# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_section_title ;Isolation and x-ray structural characterization of tetraisopropylpyrene cation radica ; _publ_contact_author_name 'Prof. Rajendra Rathore' _publ_contact_author_email RAJENDRA.RATHORE@MARQUETTE.EDU loop_ _publ_author_name R.Rathore M.Banerjee S.V.Lindeman V.S.Vyas # Attachment 'raj0k4.cif' data_raj0k4 _database_code_depnum_ccdc_archive 'CCDC 674750' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H34' _chemical_formula_weight 370.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3272(7) _cell_length_b 12.6764(7) _cell_length_c 16.9660(12) _cell_angle_alpha 94.595(4) _cell_angle_beta 92.311(4) _cell_angle_gamma 115.064(3) _cell_volume 2192.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 3102 _cell_measurement_theta_min 4 _cell_measurement_theta_max 64 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.123 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 0.463 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9130 _exptl_absorpt_correction_T_max 0.9727 _exptl_absorpt_process_details ; SADABS. Program for empirical absorption correction of area-detector data. University of Goetingen. Germany. Sheldrick, G. M. 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX2 CCD detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25845 _diffrn_reflns_av_R_equivalents 0.0397 _diffrn_reflns_av_sigmaI/netI 0.0460 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 67.24 _reflns_number_total 7547 _reflns_number_gt 5047 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2.1-4 (Bruker, 2007)' _computing_cell_refinement 'SAINT v7.23A (Bruker, 2005)' _computing_data_reduction 'TWINABS-2007/5 (Bruker, 2007)' _computing_structure_solution 'XS/SHELXTL v6.12 (Bruker, 2001)' _computing_structure_refinement 'SHELXL-97 v.97-2 (Sheldrick, 1993-1997)' _computing_molecular_graphics 'XP v5.1 (Bruker, 1998)' _computing_publication_material 'XCIF v6.12 (Bruker, 2001)' _refine_special_details ; Non-merohedral twin with 2 non-equal components rotated 180 deg about reciprocal z. Phase transition below 200K. ; _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^)+(0.1048P)^2^+0.3545P] 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 SHELXL _refine_ls_extinction_coef 0.0007(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7547 _refine_ls_number_parameters 506 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0981 _refine_ls_R_factor_gt 0.0644 _refine_ls_wR_factor_ref 0.1900 _refine_ls_wR_factor_gt 0.1740 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.000 _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 0.38483(19) 0.37211(18) 0.74743(11) 0.0290(5) Uani 1 1 d . . . C2 C 0.2939(2) 0.34418(19) 0.80640(12) 0.0299(5) Uani 1 1 d . . . C3 C 0.1956(2) 0.22894(19) 0.80561(12) 0.0323(5) Uani 1 1 d . . . C4 C 0.1911(2) 0.14568(19) 0.74548(13) 0.0350(5) Uani 1 1 d . . . H4 H 0.1247 0.0682 0.7448 0.042 Uiso 1 1 calc R . . C5 C 0.2770(2) 0.16845(19) 0.68666(13) 0.0347(5) Uani 1 1 d . . . C6 C 0.3764(2) 0.28334(18) 0.68682(12) 0.0306(5) Uani 1 1 d . . . C7 C 0.4700(2) 0.31551(19) 0.62853(12) 0.0343(5) Uani 1 1 d . . . H7 H 0.4645 0.2580 0.5872 0.041 Uiso 1 1 calc R . . C8 C 0.5654(2) 0.42470(19) 0.63054(13) 0.0346(5) Uani 1 1 d . . . H8 H 0.6254 0.4418 0.5907 0.042 Uiso 1 1 calc R . . C9 C 0.48637(19) 0.48939(18) 0.74834(11) 0.0292(5) Uani 1 1 d . . . C10 C 0.5796(2) 0.51625(19) 0.69066(12) 0.0316(5) Uani 1 1 d . . . C11 C 0.6813(2) 0.6304(2) 0.69415(13) 0.0351(5) Uani 1 1 d . . . C12 C 0.6836(2) 0.7152(2) 0.75269(13) 0.0370(5) Uani 1 1 d . . . H12 H 0.7511 0.7923 0.7541 0.044 Uiso 1 1 calc R . . C13 C 0.5929(2) 0.69346(19) 0.80885(13) 0.0346(5) Uani 1 1 d . . . C14 C 0.4940(2) 0.57889(19) 0.80809(12) 0.0313(5) Uani 1 1 d . . . C15 C 0.4002(2) 0.5466(2) 0.86630(13) 0.0350(5) Uani 1 1 d . . . H15 H 0.4042 0.6048 0.9066 0.042 Uiso 1 1 calc R . . C16 C 0.3063(2) 0.4365(2) 0.86585(13) 0.0359(5) Uani 1 1 d . . . H16 H 0.2468 0.4195 0.9060 0.043 Uiso 1 1 calc R . . C17 C 0.0948(2) 0.1961(2) 0.86655(13) 0.0362(5) Uani 1 1 d . . . H17 H 0.1379 0.2476 0.9168 0.043 Uiso 1 1 calc R . . C18 C 0.0465(2) 0.0703(2) 0.88560(14) 0.0455(6) Uani 1 1 d . . . H18A H -0.0174 0.0555 0.9255 0.068 Uiso 1 1 calc R . . H18B H 0.1205 0.0571 0.9064 0.068 Uiso 1 1 calc R . . H18C H 0.0051 0.0170 0.8373 0.068 Uiso 1 1 calc R . . C19 C -0.0192(2) 0.2231(3) 0.84001(16) 0.0524(7) Uani 1 1 d . . . H19A H 0.0146 0.3048 0.8285 0.079 Uiso 1 1 calc R . . H19B H -0.0786 0.2105 0.8824 0.079 Uiso 1 1 calc R . . H19C H -0.0666 0.1713 0.7921 0.079 Uiso 1 1 calc R . . C20 C 0.2610(2) 0.0691(2) 0.62458(13) 0.0410(6) Uani 1 1 d . . . H20 H 0.3352 0.0993 0.5900 0.049 Uiso 1 1 calc R . . C21 C 0.2663(3) -0.0337(2) 0.66159(15) 0.0491(6) Uani 1 1 d . . . H21A H 0.2549 -0.0959 0.6197 0.074 Uiso 1 1 calc R . . H21B H 0.1962 -0.0633 0.6973 0.074 Uiso 1 1 calc R . . H21C H 0.3511 -0.0084 0.6917 0.074 Uiso 1 1 calc R . . C22 C 0.1335(3) 0.0289(2) 0.57190(16) 0.0614(8) Uani 1 1 d . . . H22A H 0.1253 -0.0351 0.5324 0.092 Uiso 1 1 calc R . . H22B H 0.1342 0.0946 0.5448 0.092 Uiso 1 1 calc R . . H22C H 0.0592 0.0016 0.6047 0.092 Uiso 1 1 calc R . . C23 C 0.7834(2) 0.6639(2) 0.63396(14) 0.0420(6) Uani 1 1 d . . . H23 H 0.7812 0.5892 0.6084 0.050 Uiso 1 1 calc R . . C24 C 0.7476(4) 0.7221(3) 0.5692(2) 0.0926(13) Uani 1 1 d . . . H24A H 0.8140 0.7423 0.5308 0.139 Uiso 1 1 calc R . . H24B H 0.7430 0.7936 0.5923 0.139 Uiso 1 1 calc R . . H24C H 0.6623 0.6685 0.5424 0.139 Uiso 1 1 calc R . . C25 C 0.9213(3) 0.7356(3) 0.6723(2) 0.0918(13) Uani 1 1 d . . . H25A H 0.9834 0.7543 0.6312 0.138 Uiso 1 1 calc R . . H25B H 0.9427 0.6904 0.7100 0.138 Uiso 1 1 calc R . . H25C H 0.9268 0.8084 0.7003 0.138 Uiso 1 1 calc R . . C26 C 0.6051(2) 0.7905(2) 0.87214(14) 0.0407(6) Uani 1 1 d . . . H26 H 0.5156 0.7720 0.8892 0.049 Uiso 1 1 calc R . . C27 C 0.6898(3) 0.7911(3) 0.94450(16) 0.0661(8) Uani 1 1 d . . . H27A H 0.6968 0.8535 0.9851 0.099 Uiso 1 1 calc R . . H27B H 0.7772 0.8049 0.9290 0.099 Uiso 1 1 calc R . . H27C H 0.6498 0.7153 0.9659 0.099 Uiso 1 1 calc R . . C28 C 0.6577(3) 0.9121(2) 0.84285(18) 0.0615(8) Uani 1 1 d . . . H28A H 0.6626 0.9701 0.8862 0.092 Uiso 1 1 calc R . . H28B H 0.5990 0.9117 0.7987 0.092 Uiso 1 1 calc R . . H28C H 0.7451 0.9324 0.8249 0.092 Uiso 1 1 calc R . . C1A C 0.45222(19) 0.93974(18) 0.49805(12) 0.0284(5) Uani 1 1 d . . . C2A C 0.4627(2) 0.86722(18) 0.55569(12) 0.0303(5) Uani 1 1 d . . . C3A C 0.3660(2) 0.75036(19) 0.55356(12) 0.0328(5) Uani 1 1 d . . . C4A C 0.2646(2) 0.71007(19) 0.49404(13) 0.0338(5) Uani 1 1 d . . . H4A H 0.1994 0.6320 0.4932 0.041 Uiso 1 1 calc R . . C5A C 0.2524(2) 0.77647(19) 0.43558(12) 0.0315(5) Uani 1 1 d . . . C6A C 0.3467(2) 0.89332(18) 0.43758(12) 0.0307(5) Uani 1 1 d . . . C7A C 0.3410(2) 0.9702(2) 0.38120(13) 0.0370(5) Uani 1 1 d . . . H7A H 0.2718 0.9408 0.3402 0.044 Uiso 1 1 calc R . . C8A C 0.4304(2) 1.0827(2) 0.38452(13) 0.0358(5) Uani 1 1 d . . . H8A H 0.4221 1.1300 0.3460 0.043 Uiso 1 1 calc R . . C17A C 0.3662(2) 0.6722(2) 0.61767(13) 0.0366(5) Uani 1 1 d . . . H17A H 0.4595 0.6935 0.6353 0.044 Uiso 1 1 calc R . . C18A C 0.3019(3) 0.6975(3) 0.68959(15) 0.0586(8) Uani 1 1 d . . . H18D H 0.3027 0.6472 0.7303 0.088 Uiso 1 1 calc R . . H18E H 0.2113 0.6817 0.6736 0.088 Uiso 1 1 calc R . . H18F H 0.3503 0.7799 0.7110 0.088 Uiso 1 1 calc R . . C19A C 0.3022(3) 0.5420(2) 0.58909(16) 0.0551(7) Uani 1 1 d . . . H19D H 0.3446 0.5271 0.5430 0.083 Uiso 1 1 calc R . . H19E H 0.2092 0.5172 0.5741 0.083 Uiso 1 1 calc R . . H19F H 0.3118 0.4978 0.6318 0.083 Uiso 1 1 calc R . . C20A C 0.1373(2) 0.72390(19) 0.37273(13) 0.0364(5) Uani 1 1 d . . . H20A H 0.1689 0.7599 0.3229 0.044 Uiso 1 1 calc R . . C21A C 0.0839(2) 0.5918(2) 0.35335(15) 0.0474(6) Uani 1 1 d . . . H21D H 0.0110 0.5648 0.3123 0.071 Uiso 1 1 calc R . . H21E H 0.0531 0.5535 0.4012 0.071 Uiso 1 1 calc R . . H21F H 0.1532 0.5721 0.3341 0.071 Uiso 1 1 calc R . . C22A C 0.0277(2) 0.7573(2) 0.39649(16) 0.0538(7) Uani 1 1 d . . . H22D H -0.0455 0.7229 0.3554 0.081 Uiso 1 1 calc R . . H22E H 0.0605 0.8427 0.4022 0.081 Uiso 1 1 calc R . . H22F H -0.0021 0.7275 0.4471 0.081 Uiso 1 1 calc R . . C1B C 0.54837(19) 0.05983(18) -0.00008(12) 0.0296(5) Uani 1 1 d . . . C2B C 0.6569(2) 0.10797(19) 0.05823(12) 0.0308(5) Uani 1 1 d . . . C3B C 0.7515(2) 0.22422(19) 0.05728(12) 0.0317(5) Uani 1 1 d . . . C4B C 0.7348(2) 0.28890(19) -0.00089(12) 0.0333(5) Uani 1 1 d . . . H4B H 0.7990 0.3671 -0.0015 0.040 Uiso 1 1 calc R . . C5B C 0.6300(2) 0.24622(19) -0.05825(12) 0.0322(5) Uani 1 1 d . . . C6B C 0.5350(2) 0.12984(19) -0.05841(12) 0.0306(5) Uani 1 1 d . . . C7B C 0.4246(2) 0.0773(2) -0.11614(13) 0.0351(5) Uani 1 1 d . . . H7B H 0.4145 0.1224 -0.1558 0.042 Uiso 1 1 calc R . . C8B C 0.6650(2) 0.0338(2) 0.11574(13) 0.0358(5) Uani 1 1 d . . . H8B H 0.7366 0.0645 0.1551 0.043 Uiso 1 1 calc R . . C17B C 0.8724(2) 0.2774(2) 0.11588(13) 0.0362(5) Uani 1 1 d . . . H17B H 0.8470 0.2414 0.1665 0.043 Uiso 1 1 calc R . . C18B C 0.9790(2) 0.2449(2) 0.08564(16) 0.0499(6) Uani 1 1 d . . . H18G H 1.0563 0.2796 0.1237 0.075 Uiso 1 1 calc R . . H18H H 1.0023 0.2747 0.0342 0.075 Uiso 1 1 calc R . . H18I H 0.9468 0.1595 0.0796 0.075 Uiso 1 1 calc R . . C19B C 0.9268(2) 0.4098(2) 0.13544(15) 0.0461(6) Uani 1 1 d . . . H19G H 1.0037 0.4370 0.1735 0.069 Uiso 1 1 calc R . . H19H H 0.8599 0.4295 0.1586 0.069 Uiso 1 1 calc R . . H19I H 0.9517 0.4478 0.0868 0.069 Uiso 1 1 calc R . . C20B C 0.6215(2) 0.3220(2) -0.12153(13) 0.0371(5) Uani 1 1 d . . . H20B H 0.5268 0.3005 -0.1351 0.045 Uiso 1 1 calc R . . C21B C 0.6772(3) 0.2941(3) -0.19636(15) 0.0576(7) Uani 1 1 d . . . H21G H 0.6717 0.3431 -0.2369 0.086 Uiso 1 1 calc R . . H21H H 0.6269 0.2114 -0.2162 0.086 Uiso 1 1 calc R . . H21I H 0.7688 0.3100 -0.1842 0.086 Uiso 1 1 calc R . . C22B C 0.6885(3) 0.4534(2) -0.09447(17) 0.0547(7) Uani 1 1 d . . . H22G H 0.6790 0.4968 -0.1377 0.082 Uiso 1 1 calc R . . H22H H 0.7816 0.4770 -0.0802 0.082 Uiso 1 1 calc R . . H22I H 0.6479 0.4706 -0.0482 0.082 Uiso 1 1 calc R . . 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 0.0310(11) 0.0346(12) 0.0261(11) 0.0018(9) -0.0010(8) 0.0192(10) C2 0.0298(11) 0.0357(12) 0.0278(11) 0.0020(9) 0.0004(8) 0.0179(10) C3 0.0335(12) 0.0364(12) 0.0315(12) 0.0039(9) 0.0028(9) 0.0194(10) C4 0.0367(12) 0.0311(12) 0.0354(12) 0.0027(9) 0.0029(9) 0.0130(10) C5 0.0382(13) 0.0346(12) 0.0329(12) 0.0021(9) 0.0022(9) 0.0174(10) C6 0.0338(12) 0.0334(12) 0.0278(11) -0.0001(9) 0.0001(8) 0.0183(10) C7 0.0416(13) 0.0360(12) 0.0270(12) -0.0018(9) 0.0046(9) 0.0191(11) C8 0.0366(12) 0.0356(13) 0.0326(12) 0.0012(9) 0.0094(9) 0.0163(10) C9 0.0312(11) 0.0332(12) 0.0267(11) 0.0024(9) -0.0007(8) 0.0177(10) C10 0.0322(12) 0.0365(12) 0.0303(12) 0.0023(9) 0.0015(8) 0.0190(10) C11 0.0330(12) 0.0378(13) 0.0364(13) 0.0010(10) 0.0028(9) 0.0176(10) C12 0.0343(12) 0.0319(12) 0.0415(13) -0.0006(10) 0.0009(9) 0.0120(10) C13 0.0327(12) 0.0386(13) 0.0347(12) -0.0033(10) -0.0012(9) 0.0191(10) C14 0.0314(12) 0.0348(12) 0.0309(12) -0.0005(9) -0.0006(8) 0.0181(10) C15 0.0363(12) 0.0352(12) 0.0339(12) -0.0064(9) 0.0035(9) 0.0174(10) C16 0.0387(13) 0.0404(13) 0.0322(12) 0.0020(10) 0.0091(9) 0.0203(11) C17 0.0380(13) 0.0401(13) 0.0325(12) 0.0035(10) 0.0058(9) 0.0186(11) C18 0.0525(15) 0.0462(14) 0.0417(14) 0.0120(11) 0.0138(11) 0.0228(12) C19 0.0436(15) 0.0689(18) 0.0563(16) 0.0201(14) 0.0173(12) 0.0317(14) C20 0.0462(14) 0.0344(13) 0.0378(13) -0.0009(10) 0.0116(10) 0.0130(11) C21 0.0570(16) 0.0463(15) 0.0526(16) -0.0047(12) -0.0003(12) 0.0326(13) C22 0.086(2) 0.0526(17) 0.0481(16) -0.0090(13) -0.0172(14) 0.0363(16) C23 0.0426(14) 0.0348(13) 0.0475(14) 0.0011(10) 0.0157(11) 0.0151(11) C24 0.127(3) 0.120(3) 0.086(2) 0.064(2) 0.069(2) 0.092(3) C25 0.0440(18) 0.102(3) 0.094(3) -0.025(2) 0.0301(17) 0.0014(17) C26 0.0352(13) 0.0395(13) 0.0447(14) -0.0075(10) 0.0034(10) 0.0155(11) C27 0.0648(19) 0.082(2) 0.0520(17) -0.0274(15) -0.0133(13) 0.0396(17) C28 0.0647(19) 0.0409(15) 0.0708(19) -0.0113(13) 0.0227(14) 0.0165(13) C1A 0.0281(11) 0.0340(12) 0.0279(11) 0.0047(9) 0.0062(8) 0.0174(9) C2A 0.0349(12) 0.0327(12) 0.0285(11) 0.0039(9) 0.0054(9) 0.0192(10) C3A 0.0339(12) 0.0371(12) 0.0329(12) 0.0071(10) 0.0075(9) 0.0197(10) C4A 0.0314(12) 0.0320(12) 0.0377(13) 0.0036(10) 0.0059(9) 0.0131(10) C5A 0.0335(12) 0.0349(12) 0.0294(12) 0.0039(9) 0.0052(9) 0.0173(10) C6A 0.0322(12) 0.0333(12) 0.0301(12) 0.0037(9) 0.0032(9) 0.0173(10) C7A 0.0341(12) 0.0416(14) 0.0351(13) 0.0066(10) -0.0028(9) 0.0163(11) C8A 0.0405(13) 0.0391(13) 0.0344(12) 0.0107(10) 0.0016(9) 0.0224(11) C17A 0.0338(12) 0.0377(13) 0.0405(13) 0.0114(10) 0.0032(9) 0.0161(10) C18A 0.0718(19) 0.077(2) 0.0487(16) 0.0305(14) 0.0217(13) 0.0466(16) C19A 0.0658(18) 0.0396(14) 0.0580(17) 0.0163(12) -0.0091(13) 0.0200(13) C20A 0.0369(13) 0.0368(13) 0.0348(13) 0.0018(10) 0.0013(9) 0.0157(10) C21A 0.0491(15) 0.0411(14) 0.0454(14) -0.0030(11) -0.0065(11) 0.0151(12) C22A 0.0415(15) 0.0623(17) 0.0582(17) -0.0071(13) -0.0070(12) 0.0263(13) C1B 0.0315(12) 0.0360(12) 0.0272(11) 0.0021(9) 0.0021(8) 0.0203(10) C2B 0.0300(11) 0.0400(13) 0.0274(11) 0.0018(9) 0.0028(8) 0.0202(10) C3B 0.0311(12) 0.0375(12) 0.0292(12) 0.0008(9) 0.0036(8) 0.0177(10) C4B 0.0310(12) 0.0340(12) 0.0365(12) 0.0039(10) 0.0042(9) 0.0153(10) C5B 0.0333(12) 0.0370(12) 0.0326(12) 0.0056(9) 0.0041(9) 0.0205(10) C6B 0.0331(12) 0.0371(12) 0.0264(11) 0.0026(9) 0.0023(8) 0.0196(10) C7B 0.0381(13) 0.0404(13) 0.0323(12) 0.0084(10) -0.0007(9) 0.0216(11) C8B 0.0338(12) 0.0457(14) 0.0294(12) 0.0035(10) -0.0038(9) 0.0193(11) C17B 0.0355(12) 0.0402(13) 0.0341(12) 0.0041(10) 0.0008(9) 0.0175(10) C18B 0.0411(14) 0.0517(16) 0.0574(16) -0.0046(12) -0.0046(11) 0.0228(12) C19B 0.0426(14) 0.0454(14) 0.0478(15) -0.0045(11) -0.0069(11) 0.0191(12) C20B 0.0348(12) 0.0421(13) 0.0375(13) 0.0119(10) 0.0017(9) 0.0183(11) C21B 0.0686(19) 0.079(2) 0.0417(15) 0.0238(14) 0.0150(13) 0.0436(16) C22B 0.0573(17) 0.0436(15) 0.0619(17) 0.0161(13) -0.0106(13) 0.0198(13) _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 1.421(3) . ? C1 C6 1.431(3) . ? C1 C9 1.442(3) . ? C2 C3 1.411(3) . ? C2 C16 1.437(3) . ? C3 C4 1.391(3) . ? C3 C17 1.519(3) . ? C4 C5 1.383(3) . ? C4 H4 0.9500 . ? C5 C6 1.414(3) . ? C5 C20 1.519(3) . ? C6 C7 1.432(3) . ? C7 C8 1.344(3) . ? C7 H7 0.9500 . ? C8 C10 1.432(3) . ? C8 H8 0.9500 . ? C9 C10 1.421(3) . ? C9 C14 1.431(3) . ? C10 C11 1.412(3) . ? C11 C12 1.395(3) . ? C11 C23 1.520(3) . ? C12 C13 1.385(3) . ? C12 H12 0.9500 . ? C13 C14 1.408(3) . ? C13 C26 1.522(3) . ? C14 C15 1.433(3) . ? C15 C16 1.348(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.518(3) . ? C17 C19 1.530(3) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.512(3) . ? C20 C22 1.532(4) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.505(4) . ? C23 C25 1.520(4) . ? C23 H23 1.0000 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.524(4) . ? C26 C28 1.532(4) . ? C26 H26 1.0000 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C1A C6A 1.427(3) . ? C1A C2A 1.429(3) . ? C1A C1A 1.445(4) 2_676 ? C2A C3A 1.417(3) . ? C2A C8A 1.430(3) 2_676 ? C3A C4A 1.388(3) . ? C3A C17A 1.529(3) . ? C4A C5A 1.390(3) . ? C4A H4A 0.9500 . ? C5A C6A 1.409(3) . ? C5A C20A 1.523(3) . ? C6A C7A 1.437(3) . ? C7A C8A 1.350(3) . ? C7A H7A 0.9500 . ? C8A C2A 1.430(3) 2_676 ? C8A H8A 0.9500 . ? C17A C19A 1.522(3) . ? C17A C18A 1.526(3) . ? C17A H17A 1.0000 . ? C18A H18D 0.9800 . ? C18A H18E 0.9800 . ? C18A H18F 0.9800 . ? C19A H19D 0.9800 . ? C19A H19E 0.9800 . ? C19A H19F 0.9800 . ? C20A C21A 1.522(3) . ? C20A C22A 1.530(3) . ? C20A H20A 1.0000 . ? C21A H21D 0.9800 . ? C21A H21E 0.9800 . ? C21A H21F 0.9800 . ? C22A H22D 0.9800 . ? C22A H22E 0.9800 . ? C22A H22F 0.9800 . ? C1B C6B 1.426(3) . ? C1B C2B 1.426(3) . ? C1B C1B 1.447(4) 2_655 ? C2B C3B 1.409(3) . ? C2B C8B 1.434(3) . ? C3B C4B 1.388(3) . ? C3B C17B 1.523(3) . ? C4B C5B 1.388(3) . ? C4B H4B 0.9500 . ? C5B C6B 1.410(3) . ? C5B C20B 1.523(3) . ? C6B C7B 1.435(3) . ? C7B C8B 1.344(3) 2_655 ? C7B H7B 0.9500 . ? C8B C7B 1.344(3) 2_655 ? C8B H8B 0.9500 . ? C17B C19B 1.525(3) . ? C17B C18B 1.526(3) . ? C17B H17B 1.0000 . ? C18B H18G 0.9800 . ? C18B H18H 0.9800 . ? C18B H18I 0.9800 . ? C19B H19G 0.9800 . ? C19B H19H 0.9800 . ? C19B H19I 0.9800 . ? C20B C21B 1.522(3) . ? C20B C22B 1.530(3) . ? C20B H20B 1.0000 . ? C21B H21G 0.9800 . ? C21B H21H 0.9800 . ? C21B H21I 0.9800 . ? C22B H22G 0.9800 . ? C22B H22H 0.9800 . ? C22B H22I 0.9800 . ? 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 C6 119.96(19) . . ? C2 C1 C9 120.47(18) . . ? C6 C1 C9 119.57(18) . . ? C3 C2 C1 120.16(19) . . ? C3 C2 C16 122.04(19) . . ? C1 C2 C16 117.80(19) . . ? C4 C3 C2 117.83(19) . . ? C4 C3 C17 120.4(2) . . ? C2 C3 C17 121.79(18) . . ? C5 C4 C3 124.2(2) . . ? C5 C4 H4 117.9 . . ? C3 C4 H4 117.9 . . ? C4 C5 C6 118.6(2) . . ? C4 C5 C20 118.7(2) . . ? C6 C5 C20 122.61(19) . . ? C5 C6 C1 119.16(19) . . ? C5 C6 C7 122.80(19) . . ? C1 C6 C7 118.04(19) . . ? C8 C7 C6 121.9(2) . . ? C8 C7 H7 119.0 . . ? C6 C7 H7 119.0 . . ? C7 C8 C10 122.29(19) . . ? C7 C8 H8 118.9 . . ? C10 C8 H8 118.9 . . ? C10 C9 C14 119.85(19) . . ? C10 C9 C1 120.34(18) . . ? C14 C9 C1 119.80(18) . . ? C11 C10 C9 119.64(19) . . ? C11 C10 C8 122.58(19) . . ? C9 C10 C8 117.79(19) . . ? C12 C11 C10 118.4(2) . . ? C12 C11 C23 119.7(2) . . ? C10 C11 C23 121.82(19) . . ? C13 C12 C11 123.7(2) . . ? C13 C12 H12 118.1 . . ? C11 C12 H12 118.1 . . ? C12 C13 C14 118.45(19) . . ? C12 C13 C26 120.2(2) . . ? C14 C13 C26 121.25(19) . . ? C13 C14 C9 119.81(19) . . ? C13 C14 C15 122.46(19) . . ? C9 C14 C15 117.72(19) . . ? C16 C15 C14 122.3(2) . . ? C16 C15 H15 118.8 . . ? C14 C15 H15 118.8 . . ? C15 C16 C2 121.9(2) . . ? C15 C16 H16 119.1 . . ? C2 C16 H16 119.1 . . ? C18 C17 C3 113.93(18) . . ? C18 C17 C19 111.1(2) . . ? C3 C17 C19 109.98(18) . . ? C18 C17 H17 107.1 . . ? C3 C17 H17 107.1 . . ? C19 C17 H17 107.1 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C5 112.01(19) . . ? C21 C20 C22 110.1(2) . . ? C5 C20 C22 111.0(2) . . ? C21 C20 H20 107.9 . . ? C5 C20 H20 107.9 . . ? C22 C20 H20 107.9 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C25 112.9(3) . . ? C24 C23 C11 110.7(2) . . ? C25 C23 C11 112.7(2) . . ? C24 C23 H23 106.7 . . ? C25 C23 H23 106.7 . . ? C11 C23 H23 106.7 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C13 C26 C27 109.90(19) . . ? C13 C26 C28 113.7(2) . . ? C27 C26 C28 110.5(2) . . ? C13 C26 H26 107.5 . . ? C27 C26 H26 107.5 . . ? C28 C26 H26 107.5 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C6A C1A C2A 119.92(19) . . ? C6A C1A C1A 120.3(2) . 2_676 ? C2A C1A C1A 119.8(2) . 2_676 ? C3A C2A C1A 119.6(2) . . ? C3A C2A C8A 122.19(19) . 2_676 ? C1A C2A C8A 118.1(2) . 2_676 ? C4A C3A C2A 118.06(19) . . ? C4A C3A C17A 120.0(2) . . ? C2A C3A C17A 121.8(2) . . ? C3A C4A C5A 124.3(2) . . ? C3A C4A H4A 117.9 . . ? C5A C4A H4A 117.9 . . ? C4A C5A C6A 118.3(2) . . ? C4A C5A C20A 120.2(2) . . ? C6A C5A C20A 121.48(18) . . ? C5A C6A C1A 119.76(19) . . ? C5A C6A C7A 122.7(2) . . ? C1A C6A C7A 117.56(19) . . ? C8A C7A C6A 122.2(2) . . ? C8A C7A H7A 118.9 . . ? C6A C7A H7A 118.9 . . ? C7A C8A C2A 122.0(2) . 2_676 ? C7A C8A H8A 119.0 . . ? C2A C8A H8A 119.0 2_676 . ? C19A C17A C18A 110.4(2) . . ? C19A C17A C3A 113.85(19) . . ? C18A C17A C3A 110.14(18) . . ? C19A C17A H17A 107.4 . . ? C18A C17A H17A 107.4 . . ? C3A C17A H17A 107.4 . . ? C17A C18A H18D 109.5 . . ? C17A C18A H18E 109.5 . . ? H18D C18A H18E 109.5 . . ? C17A C18A H18F 109.5 . . ? H18D C18A H18F 109.5 . . ? H18E C18A H18F 109.5 . . ? C17A C19A H19D 109.5 . . ? C17A C19A H19E 109.5 . . ? H19D C19A H19E 109.5 . . ? C17A C19A H19F 109.5 . . ? H19D C19A H19F 109.5 . . ? H19E C19A H19F 109.5 . . ? C21A C20A C5A 114.35(19) . . ? C21A C20A C22A 110.2(2) . . ? C5A C20A C22A 110.48(18) . . ? C21A C20A H20A 107.2 . . ? C5A C20A H20A 107.2 . . ? C22A C20A H20A 107.2 . . ? C20A C21A H21D 109.5 . . ? C20A C21A H21E 109.5 . . ? H21D C21A H21E 109.5 . . ? C20A C21A H21F 109.5 . . ? H21D C21A H21F 109.5 . . ? H21E C21A H21F 109.5 . . ? C20A C22A H22D 109.5 . . ? C20A C22A H22E 109.5 . . ? H22D C22A H22E 109.5 . . ? C20A C22A H22F 109.5 . . ? H22D C22A H22F 109.5 . . ? H22E C22A H22F 109.5 . . ? C6B C1B C2B 119.91(19) . . ? C6B C1B C1B 120.0(2) . 2_655 ? C2B C1B C1B 120.1(2) . 2_655 ? C3B C2B C1B 119.77(19) . . ? C3B C2B C8B 122.70(19) . . ? C1B C2B C8B 117.5(2) . . ? C4B C3B C2B 118.31(19) . . ? C4B C3B C17B 120.1(2) . . ? C2B C3B C17B 121.59(19) . . ? C5B C4B C3B 123.9(2) . . ? C5B C4B H4B 118.0 . . ? C3B C4B H4B 118.0 . . ? C4B C5B C6B 118.43(19) . . ? C4B C5B C20B 120.5(2) . . ? C6B C5B C20B 121.00(19) . . ? C5B C6B C1B 119.63(19) . . ? C5B C6B C7B 122.49(19) . . ? C1B C6B C7B 117.9(2) . . ? C8B C7B C6B 121.9(2) 2_655 . ? C8B C7B H7B 119.1 2_655 . ? C6B C7B H7B 119.1 . . ? C7B C8B C2B 122.6(2) 2_655 . ? C7B C8B H8B 118.7 2_655 . ? C2B C8B H8B 118.7 . . ? C3B C17B C19B 114.43(18) . . ? C3B C17B C18B 110.17(18) . . ? C19B C17B C18B 109.9(2) . . ? C3B C17B H17B 107.3 . . ? C19B C17B H17B 107.3 . . ? C18B C17B H17B 107.3 . . ? C17B C18B H18G 109.5 . . ? C17B C18B H18H 109.5 . . ? H18G C18B H18H 109.5 . . ? C17B C18B H18I 109.5 . . ? H18G C18B H18I 109.5 . . ? H18H C18B H18I 109.5 . . ? C17B C19B H19G 109.5 . . ? C17B C19B H19H 109.5 . . ? H19G C19B H19H 109.5 . . ? C17B C19B H19I 109.5 . . ? H19G C19B H19I 109.5 . . ? H19H C19B H19I 109.5 . . ? C21B C20B C5B 109.71(19) . . ? C21B C20B C22B 110.5(2) . . ? C5B C20B C22B 113.68(19) . . ? C21B C20B H20B 107.6 . . ? C5B C20B H20B 107.6 . . ? C22B C20B H20B 107.6 . . ? C20B C21B H21G 109.5 . . ? C20B C21B H21H 109.5 . . ? H21G C21B H21H 109.5 . . ? C20B C21B H21I 109.5 . . ? H21G C21B H21I 109.5 . . ? H21H C21B H21I 109.5 . . ? C20B C22B H22G 109.5 . . ? C20B C22B H22H 109.5 . . ? H22G C22B H22H 109.5 . . ? C20B C22B H22I 109.5 . . ? H22G C22B H22I 109.5 . . ? H22H C22B H22I 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 0.3(3) . . . . ? C9 C1 C2 C3 -179.35(18) . . . . ? C6 C1 C2 C16 -179.87(18) . . . . ? C9 C1 C2 C16 0.5(3) . . . . ? C1 C2 C3 C4 -0.4(3) . . . . ? C16 C2 C3 C4 179.74(19) . . . . ? C1 C2 C3 C17 -178.69(18) . . . . ? C16 C2 C3 C17 1.5(3) . . . . ? C2 C3 C4 C5 0.3(3) . . . . ? C17 C3 C4 C5 178.6(2) . . . . ? C3 C4 C5 C6 0.0(3) . . . . ? C3 C4 C5 C20 179.9(2) . . . . ? C4 C5 C6 C1 -0.2(3) . . . . ? C20 C5 C6 C1 179.99(19) . . . . ? C4 C5 C6 C7 179.9(2) . . . . ? C20 C5 C6 C7 0.1(3) . . . . ? C2 C1 C6 C5 0.0(3) . . . . ? C9 C1 C6 C5 179.66(18) . . . . ? C2 C1 C6 C7 179.90(18) . . . . ? C9 C1 C6 C7 -0.4(3) . . . . ? C5 C6 C7 C8 -178.7(2) . . . . ? C1 C6 C7 C8 1.4(3) . . . . ? C6 C7 C8 C10 -0.3(3) . . . . ? C2 C1 C9 C10 178.12(18) . . . . ? C6 C1 C9 C10 -1.5(3) . . . . ? C2 C1 C9 C14 -1.3(3) . . . . ? C6 C1 C9 C14 179.07(18) . . . . ? C14 C9 C10 C11 1.7(3) . . . . ? C1 C9 C10 C11 -177.65(19) . . . . ? C14 C9 C10 C8 -178.03(18) . . . . ? C1 C9 C10 C8 2.6(3) . . . . ? C7 C8 C10 C11 178.5(2) . . . . ? C7 C8 C10 C9 -1.7(3) . . . . ? C9 C10 C11 C12 -2.7(3) . . . . ? C8 C10 C11 C12 177.0(2) . . . . ? C9 C10 C11 C23 -179.93(19) . . . . ? C8 C10 C11 C23 -0.2(3) . . . . ? C10 C11 C12 C13 1.3(3) . . . . ? C23 C11 C12 C13 178.5(2) . . . . ? C11 C12 C13 C14 1.2(3) . . . . ? C11 C12 C13 C26 178.2(2) . . . . ? C12 C13 C14 C9 -2.2(3) . . . . ? C26 C13 C14 C9 -179.21(19) . . . . ? C12 C13 C14 C15 176.7(2) . . . . ? C26 C13 C14 C15 -0.3(3) . . . . ? C10 C9 C14 C13 0.8(3) . . . . ? C1 C9 C14 C13 -179.82(18) . . . . ? C10 C9 C14 C15 -178.18(18) . . . . ? C1 C9 C14 C15 1.2(3) . . . . ? C13 C14 C15 C16 -179.3(2) . . . . ? C9 C14 C15 C16 -0.4(3) . . . . ? C14 C15 C16 C2 -0.4(3) . . . . ? C3 C2 C16 C15 -179.8(2) . . . . ? C1 C2 C16 C15 0.4(3) . . . . ? C4 C3 C17 C18 32.1(3) . . . . ? C2 C3 C17 C18 -149.7(2) . . . . ? C4 C3 C17 C19 -93.4(3) . . . . ? C2 C3 C17 C19 84.8(3) . . . . ? C4 C5 C20 C21 -56.7(3) . . . . ? C6 C5 C20 C21 123.1(2) . . . . ? C4 C5 C20 C22 66.8(3) . . . . ? C6 C5 C20 C22 -113.3(2) . . . . ? C12 C11 C23 C24 -80.2(3) . . . . ? C10 C11 C23 C24 96.9(3) . . . . ? C12 C11 C23 C25 47.2(3) . . . . ? C10 C11 C23 C25 -135.6(3) . . . . ? C12 C13 C26 C27 -89.3(3) . . . . ? C14 C13 C26 C27 87.7(3) . . . . ? C12 C13 C26 C28 35.2(3) . . . . ? C14 C13 C26 C28 -147.9(2) . . . . ? C6A C1A C2A C3A -1.6(3) . . . . ? C1A C1A C2A C3A 177.6(2) 2_676 . . . ? C6A C1A C2A C8A -179.72(18) . . . 2_676 ? C1A C1A C2A C8A -0.5(3) 2_676 . . 2_676 ? C1A C2A C3A C4A 0.9(3) . . . . ? C8A C2A C3A C4A 178.90(19) 2_676 . . . ? C1A C2A C3A C17A -174.89(18) . . . . ? C8A C2A C3A C17A 3.1(3) 2_676 . . . ? C2A C3A C4A C5A 0.8(3) . . . . ? C17A C3A C4A C5A 176.65(19) . . . . ? C3A C4A C5A C6A -1.7(3) . . . . ? C3A C4A C5A C20A 179.93(19) . . . . ? C4A C5A C6A C1A 0.9(3) . . . . ? C20A C5A C6A C1A 179.23(18) . . . . ? C4A C5A C6A C7A -178.32(19) . . . . ? C20A C5A C6A C7A 0.0(3) . . . . ? C2A C1A C6A C5A 0.7(3) . . . . ? C1A C1A C6A C5A -178.5(2) 2_676 . . . ? C2A C1A C6A C7A 179.97(18) . . . . ? C1A C1A C6A C7A 0.8(3) 2_676 . . . ? C5A C6A C7A C8A 178.7(2) . . . . ? C1A C6A C7A C8A -0.5(3) . . . . ? C6A C7A C8A C2A 0.2(3) . . . 2_676 ? C4A C3A C17A C19A 31.5(3) . . . . ? C2A C3A C17A C19A -152.8(2) . . . . ? C4A C3A C17A C18A -93.1(3) . . . . ? C2A C3A C17A C18A 82.6(3) . . . . ? C4A C5A C20A C21A -29.0(3) . . . . ? C6A C5A C20A C21A 152.7(2) . . . . ? C4A C5A C20A C22A 96.0(2) . . . . ? C6A C5A C20A C22A -82.3(3) . . . . ? C6B C1B C2B C3B -0.8(3) . . . . ? C1B C1B C2B C3B 179.4(2) 2_655 . . . ? C6B C1B C2B C8B 179.64(18) . . . . ? C1B C1B C2B C8B -0.2(3) 2_655 . . . ? C1B C2B C3B C4B 0.4(3) . . . . ? C8B C2B C3B C4B 179.99(19) . . . . ? C1B C2B C3B C17B -177.00(18) . . . . ? C8B C2B C3B C17B 2.5(3) . . . . ? C2B C3B C4B C5B 0.3(3) . . . . ? C17B C3B C4B C5B 177.82(19) . . . . ? C3B C4B C5B C6B -0.7(3) . . . . ? C3B C4B C5B C20B -178.11(19) . . . . ? C4B C5B C6B C1B 0.3(3) . . . . ? C20B C5B C6B C1B 177.72(18) . . . . ? C4B C5B C6B C7B -178.85(19) . . . . ? C20B C5B C6B C7B -1.5(3) . . . . ? C2B C1B C6B C5B 0.4(3) . . . . ? C1B C1B C6B C5B -179.8(2) 2_655 . . . ? C2B C1B C6B C7B 179.63(18) . . . . ? C1B C1B C6B C7B -0.6(3) 2_655 . . . ? C5B C6B C7B C8B 179.8(2) . . . 2_655 ? C1B C6B C7B C8B 0.6(3) . . . 2_655 ? C3B C2B C8B C7B -179.4(2) . . . 2_655 ? C1B C2B C8B C7B 0.2(3) . . . 2_655 ? C4B C3B C17B C19B 31.1(3) . . . . ? C2B C3B C17B C19B -151.5(2) . . . . ? C4B C3B C17B C18B -93.3(2) . . . . ? C2B C3B C17B C18B 84.1(2) . . . . ? C4B C5B C20B C21B 95.5(3) . . . . ? C6B C5B C20B C21B -81.8(3) . . . . ? C4B C5B C20B C22B -28.7(3) . . . . ? C6B C5B C20B C22B 154.0(2) . . . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 67.24 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 0.243 _refine_diff_density_min -0.188 _refine_diff_density_rms 0.046 # Attachment 'raj9wa.cif' data_raj9wa _database_code_depnum_ccdc_archive 'CCDC 674751' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H50 Cl6 Sb' _chemical_formula_weight 889.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.0562 5.8946 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P nma' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 13.8054(3) _cell_length_b 12.5572(3) _cell_length_c 23.6942(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4107.56(17) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7373 _cell_measurement_theta_min 3 _cell_measurement_theta_max 67 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.438 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1820 _exptl_absorpt_coefficient_mu 9.129 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.0897 _exptl_absorpt_correction_T_max 0.3613 _exptl_absorpt_process_details ; Numerical absorption correction followed by: SADABS. Program for empirical absorption correction of area-detector data. University of Goetingen. Germany. Sheldrick, G. M. 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX2 CCD detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34504 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_sigmaI/netI 0.0165 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 67.39 _reflns_number_total 3746 _reflns_number_gt 3673 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2.0-2 (Bruker, 2005)' _computing_cell_refinement 'SAINT v7.23A (Bruker, 2005)' _computing_data_reduction 'SADABS-2004/1 (Bruker, 2005)' _computing_structure_solution 'XS/SHELXTL v6.12 (Bruker, 2001)' _computing_structure_refinement 'SHELXL-97 v.97-2 (Sheldrick, 1993-1997)' _computing_molecular_graphics 'XP v5.1 (Bruker, 1998)' _computing_publication_material 'XCIF v6.12 (Bruker, 2001)' _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^)+(0.0300P)^2^+6.6580P] 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 SHELXL _refine_ls_extinction_coef 0.00017(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3746 _refine_ls_number_parameters 255 _refine_ls_number_restraints 50 _refine_ls_R_factor_all 0.0272 _refine_ls_R_factor_gt 0.0268 _refine_ls_wR_factor_ref 0.0662 _refine_ls_wR_factor_gt 0.0659 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.015 _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 Sb1 Sb 0.088096(15) 0.2500 0.322216(9) 0.02244(9) Uani 1 2 d S . . Cl1 Cl 0.22951(6) 0.2500 0.37899(4) 0.02984(19) Uani 1 2 d S . . Cl2 Cl -0.05352(6) 0.2500 0.26503(4) 0.0310(2) Uani 1 2 d S . . Cl3 Cl 0.01817(4) 0.11821(4) 0.38067(3) 0.03101(15) Uani 1 1 d . . . Cl4 Cl 0.15681(4) 0.11665(5) 0.26406(3) 0.03500(16) Uani 1 1 d . . . C1 C 0.11135(14) 0.34820(17) 0.72184(8) 0.0130(4) Uani 1 1 d . . . C2 C 0.13698(14) 0.44412(16) 0.69469(8) 0.0143(4) Uani 1 1 d . . . H2 H 0.1204 0.5101 0.7118 0.017 Uiso 1 1 calc R . . C3 C 0.18544(14) 0.44419(16) 0.64397(8) 0.0140(4) Uani 1 1 d . . . H3 H 0.2017 0.5102 0.6268 0.017 Uiso 1 1 calc R . . C4 C 0.21157(13) 0.34825(16) 0.61676(8) 0.0119(4) Uani 1 1 d . . . C5 C 0.18709(19) 0.2500 0.64317(11) 0.0110(5) Uani 1 2 d S . . C6 C 0.13692(19) 0.2500 0.69584(11) 0.0120(6) Uani 1 2 d S . . C7 C 0.26076(13) 0.34740(16) 0.56349(8) 0.0127(4) Uani 1 1 d . . . C8 C 0.2837(2) 0.2500 0.53942(11) 0.0136(6) Uani 1 2 d S . . H8 H 0.3171 0.2500 0.5044 0.016 Uiso 1 2 calc SR . . C9 C 0.05958(14) 0.34741(17) 0.77449(8) 0.0142(4) Uani 1 1 d . . . C10 C 0.0363(2) 0.2500 0.79847(12) 0.0153(6) Uani 1 2 d S . . H10 H 0.0025 0.2500 0.8334 0.018 Uiso 1 2 calc SR . . C11 C 0.28260(14) 0.45015(16) 0.53256(8) 0.0146(4) Uani 1 1 d . . . H11 H 0.2963 0.5065 0.5613 0.018 Uiso 1 1 calc R . . C12 C 0.36994(16) 0.44269(18) 0.49301(9) 0.0214(5) Uani 1 1 d . . . H12A H 0.3865 0.5139 0.4791 0.032 Uiso 1 1 calc R . . H12B H 0.3540 0.3964 0.4610 0.032 Uiso 1 1 calc R . . H12C H 0.4253 0.4129 0.5136 0.032 Uiso 1 1 calc R . . C13 C 0.19177(16) 0.48355(18) 0.49914(9) 0.0223(5) Uani 1 1 d . . . H13A H 0.2057 0.5484 0.4776 0.033 Uiso 1 1 calc R . . H13B H 0.1384 0.4972 0.5254 0.033 Uiso 1 1 calc R . . H13C H 0.1735 0.4263 0.4731 0.033 Uiso 1 1 calc R . . C14 C 0.03275(15) 0.45124(17) 0.80308(9) 0.0174(4) Uani 1 1 d . . . H14 H 0.0153 0.5031 0.7727 0.021 Uiso 1 1 calc R . . C15 C -0.05480(18) 0.4421(2) 0.84251(10) 0.0281(5) Uani 1 1 d . . . H15A H -0.0749 0.5134 0.8546 0.042 Uiso 1 1 calc R . . H15B H -0.0372 0.3996 0.8756 0.042 Uiso 1 1 calc R . . H15C H -0.1083 0.4075 0.8225 0.042 Uiso 1 1 calc R . . C16 C 0.12066(18) 0.4968(2) 0.83456(10) 0.0263(5) Uani 1 1 d . . . H16A H 0.1032 0.5652 0.8517 0.039 Uiso 1 1 calc R . . H16B H 0.1741 0.5074 0.8079 0.039 Uiso 1 1 calc R . . H16C H 0.1408 0.4469 0.8641 0.039 Uiso 1 1 calc R . . C7S C 0.8942(4) 0.7500 1.0447(2) 0.0330(13) Uiso 0.766(8) 2 d SPD A 1 H7S1 H 0.9556 0.7891 1.0461 0.049 Uiso 0.383(4) 1 calc PR A 1 H7S2 H 0.9047 0.6765 1.0571 0.049 Uiso 0.383(4) 1 calc PR A 1 H7S3 H 0.8471 0.7845 1.0696 0.049 Uiso 0.383(4) 1 calc PR A 1 C1S C 0.8560(4) 0.7500 0.98502(18) 0.0189(12) Uiso 0.766(8) 2 d SPD A 1 C2S C 0.7580(4) 0.7500 0.9759(3) 0.0274(12) Uiso 0.766(8) 2 d SPD A 1 H2S H 0.7150 0.7500 1.0072 0.033 Uiso 0.766(8) 2 calc SPR A 1 C3S C 0.7200(4) 0.7500 0.9205(2) 0.0305(12) Uiso 0.766(8) 2 d SPD A 1 H3S H 0.6521 0.7500 0.9140 0.037 Uiso 0.766(8) 2 calc SPR A 1 C4S C 0.7863(4) 0.7500 0.8747(2) 0.0280(12) Uiso 0.766(8) 2 d SPD A 1 H4S H 0.7624 0.7500 0.8371 0.034 Uiso 0.766(8) 2 calc SPR A 1 C5S C 0.8859(5) 0.7500 0.8841(2) 0.0254(13) Uiso 0.766(8) 2 d SPD A 1 H5S H 0.9304 0.7500 0.8535 0.031 Uiso 0.766(8) 2 calc SPR A 1 C6S C 0.9181(3) 0.7500 0.9392(3) 0.0220(10) Uiso 0.766(8) 2 d SPD A 1 H6S H 0.9859 0.7500 0.9461 0.026 Uiso 0.766(8) 2 calc SPR A 1 C7Q C 0.8179(15) 0.7500 1.0518(6) 0.051(5) Uiso 0.234(8) 2 d SPD A 2 H7Q1 H 0.7498 0.7435 1.0629 0.076 Uiso 0.117(4) 1 calc PR A 2 H7Q2 H 0.8445 0.8167 1.0666 0.076 Uiso 0.117(4) 1 calc PR A 2 H7Q3 H 0.8547 0.6898 1.0670 0.076 Uiso 0.117(4) 1 calc PR A 2 C1Q C 0.8253(12) 0.7500 0.9883(5) 0.019(4) Uiso 0.234(8) 2 d SPD A 2 C2Q C 0.7464(8) 0.7500 0.9536(6) 0.013(3) Uiso 0.234(8) 2 d SPD A 2 H2Q H 0.6835 0.7500 0.9699 0.015 Uiso 0.234(8) 2 calc SPR A 2 C3Q C 0.7553(10) 0.7500 0.8936(6) 0.014(3) Uiso 0.234(8) 2 d SPD A 2 H3Q H 0.7018 0.7500 0.8684 0.017 Uiso 0.234(8) 2 calc SPR A 2 C4Q C 0.8536(13) 0.7500 0.8761(7) 0.036(5) Uiso 0.234(8) 2 d SPD A 2 H4Q H 0.8652 0.7500 0.8365 0.043 Uiso 0.234(8) 2 calc SPR A 2 C5Q C 0.9354(14) 0.7500 0.9113(9) 0.053(6) Uiso 0.234(8) 2 d SPD A 2 H5Q H 0.9993 0.7500 0.8964 0.063 Uiso 0.234(8) 2 calc SPR A 2 C6Q C 0.9186(11) 0.7500 0.9672(9) 0.037(5) Uiso 0.234(8) 2 d SPD A 2 H6Q H 0.9718 0.7500 0.9926 0.045 Uiso 0.234(8) 2 calc SPR A 2 C17S C 0.3237(6) 0.2500 0.7991(3) 0.0375(18) Uiso 0.631(7) 2 d SPD . 1 H17A H 0.2576 0.2729 0.8078 0.056 Uiso 0.315(3) 1 calc PR . 1 H17B H 0.3223 0.1780 0.7832 0.056 Uiso 0.315(3) 1 calc PR . 1 H17C H 0.3526 0.2991 0.7717 0.056 Uiso 0.315(3) 1 calc PR . 1 C11S C 0.3829(4) 0.2500 0.8520(2) 0.0233(13) Uiso 0.631(7) 2 d SPD . 1 C12S C 0.4088(3) 0.1551(3) 0.8751(2) 0.0203(12) Uiso 0.631(7) 1 d PD . 1 H12S H 0.3899 0.0901 0.8578 0.024 Uiso 0.631(7) 1 calc PR . 1 C13S C 0.4652(3) 0.1546(3) 0.92618(16) 0.0246(10) Uiso 0.631(7) 1 d PD . 1 H13S H 0.4843 0.0890 0.9428 0.030 Uiso 0.631(7) 1 calc PR . 1 C14S C 0.4912(5) 0.2500 0.9508(3) 0.0299(16) Uiso 0.631(7) 2 d SPD . 1 H14S H 0.5274 0.2500 0.9849 0.036 Uiso 0.631(7) 2 calc SPR . 1 C17Q C 0.4980(10) 0.2500 0.9702(6) 0.045(4) Uiso 0.369(7) 2 d SPD . 2 H17D H 0.5635 0.2780 0.9645 0.067 Uiso 0.185(3) 1 calc PR . 2 H17E H 0.5019 0.1771 0.9847 0.067 Uiso 0.185(3) 1 calc PR . 2 H17F H 0.4634 0.2949 0.9974 0.067 Uiso 0.185(3) 1 calc PR . 2 C11Q C 0.4439(7) 0.2500 0.9144(4) 0.029(2) Uiso 0.369(7) 2 d SPD . 2 C12Q C 0.4231(5) 0.1550(5) 0.8920(4) 0.020(2) Uiso 0.369(7) 1 d PD . 2 H12Q H 0.4419 0.0910 0.9105 0.024 Uiso 0.369(7) 1 calc PR . 2 C13Q C 0.3719(6) 0.1523(7) 0.8397(4) 0.046(2) Uiso 0.369(7) 1 d PD . 2 H13Q H 0.3561 0.0864 0.8223 0.056 Uiso 0.369(7) 1 calc PR . 2 C14Q C 0.3452(15) 0.2500 0.8144(8) 0.076(6) Uiso 0.369(7) 2 d SPD . 2 H14Q H 0.3092 0.2500 0.7802 0.091 Uiso 0.369(7) 2 calc SPR . 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 Sb1 0.02210(13) 0.01572(13) 0.02951(14) 0.000 -0.01435(8) 0.000 Cl1 0.0258(4) 0.0296(4) 0.0341(4) 0.000 -0.0181(3) 0.000 Cl2 0.0254(4) 0.0278(4) 0.0399(5) 0.000 -0.0199(4) 0.000 Cl3 0.0331(3) 0.0168(3) 0.0431(3) 0.0044(2) -0.0119(3) -0.0027(2) Cl4 0.0327(3) 0.0333(3) 0.0391(3) -0.0105(3) -0.0144(3) 0.0077(3) C1 0.0092(8) 0.0178(11) 0.0121(9) -0.0002(8) -0.0019(8) 0.0019(8) C2 0.0139(9) 0.0139(10) 0.0149(9) -0.0018(8) -0.0014(8) 0.0020(8) C3 0.0140(9) 0.0142(10) 0.0137(9) 0.0013(8) -0.0018(8) -0.0006(8) C4 0.0074(8) 0.0161(10) 0.0123(9) 0.0006(8) -0.0021(7) -0.0002(8) C5 0.0058(12) 0.0159(14) 0.0113(13) 0.000 -0.0027(10) 0.000 C6 0.0081(12) 0.0175(15) 0.0105(13) 0.000 -0.0028(11) 0.000 C7 0.0084(8) 0.0180(10) 0.0115(9) 0.0012(8) -0.0028(7) -0.0016(8) C8 0.0117(13) 0.0206(15) 0.0087(13) 0.000 0.0000(11) 0.000 C9 0.0094(9) 0.0198(11) 0.0133(9) -0.0009(8) -0.0019(8) 0.0016(8) C10 0.0127(13) 0.0213(16) 0.0119(13) 0.000 0.0026(11) 0.000 C11 0.0163(10) 0.0156(10) 0.0119(9) 0.0005(8) 0.0001(8) -0.0015(8) C12 0.0247(11) 0.0209(11) 0.0185(10) 0.0026(9) 0.0070(9) -0.0022(9) C13 0.0251(11) 0.0203(12) 0.0214(11) 0.0056(9) -0.0068(9) -0.0005(9) C14 0.0202(10) 0.0171(11) 0.0148(9) 0.0000(8) 0.0067(9) 0.0024(9) C15 0.0309(12) 0.0239(12) 0.0295(12) -0.0002(10) 0.0172(11) 0.0057(10) C16 0.0353(13) 0.0239(12) 0.0197(11) -0.0073(9) 0.0035(10) -0.0045(11) _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 Sb1 Cl3 2.3642(6) 7_565 ? Sb1 Cl3 2.3642(6) . ? Sb1 Cl4 2.3671(6) . ? Sb1 Cl4 2.3671(6) 7_565 ? Sb1 Cl1 2.3709(8) . ? Sb1 Cl2 2.3788(8) . ? C1 C2 1.411(3) . ? C1 C6 1.423(2) . ? C1 C9 1.438(3) . ? C2 C3 1.375(3) . ? C2 H2 0.9500 . ? C3 C4 1.413(3) . ? C3 H3 0.9500 . ? C4 C5 1.424(2) . ? C4 C7 1.433(3) . ? C5 C4 1.424(2) 7_565 ? C5 C6 1.427(4) . ? C6 C1 1.423(2) 7_565 ? C7 C8 1.386(2) . ? C7 C11 1.514(3) . ? C8 C7 1.386(2) 7_565 ? C8 H8 0.9500 . ? C9 C10 1.386(2) . ? C9 C14 1.515(3) . ? C10 C9 1.386(2) 7_565 ? C10 H10 0.9500 . ? C11 C12 1.530(3) . ? C11 C13 1.541(3) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.532(3) . ? C14 C16 1.535(3) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C7S C1S 1.509(6) . ? C7S H7S1 0.9800 . ? C7S H7S2 0.9800 . ? C7S H7S3 0.9800 . ? C1S C2S 1.371(7) . ? C1S C6S 1.382(8) . ? C2S C3S 1.413(7) . ? C2S H2S 0.9500 . ? C3S C4S 1.419(7) . ? C3S H3S 0.9500 . ? C4S C5S 1.394(7) . ? C4S H4S 0.9500 . ? C5S C6S 1.380(8) . ? C5S H5S 0.9500 . ? C6S H6S 0.9500 . ? C7Q C1Q 1.508(13) . ? C7Q H7Q1 0.9800 . ? C7Q H7Q2 0.9800 . ? C7Q H7Q3 0.9800 . ? C1Q C2Q 1.365(13) . ? C1Q C6Q 1.381(16) . ? C2Q C3Q 1.425(14) . ? C2Q H2Q 0.9500 . ? C3Q C4Q 1.420(14) . ? C3Q H3Q 0.9500 . ? C4Q C5Q 1.404(17) . ? C4Q H4Q 0.9500 . ? C5Q C6Q 1.345(17) . ? C5Q H5Q 0.9500 . ? C6Q H6Q 0.9500 . ? C17S C11S 1.495(8) . ? C17S H17A 0.9800 . ? C17S H17B 0.9800 . ? C17S H17C 0.9800 . ? C11S C12S 1.359(5) 7_565 ? C11S C12S 1.359(5) . ? C12S C13S 1.438(6) . ? C12S H12S 0.9500 . ? C13S C14S 1.380(5) . ? C13S H13S 0.9500 . ? C14S C13S 1.380(5) 7_565 ? C14S H14S 0.9500 . ? C17Q C11Q 1.519(12) . ? C17Q H17D 0.9800 . ? C17Q H17E 0.9800 . ? C17Q H17F 0.9800 . ? C11Q C12Q 1.337(7) . ? C11Q C12Q 1.337(7) 7_565 ? C12Q C13Q 1.427(9) . ? C12Q H12Q 0.9500 . ? C13Q C14Q 1.415(11) . ? C13Q H13Q 0.9500 . ? C14Q C13Q 1.415(11) 7_565 ? C14Q H14Q 0.9500 . ? 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 Cl3 Sb1 Cl3 88.86(3) 7_565 . ? Cl3 Sb1 Cl4 179.36(2) 7_565 . ? Cl3 Sb1 Cl4 90.55(2) . . ? Cl3 Sb1 Cl4 90.54(2) 7_565 7_565 ? Cl3 Sb1 Cl4 179.36(2) . 7_565 ? Cl4 Sb1 Cl4 90.05(3) . 7_565 ? Cl3 Sb1 Cl1 90.22(2) 7_565 . ? Cl3 Sb1 Cl1 90.22(2) . . ? Cl4 Sb1 Cl1 90.02(2) . . ? Cl4 Sb1 Cl1 90.02(2) 7_565 . ? Cl3 Sb1 Cl2 89.89(2) 7_565 . ? Cl3 Sb1 Cl2 89.89(2) . . ? Cl4 Sb1 Cl2 89.87(2) . . ? Cl4 Sb1 Cl2 89.87(2) 7_565 . ? Cl1 Sb1 Cl2 179.84(3) . . ? C2 C1 C6 118.71(18) . . ? C2 C1 C9 121.76(19) . . ? C6 C1 C9 119.53(19) . . ? C3 C2 C1 121.40(18) . . ? C3 C2 H2 119.3 . . ? C1 C2 H2 119.3 . . ? C2 C3 C4 121.48(18) . . ? C2 C3 H3 119.3 . . ? C4 C3 H3 119.3 . . ? C3 C4 C5 118.53(18) . . ? C3 C4 C7 121.94(18) . . ? C5 C4 C7 119.53(18) . . ? C4 C5 C4 120.1(2) 7_565 . ? C4 C5 C6 119.96(12) 7_565 . ? C4 C5 C6 119.95(12) . . ? C1 C6 C1 120.1(3) . 7_565 ? C1 C6 C5 119.93(13) . . ? C1 C6 C5 119.93(13) 7_565 . ? C8 C7 C4 118.49(19) . . ? C8 C7 C11 120.49(18) . . ? C4 C7 C11 120.94(18) . . ? C7 C8 C7 123.9(3) 7_565 . ? C7 C8 H8 118.1 7_565 . ? C7 C8 H8 118.1 . . ? C10 C9 C1 118.48(19) . . ? C10 C9 C14 121.28(18) . . ? C1 C9 C14 120.23(18) . . ? C9 C10 C9 123.8(3) . 7_565 ? C9 C10 H10 118.1 . . ? C9 C10 H10 118.1 7_565 . ? C7 C11 C12 113.65(17) . . ? C7 C11 C13 108.58(16) . . ? C12 C11 C13 110.06(17) . . ? C7 C11 H11 108.1 . . ? C12 C11 H11 108.1 . . ? C13 C11 H11 108.1 . . ? 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 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C9 C14 C15 113.64(18) . . ? C9 C14 C16 110.16(17) . . ? C15 C14 C16 110.82(18) . . ? C9 C14 H14 107.3 . . ? C15 C14 H14 107.3 . . ? C16 C14 H14 107.3 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C2S C1S C6S 119.2(4) . . ? C2S C1S C7S 119.6(5) . . ? C6S C1S C7S 121.2(5) . . ? C1S C2S C3S 120.9(5) . . ? C1S C2S H2S 119.6 . . ? C3S C2S H2S 119.6 . . ? C2S C3S C4S 118.1(4) . . ? C2S C3S H3S 121.0 . . ? C4S C3S H3S 121.0 . . ? C5S C4S C3S 121.0(4) . . ? C5S C4S H4S 119.5 . . ? C3S C4S H4S 119.5 . . ? C6S C5S C4S 117.9(5) . . ? C6S C5S H5S 121.0 . . ? C4S C5S H5S 121.0 . . ? C1S C6S C5S 122.9(5) . . ? C1S C6S H6S 118.5 . . ? C5S C6S H6S 118.5 . . ? C1Q C7Q H7Q1 109.5 . . ? C1Q C7Q H7Q2 109.5 . . ? H7Q1 C7Q H7Q2 109.5 . . ? C1Q C7Q H7Q3 109.5 . . ? H7Q1 C7Q H7Q3 109.5 . . ? H7Q2 C7Q H7Q3 109.5 . . ? C2Q C1Q C6Q 121.8(12) . . ? C2Q C1Q C7Q 123.2(15) . . ? C6Q C1Q C7Q 115.1(14) . . ? C1Q C2Q C3Q 122.1(11) . . ? C1Q C2Q H2Q 119.0 . . ? C3Q C2Q H2Q 119.0 . . ? C4Q C3Q C2Q 112.0(11) . . ? C4Q C3Q H3Q 124.0 . . ? C2Q C3Q H3Q 124.0 . . ? C5Q C4Q C3Q 126.5(14) . . ? C5Q C4Q H4Q 116.8 . . ? C3Q C4Q H4Q 116.8 . . ? C6Q C5Q C4Q 116.5(16) . . ? C6Q C5Q H5Q 121.7 . . ? C4Q C5Q H5Q 121.7 . . ? C5Q C6Q C1Q 121.1(15) . . ? C5Q C6Q H6Q 119.4 . . ? C1Q C6Q H6Q 119.4 . . ? C12S C11S C12S 122.4(6) 7_565 . ? C12S C11S C17S 118.8(3) 7_565 . ? C12S C11S C17S 118.8(3) . . ? C11S C12S C13S 119.1(4) . . ? C11S C12S H12S 120.5 . . ? C13S C12S H12S 120.5 . . ? C14S C13S C12S 119.4(4) . . ? C14S C13S H13S 120.3 . . ? C12S C13S H13S 120.3 . . ? C13S C14S C13S 120.5(6) 7_565 . ? C13S C14S H14S 119.7 7_565 . ? C13S C14S H14S 119.7 . . ? C11Q C17Q H17D 109.5 . . ? C11Q C17Q H17E 109.5 . . ? H17D C17Q H17E 109.5 . . ? C11Q C17Q H17F 109.5 . . ? H17D C17Q H17F 109.5 . . ? H17E C17Q H17F 109.5 . . ? C12Q C11Q C12Q 126.5(10) . 7_565 ? C12Q C11Q C17Q 116.7(5) . . ? C12Q C11Q C17Q 116.8(5) 7_565 . ? C11Q C12Q C13Q 118.1(7) . . ? C11Q C12Q H12Q 120.9 . . ? C13Q C12Q H12Q 120.9 . . ? C14Q C13Q C12Q 118.5(10) . . ? C14Q C13Q H13Q 120.8 . . ? C12Q C13Q H13Q 120.8 . . ? C13Q C14Q C13Q 120.3(15) 7_565 . ? C13Q C14Q H14Q 119.9 7_565 . ? C13Q C14Q H14Q 119.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 0.2(3) . . . . ? C9 C1 C2 C3 -179.17(18) . . . . ? C1 C2 C3 C4 0.1(3) . . . . ? C2 C3 C4 C5 -0.3(3) . . . . ? C2 C3 C4 C7 179.03(18) . . . . ? C3 C4 C5 C4 179.50(15) . . . 7_565 ? C7 C4 C5 C4 0.1(4) . . . 7_565 ? C3 C4 C5 C6 0.2(3) . . . . ? C7 C4 C5 C6 -179.1(2) . . . . ? C2 C1 C6 C1 -179.41(16) . . . 7_565 ? C9 C1 C6 C1 0.0(4) . . . 7_565 ? C2 C1 C6 C5 -0.3(3) . . . . ? C9 C1 C6 C5 179.1(2) . . . . ? C4 C5 C6 C1 -179.2(2) 7_565 . . . ? C4 C5 C6 C1 0.1(4) . . . . ? C4 C5 C6 C1 -0.1(4) 7_565 . . 7_565 ? C4 C5 C6 C1 179.2(2) . . . 7_565 ? C3 C4 C7 C8 -179.8(2) . . . . ? C5 C4 C7 C8 -0.4(3) . . . . ? C3 C4 C7 C11 -3.0(3) . . . . ? C5 C4 C7 C11 176.33(19) . . . . ? C4 C7 C8 C7 0.8(4) . . . 7_565 ? C11 C7 C8 C7 -175.96(17) . . . 7_565 ? C2 C1 C9 C10 179.6(2) . . . . ? C6 C1 C9 C10 0.2(3) . . . . ? C2 C1 C9 C14 -1.3(3) . . . . ? C6 C1 C9 C14 179.32(19) . . . . ? C1 C9 C10 C9 -0.4(4) . . . 7_565 ? C14 C9 C10 C9 -179.53(18) . . . 7_565 ? C8 C7 C11 C12 -29.1(3) . . . . ? C4 C7 C11 C12 154.14(18) . . . . ? C8 C7 C11 C13 93.7(2) . . . . ? C4 C7 C11 C13 -83.0(2) . . . . ? C10 C9 C14 C15 -25.4(3) . . . . ? C1 C9 C14 C15 155.45(19) . . . . ? C10 C9 C14 C16 99.6(2) . . . . ? C1 C9 C14 C16 -79.5(2) . . . . ? C6S C1S C2S C3S 0.000(3) . . . . ? C7S C1S C2S C3S 180.000(2) . . . . ? C1S C2S C3S C4S 0.000(2) . . . . ? C2S C3S C4S C5S 0.000(3) . . . . ? C3S C4S C5S C6S 0.000(3) . . . . ? C2S C1S C6S C5S 0.000(3) . . . . ? C7S C1S C6S C5S 180.000(3) . . . . ? C4S C5S C6S C1S 0.000(3) . . . . ? C6Q C1Q C2Q C3Q 0.000(6) . . . . ? C7Q C1Q C2Q C3Q 180.000(6) . . . . ? C1Q C2Q C3Q C4Q 0.000(6) . . . . ? C2Q C3Q C4Q C5Q 0.000(10) . . . . ? C3Q C4Q C5Q C6Q 0.000(12) . . . . ? C4Q C5Q C6Q C1Q 0.000(7) . . . . ? C2Q C1Q C6Q C5Q 0.000(11) . . . . ? C7Q C1Q C6Q C5Q 180.000(7) . . . . ? C12S C11S C12S C13S 0.4(8) 7_565 . . . ? C17S C11S C12S C13S -179.6(5) . . . . ? C11S C12S C13S C14S 0.4(6) . . . . ? C12S C13S C14S C13S -1.2(9) . . . 7_565 ? C12Q C11Q C12Q C13Q -1.4(15) 7_565 . . . ? C17Q C11Q C12Q C13Q 179.7(9) . . . . ? C11Q C12Q C13Q C14Q -0.4(15) . . . . ? C12Q C13Q C14Q C13Q 2(2) . . . 7_565 ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 67.39 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.074 _refine_diff_density_min -1.066 _refine_diff_density_rms 0.064