 
data_s 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C131 H164 Cl3 O20' 
_chemical_formula_weight          2164.97 
 
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' 
 'Cl'  'Cl'   0.1484   0.1585 
 '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' 
 'H'  'H'   0.0000   0.0000 
 '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)/n'  
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x-1/2, -y-1/2, z-1/2' 
 
_cell_length_a                    11.6711(4) 
_cell_length_b                    21.5510(6) 
_cell_length_c                    23.8501(8) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  95.3210(10) 
_cell_angle_gamma                 90.00 
_cell_volume                      5973.0(3) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     273(2) 
_cell_measurement_reflns_used     9913   
_cell_measurement_theta_min       3.01 
_cell_measurement_theta_max       26.35 
 
_exptl_crystal_description        BLOCK
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           ? 
_exptl_crystal_size_mid           ? 
_exptl_crystal_size_min           ? 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.204 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              2322 
_exptl_absorpt_coefficient_mu     0.144 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       273(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   'CCD area detector'   
_diffrn_measurement_method        'phi and omega scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             30634 
_diffrn_reflns_av_R_equivalents   0.0462 
_diffrn_reflns_av_sigmaI/netI     0.0410 
_diffrn_reflns_limit_h_min        -13 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        -25 
_diffrn_reflns_limit_k_max        25 
_diffrn_reflns_limit_l_min        -28 
_diffrn_reflns_limit_l_max        23 
_diffrn_reflns_theta_min          2.96 
_diffrn_reflns_theta_max          25.00 
_reflns_number_total              10457 
_reflns_number_gt                 7689 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.0924P)²+5.4516P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          10457 
_refine_ls_number_parameters      706 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0944 
_refine_ls_R_factor_gt            0.0672 
_refine_ls_wR_factor_ref          0.1885 
_refine_ls_wR_factor_gt           0.1723 
_refine_ls_goodness_of_fit_ref    1.075 
_refine_ls_restrained_S_all       1.075 
_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 
Cl1 Cl 1.12492(14) 0.30954(7) 0.67973(8) 0.1101(5) Uani 1 1 d . . . 
O8 O 0.33539(14) 0.45300(8) 0.56176(7) 0.0240(4) Uani 1 1 d . . . 
O3 O 0.79360(15) 0.16121(9) 0.80906(7) 0.0259(4) Uani 1 1 d . . . 
O7 O 0.37666(15) 0.46811(9) 0.76714(7) 0.0268(4) Uani 1 1 d . . . 
O5 O 0.76265(14) 0.48761(9) 0.64903(7) 0.0236(4) Uani 1 1 d . . . 
O9 O 0.30300(15) 0.22497(9) 0.51992(8) 0.0267(4) Uani 1 1 d . . . 
O1 O 0.70674(15) 0.32785(8) 0.48593(8) 0.0257(4) Uani 1 1 d . . . 
O2 O 0.72847(15) 0.12548(9) 0.59135(8) 0.0298(4) Uani 1 1 d . . . 
Cl2 Cl 0.75394(15) 0.49695(10) 0.03849(8) 0.0782(5) Uani 0.50 1 d P . . 
C8 C 0.75394(15) 0.49695(10) 0.03849(8) 0.0782(5) Uani 0.50 1 d P . . 
H8A H 0.7927 0.4688 0.0154 0.117 Uiso 1 1 calc R . . 
H8B H 0.7642 0.4835 0.0770 0.117 Uiso 1 1 calc R . . 
H8C H 0.7855 0.5378 0.0355 0.117 Uiso 1 1 calc R . . 
O10 O 0.36011(15) 0.10461(9) 0.70802(8) 0.0293(4) Uani 1 1 d . . . 
O6 O 0.39987(15) 0.25107(9) 0.85124(9) 0.0328(5) Uani 1 1 d . . . 
O4 O 0.79666(15) 0.39257(9) 0.86278(8) 0.0307(5) Uani 1 1 d . . . 
C12 C 0.5344(2) 0.44750(11) 0.55288(9) 0.0170(5) Uani 1 1 d . . . 
C13 C 0.4910(2) 0.27058(11) 0.46830(10) 0.0202(5) Uani 1 1 d . . . 
H13A H 0.5477 0.2641 0.4416 0.024 Uiso 1 1 calc R . . 
H13B H 0.4152 0.2682 0.4479 0.024 Uiso 1 1 calc R . . 
C14 C 0.5951(2) 0.38642(12) 0.84348(9) 0.0197(5) Uani 1 1 d . . . 
C15 C 0.4639(2) 0.48795(11) 0.67952(10) 0.0186(5) Uani 1 1 d . . . 
H15 H 0.3918 0.4940 0.6603 0.022 Uiso 1 1 calc R . . 
C16 C 0.4131(2) 0.36487(11) 0.51359(10) 0.0181(5) Uani 1 1 d . . . 
H16 H 0.3402 0.3476 0.5068 0.022 Uiso 1 1 calc R . . 
C17 C 0.7012(2) 0.29266(12) 0.86775(10) 0.0220(5) Uani 1 1 d . . . 
H17 H 0.7717 0.2732 0.8767 0.026 Uiso 1 1 calc R . . 
C18 C 0.6280(2) 0.41776(12) 0.53278(10) 0.0197(5) Uani 1 1 d . . . 
H18 H 0.7005 0.4357 0.5385 0.024 Uiso 1 1 calc R . . 
C19 C 0.4259(2) 0.42054(11) 0.54225(9) 0.0172(5) Uani 1 1 d . . . 
C20 C 0.5621(2) 0.10680(11) 0.70299(10) 0.0183(5) Uani 1 1 d . . . 
C21 C 0.5076(2) 0.33405(11) 0.49467(9) 0.0172(5) Uani 1 1 d . . . 
C22 C 0.5029(2) 0.22010(11) 0.51296(10) 0.0181(5) Uani 1 1 d . . . 
C23 C 0.6688(2) 0.48326(11) 0.68002(10) 0.0180(5) Uani 1 1 d . . . 
C24 C 0.4942(2) 0.35103(12) 0.84097(10) 0.0220(5) Uani 1 1 d . . . 
H24 H 0.4237 0.3704 0.8318 0.026 Uiso 1 1 calc R . . 
C25 C 0.6149(2) 0.36158(11) 0.50420(10) 0.0183(5) Uani 1 1 d . . . 
C26 C 0.5508(2) 0.50623(11) 0.58759(10) 0.0185(5) Uani 1 1 d . . . 
H26A H 0.4858 0.5336 0.5784 0.022 Uiso 1 1 calc R . . 
H26B H 0.6196 0.5274 0.5780 0.022 Uiso 1 1 calc R . . 
C27 C 0.4719(2) 0.47444(11) 0.73658(10) 0.0188(5) Uani 1 1 d . . . 
C28 C 0.6766(2) 0.47165(11) 0.73765(10) 0.0179(5) Uani 1 1 d . . . 
H28 H 0.7487 0.4666 0.7572 0.022 Uiso 1 1 calc R . . 
C29 C 0.6717(2) 0.12055(11) 0.72822(10) 0.0199(5) Uani 1 1 d . . . 
H29 H 0.7353 0.1128 0.7085 0.024 Uiso 1 1 calc R . . 
C30 C 0.4684(2) 0.11819(12) 0.73405(10) 0.0210(5) Uani 1 1 d . . . 
C31 C 0.5292(2) 0.12942(11) 0.59848(10) 0.0194(5) Uani 1 1 d . . . 
C32 C 0.5788(2) 0.46747(11) 0.76674(10) 0.0181(5) Uani 1 1 d . . . 
C33 C 0.5614(2) 0.49259(11) 0.65050(10) 0.0171(5) Uani 1 1 d . . . 
C34 C 0.4077(2) 0.19915(12) 0.53930(10) 0.0195(5) Uani 1 1 d . . . 
C35 C 0.4848(2) 0.14156(11) 0.78828(11) 0.0228(6) Uani 1 1 d . . . 
H35 H 0.4214 0.1473 0.8087 0.027 Uiso 1 1 calc R . . 
C36 C 0.6097(2) 0.19533(11) 0.53007(10) 0.0211(5) Uani 1 1 d . . . 
H36 H 0.6737 0.2086 0.5128 0.025 Uiso 1 1 calc R . . 
C37 C 0.6019(2) 0.25742(12) 0.86395(10) 0.0202(5) Uani 1 1 d . . . 
C38 C 0.6236(2) 0.15104(11) 0.57241(10) 0.0205(5) Uani 1 1 d . . . 
C39 C 0.5439(2) 0.08055(11) 0.64415(10) 0.0199(5) Uani 1 1 d . . . 
H39A H 0.4761 0.0543 0.6415 0.024 Uiso 1 1 calc R . . 
H39B H 0.6093 0.0547 0.6375 0.024 Uiso 1 1 calc R . . 
C40 C 0.6882(2) 0.14569(11) 0.78216(10) 0.0204(5) Uani 1 1 d . . . 
C41 C 0.5897(2) 0.45489(11) 0.82988(10) 0.0207(5) Uani 1 1 d . . . 
H41A H 0.6588 0.4749 0.8470 0.025 Uiso 1 1 calc R . . 
H41B H 0.5244 0.4731 0.8462 0.025 Uiso 1 1 calc R . . 
C42 C 0.5937(2) 0.15655(11) 0.81291(10) 0.0195(5) Uani 1 1 d . . . 
C43 C 0.6988(2) 0.35656(12) 0.85860(10) 0.0218(5) Uani 1 1 d . . . 
C44 C 0.4218(2) 0.15419(11) 0.58114(10) 0.0196(5) Uani 1 1 d . . . 
H44 H 0.3578 0.1403 0.5980 0.023 Uiso 1 1 calc R . . 
C45 C 0.6072(2) 0.18752(12) 0.87035(10) 0.0226(6) Uani 1 1 d . . . 
H45A H 0.5463 0.1737 0.8925 0.027 Uiso 1 1 calc R . . 
H45B H 0.6803 0.1757 0.8901 0.027 Uiso 1 1 calc R . . 
C46 C 0.4968(2) 0.28787(12) 0.85180(10) 0.0224(5) Uani 1 1 d . . . 
C47 C 0.8742(2) 0.47934(13) 0.67797(11) 0.0238(6) Uani 1 1 d . . . 
H47A H 0.8805 0.4385 0.6950 0.029 Uiso 1 1 calc R . . 
H47B H 0.8880 0.5102 0.7074 0.029 Uiso 1 1 calc R . . 
C48 C 0.8942(2) 0.14540(13) 0.78218(11) 0.0254(6) Uani 1 1 d . . . 
H48A H 0.8966 0.1686 0.7475 0.031 Uiso 1 1 calc R . . 
H48B H 0.8948 0.1014 0.7735 0.031 Uiso 1 1 calc R . . 
C49 C 0.8268(2) 0.14530(13) 0.56556(12) 0.0285(6) Uani 1 1 d . . . 
H49A H 0.8351 0.1900 0.5683 0.034 Uiso 1 1 calc R . . 
H49B H 0.8202 0.1337 0.5261 0.034 Uiso 1 1 calc R . . 
C50 C 0.2252(2) 0.42347(13) 0.56072(12) 0.0289(6) Uani 1 1 d . . . 
H50A H 0.1844 0.4396 0.5912 0.035 Uiso 1 1 calc R . . 
H50B H 0.2360 0.3793 0.5667 0.035 Uiso 1 1 calc R . . 
C51 C 0.9957(2) 0.16210(15) 0.82354(13) 0.0357(7) Uani 1 1 d . . . 
H51A H 0.9954 0.2059 0.8306 0.054 Uiso 1 1 calc R . . 
H51B H 1.0659 0.1509 0.8080 0.054 Uiso 1 1 calc R . . 
H51C H 0.9903 0.1401 0.8582 0.054 Uiso 1 1 calc R . . 
C52 C 0.8080(2) 0.36056(13) 0.47346(12) 0.0295(6) Uani 1 1 d . . . 
H52A H 0.8691 0.3310 0.4690 0.035 Uiso 1 1 calc R . . 
H52B H 0.8329 0.3875 0.5048 0.035 Uiso 1 1 calc R . . 
C53 C 0.1021(2) 0.23951(15) 0.51669(13) 0.0356(7) Uani 1 1 d . . . 
H53A H 0.1154 0.2835 0.5185 0.053 Uiso 1 1 calc R . . 
H53B H 0.0343 0.2297 0.5349 0.053 Uiso 1 1 calc R . . 
H53C H 0.0917 0.2266 0.4780 0.053 Uiso 1 1 calc R . . 
C54 C 0.2039(2) 0.20620(14) 0.54605(12) 0.0284(6) Uani 1 1 d . . . 
H54A H 0.2125 0.2169 0.5857 0.034 Uiso 1 1 calc R . . 
H54B H 0.1935 0.1617 0.5427 0.034 Uiso 1 1 calc R . . 
C55 C 0.2666(2) 0.46456(16) 0.73716(12) 0.0354(7) Uani 1 1 d . . . 
H55A H 0.2651 0.4318 0.7093 0.043 Uiso 1 1 calc R . . 
H55B H 0.2481 0.5035 0.7179 0.043 Uiso 1 1 calc R . . 
C56 C 0.9597(2) 0.48639(16) 0.63510(12) 0.0361(7) Uani 1 1 d . . . 
H56A H 0.9446 0.4558 0.6061 0.054 Uiso 1 1 calc R . . 
H56B H 1.0361 0.4807 0.6530 0.054 Uiso 1 1 calc R . . 
H56C H 0.9530 0.5271 0.6189 0.054 Uiso 1 1 calc R . . 
C57 C 0.9281(2) 0.11364(16) 0.59659(14) 0.0391(7) Uani 1 1 d . . . 
H57A H 0.9342 0.1261 0.6354 0.059 Uiso 1 1 calc R . . 
H57B H 0.9970 0.1251 0.5801 0.059 Uiso 1 1 calc R . . 
H57C H 0.9179 0.0695 0.5941 0.059 Uiso 1 1 calc R . . 
C58 C 0.2887(2) 0.27757(14) 0.83736(14) 0.0365(7) Uani 1 1 d . . . 
H58A H 0.2359 0.2452 0.8231 0.044 Uiso 1 1 calc R . . 
H58B H 0.2934 0.3080 0.8077 0.044 Uiso 1 1 calc R . . 
C59 C 0.1803(2) 0.45122(16) 0.77903(13) 0.0379(7) Uani 1 1 d . . . 
H59A H 0.1962 0.4113 0.7959 0.057 Uiso 1 1 calc R . . 
H59B H 0.1041 0.4513 0.7600 0.057 Uiso 1 1 calc R . . 
H59C H 0.1859 0.4826 0.8078 0.057 Uiso 1 1 calc R . . 
C60 C 0.7879(3) 0.39893(15) 0.42071(14) 0.0422(8) Uani 1 1 d . . . 
H60A H 0.7603 0.3727 0.3898 0.063 Uiso 1 1 calc R . . 
H60B H 0.8587 0.4181 0.4127 0.063 Uiso 1 1 calc R . . 
H60C H 0.7317 0.4304 0.4260 0.063 Uiso 1 1 calc R . . 
C61 C 0.4540(3) 0.45876(15) -0.03951(13) 0.0450(9) Uani 1 1 d . . . 
H61 H 0.4230 0.4305 -0.0663 0.054 Uiso 1 1 calc R . . 
C62 C 0.5700(3) 0.45702(16) -0.02264(13) 0.0456(8) Uani 1 1 d . . . 
H62 H 0.6167 0.4280 -0.0382 0.055 Uiso 1 1 calc R . . 
C63 C 0.1537(3) 0.43394(16) 0.50566(15) 0.0448(8) Uani 1 1 d . . . 
H63A H 0.1428 0.4777 0.4996 0.067 Uiso 1 1 calc R . . 
H63B H 0.0802 0.4142 0.5068 0.067 Uiso 1 1 calc R . . 
H63C H 0.1925 0.4166 0.4755 0.067 Uiso 1 1 calc R . . 
C64 C 0.1611(2) 0.12146(18) 0.69030(14) 0.0445(8) Uani 1 1 d . . . 
H64A H 0.1730 0.1346 0.6528 0.067 Uiso 1 1 calc R . . 
H64B H 0.0966 0.1433 0.7029 0.067 Uiso 1 1 calc R . . 
H64C H 0.1460 0.0777 0.6903 0.067 Uiso 1 1 calc R . . 
C65 C 0.8930(3) 0.36959(15) 0.89767(15) 0.0430(8) Uani 1 1 d . . . 
H65A H 0.9297 0.3364 0.8785 0.052 Uiso 1 1 calc R . . 
H65B H 0.8678 0.3531 0.9323 0.052 Uiso 1 1 calc R . . 
C66 C 0.6172(3) 0.49821(16) 0.01731(13) 0.0456(8) Uani 1 1 d . . . 
C67 C 0.2658(3) 0.13506(19) 0.72867(15) 0.0500(9) Uani 1 1 d . . . 
H67A H 0.2795 0.1794 0.7303 0.060 Uiso 1 1 calc R . . 
H67B H 0.2555 0.1206 0.7664 0.060 Uiso 1 1 calc R . . 
C68 C 0.2425(3) 0.30789(16) 0.88641(17) 0.0526(10) Uani 1 1 d . . . 
H68A H 0.2416 0.2786 0.9167 0.079 Uiso 1 1 calc R . . 
H68B H 0.1656 0.3222 0.8759 0.079 Uiso 1 1 calc R . . 
H68C H 0.2904 0.3425 0.8984 0.079 Uiso 1 1 calc R . . 
C69 C 0.9758(3) 0.42108(17) 0.91051(19) 0.0583(11) Uani 1 1 d . . . 
H69A H 1.0009 0.4369 0.8761 0.087 Uiso 1 1 calc R . . 
H69B H 1.0410 0.4060 0.9341 0.087 Uiso 1 1 calc R . . 
H69C H 0.9390 0.4536 0.9297 0.087 Uiso 1 1 calc R . . 
C70 C 0.7869(4) 0.30704(17) 0.63028(15) 0.0591(11) Uani 1 1 d . . . 
H70 H 0.7419 0.3086 0.5960 0.071 Uiso 1 1 calc R . . 
C71 C 0.7340(5) 0.30335(16) 0.67980(19) 0.0678(12) Uani 1 1 d . . . 
C72 C 0.8089(6) 0.30219(19) 0.73057(17) 0.0814(17) Uani 1 1 d . . . 
H72 H 0.7781 0.3000 0.7651 0.098 Uiso 1 1 calc R . . 
C73 C 0.9745(4) 0.30726(17) 0.67960(17) 0.0615(11) Uani 1 1 d . . . 
C74 C 0.9054(4) 0.30846(19) 0.63104(17) 0.0633(11) Uani 1 1 d . . . 
H74 H 0.9385 0.3103 0.5971 0.076 Uiso 1 1 calc R . . 
C75 C 0.9279(5) 0.3043(2) 0.72874(19) 0.0766(14) Uani 1 1 d . . . 
H75 H 0.9757 0.3037 0.7622 0.092 Uiso 1 1 calc R . . 
C76 C 0.6058(5) 0.3014(2) 0.6781(3) 0.113(2) Uani 1 1 d . . . 
H76A H 0.5781 0.3404 0.6908 0.170 Uiso 1 1 calc R . . 
H76B H 0.5834 0.2688 0.7022 0.170 Uiso 1 1 calc R . . 
H76C H 0.5737 0.2938 0.6403 0.170 Uiso 1 1 calc R . . 
 
 
_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 
Cl1 C73 1.756(5) . ? 
O8 C19 1.383(3) . ? 
O8 C50 1.433(3) . ? 
O3 C40 1.374(3) . ? 
O3 C48 1.430(3) . ? 
O7 C27 1.391(3) . ? 
O7 C55 1.413(3) . ? 
O5 C23 1.380(3) . ? 
O5 C47 1.427(3) . ? 
O9 C34 1.383(3) . ? 
O9 C54 1.422(3) . ? 
O1 C25 1.397(3) . ? 
O1 C52 1.430(3) . ? 
O2 C38 1.379(3) . ? 
O2 C49 1.417(3) . ? 
Cl2 C66 1.629(4) . ? 
O10 C30 1.386(3) . ? 
O10 C67 1.409(4) . ? 
O6 C46 1.380(3) . ? 
O6 C58 1.429(3) . ? 
O4 C43 1.376(3) . ? 
O4 C65 1.424(3) . ? 
C12 C18 1.389(3) . ? 
C12 C19 1.395(3) . ? 
C12 C26 1.515(3) . ? 
C13 C21 1.510(3) . ? 
C13 C22 1.520(3) . ? 
C13 H13A 0.9700 . ? 
C13 H13B 0.9700 . ? 
C14 C43 1.389(4) . ? 
C14 C24 1.400(4) . ? 
C14 C41 1.511(3) . ? 
C15 C27 1.386(3) . ? 
C15 C33 1.390(3) . ? 
C15 H15 0.9300 . ? 
C16 C19 1.382(3) . ? 
C16 C21 1.397(3) . ? 
C16 H16 0.9300 . ? 
C17 C37 1.382(4) . ? 
C17 C43 1.394(4) . ? 
C17 H17 0.9300 . ? 
C18 C25 1.391(4) . ? 
C18 H18 0.9300 . ? 
C20 C29 1.394(3) . ? 
C20 C30 1.399(3) . ? 
C20 C39 1.510(3) . ? 
C21 C25 1.386(3) . ? 
C22 C36 1.383(4) . ? 
C22 C34 1.401(3) . ? 
C23 C28 1.392(3) . ? 
C23 C33 1.394(3) . ? 
C24 C46 1.385(4) . ? 
C24 H24 0.9300 . ? 
C26 C33 1.523(3) . ? 
C26 H26A 0.9700 . ? 
C26 H26B 0.9700 . ? 
C27 C32 1.389(3) . ? 
C28 C32 1.392(3) . ? 
C28 H28 0.9300 . ? 
C29 C40 1.393(4) . ? 
C29 H29 0.9300 . ? 
C30 C35 1.385(4) . ? 
C31 C44 1.389(3) . ? 
C31 C38 1.395(3) . ? 
C31 C39 1.513(3) . ? 
C32 C41 1.524(3) . ? 
C34 C44 1.390(3) . ? 
C35 C42 1.388(4) . ? 
C35 H35 0.9300 . ? 
C36 C38 1.388(4) . ? 
C36 H36 0.9300 . ? 
C37 C46 1.398(4) . ? 
C37 C45 1.515(4) . ? 
C39 H39A 0.9700 . ? 
C39 H39B 0.9700 . ? 
C40 C42 1.400(3) . ? 
C41 H41A 0.9700 . ? 
C41 H41B 0.9700 . ? 
C42 C45 1.519(3) . ? 
C44 H44 0.9300 . ? 
C45 H45A 0.9700 . ? 
C45 H45B 0.9700 . ? 
C47 C56 1.501(4) . ? 
C47 H47A 0.9700 . ? 
C47 H47B 0.9700 . ? 
C48 C51 1.513(4) . ? 
C48 H48A 0.9700 . ? 
C48 H48B 0.9700 . ? 
C49 C57 1.500(4) . ? 
C49 H49A 0.9700 . ? 
C49 H49B 0.9700 . ? 
C50 C63 1.506(4) . ? 
C50 H50A 0.9700 . ? 
C50 H50B 0.9700 . ? 
C51 H51A 0.9600 . ? 
C51 H51B 0.9600 . ? 
C51 H51C 0.9600 . ? 
C52 C60 1.505(4) . ? 
C52 H52A 0.9700 . ? 
C52 H52B 0.9700 . ? 
C53 C54 1.504(4) . ? 
C53 H53A 0.9600 . ? 
C53 H53B 0.9600 . ? 
C53 H53C 0.9600 . ? 
C54 H54A 0.9700 . ? 
C54 H54B 0.9700 . ? 
C55 C59 1.510(4) . ? 
C55 H55A 0.9700 . ? 
C55 H55B 0.9700 . ? 
C56 H56A 0.9600 . ? 
C56 H56B 0.9600 . ? 
C56 H56C 0.9600 . ? 
C57 H57A 0.9600 . ? 
C57 H57B 0.9600 . ? 
C57 H57C 0.9600 . ? 
C58 C68 1.484(5) . ? 
C58 H58A 0.9700 . ? 
C58 H58B 0.9700 . ? 
C59 H59A 0.9600 . ? 
C59 H59B 0.9600 . ? 
C59 H59C 0.9600 . ? 
C60 H60A 0.9600 . ? 
C60 H60B 0.9600 . ? 
C60 H60C 0.9600 . ? 
C61 C62 1.377(5) . ? 
C61 C66 1.383(5) 3_665 ? 
C61 H61 0.9300 . ? 
C62 C66 1.379(5) . ? 
C62 H62 0.9300 . ? 
C63 H63A 0.9600 . ? 
C63 H63B 0.9600 . ? 
C63 H63C 0.9600 . ? 
C64 C67 1.486(4) . ? 
C64 H64A 0.9600 . ? 
C64 H64B 0.9600 . ? 
C64 H64C 0.9600 . ? 
C65 C69 1.485(5) . ? 
C65 H65A 0.9700 . ? 
C65 H65B 0.9700 . ? 
C66 C61 1.383(5) 3_665 ? 
C67 H67A 0.9700 . ? 
C67 H67B 0.9700 . ? 
C68 H68A 0.9600 . ? 
C68 H68B 0.9600 . ? 
C68 H68C 0.9600 . ? 
C69 H69A 0.9600 . ? 
C69 H69B 0.9600 . ? 
C69 H69C 0.9600 . ? 
C70 C74 1.383(6) . ? 
C70 C71 1.385(6) . ? 
C70 H70 0.9300 . ? 
C71 C72 1.426(7) . ? 
C71 C76 1.493(7) . ? 
C72 C75 1.395(7) . ? 
C72 H72 0.9300 . ? 
C73 C75 1.338(6) . ? 
C73 C74 1.349(6) . ? 
C74 H74 0.9300 . ? 
C75 H75 0.9300 . ? 
C76 H76A 0.9600 . ? 
C76 H76B 0.9600 . ? 
C76 H76C 0.9600 . ? 
 
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 
C19 O8 C50 118.81(19) . . ? 
C40 O3 C48 117.95(19) . . ? 
C27 O7 C55 118.2(2) . . ? 
C23 O5 C47 117.77(19) . . ? 
C34 O9 C54 117.94(19) . . ? 
C25 O1 C52 118.71(19) . . ? 
C38 O2 C49 117.8(2) . . ? 
C30 O10 C67 117.0(2) . . ? 
C46 O6 C58 119.9(2) . . ? 
C43 O4 C65 116.8(2) . . ? 
C18 C12 C19 118.3(2) . . ? 
C18 C12 C26 120.7(2) . . ? 
C19 C12 C26 120.9(2) . . ? 
C21 C13 C22 110.89(19) . . ? 
C21 C13 H13A 109.5 . . ? 
C22 C13 H13A 109.5 . . ? 
C21 C13 H13B 109.5 . . ? 
C22 C13 H13B 109.5 . . ? 
H13A C13 H13B 108.0 . . ? 
C43 C14 C24 117.9(2) . . ? 
C43 C14 C41 121.7(2) . . ? 
C24 C14 C41 120.3(2) . . ? 
C27 C15 C33 121.4(2) . . ? 
C27 C15 H15 119.3 . . ? 
C33 C15 H15 119.3 . . ? 
C19 C16 C21 121.3(2) . . ? 
C19 C16 H16 119.3 . . ? 
C21 C16 H16 119.3 . . ? 
C37 C17 C43 121.9(2) . . ? 
C37 C17 H17 119.1 . . ? 
C43 C17 H17 119.0 . . ? 
C12 C18 C25 121.1(2) . . ? 
C12 C18 H18 119.4 . . ? 
C25 C18 H18 119.4 . . ? 
C16 C19 O8 123.7(2) . . ? 
C16 C19 C12 120.4(2) . . ? 
O8 C19 C12 115.9(2) . . ? 
C29 C20 C30 117.8(2) . . ? 
C29 C20 C39 121.7(2) . . ? 
C30 C20 C39 120.6(2) . . ? 
C25 C21 C16 118.2(2) . . ? 
C25 C21 C13 122.4(2) . . ? 
C16 C21 C13 119.3(2) . . ? 
C36 C22 C34 118.3(2) . . ? 
C36 C22 C13 120.3(2) . . ? 
C34 C22 C13 121.3(2) . . ? 
O5 C23 C28 124.0(2) . . ? 
O5 C23 C33 116.1(2) . . ? 
C28 C23 C33 119.9(2) . . ? 
C46 C24 C14 121.6(2) . . ? 
C46 C24 H24 119.2 . . ? 
C14 C24 H24 119.2 . . ? 
C21 C25 C18 120.6(2) . . ? 
C21 C25 O1 115.7(2) . . ? 
C18 C25 O1 123.6(2) . . ? 
C12 C26 C33 111.84(19) . . ? 
C12 C26 H26A 109.2 . . ? 
C33 C26 H26A 109.2 . . ? 
C12 C26 H26B 109.2 . . ? 
C33 C26 H26B 109.2 . . ? 
H26A C26 H26B 107.9 . . ? 
C15 C27 C32 120.4(2) . . ? 
C15 C27 O7 123.4(2) . . ? 
C32 C27 O7 116.2(2) . . ? 
C23 C28 C32 121.5(2) . . ? 
C23 C28 H28 119.3 . . ? 
C32 C28 H28 119.3 . . ? 
C40 C29 C20 121.6(2) . . ? 
C40 C29 H29 119.2 . . ? 
C20 C29 H29 119.2 . . ? 
C35 C30 O10 122.4(2) . . ? 
C35 C30 C20 120.8(2) . . ? 
O10 C30 C20 116.8(2) . . ? 
C44 C31 C38 117.8(2) . . ? 
C44 C31 C39 121.4(2) . . ? 
C38 C31 C39 120.8(2) . . ? 
C27 C32 C28 118.2(2) . . ? 
C27 C32 C41 121.3(2) . . ? 
C28 C32 C41 120.5(2) . . ? 
C15 C33 C23 118.5(2) . . ? 
C15 C33 C26 120.6(2) . . ? 
C23 C33 C26 120.9(2) . . ? 
O9 C34 C44 124.2(2) . . ? 
O9 C34 C22 115.7(2) . . ? 
C44 C34 C22 120.0(2) . . ? 
C30 C35 C42 121.4(2) . . ? 
C30 C35 H35 119.3 . . ? 
C42 C35 H35 119.3 . . ? 
C22 C36 C38 121.4(2) . . ? 
C22 C36 H36 119.3 . . ? 
C38 C36 H36 119.3 . . ? 
C17 C37 C46 118.1(2) . . ? 
C17 C37 C45 121.0(2) . . ? 
C46 C37 C45 120.9(2) . . ? 
O2 C38 C36 123.6(2) . . ? 
O2 C38 C31 115.7(2) . . ? 
C36 C38 C31 120.7(2) . . ? 
C20 C39 C31 113.9(2) . . ? 
C20 C39 H39A 108.8 . . ? 
C31 C39 H39A 108.8 . . ? 
C20 C39 H39B 108.8 . . ? 
C31 C39 H39B 108.8 . . ? 
H39A C39 H39B 107.7 . . ? 
O3 C40 C29 124.6(2) . . ? 
O3 C40 C42 115.4(2) . . ? 
C29 C40 C42 120.0(2) . . ? 
C14 C41 C32 112.6(2) . . ? 
C14 C41 H41A 109.1 . . ? 
C32 C41 H41A 109.1 . . ? 
C14 C41 H41B 109.1 . . ? 
C32 C41 H41B 109.1 . . ? 
H41A C41 H41B 107.8 . . ? 
C35 C42 C40 118.3(2) . . ? 
C35 C42 C45 119.9(2) . . ? 
C40 C42 C45 121.7(2) . . ? 
O4 C43 C14 117.1(2) . . ? 
O4 C43 C17 122.8(2) . . ? 
C14 C43 C17 120.2(2) . . ? 
C31 C44 C34 121.7(2) . . ? 
C31 C44 H44 119.2 . . ? 
C34 C44 H44 119.2 . . ? 
C37 C45 C42 110.3(2) . . ? 
C37 C45 H45A 109.6 . . ? 
C42 C45 H45A 109.6 . . ? 
C37 C45 H45B 109.6 . . ? 
C42 C45 H45B 109.6 . . ? 
H45A C45 H45B 108.1 . . ? 
O6 C46 C24 124.0(2) . . ? 
O6 C46 C37 115.8(2) . . ? 
C24 C46 C37 120.2(2) . . ? 
O5 C47 C56 107.0(2) . . ? 
O5 C47 H47A 110.3 . . ? 
C56 C47 H47A 110.3 . . ? 
O5 C47 H47B 110.3 . . ? 
C56 C47 H47B 110.3 . . ? 
H47A C47 H47B 108.6 . . ? 
O3 C48 C51 106.1(2) . . ? 
O3 C48 H48A 110.5 . . ? 
C51 C48 H48A 110.5 . . ? 
O3 C48 H48B 110.5 . . ? 
C51 C48 H48B 110.5 . . ? 
H48A C48 H48B 108.7 . . ? 
O2 C49 C57 106.4(2) . . ? 
O2 C49 H49A 110.5 . . ? 
C57 C49 H49A 110.5 . . ? 
O2 C49 H49B 110.5 . . ? 
C57 C49 H49B 110.5 . . ? 
H49A C49 H49B 108.6 . . ? 
O8 C50 C63 111.9(2) . . ? 
O8 C50 H50A 109.2 . . ? 
C63 C50 H50A 109.2 . . ? 
O8 C50 H50B 109.2 . . ? 
C63 C50 H50B 109.2 . . ? 
H50A C50 H50B 107.9 . . ? 
C48 C51 H51A 109.5 . . ? 
C48 C51 H51B 109.5 . . ? 
H51A C51 H51B 109.5 . . ? 
C48 C51 H51C 109.5 . . ? 
H51A C51 H51C 109.5 . . ? 
H51B C51 H51C 109.5 . . ? 
O1 C52 C60 112.1(2) . . ? 
O1 C52 H52A 109.2 . . ? 
C60 C52 H52A 109.2 . . ? 
O1 C52 H52B 109.2 . . ? 
C60 C52 H52B 109.2 . . ? 
H52A C52 H52B 107.9 . . ? 
C54 C53 H53A 109.5 . . ? 
C54 C53 H53B 109.5 . . ? 
H53A C53 H53B 109.5 . . ? 
C54 C53 H53C 109.5 . . ? 
H53A C53 H53C 109.5 . . ? 
H53B C53 H53C 109.5 . . ? 
O9 C54 C53 107.4(2) . . ? 
O9 C54 H54A 110.2 . . ? 
C53 C54 H54A 110.2 . . ? 
O9 C54 H54B 110.2 . . ? 
C53 C54 H54B 110.2 . . ? 
H54A C54 H54B 108.5 . . ? 
O7 C55 C59 107.8(2) . . ? 
O7 C55 H55A 110.1 . . ? 
C59 C55 H55A 110.1 . . ? 
O7 C55 H55B 110.1 . . ? 
C59 C55 H55B 110.1 . . ? 
H55A C55 H55B 108.5 . . ? 
C47 C56 H56A 109.5 . . ? 
C47 C56 H56B 109.5 . . ? 
H56A C56 H56B 109.5 . . ? 
C47 C56 H56C 109.5 . . ? 
H56A C56 H56C 109.5 . . ? 
H56B C56 H56C 109.5 . . ? 
C49 C57 H57A 109.5 . . ? 
C49 C57 H57B 109.5 . . ? 
H57A C57 H57B 109.5 . . ? 
C49 C57 H57C 109.5 . . ? 
H57A C57 H57C 109.5 . . ? 
H57B C57 H57C 109.5 . . ? 
O6 C58 C68 112.5(3) . . ? 
O6 C58 H58A 109.1 . . ? 
C68 C58 H58A 109.1 . . ? 
O6 C58 H58B 109.1 . . ? 
C68 C58 H58B 109.1 . . ? 
H58A C58 H58B 107.8 . . ? 
C55 C59 H59A 109.5 . . ? 
C55 C59 H59B 109.5 . . ? 
H59A C59 H59B 109.5 . . ? 
C55 C59 H59C 109.5 . . ? 
H59A C59 H59C 109.5 . . ? 
H59B C59 H59C 109.5 . . ? 
C52 C60 H60A 109.5 . . ? 
C52 C60 H60B 109.5 . . ? 
H60A C60 H60B 109.5 . . ? 
C52 C60 H60C 109.5 . . ? 
H60A C60 H60C 109.5 . . ? 
H60B C60 H60C 109.5 . . ? 
C62 C61 C66 121.0(3) . 3_665 ? 
C62 C61 H61 119.5 . . ? 
C66 C61 H61 119.5 3_665 . ? 
C61 C62 C66 120.2(3) . . ? 
C61 C62 H62 119.9 . . ? 
C66 C62 H62 119.9 . . ? 
C50 C63 H63A 109.5 . . ? 
C50 C63 H63B 109.5 . . ? 
H63A C63 H63B 109.5 . . ? 
C50 C63 H63C 109.5 . . ? 
H63A C63 H63C 109.5 . . ? 
H63B C63 H63C 109.5 . . ? 
C67 C64 H64A 109.5 . . ? 
C67 C64 H64B 109.5 . . ? 
H64A C64 H64B 109.5 . . ? 
C67 C64 H64C 109.5 . . ? 
H64A C64 H64C 109.5 . . ? 
H64B C64 H64C 109.5 . . ? 
O4 C65 C69 108.9(3) . . ? 
O4 C65 H65A 109.9 . . ? 
C69 C65 H65A 109.9 . . ? 
O4 C65 H65B 109.9 . . ? 
C69 C65 H65B 109.9 . . ? 
H65A C65 H65B 108.3 . . ? 
C62 C66 C61 118.7(3) . 3_665 ? 
C62 C66 Cl2 121.4(3) . . ? 
C61 C66 Cl2 119.9(3) 3_665 . ? 
O10 C67 C64 108.5(3) . . ? 
O10 C67 H67A 110.0 . . ? 
C64 C67 H67A 110.0 . . ? 
O10 C67 H67B 110.0 . . ? 
C64 C67 H67B 110.0 . . ? 
H67A C67 H67B 108.4 . . ? 
C58 C68 H68A 109.5 . . ? 
C58 C68 H68B 109.5 . . ? 
H68A C68 H68B 109.5 . . ? 
C58 C68 H68C 109.5 . . ? 
H68A C68 H68C 109.5 . . ? 
H68B C68 H68C 109.5 . . ? 
C65 C69 H69A 109.5 . . ? 
C65 C69 H69B 109.5 . . ? 
H69A C69 H69B 109.5 . . ? 
C65 C69 H69C 109.5 . . ? 
H69A C69 H69C 109.5 . . ? 
H69B C69 H69C 109.5 . . ? 
C74 C70 C71 121.0(4) . . ? 
C74 C70 H70 119.5 . . ? 
C71 C70 H70 119.5 . . ? 
C70 C71 C72 116.0(5) . . ? 
C70 C71 C76 120.2(5) . . ? 
C72 C71 C76 123.7(5) . . ? 
C75 C72 C71 120.4(4) . . ? 
C75 C72 H72 119.8 . . ? 
C71 C72 H72 119.8 . . ? 
C75 C73 C74 119.6(5) . . ? 
C75 C73 Cl1 119.1(4) . . ? 
C74 C73 Cl1 121.2(4) . . ? 
C73 C74 C70 121.9(4) . . ? 
C73 C74 H74 119.0 . . ? 
C70 C74 H74 119.0 . . ? 
C73 C75 C72 121.0(4) . . ? 
C73 C75 H75 119.5 . . ? 
C72 C75 H75 119.5 . . ? 
C71 C76 H76A 109.5 . . ? 
C71 C76 H76B 109.5 . . ? 
H76A C76 H76B 109.5 . . ? 
C71 C76 H76C 109.5 . . ? 
H76A C76 H76C 109.5 . . ? 
H76B C76 H76C 109.5 . . ? 
 
_diffrn_measured_fraction_theta_max    0.994 
_diffrn_reflns_theta_full              25.00 
_diffrn_measured_fraction_theta_full   0.994 
_refine_diff_density_max    1.817 
_refine_diff_density_min   -1.516 
_refine_diff_density_rms    0.062 
