Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_letter ; Please consider this CIF file of one structure for deposit into the Cambridge Structure Database. Thank you very much Sincerely Yours Ivana Cisarova ; _publ_contact_author_name 'J.D. Kennedy' _publ_contact_author_address ; The School of Chemistry of the University of Leeds Leeds UK LS29JT England EU ; _publ_contact_author_email J.D.Kennedy@leeds.ac.uk _publ_contact_author_fax 441333436314 _publ_contact_author_phone 441333436401 _publ_section_title ; Macropolyhedral boron-containing cluster chemistry. Synthesis of the nineteen vertex monocarbaborane [9-(^ter^BuNH~2~)-(anti){9-CB~18~H~20~}] by direct carbon-atom Aufbau ; loop_ _publ_author_name _publ_author_address T.Jelinek ; Institute of Inorganic Chemistry, Academy of Sciences of the Czech Republic 250 68 Rez Czech Republic ; I.Cisarova ; Dept. of Inorganic Chemistry, Faculty of Science, Charles University in Prague Albertov 6 128 43 Praha 2 Czech Republic ; B.Stibr ; Institute of Inorganic Chemistry, Academy of Sciences of the Czech Republic 250 68 Rez Czech Republic ; J.D.Kennedy ; The School of Chemistry of the University of Leeds Leeds UK LS29JT England EU ; data_tom207 _database_code_depnum_ccdc_archive 'CCDC 657002' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C5 H31 B18 N' _chemical_formula_sum 'C5 H31 B18 N' _chemical_formula_weight 299.89 _chemical_compound_source 'synthesized by the authors' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2131(5) _cell_length_b 10.7095(7) _cell_length_c 12.5850(10) _cell_angle_alpha 68.077(6) _cell_angle_beta 72.693(6) _cell_angle_gamma 72.317(5) _cell_volume 956.93(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15 _cell_measurement_theta_max 16 _exptl_crystal_description prism _exptl_crystal_colour colorless _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 1.041 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 316 _exptl_absorpt_coefficient_mu 0.045 _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 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CAD4-MACHIII _diffrn_measurement_method 'theta-2theta scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 1hour _diffrn_standards_decay_% 2 _diffrn_reflns_number 3395 _diffrn_reflns_av_R_equivalents 0.0175 _diffrn_reflns_av_sigmaI/netI 0.0209 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 24.97 _reflns_number_total 3354 _reflns_number_gt 2717 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4 Version 5.0' _computing_cell_refinement 'Enraf-Nonius CAD4 Version 5.0' _computing_data_reduction 'Jana98 (Petricek, 1998)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0863P)^2^+0.1115P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3354 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0609 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.1324 _refine_ls_wR_factor_gt 0.1215 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.3870(2) -0.2046(2) 0.47847(15) 0.0496(4) Uani 1 1 d . . . B2 B 0.5704(2) -0.26584(18) 0.38011(14) 0.0428(4) Uani 1 1 d . . . B3 B 0.37140(19) -0.31877(17) 0.41219(13) 0.0399(4) Uani 1 1 d . . . B4 B 0.1976(2) -0.17834(18) 0.42828(13) 0.0431(4) Uani 1 1 d . . . B5 B 0.2865(2) -0.0383(2) 0.40413(15) 0.0485(4) Uani 1 1 d . . . B6 B 0.5170(2) -0.0873(2) 0.37220(16) 0.0495(4) Uani 1 1 d . . . B7 B 0.50260(18) -0.28679(16) 0.26917(13) 0.0364(3) Uani 1 1 d . . . B8 B 0.27070(18) -0.21508(15) 0.28512(12) 0.0335(3) Uani 1 1 d . . . C9 C 0.22353(16) -0.05755(13) 0.29540(11) 0.0357(3) Uani 1 1 d . . . B10 B 0.4053(2) 0.00293(17) 0.25324(15) 0.0425(4) Uani 1 1 d . . . B11 B 0.6027(2) -0.13727(18) 0.24491(15) 0.0424(4) Uani 1 1 d . . . B1' B 0.3650(2) -0.35811(18) 0.11427(16) 0.0506(4) Uani 1 1 d . . . B2' B 0.4151(2) -0.22947(16) 0.14278(13) 0.0388(4) Uani 1 1 d . . . B3' B 0.1936(2) -0.24284(16) 0.17861(15) 0.0417(4) Uani 1 1 d . . . B4' B 0.1729(3) -0.41418(19) 0.20278(19) 0.0569(5) Uani 1 1 d . . . B5' B 0.5480(2) -0.39894(18) 0.17506(16) 0.0481(4) Uani 1 1 d . . . B8' B 0.0997(2) -0.33844(19) 0.31560(17) 0.0510(4) Uani 1 1 d . . . B9' B 0.2005(3) -0.5153(2) 0.3401(2) 0.0604(5) Uani 1 1 d . . . B10' B 0.3888(3) -0.51981(19) 0.2211(2) 0.0575(5) Uani 1 1 d . . . N1 N 0.04664(15) 0.02795(13) 0.27085(11) 0.0416(3) Uani 1 1 d . . . C1 C 0.01712(18) 0.16671(14) 0.17244(12) 0.0422(3) Uani 1 1 d . . . C2 C 0.0400(3) 0.27754(18) 0.21017(19) 0.0690(5) Uani 1 1 d . . . H2A H 0.1586 0.2589 0.2179 0.103 Uiso 1 1 calc R . . H2B H -0.0374 0.2786 0.2841 0.103 Uiso 1 1 calc R . . H2C H 0.0134 0.3656 0.1525 0.103 Uiso 1 1 calc R . . C3 C -0.1723(2) 0.19038(17) 0.16531(15) 0.0563(4) Uani 1 1 d . . . H3A H -0.2466 0.1894 0.2405 0.084 Uiso 1 1 calc R . . H3B H -0.1852 0.1186 0.1422 0.084 Uiso 1 1 calc R . . H3C H -0.2045 0.2781 0.1086 0.084 Uiso 1 1 calc R . . C4 C 0.1387(2) 0.15212(18) 0.05889(14) 0.0577(4) Uani 1 1 d . . . H4A H 0.1103 0.2341 -0.0043 0.087 Uiso 1 1 calc R . . H4B H 0.1258 0.0741 0.0444 0.087 Uiso 1 1 calc R . . H4C H 0.2572 0.1389 0.0644 0.087 Uiso 1 1 calc R . . H1 H 0.385(2) -0.241(2) 0.5755(17) 0.073(5) Uiso 1 1 d . . . H2 H 0.687(2) -0.3398(17) 0.4095(14) 0.057(5) Uiso 1 1 d . . . H3 H 0.360(2) -0.4258(17) 0.4660(14) 0.053(4) Uiso 1 1 d . . . H4 H 0.066(2) -0.1843(17) 0.4777(15) 0.060(5) Uiso 1 1 d . . . H5 H 0.207(2) 0.0424(19) 0.4407(16) 0.064(5) Uiso 1 1 d . . . H6 H 0.597(2) -0.0413(18) 0.4031(15) 0.065(5) Uiso 1 1 d . . . H75' H 0.565(2) -0.4251(17) 0.2774(15) 0.059(5) Uiso 1 1 d . . . H10 H 0.403(2) 0.1121(17) 0.2035(14) 0.054(4) Uiso 1 1 d . . . H101 H 0.503(2) -0.0649(16) 0.1796(13) 0.050(4) Uiso 1 1 d . . . H11 H 0.734(2) -0.1180(16) 0.1932(14) 0.053(4) Uiso 1 1 d . . . H1' H 0.406(2) -0.361(2) 0.0226(17) 0.075(6) Uiso 1 1 d . . . H2' H 0.453(2) -0.1437(16) 0.0693(14) 0.049(4) Uiso 1 1 d . . . H3' H 0.100(2) -0.1534(17) 0.1318(14) 0.051(4) Uiso 1 1 d . . . H4' H 0.082(2) -0.428(2) 0.1596(17) 0.076(6) Uiso 1 1 d . . . H5' H 0.677(2) -0.4281(18) 0.1250(16) 0.064(5) Uiso 1 1 d . . . H8' H -0.032(2) -0.2988(17) 0.3566(14) 0.056(4) Uiso 1 1 d . . . H89' H 0.176(2) -0.4360(18) 0.3930(14) 0.057(5) Uiso 1 1 d . . . H9' H 0.144(3) -0.607(2) 0.3991(17) 0.082(6) Uiso 1 1 d . . . H91' H 0.369(2) -0.5448(18) 0.3287(15) 0.063(5) Uiso 1 1 d . . . H10' H 0.434(2) -0.617(2) 0.2019(16) 0.073(5) Uiso 1 1 d . . . H1A H -0.022(2) 0.0470(18) 0.3346(16) 0.059(5) Uiso 1 1 d . . . H1B H -0.005(2) -0.029(2) 0.2593(16) 0.065(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.0455(9) 0.0655(11) 0.0378(8) -0.0157(8) -0.0143(7) -0.0071(8) B2 0.0322(8) 0.0513(9) 0.0450(9) -0.0108(7) -0.0153(6) -0.0074(7) B3 0.0317(7) 0.0445(9) 0.0374(8) -0.0027(7) -0.0134(6) -0.0063(6) B4 0.0342(8) 0.0536(9) 0.0334(8) -0.0102(7) -0.0048(6) -0.0047(7) B5 0.0469(9) 0.0583(10) 0.0454(9) -0.0260(8) -0.0125(7) -0.0033(8) B6 0.0460(9) 0.0586(11) 0.0543(10) -0.0223(8) -0.0187(8) -0.0119(8) B7 0.0252(7) 0.0395(8) 0.0426(8) -0.0134(6) -0.0074(6) -0.0035(6) B8 0.0254(7) 0.0365(8) 0.0350(7) -0.0068(6) -0.0075(5) -0.0060(5) C9 0.0305(6) 0.0379(7) 0.0362(7) -0.0104(5) -0.0100(5) -0.0026(5) B10 0.0395(8) 0.0418(9) 0.0491(9) -0.0146(7) -0.0114(7) -0.0100(7) B11 0.0311(8) 0.0483(9) 0.0478(9) -0.0134(7) -0.0077(6) -0.0113(7) B1' 0.0582(11) 0.0460(9) 0.0541(10) -0.0202(8) -0.0232(8) -0.0033(8) B2' 0.0366(8) 0.0411(8) 0.0376(8) -0.0131(7) -0.0077(6) -0.0057(6) B3' 0.0399(8) 0.0401(8) 0.0492(9) -0.0117(7) -0.0205(7) -0.0059(6) B4' 0.0605(11) 0.0448(10) 0.0772(13) -0.0122(9) -0.0363(10) -0.0147(8) B5' 0.0429(9) 0.0460(9) 0.0554(10) -0.0221(8) -0.0118(8) -0.0003(7) B8' 0.0356(9) 0.0542(10) 0.0621(11) -0.0074(8) -0.0171(8) -0.0149(7) B9' 0.0592(11) 0.0490(10) 0.0765(13) -0.0035(10) -0.0285(10) -0.0229(9) B10' 0.0642(12) 0.0405(9) 0.0755(13) -0.0199(9) -0.0318(10) -0.0030(8) N1 0.0329(6) 0.0408(7) 0.0427(7) -0.0099(5) -0.0079(5) 0.0000(5) C1 0.0440(8) 0.0338(7) 0.0442(7) -0.0078(6) -0.0149(6) -0.0022(6) C2 0.0777(12) 0.0445(9) 0.0939(14) -0.0261(9) -0.0355(10) -0.0032(8) C3 0.0481(9) 0.0536(9) 0.0588(10) -0.0092(8) -0.0220(7) 0.0009(7) C4 0.0586(10) 0.0580(10) 0.0437(8) -0.0052(7) -0.0063(7) -0.0126(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 B5 1.746(3) . ? B1 B4 1.757(2) . ? B1 B2 1.769(2) . ? B1 B3 1.769(2) . ? B1 B6 1.793(3) . ? B1 H1 1.131(19) . ? B2 B11 1.751(2) . ? B2 B7 1.756(2) . ? B2 B3 1.777(2) . ? B2 B6 1.797(3) . ? B2 H2 1.099(17) . ? B3 B4 1.758(2) . ? B3 B7 1.769(2) . ? B3 B8 1.838(2) . ? B3 H3 1.108(17) . ? B4 C9 1.690(2) . ? B4 B5 1.751(3) . ? B4 B8 1.872(2) . ? B4 H4 1.085(17) . ? B5 C9 1.697(2) . ? B5 B6 1.767(2) . ? B5 B10 1.813(2) . ? B5 H5 1.078(18) . ? B6 B11 1.757(2) . ? B6 B10 1.793(2) . ? B6 H6 1.146(18) . ? B7 B2' 1.763(2) . ? B7 B8 1.8047(19) . ? B7 B5' 1.874(2) . ? B7 B11 1.902(2) . ? B7 H75' 1.387(17) . ? B8 C9 1.658(2) . ? B8 B3' 1.790(2) . ? B8 B2' 1.863(2) . ? B8 B8' 2.072(2) . ? C9 N1 1.5140(16) . ? C9 B10 1.670(2) . ? B10 B11 1.852(2) . ? B10 H10 1.098(17) . ? B10 H101 1.317(15) . ? B11 H101 1.219(15) . ? B11 H11 1.116(16) . ? B1' B2' 1.731(2) . ? B1' B10' 1.748(3) . ? B1' B5' 1.752(2) . ? B1' B4' 1.767(3) . ? B1' B3' 1.782(2) . ? B1' H1' 1.11(2) . ? B2' B3' 1.776(2) . ? B2' B5' 1.778(2) . ? B2' H2' 1.078(16) . ? B3' B8' 1.728(2) . ? B3' B4' 1.797(2) . ? B3' H3' 1.121(16) . ? B4' B9' 1.702(3) . ? B4' B8' 1.758(3) . ? B4' B10' 1.818(3) . ? B4' H4' 1.117(19) . ? B5' B10' 1.934(3) . ? B5' H75' 1.254(17) . ? B5' H5' 1.078(18) . ? B8' B9' 1.770(3) . ? B8' H8' 1.079(17) . ? B8' H89' 1.282(16) . ? B9' B10' 1.808(3) . ? B9' H89' 1.203(17) . ? B9' H9' 1.13(2) . ? B9' H91' 1.302(17) . ? B10' H91' 1.249(17) . ? B10' H10' 1.08(2) . ? N1 C1 1.5448(17) . ? N1 H1A 0.888(19) . ? N1 H1B 0.91(2) . ? C1 C2 1.510(2) . ? C1 C4 1.512(2) . ? C1 C3 1.523(2) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? 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 B5 B1 B4 59.99(10) . . ? B5 B1 B2 108.58(12) . . ? B4 B1 B2 108.64(11) . . ? B5 B1 B3 107.72(11) . . ? B4 B1 B3 59.83(9) . . ? B2 B1 B3 60.29(9) . . ? B5 B1 B6 59.89(10) . . ? B4 B1 B6 108.20(12) . . ? B2 B1 B6 60.61(10) . . ? B3 B1 B6 108.31(12) . . ? B5 B1 H1 123.4(10) . . ? B4 B1 H1 120.6(10) . . ? B2 B1 H1 120.6(10) . . ? B3 B1 H1 119.6(10) . . ? B6 B1 H1 123.4(10) . . ? B11 B2 B7 65.70(9) . . ? B11 B2 B1 110.79(12) . . ? B7 B2 B1 110.15(11) . . ? B11 B2 B3 112.75(10) . . ? B7 B2 B3 60.09(8) . . ? B1 B2 B3 59.86(9) . . ? B11 B2 B6 59.35(10) . . ? B7 B2 B6 110.94(11) . . ? B1 B2 B6 60.36(10) . . ? B3 B2 B6 107.78(11) . . ? B11 B2 H2 117.6(9) . . ? B7 B2 H2 117.0(9) . . ? B1 B2 H2 122.3(9) . . ? B3 B2 H2 120.7(9) . . ? B6 B2 H2 123.6(9) . . ? B4 B3 B7 112.69(11) . . ? B4 B3 B1 59.74(10) . . ? B7 B3 B1 109.55(11) . . ? B4 B3 B2 108.21(12) . . ? B7 B3 B2 59.38(9) . . ? B1 B3 B2 59.85(10) . . ? B4 B3 B8 62.68(8) . . ? B7 B3 B8 60.02(8) . . ? B1 B3 B8 107.85(11) . . ? B2 B3 B8 105.13(10) . . ? B4 B3 H3 120.8(8) . . ? B7 B3 H3 119.8(8) . . ? B1 B3 H3 119.8(8) . . ? B2 B3 H3 120.6(8) . . ? B8 B3 H3 125.4(8) . . ? C9 B4 B5 59.04(9) . . ? C9 B4 B1 104.59(11) . . ? B5 B4 B1 59.70(10) . . ? C9 B4 B3 104.03(10) . . ? B5 B4 B3 107.96(12) . . ? B1 B4 B3 60.43(9) . . ? C9 B4 B8 55.20(8) . . ? B5 B4 B8 104.62(10) . . ? B1 B4 B8 106.88(11) . . ? B3 B4 B8 60.73(8) . . ? C9 B4 H4 118.1(9) . . ? B5 B4 H4 121.6(9) . . ? B1 B4 H4 129.4(9) . . ? B3 B4 H4 126.1(9) . . ? B8 B4 H4 119.0(9) . . ? C9 B5 B1 104.77(12) . . ? C9 B5 B4 58.67(9) . . ? B1 B5 B4 60.30(10) . . ? C9 B5 B6 104.82(11) . . ? B1 B5 B6 61.37(10) . . ? B4 B5 B6 109.63(13) . . ? C9 B5 B10 56.71(8) . . ? B1 B5 B10 107.51(12) . . ? B4 B5 B10 106.10(11) . . ? B6 B5 B10 60.10(10) . . ? C9 B5 H5 117.6(9) . . ? B1 B5 H5 127.7(9) . . ? B4 B5 H5 118.2(10) . . ? B6 B5 H5 127.4(10) . . ? B10 B5 H5 120.7(10) . . ? B11 B6 B5 113.64(11) . . ? B11 B6 B1 109.37(12) . . ? B5 B6 B1 58.74(10) . . ? B11 B6 B10 62.89(9) . . ? B5 B6 B10 61.22(9) . . ? B1 B6 B10 106.36(11) . . ? B11 B6 B2 59.00(10) . . ? B5 B6 B2 106.39(12) . . ? B1 B6 B2 59.03(10) . . ? B10 B6 B2 105.41(11) . . ? B11 B6 H6 120.7(9) . . ? B5 B6 H6 119.4(9) . . ? B1 B6 H6 119.3(9) . . ? B10 B6 H6 125.2(9) . . ? B2 B6 H6 122.9(9) . . ? B2 B7 B2' 154.98(12) . . ? B2 B7 B3 60.54(9) . . ? B2' B7 B3 122.69(10) . . ? B2 B7 B8 107.43(10) . . ? B2' B7 B8 62.95(8) . . ? B3 B7 B8 61.89(8) . . ? B2 B7 B5' 143.94(11) . . ? B2' B7 B5' 58.44(9) . . ? B3 B7 B5' 123.81(12) . . ? B8 B7 B5' 104.12(10) . . ? B2 B7 B11 57.02(9) . . ? B2' B7 B11 101.41(10) . . ? B3 B7 B11 106.23(11) . . ? B8 B7 B11 104.81(10) . . ? B5' B7 B11 129.52(11) . . ? B2 B7 H75' 105.5(7) . . ? B2' B7 H75' 99.1(7) . . ? B3 B7 H75' 94.6(7) . . ? B8 B7 H75' 119.4(7) . . ? B5' B7 H75' 42.0(7) . . ? B11 B7 H75' 135.8(7) . . ? C9 B8 B3' 119.20(11) . . ? C9 B8 B7 110.75(10) . . ? B3' B8 B7 108.94(11) . . ? C9 B8 B3 101.95(10) . . ? B3' B8 B3 138.18(12) . . ? B7 B8 B3 58.09(8) . . ? C9 B8 B2' 113.04(10) . . ? B3' B8 B2' 58.15(8) . . ? B7 B8 B2' 57.42(8) . . ? B3 B8 B2' 113.72(10) . . ? C9 B8 B4 56.82(8) . . ? B3' B8 B4 142.84(11) . . ? B7 B8 B4 105.97(10) . . ? B3 B8 B4 56.58(8) . . ? B2' B8 B4 158.39(11) . . ? C9 B8 B8' 128.10(10) . . ? B3' B8 B8' 52.54(8) . . ? B7 B8 B8' 120.26(11) . . ? B3 B8 B8' 96.95(9) . . ? B2' B8 B8' 102.17(10) . . ? B4 B8 B8' 98.38(10) . . ? N1 C9 B8 114.59(11) . . ? N1 C9 B10 124.90(11) . . ? B8 C9 B10 110.07(10) . . ? N1 C9 B4 109.69(10) . . ? B8 C9 B4 67.98(9) . . ? B10 C9 B4 115.96(11) . . ? N1 C9 B5 116.04(11) . . ? B8 C9 B5 117.50(11) . . ? B10 C9 B5 65.16(10) . . ? B4 C9 B5 62.29(10) . . ? C9 B10 B6 104.80(11) . . ? C9 B10 B5 58.13(9) . . ? B6 B10 B5 58.68(10) . . ? C9 B10 B11 111.05(11) . . ? B6 B10 B11 57.60(9) . . ? B5 B10 B11 107.17(11) . . ? C9 B10 H10 120.4(8) . . ? B6 B10 H10 122.4(8) . . ? B5 B10 H10 117.7(8) . . ? B11 B10 H10 123.9(8) . . ? C9 B10 H101 101.2(7) . . ? B6 B10 H101 98.6(7) . . ? B5 B10 H101 137.2(7) . . ? B11 B10 H101 41.1(7) . . ? H10 B10 H101 105.0(11) . . ? B2 B11 B6 61.65(10) . . ? B2 B11 B10 104.85(11) . . ? B6 B11 B10 59.50(9) . . ? B2 B11 B7 57.28(8) . . ? B6 B11 B7 106.19(11) . . ? B10 B11 B7 101.30(10) . . ? B2 B11 H101 131.1(7) . . ? B6 B11 H101 104.7(7) . . ? B10 B11 H101 45.2(7) . . ? B7 B11 H101 87.7(7) . . ? B2 B11 H11 123.6(8) . . ? B6 B11 H11 117.8(8) . . ? B10 B11 H11 123.0(8) . . ? B7 B11 H11 128.5(8) . . ? H101 B11 H11 104.6(11) . . ? B2' B1' B10' 115.72(13) . . ? B2' B1' B5' 61.37(9) . . ? B10' B1' B5' 67.07(11) . . ? B2' B1' B4' 116.22(13) . . ? B10' B1' B4' 62.30(11) . . ? B5' B1' B4' 119.74(14) . . ? B2' B1' B3' 60.73(9) . . ? B10' B1' B3' 107.38(14) . . ? B5' B1' B3' 109.15(12) . . ? B4' B1' B3' 60.86(10) . . ? B2' B1' H1' 117.5(10) . . ? B10' B1' H1' 114.7(10) . . ? B5' B1' H1' 110.6(10) . . ? B4' B1' H1' 118.6(10) . . ? B3' B1' H1' 130.4(10) . . ? B1' B2' B7 114.22(12) . . ? B1' B2' B3' 61.04(10) . . ? B7 B2' B3' 111.50(11) . . ? B1' B2' B5' 59.90(10) . . ? B7 B2' B5' 63.92(9) . . ? B3' B2' B5' 108.24(12) . . ? B1' B2' B8 106.67(11) . . ? B7 B2' B8 59.63(8) . . ? B3' B2' B8 58.87(8) . . ? B5' B2' B8 105.66(11) . . ? B1' B2' H2' 117.8(8) . . ? B7 B2' H2' 120.5(8) . . ? B3' B2' H2' 117.5(8) . . ? B5' B2' H2' 123.9(8) . . ? B8 B2' H2' 124.8(8) . . ? B8' B3' B2' 121.97(11) . . ? B8' B3' B1' 107.85(12) . . ? B2' B3' B1' 58.23(9) . . ? B8' B3' B8 72.15(10) . . ? B2' B3' B8 62.98(8) . . ? B1' B3' B8 107.70(11) . . ? B8' B3' B4' 59.80(11) . . ? B2' B3' B4' 112.41(12) . . ? B1' B3' B4' 59.15(11) . . ? B8 B3' B4' 117.96(12) . . ? B8' B3' H3' 114.5(8) . . ? B2' B3' H3' 117.2(8) . . ? B1' B3' H3' 125.9(8) . . ? B8 B3' H3' 116.1(8) . . ? B4' B3' H3' 118.2(8) . . ? B9' B4' B8' 61.50(12) . . ? B9' B4' B1' 111.92(13) . . ? B8' B4' B1' 107.19(12) . . ? B9' B4' B3' 109.70(13) . . ? B8' B4' B3' 58.15(10) . . ? B1' B4' B3' 59.98(10) . . ? B9' B4' B10' 61.70(12) . . ? B8' B4' B10' 105.16(13) . . ? B1' B4' B10' 58.36(11) . . ? B3' B4' B10' 103.78(12) . . ? B9' B4' H4' 122.1(10) . . ? B8' B4' H4' 122.6(10) . . ? B1' B4' H4' 118.5(10) . . ? B3' B4' H4' 118.8(10) . . ? B10' B4' H4' 127.4(10) . . ? B1' B5' B2' 58.73(9) . . ? B1' B5' B7 107.96(11) . . ? B2' B5' B7 57.65(8) . . ? B1' B5' B10' 56.37(10) . . ? B2' B5' B10' 105.00(11) . . ? B7 B5' B10' 115.31(12) . . ? B1' B5' H75' 132.7(8) . . ? B2' B5' H75' 103.9(8) . . ? B7 B5' H75' 47.8(8) . . ? B10' B5' H75' 94.3(8) . . ? B1' B5' H5' 119.7(10) . . ? B2' B5' H5' 124.3(9) . . ? B7 B5' H5' 122.0(10) . . ? B10' B5' H5' 117.8(10) . . ? H75' B5' H5' 106.4(12) . . ? B3' B8' B4' 62.06(11) . . ? B3' B8' B9' 109.79(14) . . ? B4' B8' B9' 57.68(12) . . ? B3' B8' B8 55.31(8) . . ? B4' B8' B8 106.46(12) . . ? B9' B8' B8 113.75(11) . . ? B3' B8' H8' 119.9(9) . . ? B4' B8' H8' 129.9(9) . . ? B9' B8' H8' 125.1(9) . . ? B8 B8' H8' 113.0(9) . . ? B3' B8' H89' 128.1(7) . . ? B4' B8' H89' 98.6(8) . . ? B9' B8' H89' 42.8(8) . . ? B8 B8' H89' 92.0(8) . . ? H8' B8' H89' 109.4(11) . . ? B4' B9' B8' 60.82(12) . . ? B4' B9' B10' 62.32(12) . . ? B8' B9' B10' 105.12(13) . . ? B4' B9' H89' 105.0(8) . . ? B8' B9' H89' 46.4(8) . . ? B10' B9' H89' 118.4(8) . . ? B4' B9' H9' 129.0(10) . . ? B8' B9' H9' 128.2(10) . . ? B10' B9' H9' 124.6(11) . . ? H89' B9' H9' 109.8(13) . . ? B4' B9' H91' 102.7(8) . . ? B8' B9' H91' 115.2(8) . . ? B10' B9' H91' 43.7(8) . . ? H89' B9' H91' 93.7(11) . . ? H9' B9' H91' 110.8(13) . . ? B1' B10' B9' 107.85(14) . . ? B1' B10' B4' 59.35(11) . . ? B9' B10' B4' 55.98(11) . . ? B1' B10' B5' 56.56(10) . . ? B9' B10' B5' 122.04(13) . . ? B4' B10' B5' 108.38(12) . . ? B1' B10' H91' 127.4(8) . . ? B9' B10' H91' 46.1(8) . . ? B4' B10' H91' 98.9(8) . . ? B5' B10' H91' 95.7(8) . . ? B1' B10' H10' 124.0(10) . . ? B9' B10' H10' 114.0(10) . . ? B4' B10' H10' 120.4(10) . . ? B5' B10' H10' 119.8(10) . . ? H91' B10' H10' 108.5(13) . . ? C9 N1 C1 124.81(11) . . ? C9 N1 H1A 110.5(11) . . ? C1 N1 H1A 103.6(11) . . ? C9 N1 H1B 106.1(12) . . ? C1 N1 H1B 106.4(12) . . ? H1A N1 H1B 103.6(16) . . ? C2 C1 C4 113.90(15) . . ? C2 C1 C3 110.37(13) . . ? C4 C1 C3 110.58(13) . . ? C2 C1 N1 108.47(13) . . ? C4 C1 N1 109.30(11) . . ? C3 C1 N1 103.69(12) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.151 _refine_diff_density_min -0.202 _refine_diff_density_rms 0.033 #===END