59 105(8) 2_756 . . 2_756 ?

_diffrn_measured_fraction_theta_max 0.963
_diffrn_measured_fraction_theta_full 0.963
_refine_diff_density_max         0.789
_refine_diff_density_min         -0.799
_refine_diff_density_rms         0.070



