# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 992389'
_audit_update_record             
;
2014-03-18 deposited with the CCDC.
2015-02-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H42 Cl6 N6 O8'
_chemical_formula_weight         995.54

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                   10.7259(9)
_cell_length_b                   14.2208(12)
_cell_length_c                   14.8907(12)
_cell_angle_alpha                92.5080(10)
_cell_angle_beta                 93.7200(10)
_cell_angle_gamma                98.8250(10)
_cell_volume                     2236.3(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4171
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      20.81

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      1.478
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1028
_exptl_absorpt_coefficient_mu    0.445
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13370
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.93
_diffrn_reflns_theta_max         20.81
_reflns_number_total             4582
_reflns_number_gt                3740
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.1197P)²+5.6112P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4582
_refine_ls_number_parameters     643
_refine_ls_number_restraints     90
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0637
_refine_ls_wR_factor_ref         0.1951
_refine_ls_wR_factor_gt          0.1797
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.080
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3942(6) 0.9364(4) 0.2563(4) 0.0341(16) Uani 1 1 d . . .
H1 H 0.3312 0.8815 0.2564 0.041 Uiso 1 1 calc R . .
C2 C 0.4844(5) 0.9528(4) 0.3270(4) 0.0287(14) Uani 1 1 d . . .
H2 H 0.4830 0.9096 0.3740 0.034 Uiso 1 1 calc R . .
C3 C 0.5789(5) 1.0333(4) 0.3302(4) 0.0206(13) Uani 1 1 d . . .
C4 C 0.5740(5) 1.0922(4) 0.2587(4) 0.0245(14) Uani 1 1 d . . .
H4 H 0.6352 1.1478 0.2570 0.029 Uiso 1 1 calc R . .
C5 C 0.4797(6) 1.0696(5) 0.1898(4) 0.0319(15) Uani 1 1 d . . .
H5 H 0.4790 1.1110 0.1414 0.038 Uiso 1 1 calc R . .
C6 C 0.6771(5) 1.0561(4) 0.4038(4) 0.0204(13) Uani 1 1 d . . .
H6 H 0.7204 1.1197 0.4103 0.024 Uiso 1 1 calc R . .
C7 C 0.7110(5) 0.9953(4) 0.4626(3) 0.0188(13) Uani 1 1 d . . .
H7 H 0.6650 0.9324 0.4574 0.023 Uiso 1 1 calc R . .
C8 C 0.8123(5) 1.0160(4) 0.5342(4) 0.0192(13) Uani 1 1 d . . .
C9 C 0.8181(5) 0.9594(3) 0.6092(3) 0.0163(13) Uani 1 1 d . . .
C10 C 0.9234(5) 0.9780(3) 0.6738(3) 0.0162(12) Uani 1 1 d . . .
C11 C 1.0217(5) 1.0538(3) 0.6649(3) 0.0171(13) Uani 1 1 d . . .
C12 C 1.0118(5) 1.1103(4) 0.5911(4) 0.0218(13) Uani 1 1 d . . .
H12 H 1.0760 1.1631 0.5850 0.026 Uiso 1 1 calc R . .
C13 C 0.9116(5) 1.0915(4) 0.5270(4) 0.0206(13) Uani 1 1 d . . .
H13 H 0.9096 1.1304 0.4768 0.025 Uiso 1 1 calc R . .
C14 C 1.1320(5) 1.0750(4) 0.7293(4) 0.0221(13) Uani 1 1 d . . .
H14 H 1.1457 1.0272 0.7698 0.026 Uiso 1 1 calc R . .
C15 C 1.2148(5) 1.1546(4) 0.7363(4) 0.0289(15) Uani 1 1 d . . .
H15 H 1.2006 1.2023 0.6958 0.035 Uiso 1 1 calc R . .
C16 C 1.3266(5) 1.1763(4) 0.8006(4) 0.0278(14) Uani 1 1 d . . .
C17 C 1.3550(5) 1.1197(4) 0.8693(4) 0.0263(14) Uani 1 1 d . . .
H17 H 1.3011 1.0615 0.8770 0.032 Uiso 1 1 calc R . .
C18 C 1.4620(6) 1.1475(4) 0.9271(4) 0.0314(15) Uani 1 1 d . . .
H18 H 1.4795 1.1059 0.9729 0.038 Uiso 1 1 calc R . .
C19 C 1.5144(9) 1.2794(6) 0.8555(6) 0.088(3) Uani 1 1 d . . .
H19 H 1.5713 1.3363 0.8487 0.105 Uiso 1 1 calc R . .
C20 C 1.4121(8) 1.2589(5) 0.7942(6) 0.070(3) Uani 1 1 d . . .
H20 H 1.3997 1.3008 0.7476 0.084 Uiso 1 1 calc R . .
C21 C 0.7080(5) 0.8828(3) 0.6243(3) 0.0164(12) Uani 1 1 d . . .
H21A H 0.6762 0.8972 0.6834 0.020 Uiso 1 1 calc R . .
H21B H 0.6391 0.8863 0.5776 0.020 Uiso 1 1 calc R . .
C22 C 0.9242(5) 0.9149(3) 0.7532(3) 0.0195(13) Uani 1 1 d . . .
H22A H 1.0015 0.9369 0.7932 0.023 Uiso 1 1 calc R . .
H22B H 0.8503 0.9217 0.7880 0.023 Uiso 1 1 calc R . .
C23 C 0.7519(5) 0.7371(3) 0.5434(4) 0.0142(9) Uani 1 1 d . . .
C24 C 1.0250(5) 0.7728(3) 0.7115(3) 0.0142(9) Uani 1 1 d . . .
C25 C 0.8036(5) 0.7538(4) 0.6989(3) 0.0178(13) Uani 1 1 d . . .
C26 C 0.7172(6) 0.7349(3) 0.7772(4) 0.0191(13) Uani 1 1 d . . .
C27 C 0.7171(6) 0.6962(5) 0.9299(4) 0.0355(16) Uani 1 1 d . . .
H27A H 0.6688 0.6310 0.9200 0.043 Uiso 1 1 calc R . .
H27B H 0.6568 0.7409 0.9409 0.043 Uiso 1 1 calc R . .
C28 C 0.8105(7) 0.7005(5) 1.0082(4) 0.0489(18) Uani 1 1 d . . .
H28A H 0.8732 0.6594 0.9950 0.073 Uiso 1 1 calc R . .
H28B H 0.7670 0.6786 1.0612 0.073 Uiso 1 1 calc R . .
H28C H 0.8531 0.7663 1.0204 0.073 Uiso 1 1 calc R . .
C29 C 0.8509(5) 0.6615(3) 0.6590(3) 0.0169(12) Uani 1 1 d . . .
C30 C 0.7843(5) 0.5701(4) 0.6979(4) 0.0182(13) Uani 1 1 d . . .
C31 C 0.5784(5) 0.4800(4) 0.7039(5) 0.0389(17) Uani 1 1 d . . .
H31A H 0.5819 0.4911 0.7702 0.047 Uiso 1 1 calc R . .
H31B H 0.6006 0.4162 0.6899 0.047 Uiso 1 1 calc R . .
C32 C 0.4486(7) 0.4869(6) 0.6625(7) 0.085(3) Uani 1 1 d . . .
H32A H 0.4269 0.5496 0.6789 0.127 Uiso 1 1 calc R . .
H32B H 0.3867 0.4371 0.6849 0.127 Uiso 1 1 calc R . .
H32C H 0.4478 0.4786 0.5968 0.127 Uiso 1 1 calc R . .
C33 C 0.8550(5) 0.5979(3) 0.4979(3) 0.0173(12) Uani 1 1 d . . .
H33A H 0.7975 0.5932 0.4426 0.021 Uiso 1 1 calc R . .
H33B H 0.8482 0.5339 0.5224 0.021 Uiso 1 1 calc R . .
C34 C 1.0685(5) 0.6227(4) 0.6388(3) 0.0180(12) Uani 1 1 d . . .
H34A H 1.0334 0.5543 0.6412 0.022 Uiso 1 1 calc R . .
H34B H 1.1515 0.6337 0.6740 0.022 Uiso 1 1 calc R . .
C35 C 0.9899(5) 0.6294(3) 0.4740(3) 0.0148(12) Uani 1 1 d . . .
C36 C 1.0904(5) 0.6434(3) 0.5410(3) 0.0162(12) Uani 1 1 d . . .
C37 C 1.2132(5) 0.6747(3) 0.5164(4) 0.0187(13) Uani 1 1 d . . .
C38 C 1.2351(5) 0.6903(4) 0.4273(4) 0.0254(14) Uani 1 1 d . . .
H38 H 1.3186 0.7117 0.4113 0.030 Uiso 1 1 calc R . .
C39 C 1.1360(5) 0.6751(4) 0.3615(4) 0.0230(14) Uani 1 1 d . . .
H39 H 1.1517 0.6860 0.3004 0.028 Uiso 1 1 calc R . .
C40 C 1.0140(5) 0.6440(3) 0.3843(4) 0.0205(13) Uani 1 1 d . . .
C41 C 1.4340(5) 0.7134(4) 0.5615(4) 0.0342(15) Uani 1 1 d . . .
H41A H 1.4561 0.6654 0.5187 0.051 Uiso 1 1 calc R . .
H41B H 1.4916 0.7187 0.6160 0.051 Uiso 1 1 calc R . .
H41C H 1.4414 0.7751 0.5339 0.051 Uiso 1 1 calc R . .
C42 C 0.9331(6) 0.6336(4) 0.2294(4) 0.0379(16) Uani 1 1 d . . .
H42A H 0.9636 0.7003 0.2184 0.057 Uiso 1 1 calc R . .
H42B H 0.8541 0.6117 0.1925 0.057 Uiso 1 1 calc R . .
H42C H 0.9967 0.5943 0.2136 0.057 Uiso 1 1 calc R . .
C43 C 0.7986(17) 0.0709(9) 0.9622(11) 0.059(6) Uani 0.574(6) 1 d PDU A 1
H43 H 0.7096 0.0671 0.9361 0.071 Uiso 0.574(6) 1 calc PR A 1
Cl1 Cl 0.8335(4) -0.0405(2) 0.9697(2) 0.0660(15) Uani 0.574(6) 1 d PDU A 1
Cl2 Cl 0.816(5) 0.1355(13) 1.0651(15) 0.076(3) Uani 0.574(6) 1 d PD A 1
Cl3 Cl 0.9072(5) 0.1366(4) 0.8870(3) 0.0658(14) Uani 0.574(6) 1 d PD A 1
C43' C 0.834(2) 0.0862(17) 0.9671(16) 0.068(11) Uani 0.426(6) 1 d PDU A 2
H43' H 0.7602 0.0408 0.9381 0.082 Uiso 0.426(6) 1 calc PR A 2
Cl1' Cl 0.9674(7) 0.0323(5) 0.9821(4) 0.099(3) Uani 0.426(6) 1 d PD . 2
Cl2' Cl 0.800(6) 0.1321(18) 1.072(2) 0.076(3) Uani 0.426(6) 1 d PD A 2
Cl3' Cl 0.8755(8) 0.1912(7) 0.8980(5) 0.090(2) Uani 0.426(6) 1 d PD A 2
C44 C 0.7566(7) 0.3844(6) 0.0379(4) 0.040(2) Uani 0.858(5) 1 d PDU B 1
H44 H 0.7163 0.3169 0.0229 0.048 Uiso 0.858(5) 1 calc PR B 1
Cl4 Cl 0.81410(18) 0.43461(13) -0.06000(13) 0.0426(7) Uani 0.858(5) 1 d PDU B 1
Cl5 Cl 0.6416(3) 0.4496(3) 0.0782(2) 0.0686(10) Uani 0.858(5) 1 d PDU B 1
Cl6 Cl 0.8820(2) 0.38607(13) 0.11969(13) 0.0514(8) Uani 0.858(5) 1 d PDU B 1
C44' C 0.708(3) 0.373(2) 0.0437(19) 0.023(14) Uani 0.142(5) 1 d PDU B 2
H44' H 0.6729 0.3141 0.0048 0.027 Uiso 0.142(5) 1 calc PR B 2
Cl4' Cl 0.855(2) 0.428(2) 0.009(2) 0.146(10) Uani 0.142(5) 1 d PDU B 2
Cl5' Cl 0.606(2) 0.4608(16) 0.0386(16) 0.081(8) Uani 0.142(5) 1 d PDU B 2
Cl6' Cl 0.736(3) 0.3461(18) 0.1563(15) 0.142(10) Uani 0.142(5) 1 d PDU B 2
N1 N 0.3894(5) 0.9930(4) 0.1870(3) 0.0361(13) Uani 1 1 d . . .
N2 N 1.5411(5) 1.2271(4) 0.9233(4) 0.0495(15) Uani 1 1 d . . .
N3 N 0.7348(4) 0.7853(3) 0.6223(3) 0.0152(10) Uani 1 1 d . . .
N4 N 0.9203(4) 0.8141(3) 0.7266(3) 0.0152(10) Uani 1 1 d . . .
N5 N 0.8153(4) 0.6636(3) 0.5639(3) 0.0147(10) Uani 1 1 d . . .
N6 N 0.9842(4) 0.6787(3) 0.6826(3) 0.0133(10) Uani 1 1 d . . .
O1 O 0.7126(3) 0.7548(2) 0.4684(2) 0.0193(9) Uani 1 1 d . . .
O2 O 1.1336(3) 0.8118(2) 0.7228(2) 0.0204(9) Uani 1 1 d . . .
O3 O 0.6065(4) 0.7310(3) 0.7710(3) 0.0399(11) Uani 1 1 d . . .
O4 O 0.7867(4) 0.7224(3) 0.8507(2) 0.0290(10) Uani 1 1 d . . .
O5 O 0.8317(4) 0.5239(3) 0.7505(3) 0.0292(10) Uani 1 1 d . . .
O6 O 0.6645(3) 0.5530(3) 0.6649(3) 0.0342(11) Uani 1 1 d . . .
O7 O 0.9106(3) 0.6254(2) 0.3229(2) 0.0245(9) Uani 1 1 d . . .
O8 O 1.3070(3) 0.6858(2) 0.5849(2) 0.0260(9) Uani 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
C1 N1 1.339(8) . ?
C1 C2 1.370(8) . ?
C1 H1 0.9500 . ?
C2 C3 1.405(8) . ?
C2 H2 0.9500 . ?
C3 C4 1.386(8) . ?
C3 C6 1.459(8) . ?
C4 C5 1.384(8) . ?
C4 H4 0.9500 . ?
C5 N1 1.339(8) . ?
C5 H5 0.9500 . ?
C6 C7 1.329(7) . ?
C6 H6 0.9500 . ?
C7 C8 1.460(8) . ?
C7 H7 0.9500 . ?
C8 C13 1.404(7) . ?
C8 C9 1.409(7) . ?
C9 C10 1.420(7) . ?
C9 C21 1.514(7) . ?
C10 C11 1.404(7) . ?
C10 C22 1.516(7) . ?
C11 C12 1.398(7) . ?
C11 C14 1.459(8) . ?
C12 C13 1.376(8) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C15 1.323(7) . ?
C14 H14 0.9500 . ?
C15 C16 1.471(8) . ?
C15 H15 0.9500 . ?
C16 C17 1.376(8) . ?
C16 C20 1.385(9) . ?
C17 C18 1.386(8) . ?
C17 H17 0.9500 . ?
C18 N2 1.311(8) . ?
C18 H18 0.9500 . ?
C19 N2 1.323(9) . ?
C19 C20 1.367(11) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 N3 1.457(6) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 N4 1.463(6) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 O1 1.217(6) . ?
C23 N5 1.366(7) . ?
C23 N3 1.372(7) . ?
C24 O2 1.208(6) . ?
C24 N4 1.372(6) . ?
C24 N6 1.384(6) . ?
C25 N4 1.430(7) . ?
C25 N3 1.443(6) . ?
C25 C26 1.543(8) . ?
C25 C29 1.584(7) . ?
C26 O3 1.178(6) . ?
C26 O4 1.317(6) . ?
C27 O4 1.468(7) . ?
C27 C28 1.480(9) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 N6 1.430(6) . ?
C29 N5 1.445(6) . ?
C29 C30 1.540(7) . ?
C30 O5 1.183(6) . ?
C30 O6 1.329(7) . ?
C31 O6 1.448(7) . ?
C31 C32 1.504(10) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 N5 1.454(6) . ?
C33 C35 1.517(7) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 N6 1.461(6) . ?
C34 C36 1.523(7) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C40 1.395(7) . ?
C35 C36 1.406(7) . ?
C36 C37 1.401(7) . ?
C37 O8 1.371(6) . ?
C37 C38 1.384(8) . ?
C38 C39 1.384(8) . ?
C38 H38 0.9500 . ?
C39 C40 1.385(8) . ?
C39 H39 0.9500 . ?
C40 O7 1.375(6) . ?
C41 O8 1.428(7) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 O7 1.435(7) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 Cl1 1.688(11) . ?
C43 Cl2 1.735(14) . ?
C43 Cl3 1.847(13) . ?
C43 H43 1.0000 . ?
C43' Cl1' 1.734(17) . ?
C43' Cl2' 1.742(17) . ?
C43' Cl3' 1.865(17) . ?
C43' H43' 1.0000 . ?
Cl1' Cl1' 1.344(12) 2_757 ?
C44 Cl6 1.751(6) . ?
C44 Cl4 1.757(7) . ?
C44 Cl5 1.771(7) . ?
C44 H44 1.0000 . ?
C44' Cl6' 1.75(2) . ?
C44' Cl4' 1.76(2) . ?
C44' Cl5' 1.79(2) . ?
C44' H44' 1.0000 . ?

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
N1 C1 C2 123.9(6) . . ?
N1 C1 H1 118.0 . . ?
C2 C1 H1 118.0 . . ?
C1 C2 C3 120.1(6) . . ?
C1 C2 H2 119.9 . . ?
C3 C2 H2 119.9 . . ?
C4 C3 C2 116.1(5) . . ?
C4 C3 C6 120.7(5) . . ?
C2 C3 C6 123.3(5) . . ?
C5 C4 C3 119.8(5) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
N1 C5 C4 124.0(6) . . ?
N1 C5 H5 118.0 . . ?
C4 C5 H5 118.0 . . ?
C7 C6 C3 125.5(5) . . ?
C7 C6 H6 117.2 . . ?
C3 C6 H6 117.2 . . ?
C6 C7 C8 126.1(5) . . ?
C6 C7 H7 116.9 . . ?
C8 C7 H7 116.9 . . ?
C13 C8 C9 118.0(5) . . ?
C13 C8 C7 119.8(5) . . ?
C9 C8 C7 122.1(5) . . ?
C8 C9 C10 120.1(5) . . ?
C8 C9 C21 120.0(4) . . ?
C10 C9 C21 119.8(4) . . ?
C11 C10 C9 120.8(4) . . ?
C11 C10 C22 121.5(5) . . ?
C9 C10 C22 117.7(4) . . ?
C12 C11 C10 117.9(5) . . ?
C12 C11 C14 119.5(5) . . ?
C10 C11 C14 122.6(5) . . ?
C13 C12 C11 121.8(5) . . ?
C13 C12 H12 119.1 . . ?
C11 C12 H12 119.1 . . ?
C12 C13 C8 121.4(5) . . ?
C12 C13 H13 119.3 . . ?
C8 C13 H13 119.3 . . ?
C15 C14 C11 125.9(5) . . ?
C15 C14 H14 117.0 . . ?
C11 C14 H14 117.0 . . ?
C14 C15 C16 126.3(5) . . ?
C14 C15 H15 116.8 . . ?
C16 C15 H15 116.8 . . ?
C17 C16 C20 115.5(5) . . ?
C17 C16 C15 124.7(5) . . ?
C20 C16 C15 119.9(6) . . ?
C16 C17 C18 120.1(5) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
N2 C18 C17 124.8(6) . . ?
N2 C18 H18 117.6 . . ?
C17 C18 H18 117.6 . . ?
N2 C19 C20 125.8(7) . . ?
N2 C19 H19 117.1 . . ?
C20 C19 H19 117.1 . . ?
C19 C20 C16 119.4(7) . . ?
C19 C20 H20 120.3 . . ?
C16 C20 H20 120.3 . . ?
N3 C21 C9 115.9(4) . . ?
N3 C21 H21A 108.3 . . ?
C9 C21 H21A 108.3 . . ?
N3 C21 H21B 108.3 . . ?
C9 C21 H21B 108.3 . . ?
H21A C21 H21B 107.4 . . ?
N4 C22 C10 113.3(4) . . ?
N4 C22 H22A 108.9 . . ?
C10 C22 H22A 108.9 . . ?
N4 C22 H22B 108.9 . . ?
C10 C22 H22B 108.9 . . ?
H22A C22 H22B 107.7 . . ?
O1 C23 N5 126.2(5) . . ?
O1 C23 N3 125.6(4) . . ?
N5 C23 N3 108.2(4) . . ?
O2 C24 N4 125.8(4) . . ?
O2 C24 N6 126.3(5) . . ?
N4 C24 N6 107.9(4) . . ?
N4 C25 N3 114.4(4) . . ?
N4 C25 C26 112.5(4) . . ?
N3 C25 C26 110.6(4) . . ?
N4 C25 C29 101.9(4) . . ?
N3 C25 C29 103.0(4) . . ?
C26 C25 C29 113.9(4) . . ?
O3 C26 O4 125.9(5) . . ?
O3 C26 C25 124.8(5) . . ?
O4 C26 C25 109.3(5) . . ?
O4 C27 C28 107.9(5) . . ?
O4 C27 H27A 110.1 . . ?
C28 C27 H27A 110.1 . . ?
O4 C27 H27B 110.1 . . ?
C28 C27 H27B 110.1 . . ?
H27A C27 H27B 108.4 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N6 C29 N5 115.1(4) . . ?
N6 C29 C30 112.6(4) . . ?
N5 C29 C30 110.8(4) . . ?
N6 C29 C25 103.7(4) . . ?
N5 C29 C25 102.1(4) . . ?
C30 C29 C25 111.9(4) . . ?
O5 C30 O6 125.5(5) . . ?
O5 C30 C29 125.3(5) . . ?
O6 C30 C29 109.1(5) . . ?
O6 C31 C32 106.1(5) . . ?
O6 C31 H31A 110.5 . . ?
C32 C31 H31A 110.5 . . ?
O6 C31 H31B 110.5 . . ?
C32 C31 H31B 110.5 . . ?
H31A C31 H31B 108.7 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N5 C33 C35 112.2(4) . . ?
N5 C33 H33A 109.2 . . ?
C35 C33 H33A 109.2 . . ?
N5 C33 H33B 109.2 . . ?
C35 C33 H33B 109.2 . . ?
H33A C33 H33B 107.9 . . ?
N6 C34 C36 115.8(4) . . ?
N6 C34 H34A 108.3 . . ?
C36 C34 H34A 108.3 . . ?
N6 C34 H34B 108.3 . . ?
C36 C34 H34B 108.3 . . ?
H34A C34 H34B 107.4 . . ?
C40 C35 C36 119.8(5) . . ?
C40 C35 C33 119.4(5) . . ?
C36 C35 C33 120.8(4) . . ?
C37 C36 C35 118.9(5) . . ?
C37 C36 C34 119.8(4) . . ?
C35 C36 C34 121.2(5) . . ?
O8 C37 C38 123.6(5) . . ?
O8 C37 C36 115.9(5) . . ?
C38 C37 C36 120.5(5) . . ?
C37 C38 C39 120.3(5) . . ?
C37 C38 H38 119.8 . . ?
C39 C38 H38 119.8 . . ?
C38 C39 C40 120.2(5) . . ?
C38 C39 H39 119.9 . . ?
C40 C39 H39 119.9 . . ?
O7 C40 C39 123.9(5) . . ?
O7 C40 C35 115.9(5) . . ?
C39 C40 C35 120.3(5) . . ?
O8 C41 H41A 109.5 . . ?
O8 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
O8 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O7 C42 H42A 109.5 . . ?
O7 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
O7 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
Cl1 C43 Cl2 113.3(10) . . ?
Cl1 C43 Cl3 108.8(7) . . ?
Cl2 C43 Cl3 107.2(11) . . ?
Cl1 C43 H43 109.1 . . ?
Cl2 C43 H43 109.1 . . ?
Cl3 C43 H43 109.1 . . ?
Cl1' C43' Cl2' 108.2(19) . . ?
Cl1' C43' Cl3' 107.4(12) . . ?
Cl2' C43' Cl3' 106.0(14) . . ?
Cl1' C43' H43' 111.7 . . ?
Cl2' C43' H43' 111.7 . . ?
Cl3' C43' H43' 111.7 . . ?
Cl1' Cl1' C43' 153.0(11) 2_757 . ?
Cl6 C44 Cl4 109.7(4) . . ?
Cl6 C44 Cl5 110.8(4) . . ?
Cl4 C44 Cl5 109.2(4) . . ?
Cl6 C44 H44 109.0 . . ?
Cl4 C44 H44 109.0 . . ?
Cl5 C44 H44 109.0 . . ?
Cl6' C44' Cl4' 106(2) . . ?
Cl6' C44' Cl5' 109.1(18) . . ?
Cl4' C44' Cl5' 105.7(18) . . ?
Cl6' C44' H44' 111.9 . . ?
Cl4' C44' H44' 111.9 . . ?
Cl5' C44' H44' 111.9 . . ?
C1 N1 C5 116.1(5) . . ?
C18 N2 C19 114.4(6) . . ?
C23 N3 C25 112.4(4) . . ?
C23 N3 C21 121.9(4) . . ?
C25 N3 C21 119.2(4) . . ?
C24 N4 C25 113.5(4) . . ?
C24 N4 C22 124.3(4) . . ?
C25 N4 C22 121.4(4) . . ?
C23 N5 C29 113.4(4) . . ?
C23 N5 C33 124.8(4) . . ?
C29 N5 C33 121.6(4) . . ?
C24 N6 C29 111.3(4) . . ?
C24 N6 C34 120.9(4) . . ?
C29 N6 C34 120.8(4) . . ?
C26 O4 C27 116.0(4) . . ?
C30 O6 C31 118.5(4) . . ?
C40 O7 C42 117.4(4) . . ?
C37 O8 C41 117.4(4) . . ?

_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full        20.81
_diffrn_measured_fraction_theta_full 0.978
_refine_diff_density_max         0.882
_refine_diff_density_min         -0.727
_refine_diff_density_rms         0.087


# start Validation Reply Form
_vrf_THETM01_1                   
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
            Calculated sin(theta_max)/wavelength =    0.4971  
RESPONSE: Although we have re-tried several times to selected better
crystals for x-ray diffraction experiment, we are failed each time. 
This may be resulted from the weak diffraction ability at the high 
two-theta angle for such a small crystal. 
;
# end Validation Reply Form
#==END
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 992390'
_audit_update_record             
;
2014-03-18 deposited with the CCDC.
2015-02-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C45 H33 Cl3 F10 N4 O8'
_chemical_formula_weight         1054.10

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'

_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                   10.8333(15)
_cell_length_b                   14.2199(19)
_cell_length_c                   15.066(2)
_cell_angle_alpha                93.122(2)
_cell_angle_beta                 108.057(2)
_cell_angle_gamma                99.045(2)
_cell_volume                     2166.0(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4120
_cell_measurement_theta_min      2.15
_cell_measurement_theta_max      25.27

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      1.616
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1072
_exptl_absorpt_coefficient_mu    0.316
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  0.9394
_exptl_absorpt_correction_T_max  0.9691
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15848
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0542
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.43
_diffrn_reflns_theta_max         25.50
_reflns_number_total             7961
_reflns_number_gt                5667
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 
 Refinement of 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+0.7500P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7961
_refine_ls_number_parameters     636
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0592
_refine_ls_wR_factor_ref         0.1893
_refine_ls_wR_factor_gt          0.1666
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_restrained_S_all      1.157
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6141(3) 0.6380(2) 0.1867(2) 0.0260(8) Uani 1 1 d . . .
C2 C 0.5393(4) 0.6144(3) 0.0922(3) 0.0341(9) Uani 1 1 d . . .
C3 C 0.5939(5) 0.6292(3) 0.0205(3) 0.0400(10) Uani 1 1 d . . .
C4 C 0.7253(4) 0.6675(3) 0.0413(3) 0.0377(10) Uani 1 1 d . . .
C5 C 0.8000(4) 0.6938(3) 0.1335(3) 0.0316(8) Uani 1 1 d . . .
C6 C 0.7448(4) 0.6794(2) 0.2036(2) 0.0268(8) Uani 1 1 d . . .
C7 C 0.5605(4) 0.6220(3) 0.2647(2) 0.0263(8) Uani 1 1 d . . .
H7 H 0.5993 0.6649 0.3206 0.032 Uiso 1 1 calc R . .
C8 C 0.4627(4) 0.5526(3) 0.2625(3) 0.0283(8) Uani 1 1 d . . .
H8 H 0.4254 0.5104 0.2060 0.034 Uiso 1 1 calc R . .
C9 C 0.4047(3) 0.5331(2) 0.3378(2) 0.0219(7) Uani 1 1 d . . .
C10 C 0.3063(3) 0.4527(2) 0.3286(2) 0.0204(7) Uani 1 1 d . . .
C11 C 0.2456(3) 0.4404(2) 0.3982(2) 0.0185(7) Uani 1 1 d . . .
C12 C 0.2882(3) 0.5050(2) 0.4814(2) 0.0213(7) Uani 1 1 d . . .
C13 C 0.3886(3) 0.5843(2) 0.4897(2) 0.0231(7) Uani 1 1 d . . .
H13 H 0.4184 0.6289 0.5445 0.028 Uiso 1 1 calc R . .
C14 C 0.4441(3) 0.5982(2) 0.4202(2) 0.0243(7) Uani 1 1 d . . .
H14 H 0.5107 0.6528 0.4275 0.029 Uiso 1 1 calc R . .
C15 C 0.2287(3) 0.4888(2) 0.5553(2) 0.0220(7) Uani 1 1 d . . .
H15 H 0.1891 0.4248 0.5572 0.026 Uiso 1 1 calc R . .
C16 C 0.2239(3) 0.5551(2) 0.6213(2) 0.0235(7) Uani 1 1 d . . .
H16 H 0.2655 0.6194 0.6226 0.028 Uiso 1 1 calc R . .
C17 C 0.1582(3) 0.5333(2) 0.6907(2) 0.0232(7) Uani 1 1 d . . .
C18 C 0.1977(3) 0.5894(3) 0.7773(2) 0.0268(8) Uani 1 1 d . . .
C19 C 0.1387(4) 0.5731(3) 0.8446(2) 0.0301(8) Uani 1 1 d . . .
C20 C 0.0314(4) 0.4995(3) 0.8276(3) 0.0303(8) Uani 1 1 d . . .
C21 C -0.0131(4) 0.4436(3) 0.7425(3) 0.0300(8) Uani 1 1 d . . .
C22 C 0.0495(4) 0.4605(3) 0.6765(2) 0.0269(8) Uani 1 1 d . . .
C23 C 0.2603(3) 0.3785(2) 0.2427(2) 0.0219(7) Uani 1 1 d . . .
H23A H 0.1678 0.3815 0.2064 0.026 Uiso 1 1 calc R . .
H23B H 0.3150 0.3955 0.2021 0.026 Uiso 1 1 calc R . .
C24 C 0.1251(3) 0.3619(2) 0.3802(2) 0.0199(7) Uani 1 1 d . . .
H24A H 0.0864 0.3712 0.4308 0.024 Uiso 1 1 calc R . .
H24B H 0.0587 0.3704 0.3205 0.024 Uiso 1 1 calc R . .
C25 C 0.3772(3) 0.2399(2) 0.2753(2) 0.0197(7) Uani 1 1 d . . .
C26 C 0.2138(3) 0.2248(2) 0.4541(2) 0.0177(7) Uani 1 1 d . . .
C27 C 0.1669(3) 0.2214(2) 0.2926(2) 0.0174(7) Uani 1 1 d . . .
C28 C 0.0363(3) 0.1975(2) 0.2091(2) 0.0252(8) Uani 1 1 d . . .
C29 C -0.0736(5) 0.1009(4) 0.0614(3) 0.0496(12) Uani 1 1 d . . .
H29A H -0.0740 0.0336 0.0404 0.059 Uiso 1 1 calc R . .
H29B H -0.1534 0.1031 0.0797 0.059 Uiso 1 1 calc R . .
C30 C -0.0717(6) 0.1609(4) -0.0132(4) 0.0692(15) Uani 1 1 d . . .
H30A H -0.0706 0.2272 0.0087 0.104 Uiso 1 1 calc R . .
H30B H -0.1506 0.1382 -0.0679 0.104 Uiso 1 1 calc R . .
H30C H 0.0074 0.1577 -0.0309 0.104 Uiso 1 1 calc R . .
C31 C 0.2336(3) 0.1342(2) 0.3262(2) 0.0158(6) Uani 1 1 d . . .
C32 C 0.1466(3) 0.0351(2) 0.2835(2) 0.0209(7) Uani 1 1 d . . .
C33 C -0.0573(4) -0.0613(3) 0.2751(3) 0.0362(9) Uani 1 1 d . . .
H33A H -0.0126 -0.1169 0.2889 0.043 Uiso 1 1 calc R . .
H33B H -0.1013 -0.0655 0.2064 0.043 Uiso 1 1 calc R . .
C34 C -0.1563(4) -0.0605(3) 0.3258(4) 0.0501(12) Uani 1 1 d . . .
H34A H -0.1117 -0.0578 0.3935 0.075 Uiso 1 1 calc R . .
H34B H -0.2237 -0.1188 0.3044 0.075 Uiso 1 1 calc R . .
H34C H -0.1982 -0.0042 0.3126 0.075 Uiso 1 1 calc R . .
C35 C 0.4603(3) 0.0978(2) 0.3409(2) 0.0197(7) Uani 1 1 d . . .
H35A H 0.5202 0.1041 0.3027 0.024 Uiso 1 1 calc R . .
H35B H 0.4221 0.0289 0.3357 0.024 Uiso 1 1 calc R . .
C36 C 0.3364(3) 0.0896(2) 0.4904(2) 0.0181(7) Uani 1 1 d . . .
H36A H 0.3140 0.0221 0.4620 0.022 Uiso 1 1 calc R . .
H36B H 0.3142 0.0914 0.5493 0.022 Uiso 1 1 calc R . .
C37 C 0.5414(3) 0.1308(2) 0.4427(2) 0.0191(7) Uani 1 1 d . . .
C38 C 0.4840(3) 0.1249(2) 0.5134(2) 0.0180(7) Uani 1 1 d . . .
C39 C 0.5626(3) 0.1510(2) 0.6077(2) 0.0236(7) Uani 1 1 d . . .
C40 C 0.6976(3) 0.1831(2) 0.6300(2) 0.0257(8) Uani 1 1 d . . .
H40 H 0.7510 0.2006 0.6937 0.031 Uiso 1 1 calc R . .
C41 C 0.7541(3) 0.1895(2) 0.5597(3) 0.0264(8) Uani 1 1 d . . .
H41 H 0.8463 0.2122 0.5752 0.032 Uiso 1 1 calc R . .
C42 C 0.6775(3) 0.1632(2) 0.4666(2) 0.0234(7) Uani 1 1 d . . .
C43 C 0.5754(4) 0.1656(3) 0.7698(2) 0.0337(9) Uani 1 1 d . . .
H43A H 0.6408 0.1237 0.7868 0.051 Uiso 1 1 calc R . .
H43B H 0.5176 0.1565 0.8087 0.051 Uiso 1 1 calc R . .
H43C H 0.6207 0.2325 0.7805 0.051 Uiso 1 1 calc R . .
C44 C 0.8660(4) 0.1975(3) 0.4139(3) 0.0355(9) Uani 1 1 d . . .
H44A H 0.8920 0.2617 0.4484 0.053 Uiso 1 1 calc R . .
H44B H 0.8873 0.1993 0.3553 0.053 Uiso 1 1 calc R . .
H44C H 0.9139 0.1531 0.4525 0.053 Uiso 1 1 calc R . .
C45 C 0.5195(4) 0.1437(3) 0.0996(3) 0.0416(10) Uani 1 1 d . . .
H45 H 0.5428 0.1982 0.1502 0.050 Uiso 1 1 calc R . .
Cl1 Cl 0.57487(13) 0.18381(9) 0.00796(8) 0.0526(3) Uani 1 1 d . . .
Cl2 Cl 0.60075(15) 0.05098(9) 0.14634(9) 0.0597(4) Uani 1 1 d . . .
Cl3 Cl 0.34793(13) 0.10545(12) 0.06122(10) 0.0740(5) Uani 1 1 d . . .
F1 F 0.4091(2) 0.57901(19) 0.06617(16) 0.0469(6) Uani 1 1 d . . .
F2 F 0.5167(3) 0.6066(2) -0.06952(16) 0.0545(7) Uani 1 1 d . . .
F3 F 0.7787(3) 0.67960(19) -0.02725(16) 0.0526(7) Uani 1 1 d . . .
F4 F 0.9292(2) 0.73157(17) 0.15513(16) 0.0399(6) Uani 1 1 d . . .
F5 F 0.8243(2) 0.70547(14) 0.29312(14) 0.0313(5) Uani 1 1 d . . .
F6 F -0.0043(2) 0.40415(15) 0.59355(14) 0.0327(5) Uani 1 1 d . . .
F7 F -0.1193(2) 0.37329(16) 0.72362(17) 0.0406(6) Uani 1 1 d . . .
F8 F -0.0278(2) 0.48288(18) 0.89248(16) 0.0454(6) Uani 1 1 d . . .
F9 F 0.1816(2) 0.62846(17) 0.92720(15) 0.0418(6) Uani 1 1 d . . .
F10 F 0.2984(2) 0.66304(16) 0.79535(15) 0.0374(5) Uani 1 1 d . . .
N1 N 0.2671(3) 0.28039(19) 0.26438(19) 0.0203(6) Uani 1 1 d . . .
N2 N 0.1469(3) 0.26298(18) 0.37489(18) 0.0176(6) Uani 1 1 d . . .
N3 N 0.3532(2) 0.14953(18) 0.30076(18) 0.0165(6) Uani 1 1 d . . .
N4 N 0.2571(3) 0.14639(19) 0.42620(18) 0.0181(6) Uani 1 1 d . . .
O1 O 0.4784(2) 0.27801(16) 0.26214(16) 0.0226(5) Uani 1 1 d . . .
O2 O 0.2284(2) 0.25458(16) 0.53449(15) 0.0211(5) Uani 1 1 d . . .
O3 O -0.0619(2) 0.22717(18) 0.20760(17) 0.0308(6) Uani 1 1 d . . .
O4 O 0.0488(3) 0.1400(2) 0.14247(18) 0.0404(7) Uani 1 1 d . . .
O5 O 0.1733(2) -0.02463(17) 0.23685(17) 0.0282(6) Uani 1 1 d . . .
O6 O 0.0381(2) 0.02789(17) 0.30822(18) 0.0277(6) Uani 1 1 d . . .
O7 O 0.4980(2) 0.14228(17) 0.67296(16) 0.0268(5) Uani 1 1 d . . .
O8 O 0.7276(2) 0.16582(19) 0.39297(18) 0.0300(6) Uani 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
C1 C6 1.384(5) . ?
C1 C2 1.395(5) . ?
C1 C7 1.475(5) . ?
C2 F1 1.345(5) . ?
C2 C3 1.392(6) . ?
C3 F2 1.345(5) . ?
C3 C4 1.372(6) . ?
C4 F3 1.339(4) . ?
C4 C5 1.369(6) . ?
C5 F4 1.347(4) . ?
C5 C6 1.375(5) . ?
C6 F5 1.351(4) . ?
C7 C8 1.321(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.476(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.403(5) . ?
C9 C14 1.416(5) . ?
C10 C11 1.404(5) . ?
C10 C23 1.525(4) . ?
C11 C12 1.418(5) . ?
C11 C24 1.521(4) . ?
C12 C13 1.409(5) . ?
C12 C15 1.462(5) . ?
C13 C14 1.367(5) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 C16 1.351(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.457(5) . ?
C16 H16 0.9500 . ?
C17 C22 1.393(5) . ?
C17 C18 1.398(5) . ?
C18 F10 1.337(4) . ?
C18 C19 1.369(5) . ?
C19 F9 1.343(4) . ?
C19 C20 1.384(6) . ?
C20 F8 1.338(4) . ?
C20 C21 1.376(5) . ?
C21 F7 1.346(4) . ?
C21 C22 1.377(5) . ?
C22 F6 1.355(4) . ?
C23 N1 1.458(4) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 N2 1.464(4) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 O1 1.222(4) . ?
C25 N3 1.370(4) . ?
C25 N1 1.373(4) . ?
C26 O2 1.214(4) . ?
C26 N4 1.369(4) . ?
C26 N2 1.380(4) . ?
C27 N2 1.436(4) . ?
C27 N1 1.450(4) . ?
C27 C28 1.548(5) . ?
C27 C31 1.562(4) . ?
C28 O3 1.199(4) . ?
C28 O4 1.313(4) . ?
C29 C30 1.450(7) . ?
C29 O4 1.500(5) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 N4 1.444(4) . ?
C31 N3 1.449(4) . ?
C31 C32 1.548(4) . ?
C32 O5 1.199(4) . ?
C32 O6 1.330(4) . ?
C33 O6 1.457(4) . ?
C33 C34 1.498(6) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 N3 1.462(4) . ?
C35 C37 1.518(4) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 N4 1.455(4) . ?
C36 C38 1.521(4) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 C38 1.390(5) . ?
C37 C42 1.398(5) . ?
C38 C39 1.405(5) . ?
C39 O7 1.373(4) . ?
C39 C40 1.388(5) . ?
C40 C41 1.378(5) . ?
C40 H40 0.9500 . ?
C41 C42 1.385(5) . ?
C41 H41 0.9500 . ?
C42 O8 1.379(4) . ?
C43 O7 1.430(4) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 O8 1.424(4) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 Cl3 1.751(4) . ?
C45 Cl1 1.755(4) . ?
C45 Cl2 1.759(5) . ?
C45 H45 1.0000 . ?

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
C6 C1 C2 115.0(3) . . ?
C6 C1 C7 121.2(3) . . ?
C2 C1 C7 123.8(3) . . ?
F1 C2 C3 116.9(3) . . ?
F1 C2 C1 120.9(3) . . ?
C3 C2 C1 122.1(4) . . ?
F2 C3 C4 119.9(4) . . ?
F2 C3 C2 119.6(4) . . ?
C4 C3 C2 120.4(4) . . ?
F3 C4 C5 120.8(4) . . ?
F3 C4 C3 120.5(4) . . ?
C5 C4 C3 118.6(4) . . ?
F4 C5 C4 119.4(3) . . ?
F4 C5 C6 120.2(3) . . ?
C4 C5 C6 120.4(4) . . ?
F5 C6 C5 117.5(3) . . ?
F5 C6 C1 119.1(3) . . ?
C5 C6 C1 123.4(3) . . ?
C8 C7 C1 124.9(3) . . ?
C8 C7 H7 117.5 . . ?
C1 C7 H7 117.5 . . ?
C7 C8 C9 127.5(3) . . ?
C7 C8 H8 116.3 . . ?
C9 C8 H8 116.3 . . ?
C10 C9 C14 118.2(3) . . ?
C10 C9 C8 121.7(3) . . ?
C14 C9 C8 120.1(3) . . ?
C9 C10 C11 120.2(3) . . ?
C9 C10 C23 121.3(3) . . ?
C11 C10 C23 118.5(3) . . ?
C10 C11 C12 120.9(3) . . ?
C10 C11 C24 119.4(3) . . ?
C12 C11 C24 119.5(3) . . ?
C13 C12 C11 117.8(3) . . ?
C13 C12 C15 121.8(3) . . ?
C11 C12 C15 120.4(3) . . ?
C14 C13 C12 121.2(3) . . ?
C14 C13 H13 119.4 . . ?
C12 C13 H13 119.4 . . ?
C13 C14 C9 121.6(3) . . ?
C13 C14 H14 119.2 . . ?
C9 C14 H14 119.2 . . ?
C16 C15 C12 127.1(3) . . ?
C16 C15 H15 116.5 . . ?
C12 C15 H15 116.5 . . ?
C15 C16 C17 123.5(3) . . ?
C15 C16 H16 118.3 . . ?
C17 C16 H16 118.3 . . ?
C22 C17 C18 114.4(3) . . ?
C22 C17 C16 124.6(3) . . ?
C18 C17 C16 120.9(3) . . ?
F10 C18 C19 118.1(3) . . ?
F10 C18 C17 118.4(3) . . ?
C19 C18 C17 123.5(3) . . ?
F9 C19 C18 121.2(3) . . ?
F9 C19 C20 118.8(3) . . ?
C18 C19 C20 120.0(3) . . ?
F8 C20 C21 120.6(3) . . ?
F8 C20 C19 120.8(3) . . ?
C21 C20 C19 118.6(3) . . ?
F7 C21 C20 119.5(3) . . ?
F7 C21 C22 120.2(3) . . ?
C20 C21 C22 120.3(3) . . ?
F6 C22 C21 116.0(3) . . ?
F6 C22 C17 120.7(3) . . ?
C21 C22 C17 123.2(3) . . ?
N1 C23 C10 114.3(3) . . ?
N1 C23 H23A 108.7 . . ?
C10 C23 H23A 108.7 . . ?
N1 C23 H23B 108.7 . . ?
C10 C23 H23B 108.7 . . ?
H23A C23 H23B 107.6 . . ?
N2 C24 C11 116.6(3) . . ?
N2 C24 H24A 108.1 . . ?
C11 C24 H24A 108.1 . . ?
N2 C24 H24B 108.1 . . ?
C11 C24 H24B 108.1 . . ?
H24A C24 H24B 107.3 . . ?
O1 C25 N3 126.0(3) . . ?
O1 C25 N1 125.2(3) . . ?
N3 C25 N1 108.7(3) . . ?
O2 C26 N4 126.2(3) . . ?
O2 C26 N2 125.5(3) . . ?
N4 C26 N2 108.2(3) . . ?
N2 C27 N1 113.4(3) . . ?
N2 C27 C28 111.4(3) . . ?
N1 C27 C28 109.7(3) . . ?
N2 C27 C31 104.1(2) . . ?
N1 C27 C31 102.3(2) . . ?
C28 C27 C31 115.7(3) . . ?
O3 C28 O4 125.7(3) . . ?
O3 C28 C27 123.8(3) . . ?
O4 C28 C27 110.5(3) . . ?
C30 C29 O4 106.5(4) . . ?
C30 C29 H29A 110.4 . . ?
O4 C29 H29A 110.4 . . ?
C30 C29 H29B 110.4 . . ?
O4 C29 H29B 110.4 . . ?
H29A C29 H29B 108.6 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N4 C31 N3 113.8(3) . . ?
N4 C31 C32 109.8(2) . . ?
N3 C31 C32 111.9(2) . . ?
N4 C31 C27 102.3(2) . . ?
N3 C31 C27 104.1(2) . . ?
C32 C31 C27 114.6(2) . . ?
O5 C32 O6 126.3(3) . . ?
O5 C32 C31 125.7(3) . . ?
O6 C32 C31 108.0(3) . . ?
O6 C33 C34 106.8(3) . . ?
O6 C33 H33A 110.4 . . ?
C34 C33 H33A 110.4 . . ?
O6 C33 H33B 110.4 . . ?
C34 C33 H33B 110.4 . . ?
H33A C33 H33B 108.6 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N3 C35 C37 115.3(3) . . ?
N3 C35 H35A 108.5 . . ?
C37 C35 H35A 108.5 . . ?
N3 C35 H35B 108.5 . . ?
C37 C35 H35B 108.5 . . ?
H35A C35 H35B 107.5 . . ?
N4 C36 C38 112.8(3) . . ?
N4 C36 H36A 109.0 . . ?
C38 C36 H36A 109.0 . . ?
N4 C36 H36B 109.0 . . ?
C38 C36 H36B 109.0 . . ?
H36A C36 H36B 107.8 . . ?
C38 C37 C42 119.3(3) . . ?
C38 C37 C35 121.1(3) . . ?
C42 C37 C35 119.5(3) . . ?
C37 C38 C39 120.0(3) . . ?
C37 C38 C36 120.9(3) . . ?
C39 C38 C36 119.1(3) . . ?
O7 C39 C40 124.0(3) . . ?
O7 C39 C38 116.1(3) . . ?
C40 C39 C38 119.9(3) . . ?
C41 C40 C39 120.0(3) . . ?
C41 C40 H40 120.0 . . ?
C39 C40 H40 120.0 . . ?
C40 C41 C42 120.5(3) . . ?
C40 C41 H41 119.8 . . ?
C42 C41 H41 119.8 . . ?
O8 C42 C41 123.7(3) . . ?
O8 C42 C37 116.0(3) . . ?
C41 C42 C37 120.4(3) . . ?
O7 C43 H43A 109.5 . . ?
O7 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
O7 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
O8 C44 H44A 109.5 . . ?
O8 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
O8 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
Cl3 C45 Cl1 111.4(2) . . ?
Cl3 C45 Cl2 110.8(2) . . ?
Cl1 C45 Cl2 109.4(2) . . ?
Cl3 C45 H45 108.4 . . ?
Cl1 C45 H45 108.4 . . ?
Cl2 C45 H45 108.4 . . ?
C25 N1 C27 112.6(3) . . ?
C25 N1 C23 123.7(3) . . ?
C27 N1 C23 122.9(3) . . ?
C26 N2 C27 111.2(2) . . ?
C26 N2 C24 121.0(3) . . ?
C27 N2 C24 120.0(3) . . ?
C25 N3 C31 111.0(2) . . ?
C25 N3 C35 121.6(3) . . ?
C31 N3 C35 121.1(2) . . ?
C26 N4 C31 112.8(3) . . ?
C26 N4 C36 124.2(3) . . ?
C31 N4 C36 122.4(2) . . ?
C28 O4 C29 117.1(3) . . ?
C32 O6 C33 116.6(3) . . ?
C39 O7 C43 117.8(3) . . ?
C42 O8 C44 118.0(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
C6 C1 C2 F1 -176.0(3) . . . . ?
C7 C1 C2 F1 3.3(6) . . . . ?
C6 C1 C2 C3 1.7(5) . . . . ?
C7 C1 C2 C3 -179.0(4) . . . . ?
F1 C2 C3 F2 -1.2(6) . . . . ?
C1 C2 C3 F2 -178.9(4) . . . . ?
F1 C2 C3 C4 178.3(4) . . . . ?
C1 C2 C3 C4 0.5(6) . . . . ?
F2 C3 C4 F3 -2.2(6) . . . . ?
C2 C3 C4 F3 178.3(4) . . . . ?
F2 C3 C4 C5 177.1(4) . . . . ?
C2 C3 C4 C5 -2.3(6) . . . . ?
F3 C4 C5 F4 -0.6(6) . . . . ?
C3 C4 C5 F4 -179.9(4) . . . . ?
F3 C4 C5 C6 -178.7(3) . . . . ?
C3 C4 C5 C6 1.9(6) . . . . ?
F4 C5 C6 F5 0.8(5) . . . . ?
C4 C5 C6 F5 178.9(3) . . . . ?
F4 C5 C6 C1 -177.7(3) . . . . ?
C4 C5 C6 C1 0.4(6) . . . . ?
C2 C1 C6 F5 179.3(3) . . . . ?
C7 C1 C6 F5 0.0(5) . . . . ?
C2 C1 C6 C5 -2.1(5) . . . . ?
C7 C1 C6 C5 178.6(3) . . . . ?
C6 C1 C7 C8 -150.7(4) . . . . ?
C2 C1 C7 C8 30.1(6) . . . . ?
C1 C7 C8 C9 -179.9(3) . . . . ?
C7 C8 C9 C10 -175.7(3) . . . . ?
C7 C8 C9 C14 6.9(5) . . . . ?
C14 C9 C10 C11 2.7(4) . . . . ?
C8 C9 C10 C11 -174.8(3) . . . . ?
C14 C9 C10 C23 -178.9(3) . . . . ?
C8 C9 C10 C23 3.6(5) . . . . ?
C9 C10 C11 C12 -4.2(5) . . . . ?
C23 C10 C11 C12 177.4(3) . . . . ?
C9 C10 C11 C24 170.5(3) . . . . ?
C23 C10 C11 C24 -8.0(4) . . . . ?
C10 C11 C12 C13 3.1(4) . . . . ?
C24 C11 C12 C13 -171.6(3) . . . . ?
C10 C11 C12 C15 -177.0(3) . . . . ?
C24 C11 C12 C15 8.4(4) . . . . ?
C11 C12 C13 C14 -0.5(5) . . . . ?
C15 C12 C13 C14 179.5(3) . . . . ?
C12 C13 C14 C9 -0.9(5) . . . . ?
C10 C9 C14 C13 -0.1(5) . . . . ?
C8 C9 C14 C13 177.4(3) . . . . ?
C13 C12 C15 C16 23.7(5) . . . . ?
C11 C12 C15 C16 -156.3(3) . . . . ?
C12 C15 C16 C17 177.8(3) . . . . ?
C15 C16 C17 C22 -29.6(5) . . . . ?
C15 C16 C17 C18 153.9(3) . . . . ?
C22 C17 C18 F10 -177.6(3) . . . . ?
C16 C17 C18 F10 -0.8(5) . . . . ?
C22 C17 C18 C19 2.2(5) . . . . ?
C16 C17 C18 C19 179.1(3) . . . . ?
F10 C18 C19 F9 -1.0(5) . . . . ?
C17 C18 C19 F9 179.1(3) . . . . ?
F10 C18 C19 C20 177.9(3) . . . . ?
C17 C18 C19 C20 -2.0(6) . . . . ?
F9 C19 C20 F8 -0.7(5) . . . . ?
C18 C19 C20 F8 -179.7(3) . . . . ?
F9 C19 C20 C21 179.3(3) . . . . ?
C18 C19 C20 C21 0.4(5) . . . . ?
F8 C20 C21 F7 1.8(5) . . . . ?
C19 C20 C21 F7 -178.3(3) . . . . ?
F8 C20 C21 C22 -179.2(3) . . . . ?
C19 C20 C21 C22 0.7(5) . . . . ?
F7 C21 C22 F6 1.4(5) . . . . ?
C20 C21 C22 F6 -177.6(3) . . . . ?
F7 C21 C22 C17 178.7(3) . . . . ?
C20 C21 C22 C17 -0.3(6) . . . . ?
C18 C17 C22 F6 176.1(3) . . . . ?
C16 C17 C22 F6 -0.6(5) . . . . ?
C18 C17 C22 C21 -1.1(5) . . . . ?
C16 C17 C22 C21 -177.8(3) . . . . ?
C9 C10 C23 N1 125.8(3) . . . . ?
C11 C10 C23 N1 -55.7(4) . . . . ?
C10 C11 C24 N2 68.1(4) . . . . ?
C12 C11 C24 N2 -117.2(3) . . . . ?
N2 C27 C28 O3 13.9(5) . . . . ?
N1 C27 C28 O3 -112.5(4) . . . . ?
C31 C27 C28 O3 132.5(3) . . . . ?
N2 C27 C28 O4 -165.1(3) . . . . ?
N1 C27 C28 O4 68.5(3) . . . . ?
C31 C27 C28 O4 -46.5(4) . . . . ?
N2 C27 C31 N4 -7.0(3) . . . . ?
N1 C27 C31 N4 111.3(3) . . . . ?
C28 C27 C31 N4 -129.6(3) . . . . ?
N2 C27 C31 N3 -125.7(2) . . . . ?
N1 C27 C31 N3 -7.4(3) . . . . ?
C28 C27 C31 N3 111.7(3) . . . . ?
N2 C27 C31 C32 111.8(3) . . . . ?
N1 C27 C31 C32 -129.9(3) . . . . ?
C28 C27 C31 C32 -10.8(4) . . . . ?
N4 C31 C32 O5 -125.5(3) . . . . ?
N3 C31 C32 O5 1.9(5) . . . . ?
C27 C31 C32 O5 120.1(4) . . . . ?
N4 C31 C32 O6 54.1(3) . . . . ?
N3 C31 C32 O6 -178.5(3) . . . . ?
C27 C31 C32 O6 -60.3(3) . . . . ?
N3 C35 C37 C38 61.8(4) . . . . ?
N3 C35 C37 C42 -121.5(3) . . . . ?
C42 C37 C38 C39 -0.3(5) . . . . ?
C35 C37 C38 C39 176.5(3) . . . . ?
C42 C37 C38 C36 -179.7(3) . . . . ?
C35 C37 C38 C36 -2.9(4) . . . . ?
N4 C36 C38 C37 -57.9(4) . . . . ?
N4 C36 C38 C39 122.7(3) . . . . ?
C37 C38 C39 O7 -179.5(3) . . . . ?
C36 C38 C39 O7 -0.1(4) . . . . ?
C37 C38 C39 C40 0.3(5) . . . . ?
C36 C38 C39 C40 179.7(3) . . . . ?
O7 C39 C40 C41 180.0(3) . . . . ?
C38 C39 C40 C41 0.2(5) . . . . ?
C39 C40 C41 C42 -0.7(5) . . . . ?
C40 C41 C42 O8 -178.6(3) . . . . ?
C40 C41 C42 C37 0.8(5) . . . . ?
C38 C37 C42 O8 179.1(3) . . . . ?
C35 C37 C42 O8 2.3(4) . . . . ?
C38 C37 C42 C41 -0.2(5) . . . . ?
C35 C37 C42 C41 -177.1(3) . . . . ?
O1 C25 N1 C27 -175.2(3) . . . . ?
N3 C25 N1 C27 6.4(4) . . . . ?
O1 C25 N1 C23 -5.2(5) . . . . ?
N3 C25 N1 C23 176.4(3) . . . . ?
N2 C27 N1 C25 112.5(3) . . . . ?
C28 C27 N1 C25 -122.3(3) . . . . ?
C31 C27 N1 C25 1.0(3) . . . . ?
N2 C27 N1 C23 -57.6(4) . . . . ?
C28 C27 N1 C23 67.6(4) . . . . ?
C31 C27 N1 C23 -169.1(3) . . . . ?
C10 C23 N1 C25 -88.1(4) . . . . ?
C10 C23 N1 C27 80.9(4) . . . . ?
O2 C26 N2 C27 170.2(3) . . . . ?
N4 C26 N2 C27 -11.5(3) . . . . ?
O2 C26 N2 C24 21.1(5) . . . . ?
N4 C26 N2 C24 -160.6(3) . . . . ?
N1 C27 N2 C26 -98.9(3) . . . . ?
C28 C27 N2 C26 136.8(3) . . . . ?
C31 C27 N2 C26 11.4(3) . . . . ?
N1 C27 N2 C24 50.5(4) . . . . ?
C28 C27 N2 C24 -73.8(3) . . . . ?
C31 C27 N2 C24 160.9(3) . . . . ?
C11 C24 N2 C26 71.1(4) . . . . ?
C11 C24 N2 C27 -75.4(4) . . . . ?
O1 C25 N3 C31 169.9(3) . . . . ?
N1 C25 N3 C31 -11.7(3) . . . . ?
O1 C25 N3 C35 17.7(5) . . . . ?
N1 C25 N3 C35 -163.9(3) . . . . ?
N4 C31 N3 C25 -98.7(3) . . . . ?
C32 C31 N3 C25 136.1(3) . . . . ?
C27 C31 N3 C25 11.8(3) . . . . ?
N4 C31 N3 C35 53.7(4) . . . . ?
C32 C31 N3 C35 -71.6(3) . . . . ?
C27 C31 N3 C35 164.2(3) . . . . ?
C37 C35 N3 C25 75.7(4) . . . . ?
C37 C35 N3 C31 -73.7(4) . . . . ?
O2 C26 N4 C31 -175.3(3) . . . . ?
N2 C26 N4 C31 6.4(3) . . . . ?
O2 C26 N4 C36 -4.4(5) . . . . ?
N2 C26 N4 C36 177.4(3) . . . . ?
N3 C31 N4 C26 112.2(3) . . . . ?
C32 C31 N4 C26 -121.5(3) . . . . ?
C27 C31 N4 C26 0.6(3) . . . . ?
N3 C31 N4 C36 -58.9(4) . . . . ?
C32 C31 N4 C36 67.4(4) . . . . ?
C27 C31 N4 C36 -170.5(3) . . . . ?
C38 C36 N4 C26 -90.9(3) . . . . ?
C38 C36 N4 C31 79.2(4) . . . . ?
O3 C28 O4 C29 -5.9(6) . . . . ?
C27 C28 O4 C29 173.1(3) . . . . ?
C30 C29 O4 C28 97.8(5) . . . . ?
O5 C32 O6 C33 -0.1(5) . . . . ?
C31 C32 O6 C33 -179.7(3) . . . . ?
C34 C33 O6 C32 169.5(3) . . . . ?
C40 C39 O7 C43 -1.5(5) . . . . ?
C38 C39 O7 C43 178.3(3) . . . . ?
C41 C42 O8 C44 0.0(5) . . . . ?
C37 C42 O8 C44 -179.4(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.824
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.100
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3
_database_code_depnum_ccdc_archive 'CCDC 992391'
_audit_update_record             
;
2014-03-18 deposited with the CCDC.
2015-02-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H46 Cl6 N6 O10'
_chemical_formula_weight         1055.59

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'

_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                   11.0037(13)
_cell_length_b                   13.2032(14)
_cell_length_c                   17.428(3)
_cell_angle_alpha                89.128(2)
_cell_angle_beta                 76.376(2)
_cell_angle_gamma                72.207(11)
_cell_volume                     2338.6(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4835
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      28.26

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      1.499
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1092
_exptl_absorpt_coefficient_mu    0.433
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  0.9183
_exptl_absorpt_correction_T_max  0.9183
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14575
_diffrn_reflns_av_R_equivalents  0.1022
_diffrn_reflns_av_sigmaI/netI    0.1087
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.96
_diffrn_reflns_theta_max         25.01
_reflns_number_total             8145
_reflns_number_gt                6350
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0909P)²+11.7393P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8145
_refine_ls_number_parameters     619
_refine_ls_number_restraints     78
_refine_ls_R_factor_all          0.1276
_refine_ls_R_factor_gt           0.1070
_refine_ls_wR_factor_ref         0.2575
_refine_ls_wR_factor_gt          0.2451
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_restrained_S_all      1.135
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.0076(4) 0.8727(3) 0.3095(3) 0.0287(11) Uani 1 1 d . . .
O2 O 0.0941(4) 0.3561(3) 0.2207(3) 0.0212(9) Uani 1 1 d . . .
O3 O 0.4866(3) 0.7276(3) 0.3221(2) 0.0131(8) Uani 1 1 d . . .
O4 O 0.5811(4) 0.3097(3) 0.2371(2) 0.0154(8) Uani 1 1 d . . .
O5 O 0.6614(4) 0.5229(3) 0.0130(2) 0.0235(10) Uani 1 1 d . . .
O6 O 0.7104(4) 0.6534(3) 0.0679(2) 0.0202(9) Uani 1 1 d . . .
O7 O 0.9167(4) 0.4332(3) 0.0988(2) 0.0169(9) Uani 1 1 d . . .
O8 O 0.9130(3) 0.5779(3) 0.1667(2) 0.0161(9) Uani 1 1 d . . .
O9 O 0.7165(4) 0.2419(3) 0.4182(2) 0.0171(9) Uani 1 1 d . . .
O10 O 0.6548(4) 0.6639(3) 0.4878(2) 0.0204(9) Uani 1 1 d . . .
N1 N 0.2043(4) 0.7784(3) 0.3310(3) 0.0131(10) Uani 1 1 d . . .
H1A H 0.2700 0.7827 0.3501 0.016 Uiso 1 1 calc R . .
N2 N 0.2867(4) 0.3507(4) 0.2470(3) 0.0131(10) Uani 1 1 d . . .
H2A H 0.3635 0.3093 0.2525 0.016 Uiso 1 1 calc R . .
N3 N 0.5278(4) 0.6425(4) 0.2002(3) 0.0117(10) Uani 1 1 d . . .
N4 N 0.5707(4) 0.4557(3) 0.1615(3) 0.0111(9) Uani 1 1 d . . .
N5 N 0.6834(4) 0.5974(3) 0.2667(3) 0.0109(9) Uani 1 1 d . . .
N6 N 0.7181(4) 0.4129(3) 0.2338(3) 0.0111(9) Uani 1 1 d . . .
C1 C 0.2659(6) 1.0693(5) 0.3814(4) 0.0268(15) Uani 1 1 d . . .
H1 H 0.3502 1.0717 0.3842 0.032 Uiso 1 1 calc R . .
C2 C 0.2546(5) 0.9749(4) 0.3574(4) 0.0171(12) Uani 1 1 d . . .
H2 H 0.3300 0.9137 0.3429 0.021 Uiso 1 1 calc R . .
C3 C 0.1310(5) 0.9698(4) 0.3546(3) 0.0146(12) Uani 1 1 d . . .
C4 C 0.0243(5) 1.0612(5) 0.3744(4) 0.0214(13) Uani 1 1 d . . .
H4 H -0.0605 1.0601 0.3717 0.026 Uiso 1 1 calc R . .
C5 C 0.0417(6) 1.1544(5) 0.3982(4) 0.0295(16) Uani 1 1 d . . .
H5 H -0.0325 1.2165 0.4127 0.035 Uiso 1 1 calc R . .
C6 C 0.1615(6) 1.1594(5) 0.4014(4) 0.0251(15) Uani 1 1 d . . .
H6 H 0.1723 1.2241 0.4172 0.030 Uiso 1 1 calc R . .
C7 C 0.1081(5) 0.8703(5) 0.3291(3) 0.0157(12) Uani 1 1 d . . .
C8 C 0.2092(5) 0.6744(4) 0.3049(3) 0.0136(11) Uani 1 1 d U . .
C9 C 0.3060(5) 0.6259(4) 0.2381(3) 0.0121(11) Uani 1 1 d U . .
C10 C 0.3292(5) 0.5184(4) 0.2174(3) 0.0112(11) Uani 1 1 d U . .
C11 C 0.2533(5) 0.4632(4) 0.2649(3) 0.0143(12) Uani 1 1 d . . .
C12 C 0.1521(5) 0.5129(4) 0.3305(3) 0.0142(12) Uani 1 1 d U . .
C13 C 0.1287(5) 0.6214(4) 0.3507(3) 0.0148(12) Uani 1 1 d U . .
C14 C 0.0772(5) 0.4504(5) 0.3851(4) 0.0187(13) Uani 1 1 d . . .
H14A H 0.1112 0.3751 0.3664 0.028 Uiso 1 1 calc R . .
H14B H -0.0164 0.4783 0.3857 0.028 Uiso 1 1 calc R . .
H14C H 0.0884 0.4575 0.4387 0.028 Uiso 1 1 calc R . .
C15 C 0.0255(5) 0.6744(5) 0.4240(4) 0.0207(13) Uani 1 1 d . . .
H15A H 0.0508 0.6406 0.4707 0.031 Uiso 1 1 calc R . .
H15B H -0.0593 0.6669 0.4212 0.031 Uiso 1 1 calc R . .
H15C H 0.0178 0.7502 0.4277 0.031 Uiso 1 1 calc R . .
C16 C 0.2073(5) 0.3044(4) 0.2224(3) 0.0153(12) Uani 1 1 d . . .
C17 C 0.2638(6) 0.1888(5) 0.1967(3) 0.0181(12) Uani 1 1 d . . .
C18 C 0.3977(7) 0.1360(6) 0.1740(4) 0.0327(16) Uani 1 1 d . . .
H18 H 0.4593 0.1721 0.1766 0.039 Uiso 1 1 calc R . .
C19 C 0.4405(8) 0.0297(6) 0.1474(5) 0.050(2) Uani 1 1 d . . .
H19 H 0.5323 -0.0062 0.1315 0.060 Uiso 1 1 calc R . .
C20 C 0.3566(8) -0.0246(5) 0.1432(4) 0.0375(18) Uani 1 1 d . . .
H20 H 0.3884 -0.0975 0.1248 0.045 Uiso 1 1 calc R . .
C21 C 0.2270(7) 0.0266(5) 0.1656(4) 0.0328(16) Uani 1 1 d . . .
H21 H 0.1672 -0.0115 0.1633 0.039 Uiso 1 1 calc R . .
C22 C 0.1775(7) 0.1324(5) 0.1916(4) 0.0251(14) Uani 1 1 d . . .
H22 H 0.0851 0.1667 0.2061 0.030 Uiso 1 1 calc R . .
C23 C 0.3936(5) 0.6846(4) 0.1898(3) 0.0128(11) Uani 1 1 d U . .
H23A H 0.3949 0.6769 0.1332 0.015 Uiso 1 1 calc R . .
H23B H 0.3578 0.7614 0.2066 0.015 Uiso 1 1 calc R . .
C24 C 0.4416(5) 0.4652(4) 0.1472(3) 0.0136(11) Uani 1 1 d . . .
H24A H 0.4379 0.3932 0.1353 0.016 Uiso 1 1 calc R . .
H24B H 0.4306 0.5071 0.1003 0.016 Uiso 1 1 calc R . .
C25 C 0.5575(5) 0.6624(4) 0.2701(3) 0.0102(11) Uani 1 1 d U . .
C26 C 0.6195(5) 0.3845(4) 0.2138(3) 0.0114(11) Uani 1 1 d . . .
C27 C 0.6190(5) 0.5459(4) 0.1563(3) 0.0129(11) Uani 1 1 d . . .
C28 C 0.6669(5) 0.5705(4) 0.0687(3) 0.0154(12) Uani 1 1 d . . .
C29 C 0.7536(6) 0.6951(5) -0.0078(4) 0.0234(14) Uani 1 1 d . . .
H29A H 0.6932 0.6963 -0.0421 0.028 Uiso 1 1 calc R . .
H29B H 0.8434 0.6507 -0.0353 0.028 Uiso 1 1 calc R . .
C30 C 0.7522(11) 0.8049(7) 0.0108(5) 0.058(3) Uani 1 1 d . . .
H30A H 0.6619 0.8487 0.0352 0.087 Uiso 1 1 calc R . .
H30B H 0.7856 0.8358 -0.0381 0.087 Uiso 1 1 calc R . .
H30C H 0.8081 0.8027 0.0474 0.087 Uiso 1 1 calc R . .
C31 C 0.7283(5) 0.5137(4) 0.2045(3) 0.0123(11) Uani 1 1 d . . .
C32 C 0.8665(5) 0.5017(4) 0.1509(3) 0.0123(11) Uani 1 1 d U . .
C33 C 1.0388(5) 0.5784(5) 0.1144(4) 0.0176(12) Uani 1 1 d . . .
H33A H 1.0370 0.5701 0.0584 0.021 Uiso 1 1 calc R . .
H33B H 1.1118 0.5189 0.1253 0.021 Uiso 1 1 calc R . .
C34 C 1.0577(6) 0.6835(5) 0.1305(4) 0.0261(15) Uani 1 1 d . . .
H34A H 0.9902 0.7412 0.1142 0.039 Uiso 1 1 calc R . .
H34B H 1.1451 0.6836 0.1007 0.039 Uiso 1 1 calc R . .
H34C H 1.0502 0.6940 0.1872 0.039 Uiso 1 1 calc R . .
C35 C 0.7446(5) 0.5924(4) 0.3327(3) 0.0128(11) Uani 1 1 d . . .
H35A H 0.7177 0.6651 0.3580 0.015 Uiso 1 1 calc R . .
H35B H 0.8412 0.5700 0.3116 0.015 Uiso 1 1 calc R . .
C36 C 0.7867(5) 0.3607(4) 0.2933(3) 0.0118(11) Uani 1 1 d . . .
H36A H 0.8793 0.3603 0.2768 0.014 Uiso 1 1 calc R . .
H36B H 0.7872 0.2856 0.2940 0.014 Uiso 1 1 calc R . .
C37 C 0.7119(5) 0.5177(4) 0.3957(3) 0.0125(11) Uani 1 1 d U . .
C38 C 0.7284(5) 0.4116(4) 0.3773(3) 0.0125(11) Uani 1 1 d U . .
C39 C 0.6988(5) 0.3456(4) 0.4395(3) 0.0139(12) Uani 1 1 d . . .
C40 C 0.6556(5) 0.3875(5) 0.5167(4) 0.0187(13) Uani 1 1 d . . .
H40 H 0.6355 0.3432 0.5580 0.022 Uiso 1 1 calc R . .
C41 C 0.6410(5) 0.4929(5) 0.5350(3) 0.0167(12) Uani 1 1 d . . .
H41 H 0.6122 0.5202 0.5885 0.020 Uiso 1 1 calc R . .
C42 C 0.6684(5) 0.5578(4) 0.4752(3) 0.0148(12) Uani 1 1 d . . .
C43 C 0.6933(6) 0.1740(5) 0.4810(4) 0.0222(13) Uani 1 1 d . . .
H43A H 0.7584 0.1658 0.5124 0.033 Uiso 1 1 calc R . .
H43B H 0.7008 0.1040 0.4588 0.033 Uiso 1 1 calc R . .
H43C H 0.6047 0.2057 0.5149 0.033 Uiso 1 1 calc R . .
C44 C 0.6074(6) 0.7081(5) 0.5667(4) 0.0222(13) Uani 1 1 d . . .
H44A H 0.5217 0.6983 0.5896 0.033 Uiso 1 1 calc R . .
H44B H 0.5979 0.7844 0.5673 0.033 Uiso 1 1 calc R . .
H44C H 0.6698 0.6723 0.5979 0.033 Uiso 1 1 calc R . .
Cl1 Cl 0.29902(19) 0.14370(14) 0.76267(11) 0.0406(5) Uani 1 1 d . . .
Cl2 Cl 0.3664(2) 0.09150(17) 0.59466(12) 0.0529(6) Uani 1 1 d . . .
Cl3 Cl 0.34662(17) -0.07316(12) 0.70303(10) 0.0319(4) Uani 1 1 d . . .
C89 C 0.2844(6) 0.0636(5) 0.6887(4) 0.0252(14) Uani 1 1 d . . .
H89 H 0.1889 0.0806 0.6899 0.030 Uiso 1 1 calc R . .
Cl7 Cl 0.9059(3) -0.0032(2) 0.1069(3) 0.1242(18) Uani 1 1 d . . .
Cl8 Cl 0.7246(4) 0.1144(4) 0.0210(2) 0.1320(19) Uani 1 1 d . . .
Cl9 Cl 0.87768(19) 0.21756(15) 0.08327(12) 0.0425(5) Uani 1 1 d . . .
C91 C 0.7968(10) 0.1225(7) 0.0973(6) 0.066(3) Uani 1 1 d . . .
H91 H 0.7260 0.1432 0.1474 0.079 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C7 1.222(7) . ?
O2 C16 1.231(7) . ?
O3 C25 1.206(6) . ?
O4 C26 1.217(7) . ?
O5 C28 1.188(7) . ?
O6 C28 1.320(7) . ?
O6 C29 1.454(7) . ?
O7 C32 1.196(7) . ?
O8 C32 1.318(7) . ?
O8 C33 1.470(6) . ?
O9 C39 1.367(7) . ?
O9 C43 1.430(7) . ?
O10 C42 1.378(7) . ?
O10 C44 1.417(7) . ?
N1 C7 1.351(7) . ?
N1 C8 1.434(7) . ?
N1 H1A 0.8800 . ?
N2 C16 1.353(7) . ?
N2 C11 1.437(7) . ?
N2 H2A 0.8800 . ?
N3 C25 1.382(7) . ?
N3 C27 1.450(7) . ?
N3 C23 1.464(6) . ?
N4 C26 1.379(7) . ?
N4 C27 1.439(7) . ?
N4 C24 1.468(6) . ?
N5 C25 1.377(6) . ?
N5 C31 1.445(7) . ?
N5 C35 1.455(7) . ?
N6 C26 1.367(7) . ?
N6 C31 1.445(7) . ?
N6 C36 1.466(7) . ?
C1 C6 1.359(8) . ?
C1 C2 1.371(9) . ?
C1 H1 0.9500 . ?
C2 C3 1.394(8) . ?
C2 H2 0.9500 . ?
C3 C4 1.382(8) . ?
C3 C7 1.504(8) . ?
C4 C5 1.386(9) . ?
C4 H4 0.9500 . ?
C5 C6 1.355(9) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C8 C9 1.387(8) . ?
C8 C13 1.393(8) . ?
C9 C10 1.399(8) . ?
C9 C23 1.515(8) . ?
C10 C11 1.394(8) . ?
C10 C24 1.518(7) . ?
C11 C12 1.398(8) . ?
C12 C13 1.411(8) . ?
C12 C14 1.512(8) . ?
C13 C15 1.506(8) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.493(8) . ?
C17 C18 1.385(9) . ?
C17 C22 1.392(9) . ?
C18 C19 1.386(10) . ?
C18 H18 0.9500 . ?
C19 C20 1.344(12) . ?
C19 H19 0.9500 . ?
C20 C21 1.342(10) . ?
C20 H20 0.9500 . ?
C21 C22 1.375(9) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C27 C28 1.557(8) . ?
C27 C31 1.576(7) . ?
C29 C30 1.484(10) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.549(7) . ?
C33 C34 1.504(9) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 C37 1.519(8) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 C38 1.526(8) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 C38 1.390(8) . ?
C37 C42 1.408(8) . ?
C38 C39 1.420(8) . ?
C39 C40 1.379(8) . ?
C40 C41 1.384(8) . ?
C40 H40 0.9500 . ?
C41 C42 1.377(8) . ?
C41 H41 0.9500 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
Cl1 C89 1.747(7) . ?
Cl2 C89 1.767(7) . ?
Cl3 C89 1.762(6) . ?
C89 H89 1.0000 . ?
Cl7 C91 1.758(12) . ?
Cl8 C91 1.721(12) . ?
Cl9 C91 1.732(8) . ?
C91 H91 1.0000 . ?

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
C28 O6 C29 118.5(5) . . ?
C32 O8 C33 116.2(4) . . ?
C39 O9 C43 116.8(5) . . ?
C42 O10 C44 117.6(5) . . ?
C7 N1 C8 126.0(5) . . ?
C7 N1 H1A 117.0 . . ?
C8 N1 H1A 117.0 . . ?
C16 N2 C11 124.0(4) . . ?
C16 N2 H2A 118.0 . . ?
C11 N2 H2A 118.0 . . ?
C25 N3 C27 113.0(4) . . ?
C25 N3 C23 121.2(4) . . ?
C27 N3 C23 120.8(4) . . ?
C26 N4 C27 112.3(4) . . ?
C26 N4 C24 120.0(4) . . ?
C27 N4 C24 121.0(4) . . ?
C25 N5 C31 112.3(4) . . ?
C25 N5 C35 122.2(4) . . ?
C31 N5 C35 122.7(4) . . ?
C26 N6 C31 113.3(4) . . ?
C26 N6 C36 123.6(4) . . ?
C31 N6 C36 121.8(4) . . ?
C6 C1 C2 122.7(6) . . ?
C6 C1 H1 118.7 . . ?
C2 C1 H1 118.7 . . ?
C1 C2 C3 119.1(5) . . ?
C1 C2 H2 120.4 . . ?
C3 C2 H2 120.4 . . ?
C4 C3 C2 118.6(5) . . ?
C4 C3 C7 118.0(5) . . ?
C2 C3 C7 123.3(5) . . ?
C3 C4 C5 119.7(5) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
C6 C5 C4 121.8(5) . . ?
C6 C5 H5 119.1 . . ?
C4 C5 H5 119.1 . . ?
C5 C6 C1 118.1(6) . . ?
C5 C6 H6 121.0 . . ?
C1 C6 H6 121.0 . . ?
O1 C7 N1 122.5(5) . . ?
O1 C7 C3 121.9(5) . . ?
N1 C7 C3 115.5(5) . . ?
C9 C8 C13 122.3(5) . . ?
C9 C8 N1 117.2(5) . . ?
C13 C8 N1 120.1(5) . . ?
C8 C9 C10 119.5(5) . . ?
C8 C9 C23 121.3(5) . . ?
C10 C9 C23 119.0(5) . . ?
C11 C10 C9 118.7(5) . . ?
C11 C10 C24 122.7(5) . . ?
C9 C10 C24 118.5(5) . . ?
C10 C11 C12 122.0(5) . . ?
C10 C11 N2 117.8(5) . . ?
C12 C11 N2 120.2(5) . . ?
C11 C12 C13 119.0(5) . . ?
C11 C12 C14 121.5(5) . . ?
C13 C12 C14 119.1(5) . . ?
C8 C13 C12 118.4(5) . . ?
C8 C13 C15 121.7(5) . . ?
C12 C13 C15 119.7(5) . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O2 C16 N2 121.2(5) . . ?
O2 C16 C17 121.8(5) . . ?
N2 C16 C17 117.0(5) . . ?
C18 C17 C22 118.3(6) . . ?
C18 C17 C16 123.4(5) . . ?
C22 C17 C16 118.2(5) . . ?
C17 C18 C19 119.1(7) . . ?
C17 C18 H18 120.5 . . ?
C19 C18 H18 120.5 . . ?
C20 C19 C18 122.4(7) . . ?
C20 C19 H19 118.8 . . ?
C18 C19 H19 118.8 . . ?
C21 C20 C19 118.4(6) . . ?
C21 C20 H20 120.8 . . ?
C19 C20 H20 120.8 . . ?
C20 C21 C22 122.4(6) . . ?
C20 C21 H21 118.8 . . ?
C22 C21 H21 118.8 . . ?
C21 C22 C17 119.4(6) . . ?
C21 C22 H22 120.3 . . ?
C17 C22 H22 120.3 . . ?
N3 C23 C9 110.7(4) . . ?
N3 C23 H23A 109.5 . . ?
C9 C23 H23A 109.5 . . ?
N3 C23 H23B 109.5 . . ?
C9 C23 H23B 109.5 . . ?
H23A C23 H23B 108.1 . . ?
N4 C24 C10 112.4(4) . . ?
N4 C24 H24A 109.1 . . ?
C10 C24 H24A 109.1 . . ?
N4 C24 H24B 109.1 . . ?
C10 C24 H24B 109.1 . . ?
H24A C24 H24B 107.9 . . ?
O3 C25 N5 127.5(5) . . ?
O3 C25 N3 125.4(5) . . ?
N5 C25 N3 107.0(4) . . ?
O4 C26 N6 126.8(5) . . ?
O4 C26 N4 125.4(5) . . ?
N6 C26 N4 107.7(5) . . ?
N4 C27 N3 115.1(4) . . ?
N4 C27 C28 111.4(5) . . ?
N3 C27 C28 109.3(4) . . ?
N4 C27 C31 103.3(4) . . ?
N3 C27 C31 102.1(4) . . ?
C28 C27 C31 115.3(4) . . ?
O5 C28 O6 126.8(5) . . ?
O5 C28 C27 124.6(5) . . ?
O6 C28 C27 108.5(5) . . ?
O6 C29 C30 105.8(5) . . ?
O6 C29 H29A 110.6 . . ?
C30 C29 H29A 110.6 . . ?
O6 C29 H29B 110.6 . . ?
C30 C29 H29B 110.6 . . ?
H29A C29 H29B 108.7 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N5 C31 N6 112.6(4) . . ?
N5 C31 C32 114.3(4) . . ?
N6 C31 C32 111.6(4) . . ?
N5 C31 C27 103.5(4) . . ?
N6 C31 C27 102.4(4) . . ?
C32 C31 C27 111.5(4) . . ?
O7 C32 O8 126.6(5) . . ?
O7 C32 C31 121.0(5) . . ?
O8 C32 C31 112.3(4) . . ?
O8 C33 C34 107.3(5) . . ?
O8 C33 H33A 110.3 . . ?
C34 C33 H33A 110.3 . . ?
O8 C33 H33B 110.3 . . ?
C34 C33 H33B 110.3 . . ?
H33A C33 H33B 108.5 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N5 C35 C37 115.4(4) . . ?
N5 C35 H35A 108.4 . . ?
C37 C35 H35A 108.4 . . ?
N5 C35 H35B 108.4 . . ?
C37 C35 H35B 108.4 . . ?
H35A C35 H35B 107.5 . . ?
N6 C36 C38 115.4(4) . . ?
N6 C36 H36A 108.4 . . ?
C38 C36 H36A 108.4 . . ?
N6 C36 H36B 108.4 . . ?
C38 C36 H36B 108.4 . . ?
H36A C36 H36B 107.5 . . ?
C38 C37 C42 119.9(5) . . ?
C38 C37 C35 122.0(5) . . ?
C42 C37 C35 118.0(5) . . ?
C37 C38 C39 119.0(5) . . ?
C37 C38 C36 122.5(5) . . ?
C39 C38 C36 118.4(5) . . ?
O9 C39 C40 123.6(5) . . ?
O9 C39 C38 116.7(5) . . ?
C40 C39 C38 119.7(5) . . ?
C39 C40 C41 121.2(5) . . ?
C39 C40 H40 119.4 . . ?
C41 C40 H40 119.4 . . ?
C42 C41 C40 119.7(5) . . ?
C42 C41 H41 120.2 . . ?
C40 C41 H41 120.2 . . ?
C41 C42 O10 123.6(5) . . ?
C41 C42 C37 120.5(5) . . ?
O10 C42 C37 115.8(5) . . ?
O9 C43 H43A 109.5 . . ?
O9 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
O9 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
O10 C44 H44A 109.5 . . ?
O10 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
O10 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
Cl1 C89 Cl3 112.1(4) . . ?
Cl1 C89 Cl2 110.4(3) . . ?
Cl3 C89 Cl2 109.5(4) . . ?
Cl1 C89 H89 108.2 . . ?
Cl3 C89 H89 108.2 . . ?
Cl2 C89 H89 108.2 . . ?
Cl8 C91 Cl9 111.8(6) . . ?
Cl8 C91 Cl7 109.5(5) . . ?
Cl9 C91 Cl7 110.6(6) . . ?
Cl8 C91 H91 108.3 . . ?
Cl9 C91 H91 108.3 . . ?
Cl7 C91 H91 108.3 . . ?

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
C6 C1 C2 C3 -1.2(10) . . . . ?
C1 C2 C3 C4 1.5(9) . . . . ?
C1 C2 C3 C7 -180.0(6) . . . . ?
C2 C3 C4 C5 -1.5(9) . . . . ?
C7 C3 C4 C5 179.9(6) . . . . ?
C3 C4 C5 C6 1.1(11) . . . . ?
C4 C5 C6 C1 -0.8(11) . . . . ?
C2 C1 C6 C5 0.8(11) . . . . ?
C8 N1 C7 O1 5.6(9) . . . . ?
C8 N1 C7 C3 -175.7(5) . . . . ?
C4 C3 C7 O1 15.8(9) . . . . ?
C2 C3 C7 O1 -162.7(6) . . . . ?
C4 C3 C7 N1 -162.8(5) . . . . ?
C2 C3 C7 N1 18.6(8) . . . . ?
C7 N1 C8 C9 111.8(6) . . . . ?
C7 N1 C8 C13 -75.1(7) . . . . ?
C13 C8 C9 C10 -3.3(8) . . . . ?
N1 C8 C9 C10 169.7(5) . . . . ?
C13 C8 C9 C23 -179.2(5) . . . . ?
N1 C8 C9 C23 -6.2(7) . . . . ?
C8 C9 C10 C11 0.2(7) . . . . ?
C23 C9 C10 C11 176.2(5) . . . . ?
C8 C9 C10 C24 -176.0(5) . . . . ?
C23 C9 C10 C24 0.0(7) . . . . ?
C9 C10 C11 C12 2.5(8) . . . . ?
C24 C10 C11 C12 178.5(5) . . . . ?
C9 C10 C11 N2 -174.3(5) . . . . ?
C24 C10 C11 N2 1.8(7) . . . . ?
C16 N2 C11 C10 -115.2(6) . . . . ?
C16 N2 C11 C12 68.0(7) . . . . ?
C10 C11 C12 C13 -2.1(8) . . . . ?
N2 C11 C12 C13 174.6(5) . . . . ?
C10 C11 C12 C14 -175.3(5) . . . . ?
N2 C11 C12 C14 1.3(8) . . . . ?
C9 C8 C13 C12 3.6(8) . . . . ?
N1 C8 C13 C12 -169.1(5) . . . . ?
C9 C8 C13 C15 178.9(5) . . . . ?
N1 C8 C13 C15 6.1(8) . . . . ?
C11 C12 C13 C8 -1.0(8) . . . . ?
C14 C12 C13 C8 172.5(5) . . . . ?
C11 C12 C13 C15 -176.3(5) . . . . ?
C14 C12 C13 C15 -2.9(7) . . . . ?
C11 N2 C16 O2 -6.8(9) . . . . ?
C11 N2 C16 C17 172.5(5) . . . . ?
O2 C16 C17 C18 158.9(6) . . . . ?
N2 C16 C17 C18 -20.3(9) . . . . ?
O2 C16 C17 C22 -17.7(9) . . . . ?
N2 C16 C17 C22 163.0(5) . . . . ?
C22 C17 C18 C19 -0.2(10) . . . . ?
C16 C17 C18 C19 -176.9(7) . . . . ?
C17 C18 C19 C20 -0.4(13) . . . . ?
C18 C19 C20 C21 0.1(13) . . . . ?
C19 C20 C21 C22 0.7(12) . . . . ?
C20 C21 C22 C17 -1.3(11) . . . . ?
C18 C17 C22 C21 1.0(9) . . . . ?
C16 C17 C22 C21 177.8(6) . . . . ?
C25 N3 C23 C9 -72.2(6) . . . . ?
C27 N3 C23 C9 80.9(6) . . . . ?
C8 C9 C23 N3 108.8(5) . . . . ?
C10 C9 C23 N3 -67.1(6) . . . . ?
C26 N4 C24 C10 71.1(6) . . . . ?
C27 N4 C24 C10 -77.9(6) . . . . ?
C11 C10 C24 N4 -109.4(6) . . . . ?
C9 C10 C24 N4 66.7(6) . . . . ?
C31 N5 C25 O3 167.5(5) . . . . ?
C35 N5 C25 O3 6.2(8) . . . . ?
C31 N5 C25 N3 -14.9(6) . . . . ?
C35 N5 C25 N3 -176.2(4) . . . . ?
C27 N3 C25 O3 -168.1(5) . . . . ?
C23 N3 C25 O3 -13.0(8) . . . . ?
C27 N3 C25 N5 14.3(6) . . . . ?
C23 N3 C25 N5 169.4(4) . . . . ?
C31 N6 C26 O4 -172.2(5) . . . . ?
C36 N6 C26 O4 -5.5(8) . . . . ?
C31 N6 C26 N4 8.3(6) . . . . ?
C36 N6 C26 N4 174.9(4) . . . . ?
C27 N4 C26 O4 169.5(5) . . . . ?
C24 N4 C26 O4 18.0(8) . . . . ?
C27 N4 C26 N6 -10.9(6) . . . . ?
C24 N4 C26 N6 -162.4(4) . . . . ?
C26 N4 C27 N3 -101.5(5) . . . . ?
C24 N4 C27 N3 49.7(7) . . . . ?
C26 N4 C27 C28 133.3(4) . . . . ?
C24 N4 C27 C28 -75.5(6) . . . . ?
C26 N4 C27 C31 8.9(6) . . . . ?
C24 N4 C27 C31 160.1(5) . . . . ?
C25 N3 C27 N4 103.2(5) . . . . ?
C23 N3 C27 N4 -52.0(7) . . . . ?
C25 N3 C27 C28 -130.6(5) . . . . ?
C23 N3 C27 C28 74.2(6) . . . . ?
C25 N3 C27 C31 -8.0(5) . . . . ?
C23 N3 C27 C31 -163.2(4) . . . . ?
C29 O6 C28 O5 1.8(8) . . . . ?
C29 O6 C28 C27 -176.5(4) . . . . ?
N4 C27 C28 O5 1.9(7) . . . . ?
N3 C27 C28 O5 -126.5(6) . . . . ?
C31 C27 C28 O5 119.2(6) . . . . ?
N4 C27 C28 O6 -179.7(4) . . . . ?
N3 C27 C28 O6 51.9(5) . . . . ?
C31 C27 C28 O6 -62.4(6) . . . . ?
C28 O6 C29 C30 161.1(6) . . . . ?
C25 N5 C31 N6 -100.1(5) . . . . ?
C35 N5 C31 N6 61.1(6) . . . . ?
C25 N5 C31 C32 131.3(5) . . . . ?
C35 N5 C31 C32 -67.6(6) . . . . ?
C25 N5 C31 C27 9.7(6) . . . . ?
C35 N5 C31 C27 170.9(4) . . . . ?
C26 N6 C31 N5 107.9(5) . . . . ?
C36 N6 C31 N5 -59.1(6) . . . . ?
C26 N6 C31 C32 -122.0(5) . . . . ?
C36 N6 C31 C32 71.0(6) . . . . ?
C26 N6 C31 C27 -2.6(6) . . . . ?
C36 N6 C31 C27 -169.6(4) . . . . ?
N4 C27 C31 N5 -120.8(4) . . . . ?
N3 C27 C31 N5 -1.0(5) . . . . ?
C28 C27 C31 N5 117.4(5) . . . . ?
N4 C27 C31 N6 -3.7(5) . . . . ?
N3 C27 C31 N6 116.2(4) . . . . ?
C28 C27 C31 N6 -125.4(5) . . . . ?
N4 C27 C31 C32 115.8(5) . . . . ?
N3 C27 C31 C32 -124.4(4) . . . . ?
C28 C27 C31 C32 -6.0(6) . . . . ?
C33 O8 C32 O7 0.5(8) . . . . ?
C33 O8 C32 C31 -175.0(4) . . . . ?
N5 C31 C32 O7 177.6(5) . . . . ?
N6 C31 C32 O7 48.4(7) . . . . ?
C27 C31 C32 O7 -65.4(6) . . . . ?
N5 C31 C32 O8 -6.6(6) . . . . ?
N6 C31 C32 O8 -135.8(5) . . . . ?
C27 C31 C32 O8 110.4(5) . . . . ?
C32 O8 C33 C34 167.3(5) . . . . ?
C25 N5 C35 C37 84.0(6) . . . . ?
C31 N5 C35 C37 -75.4(6) . . . . ?
C26 N6 C36 C38 -91.9(6) . . . . ?
C31 N6 C36 C38 73.7(6) . . . . ?
N5 C35 C37 C38 52.8(6) . . . . ?
N5 C35 C37 C42 -129.5(5) . . . . ?
C42 C37 C38 C39 0.9(7) . . . . ?
C35 C37 C38 C39 178.5(5) . . . . ?
C42 C37 C38 C36 -174.4(4) . . . . ?
C35 C37 C38 C36 3.2(7) . . . . ?
N6 C36 C38 C37 -57.0(7) . . . . ?
N6 C36 C38 C39 127.6(5) . . . . ?
C43 O9 C39 C40 -2.6(7) . . . . ?
C43 O9 C39 C38 176.9(5) . . . . ?
C37 C38 C39 O9 180.0(4) . . . . ?
C36 C38 C39 O9 -4.5(7) . . . . ?
C37 C38 C39 C40 -0.5(7) . . . . ?
C36 C38 C39 C40 175.0(5) . . . . ?
O9 C39 C40 C41 179.1(5) . . . . ?
C38 C39 C40 C41 -0.3(8) . . . . ?
C39 C40 C41 C42 0.8(8) . . . . ?
C40 C41 C42 O10 179.0(5) . . . . ?
C40 C41 C42 C37 -0.4(8) . . . . ?
C44 O10 C42 C41 -1.2(7) . . . . ?
C44 O10 C42 C37 178.2(5) . . . . ?
C38 C37 C42 C41 -0.5(7) . . . . ?
C35 C37 C42 C41 -178.1(5) . . . . ?
C38 C37 C42 O10 -179.9(4) . . . . ?
C35 C37 C42 O10 2.5(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         1.700
_refine_diff_density_min         -1.183
_refine_diff_density_rms         0.133

# start Validation Reply Form
_vrf_PLAT211_3                   
;
PROBLEM: ADP of Atom C37     is N.P.D. or (nearly) 2D ...     Please Check   
RESPONSE: Although we have re-tried several times to selected 
better crystals for x-ray diffraction experiment and the 
command ISOR was also used in the refinement for isotropic treatment,
we are failed each time for this level A Alert. This may be resulted 
from the weak diffraction ability for such a small crystal. 
;
# end Validation Reply Form

#==END
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4
_database_code_depnum_ccdc_archive 'CCDC 992392'
_audit_update_record             
;
2014-03-18 deposited with the CCDC.
2015-02-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C45 H39 Cl3 N4 O8'
_chemical_formula_weight         870.15

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'
O O 0.0106 0.0060 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   11.1774(14)
_cell_length_b                   13.9112(18)
_cell_length_c                   26.663(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.601(2)
_cell_angle_gamma                90.00
_cell_volume                     4109.4(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    220(2)
_cell_measurement_reflns_used    2579
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      16.14

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      1.406
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1808
_exptl_absorpt_coefficient_mu    0.284
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  0.9560
_exptl_absorpt_correction_T_max  0.9722
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      220(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9219
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_sigmaI/netI    0.0305
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.54
_diffrn_reflns_theta_max         16.19
_reflns_number_total             2050
_reflns_number_gt                1700
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0547P)²+6.4915P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2050
_refine_ls_number_parameters     553
_refine_ls_number_restraints     77
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0381
_refine_ls_wR_factor_ref         0.1040
_refine_ls_wR_factor_gt          0.0987
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6161(7) 0.2801(7) 0.7755(3) 0.034(2) Uani 1 1 d . . .
C2 C 0.5068(8) 0.2985(6) 0.7461(3) 0.049(2) Uani 1 1 d U . .
H2 H 0.4749 0.3611 0.7456 0.059 Uiso 1 1 calc R . .
C3 C 0.4439(7) 0.2286(6) 0.7177(3) 0.057(2) Uani 1 1 d U . .
H3 H 0.3709 0.2434 0.6974 0.068 Uiso 1 1 calc R . .
C4 C 0.4882(7) 0.1368(6) 0.7192(3) 0.054(2) Uani 1 1 d U . .
H4 H 0.4461 0.0885 0.6994 0.064 Uiso 1 1 calc R . .
C5 C 0.5926(7) 0.1151(5) 0.7490(3) 0.042(2) Uani 1 1 d U . .
H5 H 0.6214 0.0515 0.7505 0.051 Uiso 1 1 calc R . .
C6 C 0.6569(6) 0.1862(6) 0.7771(2) 0.036(2) Uani 1 1 d U . .
H6 H 0.7293 0.1705 0.7975 0.043 Uiso 1 1 calc R . .
C7 C 0.6820(8) 0.3554(7) 0.8043(3) 0.036(2) Uani 1 1 d . . .
C8 C 0.7319(8) 0.4163(8) 0.8290(4) 0.028(2) Uani 1 1 d U . .
C9 C 0.7909(9) 0.4907(9) 0.8594(3) 0.026(2) Uani 1 1 d . . .
C10 C 0.7537(7) 0.5874(9) 0.8550(3) 0.0235(19) Uani 1 1 d . . .
C11 C 0.8176(8) 0.6584(7) 0.8845(3) 0.0204(19) Uani 1 1 d . . .
C12 C 0.9174(8) 0.6317(7) 0.9192(3) 0.0220(19) Uani 1 1 d U . .
C13 C 0.9525(7) 0.5365(8) 0.9240(3) 0.037(2) Uani 1 1 d . . .
H13 H 1.0190 0.5192 0.9476 0.044 Uiso 1 1 calc R . .
C14 C 0.8909(10) 0.4670(6) 0.8945(4) 0.035(2) Uani 1 1 d . . .
H14 H 0.9163 0.4027 0.8979 0.042 Uiso 1 1 calc R . .
C15 C 0.9874(8) 0.7008(7) 0.9495(3) 0.028(2) Uani 1 1 d U . .
C16 C 1.0507(8) 0.7553(7) 0.9756(4) 0.031(2) Uani 1 1 d . . .
C17 C 1.1251(8) 0.8243(10) 1.0053(4) 0.026(2) Uani 1 1 d . . .
C18 C 1.1229(8) 0.9212(13) 0.9947(3) 0.043(2) Uani 1 1 d . . .
H18 H 1.0711 0.9441 0.9666 0.051 Uiso 1 1 calc R . .
C19 C 1.1945(14) 0.9850(7) 1.0242(6) 0.054(3) Uani 1 1 d . . .
H19 H 1.1914 1.0508 1.0163 0.065 Uiso 1 1 calc R . .
C20 C 1.2720(9) 0.9518(13) 1.0659(5) 0.056(3) Uani 1 1 d . . .
H20 H 1.3215 0.9951 1.0861 0.067 Uiso 1 1 calc R . .
C21 C 1.2755(9) 0.8556(14) 1.0772(3) 0.044(2) Uani 1 1 d . . .
H21 H 1.3275 0.8326 1.1052 0.053 Uiso 1 1 calc R . .
C22 C 1.2029(12) 0.7933(6) 1.0473(6) 0.037(2) Uani 1 1 d . . .
H22 H 1.2057 0.7275 1.0554 0.044 Uiso 1 1 calc R . .
C23 C 0.6471(8) 0.6122(5) 0.8160(3) 0.0294(19) Uani 1 1 d . . .
H23A H 0.6755 0.6520 0.7896 0.035 Uiso 1 1 calc R . .
H23B H 0.6142 0.5527 0.8000 0.035 Uiso 1 1 calc R . .
C24 C 0.7838(7) 0.7624(6) 0.8775(2) 0.0273(19) Uani 1 1 d . . .
H24A H 0.8408 0.8006 0.9005 0.033 Uiso 1 1 calc R . .
H24B H 0.7941 0.7810 0.8429 0.033 Uiso 1 1 calc R . .
C25 C 0.4456(10) 0.6190(9) 0.8470(3) 0.022(2) Uani 1 1 d . . .
C26 C 0.6290(11) 0.7851(4) 0.9343(5) 0.022(2) Uani 1 1 d . . .
C27 C 0.5595(8) 0.7629(7) 0.8495(4) 0.0181(18) Uani 1 1 d . . .
C28 C 0.5577(9) 0.8254(6) 0.8012(3) 0.033(2) Uani 1 1 d . A .
C31 C 0.4474(8) 0.7759(7) 0.8784(3) 0.0179(18) Uani 1 1 d . . .
C32 C 0.3701(11) 0.8676(6) 0.8660(2) 0.025(2) Uani 1 1 d . . .
C33 C 0.3970(6) 1.0386(6) 0.8661(3) 0.045(2) Uani 1 1 d . . .
H33A H 0.3216 1.0408 0.8427 0.054 Uiso 1 1 calc R . .
H33B H 0.4537 1.0847 0.8544 0.054 Uiso 1 1 calc R . .
C34 C 0.3735(7) 1.0640(5) 0.9186(3) 0.070(3) Uani 1 1 d . . .
H34A H 0.3145 1.0198 0.9293 0.105 Uiso 1 1 calc R . .
H34B H 0.3425 1.1291 0.9189 0.105 Uiso 1 1 calc R . .
H34C H 0.4480 1.0594 0.9417 0.105 Uiso 1 1 calc R . .
C35 C 0.2870(6) 0.6587(5) 0.8987(3) 0.0251(19) Uani 1 1 d . . .
H35A H 0.2384 0.6080 0.8804 0.030 Uiso 1 1 calc R . .
H35B H 0.2331 0.7131 0.9023 0.030 Uiso 1 1 calc R . .
C36 C 0.4377(7) 0.7799(6) 0.9726(3) 0.0276(19) Uani 1 1 d . . .
H36A H 0.3645 0.8188 0.9647 0.033 Uiso 1 1 calc R . .
H36B H 0.4863 0.8085 1.0021 0.033 Uiso 1 1 calc R . .
C37 C 0.3324(9) 0.6215(12) 0.9509(4) 0.022(2) Uani 1 1 d . . .
C38 C 0.4025(10) 0.6792(7) 0.9856(6) 0.024(2) Uani 1 1 d . . .
C39 C 0.4405(7) 0.6443(11) 1.0340(6) 0.031(2) Uani 1 1 d . . .
C40 C 0.4096(10) 0.5536(12) 1.0489(4) 0.030(2) Uani 1 1 d . . .
H40 H 0.4348 0.5314 1.0819 0.036 Uiso 1 1 calc R . .
C41 C 0.3412(10) 0.4970(6) 1.0143(7) 0.032(2) Uani 1 1 d . . .
H41 H 0.3190 0.4352 1.0238 0.038 Uiso 1 1 calc R . .
C42 C 0.3042(7) 0.5287(11) 0.9657(5) 0.026(2) Uani 1 1 d . . .
C43 C 0.5496(6) 0.6746(5) 1.1163(3) 0.045(2) Uani 1 1 d . . .
H43A H 0.4808 0.6579 1.1332 0.068 Uiso 1 1 calc R . .
H43B H 0.5950 0.7258 1.1347 0.068 Uiso 1 1 calc R . .
H43C H 0.6011 0.6188 1.1151 0.068 Uiso 1 1 calc R . .
C44 C 0.2012(6) 0.3784(5) 0.9436(3) 0.042(2) Uani 1 1 d . . .
H44A H 0.2731 0.3407 0.9542 0.063 Uiso 1 1 calc R . .
H44B H 0.1546 0.3479 0.9146 0.063 Uiso 1 1 calc R . .
H44C H 0.1528 0.3826 0.9711 0.063 Uiso 1 1 calc R . .
C45 C 0.0395(6) 0.0378(5) 0.8418(2) 0.051(2) Uani 1 1 d . . .
H45 H 0.0944 -0.0152 0.8546 0.062 Uiso 1 1 calc R . .
Cl1 Cl 0.08757(18) 0.08302(17) 0.78689(7) 0.0788(8) Uani 1 1 d . . .
Cl2 Cl -0.10639(19) -0.00873(15) 0.82884(9) 0.0830(8) Uani 1 1 d . . .
Cl3 Cl 0.0459(2) 0.12621(18) 0.88891(9) 0.0964(9) Uani 1 1 d . . .
N1 N 0.5506(8) 0.6632(6) 0.83648(19) 0.0197(15) Uani 1 1 d . . .
N2 N 0.6621(7) 0.7882(3) 0.8861(4) 0.0214(16) Uani 1 1 d . . .
N3 N 0.3772(6) 0.6896(6) 0.8676(2) 0.0191(15) Uani 1 1 d . . .
N4 N 0.5061(9) 0.7827(3) 0.9297(3) 0.0211(15) Uani 1 1 d . . .
O1 O 0.4171(4) 0.5365(4) 0.83866(16) 0.0329(16) Uani 1 1 d . . .
O2 O 0.6984(5) 0.7878(3) 0.9737(2) 0.0335(16) Uani 1 1 d . . .
O3 O 0.6365(5) 0.8761(4) 0.79191(18) 0.0479(17) Uani 1 1 d . . .
O4 O 0.4529(6) 0.8107(3) 0.7728(2) 0.0409(14) Uani 1 1 d D . .
O5 O 0.2630(6) 0.8722(4) 0.85887(17) 0.0394(17) Uani 1 1 d . . .
O6 O 0.4479(4) 0.9422(5) 0.86742(15) 0.0338(13) Uani 1 1 d . . .
O7 O 0.5087(5) 0.7059(4) 1.0663(3) 0.0355(13) Uani 1 1 d . . .
O8 O 0.2355(5) 0.4734(5) 0.9298(2) 0.0358(13) Uani 1 1 d . . .
C29 C 0.434(2) 0.853(2) 0.7213(9) 0.053(4) Uani 0.49(5) 1 d PDU A 1
H29A H 0.4339 0.8027 0.6955 0.064 Uiso 0.49(5) 1 calc PR A 1
H29B H 0.4976 0.8995 0.7169 0.064 Uiso 0.49(5) 1 calc PR A 1
C30 C 0.3113(17) 0.902(3) 0.7174(10) 0.055(4) Uani 0.49(5) 1 d PDU A 1
H30A H 0.2503 0.8555 0.7234 0.082 Uiso 0.49(5) 1 calc PR A 1
H30B H 0.2914 0.9294 0.6838 0.082 Uiso 0.49(5) 1 calc PR A 1
H30C H 0.3141 0.9529 0.7425 0.082 Uiso 0.49(5) 1 calc PR A 1
C29' C 0.4330(19) 0.872(2) 0.7278(9) 0.053(4) Uani 0.51(5) 1 d PDU A 2
H29C H 0.4840 0.8503 0.7027 0.064 Uiso 0.51(5) 1 calc PR A 2
H29D H 0.4542 0.9385 0.7369 0.064 Uiso 0.51(5) 1 calc PR A 2
C30' C 0.3047(13) 0.866(3) 0.7063(9) 0.055(4) Uani 0.51(5) 1 d PDU A 2
H30D H 0.2812 0.7989 0.7022 0.082 Uiso 0.51(5) 1 calc PR A 2
H30E H 0.2929 0.8976 0.6736 0.082 Uiso 0.51(5) 1 calc PR A 2
H30F H 0.2557 0.8970 0.7289 0.082 Uiso 0.51(5) 1 calc PR A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C6 1.383(9) . ?
C1 C2 1.385(9) . ?
C1 C7 1.442(12) . ?
C2 C3 1.369(9) . ?
C2 H2 0.9400 . ?
C3 C4 1.368(9) . ?
C3 H3 0.9400 . ?
C4 C5 1.356(9) . ?
C4 H4 0.9400 . ?
C5 C6 1.384(8) . ?
C5 H5 0.9400 . ?
C6 H6 0.9400 . ?
C7 C8 1.169(10) . ?
C8 C9 1.422(12) . ?
C9 C14 1.398(9) . ?
C9 C10 1.409(9) . ?
C10 C11 1.398(8) . ?
C10 C23 1.514(9) . ?
C11 C12 1.402(9) . ?
C11 C24 1.501(9) . ?
C12 C13 1.382(9) . ?
C12 C15 1.423(11) . ?
C13 C14 1.372(8) . ?
C13 H13 0.9400 . ?
C14 H14 0.9400 . ?
C15 C16 1.196(10) . ?
C16 C17 1.436(12) . ?
C17 C18 1.377(10) . ?
C17 C22 1.393(10) . ?
C18 C19 1.371(10) . ?
C18 H18 0.9400 . ?
C19 C20 1.394(10) . ?
C19 H19 0.9400 . ?
C20 C21 1.370(10) . ?
C20 H20 0.9400 . ?
C21 C22 1.368(9) . ?
C21 H21 0.9400 . ?
C22 H22 0.9400 . ?
C23 N1 1.456(8) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C24 N2 1.453(8) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C25 O1 1.204(9) . ?
C25 N1 1.387(9) . ?
C25 N3 1.401(9) . ?
C26 O2 1.222(9) . ?
C26 N4 1.364(9) . ?
C26 N2 1.383(9) . ?
C27 N1 1.430(8) . ?
C27 N2 1.448(8) . ?
C27 C28 1.552(10) . ?
C27 C31 1.567(8) . ?
C28 O3 1.180(8) . ?
C28 O4 1.324(8) . ?
C31 N4 1.439(8) . ?
C31 N3 1.442(8) . ?
C31 C32 1.552(10) . ?
C32 O5 1.189(9) . ?
C32 O6 1.351(9) . ?
C33 O6 1.455(7) . ?
C33 C34 1.502(9) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C34 H34C 0.9700 . ?
C35 N3 1.452(8) . ?
C35 C37 1.508(10) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C36 N4 1.457(8) . ?
C36 C38 1.507(10) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C37 C38 1.387(9) . ?
C37 C42 1.399(9) . ?
C38 C39 1.392(10) . ?
C39 O7 1.372(8) . ?
C39 C40 1.380(9) . ?
C40 C41 1.367(9) . ?
C40 H40 0.9400 . ?
C41 C42 1.378(10) . ?
C41 H41 0.9400 . ?
C42 O8 1.381(8) . ?
C43 O7 1.419(7) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C43 H43C 0.9700 . ?
C44 O8 1.437(7) . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C44 H44C 0.9700 . ?
C45 Cl1 1.743(7) . ?
C45 Cl2 1.746(7) . ?
C45 Cl3 1.752(7) . ?
C45 H45 0.9900 . ?
O4 C29' 1.464(16) . ?
O4 C29 1.483(17) . ?
C29 C30 1.525(18) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C30 H30C 0.9700 . ?
C29' C30' 1.474(17) . ?
C29' H29C 0.9800 . ?
C29' H29D 0.9800 . ?
C30' H30D 0.9700 . ?
C30' H30E 0.9700 . ?
C30' H30F 0.9700 . ?

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
C6 C1 C2 117.0(8) . . ?
C6 C1 C7 121.8(7) . . ?
C2 C1 C7 121.2(7) . . ?
C3 C2 C1 122.1(8) . . ?
C3 C2 H2 118.9 . . ?
C1 C2 H2 118.9 . . ?
C4 C3 C2 119.3(8) . . ?
C4 C3 H3 120.4 . . ?
C2 C3 H3 120.4 . . ?
C5 C4 C3 120.4(8) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C4 C5 C6 120.2(7) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C1 C6 C5 120.9(7) . . ?
C1 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?
C8 C7 C1 177.3(7) . . ?
C7 C8 C9 179.1(8) . . ?
C14 C9 C10 118.8(8) . . ?
C14 C9 C8 118.7(10) . . ?
C10 C9 C8 122.5(10) . . ?
C11 C10 C9 120.3(7) . . ?
C11 C10 C23 121.5(9) . . ?
C9 C10 C23 118.2(9) . . ?
C10 C11 C12 119.1(7) . . ?
C10 C11 C24 120.6(8) . . ?
C12 C11 C24 120.2(9) . . ?
C13 C12 C11 120.4(8) . . ?
C13 C12 C15 117.8(9) . . ?
C11 C12 C15 121.7(9) . . ?
C14 C13 C12 120.4(8) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C13 C14 C9 120.9(7) . . ?
C13 C14 H14 119.5 . . ?
C9 C14 H14 119.5 . . ?
C16 C15 C12 176.6(7) . . ?
C15 C16 C17 177.3(9) . . ?
C18 C17 C22 117.4(8) . . ?
C18 C17 C16 123.2(12) . . ?
C22 C17 C16 119.4(13) . . ?
C19 C18 C17 121.5(8) . . ?
C19 C18 H18 119.2 . . ?
C17 C18 H18 119.2 . . ?
C18 C19 C20 119.8(8) . . ?
C18 C19 H19 120.1 . . ?
C20 C19 H19 120.1 . . ?
C21 C20 C19 119.7(8) . . ?
C21 C20 H20 120.2 . . ?
C19 C20 H20 120.2 . . ?
C22 C21 C20 119.5(8) . . ?
C22 C21 H21 120.2 . . ?
C20 C21 H21 120.2 . . ?
C21 C22 C17 122.1(8) . . ?
C21 C22 H22 119.0 . . ?
C17 C22 H22 119.0 . . ?
N1 C23 C10 114.1(6) . . ?
N1 C23 H23A 108.7 . . ?
C10 C23 H23A 108.7 . . ?
N1 C23 H23B 108.7 . . ?
C10 C23 H23B 108.7 . . ?
H23A C23 H23B 107.6 . . ?
N2 C24 C11 116.4(5) . . ?
N2 C24 H24A 108.2 . . ?
C11 C24 H24A 108.2 . . ?
N2 C24 H24B 108.2 . . ?
C11 C24 H24B 108.2 . . ?
H24A C24 H24B 107.3 . . ?
O1 C25 N1 126.5(10) . . ?
O1 C25 N3 126.6(9) . . ?
N1 C25 N3 106.8(9) . . ?
O2 C26 N4 126.5(10) . . ?
O2 C26 N2 125.5(10) . . ?
N4 C26 N2 108.0(9) . . ?
N1 C27 N2 115.0(7) . . ?
N1 C27 C28 110.5(7) . . ?
N2 C27 C28 110.2(8) . . ?
N1 C27 C31 101.4(7) . . ?
N2 C27 C31 104.7(7) . . ?
C28 C27 C31 114.8(7) . . ?
O3 C28 O4 126.9(8) . . ?
O3 C28 C27 125.5(8) . . ?
O4 C28 C27 107.6(8) . . ?
N4 C31 N3 114.4(7) . . ?
N4 C31 C32 108.6(7) . . ?
N3 C31 C32 111.6(8) . . ?
N4 C31 C27 100.5(6) . . ?
N3 C31 C27 104.8(7) . . ?
C32 C31 C27 116.7(7) . . ?
O5 C32 O6 126.4(7) . . ?
O5 C32 C31 126.8(8) . . ?
O6 C32 C31 106.7(8) . . ?
O6 C33 C34 108.0(6) . . ?
O6 C33 H33A 110.1 . . ?
C34 C33 H33A 110.1 . . ?
O6 C33 H33B 110.1 . . ?
C34 C33 H33B 110.1 . . ?
H33A C33 H33B 108.4 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N3 C35 C37 117.0(6) . . ?
N3 C35 H35A 108.1 . . ?
C37 C35 H35A 108.1 . . ?
N3 C35 H35B 108.1 . . ?
C37 C35 H35B 108.1 . . ?
H35A C35 H35B 107.3 . . ?
N4 C36 C38 112.7(6) . . ?
N4 C36 H36A 109.1 . . ?
C38 C36 H36A 109.1 . . ?
N4 C36 H36B 109.1 . . ?
C38 C36 H36B 109.1 . . ?
H36A C36 H36B 107.8 . . ?
C38 C37 C42 118.3(8) . . ?
C38 C37 C35 120.6(13) . . ?
C42 C37 C35 121.1(14) . . ?
C37 C38 C39 119.6(8) . . ?
C37 C38 C36 121.7(13) . . ?
C39 C38 C36 118.7(14) . . ?
O7 C39 C40 122.0(15) . . ?
O7 C39 C38 116.1(15) . . ?
C40 C39 C38 121.9(8) . . ?
C41 C40 C39 118.1(8) . . ?
C41 C40 H40 120.9 . . ?
C39 C40 H40 120.9 . . ?
C40 C41 C42 121.4(8) . . ?
C40 C41 H41 119.3 . . ?
C42 C41 H41 119.3 . . ?
C41 C42 O8 122.9(15) . . ?
C41 C42 C37 120.7(8) . . ?
O8 C42 C37 116.3(14) . . ?
O7 C43 H43A 109.5 . . ?
O7 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
O7 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
O8 C44 H44A 109.5 . . ?
O8 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
O8 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
Cl1 C45 Cl2 110.5(4) . . ?
Cl1 C45 Cl3 111.2(4) . . ?
Cl2 C45 Cl3 110.5(4) . . ?
Cl1 C45 H45 108.2 . . ?
Cl2 C45 H45 108.2 . . ?
Cl3 C45 H45 108.2 . . ?
C25 N1 C27 114.5(7) . . ?
C25 N1 C23 123.3(8) . . ?
C27 N1 C23 122.1(8) . . ?
C26 N2 C27 109.4(7) . . ?
C26 N2 C24 120.6(8) . . ?
C27 N2 C24 120.5(7) . . ?
C25 N3 C31 110.6(7) . . ?
C25 N3 C35 118.1(8) . . ?
C31 N3 C35 122.2(7) . . ?
C26 N4 C31 114.4(7) . . ?
C26 N4 C36 123.9(8) . . ?
C31 N4 C36 121.5(8) . . ?
C28 O4 C29' 114.0(11) . . ?
C28 O4 C29 118.4(13) . . ?
C29' O4 C29 12(2) . . ?
C32 O6 C33 117.4(6) . . ?
C39 O7 C43 118.7(8) . . ?
C42 O8 C44 118.6(8) . . ?
O4 C29 C30 104.9(14) . . ?
O4 C29 H29A 110.8 . . ?
C30 C29 H29A 110.8 . . ?
O4 C29 H29B 110.8 . . ?
C30 C29 H29B 110.8 . . ?
H29A C29 H29B 108.8 . . ?
O4 C29' C30' 108.7(14) . . ?
O4 C29' H29C 109.9 . . ?
C30' C29' H29C 109.9 . . ?
O4 C29' H29D 109.9 . . ?
C30' C29' H29D 109.9 . . ?
H29C C29' H29D 108.3 . . ?
C29' C30' H30D 109.5 . . ?
C29' C30' H30E 109.5 . . ?
H30D C30' H30E 109.5 . . ?
C29' C30' H30F 109.5 . . ?
H30D C30' H30F 109.5 . . ?
H30E C30' H30F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -3.1(10) . . . . ?
C7 C1 C2 C3 178.8(6) . . . . ?
C1 C2 C3 C4 1.7(11) . . . . ?
C2 C3 C4 C5 0.9(11) . . . . ?
C3 C4 C5 C6 -1.8(10) . . . . ?
C2 C1 C6 C5 2.1(9) . . . . ?
C7 C1 C6 C5 -179.8(6) . . . . ?
C4 C5 C6 C1 0.2(10) . . . . ?
C6 C1 C7 C8 -106(16) . . . . ?
C2 C1 C7 C8 72(16) . . . . ?
C1 C7 C8 C9 -18(64) . . . . ?
C7 C8 C9 C14 118(54) . . . . ?
C7 C8 C9 C10 -63(54) . . . . ?
C14 C9 C10 C11 1.3(8) . . . . ?
C8 C9 C10 C11 -177.7(5) . . . . ?
C14 C9 C10 C23 178.6(5) . . . . ?
C8 C9 C10 C23 -0.4(9) . . . . ?
C9 C10 C11 C12 -1.3(8) . . . . ?
C23 C10 C11 C12 -178.4(5) . . . . ?
C9 C10 C11 C24 175.8(6) . . . . ?
C23 C10 C11 C24 -1.4(9) . . . . ?
C10 C11 C12 C13 0.2(8) . . . . ?
C24 C11 C12 C13 -176.8(6) . . . . ?
C10 C11 C12 C15 178.7(5) . . . . ?
C24 C11 C12 C15 1.7(9) . . . . ?
C11 C12 C13 C14 0.8(9) . . . . ?
C15 C12 C13 C14 -177.8(6) . . . . ?
C12 C13 C14 C9 -0.7(9) . . . . ?
C10 C9 C14 C13 -0.4(9) . . . . ?
C8 C9 C14 C13 178.7(6) . . . . ?
C13 C12 C15 C16 11(12) . . . . ?
C11 C12 C15 C16 -167(11) . . . . ?
C12 C15 C16 C17 142(12) . . . . ?
C15 C16 C17 C18 9(15) . . . . ?
C15 C16 C17 C22 -171(14) . . . . ?
C22 C17 C18 C19 0.1(9) . . . . ?
C16 C17 C18 C19 179.4(6) . . . . ?
C17 C18 C19 C20 0.2(10) . . . . ?
C18 C19 C20 C21 -0.3(10) . . . . ?
C19 C20 C21 C22 0.0(10) . . . . ?
C20 C21 C22 C17 0.3(10) . . . . ?
C18 C17 C22 C21 -0.4(9) . . . . ?
C16 C17 C22 C21 -179.7(6) . . . . ?
C11 C10 C23 N1 -57.4(8) . . . . ?
C9 C10 C23 N1 125.4(7) . . . . ?
C10 C11 C24 N2 60.3(8) . . . . ?
C12 C11 C24 N2 -122.7(7) . . . . ?
N1 C27 C28 O3 -117.7(8) . . . . ?
N2 C27 C28 O3 10.5(10) . . . . ?
C31 C27 C28 O3 128.4(9) . . . . ?
N1 C27 C28 O4 61.8(8) . . . . ?
N2 C27 C28 O4 -170.0(6) . . . . ?
C31 C27 C28 O4 -52.1(10) . . . . ?
N1 C27 C31 N4 106.1(7) . . . . ?
N2 C27 C31 N4 -13.8(8) . . . . ?
C28 C27 C31 N4 -134.8(8) . . . . ?
N1 C27 C31 N3 -12.8(8) . . . . ?
N2 C27 C31 N3 -132.8(7) . . . . ?
C28 C27 C31 N3 106.3(8) . . . . ?
N1 C27 C31 C32 -136.7(8) . . . . ?
N2 C27 C31 C32 103.3(8) . . . . ?
C28 C27 C31 C32 -17.6(13) . . . . ?
N4 C31 C32 O5 -111.6(8) . . . . ?
N3 C31 C32 O5 15.4(10) . . . . ?
C27 C31 C32 O5 135.8(9) . . . . ?
N4 C31 C32 O6 65.2(8) . . . . ?
N3 C31 C32 O6 -167.7(6) . . . . ?
C27 C31 C32 O6 -47.4(10) . . . . ?
N3 C35 C37 C38 59.0(8) . . . . ?
N3 C35 C37 C42 -121.7(7) . . . . ?
C42 C37 C38 C39 -1.2(8) . . . . ?
C35 C37 C38 C39 178.2(5) . . . . ?
C42 C37 C38 C36 179.6(6) . . . . ?
C35 C37 C38 C36 -1.0(9) . . . . ?
N4 C36 C38 C37 -59.2(8) . . . . ?
N4 C36 C38 C39 121.6(7) . . . . ?
C37 C38 C39 O7 -179.5(5) . . . . ?
C36 C38 C39 O7 -0.3(8) . . . . ?
C37 C38 C39 C40 -0.6(9) . . . . ?
C36 C38 C39 C40 178.7(6) . . . . ?
O7 C39 C40 C41 179.9(5) . . . . ?
C38 C39 C40 C41 1.0(9) . . . . ?
C39 C40 C41 C42 0.3(9) . . . . ?
C40 C41 C42 O8 179.8(5) . . . . ?
C40 C41 C42 C37 -2.1(9) . . . . ?
C38 C37 C42 C41 2.5(9) . . . . ?
C35 C37 C42 C41 -176.8(6) . . . . ?
C38 C37 C42 O8 -179.2(5) . . . . ?
C35 C37 C42 O8 1.4(8) . . . . ?
O1 C25 N1 C27 178.6(7) . . . . ?
N3 C25 N1 C27 0.7(7) . . . . ?
O1 C25 N1 C23 -4.0(9) . . . . ?
N3 C25 N1 C23 178.1(5) . . . . ?
N2 C27 N1 C25 120.0(7) . . . . ?
C28 C27 N1 C25 -114.5(7) . . . . ?
C31 C27 N1 C25 7.7(8) . . . . ?
N2 C27 N1 C23 -57.4(9) . . . . ?
C28 C27 N1 C23 68.1(9) . . . . ?
C31 C27 N1 C23 -169.7(6) . . . . ?
C10 C23 N1 C25 -101.0(7) . . . . ?
C10 C23 N1 C27 76.1(8) . . . . ?
O2 C26 N2 C27 167.8(6) . . . . ?
N4 C26 N2 C27 -14.8(7) . . . . ?
O2 C26 N2 C24 21.3(9) . . . . ?
N4 C26 N2 C24 -161.3(5) . . . . ?
N1 C27 N2 C26 -92.4(8) . . . . ?
C28 C27 N2 C26 141.9(6) . . . . ?
C31 C27 N2 C26 18.0(8) . . . . ?
N1 C27 N2 C24 54.2(9) . . . . ?
C28 C27 N2 C24 -71.5(8) . . . . ?
C31 C27 N2 C24 164.5(7) . . . . ?
C11 C24 N2 C26 68.9(8) . . . . ?
C11 C24 N2 C27 -74.0(9) . . . . ?
O1 C25 N3 C31 172.1(7) . . . . ?
N1 C25 N3 C31 -9.9(7) . . . . ?
O1 C25 N3 C35 24.4(9) . . . . ?
N1 C25 N3 C35 -157.7(5) . . . . ?
N4 C31 N3 C25 -94.7(8) . . . . ?
C32 C31 N3 C25 141.5(6) . . . . ?
C27 C31 N3 C25 14.4(8) . . . . ?
N4 C31 N3 C35 51.5(9) . . . . ?
C32 C31 N3 C35 -72.3(8) . . . . ?
C27 C31 N3 C35 160.6(7) . . . . ?
C37 C35 N3 C25 73.2(9) . . . . ?
C37 C35 N3 C31 -70.7(10) . . . . ?
O2 C26 N4 C31 -177.6(7) . . . . ?
N2 C26 N4 C31 5.0(7) . . . . ?
O2 C26 N4 C36 -2.2(10) . . . . ?
N2 C26 N4 C36 -179.5(5) . . . . ?
N3 C31 N4 C26 117.5(7) . . . . ?
C32 C31 N4 C26 -117.1(7) . . . . ?
C27 C31 N4 C26 5.8(8) . . . . ?
N3 C31 N4 C36 -58.1(9) . . . . ?
C32 C31 N4 C36 67.3(9) . . . . ?
C27 C31 N4 C36 -169.8(6) . . . . ?
C38 C36 N4 C26 -95.8(8) . . . . ?
C38 C36 N4 C31 79.4(9) . . . . ?
O3 C28 O4 C29' -5.9(18) . . . . ?
C27 C28 O4 C29' 174.7(17) . . . . ?
O3 C28 O4 C29 7.0(17) . . . . ?
C27 C28 O4 C29 -172.5(15) . . . . ?
O5 C32 O6 C33 7.7(9) . . . . ?
C31 C32 O6 C33 -169.1(6) . . . . ?
C34 C33 O6 C32 81.3(7) . . . . ?
C40 C39 O7 C43 0.7(8) . . . . ?
C38 C39 O7 C43 179.7(5) . . . . ?
C41 C42 O8 C44 -0.1(8) . . . . ?
C37 C42 O8 C44 -178.3(5) . . . . ?
C28 O4 C29 C30 -132(3) . . . . ?
C29' O4 C29 C30 -60(6) . . . . ?
C28 O4 C29' C30' -167(3) . . . . ?
C29 O4 C29' C30' 80(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        16.19
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.204
_refine_diff_density_rms         0.039


# start Validation Reply Form
_vrf_REFNR01_4                   
;
PROBLEM: Ratio of reflections to parameters is < 6 for a 
centrosymmetric structure  
           sine(theta)/lambda                0.3923
           Proportion of unique data used    1.0000
           Ratio reflections to parameters   3.7071
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
            Calculated sin(theta_max)/wavelength =    0.4585
RESPONSE: Although we have re-tried several times to selected better
crystals for x-ray diffraction experiment, we are failed each time. 
This may be resulted from the weak diffraction ability at the high 
two-theta angle for such a small crystal. 
;
_vrf_THETM01_4                   
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
            Calculated sin(theta_max)/wavelength =    0.3923
RESPONSE: Although we have re-tried several times to selected better
crystals for x-ray diffraction experiment, we are failed each time. 
This may be resulted from the weak diffraction ability at the high 
two-theta angle for such a small crystal. 
;
_vrf_PLAT088_4                   
;
PROBLEM: Poor Data / Parameter Ratio ....................       3.75.
RESPONSE: Although we have re-tried several times to selected better
crystals for x-ray diffraction experiment, we are failed each time. 
This may be resulted from the weak diffraction ability at the high 
two-theta angle for such a small crystal. 
;
# end Validation Reply Form

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_5
_database_code_depnum_ccdc_archive 'CCDC 992393'
_audit_update_record             
;
2014-03-18 deposited with the CCDC.
2015-02-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C47 H41 Cl3 F2 N3 O8.50'
_chemical_formula_weight         928.18

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'
F F 0.0171 0.0103 '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                   12.9379(12)
_cell_length_b                   13.0294(12)
_cell_length_c                   15.7092(14)
_cell_angle_alpha                114.0830(10)
_cell_angle_beta                 93.5220(10)
_cell_angle_gamma                111.3440(10)
_cell_volume                     2182.1(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9772
_cell_measurement_theta_min      2.54
_cell_measurement_theta_max      22.68

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      1.413
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             962
_exptl_absorpt_coefficient_mu    0.278
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  0.9464
_exptl_absorpt_correction_T_max  0.9727
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12070
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0394
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.74
_diffrn_reflns_theta_max         22.69
_reflns_number_total             5719
_reflns_number_gt                4676
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.1097P)²+2.0342P] where P=(Fo²+2Fc²)/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       0.0025(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         5719
_refine_ls_number_parameters     631
_refine_ls_number_restraints     26
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0550
_refine_ls_wR_factor_ref         0.1746
_refine_ls_wR_factor_gt          0.1622
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1953(3) 1.0299(3) 0.2338(3) 0.0270(8) Uani 1 1 d . . .
C2 C 0.2177(3) 1.0878(3) 0.3330(3) 0.0279(8) Uani 1 1 d . . .
H2 H 0.2050 1.1597 0.3666 0.033 Uiso 1 1 calc R . .
C3 C 0.2591(3) 1.0377(3) 0.3816(2) 0.0256(8) Uani 1 1 d . . .
H3 H 0.2757 1.0761 0.4499 0.031 Uiso 1 1 calc R . .
C4 C 0.2770(3) 0.9318(3) 0.3320(2) 0.0212(8) Uani 1 1 d . . .
C5 C 0.2501(3) 0.8746(3) 0.2314(2) 0.0259(8) Uani 1 1 d . . .
H5 H 0.2600 0.8010 0.1967 0.031 Uiso 1 1 calc R . .
C6 C 0.2089(3) 0.9251(3) 0.1818(3) 0.0279(8) Uani 1 1 d . . .
H6 H 0.1909 0.8873 0.1135 0.033 Uiso 1 1 calc R . .
C7 C 0.3249(3) 0.8854(3) 0.3844(2) 0.0224(8) Uani 1 1 d . . .
C8 C 0.3672(3) 0.8528(3) 0.4338(2) 0.0207(8) Uani 1 1 d . . .
C9 C 0.4136(3) 0.8105(3) 0.4907(2) 0.0198(7) Uani 1 1 d . . .
C10 C 0.4266(3) 0.8639(3) 0.5913(2) 0.0179(7) Uani 1 1 d . . .
C11 C 0.4697(3) 0.8178(3) 0.6445(2) 0.0191(7) Uani 1 1 d . . .
C12 C 0.4998(3) 0.7189(3) 0.5974(2) 0.0200(7) Uani 1 1 d . . .
C13 C 0.4889(3) 0.6693(3) 0.4987(2) 0.0250(8) Uani 1 1 d . . .
H13 H 0.5105 0.6034 0.4673 0.030 Uiso 1 1 calc R . .
C14 C 0.4473(3) 0.7142(3) 0.4457(2) 0.0228(8) Uani 1 1 d . . .
H14 H 0.4414 0.6799 0.3784 0.027 Uiso 1 1 calc R . .
C15 C 0.5449(3) 0.6704(3) 0.6508(2) 0.0236(8) Uani 1 1 d . . .
C16 C 0.5812(3) 0.6291(3) 0.6951(2) 0.0240(8) Uani 1 1 d . . .
C17 C 0.6201(3) 0.5754(3) 0.7464(2) 0.0219(8) Uani 1 1 d . . .
C18 C 0.5497(3) 0.5220(3) 0.7951(2) 0.0275(8) Uani 1 1 d . . .
H18 H 0.4773 0.5247 0.7965 0.033 Uiso 1 1 calc R . .
C19 C 0.5846(3) 0.4655(3) 0.8412(3) 0.0320(9) Uani 1 1 d . . .
H19 H 0.5368 0.4286 0.8739 0.038 Uiso 1 1 calc R . .
C20 C 0.6900(3) 0.4639(3) 0.8386(3) 0.0303(9) Uani 1 1 d . . .
C21 C 0.7622(3) 0.5158(3) 0.7924(3) 0.0294(8) Uani 1 1 d . . .
H21 H 0.8347 0.5132 0.7922 0.035 Uiso 1 1 calc R . .
C22 C 0.7269(3) 0.5718(3) 0.7462(2) 0.0258(8) Uani 1 1 d . . .
H22 H 0.7757 0.6084 0.7138 0.031 Uiso 1 1 calc R . .
C23 C 0.3973(3) 0.9732(3) 0.6411(2) 0.0193(7) Uani 1 1 d . . .
H23A H 0.4683 1.0472 0.6845 0.023 Uiso 1 1 calc R . .
H23B H 0.3676 0.9913 0.5919 0.023 Uiso 1 1 calc R . .
C24 C 0.4903(3) 0.8781(3) 0.7538(2) 0.0201(7) Uani 1 1 d . . .
H24A H 0.5250 0.8360 0.7783 0.024 Uiso 1 1 calc R . .
H24B H 0.5464 0.9661 0.7809 0.024 Uiso 1 1 calc R . .
C25 C 0.1979(3) 0.9085(3) 0.6604(2) 0.0209(8) Uani 1 1 d . . .
C26 C 0.3035(3) 0.7617(3) 0.7759(2) 0.0201(8) Uani 1 1 d . . .
C27 C 0.3407(3) 0.9585(3) 0.7897(2) 0.0178(7) Uani 1 1 d . . .
C28 C 0.4194(3) 1.0932(3) 0.8654(2) 0.0204(7) Uani 1 1 d . . .
C29 C 0.5301(3) 1.2198(3) 1.0265(2) 0.0277(8) Uani 1 1 d . . .
H29A H 0.5254 1.2201 1.0893 0.033 Uiso 1 1 calc R . .
H29B H 0.5064 1.2830 1.0245 0.033 Uiso 1 1 calc R . .
C30 C 0.6511(3) 1.2521(4) 1.0172(3) 0.0369(10) Uani 1 1 d . . .
H30A H 0.6734 1.1874 1.0162 0.055 Uiso 1 1 calc R . .
H30B H 0.7022 1.3321 1.0719 0.055 Uiso 1 1 calc R . .
H30C H 0.6569 1.2580 0.9572 0.055 Uiso 1 1 calc R . .
C31 C 0.1432(2) 0.8930(2) 0.72989(19) 0.0069(6) Uani 1 1 d . . .
C32 C 0.2188(3) 0.9010(3) 0.8070(2) 0.0205(7) Uani 1 1 d . . .
C33 C 0.2051(3) 0.9788(3) 0.9064(2) 0.0230(8) Uani 1 1 d . . .
C34 C 0.2042(3) 1.1740(3) 1.0063(3) 0.0368(9) Uani 1 1 d D . .
H34A H 0.2464 1.1709 1.0593 0.044 Uiso 0.50(3) 1 calc PR A 1
H34B H 0.2420 1.2593 1.0138 0.044 Uiso 0.50(3) 1 calc PR A 1
H34C H 0.2686 1.2569 1.0299 0.044 Uiso 0.50(3) 1 d PR A 2
H34D H 0.2071 1.1450 1.0553 0.044 Uiso 0.50(3) 1 d PR A 2
C35 C 0.0859(9) 1.1477(14) 1.0149(11) 0.046(4) Uani 0.50(3) 1 d PDU A 1
H35A H 0.0457 1.1587 0.9667 0.068 Uiso 0.50(3) 1 calc PR A 1
H35B H 0.0866 1.2049 1.0794 0.068 Uiso 0.50(3) 1 calc PR A 1
H35C H 0.0466 1.0619 1.0043 0.068 Uiso 0.50(3) 1 calc PR A 1
C35' C 0.0927(9) 1.1841(15) 0.9847(11) 0.047(4) Uani 0.50(3) 1 d PDU A 2
H35D H 0.0954 1.2150 0.9371 0.071 Uiso 0.50(3) 1 calc PR A 2
H35E H 0.0830 1.2417 1.0440 0.071 Uiso 0.50(3) 1 calc PR A 2
H35F H 0.0282 1.1019 0.9590 0.071 Uiso 0.50(3) 1 calc PR A 2
C36 C 0.0186(3) 0.8198(3) 0.7057(2) 0.0242(8) Uani 1 1 d . . .
H36A H -0.0184 0.8444 0.6651 0.029 Uiso 1 1 calc R . .
H36B H -0.0074 0.8419 0.7659 0.029 Uiso 1 1 calc R . .
C37 C 0.1018(3) 0.6860(3) 0.7892(2) 0.0243(8) Uani 1 1 d . . .
H37A H 0.0665 0.7244 0.8400 0.029 Uiso 1 1 calc R . .
H37B H 0.1190 0.6250 0.8022 0.029 Uiso 1 1 calc R . .
C38 C -0.0229(3) 0.6794(3) 0.6533(2) 0.0234(8) Uani 1 1 d . . .
C39 C 0.0151(3) 0.6170(3) 0.6924(2) 0.0217(8) Uani 1 1 d . . .
C40 C -0.0292(3) 0.4872(3) 0.6448(2) 0.0263(8) Uani 1 1 d . . .
C41 C -0.1112(3) 0.4200(3) 0.5570(2) 0.0276(8) Uani 1 1 d . . .
H41 H -0.1409 0.3320 0.5239 0.033 Uiso 1 1 calc R . .
C42 C -0.1489(3) 0.4814(3) 0.5186(2) 0.0272(8) Uani 1 1 d . . .
H42 H -0.2051 0.4353 0.4592 0.033 Uiso 1 1 calc R . .
C43 C -0.1060(3) 0.6096(3) 0.5653(2) 0.0251(8) Uani 1 1 d . . .
C44 C -0.0241(4) 0.3033(3) 0.6403(3) 0.0394(10) Uani 1 1 d . . .
H44A H -0.1069 0.2600 0.6311 0.059 Uiso 1 1 calc R . .
H44B H 0.0162 0.2787 0.6778 0.059 Uiso 1 1 calc R . .
H44C H -0.0057 0.2812 0.5775 0.059 Uiso 1 1 calc R . .
C45 C -0.2334(3) 0.6067(4) 0.4452(3) 0.0393(10) Uani 1 1 d . . .
H45A H -0.2076 0.5582 0.3922 0.059 Uiso 1 1 calc R . .
H45B H -0.2534 0.6637 0.4296 0.059 Uiso 1 1 calc R . .
H45C H -0.3007 0.5503 0.4547 0.059 Uiso 1 1 calc R . .
C47 C -0.0172(9) 0.5500(9) 0.0608(7) 0.059(3) Uani 0.50 1 d P . .
H47A H -0.0895 0.5538 0.0665 0.070 Uiso 0.50 1 d PR . .
H47B H 0.0365 0.5998 0.1225 0.070 Uiso 0.50 1 d PR . .
Cl4 Cl 0.03611(12) 0.60796(12) -0.01608(10) 0.0660(4) Uani 1 1 d . . .
C46 C 0.2157(10) 0.2381(10) 0.7850(10) 0.041(3) Uani 0.465(4) 1 d PD B 1
H46A H 0.2557 0.1887 0.7912 0.049 Uiso 0.465(4) 1 calc PR B 1
H46B H 0.2221 0.2424 0.7240 0.049 Uiso 0.465(4) 1 calc PR B 1
Cl5 Cl 0.2823(4) 0.3887(4) 0.8814(3) 0.0573(11) Uani 0.465(4) 1 d PD B 1
Cl6 Cl 0.0708(2) 0.1637(2) 0.78117(19) 0.0529(9) Uani 0.465(4) 1 d PD B 1
C46' C 0.2336(12) 0.2114(12) 0.7541(9) 0.056(4) Uani 0.535(4) 1 d PDU B 2
H46C H 0.2638 0.1762 0.7894 0.067 Uiso 0.535(4) 1 calc PR B 2
H46D H 0.1521 0.1542 0.7215 0.067 Uiso 0.535(4) 1 calc PR B 2
Cl5' Cl 0.2444(5) 0.3593(6) 0.8370(4) 0.1038(18) Uani 0.535(4) 1 d PD B 2
Cl6' Cl 0.3102(2) 0.2232(2) 0.66834(16) 0.0675(9) Uani 0.535(4) 1 d PD B 2
F1 F 0.7248(2) 0.4087(2) 0.88424(16) 0.0437(6) Uani 1 1 d . . .
F2 F 0.15802(18) 1.0821(2) 0.18616(15) 0.0373(6) Uani 1 1 d . . .
N4 N 0.3135(2) 0.9531(2) 0.69675(18) 0.0183(6) Uani 1 1 d . . .
N16 N 0.2085(2) 0.7821(2) 0.79566(18) 0.0207(6) Uani 1 1 d . . .
N17 N 0.3884(2) 0.8740(2) 0.78873(18) 0.0182(6) Uani 1 1 d . . .
O1 O 0.15295(19) 0.8906(2) 0.58255(16) 0.0244(6) Uani 1 1 d . . .
O2 O 0.31444(19) 0.6667(2) 0.75504(15) 0.0234(5) Uani 1 1 d . . .
O3 O 0.4441(2) 1.1807(2) 0.84941(16) 0.0268(6) Uani 1 1 d . . .
O4 O 0.45262(18) 1.0965(2) 0.94832(15) 0.0233(5) Uani 1 1 d . . .
O5 O 0.1908(2) 0.9447(2) 0.96690(17) 0.0335(6) Uani 1 1 d . . .
O6 O 0.2119(2) 1.0864(2) 0.91405(16) 0.0270(6) Uani 1 1 d . A .
O7 O 0.0108(2) 0.4339(2) 0.69035(17) 0.0332(6) Uani 1 1 d . . .
O8 O -0.14270(19) 0.6771(2) 0.53214(16) 0.0295(6) Uani 1 1 d . . .
C48 C 0.0343(7) 0.0381(9) 0.5026(7) 0.050(3) Uani 0.50 1 d P C -1
H48A H -0.0223 0.0119 0.5370 0.075 Uiso 0.50 1 calc PR C -1
H48B H 0.0227 -0.0336 0.4417 0.075 Uiso 0.50 1 calc PR C -1
H48C H 0.0253 0.1021 0.4895 0.075 Uiso 0.50 1 calc PR C -1
O9 O 0.1468(5) 0.0874(6) 0.5603(4) 0.0530(16) Uani 0.50 1 d P . .
H9 H 0.1947 0.0985 0.5275 0.079 Uiso 0.50 1 calc PR C .


_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
C1 C6 1.358(5) . ?
C1 F2 1.365(4) . ?
C1 C2 1.381(5) . ?
C2 C3 1.381(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.394(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.399(5) . ?
C4 C7 1.429(5) . ?
C5 C6 1.396(5) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.211(5) . ?
C8 C9 1.429(5) . ?
C9 C14 1.406(5) . ?
C9 C10 1.412(5) . ?
C10 C11 1.403(5) . ?
C10 C23 1.517(4) . ?
C11 C12 1.408(5) . ?
C11 C24 1.526(5) . ?
C12 C13 1.391(5) . ?
C12 C15 1.443(5) . ?
C13 C14 1.377(5) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 C16 1.202(5) . ?
C16 C17 1.436(5) . ?
C17 C18 1.399(5) . ?
C17 C22 1.400(5) . ?
C18 C19 1.381(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.375(5) . ?
C19 H19 0.9500 . ?
C20 F1 1.360(4) . ?
C20 C21 1.372(5) . ?
C21 C22 1.380(5) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C23 N4 1.451(4) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 N17 1.451(4) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 O1 1.211(4) . ?
C25 N4 1.376(4) . ?
C25 C31 1.380(4) . ?
C26 O2 1.210(4) . ?
C26 N16 1.376(4) . ?
C26 N17 1.396(4) . ?
C27 N17 1.441(4) . ?
C27 N4 1.448(4) . ?
C27 C28 1.542(5) . ?
C27 C32 1.575(4) . ?
C28 O3 1.202(4) . ?
C28 O4 1.325(4) . ?
C29 O4 1.470(4) . ?
C29 C30 1.500(5) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.454(4) . ?
C31 C36 1.470(4) . ?
C32 N16 1.439(4) . ?
C32 C33 1.539(5) . ?
C33 O5 1.201(4) . ?
C33 O6 1.327(4) . ?
C34 C35 1.469(11) . ?
C34 O6 1.471(4) . ?
C34 C35' 1.525(12) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 H34C 0.9900 . ?
C34 H34D 0.9899 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C35' H35D 0.9800 . ?
C35' H35E 0.9800 . ?
C35' H35F 0.9800 . ?
C36 C38 1.521(5) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 N16 1.451(4) . ?
C37 C39 1.522(5) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 C39 1.394(5) . ?
C38 C43 1.405(5) . ?
C39 C40 1.399(5) . ?
C40 O7 1.372(4) . ?
C40 C41 1.398(5) . ?
C41 C42 1.372(5) . ?
C41 H41 0.9500 . ?
C42 C43 1.383(5) . ?
C42 H42 0.9500 . ?
C43 O8 1.384(4) . ?
C44 O7 1.422(4) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 O8 1.442(4) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C47 Cl4 1.724(10) . ?
C47 Cl4 1.795(10) 2_565 ?
C47 C47 2.009(19) 2_565 ?
C47 H47A 0.9621 . ?
C47 H47B 0.9599 . ?
Cl4 C47 1.795(10) 2_565 ?
C46 Cl5 1.752(11) . ?
C46 Cl6 1.753(12) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C46' Cl6' 1.744(12) . ?
C46' Cl5' 1.779(12) . ?
C46' H46C 0.9900 . ?
C46' H46D 0.9900 . ?
C48 O9 1.427(11) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
O9 H9 0.8400 . ?

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
C6 C1 F2 118.8(3) . . ?
C6 C1 C2 123.6(3) . . ?
F2 C1 C2 117.6(3) . . ?
C1 C2 C3 117.8(3) . . ?
C1 C2 H2 121.1 . . ?
C3 C2 H2 121.1 . . ?
C2 C3 C4 121.0(3) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
C3 C4 C5 119.0(3) . . ?
C3 C4 C7 119.7(3) . . ?
C5 C4 C7 121.2(3) . . ?
C6 C5 C4 120.2(3) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C1 C6 C5 118.3(3) . . ?
C1 C6 H6 120.9 . . ?
C5 C6 H6 120.9 . . ?
C8 C7 C4 176.1(3) . . ?
C7 C8 C9 178.0(3) . . ?
C14 C9 C10 119.5(3) . . ?
C14 C9 C8 119.3(3) . . ?
C10 C9 C8 121.2(3) . . ?
C11 C10 C9 119.6(3) . . ?
C11 C10 C23 120.7(3) . . ?
C9 C10 C23 119.7(3) . . ?
C10 C11 C12 119.9(3) . . ?
C10 C11 C24 120.7(3) . . ?
C12 C11 C24 119.4(3) . . ?
C13 C12 C11 119.7(3) . . ?
C13 C12 C15 119.4(3) . . ?
C11 C12 C15 120.8(3) . . ?
C14 C13 C12 120.9(3) . . ?
C14 C13 H13 119.5 . . ?
C12 C13 H13 119.5 . . ?
C13 C14 C9 120.3(3) . . ?
C13 C14 H14 119.9 . . ?
C9 C14 H14 119.9 . . ?
C16 C15 C12 179.2(4) . . ?
C15 C16 C17 177.7(3) . . ?
C18 C17 C22 118.9(3) . . ?
C18 C17 C16 120.2(3) . . ?
C22 C17 C16 120.9(3) . . ?
C19 C18 C17 120.4(3) . . ?
C19 C18 H18 119.8 . . ?
C17 C18 H18 119.8 . . ?
C20 C19 C18 118.6(3) . . ?
C20 C19 H19 120.7 . . ?
C18 C19 H19 120.7 . . ?
F1 C20 C21 118.3(3) . . ?
F1 C20 C19 118.6(3) . . ?
C21 C20 C19 123.0(3) . . ?
C20 C21 C22 118.3(3) . . ?
C20 C21 H21 120.9 . . ?
C22 C21 H21 120.9 . . ?
C21 C22 C17 120.8(3) . . ?
C21 C22 H22 119.6 . . ?
C17 C22 H22 119.6 . . ?
N4 C23 C10 114.1(3) . . ?
N4 C23 H23A 108.7 . . ?
C10 C23 H23A 108.7 . . ?
N4 C23 H23B 108.7 . . ?
C10 C23 H23B 108.7 . . ?
H23A C23 H23B 107.6 . . ?
N17 C24 C11 114.6(3) . . ?
N17 C24 H24A 108.6 . . ?
C11 C24 H24A 108.6 . . ?
N17 C24 H24B 108.6 . . ?
C11 C24 H24B 108.6 . . ?
H24A C24 H24B 107.6 . . ?
O1 C25 N4 125.9(3) . . ?
O1 C25 C31 126.3(3) . . ?
N4 C25 C31 107.7(3) . . ?
O2 C26 N16 127.2(3) . . ?
O2 C26 N17 125.7(3) . . ?
N16 C26 N17 107.0(3) . . ?
N17 C27 N4 113.9(3) . . ?
N17 C27 C28 111.3(3) . . ?
N4 C27 C28 110.2(3) . . ?
N17 C27 C32 103.0(2) . . ?
N4 C27 C32 102.7(2) . . ?
C28 C27 C32 115.5(3) . . ?
O3 C28 O4 126.4(3) . . ?
O3 C28 C27 123.4(3) . . ?
O4 C28 C27 110.2(3) . . ?
O4 C29 C30 110.5(3) . . ?
O4 C29 H29A 109.5 . . ?
C30 C29 H29A 109.5 . . ?
O4 C29 H29B 109.5 . . ?
C30 C29 H29B 109.5 . . ?
H29A C29 H29B 108.1 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C25 C31 C32 112.0(3) . . ?
C25 C31 C36 120.8(3) . . ?
C32 C31 C36 121.2(3) . . ?
N16 C32 C31 113.8(3) . . ?
N16 C32 C33 111.3(3) . . ?
C31 C32 C33 111.6(3) . . ?
N16 C32 C27 102.7(2) . . ?
C31 C32 C27 102.7(2) . . ?
C33 C32 C27 114.3(3) . . ?
O5 C33 O6 126.3(3) . . ?
O5 C33 C32 123.6(3) . . ?
O6 C33 C32 110.1(3) . . ?
C35 C34 O6 113.4(5) . . ?
C35 C34 C35' 30.3(4) . . ?
O6 C34 C35' 105.8(5) . . ?
C35 C34 H34A 108.9 . . ?
O6 C34 H34A 108.9 . . ?
C35' C34 H34A 136.1 . . ?
C35 C34 H34B 108.9 . . ?
O6 C34 H34B 108.9 . . ?
C35' C34 H34B 85.1 . . ?
H34A C34 H34B 107.7 . . ?
C35 C34 H34C 126.7 . . ?
O6 C34 H34C 110.0 . . ?
C35' C34 H34C 108.5 . . ?
H34A C34 H34C 84.0 . . ?
H34B C34 H34C 25.3 . . ?
C35 C34 H34D 83.3 . . ?
O6 C34 H34D 110.9 . . ?
C35' C34 H34D 113.0 . . ?
H34A C34 H34D 28.0 . . ?
H34B C34 H34D 128.8 . . ?
H34C C34 H34D 108.7 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
C34 C35' H35D 109.5 . . ?
C34 C35' H35E 109.5 . . ?
H35D C35' H35E 109.5 . . ?
C34 C35' H35F 109.5 . . ?
H35D C35' H35F 109.5 . . ?
H35E C35' H35F 109.5 . . ?
C31 C36 C38 115.6(3) . . ?
C31 C36 H36A 108.4 . . ?
C38 C36 H36A 108.4 . . ?
C31 C36 H36B 108.4 . . ?
C38 C36 H36B 108.4 . . ?
H36A C36 H36B 107.4 . . ?
N16 C37 C39 114.5(3) . . ?
N16 C37 H37A 108.6 . . ?
C39 C37 H37A 108.6 . . ?
N16 C37 H37B 108.6 . . ?
C39 C37 H37B 108.6 . . ?
H37A C37 H37B 107.6 . . ?
C39 C38 C43 118.8(3) . . ?
C39 C38 C36 121.8(3) . . ?
C43 C38 C36 119.4(3) . . ?
C38 C39 C40 120.4(3) . . ?
C38 C39 C37 121.7(3) . . ?
C40 C39 C37 117.8(3) . . ?
O7 C40 C41 124.2(3) . . ?
O7 C40 C39 116.2(3) . . ?
C41 C40 C39 119.6(3) . . ?
C42 C41 C40 120.0(3) . . ?
C42 C41 H41 120.0 . . ?
C40 C41 H41 120.0 . . ?
C41 C42 C43 120.9(3) . . ?
C41 C42 H42 119.6 . . ?
C43 C42 H42 119.6 . . ?
C42 C43 O8 123.8(3) . . ?
C42 C43 C38 120.4(3) . . ?
O8 C43 C38 115.8(3) . . ?
O7 C44 H44A 109.5 . . ?
O7 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
O7 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
O8 C45 H45A 109.5 . . ?
O8 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
O8 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
Cl4 C47 Cl4 110.4(5) . 2_565 ?
Cl4 C47 C47 56.9(5) . 2_565 ?
Cl4 C47 C47 53.5(4) 2_565 2_565 ?
Cl4 C47 H47A 109.4 . . ?
Cl4 C47 H47A 109.7 2_565 . ?
C47 C47 H47A 125.8 2_565 . ?
Cl4 C47 H47B 108.5 . . ?
Cl4 C47 H47B 109.1 2_565 . ?
C47 C47 H47B 124.3 2_565 . ?
H47A C47 H47B 109.8 . . ?
C47 Cl4 C47 69.6(5) . 2_565 ?
Cl5 C46 Cl6 111.8(6) . . ?
Cl5 C46 H46A 109.3 . . ?
Cl6 C46 H46A 109.3 . . ?
Cl5 C46 H46B 109.3 . . ?
Cl6 C46 H46B 109.3 . . ?
H46A C46 H46B 107.9 . . ?
Cl6' C46' Cl5' 111.0(7) . . ?
Cl6' C46' H46C 109.4 . . ?
Cl5' C46' H46C 109.4 . . ?
Cl6' C46' H46D 109.4 . . ?
Cl5' C46' H46D 109.4 . . ?
H46C C46' H46D 108.0 . . ?
C25 N4 C27 113.1(3) . . ?
C25 N4 C23 123.1(3) . . ?
C27 N4 C23 123.1(2) . . ?
C26 N16 C32 113.2(3) . . ?
C26 N16 C37 123.2(3) . . ?
C32 N16 C37 122.8(3) . . ?
C26 N17 C27 111.3(3) . . ?
C26 N17 C24 120.8(3) . . ?
C27 N17 C24 120.3(2) . . ?
C28 O4 C29 115.8(3) . . ?
C33 O6 C34 117.0(3) . . ?
C40 O7 C44 117.8(3) . . ?
C43 O8 C45 116.7(3) . . ?
O9 C48 H48A 109.5 . . ?
O9 C48 H48B 109.5 . . ?
O9 C48 H48C 109.5 . . ?
C48 O9 H9 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 1.8(5) . . . . ?
F2 C1 C2 C3 -177.8(3) . . . . ?
C1 C2 C3 C4 -0.4(5) . . . . ?
C2 C3 C4 C5 -1.3(5) . . . . ?
C2 C3 C4 C7 177.2(3) . . . . ?
C3 C4 C5 C6 1.7(5) . . . . ?
C7 C4 C5 C6 -176.8(3) . . . . ?
F2 C1 C6 C5 178.2(3) . . . . ?
C2 C1 C6 C5 -1.4(5) . . . . ?
C4 C5 C6 C1 -0.4(5) . . . . ?
C3 C4 C7 C8 -14(5) . . . . ?
C5 C4 C7 C8 165(5) . . . . ?
C4 C7 C8 C9 130(9) . . . . ?
C7 C8 C9 C14 73(10) . . . . ?
C7 C8 C9 C10 -108(10) . . . . ?
C14 C9 C10 C11 -1.9(5) . . . . ?
C8 C9 C10 C11 178.4(3) . . . . ?
C14 C9 C10 C23 176.2(3) . . . . ?
C8 C9 C10 C23 -3.6(4) . . . . ?
C9 C10 C11 C12 0.0(4) . . . . ?
C23 C10 C11 C12 -178.0(3) . . . . ?
C9 C10 C11 C24 176.9(3) . . . . ?
C23 C10 C11 C24 -1.2(4) . . . . ?
C10 C11 C12 C13 1.4(5) . . . . ?
C24 C11 C12 C13 -175.4(3) . . . . ?
C10 C11 C12 C15 179.6(3) . . . . ?
C24 C11 C12 C15 2.8(4) . . . . ?
C11 C12 C13 C14 -1.1(5) . . . . ?
C15 C12 C13 C14 -179.3(3) . . . . ?
C12 C13 C14 C9 -0.8(5) . . . . ?
C10 C9 C14 C13 2.3(5) . . . . ?
C8 C9 C14 C13 -178.0(3) . . . . ?
C13 C12 C15 C16 -95(25) . . . . ?
C11 C12 C15 C16 87(25) . . . . ?
C12 C15 C16 C17 19(31) . . . . ?
C15 C16 C17 C18 -45(9) . . . . ?
C15 C16 C17 C22 133(8) . . . . ?
C22 C17 C18 C19 -0.7(5) . . . . ?
C16 C17 C18 C19 177.2(3) . . . . ?
C17 C18 C19 C20 0.5(5) . . . . ?
C18 C19 C20 F1 179.8(3) . . . . ?
C18 C19 C20 C21 0.0(6) . . . . ?
F1 C20 C21 C22 -180.0(3) . . . . ?
C19 C20 C21 C22 -0.2(6) . . . . ?
C20 C21 C22 C17 -0.1(5) . . . . ?
C18 C17 C22 C21 0.6(5) . . . . ?
C16 C17 C22 C21 -177.4(3) . . . . ?
C11 C10 C23 N4 -57.9(4) . . . . ?
C9 C10 C23 N4 124.1(3) . . . . ?
C10 C11 C24 N17 61.7(4) . . . . ?
C12 C11 C24 N17 -121.4(3) . . . . ?
N17 C27 C28 O3 133.9(3) . . . . ?
N4 C27 C28 O3 6.5(4) . . . . ?
C32 C27 C28 O3 -109.2(3) . . . . ?
N17 C27 C28 O4 -47.1(3) . . . . ?
N4 C27 C28 O4 -174.4(2) . . . . ?
C32 C27 C28 O4 69.8(3) . . . . ?
O1 C25 C31 C32 169.7(3) . . . . ?
N4 C25 C31 C32 -12.7(3) . . . . ?
O1 C25 C31 C36 16.9(5) . . . . ?
N4 C25 C31 C36 -165.5(3) . . . . ?
C25 C31 C32 N16 -96.2(3) . . . . ?
C36 C31 C32 N16 56.5(4) . . . . ?
C25 C31 C32 C33 136.9(3) . . . . ?
C36 C31 C32 C33 -70.5(4) . . . . ?
C25 C31 C32 C27 14.1(3) . . . . ?
C36 C31 C32 C27 166.7(3) . . . . ?
N17 C27 C32 N16 -10.0(3) . . . . ?
N4 C27 C32 N16 108.5(3) . . . . ?
C28 C27 C32 N16 -131.5(3) . . . . ?
N17 C27 C32 C31 -128.4(2) . . . . ?
N4 C27 C32 C31 -9.8(3) . . . . ?
C28 C27 C32 C31 110.1(3) . . . . ?
N17 C27 C32 C33 110.6(3) . . . . ?
N4 C27 C32 C33 -130.8(3) . . . . ?
C28 C27 C32 C33 -10.9(4) . . . . ?
N16 C32 C33 O5 1.8(4) . . . . ?
C31 C32 C33 O5 130.1(3) . . . . ?
C27 C32 C33 O5 -114.0(4) . . . . ?
N16 C32 C33 O6 -178.3(2) . . . . ?
C31 C32 C33 O6 -50.1(3) . . . . ?
C27 C32 C33 O6 65.9(3) . . . . ?
C25 C31 C36 C38 76.7(4) . . . . ?
C32 C31 C36 C38 -73.6(4) . . . . ?
C31 C36 C38 C39 57.7(4) . . . . ?
C31 C36 C38 C43 -125.4(3) . . . . ?
C43 C38 C39 C40 -0.2(4) . . . . ?
C36 C38 C39 C40 176.7(3) . . . . ?
C43 C38 C39 C37 -177.8(3) . . . . ?
C36 C38 C39 C37 -0.9(4) . . . . ?
N16 C37 C39 C38 -56.3(4) . . . . ?
N16 C37 C39 C40 126.0(3) . . . . ?
C38 C39 C40 O7 -178.0(3) . . . . ?
C37 C39 C40 O7 -0.3(4) . . . . ?
C38 C39 C40 C41 0.6(5) . . . . ?
C37 C39 C40 C41 178.3(3) . . . . ?
O7 C40 C41 C42 177.7(3) . . . . ?
C39 C40 C41 C42 -0.8(5) . . . . ?
C40 C41 C42 C43 0.6(5) . . . . ?
C41 C42 C43 O8 -177.9(3) . . . . ?
C41 C42 C43 C38 -0.1(5) . . . . ?
C39 C38 C43 C42 0.0(4) . . . . ?
C36 C38 C43 C42 -177.1(3) . . . . ?
C39 C38 C43 O8 177.9(3) . . . . ?
C36 C38 C43 O8 0.9(4) . . . . ?
Cl4 C47 Cl4 C47 0.0 2_565 . . 2_565 ?
O1 C25 N4 C27 -176.9(3) . . . . ?
C31 C25 N4 C27 5.5(3) . . . . ?
O1 C25 N4 C23 -6.4(5) . . . . ?
C31 C25 N4 C23 176.0(3) . . . . ?
N17 C27 N4 C25 113.7(3) . . . . ?
C28 C27 N4 C25 -120.5(3) . . . . ?
C32 C27 N4 C25 3.1(3) . . . . ?
N17 C27 N4 C23 -56.8(4) . . . . ?
C28 C27 N4 C23 69.0(3) . . . . ?
C32 C27 N4 C23 -167.4(3) . . . . ?
C10 C23 N4 C25 -93.5(3) . . . . ?
C10 C23 N4 C27 76.0(4) . . . . ?
O2 C26 N16 C32 -173.2(3) . . . . ?
N17 C26 N16 C32 9.4(3) . . . . ?
O2 C26 N16 C37 -3.2(5) . . . . ?
N17 C26 N16 C37 179.4(3) . . . . ?
C31 C32 N16 C26 110.9(3) . . . . ?
C33 C32 N16 C26 -122.0(3) . . . . ?
C27 C32 N16 C26 0.7(3) . . . . ?
C31 C32 N16 C37 -59.1(4) . . . . ?
C33 C32 N16 C37 68.0(4) . . . . ?
C27 C32 N16 C37 -169.3(3) . . . . ?
C39 C37 N16 C26 -93.0(4) . . . . ?
C39 C37 N16 C32 76.0(4) . . . . ?
O2 C26 N17 C27 165.8(3) . . . . ?
N16 C26 N17 C27 -16.7(3) . . . . ?
O2 C26 N17 C24 16.1(5) . . . . ?
N16 C26 N17 C24 -166.5(3) . . . . ?
N4 C27 N17 C26 -93.8(3) . . . . ?
C28 C27 N17 C26 140.9(3) . . . . ?
C32 C27 N17 C26 16.6(3) . . . . ?
N4 C27 N17 C24 56.0(4) . . . . ?
C28 C27 N17 C24 -69.2(3) . . . . ?
C32 C27 N17 C24 166.4(2) . . . . ?
C11 C24 N17 C26 69.7(4) . . . . ?
C11 C24 N17 C27 -77.3(4) . . . . ?
O3 C28 O4 C29 -2.1(5) . . . . ?
C27 C28 O4 C29 178.9(2) . . . . ?
C30 C29 O4 C28 -81.8(4) . . . . ?
O5 C33 O6 C34 1.8(5) . . . . ?
C32 C33 O6 C34 -178.1(3) . . . . ?
C35 C34 O6 C33 -82.5(11) . . . . ?
C35' C34 O6 C33 -113.8(9) . . . . ?
C41 C40 O7 C44 7.0(5) . . . . ?
C39 C40 O7 C44 -174.4(3) . . . . ?
C42 C43 O8 C45 1.9(4) . . . . ?
C38 C43 O8 C45 -176.0(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        22.69
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.074

# start Validation Reply Form
_vrf_THETM01_5                   
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
            Calculated sin(theta_max)/wavelength =    0.4971  
RESPONSE: Although we have re-tried several times to selected better
crystals for x-ray diffraction experiment, we are failed each time. 
This may be resulted from the weak diffraction ability at the high 
two-theta angle for such a small crystal. 
;
_vrf_PLAT415_5                   
;
PROBLEM: Short Inter D-H..H-X    H3  .. H9  ..    1.66 Ang.  
RESPONSE: The atom of H9 is disordered. 
;
# end Validation Reply Form
#==END
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_6
_database_code_depnum_ccdc_archive 'CCDC 992394'
_audit_update_record             
;
2014-03-18 deposited with the CCDC.
2015-02-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C53.50 H43.50 Cl4.50 N4 O8'
_chemical_formula_weight         1029.95

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                   13.1674(15)
_cell_length_b                   13.8587(16)
_cell_length_c                   15.6640(18)
_cell_angle_alpha                64.005(2)
_cell_angle_beta                 85.984(2)
_cell_angle_gamma                67.813(2)
_cell_volume                     2363.3(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4355
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      23.02

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      1.447
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1066
_exptl_absorpt_coefficient_mu    0.341
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  0.9667
_exptl_absorpt_correction_T_max  0.9667
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13815
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0433
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.46
_diffrn_reflns_theta_max         23.09
_reflns_number_total             6542
_reflns_number_gt                5135
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.1398P)²+6.3223P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6542
_refine_ls_number_parameters     691
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0965
_refine_ls_R_factor_gt           0.0784
_refine_ls_wR_factor_ref         0.2403
_refine_ls_wR_factor_gt          0.2216
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5221(5) -0.1617(5) 0.3308(5) 0.0538(17) Uani 1 1 d . . .
H1A H 0.6014 -0.1968 0.3275 0.081 Uiso 1 1 calc R . .
H1B H 0.4813 -0.1795 0.2935 0.081 Uiso 1 1 calc R . .
H1C H 0.5070 -0.1935 0.3976 0.081 Uiso 1 1 calc R . .
C2 C 0.5301(4) 0.0016(4) 0.3423(4) 0.0303(12) Uani 1 1 d . . .
C3 C 0.6045(4) -0.0726(4) 0.4252(4) 0.0332(12) Uani 1 1 d . . .
H3 H 0.6260 -0.1545 0.4510 0.040 Uiso 1 1 calc R . .
C4 C 0.6463(4) -0.0270(5) 0.4693(4) 0.0337(12) Uani 1 1 d . . .
H4 H 0.6979 -0.0777 0.5251 0.040 Uiso 1 1 calc R . .
C5 C 0.6139(4) 0.0928(4) 0.4331(3) 0.0288(11) Uani 1 1 d . . .
C6 C 0.5379(4) 0.1682(4) 0.3504(3) 0.0259(11) Uani 1 1 d . . .
C7 C 0.4975(4) 0.1212(4) 0.3046(3) 0.0264(11) Uani 1 1 d . . .
C8 C 0.7377(5) 0.0712(5) 0.5511(4) 0.0463(15) Uani 1 1 d . . .
H8A H 0.7082 0.0230 0.6047 0.069 Uiso 1 1 calc R . .
H8B H 0.7610 0.1190 0.5702 0.069 Uiso 1 1 calc R . .
H8C H 0.8011 0.0210 0.5332 0.069 Uiso 1 1 calc R . .
C9 C 0.4236(4) 0.1982(4) 0.2099(3) 0.0273(11) Uani 1 1 d . . .
H9A H 0.4671 0.2338 0.1609 0.033 Uiso 1 1 calc R . .
H9B H 0.4035 0.1480 0.1906 0.033 Uiso 1 1 calc R . .
C10 C 0.5064(4) 0.2977(4) 0.3125(3) 0.0276(11) Uani 1 1 d . . .
H10A H 0.5399 0.3113 0.3587 0.033 Uiso 1 1 calc R . .
H10B H 0.5386 0.3259 0.2518 0.033 Uiso 1 1 calc R . .
C11 C 0.3213(4) 0.3924(4) 0.2130(3) 0.0235(10) Uani 1 1 d . . .
C12 C 0.3540(4) 0.4718(4) 0.1203(4) 0.0302(12) Uani 1 1 d . A .
C13 C 0.3852(16) 0.6452(13) 0.0388(9) 0.057(4) Uani 0.679(18) 1 d PD A 1
H13A H 0.4461 0.6020 0.0123 0.068 Uiso 0.679(18) 1 calc PR A 1
H13B H 0.3199 0.6924 -0.0100 0.068 Uiso 0.679(18) 1 calc PR A 1
C14 C 0.4191(8) 0.7230(8) 0.0632(7) 0.058(3) Uani 0.679(18) 1 d PD A 1
H14A H 0.3581 0.7664 0.0883 0.087 Uiso 0.679(18) 1 calc PR A 1
H14B H 0.4378 0.7778 0.0055 0.087 Uiso 0.679(18) 1 calc PR A 1
H14C H 0.4837 0.6756 0.1115 0.087 Uiso 0.679(18) 1 calc PR A 1
C14' C 0.333(3) 0.718(3) -0.0262(17) 0.125(14) Uani 0.321(18) 1 d PD A 2
H14D H 0.3353 0.6751 -0.0628 0.187 Uiso 0.321(18) 1 calc PR A 2
H14E H 0.3543 0.7834 -0.0647 0.187 Uiso 0.321(18) 1 calc PR A 2
H14F H 0.2578 0.7470 -0.0099 0.187 Uiso 0.321(18) 1 calc PR A 2
C13' C 0.412(3) 0.637(3) 0.0645(19) 0.081(15) Uani 0.321(18) 1 d PDU A 2
H13C H 0.4834 0.5909 0.0509 0.098 Uiso 0.321(18) 1 calc PR A 2
H13D H 0.4253 0.6824 0.0939 0.098 Uiso 0.321(18) 1 calc PR A 2
C15 C 0.2012(4) 0.4478(4) 0.2356(3) 0.0214(10) Uani 1 1 d . . .
C16 C 0.1342(4) 0.5748(4) 0.1599(3) 0.0238(10) Uani 1 1 d . . .
C17 C 0.0633(5) 0.6853(4) -0.0051(4) 0.0373(13) Uani 1 1 d . . .
H17A H 0.1097 0.7309 -0.0338 0.045 Uiso 1 1 calc R . .
H17B H -0.0017 0.7318 0.0156 0.045 Uiso 1 1 calc R . .
C18 C 0.0275(5) 0.6555(4) -0.0756(4) 0.0347(12) Uani 1 1 d . . .
H18A H 0.0927 0.6126 -0.0975 0.052 Uiso 1 1 calc R . .
H18B H -0.0183 0.7272 -0.1303 0.052 Uiso 1 1 calc R . .
H18C H -0.0152 0.6072 -0.0451 0.052 Uiso 1 1 calc R . .
C19 C 0.2266(4) 0.2730(4) 0.2322(3) 0.0242(11) Uani 1 1 d . . .
C20 C 0.3272(4) 0.3856(4) 0.3650(3) 0.0229(10) Uani 1 1 d . . .
C21 C 0.0457(4) 0.3765(4) 0.2736(3) 0.0225(10) Uani 1 1 d . . .
H21A H 0.0126 0.3404 0.2474 0.027 Uiso 1 1 calc R . .
H21B H -0.0047 0.4591 0.2510 0.027 Uiso 1 1 calc R . .
C22 C 0.1280(4) 0.4582(4) 0.3873(3) 0.0253(11) Uani 1 1 d . . .
H22A H 0.0626 0.5274 0.3471 0.030 Uiso 1 1 calc R . .
H22B H 0.1510 0.4740 0.4371 0.030 Uiso 1 1 calc R . .
C23 C 0.0946(4) 0.3551(4) 0.4358(3) 0.0235(10) Uani 1 1 d . . .
C24 C 0.0546(4) 0.3156(4) 0.3818(3) 0.0227(10) Uani 1 1 d . . .
C25 C 0.0213(4) 0.2218(4) 0.4270(3) 0.0243(11) Uani 1 1 d . . .
C26 C 0.0275(4) 0.1673(5) 0.5271(3) 0.0299(11) Uani 1 1 d . . .
H26 H 0.0043 0.1042 0.5581 0.036 Uiso 1 1 calc R . .
C27 C 0.0673(4) 0.2054(4) 0.5807(3) 0.0299(12) Uani 1 1 d . . .
H27 H 0.0715 0.1677 0.6485 0.036 Uiso 1 1 calc R . .
C28 C 0.1012(4) 0.2981(4) 0.5367(3) 0.0259(11) Uani 1 1 d . . .
C29 C 0.1391(4) 0.3368(4) 0.5947(3) 0.0284(12) Uani 1 1 d . . .
C30 C 0.1709(4) 0.3671(5) 0.6458(3) 0.0301(12) Uani 1 1 d . . .
C31 C 0.2067(4) 0.4050(4) 0.7052(3) 0.0283(11) Uani 1 1 d . . .
C32 C 0.2277(4) 0.5045(5) 0.6650(4) 0.0367(13) Uani 1 1 d . . .
H32 H 0.2196 0.5474 0.5974 0.044 Uiso 1 1 calc R . .
C33 C 0.2613(5) 0.5441(5) 0.7232(4) 0.0421(14) Uani 1 1 d . . .
H33 H 0.2761 0.6130 0.6945 0.050 Uiso 1 1 calc R . .
C34 C 0.2724(4) 0.4836(5) 0.8204(4) 0.0414(14) Uani 1 1 d . . .
H34 H 0.2951 0.5108 0.8587 0.050 Uiso 1 1 calc R . .
C35 C 0.2510(4) 0.3818(5) 0.8646(4) 0.0318(12) Uani 1 1 d . . .
C36 C 0.2606(5) 0.3175(6) 0.9662(4) 0.0432(15) Uani 1 1 d . . .
H36 H 0.2825 0.3441 1.0055 0.052 Uiso 1 1 calc R . .
C37 C 0.2391(5) 0.2198(6) 1.0076(4) 0.0459(15) Uani 1 1 d . . .
H37 H 0.2450 0.1792 1.0753 0.055 Uiso 1 1 calc R . .
C38 C 0.2079(5) 0.1782(6) 0.9500(4) 0.0476(15) Uani 1 1 d . . .
H38 H 0.1944 0.1086 0.9793 0.057 Uiso 1 1 calc R . .
C39 C 0.1971(4) 0.2374(5) 0.8524(4) 0.0358(13) Uani 1 1 d . . .
H39 H 0.1753 0.2091 0.8145 0.043 Uiso 1 1 calc R . .
C40 C 0.2181(4) 0.3397(5) 0.8078(4) 0.0309(12) Uani 1 1 d . . .
C41 C -0.0205(4) 0.1813(4) 0.3722(3) 0.0240(11) Uani 1 1 d . . .
C42 C -0.0537(4) 0.1479(4) 0.3257(3) 0.0281(11) Uani 1 1 d . . .
C43 C -0.0939(4) 0.1091(4) 0.2686(3) 0.0266(11) Uani 1 1 d . . .
C44 C -0.2048(4) 0.1302(5) 0.2590(4) 0.0404(14) Uani 1 1 d . . .
H44 H -0.2546 0.1711 0.2900 0.048 Uiso 1 1 calc R . .
C45 C -0.2446(5) 0.0921(6) 0.2043(4) 0.0474(15) Uani 1 1 d . . .
H45 H -0.3214 0.1090 0.1973 0.057 Uiso 1 1 calc R . .
C46 C -0.1750(5) 0.0313(5) 0.1613(4) 0.0414(14) Uani 1 1 d . . .
H46 H -0.2038 0.0059 0.1247 0.050 Uiso 1 1 calc R . .
C47 C -0.0596(4) 0.0048(4) 0.1697(3) 0.0307(12) Uani 1 1 d . . .
C48 C 0.0156(5) -0.0606(4) 0.1285(4) 0.0370(13) Uani 1 1 d . . .
H48 H -0.0103 -0.0897 0.0936 0.044 Uiso 1 1 calc R . .
C49 C 0.1241(5) -0.0829(5) 0.1376(4) 0.0453(15) Uani 1 1 d . . .
H49 H 0.1736 -0.1280 0.1095 0.054 Uiso 1 1 calc R . .
C50 C 0.1649(5) -0.0408(5) 0.1875(4) 0.0427(14) Uani 1 1 d . . .
H50 H 0.2415 -0.0565 0.1923 0.051 Uiso 1 1 calc R . .
C51 C 0.0952(4) 0.0235(4) 0.2301(3) 0.0306(12) Uani 1 1 d . . .
H51 H 0.1235 0.0522 0.2638 0.037 Uiso 1 1 calc R . .
C52 C -0.0184(4) 0.0463(4) 0.2232(3) 0.0254(11) Uani 1 1 d . . .
C53 C 0.3455(6) 0.6003(6) 0.4149(5) 0.0519(16) Uani 1 1 d . . .
H53 H 0.3597 0.5156 0.4516 0.062 Uiso 1 1 calc R . .
Cl1 Cl 0.4050(2) 0.62268(17) 0.30730(13) 0.0751(6) Uani 1 1 d . . .
Cl2 Cl 0.20141(15) 0.68011(15) 0.39032(14) 0.0689(6) Uani 1 1 d . . .
Cl3 Cl 0.40346(13) 0.64019(14) 0.48435(11) 0.0531(5) Uani 1 1 d . . .
C54 C 0.5182(16) 0.9222(18) 0.0374(12) 0.043(6) Uani 0.25 1 d PDU B -1
H54A H 0.5864 0.8556 0.0546 0.051 Uiso 0.25 1 d PR B -1
Cl4 Cl 0.4126(7) 0.8819(8) 0.0964(6) 0.127(3) Uani 0.38 1 d PD B -1
Cl5 Cl 0.4746(7) 0.9863(4) -0.0844(4) 0.0738(19) Uani 0.38 1 d PD B -1
C54' C 0.521(5) 0.997(5) 0.0244(18) 0.130(18) Uani 0.25 1 d PDU C -2
H54D H 0.5681 0.9159 0.0542 0.156 Uiso 0.25 1 d PR C -2
Cl4' Cl 0.590(3) 1.067(3) 0.049(2) 0.419(18) Uani 0.38 1 d PDU C -2
Cl5' Cl 0.5075(11) 1.0361(15) -0.0961(9) 0.178(5) Uani 0.38 1 d PDU C -2
N1 N 0.3222(3) 0.2912(3) 0.2083(3) 0.0230(9) Uani 1 1 d . . .
N2 N 0.1510(3) 0.3716(3) 0.2364(3) 0.0207(8) Uani 1 1 d . . .
N3 N 0.2175(3) 0.4431(3) 0.3275(3) 0.0224(9) Uani 1 1 d . . .
N4 N 0.3885(3) 0.3664(3) 0.2955(3) 0.0244(9) Uani 1 1 d . . .
O1 O 0.2097(3) 0.1875(3) 0.2445(2) 0.0262(8) Uani 1 1 d . . .
O2 O 0.3633(3) 0.3598(3) 0.4449(2) 0.0264(8) Uani 1 1 d . . .
O5 O 0.3758(3) 0.4520(3) 0.0527(3) 0.0422(9) Uani 1 1 d . . .
O6 O 0.3580(3) 0.5611(3) 0.1283(3) 0.0438(10) Uani 1 1 d D . .
O7 O 0.0948(3) 0.6564(3) 0.1767(2) 0.0400(9) Uani 1 1 d . . .
O8 O 0.1269(3) 0.5738(3) 0.0767(2) 0.0312(8) Uani 1 1 d . . .
O9 O 0.4878(3) -0.0380(3) 0.2926(3) 0.0385(9) Uani 1 1 d . . .
O10 O 0.6543(3) 0.1450(3) 0.4716(2) 0.0354(9) Uani 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
C1 O9 1.434(7) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 O9 1.373(6) . ?
C2 C7 1.385(7) . ?
C2 C3 1.397(7) . ?
C3 C4 1.370(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.391(7) . ?
C4 H4 0.9500 . ?
C5 O10 1.374(6) . ?
C5 C6 1.406(7) . ?
C6 C7 1.396(7) . ?
C6 C10 1.511(7) . ?
C7 C9 1.523(7) . ?
C8 O10 1.425(6) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N1 1.457(6) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 N4 1.452(6) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 N1 1.431(6) . ?
C11 N4 1.447(6) . ?
C11 C12 1.541(7) . ?
C11 C15 1.568(6) . ?
C12 O5 1.197(6) . ?
C12 O6 1.319(6) . ?
C13 C14 1.503(9) . ?
C13 O6 1.505(10) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C14' C13' 1.512(10) . ?
C14' H14D 0.9800 . ?
C14' H14E 0.9800 . ?
C14' H14F 0.9800 . ?
C13' O6 1.469(19) . ?
C13' H13C 0.9900 . ?
C13' H13D 0.9900 . ?
C15 N2 1.437(6) . ?
C15 N3 1.440(6) . ?
C15 C16 1.558(6) . ?
C16 O7 1.190(6) . ?
C16 O8 1.320(6) . ?
C17 O8 1.473(6) . ?
C17 C18 1.493(7) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 O1 1.218(6) . ?
C19 N1 1.370(6) . ?
C19 N2 1.380(6) . ?
C20 O2 1.218(5) . ?
C20 N4 1.368(6) . ?
C20 N3 1.380(6) . ?
C21 N2 1.455(6) . ?
C21 C24 1.515(6) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 N3 1.464(6) . ?
C22 C23 1.512(7) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.407(7) . ?
C23 C28 1.416(7) . ?
C24 C25 1.402(7) . ?
C25 C26 1.402(7) . ?
C25 C41 1.442(7) . ?
C26 C27 1.385(7) . ?
C26 H26 0.9500 . ?
C27 C28 1.393(7) . ?
C27 H27 0.9500 . ?
C28 C29 1.433(7) . ?
C29 C30 1.211(7) . ?
C30 C31 1.429(7) . ?
C31 C32 1.370(8) . ?
C31 C40 1.443(7) . ?
C32 C33 1.416(8) . ?
C32 H32 0.9500 . ?
C33 C34 1.365(8) . ?
C33 H33 0.9500 . ?
C34 C35 1.402(8) . ?
C34 H34 0.9500 . ?
C35 C40 1.422(7) . ?
C35 C36 1.429(8) . ?
C36 C37 1.352(9) . ?
C36 H36 0.9500 . ?
C37 C38 1.415(8) . ?
C37 H37 0.9500 . ?
C38 C39 1.370(8) . ?
C38 H38 0.9500 . ?
C39 C40 1.404(8) . ?
C39 H39 0.9500 . ?
C41 C42 1.195(7) . ?
C42 C43 1.439(7) . ?
C43 C44 1.382(7) . ?
C43 C52 1.428(7) . ?
C44 C45 1.399(8) . ?
C44 H44 0.9500 . ?
C45 C46 1.354(8) . ?
C45 H45 0.9500 . ?
C46 C47 1.423(8) . ?
C46 H46 0.9500 . ?
C47 C48 1.401(8) . ?
C47 C52 1.433(7) . ?
C48 C49 1.347(8) . ?
C48 H48 0.9500 . ?
C49 C50 1.391(8) . ?
C49 H49 0.9500 . ?
C50 C51 1.378(8) . ?
C50 H50 0.9500 . ?
C51 C52 1.408(7) . ?
C51 H51 0.9500 . ?
C53 Cl3 1.742(6) . ?
C53 Cl1 1.758(7) . ?
C53 Cl2 1.765(7) . ?
C53 H53 1.0000 . ?
C54 Cl5 1.744(16) . ?
C54 Cl4 1.747(17) . ?
C54 H54A 0.9600 . ?
C54 H54D 0.6843 . ?
C54' Cl5' 1.72(2) . ?
C54' Cl4' 1.72(2) . ?
C54' H54D 0.9600 . ?

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
O9 C1 H1A 109.5 . . ?
O9 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O9 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O9 C2 C7 116.4(4) . . ?
O9 C2 C3 123.0(4) . . ?
C7 C2 C3 120.5(5) . . ?
C4 C3 C2 119.8(5) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C3 C4 C5 120.6(5) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
O10 C5 C4 124.0(4) . . ?
O10 C5 C6 115.9(4) . . ?
C4 C5 C6 120.0(5) . . ?
C7 C6 C5 119.2(4) . . ?
C7 C6 C10 122.5(4) . . ?
C5 C6 C10 118.3(4) . . ?
C2 C7 C6 119.9(4) . . ?
C2 C7 C9 118.7(4) . . ?
C6 C7 C9 121.3(4) . . ?
O10 C8 H8A 109.5 . . ?
O10 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O10 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 C9 C7 116.5(4) . . ?
N1 C9 H9A 108.2 . . ?
C7 C9 H9A 108.2 . . ?
N1 C9 H9B 108.2 . . ?
C7 C9 H9B 108.2 . . ?
H9A C9 H9B 107.3 . . ?
N4 C10 C6 114.9(4) . . ?
N4 C10 H10A 108.5 . . ?
C6 C10 H10A 108.5 . . ?
N4 C10 H10B 108.5 . . ?
C6 C10 H10B 108.5 . . ?
H10A C10 H10B 107.5 . . ?
N1 C11 N4 113.8(4) . . ?
N1 C11 C12 111.3(4) . . ?
N4 C11 C12 110.6(4) . . ?
N1 C11 C15 103.2(4) . . ?
N4 C11 C15 102.5(3) . . ?
C12 C11 C15 115.2(4) . . ?
O5 C12 O6 125.6(5) . . ?
O5 C12 C11 124.3(5) . . ?
O6 C12 C11 110.0(4) . . ?
C14 C13 O6 108.6(8) . . ?
C14 C13 H13A 110.0 . . ?
O6 C13 H13A 110.0 . . ?
C14 C13 H13B 110.0 . . ?
O6 C13 H13B 110.0 . . ?
H13A C13 H13B 108.4 . . ?
C13' C14' H14D 109.5 . . ?
C13' C14' H14E 109.5 . . ?
H14D C14' H14E 109.5 . . ?
C13' C14' H14F 109.5 . . ?
H14D C14' H14F 109.5 . . ?
H14E C14' H14F 109.5 . . ?
O6 C13' C14' 105.7(16) . . ?
O6 C13' H13C 110.6 . . ?
C14' C13' H13C 110.6 . . ?
O6 C13' H13D 110.6 . . ?
C14' C13' H13D 110.6 . . ?
H13C C13' H13D 108.7 . . ?
N2 C15 N3 114.5(4) . . ?
N2 C15 C16 110.0(3) . . ?
N3 C15 C16 111.2(4) . . ?
N2 C15 C11 102.8(3) . . ?
N3 C15 C11 103.8(3) . . ?
C16 C15 C11 114.3(4) . . ?
O7 C16 O8 127.2(4) . . ?
O7 C16 C15 124.7(4) . . ?
O8 C16 C15 108.0(4) . . ?
O8 C17 C18 106.3(4) . . ?
O8 C17 H17A 110.5 . . ?
C18 C17 H17A 110.5 . . ?
O8 C17 H17B 110.5 . . ?
C18 C17 H17B 110.5 . . ?
H17A C17 H17B 108.7 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O1 C19 N1 126.7(4) . . ?
O1 C19 N2 125.9(4) . . ?
N1 C19 N2 107.3(4) . . ?
O2 C20 N4 126.1(4) . . ?
O2 C20 N3 125.8(4) . . ?
N4 C20 N3 108.1(4) . . ?
N2 C21 C24 113.8(4) . . ?
N2 C21 H21A 108.8 . . ?
C24 C21 H21A 108.8 . . ?
N2 C21 H21B 108.8 . . ?
C24 C21 H21B 108.8 . . ?
H21A C21 H21B 107.7 . . ?
N3 C22 C23 114.6(4) . . ?
N3 C22 H22A 108.6 . . ?
C23 C22 H22A 108.6 . . ?
N3 C22 H22B 108.6 . . ?
C23 C22 H22B 108.6 . . ?
H22A C22 H22B 107.6 . . ?
C24 C23 C28 118.8(4) . . ?
C24 C23 C22 120.9(4) . . ?
C28 C23 C22 120.3(4) . . ?
C25 C24 C23 120.6(4) . . ?
C25 C24 C21 119.8(4) . . ?
C23 C24 C21 119.6(4) . . ?
C26 C25 C24 119.6(4) . . ?
C26 C25 C41 119.5(4) . . ?
C24 C25 C41 121.0(4) . . ?
C27 C26 C25 120.1(5) . . ?
C27 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C26 C27 C28 121.0(4) . . ?
C26 C27 H27 119.5 . . ?
C28 C27 H27 119.5 . . ?
C27 C28 C23 119.9(4) . . ?
C27 C28 C29 119.2(4) . . ?
C23 C28 C29 120.9(5) . . ?
C30 C29 C28 178.3(5) . . ?
C29 C30 C31 178.9(5) . . ?
C32 C31 C30 120.2(5) . . ?
C32 C31 C40 120.0(5) . . ?
C30 C31 C40 119.8(5) . . ?
C31 C32 C33 120.8(5) . . ?
C31 C32 H32 119.6 . . ?
C33 C32 H32 119.6 . . ?
C34 C33 C32 120.1(6) . . ?
C34 C33 H33 119.9 . . ?
C32 C33 H33 119.9 . . ?
C33 C34 C35 121.1(5) . . ?
C33 C34 H34 119.4 . . ?
C35 C34 H34 119.4 . . ?
C34 C35 C40 119.9(5) . . ?
C34 C35 C36 122.3(5) . . ?
C40 C35 C36 117.8(5) . . ?
C37 C36 C35 121.6(5) . . ?
C37 C36 H36 119.2 . . ?
C35 C36 H36 119.2 . . ?
C36 C37 C38 119.9(5) . . ?
C36 C37 H37 120.1 . . ?
C38 C37 H37 120.1 . . ?
C39 C38 C37 120.5(6) . . ?
C39 C38 H38 119.7 . . ?
C37 C38 H38 119.7 . . ?
C38 C39 C40 120.5(5) . . ?
C38 C39 H39 119.7 . . ?
C40 C39 H39 119.7 . . ?
C39 C40 C35 119.7(5) . . ?
C39 C40 C31 122.1(4) . . ?
C35 C40 C31 118.1(5) . . ?
C42 C41 C25 178.8(5) . . ?
C41 C42 C43 179.2(5) . . ?
C44 C43 C52 119.9(4) . . ?
C44 C43 C42 120.3(4) . . ?
C52 C43 C42 119.8(4) . . ?
C43 C44 C45 120.8(5) . . ?
C43 C44 H44 119.6 . . ?
C45 C44 H44 119.6 . . ?
C46 C45 C44 120.8(5) . . ?
C46 C45 H45 119.6 . . ?
C44 C45 H45 119.6 . . ?
C45 C46 C47 121.2(5) . . ?
C45 C46 H46 119.4 . . ?
C47 C46 H46 119.4 . . ?
C48 C47 C46 123.1(5) . . ?
C48 C47 C52 118.5(5) . . ?
C46 C47 C52 118.5(5) . . ?
C49 C48 C47 121.1(5) . . ?
C49 C48 H48 119.5 . . ?
C47 C48 H48 119.5 . . ?
C48 C49 C50 121.0(5) . . ?
C48 C49 H49 119.5 . . ?
C50 C49 H49 119.5 . . ?
C51 C50 C49 120.7(5) . . ?
C51 C50 H50 119.7 . . ?
C49 C50 H50 119.7 . . ?
C50 C51 C52 119.6(5) . . ?
C50 C51 H51 120.2 . . ?
C52 C51 H51 120.2 . . ?
C51 C52 C43 122.0(4) . . ?
C51 C52 C47 119.2(4) . . ?
C43 C52 C47 118.8(4) . . ?
Cl3 C53 Cl1 111.1(4) . . ?
Cl3 C53 Cl2 110.2(4) . . ?
Cl1 C53 Cl2 109.9(4) . . ?
Cl3 C53 H53 108.5 . . ?
Cl1 C53 H53 108.5 . . ?
Cl2 C53 H53 108.5 . . ?
Cl5 C54 Cl4 105.8(10) . . ?
Cl5 C54 H54A 111.1 . . ?
Cl4 C54 H54A 110.8 . . ?
Cl5 C54 H54D 122.4 . . ?
Cl4 C54 H54D 131.8 . . ?
H54A C54 H54D 53.0 . . ?
Cl5' C54' Cl4' 111.0(17) . . ?
Cl5' C54' H54D 105.6 . . ?
Cl4' C54' H54D 105.2 . . ?
C19 N1 C11 112.9(4) . . ?
C19 N1 C9 121.4(4) . . ?
C11 N1 C9 122.7(4) . . ?
C19 N2 C15 112.4(4) . . ?
C19 N2 C21 122.3(4) . . ?
C15 N2 C21 121.4(3) . . ?
C20 N3 C15 111.9(4) . . ?
C20 N3 C22 122.3(4) . . ?
C15 N3 C22 122.4(4) . . ?
C20 N4 C11 112.9(4) . . ?
C20 N4 C10 123.3(4) . . ?
C11 N4 C10 121.8(4) . . ?
C12 O6 C13' 124.2(18) . . ?
C12 O6 C13 113.0(6) . . ?
C13' O6 C13 19.3(12) . . ?
C16 O8 C17 117.1(4) . . ?
C2 O9 C1 116.7(4) . . ?
C5 O10 C8 117.6(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O9 C2 C3 C4 177.8(4) . . . . ?
C7 C2 C3 C4 -0.6(7) . . . . ?
C2 C3 C4 C5 1.1(7) . . . . ?
C3 C4 C5 O10 -178.1(4) . . . . ?
C3 C4 C5 C6 -0.3(7) . . . . ?
O10 C5 C6 C7 176.8(4) . . . . ?
C4 C5 C6 C7 -1.1(7) . . . . ?
O10 C5 C6 C10 -1.0(6) . . . . ?
C4 C5 C6 C10 -178.9(4) . . . . ?
O9 C2 C7 C6 -179.3(4) . . . . ?
C3 C2 C7 C6 -0.8(7) . . . . ?
O9 C2 C7 C9 -3.3(6) . . . . ?
C3 C2 C7 C9 175.2(4) . . . . ?
C5 C6 C7 C2 1.7(7) . . . . ?
C10 C6 C7 C2 179.4(4) . . . . ?
C5 C6 C7 C9 -174.2(4) . . . . ?
C10 C6 C7 C9 3.5(7) . . . . ?
C2 C7 C9 N1 126.9(5) . . . . ?
C6 C7 C9 N1 -57.1(6) . . . . ?
C7 C6 C10 N4 54.0(6) . . . . ?
C5 C6 C10 N4 -128.3(4) . . . . ?
N1 C11 C12 O5 0.9(7) . . . . ?
N4 C11 C12 O5 128.4(5) . . . . ?
C15 C11 C12 O5 -116.1(5) . . . . ?
N1 C11 C12 O6 -176.8(4) . . . . ?
N4 C11 C12 O6 -49.3(5) . . . . ?
C15 C11 C12 O6 66.2(5) . . . . ?
N1 C11 C15 N2 -2.2(4) . . . . ?
N4 C11 C15 N2 -120.7(4) . . . . ?
C12 C11 C15 N2 119.2(4) . . . . ?
N1 C11 C15 N3 117.4(4) . . . . ?
N4 C11 C15 N3 -1.1(4) . . . . ?
C12 C11 C15 N3 -121.2(4) . . . . ?
N1 C11 C15 C16 -121.4(4) . . . . ?
N4 C11 C15 C16 120.1(4) . . . . ?
C12 C11 C15 C16 0.1(5) . . . . ?
N2 C15 C16 O7 122.9(5) . . . . ?
N3 C15 C16 O7 -4.9(7) . . . . ?
C11 C15 C16 O7 -122.0(5) . . . . ?
N2 C15 C16 O8 -55.1(5) . . . . ?
N3 C15 C16 O8 177.0(4) . . . . ?
C11 C15 C16 O8 59.9(5) . . . . ?
N3 C22 C23 C24 -60.5(5) . . . . ?
N3 C22 C23 C28 120.8(4) . . . . ?
C28 C23 C24 C25 0.3(6) . . . . ?
C22 C23 C24 C25 -178.4(4) . . . . ?
C28 C23 C24 C21 179.3(4) . . . . ?
C22 C23 C24 C21 0.5(6) . . . . ?
N2 C21 C24 C25 -119.5(4) . . . . ?
N2 C21 C24 C23 61.6(5) . . . . ?
C23 C24 C25 C26 0.3(6) . . . . ?
C21 C24 C25 C26 -178.7(4) . . . . ?
C23 C24 C25 C41 179.6(4) . . . . ?
C21 C24 C25 C41 0.6(6) . . . . ?
C24 C25 C26 C27 -0.6(7) . . . . ?
C41 C25 C26 C27 -179.9(4) . . . . ?
C25 C26 C27 C28 0.3(7) . . . . ?
C26 C27 C28 C23 0.3(7) . . . . ?
C26 C27 C28 C29 178.3(4) . . . . ?
C24 C23 C28 C27 -0.6(6) . . . . ?
C22 C23 C28 C27 178.1(4) . . . . ?
C24 C23 C28 C29 -178.6(4) . . . . ?
C22 C23 C28 C29 0.2(6) . . . . ?
C27 C28 C29 C30 7(17) . . . . ?
C23 C28 C29 C30 -175(100) . . . . ?
C28 C29 C30 C31 -122(29) . . . . ?
C29 C30 C31 C32 -57(29) . . . . ?
C29 C30 C31 C40 121(28) . . . . ?
C30 C31 C32 C33 178.9(4) . . . . ?
C40 C31 C32 C33 0.4(7) . . . . ?
C31 C32 C33 C34 -0.4(8) . . . . ?
C32 C33 C34 C35 -0.1(8) . . . . ?
C33 C34 C35 C40 0.6(8) . . . . ?
C33 C34 C35 C36 -179.1(5) . . . . ?
C34 C35 C36 C37 179.7(5) . . . . ?
C40 C35 C36 C37 -0.1(8) . . . . ?
C35 C36 C37 C38 0.9(9) . . . . ?
C36 C37 C38 C39 -1.3(9) . . . . ?
C37 C38 C39 C40 0.7(9) . . . . ?
C38 C39 C40 C35 0.2(8) . . . . ?
C38 C39 C40 C31 -179.5(5) . . . . ?
C34 C35 C40 C39 179.7(5) . . . . ?
C36 C35 C40 C39 -0.5(7) . . . . ?
C34 C35 C40 C31 -0.6(7) . . . . ?
C36 C35 C40 C31 179.1(4) . . . . ?
C32 C31 C40 C39 179.8(5) . . . . ?
C30 C31 C40 C39 1.3(7) . . . . ?
C32 C31 C40 C35 0.2(7) . . . . ?
C30 C31 C40 C35 -178.4(4) . . . . ?
C26 C25 C41 C42 -138(24) . . . . ?
C24 C25 C41 C42 43(24) . . . . ?
C25 C41 C42 C43 -59(52) . . . . ?
C41 C42 C43 C44 -91(39) . . . . ?
C41 C42 C43 C52 90(39) . . . . ?
C52 C43 C44 C45 -0.9(8) . . . . ?
C42 C43 C44 C45 -179.5(5) . . . . ?
C43 C44 C45 C46 1.5(9) . . . . ?
C44 C45 C46 C47 -0.3(9) . . . . ?
C45 C46 C47 C48 178.2(5) . . . . ?
C45 C46 C47 C52 -1.5(8) . . . . ?
C46 C47 C48 C49 179.4(5) . . . . ?
C52 C47 C48 C49 -0.9(7) . . . . ?
C47 C48 C49 C50 -0.6(9) . . . . ?
C48 C49 C50 C51 0.9(9) . . . . ?
C49 C50 C51 C52 0.2(8) . . . . ?
C50 C51 C52 C43 177.9(5) . . . . ?
C50 C51 C52 C47 -1.7(7) . . . . ?
C44 C43 C52 C51 179.4(5) . . . . ?
C42 C43 C52 C51 -2.0(7) . . . . ?
C44 C43 C52 C47 -0.9(7) . . . . ?
C42 C43 C52 C47 177.7(4) . . . . ?
C48 C47 C52 C51 2.0(7) . . . . ?
C46 C47 C52 C51 -178.3(5) . . . . ?
C48 C47 C52 C43 -177.6(4) . . . . ?
C46 C47 C52 C43 2.1(7) . . . . ?
O1 C19 N1 C11 -171.2(4) . . . . ?
N2 C19 N1 C11 10.9(5) . . . . ?
O1 C19 N1 C9 -10.1(7) . . . . ?
N2 C19 N1 C9 172.0(4) . . . . ?
N4 C11 N1 C19 105.0(4) . . . . ?
C12 C11 N1 C19 -129.3(4) . . . . ?
C15 C11 N1 C19 -5.2(5) . . . . ?
N4 C11 N1 C9 -55.8(6) . . . . ?
C12 C11 N1 C9 69.9(5) . . . . ?
C15 C11 N1 C9 -166.0(4) . . . . ?
C7 C9 N1 C19 -88.0(5) . . . . ?
C7 C9 N1 C11 71.2(6) . . . . ?
O1 C19 N2 C15 169.6(4) . . . . ?
N1 C19 N2 C15 -12.5(5) . . . . ?
O1 C19 N2 C21 11.5(6) . . . . ?
N1 C19 N2 C21 -170.6(3) . . . . ?
N3 C15 N2 C19 -102.9(4) . . . . ?
C16 C15 N2 C19 131.1(4) . . . . ?
C11 C15 N2 C19 9.0(4) . . . . ?
N3 C15 N2 C21 55.4(5) . . . . ?
C16 C15 N2 C21 -70.6(5) . . . . ?
C11 C15 N2 C21 167.3(4) . . . . ?
C24 C21 N2 C19 77.2(5) . . . . ?
C24 C21 N2 C15 -78.9(5) . . . . ?
O2 C20 N3 C15 -173.0(4) . . . . ?
N4 C20 N3 C15 9.0(5) . . . . ?
O2 C20 N3 C22 -13.5(7) . . . . ?
N4 C20 N3 C22 168.5(4) . . . . ?
N2 C15 N3 C20 106.6(4) . . . . ?
C16 C15 N3 C20 -128.0(4) . . . . ?
C11 C15 N3 C20 -4.7(5) . . . . ?
N2 C15 N3 C22 -52.8(5) . . . . ?
C16 C15 N3 C22 72.6(5) . . . . ?
C11 C15 N3 C22 -164.1(4) . . . . ?
C23 C22 N3 C20 -83.1(5) . . . . ?
C23 C22 N3 C15 74.2(5) . . . . ?
O2 C20 N4 C11 172.1(4) . . . . ?
N3 C20 N4 C11 -9.9(5) . . . . ?
O2 C20 N4 C10 8.4(7) . . . . ?
N3 C20 N4 C10 -173.7(4) . . . . ?
N1 C11 N4 C20 -104.0(4) . . . . ?
C12 C11 N4 C20 129.9(4) . . . . ?
C15 C11 N4 C20 6.7(5) . . . . ?
N1 C11 N4 C10 60.0(6) . . . . ?
C12 C11 N4 C10 -66.1(5) . . . . ?
C15 C11 N4 C10 170.7(4) . . . . ?
C6 C10 N4 C20 85.9(5) . . . . ?
C6 C10 N4 C11 -76.4(5) . . . . ?
O5 C12 O6 C13' -13.4(15) . . . . ?
C11 C12 O6 C13' 164.2(14) . . . . ?
O5 C12 O6 C13 4.5(11) . . . . ?
C11 C12 O6 C13 -177.8(9) . . . . ?
C14' C13' O6 C12 77(3) . . . . ?
C14' C13' O6 C13 18(5) . . . . ?
C14 C13 O6 C12 -164.2(9) . . . . ?
C14 C13 O6 C13' -35(6) . . . . ?
O7 C16 O8 C17 0.1(8) . . . . ?
C15 C16 O8 C17 178.1(4) . . . . ?
C18 C17 O8 C16 -156.9(4) . . . . ?
C7 C2 O9 C1 179.5(5) . . . . ?
C3 C2 O9 C1 1.1(7) . . . . ?
C4 C5 O10 C8 2.5(7) . . . . ?
C6 C5 O10 C8 -175.4(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        23.09
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         0.962
_refine_diff_density_min         -0.948
_refine_diff_density_rms         0.092
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_e:\130228a\work\mo_130228a_0m
_database_code_depnum_ccdc_archive 'CCDC 996879'
_audit_update_record             
;
2014-04-11 deposited with the CCDC.
2015-02-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C49 H43 Cl3 N4 O8'
_chemical_formula_weight         922.22

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                   10.9368(13)
_cell_length_b                   14.8456(18)
_cell_length_c                   15.7583(19)
_cell_angle_alpha                71.070(2)
_cell_angle_beta                 89.029(2)
_cell_angle_gamma                69.365(2)
_cell_volume                     2251.2(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2625
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      22.67

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      1.361
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             960
_exptl_absorpt_coefficient_mu    0.263
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  0.9691
_exptl_absorpt_correction_T_max  0.9742
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14305
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0543
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.37
_diffrn_reflns_theta_max         23.89
_reflns_number_total             6825
_reflns_number_gt                3976
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0897P)²+0.5710P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6825
_refine_ls_number_parameters     723
_refine_ls_number_restraints     44
_refine_ls_R_factor_all          0.1059
_refine_ls_R_factor_gt           0.0565
_refine_ls_wR_factor_ref         0.1818
_refine_ls_wR_factor_gt          0.1485
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4671(3) 0.0223(2) 0.3067(2) 0.0531(9) Uani 1 1 d . A .
C2 C 0.5156(4) 0.0495(3) 0.3718(2) 0.0637(10) Uani 1 1 d . . .
H2 H 0.5864 0.0014 0.4135 0.076 Uiso 1 1 calc R . .
C3 C 0.4595(4) 0.1471(3) 0.3750(2) 0.0626(10) Uani 1 1 d . A .
H3 H 0.4941 0.1638 0.4188 0.075 Uiso 1 1 calc R . .
C4 C 0.3538(3) 0.2207(2) 0.3153(2) 0.0516(8) Uani 1 1 d D . .
C5 C 0.2984(3) 0.1930(2) 0.2522(2) 0.0466(8) Uani 1 1 d . A .
C6 C 0.3556(3) 0.0938(2) 0.2475(2) 0.0464(8) Uani 1 1 d . . .
C7 C 0.5414(3) -0.0811(3) 0.3003(2) 0.0559(9) Uani 1 1 d . . .
C8 C 0.5607(4) -0.1674(3) 0.3718(3) 0.0684(11) Uani 1 1 d . A .
H8 H 0.5267 -0.1617 0.4251 0.082 Uiso 1 1 calc R . .
C9 C 0.6313(4) -0.2665(3) 0.3677(3) 0.0743(12) Uani 1 1 d . . .
C10 C 0.6825(4) -0.2743(3) 0.2875(3) 0.0789(12) Uani 1 1 d . A .
C11 C 0.6667(4) -0.1851(4) 0.2157(3) 0.0838(13) Uani 1 1 d . . .
H11 H 0.7029 -0.1897 0.1627 0.101 Uiso 1 1 calc R A .
C12 C 0.5996(4) -0.0916(3) 0.2216(3) 0.0693(11) Uani 1 1 d . A .
H12 H 0.5917 -0.0332 0.1730 0.083 Uiso 1 1 calc R . .
C13 C 0.6509(6) -0.3562(3) 0.4421(3) 0.1044(17) Uani 1 1 d . A .
H13 H 0.6198 -0.3509 0.4963 0.125 Uiso 1 1 calc R . .
C14 C 0.7148(6) -0.4503(4) 0.4356(4) 0.126(2) Uani 1 1 d . . .
H14 H 0.7268 -0.5087 0.4854 0.151 Uiso 1 1 calc R A .
C15 C 0.7614(6) -0.4597(4) 0.3564(5) 0.129(2) Uani 1 1 d . A .
H15 H 0.8026 -0.5245 0.3524 0.155 Uiso 1 1 calc R . .
C16 C 0.7480(5) -0.3748(4) 0.2832(4) 0.1137(19) Uani 1 1 d . . .
H16 H 0.7818 -0.3824 0.2304 0.136 Uiso 1 1 calc R A .
C17 C 0.3023(11) 0.3304(6) 0.3165(14) 0.049(3) Uani 0.675(6) 1 d PGD A 1
C18 C 0.3926(8) 0.3788(6) 0.3017(10) 0.061(2) Uani 0.675(6) 1 d PG A 1
H18 H 0.4778 0.3446 0.2917 0.073 Uiso 0.675(6) 1 calc PR A 1
C19 C 0.3555(7) 0.4785(5) 0.3017(7) 0.061(2) Uani 0.675(6) 1 d PGD A 1
C20 C 0.2281(7) 0.5297(3) 0.3166(6) 0.061(3) Uani 0.675(6) 1 d PGD A 1
C21 C 0.1378(6) 0.4813(6) 0.3314(8) 0.062(3) Uani 0.675(6) 1 d PG A 1
H21 H 0.0526 0.5156 0.3414 0.074 Uiso 0.675(6) 1 calc PR A 1
C22 C 0.1749(10) 0.3816(7) 0.3314(13) 0.061(3) Uani 0.675(6) 1 d PG A 1
H22 H 0.1144 0.3492 0.3413 0.074 Uiso 0.675(6) 1 calc PR A 1
C23 C 0.4459(7) 0.5291(5) 0.2852(5) 0.095(2) Uani 0.675(6) 1 d PD A 1
H23 H 0.5317 0.4946 0.2764 0.114 Uiso 0.675(6) 1 calc PR A 1
C24 C 0.4083(9) 0.6283(5) 0.2822(5) 0.110(3) Uani 0.675(6) 1 d PD A 1
H24 H 0.4692 0.6603 0.2722 0.132 Uiso 0.675(6) 1 calc PR A 1
C25 C 0.2810(10) 0.6814(6) 0.2939(6) 0.100(3) Uani 0.675(6) 1 d PD A 1
H25 H 0.2557 0.7499 0.2888 0.120 Uiso 0.675(6) 1 calc PR A 1
C26 C 0.1925(10) 0.6343(6) 0.3127(7) 0.086(4) Uani 0.675(6) 1 d PD A 1
H26 H 0.1082 0.6698 0.3232 0.104 Uiso 0.675(6) 1 calc PR A 1
C27 C 0.3056(3) 0.0644(2) 0.1755(2) 0.0516(9) Uani 1 1 d . A .
H27A H 0.3243 0.1030 0.1176 0.062 Uiso 1 1 calc R . .
H27B H 0.3558 -0.0075 0.1861 0.062 Uiso 1 1 calc R . .
C28 C 0.1836(3) 0.2732(2) 0.1832(2) 0.0519(9) Uani 1 1 d . . .
H28A H 0.1577 0.3364 0.1963 0.062 Uiso 1 1 calc R A .
H28B H 0.2144 0.2862 0.1239 0.062 Uiso 1 1 calc R . .
C29 C 0.1179(4) 0.0093(3) 0.2227(2) 0.0513(9) Uani 1 1 d . A .
C30 C -0.0355(3) 0.2690(2) 0.2281(2) 0.0509(8) Uani 1 1 d . . .
C31 C 0.0646(3) 0.1794(2) 0.1323(2) 0.0466(8) Uani 1 1 d . . .
C32 C 0.0683(4) 0.2297(3) 0.0304(2) 0.0546(9) Uani 1 1 d . A .
C33 C -0.0438(5) 0.3787(3) -0.0951(2) 0.0892(14) Uani 1 1 d . A .
H33A H -0.1359 0.4159 -0.1179 0.107 Uiso 1 1 calc R . .
H33B H -0.0051 0.3341 -0.1296 0.107 Uiso 1 1 calc R . .
C34 C 0.0232(6) 0.4509(3) -0.1059(3) 0.1097(18) Uani 1 1 d . . .
H34A H -0.0129 0.4931 -0.0697 0.165 Uiso 1 1 calc R . .
H34B H 0.0110 0.4933 -0.1681 0.165 Uiso 1 1 calc R . .
H34C H 0.1154 0.4137 -0.0868 0.165 Uiso 1 1 calc R . .
C35 C -0.0641(3) 0.1599(2) 0.1586(2) 0.0496(8) Uani 1 1 d . A .
C36 C -0.1611(4) 0.1820(3) 0.0782(3) 0.0609(10) Uani 1 1 d D . .
C37 C -0.1813(11) 0.1349(11) -0.0497(7) 0.111(3) Uani 0.872(14) 1 d PD A 1
H37A H -0.2339 0.2067 -0.0796 0.133 Uiso 0.872(14) 1 calc PR A 1
H37B H -0.1236 0.1113 -0.0917 0.133 Uiso 0.872(14) 1 calc PR A 1
C38 C -0.2675(9) 0.0772(6) -0.0255(6) 0.132(3) Uani 0.872(14) 1 d PD A 1
H38A H -0.2156 0.0057 0.0023 0.197 Uiso 0.872(14) 1 calc PR A 1
H38B H -0.3190 0.0872 -0.0788 0.197 Uiso 0.872(14) 1 calc PR A 1
H38C H -0.3248 0.1005 0.0161 0.197 Uiso 0.872(14) 1 calc PR A 1
O5 O -0.2697(6) 0.2444(6) 0.0607(6) 0.077(2) Uani 0.872(14) 1 d PD A 1
O6 O -0.1024(7) 0.1236(5) 0.0294(5) 0.072(2) Uani 0.872(14) 1 d PD A 1
C37' C -0.201(9) 0.117(14) -0.022(4) 0.25(7) Uani 0.128(14) 1 d PD A 2
H37C H -0.2858 0.1703 -0.0271 0.295 Uiso 0.128(14) 1 calc PR A 2
H37D H -0.2153 0.0555 -0.0200 0.295 Uiso 0.128(14) 1 calc PR A 2
C38' C -0.134(7) 0.149(5) -0.101(3) 0.13(2) Uani 0.128(14) 1 d PD A 2
H38D H -0.1349 0.2162 -0.1104 0.197 Uiso 0.128(14) 1 calc PR A 2
H38E H -0.1786 0.1495 -0.1537 0.197 Uiso 0.128(14) 1 calc PR A 2
H38F H -0.0447 0.1016 -0.0921 0.197 Uiso 0.128(14) 1 calc PR A 2
O5' O -0.266(5) 0.250(6) 0.069(7) 0.16(4) Uani 0.128(14) 1 d PD A 2
O6' O -0.125(5) 0.098(2) 0.059(2) 0.061(12) Uani 0.128(14) 1 d PD A 2
C39 C -0.1002(4) 0.0023(3) 0.2609(3) 0.0671(10) Uani 1 1 d . A .
H39A H -0.0568 -0.0709 0.2748 0.081 Uiso 1 1 calc R . .
H39B H -0.1808 0.0243 0.2222 0.081 Uiso 1 1 calc R . .
C40 C -0.2252(4) 0.2155(3) 0.2657(2) 0.0636(10) Uani 1 1 d . . .
H40A H -0.2945 0.2145 0.2288 0.076 Uiso 1 1 calc R A .
H40B H -0.2613 0.2760 0.2830 0.076 Uiso 1 1 calc R . .
C41 C -0.1354(4) 0.0231(3) 0.3482(2) 0.0640(10) Uani 1 1 d . . .
C42 C -0.1887(4) 0.1225(3) 0.3503(2) 0.0624(10) Uani 1 1 d . A .
C43 C -0.2176(4) 0.1365(4) 0.4335(3) 0.0776(12) Uani 1 1 d . . .
C44 C -0.1943(5) 0.0534(5) 0.5112(3) 0.0926(15) Uani 1 1 d . A .
H44 H -0.2126 0.0634 0.5660 0.111 Uiso 1 1 calc R . .
C45 C -0.1439(5) -0.0443(5) 0.5079(3) 0.0936(15) Uani 1 1 d . . .
H45 H -0.1293 -0.1001 0.5606 0.112 Uiso 1 1 calc R A .
C46 C -0.1151(4) -0.0600(4) 0.4272(3) 0.0784(12) Uani 1 1 d . A .
C47 C -0.0710(7) -0.2396(4) 0.4901(4) 0.140(2) Uani 1 1 d . A .
H47A H -0.0171 -0.2495 0.5422 0.210 Uiso 1 1 calc R . .
H47B H -0.0394 -0.3001 0.4736 0.210 Uiso 1 1 calc R . .
H47C H -0.1602 -0.2267 0.5037 0.210 Uiso 1 1 calc R . .
C48 C -0.2810(6) 0.2574(5) 0.5111(3) 0.126(2) Uani 1 1 d . . .
H48A H -0.3243 0.2181 0.5521 0.188 Uiso 1 1 calc R A .
H48B H -0.3295 0.3290 0.4987 0.188 Uiso 1 1 calc R . .
H48C H -0.1937 0.2397 0.5378 0.188 Uiso 1 1 calc R . .
C17' C 0.334(2) 0.3253(14) 0.319(3) 0.060(9) Uani 0.325(6) 1 d PGD A 2
C18' C 0.2100(18) 0.3892(14) 0.328(3) 0.051(5) Uani 0.325(6) 1 d PG A 2
H18' H 0.1402 0.3664 0.3352 0.061 Uiso 0.325(6) 1 calc PR A 2
C19' C 0.1908(11) 0.4870(11) 0.3277(16) 0.060(5) Uani 0.325(6) 1 d PGD A 2
C20' C 0.2952(13) 0.5211(7) 0.3174(14) 0.058(6) Uani 0.325(6) 1 d PGD A 2
C21' C 0.4188(12) 0.4573(12) 0.3077(17) 0.075(6) Uani 0.325(6) 1 d PG A 2
H21' H 0.4886 0.4800 0.3008 0.090 Uiso 0.325(6) 1 calc PR A 2
C22' C 0.4379(16) 0.3594(15) 0.308(3) 0.088(8) Uani 0.325(6) 1 d PG A 2
H22' H 0.5206 0.3167 0.3018 0.106 Uiso 0.325(6) 1 calc PR A 2
C23' C 0.0664(12) 0.5504(9) 0.3361(9) 0.081(4) Uani 0.325(6) 1 d PD A 2
H23' H -0.0024 0.5264 0.3451 0.097 Uiso 0.325(6) 1 calc PR A 2
C24' C 0.0457(14) 0.6499(8) 0.3311(9) 0.092(5) Uani 0.325(6) 1 d PD A 2
H24' H -0.0368 0.6926 0.3380 0.110 Uiso 0.325(6) 1 calc PR A 2
C25' C 0.1483(17) 0.6854(11) 0.3157(13) 0.092(6) Uani 0.325(6) 1 d PD A 2
H25' H 0.1325 0.7531 0.3097 0.111 Uiso 0.325(6) 1 calc PR A 2
C26' C 0.2732(19) 0.6230(12) 0.309(2) 0.120(10) Uani 0.325(6) 1 d PD A 2
H26' H 0.3413 0.6477 0.2990 0.144 Uiso 0.325(6) 1 calc PR A 2
C49 C 0.4339(12) 0.3955(7) 0.9801(6) 0.093(4) Uani 0.802(5) 1 d PD B 1
H49 H 0.5248 0.3889 0.9699 0.112 Uiso 0.802(5) 1 calc PR B 1
Cl1 Cl 0.4073(2) 0.29242(15) 0.96667(19) 0.1290(11) Uani 0.802(5) 1 d PD B 1
Cl2 Cl 0.4107(2) 0.3939(2) 1.09034(15) 0.1388(12) Uani 0.802(5) 1 d PD B 1
Cl3 Cl 0.3296(2) 0.51138(16) 0.9068(2) 0.1478(11) Uani 0.802(5) 1 d PD B 1
C49' C 0.462(3) 0.3775(17) 0.9927(14) 0.089(17) Uani 0.198(5) 1 d PD B 2
H49' H 0.5419 0.3899 1.0032 0.107 Uiso 0.198(5) 1 calc PR B 2
Cl1' Cl 0.4647(16) 0.3568(14) 0.8917(9) 0.251(9) Uani 0.198(5) 1 d PD B 2
Cl2' Cl 0.4556(12) 0.2783(11) 1.0846(9) 0.206(7) Uani 0.198(5) 1 d PD B 2
Cl3' Cl 0.3283(10) 0.4811(9) 0.9958(11) 0.165(6) Uani 0.198(5) 1 d PD B 2
N1 N 0.1670(3) 0.07962(19) 0.16844(17) 0.0475(7) Uani 1 1 d . A .
N2 N -0.0157(3) 0.0529(2) 0.21159(18) 0.0536(7) Uani 1 1 d . . .
N3 N 0.0686(3) 0.24761(18) 0.17928(17) 0.0461(7) Uani 1 1 d . A .
N4 N -0.1200(3) 0.2262(2) 0.21004(18) 0.0534(7) Uani 1 1 d . A .
O1 O 0.1850(3) -0.07746(18) 0.26941(16) 0.0688(7) Uani 1 1 d . . .
O2 O -0.0515(2) 0.31965(18) 0.27755(16) 0.0662(7) Uani 1 1 d . A .
O3 O 0.1501(3) 0.1946(2) -0.01285(17) 0.0789(8) Uani 1 1 d . . .
O4 O -0.0318(3) 0.31734(19) 0.00021(15) 0.0756(8) Uani 1 1 d . . .
O7 O -0.0656(4) -0.1552(3) 0.4175(2) 0.1034(10) Uani 1 1 d . . .
O8 O -0.2741(3) 0.2361(3) 0.4304(2) 0.1000(10) Uani 1 1 d . A .


_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
C1 C2 1.391(5) . ?
C1 C6 1.403(4) . ?
C1 C7 1.499(4) . ?
C2 C3 1.378(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.377(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.409(4) . ?
C4 C17' 1.508(8) . ?
C4 C17 1.530(5) . ?
C5 C6 1.408(4) . ?
C5 C28 1.527(4) . ?
C6 C27 1.513(4) . ?
C7 C8 1.356(5) . ?
C7 C12 1.411(5) . ?
C8 C9 1.422(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.397(6) . ?
C9 C13 1.409(6) . ?
C10 C11 1.391(6) . ?
C10 C16 1.432(6) . ?
C11 C12 1.356(5) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C14 1.362(6) . ?
C13 H13 0.9300 . ?
C14 C15 1.371(8) . ?
C14 H14 0.9300 . ?
C15 C16 1.369(8) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 C18 1.3900 . ?
C17 C22 1.3900 . ?
C18 C19 1.3900 . ?
C18 H18 0.9300 . ?
C19 C20 1.3900 . ?
C19 C23 1.413(7) . ?
C20 C21 1.3900 . ?
C20 C26 1.441(7) . ?
C21 C22 1.3900 . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 C24 1.367(7) . ?
C23 H23 0.9300 . ?
C24 C25 1.381(8) . ?
C24 H24 0.9300 . ?
C25 C26 1.360(8) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 N1 1.451(4) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 N3 1.444(4) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 O1 1.215(4) . ?
C29 N2 1.361(4) . ?
C29 N1 1.382(4) . ?
C30 O2 1.218(4) . ?
C30 N3 1.365(4) . ?
C30 N4 1.372(4) . ?
C31 N1 1.442(4) . ?
C31 N3 1.447(4) . ?
C31 C32 1.541(5) . ?
C31 C35 1.559(5) . ?
C32 O3 1.191(4) . ?
C32 O4 1.315(4) . ?
C33 O4 1.461(4) . ?
C33 C34 1.466(6) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 N2 1.436(4) . ?
C35 N4 1.440(4) . ?
C35 C36 1.540(5) . ?
C36 O5 1.189(5) . ?
C36 O5' 1.20(2) . ?
C36 O6' 1.310(19) . ?
C36 O6 1.333(6) . ?
C37 C38 1.454(13) . ?
C37 O6 1.457(8) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C37' O6' 1.424(15) . ?
C37' C38' 1.465(17) . ?
C37' H37C 0.9700 . ?
C37' H37D 0.9700 . ?
C38' H38D 0.9600 . ?
C38' H38E 0.9600 . ?
C38' H38F 0.9600 . ?
C39 N2 1.451(4) . ?
C39 C41 1.520(5) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C40 N4 1.456(4) . ?
C40 C42 1.511(5) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C41 C46 1.392(5) . ?
C41 C42 1.394(5) . ?
C42 C43 1.405(5) . ?
C43 O8 1.372(5) . ?
C43 C44 1.376(6) . ?
C44 C45 1.377(7) . ?
C44 H44 0.9300 . ?
C45 C46 1.378(6) . ?
C45 H45 0.9300 . ?
C46 O7 1.382(5) . ?
C47 O7 1.415(5) . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C48 O8 1.402(5) . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C17' C18' 1.3900 . ?
C17' C22' 1.3900 . ?
C18' C19' 1.3900 . ?
C18' H18' 0.9300 . ?
C19' C23' 1.388(9) . ?
C19' C20' 1.3900 . ?
C20' C21' 1.3900 . ?
C20' C26' 1.406(10) . ?
C21' C22' 1.3900 . ?
C21' H21' 0.9300 . ?
C22' H22' 0.9300 . ?
C23' C24' 1.389(9) . ?
C23' H23' 0.9300 . ?
C24' C25' 1.386(9) . ?
C24' H24' 0.9300 . ?
C25' C26' 1.380(10) . ?
C25' H25' 0.9300 . ?
C26' H26' 0.9300 . ?
C49 Cl3 1.722(11) . ?
C49 Cl1 1.731(10) . ?
C49 Cl2 1.745(8) . ?
C49 H49 0.9800 . ?
C49' Cl1' 1.71(2) . ?
C49' Cl2' 1.72(2) . ?
C49' Cl3' 1.72(2) . ?
C49' H49' 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C6 119.1(3) . . ?
C2 C1 C7 117.9(3) . . ?
C6 C1 C7 122.9(3) . . ?
C3 C2 C1 120.5(3) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C4 C3 C2 121.9(3) . . ?
C4 C3 H3 119.1 . . ?
C2 C3 H3 119.1 . . ?
C3 C4 C5 118.4(3) . . ?
C3 C4 C17' 110.7(14) . . ?
C5 C4 C17' 129.9(16) . . ?
C3 C4 C17 119.9(7) . . ?
C5 C4 C17 121.7(7) . . ?
C17' C4 C17 12.2(12) . . ?
C6 C5 C4 120.3(3) . . ?
C6 C5 C28 119.6(3) . . ?
C4 C5 C28 119.9(3) . . ?
C1 C6 C5 119.6(3) . . ?
C1 C6 C27 118.7(3) . . ?
C5 C6 C27 121.5(3) . . ?
C8 C7 C12 117.9(3) . . ?
C8 C7 C1 120.7(3) . . ?
C12 C7 C1 121.3(3) . . ?
C7 C8 C9 121.9(4) . . ?
C7 C8 H8 119.0 . . ?
C9 C8 H8 119.0 . . ?
C10 C9 C13 119.5(4) . . ?
C10 C9 C8 118.6(4) . . ?
C13 C9 C8 121.8(4) . . ?
C11 C10 C9 118.9(3) . . ?
C11 C10 C16 123.3(4) . . ?
C9 C10 C16 117.8(4) . . ?
C12 C11 C10 121.2(4) . . ?
C12 C11 H11 119.4 . . ?
C10 C11 H11 119.4 . . ?
C11 C12 C7 121.3(4) . . ?
C11 C12 H12 119.3 . . ?
C7 C12 H12 119.3 . . ?
C14 C13 C9 120.9(5) . . ?
C14 C13 H13 119.6 . . ?
C9 C13 H13 119.6 . . ?
C13 C14 C15 120.5(5) . . ?
C13 C14 H14 119.8 . . ?
C15 C14 H14 119.8 . . ?
C16 C15 C14 120.7(5) . . ?
C16 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
C15 C16 C10 120.5(5) . . ?
C15 C16 H16 119.7 . . ?
C10 C16 H16 119.7 . . ?
C18 C17 C22 120.0 . . ?
C18 C17 C4 115.5(6) . . ?
C22 C17 C4 124.5(6) . . ?
C17 C18 C19 120.0 . . ?
C17 C18 H18 120.0 . . ?
C19 C18 H18 120.0 . . ?
C18 C19 C20 120.0 . . ?
C18 C19 C23 120.5(6) . . ?
C20 C19 C23 119.5(6) . . ?
C21 C20 C19 120.0 . . ?
C21 C20 C26 121.8(6) . . ?
C19 C20 C26 118.2(6) . . ?
C22 C21 C20 120.0 . . ?
C22 C21 H21 120.0 . . ?
C20 C21 H21 120.0 . . ?
C21 C22 C17 120.0 . . ?
C21 C22 H22 120.0 . . ?
C17 C22 H22 120.0 . . ?
C24 C23 C19 120.6(6) . . ?
C24 C23 H23 119.7 . . ?
C19 C23 H23 119.7 . . ?
C23 C24 C25 120.7(7) . . ?
C23 C24 H24 119.6 . . ?
C25 C24 H24 119.6 . . ?
C26 C25 C24 120.3(7) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C25 C26 C20 120.6(8) . . ?
C25 C26 H26 119.7 . . ?
C20 C26 H26 119.7 . . ?
N1 C27 C6 117.3(3) . . ?
N1 C27 H27A 108.0 . . ?
C6 C27 H27A 108.0 . . ?
N1 C27 H27B 108.0 . . ?
C6 C27 H27B 108.0 . . ?
H27A C27 H27B 107.2 . . ?
N3 C28 C5 116.1(3) . . ?
N3 C28 H28A 108.3 . . ?
C5 C28 H28A 108.3 . . ?
N3 C28 H28B 108.3 . . ?
C5 C28 H28B 108.3 . . ?
H28A C28 H28B 107.4 . . ?
O1 C29 N2 127.0(3) . . ?
O1 C29 N1 124.5(3) . . ?
N2 C29 N1 108.4(3) . . ?
O2 C30 N3 125.6(3) . . ?
O2 C30 N4 126.1(3) . . ?
N3 C30 N4 108.3(3) . . ?
N1 C31 N3 112.8(2) . . ?
N1 C31 C32 111.7(3) . . ?
N3 C31 C32 109.8(3) . . ?
N1 C31 C35 104.1(2) . . ?
N3 C31 C35 102.9(2) . . ?
C32 C31 C35 115.2(3) . . ?
O3 C32 O4 126.1(3) . . ?
O3 C32 C31 124.9(3) . . ?
O4 C32 C31 109.0(3) . . ?
O4 C33 C34 109.9(4) . . ?
O4 C33 H33A 109.7 . . ?
C34 C33 H33A 109.7 . . ?
O4 C33 H33B 109.7 . . ?
C34 C33 H33B 109.7 . . ?
H33A C33 H33B 108.2 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N2 C35 N4 113.9(3) . . ?
N2 C35 C36 110.3(3) . . ?
N4 C35 C36 111.5(3) . . ?
N2 C35 C31 102.6(3) . . ?
N4 C35 C31 103.4(2) . . ?
C36 C35 C31 114.7(3) . . ?
O5 C36 O5' 9(4) . . ?
O5 C36 O6' 124(3) . . ?
O5' C36 O6' 132(4) . . ?
O5 C36 O6 125.5(6) . . ?
O5' C36 O6 134(4) . . ?
O6' C36 O6 26.6(17) . . ?
O5 C36 C35 125.0(4) . . ?
O5' C36 C35 116(4) . . ?
O6' C36 C35 106(2) . . ?
O6 C36 C35 109.4(5) . . ?
C38 C37 O6 111.6(9) . . ?
C38 C37 H37A 109.3 . . ?
O6 C37 H37A 109.3 . . ?
C38 C37 H37B 109.3 . . ?
O6 C37 H37B 109.3 . . ?
H37A C37 H37B 108.0 . . ?
C36 O6 C37 116.4(7) . . ?
O6' C37' C38' 111(3) . . ?
O6' C37' H37C 109.4 . . ?
C38' C37' H37C 109.4 . . ?
O6' C37' H37D 109.4 . . ?
C38' C37' H37D 109.4 . . ?
H37C C37' H37D 108.0 . . ?
C37' C38' H38D 109.5 . . ?
C37' C38' H38E 109.5 . . ?
H38D C38' H38E 109.5 . . ?
C37' C38' H38F 109.5 . . ?
H38D C38' H38F 109.5 . . ?
H38E C38' H38F 109.5 . . ?
C36 O6' C37' 109(8) . . ?
N2 C39 C41 114.4(3) . . ?
N2 C39 H39A 108.7 . . ?
C41 C39 H39A 108.7 . . ?
N2 C39 H39B 108.7 . . ?
C41 C39 H39B 108.7 . . ?
H39A C39 H39B 107.6 . . ?
N4 C40 C42 116.6(3) . . ?
N4 C40 H40A 108.1 . . ?
C42 C40 H40A 108.1 . . ?
N4 C40 H40B 108.1 . . ?
C42 C40 H40B 108.1 . . ?
H40A C40 H40B 107.3 . . ?
C46 C41 C42 119.9(4) . . ?
C46 C41 C39 118.5(4) . . ?
C42 C41 C39 121.6(3) . . ?
C41 C42 C43 118.8(4) . . ?
C41 C42 C40 122.3(3) . . ?
C43 C42 C40 118.8(4) . . ?
O8 C43 C44 123.6(4) . . ?
O8 C43 C42 115.9(4) . . ?
C44 C43 C42 120.5(5) . . ?
C43 C44 C45 120.2(5) . . ?
C43 C44 H44 119.9 . . ?
C45 C44 H44 119.9 . . ?
C44 C45 C46 120.4(4) . . ?
C44 C45 H45 119.8 . . ?
C46 C45 H45 119.8 . . ?
C45 C46 O7 124.4(4) . . ?
C45 C46 C41 120.1(5) . . ?
O7 C46 C41 115.5(4) . . ?
O7 C47 H47A 109.5 . . ?
O7 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
O7 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
O8 C48 H48A 109.5 . . ?
O8 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
O8 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C18' C17' C22' 120.0 . . ?
C18' C17' C4 120.3(14) . . ?
C22' C17' C4 119.7(14) . . ?
C19' C18' C17' 120.0 . . ?
C19' C18' H18' 120.0 . . ?
C17' C18' H18' 120.0 . . ?
C23' C19' C18' 119.3(11) . . ?
C23' C19' C20' 120.7(11) . . ?
C18' C19' C20' 120.0 . . ?
C19' C20' C21' 120.0 . . ?
C19' C20' C26' 119.9(12) . . ?
C21' C20' C26' 119.9(13) . . ?
C22' C21' C20' 120.0 . . ?
C22' C21' H21' 120.0 . . ?
C20' C21' H21' 120.0 . . ?
C21' C22' C17' 120.0 . . ?
C21' C22' H22' 120.0 . . ?
C17' C22' H22' 120.0 . . ?
C19' C23' C24' 119.3(10) . . ?
C19' C23' H23' 120.3 . . ?
C24' C23' H23' 120.3 . . ?
C25' C24' C23' 119.8(10) . . ?
C25' C24' H24' 120.1 . . ?
C23' C24' H24' 120.1 . . ?
C26' C25' C24' 121.7(11) . . ?
C26' C25' H25' 119.2 . . ?
C24' C25' H25' 119.2 . . ?
C25' C26' C20' 118.5(13) . . ?
C25' C26' H26' 120.8 . . ?
C20' C26' H26' 120.8 . . ?
Cl3 C49 Cl1 112.8(6) . . ?
Cl3 C49 Cl2 108.5(5) . . ?
Cl1 C49 Cl2 109.1(5) . . ?
Cl3 C49 H49 108.8 . . ?
Cl1 C49 H49 108.8 . . ?
Cl2 C49 H49 108.8 . . ?
Cl1' C49' Cl2' 115.0(17) . . ?
Cl1' C49' Cl3' 113.4(17) . . ?
Cl2' C49' Cl3' 103.8(14) . . ?
Cl1' C49' H49' 108.1 . . ?
Cl2' C49' H49' 108.1 . . ?
Cl3' C49' H49' 108.1 . . ?
C29 N1 C31 110.8(3) . . ?
C29 N1 C27 122.5(3) . . ?
C31 N1 C27 122.9(3) . . ?
C29 N2 C35 113.0(3) . . ?
C29 N2 C39 123.6(3) . . ?
C35 N2 C39 122.5(3) . . ?
C30 N3 C28 126.0(3) . . ?
C30 N3 C31 112.6(3) . . ?
C28 N3 C31 120.7(3) . . ?
C30 N4 C35 112.1(3) . . ?
C30 N4 C40 121.7(3) . . ?
C35 N4 C40 121.8(3) . . ?
C32 O4 C33 117.5(3) . . ?
C46 O7 C47 117.5(4) . . ?
C43 O8 C48 119.2(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -3.6(5) . . . . ?
C7 C1 C2 C3 173.3(3) . . . . ?
C1 C2 C3 C4 0.6(6) . . . . ?
C2 C3 C4 C5 3.1(5) . . . . ?
C2 C3 C4 C17' -166.1(15) . . . . ?
C2 C3 C4 C17 -174.9(7) . . . . ?
C3 C4 C5 C6 -3.8(5) . . . . ?
C17' C4 C5 C6 163.0(16) . . . . ?
C17 C4 C5 C6 174.2(7) . . . . ?
C3 C4 C5 C28 -178.3(3) . . . . ?
C17' C4 C5 C28 -11.5(16) . . . . ?
C17 C4 C5 C28 -0.3(8) . . . . ?
C2 C1 C6 C5 2.8(5) . . . . ?
C7 C1 C6 C5 -173.9(3) . . . . ?
C2 C1 C6 C27 178.5(3) . . . . ?
C7 C1 C6 C27 1.8(5) . . . . ?
C4 C5 C6 C1 0.8(5) . . . . ?
C28 C5 C6 C1 175.3(3) . . . . ?
C4 C5 C6 C27 -174.8(3) . . . . ?
C28 C5 C6 C27 -0.3(5) . . . . ?
C2 C1 C7 C8 59.5(5) . . . . ?
C6 C1 C7 C8 -123.7(4) . . . . ?
C2 C1 C7 C12 -117.0(4) . . . . ?
C6 C1 C7 C12 59.8(5) . . . . ?
C12 C7 C8 C9 -3.1(6) . . . . ?
C1 C7 C8 C9 -179.7(3) . . . . ?
C7 C8 C9 C10 0.3(6) . . . . ?
C7 C8 C9 C13 -179.8(4) . . . . ?
C13 C9 C10 C11 -177.6(4) . . . . ?
C8 C9 C10 C11 2.3(6) . . . . ?
C13 C9 C10 C16 2.9(7) . . . . ?
C8 C9 C10 C16 -177.2(4) . . . . ?
C9 C10 C11 C12 -2.0(7) . . . . ?
C16 C10 C11 C12 177.5(4) . . . . ?
C10 C11 C12 C7 -0.9(7) . . . . ?
C8 C7 C12 C11 3.5(6) . . . . ?
C1 C7 C12 C11 -179.9(4) . . . . ?
C10 C9 C13 C14 -2.5(8) . . . . ?
C8 C9 C13 C14 177.6(5) . . . . ?
C9 C13 C14 C15 0.0(9) . . . . ?
C13 C14 C15 C16 1.9(10) . . . . ?
C14 C15 C16 C10 -1.3(9) . . . . ?
C11 C10 C16 C15 179.5(5) . . . . ?
C9 C10 C16 C15 -1.1(7) . . . . ?
C3 C4 C17 C18 58.9(12) . . . . ?
C5 C4 C17 C18 -119.1(7) . . . . ?
C17' C4 C17 C18 16(11) . . . . ?
C3 C4 C17 C22 -121.0(7) . . . . ?
C5 C4 C17 C22 61.1(11) . . . . ?
C17' C4 C17 C22 -164(12) . . . . ?
C22 C17 C18 C19 0.0 . . . . ?
C4 C17 C18 C19 -179.8(14) . . . . ?
C17 C18 C19 C20 0.0 . . . . ?
C17 C18 C19 C23 -179.0(10) . . . . ?
C18 C19 C20 C21 0.0 . . . . ?
C23 C19 C20 C21 179.0(10) . . . . ?
C18 C19 C20 C26 -177.7(10) . . . . ?
C23 C19 C20 C26 1.3(10) . . . . ?
C19 C20 C21 C22 0.0 . . . . ?
C26 C20 C21 C22 177.7(11) . . . . ?
C20 C21 C22 C17 0.0 . . . . ?
C18 C17 C22 C21 0.0 . . . . ?
C4 C17 C22 C21 179.8(15) . . . . ?
C18 C19 C23 C24 177.8(8) . . . . ?
C20 C19 C23 C24 -1.2(11) . . . . ?
C19 C23 C24 C25 -0.9(13) . . . . ?
C23 C24 C25 C26 3.0(13) . . . . ?
C24 C25 C26 C20 -2.9(14) . . . . ?
C21 C20 C26 C25 -176.9(9) . . . . ?
C19 C20 C26 C25 0.8(12) . . . . ?
C1 C6 C27 N1 129.0(3) . . . . ?
C5 C6 C27 N1 -55.4(4) . . . . ?
C6 C5 C28 N3 58.7(4) . . . . ?
C4 C5 C28 N3 -126.8(3) . . . . ?
N1 C31 C32 O3 -4.7(5) . . . . ?
N3 C31 C32 O3 121.2(4) . . . . ?
C35 C31 C32 O3 -123.3(4) . . . . ?
N1 C31 C32 O4 176.2(3) . . . . ?
N3 C31 C32 O4 -58.0(4) . . . . ?
C35 C31 C32 O4 57.6(4) . . . . ?
N1 C31 C35 N2 3.9(3) . . . . ?
N3 C31 C35 N2 -114.0(2) . . . . ?
C32 C31 C35 N2 126.6(3) . . . . ?
N1 C31 C35 N4 122.6(3) . . . . ?
N3 C31 C35 N4 4.7(3) . . . . ?
C32 C31 C35 N4 -114.7(3) . . . . ?
N1 C31 C35 C36 -115.8(3) . . . . ?
N3 C31 C35 C36 126.4(3) . . . . ?
C32 C31 C35 C36 7.0(4) . . . . ?
N2 C35 C36 O5 126.4(7) . . . . ?
N4 C35 C36 O5 -1.3(8) . . . . ?
C31 C35 C36 O5 -118.4(7) . . . . ?
N2 C35 C36 O5' 129(7) . . . . ?
N4 C35 C36 O5' 1(7) . . . . ?
C31 C35 C36 O5' -116(7) . . . . ?
N2 C35 C36 O6' -29(2) . . . . ?
N4 C35 C36 O6' -156(2) . . . . ?
C31 C35 C36 O6' 87(2) . . . . ?
N2 C35 C36 O6 -56.3(5) . . . . ?
N4 C35 C36 O6 176.1(4) . . . . ?
C31 C35 C36 O6 58.9(5) . . . . ?
O5 C36 O6 C37 -2.9(12) . . . . ?
O5' C36 O6 C37 -6(8) . . . . ?
O6' C36 O6 C37 93(6) . . . . ?
C35 C36 O6 C37 179.8(7) . . . . ?
C38 C37 O6 C36 -80.8(11) . . . . ?
O5 C36 O6' C37' 32(4) . . . . ?
O5' C36 O6' C37' 35(9) . . . . ?
O6 C36 O6' C37' -71(5) . . . . ?
C35 C36 O6' C37' -173(3) . . . . ?
C38' C37' O6' C36 92(11) . . . . ?
N2 C39 C41 C46 -128.2(4) . . . . ?
N2 C39 C41 C42 52.7(5) . . . . ?
C46 C41 C42 C43 1.7(5) . . . . ?
C39 C41 C42 C43 -179.2(3) . . . . ?
C46 C41 C42 C40 -173.9(3) . . . . ?
C39 C41 C42 C40 5.2(5) . . . . ?
N4 C40 C42 C41 -58.8(5) . . . . ?
N4 C40 C42 C43 125.6(4) . . . . ?
C41 C42 C43 O8 -177.7(3) . . . . ?
C40 C42 C43 O8 -2.0(5) . . . . ?
C41 C42 C43 C44 -0.4(6) . . . . ?
C40 C42 C43 C44 175.4(4) . . . . ?
O8 C43 C44 C45 176.3(4) . . . . ?
C42 C43 C44 C45 -0.8(7) . . . . ?
C43 C44 C45 C46 0.7(7) . . . . ?
C44 C45 C46 O7 -179.3(4) . . . . ?
C44 C45 C46 C41 0.7(7) . . . . ?
C42 C41 C46 C45 -1.9(6) . . . . ?
C39 C41 C46 C45 179.0(4) . . . . ?
C42 C41 C46 O7 178.1(3) . . . . ?
C39 C41 C46 O7 -1.0(5) . . . . ?
C3 C4 C17' C18' -129.8(15) . . . . ?
C5 C4 C17' C18' 63(3) . . . . ?
C17 C4 C17' C18' 11(10) . . . . ?
C3 C4 C17' C22' 53(2) . . . . ?
C5 C4 C17' C22' -114.9(15) . . . . ?
C17 C4 C17' C22' -166(13) . . . . ?
C22' C17' C18' C19' 0.0 . . . . ?
C4 C17' C18' C19' -177(3) . . . . ?
C17' C18' C19' C23' 179(2) . . . . ?
C17' C18' C19' C20' 0.0 . . . . ?
C23' C19' C20' C21' -179(2) . . . . ?
C18' C19' C20' C21' 0.0 . . . . ?
C23' C19' C20' C26' -5(3) . . . . ?
C18' C19' C20' C26' 174(3) . . . . ?
C19' C20' C21' C22' 0.0 . . . . ?
C26' C20' C21' C22' -174(3) . . . . ?
C20' C21' C22' C17' 0.0 . . . . ?
C18' C17' C22' C21' 0.0 . . . . ?
C4 C17' C22' C21' 177(3) . . . . ?
C18' C19' C23' C24' -176.8(16) . . . . ?
C20' C19' C23' C24' 2(2) . . . . ?
C19' C23' C24' C25' 1(2) . . . . ?
C23' C24' C25' C26' -3(3) . . . . ?
C24' C25' C26' C20' 0(4) . . . . ?
C19' C20' C26' C25' 3(4) . . . . ?
C21' C20' C26' C25' 178(2) . . . . ?
O1 C29 N1 C31 -171.6(3) . . . . ?
N2 C29 N1 C31 10.7(3) . . . . ?
O1 C29 N1 C27 -13.1(4) . . . . ?
N2 C29 N1 C27 169.2(2) . . . . ?
N3 C31 N1 C29 101.9(3) . . . . ?
C32 C31 N1 C29 -133.9(3) . . . . ?
C35 C31 N1 C29 -8.9(3) . . . . ?
N3 C31 N1 C27 -56.5(4) . . . . ?
C32 C31 N1 C27 67.7(4) . . . . ?
C35 C31 N1 C27 -167.3(3) . . . . ?
C6 C27 N1 C29 -83.2(3) . . . . ?
C6 C27 N1 C31 72.7(4) . . . . ?
O1 C29 N2 C35 174.3(3) . . . . ?
N1 C29 N2 C35 -8.1(3) . . . . ?
O1 C29 N2 C39 4.8(5) . . . . ?
N1 C29 N2 C39 -177.6(3) . . . . ?
N4 C35 N2 C29 -108.6(3) . . . . ?
C36 C35 N2 C29 125.0(3) . . . . ?
C31 C35 N2 C29 2.4(3) . . . . ?
N4 C35 N2 C39 61.0(4) . . . . ?
C36 C35 N2 C39 -65.4(4) . . . . ?
C31 C35 N2 C39 172.0(3) . . . . ?
C41 C39 N2 C29 91.4(4) . . . . ?
C41 C39 N2 C35 -77.1(4) . . . . ?
O2 C30 N3 C28 5.7(5) . . . . ?
N4 C30 N3 C28 -175.9(3) . . . . ?
O2 C30 N3 C31 175.7(3) . . . . ?
N4 C30 N3 C31 -5.9(3) . . . . ?
C5 C28 N3 C30 90.1(4) . . . . ?
C5 C28 N3 C31 -79.1(4) . . . . ?
N1 C31 N3 C30 -111.1(3) . . . . ?
C32 C31 N3 C30 123.6(3) . . . . ?
C35 C31 N3 C30 0.5(3) . . . . ?
N1 C31 N3 C28 59.5(4) . . . . ?
C32 C31 N3 C28 -65.8(3) . . . . ?
C35 C31 N3 C28 171.0(2) . . . . ?
O2 C30 N4 C35 -172.2(3) . . . . ?
N3 C30 N4 C35 9.4(3) . . . . ?
O2 C30 N4 C40 -15.4(5) . . . . ?
N3 C30 N4 C40 166.2(3) . . . . ?
N2 C35 N4 C30 101.8(3) . . . . ?
C36 C35 N4 C30 -132.5(3) . . . . ?
C31 C35 N4 C30 -8.7(3) . . . . ?
N2 C35 N4 C40 -55.0(4) . . . . ?
C36 C35 N4 C40 70.7(4) . . . . ?
C31 C35 N4 C40 -165.5(3) . . . . ?
C42 C40 N4 C30 -83.9(4) . . . . ?
C42 C40 N4 C35 70.7(4) . . . . ?
O3 C32 O4 C33 -0.8(6) . . . . ?
C31 C32 O4 C33 178.3(3) . . . . ?
C34 C33 O4 C32 -91.9(5) . . . . ?
C45 C46 O7 C47 13.9(7) . . . . ?
C41 C46 O7 C47 -166.0(4) . . . . ?
C44 C43 O8 C48 15.8(6) . . . . ?
C42 C43 O8 C48 -166.9(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.977
_diffrn_reflns_theta_full        23.89
_diffrn_measured_fraction_theta_full 0.977
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.040
