Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_compound_1 _database_code_depnum_ccdc_archive 'CCDC 616221' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C6 H26 B20 Se' _chemical_formula_sum 'C6 H26 B20 Se' _chemical_formula_weight 393.43 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' Se Se -0.0929 2.2259 '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 13.9969(3) _cell_length_b 11.7558(5) _cell_length_c 14.2199(5) _cell_angle_alpha 90.00 _cell_angle_beta 118.572(2) _cell_angle_gamma 90.00 _cell_volume 2054.86(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3715 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 25.682 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.272 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 1.816 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 6748 _diffrn_reflns_av_R_equivalents 0.0371 _diffrn_reflns_av_sigmaI/netI 0.0531 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 25.64 _reflns_number_total 3776 _reflns_number_gt 2969 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _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. ; _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^)+(0.0295P)^2^+1.7067P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3776 _refine_ls_number_parameters 246 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0541 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0804 _refine_ls_wR_factor_gt 0.0745 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 Se Se 0.13118(2) -0.03464(2) 0.94488(2) 0.01955(10) Uani 1 d . . . C1 C 0.26714(19) -0.1132(2) 1.0319(2) 0.0145(6) Uani 1 d . . . C2 C 0.3064(2) -0.1311(2) 1.1640(2) 0.0171(6) Uani 1 d . . . B3 B 0.2375(3) -0.2394(3) 1.0746(3) 0.0227(7) Uani 1 d . . . H3 H 0.1532 -0.2673 1.0541 0.027 Uiso 1 calc R . . B4 B 0.2836(3) -0.2368(3) 0.9773(3) 0.0224(7) Uani 1 d . . . H4 H 0.2303 -0.2647 0.8926 0.027 Uiso 1 calc R . . B5 B 0.3755(2) -0.1205(3) 1.0084(2) 0.0175(7) Uani 1 d . . . H5 H 0.3827 -0.0723 0.9441 0.021 Uiso 1 calc R . . B6 B 0.3853(2) -0.0515(3) 1.1252(2) 0.0142(6) Uani 1 d . . . H6 H 0.3973 0.0425 1.1379 0.017 Uiso 1 calc R . . B7 B 0.3514(3) -0.2660(3) 1.2015(3) 0.0249(8) Uani 1 d . . . H7 H 0.3429 -0.3138 1.2653 0.030 Uiso 1 calc R . . B8 B 0.3396(3) -0.3351(3) 1.0852(3) 0.0278(8) Uani 1 d . . . H8 H 0.3239 -0.4287 1.0722 0.033 Uiso 1 calc R . . B9 B 0.4258(3) -0.2611(3) 1.0452(3) 0.0237(8) Uani 1 d . . . H9 H 0.4678 -0.3064 1.0059 0.028 Uiso 1 calc R . . B10 B 0.4888(3) -0.1453(3) 1.1360(3) 0.0205(7) Uani 1 d . . . H10 H 0.5717 -0.1130 1.1564 0.025 Uiso 1 calc R . . B11 B 0.4433(2) -0.1512(3) 1.2334(3) 0.0210(7) Uani 1 d . . . H11 H 0.4959 -0.1234 1.3182 0.025 Uiso 1 calc R . . B12 B 0.4674(3) -0.2790(3) 1.1826(3) 0.0234(8) Uani 1 d . . . H12 H 0.5371 -0.3362 1.2338 0.028 Uiso 1 calc R . . C13 C 0.2462(2) -0.0678(3) 1.2120(2) 0.0277(7) Uani 1 d . . . H13A H 0.2940 -0.0097 1.2617 0.042 Uiso 1 calc R . . H13B H 0.2240 -0.1213 1.2507 0.042 Uiso 1 calc R . . H13C H 0.1816 -0.0312 1.1548 0.042 Uiso 1 calc R . . C21 C 0.1585(2) 0.1240(2) 0.93093(19) 0.0140(6) Uani 1 d . . . C22 C 0.1637(2) 0.1642(2) 0.8177(2) 0.0171(6) Uani 1 d . . . B23 B 0.0428(2) 0.1771(3) 0.8222(2) 0.0217(7) Uani 1 d . . . H23 H -0.0313 0.1248 0.7718 0.026 Uiso 1 calc R . . B24 B 0.0799(3) 0.2169(3) 0.9567(3) 0.0213(7) Uani 1 d . . . H24 H 0.0293 0.1922 0.9952 0.026 Uiso 1 calc R . . B25 B 0.2238(2) 0.2202(3) 1.0313(3) 0.0192(7) Uani 1 d . . . H25 H 0.2679 0.1981 1.1185 0.023 Uiso 1 calc R . . B26 B 0.2762(2) 0.1825(3) 0.9424(2) 0.0152(7) Uani 1 d . . . H26 H 0.3541 0.1342 0.9703 0.018 Uiso 1 calc R . . B27 B 0.0888(3) 0.2850(3) 0.7664(3) 0.0233(8) Uani 1 d . . . H27 H 0.0441 0.3059 0.6789 0.028 Uiso 1 calc R . . B28 B 0.0355(3) 0.3209(3) 0.8539(3) 0.0241(8) Uani 1 d . . . H28 H -0.0444 0.3657 0.8245 0.029 Uiso 1 calc R . . B29 B 0.1482(3) 0.3489(3) 0.9827(3) 0.0247(8) Uani 1 d . . . H29 H 0.1427 0.4134 1.0379 0.030 Uiso 1 calc R . . B30 B 0.2713(3) 0.3269(3) 0.9752(3) 0.0227(7) Uani 1 d . . . H30 H 0.3475 0.3760 1.0260 0.027 Uiso 1 calc R . . B31 B 0.2329(3) 0.2882(3) 0.8409(3) 0.0217(7) Uani 1 d . . . H31 H 0.2838 0.3113 0.8024 0.026 Uiso 1 calc R . . B32 B 0.1549(3) 0.3910(3) 0.8655(3) 0.0259(8) Uani 1 d . . . H32 H 0.1544 0.4828 0.8440 0.031 Uiso 1 calc R . . C33 C 0.1697(2) 0.0729(3) 0.7457(2) 0.0248(7) Uani 1 d . . . H33A H 0.2058 0.1035 0.7067 0.037 Uiso 1 calc R . . H33B H 0.0960 0.0481 0.6945 0.037 Uiso 1 calc R . . H33C H 0.2112 0.0079 0.7893 0.037 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Se 0.01262(15) 0.01708(16) 0.02297(16) 0.00512(14) 0.00370(11) -0.00113(12) C1 0.0145(13) 0.0145(15) 0.0131(14) 0.0007(11) 0.0056(10) -0.0009(11) C2 0.0192(14) 0.0195(16) 0.0128(14) 0.0036(12) 0.0078(11) 0.0000(11) B3 0.0255(17) 0.0124(18) 0.0260(19) 0.0056(14) 0.0089(14) -0.0021(14) B4 0.0236(17) 0.0179(19) 0.0200(18) -0.0046(14) 0.0060(14) 0.0019(14) B5 0.0158(15) 0.0205(19) 0.0187(16) -0.0013(14) 0.0103(13) 0.0027(13) B6 0.0129(14) 0.0156(18) 0.0123(15) -0.0006(13) 0.0047(11) -0.0012(12) B7 0.0283(18) 0.0186(19) 0.0291(19) 0.0088(15) 0.0146(15) 0.0018(14) B8 0.0313(19) 0.0129(19) 0.030(2) 0.0014(15) 0.0077(15) 0.0013(14) B9 0.0271(18) 0.022(2) 0.0215(18) -0.0026(15) 0.0112(14) 0.0068(15) B10 0.0207(16) 0.0214(19) 0.0190(17) 0.0027(14) 0.0092(13) 0.0039(14) B11 0.0198(16) 0.025(2) 0.0162(17) 0.0061(14) 0.0070(13) 0.0032(14) B12 0.0226(17) 0.0200(19) 0.0239(18) 0.0048(15) 0.0082(14) 0.0059(14) C13 0.0300(16) 0.035(2) 0.0264(17) 0.0030(14) 0.0203(14) 0.0051(14) C21 0.0155(13) 0.0160(15) 0.0104(13) 0.0043(11) 0.0062(10) 0.0049(11) C22 0.0198(14) 0.0189(16) 0.0140(14) 0.0045(12) 0.0092(11) 0.0028(12) B23 0.0155(16) 0.030(2) 0.0167(17) 0.0084(15) 0.0055(13) 0.0058(14) B24 0.0221(17) 0.025(2) 0.0211(17) 0.0054(15) 0.0140(14) 0.0114(14) B25 0.0233(17) 0.0184(19) 0.0170(17) -0.0001(14) 0.0106(13) 0.0042(14) B26 0.0167(15) 0.0138(17) 0.0149(16) 0.0014(13) 0.0075(12) 0.0005(12) B27 0.0245(17) 0.0229(19) 0.0220(18) 0.0088(15) 0.0108(14) 0.0087(14) B28 0.0241(17) 0.026(2) 0.0251(18) 0.0082(15) 0.0142(14) 0.0096(14) B29 0.0333(19) 0.0192(19) 0.0239(18) 0.0038(15) 0.0155(15) 0.0112(15) B30 0.0276(18) 0.0131(18) 0.0260(19) 0.0000(15) 0.0117(14) -0.0002(14) B31 0.0248(17) 0.0178(18) 0.0257(19) 0.0057(15) 0.0145(14) 0.0035(14) B32 0.0318(19) 0.0165(19) 0.033(2) 0.0063(16) 0.0187(16) 0.0073(15) C33 0.0331(17) 0.0249(18) 0.0179(15) -0.0009(13) 0.0133(13) 0.0035(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Se C21 1.933(3) . ? Se C1 1.937(3) . ? C1 C2 1.699(3) . ? C1 B5 1.703(4) . ? C1 B6 1.710(4) . ? C1 B4 1.714(4) . ? C1 B3 1.727(4) . ? C2 C13 1.511(4) . ? C2 B7 1.696(4) . ? C2 B11 1.701(4) . ? C2 B6 1.725(4) . ? C2 B3 1.731(4) . ? B3 B8 1.768(5) . ? B3 B7 1.773(5) . ? B3 B4 1.786(5) . ? B3 H3 1.1200 . ? B4 B9 1.771(4) . ? B4 B8 1.776(5) . ? B4 B5 1.781(5) . ? B4 H4 1.1200 . ? B5 B10 1.772(4) . ? B5 B9 1.775(5) . ? B5 B6 1.795(4) . ? B5 H5 1.1200 . ? B6 B10 1.768(4) . ? B6 B11 1.790(4) . ? B6 H6 1.1200 . ? B7 B11 1.768(5) . ? B7 B12 1.775(4) . ? B7 B8 1.777(5) . ? B7 H7 1.1200 . ? B8 B12 1.784(5) . ? B8 B9 1.787(5) . ? B8 H8 1.1200 . ? B9 B12 1.765(5) . ? B9 B10 1.792(5) . ? B9 H9 1.1200 . ? B10 B11 1.781(4) . ? B10 B12 1.786(5) . ? B10 H10 1.1200 . ? B11 B12 1.768(5) . ? B11 H11 1.1200 . ? B12 H12 1.1200 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C21 B25 1.703(4) . ? C21 B24 1.709(4) . ? C21 C22 1.712(3) . ? C21 B26 1.720(4) . ? C21 B23 1.734(4) . ? C22 C33 1.514(4) . ? C22 B31 1.693(4) . ? C22 B27 1.707(4) . ? C22 B23 1.730(4) . ? C22 B26 1.733(4) . ? B23 B28 1.766(5) . ? B23 B27 1.772(5) . ? B23 B24 1.788(4) . ? B23 H23 1.1200 . ? B24 B29 1.767(5) . ? B24 B25 1.772(4) . ? B24 B28 1.775(5) . ? B24 H24 1.1200 . ? B25 B30 1.778(5) . ? B25 B29 1.786(5) . ? B25 B26 1.794(4) . ? B25 H25 1.1200 . ? B26 B30 1.771(4) . ? B26 B31 1.777(4) . ? B26 H26 1.1200 . ? B27 B31 1.774(4) . ? B27 B32 1.775(5) . ? B27 B28 1.781(4) . ? B27 H27 1.1200 . ? B28 B29 1.785(5) . ? B28 B32 1.799(5) . ? B28 H28 1.1200 . ? B29 B32 1.783(5) . ? B29 B30 1.796(4) . ? B29 H29 1.1200 . ? B30 B31 1.778(5) . ? B30 B32 1.796(5) . ? B30 H30 1.1200 . ? B31 B32 1.772(5) . ? B31 H31 1.1200 . ? B32 H32 1.1200 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C21 Se C1 110.11(11) . . ? C2 C1 B5 111.27(19) . . ? C2 C1 B6 60.80(15) . . ? B5 C1 B6 63.43(16) . . ? C2 C1 B4 110.7(2) . . ? B5 C1 B4 62.83(18) . . ? B6 C1 B4 114.9(2) . . ? C2 C1 B3 60.68(17) . . ? B5 C1 B3 114.4(2) . . ? B6 C1 B3 113.4(2) . . ? B4 C1 B3 62.54(19) . . ? C2 C1 Se 117.67(16) . . ? B5 C1 Se 126.39(18) . . ? B6 C1 Se 125.67(19) . . ? B4 C1 Se 114.77(17) . . ? B3 C1 Se 107.83(17) . . ? C13 C2 B7 121.4(2) . . ? C13 C2 C1 118.9(2) . . ? B7 C2 C1 109.8(2) . . ? C13 C2 B11 121.6(2) . . ? B7 C2 B11 62.73(18) . . ? C1 C2 B11 109.77(19) . . ? C13 C2 B6 117.3(2) . . ? B7 C2 B6 114.2(2) . . ? C1 C2 B6 59.91(15) . . ? B11 C2 B6 62.99(17) . . ? C13 C2 B3 117.3(2) . . ? B7 C2 B3 62.30(19) . . ? C1 C2 B3 60.45(16) . . ? B11 C2 B3 113.7(2) . . ? B6 C2 B3 112.4(2) . . ? C1 B3 C2 58.86(16) . . ? C1 B3 B8 104.8(2) . . ? C2 B3 B8 105.1(2) . . ? C1 B3 B7 105.0(2) . . ? C2 B3 B7 57.90(18) . . ? B8 B3 B7 60.25(19) . . ? C1 B3 B4 58.37(17) . . ? C2 B3 B4 106.0(2) . . ? B8 B3 B4 59.98(19) . . ? B7 B3 B4 108.0(2) . . ? C1 B3 H3 124.1 . . ? C2 B3 H3 123.7 . . ? B8 B3 H3 122.9 . . ? B7 B3 H3 122.4 . . ? B4 B3 H3 121.9 . . ? C1 B4 B9 104.4(2) . . ? C1 B4 B8 105.0(2) . . ? B9 B4 B8 60.51(19) . . ? C1 B4 B5 58.30(16) . . ? B9 B4 B5 59.94(18) . . ? B8 B4 B5 108.5(2) . . ? C1 B4 B3 59.10(17) . . ? B9 B4 B3 107.7(2) . . ? B8 B4 B3 59.52(19) . . ? B5 B4 B3 107.8(2) . . ? C1 B4 H4 124.7 . . ? B9 B4 H4 122.4 . . ? B8 B4 H4 122.0 . . ? B5 B4 H4 121.5 . . ? B3 B4 H4 121.7 . . ? C1 B5 B10 104.6(2) . . ? C1 B5 B9 104.7(2) . . ? B10 B5 B9 60.68(19) . . ? C1 B5 B4 58.86(17) . . ? B10 B5 B4 108.3(2) . . ? B9 B5 B4 59.76(18) . . ? C1 B5 B6 58.46(15) . . ? B10 B5 B6 59.42(17) . . ? B9 B5 B6 107.7(2) . . ? B4 B5 B6 107.7(2) . . ? C1 B5 H5 124.8 . . ? B10 B5 H5 122.2 . . ? B9 B5 H5 122.3 . . ? B4 B5 H5 121.5 . . ? B6 B5 H5 122.0 . . ? C1 B6 C2 59.29(15) . . ? C1 B6 B10 104.5(2) . . ? C2 B6 B10 104.9(2) . . ? C1 B6 B11 105.2(2) . . ? C2 B6 B11 57.84(16) . . ? B10 B6 B11 60.08(17) . . ? C1 B6 B5 58.11(15) . . ? C2 B6 B5 105.9(2) . . ? B10 B6 B5 59.66(17) . . ? B11 B6 B5 107.6(2) . . ? C1 B6 H6 124.0 . . ? C2 B6 H6 123.6 . . ? B10 B6 H6 123.2 . . ? B11 B6 H6 122.5 . . ? B5 B6 H6 122.3 . . ? C2 B7 B11 58.75(17) . . ? C2 B7 B3 59.80(18) . . ? B11 B7 B3 108.4(2) . . ? C2 B7 B12 105.2(2) . . ? B11 B7 B12 59.88(19) . . ? B3 B7 B12 107.7(2) . . ? C2 B7 B8 106.2(2) . . ? B11 B7 B8 108.7(2) . . ? B3 B7 B8 59.75(19) . . ? B12 B7 B8 60.30(19) . . ? C2 B7 H7 123.8 . . ? B11 B7 H7 121.3 . . ? B3 B7 H7 121.4 . . ? B12 B7 H7 122.5 . . ? B8 B7 H7 121.7 . . ? B3 B8 B4 60.50(18) . . ? B3 B8 B7 60.01(19) . . ? B4 B8 B7 108.2(2) . . ? B3 B8 B12 107.5(2) . . ? B4 B8 B12 107.1(2) . . ? B7 B8 B12 59.78(18) . . ? B3 B8 B9 107.7(2) . . ? B4 B8 B9 59.61(18) . . ? B7 B8 B9 107.3(2) . . ? B12 B8 B9 59.24(18) . . ? B3 B8 H8 121.6 . . ? B4 B8 H8 121.7 . . ? B7 B8 H8 121.7 . . ? B12 B8 H8 122.4 . . ? B9 B8 H8 122.3 . . ? B12 B9 B4 108.2(2) . . ? B12 B9 B5 108.2(2) . . ? B4 B9 B5 60.30(18) . . ? B12 B9 B8 60.28(19) . . ? B4 B9 B8 59.89(19) . . ? B5 B9 B8 108.3(2) . . ? B12 B9 B10 60.29(19) . . ? B4 B9 B10 107.9(2) . . ? B5 B9 B10 59.58(18) . . ? B8 B9 B10 108.3(2) . . ? B12 B9 H9 121.4 . . ? B4 B9 H9 121.7 . . ? B5 B9 H9 121.7 . . ? B8 B9 H9 121.5 . . ? B10 B9 H9 121.8 . . ? B6 B10 B5 60.93(17) . . ? B6 B10 B11 60.58(17) . . ? B5 B10 B11 109.0(2) . . ? B6 B10 B12 107.8(2) . . ? B5 B10 B12 107.3(2) . . ? B11 B10 B12 59.42(19) . . ? B6 B10 B9 108.2(2) . . ? B5 B10 B9 59.73(18) . . ? B11 B10 B9 107.2(2) . . ? B12 B10 B9 59.12(19) . . ? B6 B10 H10 121.1 . . ? B5 B10 H10 121.3 . . ? B11 B10 H10 121.6 . . ? B12 B10 H10 122.6 . . ? B9 B10 H10 122.4 . . ? C2 B11 B7 58.52(17) . . ? C2 B11 B12 105.3(2) . . ? B7 B11 B12 60.24(19) . . ? C2 B11 B10 105.4(2) . . ? B7 B11 B10 108.5(2) . . ? B12 B11 B10 60.44(19) . . ? C2 B11 B6 59.17(16) . . ? B7 B11 B6 107.7(2) . . ? B12 B11 B6 107.6(2) . . ? B10 B11 B6 59.35(17) . . ? C2 B11 H11 124.2 . . ? B7 B11 H11 121.5 . . ? B12 B11 H11 122.1 . . ? B10 B11 H11 122.1 . . ? B6 B11 H11 121.9 . . ? B9 B12 B11 108.9(2) . . ? B9 B12 B7 108.4(2) . . ? B11 B12 B7 59.88(18) . . ? B9 B12 B8 60.48(19) . . ? B11 B12 B8 108.4(2) . . ? B7 B12 B8 59.93(19) . . ? B9 B12 B10 60.59(19) . . ? B11 B12 B10 60.13(18) . . ? B7 B12 B10 107.9(2) . . ? B8 B12 B10 108.7(2) . . ? B9 B12 H12 121.0 . . ? B11 B12 H12 121.4 . . ? B7 B12 H12 121.9 . . ? B8 B12 H12 121.4 . . ? B10 B12 H12 121.4 . . ? C2 C13 H13A 109.5 . . ? C2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? B25 C21 B24 62.57(18) . . ? B25 C21 C22 110.9(2) . . ? B24 C21 C22 110.3(2) . . ? B25 C21 B26 63.21(17) . . ? B24 C21 B26 114.2(2) . . ? C22 C21 B26 60.63(15) . . ? B25 C21 B23 114.0(2) . . ? B24 C21 B23 62.56(17) . . ? C22 C21 B23 60.25(15) . . ? B26 C21 B23 112.6(2) . . ? B25 C21 Se 127.41(17) . . ? B24 C21 Se 114.55(18) . . ? C22 C21 Se 117.52(17) . . ? B26 C21 Se 127.08(18) . . ? B23 C21 Se 107.02(18) . . ? C33 C22 B31 122.0(2) . . ? C33 C22 B27 121.5(2) . . ? B31 C22 B27 62.91(19) . . ? C33 C22 C21 118.8(2) . . ? B31 C22 C21 109.4(2) . . ? B27 C22 C21 109.8(2) . . ? C33 C22 B23 117.3(2) . . ? B31 C22 B23 113.3(2) . . ? B27 C22 B23 62.07(18) . . ? C21 C22 B23 60.50(15) . . ? C33 C22 B26 117.5(2) . . ? B31 C22 B26 62.50(17) . . ? B27 C22 B26 114.0(2) . . ? C21 C22 B26 59.90(15) . . ? B23 C22 B26 112.2(2) . . ? C22 B23 C21 59.25(15) . . ? C22 B23 B28 105.7(2) . . ? C21 B23 B28 105.1(2) . . ? C22 B23 B27 58.34(17) . . ? C21 B23 B27 105.8(2) . . ? B28 B23 B27 60.46(19) . . ? C22 B23 B24 105.9(2) . . ? C21 B23 B24 58.03(16) . . ? B28 B23 B24 59.91(19) . . ? B27 B23 B24 108.0(2) . . ? C22 B23 H23 123.4 . . ? C21 B23 H23 123.8 . . ? B28 B23 H23 122.7 . . ? B27 B23 H23 122.0 . . ? B24 B23 H23 122.3 . . ? C21 B24 B29 105.5(2) . . ? C21 B24 B25 58.56(16) . . ? B29 B24 B25 60.62(19) . . ? C21 B24 B28 105.8(2) . . ? B29 B24 B28 60.53(19) . . ? B25 B24 B28 109.2(2) . . ? C21 B24 B23 59.42(16) . . ? B29 B24 B23 107.8(2) . . ? B25 B24 B23 108.2(2) . . ? B28 B24 B23 59.42(18) . . ? C21 B24 H24 124.1 . . ? B29 B24 H24 122.0 . . ? B25 B24 H24 121.1 . . ? B28 B24 H24 121.8 . . ? B23 B24 H24 121.8 . . ? C21 B25 B24 58.87(17) . . ? C21 B25 B30 105.0(2) . . ? B24 B25 B30 108.0(2) . . ? C21 B25 B29 104.9(2) . . ? B24 B25 B29 59.55(19) . . ? B30 B25 B29 60.51(18) . . ? C21 B25 B26 58.85(16) . . ? B24 B25 B26 107.7(2) . . ? B30 B25 B26 59.45(17) . . ? B29 B25 B26 107.6(2) . . ? C21 B25 H25 124.4 . . ? B24 B25 H25 121.7 . . ? B30 B25 H25 122.2 . . ? B29 B25 H25 122.4 . . ? B26 B25 H25 121.9 . . ? C21 B26 C22 59.47(15) . . ? C21 B26 B30 104.6(2) . . ? C22 B26 B30 104.9(2) . . ? C21 B26 B31 105.2(2) . . ? C22 B26 B31 57.65(17) . . ? B30 B26 B31 60.14(18) . . ? C21 B26 B25 57.94(16) . . ? C22 B26 B25 105.9(2) . . ? B30 B26 B25 59.82(18) . . ? B31 B26 B25 107.6(2) . . ? C21 B26 H26 123.9 . . ? C22 B26 H26 123.6 . . ? B30 B26 H26 123.1 . . ? B31 B26 H26 122.5 . . ? B25 B26 H26 122.3 . . ? C22 B27 B23 59.60(17) . . ? C22 B27 B31 58.14(17) . . ? B23 B27 B31 107.5(2) . . ? C22 B27 B32 105.3(2) . . ? B23 B27 B32 108.1(2) . . ? B31 B27 B32 59.89(18) . . ? C22 B27 B28 106.0(2) . . ? B23 B27 B28 59.59(19) . . ? B31 B27 B28 108.3(2) . . ? B32 B27 B28 60.78(19) . . ? C22 B27 H27 124.0 . . ? B23 B27 H27 121.7 . . ? B31 B27 H27 122.0 . . ? B32 B27 H27 122.0 . . ? B28 B27 H27 121.8 . . ? B23 B28 B24 60.67(18) . . ? B23 B28 B27 59.96(19) . . ? B24 B28 B27 108.3(2) . . ? B23 B28 B29 108.0(2) . . ? B24 B28 B29 59.52(19) . . ? B27 B28 B29 107.5(2) . . ? B23 B28 B32 107.3(2) . . ? B24 B28 B32 107.2(2) . . ? B27 B28 B32 59.45(19) . . ? B29 B28 B32 59.67(18) . . ? B23 B28 H28 121.6 . . ? B24 B28 H28 121.7 . . ? B27 B28 H28 121.8 . . ? B29 B28 H28 122.0 . . ? B32 B28 H28 122.5 . . ? B24 B29 B32 108.3(2) . . ? B24 B29 B28 59.95(19) . . ? B32 B29 B28 60.56(19) . . ? B24 B29 B25 59.83(18) . . ? B32 B29 B25 108.1(2) . . ? B28 B29 B25 108.1(2) . . ? B24 B29 B30 107.4(2) . . ? B32 B29 B30 60.24(18) . . ? B28 B29 B30 108.4(2) . . ? B25 B29 B30 59.52(18) . . ? B24 B29 H29 122.0 . . ? B32 B29 H29 121.3 . . ? B28 B29 H29 121.4 . . ? B25 B29 H29 121.9 . . ? B30 B29 H29 121.9 . . ? B26 B30 B31 60.10(18) . . ? B26 B30 B25 60.74(17) . . ? B31 B30 B25 108.3(2) . . ? B26 B30 B29 108.2(2) . . ? B31 B30 B29 107.1(2) . . ? B25 B30 B29 59.97(18) . . ? B26 B30 B32 107.9(2) . . ? B31 B30 B32 59.44(18) . . ? B25 B30 B32 107.9(2) . . ? B29 B30 B32 59.53(18) . . ? B26 B30 H30 121.3 . . ? B31 B30 H30 122.1 . . ? B25 B30 H30 121.3 . . ? B29 B30 H30 122.1 . . ? B32 B30 H30 122.1 . . ? C22 B31 B32 106.1(2) . . ? C22 B31 B27 58.95(18) . . ? B32 B31 B27 60.09(19) . . ? C22 B31 B26 59.85(17) . . ? B32 B31 B26 108.7(2) . . ? B27 B31 B26 108.6(2) . . ? C22 B31 B30 106.3(2) . . ? B32 B31 B30 60.79(19) . . ? B27 B31 B30 108.7(2) . . ? B26 B31 B30 59.76(17) . . ? C22 B31 H31 123.5 . . ? B32 B31 H31 121.7 . . ? B27 B31 H31 121.3 . . ? B26 B31 H31 121.1 . . ? B30 B31 H31 121.7 . . ? B31 B32 B27 60.03(18) . . ? B31 B32 B29 107.9(2) . . ? B27 B32 B29 107.8(2) . . ? B31 B32 B30 59.77(18) . . ? B27 B32 B30 107.9(2) . . ? B29 B32 B30 60.23(18) . . ? B31 B32 B28 107.6(2) . . ? B27 B32 B28 59.77(19) . . ? B29 B32 B28 59.77(18) . . ? B30 B32 B28 107.7(2) . . ? B31 B32 H32 121.9 . . ? B27 B32 H32 121.8 . . ? B29 B32 H32 121.7 . . ? B30 B32 H32 121.8 . . ? B28 B32 H32 122.1 . . ? C22 C33 H33A 109.5 . . ? C22 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C22 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 C1 Se C21 96.71(19) . . . . ? C22 C21 Se C1 97.07(18) . . . . ? Se C1 C2 C13 -10.9(3) . . . . ? Se C21 C22 C33 -12.2(3) . . . . ? C33 C22 C2 C13 -151.5(2) . . . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 25.64 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.368 _refine_diff_density_min -0.442 _refine_diff_density_rms 0.072 data_compound_2 _database_code_depnum_ccdc_archive 'CCDC 616222' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C6 H26 B20 Se2' _chemical_formula_sum 'C6 H26 B20 Se2' _chemical_formula_weight 472.39 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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.1599(4) _cell_length_b 7.8129(5) _cell_length_c 21.7731(15) _cell_angle_alpha 95.738(2) _cell_angle_beta 90.839(2) _cell_angle_gamma 115.038(3) _cell_volume 1095.80(12) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3090 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 25.028 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.432 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 460 _exptl_absorpt_coefficient_mu 3.365 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 6010 _diffrn_reflns_av_R_equivalents 0.0455 _diffrn_reflns_av_sigmaI/netI 0.0879 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 25.04 _reflns_number_total 3700 _reflns_number_gt 2695 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _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. ; _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^)+(0.0675P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3700 _refine_ls_number_parameters 255 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0805 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.1339 _refine_ls_wR_factor_gt 0.1199 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 Se1 Se 0.52163(9) 0.39062(8) 0.28040(3) 0.0310(2) Uani 1 d . . . Se2 Se 0.41817(8) 0.41956(7) 0.18293(3) 0.0303(2) Uani 1 d . . . C1 C 0.4067(8) 0.5336(7) 0.3332(2) 0.0227(11) Uani 1 d . . . C2 C 0.2095(8) 0.4094(7) 0.3767(3) 0.0261(12) Uani 1 d . . . B3 B 0.4559(9) 0.5304(9) 0.4102(3) 0.0257(14) Uani 1 d . . . H3 H 0.5485 0.4586 0.4279 0.031 Uiso 1 calc R . . B4 B 0.5729(9) 0.7431(8) 0.3746(3) 0.0274(14) Uani 1 d . . . H4 H 0.7438 0.8148 0.3701 0.033 Uiso 1 calc R . . B5 B 0.3913(10) 0.7326(8) 0.3151(3) 0.0278(14) Uani 1 d . . . H5 H 0.4416 0.7969 0.2711 0.033 Uiso 1 calc R . . B6 B 0.1670(9) 0.5168(9) 0.3160(3) 0.0287(15) Uani 1 d . . . H6 H 0.0710 0.4364 0.2727 0.034 Uiso 1 calc R . . B7 B 0.2371(10) 0.5328(9) 0.4469(3) 0.0298(15) Uani 1 d . . . H7 H 0.1855 0.4652 0.4903 0.036 Uiso 1 calc R . . B8 B 0.4645(10) 0.7460(9) 0.4469(3) 0.0303(15) Uani 1 d . . . H8 H 0.5629 0.8199 0.4904 0.036 Uiso 1 calc R . . B9 B 0.4257(10) 0.8741(9) 0.3874(3) 0.0324(15) Uani 1 d . . . H9 H 0.4984 1.0333 0.3914 0.039 Uiso 1 calc R . . B10 B 0.1728(10) 0.7331(9) 0.3515(3) 0.0292(15) Uani 1 d . . . H10 H 0.0779 0.7999 0.3317 0.035 Uiso 1 calc R . . B11 B 0.0571(10) 0.5247(9) 0.3885(3) 0.0295(15) Uani 1 d . . . H11 H -0.1138 0.4523 0.3929 0.035 Uiso 1 calc R . . B12 B 0.2171(10) 0.7439(9) 0.4328(3) 0.0331(16) Uani 1 d . . . H12 H 0.1526 0.8184 0.4669 0.040 Uiso 1 calc R . . C13 C 0.1189(9) 0.1936(8) 0.3679(3) 0.0386(15) Uani 1 d . . . H13A H -0.0136 0.1416 0.3872 0.058 Uiso 1 calc R . . H13B H 0.2144 0.1518 0.3873 0.058 Uiso 1 calc R . . H13C H 0.0975 0.1482 0.3236 0.058 Uiso 1 calc R . . C21 C 0.6636(8) 0.6240(7) 0.1563(2) 0.0209(11) Uani 1 d . . . C22 C 0.7876(8) 0.5580(7) 0.0991(3) 0.0251(12) Uani 1 d . . . B23 B 0.6273(9) 0.6613(8) 0.0819(3) 0.0255(14) Uani 1 d . . . H23 H 0.4781 0.5835 0.0533 0.031 Uiso 1 calc R . . B24 B 0.6574(9) 0.8350(8) 0.1460(3) 0.0251(14) Uani 1 d . . . H24 H 0.5298 0.8757 0.1592 0.030 Uiso 1 calc R . . B25 B 0.8296(9) 0.8164(8) 0.2025(3) 0.0249(13) Uani 1 d . . . H25 H 0.8152 0.8438 0.2533 0.030 Uiso 1 calc R . . B26 B 0.9038(10) 0.6362(9) 0.1719(3) 0.0272(14) Uani 1 d . . . H26 H 0.9359 0.5427 0.2022 0.033 Uiso 1 calc R . . B27 B 0.8665(9) 0.7239(9) 0.0494(3) 0.0280(14) Uani 1 d . . . H27 H 0.8765 0.6909 -0.0014 0.034 Uiso 1 calc R . . B28 B 0.7917(10) 0.9041(9) 0.0790(3) 0.0285(14) Uani 1 d . . . H28 H 0.7532 0.9921 0.0479 0.034 Uiso 1 calc R . . B29 B 0.9201(10) 1.0012(9) 0.1535(3) 0.0311(15) Uani 1 d . . . H29 H 0.9679 1.1538 0.1719 0.037 Uiso 1 calc R . . B30 B 1.0734(10) 0.8803(9) 0.1701(3) 0.0327(15) Uani 1 d . . . H30 H 1.2214 0.9522 0.1996 0.039 Uiso 1 calc R . . B31 B 1.0407(9) 0.7099(9) 0.1049(3) 0.0283(14) Uani 1 d . . . H31 H 1.1673 0.6684 0.0911 0.034 Uiso 1 calc R . . B32 B 1.0505(10) 0.9357(9) 0.0931(3) 0.0331(15) Uani 1 d . . . H32 H 1.1833 1.0443 0.0716 0.040 Uiso 1 calc R . . C33 C 0.7129(9) 0.3487(7) 0.0760(3) 0.0320(13) Uani 1 d . . . H33A H 0.5704 0.2982 0.0585 0.048 Uiso 1 calc R . . H33B H 0.7185 0.2791 0.1105 0.048 Uiso 1 calc R . . H33C H 0.8017 0.3337 0.0440 0.048 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Se1 0.0436(4) 0.0313(4) 0.0274(4) 0.0076(2) 0.0110(3) 0.0238(3) Se2 0.0291(3) 0.0280(3) 0.0234(3) -0.0002(2) 0.0040(2) 0.0026(2) C1 0.025(3) 0.026(3) 0.018(3) 0.001(2) 0.003(2) 0.012(2) C2 0.024(3) 0.026(3) 0.030(3) 0.004(2) 0.003(2) 0.012(2) B3 0.025(3) 0.030(4) 0.022(4) 0.006(3) -0.001(3) 0.011(3) B4 0.023(3) 0.019(3) 0.034(4) -0.003(3) 0.002(3) 0.005(3) B5 0.036(4) 0.024(3) 0.030(4) 0.006(3) 0.012(3) 0.018(3) B6 0.023(3) 0.032(4) 0.032(4) -0.001(3) -0.002(3) 0.013(3) B7 0.034(3) 0.031(4) 0.024(4) 0.006(3) 0.010(3) 0.013(3) B8 0.029(3) 0.031(4) 0.027(4) -0.002(3) 0.003(3) 0.011(3) B9 0.040(4) 0.025(4) 0.034(4) 0.004(3) 0.011(3) 0.015(3) B10 0.030(3) 0.026(3) 0.034(4) 0.000(3) 0.004(3) 0.014(3) B11 0.024(3) 0.032(4) 0.035(4) 0.005(3) 0.008(3) 0.014(3) B12 0.038(4) 0.026(4) 0.036(4) 0.007(3) 0.006(3) 0.014(3) C13 0.040(3) 0.033(3) 0.040(4) 0.008(3) 0.007(3) 0.012(3) C21 0.024(3) 0.024(3) 0.016(3) 0.001(2) 0.005(2) 0.013(2) C22 0.025(3) 0.026(3) 0.027(3) 0.000(2) 0.009(2) 0.014(2) B23 0.027(3) 0.031(4) 0.022(4) 0.008(3) 0.004(3) 0.014(3) B24 0.027(3) 0.021(3) 0.029(4) 0.000(3) -0.002(3) 0.013(3) B25 0.022(3) 0.024(3) 0.025(4) -0.002(2) 0.001(3) 0.007(2) B26 0.028(3) 0.030(4) 0.025(4) 0.002(3) 0.003(3) 0.015(3) B27 0.030(3) 0.027(3) 0.025(4) 0.000(3) 0.002(3) 0.011(3) B28 0.032(3) 0.027(3) 0.029(4) 0.004(3) 0.007(3) 0.016(3) B29 0.035(4) 0.025(4) 0.026(4) -0.004(3) -0.002(3) 0.008(3) B30 0.025(3) 0.039(4) 0.031(4) 0.003(3) 0.007(3) 0.011(3) B31 0.024(3) 0.031(4) 0.029(4) -0.002(3) 0.005(3) 0.013(3) B32 0.031(3) 0.026(4) 0.037(4) 0.006(3) 0.008(3) 0.006(3) C33 0.039(3) 0.026(3) 0.035(4) 0.001(2) 0.009(3) 0.018(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 Se1 C1 1.948(5) . ? Se1 Se2 2.3012(8) . ? Se2 C21 1.953(5) . ? C1 B5 1.689(7) . ? C1 B6 1.698(8) . ? C1 C2 1.701(7) . ? C1 B4 1.712(7) . ? C1 B3 1.713(8) . ? C2 C13 1.518(7) . ? C2 B7 1.686(8) . ? C2 B11 1.692(8) . ? C2 B3 1.718(8) . ? C2 B6 1.723(8) . ? B3 B8 1.767(9) . ? B3 B7 1.776(9) . ? B3 B4 1.778(9) . ? B3 H3 1.1200 . ? B4 B9 1.761(9) . ? B4 B8 1.768(9) . ? B4 B5 1.793(9) . ? B4 H4 1.1200 . ? B5 B10 1.765(9) . ? B5 B6 1.771(9) . ? B5 B9 1.781(9) . ? B5 H5 1.1200 . ? B6 B10 1.770(9) . ? B6 B11 1.781(9) . ? B6 H6 1.1200 . ? B7 B8 1.769(9) . ? B7 B12 1.771(9) . ? B7 B11 1.775(9) . ? B7 H7 1.1200 . ? B8 B12 1.786(9) . ? B8 B9 1.800(9) . ? B8 H8 1.1200 . ? B9 B12 1.788(9) . ? B9 B10 1.789(9) . ? B9 H9 1.1200 . ? B10 B11 1.768(9) . ? B10 B12 1.781(9) . ? B10 H10 1.1200 . ? B11 B12 1.776(9) . ? B11 H11 1.1200 . ? B12 H12 1.1200 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C21 B25 1.684(7) . ? C21 C22 1.702(7) . ? C21 B24 1.705(7) . ? C21 B26 1.709(8) . ? C21 B23 1.710(7) . ? C22 C33 1.516(7) . ? C22 B31 1.688(8) . ? C22 B27 1.689(8) . ? C22 B26 1.708(8) . ? C22 B23 1.715(8) . ? B23 B27 1.752(9) . ? B23 B28 1.768(8) . ? B23 B24 1.789(9) . ? B23 H23 1.1200 . ? B24 B28 1.762(9) . ? B24 B29 1.770(9) . ? B24 B25 1.789(8) . ? B24 H24 1.1200 . ? B25 B30 1.778(8) . ? B25 B26 1.779(8) . ? B25 B29 1.784(9) . ? B25 H25 1.1200 . ? B26 B31 1.777(9) . ? B26 B30 1.780(9) . ? B26 H26 1.1200 . ? B27 B31 1.768(9) . ? B27 B28 1.776(8) . ? B27 B32 1.784(9) . ? B27 H27 1.1200 . ? B28 B32 1.780(9) . ? B28 B29 1.781(9) . ? B28 H28 1.1200 . ? B29 B30 1.779(9) . ? B29 B32 1.780(9) . ? B29 H29 1.1200 . ? B30 B31 1.788(9) . ? B30 B32 1.795(9) . ? B30 H30 1.1200 . ? B31 B32 1.780(9) . ? B31 H31 1.1200 . ? B32 H32 1.1200 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Se1 Se2 102.23(15) . . ? C21 Se2 Se1 103.16(15) . . ? B5 C1 B6 63.1(3) . . ? B5 C1 C2 111.1(4) . . ? B6 C1 C2 60.9(3) . . ? B5 C1 B4 63.6(3) . . ? B6 C1 B4 115.2(4) . . ? C2 C1 B4 110.4(4) . . ? B5 C1 B3 115.1(4) . . ? B6 C1 B3 113.6(4) . . ? C2 C1 B3 60.4(3) . . ? B4 C1 B3 62.5(3) . . ? B5 C1 Se1 123.8(4) . . ? B6 C1 Se1 120.6(4) . . ? C2 C1 Se1 117.6(3) . . ? B4 C1 Se1 118.6(3) . . ? B3 C1 Se1 112.2(3) . . ? C13 C2 B7 121.8(5) . . ? C13 C2 B11 121.2(5) . . ? B7 C2 B11 63.4(4) . . ? C13 C2 C1 118.8(4) . . ? B7 C2 C1 109.9(4) . . ? B11 C2 C1 109.5(4) . . ? C13 C2 B3 117.6(4) . . ? B7 C2 B3 62.9(4) . . ? B11 C2 B3 114.5(4) . . ? C1 C2 B3 60.1(3) . . ? C13 C2 B6 116.6(5) . . ? B7 C2 B6 114.6(4) . . ? B11 C2 B6 62.8(3) . . ? C1 C2 B6 59.5(3) . . ? B3 C2 B6 112.0(4) . . ? C1 B3 C2 59.5(3) . . ? C1 B3 B8 105.0(4) . . ? C2 B3 B8 104.9(4) . . ? C1 B3 B7 105.3(4) . . ? C2 B3 B7 57.7(3) . . ? B8 B3 B7 59.9(3) . . ? C1 B3 B4 58.7(3) . . ? C2 B3 B4 106.6(4) . . ? B8 B3 B4 59.8(4) . . ? B7 B3 B4 107.8(4) . . ? C1 B3 H3 123.6 . . ? C2 B3 H3 123.5 . . ? B8 B3 H3 123.2 . . ? B7 B3 H3 122.7 . . ? B4 B3 H3 121.8 . . ? C1 B4 B9 104.6(4) . . ? C1 B4 B8 105.0(4) . . ? B9 B4 B8 61.3(4) . . ? C1 B4 B3 58.7(3) . . ? B9 B4 B3 108.6(4) . . ? B8 B4 B3 59.8(4) . . ? C1 B4 B5 57.5(3) . . ? B9 B4 B5 60.1(4) . . ? B8 B4 B5 108.7(4) . . ? B3 B4 B5 107.0(4) . . ? C1 B4 H4 125.2 . . ? B9 B4 H4 121.7 . . ? B8 B4 H4 121.6 . . ? B3 B4 H4 121.8 . . ? B5 B4 H4 122.0 . . ? C1 B5 B10 104.9(4) . . ? C1 B5 B6 58.7(3) . . ? B10 B5 B6 60.1(3) . . ? C1 B5 B9 104.7(4) . . ? B10 B5 B9 60.6(4) . . ? B6 B5 B9 108.5(4) . . ? C1 B5 B4 58.8(3) . . ? B10 B5 B4 107.4(5) . . ? B6 B5 B4 107.8(4) . . ? B9 B5 B4 59.0(4) . . ? C1 B5 H5 124.6 . . ? B10 B5 H5 122.2 . . ? B6 B5 H5 121.3 . . ? B9 B5 H5 122.3 . . ? B4 B5 H5 122.1 . . ? C1 B6 C2 59.6(3) . . ? C1 B6 B10 104.3(4) . . ? C2 B6 B10 104.3(5) . . ? C1 B6 B5 58.2(3) . . ? C2 B6 B5 106.3(4) . . ? B10 B6 B5 59.8(3) . . ? C1 B6 B11 105.6(4) . . ? C2 B6 B11 57.7(3) . . ? B10 B6 B11 59.7(4) . . ? B5 B6 B11 108.0(4) . . ? C1 B6 H6 123.8 . . ? C2 B6 H6 123.7 . . ? B10 B6 H6 123.7 . . ? B5 B6 H6 121.9 . . ? B11 B6 H6 122.4 . . ? C2 B7 B8 106.2(4) . . ? C2 B7 B12 105.4(5) . . ? B8 B7 B12 60.6(4) . . ? C2 B7 B11 58.5(3) . . ? B8 B7 B11 108.8(5) . . ? B12 B7 B11 60.1(4) . . ? C2 B7 B3 59.4(3) . . ? B8 B7 B3 59.8(3) . . ? B12 B7 B3 107.9(4) . . ? B11 B7 B3 107.8(4) . . ? C2 B7 H7 123.9 . . ? B8 B7 H7 121.5 . . ? B12 B7 H7 122.1 . . ? B11 B7 H7 121.6 . . ? B3 B7 H7 121.7 . . ? B3 B8 B4 60.4(3) . . ? B3 B8 B7 60.3(3) . . ? B4 B8 B7 108.5(4) . . ? B3 B8 B12 107.6(4) . . ? B4 B8 B12 107.3(5) . . ? B7 B8 B12 59.7(4) . . ? B3 B8 B9 107.3(5) . . ? B4 B8 B9 59.1(4) . . ? B7 B8 B9 107.7(5) . . ? B12 B8 B9 59.8(4) . . ? B3 B8 H8 121.7 . . ? B4 B8 H8 121.8 . . ? B7 B8 H8 121.4 . . ? B12 B8 H8 122.2 . . ? B9 B8 H8 122.4 . . ? B4 B9 B5 60.8(4) . . ? B4 B9 B12 107.6(4) . . ? B5 B9 B12 107.4(5) . . ? B4 B9 B10 107.8(4) . . ? B5 B9 B10 59.3(4) . . ? B12 B9 B10 59.7(4) . . ? B4 B9 B8 59.5(4) . . ? B5 B9 B8 107.8(4) . . ? B12 B9 B8 59.7(3) . . ? B10 B9 B8 107.2(4) . . ? B4 B9 H9 121.6 . . ? B5 B9 H9 121.8 . . ? B12 B9 H9 122.1 . . ? B10 B9 H9 122.3 . . ? B8 B9 H9 122.2 . . ? B5 B10 B11 108.8(4) . . ? B5 B10 B6 60.1(3) . . ? B11 B10 B6 60.4(4) . . ? B5 B10 B12 108.4(5) . . ? B11 B10 B12 60.0(4) . . ? B6 B10 B12 108.2(4) . . ? B5 B10 B9 60.1(4) . . ? B11 B10 B9 108.5(5) . . ? B6 B10 B9 108.2(4) . . ? B12 B10 B9 60.1(4) . . ? B5 B10 H10 121.3 . . ? B11 B10 H10 121.2 . . ? B6 B10 H10 121.6 . . ? B12 B10 H10 121.7 . . ? B9 B10 H10 121.6 . . ? C2 B11 B10 105.6(4) . . ? C2 B11 B12 104.9(4) . . ? B10 B11 B12 60.3(4) . . ? C2 B11 B7 58.1(3) . . ? B10 B11 B7 107.9(4) . . ? B12 B11 B7 59.8(4) . . ? C2 B11 B6 59.4(3) . . ? B10 B11 B6 59.8(3) . . ? B12 B11 B6 108.0(4) . . ? B7 B11 B6 107.5(4) . . ? C2 B11 H11 124.3 . . ? B10 B11 H11 122.0 . . ? B12 B11 H11 122.3 . . ? B7 B11 H11 122.0 . . ? B6 B11 H11 121.5 . . ? B7 B12 B11 60.1(4) . . ? B7 B12 B10 107.6(5) . . ? B11 B12 B10 59.6(4) . . ? B7 B12 B8 59.7(4) . . ? B11 B12 B8 108.0(4) . . ? B10 B12 B8 108.1(5) . . ? B7 B12 B9 108.1(5) . . ? B11 B12 B9 108.2(5) . . ? B10 B12 B9 60.2(4) . . ? B8 B12 B9 60.5(4) . . ? B7 B12 H12 121.9 . . ? B11 B12 H12 121.8 . . ? B10 B12 H12 121.9 . . ? B8 B12 H12 121.6 . . ? B9 B12 H12 121.3 . . ? C2 C13 H13A 109.5 . . ? C2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? B25 C21 C22 111.1(4) . . ? B25 C21 B24 63.7(3) . . ? C22 C21 B24 111.1(4) . . ? B25 C21 B26 63.2(3) . . ? C22 C21 B26 60.1(3) . . ? B24 C21 B26 115.2(4) . . ? B25 C21 B23 115.4(4) . . ? C22 C21 B23 60.4(3) . . ? B24 C21 B23 63.2(3) . . ? B26 C21 B23 112.6(4) . . ? B25 C21 Se2 125.2(4) . . ? C22 C21 Se2 115.9(3) . . ? B24 C21 Se2 119.2(3) . . ? B26 C21 Se2 120.6(3) . . ? B23 C21 Se2 111.5(3) . . ? C33 C22 B31 122.0(4) . . ? C33 C22 B27 120.7(5) . . ? B31 C22 B27 63.1(3) . . ? C33 C22 C21 119.2(4) . . ? B31 C22 C21 109.9(4) . . ? B27 C22 C21 109.3(4) . . ? C33 C22 B26 118.1(5) . . ? B31 C22 B26 63.1(4) . . ? B27 C22 B26 114.5(4) . . ? C21 C22 B26 60.1(3) . . ? C33 C22 B23 116.5(4) . . ? B31 C22 B23 113.7(4) . . ? B27 C22 B23 62.0(3) . . ? C21 C22 B23 60.0(3) . . ? B26 C22 B23 112.4(4) . . ? C21 B23 C22 59.6(3) . . ? C21 B23 B27 106.0(4) . . ? C22 B23 B27 58.3(3) . . ? C21 B23 B28 104.4(4) . . ? C22 B23 B28 105.4(4) . . ? B27 B23 B28 60.6(3) . . ? C21 B23 B24 58.3(3) . . ? C22 B23 B24 106.5(4) . . ? B27 B23 B24 108.4(4) . . ? B28 B23 B24 59.4(3) . . ? C21 B23 H23 123.8 . . ? C22 B23 H23 123.2 . . ? B27 B23 H23 121.8 . . ? B28 B23 H23 123.3 . . ? B24 B23 H23 122.0 . . ? C21 B24 B28 104.8(4) . . ? C21 B24 B29 104.2(4) . . ? B28 B24 B29 60.6(4) . . ? C21 B24 B23 58.5(3) . . ? B28 B24 B23 59.7(3) . . ? B29 B24 B23 107.5(4) . . ? C21 B24 B25 57.6(3) . . ? B28 B24 B25 108.3(4) . . ? B29 B24 B25 60.2(3) . . ? B23 B24 B25 106.6(4) . . ? C21 B24 H24 125.2 . . ? B28 B24 H24 121.9 . . ? B29 B24 H24 122.3 . . ? B23 B24 H24 122.2 . . ? B25 B24 H24 122.1 . . ? C21 B25 B30 105.4(4) . . ? C21 B25 B26 59.1(3) . . ? B30 B25 B26 60.1(4) . . ? C21 B25 B29 104.5(4) . . ? B30 B25 B29 59.9(4) . . ? B26 B25 B29 107.5(4) . . ? C21 B25 B24 58.7(3) . . ? B30 B25 B24 107.7(4) . . ? B26 B25 B24 107.8(4) . . ? B29 B25 B24 59.4(3) . . ? C21 B25 H25 124.4 . . ? B30 B25 H25 122.1 . . ? B26 B25 H25 121.5 . . ? B29 B25 H25 122.9 . . ? B24 B25 H25 121.8 . . ? C22 B26 C21 59.8(3) . . ? C22 B26 B31 57.9(3) . . ? C21 B26 B31 105.5(4) . . ? C22 B26 B25 106.4(4) . . ? C21 B26 B25 57.7(3) . . ? B31 B26 B25 108.3(4) . . ? C22 B26 B30 105.3(4) . . ? C21 B26 B30 104.3(4) . . ? B31 B26 B30 60.3(3) . . ? B25 B26 B30 60.0(3) . . ? C22 B26 H26 123.2 . . ? C21 B26 H26 124.1 . . ? B31 B26 H26 122.1 . . ? B25 B26 H26 122.0 . . ? B30 B26 H26 123.1 . . ? C22 B27 B23 59.8(3) . . ? C22 B27 B31 58.4(3) . . ? B23 B27 B31 108.1(5) . . ? C22 B27 B28 106.2(4) . . ? B23 B27 B28 60.1(3) . . ? B31 B27 B28 108.1(4) . . ? C22 B27 B32 105.5(4) . . ? B23 B27 B32 108.2(5) . . ? B31 B27 B32 60.1(3) . . ? B28 B27 B32 60.0(4) . . ? C22 B27 H27 123.8 . . ? B23 B27 H27 121.2 . . ? B31 B27 H27 121.7 . . ? B28 B27 H27 121.9 . . ? B32 B27 H27 122.2 . . ? B24 B28 B23 60.9(3) . . ? B24 B28 B27 108.6(4) . . ? B23 B28 B27 59.3(3) . . ? B24 B28 B32 108.5(5) . . ? B23 B28 B32 107.7(4) . . ? B27 B28 B32 60.2(3) . . ? B24 B28 B29 59.9(4) . . ? B23 B28 B29 108.0(5) . . ? B27 B28 B29 107.9(4) . . ? B32 B28 B29 60.0(4) . . ? B24 B28 H28 121.0 . . ? B23 B28 H28 121.9 . . ? B27 B28 H28 121.8 . . ? B32 B28 H28 121.6 . . ? B29 B28 H28 121.9 . . ? B24 B29 B30 108.6(4) . . ? B24 B29 B32 108.2(4) . . ? B30 B29 B32 60.6(4) . . ? B24 B29 B28 59.5(4) . . ? B30 B29 B28 108.2(5) . . ? B32 B29 B28 60.0(4) . . ? B24 B29 B25 60.5(3) . . ? B30 B29 B25 59.9(3) . . ? B32 B29 B25 108.4(5) . . ? B28 B29 B25 107.7(4) . . ? B24 B29 H29 121.5 . . ? B30 B29 H29 121.3 . . ? B32 B29 H29 121.4 . . ? B28 B29 H29 122.1 . . ? B25 B29 H29 121.7 . . ? B25 B30 B29 60.2(4) . . ? B25 B30 B26 60.0(3) . . ? B29 B30 B26 107.7(4) . . ? B25 B30 B31 107.8(4) . . ? B29 B30 B31 107.3(5) . . ? B26 B30 B31 59.7(4) . . ? B25 B30 B32 107.9(4) . . ? B29 B30 B32 59.7(4) . . ? B26 B30 B32 107.3(4) . . ? B31 B30 B32 59.6(4) . . ? B25 B30 H30 121.5 . . ? B29 B30 H30 121.9 . . ? B26 B30 H30 122.0 . . ? B31 B30 H30 122.1 . . ? B32 B30 H30 122.1 . . ? C22 B31 B27 58.5(3) . . ? C22 B31 B26 59.0(3) . . ? B27 B31 B26 107.4(4) . . ? C22 B31 B32 105.8(4) . . ? B27 B31 B32 60.4(4) . . ? B26 B31 B32 108.2(4) . . ? C22 B31 B30 105.8(4) . . ? B27 B31 B30 108.4(4) . . ? B26 B31 B30 59.9(3) . . ? B32 B31 B30 60.4(4) . . ? C22 B31 H31 124.1 . . ? B27 B31 H31 121.7 . . ? B26 B31 H31 121.8 . . ? B32 B31 H31 121.8 . . ? B30 B31 H31 121.8 . . ? B29 B32 B28 60.0(4) . . ? B29 B32 B31 107.6(5) . . ? B28 B32 B31 107.4(4) . . ? B29 B32 B27 107.6(5) . . ? B28 B32 B27 59.8(4) . . ? B31 B32 B27 59.5(3) . . ? B29 B32 B30 59.7(4) . . ? B28 B32 B30 107.5(5) . . ? B31 B32 B30 60.0(4) . . ? B27 B32 B30 107.3(4) . . ? B29 B32 H32 121.9 . . ? B28 B32 H32 122.0 . . ? B31 B32 H32 122.0 . . ? B27 B32 H32 122.2 . . ? B30 B32 H32 122.0 . . ? C22 C33 H33A 109.5 . . ? C22 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C22 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 C1 Se1 Se2 111.2(3) . . . . ? C1 Se1 Se2 C21 99.1(2) . . . . ? C22 C21 Se2 Se1 109.8(3) . . . . ? Se1 C1 C2 C13 -5.8(6) . . . . ? Se2 C21 C22 C33 -4.4(6) . . . . ? C22 C21 Se2 Se1 109.8(3) . . . . ? C33 C22 C2 C13 3.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 0.840 _refine_diff_density_min -0.832 _refine_diff_density_rms 0.114 data_compound_2.toluene _database_code_depnum_ccdc_archive 'CCDC 616223' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C6 H26 B20 Se2, C7 H8' _chemical_formula_sum 'C13 H34 B20 Se2' _chemical_formula_weight 564.52 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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.4834(11) _cell_length_b 9.5944(2) _cell_length_c 13.8538(6) _cell_angle_alpha 90.00 _cell_angle_beta 119.4851(14) _cell_angle_gamma 90.00 _cell_volume 2717.12(18) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2527 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 25.682 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.380 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 2.727 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 4917 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 25.67 _reflns_number_total 2581 _reflns_number_gt 2082 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _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. ; _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^)+(0.0282P)^2^+6.2826P] 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 0.00094(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2581 _refine_ls_number_parameters 158 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0492 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0789 _refine_ls_wR_factor_gt 0.0739 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Se1 Se 0.016122(6) 0.780423(14) 0.183826(10) 0.02398(4) Uani 1 d . . . C1 C 0.09134(5) 0.90581(13) 0.24931(9) 0.0190(3) Uani 1 d . . . C2 C 0.16474(5) 0.83028(13) 0.29032(10) 0.0208(4) Uani 1 d . . . B3 B 0.12685(6) 0.92316(16) 0.16745(11) 0.0226(4) Uani 1 d . . . H3 H 0.1073 0.8746 0.0835 0.027 Uiso 1 calc R . . B4 B 0.08692(7) 1.06556(15) 0.19220(12) 0.0243(5) Uani 1 d . . . H4 H 0.0412 1.1127 0.1237 0.029 Uiso 1 calc R . . B5 B 0.09839(7) 1.04716(15) 0.32810(12) 0.0226(4) Uani 1 d . . . H5 H 0.0602 1.0821 0.3489 0.027 Uiso 1 calc R . . B6 B 0.14633(6) 0.89382(15) 0.38845(11) 0.0205(4) Uani 1 d . . . H6 H 0.1396 0.8263 0.4480 0.025 Uiso 1 calc R . . B7 B 0.21240(7) 0.93843(16) 0.26248(12) 0.0242(4) Uani 1 d . . . H7 H 0.2499 0.9018 0.2406 0.029 Uiso 1 calc R . . B8 B 0.16428(7) 1.09069(17) 0.20166(12) 0.0258(4) Uani 1 d . . . H8 H 0.1701 1.1550 0.1396 0.031 Uiso 1 calc R . . B9 B 0.14719(7) 1.16736(16) 0.30242(12) 0.0256(4) Uani 1 d . . . H9 H 0.1421 1.2828 0.3072 0.031 Uiso 1 calc R . . B10 B 0.18341(7) 1.06045(16) 0.42422(12) 0.0244(4) Uani 1 d . . . H10 H 0.2018 1.1048 0.5092 0.029 Uiso 1 calc R . . B11 B 0.22397(7) 0.92058(15) 0.39881(12) 0.0228(4) Uani 1 d . . . H11 H 0.2693 0.8720 0.4670 0.027 Uiso 1 calc R . . B12 B 0.22434(7) 1.08900(16) 0.34592(12) 0.0244(4) Uani 1 d . . . H12 H 0.2700 1.1531 0.3794 0.029 Uiso 1 calc R . . C13 C 0.16813(6) 0.67325(14) 0.28230(11) 0.0275(4) Uani 1 d . . . H13A H 0.1471 0.6457 0.2041 0.041 Uiso 1 calc R . . H13B H 0.1455 0.6289 0.3177 0.041 Uiso 1 calc R . . H13C H 0.2140 0.6436 0.3199 0.041 Uiso 1 calc R . . C14 C -0.02468(8) 0.4841(2) 0.01481(16) 0.0326(7) Uiso 0.50 d PD A -1 C15 C -0.03810(9) 0.5741(2) -0.07181(15) 0.0397(8) Uiso 0.50 d PD A -1 H15 H -0.0793 0.6195 -0.1097 0.048 Uiso 0.50 calc PR A -1 C16 C 0.00898(8) 0.5983(3) -0.10337(19) 0.0460(8) Uiso 0.50 d PD A -1 H16 H -0.0011 0.6582 -0.1643 0.055 Uiso 0.50 calc PR A -1 C17 C 0.07067(11) 0.5363(3) -0.04729(18) 0.0526(9) Uiso 0.50 d PD A -1 H17 H 0.1029 0.5548 -0.0681 0.063 Uiso 0.50 calc PR A -1 C18 C 0.08354(9) 0.4467(3) 0.04009(16) 0.0509(9) Uiso 0.50 d PD A -1 H18 H 0.1249 0.4018 0.0788 0.061 Uiso 0.50 calc PR A -1 C19 C 0.03631(8) 0.4223(3) 0.07118(19) 0.0367(8) Uiso 0.50 d PD A -1 H19 H 0.0462 0.3624 0.1320 0.044 Uiso 0.50 calc PR A -1 C20 C -0.07407(13) 0.4597(4) 0.0506(3) 0.0573(11) Uiso 0.50 d PD A -1 H20A H -0.0896 0.3632 0.0343 0.086 Uiso 0.50 calc PR A -1 H20B H -0.1111 0.5234 0.0107 0.086 Uiso 0.50 calc PR A -1 H20C H -0.0541 0.4766 0.1305 0.086 Uiso 0.50 calc PR A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Se1 0.01772(5) 0.02809(6) 0.02799(5) -0.00799(5) 0.01268(4) -0.00363(5) C1 0.0151(5) 0.0232(6) 0.0206(5) 0.0005(5) 0.0102(4) 0.0014(5) C2 0.0161(5) 0.0240(6) 0.0252(5) 0.0014(5) 0.0124(4) 0.0023(5) B3 0.0191(6) 0.0338(8) 0.0180(6) 0.0025(6) 0.0116(4) -0.0001(6) B4 0.0231(6) 0.0243(7) 0.0235(7) 0.0045(6) 0.0099(5) 0.0014(6) B5 0.0202(6) 0.0224(7) 0.0258(7) -0.0023(5) 0.0118(5) 0.0012(5) B6 0.0198(6) 0.0277(7) 0.0153(6) 0.0001(5) 0.0098(4) 0.0019(5) B7 0.0199(6) 0.0326(8) 0.0257(6) 0.0005(6) 0.0156(4) -0.0005(6) B8 0.0250(6) 0.0313(8) 0.0248(6) 0.0049(6) 0.0151(5) -0.0026(6) B9 0.0245(6) 0.0220(7) 0.0313(7) 0.0012(6) 0.0146(5) -0.0017(6) B10 0.0209(6) 0.0294(8) 0.0220(6) -0.0054(6) 0.0097(5) -0.0046(6) B11 0.0178(6) 0.0271(8) 0.0220(6) 0.0008(6) 0.0086(5) -0.0013(6) B12 0.0192(6) 0.0278(8) 0.0251(7) 0.0031(6) 0.0100(5) -0.0012(6) C13 0.0242(5) 0.0269(7) 0.0362(6) -0.0013(5) 0.0185(4) 0.0044(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Se1 C1 1.9526(11) . ? Se1 Se1 2.3026(3) 2 ? C1 C2 1.6897(17) . ? C1 B5 1.697(2) . ? C1 B4 1.704(2) . ? C1 B3 1.715(2) . ? C1 B6 1.7165(16) . ? C2 C13 1.5157(18) . ? C2 B11 1.6989(17) . ? C2 B7 1.704(2) . ? C2 B6 1.728(2) . ? C2 B3 1.7299(18) . ? B3 B8 1.781(2) . ? B3 B4 1.783(2) . ? B3 B7 1.7851(18) . ? B3 H3 1.1200 . ? B4 B8 1.772(2) . ? B4 B5 1.775(2) . ? B4 B9 1.7780(19) . ? B4 H4 1.1200 . ? B5 B10 1.7773(18) . ? B5 B9 1.781(2) . ? B5 B6 1.7901(19) . ? B5 H5 1.1200 . ? B6 B10 1.771(2) . ? B6 B11 1.776(2) . ? B6 H6 1.1200 . ? B7 B11 1.779(2) . ? B7 B12 1.784(2) . ? B7 B8 1.784(2) . ? B7 H7 1.1200 . ? B8 B9 1.789(3) . ? B8 B12 1.7914(18) . ? B8 H8 1.1200 . ? B9 B12 1.771(2) . ? B9 B10 1.792(2) . ? B9 H9 1.1200 . ? B10 B11 1.778(2) . ? B10 B12 1.789(3) . ? B10 H10 1.1200 . ? B11 B12 1.776(2) . ? B11 H11 1.1200 . ? B12 H12 1.1200 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C19 1.382(2) . ? C14 C15 1.383(3) . ? C14 C20 1.487(4) . ? C15 C16 1.394(3) . ? C15 H15 0.9500 . ? C16 C17 1.396(3) . ? C16 H16 0.9500 . ? C17 C18 1.391(3) . ? C17 H17 0.9500 . ? C18 C19 1.393(3) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Se1 Se1 101.94(4) . 2 ? C2 C1 B5 111.47(8) . . ? C2 C1 B4 111.14(10) . . ? B5 C1 B4 62.90(9) . . ? C2 C1 B3 61.07(8) . . ? B5 C1 B3 115.00(11) . . ? B4 C1 B3 62.87(9) . . ? C2 C1 B6 60.95(8) . . ? B5 C1 B6 63.26(8) . . ? B4 C1 B6 114.95(9) . . ? B3 C1 B6 114.03(9) . . ? C2 C1 Se1 115.58(8) . . ? B5 C1 Se1 124.80(10) . . ? B4 C1 Se1 120.26(7) . . ? B3 C1 Se1 112.07(8) . . ? B6 C1 Se1 119.28(9) . . ? C13 C2 C1 118.91(10) . . ? C13 C2 B11 121.47(9) . . ? C1 C2 B11 109.53(10) . . ? C13 C2 B7 121.64(12) . . ? C1 C2 B7 109.74(10) . . ? B11 C2 B7 63.04(9) . . ? C13 C2 B6 116.81(12) . . ? C1 C2 B6 60.29(8) . . ? B11 C2 B6 62.41(9) . . ? B7 C2 B6 114.19(10) . . ? C13 C2 B3 117.39(10) . . ? C1 C2 B3 60.18(8) . . ? B11 C2 B3 114.10(10) . . ? B7 C2 B3 62.64(8) . . ? B6 C2 B3 112.70(10) . . ? C1 B3 C2 58.74(8) . . ? C1 B3 B8 104.39(11) . . ? C2 B3 B8 104.81(9) . . ? C1 B3 B4 58.28(9) . . ? C2 B3 B4 105.65(11) . . ? B8 B3 B4 59.64(9) . . ? C1 B3 B7 104.91(10) . . ? C2 B3 B7 57.96(8) . . ? B8 B3 B7 60.05(8) . . ? B4 B3 B7 107.62(10) . . ? C1 B3 H3 124.2 . . ? C2 B3 H3 123.8 . . ? B8 B3 H3 123.2 . . ? B4 B3 H3 122.2 . . ? B7 B3 H3 122.5 . . ? C1 B4 B8 105.19(10) . . ? C1 B4 B5 58.35(8) . . ? B8 B4 B5 108.68(9) . . ? C1 B4 B9 104.74(9) . . ? B8 B4 B9 60.53(9) . . ? B5 B4 B9 60.17(9) . . ? C1 B4 B3 58.85(9) . . ? B8 B4 B3 60.11(9) . . ? B5 B4 B3 107.95(10) . . ? B9 B4 B3 108.32(10) . . ? C1 B4 H4 124.8 . . ? B8 B4 H4 121.8 . . ? B5 B4 H4 121.4 . . ? B9 B4 H4 122.1 . . ? B3 B4 H4 121.4 . . ? C1 B5 B4 58.76(8) . . ? C1 B5 B10 104.90(10) . . ? B4 B5 B10 108.40(12) . . ? C1 B5 B9 104.93(12) . . ? B4 B5 B9 60.01(9) . . ? B10 B5 B9 60.47(8) . . ? C1 B5 B6 58.90(7) . . ? B4 B5 B6 108.02(12) . . ? B10 B5 B6 59.51(8) . . ? B9 B5 B6 107.87(11) . . ? C1 B5 H5 124.6 . . ? B4 B5 H5 121.3 . . ? B10 B5 H5 122.2 . . ? B9 B5 H5 122.2 . . ? B6 B5 H5 121.7 . . ? C1 B6 C2 58.76(8) . . ? C1 B6 B10 104.38(10) . . ? C2 B6 B10 105.06(12) . . ? C1 B6 B11 104.84(11) . . ? C2 B6 B11 58.00(8) . . ? B10 B6 B11 60.19(9) . . ? C1 B6 B5 57.84(7) . . ? C2 B6 B5 105.42(10) . . ? B10 B6 B5 59.88(8) . . ? B11 B6 B5 107.68(11) . . ? C1 B6 H6 124.4 . . ? C2 B6 H6 123.8 . . ? B10 B6 H6 123.0 . . ? B11 B6 H6 122.4 . . ? B5 B6 H6 122.3 . . ? C2 B7 B11 58.34(8) . . ? C2 B7 B12 104.94(12) . . ? B11 B7 B12 59.80(9) . . ? C2 B7 B8 105.76(11) . . ? B11 B7 B8 108.08(12) . . ? B12 B7 B8 60.27(8) . . ? C2 B7 B3 59.39(8) . . ? B11 B7 B3 107.67(12) . . ? B12 B7 B3 107.78(11) . . ? B8 B7 B3 59.85(8) . . ? C2 B7 H7 124.2 . . ? B11 B7 H7 121.9 . . ? B12 B7 H7 122.4 . . ? B8 B7 H7 121.9 . . ? B3 B7 H7 121.6 . . ? B4 B8 B3 60.26(9) . . ? B4 B8 B7 108.14(11) . . ? B3 B8 B7 60.10(8) . . ? B4 B8 B9 59.90(9) . . ? B3 B8 B9 107.94(12) . . ? B7 B8 B9 107.53(11) . . ? B4 B8 B12 107.27(12) . . ? B3 B8 B12 107.65(10) . . ? B7 B8 B12 59.86(8) . . ? B9 B8 B12 59.28(9) . . ? B4 B8 H8 121.7 . . ? B3 B8 H8 121.6 . . ? B7 B8 H8 121.7 . . ? B9 B8 H8 122.1 . . ? B12 B8 H8 122.3 . . ? B12 B9 B4 107.92(11) . . ? B12 B9 B5 107.96(11) . . ? B4 B9 B5 59.82(9) . . ? B12 B9 B8 60.42(9) . . ? B4 B9 B8 59.58(9) . . ? B5 B9 B8 107.64(11) . . ? B12 B9 B10 60.30(9) . . ? B4 B9 B10 107.61(11) . . ? B5 B9 B10 59.66(8) . . ? B8 B9 B10 108.34(11) . . ? B12 B9 H9 121.4 . . ? B4 B9 H9 122.1 . . ? B5 B9 H9 122.0 . . ? B8 B9 H9 121.7 . . ? B10 B9 H9 121.7 . . ? B6 B10 B5 60.61(8) . . ? B6 B10 B11 60.05(9) . . ? B5 B10 B11 108.13(10) . . ? B6 B10 B12 107.79(12) . . ? B5 B10 B12 107.30(11) . . ? B11 B10 B12 59.71(9) . . ? B6 B10 B9 108.26(9) . . ? B5 B10 B9 59.87(8) . . ? B11 B10 B9 107.33(12) . . ? B12 B10 B9 59.27(9) . . ? B6 B10 H10 121.3 . . ? B5 B10 H10 121.6 . . ? B11 B10 H10 121.9 . . ? B12 B10 H10 122.4 . . ? B9 B10 H10 122.1 . . ? C2 B11 B6 59.59(8) . . ? C2 B11 B12 105.50(9) . . ? B6 B11 B12 108.16(10) . . ? C2 B11 B10 105.96(9) . . ? B6 B11 B10 59.77(9) . . ? B12 B11 B10 60.46(10) . . ? C2 B11 B7 58.61(8) . . ? B6 B11 B7 108.29(9) . . ? B12 B11 B7 60.24(9) . . ? B10 B11 B7 108.71(10) . . ? C2 B11 H11 124.0 . . ? B6 B11 H11 121.4 . . ? B12 B11 H11 122.1 . . ? B10 B11 H11 121.8 . . ? B7 B11 H11 121.3 . . ? B9 B12 B11 108.34(12) . . ? B9 B12 B7 108.36(9) . . ? B11 B12 B7 59.96(9) . . ? B9 B12 B10 60.43(9) . . ? B11 B12 B10 59.83(9) . . ? B7 B12 B10 107.98(11) . . ? B9 B12 B8 60.30(9) . . ? B11 B12 B8 107.90(10) . . ? B7 B12 B8 59.87(8) . . ? B10 B12 B8 108.34(10) . . ? B9 B12 H12 121.2 . . ? B11 B12 H12 121.8 . . ? B7 B12 H12 121.7 . . ? B10 B12 H12 121.6 . . ? B8 B12 H12 121.7 . . ? C2 C13 H13A 109.5 . . ? C2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C19 C14 C15 119.2(2) . . ? C19 C14 C20 120.4(2) . . ? C15 C14 C20 120.4(2) . . ? C14 C15 C16 119.93(19) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C17 121.4(2) . . ? C15 C16 H16 119.3 . . ? C17 C16 H16 119.3 . . ? C18 C17 C16 118.0(2) . . ? C18 C17 H17 121.0 . . ? C16 C17 H17 121.0 . . ? C17 C18 C19 120.5(2) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C14 C19 C18 121.0(2) . . ? C14 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 C1 Se1 Se1 111.53(9) . . . 2 ? C1 Se1 Se1 C1 101.94(7) . . 2 2 ? Se1 C1 C2 C13 -4.61(16) . . . . ? C13 C2 C2 C13 8.65(15) 2 2 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.67 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.771 _refine_diff_density_min -0.431 _refine_diff_density_rms 0.078 data_compound_3 _database_code_depnum_ccdc_archive 'CCDC 616224' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C16 H30 B20 Se2' _chemical_formula_sum 'C16 H30 B20 Se2' _chemical_formula_weight 596.52 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' Se Se -0.0929 2.2259 '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 c' _symmetry_space_group_name_Hall 'P -2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 8.0368(4) _cell_length_b 12.3095(5) _cell_length_c 14.0307(7) _cell_angle_alpha 90.00 _cell_angle_beta 91.717(5) _cell_angle_gamma 90.00 _cell_volume 1387.42(11) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3905 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 25.682 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.428 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 588 _exptl_absorpt_coefficient_mu 2.675 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 7433 _diffrn_reflns_av_R_equivalents 0.0509 _diffrn_reflns_av_sigmaI/netI 0.0770 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 25.64 _reflns_number_total 4390 _reflns_number_gt 3840 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _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. ; _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^)+(0.0227P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.001(12) _refine_ls_number_reflns 4390 _refine_ls_number_parameters 341 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0505 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.0730 _refine_ls_wR_factor_gt 0.0690 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.027 _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 Se1 Se 0.3300 0.81725(4) 1.0000 0.01301(13) Uani 1 d . . . Se2 Se 0.36657(9) 0.63873(4) 0.95599(5) 0.01301(13) Uani 1 d . . . C1 C 0.5575(6) 0.8678(4) 1.0206(3) 0.0087(10) Uani 1 d . . . C2 C 0.6122(6) 0.9009(4) 1.1369(3) 0.0099(11) Uani 1 d . . . B3 B 0.6950(7) 0.7860(5) 1.0842(4) 0.0145(14) Uani 1 d . . . H3 H 0.6662 0.7012 1.1074 0.017 Uiso 1 calc R . . B4 B 0.7234(7) 0.8194(5) 0.9622(4) 0.0137(13) Uani 1 d . . . H4 H 0.7159 0.7559 0.9051 0.016 Uiso 1 calc R . . B5 B 0.6479(8) 0.9540(5) 0.9428(4) 0.0174(14) Uani 1 d . . . H5 H 0.5903 0.9795 0.8727 0.021 Uiso 1 calc R . . B6 B 0.5719(7) 1.0012(4) 1.0523(4) 0.0131(13) Uani 1 d . . . H6 H 0.4614 1.0565 1.0544 0.016 Uiso 1 calc R . . B7 B 0.8194(7) 0.8775(5) 1.1552(4) 0.0181(14) Uani 1 d . . . H7 H 0.8767 0.8522 1.2255 0.022 Uiso 1 calc R . . B8 B 0.8935(8) 0.8272(5) 1.0466(5) 0.0200(15) Uani 1 d U . . H8 H 1.0000 0.7686 1.0451 0.024 Uiso 1 calc R . . B9 B 0.8646(10) 0.9315(4) 0.9579(6) 0.0250(14) Uani 1 d . . . H9 H 0.9517 0.9421 0.8978 0.030 Uiso 1 calc R . . B10 B 0.7701(8) 1.0451(5) 1.0146(4) 0.0181(14) Uani 1 d . . . H10 H 0.7946 1.1308 0.9921 0.022 Uiso 1 calc R . . B11 B 0.7407(8) 1.0117(5) 1.1376(4) 0.0174(14) Uani 1 d . . . H11 H 0.7440 1.0745 1.1953 0.021 Uiso 1 calc R . . B12 B 0.9225(8) 0.9660(5) 1.0775(5) 0.0223(15) Uani 1 d . . . H12 H 1.0490 0.9995 1.0959 0.027 Uiso 1 calc R . . C13 C 0.4924(6) 0.8819(4) 1.2150(4) 0.0104(12) Uani 1 d U . . C14 C 0.3533(7) 0.9472(4) 1.2250(4) 0.0174(13) Uani 1 d . . . H14 H 0.3292 1.0023 1.1792 0.021 Uiso 1 calc R . . C15 C 0.2496(7) 0.9332(5) 1.3006(4) 0.0274(15) Uani 1 d . . . H15 H 0.1541 0.9781 1.3062 0.033 Uiso 1 calc R . . C16 C 0.2843(8) 0.8540(5) 1.3685(4) 0.0331(16) Uani 1 d . . . H16 H 0.2138 0.8455 1.4211 0.040 Uiso 1 calc R . . C17 C 0.4198(9) 0.7880(5) 1.3598(4) 0.0251(16) Uani 1 d . . . H17 H 0.4428 0.7333 1.4062 0.030 Uiso 1 calc R . . C18 C 0.5252(7) 0.8008(5) 1.2826(4) 0.0213(14) Uani 1 d . . . H18 H 0.6187 0.7543 1.2763 0.026 Uiso 1 calc R . . C21 C 0.3443(6) 0.6428(4) 0.8173(3) 0.0117(11) Uani 1 d . . . C22 C 0.1765(6) 0.5706(4) 0.7682(3) 0.0101(11) Uani 1 d . . . B23 B 0.1795(8) 0.7115(5) 0.7648(4) 0.0132(14) Uani 1 d U . . H23 H 0.0912 0.7630 0.8053 0.016 Uiso 1 calc R . . B24 B 0.3901(8) 0.7508(5) 0.7476(4) 0.0180(15) Uani 1 d . . . H24 H 0.4400 0.8301 0.7752 0.022 Uiso 1 calc R . . B25 B 0.5154(8) 0.6298(5) 0.7488(4) 0.0183(14) Uani 1 d . . . H25 H 0.6473 0.6287 0.7769 0.022 Uiso 1 calc R . . B26 B 0.3781(7) 0.5182(5) 0.7669(4) 0.0143(13) Uani 1 d . . . H26 H 0.4184 0.4448 0.8088 0.017 Uiso 1 calc R . . B27 B 0.1125(9) 0.6321(5) 0.6638(4) 0.0183(15) Uani 1 d U . . H27 H -0.0195 0.6332 0.6358 0.022 Uiso 1 calc R . . B28 B 0.2493(9) 0.7440(5) 0.6499(4) 0.0207(15) Uani 1 d . . . H28 H 0.2060 0.8195 0.6122 0.025 Uiso 1 calc R . . B29 B 0.4559(9) 0.6934(5) 0.6385(5) 0.0211(15) Uani 1 d . . . H29 H 0.5492 0.7349 0.5933 0.025 Uiso 1 calc R . . B30 B 0.4475(9) 0.5489(5) 0.6491(4) 0.0220(16) Uani 1 d . . . H30 H 0.5351 0.4943 0.6111 0.026 Uiso 1 calc R . . B31 B 0.2372(8) 0.5117(5) 0.6649(4) 0.0163(14) Uani 1 d . . . H31 H 0.1866 0.4324 0.6378 0.020 Uiso 1 calc R . . B32 B 0.2867(10) 0.6199(5) 0.5877(5) 0.0237(17) Uani 1 d . . . H32 H 0.2691 0.6129 0.5084 0.028 Uiso 1 calc R . . C33 C 0.0579(6) 0.5130(4) 0.8319(3) 0.0131(12) Uani 1 d . . . C34 C 0.0467(7) 0.4007(4) 0.8287(4) 0.0194(12) Uani 1 d . . . H34 H 0.1162 0.3610 0.7875 0.023 Uiso 1 calc R . . C35 C -0.0645(7) 0.3459(4) 0.8846(4) 0.0255(14) Uani 1 d . . . H35 H -0.0699 0.2688 0.8818 0.031 Uiso 1 calc R . . C36 C -0.1667(7) 0.4010(5) 0.9439(5) 0.0275(15) Uani 1 d . . . H36 H -0.2428 0.3627 0.9822 0.033 Uiso 1 calc R . . C37 C -0.1580(7) 0.5135(4) 0.9476(4) 0.0271(14) Uani 1 d . . . H37 H -0.2284 0.5528 0.9885 0.032 Uiso 1 calc R . . C38 C -0.0462(7) 0.5686(5) 0.8915(4) 0.0234(14) Uani 1 d . . . H38 H -0.0413 0.6457 0.8941 0.028 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Se1 0.0077(3) 0.0177(3) 0.0137(3) -0.0069(2) 0.00056(19) 0.0000(2) Se2 0.0196(3) 0.0121(3) 0.0073(2) 0.0013(2) -0.0010(2) -0.0037(2) C1 0.007(3) 0.013(2) 0.007(2) -0.002(2) 0.0026(19) 0.002(2) C2 0.013(3) 0.010(3) 0.007(3) 0.002(2) -0.003(2) -0.001(2) B3 0.009(3) 0.014(3) 0.021(3) 0.006(3) -0.002(3) -0.001(2) B4 0.005(3) 0.019(3) 0.017(3) -0.003(3) 0.002(2) 0.001(2) B5 0.022(4) 0.017(3) 0.013(3) 0.007(3) 0.005(3) -0.004(3) B6 0.015(3) 0.010(3) 0.014(3) -0.002(3) 0.000(2) -0.004(2) B7 0.009(3) 0.022(3) 0.024(3) 0.001(3) -0.004(3) -0.003(3) B8 0.007(3) 0.025(3) 0.029(3) 0.003(3) 0.005(2) 0.000(2) B9 0.022(4) 0.025(3) 0.028(3) -0.001(4) 0.011(3) -0.001(4) B10 0.018(4) 0.017(3) 0.020(3) 0.005(3) 0.002(3) -0.007(3) B11 0.018(4) 0.018(3) 0.016(3) 0.000(3) -0.001(3) -0.008(3) B12 0.017(4) 0.020(3) 0.029(4) -0.001(3) 0.004(3) -0.012(3) C13 0.009(2) 0.014(2) 0.008(2) -0.0050(18) -0.0011(18) -0.0047(18) C14 0.018(3) 0.022(3) 0.013(3) -0.004(3) 0.000(2) -0.003(3) C15 0.017(4) 0.042(4) 0.023(3) -0.011(3) 0.000(3) -0.003(3) C16 0.037(4) 0.042(4) 0.021(3) -0.009(3) 0.013(3) -0.025(3) C17 0.040(4) 0.023(3) 0.012(3) 0.004(3) 0.004(3) -0.012(3) C18 0.026(4) 0.019(3) 0.019(3) -0.008(3) -0.002(3) -0.002(3) C21 0.020(3) 0.007(2) 0.009(3) -0.001(2) 0.005(2) -0.001(2) C22 0.011(3) 0.013(3) 0.007(2) -0.004(2) -0.003(2) 0.000(2) B23 0.017(3) 0.006(3) 0.017(3) 0.000(2) -0.001(2) -0.001(2) B24 0.026(4) 0.015(4) 0.013(3) 0.005(3) 0.001(3) -0.002(3) B25 0.023(4) 0.019(3) 0.012(3) -0.004(3) 0.006(3) 0.000(3) B26 0.016(4) 0.013(3) 0.013(3) 0.001(3) 0.001(3) 0.002(3) B27 0.028(3) 0.019(3) 0.007(3) 0.003(2) -0.004(2) -0.001(2) B28 0.036(5) 0.015(3) 0.012(3) 0.006(3) -0.003(3) -0.001(3) B29 0.032(4) 0.020(3) 0.011(3) 0.000(3) 0.007(3) -0.005(3) B30 0.039(5) 0.016(3) 0.012(3) 0.000(3) 0.014(3) -0.003(3) B31 0.028(4) 0.014(3) 0.007(3) 0.002(3) 0.000(3) 0.001(3) B32 0.038(5) 0.025(4) 0.008(3) -0.002(3) 0.001(3) -0.004(3) C33 0.013(3) 0.016(3) 0.010(3) 0.000(2) -0.001(2) 0.001(2) C34 0.031(4) 0.012(3) 0.015(3) 0.002(2) 0.002(2) -0.006(2) C35 0.030(4) 0.021(3) 0.025(3) 0.005(3) 0.003(3) -0.010(3) C36 0.013(4) 0.034(3) 0.035(4) 0.007(3) -0.002(3) -0.008(3) C37 0.016(4) 0.034(3) 0.032(3) 0.004(3) 0.009(3) 0.004(3) C38 0.021(3) 0.026(3) 0.023(3) 0.000(3) -0.001(3) 0.002(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 Se1 C1 1.945(5) . ? Se1 Se2 2.3038(7) . ? Se2 C21 1.949(5) . ? C1 B4 1.694(7) . ? C1 B5 1.701(7) . ? C1 B6 1.704(7) . ? C1 B3 1.723(7) . ? C1 C2 1.726(6) . ? C2 C13 1.499(7) . ? C2 B7 1.702(7) . ? C2 B11 1.710(7) . ? C2 B6 1.736(7) . ? C2 B3 1.738(8) . ? B3 B8 1.769(9) . ? B3 B4 1.781(9) . ? B3 B7 1.789(8) . ? B3 H3 1.1200 . ? B4 B5 1.782(8) . ? B4 B8 1.784(8) . ? B4 B9 1.789(9) . ? B4 H4 1.1200 . ? B5 B6 1.768(8) . ? B5 B9 1.770(10) . ? B5 B10 1.783(9) . ? B5 H5 1.1200 . ? B6 B10 1.778(8) . ? B6 B11 1.787(8) . ? B6 H6 1.1200 . ? B7 B8 1.764(9) . ? B7 B12 1.765(8) . ? B7 B11 1.783(8) . ? B7 H7 1.1200 . ? B8 B12 1.777(8) . ? B8 B9 1.798(9) . ? B8 H8 1.1200 . ? B9 B12 1.780(10) . ? B9 B10 1.789(9) . ? B9 H9 1.1200 . ? B10 B12 1.778(9) . ? B10 B11 1.797(8) . ? B10 H10 1.1200 . ? B11 B12 1.798(9) . ? B11 H11 1.1200 . ? B12 H12 1.1200 . ? C13 C14 1.388(7) . ? C13 C18 1.396(7) . ? C14 C15 1.380(8) . ? C14 H14 0.9500 . ? C15 C16 1.386(9) . ? C15 H15 0.9500 . ? C16 C17 1.367(9) . ? C16 H16 0.9500 . ? C17 C18 1.405(8) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C21 B24 1.697(7) . ? C21 B25 1.709(8) . ? C21 B26 1.715(7) . ? C21 B23 1.719(8) . ? C21 C22 1.741(7) . ? C22 C33 1.504(7) . ? C22 B31 1.705(7) . ? C22 B27 1.715(7) . ? C22 B23 1.735(7) . ? C22 B26 1.745(7) . ? B23 B28 1.768(9) . ? B23 B24 1.783(9) . ? B23 B27 1.791(8) . ? B23 H23 1.1200 . ? B24 B28 1.753(9) . ? B24 B29 1.780(9) . ? B24 B25 1.797(8) . ? B24 H24 1.1200 . ? B25 B26 1.785(8) . ? B25 B29 1.786(9) . ? B25 B30 1.789(9) . ? B25 H25 1.1200 . ? B26 B30 1.800(8) . ? B26 B31 1.800(8) . ? B26 H26 1.1200 . ? B27 B28 1.777(9) . ? B27 B31 1.789(9) . ? B27 B32 1.792(10) . ? B27 H27 1.1200 . ? B28 B29 1.784(10) . ? B28 B32 1.789(9) . ? B28 H28 1.1200 . ? B29 B32 1.766(10) . ? B29 B30 1.787(9) . ? B29 H29 1.1200 . ? B30 B32 1.764(10) . ? B30 B31 1.771(9) . ? B30 H30 1.1200 . ? B31 B32 1.770(8) . ? B31 H31 1.1200 . ? B32 H32 1.1200 . ? C33 C38 1.382(7) . ? C33 C34 1.385(7) . ? C34 C35 1.384(7) . ? C34 H34 0.9500 . ? C35 C36 1.367(8) . ? C35 H35 0.9500 . ? C36 C37 1.388(7) . ? C36 H36 0.9500 . ? C37 C38 1.389(8) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Se1 Se2 102.58(13) . . ? C21 Se2 Se1 103.54(14) . . ? B4 C1 B5 63.3(3) . . ? B4 C1 B6 114.6(4) . . ? B5 C1 B6 62.6(3) . . ? B4 C1 B3 62.8(3) . . ? B5 C1 B3 114.6(4) . . ? B6 C1 B3 113.0(4) . . ? B4 C1 C2 111.0(4) . . ? B5 C1 C2 111.0(4) . . ? B6 C1 C2 60.8(3) . . ? B3 C1 C2 60.5(3) . . ? B4 C1 Se1 124.5(3) . . ? B5 C1 Se1 121.4(3) . . ? B6 C1 Se1 113.7(3) . . ? B3 C1 Se1 118.4(3) . . ? C2 C1 Se1 115.3(3) . . ? C13 C2 B7 120.7(4) . . ? C13 C2 B11 121.5(4) . . ? B7 C2 B11 63.0(3) . . ? C13 C2 C1 120.2(4) . . ? B7 C2 C1 108.8(4) . . ? B11 C2 C1 109.3(4) . . ? C13 C2 B6 120.1(4) . . ? B7 C2 B6 112.7(4) . . ? B11 C2 B6 62.5(3) . . ? C1 C2 B6 59.0(3) . . ? C13 C2 B3 116.5(4) . . ? B7 C2 B3 62.6(3) . . ? B11 C2 B3 114.3(4) . . ? C1 C2 B3 59.7(3) . . ? B6 C2 B3 110.7(4) . . ? C1 B3 C2 59.8(3) . . ? C1 B3 B8 104.4(4) . . ? C2 B3 B8 104.7(4) . . ? C1 B3 B4 57.8(3) . . ? C2 B3 B4 106.4(4) . . ? B8 B3 B4 60.3(3) . . ? C1 B3 B7 105.0(4) . . ? C2 B3 B7 57.7(3) . . ? B8 B3 B7 59.5(3) . . ? B4 B3 B7 107.7(4) . . ? C1 B3 H3 124.0 . . ? C2 B3 H3 123.4 . . ? B8 B3 H3 123.3 . . ? B4 B3 H3 121.9 . . ? B7 B3 H3 122.8 . . ? C1 B4 B3 59.4(3) . . ? C1 B4 B5 58.5(3) . . ? B3 B4 B5 108.0(4) . . ? C1 B4 B8 105.0(4) . . ? B3 B4 B8 59.5(3) . . ? B5 B4 B8 107.6(4) . . ? C1 B4 B9 104.7(4) . . ? B3 B4 B9 108.0(5) . . ? B5 B4 B9 59.4(4) . . ? B8 B4 B9 60.4(4) . . ? C1 B4 H4 124.4 . . ? B3 B4 H4 121.4 . . ? B5 B4 H4 121.9 . . ? B8 B4 H4 122.4 . . ? B9 B4 H4 122.4 . . ? C1 B5 B6 58.8(3) . . ? C1 B5 B9 105.2(4) . . ? B6 B5 B9 108.2(5) . . ? C1 B5 B4 58.1(3) . . ? B6 B5 B4 107.3(4) . . ? B9 B5 B4 60.5(3) . . ? C1 B5 B10 105.6(4) . . ? B6 B5 B10 60.1(3) . . ? B9 B5 B10 60.5(4) . . ? B4 B5 B10 108.6(4) . . ? C1 B5 H5 124.5 . . ? B6 B5 H5 121.8 . . ? B9 B5 H5 121.9 . . ? B4 B5 H5 121.7 . . ? B10 B5 H5 121.7 . . ? C1 B6 C2 60.2(3) . . ? C1 B6 B5 58.6(3) . . ? C2 B6 B5 107.3(4) . . ? C1 B6 B10 105.6(4) . . ? C2 B6 B10 105.6(4) . . ? B5 B6 B10 60.4(3) . . ? C1 B6 B11 106.7(4) . . ? C2 B6 B11 58.0(3) . . ? B5 B6 B11 109.3(4) . . ? B10 B6 B11 60.5(3) . . ? C1 B6 H6 123.1 . . ? C2 B6 H6 123.1 . . ? B5 B6 H6 121.2 . . ? B10 B6 H6 122.8 . . ? B11 B6 H6 121.6 . . ? C2 B7 B8 106.5(4) . . ? C2 B7 B12 106.1(4) . . ? B8 B7 B12 60.5(3) . . ? C2 B7 B11 58.7(3) . . ? B8 B7 B11 109.4(4) . . ? B12 B7 B11 60.9(3) . . ? C2 B7 B3 59.7(3) . . ? B8 B7 B3 59.7(3) . . ? B12 B7 B3 108.0(4) . . ? B11 B7 B3 108.4(4) . . ? C2 B7 H7 123.7 . . ? B8 B7 H7 121.5 . . ? B12 B7 H7 121.8 . . ? B11 B7 H7 120.9 . . ? B3 B7 H7 121.6 . . ? B7 B8 B3 60.8(4) . . ? B7 B8 B12 59.8(4) . . ? B3 B8 B12 108.4(5) . . ? B7 B8 B4 108.7(5) . . ? B3 B8 B4 60.2(4) . . ? B12 B8 B4 107.8(5) . . ? B7 B8 B9 107.9(5) . . ? B3 B8 B9 108.2(5) . . ? B12 B8 B9 59.7(4) . . ? B4 B8 B9 59.9(4) . . ? B7 B8 H8 121.3 . . ? B3 B8 H8 121.2 . . ? B12 B8 H8 121.9 . . ? B4 B8 H8 121.6 . . ? B9 B8 H8 122.0 . . ? B5 B9 B12 107.7(5) . . ? B5 B9 B4 60.1(4) . . ? B12 B9 B4 107.5(5) . . ? B5 B9 B10 60.1(4) . . ? B12 B9 B10 59.8(4) . . ? B4 B9 B10 108.1(5) . . ? B5 B9 B8 107.5(5) . . ? B12 B9 B8 59.6(4) . . ? B4 B9 B8 59.7(3) . . ? B10 B9 B8 107.4(5) . . ? B5 B9 H9 121.7 . . ? B12 B9 H9 122.1 . . ? B4 B9 H9 121.8 . . ? B10 B9 H9 121.8 . . ? B8 B9 H9 122.3 . . ? B6 B10 B12 107.2(4) . . ? B6 B10 B5 59.5(3) . . ? B12 B10 B5 107.2(4) . . ? B6 B10 B9 106.9(4) . . ? B12 B10 B9 59.9(4) . . ? B5 B10 B9 59.4(4) . . ? B6 B10 B11 60.0(3) . . ? B12 B10 B11 60.4(3) . . ? B5 B10 B11 108.2(4) . . ? B9 B10 B11 108.5(5) . . ? B6 B10 H10 122.5 . . ? B12 B10 H10 122.1 . . ? B5 B10 H10 122.1 . . ? B9 B10 H10 122.0 . . ? B11 B10 H10 121.0 . . ? C2 B11 B7 58.3(3) . . ? C2 B11 B6 59.5(3) . . ? B7 B11 B6 106.6(4) . . ? C2 B11 B10 105.9(4) . . ? B7 B11 B10 106.8(4) . . ? B6 B11 B10 59.5(3) . . ? C2 B11 B12 104.3(4) . . ? B7 B11 B12 59.1(3) . . ? B6 B11 B12 106.0(4) . . ? B10 B11 B12 59.3(3) . . ? C2 B11 H11 123.8 . . ? B7 B11 H11 122.6 . . ? B6 B11 H11 122.4 . . ? B10 B11 H11 122.4 . . ? B12 B11 H11 123.5 . . ? B7 B12 B8 59.7(3) . . ? B7 B12 B10 108.4(4) . . ? B8 B12 B10 108.8(5) . . ? B7 B12 B9 108.7(4) . . ? B8 B12 B9 60.7(4) . . ? B10 B12 B9 60.4(4) . . ? B7 B12 B11 60.1(3) . . ? B8 B12 B11 108.2(4) . . ? B10 B12 B11 60.3(4) . . ? B9 B12 B11 108.9(5) . . ? B7 B12 H12 121.7 . . ? B8 B12 H12 121.5 . . ? B10 B12 H12 121.3 . . ? B9 B12 H12 121.0 . . ? B11 B12 H12 121.5 . . ? C14 C13 C18 118.8(5) . . ? C14 C13 C2 121.3(4) . . ? C18 C13 C2 119.8(5) . . ? C15 C14 C13 120.8(5) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C14 C15 C16 120.2(6) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C17 C16 C15 120.1(6) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 120.2(6) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C13 C18 C17 119.9(5) . . ? C13 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? B24 C21 B25 63.7(3) . . ? B24 C21 B26 115.0(4) . . ? B25 C21 B26 62.8(3) . . ? B24 C21 B23 62.9(3) . . ? B25 C21 B23 115.3(4) . . ? B26 C21 B23 113.1(4) . . ? B24 C21 C22 110.5(4) . . ? B25 C21 C22 110.9(4) . . ? B26 C21 C22 60.6(3) . . ? B23 C21 C22 60.2(3) . . ? B24 C21 Se2 125.5(3) . . ? B25 C21 Se2 120.6(4) . . ? B26 C21 Se2 112.2(3) . . ? B23 C21 Se2 119.2(3) . . ? C22 C21 Se2 115.4(3) . . ? C33 C22 B31 120.5(4) . . ? C33 C22 B27 122.4(4) . . ? B31 C22 B27 63.1(3) . . ? C33 C22 B23 119.8(4) . . ? B31 C22 B23 113.4(4) . . ? B27 C22 B23 62.6(3) . . ? C33 C22 C21 120.2(4) . . ? B31 C22 C21 108.4(4) . . ? B27 C22 C21 108.8(4) . . ? B23 C22 C21 59.3(3) . . ? C33 C22 B26 116.0(4) . . ? B31 C22 B26 62.9(3) . . ? B27 C22 B26 114.1(4) . . ? B23 C22 B26 110.8(4) . . ? C21 C22 B26 58.9(3) . . ? C21 B23 C22 60.5(3) . . ? C21 B23 B28 104.0(4) . . ? C22 B23 B28 104.9(4) . . ? C21 B23 B24 57.9(3) . . ? C22 B23 B24 106.8(4) . . ? B28 B23 B24 59.2(4) . . ? C21 B23 B27 106.3(4) . . ? C22 B23 B27 58.2(3) . . ? B28 B23 B27 59.9(4) . . ? B24 B23 B27 107.8(4) . . ? C21 B23 H23 123.5 . . ? C22 B23 H23 122.9 . . ? B28 B23 H23 123.9 . . ? B24 B23 H23 122.2 . . ? B27 B23 H23 122.1 . . ? C21 B24 B28 105.5(4) . . ? C21 B24 B29 105.1(4) . . ? B28 B24 B29 60.7(4) . . ? C21 B24 B23 59.1(3) . . ? B28 B24 B23 60.0(4) . . ? B29 B24 B23 108.4(4) . . ? C21 B24 B25 58.5(3) . . ? B28 B24 B25 108.4(4) . . ? B29 B24 B25 59.9(3) . . ? B23 B24 B25 107.9(4) . . ? C21 B24 H24 124.4 . . ? B28 B24 H24 121.8 . . ? B29 B24 H24 122.0 . . ? B23 B24 H24 121.4 . . ? B25 B24 H24 121.7 . . ? C21 B25 B26 58.7(3) . . ? C21 B25 B29 104.3(4) . . ? B26 B25 B29 108.1(4) . . ? C21 B25 B30 105.1(4) . . ? B26 B25 B30 60.5(3) . . ? B29 B25 B30 60.0(4) . . ? C21 B25 B24 57.8(3) . . ? B26 B25 B24 106.9(4) . . ? B29 B25 B24 59.6(3) . . ? B30 B25 B24 107.3(5) . . ? C21 B25 H25 124.9 . . ? B26 B25 H25 121.5 . . ? B29 B25 H25 122.5 . . ? B30 B25 H25 122.1 . . ? B24 B25 H25 122.5 . . ? C21 B26 C22 60.4(3) . . ? C21 B26 B25 58.4(3) . . ? C22 B26 B25 107.2(4) . . ? C21 B26 B30 104.4(4) . . ? C22 B26 B30 104.2(4) . . ? B25 B26 B30 59.9(3) . . ? C21 B26 B31 105.3(4) . . ? C22 B26 B31 57.5(3) . . ? B25 B26 B31 107.3(4) . . ? B30 B26 B31 59.0(4) . . ? C21 B26 H26 123.5 . . ? C22 B26 H26 123.1 . . ? B25 B26 H26 121.7 . . ? B30 B26 H26 123.9 . . ? B31 B26 H26 123.1 . . ? C22 B27 B28 105.4(4) . . ? C22 B27 B31 58.2(3) . . ? B28 B27 B31 107.1(5) . . ? C22 B27 B23 59.3(3) . . ? B28 B27 B23 59.4(3) . . ? B31 B27 B23 106.8(4) . . ? C22 B27 B32 104.6(5) . . ? B28 B27 B32 60.2(4) . . ? B31 B27 B32 59.2(3) . . ? B23 B27 B32 107.1(5) . . ? C22 B27 H27 124.2 . . ? B28 B27 H27 122.3 . . ? B31 B27 H27 122.5 . . ? B23 B27 H27 122.0 . . ? B32 B27 H27 122.7 . . ? B24 B28 B23 60.9(4) . . ? B24 B28 B27 109.8(4) . . ? B23 B28 B27 60.7(3) . . ? B24 B28 B29 60.4(4) . . ? B23 B28 B29 108.9(4) . . ? B27 B28 B29 108.7(5) . . ? B24 B28 B32 108.0(5) . . ? B23 B28 B32 108.3(4) . . ? B27 B28 B32 60.4(4) . . ? B29 B28 B32 59.2(4) . . ? B24 B28 H28 120.9 . . ? B23 B28 H28 121.0 . . ? B27 B28 H28 120.7 . . ? B29 B28 H28 121.6 . . ? B32 B28 H28 122.2 . . ? B32 B29 B24 107.8(5) . . ? B32 B29 B28 60.5(4) . . ? B24 B29 B28 58.9(4) . . ? B32 B29 B25 108.0(4) . . ? B24 B29 B25 60.5(3) . . ? B28 B29 B25 107.5(4) . . ? B32 B29 B30 59.5(4) . . ? B24 B29 B30 108.1(4) . . ? B28 B29 B30 107.6(4) . . ? B25 B29 B30 60.1(3) . . ? B32 B29 H29 121.7 . . ? B24 B29 H29 121.9 . . ? B28 B29 H29 122.2 . . ? B25 B29 H29 121.6 . . ? B30 B29 H29 121.9 . . ? B32 B30 B31 60.1(4) . . ? B32 B30 B29 59.6(4) . . ? B31 B30 B29 107.8(5) . . ? B32 B30 B25 107.9(5) . . ? B31 B30 B25 108.4(4) . . ? B29 B30 B25 59.9(3) . . ? B32 B30 B26 108.1(5) . . ? B31 B30 B26 60.5(3) . . ? B29 B30 B26 107.4(4) . . ? B25 B30 B26 59.7(3) . . ? B32 B30 H30 121.8 . . ? B31 B30 H30 121.3 . . ? B29 B30 H30 122.2 . . ? B25 B30 H30 121.7 . . ? B26 B30 H30 121.8 . . ? C22 B31 B32 106.0(4) . . ? C22 B31 B30 107.1(4) . . ? B32 B31 B30 59.8(4) . . ? C22 B31 B27 58.7(3) . . ? B32 B31 B27 60.5(4) . . ? B30 B31 B27 108.8(5) . . ? C22 B31 B26 59.6(3) . . ? B32 B31 B26 107.8(4) . . ? B30 B31 B26 60.5(3) . . ? B27 B31 B26 108.0(4) . . ? C22 B31 H31 123.3 . . ? B32 B31 H31 122.3 . . ? B30 B31 H31 121.4 . . ? B27 B31 H31 121.4 . . ? B26 B31 H31 121.5 . . ? B30 B32 B29 60.8(4) . . ? B30 B32 B31 60.2(4) . . ? B29 B32 B31 108.8(5) . . ? B30 B32 B28 108.4(5) . . ? B29 B32 B28 60.3(4) . . ? B31 B32 B28 107.4(4) . . ? B30 B32 B27 108.9(5) . . ? B29 B32 B27 108.8(4) . . ? B31 B32 B27 60.3(3) . . ? B28 B32 B27 59.5(4) . . ? B30 B32 H32 121.0 . . ? B29 B32 H32 120.9 . . ? B31 B32 H32 121.7 . . ? B28 B32 H32 122.2 . . ? B27 B32 H32 121.3 . . ? C38 C33 C34 118.3(5) . . ? C38 C33 C22 122.1(4) . . ? C34 C33 C22 119.5(4) . . ? C35 C34 C33 120.7(5) . . ? C35 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? C36 C35 C34 120.9(5) . . ? C36 C35 H35 119.5 . . ? C34 C35 H35 119.5 . . ? C35 C36 C37 119.2(5) . . ? C35 C36 H36 120.4 . . ? C37 C36 H36 120.4 . . ? C36 C37 C38 119.9(5) . . ? C36 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? C33 C38 C37 121.0(5) . . ? C33 C38 H38 119.5 . . ? C37 C38 H38 119.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Se1 Se2 C21 -98.9(2) . . . . ? C2 C1 Se1 Se2 -113.7(3) . . . . ? C22 C21 Se2 Se1 -116.3(3) . . . . ? Se1 C1 C2 C13 4.8(5) . . . . ? Se2 C21 C22 C33 1.6(5) . . . . ? C33 C22 C2 C13 -12.7(4) . . . . ? C1 C2 C13 C14 -73.3(6) . . . . ? C1 C2 C13 C18 110.3(5) . . . . ? C21 C22 C33 C34 -115.5(5) . . . . ? C21 C22 C33 C38 67.1(6) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.64 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.486 _refine_diff_density_min -0.429 _refine_diff_density_rms 0.097 data_compound_4 _database_code_depnum_ccdc_archive 'CCDC 616225' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C21 H28 Au B10 P Se' _chemical_formula_sum 'C21 H28 Au B10 P Se' _chemical_formula_weight 695.43 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 '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 7.93370(10) _cell_length_b 18.8060(4) _cell_length_c 17.7509(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.4646(7) _cell_angle_gamma 90.00 _cell_volume 2647.59(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9741 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 25.028 _exptl_crystal_description needle _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.745 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 7.002 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 16157 _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 25.04 _reflns_number_total 4651 _reflns_number_gt 3993 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _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 3.02 at 0.1348 0.1043 0.6341 [ 1.26 A from AU ] Deepest hole -0.79 at 0.0785 0.0573 0.6177 [ 0.87 A from AU ] ; _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^)+(0.0158P)^2^+13.4071P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4651 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0401 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0672 _refine_ls_wR_factor_gt 0.0638 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 Au Au 0.08405(2) 0.076198(11) 0.573107(11) 0.02471(8) Uani 1 d . . . Se Se -0.08539(7) -0.02304(3) 0.61456(3) 0.03023(14) Uani 1 d . . . P P 0.23905(16) 0.17382(7) 0.54457(7) 0.0211(3) Uani 1 d . . . C1 C -0.0805(6) -0.0001(3) 0.7220(3) 0.0233(11) Uani 1 d . . . C2 C -0.2579(6) 0.0325(3) 0.7617(3) 0.0250(12) Uani 1 d . . . B3 B -0.1982(8) -0.0538(3) 0.7784(4) 0.0271(14) Uani 1 d . . . H3 H -0.2710 -0.1009 0.7568 0.033 Uiso 1 calc R . . B4 B 0.0248(7) -0.0534(3) 0.7842(4) 0.0286(14) Uani 1 d . . . H4 H 0.1008 -0.1008 0.7676 0.034 Uiso 1 calc R . . B5 B 0.0928(8) 0.0346(3) 0.7663(4) 0.0286(14) Uani 1 d . . . H5 H 0.2143 0.0455 0.7377 0.034 Uiso 1 calc R . . B6 B -0.0894(7) 0.0876(3) 0.7497(4) 0.0251(13) Uani 1 d . . . H6 H -0.0908 0.1333 0.7092 0.030 Uiso 1 calc R . . B7 B -0.2751(8) 0.0014(4) 0.8514(4) 0.0345(16) Uani 1 d . . . H7 H -0.3977 -0.0096 0.8791 0.041 Uiso 1 calc R . . B8 B -0.0934(8) -0.0525(4) 0.8675(4) 0.0334(15) Uani 1 d . . . H8 H -0.0948 -0.0994 0.9063 0.040 Uiso 1 calc R . . B9 B 0.0871(8) 0.0033(4) 0.8605(4) 0.0326(15) Uani 1 d . . . H9 H 0.2049 -0.0061 0.8952 0.039 Uiso 1 calc R . . B10 B 0.0172(8) 0.0910(3) 0.8381(4) 0.0306(15) Uani 1 d . . . H10 H 0.0887 0.1393 0.8573 0.037 Uiso 1 calc R . . B11 B -0.2071(8) 0.0890(3) 0.8332(4) 0.0294(14) Uani 1 d . . . H11 H -0.2847 0.1362 0.8490 0.035 Uiso 1 calc R . . B12 B -0.0991(9) 0.0362(4) 0.9014(4) 0.0362(16) Uani 1 d . . . H12 H -0.1042 0.0481 0.9631 0.043 Uiso 1 calc R . . C13 C -0.4111(7) 0.0444(3) 0.7113(3) 0.0364(14) Uani 1 d . . . H13A H -0.4814 0.0016 0.7107 0.055 Uiso 1 calc R . . H13B H -0.3755 0.0549 0.6600 0.055 Uiso 1 calc R . . H13C H -0.4761 0.0846 0.7304 0.055 Uiso 1 calc R . . C14 C 0.1053(6) 0.2490(3) 0.5201(3) 0.0219(11) Uani 1 d . . . C15 C 0.1560(7) 0.3190(3) 0.5337(3) 0.0304(13) Uani 1 d . . . H15 H 0.2640 0.3283 0.5558 0.037 Uiso 1 calc R . . C16 C 0.0505(7) 0.3745(3) 0.5151(3) 0.0349(14) Uani 1 d . . . H16 H 0.0856 0.4221 0.5244 0.042 Uiso 1 calc R . . C17 C -0.1080(7) 0.3611(3) 0.4826(3) 0.0328(13) Uani 1 d . . . H17 H -0.1819 0.3993 0.4704 0.039 Uiso 1 calc R . . C18 C -0.1564(7) 0.2929(3) 0.4685(3) 0.0338(14) Uani 1 d . . . H18 H -0.2638 0.2840 0.4455 0.041 Uiso 1 calc R . . C19 C -0.0517(6) 0.2362(3) 0.4871(3) 0.0297(13) Uani 1 d . . . H19 H -0.0875 0.1888 0.4772 0.036 Uiso 1 calc R . . C20 C 0.3703(6) 0.2042(3) 0.6238(3) 0.0248(12) Uani 1 d . . . C21 C 0.3014(7) 0.2045(3) 0.6951(3) 0.0307(13) Uani 1 d . . . H21 H 0.1896 0.1880 0.7017 0.037 Uiso 1 calc R . . C22 C 0.3958(8) 0.2287(3) 0.7561(3) 0.0369(14) Uani 1 d . . . H22 H 0.3491 0.2282 0.8048 0.044 Uiso 1 calc R . . C23 C 0.5573(8) 0.2536(3) 0.7470(4) 0.0399(15) Uani 1 d . . . H23 H 0.6207 0.2713 0.7890 0.048 Uiso 1 calc R . . C24 C 0.6264(7) 0.2528(3) 0.6767(4) 0.0381(15) Uani 1 d . . . H24 H 0.7387 0.2690 0.6706 0.046 Uiso 1 calc R . . C25 C 0.5340(7) 0.2287(3) 0.6149(3) 0.0325(13) Uani 1 d . . . H25 H 0.5821 0.2287 0.5664 0.039 Uiso 1 calc R . . C26 C 0.3830(6) 0.1617(3) 0.4684(3) 0.0234(11) Uani 1 d . . . C27 C 0.4953(7) 0.1045(3) 0.4736(4) 0.0343(13) Uani 1 d . . . H27 H 0.4922 0.0729 0.5154 0.041 Uiso 1 calc R . . C28 C 0.6102(7) 0.0942(4) 0.4179(4) 0.0464(18) Uani 1 d . . . H28 H 0.6888 0.0562 0.4221 0.056 Uiso 1 calc R . . C29 C 0.6125(8) 0.1381(4) 0.3565(4) 0.0467(18) Uani 1 d . . . H29 H 0.6908 0.1297 0.3179 0.056 Uiso 1 calc R . . C30 C 0.5014(8) 0.1947(3) 0.3503(3) 0.0402(15) Uani 1 d . . . H30 H 0.5036 0.2253 0.3078 0.048 Uiso 1 calc R . . C31 C 0.3871(6) 0.2065(3) 0.4066(3) 0.0287(13) Uani 1 d . . . H31 H 0.3111 0.2454 0.4028 0.034 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au 0.02568(12) 0.02452(12) 0.02393(12) 0.00040(9) 0.00075(8) -0.00378(9) Se 0.0357(3) 0.0282(3) 0.0269(3) -0.0041(2) 0.0028(2) -0.0098(2) P 0.0204(6) 0.0225(7) 0.0202(7) 0.0023(6) -0.0001(5) -0.0001(5) C1 0.022(3) 0.024(3) 0.024(3) 0.000(2) 0.005(2) -0.001(2) C2 0.019(3) 0.028(3) 0.028(3) -0.001(2) 0.005(2) 0.003(2) B3 0.027(3) 0.024(3) 0.031(4) 0.004(3) 0.003(3) 0.000(2) B4 0.021(3) 0.030(4) 0.034(4) 0.000(3) -0.003(3) 0.003(3) B5 0.023(3) 0.029(4) 0.033(4) -0.001(3) -0.004(3) -0.002(3) B6 0.029(3) 0.017(3) 0.029(3) 0.001(3) -0.003(2) -0.003(2) B7 0.036(4) 0.037(4) 0.031(4) 0.007(3) 0.007(3) 0.002(3) B8 0.038(4) 0.031(4) 0.032(4) 0.010(3) 0.004(3) 0.007(3) B9 0.033(4) 0.033(4) 0.032(4) -0.003(3) -0.008(3) 0.006(3) B10 0.030(3) 0.029(4) 0.032(4) -0.002(3) -0.010(3) 0.000(3) B11 0.033(3) 0.028(4) 0.028(3) 0.001(3) 0.001(3) 0.007(3) B12 0.049(4) 0.034(4) 0.025(4) 0.001(3) -0.002(3) 0.009(3) C13 0.023(3) 0.041(4) 0.045(4) -0.003(3) -0.006(2) 0.004(2) C14 0.022(3) 0.026(3) 0.018(3) -0.001(2) 0.002(2) 0.005(2) C15 0.025(3) 0.034(3) 0.032(3) -0.004(3) -0.004(2) 0.000(2) C16 0.036(3) 0.026(3) 0.042(4) -0.005(3) -0.004(3) 0.005(2) C17 0.037(3) 0.035(3) 0.027(3) 0.005(3) 0.002(2) 0.013(3) C18 0.021(3) 0.047(4) 0.032(3) 0.006(3) -0.003(2) 0.005(3) C19 0.025(3) 0.030(3) 0.034(3) 0.002(3) -0.005(2) -0.004(2) C20 0.025(3) 0.023(3) 0.026(3) 0.003(2) -0.006(2) 0.002(2) C21 0.034(3) 0.030(3) 0.028(3) 0.002(3) -0.001(2) 0.003(2) C22 0.051(4) 0.036(3) 0.023(3) -0.003(3) -0.007(3) 0.006(3) C23 0.054(4) 0.027(3) 0.037(4) 0.000(3) -0.026(3) -0.001(3) C24 0.028(3) 0.034(3) 0.052(4) 0.001(3) -0.017(3) -0.005(3) C25 0.032(3) 0.031(3) 0.034(3) 0.005(3) -0.004(2) -0.003(2) C26 0.020(3) 0.023(3) 0.027(3) -0.003(2) 0.000(2) -0.003(2) C27 0.028(3) 0.031(3) 0.044(4) -0.001(3) 0.000(3) 0.002(2) C28 0.029(3) 0.037(4) 0.074(5) -0.023(4) 0.010(3) 0.001(3) C29 0.035(3) 0.052(4) 0.054(4) -0.030(4) 0.025(3) -0.014(3) C30 0.044(4) 0.046(4) 0.032(3) -0.007(3) 0.011(3) -0.018(3) C31 0.027(3) 0.033(3) 0.026(3) -0.006(2) 0.003(2) -0.006(2) _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 Au P 2.2740(13) . ? Au Se 2.4254(6) . ? Se C1 1.955(5) . ? P C26 1.806(5) . ? P C14 1.814(5) . ? P C20 1.821(5) . ? C1 B4 1.696(8) . ? C1 B5 1.697(8) . ? C1 C2 1.703(7) . ? C1 B3 1.715(8) . ? C1 B6 1.722(8) . ? C2 C13 1.508(7) . ? C2 B11 1.696(8) . ? C2 B7 1.705(8) . ? C2 B6 1.709(8) . ? C2 B3 1.714(8) . ? B3 B8 1.768(9) . ? B3 B4 1.769(8) . ? B3 B7 1.780(9) . ? B3 H3 1.1200 . ? B4 B8 1.771(9) . ? B4 B5 1.771(9) . ? B4 B9 1.784(9) . ? B4 H4 1.1200 . ? B5 B9 1.774(9) . ? B5 B10 1.775(9) . ? B5 B6 1.775(8) . ? B5 H5 1.1200 . ? B6 B10 1.765(8) . ? B6 B11 1.771(9) . ? B6 H6 1.1200 . ? B7 B12 1.762(10) . ? B7 B11 1.767(9) . ? B7 B8 1.779(9) . ? B7 H7 1.1200 . ? B8 B12 1.774(10) . ? B8 B9 1.783(10) . ? B8 H8 1.1200 . ? B9 B12 1.773(9) . ? B9 B10 1.781(9) . ? B9 H9 1.1200 . ? B10 B11 1.780(9) . ? B10 B12 1.797(10) . ? B10 H10 1.1200 . ? B11 B12 1.771(9) . ? B11 H11 1.1200 . ? B12 H12 1.1200 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C19 1.384(7) . ? C14 C15 1.396(8) . ? C15 C16 1.373(8) . ? C15 H15 0.9500 . ? C16 C17 1.393(8) . ? C16 H16 0.9500 . ? C17 C18 1.360(8) . ? C17 H17 0.9500 . ? C18 C19 1.386(8) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.390(8) . ? C20 C25 1.391(7) . ? C21 C22 1.378(8) . ? C21 H21 0.9500 . ? C22 C23 1.378(9) . ? C22 H22 0.9500 . ? C23 C24 1.375(9) . ? C23 H23 0.9500 . ? C24 C25 1.381(8) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C31 1.384(8) . ? C26 C27 1.399(7) . ? C27 C28 1.376(9) . ? C27 H27 0.9500 . ? C28 C29 1.367(10) . ? C28 H28 0.9500 . ? C29 C30 1.385(9) . ? C29 H29 0.9500 . ? C30 C31 1.384(8) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P Au Se 174.82(4) . . ? C1 Se Au 97.40(15) . . ? C26 P C14 107.3(2) . . ? C26 P C20 104.9(2) . . ? C14 P C20 105.0(2) . . ? C26 P Au 114.89(17) . . ? C14 P Au 111.47(17) . . ? C20 P Au 112.52(18) . . ? B4 C1 B5 62.9(3) . . ? B4 C1 C2 110.0(4) . . ? B5 C1 C2 109.8(4) . . ? B4 C1 B3 62.5(3) . . ? B5 C1 B3 113.7(4) . . ? C2 C1 B3 60.2(3) . . ? B4 C1 B6 113.8(4) . . ? B5 C1 B6 62.6(3) . . ? C2 C1 B6 59.8(3) . . ? B3 C1 B6 111.8(4) . . ? B4 C1 Se 120.1(4) . . ? B5 C1 Se 122.2(3) . . ? C2 C1 Se 119.1(3) . . ? B3 C1 Se 116.2(3) . . ? B6 C1 Se 119.3(3) . . ? C13 C2 B11 121.5(4) . . ? C13 C2 C1 118.1(4) . . ? B11 C2 C1 110.6(4) . . ? C13 C2 B7 121.5(5) . . ? B11 C2 B7 62.6(4) . . ? C1 C2 B7 110.5(4) . . ? C13 C2 B6 117.2(5) . . ? B11 C2 B6 62.7(3) . . ? C1 C2 B6 60.6(3) . . ? B7 C2 B6 114.0(4) . . ? C13 C2 B3 117.3(5) . . ? B11 C2 B3 113.9(4) . . ? C1 C2 B3 60.3(3) . . ? B7 C2 B3 62.8(4) . . ? B6 C2 B3 112.5(4) . . ? C2 B3 C1 59.6(3) . . ? C2 B3 B8 105.3(4) . . ? C1 B3 B8 105.3(4) . . ? C2 B3 B4 106.1(4) . . ? C1 B3 B4 58.2(3) . . ? B8 B3 B4 60.1(4) . . ? C2 B3 B7 58.4(3) . . ? C1 B3 B7 106.4(4) . . ? B8 B3 B7 60.2(4) . . ? B4 B3 B7 108.4(5) . . ? C2 B3 H3 123.5 . . ? C1 B3 H3 123.4 . . ? B8 B3 H3 122.9 . . ? B4 B3 H3 122.0 . . ? B7 B3 H3 121.8 . . ? C1 B4 B3 59.3(3) . . ? C1 B4 B8 106.0(4) . . ? B3 B4 B8 59.9(4) . . ? C1 B4 B5 58.6(3) . . ? B3 B4 B5 107.6(4) . . ? B8 B4 B5 108.2(5) . . ? C1 B4 B9 105.3(4) . . ? B3 B4 B9 107.7(5) . . ? B8 B4 B9 60.2(4) . . ? B5 B4 B9 59.9(4) . . ? C1 B4 H4 124.0 . . ? B3 B4 H4 121.7 . . ? B8 B4 H4 121.8 . . ? B5 B4 H4 121.8 . . ? B9 B4 H4 122.4 . . ? C1 B5 B4 58.5(3) . . ? C1 B5 B9 105.6(4) . . ? B4 B5 B9 60.4(4) . . ? C1 B5 B10 106.1(4) . . ? B4 B5 B10 108.6(5) . . ? B9 B5 B10 60.2(4) . . ? C1 B5 B6 59.4(3) . . ? B4 B5 B6 107.7(4) . . ? B9 B5 B6 107.6(5) . . ? B10 B5 B6 59.6(3) . . ? C1 B5 H5 123.8 . . ? B4 B5 H5 121.5 . . ? B9 B5 H5 122.1 . . ? B10 B5 H5 121.8 . . ? B6 B5 H5 121.9 . . ? C2 B6 C1 59.5(3) . . ? C2 B6 B10 105.7(4) . . ? C1 B6 B10 105.4(4) . . ? C2 B6 B11 58.3(3) . . ? C1 B6 B11 106.2(4) . . ? B10 B6 B11 60.4(4) . . ? C2 B6 B5 106.0(4) . . ? C1 B6 B5 58.0(3) . . ? B10 B6 B5 60.2(4) . . ? B11 B6 B5 108.3(4) . . ? C2 B6 H6 123.4 . . ? C1 B6 H6 123.5 . . ? B10 B6 H6 122.6 . . ? B11 B6 H6 121.9 . . ? B5 B6 H6 122.2 . . ? C2 B7 B12 105.2(5) . . ? C2 B7 B11 58.5(3) . . ? B12 B7 B11 60.2(4) . . ? C2 B7 B8 105.2(4) . . ? B12 B7 B8 60.1(4) . . ? B11 B7 B8 108.1(5) . . ? C2 B7 B3 58.9(3) . . ? B12 B7 B3 107.5(5) . . ? B11 B7 B3 107.4(4) . . ? B8 B7 B3 59.6(4) . . ? C2 B7 H7 124.4 . . ? B12 B7 H7 122.2 . . ? B11 B7 H7 121.7 . . ? B8 B7 H7 122.2 . . ? B3 B7 H7 122.0 . . ? B3 B8 B4 60.0(3) . . ? B3 B8 B12 107.5(5) . . ? B4 B8 B12 108.1(5) . . ? B3 B8 B7 60.2(4) . . ? B4 B8 B7 108.4(5) . . ? B12 B8 B7 59.4(4) . . ? B3 B8 B9 107.8(5) . . ? B4 B8 B9 60.3(4) . . ? B12 B8 B9 59.8(4) . . ? B7 B8 B9 107.6(5) . . ? B3 B8 H8 121.8 . . ? B4 B8 H8 121.4 . . ? B12 B8 H8 122.1 . . ? B7 B8 H8 121.8 . . ? B9 B8 H8 121.9 . . ? B12 B9 B5 108.2(4) . . ? B12 B9 B10 60.8(4) . . ? B5 B9 B10 59.9(4) . . ? B12 B9 B8 59.9(4) . . ? B5 B9 B8 107.5(4) . . ? B10 B9 B8 108.4(4) . . ? B12 B9 B4 107.5(5) . . ? B5 B9 B4 59.7(4) . . ? B10 B9 B4 107.8(4) . . ? B8 B9 B4 59.5(4) . . ? B12 B9 H9 121.5 . . ? B5 B9 H9 121.9 . . ? B10 B9 H9 121.3 . . ? B8 B9 H9 121.9 . . ? B4 B9 H9 122.2 . . ? B6 B10 B5 60.2(3) . . ? B6 B10 B11 60.0(3) . . ? B5 B10 B11 107.9(4) . . ? B6 B10 B9 107.7(4) . . ? B5 B10 B9 59.9(4) . . ? B11 B10 B9 107.3(5) . . ? B6 B10 B12 107.0(4) . . ? B5 B10 B12 107.1(5) . . ? B11 B10 B12 59.3(4) . . ? B9 B10 B12 59.4(4) . . ? B6 B10 H10 121.8 . . ? B5 B10 H10 121.8 . . ? B11 B10 H10 122.0 . . ? B9 B10 H10 122.1 . . ? B12 B10 H10 122.6 . . ? C2 B11 B7 58.9(4) . . ? C2 B11 B12 105.2(4) . . ? B7 B11 B12 59.7(4) . . ? C2 B11 B6 59.0(3) . . ? B7 B11 B6 108.0(4) . . ? B12 B11 B6 107.9(4) . . ? C2 B11 B10 105.6(4) . . ? B7 B11 B10 108.7(4) . . ? B12 B11 B10 60.8(4) . . ? B6 B11 B10 59.6(3) . . ? C2 B11 H11 124.2 . . ? B7 B11 H11 121.4 . . ? B12 B11 H11 122.2 . . ? B6 B11 H11 121.8 . . ? B10 B11 H11 121.8 . . ? B7 B12 B11 60.0(4) . . ? B7 B12 B9 108.8(5) . . ? B11 B12 B9 108.0(5) . . ? B7 B12 B8 60.4(4) . . ? B11 B12 B8 108.2(5) . . ? B9 B12 B8 60.3(4) . . ? B7 B12 B10 108.1(5) . . ? B11 B12 B10 59.8(4) . . ? B9 B12 B10 59.8(4) . . ? B8 B12 B10 108.0(5) . . ? B7 B12 H12 121.3 . . ? B11 B12 H12 121.8 . . ? B9 B12 H12 121.4 . . ? B8 B12 H12 121.5 . . ? B10 B12 H12 121.9 . . ? C2 C13 H13A 109.5 . . ? C2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C19 C14 C15 119.3(5) . . ? C19 C14 P 118.7(4) . . ? C15 C14 P 122.0(4) . . ? C16 C15 C14 120.3(5) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C17 119.9(5) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C18 C17 C16 119.7(5) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C17 C18 C19 121.1(5) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C14 C19 C18 119.6(5) . . ? C14 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C21 C20 C25 119.5(5) . . ? C21 C20 P 118.3(4) . . ? C25 C20 P 122.2(4) . . ? C22 C21 C20 119.8(5) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C23 C22 C21 120.5(6) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C24 C23 C22 119.8(5) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 C25 120.6(6) . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? C24 C25 C20 119.7(6) . . ? C24 C25 H25 120.1 . . ? C20 C25 H25 120.1 . . ? C31 C26 C27 119.5(5) . . ? C31 C26 P 123.0(4) . . ? C27 C26 P 117.5(4) . . ? C28 C27 C26 119.6(6) . . ? C28 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? C29 C28 C27 120.7(6) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C28 C29 C30 120.4(6) . . ? C28 C29 H29 119.8 . . ? C30 C29 H29 119.8 . . ? C31 C30 C29 119.5(6) . . ? C31 C30 H30 120.2 . . ? C29 C30 H30 120.2 . . ? C26 C31 C30 120.3(6) . . ? C26 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Se C1 C2 C13 -1.9(6) . . . . ? C2 C1 Se Au 107.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 3.016 _refine_diff_density_min -0.786 _refine_diff_density_rms 0.116 #===END