# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 1145 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Todd Marder' 'David Albesa-Jove' 'Andrei S. Batsanov' 'A. Beeby' 'Abdou Boucekkine' 'Jacqueline M. Burke' 'Jonathan C. Collings' 'Christopher D. Entwistle' 'Sofiane Fathallah' 'J. Halet' 'Judith Howard' 'Fatima Ibersiene' 'Jackie Mosely' 'Lars-Olof Palsson' 'Suk-Yue Poon.' 'Andreas Steffen' 'Wai-Yeung Wong.' _publ_contact_author_name 'Todd Marder' _publ_contact_author_email TODD.MARDER@DURHAM.AC.UK _publ_section_title ; Syntheses, Structures, Two-Photon Absorption Cross-Sections and Computed Second Hyperpolarisabilities of Quadrupolar A-?-A Systems Containing E-Dimesitylborylethenyl Acceptors ; # Attachment 'bisboryls.cif' #=========================================================== data_1a _database_code_depnum_ccdc_archive 'CCDC 724814' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,4-bis(E-dimesitylborylethenyl)benzene ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H52 B2' _chemical_formula_sum 'C46 H52 B2' _chemical_formula_weight 626.50 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.3031(7) _cell_length_b 28.945(2) _cell_length_c 15.8034(14) _cell_angle_alpha 90.00 _cell_angle_beta 92.370(11) _cell_angle_gamma 90.00 _cell_volume 3794.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 756 _cell_measurement_theta_min 10.2 _cell_measurement_theta_max 19.1 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.097 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 0.061 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ;The data collection nominally covered full sphere of reciprocal space, by a combination of 6 sets of \w scans; each set at different \f and/or 2\q angles and each scan (30 sec exposure) covering 0.3\% in \w. Crystal to detector distance 4.85 cm. ; _diffrn_ambient_temperature 120(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 'SMART 6000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8 _diffrn_standards_decay_% 0 _diffrn_reflns_number 78404 _diffrn_reflns_av_R_equivalents 0.0559 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 30.00 _reflns_number_total 11080 _reflns_number_gt 6916 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'SMART version 5.625 (Bruker, 2001)' _computing_data_reduction 'SAINT version 6.02A (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL version 6.12 (Bruker, 2001)' _computing_publication_material 'SHELXTL version 6.12 (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. Methyl groups C(18)H~3~, C(28)H~3~ and C(49)H~3~ were treated as ideally dosordered, other methyl groups as rigid bodies, with a common refined U for three H atoms. Other H atoms in riding model. ; _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^)+(0.0749P)^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 11080 _refine_ls_number_parameters 463 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0830 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1406 _refine_ls_wR_factor_gt 0.1239 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 C1 C 0.62436(17) 0.71043(5) 0.32136(8) 0.0330(3) Uani 1 1 d . . . H1 H 0.5472 0.7181 0.3619 0.040 Uiso 1 1 d R . . C2 C 0.73522(16) 0.67794(4) 0.34147(8) 0.0292(3) Uani 1 1 d . . . H2 H 0.8136 0.6720 0.3007 0.035 Uiso 1 1 d R . . C3 C 0.74837(15) 0.65057(4) 0.41952(8) 0.0271(3) Uani 1 1 d . . . C4 C 0.66002(16) 0.66080(4) 0.49049(8) 0.0308(3) Uani 1 1 d . . . H4 H 0.5976 0.6883 0.4914 0.037 Uiso 1 1 d R . . C5 C 0.66288(16) 0.63147(4) 0.55918(8) 0.0290(3) Uani 1 1 d . . . H5 H 0.6010 0.6389 0.6065 0.035 Uiso 1 1 d R . . C6 C 0.75485(15) 0.59089(4) 0.56061(8) 0.0253(2) Uani 1 1 d . . . C7 C 0.84978(16) 0.58194(4) 0.49128(8) 0.0291(3) Uani 1 1 d . . . H7 H 0.9166 0.5553 0.4917 0.035 Uiso 1 1 d R . . C8 C 0.84716(15) 0.61133(4) 0.42228(8) 0.0293(3) Uani 1 1 d . . . H8 H 0.9136 0.6049 0.3762 0.035 Uiso 1 1 d R . . C9 C 0.73883(15) 0.55890(4) 0.63140(8) 0.0281(3) Uani 1 1 d . . . H9 H 0.6715 0.5689 0.6750 0.034 Uiso 1 1 d R . . C10 C 0.80760(16) 0.51720(4) 0.64284(8) 0.0301(3) Uani 1 1 d . . . H10 H 0.8952 0.5086 0.6093 0.036 Uiso 1 1 d R . . C11 C 0.50156(15) 0.77894(4) 0.22107(8) 0.0274(3) Uani 1 1 d . . . C12 C 0.39829(15) 0.78335(4) 0.14794(8) 0.0270(3) Uani 1 1 d . . . C13 C 0.29775(15) 0.82147(4) 0.13759(8) 0.0298(3) Uani 1 1 d . . . H13 H 0.2281 0.8233 0.0885 0.036 Uiso 1 1 d R . . C14 C 0.29510(16) 0.85705(5) 0.19647(9) 0.0325(3) Uani 1 1 d . . . C15 C 0.39790(17) 0.85327(5) 0.26756(8) 0.0342(3) Uani 1 1 d . . . H15 H 0.3998 0.8774 0.3083 0.041 Uiso 1 1 d R . . C16 C 0.49820(17) 0.81524(5) 0.28136(8) 0.0324(3) Uani 1 1 d . . . C17 C 0.38885(17) 0.74644(5) 0.08000(8) 0.0332(3) Uani 1 1 d . . . H171 H 0.3412(11) 0.7184(3) 0.1029(3) 0.043(2) Uiso 1 1 d R . . H172 H 0.4972(9) 0.7396(2) 0.0614(4) 0.043(2) Uiso 1 1 d R . . H173 H 0.3219(10) 0.75750(16) 0.0318(5) 0.043(2) Uiso 1 1 d R . . C18 C 0.1852(2) 0.89802(5) 0.18386(11) 0.0454(4) Uani 1 1 d . . . H181 H 0.1006 0.8969 0.2253 0.052(4) Uiso 0.50 1 d PR A 1 H182 H 0.1358 0.8973 0.1265 0.052(4) Uiso 0.50 1 d PR A 1 H183 H 0.2476 0.9266 0.1917 0.052(4) Uiso 0.50 1 d PR A 1 H184 H 0.2221 0.9169 0.1370 0.052(4) Uiso 0.50 1 d PR A 2 H185 H 0.1868 0.9166 0.2358 0.052(4) Uiso 0.50 1 d PR A 2 H186 H 0.0751 0.8873 0.1706 0.052(4) Uiso 0.50 1 d PR A 2 C19 C 0.6059(2) 0.81591(6) 0.36105(10) 0.0491(4) Uani 1 1 d . . . H191 H 0.6416(13) 0.8476(4) 0.3728(5) 0.081(4) Uiso 1 1 d R . . H192 H 0.7000(13) 0.7962(4) 0.3532(3) 0.081(4) Uiso 1 1 d R . . H193 H 0.5457(8) 0.8044(4) 0.4088(6) 0.081(4) Uiso 1 1 d R . . C21 C 0.72795(15) 0.71835(4) 0.16296(8) 0.0285(3) Uani 1 1 d . . . C22 C 0.70754(16) 0.67472(4) 0.12390(8) 0.0311(3) Uani 1 1 d . . . C23 C 0.80768(17) 0.66153(5) 0.05945(8) 0.0320(3) Uani 1 1 d . . . H23 H 0.7928 0.6319 0.0344 0.038 Uiso 1 1 d R . . C24 C 0.92830(16) 0.68990(5) 0.03081(8) 0.0321(3) Uani 1 1 d . . . C25 C 0.94845(16) 0.73296(5) 0.06985(9) 0.0331(3) Uani 1 1 d . . . H25 H 1.0300 0.7531 0.0513 0.040 Uiso 1 1 d R . . C26 C 0.85248(15) 0.74704(4) 0.13505(8) 0.0291(3) Uani 1 1 d . . . C27 C 0.57395(19) 0.64182(5) 0.14688(10) 0.0429(4) Uani 1 1 d . . . H271 H 0.4948(12) 0.6405(3) 0.1014(6) 0.084(4) Uiso 1 1 d R . . H272 H 0.5251(12) 0.6526(3) 0.1969(7) 0.084(4) Uiso 1 1 d R . . H273 H 0.6178(6) 0.6117(3) 0.1568(8) 0.084(4) Uiso 1 1 d R . . C28 C 1.0346(2) 0.67478(5) -0.03905(10) 0.0427(4) Uani 1 1 d . . . H281 H 1.0093 0.6931 -0.0900 0.056(4) Uiso 0.50 1 d PR B 1 H282 H 1.0157 0.6420 -0.0514 0.056(4) Uiso 0.50 1 d PR B 1 H283 H 1.1478 0.6794 -0.0212 0.056(4) Uiso 0.50 1 d PR B 1 H284 H 1.1059 0.6499 -0.0184 0.056(4) Uiso 0.50 1 d PR B 2 H285 H 1.0995 0.7010 -0.0570 0.056(4) Uiso 0.50 1 d PR B 2 H286 H 0.9674 0.6636 -0.0872 0.056(4) Uiso 0.50 1 d PR B 2 C29 C 0.88937(17) 0.79297(5) 0.17774(10) 0.0379(3) Uani 1 1 d . . . H291 H 0.9671(13) 0.78809(8) 0.2263(6) 0.069(3) Uiso 1 1 d R . . H292 H 0.7885(10) 0.8065(2) 0.1984(6) 0.069(3) Uiso 1 1 d R . . H293 H 0.9368(13) 0.8144(2) 0.1365(4) 0.069(3) Uiso 1 1 d R . . C31 C 0.64137(15) 0.50234(4) 0.78265(8) 0.0265(3) Uani 1 1 d . . . C32 C 0.47508(16) 0.49201(4) 0.78365(8) 0.0288(3) Uani 1 1 d . . . C33 C 0.38172(17) 0.51018(5) 0.84694(8) 0.0325(3) Uani 1 1 d . . . H33 H 0.2700 0.5030 0.8465 0.039 Uiso 1 1 d R . . C34 C 0.44647(17) 0.53854(4) 0.91055(8) 0.0329(3) Uani 1 1 d . . . C35 C 0.60850(17) 0.54880(4) 0.90873(8) 0.0330(3) Uani 1 1 d . . . H35 H 0.6552 0.5681 0.9517 0.040 Uiso 1 1 d R . . C36 C 0.70627(16) 0.53193(4) 0.84613(8) 0.0296(3) Uani 1 1 d . . . C37 C 0.39251(18) 0.46380(5) 0.71440(9) 0.0386(3) Uani 1 1 d . . . H371 H 0.2827(11) 0.4573(3) 0.7292(3) 0.051(3) Uiso 1 1 d R . . H372 H 0.4502(9) 0.4350(3) 0.7078(4) 0.051(3) Uiso 1 1 d R . . H373 H 0.3917(10) 0.4809(2) 0.6618(5) 0.051(3) Uiso 1 1 d R . . C38 C 0.3427(2) 0.55801(6) 0.97813(10) 0.0450(4) Uani 1 1 d . . . H381 H 0.3962(9) 0.5526(4) 1.0350(6) 0.084(4) Uiso 1 1 d R . . H382 H 0.2353(13) 0.5424(4) 0.9752(5) 0.084(4) Uiso 1 1 d R . . H383 H 0.3280(13) 0.5919(4) 0.9689(5) 0.084(4) Uiso 1 1 d R . . C39 C 0.88193(18) 0.54590(5) 0.84947(10) 0.0425(4) Uani 1 1 d . . . H391 H 0.8907(2) 0.5787(4) 0.8367(8) 0.077(4) Uiso 1 1 d R . . H392 H 0.9393(7) 0.5281(3) 0.8079(7) 0.077(4) Uiso 1 1 d R . . H393 H 0.9291(7) 0.5399(4) 0.9059(6) 0.077(4) Uiso 1 1 d R . . C41 C 0.77646(15) 0.42928(4) 0.69750(8) 0.0273(3) Uani 1 1 d . . . C42 C 0.84511(15) 0.40176(4) 0.76372(8) 0.0281(3) Uani 1 1 d . . . C43 C 0.86384(16) 0.35425(4) 0.75302(8) 0.0306(3) Uani 1 1 d . . . H43 H 0.9123 0.3365 0.7978 0.037 Uiso 1 1 d R . . C44 C 0.81372(16) 0.33225(4) 0.67857(9) 0.0320(3) Uani 1 1 d . . . C45 C 0.74708(16) 0.35918(5) 0.61352(9) 0.0340(3) Uani 1 1 d . . . H45 H 0.7113 0.3446 0.5623 0.041 Uiso 1 1 d R . . C46 C 0.73092(16) 0.40685(4) 0.62055(8) 0.0304(3) Uani 1 1 d . . . C47 C 0.90812(19) 0.42284(5) 0.84583(8) 0.0370(3) Uani 1 1 d . . . H471 H 0.9188(13) 0.3992(2) 0.8884(5) 0.065(3) Uiso 1 1 d R . . H472 H 0.8343(10) 0.4461(3) 0.8638(4) 0.065(3) Uiso 1 1 d R . . H473 H 1.0116(12) 0.4366(4) 0.8376(2) 0.065(3) Uiso 1 1 d R . . C48 C 0.83668(19) 0.28099(5) 0.66770(11) 0.0425(4) Uani 1 1 d . . . H481 H 0.7640(13) 0.26985(16) 0.6224(8) 0.088(4) Uiso 1 1 d R . . H482 H 0.8133(15) 0.26526(19) 0.7201(6) 0.088(4) Uiso 1 1 d R . . H483 H 0.9474(13) 0.27477(10) 0.6535(8) 0.088(4) Uiso 1 1 d R . . C49 C 0.6592(2) 0.43255(5) 0.54448(9) 0.0429(4) Uani 1 1 d . . . H491 H 0.6229 0.4103 0.5010 0.051(4) Uiso 0.50 1 d PR C 1 H492 H 0.7411 0.4529 0.5215 0.051(4) Uiso 0.50 1 d PR C 1 H493 H 0.5674 0.4511 0.5617 0.051(4) Uiso 0.50 1 d PR C 1 H494 H 0.6646 0.4659 0.5551 0.051(4) Uiso 0.50 1 d PR C 2 H495 H 0.5465 0.4233 0.5346 0.051(4) Uiso 0.50 1 d PR C 2 H496 H 0.7202 0.4251 0.4945 0.051(4) Uiso 0.50 1 d PR C 2 B1 B 0.61679(18) 0.73596(5) 0.23524(9) 0.0296(3) Uani 1 1 d . . . B2 B 0.74665(17) 0.48282(5) 0.70919(9) 0.0265(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 0.0322(7) 0.0351(7) 0.0317(7) 0.0044(5) 0.0026(5) 0.0031(5) C2 0.0284(7) 0.0302(6) 0.0288(6) 0.0030(5) 0.0005(5) -0.0017(5) C3 0.0262(6) 0.0280(6) 0.0270(6) 0.0024(5) -0.0003(5) -0.0019(5) C4 0.0338(7) 0.0273(6) 0.0313(7) 0.0007(5) 0.0015(5) 0.0052(5) C5 0.0317(7) 0.0283(6) 0.0272(6) -0.0019(5) 0.0042(5) 0.0024(5) C6 0.0252(6) 0.0253(6) 0.0254(6) -0.0003(5) 0.0003(5) -0.0009(5) C7 0.0287(7) 0.0280(6) 0.0308(6) 0.0026(5) 0.0038(5) 0.0042(5) C8 0.0283(7) 0.0324(7) 0.0274(6) 0.0024(5) 0.0038(5) 0.0017(5) C9 0.0301(7) 0.0282(6) 0.0262(6) 0.0002(5) 0.0032(5) 0.0000(5) C10 0.0307(7) 0.0291(6) 0.0308(6) 0.0022(5) 0.0058(5) 0.0017(5) C11 0.0268(6) 0.0290(6) 0.0265(6) 0.0033(5) 0.0008(5) -0.0029(5) C12 0.0248(6) 0.0295(6) 0.0267(6) 0.0022(5) 0.0026(5) -0.0049(5) C13 0.0249(6) 0.0350(7) 0.0293(6) 0.0046(5) 0.0000(5) -0.0015(5) C14 0.0289(7) 0.0324(7) 0.0361(7) 0.0025(5) 0.0024(5) 0.0004(5) C15 0.0377(8) 0.0327(7) 0.0322(7) -0.0042(5) 0.0023(6) 0.0014(6) C16 0.0350(7) 0.0344(7) 0.0277(6) 0.0010(5) -0.0025(5) -0.0010(6) C17 0.0335(7) 0.0348(7) 0.0307(7) -0.0014(5) -0.0049(5) -0.0003(6) C18 0.0457(9) 0.0405(8) 0.0497(9) -0.0021(7) -0.0014(7) 0.0119(7) C19 0.0628(11) 0.0442(9) 0.0389(8) -0.0074(7) -0.0171(8) 0.0058(8) C21 0.0288(7) 0.0273(6) 0.0289(6) 0.0054(5) -0.0039(5) 0.0007(5) C22 0.0340(7) 0.0265(6) 0.0323(7) 0.0056(5) -0.0046(5) -0.0011(5) C23 0.0372(7) 0.0268(6) 0.0312(7) 0.0003(5) -0.0077(5) 0.0011(5) C24 0.0317(7) 0.0331(7) 0.0311(7) 0.0034(5) -0.0035(5) 0.0043(5) C25 0.0283(7) 0.0309(7) 0.0399(7) 0.0042(6) 0.0011(5) -0.0009(5) C26 0.0255(6) 0.0267(6) 0.0347(7) 0.0027(5) -0.0039(5) 0.0003(5) C27 0.0489(9) 0.0315(7) 0.0484(9) 0.0016(6) 0.0024(7) -0.0100(6) C28 0.0450(9) 0.0420(8) 0.0413(8) -0.0028(6) 0.0048(7) 0.0034(7) C29 0.0312(7) 0.0309(7) 0.0516(9) -0.0040(6) 0.0004(6) -0.0027(6) C31 0.0308(7) 0.0220(6) 0.0270(6) 0.0044(5) 0.0033(5) 0.0006(5) C32 0.0304(7) 0.0267(6) 0.0295(6) 0.0041(5) 0.0020(5) 0.0001(5) C33 0.0295(7) 0.0334(7) 0.0350(7) 0.0059(5) 0.0053(5) 0.0032(5) C34 0.0392(8) 0.0291(6) 0.0308(7) 0.0039(5) 0.0080(6) 0.0074(6) C35 0.0427(8) 0.0264(6) 0.0299(7) -0.0021(5) 0.0016(6) 0.0011(6) C36 0.0326(7) 0.0270(6) 0.0294(6) 0.0023(5) 0.0030(5) -0.0015(5) C37 0.0314(7) 0.0435(8) 0.0408(8) -0.0046(6) 0.0008(6) -0.0057(6) C38 0.0504(9) 0.0445(9) 0.0410(8) -0.0009(7) 0.0143(7) 0.0121(7) C39 0.0393(9) 0.0456(9) 0.0424(8) -0.0079(7) 0.0012(6) -0.0097(7) C41 0.0279(7) 0.0275(6) 0.0268(6) 0.0014(5) 0.0038(5) 0.0011(5) C42 0.0277(6) 0.0310(6) 0.0260(6) 0.0025(5) 0.0053(5) 0.0034(5) C43 0.0292(7) 0.0294(6) 0.0334(7) 0.0052(5) 0.0054(5) 0.0040(5) C44 0.0275(7) 0.0267(6) 0.0420(7) 0.0002(5) 0.0046(5) 0.0009(5) C45 0.0337(7) 0.0326(7) 0.0355(7) -0.0059(5) -0.0010(6) 0.0000(5) C46 0.0312(7) 0.0304(7) 0.0294(6) 0.0002(5) 0.0005(5) 0.0012(5) C47 0.0464(9) 0.0385(8) 0.0260(6) -0.0001(5) -0.0004(6) 0.0120(6) C48 0.0397(8) 0.0276(7) 0.0600(10) -0.0030(6) -0.0011(7) 0.0012(6) C49 0.0579(10) 0.0374(8) 0.0323(7) -0.0024(6) -0.0098(7) 0.0043(7) B1 0.0279(8) 0.0291(7) 0.0313(7) 0.0034(6) -0.0040(6) -0.0043(6) B2 0.0255(7) 0.0288(7) 0.0250(7) 0.0015(5) -0.0017(5) -0.0001(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 1.3447(18) . ? C1 B1 1.5476(19) . ? C2 C3 1.4665(17) . ? C3 C4 1.3970(17) . ? C3 C8 1.4006(18) . ? C4 C5 1.3776(17) . ? C5 C6 1.4007(17) . ? C6 C7 1.4000(17) . ? C6 C9 1.4626(17) . ? C7 C8 1.3824(17) . ? C9 C10 1.3442(17) . ? C10 B2 1.5458(18) . ? C11 C12 1.4160(17) . ? C11 C16 1.4196(18) . ? C11 B1 1.580(2) . ? C12 C13 1.3893(18) . ? C12 C17 1.5145(18) . ? C13 C14 1.3887(18) . ? C14 C15 1.3869(19) . ? C14 C18 1.504(2) . ? C15 C16 1.3921(19) . ? C16 C19 1.5141(19) . ? C21 C26 1.4109(18) . ? C21 C22 1.4128(18) . ? C21 B1 1.582(2) . ? C22 C23 1.3945(19) . ? C22 C27 1.5174(19) . ? C23 C24 1.3856(19) . ? C24 C25 1.3976(19) . ? C24 C28 1.507(2) . ? C25 C26 1.3894(19) . ? C26 C29 1.5165(18) . ? C31 C36 1.4092(18) . ? C31 C32 1.4134(18) . ? C31 B2 1.5858(19) . ? C32 C33 1.3936(18) . ? C32 C37 1.5075(19) . ? C33 C34 1.3886(19) . ? C34 C35 1.379(2) . ? C34 C38 1.5089(19) . ? C35 C36 1.3938(18) . ? C36 C39 1.512(2) . ? C41 C42 1.4160(17) . ? C41 C46 1.4162(18) . ? C41 B2 1.5814(19) . ? C42 C43 1.3951(18) . ? C42 C47 1.5078(18) . ? C43 C44 1.3865(19) . ? C44 C45 1.3870(19) . ? C44 C48 1.5066(19) . ? C45 C46 1.3911(18) . ? C46 C49 1.5145(19) . ? 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 B1 122.97(13) . . ? C1 C2 C3 127.09(12) . . ? C4 C3 C8 118.25(11) . . ? C4 C3 C2 122.50(12) . . ? C8 C3 C2 119.18(11) . . ? C5 C4 C3 120.62(12) . . ? C4 C5 C6 121.41(12) . . ? C7 C6 C5 117.83(11) . . ? C7 C6 C9 123.60(11) . . ? C5 C6 C9 118.45(11) . . ? C8 C7 C6 120.82(12) . . ? C7 C8 C3 120.90(12) . . ? C10 C9 C6 128.30(12) . . ? C9 C10 B2 121.34(12) . . ? C12 C11 C16 116.94(11) . . ? C12 C11 B1 121.98(11) . . ? C16 C11 B1 121.09(11) . . ? C13 C12 C11 120.56(12) . . ? C13 C12 C17 117.62(11) . . ? C11 C12 C17 121.79(11) . . ? C14 C13 C12 122.42(12) . . ? C15 C14 C13 117.26(12) . . ? C15 C14 C18 121.27(13) . . ? C13 C14 C18 121.47(13) . . ? C14 C15 C16 122.25(12) . . ? C15 C16 C11 120.55(12) . . ? C15 C16 C19 116.69(12) . . ? C11 C16 C19 122.71(12) . . ? C26 C21 C22 117.76(12) . . ? C26 C21 B1 119.54(11) . . ? C22 C21 B1 122.70(12) . . ? C23 C22 C21 119.97(12) . . ? C23 C22 C27 117.82(12) . . ? C21 C22 C27 122.15(13) . . ? C24 C23 C22 122.48(12) . . ? C23 C24 C25 117.35(13) . . ? C23 C24 C28 121.34(13) . . ? C25 C24 C28 121.31(13) . . ? C26 C25 C24 121.81(13) . . ? C25 C26 C21 120.62(12) . . ? C25 C26 C29 118.39(12) . . ? C21 C26 C29 120.94(12) . . ? C36 C31 C32 117.74(11) . . ? C36 C31 B2 122.11(11) . . ? C32 C31 B2 120.08(11) . . ? C33 C32 C31 120.06(12) . . ? C33 C32 C37 118.41(12) . . ? C31 C32 C37 121.44(12) . . ? C34 C33 C32 122.17(13) . . ? C35 C34 C33 117.45(12) . . ? C35 C34 C38 121.35(13) . . ? C33 C34 C38 121.19(13) . . ? C34 C35 C36 122.45(12) . . ? C35 C36 C31 120.10(12) . . ? C35 C36 C39 118.08(12) . . ? C31 C36 C39 121.82(12) . . ? C42 C41 C46 117.50(11) . . ? C42 C41 B2 121.68(11) . . ? C46 C41 B2 120.80(11) . . ? C43 C42 C41 120.56(12) . . ? C43 C42 C47 117.82(12) . . ? C41 C42 C47 121.54(11) . . ? C44 C43 C42 121.64(12) . . ? C43 C44 C45 117.86(12) . . ? C43 C44 C48 120.94(13) . . ? C45 C44 C48 121.16(13) . . ? C44 C45 C46 122.35(13) . . ? C45 C46 C41 120.01(12) . . ? C45 C46 C49 117.38(12) . . ? C41 C46 C49 122.59(12) . . ? C1 B1 C11 120.20(12) . . ? C1 B1 C21 118.51(12) . . ? C11 B1 C21 121.28(11) . . ? C10 B2 C41 119.63(11) . . ? C10 B2 C31 118.23(11) . . ? C41 B2 C31 121.89(11) . . ? 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 C22 C21 B1 C1 65.99(17) . . . . ? C21 B1 C1 C2 8.8(2) . . . . ? B1 C1 C2 C3 -177.29(12) . . . . ? C1 C2 C3 C4 -11.3(2) . . . . ? C16 C11 B1 C1 47.99(18) . . . . ? C36 C31 B2 C10 -67.46(16) . . . . ? C31 B2 C10 C9 -19.04(19) . . . . ? B2 C10 C9 C6 -164.77(12) . . . . ? C10 C9 C6 C7 -0.2(2) . . . . ? C46 C41 B2 C10 -52.23(17) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.274 _refine_diff_density_min -0.172 _refine_diff_density_rms 0.040 #=====================================END data_1a' _database_code_depnum_ccdc_archive 'CCDC 724815' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,4-bis(E-dimesitylborylethenyl)benzene, toluene trisolvate ; _chemical_name_common . _chemical_melting_point . _chemical_formula_moiety 'C46 H52 B2,3(C7 H8)' _chemical_formula_sum 'C67 H76 B2' _chemical_formula_weight 902.90 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.144(2) _cell_length_b 11.4882(15) _cell_length_c 16.240(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.46(2) _cell_angle_gamma 90.00 _cell_volume 2787.1(6) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 887 _cell_measurement_theta_min 12.0 _cell_measurement_theta_max 21.0 _exptl_crystal_description plate _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.076 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 0.060 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9566 _exptl_absorpt_correction_T_max 0.9911 _exptl_absorpt_process_details 'SADABS (G.M.Sheldrick, 1998)' _exptl_special_details ; The data collection nominally covered full sphere of reciprocal Space, by a combination of 5 sets of \w scans each set at different \f and/or 2\q angles and each scan (10s exposure) covering 0.3\% in \w. Crystal to detector distance 4.53 cm. ; _diffrn_ambient_temperature 110(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 'Bruker SMART CCD 1K area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8 _diffrn_standards_number 0 _diffrn_reflns_number 28754 _diffrn_reflns_av_R_equivalents 0.0537 _diffrn_reflns_av_sigmaI/netI 0.0477 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6398 _reflns_number_gt 4142 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART version 5.054 (Bruker, 1999)' _computing_cell_refinement 'SMART version 5.054 (Bruker, 1999)' _computing_data_reduction 'SAINT version 6.02A (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXTL version 6.14 (Bruker, 2003)' _computing_molecular_graphics 'SHELXTL version 6.14 (Bruker, 2003)' _computing_publication_material 'SHELXTL version 6.14 (Bruker, 2003)' _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. Methyl groups were refined as rigid bodies rotating around C---C bonds, with a common refined U for three H atoms. Olefinic hydrogens H(1) and H(2): refall, other H atoms: riding model (constr). Toluene molecule I [(C(31) to C(37) with attached hydrogens] is disordered between two overlapping positions, A and B, with occupancies 0.75 and 0.25, respectively. Toluene molecule II [(C(41) to C(47) with attached hydrogens] is disordered between two, partially overlapping, positions related by a crystallographic inversion centre. All toluene aryl rings were refined as rigid bodies with idealised hexagonal geometry. ; _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^)+(0.0517P)^2^+1.1298P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6398 _refine_ls_number_parameters 392 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0940 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.1418 _refine_ls_wR_factor_gt 0.1183 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.023 _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 B B 0.84545(12) 0.48047(16) 0.27307(11) 0.0239(4) Uani 1 1 d . . . C1 C 0.91340(11) 0.49665(15) 0.21187(10) 0.0256(4) Uani 1 1 d . . . H1 H 0.9760(12) 0.5199(15) 0.2339(11) 0.027(5) Uiso 1 1 d . . . C2 C 0.89161(11) 0.47940(14) 0.12903(10) 0.0225(3) Uani 1 1 d . . . H2 H 0.8312(11) 0.4569(15) 0.1063(10) 0.021(4) Uiso 1 1 d . . . C3 C 0.94827(10) 0.49150(13) 0.06473(9) 0.0209(3) Uani 1 1 d . . . C4 C 1.03694(10) 0.53010(14) 0.08102(10) 0.0220(3) Uani 1 1 d . . . H4 H 1.0627 0.5509 0.1364 0.026 Uiso 1 1 d R . . C5 C 1.08752(10) 0.53832(14) 0.01801(10) 0.0221(3) Uani 1 1 d . . . H5 H 1.1477 0.5645 0.0307 0.027 Uiso 1 1 d R . . C11 C 0.75437(10) 0.41793(15) 0.23786(10) 0.0240(3) Uani 1 1 d . . . C12 C 0.67256(11) 0.47793(16) 0.23417(10) 0.0287(4) Uani 1 1 d . . . C13 C 0.59251(11) 0.42599(17) 0.19801(11) 0.0339(4) Uani 1 1 d . . . H13 H 0.5381 0.4678 0.1962 0.041 Uiso 1 1 d R . . C14 C 0.58979(12) 0.31483(17) 0.16480(11) 0.0338(4) Uani 1 1 d . . . C15 C 0.66980(11) 0.25507(16) 0.16906(10) 0.0298(4) Uani 1 1 d . . . H15 H 0.6692 0.1786 0.1467 0.036 Uiso 1 1 d R . . C16 C 0.75116(11) 0.30386(15) 0.20511(10) 0.0259(4) Uani 1 1 d . . . C17 C 0.66982(13) 0.60117(17) 0.26695(14) 0.0413(5) Uani 1 1 d . . . H171 H 0.6088 0.6318 0.2532 0.067(4) Uiso 1 1 d R . . H172 H 0.7107 0.6504 0.2414 0.067(4) Uiso 1 1 d R . . H173 H 0.6883 0.6009 0.3277 0.067(4) Uiso 1 1 d R . . C18 C 0.50301(13) 0.2611(2) 0.12390(15) 0.0521(6) Uani 1 1 d . . . H181 H 0.4539 0.2916 0.1500 0.086(5) Uiso 1 1 d R . . H182 H 0.5063 0.1764 0.1309 0.086(5) Uiso 1 1 d R . . H183 H 0.4922 0.2801 0.0643 0.086(5) Uiso 1 1 d R . . C19 C 0.83441(12) 0.22955(16) 0.20970(12) 0.0328(4) Uani 1 1 d . . . H191 H 0.8815 0.2600 0.2530 0.056(4) Uiso 1 1 d R . . H192 H 0.8551 0.2312 0.1557 0.056(4) Uiso 1 1 d R . . H193 H 0.8204 0.1493 0.2233 0.056(4) Uiso 1 1 d R . . C21 C 0.86756(10) 0.52851(14) 0.36497(10) 0.0237(3) Uani 1 1 d . . . C22 C 0.90088(11) 0.64290(15) 0.38128(10) 0.0254(4) Uani 1 1 d . . . C23 C 0.91985(11) 0.68483(15) 0.46264(10) 0.0269(4) Uani 1 1 d . . . H23A H 0.9416 0.7621 0.4719 0.032 Uiso 1 1 d R . . C24 C 0.90800(11) 0.61707(15) 0.53044(10) 0.0273(4) Uani 1 1 d . . . C25 C 0.87598(12) 0.50514(15) 0.51496(10) 0.0291(4) Uani 1 1 d . . . H25A H 0.8680 0.4574 0.5609 0.035 Uiso 1 1 d R . . C26 C 0.85511(11) 0.45974(15) 0.43463(10) 0.0262(4) Uani 1 1 d . . . C27 C 0.91228(13) 0.72703(16) 0.31199(11) 0.0338(4) Uani 1 1 d . . . H271 H 0.9155 0.8067 0.3337 0.075(5) Uiso 1 1 d R . . H272 H 0.8612 0.7201 0.2666 0.075(5) Uiso 1 1 d R . . H273 H 0.9676 0.7087 0.2908 0.075(5) Uiso 1 1 d R . . C28 C 0.92814(13) 0.66393(17) 0.61823(11) 0.0372(5) Uani 1 1 d . . . H281 H 0.9242 0.7490 0.6168 0.094(6) Uiso 1 1 d R . . H282 H 0.9886 0.6405 0.6439 0.094(6) Uiso 1 1 d R . . H283 H 0.8847 0.6329 0.6510 0.094(6) Uiso 1 1 d R . . C29 C 0.82199(15) 0.33587(16) 0.42573(12) 0.0410(5) Uani 1 1 d . . . H291 H 0.8120 0.3067 0.4801 0.073(5) Uiso 1 1 d R . . H292 H 0.8667 0.2873 0.4050 0.073(5) Uiso 1 1 d R . . H293 H 0.7657 0.3332 0.3862 0.073(5) Uiso 1 1 d R . . C31A C 0.3085(3) 0.4191(3) 0.03437(19) 0.0456(10) Uani 0.75 1 d PG A 1 C32A C 0.2902(3) 0.4123(3) 0.1153(2) 0.0660(16) Uani 0.75 1 d PG A 1 H32A H 0.2642 0.3438 0.1336 0.079 Uiso 0.75 1 d PR A 1 C33A C 0.3101(3) 0.5058(4) 0.16953(14) 0.084(2) Uani 0.75 1 d PG A 1 H33A H 0.2976 0.5011 0.2249 0.101 Uiso 0.75 1 d PR A 1 C34A C 0.3482(2) 0.6060(3) 0.14277(16) 0.0773(14) Uani 0.75 1 d PG A 1 H34A H 0.3618 0.6699 0.1798 0.093 Uiso 0.75 1 d PR A 1 C35A C 0.3665(2) 0.6128(3) 0.06181(18) 0.0579(10) Uani 0.75 1 d PG A 1 H35A H 0.3925 0.6813 0.0435 0.070 Uiso 0.75 1 d PR A 1 C36A C 0.3466(3) 0.5193(3) 0.00762(14) 0.0424(12) Uani 0.75 1 d PG A 1 H36A H 0.3591 0.5240 -0.0477 0.051 Uiso 0.75 1 d PR A 1 C37A C 0.2894(2) 0.3183(3) -0.0261(3) 0.0662(10) Uani 0.75 1 d P A 1 H37A H 0.2843 0.2460 0.0048 0.099 Uiso 0.75 1 d PR A 1 H38A H 0.3383 0.3109 -0.0585 0.099 Uiso 0.75 1 d PR A 1 H39A H 0.2332 0.3328 -0.0641 0.099 Uiso 0.75 1 d PR A 1 C31B C 0.3594(6) 0.5663(6) 0.0882(5) 0.043(3) Uani 0.25 1 d PG B 2 C32B C 0.3491(8) 0.5004(9) 0.0155(4) 0.052(5) Uani 0.25 1 d PG B 2 H32B H 0.3718 0.5283 -0.0319 0.063 Uiso 0.25 1 d PR B 2 C33B C 0.3055(9) 0.3936(9) 0.0122(6) 0.050(3) Uani 0.25 1 d PG B 2 H33B H 0.2985 0.3486 -0.0375 0.060 Uiso 0.25 1 d PR B 2 C34B C 0.2723(6) 0.3527(7) 0.0817(7) 0.070(4) Uani 0.25 1 d PG B 2 H34B H 0.2426 0.2797 0.0794 0.084 Uiso 0.25 1 d PR B 2 C35B C 0.2827(6) 0.4186(9) 0.1544(5) 0.067(4) Uani 0.25 1 d PG B 2 H35B H 0.2600 0.3906 0.2018 0.081 Uiso 0.25 1 d PR B 2 C36B C 0.3262(6) 0.5254(9) 0.1577(4) 0.040(3) Uani 0.25 1 d PG B 2 H36B H 0.3333 0.5704 0.2073 0.049 Uiso 0.25 1 d PR B 2 C37B C 0.4107(9) 0.6715(12) 0.0941(9) 0.087(4) Uani 0.25 1 d P B 2 H37B H 0.3874 0.7228 0.0469 0.131 Uiso 0.25 1 d PR B 2 H38B H 0.4742 0.6545 0.0925 0.131 Uiso 0.25 1 d PR B 2 H39B H 0.4062 0.7121 0.1466 0.131 Uiso 0.25 1 d PR B 2 C41 C 0.4721(7) 0.0532(9) -0.0508(3) 0.097(4) Uani 0.50 1 d PG C -1 C42 C 0.4139(7) 0.0105(9) -0.0002(6) 0.104(4) Uani 0.50 1 d PG C -1 H42 H 0.3513 0.0236 -0.0148 0.125 Uiso 0.50 1 d PR C -1 C43 C 0.4472(10) -0.0514(9) 0.0717(5) 0.122(6) Uani 0.50 1 d PG C -1 H43 H 0.4074 -0.0806 0.1063 0.146 Uiso 0.50 1 d PR C -1 C44 C 0.5387(11) -0.0705(9) 0.0930(4) 0.119(5) Uani 0.50 1 d PG C -1 H44 H 0.5615 -0.1128 0.1422 0.143 Uiso 0.50 1 d PR C -1 C45 C 0.5969(8) -0.0278(9) 0.0424(7) 0.134(7) Uani 0.50 1 d PG C -1 H45 H 0.6594 -0.0409 0.0570 0.161 Uiso 0.50 1 d PR C -1 C46 C 0.5636(7) 0.0341(9) -0.0295(6) 0.109(5) Uani 0.50 1 d PG C -1 H46 H 0.6033 0.0633 -0.0641 0.131 Uiso 0.50 1 d PR C -1 C47 C 0.4336(12) 0.1144(15) -0.1276(9) 0.208(9) Uani 0.50 1 d P C -1 H47 H 0.4813 0.1371 -0.1583 0.313 Uiso 0.50 1 d PR C -1 H48 H 0.3851 0.0769 -0.1657 0.313 Uiso 0.50 1 d PR C -1 H49 H 0.4104 0.1837 -0.1031 0.313 Uiso 0.50 1 d PR C -1 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 B 0.0306(10) 0.0210(9) 0.0202(9) 0.0009(7) 0.0042(7) 0.0034(7) C1 0.0266(8) 0.0289(9) 0.0212(8) -0.0024(7) 0.0037(6) -0.0013(7) C2 0.0232(8) 0.0227(8) 0.0219(8) -0.0009(6) 0.0047(6) 0.0021(6) C3 0.0256(8) 0.0186(8) 0.0184(8) -0.0005(6) 0.0038(6) 0.0028(6) C4 0.0267(8) 0.0229(8) 0.0158(7) -0.0030(6) 0.0017(6) 0.0012(6) C5 0.0225(7) 0.0217(8) 0.0216(8) -0.0014(6) 0.0021(6) 0.0008(6) C11 0.0264(8) 0.0287(9) 0.0181(8) 0.0005(7) 0.0068(6) 0.0005(7) C12 0.0292(9) 0.0329(10) 0.0257(9) -0.0004(7) 0.0091(7) 0.0009(7) C13 0.0239(8) 0.0429(11) 0.0357(10) 0.0030(8) 0.0076(7) 0.0035(8) C14 0.0281(9) 0.0420(11) 0.0308(10) 0.0040(8) 0.0038(7) -0.0057(8) C15 0.0332(9) 0.0286(9) 0.0273(9) -0.0013(7) 0.0038(7) -0.0050(7) C16 0.0281(8) 0.0291(9) 0.0211(8) -0.0005(7) 0.0058(7) 0.0002(7) C17 0.0356(10) 0.0368(11) 0.0523(13) -0.0080(9) 0.0093(9) 0.0089(8) C18 0.0330(11) 0.0622(15) 0.0590(14) -0.0063(12) 0.0012(10) -0.0109(10) C19 0.0343(10) 0.0290(10) 0.0341(10) -0.0058(8) 0.0027(8) 0.0011(8) C21 0.0265(8) 0.0262(9) 0.0194(8) -0.0014(6) 0.0063(6) 0.0005(7) C22 0.0273(8) 0.0282(9) 0.0212(8) 0.0001(7) 0.0056(7) -0.0020(7) C23 0.0320(9) 0.0255(9) 0.0227(8) -0.0040(7) 0.0029(7) -0.0016(7) C24 0.0321(9) 0.0306(9) 0.0188(8) -0.0021(7) 0.0026(7) 0.0068(7) C25 0.0421(10) 0.0272(9) 0.0197(8) 0.0033(7) 0.0099(7) 0.0054(7) C26 0.0339(9) 0.0250(9) 0.0209(8) 0.0005(7) 0.0078(7) 0.0029(7) C27 0.0473(11) 0.0313(10) 0.0238(9) 0.0006(7) 0.0090(8) -0.0111(8) C28 0.0530(12) 0.0379(11) 0.0196(9) -0.0042(8) 0.0029(8) 0.0048(9) C29 0.0689(14) 0.0272(10) 0.0292(10) 0.0011(8) 0.0153(9) -0.0075(9) C31A 0.041(2) 0.046(2) 0.052(2) 0.0111(19) 0.0144(18) 0.0187(17) C32A 0.057(3) 0.083(4) 0.065(3) 0.037(3) 0.030(2) 0.040(3) C33A 0.089(4) 0.124(6) 0.044(3) 0.028(3) 0.028(3) 0.064(4) C34A 0.097(3) 0.095(3) 0.038(2) -0.015(2) 0.002(2) 0.052(3) C35A 0.073(3) 0.049(3) 0.050(2) -0.0059(19) 0.007(2) 0.007(2) C36A 0.041(2) 0.045(2) 0.042(2) 0.0000(19) 0.0064(18) 0.0035(17) C37A 0.0451(18) 0.0397(19) 0.109(3) -0.006(2) -0.0023(18) 0.0005(15) C31B 0.031(4) 0.050(7) 0.050(7) 0.018(5) 0.008(4) -0.003(4) C32B 0.096(12) 0.054(8) 0.011(5) 0.020(5) 0.021(6) 0.032(8) C33B 0.041(7) 0.049(8) 0.061(8) 0.015(7) 0.011(6) 0.023(6) C34B 0.036(5) 0.049(7) 0.119(12) 0.028(7) -0.001(7) 0.010(5) C35B 0.031(5) 0.100(11) 0.069(10) -0.009(8) 0.002(6) 0.013(6) C36B 0.038(5) 0.061(8) 0.024(5) 0.011(5) 0.010(4) 0.000(5) C37B 0.087(9) 0.083(10) 0.088(10) 0.015(8) 0.004(7) -0.017(7) C41 0.163(11) 0.071(5) 0.065(6) -0.042(5) 0.040(7) -0.020(6) C42 0.174(10) 0.068(6) 0.079(7) -0.045(6) 0.044(6) -0.013(6) C43 0.189(14) 0.073(6) 0.123(9) -0.058(7) 0.085(9) -0.028(7) C44 0.180(14) 0.075(8) 0.102(13) -0.061(10) 0.020(12) 0.006(8) C45 0.116(8) 0.097(9) 0.202(17) -0.105(12) 0.061(9) -0.042(7) C46 0.110(9) 0.082(8) 0.158(14) -0.074(9) 0.094(9) -0.046(6) C47 0.34(2) 0.176(17) 0.088(9) -0.027(9) -0.018(10) 0.006(14) _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 B C1 1.555(2) . ? B C21 1.575(2) . ? B C11 1.577(2) . ? C1 C2 1.346(2) . ? C1 H1 0.994(17) . ? C2 C3 1.463(2) . ? C2 H2 0.964(17) . ? C3 C4 1.398(2) . ? C3 C5 1.406(2) 3_765 ? C4 C5 1.379(2) . ? C4 H4 0.9497 . ? C5 C3 1.406(2) 3_765 ? C5 H5 0.9498 . ? C11 C12 1.410(2) . ? C11 C16 1.412(2) . ? C12 C13 1.392(2) . ? C12 C17 1.516(3) . ? C13 C14 1.384(3) . ? C13 H13 0.9496 . ? C14 C15 1.384(3) . ? C14 C18 1.504(3) . ? C15 C16 1.392(2) . ? C15 H15 0.9498 . ? C16 C19 1.514(2) . ? C17 H171 0.9799 . ? C17 H172 0.9798 . ? C17 H173 0.9799 . ? C18 H181 0.9797 . ? C18 H182 0.9798 . ? C18 H183 0.9797 . ? C19 H191 0.9798 . ? C19 H192 0.9796 . ? C19 H193 0.9798 . ? C21 C22 1.417(2) . ? C21 C26 1.418(2) . ? C22 C23 1.391(2) . ? C22 C27 1.515(2) . ? C23 C24 1.384(2) . ? C23 H23A 0.9497 . ? C24 C25 1.383(2) . ? C24 C28 1.508(2) . ? C25 C26 1.392(2) . ? C25 H25A 0.9498 . ? C26 C29 1.508(2) . ? C27 H271 0.9799 . ? C27 H272 0.9798 . ? C27 H273 0.9798 . ? C28 H281 0.9797 . ? C28 H282 0.9797 . ? C28 H283 0.9797 . ? C29 H291 0.9797 . ? C29 H292 0.9798 . ? C29 H293 0.9796 . ? C31A C32A 1.3896 . ? C31A C36A 1.3897 . ? C31A C37A 1.516(4) . ? C32A C33A 1.3896 . ? C32A H32A 0.9497 . ? C33A C34A 1.3895 . ? C33A H33A 0.9498 . ? C34A C35A 1.3895 . ? C34A H34A 0.9497 . ? C35A C36A 1.3896 . ? C35A H35A 0.9497 . ? C36A H36A 0.9496 . ? C37A H37A 0.9802 . ? C37A H38A 0.9800 . ? C37A H39A 0.9800 . ? C31B C36B 1.3895 . ? C31B C32B 1.3895 . ? C31B C37B 1.432(14) . ? C32B C33B 1.3896 . ? C32B H32B 0.9497 . ? C33B C34B 1.3896 . ? C33B H33B 0.9498 . ? C34B C35B 1.3894 . ? C34B H34B 0.9497 . ? C35B C36B 1.3897 . ? C35B H35B 0.9498 . ? C36B H36B 0.9497 . ? C37B H37B 0.9852 . ? C37B H38B 0.9853 . ? C37B H39B 0.9853 . ? C41 C42 1.3894 . ? C41 C46 1.3896 . ? C41 C47 1.466(16) . ? C42 C43 1.3896 . ? C42 H42 0.9500 . ? C43 C44 1.3896 . ? C43 H43 0.9500 . ? C44 C45 1.3896 . ? C44 H44 0.9500 . ? C45 C46 1.3895 . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 H47 0.9795 . ? C47 H48 0.9797 . ? C47 H49 0.9799 . ? 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 C1 B C21 120.26(15) . . ? C1 B C11 117.00(14) . . ? C21 B C11 122.72(14) . . ? C2 C1 B 122.81(15) . . ? C2 C1 H1 117.5(10) . . ? B C1 H1 119.7(10) . . ? C1 C2 C3 128.54(15) . . ? C1 C2 H2 118.9(10) . . ? C3 C2 H2 112.6(10) . . ? C4 C3 C5 117.76(14) . 3_765 ? C4 C3 C2 123.58(14) . . ? C5 C3 C2 118.66(14) 3_765 . ? C5 C4 C3 121.00(14) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.4 . . ? C4 C5 C3 121.24(14) . 3_765 ? C4 C5 H5 119.4 . . ? C3 C5 H5 119.4 3_765 . ? C12 C11 C16 117.51(15) . . ? C12 C11 B 120.18(15) . . ? C16 C11 B 122.23(14) . . ? C13 C12 C11 120.44(16) . . ? C13 C12 C17 118.46(16) . . ? C11 C12 C17 121.07(16) . . ? C14 C13 C12 121.88(16) . . ? C14 C13 H13 119.0 . . ? C12 C13 H13 119.2 . . ? C13 C14 C15 117.92(16) . . ? C13 C14 C18 121.25(18) . . ? C15 C14 C18 120.82(18) . . ? C14 C15 C16 121.89(17) . . ? C14 C15 H15 119.1 . . ? C16 C15 H15 119.0 . . ? C15 C16 C11 120.35(15) . . ? C15 C16 C19 117.77(16) . . ? C11 C16 C19 121.86(15) . . ? C12 C17 H171 109.6 . . ? C12 C17 H172 109.6 . . ? H171 C17 H172 109.5 . . ? C12 C17 H173 109.3 . . ? H171 C17 H173 109.5 . . ? H172 C17 H173 109.5 . . ? C14 C18 H181 109.4 . . ? C14 C18 H182 109.4 . . ? H181 C18 H182 109.5 . . ? C14 C18 H183 109.6 . . ? H181 C18 H183 109.5 . . ? H182 C18 H183 109.5 . . ? C16 C19 H191 109.7 . . ? C16 C19 H192 109.4 . . ? H191 C19 H192 109.5 . . ? C16 C19 H193 109.4 . . ? H191 C19 H193 109.5 . . ? H192 C19 H193 109.5 . . ? C22 C21 C26 117.24(14) . . ? C22 C21 B 121.06(14) . . ? C26 C21 B 121.70(15) . . ? C23 C22 C21 120.68(15) . . ? C23 C22 C27 116.98(15) . . ? C21 C22 C27 122.24(15) . . ? C24 C23 C22 121.82(16) . . ? C24 C23 H23A 119.1 . . ? C22 C23 H23A 119.1 . . ? C25 C24 C23 117.77(15) . . ? C25 C24 C28 120.96(16) . . ? C23 C24 C28 121.27(16) . . ? C24 C25 C26 122.52(16) . . ? C24 C25 H25A 118.7 . . ? C26 C25 H25A 118.8 . . ? C25 C26 C21 119.97(16) . . ? C25 C26 C29 117.65(15) . . ? C21 C26 C29 122.36(15) . . ? C22 C27 H271 109.5 . . ? C22 C27 H272 109.5 . . ? H271 C27 H272 109.5 . . ? C22 C27 H273 109.4 . . ? H271 C27 H273 109.4 . . ? H272 C27 H273 109.5 . . ? C24 C28 H281 109.3 . . ? C24 C28 H282 109.5 . . ? H281 C28 H282 109.5 . . ? C24 C28 H283 109.6 . . ? H281 C28 H283 109.5 . . ? H282 C28 H283 109.5 . . ? C26 C29 H291 109.6 . . ? C26 C29 H292 109.4 . . ? H291 C29 H292 109.5 . . ? C26 C29 H293 109.4 . . ? H291 C29 H293 109.5 . . ? H292 C29 H293 109.5 . . ? C32A C31A C36A 120.0 . . ? C32A C31A C37A 121.6(2) . . ? C36A C31A C37A 118.4(2) . . ? C33A C32A C31A 120.0 . . ? C33A C32A H32A 120.0 . . ? C31A C32A H32A 120.0 . . ? C34A C33A C32A 120.0 . . ? C34A C33A H33A 120.0 . . ? C32A C33A H33A 120.0 . . ? C33A C34A C35A 120.0 . . ? C33A C34A H34A 120.0 . . ? C35A C34A H34A 120.0 . . ? C34A C35A C36A 120.0 . . ? C34A C35A H35A 120.0 . . ? C36A C35A H35A 120.0 . . ? C35A C36A C31A 120.0 . . ? C35A C36A H36A 120.0 . . ? C31A C36A H36A 120.0 . . ? C36B C31B C32B 120.0 . . ? C36B C31B C37B 119.8(8) . . ? C32B C31B C37B 120.0(8) . . ? C31B C32B C33B 120.0 . . ? C31B C32B H32B 120.0 . . ? C33B C32B H32B 120.0 . . ? C34B C33B C32B 120.0 . . ? C34B C33B H33B 120.0 . . ? C32B C33B H33B 120.0 . . ? C35B C34B C33B 120.0 . . ? C35B C34B H34B 120.0 . . ? C33B C34B H34B 120.0 . . ? C34B C35B C36B 120.0 . . ? C34B C35B H35B 120.0 . . ? C36B C35B H35B 120.0 . . ? C31B C36B C35B 120.0 . . ? C31B C36B H36B 120.0 . . ? C35B C36B H36B 120.0 . . ? C31B C37B H37B 109.5 . . ? C31B C37B H38B 110.6 . . ? H37B C37B H38B 108.9 . . ? C31B C37B H39B 110.1 . . ? H37B C37B H39B 108.9 . . ? H38B C37B H39B 108.8 . . ? C42 C41 C46 120.0 . . ? C42 C41 C47 118.0(11) . . ? C46 C41 C47 121.9(11) . . ? C41 C42 C43 120.0 . . ? C41 C42 H42 120.0 . . ? C43 C42 H42 120.0 . . ? C44 C43 C42 120.0 . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C43 C44 C45 120.0 . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C46 C45 C44 120.0 . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C45 C46 C41 120.0 . . ? C45 C46 H46 120.0 . . ? C41 C46 H46 120.0 . . ? C41 C47 H47 109.7 . . ? C41 C47 H48 118.7 . . ? H47 C47 H48 109.5 . . ? C41 C47 H49 99.4 . . ? H47 C47 H49 109.5 . . ? H48 C47 H49 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 C16 C11 B C1 59.2(2) . . . . ? C11 B C1 C2 12.3(2) . . . . ? B C1 C2 C3 179.91(16) . . . . ? C1 C2 C3 C4 -3.2(3) . . . . ? C22 C21 B C1 47.0(2) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.235 _refine_diff_density_min -0.194 _refine_diff_density_rms 0.041 #=====================================END data_1c _database_code_depnum_ccdc_archive 'CCDC 724816' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 2,5-bis(E-dimesitylborylethenyl)thiophene ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H50 B2 S,0.5(C H2 Cl2)' _chemical_formula_sum 'C44.5 H51 B2 Cl S' _chemical_formula_weight 674.98 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' B B 0.0013 0.0007 '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' Cl Cl 0.1484 0.1585 '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 12.4785(12) _cell_length_b 17.7688(17) _cell_length_c 18.5164(18) _cell_angle_alpha 79.05(2) _cell_angle_beta 80.04(2) _cell_angle_gamma 78.07(3) _cell_volume 3905.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 981 _cell_measurement_theta_min 12.07 _cell_measurement_theta_max 21.39 _exptl_crystal_description shapeless _exptl_crystal_colour yellow _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ?' _exptl_crystal_density_diffrn 1.148 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1444 _exptl_absorpt_coefficient_mu 0.181 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1.00 0.00 0.00 0.1400 1.00 0.00 0.00 0.1400 0.00 -1.00 1.00 0.0900 0.00 1.00 -1.00 0.0900 0.00 1.00 1.00 0.0800 0.00 -1.00 -1.00 0.0800 2.00 1.00 -1.00 0.1500 _exptl_special_details ;The data collection nominally covered full sphere of reciprocal space, by a combination of 5 sets of \w scans; each set at different \f and/or 2\q angles and each scan (20 sec exposure) covering 0.3\% in \w. Crystal to detector distance 4.41 cm. ; _diffrn_ambient_temperature 120(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 'SMART 1K CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8 _diffrn_standards_number 0 _diffrn_reflns_number 48948 _diffrn_reflns_av_R_equivalents 0.0698 _diffrn_reflns_av_sigmaI/netI 0.0699 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 29.09 _reflns_number_total 20654 _reflns_number_gt 13977 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART version 5.049 (Bruker, 1998)' _computing_cell_refinement 'SMART version 5.049 (Bruker, 1998)' _computing_data_reduction 'SAINT version 6.02A (Bruker, 2001)' _computing_structure_solution 'SHELXTL version 6.14 (Bruker, 2003)' _computing_structure_refinement 'SHELXTL version 6.14 (Bruker, 2003)' _computing_molecular_graphics 'SHELXTL version 6.14 (Bruker, 2003)' _computing_publication_material 'SHELXTL version 6.14 (Bruker, 2003)' _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. Methyl groups were refined as rigid bodies rotating around C---C bonds, with a common refined U for three H atoms. Other H atoms: riding model. ; _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^)+(0.0702P)^2^+2.0541P] 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 20654 _refine_ls_number_parameters 926 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0974 _refine_ls_R_factor_gt 0.0604 _refine_ls_wR_factor_ref 0.1684 _refine_ls_wR_factor_gt 0.1439 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.008 _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 0.44184(4) 0.76959(3) 0.20075(3) 0.02335(11) Uani 1 1 d . . . B1 B 0.2523(2) 0.60997(13) 0.39707(13) 0.0290(5) Uani 1 1 d . . . B2 B 0.71046(18) 0.90915(13) 0.05561(12) 0.0235(4) Uani 1 1 d . . . C1 C 0.30653(18) 0.66492(12) 0.33209(11) 0.0301(4) Uani 1 1 d . . . H1 H 0.3539 0.6954 0.3429 0.036 Uiso 1 1 d R . . C2 C 0.28938(17) 0.67152(11) 0.26152(11) 0.0263(4) Uani 1 1 d . . . H2 H 0.2387 0.6423 0.2529 0.032 Uiso 1 1 d R . . C3 C 0.33982(16) 0.71816(11) 0.19677(11) 0.0238(4) Uani 1 1 d . . . C4 C 0.32227(17) 0.72299(12) 0.12488(11) 0.0278(4) Uani 1 1 d . . . H4 H 0.2690 0.6992 0.1114 0.033 Uiso 1 1 d R . . C5 C 0.39168(17) 0.76720(12) 0.07297(11) 0.0264(4) Uani 1 1 d . . . H5 H 0.3890 0.7767 0.0212 0.032 Uiso 1 1 d R . . C6 C 0.46315(16) 0.79482(11) 0.10513(10) 0.0228(4) Uani 1 1 d . . . C7 C 0.55152(16) 0.83511(11) 0.06749(11) 0.0241(4) Uani 1 1 d . . . H7 H 0.5654 0.8392 0.0151 0.029 Uiso 1 1 d R . . C8 C 0.61553(17) 0.86742(12) 0.09928(11) 0.0268(4) Uani 1 1 d . . . H8 H 0.6021 0.8646 0.1516 0.032 Uiso 1 1 d R . . C11 C 0.19696(19) 0.54556(12) 0.37762(11) 0.0297(4) Uani 1 1 d . . . C12 C 0.0820(2) 0.54799(13) 0.39698(12) 0.0338(5) Uani 1 1 d . . . C13 C 0.0316(2) 0.49264(14) 0.37821(13) 0.0399(5) Uani 1 1 d . . . H13 H -0.0459 0.4957 0.3909 0.048 Uiso 1 1 d R . . C14 C 0.0925(2) 0.43328(13) 0.34111(13) 0.0414(6) Uani 1 1 d . . . C15 C 0.2049(2) 0.43030(13) 0.32258(13) 0.0394(6) Uani 1 1 d . . . H15 H 0.2473 0.3895 0.2980 0.047 Uiso 1 1 d R . . C16 C 0.2587(2) 0.48592(12) 0.33897(11) 0.0325(5) Uani 1 1 d . . . C17 C 0.0099(2) 0.61238(15) 0.43512(14) 0.0431(6) Uani 1 1 d . . . H171 H 0.0082 0.6619 0.4013 0.072(6) Uiso 1 1 d R . . H172 H 0.0399 0.6156 0.4796 0.072(6) Uiso 1 1 d R . . H173 H -0.0651 0.6013 0.4492 0.072(6) Uiso 1 1 d R . . C18 C 0.0360(3) 0.37461(16) 0.32025(18) 0.0622(9) Uani 1 1 d . . . H181 H -0.0085 0.4001 0.2809 0.109(8) Uiso 1 1 d R . . H182 H -0.0118 0.3534 0.3636 0.109(8) Uiso 1 1 d R . . H183 H 0.0919 0.3324 0.3026 0.109(8) Uiso 1 1 d R . . C19 C 0.3822(2) 0.47775(14) 0.31544(14) 0.0436(6) Uani 1 1 d . . . H191 H 0.4172 0.4234 0.3286 0.082(6) Uiso 1 1 d R . . H192 H 0.4120 0.5107 0.3407 0.082(6) Uiso 1 1 d R . . H193 H 0.3972 0.4938 0.2617 0.082(6) Uiso 1 1 d R . . C21 C 0.25562(19) 0.62101(12) 0.47949(11) 0.0310(4) Uani 1 1 d . . . C22 C 0.2205(2) 0.69509(13) 0.50167(12) 0.0359(5) Uani 1 1 d . . . C23 C 0.2268(2) 0.70450(13) 0.57392(12) 0.0400(5) Uani 1 1 d . . . H23 H 0.2019 0.7545 0.5879 0.048 Uiso 1 1 d R . . C24 C 0.2681(2) 0.64337(14) 0.62553(12) 0.0387(5) Uani 1 1 d . . . C25 C 0.3030(2) 0.57104(14) 0.60367(13) 0.0400(5) Uani 1 1 d . . . H25 H 0.3328 0.5286 0.6381 0.048 Uiso 1 1 d R . . C26 C 0.2961(2) 0.55822(13) 0.53263(12) 0.0363(5) Uani 1 1 d . . . C27 C 0.1733(3) 0.76619(14) 0.45035(14) 0.0526(7) Uani 1 1 d . . . H271 H 0.1299 0.8051 0.4798 0.114(9) Uiso 1 1 d R . . H272 H 0.1258 0.7518 0.4203 0.114(9) Uiso 1 1 d R . . H273 H 0.2337 0.7879 0.4178 0.114(9) Uiso 1 1 d R . . C28 C 0.2764(3) 0.65569(17) 0.70269(14) 0.0554(8) Uani 1 1 d . . . H281 H 0.2934 0.6052 0.7342 0.101(8) Uiso 1 1 d R . . H282 H 0.2060 0.6845 0.7236 0.101(8) Uiso 1 1 d R . . H283 H 0.3350 0.6854 0.7002 0.101(8) Uiso 1 1 d R . . C29 C 0.3372(3) 0.47711(15) 0.51451(15) 0.0561(8) Uani 1 1 d . . . H291 H 0.4002 0.4776 0.4750 0.074(6) Uiso 1 1 d R . . H292 H 0.2780 0.4591 0.4980 0.074(6) Uiso 1 1 d R . . H293 H 0.3600 0.4420 0.5588 0.074(6) Uiso 1 1 d R . . C31 C 0.77398(15) 0.88014(11) -0.01808(11) 0.0229(4) Uani 1 1 d . . . C32 C 0.78905(16) 0.93298(11) -0.08482(11) 0.0240(4) Uani 1 1 d . . . C33 C 0.84375(16) 0.90609(12) -0.14973(11) 0.0275(4) Uani 1 1 d . . . H33 H 0.8516 0.9422 -0.1942 0.033 Uiso 1 1 d R . . C34 C 0.88696(16) 0.82770(13) -0.15084(12) 0.0311(4) Uani 1 1 d . . . C35 C 0.87300(17) 0.77598(12) -0.08516(13) 0.0312(5) Uani 1 1 d . . . H35 H 0.9028 0.7224 -0.0850 0.037 Uiso 1 1 d R . . C36 C 0.81666(16) 0.79990(11) -0.01963(12) 0.0263(4) Uani 1 1 d . . . C37 C 0.74545(18) 1.01933(11) -0.08815(12) 0.0297(4) Uani 1 1 d . . . H371 H 0.7873 1.0410 -0.0597 0.063(5) Uiso 1 1 d R . . H372 H 0.6674 1.0277 -0.0671 0.063(5) Uiso 1 1 d R . . H373 H 0.7536 1.0451 -0.1398 0.063(5) Uiso 1 1 d R . . C38 C 0.9427(2) 0.79882(16) -0.22226(14) 0.0436(6) Uani 1 1 d . . . H381 H 1.0092 0.7605 -0.2128 0.066(5) Uiso 1 1 d R . . H382 H 0.9630 0.8427 -0.2590 0.066(5) Uiso 1 1 d R . . H383 H 0.8920 0.7746 -0.2412 0.066(5) Uiso 1 1 d R . . C39 C 0.80602(19) 0.73721(12) 0.04836(13) 0.0351(5) Uani 1 1 d . . . H391 H 0.7365 0.7187 0.0521 0.046(4) Uiso 1 1 d R . . H392 H 0.8068 0.7589 0.0929 0.046(4) Uiso 1 1 d R . . H393 H 0.8679 0.6938 0.0437 0.046(4) Uiso 1 1 d R . . C41 C 0.73711(16) 0.97597(11) 0.09063(10) 0.0239(4) Uani 1 1 d . . . C42 C 0.64971(17) 1.03177(11) 0.11890(11) 0.0278(4) Uani 1 1 d . . . C43 C 0.6712(2) 1.08495(12) 0.15856(12) 0.0340(5) Uani 1 1 d . . . H43 H 0.6119 1.1224 0.1767 0.041 Uiso 1 1 d R . . C45 C 0.8630(2) 1.03201(13) 0.14234(13) 0.0354(5) Uani 1 1 d . . . H45 H 0.9360 1.0324 0.1499 0.042 Uiso 1 1 d R . . C44 C 0.7766(2) 1.08446(13) 0.17240(13) 0.0366(5) Uani 1 1 d . . . C46 C 0.84544(17) 0.97856(12) 0.10133(12) 0.0285(4) Uani 1 1 d . . . C47 C 0.94367(18) 0.92162(14) 0.07270(15) 0.0403(5) Uani 1 1 d . . . H471 H 1.0108 0.9312 0.0870 0.064(5) Uiso 1 1 d R . . H472 H 0.9505 0.9282 0.0186 0.064(5) Uiso 1 1 d R . . H473 H 0.9333 0.8685 0.0939 0.064(5) Uiso 1 1 d R . . C48 C 0.7963(3) 1.13878(16) 0.22012(17) 0.0555(7) Uani 1 1 d . . . H481 H 0.7331 1.1815 0.2234 0.125(10) Uiso 1 1 d R . . H482 H 0.8630 1.1598 0.1980 0.125(10) Uiso 1 1 d R . . H483 H 0.8057 1.1101 0.2698 0.125(10) Uiso 1 1 d R . . C49 C 0.53145(18) 1.03736(13) 0.10665(13) 0.0356(5) Uani 1 1 d . . . H491 H 0.4968 0.9996 0.1440 0.056(5) Uiso 1 1 d R . . H492 H 0.5305 1.0263 0.0571 0.056(5) Uiso 1 1 d R . . H493 H 0.4907 1.0899 0.1110 0.056(5) Uiso 1 1 d R . . S2 S 0.53540(4) 0.73907(3) 0.75125(3) 0.02784(12) Uani 1 1 d . . . B3 B 0.28017(18) 0.57789(13) 0.95225(13) 0.0247(4) Uani 1 1 d . . . B4 B 0.7376(2) 0.91799(14) 0.58955(13) 0.0298(5) Uani 1 1 d . . . C51 C 0.37371(16) 0.62714(12) 0.93127(11) 0.0268(4) Uani 1 1 d . . . H51 H 0.3940 0.6471 0.9699 0.032 Uiso 1 1 d R . . C52 C 0.42780(16) 0.64345(11) 0.86279(11) 0.0263(4) Uani 1 1 d . . . H52 H 0.4143 0.6186 0.8252 0.032 Uiso 1 1 d R . . C53 C 0.50581(16) 0.69662(11) 0.84255(11) 0.0249(4) Uani 1 1 d . . . C54 C 0.56296(16) 0.72257(11) 0.88773(11) 0.0252(4) Uani 1 1 d . . . H54 H 0.5586 0.7056 0.9397 0.030 Uiso 1 1 d R . . C55 C 0.62843(16) 0.77708(12) 0.84847(11) 0.0259(4) Uani 1 1 d . . . H55 H 0.6728 0.8002 0.8714 0.031 Uiso 1 1 d R . . C56 C 0.62139(16) 0.79328(11) 0.77394(11) 0.0246(4) Uani 1 1 d . . . C57 C 0.67544(17) 0.84823(11) 0.71920(11) 0.0266(4) Uani 1 1 d . . . H57 H 0.7181 0.8773 0.7369 0.032 Uiso 1 1 d R . . C58 C 0.67129(19) 0.86217(12) 0.64577(12) 0.0319(5) Uani 1 1 d . . . H58 H 0.6250 0.8364 0.6273 0.038 Uiso 1 1 d R . . C61 C 0.19529(16) 0.59945(11) 1.02185(11) 0.0237(4) Uani 1 1 d . . . C62 C 0.18367(16) 0.54537(12) 1.08773(11) 0.0268(4) Uani 1 1 d . . . C63 C 0.12022(17) 0.56925(13) 1.15199(12) 0.0311(4) Uani 1 1 d . . . H63 H 0.1151 0.5327 1.1963 0.037 Uiso 1 1 d R . . C64 C 0.06469(17) 0.64515(13) 1.15229(13) 0.0324(5) Uani 1 1 d . . . C65 C 0.07322(17) 0.69720(12) 1.08651(13) 0.0319(5) Uani 1 1 d . . . H65 H 0.0329 0.7487 1.0854 0.038 Uiso 1 1 d R . . C66 C 0.13851(16) 0.67694(11) 1.02243(12) 0.0276(4) Uani 1 1 d . . . C67 C 0.24226(19) 0.46152(12) 1.09080(13) 0.0347(5) Uani 1 1 d . . . H671 H 0.2259 0.4329 1.1408 0.071(6) Uiso 1 1 d R . . H672 H 0.3220 0.4600 1.0785 0.071(6) Uiso 1 1 d R . . H673 H 0.2169 0.4375 1.0551 0.071(6) Uiso 1 1 d R . . C68 C -0.0018(2) 0.67167(16) 1.22244(15) 0.0475(6) Uani 1 1 d . . . H681 H 0.0365 0.7060 1.2399 0.076(6) Uiso 1 1 d R . . H682 H -0.0099 0.6263 1.2607 0.076(6) Uiso 1 1 d R . . H683 H -0.0748 0.6998 1.2119 0.076(6) Uiso 1 1 d R . . C69 C 0.14793(19) 0.73924(12) 0.95469(14) 0.0357(5) Uani 1 1 d . . . H691 H 0.0820 0.7799 0.9572 0.062(5) Uiso 1 1 d R . . H692 H 0.1545 0.7162 0.9099 0.062(5) Uiso 1 1 d R . . H693 H 0.2134 0.7619 0.9533 0.062(5) Uiso 1 1 d R . . C71 C 0.27501(16) 0.51690(11) 0.90231(11) 0.0244(4) Uani 1 1 d . . . C72 C 0.17803(17) 0.51594(11) 0.87303(11) 0.0269(4) Uani 1 1 d . . . C73 C 0.18109(18) 0.46989(12) 0.81946(12) 0.0321(5) Uani 1 1 d . . . H73 H 0.1153 0.4708 0.8001 0.039 Uiso 1 1 d R . . C74 C 0.2780(2) 0.42269(12) 0.79368(13) 0.0345(5) Uani 1 1 d . . . C75 C 0.37164(18) 0.42053(12) 0.82530(13) 0.0328(5) Uani 1 1 d . . . H75 H 0.4378 0.3871 0.8098 0.039 Uiso 1 1 d R . . C76 C 0.37224(17) 0.46551(11) 0.87850(12) 0.0284(4) Uani 1 1 d . . . C77 C 0.06855(18) 0.56613(14) 0.89638(14) 0.0374(5) Uani 1 1 d . . . H771 H 0.0707 0.6206 0.8750 0.064(5) Uiso 1 1 d R . . H772 H 0.0548 0.5610 0.9505 0.064(5) Uiso 1 1 d R . . H773 H 0.0094 0.5492 0.8787 0.064(5) Uiso 1 1 d R . . C78 C 0.2824(2) 0.37383(16) 0.73476(16) 0.0489(6) Uani 1 1 d . . . H781 H 0.3532 0.3728 0.7024 0.062(5) Uiso 1 1 d R . . H782 H 0.2222 0.3962 0.7054 0.062(5) Uiso 1 1 d R . . H783 H 0.2747 0.3208 0.7583 0.062(5) Uiso 1 1 d R . . C79 C 0.47756(19) 0.45296(14) 0.91262(15) 0.0397(5) Uani 1 1 d . . . H791 H 0.5057 0.3971 0.9242 0.074(6) Uiso 1 1 d R . . H792 H 0.4621 0.4758 0.9582 0.074(6) Uiso 1 1 d R . . H793 H 0.5328 0.4779 0.8775 0.074(6) Uiso 1 1 d R . . C81 C 0.78992(18) 0.97667(12) 0.62064(11) 0.0288(4) Uani 1 1 d . . . C82 C 0.90617(18) 0.97211(12) 0.61120(11) 0.0307(4) Uani 1 1 d . . . C83 C 0.95249(19) 1.01984(12) 0.64416(12) 0.0331(5) Uani 1 1 d . . . H83 H 1.0304 1.0152 0.6378 0.040 Uiso 1 1 d R . . C84 C 0.8872(2) 1.07405(12) 0.68598(12) 0.0323(5) Uani 1 1 d . . . C85 C 0.7737(2) 1.07975(12) 0.69422(11) 0.0326(5) Uani 1 1 d . . . H85 H 0.7281 1.1171 0.7218 0.039 Uiso 1 1 d R . . C86 C 0.72390(19) 1.03223(12) 0.66300(11) 0.0310(5) Uani 1 1 d . . . C87 C 0.9829(2) 0.91383(14) 0.56795(14) 0.0392(5) Uani 1 1 d . . . H871 H 1.0581 0.9244 0.5609 0.056(5) Uiso 1 1 d R . . H872 H 0.9590 0.9181 0.5196 0.056(5) Uiso 1 1 d R . . H873 H 0.9813 0.8612 0.5953 0.056(5) Uiso 1 1 d R . . C88 C 0.9386(2) 1.12516(14) 0.72162(14) 0.0434(6) Uani 1 1 d . . . H881 H 0.8802 1.1622 0.7452 0.093(7) Uiso 1 1 d R . . H882 H 0.9868 1.1536 0.6837 0.093(7) Uiso 1 1 d R . . H883 H 0.9819 1.0927 0.7591 0.093(7) Uiso 1 1 d R . . C89 C 0.5989(2) 1.04429(14) 0.67467(13) 0.0393(5) Uani 1 1 d . . . H891 H 0.5733 1.0182 0.7241 0.085(7) Uiso 1 1 d R . . H892 H 0.5741 1.0225 0.6372 0.085(7) Uiso 1 1 d R . . H893 H 0.5687 1.1000 0.6703 0.085(7) Uiso 1 1 d R . . C91 C 0.74794(19) 0.90950(13) 0.50505(11) 0.0313(4) Uani 1 1 d . . . C92 C 0.78852(19) 0.83574(13) 0.48234(12) 0.0325(5) Uani 1 1 d . . . C93 C 0.7858(2) 0.82646(14) 0.40987(12) 0.0359(5) Uani 1 1 d . . . H93 H 0.8137 0.7768 0.3956 0.043 Uiso 1 1 d R . . C94 C 0.7437(2) 0.88712(14) 0.35775(12) 0.0372(5) Uani 1 1 d . . . C95 C 0.7060(2) 0.95961(14) 0.37939(12) 0.0406(5) Uani 1 1 d . . . H95 H 0.6773 1.0020 0.3445 0.049 Uiso 1 1 d R . . C96 C 0.7092(2) 0.97186(13) 0.45101(12) 0.0367(5) Uani 1 1 d . . . C97 C 0.8378(2) 0.76591(14) 0.53406(13) 0.0425(6) Uani 1 1 d . . . H971 H 0.8036 0.7215 0.5328 0.091(7) Uiso 1 1 d R . . H972 H 0.8243 0.7779 0.5846 0.091(7) Uiso 1 1 d R . . H973 H 0.9174 0.7531 0.5184 0.091(7) Uiso 1 1 d R . . C98 C 0.7373(3) 0.87385(17) 0.28033(13) 0.0498(7) Uani 1 1 d . . . H981 H 0.8077 0.8444 0.2604 0.114(9) Uiso 1 1 d R . . H982 H 0.7216 0.9241 0.2482 0.114(9) Uiso 1 1 d R . . H983 H 0.6783 0.8446 0.2825 0.114(9) Uiso 1 1 d R . . C99 C 0.6638(3) 1.05248(14) 0.47021(15) 0.0538(7) Uani 1 1 d . . . H991 H 0.6589 1.0902 0.4245 0.080(6) Uiso 1 1 d R . . H992 H 0.7130 1.0660 0.4995 0.080(6) Uiso 1 1 d R . . H993 H 0.5903 1.0533 0.4990 0.080(6) Uiso 1 1 d R . . Cl1 Cl 0.54458(7) 0.73799(4) 0.39726(4) 0.05530(18) Uani 1 1 d . . . Cl2 Cl 0.54869(10) 0.71567(6) 0.55590(5) 0.0878(3) Uani 1 1 d . . . C0A C 0.5091(4) 0.7785(2) 0.4781(2) 0.0534(10) Uani 0.70 1 d P A 1 H01A H 0.5438 0.8251 0.4716 0.069 Uiso 0.70 1 d PR A 1 H02A H 0.4280 0.7959 0.4862 0.069 Uiso 0.70 1 d PR A 1 C0B C 0.4695(8) 0.7281(6) 0.4865(5) 0.053(2) Uiso 0.30 1 d P A 2 H01B H 0.4117 0.7751 0.4906 0.070 Uiso 0.30 1 d PR A 2 H02B H 0.4319 0.6829 0.4936 0.070 Uiso 0.30 1 d PR A 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 S1 0.0249(2) 0.0266(2) 0.0201(2) -0.00454(17) -0.00110(18) -0.00916(18) B1 0.0338(13) 0.0263(11) 0.0253(11) -0.0043(9) 0.0003(9) -0.0052(9) B2 0.0196(10) 0.0256(10) 0.0248(10) 0.0014(8) -0.0058(8) -0.0056(8) C1 0.0349(11) 0.0317(10) 0.0263(10) -0.0058(8) -0.0005(9) -0.0143(9) C2 0.0255(10) 0.0284(10) 0.0257(10) -0.0062(8) 0.0033(8) -0.0104(8) C3 0.0217(9) 0.0247(9) 0.0250(9) -0.0047(7) 0.0012(7) -0.0074(7) C4 0.0241(10) 0.0375(11) 0.0247(10) -0.0062(8) -0.0019(8) -0.0123(8) C5 0.0268(10) 0.0333(10) 0.0199(9) -0.0039(8) -0.0023(8) -0.0082(8) C6 0.0224(9) 0.0249(9) 0.0204(9) -0.0032(7) 0.0005(7) -0.0058(7) C7 0.0262(10) 0.0256(9) 0.0200(9) -0.0034(7) -0.0008(7) -0.0060(8) C8 0.0279(10) 0.0324(10) 0.0209(9) -0.0033(8) 0.0003(8) -0.0111(8) C11 0.0407(12) 0.0273(10) 0.0200(9) -0.0010(7) -0.0001(8) -0.0095(9) C12 0.0411(13) 0.0332(11) 0.0254(10) 0.0012(8) 0.0010(9) -0.0131(9) C13 0.0448(14) 0.0385(12) 0.0374(12) 0.0056(10) -0.0071(10) -0.0192(11) C14 0.0605(16) 0.0326(12) 0.0348(12) 0.0050(9) -0.0153(11) -0.0195(11) C15 0.0639(17) 0.0260(11) 0.0290(11) -0.0032(9) -0.0092(11) -0.0088(10) C16 0.0471(13) 0.0279(10) 0.0207(10) -0.0022(8) -0.0019(9) -0.0069(9) C17 0.0397(13) 0.0491(14) 0.0373(13) -0.0079(11) 0.0068(10) -0.0097(11) C18 0.093(2) 0.0404(14) 0.0659(19) 0.0010(13) -0.0366(18) -0.0288(15) C19 0.0491(15) 0.0386(13) 0.0393(13) -0.0104(10) 0.0034(11) -0.0033(11) C21 0.0416(12) 0.0298(10) 0.0216(10) -0.0025(8) -0.0006(9) -0.0111(9) C22 0.0529(14) 0.0304(11) 0.0238(10) -0.0017(8) -0.0011(10) -0.0123(10) C23 0.0609(16) 0.0335(12) 0.0275(11) -0.0077(9) 0.0006(11) -0.0160(11) C24 0.0526(15) 0.0439(13) 0.0238(10) -0.0039(9) -0.0036(10) -0.0208(11) C25 0.0544(15) 0.0389(12) 0.0277(11) 0.0013(9) -0.0115(10) -0.0123(11) C26 0.0483(14) 0.0319(11) 0.0280(11) -0.0018(9) -0.0052(10) -0.0081(10) C27 0.094(2) 0.0298(12) 0.0283(12) -0.0029(9) -0.0075(13) 0.0005(13) C28 0.086(2) 0.0599(17) 0.0296(13) -0.0073(12) -0.0159(13) -0.0270(16) C29 0.089(2) 0.0359(13) 0.0388(14) -0.0039(11) -0.0184(14) 0.0062(14) C31 0.0182(9) 0.0258(9) 0.0254(9) -0.0027(7) -0.0031(7) -0.0068(7) C32 0.0201(9) 0.0275(9) 0.0255(10) -0.0031(7) -0.0029(7) -0.0077(7) C33 0.0244(10) 0.0339(10) 0.0256(10) -0.0047(8) -0.0013(8) -0.0103(8) C34 0.0183(9) 0.0434(12) 0.0343(11) -0.0161(9) 0.0007(8) -0.0065(8) C35 0.0206(10) 0.0283(10) 0.0463(13) -0.0113(9) -0.0075(9) -0.0006(8) C36 0.0194(9) 0.0272(10) 0.0338(11) -0.0031(8) -0.0071(8) -0.0060(7) C37 0.0358(12) 0.0260(10) 0.0263(10) -0.0005(8) -0.0031(9) -0.0079(8) C38 0.0312(12) 0.0571(15) 0.0444(14) -0.0266(12) 0.0013(10) -0.0013(11) C39 0.0298(11) 0.0260(10) 0.0463(13) 0.0032(9) -0.0094(10) -0.0025(8) C41 0.0271(10) 0.0246(9) 0.0202(9) 0.0017(7) -0.0046(7) -0.0088(8) C42 0.0316(11) 0.0274(10) 0.0240(10) -0.0002(8) -0.0060(8) -0.0065(8) C43 0.0416(13) 0.0267(10) 0.0340(12) -0.0073(9) -0.0056(10) -0.0045(9) C45 0.0367(12) 0.0343(11) 0.0403(12) -0.0008(9) -0.0126(10) -0.0168(9) C44 0.0490(14) 0.0295(11) 0.0369(12) -0.0038(9) -0.0117(10) -0.0164(10) C46 0.0275(10) 0.0288(10) 0.0293(10) 0.0020(8) -0.0051(8) -0.0108(8) C47 0.0221(11) 0.0465(13) 0.0556(15) -0.0132(11) -0.0057(10) -0.0083(9) C48 0.075(2) 0.0437(14) 0.0610(18) -0.0167(13) -0.0208(15) -0.0240(14) C49 0.0308(12) 0.0392(12) 0.0369(12) -0.0105(10) -0.0087(9) 0.0008(9) S2 0.0323(3) 0.0311(3) 0.0224(2) -0.00488(19) -0.0014(2) -0.0123(2) B3 0.0221(10) 0.0247(10) 0.0266(11) 0.0025(8) -0.0083(9) -0.0044(8) B4 0.0318(12) 0.0314(12) 0.0226(11) -0.0028(9) 0.0009(9) -0.0027(10) C51 0.0234(10) 0.0320(10) 0.0273(10) -0.0055(8) -0.0041(8) -0.0092(8) C52 0.0248(10) 0.0278(10) 0.0280(10) -0.0044(8) -0.0063(8) -0.0065(8) C53 0.0229(10) 0.0261(9) 0.0238(9) -0.0015(7) 0.0002(7) -0.0054(7) C54 0.0208(9) 0.0303(10) 0.0232(9) -0.0007(7) -0.0021(7) -0.0053(8) C55 0.0211(9) 0.0313(10) 0.0254(10) -0.0043(8) -0.0028(8) -0.0059(8) C56 0.0221(9) 0.0267(9) 0.0252(10) -0.0071(7) 0.0013(7) -0.0061(7) C57 0.0274(10) 0.0289(10) 0.0240(10) -0.0064(8) 0.0016(8) -0.0083(8) C58 0.0364(12) 0.0361(11) 0.0253(10) -0.0070(8) 0.0001(9) -0.0130(9) C61 0.0187(9) 0.0258(9) 0.0282(10) -0.0032(7) -0.0056(7) -0.0067(7) C62 0.0219(9) 0.0292(10) 0.0299(10) -0.0017(8) -0.0046(8) -0.0078(8) C63 0.0262(10) 0.0384(11) 0.0290(11) -0.0005(9) -0.0040(8) -0.0107(9) C64 0.0217(10) 0.0430(12) 0.0353(11) -0.0126(9) -0.0020(9) -0.0082(9) C65 0.0224(10) 0.0291(10) 0.0452(13) -0.0110(9) -0.0065(9) -0.0012(8) C66 0.0212(9) 0.0270(10) 0.0366(11) -0.0029(8) -0.0099(8) -0.0060(8) C67 0.0366(12) 0.0280(10) 0.0350(12) 0.0028(9) -0.0025(9) -0.0044(9) C68 0.0370(14) 0.0601(16) 0.0461(15) -0.0222(13) 0.0055(11) -0.0074(12) C69 0.0319(12) 0.0275(10) 0.0462(13) 0.0026(9) -0.0131(10) -0.0034(9) C71 0.0226(9) 0.0245(9) 0.0251(10) 0.0003(7) -0.0026(8) -0.0061(7) C72 0.0257(10) 0.0260(9) 0.0294(10) -0.0034(8) -0.0033(8) -0.0072(8) C73 0.0290(11) 0.0337(11) 0.0372(12) -0.0083(9) -0.0052(9) -0.0106(9) C74 0.0390(12) 0.0297(11) 0.0371(12) -0.0093(9) -0.0011(10) -0.0110(9) C75 0.0284(11) 0.0268(10) 0.0414(12) -0.0090(9) 0.0012(9) -0.0027(8) C76 0.0260(10) 0.0247(10) 0.0329(11) -0.0017(8) -0.0031(8) -0.0044(8) C77 0.0217(10) 0.0465(13) 0.0483(14) -0.0193(11) -0.0062(10) -0.0043(9) C78 0.0503(16) 0.0492(15) 0.0540(16) -0.0262(13) -0.0027(13) -0.0116(12) C79 0.0306(12) 0.0378(12) 0.0500(14) -0.0093(10) -0.0126(11) 0.0035(9) C81 0.0361(11) 0.0272(10) 0.0196(9) -0.0015(7) 0.0039(8) -0.0068(8) C82 0.0360(12) 0.0295(10) 0.0233(10) -0.0026(8) 0.0056(8) -0.0081(9) C83 0.0358(12) 0.0322(11) 0.0283(11) -0.0006(8) 0.0020(9) -0.0085(9) C84 0.0446(13) 0.0273(10) 0.0237(10) 0.0003(8) -0.0019(9) -0.0100(9) C85 0.0472(13) 0.0238(10) 0.0233(10) -0.0018(8) 0.0002(9) -0.0043(9) C86 0.0397(12) 0.0275(10) 0.0213(10) 0.0009(8) 0.0018(8) -0.0052(9) C87 0.0367(13) 0.0407(12) 0.0377(13) -0.0119(10) 0.0089(10) -0.0075(10) C88 0.0595(16) 0.0354(12) 0.0398(13) -0.0060(10) -0.0118(12) -0.0143(11) C89 0.0385(13) 0.0376(12) 0.0361(12) -0.0057(10) 0.0031(10) -0.0009(10) C91 0.0366(12) 0.0356(11) 0.0197(9) -0.0019(8) 0.0004(8) -0.0082(9) C92 0.0391(12) 0.0342(11) 0.0230(10) -0.0046(8) -0.0019(9) -0.0062(9) C93 0.0427(13) 0.0406(12) 0.0245(10) -0.0076(9) -0.0004(9) -0.0094(10) C94 0.0444(13) 0.0479(13) 0.0205(10) -0.0013(9) -0.0023(9) -0.0166(11) C95 0.0526(15) 0.0415(13) 0.0244(11) 0.0059(9) -0.0061(10) -0.0107(11) C96 0.0470(14) 0.0336(11) 0.0271(11) -0.0002(9) -0.0018(10) -0.0088(10) C97 0.0589(16) 0.0365(12) 0.0275(11) -0.0048(9) -0.0067(11) 0.0020(11) C98 0.0674(19) 0.0634(17) 0.0231(11) -0.0035(11) -0.0084(11) -0.0230(14) C99 0.083(2) 0.0340(13) 0.0369(14) 0.0017(10) -0.0104(14) 0.0020(13) Cl1 0.0684(5) 0.0582(4) 0.0425(4) -0.0113(3) -0.0088(3) -0.0147(3) Cl2 0.1398(9) 0.0987(7) 0.0435(4) -0.0011(4) -0.0259(5) -0.0618(7) C0A 0.061(3) 0.046(2) 0.053(2) -0.0208(18) -0.001(2) -0.0029(19) _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 C6 1.7295(19) . ? S1 C3 1.7321(19) . ? B1 C1 1.551(3) . ? B1 C11 1.577(3) . ? B1 C21 1.584(3) . ? B2 C8 1.553(3) . ? B2 C41 1.572(3) . ? B2 C31 1.575(3) . ? C1 C2 1.340(3) . ? C1 H1 0.9471 . ? C2 C3 1.448(3) . ? C2 H2 0.9471 . ? C3 C4 1.370(3) . ? C4 C5 1.413(3) . ? C4 H4 0.9470 . ? C5 C6 1.366(3) . ? C5 H5 0.9471 . ? C6 C7 1.444(3) . ? C7 C8 1.340(3) . ? C7 H7 0.9471 . ? C8 H8 0.9471 . ? C11 C16 1.410(3) . ? C11 C12 1.411(3) . ? C12 C13 1.395(3) . ? C12 C17 1.510(3) . ? C13 C14 1.388(4) . ? C13 H13 0.9470 . ? C14 C15 1.377(4) . ? C14 C18 1.512(3) . ? C15 C16 1.407(3) . ? C15 H15 0.9472 . ? C16 C19 1.512(3) . ? C17 H171 0.9773 . ? C17 H172 0.9769 . ? C17 H173 0.9770 . ? C18 H181 0.9770 . ? C18 H182 0.9772 . ? C18 H183 0.9771 . ? C19 H191 0.9772 . ? C19 H192 0.9770 . ? C19 H193 0.9771 . ? C21 C26 1.411(3) . ? C21 C22 1.414(3) . ? C22 C23 1.397(3) . ? C22 C27 1.509(3) . ? C23 C24 1.380(3) . ? C23 H23 0.9472 . ? C24 C25 1.382(3) . ? C24 C28 1.510(3) . ? C25 C26 1.396(3) . ? C25 H25 0.9472 . ? C26 C29 1.507(3) . ? C27 H271 0.9771 . ? C27 H272 0.9769 . ? C27 H273 0.9771 . ? C28 H281 0.9772 . ? C28 H282 0.9770 . ? C28 H283 0.9770 . ? C29 H291 0.9770 . ? C29 H292 0.9769 . ? C29 H293 0.9772 . ? C31 C32 1.413(3) . ? C31 C36 1.419(3) . ? C32 C33 1.392(3) . ? C32 C37 1.512(3) . ? C33 C34 1.389(3) . ? C33 H33 0.9473 . ? C34 C35 1.387(3) . ? C34 C38 1.513(3) . ? C35 C36 1.387(3) . ? C35 H35 0.9473 . ? C36 C39 1.521(3) . ? C37 H371 0.9769 . ? C37 H372 0.9770 . ? C37 H373 0.9772 . ? C38 H381 0.9770 . ? C38 H382 0.9772 . ? C38 H383 0.9769 . ? C39 H391 0.9770 . ? C39 H392 0.9770 . ? C39 H393 0.9771 . ? C41 C46 1.411(3) . ? C41 C42 1.414(3) . ? C42 C43 1.393(3) . ? C42 C49 1.512(3) . ? C43 C44 1.382(3) . ? C43 H43 0.9471 . ? C45 C44 1.383(3) . ? C45 C46 1.394(3) . ? C45 H45 0.9470 . ? C44 C48 1.506(3) . ? C46 C47 1.508(3) . ? C47 H471 0.9769 . ? C47 H472 0.9771 . ? C47 H473 0.9772 . ? C48 H481 0.9770 . ? C48 H482 0.9770 . ? C48 H483 0.9772 . ? C49 H491 0.9772 . ? C49 H492 0.9770 . ? C49 H493 0.9772 . ? S2 C53 1.726(2) . ? S2 C56 1.730(2) . ? B3 C51 1.554(3) . ? B3 C71 1.570(3) . ? B3 C61 1.574(3) . ? B4 C58 1.550(3) . ? B4 C81 1.576(3) . ? B4 C91 1.581(3) . ? C51 C52 1.339(3) . ? C51 H51 0.9471 . ? C52 C53 1.449(3) . ? C52 H52 0.9471 . ? C53 C54 1.382(3) . ? C54 C55 1.410(3) . ? C54 H54 0.9472 . ? C55 C56 1.370(3) . ? C55 H55 0.9470 . ? C56 C57 1.448(3) . ? C57 C58 1.343(3) . ? C57 H57 0.9471 . ? C58 H58 0.9471 . ? C61 C62 1.408(3) . ? C61 C66 1.413(3) . ? C62 C63 1.396(3) . ? C62 C67 1.513(3) . ? C63 C64 1.384(3) . ? C63 H63 0.9473 . ? C64 C65 1.385(3) . ? C64 C68 1.515(3) . ? C65 C66 1.381(3) . ? C65 H65 0.9472 . ? C66 C69 1.513(3) . ? C67 H671 0.9772 . ? C67 H672 0.9769 . ? C67 H673 0.9770 . ? C68 H681 0.9770 . ? C68 H682 0.9772 . ? C68 H683 0.9770 . ? C69 H691 0.9770 . ? C69 H692 0.9770 . ? C69 H693 0.9770 . ? C71 C72 1.413(3) . ? C71 C76 1.418(3) . ? C72 C73 1.392(3) . ? C72 C77 1.512(3) . ? C73 C74 1.388(3) . ? C73 H73 0.9470 . ? C74 C75 1.385(3) . ? C74 C78 1.505(3) . ? C75 C76 1.383(3) . ? C75 H75 0.9471 . ? C76 C79 1.513(3) . ? C77 H771 0.9773 . ? C77 H772 0.9771 . ? C77 H773 0.9769 . ? C78 H781 0.9770 . ? C78 H782 0.9770 . ? C78 H783 0.9772 . ? C79 H791 0.9772 . ? C79 H792 0.9771 . ? C79 H793 0.9771 . ? C81 C86 1.415(3) . ? C81 C82 1.418(3) . ? C82 C83 1.395(3) . ? C82 C87 1.506(3) . ? C83 C84 1.390(3) . ? C83 H83 0.9470 . ? C84 C85 1.383(3) . ? C84 C88 1.511(3) . ? C85 C86 1.400(3) . ? C85 H85 0.9471 . ? C86 C89 1.512(3) . ? C87 H871 0.9769 . ? C87 H872 0.9770 . ? C87 H873 0.9772 . ? C88 H881 0.9770 . ? C88 H882 0.9771 . ? C88 H883 0.9771 . ? C89 H891 0.9772 . ? C89 H892 0.9770 . ? C89 H893 0.9772 . ? C91 C96 1.410(3) . ? C91 C92 1.418(3) . ? C92 C93 1.390(3) . ? C92 C97 1.508(3) . ? C93 C94 1.384(3) . ? C93 H93 0.9472 . ? C94 C95 1.386(3) . ? C94 C98 1.514(3) . ? C95 C96 1.392(3) . ? C95 H95 0.9473 . ? C96 C99 1.513(3) . ? C97 H971 0.9771 . ? C97 H972 0.9770 . ? C97 H973 0.9770 . ? C98 H981 0.9770 . ? C98 H982 0.9772 . ? C98 H983 0.9770 . ? C99 H991 0.9772 . ? C99 H992 0.9769 . ? C99 H993 0.9770 . ? Cl1 C0A 1.733(4) . ? Cl1 C0B 1.750(10) . ? Cl2 C0B 1.708(10) . ? Cl2 C0A 1.725(4) . ? C0A H01A 0.9892 . ? C0A H02A 0.9893 . ? C0A H01B 1.2090 . ? C0B H02A 1.2086 . ? C0B H01B 0.9896 . ? C0B H02B 0.9892 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 S1 C3 91.89(9) . . ? C1 B1 C11 118.18(18) . . ? C1 B1 C21 118.54(19) . . ? C11 B1 C21 123.29(18) . . ? C8 B2 C41 116.44(18) . . ? C8 B2 C31 118.10(17) . . ? C41 B2 C31 125.43(17) . . ? C2 C1 B1 123.21(19) . . ? C2 C1 H1 118.4 . . ? B1 C1 H1 118.4 . . ? C1 C2 C3 127.35(19) . . ? C1 C2 H2 116.4 . . ? C3 C2 H2 116.3 . . ? C4 C3 C2 126.28(18) . . ? C4 C3 S1 110.80(14) . . ? C2 C3 S1 122.69(15) . . ? C3 C4 C5 113.10(18) . . ? C3 C4 H4 123.4 . . ? C5 C4 H4 123.4 . . ? C6 C5 C4 113.13(18) . . ? C6 C5 H5 123.4 . . ? C4 C5 H5 123.5 . . ? C5 C6 C7 126.94(18) . . ? C5 C6 S1 111.02(14) . . ? C7 C6 S1 121.90(15) . . ? C8 C7 C6 126.49(18) . . ? C8 C7 H7 116.8 . . ? C6 C7 H7 116.7 . . ? C7 C8 B2 123.98(18) . . ? C7 C8 H8 118.0 . . ? B2 C8 H8 118.0 . . ? C16 C11 C12 118.2(2) . . ? C16 C11 B1 121.8(2) . . ? C12 C11 B1 119.97(19) . . ? C13 C12 C11 120.5(2) . . ? C13 C12 C17 118.4(2) . . ? C11 C12 C17 121.0(2) . . ? C14 C13 C12 121.3(2) . . ? C14 C13 H13 119.3 . . ? C12 C13 H13 119.4 . . ? C15 C14 C13 118.4(2) . . ? C15 C14 C18 121.1(3) . . ? C13 C14 C18 120.5(3) . . ? C14 C15 C16 122.2(2) . . ? C14 C15 H15 118.9 . . ? C16 C15 H15 118.9 . . ? C15 C16 C11 119.4(2) . . ? C15 C16 C19 117.9(2) . . ? C11 C16 C19 122.7(2) . . ? C12 C17 H171 109.4 . . ? C12 C17 H172 109.5 . . ? H171 C17 H172 109.5 . . ? C12 C17 H173 109.5 . . ? H171 C17 H173 109.5 . . ? H172 C17 H173 109.5 . . ? C14 C18 H181 109.4 . . ? C14 C18 H182 109.7 . . ? H181 C18 H182 109.5 . . ? C14 C18 H183 109.3 . . ? H181 C18 H183 109.5 . . ? H182 C18 H183 109.5 . . ? C16 C19 H191 109.4 . . ? C16 C19 H192 109.6 . . ? H191 C19 H192 109.5 . . ? C16 C19 H193 109.4 . . ? H191 C19 H193 109.5 . . ? H192 C19 H193 109.5 . . ? C26 C21 C22 117.71(19) . . ? C26 C21 B1 121.53(19) . . ? C22 C21 B1 120.74(19) . . ? C23 C22 C21 120.2(2) . . ? C23 C22 C27 117.3(2) . . ? C21 C22 C27 122.5(2) . . ? C24 C23 C22 122.1(2) . . ? C24 C23 H23 118.9 . . ? C22 C23 H23 118.9 . . ? C23 C24 C25 117.7(2) . . ? C23 C24 C28 120.9(2) . . ? C25 C24 C28 121.4(2) . . ? C24 C25 C26 122.4(2) . . ? C24 C25 H25 118.8 . . ? C26 C25 H25 118.8 . . ? C25 C26 C21 119.9(2) . . ? C25 C26 C29 118.1(2) . . ? C21 C26 C29 122.0(2) . . ? C22 C27 H271 109.3 . . ? C22 C27 H272 109.7 . . ? H271 C27 H272 109.5 . . ? C22 C27 H273 109.4 . . ? H271 C27 H273 109.5 . . ? H272 C27 H273 109.5 . . ? C24 C28 H281 109.5 . . ? C24 C28 H282 109.4 . . ? H281 C28 H282 109.5 . . ? C24 C28 H283 109.5 . . ? H281 C28 H283 109.5 . . ? H282 C28 H283 109.5 . . ? C26 C29 H291 109.5 . . ? C26 C29 H292 109.4 . . ? H291 C29 H292 109.5 . . ? C26 C29 H293 109.5 . . ? H291 C29 H293 109.5 . . ? H292 C29 H293 109.5 . . ? C32 C31 C36 117.97(18) . . ? C32 C31 B2 121.09(17) . . ? C36 C31 B2 120.93(17) . . ? C33 C32 C31 120.28(18) . . ? C33 C32 C37 118.34(18) . . ? C31 C32 C37 121.37(18) . . ? C34 C33 C32 121.63(19) . . ? C34 C33 H33 119.2 . . ? C32 C33 H33 119.2 . . ? C35 C34 C33 118.03(19) . . ? C35 C34 C38 120.8(2) . . ? C33 C34 C38 121.1(2) . . ? C34 C35 C36 122.30(19) . . ? C34 C35 H35 118.9 . . ? C36 C35 H35 118.8 . . ? C35 C36 C31 119.75(19) . . ? C35 C36 C39 117.11(19) . . ? C31 C36 C39 123.12(19) . . ? C32 C37 H371 109.4 . . ? C32 C37 H372 109.6 . . ? H371 C37 H372 109.5 . . ? C32 C37 H373 109.5 . . ? H371 C37 H373 109.5 . . ? H372 C37 H373 109.5 . . ? C34 C38 H381 109.5 . . ? C34 C38 H382 109.4 . . ? H381 C38 H382 109.5 . . ? C34 C38 H383 109.5 . . ? H381 C38 H383 109.5 . . ? H382 C38 H383 109.5 . . ? C36 C39 H391 109.4 . . ? C36 C39 H392 109.5 . . ? H391 C39 H392 109.5 . . ? C36 C39 H393 109.5 . . ? H391 C39 H393 109.5 . . ? H392 C39 H393 109.5 . . ? C46 C41 C42 117.83(18) . . ? C46 C41 B2 122.17(18) . . ? C42 C41 B2 119.74(18) . . ? C43 C42 C41 120.1(2) . . ? C43 C42 C49 117.6(2) . . ? C41 C42 C49 122.25(18) . . ? C44 C43 C42 121.8(2) . . ? C44 C43 H43 119.1 . . ? C42 C43 H43 119.2 . . ? C44 C45 C46 121.8(2) . . ? C44 C45 H45 119.1 . . ? C46 C45 H45 119.1 . . ? C43 C44 C45 118.3(2) . . ? C43 C44 C48 120.6(2) . . ? C45 C44 C48 121.1(2) . . ? C45 C46 C41 120.1(2) . . ? C45 C46 C47 118.4(2) . . ? C41 C46 C47 121.44(19) . . ? C46 C47 H471 109.6 . . ? C46 C47 H472 109.4 . . ? H471 C47 H472 109.5 . . ? C46 C47 H473 109.5 . . ? H471 C47 H473 109.5 . . ? H472 C47 H473 109.5 . . ? C44 C48 H481 109.7 . . ? C44 C48 H482 109.3 . . ? H481 C48 H482 109.5 . . ? C44 C48 H483 109.4 . . ? H481 C48 H483 109.5 . . ? H482 C48 H483 109.5 . . ? C42 C49 H491 109.5 . . ? C42 C49 H492 109.5 . . ? H491 C49 H492 109.5 . . ? C42 C49 H493 109.4 . . ? H491 C49 H493 109.5 . . ? H492 C49 H493 109.5 . . ? C53 S2 C56 92.25(10) . . ? C51 B3 C71 119.29(18) . . ? C51 B3 C61 113.71(18) . . ? C71 B3 C61 126.92(18) . . ? C58 B4 C81 118.20(18) . . ? C58 B4 C91 116.0(2) . . ? C81 B4 C91 125.77(19) . . ? C52 C51 B3 124.98(19) . . ? C52 C51 H51 117.5 . . ? B3 C51 H51 117.5 . . ? C51 C52 C53 124.21(19) . . ? C51 C52 H52 117.9 . . ? C53 C52 H52 117.9 . . ? C54 C53 C52 129.00(18) . . ? C54 C53 S2 110.62(14) . . ? C52 C53 S2 120.36(15) . . ? C53 C54 C55 112.98(18) . . ? C53 C54 H54 123.5 . . ? C55 C54 H54 123.5 . . ? C56 C55 C54 113.30(18) . . ? C56 C55 H55 123.4 . . ? C54 C55 H55 123.3 . . ? C55 C56 C57 126.75(19) . . ? C55 C56 S2 110.83(15) . . ? C57 C56 S2 122.42(15) . . ? C58 C57 C56 126.6(2) . . ? C58 C57 H57 116.7 . . ? C56 C57 H57 116.7 . . ? C57 C58 B4 123.9(2) . . ? C57 C58 H58 118.1 . . ? B4 C58 H58 118.1 . . ? C62 C61 C66 118.20(19) . . ? C62 C61 B3 121.38(17) . . ? C66 C61 B3 120.00(18) . . ? C63 C62 C61 120.13(19) . . ? C63 C62 C67 119.02(19) . . ? C61 C62 C67 120.82(19) . . ? C64 C63 C62 121.4(2) . . ? C64 C63 H63 119.3 . . ? C62 C63 H63 119.3 . . ? C63 C64 C65 118.0(2) . . ? C63 C64 C68 121.5(2) . . ? C65 C64 C68 120.5(2) . . ? C66 C65 C64 122.5(2) . . ? C66 C65 H65 118.7 . . ? C64 C65 H65 118.8 . . ? C65 C66 C61 119.63(19) . . ? C65 C66 C69 118.55(19) . . ? C61 C66 C69 121.8(2) . . ? C62 C67 H671 109.5 . . ? C62 C67 H672 109.3 . . ? H671 C67 H672 109.5 . . ? C62 C67 H673 109.6 . . ? H671 C67 H673 109.5 . . ? H672 C67 H673 109.5 . . ? C64 C68 H681 109.5 . . ? C64 C68 H682 109.5 . . ? H681 C68 H682 109.5 . . ? C64 C68 H683 109.4 . . ? H681 C68 H683 109.5 . . ? H682 C68 H683 109.5 . . ? C66 C69 H691 109.4 . . ? C66 C69 H692 109.6 . . ? H691 C69 H692 109.5 . . ? C66 C69 H693 109.4 . . ? H691 C69 H693 109.5 . . ? H692 C69 H693 109.5 . . ? C72 C71 C76 117.20(19) . . ? C72 C71 B3 122.22(18) . . ? C76 C71 B3 120.26(18) . . ? C73 C72 C71 120.61(19) . . ? C73 C72 C77 117.45(19) . . ? C71 C72 C77 121.92(19) . . ? C74 C73 C72 121.7(2) . . ? C74 C73 H73 119.1 . . ? C72 C73 H73 119.1 . . ? C75 C74 C73 117.6(2) . . ? C75 C74 C78 120.4(2) . . ? C73 C74 C78 122.1(2) . . ? C76 C75 C74 122.5(2) . . ? C76 C75 H75 118.7 . . ? C74 C75 H75 118.8 . . ? C75 C76 C71 120.23(19) . . ? C75 C76 C79 116.99(19) . . ? C71 C76 C79 122.66(19) . . ? C72 C77 H771 109.5 . . ? C72 C77 H772 109.5 . . ? H771 C77 H772 109.5 . . ? C72 C77 H773 109.4 . . ? H771 C77 H773 109.5 . . ? H772 C77 H773 109.5 . . ? C74 C78 H781 109.5 . . ? C74 C78 H782 109.4 . . ? H781 C78 H782 109.5 . . ? C74 C78 H783 109.5 . . ? H781 C78 H783 109.5 . . ? H782 C78 H783 109.5 . . ? C76 C79 H791 109.5 . . ? C76 C79 H792 109.5 . . ? H791 C79 H792 109.5 . . ? C76 C79 H793 109.5 . . ? H791 C79 H793 109.5 . . ? H792 C79 H793 109.5 . . ? C86 C81 C82 117.5(2) . . ? C86 C81 B4 121.6(2) . . ? C82 C81 B4 120.82(19) . . ? C83 C82 C81 120.6(2) . . ? C83 C82 C87 118.3(2) . . ? C81 C82 C87 121.1(2) . . ? C84 C83 C82 121.7(2) . . ? C84 C83 H83 119.1 . . ? C82 C83 H83 119.2 . . ? C85 C84 C83 118.0(2) . . ? C85 C84 C88 120.9(2) . . ? C83 C84 C88 121.1(2) . . ? C84 C85 C86 122.1(2) . . ? C84 C85 H85 118.9 . . ? C86 C85 H85 118.9 . . ? C85 C86 C81 120.1(2) . . ? C85 C86 C89 117.6(2) . . ? C81 C86 C89 122.2(2) . . ? C82 C87 H871 109.4 . . ? C82 C87 H872 109.4 . . ? H871 C87 H872 109.5 . . ? C82 C87 H873 109.6 . . ? H871 C87 H873 109.5 . . ? H872 C87 H873 109.5 . . ? C84 C88 H881 109.5 . . ? C84 C88 H882 109.5 . . ? H881 C88 H882 109.5 . . ? C84 C88 H883 109.4 . . ? H881 C88 H883 109.5 . . ? H882 C88 H883 109.5 . . ? C86 C89 H891 109.5 . . ? C86 C89 H892 109.5 . . ? H891 C89 H892 109.5 . . ? C86 C89 H893 109.4 . . ? H891 C89 H893 109.5 . . ? H892 C89 H893 109.5 . . ? C96 C91 C92 117.43(19) . . ? C96 C91 B4 122.2(2) . . ? C92 C91 B4 120.12(18) . . ? C93 C92 C91 120.1(2) . . ? C93 C92 C97 117.8(2) . . ? C91 C92 C97 122.16(19) . . ? C94 C93 C92 122.3(2) . . ? C94 C93 H93 118.8 . . ? C92 C93 H93 118.8 . . ? C93 C94 C95 117.7(2) . . ? C93 C94 C98 120.8(2) . . ? C95 C94 C98 121.5(2) . . ? C94 C95 C96 121.9(2) . . ? C94 C95 H95 119.1 . . ? C96 C95 H95 119.0 . . ? C95 C96 C91 120.5(2) . . ? C95 C96 C99 118.2(2) . . ? C91 C96 C99 121.2(2) . . ? C92 C97 H971 109.5 . . ? C92 C97 H972 109.4 . . ? H971 C97 H972 109.5 . . ? C92 C97 H973 109.5 . . ? H971 C97 H973 109.5 . . ? H972 C97 H973 109.5 . . ? C94 C98 H981 109.6 . . ? C94 C98 H982 109.5 . . ? H981 C98 H982 109.5 . . ? C94 C98 H983 109.3 . . ? H981 C98 H983 109.5 . . ? H982 C98 H983 109.5 . . ? C96 C99 H991 109.4 . . ? C96 C99 H992 109.4 . . ? H991 C99 H992 109.5 . . ? C96 C99 H993 109.6 . . ? H991 C99 H993 109.5 . . ? H992 C99 H993 109.5 . . ? C0A Cl1 C0B 36.2(4) . . ? C0B Cl2 C0A 36.8(4) . . ? Cl2 C0A Cl1 113.8(2) . . ? Cl2 C0A H01A 108.8 . . ? Cl1 C0A H01A 108.8 . . ? Cl2 C0A H02A 108.8 . . ? Cl1 C0A H02A 108.8 . . ? H01A C0A H02A 107.6 . . ? Cl2 C0A H01B 97.6 . . ? Cl1 C0A H01B 99.6 . . ? H01A C0A H01B 128.0 . . ? H02A C0A H01B 20.4 . . ? Cl2 C0B Cl1 113.8(6) . . ? Cl2 C0B H02A 99.4 . . ? Cl1 C0B H02A 97.6 . . ? Cl2 C0B H01B 108.8 . . ? Cl1 C0B H01B 108.8 . . ? H02A C0B H01B 20.4 . . ? Cl2 C0B H02B 108.8 . . ? Cl1 C0B H02B 108.8 . . ? H02A C0B H02B 128.1 . . ? H01B C0B H02B 107.7 . . ? 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 C12 C11 B1 C1 -115.9(2) . . . . ? C11 B1 C1 C2 14.3(3) . . . . ? B1 C1 C2 C3 -176.9(2) . . . . ? C1 C2 C3 S1 4.7(3) . . . . ? C2 C3 S1 C6 173.23(17) . . . . ? C3 S1 C6 C7 -173.72(17) . . . . ? S1 C6 C7 C8 -10.3(3) . . . . ? C6 C7 C8 B2 179.20(19) . . . . ? C7 C8 B2 C31 -30.7(3) . . . . ? C8 B2 C31 C32 129.1(2) . . . . ? C62 C61 B3 C51 -116.1(2) . . . . ? C61 B3 C51 C52 -152.4(2) . . . . ? B3 C51 C52 C53 172.65(19) . . . . ? C51 C52 C53 S2 -158.05(17) . . . . ? C52 C53 S2 C56 177.03(17) . . . . ? C53 S2 C56 C57 -177.74(17) . . . . ? S2 C56 C57 C58 -3.1(3) . . . . ? C56 C57 C58 B4 -175.8(2) . . . . ? C57 C58 B4 C81 -15.3(3) . . . . ? C58 B4 C81 C82 116.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 29.09 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.659 _refine_diff_density_min -0.769 _refine_diff_density_rms 0.063 #=====================================END data_1f _database_code_depnum_ccdc_archive 'CCDC 724817' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 4,4'-bis(E-dimesitylborylethenyl)biphenyl, toluene solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H56 B2,2(C7 H8)' _chemical_formula_sum 'C66 H72 B2' _chemical_formula_weight 886.86 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'I 2/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 15.3539(12) _cell_length_b 16.3316(11) _cell_length_c 21.5221(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.75(2) _cell_angle_gamma 90.00 _cell_volume 5396.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 980 _cell_measurement_theta_min 10.2 _cell_measurement_theta_max 23.1 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.092 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1912 _exptl_absorpt_coefficient_mu 0.061 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1.00 0.00 0.00 0.0550 1.00 0.00 0.00 0.0550 0.00 -1.00 1.00 0.1400 0.00 1.00 -1.00 0.1400 0.00 1.00 1.00 0.1700 0.00 -1.00 -1.00 0.1700 0.00 0.00 1.00 0.1400 _exptl_special_details ;The data collection nominally covered full sphere of reciprocal space, by a combination of 5 sets of \w scans; each set at different \f and/or 2\q angles and each scan (10 sec exposure) covering 0.3\% in \w. Crystal to detector distance 4.55 cm. ; _diffrn_ambient_temperature 120(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 'SMART 1K CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8 _diffrn_standards_number 0 _diffrn_reflns_number 31814 _diffrn_reflns_av_R_equivalents 0.0779 _diffrn_reflns_av_sigmaI/netI 0.0558 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6191 _reflns_number_gt 3681 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART version 5.060 (Bruker, 1999)' _computing_cell_refinement 'SMART version 5.060 (Bruker, 1999)' _computing_data_reduction 'SAINT version 6.02A (Bruker, 2001)' _computing_structure_solution 'SHELXTL version 6.14 (Bruker, 2003)' _computing_structure_refinement 'SHELXTL version 6.14 (Bruker, 2003)' _computing_molecular_graphics 'SHELXTL version 6.14 (Bruker, 2003)' _computing_publication_material 'SHELXTL version 6.14 (Bruker, 2003)' _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. Methyl groups (except those of toluene molecules) were refined as rigid bodies rotating around C---C bonds, with a common refined U for three H atoms. The C(18)H~3~ and C(29)H~3~ groups were treated as ideally disordered. Other H atoms: riding model. One toluene molecule [C(41) to C(47) with attached hydrogens] is disordered between 2 positions, related via a twofold axis which passes through C(41), the other (ordered) toluene molecule and the host molecule have crystallographic twofold symmetry. ; _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^)+(0.0760P)^2^+15.4122P] 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 6191 _refine_ls_number_parameters 309 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1327 _refine_ls_R_factor_gt 0.0765 _refine_ls_wR_factor_ref 0.2276 _refine_ls_wR_factor_gt 0.1851 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.053 _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 B B 0.5688(2) 0.19458(19) 0.25521(14) 0.0265(7) Uani 1 1 d . . . C1 C 0.5623(2) 0.24318(17) 0.19356(13) 0.0323(7) Uani 1 1 d . . . H1 H 0.5846 0.2184 0.1573 0.039 Uiso 1 1 d R . . C2 C 0.52775(18) 0.31831(16) 0.18829(12) 0.0270(6) Uani 1 1 d . . . H2 H 0.5058 0.3413 0.2254 0.032 Uiso 1 1 d R . . C3 C 0.51943(19) 0.36896(17) 0.13259(12) 0.0274(6) Uani 1 1 d . . . C4 C 0.5376(3) 0.34109(19) 0.07320(14) 0.0518(10) Uani 1 1 d . . . H4 H 0.5555 0.2861 0.0676 0.062 Uiso 1 1 d R . . C5 C 0.5302(3) 0.39172(19) 0.02225(14) 0.0521(10) Uani 1 1 d . . . H5 H 0.5440 0.3709 -0.0175 0.063 Uiso 1 1 d R . . C6 C 0.50387(19) 0.47283(16) 0.02756(12) 0.0266(6) Uani 1 1 d . . . C7 C 0.4846(2) 0.50001(18) 0.08669(13) 0.0346(7) Uani 1 1 d . . . H7 H 0.4660 0.5548 0.0923 0.042 Uiso 1 1 d R . . C8 C 0.4917(2) 0.44907(18) 0.13795(13) 0.0336(7) Uani 1 1 d . . . H8 H 0.4774 0.4697 0.1777 0.040 Uiso 1 1 d R . . C11 C 0.54635(17) 0.24070(16) 0.31787(12) 0.0249(6) Uani 1 1 d . . . C12 C 0.59600(18) 0.30752(17) 0.34026(12) 0.0271(6) Uani 1 1 d . . . C13 C 0.57321(18) 0.34609(18) 0.39557(13) 0.0295(6) Uani 1 1 d . . . H13 H 0.6076 0.3904 0.4103 0.035 Uiso 1 1 d R . . C14 C 0.50219(19) 0.32185(19) 0.42954(12) 0.0314(6) Uani 1 1 d . . . C15 C 0.45224(18) 0.25726(19) 0.40705(13) 0.0315(6) Uani 1 1 d . . . H15 H 0.4026 0.2404 0.4294 0.038 Uiso 1 1 d R . . C16 C 0.47316(17) 0.21708(17) 0.35201(12) 0.0263(6) Uani 1 1 d . . . C17 C 0.6749(2) 0.33890(19) 0.30626(14) 0.0375(7) Uani 1 1 d . . . H171 H 0.6594 0.3886 0.2832 0.096(9) Uiso 1 1 d R . . H172 H 0.6950 0.2970 0.2772 0.096(9) Uiso 1 1 d R . . H173 H 0.7217 0.3514 0.3361 0.096(9) Uiso 1 1 d R . . C18 C 0.4780(2) 0.3660(2) 0.48878(15) 0.0465(9) Uani 1 1 d . . . H181 H 0.5259 0.4019 0.5019 0.044(8) Uiso 0.50 1 d PR A 1 H182 H 0.4666 0.3260 0.5215 0.044(8) Uiso 0.50 1 d PR A 1 H183 H 0.4257 0.3989 0.4812 0.044(8) Uiso 0.50 1 d PR A 1 H184 H 0.5308 0.3597 0.5142 0.044(8) Uiso 0.50 1 d PR A 2 H185 H 0.4255 0.3482 0.5101 0.044(8) Uiso 0.50 1 d PR A 2 H186 H 0.4714 0.4242 0.4789 0.044(8) Uiso 0.50 1 d PR A 2 C19 C 0.4116(2) 0.1517(2) 0.32775(15) 0.0376(7) Uani 1 1 d . . . H191 H 0.3748 0.1746 0.2947 0.060(6) Uiso 1 1 d R . . H192 H 0.3751 0.1326 0.3616 0.060(6) Uiso 1 1 d R . . H193 H 0.4451 0.1058 0.3114 0.060(6) Uiso 1 1 d R . . C21 C 0.59891(18) 0.10217(16) 0.25135(12) 0.0252(6) Uani 1 1 d . . . C22 C 0.66888(17) 0.07187(17) 0.28786(12) 0.0269(6) Uani 1 1 d . . . C23 C 0.70155(19) -0.00629(18) 0.27677(14) 0.0331(7) Uani 1 1 d . . . H23 H 0.7502 -0.0247 0.3005 0.040 Uiso 1 1 d R . . C24 C 0.6658(2) -0.05801(17) 0.23236(15) 0.0344(7) Uani 1 1 d . . . C25 C 0.59376(19) -0.02990(17) 0.19904(13) 0.0310(6) Uani 1 1 d . . . H25 H 0.5660 -0.0655 0.1702 0.037 Uiso 1 1 d R . . C26 C 0.56057(18) 0.04858(17) 0.20710(12) 0.0281(6) Uani 1 1 d . . . C27 C 0.7121(2) 0.12188(19) 0.33900(14) 0.0341(7) Uani 1 1 d . . . H271 H 0.7584 0.0896 0.3588 0.059(7) Uiso 1 1 d R . . H272 H 0.6690 0.1368 0.3701 0.059(7) Uiso 1 1 d R . . H273 H 0.7371 0.1716 0.3212 0.059(7) Uiso 1 1 d R . . C28 C 0.7015(3) -0.1427(2) 0.2218(2) 0.0564(10) Uani 1 1 d . . . H281 H 0.7621 -0.1391 0.2084 0.103(10) Uiso 1 1 d R . . H282 H 0.6668 -0.1704 0.1897 0.103(10) Uiso 1 1 d R . . H283 H 0.6989 -0.1740 0.2605 0.103(10) Uiso 1 1 d R . . C29 C 0.4801(2) 0.0701(2) 0.16949(15) 0.0396(8) Uani 1 1 d . . . H291 H 0.4525 0.1187 0.1870 0.037(8) Uiso 0.50 1 d PR B 1 H292 H 0.4391 0.0242 0.1705 0.037(8) Uiso 0.50 1 d PR B 1 H293 H 0.4964 0.0810 0.1265 0.037(8) Uiso 0.50 1 d PR B 1 H294 H 0.4657 0.0320 0.1319 0.037(8) Uiso 0.50 1 d PR B 2 H295 H 0.4865 0.1248 0.1542 0.037(8) Uiso 0.50 1 d PR B 2 H296 H 0.4312 0.0698 0.1967 0.037(8) Uiso 0.50 1 d PR B 2 C31 C 0.7500 0.1645(4) 0.0000 0.0638(16) Uani 1 2 d S . . C32 C 0.7090(3) 0.1217(4) 0.0445(2) 0.0785(16) Uani 1 1 d . . . H32 H 0.6786 0.1508 0.0761 0.094 Uiso 1 1 d R . . C33 C 0.7094(3) 0.0387(5) 0.0453(3) 0.108(2) Uani 1 1 d . . . H33 H 0.6816 0.0095 0.0781 0.130 Uiso 1 1 d R . . C34 C 0.7500 -0.0020(6) 0.0000 0.132(4) Uani 1 2 d S . . H34 H 0.7500 -0.0606 0.0000 0.158 Uiso 1 2 d SR . . C35 C 0.7500 0.2561(5) 0.0000 0.170(6) Uani 1 2 d S . . H351 H 0.7179 0.2757 0.0349 0.255 Uiso 0.50 1 d PR . . H352 H 0.8087 0.2757 0.0028 0.255 Uiso 0.50 1 d PR . . H353 H 0.7234 0.2757 -0.0376 0.255 Uiso 0.50 1 d PR . . C41 C 0.2500 0.1044(3) 0.5000 0.113(3) Uani 1 2 d SGD . . C42 C 0.2091(3) 0.1258(4) 0.44249(10) 0.065(2) Uani 0.50 1 d PGD C -1 H42 H 0.1888 0.0839 0.4148 0.078 Uiso 0.50 1 d PR C -1 C43 C 0.1991(5) 0.2077(4) 0.4269(3) 0.088(3) Uiso 0.50 1 d PG C -1 H43 H 0.1715 0.2225 0.3883 0.105 Uiso 0.50 1 d PG C -1 C44 C 0.2290(7) 0.2681(3) 0.4670(4) 0.212(11) Uiso 0.50 1 d PG C -1 H44 H 0.2220 0.3246 0.4562 0.255 Uiso 0.50 1 d PG C -1 C45 C 0.2690(6) 0.2467(4) 0.5228(3) 0.079(3) Uiso 0.50 1 d PG C -1 H45 H 0.2896 0.2885 0.5506 0.094 Uiso 0.50 1 d PG C -1 C46 C 0.2791(3) 0.1649(4) 0.53845(16) 0.071(3) Uiso 0.50 1 d PGD C -1 H46 H 0.3070 0.1507 0.5770 0.085 Uiso 0.50 1 d PG C -1 C47 C 0.2512(13) 0.0171(5) 0.5147(6) 0.117(4) Uiso 0.50 1 d PD C -1 H471 H 0.2795 0.0077 0.5539 0.175 Uiso 0.50 1 d PR C -1 H472 H 0.1920 -0.0011 0.5166 0.175 Uiso 0.50 1 d PR C -1 H473 H 0.2808 -0.0126 0.4829 0.175 Uiso 0.50 1 d PR C -1 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 B 0.0257(15) 0.0290(16) 0.0251(15) 0.0058(12) 0.0038(12) -0.0012(12) C1 0.0466(18) 0.0286(15) 0.0218(13) 0.0020(11) 0.0046(12) 0.0042(13) C2 0.0347(15) 0.0269(14) 0.0194(12) -0.0001(11) -0.0002(11) 0.0012(11) C3 0.0359(15) 0.0258(14) 0.0205(13) 0.0029(11) -0.0022(11) -0.0006(12) C4 0.108(3) 0.0239(15) 0.0237(15) -0.0002(12) 0.0034(17) 0.0204(18) C5 0.112(3) 0.0284(16) 0.0160(14) -0.0021(12) 0.0024(17) 0.0167(18) C6 0.0372(15) 0.0238(13) 0.0186(12) 0.0017(10) -0.0027(11) 0.0021(11) C7 0.0523(19) 0.0283(15) 0.0235(14) 0.0027(12) 0.0064(13) 0.0135(13) C8 0.0493(18) 0.0325(15) 0.0191(13) 0.0024(11) 0.0067(12) 0.0126(13) C11 0.0281(14) 0.0260(13) 0.0206(12) 0.0064(10) -0.0014(10) 0.0028(11) C12 0.0287(14) 0.0300(14) 0.0227(13) 0.0047(11) 0.0003(11) 0.0012(11) C13 0.0304(15) 0.0318(15) 0.0261(14) 0.0012(11) -0.0057(11) 0.0024(12) C14 0.0297(15) 0.0433(17) 0.0210(13) -0.0022(12) -0.0017(11) 0.0079(13) C15 0.0257(14) 0.0431(17) 0.0258(14) 0.0058(12) 0.0032(11) 0.0019(12) C16 0.0247(13) 0.0289(14) 0.0254(13) 0.0047(11) -0.0024(10) 0.0007(11) C17 0.0414(17) 0.0386(17) 0.0326(16) -0.0007(13) 0.0076(13) -0.0110(14) C18 0.0397(19) 0.066(2) 0.0338(17) -0.0139(16) 0.0059(14) 0.0023(16) C19 0.0302(16) 0.0414(17) 0.0412(18) 0.0007(14) 0.0036(13) -0.0048(13) C21 0.0292(14) 0.0259(13) 0.0205(12) 0.0058(10) 0.0038(10) -0.0031(11) C22 0.0253(13) 0.0289(14) 0.0264(14) 0.0057(11) 0.0035(11) -0.0048(11) C23 0.0285(14) 0.0307(15) 0.0401(16) 0.0070(13) -0.0023(12) 0.0015(12) C24 0.0332(16) 0.0249(14) 0.0452(18) -0.0003(13) 0.0024(13) 0.0002(12) C25 0.0342(16) 0.0297(15) 0.0291(14) -0.0026(12) 0.0019(12) -0.0033(12) C26 0.0335(15) 0.0287(14) 0.0221(13) 0.0043(11) 0.0022(11) -0.0011(12) C27 0.0355(16) 0.0336(16) 0.0330(16) 0.0045(12) -0.0061(13) -0.0021(13) C28 0.053(2) 0.0348(19) 0.081(3) -0.0125(18) -0.015(2) 0.0116(16) C29 0.0460(18) 0.0380(17) 0.0344(16) -0.0011(13) -0.0122(14) 0.0039(14) C31 0.049(3) 0.081(4) 0.061(4) 0.000 -0.022(3) 0.000 C32 0.039(2) 0.151(5) 0.045(2) -0.016(3) -0.0099(18) 0.023(3) C33 0.048(3) 0.162(7) 0.115(5) 0.075(5) -0.005(3) -0.018(4) C34 0.072(6) 0.071(6) 0.251(15) 0.000 -0.021(8) 0.000 C35 0.149(9) 0.069(6) 0.290(16) 0.000 -0.124(10) 0.000 C41 0.060(5) 0.116(7) 0.165(9) 0.000 0.046(5) 0.000 C42 0.023(3) 0.111(7) 0.061(5) -0.020(5) -0.001(3) -0.015(4) _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 B C1 1.548(4) . ? B C21 1.581(4) . ? B C11 1.586(4) . ? C1 C2 1.341(4) . ? C1 H1 0.9474 . ? C2 C3 1.461(4) . ? C2 H2 0.9476 . ? C3 C8 1.381(4) . ? C3 C4 1.389(4) . ? C4 C5 1.377(4) . ? C4 H4 0.9477 . ? C5 C6 1.390(4) . ? C5 H5 0.9477 . ? C6 C7 1.383(4) . ? C6 C6 1.485(5) 5_665 ? C7 C8 1.385(4) . ? C7 H7 0.9476 . ? C8 H8 0.9476 . ? C11 C16 1.405(4) . ? C11 C12 1.412(4) . ? C12 C13 1.395(4) . ? C12 C17 1.513(4) . ? C13 C14 1.379(4) . ? C13 H13 0.9476 . ? C14 C15 1.388(4) . ? C14 C18 1.515(4) . ? C15 C16 1.395(4) . ? C15 H15 0.9476 . ? C16 C19 1.514(4) . ? C17 H171 0.9791 . ? C17 H172 0.9786 . ? C17 H173 0.9787 . ? C18 H181 0.9779 . ? C18 H182 0.9781 . ? C18 H183 0.9782 . ? C18 H184 0.9774 . ? C18 H185 0.9775 . ? C18 H186 0.9776 . ? C19 H191 0.9778 . ? C19 H192 0.9772 . ? C19 H193 0.9776 . ? C21 C22 1.412(4) . ? C21 C26 1.416(4) . ? C22 C23 1.393(4) . ? C22 C27 1.517(4) . ? C23 C24 1.384(4) . ? C23 H23 0.9474 . ? C24 C25 1.389(4) . ? C24 C28 1.507(4) . ? C25 C26 1.391(4) . ? C25 H25 0.9475 . ? C26 C29 1.510(4) . ? C27 H271 0.9787 . ? C27 H272 0.9787 . ? C27 H273 0.9784 . ? C28 H281 0.9782 . ? C28 H282 0.9781 . ? C28 H283 0.9780 . ? C29 H291 0.9780 . ? C29 H292 0.9778 . ? C29 H293 0.9781 . ? C29 H294 1.0405 . ? C29 H295 0.9577 . ? C29 H296 0.9575 . ? C31 C32 1.348(7) 2_655 ? C31 C32 1.348(7) . ? C31 C35 1.496(11) . ? C32 C33 1.355(9) . ? C32 H32 0.9576 . ? C33 C34 1.340(9) . ? C33 H33 0.9579 . ? C34 C33 1.340(9) 2_655 ? C34 H34 0.9577 . ? C35 H351 0.9575 . ? C35 H352 0.9575 . ? C35 H353 0.9574 . ? C41 C46 1.360(4) 2_556 ? C41 C46 1.3596 . ? C41 C42 1.4238(19) 2_556 ? C41 C42 1.4238 . ? C41 C47 1.461(8) . ? C41 C47 1.461(8) 2_556 ? C42 C43 1.3865 . ? C42 H42 0.9575 . ? C43 C44 1.3865 . ? C43 H43 0.9578 . ? C44 C45 1.3860 . ? C44 H44 0.9574 . ? C45 C46 1.3868 . ? C45 H45 0.9579 . ? C46 H46 0.9573 . ? C47 H471 0.9576 . ? C47 H472 0.9574 . ? C47 H473 0.9578 . ? 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 C1 B C21 117.4(2) . . ? C1 B C11 118.2(2) . . ? C21 B C11 124.4(2) . . ? C2 C1 B 124.2(3) . . ? C2 C1 H1 117.9 . . ? B C1 H1 117.8 . . ? C1 C2 C3 128.2(3) . . ? C1 C2 H2 115.9 . . ? C3 C2 H2 116.0 . . ? C8 C3 C4 116.9(2) . . ? C8 C3 C2 119.5(2) . . ? C4 C3 C2 123.6(3) . . ? C5 C4 C3 121.4(3) . . ? C5 C4 H4 119.2 . . ? C3 C4 H4 119.4 . . ? C4 C5 C6 121.8(3) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.0 . . ? C7 C6 C5 116.6(2) . . ? C7 C6 C6 121.8(3) . 5_665 ? C5 C6 C6 121.6(3) . 5_665 ? C6 C7 C8 121.6(3) . . ? C6 C7 H7 119.3 . . ? C8 C7 H7 119.1 . . ? C3 C8 C7 121.6(3) . . ? C3 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? C16 C11 C12 117.8(2) . . ? C16 C11 B 119.9(2) . . ? C12 C11 B 122.3(2) . . ? C13 C12 C11 120.0(3) . . ? C13 C12 C17 118.1(3) . . ? C11 C12 C17 121.9(2) . . ? C14 C13 C12 122.1(3) . . ? C14 C13 H13 118.9 . . ? C12 C13 H13 119.0 . . ? C13 C14 C15 118.1(3) . . ? C13 C14 C18 120.9(3) . . ? C15 C14 C18 121.0(3) . . ? C14 C15 C16 121.4(3) . . ? C14 C15 H15 119.3 . . ? C16 C15 H15 119.3 . . ? C15 C16 C11 120.6(3) . . ? C15 C16 C19 118.4(3) . . ? C11 C16 C19 120.9(2) . . ? C12 C17 H171 109.6 . . ? C12 C17 H172 109.4 . . ? H171 C17 H172 109.4 . . ? C12 C17 H173 109.8 . . ? H171 C17 H173 109.3 . . ? H172 C17 H173 109.3 . . ? C14 C18 H181 109.7 . . ? C14 C18 H182 109.6 . . ? H181 C18 H182 109.4 . . ? C14 C18 H183 109.3 . . ? H181 C18 H183 109.4 . . ? H182 C18 H183 109.4 . . ? C14 C18 H184 102.2 . . ? H181 C18 H184 44.6 . . ? H182 C18 H184 71.4 . . ? H183 C18 H184 145.5 . . ? C14 C18 H185 117.7 . . ? H181 C18 H185 131.6 . . ? H182 C18 H185 46.0 . . ? H183 C18 H185 64.0 . . ? H184 C18 H185 112.8 . . ? C14 C18 H186 107.8 . . ? H181 C18 H186 63.7 . . ? H182 C18 H186 141.8 . . ? H183 C18 H186 49.3 . . ? H184 C18 H186 107.9 . . ? H185 C18 H186 107.9 . . ? C16 C19 H191 109.5 . . ? C16 C19 H192 109.3 . . ? H191 C19 H192 109.5 . . ? C16 C19 H193 109.7 . . ? H191 C19 H193 109.5 . . ? H192 C19 H193 109.4 . . ? C22 C21 C26 117.7(2) . . ? C22 C21 B 121.8(2) . . ? C26 C21 B 120.4(2) . . ? C23 C22 C21 119.9(3) . . ? C23 C22 C27 117.5(3) . . ? C21 C22 C27 122.5(3) . . ? C24 C23 C22 122.5(3) . . ? C24 C23 H23 118.7 . . ? C22 C23 H23 118.8 . . ? C23 C24 C25 117.4(3) . . ? C23 C24 C28 121.5(3) . . ? C25 C24 C28 121.0(3) . . ? C24 C25 C26 122.1(3) . . ? C24 C25 H25 118.9 . . ? C26 C25 H25 119.0 . . ? C25 C26 C21 120.2(3) . . ? C25 C26 C29 116.5(3) . . ? C21 C26 C29 123.2(3) . . ? C22 C27 H271 109.5 . . ? C22 C27 H272 109.7 . . ? H271 C27 H272 109.3 . . ? C22 C27 H273 109.4 . . ? H271 C27 H273 109.4 . . ? H272 C27 H273 109.4 . . ? C24 C28 H281 109.7 . . ? C24 C28 H282 109.5 . . ? H281 C28 H282 109.4 . . ? C24 C28 H283 109.4 . . ? H281 C28 H283 109.4 . . ? H282 C28 H283 109.4 . . ? C26 C29 H291 109.7 . . ? C26 C29 H292 109.4 . . ? H291 C29 H292 109.4 . . ? C26 C29 H293 109.3 . . ? H291 C29 H293 109.4 . . ? H292 C29 H293 109.5 . . ? C26 C29 H294 116.2 . . ? H291 C29 H294 134.1 . . ? H292 C29 H294 55.2 . . ? H293 C29 H294 55.2 . . ? C26 C29 H295 108.3 . . ? H291 C29 H295 54.5 . . ? H292 C29 H295 142.2 . . ? H293 C29 H295 58.4 . . ? H294 C29 H295 108.2 . . ? C26 C29 H296 108.3 . . ? H291 C29 H296 54.7 . . ? H292 C29 H296 58.3 . . ? H293 C29 H296 142.4 . . ? H294 C29 H296 108.2 . . ? H295 C29 H296 107.4 . . ? C32 C31 C32 117.5(7) 2_655 . ? C32 C31 C35 121.2(4) 2_655 . ? C32 C31 C35 121.2(4) . . ? C31 C32 C33 121.7(5) . . ? C31 C32 H32 119.0 . . ? C33 C32 H32 119.3 . . ? C34 C33 C32 119.3(6) . . ? C34 C33 H33 120.3 . . ? C32 C33 H33 120.4 . . ? C33 C34 C33 120.5(9) . 2_655 ? C33 C34 H34 119.8 . . ? C33 C34 H34 119.8 2_655 . ? C31 C35 H351 109.5 . . ? C31 C35 H352 109.5 . . ? H351 C35 H352 109.5 . . ? C31 C35 H353 109.5 . . ? H351 C35 H353 109.5 . . ? H352 C35 H353 109.5 . . ? C46 C41 C42 119.2 . . ? C46 C41 C47 125.1(5) . . ? C42 C41 C47 115.5(5) . . ? C43 C42 C41 119.6 . . ? C43 C42 H42 120.2 . . ? C41 C42 H42 120.2 . . ? C42 C43 C44 120.0 . . ? C45 C44 C43 120.0 . . ? C44 C45 C46 120.0 . . ? C41 C46 C45 121.2 . . ? C41 C46 H46 119.4 . . ? C41 C47 H471 110.5 . . ? C41 C47 H472 107.7 . . ? H471 C47 H472 109.5 . . ? C41 C47 H473 110.2 . . ? H471 C47 H473 109.5 . . ? H472 C47 H473 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 C12 C11 B C1 -63.9(4) . . . . ? C11 B C1 C2 -9.4(4) . . . . ? B C1 C2 C3 179.5(3) . . . . ? C1 C2 C3 C4 8.4(5) . . . . ? C26 C21 B C1 -47.8(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.874 _refine_diff_density_min -0.502 _refine_diff_density_rms 0.061 #======================================END data_1m _database_code_depnum_ccdc_archive 'CCDC 724818' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 5,5'-bis(E-dimesitylborylethenyl)terthiophene, dichloromethane solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H54 B2 S3,1.5(C H2 Cl2)' _chemical_formula_sum 'C53.5 H57 B2 Cl3 S3' _chemical_formula_weight 924.14 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' B B 0.0013 0.0007 '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' Cl Cl 0.1484 0.1585 '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 11.7193(9) _cell_length_b 12.0933(9) _cell_length_c 18.1746(14) _cell_angle_alpha 84.01(3) _cell_angle_beta 78.79(2) _cell_angle_gamma 81.32(2) _cell_volume 2490.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 1018 _cell_measurement_theta_min 5.9 _cell_measurement_theta_max 60.8 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.232 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 974 _exptl_absorpt_coefficient_mu 0.345 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ;The data collection nominally covered full sphere of reciprocal space, by a combination of 3 runs of narrow-frame \w-scans (scan width 0.3\% \w), every run at a different \f angle. Crystal to detector distance 4.85 cm. ; _diffrn_ambient_temperature 120(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 'SMART 6K CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 5.6 _diffrn_standards_number 0 _diffrn_reflns_number 34061 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_sigmaI/netI 0.0464 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 30.50 _reflns_number_total 15077 _reflns_number_gt 10008 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART V5.625 (Bruker, 2001)' _computing_cell_refinement 'SMART V5.625 (Bruker, 2001)' _computing_data_reduction 'SAINT V6.45 (Bruker, 2001)' _computing_structure_solution 'SHELXTL version 6.14 (Bruker, 2003)' _computing_structure_refinement 'SHELXTL version 6.14 (Bruker, 2003)' _computing_molecular_graphics 'SHELXTL version 6.14 (Bruker, 2003)' _computing_publication_material 'SHELXTL version 6.14 (Bruker, 2003)' _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. Methyl groups were refined as rigid bodies rotating around C---C bonds, with a common refined U for three H atoms. Other H atoms: riding model. The host packing leaves cavities centred on (0 0 1/2) with the volume of 396 \%A^3^ and total electron density of 111.5 electrons per unit cell, as calculated using SQUEEZE program of PLATON package. We assumed this cavity to contain three chaotically disordered molecules of DCM, which were approximated by arbitrary Cl and C atoms with partial occupancies. ; _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^)+(0.0877P)^2^+1.0816P] 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 15077 _refine_ls_number_parameters 607 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0952 _refine_ls_R_factor_gt 0.0583 _refine_ls_wR_factor_ref 0.1752 _refine_ls_wR_factor_gt 0.1506 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 S1 S 1.26267(4) -0.18221(4) 0.12788(3) 0.02703(11) Uani 1 1 d . . . S2 S 0.89489(4) -0.04578(5) 0.12791(3) 0.03522(13) Uani 1 1 d . . . S3 S 0.65881(4) 0.12998(4) 0.30729(3) 0.03055(12) Uani 1 1 d . . . C1 C 1.52657(16) -0.29707(16) 0.06117(11) 0.0279(4) Uani 1 1 d . . . H1 H 1.5019 -0.2927 0.1145 0.033 Uiso 1 1 d R . . C2 C 1.44835(16) -0.26004(15) 0.01581(11) 0.0265(4) Uani 1 1 d . . . H2 H 1.4785 -0.2601 -0.0372 0.032 Uiso 1 1 d R . . C3 C 1.32462(16) -0.21921(15) 0.03764(11) 0.0257(4) Uani 1 1 d . . . C4 C 1.24132(17) -0.20429(17) -0.00741(12) 0.0292(4) Uani 1 1 d . . . H4 H 1.2578 -0.2218 -0.0590 0.035 Uiso 1 1 d R . . C5 C 1.12821(17) -0.16152(17) 0.03014(12) 0.0294(4) Uani 1 1 d . . . H5 H 1.0605 -0.1460 0.0064 0.035 Uiso 1 1 d R . . C6 C 1.12536(16) -0.14388(15) 0.10354(11) 0.0262(4) Uani 1 1 d . . . C7 C 1.02695(16) -0.09391(16) 0.15704(12) 0.0286(4) Uani 1 1 d . . . C8 C 1.02045(18) -0.0737(2) 0.23010(13) 0.0369(5) Uani 1 1 d . . . H8 H 1.0850 -0.0938 0.2564 0.044 Uiso 1 1 d R . . C9 C 0.90969(19) -0.0198(2) 0.26321(13) 0.0386(5) Uani 1 1 d . . . H9 H 0.8910 0.0001 0.3144 0.046 Uiso 1 1 d R . . C10 C 0.83149(17) 0.00154(17) 0.21482(12) 0.0303(4) Uani 1 1 d . . . C11 C 0.71270(17) 0.05991(17) 0.22691(11) 0.0299(4) Uani 1 1 d . . . C12 C 0.63117(17) 0.07387(19) 0.18048(12) 0.0337(4) Uani 1 1 d . . . H12 H 0.6438 0.0396 0.1337 0.040 Uiso 1 1 d R . . C13 C 0.52629(17) 0.14268(18) 0.20900(12) 0.0328(4) Uani 1 1 d . . . H13 H 0.4611 0.1615 0.1831 0.039 Uiso 1 1 d R . . C14 C 0.52758(16) 0.18008(17) 0.27740(11) 0.0288(4) Uani 1 1 d . . . C15 C 0.43745(17) 0.25414(17) 0.32174(11) 0.0309(4) Uani 1 1 d . . . H15 H 0.3699 0.2855 0.3002 0.037 Uiso 1 1 d R . . C16 C 0.43969(19) 0.28218(19) 0.39093(12) 0.0371(5) Uani 1 1 d . . . H16 H 0.5100 0.2576 0.4110 0.045 Uiso 1 1 d R . . C17 C 1.70868(15) -0.30375(15) -0.05260(11) 0.0249(4) Uani 1 1 d . . . C18 C 1.74746(15) -0.37845(15) -0.11003(11) 0.0251(4) Uani 1 1 d . . . C19 C 1.78595(16) -0.33679(16) -0.18390(11) 0.0279(4) Uani 1 1 d . . . H19 H 1.8081 -0.3879 -0.2228 0.034 Uiso 1 1 d R . . C20 C 1.79309(17) -0.22307(17) -0.20279(12) 0.0295(4) Uani 1 1 d . . . C21 C 1.75953(17) -0.15039(16) -0.14542(12) 0.0303(4) Uani 1 1 d . . . H21 H 1.7661 -0.0721 -0.1571 0.036 Uiso 1 1 d R . . C22 C 1.71630(16) -0.18836(16) -0.07173(11) 0.0278(4) Uani 1 1 d . . . C23 C 1.75010(17) -0.50371(16) -0.09313(12) 0.0303(4) Uani 1 1 d . . . H23A H 1.7604 -0.5390 -0.1394 0.046(4) Uiso 1 1 d R . . H23B H 1.8139 -0.5329 -0.0675 0.046(4) Uiso 1 1 d R . . H23C H 1.6773 -0.5192 -0.0618 0.046(4) Uiso 1 1 d R . . C24 C 1.8375(2) -0.17993(19) -0.28278(13) 0.0378(5) Uani 1 1 d . . . H24A H 1.8653 -0.2420 -0.3134 0.063(5) Uiso 1 1 d R . . H24B H 1.7747 -0.1330 -0.3022 0.063(5) Uiso 1 1 d R . . H24C H 1.9004 -0.1372 -0.2835 0.063(5) Uiso 1 1 d R . . C25 C 1.6841(2) -0.10310(17) -0.01289(13) 0.0360(5) Uani 1 1 d . . . H25A H 1.7394 -0.0494 -0.0223 0.077(6) Uiso 1 1 d R . . H25B H 1.6064 -0.0637 -0.0143 0.077(6) Uiso 1 1 d R . . H25C H 1.6853 -0.1407 0.0366 0.077(6) Uiso 1 1 d R . . C26 C 1.72248(15) -0.43921(16) 0.07912(11) 0.0256(4) Uani 1 1 d . . . C27 C 1.66506(16) -0.52543(16) 0.12368(11) 0.0267(4) Uani 1 1 d . . . C28 C 1.72370(17) -0.60232(18) 0.17068(12) 0.0329(4) Uani 1 1 d . . . H28 H 1.6832 -0.6604 0.1997 0.039 Uiso 1 1 d R . . C29 C 1.83894(19) -0.5971(2) 0.17670(14) 0.0395(5) Uani 1 1 d . . . C30 C 1.89613(17) -0.51405(19) 0.13245(14) 0.0368(5) Uani 1 1 d . . . H30 H 1.9762 -0.5098 0.1355 0.044 Uiso 1 1 d R . . C31 C 1.84128(16) -0.43661(17) 0.08415(12) 0.0298(4) Uani 1 1 d . . . C32 C 1.54013(17) -0.54031(18) 0.12156(12) 0.0316(4) Uani 1 1 d . . . H32A H 1.5246 -0.6131 0.1444 0.045(4) Uiso 1 1 d R . . H32B H 1.4869 -0.4836 0.1486 0.045(4) Uiso 1 1 d R . . H32C H 1.5291 -0.5338 0.0702 0.045(4) Uiso 1 1 d R . . C33 C 1.8999(2) -0.6789(3) 0.22947(19) 0.0629(9) Uani 1 1 d . . . H33A H 1.8427 -0.7062 0.2700 0.100(8) Uiso 1 1 d R . . H33B H 1.9435 -0.7410 0.2028 0.100(8) Uiso 1 1 d R . . H33C H 1.9527 -0.6419 0.2497 0.100(8) Uiso 1 1 d R . . C34 C 1.91163(18) -0.34800(19) 0.04011(14) 0.0391(5) Uani 1 1 d . . . H34A H 1.9859 -0.3536 0.0561 0.061(5) Uiso 1 1 d R . . H34B H 1.9245 -0.3591 -0.0126 0.061(5) Uiso 1 1 d R . . H34C H 1.8687 -0.2750 0.0488 0.061(5) Uiso 1 1 d R . . C35 C 0.33031(19) 0.33373(18) 0.52793(12) 0.0338(4) Uani 1 1 d . . . C36 C 0.3374(2) 0.2240(2) 0.56394(13) 0.0401(5) Uani 1 1 d . . . C37 C 0.3366(2) 0.2079(2) 0.64119(13) 0.0437(5) Uani 1 1 d . . . H37 H 0.3395 0.1330 0.6648 0.052 Uiso 1 1 d R . . C38 C 0.3322(2) 0.2961(2) 0.68464(13) 0.0442(5) Uani 1 1 d . . . C39 C 0.3248(2) 0.4041(2) 0.64975(14) 0.0415(5) Uani 1 1 d . . . H39 H 0.3196 0.4667 0.6792 0.050 Uiso 1 1 d R . . C40 C 0.32325(19) 0.42436(19) 0.57260(13) 0.0365(5) Uani 1 1 d . . . C41 C 0.3408(3) 0.1208(2) 0.52290(16) 0.0610(8) Uani 1 1 d . . . H41A H 0.3149 0.0605 0.5580 0.099(8) Uiso 1 1 d R . . H41B H 0.2898 0.1377 0.4865 0.099(8) Uiso 1 1 d R . . H41C H 0.4196 0.0981 0.4975 0.099(8) Uiso 1 1 d R . . C42 C 0.3320(3) 0.2751(3) 0.76758(15) 0.0643(8) Uani 1 1 d . . . H42A H 0.3902 0.2120 0.7769 0.105(8) Uiso 1 1 d R . . H42B H 0.3501 0.3405 0.7873 0.105(8) Uiso 1 1 d R . . H42C H 0.2559 0.2582 0.7942 0.105(8) Uiso 1 1 d R . . C43 C 0.3171(2) 0.5441(2) 0.53920(16) 0.0485(6) Uani 1 1 d . . . H43A H 0.3008 0.5944 0.5786 0.072(6) Uiso 1 1 d R . . H43B H 0.3905 0.5555 0.5072 0.072(6) Uiso 1 1 d R . . H43C H 0.2554 0.5587 0.5101 0.072(6) Uiso 1 1 d R . . C44 C 0.24189(18) 0.43078(17) 0.40106(12) 0.0317(4) Uani 1 1 d . . . C45 C 0.27456(19) 0.51734(18) 0.34604(13) 0.0353(4) Uani 1 1 d . . . C46 C 0.1903(2) 0.58301(19) 0.30983(13) 0.0398(5) Uani 1 1 d . . . H46 H 0.2135 0.6427 0.2735 0.048 Uiso 1 1 d R . . C47 C 0.0733(2) 0.5649(2) 0.32513(14) 0.0409(5) Uani 1 1 d . . . C48 C 0.0409(2) 0.48032(19) 0.37970(14) 0.0387(5) Uani 1 1 d . . . H48 H -0.0397 0.4675 0.3918 0.046 Uiso 1 1 d R . . C49 C 0.12236(18) 0.41425(18) 0.41787(12) 0.0333(4) Uani 1 1 d . . . C50 C 0.3993(2) 0.5444(2) 0.32607(16) 0.0501(6) Uani 1 1 d . . . H50A H 0.4009 0.6164 0.2984 0.086(7) Uiso 1 1 d R . . H50B H 0.4300 0.5454 0.3713 0.086(7) Uiso 1 1 d R . . H50C H 0.4466 0.4879 0.2958 0.086(7) Uiso 1 1 d R . . C51 C -0.0158(3) 0.6359(3) 0.28458(19) 0.0597(8) Uani 1 1 d . . . H51A H -0.0696 0.5899 0.2735 0.095(7) Uiso 1 1 d R . . H51B H -0.0587 0.6935 0.3158 0.095(7) Uiso 1 1 d R . . H51C H 0.0233 0.6704 0.2383 0.095(7) Uiso 1 1 d R . . C52 C 0.0792(2) 0.3230(2) 0.47575(14) 0.0427(5) Uani 1 1 d . . . H52A H -0.0049 0.3299 0.4837 0.066(5) Uiso 1 1 d R . . H52B H 0.1120 0.2510 0.4579 0.066(5) Uiso 1 1 d R . . H52C H 0.1036 0.3301 0.5223 0.066(5) Uiso 1 1 d R . . B1 B 1.65490(18) -0.34771(18) 0.02998(13) 0.0260(4) Uani 1 1 d . . . B2 B 0.3359(2) 0.3519(2) 0.44035(14) 0.0331(5) Uani 1 1 d . . . Cl1 Cl 0.6734(4) 0.1573(3) 0.5226(3) 0.181(2) Uani 0.50 1 d P . . Cl2 Cl 0.6583(5) 0.1177(3) 0.6867(3) 0.191(2) Uani 0.50 1 d P . . Cl3 Cl 0.9029(10) 0.0921(9) 0.5845(4) 0.167(4) Uani 0.25 1 d P . . Cl4 Cl 0.8357(6) 0.1608(4) 0.4492(3) 0.122(2) Uani 0.25 1 d P . . Cl5 Cl 0.7724(6) 0.2065(5) 0.6178(4) 0.128(2) Uani 0.25 1 d P . . Cl6 Cl 0.6106(5) 0.0500(5) 0.6447(3) 0.1172(16) Uiso 0.25 1 d P . . Cl7 Cl 0.6589(9) 0.1658(8) 0.5909(6) 0.138(3) Uiso 0.20 1 d P . . C01 C 0.7861(11) 0.1700(11) 0.5513(7) 0.121(3) Uiso 0.50 1 d P . . C02 C 0.918(2) 0.062(2) 0.4736(16) 0.135(8) Uiso 0.25 1 d P . . C03 C 0.8845(14) 0.0827(14) 0.5647(9) 0.110(5) Uiso 0.50 1 d P . . C04 C 0.989(2) 0.004(2) 0.5342(12) 0.120(7) Uiso 0.25 1 d P . . 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 0.0232(2) 0.0267(2) 0.0285(2) -0.00235(17) -0.00210(17) 0.00224(16) S2 0.0245(2) 0.0444(3) 0.0329(3) -0.0066(2) -0.00249(19) 0.0067(2) S3 0.0256(2) 0.0337(3) 0.0282(2) -0.00093(19) -0.00220(17) 0.00476(18) C1 0.0253(9) 0.0265(9) 0.0291(9) -0.0033(7) -0.0011(7) 0.0016(7) C2 0.0226(8) 0.0245(9) 0.0297(9) -0.0020(7) 0.0004(7) -0.0010(7) C3 0.0239(8) 0.0216(8) 0.0284(9) -0.0010(7) -0.0001(7) 0.0003(6) C4 0.0252(9) 0.0313(10) 0.0299(10) -0.0024(8) -0.0036(7) -0.0013(7) C5 0.0232(9) 0.0308(10) 0.0332(10) -0.0020(8) -0.0048(7) -0.0015(7) C6 0.0205(8) 0.0234(8) 0.0322(10) -0.0009(7) -0.0016(7) -0.0003(6) C7 0.0216(8) 0.0258(9) 0.0355(10) -0.0027(7) -0.0007(7) 0.0004(7) C8 0.0259(10) 0.0456(12) 0.0368(11) -0.0098(9) -0.0056(8) 0.0068(8) C9 0.0287(10) 0.0492(13) 0.0344(11) -0.0093(9) -0.0034(8) 0.0070(9) C10 0.0236(9) 0.0312(10) 0.0320(10) -0.0027(8) 0.0004(7) 0.0022(7) C11 0.0254(9) 0.0299(10) 0.0303(10) -0.0020(8) 0.0006(7) 0.0015(7) C12 0.0251(9) 0.0409(11) 0.0328(10) -0.0071(9) -0.0010(8) 0.0001(8) C13 0.0232(9) 0.0404(11) 0.0323(10) -0.0040(8) -0.0026(7) 0.0012(8) C14 0.0228(8) 0.0303(10) 0.0296(9) 0.0024(7) -0.0013(7) 0.0005(7) C15 0.0257(9) 0.0344(10) 0.0281(9) 0.0021(8) -0.0019(7) 0.0030(7) C16 0.0317(10) 0.0428(12) 0.0330(11) -0.0034(9) -0.0049(8) 0.0064(9) C17 0.0189(8) 0.0230(8) 0.0318(9) -0.0019(7) -0.0036(7) -0.0007(6) C18 0.0186(8) 0.0232(8) 0.0328(10) -0.0021(7) -0.0041(7) -0.0011(6) C19 0.0239(8) 0.0286(9) 0.0306(9) -0.0046(7) -0.0042(7) -0.0007(7) C20 0.0239(9) 0.0315(10) 0.0321(10) 0.0011(8) -0.0060(7) -0.0023(7) C21 0.0274(9) 0.0244(9) 0.0380(11) 0.0022(8) -0.0059(8) -0.0038(7) C22 0.0245(9) 0.0247(9) 0.0335(10) -0.0033(7) -0.0052(7) -0.0009(7) C23 0.0278(9) 0.0240(9) 0.0373(11) -0.0036(8) -0.0028(8) -0.0012(7) C24 0.0379(11) 0.0390(12) 0.0339(11) 0.0050(9) -0.0051(9) -0.0044(9) C25 0.0434(12) 0.0247(9) 0.0391(11) -0.0063(8) -0.0049(9) -0.0027(8) C26 0.0207(8) 0.0252(9) 0.0299(9) -0.0037(7) -0.0036(7) -0.0002(6) C27 0.0221(8) 0.0289(9) 0.0286(9) -0.0029(7) -0.0035(7) -0.0025(7) C28 0.0273(9) 0.0317(10) 0.0389(11) 0.0060(8) -0.0081(8) -0.0046(8) C29 0.0307(10) 0.0383(12) 0.0487(13) 0.0088(10) -0.0135(9) -0.0019(8) C30 0.0211(9) 0.0388(11) 0.0502(13) 0.0017(9) -0.0101(8) -0.0020(8) C31 0.0225(8) 0.0295(10) 0.0364(10) -0.0004(8) -0.0042(7) -0.0037(7) C32 0.0248(9) 0.0339(10) 0.0365(11) 0.0027(8) -0.0074(8) -0.0065(7) C33 0.0369(13) 0.0651(18) 0.086(2) 0.0340(16) -0.0268(14) -0.0099(12) C34 0.0258(10) 0.0393(12) 0.0522(14) 0.0052(10) -0.0076(9) -0.0093(8) C35 0.0336(10) 0.0345(11) 0.0305(10) -0.0061(8) -0.0010(8) 0.0001(8) C36 0.0514(13) 0.0357(11) 0.0321(11) -0.0055(9) -0.0081(9) 0.0005(10) C37 0.0549(14) 0.0439(13) 0.0309(11) -0.0014(9) -0.0077(10) -0.0031(11) C38 0.0417(13) 0.0583(15) 0.0314(11) -0.0073(10) -0.0042(9) -0.0032(11) C39 0.0365(11) 0.0490(13) 0.0402(12) -0.0162(10) -0.0049(9) -0.0031(10) C40 0.0302(10) 0.0372(11) 0.0413(12) -0.0103(9) -0.0031(9) -0.0014(8) C41 0.108(3) 0.0327(13) 0.0426(14) -0.0030(11) -0.0193(15) -0.0033(14) C42 0.078(2) 0.082(2) 0.0327(13) -0.0105(14) -0.0118(13) -0.0041(17) C43 0.0540(15) 0.0371(12) 0.0542(15) -0.0133(11) -0.0049(12) -0.0053(11) C44 0.0299(10) 0.0305(10) 0.0310(10) -0.0035(8) 0.0005(8) 0.0010(7) C45 0.0313(10) 0.0337(11) 0.0366(11) 0.0003(8) 0.0010(8) -0.0017(8) C46 0.0405(12) 0.0339(11) 0.0404(12) 0.0037(9) -0.0033(9) 0.0003(9) C47 0.0388(12) 0.0358(11) 0.0464(13) -0.0053(10) -0.0098(10) 0.0041(9) C48 0.0308(10) 0.0392(12) 0.0433(12) -0.0062(9) -0.0025(9) 0.0007(8) C49 0.0306(10) 0.0337(10) 0.0324(10) -0.0055(8) 0.0012(8) -0.0010(8) C50 0.0369(12) 0.0529(15) 0.0549(16) 0.0102(12) 0.0004(11) -0.0095(11) C51 0.0509(16) 0.0532(16) 0.074(2) 0.0061(14) -0.0245(14) 0.0067(12) C52 0.0396(12) 0.0430(13) 0.0414(13) 0.0012(10) 0.0029(10) -0.0085(10) B1 0.0217(9) 0.0245(10) 0.0314(11) -0.0046(8) -0.0046(8) -0.0009(7) B2 0.0322(11) 0.0323(11) 0.0328(12) -0.0037(9) -0.0027(9) -0.0014(9) Cl1 0.211(4) 0.0863(19) 0.281(6) 0.044(3) -0.157(4) -0.026(2) Cl2 0.254(5) 0.089(2) 0.256(5) -0.013(3) -0.152(4) 0.034(2) Cl3 0.235(10) 0.189(8) 0.069(4) 0.047(4) -0.069(5) 0.006(6) Cl4 0.194(6) 0.086(3) 0.119(4) -0.008(3) -0.098(4) -0.030(3) Cl5 0.167(6) 0.094(3) 0.147(5) 0.010(3) -0.080(4) -0.042(4) _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 C6 1.7346(19) . ? S1 C3 1.7348(19) . ? S2 C10 1.726(2) . ? S2 C7 1.731(2) . ? S3 C11 1.729(2) . ? S3 C14 1.733(2) . ? C1 C2 1.347(3) . ? C1 B1 1.556(3) . ? C1 H1 0.9600 . ? C2 C3 1.451(2) . ? C2 H2 0.9600 . ? C3 C4 1.372(3) . ? C4 C5 1.416(3) . ? C4 H4 0.9599 . ? C5 C6 1.366(3) . ? C5 H5 0.9602 . ? C6 C7 1.455(3) . ? C7 C8 1.361(3) . ? C8 C9 1.412(3) . ? C8 H8 0.9600 . ? C9 C10 1.369(3) . ? C9 H9 0.9601 . ? C10 C11 1.450(3) . ? C11 C12 1.374(3) . ? C12 C13 1.416(3) . ? C12 H12 0.9601 . ? C13 C14 1.370(3) . ? C13 H13 0.9598 . ? C14 C15 1.450(3) . ? C15 C16 1.342(3) . ? C15 H15 0.9601 . ? C16 B2 1.556(3) . ? C16 H16 0.9599 . ? C17 C22 1.414(3) . ? C17 C18 1.414(3) . ? C17 B1 1.581(3) . ? C18 C19 1.397(3) . ? C18 C23 1.511(3) . ? C19 C20 1.393(3) . ? C19 H19 0.9600 . ? C20 C21 1.394(3) . ? C20 C24 1.512(3) . ? C21 C22 1.393(3) . ? C21 H21 0.9600 . ? C22 C25 1.518(3) . ? C23 H23A 0.9609 . ? C23 H23B 0.9607 . ? C23 H23C 0.9607 . ? C24 H24A 0.9602 . ? C24 H24B 0.9602 . ? C24 H24C 0.9601 . ? C25 H25A 0.9660 . ? C25 H25B 0.9660 . ? C25 H25C 0.9657 . ? C26 C31 1.418(3) . ? C26 C27 1.421(3) . ? C26 B1 1.566(3) . ? C27 C28 1.391(3) . ? C27 C32 1.510(3) . ? C28 C29 1.387(3) . ? C28 H28 0.9601 . ? C29 C30 1.389(3) . ? C29 C33 1.504(3) . ? C30 C31 1.388(3) . ? C30 H30 0.9600 . ? C31 C34 1.516(3) . ? C32 H32A 0.9608 . ? C32 H32B 0.9609 . ? C32 H32C 0.9607 . ? C33 H33A 0.9615 . ? C33 H33B 0.9616 . ? C33 H33C 0.9614 . ? C34 H34A 0.9603 . ? C34 H34B 0.9605 . ? C34 H34C 0.9601 . ? C35 C40 1.414(3) . ? C35 C36 1.415(3) . ? C35 B2 1.574(3) . ? C36 C37 1.396(3) . ? C36 C41 1.511(3) . ? C37 C38 1.381(4) . ? C37 H37 0.9599 . ? C38 C39 1.389(4) . ? C38 C42 1.502(4) . ? C39 C40 1.401(3) . ? C39 H39 0.9599 . ? C40 C43 1.508(3) . ? C41 H41A 0.9625 . ? C41 H41B 0.9623 . ? C41 H41C 0.9626 . ? C42 H42A 0.9682 . ? C42 H42B 0.9687 . ? C42 H42C 0.9689 . ? C43 H43A 0.9605 . ? C43 H43B 0.9604 . ? C43 H43C 0.9602 . ? C44 C45 1.413(3) . ? C44 C49 1.414(3) . ? C44 B2 1.575(3) . ? C45 C46 1.395(3) . ? C45 C50 1.513(3) . ? C46 C47 1.390(3) . ? C46 H46 0.9600 . ? C47 C48 1.390(3) . ? C47 C51 1.506(3) . ? C48 C49 1.394(3) . ? C48 H48 0.9600 . ? C49 C52 1.516(3) . ? C50 H50A 0.9601 . ? C50 H50B 0.9604 . ? C50 H50C 0.9604 . ? C51 H51A 0.9624 . ? C51 H51B 0.9624 . ? C51 H51C 0.9626 . ? C52 H52A 0.9604 . ? C52 H52B 0.9602 . ? C52 H52C 0.9603 . ? Cl1 Cl7 1.233(10) . ? Cl1 C01 1.544(13) . ? Cl1 Cl4 2.104(9) . ? Cl1 Cl5 2.428(7) . ? Cl2 Cl6 1.414(7) . ? Cl2 Cl7 1.775(11) . ? Cl2 Cl5 2.003(9) . ? Cl3 C04 1.58(3) . ? Cl3 C01 1.715(16) . ? Cl3 Cl5 1.949(13) . ? Cl3 C02 2.05(3) . ? Cl4 C02 1.50(3) . ? Cl4 C01 1.843(14) . ? Cl5 C01 1.303(13) . ? Cl5 Cl7 1.658(11) . ? Cl5 C03 2.029(18) . ? Cl6 Cl7 1.725(11) . ? Cl7 C01 1.530(15) . ? C01 C03 1.480(18) . ? C02 C04 1.24(3) 2_756 ? C02 C04 1.56(4) . ? C02 C03 1.66(3) . ? C03 C04 1.49(3) . ? C04 C04 1.23(4) 2_756 ? C04 C02 1.24(3) 2_756 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 S1 C3 91.88(9) . . ? C10 S2 C7 92.18(10) . . ? C11 S3 C14 92.12(10) . . ? C2 C1 B1 122.09(18) . . ? C2 C1 H1 118.8 . . ? B1 C1 H1 119.1 . . ? C1 C2 C3 127.69(18) . . ? C1 C2 H2 115.9 . . ? C3 C2 H2 116.4 . . ? C4 C3 C2 126.65(18) . . ? C4 C3 S1 110.72(14) . . ? C2 C3 S1 122.63(15) . . ? C3 C4 C5 113.23(18) . . ? C3 C4 H4 123.4 . . ? C5 C4 H4 123.3 . . ? C6 C5 C4 113.09(18) . . ? C6 C5 H5 123.4 . . ? C4 C5 H5 123.6 . . ? C5 C6 C7 128.03(18) . . ? C5 C6 S1 111.06(14) . . ? C7 C6 S1 120.81(15) . . ? C8 C7 C6 130.03(19) . . ? C8 C7 S2 110.66(14) . . ? C6 C7 S2 119.27(16) . . ? C7 C8 C9 113.41(19) . . ? C7 C8 H8 123.2 . . ? C9 C8 H8 123.3 . . ? C10 C9 C8 113.1(2) . . ? C10 C9 H9 123.3 . . ? C8 C9 H9 123.6 . . ? C9 C10 C11 129.14(19) . . ? C9 C10 S2 110.65(15) . . ? C11 C10 S2 120.14(16) . . ? C12 C11 C10 129.09(19) . . ? C12 C11 S3 110.73(15) . . ? C10 C11 S3 120.12(16) . . ? C11 C12 C13 113.23(19) . . ? C11 C12 H12 123.3 . . ? C13 C12 H12 123.5 . . ? C14 C13 C12 112.97(19) . . ? C14 C13 H13 123.4 . . ? C12 C13 H13 123.7 . . ? C13 C14 C15 127.98(19) . . ? C13 C14 S3 110.94(15) . . ? C15 C14 S3 121.06(16) . . ? C16 C15 C14 125.53(19) . . ? C16 C15 H15 116.9 . . ? C14 C15 H15 117.6 . . ? C15 C16 B2 124.2(2) . . ? C15 C16 H16 117.7 . . ? B2 C16 H16 118.1 . . ? C22 C17 C18 118.08(18) . . ? C22 C17 B1 121.05(17) . . ? C18 C17 B1 120.84(16) . . ? C19 C18 C17 119.92(17) . . ? C19 C18 C23 118.75(17) . . ? C17 C18 C23 121.32(17) . . ? C20 C19 C18 121.92(18) . . ? C20 C19 H19 119.0 . . ? C18 C19 H19 119.1 . . ? C19 C20 C21 117.90(19) . . ? C19 C20 C24 121.13(19) . . ? C21 C20 C24 120.96(19) . . ? C22 C21 C20 121.71(18) . . ? C22 C21 H21 119.2 . . ? C20 C21 H21 119.0 . . ? C21 C22 C17 120.35(18) . . ? C21 C22 C25 117.81(18) . . ? C17 C22 C25 121.76(18) . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.7 . . ? H23A C23 H23B 109.4 . . ? C18 C23 H23C 109.4 . . ? H23A C23 H23C 109.4 . . ? H23B C23 H23C 109.4 . . ? C20 C24 H24A 109.7 . . ? C20 C24 H24B 109.3 . . ? H24A C24 H24B 109.4 . . ? C20 C24 H24C 109.5 . . ? H24A C24 H24C 109.4 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 110.3 . . ? C22 C25 H25B 110.0 . . ? H25A C25 H25B 108.9 . . ? C22 C25 H25C 109.9 . . ? H25A C25 H25C 108.8 . . ? H25B C25 H25C 108.9 . . ? C31 C26 C27 117.10(17) . . ? C31 C26 B1 121.75(17) . . ? C27 C26 B1 121.08(16) . . ? C28 C27 C26 120.72(17) . . ? C28 C27 C32 116.74(18) . . ? C26 C27 C32 122.53(17) . . ? C29 C28 C27 121.7(2) . . ? C29 C28 H28 119.3 . . ? C27 C28 H28 119.1 . . ? C28 C29 C30 117.9(2) . . ? C28 C29 C33 121.0(2) . . ? C30 C29 C33 121.1(2) . . ? C31 C30 C29 122.23(19) . . ? C31 C30 H30 118.9 . . ? C29 C30 H30 118.9 . . ? C30 C31 C26 120.36(19) . . ? C30 C31 C34 117.49(18) . . ? C26 C31 C34 122.11(18) . . ? C27 C32 H32A 109.6 . . ? C27 C32 H32B 109.7 . . ? H32A C32 H32B 109.4 . . ? C27 C32 H32C 109.4 . . ? H32A C32 H32C 109.4 . . ? H32B C32 H32C 109.4 . . ? C29 C33 H33A 109.7 . . ? C29 C33 H33B 109.8 . . ? H33A C33 H33B 109.2 . . ? C29 C33 H33C 109.4 . . ? H33A C33 H33C 109.3 . . ? H33B C33 H33C 109.4 . . ? C31 C34 H34A 109.8 . . ? C31 C34 H34B 109.3 . . ? H34A C34 H34B 109.4 . . ? C31 C34 H34C 109.3 . . ? H34A C34 H34C 109.4 . . ? H34B C34 H34C 109.4 . . ? C40 C35 C36 117.8(2) . . ? C40 C35 B2 121.9(2) . . ? C36 C35 B2 120.20(19) . . ? C37 C36 C35 120.1(2) . . ? C37 C36 C41 117.1(2) . . ? C35 C36 C41 122.8(2) . . ? C38 C37 C36 122.2(2) . . ? C38 C37 H37 119.0 . . ? C36 C37 H37 118.8 . . ? C37 C38 C39 118.1(2) . . ? C37 C38 C42 120.5(3) . . ? C39 C38 C42 121.4(2) . . ? C38 C39 C40 121.7(2) . . ? C38 C39 H39 119.4 . . ? C40 C39 H39 118.9 . . ? C39 C40 C35 120.1(2) . . ? C39 C40 C43 118.1(2) . . ? C35 C40 C43 121.8(2) . . ? C36 C41 H41A 110.0 . . ? C36 C41 H41B 109.3 . . ? H41A C41 H41B 109.2 . . ? C36 C41 H41C 109.8 . . ? H41A C41 H41C 109.2 . . ? H41B C41 H41C 109.3 . . ? C38 C42 H42A 109.9 . . ? C38 C42 H42B 110.4 . . ? H42A C42 H42B 108.8 . . ? C38 C42 H42C 110.6 . . ? H42A C42 H42C 108.4 . . ? H42B C42 H42C 108.6 . . ? C40 C43 H43A 110.0 . . ? C40 C43 H43B 109.6 . . ? H43A C43 H43B 109.4 . . ? C40 C43 H43C 108.9 . . ? H43A C43 H43C 109.4 . . ? H43B C43 H43C 109.5 . . ? C45 C44 C49 117.88(19) . . ? C45 C44 B2 121.28(19) . . ? C49 C44 B2 120.80(19) . . ? C46 C45 C44 120.1(2) . . ? C46 C45 C50 117.9(2) . . ? C44 C45 C50 121.9(2) . . ? C47 C46 C45 121.9(2) . . ? C47 C46 H46 119.0 . . ? C45 C46 H46 119.1 . . ? C46 C47 C48 118.0(2) . . ? C46 C47 C51 121.0(2) . . ? C48 C47 C51 121.0(2) . . ? C47 C48 C49 121.7(2) . . ? C47 C48 H48 119.2 . . ? C49 C48 H48 119.1 . . ? C48 C49 C44 120.4(2) . . ? C48 C49 C52 117.9(2) . . ? C44 C49 C52 121.6(2) . . ? C45 C50 H50A 109.8 . . ? C45 C50 H50B 109.6 . . ? H50A C50 H50B 109.4 . . ? C45 C50 H50C 109.1 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.4 . . ? C47 C51 H51A 109.8 . . ? C47 C51 H51B 109.5 . . ? H51A C51 H51B 109.3 . . ? C47 C51 H51C 109.8 . . ? H51A C51 H51C 109.2 . . ? H51B C51 H51C 109.2 . . ? C49 C52 H52A 109.8 . . ? C49 C52 H52B 109.2 . . ? H52A C52 H52B 109.5 . . ? C49 C52 H52C 109.4 . . ? H52A C52 H52C 109.4 . . ? H52B C52 H52C 109.5 . . ? C1 B1 C26 120.05(17) . . ? C1 B1 C17 116.34(17) . . ? C26 B1 C17 123.59(16) . . ? C16 B2 C35 116.37(19) . . ? C16 B2 C44 119.08(19) . . ? C35 B2 C44 124.50(18) . . ? 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 C22 C17 B1 C1 58.2(2) . . . . ? C17 B1 C1 C2 28.6(3) . . . . ? B1 C1 C2 C3 174.91(18) . . . . ? C1 C2 C3 S1 14.8(3) . . . . ? C2 C3 S1 C6 178.80(16) . . . . ? C3 S1 C6 C7 -175.41(16) . . . . ? S1 C6 C7 S2 174.44(11) . . . . ? C6 C7 S2 C10 -178.02(16) . . . . ? C7 S2 C10 C11 177.01(18) . . . . ? S2 C10 C11 S3 -167.89(12) . . . . ? C10 C11 S3 C14 176.34(17) . . . . ? C11 S3 C14 C15 -177.67(17) . . . . ? S3 C14 C15 C16 -6.8(3) . . . . ? C14 C15 C16 B2 -173.4(2) . . . . ? C15 C16 B2 C44 -22.9(3) . . . . ? C16 B2 C44 C45 -58.2(3) . . . . ? C27 C26 B1 C1 39.9(3) . . . . ? C36 C35 B2 C16 -50.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 30.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.787 _refine_diff_density_min -0.565 _refine_diff_density_rms 0.067 #=========================================END