# Supplementary Material (ESI) for New Journal of Chemistry
# This journal is © The Royal Society of Chemistry and 
# The Centre National de la Recherche Scientifique, 2000
# CCDC Number: 440/164


#----------------------------------------------------------------------

      #1    Data block identification for start of deposition

data_1


#----------------------------------------------------------------------

      #2    Person making the deposition

_publ_contact_author
;
E. F. Paulus
Hoechst Marion Roussel Deutschland GmbH, G864
Hoechst AG
D-65926 Frankfurt/Main, Germany
;
_publ_contact_author_email          erich.paulus@hmrag.com


#----------------------------------------------------------------------

loop_
_publ_author_name
_publ_author_address
'Ch. Schmidt'
;
Institut fuer Organische Chemie
Johannes Gutenberg-Universitaet Mainz
J.-J. Becher Weg, 34 SB1,
D-55099 Mainz, Germany
;
'E. F. Paulus'
;
Hoechst Marion Roussel Deutschland GmbH, G864
D-65926 Frankfurt/Main, Germany
;
'V. Boehmer'
;
Institut fuer Organische Chemie
Johannes Gutenberg-Universitaet Mainz
J.-J. Becher Weg, 34 SB1,
D-55099 Mainz, Germany
;
'W. Vogt'
;
Institut fuer Organische Chemie
Johannes Gutenberg-Universitaet Mainz
J.-J. Becher Weg, 34 SB1,
D-55099 Mainz, Germany
;
_journal_name_full                 'New Journal of Chemistry'
_journal_volume                    '?'
_journal_page_first                '?'
_journal_page_last                 '?'
_journal_year                      '?'
_ccdc_journal_depnumber            '?'

      #SUBMISSION INFORMATION

      #     For a journal send the form to the address specified by the journal

      #     For a private communication to the CCDC send the form to the address
      #       deposit@chemcrys.cam.ac.uk

      #     If you have any problems with the form please contact the CCDC
      #     Technical Editors :
      #       by e-mail:     teched@chemcrys.cam.ac.uk
      #       by telephone:  +44 1223 336031/2



data_sh577

_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C85.50 H126.50 Cl N4.50 O12'
_chemical_formula_weight          1444.86

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            ?
_symmetry_space_group_name_H-M    'P4/ncc'

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

_cell_length_a                    22.03610(10)
_cell_length_b                    22.03610(10)
_cell_length_c                    17.0005(2)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      8255.27(11)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?

_exptl_crystal_description        ?
_exptl_crystal_colour             ?
_exptl_crystal_size_max           ?
_exptl_crystal_size_mid           ?
_exptl_crystal_size_min           ?
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.163
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              3136
_exptl_absorpt_coefficient_mu     0.107
_exptl_absorpt_correction_type    ?
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?

_exptl_special_details
;
 ?
;

_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'rotating anode (focus: 0.5 x 5mm)'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'CCD'
_diffrn_measurement_method        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             39520
_diffrn_reflns_av_R_equivalents   0.0360
_diffrn_reflns_av_sigmaI/netI     0.0147
_diffrn_reflns_limit_h_min        -24
_diffrn_reflns_limit_h_max        24
_diffrn_reflns_limit_k_min        -24
_diffrn_reflns_limit_k_max        24
_diffrn_reflns_limit_l_min        -18
_diffrn_reflns_limit_l_max        18
_diffrn_reflns_theta_min          1.31
_diffrn_reflns_theta_max          23.38
_reflns_number_total              3017
_reflns_number_gt                 2379
_reflns_threshold_expression      2sigma(I)

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

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

_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[\s^2^(Fo^2^)+(0.1198P)^2^+6.6821P] 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        0.0020(4)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_number_reflns          3017
_refine_ls_number_parameters      300
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0931
_refine_ls_R_factor_gt            0.0787
_refine_ls_wR_factor_ref          0.2349
_refine_ls_wR_factor_gt           0.2197
_refine_ls_goodness_of_fit_ref    1.049
_refine_ls_restrained_S_all       1.049
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000

loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_symetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
C01 C 0.35033(9) 0.18914(9) 0.43742(11) 0.0515(5) Uani 1 1 d . . .
C02 C 0.39554(9) 0.22636(9) 0.46711(12) 0.0522(5) Uani 1 1 d . . .
C03 C 0.42914(9) 0.20444(10) 0.53107(13) 0.0573(6) Uani 1 1 d . . .
C04 C 0.41988(10) 0.14628(10) 0.56233(12) 0.0581(6) Uani 1 1 d . . .
C05 C 0.37364(9) 0.11081(9) 0.52938(12) 0.0567(5) Uani 1 1 d . . .
C06 C 0.33824(9) 0.13113(9) 0.46596(11) 0.0519(5) Uani 1 1 d . . .
C07 C 0.40852(9) 0.28849(9) 0.43057(13) 0.0561(6) Uani 1 1 d . . .
C08 C 0.40527(11) 0.28740(11) 0.33947(13) 0.0661(6) Uani 1 1 d . . .
C09 C 0.44628(13) 0.24060(13) 0.29941(15) 0.0835(8) Uani 1 1 d . . .
C10 C 0.51291(15) 0.24843(18) 0.3137(2) 0.1126(11) Uani 1 1 d . . .
C11 C 0.54949(18) 0.2004(3) 0.2677(4) 0.213(3) Uani 1 1 d . . .
H11A H 0.5450 0.1625 0.2960 0.320 Uiso 1 1 calc R . .
H11B H 0.5292 0.1951 0.2176 0.320 Uiso 1 1 calc R . .
C12 C 0.5988(5) 0.2055(4) 0.2546(6) 0.470(5) Uani 1 1 d . . .
H12A H 0.6082 0.2477 0.2479 0.705 Uiso 1 1 calc R . .
H12B H 0.6084 0.1838 0.2072 0.705 Uiso 1 1 calc R . .
H12C H 0.6221 0.1894 0.2975 0.705 Uiso 1 1 calc R . .
C13 C 0.45561(11) 0.12561(11) 0.63410(14) 0.0709(7) Uani 1 1 d . . .
C14 C 0.49234(12) 0.02169(12) 0.63599(17) 0.0852(8) Uani 1 1 d . . .
C15 C 0.54247(14) -0.02517(14) 0.6373(2) 0.1159(12) Uani 1 1 d . . .
H15A H 0.5266 -0.0631 0.6558 0.174 Uiso 1 1 calc R . .
H15B H 0.5743 -0.0118 0.6717 0.174 Uiso 1 1 calc R . .
H15C H 0.5584 -0.0303 0.5851 0.174 Uiso 1 1 calc R . .
C16 C 0.56522(12) 0.09996(14) 0.59325(19) 0.0902(9) Uani 1 1 d . . .
C17 C 0.56854(17) 0.1052(2) 0.5073(2) 0.1368(15) Uani 1 1 d . . .
H17A H 0.5395 0.1354 0.4899 0.205 Uiso 1 1 calc R . .
H17B H 0.5571 0.0666 0.4841 0.205 Uiso 1 1 calc R . .
C18 C 0.6317(2) 0.1228(3) 0.4779(3) 0.211(2) Uani 1 1 d . . .
H18A H 0.6588 0.0884 0.4833 0.317 Uiso 1 1 calc R . .
H18B H 0.6294 0.1331 0.4225 0.317 Uiso 1 1 calc R . .
C19 C 0.6552(3) 0.1717(3) 0.5191(6) 0.288(5) Uani 1 1 d . . .
H19A H 0.6327 0.2076 0.5034 0.432 Uiso 1 1 calc R . .
H19B H 0.6968 0.1774 0.5020 0.432 Uiso 1 1 calc R . .
C20 C 0.65505(19) 0.1691(3) 0.6057(4) 0.209(3) Uani 1 1 d . . .
H20A H 0.6666 0.2083 0.6267 0.314 Uiso 1 1 calc R . .
H20B H 0.6846 0.1395 0.6233 0.314 Uiso 1 1 calc R . .
C21 C 0.59182(17) 0.1517(2) 0.6369(3) 0.1593(18) Uani 1 1 d . . .
H21A H 0.5950 0.1411 0.6921 0.239 Uiso 1 1 calc R . .
H21B H 0.5650 0.1864 0.6326 0.239 Uiso 1 1 calc R . .
H01 H 0.3232(9) 0.2036(9) 0.3946(12) 0.061(6) Uiso 1 1 d . . .
H07 H 0.4515(9) 0.2978(8) 0.4459(10) 0.052(5) Uiso 1 1 d . . .
H081 H 0.4126(10) 0.3273(11) 0.3184(13) 0.075(7) Uiso 1 1 d . . .
H082 H 0.3612(10) 0.2810(10) 0.3237(12) 0.065(6) Uiso 1 1 d . . .
H091 H 0.4429(12) 0.2374(13) 0.2360(18) 0.112(9) Uiso 1 1 d . . .
H092 H 0.4399(13) 0.1949(13) 0.3177(16) 0.105(9) Uiso 1 1 d . . .
H101 H 0.5305(19) 0.3013(19) 0.303(3) 0.180(16) Uiso 1 1 d . . .
H102 H 0.5157(16) 0.2344(16) 0.364(2) 0.134(12) Uiso 1 1 d . . .
H131 H 0.4742(11) 0.1630(12) 0.6593(14) 0.088(8) Uiso 1 1 d . . .
H132 H 0.4260(12) 0.1040(12) 0.6751(16) 0.095(8) Uiso 1 1 d . . .
H16 H 0.6035(18) 0.0796(18) 0.631(2) 0.169(15) Uiso 1 1 d . . .
H1 H 0.4612(13) 0.2827(13) 0.5628(16) 0.106(9) Uiso 1 1 d . . .
H2 H 0.3908(14) 0.0413(13) 0.6005(18) 0.119(10) Uiso 1 1 d . . .
N1 N 0.50490(9) 0.08072(9) 0.62179(12) 0.0729(6) Uani 1 1 d . . .
O1 O 0.47363(7) 0.23909(8) 0.56601(10) 0.0783(5) Uani 1 1 d . . .
O2 O 0.35997(7) 0.05395(7) 0.55879(10) 0.0741(5) Uani 1 1 d . . .
O3 O 0.44008(9) 0.00480(9) 0.64930(15) 0.1102(7) Uani 1 1 d . . .
C1 C 0.2500 0.2500 0.1075(4) 0.160(4) Uani 0.526(5) 4 d SP A 1
C2 C 0.2500 0.2500 0.1900(6) 0.084(3) Uani 0.526(5) 4 d SP A 1
N2 N 0.2500 0.2500 0.2546(6) 0.119(4) Uani 0.526(5) 4 d SP A 1
C3 C 0.2500 0.2500 0.1075(4) 0.160(4) Uani 0.474(5) 4 d SP . 2
Cl1 Cl 0.3074(3) 0.2250(5) 0.1666(4) 0.233(4) Uani 0.237(3) 1 d P A 2

loop_
 _atom_site_aniso_label
 _atom_site_aniso_U_11
 _atom_site_aniso_U_22
 _atom_site_aniso_U_33
 _atom_site_aniso_U_23
 _atom_site_aniso_U_13
 _atom_site_aniso_U_12
C01 0.0489(10) 0.0551(11) 0.0507(10) 0.0030(9) 0.0014(9) 0.0059(9)
C02 0.0463(10) 0.0548(11) 0.0554(10) 0.0019(9) 0.0026(9) 0.0035(9)
C03 0.0514(11) 0.0595(12) 0.0610(12) -0.0042(10) -0.0033(10) 0.0059(9)
C04 0.0568(11) 0.0593(12) 0.0582(11) -0.0003(10) -0.0026(10) 0.0108(10)
C05 0.0564(11) 0.0517(11) 0.0619(11) 0.0071(10) 0.0045(10) 0.0073(9)
C06 0.0485(10) 0.0517(11) 0.0554(10) 0.0001(9) 0.0041(9) 0.0052(9)
C07 0.0456(10) 0.0560(11) 0.0666(12) 0.0023(10) 0.0016(9) -0.0033(9)
C08 0.0690(13) 0.0661(13) 0.0630(13) 0.0055(11) 0.0097(11) -0.0051(11)
C09 0.0938(17) 0.0815(16) 0.0752(15) -0.0045(14) 0.0240(14) -0.0013(14)
C10 0.092(2) 0.125(3) 0.121(2) -0.008(2) 0.0230(19) 0.0140(19)
C11 0.101(2) 0.281(6) 0.258(5) -0.068(5) 0.061(3) 0.066(3)
C12 0.672(12) 0.351(9) 0.388(10) 0.113(8) 0.325(9) 0.314(9)
C13 0.0746(14) 0.0730(14) 0.0650(13) 0.0013(12) -0.0104(12) 0.0186(12)
C14 0.0793(16) 0.0767(16) 0.0995(18) 0.0146(14) -0.0170(15) 0.0157(13)
C15 0.099(2) 0.0831(18) 0.165(3) 0.012(2) -0.029(2) 0.0296(16)
C16 0.0697(15) 0.104(2) 0.0969(19) 0.0073(17) -0.0105(15) 0.0026(15)
C17 0.118(3) 0.191(4) 0.102(2) 0.018(3) 0.032(2) 0.021(3)
C18 0.145(3) 0.297(6) 0.193(4) 0.096(4) 0.076(3) 0.064(4)
C19 0.157(4) 0.150(5) 0.557(13) 0.042(7) 0.139(6) -0.004(4)
C20 0.079(2) 0.192(5) 0.356(8) -0.040(6) -0.029(4) -0.018(3)
C21 0.099(2) 0.162(3) 0.217(4) -0.061(3) -0.019(3) -0.024(3)
N1 0.0664(11) 0.0751(12) 0.0772(12) 0.0075(10) -0.0093(10) 0.0146(10)
O1 0.0731(9) 0.0663(10) 0.0953(11) -0.0010(9) -0.0316(9) 0.0005(8)
O2 0.0711(10) 0.0634(9) 0.0879(11) 0.0219(8) -0.0087(9) 0.0018(8)
O3 0.0838(12) 0.0901(12) 0.1567(18) 0.0492(12) -0.0177(12) 0.0088(10)
C1 0.201(5) 0.201(5) 0.078(4) 0.000 0.000 0.000
C2 0.095(4) 0.095(4) 0.061(5) 0.000 0.000 0.000
N2 0.141(5) 0.141(5) 0.077(6) 0.000 0.000 0.000
C3 0.201(5) 0.201(5) 0.078(4) 0.000 0.000 0.000
Cl1 0.185(6) 0.346(10) 0.168(5) -0.021(7) 0.009(5) 0.087(6)

_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
C01 C02 1.386(3) . ?
C01 C06 1.393(3) . ?
C01 H01 0.99(2) . ?
C02 C03 1.401(3) . ?
C02 C07 1.530(3) . ?
C03 O1 1.377(3) . ?
C03 C04 1.402(3) . ?
C04 C05 1.401(3) . ?
C04 C13 1.522(3) . ?
C05 O2 1.382(3) . ?
C05 C06 1.404(3) . ?
C06 C07 1.525(3) 4 ?
C07 C06 1.525(3) 3 ?
C07 C08 1.551(3) . ?
C07 H07 1.005(19) . ?
C08 C09 1.531(4) . ?
C08 H081 0.96(2) . ?
C08 H082 1.02(2) . ?
C09 C10 1.498(4) . ?
C09 H091 1.08(3) . ?
C09 H092 1.06(3) . ?
C10 C11 1.543(6) . ?
C10 H101 1.24(4) . ?
C10 H102 0.91(3) . ?
C11 C12 1.114(10) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 N1 1.484(3) . ?
C13 H131 1.02(3) . ?
C13 H132 1.07(3) . ?
C14 O3 1.231(3) . ?
C14 N1 1.352(3) . ?
C14 C15 1.512(4) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17 1.467(5) . ?
C16 N1 1.477(3) . ?
C16 C21 1.481(5) . ?
C16 H16 1.15(4) . ?
C17 C18 1.529(6) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.384(9) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.474(11) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.539(6) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
O1 H1 1.00(3) . ?
O2 H2 1.02(3) . ?
C1 C2 1.403(12) . ?
C2 N2 1.099(13) . ?
Cl1 Cl1 1.952(10) 4 ?
Cl1 Cl1 1.952(10) 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
C02 C01 C06 123.64(18) . . ?
C02 C01 H01 120.6(12) . . ?
C06 C01 H01 115.7(12) . . ?
C01 C02 C03 117.29(18) . . ?
C01 C02 C07 121.07(18) . . ?
C03 C02 C07 121.64(18) . . ?
O1 C03 C02 121.31(19) . . ?
O1 C03 C04 116.54(18) . . ?
C02 C03 C04 122.15(19) . . ?
C05 C04 C03 117.66(19) . . ?
C05 C04 C13 122.0(2) . . ?
C03 C04 C13 120.1(2) . . ?
O2 C05 C04 121.30(18) . . ?
O2 C05 C06 116.47(18) . . ?
C04 C05 C06 122.23(19) . . ?
C01 C06 C05 116.98(18) . . ?
C01 C06 C07 121.72(18) . 4 ?
C05 C06 C07 121.30(18) . 4 ?
C06 C07 C02 112.06(16) 3 . ?
C06 C07 C08 112.25(17) 3 . ?
C02 C07 C08 112.52(18) . . ?
C06 C07 H07 106.9(11) 3 . ?
C02 C07 H07 104.7(11) . . ?
C08 C07 H07 107.8(10) . . ?
C09 C08 C07 115.3(2) . . ?
C09 C08 H081 110.6(14) . . ?
C07 C08 H081 110.5(13) . . ?
C09 C08 H082 110.7(12) . . ?
C07 C08 H082 108.0(12) . . ?
H081 C08 H082 100.8(18) . . ?
C10 C09 C08 115.4(2) . . ?
C10 C09 H091 103.7(15) . . ?
C08 C09 H091 116.5(15) . . ?
C10 C09 H092 101.0(15) . . ?
C08 C09 H092 115.5(15) . . ?
H091 C09 H092 103(2) . . ?
C09 C10 C11 110.5(3) . . ?
C09 C10 H101 113(2) . . ?
C11 C10 H101 114(2) . . ?
C09 C10 H102 100(2) . . ?
C11 C10 H102 102(2) . . ?
H101 C10 H102 115(3) . . ?
C12 C11 C10 122.8(7) . . ?
C12 C11 H11A 106.6 . . ?
C10 C11 H11A 106.6 . . ?
C12 C11 H11B 106.6 . . ?
C10 C11 H11B 106.6 . . ?
H11A C11 H11B 106.6 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N1 C13 C04 117.72(19) . . ?
N1 C13 H131 107.7(14) . . ?
C04 C13 H131 107.7(14) . . ?
N1 C13 H132 104.0(15) . . ?
C04 C13 H132 110.0(14) . . ?
H131 C13 H132 109(2) . . ?
O3 C14 N1 121.0(2) . . ?
O3 C14 C15 118.3(3) . . ?
N1 C14 C15 120.7(3) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 N1 113.2(3) . . ?
C17 C16 C21 114.8(3) . . ?
N1 C16 C21 114.3(3) . . ?
C17 C16 H16 123(2) . . ?
N1 C16 H16 111(2) . . ?
C21 C16 H16 74(2) . . ?
C16 C17 C18 113.1(3) . . ?
C16 C17 H17A 109.0 . . ?
C18 C17 H17A 109.0 . . ?
C16 C17 H17B 109.0 . . ?
C18 C17 H17B 109.0 . . ?
H17A C17 H17B 107.8 . . ?
C19 C18 C17 111.8(5) . . ?
C19 C18 H18A 109.2 . . ?
C17 C18 H18A 109.2 . . ?
C19 C18 H18B 109.2 . . ?
C17 C18 H18B 109.2 . . ?
H18A C18 H18B 107.9 . . ?
C18 C19 C20 118.4(6) . . ?
C18 C19 H19A 107.7 . . ?
C20 C19 H19A 107.7 . . ?
C18 C19 H19B 107.7 . . ?
C20 C19 H19B 107.7 . . ?
H19A C19 H19B 107.1 . . ?
C19 C20 C21 110.8(5) . . ?
C19 C20 H20A 109.5 . . ?
C21 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C21 C20 H20B 109.5 . . ?
H20A C20 H20B 108.1 . . ?
C16 C21 C20 112.2(4) . . ?
C16 C21 H21A 109.2 . . ?
C20 C21 H21A 109.2 . . ?
C16 C21 H21B 109.2 . . ?
C20 C21 H21B 109.2 . . ?
H21A C21 H21B 107.9 . . ?
C14 N1 C16 121.3(2) . . ?
C14 N1 C13 117.8(2) . . ?
C16 N1 C13 120.9(2) . . ?
C03 O1 H1 108.3(16) . . ?
C05 O2 H2 110.7(17) . . ?
N2 C2 C1 180.000(2) . . ?
Cl1 Cl1 Cl1 90.0 4 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
C06 C01 C02 C03 -2.2(3) . . . . ?
C06 C01 C02 C07 177.07(18) . . . . ?
C01 C02 C03 O1 -177.89(18) . . . . ?
C07 C02 C03 O1 2.9(3) . . . . ?
C01 C02 C03 C04 2.8(3) . . . . ?
C07 C02 C03 C04 -176.47(19) . . . . ?
O1 C03 C04 C05 178.11(18) . . . . ?
C02 C03 C04 C05 -2.5(3) . . . . ?
O1 C03 C04 C13 3.3(3) . . . . ?
C02 C03 C04 C13 -177.31(19) . . . . ?
C03 C04 C05 O2 -177.42(19) . . . . ?
C13 C04 C05 O2 -2.7(3) . . . . ?
C03 C04 C05 C06 1.6(3) . . . . ?
C13 C04 C05 C06 176.31(19) . . . . ?
C02 C01 C06 C05 1.3(3) . . . . ?
C02 C01 C06 C07 -179.15(18) . . . 4 ?
O2 C05 C06 C01 178.05(17) . . . . ?
C04 C05 C06 C01 -1.0(3) . . . . ?
O2 C05 C06 C07 -1.5(3) . . . 4 ?
C04 C05 C06 C07 179.45(19) . . . 4 ?
C01 C02 C07 C06 87.4(2) . . . 3 ?
C03 C02 C07 C06 -93.4(2) . . . 3 ?
C01 C02 C07 C08 -40.2(3) . . . . ?
C03 C02 C07 C08 139.0(2) . . . . ?
C06 C07 C08 C09 177.17(19) 3 . . . ?
C02 C07 C08 C09 -55.3(3) . . . . ?
C07 C08 C09 C10 -61.3(3) . . . . ?
C08 C09 C10 C11 -177.7(3) . . . . ?
C09 C10 C11 C12 161.0(8) . . . . ?
C05 C04 C13 N1 79.1(3) . . . . ?
C03 C04 C13 N1 -106.4(3) . . . . ?
N1 C16 C17 C18 -177.9(4) . . . . ?
C21 C16 C17 C18 48.3(5) . . . . ?
C16 C17 C18 C19 -48.1(7) . . . . ?
C17 C18 C19 C20 50.9(7) . . . . ?
C18 C19 C20 C21 -50.2(8) . . . . ?
C17 C16 C21 C20 -47.7(5) . . . . ?
N1 C16 C21 C20 179.0(4) . . . . ?
C19 C20 C21 C16 45.7(7) . . . . ?
O3 C14 N1 C16 -170.0(3) . . . . ?
C15 C14 N1 C16 11.1(4) . . . . ?
O3 C14 N1 C13 8.7(4) . . . . ?
C15 C14 N1 C13 -170.2(3) . . . . ?
C17 C16 N1 C14 94.3(3) . . . . ?
C21 C16 N1 C14 -131.7(3) . . . . ?
C17 C16 N1 C13 -84.3(3) . . . . ?
C21 C16 N1 C13 49.7(4) . . . . ?
C04 C13 N1 C14 -97.9(3) . . . . ?
C04 C13 N1 C16 80.7(3) . . . . ?

_diffrn_measured_fraction_theta_max    0.998
_diffrn_reflns_theta_full              23.38
_diffrn_measured_fraction_theta_full   0.998
_refine_diff_density_max    0.427
_refine_diff_density_min   -0.325
_refine_diff_density_rms    0.049