# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Rajendra Rathore'
_publ_contact_author_email       RAJENDRA.RATHORE@MARQUETTE.EDU

_publ_section_title              
;
Octamethoxydibenzochrysene: Isolation and X-ray
crystallographic characterization of a twisted polyaromatic cation radical
;
loop_
_publ_author_name
'Rajendra Rathore'
'Sergey V. Lindeman'
'Tushar S. Navale'
'Linyi Zhai.'

# Attachment 'raj3d.cif'

data_raj3d
_database_code_depnum_ccdc_archive 'CCDC 720096'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H36 Cl10 O8 Sb'
_chemical_formula_weight         1072.90

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'
O O 0.0492 0.0322 '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'
Sb Sb -0.0562 5.8946 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   13.6451(5)
_cell_length_b                   14.0770(5)
_cell_length_c                   14.3621(5)
_cell_angle_alpha                61.672(2)
_cell_angle_beta                 62.275(2)
_cell_angle_gamma                70.899(2)
_cell_volume                     2129.38(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5352
_cell_measurement_theta_min      3.5
_cell_measurement_theta_max      60

_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1074
_exptl_absorpt_coefficient_mu    11.327
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.0874
_exptl_absorpt_correction_T_max  0.5044
_exptl_absorpt_process_details   
;
Numerical (based on real shape of the crystal) absorption
correction followed by:
SADABS. Program for empirical absorption correction of
area-detector data. University of Goetingen. Germany.
Sheldrick, G. M. 1996
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX2 CCD detector'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16984
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.60
_diffrn_reflns_theta_max         62.76
_reflns_number_total             6159
_reflns_number_gt                5672
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 v2.0-2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT v7.23A (Bruker, 2005)'
_computing_data_reduction        'SADABS-2004/1 (Bruker, 2005)'
_computing_structure_solution    'XS/SHELXTL v6.12 (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 v.97-2 (Sheldrick, 1993-1997)'
_computing_molecular_graphics    'XP v5.1 (Bruker, 1998)'
_computing_publication_material  'XCIF v6.12 (Bruker, 2001)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0351P)^2^+2.5961P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6159
_refine_ls_number_parameters     644
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0277
_refine_ls_wR_factor_ref         0.0728
_refine_ls_wR_factor_gt          0.0714
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_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
Sb1 Sb 0.5000 0.0000 0.5000 0.01415(9) Uani 1 2 d S . .
Cl1 Cl 0.51673(6) 0.00955(6) 0.32469(6) 0.02187(17) Uani 1 1 d . . .
Cl2 Cl 0.37087(6) 0.16378(6) 0.48035(7) 0.02428(17) Uani 1 1 d . . .
Cl3 Cl 0.64831(6) 0.10502(6) 0.40277(6) 0.02394(18) Uani 1 1 d . . .
Sb2 Sb 0.5000 0.0000 1.0000 0.01830(9) Uani 1 2 d S . .
Cl4 Cl 0.62559(7) 0.04551(7) 1.03917(7) 0.02945(19) Uani 1 1 d . . .
Cl5 Cl 0.43828(8) -0.13109(7) 1.18729(7) 0.0369(2) Uani 1 1 d . . .
Cl6 Cl 0.64170(7) -0.13462(7) 0.94038(8) 0.0368(2) Uani 1 1 d . . .
O1 O -0.19186(17) 0.33690(17) 1.12469(18) 0.0235(5) Uani 1 1 d . . .
O2 O -0.23404(16) 0.50938(17) 1.16405(17) 0.0217(5) Uani 1 1 d . . .
O3 O 0.13172(16) 0.99193(15) 0.50167(17) 0.0195(5) Uani 1 1 d . . .
O4 O -0.01511(17) 1.00473(16) 0.69136(18) 0.0240(5) Uani 1 1 d . . .
O5 O -0.16920(16) 0.30166(16) 0.70723(18) 0.0201(5) Uani 1 1 d . . .
O6 O 0.00043(16) 0.26846(16) 0.53841(18) 0.0190(5) Uani 1 1 d . . .
O7 O 0.50298(15) 0.63584(16) 0.39509(17) 0.0172(4) Uani 1 1 d . . .
O8 O 0.50597(16) 0.50546(17) 0.31551(18) 0.0210(5) Uani 1 1 d . . .
C1 C 0.0311(2) 0.5270(2) 0.7201(3) 0.0151(6) Uani 1 1 d . . .
C2 C 0.1100(2) 0.6032(2) 0.6491(2) 0.0144(6) Uani 1 1 d . . .
C11 C -0.0394(2) 0.5247(2) 0.8335(3) 0.0155(6) Uani 1 1 d . . .
C12 C -0.0844(2) 0.4294(3) 0.9237(3) 0.0168(7) Uani 1 1 d . . .
C13 C -0.1479(2) 0.4255(2) 1.0327(3) 0.0179(7) Uani 1 1 d . . .
C14 C -0.1695(2) 0.5196(3) 1.0554(3) 0.0186(7) Uani 1 1 d . . .
C15 C -0.1228(2) 0.6117(3) 0.9690(3) 0.0171(7) Uani 1 1 d . . .
C16 C -0.0560(2) 0.6160(2) 0.8583(3) 0.0154(6) Uani 1 1 d . . .
C17 C -0.1677(3) 0.2393(3) 1.1049(3) 0.0275(8) Uani 1 1 d . . .
C18 C -0.2635(3) 0.6044(3) 1.1901(3) 0.0233(7) Uani 1 1 d . . .
C21 C 0.0823(2) 0.7030(2) 0.6658(2) 0.0143(6) Uani 1 1 d . . .
C22 C 0.1287(2) 0.7982(2) 0.5747(3) 0.0145(6) Uani 1 1 d . . .
C23 C 0.0955(2) 0.8966(2) 0.5851(3) 0.0163(6) Uani 1 1 d . . .
C24 C 0.0120(2) 0.9044(2) 0.6891(3) 0.0181(7) Uani 1 1 d . . .
C25 C -0.0366(2) 0.8131(2) 0.7768(3) 0.0167(6) Uani 1 1 d . . .
C26 C -0.0039(2) 0.7124(2) 0.7669(3) 0.0156(6) Uani 1 1 d . . .
C27 C 0.2181(3) 0.9865(3) 0.3971(3) 0.0219(7) Uani 1 1 d . . .
C28 C -0.1010(3) 1.0189(3) 0.7936(3) 0.0294(8) Uani 1 1 d . . .
C31 C 0.0255(2) 0.4595(2) 0.6734(3) 0.0156(6) Uani 1 1 d . . .
C32 C -0.0725(2) 0.4110(2) 0.7184(3) 0.0165(6) Uani 1 1 d . . .
C33 C -0.0793(2) 0.3498(2) 0.6718(3) 0.0162(6) Uani 1 1 d . . .
C34 C 0.0137(2) 0.3323(2) 0.5762(3) 0.0178(7) Uani 1 1 d . . .
C35 C 0.1074(2) 0.3818(2) 0.5297(3) 0.0161(6) Uani 1 1 d . . .
C36 C 0.1153(2) 0.4471(2) 0.5746(3) 0.0159(6) Uani 1 1 d . . .
C37 C -0.2613(3) 0.3101(3) 0.8071(3) 0.0248(7) Uani 1 1 d . . .
C38 C 0.0968(3) 0.2370(3) 0.4521(3) 0.0203(7) Uani 1 1 d . . .
C41 C 0.2103(2) 0.5779(2) 0.5619(2) 0.0144(6) Uani 1 1 d . . .
C42 C 0.3084(2) 0.6235(2) 0.5196(2) 0.0141(6) Uani 1 1 d . . .
C43 C 0.4050(2) 0.5983(2) 0.4382(3) 0.0151(6) Uani 1 1 d . . .
C44 C 0.4068(2) 0.5246(2) 0.3956(2) 0.0162(6) Uani 1 1 d . . .
C45 C 0.3134(2) 0.4762(2) 0.4395(3) 0.0160(6) Uani 1 1 d . . .
C46 C 0.2146(2) 0.4999(2) 0.5243(2) 0.0150(6) Uani 1 1 d . . .
C47 C 0.5024(3) 0.7176(3) 0.4276(3) 0.0204(7) Uani 1 1 d . . .
C48 C 0.5130(3) 0.4390(3) 0.2612(3) 0.0223(7) Uani 1 1 d . . .
H12 H -0.069(2) 0.370(3) 0.910(3) 0.013(8) Uiso 1 1 d . . .
H15 H -0.133(3) 0.670(3) 0.986(3) 0.021(9) Uiso 1 1 d . . .
H17A H -0.202(3) 0.252(3) 1.050(3) 0.037(10) Uiso 1 1 d . . .
H17B H -0.204(3) 0.188(3) 1.179(3) 0.027(9) Uiso 1 1 d . . .
H17C H -0.087(3) 0.213(3) 1.080(3) 0.030(9) Uiso 1 1 d . . .
H18A H -0.313(3) 0.582(3) 1.268(3) 0.028(9) Uiso 1 1 d . . .
H18B H -0.300(3) 0.661(3) 1.142(3) 0.023(9) Uiso 1 1 d . . .
H18C H -0.196(3) 0.628(2) 1.179(3) 0.016(8) Uiso 1 1 d . . .
H22 H 0.178(3) 0.794(2) 0.507(3) 0.015(8) Uiso 1 1 d . . .
H25 H -0.093(3) 0.821(3) 0.841(3) 0.026(9) Uiso 1 1 d . . .
H27A H 0.284(3) 0.944(3) 0.408(3) 0.014(8) Uiso 1 1 d . . .
H27B H 0.189(3) 0.962(3) 0.361(3) 0.018(8) Uiso 1 1 d . . .
H27C H 0.234(3) 1.065(3) 0.347(3) 0.026(9) Uiso 1 1 d . . .
H28A H -0.111(3) 1.093(3) 0.772(3) 0.030(10) Uiso 1 1 d . . .
H28B H -0.077(3) 0.972(3) 0.862(4) 0.040(11) Uiso 1 1 d . . .
H28C H -0.175(3) 0.996(3) 0.813(3) 0.036(10) Uiso 1 1 d . . .
H32 H -0.132(3) 0.424(3) 0.774(3) 0.017(8) Uiso 1 1 d . . .
H35 H 0.165(3) 0.372(2) 0.466(3) 0.010(7) Uiso 1 1 d . . .
H37A H -0.319(3) 0.279(3) 0.818(3) 0.018(8) Uiso 1 1 d . . .
H37B H -0.240(3) 0.277(3) 0.873(3) 0.030(10) Uiso 1 1 d . . .
H37C H -0.293(3) 0.389(4) 0.792(3) 0.044(11) Uiso 1 1 d . . .
H38A H 0.071(3) 0.189(3) 0.440(3) 0.016(8) Uiso 1 1 d . . .
H38B H 0.156(3) 0.202(3) 0.481(3) 0.029(9) Uiso 1 1 d . . .
H38C H 0.117(3) 0.304(3) 0.381(3) 0.022(8) Uiso 1 1 d . . .
H42 H 0.307(3) 0.666(3) 0.552(3) 0.020(9) Uiso 1 1 d . . .
H45 H 0.319(2) 0.425(2) 0.414(2) 0.010(7) Uiso 1 1 d . . .
H47A H 0.484(3) 0.687(3) 0.516(3) 0.020(8) Uiso 1 1 d . . .
H47B H 0.578(3) 0.737(3) 0.384(3) 0.020(8) Uiso 1 1 d . . .
H47C H 0.455(3) 0.777(3) 0.406(3) 0.012(8) Uiso 1 1 d . . .
H48A H 0.498(3) 0.368(3) 0.315(3) 0.024(9) Uiso 1 1 d . . .
H48B H 0.587(3) 0.437(3) 0.208(3) 0.029(9) Uiso 1 1 d . . .
H48C H 0.462(3) 0.473(3) 0.221(3) 0.032(10) Uiso 1 1 d . . .
Cl1S Cl 0.56039(8) 0.35207(9) 0.05237(9) 0.0510(3) Uani 1 1 d . . .
Cl2S Cl 0.31904(8) 0.37024(10) 0.16472(10) 0.0566(3) Uani 1 1 d . . .
C1S C 0.4460(3) 0.2815(3) 0.1535(3) 0.0398(9) Uani 1 1 d . . .
H1SA H 0.4535 0.2446 0.2287 0.048 Uiso 1 1 calc R . .
H1SB H 0.4455 0.2249 0.1314 0.048 Uiso 1 1 calc R . .
Cl3A Cl 0.8312(2) 0.79525(18) 0.2177(2) 0.0661(7) Uani 0.50 1 d P A 1
Cl4A Cl 0.90614(17) 1.00617(17) 0.06309(17) 0.0491(5) Uani 0.50 1 d P . 1
C2SA C 0.8171(6) 0.9310(6) 0.1963(6) 0.0296(16) Uiso 0.50 1 d P A 1
H2S1 H 0.7389 0.9647 0.2049 0.035 Uiso 0.50 1 calc PR A 1
H2S2 H 0.8326 0.9337 0.2558 0.035 Uiso 0.50 1 calc PR A 1
Cl3B Cl 0.88364(19) 0.82079(18) 0.1069(2) 0.0569(6) Uani 0.50 1 d P B 2
Cl4B Cl 0.87030(18) 0.92067(17) 0.25019(19) 0.0551(5) Uani 0.50 1 d P B 2
C2SB C 0.8010(9) 0.8609(11) 0.2232(9) 0.062(3) Uiso 0.50 1 d P B 2
H2S3 H 0.7356 0.9127 0.2081 0.075 Uiso 0.50 1 calc PR B 2
H2S4 H 0.7727 0.7960 0.2922 0.075 Uiso 0.50 1 calc PR B 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Sb1 0.01166(14) 0.01462(15) 0.01507(16) -0.00774(11) -0.00114(11) -0.00320(10)
Cl1 0.0238(4) 0.0257(4) 0.0173(4) -0.0111(3) -0.0040(3) -0.0057(3)
Cl2 0.0209(4) 0.0195(4) 0.0314(4) -0.0128(3) -0.0095(3) 0.0029(3)
Cl3 0.0193(4) 0.0282(4) 0.0231(4) -0.0103(3) -0.0001(3) -0.0131(3)
Sb2 0.01933(15) 0.01960(16) 0.01525(16) -0.00855(11) -0.00237(12) -0.00512(11)
Cl4 0.0291(4) 0.0379(5) 0.0279(4) -0.0155(4) -0.0082(4) -0.0116(3)
Cl5 0.0515(5) 0.0372(5) 0.0196(4) -0.0011(3) -0.0100(4) -0.0235(4)
Cl6 0.0285(4) 0.0369(5) 0.0514(6) -0.0317(4) -0.0095(4) 0.0029(4)
O1 0.0262(11) 0.0209(12) 0.0175(12) -0.0058(9) -0.0005(10) -0.0104(9)
O2 0.0186(10) 0.0249(12) 0.0166(12) -0.0117(9) 0.0030(10) -0.0058(9)
O3 0.0170(10) 0.0124(10) 0.0214(12) -0.0093(9) 0.0031(9) -0.0041(8)
O4 0.0239(11) 0.0156(11) 0.0266(13) -0.0151(9) 0.0019(10) -0.0021(9)
O5 0.0139(10) 0.0204(11) 0.0258(12) -0.0123(9) -0.0007(9) -0.0069(8)
O6 0.0153(10) 0.0186(11) 0.0280(12) -0.0175(9) -0.0023(9) -0.0034(8)
O7 0.0126(10) 0.0183(11) 0.0231(12) -0.0141(9) -0.0004(9) -0.0049(8)
O8 0.0139(10) 0.0261(12) 0.0255(12) -0.0213(10) 0.0039(9) -0.0051(9)
C1 0.0110(13) 0.0121(14) 0.0195(17) -0.0063(12) -0.0043(13) 0.0000(11)
C2 0.0133(14) 0.0146(15) 0.0168(16) -0.0090(12) -0.0055(13) 0.0006(12)
C11 0.0091(13) 0.0172(15) 0.0197(17) -0.0108(12) -0.0022(13) -0.0004(11)
C12 0.0123(14) 0.0136(16) 0.0240(19) -0.0095(13) -0.0036(14) -0.0024(12)
C13 0.0121(14) 0.0201(16) 0.0179(17) -0.0056(13) -0.0026(13) -0.0053(12)
C14 0.0110(14) 0.0260(17) 0.0160(18) -0.0099(13) -0.0003(13) -0.0035(12)
C15 0.0128(14) 0.0171(16) 0.0219(18) -0.0123(14) -0.0028(13) -0.0008(12)
C16 0.0105(14) 0.0166(15) 0.0198(17) -0.0100(13) -0.0035(13) -0.0012(12)
C17 0.035(2) 0.0184(18) 0.022(2) -0.0042(15) -0.0020(17) -0.0132(16)
C18 0.0194(17) 0.0269(19) 0.020(2) -0.0140(15) -0.0004(16) -0.0021(15)
C21 0.0110(13) 0.0157(15) 0.0175(16) -0.0094(12) -0.0037(13) -0.0010(11)
C22 0.0091(13) 0.0161(16) 0.0171(17) -0.0099(12) -0.0006(13) -0.0014(11)
C23 0.0132(14) 0.0132(15) 0.0225(17) -0.0076(12) -0.0051(13) -0.0030(12)
C24 0.0157(14) 0.0159(16) 0.0262(18) -0.0134(13) -0.0067(14) 0.0005(12)
C25 0.0131(14) 0.0178(16) 0.0182(17) -0.0123(13) 0.0001(14) -0.0014(12)
C26 0.0117(14) 0.0170(15) 0.0196(17) -0.0109(12) -0.0055(13) 0.0016(12)
C27 0.0194(17) 0.0184(18) 0.0218(18) -0.0088(14) -0.0014(15) -0.0032(14)
C28 0.034(2) 0.0170(19) 0.029(2) -0.0158(15) -0.0013(17) 0.0009(15)
C31 0.0149(14) 0.0099(15) 0.0189(17) -0.0071(12) -0.0032(13) -0.0003(11)
C32 0.0119(14) 0.0141(15) 0.0181(18) -0.0078(13) 0.0003(14) -0.0019(12)
C33 0.0142(14) 0.0097(14) 0.0223(17) -0.0059(12) -0.0038(13) -0.0037(12)
C34 0.0185(15) 0.0100(15) 0.0250(18) -0.0071(12) -0.0085(14) -0.0011(12)
C35 0.0128(14) 0.0139(15) 0.0190(18) -0.0105(13) -0.0001(14) -0.0011(12)
C36 0.0149(14) 0.0106(15) 0.0204(17) -0.0069(12) -0.0051(13) -0.0005(11)
C37 0.0159(16) 0.029(2) 0.028(2) -0.0152(15) 0.0015(15) -0.0094(15)
C38 0.0151(15) 0.0188(17) 0.032(2) -0.0178(15) -0.0063(15) 0.0008(13)
C41 0.0141(14) 0.0112(14) 0.0158(16) -0.0068(12) -0.0027(13) -0.0012(11)
C42 0.0143(15) 0.0109(14) 0.0166(16) -0.0070(12) -0.0040(13) -0.0012(11)
C43 0.0132(14) 0.0116(15) 0.0193(16) -0.0065(12) -0.0045(13) -0.0016(12)
C44 0.0133(14) 0.0165(15) 0.0150(16) -0.0096(12) 0.0005(13) -0.0010(12)
C45 0.0175(15) 0.0128(15) 0.0200(17) -0.0112(13) -0.0042(13) -0.0016(12)
C46 0.0134(14) 0.0121(15) 0.0189(16) -0.0078(12) -0.0041(13) -0.0009(12)
C47 0.0193(17) 0.0162(17) 0.030(2) -0.0154(14) -0.0057(16) -0.0032(14)
C48 0.0169(17) 0.029(2) 0.0244(19) -0.0213(16) 0.0017(16) -0.0047(14)
Cl1S 0.0306(5) 0.0699(7) 0.0577(7) -0.0461(6) 0.0036(5) -0.0101(5)
Cl2S 0.0268(5) 0.0667(7) 0.0684(8) -0.0307(6) -0.0092(5) -0.0031(5)
C1S 0.045(2) 0.032(2) 0.043(2) -0.0169(17) -0.0160(19) -0.0035(17)
Cl3A 0.0881(17) 0.0282(12) 0.0623(17) -0.0104(10) -0.0184(14) -0.0105(11)
Cl4A 0.0550(12) 0.0505(12) 0.0438(12) -0.0191(9) -0.0042(10) -0.0296(10)
Cl3B 0.0543(12) 0.0536(13) 0.0629(16) -0.0309(11) -0.0092(12) -0.0135(10)
Cl4B 0.0559(12) 0.0469(12) 0.0544(13) -0.0234(10) -0.0068(11) -0.0124(10)

_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
Sb1 Cl1 2.3608(7) 2_656 ?
Sb1 Cl1 2.3608(7) . ?
Sb1 Cl3 2.3665(7) 2_656 ?
Sb1 Cl3 2.3665(7) . ?
Sb1 Cl2 2.3846(7) 2_656 ?
Sb1 Cl2 2.3846(7) . ?
Sb2 Cl5 2.3555(8) 2_657 ?
Sb2 Cl5 2.3555(8) . ?
Sb2 Cl4 2.3709(8) 2_657 ?
Sb2 Cl4 2.3710(8) . ?
Sb2 Cl6 2.3800(8) . ?
Sb2 Cl6 2.3800(8) 2_657 ?
O1 C13 1.360(4) . ?
O1 C17 1.436(4) . ?
O2 C14 1.350(4) . ?
O2 C18 1.440(4) . ?
O3 C23 1.356(4) . ?
O3 C27 1.433(4) . ?
O4 C24 1.350(4) . ?
O4 C28 1.447(4) . ?
O5 C33 1.363(3) . ?
O5 C37 1.428(4) . ?
O6 C34 1.341(4) . ?
O6 C38 1.445(4) . ?
O7 C43 1.354(3) . ?
O7 C47 1.430(4) . ?
O8 C44 1.355(3) . ?
O8 C48 1.435(4) . ?
C1 C2 1.430(4) . ?
C1 C31 1.433(4) . ?
C1 C11 1.447(4) . ?
C2 C21 1.436(4) . ?
C2 C41 1.442(4) . ?
C11 C16 1.415(4) . ?
C11 C12 1.416(4) . ?
C12 C13 1.376(5) . ?
C12 H12 0.88(3) . ?
C13 C14 1.420(4) . ?
C14 C15 1.380(4) . ?
C15 C16 1.399(4) . ?
C15 H15 0.91(4) . ?
C16 C26 1.463(4) . ?
C17 H17A 1.01(4) . ?
C17 H17B 0.95(4) . ?
C17 H17C 0.99(4) . ?
C18 H18A 0.95(4) . ?
C18 H18B 0.95(4) . ?
C18 H18C 0.99(3) . ?
C21 C26 1.415(4) . ?
C21 C22 1.425(4) . ?
C22 C23 1.367(4) . ?
C22 H22 0.91(3) . ?
C23 C24 1.425(4) . ?
C24 C25 1.387(4) . ?
C25 C26 1.396(4) . ?
C25 H25 0.91(4) . ?
C27 H27A 0.94(3) . ?
C27 H27B 1.00(3) . ?
C27 H27C 1.03(4) . ?
C28 H28A 0.91(4) . ?
C28 H28B 1.03(4) . ?
C28 H28C 1.03(4) . ?
C31 C36 1.423(4) . ?
C31 C32 1.431(4) . ?
C32 C33 1.362(4) . ?
C32 H32 0.88(3) . ?
C33 C34 1.432(4) . ?
C34 C35 1.383(4) . ?
C35 C36 1.401(4) . ?
C35 H35 0.92(3) . ?
C36 C46 1.466(4) . ?
C37 H37A 0.94(3) . ?
C37 H37B 0.97(4) . ?
C37 H37C 1.01(4) . ?
C38 H38A 0.97(3) . ?
C38 H38B 0.97(4) . ?
C38 H38C 1.00(3) . ?
C41 C46 1.411(4) . ?
C41 C42 1.418(4) . ?
C42 C43 1.372(4) . ?
C42 H42 0.92(4) . ?
C43 C44 1.422(4) . ?
C44 C45 1.378(4) . ?
C45 C46 1.406(4) . ?
C45 H45 0.92(3) . ?
C47 H47A 1.05(3) . ?
C47 H47B 0.97(3) . ?
C47 H47C 0.89(3) . ?
C48 H48A 0.94(4) . ?
C48 H48B 0.94(4) . ?
C48 H48C 0.96(4) . ?
Cl1S C1S 1.752(4) . ?
Cl2S C1S 1.762(4) . ?
C1S H1SA 0.9900 . ?
C1S H1SB 0.9900 . ?
Cl3A C2SA 1.743(8) . ?
Cl4A C2SA 1.736(7) . ?
Cl4A Cl4A 2.359(4) 2_775 ?
C2SA H2S1 0.9900 . ?
C2SA H2S2 0.9900 . ?
Cl3B C2SB 1.762(11) . ?
Cl4B C2SB 1.710(12) . ?
C2SB H2S3 0.9900 . ?
C2SB H2S4 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
Cl1 Sb1 Cl1 180.00(4) 2_656 . ?
Cl1 Sb1 Cl3 89.98(3) 2_656 2_656 ?
Cl1 Sb1 Cl3 90.02(3) . 2_656 ?
Cl1 Sb1 Cl3 90.02(3) 2_656 . ?
Cl1 Sb1 Cl3 89.98(3) . . ?
Cl3 Sb1 Cl3 180.0 2_656 . ?
Cl1 Sb1 Cl2 90.26(3) 2_656 2_656 ?
Cl1 Sb1 Cl2 89.74(3) . 2_656 ?
Cl3 Sb1 Cl2 89.35(3) 2_656 2_656 ?
Cl3 Sb1 Cl2 90.65(3) . 2_656 ?
Cl1 Sb1 Cl2 89.74(3) 2_656 . ?
Cl1 Sb1 Cl2 90.26(3) . . ?
Cl3 Sb1 Cl2 90.65(3) 2_656 . ?
Cl3 Sb1 Cl2 89.35(3) . . ?
Cl2 Sb1 Cl2 180.00(3) 2_656 . ?
Cl5 Sb2 Cl5 179.999(1) 2_657 . ?
Cl5 Sb2 Cl4 90.76(3) 2_657 2_657 ?
Cl5 Sb2 Cl4 89.24(3) . 2_657 ?
Cl5 Sb2 Cl4 89.24(3) 2_657 . ?
Cl5 Sb2 Cl4 90.76(3) . . ?
Cl4 Sb2 Cl4 180.0 2_657 . ?
Cl5 Sb2 Cl6 90.06(3) 2_657 . ?
Cl5 Sb2 Cl6 89.94(3) . . ?
Cl4 Sb2 Cl6 90.18(3) 2_657 . ?
Cl4 Sb2 Cl6 89.82(3) . . ?
Cl5 Sb2 Cl6 89.94(3) 2_657 2_657 ?
Cl5 Sb2 Cl6 90.06(3) . 2_657 ?
Cl4 Sb2 Cl6 89.82(3) 2_657 2_657 ?
Cl4 Sb2 Cl6 90.18(3) . 2_657 ?
Cl6 Sb2 Cl6 180.0 . 2_657 ?
C13 O1 C17 116.2(2) . . ?
C14 O2 C18 117.5(2) . . ?
C23 O3 C27 116.6(2) . . ?
C24 O4 C28 117.9(2) . . ?
C33 O5 C37 116.6(2) . . ?
C34 O6 C38 117.3(2) . . ?
C43 O7 C47 117.2(2) . . ?
C44 O8 C48 118.4(2) . . ?
C2 C1 C31 117.9(3) . . ?
C2 C1 C11 117.7(3) . . ?
C31 C1 C11 124.3(3) . . ?
C1 C2 C21 117.9(3) . . ?
C1 C2 C41 118.4(3) . . ?
C21 C2 C41 123.6(3) . . ?
C16 C11 C12 118.6(3) . . ?
C16 C11 C1 119.6(3) . . ?
C12 C11 C1 121.5(3) . . ?
C13 C12 C11 121.8(3) . . ?
C13 C12 H12 119(2) . . ?
C11 C12 H12 119(2) . . ?
O1 C13 C12 125.7(3) . . ?
O1 C13 C14 115.1(3) . . ?
C12 C13 C14 119.2(3) . . ?
O2 C14 C15 125.2(3) . . ?
O2 C14 C13 115.3(3) . . ?
C15 C14 C13 119.5(3) . . ?
C14 C15 C16 121.9(3) . . ?
C14 C15 H15 119(2) . . ?
C16 C15 H15 119(2) . . ?
C15 C16 C11 118.9(3) . . ?
C15 C16 C26 122.3(3) . . ?
C11 C16 C26 118.8(3) . . ?
O1 C17 H17A 110(2) . . ?
O1 C17 H17B 103(2) . . ?
H17A C17 H17B 110(3) . . ?
O1 C17 H17C 111(2) . . ?
H17A C17 H17C 114(3) . . ?
H17B C17 H17C 109(3) . . ?
O2 C18 H18A 104(2) . . ?
O2 C18 H18B 108(2) . . ?
H18A C18 H18B 111(3) . . ?
O2 C18 H18C 111.6(18) . . ?
H18A C18 H18C 112(3) . . ?
H18B C18 H18C 110(3) . . ?
C26 C21 C22 118.8(3) . . ?
C26 C21 C2 120.1(3) . . ?
C22 C21 C2 120.4(3) . . ?
C23 C22 C21 121.5(3) . . ?
C23 C22 H22 119.5(19) . . ?
C21 C22 H22 118.9(19) . . ?
O3 C23 C22 125.5(3) . . ?
O3 C23 C24 115.1(2) . . ?
C22 C23 C24 119.4(3) . . ?
O4 C24 C25 125.3(3) . . ?
O4 C24 C23 115.1(3) . . ?
C25 C24 C23 119.6(3) . . ?
C24 C25 C26 121.5(3) . . ?
C24 C25 H25 118(2) . . ?
C26 C25 H25 120(2) . . ?
C25 C26 C21 119.1(3) . . ?
C25 C26 C16 121.9(3) . . ?
C21 C26 C16 119.0(3) . . ?
O3 C27 H27A 111.8(19) . . ?
O3 C27 H27B 109.5(18) . . ?
H27A C27 H27B 114(3) . . ?
O3 C27 H27C 104.5(19) . . ?
H27A C27 H27C 108(3) . . ?
H27B C27 H27C 109(3) . . ?
O4 C28 H28A 102(2) . . ?
O4 C28 H28B 111(2) . . ?
H28A C28 H28B 116(3) . . ?
O4 C28 H28C 112(2) . . ?
H28A C28 H28C 108(3) . . ?
H28B C28 H28C 108(3) . . ?
C36 C31 C32 118.6(3) . . ?
C36 C31 C1 119.7(3) . . ?
C32 C31 C1 121.5(3) . . ?
C33 C32 C31 121.6(3) . . ?
C33 C32 H32 118(2) . . ?
C31 C32 H32 120(2) . . ?
C32 C33 O5 126.0(3) . . ?
C32 C33 C34 119.6(3) . . ?
O5 C33 C34 114.4(3) . . ?
O6 C34 C35 125.4(3) . . ?
O6 C34 C33 115.3(2) . . ?
C35 C34 C33 119.3(3) . . ?
C34 C35 C36 122.0(3) . . ?
C34 C35 H35 117.4(18) . . ?
C36 C35 H35 120.5(18) . . ?
C35 C36 C31 118.7(3) . . ?
C35 C36 C46 121.7(3) . . ?
C31 C36 C46 119.5(3) . . ?
O5 C37 H37A 107.3(19) . . ?
O5 C37 H37B 112(2) . . ?
H37A C37 H37B 113(3) . . ?
O5 C37 H37C 109(2) . . ?
H37A C37 H37C 105(3) . . ?
H37B C37 H37C 111(3) . . ?
O6 C38 H38A 104.5(18) . . ?
O6 C38 H38B 108(2) . . ?
H38A C38 H38B 114(3) . . ?
O6 C38 H38C 108.3(19) . . ?
H38A C38 H38C 109(3) . . ?
H38B C38 H38C 113(3) . . ?
C46 C41 C42 119.0(3) . . ?
C46 C41 C2 119.9(3) . . ?
C42 C41 C2 121.0(3) . . ?
C43 C42 C41 121.4(3) . . ?
C43 C42 H42 121(2) . . ?
C41 C42 H42 118(2) . . ?
O7 C43 C42 125.3(3) . . ?
O7 C43 C44 115.3(2) . . ?
C42 C43 C44 119.3(3) . . ?
O8 C44 C45 125.6(3) . . ?
O8 C44 C43 114.6(2) . . ?
C45 C44 C43 119.8(3) . . ?
C44 C45 C46 121.4(3) . . ?
C44 C45 H45 117.4(18) . . ?
C46 C45 H45 121.1(18) . . ?
C45 C46 C41 118.9(3) . . ?
C45 C46 C36 122.3(3) . . ?
C41 C46 C36 118.7(3) . . ?
O7 C47 H47A 111.1(17) . . ?
O7 C47 H47B 104.6(19) . . ?
H47A C47 H47B 111(3) . . ?
O7 C47 H47C 111(2) . . ?
H47A C47 H47C 112(3) . . ?
H47B C47 H47C 108(3) . . ?
O8 C48 H48A 110(2) . . ?
O8 C48 H48B 105(2) . . ?
H48A C48 H48B 110(3) . . ?
O8 C48 H48C 110(2) . . ?
H48A C48 H48C 112(3) . . ?
H48B C48 H48C 110(3) . . ?
Cl1S C1S Cl2S 111.3(2) . . ?
Cl1S C1S H1SA 109.4 . . ?
Cl2S C1S H1SA 109.4 . . ?
Cl1S C1S H1SB 109.4 . . ?
Cl2S C1S H1SB 109.4 . . ?
H1SA C1S H1SB 108.0 . . ?
C2SA Cl4A Cl4A 140.4(3) . 2_775 ?
Cl4A C2SA Cl3A 112.9(4) . . ?
Cl4A C2SA H2S1 109.0 . . ?
Cl3A C2SA H2S1 109.0 . . ?
Cl4A C2SA H2S2 109.0 . . ?
Cl3A C2SA H2S2 109.0 . . ?
H2S1 C2SA H2S2 107.8 . . ?
Cl4B C2SB Cl3B 113.9(6) . . ?
Cl4B C2SB H2S3 108.8 . . ?
Cl3B C2SB H2S3 108.8 . . ?
Cl4B C2SB H2S4 108.8 . . ?
Cl3B C2SB H2S4 108.8 . . ?
H2S3 C2SB H2S4 107.7 . . ?

_diffrn_measured_fraction_theta_max 0.937
_diffrn_reflns_theta_full        62.76
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.703
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.072

# start Validation Reply Form
_vrf_PLAT222_ALERT_3_B           
;
PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 4.40 Ratio
RESPONSE: The large ratio between temperature parameters of hydrogen
atoms is caused by large rotational motion/disorder of methyl
hydrogens as opposed to aryl hydrogens
;
# end Validation Reply Form


# Attachment 'raj2z.cif'

data_raj2z
_database_code_depnum_ccdc_archive 'CCDC 720097'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C43 H46 Cl2 N4 O8'
_chemical_formula_weight         817.74

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'
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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'

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

_cell_length_a                   31.6750(8)
_cell_length_b                   7.3983(2)
_cell_length_c                   18.0078(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.7180(10)
_cell_angle_gamma                90.00
_cell_volume                     4041.60(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9856
_cell_measurement_theta_min      3
_cell_measurement_theta_max      61

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1720
_exptl_absorpt_coefficient_mu    1.930
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6440
_exptl_absorpt_correction_T_max  0.8609
_exptl_absorpt_process_details   
;
SADABS. Program for empirical absorption correction of
area-detector data. University of Goetingen. Germany.
Sheldrick, G. M. 1996
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX2 CCD detector'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6231
_diffrn_reflns_av_R_equivalents  0.0174
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.91
_diffrn_reflns_theta_max         62.57
_reflns_number_total             3114
_reflns_number_gt                2485
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 v2.0-2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT v7.23A (Bruker, 2005)'
_computing_data_reduction        'TWINABS v1.05 (Bruker, 2005)'
_computing_structure_solution    'XS/SHELXTL v6.12 (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 v.97-2 (Sheldrick, 1993-1997)'
_computing_molecular_graphics    'XP v5.1 (Bruker, 1998)'
_computing_publication_material  'XCIF v6.12 (Bruker, 2001)'

_refine_special_details          
;
Solvate molecule of CH2Cl2 is apparently disordered over 4 positions
near to 2-fold axis. Positions of Cl atoms were combined and H atoms
were not localized
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1494P)^2^+12.3856P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3114
_refine_ls_number_parameters     342
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0944
_refine_ls_R_factor_gt           0.0817
_refine_ls_wR_factor_ref         0.2397
_refine_ls_wR_factor_gt          0.2344
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.066
_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
O1 O 0.65092(9) 0.0309(4) 0.18714(16) 0.0196(7) Uani 1 1 d . . .
O2 O 0.61187(8) 0.0784(3) 0.04231(13) 0.0210(6) Uani 1 1 d . . .
O3 O 0.34846(11) 0.4991(3) 0.03656(18) 0.0235(9) Uani 1 1 d . . .
O4 O 0.38515(8) 0.4336(4) -0.07103(13) 0.0203(6) Uani 1 1 d . . .
C1 C 0.47670(12) 0.2680(4) 0.2381(2) 0.0164(8) Uani 1 1 d . . .
C11 C 0.54544(11) 0.2275(4) 0.20279(19) 0.0168(8) Uani 1 1 d . . .
C12 C 0.58874(11) 0.1564(5) 0.22445(19) 0.0171(8) Uani 1 1 d . . .
H12 H 0.6038 0.1425 0.2780 0.021 Uiso 1 1 calc R . .
C13 C 0.60953(11) 0.1070(5) 0.1707(2) 0.0182(8) Uani 1 1 d . . .
C14 C 0.58742(11) 0.1260(5) 0.09038(19) 0.0176(8) Uani 1 1 d . . .
C15 C 0.54443(11) 0.1855(4) 0.06804(19) 0.0165(8) Uani 1 1 d . . .
H15 H 0.5292 0.1940 0.0144 0.020 Uiso 1 1 calc R . .
C16 C 0.52229(11) 0.2345(4) 0.12326(19) 0.0156(8) Uani 1 1 d . . .
C17 C 0.67257(18) -0.0043(6) 0.2678(3) 0.0341(14) Uani 1 1 d . . .
C18 C 0.59245(14) 0.1055(6) -0.0388(2) 0.0216(8) Uani 1 1 d . . .
C21 C 0.45381(11) 0.3050(4) 0.15784(19) 0.0162(8) Uani 1 1 d . . .
C22 C 0.41049(11) 0.3763(5) 0.13612(19) 0.0177(8) Uani 1 1 d . . .
H22 H 0.3959 0.3937 0.1748 0.021 Uiso 1 1 calc R . .
C23 C 0.38907(11) 0.4210(4) 0.06088(19) 0.0169(8) Uani 1 1 d . . .
C24 C 0.41014(11) 0.3931(5) 0.00224(19) 0.0175(8) Uani 1 1 d . . .
C25 C 0.45328(11) 0.3345(4) 0.02240(18) 0.0170(8) Uani 1 1 d . . .
H25 H 0.4678 0.3220 -0.0167 0.020 Uiso 1 1 calc R . .
C26 C 0.47651(11) 0.2925(4) 0.10045(19) 0.0164(8) Uani 1 1 d . . .
C27 C 0.32658(15) 0.5317(7) 0.0942(3) 0.0231(9) Uani 1 1 d . . .
C28 C 0.40299(13) 0.3859(5) -0.1329(2) 0.0211(8) Uani 1 1 d . . .
H17A H 0.6825(19) 0.110(8) 0.295(3) 0.062(17) Uiso 1 1 d . . .
H17B H 0.6522(14) -0.077(6) 0.291(2) 0.026(10) Uiso 1 1 d . . .
H17C H 0.7022(18) -0.070(8) 0.269(3) 0.055(14) Uiso 1 1 d . . .
H18A H 0.5851(14) 0.236(6) -0.053(2) 0.033(11) Uiso 1 1 d . . .
H18B H 0.6144(15) 0.080(6) -0.060(2) 0.030(11) Uiso 1 1 d . . .
H18C H 0.5680(19) 0.038(7) -0.056(3) 0.038(13) Uiso 1 1 d . . .
H27A H 0.3195(15) 0.425(7) 0.121(3) 0.035(12) Uiso 1 1 d . . .
H27B H 0.2999(13) 0.593(5) 0.068(2) 0.017(9) Uiso 1 1 d . . .
H27C H 0.3426(16) 0.626(7) 0.131(3) 0.045(13) Uiso 1 1 d . . .
H28A H 0.4148(13) 0.249(6) -0.128(2) 0.021(10) Uiso 1 1 d . . .
H28B H 0.3799(14) 0.408(6) -0.177(3) 0.030(11) Uiso 1 1 d . . .
H28C H 0.4288(15) 0.463(6) -0.131(2) 0.019(10) Uiso 1 1 d . . .
N1S N 0.29120(15) 0.9774(5) 0.5434(3) 0.0389(11) Uani 1 1 d . . .
C1S C 0.29191(12) 0.9066(5) 0.4884(2) 0.0254(9) Uani 1 1 d . . .
C2S C 0.29351(15) 0.8180(6) 0.4177(2) 0.0273(9) Uani 1 1 d . . .
H2A H 0.2664(13) 0.822(5) 0.381(2) 0.058(18) Uiso 1 1 d . . .
H2B H 0.316(2) 0.869(8) 0.405(3) 0.065(17) Uiso 1 1 d . . .
H2C H 0.3010(19) 0.699(9) 0.423(3) 0.059(16) Uiso 1 1 d . . .
N2S N 0.70859(15) 0.5062(5) 0.7498(3) 0.0384(13) Uani 1 1 d . . .
C3S C 0.70956(12) 0.5869(5) 0.6953(2) 0.0262(9) Uani 1 1 d . . .
C4S C 0.71225(15) 0.6886(6) 0.6276(2) 0.0283(9) Uani 1 1 d . . .
H4A H 0.6863(17) 0.699(6) 0.598(3) 0.035(13) Uiso 1 1 d . . .
H4B H 0.7344(15) 0.629(6) 0.601(3) 0.038(12) Uiso 1 1 d . . .
H4C H 0.719(2) 0.802(10) 0.637(4) 0.09(2) Uiso 1 1 d . . .
Cl1 Cl 0.54735(11) 0.7625(4) 0.27085(17) 0.0685(9) Uani 0.50 1 d P . .
C5S C 0.5057(8) 0.759(2) 0.2173(14) 0.030(4) Uiso 0.25 1 d P . .
Cl2 Cl 0.50396(13) 0.7611(5) 0.1725(2) 0.0814(11) Uani 0.50 1 d P . .
C6S C 0.4855(11) 0.772(3) 0.2125(17) 0.058(7) Uiso 0.25 1 d P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0130(15) 0.0295(13) 0.0155(15) -0.0018(11) 0.0029(11) 0.0004(11)
O2 0.0209(13) 0.0283(16) 0.0155(13) -0.0026(10) 0.0081(10) 0.0017(11)
O3 0.0206(19) 0.035(2) 0.0149(17) 0.0029(8) 0.0049(14) 0.0053(9)
O4 0.0209(14) 0.0269(15) 0.0126(13) 0.0044(11) 0.0039(10) 0.0032(11)
C1 0.0214(18) 0.0129(16) 0.0165(18) 0.0003(13) 0.0080(15) -0.0031(14)
C11 0.0177(18) 0.0174(17) 0.0179(18) -0.0008(13) 0.0093(14) -0.0028(13)
C12 0.0154(17) 0.0215(18) 0.0137(16) -0.0002(14) 0.0031(13) -0.0010(14)
C13 0.0142(17) 0.0194(17) 0.0204(18) 0.0001(14) 0.0039(14) -0.0023(14)
C14 0.0213(18) 0.0172(17) 0.0170(17) -0.0029(13) 0.0096(14) -0.0030(14)
C15 0.0171(18) 0.0174(17) 0.0136(16) -0.0011(13) 0.0023(13) -0.0029(14)
C16 0.0162(17) 0.0154(16) 0.0164(18) 0.0009(13) 0.0069(14) -0.0028(13)
C17 0.018(3) 0.062(4) 0.021(3) 0.0070(17) 0.003(2) 0.0107(17)
C18 0.027(2) 0.025(2) 0.0157(18) -0.0022(15) 0.0100(16) -0.0012(17)
C21 0.0151(17) 0.0177(17) 0.0163(17) -0.0015(13) 0.0054(14) -0.0038(13)
C22 0.0184(18) 0.0196(17) 0.0166(17) 0.0005(14) 0.0073(14) -0.0026(14)
C23 0.0175(18) 0.0120(19) 0.0200(18) 0.0002(13) 0.0035(14) -0.0021(13)
C24 0.0174(17) 0.0182(16) 0.0152(17) 0.0014(13) 0.0022(14) -0.0015(14)
C25 0.0191(18) 0.0183(17) 0.0147(17) -0.0009(13) 0.0069(14) -0.0057(14)
C26 0.0141(17) 0.0180(17) 0.0168(18) -0.0010(13) 0.0038(14) -0.0046(13)
C27 0.018(2) 0.0324(19) 0.020(2) 0.0007(19) 0.0077(19) 0.0036(19)
C28 0.025(2) 0.0248(19) 0.0134(18) 0.0017(14) 0.0061(16) -0.0002(17)
N1S 0.040(3) 0.048(2) 0.030(3) -0.0056(17) 0.011(2) 0.0048(17)
C1S 0.0187(19) 0.030(2) 0.028(2) 0.0057(17) 0.0086(15) -0.0007(15)
C2S 0.030(2) 0.027(2) 0.026(2) 0.0057(17) 0.0113(19) 0.0042(18)
N2S 0.030(3) 0.055(3) 0.033(3) 0.0022(15) 0.013(2) -0.0030(14)
C3S 0.0200(19) 0.030(2) 0.028(2) -0.0079(17) 0.0050(16) 0.0020(15)
C4S 0.029(2) 0.031(2) 0.023(2) -0.0018(17) 0.0040(18) 0.0012(18)
Cl1 0.080(2) 0.0718(19) 0.0569(18) -0.0064(14) 0.0256(16) -0.0149(16)
Cl2 0.099(3) 0.074(2) 0.072(2) -0.0032(17) 0.025(2) -0.0222(18)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C13 1.378(4) . ?
O1 C17 1.441(6) . ?
O2 C14 1.363(4) . ?
O2 C18 1.426(4) . ?
O3 C23 1.362(5) . ?
O3 C27 1.426(5) . ?
O4 C24 1.363(4) . ?
O4 C28 1.432(4) . ?
C1 C1 1.414(7) 2_655 ?
C1 C21 1.445(5) . ?
C1 C11 1.464(5) 2_655 ?
C11 C16 1.410(5) . ?
C11 C12 1.415(5) . ?
C11 C1 1.464(5) 2_655 ?
C12 C13 1.367(5) . ?
C13 C14 1.421(5) . ?
C14 C15 1.377(5) . ?
C15 C16 1.419(5) . ?
C16 C26 1.453(5) . ?
C21 C22 1.416(5) . ?
C21 C26 1.422(5) . ?
C22 C23 1.370(5) . ?
C23 C24 1.417(5) . ?
C24 C25 1.379(5) . ?
C25 C26 1.421(5) . ?
N1S C1S 1.126(6) . ?
C1S C2S 1.447(6) . ?
N2S C3S 1.156(6) . ?
C3S C4S 1.457(6) . ?
Cl1 C6S 1.17(3) 2_655 ?
Cl1 C5S 1.39(2) . ?
Cl1 C5S 1.75(3) 2_655 ?
Cl1 Cl2 1.904(5) . ?
Cl1 C6S 1.94(3) . ?
Cl1 Cl2 2.153(5) 2_655 ?
C5S C6S 0.63(3) . ?
C5S Cl2 0.79(2) . ?
C5S C6S 1.22(3) 2_655 ?
C5S C5S 1.33(5) 2_655 ?
C5S Cl1 1.75(3) 2_655 ?
C5S Cl2 2.09(3) 2_655 ?
Cl2 C6S 1.05(3) . ?
Cl2 C6S 2.00(3) 2_655 ?
Cl2 C5S 2.09(3) 2_655 ?
Cl2 Cl1 2.153(5) 2_655 ?
C6S Cl1 1.17(3) 2_655 ?
C6S C5S 1.22(3) 2_655 ?
C6S C6S 1.40(6) 2_655 ?
C6S Cl2 2.00(3) 2_655 ?

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
C13 O1 C17 116.0(3) . . ?
C14 O2 C18 117.2(3) . . ?
C23 O3 C27 116.7(3) . . ?
C24 O4 C28 116.8(3) . . ?
C1 C1 C21 118.9(4) 2_655 . ?
C1 C1 C11 117.2(4) 2_655 2_655 ?
C21 C1 C11 124.0(3) . 2_655 ?
C16 C11 C12 118.3(3) . . ?
C16 C11 C1 120.9(3) . 2_655 ?
C12 C11 C1 120.3(3) . 2_655 ?
C13 C12 C11 122.0(3) . . ?
C12 C13 O1 125.4(3) . . ?
C12 C13 C14 119.8(3) . . ?
O1 C13 C14 114.7(3) . . ?
O2 C14 C15 126.3(3) . . ?
O2 C14 C13 114.7(3) . . ?
C15 C14 C13 119.0(3) . . ?
C14 C15 C16 121.6(3) . . ?
C11 C16 C15 119.0(3) . . ?
C11 C16 C26 118.9(3) . . ?
C15 C16 C26 122.1(3) . . ?
C22 C21 C26 118.4(3) . . ?
C22 C21 C1 121.0(3) . . ?
C26 C21 C1 120.1(3) . . ?
C23 C22 C21 121.9(3) . . ?
O3 C23 C22 125.0(3) . . ?
O3 C23 C24 115.2(3) . . ?
C22 C23 C24 119.7(3) . . ?
O4 C24 C25 125.4(3) . . ?
O4 C24 C23 115.0(3) . . ?
C25 C24 C23 119.5(3) . . ?
C24 C25 C26 121.4(3) . . ?
C25 C26 C21 118.6(3) . . ?
C25 C26 C16 122.3(3) . . ?
C21 C26 C16 119.1(3) . . ?
N1S C1S C2S 178.8(5) . . ?
N2S C3S C4S 178.2(4) . . ?
C6S Cl1 C5S 56.0(12) 2_655 . ?
C6S Cl1 C5S 8.7(18) 2_655 2_655 ?
C5S Cl1 C5S 48.3(17) . 2_655 ?
C6S Cl1 Cl2 77.3(14) 2_655 . ?
C5S Cl1 Cl2 21.4(10) . . ?
C5S Cl1 Cl2 69.7(8) 2_655 . ?
C6S Cl1 C6S 46(2) 2_655 . ?
C5S Cl1 C6S 10.7(15) . . ?
C5S Cl1 C6S 38.1(10) 2_655 . ?
Cl2 Cl1 C6S 31.8(9) . . ?
C6S Cl1 Cl2 13.2(14) 2_655 2_655 ?
C5S Cl1 Cl2 68.6(11) . 2_655 ?
C5S Cl1 Cl2 20.3(7) 2_655 2_655 ?
Cl2 Cl1 Cl2 90.0(2) . 2_655 ?
C6S Cl1 Cl2 58.3(9) . 2_655 ?
C6S C5S Cl2 95(4) . . ?
C6S C5S C6S 93(5) . 2_655 ?
Cl2 C5S C6S 170(4) . 2_655 ?
C6S C5S C5S 66(4) . 2_655 ?
Cl2 C5S C5S 161(4) . 2_655 ?
C6S C5S C5S 28.1(16) 2_655 2_655 ?
C6S C5S Cl1 145(5) . . ?
Cl2 C5S Cl1 119(3) . . ?
C6S C5S Cl1 53(2) 2_655 . ?
C5S C5S Cl1 80(2) 2_655 . ?
C6S C5S Cl1 16(4) . 2_655 ?
Cl2 C5S Cl1 110(2) . 2_655 ?
C6S C5S Cl1 79(2) 2_655 2_655 ?
C5S C5S Cl1 51.4(17) 2_655 2_655 ?
Cl1 C5S Cl1 131.7(17) . 2_655 ?
C6S C5S Cl2 73(4) . 2_655 ?
Cl2 C5S Cl2 168(2) . 2_655 ?
C6S C5S Cl2 21(2) 2_655 2_655 ?
C5S C5S Cl2 7.1(14) 2_655 2_655 ?
Cl1 C5S Cl2 73.2(10) . 2_655 ?
Cl1 C5S Cl2 58.5(7) 2_655 2_655 ?
C5S Cl2 C6S 36.5(17) . . ?
C5S Cl2 Cl1 39.9(18) . . ?
C6S Cl2 Cl1 76.0(18) . . ?
C5S Cl2 C6S 6(2) . 2_655 ?
C6S Cl2 C6S 41(3) . 2_655 ?
Cl1 Cl2 C6S 34.6(9) . 2_655 ?
C5S Cl2 C5S 12(2) . 2_655 ?
C6S Cl2 C5S 25(2) . 2_655 ?
Cl1 Cl2 C5S 51.8(6) . 2_655 ?
C6S Cl2 C5S 17.4(8) 2_655 2_655 ?
C5S Cl2 Cl1 50.2(18) . 2_655 ?
C6S Cl2 Cl1 14.7(17) . 2_655 ?
Cl1 Cl2 Cl1 90.0(2) . 2_655 ?
C6S Cl2 Cl1 55.5(10) 2_655 2_655 ?
C5S Cl2 Cl1 38.2(6) 2_655 2_655 ?
C5S C6S Cl2 49(3) . . ?
C5S C6S Cl1 155(5) . 2_655 ?
Cl2 C6S Cl1 152(3) . 2_655 ?
C5S C6S C5S 86(5) . 2_655 ?
Cl2 C6S C5S 134(4) . 2_655 ?
Cl1 C6S C5S 71(2) 2_655 2_655 ?
C5S C6S C6S 61(4) . 2_655 ?
Cl2 C6S C6S 109(4) . 2_655 ?
Cl1 C6S C6S 98(3) 2_655 2_655 ?
C5S C6S C6S 26.6(16) 2_655 2_655 ?
C5S C6S Cl1 24(3) . . ?
Cl2 C6S Cl1 72.3(19) . . ?
Cl1 C6S Cl1 134(2) 2_655 . ?
C5S C6S Cl1 63(2) 2_655 . ?
C6S C6S Cl1 37(2) 2_655 . ?
C5S C6S Cl2 90(4) . 2_655 ?
Cl2 C6S Cl2 138(3) . 2_655 ?
Cl1 C6S Cl2 68.0(14) 2_655 2_655 ?
C5S C6S Cl2 4.1(15) 2_655 2_655 ?
C6S C6S Cl2 29.8(19) 2_655 2_655 ?
Cl1 C6S Cl2 66.2(9) . 2_655 ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        62.57
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.506
_refine_diff_density_min         -0.612
_refine_diff_density_rms         0.093