# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 1475 loop_ _publ_author_name 'Wright, Dominic S.' _publ_contact_author_name 'Wright, Dominic S.' _publ_contact_author_email DSW1000@CAM.AC.UK _publ_section_title ; Group 13 BN dehydrocoupling reagents, similar to transition metal catalysts but with unique reactivity ; # Attachment '- Compound6.cif' data_dw0969 _database_code_depnum_ccdc_archive 'CCDC 817717' #TrackingRef '- Compound6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H44 Al2 N6' _chemical_formula_sum 'C8 H22 Al N3' _chemical_formula_weight 187.27 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' Al Al 0.0645 0.0514 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/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 8.7047(2) _cell_length_b 15.6298(3) _cell_length_c 9.3874(2) _cell_angle_alpha 90.00 _cell_angle_beta 115.9220(10) _cell_angle_gamma 90.00 _cell_volume 1148.68(4) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 83968 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 25.35 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.083 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 416 _exptl_absorpt_coefficient_mu 0.137 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.836 _exptl_absorpt_correction_T_max 0.962 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_reflns_number 14062 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0304 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 30.99 _reflns_number_total 3651 _reflns_number_gt 3031 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SHELXL-97 (Sheldrick 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H atoms added at calculated positions and refined with riding model except the N-H H atom of the Al2N2 ring which was found in the differenc map and refined freely. ; _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^)+(0.0468P)^2^+0.2543P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3651 _refine_ls_number_parameters 120 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.1002 _refine_ls_wR_factor_gt 0.0941 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 Al1 Al 0.43463(3) 0.022383(18) 0.33591(3) 0.01933(9) Uani 1 1 d . . . N1 N 0.36132(10) 0.03388(5) 0.50458(9) 0.02014(16) Uani 1 1 d . . . N2 N 0.27641(11) -0.03928(6) 0.17719(10) 0.02569(18) Uani 1 1 d . . . N3 N 0.50113(11) 0.11548(6) 0.26424(10) 0.02609(18) Uani 1 1 d . . . C1 C 0.28410(13) 0.11427(7) 0.53415(12) 0.0257(2) Uani 1 1 d . . . C7 C 0.38264(15) 0.16324(7) 0.12781(13) 0.0338(2) Uani 1 1 d . . . H7A H 0.3613 0.2193 0.1622 0.051 Uiso 1 1 calc R . . H7B H 0.2748 0.1317 0.0765 0.051 Uiso 1 1 calc R . . H7C H 0.4318 0.1709 0.0526 0.051 Uiso 1 1 calc R . . C8 C 0.66268(15) 0.15979(8) 0.33589(15) 0.0387(3) Uani 1 1 d . . . H8A H 0.7107 0.1643 0.2592 0.058 Uiso 1 1 calc R . . H8B H 0.7418 0.1280 0.4291 0.058 Uiso 1 1 calc R . . H8C H 0.6453 0.2173 0.3680 0.058 Uiso 1 1 calc R . . C6 C 0.29381(16) -0.05531(9) 0.03288(13) 0.0377(3) Uani 1 1 d . . . H6A H 0.3233 -0.1155 0.0294 0.057 Uiso 1 1 calc R . . H6B H 0.3842 -0.0188 0.0306 0.057 Uiso 1 1 calc R . . H6C H 0.1856 -0.0424 -0.0589 0.057 Uiso 1 1 calc R . . C4 C 0.41635(16) 0.18547(7) 0.58428(15) 0.0364(3) Uani 1 1 d . . . H4A H 0.5153 0.1690 0.6821 0.055 Uiso 1 1 calc R . . H4B H 0.3662 0.2381 0.6025 0.055 Uiso 1 1 calc R . . H4C H 0.4528 0.1953 0.5005 0.055 Uiso 1 1 calc R . . C3 C 0.12903(15) 0.13970(9) 0.38185(14) 0.0383(3) Uani 1 1 d . . . H3A H 0.1654 0.1516 0.2987 0.058 Uiso 1 1 calc R . . H3B H 0.0762 0.1910 0.4012 0.058 Uiso 1 1 calc R . . H3C H 0.0460 0.0928 0.3480 0.058 Uiso 1 1 calc R . . C5 C 0.13750(16) -0.08973(9) 0.17809(15) 0.0397(3) Uani 1 1 d . . . H5A H 0.0327 -0.0774 0.0824 0.060 Uiso 1 1 calc R . . H5B H 0.1207 -0.0753 0.2719 0.060 Uiso 1 1 calc R . . H5C H 0.1651 -0.1507 0.1806 0.060 Uiso 1 1 calc R . . C2 C 0.22778(18) 0.09656(9) 0.66436(15) 0.0413(3) Uani 1 1 d . . . H2A H 0.1430 0.0504 0.6305 0.062 Uiso 1 1 calc R . . H2B H 0.1772 0.1484 0.6846 0.062 Uiso 1 1 calc R . . H2C H 0.3270 0.0795 0.7615 0.062 Uiso 1 1 calc R . . H1 H 0.2834(18) -0.0049(10) 0.4829(16) 0.035(4) 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 Al1 0.01978(14) 0.01952(15) 0.01697(14) 0.00020(10) 0.00645(11) -0.00023(9) N1 0.0193(3) 0.0196(4) 0.0204(3) -0.0004(3) 0.0076(3) 0.0004(3) N2 0.0252(4) 0.0290(4) 0.0204(4) -0.0039(3) 0.0077(3) -0.0052(3) N3 0.0269(4) 0.0249(4) 0.0234(4) 0.0040(3) 0.0082(3) -0.0026(3) C1 0.0268(4) 0.0257(5) 0.0253(4) 0.0003(4) 0.0119(4) 0.0071(4) C7 0.0394(6) 0.0300(5) 0.0290(5) 0.0082(4) 0.0121(4) 0.0031(4) C8 0.0359(6) 0.0382(6) 0.0357(6) 0.0062(5) 0.0099(5) -0.0132(5) C6 0.0395(6) 0.0478(7) 0.0241(5) -0.0098(5) 0.0123(4) -0.0075(5) C4 0.0394(6) 0.0231(5) 0.0434(6) -0.0044(4) 0.0150(5) 0.0027(4) C3 0.0323(5) 0.0420(6) 0.0349(6) 0.0041(5) 0.0093(5) 0.0156(5) C5 0.0356(6) 0.0458(7) 0.0361(6) -0.0105(5) 0.0139(5) -0.0171(5) C2 0.0511(7) 0.0439(7) 0.0409(6) 0.0019(5) 0.0312(6) 0.0122(6) _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 Al1 N3 1.8015(9) . ? Al1 N2 1.8032(8) . ? Al1 N1 1.9570(9) . ? Al1 N1 1.9608(8) 3_656 ? Al1 Al1 2.8654(5) 3_656 ? N1 C1 1.5070(12) . ? N1 Al1 1.9608(8) 3_656 ? N1 H1 0.866(15) . ? N2 C5 1.4467(14) . ? N2 C6 1.4492(14) . ? N3 C8 1.4432(14) . ? N3 C7 1.4514(13) . ? C1 C4 1.5204(16) . ? C1 C2 1.5280(16) . ? C1 C3 1.5287(14) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Al1 N2 112.16(4) . . ? N3 Al1 N1 119.98(4) . . ? N2 Al1 N1 108.43(4) . . ? N3 Al1 N1 108.41(4) . 3_656 ? N2 Al1 N1 120.07(4) . 3_656 ? N1 Al1 N1 86.00(4) . 3_656 ? N3 Al1 Al1 123.87(3) . 3_656 ? N2 Al1 Al1 123.97(3) . 3_656 ? N1 Al1 Al1 43.05(2) . 3_656 ? N1 Al1 Al1 42.95(3) 3_656 3_656 ? C1 N1 Al1 123.71(6) . . ? C1 N1 Al1 124.15(6) . 3_656 ? Al1 N1 Al1 94.00(4) . 3_656 ? C1 N1 H1 105.1(10) . . ? Al1 N1 H1 104.2(9) . . ? Al1 N1 H1 102.8(9) 3_656 . ? C5 N2 C6 109.90(9) . . ? C5 N2 Al1 128.68(8) . . ? C6 N2 Al1 120.71(7) . . ? C8 N3 C7 109.64(9) . . ? C8 N3 Al1 128.34(7) . . ? C7 N3 Al1 121.64(7) . . ? N1 C1 C4 109.21(8) . . ? N1 C1 C2 108.74(9) . . ? C4 C1 C2 110.45(10) . . ? N1 C1 C3 109.09(8) . . ? C4 C1 C3 109.80(10) . . ? C2 C1 C3 109.53(10) . . ? N3 C7 H7A 109.5 . . ? N3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 H8A 109.5 . . ? N3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N2 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 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 . . ? 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 . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? 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 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Al1 N1 C1 27.35(9) . . . . ? N2 Al1 N1 C1 -103.28(8) . . . . ? N1 Al1 N1 C1 136.32(9) 3_656 . . . ? Al1 Al1 N1 C1 136.32(9) 3_656 . . . ? N3 Al1 N1 Al1 -108.97(4) . . . 3_656 ? N2 Al1 N1 Al1 120.40(4) . . . 3_656 ? N1 Al1 N1 Al1 0.0 3_656 . . 3_656 ? N3 Al1 N2 C5 -147.91(10) . . . . ? N1 Al1 N2 C5 -13.13(11) . . . . ? N1 Al1 N2 C5 83.07(11) 3_656 . . . ? Al1 Al1 N2 C5 32.10(12) 3_656 . . . ? N3 Al1 N2 C6 42.84(10) . . . . ? N1 Al1 N2 C6 177.62(9) . . . . ? N1 Al1 N2 C6 -86.19(9) 3_656 . . . ? Al1 Al1 N2 C6 -137.15(8) 3_656 . . . ? N2 Al1 N3 C8 -152.50(10) . . . . ? N1 Al1 N3 C8 78.53(11) . . . . ? N1 Al1 N3 C8 -17.61(11) 3_656 . . . ? Al1 Al1 N3 C8 27.49(12) 3_656 . . . ? N2 Al1 N3 C7 35.30(10) . . . . ? N1 Al1 N3 C7 -93.68(9) . . . . ? N1 Al1 N3 C7 170.18(8) 3_656 . . . ? Al1 Al1 N3 C7 -144.71(8) 3_656 . . . ? Al1 N1 C1 C4 -64.71(10) . . . . ? Al1 N1 C1 C4 58.93(11) 3_656 . . . ? Al1 N1 C1 C2 174.71(8) . . . . ? Al1 N1 C1 C2 -61.65(11) 3_656 . . . ? Al1 N1 C1 C3 55.30(11) . . . . ? Al1 N1 C1 C3 178.94(8) 3_656 . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.267 _refine_diff_density_min -0.222 _refine_diff_density_rms 0.042 # Attachment '- Compound7.cif' data_dw1115 _database_code_depnum_ccdc_archive 'CCDC 817718' #TrackingRef '- Compound7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H32 Al2 N2' _chemical_formula_sum 'C12 H32 Al2 N2' _chemical_formula_weight 258.36 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.6013(3) _cell_length_b 15.4860(3) _cell_length_c 8.6751(2) _cell_angle_alpha 90.00 _cell_angle_beta 122.28(3) _cell_angle_gamma 90.00 _cell_volume 1658.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 7544 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 32.03 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.035 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 0.158 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.905 _exptl_absorpt_correction_T_max 0.985 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; Entry YADZIN in CSD ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_reflns_number 12424 _diffrn_reflns_av_R_equivalents 0.0270 _diffrn_reflns_av_sigmaI/netI 0.0253 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 4.13 _diffrn_reflns_theta_max 32.02 _reflns_number_total 2880 _reflns_number_gt 2312 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0480P)^2^+0.6211P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2880 _refine_ls_number_parameters 83 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0503 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.1083 _refine_ls_wR_factor_gt 0.0999 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 Al1 Al 0.23535(3) 0.309847(18) 0.60207(4) 0.03014(11) Uani 1 1 d . . . H1 H 0.3331(11) 0.3490(8) 0.7821(18) 0.036 Uiso 1 1 d . . . H2 H 0.1225(10) 0.3411(8) 0.5513(18) 0.036 Uiso 1 1 d . . . N1 N 0.24321(6) 0.18325(5) 0.60311(10) 0.02549(16) Uani 1 1 d . . . C1 C 0.34368(8) 0.14977(7) 0.77296(14) 0.0341(2) Uani 1 1 d . . . H1A H 0.4045 0.1847 0.7840 0.041 Uiso 1 1 calc R . . C2 C 0.37333(13) 0.05605(8) 0.7641(2) 0.0537(3) Uani 1 1 d . . . H2A H 0.3640 0.0451 0.6452 0.081 Uiso 1 1 calc R . . H2B H 0.3261 0.0173 0.7805 0.081 Uiso 1 1 calc R . . H2C H 0.4490 0.0456 0.8609 0.081 Uiso 1 1 calc R . . C3 C 0.34871(12) 0.16532(10) 0.95105(16) 0.0509(3) Uani 1 1 d . . . H3A H 0.3252 0.2244 0.9526 0.076 Uiso 1 1 calc R . . H3B H 0.4232 0.1572 1.0541 0.076 Uiso 1 1 calc R . . H3C H 0.3009 0.1243 0.9608 0.076 Uiso 1 1 calc R . . C4 C 0.13407(8) 0.14383(7) 0.54303(14) 0.0323(2) Uani 1 1 d . . . H4A H 0.0810 0.1749 0.4281 0.039 Uiso 1 1 calc R . . C5 C 0.09391(10) 0.15835(9) 0.67104(18) 0.0439(3) Uani 1 1 d . . . H5A H 0.1062 0.2187 0.7114 0.066 Uiso 1 1 calc R . . H5B H 0.1334 0.1203 0.7772 0.066 Uiso 1 1 calc R . . H5C H 0.0163 0.1454 0.6068 0.066 Uiso 1 1 calc R . . C6 C 0.12228(12) 0.04852(8) 0.4901(2) 0.0503(3) Uani 1 1 d . . . H6A H 0.1539 0.0384 0.4165 0.075 Uiso 1 1 calc R . . H6B H 0.0453 0.0330 0.4192 0.075 Uiso 1 1 calc R . . H6C H 0.1600 0.0130 0.6006 0.075 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 Al1 0.04297(19) 0.02307(15) 0.03094(17) -0.00171(11) 0.02412(14) -0.00223(11) N1 0.0293(4) 0.0232(4) 0.0243(4) 0.0015(3) 0.0145(3) -0.0032(3) C1 0.0336(5) 0.0343(5) 0.0289(4) 0.0054(4) 0.0129(4) -0.0004(4) C2 0.0605(8) 0.0384(6) 0.0527(7) 0.0152(5) 0.0239(6) 0.0141(6) C3 0.0518(7) 0.0665(8) 0.0270(5) 0.0064(5) 0.0160(5) -0.0006(6) C4 0.0331(4) 0.0341(5) 0.0306(5) -0.0008(4) 0.0176(4) -0.0086(4) C5 0.0445(6) 0.0517(7) 0.0465(6) -0.0003(5) 0.0318(5) -0.0078(5) C6 0.0625(8) 0.0378(6) 0.0591(8) -0.0119(5) 0.0382(7) -0.0228(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 Al1 N1 1.9636(8) . ? Al1 N1 1.9679(8) 7_556 ? Al1 Al1 2.7503(6) 7_556 ? Al1 H1 1.569(13) . ? Al1 H2 1.540(13) . ? N1 C1 1.5110(14) . ? N1 C4 1.5155(12) . ? N1 Al1 1.9679(8) 7_556 ? C1 C3 1.5261(17) . ? C1 C2 1.5282(17) . ? C1 H1A 1.0000 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.5242(16) . ? C4 C6 1.5279(16) . ? C4 H4A 1.0000 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Al1 N1 91.22(3) . 7_556 ? N1 Al1 Al1 45.67(2) . 7_556 ? N1 Al1 Al1 45.54(2) 7_556 7_556 ? N1 Al1 H1 111.2(5) . . ? N1 Al1 H1 112.3(5) 7_556 . ? Al1 Al1 H1 122.0(5) 7_556 . ? N1 Al1 H2 111.5(5) . . ? N1 Al1 H2 112.8(5) 7_556 . ? Al1 Al1 H2 122.6(5) 7_556 . ? H1 Al1 H2 115.4(7) . . ? C1 N1 C4 119.48(8) . . ? C1 N1 Al1 111.77(6) . . ? C4 N1 Al1 110.64(6) . . ? C1 N1 Al1 111.11(6) . 7_556 ? C4 N1 Al1 110.90(6) . 7_556 ? Al1 N1 Al1 88.78(3) . 7_556 ? N1 C1 C3 115.46(10) . . ? N1 C1 C2 115.49(9) . . ? C3 C1 C2 109.82(10) . . ? N1 C1 H1A 104.9 . . ? C3 C1 H1A 104.9 . . ? C2 C1 H1A 104.9 . . ? 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 . . ? N1 C4 C5 115.66(9) . . ? N1 C4 C6 114.93(9) . . ? C5 C4 C6 109.64(9) . . ? N1 C4 H4A 105.2 . . ? C5 C4 H4A 105.2 . . ? C6 C4 H4A 105.2 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 32.02 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.299 _refine_diff_density_min -0.264 _refine_diff_density_rms 0.039 # Attachment '- Compound8.cif' data_dw1116 _database_code_depnum_ccdc_archive 'CCDC 817719' #TrackingRef '- Compound8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H36 B3 N3' _chemical_formula_sum 'C12 H36 B3 N3' _chemical_formula_weight 254.87 _chemical_absolute_configuration ; 4423 Friedel pairs averaged for the refinement ; 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 hexagonal _symmetry_space_group_name_H-M P6(5) _symmetry_space_group_name_Hall 'P 65' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' '-x, -y, z+1/2' 'y, -x+y, z+1/6' 'x-y, x, z+5/6' _cell_length_a 19.5895(6) _cell_length_b 19.5895(6) _cell_length_c 31.1522(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 10353.0(5) _cell_formula_units_Z 24 _cell_measurement_temperature 260(2) _cell_measurement_reflns_used 262529 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 26.02 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.981 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3456 _exptl_absorpt_coefficient_mu 0.055 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.846 _exptl_absorpt_correction_T_max 0.998 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; Poor crystals, poor data (best of three datasets collected from three separate crystals). The -Me, -BH2 and -NH hydrogen atoms were assigned common isotropic displacement parameters (3 extra LS parameters). ; _diffrn_ambient_temperature 260(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_reflns_number 41471 _diffrn_reflns_av_R_equivalents 0.0555 _diffrn_reflns_av_sigmaI/netI 0.0551 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 26.02 _reflns_number_total 6857 _reflns_number_gt 4171 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 1(5) _refine_ls_number_reflns 6857 _refine_ls_number_parameters 688 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1696 _refine_ls_R_factor_gt 0.1236 _refine_ls_wR_factor_ref 0.3858 _refine_ls_wR_factor_gt 0.3639 _refine_ls_goodness_of_fit_ref 1.429 _refine_ls_restrained_S_all 1.429 _refine_ls_shift/su_max 0.005 _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 B11 B 0.0692(4) 0.0534(5) 0.0629(2) 0.0377(18) Uani 1 1 d . . . H11X H 0.0581 0.0171 0.0865 0.070(5) Uiso 1 1 calc R . . H11Y H 0.1198 0.1003 0.0680 0.070(5) Uiso 1 1 calc R . . N11 N 0.0711(3) 0.0132(3) 0.01861(16) 0.0329(12) Uani 1 1 d . . . H11 H 0.0671 0.0432 -0.0025 0.061(7) Uiso 1 1 calc R . . B12 B -0.0052(5) -0.0713(5) 0.0145(3) 0.0406(18) Uani 1 1 d . . . H12X H -0.0183 -0.0844 -0.0155 0.070(5) Uiso 1 1 calc R . . H12Y H 0.0045 -0.1108 0.0273 0.070(5) Uiso 1 1 calc R . . N12 N -0.0755(3) -0.0703(3) 0.03824(16) 0.0353(13) Uani 1 1 d . . . H12 H -0.0666 -0.0719 0.0668 0.061(7) Uiso 1 1 calc R . . B13 B -0.0730(5) 0.0104(5) 0.0305(2) 0.0400(19) Uani 1 1 d . . . H13X H -0.1216 0.0073 0.0400 0.070(5) Uiso 1 1 calc R . . H13Y H -0.0654 0.0243 0.0003 0.070(5) Uiso 1 1 calc R . . N13 N 0.0021(3) 0.0757(3) 0.05897(14) 0.0294(12) Uani 1 1 d . . . H13 H -0.0175 0.0689 0.0861 0.061(7) Uiso 1 1 calc R . . C110 C 0.1481(4) 0.0138(4) 0.0102(2) 0.0383(15) Uani 1 1 d . . . C111 C 0.1399(4) -0.0355(4) -0.0273(2) 0.0435(17) Uani 1 1 d . . . H11A H 0.0999 -0.0890 -0.0217 0.087(3) Uiso 1 1 calc R . . H11B H 0.1892 -0.0335 -0.0327 0.087(3) Uiso 1 1 calc R . . H11C H 0.1254 -0.0163 -0.0520 0.087(3) Uiso 1 1 calc R . . C112 C 0.2138(4) 0.0996(4) 0.0007(3) 0.055(2) Uani 1 1 d . . . H11D H 0.2618 0.1002 -0.0065 0.087(3) Uiso 1 1 calc R . . H11E H 0.2223 0.1317 0.0257 0.087(3) Uiso 1 1 calc R . . H11F H 0.1981 0.1202 -0.0229 0.087(3) Uiso 1 1 calc R . . C113 C 0.1717(4) -0.0170(5) 0.0492(2) 0.0488(19) Uani 1 1 d . . . H11G H 0.1284 -0.0673 0.0575 0.087(3) Uiso 1 1 calc R . . H11H H 0.1852 0.0195 0.0725 0.087(3) Uiso 1 1 calc R . . H11I H 0.2164 -0.0225 0.0421 0.087(3) Uiso 1 1 calc R . . C120 C -0.1579(4) -0.1437(4) 0.0292(2) 0.0427(18) Uani 1 1 d . . . C121 C -0.2115(4) -0.1485(4) 0.0664(2) 0.0503(19) Uani 1 1 d . . . H12A H -0.2656 -0.1781 0.0575 0.087(3) Uiso 1 1 calc R . . H12B H -0.1992 -0.0962 0.0745 0.087(3) Uiso 1 1 calc R . . H12C H -0.2031 -0.1740 0.0905 0.087(3) Uiso 1 1 calc R . . C122 C -0.1511(5) -0.2161(4) 0.0305(3) 0.055(2) Uani 1 1 d . . . H12D H -0.2025 -0.2618 0.0273 0.087(3) Uiso 1 1 calc R . . H12E H -0.1288 -0.2186 0.0574 0.087(3) Uiso 1 1 calc R . . H12F H -0.1178 -0.2146 0.0075 0.087(3) Uiso 1 1 calc R . . C123 C -0.1898(4) -0.1349(4) -0.0126(2) 0.0445(17) Uani 1 1 d . . . H12G H -0.2446 -0.1740 -0.0146 0.087(3) Uiso 1 1 calc R . . H12H H -0.1614 -0.1418 -0.0357 0.087(3) Uiso 1 1 calc R . . H12I H -0.1839 -0.0833 -0.0142 0.087(3) Uiso 1 1 calc R . . C130 C 0.0293(4) 0.1640(4) 0.0486(2) 0.0387(16) Uani 1 1 d . . . C131 C 0.0753(4) 0.2143(4) 0.0861(2) 0.0446(17) Uani 1 1 d . . . H13A H 0.0938 0.2687 0.0797 0.087(3) Uiso 1 1 calc R . . H13B H 0.1195 0.2070 0.0917 0.087(3) Uiso 1 1 calc R . . H13C H 0.0420 0.1991 0.1110 0.087(3) Uiso 1 1 calc R . . C132 C 0.0760(5) 0.1873(4) 0.0071(2) 0.053(2) Uani 1 1 d . . . H13D H 0.0867 0.2388 -0.0014 0.087(3) Uiso 1 1 calc R . . H13E H 0.0461 0.1499 -0.0149 0.087(3) Uiso 1 1 calc R . . H13F H 0.1248 0.1879 0.0114 0.087(3) Uiso 1 1 calc R . . C133 C -0.0446(4) 0.1717(4) 0.0424(3) 0.0503(19) Uani 1 1 d . . . H13G H -0.0290 0.2246 0.0340 0.087(3) Uiso 1 1 calc R . . H13H H -0.0734 0.1595 0.0689 0.087(3) Uiso 1 1 calc R . . H13I H -0.0774 0.1357 0.0206 0.087(3) Uiso 1 1 calc R . . B21 B 0.4298(6) 0.5110(6) 0.0704(5) 0.082(4) Uani 1 1 d . . . H21X H 0.4356 0.5267 0.1003 0.070(5) Uiso 1 1 calc R . . H21Y H 0.3799 0.5038 0.0601 0.070(5) Uiso 1 1 calc R . . N21 N 0.5014(3) 0.5784(3) 0.0425(3) 0.0568(19) Uani 1 1 d . . . H21 H 0.4870 0.5674 0.0145 0.061(7) Uiso 1 1 calc R . . B22 B 0.5790(5) 0.5728(5) 0.0482(4) 0.066(3) Uani 1 1 d . . . H22X H 0.6239 0.6195 0.0365 0.070(5) Uiso 1 1 calc R . . H22Y H 0.5887 0.5693 0.0784 0.070(5) Uiso 1 1 calc R . . N22 N 0.5682(4) 0.5005(4) 0.0250(3) 0.083(3) Uani 1 1 d . . . H22 H 0.5780 0.5168 -0.0028 0.061(7) Uiso 1 1 calc R . . B23 B 0.4766(6) 0.4326(6) 0.0240(5) 0.083(4) Uani 1 1 d . . . H23X H 0.4513 0.4411 -0.0006 0.070(5) Uiso 1 1 calc R . . H23Y H 0.4731 0.3818 0.0205 0.070(5) Uiso 1 1 calc R . . N23 N 0.4315(3) 0.4314(3) 0.0658(3) 0.0608(19) Uani 1 1 d . . . H23 H 0.4622 0.4318 0.0878 0.061(7) Uiso 1 1 calc R . . C210 C 0.5142(5) 0.6627(5) 0.0513(3) 0.068(3) Uani 1 1 d . . . C211 C 0.5583(6) 0.6933(6) 0.0940(4) 0.082(3) Uani 1 1 d . . . H21A H 0.5634 0.7435 0.1005 0.087(3) Uiso 1 1 calc R . . H21B H 0.6098 0.6990 0.0916 0.087(3) Uiso 1 1 calc R . . H21C H 0.5294 0.6566 0.1165 0.087(3) Uiso 1 1 calc R . . C212 C 0.5617(5) 0.7134(5) 0.0127(4) 0.077(3) Uani 1 1 d . . . H21D H 0.5689 0.7654 0.0155 0.087(3) Uiso 1 1 calc R . . H21E H 0.5336 0.6898 -0.0134 0.087(3) Uiso 1 1 calc R . . H21F H 0.6123 0.7167 0.0118 0.087(3) Uiso 1 1 calc R . . C213 C 0.4354(6) 0.6603(6) 0.0538(3) 0.075(3) Uani 1 1 d . . . H21G H 0.4440 0.7112 0.0623 0.087(3) Uiso 1 1 calc R . . H21H H 0.4021 0.6216 0.0745 0.087(3) Uiso 1 1 calc R . . H21I H 0.4104 0.6468 0.0261 0.087(3) Uiso 1 1 calc R . . C220 C 0.6274(6) 0.4736(6) 0.0335(4) 0.073(3) Uani 1 1 d . . . C221 C 0.6039(7) 0.4252(6) 0.0753(4) 0.091(3) Uani 1 1 d . . . H22A H 0.6388 0.4048 0.0802 0.087(3) Uiso 1 1 calc R . . H22B H 0.5507 0.3822 0.0730 0.087(3) Uiso 1 1 calc R . . H22C H 0.6075 0.4583 0.0989 0.087(3) Uiso 1 1 calc R . . C222 C 0.7091(5) 0.5462(6) 0.0363(4) 0.091(4) Uani 1 1 d . . . H22D H 0.7462 0.5311 0.0457 0.087(3) Uiso 1 1 calc R . . H22E H 0.7081 0.5830 0.0563 0.087(3) Uiso 1 1 calc R . . H22F H 0.7244 0.5705 0.0085 0.087(3) Uiso 1 1 calc R . . C223 C 0.6236(6) 0.4252(7) -0.0039(4) 0.096(4) Uani 1 1 d . . . H22G H 0.6731 0.4268 -0.0071 0.087(3) Uiso 1 1 calc R . . H22H H 0.6126 0.4456 -0.0294 0.087(3) Uiso 1 1 calc R . . H22I H 0.5825 0.3717 0.0005 0.087(3) Uiso 1 1 calc R . . C230 C 0.3520(5) 0.3565(6) 0.0723(4) 0.087(3) Uani 1 1 d . . . C231 C 0.3124(5) 0.3682(6) 0.1124(4) 0.087(3) Uani 1 1 d . . . H23A H 0.2646 0.3200 0.1187 0.087(3) Uiso 1 1 calc R . . H23B H 0.3004 0.4093 0.1070 0.087(3) Uiso 1 1 calc R . . H23C H 0.3476 0.3825 0.1364 0.087(3) Uiso 1 1 calc R . . C232 C 0.3032(7) 0.3341(7) 0.0318(5) 0.111(4) Uani 1 1 d . . . H23D H 0.3324 0.3286 0.0087 0.087(3) Uiso 1 1 calc R . . H23E H 0.2908 0.3744 0.0249 0.087(3) Uiso 1 1 calc R . . H23F H 0.2552 0.2850 0.0362 0.087(3) Uiso 1 1 calc R . . C233 C 0.3691(6) 0.2891(5) 0.0817(4) 0.094(3) Uani 1 1 d . . . H23G H 0.3984 0.2843 0.0583 0.087(3) Uiso 1 1 calc R . . H23H H 0.3203 0.2405 0.0851 0.087(3) Uiso 1 1 calc R . . H23I H 0.3994 0.3006 0.1076 0.087(3) Uiso 1 1 calc R . . B31 B 1.0701(5) 0.5527(6) 0.0225(4) 0.073(3) Uani 1 1 d . . . H31X H 1.0633 0.5214 -0.0029 0.070(5) Uiso 1 1 calc R . . H31Y H 1.1205 0.6010 0.0202 0.070(5) Uiso 1 1 calc R . . N31 N 1.0714(4) 0.5085(4) 0.0608(3) 0.081(3) Uani 1 1 d . . . H31 H 1.0689 0.5375 0.0829 0.061(7) Uiso 1 1 calc R . . B32 B 0.9907(5) 0.4251(7) 0.0662(6) 0.100(5) Uani 1 1 d . . . H32X H 0.9965 0.3835 0.0528 0.070(5) Uiso 1 1 calc R . . H32Y H 0.9796 0.4126 0.0964 0.070(5) Uiso 1 1 calc R . . N32 N 0.9216(5) 0.4299(4) 0.0448(4) 0.094(3) Uani 1 1 d . . . H32 H 0.9281 0.4278 0.0160 0.061(7) Uiso 1 1 calc R . . B33 B 0.9311(6) 0.5149(6) 0.0538(5) 0.081(4) Uani 1 1 d . . . H33X H 0.8832 0.5152 0.0463 0.070(5) Uiso 1 1 calc R . . H33Y H 0.9430 0.5292 0.0838 0.070(5) Uiso 1 1 calc R . . N33 N 1.0022(4) 0.5740(3) 0.0241(2) 0.0546(18) Uani 1 1 d . . . H33 H 0.9817 0.5634 -0.0029 0.061(7) Uiso 1 1 calc R . . C310 C 1.1467(5) 0.5049(5) 0.0711(4) 0.081(3) Uani 1 1 d . . . C311 C 1.1608(6) 0.4689(7) 0.0321(4) 0.093(4) Uani 1 1 d . . . H31A H 1.1655 0.5002 0.0074 0.087(3) Uiso 1 1 calc R . . H31B H 1.1174 0.4164 0.0283 0.087(3) Uiso 1 1 calc R . . H31C H 1.2085 0.4671 0.0358 0.087(3) Uiso 1 1 calc R . . C312 C 1.1374(6) 0.4544(6) 0.1118(5) 0.103(4) Uani 1 1 d . . . H31D H 1.1800 0.4436 0.1130 0.087(3) Uiso 1 1 calc R . . H31E H 1.0882 0.4056 0.1104 0.087(3) Uiso 1 1 calc R . . H31F H 1.1381 0.4829 0.1370 0.087(3) Uiso 1 1 calc R . . C313 C 1.2120(5) 0.5875(6) 0.0810(5) 0.106(4) Uani 1 1 d . . . H31G H 1.2147 0.6226 0.0587 0.087(3) Uiso 1 1 calc R . . H31H H 1.2613 0.5882 0.0825 0.087(3) Uiso 1 1 calc R . . H31I H 1.2017 0.6041 0.1080 0.087(3) Uiso 1 1 calc R . . C320 C 0.8412(5) 0.3628(6) 0.0547(4) 0.085(4) Uani 1 1 d . . . C321 C 0.7859(5) 0.3575(7) 0.0199(4) 0.094(3) Uani 1 1 d . . . H32A H 0.7902 0.4081 0.0160 0.087(3) Uiso 1 1 calc R . . H32B H 0.7329 0.3196 0.0278 0.087(3) Uiso 1 1 calc R . . H32C H 0.7993 0.3415 -0.0064 0.087(3) Uiso 1 1 calc R . . C322 C 0.8405(6) 0.2850(4) 0.0590(4) 0.076(3) Uani 1 1 d . . . H32D H 0.8911 0.2949 0.0686 0.087(3) Uiso 1 1 calc R . . H32E H 0.8288 0.2590 0.0316 0.087(3) Uiso 1 1 calc R . . H32F H 0.8009 0.2520 0.0794 0.087(3) Uiso 1 1 calc R . . C323 C 0.8099(6) 0.3733(5) 0.0978(4) 0.092(4) Uani 1 1 d . . . H32G H 0.8475 0.3823 0.1200 0.087(3) Uiso 1 1 calc R . . H32H H 0.7609 0.3265 0.1043 0.087(3) Uiso 1 1 calc R . . H32I H 0.8016 0.4175 0.0962 0.087(3) Uiso 1 1 calc R . . C330 C 1.0256(6) 0.6597(4) 0.0314(4) 0.071(3) Uani 1 1 d . . . C331 C 0.9566(7) 0.6708(6) 0.0371(4) 0.095(4) Uani 1 1 d . . . H33A H 0.9355 0.6546 0.0654 0.087(3) Uiso 1 1 calc R . . H33B H 0.9169 0.6396 0.0163 0.087(3) Uiso 1 1 calc R . . H33C H 0.9727 0.7254 0.0331 0.087(3) Uiso 1 1 calc R . . C332 C 1.0775(6) 0.6858(5) 0.0739(4) 0.088(3) Uani 1 1 d . . . H33D H 1.0477 0.6514 0.0970 0.087(3) Uiso 1 1 calc R . . H33E H 1.0917 0.7390 0.0809 0.087(3) Uiso 1 1 calc R . . H33F H 1.1243 0.6827 0.0693 0.087(3) Uiso 1 1 calc R . . C333 C 1.0751(7) 0.7087(6) -0.0053(4) 0.094(4) Uani 1 1 d . . . H33G H 1.0439 0.6941 -0.0310 0.087(3) Uiso 1 1 calc R . . H33H H 1.1188 0.7000 -0.0092 0.087(3) Uiso 1 1 calc R . . H33I H 1.0944 0.7634 0.0008 0.087(3) Uiso 1 1 calc R . . B41 B 0.4905(4) -0.0739(4) 0.0494(3) 0.045(2) Uani 1 1 d . . . H41X H 0.4922 -0.1200 0.0396 0.070(5) Uiso 1 1 calc R . . H41Y H 0.4748 -0.0817 0.0794 0.070(5) Uiso 1 1 calc R . . N41 N 0.5746(4) 0.0020(4) 0.0445(2) 0.0521(17) Uani 1 1 d . . . H41 H 0.5760 0.0153 0.0164 0.061(7) Uiso 1 1 calc R . . B42 B 0.4516(5) 0.0276(5) 0.0201(4) 0.062(3) Uani 1 1 d . . . H42X H 0.4863 0.0538 -0.0040 0.070(5) Uiso 1 1 calc R . . H42Y H 0.4044 0.0315 0.0167 0.070(5) Uiso 1 1 calc R . . N42 N 0.4291(4) -0.0631(4) 0.0221(3) 0.082(3) Uani 1 1 d . . . H42 H 0.4362 -0.0748 -0.0052 0.061(7) Uiso 1 1 calc R . . B43 B 0.5789(6) 0.0726(6) 0.0685(4) 0.064(3) Uani 1 1 d . . . H43X H 0.6202 0.1216 0.0564 0.070(5) Uiso 1 1 calc R . . H43Y H 0.5906 0.0708 0.0986 0.070(5) Uiso 1 1 calc R . . N43 N 0.4940(4) 0.0672(5) 0.0633(3) 0.081(3) Uani 1 1 d . . . H43 H 0.4631 0.0342 0.0845 0.061(7) Uiso 1 1 calc R . . C410 C 0.6448(4) -0.0099(4) 0.0488(3) 0.058(2) Uani 1 1 d . . . C411 C 0.6358(6) -0.0533(6) 0.0931(4) 0.082(3) Uani 1 1 d . . . H41A H 0.6352 -0.0211 0.1162 0.087(3) Uiso 1 1 calc R . . H41B H 0.6794 -0.0622 0.0969 0.087(3) Uiso 1 1 calc R . . H41C H 0.5875 -0.1029 0.0932 0.087(3) Uiso 1 1 calc R . . C412 C 0.6478(5) -0.0599(5) 0.0119(4) 0.079(3) Uani 1 1 d . . . H41D H 0.6465 -0.0366 -0.0150 0.087(3) Uiso 1 1 calc R . . H41E H 0.6032 -0.1122 0.0137 0.087(3) Uiso 1 1 calc R . . H41F H 0.6955 -0.0622 0.0138 0.087(3) Uiso 1 1 calc R . . C413 C 0.7225(4) 0.0676(5) 0.0521(3) 0.062(2) Uani 1 1 d . . . H41G H 0.7199 0.0980 0.0755 0.087(3) Uiso 1 1 calc R . . H41H H 0.7318 0.0966 0.0258 0.087(3) Uiso 1 1 calc R . . H41I H 0.7647 0.0569 0.0569 0.087(3) Uiso 1 1 calc R . . C420 C 0.3411(5) -0.1252(6) 0.0328(4) 0.076(3) Uani 1 1 d . . . C421 C 0.3206(6) -0.0987(6) 0.0737(4) 0.099(4) Uani 1 1 d . . . H42A H 0.2720 -0.1407 0.0849 0.087(3) Uiso 1 1 calc R . . H42B H 0.3148 -0.0537 0.0680 0.087(3) Uiso 1 1 calc R . . H42C H 0.3618 -0.0849 0.0944 0.087(3) Uiso 1 1 calc R . . C422 C 0.2891(6) -0.1250(7) -0.0034(4) 0.099(4) Uani 1 1 d . . . H42D H 0.2347 -0.1552 0.0051 0.087(3) Uiso 1 1 calc R . . H42E H 0.2975 -0.1479 -0.0286 0.087(3) Uiso 1 1 calc R . . H42F H 0.3020 -0.0718 -0.0094 0.087(3) Uiso 1 1 calc R . . C423 C 0.3296(6) -0.2046(6) 0.0389(4) 0.098(4) Uani 1 1 d . . . H42G H 0.2793 -0.2429 0.0275 0.087(3) Uiso 1 1 calc R . . H42H H 0.3314 -0.2142 0.0690 0.087(3) Uiso 1 1 calc R . . H42I H 0.3705 -0.2087 0.0243 0.087(3) Uiso 1 1 calc R . . C430 C 0.4942(7) 0.1460(5) 0.0707(4) 0.092(3) Uani 1 1 d . . . C431 C 0.5279(8) 0.1999(6) 0.0340(5) 0.122(5) Uani 1 1 d . . . H43A H 0.5253 0.2468 0.0393 0.087(3) Uiso 1 1 calc R . . H43B H 0.4984 0.1746 0.0085 0.087(3) Uiso 1 1 calc R . . H43C H 0.5818 0.2135 0.0301 0.087(3) Uiso 1 1 calc R . . C432 C 0.4099(7) 0.1263(6) 0.0827(5) 0.111(4) Uani 1 1 d . . . H43D H 0.4123 0.1683 0.0997 0.087(3) Uiso 1 1 calc R . . H43E H 0.3848 0.0782 0.0989 0.087(3) Uiso 1 1 calc R . . H43F H 0.3803 0.1201 0.0571 0.087(3) Uiso 1 1 calc R . . C433 C 0.5463(7) 0.1886(7) 0.1106(5) 0.113(4) Uani 1 1 d . . . H43G H 0.5485 0.2383 0.1147 0.087(3) Uiso 1 1 calc R . . H43H H 0.5986 0.1974 0.1062 0.087(3) Uiso 1 1 calc R . . H43I H 0.5238 0.1564 0.1356 0.087(3) 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 B11 0.044(4) 0.043(4) 0.018(3) -0.007(3) -0.014(3) 0.016(3) N11 0.035(3) 0.041(3) 0.026(3) 0.002(2) -0.008(2) 0.022(3) B12 0.063(5) 0.041(4) 0.030(4) -0.001(3) 0.008(3) 0.035(4) N12 0.029(3) 0.048(3) 0.023(2) 0.002(2) -0.001(2) 0.015(2) B13 0.038(4) 0.062(5) 0.030(4) 0.000(4) -0.001(3) 0.033(4) N13 0.042(3) 0.025(3) 0.015(2) -0.0013(19) 0.001(2) 0.012(2) C110 0.033(3) 0.055(4) 0.030(3) 0.007(3) -0.009(3) 0.024(3) C111 0.044(4) 0.057(4) 0.037(4) -0.006(3) 0.003(3) 0.031(3) C112 0.043(4) 0.065(5) 0.050(4) 0.002(4) 0.011(3) 0.022(4) C113 0.042(4) 0.086(6) 0.034(4) -0.005(4) -0.012(3) 0.043(4) C120 0.044(4) 0.041(4) 0.041(4) 0.010(3) -0.010(3) 0.020(3) C121 0.040(4) 0.053(4) 0.044(4) 0.000(3) -0.016(3) 0.013(3) C122 0.050(4) 0.044(4) 0.069(6) 0.017(4) -0.010(4) 0.022(4) C123 0.044(4) 0.040(4) 0.042(4) 0.008(3) -0.011(3) 0.015(3) C130 0.043(4) 0.044(4) 0.029(3) 0.008(3) -0.002(3) 0.021(3) C131 0.046(4) 0.026(3) 0.051(4) -0.005(3) -0.004(3) 0.009(3) C132 0.070(5) 0.046(4) 0.024(3) 0.015(3) 0.001(3) 0.014(4) C133 0.055(5) 0.041(4) 0.066(5) -0.001(4) -0.005(4) 0.032(4) B21 0.056(6) 0.056(6) 0.150(11) 0.056(7) 0.054(7) 0.039(5) N21 0.024(3) 0.037(3) 0.113(6) 0.007(3) 0.010(3) 0.019(3) B22 0.029(4) 0.039(5) 0.129(10) -0.006(5) -0.014(5) 0.017(4) N22 0.032(3) 0.048(4) 0.173(9) 0.017(5) 0.016(4) 0.023(3) B23 0.044(6) 0.050(6) 0.162(12) 0.010(7) 0.046(7) 0.029(5) N23 0.032(3) 0.036(3) 0.106(5) 0.027(3) 0.000(3) 0.011(3) C210 0.042(4) 0.044(5) 0.115(8) 0.033(5) 0.013(5) 0.020(4) C211 0.089(7) 0.057(6) 0.103(8) -0.007(5) 0.000(6) 0.038(5) C212 0.066(6) 0.049(5) 0.126(9) 0.034(5) 0.012(6) 0.035(5) C213 0.076(6) 0.073(6) 0.095(7) 0.007(5) 0.021(5) 0.052(5) C220 0.078(7) 0.074(6) 0.095(8) 0.026(5) 0.004(5) 0.059(6) C221 0.107(8) 0.058(6) 0.129(9) 0.024(6) 0.013(7) 0.058(6) C222 0.045(5) 0.091(7) 0.153(10) 0.043(7) 0.007(6) 0.046(5) C223 0.075(6) 0.130(10) 0.115(9) 0.061(8) 0.042(6) 0.074(7) C230 0.042(5) 0.068(6) 0.110(8) 0.016(6) 0.020(5) -0.004(4) C231 0.046(5) 0.068(6) 0.102(8) -0.008(5) 0.013(5) -0.004(4) C232 0.063(7) 0.085(8) 0.151(12) -0.006(8) -0.021(7) 0.012(6) C233 0.086(7) 0.050(5) 0.133(10) 0.004(6) 0.017(7) 0.024(5) B31 0.033(5) 0.069(7) 0.120(9) -0.005(6) -0.034(5) 0.029(5) N31 0.036(4) 0.044(4) 0.159(8) 0.010(5) -0.030(4) 0.016(3) B32 0.025(4) 0.073(7) 0.207(15) 0.061(9) 0.035(7) 0.027(5) N32 0.074(5) 0.034(4) 0.177(10) -0.009(5) -0.019(6) 0.030(4) B33 0.044(6) 0.047(5) 0.152(12) 0.009(6) -0.004(6) 0.022(5) N33 0.041(3) 0.024(3) 0.097(5) -0.020(3) -0.030(3) 0.014(3) C310 0.032(4) 0.064(6) 0.150(10) 0.011(6) -0.008(5) 0.027(4) C311 0.057(6) 0.090(8) 0.140(11) 0.013(7) -0.009(6) 0.043(6) C312 0.057(6) 0.067(6) 0.184(12) 0.028(7) -0.034(7) 0.029(5) C313 0.044(5) 0.072(6) 0.182(12) 0.007(7) -0.032(6) 0.013(5) C320 0.034(4) 0.062(6) 0.143(10) 0.055(6) -0.009(5) 0.012(4) C321 0.049(5) 0.100(8) 0.118(9) 0.026(7) -0.010(6) 0.025(5) C322 0.075(6) 0.032(4) 0.106(8) 0.020(5) 0.010(6) 0.015(4) C323 0.055(6) 0.035(5) 0.152(11) 0.005(6) -0.012(7) -0.002(4) C330 0.070(6) 0.016(4) 0.117(8) -0.002(4) 0.015(5) 0.014(4) C331 0.107(9) 0.043(5) 0.141(10) -0.016(6) -0.022(7) 0.043(6) C332 0.079(6) 0.032(4) 0.136(9) -0.003(5) -0.037(6) 0.016(4) C333 0.105(8) 0.063(6) 0.110(9) 0.019(6) -0.012(7) 0.039(6) B41 0.035(4) 0.025(4) 0.078(6) 0.002(4) 0.001(4) 0.017(3) N41 0.045(4) 0.043(4) 0.077(4) -0.005(3) -0.016(3) 0.028(3) B42 0.038(5) 0.046(5) 0.106(8) -0.003(5) -0.003(5) 0.024(4) N42 0.053(4) 0.062(5) 0.133(8) 0.022(5) 0.000(4) 0.030(4) B43 0.051(5) 0.057(6) 0.093(7) 0.000(5) -0.003(5) 0.034(5) N43 0.062(5) 0.061(5) 0.132(7) -0.028(5) -0.026(5) 0.039(4) C410 0.027(4) 0.045(4) 0.114(7) -0.002(4) -0.010(4) 0.028(3) C411 0.061(6) 0.067(6) 0.132(10) 0.008(6) -0.012(6) 0.043(5) C412 0.045(5) 0.063(6) 0.132(9) -0.016(6) 0.014(5) 0.030(4) C413 0.021(3) 0.054(5) 0.102(7) 0.000(4) -0.013(4) 0.012(3) C420 0.044(5) 0.060(6) 0.111(9) -0.024(5) 0.000(5) 0.018(4) C421 0.062(6) 0.057(6) 0.156(11) -0.017(7) -0.037(7) 0.013(5) C422 0.052(6) 0.094(8) 0.145(10) -0.041(7) -0.023(6) 0.032(5) C423 0.052(6) 0.052(6) 0.174(12) 0.005(6) 0.011(7) 0.014(5) C430 0.099(8) 0.051(5) 0.130(9) -0.046(6) -0.016(7) 0.041(5) C431 0.143(12) 0.046(6) 0.191(14) 0.032(7) 0.058(10) 0.058(7) C432 0.093(8) 0.075(7) 0.189(13) -0.022(8) -0.020(9) 0.060(7) C433 0.091(8) 0.094(8) 0.149(11) -0.049(8) -0.035(8) 0.042(7) _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 B11 N13 1.583(10) . ? B11 N11 1.597(9) . ? B11 H11X 0.9700 . ? B11 H11Y 0.9700 . ? N11 C110 1.526(8) . ? N11 B12 1.587(10) . ? N11 H11 0.9100 . ? B12 N12 1.571(9) . ? B12 H12X 0.9700 . ? B12 H12Y 0.9700 . ? N12 C120 1.560(9) . ? N12 B13 1.576(10) . ? N12 H12 0.9100 . ? B13 N13 1.645(9) . ? B13 H13X 0.9700 . ? B13 H13Y 0.9700 . ? N13 C130 1.569(8) . ? N13 H13 0.9100 . ? C110 C111 1.472(9) . ? C110 C113 1.528(9) . ? C110 C112 1.552(10) . ? C111 H11A 0.9600 . ? C111 H11B 0.9600 . ? C111 H11C 0.9600 . ? C112 H11D 0.9600 . ? C112 H11E 0.9600 . ? C112 H11F 0.9600 . ? C113 H11G 0.9600 . ? C113 H11H 0.9600 . ? C113 H11I 0.9600 . ? C120 C122 1.489(10) . ? C120 C123 1.489(9) . ? C120 C121 1.535(11) . ? C121 H12A 0.9600 . ? C121 H12B 0.9600 . ? C121 H12C 0.9600 . ? C122 H12D 0.9600 . ? C122 H12E 0.9600 . ? C122 H12F 0.9600 . ? C123 H12G 0.9600 . ? C123 H12H 0.9600 . ? C123 H12I 0.9600 . ? C130 C131 1.504(10) . ? C130 C132 1.516(10) . ? C130 C133 1.540(10) . ? C131 H13A 0.9600 . ? C131 H13B 0.9600 . ? C131 H13C 0.9600 . ? C132 H13D 0.9600 . ? C132 H13E 0.9600 . ? C132 H13F 0.9600 . ? C133 H13G 0.9600 . ? C133 H13H 0.9600 . ? C133 H13I 0.9600 . ? B21 N23 1.583(12) . ? B21 N21 1.616(11) . ? B21 H21X 0.9700 . ? B21 H21Y 0.9700 . ? N21 C210 1.565(10) . ? N21 B22 1.588(10) . ? N21 H21 0.9100 . ? B22 N22 1.507(13) . ? B22 H22X 0.9700 . ? B22 H22Y 0.9700 . ? N22 C220 1.519(10) . ? N22 B23 1.614(12) . ? N22 H22 0.9100 . ? B23 N23 1.567(14) . ? B23 H23X 0.9700 . ? B23 H23Y 0.9700 . ? N23 C230 1.528(10) . ? N23 H23 0.9100 . ? C210 C213 1.524(11) . ? C210 C211 1.534(14) . ? C210 C212 1.543(13) . ? C211 H21A 0.9600 . ? C211 H21B 0.9600 . ? C211 H21C 0.9600 . ? C212 H21D 0.9600 . ? C212 H21E 0.9600 . ? C212 H21F 0.9600 . ? C213 H21G 0.9600 . ? C213 H21H 0.9600 . ? C213 H21I 0.9600 . ? C220 C223 1.479(15) . ? C220 C222 1.521(14) . ? C220 C221 1.541(15) . ? C221 H22A 0.9600 . ? C221 H22B 0.9600 . ? C221 H22C 0.9600 . ? C222 H22D 0.9600 . ? C222 H22E 0.9600 . ? C222 H22F 0.9600 . ? C223 H22G 0.9600 . ? C223 H22H 0.9600 . ? C223 H22I 0.9600 . ? C230 C232 1.508(17) . ? C230 C233 1.545(14) . ? C230 C231 1.547(15) . ? C231 H23A 0.9600 . ? C231 H23B 0.9600 . ? C231 H23C 0.9600 . ? C232 H23D 0.9600 . ? C232 H23E 0.9600 . ? C232 H23F 0.9600 . ? C233 H23G 0.9600 . ? C233 H23H 0.9600 . ? C233 H23I 0.9600 . ? B31 N31 1.480(14) . ? B31 N33 1.582(11) . ? B31 H31X 0.9700 . ? B31 H31Y 0.9700 . ? N31 C310 1.545(10) . ? N31 B32 1.617(12) . ? N31 H31 0.9100 . ? B32 N32 1.554(13) . ? B32 H32X 0.9700 . ? B32 H32Y 0.9700 . ? N32 C320 1.494(12) . ? N32 B33 1.604(13) . ? N32 H32 0.9100 . ? B33 N33 1.587(14) . ? B33 H33X 0.9700 . ? B33 H33Y 0.9700 . ? N33 C330 1.518(9) . ? N33 H33 0.9100 . ? C310 C311 1.496(17) . ? C310 C313 1.511(13) . ? C310 C312 1.562(16) . ? C311 H31A 0.9600 . ? C311 H31B 0.9600 . ? C311 H31C 0.9600 . ? C312 H31D 0.9600 . ? C312 H31E 0.9600 . ? C312 H31F 0.9600 . ? C313 H31G 0.9600 . ? C313 H31H 0.9600 . ? C313 H31I 0.9600 . ? C320 C321 1.498(14) . ? C320 C322 1.522(12) . ? C320 C323 1.535(17) . ? C321 H32A 0.9600 . ? C321 H32B 0.9600 . ? C321 H32C 0.9600 . ? C322 H32D 0.9600 . ? C322 H32E 0.9600 . ? C322 H32F 0.9600 . ? C323 H32G 0.9600 . ? C323 H32H 0.9600 . ? C323 H32I 0.9600 . ? C330 C331 1.484(13) . ? C330 C333 1.496(14) . ? C330 C332 1.589(15) . ? C331 H33A 0.9600 . ? C331 H33B 0.9600 . ? C331 H33C 0.9600 . ? C332 H33D 0.9600 . ? C332 H33E 0.9600 . ? C332 H33F 0.9600 . ? C333 H33G 0.9600 . ? C333 H33H 0.9600 . ? C333 H33I 0.9600 . ? B41 N42 1.570(12) . ? B41 N41 1.581(10) . ? B41 H41X 0.9700 . ? B41 H41Y 0.9700 . ? N41 C410 1.512(8) . ? N41 B43 1.537(12) . ? N41 H41 0.9100 . ? B42 N43 1.567(14) . ? B42 N42 1.605(11) . ? B42 H42X 0.9700 . ? B42 H42Y 0.9700 . ? N42 C420 1.569(12) . ? N42 H42 0.9100 . ? B43 N43 1.622(11) . ? B43 H43X 0.9700 . ? B43 H43Y 0.9700 . ? N43 C430 1.557(11) . ? N43 H43 0.9100 . ? C410 C413 1.523(10) . ? C410 C412 1.530(13) . ? C410 C411 1.585(14) . ? C411 H41A 0.9600 . ? C411 H41B 0.9600 . ? C411 H41C 0.9600 . ? C412 H41D 0.9600 . ? C412 H41E 0.9600 . ? C412 H41F 0.9600 . ? C413 H41G 0.9600 . ? C413 H41H 0.9600 . ? C413 H41I 0.9600 . ? C420 C423 1.469(14) . ? C420 C421 1.505(15) . ? C420 C422 1.522(15) . ? C421 H42A 0.9600 . ? C421 H42B 0.9600 . ? C421 H42C 0.9600 . ? C422 H42D 0.9600 . ? C422 H42E 0.9600 . ? C422 H42F 0.9600 . ? C423 H42G 0.9600 . ? C423 H42H 0.9600 . ? C423 H42I 0.9600 . ? C430 C431 1.470(18) . ? C430 C432 1.542(15) . ? C430 C433 1.561(16) . ? C431 H43A 0.9600 . ? C431 H43B 0.9600 . ? C431 H43C 0.9600 . ? C432 H43D 0.9600 . ? C432 H43E 0.9600 . ? C432 H43F 0.9600 . ? C433 H43G 0.9600 . ? C433 H43H 0.9600 . ? C433 H43I 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 N13 B11 N11 107.3(5) . . ? N13 B11 H11X 110.3 . . ? N11 B11 H11X 110.3 . . ? N13 B11 H11Y 110.3 . . ? N11 B11 H11Y 110.3 . . ? H11X B11 H11Y 108.5 . . ? C110 N11 B12 114.0(5) . . ? C110 N11 B11 114.3(5) . . ? B12 N11 B11 110.0(5) . . ? C110 N11 H11 105.9 . . ? B12 N11 H11 105.9 . . ? B11 N11 H11 105.9 . . ? N12 B12 N11 108.9(5) . . ? N12 B12 H12X 109.9 . . ? N11 B12 H12X 109.9 . . ? N12 B12 H12Y 109.9 . . ? N11 B12 H12Y 109.9 . . ? H12X B12 H12Y 108.3 . . ? C120 N12 B12 114.4(5) . . ? C120 N12 B13 113.4(5) . . ? B12 N12 B13 110.6(5) . . ? C120 N12 H12 105.9 . . ? B12 N12 H12 105.9 . . ? B13 N12 H12 105.9 . . ? N12 B13 N13 105.3(5) . . ? N12 B13 H13X 110.7 . . ? N13 B13 H13X 110.7 . . ? N12 B13 H13Y 110.7 . . ? N13 B13 H13Y 110.7 . . ? H13X B13 H13Y 108.8 . . ? C130 N13 B11 116.7(5) . . ? C130 N13 B13 115.1(5) . . ? B11 N13 B13 111.7(5) . . ? C130 N13 H13 103.8 . . ? B11 N13 H13 103.8 . . ? B13 N13 H13 103.8 . . ? C111 C110 N11 110.4(5) . . ? C111 C110 C113 109.1(6) . . ? N11 C110 C113 110.6(5) . . ? C111 C110 C112 108.7(6) . . ? N11 C110 C112 108.8(5) . . ? C113 C110 C112 109.1(6) . . ? C110 C111 H11A 109.5 . . ? C110 C111 H11B 109.5 . . ? H11A C111 H11B 109.5 . . ? C110 C111 H11C 109.5 . . ? H11A C111 H11C 109.5 . . ? H11B C111 H11C 109.5 . . ? C110 C112 H11D 109.5 . . ? C110 C112 H11E 109.5 . . ? H11D C112 H11E 109.5 . . ? C110 C112 H11F 109.5 . . ? H11D C112 H11F 109.5 . . ? H11E C112 H11F 109.5 . . ? C110 C113 H11G 109.5 . . ? C110 C113 H11H 109.5 . . ? H11G C113 H11H 109.5 . . ? C110 C113 H11I 109.5 . . ? H11G C113 H11I 109.5 . . ? H11H C113 H11I 109.5 . . ? C122 C120 C123 112.1(6) . . ? C122 C120 C121 107.8(6) . . ? C123 C120 C121 110.7(6) . . ? C122 C120 N12 109.2(6) . . ? C123 C120 N12 110.6(5) . . ? C121 C120 N12 106.2(5) . . ? C120 C121 H12A 109.5 . . ? C120 C121 H12B 109.5 . . ? H12A C121 H12B 109.5 . . ? C120 C121 H12C 109.5 . . ? H12A C121 H12C 109.5 . . ? H12B C121 H12C 109.5 . . ? C120 C122 H12D 109.5 . . ? C120 C122 H12E 109.5 . . ? H12D C122 H12E 109.5 . . ? C120 C122 H12F 109.5 . . ? H12D C122 H12F 109.5 . . ? H12E C122 H12F 109.5 . . ? C120 C123 H12G 109.5 . . ? C120 C123 H12H 109.5 . . ? H12G C123 H12H 109.5 . . ? C120 C123 H12I 109.5 . . ? H12G C123 H12I 109.5 . . ? H12H C123 H12I 109.5 . . ? C131 C130 C132 113.1(6) . . ? C131 C130 C133 108.5(6) . . ? C132 C130 C133 108.7(6) . . ? C131 C130 N13 108.8(5) . . ? C132 C130 N13 109.2(6) . . ? C133 C130 N13 108.4(5) . . ? C130 C131 H13A 109.5 . . ? C130 C131 H13B 109.5 . . ? H13A C131 H13B 109.5 . . ? C130 C131 H13C 109.5 . . ? H13A C131 H13C 109.5 . . ? H13B C131 H13C 109.5 . . ? C130 C132 H13D 109.5 . . ? C130 C132 H13E 109.5 . . ? H13D C132 H13E 109.5 . . ? C130 C132 H13F 109.5 . . ? H13D C132 H13F 109.5 . . ? H13E C132 H13F 109.5 . . ? C130 C133 H13G 109.5 . . ? C130 C133 H13H 109.5 . . ? H13G C133 H13H 109.5 . . ? C130 C133 H13I 109.5 . . ? H13G C133 H13I 109.5 . . ? H13H C133 H13I 109.5 . . ? N23 B21 N21 108.5(7) . . ? N23 B21 H21X 110.0 . . ? N21 B21 H21X 110.0 . . ? N23 B21 H21Y 110.0 . . ? N21 B21 H21Y 110.0 . . ? H21X B21 H21Y 108.4 . . ? C210 N21 B22 113.5(6) . . ? C210 N21 B21 112.5(7) . . ? B22 N21 B21 110.7(7) . . ? C210 N21 H21 106.5 . . ? B22 N21 H21 106.5 . . ? B21 N21 H21 106.5 . . ? N22 B22 N21 108.8(7) . . ? N22 B22 H22X 109.9 . . ? N21 B22 H22X 109.9 . . ? N22 B22 H22Y 109.9 . . ? N21 B22 H22Y 109.9 . . ? H22X B22 H22Y 108.3 . . ? B22 N22 C220 118.1(8) . . ? B22 N22 B23 111.0(6) . . ? C220 N22 B23 116.4(7) . . ? B22 N22 H22 102.9 . . ? C220 N22 H22 102.9 . . ? B23 N22 H22 102.9 . . ? N23 B23 N22 112.5(10) . . ? N23 B23 H23X 109.1 . . ? N22 B23 H23X 109.1 . . ? N23 B23 H23Y 109.1 . . ? N22 B23 H23Y 109.1 . . ? H23X B23 H23Y 107.8 . . ? C230 N23 B23 114.9(8) . . ? C230 N23 B21 114.9(7) . . ? B23 N23 B21 110.5(7) . . ? C230 N23 H23 105.1 . . ? B23 N23 H23 105.1 . . ? B21 N23 H23 105.1 . . ? C213 C210 C211 109.4(9) . . ? C213 C210 C212 109.5(7) . . ? C211 C210 C212 112.6(7) . . ? C213 C210 N21 110.6(7) . . ? C211 C210 N21 109.0(7) . . ? C212 C210 N21 105.7(8) . . ? C210 C211 H21A 109.5 . . ? C210 C211 H21B 109.5 . . ? H21A C211 H21B 109.5 . . ? C210 C211 H21C 109.5 . . ? H21A C211 H21C 109.5 . . ? H21B C211 H21C 109.5 . . ? C210 C212 H21D 109.5 . . ? C210 C212 H21E 109.5 . . ? H21D C212 H21E 109.5 . . ? C210 C212 H21F 109.5 . . ? H21D C212 H21F 109.5 . . ? H21E C212 H21F 109.5 . . ? C210 C213 H21G 109.5 . . ? C210 C213 H21H 109.5 . . ? H21G C213 H21H 109.5 . . ? C210 C213 H21I 109.5 . . ? H21G C213 H21I 109.5 . . ? H21H C213 H21I 109.5 . . ? C223 C220 N22 106.4(8) . . ? C223 C220 C222 109.7(9) . . ? N22 C220 C222 108.2(7) . . ? C223 C220 C221 111.6(8) . . ? N22 C220 C221 108.4(8) . . ? C222 C220 C221 112.2(9) . . ? C220 C221 H22A 109.5 . . ? C220 C221 H22B 109.5 . . ? H22A C221 H22B 109.5 . . ? C220 C221 H22C 109.5 . . ? H22A C221 H22C 109.5 . . ? H22B C221 H22C 109.5 . . ? C220 C222 H22D 109.5 . . ? C220 C222 H22E 109.5 . . ? H22D C222 H22E 109.5 . . ? C220 C222 H22F 109.5 . . ? H22D C222 H22F 109.5 . . ? H22E C222 H22F 109.5 . . ? C220 C223 H22G 109.5 . . ? C220 C223 H22H 109.5 . . ? H22G C223 H22H 109.5 . . ? C220 C223 H22I 109.5 . . ? H22G C223 H22I 109.5 . . ? H22H C223 H22I 109.5 . . ? C232 C230 N23 111.2(9) . . ? C232 C230 C233 106.7(10) . . ? N23 C230 C233 107.0(7) . . ? C232 C230 C231 115.2(9) . . ? N23 C230 C231 108.1(8) . . ? C233 C230 C231 108.2(9) . . ? C230 C231 H23A 109.5 . . ? C230 C231 H23B 109.5 . . ? H23A C231 H23B 109.5 . . ? C230 C231 H23C 109.5 . . ? H23A C231 H23C 109.5 . . ? H23B C231 H23C 109.5 . . ? C230 C232 H23D 109.5 . . ? C230 C232 H23E 109.5 . . ? H23D C232 H23E 109.5 . . ? C230 C232 H23F 109.5 . . ? H23D C232 H23F 109.5 . . ? H23E C232 H23F 109.5 . . ? C230 C233 H23G 109.5 . . ? C230 C233 H23H 109.5 . . ? H23G C233 H23H 109.5 . . ? C230 C233 H23I 109.5 . . ? H23G C233 H23I 109.5 . . ? H23H C233 H23I 109.5 . . ? N31 B31 N33 113.1(9) . . ? N31 B31 H31X 109.0 . . ? N33 B31 H31X 109.0 . . ? N31 B31 H31Y 109.0 . . ? N33 B31 H31Y 109.0 . . ? H31X B31 H31Y 107.8 . . ? B31 N31 C310 119.3(8) . . ? B31 N31 B32 112.4(8) . . ? C310 N31 B32 113.9(6) . . ? B31 N31 H31 102.8 . . ? C310 N31 H31 102.8 . . ? B32 N31 H31 102.8 . . ? N32 B32 N31 109.6(7) . . ? N32 B32 H32X 109.8 . . ? N31 B32 H32X 109.8 . . ? N32 B32 H32Y 109.8 . . ? N31 B32 H32Y 109.8 . . ? H32X B32 H32Y 108.2 . . ? C320 N32 B32 115.2(7) . . ? C320 N32 B33 113.8(8) . . ? B32 N32 B33 109.7(8) . . ? C320 N32 H32 105.8 . . ? B32 N32 H32 105.8 . . ? B33 N32 H32 105.8 . . ? N33 B33 N32 105.1(9) . . ? N33 B33 H33X 110.7 . . ? N32 B33 H33X 110.7 . . ? N33 B33 H33Y 110.7 . . ? N32 B33 H33Y 110.7 . . ? H33X B33 H33Y 108.8 . . ? C330 N33 B31 117.8(6) . . ? C330 N33 B33 112.9(7) . . ? B31 N33 B33 111.8(7) . . ? C330 N33 H33 104.2 . . ? B31 N33 H33 104.2 . . ? B33 N33 H33 104.2 . . ? C311 C310 C313 114.4(10) . . ? C311 C310 N31 105.0(9) . . ? C313 C310 N31 108.1(7) . . ? C311 C310 C312 110.6(8) . . ? C313 C310 C312 106.3(10) . . ? N31 C310 C312 112.7(8) . . ? C310 C311 H31A 109.5 . . ? C310 C311 H31B 109.5 . . ? H31A C311 H31B 109.5 . . ? C310 C311 H31C 109.5 . . ? H31A C311 H31C 109.5 . . ? H31B C311 H31C 109.5 . . ? C310 C312 H31D 109.5 . . ? C310 C312 H31E 109.5 . . ? H31D C312 H31E 109.5 . . ? C310 C312 H31F 109.5 . . ? H31D C312 H31F 109.5 . . ? H31E C312 H31F 109.5 . . ? C310 C313 H31G 109.5 . . ? C310 C313 H31H 109.5 . . ? H31G C313 H31H 109.5 . . ? C310 C313 H31I 109.5 . . ? H31G C313 H31I 109.5 . . ? H31H C313 H31I 109.5 . . ? N32 C320 C321 108.7(8) . . ? N32 C320 C322 112.2(8) . . ? C321 C320 C322 110.5(10) . . ? N32 C320 C323 112.2(10) . . ? C321 C320 C323 108.6(9) . . ? C322 C320 C323 104.6(8) . . ? C320 C321 H32A 109.5 . . ? C320 C321 H32B 109.5 . . ? H32A C321 H32B 109.5 . . ? C320 C321 H32C 109.5 . . ? H32A C321 H32C 109.5 . . ? H32B C321 H32C 109.5 . . ? C320 C322 H32D 109.5 . . ? C320 C322 H32E 109.5 . . ? H32D C322 H32E 109.5 . . ? C320 C322 H32F 109.5 . . ? H32D C322 H32F 109.5 . . ? H32E C322 H32F 109.5 . . ? C320 C323 H32G 109.5 . . ? C320 C323 H32H 109.5 . . ? H32G C323 H32H 109.5 . . ? C320 C323 H32I 109.5 . . ? H32G C323 H32I 109.5 . . ? H32H C323 H32I 109.5 . . ? C331 C330 C333 110.0(9) . . ? C331 C330 N33 112.7(7) . . ? C333 C330 N33 109.7(8) . . ? C331 C330 C332 109.7(9) . . ? C333 C330 C332 108.9(8) . . ? N33 C330 C332 105.8(7) . . ? C330 C331 H33A 109.5 . . ? C330 C331 H33B 109.5 . . ? H33A C331 H33B 109.5 . . ? C330 C331 H33C 109.5 . . ? H33A C331 H33C 109.5 . . ? H33B C331 H33C 109.5 . . ? C330 C332 H33D 109.5 . . ? C330 C332 H33E 109.5 . . ? H33D C332 H33E 109.5 . . ? C330 C332 H33F 109.5 . . ? H33D C332 H33F 109.5 . . ? H33E C332 H33F 109.5 . . ? C330 C333 H33G 109.5 . . ? C330 C333 H33H 109.5 . . ? H33G C333 H33H 109.5 . . ? C330 C333 H33I 109.5 . . ? H33G C333 H33I 109.5 . . ? H33H C333 H33I 109.5 . . ? N42 B41 N41 109.2(6) . . ? N42 B41 H41X 109.8 . . ? N41 B41 H41X 109.8 . . ? N42 B41 H41Y 109.8 . . ? N41 B41 H41Y 109.8 . . ? H41X B41 H41Y 108.3 . . ? C410 N41 B43 116.8(6) . . ? C410 N41 B41 116.6(5) . . ? B43 N41 B41 111.2(6) . . ? C410 N41 H41 103.3 . . ? B43 N41 H41 103.3 . . ? B41 N41 H41 103.3 . . ? N43 B42 N42 107.4(8) . . ? N43 B42 H42X 110.2 . . ? N42 B42 H42X 110.2 . . ? N43 B42 H42Y 110.2 . . ? N42 B42 H42Y 110.2 . . ? H42X B42 H42Y 108.5 . . ? C420 N42 B41 113.5(7) . . ? C420 N42 B42 116.9(7) . . ? B41 N42 B42 111.4(7) . . ? C420 N42 H42 104.5 . . ? B41 N42 H42 104.5 . . ? B42 N42 H42 104.5 . . ? N41 B43 N43 107.5(7) . . ? N41 B43 H43X 110.2 . . ? N43 B43 H43X 110.2 . . ? N41 B43 H43Y 110.2 . . ? N43 B43 H43Y 110.2 . . ? H43X B43 H43Y 108.5 . . ? C430 N43 B42 110.8(7) . . ? C430 N43 B43 115.2(7) . . ? B42 N43 B43 112.9(7) . . ? C430 N43 H43 105.7 . . ? B42 N43 H43 105.7 . . ? B43 N43 H43 105.7 . . ? N41 C410 C413 112.6(6) . . ? N41 C410 C412 111.1(7) . . ? C413 C410 C412 110.4(7) . . ? N41 C410 C411 107.1(7) . . ? C413 C410 C411 105.3(7) . . ? C412 C410 C411 110.0(7) . . ? C410 C411 H41A 109.5 . . ? C410 C411 H41B 109.5 . . ? H41A C411 H41B 109.5 . . ? C410 C411 H41C 109.5 . . ? H41A C411 H41C 109.5 . . ? H41B C411 H41C 109.5 . . ? C410 C412 H41D 109.5 . . ? C410 C412 H41E 109.5 . . ? H41D C412 H41E 109.5 . . ? C410 C412 H41F 109.5 . . ? H41D C412 H41F 109.5 . . ? H41E C412 H41F 109.5 . . ? C410 C413 H41G 109.5 . . ? C410 C413 H41H 109.5 . . ? H41G C413 H41H 109.5 . . ? C410 C413 H41I 109.5 . . ? H41G C413 H41I 109.5 . . ? H41H C413 H41I 109.5 . . ? C423 C420 C421 109.2(10) . . ? C423 C420 C422 110.5(9) . . ? C421 C420 C422 109.4(8) . . ? C423 C420 N42 112.1(7) . . ? C421 C420 N42 107.0(8) . . ? C422 C420 N42 108.6(9) . . ? C420 C421 H42A 109.5 . . ? C420 C421 H42B 109.5 . . ? H42A C421 H42B 109.5 . . ? C420 C421 H42C 109.5 . . ? H42A C421 H42C 109.5 . . ? H42B C421 H42C 109.5 . . ? C420 C422 H42D 109.5 . . ? C420 C422 H42E 109.5 . . ? H42D C422 H42E 109.5 . . ? C420 C422 H42F 109.5 . . ? H42D C422 H42F 109.5 . . ? H42E C422 H42F 109.5 . . ? C420 C423 H42G 109.5 . . ? C420 C423 H42H 109.5 . . ? H42G C423 H42H 109.5 . . ? C420 C423 H42I 109.5 . . ? H42G C423 H42I 109.5 . . ? H42H C423 H42I 109.5 . . ? C431 C430 C432 114.1(11) . . ? C431 C430 N43 112.1(9) . . ? C432 C430 N43 108.4(8) . . ? C431 C430 C433 107.3(10) . . ? C432 C430 C433 105.7(10) . . ? N43 C430 C433 109.0(10) . . ? C430 C431 H43A 109.5 . . ? C430 C431 H43B 109.5 . . ? H43A C431 H43B 109.5 . . ? C430 C431 H43C 109.5 . . ? H43A C431 H43C 109.5 . . ? H43B C431 H43C 109.5 . . ? C430 C432 H43D 109.5 . . ? C430 C432 H43E 109.5 . . ? H43D C432 H43E 109.5 . . ? C430 C432 H43F 109.5 . . ? H43D C432 H43F 109.5 . . ? H43E C432 H43F 109.5 . . ? C430 C433 H43G 109.5 . . ? C430 C433 H43H 109.5 . . ? H43G C433 H43H 109.5 . . ? C430 C433 H43I 109.5 . . ? H43G C433 H43I 109.5 . . ? H43H C433 H43I 109.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.545 _refine_diff_density_min -0.368 _refine_diff_density_rms 0.070 # Attachment '- compound9.cif' data_dw1117 _database_code_depnum_ccdc_archive 'CCDC 817720' #TrackingRef '- compound9.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H105 B4 N9 Si12, C4 H8 O' _chemical_formula_sum 'C37 H113 B4 N9 O Si12' _chemical_formula_weight 1080.68 _chemical_absolute_configuration ; 2879 Friedel pairs were averaged for the refinement ; 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' Si Si 0.0817 0.0704 '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' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M P6(3) _symmetry_space_group_name_Hall 'P 6c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' _cell_length_a 29.3467(5) _cell_length_b 29.3467(5) _cell_length_c 14.9405(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 11143.3(4) _cell_formula_units_Z 6 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 13468 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 22.46 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.966 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3564 _exptl_absorpt_coefficient_mu 0.240 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.781 _exptl_absorpt_correction_T_max 0.901 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; Poor data (theta(max)=22.5 degrees), 2879 Friedel pairs were averaged for the refinement. 1/3 of the molecule is disordered about two sites (occupancies 0.54, 0.46) and the disordered -Me groups are poorly resolved. Bond length restraints for the disordered -Si(Me)3 groups (1 extra LS parameter) and common, isotropic displacement parameters for all save the Si atoms (3 extra LS parameters). The two solvent THF molecules are VERY poorly resolved, modelled as 1/2 weight with severe geometry constraints and a common, isotropic displacement parameter (2 extra LS parameters). Considering the circumstances, this is an extremely good result (JED). ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_reflns_number 20082 _diffrn_reflns_av_R_equivalents 0.0633 _diffrn_reflns_av_sigmaI/netI 0.0565 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.64 _diffrn_reflns_theta_max 22.46 _reflns_number_total 4976 _reflns_number_gt 3446 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.6(6) _refine_ls_number_reflns 4976 _refine_ls_number_parameters 323 _refine_ls_number_restraints 57 _refine_ls_R_factor_all 0.1667 _refine_ls_R_factor_gt 0.1235 _refine_ls_wR_factor_ref 0.3335 _refine_ls_wR_factor_gt 0.3072 _refine_ls_goodness_of_fit_ref 2.198 _refine_ls_restrained_S_all 2.191 _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 B0 B -0.0012(7) 0.6659(7) 0.825(2) 0.040(3) Uiso 1 1 d . . . N11 N 0.0523(4) 0.7101(5) 0.8387(11) 0.052(3) Uiso 1 1 d . A . H11Z H 0.0557 0.7417 0.8368 0.077 Uiso 1 1 calc R . . B11 B 0.0992(6) 0.7086(7) 0.8549(15) 0.046(4) Uiso 1 1 d . . . H11 H 0.0961 0.6748 0.8579 0.069 Uiso 1 1 calc R A . N12 N 0.1511(4) 0.7531(4) 0.8672(10) 0.0402(10) Uiso 1 1 d . A . Si11 Si 0.15794(15) 0.81609(15) 0.8537(6) 0.0458(12) Uani 1 1 d . . . C111 C 0.2283(7) 0.8706(7) 0.8555(19) 0.0941(12) Uiso 1 1 d . A . H11B H 0.2488 0.8628 0.8128 0.141 Uiso 1 1 calc R . . H11C H 0.2427 0.8738 0.9158 0.141 Uiso 1 1 calc R . . H11D H 0.2300 0.9038 0.8387 0.141 Uiso 1 1 calc R . . C112 C 0.1334(8) 0.8219(8) 0.7447(17) 0.0941(12) Uiso 1 1 d . A . H11E H 0.0990 0.7907 0.7338 0.141 Uiso 1 1 calc R . . H11F H 0.1581 0.8247 0.6980 0.141 Uiso 1 1 calc R . . H11G H 0.1299 0.8534 0.7438 0.141 Uiso 1 1 calc R . . C113 C 0.1238(8) 0.8288(8) 0.9449(17) 0.0941(12) Uiso 1 1 d . A . H11H H 0.0870 0.8157 0.9280 0.141 Uiso 1 1 calc R . . H11I H 0.1410 0.8668 0.9560 0.141 Uiso 1 1 calc R . . H11J H 0.1251 0.8109 0.9993 0.141 Uiso 1 1 calc R . . Si14 Si 0.20251(14) 0.74367(14) 0.9006(6) 0.0414(11) Uani 1 1 d D . . C115 C 0.2256(7) 0.7768(6) 1.0102(12) 0.080(5) Uiso 1 1 d D A . H11K H 0.2436 0.8150 1.0018 0.120 Uiso 1 1 calc R . . H11L H 0.2501 0.7670 1.0366 0.120 Uiso 1 1 calc R . . H11M H 0.1955 0.7658 1.0502 0.120 Uiso 1 1 calc R . . C116 C 0.1798(6) 0.6737(4) 0.9274(12) 0.062(4) Uiso 1 1 d D A . H11N H 0.1692 0.6529 0.8722 0.094 Uiso 1 1 calc R . . H11O H 0.1497 0.6603 0.9683 0.094 Uiso 1 1 calc R . . H11P H 0.2084 0.6711 0.9559 0.094 Uiso 1 1 calc R . . N13 N 0.2530(4) 0.7671(4) 0.8212(10) 0.0402(10) Uiso 1 1 d . A . Si12 Si 0.31918(16) 0.79795(17) 0.8589(6) 0.0729(18) Uani 1 1 d . . . C121 C 0.3670(7) 0.8202(7) 0.7607(15) 0.0941(12) Uiso 1 1 d . A . H12A H 0.3607 0.7895 0.7252 0.141 Uiso 1 1 calc R . . H12B H 0.4032 0.8381 0.7833 0.141 Uiso 1 1 calc R . . H12C H 0.3617 0.8445 0.7231 0.141 Uiso 1 1 calc R . . C122 C 0.3429(7) 0.8588(7) 0.9243(16) 0.0941(12) Uiso 1 1 d . A . H12D H 0.3204 0.8518 0.9768 0.141 Uiso 1 1 calc R . . H12E H 0.3418 0.8857 0.8871 0.141 Uiso 1 1 calc R . . H12F H 0.3791 0.8713 0.9437 0.141 Uiso 1 1 calc R . . C123 C 0.3290(7) 0.7502(7) 0.9215(15) 0.0941(12) Uiso 1 1 d . A . H12G H 0.3032 0.7355 0.9701 0.141 Uiso 1 1 calc R . . H12H H 0.3646 0.7675 0.9466 0.141 Uiso 1 1 calc R . . H12I H 0.3244 0.7218 0.8814 0.141 Uiso 1 1 calc R . . Si13 Si 0.23943(18) 0.7445(2) 0.7136(6) 0.0764(16) Uani 1 1 d . . . C131 C 0.2614(7) 0.7990(7) 0.6327(17) 0.0941(12) Uiso 1 1 d . A . H13A H 0.2821 0.8326 0.6639 0.141 Uiso 1 1 calc R . . H13B H 0.2306 0.7980 0.6050 0.141 Uiso 1 1 calc R . . H13C H 0.2830 0.7954 0.5864 0.141 Uiso 1 1 calc R . . C132 C 0.1665(7) 0.7074(7) 0.6873(17) 0.0941(12) Uiso 1 1 d . A . H13D H 0.1521 0.6700 0.7012 0.141 Uiso 1 1 calc R . . H13E H 0.1613 0.7113 0.6236 0.141 Uiso 1 1 calc R . . H13F H 0.1486 0.7215 0.7234 0.141 Uiso 1 1 calc R . . C133 C 0.2618(7) 0.6997(7) 0.6841(16) 0.0941(12) Uiso 1 1 d . A . H13G H 0.2363 0.6643 0.7054 0.141 Uiso 1 1 calc R . . H13H H 0.2961 0.7112 0.7119 0.141 Uiso 1 1 calc R . . H13I H 0.2651 0.6991 0.6189 0.141 Uiso 1 1 calc R . . N21 N -0.0095(4) 0.6146(4) 0.8128(10) 0.040(3) Uiso 1 1 d . A . H21Z H 0.0188 0.6117 0.8187 0.060 Uiso 1 1 calc R . . B21 B -0.0574(6) 0.5661(6) 0.7924(12) 0.035(4) Uiso 1 1 d . . . H21 H -0.0885 0.5682 0.7849 0.053 Uiso 1 1 calc R A . N22 N -0.0625(4) 0.5163(4) 0.7826(10) 0.0402(10) Uiso 1 1 d . A . Si21 Si -0.00802(17) 0.50775(17) 0.8071(6) 0.0536(14) Uani 1 1 d . . . C211 C 0.0426(7) 0.5424(8) 0.7145(17) 0.0941(12) Uiso 1 1 d . A . H21B H 0.0484 0.5781 0.7063 0.141 Uiso 1 1 calc R . . H21C H 0.0295 0.5227 0.6585 0.141 Uiso 1 1 calc R . . H21D H 0.0758 0.5444 0.7312 0.141 Uiso 1 1 calc R . . C212 C -0.0239(8) 0.4385(7) 0.8027(18) 0.0941(12) Uiso 1 1 d . A . H21E H -0.0532 0.4174 0.8434 0.141 Uiso 1 1 calc R . . H21F H 0.0070 0.4362 0.8209 0.141 Uiso 1 1 calc R . . H21G H -0.0339 0.4252 0.7415 0.141 Uiso 1 1 calc R . . C213 C 0.0211(8) 0.5337(8) 0.9175(17) 0.0941(12) Uiso 1 1 d . A . H21H H -0.0068 0.5213 0.9626 0.141 Uiso 1 1 calc R . . H21I H 0.0401 0.5722 0.9158 0.141 Uiso 1 1 calc R . . H21J H 0.0456 0.5213 0.9329 0.141 Uiso 1 1 calc R . . Si24 Si -0.12254(14) 0.46514(14) 0.7420(6) 0.0405(10) Uani 1 1 d D . . C215 C -0.1083(6) 0.4465(6) 0.6326(11) 0.067(4) Uiso 1 1 d D A . H21K H -0.0837 0.4334 0.6404 0.100 Uiso 1 1 calc R . . H21L H -0.0926 0.4773 0.5931 0.100 Uiso 1 1 calc R . . H21M H -0.1410 0.4189 0.6060 0.100 Uiso 1 1 calc R . . C216 C -0.1705(6) 0.4876(6) 0.7197(14) 0.073(5) Uiso 1 1 d D A . H21N H -0.1836 0.4931 0.7766 0.110 Uiso 1 1 calc R . . H21O H -0.2000 0.4608 0.6846 0.110 Uiso 1 1 calc R . . H21P H -0.1531 0.5207 0.6860 0.110 Uiso 1 1 calc R . . N23 N -0.1524(4) 0.4129(4) 0.8149(11) 0.0402(10) Uiso 1 1 d . A . Si22 Si -0.18638(18) 0.34719(16) 0.7795(7) 0.0696(16) Uani 1 1 d . . . C221 C -0.2439(7) 0.3351(7) 0.6980(15) 0.0941(12) Uiso 1 1 d . A . H22A H -0.2704 0.3396 0.7307 0.141 Uiso 1 1 calc R . . H22B H -0.2602 0.2992 0.6740 0.141 Uiso 1 1 calc R . . H22C H -0.2300 0.3604 0.6486 0.141 Uiso 1 1 calc R . . C222 C -0.2093(7) 0.2976(7) 0.8711(15) 0.0941(12) Uiso 1 1 d . A . H22D H -0.1841 0.3113 0.9207 0.141 Uiso 1 1 calc R . . H22E H -0.2119 0.2650 0.8486 0.141 Uiso 1 1 calc R . . H22F H -0.2439 0.2905 0.8921 0.141 Uiso 1 1 calc R . . C223 C -0.1448(7) 0.3271(7) 0.7138(17) 0.0941(12) Uiso 1 1 d . A . H22G H -0.1199 0.3243 0.7540 0.141 Uiso 1 1 calc R . . H22H H -0.1253 0.3535 0.6676 0.141 Uiso 1 1 calc R . . H22I H -0.1674 0.2929 0.6854 0.141 Uiso 1 1 calc R . . Si23 Si -0.16327(19) 0.42488(18) 0.9271(6) 0.0729(16) Uani 1 1 d . . . C231 C -0.2369(6) 0.3957(7) 0.9386(16) 0.0941(12) Uiso 1 1 d . A . H23A H -0.2477 0.4184 0.9082 0.141 Uiso 1 1 calc R . . H23B H -0.2463 0.3929 1.0021 0.141 Uiso 1 1 calc R . . H23C H -0.2550 0.3606 0.9113 0.141 Uiso 1 1 calc R . . C232 C -0.1344(7) 0.4001(7) 1.0091(16) 0.0941(12) Uiso 1 1 d . A . H23D H -0.0975 0.4268 1.0192 0.141 Uiso 1 1 calc R . . H23E H -0.1364 0.3679 0.9863 0.141 Uiso 1 1 calc R . . H23F H -0.1538 0.3926 1.0656 0.141 Uiso 1 1 calc R . . C233 C -0.1366(7) 0.4957(7) 0.9509(17) 0.0941(12) Uiso 1 1 d . A . H23G H -0.0981 0.5138 0.9510 0.141 Uiso 1 1 calc R . . H23H H -0.1491 0.4997 1.0096 0.141 Uiso 1 1 calc R . . H23I H -0.1486 0.5110 0.9048 0.141 Uiso 1 1 calc R . . N31 N -0.0427(4) 0.6763(4) 0.8186(10) 0.0402(10) Uiso 0.46 1 d P A 1 H31Y H -0.0716 0.6525 0.7919 0.060 Uiso 0.46 1 calc PR A 1 B31 B -0.0427(15) 0.7237(15) 0.853(3) 0.0505(8) Uiso 0.46 1 d P A 1 H31 H -0.0094 0.7527 0.8684 0.076 Uiso 0.46 1 calc PR A 1 N32 N -0.0891(8) 0.7310(8) 0.8655(19) 0.0402(10) Uiso 0.46 1 d P A 1 Si1 Si -0.1506(4) 0.6748(4) 0.8422(9) 0.0505(8) Uiso 0.46 1 d P A 1 C11 C -0.1539(12) 0.6545(12) 0.732(3) 0.0505(8) Uiso 0.46 1 d P A 1 H11Q H -0.1271 0.6444 0.7217 0.076 Uiso 0.46 1 calc PR A 1 H11R H -0.1475 0.6834 0.6913 0.076 Uiso 0.46 1 calc PR A 1 H11S H -0.1888 0.6242 0.7199 0.076 Uiso 0.46 1 calc PR A 1 C12 C -0.1696(11) 0.6211(11) 0.901(2) 0.0505(8) Uiso 0.46 1 d P A 1 H12J H -0.1417 0.6121 0.9014 0.076 Uiso 0.46 1 calc PR A 1 H12K H -0.2015 0.5921 0.8746 0.076 Uiso 0.46 1 calc PR A 1 H12L H -0.1770 0.6270 0.9627 0.076 Uiso 0.46 1 calc PR A 1 C13 C -0.2056(12) 0.6914(12) 0.843(2) 0.0505(8) Uiso 0.46 1 d P A 1 H13J H -0.1963 0.7213 0.8029 0.076 Uiso 0.46 1 calc PR A 1 H13K H -0.2105 0.7006 0.9037 0.076 Uiso 0.46 1 calc PR A 1 H13L H -0.2384 0.6609 0.8222 0.076 Uiso 0.46 1 calc PR A 1 Si4 Si -0.0833(3) 0.7863(3) 0.9161(8) 0.0505(8) Uiso 0.46 1 d PD A 1 C45 C -0.0149(7) 0.8323(10) 0.951(2) 0.0505(8) Uiso 0.46 1 d PD A 1 H45A H 0.0076 0.8455 0.8976 0.076 Uiso 0.46 1 calc PR A 1 H45B H -0.0024 0.8139 0.9895 0.076 Uiso 0.46 1 calc PR A 1 H45C H -0.0136 0.8618 0.9835 0.076 Uiso 0.46 1 calc PR A 1 C46 C -0.1196(9) 0.7668(10) 1.0255(16) 0.0505(8) Uiso 0.46 1 d PD A 1 H46A H -0.1570 0.7420 1.0145 0.076 Uiso 0.46 1 calc PR A 1 H46B H -0.1159 0.7982 1.0556 0.076 Uiso 0.46 1 calc PR A 1 H46C H -0.1050 0.7501 1.0636 0.076 Uiso 0.46 1 calc PR A 1 N33 N -0.1066(14) 0.8142(13) 0.857(2) 0.0402(10) Uiso 0.46 1 d P A 1 Si2 Si -0.1380(3) 0.8499(3) 0.8789(6) 0.0505(8) Uiso 0.46 1 d PD A 1 C21 C -0.1918(7) 0.8082(9) 0.9516(14) 0.0941(12) Uiso 0.46 1 d PD A 1 H21Q H -0.1788 0.7958 1.0009 0.141 Uiso 0.46 1 calc PR A 1 H21R H -0.2183 0.7779 0.9176 0.141 Uiso 0.46 1 calc PR A 1 H21S H -0.2077 0.8281 0.9757 0.141 Uiso 0.46 1 calc PR A 1 C22 C -0.0888(8) 0.9057(7) 0.9403(16) 0.0941(12) Uiso 0.46 1 d PD A 1 H22J H -0.0765 0.8934 0.9908 0.141 Uiso 0.46 1 calc PR A 1 H22K H -0.1041 0.9265 0.9628 0.141 Uiso 0.46 1 calc PR A 1 H22L H -0.0591 0.9275 0.9008 0.141 Uiso 0.46 1 calc PR A 1 C23 C -0.1615(10) 0.8718(11) 0.7865(12) 0.0941(12) Uiso 0.46 1 d PD A 1 H23J H -0.1319 0.8950 0.7478 0.141 Uiso 0.46 1 calc PR A 1 H23K H -0.1784 0.8911 0.8093 0.141 Uiso 0.46 1 calc PR A 1 H23L H -0.1872 0.8413 0.7519 0.141 Uiso 0.46 1 calc PR A 1 Si3 Si -0.0771(3) 0.8355(3) 0.7315(8) 0.0505(8) Uiso 0.46 1 d PD A 1 C31 C -0.1320(7) 0.8085(9) 0.6554(17) 0.0941(12) Uiso 0.46 1 d PD A 1 H31B H -0.1190 0.8177 0.5938 0.141 Uiso 0.46 1 calc PR A 1 H31C H -0.1548 0.8231 0.6691 0.141 Uiso 0.46 1 calc PR A 1 H31D H -0.1520 0.7702 0.6618 0.141 Uiso 0.46 1 calc PR A 1 C32 C -0.0380(8) 0.9056(3) 0.717(2) 0.0941(12) Uiso 0.46 1 d PD A 1 H32A H -0.0242 0.9134 0.6555 0.141 Uiso 0.46 1 calc PR A 1 H32B H -0.0087 0.9200 0.7593 0.141 Uiso 0.46 1 calc PR A 1 H32C H -0.0599 0.9216 0.7271 0.141 Uiso 0.46 1 calc PR A 1 C33 C -0.0374(9) 0.8054(10) 0.713(2) 0.0941(12) Uiso 0.46 1 d PD A 1 H33A H -0.0222 0.8143 0.6525 0.141 Uiso 0.46 1 calc PR A 1 H33B H -0.0593 0.7672 0.7183 0.141 Uiso 0.46 1 calc PR A 1 H33C H -0.0091 0.8185 0.7571 0.141 Uiso 0.46 1 calc PR A 1 N31' N -0.0427(4) 0.6763(4) 0.8186(10) 0.0402(10) Uiso 0.54 1 d P A 2 H31Z H -0.0744 0.6495 0.8284 0.060 Uiso 0.54 1 calc PR A 2 B31' B -0.0402(13) 0.7244(13) 0.799(3) 0.0505(8) Uiso 0.54 1 d P A 2 H31' H -0.0068 0.7540 0.7856 0.076 Uiso 0.54 1 calc PR A 2 N32' N -0.0863(7) 0.7312(8) 0.7969(15) 0.0402(10) Uiso 0.54 1 d P A 2 Si1' Si -0.1502(4) 0.6751(4) 0.8061(8) 0.0505(8) Uiso 0.54 1 d P A 2 C11' C -0.1598(10) 0.6325(10) 0.708(2) 0.0505(8) Uiso 0.54 1 d P A 2 H11T H -0.1558 0.6523 0.6530 0.076 Uiso 0.54 1 calc PR A 2 H11U H -0.1952 0.6016 0.7103 0.076 Uiso 0.54 1 calc PR A 2 H11V H -0.1335 0.6212 0.7094 0.076 Uiso 0.54 1 calc PR A 2 C12' C -0.1579(11) 0.6382(10) 0.927(2) 0.0505(8) Uiso 0.54 1 d P A 2 H12M H -0.1306 0.6284 0.9326 0.076 Uiso 0.54 1 calc PR A 2 H12N H -0.1927 0.6066 0.9310 0.076 Uiso 0.54 1 calc PR A 2 H12O H -0.1539 0.6623 0.9762 0.076 Uiso 0.54 1 calc PR A 2 C13' C -0.2035(11) 0.6929(11) 0.799(2) 0.0505(8) Uiso 0.54 1 d P A 2 H13M H -0.1994 0.7123 0.7433 0.076 Uiso 0.54 1 calc PR A 2 H13N H -0.2007 0.7150 0.8502 0.076 Uiso 0.54 1 calc PR A 2 H13O H -0.2380 0.6608 0.7995 0.076 Uiso 0.54 1 calc PR A 2 Si4' Si -0.0760(3) 0.7942(3) 0.7707(8) 0.0505(8) Uiso 0.54 1 d PD A 2 C45' C -0.0026(6) 0.8413(8) 0.7554(18) 0.0505(8) Uiso 0.54 1 d PD A 2 H45D H 0.0155 0.8457 0.8125 0.076 Uiso 0.54 1 calc PR A 2 H45E H 0.0032 0.8754 0.7348 0.076 Uiso 0.54 1 calc PR A 2 H45F H 0.0113 0.8269 0.7108 0.076 Uiso 0.54 1 calc PR A 2 C46' C -0.1021(8) 0.7903(9) 0.6564(14) 0.0505(8) Uiso 0.54 1 d PD A 2 H46D H -0.1404 0.7670 0.6567 0.076 Uiso 0.54 1 calc PR A 2 H46E H -0.0861 0.7764 0.6152 0.076 Uiso 0.54 1 calc PR A 2 H46F H -0.0938 0.8256 0.6368 0.076 Uiso 0.54 1 calc PR A 2 N33' N -0.1026(13) 0.8198(12) 0.838(2) 0.0402(10) Uiso 0.54 1 d P A 2 Si2' Si -0.0846(3) 0.8203(3) 0.9615(7) 0.0505(8) Uiso 0.54 1 d PD A 2 C21' C -0.1464(6) 0.7846(7) 1.0279(18) 0.0941(12) Uiso 0.54 1 d PD A 2 H21T H -0.1378 0.7858 1.0915 0.141 Uiso 0.54 1 calc PR A 2 H21U H -0.1663 0.7479 1.0081 0.141 Uiso 0.54 1 calc PR A 2 H21V H -0.1678 0.8014 1.0189 0.141 Uiso 0.54 1 calc PR A 2 C22' C -0.0445(7) 0.7877(7) 0.977(2) 0.0941(12) Uiso 0.54 1 d PD A 2 H22M H -0.0349 0.7894 1.0402 0.141 Uiso 0.54 1 calc PR A 2 H22N H -0.0125 0.8058 0.9406 0.141 Uiso 0.54 1 calc PR A 2 H22O H -0.0651 0.7508 0.9582 0.141 Uiso 0.54 1 calc PR A 2 C23' C -0.0463(7) 0.8898(5) 1.000(2) 0.0941(12) Uiso 0.54 1 d PD A 2 H23M H -0.0372 0.8905 1.0637 0.141 Uiso 0.54 1 calc PR A 2 H23N H -0.0676 0.9068 0.9932 0.141 Uiso 0.54 1 calc PR A 2 H23O H -0.0141 0.9087 0.9649 0.141 Uiso 0.54 1 calc PR A 2 Si3' Si -0.1312(3) 0.8557(3) 0.8167(5) 0.0505(8) Uiso 0.54 1 d PD A 2 C31' C -0.1901(6) 0.8166(9) 0.7449(13) 0.0941(12) Uiso 0.54 1 d PD A 2 H31F H -0.1797 0.8054 0.6906 0.141 Uiso 0.54 1 calc PR A 2 H31G H -0.2057 0.8382 0.7284 0.141 Uiso 0.54 1 calc PR A 2 H31H H -0.2161 0.7855 0.7779 0.141 Uiso 0.54 1 calc PR A 2 C32' C -0.0828(8) 0.9159(6) 0.7551(14) 0.0941(12) Uiso 0.54 1 d PD A 2 H32D H -0.0718 0.9056 0.7003 0.141 Uiso 0.54 1 calc PR A 2 H32E H -0.0520 0.9367 0.7930 0.141 Uiso 0.54 1 calc PR A 2 H32F H -0.0991 0.9369 0.7395 0.141 Uiso 0.54 1 calc PR A 2 C33' C -0.1515(9) 0.8753(9) 0.9214(9) 0.0941(12) Uiso 0.54 1 d PD A 2 H33D H -0.1204 0.8967 0.9585 0.141 Uiso 0.54 1 calc PR A 2 H33E H -0.1762 0.8437 0.9546 0.141 Uiso 0.54 1 calc PR A 2 H33F H -0.1684 0.8958 0.9063 0.141 Uiso 0.54 1 calc PR A 2 O51 O -0.0398(11) 0.6391(13) 0.575(3) 0.165(6) Uiso 0.50 1 d PD . . C52 C -0.0050(16) 0.6932(14) 0.590(4) 0.165(6) Uiso 0.50 1 d PD . . H52A H -0.0184 0.7142 0.5599 0.198 Uiso 0.50 1 calc PR . . H52B H -0.0025 0.7009 0.6551 0.198 Uiso 0.50 1 calc PR . . C53 C 0.0434(14) 0.7063(13) 0.557(5) 0.165(6) Uiso 0.50 1 d PD . . H53A H 0.0701 0.7216 0.6053 0.198 Uiso 0.50 1 calc PR . . H53B H 0.0533 0.7327 0.5089 0.198 Uiso 0.50 1 calc PR . . C54 C 0.0411(15) 0.6609(18) 0.524(4) 0.165(6) Uiso 0.50 1 d PD . . H54A H 0.0493 0.6648 0.4592 0.198 Uiso 0.50 1 calc PR . . H54B H 0.0670 0.6543 0.5551 0.198 Uiso 0.50 1 calc PR . . C55 C -0.0094(17) 0.6193(13) 0.538(5) 0.165(6) Uiso 0.50 1 d PD . . H55A H -0.0084 0.5934 0.5794 0.198 Uiso 0.50 1 calc PR . . H55B H -0.0250 0.6014 0.4808 0.198 Uiso 0.50 1 calc PR . . O61 O -0.0429(10) 0.3073(12) 0.603(3) 0.165(6) Uiso 0.50 1 d PD . . C62 C -0.0042(15) 0.2929(12) 0.601(4) 0.165(6) Uiso 0.50 1 d PD . . H62A H -0.0126 0.2647 0.6457 0.198 Uiso 0.50 1 calc PR . . H62B H -0.0024 0.2797 0.5414 0.198 Uiso 0.50 1 calc PR . . C63 C 0.0434(13) 0.3371(16) 0.622(5) 0.165(6) Uiso 0.50 1 d PD . . H63A H 0.0696 0.3440 0.5750 0.198 Uiso 0.50 1 calc PR . . H63B H 0.0571 0.3317 0.6797 0.198 Uiso 0.50 1 calc PR . . C64 C 0.0346(14) 0.3799(13) 0.630(4) 0.165(6) Uiso 0.50 1 d PD . . H64A H 0.0363 0.3904 0.6932 0.198 Uiso 0.50 1 calc PR . . H64B H 0.0614 0.4105 0.5955 0.198 Uiso 0.50 1 calc PR . . C65 C -0.0155(15) 0.3625(13) 0.595(5) 0.165(6) Uiso 0.50 1 d PD . . H65A H -0.0131 0.3729 0.5312 0.198 Uiso 0.50 1 calc PR . . H65B H -0.0336 0.3778 0.6286 0.198 Uiso 0.50 1 calc PR . . 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 Si11 0.035(2) 0.031(2) 0.072(3) -0.013(2) -0.011(2) 0.0172(17) Si14 0.0303(19) 0.038(2) 0.059(3) 0.007(2) -0.0019(19) 0.0195(16) Si12 0.032(2) 0.064(3) 0.116(5) 0.004(3) -0.007(3) 0.018(2) Si13 0.058(3) 0.096(4) 0.063(4) -0.021(3) 0.010(3) 0.030(3) Si21 0.035(2) 0.043(2) 0.089(4) -0.005(2) -0.016(2) 0.025(2) Si24 0.041(2) 0.036(2) 0.041(2) -0.0006(18) -0.0022(19) 0.0160(17) Si22 0.056(3) 0.024(2) 0.108(4) -0.004(2) -0.010(3) 0.0045(19) Si23 0.083(3) 0.065(3) 0.067(4) 0.010(3) 0.037(3) 0.034(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 B0 N31 1.40(2) . ? B0 N21 1.41(2) . ? B0 N11 1.47(2) . ? N11 B11 1.421(19) . ? N11 H11Z 0.8800 . ? B11 N12 1.438(19) . ? B11 H11 0.9500 . ? N12 Si14 1.738(12) . ? N12 Si11 1.767(11) . ? Si11 C112 1.82(2) . ? Si11 C113 1.84(2) . ? Si11 C111 1.876(18) . ? C111 H11B 0.9800 . ? C111 H11C 0.9800 . ? C111 H11D 0.9800 . ? C112 H11E 0.9800 . ? C112 H11F 0.9800 . ? C112 H11G 0.9800 . ? C113 H11H 0.9800 . ? C113 H11I 0.9800 . ? C113 H11J 0.9800 . ? Si14 N13 1.748(13) . ? Si14 C115 1.850(13) . ? Si14 C116 1.858(11) . ? C115 H11K 0.9800 . ? C115 H11L 0.9800 . ? C115 H11M 0.9800 . ? C116 H11N 0.9800 . ? C116 H11O 0.9800 . ? C116 H11P 0.9800 . ? N13 Si13 1.709(14) . ? N13 Si12 1.776(12) . ? Si12 C123 1.824(18) . ? Si12 C122 1.839(19) . ? Si12 C121 1.91(2) . ? C121 H12A 0.9800 . ? C121 H12B 0.9800 . ? C121 H12C 0.9800 . ? C122 H12D 0.9800 . ? C122 H12E 0.9800 . ? C122 H12F 0.9800 . ? C123 H12G 0.9800 . ? C123 H12H 0.9800 . ? C123 H12I 0.9800 . ? Si13 C133 1.794(17) . ? Si13 C131 1.84(2) . ? Si13 C132 1.894(18) . ? C131 H13A 0.9800 . ? C131 H13B 0.9800 . ? C131 H13C 0.9800 . ? C132 H13D 0.9800 . ? C132 H13E 0.9800 . ? C132 H13F 0.9800 . ? C133 H13G 0.9800 . ? C133 H13H 0.9800 . ? C133 H13I 0.9800 . ? N21 B21 1.449(18) . ? N21 H21Z 0.8800 . ? B21 N22 1.401(18) . ? B21 H21 0.9500 . ? N22 Si24 1.754(12) . ? N22 Si21 1.776(11) . ? Si21 C213 1.84(2) . ? Si21 C212 1.85(2) . ? Si21 C211 1.91(2) . ? C211 H21B 0.9800 . ? C211 H21C 0.9800 . ? C211 H21D 0.9800 . ? C212 H21E 0.9800 . ? C212 H21F 0.9800 . ? C212 H21G 0.9800 . ? C213 H21H 0.9800 . ? C213 H21I 0.9800 . ? C213 H21J 0.9800 . ? Si24 N23 1.720(13) . ? Si24 C215 1.837(13) . ? Si24 C216 1.858(12) . ? C215 H21K 0.9800 . ? C215 H21L 0.9800 . ? C215 H21M 0.9800 . ? C216 H21N 0.9800 . ? C216 H21O 0.9800 . ? C216 H21P 0.9800 . ? N23 Si22 1.753(12) . ? N23 Si23 1.774(14) . ? Si22 C222 1.86(2) . ? Si22 C223 1.88(2) . ? Si22 C221 1.966(19) . ? C221 H22A 0.9800 . ? C221 H22B 0.9800 . ? C221 H22C 0.9800 . ? C222 H22D 0.9800 . ? C222 H22E 0.9800 . ? C222 H22F 0.9800 . ? C223 H22G 0.9800 . ? C223 H22H 0.9800 . ? C223 H22I 0.9800 . ? Si23 C232 1.83(2) . ? Si23 C233 1.852(18) . ? Si23 C231 1.893(16) . ? C231 H23A 0.9800 . ? C231 H23B 0.9800 . ? C231 H23C 0.9800 . ? C232 H23D 0.9800 . ? C232 H23E 0.9800 . ? C232 H23F 0.9800 . ? C233 H23G 0.9800 . ? C233 H23H 0.9800 . ? C233 H23I 0.9800 . ? N31 B31 1.48(4) . ? N31 H31Y 0.8800 . ? B31 N32 1.49(4) . ? B31 H31 0.9500 . ? N32 Si4 1.72(2) . ? N32 Si1 1.77(2) . ? Si1 C12 1.64(3) . ? Si1 C11 1.74(4) . ? Si1 C13 1.91(3) . ? C11 H11Q 0.9800 . ? C11 H11R 0.9800 . ? C11 H11S 0.9800 . ? C12 H12J 0.9800 . ? C12 H12K 0.9800 . ? C12 H12L 0.9800 . ? C13 H13J 0.9800 . ? C13 H13K 0.9800 . ? C13 H13L 0.9800 . ? Si4 N33 1.57(3) . ? Si4 C45 1.846(17) . ? Si4 C46 1.878(17) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? N33 Si2 1.73(4) . ? N33 Si3 2.03(3) . ? Si2 C22 1.8003(10) . ? Si2 C21 1.8004(10) . ? Si2 C23 1.8004(10) . ? C21 H21Q 0.9800 . ? C21 H21R 0.9800 . ? C21 H21S 0.9800 . ? C22 H22J 0.9800 . ? C22 H22K 0.9800 . ? C22 H22L 0.9800 . ? C23 H23J 0.9800 . ? C23 H23K 0.9800 . ? C23 H23L 0.9800 . ? Si3 C32 1.8000(11) . ? Si3 C33 1.8001(11) . ? Si3 C31 1.8001(11) . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C31 H31D 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? B31' N32' 1.46(4) . ? B31' H31' 0.9500 . ? N32' Si4' 1.76(2) . ? N32' Si1' 1.78(2) . ? Si1' C11' 1.85(3) . ? Si1' C13' 1.88(3) . ? Si1' C12' 2.06(3) . ? C11' H11T 0.9800 . ? C11' H11U 0.9800 . ? C11' H11V 0.9800 . ? C12' H12M 0.9800 . ? C12' H12N 0.9800 . ? C12' H12O 0.9800 . ? C13' H13M 0.9800 . ? C13' H13N 0.9800 . ? C13' H13O 0.9800 . ? Si4' N33' 1.66(4) . ? Si4' C46' 1.853(16) . ? Si4' C45' 1.903(15) . ? C45' H45D 0.9800 . ? C45' H45E 0.9800 . ? C45' H45F 0.9800 . ? C46' H46D 0.9800 . ? C46' H46E 0.9800 . ? C46' H46F 0.9800 . ? N33' Si3' 1.67(3) . ? N33' Si2' 1.92(3) . ? Si2' C23' 1.863(6) . ? Si2' C22' 1.864(6) . ? Si2' C21' 1.864(6) . ? C21' H21T 0.9800 . ? C21' H21U 0.9800 . ? C21' H21V 0.9800 . ? C22' H22M 0.9800 . ? C22' H22N 0.9800 . ? C22' H22O 0.9800 . ? C23' H23M 0.9800 . ? C23' H23N 0.9800 . ? C23' H23O 0.9800 . ? Si3' C32' 1.864(6) . ? Si3' C31' 1.864(6) . ? Si3' C33' 1.864(6) . ? C31' H31F 0.9800 . ? C31' H31G 0.9800 . ? C31' H31H 0.9800 . ? C32' H32D 0.9800 . ? C32' H32E 0.9800 . ? C32' H32F 0.9800 . ? C33' H33D 0.9800 . ? C33' H33E 0.9800 . ? C33' H33F 0.9800 . ? O51 C55 1.40(2) . ? O51 C52 1.41(2) . ? C52 C53 1.36(2) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.39(2) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.39(2) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? O61 C62 1.40(2) . ? O61 C65 1.41(2) . ? C62 C63 1.39(2) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.41(2) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.39(2) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? 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 N31 B0 N21 121.3(15) . . ? N31 B0 N11 118.7(14) . . ? N21 B0 N11 119.9(15) . . ? B11 N11 B0 128.5(13) . . ? B11 N11 H11Z 115.8 . . ? B0 N11 H11Z 115.8 . . ? N11 B11 N12 126.6(14) . . ? N11 B11 H11 116.7 . . ? N12 B11 H11 116.7 . . ? B11 N12 Si14 120.0(10) . . ? B11 N12 Si11 116.8(10) . . ? Si14 N12 Si11 123.1(6) . . ? N12 Si11 C112 110.8(8) . . ? N12 Si11 C113 109.9(8) . . ? C112 Si11 C113 111.2(9) . . ? N12 Si11 C111 113.1(7) . . ? C112 Si11 C111 104.5(11) . . ? C113 Si11 C111 107.2(10) . . ? Si11 C111 H11B 109.5 . . ? Si11 C111 H11C 109.5 . . ? H11B C111 H11C 109.5 . . ? Si11 C111 H11D 109.5 . . ? H11B C111 H11D 109.5 . . ? H11C C111 H11D 109.5 . . ? Si11 C112 H11E 109.5 . . ? Si11 C112 H11F 109.5 . . ? H11E C112 H11F 109.5 . . ? Si11 C112 H11G 109.5 . . ? H11E C112 H11G 109.5 . . ? H11F C112 H11G 109.5 . . ? Si11 C113 H11H 109.5 . . ? Si11 C113 H11I 109.5 . . ? H11H C113 H11I 109.5 . . ? Si11 C113 H11J 109.5 . . ? H11H C113 H11J 109.5 . . ? H11I C113 H11J 109.5 . . ? N12 Si14 N13 112.0(6) . . ? N12 Si14 C115 106.9(7) . . ? N13 Si14 C115 112.2(7) . . ? N12 Si14 C116 112.2(6) . . ? N13 Si14 C116 110.3(6) . . ? C115 Si14 C116 103.0(7) . . ? Si14 C115 H11K 109.5 . . ? Si14 C115 H11L 109.5 . . ? H11K C115 H11L 109.5 . . ? Si14 C115 H11M 109.5 . . ? H11K C115 H11M 109.5 . . ? H11L C115 H11M 109.5 . . ? Si14 C116 H11N 109.5 . . ? Si14 C116 H11O 109.5 . . ? H11N C116 H11O 109.5 . . ? Si14 C116 H11P 109.5 . . ? H11N C116 H11P 109.5 . . ? H11O C116 H11P 109.5 . . ? Si13 N13 Si14 120.0(7) . . ? Si13 N13 Si12 118.6(7) . . ? Si14 N13 Si12 118.8(8) . . ? N13 Si12 C123 108.9(7) . . ? N13 Si12 C122 116.7(7) . . ? C123 Si12 C122 110.2(10) . . ? N13 Si12 C121 111.2(8) . . ? C123 Si12 C121 106.7(8) . . ? C122 Si12 C121 102.7(9) . . ? Si12 C121 H12A 109.5 . . ? Si12 C121 H12B 109.5 . . ? H12A C121 H12B 109.5 . . ? Si12 C121 H12C 109.5 . . ? H12A C121 H12C 109.5 . . ? H12B C121 H12C 109.5 . . ? Si12 C122 H12D 109.5 . . ? Si12 C122 H12E 109.5 . . ? H12D C122 H12E 109.5 . . ? Si12 C122 H12F 109.5 . . ? H12D C122 H12F 109.5 . . ? H12E C122 H12F 109.5 . . ? Si12 C123 H12G 109.5 . . ? Si12 C123 H12H 109.5 . . ? H12G C123 H12H 109.5 . . ? Si12 C123 H12I 109.5 . . ? H12G C123 H12I 109.5 . . ? H12H C123 H12I 109.5 . . ? N13 Si13 C133 114.6(9) . . ? N13 Si13 C131 111.6(9) . . ? C133 Si13 C131 112.2(10) . . ? N13 Si13 C132 113.3(9) . . ? C133 Si13 C132 104.4(8) . . ? C131 Si13 C132 99.6(9) . . ? Si13 C131 H13A 109.5 . . ? Si13 C131 H13B 109.5 . . ? H13A C131 H13B 109.5 . . ? Si13 C131 H13C 109.5 . . ? H13A C131 H13C 109.5 . . ? H13B C131 H13C 109.5 . . ? Si13 C132 H13D 109.5 . . ? Si13 C132 H13E 109.5 . . ? H13D C132 H13E 109.5 . . ? Si13 C132 H13F 109.5 . . ? H13D C132 H13F 109.5 . . ? H13E C132 H13F 109.5 . . ? Si13 C133 H13G 109.5 . . ? Si13 C133 H13H 109.5 . . ? H13G C133 H13H 109.5 . . ? Si13 C133 H13I 109.5 . . ? H13G C133 H13I 109.5 . . ? H13H C133 H13I 109.5 . . ? B0 N21 B21 129.8(13) . . ? B0 N21 H21Z 115.1 . . ? B21 N21 H21Z 115.1 . . ? N22 B21 N21 126.3(13) . . ? N22 B21 H21 116.8 . . ? N21 B21 H21 116.8 . . ? B21 N22 Si24 117.8(9) . . ? B21 N22 Si21 119.5(9) . . ? Si24 N22 Si21 122.7(6) . . ? N22 Si21 C213 113.0(8) . . ? N22 Si21 C212 113.5(8) . . ? C213 Si21 C212 107.2(11) . . ? N22 Si21 C211 106.9(8) . . ? C213 Si21 C211 110.6(9) . . ? C212 Si21 C211 105.2(9) . . ? Si21 C211 H21B 109.5 . . ? Si21 C211 H21C 109.5 . . ? H21B C211 H21C 109.5 . . ? Si21 C211 H21D 109.5 . . ? H21B C211 H21D 109.5 . . ? H21C C211 H21D 109.5 . . ? Si21 C212 H21E 109.5 . . ? Si21 C212 H21F 109.5 . . ? H21E C212 H21F 109.5 . . ? Si21 C212 H21G 109.5 . . ? H21E C212 H21G 109.5 . . ? H21F C212 H21G 109.5 . . ? Si21 C213 H21H 109.5 . . ? Si21 C213 H21I 109.5 . . ? H21H C213 H21I 109.5 . . ? Si21 C213 H21J 109.5 . . ? H21H C213 H21J 109.5 . . ? H21I C213 H21J 109.5 . . ? N23 Si24 N22 112.9(6) . . ? N23 Si24 C215 112.9(7) . . ? N22 Si24 C215 106.4(7) . . ? N23 Si24 C216 106.9(7) . . ? N22 Si24 C216 111.9(6) . . ? C215 Si24 C216 105.7(7) . . ? Si24 C215 H21K 109.5 . . ? Si24 C215 H21L 109.5 . . ? H21K C215 H21L 109.5 . . ? Si24 C215 H21M 109.5 . . ? H21K C215 H21M 109.5 . . ? H21L C215 H21M 109.5 . . ? Si24 C216 H21N 109.5 . . ? Si24 C216 H21O 109.5 . . ? H21N C216 H21O 109.5 . . ? Si24 C216 H21P 109.5 . . ? H21N C216 H21P 109.5 . . ? H21O C216 H21P 109.5 . . ? Si24 N23 Si22 123.0(8) . . ? Si24 N23 Si23 119.0(7) . . ? Si22 N23 Si23 116.3(7) . . ? N23 Si22 C222 115.0(8) . . ? N23 Si22 C223 113.7(8) . . ? C222 Si22 C223 100.2(9) . . ? N23 Si22 C221 110.6(7) . . ? C222 Si22 C221 111.9(9) . . ? C223 Si22 C221 104.7(10) . . ? Si22 C221 H22A 109.5 . . ? Si22 C221 H22B 109.5 . . ? H22A C221 H22B 109.5 . . ? Si22 C221 H22C 109.5 . . ? H22A C221 H22C 109.5 . . ? H22B C221 H22C 109.5 . . ? Si22 C222 H22D 109.5 . . ? Si22 C222 H22E 109.5 . . ? H22D C222 H22E 109.5 . . ? Si22 C222 H22F 109.5 . . ? H22D C222 H22F 109.5 . . ? H22E C222 H22F 109.5 . . ? Si22 C223 H22G 109.5 . . ? Si22 C223 H22H 109.5 . . ? H22G C223 H22H 109.5 . . ? Si22 C223 H22I 109.5 . . ? H22G C223 H22I 109.5 . . ? H22H C223 H22I 109.5 . . ? N23 Si23 C232 112.8(8) . . ? N23 Si23 C233 112.7(9) . . ? C232 Si23 C233 107.3(10) . . ? N23 Si23 C231 105.9(8) . . ? C232 Si23 C231 114.2(9) . . ? C233 Si23 C231 103.7(8) . . ? Si23 C231 H23A 109.5 . . ? Si23 C231 H23B 109.5 . . ? H23A C231 H23B 109.5 . . ? Si23 C231 H23C 109.5 . . ? H23A C231 H23C 109.5 . . ? H23B C231 H23C 109.5 . . ? Si23 C232 H23D 109.5 . . ? Si23 C232 H23E 109.5 . . ? H23D C232 H23E 109.5 . . ? Si23 C232 H23F 109.5 . . ? H23D C232 H23F 109.5 . . ? H23E C232 H23F 109.5 . . ? Si23 C233 H23G 109.5 . . ? Si23 C233 H23H 109.5 . . ? H23G C233 H23H 109.5 . . ? Si23 C233 H23I 109.5 . . ? H23G C233 H23I 109.5 . . ? H23H C233 H23I 109.5 . . ? B0 N31 B31 126.2(19) . . ? B0 N31 H31Y 116.9 . . ? B31 N31 H31Y 116.9 . . ? N31 B31 N32 127(3) . . ? N31 B31 H31 116.3 . . ? N32 B31 H31 116.3 . . ? B31 N32 Si4 122(2) . . ? B31 N32 Si1 115(2) . . ? Si4 N32 Si1 122.6(13) . . ? C12 Si1 C11 104.3(16) . . ? C12 Si1 N32 119.2(15) . . ? C11 Si1 N32 111.2(15) . . ? C12 Si1 C13 108.6(15) . . ? C11 Si1 C13 100.6(16) . . ? N32 Si1 C13 111.2(13) . . ? Si1 C11 H11Q 109.5 . . ? Si1 C11 H11R 109.5 . . ? H11Q C11 H11R 109.5 . . ? Si1 C11 H11S 109.5 . . ? H11Q C11 H11S 109.5 . . ? H11R C11 H11S 109.5 . . ? Si1 C12 H12J 109.5 . . ? Si1 C12 H12K 109.5 . . ? H12J C12 H12K 109.5 . . ? Si1 C12 H12L 109.5 . . ? H12J C12 H12L 109.5 . . ? H12K C12 H12L 109.5 . . ? Si1 C13 H13J 109.5 . . ? Si1 C13 H13K 109.5 . . ? H13J C13 H13K 109.5 . . ? Si1 C13 H13L 109.5 . . ? H13J C13 H13L 109.5 . . ? H13K C13 H13L 109.5 . . ? N33 Si4 N32 112.6(17) . . ? N33 Si4 C45 111.9(16) . . ? N32 Si4 C45 111.7(12) . . ? N33 Si4 C46 108.4(15) . . ? N32 Si4 C46 108.8(13) . . ? C45 Si4 C46 102.9(11) . . ? Si4 C45 H45A 109.5 . . ? Si4 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? Si4 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? Si4 C46 H46A 109.5 . . ? Si4 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? Si4 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? Si4 N33 Si2 135(2) . . ? Si4 N33 Si3 116.5(19) . . ? Si2 N33 Si3 105.1(15) . . ? N33 Si2 C22 102.6(16) . . ? N33 Si2 C21 104.6(14) . . ? C22 Si2 C21 110.02(9) . . ? N33 Si2 C23 119.2(16) . . ? C22 Si2 C23 110.02(9) . . ? C21 Si2 C23 110.01(9) . . ? Si2 C21 H21Q 109.5 . . ? Si2 C21 H21R 109.5 . . ? H21Q C21 H21R 109.5 . . ? Si2 C21 H21S 109.5 . . ? H21Q C21 H21S 109.5 . . ? H21R C21 H21S 109.5 . . ? Si2 C22 H22J 109.5 . . ? Si2 C22 H22K 109.5 . . ? H22J C22 H22K 109.5 . . ? Si2 C22 H22L 109.5 . . ? H22J C22 H22L 109.5 . . ? H22K C22 H22L 109.5 . . ? Si2 C23 H23J 109.5 . . ? Si2 C23 H23K 109.5 . . ? H23J C23 H23K 109.5 . . ? Si2 C23 H23L 109.5 . . ? H23J C23 H23L 109.5 . . ? H23K C23 H23L 109.5 . . ? C32 Si3 C33 110.05(9) . . ? C32 Si3 C31 110.05(9) . . ? C33 Si3 C31 110.04(9) . . ? C32 Si3 N33 113.2(15) . . ? C33 Si3 N33 106.0(15) . . ? C31 Si3 N33 107.4(14) . . ? Si3 C31 H31B 109.5 . . ? Si3 C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si3 C31 H31D 109.5 . . ? H31B C31 H31D 109.5 . . ? H31C C31 H31D 109.5 . . ? Si3 C32 H32A 109.5 . . ? Si3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si3 C33 H33A 109.5 . . ? Si3 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si3 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N32' B31' H31' 118.3 . . ? B31' N32' Si4' 117.5(17) . . ? B31' N32' Si1' 119.5(18) . . ? Si4' N32' Si1' 122.5(11) . . ? N32' Si1' C11' 107.3(12) . . ? N32' Si1' C13' 112.1(12) . . ? C11' Si1' C13' 106.0(13) . . ? N32' Si1' C12' 109.9(11) . . ? C11' Si1' C12' 113.6(12) . . ? C13' Si1' C12' 107.9(13) . . ? Si1' C11' H11T 109.5 . . ? Si1' C11' H11U 109.5 . . ? H11T C11' H11U 109.5 . . ? Si1' C11' H11V 109.5 . . ? H11T C11' H11V 109.5 . . ? H11U C11' H11V 109.5 . . ? Si1' C12' H12M 109.5 . . ? Si1' C12' H12N 109.5 . . ? H12M C12' H12N 109.5 . . ? Si1' C12' H12O 109.5 . . ? H12M C12' H12O 109.5 . . ? H12N C12' H12O 109.5 . . ? Si1' C13' H13M 109.5 . . ? Si1' C13' H13N 109.5 . . ? H13M C13' H13N 109.5 . . ? Si1' C13' H13O 109.5 . . ? H13M C13' H13O 109.5 . . ? H13N C13' H13O 109.5 . . ? N33' Si4' N32' 117.9(12) . . ? N33' Si4' C46' 107.9(14) . . ? N32' Si4' C46' 107.0(11) . . ? N33' Si4' C45' 111.3(14) . . ? N32' Si4' C45' 109.1(10) . . ? C46' Si4' C45' 102.6(10) . . ? Si4' C45' H45D 109.5 . . ? Si4' C45' H45E 109.5 . . ? H45D C45' H45E 109.5 . . ? Si4' C45' H45F 109.5 . . ? H45D C45' H45F 109.5 . . ? H45E C45' H45F 109.5 . . ? Si4' C46' H46D 109.5 . . ? Si4' C46' H46E 109.5 . . ? H46D C46' H46E 109.5 . . ? Si4' C46' H46F 109.5 . . ? H46D C46' H46F 109.5 . . ? H46E C46' H46F 109.5 . . ? Si4' N33' Si3' 132(2) . . ? Si4' N33' Si2' 113.1(18) . . ? Si3' N33' Si2' 113.4(19) . . ? C23' Si2' C22' 109.46(9) . . ? C23' Si2' C21' 109.47(8) . . ? C22' Si2' C21' 109.46(9) . . ? C23' Si2' N33' 108.8(14) . . ? C22' Si2' N33' 110.9(14) . . ? C21' Si2' N33' 108.7(14) . . ? Si2' C21' H21T 109.5 . . ? Si2' C21' H21U 109.5 . . ? H21T C21' H21U 109.5 . . ? Si2' C21' H21V 109.5 . . ? H21T C21' H21V 109.5 . . ? H21U C21' H21V 109.5 . . ? Si2' C22' H22M 109.5 . . ? Si2' C22' H22N 109.5 . . ? H22M C22' H22N 109.5 . . ? Si2' C22' H22O 109.5 . . ? H22M C22' H22O 109.5 . . ? H22N C22' H22O 109.5 . . ? Si2' C23' H23M 109.5 . . ? Si2' C23' H23N 109.5 . . ? H23M C23' H23N 109.5 . . ? Si2' C23' H23O 109.5 . . ? H23M C23' H23O 109.5 . . ? H23N C23' H23O 109.5 . . ? N33' Si3' C32' 107.7(13) . . ? N33' Si3' C31' 108.7(15) . . ? C32' Si3' C31' 109.44(8) . . ? N33' Si3' C33' 112.1(15) . . ? C32' Si3' C33' 109.43(8) . . ? C31' Si3' C33' 109.43(9) . . ? Si3' C31' H31F 109.5 . . ? Si3' C31' H31G 109.5 . . ? H31F C31' H31G 109.5 . . ? Si3' C31' H31H 109.5 . . ? H31F C31' H31H 109.5 . . ? H31G C31' H31H 109.5 . . ? Si3' C32' H32D 109.5 . . ? Si3' C32' H32E 109.5 . . ? H32D C32' H32E 109.5 . . ? Si3' C32' H32F 109.5 . . ? H32D C32' H32F 109.5 . . ? H32E C32' H32F 109.5 . . ? Si3' C33' H33D 109.5 . . ? Si3' C33' H33E 109.5 . . ? H33D C33' H33E 109.5 . . ? Si3' C33' H33F 109.5 . . ? H33D C33' H33F 109.5 . . ? H33E C33' H33F 109.5 . . ? C55 O51 C52 106.1(11) . . ? C53 C52 O51 109.0(12) . . ? C53 C52 H52A 109.9 . . ? O51 C52 H52A 109.9 . . ? C53 C52 H52B 109.9 . . ? O51 C52 H52B 109.9 . . ? H52A C52 H52B 108.3 . . ? C52 C53 C54 108.3(11) . . ? C52 C53 H53A 110.0 . . ? C54 C53 H53A 110.0 . . ? C52 C53 H53B 110.0 . . ? C54 C53 H53B 110.0 . . ? H53A C53 H53B 108.4 . . ? C55 C54 C53 107.9(11) . . ? C55 C54 H54A 110.1 . . ? C53 C54 H54A 110.1 . . ? C55 C54 H54B 110.1 . . ? C53 C54 H54B 110.1 . . ? H54A C54 H54B 108.4 . . ? C54 C55 O51 108.5(11) . . ? C54 C55 H55A 110.0 . . ? O51 C55 H55A 110.0 . . ? C54 C55 H55B 110.0 . . ? O51 C55 H55B 110.0 . . ? H55A C55 H55B 108.4 . . ? C62 O61 C65 105.2(15) . . ? C63 C62 O61 107.8(13) . . ? C63 C62 H62A 110.1 . . ? O61 C62 H62A 110.1 . . ? C63 C62 H62B 110.1 . . ? O61 C62 H62B 110.1 . . ? H62A C62 H62B 108.5 . . ? C62 C63 C64 107.7(11) . . ? C62 C63 H63A 110.2 . . ? C64 C63 H63A 110.2 . . ? C62 C63 H63B 110.2 . . ? C64 C63 H63B 110.2 . . ? H63A C63 H63B 108.5 . . ? C65 C64 C63 105.9(14) . . ? C65 C64 H64A 110.6 . . ? C63 C64 H64A 110.6 . . ? C65 C64 H64B 110.6 . . ? C63 C64 H64B 110.6 . . ? H64A C64 H64B 108.7 . . ? C64 C65 O61 106.4(16) . . ? C64 C65 H65A 110.5 . . ? O61 C65 H65A 110.5 . . ? C64 C65 H65B 110.5 . . ? O61 C65 H65B 110.5 . . ? H65A C65 H65B 108.6 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 22.46 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.894 _refine_diff_density_min -0.656 _refine_diff_density_rms 0.132