 
data_02sot007
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C68 H96 Cl4 N8 O4' 
_chemical_formula_weight          1231.33 
 
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    Pn
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 'x+1/2, -y, z+1/2' 
 
_cell_length_a                    13.2385(4) 
_cell_length_b                    16.9228(5) 
_cell_length_c                    15.0678(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  99.944(2) 
_cell_angle_gamma                 90.00 
_cell_volume                      3324.96(17) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     120(2) 
_cell_measurement_reflns_used     12049 
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        block 
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.15 
_exptl_crystal_size_mid           0.15 
_exptl_crystal_size_min           0.10 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.230 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1320 
_exptl_absorpt_coefficient_mu     0.231 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.9662 
_exptl_absorpt_correction_T_max   0.9773 
_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             19094 
_diffrn_reflns_av_R_equivalents   0.0588 
_diffrn_reflns_av_sigmaI/netI     0.0981 
_diffrn_reflns_limit_h_min        -15 
_diffrn_reflns_limit_h_max        14 
_diffrn_reflns_limit_k_min        -20 
_diffrn_reflns_limit_k_max        20 
_diffrn_reflns_limit_l_min        -17 
_diffrn_reflns_limit_l_max        17 
_diffrn_reflns_theta_min          3.00 
_diffrn_reflns_theta_max          25.03 
_reflns_number_total              10094 
_reflns_number_gt                 7453 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)'
_computing_cell_refinement        'DENZO & COLLECT'
_computing_data_reduction         'DENZO & COLLECT'
_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)+(0.0345P)²+0.0000P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.0034(4) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    -0.05(4) 
_refine_ls_number_reflns          10094 
_refine_ls_number_parameters      766 
_refine_ls_number_restraints      2 
_refine_ls_R_factor_all           0.0819 
_refine_ls_R_factor_gt            0.0476 
_refine_ls_wR_factor_ref          0.0984 
_refine_ls_wR_factor_gt           0.0868 
_refine_ls_goodness_of_fit_ref    0.988 
_refine_ls_restrained_S_all       0.987 
_refine_ls_shift/su_max           0.013 
_refine_ls_shift/su_mean          0.001 
 
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
C1 C 0.5584(3) 0.7204(2) 0.8172(2) 0.0283(10) Uani 1 1 d . . . 
H1 H 0.5821 0.6857 0.7756 0.034 Uiso 1 1 calc R . . 
C2 C 0.6223(3) 0.7400(2) 0.8973(3) 0.0343(10) Uani 1 1 d . . . 
H2 H 0.6903 0.7200 0.9092 0.041 Uiso 1 1 calc R . . 
C3 C 0.5885(3) 0.7880(2) 0.9597(3) 0.0324(10) Uani 1 1 d . . . 
H3 H 0.6321 0.8004 1.0148 0.039 Uiso 1 1 calc R . . 
C4 C 0.4909(3) 0.8178(2) 0.9411(2) 0.0304(10) Uani 1 1 d . . . 
H4 H 0.4672 0.8514 0.9836 0.036 Uiso 1 1 calc R . . 
C5 C 0.4266(3) 0.7998(2) 0.8615(2) 0.0256(9) Uani 1 1 d . . . 
H5 H 0.3590 0.8206 0.8500 0.031 Uiso 1 1 calc R . . 
C6 C 0.4604(3) 0.7513(2) 0.7979(2) 0.0241(9) Uani 1 1 d . . . 
C7 C 0.4162(3) 0.7099(2) 0.6365(2) 0.0223(9) Uani 1 1 d . . . 
C8 C 0.3246(3) 0.6968(2) 0.5673(2) 0.0205(9) Uani 1 1 d . . . 
C9 C 0.1614(3) 0.6916(2) 0.5102(2) 0.0204(9) Uani 1 1 d . . . 
C10 C 0.2146(3) 0.6759(2) 0.4400(2) 0.0222(9) Uani 1 1 d . . . 
C11 C 0.3186(3) 0.6799(2) 0.4761(2) 0.0208(9) Uani 1 1 d . . . 
C12 C 0.0507(3) 0.6955(2) 0.5090(2) 0.0207(9) Uani 1 1 d . . . 
C13 C -0.0733(3) 0.7263(2) 0.6134(2) 0.0238(9) Uani 1 1 d . . . 
C14 C -0.0773(3) 0.7635(2) 0.6952(3) 0.0306(10) Uani 1 1 d . . . 
H14 H -0.0159 0.7805 0.7326 0.037 Uiso 1 1 calc R . . 
C15 C -0.1714(3) 0.7755(2) 0.7216(3) 0.0359(10) Uani 1 1 d . . . 
H15 H -0.1743 0.8008 0.7774 0.043 Uiso 1 1 calc R . . 
C16 C -0.2609(3) 0.7513(2) 0.6676(3) 0.0362(11) Uani 1 1 d . . . 
H16 H -0.3253 0.7608 0.6851 0.043 Uiso 1 1 calc R . . 
C17 C -0.2555(3) 0.7130(2) 0.5879(3) 0.0330(10) Uani 1 1 d . . . 
H17 H -0.3170 0.6952 0.5513 0.040 Uiso 1 1 calc R . . 
C18 C -0.1617(3) 0.6996(2) 0.5595(3) 0.0261(9) Uani 1 1 d . . . 
H18 H -0.1590 0.6728 0.5046 0.031 Uiso 1 1 calc R . . 
C53 C 0.8669(3) 0.4658(2) 0.7210(2) 0.0235(9) Uani 1 1 d . . . 
H53A H 0.8102 0.4469 0.7506 0.028 Uiso 1 1 calc R . . 
H53B H 0.9292 0.4360 0.7472 0.028 Uiso 1 1 calc R . . 
C54 C 0.8850(3) 0.5524(2) 0.7433(2) 0.0263(9) Uani 1 1 d . . . 
H54A H 0.8297 0.5844 0.7078 0.032 Uiso 1 1 calc R . . 
H54B H 0.9511 0.5691 0.7269 0.032 Uiso 1 1 calc R . . 
C55 C 0.8872(3) 0.5667(2) 0.8438(2) 0.0293(10) Uani 1 1 d . . . 
H55A H 0.9354 0.5288 0.8788 0.035 Uiso 1 1 calc R . . 
H55B H 0.9135 0.6207 0.8593 0.035 Uiso 1 1 calc R . . 
C56 C 0.7832(3) 0.5581(2) 0.8713(3) 0.0355(10) Uani 1 1 d . . . 
H56A H 0.7334 0.5916 0.8329 0.053 Uiso 1 1 calc R . . 
H56B H 0.7876 0.5741 0.9344 0.053 Uiso 1 1 calc R . . 
H56C H 0.7611 0.5028 0.8645 0.053 Uiso 1 1 calc R . . 
C57 C 0.7453(3) 0.4901(2) 0.5774(2) 0.0209(9) Uani 1 1 d . . . 
H57A H 0.7266 0.4714 0.5144 0.025 Uiso 1 1 calc R . . 
H57B H 0.7625 0.5469 0.5751 0.025 Uiso 1 1 calc R . . 
C58 C 0.6516(3) 0.4822(2) 0.6223(2) 0.0281(10) Uani 1 1 d . . . 
H58A H 0.6418 0.4262 0.6379 0.034 Uiso 1 1 calc R . . 
H58B H 0.6613 0.5136 0.6786 0.034 Uiso 1 1 calc R . . 
C59 C 0.5589(3) 0.5114(2) 0.5589(2) 0.0323(10) Uani 1 1 d . . . 
H59A H 0.5522 0.4809 0.5022 0.039 Uiso 1 1 calc R . . 
H59B H 0.5701 0.5674 0.5442 0.039 Uiso 1 1 calc R . . 
C60 C 0.4597(3) 0.5052(2) 0.5950(3) 0.0310(10) Uani 1 1 d . . . 
H60A H 0.4479 0.4500 0.6100 0.046 Uiso 1 1 calc R . . 
H60B H 0.4030 0.5237 0.5492 0.046 Uiso 1 1 calc R . . 
H60C H 0.4640 0.5378 0.6493 0.046 Uiso 1 1 calc R . . 
C61 C 0.8170(3) 0.3583(2) 0.6112(2) 0.0233(9) Uani 1 1 d . . . 
H61A H 0.7649 0.3455 0.6489 0.028 Uiso 1 1 calc R . . 
H61B H 0.7855 0.3481 0.5478 0.028 Uiso 1 1 calc R . . 
C62 C 0.9057(3) 0.3023(2) 0.6360(3) 0.0325(10) Uani 1 1 d . . . 
H62A H 0.9412 0.3139 0.6980 0.039 Uiso 1 1 calc R . . 
H62B H 0.9553 0.3102 0.5946 0.039 Uiso 1 1 calc R . . 
C63 C 0.8695(3) 0.2174(2) 0.6306(3) 0.0319(10) Uani 1 1 d . . . 
H63A H 0.9302 0.1823 0.6401 0.038 Uiso 1 1 calc R . . 
H63B H 0.8313 0.2073 0.5691 0.038 Uiso 1 1 calc R . . 
C64 C 0.8006(4) 0.1956(2) 0.6990(3) 0.0410(11) Uani 1 1 d . . . 
H64A H 0.8326 0.2138 0.7591 0.061 Uiso 1 1 calc R . . 
H64B H 0.7918 0.1381 0.6998 0.061 Uiso 1 1 calc R . . 
H64C H 0.7336 0.2210 0.6818 0.061 Uiso 1 1 calc R . . 
C65 C 0.9280(3) 0.4701(2) 0.5751(2) 0.0240(9) Uani 1 1 d . . . 
H65A H 0.9901 0.4409 0.6033 0.029 Uiso 1 1 calc R . . 
H65B H 0.9417 0.5271 0.5865 0.029 Uiso 1 1 calc R . . 
C66 C 0.9122(3) 0.4563(2) 0.4741(2) 0.0300(10) Uani 1 1 d . . . 
H66A H 0.8920 0.4007 0.4610 0.036 Uiso 1 1 calc R . . 
H66B H 0.8558 0.4905 0.4440 0.036 Uiso 1 1 calc R . . 
C67 C 1.0089(3) 0.4742(2) 0.4369(2) 0.0291(10) Uani 1 1 d . . . 
H67A H 1.0596 0.4315 0.4542 0.035 Uiso 1 1 calc R . . 
H67B H 1.0392 0.5244 0.4628 0.035 Uiso 1 1 calc R . . 
C68 C 0.9847(3) 0.4810(2) 0.3343(2) 0.0345(10) Uani 1 1 d . . . 
H68A H 0.9497 0.4329 0.3090 0.052 Uiso 1 1 calc R . . 
H68B H 1.0486 0.4876 0.3106 0.052 Uiso 1 1 calc R . . 
H68C H 0.9402 0.5268 0.3174 0.052 Uiso 1 1 calc R . . 
N1 N 0.3922(2) 0.73402(17) 0.71770(18) 0.0232(7) Uani 1 1 d . . . 
H1A H 0.3265 0.7393 0.7197 0.028 Uiso 1 1 calc R . . 
N2 N 0.2288(2) 0.70454(16) 0.58764(18) 0.0198(7) Uani 1 1 d . . . 
N3 N 0.0264(2) 0.71747(16) 0.59057(19) 0.0212(7) Uani 1 1 d . . . 
H3A H 0.0785 0.7273 0.6339 0.025 Uiso 1 1 calc R . . 
N8 N 0.8407(2) 0.44614(16) 0.62115(18) 0.0210(7) Uani 1 1 d . . . 
O1 O 0.5042(2) 0.69959(15) 0.62373(16) 0.0302(7) Uani 1 1 d . . . 
O2 O -0.0134(2) 0.68166(14) 0.44229(16) 0.0273(6) Uani 1 1 d . . . 
Cl1 Cl 0.41730(7) 0.66837(6) 0.41544(6) 0.0305(2) Uani 1 1 d . . . 
Cl2 Cl 0.16460(8) 0.65831(5) 0.32786(6) 0.0297(2) Uani 1 1 d . . . 
C19 C 0.1557(3) 0.4836(2) 0.8058(2) 0.0262(9) Uani 1 1 d . . . 
H19 H 0.1337 0.4999 0.8597 0.031 Uiso 1 1 calc R . . 
C20 C 0.1589(3) 0.4046(2) 0.7860(3) 0.0360(11) Uani 1 1 d . . . 
H20 H 0.1408 0.3665 0.8269 0.043 Uiso 1 1 calc R . . 
C21 C 0.1886(3) 0.3799(2) 0.7060(3) 0.0337(10) Uani 1 1 d . . . 
H21 H 0.1900 0.3253 0.6917 0.040 Uiso 1 1 calc R . . 
C22 C 0.2159(3) 0.4357(2) 0.6478(3) 0.0293(10) Uani 1 1 d . . . 
H22 H 0.2362 0.4193 0.5932 0.035 Uiso 1 1 calc R . . 
C23 C 0.2142(3) 0.5146(2) 0.6680(3) 0.0271(9) Uani 1 1 d . . . 
H23 H 0.2336 0.5522 0.6274 0.033 Uiso 1 1 calc R . . 
C24 C 0.1844(3) 0.5402(2) 0.7477(2) 0.0234(9) Uani 1 1 d . . . 
C25 C 0.1663(3) 0.6607(2) 0.8390(2) 0.0248(9) Uani 1 1 d . . . 
C26 C 0.1636(3) 0.7470(2) 0.8308(2) 0.0233(9) Uani 1 1 d . . . 
C27 C 0.1679(3) 0.8631(2) 0.7675(2) 0.0227(9) Uani 1 1 d . . . 
C28 C 0.1421(3) 0.8755(2) 0.8521(2) 0.0268(9) Uani 1 1 d . . . 
C29 C 0.1401(3) 0.8029(2) 0.8923(2) 0.0253(9) Uani 1 1 d . . . 
C30 C 0.1835(3) 0.9215(2) 0.6991(2) 0.0253(9) Uani 1 1 d . . . 
C31 C 0.2467(3) 0.9330(2) 0.5531(2) 0.0228(9) Uani 1 1 d . . . 
C32 C 0.2867(3) 0.8891(2) 0.4897(2) 0.0331(11) Uani 1 1 d . . . 
H32 H 0.2872 0.8331 0.4938 0.040 Uiso 1 1 calc R . . 
C33 C 0.3259(4) 0.9251(2) 0.4207(3) 0.0430(12) Uani 1 1 d . . . 
H33 H 0.3534 0.8940 0.3782 0.052 Uiso 1 1 calc R . . 
C34 C 0.3249(4) 1.0057(2) 0.4139(3) 0.0406(12) Uani 1 1 d . . . 
H34 H 0.3521 1.0308 0.3667 0.049 Uiso 1 1 calc R . . 
C35 C 0.2845(3) 1.0501(2) 0.4753(3) 0.0373(11) Uani 1 1 d . . . 
H35 H 0.2830 1.1060 0.4699 0.045 Uiso 1 1 calc R . . 
C36 C 0.2459(3) 1.0146(2) 0.5452(3) 0.0322(10) Uani 1 1 d . . . 
H36 H 0.2188 1.0461 0.5877 0.039 Uiso 1 1 calc R . . 
N4 N 0.1826(2) 0.62218(17) 0.76231(19) 0.0247(8) Uani 1 1 d . . . 
H4A H 0.1932 0.6523 0.7172 0.030 Uiso 1 1 calc R . . 
N5 N 0.1801(2) 0.78412(16) 0.75426(18) 0.0217(7) Uani 1 1 d . . . 
N6 N 0.2125(2) 0.89134(17) 0.62256(19) 0.0274(8) Uani 1 1 d . . . 
H6 H 0.2092 0.8396 0.6165 0.033 Uiso 1 1 calc R . . 
O3 O 0.1548(2) 0.62647(15) 0.90791(16) 0.0335(7) Uani 1 1 d . . . 
O4 O 0.1712(2) 0.99286(16) 0.71015(17) 0.0380(7) Uani 1 1 d . . . 
Cl3 Cl 0.10948(9) 0.78736(6) 0.99745(6) 0.0417(3) Uani 1 1 d . . . 
Cl4 Cl 0.11754(9) 0.96402(6) 0.90210(7) 0.0434(3) Uani 1 1 d . . . 
C37 C 0.9860(4) 0.8963(2) 0.4256(3) 0.0416(12) Uani 1 1 d . . . 
H37A H 0.9764 0.8447 0.4539 0.050 Uiso 1 1 calc R . . 
H37B H 1.0598 0.9014 0.4227 0.050 Uiso 1 1 calc R . . 
C38 C 0.9584(4) 0.9606(3) 0.4868(3) 0.0577(15) Uani 1 1 d . . . 
H38A H 1.0203 0.9929 0.5072 0.069 Uiso 1 1 calc R . . 
H38B H 0.9067 0.9954 0.4509 0.069 Uiso 1 1 calc R . . 
C39 C 0.9196(5) 0.9354(3) 0.5634(3) 0.081(2) Uani 1 1 d . . . 
H39A H 0.9704 0.8990 0.5977 0.097 Uiso 1 1 calc R . . 
H39B H 0.8566 0.9044 0.5424 0.097 Uiso 1 1 calc R . . 
C40 C 0.8942(5) 0.9973(3) 0.6275(3) 0.0624(15) Uani 1 1 d . . . 
H40A H 0.9569 1.0254 0.6540 0.094 Uiso 1 1 calc R . . 
H40B H 0.8643 0.9719 0.6755 0.094 Uiso 1 1 calc R . . 
H40C H 0.8449 1.0348 0.5950 0.094 Uiso 1 1 calc R . . 
C41 C 0.8133(4) 0.8898(2) 0.3292(3) 0.0381(11) Uani 1 1 d . . . 
H41A H 0.7773 0.8972 0.2665 0.046 Uiso 1 1 calc R . . 
H41B H 0.7932 0.9339 0.3656 0.046 Uiso 1 1 calc R . . 
C42 C 0.7770(4) 0.8133(2) 0.3648(3) 0.0382(11) Uani 1 1 d . . . 
H42A H 0.8226 0.7992 0.4218 0.046 Uiso 1 1 calc R . . 
H42B H 0.7812 0.7705 0.3208 0.046 Uiso 1 1 calc R . . 
C43 C 0.6666(4) 0.8199(3) 0.3816(3) 0.0449(12) Uani 1 1 d . . . 
H43A H 0.6481 0.7705 0.4103 0.054 Uiso 1 1 calc R . . 
H43B H 0.6623 0.8638 0.4242 0.054 Uiso 1 1 calc R . . 
C44 C 0.5903(4) 0.8341(3) 0.2967(3) 0.0472(12) Uani 1 1 d . . . 
H44A H 0.6042 0.8853 0.2709 0.071 Uiso 1 1 calc R . . 
H44B H 0.5207 0.8342 0.3107 0.071 Uiso 1 1 calc R . . 
H44C H 0.5963 0.7921 0.2531 0.071 Uiso 1 1 calc R . . 
C45 C 0.9639(3) 0.8230(2) 0.2840(2) 0.0310(10) Uani 1 1 d . . . 
H45A H 1.0388 0.8281 0.2858 0.037 Uiso 1 1 calc R . . 
H45B H 0.9525 0.7753 0.3190 0.037 Uiso 1 1 calc R . . 
C46 C 0.9129(4) 0.8106(2) 0.1872(3) 0.0363(11) Uani 1 1 d . . . 
H46A H 0.9318 0.8545 0.1498 0.044 Uiso 1 1 calc R . . 
H46B H 0.8375 0.8115 0.1835 0.044 Uiso 1 1 calc R . . 
C47 C 0.9439(3) 0.7328(2) 0.1497(2) 0.0312(10) Uani 1 1 d . . . 
H47A H 1.0183 0.7338 0.1478 0.037 Uiso 1 1 calc R . . 
H47B H 0.9309 0.6892 0.1901 0.037 Uiso 1 1 calc R . . 
C48 C 0.8851(4) 0.7177(2) 0.0562(3) 0.0418(12) Uani 1 1 d . . . 
H48A H 0.8116 0.7149 0.0583 0.063 Uiso 1 1 calc R . . 
H48B H 0.9076 0.6675 0.0336 0.063 Uiso 1 1 calc R . . 
H48C H 0.8978 0.7607 0.0161 0.063 Uiso 1 1 calc R . . 
C49 C 0.9480(4) 0.9706(2) 0.2807(3) 0.0405(12) Uani 1 1 d . . . 
H49A H 0.9092 0.9679 0.2184 0.049 Uiso 1 1 calc R . . 
H49B H 0.9207 1.0158 0.3109 0.049 Uiso 1 1 calc R . . 
C50 C 1.0596(5) 0.9868(3) 0.2762(4) 0.0721(17) Uani 1 1 d . . . 
H50A H 1.0984 0.9919 0.3383 0.087 Uiso 1 1 calc R . . 
H50B H 1.0880 0.9410 0.2478 0.087 Uiso 1 1 calc R . . 
C51 C 1.0756(5) 1.0608(3) 0.2237(4) 0.0805(19) Uani 1 1 d . . . 
H51A H 1.0360 1.1046 0.2446 0.097 Uiso 1 1 calc R . . 
H51B H 1.1491 1.0755 0.2371 0.097 Uiso 1 1 calc R . . 
C52 C 1.0471(8) 1.0531(5) 0.1330(5) 0.158(4) Uani 1 1 d . . . 
H52A H 1.0546 0.9978 0.1159 0.236 Uiso 1 1 calc R . . 
H52B H 1.0907 1.0866 0.1024 0.236 Uiso 1 1 calc R . . 
H52C H 0.9754 1.0693 0.1154 0.236 Uiso 1 1 calc R . . 
N7 N 0.9272(3) 0.89456(17) 0.3302(2) 0.0322(9) Uani 1 1 d . . . 
 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
C1 C6 1.383(5) . ? 
C1 C2 1.390(5) . ? 
C2 C3 1.374(5) . ? 
C3 C4 1.370(5) . ? 
C4 C5 1.379(5) . ? 
C5 C6 1.394(5) . ? 
C6 N1 1.409(4) . ? 
C7 O1 1.226(4) . ? 
C7 N1 1.378(4) . ? 
C7 C8 1.473(5) . ? 
C8 N2 1.361(4) . ? 
C8 C11 1.393(5) . ? 
C9 N2 1.358(4) . ? 
C9 C10 1.393(5) . ? 
C9 C12 1.465(5) . ? 
C10 C11 1.392(5) . ? 
C10 Cl2 1.731(4) . ? 
C11 Cl1 1.729(4) . ? 
C12 O2 1.221(4) . ? 
C12 N3 1.374(4) . ? 
C13 C18 1.381(5) . ? 
C13 C14 1.394(5) . ? 
C13 N3 1.428(4) . ? 
C14 C15 1.387(5) . ? 
C15 C16 1.379(6) . ? 
C16 C17 1.376(5) . ? 
C17 C18 1.400(5) . ? 
C53 C54 1.513(5) . ? 
C53 N8 1.521(4) . ? 
C54 C55 1.529(5) . ? 
C55 C56 1.512(5) . ? 
C57 N8 1.516(4) . ? 
C57 C58 1.519(5) . ? 
C58 C59 1.502(5) . ? 
C59 C60 1.509(5) . ? 
C61 C62 1.505(5) . ? 
C61 N8 1.521(4) . ? 
C62 C63 1.513(5) . ? 
C63 C64 1.534(5) . ? 
C65 N8 1.504(4) . ? 
C65 C66 1.518(5) . ? 
C66 C67 1.515(5) . ? 
C67 C68 1.528(5) . ? 
C19 C20 1.373(5) . ? 
C19 C24 1.395(5) . ? 
C20 C21 1.395(5) . ? 
C21 C22 1.378(5) . ? 
C22 C23 1.370(5) . ? 
C23 C24 1.396(5) . ? 
C24 N4 1.405(4) . ? 
C25 O3 1.222(4) . ? 
C25 N4 1.376(4) . ? 
C25 C26 1.466(5) . ? 
C26 N5 1.363(4) . ? 
C26 C29 1.396(5) . ? 
C27 N5 1.366(4) . ? 
C27 C28 1.392(5) . ? 
C27 C30 1.467(5) . ? 
C28 C29 1.371(5) . ? 
C28 Cl4 1.733(4) . ? 
C29 Cl3 1.723(3) . ? 
C30 O4 1.234(4) . ? 
C30 N6 1.375(4) . ? 
C31 C32 1.385(5) . ? 
C31 C36 1.385(5) . ? 
C31 N6 1.401(4) . ? 
C32 C33 1.381(5) . ? 
C33 C34 1.367(6) . ? 
C34 C35 1.371(6) . ? 
C35 C36 1.385(5) . ? 
C37 C38 1.511(5) . ? 
C37 N7 1.512(5) . ? 
C38 C39 1.407(6) . ? 
C39 C40 1.502(6) . ? 
C41 N7 1.508(5) . ? 
C41 C42 1.511(5) . ? 
C42 C43 1.530(6) . ? 
C43 C44 1.507(6) . ? 
C45 C46 1.513(5) . ? 
C45 N7 1.518(4) . ? 
C46 C47 1.516(5) . ? 
C47 C48 1.509(5) . ? 
C49 C50 1.517(7) . ? 
C49 N7 1.535(5) . ? 
C50 C51 1.516(7) . ? 
C51 C52 1.360(8) . ? 
 
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
C6 C1 C2 120.0(4) . . ? 
C3 C2 C1 121.0(4) . . ? 
C4 C3 C2 119.0(4) . . ? 
C3 C4 C5 121.0(4) . . ? 
C4 C5 C6 120.3(4) . . ? 
C1 C6 C5 118.7(3) . . ? 
C1 C6 N1 122.8(3) . . ? 
C5 C6 N1 118.5(3) . . ? 
O1 C7 N1 123.6(3) . . ? 
O1 C7 C8 123.8(3) . . ? 
N1 C7 C8 112.6(3) . . ? 
N2 C8 C11 110.2(3) . . ? 
N2 C8 C7 120.8(3) . . ? 
C11 C8 C7 128.9(4) . . ? 
N2 C9 C10 109.9(3) . . ? 
N2 C9 C12 120.7(3) . . ? 
C10 C9 C12 129.5(3) . . ? 
C11 C10 C9 106.9(3) . . ? 
C11 C10 Cl2 125.1(3) . . ? 
C9 C10 Cl2 128.0(3) . . ? 
C10 C11 C8 106.2(3) . . ? 
C10 C11 Cl1 125.1(3) . . ? 
C8 C11 Cl1 128.7(3) . . ? 
O2 C12 N3 123.5(3) . . ? 
O2 C12 C9 123.6(3) . . ? 
N3 C12 C9 112.9(3) . . ? 
C18 C13 C14 120.7(4) . . ? 
C18 C13 N3 123.3(3) . . ? 
C14 C13 N3 116.0(3) . . ? 
C15 C14 C13 119.6(4) . . ? 
C16 C15 C14 120.6(4) . . ? 
C17 C16 C15 119.1(4) . . ? 
C16 C17 C18 121.7(4) . . ? 
C13 C18 C17 118.3(4) . . ? 
C54 C53 N8 115.6(3) . . ? 
C53 C54 C55 110.4(3) . . ? 
C56 C55 C54 113.2(3) . . ? 
N8 C57 C58 116.5(3) . . ? 
C59 C58 C57 109.1(3) . . ? 
C58 C59 C60 114.4(3) . . ? 
C62 C61 N8 116.9(3) . . ? 
C61 C62 C63 111.0(3) . . ? 
C62 C63 C64 114.3(3) . . ? 
N8 C65 C66 115.9(3) . . ? 
C67 C66 C65 111.2(3) . . ? 
C66 C67 C68 110.3(3) . . ? 
C7 N1 C6 127.7(3) . . ? 
C9 N2 C8 106.8(3) . . ? 
C12 N3 C13 127.7(3) . . ? 
C65 N8 C57 108.4(3) . . ? 
C65 N8 C61 112.4(3) . . ? 
C57 N8 C61 107.1(3) . . ? 
C65 N8 C53 109.6(3) . . ? 
C57 N8 C53 110.7(3) . . ? 
C61 N8 C53 108.6(3) . . ? 
C20 C19 C24 120.7(4) . . ? 
C19 C20 C21 120.3(4) . . ? 
C22 C21 C20 119.2(4) . . ? 
C23 C22 C21 120.7(4) . . ? 
C22 C23 C24 120.8(4) . . ? 
C19 C24 C23 118.3(3) . . ? 
C19 C24 N4 124.5(3) . . ? 
C23 C24 N4 117.2(3) . . ? 
O3 C25 N4 123.3(3) . . ? 
O3 C25 C26 122.6(3) . . ? 
N4 C25 C26 114.0(3) . . ? 
N5 C26 C29 109.7(3) . . ? 
N5 C26 C25 121.7(3) . . ? 
C29 C26 C25 128.6(3) . . ? 
N5 C27 C28 109.6(3) . . ? 
N5 C27 C30 121.5(3) . . ? 
C28 C27 C30 129.0(3) . . ? 
C29 C28 C27 107.2(3) . . ? 
C29 C28 Cl4 124.3(3) . . ? 
C27 C28 Cl4 128.5(3) . . ? 
C28 C29 C26 106.9(3) . . ? 
C28 C29 Cl3 124.7(3) . . ? 
C26 C29 Cl3 128.4(3) . . ? 
O4 C30 N6 122.6(3) . . ? 
O4 C30 C27 121.7(3) . . ? 
N6 C30 C27 115.7(3) . . ? 
C32 C31 C36 118.3(3) . . ? 
C32 C31 N6 117.1(3) . . ? 
C36 C31 N6 124.5(3) . . ? 
C33 C32 C31 121.3(4) . . ? 
C34 C33 C32 119.8(4) . . ? 
C33 C34 C35 119.7(4) . . ? 
C34 C35 C36 120.9(4) . . ? 
C35 C36 C31 119.9(4) . . ? 
C25 N4 C24 127.5(3) . . ? 
C26 N5 C27 106.7(3) . . ? 
C30 N6 C31 127.8(3) . . ? 
C38 C37 N7 117.1(4) . . ? 
C39 C38 C37 116.3(4) . . ? 
C38 C39 C40 118.1(4) . . ? 
N7 C41 C42 114.9(3) . . ? 
C41 C42 C43 111.6(3) . . ? 
C44 C43 C42 113.0(4) . . ? 
C46 C45 N7 115.4(3) . . ? 
C45 C46 C47 112.0(3) . . ? 
C48 C47 C46 111.5(3) . . ? 
C50 C49 N7 115.5(4) . . ? 
C51 C50 C49 113.5(5) . . ? 
C52 C51 C50 113.9(5) . . ? 
C41 N7 C37 111.1(3) . . ? 
C41 N7 C45 110.6(3) . . ? 
C37 N7 C45 107.4(3) . . ? 
C41 N7 C49 107.6(3) . . ? 
C37 N7 C49 109.8(3) . . ? 
C45 N7 C49 110.3(3) . . ? 
 
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 
N1 H1A N5  0.88 2.22 3.072(4) 161.5 . 
N3 H3A N5  0.88 2.28 3.124(4) 161.9 . 
N4 H4A N2  0.88 2.27 3.130(4) 167.4 . 
N6 H6 N2  0.88 2.35 3.218(4) 168.9 . 
 
_diffrn_measured_fraction_theta_max    0.991 
_diffrn_reflns_theta_full              25.03 
_diffrn_measured_fraction_theta_full   0.991 
_refine_diff_density_max    0.325 
_refine_diff_density_min   -0.226 
_refine_diff_density_rms    0.051 
