# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
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data_49a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H29 Cl3 N O4 S2'
_chemical_formula_weight         686.05

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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   P21/c

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

_cell_length_a                   12.6039(11)
_cell_length_b                   13.6946(12)
_cell_length_c                   18.7475(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.730(2)
_cell_angle_gamma                90.00
_cell_volume                     3213.6(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.85
_cell_measurement_theta_max      25.00

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.28
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1420
_exptl_absorpt_coefficient_mu    0.455
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.857
_exptl_absorpt_correction_T_max  0.880
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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 CCD area-detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18191
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_av_sigmaI/netI    0.0656
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.85
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5589
_reflns_number_gt                3667
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 1997)'
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-PLUS (Sheldrick, 1990)'
_computing_publication_material  SHELXL-97

_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)+(0.0700P)²+0.0000P] 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         5589
_refine_ls_number_parameters     397
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_gt           0.0568
_refine_ls_wR_factor_ref         0.1464
_refine_ls_wR_factor_gt          0.1247
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          1.922
_refine_ls_shift/su_mean         0.097

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
S1 S 0.21485(7) 0.60822(7) 0.23600(6) 0.0436(3) Uani 1 1 d . . .
Cl1 Cl 0.11748(9) 1.18375(9) 0.04853(8) 0.0819(5) Uani 1 1 d . . .
O1 O 0.40190(18) 0.67545(16) 0.20301(12) 0.0326(6) Uani 1 1 d . . .
N1 N 0.5302(2) 0.97803(19) 0.26218(15) 0.0315(7) Uani 1 1 d . . .
C1 C 0.4238(3) 0.7309(2) 0.3941(2) 0.0341(9) Uani 1 1 d . . .
C2 C 0.3890(3) 1.0324(3) 0.0780(2) 0.0428(10) Uani 1 1 d . . .
H2A H 0.4350 1.0028 0.0492 0.051 Uiso 1 1 calc R . .
C3 C 0.3418(3) 1.0714(3) 0.1935(2) 0.0397(9) Uani 1 1 d . . .
H3A H 0.3559 1.0696 0.2433 0.048 Uiso 1 1 calc R . .
C4 C 0.7983(3) 1.0497(3) 0.46261(19) 0.0353(9) Uani 1 1 d . . .
C5 C 0.2317(3) 1.1242(3) 0.0886(3) 0.0479(11) Uani 1 1 d . . .
C6 C 0.3002(3) 1.0815(3) 0.0461(2) 0.0498(11) Uani 1 1 d . . .
H6A H 0.2869 1.0855 -0.0037 0.060 Uiso 1 1 calc R . .
C7 C 0.5903(3) 0.7313(3) 0.10565(19) 0.0365(9) Uani 1 1 d . . .
H7A H 0.5243 0.7145 0.0812 0.044 Uiso 1 1 calc R . .
C8 C 0.7198(3) 0.9137(3) 0.3970(2) 0.0389(9) Uani 1 1 d . . .
H8A H 0.7272 0.8565 0.3713 0.047 Uiso 1 1 calc R . .
C9 C 0.7876(3) 0.7804(3) 0.1768(2) 0.0423(10) Uani 1 1 d . . .
H9A H 0.8539 0.7972 0.2007 0.051 Uiso 1 1 calc R . .
C10 C 0.6963(3) 0.8291(3) 0.1906(2) 0.0400(9) Uani 1 1 d . . .
H10A H 0.7022 0.8793 0.2242 0.048 Uiso 1 1 calc R . .
C11 C 0.2509(3) 1.1197(3) 0.1613(2) 0.0483(11) Uani 1 1 d . . .
H11A H 0.2038 1.1487 0.1896 0.058 Uiso 1 1 calc R . .
C12 C 0.5284(3) 0.7843(2) 0.40175(19) 0.0331(8) Uani 1 1 d . . .
H12A H 0.5775 0.7501 0.3744 0.040 Uiso 1 1 calc R . .
H12B H 0.5584 0.7831 0.4518 0.040 Uiso 1 1 calc R . .
C13 C 0.7785(3) 0.7063(3) 0.12690(19) 0.0337(8) Uani 1 1 d . . .
C14 C 0.2797(3) 0.6497(2) 0.3176(2) 0.0320(8) Uani 1 1 d . . .
C15 C 0.5082(3) 0.9687(2) 0.18438(18) 0.0300(8) Uani 1 1 d . . .
H15A H 0.5709 0.9905 0.1624 0.036 Uiso 1 1 calc R . .
C16 C 0.4698(2) 0.8233(2) 0.24746(18) 0.0270(8) Uani 1 1 d . . .
C17 C 0.6997(3) 1.0857(3) 0.47242(19) 0.0350(9) Uani 1 1 d . . .
H17A H 0.6930 1.1435 0.4975 0.042 Uiso 1 1 calc R . .
C18 C 0.6182(2) 0.9479(2) 0.40647(18) 0.0281(8) Uani 1 1 d . . .
C19 C 0.8095(3) 0.9647(3) 0.4257(2) 0.0396(9) Uani 1 1 d . . .
H19A H 0.8772 0.9413 0.4199 0.048 Uiso 1 1 calc R . .
C20 C 0.3737(2) 0.7026(2) 0.32331(18) 0.0275(8) Uani 1 1 d . . .
C21 C 0.6095(3) 1.0336(2) 0.44400(18) 0.0297(8) Uani 1 1 d . . .
H21A H 0.5421 1.0570 0.4505 0.036 Uiso 1 1 calc R . .
C22 C 0.4952(3) 0.8560(2) 0.17398(18) 0.0286(8) Uani 1 1 d . . .
H22A H 0.4351 0.8415 0.1374 0.034 Uiso 1 1 calc R . .
C23 C 0.4185(2) 0.7309(2) 0.25602(18) 0.0256(8) Uani 1 1 d . . .
C24 C 0.6803(3) 0.6813(3) 0.0909(2) 0.0397(9) Uani 1 1 d . . .
H24A H 0.6749 0.6313 0.0571 0.048 Uiso 1 1 calc R . .
C25 C 0.5958(2) 0.8057(2) 0.15583(18) 0.0265(8) Uani 1 1 d . . .
C26 C 0.4109(3) 1.0263(2) 0.15193(19) 0.0300(8) Uani 1 1 d . . .
C27 C 0.5030(2) 0.8955(2) 0.29572(18) 0.0272(8) Uani 1 1 d . . .
C28 C 0.5193(3) 0.8910(2) 0.37619(18) 0.0293(8) Uani 1 1 d . . .
H28A H 0.4569 0.9204 0.3945 0.035 Uiso 1 1 calc R . .
C29 C 0.1112(3) 0.5456(3) 0.3441(3) 0.0583(12) Uani 1 1 d . . .
H30A H 0.1333 0.4779 0.3426 0.070 Uiso 1 1 calc R . .
H30B H 0.0475 0.5488 0.3684 0.070 Uiso 1 1 calc R . .
C30 C 0.1943(4) 0.9064(3) 0.3233(3) 0.0700(14) Uani 1 1 d . . .
H30C H 0.1540 0.9095 0.3636 0.105 Uiso 1 1 calc R . .
H30D H 0.2217 0.9701 0.3143 0.105 Uiso 1 1 calc R . .
H30E H 0.2526 0.8615 0.3335 0.105 Uiso 1 1 calc R . .
C31 C 0.1249(4) 0.8730(3) 0.2598(3) 0.0617(13) Uani 1 1 d . . .
O4 O 0.1762(3) 0.8678(2) 0.2027(2) 0.0773(10) Uani 1 1 d . . .
O3 O 0.0318(3) 0.8522(3) 0.2590(2) 0.1107(15) Uani 1 1 d . . .
C34 C 0.0880(3) 0.5841(4) 0.2705(3) 0.0665(14) Uani 1 1 d . . .
H51A H 0.0467 0.6439 0.2708 0.080 Uiso 1 1 calc R . .
H51B H 0.0469 0.5369 0.2402 0.080 Uiso 1 1 calc R . .
C32 C 0.1150(5) 0.8355(5) 0.1380(3) 0.100(2) Uani 1 1 d . . .
H32A H 0.0956 0.7675 0.1432 0.120 Uiso 1 1 calc R . .
H32B H 0.0495 0.8733 0.1301 0.120 Uiso 1 1 calc R . .
S2 S 0.21705(8) 0.61797(7) 0.39267(6) 0.0478(3) Uani 1 1 d . . .
Cl2 Cl 0.91204(7) 1.11333(8) 0.49813(6) 0.0554(3) Uani 1 1 d . . .
O2 O 0.3831(2) 0.7114(2) 0.44897(14) 0.0508(7) Uani 1 1 d . . .
C33 C 0.1684(7) 0.8448(6) 0.0817(4) 0.184(5) Uani 1 1 d . . .
H33A H 0.1242 0.8237 0.0392 0.276 Uiso 1 1 calc R . .
H33B H 0.2317 0.8053 0.0885 0.276 Uiso 1 1 calc R . .
H33C H 0.1878 0.9119 0.0765 0.276 Uiso 1 1 calc R . .
Cl3 Cl 0.89248(7) 0.64462(7) 0.10767(6) 0.0482(3) 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
S1 C14 1.743(4) . ?
S1 C34 1.823(4) . ?
Cl1 C5 1.746(4) . ?
O1 C23 1.249(4) . ?
N1 C27 1.356(4) . ?
N1 C15 1.458(4) . ?
C1 O2 1.231(4) . ?
C1 C20 1.453(5) . ?
C1 C12 1.500(5) . ?
C2 C6 1.381(5) . ?
C2 C26 1.384(5) . ?
C3 C26 1.380(5) . ?
C3 C11 1.397(5) . ?
C4 C17 1.370(5) . ?
C4 C19 1.370(5) . ?
C4 Cl2 1.742(3) . ?
C5 C11 1.358(6) . ?
C5 C6 1.373(6) . ?
C7 C24 1.381(5) . ?
C7 C25 1.383(5) . ?
C8 C19 1.382(5) . ?
C8 C18 1.394(4) . ?
C9 C13 1.375(5) . ?
C9 C10 1.380(5) . ?
C10 C25 1.393(5) . ?
C12 C28 1.539(4) . ?
C13 C24 1.382(5) . ?
C13 Cl3 1.740(3) . ?
C14 C20 1.382(4) . ?
C14 S2 1.748(4) . ?
C15 C26 1.523(4) . ?
C15 C22 1.563(4) . ?
C16 C27 1.373(4) . ?
C16 C23 1.438(4) . ?
C16 C22 1.518(5) . ?
C17 C21 1.394(4) . ?
C18 C21 1.378(4) . ?
C18 C28 1.523(4) . ?
C20 C23 1.493(4) . ?
C22 C25 1.517(4) . ?
C27 C28 1.500(5) . ?
C29 C34 1.475(6) . ?
C29 S2 1.818(4) . ?
C30 C31 1.465(6) . ?
C31 O3 1.206(5) . ?
C31 O4 1.315(6) . ?
O4 C32 1.429(6) . ?
C32 C33 1.324(8) . ?

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
C14 S1 C34 95.1(2) . . ?
C27 N1 C15 111.2(3) . . ?
O2 C1 C20 121.8(3) . . ?
O2 C1 C12 118.2(3) . . ?
C20 C1 C12 120.0(3) . . ?
C6 C2 C26 121.3(4) . . ?
C26 C3 C11 120.6(4) . . ?
C17 C4 C19 121.5(3) . . ?
C17 C4 Cl2 119.2(3) . . ?
C19 C4 Cl2 119.3(3) . . ?
C11 C5 C6 120.9(4) . . ?
C11 C5 Cl1 119.6(4) . . ?
C6 C5 Cl1 119.5(4) . . ?
C2 C6 C5 119.3(4) . . ?
C24 C7 C25 121.6(3) . . ?
C19 C8 C18 120.1(3) . . ?
C13 C9 C10 118.6(3) . . ?
C9 C10 C25 122.2(3) . . ?
C5 C11 C3 119.7(4) . . ?
C1 C12 C28 113.6(3) . . ?
C24 C13 C9 120.9(3) . . ?
C24 C13 Cl3 119.5(3) . . ?
C9 C13 Cl3 119.6(3) . . ?
C20 C14 S1 123.3(3) . . ?
C20 C14 S2 122.1(3) . . ?
S1 C14 S2 114.58(19) . . ?
N1 C15 C26 113.9(3) . . ?
N1 C15 C22 102.5(3) . . ?
C26 C15 C22 113.2(3) . . ?
C27 C16 C23 131.8(3) . . ?
C27 C16 C22 107.8(3) . . ?
C23 C16 C22 120.4(3) . . ?
C4 C17 C21 118.5(3) . . ?
C21 C18 C8 118.7(3) . . ?
C21 C18 C28 121.0(3) . . ?
C8 C18 C28 120.3(3) . . ?
C4 C19 C8 119.9(3) . . ?
C14 C20 C1 119.2(3) . . ?
C14 C20 C23 118.4(3) . . ?
C1 C20 C23 122.4(3) . . ?
C18 C21 C17 121.4(3) . . ?
C25 C22 C16 109.9(3) . . ?
C25 C22 C15 113.5(3) . . ?
C16 C22 C15 102.0(3) . . ?
O1 C23 C16 118.8(3) . . ?
O1 C23 C20 118.0(3) . . ?
C16 C23 C20 122.8(3) . . ?
C13 C24 C7 119.3(3) . . ?
C7 C25 C10 117.3(3) . . ?
C7 C25 C22 120.7(3) . . ?
C10 C25 C22 122.0(3) . . ?
C3 C26 C2 118.2(3) . . ?
C3 C26 C15 122.5(3) . . ?
C2 C26 C15 119.2(3) . . ?
N1 C27 C16 111.7(3) . . ?
N1 C27 C28 119.2(3) . . ?
C16 C27 C28 128.9(3) . . ?
C27 C28 C18 111.3(3) . . ?
C27 C28 C12 110.4(3) . . ?
C18 C28 C12 110.0(3) . . ?
C34 C29 S2 109.1(3) . . ?
O3 C31 O4 123.3(5) . . ?
O3 C31 C30 124.7(6) . . ?
O4 C31 C30 112.0(4) . . ?
C31 O4 C32 116.0(5) . . ?
C29 C34 S1 108.1(3) . . ?
C33 C32 O4 111.9(6) . . ?
C14 S2 C29 96.12(19) . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.551
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.064
_database_code_depnum_ccdc_archive 'CCDC 1002968'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_added_by_encifer
#===================================================================          
# 1                                                                                                                                    
_contact_author_name             'Ling Pan'
_contact_author_address          
;                                                                             
 Department of Chemistry, 
Northeast Normal University, 
Changchun 130024, P. R. China  
;
_contact_author_email            panl948@nenu.edu.cn
_contact_author_phone            +86-431-85099759
_requested_journal               ?


#=============================================================================
# 2 data_p-1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C49.50 H42 Cl4.50 N1.50 O6 S3'
_chemical_formula_weight         1009.55

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   10.069(5)
_cell_length_b                   13.141(5)
_cell_length_c                   18.165(5)
_cell_angle_alpha                110.735(5)
_cell_angle_beta                 93.826(5)
_cell_angle_gamma                107.061(5)
_cell_volume                     2109.4(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4772
_cell_measurement_theta_min      1.7
_cell_measurement_theta_max      25.0

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1044
_exptl_absorpt_coefficient_mu    0.518
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.940
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Diffraction Gemini R Ultra'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10697
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0643
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.71
_diffrn_reflns_theta_max         25.05
_reflns_number_total             7324
_reflns_number_gt                4772
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'CrysAlis (Oxford Diffraction, 2006)'
_computing_cell_refinement       CrysAlis
_computing_data_reduction        CrysAlis
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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 > 2σ(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)+(0.2000P)²+0.0000P] 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         7324
_refine_ls_number_parameters     463
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1848
_refine_ls_R_factor_gt           0.1443
_refine_ls_wR_factor_ref         0.4431
_refine_ls_wR_factor_gt          0.3967
_refine_ls_goodness_of_fit_ref   1.588
_refine_ls_restrained_S_all      1.588
_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
C1 C 0.0587(9) 0.0303(8) 0.8047(5) 0.044(2) Uani 1 1 d . . .
C2 C 0.1799(9) 0.0079(10) 0.8347(5) 0.050(2) Uani 1 1 d . . .
C3 C 0.2662(9) -0.0489(8) 0.7796(5) 0.043(2) Uani 1 1 d . . .
C4 C 0.2902(8) -0.0283(8) 0.7066(5) 0.0374(19) Uani 1 1 d . . .
H4A H 0.2415 -0.1004 0.6611 0.045 Uiso 1 1 calc R . .
H4B H 0.3906 -0.0100 0.7060 0.045 Uiso 1 1 calc R . .
C5 C 0.2454(8) 0.0660(8) 0.6929(5) 0.0372(19) Uani 1 1 d . . .
H5 H 0.2654 0.1302 0.7451 0.045 Uiso 1 1 calc R . .
C6 C 0.0820(8) 0.0214(7) 0.6603(4) 0.0327(18) Uani 1 1 d . . .
C7 C -0.0076(8) -0.0208(7) 0.7166(5) 0.0338(18) Uani 1 1 d . . .
H7 H -0.0915 0.0019 0.7136 0.041 Uiso 1 1 calc R . .
C8 C -0.0602(8) -0.1537(7) 0.6738(5) 0.0340(18) Uani 1 1 d . . .
H8 H 0.0191 -0.1801 0.6816 0.041 Uiso 1 1 calc R . .
C9 C -0.0867(8) -0.1673(7) 0.5871(5) 0.0325(18) Uani 1 1 d . . .
H9 H -0.1692 -0.1454 0.5773 0.039 Uiso 1 1 calc R . .
C10 C 0.2155(10) 0.0387(12) 0.9167(6) 0.067(3) Uani 1 1 d . . .
C11 C 0.2259(12) 0.1051(17) 1.0738(6) 0.099(5) Uani 1 1 d . . .
H11A H 0.2277 0.1686 1.1223 0.119 Uiso 1 1 calc R . .
H11B H 0.1798 0.0329 1.0793 0.119 Uiso 1 1 calc R . .
C12 C 0.3721(12) 0.1143(15) 1.0603(6) 0.087(4) Uani 1 1 d . . .
H12A H 0.4198 0.0934 1.0979 0.104 Uiso 1 1 calc R . .
H12B H 0.4255 0.1932 1.0683 0.104 Uiso 1 1 calc R . .
C13 C 0.3280(8) 0.1136(7) 0.6378(5) 0.0352(18) Uani 1 1 d . . .
C14 C 0.3976(10) 0.2306(7) 0.6639(6) 0.046(2) Uani 1 1 d . . .
H14 H 0.3928 0.2786 0.7148 0.056 Uiso 1 1 calc R . .
C15 C 0.4745(10) 0.2793(8) 0.6172(7) 0.051(2) Uani 1 1 d . . .
H15 H 0.5214 0.3587 0.6363 0.061 Uiso 1 1 calc R . .
C16 C 0.4800(10) 0.2070(9) 0.5415(6) 0.051(2) Uani 1 1 d . . .
C17 C 0.4119(10) 0.0904(8) 0.5140(6) 0.048(2) Uani 1 1 d . . .
H17 H 0.4184 0.0421 0.4636 0.057 Uiso 1 1 calc R . .
C18 C 0.3328(9) 0.0442(8) 0.5614(5) 0.040(2) Uani 1 1 d . . .
H18 H 0.2823 -0.0348 0.5414 0.048 Uiso 1 1 calc R . .
C19 C -0.1079(8) -0.2866(7) 0.5249(5) 0.0341(18) Uani 1 1 d . . .
C20 C 0.0045(9) -0.3204(7) 0.4966(5) 0.041(2) Uani 1 1 d . . .
H20 H 0.0968 -0.2686 0.5157 0.050 Uiso 1 1 calc R . .
C21 C -0.0214(9) -0.4311(7) 0.4398(5) 0.0384(19) Uani 1 1 d . . .
H21 H 0.0530 -0.4525 0.4194 0.046 Uiso 1 1 calc R . .
C22 C -0.1553(8) -0.5081(7) 0.4142(5) 0.0376(19) Uani 1 1 d . . .
C23 C -0.2697(10) -0.4791(8) 0.4417(5) 0.045(2) Uani 1 1 d . . .
H23 H -0.3610 -0.5327 0.4238 0.054 Uiso 1 1 calc R . .
C24 C -0.2436(8) -0.3689(8) 0.4964(5) 0.039(2) Uani 1 1 d . . .
H24 H -0.3194 -0.3480 0.5153 0.047 Uiso 1 1 calc R . .
C25 C -0.1851(8) -0.2218(8) 0.6989(5) 0.038(2) Uani 1 1 d . . .
C26 C -0.1834(9) -0.3176(8) 0.7116(6) 0.045(2) Uani 1 1 d . . .
H26 H -0.1037 -0.3395 0.7058 0.054 Uiso 1 1 calc R . .
C27 C -0.2979(9) -0.3838(9) 0.7330(6) 0.047(2) Uani 1 1 d . . .
H27 H -0.2940 -0.4481 0.7424 0.057 Uiso 1 1 calc R . .
C28 C -0.4151(9) -0.3526(9) 0.7399(5) 0.048(2) Uani 1 1 d . . .
C29 C -0.4229(9) -0.2559(9) 0.7284(5) 0.045(2) Uani 1 1 d . . .
H29 H -0.5037 -0.2355 0.7341 0.054 Uiso 1 1 calc R . .
C30 C -0.3091(8) -0.1908(9) 0.7086(5) 0.044(2) Uani 1 1 d . . .
H30 H -0.3127 -0.1250 0.7013 0.053 Uiso 1 1 calc R . .
C31 C 0.0442(8) 0.1213(7) 0.6489(4) 0.0316(18) Uani 1 1 d . . .
C32 C 0.0700(12) 0.3167(8) 0.7121(6) 0.056(3) Uani 1 1 d . . .
H32A H 0.1017 0.3786 0.7642 0.084 Uiso 1 1 calc R . .
H32B H -0.0275 0.3028 0.6931 0.084 Uiso 1 1 calc R . .
H32C H 0.1262 0.3376 0.6756 0.084 Uiso 1 1 calc R . .
C34 C -0.2413(13) 0.1965(11) 0.8095(7) 0.075(3) Uani 1 1 d . . .
C43 C 0.328(2) 0.3670(17) 0.8968(12) 0.124(6) Uiso 1 1 d . . .
N1 N 0.0418(7) -0.0795(6) 0.5847(4) 0.0324(15) Uani 1 1 d D . .
O1 O -0.0008(6) 0.0913(7) 0.8521(4) 0.0557(18) Uani 1 1 d . . .
O2 O 0.3318(7) -0.1013(6) 0.8030(4) 0.0565(18) Uani 1 1 d . . .
O3 O -0.0125(7) 0.1153(5) 0.5873(3) 0.0448(15) Uani 1 1 d . . .
O4 O 0.0844(6) 0.2140(5) 0.7171(3) 0.0438(15) Uani 1 1 d . . .
S1 S 0.1307(3) 0.1105(4) 0.98584(15) 0.0938(14) Uani 1 1 d . . .
S2 S 0.3615(3) 0.0184(4) 0.95945(16) 0.0767(11) Uani 1 1 d . . .
Cl1 Cl 0.5795(3) 0.2640(3) 0.4817(2) 0.0748(9) Uani 1 1 d . . .
Cl2 Cl -0.1873(2) -0.64806(19) 0.34341(15) 0.0524(7) Uani 1 1 d . . .
Cl3 Cl -0.5589(2) -0.4346(2) 0.76706(16) 0.0600(8) Uani 1 1 d . . .
Cl4 Cl -0.2331(6) 0.3382(4) 0.8381(3) 0.1371(19) Uani 1 1 d . . .
Cl5 Cl -0.2915(3) 0.1254(3) 0.70300(16) 0.0689(9) Uani 1 1 d . . .
Cl6 Cl -0.3638(4) 0.1213(5) 0.8525(2) 0.1156(16) Uani 1 1 d . . .
Cl40 Cl 0.3484(8) 0.4078(6) 1.0658(4) 0.167(2) Uiso 1 1 d . . .
Cl42 Cl 0.2552(18) 0.4605(14) 0.9357(10) 0.354(8) Uiso 1 1 d . . .
Cl41 Cl 0.4188(13) 0.3057(9) 0.9102(7) 0.255(4) Uiso 1 1 d . . .
Cl30 Cl 0.2782(8) 0.6904(6) 0.9307(5) 0.178(3) Uiso 1 1 d . . .
Cl31 Cl 0.0247(8) 0.6374(6) 0.9898(5) 0.093(2) Uiso 0.50 1 d P . .
Cl32 Cl 0.0168(11) 0.7187(9) 0.8633(7) 0.125(3) Uiso 0.50 1 d P . .
C38 C 0.124(3) 0.712(3) 0.9463(18) 0.088(8) Uiso 0.50 1 d P . .
C38' C 0.145(3) 0.691(2) 0.8683(18) 0.085(7) Uiso 0.50 1 d P . .
L32' Cl 0.0439(10) 0.5681(8) 0.8175(6) 0.115(3) Uiso 0.50 1 d P . .
L31' Cl 0.0625(15) 0.7866(12) 0.9335(9) 0.160(4) Uiso 0.50 1 d P . .
HN1 H 0.041(8) -0.066(6) 0.537(2) 0.023(18) Uiso 1 1 d D . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 O1 1.268(11) . ?
C1 C2 1.453(13) . ?
C1 C7 1.513(11) . ?
C2 C10 1.388(12) . ?
C2 C3 1.510(14) . ?
C3 O2 1.236(11) . ?
C3 C4 1.465(11) . ?
C4 C5 1.526(12) . ?
C5 C13 1.528(11) . ?
C5 C6 1.568(10) . ?
C6 N1 1.459(10) . ?
C6 C31 1.545(11) . ?
C6 C7 1.549(10) . ?
C7 C8 1.541(12) . ?
C8 C25 1.515(11) . ?
C8 C9 1.517(10) . ?
C9 N1 1.474(10) . ?
C9 C19 1.516(11) . ?
C10 S1 1.725(12) . ?
C10 S2 1.750(10) . ?
C11 C12 1.485(16) . ?
C11 S1 1.843(11) . ?
C12 S2 1.793(13) . ?
C13 C14 1.373(12) . ?
C13 C18 1.378(12) . ?
C14 C15 1.382(13) . ?
C15 C16 1.384(14) . ?
C16 C17 1.366(14) . ?
C16 Cl1 1.739(9) . ?
C17 C18 1.387(12) . ?
C19 C24 1.395(11) . ?
C19 C20 1.398(12) . ?
C20 C21 1.388(12) . ?
C21 C22 1.356(11) . ?
C22 C23 1.386(13) . ?
C22 Cl2 1.750(8) . ?
C23 C24 1.371(13) . ?
C25 C26 1.363(12) . ?
C25 C30 1.425(12) . ?
C26 C27 1.396(12) . ?
C27 C28 1.358(13) . ?
C28 C29 1.381(14) . ?
C28 Cl3 1.749(9) . ?
C29 C30 1.368(12) . ?
C31 O3 1.187(9) . ?
C31 O4 1.325(9) . ?
C32 O4 1.433(11) . ?
C34 Cl4 1.723(14) . ?
C34 Cl6 1.750(14) . ?
C34 Cl5 1.785(11) . ?
C43 Cl41 1.45(2) . ?
C43 Cl42 1.59(2) . ?
Cl30 C38 1.69(3) . ?
Cl30 C38' 1.70(3) . ?
Cl31 C38 1.63(3) . ?
Cl31 L31' 2.464(16) . ?
Cl32 L31' 1.229(15) . ?
Cl32 C38' 1.45(3) . ?
Cl32 C38 1.84(3) . ?
Cl32 L32' 1.965(13) . ?
C38 L31' 1.38(3) . ?
C38 C38' 1.39(4) . ?
C38' L32' 1.53(3) . ?
C38' L31' 1.83(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 121.1(8) . . ?
O1 C1 C7 116.2(8) . . ?
C2 C1 C7 122.7(8) . . ?
C10 C2 C1 118.4(9) . . ?
C10 C2 C3 119.5(8) . . ?
C1 C2 C3 122.1(7) . . ?
O2 C3 C4 120.0(9) . . ?
O2 C3 C2 117.8(8) . . ?
C4 C3 C2 121.5(8) . . ?
C3 C4 C5 118.7(8) . . ?
C4 C5 C13 112.9(7) . . ?
C4 C5 C6 110.7(7) . . ?
C13 C5 C6 110.7(6) . . ?
N1 C6 C31 110.6(6) . . ?
N1 C6 C7 104.5(6) . . ?
C31 C6 C7 109.9(6) . . ?
N1 C6 C5 111.0(6) . . ?
C31 C6 C5 107.9(6) . . ?
C7 C6 C5 113.1(6) . . ?
C1 C7 C8 117.0(7) . . ?
C1 C7 C6 117.2(6) . . ?
C8 C7 C6 103.9(6) . . ?
C25 C8 C9 114.5(6) . . ?
C25 C8 C7 117.5(7) . . ?
C9 C8 C7 100.4(6) . . ?
N1 C9 C19 112.0(6) . . ?
N1 C9 C8 101.6(6) . . ?
C19 C9 C8 115.6(7) . . ?
C2 C10 S1 123.7(8) . . ?
C2 C10 S2 122.2(9) . . ?
S1 C10 S2 114.0(5) . . ?
C12 C11 S1 106.7(8) . . ?
C11 C12 S2 108.3(9) . . ?
C14 C13 C18 118.1(8) . . ?
C14 C13 C5 119.3(8) . . ?
C18 C13 C5 122.7(7) . . ?
C13 C14 C15 122.3(9) . . ?
C14 C15 C16 118.3(9) . . ?
C17 C16 C15 120.7(9) . . ?
C17 C16 Cl1 119.4(8) . . ?
C15 C16 Cl1 119.9(8) . . ?
C16 C17 C18 119.7(9) . . ?
C13 C18 C17 120.9(8) . . ?
C24 C19 C20 117.7(8) . . ?
C24 C19 C9 119.6(7) . . ?
C20 C19 C9 122.6(7) . . ?
C21 C20 C19 120.0(8) . . ?
C22 C21 C20 120.0(8) . . ?
C21 C22 C23 121.9(8) . . ?
C21 C22 Cl2 119.9(7) . . ?
C23 C22 Cl2 118.2(6) . . ?
C24 C23 C22 117.7(8) . . ?
C23 C24 C19 122.6(8) . . ?
C26 C25 C30 117.3(8) . . ?
C26 C25 C8 120.4(8) . . ?
C30 C25 C8 122.2(8) . . ?
C25 C26 C27 121.9(8) . . ?
C28 C27 C26 118.8(9) . . ?
C27 C28 C29 122.0(8) . . ?
C27 C28 Cl3 119.1(8) . . ?
C29 C28 Cl3 118.8(7) . . ?
C30 C29 C28 118.6(9) . . ?
C29 C30 C25 121.3(9) . . ?
O3 C31 O4 125.2(8) . . ?
O3 C31 C6 124.3(7) . . ?
O4 C31 C6 110.5(6) . . ?
Cl4 C34 Cl6 112.1(8) . . ?
Cl4 C34 Cl5 109.1(7) . . ?
Cl6 C34 Cl5 108.7(6) . . ?
Cl41 C43 Cl42 147.0(18) . . ?
C6 N1 C9 108.9(6) . . ?
C31 O4 C32 115.8(6) . . ?
C10 S1 C11 96.3(5) . . ?
C10 S2 C12 96.3(5) . . ?
C38 Cl30 C38' 48.4(14) . . ?
C38 Cl31 L31' 31.7(10) . . ?
L31' Cl32 C38' 86.2(15) . . ?
L31' Cl32 C38 48.5(11) . . ?
C38' Cl32 C38 48.3(15) . . ?
L31' Cl32 L32' 124.0(10) . . ?
C38' Cl32 L32' 50.6(12) . . ?
C38 Cl32 L32' 75.5(10) . . ?
L31' C38 C38' 83(2) . . ?
L31' C38 Cl31 110(2) . . ?
C38' C38 Cl31 135(2) . . ?
L31' C38 Cl30 133(2) . . ?
C38' C38 Cl30 66.3(17) . . ?
Cl31 C38 Cl30 117.1(18) . . ?
L31' C38 Cl32 42.0(10) . . ?
C38' C38 Cl32 51.0(16) . . ?
Cl31 C38 Cl32 111.2(17) . . ?
Cl30 C38 Cl32 117.0(18) . . ?
C38 C38' Cl32 81(2) . . ?
C38 C38' L32' 106(2) . . ?
Cl32 C38' L32' 82.5(16) . . ?
C38 C38' Cl30 65.3(18) . . ?
Cl32 C38' Cl30 145(2) . . ?
L32' C38' Cl30 111.7(17) . . ?
C38 C38' L31' 48.1(15) . . ?
Cl32 C38' L31' 41.9(9) . . ?
L32' C38' L31' 114.8(19) . . ?
Cl30 C38' L31' 105.3(16) . . ?
C38' L32' Cl32 46.8(11) . . ?
Cl32 L31' C38 89.5(16) . . ?
Cl32 L31' C38' 51.9(11) . . ?
C38 L31' C38' 48.7(15) . . ?
Cl32 L31' Cl31 95.8(9) . . ?
C38 L31' Cl31 38.5(14) . . ?
C38' L31' Cl31 79.5(11) . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         2.136
_refine_diff_density_min         -1.666
_refine_diff_density_rms         0.180
_database_code_depnum_ccdc_archive 'CCDC 1003600'
