# Supplementary Material (ESI) for Perkin Transactions
# This journal is © The Royal Society of Chemistry 2002


data_global

_journal_coden_Cambridge      207

_publ_requested_journal       'Perkin Transactions 1'

loop_
_publ_author_name
'Gallagher, Timothy'
'Andrews, Mark'
'Brown, David'
'Brown, Giles A.'
'Butts, Craig P.'
'Hales, Neil J.'
'Large, Jonathan M.'
'Urban, Dominique'

_publ_contact_author_name     	'Prof Timothy Gallagher'  
_publ_contact_author_address 
;
Department of Chemistry
University of Bristol
School of Chemistry
Bristol
BS8 1TS
UNITED KINGDOM
;

_publ_contact_author_email       'T.GALLAGHER@BRISTOL.AC.UK'

_publ_section_title		
;
The Azomethine Ylid Strategy for b-Lactam Synthesis.  Azapenams
and 1-Azacephams
;

data_rushjob

_database_code_CSD	184386


_audit_creation_method            SHELXL
_chemical_name_systematic
;
?
;
_chemical_name_common             ?
_chemical_formula_moiety          ?
_chemical_formula_structural      ?
_chemical_formula_analytical      ?
_chemical_formula_sum             'C30 H25 N3 O7 S'
_chemical_formula_weight          571.59
_chemical_melting_point           ?
_chemical_compound_source         ?

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'
'S'  'S'   0.1246   0.1234
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting            Monoclinic
_symmetry_space_group_name_H-M    C2/c

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

_cell_length_a                    43.767(8)
_cell_length_b                    5.8471(10)
_cell_length_c                    22.777(5)
_cell_angle_alpha                 90.00
_cell_angle_beta                  113.782(13)
_cell_angle_gamma                 90.00
_cell_volume                      5333.9(18)
_cell_formula_units_Z             8
_cell_measurement_temperature     173(2)
_cell_measurement_reflns_used     150
_cell_measurement_theta_min       1.75
_cell_measurement_theta_max       27.5

_exptl_crystal_description        Rectangular
_exptl_crystal_colour             Colourless
_exptl_crystal_size_max           .65
_exptl_crystal_size_mid           .26
_exptl_crystal_size_min           .1
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.424
_exptl_crystal_density_method     None
_exptl_crystal_F_000              2384
_exptl_absorpt_coefficient_mu     0.177
_exptl_absorpt_correction_type    none
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?

_exptl_special_details
;
?
;

_diffrn_ambient_temperature       173(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        'Siemens SMART Area Detector'
_diffrn_measurement_method        '\w rotation with narrow frames'
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             26690
_diffrn_reflns_av_R_equivalents   0.0672
_diffrn_reflns_av_sigmaI/netI     0.0534
_diffrn_reflns_limit_h_min        -56
_diffrn_reflns_limit_h_max        56
_diffrn_reflns_limit_k_min        -7
_diffrn_reflns_limit_k_max        7
_diffrn_reflns_limit_l_min        -29
_diffrn_reflns_limit_l_max        29
_diffrn_reflns_theta_min          1.80
_diffrn_reflns_theta_max          27.49
_reflns_number_total              6143
_reflns_number_gt                 3655
_reflns_threshold_expression                 >2sigma(I)

_computing_data_collection        'SMART (Siemens, 1995b)'
_computing_cell_refinement        'SMART (Siemens, 1995b)'
_computing_data_reduction         'SMART (Siemens, 1995b)'
_computing_structure_solution     'SHELXTL (Siemens, 1995a)'
_computing_structure_refinement   'SHELXTL (Siemens, 1995a)'
_computing_molecular_graphics     'SHELXTL (Siemens, 1995a)'
_computing_publication_material   'SHELXTL (Siemens, 1995a)'

_refine_special_details
;
Refinement on F^2^ for ALL reflections except for 0 with very negative
F^2^ or flagged by the user for potential systematic errors.  Weighted 
R-factors wR and all goodnesses 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 observed 
criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     noref
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          6143
_refine_ls_number_parameters      370
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1021
_refine_ls_R_factor_gt           0.0491
_refine_ls_wR_factor_all          0.1185
_refine_ls_wR_factor_ref          0.0992
_refine_ls_goodness_of_fit_all    1.009
_refine_ls_goodness_of_fit_ref    1.115
_refine_ls_restrained_S_all       1.009
_refine_ls_restrained_S_obs       1.115
_refine_ls_shift/su_max          0.001
_refine_ls_shift/esd_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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
N1 N 0.06086(4) 0.1705(3) 0.13100(8) 0.0365(4) Uani 1 d . .
C2 C 0.06974(5) 0.2643(4) 0.19679(10) 0.0346(5) Uani 1 d . .
H2A H 0.06796(5) 0.4348(4) 0.19384(10) 0.042 Uiso 1 calc R .
C3 C 0.04133(5) 0.1706(4) 0.21577(10) 0.0382(5) Uani 1 d . .
H3A H 0.03372(5) 0.2942(4) 0.23710(10) 0.046 Uiso 1 calc R .
N4 N 0.01480(4) 0.1147(3) 0.15448(9) 0.0412(5) Uani 1 d . .
C5 C 0.02681(5) 0.0714(4) 0.10399(11) 0.0409(6) Uani 1 d . .
H5A H 0.02598(5) -0.0930(4) 0.09134(11) 0.049 Uiso 1 calc R .
C6 C -0.00255(6) 0.2174(5) 0.05758(12) 0.0559(7) Uani 1 d . .
H6A H 0.00429(6) 0.3492(5) 0.03838(12) 0.067 Uiso 1 calc R .
H6B H -0.02060(6) 0.1280(5) 0.02473(12) 0.067 Uiso 1 calc R .
C7 C -0.00874(6) 0.2747(5) 0.11655(14) 0.0564(7) Uani 1 d . .
O8 O -0.02551(5) 0.4051(4) 0.13112(10) 0.0825(7) Uani 1 d . .
S9 S 0.074608(14) 0.29938(11) 0.08227(3) 0.0420(2) Uani 1 d . .
O10 O 0.07283(4) 0.5427(3) 0.08796(8) 0.0529(5) Uani 1 d . .
O11 O 0.05717(4) 0.1934(3) 0.02086(7) 0.0565(5) Uani 1 d . .
C12 C 0.11705(5) 0.2231(4) 0.11170(10) 0.0361(5) Uani 1 d . .
C13 C 0.12618(6) 0.0119(4) 0.09628(10) 0.0402(6) Uani 1 d . .
H13A H 0.10975(6) -0.0895(4) 0.06848(10) 0.048 Uiso 1 calc R .
C14 C 0.15962(6) -0.0492(4) 0.12198(11) 0.0423(6) Uani 1 d . .
H14A H 0.16601(6) -0.1929(4) 0.11103(11) 0.051 Uiso 1 calc R .
C15 C 0.18404(6) 0.0956(4) 0.16352(11) 0.0419(6) Uani 1 d . .
C16 C 0.17411(6) 0.3072(4) 0.17763(11) 0.0415(6) Uani 1 d . .
H16A H 0.19048(6) 0.4086(4) 0.20561(11) 0.050 Uiso 1 calc R .
C17 C 0.14104(6) 0.3732(4) 0.15192(10) 0.0383(5) Uani 1 d . .
H17A H 0.13472(6) 0.5192(4) 0.16156(10) 0.046 Uiso 1 calc R .
C18 C 0.22021(6) 0.0237(5) 0.19304(13) 0.0607(8) Uani 1 d . .
H18A H 0.22245(6) -0.1293(5) 0.17766(13) 0.091 Uiso 1 calc R .
H18B H 0.22806(6) 0.0212(5) 0.23986(13) 0.091 Uiso 1 calc R .
H18C H 0.23362(6) 0.1326(5) 0.18075(13) 0.091 Uiso 1 calc R .
C19 C 0.10484(5) 0.2017(4) 0.24260(9) 0.0328(5) Uani 1 d . .
C20 C 0.12336(5) 0.3560(4) 0.28807(10) 0.0333(5) Uani 1 d . .
H20A H 0.11360(5) 0.4975(4) 0.29171(10) 0.040 Uiso 1 calc R .
C21 C 0.15721(5) 0.3082(4) 0.33032(9) 0.0321(5) Uani 1 d . .
C22 C 0.17683(6) 0.4663(4) 0.37694(10) 0.0387(5) Uani 1 d . .
H22A H 0.16728(6) 0.6067(4) 0.38213(10) 0.046 Uiso 1 calc R .
C23 C 0.20932(6) 0.4197(4) 0.41456(11) 0.0439(6) Uani 1 d . .
H23A H 0.22226(6) 0.5277(4) 0.44585(11) 0.053 Uiso 1 calc R .
C24 C 0.22401(6) 0.2124(4) 0.40760(11) 0.0440(6) Uani 1 d . .
H24A H 0.24681(6) 0.1829(4) 0.43390(11) 0.053 Uiso 1 calc R .
C25 C 0.20580(6) 0.0545(4) 0.36357(10) 0.0410(6) Uani 1 d . .
H25A H 0.21592(6) -0.0851(4) 0.35966(10) 0.049 Uiso 1 calc R .
C26 C 0.17144(5) 0.0971(4) 0.32296(10) 0.0334(5) Uani 1 d . .
C27 C 0.15151(5) -0.0617(4) 0.27631(10) 0.0364(5) Uani 1 d . .
H27A H 0.16075(5) -0.2044(4) 0.27193(10) 0.044 Uiso 1 calc R .
C28 C 0.11923(5) -0.0119(4) 0.23772(10) 0.0348(5) Uani 1 d . .
H28A H 0.10612(5) -0.1213(4) 0.20708(10) 0.042 Uiso 1 calc R .
C29 C 0.05088(6) -0.0401(5) 0.25828(12) 0.0423(6) Uani 1 d . .
O30 O 0.05160(5) -0.2304(3) 0.23943(9) 0.0627(5) Uani 1 d . .
O31 O 0.05765(4) 0.0171(3) 0.31877(8) 0.0535(5) Uani 1 d . .
C32 C 0.06239(6) -0.1704(5) 0.36370(13) 0.0626(8) Uani 1 d . .
H32A H 0.05410(6) -0.3138(5) 0.33933(13) 0.075 Uiso 1 calc R .
H32B H 0.04898(6) -0.1407(5) 0.38903(13) 0.075 Uiso 1 calc R .
C33 C 0.09818(6) -0.2010(4) 0.40848(11) 0.0409(6) Uani 1 d . .
C34 C 0.12280(6) -0.0388(4) 0.41758(11) 0.0428(6) Uani 1 d . .
H34A H 0.11732(6) 0.0983(4) 0.39315(11) 0.051 Uiso 1 calc R .
C35 C 0.15520(6) -0.0735(4) 0.46163(11) 0.0434(6) Uani 1 d . .
H35A H 0.17202(6) 0.0378(4) 0.46774(11) 0.052 Uiso 1 calc R .
C36 C 0.16246(6) -0.2742(4) 0.49651(10) 0.0394(5) Uani 1 d . .
C37 C 0.13859(6) -0.4400(4) 0.48846(11) 0.0412(6) Uani 1 d . .
H37A H 0.14422(6) -0.5771(4) 0.51292(11) 0.049 Uiso 1 calc R .
C38 C 0.10651(6) -0.4025(4) 0.44429(11) 0.0419(6) Uani 1 d . .
H38A H 0.08984(6) -0.5151(4) 0.43810(11) 0.050 Uiso 1 calc R .
N39 N 0.19673(5) -0.3167(4) 0.54286(10) 0.0525(6) Uani 1 d . .
O40 O 0.21800(5) -0.1724(4) 0.54843(10) 0.0742(6) Uani 1 d . .
O41 O 0.20265(4) -0.4940(4) 0.57417(9) 0.0664(6) Uani 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
N1 0.0344(10) 0.0378(11) 0.0336(9) 0.0024(8) 0.0099(8) -0.0068(8)
C2 0.0384(12) 0.0261(12) 0.0359(11) 0.0021(9) 0.0113(10) 0.0029(9)
C3 0.0380(12) 0.0359(13) 0.0419(13) 0.0035(10) 0.0174(10) 0.0069(10)
N4 0.0319(10) 0.0413(12) 0.0492(11) 0.0023(9) 0.0152(9) 0.0033(8)
C5 0.0370(13) 0.0390(14) 0.0440(13) -0.0002(11) 0.0135(11) -0.0065(10)
C6 0.0417(14) 0.064(2) 0.049(2) 0.0069(14) 0.0053(12) -0.0040(13)
C7 0.0377(14) 0.055(2) 0.066(2) 0.0055(14) 0.0106(13) 0.0076(13)
O8 0.0625(13) 0.085(2) 0.088(2) 0.0068(13) 0.0179(12) 0.0383(12)
S9 0.0412(3) 0.0435(4) 0.0374(3) 0.0098(3) 0.0119(3) -0.0051(3)
O10 0.0539(10) 0.0384(10) 0.0636(11) 0.0203(9) 0.0208(9) 0.0030(8)
O11 0.0505(10) 0.0792(13) 0.0333(9) 0.0052(9) 0.0099(8) -0.0149(10)
C12 0.0429(13) 0.0348(13) 0.0325(11) 0.0035(10) 0.0172(10) -0.0046(10)
C13 0.0503(15) 0.0372(14) 0.0350(12) -0.0047(10) 0.0191(11) -0.0135(11)
C14 0.057(2) 0.0334(14) 0.0445(13) 0.0013(11) 0.0290(12) -0.0003(12)
C15 0.0451(14) 0.0431(15) 0.0405(13) 0.0032(11) 0.0204(11) -0.0034(12)
C16 0.0443(14) 0.0385(14) 0.0415(13) -0.0029(11) 0.0172(11) -0.0119(11)
C17 0.0458(14) 0.0299(13) 0.0406(13) -0.0005(10) 0.0187(11) -0.0072(10)
C18 0.051(2) 0.067(2) 0.062(2) 0.0028(15) 0.0200(14) 0.0067(14)
C19 0.0369(12) 0.0320(12) 0.0306(11) 0.0066(10) 0.0148(9) -0.0011(10)
C20 0.0409(12) 0.0275(12) 0.0339(11) 0.0038(9) 0.0176(10) 0.0019(10)
C21 0.0403(12) 0.0287(12) 0.0314(11) 0.0036(9) 0.0188(10) -0.0011(10)
C22 0.0495(14) 0.0356(13) 0.0346(12) -0.0012(10) 0.0207(11) -0.0016(11)
C23 0.0424(14) 0.050(2) 0.0369(12) 0.0003(11) 0.0137(11) -0.0053(12)
C24 0.0344(12) 0.055(2) 0.0392(13) 0.0040(12) 0.0112(10) 0.0012(12)
C25 0.0410(13) 0.0428(14) 0.0398(12) 0.0052(11) 0.0168(11) 0.0035(11)
C26 0.0408(13) 0.0311(12) 0.0321(11) 0.0035(9) 0.0188(10) -0.0016(10)
C27 0.0448(13) 0.0277(12) 0.0392(12) 0.0045(10) 0.0195(11) 0.0046(10)
C28 0.0415(13) 0.0279(12) 0.0353(12) 0.0038(9) 0.0157(10) -0.0003(10)
C29 0.0373(13) 0.044(2) 0.0523(15) 0.0106(12) 0.0255(11) 0.0082(11)
O30 0.0864(14) 0.0395(12) 0.0768(13) 0.0130(10) 0.0482(11) 0.0123(10)
O31 0.0565(11) 0.0606(12) 0.0463(10) 0.0157(9) 0.0238(8) 0.0064(9)
C32 0.053(2) 0.082(2) 0.056(2) 0.032(2) 0.0252(13) 0.0027(15)
C33 0.0465(13) 0.0466(15) 0.0380(12) 0.0042(11) 0.0256(11) 0.0031(12)
C34 0.057(2) 0.0365(14) 0.0462(13) 0.0024(11) 0.0321(12) 0.0016(12)
C35 0.0515(15) 0.0419(15) 0.0466(14) -0.0100(11) 0.0300(12) -0.0099(12)
C36 0.0425(13) 0.0439(15) 0.0377(12) -0.0019(11) 0.0223(11) 0.0024(11)
C37 0.0532(15) 0.0345(14) 0.0444(13) 0.0039(11) 0.0285(12) 0.0016(11)
C38 0.0459(14) 0.0411(14) 0.0438(13) -0.0006(11) 0.0232(12) -0.0067(11)
N39 0.0458(13) 0.069(2) 0.0507(13) -0.0038(12) 0.0276(11) -0.0005(13)
O40 0.0515(12) 0.097(2) 0.0720(13) -0.0006(12) 0.0230(10) -0.0191(12)
O41 0.0546(12) 0.0794(15) 0.0699(13) 0.0195(12) 0.0300(10) 0.0200(11)

_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
N1 C5 1.481(3) . ?
N1 C2 1.493(3) . ?
N1 S9 1.643(2) . ?
C2 C19 1.513(3) . ?
C2 C3 1.571(3) . ?
C3 N4 1.448(3) . ?
C3 C29 1.518(3) . ?
N4 C7 1.402(3) . ?
N4 C5 1.466(3) . ?
C5 C6 1.550(3) . ?
C6 C7 1.511(4) . ?
C7 O8 1.195(3) . ?
S9 O10 1.434(2) . ?
S9 O11 1.436(2) . ?
S9 C12 1.759(2) . ?
C12 C13 1.386(3) . ?
C12 C17 1.391(3) . ?
C13 C14 1.386(3) . ?
C14 C15 1.393(3) . ?
C15 C16 1.391(3) . ?
C15 C18 1.509(3) . ?
C16 C17 1.380(3) . ?
C19 C20 1.366(3) . ?
C19 C28 1.423(3) . ?
C20 C21 1.431(3) . ?
C21 C22 1.409(3) . ?
C21 C26 1.422(3) . ?
C22 C23 1.359(3) . ?
C23 C24 1.410(3) . ?
C24 C25 1.360(3) . ?
C25 C26 1.434(3) . ?
C26 C27 1.416(3) . ?
C27 C28 1.361(3) . ?
C29 O30 1.197(3) . ?
C29 O31 1.330(3) . ?
O31 C32 1.456(3) . ?
C32 C33 1.496(3) . ?
C33 C34 1.387(3) . ?
C33 C38 1.395(3) . ?
C34 C35 1.382(3) . ?
C35 C36 1.380(3) . ?
C36 C37 1.382(3) . ?
C36 N39 1.466(3) . ?
C37 C38 1.376(3) . ?
N39 O40 1.224(3) . ?
N39 O41 1.226(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
C5 N1 C2 111.8(2) . . ?
C5 N1 S9 118.67(14) . . ?
C2 N1 S9 119.42(14) . . ?
N1 C2 C19 112.6(2) . . ?
N1 C2 C3 103.5(2) . . ?
C19 C2 C3 115.0(2) . . ?
N4 C3 C29 109.8(2) . . ?
N4 C3 C2 103.3(2) . . ?
C29 C3 C2 114.5(2) . . ?
C7 N4 C3 123.2(2) . . ?
C7 N4 C5 92.2(2) . . ?
C3 N4 C5 113.2(2) . . ?
N4 C5 N1 103.0(2) . . ?
N4 C5 C6 88.8(2) . . ?
N1 C5 C6 119.1(2) . . ?
C7 C6 C5 85.0(2) . . ?
O8 C7 N4 129.5(3) . . ?
O8 C7 C6 137.6(3) . . ?
N4 C7 C6 92.8(2) . . ?
O10 S9 O11 119.30(11) . . ?
O10 S9 N1 110.25(10) . . ?
O11 S9 N1 105.34(10) . . ?
O10 S9 C12 107.73(10) . . ?
O11 S9 C12 109.06(11) . . ?
N1 S9 C12 104.14(10) . . ?
C13 C12 C17 120.7(2) . . ?
C13 C12 S9 119.8(2) . . ?
C17 C12 S9 119.4(2) . . ?
C14 C13 C12 119.1(2) . . ?
C13 C14 C15 121.4(2) . . ?
C16 C15 C14 118.2(2) . . ?
C16 C15 C18 120.9(2) . . ?
C14 C15 C18 120.9(2) . . ?
C17 C16 C15 121.5(2) . . ?
C16 C17 C12 119.2(2) . . ?
C20 C19 C28 119.5(2) . . ?
C20 C19 C2 119.3(2) . . ?
C28 C19 C2 121.1(2) . . ?
C19 C20 C21 121.2(2) . . ?
C22 C21 C26 119.7(2) . . ?
C22 C21 C20 122.0(2) . . ?
C26 C21 C20 118.3(2) . . ?
C23 C22 C21 120.5(2) . . ?
C22 C23 C24 120.7(2) . . ?
C25 C24 C23 120.5(2) . . ?
C24 C25 C26 120.5(2) . . ?
C27 C26 C21 119.4(2) . . ?
C27 C26 C25 122.6(2) . . ?
C21 C26 C25 118.0(2) . . ?
C28 C27 C26 120.6(2) . . ?
C27 C28 C19 121.0(2) . . ?
O30 C29 O31 125.3(2) . . ?
O30 C29 C3 124.5(2) . . ?
O31 C29 C3 110.2(2) . . ?
C29 O31 C32 116.6(2) . . ?
O31 C32 C33 112.5(2) . . ?
C34 C33 C38 119.1(2) . . ?
C34 C33 C32 123.9(2) . . ?
C38 C33 C32 117.0(2) . . ?
C35 C34 C33 121.1(2) . . ?
C36 C35 C34 118.2(2) . . ?
C35 C36 C37 122.3(2) . . ?
C35 C36 N39 119.3(2) . . ?
C37 C36 N39 118.4(2) . . ?
C38 C37 C36 118.6(2) . . ?
C37 C38 C33 120.8(2) . . ?
O40 N39 O41 123.3(2) . . ?
O40 N39 C36 118.2(2) . . ?
O41 N39 C36 118.5(2) . . ?

_refine_diff_density_max    0.292
_refine_diff_density_min   -0.355
_refine_diff_density_rms    0.046

#END


data_rj2

_database_code_CSD	184387


_audit_creation_method            SHELXL
_chemical_name_systematic
;
?
;
_chemical_name_common             ?
_chemical_formula_moiety          ?
_chemical_formula_structural      ?
_chemical_formula_analytical      ?
_chemical_formula_sum             'C22 H17 Cl2 N3 O7'
_chemical_formula_weight          506.29
_chemical_melting_point           ?
_chemical_compound_source         ?

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

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

_cell_length_a                    8.0069(13)
_cell_length_b                    11.908(2)
_cell_length_c                    12.814(2)
_cell_angle_alpha                 65.448(2)
_cell_angle_beta                  80.677(3)
_cell_angle_gamma                 79.668(3)
_cell_volume                      1088.1(3)
_cell_formula_units_Z             2
_cell_measurement_temperature     173(2)
_cell_measurement_reflns_used     156
_cell_measurement_theta_min       1.75
_cell_measurement_theta_max       27.5

_exptl_crystal_description        'narrow plate'
_exptl_crystal_colour             Colourless
_exptl_crystal_size_max           0.60
_exptl_crystal_size_mid           0.22
_exptl_crystal_size_min           0.12
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.545
_exptl_crystal_density_method     None
_exptl_crystal_F_000              520
_exptl_absorpt_coefficient_mu     0.350
_exptl_absorpt_correction_type    none
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?

_exptl_special_details
;
?
;

_diffrn_ambient_temperature       173(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        'Siemens SMART Area Detector'
_diffrn_measurement_method        '\w rotation with narrow frames'
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             11461
_diffrn_reflns_av_R_equivalents   0.0296
_diffrn_reflns_av_sigmaI/netI     0.0509
_diffrn_reflns_limit_h_min        -10
_diffrn_reflns_limit_h_max        10
_diffrn_reflns_limit_k_min        -15
_diffrn_reflns_limit_k_max        15
_diffrn_reflns_limit_l_min        -16
_diffrn_reflns_limit_l_max        16
_diffrn_reflns_theta_min          1.76
_diffrn_reflns_theta_max          27.55
_reflns_number_total              4958
_reflns_number_gt          3374
_reflns_threshold_expression      >2sigma(I)

_computing_data_collection        'SMART (Siemens, 1995b)'
_computing_cell_refinement        'SMART (Siemens, 1995b)'
_computing_data_reduction         'SMART (Siemens, 1995b)'
_computing_structure_solution     'SHELXTL (Siemens, 1995a)'
_computing_structure_refinement   'SHELXTL (Siemens, 1995a)'
_computing_molecular_graphics     'SHELXTL (Siemens, 1995a)'
_computing_publication_material   'SHELXTL (Siemens, 1995a)'

_refine_special_details
;
Refinement on F^2^ for ALL reflections except for 0 with very negative
F^2^
or flagged by the user for potential systematic errors.  Weighted 
R-factors
wR and all goodnesses 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 observed 
criterion
of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     noref
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          4958
_refine_ls_number_parameters      307
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0610
_refine_ls_R_factor_gt          0.0382
_refine_ls_wR_factor_all          0.1042
_refine_ls_wR_factor_ref         0.0986
_refine_ls_goodness_of_fit_all    0.948
_refine_ls_goodness_of_fit_ref    1.103
_refine_ls_restrained_S_all       0.948
_refine_ls_restrained_S_obs       1.103
_refine_ls_shift/su_max          0.000
_refine_ls_shift/esd_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
N1 N -0.0496(2) 0.31910(14) 0.32715(13) 0.0263(4) Uani 1 1 d . . .
C2 C -0.2351(2) 0.32443(18) 0.36839(16) 0.0254(4) Uani 1 1 d . . .
C3 C -0.2599(2) 0.26786(18) 0.50185(16) 0.0260(4) Uani 1 1 d . . .
H3A H -0.3355 0.3267 0.5317 0.031 Uiso 1 1 calc R . .
N4 N -0.0862(2) 0.25055(15) 0.53003(13) 0.0275(4) Uani 1 1 d . . .
C5 C 0.0413(3) 0.25213(19) 0.43179(16) 0.0291(4) Uani 1 1 d . . .
H5A H 0.0980 0.1675 0.4395 0.035 Uiso 1 1 calc R . .
C6 C 0.1490(3) 0.3232(2) 0.46812(18) 0.0334(5) Uani 1 1 d . . .
H6A H 0.2544 0.2734 0.5024 0.040 Uiso 1 1 calc R . .
H6B H 0.1719 0.4055 0.4080 0.040 Uiso 1 1 calc R . .
C7 C -0.0033(3) 0.32760(18) 0.55640(17) 0.0293(4) Uani 1 1 d . . .
O8 O -0.0473(2) 0.37780(14) 0.62246(12) 0.0387(4) Uani 1 1 d . . .
C9 C -0.1464(2) 0.43926(17) 0.31898(16) 0.0248(4) Uani 1 1 d . . .
H9A H -0.1236 0.4689 0.3771 0.030 Uiso 1 1 calc R . .
C10 C -0.1686(2) 0.53869(17) 0.20205(16) 0.0253(4) Uani 1 1 d . . .
C11 C -0.0326(2) 0.57085(18) 0.11452(17) 0.0275(4) Uani 1 1 d . . .
C12 C -0.0563(3) 0.65955(19) 0.00452(17) 0.0335(5) Uani 1 1 d . . .
H12A H 0.0366 0.6761 -0.0539 0.040 Uiso 1 1 calc R . .
C13 C -0.2178(3) 0.7240(2) -0.01940(18) 0.0357(5) Uani 1 1 d . . .
H13A H -0.2354 0.7845 -0.0948 0.043 Uiso 1 1 calc R . .
C14 C -0.3527(3) 0.70093(19) 0.06547(18) 0.0331(5) Uani 1 1 d . . .
H14A H -0.4621 0.7473 0.0499 0.040 Uiso 1 1 calc R . .
C15 C -0.3261(3) 0.60911(18) 0.17368(17) 0.0276(4) Uani 1 1 d . . .
Cl16 Cl 0.17320(6) 0.50340(5) 0.14698(4) 0.03714(15) Uani 1 1 d . . .
Cl17 Cl -0.49999(7) 0.58192(5) 0.27901(5) 0.03824(15) Uani 1 1 d . . .
C18 C -0.3549(3) 0.29762(18) 0.30679(16) 0.0273(4) Uani 1 1 d . . .
O19 O -0.48235(18) 0.24967(14) 0.35481(12) 0.0368(4) Uani 1 1 d . . .
O20 O -0.30662(17) 0.33271(13) 0.19444(11) 0.0306(3) Uani 1 1 d . . .
C21 C -0.4190(3) 0.3135(2) 0.12707(18) 0.0348(5) Uani 1 1 d . . .
H21A H -0.3712 0.3424 0.0462 0.052 Uiso 1 1 calc R . .
H21B H -0.5314 0.3603 0.1329 0.052 Uiso 1 1 calc R . .
H21C H -0.4302 0.2247 0.1565 0.052 Uiso 1 1 calc R . .
C22 C -0.3250(3) 0.14096(18) 0.55104(16) 0.0270(4) Uani 1 1 d . . .
O23 O -0.24740(18) 0.05265(13) 0.53471(12) 0.0357(4) Uani 1 1 d . . .
O24 O -0.47146(17) 0.14016(12) 0.61744(11) 0.0307(3) Uani 1 1 d . . .
C25 C -0.5376(3) 0.02072(19) 0.6695(2) 0.0386(5) Uani 1 1 d . . .
H25A H -0.4614 -0.0414 0.7260 0.046 Uiso 1 1 calc R . .
H25B H -0.5447 -0.0098 0.6095 0.046 Uiso 1 1 calc R . .
C26 C -0.7122(3) 0.03928(18) 0.72867(17) 0.0306(5) Uani 1 1 d . . .
C27 C -0.8473(3) -0.00701(19) 0.71144(17) 0.0337(5) Uani 1 1 d . . .
H27A H -0.8287 -0.0508 0.6625 0.040 Uiso 1 1 calc R . .
C28 C -1.0090(3) 0.00975(19) 0.76464(17) 0.0336(5) Uani 1 1 d . . .
H28A H -1.1014 -0.0231 0.7538 0.040 Uiso 1 1 calc R . .
C29 C -1.0324(3) 0.07539(19) 0.83371(16) 0.0300(5) Uani 1 1 d . . .
C30 C -0.9006(3) 0.1222(2) 0.85297(17) 0.0340(5) Uani 1 1 d . . .
H30A H -0.9204 0.1670 0.9011 0.041 Uiso 1 1 calc R . .
C31 C -0.7393(3) 0.1029(2) 0.80123(18) 0.0357(5) Uani 1 1 d . . .
H31A H -0.6465 0.1329 0.8150 0.043 Uiso 1 1 calc R . .
N32 N -1.2055(2) 0.09978(18) 0.88610(17) 0.0410(5) Uani 1 1 d . . .
O33 O -1.2240(2) 0.15952(17) 0.94671(15) 0.0514(4) Uani 1 1 d . . .
O33A O -1.3218(2) 0.05871(19) 0.86761(17) 0.0622(5) 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
N1 0.0229(9) 0.0265(8) 0.0294(9) -0.0114(7) -0.0010(7) -0.0038(7)
C2 0.0232(10) 0.0270(10) 0.0283(10) -0.0141(8) 0.0010(8) -0.0044(8)
C3 0.0265(11) 0.0251(10) 0.0282(10) -0.0128(8) 0.0000(8) -0.0043(8)
N4 0.0283(9) 0.0257(8) 0.0285(9) -0.0108(7) -0.0021(7) -0.0039(7)
C5 0.0282(11) 0.0265(10) 0.0296(10) -0.0090(8) -0.0029(8) -0.0014(8)
C6 0.0258(11) 0.0330(11) 0.0376(11) -0.0088(9) -0.0079(9) -0.0031(9)
C7 0.0330(12) 0.0239(10) 0.0290(10) -0.0070(9) -0.0088(9) -0.0026(8)
O8 0.0486(10) 0.0383(8) 0.0342(8) -0.0159(7) -0.0070(7) -0.0110(7)
C9 0.0231(10) 0.0272(10) 0.0268(10) -0.0133(8) -0.0009(8) -0.0052(8)
C10 0.0259(10) 0.0244(9) 0.0301(10) -0.0139(8) -0.0044(8) -0.0050(8)
C11 0.0260(11) 0.0275(10) 0.0321(10) -0.0144(9) -0.0050(8) -0.0028(8)
C12 0.0363(12) 0.0363(12) 0.0292(11) -0.0135(9) 0.0019(9) -0.0109(10)
C13 0.0453(14) 0.0350(12) 0.0277(11) -0.0091(9) -0.0089(9) -0.0107(10)
C14 0.0319(12) 0.0313(11) 0.0411(12) -0.0181(10) -0.0126(9) 0.0009(9)
C15 0.0268(11) 0.0281(10) 0.0325(10) -0.0165(9) -0.0009(8) -0.0057(8)
Cl16 0.0246(3) 0.0430(3) 0.0381(3) -0.0120(2) 0.0009(2) -0.0044(2)
Cl17 0.0265(3) 0.0417(3) 0.0454(3) -0.0197(3) 0.0035(2) -0.0018(2)
C18 0.0284(11) 0.0267(10) 0.0294(10) -0.0152(8) 0.0017(8) -0.0035(8)
O19 0.0340(9) 0.0467(9) 0.0354(8) -0.0190(7) 0.0033(7) -0.0183(7)
O20 0.0318(8) 0.0378(8) 0.0267(7) -0.0149(6) -0.0004(6) -0.0118(6)
C21 0.0353(12) 0.0414(12) 0.0316(11) -0.0145(9) -0.0079(9) -0.0100(10)
C22 0.0310(11) 0.0276(10) 0.0242(10) -0.0115(8) -0.0018(8) -0.0061(8)
O23 0.0372(9) 0.0299(8) 0.0435(9) -0.0202(7) 0.0052(7) -0.0073(7)
O24 0.0326(8) 0.0271(7) 0.0331(8) -0.0142(6) 0.0079(6) -0.0101(6)
C25 0.0425(13) 0.0254(11) 0.0472(13) -0.0160(10) 0.0114(11) -0.0127(10)
C26 0.0344(12) 0.0232(10) 0.0311(11) -0.0094(9) 0.0045(9) -0.0066(9)
C27 0.0422(13) 0.0297(11) 0.0308(11) -0.0134(9) -0.0019(9) -0.0070(9)
C28 0.0327(12) 0.0329(11) 0.0342(11) -0.0095(9) -0.0076(9) -0.0071(9)
C29 0.0273(11) 0.0300(11) 0.0261(10) -0.0060(8) -0.0022(8) -0.0007(9)
C30 0.0362(12) 0.0367(12) 0.0331(11) -0.0185(10) -0.0007(9) -0.0050(10)
C31 0.0334(12) 0.0371(12) 0.0434(12) -0.0220(10) -0.0004(10)  -0.0086(10)
N32 0.0294(11) 0.0410(11) 0.0428(11) -0.0098(9) -0.0040(9) 0.0026(9)
O33 0.0421(10) 0.0609(11) 0.0527(10) -0.0310(9) 0.0032(8) 0.0042(8)
O33A 0.0283(9) 0.0774(13) 0.0893(14) -0.0422(12) -0.0054(9)
-0.0047(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
N1 C9 1.471(2) . ?
N1 C5 1.478(2) . ?
N1 C2 1.493(2) . ?
C2 C18 1.487(3) . ?
C2 C9 1.503(3) . ?
C2 C3 1.549(3) . ?
C3 N4 1.451(3) . ?
C3 C22 1.529(3) . ?
N4 C7 1.395(3) . ?
N4 C5 1.483(2) . ?
C5 C6 1.547(3) . ?
C6 C7 1.533(3) . ?
C7 O8 1.203(2) . ?
C9 C10 1.488(3) . ?
C10 C15 1.394(3) . ?
C10 C11 1.409(3) . ?
C11 C12 1.384(3) . ?
C11 Cl16 1.733(2) . ?
C12 C13 1.390(3) . ?
C13 C14 1.379(3) . ?
C14 C15 1.384(3) . ?
C15 Cl17 1.748(2) . ?
C18 O19 1.208(2) . ?
C18 O20 1.332(2) . ?
O20 C21 1.448(2) . ?
C22 O23 1.201(2) . ?
C22 O24 1.331(2) . ?
O24 C25 1.455(2) . ?
C25 C26 1.505(3) . ?
C26 C27 1.383(3) . ?
C26 C31 1.395(3) . ?
C27 C28 1.384(3) . ?
C28 C29 1.378(3) . ?
C29 C30 1.376(3) . ?
C29 N32 1.474(3) . ?
C30 C31 1.380(3) . ?
N32 O33A 1.222(3) . ?
N32 O33 1.231(2) . ?

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
C9 N1 C5 114.38(15) . . ?
C9 N1 C2 60.92(12) . . ?
C5 N1 C2 105.85(14) . . ?
C18 C2 N1 119.07(16) . . ?
C18 C2 C9 124.04(17) . . ?
N1 C2 C9 58.81(11) . . ?
C18 C2 C3 117.51(16) . . ?
N1 C2 C3 110.30(15) . . ?
C9 C2 C3 113.11(16) . . ?
N4 C3 C22 108.75(16) . . ?
N4 C3 C2 101.43(14) . . ?
C22 C3 C2 112.38(15) . . ?
C7 N4 C3 129.37(16) . . ?
C7 N4 C5 93.26(15) . . ?
C3 N4 C5 112.26(15) . . ?
N1 C5 N4 105.97(15) . . ?
N1 C5 C6 119.44(16) . . ?
N4 C5 C6 88.25(15) . . ?
C7 C6 C5 85.57(15) . . ?
O8 C7 N4 130.6(2) . . ?
O8 C7 C6 137.2(2) . . ?
N4 C7 C6 92.12(16) . . ?
N1 C9 C10 117.99(15) . . ?
N1 C9 C2 60.27(12) . . ?
C10 C9 C2 123.44(17) . . ?
C15 C10 C11 115.66(17) . . ?
C15 C10 C9 121.45(17) . . ?
C11 C10 C9 122.86(17) . . ?
C12 C11 C10 122.27(19) . . ?
C12 C11 Cl16 118.48(15) . . ?
C10 C11 Cl16 119.16(15) . . ?
C11 C12 C13 119.17(19) . . ?
C14 C13 C12 120.57(19) . . ?
C13 C14 C15 118.9(2) . . ?
C14 C15 C10 123.26(19) . . ?
C14 C15 Cl17 117.67(16) . . ?
C10 C15 Cl17 119.07(15) . . ?
O19 C18 O20 124.43(19) . . ?
O19 C18 C2 122.79(18) . . ?
O20 C18 C2 112.78(16) . . ?
C18 O20 C21 116.45(15) . . ?
O23 C22 O24 125.22(18) . . ?
O23 C22 C3 123.01(18) . . ?
O24 C22 C3 111.69(16) . . ?
C22 O24 C25 114.29(15) . . ?
O24 C25 C26 107.67(16) . . ?
C27 C26 C31 119.53(19) . . ?
C27 C26 C25 120.00(19) . . ?
C31 C26 C25 120.5(2) . . ?
C26 C27 C28 120.83(19) . . ?
C29 C28 C27 118.2(2) . . ?
C30 C29 C28 122.35(19) . . ?
C30 C29 N32 118.70(19) . . ?
C28 C29 N32 118.92(19) . . ?
C29 C30 C31 118.91(19) . . ?
C30 C31 C26 120.1(2) . . ?
O33A N32 O33 123.9(2) . . ?
O33A N32 C29 118.1(2) . . ?
O33 N32 C29 117.9(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
C9 N1 C2 C18 114.3(2) . . . . ?
C5 N1 C2 C18 -136.20(18) . . . . ?
C5 N1 C2 C9 109.46(16) . . . . ?
C9 N1 C2 C3 -105.39(17) . . . . ?
C5 N1 C2 C3 4.07(19) . . . . ?
C18 C2 C3 N4 149.42(17) . . . . ?
N1 C2 C3 N4 8.46(19) . . . . ?
C9 C2 C3 N4 -55.27(19) . . . . ?
C18 C2 C3 C22 33.5(2) . . . . ?
N1 C2 C3 C22 -107.50(18) . . . . ?
C9 C2 C3 C22 -171.24(16) . . . . ?
C22 C3 N4 C7 -145.29(18) . . . . ?
C2 C3 N4 C7 96.1(2) . . . . ?
C22 C3 N4 C5 100.17(17) . . . . ?
C2 C3 N4 C5 -18.44(19) . . . . ?
C9 N1 C5 N4 49.92(19) . . . . ?
C2 N1 C5 N4 -14.87(18) . . . . ?
C9 N1 C5 C6 -47.3(2) . . . . ?
C2 N1 C5 C6 -112.04(18) . . . . ?
C7 N4 C5 N1 -113.23(16) . . . . ?
C3 N4 C5 N1 22.0(2) . . . . ?
C7 N4 C5 C6 6.94(15) . . . . ?
C3 N4 C5 C6 142.17(15) . . . . ?
N1 C5 C6 C7 101.06(18) . . . . ?
N4 C5 C6 C7 -6.32(13) . . . . ?
C3 N4 C7 O8 48.4(3) . . . . ?
C5 N4 C7 O8 171.0(2) . . . . ?
C3 N4 C7 C6 -129.53(19) . . . . ?
C5 N4 C7 C6 -7.01(15) . . . . ?
C5 C6 C7 O8 -171.0(3) . . . . ?
C5 C6 C7 N4 6.73(14) . . . . ?
C5 N1 C9 C10 150.24(17) . . . . ?
C2 N1 C9 C10 -114.53(19) . . . . ?
C5 N1 C9 C2 -95.23(16) . . . . ?
C18 C2 C9 N1 -106.1(2) . . . . ?
C3 C2 C9 N1 100.52(17) . . . . ?
C18 C2 C9 C10 -0.4(3) . . . . ?
N1 C2 C9 C10 105.69(19) . . . . ?
C3 C2 C9 C10 -153.79(17) . . . . ?
N1 C9 C10 C15 134.81(19) . . . . ?
C2 C9 C10 C15 63.6(3) . . . . ?
N1 C9 C10 C11 -47.4(3) . . . . ?
C2 C9 C10 C11 -118.6(2) . . . . ?
C15 C10 C11 C12 -5.1(3) . . . . ?
C9 C10 C11 C12 176.96(18) . . . . ?
C15 C10 C11 Cl16 171.45(15) . . . . ?
C9 C10 C11 Cl16 -6.5(3) . . . . ?
C10 C11 C12 C13 3.4(3) . . . . ?
Cl16 C11 C12 C13 -173.19(16) . . . . ?
C11 C12 C13 C14 0.6(3) . . . . ?
C12 C13 C14 C15 -2.4(3) . . . . ?
C13 C14 C15 C10 0.5(3) . . . . ?
C13 C14 C15 Cl17 -179.78(15) . . . . ?
C11 C10 C15 C14 3.2(3) . . . . ?
C9 C10 C15 C14 -178.88(18) . . . . ?
C11 C10 C15 Cl17 -176.57(14) . . . . ?
C9 C10 C15 Cl17 1.4(3) . . . . ?
N1 C2 C18 O19 148.16(19) . . . . ?
C9 C2 C18 O19 -141.7(2) . . . . ?
C3 C2 C18 O19 10.7(3) . . . . ?
N1 C2 C18 O20 -32.2(2) . . . . ?
C9 C2 C18 O20 37.9(3) . . . . ?
C3 C2 C18 O20 -169.68(16) . . . . ?
O19 C18 O20 C21 1.4(3) . . . . ?
C2 C18 O20 C21 -178.18(17) . . . . ?
N4 C3 C22 O23 -50.8(2) . . . . ?
C2 C3 C22 O23 60.7(3) . . . . ?
N4 C3 C22 O24 126.13(17) . . . . ?
C2 C3 C22 O24 -122.40(17) . . . . ?
O23 C22 O24 C25 -1.5(3) . . . . ?
C3 C22 O24 C25 -178.38(17) . . . . ?
C22 O24 C25 C26 -172.95(17) . . . . ?
O24 C25 C26 C27 132.1(2) . . . . ?
O24 C25 C26 C31 -48.0(3) . . . . ?
C31 C26 C27 C28 0.5(3) . . . . ?
C25 C26 C27 C28 -179.64(19) . . . . ?
C26 C27 C28 C29 1.0(3) . . . . ?
C27 C28 C29 C30 -1.3(3) . . . . ?
C27 C28 C29 N32 176.81(18) . . . . ?
C28 C29 C30 C31 0.1(3) . . . . ?
N32 C29 C30 C31 -178.02(18) . . . . ?
C29 C30 C31 C26 1.4(3) . . . . ?
C27 C26 C31 C30 -1.7(3) . . . . ?
C25 C26 C31 C30 178.4(2) . . . . ?
C30 C29 N32 O33A 179.4(2) . . . . ?
C28 C29 N32 O33A 1.2(3) . . . . ?
C30 C29 N32 O33 -1.2(3) . . . . ?
C28 C29 N32 O33 -179.37(19) . . . . ?

_diffrn_measured_fraction_theta_max    0.986
_diffrn_reflns_theta_full              27.55
_diffrn_measured_fraction_theta_full   0.986
_refine_diff_density_max    0.357
_refine_diff_density_min   -0.284
_refine_diff_density_rms    0.050