 
data_01sot061
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C17.33 H40.67 Cl2.67 N O4 P' 
_chemical_formula_weight          452.68 
 
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' 
 'P'  'P'   0.1023   0.0942 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cl'  'Cl'   0.1484   0.1585 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            Triclinic 
_symmetry_space_group_name_H-M    P-1 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, -z' 
 
_cell_length_a                    16.1733(3) 
_cell_length_b                    17.8443(3) 
_cell_length_c                    26.7000(5) 
_cell_angle_alpha                 77.520(3) 
_cell_angle_beta                  77.237(3) 
_cell_angle_gamma                 83.124(3) 
_cell_volume                      7316.7(2) 
_cell_formula_units_Z             12 
_cell_measurement_temperature     120(2) 
_cell_measurement_reflns_used     242259 
_cell_measurement_theta_min       1.02 
_cell_measurement_theta_max       25.03 
 
_exptl_crystal_description        block 
_exptl_crystal_colour             colourless 
_exptl_crystal_size_max           0.50 
_exptl_crystal_size_mid           0.15 
_exptl_crystal_size_min           0.10 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.233 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              2928 
_exptl_absorpt_coefficient_mu     0.425 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.8155 
_exptl_absorpt_correction_T_max   0.9587 
_exptl_absorpt_process_details    'SORTAV (Blessing, 1997)' 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       120(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'Bruker-Nonius FR591 rotating anode' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Bruker-Nonius KappaCCD' 
_diffrn_measurement_method        'Φ & ω scans' 
_diffrn_detector_area_resol_mean  9.091 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             54851 
_diffrn_reflns_av_R_equivalents   0.0957 
_diffrn_reflns_av_sigmaI/netI     0.1186 
_diffrn_reflns_limit_h_min        -17 
_diffrn_reflns_limit_h_max        17 
_diffrn_reflns_limit_k_min        -19 
_diffrn_reflns_limit_k_max        19 
_diffrn_reflns_limit_l_min        -29 
_diffrn_reflns_limit_l_max        29 
_diffrn_reflns_theta_min          2.92 
_diffrn_reflns_theta_max          23.25 
_reflns_number_total              20248 
_reflns_number_gt                 10118 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'COLLECT (Hooft, 1998)' 
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)'  
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)'  
_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)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     constr 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          20248 
_refine_ls_number_parameters      1417 
_refine_ls_number_restraints      860 
_refine_ls_R_factor_all           0.2638 
_refine_ls_R_factor_gt            0.1694 
_refine_ls_wR_factor_ref          0.4813 
_refine_ls_wR_factor_gt           0.4281 
_refine_ls_goodness_of_fit_ref    1.577 
_refine_ls_restrained_S_all       1.920 
_refine_ls_shift/su_max           3.644 
_refine_ls_shift/su_mean          0.069 
 
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 
N1 N 0.2198(7) 0.5222(6) 0.3026(3) 0.047(3) Uani 1 1 d D . . 
C1 C 0.2036(8) 0.4379(6) 0.3053(5) 0.044(4) Uani 1 1 d D . . 
H1A H 0.1908 0.4331 0.2715 0.053 Uiso 1 1 calc R . . 
H1B H 0.2560 0.4048 0.3102 0.053 Uiso 1 1 calc R . . 
C2 C 0.1315(8) 0.4092(6) 0.3488(5) 0.036(3) Uani 1 1 d D . . 
H2A H 0.0783 0.4412 0.3440 0.043 Uiso 1 1 calc R . . 
H2B H 0.1436 0.4134 0.3829 0.043 Uiso 1 1 calc R . . 
C3 C 0.1204(8) 0.3245(6) 0.3488(6) 0.047(4) Uani 1 1 d D . . 
H3A H 0.1137 0.3201 0.3136 0.057 Uiso 1 1 calc R . . 
H3B H 0.1720 0.2923 0.3565 0.057 Uiso 1 1 calc R . . 
C4 C 0.0429(9) 0.2947(8) 0.3894(5) 0.058(5) Uani 1 1 d D . . 
H4A H 0.0383 0.2407 0.3888 0.086 Uiso 1 1 calc R . . 
H4B H -0.0086 0.3254 0.3812 0.086 Uiso 1 1 calc R . . 
H4C H 0.0493 0.2991 0.4243 0.086 Uiso 1 1 calc R . . 
C5 C 0.1398(8) 0.5739(7) 0.2930(5) 0.042(4) Uani 1 1 d D . . 
H5A H 0.0953 0.5633 0.3251 0.050 Uiso 1 1 calc R . . 
H5B H 0.1531 0.6280 0.2883 0.050 Uiso 1 1 calc R . . 
C6 C 0.1029(10) 0.5674(8) 0.2481(5) 0.064(5) Uani 1 1 d D . . 
H6A H 0.0784 0.5169 0.2557 0.076 Uiso 1 1 calc R . . 
H6B H 0.1491 0.5686 0.2167 0.076 Uiso 1 1 calc R . . 
C7 C 0.0351(10) 0.6298(9) 0.2359(6) 0.075(6) Uani 1 1 d D . . 
H7A H -0.0073 0.6327 0.2685 0.090 Uiso 1 1 calc R . . 
H7B H 0.0057 0.6152 0.2110 0.090 Uiso 1 1 calc R . . 
C8 C 0.0667(13) 0.7094(8) 0.2127(6) 0.086(6) Uani 1 1 d D . . 
H8A H 0.0182 0.7466 0.2070 0.129 Uiso 1 1 calc R . . 
H8B H 0.1062 0.7083 0.1792 0.129 Uiso 1 1 calc R . . 
H8C H 0.0959 0.7248 0.2369 0.129 Uiso 1 1 calc R . . 
C9 C 0.2914(9) 0.5429(8) 0.2553(5) 0.067(5) Uani 1 1 d D . . 
H9A H 0.2771 0.5277 0.2248 0.080 Uiso 1 1 calc R . . 
H9B H 0.3440 0.5119 0.2625 0.080 Uiso 1 1 calc R . . 
C10 C 0.3100(11) 0.6286(9) 0.2400(6) 0.109(9) Uani 1 1 d D . . 
H10A H 0.2618 0.6594 0.2263 0.131 Uiso 1 1 calc R . . 
H10B H 0.3156 0.6468 0.2715 0.131 Uiso 1 1 calc R . . 
C11 C 0.3898(13) 0.6407(13) 0.1994(7) 0.131(11) Uani 1 1 d D . . 
H11A H 0.3935 0.6054 0.1749 0.157 Uiso 1 1 calc R . . 
H11B H 0.3861 0.6940 0.1791 0.157 Uiso 1 1 calc R . . 
C12 C 0.4653(12) 0.628(2) 0.2197(12) 0.209(19) Uani 1 1 d D . . 
H12A H 0.5144 0.6382 0.1908 0.313 Uiso 1 1 calc R . . 
H12B H 0.4709 0.5751 0.2386 0.313 Uiso 1 1 calc R . . 
H12C H 0.4627 0.6635 0.2437 0.313 Uiso 1 1 calc R . . 
C13 C 0.2426(8) 0.5340(7) 0.3513(4) 0.036(3) Uani 1 1 d D . . 
H13A H 0.1925 0.5238 0.3801 0.043 Uiso 1 1 calc R . . 
H13B H 0.2522 0.5892 0.3463 0.043 Uiso 1 1 calc R . . 
C14 C 0.3183(9) 0.4877(8) 0.3695(5) 0.051(4) Uani 1 1 d D . . 
H14A H 0.3706 0.5016 0.3433 0.062 Uiso 1 1 calc R . . 
H14B H 0.3123 0.4323 0.3726 0.062 Uiso 1 1 calc R . . 
C15 C 0.3262(9) 0.5028(8) 0.4230(5) 0.058(5) Uani 1 1 d D . . 
H15A H 0.3293 0.5586 0.4203 0.070 Uiso 1 1 calc R . . 
H15B H 0.2749 0.4867 0.4495 0.070 Uiso 1 1 calc R . . 
C16 C 0.4040(9) 0.4597(9) 0.4406(6) 0.067(5) Uani 1 1 d D . . 
H16A H 0.4075 0.4709 0.4744 0.101 Uiso 1 1 calc R . . 
H16B H 0.4548 0.4758 0.4146 0.101 Uiso 1 1 calc R . . 
H16C H 0.4002 0.4043 0.4443 0.101 Uiso 1 1 calc R . . 
N2 N 0.9857(6) 0.8746(5) 0.4273(4) 0.039(3) Uani 1 1 d D . . 
C17 C 0.9990(8) 0.9612(6) 0.4102(6) 0.047(4) Uani 1 1 d D . . 
H17A H 0.9543 0.9864 0.3908 0.056 Uiso 1 1 calc R . . 
H17B H 0.9913 0.9835 0.4420 0.056 Uiso 1 1 calc R . . 
C18 C 1.0844(9) 0.9803(7) 0.3764(6) 0.059(5) Uani 1 1 d D . . 
H18A H 1.0914 0.9624 0.3430 0.070 Uiso 1 1 calc R . . 
H18B H 1.1302 0.9537 0.3945 0.070 Uiso 1 1 calc R . . 
C19 C 1.0910(9) 1.0681(7) 0.3653(7) 0.060(5) Uani 1 1 d D . . 
H19A H 1.0463 1.0941 0.3462 0.072 Uiso 1 1 calc R . . 
H19B H 1.0810 1.0858 0.3990 0.072 Uiso 1 1 calc R . . 
C20 C 1.1763(9) 1.0903(8) 0.3337(7) 0.076(6) Uani 1 1 d D . . 
H20A H 1.1782 1.1463 0.3278 0.114 Uiso 1 1 calc R . . 
H20B H 1.1858 1.0741 0.3000 0.114 Uiso 1 1 calc R . . 
H20C H 1.2207 1.0651 0.3527 0.114 Uiso 1 1 calc R . . 
C21 C 1.0565(8) 0.8315(7) 0.4548(5) 0.042(4) Uani 1 1 d D . . 
H21A H 1.0448 0.7764 0.4657 0.050 Uiso 1 1 calc R . . 
H21B H 1.1109 0.8347 0.4290 0.050 Uiso 1 1 calc R . . 
C22 C 1.0676(8) 0.8594(7) 0.5022(5) 0.042(4) Uani 1 1 d D . . 
H22A H 1.0131 0.8593 0.5279 0.050 Uiso 1 1 calc R . . 
H22B H 1.0851 0.9128 0.4917 0.050 Uiso 1 1 calc R . . 
C23 C 1.1356(9) 0.8067(8) 0.5273(5) 0.054(4) Uani 1 1 d D . . 
H23A H 1.1185 0.7532 0.5370 0.065 Uiso 1 1 calc R . . 
H23B H 1.1901 0.8075 0.5016 0.065 Uiso 1 1 calc R . . 
C24 C 1.1478(10) 0.8323(9) 0.5761(6) 0.066(5) Uani 1 1 d D . . 
H24A H 1.1926 0.7986 0.5908 0.099 Uiso 1 1 calc R . . 
H24B H 1.0945 0.8293 0.6021 0.099 Uiso 1 1 calc R . . 
H24C H 1.1641 0.8855 0.5665 0.099 Uiso 1 1 calc R . . 
C25 C 0.8992(7) 0.8670(6) 0.4636(5) 0.041(4) Uani 1 1 d D . . 
H25A H 0.8573 0.9029 0.4466 0.049 Uiso 1 1 calc R . . 
H25B H 0.9017 0.8840 0.4961 0.049 Uiso 1 1 calc R . . 
C26 C 0.8660(8) 0.7863(7) 0.4787(5) 0.041(4) Uani 1 1 d D . . 
H26A H 0.9107 0.7479 0.4906 0.049 Uiso 1 1 calc R . . 
H26B H 0.8517 0.7724 0.4478 0.049 Uiso 1 1 calc R . . 
C27 C 0.7866(8) 0.7849(7) 0.5228(5) 0.044(4) Uani 1 1 d D . . 
H27A H 0.8020 0.7962 0.5541 0.052 Uiso 1 1 calc R . . 
H27B H 0.7436 0.8256 0.5115 0.052 Uiso 1 1 calc R . . 
C28 C 0.7497(11) 0.7095(8) 0.5366(7) 0.076(6) Uani 1 1 d D . . 
H28A H 0.7004 0.7102 0.5655 0.115 Uiso 1 1 calc R . . 
H28B H 0.7924 0.6690 0.5474 0.115 Uiso 1 1 calc R . . 
H28C H 0.7317 0.6994 0.5061 0.115 Uiso 1 1 calc R . . 
C29 C 0.9906(8) 0.8400(7) 0.3799(4) 0.044(4) Uani 1 1 d D . . 
H29A H 0.9821 0.7844 0.3921 0.052 Uiso 1 1 calc R . . 
H29B H 1.0489 0.8442 0.3585 0.052 Uiso 1 1 calc R . . 
C30 C 0.9288(10) 0.8740(8) 0.3447(6) 0.062(5) Uani 1 1 d D . . 
H30A H 0.9457 0.9253 0.3249 0.075 Uiso 1 1 calc R . . 
H30B H 0.8712 0.8808 0.3663 0.075 Uiso 1 1 calc R . . 
C31 C 0.9265(11) 0.8223(9) 0.3065(6) 0.071(5) Uani 1 1 d D . . 
H31A H 0.8966 0.8516 0.2789 0.086 Uiso 1 1 calc R . . 
H31B H 0.9855 0.8086 0.2893 0.086 Uiso 1 1 calc R . . 
C32 C 0.8836(11) 0.7502(8) 0.3314(7) 0.076(5) Uani 1 1 d D . . 
H32A H 0.8860 0.7192 0.3049 0.114 Uiso 1 1 calc R . . 
H32B H 0.8241 0.7632 0.3467 0.114 Uiso 1 1 calc R . . 
H32C H 0.9125 0.7209 0.3589 0.114 Uiso 1 1 calc R . . 
N3 N 0.7575(6) 0.4928(5) 0.1899(3) 0.038(3) Uani 1 1 d D . . 
C33 C 0.8329(7) 0.4382(7) 0.2054(4) 0.037(4) Uani 1 1 d D . . 
H33A H 0.8164 0.3847 0.2127 0.045 Uiso 1 1 calc R . . 
H33B H 0.8811 0.4434 0.1750 0.045 Uiso 1 1 calc R . . 
C34 C 0.8631(9) 0.4510(7) 0.2519(5) 0.050(4) Uani 1 1 d D . . 
H34A H 0.8146 0.4500 0.2820 0.060 Uiso 1 1 calc R . . 
H34B H 0.8860 0.5022 0.2438 0.060 Uiso 1 1 calc R . . 
C35 C 0.9323(9) 0.3886(7) 0.2665(6) 0.049(4) Uani 1 1 d D . . 
H35A H 0.9775 0.3858 0.2350 0.059 Uiso 1 1 calc R . . 
H35B H 0.9583 0.4033 0.2930 0.059 Uiso 1 1 calc R . . 
C36 C 0.8992(10) 0.3116(8) 0.2877(6) 0.069(5) Uani 1 1 d D . . 
H36A H 0.9458 0.2740 0.2962 0.103 Uiso 1 1 calc R . . 
H36B H 0.8743 0.2964 0.2614 0.103 Uiso 1 1 calc R . . 
H36C H 0.8555 0.3137 0.3194 0.103 Uiso 1 1 calc R . . 
C37 C 0.7787(8) 0.5768(6) 0.1816(5) 0.040(4) Uani 1 1 d D . . 
H37A H 0.7308 0.6108 0.1699 0.048 Uiso 1 1 calc R . . 
H37B H 0.7832 0.5874 0.2158 0.048 Uiso 1 1 calc R . . 
C38 C 0.8588(8) 0.5976(7) 0.1430(5) 0.046(4) Uani 1 1 d D . . 
H38A H 0.8551 0.5882 0.1084 0.055 Uiso 1 1 calc R . . 
H38B H 0.9077 0.5650 0.1545 0.055 Uiso 1 1 calc R . . 
C39 C 0.8724(8) 0.6823(6) 0.1383(6) 0.049(4) Uani 1 1 d D . . 
H39A H 0.8731 0.6921 0.1733 0.059 Uiso 1 1 calc R . . 
H39B H 0.8245 0.7149 0.1253 0.059 Uiso 1 1 calc R . . 
C40 C 0.9558(9) 0.7044(8) 0.1010(6) 0.066(5) Uani 1 1 d D . . 
H40A H 0.9621 0.7592 0.0981 0.098 Uiso 1 1 calc R . . 
H40B H 0.9555 0.6943 0.0664 0.098 Uiso 1 1 calc R . . 
H40C H 1.0035 0.6737 0.1146 0.098 Uiso 1 1 calc R . . 
C41 C 0.7422(7) 0.4745(7) 0.1404(4) 0.036(3) Uani 1 1 d D . . 
H41A H 0.7342 0.4189 0.1470 0.043 Uiso 1 1 calc R . . 
H41B H 0.7944 0.4839 0.1132 0.043 Uiso 1 1 calc R . . 
C42 C 0.6669(7) 0.5185(7) 0.1178(5) 0.038(4) Uani 1 1 d D . . 
H42A H 0.6131 0.5053 0.1426 0.046 Uiso 1 1 calc R . . 
H42B H 0.6714 0.5745 0.1128 0.046 Uiso 1 1 calc R . . 
C43 C 0.6662(9) 0.4979(8) 0.0662(5) 0.052(4) Uani 1 1 d D . . 
H43A H 0.7208 0.5102 0.0419 0.062 Uiso 1 1 calc R . . 
H43B H 0.6619 0.4418 0.0716 0.062 Uiso 1 1 calc R . . 
C44 C 0.5948(9) 0.5392(9) 0.0413(6) 0.071(6) Uani 1 1 d D . . 
H44A H 0.5973 0.5230 0.0082 0.107 Uiso 1 1 calc R . . 
H44B H 0.5998 0.5949 0.0346 0.107 Uiso 1 1 calc R . . 
H44C H 0.5404 0.5269 0.0649 0.107 Uiso 1 1 calc R . . 
C45 C 0.6792(8) 0.4809(7) 0.2332(5) 0.050(4) Uani 1 1 d D . . 
H45A H 0.6915 0.4954 0.2644 0.060 Uiso 1 1 calc R . . 
H45B H 0.6326 0.5174 0.2220 0.060 Uiso 1 1 calc R . . 
C46 C 0.6478(12) 0.4039(9) 0.2493(7) 0.098(8) Uani 1 1 d D . . 
H46A H 0.6904 0.3675 0.2652 0.117 Uiso 1 1 calc R . . 
H46B H 0.6399 0.3861 0.2181 0.117 Uiso 1 1 calc R . . 
C47 C 0.5610(11) 0.4043(11) 0.2899(10) 0.186(16) Uani 1 1 d D . . 
H47A H 0.5718 0.4109 0.3237 0.223 Uiso 1 1 calc R . . 
H47B H 0.5233 0.4489 0.2771 0.223 Uiso 1 1 calc R . . 
C48 C 0.518(2) 0.3349(18) 0.2984(16) 0.31(3) Uani 1 1 d D . . 
H48A H 0.4642 0.3388 0.3235 0.467 Uiso 1 1 calc R . . 
H48B H 0.5541 0.2906 0.3122 0.467 Uiso 1 1 calc R . . 
H48C H 0.5066 0.3282 0.2651 0.467 Uiso 1 1 calc R . . 
N4 N 0.5388(5) 0.2222(5) 0.0611(3) 0.031(3) Uani 1 1 d D . . 
C49 C 0.6085(7) 0.1579(6) 0.0733(4) 0.033(3) Uani 1 1 d D . . 
H49A H 0.6610 0.1821 0.0723 0.040 Uiso 1 1 calc R . . 
H49B H 0.5901 0.1291 0.1095 0.040 Uiso 1 1 calc R . . 
C50 C 0.6294(8) 0.1017(7) 0.0368(5) 0.047(4) Uani 1 1 d D . . 
H50A H 0.6538 0.1284 0.0010 0.056 Uiso 1 1 calc R . . 
H50B H 0.5772 0.0788 0.0357 0.056 Uiso 1 1 calc R . . 
C51 C 0.6939(9) 0.0385(7) 0.0571(6) 0.053(4) Uani 1 1 d D . . 
H51A H 0.7454 0.0623 0.0585 0.064 Uiso 1 1 calc R . . 
H51B H 0.6691 0.0129 0.0932 0.064 Uiso 1 1 calc R . . 
C52 C 0.7187(12) -0.0205(9) 0.0233(7) 0.088(6) Uani 1 1 d D . . 
H52A H 0.7589 -0.0602 0.0379 0.132 Uiso 1 1 calc R . . 
H52B H 0.7454 0.0042 -0.0122 0.132 Uiso 1 1 calc R . . 
H52C H 0.6679 -0.0443 0.0218 0.132 Uiso 1 1 calc R . . 
C53 C 0.5636(8) 0.2691(8) 0.0057(4) 0.044(4) Uani 1 1 d D . . 
H53A H 0.5665 0.2349 -0.0194 0.053 Uiso 1 1 calc R . . 
H53B H 0.5176 0.3099 -0.0002 0.053 Uiso 1 1 calc R . . 
C54 C 0.6455(8) 0.3061(9) -0.0068(4) 0.049(4) Uani 1 1 d D . . 
H54A H 0.6921 0.2672 0.0013 0.059 Uiso 1 1 calc R . . 
H54B H 0.6416 0.3459 0.0145 0.059 Uiso 1 1 calc R . . 
C55 C 0.6636(9) 0.3427(9) -0.0647(5) 0.061(5) Uani 1 1 d D . . 
H55A H 0.6627 0.3028 -0.0852 0.074 Uiso 1 1 calc R . . 
H55B H 0.6173 0.3826 -0.0717 0.074 Uiso 1 1 calc R . . 
C56 C 0.7469(10) 0.3789(10) -0.0839(6) 0.071(5) Uani 1 1 d D . . 
H56A H 0.7539 0.4003 -0.1215 0.107 Uiso 1 1 calc R . . 
H56B H 0.7935 0.3398 -0.0777 0.107 Uiso 1 1 calc R . . 
H56C H 0.7477 0.4201 -0.0651 0.107 Uiso 1 1 calc R . . 
C57 C 0.4553(7) 0.1886(7) 0.0643(5) 0.035(3) Uani 1 1 d D . . 
H57A H 0.4123 0.2318 0.0572 0.042 Uiso 1 1 calc R . . 
H57B H 0.4633 0.1591 0.0360 0.042 Uiso 1 1 calc R . . 
C58 C 0.4188(8) 0.1363(8) 0.1157(5) 0.049(4) Uani 1 1 d D . . 
H58A H 0.4103 0.1646 0.1447 0.058 Uiso 1 1 calc R . . 
H58B H 0.4595 0.0912 0.1228 0.058 Uiso 1 1 calc R . . 
C59 C 0.3341(8) 0.1092(9) 0.1131(6) 0.073(6) Uani 1 1 d D . . 
H59A H 0.2938 0.1545 0.1055 0.088 Uiso 1 1 calc R . . 
H59B H 0.3429 0.0808 0.0840 0.088 Uiso 1 1 calc R . . 
C60 C 0.2971(11) 0.0594(10) 0.1618(7) 0.103(8) Uani 1 1 d D . . 
H60A H 0.2432 0.0429 0.1585 0.154 Uiso 1 1 calc R . . 
H60B H 0.2868 0.0877 0.1905 0.154 Uiso 1 1 calc R . . 
H60C H 0.3365 0.0141 0.1692 0.154 Uiso 1 1 calc R . . 
C61 C 0.5314(8) 0.2705(7) 0.1027(5) 0.039(4) Uani 1 1 d D . . 
H61A H 0.5201 0.2360 0.1375 0.046 Uiso 1 1 calc R . . 
H61B H 0.5871 0.2914 0.0986 0.046 Uiso 1 1 calc R . . 
C62 C 0.4646(9) 0.3360(7) 0.1023(5) 0.052(4) Uani 1 1 d D . . 
H62A H 0.4075 0.3165 0.1097 0.062 Uiso 1 1 calc R . . 
H62B H 0.4733 0.3709 0.0676 0.062 Uiso 1 1 calc R . . 
C63 C 0.4719(10) 0.3794(8) 0.1448(7) 0.069(5) Uani 1 1 d D . . 
H63A H 0.4695 0.3425 0.1785 0.083 Uiso 1 1 calc R . . 
H63B H 0.5277 0.4017 0.1355 0.083 Uiso 1 1 calc R . . 
C64 C 0.4045(13) 0.4408(11) 0.1511(8) 0.129(9) Uani 1 1 d D . . 
H64A H 0.4123 0.4674 0.1781 0.194 Uiso 1 1 calc R . . 
H64B H 0.3491 0.4187 0.1617 0.194 Uiso 1 1 calc R . . 
H64C H 0.4067 0.4776 0.1178 0.194 Uiso 1 1 calc R . . 
N5 N 0.0224(6) 0.1355(5) 0.0887(4) 0.040(3) Uani 1 1 d D . . 
C65 C 0.0124(8) 0.0487(6) 0.1096(5) 0.047(4) Uani 1 1 d D . . 
H65A H 0.0132 0.0238 0.0797 0.057 Uiso 1 1 calc R . . 
H65B H 0.0620 0.0258 0.1253 0.057 Uiso 1 1 calc R . . 
C66 C -0.0680(10) 0.0306(8) 0.1500(6) 0.081(6) Uani 1 1 d D . . 
H66A H -0.1174 0.0607 0.1373 0.097 Uiso 1 1 calc R . . 
H66B H -0.0642 0.0453 0.1830 0.097 Uiso 1 1 calc R . . 
C67 C -0.0809(11) -0.0559(8) 0.1602(7) 0.077(6) Uani 1 1 d D . . 
H67A H -0.0260 -0.0864 0.1622 0.092 Uiso 1 1 calc R . . 
H67B H -0.1209 -0.0708 0.1939 0.092 Uiso 1 1 calc R . . 
C68 C -0.1150(14) -0.0712(10) 0.1173(9) 0.120(9) Uani 1 1 d D . . 
H68A H -0.1227 -0.1263 0.1230 0.180 Uiso 1 1 calc R . . 
H68B H -0.0752 -0.0559 0.0841 0.180 Uiso 1 1 calc R . . 
H68C H -0.1699 -0.0417 0.1161 0.180 Uiso 1 1 calc R . . 
C69 C 0.1101(7) 0.1426(6) 0.0524(5) 0.041(4) Uani 1 1 d D . . 
H69A H 0.1524 0.1105 0.0711 0.049 Uiso 1 1 calc R . . 
H69B H 0.1094 0.1206 0.0215 0.049 Uiso 1 1 calc R . . 
C70 C 0.1397(8) 0.2218(6) 0.0333(5) 0.040(4) Uani 1 1 d D . . 
H70A H 0.1530 0.2407 0.0627 0.048 Uiso 1 1 calc R . . 
H70B H 0.0940 0.2572 0.0199 0.048 Uiso 1 1 calc R . . 
C71 C 0.2183(8) 0.2212(7) -0.0099(5) 0.053(4) Uani 1 1 d D . . 
H71A H 0.2036 0.2070 -0.0406 0.063 Uiso 1 1 calc R . . 
H71B H 0.2621 0.1822 0.0024 0.063 Uiso 1 1 calc R . . 
C72 C 0.2531(10) 0.2999(7) -0.0257(6) 0.067(5) Uani 1 1 d D . . 
H72A H 0.3025 0.2996 -0.0545 0.101 Uiso 1 1 calc R . . 
H72B H 0.2702 0.3126 0.0043 0.101 Uiso 1 1 calc R . . 
H72C H 0.2091 0.3385 -0.0371 0.101 Uiso 1 1 calc R . . 
C73 C 0.0161(8) 0.1757(7) 0.1339(5) 0.052(4) Uani 1 1 d D . . 
H73A H -0.0418 0.1710 0.1558 0.062 Uiso 1 1 calc R . . 
H73B H 0.0227 0.2311 0.1196 0.062 Uiso 1 1 calc R . . 
C74 C 0.0810(10) 0.1459(8) 0.1693(6) 0.063(5) Uani 1 1 d D . . 
H74A H 0.0708 0.0922 0.1874 0.076 Uiso 1 1 calc R . . 
H74B H 0.1392 0.1461 0.1476 0.076 Uiso 1 1 calc R . . 
C75 C 0.0738(11) 0.1959(9) 0.2097(6) 0.073(5) Uani 1 1 d D . . 
H75A H 0.0138 0.2018 0.2279 0.088 Uiso 1 1 calc R . . 
H75B H 0.1079 0.1704 0.2361 0.088 Uiso 1 1 calc R . . 
C76 C 0.1037(13) 0.2714(9) 0.1853(8) 0.098(7) Uani 1 1 d D . . 
H76A H 0.0988 0.3023 0.2121 0.147 Uiso 1 1 calc R . . 
H76B H 0.0692 0.2971 0.1597 0.147 Uiso 1 1 calc R . . 
H76C H 0.1634 0.2656 0.1675 0.147 Uiso 1 1 calc R . . 
C77 C -0.0474(7) 0.1717(7) 0.0602(5) 0.043(4) Uani 1 1 d D . . 
H77A H -0.0386 0.2271 0.0477 0.051 Uiso 1 1 calc R . . 
H77B H -0.1021 0.1678 0.0857 0.051 Uiso 1 1 calc R . . 
C78 C -0.0561(8) 0.1389(7) 0.0138(5) 0.045(4) Uani 1 1 d D . . 
H78A H -0.0684 0.0841 0.0255 0.054 Uiso 1 1 calc R . . 
H78B H -0.0021 0.1419 -0.0124 0.054 Uiso 1 1 calc R . . 
C79 C -0.1281(9) 0.1847(8) -0.0107(5) 0.053(4) Uani 1 1 d D . . 
H79A H -0.1807 0.1842 0.0166 0.064 Uiso 1 1 calc R . . 
H79B H -0.1138 0.2388 -0.0235 0.064 Uiso 1 1 calc R . . 
C80 C -0.1444(10) 0.1533(9) -0.0554(5) 0.064(5) Uani 1 1 d D . . 
H80A H -0.1915 0.1843 -0.0693 0.096 Uiso 1 1 calc R . . 
H80B H -0.1591 0.0998 -0.0428 0.096 Uiso 1 1 calc R . . 
H80C H -0.0931 0.1552 -0.0831 0.096 Uiso 1 1 calc R . . 
N6 N 0.4708(6) 0.7649(5) 0.4391(4) 0.044(3) Uani 1 1 d D . . 
C81 C 0.5510(7) 0.8016(7) 0.4429(5) 0.044(4) Uani 1 1 d D . . 
H81A H 0.5362 0.8287 0.4728 0.053 Uiso 1 1 calc R . . 
H81B H 0.5953 0.7600 0.4505 0.053 Uiso 1 1 calc R . . 
C82 C 0.5879(8) 0.8585(8) 0.3937(5) 0.053(4) Uani 1 1 d D . . 
H82A H 0.5444 0.9002 0.3847 0.063 Uiso 1 1 calc R . . 
H82B H 0.6074 0.8319 0.3637 0.063 Uiso 1 1 calc R . . 
C83 C 0.6634(9) 0.8916(9) 0.4059(7) 0.078(6) Uani 1 1 d D . . 
H83A H 0.6430 0.9164 0.4366 0.093 Uiso 1 1 calc R . . 
H83B H 0.7059 0.8489 0.4151 0.093 Uiso 1 1 calc R . . 
C84 C 0.7047(11) 0.9484(10) 0.3614(8) 0.119(9) Uani 1 1 d D . . 
H84A H 0.7531 0.9666 0.3706 0.178 Uiso 1 1 calc R . . 
H84B H 0.6637 0.9921 0.3532 0.178 Uiso 1 1 calc R . . 
H84C H 0.7247 0.9243 0.3307 0.178 Uiso 1 1 calc R . . 
C85 C 0.4002(8) 0.8273(6) 0.4272(5) 0.042(4) Uani 1 1 d D . . 
H85A H 0.4190 0.8573 0.3914 0.050 Uiso 1 1 calc R . . 
H85B H 0.3494 0.8015 0.4269 0.050 Uiso 1 1 calc R . . 
C86 C 0.3740(9) 0.8828(7) 0.4642(5) 0.051(4) Uani 1 1 d D . . 
H86A H 0.4238 0.9085 0.4661 0.061 Uiso 1 1 calc R . . 
H86B H 0.3496 0.8551 0.4997 0.061 Uiso 1 1 calc R . . 
C87 C 0.3073(9) 0.9426(7) 0.4428(6) 0.056(4) Uani 1 1 d D . . 
H87A H 0.3323 0.9691 0.4070 0.068 Uiso 1 1 calc R . . 
H87B H 0.2583 0.9160 0.4406 0.068 Uiso 1 1 calc R . . 
C88 C 0.2764(12) 1.0018(9) 0.4773(7) 0.086(6) Uani 1 1 d D . . 
H88A H 0.2337 1.0385 0.4627 0.128 Uiso 1 1 calc R . . 
H88B H 0.3245 1.0293 0.4788 0.128 Uiso 1 1 calc R . . 
H88C H 0.2512 0.9758 0.5127 0.128 Uiso 1 1 calc R . . 
C89 C 0.4443(9) 0.7141(8) 0.4931(5) 0.061(5) Uani 1 1 d D . . 
H89A H 0.4937 0.6790 0.5015 0.074 Uiso 1 1 calc R . . 
H89B H 0.4284 0.7473 0.5196 0.074 Uiso 1 1 calc R . . 
C90 C 0.3702(11) 0.6664(12) 0.4973(7) 0.138(11) Uani 1 1 d D . . 
H90A H 0.3181 0.7012 0.4950 0.166 Uiso 1 1 calc R . . 
H90B H 0.3819 0.6394 0.4675 0.166 Uiso 1 1 calc R . . 
C91 C 0.3551(13) 0.6085(15) 0.5475(9) 0.184(17) Uani 1 1 d D . . 
H91A H 0.3479 0.5580 0.5399 0.221 Uiso 1 1 calc R . . 
H91B H 0.4053 0.6025 0.5640 0.221 Uiso 1 1 calc R . . 
C92 C 0.284(2) 0.631(2) 0.5819(9) 0.23(2) Uani 1 1 d D . . 
H92A H 0.2877 0.6051 0.6178 0.345 Uiso 1 1 calc R . . 
H92B H 0.2328 0.6157 0.5733 0.345 Uiso 1 1 calc R . . 
H92C H 0.2798 0.6865 0.5790 0.345 Uiso 1 1 calc R . . 
C93 C 0.4909(10) 0.7210(7) 0.3944(5) 0.056(4) Uani 1 1 d D . . 
H93A H 0.4378 0.7008 0.3920 0.068 Uiso 1 1 calc R . . 
H93B H 0.5093 0.7578 0.3613 0.068 Uiso 1 1 calc R . . 
C94 C 0.5576(12) 0.6552(9) 0.3984(6) 0.089(6) Uani 1 1 d D . . 
H94A H 0.5416 0.6191 0.4321 0.107 Uiso 1 1 calc R . . 
H94B H 0.6125 0.6751 0.3979 0.107 Uiso 1 1 calc R . . 
C95 C 0.5686(15) 0.6116(10) 0.3526(7) 0.111(8) Uani 1 1 d D . . 
H95A H 0.6011 0.5613 0.3606 0.134 Uiso 1 1 calc R . . 
H95B H 0.5123 0.6023 0.3473 0.134 Uiso 1 1 calc R . . 
C96 C 0.6166(17) 0.6616(12) 0.3034(8) 0.163(12) Uani 1 1 d D . . 
H96A H 0.6218 0.6367 0.2734 0.244 Uiso 1 1 calc R . . 
H96B H 0.6733 0.6681 0.3084 0.244 Uiso 1 1 calc R . . 
H96C H 0.5853 0.7121 0.2968 0.244 Uiso 1 1 calc R . . 
P1 P 0.0637(2) 0.59868(18) 0.45683(13) 0.0314(9) Uani 1 1 d D . . 
O1 O 0.0811(6) 0.5159(4) 0.4506(3) 0.055(3) Uani 1 1 d D . . 
O2 O 0.1354(5) 0.6231(5) 0.4786(3) 0.052(3) Uani 1 1 d D . . 
H02 H 0.1697 0.6474 0.4539 0.078 Uiso 1 1 calc RD . . 
O3 O 0.0527(5) 0.6556(5) 0.4070(3) 0.042(3) Uani 1 1 d D . . 
O4 O -0.0185(5) 0.6054(4) 0.4994(3) 0.036(2) Uani 1 1 d D . . 
H04 H -0.0349 0.5613 0.5131 0.053 Uiso 1 1 calc RD . . 
P2 P 0.2445(2) 0.75037(18) 0.36253(14) 0.0322(9) Uani 1 1 d D . . 
O5 O 0.2373(7) 0.7151(6) 0.4196(3) 0.067(3) Uani 1 1 d D . . 
O6 O 0.3276(5) 0.7273(5) 0.3289(4) 0.054(3) Uani 1 1 d D . . 
O7 O 0.2326(5) 0.8391(4) 0.3564(3) 0.042(2) Uani 1 1 d D . . 
H07 H 0.2714 0.8591 0.3326 0.064 Uiso 1 1 calc RD . . 
O8 O 0.1707(5) 0.7254(4) 0.3421(3) 0.032(2) Uani 1 1 d D . . 
H08 H 0.1388 0.6987 0.3670 0.048 Uiso 1 1 calc RD . . 
P3 P 0.9306(2) 0.40506(17) 0.04494(13) 0.0282(9) Uani 1 1 d D . . 
O9 O 0.8622(6) 0.3735(5) 0.0238(3) 0.044(3) Uani 1 1 d D . . 
H09 H 0.8303 0.3471 0.0488 0.066 Uiso 1 1 calc RD . . 
O10 O 0.9099(6) 0.4892(4) 0.0453(3) 0.050(3) Uani 1 1 d D . . 
O11 O 1.0151(5) 0.3935(4) 0.0058(3) 0.037(2) Uani 1 1 d D . . 
H011 H 1.0295 0.4364 -0.0122 0.056 Uiso 1 1 calc RD . . 
O12 O 0.9364(5) 0.3566(5) 0.0985(3) 0.039(2) Uani 1 1 d D . . 
P4 P 0.7528(2) 0.24823(18) 0.14265(13) 0.0297(9) Uani 1 1 d D . . 
O13 O 0.7462(6) 0.2975(5) 0.0897(3) 0.047(3) Uani 1 1 d D . . 
O14 O 0.8252(5) 0.2755(5) 0.1635(3) 0.034(2) Uani 1 1 d D . . 
H014 H 0.8550 0.3047 0.1390 0.051 Uiso 1 1 calc RD . . 
O15 O 0.7681(5) 0.1634(4) 0.1423(3) 0.040(2) Uani 1 1 d D . . 
O16 O 0.6712(5) 0.2632(5) 0.1831(4) 0.045(3) Uani 1 1 d D . . 
H016 H 0.6535 0.2210 0.2004 0.067 Uiso 1 1 calc RD . . 
P5 P 0.5916(3) 0.0736(2) 0.22562(16) 0.0515(13) Uani 1 1 d D . . 
O17 O 0.6891(5) 0.0585(5) 0.2096(3) 0.052(3) Uani 1 1 d D . . 
H017 H 0.7085 0.0947 0.1856 0.079 Uiso 1 1 calc RD . . 
O18 O 0.5701(6) 0.1575(6) 0.2184(5) 0.095(5) Uani 1 1 d D . . 
O19 O 0.5633(6) 0.0286(6) 0.2810(3) 0.065(3) Uani 1 1 d D . . 
O20 O 0.5502(8) 0.0442(8) 0.1882(4) 0.133(7) Uani 1 1 d D . . 
H020 H 0.5110 0.0165 0.2055 0.200 Uiso 1 1 calc RD . . 
P6 P 0.4266(3) 0.8974(3) 0.26772(18) 0.0752(18) Uani 1 1 d D . . 
O21 O 0.4543(6) 0.9402(6) 0.2129(3) 0.068(4) Uani 1 1 d D . . 
O22 O 0.4976(8) 0.8950(8) 0.2970(5) 0.112(5) Uani 1 1 d DU . . 
H022 H 0.5444 0.8977 0.2756 0.168 Uiso 1 1 calc RD . . 
O23 O 0.4293(7) 0.8108(7) 0.2661(6) 0.152(8) Uani 1 1 d D . . 
H023 H 0.3823 0.7937 0.2817 0.228 Uiso 1 1 calc RD . . 
O24 O 0.3385(7) 0.9235(5) 0.2922(4) 0.078(4) Uani 1 1 d D . . 
C97 C 0.5139(14) 0.1385(9) 0.8841(6) 0.139(11) Uani 1 1 d D . . 
H97A H 0.4749 0.1228 0.8651 0.166 Uiso 1 1 calc R . . 
H97B H 0.5672 0.1516 0.8587 0.166 Uiso 1 1 calc R . . 
Cl1 Cl 0.5364(5) 0.0621(4) 0.9319(2) 0.133(2) Uani 1 1 d DU . . 
Cl2 Cl 0.4677(5) 0.2207(4) 0.9083(3) 0.136(2) Uani 1 1 d DU . . 
C98 C 0.8680(8) 0.5453(9) 0.4224(5) 0.059(5) Uani 1 1 d D . . 
H98A H 0.8687 0.5004 0.4516 0.070 Uiso 1 1 calc R . . 
H98B H 0.9106 0.5798 0.4240 0.070 Uiso 1 1 calc R . . 
Cl3 Cl 0.7676(3) 0.5942(3) 0.42984(19) 0.0814(15) Uani 1 1 d DU . . 
Cl4 Cl 0.8957(3) 0.5137(3) 0.36270(17) 0.0804(15) Uani 1 1 d DU . . 
C99 C 0.3292(14) 0.1426(12) 0.7849(8) 0.139(10) Uani 1 1 d D . . 
H99A H 0.3854 0.1502 0.7614 0.167 Uiso 1 1 calc R . . 
H99B H 0.3221 0.0866 0.7947 0.167 Uiso 1 1 calc R . . 
Cl5 Cl 0.2504(4) 0.1882(4) 0.7525(3) 0.127(2) Uani 1 1 d DU . . 
Cl6 Cl 0.3253(4) 0.1791(4) 0.8418(3) 0.133(2) Uani 1 1 d DU . . 
C100 C 0.4915(14) 0.1276(8) 0.3879(6) 0.093(6) Uani 1 1 d D . . 
H10C H 0.4336 0.1230 0.3829 0.111 Uiso 1 1 calc R . . 
H10D H 0.5322 0.1230 0.3549 0.111 Uiso 1 1 calc R . . 
Cl7 Cl 0.5158(4) 0.0568(4) 0.4376(2) 0.121(2) Uani 1 1 d DU . . 
Cl8 Cl 0.4968(5) 0.2172(4) 0.4040(3) 0.158(3) Uani 1 1 d DU . . 
C101 C 0.2125(9) 0.8673(8) 0.2282(5) 0.059(5) Uani 1 1 d D . . 
H10E H 0.2576 0.8933 0.2360 0.071 Uiso 1 1 calc R . . 
H10F H 0.2041 0.8187 0.2543 0.071 Uiso 1 1 calc R . . 
Cl9 Cl 0.2448(4) 0.8464(3) 0.1661(2) 0.112(2) Uani 1 1 d DU . . 
Cl10 Cl 0.1166(3) 0.9273(3) 0.2340(2) 0.1005(18) Uani 1 1 d DU . . 
C102 C 0.1247(8) 0.4537(9) 0.0830(5) 0.054(4) Uani 1 1 d D . . 
H10E H 0.0868 0.4152 0.0811 0.065 Uiso 1 1 calc R . . 
H10F H 0.1243 0.4961 0.0522 0.065 Uiso 1 1 calc R . . 
Cl11 Cl 0.2283(3) 0.4108(3) 0.0814(2) 0.0934(17) Uani 1 1 d DU . . 
Cl12 Cl 0.0863(3) 0.4903(2) 0.14084(16) 0.0614(12) Uani 1 1 d DU . . 
C103 C 0.2181(9) 0.8633(10) 0.7234(5) 0.081(6) Uani 1 1 d D . . 
H10G H 0.2052 0.8227 0.7552 0.097 Uiso 1 1 calc R . . 
H10H H 0.2482 0.9026 0.7319 0.097 Uiso 1 1 calc R . . 
Cl13 Cl 0.1237(3) 0.9054(3) 0.70496(19) 0.0847(15) Uani 1 1 d DU . . 
Cl14 Cl 0.2838(4) 0.8229(3) 0.6726(2) 0.1016(18) Uani 1 1 d DU . . 
C104 C 0.3691(12) 0.1958(14) 0.2628(6) 0.136(10) Uani 1 1 d D . . 
H10I H 0.4284 0.2001 0.2430 0.164 Uiso 1 1 calc R . . 
H10J H 0.3577 0.1407 0.2719 0.164 Uiso 1 1 calc R . . 
Cl15 Cl 0.2996(5) 0.2468(4) 0.2241(3) 0.139(2) Uani 1 1 d DU . . 
Cl16 Cl 0.3570(8) 0.2321(8) 0.3209(5) 0.274(5) Uani 1 1 d DU . . 
 
 
_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 C13 1.491(12) . ? 
N1 C9 1.526(12) . ? 
N1 C5 1.532(13) . ? 
N1 C1 1.541(12) . ? 
C1 C2 1.503(12) . ? 
C2 C3 1.544(13) . ? 
C3 C4 1.529(14) . ? 
C5 C6 1.484(14) . ? 
C6 C7 1.502(15) . ? 
C7 C8 1.523(15) . ? 
C9 C10 1.544(15) . ? 
C10 C11 1.494(15) . ? 
C11 C12 1.417(18) . ? 
C13 C14 1.505(14) . ? 
C14 C15 1.544(14) . ? 
C15 C16 1.506(15) . ? 
N2 C29 1.507(12) . ? 
N2 C25 1.519(12) . ? 
N2 C21 1.535(12) . ? 
N2 C17 1.541(12) . ? 
C17 C18 1.506(14) . ? 
C18 C19 1.543(14) . ? 
C19 C20 1.498(15) . ? 
C21 C22 1.510(13) . ? 
C22 C23 1.532(14) . ? 
C23 C24 1.528(14) . ? 
C25 C26 1.538(13) . ? 
C26 C27 1.537(13) . ? 
C27 C28 1.477(14) . ? 
C29 C30 1.508(13) . ? 
C30 C31 1.525(15) . ? 
C31 C32 1.490(15) . ? 
N3 C41 1.503(12) . ? 
N3 C45 1.515(12) . ? 
N3 C37 1.538(12) . ? 
N3 C33 1.540(12) . ? 
C33 C34 1.501(13) . ? 
C34 C35 1.533(14) . ? 
C35 C36 1.483(14) . ? 
C37 C38 1.496(13) . ? 
C38 C39 1.528(13) . ? 
C39 C40 1.527(14) . ? 
C41 C42 1.534(13) . ? 
C42 C43 1.504(14) . ? 
C43 C44 1.497(14) . ? 
C45 C46 1.465(14) . ? 
C46 C47 1.573(17) . ? 
C47 C48 1.443(18) . ? 
N4 C57 1.521(11) . ? 
N4 C61 1.525(12) . ? 
N4 C53 1.526(11) . ? 
N4 C49 1.544(12) . ? 
C49 C50 1.506(13) . ? 
C50 C51 1.536(14) . ? 
C51 C52 1.495(15) . ? 
C53 C54 1.490(13) . ? 
C54 C55 1.520(13) . ? 
C55 C56 1.501(14) . ? 
C57 C58 1.522(13) . ? 
C58 C59 1.528(14) . ? 
C59 C60 1.457(15) . ? 
C61 C62 1.494(14) . ? 
C62 C63 1.535(15) . ? 
C63 C64 1.460(16) . ? 
N5 C77 1.505(12) . ? 
N5 C73 1.511(12) . ? 
N5 C69 1.533(12) . ? 
N5 C65 1.543(12) . ? 
C65 C66 1.514(14) . ? 
C66 C67 1.539(14) . ? 
C67 C68 1.464(17) . ? 
C69 C70 1.494(12) . ? 
C70 C71 1.517(13) . ? 
C71 C72 1.516(13) . ? 
C73 C74 1.538(14) . ? 
C74 C75 1.518(15) . ? 
C75 C76 1.452(15) . ? 
C77 C78 1.518(13) . ? 
C78 C79 1.526(14) . ? 
C79 C80 1.508(14) . ? 
N6 C93 1.523(13) . ? 
N6 C89 1.530(12) . ? 
N6 C85 1.532(12) . ? 
N6 C81 1.552(12) . ? 
C81 C82 1.529(13) . ? 
C82 C83 1.542(15) . ? 
C83 C84 1.476(16) . ? 
C85 C86 1.508(13) . ? 
C86 C87 1.536(14) . ? 
C87 C88 1.518(14) . ? 
C89 C90 1.522(15) . ? 
C90 C91 1.497(16) . ? 
C91 C92 1.384(18) . ? 
C93 C94 1.499(15) . ? 
C94 C95 1.553(16) . ? 
C95 C96 1.526(17) . ? 
P1 O1 1.508(8) . ? 
P1 O3 1.520(7) . ? 
P1 O2 1.549(8) . ? 
P1 O4 1.558(7) . ? 
P2 O5 1.502(8) . ? 
P2 O6 1.510(8) . ? 
P2 O7 1.549(7) . ? 
P2 O8 1.562(7) . ? 
P3 O10 1.500(8) . ? 
P3 O12 1.519(7) . ? 
P3 O11 1.548(7) . ? 
P3 O9 1.555(8) . ? 
P4 O15 1.505(8) . ? 
P4 O13 1.513(8) . ? 
P4 O16 1.545(8) . ? 
P4 O14 1.570(7) . ? 
P5 O18 1.477(10) . ? 
P5 O19 1.522(8) . ? 
P5 O20 1.526(10) . ? 
P5 O17 1.545(9) . ? 
P6 O21 1.495(8) . ? 
P6 O24 1.495(10) . ? 
P6 O22 1.516(11) . ? 
P6 O23 1.550(12) . ? 
C97 Cl1 1.719(13) . ? 
C97 Cl2 1.748(13) . ? 
C98 Cl3 1.741(12) . ? 
C98 Cl4 1.752(12) . ? 
C99 Cl5 1.724(14) . ? 
C99 Cl6 1.764(15) . ? 
C100 Cl7 1.703(14) . ? 
C100 Cl8 1.760(13) . ? 
C101 Cl9 1.733(12) . ? 
C101 Cl10 1.773(12) . ? 
C102 Cl11 1.752(12) . ? 
C102 Cl12 1.763(12) . ? 
C103 Cl13 1.742(13) . ? 
C103 Cl14 1.758(13) . ? 
C104 Cl15 1.740(15) . ? 
C104 Cl16 1.769(15) . ? 
 
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 N1 C9 111.0(9) . . ? 
C13 N1 C5 109.2(9) . . ? 
C9 N1 C5 108.4(10) . . ? 
C13 N1 C1 112.6(9) . . ? 
C9 N1 C1 106.4(9) . . ? 
C5 N1 C1 109.1(9) . . ? 
C2 C1 N1 113.2(9) . . ? 
C1 C2 C3 109.5(9) . . ? 
C4 C3 C2 111.6(10) . . ? 
C6 C5 N1 118.0(10) . . ? 
C5 C6 C7 113.9(12) . . ? 
C6 C7 C8 115.1(13) . . ? 
N1 C9 C10 115.6(11) . . ? 
C11 C10 C9 111.3(14) . . ? 
C12 C11 C10 114.5(17) . . ? 
N1 C13 C14 118.9(10) . . ? 
C13 C14 C15 110.9(10) . . ? 
C16 C15 C14 111.5(12) . . ? 
C29 N2 C25 111.4(9) . . ? 
C29 N2 C21 106.4(9) . . ? 
C25 N2 C21 111.1(9) . . ? 
C29 N2 C17 109.9(9) . . ? 
C25 N2 C17 107.1(8) . . ? 
C21 N2 C17 111.0(9) . . ? 
C18 C17 N2 115.0(9) . . ? 
C17 C18 C19 109.4(10) . . ? 
C20 C19 C18 111.9(11) . . ? 
C22 C21 N2 116.2(10) . . ? 
C21 C22 C23 109.4(10) . . ? 
C24 C23 C22 111.1(12) . . ? 
N2 C25 C26 116.3(9) . . ? 
C25 C26 C27 109.8(9) . . ? 
C28 C27 C26 111.7(11) . . ? 
N2 C29 C30 117.1(11) . . ? 
C29 C30 C31 111.2(11) . . ? 
C32 C31 C30 113.9(13) . . ? 
C41 N3 C45 110.7(9) . . ? 
C41 N3 C37 111.3(9) . . ? 
C45 N3 C37 107.7(8) . . ? 
C41 N3 C33 107.1(8) . . ? 
C45 N3 C33 110.3(9) . . ? 
C37 N3 C33 109.7(9) . . ? 
C34 C33 N3 115.8(9) . . ? 
C33 C34 C35 110.7(11) . . ? 
C36 C35 C34 112.7(11) . . ? 
C38 C37 N3 115.3(9) . . ? 
C37 C38 C39 110.1(10) . . ? 
C38 C39 C40 111.3(10) . . ? 
N3 C41 C42 117.8(9) . . ? 
C43 C42 C41 110.3(10) . . ? 
C44 C43 C42 113.4(12) . . ? 
C46 C45 N3 117.9(11) . . ? 
C45 C46 C47 110.9(13) . . ? 
C48 C47 C46 113(2) . . ? 
C57 N4 C61 111.5(9) . . ? 
C57 N4 C53 107.0(8) . . ? 
C61 N4 C53 112.2(9) . . ? 
C57 N4 C49 111.0(8) . . ? 
C61 N4 C49 104.1(8) . . ? 
C53 N4 C49 111.1(9) . . ? 
C50 C49 N4 115.0(9) . . ? 
C49 C50 C51 108.2(10) . . ? 
C52 C51 C50 112.2(12) . . ? 
C54 C53 N4 116.3(9) . . ? 
C53 C54 C55 108.6(10) . . ? 
C56 C55 C54 114.8(11) . . ? 
C58 C57 N4 117.1(9) . . ? 
C57 C58 C59 110.6(10) . . ? 
C60 C59 C58 111.9(12) . . ? 
C62 C61 N4 116.3(10) . . ? 
C61 C62 C63 107.6(11) . . ? 
C64 C63 C62 112.4(14) . . ? 
C77 N5 C73 107.3(9) . . ? 
C77 N5 C69 111.4(9) . . ? 
C73 N5 C69 110.7(9) . . ? 
C77 N5 C65 110.8(9) . . ? 
C73 N5 C65 109.8(9) . . ? 
C69 N5 C65 106.8(8) . . ? 
C66 C65 N5 114.3(10) . . ? 
C65 C66 C67 110.2(12) . . ? 
C68 C67 C66 108.5(14) . . ? 
C70 C69 N5 116.7(9) . . ? 
C69 C70 C71 110.1(9) . . ? 
C70 C71 C72 110.0(11) . . ? 
N5 C73 C74 115.9(10) . . ? 
C75 C74 C73 110.8(12) . . ? 
C76 C75 C74 111.1(13) . . ? 
N5 C77 C78 117.2(10) . . ? 
C77 C78 C79 109.3(10) . . ? 
C80 C79 C78 112.9(12) . . ? 
C93 N6 C89 113.8(10) . . ? 
C93 N6 C85 106.6(9) . . ? 
C89 N6 C85 110.9(10) . . ? 
C93 N6 C81 110.6(9) . . ? 
C89 N6 C81 104.4(8) . . ? 
C85 N6 C81 110.7(9) . . ? 
C82 C81 N6 114.4(9) . . ? 
C81 C82 C83 106.8(10) . . ? 
C84 C83 C82 112.5(13) . . ? 
C86 C85 N6 116.5(10) . . ? 
C85 C86 C87 107.4(10) . . ? 
C88 C87 C86 111.8(12) . . ? 
C90 C89 N6 113.9(10) . . ? 
C91 C90 C89 112.3(14) . . ? 
C92 C91 C90 111(2) . . ? 
C94 C93 N6 116.1(11) . . ? 
C93 C94 C95 111.5(13) . . ? 
C96 C95 C94 107.7(15) . . ? 
O1 P1 O3 114.5(5) . . ? 
O1 P1 O2 110.3(6) . . ? 
O3 P1 O2 109.1(4) . . ? 
O1 P1 O4 108.5(4) . . ? 
O3 P1 O4 108.7(5) . . ? 
O2 P1 O4 105.3(5) . . ? 
O5 P2 O6 113.3(6) . . ? 
O5 P2 O7 108.8(6) . . ? 
O6 P2 O7 110.0(5) . . ? 
O5 P2 O8 109.4(5) . . ? 
O6 P2 O8 108.1(5) . . ? 
O7 P2 O8 107.0(5) . . ? 
O10 P3 O12 113.5(5) . . ? 
O10 P3 O11 109.6(4) . . ? 
O12 P3 O11 109.6(5) . . ? 
O10 P3 O9 110.1(5) . . ? 
O12 P3 O9 108.4(4) . . ? 
O11 P3 O9 105.3(5) . . ? 
O15 P4 O13 113.7(5) . . ? 
O15 P4 O16 109.8(4) . . ? 
O13 P4 O16 109.5(5) . . ? 
O15 P4 O14 109.9(5) . . ? 
O13 P4 O14 109.4(4) . . ? 
O16 P4 O14 104.1(5) . . ? 
O18 P5 O19 115.2(7) . . ? 
O18 P5 O20 106.8(8) . . ? 
O19 P5 O20 109.3(5) . . ? 
O18 P5 O17 108.8(5) . . ? 
O19 P5 O17 108.1(6) . . ? 
O20 P5 O17 108.4(7) . . ? 
O21 P6 O24 112.6(7) . . ? 
O21 P6 O22 108.2(6) . . ? 
O24 P6 O22 118.5(8) . . ? 
O21 P6 O23 107.9(8) . . ? 
O24 P6 O23 108.8(6) . . ? 
O22 P6 O23 99.6(8) . . ? 
Cl1 C97 Cl2 113.6(9) . . ? 
Cl3 C98 Cl4 111.4(7) . . ? 
Cl5 C99 Cl6 110.9(10) . . ? 
Cl7 C100 Cl8 108.5(9) . . ? 
Cl9 C101 Cl10 111.7(8) . . ? 
Cl11 C102 Cl12 110.9(7) . . ? 
Cl13 C103 Cl14 110.4(8) . . ? 
Cl15 C104 Cl16 110.6(11) . . ? 
 
loop_ 
 _geom_hbond_atom_site_label_D 
 _geom_hbond_atom_site_label_H 
 _geom_hbond_atom_site_label_A 
 _geom_hbond_distance_DH 
 _geom_hbond_distance_HA 
 _geom_hbond_distance_DA 
 _geom_hbond_angle_DHA 
 _geom_hbond_site_symmetry_A 
O2 H02 O5  0.84 1.70 2.507(11) 160.4 . 
O4 H04 O1  0.84 1.66 2.484(10) 167.6 2_566 
O7 H07 O24  0.84 1.70 2.518(10) 162.7 . 
O8 H08 O3  0.84 1.71 2.525(9) 163.5 . 
O9 H09 O13  0.84 1.74 2.565(11) 165.6 . 
O11 H011 O10  0.84 1.71 2.521(10) 161.6 2_765 
O14 H014 O12  0.84 1.73 2.548(8) 165.1 . 
O16 H016 O18  0.84 1.78 2.532(13) 147.4 . 
O17 H017 O15  0.84 1.72 2.544(9) 167.3 . 
O20 H020 O21  0.84 1.68 2.448(12) 150.2 1_545 
O22 H022 O19  0.84 2.43 2.639(16) 95.2 1_565 
O23 H023 O6  0.84 1.70 2.455(14) 148.5 . 
 
_diffrn_measured_fraction_theta_max    0.964 
_diffrn_reflns_theta_full              23.25 
_diffrn_measured_fraction_theta_full   0.964 
_refine_diff_density_max    3.236 
_refine_diff_density_min   -1.658 
_refine_diff_density_rms    0.173 
