# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Francesc Teixidor' _publ_contact_author_email TEIXIDOR@ICMAB.ES _publ_section_title ; Using the Wittig reaction to produce alkenylcarbaboranes ; loop_ _publ_author_name 'Francesc Teixidor' 'Antonio Sousa-Pedrares' 'Clara Vinas' # Attachment 'E,E-2.cif' data_asb27b2 _database_code_depnum_ccdc_archive 'CCDC 746811' #TrackingRef 'E,E-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H34 B20' _chemical_formula_weight 514.69 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 2(1)/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 6.7914(2) _cell_length_b 21.7400(7) _cell_length_c 9.7036(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.800(2) _cell_angle_gamma 90.00 _cell_volume 1385.16(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1961 _cell_measurement_theta_min 2.87 _cell_measurement_theta_max 25.86 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.234 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 532 _exptl_absorpt_coefficient_mu 0.059 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9815 _exptl_absorpt_correction_T_max 0.9872 _exptl_absorpt_process_details ; Sheldrick, G.M. SADABS: Program for absorption correction using area detector data. University of G\"ottingen, Germany, 1996. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 APEX-II CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21103 _diffrn_reflns_av_R_equivalents 0.0329 _diffrn_reflns_av_sigmaI/netI 0.0211 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 26.01 _reflns_number_total 2723 _reflns_number_gt 2266 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2723 _refine_ls_number_parameters 193 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1223 _refine_ls_R_factor_gt 0.1094 _refine_ls_wR_factor_ref 0.3995 _refine_ls_wR_factor_gt 0.3810 _refine_ls_goodness_of_fit_ref 1.839 _refine_ls_restrained_S_all 1.840 _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 B3 B 0.0522(8) 0.90030(18) 0.8931(4) 0.0407(11) Uani 1 1 d . . . H3 H -0.0426 0.9295 0.8061 0.049 Uiso 1 1 calc R . . B4 B 0.1979(6) 0.93387(17) 1.0489(5) 0.0366(10) Uani 1 1 d . . . H4 H 0.2054 0.9849 1.0658 0.044 Uiso 1 1 calc R . . B5 B 0.3991(5) 0.88436(16) 1.1075(5) 0.0338(10) Uani 1 1 d . . . H5 H 0.5487 0.9046 1.1662 0.041 Uiso 1 1 calc R . . B6 B 0.3978(6) 0.82624(19) 0.9972(5) 0.0398(12) Uani 1 1 d . . . H6 H 0.5417 0.8063 0.9800 0.048 Uiso 1 1 calc R . . B7 B -0.0280(6) 0.82663(16) 0.9346(4) 0.0307(9) Uani 1 1 d . . . H7 H -0.1766 0.8065 0.8738 0.037 Uiso 1 1 calc R . . B8 B -0.0158(5) 0.88924(15) 1.0558(4) 0.0232(8) Uani 1 1 d . . . H8 H -0.1554 0.9106 1.0769 0.028 Uiso 1 1 calc R . . B9 B 0.2101(5) 0.88080(17) 1.1920(4) 0.0295(9) Uani 1 1 d . . . H9 H 0.2232 0.8971 1.3035 0.035 Uiso 1 1 calc R . . B10 B 0.3376(5) 0.81362(16) 1.1593(4) 0.0274(9) Uani 1 1 d . . . H10 H 0.4345 0.7856 1.2480 0.033 Uiso 1 1 calc R . . B11 B 0.1899(6) 0.77982(16) 0.9989(4) 0.0286(9) Uani 1 1 d . . . H11 H 0.1878 0.7289 0.9812 0.034 Uiso 1 1 calc R . . B12 B 0.0680(5) 0.81450(15) 1.1209(4) 0.0227(8) Uani 1 1 d . . . H12 H -0.0167 0.7865 1.1838 0.027 Uiso 1 1 calc R . . C1 C 0.3080(9) 0.8963(2) 0.9271(6) 0.0689(18) Uani 1 1 d . . . C2 C 0.1791(9) 0.8331(2) 0.8583(5) 0.0609(15) Uani 1 1 d D . . C3 C 0.3953(8) 0.9252(2) 0.8242(5) 0.0608(13) Uani 1 1 d . . . H3A H 0.5370 0.9334 0.8565 0.073 Uiso 1 1 calc R . . C4 C 0.3109(8) 0.9424(2) 0.6914(6) 0.0623(14) Uani 1 1 d . . . H4A H 0.1688 0.9347 0.6597 0.075 Uiso 1 1 calc R . . C5 C 0.3962(5) 0.96983(16) 0.5900(3) 0.0306(9) Uani 1 1 d . . . C6 C 0.5482(5) 0.93801(14) 0.5416(3) 0.0268(8) Uani 1 1 d . . . C7 C 0.5948(6) 0.87446(15) 0.5768(3) 0.0319(9) Uani 1 1 d . . . H7A H 0.5233 0.8531 0.6344 0.038 Uiso 1 1 calc R . . C8 C 0.7397(6) 0.84488(16) 0.5287(4) 0.0390(10) Uani 1 1 d . . . H8A H 0.7682 0.8028 0.5522 0.047 Uiso 1 1 calc R . . C9 C 0.8498(6) 0.87631(18) 0.4431(4) 0.0414(10) Uani 1 1 d . . . H9A H 0.9527 0.8553 0.4113 0.050 Uiso 1 1 calc R . . C10 C 0.8083(6) 0.93661(17) 0.4064(3) 0.0356(10) Uani 1 1 d . . . H10A H 0.8830 0.9571 0.3495 0.043 Uiso 1 1 calc R . . C11 C 0.6540(5) 0.96908(15) 0.4526(3) 0.0271(8) Uani 1 1 d . . . H2 H 0.171(6) 0.8285(16) 0.751(2) 0.032 Uiso 1 1 d 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 B3 0.066(3) 0.032(2) 0.035(2) 0.0157(16) 0.031(2) 0.0243(19) B4 0.036(2) 0.0191(17) 0.063(3) 0.0027(17) 0.029(2) 0.0024(15) B5 0.0188(17) 0.0187(17) 0.069(3) 0.0029(16) 0.0211(18) -0.0020(13) B6 0.030(2) 0.034(2) 0.066(3) 0.029(2) 0.032(2) 0.0147(16) B7 0.045(2) 0.0265(17) 0.0173(17) -0.0028(13) 0.0024(15) 0.0077(15) B8 0.0245(17) 0.0256(17) 0.0218(17) -0.0055(13) 0.0102(13) -0.0010(13) B9 0.0252(18) 0.034(2) 0.030(2) -0.0064(15) 0.0077(15) -0.0057(14) B10 0.0237(17) 0.0283(18) 0.0305(19) 0.0046(14) 0.0073(14) -0.0019(14) B11 0.044(2) 0.0226(17) 0.0210(18) 0.0032(13) 0.0112(15) 0.0060(15) B12 0.0244(17) 0.0268(17) 0.0174(16) 0.0006(12) 0.0064(13) -0.0065(13) C1 0.105(4) 0.052(3) 0.078(4) 0.041(2) 0.076(3) 0.049(3) C2 0.115(4) 0.047(2) 0.037(2) 0.0184(18) 0.048(3) 0.045(3) C3 0.065(3) 0.056(3) 0.063(3) 0.003(2) 0.019(3) -0.005(2) C4 0.058(3) 0.063(3) 0.065(3) 0.000(2) 0.014(2) 0.003(2) C5 0.0430(19) 0.0351(19) 0.0189(16) 0.0088(12) 0.0172(14) 0.0152(14) C6 0.0391(19) 0.0298(17) 0.0122(14) 0.0048(12) 0.0081(13) 0.0117(14) C7 0.047(2) 0.0309(18) 0.0172(16) 0.0025(12) 0.0076(14) 0.0097(14) C8 0.056(2) 0.0344(19) 0.0222(17) -0.0024(13) 0.0014(15) 0.0203(17) C9 0.052(2) 0.052(2) 0.0222(18) 0.0007(15) 0.0125(16) 0.0291(18) C10 0.044(2) 0.048(2) 0.0171(16) 0.0032(14) 0.0130(14) 0.0188(16) C11 0.0351(18) 0.0340(18) 0.0142(15) 0.0022(12) 0.0099(12) 0.0115(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 B3 C1 1.686(7) . ? B3 B4 1.741(7) . ? B3 B8 1.770(5) . ? B3 B7 1.771(6) . ? B3 C2 1.772(5) . ? B4 B5 1.718(5) . ? B4 C1 1.754(6) . ? B4 B8 1.761(5) . ? B4 B9 1.791(6) . ? B5 B6 1.654(6) . ? B5 B9 1.693(5) . ? B5 B10 1.703(5) . ? B5 C1 1.721(7) . ? B6 C1 1.716(5) . ? B6 C2 1.739(7) . ? B6 B11 1.739(6) . ? B6 B10 1.745(5) . ? B7 C2 1.755(6) . ? B7 B11 1.773(5) . ? B7 B12 1.778(5) . ? B7 B8 1.787(5) . ? B8 B9 1.760(5) . ? B8 B12 1.783(5) . ? B9 B10 1.768(5) . ? B9 B12 1.773(5) . ? B10 B12 1.773(5) . ? B10 B11 1.780(5) . ? B11 B12 1.776(5) . ? B11 C2 1.777(5) . ? C1 C3 1.430(6) . ? C1 C2 1.674(9) . ? C3 C4 1.323(7) . ? C4 C5 1.397(6) . ? C5 C11 1.407(5) 3_676 ? C5 C6 1.419(4) . ? C6 C11 1.426(4) . ? C6 C7 1.439(4) . ? C7 C8 1.354(5) . ? C8 C9 1.426(6) . ? C9 C10 1.369(5) . ? C10 C11 1.428(4) . ? C11 C5 1.407(5) 3_676 ? 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 B3 B4 61.5(3) . . ? C1 B3 B8 108.0(3) . . ? B4 B3 B8 60.2(2) . . ? C1 B3 B7 105.7(3) . . ? B4 B3 B7 108.8(3) . . ? B8 B3 B7 60.6(2) . . ? C1 B3 C2 57.8(3) . . ? B4 B3 C2 108.4(3) . . ? B8 B3 C2 108.0(3) . . ? B7 B3 C2 59.4(2) . . ? B5 B4 B3 104.6(3) . . ? B5 B4 C1 59.4(3) . . ? B3 B4 C1 57.7(3) . . ? B5 B4 B8 103.6(3) . . ? B3 B4 B8 60.7(2) . . ? C1 B4 B8 105.5(3) . . ? B5 B4 B9 57.6(2) . . ? B3 B4 B9 107.8(3) . . ? C1 B4 B9 106.2(2) . . ? B8 B4 B9 59.4(2) . . ? B6 B5 B9 113.5(3) . . ? B6 B5 B10 62.6(2) . . ? B9 B5 B10 62.7(2) . . ? B6 B5 B4 113.1(3) . . ? B9 B5 B4 63.3(2) . . ? B10 B5 B4 115.4(3) . . ? B6 B5 C1 61.1(3) . . ? B9 B5 C1 112.3(3) . . ? B10 B5 C1 112.7(3) . . ? B4 B5 C1 61.3(2) . . ? B5 B6 C1 61.4(3) . . ? B5 B6 C2 107.3(3) . . ? C1 B6 C2 58.0(3) . . ? B5 B6 B11 107.9(3) . . ? C1 B6 B11 108.2(3) . . ? C2 B6 B11 61.5(3) . . ? B5 B6 B10 60.1(2) . . ? C1 B6 B10 110.8(3) . . ? C2 B6 B10 111.2(3) . . ? B11 B6 B10 61.5(2) . . ? C2 B7 B3 60.3(2) . . ? C2 B7 B11 60.5(2) . . ? B3 B7 B11 108.8(3) . . ? C2 B7 B12 108.4(3) . . ? B3 B7 B12 108.1(3) . . ? B11 B7 B12 60.02(19) . . ? C2 B7 B8 108.0(3) . . ? B3 B7 B8 59.7(2) . . ? B11 B7 B8 108.1(3) . . ? B12 B7 B8 60.03(19) . . ? B9 B8 B4 61.1(2) . . ? B9 B8 B3 107.9(3) . . ? B4 B8 B3 59.1(3) . . ? B9 B8 B12 60.0(2) . . ? B4 B8 B12 108.9(3) . . ? B3 B8 B12 107.9(2) . . ? B9 B8 B7 107.5(2) . . ? B4 B8 B7 107.2(2) . . ? B3 B8 B7 59.7(2) . . ? B12 B8 B7 59.74(18) . . ? B5 B9 B8 104.8(3) . . ? B5 B9 B10 58.91(19) . . ? B8 B9 B10 108.9(2) . . ? B5 B9 B12 104.7(3) . . ? B8 B9 B12 60.62(19) . . ? B10 B9 B12 60.1(2) . . ? B5 B9 B4 59.0(2) . . ? B8 B9 B4 59.5(2) . . ? B10 B9 B4 108.7(3) . . ? B12 B9 B4 108.0(3) . . ? B5 B10 B6 57.3(2) . . ? B5 B10 B9 58.4(2) . . ? B6 B10 B9 105.7(3) . . ? B5 B10 B12 104.3(2) . . ? B6 B10 B12 106.0(3) . . ? B9 B10 B12 60.12(19) . . ? B5 B10 B11 103.9(3) . . ? B6 B10 B11 59.1(2) . . ? B9 B10 B11 107.8(3) . . ? B12 B10 B11 60.0(2) . . ? B6 B11 B7 105.7(3) . . ? B6 B11 B12 106.1(3) . . ? B7 B11 B12 60.13(19) . . ? B6 B11 C2 59.3(3) . . ? B7 B11 C2 59.2(2) . . ? B12 B11 C2 107.5(2) . . ? B6 B11 B10 59.4(2) . . ? B7 B11 B10 107.7(2) . . ? B12 B11 B10 59.79(19) . . ? C2 B11 B10 107.8(3) . . ? B10 B12 B9 59.8(2) . . ? B10 B12 B11 60.2(2) . . ? B9 B12 B11 107.7(2) . . ? B10 B12 B7 107.8(2) . . ? B9 B12 B7 107.3(2) . . ? B11 B12 B7 59.8(2) . . ? B10 B12 B8 107.7(2) . . ? B9 B12 B8 59.33(19) . . ? B11 B12 B8 108.1(2) . . ? B7 B12 B8 60.23(19) . . ? C3 C1 C2 110.5(4) . . ? C3 C1 B3 115.6(4) . . ? C2 C1 B3 63.7(3) . . ? C3 C1 B6 119.9(3) . . ? C2 C1 B6 61.7(3) . . ? B3 C1 B6 111.5(3) . . ? C3 C1 B5 132.2(5) . . ? C2 C1 B5 107.3(3) . . ? B3 C1 B5 106.9(3) . . ? B6 C1 B5 57.5(3) . . ? C3 C1 B4 126.2(4) . . ? C2 C1 B4 112.4(3) . . ? B3 C1 B4 60.8(2) . . ? B6 C1 B4 108.4(3) . . ? B5 C1 B4 59.3(2) . . ? C1 C2 B6 60.3(3) . . ? C1 C2 B7 107.0(3) . . ? B6 C2 B7 106.5(3) . . ? C1 C2 B3 58.5(3) . . ? B6 C2 B3 106.5(3) . . ? B7 C2 B3 60.3(2) . . ? C1 C2 B11 108.3(3) . . ? B6 C2 B11 59.3(2) . . ? B7 C2 B11 60.3(2) . . ? B3 C2 B11 108.5(2) . . ? C4 C3 C1 130.6(5) . . ? C3 C4 C5 130.7(5) . . ? C4 C5 C11 119.9(3) . 3_676 ? C4 C5 C6 119.5(3) . . ? C11 C5 C6 120.3(3) 3_676 . ? C5 C6 C11 119.4(3) . . ? C5 C6 C7 121.6(3) . . ? C11 C6 C7 119.0(3) . . ? C8 C7 C6 120.6(3) . . ? C7 C8 C9 120.6(3) . . ? C10 C9 C8 120.4(3) . . ? C9 C10 C11 120.7(3) . . ? C5 C11 C6 120.2(3) 3_676 . ? C5 C11 C10 121.1(3) 3_676 . ? C6 C11 C10 118.7(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.743 _refine_diff_density_min -1.032 _refine_diff_density_rms 0.118 # Attachment 'E-1.cif' data_asb27b1 _database_code_depnum_ccdc_archive 'CCDC 746812' #TrackingRef 'E-1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H22 B10' _chemical_formula_weight 346.46 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 0.0000 '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 0.0000 '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 n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 13.7778(3) _cell_length_b 14.5476(3) _cell_length_c 19.4191(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.0820(10) _cell_angle_gamma 90.00 _cell_volume 3862.55(14) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2761 _cell_measurement_theta_min 2.8085 _cell_measurement_theta_max 21.5485 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.192 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 0.059 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9888 _exptl_absorpt_correction_T_max 0.9959 _exptl_absorpt_process_details ; Sheldrick, G.M. SADABS: Program for absorption correction using area detector data. University of G\"ottingen, Germany, 1996. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 X8 KappaAPEXII' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15084 _diffrn_reflns_av_R_equivalents 0.0549 _diffrn_reflns_av_sigmaI/netI 0.0856 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 26.38 _reflns_number_total 7889 _reflns_number_gt 5405 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER APEX' _computing_cell_refinement 'BRUKER APEX' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0681P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7889 _refine_ls_number_parameters 1021 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0909 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.1365 _refine_ls_wR_factor_gt 0.1223 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.977 _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 B3 B 0.4531(4) 0.0863(4) 0.4567(3) 0.0246(11) Uani 1 1 d . . . H3 H 0.3866 0.0865 0.4172 0.029 Uiso 1 1 calc R . . B4 B 0.5143(4) 0.1894(4) 0.4852(3) 0.0282(12) Uani 1 1 d . . . H4 H 0.4885 0.2585 0.4652 0.034 Uiso 1 1 calc R . . B5 B 0.6405(4) 0.1637(4) 0.5046(3) 0.0246(12) Uani 1 1 d . . . H5 H 0.6976 0.2164 0.4972 0.029 Uiso 1 1 calc R . . B6 B 0.6587(4) 0.0463(4) 0.4874(3) 0.0281(12) Uani 1 1 d . . . H6 H 0.7270 0.0204 0.4681 0.034 Uiso 1 1 calc R . . B7 B 0.4671(4) 0.0052(4) 0.5237(2) 0.0237(12) Uani 1 1 d . . . H7 H 0.4100 -0.0483 0.5290 0.028 Uiso 1 1 calc R . . B8 B 0.4491(4) 0.1233(4) 0.5419(3) 0.0266(12) Uani 1 1 d . . . H8 H 0.3800 0.1490 0.5601 0.032 Uiso 1 1 calc R . . B9 B 0.5666(4) 0.1713(4) 0.5727(3) 0.0241(12) Uani 1 1 d . . . H9 H 0.5750 0.2285 0.6116 0.029 Uiso 1 1 calc R . . B10 B 0.6567(4) 0.0826(4) 0.5731(3) 0.0231(12) Uani 1 1 d . . . H10 H 0.7241 0.0813 0.6118 0.028 Uiso 1 1 calc R . . B11 B 0.5942(4) -0.0201(4) 0.5432(2) 0.0235(11) Uani 1 1 d . . . H11 H 0.6202 -0.0899 0.5615 0.028 Uiso 1 1 calc R . . B12 B 0.5363(4) 0.0572(4) 0.5962(2) 0.0230(12) Uani 1 1 d . . . H12 H 0.5244 0.0392 0.6506 0.028 Uiso 1 1 calc R . . C1 C 0.5694(4) 0.1103(3) 0.4386(2) 0.0270(11) Uani 1 1 d . . . C2 C 0.5436(3) 0.0056(3) 0.4616(2) 0.0259(10) Uani 1 1 d . . . C3 C 0.5808(5) 0.1296(3) 0.3643(2) 0.0450(16) Uani 1 1 d . . . H3A H 0.5797 0.1933 0.3533 0.054 Uiso 1 1 calc R . . C4 C 0.5910(5) 0.0815(4) 0.3163(3) 0.0596(19) Uani 1 1 d . . . H4A H 0.5920 0.0175 0.3261 0.072 Uiso 1 1 calc R . . C5 C 0.6023(4) 0.1053(3) 0.2429(2) 0.0270(12) Uani 1 1 d . . . C6 C 0.6957(3) 0.1158(3) 0.2229(2) 0.0246(10) Uani 1 1 d . . . C7 C 0.7838(4) 0.1070(3) 0.2689(2) 0.0344(12) Uani 1 1 d . . . H7A H 0.7801 0.0938 0.3164 0.041 Uiso 1 1 calc R . . C8 C 0.8735(4) 0.1169(3) 0.2469(3) 0.0391(13) Uani 1 1 d . . . H8A H 0.9309 0.1105 0.2792 0.047 Uiso 1 1 calc R . . C9 C 0.8818(4) 0.1364(3) 0.1771(3) 0.0369(13) Uani 1 1 d . . . H9A H 0.9446 0.1426 0.1622 0.044 Uiso 1 1 calc R . . C10 C 0.8001(3) 0.1465(3) 0.1308(2) 0.0274(11) Uani 1 1 d . . . H10A H 0.8066 0.1605 0.0838 0.033 Uiso 1 1 calc R . . C11 C 0.7049(4) 0.1365(3) 0.1513(2) 0.0237(10) Uani 1 1 d . . . C12 C 0.6215(3) 0.1456(3) 0.1038(2) 0.0237(11) Uani 1 1 d . . . H12A H 0.6283 0.1600 0.0569 0.028 Uiso 1 1 calc R . . C13 C 0.5281(3) 0.1343(3) 0.1231(2) 0.0247(11) Uani 1 1 d . . . C14 C 0.4434(4) 0.1430(3) 0.0743(3) 0.0301(12) Uani 1 1 d . . . H14 H 0.4505 0.1556 0.0272 0.036 Uiso 1 1 calc R . . C15 C 0.3526(4) 0.1340(3) 0.0932(3) 0.0400(13) Uani 1 1 d . . . H15 H 0.2966 0.1405 0.0598 0.048 Uiso 1 1 calc R . . C16 C 0.3416(4) 0.1146(3) 0.1638(3) 0.0428(14) Uani 1 1 d . . . H16 H 0.2779 0.1084 0.1773 0.051 Uiso 1 1 calc R . . C17 C 0.4206(4) 0.1050(3) 0.2114(3) 0.0360(13) Uani 1 1 d . . . H17 H 0.4109 0.0920 0.2580 0.043 Uiso 1 1 calc R . . C18 C 0.5183(4) 0.1134(3) 0.1949(2) 0.0263(11) Uani 1 1 d . . . H2 H 0.539(3) -0.037(3) 0.425(2) 0.032 Uiso 1 1 d . . . B103 B 1.0196(3) 0.5030(4) 0.1021(2) 0.0255(12) Uani 1 1 d . . . H103 H 1.0208 0.5451 0.1505 0.031 Uiso 1 1 calc R . . B104 B 0.9438(4) 0.5302(4) 0.0247(2) 0.0241(12) Uani 1 1 d . . . H104 H 0.8943 0.5915 0.0212 0.029 Uiso 1 1 calc R . . B105 B 0.9074(4) 0.4273(4) -0.0194(2) 0.0224(11) Uani 1 1 d . . . H105 H 0.8348 0.4199 -0.0518 0.027 Uiso 1 1 calc R . . B106 B 0.9601(4) 0.3350(4) 0.0315(3) 0.0297(13) Uani 1 1 d . . . H106 H 0.9225 0.2670 0.0339 0.036 Uiso 1 1 calc R . . B107 B 1.1252(3) 0.4480(4) 0.0806(2) 0.0209(11) Uani 1 1 d . . . H107 H 1.1969 0.4537 0.1145 0.025 Uiso 1 1 calc R . . B108 B 1.0727(4) 0.5410(4) 0.0305(3) 0.0245(12) Uani 1 1 d . . . H108 H 1.1099 0.6094 0.0304 0.029 Uiso 1 1 calc R . . B109 B 1.0039(3) 0.4947(4) -0.0459(3) 0.0209(11) Uani 1 1 d . . . H109 H 0.9959 0.5327 -0.0964 0.025 Uiso 1 1 calc R . . B110 B 1.0138(4) 0.3730(4) -0.0421(3) 0.0249(12) Uani 1 1 d . . . H110 H 1.0121 0.3302 -0.0901 0.030 Uiso 1 1 calc R . . B111 B 1.0901(4) 0.3441(4) 0.0365(3) 0.0217(11) Uani 1 1 d . . . H111 H 1.1385 0.2819 0.0413 0.026 Uiso 1 1 calc R . . B112 B 1.1164(3) 0.4430(4) -0.0116(2) 0.0233(12) Uani 1 1 d . . . H112 H 1.1826 0.4465 -0.0397 0.028 Uiso 1 1 calc R . . C101 C 0.9233(3) 0.4345(3) 0.0688(2) 0.0256(11) Uani 1 1 d . . . C102 C 1.0288(3) 0.3868(3) 0.0999(2) 0.0231(10) Uani 1 1 d . . . C103 C 0.8382(3) 0.4330(4) 0.1108(2) 0.0355(13) Uani 1 1 d . . . H10B H 0.8431 0.4675 0.1526 0.043 Uiso 1 1 calc R . . C104 C 0.7598(3) 0.3876(3) 0.0928(2) 0.0292(11) Uani 1 1 d . . . H10C H 0.7608 0.3514 0.0522 0.035 Uiso 1 1 calc R . . C105 C 0.6671(3) 0.3818(3) 0.1247(2) 0.0230(10) Uani 1 1 d . . . C106 C 0.5780(3) 0.3815(3) 0.0794(2) 0.0226(10) Uani 1 1 d . . . C107 C 0.5734(3) 0.3895(3) 0.0062(2) 0.0279(11) Uani 1 1 d . . . H10D H 0.6322 0.3968 -0.0142 0.034 Uiso 1 1 calc R . . C108 C 0.4865(3) 0.3871(3) -0.0354(2) 0.0276(11) Uani 1 1 d . . . H10E H 0.4859 0.3922 -0.0842 0.033 Uiso 1 1 calc R . . C109 C 0.3978(3) 0.3771(3) -0.0078(3) 0.0330(12) Uani 1 1 d . . . H10F H 0.3378 0.3751 -0.0377 0.040 Uiso 1 1 calc R . . C110 C 0.3984(3) 0.3703(3) 0.0615(3) 0.0300(12) Uani 1 1 d . . . H11A H 0.3380 0.3644 0.0800 0.036 Uiso 1 1 calc R . . C111 C 0.4881(3) 0.3720(3) 0.1080(2) 0.0239(11) Uani 1 1 d . . . C112 C 0.4891(3) 0.3631(3) 0.1793(2) 0.0256(11) Uani 1 1 d . . . H11B H 0.4288 0.3566 0.1978 0.031 Uiso 1 1 calc R . . C113 C 0.5754(3) 0.3635(3) 0.2244(2) 0.0230(10) Uani 1 1 d . . . C114 C 0.5756(3) 0.3580(3) 0.2971(2) 0.0281(11) Uani 1 1 d . . . H114 H 0.5150 0.3534 0.3155 0.034 Uiso 1 1 calc R . . C115 C 0.6603(4) 0.3590(3) 0.3417(2) 0.0299(12) Uani 1 1 d . . . H115 H 0.6583 0.3584 0.3904 0.036 Uiso 1 1 calc R . . C116 C 0.7498(4) 0.3610(4) 0.3150(2) 0.0369(13) Uani 1 1 d . . . H116 H 0.8089 0.3581 0.3459 0.044 Uiso 1 1 calc R . . C117 C 0.7537(3) 0.3671(4) 0.2454(2) 0.0321(12) Uani 1 1 d . . . H117 H 0.8156 0.3676 0.2287 0.039 Uiso 1 1 calc R . . C118 C 0.6674(3) 0.3726(3) 0.1970(2) 0.0220(10) Uani 1 1 d . . . H102 H 1.030(3) 0.358(3) 0.147(2) 0.026 Uiso 1 1 d . . . B203 B 0.6965(4) 0.7638(4) -0.0993(3) 0.0338(14) Uani 1 1 d . . . H203 H 0.7180 0.8200 -0.0611 0.041 Uiso 1 1 calc R . . B204 B 0.5729(4) 0.7325(4) -0.1235(3) 0.0293(13) Uani 1 1 d . . . H204 H 0.5123 0.7692 -0.1014 0.035 Uiso 1 1 calc R . . B205 B 0.5665(4) 0.6134(4) -0.1400(3) 0.0274(12) Uani 1 1 d . . . H205 H 0.5017 0.5720 -0.1289 0.033 Uiso 1 1 calc R . . B206 B 0.6868(4) 0.5685(4) -0.1274(3) 0.0302(13) Uani 1 1 d . . . H206 H 0.7026 0.4971 -0.1077 0.036 Uiso 1 1 calc R . . B207 B 0.7628(4) 0.7412(4) -0.1708(2) 0.0266(12) Uani 1 1 d . . . H207 H 0.8281 0.7832 -0.1802 0.032 Uiso 1 1 calc R . . B208 B 0.6421(4) 0.7849(4) -0.1857(3) 0.0293(13) Uani 1 1 d . . . H208 H 0.6269 0.8563 -0.2058 0.035 Uiso 1 1 calc R . . B209 B 0.5616(4) 0.6921(4) -0.2103(2) 0.0234(11) Uani 1 1 d . . . H209 H 0.4930 0.7025 -0.2469 0.028 Uiso 1 1 calc R . . B210 B 0.6322(4) 0.5897(4) -0.2116(3) 0.0254(12) Uani 1 1 d . . . H210 H 0.6106 0.5324 -0.2488 0.030 Uiso 1 1 calc R . . B211 B 0.7564(4) 0.6202(4) -0.1863(3) 0.0259(12) Uani 1 1 d . . . H211 H 0.8185 0.5825 -0.2056 0.031 Uiso 1 1 calc R . . B212 B 0.6788(4) 0.6962(4) -0.2392(3) 0.0242(12) Uani 1 1 d . . . H212 H 0.6882 0.7088 -0.2949 0.029 Uiso 1 1 calc R . . C201 C 0.6510(3) 0.6577(4) -0.0779(2) 0.0277(11) Uani 1 1 d . . . C202 C 0.7592(3) 0.6635(4) -0.1064(2) 0.0286(12) Uani 1 1 d . . . C203 C 0.6528(4) 0.6329(4) -0.0029(2) 0.0371(13) Uani 1 1 d . . . H20A H 0.6923 0.5819 0.0130 0.044 Uiso 1 1 calc R . . C204 C 0.6075(3) 0.6725(4) 0.0414(2) 0.0312(11) Uani 1 1 d . . . H20B H 0.5677 0.7235 0.0258 0.037 Uiso 1 1 calc R . . C205 C 0.6106(3) 0.6466(3) 0.1160(2) 0.0192(10) Uani 1 1 d . . . C206 C 0.5219(3) 0.6233(3) 0.1412(2) 0.0198(10) Uani 1 1 d . . . C207 C 0.4295(3) 0.6244(3) 0.0979(2) 0.0291(11) Uani 1 1 d . . . H20C H 0.4270 0.6407 0.0504 0.035 Uiso 1 1 calc R . . C208 C 0.3459(3) 0.6023(3) 0.1243(3) 0.0313(12) Uani 1 1 d . . . H20D H 0.2852 0.6035 0.0951 0.038 Uiso 1 1 calc R . . C209 C 0.3483(3) 0.5776(3) 0.1942(2) 0.0297(12) Uani 1 1 d . . . H20E H 0.2889 0.5638 0.2121 0.036 Uiso 1 1 calc R . . C210 C 0.4329(3) 0.5732(3) 0.2364(2) 0.0255(11) Uani 1 1 d . . . H21A H 0.4328 0.5535 0.2831 0.031 Uiso 1 1 calc R . . C211 C 0.5231(3) 0.5976(3) 0.2121(2) 0.0210(10) Uani 1 1 d . . . C212 C 0.6115(3) 0.5940(3) 0.2547(2) 0.0212(10) Uani 1 1 d . . . H21B H 0.6121 0.5739 0.3013 0.025 Uiso 1 1 calc R . . C213 C 0.6987(3) 0.6187(3) 0.2315(2) 0.0203(10) Uani 1 1 d . . . C214 C 0.7910(4) 0.6160(4) 0.2756(3) 0.0348(12) Uani 1 1 d . . . H214 H 0.7930 0.5940 0.3218 0.042 Uiso 1 1 calc R . . C215 C 0.8745(3) 0.6441(3) 0.2526(3) 0.0298(11) Uani 1 1 d . . . H215 H 0.9344 0.6418 0.2825 0.036 Uiso 1 1 calc R . . C216 C 0.8732(3) 0.6765(3) 0.1846(2) 0.0274(11) Uani 1 1 d . . . H216 H 0.9321 0.6985 0.1697 0.033 Uiso 1 1 calc R . . C217 C 0.7905(3) 0.6774(3) 0.1399(2) 0.0257(11) Uani 1 1 d . . . H217 H 0.7927 0.6984 0.0937 0.031 Uiso 1 1 calc R . . C218 C 0.6993(3) 0.6475(3) 0.1604(2) 0.0183(9) Uani 1 1 d . . . H202 H 0.813(3) 0.655(3) -0.071(2) 0.022 Uiso 1 1 d . . . B303 B 0.2462(3) 0.9424(3) 0.3322(2) 0.0171(10) Uani 1 1 d . . . H303 H 0.2765 1.0135 0.3292 0.020 Uiso 1 1 calc R . . B304 B 0.3099(3) 0.8538(3) 0.3817(2) 0.0183(11) Uani 1 1 d . . . H304 H 0.3828 0.8660 0.4128 0.022 Uiso 1 1 calc R . . B305 B 0.2827(3) 0.7478(4) 0.3386(2) 0.0175(10) Uani 1 1 d . . . H305 H 0.3376 0.6908 0.3411 0.021 Uiso 1 1 calc R . . B306 B 0.2012(3) 0.7691(3) 0.2613(2) 0.0182(10) Uani 1 1 d . . . H306 H 0.2021 0.7276 0.2128 0.022 Uiso 1 1 calc R . . B307 B 0.1182(4) 0.9230(4) 0.3298(3) 0.0209(11) Uani 1 1 d . . . H307 H 0.0642 0.9809 0.3258 0.025 Uiso 1 1 calc R . . B308 B 0.2004(4) 0.9004(3) 0.4065(3) 0.0214(11) Uani 1 1 d . . . H308 H 0.2005 0.9434 0.4543 0.026 Uiso 1 1 calc R . . B309 B 0.2217(3) 0.7804(3) 0.4099(2) 0.0196(11) Uani 1 1 d . . . H309 H 0.2354 0.7436 0.4609 0.023 Uiso 1 1 calc R . . B310 B 0.1546(3) 0.7265(3) 0.3369(2) 0.0187(10) Uani 1 1 d . . . H310 H 0.1245 0.6553 0.3392 0.022 Uiso 1 1 calc R . . B311 B 0.0913(3) 0.8150(3) 0.2863(2) 0.0191(11) Uani 1 1 d . . . H311 H 0.0194 0.8027 0.2539 0.023 Uiso 1 1 calc R . . B312 B 0.1039(3) 0.8220(4) 0.3786(2) 0.0204(11) Uani 1 1 d . . . H312 H 0.0397 0.8134 0.4082 0.024 Uiso 1 1 calc R . . C301 C 0.2917(3) 0.8475(3) 0.29325(19) 0.0138(9) Uani 1 1 d . . . C302 C 0.1814(3) 0.8849(3) 0.2651(2) 0.0167(9) Uani 1 1 d . . . C303 C 0.3725(3) 0.8683(3) 0.2519(2) 0.0163(9) Uani 1 1 d . . . H30A H 0.3653 0.9188 0.2206 0.020 Uiso 1 1 calc R . . C304 C 0.4543(3) 0.8196(3) 0.2565(2) 0.0211(9) Uani 1 1 d . . . H30B H 0.4554 0.7634 0.2815 0.025 Uiso 1 1 calc R . . C305 C 0.5444(3) 0.8451(3) 0.2262(2) 0.0177(9) Uani 1 1 d . . . C306 C 0.6326(3) 0.8451(3) 0.2720(2) 0.0196(10) Uani 1 1 d . . . C307 C 0.6375(3) 0.8205(3) 0.3435(2) 0.0242(10) Uani 1 1 d . . . H30C H 0.5796 0.8017 0.3614 0.029 Uiso 1 1 calc R . . C308 C 0.7235(3) 0.8235(3) 0.3866(2) 0.0294(11) Uani 1 1 d . . . H30D H 0.7244 0.8062 0.4339 0.035 Uiso 1 1 calc R . . C309 C 0.8112(4) 0.8519(3) 0.3622(3) 0.0337(12) Uani 1 1 d . . . H30E H 0.8704 0.8550 0.3929 0.040 Uiso 1 1 calc R . . C310 C 0.8095(3) 0.8746(3) 0.2945(3) 0.0295(11) Uani 1 1 d . . . H31A H 0.8688 0.8923 0.2779 0.035 Uiso 1 1 calc R . . C311 C 0.7219(3) 0.8728(3) 0.2472(2) 0.0209(10) Uani 1 1 d . . . C312 C 0.7199(3) 0.8995(3) 0.1782(2) 0.0229(10) Uani 1 1 d . . . H31B H 0.7789 0.9190 0.1620 0.028 Uiso 1 1 calc R . . C313 C 0.6341(3) 0.8983(3) 0.1322(2) 0.0203(10) Uani 1 1 d . . . C314 C 0.6326(3) 0.9262(3) 0.0615(2) 0.0248(10) Uani 1 1 d . . . H314 H 0.6918 0.9459 0.0457 0.030 Uiso 1 1 calc R . . C315 C 0.5498(4) 0.9254(3) 0.0167(2) 0.0284(11) Uani 1 1 d . . . H315 H 0.5507 0.9454 -0.0298 0.034 Uiso 1 1 calc R . . C316 C 0.4610(3) 0.8945(3) 0.0393(2) 0.0268(11) Uani 1 1 d . . . H316 H 0.4028 0.8926 0.0075 0.032 Uiso 1 1 calc R . . C317 C 0.4588(3) 0.8676(3) 0.1061(2) 0.0232(10) Uani 1 1 d . . . H317 H 0.3989 0.8467 0.1200 0.028 Uiso 1 1 calc R . . C318 C 0.5438(3) 0.8697(3) 0.1558(2) 0.0184(9) Uani 1 1 d . . . H302 H 0.167(3) 0.913(3) 0.220(2) 0.022 Uiso 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 B3 0.024(3) 0.024(3) 0.024(3) -0.005(2) -0.007(2) -0.002(2) B4 0.037(3) 0.022(3) 0.023(3) -0.008(2) -0.003(2) 0.003(2) B5 0.025(3) 0.026(3) 0.023(3) -0.006(2) 0.003(2) -0.008(2) B6 0.029(3) 0.032(3) 0.024(3) -0.001(2) 0.007(2) 0.003(2) B7 0.020(3) 0.034(3) 0.017(3) -0.005(2) 0.001(2) -0.007(2) B8 0.018(3) 0.033(3) 0.028(3) -0.008(2) 0.000(2) -0.005(2) B9 0.020(3) 0.032(3) 0.020(3) -0.006(2) 0.000(2) -0.005(2) B10 0.018(3) 0.026(3) 0.025(3) -0.001(2) 0.001(2) -0.010(2) B11 0.028(3) 0.027(3) 0.015(2) 0.006(2) 0.000(2) 0.004(2) B12 0.020(3) 0.040(3) 0.010(2) -0.002(2) 0.0031(19) -0.006(2) C1 0.042(3) 0.022(3) 0.015(2) -0.0027(19) -0.003(2) -0.006(2) C2 0.039(3) 0.021(3) 0.017(2) -0.0017(19) 0.004(2) -0.001(2) C3 0.111(5) 0.012(3) 0.015(2) -0.003(2) 0.018(3) -0.014(3) C4 0.142(6) 0.018(3) 0.026(3) -0.001(2) 0.037(3) -0.002(3) C5 0.057(4) 0.013(2) 0.012(2) -0.0021(17) 0.011(2) -0.002(2) C6 0.039(3) 0.015(2) 0.020(2) -0.0031(18) 0.002(2) -0.003(2) C7 0.057(4) 0.022(3) 0.024(3) -0.003(2) 0.002(2) 0.008(3) C8 0.042(3) 0.027(3) 0.044(3) -0.005(2) -0.012(2) 0.006(3) C9 0.033(3) 0.021(3) 0.055(4) -0.006(2) 0.000(2) -0.003(2) C10 0.034(3) 0.019(3) 0.030(3) -0.0035(19) 0.010(2) -0.004(2) C11 0.039(3) 0.012(2) 0.021(3) -0.0026(18) 0.010(2) -0.001(2) C12 0.040(3) 0.015(2) 0.017(2) -0.0009(18) 0.011(2) 0.003(2) C13 0.038(3) 0.011(2) 0.027(3) -0.0004(18) 0.009(2) 0.001(2) C14 0.042(3) 0.021(3) 0.027(3) 0.007(2) 0.005(2) -0.002(2) C15 0.036(3) 0.027(3) 0.057(4) 0.007(2) 0.003(3) -0.001(2) C16 0.034(3) 0.020(3) 0.079(4) -0.003(3) 0.025(3) -0.005(2) C17 0.054(4) 0.021(3) 0.039(3) -0.007(2) 0.030(3) -0.010(2) C18 0.047(3) 0.011(2) 0.025(3) -0.0017(18) 0.020(2) -0.001(2) B103 0.018(3) 0.036(3) 0.021(3) 0.001(2) -0.002(2) 0.011(2) B104 0.023(3) 0.030(3) 0.018(3) 0.007(2) -0.001(2) 0.008(2) B105 0.022(3) 0.025(3) 0.020(3) 0.002(2) 0.003(2) 0.000(2) B106 0.024(3) 0.030(3) 0.033(3) 0.004(2) -0.002(2) -0.002(2) B107 0.017(3) 0.021(3) 0.023(3) 0.005(2) -0.005(2) 0.004(2) B108 0.026(3) 0.020(3) 0.026(3) 0.002(2) -0.003(2) -0.001(2) B109 0.016(2) 0.029(3) 0.019(3) 0.004(2) 0.0052(19) -0.002(2) B110 0.023(3) 0.028(3) 0.022(3) -0.004(2) -0.005(2) 0.005(2) B111 0.014(2) 0.024(3) 0.026(3) 0.002(2) 0.002(2) 0.006(2) B112 0.011(2) 0.038(3) 0.021(3) 0.000(2) 0.0009(19) -0.002(2) C101 0.013(2) 0.039(3) 0.025(2) 0.011(2) 0.0022(18) 0.003(2) C102 0.016(2) 0.030(3) 0.023(2) 0.010(2) 0.0001(18) -0.001(2) C103 0.023(3) 0.064(4) 0.020(2) 0.012(2) 0.0041(19) 0.002(3) C104 0.024(3) 0.048(3) 0.015(2) -0.009(2) 0.0015(18) -0.008(2) C105 0.026(2) 0.017(3) 0.028(3) -0.0080(19) 0.0122(19) -0.0067(19) C106 0.021(2) 0.015(2) 0.033(3) -0.0047(19) 0.009(2) -0.0021(18) C107 0.023(2) 0.026(3) 0.036(3) -0.001(2) 0.009(2) 0.003(2) C108 0.029(3) 0.025(3) 0.028(3) 0.001(2) 0.001(2) 0.006(2) C109 0.024(3) 0.033(3) 0.042(3) -0.005(2) 0.002(2) 0.005(2) C110 0.021(3) 0.023(3) 0.047(3) -0.004(2) 0.008(2) 0.003(2) C111 0.026(3) 0.011(2) 0.036(3) -0.0082(19) 0.010(2) 0.0045(19) C112 0.021(2) 0.019(3) 0.039(3) -0.004(2) 0.013(2) 0.0002(19) C113 0.027(3) 0.013(2) 0.032(3) -0.0013(19) 0.013(2) -0.0013(19) C114 0.033(3) 0.015(3) 0.040(3) -0.004(2) 0.018(2) -0.004(2) C115 0.042(3) 0.026(3) 0.024(3) -0.005(2) 0.014(2) -0.004(2) C116 0.029(3) 0.053(4) 0.028(3) -0.009(2) 0.003(2) -0.006(2) C117 0.026(3) 0.045(3) 0.028(3) -0.007(2) 0.012(2) -0.005(2) C118 0.024(2) 0.016(2) 0.027(3) -0.0098(18) 0.0077(19) -0.0050(19) B203 0.029(3) 0.041(4) 0.031(3) -0.012(3) 0.003(2) -0.001(3) B204 0.027(3) 0.036(4) 0.025(3) -0.012(2) 0.004(2) 0.002(3) B205 0.026(3) 0.033(3) 0.022(3) 0.006(2) -0.004(2) 0.002(2) B206 0.030(3) 0.028(3) 0.032(3) 0.009(2) 0.002(2) 0.009(3) B207 0.037(3) 0.032(3) 0.012(2) -0.003(2) 0.007(2) 0.000(3) B208 0.028(3) 0.024(3) 0.034(3) 0.002(2) -0.003(2) 0.001(2) B209 0.025(3) 0.025(3) 0.019(3) 0.005(2) -0.003(2) -0.001(2) B210 0.030(3) 0.022(3) 0.025(3) 0.000(2) 0.004(2) 0.004(2) B211 0.025(3) 0.037(3) 0.016(3) -0.002(2) 0.005(2) 0.008(2) B212 0.029(3) 0.024(3) 0.019(3) -0.003(2) 0.001(2) -0.001(2) C201 0.022(2) 0.042(3) 0.019(2) 0.002(2) 0.0022(19) 0.000(2) C202 0.019(2) 0.052(4) 0.013(2) 0.001(2) -0.0036(19) 0.006(2) C203 0.035(3) 0.047(4) 0.029(3) 0.003(2) 0.002(2) 0.002(2) C204 0.027(3) 0.041(3) 0.026(3) 0.000(2) 0.001(2) -0.004(2) C205 0.024(3) 0.018(2) 0.016(2) -0.0025(17) 0.0049(19) 0.0000(19) C206 0.025(2) 0.012(2) 0.023(2) -0.0031(18) 0.0061(19) 0.0034(19) C207 0.030(3) 0.028(3) 0.027(3) 0.005(2) -0.002(2) 0.000(2) C208 0.023(3) 0.027(3) 0.044(3) 0.003(2) 0.002(2) -0.001(2) C209 0.031(3) 0.021(3) 0.042(3) 0.002(2) 0.023(2) 0.002(2) C210 0.036(3) 0.017(3) 0.025(3) -0.0027(18) 0.012(2) -0.005(2) C211 0.030(3) 0.012(2) 0.022(2) -0.0055(17) 0.0095(19) -0.0004(19) C212 0.034(3) 0.016(2) 0.013(2) 0.0031(17) 0.0048(19) -0.007(2) C213 0.030(3) 0.011(2) 0.019(2) -0.0023(17) 0.0023(19) -0.0060(19) C214 0.040(3) 0.034(3) 0.029(3) 0.005(2) -0.003(2) -0.009(2) C215 0.021(2) 0.029(3) 0.037(3) 0.001(2) -0.007(2) -0.004(2) C216 0.025(3) 0.023(3) 0.035(3) -0.013(2) 0.007(2) -0.005(2) C217 0.026(3) 0.028(3) 0.024(2) -0.007(2) 0.008(2) -0.002(2) C218 0.022(2) 0.014(2) 0.019(2) -0.0057(17) 0.0047(18) 0.0007(18) B303 0.011(2) 0.019(3) 0.020(2) -0.005(2) -0.0019(18) -0.0013(19) B304 0.018(2) 0.024(3) 0.012(2) -0.0039(19) -0.0037(19) 0.003(2) B305 0.018(2) 0.021(3) 0.015(2) 0.0013(19) 0.0053(18) 0.001(2) B306 0.017(2) 0.017(3) 0.020(3) 0.000(2) 0.0000(19) -0.002(2) B307 0.018(3) 0.026(3) 0.020(3) 0.001(2) 0.008(2) 0.004(2) B308 0.021(3) 0.020(3) 0.023(3) -0.002(2) 0.005(2) 0.004(2) B309 0.021(3) 0.023(3) 0.015(2) 0.007(2) 0.005(2) 0.005(2) B310 0.020(2) 0.014(3) 0.022(3) 0.002(2) 0.002(2) -0.001(2) B311 0.012(2) 0.022(3) 0.023(3) -0.002(2) -0.0008(19) -0.006(2) B312 0.019(3) 0.023(3) 0.021(3) 0.001(2) 0.009(2) 0.005(2) C301 0.017(2) 0.014(2) 0.010(2) 0.0006(15) 0.0009(16) 0.0008(17) C302 0.017(2) 0.020(2) 0.012(2) 0.0011(17) -0.0019(17) -0.0007(18) C303 0.017(2) 0.015(2) 0.017(2) 0.0018(16) 0.0029(16) -0.0009(17) C304 0.028(2) 0.013(2) 0.024(2) -0.0020(17) 0.0112(18) -0.0019(19) C305 0.020(2) 0.008(2) 0.027(2) 0.0012(17) 0.0101(19) 0.0016(17) C306 0.020(2) 0.013(2) 0.027(2) -0.0055(17) 0.0080(19) 0.0016(18) C307 0.028(3) 0.019(3) 0.029(3) 0.0035(19) 0.015(2) 0.001(2) C308 0.025(3) 0.035(3) 0.028(3) 0.003(2) 0.004(2) 0.006(2) C309 0.024(3) 0.037(3) 0.038(3) 0.004(2) 0.000(2) 0.004(2) C310 0.016(2) 0.025(3) 0.048(3) -0.003(2) 0.009(2) -0.001(2) C311 0.020(2) 0.016(2) 0.029(3) 0.0007(18) 0.0102(19) 0.0010(18) C312 0.020(2) 0.018(3) 0.033(3) -0.0020(19) 0.013(2) -0.0036(19) C313 0.029(3) 0.007(2) 0.027(2) -0.0048(18) 0.015(2) -0.0011(19) C314 0.032(3) 0.016(3) 0.030(3) 0.0035(19) 0.021(2) -0.003(2) C315 0.044(3) 0.018(3) 0.025(3) -0.0004(19) 0.012(2) -0.001(2) C316 0.035(3) 0.027(3) 0.020(2) -0.002(2) 0.009(2) 0.000(2) C317 0.026(3) 0.018(3) 0.029(3) -0.0080(19) 0.012(2) -0.001(2) C318 0.019(2) 0.010(2) 0.028(2) -0.0017(17) 0.0089(19) 0.0012(18) _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 B3 C2 1.707(7) . ? B3 C1 1.718(7) . ? B3 B8 1.747(7) . ? B3 B7 1.750(7) . ? B3 B4 1.775(7) . ? B4 C1 1.700(7) . ? B4 B5 1.774(7) . ? B4 B9 1.781(7) . ? B4 B8 1.784(8) . ? B5 C1 1.703(7) . ? B5 B6 1.764(8) . ? B5 B9 1.769(7) . ? B5 B10 1.771(7) . ? B6 C2 1.709(7) . ? B6 C1 1.730(7) . ? B6 B10 1.750(7) . ? B6 B11 1.770(7) . ? B7 C2 1.696(6) . ? B7 B12 1.772(7) . ? B7 B8 1.778(8) . ? B7 B11 1.784(7) . ? B8 B12 1.781(8) . ? B8 B9 1.797(7) . ? B9 B12 1.784(8) . ? B9 B10 1.790(8) . ? B10 B11 1.785(7) . ? B10 B12 1.809(7) . ? B11 C2 1.692(6) . ? B11 B12 1.779(7) . ? C1 C3 1.497(6) . ? C1 C2 1.639(6) . ? C3 C4 1.188(6) . ? C4 C5 1.493(6) . ? C5 C6 1.397(6) . ? C5 C18 1.399(7) . ? C6 C7 1.421(7) . ? C6 C11 1.444(6) . ? C7 C8 1.364(7) . ? C8 C9 1.403(7) . ? C9 C10 1.360(7) . ? C10 C11 1.424(6) . ? C11 C12 1.388(6) . ? C12 C13 1.394(6) . ? C13 C14 1.415(7) . ? C13 C18 1.450(6) . ? C14 C15 1.353(7) . ? C15 C16 1.424(7) . ? C16 C17 1.346(7) . ? C17 C18 1.426(7) . ? B103 C102 1.695(7) . ? B103 C101 1.720(7) . ? B103 B108 1.740(7) . ? B103 B107 1.755(6) . ? B103 B104 1.766(6) . ? B104 C101 1.676(7) . ? B104 B109 1.764(7) . ? B104 B105 1.766(7) . ? B104 B108 1.772(7) . ? B105 C101 1.704(6) . ? B105 B110 1.767(7) . ? B105 B106 1.769(7) . ? B105 B109 1.778(7) . ? B106 C102 1.708(7) . ? B106 C101 1.723(7) . ? B106 B110 1.777(8) . ? B106 B111 1.787(7) . ? B107 C102 1.679(6) . ? B107 B108 1.769(7) . ? B107 B111 1.774(7) . ? B107 B112 1.781(7) . ? B108 B112 1.783(7) . ? B108 B109 1.789(7) . ? B109 B110 1.776(7) . ? B109 B112 1.776(7) . ? B110 B112 1.783(7) . ? B110 B111 1.794(7) . ? B111 C102 1.695(7) . ? B111 B112 1.777(7) . ? C101 C103 1.508(6) . ? C101 C102 1.655(6) . ? C103 C104 1.277(6) . ? C104 C105 1.489(6) . ? C105 C118 1.409(6) . ? C105 C106 1.420(6) . ? C106 C107 1.422(6) . ? C106 C111 1.425(6) . ? C107 C108 1.359(6) . ? C108 C109 1.400(6) . ? C109 C110 1.347(6) . ? C110 C111 1.439(6) . ? C111 C112 1.389(6) . ? C112 C113 1.386(6) . ? C113 C114 1.414(6) . ? C113 C118 1.440(6) . ? C114 C115 1.364(6) . ? C115 C116 1.396(6) . ? C116 C117 1.362(6) . ? C117 C118 1.424(6) . ? B203 C202 1.709(8) . ? B203 C201 1.735(8) . ? B203 B204 1.769(8) . ? B203 B208 1.778(8) . ? B203 B207 1.784(7) . ? B204 C201 1.700(7) . ? B204 B205 1.762(8) . ? B204 B209 1.774(7) . ? B204 B208 1.798(8) . ? B205 C201 1.697(7) . ? B205 B206 1.771(7) . ? B205 B209 1.776(7) . ? B205 B210 1.783(7) . ? B206 C202 1.723(8) . ? B206 C201 1.724(7) . ? B206 B210 1.740(7) . ? B206 B211 1.748(7) . ? B207 C202 1.692(7) . ? B207 B208 1.771(8) . ? B207 B212 1.775(7) . ? B207 B211 1.787(8) . ? B208 B212 1.769(7) . ? B208 B209 1.775(7) . ? B209 B212 1.775(7) . ? B209 B210 1.780(7) . ? B210 B211 1.777(8) . ? B210 B212 1.785(7) . ? B211 C202 1.670(7) . ? B211 B212 1.775(7) . ? C201 C203 1.496(6) . ? C201 C202 1.654(6) . ? C203 C204 1.263(6) . ? C204 C205 1.493(6) . ? C205 C218 1.405(6) . ? C205 C206 1.411(6) . ? C206 C211 1.426(6) . ? C206 C207 1.436(6) . ? C207 C208 1.356(6) . ? C208 C209 1.401(7) . ? C209 C210 1.341(6) . ? C210 C211 1.428(6) . ? C211 C212 1.386(6) . ? C212 C213 1.382(6) . ? C213 C214 1.444(6) . ? C213 C218 1.444(6) . ? C214 C215 1.348(7) . ? C215 C216 1.400(6) . ? C216 C217 1.344(6) . ? C217 C218 1.433(6) . ? B303 C302 1.704(6) . ? B303 C301 1.728(6) . ? B303 B308 1.754(7) . ? B303 B304 1.774(7) . ? B303 B307 1.781(6) . ? B304 C301 1.707(6) . ? B304 B309 1.755(7) . ? B304 B305 1.772(7) . ? B304 B308 1.773(7) . ? B305 C301 1.708(6) . ? B305 B309 1.772(6) . ? B305 B306 1.787(6) . ? B305 B310 1.788(6) . ? B306 C302 1.710(6) . ? B306 C301 1.746(6) . ? B306 B311 1.777(6) . ? B306 B310 1.783(6) . ? B307 C302 1.707(6) . ? B307 B312 1.773(7) . ? B307 B308 1.787(7) . ? B307 B311 1.801(7) . ? B308 B309 1.770(7) . ? B308 B312 1.785(7) . ? B309 B312 1.768(7) . ? B309 B310 1.777(7) . ? B310 B311 1.781(7) . ? B310 B312 1.793(7) . ? B311 C302 1.695(6) . ? B311 B312 1.782(7) . ? C301 C303 1.483(5) . ? C301 C302 1.642(6) . ? C303 C304 1.325(6) . ? C304 C305 1.485(5) . ? C305 C318 1.413(6) . ? C305 C306 1.414(6) . ? C306 C307 1.427(6) . ? C306 C311 1.434(6) . ? C307 C308 1.365(6) . ? C308 C309 1.414(6) . ? C309 C310 1.354(6) . ? C310 C311 1.424(6) . ? C311 C312 1.391(6) . ? C312 C313 1.392(6) . ? C313 C314 1.429(6) . ? C313 C318 1.439(6) . ? C314 C315 1.347(6) . ? C315 C316 1.423(6) . ? C316 C317 1.358(6) . ? C317 C318 1.424(6) . ? 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 B3 C1 57.2(3) . . ? C2 B3 B8 105.5(4) . . ? C1 B3 B8 105.7(3) . . ? C2 B3 B7 58.7(3) . . ? C1 B3 B7 105.6(4) . . ? B8 B3 B7 61.1(3) . . ? C2 B3 B4 104.4(4) . . ? C1 B3 B4 58.2(3) . . ? B8 B3 B4 60.9(3) . . ? B7 B3 B4 109.4(4) . . ? C1 B4 B5 58.7(3) . . ? C1 B4 B3 59.2(3) . . ? B5 B4 B3 107.7(4) . . ? C1 B4 B9 104.7(4) . . ? B5 B4 B9 59.7(3) . . ? B3 B4 B9 107.1(4) . . ? C1 B4 B8 104.8(4) . . ? B5 B4 B8 108.1(4) . . ? B3 B4 B8 58.8(3) . . ? B9 B4 B8 60.5(3) . . ? C1 B5 B6 59.8(3) . . ? C1 B5 B9 105.1(4) . . ? B6 B5 B9 108.1(4) . . ? C1 B5 B10 105.6(4) . . ? B6 B5 B10 59.3(3) . . ? B9 B5 B10 60.7(3) . . ? C1 B5 B4 58.5(3) . . ? B6 B5 B4 108.8(4) . . ? B9 B5 B4 60.4(3) . . ? B10 B5 B4 109.2(4) . . ? C2 B6 C1 56.9(3) . . ? C2 B6 B10 105.1(3) . . ? C1 B6 B10 105.4(4) . . ? C2 B6 B5 104.0(4) . . ? C1 B6 B5 58.3(3) . . ? B10 B6 B5 60.5(3) . . ? C2 B6 B11 58.2(3) . . ? C1 B6 B11 104.6(3) . . ? B10 B6 B11 61.0(3) . . ? B5 B6 B11 108.6(4) . . ? C2 B7 B3 59.4(3) . . ? C2 B7 B12 104.1(3) . . ? B3 B7 B12 107.6(4) . . ? C2 B7 B8 104.6(4) . . ? B3 B7 B8 59.4(3) . . ? B12 B7 B8 60.2(3) . . ? C2 B7 B11 58.1(3) . . ? B3 B7 B11 108.2(4) . . ? B12 B7 B11 60.1(3) . . ? B8 B7 B11 108.3(4) . . ? B3 B8 B7 59.5(3) . . ? B3 B8 B12 107.3(4) . . ? B7 B8 B12 59.7(3) . . ? B3 B8 B4 60.3(3) . . ? B7 B8 B4 107.8(3) . . ? B12 B8 B4 107.6(4) . . ? B3 B8 B9 107.6(4) . . ? B7 B8 B9 107.4(4) . . ? B12 B8 B9 59.8(3) . . ? B4 B8 B9 59.7(3) . . ? B5 B9 B4 60.0(3) . . ? B5 B9 B12 107.9(4) . . ? B4 B9 B12 107.6(4) . . ? B5 B9 B10 59.7(3) . . ? B4 B9 B10 108.0(3) . . ? B12 B9 B10 60.8(3) . . ? B5 B9 B8 107.7(3) . . ? B4 B9 B8 59.8(3) . . ? B12 B9 B8 59.6(3) . . ? B10 B9 B8 108.5(4) . . ? B6 B10 B5 60.2(3) . . ? B6 B10 B11 60.1(3) . . ? B5 B10 B11 107.6(3) . . ? B6 B10 B9 107.8(4) . . ? B5 B10 B9 59.6(3) . . ? B11 B10 B9 107.2(3) . . ? B6 B10 B12 107.3(3) . . ? B5 B10 B12 106.7(4) . . ? B11 B10 B12 59.3(3) . . ? B9 B10 B12 59.4(3) . . ? C2 B11 B6 59.1(3) . . ? C2 B11 B12 103.9(3) . . ? B6 B11 B12 107.7(4) . . ? C2 B11 B7 58.3(3) . . ? B6 B11 B7 108.1(4) . . ? B12 B11 B7 59.6(3) . . ? C2 B11 B10 104.3(4) . . ? B6 B11 B10 59.0(3) . . ? B12 B11 B10 61.0(3) . . ? B7 B11 B10 108.6(4) . . ? B7 B12 B11 60.3(3) . . ? B7 B12 B8 60.1(3) . . ? B11 B12 B8 108.4(3) . . ? B7 B12 B9 108.3(4) . . ? B11 B12 B9 107.7(3) . . ? B8 B12 B9 60.6(3) . . ? B7 B12 B10 108.0(3) . . ? B11 B12 B10 59.7(3) . . ? B8 B12 B10 108.4(4) . . ? B9 B12 B10 59.7(3) . . ? C3 C1 C2 119.3(4) . . ? C3 C1 B4 119.6(4) . . ? C2 C1 B4 110.9(4) . . ? C3 C1 B5 121.4(4) . . ? C2 C1 B5 110.0(4) . . ? B4 C1 B5 62.8(3) . . ? C3 C1 B3 116.5(4) . . ? C2 C1 B3 61.1(3) . . ? B4 C1 B3 62.6(3) . . ? B5 C1 B3 113.8(3) . . ? C3 C1 B6 118.5(4) . . ? C2 C1 B6 60.9(3) . . ? B4 C1 B6 114.0(3) . . ? B5 C1 B6 61.8(3) . . ? B3 C1 B6 113.4(3) . . ? C1 C2 B11 112.5(4) . . ? C1 C2 B7 111.9(4) . . ? B11 C2 B7 63.5(3) . . ? C1 C2 B3 61.8(3) . . ? B11 C2 B3 114.8(3) . . ? B7 C2 B3 61.9(3) . . ? C1 C2 B6 62.2(3) . . ? B11 C2 B6 62.7(3) . . ? B7 C2 B6 115.4(3) . . ? B3 C2 B6 115.1(4) . . ? C4 C3 C1 133.0(5) . . ? C3 C4 C5 130.4(5) . . ? C6 C5 C18 121.4(4) . . ? C6 C5 C4 119.9(5) . . ? C18 C5 C4 118.7(5) . . ? C5 C6 C7 124.1(4) . . ? C5 C6 C11 118.9(4) . . ? C7 C6 C11 117.0(4) . . ? C8 C7 C6 122.1(5) . . ? C7 C8 C9 120.5(5) . . ? C10 C9 C8 120.1(5) . . ? C9 C10 C11 121.4(5) . . ? C12 C11 C10 121.3(4) . . ? C12 C11 C6 119.8(4) . . ? C10 C11 C6 118.9(4) . . ? C11 C12 C13 121.7(4) . . ? C12 C13 C14 121.5(4) . . ? C12 C13 C18 118.8(4) . . ? C14 C13 C18 119.7(4) . . ? C15 C14 C13 121.6(5) . . ? C14 C15 C16 119.5(5) . . ? C17 C16 C15 120.5(5) . . ? C16 C17 C18 122.9(5) . . ? C5 C18 C17 124.7(4) . . ? C5 C18 C13 119.4(4) . . ? C17 C18 C13 115.8(5) . . ? C102 B103 C101 58.0(3) . . ? C102 B103 B108 104.9(4) . . ? C101 B103 B108 105.4(3) . . ? C102 B103 B107 58.2(3) . . ? C101 B103 B107 105.7(4) . . ? B108 B103 B107 60.8(3) . . ? C102 B103 B104 103.9(4) . . ? C101 B103 B104 57.5(3) . . ? B108 B103 B104 60.7(3) . . ? B107 B103 B104 108.7(3) . . ? C101 B104 B109 106.2(4) . . ? C101 B104 B103 59.9(3) . . ? B109 B104 B103 108.1(3) . . ? C101 B104 B105 59.3(3) . . ? B109 B104 B105 60.5(3) . . ? B103 B104 B105 109.0(4) . . ? C101 B104 B108 105.8(3) . . ? B109 B104 B108 60.8(3) . . ? B103 B104 B108 58.9(3) . . ? B105 B104 B108 109.1(4) . . ? C101 B105 B104 57.7(3) . . ? C101 B105 B110 105.7(3) . . ? B104 B105 B110 107.7(4) . . ? C101 B105 B106 59.5(3) . . ? B104 B105 B106 107.4(4) . . ? B110 B105 B106 60.3(3) . . ? C101 B105 B109 104.4(3) . . ? B104 B105 B109 59.7(3) . . ? B110 B105 B109 60.1(3) . . ? B106 B105 B109 108.1(4) . . ? C102 B106 C101 57.7(3) . . ? C102 B106 B105 104.4(4) . . ? C101 B106 B105 58.4(3) . . ? C102 B106 B110 104.0(4) . . ? C101 B106 B110 104.5(4) . . ? B105 B106 B110 59.8(3) . . ? C102 B106 B111 58.0(3) . . ? C101 B106 B111 105.0(4) . . ? B105 B106 B111 108.3(4) . . ? B110 B106 B111 60.4(3) . . ? C102 B107 B103 59.1(3) . . ? C102 B107 B108 104.3(3) . . ? B103 B107 B108 59.2(3) . . ? C102 B107 B111 58.7(3) . . ? B103 B107 B111 108.6(4) . . ? B108 B107 B111 108.5(3) . . ? C102 B107 B112 104.2(3) . . ? B103 B107 B112 107.6(3) . . ? B108 B107 B112 60.3(3) . . ? B111 B107 B112 60.0(3) . . ? B103 B108 B107 60.0(3) . . ? B103 B108 B104 60.4(3) . . ? B107 B108 B104 107.8(4) . . ? B103 B108 B112 108.1(4) . . ? B107 B108 B112 60.2(3) . . ? B104 B108 B112 107.0(4) . . ? B103 B108 B109 108.1(4) . . ? B107 B108 B109 107.9(4) . . ? B104 B108 B109 59.4(3) . . ? B112 B108 B109 59.6(3) . . ? B104 B109 B110 107.5(4) . . ? B104 B109 B112 107.7(3) . . ? B110 B109 B112 60.3(3) . . ? B104 B109 B105 59.8(3) . . ? B110 B109 B105 59.6(3) . . ? B112 B109 B105 107.9(4) . . ? B104 B109 B108 59.8(3) . . ? B110 B109 B108 108.1(4) . . ? B112 B109 B108 60.0(3) . . ? B105 B109 B108 107.9(3) . . ? B105 B110 B109 60.3(3) . . ? B105 B110 B106 59.9(3) . . ? B109 B110 B106 107.8(4) . . ? B105 B110 B112 108.1(4) . . ? B109 B110 B112 59.9(3) . . ? B106 B110 B112 107.6(4) . . ? B105 B110 B111 108.0(4) . . ? B109 B110 B111 107.6(4) . . ? B106 B110 B111 60.1(3) . . ? B112 B110 B111 59.6(3) . . ? C102 B111 B107 57.8(3) . . ? C102 B111 B112 103.7(4) . . ? B107 B111 B112 60.2(3) . . ? C102 B111 B106 58.7(3) . . ? B107 B111 B106 107.5(4) . . ? B112 B111 B106 107.4(4) . . ? C102 B111 B110 103.9(3) . . ? B107 B111 B110 107.9(4) . . ? B112 B111 B110 59.9(3) . . ? B106 B111 B110 59.5(3) . . ? B109 B112 B111 108.4(3) . . ? B109 B112 B107 107.9(3) . . ? B111 B112 B107 59.8(3) . . ? B109 B112 B110 59.9(3) . . ? B111 B112 B110 60.5(3) . . ? B107 B112 B110 108.1(3) . . ? B109 B112 B108 60.4(3) . . ? B111 B112 B108 107.7(3) . . ? B107 B112 B108 59.5(3) . . ? B110 B112 B108 108.0(3) . . ? C103 C101 C102 120.2(3) . . ? C103 C101 B104 118.6(4) . . ? C102 C101 B104 109.8(3) . . ? C103 C101 B105 122.0(4) . . ? C102 C101 B105 109.8(3) . . ? B104 C101 B105 63.0(3) . . ? C103 C101 B103 114.9(4) . . ? C102 C101 B103 60.3(3) . . ? B104 C101 B103 62.6(3) . . ? B105 C101 B103 114.3(3) . . ? C103 C101 B106 120.2(4) . . ? C102 C101 B106 60.7(3) . . ? B104 C101 B106 113.9(3) . . ? B105 C101 B106 62.2(3) . . ? B103 C101 B106 113.0(3) . . ? C101 C102 B107 112.3(3) . . ? C101 C102 B111 112.5(3) . . ? B107 C102 B111 63.4(3) . . ? C101 C102 B103 61.8(3) . . ? B107 C102 B103 62.7(3) . . ? B111 C102 B103 115.4(3) . . ? C101 C102 B106 61.6(3) . . ? B107 C102 B106 116.0(4) . . ? B111 C102 B106 63.3(3) . . ? B103 C102 B106 115.0(4) . . ? C104 C103 C101 123.2(5) . . ? C103 C104 C105 130.9(4) . . ? C118 C105 C106 120.8(4) . . ? C118 C105 C104 121.5(4) . . ? C106 C105 C104 117.6(4) . . ? C105 C106 C107 123.3(4) . . ? C105 C106 C111 119.1(4) . . ? C107 C106 C111 117.7(4) . . ? C108 C107 C106 121.3(4) . . ? C107 C108 C109 121.5(4) . . ? C110 C109 C108 119.4(5) . . ? C109 C110 C111 121.7(4) . . ? C112 C111 C106 119.7(4) . . ? C112 C111 C110 121.8(4) . . ? C106 C111 C110 118.5(4) . . ? C113 C112 C111 122.1(4) . . ? C112 C113 C114 121.8(4) . . ? C112 C113 C118 119.5(4) . . ? C114 C113 C118 118.7(4) . . ? C115 C114 C113 121.9(4) . . ? C114 C115 C116 119.4(4) . . ? C117 C116 C115 120.9(5) . . ? C116 C117 C118 121.8(4) . . ? C105 C118 C117 124.2(4) . . ? C105 C118 C113 118.8(4) . . ? C117 C118 C113 116.9(4) . . ? C202 B203 C201 57.4(3) . . ? C202 B203 B204 103.8(4) . . ? C201 B203 B204 58.0(3) . . ? C202 B203 B208 103.3(4) . . ? C201 B203 B208 104.9(4) . . ? B204 B203 B208 60.9(3) . . ? C202 B203 B207 57.9(3) . . ? C201 B203 B207 105.0(4) . . ? B204 B203 B207 108.4(4) . . ? B208 B203 B207 59.6(3) . . ? C201 B204 B205 58.7(3) . . ? C201 B204 B203 60.0(3) . . ? B205 B204 B203 109.0(4) . . ? C201 B204 B209 105.0(4) . . ? B205 B204 B209 60.3(3) . . ? B203 B204 B209 107.8(4) . . ? C201 B204 B208 105.5(3) . . ? B205 B204 B208 108.3(4) . . ? B203 B204 B208 59.8(3) . . ? B209 B204 B208 59.6(3) . . ? C201 B205 B204 58.9(3) . . ? C201 B205 B206 59.6(3) . . ? B204 B205 B206 108.2(4) . . ? C201 B205 B209 105.0(4) . . ? B204 B205 B209 60.2(3) . . ? B206 B205 B209 106.8(4) . . ? C201 B205 B210 104.9(4) . . ? B204 B205 B210 108.2(4) . . ? B206 B205 B210 58.6(3) . . ? B209 B205 B210 60.0(3) . . ? C202 B206 C201 57.4(3) . . ? C202 B206 B210 104.6(4) . . ? C201 B206 B210 105.7(4) . . ? C202 B206 B211 57.5(3) . . ? C201 B206 B211 105.0(4) . . ? B210 B206 B211 61.3(3) . . ? C202 B206 B205 104.0(4) . . ? C201 B206 B205 58.1(3) . . ? B210 B206 B205 61.0(3) . . ? B211 B206 B205 109.3(4) . . ? C202 B207 B208 104.3(4) . . ? C202 B207 B212 103.3(4) . . ? B208 B207 B212 59.9(3) . . ? C202 B207 B203 58.8(3) . . ? B208 B207 B203 60.0(3) . . ? B212 B207 B203 107.5(4) . . ? C202 B207 B211 57.3(3) . . ? B208 B207 B211 107.5(4) . . ? B212 B207 B211 59.8(3) . . ? B203 B207 B211 107.0(4) . . ? B212 B208 B207 60.2(3) . . ? B212 B208 B209 60.1(3) . . ? B207 B208 B209 108.3(4) . . ? B212 B208 B203 108.0(4) . . ? B207 B208 B203 60.4(3) . . ? B209 B208 B203 107.4(4) . . ? B212 B208 B204 107.4(4) . . ? B207 B208 B204 107.7(4) . . ? B209 B208 B204 59.5(3) . . ? B203 B208 B204 59.3(3) . . ? B204 B209 B208 60.9(3) . . ? B204 B209 B212 108.2(4) . . ? B208 B209 B212 59.8(3) . . ? B204 B209 B205 59.5(3) . . ? B208 B209 B205 108.7(4) . . ? B212 B209 B205 108.4(4) . . ? B204 B209 B210 107.8(4) . . ? B208 B209 B210 108.4(4) . . ? B212 B209 B210 60.3(3) . . ? B205 B209 B210 60.2(3) . . ? B206 B210 B211 59.6(3) . . ? B206 B210 B209 108.0(4) . . ? B211 B210 B209 107.3(4) . . ? B206 B210 B205 60.3(3) . . ? B211 B210 B205 107.5(4) . . ? B209 B210 B205 59.8(3) . . ? B206 B210 B212 107.8(4) . . ? B211 B210 B212 59.8(3) . . ? B209 B210 B212 59.7(3) . . ? B205 B210 B212 107.6(4) . . ? C202 B211 B206 60.5(3) . . ? C202 B211 B212 104.2(4) . . ? B206 B211 B212 107.9(4) . . ? C202 B211 B210 105.2(3) . . ? B206 B211 B210 59.1(3) . . ? B212 B211 B210 60.3(3) . . ? C202 B211 B207 58.5(3) . . ? B206 B211 B207 109.5(4) . . ? B212 B211 B207 59.8(3) . . ? B210 B211 B207 108.5(4) . . ? B208 B212 B207 60.0(3) . . ? B208 B212 B209 60.1(3) . . ? B207 B212 B209 108.1(3) . . ? B208 B212 B211 108.1(4) . . ? B207 B212 B211 60.4(3) . . ? B209 B212 B211 107.6(4) . . ? B208 B212 B210 108.5(4) . . ? B207 B212 B210 108.7(4) . . ? B209 B212 B210 60.0(3) . . ? B211 B212 B210 59.9(3) . . ? C203 C201 C202 115.5(4) . . ? C203 C201 B205 121.8(4) . . ? C202 C201 B205 110.4(3) . . ? C203 C201 B204 126.4(4) . . ? C202 C201 B204 109.4(4) . . ? B205 C201 B204 62.5(3) . . ? C203 C201 B206 113.0(4) . . ? C202 C201 B206 61.3(3) . . ? B205 C201 B206 62.3(3) . . ? B204 C201 B206 113.4(3) . . ? C203 C201 B203 119.0(4) . . ? C202 C201 B203 60.5(3) . . ? B205 C201 B203 113.8(4) . . ? B204 C201 B203 62.0(3) . . ? B206 C201 B203 113.5(4) . . ? C201 C202 B211 111.9(4) . . ? C201 C202 B207 113.0(4) . . ? B211 C202 B207 64.2(3) . . ? C201 C202 B203 62.1(3) . . ? B211 C202 B203 116.3(4) . . ? B207 C202 B203 63.3(3) . . ? C201 C202 B206 61.3(3) . . ? B211 C202 B206 62.0(3) . . ? B207 C202 B206 115.4(4) . . ? B203 C202 B206 114.9(4) . . ? C204 C203 C201 127.1(5) . . ? C203 C204 C205 126.2(5) . . ? C218 C205 C206 121.0(4) . . ? C218 C205 C204 120.7(4) . . ? C206 C205 C204 118.3(4) . . ? C205 C206 C211 119.3(4) . . ? C205 C206 C207 122.6(4) . . ? C211 C206 C207 118.1(4) . . ? C208 C207 C206 120.7(4) . . ? C207 C208 C209 120.4(5) . . ? C210 C209 C208 121.4(4) . . ? C209 C210 C211 120.8(4) . . ? C212 C211 C206 119.4(4) . . ? C212 C211 C210 122.0(4) . . ? C206 C211 C210 118.6(4) . . ? C213 C212 C211 122.1(4) . . ? C212 C213 C214 122.5(4) . . ? C212 C213 C218 119.6(4) . . ? C214 C213 C218 117.9(4) . . ? C215 C214 C213 121.3(4) . . ? C214 C215 C216 120.2(4) . . ? C217 C216 C215 121.6(4) . . ? C216 C217 C218 121.3(4) . . ? C205 C218 C217 123.9(4) . . ? C205 C218 C213 118.5(4) . . ? C217 C218 C213 117.5(4) . . ? C302 B303 C301 57.2(2) . . ? C302 B303 B308 104.5(3) . . ? C301 B303 B308 105.6(3) . . ? C302 B303 B304 103.6(3) . . ? C301 B303 B304 58.4(2) . . ? B308 B303 B304 60.3(3) . . ? C302 B303 B307 58.6(3) . . ? C301 B303 B307 105.9(3) . . ? B308 B303 B307 60.7(3) . . ? B304 B303 B307 108.7(3) . . ? C301 B304 B309 105.1(3) . . ? C301 B304 B305 58.8(2) . . ? B309 B304 B305 60.3(3) . . ? C301 B304 B308 105.6(3) . . ? B309 B304 B308 60.2(3) . . ? B305 B304 B308 108.9(3) . . ? C301 B304 B303 59.5(2) . . ? B309 B304 B303 107.2(3) . . ? B305 B304 B303 108.3(3) . . ? B308 B304 B303 59.3(3) . . ? C301 B305 B309 104.3(3) . . ? C301 B305 B304 58.7(3) . . ? B309 B305 B304 59.4(3) . . ? C301 B305 B306 59.9(3) . . ? B309 B305 B306 107.5(3) . . ? B304 B305 B306 108.7(3) . . ? C301 B305 B310 105.8(3) . . ? B309 B305 B310 59.9(3) . . ? B304 B305 B310 108.1(3) . . ? B306 B305 B310 59.9(2) . . ? C302 B306 C301 56.7(2) . . ? C302 B306 B311 58.1(3) . . ? C301 B306 B311 104.6(3) . . ? C302 B306 B310 103.4(3) . . ? C301 B306 B310 104.3(3) . . ? B311 B306 B310 60.0(3) . . ? C302 B306 B305 102.8(3) . . ? C301 B306 B305 57.8(2) . . ? B311 B306 B305 107.7(3) . . ? B310 B306 B305 60.1(3) . . ? C302 B307 B312 103.0(3) . . ? C302 B307 B303 58.5(2) . . ? B312 B307 B303 107.0(3) . . ? C302 B307 B308 103.0(3) . . ? B312 B307 B308 60.2(3) . . ? B303 B307 B308 58.9(3) . . ? C302 B307 B311 57.7(3) . . ? B312 B307 B311 59.8(3) . . ? B303 B307 B311 107.2(3) . . ? B308 B307 B311 107.6(4) . . ? B303 B308 B309 107.4(3) . . ? B303 B308 B304 60.4(3) . . ? B309 B308 B304 59.4(3) . . ? B303 B308 B312 107.6(3) . . ? B309 B308 B312 59.6(3) . . ? B304 B308 B312 107.5(3) . . ? B303 B308 B307 60.4(3) . . ? B309 B308 B307 107.3(4) . . ? B304 B308 B307 108.5(3) . . ? B312 B308 B307 59.5(3) . . ? B304 B309 B312 109.0(3) . . ? B304 B309 B308 60.4(3) . . ? B312 B309 B308 60.6(3) . . ? B304 B309 B305 60.3(3) . . ? B312 B309 B305 109.0(3) . . ? B308 B309 B305 109.0(3) . . ? B304 B309 B310 109.3(3) . . ? B312 B309 B310 60.8(3) . . ? B308 B309 B310 109.7(3) . . ? B305 B309 B310 60.5(3) . . ? B309 B310 B311 107.0(3) . . ? B309 B310 B306 107.4(3) . . ? B311 B310 B306 59.8(3) . . ? B309 B310 B305 59.6(2) . . ? B311 B310 B305 107.5(3) . . ? B306 B310 B305 60.0(2) . . ? B309 B310 B312 59.4(3) . . ? B311 B310 B312 59.8(3) . . ? B306 B310 B312 107.6(3) . . ? B305 B310 B312 107.2(3) . . ? C302 B311 B306 59.0(3) . . ? C302 B311 B310 104.1(3) . . ? B306 B311 B310 60.2(3) . . ? C302 B311 B312 103.1(3) . . ? B306 B311 B312 108.4(3) . . ? B310 B311 B312 60.4(3) . . ? C302 B311 B307 58.4(3) . . ? B306 B311 B307 108.8(3) . . ? B310 B311 B307 108.3(3) . . ? B312 B311 B307 59.3(3) . . ? B309 B312 B307 108.1(3) . . ? B309 B312 B311 107.4(3) . . ? B307 B312 B311 60.9(3) . . ? B309 B312 B308 59.8(3) . . ? B307 B312 B308 60.3(3) . . ? B311 B312 B308 108.6(3) . . ? B309 B312 B310 59.8(3) . . ? B307 B312 B310 109.0(3) . . ? B311 B312 B310 59.8(3) . . ? B308 B312 B310 108.3(3) . . ? C303 C301 C302 118.5(3) . . ? C303 C301 B304 120.5(3) . . ? C302 C301 B304 109.4(3) . . ? C303 C301 B305 124.0(3) . . ? C302 C301 B305 109.3(3) . . ? B304 C301 B305 62.5(3) . . ? C303 C301 B303 114.2(3) . . ? C302 C301 B303 60.7(2) . . ? B304 C301 B303 62.2(3) . . ? B305 C301 B303 113.6(3) . . ? C303 C301 B306 119.5(3) . . ? C302 C301 B306 60.5(2) . . ? B304 C301 B306 113.7(3) . . ? B305 C301 B306 62.3(3) . . ? B303 C301 B306 113.3(3) . . ? C301 C302 B311 113.3(3) . . ? C301 C302 B303 62.1(2) . . ? B311 C302 B303 116.0(3) . . ? C301 C302 B307 113.4(3) . . ? B311 C302 B307 63.9(3) . . ? B303 C302 B307 62.9(3) . . ? C301 C302 B306 62.7(3) . . ? B311 C302 B306 62.9(3) . . ? B303 C302 B306 116.4(3) . . ? B307 C302 B306 116.8(3) . . ? C304 C303 C301 122.9(4) . . ? C303 C304 C305 125.8(4) . . ? C318 C305 C306 120.7(4) . . ? C318 C305 C304 122.8(4) . . ? C306 C305 C304 116.5(4) . . ? C305 C306 C307 123.1(4) . . ? C305 C306 C311 119.7(4) . . ? C307 C306 C311 117.2(4) . . ? C308 C307 C306 121.5(4) . . ? C307 C308 C309 121.1(4) . . ? C310 C309 C308 119.0(5) . . ? C309 C310 C311 122.3(4) . . ? C312 C311 C310 122.0(4) . . ? C312 C311 C306 119.1(4) . . ? C310 C311 C306 118.9(4) . . ? C311 C312 C313 121.9(4) . . ? C312 C313 C314 121.5(4) . . ? C312 C313 C318 119.9(4) . . ? C314 C313 C318 118.5(4) . . ? C315 C314 C313 121.9(4) . . ? C314 C315 C316 119.8(4) . . ? C317 C316 C315 120.4(4) . . ? C316 C317 C318 121.9(4) . . ? C305 C318 C317 123.9(4) . . ? C305 C318 C313 118.7(4) . . ? C317 C318 C313 117.4(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.370 _refine_diff_density_min -0.260 _refine_diff_density_rms 0.049