Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_section_title ;Porphyrin complexes containing coordinated BOB groups: synthesis, chemical reactivity and the structure of [BOB(tpClpp)]2+ ; _publ_contact_author_name 'Prof. Penny Brothers' _publ_contact_author_email P.BROTHERS@AUCKLAND.AC.NZ loop_ _publ_author_name W.J.Belcher M.C.Hodgson K.Sumida A.Torvisco K.Ruhlandt-Senge P.D.W.Boyd P.J.Brothers D.C.Ware # Attachment 'squeeze_Jan_2008.cif' data_squeeze _database_code_depnum_ccdc_archive 'CCDC 664478' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68.5 H52 B4 Br8 Cl4 N4 O' _chemical_formula_weight 1765.48 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' N N 0.0061 0.0033 '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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 15.2434(2) _cell_length_b 18.2050(3) _cell_length_c 25.7639(1) _cell_angle_alpha 85.711(1) _cell_angle_beta 82.190(1) _cell_angle_gamma 81.760(1) _cell_volume 6999.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.12 _cell_measurement_theta_max 26.41 _exptl_crystal_description plate _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.550 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3168 _exptl_absorpt_coefficient_mu 4.774 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3284 _exptl_absorpt_correction_T_max 0.4485 _exptl_absorpt_process_details 'R. Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% NO _diffrn_reflns_number 54354 _diffrn_reflns_av_R_equivalents 0.2204 _diffrn_reflns_av_sigmaI/netI 0.1691 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 0.80 _diffrn_reflns_theta_max 24.00 _reflns_number_total 21768 _reflns_number_gt 12576 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1453P)^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 21768 _refine_ls_number_parameters 1423 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1382 _refine_ls_R_factor_gt 0.0943 _refine_ls_wR_factor_ref 0.2826 _refine_ls_wR_factor_gt 0.2421 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 1.0113(7) 0.5803(7) 0.1881(5) 0.037(3) Uani 1 1 d . . . B2 B 0.8983(8) 0.5407(7) 0.2389(4) 0.035(3) Uani 1 1 d . . . O1 O 0.9473(4) 0.5965(4) 0.2265(2) 0.0349(16) Uani 1 1 d . . . N1 N 0.9981(5) 0.5931(4) 0.1337(3) 0.0281(18) Uani 1 1 d . . . N2 N 0.8223(5) 0.5352(4) 0.2161(3) 0.0302(19) Uani 1 1 d . . . N3 N 0.9215(5) 0.4866(4) 0.2807(3) 0.0316(19) Uani 1 1 d . . . N4 N 1.0971(6) 0.5411(5) 0.1971(3) 0.035(2) Uani 1 1 d . . . C1 C 1.0712(7) 0.5973(6) 0.0969(4) 0.035(2) Uani 1 1 d . . . C2 C 1.0370(8) 0.6348(6) 0.0514(4) 0.042(3) Uani 1 1 d . . . H2A H 1.0722 0.6452 0.0190 0.050 Uiso 1 1 calc R . . C3 C 0.9507(6) 0.6526(5) 0.0609(3) 0.029(2) Uani 1 1 d . . . H3A H 0.9136 0.6802 0.0375 0.034 Uiso 1 1 calc R . . C4 C 0.9211(6) 0.6239(6) 0.1122(3) 0.030(2) Uani 1 1 d . . . C5 C 0.8326(7) 0.6186(5) 0.1312(4) 0.031(2) Uani 1 1 d . . . C6 C 0.7903(6) 0.5743(6) 0.1728(4) 0.036(2) Uani 1 1 d . . . C7 C 0.7061(7) 0.5570(6) 0.1732(4) 0.036(3) Uani 1 1 d . . . H7A H 0.6658 0.5777 0.1493 0.044 Uiso 1 1 calc R . . C8 C 0.6885(7) 0.5059(6) 0.2128(4) 0.041(3) Uani 1 1 d . . . H8A H 0.6355 0.4833 0.2206 0.049 Uiso 1 1 calc R . . C9 C 0.7618(6) 0.4931(6) 0.2395(4) 0.032(2) Uani 1 1 d . . . C10 C 0.7773(7) 0.4479(5) 0.2862(4) 0.036(2) Uani 1 1 d . . . C11 C 0.8555(6) 0.4474(6) 0.3066(4) 0.033(2) Uani 1 1 d . . . C12 C 0.8851(7) 0.4187(6) 0.3547(4) 0.036(3) Uani 1 1 d . . . H12A H 0.8531 0.3901 0.3812 0.043 Uiso 1 1 calc R . . C13 C 0.9641(7) 0.4381(6) 0.3567(4) 0.041(3) Uani 1 1 d . . . H13A H 0.9974 0.4278 0.3857 0.049 Uiso 1 1 calc R . . C14 C 0.9920(6) 0.4767(6) 0.3095(3) 0.031(2) Uani 1 1 d . . . C15 C 1.0804(6) 0.4916(5) 0.2925(3) 0.027(2) Uani 1 1 d . . . C16 C 1.1268(7) 0.5071(6) 0.2434(3) 0.032(2) Uani 1 1 d . . . C17 C 1.2173(7) 0.4840(6) 0.2317(4) 0.038(3) Uani 1 1 d . . . H17A H 1.2553 0.4596 0.2559 0.045 Uiso 1 1 calc R . . C18 C 1.2444(7) 0.5019(6) 0.1789(4) 0.039(3) Uani 1 1 d . . . H18A H 1.3027 0.4905 0.1606 0.047 Uiso 1 1 calc R . . C19 C 1.1684(6) 0.5403(6) 0.1578(4) 0.033(2) Uani 1 1 d . . . C20 C 1.1562(6) 0.5719(6) 0.1080(4) 0.032(2) Uani 1 1 d . . . C21 C 0.7657(6) 0.6569(5) 0.0979(4) 0.029(2) Uani 1 1 d . . . C22 C 0.7510(8) 0.6307(7) 0.0517(4) 0.046(3) Uani 1 1 d . . . H22A H 0.7890 0.5883 0.0388 0.055 Uiso 1 1 calc R . . C23 C 0.6846(8) 0.6624(7) 0.0235(4) 0.051(3) Uani 1 1 d . . . H23A H 0.6754 0.6422 -0.0079 0.061 Uiso 1 1 calc R . . C24 C 0.6334(7) 0.7222(6) 0.0415(4) 0.041(3) Uani 1 1 d . . . C25 C 0.6461(8) 0.7548(7) 0.0852(5) 0.050(3) Uani 1 1 d . . . H25A H 0.6103 0.7997 0.0956 0.060 Uiso 1 1 calc R . . C26 C 0.7126(7) 0.7209(7) 0.1141(4) 0.046(3) Uani 1 1 d . . . H26A H 0.7216 0.7420 0.1453 0.056 Uiso 1 1 calc R . . C31 C 0.7064(6) 0.4067(6) 0.3125(4) 0.036(3) Uani 1 1 d . . . C32 C 0.6215(7) 0.4417(6) 0.3254(4) 0.044(3) Uani 1 1 d . . . H32A H 0.6066 0.4936 0.3183 0.053 Uiso 1 1 calc R . . C33 C 0.5595(8) 0.3992(6) 0.3490(4) 0.046(3) Uani 1 1 d . . . H33A H 0.5009 0.4227 0.3602 0.055 Uiso 1 1 calc R . . C34 C 0.5780(7) 0.3250(6) 0.3570(4) 0.038(3) Uani 1 1 d . . . C35 C 0.6637(7) 0.2900(7) 0.3460(5) 0.047(3) Uani 1 1 d . . . H35A H 0.6790 0.2381 0.3531 0.056 Uiso 1 1 calc R . . C36 C 0.7235(8) 0.3323(6) 0.3251(4) 0.050(3) Uani 1 1 d . . . H36A H 0.7836 0.3094 0.3182 0.060 Uiso 1 1 calc R . . C41 C 1.1445(6) 0.4768(6) 0.3335(3) 0.028(2) Uani 1 1 d . . . C42 C 1.1662(7) 0.4078(6) 0.3549(4) 0.043(3) Uani 1 1 d . . . H42A H 1.1395 0.3673 0.3457 0.051 Uiso 1 1 calc R . . C43 C 1.2294(8) 0.3964(7) 0.3912(4) 0.052(3) Uani 1 1 d . . . H43A H 1.2466 0.3482 0.4064 0.062 Uiso 1 1 calc R . . C44 C 1.2647(7) 0.4561(7) 0.4039(4) 0.042(3) Uani 1 1 d . . . C45 C 1.2411(7) 0.5244(6) 0.3819(4) 0.035(2) Uani 1 1 d . . . H45A H 1.2666 0.5655 0.3910 0.041 Uiso 1 1 calc R . . C46 C 1.1801(7) 0.5349(5) 0.3462(4) 0.033(2) Uani 1 1 d . . . H46A H 1.1634 0.5831 0.3309 0.039 Uiso 1 1 calc R . . C51 C 1.2357(6) 0.5743(6) 0.0695(3) 0.032(2) Uani 1 1 d . . . C52 C 1.3046(7) 0.6082(6) 0.0801(4) 0.045(3) Uani 1 1 d . . . H52A H 1.3002 0.6289 0.1133 0.054 Uiso 1 1 calc R . . C53 C 1.3802(7) 0.6141(7) 0.0452(5) 0.053(3) Uani 1 1 d . . . H53A H 1.4277 0.6377 0.0537 0.063 Uiso 1 1 calc R . . C54 C 1.3837(8) 0.5841(7) -0.0022(4) 0.049(3) Uani 1 1 d . . . C55 C 1.3178(9) 0.5518(7) -0.0150(4) 0.053(3) Uani 1 1 d . . . H55A H 1.3234 0.5306 -0.0480 0.063 Uiso 1 1 calc R . . C56 C 1.2405(7) 0.5489(6) 0.0200(4) 0.042(3) Uani 1 1 d . . . H56A H 1.1912 0.5295 0.0099 0.051 Uiso 1 1 calc R . . Cl1 Cl 0.5477(2) 0.7635(2) 0.00735(14) 0.0814(12) Uani 1 1 d . . . Cl2 Cl 0.4951(2) 0.2730(2) 0.38441(14) 0.0695(10) Uani 1 1 d . . . Cl3 Cl 1.3405(3) 0.4434(2) 0.44814(14) 0.0801(12) Uani 1 1 d . . . Cl4 Cl 1.4795(2) 0.5848(2) -0.04542(13) 0.0762(11) Uani 1 1 d . . . B1' B -0.0450(7) 0.9935(6) 0.2544(4) 0.030(3) Uani 1 1 d . . . B2' B 0.0304(8) 0.9918(6) 0.3222(5) 0.032(3) Uani 1 1 d . . . O1' O -0.0330(4) 1.0279(3) 0.2970(2) 0.0265(14) Uani 1 1 d . . . N1' N -0.1015(5) 0.9402(5) 0.2582(3) 0.0292(19) Uani 1 1 d . . . N2' N 0.0143(5) 0.9356(4) 0.3625(3) 0.0282(18) Uani 1 1 d . . . N3' N 0.1215(5) 1.0023(4) 0.3078(3) 0.0237(17) Uani 1 1 d . . . N4' N 0.0018(5) 1.0089(4) 0.2051(3) 0.0262(18) Uani 1 1 d . . . C1' C -0.1325(7) 0.9195(6) 0.2133(4) 0.036(2) Uani 1 1 d . . . C2' C -0.1979(7) 0.8755(6) 0.2304(4) 0.035(2) Uani 1 1 d . . . H2'A H -0.2292 0.8531 0.2077 0.042 Uiso 1 1 calc R . . C3' C -0.2120(7) 0.8681(6) 0.2827(4) 0.033(2) Uani 1 1 d . . . H3'A H -0.2552 0.8414 0.3030 0.040 Uiso 1 1 calc R . . C4' C -0.1505(6) 0.9077(6) 0.3028(4) 0.033(2) Uani 1 1 d . . . C5' C -0.1339(6) 0.8982(5) 0.3550(3) 0.027(2) Uani 1 1 d . . . C6' C -0.0614(6) 0.9062(6) 0.3801(3) 0.029(2) Uani 1 1 d . . . C7' C -0.0494(7) 0.8698(5) 0.4302(4) 0.029(2) Uani 1 1 d . . . H7'A H -0.0921 0.8453 0.4528 0.035 Uiso 1 1 calc R . . C8' C 0.0352(8) 0.8768(6) 0.4395(4) 0.041(3) Uani 1 1 d . . . H8'A H 0.0614 0.8572 0.4699 0.050 Uiso 1 1 calc R . . C9' C 0.0766(8) 0.9169(5) 0.3980(4) 0.034(2) Uani 1 1 d . . . C10' C 0.1548(8) 0.9399(6) 0.3882(4) 0.038(3) Uani 1 1 d . . . C11' C 0.1821(6) 0.9846(6) 0.3439(3) 0.031(2) Uani 1 1 d . . . C12' C 0.2551(7) 1.0205(6) 0.3280(4) 0.037(3) Uani 1 1 d . . . H12B H 0.3068 1.0174 0.3453 0.045 Uiso 1 1 calc R . . C13' C 0.2401(6) 1.0615(5) 0.2828(3) 0.029(2) Uani 1 1 d . . . H13B H 0.2794 1.0931 0.2640 0.034 Uiso 1 1 calc R . . C14' C 0.1581(7) 1.0500(6) 0.2681(3) 0.032(2) Uani 1 1 d . . . C15' C 0.1305(7) 1.0765(5) 0.2188(4) 0.032(2) Uani 1 1 d . . . C16' C 0.0687(6) 1.0524(5) 0.1894(3) 0.027(2) Uani 1 1 d . . . C17' C 0.0737(7) 1.0664(6) 0.1341(4) 0.040(3) Uani 1 1 d . . . H17C H 0.1108 1.0976 0.1129 0.048 Uiso 1 1 calc R . . C18' C 0.0167(8) 1.0275(6) 0.1176(4) 0.044(3) Uani 1 1 d . . . H18C H 0.0079 1.0256 0.0820 0.052 Uiso 1 1 calc R . . C19' C -0.0294(6) 0.9894(6) 0.1603(4) 0.031(2) Uani 1 1 d . . . C20' C -0.0960(8) 0.9444(6) 0.1641(4) 0.039(3) Uani 1 1 d . . . C21' C -0.2083(7) 0.8633(5) 0.3897(4) 0.033(2) Uani 1 1 d . . . C22' C -0.2857(7) 0.9054(7) 0.4053(4) 0.041(3) Uani 1 1 d . . . H22B H -0.2938 0.9572 0.3960 0.049 Uiso 1 1 calc R . . C23' C -0.3532(7) 0.8726(7) 0.4351(5) 0.051(3) Uani 1 1 d . . . H23C H -0.4087 0.9016 0.4460 0.061 Uiso 1 1 calc R . . C24' C -0.3407(7) 0.7992(7) 0.4487(4) 0.042(3) Uani 1 1 d . . . C25' C -0.2612(7) 0.7554(6) 0.4337(4) 0.038(3) Uani 1 1 d . . . H25B H -0.2526 0.7038 0.4434 0.046 Uiso 1 1 calc R . . C26' C -0.1953(7) 0.7893(7) 0.4041(5) 0.053(3) Uani 1 1 d . . . H26B H -0.1394 0.7607 0.3934 0.063 Uiso 1 1 calc R . . C31' C 0.2195(7) 0.9265(6) 0.4295(4) 0.040(3) Uani 1 1 d . . . C32' C 0.1880(7) 0.9490(6) 0.4810(4) 0.040(3) Uani 1 1 d . . . H32B H 0.1281 0.9718 0.4892 0.048 Uiso 1 1 calc R . . C33' C 0.2435(7) 0.9382(7) 0.5186(4) 0.051(3) Uani 1 1 d . . . H33B H 0.2232 0.9522 0.5534 0.061 Uiso 1 1 calc R . . C34' C 0.3300(9) 0.9061(7) 0.5047(5) 0.057(3) Uani 1 1 d . . . C35' C 0.3615(7) 0.8871(6) 0.4542(4) 0.046(3) Uani 1 1 d . . . H35B H 0.4220 0.8664 0.4453 0.055 Uiso 1 1 calc R . . C36' C 0.3050(7) 0.8984(6) 0.4177(4) 0.043(3) Uani 1 1 d . . . H36B H 0.3266 0.8860 0.3827 0.052 Uiso 1 1 calc R . . C41' C 0.1876(6) 1.1310(6) 0.1900(3) 0.030(2) Uani 1 1 d . . . C42' C 0.2659(7) 1.1122(7) 0.1635(4) 0.042(3) Uani 1 1 d . . . H42B H 0.2877 1.0611 0.1597 0.050 Uiso 1 1 calc R . . C43' C 0.3176(8) 1.1654(8) 0.1409(4) 0.054(3) Uani 1 1 d . . . H43B H 0.3746 1.1516 0.1217 0.065 Uiso 1 1 calc R . . C44' C 0.2841(8) 1.2388(7) 0.1470(4) 0.047(3) Uani 1 1 d . . . C45' C 0.2032(7) 1.2582(6) 0.1724(5) 0.044(3) Uani 1 1 d . . . H45B H 0.1803 1.3091 0.1762 0.053 Uiso 1 1 calc R . . C46' C 0.1535(7) 1.2042(6) 0.1928(4) 0.039(3) Uani 1 1 d . . . H46B H 0.0942 1.2176 0.2093 0.047 Uiso 1 1 calc R . . C51' C -0.1258(7) 0.9210(6) 0.1176(4) 0.035(2) Uani 1 1 d . . . C52' C -0.0676(8) 0.8873(6) 0.0798(4) 0.043(3) Uani 1 1 d . . . H52B H -0.0059 0.8791 0.0839 0.051 Uiso 1 1 calc R . . C53' C -0.0945(7) 0.8643(7) 0.0351(4) 0.043(3) Uani 1 1 d . . . H53B H -0.0530 0.8414 0.0083 0.051 Uiso 1 1 calc R . . C54' C -0.1839(9) 0.8762(7) 0.0319(4) 0.050(3) Uani 1 1 d . . . C55' C -0.2457(7) 0.9097(7) 0.0674(4) 0.042(3) Uani 1 1 d . . . H55B H -0.3074 0.9176 0.0632 0.050 Uiso 1 1 calc R . . C56' C -0.2143(7) 0.9320(6) 0.1105(4) 0.037(3) Uani 1 1 d . . . H56B H -0.2560 0.9563 0.1367 0.045 Uiso 1 1 calc R . . Cl1' Cl -0.4239(2) 0.7591(2) 0.48629(13) 0.0674(10) Uani 1 1 d . . . Cl2' Cl 0.4020(3) 0.8985(3) 0.55181(14) 0.0876(13) Uani 1 1 d . . . Cl3' Cl 0.3517(2) 1.3044(2) 0.12139(14) 0.0681(10) Uani 1 1 d . . . Cl4' Cl -0.2221(2) 0.8482(2) -0.02365(11) 0.0661(10) Uani 1 1 d . . . B3 B 0.9801(10) 0.2080(8) 0.4019(5) 0.047(3) Uani 1 1 d . . . Br1 Br 0.85193(9) 0.21852(8) 0.41446(6) 0.0685(4) Uani 1 1 d . . . Br2 Br 1.02484(11) 0.23453(9) 0.32761(5) 0.0700(4) Uani 1 1 d . . . Br3 Br 1.02948(10) 0.10084(7) 0.41933(5) 0.0629(4) Uani 1 1 d . . . Br4 Br 1.02734(10) 0.27112(7) 0.44917(5) 0.0592(4) Uani 1 1 d . . . B4 B 0.9980(9) 0.3697(7) 0.1070(5) 0.041(3) Uani 1 1 d . . . Br5 Br 1.11615(11) 0.39688(9) 0.07642(5) 0.0710(4) Uani 1 1 d . . . Br6 Br 0.90255(11) 0.44297(8) 0.08067(6) 0.0782(5) Uani 1 1 d . . . Br7 Br 0.98907(9) 0.26932(7) 0.08560(5) 0.0567(4) Uani 1 1 d . . . Br8 Br 0.98512(9) 0.37208(7) 0.18455(4) 0.0559(4) Uani 1 1 d . . . B5 B 0.0939(8) 0.7554(7) 0.2409(4) 0.039(3) Uani 1 1 d . . . Br9 Br 0.02150(8) 0.71904(8) 0.30685(5) 0.0568(4) Uani 1 1 d . . . Br10 Br 0.02502(9) 0.75564(7) 0.18057(5) 0.0537(3) Uani 1 1 d . . . Br11 Br 0.12514(9) 0.85247(7) 0.24933(5) 0.0541(3) Uani 1 1 d . . . Br12 Br 0.20613(8) 0.68318(6) 0.22819(5) 0.0480(3) Uani 1 1 d . . . B6 B 0.4868(11) 0.9064(12) 0.2473(6) 0.076(5) Uani 1 1 d . . . Br13 Br 0.47252(12) 1.01577(10) 0.22513(9) 0.0997(6) Uani 1 1 d . . . Br14 Br 0.52359(12) 0.89358(12) 0.31905(6) 0.0936(6) Uani 1 1 d . . . Br15 Br 0.37137(9) 0.87001(9) 0.24844(6) 0.0736(4) Uani 1 1 d . . . Br16 Br 0.57933(10) 0.85395(10) 0.19802(6) 0.0771(5) Uani 1 1 d . . . C1S C 0.3309(11) 0.1848(9) 0.3444(6) 0.071(4) Uani 1 1 d . . . C2S C 0.4066(9) 0.1356(8) 0.3416(6) 0.067(4) Uani 1 1 d . . . H2SA H 0.4486 0.1347 0.3107 0.081 Uiso 1 1 calc R . . C3S C 0.4218(11) 0.0872(8) 0.3836(7) 0.074(4) Uani 1 1 d . . . H3SA H 0.4754 0.0531 0.3821 0.089 Uiso 1 1 calc R . . C4S C 0.3633(15) 0.0871(11) 0.4260(7) 0.098(6) Uani 1 1 d . . . H4SA H 0.3766 0.0539 0.4549 0.118 Uiso 1 1 calc R . . C5S C 0.2825(14) 0.1340(11) 0.4300(7) 0.098(6) Uani 1 1 d . . . H5SA H 0.2403 0.1329 0.4607 0.117 Uiso 1 1 calc R . . C6S C 0.2660(13) 0.1833(9) 0.3864(7) 0.088(5) Uani 1 1 d . . . H6SA H 0.2107 0.2148 0.3863 0.105 Uiso 1 1 calc R . . C7S C 0.3132(14) 0.2399(9) 0.2975(6) 0.098(6) Uani 1 1 d . . . H7SA H 0.2572 0.2728 0.3064 0.147 Uiso 1 1 calc R . . H7SB H 0.3084 0.2123 0.2669 0.147 Uiso 1 1 calc R . . H7SC H 0.3626 0.2695 0.2892 0.147 Uiso 1 1 calc R . . C8S C 0.3191(12) 0.6849(9) 0.4577(5) 0.076(4) Uani 1 1 d . . . C9S C 0.2280(10) 0.6939(8) 0.4540(6) 0.074(4) Uani 1 1 d . . . H9SA H 0.1871 0.6843 0.4841 0.089 Uiso 1 1 calc R . . C10S C 0.1959(13) 0.7169(9) 0.4064(7) 0.088(5) Uani 1 1 d . . . H10A H 0.1340 0.7213 0.4031 0.105 Uiso 1 1 calc R . . C11S C 0.2538(17) 0.7318(9) 0.3669(7) 0.098(7) Uani 1 1 d . . . H11A H 0.2322 0.7485 0.3346 0.117 Uiso 1 1 calc R . . C12S C 0.3455(15) 0.7251(9) 0.3684(6) 0.085(5) Uani 1 1 d . . . H12C H 0.3854 0.7389 0.3388 0.102 Uiso 1 1 calc R . . C13S C 0.3760(11) 0.6965(9) 0.4163(6) 0.080(5) Uani 1 1 d . . . H13C H 0.4384 0.6856 0.4184 0.096 Uiso 1 1 calc R . . C14S C 0.3435(15) 0.6592(13) 0.5122(7) 0.141(9) Uani 1 1 d . . . H14A H 0.4085 0.6535 0.5115 0.211 Uiso 1 1 calc R . . H14B H 0.3221 0.6114 0.5228 0.211 Uiso 1 1 calc R . . H14C H 0.3155 0.6961 0.5373 0.211 Uiso 1 1 calc R . . C22S C 0.2196(12) 0.8781(12) 0.0700(6) 0.087(5) Uani 1 1 d . . . C23S C 0.2022(17) 0.8115(12) 0.0648(12) 0.129(10) Uani 1 1 d . . . H23D H 0.2132 0.7763 0.0931 0.155 Uiso 1 1 calc R . . C24S C 0.172(2) 0.7870(17) 0.0254(15) 0.175(15) Uani 1 1 d . . . H24A H 0.1661 0.7363 0.0219 0.210 Uiso 1 1 calc R . . C25S C 0.1453(19) 0.851(2) -0.0145(9) 0.156(12) Uani 1 1 d . . . H25C H 0.1181 0.8410 -0.0440 0.187 Uiso 1 1 calc R . . C26S C 0.1610(12) 0.9191(12) -0.0078(7) 0.096(6) Uani 1 1 d . . . H26C H 0.1455 0.9587 -0.0324 0.115 Uiso 1 1 calc R . . C27S C 0.1996(12) 0.9318(8) 0.0351(6) 0.084(5) Uani 1 1 d . . . H27A H 0.2122 0.9804 0.0395 0.101 Uiso 1 1 calc R . . C28S C 0.2634(15) 0.8949(15) 0.1161(9) 0.152(9) Uani 1 1 d . . . H28A H 0.2768 0.8491 0.1376 0.228 Uiso 1 1 calc R . . H28B H 0.2228 0.9312 0.1372 0.228 Uiso 1 1 calc R . . H28C H 0.3189 0.9154 0.1033 0.228 Uiso 1 1 calc R . . C43S C 0.4574(10) 0.5947(11) 0.1929(8) 0.085(5) Uani 1 1 d . . . C44S C 0.4828(8) 0.5387(9) 0.1631(6) 0.066(4) Uani 1 1 d . . . H44A H 0.5041 0.5466 0.1270 0.079 Uiso 1 1 calc R . . C45S C 0.4781(9) 0.4675(8) 0.1853(7) 0.066(4) Uani 1 1 d . . . H45C H 0.4955 0.4266 0.1636 0.079 Uiso 1 1 calc R . . C46S C 0.4503(11) 0.4546(11) 0.2353(8) 0.092(6) Uani 1 1 d . . . H46C H 0.4484 0.4055 0.2504 0.111 Uiso 1 1 calc R . . C47S C 0.4240(11) 0.5166(14) 0.2650(6) 0.103(7) Uani 1 1 d . . . H47A H 0.4045 0.5097 0.3014 0.123 Uiso 1 1 calc R . . C48S C 0.4254(10) 0.5868(11) 0.2431(7) 0.086(5) Uani 1 1 d . . . H48A H 0.4040 0.6289 0.2632 0.103 Uiso 1 1 calc R . . C49S C 0.4642(11) 0.6757(11) 0.1711(8) 0.108(6) Uani 1 1 d . . . H49A H 0.4863 0.6759 0.1336 0.162 Uiso 1 1 calc R . . H49B H 0.5055 0.6972 0.1897 0.162 Uiso 1 1 calc R . . H49C H 0.4050 0.7053 0.1763 0.162 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.009(6) 0.050(8) 0.051(8) 0.018(6) -0.010(5) -0.004(5) B2 0.037(7) 0.045(7) 0.019(6) 0.005(5) 0.008(5) -0.006(6) O1 0.031(4) 0.047(4) 0.022(3) 0.005(3) 0.005(3) -0.003(3) N1 0.022(4) 0.041(5) 0.023(4) 0.002(3) -0.005(3) -0.008(3) N2 0.016(4) 0.046(5) 0.024(4) 0.010(4) 0.003(3) -0.002(4) N3 0.030(5) 0.042(5) 0.020(4) 0.009(4) -0.003(3) -0.002(4) N4 0.033(5) 0.050(5) 0.021(4) 0.011(4) -0.005(4) -0.002(4) C1 0.038(6) 0.036(6) 0.029(5) 0.006(4) -0.006(5) -0.002(5) C2 0.055(8) 0.046(7) 0.023(5) 0.014(5) -0.017(5) -0.002(5) C3 0.023(6) 0.044(6) 0.021(5) 0.005(4) -0.011(4) -0.008(4) C4 0.025(6) 0.047(6) 0.013(4) 0.008(4) -0.001(4) 0.001(4) C5 0.030(6) 0.031(6) 0.033(5) -0.001(4) -0.010(4) -0.004(4) C6 0.020(5) 0.056(7) 0.029(5) 0.016(5) -0.009(4) -0.003(5) C7 0.026(6) 0.049(7) 0.032(6) 0.017(5) -0.011(4) -0.004(5) C8 0.024(6) 0.050(7) 0.043(6) 0.006(5) 0.001(5) 0.004(5) C9 0.025(6) 0.041(6) 0.025(5) -0.001(4) 0.001(4) 0.004(4) C10 0.042(7) 0.034(6) 0.029(5) 0.004(4) 0.000(5) -0.006(5) C11 0.019(5) 0.047(6) 0.024(5) 0.016(4) -0.002(4) 0.012(4) C12 0.023(6) 0.048(7) 0.035(6) 0.018(5) -0.005(4) -0.005(5) C13 0.021(6) 0.060(7) 0.036(6) 0.015(5) -0.003(4) -0.001(5) C14 0.028(6) 0.051(6) 0.015(5) 0.000(4) -0.009(4) -0.006(5) C15 0.025(5) 0.034(6) 0.021(5) 0.004(4) -0.001(4) -0.001(4) C16 0.033(6) 0.046(6) 0.016(5) 0.006(4) -0.005(4) -0.002(5) C17 0.031(6) 0.058(7) 0.025(5) 0.013(5) -0.009(4) -0.010(5) C18 0.023(6) 0.054(7) 0.033(6) 0.024(5) 0.002(4) 0.003(5) C19 0.020(5) 0.059(7) 0.020(5) 0.007(4) -0.003(4) -0.011(5) C20 0.027(6) 0.043(6) 0.022(5) -0.003(4) -0.006(4) 0.009(4) C21 0.024(5) 0.032(5) 0.031(5) 0.008(4) -0.018(4) 0.008(4) C22 0.045(7) 0.060(8) 0.030(6) 0.004(5) -0.017(5) 0.009(6) C23 0.044(7) 0.077(9) 0.031(6) 0.000(6) -0.011(5) -0.004(7) C24 0.026(6) 0.051(7) 0.042(6) 0.021(5) -0.012(5) 0.002(5) C25 0.039(7) 0.064(8) 0.047(7) 0.009(6) -0.025(5) 0.003(6) C26 0.034(6) 0.062(8) 0.041(6) 0.004(6) -0.001(5) -0.006(6) C31 0.022(6) 0.058(7) 0.026(5) 0.012(5) -0.001(4) -0.014(5) C32 0.028(6) 0.056(7) 0.039(6) 0.024(5) 0.007(5) 0.004(5) C33 0.040(7) 0.051(7) 0.041(6) 0.009(5) 0.002(5) 0.001(5) C34 0.029(6) 0.052(7) 0.035(6) 0.018(5) -0.007(4) -0.017(5) C35 0.024(6) 0.051(7) 0.063(8) 0.023(6) -0.007(5) -0.005(5) C36 0.043(7) 0.048(7) 0.050(7) 0.010(6) 0.009(5) 0.003(6) C41 0.026(5) 0.050(7) 0.012(4) 0.007(4) -0.011(4) -0.013(5) C42 0.042(7) 0.046(7) 0.045(7) 0.000(5) -0.019(5) -0.010(5) C43 0.050(8) 0.070(9) 0.033(6) 0.015(6) -0.019(5) 0.006(6) C44 0.026(6) 0.071(8) 0.030(6) 0.010(5) -0.021(5) -0.002(5) C45 0.032(6) 0.048(7) 0.030(5) -0.017(5) -0.012(4) -0.009(5) C46 0.046(6) 0.029(6) 0.026(5) -0.002(4) -0.011(5) -0.010(5) C51 0.025(5) 0.057(7) 0.015(5) 0.018(4) -0.014(4) -0.005(5) C52 0.035(7) 0.062(8) 0.042(6) -0.011(6) -0.011(5) -0.007(5) C53 0.022(6) 0.081(9) 0.054(8) 0.019(7) -0.002(5) -0.015(6) C54 0.042(7) 0.069(8) 0.031(6) -0.002(6) 0.020(5) -0.017(6) C55 0.066(9) 0.059(8) 0.029(6) -0.005(5) 0.017(6) -0.017(7) C56 0.028(6) 0.066(8) 0.033(6) 0.001(5) -0.002(5) -0.013(5) Cl1 0.054(2) 0.116(3) 0.068(2) 0.015(2) -0.0340(18) 0.021(2) Cl2 0.059(2) 0.086(3) 0.064(2) 0.0224(18) -0.0010(16) -0.0346(19) Cl3 0.075(2) 0.115(3) 0.052(2) -0.0041(19) -0.0468(19) 0.016(2) Cl4 0.047(2) 0.119(3) 0.053(2) 0.0057(19) 0.0204(16) -0.0110(19) B1' 0.017(6) 0.038(7) 0.029(6) 0.010(5) -0.004(5) 0.004(5) B2' 0.038(7) 0.022(6) 0.039(7) -0.014(5) -0.020(6) 0.012(5) O1' 0.030(4) 0.031(4) 0.020(3) 0.001(3) -0.010(3) -0.005(3) N1' 0.024(4) 0.045(5) 0.020(4) 0.001(4) -0.012(3) -0.002(4) N2' 0.035(5) 0.039(5) 0.014(4) 0.003(3) -0.007(3) -0.014(4) N3' 0.032(5) 0.022(4) 0.014(4) 0.003(3) -0.001(3) 0.001(3) N4' 0.024(4) 0.031(4) 0.023(4) -0.001(3) -0.006(3) -0.002(3) C1' 0.041(6) 0.045(6) 0.023(5) 0.004(5) -0.010(5) -0.004(5) C2' 0.036(6) 0.043(6) 0.026(5) -0.002(4) 0.005(4) -0.008(5) C3' 0.027(6) 0.040(6) 0.031(6) -0.001(4) 0.010(4) -0.014(5) C4' 0.016(5) 0.051(7) 0.030(5) 0.010(5) 0.001(4) -0.005(4) C5' 0.028(5) 0.038(6) 0.015(4) 0.006(4) -0.001(4) -0.006(4) C6' 0.026(5) 0.047(6) 0.014(4) -0.005(4) -0.004(4) -0.004(4) C7' 0.034(6) 0.029(5) 0.023(5) 0.010(4) -0.001(4) -0.004(4) C8' 0.056(8) 0.046(7) 0.022(5) -0.004(5) -0.005(5) -0.004(5) C9' 0.051(7) 0.031(6) 0.020(5) -0.005(4) -0.008(5) -0.006(5) C10' 0.054(8) 0.042(6) 0.020(5) 0.007(4) -0.019(5) -0.004(5) C11' 0.029(6) 0.053(7) 0.013(4) -0.001(4) -0.003(4) -0.008(5) C12' 0.035(6) 0.056(7) 0.015(5) 0.009(4) 0.002(4) 0.002(5) C13' 0.027(5) 0.041(6) 0.021(5) -0.002(4) -0.013(4) -0.007(4) C14' 0.034(6) 0.044(6) 0.016(5) 0.003(4) 0.000(4) -0.002(5) C15' 0.032(6) 0.033(6) 0.029(5) 0.010(4) -0.010(4) 0.004(4) C16' 0.027(5) 0.037(6) 0.018(5) 0.001(4) -0.006(4) -0.008(4) C17' 0.036(6) 0.068(8) 0.017(5) 0.002(5) -0.001(4) -0.016(6) C18' 0.049(7) 0.059(8) 0.022(5) 0.007(5) -0.006(5) -0.008(6) C19' 0.025(6) 0.046(6) 0.022(5) 0.002(4) -0.008(4) 0.005(5) C20' 0.051(7) 0.036(6) 0.025(5) 0.006(4) -0.007(5) 0.009(5) C21' 0.047(7) 0.033(6) 0.023(5) 0.002(4) -0.021(5) -0.007(5) C22' 0.020(6) 0.060(7) 0.038(6) 0.012(5) -0.006(5) 0.007(5) C23' 0.026(6) 0.066(9) 0.055(7) -0.001(6) -0.008(5) 0.010(6) C24' 0.035(6) 0.070(8) 0.023(5) -0.005(5) -0.013(5) -0.010(6) C25' 0.033(6) 0.050(7) 0.027(5) 0.006(5) 0.006(4) -0.007(5) C26' 0.023(6) 0.070(9) 0.061(8) 0.008(6) 0.000(5) 0.001(5) C31' 0.040(7) 0.045(7) 0.040(6) 0.013(5) -0.021(5) -0.019(5) C32' 0.039(6) 0.062(7) 0.018(5) 0.001(5) -0.008(4) 0.000(5) C33' 0.037(7) 0.084(9) 0.026(6) 0.004(6) -0.014(5) 0.017(6) C34' 0.066(9) 0.065(8) 0.045(7) 0.004(6) -0.040(7) -0.003(7) C35' 0.027(6) 0.065(8) 0.045(7) 0.007(6) -0.021(5) 0.010(5) C36' 0.031(7) 0.057(7) 0.038(6) -0.006(5) -0.009(5) 0.010(5) C41' 0.025(6) 0.052(7) 0.014(4) 0.008(4) -0.007(4) -0.008(5) C42' 0.044(7) 0.053(7) 0.033(6) 0.000(5) -0.007(5) -0.020(6) C43' 0.038(7) 0.084(10) 0.035(6) 0.018(6) -0.001(5) -0.009(7) C44' 0.041(7) 0.070(9) 0.030(6) 0.016(6) -0.018(5) -0.010(6) C45' 0.041(7) 0.034(6) 0.057(7) 0.023(5) -0.012(6) -0.006(5) C46' 0.026(6) 0.059(7) 0.026(5) 0.019(5) 0.008(4) -0.005(5) C51' 0.045(7) 0.041(6) 0.022(5) 0.004(4) -0.007(5) -0.019(5) C52' 0.042(7) 0.048(7) 0.032(6) 0.005(5) -0.011(5) 0.019(5) C53' 0.034(7) 0.071(8) 0.024(5) 0.001(5) -0.002(5) -0.012(6) C54' 0.071(9) 0.063(8) 0.023(6) 0.016(5) -0.026(6) -0.028(7) C55' 0.036(6) 0.075(8) 0.013(5) 0.008(5) -0.009(4) -0.005(6) C56' 0.030(6) 0.046(7) 0.030(6) 0.006(5) 0.012(4) -0.005(5) Cl1' 0.050(2) 0.085(2) 0.060(2) 0.0180(17) 0.0211(15) -0.0214(17) Cl2' 0.073(3) 0.136(4) 0.054(2) -0.009(2) -0.0490(19) 0.024(2) Cl3' 0.054(2) 0.085(3) 0.065(2) 0.0294(18) -0.0049(16) -0.0318(18) Cl4' 0.078(2) 0.104(3) 0.0278(15) -0.0026(15) -0.0146(15) -0.043(2) B3 0.058(9) 0.061(9) 0.025(6) -0.003(6) -0.020(6) -0.002(7) Br1 0.0540(9) 0.0770(10) 0.0664(9) 0.0119(7) -0.0007(7) 0.0041(7) Br2 0.0938(11) 0.0869(10) 0.0244(6) 0.0100(6) 0.0029(6) -0.0119(8) Br3 0.0918(11) 0.0473(7) 0.0410(7) -0.0016(5) -0.0072(6) 0.0186(7) Br4 0.0843(10) 0.0575(8) 0.0348(6) 0.0004(5) -0.0058(6) -0.0090(7) B4 0.059(9) 0.039(7) 0.029(6) 0.016(5) -0.021(6) -0.021(6) Br5 0.0757(10) 0.0838(10) 0.0538(8) 0.0051(7) 0.0006(7) -0.0250(8) Br6 0.0954(12) 0.0707(10) 0.0676(9) -0.0142(7) -0.0445(8) 0.0290(8) Br7 0.0755(9) 0.0484(7) 0.0466(7) -0.0078(6) -0.0105(6) -0.0046(6) Br8 0.0617(8) 0.0706(9) 0.0311(6) -0.0073(6) -0.0086(5) 0.0103(6) B5 0.031(7) 0.062(9) 0.024(6) -0.008(6) -0.010(5) 0.002(6) Br9 0.0419(7) 0.0879(10) 0.0369(6) 0.0043(6) 0.0011(5) -0.0060(6) Br10 0.0681(9) 0.0551(8) 0.0422(7) 0.0047(5) -0.0263(6) -0.0084(6) Br11 0.0524(8) 0.0450(7) 0.0668(8) -0.0114(6) -0.0183(6) 0.0013(6) Br12 0.0437(7) 0.0468(7) 0.0486(7) -0.0038(5) 0.0001(5) 0.0054(5) B6 0.051(10) 0.133(16) 0.037(8) -0.017(9) 0.007(7) 0.005(10) Br13 0.0647(11) 0.0828(12) 0.1458(18) -0.0063(11) 0.0035(11) -0.0060(9) Br14 0.0724(11) 0.1562(17) 0.0560(9) -0.0271(10) -0.0095(8) -0.0165(11) Br15 0.0435(8) 0.0992(12) 0.0806(10) -0.0155(8) -0.0051(7) -0.0153(7) Br16 0.0506(9) 0.1120(13) 0.0636(9) -0.0237(8) 0.0008(7) 0.0089(8) C1S 0.077(11) 0.082(11) 0.068(10) -0.003(8) -0.024(8) -0.049(9) C2S 0.044(8) 0.073(10) 0.091(11) -0.008(8) -0.018(7) -0.015(7) C3S 0.075(11) 0.057(9) 0.099(13) -0.010(9) -0.028(10) -0.016(8) C4S 0.115(17) 0.124(16) 0.073(12) -0.025(11) -0.056(12) -0.022(13) C5S 0.110(16) 0.119(16) 0.067(11) -0.034(11) 0.009(10) -0.031(13) C6S 0.106(14) 0.076(11) 0.082(12) -0.039(10) -0.014(11) 0.005(9) C7S 0.142(17) 0.084(12) 0.069(10) 0.006(9) -0.041(11) 0.005(11) C8S 0.093(13) 0.102(12) 0.036(8) -0.010(7) -0.032(8) 0.002(9) C9S 0.068(11) 0.070(10) 0.082(11) -0.022(8) -0.003(8) 0.000(8) C10S 0.088(13) 0.092(13) 0.082(12) -0.016(10) -0.035(11) 0.021(10) C11S 0.16(2) 0.069(11) 0.070(12) -0.014(9) -0.071(14) 0.014(12) C12S 0.138(17) 0.078(11) 0.041(8) -0.011(7) -0.015(9) -0.015(11) C13S 0.073(11) 0.092(12) 0.069(10) -0.024(9) -0.018(9) 0.030(9) C14S 0.16(2) 0.19(2) 0.058(11) -0.004(13) -0.043(12) 0.049(17) C22S 0.096(13) 0.115(15) 0.044(8) -0.005(9) 0.000(8) -0.008(11) C23S 0.13(2) 0.052(13) 0.19(3) 0.029(14) 0.029(18) -0.019(12) C24S 0.17(3) 0.14(3) 0.22(4) -0.03(2) 0.06(3) -0.10(2) C25S 0.18(3) 0.23(3) 0.088(16) -0.051(19) -0.002(16) -0.12(3) C26S 0.078(12) 0.138(18) 0.074(12) 0.041(11) -0.026(9) -0.031(11) C27S 0.130(15) 0.048(9) 0.069(10) 0.000(8) -0.005(10) 0.001(9) C28S 0.107(18) 0.22(3) 0.124(19) -0.032(18) -0.008(15) 0.011(17) C43S 0.038(9) 0.120(15) 0.101(14) -0.002(12) -0.028(9) -0.005(9) C44S 0.027(7) 0.096(12) 0.073(9) -0.014(9) -0.018(6) 0.010(7) C45S 0.041(8) 0.070(10) 0.090(12) -0.011(8) -0.034(8) 0.010(7) C46S 0.053(10) 0.123(16) 0.100(14) 0.039(13) -0.027(10) -0.012(10) C47S 0.071(12) 0.17(2) 0.049(9) 0.002(12) -0.011(8) 0.029(13) C48S 0.060(10) 0.121(15) 0.071(11) -0.026(10) -0.029(9) 0.031(10) C49S 0.052(11) 0.123(16) 0.142(18) -0.010(13) 0.020(10) -0.025(10) _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 B1 O1 1.312(14) . ? B1 N4 1.437(13) . ? B1 N1 1.439(14) . ? B2 O1 1.340(14) . ? B2 N2 1.386(15) . ? B2 N3 1.449(13) . ? N1 C1 1.369(12) . ? N1 C4 1.392(12) . ? N2 C9 1.336(12) . ? N2 C6 1.387(11) . ? N3 C14 1.372(12) . ? N3 C11 1.386(12) . ? N4 C19 1.381(12) . ? N4 C16 1.403(11) . ? C1 C20 1.372(14) . ? C1 C2 1.435(13) . ? C2 C3 1.304(15) . ? C2 H2A 0.9500 . ? C3 C4 1.424(12) . ? C3 H3A 0.9500 . ? C4 C5 1.385(13) . ? C5 C6 1.431(13) . ? C5 C21 1.485(12) . ? C6 C7 1.363(14) . ? C7 C8 1.353(14) . ? C7 H7A 0.9500 . ? C8 C9 1.375(14) . ? C8 H8A 0.9500 . ? C9 C10 1.431(13) . ? C10 C11 1.366(14) . ? C10 C31 1.465(13) . ? C11 C12 1.416(13) . ? C12 C13 1.313(14) . ? C12 H12A 0.9500 . ? C13 C14 1.403(13) . ? C13 H13A 0.9500 . ? C14 C15 1.416(13) . ? C15 C16 1.394(13) . ? C15 C41 1.518(12) . ? C16 C17 1.383(14) . ? C17 C18 1.395(13) . ? C17 H17A 0.9500 . ? C18 C19 1.417(13) . ? C18 H18A 0.9500 . ? C19 C20 1.392(13) . ? C20 C51 1.461(13) . ? C21 C22 1.372(14) . ? C21 C26 1.378(15) . ? C22 C23 1.362(15) . ? C22 H22A 0.9500 . ? C23 C24 1.319(16) . ? C23 H23A 0.9500 . ? C24 C25 1.361(16) . ? C24 Cl1 1.726(10) . ? C25 C26 1.387(15) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C31 C36 1.365(15) . ? C31 C32 1.367(14) . ? C32 C33 1.358(15) . ? C32 H32A 0.9500 . ? C33 C34 1.347(15) . ? C33 H33A 0.9500 . ? C34 C35 1.372(15) . ? C34 Cl2 1.729(10) . ? C35 C36 1.311(15) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C41 C46 1.336(13) . ? C41 C42 1.349(14) . ? C42 C43 1.416(15) . ? C42 H42A 0.9500 . ? C43 C44 1.359(17) . ? C43 H43A 0.9500 . ? C44 C45 1.348(15) . ? C44 Cl3 1.712(9) . ? C45 C46 1.378(13) . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? C51 C52 1.360(14) . ? C51 C56 1.376(14) . ? C52 C53 1.375(15) . ? C52 H52A 0.9500 . ? C53 C54 1.367(17) . ? C53 H53A 0.9500 . ? C54 C55 1.322(17) . ? C54 Cl4 1.713(10) . ? C55 C56 1.388(15) . ? C55 H55A 0.9500 . ? C56 H56A 0.9500 . ? B1' O1' 1.351(13) . ? B1' N1' 1.377(14) . ? B1' N4' 1.398(13) . ? B2' O1' 1.307(12) . ? B2' N3' 1.423(14) . ? B2' N2' 1.425(14) . ? N1' C1' 1.403(12) . ? N1' C4' 1.422(12) . ? N2' C6' 1.350(12) . ? N2' C9' 1.398(12) . ? N3' C11' 1.388(12) . ? N3' C14' 1.402(12) . ? N4' C16' 1.380(12) . ? N4' C19' 1.394(12) . ? C1' C2' 1.373(14) . ? C1' C20' 1.385(14) . ? C2' C3' 1.336(14) . ? C2' H2'A 0.9500 . ? C3' C4' 1.431(14) . ? C3' H3'A 0.9500 . ? C4' C5' 1.394(13) . ? C5' C6' 1.385(13) . ? C5' C21' 1.530(13) . ? C6' C7' 1.429(12) . ? C7' C8' 1.368(15) . ? C7' H7'A 0.9500 . ? C8' C9' 1.380(14) . ? C8' H8'A 0.9500 . ? C9' C10' 1.307(15) . ? C10' C11' 1.402(14) . ? C10' C31' 1.531(13) . ? C11' C12' 1.369(14) . ? C12' C13' 1.364(13) . ? C12' H12B 0.9500 . ? C13' C14' 1.401(13) . ? C13' H13B 0.9500 . ? C14' C15' 1.419(13) . ? C15' C16' 1.419(13) . ? C15' C41' 1.502(13) . ? C16' C17' 1.423(13) . ? C17' C18' 1.325(15) . ? C17' H17C 0.9500 . ? C18' C19' 1.414(14) . ? C18' H18C 0.9500 . ? C19' C20' 1.382(15) . ? C20' C51' 1.450(14) . ? C21' C22' 1.341(14) . ? C21' C26' 1.364(15) . ? C22' C23' 1.379(15) . ? C22' H22B 0.9500 . ? C23' C24' 1.349(16) . ? C23' H23C 0.9500 . ? C24' C25' 1.376(15) . ? C24' Cl1' 1.704(11) . ? C25' C26' 1.368(15) . ? C25' H25B 0.9500 . ? C26' H26B 0.9500 . ? C31' C36' 1.334(15) . ? C31' C32' 1.418(15) . ? C32' C33' 1.354(14) . ? C32' H32B 0.9500 . ? C33' C34' 1.375(17) . ? C33' H33B 0.9500 . ? C34' C35' 1.374(17) . ? C34' Cl2' 1.730(11) . ? C35' C36' 1.345(14) . ? C35' H35B 0.9500 . ? C36' H36B 0.9500 . ? C41' C42' 1.306(15) . ? C41' C46' 1.363(14) . ? C42' C43' 1.381(16) . ? C42' H42B 0.9500 . ? C43' C44' 1.373(17) . ? C43' H43B 0.9500 . ? C44' C45' 1.329(16) . ? C44' Cl3' 1.724(12) . ? C45' C46' 1.358(14) . ? C45' H45B 0.9500 . ? C46' H46B 0.9500 . ? C51' C52' 1.345(15) . ? C51' C56' 1.370(14) . ? C52' C53' 1.386(15) . ? C52' H52B 0.9500 . ? C53' C54' 1.361(16) . ? C53' H53B 0.9500 . ? C54' C55' 1.335(17) . ? C54' Cl4' 1.752(11) . ? C55' C56' 1.378(15) . ? C55' H55B 0.9500 . ? C56' H56B 0.9500 . ? B3 Br1 1.920(15) . ? B3 Br2 1.990(13) . ? B3 Br4 2.003(13) . ? B3 Br3 2.028(14) . ? B4 Br7 1.976(13) . ? B4 Br5 1.980(13) . ? B4 Br8 1.984(12) . ? B4 Br6 1.984(13) . ? B5 Br11 1.930(14) . ? B5 Br10 1.990(11) . ? B5 Br12 2.008(12) . ? B5 Br9 2.018(12) . ? B6 Br16 1.956(15) . ? B6 Br15 1.963(18) . ? B6 Br14 1.991(16) . ? B6 Br13 2.02(2) . ? C1S C2S 1.35(2) . ? C1S C6S 1.36(2) . ? C1S C7S 1.54(2) . ? C2S C3S 1.37(2) . ? C2S H2SA 0.9500 . ? C3S C4S 1.31(2) . ? C3S H3SA 0.9500 . ? C4S C5S 1.39(3) . ? C4S H4SA 0.9500 . ? C5S C6S 1.41(2) . ? C5S H5SA 0.9500 . ? C6S H6SA 0.9500 . ? C7S H7SA 0.9800 . ? C7S H7SB 0.9800 . ? C7S H7SC 0.9800 . ? C8S C13S 1.30(2) . ? C8S C9S 1.39(2) . ? C8S C14S 1.52(2) . ? C9S C10S 1.39(2) . ? C9S H9SA 0.9500 . ? C10S C11S 1.29(3) . ? C10S H10A 0.9500 . ? C11S C12S 1.39(3) . ? C11S H11A 0.9500 . ? C12S C13S 1.42(2) . ? C12S H12C 0.9500 . ? C13S H13C 0.9500 . ? C14S H14A 0.9800 . ? C14S H14B 0.9800 . ? C14S H14C 0.9800 . ? C22S C23S 1.30(3) . ? C22S C27S 1.31(2) . ? C22S C28S 1.51(3) . ? C23S C24S 1.31(4) . ? C23S H23D 0.9500 . ? C24S C25S 1.54(4) . ? C24S H24A 0.9500 . ? C25S C26S 1.33(3) . ? C25S H25C 0.9500 . ? C26S C27S 1.37(2) . ? C26S H26C 0.9500 . ? C27S H27A 0.9500 . ? C28S H28A 0.9800 . ? C28S H28B 0.9800 . ? C28S H28C 0.9800 . ? C43S C44S 1.30(2) . ? C43S C48S 1.32(2) . ? C43S C49S 1.55(2) . ? C44S C45S 1.38(2) . ? C44S H44A 0.9500 . ? C45S C46S 1.32(2) . ? C45S H45C 0.9500 . ? C46S C47S 1.39(3) . ? C46S H46C 0.9500 . ? C47S C48S 1.36(3) . ? C47S H47A 0.9500 . ? C48S H48A 0.9500 . ? C49S H49A 0.9800 . ? C49S H49B 0.9800 . ? C49S H49C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 B1 N4 122.2(10) . . ? O1 B1 N1 122.7(9) . . ? N4 B1 N1 114.8(10) . . ? O1 B2 N2 123.0(9) . . ? O1 B2 N3 118.7(10) . . ? N2 B2 N3 118.1(10) . . ? B1 O1 B2 111.5(9) . . ? C1 N1 C4 109.6(7) . . ? C1 N1 B1 118.6(8) . . ? C4 N1 B1 128.8(8) . . ? C9 N2 B2 120.5(8) . . ? C9 N2 C6 109.3(8) . . ? B2 N2 C6 129.8(8) . . ? C14 N3 C11 108.2(7) . . ? C14 N3 B2 131.7(9) . . ? C11 N3 B2 118.2(8) . . ? C19 N4 C16 109.4(8) . . ? C19 N4 B1 120.0(8) . . ? C16 N4 B1 130.2(9) . . ? N1 C1 C20 121.8(8) . . ? N1 C1 C2 105.4(9) . . ? C20 C1 C2 132.7(10) . . ? C3 C2 C1 110.0(10) . . ? C3 C2 H2A 125.0 . . ? C1 C2 H2A 125.0 . . ? C2 C3 C4 108.8(9) . . ? C2 C3 H3A 125.6 . . ? C4 C3 H3A 125.6 . . ? C5 C4 N1 129.0(8) . . ? C5 C4 C3 124.3(9) . . ? N1 C4 C3 105.9(8) . . ? C4 C5 C6 133.4(9) . . ? C4 C5 C21 115.6(8) . . ? C6 C5 C21 110.2(8) . . ? C7 C6 N2 105.4(8) . . ? C7 C6 C5 122.9(9) . . ? N2 C6 C5 131.4(9) . . ? C8 C7 C6 109.9(9) . . ? C8 C7 H7A 125.0 . . ? C6 C7 H7A 125.0 . . ? C7 C8 C9 107.0(10) . . ? C7 C8 H8A 126.5 . . ? C9 C8 H8A 126.5 . . ? N2 C9 C8 108.2(8) . . ? N2 C9 C10 121.0(9) . . ? C8 C9 C10 130.8(10) . . ? C11 C10 C9 119.3(9) . . ? C11 C10 C31 121.6(9) . . ? C9 C10 C31 119.0(9) . . ? C10 C11 N3 120.3(8) . . ? C10 C11 C12 132.9(9) . . ? N3 C11 C12 106.4(8) . . ? C13 C12 C11 108.5(9) . . ? C13 C12 H12A 125.7 . . ? C11 C12 H12A 125.7 . . ? C12 C13 C14 109.5(9) . . ? C12 C13 H13A 125.2 . . ? C14 C13 H13A 125.2 . . ? N3 C14 C13 106.8(8) . . ? N3 C14 C15 127.2(8) . . ? C13 C14 C15 125.4(9) . . ? C16 C15 C14 133.4(9) . . ? C16 C15 C41 110.1(8) . . ? C14 C15 C41 115.8(7) . . ? C17 C16 C15 121.9(8) . . ? C17 C16 N4 106.7(8) . . ? C15 C16 N4 131.2(9) . . ? C16 C17 C18 109.6(9) . . ? C16 C17 H17A 125.2 . . ? C18 C17 H17A 125.2 . . ? C17 C18 C19 107.0(9) . . ? C17 C18 H18A 126.5 . . ? C19 C18 H18A 126.5 . . ? N4 C19 C20 120.4(8) . . ? N4 C19 C18 107.2(8) . . ? C20 C19 C18 132.3(9) . . ? C1 C20 C19 119.2(9) . . ? C1 C20 C51 123.4(8) . . ? C19 C20 C51 117.5(8) . . ? C22 C21 C26 116.8(9) . . ? C22 C21 C5 123.4(9) . . ? C26 C21 C5 119.7(9) . . ? C23 C22 C21 123.3(11) . . ? C23 C22 H22A 118.3 . . ? C21 C22 H22A 118.3 . . ? C24 C23 C22 117.7(11) . . ? C24 C23 H23A 121.2 . . ? C22 C23 H23A 121.2 . . ? C23 C24 C25 123.3(10) . . ? C23 C24 Cl1 119.2(10) . . ? C25 C24 Cl1 117.5(9) . . ? C24 C25 C26 118.3(11) . . ? C24 C25 H25A 120.9 . . ? C26 C25 H25A 120.9 . . ? C21 C26 C25 120.4(11) . . ? C21 C26 H26A 119.8 . . ? C25 C26 H26A 119.8 . . ? C36 C31 C32 118.2(10) . . ? C36 C31 C10 120.8(10) . . ? C32 C31 C10 121.0(10) . . ? C33 C32 C31 117.2(10) . . ? C33 C32 H32A 121.4 . . ? C31 C32 H32A 121.4 . . ? C34 C33 C32 122.4(11) . . ? C34 C33 H33A 118.8 . . ? C32 C33 H33A 118.8 . . ? C33 C34 C35 120.4(10) . . ? C33 C34 Cl2 120.5(9) . . ? C35 C34 Cl2 119.0(9) . . ? C36 C35 C34 116.2(11) . . ? C36 C35 H35A 121.9 . . ? C34 C35 H35A 121.9 . . ? C35 C36 C31 125.3(11) . . ? C35 C36 H36A 117.4 . . ? C31 C36 H36A 117.4 . . ? C46 C41 C42 121.8(9) . . ? C46 C41 C15 116.9(9) . . ? C42 C41 C15 121.3(9) . . ? C41 C42 C43 119.1(10) . . ? C41 C42 H42A 120.5 . . ? C43 C42 H42A 120.5 . . ? C44 C43 C42 118.4(10) . . ? C44 C43 H43A 120.8 . . ? C42 C43 H43A 120.8 . . ? C45 C44 C43 120.8(9) . . ? C45 C44 Cl3 120.2(9) . . ? C43 C44 Cl3 119.0(9) . . ? C44 C45 C46 120.4(10) . . ? C44 C45 H45A 119.8 . . ? C46 C45 H45A 119.8 . . ? C41 C46 C45 119.5(9) . . ? C41 C46 H46A 120.2 . . ? C45 C46 H46A 120.2 . . ? C52 C51 C56 117.6(10) . . ? C52 C51 C20 120.2(9) . . ? C56 C51 C20 121.9(9) . . ? C51 C52 C53 123.2(11) . . ? C51 C52 H52A 118.4 . . ? C53 C52 H52A 118.4 . . ? C54 C53 C52 116.6(11) . . ? C54 C53 H53A 121.7 . . ? C52 C53 H53A 121.7 . . ? C55 C54 C53 122.6(10) . . ? C55 C54 Cl4 119.0(9) . . ? C53 C54 Cl4 118.3(9) . . ? C54 C55 C56 120.0(11) . . ? C54 C55 H55A 120.0 . . ? C56 C55 H55A 120.0 . . ? C51 C56 C55 119.7(10) . . ? C51 C56 H56A 120.1 . . ? C55 C56 H56A 120.1 . . ? O1' B1' N1' 121.1(9) . . ? O1' B1' N4' 121.2(10) . . ? N1' B1' N4' 117.6(10) . . ? O1' B2' N3' 121.6(10) . . ? O1' B2' N2' 122.6(10) . . ? N3' B2' N2' 115.7(8) . . ? B2' O1' B1' 112.7(8) . . ? B1' N1' C1' 120.6(8) . . ? B1' N1' C4' 130.7(9) . . ? C1' N1' C4' 107.9(8) . . ? C6' N2' C9' 110.0(8) . . ? C6' N2' B2' 130.0(8) . . ? C9' N2' B2' 118.4(8) . . ? C11' N3' C14' 107.9(8) . . ? C11' N3' B2' 120.1(8) . . ? C14' N3' B2' 128.7(8) . . ? C16' N4' C19' 108.1(7) . . ? C16' N4' B1' 131.8(8) . . ? C19' N4' B1' 119.1(9) . . ? C2' C1' C20' 133.5(10) . . ? C2' C1' N1' 106.8(8) . . ? C20' C1' N1' 119.7(10) . . ? C3' C2' C1' 111.8(10) . . ? C3' C2' H2'A 124.1 . . ? C1' C2' H2'A 124.1 . . ? C2' C3' C4' 107.8(9) . . ? C2' C3' H3'A 126.1 . . ? C4' C3' H3'A 126.1 . . ? C5' C4' N1' 130.4(9) . . ? C5' C4' C3' 122.3(9) . . ? N1' C4' C3' 105.8(8) . . ? C6' C5' C4' 133.7(9) . . ? C6' C5' C21' 114.5(7) . . ? C4' C5' C21' 111.4(8) . . ? N2' C6' C5' 130.7(8) . . ? N2' C6' C7' 107.0(8) . . ? C5' C6' C7' 121.5(9) . . ? C8' C7' C6' 107.0(8) . . ? C8' C7' H7'A 126.5 . . ? C6' C7' H7'A 126.5 . . ? C7' C8' C9' 109.6(9) . . ? C7' C8' H8'A 125.2 . . ? C9' C8' H8'A 125.2 . . ? C10' C9' C8' 133.9(10) . . ? C10' C9' N2' 119.8(9) . . ? C8' C9' N2' 106.3(9) . . ? C9' C10' C11' 124.6(9) . . ? C9' C10' C31' 119.9(9) . . ? C11' C10' C31' 115.1(10) . . ? C12' C11' N3' 108.9(8) . . ? C12' C11' C10' 134.8(9) . . ? N3' C11' C10' 116.1(9) . . ? C13' C12' C11' 107.6(9) . . ? C13' C12' H12B 126.2 . . ? C11' C12' H12B 126.2 . . ? C12' C13' C14' 109.9(9) . . ? C12' C13' H13B 125.0 . . ? C14' C13' H13B 125.0 . . ? C13' C14' N3' 105.6(8) . . ? C13' C14' C15' 122.8(9) . . ? N3' C14' C15' 131.2(9) . . ? C16' C15' C14' 131.3(9) . . ? C16' C15' C41' 115.1(8) . . ? C14' C15' C41' 112.7(8) . . ? N4' C16' C15' 129.9(8) . . ? N4' C16' C17' 108.0(8) . . ? C15' C16' C17' 121.9(9) . . ? C18' C17' C16' 107.0(9) . . ? C18' C17' H17C 126.5 . . ? C16' C17' H17C 126.5 . . ? C17' C18' C19' 110.9(9) . . ? C17' C18' H18C 124.6 . . ? C19' C18' H18C 124.6 . . ? C20' C19' N4' 121.0(9) . . ? C20' C19' C18' 133.2(9) . . ? N4' C19' C18' 105.8(9) . . ? C19' C20' C1' 119.0(10) . . ? C19' C20' C51' 121.3(9) . . ? C1' C20' C51' 119.8(10) . . ? C22' C21' C26' 120.8(10) . . ? C22' C21' C5' 119.8(9) . . ? C26' C21' C5' 119.4(9) . . ? C21' C22' C23' 119.1(11) . . ? C21' C22' H22B 120.5 . . ? C23' C22' H22B 120.5 . . ? C24' C23' C22' 120.0(10) . . ? C24' C23' H23C 120.0 . . ? C22' C23' H23C 120.0 . . ? C23' C24' C25' 121.5(11) . . ? C23' C24' Cl1' 119.8(9) . . ? C25' C24' Cl1' 118.7(9) . . ? C26' C25' C24' 117.4(11) . . ? C26' C25' H25B 121.3 . . ? C24' C25' H25B 121.3 . . ? C21' C26' C25' 121.1(11) . . ? C21' C26' H26B 119.4 . . ? C25' C26' H26B 119.4 . . ? C36' C31' C32' 119.6(10) . . ? C36' C31' C10' 121.9(10) . . ? C32' C31' C10' 118.4(10) . . ? C33' C32' C31' 119.9(10) . . ? C33' C32' H32B 120.0 . . ? C31' C32' H32B 120.0 . . ? C32' C33' C34' 117.9(11) . . ? C32' C33' H33B 121.0 . . ? C34' C33' H33B 121.0 . . ? C35' C34' C33' 122.1(10) . . ? C35' C34' Cl2' 120.3(10) . . ? C33' C34' Cl2' 117.3(10) . . ? C36' C35' C34' 118.8(11) . . ? C36' C35' H35B 120.6 . . ? C34' C35' H35B 120.6 . . ? C31' C36' C35' 121.5(11) . . ? C31' C36' H36B 119.2 . . ? C35' C36' H36B 119.2 . . ? C42' C41' C46' 119.7(9) . . ? C42' C41' C15' 124.2(10) . . ? C46' C41' C15' 116.1(9) . . ? C41' C42' C43' 121.2(12) . . ? C41' C42' H42B 119.4 . . ? C43' C42' H42B 119.4 . . ? C44' C43' C42' 118.0(11) . . ? C44' C43' H43B 121.0 . . ? C42' C43' H43B 121.0 . . ? C45' C44' C43' 120.9(11) . . ? C45' C44' Cl3' 121.6(10) . . ? C43' C44' Cl3' 117.5(9) . . ? C44' C45' C46' 119.2(11) . . ? C44' C45' H45B 120.4 . . ? C46' C45' H45B 120.4 . . ? C45' C46' C41' 120.8(10) . . ? C45' C46' H46B 119.6 . . ? C41' C46' H46B 119.6 . . ? C52' C51' C56' 117.4(10) . . ? C52' C51' C20' 121.2(10) . . ? C56' C51' C20' 121.3(10) . . ? C51' C52' C53' 122.2(11) . . ? C51' C52' H52B 118.9 . . ? C53' C52' H52B 118.9 . . ? C54' C53' C52' 116.3(10) . . ? C54' C53' H53B 121.9 . . ? C52' C53' H53B 121.9 . . ? C55' C54' C53' 125.1(10) . . ? C55' C54' Cl4' 116.5(9) . . ? C53' C54' Cl4' 118.4(10) . . ? C54' C55' C56' 115.6(10) . . ? C54' C55' H55B 122.2 . . ? C56' C55' H55B 122.2 . . ? C51' C56' C55' 123.3(10) . . ? C51' C56' H56B 118.3 . . ? C55' C56' H56B 118.3 . . ? Br1 B3 Br2 112.4(6) . . ? Br1 B3 Br4 110.4(7) . . ? Br2 B3 Br4 109.3(7) . . ? Br1 B3 Br3 108.9(7) . . ? Br2 B3 Br3 108.6(6) . . ? Br4 B3 Br3 107.2(6) . . ? Br7 B4 Br5 108.3(7) . . ? Br7 B4 Br8 111.0(5) . . ? Br5 B4 Br8 109.8(6) . . ? Br7 B4 Br6 110.1(6) . . ? Br5 B4 Br6 109.3(5) . . ? Br8 B4 Br6 108.3(7) . . ? Br11 B5 Br10 111.9(6) . . ? Br11 B5 Br12 109.1(6) . . ? Br10 B5 Br12 108.3(5) . . ? Br11 B5 Br9 110.5(6) . . ? Br10 B5 Br9 109.2(6) . . ? Br12 B5 Br9 107.8(6) . . ? Br16 B6 Br15 111.5(9) . . ? Br16 B6 Br14 109.6(8) . . ? Br15 B6 Br14 109.5(8) . . ? Br16 B6 Br13 108.8(8) . . ? Br15 B6 Br13 108.6(8) . . ? Br14 B6 Br13 108.7(9) . . ? C2S C1S C6S 121.6(16) . . ? C2S C1S C7S 119.7(16) . . ? C6S C1S C7S 118.5(17) . . ? C1S C2S C3S 119.2(16) . . ? C1S C2S H2SA 120.4 . . ? C3S C2S H2SA 120.4 . . ? C4S C3S C2S 120.8(17) . . ? C4S C3S H3SA 119.6 . . ? C2S C3S H3SA 119.6 . . ? C3S C4S C5S 122.3(18) . . ? C3S C4S H4SA 118.8 . . ? C5S C4S H4SA 118.8 . . ? C4S C5S C6S 117.0(17) . . ? C4S C5S H5SA 121.5 . . ? C6S C5S H5SA 121.5 . . ? C1S C6S C5S 118.8(17) . . ? C1S C6S H6SA 120.6 . . ? C5S C6S H6SA 120.6 . . ? C1S C7S H7SA 109.5 . . ? C1S C7S H7SB 109.5 . . ? H7SA C7S H7SB 109.5 . . ? C1S C7S H7SC 109.5 . . ? H7SA C7S H7SC 109.5 . . ? H7SB C7S H7SC 109.5 . . ? C13S C8S C9S 120.2(13) . . ? C13S C8S C14S 125.3(17) . . ? C9S C8S C14S 114.4(16) . . ? C8S C9S C10S 120.8(16) . . ? C8S C9S H9SA 119.6 . . ? C10S C9S H9SA 119.6 . . ? C11S C10S C9S 117.3(18) . . ? C11S C10S H10A 121.3 . . ? C9S C10S H10A 121.3 . . ? C10S C11S C12S 124.6(16) . . ? C10S C11S H11A 117.7 . . ? C12S C11S H11A 117.7 . . ? C11S C12S C13S 116.3(16) . . ? C11S C12S H12C 121.9 . . ? C13S C12S H12C 121.9 . . ? C8S C13S C12S 120.4(16) . . ? C8S C13S H13C 119.8 . . ? C12S C13S H13C 119.8 . . ? C8S C14S H14A 109.5 . . ? C8S C14S H14B 109.5 . . ? H14A C14S H14B 109.5 . . ? C8S C14S H14C 109.5 . . ? H14A C14S H14C 109.5 . . ? H14B C14S H14C 109.5 . . ? C23S C22S C27S 120(2) . . ? C23S C22S C28S 121(2) . . ? C27S C22S C28S 119(2) . . ? C22S C23S C24S 128(3) . . ? C22S C23S H23D 116.1 . . ? C24S C23S H23D 116.1 . . ? C23S C24S C25S 111(2) . . ? C23S C24S H24A 124.3 . . ? C25S C24S H24A 124.3 . . ? C26S C25S C24S 120(2) . . ? C26S C25S H25C 120.2 . . ? C24S C25S H25C 120.2 . . ? C25S C26S C27S 119.3(19) . . ? C25S C26S H26C 120.4 . . ? C27S C26S H26C 120.4 . . ? C22S C27S C26S 121.1(17) . . ? C22S C27S H27A 119.4 . . ? C26S C27S H27A 119.4 . . ? C22S C28S H28A 109.5 . . ? C22S C28S H28B 109.5 . . ? H28A C28S H28B 109.5 . . ? C22S C28S H28C 109.5 . . ? H28A C28S H28C 109.5 . . ? H28B C28S H28C 109.5 . . ? C44S C43S C48S 123.1(19) . . ? C44S C43S C49S 121.2(18) . . ? C48S C43S C49S 115.6(19) . . ? C43S C44S C45S 118.5(17) . . ? C43S C44S H44A 120.7 . . ? C45S C44S H44A 120.7 . . ? C46S C45S C44S 122.3(16) . . ? C46S C45S H45C 118.9 . . ? C44S C45S H45C 118.9 . . ? C45S C46S C47S 116.5(17) . . ? C45S C46S H46C 121.8 . . ? C47S C46S H46C 121.8 . . ? C48S C47S C46S 121.6(16) . . ? C48S C47S H47A 119.2 . . ? C46S C47S H47A 119.2 . . ? C43S C48S C47S 117.9(17) . . ? C43S C48S H48A 121.1 . . ? C47S C48S H48A 121.1 . . ? C43S C49S H49A 109.5 . . ? C43S C49S H49B 109.5 . . ? H49A C49S H49B 109.5 . . ? C43S C49S H49C 109.5 . . ? H49A C49S H49C 109.5 . . ? H49B C49S H49C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.786 _refine_diff_density_min -1.221 _refine_diff_density_rms 0.196