Electronic Supplementary Material for Dalton Transactions This Journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Mark Fox' 'Lynn A. Boyd' 'William Clegg' 'R. Copley' 'Matthew G. Davidson' 'Thomas G. Hibbert' 'Judith A. K. Howard' 'Angus Mackinnon' 'Richard J. Peace' 'K. Wade' _publ_contact_author_name 'Dr Mark Fox' _publ_contact_author_address ; Department of Chemistry University of Durham South Road Durham DH1 3LE UNITED KINGDOM ; _publ_contact_author_email M.A.FOX@DURHAM.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Exo-pi-bonding to an ortho-carborane hypercarbon atom: systematic icosahedral cage distortions reflected in the structures of the fluoro-, hydroxy- and amino-carboranes, 1-X-2-Ph-1,2-C2B10H10 (X = F, OH or NH2) and related anions† ; data_1 _database_code_depnum_ccdc_archive 'CCDC 237438' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H16 B10 O, 0.5 H2 O' _chemical_formula_sum 'C8 H17 B10 O1.50' _chemical_formula_weight 245.32 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' O O 0.0106 0.0060 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' 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 12.628(3) _cell_length_b 6.8043(16) _cell_length_c 16.020(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.97(3) _cell_angle_gamma 90.00 _cell_volume 1366.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 32 _cell_measurement_theta_min 10.44 _cell_measurement_theta_max 12.37 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.52 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.193 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 508 _exptl_absorpt_coefficient_mu 0.064 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe-Siemens four-circle diffractometer' _diffrn_measurement_method '\w/\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 5 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _diffrn_reflns_number 3045 _diffrn_reflns_av_R_equivalents 0.0459 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2395 _reflns_number_gt 1910 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'local programs' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0630P)^2^+0.7063P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.004(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2395 _refine_ls_number_parameters 194 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0704 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1459 _refine_ls_wR_factor_gt 0.1326 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.024 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.48623(13) 0.6561(2) 0.44376(9) 0.0332(4) Uani 1 1 d D . . H1A H 0.489(5) 0.565(6) 0.476(3) 0.050 Uiso 0.50 1 d PD . . H1B H 0.479(4) 0.765(5) 0.462(3) 0.050 Uiso 0.50 1 d PD . . C1 C 0.48126(15) 0.6193(3) 0.35960(12) 0.0251(5) Uani 1 1 d . . . C2 C 0.59554(15) 0.5239(3) 0.32662(12) 0.0228(4) Uani 1 1 d . . . B3 B 0.48337(17) 0.3777(3) 0.33029(14) 0.0240(5) Uani 1 1 d . . . H3 H 0.4809 0.2525 0.3754 0.029 Uiso 1 1 calc R . . B4 B 0.37012(18) 0.5282(4) 0.30158(15) 0.0305(6) Uani 1 1 d . . . H4 H 0.2922 0.5011 0.3263 0.037 Uiso 1 1 calc R . . B5 B 0.4171(2) 0.7702(4) 0.28568(15) 0.0318(6) Uani 1 1 d . . . H5 H 0.3701 0.9030 0.3001 0.038 Uiso 1 1 calc R . . B6 B 0.55901(19) 0.7654(3) 0.30372(14) 0.0291(5) Uani 1 1 d . . . H6 H 0.6059 0.8946 0.3312 0.035 Uiso 1 1 calc R . . B7 B 0.56069(17) 0.3669(3) 0.24476(14) 0.0252(5) Uani 1 1 d . . . H7 H 0.6080 0.2332 0.2320 0.030 Uiso 1 1 calc R . . B8 B 0.41815(18) 0.3706(4) 0.22647(15) 0.0285(5) Uani 1 1 d . . . H8 H 0.3714 0.2394 0.2010 0.034 Uiso 1 1 calc R . . B9 B 0.3779(2) 0.6152(4) 0.19817(16) 0.0340(6) Uani 1 1 d . . . H9 H 0.3046 0.6459 0.1534 0.041 Uiso 1 1 calc R . . B10 B 0.4951(2) 0.7632(4) 0.20006(15) 0.0336(6) Uani 1 1 d . . . H10 H 0.4991 0.8921 0.1571 0.040 Uiso 1 1 calc R . . B11 B 0.60779(19) 0.6090(4) 0.22817(14) 0.0286(5) Uani 1 1 d . . . H11 H 0.6863 0.6357 0.2043 0.034 Uiso 1 1 calc R . . B12 B 0.49523(18) 0.5159(4) 0.16292(14) 0.0288(5) Uani 1 1 d . . . H12 H 0.4990 0.4810 0.0950 0.035 Uiso 1 1 calc R . . C3 C 0.68927(15) 0.4865(3) 0.39198(12) 0.0254(5) Uani 1 1 d . . . C4 C 0.70735(17) 0.3000(3) 0.42471(13) 0.0324(5) Uani 1 1 d . . . H4A H 0.6605 0.1958 0.4056 0.039 Uiso 1 1 calc R . . C5 C 0.79329(19) 0.2635(4) 0.48522(14) 0.0409(6) Uani 1 1 d . . . H5A H 0.8050 0.1345 0.5071 0.049 Uiso 1 1 calc R . . C6 C 0.86175(18) 0.4133(4) 0.51374(14) 0.0402(6) Uani 1 1 d . . . H6A H 0.9199 0.3885 0.5558 0.048 Uiso 1 1 calc R . . C7 C 0.84523(18) 0.5989(4) 0.48076(14) 0.0426(6) Uani 1 1 d . . . H7A H 0.8924 0.7024 0.5001 0.051 Uiso 1 1 calc R . . C8 C 0.76032(17) 0.6363(4) 0.41949(14) 0.0364(5) Uani 1 1 d . . . H8A H 0.7505 0.7643 0.3962 0.044 Uiso 1 1 calc R . . O2 O 0.5911(3) 0.9739(6) 0.5158(2) 0.0557(10) Uani 0.50 1 d PD . . H2A H 0.633(5) 0.940(11) 0.556(3) 0.084 Uiso 0.50 1 d PD . . H2B H 0.537(3) 0.936(10) 0.489(4) 0.084 Uiso 0.50 1 d PD . . 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 O1 0.0437(9) 0.0329(9) 0.0244(8) -0.0047(7) 0.0090(6) 0.0038(8) C1 0.0286(10) 0.0217(10) 0.0251(10) -0.0009(8) 0.0045(8) 0.0021(8) C2 0.0240(10) 0.0214(10) 0.0234(10) -0.0013(8) 0.0043(7) -0.0018(8) B3 0.0240(11) 0.0208(11) 0.0273(11) -0.0006(9) 0.0041(9) -0.0019(9) B4 0.0242(11) 0.0310(13) 0.0362(13) -0.0003(11) 0.0036(9) 0.0021(10) B5 0.0358(13) 0.0254(13) 0.0327(13) 0.0023(10) -0.0021(10) 0.0075(10) B6 0.0374(13) 0.0228(12) 0.0265(12) 0.0007(10) 0.0018(10) -0.0048(10) B7 0.0247(11) 0.0289(12) 0.0217(11) -0.0059(9) 0.0013(8) -0.0020(9) B8 0.0255(11) 0.0298(13) 0.0292(12) -0.0024(10) -0.0017(9) -0.0028(10) B9 0.0311(12) 0.0356(14) 0.0334(13) 0.0001(11) -0.0035(10) 0.0038(11) B10 0.0404(14) 0.0282(13) 0.0306(13) 0.0052(10) -0.0025(10) -0.0027(11) B11 0.0330(12) 0.0305(13) 0.0221(11) 0.0016(10) 0.0029(9) -0.0074(10) B12 0.0308(12) 0.0302(13) 0.0242(11) -0.0011(10) -0.0015(9) -0.0019(10) C3 0.0234(9) 0.0317(11) 0.0213(9) -0.0019(8) 0.0032(7) -0.0001(9) C4 0.0350(11) 0.0300(12) 0.0304(11) -0.0036(9) -0.0035(9) 0.0015(9) C5 0.0436(13) 0.0401(14) 0.0365(12) -0.0007(11) -0.0052(10) 0.0102(11) C6 0.0308(11) 0.0579(16) 0.0296(11) -0.0041(11) -0.0066(9) 0.0063(11) C7 0.0334(12) 0.0545(16) 0.0376(13) -0.0057(12) -0.0056(10) -0.0105(11) C8 0.0344(12) 0.0372(13) 0.0362(12) 0.0025(10) -0.0015(9) -0.0080(10) O2 0.067(3) 0.058(2) 0.041(2) 0.0097(19) 0.0036(17) -0.019(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 O1 H1A 0.81(3) . ? O1 H1B 0.81(3) . ? O1 C1 1.365(2) . ? H1A H1A 1.17(6) 3_666 ? C1 C2 1.723(3) . ? C1 B3 1.711(3) . ? C1 B4 1.703(3) . ? C1 B5 1.697(3) . ? C1 B6 1.722(3) . ? C2 B3 1.738(3) . ? C2 B6 1.733(3) . ? C2 B7 1.708(3) . ? C2 B11 1.705(3) . ? C2 C3 1.504(3) . ? B3 B4 1.773(3) . ? B3 B7 1.778(3) . ? B3 B8 1.765(3) . ? B4 B5 1.779(3) . ? B4 B8 1.773(3) . ? B4 B9 1.773(4) . ? B5 B6 1.781(3) . ? B5 B9 1.776(3) . ? B5 B10 1.784(4) . ? B6 B10 1.756(3) . ? B6 B11 1.777(3) . ? B7 B8 1.788(3) . ? B7 B11 1.783(3) . ? B7 B12 1.780(3) . ? B8 B9 1.782(4) . ? B8 B12 1.789(3) . ? B9 B10 1.787(4) . ? B9 B12 1.781(3) . ? B10 B11 1.781(3) . ? B10 B12 1.784(4) . ? B11 B12 1.776(3) . ? C3 C4 1.381(3) . ? C3 C8 1.394(3) . ? C4 C5 1.387(3) . ? C5 C6 1.378(3) . ? C6 C7 1.375(4) . ? C7 C8 1.386(3) . ? O2 H2A 0.81(3) . ? O2 H2B 0.80(3) . ? 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 H1A O1 H1B 118(6) . . ? H1A O1 C1 119(4) . . ? H1B O1 C1 122(4) . . ? O1 H1A H1A 169(10) . 3_666 ? O1 C1 C2 115.61(16) . . ? O1 C1 B3 116.55(16) . . ? O1 C1 B4 122.80(17) . . ? O1 C1 B5 122.61(17) . . ? O1 C1 B6 116.53(16) . . ? C2 C1 B3 60.81(12) . . ? C2 C1 B4 111.15(15) . . ? C2 C1 B5 111.14(15) . . ? C2 C1 B6 60.42(12) . . ? B3 C1 B4 62.59(13) . . ? B3 C1 B5 114.31(16) . . ? B3 C1 B6 112.51(15) . . ? B4 C1 B5 63.09(14) . . ? B4 C1 B6 114.22(16) . . ? B5 C1 B6 62.76(14) . . ? C1 C2 B3 59.25(11) . . ? C1 C2 B6 59.77(12) . . ? C1 C2 B7 108.90(14) . . ? C1 C2 B11 109.22(15) . . ? C1 C2 C3 117.91(15) . . ? B3 C2 B6 110.65(15) . . ? B3 C2 B7 62.13(12) . . ? B3 C2 B11 113.06(15) . . ? B3 C2 C3 117.09(16) . . ? B6 C2 B7 113.17(15) . . ? B6 C2 B11 62.22(13) . . ? B6 C2 C3 118.34(16) . . ? B7 C2 B11 62.99(13) . . ? B7 C2 C3 122.44(16) . . ? B11 C2 C3 123.35(16) . . ? C1 B3 C2 59.94(12) . . ? C1 B3 B4 58.51(13) . . ? C1 B3 B7 106.25(15) . . ? C1 B3 B8 105.31(16) . . ? C2 B3 B4 107.20(16) . . ? C2 B3 B7 58.10(12) . . ? C2 B3 B8 105.83(15) . . ? B4 B3 B7 108.97(16) . . ? B4 B3 B8 60.13(13) . . ? B7 B3 B8 60.64(13) . . ? C1 B4 B3 58.91(12) . . ? C1 B4 B5 58.28(13) . . ? C1 B4 B8 105.28(16) . . ? C1 B4 B9 104.63(17) . . ? B3 B4 B5 107.40(16) . . ? B3 B4 B8 59.69(13) . . ? B3 B4 B9 107.49(17) . . ? B5 B4 B8 108.37(17) . . ? B5 B4 B9 59.99(14) . . ? B8 B4 B9 60.35(14) . . ? C1 B5 B4 58.63(13) . . ? C1 B5 B6 59.31(13) . . ? C1 B5 B9 104.79(17) . . ? C1 B5 B10 105.00(16) . . ? B4 B5 B6 107.82(16) . . ? B4 B5 B9 59.84(14) . . ? B4 B5 B10 108.06(17) . . ? B6 B5 B9 107.18(17) . . ? B6 B5 B10 59.04(13) . . ? B9 B5 B10 60.25(14) . . ? C1 B6 C2 59.81(12) . . ? C1 B6 B5 57.93(13) . . ? C1 B6 B10 105.13(16) . . ? C1 B6 B11 105.98(16) . . ? C2 B6 B5 106.78(16) . . ? C2 B6 B10 105.79(16) . . ? C2 B6 B11 58.09(12) . . ? B5 B6 B10 60.56(14) . . ? B5 B6 B11 109.02(17) . . ? B10 B6 B11 60.55(14) . . ? C2 B7 B3 59.77(12) . . ? C2 B7 B8 106.10(16) . . ? C2 B7 B11 58.42(12) . . ? C2 B7 B12 105.21(16) . . ? B3 B7 B8 59.32(13) . . ? B3 B7 B11 107.51(16) . . ? B3 B7 B12 107.13(16) . . ? B8 B7 B11 108.04(17) . . ? B8 B7 B12 60.19(13) . . ? B11 B7 B12 59.80(13) . . ? B3 B8 B4 60.18(13) . . ? B3 B8 B7 60.04(12) . . ? B3 B8 B9 107.47(16) . . ? B3 B8 B12 107.29(15) . . ? B4 B8 B7 108.54(16) . . ? B4 B8 B9 59.84(14) . . ? B4 B8 B12 107.86(17) . . ? B7 B8 B9 107.76(17) . . ? B7 B8 B12 59.66(13) . . ? B9 B8 B12 59.82(14) . . ? B4 B9 B5 60.17(14) . . ? B4 B9 B8 59.80(14) . . ? B4 B9 B10 108.19(17) . . ? B4 B9 B12 108.19(17) . . ? B5 B9 B8 108.07(16) . . ? B5 B9 B10 60.09(14) . . ? B5 B9 B12 108.23(17) . . ? B8 B9 B10 108.18(17) . . ? B8 B9 B12 60.28(14) . . ? B10 B9 B12 60.02(14) . . ? B5 B10 B6 60.40(14) . . ? B5 B10 B9 59.66(14) . . ? B5 B10 B11 108.68(16) . . ? B5 B10 B12 107.74(17) . . ? B6 B10 B9 107.79(17) . . ? B6 B10 B11 60.29(13) . . ? B6 B10 B12 107.72(17) . . ? B9 B10 B11 107.88(17) . . ? B9 B10 B12 59.83(14) . . ? B11 B10 B12 59.74(13) . . ? C2 B11 B6 59.68(12) . . ? C2 B11 B7 58.58(12) . . ? C2 B11 B10 105.93(16) . . ? C2 B11 B12 105.51(16) . . ? B6 B11 B7 107.60(16) . . ? B6 B11 B10 59.15(14) . . ? B6 B11 B12 107.19(17) . . ? B7 B11 B10 108.13(16) . . ? B7 B11 B12 60.02(13) . . ? B10 B11 B12 60.22(14) . . ? B7 B12 B8 60.14(13) . . ? B7 B12 B9 108.21(16) . . ? B7 B12 B10 108.11(16) . . ? B7 B12 B11 60.18(13) . . ? B8 B12 B9 59.90(14) . . ? B8 B12 B10 107.97(17) . . ? B8 B12 B11 108.30(16) . . ? B9 B12 B10 60.14(14) . . ? B9 B12 B11 108.37(17) . . ? B10 B12 B11 60.04(14) . . ? C2 C3 C4 119.99(18) . . ? C2 C3 C8 121.23(19) . . ? C4 C3 C8 118.77(19) . . ? C3 C4 C5 120.6(2) . . ? C4 C5 C6 120.4(2) . . ? C5 C6 C7 119.5(2) . . ? C6 C7 C8 120.6(2) . . ? C3 C8 C7 120.2(2) . . ? H2A O2 H2B 139(8) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.259 _refine_diff_density_min -0.217 _refine_diff_density_rms 0.044 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 237439' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H18 P +,C8 H15 B10 O -' _chemical_formula_sum 'C27 H33 B10 O P' _chemical_formula_weight 512.60 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' O O 0.0106 0.0060 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.845(1) _cell_length_b 11.260(1) _cell_length_c 11.511(1) _cell_angle_alpha 84.97(1) _cell_angle_beta 86.27(1) _cell_angle_gamma 86.21(1) _cell_volume 1394.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 512 _cell_measurement_theta_min 10 _cell_measurement_theta_max 20 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.221 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 0.120 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; The data collection nominally covered over a hemisphere of reciprocal space, by a combination of 4 sets of \w scans; each set at different \f and/or 2\q angles and each scan covering 0.3\% in \w. Crystal to detector distance 4.5 cm. The absence of crystal decay was monitored by repeating 50 initial frames at the end of data collection and comparing duplicate reflections. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART 1K CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8 _diffrn_reflns_number 5922 _diffrn_reflns_av_R_equivalents 0.0459 _diffrn_reflns_av_sigmaI/netI 0.0503 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 24.99 _reflns_number_total 4393 _reflns_number_gt 3415 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SMART (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 1998)' _computing_publication_material 'SHELXTL (Bruker, 1998)' _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+7.2058P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4393 _refine_ls_number_parameters 354 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1304 _refine_ls_R_factor_gt 0.0980 _refine_ls_wR_factor_ref 0.2298 _refine_ls_wR_factor_gt 0.2034 _refine_ls_goodness_of_fit_ref 1.338 _refine_ls_restrained_S_all 1.338 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O O 0.3968(4) 0.6431(3) 0.3812(3) 0.0303(10) Uani 1 1 d . . . C1 C 0.3192(5) 0.6986(5) 0.3211(5) 0.0251(13) Uani 1 1 d . . . C2 C 0.3523(5) 0.8708(5) 0.2562(5) 0.0243(12) Uani 1 1 d . . . B3 B 0.2466(6) 0.8405(6) 0.3670(6) 0.0250(14) Uani 1 1 d . . . H3 H 0.2649 0.8653 0.4561 0.030 Uiso 1 1 calc R . . B4 B 0.1654(6) 0.7136(6) 0.3436(6) 0.0285(15) Uani 1 1 d . . . H4 H 0.1204 0.6575 0.4175 0.034 Uiso 1 1 calc R . . B5 B 0.2403(6) 0.6561(6) 0.2127(6) 0.0289(15) Uani 1 1 d . . . H5 H 0.2478 0.5598 0.1941 0.035 Uiso 1 1 calc R . . B6 B 0.3612(6) 0.7542(6) 0.1696(6) 0.0268(15) Uani 1 1 d . . . H6 H 0.4535 0.7231 0.1300 0.032 Uiso 1 1 calc R . . B7 B 0.2179(6) 0.9547(6) 0.2520(7) 0.0321(16) Uani 1 1 d . . . H7 H 0.2091 1.0522 0.2655 0.039 Uiso 1 1 calc R . . B8 B 0.1001(7) 0.8587(6) 0.3046(7) 0.0353(17) Uani 1 1 d . . . H8 H 0.0145 0.8938 0.3531 0.042 Uiso 1 1 calc R . . B9 B 0.0983(7) 0.7452(7) 0.2059(7) 0.0347(17) Uani 1 1 d . . . H9 H 0.0105 0.7055 0.1870 0.042 Uiso 1 1 calc R . . B10 B 0.2202(7) 0.7684(7) 0.0968(7) 0.0361(18) Uani 1 1 d . . . H10 H 0.2151 0.7434 0.0052 0.043 Uiso 1 1 calc R . . B11 B 0.2922(7) 0.8991(6) 0.1253(6) 0.0330(16) Uani 1 1 d . . . H11 H 0.3342 0.9591 0.0527 0.040 Uiso 1 1 calc R . . B12 B 0.1291(7) 0.8929(7) 0.1511(7) 0.0395(19) Uani 1 1 d . . . H12 H 0.0621 0.9492 0.0966 0.047 Uiso 1 1 calc R . . C21 C 0.4730(5) 0.9171(5) 0.2816(5) 0.0246(13) Uani 1 1 d . . . C22 C 0.5224(6) 0.8900(6) 0.3902(5) 0.0320(14) Uani 1 1 d . . . H22 H 0.4775 0.8445 0.4501 0.038 Uiso 1 1 calc R . . C23 C 0.6363(6) 0.9288(6) 0.4112(6) 0.0382(16) Uani 1 1 d . . . H23 H 0.6691 0.9085 0.4854 0.046 Uiso 1 1 calc R . . C24 C 0.7036(6) 0.9965(6) 0.3268(6) 0.0377(16) Uani 1 1 d . . . H24 H 0.7822 1.0223 0.3420 0.045 Uiso 1 1 calc R . . C25 C 0.6541(6) 1.0258(6) 0.2198(6) 0.0374(16) Uani 1 1 d . . . H25 H 0.6983 1.0735 0.1612 0.045 Uiso 1 1 calc R . . C26 C 0.5408(6) 0.9864(6) 0.1972(5) 0.0336(15) Uani 1 1 d . . . H26 H 0.5084 1.0069 0.1229 0.040 Uiso 1 1 calc R . . P P 0.72649(13) 0.49794(13) 0.27515(13) 0.0223(4) Uani 1 1 d . . . C30 C 0.6833(5) 0.5808(5) 0.3978(5) 0.0280(13) Uani 1 1 d . . . H301 H 0.6057 0.6281 0.3841 0.049(12) Uiso 1 1 calc R . . H302 H 0.7485 0.6343 0.4089 0.049(12) Uiso 1 1 calc R . . H303 H 0.6720 0.5257 0.4678 0.049(12) Uiso 1 1 calc R . . C31 C 0.7700(5) 0.5964(5) 0.1503(5) 0.0211(12) Uani 1 1 d . . . C32 C 0.7472(5) 0.7193(5) 0.1500(5) 0.0276(13) Uani 1 1 d . . . H32 H 0.7018 0.7524 0.2141 0.033 Uiso 1 1 calc R . . C33 C 0.7906(6) 0.7934(6) 0.0560(6) 0.0341(15) Uani 1 1 d . . . H33 H 0.7759 0.8776 0.0559 0.041 Uiso 1 1 calc R . . C34 C 0.8553(6) 0.7448(6) -0.0372(5) 0.0323(14) Uani 1 1 d . . . H34 H 0.8868 0.7962 -0.1006 0.039 Uiso 1 1 calc R . . C35 C 0.8752(6) 0.6228(6) -0.0402(5) 0.0301(14) Uani 1 1 d . . . H35 H 0.9171 0.5902 -0.1063 0.036 Uiso 1 1 calc R . . C36 C 0.8332(5) 0.5478(5) 0.0549(5) 0.0271(13) Uani 1 1 d . . . H36 H 0.8477 0.4637 0.0545 0.033 Uiso 1 1 calc R . . C41 C 0.5999(5) 0.4124(5) 0.2479(4) 0.0212(12) Uani 1 1 d . . . C42 C 0.5631(6) 0.4054(5) 0.1351(5) 0.0302(14) Uani 1 1 d . . . H42 H 0.6058 0.4456 0.0701 0.036 Uiso 1 1 calc R . . C43 C 0.4628(6) 0.3387(6) 0.1188(5) 0.0330(14) Uani 1 1 d . . . H43 H 0.4366 0.3340 0.0423 0.040 Uiso 1 1 calc R . . C44 C 0.4020(6) 0.2802(6) 0.2119(6) 0.0350(15) Uani 1 1 d . . . H44 H 0.3344 0.2340 0.2000 0.042 Uiso 1 1 calc R . . C45 C 0.4389(6) 0.2882(7) 0.3232(6) 0.0437(18) Uani 1 1 d . . . H45 H 0.3945 0.2488 0.3876 0.052 Uiso 1 1 calc R . . C46 C 0.5377(6) 0.3513(6) 0.3431(5) 0.0337(15) Uani 1 1 d . . . H46 H 0.5636 0.3537 0.4200 0.040 Uiso 1 1 calc R . . C51 C 0.8606(5) 0.4022(5) 0.3101(4) 0.0198(12) Uani 1 1 d . . . C52 C 0.9651(5) 0.4559(5) 0.3398(5) 0.0240(12) Uani 1 1 d . . . H52 H 0.9644 0.5404 0.3392 0.029 Uiso 1 1 calc R . . C53 C 1.0695(6) 0.3862(6) 0.3700(5) 0.0324(14) Uani 1 1 d . . . H53 H 1.1404 0.4229 0.3906 0.039 Uiso 1 1 calc R . . C54 C 1.0715(6) 0.2631(6) 0.3705(6) 0.0342(15) Uani 1 1 d . . . H54 H 1.1434 0.2154 0.3919 0.041 Uiso 1 1 calc R . . C55 C 0.9689(6) 0.2099(6) 0.3397(6) 0.0384(16) Uani 1 1 d . . . H55 H 0.9705 0.1255 0.3393 0.046 Uiso 1 1 calc R . . C56 C 0.8631(6) 0.2790(5) 0.3093(6) 0.0315(14) Uani 1 1 d . . . H56 H 0.7926 0.2419 0.2880 0.038 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O 0.033(2) 0.027(2) 0.031(2) 0.0009(18) -0.0097(19) -0.0012(18) C1 0.024(3) 0.025(3) 0.025(3) 0.003(2) -0.007(2) 0.000(2) C2 0.027(3) 0.021(3) 0.024(3) 0.000(2) 0.002(2) -0.001(2) B3 0.022(3) 0.022(3) 0.031(4) -0.001(3) -0.001(3) -0.006(3) B4 0.023(4) 0.027(4) 0.037(4) -0.004(3) -0.001(3) -0.008(3) B5 0.033(4) 0.028(4) 0.028(4) -0.007(3) -0.008(3) -0.006(3) B6 0.031(4) 0.026(4) 0.024(3) -0.005(3) -0.003(3) -0.006(3) B7 0.027(4) 0.019(3) 0.048(4) 0.006(3) -0.001(3) 0.002(3) B8 0.023(4) 0.031(4) 0.050(5) 0.005(3) 0.001(3) 0.000(3) B9 0.029(4) 0.037(4) 0.037(4) 0.008(3) -0.010(3) -0.007(3) B10 0.034(4) 0.042(4) 0.033(4) 0.008(3) -0.016(3) -0.013(3) B11 0.035(4) 0.031(4) 0.034(4) 0.006(3) -0.009(3) -0.008(3) B12 0.028(4) 0.039(4) 0.050(5) 0.019(4) -0.013(3) -0.009(3) C21 0.024(3) 0.016(3) 0.034(3) -0.003(2) 0.005(3) -0.004(2) C22 0.030(3) 0.034(3) 0.032(3) 0.003(3) -0.006(3) -0.008(3) C23 0.035(4) 0.039(4) 0.042(4) 0.005(3) -0.018(3) -0.007(3) C24 0.032(4) 0.032(4) 0.051(4) -0.004(3) -0.010(3) -0.006(3) C25 0.039(4) 0.035(4) 0.040(4) -0.007(3) 0.007(3) -0.019(3) C26 0.038(4) 0.033(3) 0.030(3) -0.001(3) 0.002(3) -0.012(3) P 0.0208(8) 0.0216(7) 0.0243(8) -0.0004(6) -0.0022(6) -0.0026(6) C30 0.029(3) 0.033(3) 0.022(3) -0.007(3) 0.002(2) 0.000(3) C31 0.021(3) 0.023(3) 0.021(3) -0.001(2) -0.005(2) -0.005(2) C32 0.026(3) 0.028(3) 0.029(3) -0.005(3) 0.002(3) 0.002(2) C33 0.034(4) 0.029(3) 0.040(4) 0.002(3) -0.014(3) -0.003(3) C34 0.030(3) 0.035(4) 0.030(3) 0.010(3) -0.007(3) -0.003(3) C35 0.029(3) 0.040(4) 0.020(3) -0.002(3) -0.002(2) 0.002(3) C36 0.024(3) 0.032(3) 0.026(3) -0.005(3) -0.004(2) -0.003(2) C41 0.023(3) 0.025(3) 0.017(3) -0.004(2) -0.003(2) -0.001(2) C42 0.033(3) 0.028(3) 0.030(3) 0.002(3) 0.001(3) -0.015(3) C43 0.035(4) 0.039(4) 0.026(3) -0.004(3) -0.007(3) -0.007(3) C44 0.028(3) 0.037(4) 0.041(4) -0.001(3) -0.006(3) -0.011(3) C45 0.040(4) 0.064(5) 0.029(3) 0.011(3) -0.006(3) -0.034(4) C46 0.036(4) 0.043(4) 0.022(3) 0.010(3) -0.012(3) -0.015(3) C51 0.020(3) 0.023(3) 0.015(3) 0.000(2) 0.000(2) 0.001(2) C52 0.025(3) 0.020(3) 0.027(3) -0.004(2) 0.000(2) -0.001(2) C53 0.026(3) 0.039(4) 0.032(3) 0.003(3) -0.006(3) -0.007(3) C54 0.031(3) 0.030(3) 0.039(4) 0.001(3) -0.003(3) 0.007(3) C55 0.029(3) 0.028(3) 0.058(4) 0.003(3) -0.005(3) -0.003(3) C56 0.028(3) 0.022(3) 0.046(4) -0.007(3) -0.004(3) -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 O C1 1.228(7) . ? C1 B4 1.671(8) . ? C1 B5 1.679(8) . ? C1 B3 1.838(8) . ? C1 B6 1.838(8) . ? C2 C21 1.496(8) . ? C2 B11 1.678(9) . ? C2 B7 1.684(9) . ? C2 B3 1.685(8) . ? C2 B6 1.710(8) . ? B3 B4 1.775(9) . ? B3 B8 1.777(10) . ? B3 B7 1.790(9) . ? B4 B8 1.769(10) . ? B4 B9 1.785(10) . ? B4 B5 1.815(10) . ? B5 B10 1.770(10) . ? B5 B9 1.784(10) . ? B5 B6 1.787(9) . ? B6 B10 1.783(9) . ? B6 B11 1.796(10) . ? B7 B11 1.764(11) . ? B7 B8 1.770(10) . ? B7 B12 1.771(11) . ? B8 B9 1.784(11) . ? B8 B12 1.787(11) . ? B9 B12 1.771(10) . ? B9 B10 1.779(11) . ? B10 B11 1.775(10) . ? B10 B12 1.794(12) . ? B11 B12 1.779(10) . ? C21 C22 1.393(8) . ? C21 C26 1.394(8) . ? C22 C23 1.379(9) . ? C23 C24 1.382(9) . ? C24 C25 1.380(9) . ? C25 C26 1.381(9) . ? P C30 1.781(6) . ? P C41 1.787(6) . ? P C31 1.794(5) . ? P C51 1.798(5) . ? C31 C32 1.390(8) . ? C31 C36 1.390(8) . ? C32 C33 1.384(9) . ? C33 C34 1.378(9) . ? C34 C35 1.380(9) . ? C35 C36 1.393(8) . ? C41 C42 1.393(8) . ? C41 C46 1.401(8) . ? C42 C43 1.392(8) . ? C43 C44 1.363(9) . ? C44 C45 1.379(9) . ? C45 C46 1.366(8) . ? C51 C56 1.387(8) . ? C51 C52 1.394(8) . ? C52 C53 1.380(8) . ? C53 C54 1.385(9) . ? C54 C55 1.379(9) . ? C55 C56 1.390(9) . ? 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 O C1 B4 129.9(5) . . ? O C1 B5 130.7(5) . . ? B4 C1 B5 65.6(4) . . ? O C1 B3 119.6(5) . . ? B4 C1 B3 60.6(4) . . ? B5 C1 B3 108.5(4) . . ? O C1 B6 120.3(5) . . ? B4 C1 B6 108.7(4) . . ? B5 C1 B6 60.9(4) . . ? B3 C1 B6 96.4(4) . . ? C21 C2 B11 121.8(5) . . ? C21 C2 B7 124.0(5) . . ? B11 C2 B7 63.3(4) . . ? C21 C2 B3 119.4(5) . . ? B11 C2 B3 114.1(5) . . ? B7 C2 B3 64.2(4) . . ? C21 C2 B6 116.0(5) . . ? B11 C2 B6 64.0(4) . . ? B7 C2 B6 114.2(5) . . ? B3 C2 B6 107.6(4) . . ? C2 B3 B4 111.1(5) . . ? C2 B3 B8 105.9(5) . . ? B4 B3 B8 59.7(4) . . ? C2 B3 B7 57.9(4) . . ? B4 B3 B7 109.0(5) . . ? B8 B3 B7 59.5(4) . . ? C2 B3 C1 71.4(4) . . ? B4 B3 C1 55.1(3) . . ? B8 B3 C1 106.2(5) . . ? B7 B3 C1 115.8(5) . . ? C1 B4 B8 114.4(5) . . ? C1 B4 B3 64.4(4) . . ? B8 B4 B3 60.2(4) . . ? C1 B4 B9 108.8(5) . . ? B8 B4 B9 60.3(4) . . ? B3 B4 B9 106.5(5) . . ? C1 B4 B5 57.4(4) . . ? B8 B4 B5 107.8(5) . . ? B3 B4 B5 105.4(5) . . ? B9 B4 B5 59.4(4) . . ? C1 B5 B10 113.6(5) . . ? C1 B5 B9 108.5(5) . . ? B10 B5 B9 60.1(4) . . ? C1 B5 B6 64.0(4) . . ? B10 B5 B6 60.2(4) . . ? B9 B5 B6 106.5(5) . . ? C1 B5 B4 57.0(3) . . ? B10 B5 B4 107.2(5) . . ? B9 B5 B4 59.5(4) . . ? B6 B5 B4 104.8(4) . . ? C2 B6 B10 105.0(5) . . ? C2 B6 B5 110.4(5) . . ? B10 B6 B5 59.4(4) . . ? C2 B6 B11 57.1(4) . . ? B10 B6 B11 59.5(4) . . ? B5 B6 B11 108.5(5) . . ? C2 B6 C1 70.9(4) . . ? B10 B6 C1 105.7(5) . . ? B5 B6 C1 55.1(3) . . ? B11 B6 C1 114.7(5) . . ? C2 B7 B11 58.2(4) . . ? C2 B7 B8 106.3(5) . . ? B11 B7 B8 108.3(5) . . ? C2 B7 B12 106.1(5) . . ? B11 B7 B12 60.4(4) . . ? B8 B7 B12 60.6(4) . . ? C2 B7 B3 57.9(3) . . ? B11 B7 B3 105.2(5) . . ? B8 B7 B3 59.9(4) . . ? B12 B7 B3 107.1(5) . . ? B4 B8 B7 110.2(5) . . ? B4 B8 B3 60.1(4) . . ? B7 B8 B3 60.6(4) . . ? B4 B8 B9 60.3(4) . . ? B7 B8 B9 107.7(5) . . ? B3 B8 B9 106.5(5) . . ? B4 B8 B12 108.8(5) . . ? B7 B8 B12 59.7(4) . . ? B3 B8 B12 106.9(5) . . ? B9 B8 B12 59.5(4) . . ? B12 B9 B10 60.7(4) . . ? B12 B9 B5 109.4(5) . . ? B10 B9 B5 59.6(4) . . ? B12 B9 B8 60.4(4) . . ? B10 B9 B8 107.8(5) . . ? B5 B9 B8 108.5(5) . . ? B12 B9 B4 108.8(5) . . ? B10 B9 B4 108.1(5) . . ? B5 B9 B4 61.1(4) . . ? B8 B9 B4 59.4(4) . . ? B5 B10 B11 110.3(5) . . ? B5 B10 B9 60.4(4) . . ? B11 B10 B9 107.7(6) . . ? B5 B10 B6 60.4(4) . . ? B11 B10 B6 60.6(4) . . ? B9 B10 B6 106.9(5) . . ? B5 B10 B12 109.0(5) . . ? B11 B10 B12 59.8(4) . . ? B9 B10 B12 59.4(4) . . ? B6 B10 B12 107.4(5) . . ? C2 B11 B7 58.5(4) . . ? C2 B11 B10 106.7(5) . . ? B7 B11 B10 108.4(5) . . ? C2 B11 B12 106.1(5) . . ? B7 B11 B12 60.0(4) . . ? B10 B11 B12 60.6(4) . . ? C2 B11 B6 58.9(4) . . ? B7 B11 B6 106.5(5) . . ? B10 B11 B6 59.9(4) . . ? B12 B11 B6 107.5(5) . . ? B7 B12 B9 108.3(5) . . ? B7 B12 B11 59.6(4) . . ? B9 B12 B11 107.8(5) . . ? B7 B12 B8 59.7(4) . . ? B9 B12 B8 60.2(4) . . ? B11 B12 B8 106.9(5) . . ? B7 B12 B10 107.2(5) . . ? B9 B12 B10 59.9(4) . . ? B11 B12 B10 59.6(4) . . ? B8 B12 B10 107.1(5) . . ? C22 C21 C26 117.9(6) . . ? C22 C21 C2 120.7(5) . . ? C26 C21 C2 121.3(5) . . ? C23 C22 C21 120.3(6) . . ? C22 C23 C24 121.5(6) . . ? C25 C24 C23 118.5(6) . . ? C24 C25 C26 120.6(6) . . ? C25 C26 C21 121.2(6) . . ? C30 P C41 108.6(3) . . ? C30 P C31 110.4(3) . . ? C41 P C31 111.7(2) . . ? C30 P C51 107.7(3) . . ? C41 P C51 111.0(3) . . ? C31 P C51 107.4(2) . . ? C32 C31 C36 120.0(5) . . ? C32 C31 P 121.3(4) . . ? C36 C31 P 118.6(4) . . ? C33 C32 C31 119.9(6) . . ? C34 C33 C32 119.8(6) . . ? C33 C34 C35 121.1(6) . . ? C34 C35 C36 119.3(6) . . ? C31 C36 C35 119.9(6) . . ? C42 C41 C46 120.0(5) . . ? C42 C41 P 121.5(4) . . ? C46 C41 P 118.5(4) . . ? C43 C42 C41 119.2(5) . . ? C44 C43 C42 120.5(6) . . ? C43 C44 C45 119.8(6) . . ? C46 C45 C44 121.6(6) . . ? C45 C46 C41 118.8(5) . . ? C56 C51 C52 119.7(5) . . ? C56 C51 P 122.7(4) . . ? C52 C51 P 117.6(4) . . ? C53 C52 C51 119.9(5) . . ? C52 C53 C54 120.5(6) . . ? C55 C54 C53 119.7(6) . . ? C54 C55 C56 120.4(6) . . ? C51 C56 C55 119.8(6) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C30 H301 O 0.98 2.26 3.154(7) 151 . _diffrn_measured_fraction_theta_max 0.896 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.896 _refine_diff_density_max 0.375 _refine_diff_density_min -0.362 _refine_diff_density_rms 0.082 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 237440' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H17 B10 N' _chemical_formula_sum 'C8 H17 B10 N' _chemical_formula_weight 235.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.6738(7) _cell_length_b 22.3100(16) _cell_length_c 23.3165(16) _cell_angle_alpha 90.00 _cell_angle_beta 102.677(2) _cell_angle_gamma 90.00 _cell_volume 5417.1(6) _cell_formula_units_Z 16 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 14291 _cell_measurement_theta_min 2.03 _cell_measurement_theta_max 28.26 _exptl_crystal_description tablet _exptl_crystal_colour colourless _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.154 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 0.056 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method 'thin-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33320 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_sigmaI/netI 0.0594 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 28.55 _reflns_number_total 12397 _reflns_number_gt 7978 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1385P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12397 _refine_ls_number_parameters 703 _refine_ls_number_restraints 33 _refine_ls_R_factor_all 0.1071 _refine_ls_R_factor_gt 0.0691 _refine_ls_wR_factor_ref 0.2193 _refine_ls_wR_factor_gt 0.1952 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1A C 0.95167(19) 0.66335(10) 0.24440(9) 0.0279(5) Uani 1 1 d D . . C2A C 0.97396(18) 0.61673(9) 0.18519(9) 0.0234(4) Uani 1 1 d . . . B3A B 0.8848(2) 0.68198(10) 0.17269(11) 0.0275(5) Uani 1 1 d . . . H3A H 0.9172 0.7221 0.1510 0.033 Uiso 1 1 calc R . . B4A B 0.7984(2) 0.68902(11) 0.22906(11) 0.0311(6) Uani 1 1 d . . . H4A H 0.7697 0.7338 0.2438 0.037 Uiso 1 1 calc R . . B5A B 0.8480(2) 0.62864(12) 0.27907(11) 0.0321(6) Uani 1 1 d . . . H5A H 0.8524 0.6329 0.3273 0.039 Uiso 1 1 calc R . . B6A B 0.9628(2) 0.58670(11) 0.25168(11) 0.0298(5) Uani 1 1 d . . . H6A H 1.0464 0.5646 0.2816 0.036 Uiso 1 1 calc R . . B7A B 0.8349(2) 0.61356(11) 0.13343(10) 0.0261(5) Uani 1 1 d . . . H7A H 0.8305 0.6087 0.0852 0.031 Uiso 1 1 calc R . . B8A B 0.7220(2) 0.65833(11) 0.16013(11) 0.0291(5) Uani 1 1 d . . . H8A H 0.6433 0.6829 0.1294 0.035 Uiso 1 1 calc R . . B9A B 0.7004(2) 0.62477(12) 0.22640(11) 0.0305(5) Uani 1 1 d . . . H9A H 0.6057 0.6267 0.2396 0.037 Uiso 1 1 calc R . . B10A B 0.8033(2) 0.56096(12) 0.24167(11) 0.0321(6) Uani 1 1 d . . . H10A H 0.7782 0.5206 0.2654 0.039 Uiso 1 1 calc R . . B11A B 0.8844(2) 0.55371(11) 0.18362(11) 0.0289(5) Uani 1 1 d . . . H11A H 0.9130 0.5089 0.1690 0.035 Uiso 1 1 calc R . . B12A B 0.7220(2) 0.57861(11) 0.16798(11) 0.0280(5) Uani 1 1 d . . . H12A H 0.6420 0.5502 0.1428 0.034 Uiso 1 1 calc R . . C13A C 1.10210(19) 0.61802(9) 0.16864(9) 0.0281(5) Uani 1 1 d . . . C14A C 1.1136(2) 0.64827(10) 0.11768(10) 0.0348(5) Uani 1 1 d . . . H14A H 1.0413 0.6684 0.0947 0.042 Uiso 1 1 calc R . . C15A C 1.2296(2) 0.64918(12) 0.10037(12) 0.0451(7) Uani 1 1 d . . . H15A H 1.2364 0.6694 0.0653 0.054 Uiso 1 1 calc R . . C16A C 1.3360(2) 0.62048(13) 0.13427(13) 0.0501(7) Uani 1 1 d . . . H16A H 1.4161 0.6216 0.1229 0.060 Uiso 1 1 calc R . . C17A C 1.3247(2) 0.59046(12) 0.18423(13) 0.0477(7) Uani 1 1 d . . . H17A H 1.3974 0.5706 0.2072 0.057 Uiso 1 1 calc R . . C18A C 1.2081(2) 0.58865(10) 0.20190(11) 0.0364(5) Uani 1 1 d . . . H18A H 1.2013 0.5675 0.2364 0.044 Uiso 1 1 calc R . . N19A N 1.05566(18) 0.69657(9) 0.27479(9) 0.0389(5) Uani 1 1 d D . . H1A H 1.0718(19) 0.7324(8) 0.2537(9) 0.047 Uiso 1 1 d D . . H2A H 1.1125(17) 0.6784(9) 0.3081(8) 0.047 Uiso 1 1 d D . . C1B C 0.4212(2) 0.79785(10) 0.22613(10) 0.0345(5) Uani 1 1 d . . . C2B C 0.45647(18) 0.85833(9) 0.18352(8) 0.0232(4) Uani 1 1 d . . . B3B B 0.4519(3) 0.86732(14) 0.25587(11) 0.0406(7) Uani 1 1 d . . . H3B H 0.5401 0.8774 0.2905 0.049 Uiso 1 1 calc R . . B4B B 0.3264(2) 0.82181(13) 0.27063(12) 0.0373(6) Uani 1 1 d . . . H4B H 0.3289 0.8026 0.3152 0.045 Uiso 1 1 calc R . . B5B B 0.2624(3) 0.78168(12) 0.20609(12) 0.0361(6) Uani 1 1 d . . . H5B H 0.2219 0.7355 0.2074 0.043 Uiso 1 1 calc R . . B6B B 0.3500(2) 0.80306(12) 0.15364(12) 0.0328(6) Uani 1 1 d . . . H6B H 0.3716 0.7706 0.1205 0.039 Uiso 1 1 calc R . . B7B B 0.3832(3) 0.92051(12) 0.20052(14) 0.0414(7) Uani 1 1 d . . . H7B H 0.4226 0.9668 0.1989 0.050 Uiso 1 1 calc R . . B8B B 0.3004(3) 0.89888(13) 0.25566(14) 0.0448(7) Uani 1 1 d . . . H8B H 0.2862 0.9310 0.2906 0.054 Uiso 1 1 calc R . . B9B B 0.1820(2) 0.84580(12) 0.22384(11) 0.0309(5) Uani 1 1 d . . . H9B H 0.0877 0.8432 0.2373 0.037 Uiso 1 1 calc R . . B10B B 0.1965(2) 0.83184(14) 0.15070(12) 0.0386(6) Uani 1 1 d . . . H10B H 0.1121 0.8188 0.1152 0.046 Uiso 1 1 calc R . . B11B B 0.3200(2) 0.87900(12) 0.13634(11) 0.0333(6) Uani 1 1 d . . . H11B H 0.3177 0.8973 0.0914 0.040 Uiso 1 1 calc R . . B12B B 0.2157(3) 0.90533(13) 0.18009(14) 0.0426(7) Uani 1 1 d . . . H12B H 0.1435 0.9415 0.1644 0.051 Uiso 1 1 calc R . . C13B C 0.58421(18) 0.85892(9) 0.16685(9) 0.0252(4) Uani 1 1 d . . . C14B C 0.6897(2) 0.88694(10) 0.20212(10) 0.0317(5) Uani 1 1 d . . . H14B H 0.6821 0.9045 0.2383 0.038 Uiso 1 1 calc R . . C15B C 0.8065(2) 0.88948(11) 0.18496(11) 0.0393(6) Uani 1 1 d . . . H15B H 0.8777 0.9091 0.2093 0.047 Uiso 1 1 calc R . . C16B C 0.8195(2) 0.86374(11) 0.13297(11) 0.0400(6) Uani 1 1 d . . . H16B H 0.8996 0.8654 0.1215 0.048 Uiso 1 1 calc R . . C17B C 0.7156(2) 0.83556(11) 0.09751(11) 0.0405(6) Uani 1 1 d . . . H17B H 0.7243 0.8178 0.0615 0.049 Uiso 1 1 calc R . . C18B C 0.5982(2) 0.83295(10) 0.11419(10) 0.0330(5) Uani 1 1 d . . . H18B H 0.5273 0.8134 0.0896 0.040 Uiso 1 1 calc R . . N19B N 0.5171(2) 0.75405(11) 0.24099(11) 0.0641(8) Uani 1 1 d . . . C1C C 0.94547(18) 0.16457(9) 0.11200(9) 0.0245(4) Uani 1 1 d D . . C2C C 0.89091(18) 0.10452(8) 0.06520(8) 0.0219(4) Uani 1 1 d . . . B3C B 1.0004(2) 0.09389(10) 0.13209(10) 0.0234(5) Uani 1 1 d . . . H3C H 0.9759 0.0694 0.1701 0.028 Uiso 1 1 calc R . . B4C B 1.1051(2) 0.15641(11) 0.14285(11) 0.0281(5) Uani 1 1 d . . . H4C H 1.1522 0.1730 0.1878 0.034 Uiso 1 1 calc R . . B5C B 1.0499(2) 0.20598(11) 0.08321(11) 0.0292(5) Uani 1 1 d . . . H5C H 1.0600 0.2557 0.0887 0.035 Uiso 1 1 calc R . . B6C B 0.9134(2) 0.17304(10) 0.03640(10) 0.0249(5) Uani 1 1 d . . . H6C H 0.8318 0.2007 0.0116 0.030 Uiso 1 1 calc R . . B7C B 1.0152(2) 0.05637(11) 0.06625(10) 0.0273(5) Uani 1 1 d . . . H7C H 1.0027 0.0067 0.0610 0.033 Uiso 1 1 calc R . . B8C B 1.1524(2) 0.08840(12) 0.11406(11) 0.0296(5) Uani 1 1 d . . . H8C H 1.2310 0.0598 0.1401 0.035 Uiso 1 1 calc R . . B9C B 1.1840(2) 0.15856(12) 0.08315(11) 0.0327(6) Uani 1 1 d . . . H9C H 1.2838 0.1765 0.0884 0.039 Uiso 1 1 calc R . . B10C B 1.0644(2) 0.16981(12) 0.01711(11) 0.0316(6) Uani 1 1 d . . . H10C H 1.0848 0.1956 -0.0210 0.038 Uiso 1 1 calc R . . B11C B 0.9618(2) 0.10592(11) 0.00668(10) 0.0271(5) Uani 1 1 d . . . H11C H 0.9147 0.0893 -0.0382 0.033 Uiso 1 1 calc R . . B12C B 1.1289(2) 0.09668(12) 0.03630(11) 0.0318(6) Uani 1 1 d . . . H12C H 1.1930 0.0739 0.0109 0.038 Uiso 1 1 calc R . . C13C C 0.75688(18) 0.08248(9) 0.06371(8) 0.0230(4) Uani 1 1 d . . . C14C C 0.7376(2) 0.02735(10) 0.08842(11) 0.0366(5) Uani 1 1 d . . . H14C H 0.8094 0.0031 0.1052 0.044 Uiso 1 1 calc R . . C15C C 0.6145(2) 0.00758(11) 0.08867(11) 0.0435(6) Uani 1 1 d . . . H15C H 0.6029 -0.0302 0.1056 0.052 Uiso 1 1 calc R . . C16C C 0.5094(2) 0.04187(11) 0.06482(10) 0.0377(6) Uani 1 1 d . . . H16C H 0.4255 0.0281 0.0655 0.045 Uiso 1 1 calc R . . C17C C 0.5263(2) 0.09608(11) 0.03994(11) 0.0391(6) Uani 1 1 d . . . H17C H 0.4537 0.1200 0.0233 0.047 Uiso 1 1 calc R . . C18C C 0.6490(2) 0.11624(10) 0.03890(10) 0.0328(5) Uani 1 1 d . . . H18C H 0.6593 0.1536 0.0210 0.039 Uiso 1 1 calc R . . N19C N 0.86211(19) 0.19180(9) 0.14230(9) 0.0378(5) Uani 1 1 d D . . H1C H 0.8187(18) 0.1606(9) 0.1647(9) 0.045 Uiso 1 1 d D . . H2C H 0.7851(16) 0.2123(9) 0.1153(8) 0.045 Uiso 1 1 d D . . C1D C 0.5156(2) 0.39399(9) 0.12842(9) 0.0262(4) Uani 1 1 d D . . C2D C 0.39810(18) 0.38248(8) 0.06265(8) 0.0221(4) Uani 1 1 d . . . B3D B 0.4461(2) 0.32505(10) 0.11259(11) 0.0270(5) Uani 1 1 d . . . H3D H 0.3804 0.3052 0.1390 0.032 Uiso 1 1 calc R . . B4D B 0.6133(2) 0.33244(11) 0.14214(12) 0.0313(6) Uani 1 1 d . . . H4D H 0.6598 0.3163 0.1873 0.038 Uiso 1 1 calc R . . B5D B 0.6629(2) 0.39933(11) 0.11203(11) 0.0297(5) Uani 1 1 d . . . H5D H 0.7423 0.4280 0.1373 0.036 Uiso 1 1 calc R . . B6D B 0.5243(2) 0.43047(10) 0.06396(10) 0.0248(5) Uani 1 1 d . . . H6D H 0.5105 0.4801 0.0583 0.030 Uiso 1 1 calc R . . B7D B 0.4207(2) 0.31391(10) 0.03526(11) 0.0282(5) Uani 1 1 d . . . H7D H 0.3404 0.2855 0.0104 0.034 Uiso 1 1 calc R . . B8D B 0.5571(2) 0.28202(11) 0.08398(12) 0.0341(6) Uani 1 1 d . . . H8D H 0.5670 0.2324 0.0910 0.041 Uiso 1 1 calc R . . B9D B 0.6911(2) 0.32869(12) 0.08251(12) 0.0348(6) Uani 1 1 d . . . H9D H 0.7905 0.3101 0.0879 0.042 Uiso 1 1 calc R . . B10D B 0.6376(2) 0.38987(11) 0.03468(11) 0.0306(5) Uani 1 1 d . . . H10D H 0.7017 0.4122 0.0090 0.037 Uiso 1 1 calc R . . B11D B 0.4706(2) 0.38048(11) 0.00482(10) 0.0279(5) Uani 1 1 d . . . H11D H 0.4243 0.3966 -0.0403 0.034 Uiso 1 1 calc R . . B12D B 0.5725(3) 0.31659(11) 0.01690(12) 0.0345(6) Uani 1 1 d . . . H12D H 0.5934 0.2899 -0.0206 0.041 Uiso 1 1 calc R . . C13D C 0.26693(19) 0.40689(9) 0.06167(9) 0.0250(4) Uani 1 1 d . . . C14D C 0.1646(2) 0.36759(11) 0.05814(12) 0.0410(6) Uani 1 1 d . . . H14D H 0.1783 0.3257 0.0551 0.049 Uiso 1 1 calc R . . C15D C 0.0430(2) 0.38850(12) 0.05894(13) 0.0482(7) Uani 1 1 d . . . H15D H -0.0263 0.3611 0.0558 0.058 Uiso 1 1 calc R . . C16D C 0.0221(2) 0.44877(12) 0.06425(11) 0.0439(6) Uani 1 1 d . . . H16D H -0.0609 0.4631 0.0658 0.053 Uiso 1 1 calc R . . C17D C 0.1224(2) 0.48821(11) 0.06723(12) 0.0461(6) Uani 1 1 d . . . H17D H 0.1083 0.5300 0.0706 0.055 Uiso 1 1 calc R . . C18D C 0.2438(2) 0.46758(10) 0.06544(11) 0.0384(6) Uani 1 1 d . . . H18D H 0.3118 0.4954 0.0668 0.046 Uiso 1 1 calc R . . N19D N 0.4852(2) 0.42821(10) 0.17403(9) 0.0419(5) Uani 1 1 d D . . H1D H 0.4106(19) 0.4115(9) 0.1900(9) 0.050 Uiso 1 1 d D . . H2D H 0.489(2) 0.4732(6) 0.1685(10) 0.050 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1A 0.0243(10) 0.0350(12) 0.0268(11) -0.0105(9) 0.0112(8) -0.0059(9) C2A 0.0237(10) 0.0267(10) 0.0220(10) -0.0038(8) 0.0098(8) -0.0023(8) B3A 0.0299(12) 0.0240(12) 0.0312(13) -0.0015(10) 0.0125(10) 0.0002(9) B4A 0.0221(11) 0.0363(14) 0.0388(14) -0.0108(11) 0.0153(10) -0.0026(10) B5A 0.0266(12) 0.0473(15) 0.0256(12) -0.0046(11) 0.0124(10) -0.0073(11) B6A 0.0284(12) 0.0355(14) 0.0263(12) 0.0039(10) 0.0080(10) -0.0009(10) B7A 0.0268(12) 0.0298(12) 0.0228(11) -0.0042(9) 0.0075(9) -0.0053(9) B8A 0.0251(12) 0.0316(13) 0.0317(13) -0.0016(10) 0.0088(10) 0.0003(10) B9A 0.0240(12) 0.0403(14) 0.0296(13) -0.0051(11) 0.0111(10) -0.0070(10) B10A 0.0306(13) 0.0369(14) 0.0315(13) 0.0034(11) 0.0125(11) -0.0061(11) B11A 0.0288(12) 0.0268(12) 0.0330(13) -0.0018(10) 0.0106(10) -0.0063(10) B12A 0.0258(12) 0.0301(13) 0.0289(12) -0.0039(10) 0.0079(10) -0.0077(10) C13A 0.0255(10) 0.0305(11) 0.0314(11) -0.0123(9) 0.0130(9) -0.0075(9) C14A 0.0357(12) 0.0381(13) 0.0369(13) -0.0103(10) 0.0215(10) -0.0090(10) C15A 0.0452(15) 0.0513(15) 0.0487(15) -0.0193(12) 0.0318(12) -0.0196(12) C16A 0.0366(14) 0.0623(17) 0.0610(18) -0.0344(15) 0.0317(13) -0.0204(12) C17A 0.0252(12) 0.0577(17) 0.0608(18) -0.0257(14) 0.0106(11) -0.0041(11) C18A 0.0287(11) 0.0421(13) 0.0400(13) -0.0123(11) 0.0112(10) -0.0020(10) N19A 0.0312(10) 0.0474(12) 0.0397(12) -0.0137(10) 0.0111(9) -0.0144(9) C1B 0.0329(12) 0.0426(13) 0.0334(12) 0.0171(10) 0.0191(10) 0.0135(10) C2B 0.0242(10) 0.0245(10) 0.0213(10) 0.0020(8) 0.0063(8) 0.0015(8) B3B 0.0286(13) 0.071(2) 0.0229(13) -0.0096(13) 0.0084(10) -0.0033(13) B4B 0.0303(13) 0.0555(17) 0.0296(14) 0.0082(12) 0.0142(11) 0.0083(12) B5B 0.0403(15) 0.0338(14) 0.0423(15) 0.0015(12) 0.0265(12) -0.0021(11) B6B 0.0361(13) 0.0325(13) 0.0352(14) -0.0054(11) 0.0196(11) -0.0097(11) B7B 0.0391(15) 0.0277(13) 0.0628(19) -0.0081(13) 0.0231(14) -0.0002(11) B8B 0.0395(16) 0.0458(17) 0.0547(19) -0.0203(14) 0.0228(14) -0.0040(13) B9B 0.0234(12) 0.0415(14) 0.0293(13) 0.0061(11) 0.0092(10) 0.0053(10) B10B 0.0293(13) 0.0590(18) 0.0294(14) 0.0006(12) 0.0106(11) -0.0089(12) B11B 0.0244(12) 0.0472(16) 0.0278(13) 0.0142(11) 0.0048(10) 0.0013(11) B12B 0.0326(14) 0.0407(16) 0.0584(19) 0.0191(14) 0.0181(13) 0.0129(12) C13B 0.0244(10) 0.0271(11) 0.0256(10) 0.0051(8) 0.0088(8) 0.0022(8) C14B 0.0291(11) 0.0380(12) 0.0273(11) 0.0023(9) 0.0046(9) 0.0004(9) C15B 0.0239(11) 0.0500(15) 0.0415(14) 0.0069(11) 0.0015(10) -0.0031(10) C16B 0.0261(12) 0.0482(15) 0.0488(15) 0.0099(12) 0.0148(11) 0.0041(10) C17B 0.0350(13) 0.0529(15) 0.0395(13) -0.0017(11) 0.0210(11) 0.0022(11) C18B 0.0283(11) 0.0429(13) 0.0306(12) -0.0045(10) 0.0124(9) -0.0054(10) N19B 0.0525(14) 0.0713(16) 0.0820(18) 0.0490(14) 0.0443(13) 0.0373(12) C1C 0.0271(10) 0.0230(10) 0.0247(10) -0.0039(8) 0.0087(8) -0.0021(8) C2C 0.0238(10) 0.0206(10) 0.0208(10) -0.0036(8) 0.0037(8) 0.0015(8) B3C 0.0264(11) 0.0225(11) 0.0204(11) -0.0016(9) 0.0028(9) 0.0017(9) B4C 0.0235(11) 0.0335(13) 0.0272(12) -0.0059(10) 0.0053(10) -0.0051(10) B5C 0.0298(12) 0.0279(12) 0.0329(13) -0.0013(10) 0.0136(10) -0.0062(10) B6C 0.0273(12) 0.0267(12) 0.0228(12) 0.0021(9) 0.0098(9) 0.0002(9) B7C 0.0254(12) 0.0293(12) 0.0254(12) -0.0055(10) 0.0017(9) 0.0080(10) B8C 0.0232(12) 0.0366(14) 0.0265(12) -0.0057(10) 0.0000(10) 0.0045(10) B9C 0.0263(12) 0.0438(15) 0.0295(13) -0.0059(11) 0.0094(10) -0.0023(11) B10C 0.0294(13) 0.0410(14) 0.0275(13) 0.0010(11) 0.0126(10) -0.0007(11) B11C 0.0282(12) 0.0344(13) 0.0200(11) -0.0020(10) 0.0078(9) 0.0062(10) B12C 0.0256(12) 0.0434(15) 0.0275(13) -0.0074(11) 0.0081(10) 0.0081(11) C13C 0.0243(10) 0.0244(10) 0.0201(10) -0.0030(8) 0.0046(8) -0.0011(8) C14C 0.0312(12) 0.0306(12) 0.0452(14) 0.0084(10) 0.0022(10) -0.0025(9) C15C 0.0414(14) 0.0378(14) 0.0497(15) 0.0080(12) 0.0066(12) -0.0136(11) C16C 0.0289(11) 0.0492(15) 0.0353(13) -0.0012(11) 0.0077(10) -0.0108(10) C17C 0.0248(11) 0.0480(15) 0.0442(14) 0.0074(11) 0.0070(10) 0.0031(10) C18C 0.0279(11) 0.0326(12) 0.0388(13) 0.0067(10) 0.0090(10) 0.0029(9) N19C 0.0413(11) 0.0382(11) 0.0385(11) -0.0042(9) 0.0191(9) 0.0006(9) C1D 0.0309(11) 0.0272(11) 0.0204(10) 0.0011(8) 0.0054(8) -0.0009(8) C2D 0.0272(10) 0.0208(10) 0.0189(9) 0.0015(8) 0.0067(8) -0.0036(8) B3D 0.0298(12) 0.0225(11) 0.0306(13) 0.0058(10) 0.0107(10) -0.0013(9) B4D 0.0324(13) 0.0278(13) 0.0344(14) 0.0093(11) 0.0086(11) 0.0046(10) B5D 0.0266(12) 0.0311(13) 0.0309(13) 0.0038(10) 0.0053(10) -0.0018(10) B6D 0.0277(12) 0.0249(12) 0.0221(11) 0.0025(9) 0.0063(9) -0.0065(9) B7D 0.0299(12) 0.0252(12) 0.0325(13) -0.0064(10) 0.0135(10) -0.0060(10) B8D 0.0317(13) 0.0241(12) 0.0504(16) 0.0011(11) 0.0171(12) 0.0000(10) B9D 0.0294(13) 0.0311(13) 0.0466(16) 0.0020(12) 0.0144(12) 0.0004(10) B10D 0.0297(13) 0.0318(13) 0.0334(13) 0.0015(11) 0.0135(11) -0.0062(10) B11D 0.0306(13) 0.0329(13) 0.0230(12) -0.0025(10) 0.0119(10) -0.0083(10) B12D 0.0376(14) 0.0324(14) 0.0393(15) -0.0074(11) 0.0210(12) -0.0062(11) C13D 0.0254(10) 0.0273(11) 0.0224(10) 0.0009(8) 0.0058(8) 0.0008(8) C14D 0.0329(13) 0.0300(12) 0.0630(17) 0.0059(12) 0.0168(12) -0.0022(10) C15D 0.0307(13) 0.0469(15) 0.0715(19) 0.0078(14) 0.0207(13) 0.0003(11) C16D 0.0345(13) 0.0531(16) 0.0447(15) 0.0006(12) 0.0105(11) 0.0114(11) C17D 0.0388(14) 0.0391(14) 0.0572(17) -0.0113(12) 0.0033(12) 0.0101(11) C18D 0.0347(12) 0.0309(12) 0.0474(14) -0.0064(11) 0.0041(11) -0.0001(10) N19D 0.0533(13) 0.0432(12) 0.0311(11) -0.0021(9) 0.0133(9) -0.0015(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1A C2A 1.785(3) . ? C1A B3A 1.719(3) . ? C1A B4A 1.695(3) . ? C1A B5A 1.694(3) . ? C1A B6A 1.720(3) . ? C1A N19A 1.392(3) . ? C2A B3A 1.729(3) . ? C2A B6A 1.717(3) . ? C2A B7A 1.697(3) . ? C2A B11A 1.696(3) . ? C2A C13A 1.501(3) . ? B3A B4A 1.770(3) . ? B3A B7A 1.800(3) . ? B3A B8A 1.778(3) . ? B4A B5A 1.784(4) . ? B4A B8A 1.773(4) . ? B4A B9A 1.768(3) . ? B5A B6A 1.768(3) . ? B5A B9A 1.775(3) . ? B5A B10A 1.757(4) . ? B6A B10A 1.763(3) . ? B6A B11A 1.782(3) . ? B7A B8A 1.779(3) . ? B7A B11A 1.778(3) . ? B7A B12A 1.770(3) . ? B8A B9A 1.777(3) . ? B8A B12A 1.788(3) . ? B9A B10A 1.786(4) . ? B9A B12A 1.763(3) . ? B10A B11A 1.767(3) . ? B10A B12A 1.790(3) . ? B11A B12A 1.780(3) . ? C13A C14A 1.395(3) . ? C13A C18A 1.388(3) . ? C14A C15A 1.384(3) . ? C15A C16A 1.390(4) . ? C16A C17A 1.372(4) . ? C17A C18A 1.395(3) . ? N19A H1A 0.973(14) . ? N19A H2A 0.964(14) . ? C1B C2B 1.765(3) . ? C1B B3B 1.700(4) . ? C1B B4B 1.687(3) . ? C1B B5B 1.695(3) . ? C1B B6B 1.698(3) . ? C1B N19B 1.403(3) . ? C2B B3B 1.710(3) . ? C2B B6B 1.717(3) . ? C2B B7B 1.682(3) . ? C2B B11B 1.686(3) . ? C2B C13B 1.498(3) . ? B3B B4B 1.774(4) . ? B3B B7B 1.788(4) . ? B3B B8B 1.763(4) . ? B4B B5B 1.756(4) . ? B4B B8B 1.764(4) . ? B4B B9B 1.764(3) . ? B5B B6B 1.761(3) . ? B5B B9B 1.763(4) . ? B5B B10B 1.737(4) . ? B6B B10B 1.747(4) . ? B6B B11B 1.755(4) . ? B7B B8B 1.779(4) . ? B7B B11B 1.763(4) . ? B7B B12B 1.779(4) . ? B8B B9B 1.771(4) . ? B8B B12B 1.801(4) . ? B9B B10B 1.773(4) . ? B9B B12B 1.759(4) . ? B10B B11B 1.775(4) . ? B10B B12B 1.771(4) . ? B11B B12B 1.767(4) . ? C13B C14B 1.389(3) . ? C13B C18B 1.395(3) . ? C14B C15B 1.391(3) . ? C15B C16B 1.376(3) . ? C16B C17B 1.380(3) . ? C17B C18B 1.392(3) . ? C1C C2C 1.745(3) . ? C1C B3C 1.711(3) . ? C1C B4C 1.708(3) . ? C1C B5C 1.696(3) . ? C1C B6C 1.731(3) . ? C1C N19C 1.391(3) . ? C2C B3C 1.748(3) . ? C2C B6C 1.708(3) . ? C2C B7C 1.703(3) . ? C2C B11C 1.700(3) . ? C2C C13C 1.506(3) . ? B3C B4C 1.771(3) . ? B3C B7C 1.786(3) . ? B3C B8C 1.768(3) . ? B4C B5C 1.773(3) . ? B4C B8C 1.777(3) . ? B4C B9C 1.778(3) . ? B5C B6C 1.776(3) . ? B5C B9C 1.780(3) . ? B5C B10C 1.776(3) . ? B6C B10C 1.766(3) . ? B6C B11C 1.774(3) . ? B7C B8C 1.784(3) . ? B7C B11C 1.769(3) . ? B7C B12C 1.773(4) . ? B8C B9C 1.786(4) . ? B8C B12C 1.785(3) . ? B9C B10C 1.789(4) . ? B9C B12C 1.778(4) . ? B10C B11C 1.781(4) . ? B10C B12C 1.789(4) . ? B11C B12C 1.778(3) . ? C13C C14C 1.393(3) . ? C13C C18C 1.391(3) . ? C14C C15C 1.387(3) . ? C15C C16C 1.371(3) . ? C16C C17C 1.370(3) . ? C17C C18C 1.390(3) . ? N19C H1C 1.038(14) . ? N19C H2C 1.027(14) . ? C1D C2D 1.774(3) . ? C1D B3D 1.712(3) . ? C1D B4D 1.711(3) . ? C1D B5D 1.701(3) . ? C1D B6D 1.729(3) . ? C1D N19D 1.404(3) . ? C2D B3D 1.731(3) . ? C2D B6D 1.716(3) . ? C2D B7D 1.695(3) . ? C2D B11D 1.696(3) . ? C2D C13D 1.498(3) . ? B3D B4D 1.775(3) . ? B3D B7D 1.781(3) . ? B3D B8D 1.766(3) . ? B4D B5D 1.778(3) . ? B4D B8D 1.763(4) . ? B4D B9D 1.770(4) . ? B5D B6D 1.789(3) . ? B5D B9D 1.772(4) . ? B5D B10D 1.777(4) . ? B6D B10D 1.764(3) . ? B6D B11D 1.768(3) . ? B7D B8D 1.787(4) . ? B7D B11D 1.777(3) . ? B7D B12D 1.766(3) . ? B8D B9D 1.775(3) . ? B8D B12D 1.783(4) . ? B9D B10D 1.776(4) . ? B9D B12D 1.779(4) . ? B10D B11D 1.779(3) . ? B10D B12D 1.789(3) . ? B11D B12D 1.778(4) . ? C13D C14D 1.389(3) . ? C13D C18D 1.383(3) . ? C14D C15D 1.383(3) . ? C15D C16D 1.373(4) . ? C16D C17D 1.376(3) . ? C17D C18D 1.383(3) . ? N19D H1D 1.021(14) . ? N19D H2D 1.015(14) . ? 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 C2A C1A B3A 59.08(12) . . ? C2A C1A B4A 108.65(15) . . ? C2A C1A B5A 108.34(15) . . ? C2A C1A B6A 58.62(12) . . ? C2A C1A N19A 118.49(16) . . ? B3A C1A B4A 62.46(14) . . ? B3A C1A B5A 113.55(16) . . ? B3A C1A B6A 109.97(16) . . ? B3A C1A N19A 118.75(18) . . ? B4A C1A B5A 63.52(14) . . ? B4A C1A B6A 113.52(16) . . ? B4A C1A N19A 123.50(18) . . ? B5A C1A B6A 62.39(14) . . ? B5A C1A N19A 122.11(18) . . ? B6A C1A N19A 116.69(18) . . ? C1A C2A B3A 58.53(12) . . ? C1A C2A B6A 58.78(13) . . ? C1A C2A B7A 109.27(15) . . ? C1A C2A B11A 109.25(15) . . ? C1A C2A C13A 118.12(15) . . ? B3A C2A B6A 109.64(16) . . ? B3A C2A B7A 63.37(13) . . ? B3A C2A B11A 114.06(16) . . ? B3A C2A C13A 116.08(17) . . ? B6A C2A B7A 113.74(16) . . ? B6A C2A B11A 62.97(14) . . ? B6A C2A C13A 119.19(18) . . ? B7A C2A B11A 63.20(13) . . ? B7A C2A C13A 121.49(17) . . ? B11A C2A C13A 123.46(17) . . ? C1A B3A C2A 62.39(13) . . ? C1A B3A B4A 58.13(13) . . ? C1A B3A B7A 107.65(16) . . ? C1A B3A B8A 105.72(16) . . ? C2A B3A B4A 107.86(17) . . ? C2A B3A B7A 57.46(12) . . ? C2A B3A B8A 105.07(16) . . ? B4A B3A B7A 107.98(16) . . ? B4A B3A B8A 59.95(13) . . ? B7A B3A B8A 59.65(13) . . ? C1A B4A B3A 59.41(13) . . ? C1A B4A B5A 58.20(13) . . ? C1A B4A B8A 106.95(16) . . ? C1A B4A B9A 105.66(17) . . ? B3A B4A B5A 106.87(17) . . ? B3A B4A B8A 60.23(13) . . ? B3A B4A B9A 107.63(17) . . ? B5A B4A B8A 108.21(17) . . ? B5A B4A B9A 59.95(14) . . ? B8A B4A B9A 60.26(14) . . ? C1A B5A B4A 58.28(13) . . ? C1A B5A B6A 59.53(13) . . ? C1A B5A B9A 105.41(17) . . ? C1A B5A B10A 106.91(17) . . ? B4A B5A B6A 107.05(17) . . ? B4A B5A B9A 59.56(14) . . ? B4A B5A B10A 108.37(18) . . ? B6A B5A B9A 107.73(17) . . ? B6A B5A B10A 60.01(14) . . ? B9A B5A B10A 60.74(14) . . ? C1A B6A C2A 62.59(13) . . ? C1A B6A B5A 58.09(13) . . ? C1A B6A B10A 105.50(17) . . ? C1A B6A B11A 108.29(17) . . ? C2A B6A B5A 108.09(17) . . ? C2A B6A B10A 105.31(17) . . ? C2A B6A B11A 57.93(13) . . ? B5A B6A B10A 59.67(14) . . ? B5A B6A B11A 108.26(17) . . ? B10A B6A B11A 59.80(14) . . ? C2A B7A B3A 59.17(12) . . ? C2A B7A B8A 106.36(16) . . ? C2A B7A B11A 58.37(12) . . ? C2A B7A B12A 105.73(16) . . ? B3A B7A B8A 59.57(13) . . ? B3A B7A B11A 106.86(16) . . ? B3A B7A B12A 107.29(16) . . ? B8A B7A B11A 108.54(17) . . ? B8A B7A B12A 60.49(13) . . ? B11A B7A B12A 60.24(13) . . ? B3A B8A B4A 59.81(13) . . ? B3A B8A B7A 60.79(13) . . ? B3A B8A B9A 106.88(17) . . ? B3A B8A B12A 107.46(16) . . ? B4A B8A B7A 108.78(16) . . ? B4A B8A B9A 59.73(14) . . ? B4A B8A B12A 107.55(18) . . ? B7A B8A B9A 107.15(17) . . ? B7A B8A B12A 59.50(13) . . ? B9A B8A B12A 59.27(14) . . ? B4A B9A B5A 60.48(14) . . ? B4A B9A B8A 60.01(14) . . ? B4A B9A B10A 107.82(17) . . ? B4A B9A B12A 108.89(17) . . ? B5A B9A B8A 108.43(16) . . ? B5A B9A B10A 59.13(14) . . ? B5A B9A B12A 108.42(17) . . ? B8A B9A B10A 108.52(17) . . ? B8A B9A B12A 60.66(14) . . ? B10A B9A B12A 60.60(14) . . ? B5A B10A B6A 60.32(14) . . ? B5A B10A B9A 60.13(14) . . ? B5A B10A B11A 109.46(17) . . ? B5A B10A B12A 108.00(18) . . ? B6A B10A B9A 107.49(17) . . ? B6A B10A B11A 60.65(14) . . ? B6A B10A B12A 107.80(17) . . ? B9A B10A B11A 107.68(18) . . ? B9A B10A B12A 59.07(14) . . ? B11A B10A B12A 60.04(14) . . ? C2A B11A B6A 59.10(13) . . ? C2A B11A B7A 58.44(12) . . ? C2A B11A B10A 106.03(17) . . ? C2A B11A B12A 105.33(17) . . ? B6A B11A B7A 106.85(17) . . ? B6A B11A B10A 59.55(14) . . ? B6A B11A B12A 107.39(17) . . ? B7A B11A B10A 108.08(17) . . ? B7A B11A B12A 59.67(13) . . ? B10A B11A B12A 60.62(14) . . ? B7A B12A B8A 60.01(13) . . ? B7A B12A B9A 108.19(16) . . ? B7A B12A B10A 107.41(16) . . ? B7A B12A B11A 60.10(13) . . ? B8A B12A B9A 60.06(14) . . ? B8A B12A B10A 107.84(17) . . ? B8A B12A B11A 108.04(16) . . ? B9A B12A B10A 60.33(14) . . ? B9A B12A B11A 108.12(17) . . ? B10A B12A B11A 59.34(13) . . ? C2A C13A C14A 118.9(2) . . ? C2A C13A C18A 121.6(2) . . ? C14A C13A C18A 119.4(2) . . ? C13A C14A C15A 120.5(2) . . ? C14A C15A C16A 119.9(2) . . ? C15A C16A C17A 119.7(2) . . ? C16A C17A C18A 121.0(3) . . ? C13A C18A C17A 119.5(2) . . ? C1A N19A H1A 112.9(11) . . ? C1A N19A H2A 118.5(12) . . ? H1A N19A H2A 127.1(17) . . ? C2B C1B B3B 59.12(13) . . ? C2B C1B B4B 109.57(17) . . ? C2B C1B B5B 109.36(16) . . ? C2B C1B B6B 59.43(12) . . ? C2B C1B N19B 115.93(17) . . ? B3B C1B B4B 63.16(16) . . ? B3B C1B B5B 113.47(18) . . ? B3B C1B B6B 110.35(18) . . ? B3B C1B N19B 118.0(2) . . ? B4B C1B B5B 62.54(15) . . ? B4B C1B B6B 113.14(17) . . ? B4B C1B N19B 124.93(19) . . ? B5B C1B B6B 62.52(14) . . ? B5B C1B N19B 123.5(2) . . ? B6B C1B N19B 115.9(2) . . ? C1B C2B B3B 58.56(14) . . ? C1B C2B B6B 58.36(13) . . ? C1B C2B B7B 109.27(16) . . ? C1B C2B B11B 108.41(15) . . ? C1B C2B C13B 118.15(15) . . ? B3B C2B B6B 108.96(17) . . ? B3B C2B B7B 63.60(16) . . ? B3B C2B B11B 113.83(17) . . ? B3B C2B C13B 118.66(17) . . ? B6B C2B B7B 112.79(17) . . ? B6B C2B B11B 62.07(14) . . ? B6B C2B C13B 117.37(17) . . ? B7B C2B B11B 63.14(16) . . ? B7B C2B C13B 123.44(18) . . ? B11B C2B C13B 122.27(17) . . ? C1B B3B C2B 62.32(13) . . ? C1B B3B B4B 58.06(15) . . ? C1B B3B B7B 107.38(18) . . ? C1B B3B B8B 105.56(18) . . ? C2B B3B B4B 108.09(18) . . ? C2B B3B B7B 57.44(14) . . ? C2B B3B B8B 105.59(19) . . ? B4B B3B B7B 108.19(19) . . ? B4B B3B B8B 59.85(15) . . ? B7B B3B B8B 60.13(16) . . ? C1B B4B B3B 58.78(14) . . ? C1B B4B B5B 58.95(15) . . ? C1B B4B B8B 106.06(18) . . ? C1B B4B B9B 106.02(18) . . ? B3B B4B B5B 107.09(18) . . ? B3B B4B B8B 59.77(16) . . ? B3B B4B B9B 107.50(19) . . ? B5B B4B B8B 108.22(19) . . ? B5B B4B B9B 60.13(15) . . ? B8B B4B B9B 60.26(16) . . ? C1B B5B B4B 58.51(14) . . ? C1B B5B B6B 58.83(14) . . ? C1B B5B B9B 105.73(19) . . ? C1B B5B B10B 106.57(17) . . ? B4B B5B B6B 106.93(18) . . ? B4B B5B B9B 60.19(14) . . ? B4B B5B B10B 109.07(19) . . ? B6B B5B B9B 107.65(18) . . ? B6B B5B B10B 59.95(15) . . ? B9B B5B B10B 60.87(15) . . ? C1B B6B C2B 62.21(14) . . ? C1B B6B B5B 58.65(14) . . ? C1B B6B B10B 105.94(17) . . ? C1B B6B B11B 108.30(18) . . ? C2B B6B B5B 108.52(18) . . ? C2B B6B B10B 106.45(18) . . ? C2B B6B B11B 58.08(13) . . ? B5B B6B B10B 59.34(14) . . ? B5B B6B B11B 108.84(18) . . ? B10B B6B B11B 60.89(15) . . ? C2B B7B B3B 58.96(14) . . ? C2B B7B B8B 106.09(19) . . ? C2B B7B B11B 58.53(14) . . ? C2B B7B B12B 105.78(19) . . ? B3B B7B B8B 59.24(16) . . ? B3B B7B B11B 106.50(18) . . ? B3B B7B B12B 107.23(19) . . ? B8B B7B B11B 108.22(19) . . ? B8B B7B B12B 60.83(16) . . ? B11B B7B B12B 59.86(16) . . ? B3B B8B B4B 60.39(16) . . ? B3B B8B B7B 60.63(15) . . ? B3B B8B B9B 107.68(19) . . ? B3B B8B B12B 107.34(19) . . ? B4B B8B B7B 109.02(18) . . ? B4B B8B B9B 59.87(15) . . ? B4B B8B B12B 107.1(2) . . ? B7B B8B B9B 107.5(2) . . ? B7B B8B B12B 59.58(16) . . ? B9B B8B B12B 58.99(15) . . ? B4B B9B B5B 59.69(15) . . ? B4B B9B B8B 59.86(16) . . ? B4B B9B B10B 107.03(18) . . ? B4B B9B B12B 109.02(18) . . ? B5B B9B B8B 107.56(18) . . ? B5B B9B B10B 58.82(15) . . ? B5B B9B B12B 107.74(18) . . ? B8B B9B B10B 108.40(18) . . ? B8B B9B B12B 61.35(17) . . ? B10B B9B B12B 60.20(16) . . ? B5B B10B B6B 60.71(15) . . ? B5B B10B B9B 60.31(15) . . ? B5B B10B B11B 109.02(18) . . ? B5B B10B B12B 108.38(19) . . ? B6B B10B B9B 107.80(18) . . ? B6B B10B B11B 59.76(14) . . ? B6B B10B B12B 107.29(18) . . ? B9B B10B B11B 107.60(19) . . ? B9B B10B B12B 59.50(15) . . ? B11B B10B B12B 59.78(15) . . ? C2B B11B B6B 59.84(13) . . ? C2B B11B B7B 58.33(14) . . ? C2B B11B B10B 106.61(17) . . ? C2B B11B B12B 106.14(18) . . ? B6B B11B B7B 107.18(18) . . ? B6B B11B B10B 59.35(15) . . ? B6B B11B B12B 107.15(17) . . ? B7B B11B B10B 108.23(18) . . ? B7B B11B B12B 60.51(16) . . ? B10B B11B B12B 60.02(15) . . ? B7B B12B B8B 59.59(16) . . ? B7B B12B B9B 108.03(19) . . ? B7B B12B B10B 107.69(18) . . ? B7B B12B B11B 59.64(15) . . ? B8B B12B B9B 59.66(15) . . ? B8B B12B B10B 107.16(19) . . ? B8B B12B B11B 107.07(18) . . ? B9B B12B B10B 60.30(15) . . ? B9B B12B B11B 108.56(19) . . ? B10B B12B B11B 60.20(16) . . ? C2B C13B C14B 121.09(19) . . ? C2B C13B C18B 120.30(18) . . ? C14B C13B C18B 118.57(19) . . ? C13B C14B C15B 120.6(2) . . ? C14B C15B C16B 120.4(2) . . ? C15B C16B C17B 119.6(2) . . ? C16B C17B C18B 120.4(2) . . ? C13B C18B C17B 120.4(2) . . ? C2C C1C B3C 60.73(11) . . ? C2C C1C B4C 110.28(15) . . ? C2C C1C B5C 109.19(15) . . ? C2C C1C B6C 58.84(12) . . ? C2C C1C N19C 119.34(16) . . ? B3C C1C B4C 62.38(13) . . ? B3C C1C B5C 113.25(16) . . ? B3C C1C B6C 111.01(15) . . ? B3C C1C N19C 118.83(17) . . ? B4C C1C B5C 62.79(14) . . ? B4C C1C B6C 113.35(16) . . ? B4C C1C N19C 121.53(18) . . ? B5C C1C B6C 62.45(13) . . ? B5C C1C N19C 120.82(17) . . ? B6C C1C N19C 117.65(17) . . ? C1C C2C B3C 58.68(11) . . ? C1C C2C B6C 60.15(12) . . ? C1C C2C B7C 108.86(14) . . ? C1C C2C B11C 109.97(15) . . ? C1C C2C C13C 116.74(15) . . ? B3C C2C B6C 110.38(15) . . ? B3C C2C B7C 62.31(12) . . ? B3C C2C B11C 112.99(15) . . ? B3C C2C C13C 114.96(16) . . ? B6C C2C B7C 113.20(16) . . ? B6C C2C B11C 62.74(13) . . ? B6C C2C C13C 119.88(16) . . ? B7C C2C B11C 62.64(13) . . ? B7C C2C C13C 121.83(16) . . ? B11C C2C C13C 125.15(16) . . ? C1C B3C C2C 60.59(11) . . ? C1C B3C B4C 58.71(12) . . ? C1C B3C B7C 106.63(16) . . ? C1C B3C B8C 106.02(16) . . ? C2C B3C B4C 107.29(16) . . ? C2C B3C B7C 57.61(12) . . ? C2C B3C B8C 105.43(16) . . ? B4C B3C B7C 108.59(17) . . ? B4C B3C B8C 60.28(13) . . ? B7C B3C B8C 60.27(13) . . ? C1C B4C B3C 58.91(12) . . ? C1C B4C B5C 58.27(13) . . ? C1C B4C B8C 105.78(16) . . ? C1C B4C B9C 105.51(17) . . ? B3C B4C B5C 106.82(16) . . ? B3C B4C B8C 59.78(13) . . ? B3C B4C B9C 107.63(17) . . ? B5C B4C B8C 108.03(17) . . ? B5C B4C B9C 60.15(14) . . ? B8C B4C B9C 60.32(14) . . ? C1C B5C B4C 58.94(13) . . ? C1C B5C B6C 59.74(12) . . ? C1C B5C B9C 105.96(17) . . ? C1C B5C B10C 106.61(16) . . ? B4C B5C B6C 108.08(16) . . ? B4C B5C B9C 60.07(14) . . ? B4C B5C B10C 108.66(17) . . ? B6C B5C B9C 107.74(17) . . ? B6C B5C B10C 59.64(13) . . ? B9C B5C B10C 60.42(14) . . ? C1C B6C C2C 61.00(12) . . ? C1C B6C B5C 57.81(12) . . ? C1C B6C B10C 105.51(16) . . ? C1C B6C B11C 107.24(16) . . ? C2C B6C B5C 107.22(16) . . ? C2C B6C B10C 106.18(16) . . ? C2C B6C B11C 58.42(12) . . ? B5C B6C B10C 60.17(13) . . ? B5C B6C B11C 108.62(17) . . ? B10C B6C B11C 60.40(14) . . ? C2C B7C B3C 60.08(12) . . ? C2C B7C B8C 106.65(16) . . ? C2C B7C B11C 58.60(12) . . ? C2C B7C B12C 105.84(17) . . ? B3C B7C B8C 59.36(13) . . ? B3C B7C B11C 107.95(16) . . ? B3C B7C B12C 107.35(17) . . ? B8C B7C B11C 108.60(18) . . ? B8C B7C B12C 60.23(14) . . ? B11C B7C B12C 60.25(14) . . ? B3C B8C B4C 59.95(13) . . ? B3C B8C B7C 60.36(13) . . ? B3C B8C B9C 107.43(17) . . ? B3C B8C B12C 107.63(16) . . ? B4C B8C B7C 108.40(16) . . ? B4C B8C B9C 59.89(14) . . ? B4C B8C B12C 107.89(18) . . ? B7C B8C B9C 107.49(17) . . ? B7C B8C B12C 59.58(14) . . ? B9C B8C B12C 59.74(14) . . ? B4C B9C B5C 59.79(13) . . ? B4C B9C B8C 59.80(14) . . ? B4C B9C B10C 107.85(17) . . ? B4C B9C B12C 108.10(18) . . ? B5C B9C B8C 107.33(17) . . ? B5C B9C B10C 59.69(14) . . ? B5C B9C B12C 107.74(17) . . ? B8C B9C B10C 107.95(17) . . ? B8C B9C B12C 60.10(14) . . ? B10C B9C B12C 60.21(14) . . ? B5C B10C B6C 60.20(13) . . ? B5C B10C B9C 59.89(14) . . ? B5C B10C B11C 108.33(16) . . ? B5C B10C B12C 107.42(18) . . ? B6C B10C B9C 107.76(17) . . ? B6C B10C B11C 60.00(13) . . ? B6C B10C B12C 107.23(17) . . ? B9C B10C B11C 107.84(18) . . ? B9C B10C B12C 59.60(14) . . ? B11C B10C B12C 59.72(14) . . ? C2C B11C B6C 58.84(12) . . ? C2C B11C B7C 58.76(12) . . ? C2C B11C B10C 105.88(16) . . ? C2C B11C B12C 105.76(16) . . ? B6C B11C B7C 106.97(16) . . ? B6C B11C B10C 59.60(13) . . ? B6C B11C B12C 107.43(17) . . ? B7C B11C B10C 108.11(17) . . ? B7C B11C B12C 59.99(14) . . ? B10C B11C B12C 60.38(14) . . ? B7C B12C B8C 60.19(14) . . ? B7C B12C B9C 108.32(17) . . ? B7C B12C B10C 107.54(16) . . ? B7C B12C B11C 59.76(13) . . ? B8C B12C B9C 60.16(14) . . ? B8C B12C B10C 108.00(17) . . ? B8C B12C B11C 108.18(17) . . ? B9C B12C B10C 60.20(14) . . ? B9C B12C B11C 108.46(17) . . ? B10C B12C B11C 59.90(14) . . ? C2C C13C C14C 120.31(18) . . ? C2C C13C C18C 121.90(18) . . ? C14C C13C C18C 117.78(19) . . ? C13C C14C C15C 120.6(2) . . ? C14C C15C C16C 120.8(2) . . ? C15C C16C C17C 119.5(2) . . ? C16C C17C C18C 120.3(2) . . ? C13C C18C C17C 121.0(2) . . ? C1C N19C H1C 111.7(11) . . ? C1C N19C H2C 113.5(11) . . ? H1C N19C H2C 102.8(16) . . ? C2D C1D B3D 59.53(12) . . ? C2D C1D B4D 109.38(15) . . ? C2D C1D B5D 109.21(15) . . ? C2D C1D B6D 58.63(11) . . ? C2D C1D N19D 119.75(17) . . ? B3D C1D B4D 62.44(14) . . ? B3D C1D B5D 113.13(16) . . ? B3D C1D B6D 109.80(15) . . ? B3D C1D N19D 119.36(18) . . ? B4D C1D B5D 62.81(13) . . ? B4D C1D B6D 113.17(16) . . ? B4D C1D N19D 121.84(18) . . ? B5D C1D B6D 62.85(13) . . ? B5D C1D N19D 120.71(18) . . ? B6D C1D N19D 117.88(17) . . ? C1D C2D B3D 58.47(12) . . ? C1D C2D B6D 59.39(11) . . ? C1D C2D B7D 108.93(15) . . ? C1D C2D B11D 109.37(15) . . ? C1D C2D C13D 116.23(15) . . ? B3D C2D B6D 109.55(15) . . ? B3D C2D B7D 62.62(14) . . ? B3D C2D B11D 113.33(16) . . ? B3D C2D C13D 114.64(16) . . ? B6D C2D B7D 113.21(16) . . ? B6D C2D B11D 62.44(13) . . ? B6D C2D C13D 120.06(16) . . ? B7D C2D B11D 63.22(13) . . ? B7D C2D C13D 122.14(16) . . ? B11D C2D C13D 125.82(17) . . ? C1D B3D C2D 62.00(12) . . ? C1D B3D B4D 58.75(13) . . ? C1D B3D B7D 107.82(16) . . ? C1D B3D B8D 105.93(16) . . ? C2D B3D B4D 108.43(16) . . ? C2D B3D B7D 57.69(12) . . ? C2D B3D B8D 105.80(17) . . ? B4D B3D B7D 108.83(17) . . ? B4D B3D B8D 59.71(14) . . ? B7D B3D B8D 60.50(14) . . ? C1D B4D B3D 58.81(13) . . ? C1D B4D B5D 58.31(13) . . ? C1D B4D B8D 106.12(17) . . ? C1D B4D B9D 105.22(17) . . ? B3D B4D B5D 106.59(16) . . ? B3D B4D B8D 59.89(14) . . ? B3D B4D B9D 107.19(18) . . ? B5D B4D B8D 108.21(18) . . ? B5D B4D B9D 59.91(14) . . ? B8D B4D B9D 60.32(15) . . ? C1D B5D B4D 58.89(13) . . ? C1D B5D B6D 59.35(12) . . ? C1D B5D B9D 105.60(17) . . ? C1D B5D B10D 106.14(17) . . ? B4D B5D B6D 107.27(16) . . ? B4D B5D B9D 59.82(14) . . ? B4D B5D B10D 108.00(18) . . ? B6D B5D B9D 106.84(18) . . ? B6D B5D B10D 59.32(14) . . ? B9D B5D B10D 60.05(15) . . ? C1D B6D C2D 61.98(12) . . ? C1D B6D B5D 57.80(12) . . ? C1D B6D B10D 105.46(16) . . ? C1D B6D B11D 108.11(16) . . ? C2D B6D B5D 107.86(16) . . ? C2D B6D B10D 105.96(16) . . ? C2D B6D B11D 58.24(12) . . ? B5D B6D B10D 60.00(14) . . ? B5D B6D B11D 109.00(17) . . ? B10D B6D B11D 60.46(14) . . ? C2D B7D B3D 59.69(12) . . ? C2D B7D B8D 106.44(17) . . ? C2D B7D B11D 58.41(12) . . ? C2D B7D B12D 105.94(16) . . ? B3D B7D B8D 59.33(14) . . ? B3D B7D B11D 107.17(16) . . ? B3D B7D B12D 107.25(17) . . ? B8D B7D B11D 108.22(17) . . ? B8D B7D B12D 60.26(14) . . ? B11D B7D B12D 60.23(14) . . ? B3D B8D B4D 60.40(14) . . ? B3D B8D B7D 60.17(13) . . ? B3D B8D B9D 107.38(18) . . ? B3D B8D B12D 107.15(17) . . ? B4D B8D B7D 109.12(17) . . ? B4D B8D B9D 60.06(15) . . ? B4D B8D B12D 108.50(17) . . ? B7D B8D B9D 107.57(18) . . ? B7D B8D B12D 59.29(14) . . ? B9D B8D B12D 59.99(15) . . ? B4D B9D B5D 60.27(14) . . ? B4D B9D B8D 59.63(14) . . ? B4D B9D B10D 108.40(18) . . ? B4D B9D B12D 108.36(17) . . ? B5D B9D B8D 107.94(17) . . ? B5D B9D B10D 60.11(14) . . ? B5D B9D B12D 108.64(18) . . ? B8D B9D B10D 108.30(18) . . ? B8D B9D B12D 60.25(15) . . ? B10D B9D B12D 60.44(15) . . ? B5D B10D B6D 60.67(13) . . ? B5D B10D B9D 59.83(14) . . ? B5D B10D B11D 109.08(17) . . ? B5D B10D B12D 107.96(17) . . ? B6D B10D B9D 107.73(17) . . ? B6D B10D B11D 59.88(13) . . ? B6D B10D B12D 107.11(16) . . ? B9D B10D B11D 108.15(17) . . ? B9D B10D B12D 59.87(15) . . ? B11D B10D B12D 59.77(14) . . ? C2D B11D B6D 59.32(12) . . ? C2D B11D B7D 58.37(12) . . ? C2D B11D B10D 106.19(16) . . ? C2D B11D B12D 105.38(17) . . ? B6D B11D B7D 106.86(16) . . ? B6D B11D B10D 59.67(13) . . ? B6D B11D B12D 107.44(17) . . ? B7D B11D B10D 107.74(18) . . ? B7D B11D B12D 59.56(14) . . ? B10D B11D B12D 60.41(14) . . ? B7D B12D B8D 60.45(14) . . ? B7D B12D B9D 108.31(18) . . ? B7D B12D B10D 107.78(17) . . ? B7D B12D B11D 60.21(13) . . ? B8D B12D B9D 59.77(15) . . ? B8D B12D B10D 107.33(18) . . ? B8D B12D B11D 108.34(17) . . ? B9D B12D B10D 59.69(14) . . ? B9D B12D B11D 108.04(18) . . ? B10D B12D B11D 59.82(14) . . ? C2D C13D C14D 119.46(19) . . ? C2D C13D C18D 122.32(19) . . ? C14D C13D C18D 118.2(2) . . ? C13D C14D C15D 121.0(2) . . ? C14D C15D C16D 120.2(2) . . ? C15D C16D C17D 119.4(2) . . ? C16D C17D C18D 120.6(2) . . ? C13D C18D C17D 120.6(2) . . ? C1D N19D H1D 114.0(11) . . ? C1D N19D H2D 114.9(11) . . ? H1D N19D H2D 117.5(16) . . ? _diffrn_measured_fraction_theta_max 0.897 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.830 _refine_diff_density_min -0.328 _refine_diff_density_rms 0.067 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 237441' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C14 H35 B10 N4 O P' _chemical_formula_sum 'C14 H35 B10 N4 O P' _chemical_formula_weight 414.53 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.526(3) _cell_length_b 21.680(3) _cell_length_c 12.111(2) _cell_angle_alpha 90.00 _cell_angle_beta 115.48(2) _cell_angle_gamma 90.00 _cell_volume 2495.0(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9.57 _cell_measurement_theta_max 21.66 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.104 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 1.054 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.863 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'TEXSAN v.5.1 (MSC, 1989), from 108 \y-scans of 3 reflections' _exptl_special_details ; 3124 unique reflections after merging Friedel equivalents ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku AFC6S 4-circle diffractometer' _diffrn_measurement_method '2\q/\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 5324 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_sigmaI/netI 0.0562 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 4.04 _diffrn_reflns_theta_max 60.00 _reflns_number_total 4179 _reflns_number_observed 3104 _reflns_observed_criterion I>2\s(I) _reflns_Friedel_coverage 0.34 _computing_data_collection 'AFC (MSC, 1989)' _computing_cell_refinement 'AFC (MSC, 1989)' _computing_data_reduction 'TEXSAN version 5.1 (MSC, 1989)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL version 5.10 (Bruker, 1997)' _computing_publication_material 'SHELXTL version 5.10 (Bruker, 1997)' _refine_special_details ; Refinement on F^2^ for ALL reflections. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0699P)^2^+0.2009P] 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 0.0019(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(3) _refine_ls_number_reflns 4179 _refine_ls_number_parameters 567 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0762 _refine_ls_R_factor_obs 0.0496 _refine_ls_wR_factor_all 0.1291 _refine_ls_wR_factor_obs 0.1143 _refine_ls_goodness_of_fit_all 1.059 _refine_ls_goodness_of_fit_obs 1.116 _refine_ls_restrained_S_all 1.059 _refine_ls_restrained_S_obs 1.115 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group P1 P 0.6297(2) 0.80737(7) 0.57544(14) 0.0659(5) Uani 1 d . . O1 O 0.4820(4) 0.8108(2) 0.4866(4) 0.0914(14) Uani 1 d . . N11 N 0.7274(8) 0.7793(4) 0.5092(7) 0.114(2) Uani 1 d . . C12 C 0.6720(13) 0.7532(8) 0.3946(11) 0.258(9) Uani 1 d . . H121 H 0.6944(151) 0.7785(40) 0.3403(38) 0.387 Uiso 1 calc R . H122 H 0.5716(22) 0.7501(72) 0.3644(65) 0.387 Uiso 1 calc R . H123 H 0.7112(132) 0.7128(30) 0.3991(27) 0.387 Uiso 1 calc R . C13 C 0.8703(12) 0.7774(11) 0.5609(11) 0.298(13) Uani 1 d . . H131 H 0.9008(12) 0.7388(36) 0.5418(155) 0.448 Uiso 1 calc R . H132 H 0.9058(13) 0.7816(98) 0.6480(20) 0.448 Uiso 1 calc R . H133 H 0.9054(13) 0.8106(54) 0.5293(140) 0.448 Uiso 1 calc R . N14 N 0.6478(8) 0.7638(3) 0.6884(6) 0.106(2) Uani 1 d . . C15 C 0.7864(12) 0.7536(8) 0.7943(10) 0.281(10) Uani 1 d . . H151 H 0.7719(12) 0.7387(85) 0.8627(55) 0.421 Uiso 1 calc R . H152 H 0.8375(82) 0.7918(18) 0.8160(107) 0.421 Uiso 1 calc R . H153 H 0.8391(80) 0.7237(62) 0.7727(60) 0.421 Uiso 1 calc R . C16 C 0.5430(13) 0.7266(5) 0.6910(8) 0.174(5) Uani 1 d . . H161 H 0.5598(54) 0.7193(35) 0.7743(8) 0.261 Uiso 1 calc R . H162 H 0.5426(62) 0.6880(16) 0.6519(73) 0.261 Uiso 1 calc R . H163 H 0.4536(17) 0.7466(18) 0.6484(71) 0.261 Uiso 1 calc R . N17 N 0.7051(7) 0.8714(3) 0.6370(6) 0.101(2) Uani 1 d . . C18 C 0.6769(14) 0.9040(7) 0.7187(11) 0.221(7) Uani 1 d . . H181 H 0.7000(146) 0.9466(13) 0.7153(95) 0.331 Uiso 1 calc R . H182 H 0.7320(114) 0.8883(43) 0.7994(19) 0.331 Uiso 1 calc R . H183 H 0.5787(33) 0.9004(56) 0.6994(80) 0.331 Uiso 1 calc R . C19 C 0.7389(16) 0.9125(6) 0.5527(11) 0.226(7) Uani 1 d . . H191 H 0.7984(124) 0.9457(37) 0.5989(26) 0.339 Uiso 1 calc R . H192 H 0.6533(20) 0.9290(52) 0.4908(78) 0.339 Uiso 1 calc R . H193 H 0.7866(130) 0.8890(16) 0.5148(97) 0.339 Uiso 1 calc R . P2 P 0.3413(2) 0.82682(8) 0.99038(14) 0.0670(5) Uani 1 d . . O2 O 0.2724(4) 0.8311(2) 1.0736(3) 0.0770(12) Uani 1 d . . N21 N 0.5050(6) 0.8505(3) 1.0614(5) 0.086(2) Uani 1 d . . C22 C 0.5475(10) 0.8927(5) 1.1588(9) 0.164(4) Uani 1 d . . H221 H 0.4678(21) 0.9164(28) 1.1528(45) 0.246 Uiso 1 calc R . H222 H 0.6176(66) 0.9199(25) 1.1551(45) 0.246 Uiso 1 calc R . H223 H 0.5861(81) 0.8707(6) 1.2350(9) 0.246 Uiso 1 calc R . C23 C 0.6090(9) 0.8447(5) 1.0119(8) 0.151(4) Uani 1 d . . H231 H 0.6300(61) 0.8848(7) 0.9903(66) 0.227 Uiso 1 calc R . H232 H 0.5718(36) 0.8190(31) 0.9404(46) 0.227 Uiso 1 calc R . H233 H 0.6934(33) 0.8265(34) 1.0723(30) 0.227 Uiso 1 calc R . N24 N 0.2533(7) 0.8667(3) 0.8667(5) 0.097(2) Uani 1 d . . C25 C 0.2920(11) 0.8719(5) 0.7659(8) 0.167(4) Uani 1 d . . H251 H 0.2085(11) 0.8745(44) 0.6904(10) 0.251 Uiso 1 calc R . H252 H 0.3455(83) 0.8363(20) 0.7644(51) 0.251 Uiso 1 calc R . H253 H 0.3478(81) 0.9083(22) 0.7762(44) 0.251 Uiso 1 calc R . C26 C 0.1552(12) 0.9118(5) 0.8633(8) 0.185(6) Uani 1 d . . H261 H 0.0954(68) 0.9221(33) 0.7798(8) 0.278 Uiso 1 calc R . H262 H 0.2044(13) 0.9480(16) 0.9059(76) 0.278 Uiso 1 calc R . H263 H 0.0991(67) 0.8959(16) 0.9018(78) 0.278 Uiso 1 calc R . N27 N 0.3569(7) 0.7599(3) 0.9396(5) 0.085(2) Uani 1 d . . C28 C 0.2354(10) 0.7294(4) 0.8421(7) 0.122(3) Uani 1 d . . H281 H 0.2644(18) 0.7107(26) 0.7847(33) 0.183 Uiso 1 calc R . H282 H 0.1634(29) 0.7594(7) 0.8007(39) 0.183 Uiso 1 calc R . H283 H 0.1993(43) 0.6982(21) 0.8772(10) 0.183 Uiso 1 calc R . C29 C 0.4552(10) 0.7145(4) 1.0235(7) 0.124(3) Uani 1 d . . H291 H 0.5017(50) 0.6927(21) 0.9822(20) 0.186 Uiso 1 calc R . H292 H 0.4041(13) 0.6857(17) 1.0493(45) 0.186 Uiso 1 calc R . H293 H 0.5240(40) 0.7354(4) 1.0936(29) 0.186 Uiso 1 calc R . N1 N 0.7192(8) 0.3931(3) 0.7032(5) 0.084(2) Uani 1 d D . H1A H 0.7509(71) 0.3759(28) 0.7763(31) 0.100 Uiso 1 d D . H1B H 0.6642(58) 0.3698(25) 0.6372(39) 0.100 Uiso 1 d D . C101 C 0.8157(7) 0.4322(3) 0.6942(5) 0.061(2) Uani 1 d . . C102 C 0.7849(6) 0.5150(3) 0.7117(5) 0.055(2) Uani 1 d . . B103 B 0.9189(8) 0.4744(3) 0.8219(6) 0.064(2) Uani 1 d . . H103 H 0.9188(8) 0.4648(3) 0.9102(6) 0.076 Uiso 1 calc R . B104 B 0.9890(9) 0.4233(4) 0.7505(6) 0.073(2) Uani 1 d . . H104 H 1.0410(9) 0.3808(4) 0.7951(6) 0.088 Uiso 1 calc R . B105 B 0.8809(9) 0.4273(4) 0.5897(6) 0.077(2) Uani 1 d . . H105 H 0.8601(9) 0.3881(4) 0.5280(6) 0.092 Uiso 1 calc R . B106 B 0.7524(9) 0.4839(3) 0.5710(6) 0.063(2) Uani 1 d . . H106 H 0.6460(9) 0.4800(3) 0.4985(6) 0.076 Uiso 1 calc R . B107 B 0.9416(8) 0.5507(4) 0.7792(6) 0.070(2) Uani 1 d . . H107 H 0.9621(8) 0.5899(4) 0.8410(6) 0.084 Uiso 1 calc R . B108 B 1.0702(9) 0.4930(4) 0.8008(7) 0.079(2) Uani 1 d . . H108 H 1.1742(9) 0.4951(4) 0.8775(7) 0.095 Uiso 1 calc R . B109 B 1.0479(10) 0.4664(5) 0.6565(7) 0.087(3) Uani 1 d . . H109 H 1.1358(10) 0.4520(5) 0.6377(7) 0.105 Uiso 1 calc R . B110 B 0.8988(8) 0.5044(4) 0.5451(7) 0.074(2) Uani 1 d . . H110 H 0.8895(8) 0.5144(4) 0.4538(7) 0.089 Uiso 1 calc R . B111 B 0.8344(8) 0.5572(4) 0.6200(6) 0.067(2) Uani 1 d . . H111 H 0.7841(8) 0.6004(4) 0.5776(6) 0.081 Uiso 1 calc R . B112 B 1.0183(9) 0.5437(4) 0.6753(7) 0.078(2) Uani 1 d . . H112 H 1.0889(9) 0.5791(4) 0.6695(7) 0.094 Uiso 1 calc R . C113 C 0.6626(7) 0.5324(3) 0.7378(6) 0.056(2) Uani 1 d . . C114 C 0.5254(8) 0.5371(3) 0.6467(6) 0.072(2) Uani 1 d . . H114 H 0.5079(8) 0.5288(3) 0.5661(6) 0.087 Uiso 1 calc R . C115 C 0.4155(8) 0.5537(4) 0.6729(7) 0.084(2) Uani 1 d . . H115 H 0.3251(8) 0.5564(4) 0.6101(7) 0.100 Uiso 1 calc R . C116 C 0.4379(8) 0.5661(3) 0.7902(8) 0.083(2) Uani 1 d . . H116 H 0.3631(8) 0.5756(3) 0.8087(8) 0.099 Uiso 1 calc R . C117 C 0.5707(9) 0.5643(4) 0.8788(7) 0.090(2) Uani 1 d . . H117 H 0.5875(9) 0.5753(4) 0.9581(7) 0.109 Uiso 1 calc R . C118 C 0.6843(7) 0.5465(3) 0.8546(6) 0.075(2) Uani 1 d . . H118 H 0.7744(7) 0.5442(3) 0.9180(6) 0.090 Uiso 1 calc R . N2 N 0.2879(7) 0.7407(2) 0.2550(5) 0.077(2) Uani 1 d D . H2A H 0.3520(52) 0.7540(29) 0.3277(31) 0.093 Uiso 1 d D . H2B H 0.2894(64) 0.7667(24) 0.1981(42) 0.093 Uiso 1 d D . C201 C 0.1739(8) 0.7091(3) 0.2499(5) 0.069(2) Uani 1 d . . C202 C 0.1809(7) 0.6257(3) 0.2387(5) 0.055(2) Uani 1 d . . B203 B 0.2005(9) 0.6612(3) 0.3709(6) 0.074(2) Uani 1 d . . H203 H 0.3008(9) 0.6609(3) 0.4520(6) 0.088 Uiso 1 calc R . B204 B 0.0834(10) 0.7245(4) 0.3346(7) 0.085(3) Uani 1 d . . H204 H 0.1047(10) 0.7644(4) 0.3948(7) 0.102 Uiso 1 calc R . B205 B 0.0023(8) 0.7289(4) 0.1710(7) 0.082(3) Uani 1 d . . H205 H -0.0307(8) 0.7724(4) 0.1221(7) 0.099 Uiso 1 calc R . B206 B 0.0734(8) 0.6688(3) 0.1181(6) 0.064(2) Uani 1 d . . H206 H 0.0922(8) 0.6740(3) 0.0369(6) 0.076 Uiso 1 calc R . B207 B 0.0986(9) 0.5929(4) 0.3164(7) 0.076(2) Uani 1 d . . H207 H 0.1296(9) 0.5491(4) 0.3647(7) 0.091 Uiso 1 calc R . B208 B 0.0329(10) 0.6543(5) 0.3728(8) 0.094(3) Uani 1 d . . H208 H 0.0205(10) 0.6497(5) 0.4572(8) 0.113 Uiso 1 calc R . B209 B -0.0878(12) 0.6969(5) 0.2466(8) 0.103(3) Uani 1 d . . H209 H -0.1793(12) 0.7201(5) 0.2475(8) 0.123 Uiso 1 calc R . B210 B -0.0929(8) 0.6611(4) 0.1136(7) 0.082(3) Uani 1 d . . H210 H -0.1880(8) 0.6607(4) 0.0277(7) 0.099 Uiso 1 calc R . B211 B 0.0191(8) 0.5980(4) 0.1545(6) 0.067(2) Uani 1 d . . H211 H -0.0024(8) 0.5576(4) 0.0957(6) 0.080 Uiso 1 calc R . B212 B -0.0765(11) 0.6153(5) 0.2391(8) 0.095(3) Uani 1 d . . H212 H -0.1608(11) 0.5853(5) 0.2367(8) 0.114 Uiso 1 calc R . C213 C 0.3071(7) 0.5995(3) 0.2283(6) 0.057(2) Uani 1 d . . C214 C 0.2916(8) 0.5652(3) 0.1259(7) 0.079(2) Uani 1 d . . H214 H 0.2016(8) 0.5581(3) 0.0648(7) 0.095 Uiso 1 calc R . C215 C 0.4029(9) 0.5419(4) 0.1127(7) 0.093(2) Uani 1 d . . H215 H 0.3885(9) 0.5192(4) 0.0432(7) 0.112 Uiso 1 calc R . C216 C 0.5386(9) 0.5515(4) 0.2017(8) 0.093(2) Uani 1 d . . H216 H 0.6152(9) 0.5349(4) 0.1928(8) 0.112 Uiso 1 calc R . C217 C 0.5583(9) 0.5853(4) 0.3014(7) 0.090(2) Uani 1 d . . H217 H 0.6489(9) 0.5930(4) 0.3607(7) 0.108 Uiso 1 calc R . C218 C 0.4425(9) 0.6086(3) 0.3158(6) 0.077(2) Uani 1 d . . H218 H 0.4573(9) 0.6308(3) 0.3860(6) 0.092 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 P1 0.0659(12) 0.0618(11) 0.0699(10) 0.0060(9) 0.0292(10) 0.0057(10) O1 0.065(3) 0.104(4) 0.092(3) 0.013(3) 0.020(2) 0.007(3) N11 0.089(5) 0.160(7) 0.113(5) -0.009(5) 0.061(4) 0.007(5) C12 0.196(12) 0.415(24) 0.213(11) -0.208(14) 0.134(10) -0.100(13) C13 0.101(8) 0.617(40) 0.173(10) -0.068(16) 0.056(8) 0.092(15) N14 0.100(5) 0.115(5) 0.108(5) 0.039(4) 0.050(4) 0.006(4) C15 0.149(11) 0.474(28) 0.196(11) 0.221(16) 0.053(10) 0.067(14) C16 0.261(13) 0.143(9) 0.132(7) -0.020(6) 0.097(9) -0.117(9) N17 0.102(5) 0.079(5) 0.113(5) 0.008(4) 0.038(4) 0.000(4) C18 0.245(15) 0.250(16) 0.236(12) -0.156(13) 0.168(12) -0.090(12) C19 0.276(17) 0.156(12) 0.215(12) 0.054(10) 0.076(12) -0.063(11) P2 0.0759(13) 0.0678(12) 0.0619(10) 0.0022(9) 0.0339(10) -0.0008(10) O2 0.089(3) 0.079(3) 0.082(2) 0.001(2) 0.055(2) -0.004(3) N21 0.079(4) 0.101(5) 0.078(3) -0.021(3) 0.034(3) -0.019(4) C22 0.126(8) 0.191(10) 0.176(9) -0.105(9) 0.066(7) -0.045(8) C23 0.109(7) 0.215(12) 0.167(8) -0.055(8) 0.094(6) -0.047(7) N24 0.123(6) 0.095(5) 0.074(4) 0.023(3) 0.043(4) 0.018(4) C25 0.215(12) 0.201(11) 0.103(6) 0.044(7) 0.085(8) 0.024(9) C26 0.247(14) 0.173(11) 0.108(7) 0.043(7) 0.050(8) 0.123(11) N27 0.100(5) 0.077(4) 0.081(4) -0.011(4) 0.043(4) -0.008(4) C28 0.139(8) 0.105(6) 0.114(6) -0.035(5) 0.048(6) -0.008(6) C29 0.169(9) 0.079(6) 0.128(6) -0.001(5) 0.068(6) 0.028(6) N1 0.119(6) 0.063(4) 0.069(4) -0.003(3) 0.041(4) -0.031(4) C101 0.078(5) 0.047(4) 0.059(4) 0.000(3) 0.030(4) -0.007(4) C102 0.054(4) 0.047(4) 0.063(4) 0.001(3) 0.025(3) 0.000(3) B103 0.069(6) 0.056(5) 0.054(4) 0.007(4) 0.016(4) 0.007(4) B104 0.081(7) 0.069(6) 0.061(4) -0.002(4) 0.023(5) 0.013(5) B105 0.087(6) 0.092(6) 0.059(4) 0.004(4) 0.038(5) 0.009(5) B106 0.078(6) 0.054(4) 0.049(4) -0.001(3) 0.020(4) -0.005(4) B107 0.062(6) 0.071(5) 0.067(5) -0.006(4) 0.019(4) -0.020(5) B108 0.056(5) 0.106(7) 0.070(5) -0.003(5) 0.022(4) 0.003(5) B109 0.081(7) 0.117(8) 0.075(5) -0.008(5) 0.044(5) -0.003(6) B110 0.077(6) 0.091(6) 0.065(5) 0.004(4) 0.039(5) -0.009(5) B111 0.067(5) 0.068(5) 0.067(4) 0.000(4) 0.029(4) -0.017(4) B112 0.073(6) 0.084(6) 0.088(6) 0.001(5) 0.045(5) -0.010(5) C113 0.049(5) 0.049(4) 0.067(4) -0.004(3) 0.023(4) -0.007(3) C114 0.064(5) 0.079(5) 0.067(4) 0.000(4) 0.021(4) -0.007(4) C115 0.046(5) 0.099(6) 0.100(6) 0.007(5) 0.025(4) 0.004(4) C116 0.059(6) 0.087(6) 0.106(6) -0.010(5) 0.039(5) -0.013(4) C117 0.082(6) 0.111(6) 0.094(5) -0.025(5) 0.053(5) -0.008(5) C118 0.051(5) 0.106(5) 0.064(4) -0.019(4) 0.022(4) 0.000(4) N2 0.088(5) 0.060(4) 0.078(4) 0.008(3) 0.029(4) -0.021(4) C201 0.099(6) 0.052(4) 0.059(4) 0.003(3) 0.036(4) -0.005(4) C202 0.059(4) 0.043(4) 0.062(4) 0.006(3) 0.026(3) 0.004(3) B203 0.103(7) 0.063(5) 0.061(4) 0.009(4) 0.042(5) 0.004(5) B204 0.125(9) 0.077(6) 0.076(5) -0.003(5) 0.065(6) 0.028(6) B205 0.074(6) 0.086(6) 0.081(5) 0.021(5) 0.028(5) 0.027(5) B206 0.063(5) 0.059(5) 0.062(4) 0.015(4) 0.020(4) 0.000(4) B207 0.077(6) 0.073(6) 0.084(5) 0.017(5) 0.041(5) -0.007(5) B208 0.109(8) 0.113(8) 0.085(6) 0.009(6) 0.065(6) 0.003(7) B209 0.104(8) 0.117(9) 0.116(7) 0.004(6) 0.075(7) 0.025(7) B210 0.061(6) 0.097(7) 0.093(6) -0.005(5) 0.037(5) 0.004(5) B211 0.057(5) 0.068(5) 0.073(5) -0.003(4) 0.026(4) -0.019(4) B212 0.090(7) 0.097(7) 0.115(7) 0.015(6) 0.061(6) -0.002(6) C213 0.058(5) 0.046(4) 0.058(4) 0.007(3) 0.016(4) -0.003(3) C214 0.059(5) 0.081(5) 0.094(5) -0.016(4) 0.030(4) -0.006(4) C215 0.074(6) 0.099(6) 0.108(6) -0.030(5) 0.040(6) -0.006(5) C216 0.064(6) 0.088(6) 0.119(6) -0.003(5) 0.032(5) 0.008(5) C217 0.074(7) 0.095(6) 0.084(5) 0.003(5) 0.018(5) 0.008(5) C218 0.073(6) 0.084(5) 0.064(4) 0.002(4) 0.019(5) 0.007(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 P1 O1 1.463(4) . Y P1 N14 1.605(6) . Y P1 N17 1.614(7) . Y P1 N11 1.668(7) . Y N11 C13 1.359(11) . Y N11 C12 1.375(11) . Y C12 H121 0.96 . ? C12 H122 0.96 . ? C12 H123 0.96 . ? C13 H131 0.96 . ? C13 H132 0.96 . ? C13 H133 0.96 . ? N14 C16 1.377(10) . Y N14 C15 1.488(12) . Y C15 H151 0.96 . ? C15 H152 0.96 . ? C15 H153 0.96 . ? C16 H161 0.96 . ? C16 H162 0.96 . ? C16 H163 0.96 . ? N17 C18 1.349(10) . Y N17 C19 1.508(12) . Y C18 H181 0.96 . ? C18 H182 0.96 . ? C18 H183 0.96 . ? C19 H191 0.96 . ? C19 H192 0.96 . ? C19 H193 0.96 . ? P2 O2 1.476(4) . Y P2 N27 1.611(6) . Y P2 N24 1.629(6) . Y P2 N21 1.642(6) . Y N21 C22 1.405(9) . Y N21 C23 1.463(8) . Y C22 H221 0.96 . ? C22 H222 0.96 . ? C22 H223 0.96 . ? C23 H231 0.96 . ? C23 H232 0.96 . ? C23 H233 0.96 . ? N24 C26 1.409(10) . Y N24 C25 1.448(10) . Y C25 H251 0.96 . ? C25 H252 0.96 . ? C25 H253 0.96 . ? C26 H261 0.96 . ? C26 H262 0.96 . ? C26 H263 0.96 . ? N27 C29 1.473(9) . Y N27 C28 1.473(9) . Y C28 H281 0.96 . ? C28 H282 0.96 . ? C28 H283 0.96 . ? C29 H291 0.96 . ? C29 H292 0.96 . ? C29 H293 0.96 . ? N1 C101 1.363(8) . Y N1 H1A 0.88(2) . ? N1 H1B 0.91(2) . ? C101 B104 1.661(11) . Y C101 B105 1.683(9) . Y C101 B103 1.722(9) . Y C101 B106 1.751(9) . Y C101 C102 1.853(8) . Y C102 C113 1.500(8) . Y C102 B107 1.682(9) . Y C102 B111 1.685(9) . Y C102 B103 1.711(9) . Y C102 B106 1.724(9) . Y B103 B104 1.753(11) . Y B103 B108 1.765(12) . Y B103 B107 1.779(11) . Y B103 H103 1.09 . ? B104 B108 1.713(12) . Y B104 B109 1.777(12) . Y B104 B105 1.785(10) . Y B104 H104 1.09 . ? B105 B106 1.767(11) . Y B105 B110 1.793(12) . Y B105 B109 1.800(12) . Y B105 H105 1.09 . ? B106 B110 1.757(11) . Y B106 B111 1.785(11) . Y B106 H106 1.09 . ? B107 B112 1.770(11) . Y B107 B111 1.772(10) . Y B107 B108 1.779(12) . Y B107 H107 1.09 . ? B108 B109 1.757(12) . Y B108 B112 1.762(12) . Y B108 H108 1.09 . ? B109 B112 1.738(13) . Y B109 B110 1.772(12) . Y B109 H109 1.09 . ? B110 B112 1.757(11) . Y B110 B111 1.766(11) . Y B110 H110 1.09 . ? B111 B112 1.779(11) . Y B111 H111 1.09 . ? B112 H112 1.09 . ? C113 C118 1.367(8) . Y C113 C114 1.393(8) . Y C114 C115 1.372(9) . Y C114 H114 0.93 . ? C115 C116 1.364(9) . Y C115 H115 0.93 . ? C116 C117 1.348(9) . Y C116 H116 0.93 . ? C117 C118 1.402(9) . Y C117 H117 0.93 . ? C118 H118 0.93 . ? N2 C201 1.360(9) . Y N2 H2A 0.90(2) . ? N2 H2B 0.90(2) . ? C201 B205 1.695(10) . Y C201 B204 1.706(10) . Y C201 B203 1.718(9) . Y C201 B206 1.726(10) . Y C201 C202 1.816(8) . Y C202 C213 1.500(9) . Y C202 B211 1.675(9) . Y C202 B207 1.687(9) . Y C202 B206 1.692(9) . Y C202 B203 1.706(9) . Y B203 B204 1.770(12) . Y B203 B207 1.779(11) . Y B203 B208 1.781(12) . Y B203 H203 1.09 . ? B204 B208 1.739(13) . Y B204 B209 1.757(14) . Y B204 B205 1.791(12) . Y B204 H204 1.09 . ? B205 B209 1.722(13) . Y B205 B210 1.745(12) . Y B205 B206 1.754(11) . Y B205 H205 1.09 . ? B206 B210 1.736(11) . Y B206 B211 1.758(10) . Y B206 H206 1.09 . ? B207 B212 1.739(12) . Y B207 B208 1.767(12) . Y B207 B211 1.774(11) . Y B207 H207 1.09 . ? B208 B212 1.749(13) . Y B208 B209 1.769(14) . Y B208 H208 1.09 . ? B209 B210 1.768(12) . Y B209 B212 1.780(14) . Y B209 H209 1.09 . ? B210 B211 1.734(11) . Y B210 B212 1.762(12) . Y B210 H210 1.09 . ? B211 B212 1.758(12) . Y B211 H211 1.09 . ? B212 H212 1.09 . ? C213 C218 1.376(9) . Y C213 C214 1.394(8) . Y C214 C215 1.346(9) . Y C214 H214 0.93 . ? C215 C216 1.386(9) . Y C215 H215 0.93 . ? C216 C217 1.350(9) . Y C216 H216 0.93 . ? C217 C218 1.398(10) . Y C217 H217 0.93 . ? C218 H218 0.93 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 P1 N14 110.8(3) . . Y O1 P1 N17 116.9(3) . . Y N14 P1 N17 104.9(4) . . Y O1 P1 N11 110.2(3) . . Y N14 P1 N11 108.9(4) . . Y N17 P1 N11 104.7(4) . . Y C13 N11 C12 111.0(9) . . Y C13 N11 P1 125.4(7) . . Y C12 N11 P1 123.6(7) . . Y N11 C12 H121 109.5 . . ? N11 C12 H122 109.5 . . ? H121 C12 H122 109.5 . . ? N11 C12 H123 109.5 . . ? H121 C12 H123 109.5 . . ? H122 C12 H123 109.5 . . ? N11 C13 H131 109.5 . . ? N11 C13 H132 109.5 . . ? H131 C13 H132 109.5 . . ? N11 C13 H133 109.5 . . ? H131 C13 H133 109.5 . . ? H132 C13 H133 109.5 . . ? C16 N14 C15 113.0(7) . . Y C16 N14 P1 124.1(7) . . Y C15 N14 P1 122.4(7) . . Y N14 C15 H151 109.5 . . ? N14 C15 H152 109.5 . . ? H151 C15 H152 109.5 . . ? N14 C15 H153 109.5 . . ? H151 C15 H153 109.5 . . ? H152 C15 H153 109.5 . . ? N14 C16 H161 109.5 . . ? N14 C16 H162 109.5 . . ? H161 C16 H162 109.5 . . ? N14 C16 H163 109.5 . . ? H161 C16 H163 109.5 . . ? H162 C16 H163 109.5 . . ? C18 N17 C19 112.1(9) . . Y C18 N17 P1 124.7(7) . . Y C19 N17 P1 114.1(7) . . Y N17 C18 H181 109.5 . . ? N17 C18 H182 109.5 . . ? H181 C18 H182 109.5 . . ? N17 C18 H183 109.5 . . ? H181 C18 H183 109.5 . . ? H182 C18 H183 109.5 . . ? N17 C19 H191 109.5 . . ? N17 C19 H192 109.5 . . ? H191 C19 H192 109.5 . . ? N17 C19 H193 109.5 . . ? H191 C19 H193 109.5 . . ? H192 C19 H193 109.5 . . ? O2 P2 N27 118.6(3) . . Y O2 P2 N24 110.0(3) . . Y N27 P2 N24 103.8(3) . . Y O2 P2 N21 109.6(3) . . Y N27 P2 N21 103.0(3) . . Y N24 P2 N21 111.7(3) . . Y C22 N21 C23 112.1(7) . . Y C22 N21 P2 121.8(6) . . Y C23 N21 P2 124.0(5) . . Y N21 C22 H221 109.5 . . ? N21 C22 H222 109.5 . . ? H221 C22 H222 109.5 . . ? N21 C22 H223 109.5 . . ? H221 C22 H223 109.5 . . ? H222 C22 H223 109.5 . . ? N21 C23 H231 109.5 . . ? N21 C23 H232 109.5 . . ? H231 C23 H232 109.5 . . ? N21 C23 H233 109.5 . . ? H231 C23 H233 109.5 . . ? H232 C23 H233 109.5 . . ? C26 N24 C25 112.9(7) . . Y C26 N24 P2 121.0(6) . . Y C25 N24 P2 124.1(6) . . Y N24 C25 H251 109.5 . . ? N24 C25 H252 109.5 . . ? H251 C25 H252 109.5 . . ? N24 C25 H253 109.5 . . ? H251 C25 H253 109.5 . . ? H252 C25 H253 109.5 . . ? N24 C26 H261 109.5 . . ? N24 C26 H262 109.5 . . ? H261 C26 H262 109.5 . . ? N24 C26 H263 109.5 . . ? H261 C26 H263 109.5 . . ? H262 C26 H263 109.5 . . ? C29 N27 C28 111.3(6) . . Y C29 N27 P2 119.7(5) . . Y C28 N27 P2 121.0(5) . . Y N27 C28 H281 109.5 . . ? N27 C28 H282 109.5 . . ? H281 C28 H282 109.5 . . ? N27 C28 H283 109.5 . . ? H281 C28 H283 109.5 . . ? H282 C28 H283 109.5 . . ? N27 C29 H291 109.5 . . ? N27 C29 H292 109.5 . . ? H291 C29 H292 109.5 . . ? N27 C29 H293 109.5 . . ? H291 C29 H293 109.5 . . ? H292 C29 H293 109.5 . . ? C101 N1 H1A 111.7(49) . . ? C101 N1 H1B 119.2(43) . . ? H1A N1 H1B 117.9(65) . . ? N1 C101 B104 128.3(6) . . Y N1 C101 B105 125.4(5) . . Y B104 C101 B105 64.5(5) . . Y N1 C101 B103 117.6(5) . . Y B104 C101 B103 62.4(4) . . Y B105 C101 B103 113.9(6) . . Y N1 C101 B106 116.3(6) . . Y B104 C101 B106 111.8(6) . . Y B105 C101 B106 61.9(4) . . Y B103 C101 B106 106.7(5) . . Y N1 C101 C102 114.9(5) . . Y B104 C101 C102 106.3(5) . . Y B105 C101 C102 107.2(5) . . Y B103 C101 C102 57.0(3) . . Y B106 C101 C102 57.1(3) . . Y C113 C102 B107 122.2(5) . . Y C113 C102 B111 122.6(5) . . Y B107 C102 B111 63.5(4) . . Y C113 C102 B103 117.3(5) . . Y B107 C102 B103 63.3(4) . . Y B111 C102 B103 114.1(5) . . Y C113 C102 B106 118.9(5) . . Y B107 C102 B106 113.4(5) . . Y B111 C102 B106 63.1(4) . . Y B103 C102 B106 108.4(5) . . Y C113 C102 C101 118.4(5) . . Y B107 C102 C101 108.6(5) . . Y B111 C102 C101 109.4(5) . . Y B103 C102 C101 57.6(4) . . Y B106 C102 C101 58.5(3) . . Y C102 B103 C101 65.3(4) . . Y C102 B103 B104 108.7(5) . . Y C101 B103 B104 57.1(4) . . Y C102 B103 B108 105.2(5) . . Y C101 B103 B108 104.5(5) . . Y B104 B103 B108 58.3(5) . . Y C102 B103 B107 57.6(4) . . Y C101 B103 B107 110.2(5) . . Y B104 B103 B107 107.8(5) . . Y B108 B103 B107 60.2(5) . . Y C102 B103 H103 121.0 . . ? C101 B103 H103 120.9 . . ? B104 B103 H103 122.8 . . ? B108 B103 H103 124.6 . . ? B107 B103 H103 121.3 . . ? C101 B104 B108 109.6(6) . . Y C101 B104 B103 60.5(4) . . Y B108 B104 B103 61.2(5) . . Y C101 B104 B109 107.5(6) . . Y B108 B104 B109 60.4(5) . . Y B103 B104 B109 108.7(6) . . Y C101 B104 B105 58.3(4) . . Y B108 B104 B105 109.4(6) . . Y B103 B104 B105 107.6(6) . . Y B109 B104 B105 60.7(4) . . Y C101 B104 H104 122.0 . . ? B108 B104 H104 120.1 . . ? B103 B104 H104 121.2 . . ? B109 B104 H104 121.5 . . ? B105 B104 H104 122.0 . . ? C101 B105 B106 61.0(4) . . Y C101 B105 B104 57.2(4) . . Y B106 B105 B104 105.4(5) . . Y C101 B105 B110 107.3(6) . . Y B106 B105 B110 59.1(5) . . Y B104 B105 B110 105.8(6) . . Y C101 B105 B109 105.5(5) . . Y B106 B105 B109 106.0(6) . . Y B104 B105 B109 59.4(4) . . Y B110 B105 B109 59.1(5) . . Y C101 B105 H105 122.6 . . ? B106 B105 H105 122.5 . . ? B104 B105 H105 123.8 . . ? B110 B105 H105 122.5 . . ? B109 B105 H105 123.0 . . ? C102 B106 C101 64.4(3) . . Y C102 B106 B110 105.1(5) . . Y C101 B106 B110 105.8(5) . . Y C102 B106 B105 109.3(5) . . Y C101 B106 B105 57.1(4) . . Y B110 B106 B105 61.1(5) . . Y C102 B106 B111 57.4(4) . . Y C101 B106 B111 109.5(5) . . Y B110 B106 B111 59.8(4) . . Y B105 B106 B111 110.0(6) . . Y C102 B106 H106 121.7 . . ? C101 B106 H106 121.3 . . ? B110 B106 H106 123.5 . . ? B105 B106 H106 121.0 . . ? B111 B106 H106 121.3 . . ? C102 B107 B112 105.5(5) . . Y C102 B107 B111 58.3(4) . . Y B112 B107 B111 60.3(4) . . Y C102 B107 B108 105.9(5) . . Y B112 B107 B108 59.5(5) . . Y B111 B107 B108 107.7(6) . . Y C102 B107 B103 59.2(4) . . Y B112 B107 B103 106.7(6) . . Y B111 B107 B103 106.7(5) . . Y B108 B107 B103 59.5(5) . . Y C102 B107 H107 123.8 . . ? B112 B107 H107 122.5 . . ? B111 B107 H107 122.0 . . ? B108 B107 H107 122.2 . . ? B103 B107 H107 122.4 . . ? B104 B108 B109 61.6(5) . . Y B104 B108 B112 108.7(6) . . Y B109 B108 B112 59.2(5) . . Y B104 B108 B103 60.5(5) . . Y B109 B108 B103 109.1(6) . . Y B112 B108 B103 107.6(6) . . Y B104 B108 B107 109.6(6) . . Y B109 B108 B107 108.5(6) . . Y B112 B108 B107 60.0(5) . . Y B103 B108 B107 60.3(4) . . Y B104 B108 H108 120.3 . . ? B109 B108 H108 121.2 . . ? B112 B108 H108 122.3 . . ? B103 B108 H108 121.6 . . ? B107 B108 H108 121.1 . . ? B112 B109 B108 60.5(5) . . Y B112 B109 B110 60.1(5) . . Y B108 B109 B110 107.5(6) . . Y B112 B109 B104 107.0(6) . . Y B108 B109 B104 58.0(5) . . Y B110 B109 B104 107.1(6) . . Y B112 B109 B105 108.6(6) . . Y B108 B109 B105 106.8(6) . . Y B110 B109 B105 60.2(5) . . Y B104 B109 B105 59.9(5) . . Y B112 B109 H109 121.3 . . ? B108 B109 H109 122.6 . . ? B110 B109 H109 121.8 . . ? B104 B109 H109 123.0 . . ? B105 B109 H109 121.6 . . ? B106 B110 B112 107.9(5) . . Y B106 B110 B111 60.9(4) . . Y B112 B110 B111 60.7(4) . . Y B106 B110 B109 107.7(5) . . Y B112 B110 B109 59.0(5) . . Y B111 B110 B109 108.7(5) . . Y B106 B110 B105 59.7(4) . . Y B112 B110 B105 108.0(5) . . Y B111 B110 B105 109.7(5) . . Y B109 B110 B105 60.7(5) . . Y B106 B110 H110 121.9 . . ? B112 B110 H110 122.1 . . ? B111 B110 H110 120.4 . . ? B109 B110 H110 121.9 . . ? B105 B110 H110 121.1 . . ? C102 B111 B110 106.4(5) . . Y C102 B111 B107 58.2(4) . . Y B110 B111 B107 107.6(6) . . Y C102 B111 B112 104.9(5) . . Y B110 B111 B112 59.4(5) . . Y B107 B111 B112 59.8(4) . . Y C102 B111 B106 59.5(4) . . Y B110 B111 B106 59.3(4) . . Y B107 B111 B106 106.3(5) . . Y B112 B111 B106 105.7(6) . . Y C102 B111 H111 123.5 . . ? B110 B111 H111 122.0 . . ? B107 B111 H111 122.3 . . ? B112 B111 H111 123.2 . . ? B106 B111 H111 122.8 . . ? B109 B112 B110 60.9(5) . . Y B109 B112 B108 60.3(5) . . Y B110 B112 B108 107.9(6) . . Y B109 B112 B107 109.7(6) . . Y B110 B112 B107 108.0(6) . . Y B108 B112 B107 60.5(5) . . Y B109 B112 B111 109.6(6) . . Y B110 B112 B111 59.9(4) . . Y B108 B112 B111 108.1(6) . . Y B107 B112 B111 59.9(4) . . Y B109 B112 H112 120.2 . . ? B110 B112 H112 121.8 . . ? B108 B112 H112 121.8 . . ? B107 B112 H112 121.2 . . ? B111 B112 H112 121.5 . . ? C118 C113 C114 117.3(6) . . Y C118 C113 C102 119.9(6) . . Y C114 C113 C102 122.8(6) . . Y C115 C114 C113 121.7(6) . . Y C115 C114 H114 119.1 . . ? C113 C114 H114 119.1 . . ? C116 C115 C114 120.5(7) . . Y C116 C115 H115 119.7 . . ? C114 C115 H115 119.7 . . ? C117 C116 C115 118.6(7) . . Y C117 C116 H116 120.7 . . ? C115 C116 H116 120.7 . . ? C116 C117 C118 121.8(7) . . Y C116 C117 H117 119.1 . . ? C118 C117 H117 119.1 . . ? C113 C118 C117 120.0(6) . . Y C113 C118 H118 120.0 . . ? C117 C118 H118 120.0 . . ? C201 N2 H2A 118.9(42) . . ? C201 N2 H2B 126.2(41) . . ? H2A N2 H2B 107.3(60) . . ? N2 C201 B205 127.1(5) . . Y N2 C201 B204 125.7(6) . . Y B205 C201 B204 63.5(5) . . Y N2 C201 B203 116.7(6) . . Y B205 C201 B203 112.1(6) . . Y B204 C201 B203 62.3(4) . . Y N2 C201 B206 118.3(5) . . Y B205 C201 B206 61.7(4) . . Y B204 C201 B206 112.1(6) . . Y B203 C201 B206 107.0(5) . . Y N2 C201 C202 116.1(6) . . Y B205 C201 C202 106.1(5) . . Y B204 C201 C202 106.9(5) . . Y B203 C201 C202 57.7(4) . . Y B206 C201 C202 57.0(4) . . Y C213 C202 B211 121.2(5) . . Y C213 C202 B207 125.0(5) . . Y B211 C202 B207 63.7(4) . . Y C213 C202 B206 115.1(5) . . Y B211 C202 B206 62.9(4) . . Y B207 C202 B206 113.6(5) . . Y C213 C202 B203 119.7(5) . . Y B211 C202 B203 114.4(6) . . Y B207 C202 B203 63.3(4) . . Y B206 C202 B203 109.1(5) . . Y C213 C202 C201 116.8(5) . . Y B211 C202 C201 109.8(5) . . Y B207 C202 C201 109.3(5) . . Y B206 C202 C201 58.8(4) . . Y B203 C202 C201 58.3(4) . . Y C202 B203 C201 64.1(3) . . Y C202 B203 B204 109.0(5) . . Y C201 B203 B204 58.5(4) . . Y C202 B203 B207 57.8(4) . . Y C201 B203 B207 109.6(5) . . Y B204 B203 B207 108.0(6) . . Y C202 B203 B208 104.7(6) . . Y C201 B203 B208 105.2(6) . . Y B204 B203 B208 58.7(5) . . Y B207 B203 B208 59.5(5) . . Y C202 B203 H203 121.5 . . ? C201 B203 H203 120.8 . . ? B204 B203 H203 122.0 . . ? B207 B203 H203 121.7 . . ? B208 B203 H203 124.6 . . ? C201 B204 B208 107.6(6) . . Y C201 B204 B209 105.1(6) . . Y B208 B204 B209 60.8(6) . . Y C201 B204 B203 59.2(4) . . Y B208 B204 B203 61.0(5) . . Y B209 B204 B203 108.0(6) . . Y C201 B204 B205 57.9(4) . . Y B208 B204 B205 106.6(7) . . Y B209 B204 B205 58.0(5) . . Y B203 B204 B205 105.4(5) . . Y C201 B204 H204 123.4 . . ? B208 B204 H204 121.0 . . ? B209 B204 H204 122.5 . . ? B203 B204 H204 121.9 . . ? B205 B204 H204 124.1 . . ? C201 B205 B209 107.2(6) . . Y C201 B205 B210 107.6(6) . . Y B209 B205 B210 61.3(5) . . Y C201 B205 B206 60.0(4) . . Y B209 B205 B206 108.4(7) . . Y B210 B205 B206 59.5(5) . . Y C201 B205 B204 58.5(4) . . Y B209 B205 B204 60.0(5) . . Y B210 B205 B204 108.4(6) . . Y B206 B205 B204 106.9(5) . . Y C201 B205 H205 122.6 . . ? B209 B205 H205 121.2 . . ? B210 B205 H205 121.2 . . ? B206 B205 H205 122.1 . . ? B204 B205 H205 122.4 . . ? C202 B206 C201 64.2(4) . . Y C202 B206 B210 105.4(5) . . Y C201 B206 B210 106.6(6) . . Y C202 B206 B205 109.0(5) . . Y C201 B206 B205 58.3(4) . . Y B210 B206 B205 60.0(5) . . Y C202 B206 B211 58.1(4) . . Y C201 B206 B211 110.2(5) . . Y B210 B206 B211 59.5(5) . . Y B205 B206 B211 108.7(5) . . Y C202 B206 H206 121.5 . . ? C201 B206 H206 120.4 . . ? B210 B206 H206 123.7 . . ? B205 B206 H206 121.7 . . ? B211 B206 H206 121.4 . . ? C202 B207 B212 105.2(5) . . Y C202 B207 B208 106.1(6) . . Y B212 B207 B208 59.8(5) . . Y C202 B207 B211 57.8(4) . . Y B212 B207 B211 60.1(5) . . Y B208 B207 B211 107.6(6) . . Y C202 B207 B203 58.9(4) . . Y B212 B207 B203 107.4(6) . . Y B208 B207 B203 60.3(5) . . Y B211 B207 B203 106.3(5) . . Y C202 B207 H207 124.1 . . ? B212 B207 H207 122.4 . . ? B208 B207 H207 121.8 . . ? B211 B207 H207 122.5 . . ? B203 B207 H207 122.2 . . ? B204 B208 B212 109.4(6) . . Y B204 B208 B207 110.0(6) . . Y B212 B208 B207 59.3(5) . . Y B204 B208 B209 60.1(5) . . Y B212 B208 B209 60.8(5) . . Y B207 B208 B209 108.3(6) . . Y B204 B208 B203 60.4(5) . . Y B212 B208 B203 106.8(6) . . Y B207 B208 B203 60.2(5) . . Y B209 B208 B203 107.0(6) . . Y B204 B208 H208 120.3 . . ? B212 B208 H208 121.8 . . ? B207 B208 H208 121.1 . . ? B209 B208 H208 121.8 . . ? B203 B208 H208 122.6 . . ? B205 B209 B204 61.9(5) . . Y B205 B209 B210 60.0(5) . . Y B204 B209 B210 108.9(6) . . Y B205 B209 B208 108.3(7) . . Y B204 B209 B208 59.1(5) . . Y B210 B209 B208 106.7(7) . . Y B205 B209 B212 108.0(6) . . Y B204 B209 B212 107.2(7) . . Y B210 B209 B212 59.6(5) . . Y B208 B209 B212 59.1(6) . . Y B205 B209 H209 120.7 . . ? B204 B209 H209 121.2 . . ? B210 B209 H209 122.0 . . ? B208 B209 H209 122.8 . . ? B212 B209 H209 122.5 . . ? B211 B210 B206 60.9(4) . . Y B211 B210 B205 110.3(5) . . Y B206 B210 B205 60.5(4) . . Y B211 B210 B212 60.4(5) . . Y B206 B210 B212 107.7(6) . . Y B205 B210 B212 107.8(6) . . Y B211 B210 B209 109.6(6) . . Y B206 B210 B209 107.1(6) . . Y B205 B210 B209 58.7(5) . . Y B212 B210 B209 60.6(5) . . Y B211 B210 H210 119.9 . . ? B206 B210 H210 122.0 . . ? B205 B210 H210 121.4 . . ? B212 B210 H210 121.9 . . ? B209 B210 H210 122.0 . . ? C202 B211 B210 106.2(5) . . Y C202 B211 B206 59.0(4) . . Y B210 B211 B206 59.6(4) . . Y C202 B211 B212 104.8(5) . . Y B210 B211 B212 60.6(5) . . Y B206 B211 B212 106.9(6) . . Y C202 B211 B207 58.5(4) . . Y B210 B211 B207 107.7(6) . . Y B206 B211 B207 106.4(5) . . Y B212 B211 B207 59.0(5) . . Y C202 B211 H211 123.8 . . ? B210 B211 H211 121.6 . . ? B206 B211 H211 122.5 . . ? B212 B211 H211 122.8 . . ? B207 B211 H211 122.6 . . ? B207 B212 B208 60.9(5) . . Y B207 B212 B211 61.0(5) . . Y B208 B212 B211 109.2(7) . . Y B207 B212 B210 108.0(6) . . Y B208 B212 B210 107.8(7) . . Y B211 B212 B210 59.0(4) . . Y B207 B212 B209 109.2(7) . . Y B208 B212 B209 60.2(6) . . Y B211 B212 B209 108.0(6) . . Y B210 B212 B209 59.9(5) . . Y B207 B212 H212 120.7 . . ? B208 B212 H212 121.1 . . ? B211 B212 H212 121.5 . . ? B210 B212 H212 122.5 . . ? B209 B212 H212 121.5 . . ? C218 C213 C214 116.6(7) . . Y C218 C213 C202 122.8(6) . . Y C214 C213 C202 120.5(6) . . Y C215 C214 C213 122.0(7) . . Y C215 C214 H214 119.0 . . ? C213 C214 H214 119.0 . . ? C214 C215 C216 120.7(7) . . Y C214 C215 H215 119.6 . . ? C216 C215 H215 119.6 . . ? C217 C216 C215 119.1(8) . . Y C217 C216 H216 120.5 . . ? C215 C216 H216 120.5 . . ? C216 C217 C218 120.1(8) . . Y C216 C217 H217 119.9 . . ? C218 C217 H217 119.9 . . ? C213 C218 C217 121.4(7) . . Y C213 C218 H218 119.3 . . ? C217 C218 H218 119.3 . . ? _refine_diff_density_max 0.163 _refine_diff_density_min -0.160 _refine_diff_density_rms 0.032 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 237442' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H30 B20 S3' _chemical_formula_sum 'C16 H30 B20 S3' _chemical_formula_weight 534.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 8.0923(3) _cell_length_b 14.8660(7) _cell_length_c 24.1238(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2902.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 32 _cell_measurement_theta_min 23.34 _cell_measurement_theta_max 29.60 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.224 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 2.370 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.40 _exptl_absorpt_correction_T_max 0.56 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe-Siemens diffractometer' _diffrn_measurement_method '\w/\q scans with on-line profile fitting' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _diffrn_reflns_number 6796 _diffrn_reflns_av_R_equivalents 0.0173 _diffrn_reflns_av_sigmaI/netI 0.0281 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.49 _diffrn_reflns_theta_max 64.97 _reflns_number_total 4793 _reflns_number_gt 4351 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'local programs' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0431P)^2^+0.7250P] 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 0.00155(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.012(16) _refine_ls_number_reflns 4793 _refine_ls_number_parameters 353 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0386 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0903 _refine_ls_wR_factor_gt 0.0837 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9249(3) 0.85725(15) 0.24548(9) 0.0434(6) Uani 1 1 d . . . C2 C 0.9244(3) 0.74132(15) 0.23858(9) 0.0409(5) Uani 1 1 d . . . B3 B 0.8783(5) 0.81097(19) 0.18246(11) 0.0521(8) Uani 1 1 d . . . H3 H 0.7549 0.8145 0.1635 0.062 Uiso 1 1 calc R . . B4 B 1.0087(5) 0.9072(2) 0.18833(13) 0.0653(10) Uani 1 1 d . . . H4 H 0.9719 0.9733 0.1720 0.078 Uiso 1 1 calc R . . B5 B 1.1204(4) 0.8967(2) 0.25120(13) 0.0582(8) Uani 1 1 d . . . H5 H 1.1554 0.9560 0.2758 0.070 Uiso 1 1 calc R . . B6 B 1.0623(4) 0.79331(19) 0.28344(12) 0.0470(6) Uani 1 1 d . . . H6 H 1.0571 0.7858 0.3288 0.056 Uiso 1 1 calc R . . B7 B 1.0082(4) 0.7151(2) 0.17607(12) 0.0526(8) Uani 1 1 d . . . H7 H 0.9706 0.6564 0.1514 0.063 Uiso 1 1 calc R . . B8 B 1.0639(6) 0.8181(2) 0.14402(14) 0.0701(11) Uani 1 1 d . . . H8 H 1.0631 0.8262 0.0987 0.084 Uiso 1 1 calc R . . B9 B 1.2155(6) 0.8702(2) 0.18701(16) 0.0766(12) Uani 1 1 d . . . H9 H 1.3151 0.9119 0.1696 0.092 Uiso 1 1 calc R . . B10 B 1.2486(5) 0.8005(2) 0.24599(16) 0.0668(9) Uani 1 1 d . . . H10 H 1.3690 0.7974 0.2671 0.080 Uiso 1 1 calc R . . B11 B 1.1218(4) 0.7033(2) 0.23890(13) 0.0513(7) Uani 1 1 d . . . H11 H 1.1585 0.6372 0.2553 0.062 Uiso 1 1 calc R . . B12 B 1.2157(5) 0.7513(2) 0.17914(15) 0.0661(10) Uani 1 1 d . . . H12 H 1.3146 0.7162 0.1566 0.079 Uiso 1 1 calc R . . C13 C 0.7828(3) 0.68850(14) 0.26193(9) 0.0421(5) Uani 1 1 d . . . C14 C 0.7644(4) 0.67363(17) 0.31821(10) 0.0553(7) Uani 1 1 d . . . H14 H 0.8412 0.6972 0.3429 0.066 Uiso 1 1 calc R . . C15 C 0.6329(4) 0.62401(19) 0.33786(13) 0.0667(8) Uani 1 1 d . . . H15 H 0.6209 0.6148 0.3758 0.080 Uiso 1 1 calc R . . C16 C 0.5198(4) 0.5882(2) 0.30186(14) 0.0690(8) Uani 1 1 d . . . H16 H 0.4316 0.5547 0.3154 0.083 Uiso 1 1 calc R . . C17 C 0.5362(4) 0.6017(2) 0.24628(14) 0.0665(8) Uani 1 1 d . . . H17 H 0.4591 0.5774 0.2219 0.080 Uiso 1 1 calc R . . C18 C 0.6671(4) 0.65137(17) 0.22609(11) 0.0552(6) Uani 1 1 d . . . H18 H 0.6779 0.6601 0.1881 0.066 Uiso 1 1 calc R . . S19 S 0.74514(8) 0.90532(4) 0.27690(2) 0.04843(16) Uani 1 1 d . . . C1' C 0.5996(3) 0.91664(16) 0.43585(9) 0.0431(5) Uani 1 1 d . . . C2' C 0.5688(3) 0.99656(15) 0.48747(9) 0.0404(5) Uani 1 1 d . . . B3' B 0.4920(4) 1.0131(2) 0.42145(11) 0.0480(7) Uani 1 1 d . . . H3' H 0.5385 1.0661 0.3937 0.058 Uiso 1 1 calc R . . B4' B 0.4284(4) 0.9065(2) 0.39586(12) 0.0516(7) Uani 1 1 d . . . H4' H 0.4308 0.8908 0.3513 0.062 Uiso 1 1 calc R . . B5' B 0.4775(4) 0.8244(2) 0.44677(13) 0.0526(7) Uani 1 1 d . . . H5' H 0.5110 0.7551 0.4354 0.063 Uiso 1 1 calc R . . B6' B 0.5739(4) 0.88207(19) 0.50317(11) 0.0465(7) Uani 1 1 d . . . H6' H 0.6730 0.8510 0.5278 0.056 Uiso 1 1 calc R . . B7' B 0.3727(4) 1.0376(2) 0.48200(12) 0.0530(7) Uani 1 1 d . . . H7' H 0.3378 1.1067 0.4932 0.064 Uiso 1 1 calc R . . B8' B 0.2814(4) 0.9814(2) 0.42492(13) 0.0580(8) Uani 1 1 d . . . H8' H 0.1869 1.0142 0.3991 0.070 Uiso 1 1 calc R . . B9' B 0.2728(4) 0.8645(2) 0.44097(13) 0.0586(8) Uani 1 1 d . . . H9' H 0.1721 0.8213 0.4259 0.070 Uiso 1 1 calc R . . B10' B 0.3651(4) 0.8495(2) 0.50765(13) 0.0557(8) Uani 1 1 d . . . H10' H 0.3255 0.7959 0.5362 0.067 Uiso 1 1 calc R . . B11' B 0.4245(4) 0.9563(2) 0.53273(12) 0.0506(7) Uani 1 1 d . . . H11' H 0.4241 0.9723 0.5772 0.061 Uiso 1 1 calc R . . B12' B 0.2403(4) 0.9451(2) 0.49433(14) 0.0599(8) Uani 1 1 d . . . H12' H 0.1183 0.9537 0.5138 0.072 Uiso 1 1 calc R . . C13' C 0.7131(3) 1.05119(15) 0.50694(9) 0.0427(6) Uani 1 1 d . . . C14' C 0.7795(5) 1.12002(19) 0.47560(12) 0.0717(9) Uani 1 1 d . . . H14' H 0.7347 1.1332 0.4410 0.086 Uiso 1 1 calc R . . C15' C 0.9121(5) 1.1697(2) 0.49505(16) 0.0893(12) Uani 1 1 d . . . H15' H 0.9579 1.2145 0.4730 0.107 Uiso 1 1 calc R . . C16' C 0.9758(5) 1.1534(2) 0.54619(13) 0.0723(9) Uani 1 1 d . . . H16' H 1.0626 1.1881 0.5596 0.087 Uiso 1 1 calc R . . C17' C 0.9118(4) 1.0859(2) 0.57753(12) 0.0645(8) Uani 1 1 d . . . H17' H 0.9559 1.0741 0.6124 0.077 Uiso 1 1 calc R . . C18' C 0.7817(4) 1.03452(19) 0.55813(10) 0.0548(6) Uani 1 1 d . . . H18' H 0.7401 0.9882 0.5799 0.066 Uiso 1 1 calc R . . S19' S 0.80636(8) 0.89883(5) 0.41237(2) 0.05075(17) Uani 1 1 d . . . S20 S 0.83111(9) 0.97622(4) 0.34318(3) 0.05268(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0593(15) 0.0346(11) 0.0363(12) -0.0021(10) 0.0074(11) -0.0019(11) C2 0.0513(14) 0.0349(11) 0.0367(12) -0.0032(9) -0.0016(10) -0.0003(10) B3 0.080(2) 0.0425(15) 0.0334(13) -0.0001(11) 0.0044(14) 0.0015(15) B4 0.102(3) 0.0445(16) 0.0498(17) 0.0007(14) 0.0305(18) -0.0072(18) B5 0.0605(19) 0.0500(16) 0.0641(18) -0.0186(15) 0.0211(16) -0.0155(16) B6 0.0468(16) 0.0490(15) 0.0452(15) -0.0095(12) -0.0011(13) -0.0020(13) B7 0.073(2) 0.0448(16) 0.0402(15) -0.0111(12) 0.0088(15) 0.0000(15) B8 0.111(3) 0.0512(17) 0.0482(18) -0.0052(14) 0.0301(19) -0.004(2) B9 0.092(3) 0.0574(19) 0.080(2) -0.0187(17) 0.047(2) -0.023(2) B10 0.0527(18) 0.0662(19) 0.081(2) -0.0278(18) 0.0181(18) -0.0096(17) B11 0.0504(17) 0.0487(15) 0.0550(17) -0.0129(13) 0.0014(14) 0.0025(14) B12 0.073(3) 0.0582(18) 0.067(2) -0.0221(16) 0.0267(19) -0.0068(17) C13 0.0501(15) 0.0315(10) 0.0447(12) 0.0020(9) -0.0031(10) 0.0002(10) C14 0.0705(19) 0.0496(14) 0.0456(13) 0.0067(11) -0.0053(13) -0.0102(14) C15 0.082(2) 0.0604(16) 0.0576(16) 0.0156(14) 0.0086(16) -0.0136(16) C16 0.0639(19) 0.0519(16) 0.091(2) 0.0143(16) 0.0080(17) -0.0111(15) C17 0.0556(17) 0.0587(17) 0.085(2) 0.0004(16) -0.0099(15) -0.0150(15) C18 0.0628(17) 0.0518(14) 0.0511(14) -0.0009(12) -0.0081(14) -0.0064(14) S19 0.0566(4) 0.0475(3) 0.0413(3) -0.0028(2) 0.0028(3) 0.0087(3) C1' 0.0461(14) 0.0496(13) 0.0335(11) -0.0061(10) -0.0009(10) 0.0054(11) C2' 0.0464(13) 0.0420(13) 0.0326(11) -0.0025(9) 0.0023(10) 0.0066(10) B3' 0.0530(17) 0.0525(16) 0.0383(14) 0.0016(12) -0.0067(12) 0.0071(14) B4' 0.0442(15) 0.0690(19) 0.0416(14) -0.0082(14) -0.0072(12) 0.0040(16) B5' 0.0569(19) 0.0485(16) 0.0525(17) -0.0090(14) -0.0021(14) 0.0009(14) B6' 0.0578(17) 0.0443(14) 0.0374(14) 0.0021(11) -0.0012(13) 0.0031(13) B7' 0.0491(17) 0.0588(18) 0.0510(16) -0.0052(13) 0.0036(14) 0.0157(14) B8' 0.0498(18) 0.0710(19) 0.0531(17) -0.0004(15) -0.0066(14) 0.0116(16) B9' 0.0505(19) 0.0662(18) 0.0590(18) -0.0094(15) 0.0006(15) -0.0058(16) B10' 0.059(2) 0.0561(17) 0.0519(16) 0.0009(14) 0.0063(15) -0.0059(15) B11' 0.0557(18) 0.0563(17) 0.0398(14) -0.0025(13) 0.0071(14) -0.0007(14) B12' 0.0500(18) 0.0709(19) 0.0587(18) -0.0094(16) 0.0100(16) 0.0022(16) C13' 0.0493(15) 0.0409(11) 0.0380(11) -0.0038(9) 0.0003(11) 0.0027(10) C14' 0.100(3) 0.0557(15) 0.0595(16) 0.0120(13) -0.0228(17) -0.0204(17) C15' 0.112(3) 0.067(2) 0.088(2) 0.0171(18) -0.020(2) -0.039(2) C16' 0.074(2) 0.0687(19) 0.074(2) -0.0183(17) -0.0093(17) -0.0156(17) C17' 0.0630(18) 0.081(2) 0.0495(15) -0.0101(15) -0.0089(13) 0.0005(17) C18' 0.0573(16) 0.0660(16) 0.0411(12) 0.0034(12) -0.0052(12) -0.0076(13) S19' 0.0448(3) 0.0669(4) 0.0406(3) -0.0080(3) 0.0003(3) 0.0109(3) S20 0.0640(4) 0.0411(3) 0.0530(3) -0.0127(3) 0.0177(3) -0.0089(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 C1 C2 1.731(3) . ? C1 B3 1.711(3) . ? C1 B4 1.706(4) . ? C1 B5 1.693(4) . ? C1 B6 1.725(4) . ? C1 S19 1.789(3) . ? C2 B3 1.745(4) . ? C2 B6 1.736(4) . ? C2 B7 1.699(4) . ? C2 B11 1.694(4) . ? C2 C13 1.499(3) . ? B3 B4 1.783(5) . ? B3 B7 1.777(4) . ? B3 B8 1.768(5) . ? B4 B5 1.773(5) . ? B4 B8 1.759(4) . ? B4 B9 1.762(6) . ? B5 B6 1.785(4) . ? B5 B9 1.774(4) . ? B5 B10 1.771(5) . ? B6 B10 1.761(5) . ? B6 B11 1.783(4) . ? B7 B8 1.773(4) . ? B7 B11 1.781(5) . ? B7 B12 1.765(5) . ? B8 B9 1.784(6) . ? B8 B12 1.792(6) . ? B9 B10 1.781(6) . ? B9 B12 1.778(5) . ? B10 B11 1.781(5) . ? B10 B12 1.790(5) . ? B11 B12 1.779(5) . ? C13 C14 1.384(3) . ? C13 C18 1.389(3) . ? C14 C15 1.379(4) . ? C15 C16 1.369(4) . ? C16 C17 1.362(4) . ? C17 C18 1.380(4) . ? S19 S20 2.0375(9) . ? C1' C2' 1.739(3) . ? C1' B3' 1.713(4) . ? C1' B4' 1.696(4) . ? C1' B5' 1.711(4) . ? C1' B6' 1.716(3) . ? C1' S19' 1.786(2) . ? C2' B3' 1.727(3) . ? C2' B6' 1.744(3) . ? C2' B7' 1.706(4) . ? C2' B11' 1.708(4) . ? C2' C13' 1.498(3) . ? B3' B4' 1.777(4) . ? B3' B7' 1.788(4) . ? B3' B8' 1.770(5) . ? B4' B5' 1.777(4) . ? B4' B8' 1.774(4) . ? B4' B9' 1.778(5) . ? B5' B6' 1.788(4) . ? B5' B9' 1.766(5) . ? B5' B10' 1.767(4) . ? B6' B10' 1.762(5) . ? B6' B11' 1.786(4) . ? B7' B8' 1.772(4) . ? B7' B11' 1.770(4) . ? B7' B12' 1.768(5) . ? B8' B9' 1.782(5) . ? B8' B12' 1.790(5) . ? B9' B10' 1.787(5) . ? B9' B12' 1.779(4) . ? B10' B11' 1.765(4) . ? B10' B12' 1.773(5) . ? B11' B12' 1.763(5) . ? C13' C14' 1.381(4) . ? C13' C18' 1.376(3) . ? C14' C15' 1.384(5) . ? C15' C16' 1.359(5) . ? C16' C17' 1.359(4) . ? C17' C18' 1.382(4) . ? S19' S20 2.0371(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 B3 60.91(14) . . ? C2 C1 B4 110.86(18) . . ? C2 C1 B5 110.8(2) . . ? C2 C1 B6 60.28(14) . . ? C2 C1 S19 115.87(17) . . ? B3 C1 B4 62.90(18) . . ? B3 C1 B5 114.7(2) . . ? B3 C1 B6 113.09(19) . . ? B3 C1 S19 110.96(19) . . ? B4 C1 B5 62.9(2) . . ? B4 C1 B6 114.4(2) . . ? B4 C1 S19 119.44(19) . . ? B5 C1 B6 62.96(18) . . ? B5 C1 S19 125.95(17) . . ? B6 C1 S19 121.26(16) . . ? C1 C2 B3 58.96(14) . . ? C1 C2 B6 59.69(15) . . ? C1 C2 B7 108.22(18) . . ? C1 C2 B11 109.2(2) . . ? C1 C2 C13 119.1(2) . . ? B3 C2 B6 110.92(19) . . ? B3 C2 B7 62.13(17) . . ? B3 C2 B11 113.8(2) . . ? B3 C2 C13 116.0(2) . . ? B6 C2 B7 113.5(2) . . ? B6 C2 B11 62.62(16) . . ? B6 C2 C13 119.35(19) . . ? B7 C2 B11 63.34(18) . . ? B7 C2 C13 121.2(2) . . ? B11 C2 C13 123.0(2) . . ? C1 B3 C2 60.13(14) . . ? C1 B3 B4 58.43(16) . . ? C1 B3 B7 105.6(2) . . ? C1 B3 B8 104.7(2) . . ? C2 B3 B4 106.7(2) . . ? C2 B3 B7 57.66(15) . . ? C2 B3 B8 105.1(2) . . ? B4 B3 B7 107.4(3) . . ? B4 B3 B8 59.39(19) . . ? B7 B3 B8 60.02(19) . . ? C1 B4 B3 58.68(15) . . ? C1 B4 B5 58.19(17) . . ? C1 B4 B8 105.3(2) . . ? C1 B4 B9 104.9(3) . . ? B3 B4 B5 107.4(2) . . ? B3 B4 B8 59.9(2) . . ? B3 B4 B9 108.1(2) . . ? B5 B4 B8 108.9(3) . . ? B5 B4 B9 60.2(2) . . ? B8 B4 B9 60.9(2) . . ? C1 B5 B4 58.94(17) . . ? C1 B5 B6 59.41(16) . . ? C1 B5 B9 104.9(2) . . ? C1 B5 B10 105.2(2) . . ? B4 B5 B6 108.3(2) . . ? B4 B5 B9 59.6(2) . . ? B4 B5 B10 108.0(2) . . ? B6 B5 B9 107.7(2) . . ? B6 B5 B10 59.37(19) . . ? B9 B5 B10 60.3(2) . . ? C1 B6 C2 60.03(14) . . ? C1 B6 B5 57.62(17) . . ? C1 B6 B10 104.2(2) . . ? C1 B6 B11 105.5(2) . . ? C2 B6 B5 106.3(2) . . ? C2 B6 B10 104.9(2) . . ? C2 B6 B11 57.56(16) . . ? B5 B6 B10 59.92(19) . . ? B5 B6 B11 108.2(2) . . ? B10 B6 B11 60.32(17) . . ? C2 B7 B3 60.21(15) . . ? C2 B7 B8 106.9(2) . . ? C2 B7 B11 58.22(16) . . ? C2 B7 B12 105.8(2) . . ? B3 B7 B8 59.74(19) . . ? B3 B7 B11 108.1(2) . . ? B3 B7 B12 108.3(2) . . ? B8 B7 B11 109.0(2) . . ? B8 B7 B12 60.9(2) . . ? B11 B7 B12 60.2(2) . . ? B3 B8 B4 60.72(19) . . ? B3 B8 B7 60.25(18) . . ? B3 B8 B9 107.8(2) . . ? B3 B8 B12 107.5(2) . . ? B4 B8 B7 108.7(2) . . ? B4 B8 B9 59.6(2) . . ? B4 B8 B12 107.7(3) . . ? B7 B8 B9 107.2(3) . . ? B7 B8 B12 59.3(2) . . ? B9 B8 B12 59.6(2) . . ? B4 B9 B5 60.2(2) . . ? B4 B9 B8 59.5(2) . . ? B4 B9 B10 108.0(2) . . ? B4 B9 B12 108.2(3) . . ? B5 B9 B8 107.8(3) . . ? B5 B9 B10 59.8(2) . . ? B5 B9 B12 108.3(2) . . ? B8 B9 B10 108.3(2) . . ? B8 B9 B12 60.4(2) . . ? B10 B9 B12 60.4(2) . . ? B5 B10 B6 60.71(18) . . ? B5 B10 B9 59.9(2) . . ? B5 B10 B11 108.9(2) . . ? B5 B10 B12 107.8(3) . . ? B6 B10 B9 108.4(3) . . ? B6 B10 B11 60.44(18) . . ? B6 B10 B12 108.1(3) . . ? B9 B10 B11 108.0(3) . . ? B9 B10 B12 59.7(2) . . ? B11 B10 B12 59.78(18) . . ? C2 B11 B6 59.83(16) . . ? C2 B11 B7 58.44(16) . . ? C2 B11 B10 105.8(2) . . ? C2 B11 B12 105.4(2) . . ? B6 B11 B7 107.4(2) . . ? B6 B11 B10 59.24(17) . . ? B6 B11 B12 107.6(2) . . ? B7 B11 B10 107.4(2) . . ? B7 B11 B12 59.42(19) . . ? B10 B11 B12 60.39(19) . . ? B7 B12 B8 59.8(2) . . ? B7 B12 B9 107.9(3) . . ? B7 B12 B10 107.7(2) . . ? B7 B12 B11 60.35(18) . . ? B8 B12 B9 59.9(2) . . ? B8 B12 B10 107.6(2) . . ? B8 B12 B11 108.2(3) . . ? B9 B12 B10 59.9(2) . . ? B9 B12 B11 108.2(2) . . ? B10 B12 B11 59.84(18) . . ? C2 C13 C14 122.3(2) . . ? C2 C13 C18 119.3(2) . . ? C14 C13 C18 118.3(2) . . ? C13 C14 C15 120.4(3) . . ? C14 C15 C16 120.4(3) . . ? C15 C16 C17 120.2(3) . . ? C16 C17 C18 120.1(3) . . ? C13 C18 C17 120.7(3) . . ? C1 S19 S20 105.15(9) . . ? C2' C1' B3' 60.04(14) . . ? C2' C1' B4' 110.55(19) . . ? C2' C1' B5' 110.76(18) . . ? C2' C1' B6' 60.63(14) . . ? C2' C1' S19' 117.56(16) . . ? B3' C1' B4' 62.82(17) . . ? B3' C1' B5' 114.1(2) . . ? B3' C1' B6' 112.38(19) . . ? B3' C1' S19' 122.42(18) . . ? B4' C1' B5' 62.88(18) . . ? B4' C1' B6' 114.4(2) . . ? B4' C1' S19' 124.90(16) . . ? B5' C1' B6' 62.88(16) . . ? B5' C1' S19' 118.12(17) . . ? B6' C1' S19' 111.67(17) . . ? C1' C2' B3' 59.24(14) . . ? C1' C2' B6' 59.03(14) . . ? C1' C2' B7' 108.80(18) . . ? C1' C2' B11' 108.44(18) . . ? C1' C2' C13' 118.90(19) . . ? B3' C2' B6' 110.33(19) . . ? B3' C2' B7' 62.78(16) . . ? B3' C2' B11' 113.1(2) . . ? B3' C2' C13' 119.5(2) . . ? B6' C2' B7' 112.8(2) . . ? B6' C2' B11' 62.30(16) . . ? B6' C2' C13' 116.3(2) . . ? B7' C2' B11' 62.48(17) . . ? B7' C2' C13' 123.77(19) . . ? B11' C2' C13' 121.53(19) . . ? C1' B3' C2' 60.72(14) . . ? C1' B3' B4' 58.10(15) . . ? C1' B3' B7' 106.22(19) . . ? C1' B3' B8' 104.9(2) . . ? C2' B3' B4' 107.3(2) . . ? C2' B3' B7' 58.02(15) . . ? C2' B3' B8' 105.4(2) . . ? B4' B3' B7' 108.0(2) . . ? B4' B3' B8' 60.01(18) . . ? B7' B3' B8' 59.73(18) . . ? C1' B4' B3' 59.08(16) . . ? C1' B4' B5' 58.98(17) . . ? C1' B4' B8' 105.5(2) . . ? C1' B4' B9' 105.2(2) . . ? B3' B4' B5' 107.9(2) . . ? B3' B4' B8' 59.82(18) . . ? B3' B4' B9' 107.8(2) . . ? B5' B4' B8' 107.9(2) . . ? B5' B4' B9' 59.57(19) . . ? B8' B4' B9' 60.24(19) . . ? C1' B5' B4' 58.14(16) . . ? C1' B5' B6' 58.70(15) . . ? C1' B5' B9' 105.0(2) . . ? C1' B5' B10' 104.8(2) . . ? B4' B5' B6' 107.1(2) . . ? B4' B5' B9' 60.24(18) . . ? B4' B5' B10' 108.3(2) . . ? B6' B5' B9' 107.9(2) . . ? B6' B5' B10' 59.41(17) . . ? B9' B5' B10' 60.78(19) . . ? C1' B6' C2' 60.34(14) . . ? C1' B6' B5' 58.42(16) . . ? C1' B6' B10' 104.9(2) . . ? C1' B6' B11' 106.0(2) . . ? C2' B6' B5' 107.01(19) . . ? C2' B6' B10' 105.0(2) . . ? C2' B6' B11' 57.85(15) . . ? B5' B6' B10' 59.73(18) . . ? B5' B6' B11' 107.7(2) . . ? B10' B6' B11' 59.69(18) . . ? C2' B7' B3' 59.20(15) . . ? C2' B7' B8' 106.2(2) . . ? C2' B7' B11' 58.82(16) . . ? C2' B7' B12' 105.9(2) . . ? B3' B7' B8' 59.63(17) . . ? B3' B7' B11' 107.3(2) . . ? B3' B7' B12' 107.8(2) . . ? B8' B7' B11' 108.3(2) . . ? B8' B7' B12' 60.75(19) . . ? B11' B7' B12' 59.76(19) . . ? B3' B8' B4' 60.18(18) . . ? B3' B8' B7' 60.64(18) . . ? B3' B8' B9' 107.9(2) . . ? B3' B8' B12' 107.6(2) . . ? B4' B8' B7' 108.9(2) . . ? B4' B8' B9' 59.99(19) . . ? B4' B8' B12' 107.8(2) . . ? B7' B8' B9' 107.9(2) . . ? B7' B8' B12' 59.51(18) . . ? B9' B8' B12' 59.73(18) . . ? B4' B9' B5' 60.19(18) . . ? B4' B9' B8' 59.77(19) . . ? B4' B9' B10' 107.4(2) . . ? B4' B9' B12' 108.1(2) . . ? B5' B9' B8' 108.1(2) . . ? B5' B9' B10' 59.66(18) . . ? B5' B9' B12' 108.0(2) . . ? B8' B9' B10' 107.5(2) . . ? B8' B9' B12' 60.35(19) . . ? B10' B9' B12' 59.63(19) . . ? B5' B10' B6' 60.87(18) . . ? B5' B10' B9' 59.56(18) . . ? B5' B10' B11' 109.5(2) . . ? B5' B10' B12' 108.2(2) . . ? B6' B10' B9' 108.1(2) . . ? B6' B10' B11' 60.84(17) . . ? B6' B10' B12' 108.4(2) . . ? B9' B10' B11' 108.1(2) . . ? B9' B10' B12' 59.95(18) . . ? B11' B10' B12' 59.76(19) . . ? C2' B11' B6' 59.85(15) . . ? C2' B11' B7' 58.70(15) . . ? C2' B11' B10' 106.4(2) . . ? C2' B11' B12' 106.0(2) . . ? B6' B11' B7' 107.8(2) . . ? B6' B11' B10' 59.47(17) . . ? B6' B11' B12' 107.7(2) . . ? B7' B11' B10' 108.2(2) . . ? B7' B11' B12' 60.05(19) . . ? B10' B11' B12' 60.33(19) . . ? B7' B12' B8' 59.74(18) . . ? B7' B12' B9' 108.2(2) . . ? B7' B12' B10' 108.0(2) . . ? B7' B12' B11' 60.19(18) . . ? B8' B12' B9' 59.91(19) . . ? B8' B12' B10' 107.8(2) . . ? B8' B12' B11' 107.8(2) . . ? B9' B12' B10' 60.42(19) . . ? B9' B12' B11' 108.6(2) . . ? B10' B12' B11' 59.91(18) . . ? C2' C13' C14' 122.2(2) . . ? C2' C13' C18' 119.9(2) . . ? C14' C13' C18' 117.9(3) . . ? C13' C14' C15' 120.7(3) . . ? C14' C15' C16' 120.4(3) . . ? C15' C16' C17' 119.5(3) . . ? C16' C17' C18' 120.7(3) . . ? C13' C18' C17' 120.8(3) . . ? C1' S19' S20 105.56(9) . . ? S19 S20 S19' 108.50(4) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 64.97 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.154 _refine_diff_density_min -0.195 _refine_diff_density_rms 0.034 #===END