Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_section_title ; A solvent-free regioselective iodination route of ortho-carboranes ; _publ_contact_author_name 'Clara Vinas' _publ_contact_author_address ; Materials Moleculars i Supramoleculars ICMAB (CSIC) Campus UAB Bellaterra 08193 SPAIN ; _publ_contact_author_phone '+34 93 5801853' _publ_contact_author_fax '+34 93 5805729' _publ_contact_author_email clara@icmab.es loop_ _publ_author_name _publ_author_address 'Albert Vaca' ; Institut de Ciencia de Materials de Barcelona CSCI Campus UAB E-08193 Bellaterra Spain ; 'Francesc Teixidor' ; Institut de Ciencia de Materials de Barcelona CSCI Campus UAB 08193 Bellaterra Spain ; 'Raikko Kivekas' ; Department of Chemistry POBox 55 FIN-00014 University of Helsinki Finland ; 'Reijo Sillanpaa' ; Department of Chemistry University of Jyvaskyla FIN-40351 Jyvaskyla Finland ; 'Clara Vinas' ; Institut de Ciencia de Materials de Barcelona CSCI Campus UAB 08193 Bellaterra Spain ; data_compound_1 _database_code_depnum_ccdc_archive 'CCDC 611426' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C2 H8 B10 I4' _chemical_formula_sum 'C2 H8 B10 I4' _chemical_formula_weight 647.78 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.0422(5) _cell_length_b 14.8814(5) _cell_length_c 14.3581(5) _cell_angle_alpha 90.00 _cell_angle_beta 110.378(2) _cell_angle_gamma 90.00 _cell_volume 3012.90(18) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6090 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 28.7 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.856 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2256 _exptl_absorpt_correction_type refdelf _exptl_absorpt_coefficient_mu 8.235 _exptl_absorpt_factor_muR 0.000 _exptl_absorpt_process_details ; Sheldrick, G.M. (anon) SHELX97 Release 97-2 (1998) I/sigma threshold for reflections = 5.000 Delta(U)/lambda**2 = 0.000 Highest even order spherical harmonic = 6 Highest odd order spherical harmonic = 3 ; _exptl_absorpt_correction_T_min 0.3265 _exptl_absorpt_correction_T_max 0.6927 _exptl_absorpt_Rmerge_before 0.0804 _exptl_absorpt_Rmerge_after 0.0389 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_type Mok\a _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_radiation_probe x-ray _diffrn_radiation_wavelength 0.71073 _diffrn_source 'Enraf Nonius FR590' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_decay_% <1 _diffrn_reflns_number 18481 _diffrn_reflns_av_R_equivalents 0.0581 _diffrn_reflns_av_sigmaI/netI 0.0731 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 27.00 _reflns_number_total 6563 _reflns_number_gt 4452 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. Electron density synthesis with coefficients Fo-Fc Highest peak 3.12 at 0.4718 0.5671 0.0997 [ 0.88 A from I29 ] Deepest hole -1.87 at 0.2928 0.6604 0.0163 [ 0.67 A from I28 ] ; _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^)+(0.0371P)^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 SHELXL _refine_ls_extinction_coef 0.00018(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6563 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0814 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.0930 _refine_ls_wR_factor_gt 0.0855 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I8 I 0.21627(4) 0.11808(4) 0.51033(4) 0.03096(15) Uani 1 d . . . I9 I -0.05981(4) 0.05227(3) 0.35664(4) 0.03014(15) Uani 1 d . . . I10 I -0.09701(5) 0.07420(4) 0.05822(5) 0.04447(18) Uani 1 d . . . I12 I 0.15991(4) -0.01711(3) 0.25268(4) 0.02939(15) Uani 1 d . . . C1 C 0.0435(6) 0.3236(5) 0.2602(6) 0.0249(19) Uani 1 d . . . H1 H 0.0217 0.3954 0.2610 0.030 Uiso 1 calc R . . C2 C 0.1274(6) 0.2972(5) 0.2211(6) 0.0262(19) Uani 1 d . . . H2 H 0.1651 0.3505 0.1940 0.031 Uiso 1 calc R . . B3 B 0.1494(7) 0.2938(6) 0.3458(7) 0.025(2) Uani 1 d . . . H3 H 0.1980 0.3404 0.4019 0.030 Uiso 1 calc R . . B4 B 0.0406(6) 0.2557(5) 0.3552(7) 0.022(2) Uani 1 d . . . H4 H 0.0173 0.2763 0.4182 0.026 Uiso 1 calc R . . B5 B -0.0432(7) 0.2440(6) 0.2318(7) 0.026(2) Uani 1 d . . . H5 H -0.1205 0.2574 0.2146 0.031 Uiso 1 calc R . . B6 B 0.0146(7) 0.2726(7) 0.1460(8) 0.032(2) Uani 1 d . . . H6 H -0.0241 0.3051 0.0727 0.038 Uiso 1 calc R . . B7 B 0.1930(7) 0.2095(6) 0.2858(8) 0.028(2) Uani 1 d . . . H7 H 0.2709 0.1997 0.3028 0.034 Uiso 1 calc R . . B8 B 0.1362(7) 0.1794(6) 0.3717(7) 0.023(2) Uani 1 d . . . B9 B 0.0166(6) 0.1470(6) 0.3008(7) 0.0189(19) Uani 1 d . . . B10 B -0.0005(7) 0.1577(6) 0.1703(7) 0.025(2) Uani 1 d . . . B11 B 0.1087(7) 0.1958(6) 0.1610(7) 0.025(2) Uani 1 d . . . H11 H 0.1316 0.1771 0.0972 0.030 Uiso 1 calc R . . B12 B 0.1114(6) 0.1181(6) 0.2570(6) 0.0190(19) Uani 1 d . . . I28 I 0.73552(5) 0.16349(5) 0.45656(5) 0.0500(2) Uani 1 d . . . I29 I 0.46616(4) 0.06887(3) 0.37774(4) 0.02804(15) Uani 1 d . . . I30 I 0.35985(4) 0.03052(4) 0.07819(5) 0.04104(17) Uani 1 d . . . I32 I 0.64076(4) -0.03199(3) 0.22907(4) 0.02820(15) Uani 1 d . . . C21 C 0.5106(7) 0.3081(6) 0.1819(8) 0.044(3) Uani 1 d . . . H21 H 0.4832 0.3787 0.1686 0.052 Uiso 1 calc R . . C22 C 0.5804(7) 0.2684(6) 0.1287(8) 0.044(3) Uani 1 d . . . H22 H 0.6040 0.3117 0.0778 0.053 Uiso 1 calc R . . B23 B 0.6281(8) 0.2924(7) 0.2497(9) 0.041(3) Uani 1 d . . . H23 H 0.6800 0.3479 0.2817 0.050 Uiso 1 calc R . . B24 B 0.5386(8) 0.2638(7) 0.2994(9) 0.041(3) Uani 1 d . . . H24 H 0.5318 0.2998 0.3651 0.049 Uiso 1 calc R . . B25 B 0.4388(7) 0.2277(6) 0.1982(8) 0.030(2) Uani 1 d . . . H25 H 0.3653 0.2400 0.1981 0.036 Uiso 1 calc R . . B26 B 0.4649(7) 0.2356(7) 0.0883(8) 0.034(3) Uani 1 d . . . H26 H 0.4106 0.2538 0.0149 0.041 Uiso 1 calc R . . B27 B 0.6607(9) 0.1935(7) 0.1992(9) 0.043(3) Uani 1 d . . . H27 H 0.7342 0.1828 0.1988 0.052 Uiso 1 calc R . . B28 B 0.6323(7) 0.1867(6) 0.3105(8) 0.031(2) Uani 1 d . . . B29 B 0.5142(7) 0.1467(6) 0.2780(7) 0.024(2) Uani 1 d . . . B30 B 0.4662(7) 0.1307(6) 0.1462(7) 0.023(2) Uani 1 d . . . B31 B 0.5578(7) 0.1583(6) 0.0977(8) 0.032(2) Uani 1 d . . . H31 H 0.5641 0.1245 0.0306 0.038 Uiso 1 calc R . . B32 B 0.5890(6) 0.1048(6) 0.2150(7) 0.022(2) Uani 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 I8 0.0331(3) 0.0346(3) 0.0203(3) 0.0020(2) 0.0031(3) 0.0038(3) I9 0.0347(3) 0.0224(3) 0.0418(4) -0.0013(2) 0.0241(3) -0.0053(2) I10 0.0385(4) 0.0493(4) 0.0336(4) -0.0141(3) -0.0026(3) -0.0029(3) I12 0.0298(3) 0.0224(3) 0.0386(3) -0.0043(2) 0.0153(3) 0.0035(2) C1 0.025(5) 0.013(4) 0.034(5) -0.001(3) 0.006(4) 0.000(3) C2 0.026(5) 0.026(4) 0.030(5) 0.005(4) 0.014(4) 0.000(4) B3 0.026(6) 0.018(4) 0.028(6) 0.000(4) 0.005(5) -0.003(4) B4 0.017(5) 0.014(4) 0.029(5) -0.003(4) 0.001(4) 0.001(4) B5 0.025(5) 0.027(5) 0.023(5) 0.002(4) 0.005(5) -0.009(4) B6 0.028(6) 0.032(5) 0.034(6) 0.007(5) 0.010(5) 0.011(5) B7 0.019(5) 0.028(5) 0.035(6) 0.003(4) 0.005(5) 0.002(4) B8 0.027(5) 0.017(4) 0.026(5) -0.001(4) 0.011(5) -0.006(4) B9 0.024(5) 0.015(4) 0.022(5) 0.000(4) 0.014(4) -0.004(4) B10 0.023(5) 0.024(5) 0.025(5) -0.002(4) 0.004(4) 0.002(4) B11 0.037(6) 0.024(5) 0.015(5) 0.000(4) 0.011(5) -0.007(4) B12 0.022(5) 0.017(4) 0.017(5) -0.004(4) 0.005(4) -0.001(4) I28 0.0322(4) 0.0616(4) 0.0496(4) -0.0207(4) 0.0058(3) -0.0003(3) I29 0.0423(4) 0.0225(3) 0.0243(3) 0.0035(2) 0.0178(3) -0.0002(2) I30 0.0359(4) 0.0473(4) 0.0319(4) -0.0040(3) 0.0017(3) 0.0005(3) I32 0.0307(3) 0.0214(3) 0.0325(3) 0.0052(2) 0.0109(3) 0.0076(2) C21 0.063(7) 0.026(5) 0.062(7) -0.002(5) 0.046(6) -0.006(5) C22 0.059(7) 0.028(5) 0.065(7) 0.020(5) 0.046(6) 0.012(4) B23 0.043(7) 0.028(5) 0.061(8) -0.004(5) 0.028(7) -0.009(5) B24 0.049(7) 0.029(6) 0.046(7) 0.002(5) 0.020(6) 0.012(5) B25 0.027(6) 0.029(5) 0.040(6) 0.007(5) 0.018(5) 0.009(4) B26 0.027(6) 0.043(6) 0.038(6) 0.025(5) 0.018(5) 0.022(5) B27 0.050(8) 0.023(5) 0.066(9) 0.005(5) 0.031(7) -0.004(5) B28 0.035(6) 0.026(5) 0.033(6) -0.009(4) 0.012(5) -0.007(4) B29 0.021(5) 0.024(5) 0.030(6) 0.002(4) 0.013(5) -0.008(4) B30 0.026(5) 0.018(5) 0.027(5) 0.001(4) 0.013(5) 0.002(4) B31 0.042(7) 0.024(5) 0.035(6) 0.017(5) 0.020(5) 0.008(5) B32 0.023(5) 0.016(4) 0.027(5) 0.009(4) 0.009(4) 0.004(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I8 B8 2.139(10) . ? I9 B9 2.143(8) . ? I10 B10 2.148(9) . ? I12 B12 2.149(8) . ? C1 C2 1.599(10) . ? C1 B3 1.697(12) . ? C1 B5 1.702(11) . ? C1 B4 1.710(12) . ? C1 B6 1.719(13) . ? C1 H1 1.1200 . ? C2 B6 1.704(13) . ? C2 B7 1.704(12) . ? C2 B3 1.705(12) . ? C2 B11 1.712(12) . ? C2 H2 1.1200 . ? B3 B8 1.768(12) . ? B3 B7 1.773(13) . ? B3 B4 1.780(13) . ? B3 H3 1.1200 . ? B4 B9 1.778(11) . ? B4 B8 1.782(12) . ? B4 B5 1.790(13) . ? B4 H4 1.1200 . ? B5 B6 1.789(13) . ? B5 B10 1.799(13) . ? B5 B9 1.804(13) . ? B5 H5 1.1200 . ? B6 B11 1.774(13) . ? B6 B10 1.775(13) . ? B6 H6 1.1200 . ? B7 B12 1.781(13) . ? B7 B8 1.785(13) . ? B7 B11 1.809(14) . ? B7 H7 1.1200 . ? B8 B9 1.797(13) . ? B8 B12 1.805(12) . ? B9 B12 1.799(11) . ? B9 B10 1.809(12) . ? B10 B11 1.786(13) . ? B10 B12 1.808(13) . ? B11 B12 1.788(12) . ? B11 H11 1.1200 . ? I28 B28 2.158(11) . ? I29 B29 2.152(8) . ? I30 B30 2.156(9) . ? I32 B32 2.164(8) . ? C21 C22 1.611(12) . ? C21 B26 1.673(15) . ? C21 B25 1.681(12) . ? C21 B23 1.711(16) . ? C21 B24 1.721(14) . ? C21 H21 1.1200 . ? C22 B23 1.670(15) . ? C22 B27 1.695(15) . ? C22 B26 1.700(14) . ? C22 B31 1.701(13) . ? C22 H22 1.1200 . ? B23 B24 1.781(15) . ? B23 B27 1.782(14) . ? B23 B28 1.789(14) . ? B23 H23 1.1200 . ? B24 B25 1.771(16) . ? B24 B28 1.780(14) . ? B24 B29 1.785(13) . ? B24 H24 1.1200 . ? B25 B30 1.740(12) . ? B25 B26 1.757(13) . ? B25 B29 1.775(13) . ? B25 H25 1.1200 . ? B26 B30 1.766(12) . ? B26 B31 1.779(13) . ? B26 H26 1.1200 . ? B27 B32 1.768(13) . ? B27 B28 1.795(14) . ? B27 B31 1.795(17) . ? B27 H27 1.1200 . ? B28 B29 1.776(13) . ? B28 B32 1.781(13) . ? B29 B32 1.784(12) . ? B29 B30 1.791(13) . ? B30 B31 1.795(13) . ? B30 B32 1.807(13) . ? B31 B32 1.773(12) . ? B31 H31 1.1200 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 B3 62.2(5) . . ? C2 C1 B5 112.2(6) . . ? B3 C1 B5 116.1(6) . . ? C2 C1 B4 112.2(6) . . ? B3 C1 B4 63.0(5) . . ? B5 C1 B4 63.3(5) . . ? C2 C1 B6 61.7(5) . . ? B3 C1 B6 115.9(6) . . ? B5 C1 B6 63.0(5) . . ? B4 C1 B6 115.6(6) . . ? C2 C1 H1 120.5 . . ? B3 C1 H1 116.5 . . ? B5 C1 H1 117.7 . . ? B4 C1 H1 117.9 . . ? B6 C1 H1 116.9 . . ? C1 C2 B6 62.6(5) . . ? C1 C2 B7 112.0(6) . . ? B6 C2 B7 116.1(7) . . ? C1 C2 B3 61.7(5) . . ? B6 C2 B3 116.3(6) . . ? B7 C2 B3 62.7(5) . . ? C1 C2 B11 112.4(6) . . ? B6 C2 B11 62.6(6) . . ? B7 C2 B11 64.0(5) . . ? B3 C2 B11 116.1(6) . . ? C1 C2 H2 120.4 . . ? B6 C2 H2 116.4 . . ? B7 C2 H2 117.7 . . ? B3 C2 H2 116.8 . . ? B11 C2 H2 117.6 . . ? C1 B3 C2 56.1(5) . . ? C1 B3 B8 105.0(6) . . ? C2 B3 B8 104.8(6) . . ? C1 B3 B7 104.2(7) . . ? C2 B3 B7 58.6(5) . . ? B8 B3 B7 60.5(5) . . ? C1 B3 B4 58.9(5) . . ? C2 B3 B4 104.0(6) . . ? B8 B3 B4 60.3(5) . . ? B7 B3 B4 108.5(6) . . ? C1 B3 H3 124.9 . . ? C2 B3 H3 125.2 . . ? B8 B3 H3 122.5 . . ? B7 B3 H3 121.9 . . ? B4 B3 H3 122.0 . . ? C1 B4 B9 104.2(6) . . ? C1 B4 B3 58.1(5) . . ? B9 B4 B3 107.9(6) . . ? C1 B4 B8 103.8(6) . . ? B9 B4 B8 60.6(5) . . ? B3 B4 B8 59.5(5) . . ? C1 B4 B5 58.2(5) . . ? B9 B4 B5 60.7(5) . . ? B3 B4 B5 107.7(6) . . ? B8 B4 B5 109.1(6) . . ? C1 B4 H4 125.8 . . ? B9 B4 H4 122.0 . . ? B3 B4 H4 121.9 . . ? B8 B4 H4 122.2 . . ? B5 B4 H4 121.0 . . ? C1 B5 B6 58.9(5) . . ? C1 B5 B4 58.6(5) . . ? B6 B5 B4 108.4(7) . . ? C1 B5 B10 103.8(6) . . ? B6 B5 B10 59.3(5) . . ? B4 B5 B10 107.9(7) . . ? C1 B5 B9 103.4(6) . . ? B6 B5 B9 107.5(6) . . ? B4 B5 B9 59.3(5) . . ? B10 B5 B9 60.3(5) . . ? C1 B5 H5 125.4 . . ? B6 B5 H5 121.4 . . ? B4 B5 H5 121.4 . . ? B10 B5 H5 122.6 . . ? B9 B5 H5 123.0 . . ? C2 B6 C1 55.7(5) . . ? C2 B6 B11 59.0(5) . . ? C1 B6 B11 104.0(7) . . ? C2 B6 B10 104.5(7) . . ? C1 B6 B10 104.2(7) . . ? B11 B6 B10 60.4(5) . . ? C2 B6 B5 103.4(7) . . ? C1 B6 B5 58.0(5) . . ? B11 B6 B5 108.8(7) . . ? B10 B6 B5 60.6(5) . . ? C2 B6 H6 125.4 . . ? C1 B6 H6 125.6 . . ? B11 B6 H6 121.6 . . ? B10 B6 H6 122.7 . . ? B5 B6 H6 122.1 . . ? C2 B7 B3 58.7(5) . . ? C2 B7 B12 103.7(6) . . ? B3 B7 B12 108.1(6) . . ? C2 B7 B8 104.1(6) . . ? B3 B7 B8 59.6(5) . . ? B12 B7 B8 60.8(5) . . ? C2 B7 B11 58.3(5) . . ? B3 B7 B11 108.1(7) . . ? B12 B7 B11 59.7(5) . . ? B8 B7 B11 108.5(7) . . ? C2 B7 H7 125.6 . . ? B3 B7 H7 121.4 . . ? B12 B7 H7 122.4 . . ? B8 B7 H7 122.1 . . ? B11 B7 H7 121.4 . . ? B3 B8 B4 60.2(5) . . ? B3 B8 B7 59.9(5) . . ? B4 B8 B7 107.9(6) . . ? B3 B8 B9 107.6(7) . . ? B4 B8 B9 59.6(5) . . ? B7 B8 B9 107.5(6) . . ? B3 B8 B12 107.3(6) . . ? B4 B8 B12 107.4(7) . . ? B7 B8 B12 59.5(5) . . ? B9 B8 B12 59.9(5) . . ? B3 B8 I8 122.6(6) . . ? B4 B8 I8 124.2(6) . . ? B7 B8 I8 120.0(6) . . ? B9 B8 I8 122.7(5) . . ? B12 B8 I8 120.3(5) . . ? B4 B9 B8 59.8(5) . . ? B4 B9 B12 107.9(6) . . ? B8 B9 B12 60.3(5) . . ? B4 B9 B5 60.0(5) . . ? B8 B9 B5 107.8(6) . . ? B12 B9 B5 107.6(6) . . ? B4 B9 B10 108.0(6) . . ? B8 B9 B10 108.5(6) . . ? B12 B9 B10 60.2(5) . . ? B5 B9 B10 59.7(5) . . ? B4 B9 I9 119.2(5) . . ? B8 B9 I9 121.8(5) . . ? B12 B9 I9 124.5(5) . . ? B5 B9 I9 120.1(5) . . ? B10 B9 I9 123.0(5) . . ? B6 B10 B11 59.8(5) . . ? B6 B10 B5 60.1(5) . . ? B11 B10 B5 107.8(6) . . ? B6 B10 B12 107.3(7) . . ? B11 B10 B12 59.7(5) . . ? B5 B10 B12 107.5(6) . . ? B6 B10 B9 107.8(6) . . ? B11 B10 B9 107.6(6) . . ? B5 B10 B9 60.0(5) . . ? B12 B10 B9 59.7(5) . . ? B6 B10 I10 120.7(6) . . ? B11 B10 I10 121.8(6) . . ? B5 B10 I10 121.1(6) . . ? B12 B10 I10 123.4(5) . . ? B9 B10 I10 122.7(5) . . ? C2 B11 B6 58.5(5) . . ? C2 B11 B10 103.6(6) . . ? B6 B11 B10 59.8(5) . . ? C2 B11 B12 103.1(6) . . ? B6 B11 B12 108.2(6) . . ? B10 B11 B12 60.8(5) . . ? C2 B11 B7 57.8(5) . . ? B6 B11 B7 107.6(7) . . ? B10 B11 B7 107.9(6) . . ? B12 B11 B7 59.3(5) . . ? C2 B11 H11 126.0 . . ? B6 B11 H11 121.4 . . ? B10 B11 H11 122.3 . . ? B12 B11 H11 122.6 . . ? B7 B11 H11 121.9 . . ? B7 B12 B11 60.9(5) . . ? B7 B12 B9 107.6(6) . . ? B11 B12 B9 107.9(6) . . ? B7 B12 B8 59.7(5) . . ? B11 B12 B8 108.6(6) . . ? B9 B12 B8 59.8(5) . . ? B7 B12 B10 108.2(6) . . ? B11 B12 B10 59.6(5) . . ? B9 B12 B10 60.2(5) . . ? B8 B12 B10 108.1(6) . . ? B7 B12 I12 120.5(5) . . ? B11 B12 I12 120.0(5) . . ? B9 B12 I12 123.5(5) . . ? B8 B12 I12 122.3(5) . . ? B10 B12 I12 122.0(5) . . ? C22 C21 B26 62.3(6) . . ? C22 C21 B25 111.2(7) . . ? B26 C21 B25 63.2(6) . . ? C22 C21 B23 60.3(6) . . ? B26 C21 B23 115.0(7) . . ? B25 C21 B23 114.2(7) . . ? C22 C21 B24 110.3(8) . . ? B26 C21 B24 115.6(7) . . ? B25 C21 B24 62.7(6) . . ? B23 C21 B24 62.5(6) . . ? C22 C21 H21 121.6 . . ? B26 C21 H21 116.3 . . ? B25 C21 H21 118.4 . . ? B23 C21 H21 118.1 . . ? B24 C21 H21 118.5 . . ? C21 C22 B23 62.9(6) . . ? C21 C22 B27 113.9(8) . . ? B23 C22 B27 64.0(7) . . ? C21 C22 B26 60.6(6) . . ? B23 C22 B26 115.7(7) . . ? B27 C22 B26 116.5(7) . . ? C21 C22 B31 112.0(7) . . ? B23 C22 B31 116.9(7) . . ? B27 C22 B31 63.8(6) . . ? B26 C22 B31 63.1(6) . . ? C21 C22 H22 120.4 . . ? B23 C22 H22 115.9 . . ? B27 C22 H22 116.5 . . ? B26 C22 H22 117.4 . . ? B31 C22 H22 117.5 . . ? C22 B23 C21 56.9(6) . . ? C22 B23 B24 104.8(8) . . ? C21 B23 B24 59.0(6) . . ? C22 B23 B27 58.7(6) . . ? C21 B23 B27 104.9(8) . . ? B24 B23 B27 108.6(7) . . ? C22 B23 B28 104.5(7) . . ? C21 B23 B28 104.6(7) . . ? B24 B23 B28 59.8(6) . . ? B27 B23 B28 60.3(6) . . ? C22 B23 H23 124.8 . . ? C21 B23 H23 124.5 . . ? B24 B23 H23 121.8 . . ? B27 B23 H23 121.7 . . ? B28 B23 H23 123.1 . . ? C21 B24 B25 57.5(6) . . ? C21 B24 B28 104.5(7) . . ? B25 B24 B28 107.3(7) . . ? C21 B24 B23 58.5(6) . . ? B25 B24 B23 106.7(8) . . ? B28 B24 B23 60.3(6) . . ? C21 B24 B29 103.9(7) . . ? B25 B24 B29 59.9(6) . . ? B28 B24 B29 59.8(5) . . ? B23 B24 B29 107.7(7) . . ? C21 B24 H24 125.3 . . ? B25 B24 H24 122.4 . . ? B28 B24 H24 122.3 . . ? B23 B24 H24 121.8 . . ? B29 B24 H24 122.6 . . ? C21 B25 B30 105.7(6) . . ? C21 B25 B26 58.2(6) . . ? B30 B25 B26 60.7(5) . . ? C21 B25 B24 59.8(6) . . ? B30 B25 B24 110.1(7) . . ? B26 B25 B24 109.0(7) . . ? C21 B25 B29 106.0(7) . . ? B30 B25 B29 61.2(5) . . ? B26 B25 B29 109.4(6) . . ? B24 B25 B29 60.5(6) . . ? C21 B25 H25 124.4 . . ? B30 B25 H25 121.1 . . ? B26 B25 H25 121.2 . . ? B24 B25 H25 120.4 . . ? B29 B25 H25 121.3 . . ? C21 B26 C22 57.0(6) . . ? C21 B26 B25 58.6(5) . . ? C22 B26 B25 103.5(8) . . ? C21 B26 B30 104.9(7) . . ? C22 B26 B30 104.5(7) . . ? B25 B26 B30 59.2(5) . . ? C21 B26 B31 105.3(8) . . ? C22 B26 B31 58.5(5) . . ? B25 B26 B31 107.7(7) . . ? B30 B26 B31 60.9(5) . . ? C21 B26 H26 124.2 . . ? C22 B26 H26 125.2 . . ? B25 B26 H26 122.9 . . ? B30 B26 H26 122.9 . . ? B31 B26 H26 121.6 . . ? C22 B27 B32 103.2(8) . . ? C22 B27 B23 57.3(6) . . ? B32 B27 B23 107.3(7) . . ? C22 B27 B28 103.2(7) . . ? B32 B27 B28 60.0(5) . . ? B23 B27 B28 60.0(6) . . ? C22 B27 B31 58.2(6) . . ? B32 B27 B31 59.7(5) . . ? B23 B27 B31 106.8(8) . . ? B28 B27 B31 107.6(7) . . ? C22 B27 H27 126.1 . . ? B32 B27 H27 122.8 . . ? B23 B27 H27 122.1 . . ? B28 B27 H27 122.6 . . ? B31 B27 H27 121.8 . . ? B29 B28 B24 60.3(6) . . ? B29 B28 B32 60.2(5) . . ? B24 B28 B32 107.8(7) . . ? B29 B28 B23 107.7(8) . . ? B24 B28 B23 59.9(6) . . ? B32 B28 B23 106.5(7) . . ? B29 B28 B27 108.1(7) . . ? B24 B28 B27 108.1(8) . . ? B32 B28 B27 59.3(5) . . ? B23 B28 B27 59.6(6) . . ? B29 B28 I28 121.1(6) . . ? B24 B28 I28 118.0(6) . . ? B32 B28 I28 125.8(6) . . ? B23 B28 I28 120.5(6) . . ? B27 B28 I28 124.1(7) . . ? B25 B29 B28 107.3(6) . . ? B25 B29 B32 106.5(6) . . ? B28 B29 B32 60.0(5) . . ? B25 B29 B24 59.6(6) . . ? B28 B29 B24 60.0(6) . . ? B32 B29 B24 107.4(6) . . ? B25 B29 B30 58.4(5) . . ? B28 B29 B30 108.7(6) . . ? B32 B29 B30 60.7(5) . . ? B24 B29 B30 107.1(7) . . ? B25 B29 I29 120.6(5) . . ? B28 B29 I29 122.9(6) . . ? B32 B29 I29 124.5(5) . . ? B24 B29 I29 120.5(6) . . ? B30 B29 I29 121.8(5) . . ? B25 B30 B26 60.1(5) . . ? B25 B30 B29 60.3(5) . . ? B26 B30 B29 108.3(7) . . ? B25 B30 B31 107.7(6) . . ? B26 B30 B31 59.9(5) . . ? B29 B30 B31 107.4(7) . . ? B25 B30 B32 107.0(7) . . ? B26 B30 B32 106.7(6) . . ? B29 B30 B32 59.5(5) . . ? B31 B30 B32 59.0(5) . . ? B25 B30 I30 121.2(6) . . ? B26 B30 I30 120.9(6) . . ? B29 B30 I30 122.2(5) . . ? B31 B30 I30 122.1(6) . . ? B32 B30 I30 123.8(5) . . ? C22 B31 B32 102.8(7) . . ? C22 B31 B26 58.5(6) . . ? B32 B31 B26 107.6(7) . . ? C22 B31 B27 57.9(6) . . ? B32 B31 B27 59.4(5) . . ? B26 B31 B27 107.8(8) . . ? C22 B31 B30 103.2(6) . . ? B32 B31 B30 60.8(5) . . ? B26 B31 B30 59.2(5) . . ? B27 B31 B30 108.2(7) . . ? C22 B31 H31 126.2 . . ? B32 B31 H31 122.8 . . ? B26 B31 H31 121.7 . . ? B27 B31 H31 121.6 . . ? B30 B31 H31 122.4 . . ? B27 B32 B31 60.9(6) . . ? B27 B32 B28 60.8(6) . . ? B31 B32 B28 109.2(6) . . ? B27 B32 B29 108.9(6) . . ? B31 B32 B29 108.7(6) . . ? B28 B32 B29 59.8(5) . . ? B27 B32 B30 108.9(7) . . ? B31 B32 B30 60.2(5) . . ? B28 B32 B30 107.8(6) . . ? B29 B32 B30 59.8(5) . . ? B27 B32 I32 119.9(6) . . ? B31 B32 I32 118.6(6) . . ? B28 B32 I32 123.3(6) . . ? B29 B32 I32 123.5(5) . . ? B30 B32 I32 121.2(5) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C1 H1 I9 1.12 3.05 3.840(7) 127.9 2 C1 H1 I12 1.12 2.97 3.824(8) 133.1 2 C2 H2 I8 1.12 3.03 3.918(7) 136.4 4_565 C21 H21 I29 1.12 3.06 4.016(9) 143.1 2_655 C21 H21 I32 1.12 3.05 3.808(9) 125.1 2_655 C22 H22 I28 1.12 3.08 4.074(8) 148.2 4_565 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.121 _refine_diff_density_min -1.874 _refine_diff_density_rms 0.233 #===END data_compound_3 _database_code_depnum_ccdc_archive 'CCDC 611427' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C8 H12 B10 I4' _chemical_formula_sum 'C8 H12 B10 I4' _chemical_formula_weight 723.88 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.0569(4) _cell_length_b 15.2555(5) _cell_length_c 13.0206(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.686(2) _cell_angle_gamma 90.00 _cell_volume 1969.18(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3907 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 26.733 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.442 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 6.314 _exptl_absorpt_correction_type refdelf _exptl_absorpt_factor_muR 0.000 _exptl_absorpt_process_details ; Sheldrick, G.M. (anon) SHELX97 Release 97-2 (1998) I/sigma threshold for reflections = 5.000 Delta(U)/lambda**2 = 0.000 Highest even order spherical harmonic = 6 Highest odd order spherical harmonic = 3 ; _exptl_absorpt_correction_T_min 0.3302 _exptl_absorpt_correction_T_max 0.7581 _exptl_absorpt_Rmerge_before 0.0431 _exptl_absorpt_Rmerge_after 0.0386 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_type Mok\a _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_radiation_probe x-ray _diffrn_radiation_wavelength 0.71073 _diffrn_source 'Enraf Nonius FR590' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_decay_% <1 _diffrn_reflns_number 11228 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_sigmaI/netI 0.0446 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 26.74 _reflns_number_total 4181 _reflns_number_gt 3500 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowsky & Minor, 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowsky & Minor, 1997) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. Electron density synthesis with coefficients Fo-Fc Highest peak 1.23 at 0.1646 0.1646 0.3514 [ 0.88 A from I9 ] Deepest hole -1.50 at 0.2532 0.1567 0.4621 [ 0.69 A from I9 ] ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0093P)^2^+16.7265P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00032(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4181 _refine_ls_number_parameters 200 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0520 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.0793 _refine_ls_wR_factor_gt 0.0744 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I8 I 0.25559(6) 0.37519(4) 0.60429(4) 0.04781(16) Uani 1 d . . . I9 I 0.21665(6) 0.16147(3) 0.41270(4) 0.04208(15) Uani 1 d . . . I10 I 0.36425(4) 0.23564(3) 0.14146(3) 0.03119(12) Uani 1 d . . . I12 I 0.54796(5) 0.32135(3) 0.42493(4) 0.03970(14) Uani 1 d . . . C1 C 0.0420(6) 0.4272(4) 0.2555(5) 0.0257(13) Uani 1 d . . . C2 C 0.1778(6) 0.4904(4) 0.2646(5) 0.0260(13) Uani 1 d . . . H2 H 0.1667 0.5594 0.2349 0.031 Uiso 1 calc R . . C13 C -0.0920(6) 0.4635(4) 0.2056(5) 0.0282(14) Uani 1 d . . . C14 C -0.2054(7) 0.4120(5) 0.2049(6) 0.0413(18) Uani 1 d . . . H14 H -0.1965 0.3552 0.2353 0.050 Uiso 1 calc R . . C15 C -0.3322(7) 0.4424(6) 0.1601(6) 0.046(2) Uani 1 d . . . H15 H -0.4095 0.4066 0.1598 0.055 Uiso 1 calc R . . C16 C -0.3454(8) 0.5248(6) 0.1159(6) 0.047(2) Uani 1 d . . . H16 H -0.4320 0.5461 0.0857 0.057 Uiso 1 calc R . . C17 C -0.2322(8) 0.5762(6) 0.1157(6) 0.046(2) Uani 1 d . . . H17 H -0.2410 0.6328 0.0849 0.056 Uiso 1 calc R . . C18 C -0.1049(7) 0.5454(5) 0.1607(6) 0.0393(17) Uani 1 d . . . H18 H -0.0273 0.5809 0.1603 0.047 Uiso 1 calc R . . B3 B 0.1170(8) 0.4690(5) 0.3761(6) 0.0292(16) Uani 1 d . . . H3 H 0.0678 0.5181 0.4216 0.035 Uiso 1 calc R . . B4 B 0.0610(8) 0.3588(5) 0.3602(6) 0.0290(16) Uani 1 d . . . H4 H -0.0255 0.3343 0.3962 0.035 Uiso 1 calc R . . B5 B 0.0870(7) 0.3201(5) 0.2355(6) 0.0254(15) Uani 1 d . . . H5 H 0.0189 0.2705 0.1901 0.030 Uiso 1 calc R . . B6 B 0.1592(7) 0.4081(5) 0.1736(6) 0.0266(15) Uani 1 d . . . H6 H 0.1378 0.4176 0.0871 0.032 Uiso 1 calc R . . B7 B 0.2940(8) 0.4722(5) 0.3734(6) 0.0314(17) Uani 1 d . . . H7 H 0.3621 0.5227 0.4171 0.038 Uiso 1 calc R . . B8 B 0.2207(8) 0.3853(5) 0.4369(6) 0.0316(17) Uani 1 d . . . B9 B 0.2031(8) 0.2922(4) 0.3507(6) 0.0260(15) Uani 1 d . . . B10 B 0.2643(8) 0.3239(4) 0.2329(5) 0.0253(15) Uani 1 d . . . B11 B 0.3172(7) 0.4349(4) 0.2484(6) 0.0254(15) Uani 1 d . . . H11 H 0.4005 0.4618 0.2105 0.030 Uiso 1 calc R . . B12 B 0.3475(8) 0.3627(5) 0.3577(6) 0.0279(16) Uani 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 I8 0.0652(4) 0.0534(3) 0.0242(2) -0.0042(2) 0.0059(2) 0.0189(3) I9 0.0600(3) 0.0238(2) 0.0470(3) 0.0046(2) 0.0220(2) -0.0003(2) I10 0.0334(2) 0.0305(2) 0.0306(2) -0.00646(18) 0.00780(18) 0.00500(18) I12 0.0324(3) 0.0379(3) 0.0441(3) -0.0068(2) -0.0072(2) 0.00661(19) C1 0.024(3) 0.030(3) 0.024(3) -0.002(3) 0.005(3) -0.002(3) C2 0.020(3) 0.027(3) 0.032(3) 0.003(3) 0.007(3) 0.002(2) C13 0.026(3) 0.033(3) 0.027(3) -0.010(3) 0.010(3) 0.003(3) C14 0.033(4) 0.037(4) 0.056(5) -0.006(4) 0.014(4) 0.001(3) C15 0.023(4) 0.059(5) 0.055(5) -0.014(4) 0.004(3) -0.003(3) C16 0.034(4) 0.071(6) 0.038(4) -0.014(4) 0.008(3) 0.009(4) C17 0.041(4) 0.056(5) 0.041(4) 0.004(4) 0.003(4) 0.016(4) C18 0.034(4) 0.049(4) 0.036(4) 0.007(3) 0.008(3) 0.002(3) B3 0.029(4) 0.036(4) 0.024(4) -0.005(3) 0.007(3) -0.003(3) B4 0.032(4) 0.028(4) 0.028(4) 0.002(3) 0.011(3) -0.001(3) B5 0.024(4) 0.026(4) 0.028(4) 0.000(3) 0.010(3) 0.001(3) B6 0.025(4) 0.032(4) 0.023(4) -0.006(3) 0.006(3) -0.002(3) B7 0.034(4) 0.024(4) 0.035(4) -0.003(3) 0.001(3) -0.001(3) B8 0.042(5) 0.028(4) 0.025(4) -0.005(3) 0.005(3) 0.002(3) B9 0.031(4) 0.017(3) 0.031(4) -0.004(3) 0.007(3) -0.003(3) B10 0.034(4) 0.021(3) 0.022(4) -0.005(3) 0.008(3) 0.000(3) B11 0.017(3) 0.022(3) 0.039(4) 0.000(3) 0.008(3) -0.002(3) B12 0.029(4) 0.026(4) 0.028(4) -0.003(3) 0.002(3) 0.006(3) _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 I8 B8 2.153(8) . ? I9 B9 2.147(7) . ? I10 B10 2.155(7) . ? I12 B12 2.153(7) . ? C1 C13 1.501(9) . ? C1 C2 1.659(9) . ? C1 B4 1.702(9) . ? C1 B5 1.727(9) . ? C1 B6 1.742(9) . ? C1 B3 1.744(9) . ? C2 B11 1.682(9) . ? C2 B3 1.699(10) . ? C2 B7 1.700(10) . ? C2 B6 1.715(9) . ? C2 H2 1.1200 . ? C13 C18 1.376(10) . ? C13 C14 1.384(10) . ? C14 C15 1.390(10) . ? C14 H14 0.9500 . ? C15 C16 1.379(12) . ? C15 H15 0.9500 . ? C16 C17 1.383(12) . ? C16 H16 0.9500 . ? C17 C18 1.397(10) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? B3 B8 1.752(11) . ? B3 B4 1.774(11) . ? B3 B7 1.787(11) . ? B3 H3 1.1200 . ? B4 B9 1.775(11) . ? B4 B5 1.788(10) . ? B4 B8 1.789(11) . ? B4 H4 1.1200 . ? B5 B6 1.783(10) . ? B5 B10 1.790(10) . ? B5 B9 1.791(10) . ? B5 H5 1.1200 . ? B6 B10 1.758(10) . ? B6 B11 1.766(10) . ? B6 H6 1.1200 . ? B7 B11 1.777(11) . ? B7 B12 1.778(10) . ? B7 B8 1.786(11) . ? B7 H7 1.1200 . ? B8 B9 1.801(10) . ? B8 B12 1.803(11) . ? B9 B12 1.797(10) . ? B9 B10 1.812(10) . ? B10 B11 1.776(10) . ? B10 B12 1.798(10) . ? B11 B12 1.785(10) . ? B11 H11 1.1200 . ? 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 C13 C1 C2 119.0(5) . . ? C13 C1 B4 123.0(5) . . ? C2 C1 B4 108.6(5) . . ? C13 C1 B5 121.5(5) . . ? C2 C1 B5 109.1(5) . . ? B4 C1 B5 62.9(4) . . ? C13 C1 B6 116.6(5) . . ? C2 C1 B6 60.5(4) . . ? B4 C1 B6 113.1(5) . . ? B5 C1 B6 61.8(4) . . ? C13 C1 B3 118.4(5) . . ? C2 C1 B3 59.8(4) . . ? B4 C1 B3 61.9(4) . . ? B5 C1 B3 113.4(5) . . ? B6 C1 B3 112.2(5) . . ? C1 C2 B11 113.1(5) . . ? C1 C2 B3 62.6(4) . . ? B11 C2 B3 116.0(5) . . ? C1 C2 B7 114.0(5) . . ? B11 C2 B7 63.4(4) . . ? B3 C2 B7 63.4(4) . . ? C1 C2 B6 62.2(4) . . ? B11 C2 B6 62.6(4) . . ? B3 C2 B6 115.9(5) . . ? B7 C2 B6 115.8(5) . . ? C1 C2 H2 119.2 . . ? B11 C2 H2 117.8 . . ? B3 C2 H2 116.5 . . ? B7 C2 H2 117.1 . . ? B6 C2 H2 117.1 . . ? C18 C13 C14 119.7(7) . . ? C18 C13 C1 122.2(6) . . ? C14 C13 C1 118.2(6) . . ? C13 C14 C15 120.6(7) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C16 C15 C14 119.8(7) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 119.7(7) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C16 C17 C18 120.4(8) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C13 C18 C17 119.8(7) . . ? C13 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C2 B3 C1 57.6(4) . . ? C2 B3 B8 104.7(5) . . ? C1 B3 B8 106.0(5) . . ? C2 B3 B4 103.6(5) . . ? C1 B3 B4 57.9(4) . . ? B8 B3 B4 61.0(4) . . ? C2 B3 B7 58.3(4) . . ? C1 B3 B7 105.9(5) . . ? B8 B3 B7 60.6(5) . . ? B4 B3 B7 108.7(5) . . ? C2 B3 H3 125.2 . . ? C1 B3 H3 123.9 . . ? B8 B3 H3 122.1 . . ? B4 B3 H3 122.4 . . ? B7 B3 H3 121.4 . . ? C1 B4 B3 60.2(4) . . ? C1 B4 B9 106.2(5) . . ? B3 B4 B9 107.9(5) . . ? C1 B4 B5 59.3(4) . . ? B3 B4 B5 109.1(5) . . ? B9 B4 B5 60.3(4) . . ? C1 B4 B8 106.1(5) . . ? B3 B4 B8 58.9(4) . . ? B9 B4 B8 60.7(4) . . ? B5 B4 B8 109.1(5) . . ? C1 B4 H4 123.3 . . ? B3 B4 H4 121.5 . . ? B9 B4 H4 121.9 . . ? B5 B4 H4 120.8 . . ? B8 B4 H4 122.0 . . ? C1 B5 B6 59.5(4) . . ? C1 B5 B4 57.9(4) . . ? B6 B5 B4 107.2(5) . . ? C1 B5 B10 105.0(5) . . ? B6 B5 B10 58.9(4) . . ? B4 B5 B10 107.7(5) . . ? C1 B5 B9 104.4(5) . . ? B6 B5 B9 107.5(5) . . ? B4 B5 B9 59.5(4) . . ? B10 B5 B9 60.8(4) . . ? C1 B5 H5 124.5 . . ? B6 B5 H5 121.9 . . ? B4 B5 H5 122.2 . . ? B10 B5 H5 122.2 . . ? B9 B5 H5 122.4 . . ? C2 B6 C1 57.3(4) . . ? C2 B6 B10 104.1(5) . . ? C1 B6 B10 105.8(5) . . ? C2 B6 B11 57.8(4) . . ? C1 B6 B11 105.2(5) . . ? B10 B6 B11 60.5(4) . . ? C2 B6 B5 104.1(5) . . ? C1 B6 B5 58.7(4) . . ? B10 B6 B5 60.8(4) . . ? B11 B6 B5 108.8(5) . . ? C2 B6 H6 125.5 . . ? C1 B6 H6 124.0 . . ? B10 B6 H6 122.4 . . ? B11 B6 H6 121.8 . . ? B5 B6 H6 121.9 . . ? C2 B7 B11 57.8(4) . . ? C2 B7 B12 103.7(5) . . ? B11 B7 B12 60.3(4) . . ? C2 B7 B8 103.2(5) . . ? B11 B7 B8 108.3(5) . . ? B12 B7 B8 60.8(4) . . ? C2 B7 B3 58.2(4) . . ? B11 B7 B3 107.1(5) . . ? B12 B7 B3 107.4(5) . . ? B8 B7 B3 58.7(4) . . ? C2 B7 H7 125.9 . . ? B11 B7 H7 121.5 . . ? B12 B7 H7 122.2 . . ? B8 B7 H7 122.6 . . ? B3 B7 H7 122.3 . . ? B3 B8 B7 60.7(4) . . ? B3 B8 B4 60.1(4) . . ? B7 B8 B4 108.1(5) . . ? B3 B8 B9 107.7(5) . . ? B7 B8 B9 107.6(5) . . ? B4 B8 B9 59.3(4) . . ? B3 B8 B12 107.8(5) . . ? B7 B8 B12 59.4(4) . . ? B4 B8 B12 107.0(5) . . ? B9 B8 B12 59.8(4) . . ? B3 B8 I8 119.5(5) . . ? B7 B8 I8 120.8(5) . . ? B4 B8 I8 121.8(5) . . ? B9 B8 I8 123.8(5) . . ? B12 B8 I8 123.7(5) . . ? B4 B9 B5 60.2(4) . . ? B4 B9 B12 107.9(5) . . ? B5 B9 B12 107.9(5) . . ? B4 B9 B8 60.0(4) . . ? B5 B9 B8 108.4(5) . . ? B12 B9 B8 60.2(4) . . ? B4 B9 B10 107.4(5) . . ? B5 B9 B10 59.6(4) . . ? B12 B9 B10 59.8(4) . . ? B8 B9 B10 107.8(5) . . ? B4 B9 I9 120.5(5) . . ? B5 B9 I9 121.8(4) . . ? B12 B9 I9 122.5(4) . . ? B8 B9 I9 120.3(5) . . ? B10 B9 I9 123.9(4) . . ? B6 B10 B11 60.0(4) . . ? B6 B10 B5 60.3(4) . . ? B11 B10 B5 108.0(5) . . ? B6 B10 B12 108.1(5) . . ? B11 B10 B12 59.9(4) . . ? B5 B10 B12 107.9(5) . . ? B6 B10 B9 107.6(5) . . ? B11 B10 B9 107.3(5) . . ? B5 B10 B9 59.6(4) . . ? B12 B10 B9 59.7(4) . . ? B6 B10 I10 121.0(4) . . ? B11 B10 I10 120.0(4) . . ? B5 B10 I10 123.3(4) . . ? B12 B10 I10 121.0(4) . . ? B9 B10 I10 123.9(4) . . ? C2 B11 B6 59.6(4) . . ? C2 B11 B10 104.7(5) . . ? B6 B11 B10 59.5(4) . . ? C2 B11 B7 58.8(4) . . ? B6 B11 B7 109.6(5) . . ? B10 B11 B7 109.1(5) . . ? C2 B11 B12 104.2(5) . . ? B6 B11 B12 108.3(5) . . ? B10 B11 B12 60.7(4) . . ? B7 B11 B12 59.9(4) . . ? C2 B11 H11 124.9 . . ? B6 B11 H11 120.8 . . ? B10 B11 H11 122.1 . . ? B7 B11 H11 120.7 . . ? B12 B11 H11 122.5 . . ? B7 B12 B11 59.8(4) . . ? B7 B12 B9 108.1(5) . . ? B11 B12 B9 107.5(5) . . ? B7 B12 B10 108.0(5) . . ? B11 B12 B10 59.4(4) . . ? B9 B12 B10 60.5(4) . . ? B7 B12 B8 59.8(4) . . ? B11 B12 B8 107.2(5) . . ? B9 B12 B8 60.0(4) . . ? B10 B12 B8 108.3(5) . . ? B7 B12 I12 120.6(5) . . ? B11 B12 I12 121.8(5) . . ? B9 B12 I12 122.6(4) . . ? B10 B12 I12 122.2(4) . . ? B8 B12 I12 121.8(5) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C2 H2 I9 1.12 2.87 3.754(6) 135.4 2 C2 H2 I10 1.12 3.18 3.980(6) 129.3 2 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.74 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.228 _refine_diff_density_min -1.504 _refine_diff_density_rms 0.182 #===END