data_cb1_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H38.24 Cl1.76 O4.12' _chemical_formula_weight 635.25 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' '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 Orthorhombic _symmetry_space_group_name_H-M Pcca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x, y, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x, -y, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 39.1560(10) _cell_length_b 14.1598(4) _cell_length_c 11.7448(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6511.8(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5905 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 30.58 _exptl_crystal_description 'prism frag' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.296 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2681 _exptl_absorpt_coefficient_mu 0.221 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9468 _exptl_absorpt_correction_T_max 0.9600 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Normal-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 99526 _diffrn_reflns_av_R_equivalents 0.0584 _diffrn_reflns_av_sigmaI/netI 0.0358 _diffrn_reflns_limit_h_min -55 _diffrn_reflns_limit_h_max 55 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 30.51 _reflns_number_total 9949 _reflns_number_gt 7098 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0736P)^2^+2.0350P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9949 _refine_ls_number_parameters 436 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0714 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1374 _refine_ls_wR_factor_gt 0.1228 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.038 _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 C1 C 0.34114(3) 0.08698(9) 0.93064(11) 0.0152(2) Uani 1 1 d . . . H1 H 0.3513 0.0869 1.0040 0.018 Uiso 1 1 calc R . . C2 C 0.32230(4) 0.00936(9) 0.89471(12) 0.0186(3) Uani 1 1 d . . . H2 H 0.3197 -0.0438 0.9433 0.022 Uiso 1 1 calc R . . C3 C 0.30728(3) 0.00966(10) 0.78748(12) 0.0188(3) Uani 1 1 d . . . H3 H 0.2944 -0.0434 0.7627 0.023 Uiso 1 1 calc R . . C4 C 0.31103(3) 0.08766(9) 0.71619(11) 0.0147(2) Uani 1 1 d . . . H4 H 0.3008 0.0875 0.6429 0.018 Uiso 1 1 calc R . . C4A C 0.32974(3) 0.16593(8) 0.75203(10) 0.0109(2) Uani 1 1 d . . . C5 C 0.33662(3) 0.25302(8) 0.67811(11) 0.0108(2) Uani 1 1 d . . . C5A C 0.33214(3) 0.34098(8) 0.75300(11) 0.0116(2) Uani 1 1 d . . . C6 C 0.31601(3) 0.42332(9) 0.71701(11) 0.0150(2) Uani 1 1 d . . . H6 H 0.3058 0.4258 0.6437 0.018 Uiso 1 1 calc R . . C7 C 0.31470(3) 0.50219(9) 0.78774(12) 0.0180(3) Uani 1 1 d . . . H7 H 0.3038 0.5583 0.7623 0.022 Uiso 1 1 calc R . . C8 C 0.32934(3) 0.49892(9) 0.89587(12) 0.0179(3) Uani 1 1 d . . . H8 H 0.3283 0.5525 0.9445 0.021 Uiso 1 1 calc R . . C9 C 0.34545(3) 0.41687(9) 0.93207(11) 0.0147(2) Uani 1 1 d . . . H9 H 0.3554 0.4144 1.0059 0.018 Uiso 1 1 calc R . . C9A C 0.34724(3) 0.33808(9) 0.86125(11) 0.0119(2) Uani 1 1 d . . . C10 C 0.36615(3) 0.24968(8) 0.89531(11) 0.0111(2) Uani 1 1 d . . . H10 H 0.3678 0.2490 0.9803 0.013 Uiso 1 1 calc R . . C10A C 0.34517(3) 0.16507(9) 0.85955(10) 0.0116(2) Uani 1 1 d . . . C11 C 0.31161(3) 0.25989(9) 0.57680(11) 0.0135(2) Uani 1 1 d . . . O1 O 0.27939(2) 0.25382(6) 0.61199(8) 0.01474(19) Uani 1 1 d . . . O2 O 0.32030(3) 0.27341(8) 0.47962(9) 0.0242(2) Uani 1 1 d . . . C12 C 0.25032(3) 0.25905(9) 0.53039(12) 0.0163(3) Uani 1 1 d . . . C13 C 0.24908(4) 0.35611(12) 0.47576(16) 0.0347(4) Uani 1 1 d . . . H13A H 0.2492 0.4046 0.5353 0.052 Uiso 1 1 calc R . . H13B H 0.2282 0.3619 0.4303 0.052 Uiso 1 1 calc R . . H13C H 0.2690 0.3644 0.4264 0.052 Uiso 1 1 calc R . . C14 C 0.25285(4) 0.18063(13) 0.44268(15) 0.0327(4) Uani 1 1 d . . . H14A H 0.2732 0.1904 0.3956 0.049 Uiso 1 1 calc R . . H14B H 0.2325 0.1813 0.3943 0.049 Uiso 1 1 calc R . . H14C H 0.2545 0.1196 0.4816 0.049 Uiso 1 1 calc R . . C15 C 0.21979(4) 0.24467(12) 0.60736(14) 0.0268(3) Uani 1 1 d . . . H15A H 0.2212 0.1822 0.6431 0.040 Uiso 1 1 calc R . . H15B H 0.1988 0.2489 0.5624 0.040 Uiso 1 1 calc R . . H15C H 0.2196 0.2935 0.6665 0.040 Uiso 1 1 calc R . . C1' C 0.39669(3) 0.08277(9) 0.59230(11) 0.0152(3) Uani 1 1 d . . . H1' H 0.3868 0.0846 0.5185 0.018 Uiso 1 1 calc R . . C2' C 0.41364(3) 0.00187(10) 0.62850(12) 0.0184(3) Uani 1 1 d . . . H2' H 0.4152 -0.0516 0.5799 0.022 Uiso 1 1 calc R . . C3' C 0.42829(3) -0.00028(10) 0.73656(12) 0.0188(3) Uani 1 1 d . . . H3' H 0.4397 -0.0556 0.7620 0.023 Uiso 1 1 calc R . . C4' C 0.42625(3) 0.07842(9) 0.80741(11) 0.0149(2) Uani 1 1 d . . . H4' H 0.4364 0.0767 0.8809 0.018 Uiso 1 1 calc R . . C4B C 0.40944(3) 0.15961(9) 0.77106(10) 0.0116(2) Uani 1 1 d . . . C5' C 0.40454(3) 0.24781(8) 0.84468(10) 0.0104(2) Uani 1 1 d . . . C5B C 0.41091(3) 0.33498(8) 0.76946(10) 0.0116(2) Uani 1 1 d . . . C6' C 0.42945(3) 0.41348(9) 0.80465(11) 0.0148(2) Uani 1 1 d . . . H6' H 0.4394 0.4144 0.8784 0.018 Uiso 1 1 calc R . . C7' C 0.43350(4) 0.49071(10) 0.73248(12) 0.0186(3) Uani 1 1 d . . . H7' H 0.4462 0.5441 0.7569 0.022 Uiso 1 1 calc R . . C8' C 0.41888(4) 0.48957(9) 0.62453(12) 0.0186(3) Uani 1 1 d . . . H8' H 0.4217 0.5421 0.5751 0.022 Uiso 1 1 calc R . . C9' C 0.40021(3) 0.41144(9) 0.58925(11) 0.0153(2) Uani 1 1 d . . . H9' H 0.3903 0.4107 0.5154 0.018 Uiso 1 1 calc R . . C9B C 0.39591(3) 0.33420(9) 0.66142(11) 0.0119(2) Uani 1 1 d . . . C10' C 0.37498(3) 0.24904(8) 0.62775(11) 0.0112(2) Uani 1 1 d . . . H10' H 0.3733 0.2485 0.5428 0.013 Uiso 1 1 calc R . . C10B C 0.39408(3) 0.16133(9) 0.66349(10) 0.0119(2) Uani 1 1 d . . . C11' C 0.43003(3) 0.25023(9) 0.94467(11) 0.0134(2) Uani 1 1 d . . . O1' O 0.46177(2) 0.24112(6) 0.90713(8) 0.01553(19) Uani 1 1 d . . . O2' O 0.42206(3) 0.26250(9) 1.04275(9) 0.0305(3) Uani 1 1 d . . . C12' C 0.49188(3) 0.24370(9) 0.98456(12) 0.0165(3) Uani 1 1 d . . . C13' C 0.49435(4) 0.33944(12) 1.04053(18) 0.0399(5) Uani 1 1 d . . . H13D H 0.4932 0.3888 0.9822 0.060 Uiso 1 1 calc R . . H13E H 0.5161 0.3443 1.0816 0.060 Uiso 1 1 calc R . . H13F H 0.4754 0.3473 1.0941 0.060 Uiso 1 1 calc R . . C14' C 0.48963(5) 0.16401(14) 1.07008(17) 0.0410(5) Uani 1 1 d . . . H14D H 0.4698 0.1739 1.1195 0.062 Uiso 1 1 calc R . . H14E H 0.5104 0.1627 1.1164 0.062 Uiso 1 1 calc R . . H14F H 0.4872 0.1038 1.0297 0.062 Uiso 1 1 calc R . . C15' C 0.52109(4) 0.22840(16) 0.90305(15) 0.0408(5) Uani 1 1 d . . . H15D H 0.5180 0.1680 0.8635 0.061 Uiso 1 1 calc R . . H15E H 0.5426 0.2274 0.9454 0.061 Uiso 1 1 calc R . . H15F H 0.5216 0.2798 0.8472 0.061 Uiso 1 1 calc R . . C1S C 0.11932(4) 0.28693(12) 0.77147(15) 0.0194(3) Uani 0.8267(16) 1 d P A 1 H1S1 H 0.1149 0.3210 0.6994 0.023 Uiso 0.8267(16) 1 calc PR A 1 H1S2 H 0.1332 0.3284 0.8211 0.023 Uiso 0.8267(16) 1 calc PR A 1 Cl1 Cl 0.079799(13) 0.26107(4) 0.83985(4) 0.02387(12) Uani 0.8267(16) 1 d P A 1 Cl2 Cl 0.141996(12) 0.18272(4) 0.74266(5) 0.03199(14) Uani 0.8267(16) 1 d P A 1 C1D C 0.1065(3) 0.288(2) 0.8274(13) 0.0194(3) Uani 0.0523(10) 1 d PDU B 2 H1DA H 0.1023 0.3442 0.8748 0.023 Uiso 0.0523(10) 1 calc PR B 2 H1DB H 0.1145 0.2371 0.8793 0.023 Uiso 0.0523(10) 1 calc PR B 2 Cl1D Cl 0.0669(2) 0.2516(6) 0.7723(7) 0.037(2) Uani 0.0523(10) 1 d PDU B 2 Cl2D Cl 0.14027(18) 0.3142(6) 0.7355(7) 0.03199(14) Uani 0.0523(10) 1 d PDU B 2 C1E C 0.1215(3) 0.2156(8) 0.7737(10) 0.0194(3) Uani 0.1209(19) 1 d PDU C 3 H1EA H 0.1359 0.2656 0.7420 0.029 Uiso 0.1209(19) 1 calc PR C 3 H1EB H 0.1139 0.1735 0.7123 0.029 Uiso 0.1209(19) 1 calc PR C 3 H1EC H 0.1345 0.1793 0.8298 0.029 Uiso 0.1209(19) 1 calc PR C 3 O1E O 0.0913(2) 0.2583(7) 0.8295(9) 0.01474(19) Uani 0.1209(19) 1 d PDU C 3 H1E H 0.0789 0.2154 0.8565 0.018 Uiso 0.1209(19) 1 calc PR C 3 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 C1 0.0145(6) 0.0171(6) 0.0139(6) 0.0024(5) -0.0008(5) 0.0006(5) C2 0.0207(6) 0.0157(6) 0.0195(7) 0.0038(5) 0.0014(5) -0.0025(5) C3 0.0196(6) 0.0146(6) 0.0222(7) 0.0001(5) -0.0010(5) -0.0046(5) C4 0.0131(6) 0.0156(6) 0.0152(6) -0.0012(5) -0.0007(5) -0.0020(5) C4A 0.0091(5) 0.0108(5) 0.0129(5) 0.0000(4) 0.0011(4) 0.0003(4) C5 0.0089(5) 0.0124(5) 0.0110(5) -0.0010(4) -0.0008(4) 0.0009(4) C5A 0.0085(5) 0.0120(5) 0.0142(6) -0.0013(4) 0.0010(4) -0.0001(4) C6 0.0144(6) 0.0148(6) 0.0158(6) 0.0003(5) -0.0006(5) 0.0021(5) C7 0.0187(6) 0.0130(6) 0.0224(7) 0.0001(5) 0.0011(5) 0.0029(5) C8 0.0178(6) 0.0138(6) 0.0220(7) -0.0057(5) 0.0022(5) 0.0005(5) C9 0.0123(5) 0.0169(6) 0.0148(6) -0.0035(5) 0.0003(5) -0.0011(5) C9A 0.0088(5) 0.0131(5) 0.0138(6) -0.0012(4) 0.0015(4) -0.0003(4) C10 0.0090(5) 0.0130(5) 0.0113(5) -0.0004(4) 0.0000(4) -0.0003(4) C10A 0.0087(5) 0.0127(5) 0.0135(6) -0.0006(4) 0.0003(4) -0.0002(4) C11 0.0111(5) 0.0141(6) 0.0152(6) -0.0005(5) -0.0027(4) 0.0002(4) O1 0.0097(4) 0.0192(5) 0.0154(4) 0.0006(3) -0.0028(3) 0.0003(3) O2 0.0153(5) 0.0420(6) 0.0153(5) 0.0024(4) -0.0020(4) 0.0003(4) C12 0.0094(5) 0.0209(6) 0.0187(6) 0.0024(5) -0.0048(5) -0.0002(5) C13 0.0201(7) 0.0326(8) 0.0515(11) 0.0215(8) -0.0126(7) -0.0029(6) C14 0.0212(7) 0.0414(9) 0.0354(9) -0.0187(8) -0.0113(7) 0.0031(7) C15 0.0121(6) 0.0407(9) 0.0275(8) 0.0034(7) -0.0007(5) -0.0017(6) C1' 0.0131(6) 0.0175(6) 0.0151(6) -0.0036(5) -0.0004(5) 0.0001(5) C2' 0.0186(6) 0.0156(6) 0.0210(6) -0.0057(5) 0.0007(5) 0.0022(5) C3' 0.0194(6) 0.0145(6) 0.0226(7) -0.0007(5) -0.0002(5) 0.0051(5) C4' 0.0134(6) 0.0160(6) 0.0152(6) 0.0002(5) -0.0002(5) 0.0020(4) C4B 0.0089(5) 0.0126(5) 0.0132(6) -0.0007(4) 0.0010(4) -0.0003(4) C5' 0.0082(5) 0.0127(5) 0.0104(5) -0.0003(4) -0.0003(4) -0.0002(4) C5B 0.0090(5) 0.0122(5) 0.0136(6) 0.0001(4) 0.0011(4) 0.0006(4) C6' 0.0142(6) 0.0149(6) 0.0153(6) -0.0006(5) -0.0003(5) -0.0014(5) C7' 0.0184(6) 0.0149(6) 0.0224(7) 0.0005(5) -0.0005(5) -0.0050(5) C8' 0.0196(6) 0.0152(6) 0.0210(6) 0.0045(5) 0.0004(5) -0.0022(5) C9' 0.0134(6) 0.0177(6) 0.0150(6) 0.0027(5) -0.0002(5) -0.0003(5) C9B 0.0094(5) 0.0126(5) 0.0137(6) 0.0002(4) 0.0004(4) 0.0001(4) C10' 0.0087(5) 0.0133(5) 0.0116(5) -0.0006(4) -0.0001(4) 0.0005(4) C10B 0.0093(5) 0.0134(5) 0.0128(6) -0.0011(4) 0.0004(4) -0.0001(4) C11' 0.0106(5) 0.0149(6) 0.0148(6) 0.0005(5) -0.0014(4) -0.0005(4) O1' 0.0091(4) 0.0233(5) 0.0142(4) -0.0008(4) -0.0012(3) 0.0004(3) O2' 0.0137(5) 0.0642(8) 0.0135(5) -0.0039(5) -0.0015(4) 0.0016(5) C12' 0.0092(5) 0.0229(6) 0.0173(6) -0.0004(5) -0.0037(5) 0.0006(5) C13' 0.0240(8) 0.0335(9) 0.0622(13) -0.0194(9) -0.0234(8) 0.0047(7) C14' 0.0259(8) 0.0449(10) 0.0522(12) 0.0255(9) -0.0214(8) -0.0077(7) C15' 0.0115(7) 0.0838(15) 0.0272(9) -0.0079(9) -0.0010(6) 0.0059(8) C1S 0.0188(8) 0.0219(8) 0.0176(8) 0.0001(6) 0.0022(6) -0.0023(6) Cl1 0.0157(2) 0.0329(2) 0.0229(2) -0.00216(17) 0.0058(2) 0.0007(2) Cl2 0.0227(2) 0.0353(3) 0.0380(3) -0.0111(2) 0.00282(19) 0.00468(18) C1D 0.0188(8) 0.0219(8) 0.0176(8) 0.0001(6) 0.0022(6) -0.0023(6) Cl1D 0.040(4) 0.047(5) 0.023(4) 0.004(3) -0.001(3) 0.003(3) Cl2D 0.0227(2) 0.0353(3) 0.0380(3) -0.0111(2) 0.00282(19) 0.00468(18) C1E 0.0188(8) 0.0219(8) 0.0176(8) 0.0001(6) 0.0022(6) -0.0023(6) O1E 0.0097(4) 0.0192(5) 0.0154(4) 0.0006(3) -0.0028(3) 0.0003(3) _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 C2 1.3894(18) . ? C1 C10A 1.3946(17) . ? C2 C3 1.3900(19) . ? C3 C4 1.3937(18) . ? C4 C4A 1.3936(17) . ? C4A C10A 1.4000(17) . ? C4A C5 1.5321(17) . ? C5 C5A 1.5349(16) . ? C5 C11 1.5440(17) . ? C5 C10' 1.6154(17) . ? C5A C6 1.3918(17) . ? C5A C9A 1.4028(17) . ? C6 C7 1.3928(18) . ? C7 C8 1.3942(19) . ? C8 C9 1.3887(18) . ? C9 C9A 1.3933(17) . ? C9A C10 1.5084(17) . ? C10 C10A 1.5121(17) . ? C10 C5' 1.6167(17) . ? C11 O2 1.2062(16) . ? C11 O1 1.3306(15) . ? O1 C12 1.4899(15) . ? C12 C15 1.512(2) . ? C12 C13 1.517(2) . ? C12 C14 1.518(2) . ? C1' C2' 1.3905(19) . ? C1' C10B 1.3953(17) . ? C2' C3' 1.393(2) . ? C3' C4' 1.3931(18) . ? C4' C4B 1.3919(17) . ? C4B C10B 1.3994(17) . ? C4B C5' 1.5310(16) . ? C5' C5B 1.5382(17) . ? C5' C11' 1.5416(17) . ? C5B C6' 1.3905(17) . ? C5B C9B 1.3982(17) . ? C6' C7' 1.3927(18) . ? C7' C8' 1.391(2) . ? C8' C9' 1.3892(18) . ? C9' C9B 1.3939(17) . ? C9B C10' 1.5107(17) . ? C10' C10B 1.5093(17) . ? C11' O2' 1.2060(17) . ? C11' O1' 1.3252(15) . ? O1' C12' 1.4893(15) . ? C12' C15' 1.507(2) . ? C12' C13' 1.510(2) . ? C12' C14' 1.513(2) . ? C1S Cl2 1.7551(18) . ? C1S Cl1 1.7815(18) . ? C1D Cl2D 1.748(10) . ? C1D Cl1D 1.753(10) . ? C1E O1E 1.480(9) . ? 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 C2 C1 C10A 120.36(12) . . ? C1 C2 C3 119.83(12) . . ? C2 C3 C4 120.15(12) . . ? C4A C4 C3 120.28(12) . . ? C4 C4A C10A 119.50(11) . . ? C4 C4A C5 124.16(11) . . ? C10A C4A C5 116.24(10) . . ? C4A C5 C5A 107.95(10) . . ? C4A C5 C11 112.08(10) . . ? C5A C5 C11 108.54(10) . . ? C4A C5 C10' 110.06(9) . . ? C5A C5 C10' 110.15(9) . . ? C11 C5 C10' 108.05(10) . . ? C6 C5A C9A 119.41(11) . . ? C6 C5A C5 123.89(11) . . ? C9A C5A C5 116.58(10) . . ? C5A C6 C7 120.48(12) . . ? C6 C7 C8 120.10(12) . . ? C9 C8 C7 119.58(12) . . ? C8 C9 C9A 120.65(12) . . ? C9 C9A C5A 119.77(11) . . ? C9 C9A C10 122.06(11) . . ? C5A C9A C10 118.13(11) . . ? C9A C10 C10A 108.50(10) . . ? C9A C10 C5' 111.87(9) . . ? C10A C10 C5' 112.95(9) . . ? C1 C10A C4A 119.87(11) . . ? C1 C10A C10 121.56(11) . . ? C4A C10A C10 118.56(11) . . ? O2 C11 O1 124.85(12) . . ? O2 C11 C5 124.09(12) . . ? O1 C11 C5 110.98(11) . . ? C11 O1 C12 121.43(10) . . ? O1 C12 C15 102.28(11) . . ? O1 C12 C13 109.97(11) . . ? C15 C12 C13 110.45(12) . . ? O1 C12 C14 110.51(11) . . ? C15 C12 C14 111.02(12) . . ? C13 C12 C14 112.19(14) . . ? C2' C1' C10B 120.57(12) . . ? C1' C2' C3' 119.54(12) . . ? C2' C3' C4' 120.21(12) . . ? C4B C4' C3' 120.30(12) . . ? C4' C4B C10B 119.64(11) . . ? C4' C4B C5' 124.04(11) . . ? C10B C4B C5' 116.22(11) . . ? C4B C5' C5B 108.05(10) . . ? C4B C5' C11' 111.54(10) . . ? C5B C5' C11' 108.34(10) . . ? C4B C5' C10 109.73(9) . . ? C5B C5' C10 110.42(9) . . ? C11' C5' C10 108.75(10) . . ? C6' C5B C9B 119.69(11) . . ? C6' C5B C5' 123.74(11) . . ? C9B C5B C5' 116.54(10) . . ? C5B C6' C7' 120.41(12) . . ? C8' C7' C6' 119.91(12) . . ? C9' C8' C7' 119.85(12) . . ? C8' C9' C9B 120.46(12) . . ? C9' C9B C5B 119.67(11) . . ? C9' C9B C10' 122.18(11) . . ? C5B C9B C10' 118.14(11) . . ? C10B C10' C9B 108.37(10) . . ? C10B C10' C5 112.81(10) . . ? C9B C10' C5 112.39(9) . . ? C1' C10B C4B 119.71(11) . . ? C1' C10B C10' 121.71(11) . . ? C4B C10B C10' 118.57(11) . . ? O2' C11' O1' 125.05(12) . . ? O2' C11' C5' 124.29(12) . . ? O1' C11' C5' 110.60(11) . . ? C11' O1' C12' 122.48(10) . . ? O1' C12' C15' 102.08(11) . . ? O1' C12' C13' 109.80(11) . . ? C15' C12' C13' 110.92(14) . . ? O1' C12' C14' 109.93(11) . . ? C15' C12' C14' 111.02(14) . . ? C13' C12' C14' 112.60(15) . . ? Cl2 C1S Cl1 110.70(10) . . ? Cl2D C1D Cl1D 120.2(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10A C1 C2 C3 -0.2(2) . . . . ? C1 C2 C3 C4 -0.1(2) . . . . ? C2 C3 C4 C4A -0.2(2) . . . . ? C3 C4 C4A C10A 0.96(19) . . . . ? C3 C4 C4A C5 177.20(12) . . . . ? C4 C4A C5 C5A 138.03(12) . . . . ? C10A C4A C5 C5A -45.62(14) . . . . ? C4 C4A C5 C11 18.55(16) . . . . ? C10A C4A C5 C11 -165.10(10) . . . . ? C4 C4A C5 C10' -101.71(13) . . . . ? C10A C4A C5 C10' 74.63(13) . . . . ? C4A C5 C5A C6 -138.86(12) . . . . ? C11 C5 C5A C6 -17.16(16) . . . . ? C10' C5 C5A C6 100.94(13) . . . . ? C4A C5 C5A C9A 45.06(14) . . . . ? C11 C5 C5A C9A 166.75(11) . . . . ? C10' C5 C5A C9A -75.14(13) . . . . ? C9A C5A C6 C7 -0.24(19) . . . . ? C5 C5A C6 C7 -176.22(12) . . . . ? C5A C6 C7 C8 -0.5(2) . . . . ? C6 C7 C8 C9 0.5(2) . . . . ? C7 C8 C9 C9A 0.29(19) . . . . ? C8 C9 C9A C5A -1.07(19) . . . . ? C8 C9 C9A C10 176.66(12) . . . . ? C6 C5A C9A C9 1.04(18) . . . . ? C5 C5A C9A C9 177.31(11) . . . . ? C6 C5A C9A C10 -176.78(11) . . . . ? C5 C5A C9A C10 -0.51(16) . . . . ? C9 C9A C10 C10A 138.78(12) . . . . ? C5A C9A C10 C10A -43.45(15) . . . . ? C9 C9A C10 C5' -95.96(13) . . . . ? C5A C9A C10 C5' 81.81(13) . . . . ? C2 C1 C10A C4A 0.96(19) . . . . ? C2 C1 C10A C10 -178.68(12) . . . . ? C4 C4A C10A C1 -1.32(18) . . . . ? C5 C4A C10A C1 -177.85(11) . . . . ? C4 C4A C10A C10 178.34(11) . . . . ? C5 C4A C10A C10 1.81(16) . . . . ? C9A C10 C10A C1 -137.43(12) . . . . ? C5' C10 C10A C1 97.94(13) . . . . ? C9A C10 C10A C4A 42.91(15) . . . . ? C5' C10 C10A C4A -81.71(13) . . . . ? C4A C5 C11 O2 -130.94(13) . . . . ? C5A C5 C11 O2 109.93(14) . . . . ? C10' C5 C11 O2 -9.51(17) . . . . ? C4A C5 C11 O1 52.27(13) . . . . ? C5A C5 C11 O1 -66.86(12) . . . . ? C10' C5 C11 O1 173.71(9) . . . . ? O2 C11 O1 C12 2.93(19) . . . . ? C5 C11 O1 C12 179.68(10) . . . . ? C11 O1 C12 C15 177.54(11) . . . . ? C11 O1 C12 C13 -65.11(16) . . . . ? C11 O1 C12 C14 59.29(15) . . . . ? C10B C1' C2' C3' -0.4(2) . . . . ? C1' C2' C3' C4' -0.6(2) . . . . ? C2' C3' C4' C4B 0.3(2) . . . . ? C3' C4' C4B C10B 1.01(19) . . . . ? C3' C4' C4B C5' 177.22(12) . . . . ? C4' C4B C5' C5B 138.35(12) . . . . ? C10B C4B C5' C5B -45.32(14) . . . . ? C4' C4B C5' C11' 19.38(16) . . . . ? C10B C4B C5' C11' -164.30(11) . . . . ? C4' C4B C5' C10 -101.20(13) . . . . ? C10B C4B C5' C10 75.13(13) . . . . ? C9A C10 C5' C4B -122.01(11) . . . . ? C10A C10 C5' C4B 0.76(14) . . . . ? C9A C10 C5' C5B -3.01(13) . . . . ? C10A C10 C5' C5B 119.76(11) . . . . ? C9A C10 C5' C11' 115.74(11) . . . . ? C10A C10 C5' C11' -121.50(11) . . . . ? C4B C5' C5B C6' -137.44(12) . . . . ? C11' C5' C5B C6' -16.45(16) . . . . ? C10 C5' C5B C6' 102.55(13) . . . . ? C4B C5' C5B C9B 44.69(14) . . . . ? C11' C5' C5B C9B 165.68(10) . . . . ? C10 C5' C5B C9B -75.33(13) . . . . ? C9B C5B C6' C7' -0.76(19) . . . . ? C5' C5B C6' C7' -178.57(12) . . . . ? C5B C6' C7' C8' 0.1(2) . . . . ? C6' C7' C8' C9' 0.2(2) . . . . ? C7' C8' C9' C9B 0.2(2) . . . . ? C8' C9' C9B C5B -0.86(19) . . . . ? C8' C9' C9B C10' 178.22(12) . . . . ? C6' C5B C9B C9' 1.13(18) . . . . ? C5' C5B C9B C9' 179.10(11) . . . . ? C6' C5B C9B C10' -177.99(11) . . . . ? C5' C5B C9B C10' -0.02(16) . . . . ? C9' C9B C10' C10B 136.97(12) . . . . ? C5B C9B C10' C10B -43.94(15) . . . . ? C9' C9B C10' C5 -97.68(14) . . . . ? C5B C9B C10' C5 81.41(13) . . . . ? C4A C5 C10' C10B 0.99(14) . . . . ? C5A C5 C10' C10B 119.91(11) . . . . ? C11 C5 C10' C10B -121.68(11) . . . . ? C4A C5 C10' C9B -121.90(11) . . . . ? C5A C5 C10' C9B -2.98(14) . . . . ? C11 C5 C10' C9B 115.43(11) . . . . ? C2' C1' C10B C4B 1.70(19) . . . . ? C2' C1' C10B C10' -178.23(12) . . . . ? C4' C4B C10B C1' -2.01(18) . . . . ? C5' C4B C10B C1' -178.50(11) . . . . ? C4' C4B C10B C10' 177.93(11) . . . . ? C5' C4B C10B C10' 1.44(16) . . . . ? C9B C10' C10B C1' -136.73(12) . . . . ? C5 C10' C10B C1' 98.17(13) . . . . ? C9B C10' C10B C4B 43.33(15) . . . . ? C5 C10' C10B C4B -81.77(13) . . . . ? C4B C5' C11' O2' -128.88(14) . . . . ? C5B C5' C11' O2' 112.31(14) . . . . ? C10 C5' C11' O2' -7.74(17) . . . . ? C4B C5' C11' O1' 53.82(13) . . . . ? C5B C5' C11' O1' -64.98(12) . . . . ? C10 C5' C11' O1' 174.97(9) . . . . ? O2' C11' O1' C12' 1.0(2) . . . . ? C5' C11' O1' C12' 178.23(10) . . . . ? C11' O1' C12' C15' 178.77(13) . . . . ? C11' O1' C12' C13' -63.51(17) . . . . ? C11' O1' C12' C14' 60.88(17) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.823 _refine_diff_density_min -0.464 _refine_diff_density_rms 0.064