Supplementary Material (ESI) for Chemical Communications
This journal is © The Royal Society of Chemistry 2001

data_new 
_database_code_CSD                  161379

_journal_coden_Cambridge      182

_publ_requested_journal       'Chemical Communications'

loop_
_publ_author_name
'Bing-guang, Zhang'
'Cheng, He'
'Chun-hua, Yan'
'Chun-ying, Duan'
'Hong, Mo'
'Qing-jin, Meng'
'Zhe-ming, Wang'

_publ_contact_author_name     	'Dr Duan Chun-ying'  
_publ_contact_author_address 
;
Dr Duan Chun-ying
Coordination Chemistry Institute
State Key Laboratory of Coordination Chemistry
Nanjing University
Nanjing
210093
CHINA
;

_publ_contact_author_email       'DUANCY@NJU.EDU.CN'




_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
'C36 H79 Cl3 N16 O14' 
_chemical_formula_weight          1066.50 

loop_ 
_atom_type_symbol 
_atom_type_description 
_atom_type_scat_dispersion_real 
_atom_type_scat_dispersion_imag 
_atom_type_scat_source 
'C'  'C'   0.0033   0.0016 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'H'  'H'   0.0000   0.0000 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'N'  'N'   0.0061   0.0033 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'O'  'O'   0.0106   0.0060 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'Cl'  'Cl'   0.1484   0.1585 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 

_symmetry_cell_setting            monoclinic 
_symmetry_space_group_name_H-M    P2(1) 

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

_cell_length_a                    11.483(2) 
_cell_length_b                    16.512(3) 
_cell_length_c                    13.051(3) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  94.82(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      2465.8(9) 
_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        'block' 
_exptl_crystal_colour             'pale-yellow' 
_exptl_crystal_size_max           0.4 
_exptl_crystal_size_mid           0.3 
_exptl_crystal_size_min           0.3 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.436 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1140 
_exptl_absorpt_coefficient_mu     0.265 
_exptl_absorpt_correction_type    none 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
_exptl_absorpt_process_details    ? 

_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'NONIUS KappaCCD' 
_diffrn_measurement_method        'CCD' 
_diffrn_detector_area_resol_mean  0.76 
_diffrn_reflns_number             49970 
_diffrn_reflns_av_R_equivalents   0.0527 
_diffrn_reflns_av_sigmaI/netI     0.1150 
_diffrn_reflns_limit_h_min        -15 
_diffrn_reflns_limit_h_max        14 
_diffrn_reflns_limit_k_min        -21 
_diffrn_reflns_limit_k_max        21 
_diffrn_reflns_limit_l_min        -17 
_diffrn_reflns_limit_l_max        17 
_diffrn_reflns_theta_min          3.47 
_diffrn_reflns_theta_max          27.90 
_reflns_number_total              11638 
_reflns_number_gt                 5921 
_reflns_threshold_expression      >2sigma(I) 


_computing_data_collection        'KappaCCD (Nonius B. V., 1998)' 
_computing_cell_refinement        'HKL Scalepack (Otwinowski & Minor, 1997)' 
_computing_data_reduction
'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'Bruker SHELXTL V5.1 (Sheldrick, 1998)' 
_computing_publication_material   'SHELXL-97 (Sheldrick, 1997)' 

_publ_section_references
;
collect:
"Collect" data collection software, Nonius B.V., Delft, The Netherlands, 1998.

HKL Scalepack & HKL Denzo:
Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected
in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular
Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R.M. Sweet,
Eds., Academic Press.

maXus: 
S.Mackay, C.J.Gilmore, C.Edwards, M. Tremayne, N. Stuart, K.Shankland
maXus: a computer program for the solution and refinement of crystal
structures from diffraction data", University of Glasgow, Scotland, UK,
Nonius BV, Delft, The Netherlands and MacScience Co. Ltd., Yokohama,
Japan (1998).

Sheldrick, G. M. (1998). SHELXTL Version 5.1. Bruker Analytical X-ray
Instruments Inc., Madison, Wisconsin, USA.

Sheldrick, G. M. (1997). SHELX-97. PC Version. University of Goettingen,
Germany.
; 
_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^)+(0.0850P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.054(4) 
_refine_ls_extinction_expression 
'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_abs_structure_details 
'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.16(8) 
_refine_ls_number_reflns          11638 
_refine_ls_number_parameters      705 
_refine_ls_number_restraints      340 
_refine_ls_R_factor_all           0.1310 
_refine_ls_R_factor_gt            0.0735 
_refine_ls_wR_factor_ref          0.1902 
_refine_ls_wR_factor_gt           0.1759 
_refine_ls_goodness_of_fit_ref    1.059 
_refine_ls_restrained_S_all       1.218 
_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 
O1W O 0.7318(3) 1.0888(2) 0.3392(3) 0.0592(9) Uani 1 1 d . . . 
H1WA H 0.7942 1.0774 0.3919 0.071 Uiso 1 1 d R . . 
H1WB H 0.7376 1.0506 0.2833 0.071 Uiso 1 1 d R . . 
O2W O 0.7751(3) 0.9924(2) 0.1678(3) 0.0590(9) Uani 1 1 d . . . 
H2WA H 0.7326 1.0158 0.1075 0.071 Uiso 1 1 d R . . 
H2WB H 0.7476 0.9372 0.1742 0.071 Uiso 1 1 d R . . 
N1 N 0.6895(4) 0.9722(3) 0.5295(4) 0.0687(13) Uani 1 1 d . . . 
N2 N 0.9206(4) 1.0515(3) 0.5051(4) 0.0683(13) Uani 1 1 d . . . 
N3 N 1.0796(4) 1.0838(3) 0.3991(4) 0.0696(14) Uani 1 1 d . . . 
N4 N 0.9349(4) 1.1836(3) 0.4342(4) 0.0662(13) Uani 1 1 d . . . 
N5 N 0.5127(4) 1.0865(3) 0.4253(4) 0.0622(12) Uani 1 1 d . . . 
H5C H 0.5770 1.0673 0.3970 0.075 Uiso 1 1 calc R . . 
N6 N 0.5134(4) 1.1922(3) 0.3034(4) 0.0718(14) Uani 1 1 d . . . 
N7 N 0.4028(4) 1.0720(3) 0.2595(4) 0.0738(15) Uani 1 1 d . . . 
N8 N 0.7530(7) 0.8091(4) 0.3448(4) 0.0957(18) Uani 1 1 d . . . 
N9 N 0.7004(4) 0.8304(3) 0.1625(3) 0.0575(11) Uani 1 1 d . . . 
N10 N 0.9011(5) 0.8350(3) 0.2250(4) 0.0774(15) Uani 1 1 d . . . 
N11 N 0.7458(4) 1.2637(3) 0.2811(4) 0.0637(12) Uani 1 1 d . . . 
H11C H 0.7408 1.2114 0.3024 0.076 Uiso 1 1 calc R . . 
N12 N 0.5283(4) 0.9444(3) 0.0563(4) 0.0660(13) Uani 1 1 d . . . 
N13 N 1.0417(4) 0.9728(4) 0.1458(5) 0.0886(19) Uani 1 1 d . . . 
H13N H 0.9632 0.9801 0.1466 0.106 Uiso 1 1 calc R . . 
N14 N 0.7989(6) 1.1962(3) 0.0129(4) 0.0820(16) Uani 1 1 d . . . 
N15 N 0.6830(4) 1.0750(3) -0.0232(4) 0.0629(12) Uani 1 1 d . . . 
N16 N 0.8896(4) 1.0673(3) -0.0091(4) 0.0721(14) Uani 1 1 d . . . 
C1 C 0.7691(6) 1.0007(4) 0.6165(5) 0.0750(17) Uani 1 1 d . . . 
H1A H 0.7608 0.9657 0.6751 0.090 Uiso 1 1 calc R . . 
H1B H 0.7456 1.0548 0.6352 0.090 Uiso 1 1 calc R . . 
C2 C 0.8963(6) 1.0027(5) 0.5949(5) 0.0802(19) Uani 1 1 d . . . 
H2A H 0.9417 1.0240 0.6550 0.096 Uiso 1 1 calc R . . 
H2B H 0.9223 0.9477 0.5844 0.096 Uiso 1 1 calc R . . 
C3 C 0.5648(6) 0.9811(5) 0.5565(5) 0.0809(19) Uani 1 1 d . . . 
H3A H 0.5153 0.9432 0.5161 0.097 Uiso 1 1 calc R . . 
H3B H 0.5602 0.9684 0.6286 0.097 Uiso 1 1 calc R . . 
C4 C 0.5231(6) 1.0641(5) 0.5360(5) 0.087(2) Uani 1 1 d . . . 
H4A H 0.5765 1.1015 0.5730 0.105 Uiso 1 1 calc R . . 
H4B H 0.4473 1.0703 0.5627 0.105 Uiso 1 1 calc R . . 
C5 C 0.7142(6) 0.8892(4) 0.4952(5) 0.0786(18) Uani 1 1 d . . . 
H5A H 0.6482 0.8543 0.5052 0.094 Uiso 1 1 calc R . . 
H5B H 0.7821 0.8678 0.5355 0.094 Uiso 1 1 calc R . . 
C6 C 0.7362(9) 0.8904(4) 0.3850(5) 0.104(3) Uani 1 1 d . . . 
H6A H 0.6705 0.9158 0.3459 0.125 Uiso 1 1 calc R . . 
H6B H 0.8052 0.9227 0.3763 0.125 Uiso 1 1 calc R . . 
C7 C 1.0461(5) 1.0389(4) 0.4844(5) 0.0729(17) Uani 1 1 d . . . 
H7A H 1.0957 1.0544 0.5451 0.087 Uiso 1 1 calc R . . 
H7B H 1.0588 0.9818 0.4721 0.087 Uiso 1 1 calc R . . 
C8 C 1.0555(5) 1.1695(4) 0.4168(5) 0.0746(17) Uani 1 1 d . . . 
H8A H 1.1049 1.1883 0.4760 0.090 Uiso 1 1 calc R . . 
H8B H 1.0750 1.2007 0.3576 0.090 Uiso 1 1 calc R . . 
C9 C 0.9085(5) 1.1399(4) 0.5241(4) 0.0629(14) Uani 1 1 d . . . 
H9A H 0.8294 1.1520 0.5401 0.075 Uiso 1 1 calc R . . 
H9B H 0.9616 1.1561 0.5823 0.075 Uiso 1 1 calc R . . 
C10 C 0.9005(5) 1.2677(4) 0.4322(5) 0.0645(15) Uani 1 1 d . . . 
H10A H 0.9658 1.3001 0.4608 0.077 Uiso 1 1 calc R . . 
H10B H 0.8369 1.2747 0.4760 0.077 Uiso 1 1 calc R . . 
C11 C 0.8617(5) 1.2991(4) 0.3256(4) 0.0703(15) Uani 1 1 d . . . 
H11A H 0.9215 1.2864 0.2798 0.084 Uiso 1 1 calc R . . 
H11B H 0.8546 1.3576 0.3285 0.084 Uiso 1 1 calc R . . 
C12 C 0.6468(5) 1.3112(4) 0.3195(6) 0.0811(18) Uani 1 1 d . . . 
H12A H 0.6561 1.3116 0.3940 0.097 Uiso 1 1 calc R . . 
H12B H 0.6527 1.3667 0.2964 0.097 Uiso 1 1 calc R . . 
C13 C 0.5288(6) 1.2811(4) 0.2868(6) 0.086(2) Uani 1 1 d . . . 
H13A H 0.5116 1.2929 0.2143 0.103 Uiso 1 1 calc R . . 
H13B H 0.4725 1.3103 0.3243 0.103 Uiso 1 1 calc R . . 
C14 C 0.5099(5) 1.1745(4) 0.4115(5) 0.0731(17) Uani 1 1 d . . . 
H14A H 0.4391 1.1966 0.4363 0.088 Uiso 1 1 calc R . . 
H14B H 0.5765 1.1990 0.4505 0.088 Uiso 1 1 calc R . . 
C15 C 0.4085(5) 1.1595(4) 0.2474(6) 0.0777(18) Uani 1 1 d . . . 
H15A H 0.4089 1.1727 0.1750 0.093 Uiso 1 1 calc R . . 
H15B H 0.3398 1.1841 0.2729 0.093 Uiso 1 1 calc R . . 
C16 C 0.4078(5) 1.0511(4) 0.3670(5) 0.0752(17) Uani 1 1 d . . . 
H16A H 0.4097 0.9927 0.3741 0.090 Uiso 1 1 calc R . . 
H16B H 0.3379 1.0708 0.3958 0.090 Uiso 1 1 calc R . . 
C17 C 0.4887(5) 1.0263(4) 0.2035(5) 0.0726(17) Uani 1 1 d . . . 
H17A H 0.5538 1.0617 0.1921 0.087 Uiso 1 1 calc R . . 
H17B H 0.5187 0.9817 0.2462 0.087 Uiso 1 1 calc R . . 
C18 C 0.4399(5) 0.9940(4) 0.1036(5) 0.0758(18) Uani 1 1 d . . . 
H18A H 0.4157 1.0385 0.0582 0.091 Uiso 1 1 calc R . . 
H18B H 0.3718 0.9612 0.1136 0.091 Uiso 1 1 calc R . . 
C19 C 0.5080(5) 0.8575(4) 0.0708(6) 0.0739(17) Uani 1 1 d . . . 
H19A H 0.4526 0.8386 0.0158 0.089 Uiso 1 1 calc R . . 
H19B H 0.4726 0.8500 0.1351 0.089 Uiso 1 1 calc R . . 
C20 C 0.6156(5) 0.8066(4) 0.0726(5) 0.0712(15) Uani 1 1 d . . . 
H20A H 0.6522 0.8137 0.0089 0.085 Uiso 1 1 calc R . . 
H20B H 0.5948 0.7499 0.0785 0.085 Uiso 1 1 calc R . . 
C21 C 0.6786(7) 0.7880(4) 0.2618(5) 0.086(2) Uani 1 1 d . . . 
H21A H 0.5993 0.7996 0.2776 0.104 Uiso 1 1 calc R . . 
H21B H 0.6844 0.7301 0.2513 0.104 Uiso 1 1 calc R . . 
C22 C 0.8246(5) 0.8082(4) 0.1400(4) 0.0707(15) Uani 1 1 d . . . 
H22A H 0.8314 0.7500 0.1316 0.085 Uiso 1 1 calc R . . 
H22B H 0.8444 0.8343 0.0772 0.085 Uiso 1 1 calc R . . 
C23 C 0.8713(9) 0.7931(4) 0.3214(6) 0.113(3) Uani 1 1 d . . . 
H23A H 0.8816 0.7352 0.3136 0.136 Uiso 1 1 calc R . . 
H23B H 0.9248 0.8110 0.3784 0.136 Uiso 1 1 calc R . . 
C24 C 1.0231(8) 0.8251(6) 0.2026(9) 0.121(3) Uani 1 1 d . . . 
H24A H 1.0725 0.8305 0.2663 0.145 Uiso 1 1 calc R . . 
H24B H 1.0334 0.7707 0.1769 0.145 Uiso 1 1 calc R . . 
C25 C 1.0629(6) 0.8826(6) 0.1281(7) 0.100(3) Uani 1 1 d . . . 
H25A H 1.0255 0.8685 0.0610 0.120 Uiso 1 1 calc R . . 
H25B H 1.1462 0.8748 0.1250 0.120 Uiso 1 1 calc R . . 
C26 C 1.0983(5) 0.9998(5) 0.2491(6) 0.102(3) Uani 1 1 d . . . 
H26A H 1.1106 0.9530 0.2937 0.122 Uiso 1 1 calc R . . 
H26B H 1.1740 1.0235 0.2399 0.122 Uiso 1 1 calc R . . 
C27 C 1.0252(5) 1.0597(5) 0.2983(5) 0.089(2) Uani 1 1 d . . . 
H27A H 1.0144 1.1070 0.2545 0.107 Uiso 1 1 calc R . . 
H27B H 0.9489 1.0365 0.3062 0.107 Uiso 1 1 calc R . . 
C28 C 0.7403(6) 1.2654(4) 0.1656(5) 0.0741(17) Uani 1 1 d . . . 
H28A H 0.7714 1.3165 0.1435 0.089 Uiso 1 1 calc R . . 
H28B H 0.6593 1.2619 0.1381 0.089 Uiso 1 1 calc R . . 
C29 C 0.8085(6) 1.1964(4) 0.1224(5) 0.0747(17) Uani 1 1 d . . . 
H29A H 0.8902 1.2012 0.1474 0.090 Uiso 1 1 calc R . . 
H29B H 0.7797 1.1453 0.1469 0.090 Uiso 1 1 calc R . . 
C30 C 0.5373(5) 0.9620(4) -0.0534(4) 0.0703(17) Uani 1 1 d . . . 
H30A H 0.4626 0.9500 -0.0906 0.084 Uiso 1 1 calc R . . 
H30B H 0.5946 0.9256 -0.0788 0.084 Uiso 1 1 calc R . . 
C31 C 0.5707(6) 1.0473(4) -0.0777(5) 0.0745(17) Uani 1 1 d . . . 
H31A H 0.5765 1.0518 -0.1512 0.089 Uiso 1 1 calc R . . 
H31B H 0.5088 1.0834 -0.0599 0.089 Uiso 1 1 calc R . . 
C32 C 1.0805(5) 1.0218(5) 0.0626(6) 0.091(2) Uani 1 1 d . . . 
H32A H 1.1544 1.0004 0.0437 0.110 Uiso 1 1 calc R . . 
H32B H 1.0947 1.0765 0.0879 0.110 Uiso 1 1 calc R . . 
C33 C 0.9960(6) 1.0258(6) -0.0333(6) 0.102(3) Uani 1 1 d . . . 
H33A H 1.0318 1.0548 -0.0872 0.122 Uiso 1 1 calc R . . 
H33B H 0.9773 0.9715 -0.0577 0.122 Uiso 1 1 calc R . . 
C34 C 0.6939(7) 1.1639(4) -0.0351(5) 0.0816(19) Uani 1 1 d . . . 
H34A H 0.6895 1.1768 -0.1079 0.098 Uiso 1 1 calc R . . 
H34B H 0.6283 1.1899 -0.0064 0.098 Uiso 1 1 calc R . . 
C35 C 0.7843(5) 1.0382(4) -0.0654(4) 0.0723(17) Uani 1 1 d . . . 
H35A H 0.7800 0.9797 -0.0598 0.087 Uiso 1 1 calc R . . 
H35B H 0.7850 1.0522 -0.1375 0.087 Uiso 1 1 calc R . . 
C36 C 0.8963(8) 1.1556(5) -0.0274(5) 0.103(3) Uani 1 1 d . . . 
H36A H 0.9689 1.1767 0.0056 0.123 Uiso 1 1 calc R . . 
H36B H 0.8956 1.1659 -0.1006 0.123 Uiso 1 1 calc R . . 
Cl1 Cl 1.14648(10) 1.30175(8) 0.16077(10) 0.0485(3) Uani 1 1 d DU . . 
O11 O 1.2529(6) 1.3342(5) 0.1398(7) 0.183(3) Uani 1 1 d DU A . 
O12 O 1.1419(14) 1.2243(6) 0.1337(8) 0.176(6) Uani 0.50 1 d PDU A 1 
O13 O 1.1575(12) 1.3023(9) 0.2720(6) 0.119(4) Uani 0.50 1 d PDU A 1 
O14 O 1.0510(10) 1.3448(8) 0.1346(10) 0.152(5) Uani 0.50 1 d PDU A 1 
O12' O 1.1493(13) 1.2224(6) 0.1767(8) 0.161(5) Uani 0.50 1 d PDU A 2 
O13' O 1.0608(12) 1.3225(9) 0.0902(10) 0.173(6) Uani 0.50 1 d PDU A 2 
O14' O 1.1233(15) 1.3390(9) 0.2528(9) 0.157(5) Uani 0.50 1 d PDU A 2 
Cl2 Cl 0.33345(10) 0.80698(10) 0.34524(10) 0.0607(4) Uani 1 1 d DU . . 
O21 O 0.2568(7) 0.8574(5) 0.3992(6) 0.170(3) Uani 1 1 d DU B . 
O22 O 0.4465(8) 0.8330(9) 0.3729(12) 0.151(5) Uani 0.50 1 d PDU B 1 
O23 O 0.3092(12) 0.8235(10) 0.2393(7) 0.131(6) Uani 0.50 1 d PDU B 1 
O24 O 0.3067(14) 0.7272(6) 0.3643(11) 0.140(5) Uani 0.50 1 d PDU B 1 
O22' O 0.4404(9) 0.8008(10) 0.3991(12) 0.167(6) Uani 0.50 1 d PDU B 2 
O23' O 0.3432(13) 0.8522(9) 0.2531(8) 0.120(5) Uani 0.50 1 d PDU B 2 
O24' O 0.2712(13) 0.7367(7) 0.3219(11) 0.153(6) Uani 0.50 1 d PDU B 2 
Cl3 Cl 1.24741(14) 1.04859(12) 0.79293(14) 0.0837(5) Uani 1 1 d DU . . 
O31 O 1.1442(5) 1.0837(4) 0.7498(5) 0.138(2) Uani 1 1 d DU C . 
O32 O 1.3445(10) 1.0644(10) 0.7372(11) 0.149(6) Uani 0.50 1 d PDU C 1 
O33 O 1.2705(12) 1.0918(9) 0.8877(8) 0.108(4) Uani 0.50 1 d PDU C 1 
O34 O 1.2322(16) 0.9675(5) 0.8158(13) 0.142(6) Uani 0.50 1 d PDU C 1 
O32' O 1.3187(13) 1.0215(10) 0.7167(11) 0.159(6) Uani 0.50 1 d PDU C 2 
O33' O 1.3074(14) 1.1041(9) 0.8603(11) 0.140(6) Uani 0.50 1 d PDU C 2 
O34' O 1.2224(15) 0.9797(6) 0.8514(11) 0.121(5) Uani 0.50 1 d PDU C 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 
O1W 0.056(2) 0.069(2) 0.052(2) 0.0018(18) 0.0003(16) 0.0003(18) 
O2W 0.061(2) 0.052(2) 0.063(2) -0.0021(18) -0.0032(18) -0.0015(17) 
N1 0.089(3) 0.060(3) 0.055(3) -0.005(2) -0.002(2) -0.008(3) 
N2 0.074(3) 0.064(3) 0.065(3) 0.000(3) -0.003(2) -0.002(3) 
N3 0.056(3) 0.088(4) 0.063(3) -0.024(3) -0.007(2) 0.005(3) 
N4 0.070(3) 0.065(3) 0.063(3) -0.005(2) 0.007(2) -0.005(2) 
N5 0.050(2) 0.070(3) 0.068(3) -0.008(2) 0.015(2) -0.004(2) 
N6 0.065(3) 0.060(3) 0.089(4) 0.000(3) -0.003(3) 0.008(2) 
N7 0.047(2) 0.082(4) 0.093(4) -0.019(3) 0.008(2) 0.003(2) 
N8 0.162(6) 0.060(4) 0.062(3) -0.006(3) -0.013(4) 0.019(4) 
N9 0.069(3) 0.051(3) 0.050(3) -0.0062(19) -0.008(2) 0.000(2) 
N10 0.075(3) 0.067(3) 0.085(4) -0.018(3) -0.027(3) 0.009(2) 
N11 0.072(3) 0.051(3) 0.067(3) 0.002(2) 0.003(2) 0.002(2) 
N12 0.060(3) 0.061(3) 0.075(3) -0.007(3) -0.004(2) 0.000(2) 
N13 0.050(3) 0.108(5) 0.107(5) -0.053(4) 0.000(3) 0.000(3) 
N14 0.131(5) 0.062(3) 0.051(3) 0.009(2) -0.005(3) -0.020(3) 
N15 0.060(3) 0.069(3) 0.057(3) 0.001(2) -0.009(2) -0.001(2) 
N16 0.070(3) 0.085(4) 0.062(3) -0.017(3) 0.012(2) -0.025(3) 
C1 0.092(4) 0.079(4) 0.052(3) 0.004(3) -0.005(3) -0.016(4) 
C2 0.093(5) 0.076(4) 0.069(4) 0.009(3) -0.009(4) -0.009(4) 
C3 0.087(4) 0.085(5) 0.072(4) 0.007(4) 0.014(3) -0.016(4) 
C4 0.084(4) 0.103(6) 0.079(5) -0.022(4) 0.031(4) -0.019(4) 
C5 0.107(5) 0.068(4) 0.059(4) 0.010(3) -0.005(3) -0.005(4) 
C6 0.193(8) 0.060(4) 0.059(4) -0.001(3) 0.008(4) 0.013(5) 
C7 0.060(3) 0.075(4) 0.082(4) -0.008(4) -0.008(3) 0.002(3) 
C8 0.068(4) 0.089(5) 0.068(4) -0.014(3) 0.010(3) -0.014(3) 
C9 0.074(4) 0.060(4) 0.053(3) -0.011(3) -0.002(3) -0.002(3) 
C10 0.074(4) 0.052(3) 0.068(4) -0.011(3) 0.003(3) -0.007(3) 
C11 0.076(3) 0.077(4) 0.057(3) 0.004(3) 0.001(3) -0.023(4) 
C12 0.075(4) 0.052(4) 0.115(5) -0.015(4) 0.004(3) 0.005(3) 
C13 0.093(5) 0.051(4) 0.109(5) 0.000(3) -0.007(4) 0.017(3) 
C14 0.070(4) 0.061(4) 0.091(5) -0.022(3) 0.020(3) -0.001(3) 
C15 0.055(3) 0.070(4) 0.104(5) -0.011(4) -0.017(3) 0.006(3) 
C16 0.063(3) 0.076(4) 0.088(5) -0.022(4) 0.017(3) -0.018(3) 
C17 0.060(3) 0.082(5) 0.074(4) -0.016(3) -0.001(3) 0.007(3) 
C18 0.051(3) 0.084(5) 0.090(5) -0.013(4) -0.009(3) 0.011(3) 
C19 0.054(3) 0.074(4) 0.091(5) 0.002(4) -0.004(3) -0.007(3) 
C20 0.076(3) 0.059(4) 0.078(4) -0.014(4) 0.005(3) 0.008(3) 
C21 0.140(6) 0.051(4) 0.071(4) 0.001(3) 0.023(4) -0.013(4) 
C22 0.074(3) 0.072(4) 0.064(3) -0.010(3) -0.005(3) 0.011(3) 
C23 0.187(9) 0.050(4) 0.089(5) 0.000(4) -0.070(6) 0.023(5) 
C24 0.092(5) 0.102(7) 0.160(9) -0.053(6) -0.037(6) 0.033(5) 
C25 0.057(4) 0.113(7) 0.128(7) -0.062(6) -0.010(4) 0.023(4) 
C26 0.055(3) 0.134(7) 0.111(6) -0.071(5) -0.021(3) 0.018(4) 
C27 0.061(3) 0.118(6) 0.085(5) -0.046(4) -0.010(3) 0.008(4) 
C28 0.092(4) 0.055(4) 0.074(4) 0.008(3) 0.001(3) 0.000(3) 
C29 0.097(4) 0.067(4) 0.058(4) 0.007(3) -0.006(3) -0.001(3) 
C30 0.060(3) 0.084(5) 0.064(4) -0.019(3) -0.010(3) -0.002(3) 
C31 0.079(4) 0.074(4) 0.066(4) 0.008(3) -0.022(3) -0.004(3) 
C32 0.057(4) 0.133(7) 0.086(5) -0.037(5) 0.019(4) -0.022(4) 
C33 0.077(4) 0.147(8) 0.085(5) -0.036(5) 0.026(4) -0.013(5) 
C34 0.111(5) 0.059(4) 0.070(4) 0.010(3) -0.025(4) -0.011(4) 
C35 0.089(4) 0.081(4) 0.047(3) 0.002(3) 0.004(3) -0.015(3) 
C36 0.147(7) 0.105(6) 0.060(4) -0.009(4) 0.027(5) -0.068(6) 
Cl1 0.0503(6) 0.0428(6) 0.0537(7) 0.0177(7) 0.0120(5) -0.0024(6) 
O11 0.154(6) 0.184(8) 0.221(8) -0.016(6) 0.084(6) -0.053(5) 
O12 0.118(8) 0.375(15) 0.027(7) 0.011(9) -0.040(7) -0.018(10) 
O13 0.142(9) 0.135(10) 0.083(7) 0.039(7) 0.018(6) 0.005(8) 
O14 0.226(11) 0.133(10) 0.099(9) 0.001(8) 0.039(9) -0.043(9) 
O12' 0.096(7) 0.344(15) 0.038(8) -0.027(9) -0.027(7) -0.001(9) 
O13' 0.261(13) 0.123(11) 0.139(12) -0.043(9) 0.043(11) 0.004(10) 
O14' 0.183(11) 0.126(11) 0.167(10) -0.013(9) 0.045(9) -0.023(9) 
Cl2 0.0446(6) 0.0819(10) 0.0548(7) 0.0282(8) 0.0000(5) -0.0165(7) 
O21 0.173(7) 0.188(8) 0.152(6) 0.022(6) 0.033(5) -0.024(6) 
O22 0.165(10) 0.113(11) 0.172(12) 0.042(9) -0.002(9) 0.025(8) 
O23 0.081(7) 0.178(13) 0.136(10) 0.055(9) 0.017(7) -0.021(8) 
O24 0.168(11) 0.146(10) 0.097(10) 0.025(8) -0.036(8) -0.024(9) 
O22' 0.177(11) 0.152(12) 0.173(11) 0.100(9) 0.014(9) -0.015(10) 
O23' 0.123(11) 0.150(11) 0.086(7) 0.071(7) 0.013(6) -0.022(8) 
O24' 0.196(13) 0.154(11) 0.108(11) 0.031(9) 0.000(10) 0.020(10) 
Cl3 0.0687(9) 0.0879(12) 0.0941(12) 0.0122(11) 0.0042(8) 0.0005(9) 
O31 0.097(4) 0.163(6) 0.147(5) 0.043(5) -0.036(4) 0.012(4) 
O32 0.100(7) 0.192(14) 0.167(11) 0.008(10) 0.076(8) -0.034(8) 
O33 0.116(8) 0.123(9) 0.089(7) -0.015(7) 0.030(6) -0.010(7) 
O34 0.197(11) 0.063(7) 0.171(13) -0.017(8) 0.055(10) 0.007(8) 
O32' 0.157(11) 0.172(14) 0.162(10) -0.001(10) 0.100(9) 0.014(10) 
O33' 0.146(11) 0.119(10) 0.143(11) -0.007(9) -0.057(10) -0.003(9) 
O34' 0.167(9) 0.076(8) 0.129(10) 0.004(7) 0.072(8) 0.020(7) 

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

loop_ 
_geom_bond_atom_site_label_1 
_geom_bond_atom_site_label_2 
_geom_bond_distance 
_geom_bond_site_symmetry_2 
_geom_bond_publ_flag 
N1 C1 1.473(8) . ? 
N1 C5 1.478(8) . ? 
N1 C3 1.510(8) . ? 
N2 C2 1.469(8) . ? 
N2 C9 1.488(8) . ? 
N2 C7 1.503(7) . ? 
N3 C7 1.417(8) . ? 
N3 C8 1.464(8) . ? 
N3 C27 1.464(8) . ? 
N4 C9 1.432(7) . ? 
N4 C8 1.441(8) . ? 
N4 C10 1.444(8) . ? 
N5 C14 1.464(8) . ? 
N5 C16 1.489(7) . ? 
N5 C4 1.486(8) . ? 
N6 C14 1.445(8) . ? 
N6 C15 1.460(8) . ? 
N6 C13 1.496(8) . ? 
N7 C16 1.442(8) . ? 
N7 C15 1.454(8) . ? 
N7 C17 1.482(7) . ? 
N8 C21 1.367(9) . ? 
N8 C23 1.442(11) . ? 
N8 C6 1.461(9) . ? 
N9 C21 1.511(8) . ? 
N9 C20 1.512(7) . ? 
N9 C22 1.524(7) . ? 
N10 C22 1.426(7) . ? 
N10 C24 1.464(11) . ? 
N10 C23 1.501(10) . ? 
N11 C12 1.501(8) . ? 
N11 C28 1.504(8) . ? 
N11 C11 1.522(7) . ? 
N12 C19 1.468(8) . ? 
N12 C30 1.472(8) . ? 
N12 C18 1.480(7) . ? 
N13 C32 1.453(10) . ? 
N13 C26 1.514(8) . ? 
N13 C25 1.531(10) . ? 
N14 C34 1.417(9) . ? 
N14 C29 1.424(8) . ? 
N14 C36 1.441(10) . ? 
N15 C35 1.459(8) . ? 
N15 C34 1.482(8) . ? 
N15 C31 1.491(7) . ? 
N16 C35 1.443(8) . ? 
N16 C33 1.459(8) . ? 
N16 C36 1.480(10) . ? 
C1 C2 1.511(9) . ? 
C3 C4 1.469(10) . ? 
C5 C6 1.481(9) . ? 
C10 C11 1.517(8) . ? 
C12 C13 1.472(9) . ? 
C17 C18 1.474(9) . ? 
C19 C20 1.493(8) . ? 
C24 C25 1.459(12) . ? 
C26 C27 1.478(9) . ? 
C28 C29 1.517(9) . ? 
C30 C31 1.502(9) . ? 
C32 C33 1.520(10) . ? 
Cl1 O14 1.327(9) . ? 
Cl1 O12' 1.326(9) . ? 
Cl1 O12 1.326(9) . ? 
Cl1 O13' 1.335(9) . ? 
Cl1 O11 1.383(6) . ? 
Cl1 O14' 1.395(9) . ? 
Cl1 O13 1.446(8) . ? 
Cl2 O22' 1.366(9) . ? 
Cl2 O24 1.380(8) . ? 
Cl2 O24' 1.383(8) . ? 
Cl2 O22 1.387(8) . ? 
Cl2 O23 1.414(8) . ? 
Cl2 O23' 1.428(7) . ? 
Cl2 O21 1.438(7) . ? 
Cl3 O34 1.386(8) . ? 
Cl3 O31 1.395(5) . ? 
Cl3 O32 1.406(7) . ? 
Cl3 O33' 1.410(8) . ? 
Cl3 O32' 1.413(8) . ? 
Cl3 O34' 1.413(8) . ? 
Cl3 O33 1.433(7) . ? 

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 
C1 N1 C5 114.1(5) . . ? 
C1 N1 C3 109.2(5) . . ? 
C5 N1 C3 111.7(5) . . ? 
C2 N2 C9 112.2(5) . . ? 
C2 N2 C7 108.5(5) . . ? 
C9 N2 C7 105.7(5) . . ? 
C7 N3 C8 108.3(5) . . ? 
C7 N3 C27 116.1(6) . . ? 
C8 N3 C27 109.5(6) . . ? 
C9 N4 C8 108.7(5) . . ? 
C9 N4 C10 115.0(5) . . ? 
C8 N4 C10 114.7(5) . . ? 
C14 N5 C16 108.6(5) . . ? 
C14 N5 C4 111.5(5) . . ? 
C16 N5 C4 113.2(5) . . ? 
C14 N6 C15 109.0(5) . . ? 
C14 N6 C13 110.7(5) . . ? 
C15 N6 C13 113.2(5) . . ? 
C16 N7 C15 110.2(5) . . ? 
C16 N7 C17 112.6(5) . . ? 
C15 N7 C17 114.5(5) . . ? 
C21 N8 C23 108.8(6) . . ? 
C21 N8 C6 115.2(7) . . ? 
C23 N8 C6 113.6(7) . . ? 
C21 N9 C20 113.8(5) . . ? 
C21 N9 C22 106.2(5) . . ? 
C20 N9 C22 109.9(4) . . ? 
C22 N10 C24 110.4(5) . . ? 
C22 N10 C23 109.8(5) . . ? 
C24 N10 C23 113.9(7) . . ? 
C12 N11 C28 110.8(5) . . ? 
C12 N11 C11 109.6(5) . . ? 
C28 N11 C11 109.7(4) . . ? 
C19 N12 C30 110.1(5) . . ? 
C19 N12 C18 111.4(5) . . ? 
C30 N12 C18 113.8(5) . . ? 
C32 N13 C26 111.4(6) . . ? 
C32 N13 C25 111.5(6) . . ? 
C26 N13 C25 111.0(6) . . ? 
C34 N14 C29 115.9(6) . . ? 
C34 N14 C36 108.7(6) . . ? 
C29 N14 C36 111.7(6) . . ? 
C35 N15 C34 107.2(5) . . ? 
C35 N15 C31 112.2(5) . . ? 
C34 N15 C31 109.3(5) . . ? 
C35 N16 C33 114.5(5) . . ? 
C35 N16 C36 107.4(6) . . ? 
C33 N16 C36 111.8(6) . . ? 
N1 C1 C2 114.2(5) . . ? 
N2 C2 C1 114.3(5) . . ? 
C4 C3 N1 110.4(5) . . ? 
C3 C4 N5 114.1(6) . . ? 
N1 C5 C6 109.5(5) . . ? 
N8 C6 C5 112.0(6) . . ? 
N3 C7 N2 113.4(5) . . ? 
N4 C8 N3 112.1(5) . . ? 
N4 C9 N2 109.1(4) . . ? 
N4 C10 C11 113.8(5) . . ? 
C10 C11 N11 113.5(5) . . ? 
C13 C12 N11 115.6(6) . . ? 
C12 C13 N6 113.9(5) . . ? 
N6 C14 N5 108.6(5) . . ? 
N6 C15 N7 110.9(5) . . ? 
N7 C16 N5 111.6(5) . . ? 
C18 C17 N7 113.7(5) . . ? 
C17 C18 N12 110.3(5) . . ? 
N12 C19 C20 114.3(5) . . ? 
C19 C20 N9 110.1(5) . . ? 
N8 C21 N9 115.1(6) . . ? 
N10 C22 N9 107.5(4) . . ? 
N8 C23 N10 112.2(5) . . ? 
C25 C24 N10 114.8(7) . . ? 
C24 C25 N13 118.0(7) . . ? 
C27 C26 N13 111.5(5) . . ? 
N3 C27 C26 110.9(5) . . ? 
N11 C28 C29 112.3(5) . . ? 
N14 C29 C28 112.0(5) . . ? 
N12 C30 C31 115.5(5) . . ? 
N15 C31 C30 114.4(5) . . ? 
N13 C32 C33 115.1(6) . . ? 
N16 C33 C32 109.3(5) . . ? 
N14 C34 N15 113.8(5) . . ? 
N16 C35 N15 109.3(5) . . ? 
N14 C36 N16 110.3(5) . . ? 
O14 Cl1 O12' 125.3(10) . . ? 
O14 Cl1 O12 115.7(8) . . ? 
O12' Cl1 O12 24.4(6) . . ? 
O14 Cl1 O13' 30.6(8) . . ? 
O12' Cl1 O13' 111.6(8) . . ? 
O12 Cl1 O13' 93.1(9) . . ? 
O14 Cl1 O11 117.8(7) . . ? 
O12' Cl1 O11 113.8(7) . . ? 
O12 Cl1 O11 109.7(8) . . ? 
O13' Cl1 O11 112.1(8) . . ? 
O14 Cl1 O14' 76.8(9) . . ? 
O12' Cl1 O14' 107.7(8) . . ? 
O12 Cl1 O14' 130.4(9) . . ? 
O13' Cl1 O14' 107.3(8) . . ? 
O11 Cl1 O14' 103.7(7) . . ? 
O14 Cl1 O13 104.8(7) . . ? 
O12' Cl1 O13 81.4(7) . . ? 
O12 Cl1 O13 105.8(7) . . ? 
O13' Cl1 O13 133.5(8) . . ? 
O11 Cl1 O13 101.1(6) . . ? 
O14' Cl1 O13 30.7(8) . . ? 
O22' Cl2 O24 92.3(9) . . ? 
O22' Cl2 O24' 118.4(8) . . ? 
O24 Cl2 O24' 28.4(7) . . ? 
O22' Cl2 O22 26.8(8) . . ? 
O24 Cl2 O22 117.8(8) . . ? 
O24' Cl2 O22 140.6(9) . . ? 
O22' Cl2 O23 127.7(9) . . ? 
O24 Cl2 O23 109.4(8) . . ? 
O24' Cl2 O23 83.7(9) . . ? 
O22 Cl2 O23 107.4(8) . . ? 
O22' Cl2 O23' 110.0(7) . . ? 
O24 Cl2 O23' 133.2(9) . . ? 
O24' Cl2 O23' 109.2(8) . . ? 
O22 Cl2 O23' 85.4(9) . . ? 
O23 Cl2 O23' 25.6(9) . . ? 
O22' Cl2 O21 110.6(8) . . ? 
O24 Cl2 O21 108.0(8) . . ? 
O24' Cl2 O21 105.5(7) . . ? 
O22 Cl2 O21 106.9(7) . . ? 
O23 Cl2 O21 106.8(7) . . ? 
O23' Cl2 O21 101.8(7) . . ? 
O34 Cl3 O31 111.7(8) . . ? 
O34 Cl3 O32 114.2(9) . . ? 
O31 Cl3 O32 113.5(7) . . ? 
O34 Cl3 O33' 123.9(12) . . ? 
O31 Cl3 O33' 109.6(7) . . ? 
O32 Cl3 O33' 80.5(10) . . ? 
O34 Cl3 O32' 86.4(10) . . ? 
O31 Cl3 O32' 111.8(8) . . ? 
O32 Cl3 O32' 33.2(8) . . ? 
O33' Cl3 O32' 111.3(9) . . ? 
O34 Cl3 O34' 21.7(11) . . ? 
O31 Cl3 O34' 110.4(8) . . ? 
O32 Cl3 O34' 129.4(10) . . ? 
O33' Cl3 O34' 107.3(8) . . ? 
O32' Cl3 O34' 106.3(8) . . ? 
O34 Cl3 O33 108.2(8) . . ? 
O31 Cl3 O33 103.3(7) . . ? 
O32 Cl3 O33 104.9(7) . . ? 
O33' Cl3 O33 24.8(9) . . ? 
O32' Cl3 O33 133.5(9) . . ? 
O34' Cl3 O33 88.1(10) . . ? 

_diffrn_measured_fraction_theta_max    0.990 
_diffrn_reflns_theta_full              27.90 
_diffrn_measured_fraction_theta_full   0.990 
_refine_diff_density_max    1.036 
_refine_diff_density_min   -0.400 
_refine_diff_density_rms    0.086