# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Takuhiro Taniguchi' _publ_contact_author_email tanitaku@mbox.chem.nagoya-u.ac.jp loop_ _publ_author_name 'Takuhiro Taniguchi' 'Jian Wang' 'Stephan Irle' 'Shigehiro Yamaguchi' data_compound3a _database_code_depnum_ccdc_archive 'CCDC 794958' #TrackingRef 'compound3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; N-(dimesitylboryl)carbazole ; _chemical_name_common N-(dimesitylboryl)carbazole _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H30 B N' _chemical_formula_weight 415.36 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' 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 monoclinic _symmetry_space_group_name_H-M C2/c 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 12.716(3) _cell_length_b 10.577(2) _cell_length_c 17.530(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.626(3) _cell_angle_gamma 90.00 _cell_volume 2357.7(9) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 3558 _cell_measurement_theta_min 3.3953 _cell_measurement_theta_max 31.5050 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.170 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 0.066 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9869 _exptl_absorpt_correction_T_max 0.9901 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Saturn70 CCD (4x4 bin mode) with MicroMax-007 ; _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7634 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0263 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2069 _reflns_number_gt 1730 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear 1.3.5 (Rigaku Corp)' _computing_cell_refinement 'CrystalClear 1.3.5 (Rigaku Corp)' _computing_data_reduction 'CrystalClear 1.3.5 (Rigaku Corp)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Yadokari-XG (Wakita, 2005)' _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^)+(0.0682P)^2^+0.8480P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2069 _refine_ls_number_parameters 149 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0509 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.1187 _refine_ls_wR_factor_gt 0.1115 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _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 C1 C -0.02370(10) 0.08385(13) 0.81244(8) 0.0210(3) Uani 1 1 d . . . C2 C -0.04750(11) 0.05332(13) 0.88754(8) 0.0264(3) Uani 1 1 d . . . H1 H -0.0515 -0.0323 0.9036 0.032 Uiso 1 1 calc R . . C3 C -0.06520(12) 0.15120(14) 0.93799(8) 0.0297(4) Uani 1 1 d . . . H2 H -0.0821 0.1320 0.9894 0.036 Uiso 1 1 calc R . . C4 C -0.05890(12) 0.27735(14) 0.91546(8) 0.0290(4) Uani 1 1 d . . . H3 H -0.0725 0.3427 0.9512 0.035 Uiso 1 1 calc R . . C5 C -0.03290(11) 0.30782(13) 0.84132(8) 0.0253(3) Uani 1 1 d . . . H4 H -0.0274 0.3937 0.8259 0.030 Uiso 1 1 calc R . . C6 C -0.01497(10) 0.21071(12) 0.78970(8) 0.0208(3) Uani 1 1 d . . . N1 N 0.0000 0.00287(14) 0.7500 0.0211(4) Uani 1 2 d S . . B1 B 0.0000 -0.1334(2) 0.7500 0.0210(5) Uani 1 2 d S . . C7 C -0.06670(10) -0.20827(12) 0.81031(8) 0.0211(3) Uani 1 1 d . . . C8 C -0.02067(11) -0.29981(12) 0.85889(8) 0.0223(3) Uani 1 1 d . . . C9 C -0.08360(11) -0.36946(13) 0.90774(8) 0.0253(3) Uani 1 1 d . . . H5 H -0.0511 -0.4288 0.9412 0.030 Uiso 1 1 calc R . . C10 C -0.19180(12) -0.35569(13) 0.90953(8) 0.0280(4) Uani 1 1 d . . . C11 C -0.23696(11) -0.26592(13) 0.86135(9) 0.0280(4) Uani 1 1 d . . . H6 H -0.3111 -0.2552 0.8614 0.034 Uiso 1 1 calc R . . C12 C -0.17688(11) -0.19129(13) 0.81315(8) 0.0245(3) Uani 1 1 d . . . C13 C 0.09664(12) -0.32174(14) 0.86161(9) 0.0305(4) Uani 1 1 d . . . H7 H 0.1131 -0.3867 0.8998 0.046 Uiso 1 1 calc R . . H8 H 0.1325 -0.2428 0.8754 0.046 Uiso 1 1 calc R . . H9 H 0.1205 -0.3500 0.8114 0.046 Uiso 1 1 calc R . . C14 C -0.25855(14) -0.43535(16) 0.96123(10) 0.0409(4) Uani 1 1 d . . . H10 H -0.2667 -0.5201 0.9393 0.061 Uiso 1 1 calc R . . H11 H -0.3279 -0.3961 0.9665 0.061 Uiso 1 1 calc R . . H12 H -0.2245 -0.4417 1.0115 0.061 Uiso 1 1 calc R . . C15 C -0.23349(11) -0.09419(15) 0.76427(9) 0.0329(4) Uani 1 1 d . . . H13 H -0.3094 -0.1095 0.7659 0.049 Uiso 1 1 calc R . . H14 H -0.2095 -0.1010 0.7115 0.049 Uiso 1 1 calc R . . H15 H -0.2182 -0.0092 0.7838 0.049 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 C1 0.0211(7) 0.0213(7) 0.0206(7) -0.0021(6) -0.0016(5) -0.0002(5) C2 0.0341(8) 0.0220(7) 0.0230(8) 0.0013(6) 0.0000(6) -0.0017(6) C3 0.0378(9) 0.0304(8) 0.0210(7) -0.0022(6) 0.0025(6) -0.0015(6) C4 0.0354(9) 0.0264(8) 0.0254(8) -0.0070(6) 0.0005(6) 0.0010(6) C5 0.0275(8) 0.0204(7) 0.0280(8) -0.0022(6) -0.0032(6) -0.0002(6) C6 0.0194(7) 0.0204(7) 0.0225(7) 0.0005(5) -0.0038(5) 0.0004(5) N1 0.0267(9) 0.0184(8) 0.0181(8) 0.000 0.0002(6) 0.000 B1 0.0220(11) 0.0199(10) 0.0208(11) 0.000 -0.0061(8) 0.000 C7 0.0248(8) 0.0174(7) 0.0211(7) -0.0043(5) -0.0003(5) -0.0003(5) C8 0.0289(8) 0.0164(7) 0.0217(7) -0.0043(5) 0.0005(6) 0.0002(5) C9 0.0354(9) 0.0192(7) 0.0215(7) -0.0001(6) -0.0005(6) -0.0001(6) C10 0.0345(9) 0.0245(7) 0.0252(8) -0.0039(6) 0.0046(6) -0.0061(6) C11 0.0228(8) 0.0296(8) 0.0318(8) -0.0057(6) 0.0029(6) -0.0034(6) C12 0.0265(8) 0.0214(7) 0.0254(8) -0.0045(6) -0.0006(6) 0.0003(5) C13 0.0307(8) 0.0304(8) 0.0304(8) 0.0054(6) 0.0000(6) 0.0074(6) C14 0.0451(10) 0.0402(9) 0.0377(9) 0.0033(7) 0.0105(7) -0.0093(7) C15 0.0259(8) 0.0344(8) 0.0384(9) 0.0032(7) -0.0030(6) 0.0039(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 C1 C2 1.3921(19) . ? C1 C6 1.4045(19) . ? C1 N1 1.4248(16) . ? C2 C3 1.382(2) . ? C3 C4 1.394(2) . ? C4 C5 1.383(2) . ? C5 C6 1.3894(19) . ? C6 C6 1.447(3) 2_556 ? N1 C1 1.4248(16) 2_556 ? N1 B1 1.442(3) . ? B1 C7 1.5760(17) 2_556 ? B1 C7 1.5760(17) . ? C7 C8 1.4122(19) . ? C7 C12 1.4139(19) . ? C8 C9 1.390(2) . ? C8 C13 1.510(2) . ? C9 C10 1.384(2) . ? C10 C11 1.391(2) . ? C10 C14 1.506(2) . ? C11 C12 1.391(2) . ? C12 C15 1.515(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 120.58(13) . . ? C2 C1 N1 129.58(13) . . ? C6 C1 N1 109.77(12) . . ? C3 C2 C1 118.04(13) . . ? C2 C3 C4 121.70(13) . . ? C5 C4 C3 120.30(13) . . ? C4 C5 C6 118.85(13) . . ? C5 C6 C1 120.49(13) . . ? C5 C6 C6 132.32(8) . 2_556 ? C1 C6 C6 107.18(8) . 2_556 ? C1 N1 C1 106.09(15) 2_556 . ? C1 N1 B1 126.96(7) 2_556 . ? C1 N1 B1 126.96(7) . . ? N1 B1 C7 120.15(8) . 2_556 ? N1 B1 C7 120.15(8) . . ? C7 B1 C7 119.70(16) 2_556 . ? C8 C7 C12 118.05(12) . . ? C8 C7 B1 121.76(11) . . ? C12 C7 B1 120.04(11) . . ? C9 C8 C7 119.83(13) . . ? C9 C8 C13 118.32(13) . . ? C7 C8 C13 121.82(12) . . ? C10 C9 C8 122.50(14) . . ? C9 C10 C11 117.52(13) . . ? C9 C10 C14 121.43(14) . . ? C11 C10 C14 121.04(14) . . ? C10 C11 C12 122.03(14) . . ? C11 C12 C7 120.02(13) . . ? C11 C12 C15 117.88(13) . . ? C7 C12 C15 122.09(13) . . ? 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 C6 C1 C2 C3 1.9(2) . . . . ? N1 C1 C2 C3 178.47(12) . . . . ? C1 C2 C3 C4 -0.5(2) . . . . ? C2 C3 C4 C5 -1.0(2) . . . . ? C3 C4 C5 C6 1.0(2) . . . . ? C4 C5 C6 C1 0.3(2) . . . . ? C4 C5 C6 C6 -178.59(17) . . . 2_556 ? C2 C1 C6 C5 -1.8(2) . . . . ? N1 C1 C6 C5 -179.04(11) . . . . ? C2 C1 C6 C6 177.34(13) . . . 2_556 ? N1 C1 C6 C6 0.13(17) . . . 2_556 ? C2 C1 N1 C1 -176.93(16) . . . 2_556 ? C6 C1 N1 C1 -0.05(7) . . . 2_556 ? C2 C1 N1 B1 3.07(16) . . . . ? C6 C1 N1 B1 179.95(7) . . . . ? C1 N1 B1 C7 23.14(8) 2_556 . . 2_556 ? C1 N1 B1 C7 -156.86(8) . . . 2_556 ? C1 N1 B1 C7 -156.86(8) 2_556 . . . ? C1 N1 B1 C7 23.14(8) . . . . ? N1 B1 C7 C8 -124.96(10) . . . . ? C7 B1 C7 C8 55.04(10) 2_556 . . . ? N1 B1 C7 C12 59.63(12) . . . . ? C7 B1 C7 C12 -120.37(12) 2_556 . . . ? C12 C7 C8 C9 -0.28(19) . . . . ? B1 C7 C8 C9 -175.79(12) . . . . ? C12 C7 C8 C13 -178.07(12) . . . . ? B1 C7 C8 C13 6.4(2) . . . . ? C7 C8 C9 C10 2.0(2) . . . . ? C13 C8 C9 C10 179.82(13) . . . . ? C8 C9 C10 C11 -1.6(2) . . . . ? C8 C9 C10 C14 178.00(13) . . . . ? C9 C10 C11 C12 -0.4(2) . . . . ? C14 C10 C11 C12 179.98(13) . . . . ? C10 C11 C12 C7 2.0(2) . . . . ? C10 C11 C12 C15 -178.61(13) . . . . ? C8 C7 C12 C11 -1.64(19) . . . . ? B1 C7 C12 C11 173.94(13) . . . . ? C8 C7 C12 C15 179.03(13) . . . . ? B1 C7 C12 C15 -5.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.178 _refine_diff_density_min -0.178 _refine_diff_density_rms 0.038 # Attachment 'compound4.CIF' data_compound4 _database_code_depnum_ccdc_archive 'CCDC 794959' #TrackingRef 'compound4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; N-(dimesitylboryl)-2,5-di(2-thienyl)pyrrole ; _chemical_name_common N-(dimesitylboryl)-2,5-di(2-thienyl)pyrrole _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H30 B N S2' _chemical_formula_weight 479.48 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.49(3) _cell_length_b 12.61(4) _cell_length_c 12.72(6) _cell_angle_alpha 105.34(9) _cell_angle_beta 91.55(8) _cell_angle_gamma 102.24(8) _cell_volume 1278(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 66 _cell_measurement_theta_min 2.0364 _cell_measurement_theta_max 31.5050 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.246 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 508 _exptl_absorpt_coefficient_mu 0.228 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9559 _exptl_absorpt_correction_T_max 0.9776 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Saturn70 CCD (4x4 bin mode) with MicroMax-007 ; _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8656 _diffrn_reflns_av_R_equivalents 0.0402 _diffrn_reflns_av_sigmaI/netI 0.0631 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4408 _reflns_number_gt 2797 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear 1.3.5 (Rigaku Corp)' _computing_cell_refinement 'CrystalClear 1.3.5 (Rigaku Corp)' _computing_data_reduction 'CrystalClear 1.3.5 (Rigaku Corp)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Yadokari-XG (Wakita, 2005)' _computing_publication_material 'SHELXS-97 (Sheldrick, 1990)' _refine_special_details ; The thiophene ring consisting of (S2, C9-C12) was disordered and was solved using appropriate models. Thus, two sets of thiophene ring, i.e., (S2A, C9, C10A, C11A, C12A) and (S2B, C9, C10B, C11B, C12B), were placed and their occupancies were refined to be 0.85 and 0.15. These disordered thiophene rings were restrained by SADI and SIMU instruction during refinement. 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^)+(0.1229P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4408 _refine_ls_number_parameters 344 _refine_ls_number_restraints 53 _refine_ls_R_factor_all 0.0942 _refine_ls_R_factor_gt 0.0639 _refine_ls_wR_factor_ref 0.2078 _refine_ls_wR_factor_gt 0.1834 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.069 _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 N1 N 0.7400(3) 0.2044(2) 0.6391(2) 0.0273(6) Uani 1 1 d . . . C1 C 0.8038(4) 0.2652(3) 0.5663(3) 0.0296(8) Uani 1 1 d . . . C2 C 0.8705(4) 0.1963(3) 0.4868(3) 0.0328(8) Uani 1 1 d . . . H1 H 0.9242 0.2168 0.4281 0.039 Uiso 1 1 calc R . . C3 C 0.8458(4) 0.0901(3) 0.5071(3) 0.0326(8) Uani 1 1 d . . . H2 H 0.8789 0.0260 0.4640 0.039 Uiso 1 1 calc R . . C4 C 0.7664(4) 0.0945(3) 0.5991(3) 0.0275(7) Uani 1 1 d . A . C5 C 0.8094(4) 0.3853(3) 0.5813(3) 0.0307(8) Uani 1 1 d . . . C6 C 0.9138(5) 0.4770(3) 0.6518(3) 0.0414(9) Uani 1 1 d . . . H3 H 0.9974 0.4715 0.6999 0.050 Uiso 1 1 calc R . . C7 C 0.8815(5) 0.5803(3) 0.6438(3) 0.0499(10) Uani 1 1 d . . . H4 H 0.9388 0.6519 0.6886 0.060 Uiso 1 1 calc R . . C8 C 0.7627(5) 0.5674(3) 0.5675(3) 0.0472(10) Uani 1 1 d . . . H5 H 0.7276 0.6283 0.5507 0.057 Uiso 1 1 calc R . . S1 S 0.68207(14) 0.42953(9) 0.50405(8) 0.0493(3) Uani 1 1 d . . . C9 C 0.6966(4) 0.0020(3) 0.6448(3) 0.0288(8) Uani 1 1 d D . . C11A C 0.5103(8) -0.1368(6) 0.6971(7) 0.0381(13) Uani 0.852(5) 1 d PDU A 1 H28 H 0.4062 -0.1758 0.7083 0.046 Uiso 0.852(5) 1 calc PR A 1 C12A C 0.6519(6) -0.1632(6) 0.7200(6) 0.0398(14) Uani 0.852(5) 1 d PDU A 1 H29 H 0.6595 -0.2238 0.7496 0.048 Uiso 0.852(5) 1 calc PR A 1 S2B S 0.500(2) -0.044(2) 0.650(3) 0.031(3) Uani 0.148(5) 1 d PDU A 2 B1 B 0.6888(4) 0.2523(3) 0.7478(3) 0.0269(8) Uani 1 1 d . . . C16 C 0.7394(4) 0.2053(3) 0.8443(2) 0.0260(7) Uani 1 1 d . . . C17 C 0.6260(4) 0.1659(3) 0.9124(3) 0.0286(8) Uani 1 1 d . . . C18 C 0.6769(4) 0.1311(3) 0.9998(3) 0.0320(8) Uani 1 1 d . . . H6 H 0.5984 0.1019 1.0429 0.038 Uiso 1 1 calc R . . C19 C 0.8394(5) 0.1376(3) 1.0259(3) 0.0358(8) Uani 1 1 d . . . C20 C 0.9509(4) 0.1784(3) 0.9605(3) 0.0345(8) Uani 1 1 d . . . H7 H 1.0627 0.1853 0.9785 0.041 Uiso 1 1 calc R . . C21 C 0.9052(4) 0.2095(3) 0.8694(3) 0.0304(8) Uani 1 1 d . . . C22 C 0.4483(4) 0.1619(3) 0.8936(3) 0.0379(9) Uani 1 1 d . . . H8 H 0.4303 0.1894 0.8301 0.057 Uiso 1 1 calc R . . H9 H 0.4132 0.2098 0.9585 0.057 Uiso 1 1 calc R . . H10 H 0.3860 0.0840 0.8801 0.057 Uiso 1 1 calc R . . C23 C 0.8936(6) 0.1036(4) 1.1242(3) 0.0527(11) Uani 1 1 d . . . H11 H 1.0116 0.1143 1.1296 0.079 Uiso 1 1 calc R . . H12 H 0.8432 0.0240 1.1158 0.079 Uiso 1 1 calc R . . H13 H 0.8610 0.1505 1.1908 0.079 Uiso 1 1 calc R . . C24 C 1.0379(4) 0.2518(3) 0.8037(3) 0.0433(10) Uani 1 1 d . . . H14 H 0.9901 0.2708 0.7420 0.065 Uiso 1 1 calc R . . H15 H 1.0973 0.1929 0.7760 0.065 Uiso 1 1 calc R . . H16 H 1.1124 0.3192 0.8505 0.065 Uiso 1 1 calc R . . C25 C 0.5941(4) 0.3480(3) 0.7651(2) 0.0259(7) Uani 1 1 d . . . C26 C 0.4497(4) 0.3328(3) 0.6992(2) 0.0275(7) Uani 1 1 d . . . C27 C 0.3634(4) 0.4173(3) 0.7173(3) 0.0300(8) Uani 1 1 d . . . H17 H 0.2653 0.4046 0.6734 0.036 Uiso 1 1 calc R . . C28 C 0.4153(4) 0.5193(3) 0.7970(3) 0.0332(8) Uani 1 1 d . . . C29 C 0.5562(5) 0.5339(3) 0.8621(3) 0.0364(9) Uani 1 1 d . . . H18 H 0.5927 0.6027 0.9180 0.044 Uiso 1 1 calc R . . C30 C 0.6461(4) 0.4517(3) 0.8488(3) 0.0313(8) Uani 1 1 d . . . C31 C 0.3816(4) 0.2259(3) 0.6100(3) 0.0339(8) Uani 1 1 d . . . H19 H 0.4529 0.1734 0.6062 0.051 Uiso 1 1 calc R . . H20 H 0.3740 0.2436 0.5398 0.051 Uiso 1 1 calc R . . H21 H 0.2736 0.1911 0.6259 0.051 Uiso 1 1 calc R . . C32 C 0.3219(5) 0.6109(3) 0.8136(3) 0.0478(10) Uani 1 1 d . . . H22 H 0.2267 0.5860 0.7603 0.072 Uiso 1 1 calc R . . H23 H 0.3913 0.6796 0.8033 0.072 Uiso 1 1 calc R . . H24 H 0.2871 0.6269 0.8879 0.072 Uiso 1 1 calc R . . C33 C 0.8004(5) 0.4785(3) 0.9218(3) 0.0504(11) Uani 1 1 d . . . H25 H 0.8516 0.4139 0.9036 0.076 Uiso 1 1 calc R . . H26 H 0.7757 0.4938 0.9984 0.076 Uiso 1 1 calc R . . H27 H 0.8743 0.5450 0.9108 0.076 Uiso 1 1 calc R . . S2A S 0.81615(18) -0.07379(13) 0.68926(16) 0.0402(5) Uani 0.852(5) 1 d PDU A 1 C10A C 0.5411(12) -0.0415(15) 0.6534(16) 0.030(2) Uani 0.852(5) 1 d PDU A 1 H30 H 0.4562 -0.0110 0.6320 0.036 Uiso 0.852(5) 1 calc PR A 1 C10B C 0.788(4) -0.051(3) 0.693(4) 0.041(3) Uani 0.148(5) 1 d PDU A 2 H31 H 0.9020 -0.0252 0.7078 0.049 Uiso 0.148(5) 1 calc PR A 2 C11B C 0.703(5) -0.148(3) 0.721(4) 0.038(2) Uani 0.148(5) 1 d PDU A 2 H32 H 0.7468 -0.2012 0.7462 0.046 Uiso 0.148(5) 1 calc PR A 2 C12B C 0.544(6) -0.148(4) 0.704(4) 0.038(2) Uani 0.148(5) 1 d PDU A 2 H33 H 0.4605 -0.2025 0.7214 0.046 Uiso 0.148(5) 1 calc PR A 2 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 N1 0.0297(15) 0.0258(15) 0.0295(15) 0.0088(12) 0.0026(12) 0.0115(12) C1 0.0292(18) 0.0302(18) 0.0315(18) 0.0123(15) 0.0002(14) 0.0068(15) C2 0.0331(19) 0.038(2) 0.0312(18) 0.0135(15) 0.0095(15) 0.0111(16) C3 0.036(2) 0.033(2) 0.0320(19) 0.0079(15) 0.0080(15) 0.0156(16) C4 0.0286(18) 0.0275(18) 0.0290(17) 0.0094(14) -0.0013(14) 0.0102(14) C5 0.0301(18) 0.0330(19) 0.0350(19) 0.0158(15) 0.0099(15) 0.0114(15) C6 0.044(2) 0.032(2) 0.049(2) 0.0182(17) -0.0084(18) 0.0028(17) C7 0.057(3) 0.030(2) 0.058(3) 0.0097(18) 0.004(2) 0.0016(19) C8 0.065(3) 0.037(2) 0.052(2) 0.0205(18) 0.015(2) 0.024(2) S1 0.0604(7) 0.0397(6) 0.0525(7) 0.0185(5) -0.0085(5) 0.0161(5) C9 0.0316(19) 0.0246(18) 0.0304(18) 0.0031(14) 0.0013(14) 0.0131(15) C11A 0.045(4) 0.033(2) 0.040(2) 0.0133(17) 0.008(2) 0.011(2) C12A 0.048(4) 0.033(2) 0.044(2) 0.0173(18) 0.007(3) 0.012(2) S2B 0.019(7) 0.030(3) 0.044(3) 0.009(3) 0.005(5) 0.004(5) B1 0.0231(19) 0.027(2) 0.0269(19) 0.0045(15) 0.0016(15) 0.0022(16) C16 0.0279(17) 0.0252(17) 0.0253(16) 0.0050(13) 0.0024(13) 0.0092(14) C17 0.0324(19) 0.0268(18) 0.0275(17) 0.0070(14) 0.0008(14) 0.0093(14) C18 0.043(2) 0.0257(18) 0.0282(18) 0.0076(14) 0.0061(15) 0.0089(16) C19 0.050(2) 0.0258(18) 0.0303(18) 0.0051(14) -0.0068(16) 0.0095(16) C20 0.033(2) 0.031(2) 0.039(2) 0.0060(16) -0.0062(15) 0.0113(16) C21 0.0310(19) 0.0275(18) 0.0328(18) 0.0061(14) 0.0017(14) 0.0099(15) C22 0.031(2) 0.044(2) 0.041(2) 0.0155(17) 0.0088(16) 0.0088(17) C23 0.067(3) 0.047(3) 0.044(2) 0.0161(19) -0.013(2) 0.012(2) C24 0.0241(19) 0.057(3) 0.048(2) 0.0170(19) 0.0003(16) 0.0059(18) C25 0.0289(18) 0.0257(17) 0.0249(16) 0.0097(13) 0.0034(13) 0.0065(14) C26 0.0311(18) 0.0258(17) 0.0271(17) 0.0092(13) 0.0042(14) 0.0069(14) C27 0.0296(18) 0.0304(19) 0.0326(18) 0.0100(15) 0.0051(15) 0.0105(15) C28 0.038(2) 0.0264(19) 0.0383(19) 0.0104(15) 0.0085(16) 0.0120(16) C29 0.047(2) 0.0268(19) 0.0301(18) 0.0013(15) 0.0041(16) 0.0058(17) C30 0.0330(19) 0.0283(19) 0.0294(18) 0.0062(14) -0.0010(15) 0.0029(15) C31 0.035(2) 0.0259(18) 0.0392(19) 0.0034(15) -0.0032(16) 0.0114(15) C32 0.052(3) 0.033(2) 0.059(3) 0.0056(19) 0.008(2) 0.021(2) C33 0.052(3) 0.036(2) 0.052(2) 0.0000(18) -0.0181(19) 0.0032(19) S2A 0.0403(8) 0.0414(9) 0.0511(8) 0.0241(7) 0.0049(6) 0.0210(6) C10A 0.022(6) 0.030(3) 0.040(2) 0.008(2) 0.002(5) 0.010(5) C10B 0.040(5) 0.040(5) 0.054(5) 0.025(5) 0.005(5) 0.019(5) C11B 0.046(5) 0.032(4) 0.042(3) 0.017(3) 0.007(4) 0.012(4) C12B 0.046(5) 0.032(4) 0.041(3) 0.017(3) 0.009(4) 0.011(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C1 1.401(6) . ? N1 C4 1.413(6) . ? N1 B1 1.472(7) . ? C1 C2 1.369(6) . ? C1 C5 1.466(7) . ? C2 C3 1.405(6) . ? C2 H1 0.9500 . ? C3 C4 1.359(7) . ? C3 H2 0.9500 . ? C4 C9 1.462(6) . ? C5 C6 1.379(6) . ? C5 S1 1.712(6) . ? C6 C7 1.415(7) . ? C6 H3 0.9500 . ? C7 C8 1.334(7) . ? C7 H4 0.9500 . ? C8 S1 1.693(6) . ? C8 H5 0.9500 . ? C9 C10A 1.336(12) . ? C9 C10B 1.36(2) . ? C9 S2B 1.659(17) . ? C9 S2A 1.711(5) . ? C11A C12A 1.357(8) . ? C11A C10A 1.431(16) . ? C11A H28 0.9500 . ? C12A S2A 1.721(7) . ? C12A H29 0.9500 . ? S2B C12B 1.73(2) . ? B1 C25 1.559(6) . ? B1 C16 1.583(7) . ? C16 C17 1.412(6) . ? C16 C21 1.421(7) . ? C17 C18 1.388(7) . ? C17 C22 1.508(8) . ? C18 C19 1.390(7) . ? C18 H6 0.9500 . ? C19 C20 1.384(6) . ? C19 C23 1.514(7) . ? C20 C21 1.388(7) . ? C20 H7 0.9500 . ? C21 C24 1.511(6) . ? C22 H8 0.9800 . ? C22 H9 0.9800 . ? C22 H10 0.9800 . ? C23 H11 0.9800 . ? C23 H12 0.9800 . ? C23 H13 0.9800 . ? C24 H14 0.9800 . ? C24 H15 0.9800 . ? C24 H16 0.9800 . ? C25 C26 1.414(6) . ? C25 C30 1.426(6) . ? C26 C27 1.391(6) . ? C26 C31 1.504(6) . ? C27 C28 1.386(6) . ? C27 H17 0.9500 . ? C28 C29 1.386(7) . ? C28 C32 1.509(6) . ? C29 C30 1.391(6) . ? C29 H18 0.9500 . ? C30 C33 1.507(7) . ? C31 H19 0.9800 . ? C31 H20 0.9800 . ? C31 H21 0.9800 . ? C32 H22 0.9800 . ? C32 H23 0.9800 . ? C32 H24 0.9800 . ? C33 H25 0.9800 . ? C33 H26 0.9800 . ? C33 H27 0.9800 . ? C10A H30 0.9500 . ? C10B C11B 1.42(2) . ? C10B H31 0.9500 . ? C11B C12B 1.36(2) . ? C11B H32 0.9500 . ? C12B H33 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 C4 106.7(3) . . ? C1 N1 B1 126.1(4) . . ? C4 N1 B1 126.0(3) . . ? C2 C1 N1 108.4(4) . . ? C2 C1 C5 127.0(3) . . ? N1 C1 C5 124.3(3) . . ? C1 C2 C3 108.1(4) . . ? C1 C2 H1 126.0 . . ? C3 C2 H1 126.0 . . ? C4 C3 C2 108.4(3) . . ? C4 C3 H2 125.8 . . ? C2 C3 H2 125.8 . . ? C3 C4 N1 108.4(3) . . ? C3 C4 C9 128.5(3) . . ? N1 C4 C9 122.6(3) . . ? C6 C5 C1 128.1(4) . . ? C6 C5 S1 110.2(4) . . ? C1 C5 S1 121.8(3) . . ? C5 C6 C7 111.9(4) . . ? C5 C6 H3 124.0 . . ? C7 C6 H3 124.0 . . ? C8 C7 C6 113.5(4) . . ? C8 C7 H4 123.3 . . ? C6 C7 H4 123.3 . . ? C7 C8 S1 111.8(3) . . ? C7 C8 H5 124.1 . . ? S1 C8 H5 124.1 . . ? C8 S1 C5 92.6(3) . . ? C10A C9 C10B 108(2) . . ? C10A C9 C4 129.1(8) . . ? C10B C9 C4 123.0(17) . . ? C10A C9 S2B 5.0(16) . . ? C10B C9 S2B 112.8(18) . . ? C4 C9 S2B 124.1(9) . . ? C10A C9 S2A 109.8(8) . . ? C10B C9 S2A 7(2) . . ? C4 C9 S2A 121.0(3) . . ? S2B C9 S2A 114.8(10) . . ? C12A C11A C10A 110.0(8) . . ? C12A C11A H28 125.0 . . ? C10A C11A H28 125.0 . . ? C11A C12A S2A 112.0(6) . . ? C11A C12A H29 124.0 . . ? S2A C12A H29 124.0 . . ? C9 S2B C12B 88(2) . . ? N1 B1 C25 120.1(3) . . ? N1 B1 C16 117.1(4) . . ? C25 B1 C16 122.8(3) . . ? C17 C16 C21 117.9(4) . . ? C17 C16 B1 122.1(4) . . ? C21 C16 B1 119.8(3) . . ? C18 C17 C16 120.2(4) . . ? C18 C17 C22 118.4(3) . . ? C16 C17 C22 121.4(4) . . ? C17 C18 C19 121.9(3) . . ? C17 C18 H6 119.0 . . ? C19 C18 H6 119.0 . . ? C20 C19 C18 117.8(4) . . ? C20 C19 C23 120.9(4) . . ? C18 C19 C23 121.2(4) . . ? C19 C20 C21 122.3(4) . . ? C19 C20 H7 118.8 . . ? C21 C20 H7 118.8 . . ? C20 C21 C16 119.7(3) . . ? C20 C21 C24 117.5(4) . . ? C16 C21 C24 122.8(4) . . ? C17 C22 H8 109.5 . . ? C17 C22 H9 109.5 . . ? H8 C22 H9 109.5 . . ? C17 C22 H10 109.5 . . ? H8 C22 H10 109.5 . . ? H9 C22 H10 109.5 . . ? C19 C23 H11 109.5 . . ? C19 C23 H12 109.5 . . ? H11 C23 H12 109.5 . . ? C19 C23 H13 109.5 . . ? H11 C23 H13 109.5 . . ? H12 C23 H13 109.5 . . ? C21 C24 H14 109.5 . . ? C21 C24 H15 109.5 . . ? H14 C24 H15 109.5 . . ? C21 C24 H16 109.5 . . ? H14 C24 H16 109.5 . . ? H15 C24 H16 109.5 . . ? C26 C25 C30 117.7(3) . . ? C26 C25 B1 120.5(3) . . ? C30 C25 B1 121.8(4) . . ? C27 C26 C25 120.1(3) . . ? C27 C26 C31 117.6(4) . . ? C25 C26 C31 122.3(3) . . ? C28 C27 C26 122.5(4) . . ? C28 C27 H17 118.8 . . ? C26 C27 H17 118.8 . . ? C29 C28 C27 117.4(3) . . ? C29 C28 C32 120.9(4) . . ? C27 C28 C32 121.6(4) . . ? C28 C29 C30 122.6(4) . . ? C28 C29 H18 118.7 . . ? C30 C29 H18 118.7 . . ? C29 C30 C25 119.7(4) . . ? C29 C30 C33 118.0(4) . . ? C25 C30 C33 122.3(3) . . ? C26 C31 H19 109.5 . . ? C26 C31 H20 109.5 . . ? H19 C31 H20 109.5 . . ? C26 C31 H21 109.5 . . ? H19 C31 H21 109.5 . . ? H20 C31 H21 109.5 . . ? C28 C32 H22 109.5 . . ? C28 C32 H23 109.5 . . ? H22 C32 H23 109.5 . . ? C28 C32 H24 109.5 . . ? H22 C32 H24 109.5 . . ? H23 C32 H24 109.5 . . ? C30 C33 H25 109.5 . . ? C30 C33 H26 109.5 . . ? H25 C33 H26 109.5 . . ? C30 C33 H27 109.5 . . ? H25 C33 H27 109.5 . . ? H26 C33 H27 109.5 . . ? C9 S2A C12A 92.4(4) . . ? C9 C10A C11A 115.8(10) . . ? C9 C10A H30 122.1 . . ? C11A C10A H30 122.1 . . ? C9 C10B C11B 116(3) . . ? C9 C10B H31 122.0 . . ? C11B C10B H31 122.0 . . ? C12B C11B C10B 105(4) . . ? C12B C11B H32 127.7 . . ? C10B C11B H32 127.7 . . ? C11B C12B S2B 117(4) . . ? C11B C12B H33 121.4 . . ? S2B C12B H33 121.4 . . ? 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 C4 N1 C1 C2 -1.6(4) . . . . ? B1 N1 C1 C2 166.2(3) . . . . ? C4 N1 C1 C5 -176.5(3) . . . . ? B1 N1 C1 C5 -8.6(5) . . . . ? N1 C1 C2 C3 1.5(4) . . . . ? C5 C1 C2 C3 176.1(3) . . . . ? C1 C2 C3 C4 -0.7(4) . . . . ? C2 C3 C4 N1 -0.3(4) . . . . ? C2 C3 C4 C9 171.6(3) . . . . ? C1 N1 C4 C3 1.2(4) . . . . ? B1 N1 C4 C3 -166.7(3) . . . . ? C1 N1 C4 C9 -171.3(3) . . . . ? B1 N1 C4 C9 20.8(5) . . . . ? C2 C1 C5 C6 -97.7(6) . . . . ? N1 C1 C5 C6 76.1(6) . . . . ? C2 C1 C5 S1 79.8(6) . . . . ? N1 C1 C5 S1 -106.4(5) . . . . ? C1 C5 C6 C7 -179.6(3) . . . . ? S1 C5 C6 C7 2.7(4) . . . . ? C5 C6 C7 C8 -2.6(5) . . . . ? C6 C7 C8 S1 1.3(5) . . . . ? C7 C8 S1 C5 0.2(3) . . . . ? C6 C5 S1 C8 -1.7(3) . . . . ? C1 C5 S1 C8 -179.6(3) . . . . ? C3 C4 C9 C10A -112.5(12) . . . . ? N1 C4 C9 C10A 58.3(12) . . . . ? C3 C4 C9 C10B 72(3) . . . . ? N1 C4 C9 C10B -118(3) . . . . ? C3 C4 C9 S2B -112.5(15) . . . . ? N1 C4 C9 S2B 58.3(15) . . . . ? C3 C4 C9 S2A 63.1(5) . . . . ? N1 C4 C9 S2A -126.0(3) . . . . ? C10A C11A C12A S2A 0.1(11) . . . . ? C10A C9 S2B C12B -3(22) . . . . ? C10B C9 S2B C12B -7(4) . . . . ? C4 C9 S2B C12B 177(2) . . . . ? S2A C9 S2B C12B 1(3) . . . . ? C1 N1 B1 C25 41.1(5) . . . . ? C4 N1 B1 C25 -153.4(3) . . . . ? C1 N1 B1 C16 -136.9(4) . . . . ? C4 N1 B1 C16 28.6(5) . . . . ? N1 B1 C16 C17 -128.7(4) . . . . ? C25 B1 C16 C17 53.3(5) . . . . ? N1 B1 C16 C21 55.9(5) . . . . ? C25 B1 C16 C21 -122.0(4) . . . . ? C21 C16 C17 C18 -1.0(5) . . . . ? B1 C16 C17 C18 -176.5(3) . . . . ? C21 C16 C17 C22 178.2(3) . . . . ? B1 C16 C17 C22 2.7(5) . . . . ? C16 C17 C18 C19 2.6(5) . . . . ? C22 C17 C18 C19 -176.6(3) . . . . ? C17 C18 C19 C20 -1.2(5) . . . . ? C17 C18 C19 C23 177.5(3) . . . . ? C18 C19 C20 C21 -1.7(5) . . . . ? C23 C19 C20 C21 179.5(3) . . . . ? C19 C20 C21 C16 3.2(5) . . . . ? C19 C20 C21 C24 -179.4(3) . . . . ? C17 C16 C21 C20 -1.7(5) . . . . ? B1 C16 C21 C20 173.8(3) . . . . ? C17 C16 C21 C24 -179.0(3) . . . . ? B1 C16 C21 C24 -3.4(5) . . . . ? N1 B1 C25 C26 54.9(5) . . . . ? C16 B1 C25 C26 -127.2(4) . . . . ? N1 B1 C25 C30 -126.9(4) . . . . ? C16 B1 C25 C30 51.0(5) . . . . ? C30 C25 C26 C27 -0.1(5) . . . . ? B1 C25 C26 C27 178.1(3) . . . . ? C30 C25 C26 C31 -178.8(3) . . . . ? B1 C25 C26 C31 -0.5(5) . . . . ? C25 C26 C27 C28 1.6(5) . . . . ? C31 C26 C27 C28 -179.7(3) . . . . ? C26 C27 C28 C29 -2.0(5) . . . . ? C26 C27 C28 C32 178.6(3) . . . . ? C27 C28 C29 C30 1.1(5) . . . . ? C32 C28 C29 C30 -179.5(3) . . . . ? C28 C29 C30 C25 0.3(5) . . . . ? C28 C29 C30 C33 177.9(3) . . . . ? C26 C25 C30 C29 -0.8(5) . . . . ? B1 C25 C30 C29 -179.0(3) . . . . ? C26 C25 C30 C33 -178.3(3) . . . . ? B1 C25 C30 C33 3.5(5) . . . . ? C10A C9 S2A C12A -0.5(10) . . . . ? C10B C9 S2A C12A 75(13) . . . . ? C4 C9 S2A C12A -176.9(3) . . . . ? S2B C9 S2A C12A -0.8(13) . . . . ? C11A C12A S2A C9 0.2(5) . . . . ? C10B C9 C10A C11A -7(3) . . . . ? C4 C9 C10A C11A 176.7(8) . . . . ? S2B C9 C10A C11A 177(25) . . . . ? S2A C9 C10A C11A 0.6(17) . . . . ? C12A C11A C10A C9 -0.5(18) . . . . ? C10A C9 C10B C11B 11(5) . . . . ? C4 C9 C10B C11B -172(3) . . . . ? S2B C9 C10B C11B 11(5) . . . . ? S2A C9 C10B C11B -96(15) . . . . ? C9 C10B C11B C12B -9(6) . . . . ? C10B C11B C12B S2B 4(6) . . . . ? C9 S2B C12B C11B 2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.471 _refine_diff_density_min -0.428 _refine_diff_density_rms 0.070