# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2011 data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email narcis.avarvari@univ-angers.fr _publ_contact_author_name 'Narcis Avarvari' loop_ _publ_author_name 'Francois Riobe' 'Flavia Piron' 'Celine Rethore' 'Augustin M. Madalan' 'Carlos J. Gomez-Garcia' ; J.Lacour ; 'John D. Wallis' 'Narcis Avarvari' data_1 _database_code_depnum_ccdc_archive 'CCDC 820751' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common BEDT-Trisphat _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H10 Cl14 O6 P S8' _chemical_formula_weight 1238.12 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' 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 12.1440(16) _cell_length_b 12.7445(16) _cell_length_c 15.4458(18) _cell_angle_alpha 90.811(15) _cell_angle_beta 103.889(15) _cell_angle_gamma 109.156(15) _cell_volume 2180.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 1.95 _cell_measurement_theta_max 25.7 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.7 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.885 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1226 _exptl_absorpt_coefficient_mu 1.347 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6788 _exptl_absorpt_correction_T_max 0.6939 _exptl_absorpt_process_details wingx _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE-IPDS I' _diffrn_measurement_method 'Oscillation, Phi. incr. = 1.5' _diffrn_detector_area_resol_mean 6.6 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21562 _diffrn_reflns_av_R_equivalents 0.0803 _diffrn_reflns_av_sigmaI/netI 0.1190 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 25.98 _reflns_number_total 7885 _reflns_number_gt 3781 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE [STOE-IPDS]' _computing_cell_refinement 'SELECT, CELL [STOE-IPDS]' _computing_data_reduction 'INTEGRATE [STOE-IPDS]' _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 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^)+(0.0403P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7885 _refine_ls_number_parameters 550 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1218 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1030 _refine_ls_wR_factor_gt 0.0860 _refine_ls_goodness_of_fit_ref 0.827 _refine_ls_restrained_S_all 0.828 _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 0.8054(8) 0.2617(9) 0.2613(6) 0.123(3) Uani 1 1 d . . . H1A H 0.8631 0.3366 0.2663 0.148 Uiso 1 1 calc R . . H1B H 0.7463 0.2517 0.2043 0.148 Uiso 1 1 calc R . . C2 C 0.7459(7) 0.2620(9) 0.3257(6) 0.115(3) Uani 1 1 d . . . H2A H 0.6748 0.1951 0.3120 0.138 Uiso 1 1 calc R . . H2B H 0.7176 0.3251 0.3189 0.138 Uiso 1 1 calc R . . C3 C 0.9505(4) 0.1671(4) 0.3639(4) 0.0472(14) Uani 1 1 d . . . C4 C 0.9251(4) 0.2046(5) 0.4365(4) 0.0477(14) Uani 1 1 d . . . C5 C 1.0975(4) 0.1295(4) 0.4987(4) 0.0431(14) Uani 1 1 d . . . C6 C 1.1929(4) 0.1063(4) 0.5538(3) 0.0439(14) Uani 1 1 d . . . C7 C 1.3779(5) 0.0516(4) 0.6209(4) 0.0508(15) Uani 1 1 d . . . C8 C 1.3506(5) 0.0895(4) 0.6915(4) 0.0506(15) Uani 1 1 d . . . C9 C 1.5791(7) 0.0293(8) 0.7353(6) 0.122(4) Uani 1 1 d . . . H9A H 1.5567 -0.0404 0.7620 0.147 Uiso 1 1 calc R . . H9B H 1.6635 0.0483 0.7361 0.147 Uiso 1 1 calc R . . C10 C 1.5717(6) 0.1107(7) 0.7929(5) 0.099(3) Uani 1 1 d . . . H10A H 1.6081 0.1829 0.7730 0.118 Uiso 1 1 calc R . . H10B H 1.6213 0.1092 0.8520 0.118 Uiso 1 1 calc R . . C11 C 0.4811(4) 0.3941(4) 0.1523(3) 0.0364(12) Uani 1 1 d . . . C12 C 0.5604(4) 0.4829(4) 0.1236(3) 0.0388(13) Uani 1 1 d . . . C13 C 0.6347(4) 0.4608(4) 0.0746(4) 0.0416(13) Uani 1 1 d . . . C14 C 0.6296(4) 0.3519(4) 0.0557(3) 0.0415(13) Uani 1 1 d . . . C15 C 0.5470(4) 0.2629(4) 0.0838(3) 0.0360(12) Uani 1 1 d . . . C16 C 0.4746(4) 0.2851(4) 0.1312(3) 0.0362(12) Uani 1 1 d . . . C17 C 0.1118(4) 0.1755(4) 0.1200(3) 0.0361(12) Uani 1 1 d . . . C18 C 0.0032(4) 0.1543(4) 0.0568(3) 0.0385(13) Uani 1 1 d . . . C19 C -0.0888(4) 0.0523(5) 0.0546(4) 0.0448(15) Uani 1 1 d . . . C20 C -0.0702(4) -0.0250(4) 0.1127(4) 0.0457(15) Uani 1 1 d . . . C21 C 0.0416(4) -0.0031(4) 0.1768(4) 0.0415(13) Uani 1 1 d . . . C22 C 0.1291(4) 0.1005(4) 0.1795(3) 0.0373(12) Uani 1 1 d . . . C23 C 0.3066(4) 0.3484(4) 0.3698(4) 0.0381(13) Uani 1 1 d . . . C24 C 0.2726(4) 0.3951(4) 0.4350(4) 0.0443(14) Uani 1 1 d . . . C25 C 0.3383(5) 0.4029(4) 0.5250(4) 0.0483(15) Uani 1 1 d . . . C26 C 0.4360(5) 0.3676(4) 0.5456(3) 0.0462(15) Uani 1 1 d . . . C27 C 0.4719(4) 0.3222(4) 0.4790(4) 0.0416(13) Uani 1 1 d . . . C28 C 0.4065(4) 0.3140(4) 0.3913(3) 0.0382(13) Uani 1 1 d . . . Cl1 Cl 0.56299(12) 0.61651(10) 0.14559(10) 0.0542(4) Uani 1 1 d . . . Cl2 Cl 0.73159(13) 0.56942(12) 0.03543(12) 0.0681(5) Uani 1 1 d . . . Cl3 Cl 0.72306(14) 0.32514(13) -0.00250(12) 0.0729(5) Uani 1 1 d . . . Cl4 Cl 0.53841(12) 0.12682(11) 0.06072(10) 0.0543(4) Uani 1 1 d . . . Cl5 Cl -0.01731(12) 0.25127(13) -0.01568(10) 0.0609(4) Uani 1 1 d . . . Cl6 Cl -0.22790(12) 0.02437(14) -0.02011(11) 0.0710(5) Uani 1 1 d . . . Cl7 Cl -0.18388(12) -0.15116(12) 0.10940(11) 0.0662(5) Uani 1 1 d . . . Cl8 Cl 0.07218(13) -0.09976(11) 0.24602(10) 0.0564(4) Uani 1 1 d . . . Cl9 Cl 0.15270(13) 0.44254(12) 0.40620(11) 0.0635(4) Uani 1 1 d . . . Cl10 Cl 0.29456(16) 0.45643(13) 0.60904(11) 0.0736(5) Uani 1 1 d . . . Cl11 Cl 0.51731(15) 0.37744(13) 0.65611(10) 0.0682(5) Uani 1 1 d . . . Cl12 Cl 0.59226(12) 0.27576(13) 0.50330(10) 0.0598(4) Uani 1 1 d . . . O1 O 0.4036(3) 0.3998(2) 0.1995(2) 0.0396(9) Uani 1 1 d . . . O2 O 0.3928(3) 0.2087(2) 0.1644(2) 0.0376(8) Uani 1 1 d . . . O3 O 0.2096(3) 0.2674(2) 0.1286(2) 0.0411(9) Uani 1 1 d . . . O4 O 0.2397(3) 0.1364(3) 0.2394(2) 0.0395(8) Uani 1 1 d . . . O5 O 0.2531(3) 0.3332(3) 0.2813(2) 0.0418(9) Uani 1 1 d . . . O6 O 0.4283(3) 0.2710(3) 0.3188(2) 0.0401(9) Uani 1 1 d . . . P1 P 0.32150(11) 0.27022(11) 0.22163(9) 0.0374(3) Uani 1 1 d . . . S1 S 0.88332(15) 0.17137(17) 0.25114(11) 0.0746(5) Uani 1 1 d . . . S2 S 0.82071(17) 0.26836(18) 0.44207(13) 0.0845(6) Uani 1 1 d . . . S3 S 1.06404(11) 0.10961(12) 0.38362(9) 0.0470(4) Uani 1 1 d . . . S4 S 1.00943(12) 0.18885(12) 0.54010(10) 0.0520(4) Uani 1 1 d . . . S5 S 1.28658(12) 0.05296(12) 0.51465(10) 0.0511(4) Uani 1 1 d . . . S6 S 1.22786(13) 0.13458(12) 0.66870(10) 0.0544(4) Uani 1 1 d . . . S7 S 1.49600(16) 0.00131(16) 0.62080(13) 0.0767(5) Uani 1 1 d . . . S8 S 1.42827(16) 0.10333(15) 0.80428(11) 0.0717(5) Uani 1 1 d . . . C1SA C 1.0012(14) 0.4664(18) 0.8129(12) 0.22(2) Uani 0.50 1 d PD A 1 H1S1 H 1.0251 0.5468 0.8127 0.264 Uiso 0.50 1 calc PR A 1 H1S2 H 1.0480 0.4505 0.8682 0.264 Uiso 0.50 1 calc PR A 1 Cl1A Cl 0.8505(14) 0.413(3) 0.8099(10) 0.48(2) Uani 0.50 1 d PD A 1 Cl2A Cl 1.0331(12) 0.4115(9) 0.7236(10) 0.325(7) Uani 0.50 1 d PD A 1 C1SB C 0.8462(13) 0.4662(19) 0.811(2) 0.43(6) Uani 0.50 1 d PD B 2 H1S3 H 0.8229 0.5181 0.7718 0.515 Uiso 0.50 1 calc PR B 2 H1S4 H 0.7997 0.4542 0.8555 0.515 Uiso 0.50 1 calc PR B 2 Cl1B Cl 0.8153(9) 0.3413(6) 0.7500(8) 0.297(9) Uani 0.50 1 d PD B 2 Cl2B Cl 0.9976(11) 0.5221(8) 0.8644(9) 0.257(6) Uani 0.50 1 d PD B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.120(7) 0.196(10) 0.078(6) 0.012(7) -0.009(5) 0.110(7) C2 0.106(6) 0.196(10) 0.091(6) 0.048(7) 0.037(5) 0.105(7) C3 0.043(3) 0.051(3) 0.043(3) 0.004(3) 0.009(2) 0.012(2) C4 0.043(3) 0.056(3) 0.045(4) 0.006(3) 0.009(3) 0.019(3) C5 0.043(3) 0.046(3) 0.041(3) 0.006(3) 0.016(3) 0.013(2) C6 0.046(3) 0.039(3) 0.042(3) 0.010(3) 0.012(3) 0.007(2) C7 0.054(3) 0.043(3) 0.056(4) 0.015(3) 0.011(3) 0.019(3) C8 0.061(4) 0.039(3) 0.049(4) 0.007(3) 0.007(3) 0.019(3) C9 0.072(5) 0.170(9) 0.128(8) -0.039(7) -0.014(5) 0.077(6) C10 0.071(5) 0.128(7) 0.081(6) -0.003(5) -0.002(4) 0.030(5) C11 0.034(3) 0.033(3) 0.037(3) 0.005(2) 0.010(2) 0.005(2) C12 0.043(3) 0.034(3) 0.037(3) 0.000(2) 0.008(2) 0.012(2) C13 0.038(3) 0.035(3) 0.045(3) 0.012(3) 0.012(2) 0.003(2) C14 0.039(3) 0.050(3) 0.042(3) 0.011(3) 0.019(2) 0.018(2) C15 0.032(3) 0.039(3) 0.034(3) -0.001(2) 0.006(2) 0.010(2) C16 0.035(3) 0.034(3) 0.032(3) 0.004(2) 0.004(2) 0.005(2) C17 0.037(3) 0.039(3) 0.036(3) 0.001(3) 0.013(2) 0.014(2) C18 0.037(3) 0.046(3) 0.035(3) 0.002(3) 0.015(2) 0.015(2) C19 0.027(3) 0.054(3) 0.048(4) -0.015(3) 0.009(2) 0.007(2) C20 0.038(3) 0.039(3) 0.054(4) -0.008(3) 0.020(3) -0.001(2) C21 0.044(3) 0.036(3) 0.046(3) 0.002(3) 0.020(3) 0.010(2) C22 0.039(3) 0.035(3) 0.038(3) 0.005(3) 0.017(2) 0.008(2) C23 0.036(3) 0.032(3) 0.044(4) -0.001(3) 0.018(2) 0.003(2) C24 0.039(3) 0.034(3) 0.057(4) 0.002(3) 0.019(3) 0.003(2) C25 0.061(4) 0.035(3) 0.047(4) -0.005(3) 0.026(3) 0.006(3) C26 0.057(3) 0.034(3) 0.039(3) -0.001(3) 0.018(3) 0.000(3) C27 0.038(3) 0.031(3) 0.050(4) 0.002(3) 0.014(3) 0.003(2) C28 0.038(3) 0.030(3) 0.040(3) -0.003(2) 0.013(2) 0.000(2) Cl1 0.0661(9) 0.0309(7) 0.0611(10) 0.0033(7) 0.0208(7) 0.0077(6) Cl2 0.0685(10) 0.0466(8) 0.0882(12) 0.0157(8) 0.0442(9) 0.0009(7) Cl3 0.0740(10) 0.0614(9) 0.0972(13) 0.0074(9) 0.0570(9) 0.0167(8) Cl4 0.0626(8) 0.0367(7) 0.0681(10) 0.0023(7) 0.0273(7) 0.0159(6) Cl5 0.0580(9) 0.0696(10) 0.0558(10) 0.0166(8) 0.0101(7) 0.0257(7) Cl6 0.0386(8) 0.0828(11) 0.0733(11) -0.0115(9) -0.0040(7) 0.0107(7) Cl7 0.0487(8) 0.0484(8) 0.0846(12) -0.0106(8) 0.0246(8) -0.0099(7) Cl8 0.0644(9) 0.0411(7) 0.0639(10) 0.0126(7) 0.0256(7) 0.0116(7) Cl9 0.0576(9) 0.0611(9) 0.0782(11) 0.0007(8) 0.0263(8) 0.0228(7) Cl10 0.0998(12) 0.0685(10) 0.0607(11) -0.0058(9) 0.0402(9) 0.0260(9) Cl11 0.0896(11) 0.0608(9) 0.0399(9) -0.0005(8) 0.0093(8) 0.0125(8) Cl12 0.0545(8) 0.0654(9) 0.0542(10) 0.0029(8) 0.0040(7) 0.0207(7) O1 0.0361(18) 0.0298(17) 0.049(2) -0.0029(17) 0.0158(16) 0.0024(14) O2 0.0411(19) 0.0290(17) 0.038(2) 0.0019(16) 0.0141(15) 0.0023(14) O3 0.0386(18) 0.0338(18) 0.041(2) 0.0066(17) 0.0082(15) 0.0008(15) O4 0.0359(18) 0.0389(19) 0.036(2) 0.0061(17) 0.0082(15) 0.0029(15) O5 0.0413(19) 0.044(2) 0.037(2) 0.0054(18) 0.0106(16) 0.0105(15) O6 0.0369(18) 0.044(2) 0.036(2) -0.0051(17) 0.0073(15) 0.0116(15) P1 0.0350(7) 0.0349(7) 0.0371(8) 0.0035(6) 0.0106(6) 0.0042(6) S1 0.0793(11) 0.1084(14) 0.0434(10) 0.0082(10) 0.0077(8) 0.0474(10) S2 0.0849(12) 0.1234(16) 0.0693(13) 0.0011(12) 0.0157(9) 0.0704(11) S3 0.0477(8) 0.0535(8) 0.0419(9) 0.0068(7) 0.0157(6) 0.0172(6) S4 0.0573(9) 0.0614(9) 0.0419(9) 0.0039(8) 0.0140(7) 0.0253(7) S5 0.0522(8) 0.0545(9) 0.0497(9) 0.0095(8) 0.0157(7) 0.0203(7) S6 0.0611(9) 0.0604(9) 0.0452(9) 0.0052(8) 0.0078(7) 0.0296(7) S7 0.0783(11) 0.0957(13) 0.0739(13) 0.0095(11) 0.0141(9) 0.0571(10) S8 0.0833(11) 0.0815(12) 0.0523(11) 0.0068(9) -0.0016(8) 0.0444(9) C1SA 0.23(3) 0.11(2) 0.24(4) 0.00(2) -0.13(3) 0.08(2) Cl1A 0.26(2) 1.00(6) 0.223(16) 0.30(3) 0.089(15) 0.23(3) Cl2A 0.447(19) 0.175(8) 0.356(17) 0.042(10) 0.038(14) 0.158(10) C1SB 0.58(12) 0.21(4) 0.55(12) 0.23(6) 0.08(9) 0.23(6) Cl1B 0.188(8) 0.134(6) 0.42(2) 0.135(8) -0.088(10) -0.029(5) Cl2B 0.261(11) 0.177(9) 0.266(13) -0.043(8) -0.017(9) 0.049(8) _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 1.364(11) . ? C1 S1 1.739(8) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 S2 1.796(8) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.352(7) . ? C3 S3 1.732(6) . ? C3 S1 1.747(6) . ? C4 S2 1.733(6) . ? C4 S4 1.734(6) . ? C5 C6 1.382(7) . ? C5 S3 1.721(5) . ? C5 S4 1.724(5) . ? C6 S5 1.717(6) . ? C6 S6 1.726(5) . ? C7 C8 1.340(8) . ? C7 S5 1.750(6) . ? C7 S7 1.752(6) . ? C8 S6 1.730(6) . ? C8 S8 1.746(6) . ? C9 C10 1.396(10) . ? C9 S7 1.778(8) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 S8 1.765(8) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 O1 1.339(5) . ? C11 C12 1.382(7) . ? C11 C16 1.394(7) . ? C12 C13 1.398(7) . ? C12 Cl1 1.720(5) . ? C13 C14 1.393(7) . ? C13 Cl2 1.721(5) . ? C14 C15 1.400(7) . ? C14 Cl3 1.716(5) . ? C15 C16 1.363(6) . ? C15 Cl4 1.729(5) . ? C16 O2 1.350(5) . ? C17 O3 1.344(5) . ? C17 C22 1.366(7) . ? C17 C18 1.381(7) . ? C18 C19 1.403(7) . ? C18 Cl5 1.717(6) . ? C19 C20 1.377(8) . ? C19 Cl6 1.724(5) . ? C20 C21 1.414(7) . ? C20 Cl7 1.733(5) . ? C21 C22 1.390(6) . ? C21 Cl8 1.716(6) . ? C22 O4 1.362(5) . ? C23 O5 1.346(6) . ? C23 C24 1.371(7) . ? C23 C28 1.391(7) . ? C24 C25 1.411(8) . ? C24 Cl9 1.720(6) . ? C25 C26 1.373(8) . ? C25 Cl10 1.726(5) . ? C26 C27 1.395(7) . ? C26 Cl11 1.734(6) . ? C27 C28 1.379(7) . ? C27 Cl12 1.714(5) . ? C28 O6 1.359(6) . ? O1 P1 1.713(3) . ? O2 P1 1.714(3) . ? O3 P1 1.715(4) . ? O4 P1 1.732(3) . ? O5 P1 1.723(4) . ? O6 P1 1.730(3) . ? C1SA Cl2A 1.718(5) . ? C1SA Cl1A 1.719(5) . ? C1SA H1S1 0.9700 . ? C1SA H1S2 0.9700 . ? C1SB Cl2B 1.720(5) . ? C1SB Cl1B 1.722(5) . ? C1SB H1S3 0.9700 . ? C1SB H1S4 0.9700 . ? 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 S1 124.9(8) . . ? C2 C1 H1A 106.1 . . ? S1 C1 H1A 106.1 . . ? C2 C1 H1B 106.1 . . ? S1 C1 H1B 106.1 . . ? H1A C1 H1B 106.3 . . ? C1 C2 S2 120.5(6) . . ? C1 C2 H2A 107.2 . . ? S2 C2 H2A 107.2 . . ? C1 C2 H2B 107.2 . . ? S2 C2 H2B 107.2 . . ? H2A C2 H2B 106.8 . . ? C4 C3 S3 117.0(4) . . ? C4 C3 S1 127.6(5) . . ? S3 C3 S1 115.4(3) . . ? C3 C4 S2 129.5(5) . . ? C3 C4 S4 116.3(4) . . ? S2 C4 S4 114.2(3) . . ? C6 C5 S3 122.5(4) . . ? C6 C5 S4 122.3(4) . . ? S3 C5 S4 115.0(3) . . ? C5 C6 S5 123.6(4) . . ? C5 C6 S6 120.8(4) . . ? S5 C6 S6 115.5(3) . . ? C8 C7 S5 117.0(4) . . ? C8 C7 S7 128.1(5) . . ? S5 C7 S7 114.9(4) . . ? C7 C8 S6 116.8(4) . . ? C7 C8 S8 127.3(5) . . ? S6 C8 S8 115.9(3) . . ? C10 C9 S7 121.9(6) . . ? C10 C9 H9A 106.8 . . ? S7 C9 H9A 106.8 . . ? C10 C9 H9B 106.8 . . ? S7 C9 H9B 106.8 . . ? H9A C9 H9B 106.7 . . ? C9 C10 S8 118.6(6) . . ? C9 C10 H10A 107.7 . . ? S8 C10 H10A 107.7 . . ? C9 C10 H10B 107.7 . . ? S8 C10 H10B 107.7 . . ? H10A C10 H10B 107.1 . . ? O1 C11 C12 126.5(4) . . ? O1 C11 C16 113.2(4) . . ? C12 C11 C16 120.3(5) . . ? C11 C12 C13 118.5(4) . . ? C11 C12 Cl1 119.9(4) . . ? C13 C12 Cl1 121.6(4) . . ? C14 C13 C12 120.8(4) . . ? C14 C13 Cl2 119.7(4) . . ? C12 C13 Cl2 119.5(4) . . ? C13 C14 C15 119.8(4) . . ? C13 C14 Cl3 120.8(4) . . ? C15 C14 Cl3 119.4(4) . . ? C16 C15 C14 118.9(4) . . ? C16 C15 Cl4 120.3(4) . . ? C14 C15 Cl4 120.7(4) . . ? O2 C16 C15 125.8(4) . . ? O2 C16 C11 112.6(4) . . ? C15 C16 C11 121.6(5) . . ? O3 C17 C22 113.7(4) . . ? O3 C17 C18 125.0(5) . . ? C22 C17 C18 121.3(4) . . ? C17 C18 C19 117.8(5) . . ? C17 C18 Cl5 120.4(4) . . ? C19 C18 Cl5 121.7(4) . . ? C20 C19 C18 120.9(5) . . ? C20 C19 Cl6 119.6(4) . . ? C18 C19 Cl6 119.5(5) . . ? C19 C20 C21 121.0(4) . . ? C19 C20 Cl7 120.7(4) . . ? C21 C20 Cl7 118.3(5) . . ? C22 C21 C20 116.6(5) . . ? C22 C21 Cl8 120.6(4) . . ? C20 C21 Cl8 122.7(4) . . ? O4 C22 C17 113.7(4) . . ? O4 C22 C21 124.1(5) . . ? C17 C22 C21 122.2(5) . . ? O5 C23 C24 126.1(5) . . ? O5 C23 C28 112.9(4) . . ? C24 C23 C28 121.0(5) . . ? C23 C24 C25 118.3(5) . . ? C23 C24 Cl9 120.1(4) . . ? C25 C24 Cl9 121.6(4) . . ? C26 C25 C24 120.3(5) . . ? C26 C25 Cl10 120.2(5) . . ? C24 C25 Cl10 119.5(5) . . ? C25 C26 C27 121.3(5) . . ? C25 C26 Cl11 120.4(4) . . ? C27 C26 Cl11 118.4(5) . . ? C28 C27 C26 118.1(5) . . ? C28 C27 Cl12 119.8(4) . . ? C26 C27 Cl12 122.1(4) . . ? O6 C28 C27 125.6(5) . . ? O6 C28 C23 113.3(4) . . ? C27 C28 C23 121.1(5) . . ? C11 O1 P1 111.8(3) . . ? C16 O2 P1 111.6(3) . . ? C17 O3 P1 111.2(3) . . ? C22 O4 P1 110.0(3) . . ? C23 O5 P1 112.0(3) . . ? C28 O6 P1 111.1(3) . . ? O1 P1 O2 90.82(16) . . ? O1 P1 O3 88.25(17) . . ? O2 P1 O3 94.33(17) . . ? O1 P1 O5 88.79(16) . . ? O2 P1 O5 178.57(17) . . ? O3 P1 O5 87.03(17) . . ? O1 P1 O6 93.79(16) . . ? O2 P1 O6 88.07(16) . . ? O3 P1 O6 176.83(18) . . ? O5 P1 O6 90.58(16) . . ? O1 P1 O4 177.17(18) . . ? O2 P1 O4 86.59(16) . . ? O3 P1 O4 90.80(15) . . ? O5 P1 O4 93.82(16) . . ? O6 P1 O4 87.28(16) . . ? C1 S1 C3 100.4(3) . . ? C4 S2 C2 101.8(3) . . ? C5 S3 C3 95.7(3) . . ? C5 S4 C4 96.0(3) . . ? C6 S5 C7 95.1(3) . . ? C6 S6 C8 95.7(3) . . ? C7 S7 C9 102.4(3) . . ? C8 S8 C10 99.9(3) . . ? Cl2A C1SA Cl1A 112.2(5) . . ? Cl2A C1SA H1S1 109.2 . . ? Cl1A C1SA H1S1 109.2 . . ? Cl2A C1SA H1S2 109.2 . . ? Cl1A C1SA H1S2 109.2 . . ? H1S1 C1SA H1S2 107.9 . . ? Cl2B C1SB Cl1B 110.4(4) . . ? Cl2B C1SB H1S3 109.6 . . ? Cl1B C1SB H1S3 109.6 . . ? Cl2B C1SB H1S4 109.6 . . ? Cl1B C1SB H1S4 109.6 . . ? H1S3 C1SB H1S4 108.1 . . ? _diffrn_measured_fraction_theta_max 0.923 _diffrn_reflns_theta_full 25.98 _diffrn_measured_fraction_theta_full 0.923 _refine_diff_density_max 0.423 _refine_diff_density_min -0.299 _refine_diff_density_rms 0.074 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 820752' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common BEDT-Trisphat _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H14 Cl12 N2 O6 P S8' _chemical_formula_weight 1235.30 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' 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' _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 10.2344(12) _cell_length_b 14.6453(18) _cell_length_c 16.1178(19) _cell_angle_alpha 81.546(14) _cell_angle_beta 75.286(14) _cell_angle_gamma 79.334(14) _cell_volume 2283.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5788 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 24.50 _exptl_crystal_description prism _exptl_crystal_colour violet _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.797 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1230 _exptl_absorpt_coefficient_mu 1.175 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8224 _exptl_absorpt_correction_T_max 0.9069 _exptl_absorpt_process_details wingx _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE-IPDS I' _diffrn_measurement_method 'Oscillation, Phi. incr. = 1.4' _diffrn_detector_area_resol_mean 6.6 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20911 _diffrn_reflns_av_R_equivalents 0.1424 _diffrn_reflns_av_sigmaI/netI 0.2023 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 24.94 _reflns_number_total 7512 _reflns_number_gt 3030 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE [STOE-IPDS]' _computing_cell_refinement 'SELECT, CELL [STOE-IPDS]' _computing_data_reduction 'INTEGRATE [STOE-IPDS]' _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 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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7512 _refine_ls_number_parameters 552 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1480 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.0799 _refine_ls_wR_factor_gt 0.0672 _refine_ls_goodness_of_fit_ref 0.688 _refine_ls_restrained_S_all 0.695 _refine_ls_shift/su_max 0.064 _refine_ls_shift/su_mean 0.003 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 0.5926(9) 0.7391(7) 0.3028(6) 0.127(4) Uani 1 1 d D . . H1A H 0.6450 0.6836 0.2774 0.153 Uiso 1 1 calc R . . H1B H 0.5485 0.7191 0.3617 0.153 Uiso 1 1 calc R . . C2 C 0.4833(7) 0.7752(6) 0.2559(4) 0.078(3) Uani 1 1 d D . . H2A H 0.4189 0.8216 0.2890 0.093 Uiso 1 1 calc R . . H2B H 0.4349 0.7239 0.2567 0.093 Uiso 1 1 calc R . . C3 C 0.7665(6) 0.8379(4) 0.1952(4) 0.0448(17) Uani 1 1 d . . . C4 C 0.6929(6) 0.8430(4) 0.1360(4) 0.0395(16) Uani 1 1 d . . . C5 C 0.9376(6) 0.8730(4) 0.0532(4) 0.0385(16) Uani 1 1 d . . . C6 C 1.0536(6) 0.8898(4) -0.0090(4) 0.0388(16) Uani 1 1 d . . . C7 C 1.3001(6) 0.9011(4) -0.0928(4) 0.0368(15) Uani 1 1 d . . . C8 C 1.2302(6) 0.9054(4) -0.1518(4) 0.0437(17) Uani 1 1 d . . . C9 C 1.5325(8) 0.8927(9) -0.2118(6) 0.156(6) Uani 1 1 d D . . H9A H 1.6101 0.9261 -0.2311 0.188 Uiso 1 1 calc R . . H9B H 1.5702 0.8270 -0.2129 0.188 Uiso 1 1 calc R . . C10 C 1.4591(10) 0.9147(11) -0.2821(7) 0.182(6) Uani 1 1 d DU . . H10A H 1.5038 0.8714 -0.3245 0.219 Uiso 1 1 calc R . . H10B H 1.4754 0.9765 -0.3094 0.219 Uiso 1 1 calc R . . C11 C 0.8074(5) 0.6655(4) 0.6210(4) 0.0323(15) Uani 1 1 d . . . C12 C 0.7309(5) 0.6551(4) 0.5665(4) 0.0369(16) Uani 1 1 d . . . C13 C 0.7420(6) 0.5667(5) 0.5386(4) 0.0415(16) Uani 1 1 d . . . C14 C 0.8277(6) 0.4913(4) 0.5682(4) 0.0375(15) Uani 1 1 d . . . C15 C 0.9072(5) 0.5014(4) 0.6240(4) 0.0385(16) Uani 1 1 d . . . C16 C 0.8931(6) 0.5898(4) 0.6509(4) 0.0358(16) Uani 1 1 d . . . C17 C 0.8034(6) 0.6751(4) 0.8799(4) 0.0381(16) Uani 1 1 d . . . C18 C 0.7099(6) 0.6473(4) 0.9564(4) 0.0411(16) Uani 1 1 d . . . C19 C 0.7609(7) 0.6170(4) 1.0290(4) 0.0421(16) Uani 1 1 d . . . C20 C 0.8956(7) 0.6183(4) 1.0299(4) 0.0524(19) Uani 1 1 d . . . C21 C 0.9902(6) 0.6478(4) 0.9506(4) 0.0408(16) Uani 1 1 d . . . C22 C 0.9381(6) 0.6759(4) 0.8795(4) 0.0326(14) Uani 1 1 d . . . C23 C 0.9509(6) 0.8955(4) 0.6851(4) 0.0398(16) Uani 1 1 d . . . C24 C 0.9375(6) 0.9917(4) 0.6784(5) 0.0481(19) Uani 1 1 d . . . C25 C 1.0314(8) 1.0352(4) 0.6135(5) 0.0491(19) Uani 1 1 d . . . C26 C 1.1332(7) 0.9844(5) 0.5596(5) 0.052(2) Uani 1 1 d . . . C27 C 1.1487(6) 0.8857(4) 0.5672(4) 0.0452(18) Uani 1 1 d . . . C28 C 1.0542(6) 0.8448(4) 0.6314(4) 0.0353(15) Uani 1 1 d . . . Cl1 Cl 0.61992(16) 0.74945(12) 0.53429(11) 0.0548(5) Uani 1 1 d . . . Cl2 Cl 0.64369(18) 0.55305(13) 0.47064(12) 0.0652(6) Uani 1 1 d . . . Cl3 Cl 0.8386(2) 0.38259(12) 0.53542(13) 0.0695(6) Uani 1 1 d . . . Cl4 Cl 1.01521(17) 0.41032(11) 0.66233(12) 0.0574(5) Uani 1 1 d . . . Cl5 Cl 0.54309(16) 0.64793(13) 0.95437(12) 0.0622(5) Uani 1 1 d . . . Cl6 Cl 0.65270(19) 0.57608(13) 1.12225(12) 0.0708(6) Uani 1 1 d . . . Cl7 Cl 0.9529(2) 0.58584(14) 1.12153(12) 0.0765(6) Uani 1 1 d . . . Cl8 Cl 1.15659(17) 0.65023(13) 0.94755(12) 0.0630(5) Uani 1 1 d . . . Cl9 Cl 0.80711(19) 1.05114(13) 0.75055(15) 0.0798(6) Uani 1 1 d . . . Cl10 Cl 1.0142(2) 1.15616(12) 0.60516(16) 0.0938(8) Uani 1 1 d . . . Cl11 Cl 1.2498(2) 1.04025(15) 0.48026(14) 0.0915(8) Uani 1 1 d . . . Cl12 Cl 1.27821(16) 0.82021(13) 0.50128(12) 0.0644(5) Uani 1 1 d . . . O1 O 0.8091(4) 0.7449(3) 0.6539(2) 0.0381(10) Uani 1 1 d . . . O2 O 0.9599(4) 0.6108(2) 0.7058(2) 0.0374(10) Uani 1 1 d . . . O3 O 0.7703(3) 0.7043(3) 0.8044(3) 0.0424(11) Uani 1 1 d . . . O4 O 1.0107(4) 0.7043(3) 0.7993(3) 0.0424(11) Uani 1 1 d . . . O5 O 0.8667(4) 0.8426(3) 0.7422(3) 0.0416(11) Uani 1 1 d . . . O6 O 1.0539(3) 0.7509(3) 0.6462(2) 0.0368(10) Uani 1 1 d . . . P1 P 0.91198(16) 0.72605(12) 0.72488(11) 0.0371(4) Uani 1 1 d . . . S1 S 0.70750(19) 0.81022(16) 0.30714(12) 0.0715(6) Uani 1 1 d . . . S2 S 0.52720(16) 0.82619(13) 0.14725(12) 0.0541(5) Uani 1 1 d . . . S3 S 0.93617(16) 0.85316(13) 0.16143(11) 0.0506(5) Uani 1 1 d . . . S4 S 0.78487(15) 0.86575(12) 0.02877(11) 0.0445(4) Uani 1 1 d . . . S5 S 1.20703(16) 0.89023(12) 0.01512(11) 0.0493(5) Uani 1 1 d . . . S6 S 1.05610(15) 0.90015(12) -0.11770(11) 0.0448(4) Uani 1 1 d . . . S7 S 1.47230(17) 0.90799(14) -0.10471(14) 0.0653(6) Uani 1 1 d . . . S8 S 1.2908(2) 0.91402(18) -0.26447(13) 0.0801(7) Uani 1 1 d U . . C1S C 0.2652(7) 0.6482(7) 0.1661(5) 0.060(2) Uani 1 1 d . . . C2S C 0.2940(7) 0.5479(5) 0.1567(5) 0.068(2) Uani 1 1 d . . . H2S1 H 0.3215 0.5389 0.0965 0.103 Uiso 1 1 calc R . . H2S2 H 0.2132 0.5204 0.1829 0.103 Uiso 1 1 calc R . . H2S3 H 0.3662 0.5188 0.1844 0.103 Uiso 1 1 calc R . . N1S N 0.2483(7) 0.7246(5) 0.1707(5) 0.088(2) Uani 1 1 d . . . C3S C 0.5718(9) 0.4549(8) 0.3073(6) 0.094(3) Uani 1 1 d . . . C4S C 0.6834(9) 0.3842(6) 0.3159(6) 0.112(3) Uani 1 1 d . . . H4S1 H 0.7674 0.4085 0.2915 0.169 Uiso 1 1 calc R . . H4S2 H 0.6811 0.3326 0.2861 0.169 Uiso 1 1 calc R . . H4S3 H 0.6775 0.3634 0.3759 0.169 Uiso 1 1 calc R . . N2S N 0.4861(8) 0.5155(7) 0.3043(6) 0.120(3) Uani 1 1 d . . . 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 0.144(8) 0.184(11) 0.070(6) 0.053(7) -0.038(6) -0.097(8) C2 0.069(5) 0.113(7) 0.049(5) 0.031(5) -0.008(4) -0.048(5) C3 0.047(4) 0.040(4) 0.043(4) -0.001(3) -0.012(3) 0.004(3) C4 0.052(4) 0.031(4) 0.031(4) -0.009(3) -0.005(3) 0.002(3) C5 0.043(4) 0.026(4) 0.041(4) -0.008(3) -0.001(3) 0.000(3) C6 0.048(4) 0.018(3) 0.047(4) -0.008(3) -0.006(3) -0.001(3) C7 0.038(3) 0.030(4) 0.040(4) -0.003(3) -0.006(3) -0.003(3) C8 0.039(4) 0.041(4) 0.050(5) -0.008(4) -0.004(3) -0.008(3) C9 0.040(5) 0.276(16) 0.092(8) 0.031(9) 0.036(5) 0.016(7) C10 0.101(8) 0.356(18) 0.092(9) -0.061(11) 0.017(7) -0.069(10) C11 0.037(3) 0.035(4) 0.023(3) 0.002(3) -0.004(3) -0.010(3) C12 0.039(3) 0.036(4) 0.033(4) 0.010(3) -0.005(3) -0.016(3) C13 0.039(4) 0.051(4) 0.039(4) -0.010(4) -0.004(3) -0.020(3) C14 0.044(4) 0.032(4) 0.038(4) -0.010(3) -0.005(3) -0.011(3) C15 0.039(3) 0.036(4) 0.039(4) 0.001(3) -0.003(3) -0.013(3) C16 0.040(3) 0.042(4) 0.028(4) 0.005(3) -0.006(3) -0.023(3) C17 0.050(4) 0.031(4) 0.035(4) -0.007(3) -0.009(3) -0.011(3) C18 0.050(4) 0.033(4) 0.038(4) -0.009(3) -0.002(3) -0.008(3) C19 0.059(4) 0.029(4) 0.033(4) -0.007(3) 0.000(3) -0.005(3) C20 0.079(5) 0.031(4) 0.050(5) -0.006(4) -0.032(4) 0.007(4) C21 0.049(4) 0.032(4) 0.043(4) -0.010(3) -0.016(4) 0.003(3) C22 0.043(4) 0.022(3) 0.031(4) -0.015(3) 0.003(3) -0.005(3) C23 0.033(4) 0.036(4) 0.058(5) -0.015(4) -0.018(3) -0.006(3) C24 0.047(4) 0.025(4) 0.082(6) -0.013(4) -0.037(4) 0.006(3) C25 0.067(5) 0.023(4) 0.068(5) 0.000(4) -0.032(4) -0.012(4) C26 0.056(4) 0.046(5) 0.066(5) 0.015(4) -0.033(4) -0.028(4) C27 0.051(4) 0.038(4) 0.054(5) 0.004(4) -0.026(4) -0.012(3) C28 0.032(3) 0.032(4) 0.043(4) -0.001(3) -0.008(3) -0.010(3) Cl1 0.0576(10) 0.0526(11) 0.0586(12) 0.0003(9) -0.0254(9) -0.0082(9) Cl2 0.0732(12) 0.0734(13) 0.0647(13) -0.0122(11) -0.0287(11) -0.0295(10) Cl3 0.0924(13) 0.0434(11) 0.0806(14) -0.0219(11) -0.0190(12) -0.0203(10) Cl4 0.0656(11) 0.0374(10) 0.0649(13) 0.0012(9) -0.0140(10) -0.0039(9) Cl5 0.0504(10) 0.0658(13) 0.0621(13) 0.0045(11) 0.0022(9) -0.0183(9) Cl6 0.0884(13) 0.0587(13) 0.0482(12) 0.0071(11) 0.0058(10) -0.0084(11) Cl7 0.1001(15) 0.0802(15) 0.0490(12) 0.0050(11) -0.0298(12) -0.0056(12) Cl8 0.0618(11) 0.0630(13) 0.0712(14) -0.0082(11) -0.0324(11) -0.0028(10) Cl9 0.0731(12) 0.0599(13) 0.1160(18) -0.0456(13) -0.0386(13) 0.0170(11) Cl10 0.1310(18) 0.0312(11) 0.145(2) 0.0088(13) -0.0844(17) -0.0198(11) Cl11 0.1129(16) 0.0808(16) 0.0895(17) 0.0365(13) -0.0314(14) -0.0617(13) Cl12 0.0513(10) 0.0758(14) 0.0567(12) 0.0001(11) 0.0045(9) -0.0155(10) O1 0.050(2) 0.027(2) 0.040(3) -0.003(2) -0.014(2) -0.010(2) O2 0.047(2) 0.027(2) 0.041(3) -0.001(2) -0.014(2) -0.009(2) O3 0.037(2) 0.055(3) 0.038(3) -0.007(2) -0.005(2) -0.018(2) O4 0.036(2) 0.052(3) 0.042(3) -0.009(2) -0.009(2) -0.013(2) O5 0.033(2) 0.039(3) 0.053(3) -0.020(2) 0.000(2) -0.008(2) O6 0.035(2) 0.029(3) 0.042(3) -0.006(2) 0.000(2) -0.0059(19) P1 0.0377(9) 0.0396(11) 0.0357(10) -0.0071(9) -0.0054(8) -0.0118(8) S1 0.0663(12) 0.1105(18) 0.0402(12) 0.0102(12) -0.0128(10) -0.0335(12) S2 0.0426(10) 0.0637(13) 0.0528(12) 0.0104(10) -0.0103(9) -0.0141(9) S3 0.0424(9) 0.0635(12) 0.0452(11) 0.0031(10) -0.0125(9) -0.0097(9) S4 0.0468(10) 0.0454(11) 0.0419(11) -0.0078(9) -0.0069(9) -0.0110(8) S5 0.0491(10) 0.0542(12) 0.0459(11) 0.0041(10) -0.0164(9) -0.0116(9) S6 0.0432(9) 0.0547(12) 0.0397(10) -0.0114(9) -0.0075(8) -0.0138(9) S7 0.0365(10) 0.0726(14) 0.0857(16) 0.0021(12) -0.0154(10) -0.0121(10) S8 0.0646(13) 0.136(2) 0.0424(12) -0.0210(13) 0.0041(10) -0.0374(14) C1S 0.051(4) 0.070(6) 0.054(5) -0.007(5) -0.006(4) -0.009(5) C2S 0.065(5) 0.062(6) 0.079(6) -0.013(5) -0.017(4) -0.007(4) N1S 0.094(5) 0.061(5) 0.107(6) -0.012(5) -0.026(5) -0.005(4) C3S 0.060(6) 0.125(9) 0.074(7) 0.034(6) 0.002(5) -0.016(6) C4S 0.105(7) 0.093(7) 0.113(8) -0.012(6) -0.010(6) 0.029(6) N2S 0.073(5) 0.154(9) 0.110(7) 0.027(6) -0.009(5) -0.006(5) _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 1.481(12) . ? C1 S1 1.730(8) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 S2 1.780(6) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.344(7) . ? C3 S3 1.729(6) . ? C3 S1 1.762(6) . ? C4 S2 1.719(6) . ? C4 S4 1.762(6) . ? C5 C6 1.381(7) . ? C5 S3 1.723(6) . ? C5 S4 1.730(6) . ? C6 S5 1.713(6) . ? C6 S6 1.730(6) . ? C7 C8 1.316(8) . ? C7 S7 1.744(6) . ? C7 S5 1.758(6) . ? C8 S6 1.738(6) . ? C8 S8 1.757(7) . ? C9 C10 1.479(11) . ? C9 S7 1.712(10) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 S8 1.674(9) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 O1 1.350(6) . ? C11 C12 1.358(7) . ? C11 C16 1.389(7) . ? C12 C13 1.408(8) . ? C12 Cl1 1.725(6) . ? C13 C14 1.383(8) . ? C13 Cl2 1.717(6) . ? C14 C15 1.396(8) . ? C14 Cl3 1.726(6) . ? C15 C16 1.397(8) . ? C15 Cl4 1.715(6) . ? C16 O2 1.345(6) . ? C17 O3 1.334(6) . ? C17 C22 1.379(7) . ? C17 C18 1.415(8) . ? C18 C19 1.382(8) . ? C18 Cl5 1.714(6) . ? C19 C20 1.386(8) . ? C19 Cl6 1.726(6) . ? C20 C21 1.456(8) . ? C20 Cl7 1.697(6) . ? C21 C22 1.363(7) . ? C21 Cl8 1.698(6) . ? C22 O4 1.367(6) . ? C23 O5 1.351(7) . ? C23 C28 1.360(8) . ? C23 C24 1.382(8) . ? C24 C25 1.395(9) . ? C24 Cl9 1.723(7) . ? C25 C26 1.355(9) . ? C25 Cl10 1.736(6) . ? C26 C27 1.416(8) . ? C26 Cl11 1.734(7) . ? C27 C28 1.374(8) . ? C27 Cl12 1.708(7) . ? C28 O6 1.362(6) . ? O1 P1 1.705(4) . ? O2 P1 1.719(4) . ? O3 P1 1.719(4) . ? O4 P1 1.715(4) . ? O5 P1 1.728(4) . ? O6 P1 1.724(4) . ? C1S N1S 1.111(9) . ? C1S C2S 1.466(11) . ? C2S H2S1 0.9600 . ? C2S H2S2 0.9600 . ? C2S H2S3 0.9600 . ? C3S N2S 1.131(10) . ? C3S C4S 1.413(11) . ? C4S H4S1 0.9600 . ? C4S H4S2 0.9600 . ? C4S H4S3 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 C2 C1 S1 119.8(6) . . ? C2 C1 H1A 107.4 . . ? S1 C1 H1A 107.4 . . ? C2 C1 H1B 107.4 . . ? S1 C1 H1B 107.4 . . ? H1A C1 H1B 106.9 . . ? C1 C2 S2 119.5(5) . . ? C1 C2 H2A 107.5 . . ? S2 C2 H2A 107.5 . . ? C1 C2 H2B 107.5 . . ? S2 C2 H2B 107.5 . . ? H2A C2 H2B 107.0 . . ? C4 C3 S3 119.2(5) . . ? C4 C3 S1 125.3(5) . . ? S3 C3 S1 115.4(3) . . ? C3 C4 S2 130.8(5) . . ? C3 C4 S4 114.2(4) . . ? S2 C4 S4 115.0(3) . . ? C6 C5 S3 122.2(4) . . ? C6 C5 S4 123.0(4) . . ? S3 C5 S4 114.8(3) . . ? C5 C6 S5 122.7(5) . . ? C5 C6 S6 121.2(4) . . ? S5 C6 S6 115.7(4) . . ? C8 C7 S7 129.9(5) . . ? C8 C7 S5 116.2(5) . . ? S7 C7 S5 113.9(3) . . ? C7 C8 S6 118.3(5) . . ? C7 C8 S8 128.1(5) . . ? S6 C8 S8 113.6(3) . . ? C10 C9 S7 129.1(7) . . ? C10 C9 H9A 105.0 . . ? S7 C9 H9A 105.0 . . ? C10 C9 H9B 105.0 . . ? S7 C9 H9B 105.0 . . ? H9A C9 H9B 105.9 . . ? C9 C10 S8 122.3(7) . . ? C9 C10 H10A 106.7 . . ? S8 C10 H10A 106.7 . . ? C9 C10 H10B 106.8 . . ? S8 C10 H10B 106.8 . . ? H10A C10 H10B 106.6 . . ? O1 C11 C12 126.8(5) . . ? O1 C11 C16 112.5(5) . . ? C12 C11 C16 120.8(6) . . ? C11 C12 C13 119.1(5) . . ? C11 C12 Cl1 119.6(5) . . ? C13 C12 Cl1 121.3(4) . . ? C14 C13 C12 120.1(5) . . ? C14 C13 Cl2 120.7(5) . . ? C12 C13 Cl2 119.2(5) . . ? C13 C14 C15 121.3(6) . . ? C13 C14 Cl3 119.9(5) . . ? C15 C14 Cl3 118.8(5) . . ? C14 C15 C16 117.2(5) . . ? C14 C15 Cl4 123.1(5) . . ? C16 C15 Cl4 119.7(4) . . ? O2 C16 C11 113.8(6) . . ? O2 C16 C15 124.7(5) . . ? C11 C16 C15 121.5(5) . . ? O3 C17 C22 114.9(5) . . ? O3 C17 C18 124.2(5) . . ? C22 C17 C18 120.9(6) . . ? C19 C18 C17 117.1(5) . . ? C19 C18 Cl5 123.3(5) . . ? C17 C18 Cl5 119.5(5) . . ? C18 C19 C20 122.6(6) . . ? C18 C19 Cl6 118.8(5) . . ? C20 C19 Cl6 118.7(5) . . ? C19 C20 C21 119.4(5) . . ? C19 C20 Cl7 121.3(6) . . ? C21 C20 Cl7 119.3(5) . . ? C22 C21 C20 116.9(5) . . ? C22 C21 Cl8 121.5(5) . . ? C20 C21 Cl8 121.6(5) . . ? C21 C22 O4 125.6(5) . . ? C21 C22 C17 123.0(6) . . ? O4 C22 C17 111.4(5) . . ? O5 C23 C28 113.5(5) . . ? O5 C23 C24 125.5(6) . . ? C28 C23 C24 121.0(6) . . ? C23 C24 C25 117.7(6) . . ? C23 C24 Cl9 118.5(6) . . ? C25 C24 Cl9 123.7(5) . . ? C26 C25 C24 120.9(6) . . ? C26 C25 Cl10 121.5(6) . . ? C24 C25 Cl10 117.6(6) . . ? C25 C26 C27 121.5(6) . . ? C25 C26 Cl11 119.9(6) . . ? C27 C26 Cl11 118.5(6) . . ? C28 C27 C26 116.2(6) . . ? C28 C27 Cl12 121.5(5) . . ? C26 C27 Cl12 122.3(5) . . ? C23 C28 O6 114.1(5) . . ? C23 C28 C27 122.5(6) . . ? O6 C28 C27 123.4(6) . . ? C11 O1 P1 111.7(3) . . ? C16 O2 P1 110.7(4) . . ? C17 O3 P1 111.1(3) . . ? C22 O4 P1 111.8(3) . . ? C23 O5 P1 111.1(4) . . ? C28 O6 P1 110.4(4) . . ? O1 P1 O4 177.6(2) . . ? O1 P1 O3 87.20(18) . . ? O4 P1 O3 90.55(19) . . ? O1 P1 O2 91.27(19) . . ? O4 P1 O2 87.91(19) . . ? O3 P1 O2 93.4(2) . . ? O1 P1 O6 93.35(19) . . ? O4 P1 O6 88.93(18) . . ? O3 P1 O6 178.3(2) . . ? O2 P1 O6 88.2(2) . . ? O1 P1 O5 88.70(19) . . ? O4 P1 O5 92.18(19) . . ? O3 P1 O5 87.8(2) . . ? O2 P1 O5 178.8(2) . . ? O6 P1 O5 90.59(19) . . ? C1 S1 C3 97.7(4) . . ? C4 S2 C2 102.5(3) . . ? C5 S3 C3 95.4(3) . . ? C5 S4 C4 96.4(3) . . ? C6 S5 C7 95.2(3) . . ? C6 S6 C8 94.6(3) . . ? C9 S7 C7 99.9(4) . . ? C10 S8 C8 105.4(4) . . ? N1S C1S C2S 177.1(10) . . ? C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? N2S C3S C4S 174.5(13) . . ? C3S C4S H4S1 109.5 . . ? C3S C4S H4S2 109.5 . . ? H4S1 C4S H4S2 109.5 . . ? C3S C4S H4S3 109.5 . . ? H4S1 C4S H4S3 109.5 . . ? H4S2 C4S H4S3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 24.94 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 0.461 _refine_diff_density_min -0.349 _refine_diff_density_rms 0.065 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 820753' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[{(R/S)-EDT-TTF-oxazoline}Trisphat]' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H14 Cl12 N2 O7 P S6' _chemical_formula_weight 1187.18 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 11.7420(8) _cell_length_b 12.2491(8) _cell_length_c 16.3553(12) _cell_angle_alpha 96.874(8) _cell_angle_beta 101.997(8) _cell_angle_gamma 104.320(7) _cell_volume 2192.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 149 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 24 _exptl_crystal_description prism _exptl_crystal_colour brown-red _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.798 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1182 _exptl_absorpt_coefficient_mu 1.129 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7543 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi_omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17528 _diffrn_reflns_av_R_equivalents 0.0468 _diffrn_reflns_av_sigmaI/netI 0.1169 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.37 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8407 _reflns_number_gt 4094 _reflns_threshold_expression >2sigma(I) _computing_data_collection KappaCCD _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'Denzo and Scalepak' _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 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^)+(0.0443P)^2^+1.3280P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8407 _refine_ls_number_parameters 542 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1562 _refine_ls_R_factor_gt 0.0590 _refine_ls_wR_factor_ref 0.1278 _refine_ls_wR_factor_gt 0.1028 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.002 _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 S1 S 0.56374(13) 1.14865(11) -0.07723(9) 0.0495(4) Uani 1 1 d . . . S2 S 0.49028(15) 1.17654(12) 0.08295(9) 0.0581(4) Uani 1 1 d . . . S3 S 0.79878(14) 1.07625(11) 0.02526(9) 0.0510(4) Uani 1 1 d . . . S4 S 0.70910(15) 1.09503(12) 0.17716(9) 0.0594(4) Uani 1 1 d . . . S5 S 1.03070(18) 1.03933(16) 0.11117(12) 0.0811(6) Uani 1 1 d . . . S6 S 0.9121(2) 1.04807(16) 0.29009(11) 0.0883(6) Uani 1 1 d . . . C1 C 0.4383(5) 1.1998(4) -0.0768(4) 0.0489(15) Uani 1 1 d . . . C2 C 0.4064(5) 1.2122(4) -0.0032(4) 0.0510(15) Uani 1 1 d . . . H2 H 0.3403 1.2395 0.0012 0.061 Uiso 1 1 calc R . . C3 C 0.5921(5) 1.1386(4) 0.0294(3) 0.0462(14) Uani 1 1 d . . . C4 C 0.6898(5) 1.1064(4) 0.0719(3) 0.0435(14) Uani 1 1 d . . . C5 C 0.8923(5) 1.0577(4) 0.1180(4) 0.0519(15) Uani 1 1 d . . . C6 C 0.8479(6) 1.0646(4) 0.1888(4) 0.0541(16) Uani 1 1 d . . . C7 C 1.0660(9) 0.9761(7) 0.2030(5) 0.115(3) Uani 1 1 d . . . H7A H 1.0145 0.8979 0.1909 0.138 Uiso 1 1 calc R . . H7B H 1.1491 0.9725 0.2112 0.138 Uiso 1 1 calc R . . C8 C 1.0536(9) 1.0309(10) 0.2807(6) 0.150(4) Uani 1 1 d . . . H8A H 1.1108 1.1065 0.2948 0.180 Uiso 1 1 calc R . . H8B H 1.0795 0.9887 0.3242 0.180 Uiso 1 1 calc R . . C9 C 0.3796(5) 1.2269(4) -0.1576(4) 0.0508(15) Uani 1 1 d . . . C10 C 0.2394(8) 1.2833(7) -0.2407(4) 0.102(3) Uani 1 1 d . . . H10A H 0.2304 1.3598 -0.2415 0.122 Uiso 1 1 calc R . . H10B H 0.1620 1.2278 -0.2680 0.122 Uiso 1 1 calc R . . C11 C 0.3358(7) 1.2652(6) -0.2835(4) 0.080(2) Uani 1 1 d . . . H11 H 0.2998 1.2125 -0.3381 0.096 Uiso 1 1 calc R . . C12 C 0.4092(8) 1.3832(7) -0.2969(5) 0.130(3) Uani 1 1 d . . . H12A H 0.4709 1.3727 -0.3249 0.195 Uiso 1 1 calc R . . H12B H 0.4465 1.4326 -0.2427 0.195 Uiso 1 1 calc R . . H12C H 0.3557 1.4171 -0.3312 0.195 Uiso 1 1 calc R . . N1 N 0.4145(5) 1.2153(4) -0.2241(3) 0.0653(14) Uani 1 1 d . . . O1 O 0.2833(5) 1.2674(4) -0.1539(3) 0.0934(15) Uani 1 1 d . . . P1 P 0.18431(12) 0.69589(10) 0.28097(8) 0.0354(3) Uani 1 1 d . . . Cl1 Cl 0.51022(13) 0.71844(12) 0.51331(9) 0.0583(4) Uani 1 1 d . . . Cl2 Cl 0.71751(13) 0.94823(13) 0.53180(10) 0.0711(5) Uani 1 1 d . . . Cl3 Cl 0.68179(14) 1.11546(12) 0.40550(11) 0.0721(5) Uani 1 1 d . . . Cl4 Cl 0.43264(14) 1.05932(11) 0.26659(9) 0.0615(4) Uani 1 1 d . . . Cl5 Cl 0.36497(15) 0.52737(12) 0.08350(10) 0.0708(5) Uani 1 1 d . . . Cl6 Cl 0.2378(2) 0.54837(15) -0.10117(11) 0.1029(7) Uani 1 1 d . . . Cl7 Cl 0.0100(2) 0.63999(13) -0.12936(9) 0.0943(7) Uani 1 1 d . . . Cl8 Cl -0.08229(16) 0.72265(12) 0.02757(10) 0.0754(5) Uani 1 1 d . . . Cl9 Cl -0.05780(14) 0.35176(10) 0.33483(9) 0.0573(4) Uani 1 1 d . . . Cl10 Cl -0.22331(15) 0.41449(12) 0.45213(11) 0.0704(5) Uani 1 1 d . . . Cl11 Cl -0.20514(15) 0.67087(13) 0.51286(10) 0.0671(4) Uani 1 1 d . . . Cl12 Cl -0.02127(14) 0.86448(10) 0.45900(9) 0.0556(4) Uani 1 1 d . . . O2 O 0.2961(3) 0.6944(2) 0.36568(18) 0.0376(8) Uani 1 1 d . . . O3 O 0.2661(3) 0.8278(2) 0.2690(2) 0.0388(8) Uani 1 1 d . . . O4 O 0.2505(3) 0.6238(2) 0.2164(2) 0.0407(9) Uani 1 1 d . . . O5 O 0.0754(3) 0.6997(3) 0.1937(2) 0.0416(9) Uani 1 1 d . . . O6 O 0.1029(3) 0.5669(2) 0.29564(19) 0.0365(8) Uani 1 1 d . . . O7 O 0.1145(3) 0.7667(2) 0.34331(19) 0.0365(8) Uani 1 1 d . . . C13 C 0.3915(5) 0.7894(4) 0.3821(3) 0.0341(12) Uani 1 1 d . . . C14 C 0.4952(5) 0.8139(4) 0.4463(3) 0.0420(13) Uani 1 1 d . . . C15 C 0.5850(5) 0.9152(4) 0.4534(3) 0.0437(14) Uani 1 1 d . . . C16 C 0.5695(5) 0.9908(4) 0.3978(3) 0.0460(14) Uani 1 1 d . . . C17 C 0.4617(5) 0.9665(4) 0.3343(3) 0.0410(13) Uani 1 1 d . . . C18 C 0.3743(4) 0.8648(4) 0.3267(3) 0.0343(12) Uani 1 1 d . . . C19 C 0.2010(5) 0.6217(4) 0.1334(3) 0.0403(13) Uani 1 1 d . . . C20 C 0.2435(5) 0.5822(4) 0.0662(4) 0.0492(15) Uani 1 1 d . . . C21 C 0.1816(7) 0.5894(4) -0.0162(4) 0.0587(18) Uani 1 1 d . . . C22 C 0.0831(7) 0.6319(4) -0.0279(3) 0.0597(19) Uani 1 1 d . . . C23 C 0.0403(5) 0.6702(4) 0.0400(3) 0.0491(15) Uani 1 1 d . . . C24 C 0.1028(5) 0.6647(4) 0.1212(3) 0.0382(13) Uani 1 1 d . . . C25 C 0.0284(4) 0.5797(4) 0.3459(3) 0.0331(12) Uani 1 1 d . . . C26 C -0.0505(5) 0.4925(4) 0.3691(3) 0.0389(13) Uani 1 1 d . . . C27 C -0.1225(5) 0.5209(4) 0.4230(3) 0.0407(13) Uani 1 1 d . . . C28 C -0.1147(5) 0.6344(4) 0.4505(3) 0.0408(13) Uani 1 1 d . . . C29 C -0.0331(4) 0.7220(4) 0.4263(3) 0.0338(12) Uani 1 1 d . . . C30 C 0.0355(4) 0.6935(4) 0.3738(3) 0.0305(12) Uani 1 1 d . . . C1S C 0.3100(8) 0.3149(7) 0.2245(6) 0.088(3) Uani 1 1 d . . . C2S C 0.2958(9) 0.3891(7) 0.2943(5) 0.123(3) Uani 1 1 d . . . H2S1 H 0.3741 0.4290 0.3310 0.184 Uiso 1 1 calc R . . H2S2 H 0.2474 0.3444 0.3257 0.184 Uiso 1 1 calc R . . H2S3 H 0.2565 0.4436 0.2729 0.184 Uiso 1 1 calc R . . N1S N 0.3235(8) 0.2585(7) 0.1706(6) 0.125(3) Uani 1 1 d . . . 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 S1 0.0482(10) 0.0510(8) 0.0537(9) 0.0124(6) 0.0179(7) 0.0158(7) S2 0.0674(12) 0.0641(9) 0.0540(10) 0.0164(7) 0.0256(8) 0.0274(8) S3 0.0536(10) 0.0533(8) 0.0506(9) 0.0164(6) 0.0153(8) 0.0177(7) S4 0.0727(12) 0.0652(10) 0.0475(9) 0.0142(7) 0.0205(8) 0.0253(8) S5 0.0790(14) 0.1101(14) 0.0782(13) 0.0372(10) 0.0240(11) 0.0564(11) S6 0.1236(19) 0.1037(14) 0.0534(11) 0.0245(9) 0.0128(11) 0.0632(13) C1 0.048(4) 0.044(3) 0.055(4) 0.006(3) 0.015(3) 0.012(3) C2 0.046(4) 0.049(3) 0.062(4) 0.013(3) 0.014(3) 0.018(3) C3 0.053(4) 0.035(3) 0.052(4) 0.007(2) 0.020(3) 0.009(3) C4 0.050(4) 0.033(3) 0.054(4) 0.012(2) 0.019(3) 0.015(3) C5 0.053(4) 0.045(3) 0.064(4) 0.015(3) 0.012(3) 0.024(3) C6 0.071(5) 0.047(3) 0.051(4) 0.015(3) 0.015(3) 0.024(3) C7 0.146(9) 0.140(7) 0.077(6) 0.023(5) -0.007(6) 0.099(7) C8 0.128(9) 0.229(11) 0.090(7) 0.069(7) -0.010(7) 0.057(8) C9 0.034(4) 0.057(4) 0.062(5) 0.002(3) 0.006(3) 0.022(3) C10 0.122(8) 0.130(6) 0.057(5) 0.015(4) -0.010(5) 0.072(6) C11 0.070(5) 0.115(6) 0.050(4) 0.008(4) 0.005(4) 0.031(5) C12 0.134(8) 0.154(8) 0.091(6) 0.057(6) 0.004(6) 0.022(6) N1 0.078(4) 0.081(4) 0.049(3) 0.006(3) 0.026(3) 0.037(3) O1 0.086(4) 0.144(4) 0.063(3) 0.014(3) 0.014(3) 0.062(3) P1 0.0326(8) 0.0357(7) 0.0358(8) 0.0098(5) 0.0086(6) 0.0043(6) Cl1 0.0459(10) 0.0783(10) 0.0528(9) 0.0210(7) 0.0062(7) 0.0218(7) Cl2 0.0370(9) 0.0818(11) 0.0745(11) -0.0129(8) -0.0028(8) 0.0073(8) Cl3 0.0519(10) 0.0517(9) 0.0982(13) -0.0070(8) 0.0319(9) -0.0134(7) Cl4 0.0728(11) 0.0474(8) 0.0679(10) 0.0219(7) 0.0323(8) 0.0053(7) Cl5 0.0733(12) 0.0651(10) 0.0762(11) 0.0009(8) 0.0367(9) 0.0135(8) Cl6 0.168(2) 0.0814(12) 0.0560(11) -0.0017(8) 0.0580(12) 0.0099(12) Cl7 0.1468(18) 0.0654(10) 0.0353(9) 0.0097(7) -0.0098(10) -0.0076(10) Cl8 0.0690(12) 0.0665(10) 0.0716(11) 0.0181(8) -0.0187(9) 0.0119(8) Cl9 0.0675(11) 0.0344(7) 0.0654(10) 0.0107(6) 0.0172(8) 0.0044(7) Cl10 0.0632(11) 0.0654(10) 0.0873(12) 0.0363(8) 0.0375(9) 0.0002(8) Cl11 0.0624(11) 0.0856(11) 0.0687(11) 0.0235(8) 0.0400(9) 0.0245(8) Cl12 0.0664(11) 0.0430(8) 0.0583(9) 0.0001(6) 0.0238(8) 0.0141(7) O2 0.037(2) 0.0370(18) 0.0329(19) 0.0086(14) 0.0052(16) 0.0016(16) O3 0.031(2) 0.0383(18) 0.044(2) 0.0165(14) 0.0061(17) 0.0009(15) O4 0.040(2) 0.047(2) 0.035(2) 0.0075(15) 0.0107(17) 0.0107(16) O5 0.033(2) 0.049(2) 0.039(2) 0.0105(15) 0.0030(17) 0.0091(16) O6 0.036(2) 0.0335(18) 0.039(2) 0.0063(14) 0.0142(17) 0.0049(15) O7 0.036(2) 0.0285(17) 0.043(2) 0.0055(14) 0.0157(16) 0.0016(15) C13 0.035(3) 0.033(3) 0.034(3) 0.004(2) 0.014(3) 0.006(2) C14 0.040(4) 0.047(3) 0.037(3) 0.002(2) 0.012(3) 0.009(3) C15 0.030(3) 0.050(3) 0.044(3) -0.012(3) 0.012(3) 0.007(3) C16 0.037(4) 0.044(3) 0.055(4) -0.008(3) 0.028(3) 0.001(3) C17 0.045(4) 0.033(3) 0.046(3) 0.003(2) 0.023(3) 0.005(2) C18 0.032(3) 0.033(3) 0.040(3) 0.004(2) 0.015(3) 0.008(2) C19 0.040(4) 0.036(3) 0.039(4) 0.006(2) 0.012(3) -0.002(3) C20 0.065(4) 0.032(3) 0.050(4) 0.006(2) 0.023(3) 0.004(3) C21 0.088(5) 0.035(3) 0.041(4) -0.004(2) 0.029(4) -0.010(3) C22 0.087(5) 0.036(3) 0.034(4) 0.005(2) 0.002(4) -0.010(3) C23 0.060(4) 0.034(3) 0.039(4) 0.007(2) 0.003(3) -0.005(3) C24 0.042(4) 0.032(3) 0.034(3) 0.005(2) 0.010(3) -0.001(2) C25 0.028(3) 0.034(3) 0.033(3) 0.006(2) 0.003(2) 0.004(2) C26 0.039(3) 0.031(3) 0.040(3) 0.008(2) 0.002(3) 0.003(2) C27 0.035(3) 0.045(3) 0.041(3) 0.021(2) 0.009(3) 0.004(2) C28 0.036(3) 0.052(3) 0.034(3) 0.012(2) 0.008(2) 0.010(3) C29 0.028(3) 0.035(3) 0.034(3) 0.004(2) 0.002(2) 0.008(2) C30 0.027(3) 0.034(3) 0.025(3) 0.007(2) 0.002(2) 0.003(2) C1S 0.097(6) 0.109(6) 0.109(7) 0.063(5) 0.070(6) 0.065(5) C2S 0.185(10) 0.144(7) 0.101(7) 0.057(6) 0.083(7) 0.102(7) N1S 0.147(7) 0.147(7) 0.139(7) 0.058(5) 0.082(6) 0.092(6) _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 S1 C3 1.732(5) . ? S1 C1 1.739(6) . ? S2 C2 1.711(6) . ? S2 C3 1.739(6) . ? S3 C4 1.711(6) . ? S3 C5 1.753(6) . ? S4 C4 1.717(5) . ? S4 C6 1.737(6) . ? S5 C5 1.719(6) . ? S5 C7 1.791(7) . ? S6 C6 1.730(6) . ? S6 C8 1.760(11) . ? C1 C2 1.336(7) . ? C1 C9 1.473(8) . ? C2 H2 0.9300 . ? C3 C4 1.383(7) . ? C5 C6 1.367(8) . ? C7 C8 1.417(11) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 N1 1.246(7) . ? C9 O1 1.352(7) . ? C10 O1 1.460(7) . ? C10 C11 1.497(10) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N1 1.490(8) . ? C11 C12 1.554(10) . ? C11 H11 0.9800 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? P1 O2 1.704(3) . ? P1 O6 1.705(3) . ? P1 O7 1.718(3) . ? P1 O4 1.719(4) . ? P1 O3 1.720(3) . ? P1 O5 1.721(3) . ? Cl1 C14 1.711(5) . ? Cl2 C15 1.722(5) . ? Cl3 C16 1.724(5) . ? Cl4 C17 1.724(5) . ? Cl5 C20 1.708(6) . ? Cl6 C21 1.731(6) . ? Cl7 C22 1.730(6) . ? Cl8 C23 1.701(6) . ? Cl9 C26 1.723(5) . ? Cl10 C27 1.716(5) . ? Cl11 C28 1.716(6) . ? Cl12 C29 1.725(5) . ? O2 C13 1.355(5) . ? O3 C18 1.351(5) . ? O4 C19 1.355(6) . ? O5 C24 1.340(6) . ? O6 C25 1.342(6) . ? O7 C30 1.342(5) . ? C13 C14 1.375(6) . ? C13 C18 1.389(6) . ? C14 C15 1.391(7) . ? C15 C16 1.390(7) . ? C16 C17 1.401(7) . ? C17 C18 1.377(6) . ? C19 C24 1.370(7) . ? C19 C20 1.383(7) . ? C20 C21 1.416(8) . ? C21 C22 1.369(9) . ? C22 C23 1.388(8) . ? C23 C24 1.396(7) . ? C25 C26 1.378(6) . ? C25 C30 1.390(6) . ? C26 C27 1.412(7) . ? C27 C28 1.384(6) . ? C28 C29 1.407(7) . ? C29 C30 1.365(7) . ? C1S N1S 1.117(9) . ? C1S C2S 1.436(11) . ? C2S H2S1 0.9600 . ? C2S H2S2 0.9600 . ? C2S H2S3 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 C3 S1 C1 94.7(3) . . ? C2 S2 C3 94.8(3) . . ? C4 S3 C5 96.2(3) . . ? C4 S4 C6 96.0(3) . . ? C5 S5 C7 100.2(4) . . ? C6 S6 C8 102.4(4) . . ? C2 C1 C9 126.9(6) . . ? C2 C1 S1 116.8(4) . . ? C9 C1 S1 116.4(5) . . ? C1 C2 S2 118.3(5) . . ? C1 C2 H2 120.8 . . ? S2 C2 H2 120.8 . . ? C4 C3 S1 123.9(4) . . ? C4 C3 S2 120.7(4) . . ? S1 C3 S2 115.3(3) . . ? C3 C4 S3 123.5(4) . . ? C3 C4 S4 121.0(4) . . ? S3 C4 S4 115.5(3) . . ? C6 C5 S5 127.5(5) . . ? C6 C5 S3 115.4(4) . . ? S5 C5 S3 117.0(4) . . ? C5 C6 S6 128.6(5) . . ? C5 C6 S4 116.7(4) . . ? S6 C6 S4 114.7(4) . . ? C8 C7 S5 117.4(6) . . ? C8 C7 H7A 108.0 . . ? S5 C7 H7A 108.0 . . ? C8 C7 H7B 108.0 . . ? S5 C7 H7B 108.0 . . ? H7A C7 H7B 107.2 . . ? C7 C8 S6 120.4(7) . . ? C7 C8 H8A 107.2 . . ? S6 C8 H8A 107.2 . . ? C7 C8 H8B 107.2 . . ? S6 C8 H8B 107.2 . . ? H8A C8 H8B 106.9 . . ? N1 C9 O1 121.7(6) . . ? N1 C9 C1 124.1(6) . . ? O1 C9 C1 114.2(6) . . ? O1 C10 C11 103.9(6) . . ? O1 C10 H10A 111.0 . . ? C11 C10 H10A 111.0 . . ? O1 C10 H10B 111.0 . . ? C11 C10 H10B 111.0 . . ? H10A C10 H10B 109.0 . . ? N1 C11 C10 105.7(6) . . ? N1 C11 C12 110.6(6) . . ? C10 C11 C12 108.6(7) . . ? N1 C11 H11 110.6 . . ? C10 C11 H11 110.6 . . ? C12 C11 H11 110.6 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 N1 C11 103.5(5) . . ? C9 O1 C10 103.7(6) . . ? O2 P1 O6 88.29(15) . . ? O2 P1 O7 92.90(16) . . ? O6 P1 O7 90.90(16) . . ? O2 P1 O4 88.59(17) . . ? O6 P1 O4 88.61(16) . . ? O7 P1 O4 178.41(17) . . ? O2 P1 O3 91.01(15) . . ? O6 P1 O3 178.35(18) . . ? O7 P1 O3 87.64(16) . . ? O4 P1 O3 92.87(16) . . ? O2 P1 O5 177.90(18) . . ? O6 P1 O5 93.40(15) . . ? O7 P1 O5 88.32(17) . . ? O4 P1 O5 90.20(17) . . ? O3 P1 O5 87.33(15) . . ? C13 O2 P1 111.8(3) . . ? C18 O3 P1 111.3(3) . . ? C19 O4 P1 110.8(3) . . ? C24 O5 P1 111.2(3) . . ? C25 O6 P1 111.5(3) . . ? C30 O7 P1 111.6(3) . . ? O2 C13 C14 125.9(4) . . ? O2 C13 C18 112.7(4) . . ? C14 C13 C18 121.4(4) . . ? C13 C14 C15 118.3(4) . . ? C13 C14 Cl1 119.2(4) . . ? C15 C14 Cl1 122.5(4) . . ? C16 C15 C14 120.9(5) . . ? C16 C15 Cl2 119.2(4) . . ? C14 C15 Cl2 119.9(4) . . ? C15 C16 C17 120.2(4) . . ? C15 C16 Cl3 120.9(4) . . ? C17 C16 Cl3 118.9(4) . . ? C18 C17 C16 118.5(4) . . ? C18 C17 Cl4 118.7(4) . . ? C16 C17 Cl4 122.8(4) . . ? O3 C18 C17 126.1(4) . . ? O3 C18 C13 113.1(4) . . ? C17 C18 C13 120.7(5) . . ? O4 C19 C24 113.2(5) . . ? O4 C19 C20 125.0(5) . . ? C24 C19 C20 121.8(5) . . ? C19 C20 C21 116.9(6) . . ? C19 C20 Cl5 120.6(5) . . ? C21 C20 Cl5 122.5(5) . . ? C22 C21 C20 120.9(6) . . ? C22 C21 Cl6 121.1(5) . . ? C20 C21 Cl6 118.0(6) . . ? C21 C22 C23 121.8(5) . . ? C21 C22 Cl7 119.7(6) . . ? C23 C22 Cl7 118.5(6) . . ? C22 C23 C24 117.1(6) . . ? C22 C23 Cl8 122.9(5) . . ? C24 C23 Cl8 120.0(5) . . ? O5 C24 C19 113.5(4) . . ? O5 C24 C23 125.1(5) . . ? C19 C24 C23 121.5(5) . . ? O6 C25 C26 126.0(4) . . ? O6 C25 C30 113.5(4) . . ? C26 C25 C30 120.6(5) . . ? C25 C26 C27 118.8(4) . . ? C25 C26 Cl9 120.2(4) . . ? C27 C26 Cl9 121.0(4) . . ? C28 C27 C26 120.2(4) . . ? C28 C27 Cl10 119.7(4) . . ? C26 C27 Cl10 120.1(4) . . ? C27 C28 C29 120.1(5) . . ? C27 C28 Cl11 121.0(4) . . ? C29 C28 Cl11 118.9(4) . . ? C30 C29 C28 119.2(4) . . ? C30 C29 Cl12 119.4(4) . . ? C28 C29 Cl12 121.4(4) . . ? O7 C30 C29 126.3(4) . . ? O7 C30 C25 112.6(5) . . ? C29 C30 C25 121.1(4) . . ? N1S C1S C2S 178.5(11) . . ? C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.525 _refine_diff_density_min -0.364 _refine_diff_density_rms 0.076 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 820754' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(S,S,S,S)-TMBEDT-TTF TRISPHAT' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H22 Cl12 N2 O6 P S8' _chemical_formula_weight 1291.41 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' 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 11.5872(8) _cell_length_b 14.1039(17) _cell_length_c 17.104(2) _cell_angle_alpha 76.726(8) _cell_angle_beta 89.191(7) _cell_angle_gamma 67.221(7) _cell_volume 2499.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 21796 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.716 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1294 _exptl_absorpt_coefficient_mu 1.077 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.806804 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _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 49157 _diffrn_reflns_av_R_equivalents 0.0419 _diffrn_reflns_av_sigmaI/netI 0.0857 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 27.50 _reflns_number_total 21780 _reflns_number_gt 12001 _reflns_threshold_expression >2sigma(I) _computing_data_collection KappaCCD _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'Denzo and Scalepak' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0318P)^2^+1.0694P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _chemical_absolute_configuration syn _refine_ls_abs_structure_Flack 0.12(8) _refine_ls_number_reflns 21780 _refine_ls_number_parameters 1175 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1296 _refine_ls_R_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.1034 _refine_ls_wR_factor_gt 0.0827 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.002 _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 S1A S 0.6252(3) 0.4711(2) 0.45635(16) 0.0521(7) Uani 1 1 d . . . S2A S 0.5046(3) 0.3974(2) 0.30450(15) 0.0532(8) Uani 1 1 d . . . S3A S 0.5101(2) 0.3439(2) 0.56422(15) 0.0436(6) Uani 1 1 d . . . S4A S 0.4082(2) 0.2856(2) 0.43632(15) 0.0464(7) Uani 1 1 d . . . S5A S 0.3829(2) 0.2198(2) 0.69474(15) 0.0425(6) Uani 1 1 d . . . S6A S 0.2798(2) 0.1627(2) 0.56727(15) 0.0438(7) Uani 1 1 d . . . S7A S 0.2683(3) 0.1242(3) 0.82515(18) 0.0785(10) Uani 1 1 d . . . S8A S 0.1440(3) 0.0529(2) 0.67427(17) 0.0616(8) Uani 1 1 d . . . C5A C 0.5353(8) 0.3938(8) 0.4644(6) 0.040(2) Uani 1 1 d . . . C6A C 0.4918(8) 0.3648(7) 0.4056(6) 0.041(2) Uani 1 1 d . . . C7A C 0.4272(8) 0.2780(7) 0.5371(5) 0.036(2) Uani 1 1 d . . . C8A C 0.3706(8) 0.2254(8) 0.5923(5) 0.042(3) Uani 1 1 d . . . C9A C 0.2903(9) 0.1483(7) 0.7225(5) 0.040(2) Uani 1 1 d . . . C10A C 0.2440(8) 0.1220(7) 0.6621(6) 0.038(2) Uani 1 1 d . . . C1A C 0.5931(7) 0.5379(5) 0.3485(4) 0.0510(18) Uani 1 1 d . . . H1A H 0.5056 0.5891 0.3379 0.061 Uiso 1 1 calc R . . C2A C 0.6170(6) 0.4597(5) 0.2966(4) 0.0444(15) Uani 1 1 d . . . H2A H 0.7010 0.4039 0.3133 0.053 Uiso 1 1 calc R . . C3A C 0.6807(12) 0.5969(10) 0.3318(7) 0.080(3) Uani 1 1 d . . . H3A1 H 0.6633 0.6460 0.3654 0.119 Uiso 1 1 calc R . . H3A2 H 0.6673 0.6349 0.2762 0.119 Uiso 1 1 calc R . . H3A3 H 0.7664 0.5469 0.3434 0.119 Uiso 1 1 calc R . . C4A C 0.6106(11) 0.5084(9) 0.2061(6) 0.076(3) Uani 1 1 d . . . H4A1 H 0.6269 0.4544 0.1771 0.115 Uiso 1 1 calc R . . H4A2 H 0.6724 0.5386 0.1960 0.115 Uiso 1 1 calc R . . H4A3 H 0.5285 0.5629 0.1884 0.115 Uiso 1 1 calc R . . C11A C 0.1779(6) 0.0426(6) 0.8377(4) 0.0554(17) Uani 1 1 d . . . H11A H 0.2353 -0.0315 0.8438 0.066 Uiso 1 1 calc R . . C12A C 0.0804(8) 0.0735(7) 0.7692(6) 0.059(2) Uani 1 1 d . . . H12A H 0.0241 0.1482 0.7620 0.071 Uiso 1 1 calc R . . C13A C 0.1213(10) 0.0563(10) 0.9201(7) 0.096(4) Uani 1 1 d . . . H13A H 0.1880 0.0353 0.9611 0.144 Uiso 1 1 calc R . . H13B H 0.0741 0.0128 0.9345 0.144 Uiso 1 1 calc R . . H13C H 0.0669 0.1292 0.9151 0.144 Uiso 1 1 calc R . . C14A C 0.0009(10) 0.0035(10) 0.7854(7) 0.076(4) Uani 1 1 d . . . H14A H -0.0605 0.0251 0.7408 0.114 Uiso 1 1 calc R . . H14B H -0.0409 0.0122 0.8338 0.114 Uiso 1 1 calc R . . H14C H 0.0555 -0.0697 0.7917 0.114 Uiso 1 1 calc R . . P1A P 1.2879(2) 0.4816(2) 0.81056(16) 0.0416(7) Uani 1 1 d . . . O1A O 1.4256(6) 0.3785(5) 0.8022(4) 0.0403(16) Uani 1 1 d . . . O2A O 1.2535(6) 0.4004(5) 0.8902(4) 0.0414(16) Uani 1 1 d . . . O3A O 1.3218(6) 0.5587(5) 0.7287(4) 0.0463(18) Uani 1 1 d . . . O4A O 1.1999(6) 0.4491(5) 0.7491(4) 0.0465(18) Uani 1 1 d . . . O5A O 1.3733(5) 0.5156(5) 0.8709(4) 0.0412(17) Uani 1 1 d . . . O6A O 1.1517(6) 0.5832(5) 0.8246(4) 0.0435(17) Uani 1 1 d . . . Cl1 Cl 1.2229(3) 0.2403(2) 1.03267(17) 0.0669(8) Uani 1 1 d . . . Cl2 Cl 1.4626(3) 0.0247(2) 1.07134(19) 0.0865(11) Uani 1 1 d . . . Cl3 Cl 1.6912(3) -0.0002(2) 0.9653(2) 0.0833(11) Uani 1 1 d . . . Cl4 Cl 1.6728(3) 0.1885(3) 0.81815(19) 0.0712(9) Uani 1 1 d . . . Cl5 Cl 1.0525(3) 0.4097(2) 0.6247(2) 0.0672(9) Uani 1 1 d . . . Cl6 Cl 1.0836(3) 0.5197(3) 0.44716(19) 0.0828(10) Uani 1 1 d . . . Cl7 Cl 1.2467(3) 0.6547(3) 0.41973(17) 0.0757(10) Uani 1 1 d . . . Cl8 Cl 1.3725(3) 0.6841(2) 0.57004(17) 0.0673(8) Uani 1 1 d . . . Cl9 Cl 0.9274(2) 0.7532(2) 0.87396(19) 0.0682(9) Uani 1 1 d . . . Cl10 Cl 1.0075(3) 0.8368(2) 1.01086(19) 0.0683(8) Uani 1 1 d . . . Cl11 Cl 1.2929(3) 0.7579(3) 1.06545(18) 0.0756(9) Uani 1 1 d . . . Cl12 Cl 1.4933(2) 0.5786(2) 0.99705(15) 0.0524(7) Uani 1 1 d . . . C15A C 1.4464(8) 0.2912(8) 0.8631(6) 0.041(2) Uani 1 1 d . . . C16A C 1.3486(8) 0.3029(8) 0.9131(6) 0.039(2) Uani 1 1 d . . . C17A C 1.3486(9) 0.2239(8) 0.9763(6) 0.045(3) Uani 1 1 d . . . C18A C 1.4588(10) 0.1264(8) 0.9905(6) 0.057(3) Uani 1 1 d . . . C19A C 1.5583(9) 0.1161(9) 0.9426(7) 0.053(3) Uani 1 1 d . . . C20A C 1.5521(8) 0.1988(8) 0.8780(6) 0.044(3) Uani 1 1 d . . . C21A C 1.2721(9) 0.5566(8) 0.6597(6) 0.044(3) Uani 1 1 d . . . C22A C 1.2070(9) 0.4958(8) 0.6700(5) 0.042(3) Uani 1 1 d . . . C23A C 1.1428(9) 0.4825(7) 0.6066(7) 0.051(3) Uani 1 1 d . . . C24A C 1.1586(11) 0.5359(9) 0.5269(6) 0.058(3) Uani 1 1 d . . . C25A C 1.2303(9) 0.5930(9) 0.5169(6) 0.053(3) Uani 1 1 d . . . C26A C 1.2862(9) 0.6050(8) 0.5826(6) 0.049(3) Uani 1 1 d . . . C27A C 1.2978(9) 0.5899(7) 0.9057(6) 0.035(2) Uani 1 1 d . . . C28A C 1.1718(9) 0.6321(8) 0.8803(5) 0.039(2) Uani 1 1 d . . . C29A C 1.0845(8) 0.7079(7) 0.9099(6) 0.040(2) Uani 1 1 d . . . C30A C 1.1178(10) 0.7444(8) 0.9686(6) 0.044(2) Uani 1 1 d . . . C31A C 1.2446(9) 0.7094(7) 0.9944(6) 0.044(3) Uani 1 1 d . . . C32A C 1.3354(9) 0.6295(8) 0.9647(5) 0.044(3) Uani 1 1 d . . . S1B S 0.9648(3) 0.2891(3) 0.41877(17) 0.0624(9) Uani 1 1 d . . . S2B S 0.8563(3) 0.2105(2) 0.26640(16) 0.0578(8) Uani 1 1 d . . . S3B S 0.8318(2) 0.1775(2) 0.52305(15) 0.0455(7) Uani 1 1 d . . . S4B S 0.7334(2) 0.1165(2) 0.39536(15) 0.0412(6) Uani 1 1 d . . . S5B S 0.7036(2) 0.0577(2) 0.65302(15) 0.0480(7) Uani 1 1 d . . . S6B S 0.6012(2) -0.0042(2) 0.52779(15) 0.0449(7) Uani 1 1 d . . . S7B S 0.6195(3) -0.0596(3) 0.78800(16) 0.0597(8) Uani 1 1 d . . . S8B S 0.4951(3) -0.1357(2) 0.63867(17) 0.0591(8) Uani 1 1 d . . . C5B C 0.8729(8) 0.2171(8) 0.4248(5) 0.045(3) Uani 1 1 d . . . C6B C 0.8264(8) 0.1872(8) 0.3664(6) 0.044(3) Uani 1 1 d . . . C7B C 0.7432(8) 0.1156(7) 0.4941(5) 0.035(2) Uani 1 1 d . . . C8B C 0.6881(8) 0.0644(8) 0.5513(5) 0.042(2) Uani 1 1 d . . . C9B C 0.6280(8) -0.0277(8) 0.6835(5) 0.042(3) Uani 1 1 d . . . C10B C 0.5766(9) -0.0558(8) 0.6252(6) 0.043(3) Uani 1 1 d . . . C1B C 1.0029(8) 0.3075(7) 0.3137(5) 0.057(2) Uani 1 1 d . . . H1B H 0.9398 0.3746 0.2823 0.068 Uiso 1 1 calc R . . C2B C 1.0086(6) 0.2200(6) 0.2746(4) 0.0543(16) Uani 1 1 d . . . H2B H 1.0696 0.1523 0.3067 0.065 Uiso 1 1 calc R . . C3B C 1.1273(11) 0.3189(11) 0.3171(8) 0.084(4) Uani 1 1 d . . . H3B1 H 1.1190 0.3750 0.3424 0.126 Uiso 1 1 calc R . . H3B2 H 1.1515 0.3352 0.2633 0.126 Uiso 1 1 calc R . . H3B3 H 1.1903 0.2536 0.3476 0.126 Uiso 1 1 calc R . . C4B C 1.0479(11) 0.2383(10) 0.1900(6) 0.098(4) Uani 1 1 d . . . H4B1 H 1.0502 0.1818 0.1668 0.148 Uiso 1 1 calc R . . H4B2 H 1.1298 0.2402 0.1911 0.148 Uiso 1 1 calc R . . H4B3 H 0.9887 0.3046 0.1581 0.148 Uiso 1 1 calc R . . C11B C 0.5783(7) -0.1711(6) 0.8011(4) 0.067(2) Uani 1 1 d . . . H11B H 0.6502 -0.2311 0.7906 0.081 Uiso 1 1 calc R . . C12B C 0.4643(7) -0.1503(6) 0.7456(4) 0.0572(19) Uani 1 1 d . . . H12B H 0.3955 -0.0854 0.7517 0.069 Uiso 1 1 calc R . . C13B C 0.5540(12) -0.1969(10) 0.8891(6) 0.094(4) Uani 1 1 d . . . H13D H 0.6272 -0.2093 0.9222 0.142 Uiso 1 1 calc R . . H13E H 0.5357 -0.2593 0.9009 0.142 Uiso 1 1 calc R . . H13F H 0.4839 -0.1385 0.8999 0.142 Uiso 1 1 calc R . . C14B C 0.4181(13) -0.2405(10) 0.7613(7) 0.096(4) Uani 1 1 d . . . H14D H 0.3471 -0.2218 0.7241 0.144 Uiso 1 1 calc R . . H14E H 0.3940 -0.2521 0.8155 0.144 Uiso 1 1 calc R . . H14F H 0.4842 -0.3041 0.7542 0.144 Uiso 1 1 calc R . . P1B P 0.8330(2) 0.8526(2) 0.28299(16) 0.0390(6) Uani 1 1 d . . . O1B O 0.8684(5) 0.9312(5) 0.2010(4) 0.0427(17) Uani 1 1 d . . . O2B O 0.6958(6) 0.9581(5) 0.2884(4) 0.0446(17) Uani 1 1 d . . . O3B O 0.7469(5) 0.8162(5) 0.2233(3) 0.0389(16) Uani 1 1 d . . . O4B O 0.9662(5) 0.7498(5) 0.2748(3) 0.0387(16) Uani 1 1 d . . . O5B O 0.9193(6) 0.8868(5) 0.3436(4) 0.0427(17) Uani 1 1 d . . . O6B O 0.7955(6) 0.7780(5) 0.3664(4) 0.0429(17) Uani 1 1 d . . . Cl13 Cl 0.4485(2) 1.1497(2) 0.27098(17) 0.0597(8) Uani 1 1 d . . . Cl14 Cl 0.4376(3) 1.3368(2) 0.12243(18) 0.0647(8) Uani 1 1 d . . . Cl15 Cl 0.6659(3) 1.3064(2) 0.01888(18) 0.0738(9) Uani 1 1 d . . . Cl16 Cl 0.9013(3) 1.0907(2) 0.05924(17) 0.0621(8) Uani 1 1 d . . . Cl17 Cl 1.1939(2) 0.5777(2) 0.22542(18) 0.0585(8) Uani 1 1 d . . . Cl18 Cl 1.1128(3) 0.4881(2) 0.09178(19) 0.0697(9) Uani 1 1 d . . . Cl19 Cl 0.8284(3) 0.5681(3) 0.03477(18) 0.0703(8) Uani 1 1 d . . . Cl20 Cl 0.6284(2) 0.7507(2) 0.10142(15) 0.0521(7) Uani 1 1 d . . . Cl21 Cl 0.7468(3) 0.6575(3) 0.52773(17) 0.0684(8) Uani 1 1 d . . . Cl22 Cl 0.8762(3) 0.6892(3) 0.67424(17) 0.0816(10) Uani 1 1 d . . . Cl23 Cl 1.0335(3) 0.8275(3) 0.64426(19) 0.0851(11) Uani 1 1 d . . . Cl24 Cl 1.0660(3) 0.9332(2) 0.4657(2) 0.0660(9) Uani 1 1 d . . . C15B C 0.7774(8) 1.0276(7) 0.1793(6) 0.037(2) Uani 1 1 d . . . C16B C 0.6780(9) 1.0430(7) 0.2273(6) 0.038(2) Uani 1 1 d . . . C17B C 0.5728(9) 1.1379(8) 0.2110(6) 0.043(3) Uani 1 1 d . . . C18B C 0.5701(9) 1.2174(7) 0.1446(6) 0.045(3) Uani 1 1 d . . . C19B C 0.6699(9) 1.2043(8) 0.0977(5) 0.041(2) Uani 1 1 d . . . C20B C 0.7712(9) 1.1102(8) 0.1154(6) 0.042(3) Uani 1 1 d . . . C21B C 0.8229(9) 0.7380(7) 0.1892(6) 0.037(2) Uani 1 1 d . . . C22B C 0.9483(8) 0.7034(6) 0.2189(5) 0.037(2) Uani 1 1 d . . . C23B C 1.0405(8) 0.6250(7) 0.1894(6) 0.041(2) Uani 1 1 d . . . C24B C 0.9992(9) 0.5824(8) 0.1318(6) 0.047(3) Uani 1 1 d . . . C25B C 0.8746(10) 0.6219(8) 0.1046(6) 0.046(3) Uani 1 1 d . . . C26B C 0.7829(8) 0.7021(7) 0.1332(6) 0.034(2) Uani 1 1 d . . . C27B C 0.9202(8) 0.8450(7) 0.4220(6) 0.041(2) Uani 1 1 d . . . C28B C 0.8469(8) 0.7829(7) 0.4367(6) 0.039(2) Uani 1 1 d . . . C29B C 0.8337(9) 0.7318(8) 0.5123(6) 0.045(3) Uani 1 1 d . . . C30B C 0.8948(10) 0.7464(9) 0.5780(5) 0.054(3) Uani 1 1 d . . . C31B C 0.9625(9) 0.8108(8) 0.5625(6) 0.048(3) Uani 1 1 d . . . C32B C 0.9775(9) 0.8575(8) 0.4858(6) 0.048(3) Uani 1 1 d . . . C33A C 0.1509(12) 0.9058(15) 0.2257(10) 0.139(6) Uani 1 1 d . . . H33A H 0.1285 0.9386 0.2702 0.208 Uiso 1 1 calc R . . H33B H 0.0981 0.8687 0.2211 0.208 Uiso 1 1 calc R . . H33C H 0.1397 0.9593 0.1769 0.208 Uiso 1 1 calc R . . C34A C 0.2765(11) 0.8342(13) 0.2390(8) 0.091(5) Uani 1 1 d . . . N1A N 0.3772(13) 0.7877(16) 0.2438(11) 0.209(9) Uani 1 1 d . . . C33B C 0.4712(12) 0.8715(11) 0.3888(9) 0.101(5) Uani 1 1 d . . . H33D H 0.4750 0.8088 0.4274 0.151 Uiso 1 1 calc R . . H33E H 0.5478 0.8813 0.3950 0.151 Uiso 1 1 calc R . . H33F H 0.4606 0.8640 0.3353 0.151 Uiso 1 1 calc R . . C34B C 0.3674(12) 0.9613(12) 0.4018(8) 0.081(4) Uani 1 1 d . . . N1B N 0.2796(12) 1.0316(12) 0.4039(9) 0.140(5) Uani 1 1 d . . . C33C C 0.6458(13) 0.4706(12) 0.6958(9) 0.104(5) Uani 1 1 d . . . H33G H 0.5866 0.4971 0.6493 0.157 Uiso 1 1 calc R . . H33H H 0.6720 0.5252 0.7025 0.157 Uiso 1 1 calc R . . H33I H 0.6071 0.4493 0.7428 0.157 Uiso 1 1 calc R . . C34C C 0.7531(14) 0.3811(12) 0.6849(9) 0.088(4) Uani 1 1 d . . . N1C N 0.8292(12) 0.3108(11) 0.6717(8) 0.127(5) Uani 1 1 d . . . C33D C 0.9638(13) 0.4123(16) 0.8688(12) 0.198(10) Uani 1 1 d . . . H33J H 1.0145 0.4294 0.8275 0.297 Uiso 1 1 calc R . . H33K H 0.9591 0.3463 0.8673 0.297 Uiso 1 1 calc R . . H33L H 1.0009 0.4062 0.9205 0.297 Uiso 1 1 calc R . . C34D C 0.8456(14) 0.4907(12) 0.8559(9) 0.109(6) Uani 1 1 d . . . N1D N 0.7520(14) 0.5619(9) 0.8384(9) 0.131(5) Uani 1 1 d . . . 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 S1A 0.071(2) 0.0593(18) 0.0420(15) -0.0170(13) 0.0072(14) -0.0400(16) S2A 0.0622(17) 0.074(2) 0.0303(14) -0.0111(13) 0.0007(12) -0.0356(15) S3A 0.0534(15) 0.0500(15) 0.0368(14) -0.0195(12) 0.0063(11) -0.0253(12) S4A 0.0467(15) 0.0604(16) 0.0386(14) -0.0160(12) 0.0012(11) -0.0255(13) S5A 0.0508(15) 0.0493(16) 0.0398(14) -0.0192(12) 0.0066(11) -0.0282(13) S6A 0.0458(14) 0.0523(16) 0.0401(14) -0.0174(12) -0.0007(11) -0.0231(12) S7A 0.111(3) 0.128(3) 0.0450(17) -0.0324(18) 0.0197(16) -0.093(2) S8A 0.0677(18) 0.083(2) 0.0587(18) -0.0223(16) 0.0063(14) -0.0530(16) C5A 0.041(5) 0.044(6) 0.033(5) -0.003(4) 0.009(4) -0.019(4) C6A 0.041(5) 0.040(6) 0.046(6) -0.016(5) 0.000(5) -0.017(5) C7A 0.042(5) 0.028(4) 0.036(5) -0.001(4) 0.008(4) -0.015(4) C8A 0.036(5) 0.047(6) 0.037(5) -0.021(4) -0.003(4) -0.004(4) C9A 0.057(6) 0.045(6) 0.028(5) -0.009(4) 0.012(4) -0.030(5) C10A 0.033(5) 0.043(6) 0.051(5) -0.018(4) -0.003(4) -0.025(4) C1A 0.067(5) 0.039(4) 0.046(4) -0.008(3) 0.005(4) -0.022(3) C2A 0.049(4) 0.047(4) 0.037(3) -0.009(3) 0.002(3) -0.020(3) C3A 0.120(8) 0.074(7) 0.069(7) -0.014(5) 0.023(6) -0.067(6) C4A 0.117(8) 0.065(5) 0.045(5) -0.002(4) 0.005(5) -0.040(5) C11A 0.066(5) 0.056(4) 0.055(4) -0.020(4) 0.021(4) -0.032(4) C12A 0.047(4) 0.061(6) 0.073(5) -0.021(5) 0.013(4) -0.025(4) C13A 0.109(7) 0.140(9) 0.077(7) -0.040(6) 0.050(5) -0.084(7) C14A 0.055(6) 0.106(9) 0.086(8) -0.024(6) 0.028(5) -0.053(6) P1A 0.0418(15) 0.0403(16) 0.0396(15) -0.0149(12) 0.0017(12) -0.0101(13) O1A 0.050(4) 0.033(4) 0.035(4) -0.013(3) 0.009(3) -0.011(3) O2A 0.044(4) 0.040(4) 0.042(4) -0.015(3) 0.005(3) -0.016(3) O3A 0.054(4) 0.041(4) 0.038(4) -0.007(3) -0.003(3) -0.014(3) O4A 0.052(4) 0.049(4) 0.043(4) -0.023(3) 0.005(3) -0.018(4) O5A 0.037(4) 0.044(4) 0.041(4) -0.024(3) 0.003(3) -0.007(3) O6A 0.040(4) 0.037(4) 0.050(4) -0.013(3) 0.000(3) -0.009(3) Cl1 0.080(2) 0.068(2) 0.0539(16) -0.0138(14) 0.0182(15) -0.0310(17) Cl2 0.125(3) 0.0502(17) 0.0657(18) -0.0006(14) -0.0137(18) -0.0209(18) Cl3 0.0733(19) 0.0553(18) 0.091(2) -0.0341(16) -0.0328(16) 0.0166(15) Cl4 0.0477(16) 0.084(2) 0.082(2) -0.0468(18) 0.0127(15) -0.0116(15) Cl5 0.0604(18) 0.0617(18) 0.083(2) -0.0328(16) -0.0100(15) -0.0185(15) Cl6 0.090(2) 0.086(2) 0.0591(18) -0.0365(15) -0.0173(16) -0.0095(16) Cl7 0.083(2) 0.077(2) 0.0382(15) -0.0073(14) 0.0044(14) -0.0048(16) Cl8 0.0804(19) 0.0680(18) 0.0526(16) -0.0079(13) 0.0111(14) -0.0322(15) Cl9 0.0421(15) 0.071(2) 0.085(2) -0.0304(16) 0.0016(14) -0.0095(14) Cl10 0.0694(18) 0.0561(16) 0.0758(17) -0.0341(13) 0.0221(14) -0.0111(13) Cl11 0.092(2) 0.0773(19) 0.0675(18) -0.0437(15) 0.0004(16) -0.0287(17) Cl12 0.0513(15) 0.0515(15) 0.0495(14) -0.0112(12) -0.0081(12) -0.0151(12) C15A 0.035(5) 0.052(6) 0.039(5) -0.021(5) 0.003(4) -0.018(5) C16A 0.033(5) 0.042(6) 0.040(5) -0.019(5) -0.003(4) -0.005(4) C17A 0.062(7) 0.031(6) 0.041(6) -0.017(5) 0.000(5) -0.014(5) C18A 0.079(8) 0.032(5) 0.048(6) -0.010(5) -0.023(5) -0.008(5) C19A 0.034(5) 0.062(7) 0.055(6) -0.037(5) -0.007(4) 0.002(5) C20A 0.033(5) 0.048(6) 0.042(5) -0.018(5) -0.012(4) -0.002(5) C21A 0.044(6) 0.038(6) 0.041(6) -0.017(5) 0.006(5) -0.004(5) C22A 0.048(5) 0.045(6) 0.032(5) -0.029(4) -0.006(4) -0.005(5) C23A 0.047(6) 0.028(5) 0.074(8) -0.028(5) 0.002(5) -0.003(5) C24A 0.065(7) 0.058(7) 0.037(6) -0.022(5) -0.011(5) -0.001(6) C25A 0.038(6) 0.046(6) 0.052(7) -0.010(5) 0.004(5) 0.005(5) C26A 0.049(6) 0.046(7) 0.043(7) -0.015(5) 0.003(5) -0.006(5) C27A 0.044(6) 0.031(5) 0.034(5) -0.009(4) 0.007(4) -0.017(4) C28A 0.046(6) 0.048(6) 0.034(5) -0.016(4) 0.004(4) -0.027(5) C29A 0.035(5) 0.036(5) 0.042(5) -0.011(4) 0.010(4) -0.005(4) C30A 0.055(6) 0.031(5) 0.046(5) -0.019(4) 0.013(4) -0.011(4) C31A 0.054(6) 0.037(5) 0.039(5) -0.022(4) 0.009(4) -0.009(5) C32A 0.051(6) 0.044(6) 0.027(5) -0.004(4) -0.004(4) -0.010(5) S1B 0.0655(17) 0.093(2) 0.0625(19) -0.0433(17) 0.0185(14) -0.0540(17) S2B 0.0777(19) 0.079(2) 0.0396(15) -0.0233(14) 0.0115(14) -0.0501(17) S3B 0.0459(14) 0.0550(16) 0.0407(14) -0.0184(12) -0.0002(11) -0.0213(12) S4B 0.0499(15) 0.0426(15) 0.0387(14) -0.0181(12) 0.0041(11) -0.0218(12) S5B 0.0493(15) 0.0642(17) 0.0365(13) -0.0149(12) -0.0021(11) -0.0270(13) S6B 0.0635(16) 0.0466(15) 0.0349(14) -0.0177(12) 0.0088(12) -0.0286(13) S7B 0.0689(18) 0.078(2) 0.0348(15) -0.0113(14) -0.0018(13) -0.0326(16) S8B 0.083(2) 0.072(2) 0.0445(16) -0.0242(14) 0.0180(15) -0.0483(18) C5B 0.049(6) 0.051(6) 0.034(5) -0.016(4) 0.015(4) -0.015(5) C6B 0.036(5) 0.054(6) 0.049(6) -0.029(5) 0.005(4) -0.016(5) C7B 0.038(5) 0.029(5) 0.043(5) -0.013(4) 0.010(4) -0.015(4) C8B 0.040(5) 0.056(6) 0.037(5) -0.027(4) -0.001(4) -0.017(5) C9B 0.040(5) 0.054(6) 0.023(5) -0.008(4) 0.005(4) -0.010(5) C10B 0.046(5) 0.042(6) 0.039(5) -0.023(4) 0.003(4) -0.007(4) C1B 0.068(5) 0.066(6) 0.051(4) -0.019(4) 0.014(4) -0.039(5) C2B 0.063(4) 0.066(5) 0.053(4) -0.033(4) 0.027(3) -0.035(4) C3B 0.089(8) 0.125(10) 0.081(7) -0.048(7) 0.021(6) -0.077(8) C4B 0.142(9) 0.156(11) 0.064(6) -0.064(7) 0.055(6) -0.110(9) C11B 0.080(5) 0.056(5) 0.046(4) 0.000(4) -0.005(4) -0.012(4) C12B 0.071(5) 0.057(5) 0.050(4) -0.010(4) 0.020(4) -0.034(4) C13B 0.140(9) 0.114(9) 0.037(5) 0.007(5) 0.002(5) -0.072(8) C14B 0.170(11) 0.104(9) 0.052(7) -0.010(6) 0.009(7) -0.099(8) P1B 0.0439(15) 0.0366(15) 0.0385(14) -0.0145(12) 0.0044(12) -0.0152(12) O1B 0.036(3) 0.036(4) 0.045(4) -0.011(3) 0.010(3) -0.001(3) O2B 0.038(4) 0.048(4) 0.050(4) -0.024(4) 0.010(3) -0.012(3) O3B 0.040(4) 0.038(4) 0.036(4) -0.010(3) 0.000(3) -0.011(3) O4B 0.042(4) 0.039(4) 0.031(3) -0.016(3) -0.004(3) -0.007(3) O5B 0.048(4) 0.040(4) 0.043(4) -0.015(3) -0.002(3) -0.018(3) O6B 0.055(4) 0.053(4) 0.034(4) -0.020(3) 0.007(3) -0.030(3) Cl13 0.0432(15) 0.0655(18) 0.0698(18) -0.0318(15) 0.0141(13) -0.0126(13) Cl14 0.0566(15) 0.0538(17) 0.0666(16) -0.0200(14) -0.0106(12) -0.0001(13) Cl15 0.092(2) 0.0509(17) 0.0614(17) -0.0030(14) 0.0031(15) -0.0158(16) Cl16 0.0665(17) 0.0578(18) 0.0623(17) -0.0184(14) 0.0250(14) -0.0233(15) Cl17 0.0394(14) 0.0583(17) 0.0713(17) -0.0217(14) 0.0031(12) -0.0091(13) Cl18 0.0695(18) 0.0583(16) 0.0789(18) -0.0398(14) 0.0197(14) -0.0103(13) Cl19 0.0778(19) 0.0754(18) 0.0657(17) -0.0435(15) 0.0013(15) -0.0236(15) Cl20 0.0532(15) 0.0509(15) 0.0448(13) -0.0070(11) -0.0122(11) -0.0147(12) Cl21 0.0734(18) 0.076(2) 0.0536(16) -0.0064(14) 0.0086(14) -0.0328(16) Cl22 0.085(2) 0.094(2) 0.0397(16) -0.0159(15) 0.0016(14) -0.0080(18) Cl23 0.083(2) 0.096(2) 0.0663(19) -0.0451(17) -0.0257(16) -0.0093(17) Cl24 0.0553(17) 0.0562(17) 0.089(2) -0.0322(16) -0.0129(15) -0.0155(14) C15B 0.042(5) 0.033(5) 0.041(6) -0.025(4) 0.008(4) -0.013(4) C16B 0.050(6) 0.025(5) 0.039(5) -0.016(4) -0.002(5) -0.008(4) C17B 0.047(5) 0.056(7) 0.042(5) -0.035(5) 0.017(4) -0.024(5) C18B 0.053(6) 0.032(5) 0.043(5) -0.013(4) -0.010(4) -0.005(4) C19B 0.053(6) 0.045(6) 0.033(5) -0.019(4) 0.007(4) -0.022(5) C20B 0.042(6) 0.054(7) 0.035(5) -0.019(5) 0.002(5) -0.020(5) C21B 0.041(6) 0.030(5) 0.034(5) -0.007(4) 0.004(4) -0.010(4) C22B 0.043(6) 0.018(4) 0.037(5) -0.001(4) 0.001(4) -0.002(4) C23B 0.037(5) 0.037(6) 0.048(6) -0.011(4) 0.001(4) -0.014(4) C24B 0.052(6) 0.041(5) 0.043(5) -0.018(4) 0.013(4) -0.011(4) C25B 0.064(7) 0.049(6) 0.034(5) -0.011(4) -0.003(5) -0.030(5) C26B 0.041(5) 0.026(5) 0.037(5) -0.005(4) 0.010(4) -0.017(4) C27B 0.035(5) 0.030(5) 0.051(6) -0.009(4) 0.007(4) -0.006(4) C28B 0.038(5) 0.037(5) 0.044(6) -0.019(5) -0.003(4) -0.010(4) C29B 0.049(6) 0.035(6) 0.037(6) -0.008(5) 0.006(5) -0.002(5) C30B 0.064(7) 0.055(7) 0.027(5) -0.016(5) -0.003(5) -0.002(6) C31B 0.042(6) 0.041(5) 0.043(6) -0.021(4) -0.011(5) 0.008(4) C32B 0.033(5) 0.053(6) 0.049(6) -0.023(5) -0.009(5) -0.002(5) C33A 0.068(9) 0.195(16) 0.153(14) -0.056(12) 0.027(8) -0.044(10) C34A 0.056(7) 0.160(14) 0.086(9) -0.058(9) 0.023(6) -0.059(8) N1A 0.101(10) 0.32(2) 0.200(15) -0.152(15) -0.019(10) -0.025(13) C33B 0.078(9) 0.082(9) 0.118(11) -0.016(8) -0.014(8) -0.009(8) C34B 0.055(8) 0.094(10) 0.081(8) 0.007(7) -0.009(6) -0.033(7) N1B 0.070(7) 0.132(10) 0.180(12) 0.015(8) 0.008(7) -0.031(7) C33C 0.093(10) 0.104(11) 0.129(12) -0.053(10) -0.001(9) -0.039(9) C34C 0.077(9) 0.085(10) 0.116(11) -0.032(8) 0.009(8) -0.042(8) N1C 0.105(9) 0.124(10) 0.140(9) -0.067(8) 0.009(7) -0.014(8) C33D 0.075(11) 0.208(19) 0.22(2) -0.048(15) -0.020(11) 0.044(11) C34D 0.118(12) 0.089(9) 0.100(10) -0.036(8) -0.035(9) -0.010(9) N1D 0.140(12) 0.088(7) 0.133(10) -0.029(6) -0.023(8) -0.009(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1A C5A 1.760(10) . ? S1A C1A 1.838(7) . ? S2A C6A 1.705(10) . ? S2A C2A 1.820(7) . ? S3A C7A 1.703(10) . ? S3A C5A 1.757(9) . ? S4A C7A 1.715(9) . ? S4A C6A 1.736(10) . ? S5A C9A 1.730(10) . ? S5A C8A 1.741(9) . ? S6A C10A 1.695(10) . ? S6A C8A 1.726(10) . ? S7A C9A 1.745(9) . ? S7A C11A 1.811(7) . ? S8A C10A 1.763(9) . ? S8A C12A 1.811(10) . ? C5A C6A 1.340(13) . ? C7A C8A 1.381(13) . ? C9A C10A 1.355(12) . ? C1A C2A 1.512(9) . ? C1A C3A 1.531(13) . ? C1A H1A 0.9800 . ? C2A C4A 1.533(12) . ? C2A H2A 0.9800 . ? C3A H3A1 0.9600 . ? C3A H3A2 0.9600 . ? C3A H3A3 0.9600 . ? C4A H4A1 0.9600 . ? C4A H4A2 0.9600 . ? C4A H4A3 0.9600 . ? C11A C12A 1.504(10) . ? C11A C13A 1.566(12) . ? C11A H11A 0.9800 . ? C12A C14A 1.572(14) . ? C12A H12A 0.9800 . ? C13A H13A 0.9600 . ? C13A H13B 0.9600 . ? C13A H13C 0.9600 . ? C14A H14A 0.9600 . ? C14A H14B 0.9600 . ? C14A H14C 0.9600 . ? P1A O5A 1.702(7) . ? P1A O3A 1.706(7) . ? P1A O2A 1.717(7) . ? P1A O4A 1.723(7) . ? P1A O1A 1.725(6) . ? P1A O6A 1.730(6) . ? O1A C15A 1.359(11) . ? O2A C16A 1.360(10) . ? O3A C21A 1.333(11) . ? O4A C22A 1.379(11) . ? O5A C27A 1.334(11) . ? O6A C28A 1.369(11) . ? Cl1 C17A 1.705(11) . ? Cl2 C18A 1.736(11) . ? Cl3 C19A 1.726(10) . ? Cl4 C20A 1.701(10) . ? Cl5 C23A 1.710(12) . ? Cl6 C24A 1.731(11) . ? Cl7 C25A 1.735(11) . ? Cl8 C26A 1.743(12) . ? Cl9 C29A 1.746(10) . ? Cl10 C30A 1.724(10) . ? Cl11 C31A 1.719(10) . ? Cl12 C32A 1.732(10) . ? C15A C20A 1.373(12) . ? C15A C16A 1.392(13) . ? C16A C17A 1.362(14) . ? C17A C18A 1.441(13) . ? C18A C19A 1.385(16) . ? C19A C20A 1.391(15) . ? C21A C22A 1.329(14) . ? C21A C26A 1.377(14) . ? C22A C23A 1.410(13) . ? C23A C24A 1.444(16) . ? C24A C25A 1.348(16) . ? C25A C26A 1.381(15) . ? C27A C28A 1.379(12) . ? C27A C32A 1.408(13) . ? C28A C29A 1.348(13) . ? C29A C30A 1.351(14) . ? C30A C31A 1.397(13) . ? C31A C32A 1.402(13) . ? S1B C5B 1.722(11) . ? S1B C1B 1.829(9) . ? S2B C6B 1.722(10) . ? S2B C2B 1.831(7) . ? S3B C7B 1.723(10) . ? S3B C5B 1.765(9) . ? S4B C7B 1.690(9) . ? S4B C6B 1.729(11) . ? S5B C8B 1.729(9) . ? S5B C9B 1.734(11) . ? S6B C10B 1.726(10) . ? S6B C8B 1.749(10) . ? S7B C9B 1.752(9) . ? S7B C11B 1.780(8) . ? S8B C10B 1.707(11) . ? S8B C12B 1.839(8) . ? C5B C6B 1.361(13) . ? C7B C8B 1.379(13) . ? C9B C10B 1.373(13) . ? C1B C2B 1.513(10) . ? C1B C3B 1.513(14) . ? C1B H1B 0.9800 . ? C2B C4B 1.506(11) . ? C2B H2B 0.9800 . ? C3B H3B1 0.9600 . ? C3B H3B2 0.9600 . ? C3B H3B3 0.9600 . ? C4B H4B1 0.9600 . ? C4B H4B2 0.9600 . ? C4B H4B3 0.9600 . ? C11B C13B 1.514(12) . ? C11B C12B 1.529(10) . ? C11B H11B 0.9800 . ? C12B C14B 1.531(13) . ? C12B H12B 0.9800 . ? C13B H13D 0.9600 . ? C13B H13E 0.9600 . ? C13B H13F 0.9600 . ? C14B H14D 0.9600 . ? C14B H14E 0.9600 . ? C14B H14F 0.9600 . ? P1B O4B 1.691(6) . ? P1B O5B 1.716(7) . ? P1B O3B 1.722(7) . ? P1B O2B 1.725(6) . ? P1B O6B 1.726(7) . ? P1B O1B 1.728(7) . ? O1B C15B 1.330(10) . ? O2B C16B 1.345(11) . ? O3B C21B 1.364(11) . ? O4B C22B 1.335(11) . ? O5B C27B 1.333(11) . ? O6B C28B 1.376(10) . ? Cl13 C17B 1.734(10) . ? Cl14 C18B 1.748(9) . ? Cl15 C19B 1.719(10) . ? Cl16 C20B 1.742(10) . ? Cl17 C23B 1.705(9) . ? Cl18 C24B 1.733(10) . ? Cl19 C25B 1.743(10) . ? Cl20 C26B 1.696(9) . ? Cl21 C29B 1.693(12) . ? Cl22 C30B 1.708(11) . ? Cl23 C31B 1.738(11) . ? Cl24 C32B 1.725(12) . ? C15B C20B 1.382(13) . ? C15B C16B 1.382(13) . ? C16B C17B 1.389(12) . ? C17B C18B 1.392(14) . ? C18B C19B 1.375(14) . ? C19B C20B 1.360(12) . ? C21B C26B 1.344(13) . ? C21B C22B 1.402(13) . ? C22B C23B 1.395(13) . ? C23B C24B 1.438(14) . ? C24B C25B 1.374(13) . ? C25B C26B 1.400(13) . ? C27B C32B 1.364(13) . ? C27B C28B 1.422(14) . ? C28B C29B 1.367(13) . ? C29B C30B 1.431(14) . ? C30B C31B 1.396(16) . ? C31B C32B 1.368(15) . ? C33A C34A 1.399(17) . ? C33A H33A 0.9600 . ? C33A H33B 0.9600 . ? C33A H33C 0.9600 . ? C34A N1A 1.087(16) . ? C33B C34B 1.429(19) . ? C33B H33D 0.9600 . ? C33B H33E 0.9600 . ? C33B H33F 0.9600 . ? C34B N1B 1.120(17) . ? C33C C34C 1.435(19) . ? C33C H33G 0.9600 . ? C33C H33H 0.9600 . ? C33C H33I 0.9600 . ? C34C N1C 1.110(17) . ? C33D C34D 1.368(18) . ? C33D H33J 0.9600 . ? C33D H33K 0.9600 . ? C33D H33L 0.9600 . ? C34D N1D 1.141(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 C5A S1A C1A 100.7(4) . . ? C6A S2A C2A 103.4(4) . . ? C7A S3A C5A 93.8(5) . . ? C7A S4A C6A 95.4(5) . . ? C9A S5A C8A 95.6(5) . . ? C10A S6A C8A 96.5(4) . . ? C9A S7A C11A 104.3(4) . . ? C10A S8A C12A 102.3(5) . . ? C6A C5A S3A 117.9(7) . . ? C6A C5A S1A 128.3(7) . . ? S3A C5A S1A 113.6(6) . . ? C5A C6A S2A 128.8(8) . . ? C5A C6A S4A 115.6(7) . . ? S2A C6A S4A 115.6(6) . . ? C8A C7A S3A 122.4(7) . . ? C8A C7A S4A 120.3(7) . . ? S3A C7A S4A 117.1(5) . . ? C7A C8A S6A 124.2(7) . . ? C7A C8A S5A 121.8(7) . . ? S6A C8A S5A 114.0(6) . . ? C10A C9A S5A 116.2(7) . . ? C10A C9A S7A 130.0(8) . . ? S5A C9A S7A 113.8(6) . . ? C9A C10A S6A 117.7(7) . . ? C9A C10A S8A 124.9(7) . . ? S6A C10A S8A 117.3(5) . . ? C2A C1A C3A 111.3(7) . . ? C2A C1A S1A 111.7(5) . . ? C3A C1A S1A 105.3(6) . . ? C2A C1A H1A 109.5 . . ? C3A C1A H1A 109.5 . . ? S1A C1A H1A 109.5 . . ? C1A C2A C4A 114.1(7) . . ? C1A C2A S2A 113.9(5) . . ? C4A C2A S2A 104.0(6) . . ? C1A C2A H2A 108.2 . . ? C4A C2A H2A 108.2 . . ? S2A C2A H2A 108.2 . . ? C1A C3A H3A1 109.5 . . ? C1A C3A H3A2 109.5 . . ? H3A1 C3A H3A2 109.5 . . ? C1A C3A H3A3 109.5 . . ? H3A1 C3A H3A3 109.5 . . ? H3A2 C3A H3A3 109.5 . . ? C2A C4A H4A1 109.5 . . ? C2A C4A H4A2 109.5 . . ? H4A1 C4A H4A2 109.5 . . ? C2A C4A H4A3 109.5 . . ? H4A1 C4A H4A3 109.5 . . ? H4A2 C4A H4A3 109.5 . . ? C12A C11A C13A 113.6(7) . . ? C12A C11A S7A 113.9(5) . . ? C13A C11A S7A 102.1(6) . . ? C12A C11A H11A 109.0 . . ? C13A C11A H11A 109.0 . . ? S7A C11A H11A 109.0 . . ? C11A C12A C14A 111.5(8) . . ? C11A C12A S8A 114.4(5) . . ? C14A C12A S8A 103.2(7) . . ? C11A C12A H12A 109.2 . . ? C14A C12A H12A 109.2 . . ? S8A C12A H12A 109.2 . . ? C11A C13A H13A 109.5 . . ? C11A C13A H13B 109.5 . . ? H13A C13A H13B 109.5 . . ? C11A C13A H13C 109.5 . . ? H13A C13A H13C 109.5 . . ? H13B C13A H13C 109.5 . . ? C12A C14A H14A 109.5 . . ? C12A C14A H14B 109.5 . . ? H14A C14A H14B 109.5 . . ? C12A C14A H14C 109.5 . . ? H14A C14A H14C 109.5 . . ? H14B C14A H14C 109.5 . . ? O5A P1A O3A 89.1(3) . . ? O5A P1A O2A 93.1(3) . . ? O3A P1A O2A 177.4(4) . . ? O5A P1A O4A 179.2(3) . . ? O3A P1A O4A 90.5(3) . . ? O2A P1A O4A 87.2(3) . . ? O5A P1A O1A 87.4(3) . . ? O3A P1A O1A 88.1(3) . . ? O2A P1A O1A 90.7(3) . . ? O4A P1A O1A 93.3(3) . . ? O5A P1A O6A 90.5(3) . . ? O3A P1A O6A 94.2(3) . . ? O2A P1A O6A 87.2(3) . . ? O4A P1A O6A 88.8(3) . . ? O1A P1A O6A 176.9(3) . . ? C15A O1A P1A 111.1(6) . . ? C16A O2A P1A 112.1(6) . . ? C21A O3A P1A 112.5(7) . . ? C22A O4A P1A 108.8(6) . . ? C27A O5A P1A 110.6(6) . . ? C28A O6A P1A 112.0(5) . . ? O1A C15A C20A 126.0(9) . . ? O1A C15A C16A 113.5(8) . . ? C20A C15A C16A 120.5(9) . . ? O2A C16A C17A 124.7(9) . . ? O2A C16A C15A 112.2(9) . . ? C17A C16A C15A 123.1(9) . . ? C16A C17A C18A 116.0(9) . . ? C16A C17A Cl1 121.2(7) . . ? C18A C17A Cl1 122.8(8) . . ? C19A C18A C17A 120.9(10) . . ? C19A C18A Cl2 121.9(8) . . ? C17A C18A Cl2 117.1(9) . . ? C18A C19A C20A 120.6(9) . . ? C18A C19A Cl3 119.1(9) . . ? C20A C19A Cl3 120.4(8) . . ? C15A C20A C19A 118.9(9) . . ? C15A C20A Cl4 119.5(8) . . ? C19A C20A Cl4 121.6(7) . . ? C22A C21A O3A 113.1(9) . . ? C22A C21A C26A 119.3(11) . . ? O3A C21A C26A 127.6(11) . . ? C21A C22A O4A 115.1(8) . . ? C21A C22A C23A 124.0(10) . . ? O4A C22A C23A 120.8(10) . . ? C22A C23A C24A 114.8(11) . . ? C22A C23A Cl5 121.5(9) . . ? C24A C23A Cl5 123.7(9) . . ? C25A C24A C23A 120.7(10) . . ? C25A C24A Cl6 123.0(9) . . ? C23A C24A Cl6 116.3(10) . . ? C24A C25A C26A 120.7(10) . . ? C24A C25A Cl7 118.7(9) . . ? C26A C25A Cl7 120.5(10) . . ? C21A C26A C25A 120.4(11) . . ? C21A C26A Cl8 118.7(9) . . ? C25A C26A Cl8 120.9(9) . . ? O5A C27A C28A 116.5(9) . . ? O5A C27A C32A 126.0(9) . . ? C28A C27A C32A 117.5(9) . . ? C29A C28A O6A 127.1(9) . . ? C29A C28A C27A 123.1(9) . . ? O6A C28A C27A 109.8(8) . . ? C28A C29A C30A 120.3(9) . . ? C28A C29A Cl9 118.7(8) . . ? C30A C29A Cl9 120.9(8) . . ? C29A C30A C31A 119.8(9) . . ? C29A C30A Cl10 121.4(8) . . ? C31A C30A Cl10 118.8(8) . . ? C30A C31A C32A 119.8(9) . . ? C30A C31A Cl11 121.7(8) . . ? C32A C31A Cl11 118.4(8) . . ? C31A C32A C27A 119.2(9) . . ? C31A C32A Cl12 122.3(8) . . ? C27A C32A Cl12 118.5(7) . . ? C5B S1B C1B 103.7(4) . . ? C6B S2B C2B 100.5(4) . . ? C7B S3B C5B 94.4(5) . . ? C7B S4B C6B 95.4(5) . . ? C8B S5B C9B 95.7(5) . . ? C10B S6B C8B 97.3(5) . . ? C9B S7B C11B 101.4(5) . . ? C10B S8B C12B 103.1(4) . . ? C6B C5B S1B 130.6(8) . . ? C6B C5B S3B 115.5(8) . . ? S1B C5B S3B 114.0(6) . . ? C5B C6B S2B 125.4(8) . . ? C5B C6B S4B 117.4(8) . . ? S2B C6B S4B 117.2(6) . . ? C8B C7B S4B 122.9(7) . . ? C8B C7B S3B 119.7(7) . . ? S4B C7B S3B 117.3(5) . . ? C7B C8B S5B 123.2(7) . . ? C7B C8B S6B 122.8(7) . . ? S5B C8B S6B 113.9(6) . . ? C10B C9B S5B 118.3(7) . . ? C10B C9B S7B 128.5(8) . . ? S5B C9B S7B 113.0(6) . . ? C9B C10B S8B 127.7(8) . . ? C9B C10B S6B 114.6(8) . . ? S8B C10B S6B 117.7(6) . . ? C2B C1B C3B 112.6(8) . . ? C2B C1B S1B 115.0(6) . . ? C3B C1B S1B 103.5(7) . . ? C2B C1B H1B 108.5 . . ? C3B C1B H1B 108.5 . . ? S1B C1B H1B 108.5 . . ? C4B C2B C1B 111.5(7) . . ? C4B C2B S2B 106.1(6) . . ? C1B C2B S2B 112.5(5) . . ? C4B C2B H2B 108.9 . . ? C1B C2B H2B 108.9 . . ? S2B C2B H2B 108.9 . . ? C1B C3B H3B1 109.5 . . ? C1B C3B H3B2 109.5 . . ? H3B1 C3B H3B2 109.5 . . ? C1B C3B H3B3 109.5 . . ? H3B1 C3B H3B3 109.5 . . ? H3B2 C3B H3B3 109.5 . . ? C2B C4B H4B1 109.5 . . ? C2B C4B H4B2 109.5 . . ? H4B1 C4B H4B2 109.5 . . ? C2B C4B H4B3 109.5 . . ? H4B1 C4B H4B3 109.5 . . ? H4B2 C4B H4B3 109.5 . . ? C13B C11B C12B 111.6(8) . . ? C13B C11B S7B 105.2(7) . . ? C12B C11B S7B 113.1(5) . . ? C13B C11B H11B 108.9 . . ? C12B C11B H11B 108.9 . . ? S7B C11B H11B 108.9 . . ? C11B C12B C14B 114.4(7) . . ? C11B C12B S8B 113.5(5) . . ? C14B C12B S8B 102.3(7) . . ? C11B C12B H12B 108.8 . . ? C14B C12B H12B 108.8 . . ? S8B C12B H12B 108.8 . . ? C11B C13B H13D 109.5 . . ? C11B C13B H13E 109.5 . . ? H13D C13B H13E 109.5 . . ? C11B C13B H13F 109.5 . . ? H13D C13B H13F 109.5 . . ? H13E C13B H13F 109.5 . . ? C12B C14B H14D 109.5 . . ? C12B C14B H14E 109.5 . . ? H14D C14B H14E 109.5 . . ? C12B C14B H14F 109.5 . . ? H14D C14B H14F 109.5 . . ? H14E C14B H14F 109.5 . . ? O4B P1B O5B 88.3(3) . . ? O4B P1B O3B 91.2(3) . . ? O5B P1B O3B 179.0(3) . . ? O4B P1B O2B 178.3(3) . . ? O5B P1B O2B 93.0(3) . . ? O3B P1B O2B 87.5(3) . . ? O4B P1B O6B 92.8(3) . . ? O5B P1B O6B 90.6(3) . . ? O3B P1B O6B 88.6(3) . . ? O2B P1B O6B 88.3(3) . . ? O4B P1B O1B 88.9(3) . . ? O5B P1B O1B 88.2(3) . . ? O3B P1B O1B 92.6(3) . . ? O2B P1B O1B 90.0(3) . . ? O6B P1B O1B 177.9(4) . . ? C15B O1B P1B 111.6(6) . . ? C16B O2B P1B 111.5(6) . . ? C21B O3B P1B 111.4(6) . . ? C22B O4B P1B 110.9(5) . . ? C27B O5B P1B 113.6(7) . . ? C28B O6B P1B 111.4(6) . . ? O1B C15B C20B 127.9(9) . . ? O1B C15B C16B 113.8(8) . . ? C20B C15B C16B 118.3(8) . . ? O2B C16B C15B 112.9(8) . . ? O2B C16B C17B 125.9(9) . . ? C15B C16B C17B 121.3(9) . . ? C16B C17B C18B 118.0(9) . . ? C16B C17B Cl13 118.8(8) . . ? C18B C17B Cl13 123.1(7) . . ? C19B C18B C17B 121.3(8) . . ? C19B C18B Cl14 120.0(8) . . ? C17B C18B Cl14 118.7(8) . . ? C20B C19B C18B 118.9(9) . . ? C20B C19B Cl15 121.1(7) . . ? C18B C19B Cl15 120.0(7) . . ? C19B C20B C15B 122.1(9) . . ? C19B C20B Cl16 120.7(8) . . ? C15B C20B Cl16 117.2(7) . . ? C26B C21B O3B 124.4(9) . . ? C26B C21B C22B 125.2(9) . . ? O3B C21B C22B 110.4(9) . . ? O4B C22B C23B 126.5(8) . . ? O4B C22B C21B 114.9(8) . . ? C23B C22B C21B 118.6(9) . . ? C22B C23B C24B 117.1(8) . . ? C22B C23B Cl17 120.5(8) . . ? C24B C23B Cl17 122.3(8) . . ? C25B C24B C23B 120.7(9) . . ? C25B C24B Cl18 121.2(9) . . ? C23B C24B Cl18 117.9(7) . . ? C24B C25B C26B 121.8(9) . . ? C24B C25B Cl19 119.3(9) . . ? C26B C25B Cl19 118.9(8) . . ? C21B C26B C25B 116.5(8) . . ? C21B C26B Cl20 121.0(7) . . ? C25B C26B Cl20 122.5(8) . . ? O5B C27B C32B 128.6(10) . . ? O5B C27B C28B 112.2(9) . . ? C32B C27B C28B 119.2(9) . . ? C29B C28B O6B 124.8(10) . . ? C29B C28B C27B 123.0(10) . . ? O6B C28B C27B 112.2(8) . . ? C28B C29B C30B 116.5(10) . . ? C28B C29B Cl21 121.8(8) . . ? C30B C29B Cl21 121.6(8) . . ? C31B C30B C29B 119.6(9) . . ? C31B C30B Cl22 121.6(8) . . ? C29B C30B Cl22 118.8(10) . . ? C32B C31B C30B 122.1(10) . . ? C32B C31B Cl23 119.9(10) . . ? C30B C31B Cl23 118.0(8) . . ? C27B C32B C31B 119.5(11) . . ? C27B C32B Cl24 118.0(8) . . ? C31B C32B Cl24 122.5(9) . . ? C34A C33A H33A 109.5 . . ? C34A C33A H33B 109.5 . . ? H33A C33A H33B 109.5 . . ? C34A C33A H33C 109.5 . . ? H33A C33A H33C 109.5 . . ? H33B C33A H33C 109.5 . . ? N1A C34A C33A 171.8(19) . . ? C34B C33B H33D 109.5 . . ? C34B C33B H33E 109.5 . . ? H33D C33B H33E 109.5 . . ? C34B C33B H33F 109.5 . . ? H33D C33B H33F 109.5 . . ? H33E C33B H33F 109.5 . . ? N1B C34B C33B 171.8(16) . . ? C34C C33C H33G 109.5 . . ? C34C C33C H33H 109.5 . . ? H33G C33C H33H 109.5 . . ? C34C C33C H33I 109.5 . . ? H33G C33C H33I 109.5 . . ? H33H C33C H33I 109.5 . . ? N1C C34C C33C 173.7(16) . . ? C34D C33D H33J 109.5 . . ? C34D C33D H33K 109.5 . . ? H33J C33D H33K 109.5 . . ? C34D C33D H33L 109.5 . . ? H33J C33D H33L 109.5 . . ? H33K C33D H33L 109.5 . . ? N1D C34D C33D 172(2) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.398 _refine_diff_density_min -0.438 _refine_diff_density_rms 0.066 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 820755' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(R,R,R,R)-TMBEDT-TTF TRISPHAT' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H22 Cl12 N2 O6 P S8' _chemical_formula_weight 1291.41 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' 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 11.5900(7) _cell_length_b 14.1051(9) _cell_length_c 17.1138(8) _cell_angle_alpha 76.714(4) _cell_angle_beta 89.170(4) _cell_angle_gamma 67.160(5) _cell_volume 2500.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 21304 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.715 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1294 _exptl_absorpt_coefficient_mu 1.077 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.785000 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _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 44365 _diffrn_reflns_av_R_equivalents 0.0372 _diffrn_reflns_av_sigmaI/netI 0.0833 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 27.50 _reflns_number_total 21289 _reflns_number_gt 11811 _reflns_threshold_expression >2sigma(I) _computing_data_collection KappaCCD _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'Denzo and Scalepak' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0215P)^2^+1.4632P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _chemical_absolute_configuration syn _refine_ls_abs_structure_Flack -0.01(8) _refine_ls_number_reflns 21289 _refine_ls_number_parameters 1175 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1340 _refine_ls_R_factor_gt 0.0557 _refine_ls_wR_factor_ref 0.0934 _refine_ls_wR_factor_gt 0.0752 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.002 _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 S1A S 0.3752(3) 0.5285(2) 0.54354(16) 0.0520(8) Uani 1 1 d . . . S2A S 0.4958(3) 0.6026(3) 0.69545(15) 0.0533(8) Uani 1 1 d . . . S3A S 0.4899(3) 0.6558(2) 0.43591(15) 0.0453(7) Uani 1 1 d . . . S4A S 0.5919(2) 0.7137(2) 0.56392(15) 0.0470(7) Uani 1 1 d . . . S5A S 0.6174(3) 0.7800(2) 0.30557(15) 0.0425(7) Uani 1 1 d . . . S6A S 0.7204(3) 0.8369(2) 0.43295(16) 0.0465(7) Uani 1 1 d . . . S7A S 0.7316(4) 0.8762(3) 0.17525(19) 0.0773(11) Uani 1 1 d . . . S8A S 0.8563(3) 0.9470(3) 0.32556(18) 0.0639(9) Uani 1 1 d . . . C5A C 0.4669(10) 0.6070(8) 0.5334(6) 0.038(2) Uani 1 1 d . . . C6A C 0.5107(9) 0.6383(8) 0.5931(6) 0.045(3) Uani 1 1 d . . . C7A C 0.5746(9) 0.7222(8) 0.4645(6) 0.042(3) Uani 1 1 d . . . C8A C 0.6279(9) 0.7749(7) 0.4050(6) 0.041(3) Uani 1 1 d . . . C9A C 0.7112(9) 0.8527(8) 0.2744(6) 0.043(3) Uani 1 1 d . . . C10A C 0.7550(9) 0.8776(8) 0.3386(6) 0.041(3) Uani 1 1 d . . . C1A C 0.4081(7) 0.4621(6) 0.6508(4) 0.054(2) Uani 1 1 d . . . H1A H 0.4962 0.4121 0.6613 0.065 Uiso 1 1 calc R . . C2A C 0.3820(7) 0.5396(5) 0.7030(4) 0.0456(16) Uani 1 1 d . . . H2A H 0.2980 0.5954 0.6859 0.055 Uiso 1 1 calc R . . C3A C 0.3222(13) 0.4008(10) 0.6704(7) 0.081(4) Uani 1 1 d . . . H3A1 H 0.3392 0.3511 0.6374 0.121 Uiso 1 1 calc R . . H3A2 H 0.2359 0.4497 0.6599 0.121 Uiso 1 1 calc R . . H3A3 H 0.3381 0.3633 0.7262 0.121 Uiso 1 1 calc R . . C4A C 0.3887(12) 0.4931(9) 0.7941(6) 0.071(3) Uani 1 1 d . . . H4A1 H 0.3703 0.5486 0.8218 0.106 Uiso 1 1 calc R . . H4A2 H 0.4715 0.4401 0.8123 0.106 Uiso 1 1 calc R . . H4A3 H 0.3285 0.4614 0.8050 0.106 Uiso 1 1 calc R . . C11A C 0.8229(7) 0.9570(6) 0.1615(4) 0.0569(18) Uani 1 1 d . . . H11A H 0.7650 1.0310 0.1556 0.068 Uiso 1 1 calc R . . C12A C 0.9215(9) 0.9274(7) 0.2310(6) 0.062(3) Uani 1 1 d . . . H12A H 0.9780 0.8527 0.2385 0.074 Uiso 1 1 calc R . . C13A C 0.8790(11) 0.9460(9) 0.0808(6) 0.089(4) Uani 1 1 d . . . H13A H 0.8128 0.9655 0.0397 0.134 Uiso 1 1 calc R . . H13B H 0.9361 0.8738 0.0854 0.134 Uiso 1 1 calc R . . H13C H 0.9233 0.9918 0.0667 0.134 Uiso 1 1 calc R . . C14A C 0.9990(12) 0.9948(11) 0.2138(8) 0.086(4) Uani 1 1 d . . . H14A H 1.0600 0.9742 0.2584 0.129 Uiso 1 1 calc R . . H14B H 0.9446 1.0683 0.2064 0.129 Uiso 1 1 calc R . . H14C H 1.0411 0.9844 0.1659 0.129 Uiso 1 1 calc R . . P1A P -0.2878(3) 0.5184(2) 0.18918(16) 0.0405(7) Uani 1 1 d . . . O1A O -0.4239(6) 0.6203(5) 0.1987(4) 0.0418(17) Uani 1 1 d . . . O2A O -0.2531(6) 0.5993(5) 0.1097(4) 0.0436(18) Uani 1 1 d . . . O3A O -0.3221(6) 0.4409(5) 0.2708(4) 0.0448(19) Uani 1 1 d . . . O4A O -0.1998(7) 0.5515(6) 0.2503(4) 0.050(2) Uani 1 1 d . . . O5A O -0.3742(6) 0.4840(5) 0.1288(4) 0.0420(18) Uani 1 1 d . . . O6A O -0.1508(6) 0.4161(5) 0.1765(4) 0.0441(18) Uani 1 1 d . . . Cl1 Cl -0.2238(3) 0.7602(2) -0.03287(17) 0.0655(9) Uani 1 1 d . . . Cl2 Cl -0.4621(4) 0.9744(2) -0.0709(2) 0.0887(12) Uani 1 1 d . . . Cl3 Cl -0.6913(3) 1.0007(2) 0.0345(2) 0.0816(11) Uani 1 1 d . . . Cl4 Cl -0.6729(3) 0.8128(3) 0.1814(2) 0.0700(10) Uani 1 1 d . . . Cl5 Cl -0.0530(3) 0.5903(2) 0.3753(2) 0.0677(9) Uani 1 1 d . . . Cl6 Cl -0.0837(3) 0.4803(3) 0.55264(19) 0.0818(11) Uani 1 1 d . . . Cl7 Cl -0.2461(3) 0.3446(3) 0.57998(17) 0.0759(10) Uani 1 1 d . . . Cl8 Cl -0.3723(3) 0.3157(3) 0.43015(18) 0.0677(9) Uani 1 1 d . . . Cl9 Cl 0.0718(3) 0.2474(3) 0.1258(2) 0.0704(10) Uani 1 1 d . . . Cl10 Cl -0.0070(3) 0.1635(2) -0.01088(19) 0.0695(9) Uani 1 1 d . . . Cl11 Cl -0.2946(3) 0.2429(3) -0.06577(19) 0.0727(9) Uani 1 1 d . . . Cl12 Cl -0.4939(3) 0.4213(2) 0.00338(16) 0.0548(8) Uani 1 1 d . . . C15A C -0.4439(10) 0.7066(8) 0.1389(6) 0.039(3) Uani 1 1 d . . . C16A C -0.3496(9) 0.6965(7) 0.0883(6) 0.037(3) Uani 1 1 d . . . C17A C -0.3500(10) 0.7764(8) 0.0237(6) 0.044(3) Uani 1 1 d . . . C18A C -0.4565(11) 0.8750(8) 0.0072(6) 0.049(3) Uani 1 1 d . . . C19A C -0.5553(10) 0.8820(8) 0.0565(7) 0.055(3) Uani 1 1 d . . . C20A C -0.5511(10) 0.7995(9) 0.1222(6) 0.046(3) Uani 1 1 d . . . C21A C -0.2720(11) 0.4446(8) 0.3403(6) 0.046(3) Uani 1 1 d . . . C22A C -0.2064(10) 0.5049(8) 0.3307(6) 0.042(3) Uani 1 1 d . . . C23A C -0.1425(11) 0.5165(8) 0.3936(7) 0.048(3) Uani 1 1 d . . . C24A C -0.1593(10) 0.4643(8) 0.4716(6) 0.046(3) Uani 1 1 d . . . C25A C -0.2310(10) 0.4063(9) 0.4819(6) 0.051(3) Uani 1 1 d . . . C26A C -0.2874(10) 0.3948(8) 0.4182(6) 0.048(3) Uani 1 1 d . . . C27A C -0.2993(10) 0.4117(7) 0.0933(6) 0.036(2) Uani 1 1 d . . . C28A C -0.1722(10) 0.3701(8) 0.1201(5) 0.042(3) Uani 1 1 d . . . C29A C -0.0834(9) 0.2939(8) 0.0909(6) 0.041(3) Uani 1 1 d . . . C30A C -0.1210(10) 0.2573(8) 0.0303(6) 0.047(3) Uani 1 1 d . . . C31A C -0.2487(11) 0.2928(8) 0.0046(6) 0.049(3) Uani 1 1 d . . . C32A C -0.3382(10) 0.3703(7) 0.0354(5) 0.040(3) Uani 1 1 d . . . S1B S 0.0353(3) 0.7108(3) 0.58127(17) 0.0604(9) Uani 1 1 d . . . S2B S 0.1435(3) 0.7900(3) 0.73389(16) 0.0602(9) Uani 1 1 d . . . S3B S 0.1683(3) 0.8223(2) 0.47705(15) 0.0445(7) Uani 1 1 d . . . S4B S 0.2670(3) 0.8831(2) 0.60493(15) 0.0424(7) Uani 1 1 d . . . S5B S 0.2965(3) 0.9417(2) 0.34724(15) 0.0490(8) Uani 1 1 d . . . S6B S 0.3985(3) 1.0041(2) 0.47239(15) 0.0438(7) Uani 1 1 d . . . S7B S 0.3804(3) 1.0596(3) 0.21217(17) 0.0612(9) Uani 1 1 d . . . S8B S 0.5049(3) 1.1352(3) 0.36130(17) 0.0607(9) Uani 1 1 d . . . C5B C 0.1257(10) 0.7827(7) 0.5756(5) 0.043(3) Uani 1 1 d . . . C6B C 0.1758(9) 0.8132(8) 0.6307(5) 0.042(3) Uani 1 1 d . . . C7B C 0.2555(9) 0.8843(8) 0.5029(5) 0.039(3) Uani 1 1 d . . . C8B C 0.3120(9) 0.9359(8) 0.4496(5) 0.039(3) Uani 1 1 d . . . C9B C 0.3744(9) 1.0300(7) 0.3158(6) 0.038(2) Uani 1 1 d . . . C10B C 0.4249(10) 1.0570(8) 0.3726(6) 0.042(3) Uani 1 1 d . . . C1B C -0.0023(9) 0.6927(7) 0.6869(5) 0.056(2) Uani 1 1 d . . . H1B H 0.0621 0.6261 0.7180 0.067 Uiso 1 1 calc R . . C2B C -0.0078(7) 0.7791(6) 0.7252(4) 0.0551(18) Uani 1 1 d . . . H2B H -0.0680 0.8465 0.6920 0.066 Uiso 1 1 calc R . . C3B C -0.1253(11) 0.6774(10) 0.6830(8) 0.072(3) Uani 1 1 d . . . H3B1 H -0.1140 0.6207 0.6576 0.108 Uiso 1 1 calc R . . H3B2 H -0.1897 0.7417 0.6523 0.108 Uiso 1 1 calc R . . H3B3 H -0.1495 0.6602 0.7365 0.108 Uiso 1 1 calc R . . C4B C -0.0484(11) 0.7664(9) 0.8099(6) 0.090(4) Uani 1 1 d . . . H4B1 H -0.0500 0.8246 0.8307 0.135 Uiso 1 1 calc R . . H4B2 H 0.0099 0.7010 0.8436 0.135 Uiso 1 1 calc R . . H4B3 H -0.1307 0.7655 0.8094 0.135 Uiso 1 1 calc R . . C11B C 0.4224(7) 1.1711(6) 0.1993(4) 0.062(2) Uani 1 1 d . . . H11B H 0.3503 1.2311 0.2096 0.074 Uiso 1 1 calc R . . C12B C 0.5366(8) 1.1518(6) 0.2547(4) 0.056(2) Uani 1 1 d . . . H12B H 0.6052 1.0866 0.2489 0.067 Uiso 1 1 calc R . . C13B C 0.4465(13) 1.1972(11) 0.1107(7) 0.102(5) Uani 1 1 d . . . H13D H 0.3736 1.2089 0.0777 0.153 Uiso 1 1 calc R . . H13E H 0.5173 1.1392 0.0998 0.153 Uiso 1 1 calc R . . H13F H 0.4638 1.2601 0.0986 0.153 Uiso 1 1 calc R . . C14B C 0.5853(14) 1.2391(10) 0.2408(7) 0.085(4) Uani 1 1 d . . . H14D H 0.6560 1.2187 0.2787 0.127 Uiso 1 1 calc R . . H14E H 0.5201 1.3033 0.2479 0.127 Uiso 1 1 calc R . . H14F H 0.6107 1.2507 0.1870 0.127 Uiso 1 1 calc R . . P1B P 0.1674(3) 0.1477(2) 0.71656(16) 0.0412(7) Uani 1 1 d . . . O1B O 0.1318(6) 0.0690(5) 0.7984(4) 0.0417(18) Uani 1 1 d . . . O2B O 0.3061(6) 0.0408(5) 0.7124(4) 0.0437(19) Uani 1 1 d . . . O3B O 0.2519(6) 0.1835(5) 0.7758(4) 0.0388(18) Uani 1 1 d . . . O4B O 0.0345(6) 0.2497(5) 0.7262(4) 0.0398(18) Uani 1 1 d . . . O5B O 0.0809(6) 0.1135(5) 0.6561(4) 0.0416(18) Uani 1 1 d . . . O6B O 0.2040(6) 0.2222(5) 0.6329(4) 0.0435(18) Uani 1 1 d . . . Cl13 Cl 0.5518(3) -0.1484(2) 0.72862(18) 0.0622(9) Uani 1 1 d . . . Cl14 Cl 0.5622(3) -0.3366(2) 0.87744(18) 0.0663(9) Uani 1 1 d . . . Cl15 Cl 0.3349(3) -0.3072(2) 0.98152(18) 0.0725(9) Uani 1 1 d . . . Cl16 Cl 0.0980(3) -0.0902(2) 0.94038(17) 0.0635(9) Uani 1 1 d . . . Cl17 Cl -0.1946(3) 0.4226(2) 0.77454(18) 0.0573(8) Uani 1 1 d . . . Cl18 Cl -0.1126(3) 0.5124(2) 0.90807(19) 0.0676(9) Uani 1 1 d . . . Cl19 Cl 0.1701(3) 0.4324(3) 0.96490(18) 0.0721(9) Uani 1 1 d . . . Cl20 Cl 0.3711(3) 0.2492(2) 0.89890(16) 0.0517(7) Uani 1 1 d . . . Cl21 Cl 0.2534(3) 0.3422(3) 0.47252(18) 0.0693(9) Uani 1 1 d . . . Cl22 Cl 0.1241(3) 0.3104(3) 0.32563(18) 0.0831(11) Uani 1 1 d . . . Cl23 Cl -0.0335(3) 0.1723(3) 0.3558(2) 0.0876(12) Uani 1 1 d . . . Cl24 Cl -0.0662(3) 0.0667(2) 0.5342(2) 0.0666(9) Uani 1 1 d . . . C15B C 0.2234(9) -0.0286(8) 0.8219(6) 0.041(3) Uani 1 1 d . . . C16B C 0.3252(10) -0.0446(8) 0.7738(6) 0.037(3) Uani 1 1 d . . . C17B C 0.4279(9) -0.1388(8) 0.7888(6) 0.043(3) Uani 1 1 d . . . C18B C 0.4331(10) -0.2189(8) 0.8545(6) 0.045(3) Uani 1 1 d . . . C19B C 0.3309(11) -0.2013(8) 0.9005(5) 0.050(3) Uani 1 1 d . . . C20B C 0.2270(10) -0.1096(8) 0.8849(6) 0.044(3) Uani 1 1 d . . . C21B C 0.1757(10) 0.2634(7) 0.8099(5) 0.034(2) Uani 1 1 d . . . C22B C 0.0515(9) 0.2984(7) 0.7811(6) 0.037(3) Uani 1 1 d . . . C23B C -0.0393(9) 0.3770(8) 0.8115(6) 0.042(3) Uani 1 1 d . . . C24B C -0.0011(9) 0.4182(7) 0.8681(6) 0.042(3) Uani 1 1 d . . . C25B C 0.1217(10) 0.3805(8) 0.8947(6) 0.042(3) Uani 1 1 d . . . C26B C 0.2139(9) 0.2984(7) 0.8661(6) 0.039(3) Uani 1 1 d . . . C28B C 0.1537(9) 0.2179(8) 0.5634(6) 0.039(3) Uani 1 1 d . . . C27B C 0.0802(10) 0.1550(8) 0.5788(6) 0.043(3) Uani 1 1 d . . . C29B C 0.1661(10) 0.2675(8) 0.4889(6) 0.049(3) Uani 1 1 d . . . C30B C 0.1033(11) 0.2522(9) 0.4213(6) 0.058(3) Uani 1 1 d . . . C31B C 0.0351(11) 0.1867(9) 0.4366(7) 0.058(3) Uani 1 1 d . . . C32B C 0.0232(10) 0.1411(8) 0.5150(7) 0.051(3) Uani 1 1 d . . . N1A N 0.6280(13) 0.2298(9) 0.7469(8) 0.128(5) Uani 1 1 d . . . C33A C 0.8491(13) 0.0962(15) 0.7725(10) 0.129(5) Uani 1 1 d . . . H33A H 0.8991 0.1364 0.7742 0.194 Uiso 1 1 calc R . . H33B H 0.8704 0.0627 0.7284 0.194 Uiso 1 1 calc R . . H33C H 0.8652 0.0430 0.8221 0.194 Uiso 1 1 calc R . . C34A C 0.7227(12) 0.1634(10) 0.7620(8) 0.080(4) Uani 1 1 d . . . N1B N 0.7175(11) -0.0273(9) 0.5953(8) 0.127(5) Uani 1 1 d . . . C33B C 0.5238(13) 0.1284(10) 0.6090(8) 0.089(4) Uani 1 1 d . . . H33D H 0.5227 0.1284 0.6651 0.133 Uiso 1 1 calc R . . H33E H 0.4487 0.1232 0.5913 0.133 Uiso 1 1 calc R . . H33F H 0.5279 0.1931 0.5783 0.133 Uiso 1 1 calc R . . C34B C 0.6312(11) 0.0399(11) 0.5974(8) 0.070(4) Uani 1 1 d . . . N1C N 0.1705(15) 0.6932(13) 0.3280(8) 0.135(5) Uani 1 1 d . . . C33C C 0.3480(15) 0.5280(13) 0.3022(11) 0.124(6) Uani 1 1 d . . . H33G H 0.3944 0.5490 0.2597 0.186 Uiso 1 1 calc R . . H33H H 0.3173 0.4792 0.2885 0.186 Uiso 1 1 calc R . . H33I H 0.4018 0.4943 0.3513 0.186 Uiso 1 1 calc R . . C34C C 0.2449(18) 0.6189(14) 0.3130(10) 0.104(5) Uani 1 1 d . . . N1D N 0.2515(16) 0.4599(17) 0.1503(11) 0.214(9) Uani 1 1 d . . . C33D C 0.0342(14) 0.5916(18) 0.1274(13) 0.222(12) Uani 1 1 d . . . H33J H -0.0214 0.5808 0.1673 0.333 Uiso 1 1 calc R . . H33K H -0.0002 0.5959 0.0753 0.333 Uiso 1 1 calc R . . H33L H 0.0438 0.6563 0.1268 0.333 Uiso 1 1 calc R . . C34D C 0.1512(19) 0.5068(18) 0.1457(10) 0.125(8) Uani 1 1 d . . . 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 S1A 0.073(2) 0.0556(18) 0.0438(16) -0.0192(13) 0.0088(14) -0.0387(17) S2A 0.0581(19) 0.080(2) 0.0298(14) -0.0143(14) 0.0025(12) -0.0347(17) S3A 0.0563(18) 0.0507(16) 0.0371(14) -0.0178(12) 0.0047(12) -0.0260(14) S4A 0.0414(16) 0.0648(17) 0.0420(14) -0.0189(13) -0.0004(11) -0.0252(13) S5A 0.0491(17) 0.0467(16) 0.0404(14) -0.0181(12) 0.0056(12) -0.0240(14) S6A 0.0462(17) 0.0553(17) 0.0440(15) -0.0197(13) 0.0001(12) -0.0220(14) S7A 0.102(3) 0.121(3) 0.0495(18) -0.0276(18) 0.0171(17) -0.083(2) S8A 0.065(2) 0.084(2) 0.0656(19) -0.0226(17) 0.0015(14) -0.0507(17) C5A 0.040(5) 0.036(5) 0.041(5) -0.009(4) 0.005(4) -0.019(4) C6A 0.031(6) 0.049(6) 0.041(6) -0.016(5) -0.002(4) 0.003(5) C7A 0.039(6) 0.038(5) 0.052(6) -0.011(4) 0.010(4) -0.019(5) C8A 0.030(6) 0.030(5) 0.060(6) -0.019(5) -0.004(5) -0.006(5) C9A 0.037(6) 0.040(6) 0.065(6) -0.018(5) 0.021(4) -0.024(5) C10A 0.035(5) 0.050(6) 0.054(6) -0.024(5) -0.003(4) -0.027(5) C1A 0.058(5) 0.050(5) 0.052(4) -0.011(3) 0.009(4) -0.021(4) C2A 0.047(4) 0.047(4) 0.045(4) -0.010(3) 0.007(3) -0.022(3) C3A 0.121(9) 0.079(7) 0.071(7) -0.024(5) 0.019(6) -0.066(7) C4A 0.114(8) 0.065(5) 0.042(5) -0.007(4) 0.005(5) -0.048(6) C11A 0.058(5) 0.068(5) 0.057(4) -0.024(4) 0.016(4) -0.034(4) C12A 0.050(5) 0.062(6) 0.072(6) -0.023(5) 0.012(4) -0.018(4) C13A 0.113(8) 0.112(8) 0.070(6) -0.039(6) 0.045(5) -0.065(7) C14A 0.088(9) 0.143(11) 0.082(7) -0.042(7) 0.037(6) -0.099(9) P1A 0.0416(17) 0.0396(16) 0.0383(15) -0.0131(12) 0.0036(12) -0.0118(14) O1A 0.047(4) 0.042(4) 0.041(4) -0.016(3) 0.012(3) -0.020(3) O2A 0.043(4) 0.034(4) 0.049(4) -0.018(3) 0.013(3) -0.007(3) O3A 0.054(5) 0.053(4) 0.028(4) -0.012(3) -0.005(3) -0.020(4) O4A 0.056(5) 0.052(4) 0.047(5) -0.020(4) 0.004(4) -0.022(4) O5A 0.035(4) 0.049(4) 0.043(4) -0.022(3) -0.001(3) -0.011(4) O6A 0.046(4) 0.035(4) 0.050(4) -0.018(3) -0.003(3) -0.010(3) Cl1 0.075(2) 0.0632(19) 0.0552(17) -0.0091(14) 0.0160(14) -0.0274(17) Cl2 0.131(3) 0.0491(18) 0.0627(19) 0.0044(15) -0.0170(18) -0.0203(19) Cl3 0.073(2) 0.0569(19) 0.088(2) -0.0347(16) -0.0310(16) 0.0131(16) Cl4 0.0472(18) 0.086(2) 0.080(2) -0.0472(18) 0.0137(15) -0.0144(17) Cl5 0.059(2) 0.0648(19) 0.082(2) -0.0337(16) -0.0078(16) -0.0183(16) Cl6 0.086(2) 0.087(2) 0.0600(18) -0.0344(16) -0.0193(16) -0.0118(18) Cl7 0.088(2) 0.078(2) 0.0356(15) -0.0053(13) 0.0031(14) -0.0094(17) Cl8 0.079(2) 0.0656(18) 0.0567(17) -0.0065(14) 0.0091(15) -0.0315(17) Cl9 0.0401(18) 0.074(2) 0.089(2) -0.0313(17) 0.0030(14) -0.0076(16) Cl10 0.073(2) 0.0540(16) 0.0779(18) -0.0338(13) 0.0231(14) -0.0118(14) Cl11 0.083(2) 0.0743(19) 0.0699(18) -0.0419(15) 0.0016(15) -0.0269(17) Cl12 0.0516(17) 0.0573(16) 0.0486(15) -0.0122(12) -0.0101(12) -0.0141(14) C15A 0.041(6) 0.041(6) 0.045(6) -0.029(5) 0.008(5) -0.014(5) C16A 0.042(6) 0.026(5) 0.040(5) -0.011(4) -0.013(4) -0.008(5) C17A 0.054(7) 0.049(7) 0.037(6) -0.025(5) 0.003(5) -0.022(6) C18A 0.057(7) 0.028(5) 0.051(6) -0.017(4) -0.021(5) -0.001(5) C19A 0.038(6) 0.045(7) 0.069(7) -0.036(6) -0.022(5) 0.012(5) C20A 0.047(7) 0.049(6) 0.046(6) -0.023(5) -0.002(5) -0.016(5) C21A 0.052(7) 0.033(6) 0.042(6) -0.008(5) 0.009(5) -0.007(5) C22A 0.052(7) 0.038(6) 0.033(6) -0.017(5) -0.002(5) -0.010(5) C23A 0.047(7) 0.026(5) 0.066(7) -0.018(5) -0.006(5) -0.007(5) C24A 0.048(6) 0.043(5) 0.038(5) -0.029(4) -0.009(4) 0.004(5) C25A 0.037(6) 0.056(7) 0.043(6) -0.011(5) 0.014(4) -0.001(5) C26A 0.052(7) 0.048(6) 0.040(6) -0.022(5) 0.010(5) -0.009(6) C27A 0.042(6) 0.025(5) 0.038(5) -0.007(4) 0.005(4) -0.010(4) C28A 0.050(7) 0.047(6) 0.030(5) -0.013(4) 0.006(4) -0.018(5) C29A 0.043(6) 0.040(6) 0.044(5) -0.013(4) 0.013(5) -0.018(5) C30A 0.062(7) 0.040(5) 0.046(5) -0.026(4) 0.026(5) -0.018(5) C31A 0.062(7) 0.042(6) 0.034(5) -0.007(4) -0.004(4) -0.013(5) C32A 0.059(7) 0.038(6) 0.016(4) -0.007(4) 0.001(4) -0.012(5) S1B 0.068(2) 0.089(2) 0.0581(18) -0.0413(16) 0.0215(14) -0.0537(18) S2B 0.086(2) 0.087(2) 0.0368(15) -0.0296(15) 0.0158(14) -0.056(2) S3B 0.0475(17) 0.0548(16) 0.0367(14) -0.0154(12) -0.0007(11) -0.0234(13) S4B 0.0538(18) 0.0458(16) 0.0385(14) -0.0198(12) 0.0050(12) -0.0258(14) S5B 0.0549(18) 0.0610(17) 0.0351(14) -0.0128(12) -0.0010(12) -0.0265(14) S6B 0.0580(18) 0.0455(15) 0.0375(14) -0.0191(12) 0.0092(12) -0.0257(14) S7B 0.074(2) 0.074(2) 0.0381(16) -0.0090(15) -0.0038(14) -0.0340(18) S8B 0.082(2) 0.075(2) 0.0447(17) -0.0221(15) 0.0159(15) -0.048(2) C5B 0.056(6) 0.036(5) 0.030(5) -0.008(4) 0.014(4) -0.011(5) C6B 0.053(6) 0.053(6) 0.025(5) -0.019(4) -0.003(4) -0.021(5) C7B 0.047(6) 0.048(6) 0.024(5) -0.016(4) 0.010(4) -0.017(5) C8B 0.037(5) 0.051(6) 0.027(5) -0.022(4) -0.006(4) -0.010(5) C9B 0.047(6) 0.040(6) 0.033(5) -0.005(4) 0.001(4) -0.025(5) C10B 0.042(6) 0.044(6) 0.034(5) -0.017(4) 0.011(4) -0.007(5) C1B 0.058(6) 0.066(6) 0.054(5) -0.014(4) 0.006(4) -0.037(5) C2B 0.059(5) 0.069(5) 0.055(4) -0.028(4) 0.023(3) -0.038(4) C3B 0.055(7) 0.088(8) 0.084(7) -0.029(6) 0.010(5) -0.035(6) C4B 0.127(9) 0.125(9) 0.067(6) -0.047(6) 0.048(6) -0.091(8) C11B 0.074(6) 0.051(5) 0.038(4) 0.002(3) -0.003(4) -0.009(4) C12B 0.075(6) 0.067(5) 0.036(4) -0.011(4) 0.020(4) -0.039(4) C13B 0.134(10) 0.121(10) 0.046(6) 0.017(6) 0.000(5) -0.066(8) C14B 0.135(10) 0.088(8) 0.053(6) 0.009(5) 0.007(6) -0.081(7) P1B 0.0434(18) 0.0388(15) 0.0432(15) -0.0179(12) 0.0050(12) -0.0137(14) O1B 0.036(4) 0.041(4) 0.043(4) -0.010(3) 0.006(3) -0.010(3) O2B 0.036(4) 0.040(4) 0.048(4) -0.021(3) 0.009(3) -0.003(3) O3B 0.040(4) 0.033(4) 0.038(4) -0.013(3) 0.002(3) -0.007(3) O4B 0.035(4) 0.045(4) 0.036(4) -0.014(3) 0.000(3) -0.010(3) O5B 0.046(5) 0.040(4) 0.042(4) -0.018(3) 0.001(3) -0.016(4) O6B 0.057(5) 0.040(4) 0.039(4) -0.011(3) 0.009(3) -0.024(4) Cl13 0.0446(18) 0.0645(19) 0.0743(19) -0.0324(16) 0.0127(14) -0.0097(15) Cl14 0.0548(17) 0.0557(18) 0.0678(17) -0.0191(14) -0.0105(13) 0.0027(14) Cl15 0.090(2) 0.0513(18) 0.0641(18) -0.0064(14) 0.0053(15) -0.0190(17) Cl16 0.067(2) 0.0642(18) 0.0633(18) -0.0242(14) 0.0274(14) -0.0264(16) Cl17 0.0412(16) 0.0561(17) 0.0694(17) -0.0216(13) 0.0024(12) -0.0100(14) Cl18 0.0646(19) 0.0574(16) 0.0809(18) -0.0418(14) 0.0207(14) -0.0106(14) Cl19 0.085(2) 0.0727(18) 0.0632(17) -0.0423(14) -0.0017(15) -0.0217(17) Cl20 0.0521(17) 0.0490(15) 0.0490(15) -0.0092(12) -0.0087(12) -0.0157(13) Cl21 0.076(2) 0.077(2) 0.0533(17) -0.0075(14) 0.0105(15) -0.0330(18) Cl22 0.083(2) 0.093(2) 0.0450(17) -0.0197(15) 0.0034(15) -0.0025(18) Cl23 0.085(2) 0.097(2) 0.068(2) -0.0491(17) -0.0239(17) -0.0056(18) Cl24 0.057(2) 0.0558(17) 0.091(2) -0.0322(16) -0.0135(16) -0.0177(15) C15B 0.041(6) 0.050(6) 0.038(5) -0.029(5) 0.015(4) -0.014(5) C16B 0.040(6) 0.034(5) 0.031(5) -0.006(4) -0.008(4) -0.009(5) C17B 0.031(6) 0.050(7) 0.048(6) -0.028(5) 0.004(4) -0.008(5) C18B 0.055(7) 0.040(6) 0.041(6) -0.013(5) -0.005(5) -0.017(5) C19B 0.078(8) 0.052(7) 0.028(5) -0.012(4) 0.002(5) -0.031(6) C20B 0.045(7) 0.033(6) 0.040(6) -0.009(5) -0.003(5) -0.001(5) C21B 0.044(6) 0.032(5) 0.025(5) -0.010(4) 0.004(4) -0.014(5) C22B 0.039(6) 0.018(5) 0.046(6) -0.002(4) -0.003(4) -0.006(4) C23B 0.032(6) 0.031(5) 0.050(6) -0.004(4) -0.003(4) -0.001(5) C24B 0.040(6) 0.027(4) 0.049(5) -0.007(4) -0.001(4) -0.005(4) C25B 0.052(7) 0.044(5) 0.040(5) -0.022(4) 0.006(4) -0.024(5) C26B 0.031(5) 0.031(5) 0.054(6) -0.004(4) 0.006(4) -0.015(5) C28B 0.031(6) 0.044(6) 0.036(6) -0.020(5) -0.006(4) -0.004(5) C27B 0.035(6) 0.038(6) 0.050(7) -0.021(5) 0.004(5) -0.002(5) C29B 0.042(7) 0.034(6) 0.049(7) -0.004(5) -0.006(5) 0.004(5) C30B 0.071(8) 0.047(6) 0.034(5) -0.017(5) -0.015(5) 0.004(6) C31B 0.059(7) 0.043(6) 0.060(7) -0.021(5) -0.009(5) -0.002(5) C32B 0.040(6) 0.052(6) 0.053(7) -0.028(5) -0.002(5) -0.001(5) N1A 0.112(11) 0.079(6) 0.152(10) -0.010(6) -0.038(8) -0.002(6) C33A 0.070(10) 0.189(15) 0.129(11) -0.040(10) 0.006(8) -0.050(11) C34A 0.057(8) 0.078(8) 0.086(9) -0.031(7) -0.014(7) 0.000(7) N1B 0.061(7) 0.087(8) 0.198(12) -0.001(7) 0.033(7) -0.012(6) C33B 0.084(10) 0.077(8) 0.113(11) -0.038(8) -0.013(8) -0.031(8) C34B 0.035(6) 0.071(8) 0.090(9) -0.006(7) -0.006(6) -0.015(6) N1C 0.136(12) 0.155(12) 0.127(8) -0.077(8) 0.003(7) -0.047(10) C33C 0.085(11) 0.104(12) 0.156(16) -0.031(11) -0.002(10) -0.008(9) C34C 0.127(15) 0.099(12) 0.115(12) -0.040(10) 0.029(10) -0.070(11) N1D 0.103(12) 0.34(2) 0.207(16) -0.182(15) -0.002(11) -0.035(14) C33D 0.056(11) 0.26(2) 0.24(2) -0.058(17) -0.012(12) 0.065(13) C34D 0.125(15) 0.22(2) 0.092(11) -0.069(12) 0.026(10) -0.117(16) _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 S1A C5A 1.790(11) . ? S1A C1A 1.829(8) . ? S2A C6A 1.734(10) . ? S2A C2A 1.843(8) . ? S3A C5A 1.711(10) . ? S3A C7A 1.737(11) . ? S4A C6A 1.669(12) . ? S4A C7A 1.688(10) . ? S5A C8A 1.691(10) . ? S5A C9A 1.765(11) . ? S6A C10A 1.682(10) . ? S6A C8A 1.754(11) . ? S7A C9A 1.684(11) . ? S7A C11A 1.811(8) . ? S8A C10A 1.780(10) . ? S8A C12A 1.810(10) . ? C5A C6A 1.375(14) . ? C7A C8A 1.401(14) . ? C9A C10A 1.387(13) . ? C1A C2A 1.506(9) . ? C1A C3A 1.541(14) . ? C1A H1A 0.9800 . ? C2A C4A 1.537(12) . ? C2A H2A 0.9800 . ? C3A H3A1 0.9600 . ? C3A H3A2 0.9600 . ? C3A H3A3 0.9600 . ? C4A H4A1 0.9600 . ? C4A H4A2 0.9600 . ? C4A H4A3 0.9600 . ? C11A C12A 1.528(11) . ? C11A C13A 1.532(12) . ? C11A H11A 0.9800 . ? C12A C14A 1.524(16) . ? C12A H12A 0.9800 . ? C13A H13A 0.9600 . ? C13A H13B 0.9600 . ? C13A H13C 0.9600 . ? C14A H14A 0.9600 . ? C14A H14B 0.9600 . ? C14A H14C 0.9600 . ? P1A O1A 1.709(7) . ? P1A O3A 1.710(7) . ? P1A O5A 1.715(7) . ? P1A O2A 1.715(7) . ? P1A O4A 1.726(8) . ? P1A O6A 1.733(7) . ? O1A C15A 1.341(12) . ? O2A C16A 1.362(10) . ? O3A C21A 1.353(12) . ? O4A C22A 1.397(12) . ? O5A C27A 1.321(11) . ? O6A C28A 1.354(11) . ? Cl1 C17A 1.712(11) . ? Cl2 C18A 1.681(11) . ? Cl3 C19A 1.763(10) . ? Cl4 C20A 1.701(12) . ? Cl5 C23A 1.714(13) . ? Cl6 C24A 1.754(10) . ? Cl7 C25A 1.744(10) . ? Cl8 C26A 1.732(13) . ? Cl9 C29A 1.719(11) . ? Cl10 C30A 1.743(10) . ? Cl11 C31A 1.712(11) . ? Cl12 C32A 1.707(11) . ? C15A C16A 1.369(14) . ? C15A C20A 1.384(13) . ? C16A C17A 1.383(14) . ? C17A C18A 1.426(13) . ? C18A C19A 1.399(17) . ? C19A C20A 1.406(16) . ? C21A C22A 1.327(15) . ? C21A C26A 1.402(14) . ? C22A C23A 1.391(14) . ? C23A C24A 1.418(16) . ? C24A C25A 1.359(16) . ? C25A C26A 1.351(15) . ? C27A C28A 1.396(14) . ? C27A C32A 1.418(13) . ? C28A C29A 1.356(13) . ? C29A C30A 1.403(14) . ? C30A C31A 1.406(15) . ? C31A C32A 1.384(13) . ? S1B C5B 1.707(12) . ? S1B C1B 1.837(9) . ? S2B C6B 1.782(9) . ? S2B C2B 1.830(8) . ? S3B C7B 1.691(11) . ? S3B C5B 1.777(9) . ? S4B C6B 1.698(11) . ? S4B C7B 1.749(9) . ? S5B C8B 1.744(9) . ? S5B C9B 1.791(11) . ? S6B C8B 1.735(11) . ? S6B C10B 1.773(10) . ? S7B C9B 1.732(10) . ? S7B C11B 1.787(8) . ? S8B C10B 1.676(12) . ? S8B C12B 1.836(7) . ? C5B C6B 1.344(13) . ? C7B C8B 1.355(14) . ? C9B C10B 1.339(13) . ? C1B C2B 1.492(10) . ? C1B C3B 1.527(15) . ? C1B H1B 0.9800 . ? C2B C4B 1.511(11) . ? C2B H2B 0.9800 . ? C3B H3B1 0.9600 . ? C3B H3B2 0.9600 . ? C3B H3B3 0.9600 . ? C4B H4B1 0.9600 . ? C4B H4B2 0.9600 . ? C4B H4B3 0.9600 . ? C11B C13B 1.525(13) . ? C11B C12B 1.536(10) . ? C11B H11B 0.9800 . ? C12B C14B 1.515(14) . ? C12B H12B 0.9800 . ? C13B H13D 0.9600 . ? C13B H13E 0.9600 . ? C13B H13F 0.9600 . ? C14B H14D 0.9600 . ? C14B H14E 0.9600 . ? C14B H14F 0.9600 . ? P1B O4B 1.688(7) . ? P1B O3B 1.700(7) . ? P1B O5B 1.716(7) . ? P1B O6B 1.723(7) . ? P1B O1B 1.729(7) . ? P1B O2B 1.740(7) . ? O1B C15B 1.344(11) . ? O2B C16B 1.349(11) . ? O3B C21B 1.380(11) . ? O4B C22B 1.343(11) . ? O5B C27B 1.317(12) . ? O6B C28B 1.356(11) . ? Cl13 C17B 1.736(11) . ? Cl14 C18B 1.714(10) . ? Cl15 C19B 1.775(10) . ? Cl16 C20B 1.724(11) . ? Cl17 C23B 1.733(10) . ? Cl18 C24B 1.721(10) . ? Cl19 C25B 1.742(10) . ? Cl20 C26B 1.728(10) . ? Cl21 C29B 1.701(13) . ? Cl22 C30B 1.714(12) . ? Cl23 C31B 1.695(12) . ? Cl24 C32B 1.720(14) . ? C15B C20B 1.368(14) . ? C15B C16B 1.403(14) . ? C16B C17B 1.368(13) . ? C17B C18B 1.382(14) . ? C18B C19B 1.385(15) . ? C19B C20B 1.355(13) . ? C21B C26B 1.329(13) . ? C21B C22B 1.384(14) . ? C22B C23B 1.397(13) . ? C23B C24B 1.393(14) . ? C24B C25B 1.354(14) . ? C25B C26B 1.417(13) . ? C28B C29B 1.342(14) . ? C28B C27B 1.433(15) . ? C27B C32B 1.373(14) . ? C29B C30B 1.475(15) . ? C30B C31B 1.413(17) . ? C31B C32B 1.378(16) . ? N1A C34A 1.117(14) . ? C33A C34A 1.388(17) . ? C33A H33A 0.9600 . ? C33A H33B 0.9600 . ? C33A H33C 0.9600 . ? N1B C34B 1.086(15) . ? C33B C34B 1.432(17) . ? C33B H33D 0.9600 . ? C33B H33E 0.9600 . ? C33B H33F 0.9600 . ? N1C C34C 1.15(2) . ? C33C C34C 1.42(2) . ? C33C H33G 0.9600 . ? C33C H33H 0.9600 . ? C33C H33I 0.9600 . ? N1D C34D 1.08(2) . ? C33D C34D 1.40(2) . ? C33D H33J 0.9600 . ? C33D H33K 0.9600 . ? C33D H33L 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 C5A S1A C1A 101.3(4) . . ? C6A S2A C2A 104.7(5) . . ? C5A S3A C7A 92.8(5) . . ? C6A S4A C7A 96.0(5) . . ? C8A S5A C9A 97.6(5) . . ? C10A S6A C8A 94.9(5) . . ? C9A S7A C11A 104.8(5) . . ? C10A S8A C12A 103.7(5) . . ? C6A C5A S3A 117.9(8) . . ? C6A C5A S1A 127.7(8) . . ? S3A C5A S1A 114.2(6) . . ? C5A C6A S4A 116.3(8) . . ? C5A C6A S2A 126.6(9) . . ? S4A C6A S2A 117.0(6) . . ? C8A C7A S4A 124.4(8) . . ? C8A C7A S3A 118.7(7) . . ? S4A C7A S3A 116.8(6) . . ? C7A C8A S5A 125.4(8) . . ? C7A C8A S6A 119.5(8) . . ? S5A C8A S6A 115.0(7) . . ? C10A C9A S7A 133.0(8) . . ? C10A C9A S5A 111.7(7) . . ? S7A C9A S5A 115.2(6) . . ? C9A C10A S6A 120.7(8) . . ? C9A C10A S8A 121.6(8) . . ? S6A C10A S8A 117.6(5) . . ? C2A C1A C3A 109.5(7) . . ? C2A C1A S1A 112.1(5) . . ? C3A C1A S1A 106.9(6) . . ? C2A C1A H1A 109.4 . . ? C3A C1A H1A 109.4 . . ? S1A C1A H1A 109.4 . . ? C1A C2A C4A 115.9(6) . . ? C1A C2A S2A 112.9(5) . . ? C4A C2A S2A 102.7(6) . . ? C1A C2A H2A 108.3 . . ? C4A C2A H2A 108.3 . . ? S2A C2A H2A 108.3 . . ? C1A C3A H3A1 109.5 . . ? C1A C3A H3A2 109.5 . . ? H3A1 C3A H3A2 109.5 . . ? C1A C3A H3A3 109.5 . . ? H3A1 C3A H3A3 109.5 . . ? H3A2 C3A H3A3 109.5 . . ? C2A C4A H4A1 109.5 . . ? C2A C4A H4A2 109.5 . . ? H4A1 C4A H4A2 109.5 . . ? C2A C4A H4A3 109.5 . . ? H4A1 C4A H4A3 109.5 . . ? H4A2 C4A H4A3 109.5 . . ? C12A C11A C13A 113.4(8) . . ? C12A C11A S7A 114.3(6) . . ? C13A C11A S7A 104.3(6) . . ? C12A C11A H11A 108.2 . . ? C13A C11A H11A 108.2 . . ? S7A C11A H11A 108.2 . . ? C14A C12A C11A 111.6(8) . . ? C14A C12A S8A 105.0(8) . . ? C11A C12A S8A 114.0(6) . . ? C14A C12A H12A 108.7 . . ? C11A C12A H12A 108.7 . . ? S8A C12A H12A 108.7 . . ? C11A C13A H13A 109.5 . . ? C11A C13A H13B 109.5 . . ? H13A C13A H13B 109.5 . . ? C11A C13A H13C 109.5 . . ? H13A C13A H13C 109.5 . . ? H13B C13A H13C 109.5 . . ? C12A C14A H14A 109.5 . . ? C12A C14A H14B 109.5 . . ? H14A C14A H14B 109.5 . . ? C12A C14A H14C 109.5 . . ? H14A C14A H14C 109.5 . . ? H14B C14A H14C 109.5 . . ? O1A P1A O3A 87.7(3) . . ? O1A P1A O5A 87.8(3) . . ? O3A P1A O5A 88.5(4) . . ? O1A P1A O2A 91.3(3) . . ? O3A P1A O2A 177.7(4) . . ? O5A P1A O2A 93.4(3) . . ? O1A P1A O4A 92.7(3) . . ? O3A P1A O4A 91.1(3) . . ? O5A P1A O4A 179.4(4) . . ? O2A P1A O4A 86.9(4) . . ? O1A P1A O6A 178.4(3) . . ? O3A P1A O6A 93.5(3) . . ? O5A P1A O6A 91.1(3) . . ? O2A P1A O6A 87.6(3) . . ? O4A P1A O6A 88.4(3) . . ? C15A O1A P1A 110.5(6) . . ? C16A O2A P1A 110.7(6) . . ? C21A O3A P1A 111.3(7) . . ? C22A O4A P1A 109.1(7) . . ? C27A O5A P1A 110.5(6) . . ? C28A O6A P1A 110.5(6) . . ? O1A C15A C16A 114.7(8) . . ? O1A C15A C20A 126.4(10) . . ? C16A C15A C20A 118.8(10) . . ? O2A C16A C15A 112.3(9) . . ? O2A C16A C17A 123.4(10) . . ? C15A C16A C17A 124.2(9) . . ? C16A C17A C18A 118.4(10) . . ? C16A C17A Cl1 121.2(8) . . ? C18A C17A Cl1 120.3(9) . . ? C19A C18A C17A 116.7(10) . . ? C19A C18A Cl2 123.0(8) . . ? C17A C18A Cl2 120.2(9) . . ? C18A C19A C20A 123.3(9) . . ? C18A C19A Cl3 117.8(9) . . ? C20A C19A Cl3 118.9(9) . . ? C15A C20A C19A 118.4(10) . . ? C15A C20A Cl4 120.2(9) . . ? C19A C20A Cl4 121.4(8) . . ? C22A C21A O3A 114.4(9) . . ? C22A C21A C26A 119.5(11) . . ? O3A C21A C26A 126.0(12) . . ? C21A C22A C23A 124.0(10) . . ? C21A C22A O4A 114.0(9) . . ? C23A C22A O4A 121.9(11) . . ? C22A C23A C24A 114.8(11) . . ? C22A C23A Cl5 120.9(9) . . ? C24A C23A Cl5 124.3(9) . . ? C25A C24A C23A 121.3(10) . . ? C25A C24A Cl6 122.6(9) . . ? C23A C24A Cl6 116.1(10) . . ? C26A C25A C24A 121.2(10) . . ? C26A C25A Cl7 120.6(10) . . ? C24A C25A Cl7 118.2(9) . . ? C25A C26A C21A 119.0(12) . . ? C25A C26A Cl8 121.8(9) . . ? C21A C26A Cl8 119.2(9) . . ? O5A C27A C28A 115.2(9) . . ? O5A C27A C32A 125.7(9) . . ? C28A C27A C32A 119.0(9) . . ? O6A C28A C29A 125.6(10) . . ? O6A C28A C27A 111.8(9) . . ? C29A C28A C27A 122.6(10) . . ? C28A C29A C30A 118.3(9) . . ? C28A C29A Cl9 120.2(8) . . ? C30A C29A Cl9 121.5(8) . . ? C29A C30A C31A 120.9(9) . . ? C29A C30A Cl10 118.9(8) . . ? C31A C30A Cl10 120.1(8) . . ? C32A C31A C30A 119.8(10) . . ? C32A C31A Cl11 119.5(8) . . ? C30A C31A Cl11 120.7(8) . . ? C31A C32A C27A 119.2(9) . . ? C31A C32A Cl12 122.2(8) . . ? C27A C32A Cl12 118.6(7) . . ? C5B S1B C1B 103.2(5) . . ? C6B S2B C2B 100.5(4) . . ? C7B S3B C5B 96.2(5) . . ? C6B S4B C7B 93.5(5) . . ? C8B S5B C9B 95.4(5) . . ? C8B S6B C10B 98.0(5) . . ? C9B S7B C11B 99.8(4) . . ? C10B S8B C12B 103.0(5) . . ? C6B C5B S1B 133.5(8) . . ? C6B C5B S3B 112.4(8) . . ? S1B C5B S3B 114.1(6) . . ? C5B C6B S4B 121.7(7) . . ? C5B C6B S2B 122.5(8) . . ? S4B C6B S2B 115.7(5) . . ? C8B C7B S3B 124.1(7) . . ? C8B C7B S4B 119.7(8) . . ? S3B C7B S4B 116.2(6) . . ? C7B C8B S6B 126.0(7) . . ? C7B C8B S5B 120.1(8) . . ? S6B C8B S5B 113.9(6) . . ? C10B C9B S7B 130.2(8) . . ? C10B C9B S5B 118.2(7) . . ? S7B C9B S5B 111.4(6) . . ? C9B C10B S8B 128.7(8) . . ? C9B C10B S6B 114.3(9) . . ? S8B C10B S6B 117.0(6) . . ? C2B C1B C3B 114.7(8) . . ? C2B C1B S1B 115.1(6) . . ? C3B C1B S1B 102.6(7) . . ? C2B C1B H1B 108.0 . . ? C3B C1B H1B 108.0 . . ? S1B C1B H1B 108.0 . . ? C1B C2B C4B 114.0(7) . . ? C1B C2B S2B 113.3(6) . . ? C4B C2B S2B 104.8(6) . . ? C1B C2B H2B 108.2 . . ? C4B C2B H2B 108.2 . . ? S2B C2B H2B 108.2 . . ? C1B C3B H3B1 109.5 . . ? C1B C3B H3B2 109.5 . . ? H3B1 C3B H3B2 109.5 . . ? C1B C3B H3B3 109.5 . . ? H3B1 C3B H3B3 109.5 . . ? H3B2 C3B H3B3 109.5 . . ? C2B C4B H4B1 109.5 . . ? C2B C4B H4B2 109.5 . . ? H4B1 C4B H4B2 109.5 . . ? C2B C4B H4B3 109.5 . . ? H4B1 C4B H4B3 109.5 . . ? H4B2 C4B H4B3 109.5 . . ? C13B C11B C12B 111.5(8) . . ? C13B C11B S7B 105.1(7) . . ? C12B C11B S7B 114.2(5) . . ? C13B C11B H11B 108.6 . . ? C12B C11B H11B 108.6 . . ? S7B C11B H11B 108.6 . . ? C14B C12B C11B 116.7(7) . . ? C14B C12B S8B 102.7(7) . . ? C11B C12B S8B 112.8(5) . . ? C14B C12B H12B 108.1 . . ? C11B C12B H12B 108.1 . . ? S8B C12B H12B 108.1 . . ? C11B C13B H13D 109.5 . . ? C11B C13B H13E 109.5 . . ? H13D C13B H13E 109.5 . . ? C11B C13B H13F 109.5 . . ? H13D C13B H13F 109.5 . . ? H13E C13B H13F 109.5 . . ? C12B C14B H14D 109.5 . . ? C12B C14B H14E 109.5 . . ? H14D C14B H14E 109.5 . . ? C12B C14B H14F 109.5 . . ? H14D C14B H14F 109.5 . . ? H14E C14B H14F 109.5 . . ? O4B P1B O3B 90.7(3) . . ? O4B P1B O5B 88.6(3) . . ? O3B P1B O5B 179.2(4) . . ? O4B P1B O6B 93.3(3) . . ? O3B P1B O6B 89.2(4) . . ? O5B P1B O6B 90.3(4) . . ? O4B P1B O1B 88.2(3) . . ? O3B P1B O1B 92.6(3) . . ? O5B P1B O1B 88.0(4) . . ? O6B P1B O1B 177.6(4) . . ? O4B P1B O2B 176.8(3) . . ? O3B P1B O2B 87.2(3) . . ? O5B P1B O2B 93.5(3) . . ? O6B P1B O2B 89.0(3) . . ? O1B P1B O2B 89.5(3) . . ? C15B O1B P1B 112.5(6) . . ? C16B O2B P1B 112.4(6) . . ? C21B O3B P1B 111.9(6) . . ? C22B O4B P1B 112.1(6) . . ? C27B O5B P1B 113.3(8) . . ? C28B O6B P1B 112.2(7) . . ? O1B C15B C20B 127.8(9) . . ? O1B C15B C16B 113.2(9) . . ? C20B C15B C16B 119.0(9) . . ? O2B C16B C17B 126.2(10) . . ? O2B C16B C15B 112.1(8) . . ? C17B C16B C15B 121.7(10) . . ? C16B C17B C18B 119.1(10) . . ? C16B C17B Cl13 118.0(9) . . ? C18B C17B Cl13 122.7(8) . . ? C17B C18B C19B 118.0(9) . . ? C17B C18B Cl14 120.6(8) . . ? C19B C18B Cl14 121.4(8) . . ? C20B C19B C18B 123.6(10) . . ? C20B C19B Cl15 118.7(9) . . ? C18B C19B Cl15 117.6(8) . . ? C19B C20B C15B 118.6(10) . . ? C19B C20B Cl16 123.2(8) . . ? C15B C20B Cl16 118.2(7) . . ? C26B C21B O3B 125.2(9) . . ? C26B C21B C22B 124.0(9) . . ? O3B C21B C22B 110.7(9) . . ? O4B C22B C21B 113.7(8) . . ? O4B C22B C23B 128.1(9) . . ? C21B C22B C23B 118.3(10) . . ? C24B C23B C22B 118.9(9) . . ? C24B C23B Cl17 122.7(8) . . ? C22B C23B Cl17 118.4(9) . . ? C25B C24B C23B 120.5(9) . . ? C25B C24B Cl18 120.2(8) . . ? C23B C24B Cl18 119.2(8) . . ? C24B C25B C26B 121.0(9) . . ? C24B C25B Cl19 120.7(8) . . ? C26B C25B Cl19 118.3(8) . . ? C21B C26B C25B 117.3(9) . . ? C21B C26B Cl20 120.7(8) . . ? C25B C26B Cl20 121.9(8) . . ? C29B C28B O6B 125.7(11) . . ? C29B C28B C27B 122.8(10) . . ? O6B C28B C27B 111.4(9) . . ? O5B C27B C32B 127.8(12) . . ? O5B C27B C28B 112.8(10) . . ? C32B C27B C28B 119.3(10) . . ? C28B C29B C30B 116.9(12) . . ? C28B C29B Cl21 121.8(9) . . ? C30B C29B Cl21 121.3(9) . . ? C31B C30B C29B 120.0(10) . . ? C31B C30B Cl22 122.5(9) . . ? C29B C30B Cl22 117.4(11) . . ? C32B C31B C30B 119.6(11) . . ? C32B C31B Cl23 123.1(12) . . ? C30B C31B Cl23 117.2(10) . . ? C27B C32B C31B 121.2(12) . . ? C27B C32B Cl24 118.9(9) . . ? C31B C32B Cl24 119.9(10) . . ? C34A C33A H33A 109.5 . . ? C34A C33A H33B 109.5 . . ? H33A C33A H33B 109.5 . . ? C34A C33A H33C 109.5 . . ? H33A C33A H33C 109.5 . . ? H33B C33A H33C 109.5 . . ? N1A C34A C33A 168.3(18) . . ? C34B C33B H33D 109.5 . . ? C34B C33B H33E 109.5 . . ? H33D C33B H33E 109.5 . . ? C34B C33B H33F 109.5 . . ? H33D C33B H33F 109.5 . . ? H33E C33B H33F 109.5 . . ? N1B C34B C33B 173.3(15) . . ? C34C C33C H33G 109.5 . . ? C34C C33C H33H 109.5 . . ? H33G C33C H33H 109.5 . . ? C34C C33C H33I 109.5 . . ? H33G C33C H33I 109.5 . . ? H33H C33C H33I 109.5 . . ? N1C C34C C33C 172.2(18) . . ? C34D C33D H33J 109.5 . . ? C34D C33D H33K 109.5 . . ? H33J C33D H33K 109.5 . . ? C34D C33D H33L 109.5 . . ? H33J C33D H33L 109.5 . . ? H33K C33D H33L 109.5 . . ? N1D C34D C33D 162(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.449 _refine_diff_density_min -0.437 _refine_diff_density_rms 0.070