# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2005 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Raymond Ziessel' _publ_contact_author_address ; Laboratoire de Chimie Universit\'e Louis Pasteur, d'Electronique et de Photonique Moleculaires ECPM, 1 rue Blaise Pascal Strasbourg F-67008 FRANCE ; _publ_contact_author_email ZIESSEL@CHIMIE.U-STRASBG.FR loop_ _publ_author_name _publ_author_address R.Ziessel ;Laboratoire de Chimie Mol\'eculaire, Ecole de Chimie, Polym\`eres, Mat\'eriaux (ECPM), Universite Louis Pasteur (ULP), 25 rue Becquerel 67087 Strasbourg Cedex 02 France ; G.Ulrich ; Laboratoire de Chimie Mol\'eculaire, Ecole de Chimie, Polym\`eres, Mat\'eriaux (ECPM), Universite Louis Pasteur (ULP), 25 rue Becquerel 67087 Strasbourg Cedex 02 France ; P.Retailleau ; ICSN-CNRS 1 avenue de la Terrasse 91198 Gif sur Yvette France ; A.Harriman ; Molecular Photonics Laboratory School of Natural Sciences - Chemistry Bedson Building University of Newcastle Newcastle upon Tyne NE1 7RU UK ; _publ_section_title ; Engineering of Electronically Decoupled Difluoroindacene-pyrene Dyad Possessing Large Stokes Shifts and High Affinity for DNA ; data_GU65 _database_code_depnum_ccdc_archive 'CCDC 263269' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 4,4-difluoro-8-(-1-pyrenyl)-1,3,5,7-tetramethyl-2,4-diethyl-4-bora- 3a,4a-diaza-s-indacene ; _chemical_name_common ; 4,4-difluoro-8-(-1-pyrenyl)-1,3,5,7-tetramethyl-2,4-diethyl-4- bora-3a,4a-diaza-s-indacene ; _chemical_melting_point ? _chemical_formula_moiety 'C33 H31 B F2 N2, C1 H3 N1 O2' _chemical_formula_sum 'C34 H34 B F2 N3 O2' _chemical_formula_weight 565.45 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.266(4) _cell_length_b 12.168(3) _cell_length_c 17.628(4) _cell_angle_alpha 100.33 _cell_angle_beta 90.79(2) _cell_angle_gamma 104.64 _cell_volume 1480.6(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2967 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 23.257 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_min 0.025 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.268 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 596 _exptl_absorpt_coefficient_mu 0.087 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; very thin plate poorly diffracting ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius kappa-CCD diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6784 _diffrn_reflns_av_R_equivalents 0.0271 _diffrn_reflns_av_sigmaI/netI 0.0534 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 23.24 _reflns_number_total 4181 _reflns_number_gt 2784 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO (Otwinowski & Minor, 1997) COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) COLLECT (Hooft, 1998)' _computing_data_reduction 'HKL package (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1980-2004)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections except for four Fo^2^<< Fc^2^ near the beamstop. 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. Maximum residual electron density is located nearby the nitromethane molecule (0.70 at 1.29 A from N1'). ; _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^)+(0.1192P)^2^+1.0874P] 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 4181 _refine_ls_number_parameters 381 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1091 _refine_ls_R_factor_gt 0.0740 _refine_ls_wR_factor_ref 0.2367 _refine_ls_wR_factor_gt 0.2070 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.030 _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 B B 0.0546(8) 0.0234(4) 0.3376(3) 0.0600(13) Uani 1 1 d . . . F1 F -0.0791(4) -0.0826(2) 0.31429(15) 0.0828(8) Uani 1 1 d . . . F2 F 0.1340(4) 0.0267(2) 0.41046(12) 0.0834(8) Uani 1 1 d . . . N1A N -0.0403(5) 0.1234(3) 0.34004(17) 0.0546(8) Uani 1 1 d . . . N1B N 0.2126(5) 0.0395(3) 0.28009(17) 0.0538(8) Uani 1 1 d . . . C2A C -0.1139(6) 0.2853(3) 0.3148(2) 0.0595(10) Uani 1 1 d . . . C2B C 0.4157(6) 0.1154(3) 0.1944(2) 0.0535(10) Uani 1 1 d . . . C3A C -0.2361(6) 0.2404(4) 0.3681(2) 0.0659(11) Uani 1 1 d . . . C3B C 0.4597(6) 0.0159(3) 0.2084(2) 0.0588(11) Uani 1 1 d . . . C4A C -0.1876(6) 0.1412(4) 0.3824(2) 0.0611(11) Uani 1 1 d . . . C4B C 0.3326(6) -0.0287(3) 0.2617(2) 0.0564(10) Uani 1 1 d . . . C5A C 0.0091(6) 0.2116(3) 0.2970(2) 0.0527(10) Uani 1 1 d . . . C5B C 0.2592(6) 0.1298(3) 0.2391(2) 0.0508(10) Uani 1 1 d . . . C6A C -0.1206(7) 0.3908(4) 0.2830(3) 0.0772(13) Uani 1 1 d . . . H6A H -0.0229 0.4560 0.3093 0.093 Uiso 1 1 calc R . . H6B H -0.2430 0.4062 0.2905 0.093 Uiso 1 1 calc R . . H6C H -0.1001 0.3778 0.2288 0.093 Uiso 1 1 calc R . . C6B C 0.5211(6) 0.1907(4) 0.1420(3) 0.0695(12) Uani 1 1 d . . . H6D H 0.6452 0.1777 0.1353 0.083 Uiso 1 1 calc R . . H6E H 0.5338 0.2705 0.1643 0.083 Uiso 1 1 calc R . . H6F H 0.4516 0.1723 0.0926 0.083 Uiso 1 1 calc R . . C7A C -0.3865(7) 0.2915(5) 0.4071(3) 0.0889(15) Uani 1 1 d . . . H7A H -0.4820 0.2308 0.4240 0.102 Uiso 1 1 calc R . . H7B H -0.4488 0.3226 0.3702 0.102 Uiso 1 1 calc R . . C8A C -0.3049(10) 0.3868(6) 0.4763(4) 0.135(3) Uani 1 1 d . . . H8A H -0.2522 0.3550 0.5149 0.162 Uiso 1 1 calc R . . H8B H -0.4042 0.4198 0.4973 0.162 Uiso 1 1 calc R . . H8C H -0.2066 0.4456 0.4603 0.162 Uiso 1 1 calc R . . C7B C 0.6097(6) -0.0376(4) 0.1717(3) 0.0733(13) Uani 1 1 d . . . H7C H 0.6262 -0.0971 0.1991 0.084 Uiso 1 1 calc R . . H7D H 0.7299 0.0211 0.1769 0.084 Uiso 1 1 calc R . . C8B C 0.5616(7) -0.0903(4) 0.0872(3) 0.0810(14) Uani 1 1 d . . . H8D H 0.4384 -0.1445 0.0812 0.097 Uiso 1 1 calc R . . H8E H 0.6556 -0.1296 0.0682 0.097 Uiso 1 1 calc R . . H8F H 0.5603 -0.0304 0.0586 0.097 Uiso 1 1 calc R . . C9A C -0.2821(7) 0.0623(4) 0.4346(3) 0.0815(14) Uani 1 1 d . . . H9A H -0.2018 0.0754 0.4808 0.098 Uiso 1 1 calc R . . H9B H -0.3031 -0.0166 0.4086 0.098 Uiso 1 1 calc R . . H9C H -0.4021 0.0777 0.4479 0.098 Uiso 1 1 calc R . . C9B C 0.3231(7) -0.1345(4) 0.2947(3) 0.0774(13) Uani 1 1 d . . . H9D H 0.2635 -0.1280 0.3430 0.093 Uiso 1 1 calc R . . H9E H 0.4497 -0.1422 0.3031 0.093 Uiso 1 1 calc R . . H9F H 0.2501 -0.2013 0.2594 0.093 Uiso 1 1 calc R . . C10 C 0.1578(5) 0.2140(3) 0.2473(2) 0.0500(10) Uani 1 1 d . . . C19 C 0.2091(5) 0.3099(3) 0.2027(2) 0.0488(9) Uani 1 1 d . . . C20 C 0.3141(6) 0.4182(3) 0.2397(2) 0.0582(10) Uani 1 1 d . . . H20 H 0.3524 0.4296 0.2917 0.067 Uiso 1 1 calc R . . C21 C 0.3629(6) 0.5092(3) 0.2015(2) 0.0616(11) Uani 1 1 d . . . H21 H 0.4328 0.5812 0.2280 0.071 Uiso 1 1 calc R . . C22 C 0.3090(5) 0.4951(3) 0.1233(2) 0.0530(10) Uani 1 1 d . . . C23 C 0.3566(6) 0.5874(4) 0.0811(3) 0.0672(12) Uani 1 1 d . . . H23 H 0.4226 0.6607 0.1070 0.077 Uiso 1 1 calc R . . C24 C 0.3099(6) 0.5723(4) 0.0065(3) 0.0716(13) Uani 1 1 d . . . H24 H 0.3432 0.6351 -0.0185 0.082 Uiso 1 1 calc R . . C25 C 0.2086(6) 0.4610(4) -0.0370(2) 0.0620(11) Uani 1 1 d . . . C26 C 0.1663(7) 0.4395(5) -0.1162(3) 0.0788(14) Uani 1 1 d . . . H26 H 0.1999 0.5000 -0.1431 0.091 Uiso 1 1 calc R . . C27 C 0.0773(7) 0.3321(6) -0.1552(3) 0.0881(16) Uani 1 1 d . . . H27 H 0.0550 0.3198 -0.2085 0.101 Uiso 1 1 calc R . . C28 C 0.0187(6) 0.2401(5) -0.1171(2) 0.0742(13) Uani 1 1 d . . . H28 H -0.0440 0.1673 -0.1448 0.085 Uiso 1 1 calc R . . C29 C 0.0538(5) 0.2564(4) -0.0370(2) 0.0552(10) Uani 1 1 d . . . C30 C -0.0018(5) 0.1652(3) 0.0051(2) 0.0549(10) Uani 1 1 d . . . H30 H -0.0708 0.0926 -0.0208 0.063 Uiso 1 1 calc R . . C31 C 0.0430(5) 0.1813(3) 0.0815(2) 0.0511(9) Uani 1 1 d . . . H31 H 0.0031 0.1198 0.1073 0.059 Uiso 1 1 calc R . . C32 C 0.1531(5) 0.3672(3) 0.0032(2) 0.0500(9) Uani 1 1 d . . . C33 C 0.2039(5) 0.3850(3) 0.0839(2) 0.0462(9) Uani 1 1 d . . . C34 C 0.1510(5) 0.2913(3) 0.1240(2) 0.0442(9) Uani 1 1 d . . . C1' C 0.1562(10) 0.2414(6) 0.5441(4) 0.134(2) Uani 1 1 d . . . H1'1 H 0.0280 0.2139 0.5583 0.200 Uiso 1 1 calc R . . H1'2 H 0.2060 0.1767 0.5243 0.200 Uiso 1 1 calc R . . H1'3 H 0.1568 0.2873 0.5051 0.200 Uiso 1 1 calc R . . N1' N 0.2713(13) 0.3098(8) 0.6100(5) 0.166(3) Uiso 1 1 d D . . O1A O 0.202(2) 0.3630(8) 0.6484(5) 0.427(12) Uani 1 1 d D . . O1B O 0.4210(12) 0.2771(8) 0.6090(6) 0.291(5) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B 0.086(4) 0.050(3) 0.045(3) 0.016(2) 0.000(2) 0.017(3) F1 0.101(2) 0.0560(15) 0.0881(19) 0.0215(13) 0.0164(15) 0.0090(14) F2 0.127(2) 0.0954(19) 0.0465(14) 0.0284(13) 0.0048(13) 0.0520(17) N1A 0.067(2) 0.057(2) 0.0430(18) 0.0163(15) 0.0066(16) 0.0170(16) N1B 0.074(2) 0.0481(18) 0.0442(18) 0.0142(15) 0.0017(16) 0.0204(17) C2A 0.072(3) 0.061(2) 0.052(2) 0.017(2) 0.007(2) 0.025(2) C2B 0.059(2) 0.051(2) 0.052(2) 0.0119(18) -0.0008(19) 0.0150(19) C3A 0.067(3) 0.075(3) 0.062(3) 0.017(2) 0.007(2) 0.028(2) C3B 0.061(3) 0.059(3) 0.058(2) 0.010(2) -0.008(2) 0.019(2) C4A 0.066(3) 0.069(3) 0.048(2) 0.017(2) 0.005(2) 0.014(2) C4B 0.070(3) 0.051(2) 0.050(2) 0.0086(19) -0.008(2) 0.021(2) C5A 0.068(3) 0.053(2) 0.041(2) 0.0143(18) 0.0028(19) 0.018(2) C5B 0.066(3) 0.046(2) 0.043(2) 0.0143(17) 0.0010(19) 0.0168(19) C6A 0.092(3) 0.073(3) 0.083(3) 0.028(3) 0.016(3) 0.042(3) C6B 0.065(3) 0.067(3) 0.081(3) 0.024(2) 0.014(2) 0.018(2) C7A 0.087(4) 0.107(4) 0.090(4) 0.036(3) 0.028(3) 0.043(3) C8A 0.132(6) 0.139(6) 0.137(6) -0.011(5) 0.044(5) 0.064(5) C7B 0.067(3) 0.075(3) 0.089(3) 0.023(3) 0.004(2) 0.033(2) C8B 0.089(3) 0.076(3) 0.090(4) 0.015(3) 0.021(3) 0.042(3) C9A 0.086(3) 0.093(3) 0.071(3) 0.034(3) 0.020(3) 0.019(3) C9B 0.101(4) 0.064(3) 0.078(3) 0.024(2) -0.006(3) 0.033(3) C10 0.067(3) 0.044(2) 0.039(2) 0.0099(17) -0.0023(18) 0.0115(19) C19 0.060(2) 0.044(2) 0.046(2) 0.0124(17) 0.0053(18) 0.0173(18) C20 0.075(3) 0.049(2) 0.050(2) 0.0084(19) -0.004(2) 0.016(2) C21 0.068(3) 0.041(2) 0.072(3) 0.009(2) -0.004(2) 0.010(2) C22 0.052(2) 0.043(2) 0.066(3) 0.0196(19) 0.0049(19) 0.0113(18) C23 0.068(3) 0.050(2) 0.088(3) 0.028(2) 0.007(2) 0.012(2) C24 0.067(3) 0.068(3) 0.092(4) 0.048(3) 0.015(2) 0.017(2) C25 0.052(2) 0.082(3) 0.067(3) 0.042(2) 0.014(2) 0.026(2) C26 0.066(3) 0.113(4) 0.072(3) 0.055(3) 0.009(2) 0.025(3) C27 0.081(3) 0.139(5) 0.055(3) 0.045(3) 0.002(3) 0.028(3) C28 0.067(3) 0.101(4) 0.056(3) 0.015(3) 0.000(2) 0.025(3) C29 0.047(2) 0.074(3) 0.051(2) 0.017(2) 0.0069(18) 0.023(2) C30 0.054(2) 0.054(2) 0.055(2) 0.0082(19) 0.0008(18) 0.0138(19) C31 0.054(2) 0.046(2) 0.057(2) 0.0169(18) 0.0092(18) 0.0129(18) C32 0.044(2) 0.063(3) 0.054(2) 0.023(2) 0.0105(17) 0.0226(19) C33 0.044(2) 0.049(2) 0.053(2) 0.0186(18) 0.0079(17) 0.0180(17) C34 0.045(2) 0.044(2) 0.048(2) 0.0145(17) 0.0079(16) 0.0153(17) C1' 0.141(6) 0.121(5) 0.116(5) 0.023(4) -0.034(4) -0.006(4) O1A 0.95(4) 0.219(9) 0.208(8) 0.004(7) 0.120(14) 0.347(16) O1B 0.200(8) 0.346(12) 0.310(11) 0.178(10) -0.038(8) -0.038(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B F2 1.391(5) . ? B F1 1.393(5) . ? B N1A 1.538(6) . ? B N1B 1.540(6) . ? N1A C4A 1.353(5) . ? N1A C5A 1.400(4) . ? N1B C4B 1.354(5) . ? N1B C5B 1.397(4) . ? C2A C3A 1.390(6) . ? C2A C5A 1.419(5) . ? C2A C6A 1.502(6) . ? C2B C3B 1.389(5) . ? C2B C5B 1.422(5) . ? C2B C6B 1.500(5) . ? C3A C4A 1.402(6) . ? C3A C7A 1.504(6) . ? C3B C4B 1.408(6) . ? C3B C7B 1.503(6) . ? C4A C9A 1.497(6) . ? C4B C9B 1.492(5) . ? C5A C10 1.399(5) . ? C5B C10 1.394(5) . ? C7A C8A 1.519(8) . ? C7B C8B 1.510(6) . ? C10 C19 1.496(5) . ? C19 C20 1.384(5) . ? C19 C34 1.406(5) . ? C20 C21 1.371(5) . ? C21 C22 1.397(5) . ? C22 C33 1.412(5) . ? C22 C23 1.430(5) . ? C23 C24 1.322(6) . ? C24 C25 1.439(6) . ? C25 C26 1.389(6) . ? C25 C32 1.426(5) . ? C26 C27 1.355(7) . ? C27 C28 1.386(7) . ? C28 C29 1.401(6) . ? C29 C32 1.411(5) . ? C29 C30 1.422(5) . ? C30 C31 1.350(5) . ? C31 C34 1.435(5) . ? C32 C33 1.429(5) . ? C33 C34 1.422(5) . ? C1' N1' 1.420(9) . ? N1' O1A 1.069(9) . ? N1' O1B 1.248(5) . ? 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 F2 B F1 108.7(3) . . ? F2 B N1A 110.0(3) . . ? F1 B N1A 110.4(4) . . ? F2 B N1B 109.7(4) . . ? F1 B N1B 110.6(3) . . ? N1A B N1B 107.4(3) . . ? C4A N1A C5A 107.7(3) . . ? C4A N1A B 126.7(3) . . ? C5A N1A B 125.5(3) . . ? C4B N1B C5B 108.1(3) . . ? C4B N1B B 126.6(3) . . ? C5B N1B B 125.3(3) . . ? C3A C2A C5A 106.8(3) . . ? C3A C2A C6A 124.5(4) . . ? C5A C2A C6A 128.7(4) . . ? C3B C2B C5B 107.1(3) . . ? C3B C2B C6B 124.3(4) . . ? C5B C2B C6B 128.6(3) . . ? C2A C3A C4A 107.5(4) . . ? C2A C3A C7A 126.7(4) . . ? C4A C3A C7A 125.7(4) . . ? C2B C3B C4B 107.4(4) . . ? C2B C3B C7B 126.8(4) . . ? C4B C3B C7B 125.8(4) . . ? N1A C4A C3A 109.9(3) . . ? N1A C4A C9A 123.1(4) . . ? C3A C4A C9A 127.0(4) . . ? N1B C4B C3B 109.6(3) . . ? N1B C4B C9B 122.7(4) . . ? C3B C4B C9B 127.6(4) . . ? C10 C5A N1A 119.9(3) . . ? C10 C5A C2A 132.0(3) . . ? N1A C5A C2A 108.1(3) . . ? C10 C5B N1B 120.4(3) . . ? C10 C5B C2B 131.8(3) . . ? N1B C5B C2B 107.8(3) . . ? C3A C7A C8A 112.4(4) . . ? C3B C7B C8B 113.1(3) . . ? C5B C10 C5A 121.5(3) . . ? C5B C10 C19 119.7(3) . . ? C5A C10 C19 118.8(3) . . ? C20 C19 C34 119.9(3) . . ? C20 C19 C10 119.4(3) . . ? C34 C19 C10 120.8(3) . . ? C21 C20 C19 121.5(4) . . ? C20 C21 C22 120.8(4) . . ? C21 C22 C33 118.7(3) . . ? C21 C22 C23 122.8(4) . . ? C33 C22 C23 118.5(4) . . ? C24 C23 C22 122.3(4) . . ? C23 C24 C25 121.5(4) . . ? C26 C25 C32 118.3(4) . . ? C26 C25 C24 123.5(4) . . ? C32 C25 C24 118.1(4) . . ? C27 C26 C25 121.4(4) . . ? C26 C27 C28 121.2(4) . . ? C27 C28 C29 120.2(5) . . ? C28 C29 C32 118.6(4) . . ? C28 C29 C30 122.7(4) . . ? C32 C29 C30 118.7(3) . . ? C31 C30 C29 121.7(4) . . ? C30 C31 C34 121.4(3) . . ? C29 C32 C25 120.1(4) . . ? C29 C32 C33 120.1(3) . . ? C25 C32 C33 119.7(4) . . ? C22 C33 C34 120.3(3) . . ? C22 C33 C32 119.9(3) . . ? C34 C33 C32 119.8(3) . . ? C19 C34 C33 118.7(3) . . ? C19 C34 C31 123.1(3) . . ? C33 C34 C31 118.2(3) . . ? O1A N1' O1B 138.7(13) . . ? O1A N1' C1' 114.9(11) . . ? O1B N1' C1' 105.7(9) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 23.24 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.705 _refine_diff_density_min -0.475 _refine_diff_density_rms 0.050