# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1005494'
_audit_update_record             
;
2014-05-27 deposited with the CCDC.
2016-06-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H40 B4 N4 O8 S2, C14 H10, C H2 Cl2'
_chemical_formula_sum            'C59 H52 B4 Cl2 N4 O8 S2'
_chemical_formula_weight         1123.31

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Cmc21

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

_cell_length_a                   18.5357(5)
_cell_length_b                   20.6392(10)
_cell_length_c                   14.1552(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5415.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    198(2)
_cell_measurement_reflns_used    1714
_cell_measurement_theta_min      3.12
_cell_measurement_theta_max      67.99

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2336
_exptl_absorpt_coefficient_mu    2.293
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6071
_exptl_absorpt_correction_T_max  0.8185
_exptl_absorpt_process_details   'Absorption was corrected by ABSCOR'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      198(2)
_diffrn_radiation_wavelength     1.54186
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'rotating anode X-ray tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID II IP 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            30899
_diffrn_reflns_av_R_equivalents  0.0949
_diffrn_reflns_av_sigmaI/netI    0.0760
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.20
_diffrn_reflns_theta_max         68.14
_reflns_number_total             5031
_reflns_number_gt                3575
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'PROCESS-AUTO (Rigaku, 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0978P)²+7.5441P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.45(3)
_refine_ls_number_reflns         5031
_refine_ls_number_parameters     366
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0965
_refine_ls_R_factor_gt           0.0691
_refine_ls_wR_factor_ref         0.2190
_refine_ls_wR_factor_gt          0.1682
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_restrained_S_all      1.141
_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 0.2763(3) 0.4073(2) -0.2066(4) 0.0301(11) Uani 1 1 d . . .
H1 H 0.3186 0.4140 -0.1638 0.036 Uiso 1 1 calc R . .
C2 C 0.2703(3) 0.4619(2) -0.2822(4) 0.0316(11) Uani 1 1 d . . .
H2 H 0.3003 0.5004 -0.2646 0.038 Uiso 1 1 calc R . .
C3 C 0.2952(3) 0.4326(2) -0.3770(4) 0.0323(12) Uani 1 1 d . . .
C4 C 0.2856(3) 0.3599(2) -0.3592(4) 0.0307(11) Uani 1 1 d . . .
C5 C 0.2843(3) 0.3107(2) -0.4257(4) 0.0317(11) Uani 1 1 d . . .
H5 H 0.2837 0.3201 -0.4914 0.038 Uiso 1 1 calc R . .
C6 C 0.2838(3) 0.2468(2) -0.3930(3) 0.0280(10) Uani 1 1 d . . .
C7 C 0.2768(3) 0.1853(2) -0.4485(4) 0.0330(11) Uani 1 1 d . . .
H7 H 0.3179 0.1788 -0.4932 0.040 Uiso 1 1 calc R . .
C8 C 0.2728(3) 0.1310(2) -0.3721(4) 0.0313(11) Uani 1 1 d . . .
H8 H 0.3022 0.0924 -0.3903 0.038 Uiso 1 1 calc R . .
C9 C 0.2995(3) 0.1613(2) -0.2782(3) 0.0297(11) Uani 1 1 d . . .
C10 C 0.2875(3) 0.2337(2) -0.2959(3) 0.0279(10) Uani 1 1 d . . .
C11 C 0.2858(3) 0.2830(2) -0.2294(4) 0.0311(10) Uani 1 1 d . . .
H11 H 0.2863 0.2740 -0.1636 0.037 Uiso 1 1 calc R . .
C12 C 0.2834(3) 0.3464(2) -0.2631(4) 0.0289(11) Uani 1 1 d . . .
C13 C 0.3761(3) 0.4450(3) -0.3886(5) 0.0500(15) Uani 1 1 d . . .
H13A H 0.4018 0.4296 -0.3324 0.075 Uiso 1 1 calc R . .
H13B H 0.3846 0.4915 -0.3966 0.075 Uiso 1 1 calc R . .
H13C H 0.3938 0.4217 -0.4444 0.075 Uiso 1 1 calc R . .
C14 C 0.2541(3) 0.4578(3) -0.4632(4) 0.0479(14) Uani 1 1 d . . .
H14A H 0.2716 0.4358 -0.5201 0.072 Uiso 1 1 calc R . .
H14B H 0.2619 0.5046 -0.4695 0.072 Uiso 1 1 calc R . .
H14C H 0.2024 0.4492 -0.4553 0.072 Uiso 1 1 calc R . .
C15 C 0.3816(3) 0.1499(3) -0.2709(4) 0.0439(14) Uani 1 1 d . . .
H15A H 0.4050 0.1647 -0.3291 0.066 Uiso 1 1 calc R . .
H15B H 0.3910 0.1036 -0.2619 0.066 Uiso 1 1 calc R . .
H15C H 0.4008 0.1742 -0.2170 0.066 Uiso 1 1 calc R . .
C16 C 0.2625(3) 0.1354(3) -0.1919(4) 0.0447(13) Uani 1 1 d . . .
H16A H 0.2801 0.1585 -0.1360 0.067 Uiso 1 1 calc R . .
H16B H 0.2730 0.0891 -0.1855 0.067 Uiso 1 1 calc R . .
H16C H 0.2103 0.1417 -0.1980 0.067 Uiso 1 1 calc R . .
C17 C 0.0390(3) 0.1602(3) -0.5334(4) 0.0355(12) Uani 1 1 d . . .
C18 C 0.0796(3) 0.1424(2) -0.4512(4) 0.0321(11) Uani 1 1 d . . .
C19 C 0.0387(3) 0.1235(2) -0.3743(4) 0.0377(12) Uani 1 1 d . . .
H19 H 0.0631 0.1098 -0.3187 0.045 Uiso 1 1 calc R . .
C20 C 0.0384(3) 0.4714(2) -0.2725(4) 0.0393(13) Uani 1 1 d . . .
H20 H 0.0629 0.4857 -0.3277 0.047 Uiso 1 1 calc R . .
C21 C 0.0786(3) 0.4517(2) -0.1961(4) 0.0327(11) Uani 1 1 d . . .
C22 C 0.0390(3) 0.4332(3) -0.1145(4) 0.0363(12) Uani 1 1 d . . .
B1 B 0.1619(3) 0.4463(3) -0.2082(4) 0.0356(13) Uani 1 1 d . . .
B2 B 0.1620(3) 0.1469(3) -0.4402(4) 0.0341(13) Uani 1 1 d . . .
N1 N 0.0673(2) 0.1774(3) -0.6174(3) 0.0461(12) Uani 1 1 d . . .
N2 N 0.0680(2) 0.4137(2) -0.0305(3) 0.0440(12) Uani 1 1 d . . .
O1 O 0.20825(18) 0.40902(16) -0.1550(3) 0.0352(8) Uani 1 1 d . . .
O2 O 0.19469(18) 0.47756(15) -0.2822(2) 0.0344(8) Uani 1 1 d . . .
O3 O 0.20693(18) 0.18395(17) -0.4962(2) 0.0344(8) Uani 1 1 d . . .
O4 O 0.19669(18) 0.11588(17) -0.3680(2) 0.0364(8) Uani 1 1 d . . .
S1 S 0.0000 0.19183(14) -0.68621(15) 0.0622(7) Uani 1 2 d S . .
S2 S 0.0000 0.39825(12) 0.03763(15) 0.0563(6) Uani 1 2 d S . .
C23 C 0.0384(5) 0.3614(6) -0.5066(8) 0.117(4) Uani 1 1 d . . .
H23 H 0.0640 0.3802 -0.5580 0.140 Uiso 1 1 calc R . .
C24 C 0.0756(5) 0.3345(5) -0.4326(8) 0.091(3) Uani 1 1 d . . .
H24 H 0.1269 0.3339 -0.4341 0.109 Uiso 1 1 calc R . .
C25 C 0.0392(4) 0.3076(4) -0.3546(7) 0.075(2) Uani 1 1 d . . .
C26 C 0.0755(4) 0.2831(4) -0.2742(7) 0.081(3) Uani 1 1 d . . .
H26 H 0.1268 0.2824 -0.2742 0.097 Uiso 1 1 calc R . .
C27 C 0.0391(3) 0.2599(4) -0.1952(8) 0.074(2) Uani 1 1 d . . .
C28 C 0.0752(4) 0.2381(4) -0.1143(8) 0.088(3) Uani 1 1 d . . .
H28 H 0.1265 0.2372 -0.1139 0.106 Uiso 1 1 calc R . .
C29 C 0.0384(4) 0.2180(4) -0.0358(9) 0.097(3) Uani 1 1 d . . .
H29 H 0.0641 0.2040 0.0186 0.116 Uiso 1 1 calc R . .
C30 C 0.0000 -0.0304(8) -0.5866(10) 0.115(6) Uani 1 2 d S . 1
H30A H 0.0000 -0.0736 -0.5561 0.138 Uiso 1 2 calc SR . 1
H30B H 0.0000 0.0023 -0.5354 0.138 Uiso 1 2 calc SR . 1
Cl1 Cl 0.07757(13) -0.02279(15) -0.64578(19) 0.1185(10) 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 O1 1.458(6) . ?
C1 C12 1.496(6) . ?
C1 C2 1.559(7) . ?
C1 H1 1.0000 . ?
C2 O2 1.439(5) . ?
C2 C3 1.543(7) . ?
C2 H2 1.0000 . ?
C3 C14 1.531(7) . ?
C3 C4 1.531(7) . ?
C3 C13 1.531(7) . ?
C4 C5 1.385(6) . ?
C4 C12 1.390(7) . ?
C5 C6 1.397(7) . ?
C5 H5 0.9500 . ?
C6 C10 1.402(7) . ?
C6 C7 1.498(6) . ?
C7 O3 1.461(5) . ?
C7 C8 1.558(7) . ?
C7 H7 1.0000 . ?
C8 O4 1.446(5) . ?
C8 C9 1.550(7) . ?
C8 H8 1.0000 . ?
C9 C16 1.499(7) . ?
C9 C10 1.531(6) . ?
C9 C15 1.542(7) . ?
C10 C11 1.387(6) . ?
C11 C12 1.392(7) . ?
C11 H11 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
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 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 N1 1.347(7) . ?
C17 C18 1.435(7) . ?
C17 C17 1.444(10) 3 ?
C18 C19 1.384(7) . ?
C18 B2 1.537(7) . ?
C19 C19 1.435(10) 3 ?
C19 H19 0.9500 . ?
C20 C21 1.375(7) . ?
C20 C20 1.422(10) 3 ?
C20 H20 0.9500 . ?
C21 C22 1.422(7) . ?
C21 B1 1.557(7) . ?
C22 N2 1.366(6) . ?
C22 C22 1.444(10) 3 ?
B1 O2 1.372(7) . ?
B1 O1 1.377(7) . ?
B2 O4 1.367(6) . ?
B2 O3 1.380(6) . ?
N1 S1 1.610(5) . ?
N2 S2 1.619(5) . ?
S1 N1 1.610(5) 3 ?
S2 N2 1.618(5) 3 ?
C23 C24 1.372(14) . ?
C23 C23 1.424(19) 3 ?
C23 H23 0.9500 . ?
C24 C25 1.408(12) . ?
C24 H24 0.9500 . ?
C25 C26 1.415(12) . ?
C25 C25 1.455(13) 3 ?
C26 C27 1.391(12) . ?
C26 H26 0.9500 . ?
C27 C28 1.402(12) . ?
C27 C27 1.448(13) 3 ?
C28 C29 1.368(13) . ?
C28 H28 0.9500 . ?
C29 C29 1.425(15) 3 ?
C29 H29 0.9500 . ?
C30 Cl1 1.671(7) 3 ?
C30 Cl1 1.671(7) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?

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 C12 111.3(4) . . ?
O1 C1 C2 105.3(4) . . ?
C12 C1 C2 104.3(4) . . ?
O1 C1 H1 111.8 . . ?
C12 C1 H1 111.8 . . ?
C2 C1 H1 111.8 . . ?
O2 C2 C3 112.3(4) . . ?
O2 C2 C1 103.4(4) . . ?
C3 C2 C1 106.9(4) . . ?
O2 C2 H2 111.3 . . ?
C3 C2 H2 111.3 . . ?
C1 C2 H2 111.3 . . ?
C14 C3 C4 114.0(4) . . ?
C14 C3 C13 110.2(5) . . ?
C4 C3 C13 107.2(4) . . ?
C14 C3 C2 114.3(4) . . ?
C4 C3 C2 102.0(4) . . ?
C13 C3 C2 108.7(4) . . ?
C5 C4 C12 121.2(5) . . ?
C5 C4 C3 127.5(5) . . ?
C12 C4 C3 111.2(4) . . ?
C4 C5 C6 117.9(5) . . ?
C4 C5 H5 121.1 . . ?
C6 C5 H5 121.1 . . ?
C5 C6 C10 120.4(4) . . ?
C5 C6 C7 128.8(5) . . ?
C10 C6 C7 110.8(4) . . ?
O3 C7 C6 109.6(4) . . ?
O3 C7 C8 105.4(4) . . ?
C6 C7 C8 104.4(4) . . ?
O3 C7 H7 112.3 . . ?
C6 C7 H7 112.3 . . ?
C8 C7 H7 112.3 . . ?
O4 C8 C9 111.4(4) . . ?
O4 C8 C7 103.3(4) . . ?
C9 C8 C7 106.8(4) . . ?
O4 C8 H8 111.6 . . ?
C9 C8 H8 111.6 . . ?
C7 C8 H8 111.6 . . ?
C16 C9 C10 114.5(4) . . ?
C16 C9 C15 110.0(5) . . ?
C10 C9 C15 107.7(4) . . ?
C16 C9 C8 114.1(4) . . ?
C10 C9 C8 102.0(4) . . ?
C15 C9 C8 108.1(4) . . ?
C11 C10 C6 121.5(4) . . ?
C11 C10 C9 127.5(4) . . ?
C6 C10 C9 110.8(4) . . ?
C10 C11 C12 117.2(4) . . ?
C10 C11 H11 121.4 . . ?
C12 C11 H11 121.4 . . ?
C4 C12 C11 121.5(5) . . ?
C4 C12 C1 111.0(4) . . ?
C11 C12 C1 127.5(5) . . ?
C3 C13 H13A 109.5 . . ?
C3 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C3 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C3 C14 H14A 109.5 . . ?
C3 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C3 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C9 C15 H15A 109.5 . . ?
C9 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C9 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C9 C16 H16A 109.5 . . ?
C9 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C9 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N1 C17 C18 125.3(5) . . ?
N1 C17 C17 113.0(3) . 3 ?
C18 C17 C17 121.7(3) . 3 ?
C19 C18 C17 115.0(5) . . ?
C19 C18 B2 118.8(5) . . ?
C17 C18 B2 126.0(5) . . ?
C18 C19 C19 123.2(3) . 3 ?
C18 C19 H19 118.4 . . ?
C19 C19 H19 118.4 3 . ?
C21 C20 C20 122.9(3) . 3 ?
C21 C20 H20 118.6 . . ?
C20 C20 H20 118.6 3 . ?
C20 C21 C22 116.0(5) . . ?
C20 C21 B1 118.2(5) . . ?
C22 C21 B1 125.6(5) . . ?
N2 C22 C21 125.7(5) . . ?
N2 C22 C22 113.2(3) . 3 ?
C21 C22 C22 121.1(3) . 3 ?
O2 B1 O1 113.8(5) . . ?
O2 B1 C21 119.3(5) . . ?
O1 B1 C21 126.8(5) . . ?
O4 B2 O3 113.9(5) . . ?
O4 B2 C18 121.0(5) . . ?
O3 B2 C18 125.1(5) . . ?
C17 N1 S1 106.3(4) . . ?
C22 N2 S2 105.7(4) . . ?
B1 O1 C1 106.3(4) . . ?
B1 O2 C2 109.1(4) . . ?
B2 O3 C7 106.2(4) . . ?
B2 O4 C8 109.1(4) . . ?
N1 S1 N1 101.6(3) . 3 ?
N2 S2 N2 102.3(3) 3 . ?
C24 C23 C23 120.2(6) . 3 ?
C24 C23 H23 119.9 . . ?
C23 C23 H23 119.9 3 . ?
C23 C24 C25 121.2(9) . . ?
C23 C24 H24 119.4 . . ?
C25 C24 H24 119.4 . . ?
C24 C25 C26 122.9(8) . . ?
C24 C25 C25 118.6(5) . 3 ?
C26 C25 C25 118.4(5) . 3 ?
C27 C26 C25 122.5(7) . . ?
C27 C26 H26 118.7 . . ?
C25 C26 H26 118.7 . . ?
C26 C27 C28 122.4(7) . . ?
C26 C27 C27 119.1(5) . 3 ?
C28 C27 C27 118.5(5) . 3 ?
C29 C28 C27 121.5(8) . . ?
C29 C28 H28 119.2 . . ?
C27 C28 H28 119.2 . . ?
C28 C29 C29 119.9(5) . 3 ?
C28 C29 H29 120.0 . . ?
C29 C29 H29 120.0 3 . ?
Cl1 C30 Cl1 118.7(8) 3 . ?
Cl1 C30 H30A 107.6 3 . ?
Cl1 C30 H30A 107.6 . . ?
Cl1 C30 H30B 107.6 3 . ?
Cl1 C30 H30B 107.6 . . ?
H30A C30 H30B 107.1 . . ?

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
O1 C1 C2 O2 -14.1(5) . . . . ?
C12 C1 C2 O2 103.2(4) . . . . ?
O1 C1 C2 C3 -132.7(4) . . . . ?
C12 C1 C2 C3 -15.4(5) . . . . ?
O2 C2 C3 C14 31.7(6) . . . . ?
C1 C2 C3 C14 144.5(4) . . . . ?
O2 C2 C3 C4 -91.8(4) . . . . ?
C1 C2 C3 C4 21.0(5) . . . . ?
O2 C2 C3 C13 155.3(4) . . . . ?
C1 C2 C3 C13 -92.0(5) . . . . ?
C14 C3 C4 C5 40.7(7) . . . . ?
C13 C3 C4 C5 -81.5(7) . . . . ?
C2 C3 C4 C5 164.4(5) . . . . ?
C14 C3 C4 C12 -143.8(5) . . . . ?
C13 C3 C4 C12 94.0(5) . . . . ?
C2 C3 C4 C12 -20.1(5) . . . . ?
C12 C4 C5 C6 -2.8(8) . . . . ?
C3 C4 C5 C6 172.3(5) . . . . ?
C4 C5 C6 C10 -2.6(7) . . . . ?
C4 C5 C6 C7 174.9(5) . . . . ?
C5 C6 C7 O3 -62.5(6) . . . . ?
C10 C6 C7 O3 115.2(5) . . . . ?
C5 C6 C7 C8 -174.9(5) . . . . ?
C10 C6 C7 C8 2.7(5) . . . . ?
O3 C7 C8 O4 -13.9(5) . . . . ?
C6 C7 C8 O4 101.6(4) . . . . ?
O3 C7 C8 C9 -131.5(4) . . . . ?
C6 C7 C8 C9 -16.0(5) . . . . ?
O4 C8 C9 C16 34.0(6) . . . . ?
C7 C8 C9 C16 146.1(4) . . . . ?
O4 C8 C9 C10 -90.0(4) . . . . ?
C7 C8 C9 C10 22.1(5) . . . . ?
O4 C8 C9 C15 156.7(4) . . . . ?
C7 C8 C9 C15 -91.2(5) . . . . ?
C5 C6 C10 C11 5.4(8) . . . . ?
C7 C6 C10 C11 -172.5(4) . . . . ?
C5 C6 C10 C9 -170.0(4) . . . . ?
C7 C6 C10 C9 12.1(6) . . . . ?
C16 C9 C10 C11 39.9(7) . . . . ?
C15 C9 C10 C11 -82.7(6) . . . . ?
C8 C9 C10 C11 163.6(5) . . . . ?
C16 C9 C10 C6 -145.0(5) . . . . ?
C15 C9 C10 C6 92.4(5) . . . . ?
C8 C9 C10 C6 -21.3(5) . . . . ?
C6 C10 C11 C12 -2.7(8) . . . . ?
C9 C10 C11 C12 171.9(4) . . . . ?
C5 C4 C12 C11 5.5(8) . . . . ?
C3 C4 C12 C11 -170.3(4) . . . . ?
C5 C4 C12 C1 -173.1(5) . . . . ?
C3 C4 C12 C1 11.2(6) . . . . ?
C10 C11 C12 C4 -2.7(8) . . . . ?
C10 C11 C12 C1 175.6(5) . . . . ?
O1 C1 C12 C4 116.0(5) . . . . ?
C2 C1 C12 C4 2.9(5) . . . . ?
O1 C1 C12 C11 -62.5(6) . . . . ?
C2 C1 C12 C11 -175.6(5) . . . . ?
N1 C17 C18 C19 -176.9(5) . . . . ?
C17 C17 C18 C19 2.0(6) 3 . . . ?
N1 C17 C18 B2 7.4(9) . . . . ?
C17 C17 C18 B2 -173.7(4) 3 . . . ?
C17 C18 C19 C19 -2.1(6) . . . 3 ?
B2 C18 C19 C19 174.0(3) . . . 3 ?
C20 C20 C21 C22 -2.2(6) 3 . . . ?
C20 C20 C21 B1 173.1(3) 3 . . . ?
C20 C21 C22 N2 -178.3(5) . . . . ?
B1 C21 C22 N2 6.7(9) . . . . ?
C20 C21 C22 C22 2.2(5) . . . 3 ?
B1 C21 C22 C22 -172.8(4) . . . 3 ?
C20 C21 B1 O2 18.1(7) . . . . ?
C22 C21 B1 O2 -167.0(5) . . . . ?
C20 C21 B1 O1 -157.1(5) . . . . ?
C22 C21 B1 O1 17.8(9) . . . . ?
C19 C18 B2 O4 18.9(8) . . . . ?
C17 C18 B2 O4 -165.5(5) . . . . ?
C19 C18 B2 O3 -157.4(5) . . . . ?
C17 C18 B2 O3 18.2(8) . . . . ?
C18 C17 N1 S1 179.3(4) . . . . ?
C17 C17 N1 S1 0.3(4) 3 . . . ?
C21 C22 N2 S2 -179.9(4) . . . . ?
C22 C22 N2 S2 -0.3(4) 3 . . . ?
O2 B1 O1 C1 -9.2(6) . . . . ?
C21 B1 O1 C1 166.2(5) . . . . ?
C12 C1 O1 B1 -98.4(5) . . . . ?
C2 C1 O1 B1 14.1(5) . . . . ?
O1 B1 O2 C2 -0.3(6) . . . . ?
C21 B1 O2 C2 -176.1(4) . . . . ?
C3 C2 O2 B1 123.9(4) . . . . ?
C1 C2 O2 B1 9.0(5) . . . . ?
O4 B2 O3 C7 -9.0(6) . . . . ?
C18 B2 O3 C7 167.6(5) . . . . ?
C6 C7 O3 B2 -98.0(5) . . . . ?
C8 C7 O3 B2 13.8(5) . . . . ?
O3 B2 O4 C8 -0.5(6) . . . . ?
C18 B2 O4 C8 -177.1(4) . . . . ?
C9 C8 O4 B2 123.3(4) . . . . ?
C7 C8 O4 B2 9.0(5) . . . . ?
C17 N1 S1 N1 -0.4(6) . . . 3 ?
C22 N2 S2 N2 0.5(6) . . . 3 ?
C23 C23 C24 C25 -1.4(11) 3 . . . ?
C23 C24 C25 C26 -175.9(8) . . . . ?
C23 C24 C25 C25 1.3(10) . . . 3 ?
C24 C25 C26 C27 176.3(7) . . . . ?
C25 C25 C26 C27 -0.9(8) 3 . . . ?
C25 C26 C27 C28 -177.4(7) . . . . ?
C25 C26 C27 C27 0.9(8) . . . 3 ?
C26 C27 C28 C29 177.3(7) . . . . ?
C27 C27 C28 C29 -1.0(9) 3 . . . ?
C27 C28 C29 C29 1.0(10) . . . 3 ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        68.14
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.600
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.082
####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1005495'
_audit_update_record             
;
2014-05-27 deposited with the CCDC.
2016-06-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H40 B4 N4 O8 S2, C10 H8, 2(C H Cl3)'
_chemical_formula_sum            'C58 H52 B4 Cl12 N4 O8 S2'
_chemical_formula_weight         1465.79

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

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

_cell_length_a                   13.7340(6)
_cell_length_b                   14.1169(5)
_cell_length_c                   20.8001(7)
_cell_angle_alpha                90
_cell_angle_beta                 122.833(2)
_cell_angle_gamma                90
_cell_volume                     3388.5(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_F_000             1496
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.294
_exptl_crystal_size_mid          0.285
_exptl_crystal_size_min          0.174
_exptl_absorpt_coefficient_mu    5.510
_shelx_estimated_absorpt_T_min   0.294
_shelx_estimated_absorpt_T_max   0.447
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.383
_exptl_absorpt_correction_T_max  0.447
_exptl_absorpt_process_details   'Absorption was corrected by ABSCOR'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54186
_diffrn_radiation_type           CuK\a
_diffrn_source                   'rotating anode X-ray tube'
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID II IP Area Detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37551
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_av_R_equivalents  0.0663
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.830
_diffrn_reflns_theta_max         68.224
_diffrn_reflns_theta_full        67.686
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             6111
_reflns_number_gt                4788
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'PROCESS-AUTO (Rigaku, 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2008)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'

_refine_special_details          
; 
 ? 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0528P)²+1.1897P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6111
_refine_ls_number_parameters     442
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0518
_refine_ls_wR_factor_ref         0.1371
_refine_ls_wR_factor_gt          0.1270
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_restrained_S_all      1.164
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.70901(7) -0.17909(5) 0.24940(4) 0.0581(2) Uani 1 1 d . . . . .
O1 O 0.56258(14) 0.04596(11) 0.34118(9) 0.0395(4) Uani 1 1 d . . . . .
O2 O 0.59223(15) 0.01153(11) 0.45839(10) 0.0437(4) Uani 1 1 d . . . . .
O3 O 0.98390(13) 0.35234(11) 0.54818(9) 0.0368(4) Uani 1 1 d . . . . .
O4 O 0.98837(14) 0.35806(13) 0.43991(10) 0.0453(4) Uani 1 1 d . . . . .
N1 N 0.80077(19) -0.24275(15) 0.32180(12) 0.0469(5) Uani 1 1 d . . . . .
N2 N 0.65609(19) -0.11391(15) 0.28692(13) 0.0480(5) Uani 1 1 d . . . . .
C1 C 0.6917(2) -0.09949(17) 0.41645(14) 0.0375(5) Uani 1 1 d . . . . .
C2 C 0.7560(2) -0.13859(18) 0.48823(15) 0.0427(6) Uani 1 1 d . . . . .
H2 H 0.7449 -0.1159 0.5258 0.051 Uiso 1 1 calc R U . . .
C3 C 0.8383(2) -0.21155(18) 0.50813(15) 0.0420(6) Uani 1 1 d . . . . .
H3 H 0.8785 -0.2343 0.5581 0.050 Uiso 1 1 calc R U . . .
C4 C 0.8617(2) -0.25044(17) 0.45754(14) 0.0370(5) Uani 1 1 d . . . . .
C5 C 0.7946(2) -0.21389(16) 0.38141(14) 0.0367(5) Uani 1 1 d . . . . .
C6 C 0.7112(2) -0.13950(16) 0.36122(14) 0.0375(5) Uani 1 1 d . . . . .
C7 C 0.5163(2) 0.12601(16) 0.36039(14) 0.0372(5) Uani 1 1 d . . . . .
H7 H 0.4378 0.1432 0.3186 0.045 Uiso 1 1 calc R U . . .
C8 C 0.5215(2) 0.09562(16) 0.43419(15) 0.0390(6) Uani 1 1 d . . . . .
H8 H 0.4439 0.0817 0.4230 0.047 Uiso 1 1 calc R U . . .
C9 C 0.5784(2) 0.17696(17) 0.49241(15) 0.0384(6) Uani 1 1 d . . . . .
C10 C 0.64364(19) 0.22997(15) 0.46282(13) 0.0325(5) Uani 1 1 d . . . . .
C11 C 0.73325(19) 0.29489(16) 0.50134(14) 0.0345(5) Uani 1 1 d . . . . .
H11 H 0.7643 0.3092 0.5526 0.041 Uiso 1 1 calc R U . . .
C12 C 0.77505(19) 0.33781(15) 0.46062(13) 0.0319(5) Uani 1 1 d . . . . .
C13 C 0.87859(19) 0.40214(16) 0.49107(14) 0.0346(5) Uani 1 1 d . . . . .
H13 H 0.8684 0.4620 0.5106 0.042 Uiso 1 1 calc R U . . .
C14 C 0.8910(2) 0.41697(16) 0.42184(14) 0.0366(5) Uani 1 1 d . . . . .
H14 H 0.9062 0.4836 0.4170 0.044 Uiso 1 1 calc R U . . .
C15 C 0.7777(2) 0.38272(17) 0.34972(14) 0.0379(6) Uani 1 1 d . . . . .
C16 C 0.72566(19) 0.32055(16) 0.38302(13) 0.0329(5) Uani 1 1 d . . . . .
C17 C 0.6375(2) 0.25434(16) 0.34519(14) 0.0366(5) Uani 1 1 d . . . . .
H17 H 0.6050 0.2413 0.2936 0.044 Uiso 1 1 calc R U . . .
C18 C 0.59929(19) 0.20813(16) 0.38636(13) 0.0327(5) Uani 1 1 d . . . . .
C19 C 0.6552(3) 0.1433(2) 0.57494(16) 0.0561(7) Uani 1 1 d . . . . .
H19A H 0.7135 0.1013 0.5794 0.084 Uiso 1 1 calc R U . . .
H19B H 0.6088 0.1105 0.5895 0.084 Uiso 1 1 calc R U . . .
H19C H 0.6917 0.1969 0.6079 0.084 Uiso 1 1 calc R U . . .
C20 C 0.4817(2) 0.24177(19) 0.48336(18) 0.0526(7) Uani 1 1 d . . . . .
H20A H 0.5154 0.2984 0.5129 0.079 Uiso 1 1 calc R U . . .
H20B H 0.4392 0.2092 0.5011 0.079 Uiso 1 1 calc R U . . .
H20C H 0.4303 0.2582 0.4304 0.079 Uiso 1 1 calc R U . . .
C21 C 0.7970(3) 0.3312(2) 0.29298(18) 0.0626(8) Uani 1 1 d . . . . .
H21A H 0.8426 0.2754 0.3166 0.094 Uiso 1 1 calc R U . . .
H21B H 0.8371 0.3723 0.2780 0.094 Uiso 1 1 calc R U . . .
H21C H 0.7235 0.3136 0.2486 0.094 Uiso 1 1 calc R U . . .
C22 C 0.7001(2) 0.4699(2) 0.31190(19) 0.0625(9) Uani 1 1 d . . . . .
H22A H 0.6238 0.4498 0.2723 0.094 Uiso 1 1 calc R U . . .
H22B H 0.7323 0.5090 0.2901 0.094 Uiso 1 1 calc R U . . .
H22C H 0.6958 0.5055 0.3496 0.094 Uiso 1 1 calc R U . . .
B1 B 0.6128(2) -0.01322(19) 0.40306(17) 0.0383(6) Uani 1 1 d . . . . .
B2 B 1.0368(2) 0.32208(19) 0.51170(17) 0.0372(6) Uani 1 1 d . . . . .
C101 C 0.9125(3) 0.0899(3) 0.5105(3) 0.0831(12) Uani 1 1 d . U . . .
H101 H 0.8542 0.1334 0.4807 0.100 Uiso 1 1 calc R U . . .
C102 C 0.9547(5) 0.0821(4) 0.5859(4) 0.1060(16) Uani 1 1 d . U . . .
H102 H 0.9253 0.1209 0.6076 0.127 Uiso 1 1 calc R U . . .
C103 C 1.0403(5) 0.0180(4) 0.6312(3) 0.1064(16) Uani 1 1 d . U . . .
H103 H 1.0676 0.0135 0.6830 0.128 Uiso 1 1 calc R U . . .
C104 C 1.0859(3) -0.0394(3) 0.6007(2) 0.0844(12) Uani 1 1 d . U . . .
H104 H 1.1442 -0.0823 0.6318 0.101 Uiso 1 1 calc R U . . .
C105 C 0.9556(2) 0.03339(19) 0.47769(19) 0.0558(8) Uani 1 1 d . . . . .
C201 C 0.9530(3) -0.3696(3) 0.27742(18) 0.0663(9) Uani 1 1 d . . . . .
H201 H 0.9376 -0.3444 0.3150 0.080 Uiso 1 1 calc R U . A 1
Cl1A Cl 1.03208(17) -0.28663(13) 0.26364(10) 0.1049(6) Uani 0.887(4) 1 d . . P
B 1
Cl2A Cl 0.82013(16) -0.3939(2) 0.19277(11) 0.0994(6) Uani 0.887(4) 1 d . U P B
1
Cl3A Cl 1.03693(14) -0.47494(13) 0.31549(7) 0.0946(6) Uani 0.887(4) 1 d . . P B
1
Cl1B Cl 0.9679(15) -0.2475(11) 0.2368(9) 0.117(5) Uiso 0.113(4) 1 d . . P B 2
Cl2B Cl 0.8412(13) -0.4234(9) 0.1954(10) 0.066(3) Uiso 0.113(4) 1 d . . P B 2
Cl3B Cl 1.0632(10) -0.4236(10) 0.3060(7) 0.092(4) Uiso 0.113(4) 1 d . . P B 2
C301 C 0.5417(2) 0.0614(2) 0.16521(18) 0.0559(7) Uani 1 1 d . . . . .
H301 H 0.5504 0.0299 0.2100 0.067 Uiso 1 1 calc R U . C 3
Cl4A Cl 0.4790(6) -0.0155(9) 0.0860(8) 0.111(3) Uani 0.50(3) 1 d . . P D 3
Cl5A Cl 0.4580(7) 0.1655(6) 0.1426(3) 0.0580(13) Uani 0.50(3) 1 d . . P D 3
Cl6A Cl 0.6749(9) 0.0893(10) 0.1807(6) 0.108(3) Uani 0.50(3) 1 d . . P D 3
Cl4B Cl 0.4805(4) -0.0288(5) 0.0988(4) 0.0638(17) Uani 0.50(3) 1 d . . P D 4
Cl5B Cl 0.4418(11) 0.1541(8) 0.1368(5) 0.088(2) Uani 0.50(3) 1 d . . P D 4
Cl6B Cl 0.6787(8) 0.1017(8) 0.1865(4) 0.0725(17) Uani 0.50(3) 1 d . . P D 4


_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 N2 1.612(2) . ?
S1 N1 1.614(2) . ?
O1 B1 1.367(3) . ?
O1 C7 1.455(3) . ?
O2 B1 1.370(3) . ?
O2 C8 1.441(3) . ?
O3 B2 1.372(3) . ?
O3 C13 1.461(3) . ?
O4 B2 1.361(3) . ?
O4 C14 1.441(3) . ?
N1 C5 1.350(3) . ?
N2 C6 1.350(3) . ?
C1 C2 1.373(3) . ?
C1 C6 1.429(3) . ?
C1 B1 1.552(4) . ?
C2 C3 1.415(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.371(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.429(3) . ?
C4 B2 1.552(3) 3_756 ?
C5 C6 1.439(3) . ?
C7 C18 1.506(3) . ?
C7 C8 1.557(3) . ?
C7 H7 0.9800 . ?
C8 C9 1.539(3) . ?
C8 H8 0.9800 . ?
C9 C19 1.524(4) . ?
C9 C10 1.530(3) . ?
C9 C20 1.538(3) . ?
C10 C11 1.388(3) . ?
C10 C18 1.395(3) . ?
C11 C12 1.393(3) . ?
C11 H11 0.9300 . ?
C12 C16 1.392(3) . ?
C12 C13 1.507(3) . ?
C13 C14 1.553(3) . ?
C13 H13 0.9800 . ?
C14 C15 1.540(3) . ?
C14 H14 0.9800 . ?
C15 C16 1.516(3) . ?
C15 C21 1.527(4) . ?
C15 C22 1.536(3) . ?
C16 C17 1.387(3) . ?
C17 C18 1.387(3) . ?
C17 H17 0.9300 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
B2 C4 1.552(3) 3_756 ?
C101 C102 1.350(6) . ?
C101 C105 1.375(5) . ?
C101 H101 0.9300 . ?
C102 C103 1.374(7) . ?
C102 H102 0.9300 . ?
C103 C104 1.372(6) . ?
C103 H103 0.9300 . ?
C104 C105 1.408(5) 3_756 ?
C104 H104 0.9300 . ?
C105 C104 1.408(5) 3_756 ?
C105 C105 1.417(6) 3_756 ?
C201 Cl3B 1.500(11) . ?
C201 Cl1A 1.723(3) . ?
C201 Cl2B 1.734(17) . ?
C201 Cl2A 1.751(4) . ?
C201 Cl3A 1.783(4) . ?
C201 Cl1B 1.978(15) . ?
C201 H201 0.9800 . ?
C301 Cl6A 1.723(11) . ?
C301 Cl4B 1.725(7) . ?
C301 Cl5B 1.752(9) . ?
C301 Cl4A 1.760(9) . ?
C301 Cl5A 1.766(7) . ?
C301 Cl6B 1.776(10) . ?
C301 H301 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
N2 S1 N1 101.25(12) . . ?
B1 O1 C7 106.76(19) . . ?
B1 O2 C8 108.87(19) . . ?
B2 O3 C13 106.72(18) . . ?
B2 O4 C14 109.50(19) . . ?
C5 N1 S1 106.42(17) . . ?
C6 N2 S1 106.33(17) . . ?
C2 C1 C6 115.2(2) . . ?
C2 C1 B1 119.0(2) . . ?
C6 C1 B1 125.6(2) . . ?
C1 C2 C3 123.5(2) . . ?
C1 C2 H2 118.3 . . ?
C3 C2 H2 118.3 . . ?
C4 C3 C2 123.3(2) . . ?
C4 C3 H3 118.3 . . ?
C2 C3 H3 118.3 . . ?
C3 C4 C5 115.3(2) . . ?
C3 C4 B2 118.5(2) . 3_756 ?
C5 C4 B2 126.0(2) . 3_756 ?
N1 C5 C4 125.8(2) . . ?
N1 C5 C6 112.9(2) . . ?
C4 C5 C6 121.3(2) . . ?
N2 C6 C1 125.5(2) . . ?
N2 C6 C5 113.1(2) . . ?
C1 C6 C5 121.3(2) . . ?
O1 C7 C18 109.73(18) . . ?
O1 C7 C8 105.27(18) . . ?
C18 C7 C8 103.72(19) . . ?
O1 C7 H7 112.5 . . ?
C18 C7 H7 112.5 . . ?
C8 C7 H7 112.5 . . ?
O2 C8 C9 112.4(2) . . ?
O2 C8 C7 103.49(18) . . ?
C9 C8 C7 107.60(18) . . ?
O2 C8 H8 111.0 . . ?
C9 C8 H8 111.0 . . ?
C7 C8 H8 111.0 . . ?
C19 C9 C10 114.0(2) . . ?
C19 C9 C20 110.4(2) . . ?
C10 C9 C20 108.3(2) . . ?
C19 C9 C8 113.6(2) . . ?
C10 C9 C8 101.93(19) . . ?
C20 C9 C8 108.1(2) . . ?
C11 C10 C18 120.4(2) . . ?
C11 C10 C9 128.3(2) . . ?
C18 C10 C9 111.21(19) . . ?
C10 C11 C12 117.7(2) . . ?
C10 C11 H11 121.2 . . ?
C12 C11 H11 121.2 . . ?
C16 C12 C11 121.8(2) . . ?
C16 C12 C13 110.4(2) . . ?
C11 C12 C13 127.8(2) . . ?
O3 C13 C12 110.14(18) . . ?
O3 C13 C14 105.13(17) . . ?
C12 C13 C14 104.15(19) . . ?
O3 C13 H13 112.3 . . ?
C12 C13 H13 112.3 . . ?
C14 C13 H13 112.3 . . ?
O4 C14 C15 112.16(19) . . ?
O4 C14 C13 103.48(18) . . ?
C15 C14 C13 107.47(18) . . ?
O4 C14 H14 111.1 . . ?
C15 C14 H14 111.1 . . ?
C13 C14 H14 111.1 . . ?
C16 C15 C21 113.6(2) . . ?
C16 C15 C22 109.3(2) . . ?
C21 C15 C22 110.4(2) . . ?
C16 C15 C14 102.36(19) . . ?
C21 C15 C14 113.3(2) . . ?
C22 C15 C14 107.5(2) . . ?
C17 C16 C12 120.2(2) . . ?
C17 C16 C15 127.8(2) . . ?
C12 C16 C15 112.0(2) . . ?
C18 C17 C16 118.2(2) . . ?
C18 C17 H17 120.9 . . ?
C16 C17 H17 120.9 . . ?
C17 C18 C10 121.5(2) . . ?
C17 C18 C7 127.4(2) . . ?
C10 C18 C7 110.9(2) . . ?
C9 C19 H19A 109.5 . . ?
C9 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C9 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C9 C20 H20A 109.5 . . ?
C9 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C9 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C15 C21 H21A 109.5 . . ?
C15 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C15 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C15 C22 H22A 109.5 . . ?
C15 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C15 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O1 B1 O2 114.0(2) . . ?
O1 B1 C1 126.5(2) . . ?
O2 B1 C1 119.4(2) . . ?
O4 B2 O3 113.6(2) . . ?
O4 B2 C4 119.4(2) . 3_756 ?
O3 B2 C4 127.0(2) . 3_756 ?
C102 C101 C105 120.0(4) . . ?
C102 C101 H101 120.0 . . ?
C105 C101 H101 120.0 . . ?
C101 C102 C103 121.4(4) . . ?
C101 C102 H102 119.3 . . ?
C103 C102 H102 119.3 . . ?
C104 C103 C102 120.4(4) . . ?
C104 C103 H103 119.8 . . ?
C102 C103 H103 119.8 . . ?
C103 C104 C105 120.1(4) . 3_756 ?
C103 C104 H104 120.0 . . ?
C105 C104 H104 120.0 3_756 . ?
C101 C105 C104 121.8(3) . 3_756 ?
C101 C105 C105 120.6(4) . 3_756 ?
C104 C105 C105 117.6(4) 3_756 3_756 ?
Cl3B C201 Cl2B 109.4(6) . . ?
Cl1A C201 Cl2A 111.9(2) . . ?
Cl1A C201 Cl3A 109.08(19) . . ?
Cl2A C201 Cl3A 110.7(2) . . ?
Cl3B C201 Cl1B 107.2(6) . . ?
Cl2B C201 Cl1B 101.7(7) . . ?
Cl1A C201 H201 108.3 . . ?
Cl2A C201 H201 108.3 . . ?
Cl3A C201 H201 108.3 . . ?
Cl4B C301 Cl5B 109.2(4) . . ?
Cl6A C301 Cl4A 104.3(7) . . ?
Cl6A C301 Cl5A 109.4(5) . . ?
Cl4A C301 Cl5A 110.3(4) . . ?
Cl4B C301 Cl6B 115.3(5) . . ?
Cl5B C301 Cl6B 112.0(6) . . ?
Cl6A C301 H301 110.9 . . ?
Cl4A C301 H301 110.9 . . ?
Cl5A C301 H301 110.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 S1 N1 C5 -0.6(2) . . . . ?
N1 S1 N2 C6 0.7(2) . . . . ?
C6 C1 C2 C3 1.6(4) . . . . ?
B1 C1 C2 C3 -174.1(2) . . . . ?
C1 C2 C3 C4 -0.1(4) . . . . ?
C2 C3 C4 C5 -1.5(4) . . . . ?
C2 C3 C4 B2 173.3(2) . . . 3_756 ?
S1 N1 C5 C4 -179.5(2) . . . . ?
S1 N1 C5 C6 0.4(3) . . . . ?
C3 C4 C5 N1 -178.5(2) . . . . ?
B2 C4 C5 N1 7.1(4) 3_756 . . . ?
C3 C4 C5 C6 1.7(3) . . . . ?
B2 C4 C5 C6 -172.7(2) 3_756 . . . ?
S1 N2 C6 C1 179.7(2) . . . . ?
S1 N2 C6 C5 -0.5(3) . . . . ?
C2 C1 C6 N2 178.4(2) . . . . ?
B1 C1 C6 N2 -6.3(4) . . . . ?
C2 C1 C6 C5 -1.3(3) . . . . ?
B1 C1 C6 C5 174.0(2) . . . . ?
N1 C5 C6 N2 0.1(3) . . . . ?
C4 C5 C6 N2 180.0(2) . . . . ?
N1 C5 C6 C1 179.9(2) . . . . ?
C4 C5 C6 C1 -0.3(3) . . . . ?
B1 O1 C7 C18 98.8(2) . . . . ?
B1 O1 C7 C8 -12.2(2) . . . . ?
B1 O2 C8 C9 -123.2(2) . . . . ?
B1 O2 C8 C7 -7.4(2) . . . . ?
O1 C7 C8 O2 12.0(2) . . . . ?
C18 C7 C8 O2 -103.31(19) . . . . ?
O1 C7 C8 C9 131.12(19) . . . . ?
C18 C7 C8 C9 15.8(2) . . . . ?
O2 C8 C9 C19 -31.0(3) . . . . ?
C7 C8 C9 C19 -144.3(2) . . . . ?
O2 C8 C9 C10 92.1(2) . . . . ?
C7 C8 C9 C10 -21.1(2) . . . . ?
O2 C8 C9 C20 -153.8(2) . . . . ?
C7 C8 C9 C20 92.9(2) . . . . ?
C19 C9 C10 C11 -39.6(3) . . . . ?
C20 C9 C10 C11 83.8(3) . . . . ?
C8 C9 C10 C11 -162.3(2) . . . . ?
C19 C9 C10 C18 142.5(2) . . . . ?
C20 C9 C10 C18 -94.1(2) . . . . ?
C8 C9 C10 C18 19.8(2) . . . . ?
C18 C10 C11 C12 1.0(3) . . . . ?
C9 C10 C11 C12 -176.7(2) . . . . ?
C10 C11 C12 C16 3.2(3) . . . . ?
C10 C11 C12 C13 -173.1(2) . . . . ?
B2 O3 C13 C12 99.1(2) . . . . ?
B2 O3 C13 C14 -12.5(2) . . . . ?
C16 C12 C13 O3 -115.9(2) . . . . ?
C11 C12 C13 O3 60.8(3) . . . . ?
C16 C12 C13 C14 -3.6(2) . . . . ?
C11 C12 C13 C14 173.1(2) . . . . ?
B2 O4 C14 C15 -121.8(2) . . . . ?
B2 O4 C14 C13 -6.3(2) . . . . ?
O3 C13 C14 O4 11.4(2) . . . . ?
C12 C13 C14 O4 -104.48(19) . . . . ?
O3 C13 C14 C15 130.19(18) . . . . ?
C12 C13 C14 C15 14.3(2) . . . . ?
O4 C14 C15 C16 94.3(2) . . . . ?
C13 C14 C15 C16 -18.8(2) . . . . ?
O4 C14 C15 C21 -28.5(3) . . . . ?
C13 C14 C15 C21 -141.5(2) . . . . ?
O4 C14 C15 C22 -150.7(2) . . . . ?
C13 C14 C15 C22 96.2(2) . . . . ?
C11 C12 C16 C17 -4.5(3) . . . . ?
C13 C12 C16 C17 172.5(2) . . . . ?
C11 C12 C16 C15 174.1(2) . . . . ?
C13 C12 C16 C15 -9.0(3) . . . . ?
C21 C15 C16 C17 -41.6(3) . . . . ?
C22 C15 C16 C17 82.1(3) . . . . ?
C14 C15 C16 C17 -164.1(2) . . . . ?
C21 C15 C16 C12 139.9(2) . . . . ?
C22 C15 C16 C12 -96.3(3) . . . . ?
C14 C15 C16 C12 17.4(2) . . . . ?
C12 C16 C17 C18 1.3(3) . . . . ?
C15 C16 C17 C18 -177.0(2) . . . . ?
C16 C17 C18 C10 2.9(3) . . . . ?
C16 C17 C18 C7 -171.8(2) . . . . ?
C11 C10 C18 C17 -4.2(3) . . . . ?
C9 C10 C18 C17 173.9(2) . . . . ?
C11 C10 C18 C7 171.4(2) . . . . ?
C9 C10 C18 C7 -10.5(3) . . . . ?
O1 C7 C18 C17 59.7(3) . . . . ?
C8 C7 C18 C17 171.7(2) . . . . ?
O1 C7 C18 C10 -115.5(2) . . . . ?
C8 C7 C18 C10 -3.5(2) . . . . ?
C7 O1 B1 O2 8.3(3) . . . . ?
C7 O1 B1 C1 -169.0(2) . . . . ?
C8 O2 B1 O1 -0.1(3) . . . . ?
C8 O2 B1 C1 177.4(2) . . . . ?
C2 C1 B1 O1 165.4(2) . . . . ?
C6 C1 B1 O1 -9.7(4) . . . . ?
C2 C1 B1 O2 -11.8(3) . . . . ?
C6 C1 B1 O2 173.1(2) . . . . ?
C14 O4 B2 O3 -1.6(3) . . . . ?
C14 O4 B2 C4 175.7(2) . . . 3_756 ?
C13 O3 B2 O4 9.4(3) . . . . ?
C13 O3 B2 C4 -167.8(2) . . . 3_756 ?
C105 C101 C102 C103 -0.4(6) . . . . ?
C101 C102 C103 C104 0.6(7) . . . . ?
C102 C103 C104 C105 -0.5(6) . . . 3_756 ?
C102 C101 C105 C104 -179.9(3) . . . 3_756 ?
C102 C101 C105 C105 0.1(6) . . . 3_756 ?

_refine_diff_density_max         0.355
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.052

_shelxl_version_number           2013-3



####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1005496'
_audit_update_record             
;
2014-05-27 deposited with the CCDC.
2016-06-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H40 B4 N4 O8 S2, C14 H10, 4(C H Cl3)'
_chemical_formula_sum            'C62 H54 B4 Cl12 N4 O8 S2'
_chemical_formula_weight         1515.85

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 '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                   10.54186(19)
_cell_length_b                   12.9408(2)
_cell_length_c                   14.3073(3)
_cell_angle_alpha                69.8702(7)
_cell_angle_beta                 73.6990(7)
_cell_angle_gamma                79.7710(7)
_cell_volume                     1751.79(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    14536
_cell_measurement_theta_min      4.39
_cell_measurement_theta_max      68.17

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             774
_exptl_absorpt_coefficient_mu    5.350
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5475
_exptl_absorpt_correction_T_max  0.6446
_exptl_absorpt_process_details   'Absorption was corrected by ABSCOR'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54186
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'rotating anode X-ray tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID II IP 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            20272
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_sigmaI/netI    0.0342
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_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         5.96
_diffrn_reflns_theta_max         68.22
_reflns_number_total             6288
_reflns_number_gt                4477
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'PROCESS-AUTO (Rigaku, 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0612P)²+1.2340P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6288
_refine_ls_number_parameters     471
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0514
_refine_ls_wR_factor_ref         0.1637
_refine_ls_wR_factor_gt          0.1284
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_restrained_S_all      1.139
_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
S1 S 0.85490(8) 0.95484(6) 0.46205(7) 0.0616(2) Uani 1 1 d . . .
O1 O 1.41187(19) 0.74224(17) 0.36396(15) 0.0526(5) Uani 1 1 d . . .
O2 O 1.26763(19) 0.83707(15) 0.26376(15) 0.0512(5) Uani 1 1 d . . .
O3 O 1.0727(2) 0.42127(19) 0.16242(16) 0.0608(6) Uani 1 1 d . . .
O4 O 1.25663(19) 0.33713(15) 0.22282(16) 0.0525(5) Uani 1 1 d . . .
N1 N 1.0050(2) 0.92045(19) 0.4078(2) 0.0534(6) Uani 1 1 d . . .
N2 N 0.8352(2) 0.8617(2) 0.5717(2) 0.0540(6) Uani 1 1 d . . .
C1 C 1.1815(3) 0.4626(3) 0.0781(2) 0.0532(7) Uani 1 1 d . . .
H1 H 1.1871 0.4346 0.0215 0.064 Uiso 1 1 calc R . .
C2 C 1.3044(3) 0.4182(2) 0.1240(2) 0.0503(7) Uani 1 1 d . . .
H2 H 1.3766 0.3862 0.0791 0.060 Uiso 1 1 calc R . .
C3 C 1.3424(3) 0.5177(2) 0.1380(2) 0.0435(6) Uani 1 1 d . . .
C4 C 1.4376(3) 0.5204(2) 0.1874(2) 0.0459(6) Uani 1 1 d . . .
H4 H 1.4908 0.4570 0.2126 0.055 Uiso 1 1 calc R . .
C5 C 1.4509(3) 0.6202(2) 0.1979(2) 0.0434(6) Uani 1 1 d . . .
C6 C 1.5509(3) 0.6452(2) 0.2438(2) 0.0503(7) Uani 1 1 d . . .
C7 C 1.4904(3) 0.7571(2) 0.2611(2) 0.0497(7) Uani 1 1 d . . .
H7 H 1.5594 0.8069 0.2438 0.060 Uiso 1 1 calc R . .
C8 C 1.3886(3) 0.8076(2) 0.1944(2) 0.0483(7) Uani 1 1 d . . .
H8 H 1.4200 0.8713 0.1356 0.058 Uiso 1 1 calc R . .
C9 C 1.3681(3) 0.7139(2) 0.1624(2) 0.0427(6) Uani 1 1 d . . .
C10 C 1.2755(3) 0.7120(2) 0.1100(2) 0.0466(6) Uani 1 1 d . . .
H10 H 1.2229 0.7756 0.0841 0.056 Uiso 1 1 calc R . .
C11 C 1.2643(3) 0.6126(2) 0.0976(2) 0.0433(6) Uani 1 1 d . . .
C12 C 1.1743(3) 0.5905(3) 0.0413(2) 0.0491(7) Uani 1 1 d . . .
C13 C 1.0341(3) 0.6456(3) 0.0648(3) 0.0674(9) Uani 1 1 d . . .
H13A H 0.9972 0.6217 0.1375 0.101 Uiso 1 1 calc R . .
H13B H 0.9801 0.6256 0.0309 0.101 Uiso 1 1 calc R . .
H13C H 1.0366 0.7244 0.0410 0.101 Uiso 1 1 calc R . .
C14 C 1.2344(4) 0.6300(3) -0.0741(2) 0.0672(9) Uani 1 1 d . . .
H14A H 1.2405 0.7083 -0.0965 0.101 Uiso 1 1 calc R . .
H14B H 1.1792 0.6136 -0.1093 0.101 Uiso 1 1 calc R . .
H14C H 1.3215 0.5930 -0.0889 0.101 Uiso 1 1 calc R . .
C15 C 1.6830(3) 0.6637(4) 0.1632(3) 0.0827(12) Uani 1 1 d . . .
H15A H 1.7175 0.5968 0.1464 0.124 Uiso 1 1 calc R . .
H15B H 1.7452 0.6840 0.1902 0.124 Uiso 1 1 calc R . .
H15C H 1.6689 0.7218 0.1027 0.124 Uiso 1 1 calc R . .
C16 C 1.5718(4) 0.5546(3) 0.3410(3) 0.0746(10) Uani 1 1 d . . .
H16A H 1.4889 0.5445 0.3912 0.112 Uiso 1 1 calc R . .
H16B H 1.6343 0.5753 0.3674 0.112 Uiso 1 1 calc R . .
H16C H 1.6055 0.4869 0.3256 0.112 Uiso 1 1 calc R . .
C17 C 1.1774(3) 0.7722(2) 0.4623(2) 0.0471(6) Uani 1 1 d . . .
C18 C 1.2010(3) 0.6862(3) 0.5454(2) 0.0551(7) Uani 1 1 d . . .
H18 H 1.2848 0.6479 0.5401 0.066 Uiso 1 1 calc R . .
C19 C 1.1047(3) 0.6522(3) 0.6391(2) 0.0574(8) Uani 1 1 d . . .
H19 H 1.1284 0.5929 0.6922 0.069 Uiso 1 1 calc R . .
C20 C 0.9781(3) 0.7028(2) 0.6551(2) 0.0501(7) Uani 1 1 d . . .
C21 C 0.9503(3) 0.7957(2) 0.5718(2) 0.0464(6) Uani 1 1 d . . .
C22 C 1.0475(3) 0.8298(2) 0.4772(2) 0.0448(6) Uani 1 1 d . . .
B1 B 1.2855(3) 0.7883(3) 0.3609(3) 0.0462(7) Uani 1 1 d . . .
B2 B 1.1207(3) 0.3494(3) 0.2422(3) 0.0505(8) Uani 1 1 d . . .
C23 C 0.8752(4) 0.5609(3) 0.5147(3) 0.0685(9) Uani 1 1 d . . .
C24 C 0.7513(4) 0.6259(4) 0.5257(4) 0.0858(12) Uani 1 1 d . . .
H24 H 0.6866 0.6048 0.5865 0.103 Uiso 1 1 calc R . .
C25 C 0.7259(5) 0.7169(4) 0.4504(4) 0.0956(14) Uani 1 1 d . . .
H25 H 0.6439 0.7576 0.4595 0.115 Uiso 1 1 calc R . .
C26 C 0.8220(6) 0.7516(4) 0.3577(4) 0.0953(14) Uani 1 1 d . . .
H26 H 0.8031 0.8148 0.3060 0.114 Uiso 1 1 calc R . .
C27 C 0.9427(5) 0.6927(4) 0.3438(3) 0.0839(12) Uani 1 1 d . . .
H27 H 1.0058 0.7170 0.2826 0.101 Uiso 1 1 calc R . .
C28 C 0.9740(4) 0.5956(3) 0.4201(3) 0.0691(9) Uani 1 1 d . . .
C29 C 0.9038(4) 0.4666(3) 0.5911(3) 0.0724(10) Uani 1 1 d . . .
H29 H 0.8395 0.4441 0.6518 0.087 Uiso 1 1 calc R . .
C30 C 1.5264(4) 0.8752(3) -0.2941(4) 0.0866(12) Uani 1 1 d . . .
H30 H 1.6176 0.8404 -0.3032 0.104 Uiso 1 1 calc R . .
Cl1 Cl 1.46322(15) 0.86283(16) -0.16408(13) 0.1387(6) Uani 1 1 d . . .
Cl2 Cl 1.43153(13) 0.80434(10) -0.33071(11) 0.1083(4) Uani 1 1 d . . .
Cl3 Cl 1.52906(14) 1.01318(9) -0.37047(14) 0.1277(6) Uani 1 1 d . . .
C31 C 0.9124(4) 0.9578(3) 0.8380(3) 0.0915(13) Uani 1 1 d D . .
H31 H 0.8940 1.0250 0.7835 0.110 Uiso 1 1 calc R A 1
Cl4 Cl 1.0765(6) 0.9464(9) 0.8414(5) 0.123(4) Uani 0.334(11) 1 d P B 1
Cl5 Cl 0.8310(16) 0.8544(10) 0.8397(11) 0.151(6) Uani 0.444(12) 1 d PD B 1
Cl6 Cl 0.8202(10) 0.9726(7) 0.9628(4) 0.105(3) Uani 0.334(11) 1 d PD B 1
Cl7 Cl 1.0713(6) 0.8880(8) 0.7972(8) 0.170(6) Uani 0.444(12) 1 d PD B 2
Cl8 Cl 0.7926(19) 0.8749(13) 0.8572(13) 0.134(4) Uani 0.334(11) 1 d P B 2
Cl9 Cl 0.8854(14) 0.9875(7) 0.9473(8) 0.194(6) Uani 0.444(12) 1 d PD B 2
Cl10 Cl 0.998(2) 0.8484(8) 0.8022(10) 0.192(11) Uani 0.232(7) 1 d PD B 3
Cl11 Cl 0.7786(16) 0.921(2) 0.9388(15) 0.311(12) Uiso 0.232(7) 1 d PD B 3
Cl12 Cl 1.005(2) 1.0229(11) 0.8765(13) 0.201(8) Uani 0.232(7) 1 d PD B 3


_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 N2 1.600(3) . ?
S1 N1 1.613(3) . ?
O1 B1 1.365(4) . ?
O1 C7 1.438(3) . ?
O2 B1 1.367(4) . ?
O2 C8 1.461(3) . ?
O3 B2 1.360(4) . ?
O3 C1 1.434(3) . ?
O4 B2 1.372(4) . ?
O4 C2 1.457(3) . ?
N1 C22 1.350(4) . ?
N2 C21 1.355(4) . ?
C1 C2 1.546(4) . ?
C1 C12 1.549(4) . ?
C1 H1 0.9800 . ?
C2 C3 1.504(4) . ?
C2 H2 0.9800 . ?
C3 C4 1.392(4) . ?
C3 C11 1.393(4) . ?
C4 C5 1.387(4) . ?
C4 H4 0.9300 . ?
C5 C9 1.393(4) . ?
C5 C6 1.517(4) . ?
C6 C16 1.521(5) . ?
C6 C15 1.534(4) . ?
C6 C7 1.547(4) . ?
C7 C8 1.544(4) . ?
C7 H7 0.9800 . ?
C8 C9 1.503(4) . ?
C8 H8 0.9800 . ?
C9 C10 1.395(4) . ?
C10 C11 1.387(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.522(4) . ?
C12 C13 1.522(4) . ?
C12 C14 1.528(4) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C18 1.367(4) . ?
C17 C22 1.435(4) . ?
C17 B1 1.548(4) . ?
C18 C19 1.418(4) . ?
C18 H18 0.9300 . ?
C19 C20 1.372(4) . ?
C19 H19 0.9300 . ?
C20 C21 1.427(4) . ?
C20 B2 1.552(4) 2_766 ?
C21 C22 1.431(4) . ?
B2 C20 1.552(4) 2_766 ?
C23 C29 1.382(6) . ?
C23 C24 1.422(6) . ?
C23 C28 1.440(5) . ?
C24 C25 1.339(6) . ?
C24 H24 0.9300 . ?
C25 C26 1.409(7) . ?
C25 H25 0.9300 . ?
C26 C27 1.363(6) . ?
C26 H26 0.9300 . ?
C27 C28 1.411(6) . ?
C27 H27 0.9300 . ?
C28 C29 1.393(5) 2_766 ?
C29 C28 1.393(5) 2_766 ?
C29 H29 0.9300 . ?
C30 Cl3 1.744(4) . ?
C30 Cl2 1.751(5) . ?
C30 Cl1 1.751(5) . ?
C30 H30 0.9800 . ?
C31 Cl9 1.674(8) . ?
C31 Cl10 1.693(7) . ?
C31 Cl12 1.699(9) . ?
C31 Cl5 1.703(8) . ?
C31 Cl8 1.705(12) . ?
C31 Cl11 1.710(10) . ?
C31 Cl4 1.723(7) . ?
C31 Cl7 1.799(6) . ?
C31 Cl6 1.835(6) . ?
C31 H31 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
N2 S1 N1 101.35(13) . . ?
B1 O1 C7 109.2(2) . . ?
B1 O2 C8 106.7(2) . . ?
B2 O3 C1 109.2(2) . . ?
B2 O4 C2 106.5(2) . . ?
C22 N1 S1 106.0(2) . . ?
C21 N2 S1 106.8(2) . . ?
O3 C1 C2 103.7(2) . . ?
O3 C1 C12 112.1(2) . . ?
C2 C1 C12 107.9(2) . . ?
O3 C1 H1 111.0 . . ?
C2 C1 H1 111.0 . . ?
C12 C1 H1 111.0 . . ?
O4 C2 C3 110.7(2) . . ?
O4 C2 C1 105.3(2) . . ?
C3 C2 C1 104.0(2) . . ?
O4 C2 H2 112.1 . . ?
C3 C2 H2 112.1 . . ?
C1 C2 H2 112.1 . . ?
C4 C3 C11 121.5(2) . . ?
C4 C3 C2 127.4(3) . . ?
C11 C3 C2 111.1(2) . . ?
C5 C4 C3 118.1(3) . . ?
C5 C4 H4 120.9 . . ?
C3 C4 H4 120.9 . . ?
C4 C5 C9 120.4(3) . . ?
C4 C5 C6 127.9(3) . . ?
C9 C5 C6 111.6(2) . . ?
C5 C6 C16 113.0(3) . . ?
C5 C6 C15 108.9(3) . . ?
C16 C6 C15 110.1(3) . . ?
C5 C6 C7 102.4(2) . . ?
C16 C6 C7 113.7(3) . . ?
C15 C6 C7 108.3(3) . . ?
O1 C7 C8 103.7(2) . . ?
O1 C7 C6 111.6(2) . . ?
C8 C7 C6 107.6(2) . . ?
O1 C7 H7 111.2 . . ?
C8 C7 H7 111.2 . . ?
C6 C7 H7 111.2 . . ?
O2 C8 C9 110.0(2) . . ?
O2 C8 C7 105.2(2) . . ?
C9 C8 C7 104.3(2) . . ?
O2 C8 H8 112.3 . . ?
C9 C8 H8 112.3 . . ?
C7 C8 H8 112.3 . . ?
C5 C9 C10 121.3(2) . . ?
C5 C9 C8 110.8(2) . . ?
C10 C9 C8 127.7(2) . . ?
C11 C10 C9 118.1(3) . . ?
C11 C10 H10 121.0 . . ?
C9 C10 H10 121.0 . . ?
C10 C11 C3 120.4(3) . . ?
C10 C11 C12 127.8(3) . . ?
C3 C11 C12 111.8(2) . . ?
C11 C12 C13 112.8(2) . . ?
C11 C12 C14 109.6(2) . . ?
C13 C12 C14 109.7(3) . . ?
C11 C12 C1 102.3(2) . . ?
C13 C12 C1 113.7(3) . . ?
C14 C12 C1 108.6(2) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
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 . . ?
C6 C15 H15A 109.5 . . ?
C6 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C6 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C6 C16 H16A 109.5 . . ?
C6 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C6 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 C22 115.1(3) . . ?
C18 C17 B1 117.2(3) . . ?
C22 C17 B1 127.3(3) . . ?
C17 C18 C19 123.7(3) . . ?
C17 C18 H18 118.2 . . ?
C19 C18 H18 118.2 . . ?
C20 C19 C18 123.0(3) . . ?
C20 C19 H19 118.5 . . ?
C18 C19 H19 118.5 . . ?
C19 C20 C21 115.4(3) . . ?
C19 C20 B2 117.5(3) . 2_766 ?
C21 C20 B2 127.0(3) . 2_766 ?
N2 C21 C20 126.0(3) . . ?
N2 C21 C22 112.5(3) . . ?
C20 C21 C22 121.5(3) . . ?
N1 C22 C21 113.4(2) . . ?
N1 C22 C17 125.2(3) . . ?
C21 C22 C17 121.3(3) . . ?
O1 B1 O2 113.6(3) . . ?
O1 B1 C17 119.2(3) . . ?
O2 B1 C17 127.0(3) . . ?
O3 B2 O4 113.8(3) . . ?
O3 B2 C20 119.2(3) . 2_766 ?
O4 B2 C20 126.9(3) . 2_766 ?
C29 C23 C24 122.5(4) . . ?
C29 C23 C28 119.3(4) . . ?
C24 C23 C28 118.2(4) . . ?
C25 C24 C23 121.4(5) . . ?
C25 C24 H24 119.3 . . ?
C23 C24 H24 119.3 . . ?
C24 C25 C26 120.8(5) . . ?
C24 C25 H25 119.6 . . ?
C26 C25 H25 119.6 . . ?
C27 C26 C25 120.1(5) . . ?
C27 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C26 C27 C28 121.4(4) . . ?
C26 C27 H27 119.3 . . ?
C28 C27 H27 119.3 . . ?
C29 C28 C27 123.1(4) 2_766 . ?
C29 C28 C23 118.8(4) 2_766 . ?
C27 C28 C23 118.1(4) . . ?
C23 C29 C28 122.0(4) . 2_766 ?
C23 C29 H29 119.0 . . ?
C28 C29 H29 119.0 2_766 . ?
Cl3 C30 Cl2 110.9(3) . . ?
Cl3 C30 Cl1 111.6(2) . . ?
Cl2 C30 Cl1 109.2(2) . . ?
Cl3 C30 H30 108.3 . . ?
Cl2 C30 H30 108.3 . . ?
Cl1 C30 H30 108.3 . . ?
Cl9 C31 Cl10 131.1(5) . . ?
Cl9 C31 Cl12 49.6(9) . . ?
Cl10 C31 Cl12 112.9(9) . . ?
Cl9 C31 Cl5 117.5(7) . . ?
Cl10 C31 Cl5 59.6(8) . . ?
Cl12 C31 Cl5 158.2(8) . . ?
Cl9 C31 Cl8 105.7(9) . . ?
Cl10 C31 Cl8 76.2(9) . . ?
Cl12 C31 Cl8 154.2(8) . . ?
Cl5 C31 Cl8 16.8(9) . . ?
Cl9 C31 Cl11 56.0(11) . . ?
Cl10 C31 Cl11 112.5(10) . . ?
Cl12 C31 Cl11 105.5(11) . . ?
Cl5 C31 Cl11 64.1(10) . . ?
Cl8 C31 Cl11 50.0(11) . . ?
Cl9 C31 Cl4 83.3(4) . . ?
Cl10 C31 Cl4 68.8(7) . . ?
Cl12 C31 Cl4 44.3(8) . . ?
Cl5 C31 Cl4 125.4(8) . . ?
Cl8 C31 Cl4 139.3(9) . . ?
Cl11 C31 Cl4 127.9(9) . . ?
Cl9 C31 Cl7 116.8(5) . . ?
Cl10 C31 Cl7 32.2(7) . . ?
Cl12 C31 Cl7 82.4(10) . . ?
Cl5 C31 Cl7 91.7(8) . . ?
Cl8 C31 Cl7 108.2(10) . . ?
Cl11 C31 Cl7 133.8(8) . . ?
Cl4 C31 Cl7 38.3(4) . . ?
Cl9 C31 Cl6 22.4(4) . . ?
Cl10 C31 Cl6 132.6(6) . . ?
Cl12 C31 Cl6 71.7(9) . . ?
Cl5 C31 Cl6 98.0(6) . . ?
Cl8 C31 Cl6 84.4(8) . . ?
Cl11 C31 Cl6 34.3(11) . . ?
Cl4 C31 Cl6 104.1(4) . . ?
Cl7 C31 Cl6 132.4(5) . . ?
Cl9 C31 H31 109.3 . . ?
Cl10 C31 H31 117.4 . . ?
Cl12 C31 H31 92.4 . . ?
Cl5 C31 H31 109.3 . . ?
Cl8 C31 H31 104.9 . . ?
Cl11 C31 H31 113.9 . . ?
Cl4 C31 H31 109.3 . . ?
Cl7 C31 H31 111.1 . . ?
Cl6 C31 H31 109.3 . . ?

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
N2 S1 N1 C22 0.1(2) . . . . ?
N1 S1 N2 C21 0.0(2) . . . . ?
B2 O3 C1 C2 -8.2(3) . . . . ?
B2 O3 C1 C12 -124.2(3) . . . . ?
B2 O4 C2 C3 100.5(3) . . . . ?
B2 O4 C2 C1 -11.3(3) . . . . ?
O3 C1 C2 O4 11.8(3) . . . . ?
C12 C1 C2 O4 130.8(2) . . . . ?
O3 C1 C2 C3 -104.7(2) . . . . ?
C12 C1 C2 C3 14.4(3) . . . . ?
O4 C2 C3 C4 59.6(4) . . . . ?
C1 C2 C3 C4 172.2(3) . . . . ?
O4 C2 C3 C11 -118.0(3) . . . . ?
C1 C2 C3 C11 -5.3(3) . . . . ?
C11 C3 C4 C5 1.6(4) . . . . ?
C2 C3 C4 C5 -175.6(3) . . . . ?
C3 C4 C5 C9 1.8(4) . . . . ?
C3 C4 C5 C6 -176.8(3) . . . . ?
C4 C5 C6 C16 -42.0(4) . . . . ?
C9 C5 C6 C16 139.3(3) . . . . ?
C4 C5 C6 C15 80.8(4) . . . . ?
C9 C5 C6 C15 -98.0(3) . . . . ?
C4 C5 C6 C7 -164.7(3) . . . . ?
C9 C5 C6 C7 16.6(3) . . . . ?
B1 O1 C7 C8 -6.3(3) . . . . ?
B1 O1 C7 C6 -121.8(3) . . . . ?
C5 C6 C7 O1 95.2(3) . . . . ?
C16 C6 C7 O1 -27.0(4) . . . . ?
C15 C6 C7 O1 -149.8(3) . . . . ?
C5 C6 C7 C8 -18.0(3) . . . . ?
C16 C6 C7 C8 -140.2(3) . . . . ?
C15 C6 C7 C8 97.0(3) . . . . ?
B1 O2 C8 C9 99.8(3) . . . . ?
B1 O2 C8 C7 -12.0(3) . . . . ?
O1 C7 C8 O2 11.1(3) . . . . ?
C6 C7 C8 O2 129.4(2) . . . . ?
O1 C7 C8 C9 -104.7(2) . . . . ?
C6 C7 C8 C9 13.6(3) . . . . ?
C4 C5 C9 C10 -4.0(4) . . . . ?
C6 C5 C9 C10 174.9(2) . . . . ?
C4 C5 C9 C8 172.5(2) . . . . ?
C6 C5 C9 C8 -8.6(3) . . . . ?
O2 C8 C9 C5 -115.8(2) . . . . ?
C7 C8 C9 C5 -3.4(3) . . . . ?
O2 C8 C9 C10 60.4(4) . . . . ?
C7 C8 C9 C10 172.8(3) . . . . ?
C5 C9 C10 C11 2.5(4) . . . . ?
C8 C9 C10 C11 -173.3(3) . . . . ?
C9 C10 C11 C3 1.0(4) . . . . ?
C9 C10 C11 C12 -178.2(2) . . . . ?
C4 C3 C11 C10 -3.1(4) . . . . ?
C2 C3 C11 C10 174.6(2) . . . . ?
C4 C3 C11 C12 176.2(2) . . . . ?
C2 C3 C11 C12 -6.1(3) . . . . ?
C10 C11 C12 C13 -43.7(4) . . . . ?
C3 C11 C12 C13 137.0(3) . . . . ?
C10 C11 C12 C14 78.8(3) . . . . ?
C3 C11 C12 C14 -100.5(3) . . . . ?
C10 C11 C12 C1 -166.2(3) . . . . ?
C3 C11 C12 C1 14.6(3) . . . . ?
O3 C1 C12 C11 96.2(3) . . . . ?
C2 C1 C12 C11 -17.3(3) . . . . ?
O3 C1 C12 C13 -25.6(3) . . . . ?
C2 C1 C12 C13 -139.2(3) . . . . ?
O3 C1 C12 C14 -148.0(2) . . . . ?
C2 C1 C12 C14 98.4(3) . . . . ?
C22 C17 C18 C19 2.1(4) . . . . ?
B1 C17 C18 C19 -171.3(3) . . . . ?
C17 C18 C19 C20 0.1(5) . . . . ?
C18 C19 C20 C21 -2.3(5) . . . . ?
C18 C19 C20 B2 174.7(3) . . . 2_766 ?
S1 N2 C21 C20 178.7(2) . . . . ?
S1 N2 C21 C22 -0.1(3) . . . . ?
C19 C20 C21 N2 -176.4(3) . . . . ?
B2 C20 C21 N2 6.9(5) 2_766 . . . ?
C19 C20 C21 C22 2.3(4) . . . . ?
B2 C20 C21 C22 -174.3(3) 2_766 . . . ?
S1 N1 C22 C21 -0.1(3) . . . . ?
S1 N1 C22 C17 -178.6(2) . . . . ?
N2 C21 C22 N1 0.1(3) . . . . ?
C20 C21 C22 N1 -178.7(2) . . . . ?
N2 C21 C22 C17 178.7(2) . . . . ?
C20 C21 C22 C17 -0.2(4) . . . . ?
C18 C17 C22 N1 176.4(3) . . . . ?
B1 C17 C22 N1 -11.0(5) . . . . ?
C18 C17 C22 C21 -2.0(4) . . . . ?
B1 C17 C22 C21 170.6(3) . . . . ?
C7 O1 B1 O2 -1.3(3) . . . . ?
C7 O1 B1 C17 173.5(2) . . . . ?
C8 O2 B1 O1 8.7(3) . . . . ?
C8 O2 B1 C17 -165.5(3) . . . . ?
C18 C17 B1 O1 -20.1(4) . . . . ?
C22 C17 B1 O1 167.4(3) . . . . ?
C18 C17 B1 O2 153.8(3) . . . . ?
C22 C17 B1 O2 -18.6(5) . . . . ?
C1 O3 B2 O4 1.2(4) . . . . ?
C1 O3 B2 C20 177.2(3) . . . 2_766 ?
C2 O4 B2 O3 6.8(3) . . . . ?
C2 O4 B2 C20 -168.8(3) . . . 2_766 ?
C29 C23 C24 C25 -179.9(4) . . . . ?
C28 C23 C24 C25 0.3(5) . . . . ?
C23 C24 C25 C26 -0.5(6) . . . . ?
C24 C25 C26 C27 -0.1(6) . . . . ?
C25 C26 C27 C28 0.9(6) . . . . ?
C26 C27 C28 C29 -179.8(4) . . . 2_766 ?
C26 C27 C28 C23 -1.0(5) . . . . ?
C29 C23 C28 C29 -0.6(5) . . . 2_766 ?
C24 C23 C28 C29 179.3(3) . . . 2_766 ?
C29 C23 C28 C27 -179.4(3) . . . . ?
C24 C23 C28 C27 0.4(5) . . . . ?
C24 C23 C29 C28 -179.2(3) . . . 2_766 ?
C28 C23 C29 C28 0.6(5) . . . 2_766 ?

_diffrn_measured_fraction_theta_max 0.979
_diffrn_reflns_theta_full        68.22
_diffrn_measured_fraction_theta_full 0.979
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.063
####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1005497'
_audit_update_record             
;
2014-05-27 deposited with the CCDC.
2016-06-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H40 B4 N4 O8 S2, 5(C H Cl3)'
_chemical_formula_sum            'C49 H45 B4 Cl15 N4 O8 S2'
_chemical_formula_weight         1457.00

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

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

_cell_length_a                   13.7207(3)
_cell_length_b                   14.0837(3)
_cell_length_c                   20.4986(3)
_cell_angle_alpha                90
_cell_angle_beta                 122.8400(10)
_cell_angle_gamma                90
_cell_volume                     3328.08(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    13150
_cell_measurement_theta_min      3.14
_cell_measurement_theta_max      68.20

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_F_000             1476
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.178
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.104
_exptl_absorpt_coefficient_mu    6.686
_shelx_estimated_absorpt_T_min   0.382
_shelx_estimated_absorpt_T_max   0.543
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8226
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'Absorption was corrected by ABSCOR'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     1.54186
_diffrn_radiation_type           CuK\a
_diffrn_source                   'rotating anode X-ray tube'
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID II IP Area Detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37340
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_av_R_equivalents  0.0609
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.835
_diffrn_reflns_theta_max         68.228
_diffrn_reflns_theta_full        67.686
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6087
_reflns_number_gt                5469
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'PROCESS-AUTO (Rigaku, 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2008)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'

_refine_special_details          
; 
 ? 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0506P)²+4.7534P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6087
_refine_ls_number_parameters     405
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0481
_refine_ls_wR_factor_ref         0.1233
_refine_ls_wR_factor_gt          0.1183
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.098
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.20597(7) 0.18081(5) -0.25448(4) 0.02885(18) Uani 1 1 d . . . . .
O1 O 0.06185(14) -0.04364(11) -0.15909(9) 0.0161(4) Uani 1 1 d . . . . .
O2 O 0.08987(15) -0.00784(12) -0.04058(10) 0.0187(4) Uani 1 1 d . . . . .
O3 O 0.48836(14) -0.35397(12) 0.05110(9) 0.0157(4) Uani 1 1 d . . . . .
O4 O 0.49072(14) -0.36282(12) -0.05998(10) 0.0187(4) Uani 1 1 d . . . . .
N1 N 0.1516(2) 0.11658(16) -0.21640(12) 0.0226(5) Uani 1 1 d . . . . .
N2 N 0.2971(2) 0.24614(16) -0.18139(13) 0.0235(5) Uani 1 1 d . . . . .
B1 B 0.1091(2) 0.0170(2) -0.09711(16) 0.0156(5) Uani 1 1 d . . . . .
B2 B 0.4592(2) 0.32666(19) -0.01320(16) 0.0156(5) Uani 1 1 d . . . . .
C1 C 0.1851(2) 0.10579(17) -0.08539(14) 0.0162(5) Uani 1 1 d . . . . .
C2 C 0.2055(2) 0.14463(17) -0.14141(14) 0.0163(5) Uani 1 1 d . . . . .
C3 C 0.2889(2) 0.21877(17) -0.12138(14) 0.0162(5) Uani 1 1 d . . . . .
C4 C 0.3547(2) 0.25714(17) -0.04432(14) 0.0167(5) Uani 1 1 d . . . . .
C5 C 0.3301(2) 0.22061(19) 0.00727(15) 0.0209(5) Uani 1 1 d . . . . .
H5 H 0.3698 0.2456 0.0585 0.025 Uiso 1 1 calc R U . . .
C6 C 0.2476(2) 0.14693(19) -0.01284(15) 0.0193(5) Uani 1 1 d . . . . .
H6 H 0.2349 0.1249 0.0258 0.023 Uiso 1 1 calc R U . . .
C7 C 0.0186(2) -0.12527(17) -0.13810(14) 0.0150(5) Uani 1 1 d . . . . .
H7 H -0.0612 -0.1443 -0.1810 0.018 Uiso 1 1 calc R U . . .
C8 C 0.0230(2) -0.09440(17) -0.06353(14) 0.0162(5) Uani 1 1 d . . . . .
H8 H -0.0566 -0.0831 -0.0747 0.019 Uiso 1 1 calc R U . . .
C9 C 0.0859(2) -0.17457(18) -0.00290(14) 0.0182(5) Uani 1 1 d . . . . .
C10 C 0.1500(2) -0.22721(16) -0.03347(14) 0.0138(5) Uani 1 1 d . . . . .
C11 C 0.2398(2) -0.29207(17) 0.00553(14) 0.0157(5) Uani 1 1 d . . . . .
H11 H 0.2729 -0.3057 0.0589 0.019 Uiso 1 1 calc R U . . .
C12 C 0.2796(2) -0.33651(16) -0.03651(14) 0.0137(5) Uani 1 1 d . . . . .
C13 C 0.3812(2) -0.40298(16) -0.00647(14) 0.0141(5) Uani 1 1 d . . . . .
H13 H 0.3698 -0.4635 0.0140 0.017 Uiso 1 1 calc R U . . .
C14 C 0.3917(2) -0.41959(17) -0.07755(14) 0.0158(5) Uani 1 1 d . . . . .
H14 H 0.4051 -0.4882 -0.0827 0.019 Uiso 1 1 calc R U . . .
C15 C 0.2782(2) -0.38381(17) -0.15034(14) 0.0161(5) Uani 1 1 d . . . . .
C16 C 0.2280(2) -0.31991(16) -0.11596(13) 0.0135(5) Uani 1 1 d . . . . .
C17 C 0.1399(2) -0.25355(17) -0.15435(14) 0.0145(5) Uani 1 1 d . . . . .
H17 H 0.1055 -0.2408 -0.2080 0.017 Uiso 1 1 calc R U . . .
C18 C 0.1034(2) -0.20630(16) -0.11158(14) 0.0141(5) Uani 1 1 d . . . . .
C19 C 0.1650(3) -0.1379(2) 0.08006(15) 0.0291(7) Uani 1 1 d . . . . .
H19A H 0.2021 -0.1918 0.1155 0.044 Uiso 1 1 calc R U . . .
H19B H 0.1190 -0.1019 0.0950 0.044 Uiso 1 1 calc R U . . .
H19C H 0.2247 -0.0967 0.0829 0.044 Uiso 1 1 calc R U . . .
C20 C -0.0073(3) -0.24131(19) -0.00819(17) 0.0264(6) Uani 1 1 d . . . . .
H20A H -0.0609 -0.2606 -0.0623 0.040 Uiso 1 1 calc R U . . .
H20B H -0.0504 -0.2080 0.0105 0.040 Uiso 1 1 calc R U . . .
H20C H 0.0301 -0.2977 0.0239 0.040 Uiso 1 1 calc R U . . .
C21 C 0.2979(2) -0.3333(2) -0.20816(16) 0.0256(6) Uani 1 1 d . . . . .
H21A H 0.2230 -0.3153 -0.2542 0.038 Uiso 1 1 calc R U . . .
H21B H 0.3387 -0.3760 -0.2234 0.038 Uiso 1 1 calc R U . . .
H21C H 0.3448 -0.2762 -0.1840 0.038 Uiso 1 1 calc R U . . .
C22 C 0.1976(2) -0.4702(2) -0.18882(17) 0.0278(6) Uani 1 1 d . . . . .
H22A H 0.1920 -0.5054 -0.1497 0.042 Uiso 1 1 calc R U . . .
H22B H 0.2293 -0.5117 -0.2113 0.042 Uiso 1 1 calc R U . . .
H22C H 0.1203 -0.4483 -0.2299 0.042 Uiso 1 1 calc R U . . .
C101 C 0.0448(2) -0.05886(18) -0.33024(15) 0.0208(5) Uani 1 1 d D . . . .
H101 H 0.0517 -0.0299 -0.2834 0.025 Uiso 1 1 calc R U . . .
Cl1 Cl -0.01462(7) 0.02602(5) -0.40511(4) 0.03283(18) Uani 1 1 d D . . . .
Cl2 Cl -0.04759(6) -0.15932(5) -0.35857(4) 0.02620(16) Uani 1 1 d D . . . .
Cl3 Cl 0.18395(6) -0.09325(5) -0.30609(5) 0.03585(19) Uani 1 1 d D . . . .
C102 C 0.5489(3) -0.1303(2) -0.27474(17) 0.0304(6) Uani 1 1 d . . . . .
H102 H 0.5615 -0.1534 -0.3158 0.036 Uiso 1 1 calc R U . A 1
Cl4 Cl 0.6843(2) -0.10470(19) -0.19009(17) 0.0447(8) Uani 0.889(7) 1 d . . P B
1
Cl5 Cl 0.47857(17) -0.21812(16) -0.25603(7) 0.0570(6) Uani 0.889(7) 1 d . . P B
1
Cl6 Cl 0.46308(13) -0.02538(15) -0.30836(7) 0.0496(5) Uani 0.889(7) 1 d . . P B
1
Cl4B Cl 0.6945(15) -0.0972(9) -0.1906(10) 0.010(3) Uiso 0.111(7) 1 d . . P B 2
Cl5B Cl 0.5177(14) -0.2514(10) -0.2449(9) 0.058(4) Uiso 0.111(7) 1 d . . P B 2
Cl6B Cl 0.4436(8) -0.0633(11) -0.2995(6) 0.041(3) Uiso 0.111(7) 1 d . . P B 2
C104 C 0.5219(8) -0.0141(9) 0.0140(7) 0.090(4) Uani 0.5 1 d D . P C -1
H104 H 0.5824 -0.0636 0.0280 0.108 Uiso 0.5 1 d R U P C -1
Cl7 Cl 0.5689(7) 0.0840(4) -0.0151(6) 0.206(3) Uani 0.5 1 d D U P C -1
Cl8 Cl 0.5187(5) -0.0030(5) 0.0984(3) 0.179(2) Uani 0.5 1 d D U P C -1
Cl9 Cl 0.3975(4) -0.0601(5) -0.0635(4) 0.198(3) Uani 0.5 1 d D U P C -1


_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 N1 1.618(2) . ?
S1 N2 1.620(2) . ?
O1 B1 1.368(3) . ?
O1 C7 1.461(3) . ?
O2 B1 1.367(3) . ?
O2 C8 1.442(3) . ?
O3 B2 1.369(3) 3_655 ?
O3 C13 1.466(3) . ?
O4 B2 1.365(3) 3_655 ?
O4 C14 1.444(3) . ?
N1 C2 1.354(3) . ?
N2 C3 1.351(3) . ?
B1 C1 1.561(4) . ?
B2 O4 1.365(3) 3_655 ?
B2 O3 1.369(3) 3_655 ?
B2 C4 1.558(4) . ?
C1 C6 1.378(3) . ?
C1 C2 1.431(3) . ?
C2 C3 1.434(3) . ?
C3 C4 1.434(3) . ?
C4 C5 1.373(4) . ?
C5 C6 1.422(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C18 1.505(3) . ?
C7 C8 1.558(3) . ?
C7 H7 1.0000 . ?
C8 C9 1.550(3) . ?
C8 H8 1.0000 . ?
C9 C10 1.521(3) . ?
C9 C19 1.528(4) . ?
C9 C20 1.543(4) . ?
C10 C11 1.386(3) . ?
C10 C18 1.396(3) . ?
C11 C12 1.394(3) . ?
C11 H11 0.9500 . ?
C12 C16 1.399(3) . ?
C12 C13 1.506(3) . ?
C13 C14 1.557(3) . ?
C13 H13 1.0000 . ?
C14 C15 1.545(3) . ?
C14 H14 1.0000 . ?
C15 C16 1.518(3) . ?
C15 C21 1.527(3) . ?
C15 C22 1.542(3) . ?
C16 C17 1.387(3) . ?
C17 C18 1.392(3) . ?
C17 H17 0.9500 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C101 Cl1 1.758(3) . ?
C101 Cl3 1.761(3) . ?
C101 Cl2 1.774(3) . ?
C101 H101 1.0000 . ?
C102 Cl6B 1.562(11) . ?
C102 Cl5 1.735(3) . ?
C102 Cl4 1.759(4) . ?
C102 Cl6 1.779(3) . ?
C102 Cl4B 1.855(18) . ?
C102 Cl5B 1.937(14) . ?
C102 H102 1.0000 . ?
C104 Cl9 1.707(12) . ?
C104 Cl8 1.760(14) . ?
C104 Cl7 1.759(14) . ?
C104 H104 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 S1 N2 101.43(12) . . ?
B1 O1 C7 106.35(19) . . ?
B1 O2 C8 108.72(19) . . ?
B2 O3 C13 106.35(18) 3_655 . ?
B2 O4 C14 108.99(19) 3_655 . ?
C2 N1 S1 105.86(18) . . ?
C3 N2 S1 106.04(17) . . ?
O2 B1 O1 114.5(2) . . ?
O2 B1 C1 119.6(2) . . ?
O1 B1 C1 125.7(2) . . ?
O4 B2 O3 114.4(2) 3_655 3_655 ?
O4 B2 C4 119.2(2) 3_655 . ?
O3 B2 C4 126.4(2) 3_655 . ?
C6 C1 C2 115.3(2) . . ?
C6 C1 B1 118.4(2) . . ?
C2 C1 B1 126.0(2) . . ?
N1 C2 C1 125.1(2) . . ?
N1 C2 C3 113.4(2) . . ?
C1 C2 C3 121.4(2) . . ?
N2 C3 C4 125.6(2) . . ?
N2 C3 C2 113.2(2) . . ?
C4 C3 C2 121.2(2) . . ?
C5 C4 C3 115.9(2) . . ?
C5 C4 B2 118.4(2) . . ?
C3 C4 B2 125.3(2) . . ?
C4 C5 C6 122.7(2) . . ?
C4 C5 H5 118.7 . . ?
C6 C5 H5 118.7 . . ?
C1 C6 C5 123.5(2) . . ?
C1 C6 H6 118.3 . . ?
C5 C6 H6 118.3 . . ?
O1 C7 C18 110.21(19) . . ?
O1 C7 C8 105.26(18) . . ?
C18 C7 C8 104.23(19) . . ?
O1 C7 H7 112.2 . . ?
C18 C7 H7 112.2 . . ?
C8 C7 H7 112.2 . . ?
O2 C8 C9 112.0(2) . . ?
O2 C8 C7 103.61(18) . . ?
C9 C8 C7 106.98(19) . . ?
O2 C8 H8 111.3 . . ?
C9 C8 H8 111.3 . . ?
C7 C8 H8 111.3 . . ?
C10 C9 C19 113.7(2) . . ?
C10 C9 C20 108.5(2) . . ?
C19 C9 C20 110.2(2) . . ?
C10 C9 C8 102.68(19) . . ?
C19 C9 C8 113.4(2) . . ?
C20 C9 C8 107.9(2) . . ?
C11 C10 C18 120.8(2) . . ?
C11 C10 C9 127.9(2) . . ?
C18 C10 C9 111.2(2) . . ?
C10 C11 C12 117.6(2) . . ?
C10 C11 H11 121.2 . . ?
C12 C11 H11 121.2 . . ?
C11 C12 C16 121.6(2) . . ?
C11 C12 C13 127.8(2) . . ?
C16 C12 C13 110.6(2) . . ?
O3 C13 C12 109.78(18) . . ?
O3 C13 C14 105.24(18) . . ?
C12 C13 C14 104.21(19) . . ?
O3 C13 H13 112.4 . . ?
C12 C13 H13 112.4 . . ?
C14 C13 H13 112.4 . . ?
O4 C14 C15 112.33(19) . . ?
O4 C14 C13 103.61(18) . . ?
C15 C14 C13 107.35(18) . . ?
O4 C14 H14 111.1 . . ?
C15 C14 H14 111.1 . . ?
C13 C14 H14 111.1 . . ?
C16 C15 C21 113.6(2) . . ?
C16 C15 C22 109.0(2) . . ?
C21 C15 C22 110.5(2) . . ?
C16 C15 C14 102.61(19) . . ?
C21 C15 C14 113.0(2) . . ?
C22 C15 C14 107.7(2) . . ?
C17 C16 C12 120.5(2) . . ?
C17 C16 C15 127.7(2) . . ?
C12 C16 C15 111.8(2) . . ?
C16 C17 C18 117.7(2) . . ?
C16 C17 H17 121.1 . . ?
C18 C17 H17 121.1 . . ?
C17 C18 C10 121.6(2) . . ?
C17 C18 C7 127.3(2) . . ?
C10 C18 C7 111.0(2) . . ?
C9 C19 H19A 109.5 . . ?
C9 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C9 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C9 C20 H20A 109.5 . . ?
C9 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C9 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C15 C21 H21A 109.5 . . ?
C15 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C15 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C15 C22 H22A 109.5 . . ?
C15 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C15 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Cl1 C101 Cl3 110.56(14) . . ?
Cl1 C101 Cl2 110.22(14) . . ?
Cl3 C101 Cl2 110.24(14) . . ?
Cl1 C101 H101 108.6 . . ?
Cl3 C101 H101 108.6 . . ?
Cl2 C101 H101 108.6 . . ?
Cl5 C102 Cl4 110.14(18) . . ?
Cl5 C102 Cl6 110.28(18) . . ?
Cl4 C102 Cl6 109.58(19) . . ?
Cl6B C102 Cl4B 119.4(6) . . ?
Cl6B C102 Cl5B 108.1(5) . . ?
Cl4B C102 Cl5B 103.8(6) . . ?
Cl5 C102 H102 108.9 . . ?
Cl4 C102 H102 108.9 . . ?
Cl6 C102 H102 108.9 . . ?
Cl9 C104 Cl8 113.8(8) . . ?
Cl9 C104 Cl7 110.4(7) . . ?
Cl8 C104 Cl7 118.2(8) . . ?
Cl9 C104 H104 105.0 . . ?
Cl8 C104 H104 103.8 . . ?
Cl7 C104 H104 104.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 S1 N1 C2 -0.4(2) . . . . ?
N1 S1 N2 C3 0.4(2) . . . . ?
C8 O2 B1 O1 0.2(3) . . . . ?
C8 O2 B1 C1 -177.0(2) . . . . ?
C7 O1 B1 O2 -8.1(3) . . . . ?
C7 O1 B1 C1 168.9(2) . . . . ?
O2 B1 C1 C6 11.4(3) . . . . ?
O1 B1 C1 C6 -165.5(2) . . . . ?
O2 B1 C1 C2 -174.9(2) . . . . ?
O1 B1 C1 C2 8.2(4) . . . . ?
S1 N1 C2 C1 -179.3(2) . . . . ?
S1 N1 C2 C3 0.2(3) . . . . ?
C6 C1 C2 N1 -178.3(2) . . . . ?
B1 C1 C2 N1 7.9(4) . . . . ?
C6 C1 C2 C3 2.2(3) . . . . ?
B1 C1 C2 C3 -171.6(2) . . . . ?
S1 N2 C3 C4 179.5(2) . . . . ?
S1 N2 C3 C2 -0.3(3) . . . . ?
N1 C2 C3 N2 0.0(3) . . . . ?
C1 C2 C3 N2 179.6(2) . . . . ?
N1 C2 C3 C4 -179.8(2) . . . . ?
C1 C2 C3 C4 -0.2(3) . . . . ?
N2 C3 C4 C5 178.2(2) . . . . ?
C2 C3 C4 C5 -2.0(3) . . . . ?
N2 C3 C4 B2 -9.2(4) . . . . ?
C2 C3 C4 B2 170.6(2) . . . . ?
O4 B2 C4 C5 -12.0(3) 3_655 . . . ?
O3 B2 C4 C5 165.2(2) 3_655 . . . ?
O4 B2 C4 C3 175.6(2) 3_655 . . . ?
O3 B2 C4 C3 -7.2(4) 3_655 . . . ?
C3 C4 C5 C6 2.2(4) . . . . ?
B2 C4 C5 C6 -171.0(2) . . . . ?
C2 C1 C6 C5 -2.1(4) . . . . ?
B1 C1 C6 C5 172.3(2) . . . . ?
C4 C5 C6 C1 -0.1(4) . . . . ?
B1 O1 C7 C18 -100.0(2) . . . . ?
B1 O1 C7 C8 11.8(2) . . . . ?
B1 O2 C8 C9 122.1(2) . . . . ?
B1 O2 C8 C7 7.1(2) . . . . ?
O1 C7 C8 O2 -11.6(2) . . . . ?
C18 C7 C8 O2 104.5(2) . . . . ?
O1 C7 C8 C9 -130.08(19) . . . . ?
C18 C7 C8 C9 -14.1(2) . . . . ?
O2 C8 C9 C10 -93.6(2) . . . . ?
C7 C8 C9 C10 19.3(2) . . . . ?
O2 C8 C9 C19 29.6(3) . . . . ?
C7 C8 C9 C19 142.5(2) . . . . ?
O2 C8 C9 C20 152.0(2) . . . . ?
C7 C8 C9 C20 -95.1(2) . . . . ?
C19 C9 C10 C11 41.6(4) . . . . ?
C20 C9 C10 C11 -81.4(3) . . . . ?
C8 C9 C10 C11 164.6(2) . . . . ?
C19 C9 C10 C18 -141.4(2) . . . . ?
C20 C9 C10 C18 95.6(2) . . . . ?
C8 C9 C10 C18 -18.5(3) . . . . ?
C18 C10 C11 C12 -1.2(3) . . . . ?
C9 C10 C11 C12 175.5(2) . . . . ?
C10 C11 C12 C16 -2.8(3) . . . . ?
C10 C11 C12 C13 174.7(2) . . . . ?
B2 O3 C13 C12 -99.7(2) 3_655 . . . ?
B2 O3 C13 C14 11.9(2) 3_655 . . . ?
C11 C12 C13 O3 -61.2(3) . . . . ?
C16 C12 C13 O3 116.5(2) . . . . ?
C11 C12 C13 C14 -173.5(2) . . . . ?
C16 C12 C13 C14 4.2(2) . . . . ?
B2 O4 C14 C15 121.7(2) 3_655 . . . ?
B2 O4 C14 C13 6.1(2) 3_655 . . . ?
O3 C13 C14 O4 -10.9(2) . . . . ?
C12 C13 C14 O4 104.6(2) . . . . ?
O3 C13 C14 C15 -129.96(19) . . . . ?
C12 C13 C14 C15 -14.4(2) . . . . ?
O4 C14 C15 C16 -94.7(2) . . . . ?
C13 C14 C15 C16 18.5(2) . . . . ?
O4 C14 C15 C21 28.0(3) . . . . ?
C13 C14 C15 C21 141.2(2) . . . . ?
O4 C14 C15 C22 150.31(19) . . . . ?
C13 C14 C15 C22 -96.4(2) . . . . ?
C11 C12 C16 C17 4.2(4) . . . . ?
C13 C12 C16 C17 -173.7(2) . . . . ?
C11 C12 C16 C15 -174.1(2) . . . . ?
C13 C12 C16 C15 8.1(3) . . . . ?
C21 C15 C16 C17 42.9(3) . . . . ?
C22 C15 C16 C17 -80.7(3) . . . . ?
C14 C15 C16 C17 165.2(2) . . . . ?
C21 C15 C16 C12 -139.0(2) . . . . ?
C22 C15 C16 C12 97.4(2) . . . . ?
C14 C15 C16 C12 -16.6(3) . . . . ?
C12 C16 C17 C18 -1.4(3) . . . . ?
C15 C16 C17 C18 176.5(2) . . . . ?
C16 C17 C18 C10 -2.6(3) . . . . ?
C16 C17 C18 C7 173.4(2) . . . . ?
C11 C10 C18 C17 4.0(4) . . . . ?
C9 C10 C18 C17 -173.3(2) . . . . ?
C11 C10 C18 C7 -172.6(2) . . . . ?
C9 C10 C18 C7 10.2(3) . . . . ?
O1 C7 C18 C17 -61.1(3) . . . . ?
C8 C7 C18 C17 -173.6(2) . . . . ?
O1 C7 C18 C10 115.2(2) . . . . ?
C8 C7 C18 C10 2.7(3) . . . . ?

_refine_diff_density_max         0.669
_refine_diff_density_min         -0.827
_refine_diff_density_rms         0.077


####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1005498'
_audit_update_record             
;
2014-05-27 deposited with the CCDC.
2016-06-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C56 H50 B4 Cl12 N4 O8 S3'
_chemical_formula_sum            'C56 H50 B4 Cl12 N4 O8 S3'
_chemical_formula_weight         1471.82

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'
B B 0.0013 0.0007 '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                   13.6699(7)
_cell_length_b                   14.0308(9)
_cell_length_c                   20.6325(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 122.572(3)
_cell_angle_gamma                90.00
_cell_volume                     3334.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    34125
_cell_measurement_theta_min      3.02
_cell_measurement_theta_max      27.41

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1500
_exptl_absorpt_coefficient_mu    0.646
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7456
_exptl_absorpt_correction_T_max  0.9459
_exptl_absorpt_process_details   'Absorption was corrected by ABSCOR'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode X-ray tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID II IP 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            52063
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         27.41
_reflns_number_total             7560
_reflns_number_gt                5594
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'PROCESS-AUTO (Rigaku, 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0796P)²+1.5154P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7560
_refine_ls_number_parameters     418
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0503
_refine_ls_wR_factor_ref         0.1473
_refine_ls_wR_factor_gt          0.1339
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.058
_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 -0.20308(19) 0.78846(17) -0.11981(13) 0.0254(5) Uani 1 1 d . . .
C2 C -0.28687(19) 0.86312(17) -0.13957(13) 0.0260(5) Uani 1 1 d . . .
C3 C -0.30740(19) 0.90237(16) -0.08417(13) 0.0252(5) Uani 1 1 d . . .
C4 C -0.2436(2) 0.86315(18) -0.01174(14) 0.0293(5) Uani 1 1 d . . .
H4 H -0.2551 0.8867 0.0268 0.035 Uiso 1 1 calc R . .
C5 C -0.1612(2) 0.78907(18) 0.00800(13) 0.0293(5) Uani 1 1 d . . .
H5 H -0.1209 0.7649 0.0590 0.035 Uiso 1 1 calc R . .
C6 C -0.13712(18) 0.75064(17) -0.04336(13) 0.0258(5) Uani 1 1 d . . .
C7 C 0.12131(18) 0.59506(16) 0.00711(12) 0.0235(4) Uani 1 1 d . . .
H7 H 0.1310 0.5335 -0.0133 0.028 Uiso 1 1 calc R . .
C8 C 0.10771(18) 0.58038(16) 0.07673(13) 0.0238(4) Uani 1 1 d . . .
H8 H 0.0899 0.5123 0.0808 0.029 Uiso 1 1 calc R . .
C9 C 0.22223(19) 0.61211(17) 0.14957(12) 0.0254(5) Uani 1 1 d . . .
C10 C 0.27562(18) 0.67537(16) 0.11662(12) 0.0230(4) Uani 1 1 d . . .
C11 C 0.36438(18) 0.74180(17) 0.15542(12) 0.0247(5) Uani 1 1 d . . .
H11 H 0.3974 0.7547 0.2085 0.030 Uiso 1 1 calc R . .
C12 C 0.40319(18) 0.78871(16) 0.11377(12) 0.0223(4) Uani 1 1 d . . .
C13 C 0.48581(18) 0.87159(16) 0.14004(13) 0.0248(5) Uani 1 1 d . . .
H13 H 0.5660 0.8541 0.1829 0.030 Uiso 1 1 calc R . .
C14 C 0.48127(19) 0.90304(16) 0.06593(13) 0.0251(5) Uani 1 1 d . . .
H14 H 0.5605 0.9181 0.0773 0.030 Uiso 1 1 calc R . .
C15 C 0.4246(2) 0.82045(17) 0.00719(13) 0.0260(5) Uani 1 1 d . . .
C16 C 0.35914(18) 0.76715(16) 0.03667(12) 0.0227(4) Uani 1 1 d . . .
C17 C 0.26842(18) 0.70195(16) -0.00267(12) 0.0234(4) Uani 1 1 d . . .
H17 H 0.2368 0.6874 -0.0553 0.028 Uiso 1 1 calc R . .
C18 C 0.22618(17) 0.65913(16) 0.03832(12) 0.0222(4) Uani 1 1 d . . .
C19 C 0.2987(2) 0.5232(2) 0.18585(17) 0.0410(6) Uani 1 1 d . . .
H19A H 0.3035 0.4883 0.1465 0.061 Uiso 1 1 calc R . .
H19B H 0.2646 0.4820 0.2070 0.061 Uiso 1 1 calc R . .
H19C H 0.3767 0.5427 0.2272 0.061 Uiso 1 1 calc R . .
C20 C 0.2050(2) 0.6634(2) 0.20809(16) 0.0409(6) Uani 1 1 d . . .
H20A H 0.2808 0.6798 0.2536 0.061 Uiso 1 1 calc R . .
H20B H 0.1631 0.6215 0.2232 0.061 Uiso 1 1 calc R . .
H20C H 0.1599 0.7217 0.1850 0.061 Uiso 1 1 calc R . .
C21 C 0.5221(2) 0.75551(19) 0.01651(15) 0.0347(6) Uani 1 1 d . . .
H21A H 0.5747 0.7391 0.0709 0.052 Uiso 1 1 calc R . .
H21B H 0.5656 0.7889 -0.0019 0.052 Uiso 1 1 calc R . .
H21C H 0.4883 0.6971 -0.0135 0.052 Uiso 1 1 calc R . .
C22 C 0.3484(2) 0.8551(2) -0.07612(14) 0.0364(6) Uani 1 1 d . . .
H22A H 0.3175 0.8000 -0.1107 0.055 Uiso 1 1 calc R . .
H22B H 0.3949 0.8944 -0.0890 0.055 Uiso 1 1 calc R . .
H22C H 0.2839 0.8930 -0.0819 0.055 Uiso 1 1 calc R . .
B1 B -0.0353(2) 0.67786(19) -0.01259(15) 0.0250(5) Uani 1 1 d . . .
B2 B 0.3876(2) 1.01074(19) 0.09719(15) 0.0257(5) Uani 1 1 d . . .
N1 N -0.19561(18) 0.76010(16) -0.17933(11) 0.0329(5) Uani 1 1 d . . .
N2 N -0.34112(19) 0.89013(16) -0.21421(12) 0.0338(5) Uani 1 1 d . . .
O1 O 0.01671(13) 0.64669(11) -0.04995(8) 0.0245(3) Uani 1 1 d . . .
O2 O 0.01216(14) 0.64137(13) 0.05973(9) 0.0302(4) Uani 1 1 d . . .
O3 O 0.43877(13) 0.95189(11) 0.15970(9) 0.0260(3) Uani 1 1 d . . .
O4 O 0.40866(14) 0.98698(12) 0.04134(9) 0.0285(4) Uani 1 1 d . . .
S1 S -0.28656(6) 0.82520(5) -0.25198(4) 0.03973(18) Uani 1 1 d . . .
C31 C 0.0404(2) 0.96989(19) 0.03371(16) 0.0489(7) Uani 0.50 1 d PGU A -1
C32 C 0.0981(3) 0.9062(2) 0.0140(2) 0.0489(7) Uani 0.50 1 d PGU A -1
H32 H 0.1550 0.8644 0.0518 0.059 Uiso 0.50 1 calc PR A -1
C33 C 0.0725(4) 0.9035(3) -0.0609(3) 0.0489(7) Uani 0.50 1 d PGU A -1
H33 H 0.1119 0.8599 -0.0744 0.059 Uiso 0.50 1 calc PR A -1
C34 C -0.0108(4) 0.9645(3) -0.1162(2) 0.0489(7) Uani 0.50 1 d PGU A -1
H34 H -0.0283 0.9626 -0.1674 0.059 Uiso 0.50 1 calc PR A -1
C35 C -0.0685(4) 1.0282(3) -0.09649(15) 0.0489(7) Uani 0.50 1 d PGU A -1
H35 H -0.1255 1.0699 -0.1343 0.059 Uiso 0.50 1 calc PR A -1
C36 C -0.0429(3) 1.0309(2) -0.02155(15) 0.0489(7) Uani 0.50 1 d PGU A -1
S2 S 0.0518(3) 0.9869(2) 0.11812(14) 0.1011(9) Uani 0.50 1 d PGU A -1
C37 C -0.1014(3) 1.1004(2) 0.0101(2) 0.0250(10) Uani 0.50 1 d PGU A -1
H37 H -0.1592 1.1483 -0.0151 0.030 Uiso 0.50 1 calc PR A -1
C38 C -0.0409(7) 1.0685(7) 0.0865(5) 0.063(2) Uani 0.50 1 d PU A -1
H38 H -0.0570 1.0982 0.1211 0.075 Uiso 0.50 1 calc PR A -1
C23 C 0.0450(2) 0.3692(2) 0.22344(16) 0.0428(7) Uani 1 1 d . . .
H23 H 0.0600 0.3450 0.1840 0.051 Uiso 1 1 calc R B 1
Cl1A Cl 0.1797(8) 0.3902(8) 0.3096(4) 0.0657(14) Uani 0.72(3) 1 d P C 1
Cl2A Cl -0.0386(5) 0.4749(3) 0.1880(3) 0.0604(10) Uani 0.72(3) 1 d P C 1
Cl3A Cl -0.0333(5) 0.2825(4) 0.2380(3) 0.0676(11) Uani 0.72(3) 1 d P C 1
Cl1B Cl 0.1746(19) 0.4066(15) 0.3056(11) 0.053(3) Uani 0.28(3) 1 d P C 2
Cl2B Cl -0.0541(19) 0.458(2) 0.1937(11) 0.098(4) Uani 0.28(3) 1 d P C 2
Cl3B Cl -0.004(3) 0.266(2) 0.2462(15) 0.105(5) Uani 0.28(3) 1 d P C 2
C24 C 0.5441(2) 0.43493(19) 0.16798(15) 0.0344(5) Uani 1 1 d . . .
H24 H 0.5536 0.4640 0.2153 0.041 Uiso 1 1 calc R . .
Cl4 Cl 0.68140(7) 0.39985(6) 0.18847(5) 0.0574(2) Uani 1 1 d . . .
Cl5 Cl 0.48325(8) 0.52029(6) 0.09450(5) 0.0556(2) Uani 1 1 d . . .
Cl6 Cl 0.45207(6) 0.33456(5) 0.14201(4) 0.04493(18) 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 1.346(3) . ?
C1 C6 1.432(3) . ?
C1 C2 1.440(3) . ?
C2 N2 1.355(3) . ?
C2 C3 1.426(3) . ?
C3 C4 1.376(3) . ?
C3 B2 1.563(3) 3_575 ?
C4 C5 1.421(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.378(3) . ?
C5 H5 0.9500 . ?
C6 B1 1.559(3) . ?
C7 O1 1.464(3) . ?
C7 C18 1.511(3) . ?
C7 C8 1.558(3) . ?
C7 H7 1.0000 . ?
C8 O2 1.438(3) . ?
C8 C9 1.541(3) . ?
C8 H8 1.0000 . ?
C9 C10 1.522(3) . ?
C9 C20 1.529(3) . ?
C9 C19 1.538(3) . ?
C10 C11 1.391(3) . ?
C10 C18 1.394(3) . ?
C11 C12 1.394(3) . ?
C11 H11 0.9500 . ?
C12 C16 1.398(3) . ?
C12 C13 1.504(3) . ?
C13 O3 1.459(3) . ?
C13 C14 1.560(3) . ?
C13 H13 1.0000 . ?
C14 O4 1.445(3) . ?
C14 C15 1.549(3) . ?
C14 H14 1.0000 . ?
C15 C16 1.521(3) . ?
C15 C22 1.532(3) . ?
C15 C21 1.539(3) . ?
C16 C17 1.396(3) . ?
C17 C18 1.391(3) . ?
C17 H17 0.9500 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
B1 O2 1.366(3) . ?
B1 O1 1.371(3) . ?
B2 O3 1.365(3) . ?
B2 O4 1.371(3) . ?
B2 C3 1.563(3) 3_575 ?
N1 S1 1.619(2) . ?
N2 S1 1.618(2) . ?
C31 C32 1.3900 . ?
C31 C36 1.3900 . ?
C31 S2 1.6798 . ?
C32 C33 1.3900 . ?
C32 H32 0.9500 . ?
C33 C34 1.3900 . ?
C33 H33 0.9500 . ?
C34 C35 1.3900 . ?
C34 H34 0.9500 . ?
C35 C36 1.3900 . ?
C35 H35 0.9500 . ?
C36 C37 1.6061 . ?
S2 C38 1.566(9) . ?
C37 C38 1.401(10) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
C23 Cl2B 1.699(17) . ?
C23 Cl1B 1.748(19) . ?
C23 Cl3A 1.749(6) . ?
C23 Cl3B 1.76(2) . ?
C23 Cl1A 1.764(8) . ?
C23 Cl2A 1.773(5) . ?
C23 H23 1.0000 . ?
C24 Cl5 1.751(3) . ?
C24 Cl4 1.758(3) . ?
C24 Cl6 1.768(3) . ?
C24 H24 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 C6 125.7(2) . . ?
N1 C1 C2 113.4(2) . . ?
C6 C1 C2 121.0(2) . . ?
N2 C2 C3 125.4(2) . . ?
N2 C2 C1 113.0(2) . . ?
C3 C2 C1 121.6(2) . . ?
C4 C3 C2 115.6(2) . . ?
C4 C3 B2 118.3(2) . 3_575 ?
C2 C3 B2 125.9(2) . 3_575 ?
C3 C4 C5 123.0(2) . . ?
C3 C4 H4 118.5 . . ?
C5 C4 H4 118.5 . . ?
C6 C5 C4 123.1(2) . . ?
C6 C5 H5 118.4 . . ?
C4 C5 H5 118.4 . . ?
C5 C6 C1 115.6(2) . . ?
C5 C6 B1 118.3(2) . . ?
C1 C6 B1 125.9(2) . . ?
O1 C7 C18 109.88(17) . . ?
O1 C7 C8 104.90(16) . . ?
C18 C7 C8 104.03(17) . . ?
O1 C7 H7 112.5 . . ?
C18 C7 H7 112.5 . . ?
C8 C7 H7 112.5 . . ?
O2 C8 C9 112.24(18) . . ?
O2 C8 C7 103.88(17) . . ?
C9 C8 C7 107.34(17) . . ?
O2 C8 H8 111.0 . . ?
C9 C8 H8 111.0 . . ?
C7 C8 H8 111.0 . . ?
C10 C9 C20 113.2(2) . . ?
C10 C9 C19 109.06(18) . . ?
C20 C9 C19 110.5(2) . . ?
C10 C9 C8 102.27(17) . . ?
C20 C9 C8 113.47(19) . . ?
C19 C9 C8 107.9(2) . . ?
C11 C10 C18 120.3(2) . . ?
C11 C10 C9 127.8(2) . . ?
C18 C10 C9 111.87(19) . . ?
C10 C11 C12 117.70(19) . . ?
C10 C11 H11 121.1 . . ?
C12 C11 H11 121.1 . . ?
C11 C12 C16 121.7(2) . . ?
C11 C12 C13 127.1(2) . . ?
C16 C12 C13 110.93(19) . . ?
O3 C13 C12 109.84(17) . . ?
O3 C13 C14 105.26(17) . . ?
C12 C13 C14 103.86(17) . . ?
O3 C13 H13 112.4 . . ?
C12 C13 H13 112.4 . . ?
C14 C13 H13 112.4 . . ?
O4 C14 C15 112.03(18) . . ?
O4 C14 C13 103.41(17) . . ?
C15 C14 C13 107.11(17) . . ?
O4 C14 H14 111.3 . . ?
C15 C14 H14 111.3 . . ?
C13 C14 H14 111.3 . . ?
C16 C15 C22 114.41(19) . . ?
C16 C15 C21 108.38(19) . . ?
C22 C15 C21 110.4(2) . . ?
C16 C15 C14 102.07(17) . . ?
C22 C15 C14 113.1(2) . . ?
C21 C15 C14 108.06(18) . . ?
C17 C16 C12 120.5(2) . . ?
C17 C16 C15 128.2(2) . . ?
C12 C16 C15 111.28(19) . . ?
C18 C17 C16 117.3(2) . . ?
C18 C17 H17 121.3 . . ?
C16 C17 H17 121.3 . . ?
C17 C18 C10 122.2(2) . . ?
C17 C18 C7 127.36(19) . . ?
C10 C18 C7 110.36(19) . . ?
C9 C19 H19A 109.5 . . ?
C9 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C9 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C9 C20 H20A 109.5 . . ?
C9 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C9 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C15 C21 H21A 109.5 . . ?
C15 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C15 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C15 C22 H22A 109.5 . . ?
C15 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C15 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O2 B1 O1 114.2(2) . . ?
O2 B1 C6 119.0(2) . . ?
O1 B1 C6 126.8(2) . . ?
O3 B2 O4 114.5(2) . . ?
O3 B2 C3 126.1(2) . 3_575 ?
O4 B2 C3 119.4(2) . 3_575 ?
C1 N1 S1 106.27(17) . . ?
C2 N2 S1 106.12(17) . . ?
B1 O1 C7 106.45(17) . . ?
B1 O2 C8 108.92(18) . . ?
B2 O3 C13 106.44(18) . . ?
B2 O4 C14 108.58(18) . . ?
N2 S1 N1 101.25(11) . . ?
C32 C31 C36 120.0 . . ?
C32 C31 S2 130.1 . . ?
C36 C31 S2 109.9 . . ?
C31 C32 C33 120.0 . . ?
C31 C32 H32 120.0 . . ?
C33 C32 H32 120.0 . . ?
C32 C33 C34 120.0 . . ?
C32 C33 H33 120.0 . . ?
C34 C33 H33 120.0 . . ?
C35 C34 C33 120.0 . . ?
C35 C34 H34 120.0 . . ?
C33 C34 H34 120.0 . . ?
C36 C35 C34 120.0 . . ?
C36 C35 H35 120.0 . . ?
C34 C35 H35 120.0 . . ?
C35 C36 C31 120.0 . . ?
C35 C36 C37 125.9 . . ?
C31 C36 C37 114.1 . . ?
C38 S2 C31 94.0(3) . . ?
C38 C37 C36 98.1(3) . . ?
C38 C37 H37 130.9 . . ?
C36 C37 H37 130.9 . . ?
C37 C38 S2 123.9(5) . . ?
C37 C38 H38 118.1 . . ?
S2 C38 H38 118.1 . . ?
Cl2B C23 Cl1B 108.9(10) . . ?
Cl2B C23 Cl3A 97.5(13) . . ?
Cl1B C23 Cl3A 115.9(6) . . ?
Cl2B C23 Cl3B 111.2(7) . . ?
Cl1B C23 Cl3B 108.6(10) . . ?
Cl3A C23 Cl3B 13.7(14) . . ?
Cl2B C23 Cl1A 116.0(7) . . ?
Cl1B C23 Cl1A 7.9(10) . . ?
Cl3A C23 Cl1A 110.3(4) . . ?
Cl3B C23 Cl1A 102.0(9) . . ?
Cl2B C23 Cl2A 12.1(13) . . ?
Cl1B C23 Cl2A 103.9(8) . . ?
Cl3A C23 Cl2A 109.5(3) . . ?
Cl3B C23 Cl2A 123.2(14) . . ?
Cl1A C23 Cl2A 111.6(4) . . ?
Cl2B C23 H23 115.4 . . ?
Cl1B C23 H23 110.3 . . ?
Cl3A C23 H23 108.5 . . ?
Cl3B C23 H23 102.1 . . ?
Cl1A C23 H23 108.5 . . ?
Cl2A C23 H23 108.5 . . ?
Cl5 C24 Cl4 110.33(15) . . ?
Cl5 C24 Cl6 110.70(14) . . ?
Cl4 C24 Cl6 110.07(15) . . ?
Cl5 C24 H24 108.6 . . ?
Cl4 C24 H24 108.6 . . ?
Cl6 C24 H24 108.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 N2 -0.3(3) . . . . ?
C6 C1 C2 N2 -180.0(2) . . . . ?
N1 C1 C2 C3 179.8(2) . . . . ?
C6 C1 C2 C3 0.1(3) . . . . ?
N2 C2 C3 C4 179.1(2) . . . . ?
C1 C2 C3 C4 -1.0(3) . . . . ?
N2 C2 C3 B2 -5.8(4) . . . 3_575 ?
C1 C2 C3 B2 174.1(2) . . . 3_575 ?
C2 C3 C4 C5 0.7(3) . . . . ?
B2 C3 C4 C5 -174.9(2) 3_575 . . . ?
C3 C4 C5 C6 0.7(4) . . . . ?
C4 C5 C6 C1 -1.6(3) . . . . ?
C4 C5 C6 B1 173.2(2) . . . . ?
N1 C1 C6 C5 -178.5(2) . . . . ?
C2 C1 C6 C5 1.2(3) . . . . ?
N1 C1 C6 B1 7.2(4) . . . . ?
C2 C1 C6 B1 -173.2(2) . . . . ?
O1 C7 C8 O2 -11.9(2) . . . . ?
C18 C7 C8 O2 103.54(19) . . . . ?
O1 C7 C8 C9 -130.93(18) . . . . ?
C18 C7 C8 C9 -15.5(2) . . . . ?
O2 C8 C9 C10 -93.5(2) . . . . ?
C7 C8 C9 C10 20.1(2) . . . . ?
O2 C8 C9 C20 28.8(3) . . . . ?
C7 C8 C9 C20 142.3(2) . . . . ?
O2 C8 C9 C19 151.61(19) . . . . ?
C7 C8 C9 C19 -94.9(2) . . . . ?
C20 C9 C10 C11 40.4(3) . . . . ?
C19 C9 C10 C11 -83.0(3) . . . . ?
C8 C9 C10 C11 162.9(2) . . . . ?
C20 C9 C10 C18 -140.8(2) . . . . ?
C19 C9 C10 C18 95.8(2) . . . . ?
C8 C9 C10 C18 -18.3(2) . . . . ?
C18 C10 C11 C12 -1.7(3) . . . . ?
C9 C10 C11 C12 177.0(2) . . . . ?
C10 C11 C12 C16 -3.0(3) . . . . ?
C10 C11 C12 C13 171.3(2) . . . . ?
C11 C12 C13 O3 -59.3(3) . . . . ?
C16 C12 C13 O3 115.5(2) . . . . ?
C11 C12 C13 C14 -171.5(2) . . . . ?
C16 C12 C13 C14 3.3(2) . . . . ?
O3 C13 C14 O4 -12.8(2) . . . . ?
C12 C13 C14 O4 102.69(18) . . . . ?
O3 C13 C14 C15 -131.24(17) . . . . ?
C12 C13 C14 C15 -15.8(2) . . . . ?
O4 C14 C15 C16 -91.4(2) . . . . ?
C13 C14 C15 C16 21.3(2) . . . . ?
O4 C14 C15 C22 32.0(3) . . . . ?
C13 C14 C15 C22 144.74(19) . . . . ?
O4 C14 C15 C21 154.47(18) . . . . ?
C13 C14 C15 C21 -92.8(2) . . . . ?
C11 C12 C16 C17 4.5(3) . . . . ?
C13 C12 C16 C17 -170.7(2) . . . . ?
C11 C12 C16 C15 -173.9(2) . . . . ?
C13 C12 C16 C15 10.9(3) . . . . ?
C22 C15 C16 C17 39.1(3) . . . . ?
C21 C15 C16 C17 -84.5(3) . . . . ?
C14 C15 C16 C17 161.6(2) . . . . ?
C22 C15 C16 C12 -142.6(2) . . . . ?
C21 C15 C16 C12 93.8(2) . . . . ?
C14 C15 C16 C12 -20.1(2) . . . . ?
C12 C16 C17 C18 -1.0(3) . . . . ?
C15 C16 C17 C18 177.1(2) . . . . ?
C16 C17 C18 C10 -3.7(3) . . . . ?
C16 C17 C18 C7 172.9(2) . . . . ?
C11 C10 C18 C17 5.2(3) . . . . ?
C9 C10 C18 C17 -173.7(2) . . . . ?
C11 C10 C18 C7 -172.0(2) . . . . ?
C9 C10 C18 C7 9.1(3) . . . . ?
O1 C7 C18 C17 -60.9(3) . . . . ?
C8 C7 C18 C17 -172.7(2) . . . . ?
O1 C7 C18 C10 116.0(2) . . . . ?
C8 C7 C18 C10 4.2(2) . . . . ?
C5 C6 B1 O2 12.0(3) . . . . ?
C1 C6 B1 O2 -173.8(2) . . . . ?
C5 C6 B1 O1 -166.0(2) . . . . ?
C1 C6 B1 O1 8.2(4) . . . . ?
C6 C1 N1 S1 -179.51(19) . . . . ?
C2 C1 N1 S1 0.8(2) . . . . ?
C3 C2 N2 S1 179.51(19) . . . . ?
C1 C2 N2 S1 -0.4(2) . . . . ?
O2 B1 O1 C7 -9.3(3) . . . . ?
C6 B1 O1 C7 168.8(2) . . . . ?
C18 C7 O1 B1 -98.6(2) . . . . ?
C8 C7 O1 B1 12.7(2) . . . . ?
O1 B1 O2 C8 1.3(3) . . . . ?
C6 B1 O2 C8 -176.99(19) . . . . ?
C9 C8 O2 B1 122.4(2) . . . . ?
C7 C8 O2 B1 6.8(2) . . . . ?
O4 B2 O3 C13 -9.0(3) . . . . ?
C3 B2 O3 C13 169.3(2) 3_575 . . . ?
C12 C13 O3 B2 -98.1(2) . . . . ?
C14 C13 O3 B2 13.1(2) . . . . ?
O3 B2 O4 C14 0.3(3) . . . . ?
C3 B2 O4 C14 -178.08(19) 3_575 . . . ?
C15 C14 O4 B2 122.9(2) . . . . ?
C13 C14 O4 B2 7.8(2) . . . . ?
C2 N2 S1 N1 0.79(19) . . . . ?
C1 N1 S1 N2 -0.93(19) . . . . ?
C36 C31 C32 C33 0.0 . . . . ?
S2 C31 C32 C33 178.7 . . . . ?
C31 C32 C33 C34 0.0 . . . . ?
C32 C33 C34 C35 0.0 . . . . ?
C33 C34 C35 C36 0.0 . . . . ?
C34 C35 C36 C31 0.0 . . . . ?
C34 C35 C36 C37 179.8 . . . . ?
C32 C31 C36 C35 0.0 . . . . ?
S2 C31 C36 C35 -178.9 . . . . ?
C32 C31 C36 C37 -179.8 . . . . ?
S2 C31 C36 C37 1.3 . . . . ?
C32 C31 S2 C38 179.8(3) . . . . ?
C36 C31 S2 C38 -1.4(3) . . . . ?
C35 C36 C37 C38 179.7(3) . . . . ?
C31 C36 C37 C38 -0.5(3) . . . . ?
C36 C37 C38 S2 -0.6(7) . . . . ?
C31 S2 C38 C37 1.3(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.41
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.797
_refine_diff_density_min         -0.957
_refine_diff_density_rms         0.077
####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1005499'
_audit_update_record             
;
2014-05-27 deposited with the CCDC.
2016-06-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H40 B4 N4 O8 S2, C8 H6 O, 4(C H Cl3)'
_chemical_formula_sum            'C56 H50 B4 Cl12 N4 O9 S2'
_chemical_formula_weight         1455.76

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'
B B 0.0013 0.0007 '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                   13.6823(12)
_cell_length_b                   14.0543(13)
_cell_length_c                   20.5851(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 122.711(4)
_cell_angle_gamma                90.00
_cell_volume                     3330.6(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    26490
_cell_measurement_theta_min      3.01
_cell_measurement_theta_max      27.42

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1484
_exptl_absorpt_coefficient_mu    0.617
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7825
_exptl_absorpt_correction_T_max  0.9483
_exptl_absorpt_process_details   'Absorption was corrected by ABSCOR'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode X-ray tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID II IP 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            51293
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         27.42
_reflns_number_total             7581
_reflns_number_gt                6101
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'PROCESS-AUTO (Rigaku, 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0830P)²+1.5851P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7581
_refine_ls_number_parameters     405
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0502
_refine_ls_wR_factor_ref         0.1455
_refine_ls_wR_factor_gt          0.1366
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.004
_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 0.79553(17) 0.71319(14) 0.37991(11) 0.0280(4) Uani 1 1 d . . .
C2 C 0.86083(17) 0.75107(14) 0.45628(11) 0.0276(4) Uani 1 1 d . . .
C3 C 0.83664(18) 0.71286(16) 0.50754(12) 0.0319(4) Uani 1 1 d . . .
H3 H 0.8771 0.7369 0.5588 0.038 Uiso 1 1 calc R . .
C4 C 0.75430(18) 0.63945(16) 0.48762(12) 0.0317(4) Uani 1 1 d . . .
H4 H 0.7422 0.6166 0.5262 0.038 Uiso 1 1 calc R . .
C5 C 0.69112(17) 0.59965(14) 0.41531(12) 0.0274(4) Uani 1 1 d . . .
C6 C 0.71154(17) 0.63845(14) 0.35966(11) 0.0274(4) Uani 1 1 d . . .
C7 C 0.51525(16) 0.37279(14) 0.36010(11) 0.0261(4) Uani 1 1 d . . .
H7 H 0.4350 0.3549 0.3172 0.031 Uiso 1 1 calc R . .
C8 C 0.52037(17) 0.40415(13) 0.43453(11) 0.0261(4) Uani 1 1 d . . .
H8 H 0.4410 0.4184 0.4233 0.031 Uiso 1 1 calc R . .
C9 C 0.57862(17) 0.32226(14) 0.49397(11) 0.0279(4) Uani 1 1 d . . .
C10 C 0.64365(16) 0.26902(13) 0.46407(11) 0.0238(4) Uani 1 1 d . . .
C11 C 0.73415(16) 0.20436(13) 0.50341(11) 0.0250(4) Uani 1 1 d . . .
H11 H 0.7666 0.1905 0.5564 0.030 Uiso 1 1 calc R . .
C12 C 0.77551(15) 0.16065(13) 0.46210(10) 0.0226(4) Uani 1 1 d . . .
C13 C 0.87923(16) 0.09588(13) 0.49304(11) 0.0239(4) Uani 1 1 d . . .
H13 H 0.8689 0.0347 0.5135 0.029 Uiso 1 1 calc R . .
C14 C 0.89218(16) 0.08054(13) 0.42320(11) 0.0249(4) Uani 1 1 d . . .
H14 H 0.9085 0.0123 0.4188 0.030 Uiso 1 1 calc R . .
C15 C 0.77794(17) 0.11361(14) 0.35022(11) 0.0269(4) Uani 1 1 d . . .
C16 C 0.72547(16) 0.17703(13) 0.38341(11) 0.0239(4) Uani 1 1 d . . .
C17 C 0.63687(16) 0.24326(14) 0.34471(11) 0.0255(4) Uani 1 1 d . . .
H17 H 0.6032 0.2560 0.2914 0.031 Uiso 1 1 calc R . .
C18 C 0.59916(16) 0.29020(13) 0.38670(11) 0.0235(4) Uani 1 1 d . . .
C19 C 0.4821(2) 0.25705(16) 0.48565(14) 0.0380(5) Uani 1 1 d . . .
H19A H 0.4282 0.2411 0.4311 0.057 Uiso 1 1 calc R . .
H19B H 0.4399 0.2900 0.5052 0.057 Uiso 1 1 calc R . .
H19C H 0.5167 0.1986 0.5153 0.057 Uiso 1 1 calc R . .
C20 C 0.6557(2) 0.35727(18) 0.57686(13) 0.0407(5) Uani 1 1 d . . .
H20A H 0.6913 0.3026 0.6115 0.061 Uiso 1 1 calc R . .
H20B H 0.6087 0.3932 0.5912 0.061 Uiso 1 1 calc R . .
H20C H 0.7168 0.3985 0.5812 0.061 Uiso 1 1 calc R . .
C21 C 0.7004(2) 0.02566(18) 0.31338(15) 0.0440(6) Uani 1 1 d . . .
H21A H 0.6959 -0.0095 0.3528 0.066 Uiso 1 1 calc R . .
H21B H 0.7335 -0.0154 0.2916 0.066 Uiso 1 1 calc R . .
H21C H 0.6223 0.0458 0.2723 0.066 Uiso 1 1 calc R . .
C22 C 0.7964(2) 0.16455(19) 0.29234(14) 0.0427(5) Uani 1 1 d . . .
H22A H 0.7210 0.1818 0.2466 0.064 Uiso 1 1 calc R . .
H22B H 0.8377 0.1223 0.2771 0.064 Uiso 1 1 calc R . .
H22C H 0.8425 0.2222 0.3160 0.064 Uiso 1 1 calc R . .
B1 B 0.61183(18) 0.51261(15) 0.40251(13) 0.0257(4) Uani 1 1 d . . .
B2 B 1.03693(19) 0.17679(16) 0.51300(13) 0.0262(4) Uani 1 1 d . . .
N1 N 0.80304(17) 0.74136(14) 0.32004(10) 0.0356(4) Uani 1 1 d . . .
N2 N 0.65777(17) 0.61130(13) 0.28514(11) 0.0361(4) Uani 1 1 d . . .
O1 O 0.56164(12) 0.45290(10) 0.34013(8) 0.0273(3) Uani 1 1 d . . .
O2 O 0.59147(13) 0.48833(10) 0.45861(8) 0.0302(3) Uani 1 1 d . . .
O3 O 0.98892(12) 0.14012(11) 0.44042(8) 0.0315(3) Uani 1 1 d . . .
O4 O 0.98471(11) 0.14675(9) 0.55041(7) 0.0255(3) Uani 1 1 d . . .
S1 S 0.71225(6) 0.67614(4) 0.24738(3) 0.04330(17) Uani 1 1 d . . .
C201 C 1.0264(7) 0.4772(5) 0.6163(3) 0.0812(8) Uani 0.50 1 d PG A -1
H201 H 1.0486 0.4778 0.6687 0.097 Uiso 0.50 1 calc PR A -1
C202 C 0.9424(6) 0.4136(5) 0.5645(4) 0.0812(8) Uani 0.50 1 d PG A -1
H202 H 0.9072 0.3707 0.5816 0.097 Uiso 0.50 1 calc PR A -1
C203 C 0.9098(5) 0.4128(4) 0.4878(4) 0.0812(8) Uani 0.50 1 d PG A -1
H203 H 0.8524 0.3693 0.4525 0.097 Uiso 0.50 1 calc PR A -1
C204 C 0.9613(7) 0.4756(5) 0.4628(3) 0.0812(8) Uani 0.50 1 d PG A -1
C205 C 1.0453(6) 0.5393(5) 0.5146(4) 0.0812(8) Uani 0.50 1 d PG A -1
C206 C 1.0779(5) 0.5401(4) 0.5913(3) 0.0812(8) Uani 0.50 1 d PG A -1
H206 H 1.1353 0.5836 0.6266 0.097 Uiso 0.50 1 calc PR A -1
C207 C 0.9485(8) 0.4846(7) 0.3921(6) 0.0812(8) Uani 0.50 1 d P A -1
H207 H 0.8991 0.4504 0.3457 0.097 Uiso 0.50 1 calc PR A -1
C208 C 1.0215(9) 0.5521(7) 0.4052(6) 0.0812(8) Uani 0.50 1 d P A -1
H208 H 1.0307 0.5749 0.3653 0.097 Uiso 0.50 1 calc PR A -1
O201 O 1.0873(5) 0.5910(4) 0.4806(4) 0.0812(8) Uani 0.50 1 d P A -1
C23 C 0.0460(2) 0.3698(2) 0.22405(14) 0.0450(6) Uani 1 1 d . . .
H23 H 0.0612 0.3451 0.1848 0.054 Uiso 1 1 calc R B 1
Cl1A Cl 0.1781(7) 0.4021(6) 0.3072(4) 0.0602(13) Uani 0.66(3) 1 d P C 1
Cl2A Cl -0.0381(4) 0.4758(2) 0.1881(2) 0.0618(9) Uani 0.66(3) 1 d P C 1
Cl3A Cl -0.0318(4) 0.2847(4) 0.2396(3) 0.0692(11) Uani 0.66(3) 1 d P C 1
Cl1B Cl 0.1835(15) 0.3815(17) 0.3129(9) 0.067(3) Uani 0.34(3) 1 d P C 2
Cl2B Cl -0.0498(11) 0.4594(15) 0.1965(8) 0.100(3) Uani 0.34(3) 1 d P C 2
Cl3B Cl -0.005(2) 0.2641(16) 0.2440(9) 0.106(4) Uani 0.34(3) 1 d P C 2
C24 C 0.54373(19) 0.43647(16) 0.16782(13) 0.0350(5) Uani 1 1 d . . .
H24 H 0.5529 0.4654 0.2152 0.042 Uiso 1 1 calc R . .
Cl4A Cl 0.68137(6) 0.40160(5) 0.18914(5) 0.0607(2) Uani 1 1 d . . .
Cl5A Cl 0.48349(7) 0.52184(5) 0.09422(4) 0.05737(19) Uani 1 1 d . . .
Cl6A Cl 0.45191(6) 0.33661(4) 0.14152(4) 0.04592(16) 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 1.350(3) . ?
C1 C2 1.427(3) . ?
C1 C6 1.442(3) . ?
C2 C3 1.374(3) . ?
C2 B2 1.558(3) 3_766 ?
C3 C4 1.415(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.373(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.426(3) . ?
C5 B1 1.560(3) . ?
C6 N2 1.349(3) . ?
C7 O1 1.456(2) . ?
C7 C18 1.512(3) . ?
C7 C8 1.559(3) . ?
C7 H7 1.0000 . ?
C8 O2 1.439(2) . ?
C8 C9 1.550(3) . ?
C8 H8 1.0000 . ?
C9 C20 1.523(3) . ?
C9 C10 1.524(3) . ?
C9 C19 1.539(3) . ?
C10 C11 1.390(3) . ?
C10 C18 1.395(3) . ?
C11 C12 1.393(3) . ?
C11 H11 0.9500 . ?
C12 C16 1.395(3) . ?
C12 C13 1.507(2) . ?
C13 O4 1.465(2) . ?
C13 C14 1.556(3) . ?
C13 H13 1.0000 . ?
C14 O3 1.439(2) . ?
C14 C15 1.542(3) . ?
C14 H14 1.0000 . ?
C15 C16 1.519(3) . ?
C15 C22 1.524(3) . ?
C15 C21 1.536(3) . ?
C16 C17 1.388(3) . ?
C17 C18 1.390(3) . ?
C17 H17 0.9500 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
B1 O1 1.368(3) . ?
B1 O2 1.369(3) . ?
B2 O3 1.367(3) . ?
B2 O4 1.370(3) . ?
B2 C2 1.558(3) 3_766 ?
N1 S1 1.6164(19) . ?
N2 S1 1.6174(19) . ?
C201 C202 1.3900 . ?
C201 C206 1.3900 . ?
C201 H201 0.9500 . ?
C202 C203 1.3900 . ?
C202 H202 0.9500 . ?
C203 C204 1.3900 . ?
C203 H203 0.9500 . ?
C204 C207 1.376(10) . ?
C204 C205 1.3900 . ?
C205 O201 1.335(7) . ?
C205 C206 1.3900 . ?
C206 H206 0.9500 . ?
C207 C208 1.295(14) . ?
C207 H207 0.9500 . ?
C208 O201 1.417(12) . ?
C208 H208 0.9500 . ?
C23 Cl2B 1.680(12) . ?
C23 Cl3A 1.742(5) . ?
C23 Cl1A 1.748(8) . ?
C23 Cl3B 1.780(15) . ?
C23 Cl2A 1.781(5) . ?
C23 Cl1B 1.787(16) . ?
C23 H23 1.0000 . ?
C24 Cl5A 1.751(2) . ?
C24 Cl4A 1.757(2) . ?
C24 Cl6A 1.762(2) . ?
C24 H24 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 125.81(19) . . ?
N1 C1 C6 113.05(18) . . ?
C2 C1 C6 121.14(18) . . ?
C3 C2 C1 115.66(18) . . ?
C3 C2 B2 118.59(18) . 3_766 ?
C1 C2 B2 125.47(18) . 3_766 ?
C2 C3 C4 123.14(19) . . ?
C2 C3 H3 118.4 . . ?
C4 C3 H3 118.4 . . ?
C5 C4 C3 123.20(19) . . ?
C5 C4 H4 118.4 . . ?
C3 C4 H4 118.4 . . ?
C4 C5 C6 115.67(18) . . ?
C4 C5 B1 118.40(18) . . ?
C6 C5 B1 125.76(18) . . ?
N2 C6 C5 125.59(18) . . ?
N2 C6 C1 113.23(18) . . ?
C5 C6 C1 121.17(18) . . ?
O1 C7 C18 109.54(15) . . ?
O1 C7 C8 105.30(15) . . ?
C18 C7 C8 103.82(15) . . ?
O1 C7 H7 112.5 . . ?
C18 C7 H7 112.5 . . ?
C8 C7 H7 112.5 . . ?
O2 C8 C9 112.02(16) . . ?
O2 C8 C7 103.52(15) . . ?
C9 C8 C7 107.26(15) . . ?
O2 C8 H8 111.2 . . ?
C9 C8 H8 111.2 . . ?
C7 C8 H8 111.2 . . ?
C20 C9 C10 114.13(17) . . ?
C20 C9 C19 110.50(18) . . ?
C10 C9 C19 108.41(16) . . ?
C20 C9 C8 113.19(17) . . ?
C10 C9 C8 102.07(15) . . ?
C19 C9 C8 108.06(17) . . ?
C11 C10 C18 120.42(17) . . ?
C11 C10 C9 128.06(17) . . ?
C18 C10 C9 111.50(16) . . ?
C10 C11 C12 117.43(17) . . ?
C10 C11 H11 121.3 . . ?
C12 C11 H11 121.3 . . ?
C11 C12 C16 121.97(17) . . ?
C11 C12 C13 127.50(17) . . ?
C16 C12 C13 110.45(16) . . ?
O4 C13 C12 109.77(14) . . ?
O4 C13 C14 104.95(14) . . ?
C12 C13 C14 104.17(15) . . ?
O4 C13 H13 112.5 . . ?
C12 C13 H13 112.5 . . ?
C14 C13 H13 112.5 . . ?
O3 C14 C15 112.19(16) . . ?
O3 C14 C13 103.93(14) . . ?
C15 C14 C13 107.26(15) . . ?
O3 C14 H14 111.1 . . ?
C15 C14 H14 111.1 . . ?
C13 C14 H14 111.1 . . ?
C16 C15 C22 113.24(17) . . ?
C16 C15 C21 109.02(16) . . ?
C22 C15 C21 110.76(19) . . ?
C16 C15 C14 102.44(15) . . ?
C22 C15 C14 113.21(17) . . ?
C21 C15 C14 107.73(17) . . ?
C17 C16 C12 120.36(17) . . ?
C17 C16 C15 127.87(17) . . ?
C12 C16 C15 111.76(16) . . ?
C16 C17 C18 117.65(17) . . ?
C16 C17 H17 121.2 . . ?
C18 C17 H17 121.2 . . ?
C17 C18 C10 121.94(17) . . ?
C17 C18 C7 127.14(17) . . ?
C10 C18 C7 110.78(16) . . ?
C9 C19 H19A 109.5 . . ?
C9 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C9 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C9 C20 H20A 109.5 . . ?
C9 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C9 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C15 C21 H21A 109.5 . . ?
C15 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C15 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C15 C22 H22A 109.5 . . ?
C15 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C15 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O1 B1 O2 114.27(18) . . ?
O1 B1 C5 126.15(18) . . ?
O2 B1 C5 119.52(18) . . ?
O3 B2 O4 114.18(17) . . ?
O3 B2 C2 118.98(18) . 3_766 ?
O4 B2 C2 126.80(18) . 3_766 ?
C1 N1 S1 106.19(14) . . ?
C6 N2 S1 106.10(14) . . ?
B1 O1 C7 106.47(15) . . ?
B1 O2 C8 108.79(15) . . ?
B2 O3 C14 108.86(15) . . ?
B2 O4 C13 106.45(15) . . ?
N1 S1 N2 101.43(10) . . ?
C202 C201 C206 120.0 . . ?
C202 C201 H201 120.0 . . ?
C206 C201 H201 120.0 . . ?
C203 C202 C201 120.0 . . ?
C203 C202 H202 120.0 . . ?
C201 C202 H202 120.0 . . ?
C202 C203 C204 120.0 . . ?
C202 C203 H203 120.0 . . ?
C204 C203 H203 120.0 . . ?
C207 C204 C203 130.6(5) . . ?
C207 C204 C205 109.3(5) . . ?
C203 C204 C205 120.0 . . ?
O201 C205 C206 128.8(5) . . ?
O201 C205 C204 111.1(5) . . ?
C206 C205 C204 120.0 . . ?
C205 C206 C201 120.0 . . ?
C205 C206 H206 120.0 . . ?
C201 C206 H206 120.0 . . ?
C208 C207 C204 101.8(8) . . ?
C208 C207 H207 129.1 . . ?
C204 C207 H207 129.1 . . ?
C207 C208 O201 118.2(9) . . ?
C207 C208 H208 120.9 . . ?
O201 C208 H208 120.9 . . ?
C205 O201 C208 99.5(6) . . ?
Cl2B C23 Cl3A 97.7(8) . . ?
Cl2B C23 Cl1A 109.9(6) . . ?
Cl3A C23 Cl1A 114.2(3) . . ?
Cl2B C23 Cl3B 111.9(4) . . ?
Cl3A C23 Cl3B 14.3(8) . . ?
Cl1A C23 Cl3B 108.4(7) . . ?
Cl2B C23 Cl2A 11.9(9) . . ?
Cl3A C23 Cl2A 109.2(2) . . ?
Cl1A C23 Cl2A 106.5(4) . . ?
Cl3B C23 Cl2A 123.3(9) . . ?
Cl2B C23 Cl1B 118.3(9) . . ?
Cl3A C23 Cl1B 106.6(7) . . ?
Cl1A C23 Cl1B 9.8(9) . . ?
Cl3B C23 Cl1B 99.6(13) . . ?
Cl2A C23 Cl1B 115.8(8) . . ?
Cl2B C23 H23 117.0 . . ?
Cl3A C23 H23 109.0 . . ?
Cl1A C23 H23 109.0 . . ?
Cl3B C23 H23 100.0 . . ?
Cl2A C23 H23 109.0 . . ?
Cl1B C23 H23 107.2 . . ?
Cl5A C24 Cl4A 110.31(13) . . ?
Cl5A C24 Cl6A 110.85(12) . . ?
Cl4A C24 Cl6A 110.16(12) . . ?
Cl5A C24 H24 108.5 . . ?
Cl4A C24 H24 108.5 . . ?
Cl6A C24 H24 108.5 . . ?

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
N1 C1 C2 C3 178.5(2) . . . . ?
C6 C1 C2 C3 -1.0(3) . . . . ?
N1 C1 C2 B2 -7.8(3) . . . 3_766 ?
C6 C1 C2 B2 172.67(18) . . . 3_766 ?
C1 C2 C3 C4 1.1(3) . . . . ?
B2 C2 C3 C4 -173.03(19) 3_766 . . . ?
C2 C3 C4 C5 0.0(3) . . . . ?
C3 C4 C5 C6 -1.3(3) . . . . ?
C3 C4 C5 B1 174.17(19) . . . . ?
C4 C5 C6 N2 -178.8(2) . . . . ?
B1 C5 C6 N2 6.1(3) . . . . ?
C4 C5 C6 C1 1.3(3) . . . . ?
B1 C5 C6 C1 -173.74(18) . . . . ?
N1 C1 C6 N2 0.3(3) . . . . ?
C2 C1 C6 N2 179.92(19) . . . . ?
N1 C1 C6 C5 -179.78(18) . . . . ?
C2 C1 C6 C5 -0.2(3) . . . . ?
O1 C7 C8 O2 -12.20(17) . . . . ?
C18 C7 C8 O2 102.91(16) . . . . ?
O1 C7 C8 C9 -130.79(15) . . . . ?
C18 C7 C8 C9 -15.68(19) . . . . ?
O2 C8 C9 C20 31.2(2) . . . . ?
C7 C8 C9 C20 144.12(17) . . . . ?
O2 C8 C9 C10 -91.95(18) . . . . ?
C7 C8 C9 C10 21.00(19) . . . . ?
O2 C8 C9 C19 153.88(16) . . . . ?
C7 C8 C9 C19 -93.17(18) . . . . ?
C20 C9 C10 C11 39.6(3) . . . . ?
C19 C9 C10 C11 -84.0(2) . . . . ?
C8 C9 C10 C11 162.13(19) . . . . ?
C20 C9 C10 C18 -142.14(19) . . . . ?
C19 C9 C10 C18 94.2(2) . . . . ?
C8 C9 C10 C18 -19.7(2) . . . . ?
C18 C10 C11 C12 -1.6(3) . . . . ?
C9 C10 C11 C12 176.47(18) . . . . ?
C10 C11 C12 C16 -2.9(3) . . . . ?
C10 C11 C12 C13 173.65(18) . . . . ?
C11 C12 C13 O4 -60.7(2) . . . . ?
C16 C12 C13 O4 116.16(17) . . . . ?
C11 C12 C13 C14 -172.66(18) . . . . ?
C16 C12 C13 C14 4.2(2) . . . . ?
O4 C13 C14 O3 -11.58(18) . . . . ?
C12 C13 C14 O3 103.79(16) . . . . ?
O4 C13 C14 C15 -130.57(15) . . . . ?
C12 C13 C14 C15 -15.19(19) . . . . ?
O3 C14 C15 C16 -93.92(17) . . . . ?
C13 C14 C15 C16 19.60(18) . . . . ?
O3 C14 C15 C22 28.4(2) . . . . ?
C13 C14 C15 C22 141.88(17) . . . . ?
O3 C14 C15 C21 151.19(16) . . . . ?
C13 C14 C15 C21 -95.30(18) . . . . ?
C11 C12 C16 C17 4.5(3) . . . . ?
C13 C12 C16 C17 -172.62(17) . . . . ?
C11 C12 C16 C15 -174.13(17) . . . . ?
C13 C12 C16 C15 8.8(2) . . . . ?
C22 C15 C16 C17 41.5(3) . . . . ?
C21 C15 C16 C17 -82.3(2) . . . . ?
C14 C15 C16 C17 163.74(19) . . . . ?
C22 C15 C16 C12 -140.06(18) . . . . ?
C21 C15 C16 C12 96.2(2) . . . . ?
C14 C15 C16 C12 -17.8(2) . . . . ?
C12 C16 C17 C18 -1.4(3) . . . . ?
C15 C16 C17 C18 177.00(18) . . . . ?
C16 C17 C18 C10 -3.2(3) . . . . ?
C16 C17 C18 C7 171.98(18) . . . . ?
C11 C10 C18 C17 4.7(3) . . . . ?
C9 C10 C18 C17 -173.63(17) . . . . ?
C11 C10 C18 C7 -171.13(17) . . . . ?
C9 C10 C18 C7 10.5(2) . . . . ?
O1 C7 C18 C17 -60.0(2) . . . . ?
C8 C7 C18 C17 -172.09(18) . . . . ?
O1 C7 C18 C10 115.58(17) . . . . ?
C8 C7 C18 C10 3.5(2) . . . . ?
C4 C5 B1 O1 -166.12(19) . . . . ?
C6 C5 B1 O1 8.8(3) . . . . ?
C4 C5 B1 O2 11.1(3) . . . . ?
C6 C5 B1 O2 -173.95(18) . . . . ?
C2 C1 N1 S1 179.68(17) . . . . ?
C6 C1 N1 S1 -0.8(2) . . . . ?
C5 C6 N2 S1 -179.61(17) . . . . ?
C1 C6 N2 S1 0.3(2) . . . . ?
O2 B1 O1 C7 -8.2(2) . . . . ?
C5 B1 O1 C7 169.18(18) . . . . ?
C18 C7 O1 B1 -98.81(18) . . . . ?
C8 C7 O1 B1 12.29(18) . . . . ?
O1 B1 O2 C8 -0.2(2) . . . . ?
C5 B1 O2 C8 -177.68(16) . . . . ?
C9 C8 O2 B1 122.98(17) . . . . ?
C7 C8 O2 B1 7.74(19) . . . . ?
O4 B2 O3 C14 1.6(2) . . . . ?
C2 B2 O3 C14 -176.37(16) 3_766 . . . ?
C15 C14 O3 B2 122.01(17) . . . . ?
C13 C14 O3 B2 6.46(19) . . . . ?
O3 B2 O4 C13 -9.4(2) . . . . ?
C2 B2 O4 C13 168.34(18) 3_766 . . . ?
C12 C13 O4 B2 -98.83(17) . . . . ?
C14 C13 O4 B2 12.58(18) . . . . ?
C1 N1 S1 N2 0.84(17) . . . . ?
C6 N2 S1 N1 -0.65(18) . . . . ?
C206 C201 C202 C203 0.0 . . . . ?
C201 C202 C203 C204 0.0 . . . . ?
C202 C203 C204 C207 176.0(9) . . . . ?
C202 C203 C204 C205 0.0 . . . . ?
C207 C204 C205 O201 1.0(6) . . . . ?
C203 C204 C205 O201 177.7(6) . . . . ?
C207 C204 C205 C206 -176.8(7) . . . . ?
C203 C204 C205 C206 0.0 . . . . ?
O201 C205 C206 C201 -177.3(7) . . . . ?
C204 C205 C206 C201 0.0 . . . . ?
C202 C201 C206 C205 0.0 . . . . ?
C203 C204 C207 C208 -177.5(6) . . . . ?
C205 C204 C207 C208 -1.2(7) . . . . ?
C204 C207 C208 O201 1.1(9) . . . . ?
C206 C205 O201 C208 177.2(6) . . . . ?
C204 C205 O201 C208 -0.3(5) . . . . ?
C207 C208 O201 C205 -0.6(8) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.42
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.990
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.076
####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1005500'
_audit_update_record             
;
2014-05-27 deposited with the CCDC.
2016-06-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C57 H51 B4 Cl12 N5 O8 S2'
_chemical_formula_weight         1466.79

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'
B B 0.0013 0.0007 '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           ?
_symmetry_space_group_name_H-M   ?

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                   13.6829(10)
_cell_length_b                   14.0362(10)
_cell_length_c                   20.6735(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 122.667(3)
_cell_angle_gamma                90.00
_cell_volume                     3342.4(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.39
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1496
_exptl_absorpt_coefficient_mu    0.615
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.7494
_exptl_absorpt_correction_T_max  0.7964
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            51895
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_sigmaI/netI    0.0338
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         27.44
_reflns_number_total             7625
_reflns_number_gt                6254
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 
 Refinement of 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)+(0.0824P)²+2.8750P] 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         7625
_refine_ls_number_parameters     391
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0563
_refine_ls_wR_factor_ref         0.1576
_refine_ls_wR_factor_gt          0.1492
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_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 1.13857(18) 0.25082(16) 0.54275(12) 0.0272(4) Uani 1 1 d . . .
C2 C 1.1621(2) 0.21210(18) 0.49146(13) 0.0315(5) Uani 1 1 d . . .
H2 H 1.1212 0.2360 0.4404 0.038 Uiso 1 1 calc R . .
C3 C 1.2443(2) 0.13835(18) 0.51101(13) 0.0313(5) Uani 1 1 d . . .
H3 H 1.2554 0.1147 0.4723 0.038 Uiso 1 1 calc R . .
C4 C 1.30898(19) 0.09936(16) 0.58350(13) 0.0267(4) Uani 1 1 d . . .
C5 C 1.28920(19) 0.13887(15) 0.63899(12) 0.0259(4) Uani 1 1 d . . .
C6 C 1.20514(19) 0.21355(16) 0.61895(12) 0.0263(4) Uani 1 1 d . . .
C7 C 0.87877(18) 0.40374(14) 0.49200(12) 0.0233(4) Uani 1 1 d . . .
H7 H 0.8686 0.4652 0.5122 0.028 Uiso 1 1 calc R . .
C8 C 0.89142(18) 0.41848(15) 0.42239(12) 0.0241(4) Uani 1 1 d . . .
H8 H 0.9074 0.4868 0.4176 0.029 Uiso 1 1 calc R . .
C9 C 0.77746(18) 0.38463(16) 0.34994(12) 0.0259(4) Uani 1 1 d . . .
C10 C 0.72516(18) 0.32213(15) 0.38342(12) 0.0229(4) Uani 1 1 d . . .
C11 C 0.63631(18) 0.25573(16) 0.34507(12) 0.0250(4) Uani 1 1 d . . .
H11 H 0.6028 0.2424 0.2921 0.030 Uiso 1 1 calc R . .
C12 C 0.59834(17) 0.20955(15) 0.38703(12) 0.0232(4) Uani 1 1 d . . .
C13 C 0.51456(18) 0.12703(15) 0.36084(12) 0.0250(4) Uani 1 1 d . . .
H13 H 0.4343 0.1448 0.3182 0.030 Uiso 1 1 calc R . .
C14 C 0.52007(18) 0.09615(15) 0.43529(13) 0.0254(4) Uani 1 1 d . . .
H14 H 0.4410 0.0815 0.4243 0.030 Uiso 1 1 calc R . .
C15 C 0.57739(19) 0.17844(16) 0.49346(13) 0.0266(4) Uani 1 1 d . . .
C16 C 0.64297(18) 0.23117(15) 0.46401(12) 0.0230(4) Uani 1 1 d . . .
C17 C 0.73340(18) 0.29613(15) 0.50283(12) 0.0238(4) Uani 1 1 d . . .
H17 H 0.7655 0.3107 0.5555 0.029 Uiso 1 1 calc R . .
C18 C 0.77512(17) 0.33897(14) 0.46164(12) 0.0220(4) Uani 1 1 d . . .
C19 C 0.7963(3) 0.3327(2) 0.29280(15) 0.0429(6) Uani 1 1 d . . .
H19A H 0.8427 0.2752 0.3169 0.064 Uiso 1 1 calc R . .
H19B H 0.8373 0.3747 0.2772 0.064 Uiso 1 1 calc R . .
H19C H 0.7210 0.3147 0.2475 0.064 Uiso 1 1 calc R . .
C20 C 0.6999(2) 0.4725(2) 0.31248(17) 0.0441(7) Uani 1 1 d . . .
H20A H 0.6222 0.4521 0.2712 0.066 Uiso 1 1 calc R . .
H20B H 0.7337 0.5136 0.2912 0.066 Uiso 1 1 calc R . .
H20C H 0.6942 0.5080 0.3512 0.066 Uiso 1 1 calc R . .
C21 C 0.6538(2) 0.1448(2) 0.57655(14) 0.0397(6) Uani 1 1 d . . .
H21A H 0.7153 0.1033 0.5817 0.060 Uiso 1 1 calc R . .
H21B H 0.6065 0.1093 0.5908 0.060 Uiso 1 1 calc R . .
H21C H 0.6888 0.2000 0.6105 0.060 Uiso 1 1 calc R . .
C22 C 0.4806(2) 0.24408(19) 0.48445(16) 0.0373(5) Uani 1 1 d . . .
H22A H 0.5152 0.3018 0.5153 0.056 Uiso 1 1 calc R . .
H22B H 0.4362 0.2106 0.5021 0.056 Uiso 1 1 calc R . .
H22C H 0.4287 0.2616 0.4303 0.056 Uiso 1 1 calc R . .
B1 B 1.0366(2) 0.32279(17) 0.51202(14) 0.0252(5) Uani 1 1 d . . .
B2 B 1.3885(2) 0.01246(18) 0.59650(14) 0.0256(5) Uani 1 1 d . . .
N1 N 1.19832(18) 0.24191(15) 0.67843(11) 0.0335(4) Uani 1 1 d . . .
N2 N 1.34422(19) 0.11242(15) 0.71345(11) 0.0338(4) Uani 1 1 d . . .
O1 O 0.98430(12) 0.35291(11) 0.54914(8) 0.0243(3) Uani 1 1 d . . .
O2 O 0.98821(14) 0.35902(12) 0.43964(9) 0.0309(4) Uani 1 1 d . . .
O3 O 0.56080(13) 0.04648(11) 0.34121(9) 0.0269(3) Uani 1 1 d . . .
O4 O 0.59213(14) 0.01217(11) 0.45967(9) 0.0295(3) Uani 1 1 d . . .
S1 S 1.29046(6) 0.17774(5) 0.75124(3) 0.04030(18) Uani 1 1 d . . .
N101 N 1.1008(4) -0.1015(3) 0.5003(2) 0.0596(5) Uiso 0.50 1 d PG A -1
C101 C 1.0603(4) -0.0958(3) 0.4263(2) 0.0596(5) Uiso 0.50 1 d PG A -1
H101 H 1.0935 -0.1422 0.4055 0.072 Uiso 0.50 1 d PG A -1
C102 C 0.9740(4) -0.0320(3) 0.3754(2) 0.0596(5) Uiso 0.50 1 d PG A -1
H102 H 0.9469 -0.0337 0.3207 0.072 Uiso 0.50 1 d PG A -1
C103 C 0.9278(4) 0.0286(3) 0.4027(2) 0.0596(5) Uiso 0.50 1 d PG A -1
H103 H 0.8668 0.0744 0.3710 0.072 Uiso 0.50 1 d PG A -1
C104 C 0.9207(4) 0.0851(3) 0.5146(3) 0.0596(5) Uiso 0.50 1 d PG A -1
H104 H 0.8626 0.1295 0.4823 0.072 Uiso 0.50 1 d PG A -1
C105 C 0.9585(4) 0.0766(3) 0.5901(3) 0.0596(5) Uiso 0.50 1 d PG A -1
H105 H 0.9257 0.1136 0.6133 0.072 Uiso 0.50 1 d PG A -1
C106 C 1.0450(4) 0.0095(3) 0.6368(2) 0.0596(5) Uiso 0.50 1 d PG A -1
H106 H 1.0716 0.0027 0.6936 0.072 Uiso 0.50 1 d PG A -1
C107 C 1.0920(4) -0.0474(3) 0.6069(2) 0.0596(5) Uiso 0.50 1 d PG A -1
H107 H 1.1526 -0.0940 0.6382 0.072 Uiso 0.50 1 d PG A -1
C108 C 1.0535(3) -0.0408(3) 0.5284(2) 0.0596(5) Uiso 0.50 1 d PG A -1
C109 C 0.9663(3) 0.0263(3) 0.4814(2) 0.0596(5) Uiso 0.50 1 d PG A -1
C201 C -0.0462(2) 0.6296(2) 0.27758(15) 0.0446(6) Uani 1 1 d . . .
H201 H -0.0611 0.6562 0.3164 0.054 Uiso 1 1 calc R B 1
Cl1A Cl -0.1812(6) 0.6085(7) 0.1910(3) 0.0716(13) Uani 0.70(3) 1 d P C 1
Cl2A Cl 0.0339(6) 0.5221(3) 0.3143(3) 0.0623(10) Uani 0.70(3) 1 d P C 1
Cl3A Cl 0.0343(4) 0.7125(4) 0.2620(3) 0.0666(11) Uani 0.70(3) 1 d P C 1
Cl1B Cl -0.1751(13) 0.5932(11) 0.1954(8) 0.060(2) Uani 0.30(3) 1 d P C 2
Cl2B Cl 0.0519(19) 0.542(2) 0.3128(9) 0.095(4) Uani 0.30(3) 1 d P C 2
Cl3B Cl 0.006(3) 0.732(2) 0.2557(12) 0.115(5) Uani 0.30(3) 1 d P C 2
C202 C 0.4558(2) 0.56254(18) 0.33183(14) 0.0363(5) Uani 1 1 d . D 1
H202 H 0.4459 0.5342 0.2843 0.044 Uiso 1 1 calc R D 1
Cl4 Cl 0.31879(7) 0.59707(6) 0.31183(6) 0.0612(2) Uani 1 1 d . D 1
Cl5 Cl 0.51710(8) 0.47674(6) 0.40446(5) 0.0584(2) Uani 1 1 d . D 1
Cl6 Cl 0.54722(7) 0.66299(5) 0.35810(4) 0.04778(19) Uani 1 1 d . D 1


_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 1.376(3) . ?
C1 C6 1.427(3) . ?
C1 B1 1.554(3) . ?
C2 C3 1.418(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.377(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.425(3) . ?
C4 B2 1.558(3) . ?
C5 N2 1.350(3) . ?
C5 C6 1.442(3) . ?
C6 N1 1.343(3) . ?
C7 O1 1.466(2) . ?
C7 C18 1.507(3) . ?
C7 C8 1.553(3) . ?
C7 H7 1.0000 . ?
C8 O2 1.438(3) . ?
C8 C9 1.542(3) . ?
C8 H8 1.0000 . ?
C9 C10 1.515(3) . ?
C9 C19 1.524(3) . ?
C9 C20 1.537(3) . ?
C10 C11 1.391(3) . ?
C10 C18 1.395(3) . ?
C11 C12 1.389(3) . ?
C11 H11 0.9500 . ?
C12 C16 1.396(3) . ?
C12 C13 1.510(3) . ?
C13 O3 1.456(3) . ?
C13 C14 1.561(3) . ?
C13 H13 1.0000 . ?
C14 O4 1.442(3) . ?
C14 C15 1.542(3) . ?
C14 H14 1.0000 . ?
C15 C16 1.521(3) . ?
C15 C21 1.526(3) . ?
C15 C22 1.540(3) . ?
C16 C17 1.391(3) . ?
C17 C18 1.392(3) . ?
C17 H17 0.9500 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
B1 O2 1.366(3) . ?
B1 O1 1.368(3) . ?
B2 O3 1.364(3) 3_756 ?
B2 O4 1.368(3) 3_756 ?
N1 S1 1.618(2) . ?
N2 S1 1.616(2) . ?
O3 B2 1.364(3) 3_756 ?
O4 B2 1.368(3) 3_756 ?
N101 C101 1.3186 . ?
N101 C108 1.3742 . ?
C101 C102 1.4004 . ?
C101 H101 1.0130 . ?
C102 C103 1.3502 . ?
C102 H102 0.9834 . ?
C103 C109 1.4142 . ?
C103 H103 0.9741 . ?
C104 C105 1.3586 . ?
C104 C109 1.4163 . ?
C104 H104 0.9460 . ?
C105 C106 1.4092 . ?
C105 H105 0.9664 . ?
C106 C107 1.3653 . ?
C106 H106 1.0287 . ?
C107 C108 1.4123 . ?
C107 H107 0.9762 . ?
C108 C109 1.4152 . ?
C201 Cl2B 1.673(17) . ?
C201 Cl1B 1.739(13) . ?
C201 Cl3A 1.748(5) . ?
C201 Cl3B 1.766(17) . ?
C201 Cl1A 1.770(6) . ?
C201 Cl2A 1.777(6) . ?
C201 H201 1.0000 . ?
C202 Cl5 1.746(3) . ?
C202 Cl4 1.756(3) . ?
C202 Cl6 1.765(3) . ?
C202 H202 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
C2 C1 C6 115.5(2) . . ?
C2 C1 B1 118.3(2) . . ?
C6 C1 B1 125.9(2) . . ?
C1 C2 C3 123.3(2) . . ?
C1 C2 H2 118.4 . . ?
C3 C2 H2 118.4 . . ?
C4 C3 C2 123.0(2) . . ?
C4 C3 H3 118.5 . . ?
C2 C3 H3 118.5 . . ?
C3 C4 C5 115.6(2) . . ?
C3 C4 B2 118.5(2) . . ?
C5 C4 B2 125.7(2) . . ?
N2 C5 C4 125.4(2) . . ?
N2 C5 C6 113.2(2) . . ?
C4 C5 C6 121.34(19) . . ?
N1 C6 C1 125.7(2) . . ?
N1 C6 C5 113.05(19) . . ?
C1 C6 C5 121.2(2) . . ?
O1 C7 C18 109.77(16) . . ?
O1 C7 C8 104.93(16) . . ?
C18 C7 C8 104.18(16) . . ?
O1 C7 H7 112.5 . . ?
C18 C7 H7 112.5 . . ?
C8 C7 H7 112.5 . . ?
O2 C8 C9 112.03(17) . . ?
O2 C8 C7 103.96(16) . . ?
C9 C8 C7 107.39(16) . . ?
O2 C8 H8 111.1 . . ?
C9 C8 H8 111.1 . . ?
C7 C8 H8 111.1 . . ?
C10 C9 C19 113.35(19) . . ?
C10 C9 C20 109.08(18) . . ?
C19 C9 C20 110.7(2) . . ?
C10 C9 C8 102.36(16) . . ?
C19 C9 C8 113.26(19) . . ?
C20 C9 C8 107.65(19) . . ?
C11 C10 C18 120.34(19) . . ?
C11 C10 C9 127.63(19) . . ?
C18 C10 C9 112.02(18) . . ?
C12 C11 C10 117.59(19) . . ?
C12 C11 H11 121.2 . . ?
C10 C11 H11 121.2 . . ?
C11 C12 C16 121.98(19) . . ?
C11 C12 C13 126.99(19) . . ?
C16 C12 C13 110.85(18) . . ?
O3 C13 C12 109.61(17) . . ?
O3 C13 C14 105.20(16) . . ?
C12 C13 C14 103.66(17) . . ?
O3 C13 H13 112.6 . . ?
C12 C13 H13 112.6 . . ?
C14 C13 H13 112.6 . . ?
O4 C14 C15 112.07(17) . . ?
O4 C14 C13 103.40(16) . . ?
C15 C14 C13 107.13(17) . . ?
O4 C14 H14 111.3 . . ?
C15 C14 H14 111.3 . . ?
C13 C14 H14 111.3 . . ?
C16 C15 C21 114.05(19) . . ?
C16 C15 C22 108.38(18) . . ?
C21 C15 C22 110.1(2) . . ?
C16 C15 C14 102.35(17) . . ?
C21 C15 C14 113.38(19) . . ?
C22 C15 C14 108.15(18) . . ?
C17 C16 C12 120.39(19) . . ?
C17 C16 C15 128.42(19) . . ?
C12 C16 C15 111.16(18) . . ?
C16 C17 C18 117.46(18) . . ?
C16 C17 H17 121.3 . . ?
C18 C17 H17 121.3 . . ?
C17 C18 C10 122.01(19) . . ?
C17 C18 C7 127.62(18) . . ?
C10 C18 C7 110.31(18) . . ?
C9 C19 H19A 109.5 . . ?
C9 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C9 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C9 C20 H20A 109.5 . . ?
C9 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C9 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C15 C21 H21A 109.5 . . ?
C15 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C15 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C15 C22 H22A 109.5 . . ?
C15 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C15 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O2 B1 O1 114.12(19) . . ?
O2 B1 C1 119.1(2) . . ?
O1 B1 C1 126.7(2) . . ?
O3 B2 O4 114.6(2) 3_756 3_756 ?
O3 B2 C4 126.1(2) 3_756 . ?
O4 B2 C4 119.3(2) 3_756 . ?
C6 N1 S1 106.41(16) . . ?
C5 N2 S1 106.02(16) . . ?
B1 O1 C7 106.51(16) . . ?
B1 O2 C8 108.93(17) . . ?
B2 O3 C13 106.49(17) 3_756 . ?
B2 O4 C14 108.61(17) 3_756 . ?
N2 S1 N1 101.28(10) . . ?
C101 N101 C108 117.0 . . ?
N101 C101 C102 124.5 . . ?
C103 C102 C101 118.9 . . ?
C102 C103 C109 119.8 . . ?
C105 C104 C109 120.8 . . ?
C104 C105 C106 120.3 . . ?
C107 C106 C105 120.5 . . ?
C106 C107 C108 120.4 . . ?
N101 C108 C107 118.4 . . ?
N101 C108 C109 122.4 . . ?
C107 C108 C109 119.2 . . ?
C103 C109 C108 117.3 . . ?
C103 C109 C104 123.8 . . ?
C108 C109 C104 118.8 . . ?
Cl2B C201 Cl1B 111.2(9) . . ?
Cl2B C201 Cl3A 97.6(12) . . ?
Cl1B C201 Cl3A 115.1(4) . . ?
Cl2B C201 Cl3B 111.8(6) . . ?
Cl1B C201 Cl3B 109.0(9) . . ?
Cl3A C201 Cl3B 14.2(13) . . ?
Cl2B C201 Cl1A 118.1(7) . . ?
Cl1B C201 Cl1A 7.5(7) . . ?
Cl3A C201 Cl1A 110.1(3) . . ?
Cl3B C201 Cl1A 102.8(8) . . ?
Cl2B C201 Cl2A 12.2(13) . . ?
Cl1B C201 Cl2A 103.5(6) . . ?
Cl3A C201 Cl2A 109.8(3) . . ?
Cl3B C201 Cl2A 124.0(13) . . ?
Cl1A C201 Cl2A 110.9(4) . . ?
Cl2B C201 H201 112.9 . . ?
Cl1B C201 H201 110.8 . . ?
Cl3A C201 H201 108.7 . . ?
Cl3B C201 H201 100.8 . . ?
Cl1A C201 H201 108.7 . . ?
Cl2A C201 H201 108.7 . . ?
Cl5 C202 Cl4 110.44(15) . . ?
Cl5 C202 Cl6 110.77(14) . . ?
Cl4 C202 Cl6 109.96(14) . . ?
Cl5 C202 H202 108.5 . . ?
Cl4 C202 H202 108.5 . . ?
Cl6 C202 H202 108.5 . . ?

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 1.6(3) . . . . ?
B1 C1 C2 C3 -173.0(2) . . . . ?
C1 C2 C3 C4 -0.6(4) . . . . ?
C2 C3 C4 C5 -0.8(3) . . . . ?
C2 C3 C4 B2 174.5(2) . . . . ?
C3 C4 C5 N2 -178.9(2) . . . . ?
B2 C4 C5 N2 6.2(4) . . . . ?
C3 C4 C5 C6 1.0(3) . . . . ?
B2 C4 C5 C6 -173.8(2) . . . . ?
C2 C1 C6 N1 178.7(2) . . . . ?
B1 C1 C6 N1 -7.3(4) . . . . ?
C2 C1 C6 C5 -1.2(3) . . . . ?
B1 C1 C6 C5 172.8(2) . . . . ?
N2 C5 C6 N1 0.0(3) . . . . ?
C4 C5 C6 N1 -180.0(2) . . . . ?
N2 C5 C6 C1 179.9(2) . . . . ?
C4 C5 C6 C1 -0.1(3) . . . . ?
O1 C7 C8 O2 11.4(2) . . . . ?
C18 C7 C8 O2 -104.01(18) . . . . ?
O1 C7 C8 C9 130.23(17) . . . . ?
C18 C7 C8 C9 14.9(2) . . . . ?
O2 C8 C9 C10 94.39(19) . . . . ?
C7 C8 C9 C10 -19.1(2) . . . . ?
O2 C8 C9 C19 -28.0(3) . . . . ?
C7 C8 C9 C19 -141.5(2) . . . . ?
O2 C8 C9 C20 -150.71(18) . . . . ?
C7 C8 C9 C20 95.7(2) . . . . ?
C19 C9 C10 C11 -41.7(3) . . . . ?
C20 C9 C10 C11 82.1(3) . . . . ?
C8 C9 C10 C11 -164.0(2) . . . . ?
C19 C9 C10 C18 139.7(2) . . . . ?
C20 C9 C10 C18 -96.5(2) . . . . ?
C8 C9 C10 C18 17.4(2) . . . . ?
C18 C10 C11 C12 1.5(3) . . . . ?
C9 C10 C11 C12 -177.0(2) . . . . ?
C10 C11 C12 C16 2.9(3) . . . . ?
C10 C11 C12 C13 -171.9(2) . . . . ?
C11 C12 C13 O3 59.8(3) . . . . ?
C16 C12 C13 O3 -115.47(19) . . . . ?
C11 C12 C13 C14 171.7(2) . . . . ?
C16 C12 C13 C14 -3.6(2) . . . . ?
O3 C13 C14 O4 12.6(2) . . . . ?
C12 C13 C14 O4 -102.44(18) . . . . ?
O3 C13 C14 C15 131.18(17) . . . . ?
C12 C13 C14 C15 16.1(2) . . . . ?
O4 C14 C15 C16 91.1(2) . . . . ?
C13 C14 C15 C16 -21.6(2) . . . . ?
O4 C14 C15 C21 -32.2(3) . . . . ?
C13 C14 C15 C21 -144.95(19) . . . . ?
O4 C14 C15 C22 -154.59(18) . . . . ?
C13 C14 C15 C22 92.7(2) . . . . ?
C11 C12 C16 C17 -4.3(3) . . . . ?
C13 C12 C16 C17 171.24(19) . . . . ?
C11 C12 C16 C15 173.73(19) . . . . ?
C13 C12 C16 C15 -10.8(2) . . . . ?
C21 C15 C16 C17 -39.1(3) . . . . ?
C22 C15 C16 C17 83.9(3) . . . . ?
C14 C15 C16 C17 -162.0(2) . . . . ?
C21 C15 C16 C12 143.1(2) . . . . ?
C22 C15 C16 C12 -93.9(2) . . . . ?
C14 C15 C16 C12 20.3(2) . . . . ?
C12 C16 C17 C18 1.1(3) . . . . ?
C15 C16 C17 C18 -176.5(2) . . . . ?
C16 C17 C18 C10 3.4(3) . . . . ?
C16 C17 C18 C7 -173.6(2) . . . . ?
C11 C10 C18 C17 -4.8(3) . . . . ?
C9 C10 C18 C17 173.96(19) . . . . ?
C11 C10 C18 C7 172.69(19) . . . . ?
C9 C10 C18 C7 -8.6(2) . . . . ?
O1 C7 C18 C17 61.2(3) . . . . ?
C8 C7 C18 C17 173.1(2) . . . . ?
O1 C7 C18 C10 -116.06(19) . . . . ?
C8 C7 C18 C10 -4.2(2) . . . . ?
C2 C1 B1 O2 -12.3(3) . . . . ?
C6 C1 B1 O2 173.8(2) . . . . ?
C2 C1 B1 O1 165.0(2) . . . . ?
C6 C1 B1 O1 -8.9(4) . . . . ?
C3 C4 B2 O3 -165.7(2) . . . 3_756 ?
C5 C4 B2 O3 9.0(4) . . . 3_756 ?
C3 C4 B2 O4 11.3(3) . . . 3_756 ?
C5 C4 B2 O4 -173.9(2) . . . 3_756 ?
C1 C6 N1 S1 179.76(19) . . . . ?
C5 C6 N1 S1 -0.3(2) . . . . ?
C4 C5 N2 S1 -179.71(19) . . . . ?
C6 C5 N2 S1 0.3(2) . . . . ?
O2 B1 O1 C7 9.1(2) . . . . ?
C1 B1 O1 C7 -168.3(2) . . . . ?
C18 C7 O1 B1 99.14(19) . . . . ?
C8 C7 O1 B1 -12.3(2) . . . . ?
O1 B1 O2 C8 -1.4(3) . . . . ?
C1 B1 O2 C8 176.24(19) . . . . ?
C9 C8 O2 B1 -122.04(19) . . . . ?
C7 C8 O2 B1 -6.4(2) . . . . ?
C12 C13 O3 B2 98.3(2) . . . 3_756 ?
C14 C13 O3 B2 -12.6(2) . . . 3_756 ?
C15 C14 O4 B2 -123.26(19) . . . 3_756 ?
C13 C14 O4 B2 -8.2(2) . . . 3_756 ?
C5 N2 S1 N1 -0.47(19) . . . . ?
C6 N1 S1 N2 0.47(19) . . . . ?
C108 N101 C101 C102 0.6 . . . . ?
N101 C101 C102 C103 0.1 . . . . ?
C101 C102 C103 C109 -0.5 . . . . ?
C109 C104 C105 C106 0.7 . . . . ?
C104 C105 C106 C107 0.3 . . . . ?
C105 C106 C107 C108 -1.0 . . . . ?
C101 N101 C108 C107 177.8 . . . . ?
C101 N101 C108 C109 -0.9 . . . . ?
C106 C107 C108 N101 -178.0 . . . . ?
C106 C107 C108 C109 0.7 . . . . ?
C102 C103 C109 C108 0.3 . . . . ?
C102 C103 C109 C104 -178.2 . . . . ?
N101 C108 C109 C103 0.4 . . . . ?
C107 C108 C109 C103 -178.2 . . . . ?
N101 C108 C109 C104 178.9 . . . . ?
C107 C108 C109 C104 0.3 . . . . ?
C105 C104 C109 C103 177.4 . . . . ?
C105 C104 C109 C108 -1.0 . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.44
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.197
_refine_diff_density_min         -0.851
_refine_diff_density_rms         0.080
