data_Global _audit_creation_method SHELXL-97 #------------------------------------------------------------------------------ _publ_contact_author ; Masood Parvez Department of Chemistry University of Calgary 2500 University Drive N.W. Calgary, Alberta, Canada T2N 1N4 ; #----------------------------------------------------------------------------- _publ_requested_journal ' ? ' _publ_requested_coeditor_name ' ? ' _publ_contact_author_phone ' (403)220-5348 ' _publ_contact_author_fax ' (403)289-9488 ' _publ_contact_author_email ' parvez@ucalgary.ca ' #------------------------------------------------------------------------------ _publ_section_title ; ? ; loop_ _publ_author_name _publ_author_address 'Parvez, Masood' ; Department of Chemistry The University of Calgary 2500 University Drive NW Calgary Alberta Canada T2N 1N4 ; #------------------------------------------------------------------------------ data_Compound_I #----------------------------------------------------------------------------- _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'HKL DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SAPI91 (Fan, 1991)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' #----------------------------------------------------------------------------- _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H25 B F10 N2' _chemical_formula_weight 614.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 '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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.170(3) _cell_length_b 11.360(3) _cell_length_c 12.443(4) _cell_angle_alpha 96.362(19) _cell_angle_beta 99.83(2) _cell_angle_gamma 105.61(2) _cell_volume 1345.4(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8393 _cell_measurement_theta_min 3.23 _cell_measurement_theta_max 25.30 _exptl_crystal_description 'prism' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.516 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 628 _exptl_absorpt_coefficient_mu 0.137 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.9627 _exptl_absorpt_correction_T_max 0.9784 _exptl_absorpt_process_details 'SORTAV: (Blessing, 1997)' _diffrn_ambient_temperature 173(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 KappaCCD' _diffrn_measurement_method ' \w and \f ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8393 _diffrn_reflns_av_R_equivalents 0.0237 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 25.30 _reflns_number_total 4808 _reflns_number_gt 4093 _reflns_threshold_expression >2sigma(I) _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^)+(0.0470P)^2^+0.7500P] 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 4808 _refine_ls_number_parameters 395 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0479 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.1052 _refine_ls_wR_factor_gt 0.0984 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 F1 F 0.11654(11) 0.54444(10) 0.39655(10) 0.0377(3) Uani 1 1 d . . . F2 F 0.30432(13) 0.76508(10) 0.43360(11) 0.0463(3) Uani 1 1 d . . . F3 F 0.54186(12) 0.79842(10) 0.35201(10) 0.0420(3) Uani 1 1 d . . . F4 F 0.58783(12) 0.60093(11) 0.23733(10) 0.0461(3) Uani 1 1 d . . . F5 F 0.41058(12) 0.37937(10) 0.20500(10) 0.0444(3) Uani 1 1 d . . . F6 F 0.23390(11) 0.41083(9) 0.52641(8) 0.0341(3) Uani 1 1 d . . . F7 F 0.12033(12) 0.31221(11) 0.68431(8) 0.0406(3) Uani 1 1 d . . . F8 F -0.09491(12) 0.10049(11) 0.63598(9) 0.0419(3) Uani 1 1 d . . . F9 F -0.20006(12) -0.01024(10) 0.42095(9) 0.0425(3) Uani 1 1 d . . . F10 F -0.09525(11) 0.08943(10) 0.25968(8) 0.0347(3) Uani 1 1 d . . . N1 N 0.18760(14) 0.20675(12) 0.22478(11) 0.0224(3) Uani 1 1 d . . . N2 N 0.00614(14) 0.31446(13) 0.18152(11) 0.0226(3) Uani 1 1 d . . . C1 C 0.27492(18) 0.15117(15) 0.27828(14) 0.0248(4) Uani 1 1 d . . . C2 C 0.30926(18) 0.06977(15) 0.20175(14) 0.0269(4) Uani 1 1 d . . . C3 C 0.24655(18) 0.08099(16) 0.09687(14) 0.0279(4) Uani 1 1 d . . . C4 C 0.17147(18) 0.16883(15) 0.11105(13) 0.0247(4) Uani 1 1 d . . . C5 C 0.09682(18) 0.22176(16) 0.03517(14) 0.0266(4) Uani 1 1 d . . . C6 C 0.01569(18) 0.29463(15) 0.06951(13) 0.0250(4) Uani 1 1 d . . . C7 C -0.08869(18) 0.33635(16) 0.00687(14) 0.0279(4) Uani 1 1 d . . . C8 C -0.16240(19) 0.37605(16) 0.08023(15) 0.0288(4) Uani 1 1 d . . . C9 C -0.10333(18) 0.36034(15) 0.18708(14) 0.0255(4) Uani 1 1 d . . . C10 C 0.3356(2) 0.18198(18) 0.39925(14) 0.0324(4) Uani 1 1 d . . . H10A H 0.4157 0.1497 0.4156 0.039 Uiso 1 1 calc R . . H10B H 0.2648 0.1443 0.4397 0.039 Uiso 1 1 calc R . . H10C H 0.3661 0.2721 0.4221 0.039 Uiso 1 1 calc R . . C11 C 0.4024(2) -0.00936(17) 0.23128(17) 0.0342(4) Uani 1 1 d . . . H11A H 0.3951 -0.0307 0.3030 0.041 Uiso 1 1 d R . . H11B H 0.3748 -0.0837 0.1775 0.041 Uiso 1 1 d R . . C12 C 0.5553(2) 0.0555(2) 0.2355(2) 0.0488(6) Uani 1 1 d . . . H12A H 0.6104 -0.0018 0.2505 0.059 Uiso 1 1 calc R . . H12B H 0.5885 0.1280 0.2943 0.059 Uiso 1 1 calc R . . H12C H 0.5655 0.0821 0.1643 0.059 Uiso 1 1 calc R . . C13 C 0.2558(2) 0.00791(19) -0.00845(16) 0.0405(5) Uani 1 1 d . . . H13A H 0.1625 -0.0261 -0.0560 0.049 Uiso 1 1 calc R . . H13B H 0.2938 -0.0600 0.0089 0.049 Uiso 1 1 calc R . . H13C H 0.3173 0.0622 -0.0469 0.049 Uiso 1 1 calc R . . C14 C 0.1021(2) 0.1979(2) -0.08500(15) 0.0427(5) Uani 1 1 d . . . H14A H 0.0938 0.2702 -0.1188 0.051 Uiso 1 1 calc R . . H14B H 0.0248 0.1251 -0.1227 0.051 Uiso 1 1 calc R . . H14C H 0.1910 0.1829 -0.0918 0.051 Uiso 1 1 calc R . . C15 C -0.1220(2) 0.33612(19) -0.11558(15) 0.0368(4) Uani 1 1 d . . . H15A H -0.2000 0.3707 -0.1336 0.044 Uiso 1 1 calc R . . H15B H -0.1479 0.2509 -0.1550 0.044 Uiso 1 1 calc R . . H15C H -0.0399 0.3866 -0.1380 0.044 Uiso 1 1 calc R . . C16 C -0.2864(2) 0.42364(19) 0.05202(17) 0.0374(4) Uani 1 1 d . . . H16A H -0.2952 0.4727 0.1169 0.045 Uiso 1 1 d R . . H16B H -0.2732 0.4738 -0.0047 0.045 Uiso 1 1 d R . . C17 C -0.4242(2) 0.3216(2) 0.00983(19) 0.0460(5) Uani 1 1 d . . . H17A H -0.5001 0.3589 -0.0071 0.055 Uiso 1 1 calc R . . H17B H -0.4421 0.2697 0.0667 0.055 Uiso 1 1 calc R . . H17C H -0.4189 0.2706 -0.0573 0.055 Uiso 1 1 calc R . . C18 C -0.16125(19) 0.38193(17) 0.28754(15) 0.0316(4) Uani 1 1 d . . . H18A H -0.1937 0.4556 0.2863 0.038 Uiso 1 1 calc R . . H18B H -0.0884 0.3946 0.3540 0.038 Uiso 1 1 calc R . . H18C H -0.2397 0.3098 0.2883 0.038 Uiso 1 1 calc R . . C19 C 0.25064(17) 0.44580(15) 0.30015(13) 0.0232(3) Uani 1 1 d . . . C20 C 0.23393(18) 0.55195(16) 0.35675(14) 0.0265(4) Uani 1 1 d . . . C21 C 0.32891(19) 0.66831(16) 0.37635(15) 0.0305(4) Uani 1 1 d . . . C22 C 0.44877(19) 0.68565(16) 0.33604(15) 0.0301(4) Uani 1 1 d . . . C23 C 0.47131(18) 0.58568(17) 0.27818(15) 0.0306(4) Uani 1 1 d . . . C24 C 0.37456(19) 0.46975(16) 0.26197(14) 0.0280(4) Uani 1 1 d . . . C25 C 0.06960(17) 0.26026(15) 0.38217(13) 0.0231(3) Uani 1 1 d . . . C26 C 0.12052(18) 0.31002(15) 0.49366(14) 0.0255(4) Uani 1 1 d . . . C27 C 0.06590(19) 0.25926(17) 0.57839(13) 0.0276(4) Uani 1 1 d . . . C28 C -0.04260(19) 0.15185(17) 0.55428(14) 0.0289(4) Uani 1 1 d . . . C29 C -0.09548(18) 0.09621(16) 0.44569(15) 0.0283(4) Uani 1 1 d . . . C30 C -0.03889(18) 0.15034(16) 0.36388(13) 0.0252(4) Uani 1 1 d . . . B1 B 0.1289(2) 0.30867(17) 0.27495(15) 0.0225(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 F1 0.0343(6) 0.0351(6) 0.0458(7) 0.0002(5) 0.0166(5) 0.0111(5) F2 0.0486(7) 0.0280(6) 0.0589(8) -0.0057(5) 0.0116(6) 0.0107(5) F3 0.0384(6) 0.0302(6) 0.0465(7) 0.0081(5) 0.0001(5) -0.0035(5) F4 0.0319(6) 0.0505(7) 0.0527(7) 0.0066(6) 0.0191(5) 0.0008(5) F5 0.0405(6) 0.0367(6) 0.0552(7) -0.0055(5) 0.0278(6) 0.0040(5) F6 0.0372(6) 0.0350(6) 0.0199(5) 0.0010(4) 0.0027(4) -0.0028(5) F7 0.0512(7) 0.0489(7) 0.0153(5) 0.0029(4) 0.0069(5) 0.0049(5) F8 0.0454(7) 0.0535(7) 0.0280(6) 0.0188(5) 0.0155(5) 0.0070(5) F9 0.0382(6) 0.0411(6) 0.0368(6) 0.0134(5) 0.0036(5) -0.0074(5) F10 0.0393(6) 0.0342(6) 0.0200(5) 0.0002(4) 0.0009(4) -0.0020(5) N1 0.0264(7) 0.0256(7) 0.0152(7) 0.0035(5) 0.0043(5) 0.0074(6) N2 0.0245(7) 0.0266(7) 0.0169(7) 0.0043(5) 0.0046(6) 0.0073(6) C1 0.0254(9) 0.0266(8) 0.0223(8) 0.0072(7) 0.0055(7) 0.0062(7) C2 0.0273(9) 0.0240(8) 0.0291(9) 0.0038(7) 0.0075(7) 0.0061(7) C3 0.0280(9) 0.0276(9) 0.0258(9) -0.0007(7) 0.0062(7) 0.0058(7) C4 0.0273(9) 0.0278(8) 0.0177(8) 0.0018(6) 0.0055(7) 0.0059(7) C5 0.0267(9) 0.0323(9) 0.0182(8) 0.0036(7) 0.0042(7) 0.0052(7) C6 0.0261(9) 0.0289(9) 0.0181(8) 0.0057(7) 0.0040(7) 0.0048(7) C7 0.0288(9) 0.0287(9) 0.0237(9) 0.0085(7) 0.0016(7) 0.0054(7) C8 0.0297(9) 0.0269(9) 0.0289(9) 0.0065(7) 0.0034(7) 0.0079(7) C9 0.0255(9) 0.0238(8) 0.0264(9) 0.0039(7) 0.0057(7) 0.0060(7) C10 0.0366(10) 0.0437(11) 0.0218(9) 0.0102(8) 0.0054(8) 0.0187(9) C11 0.0373(10) 0.0299(9) 0.0380(10) 0.0063(8) 0.0086(8) 0.0138(8) C12 0.0386(12) 0.0571(14) 0.0628(15) 0.0255(11) 0.0197(11) 0.0223(10) C13 0.0483(12) 0.0415(11) 0.0306(10) -0.0066(8) 0.0082(9) 0.0166(10) C14 0.0499(12) 0.0667(14) 0.0191(9) 0.0066(9) 0.0084(8) 0.0293(11) C15 0.0406(11) 0.0454(11) 0.0245(9) 0.0132(8) 0.0020(8) 0.0130(9) C16 0.0415(11) 0.0415(11) 0.0341(10) 0.0103(8) 0.0042(9) 0.0210(9) C17 0.0346(11) 0.0597(14) 0.0462(12) 0.0086(10) 0.0037(9) 0.0209(10) C18 0.0290(9) 0.0340(9) 0.0319(10) 0.0025(8) 0.0070(8) 0.0103(8) C19 0.0250(8) 0.0271(8) 0.0166(8) 0.0056(6) 0.0036(6) 0.0060(7) C20 0.0261(9) 0.0309(9) 0.0235(8) 0.0063(7) 0.0053(7) 0.0092(7) C21 0.0360(10) 0.0260(9) 0.0273(9) 0.0019(7) 0.0006(8) 0.0104(8) C22 0.0284(9) 0.0266(9) 0.0276(9) 0.0082(7) -0.0027(7) -0.0007(7) C23 0.0249(9) 0.0385(10) 0.0274(9) 0.0094(8) 0.0077(7) 0.0049(8) C24 0.0305(9) 0.0293(9) 0.0241(9) 0.0026(7) 0.0074(7) 0.0080(7) C25 0.0241(8) 0.0268(8) 0.0192(8) 0.0039(6) 0.0050(7) 0.0085(7) C26 0.0265(9) 0.0261(8) 0.0219(8) 0.0032(7) 0.0043(7) 0.0052(7) C27 0.0331(9) 0.0356(9) 0.0153(8) 0.0039(7) 0.0049(7) 0.0122(8) C28 0.0316(9) 0.0368(10) 0.0239(9) 0.0137(7) 0.0123(7) 0.0119(8) C29 0.0242(9) 0.0295(9) 0.0293(9) 0.0096(7) 0.0047(7) 0.0034(7) C30 0.0279(9) 0.0293(9) 0.0169(8) 0.0025(7) 0.0025(7) 0.0078(7) B1 0.0232(9) 0.0267(9) 0.0169(9) 0.0035(7) 0.0034(7) 0.0066(8) 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 F1 C20 1.354(2) . ? F2 C21 1.347(2) . ? F3 C22 1.343(2) . ? F4 C23 1.344(2) . ? F5 C24 1.349(2) . ? F6 C26 1.354(2) . ? F7 C27 1.342(2) . ? F8 C28 1.344(2) . ? F9 C29 1.342(2) . ? F10 C30 1.350(2) . ? N1 C1 1.350(2) . ? N1 C4 1.401(2) . ? N1 B1 1.557(2) . ? N2 C9 1.359(2) . ? N2 C6 1.411(2) . ? N2 B1 1.575(2) . ? C1 C2 1.406(2) . ? C1 C10 1.490(2) . ? C2 C3 1.387(3) . ? C2 C11 1.501(3) . ? C3 C4 1.424(3) . ? C3 C13 1.503(3) . ? C4 C5 1.399(3) . ? C5 C6 1.399(3) . ? C5 C14 1.502(2) . ? C6 C7 1.424(2) . ? C7 C8 1.387(3) . ? C7 C15 1.503(2) . ? C8 C9 1.413(2) . ? C8 C16 1.504(3) . ? C9 C18 1.494(2) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.520(3) . ? C11 H11A 0.9599 . ? C11 H11B 0.9600 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.524(3) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C24 1.392(2) . ? C19 C20 1.394(2) . ? C19 B1 1.667(2) . ? C20 C21 1.379(3) . ? C21 C22 1.370(3) . ? C22 C23 1.370(3) . ? C23 C24 1.385(3) . ? C25 C26 1.391(2) . ? C25 C30 1.392(2) . ? C25 B1 1.645(2) . ? C26 C27 1.384(2) . ? C27 C28 1.370(3) . ? C28 C29 1.376(3) . ? C29 C30 1.376(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 C1 N1 C4 107.68(14) . . ? C1 N1 B1 127.91(14) . . ? C4 N1 B1 123.93(14) . . ? C9 N2 C6 107.82(14) . . ? C9 N2 B1 130.83(14) . . ? C6 N2 B1 119.96(14) . . ? N1 C1 C2 109.92(15) . . ? N1 C1 C10 124.21(15) . . ? C2 C1 C10 125.62(16) . . ? C3 C2 C1 107.47(16) . . ? C3 C2 C11 127.58(16) . . ? C1 C2 C11 124.90(16) . . ? C2 C3 C4 106.85(15) . . ? C2 C3 C13 124.33(17) . . ? C4 C3 C13 128.78(17) . . ? C5 C4 N1 119.99(15) . . ? C5 C4 C3 132.02(16) . . ? N1 C4 C3 107.91(15) . . ? C4 C5 C6 120.86(15) . . ? C4 C5 C14 119.36(16) . . ? C6 C5 C14 119.77(16) . . ? C5 C6 N2 120.38(15) . . ? C5 C6 C7 130.46(16) . . ? N2 C6 C7 107.78(15) . . ? C8 C7 C6 107.05(15) . . ? C8 C7 C15 123.92(17) . . ? C6 C7 C15 129.00(17) . . ? C7 C8 C9 107.89(16) . . ? C7 C8 C16 126.65(17) . . ? C9 C8 C16 125.44(17) . . ? N2 C9 C8 109.38(15) . . ? N2 C9 C18 126.13(16) . . ? C8 C9 C18 124.32(16) . . ? C1 C10 H10A 109.5 . . ? C1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C2 C11 C12 112.88(16) . . ? C2 C11 H11A 109.4 . . ? C12 C11 H11A 107.5 . . ? C2 C11 H11B 109.8 . . ? C12 C11 H11B 107.8 . . ? H11A C11 H11B 109.5 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C3 C13 H13A 109.5 . . ? C3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C5 C14 H14A 109.5 . . ? C5 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C5 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C7 C15 H15A 109.5 . . ? C7 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C7 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C8 C16 C17 113.78(16) . . ? C8 C16 H16A 109.2 . . ? C17 C16 H16A 107.5 . . ? C8 C16 H16B 109.5 . . ? C17 C16 H16B 107.3 . . ? H16A C16 H16B 109.5 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C9 C18 H18A 109.5 . . ? C9 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C9 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C24 C19 C20 112.44(15) . . ? C24 C19 B1 124.73(15) . . ? C20 C19 B1 122.71(15) . . ? F1 C20 C21 115.39(15) . . ? F1 C20 C19 119.54(15) . . ? C21 C20 C19 125.07(16) . . ? F2 C21 C22 119.80(16) . . ? F2 C21 C20 120.68(17) . . ? C22 C21 C20 119.52(17) . . ? F3 C22 C23 120.54(17) . . ? F3 C22 C21 120.82(17) . . ? C23 C22 C21 118.63(16) . . ? F4 C23 C22 119.54(16) . . ? F4 C23 C24 120.34(17) . . ? C22 C23 C24 120.13(16) . . ? F5 C24 C23 113.99(15) . . ? F5 C24 C19 121.82(15) . . ? C23 C24 C19 124.20(16) . . ? C26 C25 C30 113.21(15) . . ? C26 C25 B1 128.41(15) . . ? C30 C25 B1 118.19(14) . . ? F6 C26 C27 115.21(15) . . ? F6 C26 C25 120.78(15) . . ? C27 C26 C25 123.94(16) . . ? F7 C27 C28 119.48(15) . . ? F7 C27 C26 120.77(16) . . ? C28 C27 C26 119.73(16) . . ? F8 C28 C27 120.28(16) . . ? F8 C28 C29 120.52(16) . . ? C27 C28 C29 119.19(15) . . ? F9 C29 C28 119.87(15) . . ? F9 C29 C30 120.91(16) . . ? C28 C29 C30 119.21(16) . . ? F10 C30 C29 115.67(15) . . ? F10 C30 C25 119.66(14) . . ? C29 C30 C25 124.67(15) . . ? N1 B1 N2 105.47(13) . . ? N1 B1 C25 106.40(13) . . ? N2 B1 C25 110.88(13) . . ? N1 B1 C19 109.76(14) . . ? N2 B1 C19 107.63(13) . . ? C25 B1 C19 116.19(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 C4 N1 C1 C2 -4.18(18) . . . . ? B1 N1 C1 C2 -176.39(15) . . . . ? C4 N1 C1 C10 170.35(16) . . . . ? B1 N1 C1 C10 -1.9(3) . . . . ? N1 C1 C2 C3 3.30(19) . . . . ? C10 C1 C2 C3 -171.14(16) . . . . ? N1 C1 C2 C11 -179.09(16) . . . . ? C10 C1 C2 C11 6.5(3) . . . . ? C1 C2 C3 C4 -1.05(19) . . . . ? C11 C2 C3 C4 -178.57(16) . . . . ? C1 C2 C3 C13 -179.01(17) . . . . ? C11 C2 C3 C13 3.5(3) . . . . ? C1 N1 C4 C5 -173.78(15) . . . . ? B1 N1 C4 C5 -1.2(2) . . . . ? C1 N1 C4 C3 3.47(18) . . . . ? B1 N1 C4 C3 176.06(14) . . . . ? C2 C3 C4 C5 175.34(18) . . . . ? C13 C3 C4 C5 -6.8(3) . . . . ? C2 C3 C4 N1 -1.44(19) . . . . ? C13 C3 C4 N1 176.40(18) . . . . ? N1 C4 C5 C6 -12.2(2) . . . . ? C3 C4 C5 C6 171.38(18) . . . . ? N1 C4 C5 C14 168.96(16) . . . . ? C3 C4 C5 C14 -7.5(3) . . . . ? C4 C5 C6 N2 -1.0(2) . . . . ? C14 C5 C6 N2 177.93(16) . . . . ? C4 C5 C6 C7 -165.83(17) . . . . ? C14 C5 C6 C7 13.1(3) . . . . ? C9 N2 C6 C5 -165.07(15) . . . . ? B1 N2 C6 C5 26.9(2) . . . . ? C9 N2 C6 C7 2.90(18) . . . . ? B1 N2 C6 C7 -165.10(14) . . . . ? C5 C6 C7 C8 164.17(18) . . . . ? N2 C6 C7 C8 -2.15(19) . . . . ? C5 C6 C7 C15 -13.8(3) . . . . ? N2 C6 C7 C15 179.84(17) . . . . ? C6 C7 C8 C9 0.63(19) . . . . ? C15 C7 C8 C9 178.77(16) . . . . ? C6 C7 C8 C16 -177.51(17) . . . . ? C15 C7 C8 C16 0.6(3) . . . . ? C6 N2 C9 C8 -2.53(18) . . . . ? B1 N2 C9 C8 163.70(16) . . . . ? C6 N2 C9 C18 172.92(16) . . . . ? B1 N2 C9 C18 -20.9(3) . . . . ? C7 C8 C9 N2 1.2(2) . . . . ? C16 C8 C9 N2 179.36(16) . . . . ? C7 C8 C9 C18 -174.36(16) . . . . ? C16 C8 C9 C18 3.8(3) . . . . ? C3 C2 C11 C12 87.6(2) . . . . ? C1 C2 C11 C12 -89.5(2) . . . . ? C7 C8 C16 C17 81.5(2) . . . . ? C9 C8 C16 C17 -96.3(2) . . . . ? C24 C19 C20 F1 178.26(15) . . . . ? B1 C19 C20 F1 2.1(2) . . . . ? C24 C19 C20 C21 -1.4(2) . . . . ? B1 C19 C20 C21 -177.58(16) . . . . ? F1 C20 C21 F2 1.4(2) . . . . ? C19 C20 C21 F2 -178.91(16) . . . . ? F1 C20 C21 C22 -177.90(15) . . . . ? C19 C20 C21 C22 1.8(3) . . . . ? F2 C21 C22 F3 -0.6(3) . . . . ? C20 C21 C22 F3 178.70(15) . . . . ? F2 C21 C22 C23 179.94(16) . . . . ? C20 C21 C22 C23 -0.8(3) . . . . ? F3 C22 C23 F4 0.1(3) . . . . ? C21 C22 C23 F4 179.56(16) . . . . ? F3 C22 C23 C24 -179.88(16) . . . . ? C21 C22 C23 C24 -0.4(3) . . . . ? F4 C23 C24 F5 0.9(2) . . . . ? C22 C23 C24 F5 -179.15(16) . . . . ? F4 C23 C24 C19 -179.24(16) . . . . ? C22 C23 C24 C19 0.7(3) . . . . ? C20 C19 C24 F5 -179.96(16) . . . . ? B1 C19 C24 F5 -3.9(3) . . . . ? C20 C19 C24 C23 0.2(3) . . . . ? B1 C19 C24 C23 176.21(16) . . . . ? C30 C25 C26 F6 174.24(15) . . . . ? B1 C25 C26 F6 -0.6(3) . . . . ? C30 C25 C26 C27 -2.6(3) . . . . ? B1 C25 C26 C27 -177.45(17) . . . . ? F6 C26 C27 F7 2.9(2) . . . . ? C25 C26 C27 F7 179.97(16) . . . . ? F6 C26 C27 C28 -175.30(16) . . . . ? C25 C26 C27 C28 1.7(3) . . . . ? F7 C27 C28 F8 0.6(3) . . . . ? C26 C27 C28 F8 178.82(16) . . . . ? F7 C27 C28 C29 -178.27(16) . . . . ? C26 C27 C28 C29 0.0(3) . . . . ? F8 C28 C29 F9 0.0(3) . . . . ? C27 C28 C29 F9 178.79(16) . . . . ? F8 C28 C29 C30 -179.37(16) . . . . ? C27 C28 C29 C30 -0.5(3) . . . . ? F9 C29 C30 F10 -0.1(2) . . . . ? C28 C29 C30 F10 179.23(16) . . . . ? F9 C29 C30 C25 -179.90(16) . . . . ? C28 C29 C30 C25 -0.6(3) . . . . ? C26 C25 C30 F10 -177.74(15) . . . . ? B1 C25 C30 F10 -2.3(2) . . . . ? C26 C25 C30 C29 2.1(3) . . . . ? B1 C25 C30 C29 177.46(16) . . . . ? C1 N1 B1 N2 -166.35(14) . . . . ? C4 N1 B1 N2 22.6(2) . . . . ? C1 N1 B1 C25 -48.5(2) . . . . ? C4 N1 B1 C25 140.45(15) . . . . ? C1 N1 B1 C19 78.0(2) . . . . ? C4 N1 B1 C19 -93.07(17) . . . . ? C9 N2 B1 N1 160.34(15) . . . . ? C6 N2 B1 N1 -34.83(19) . . . . ? C9 N2 B1 C25 45.6(2) . . . . ? C6 N2 B1 C25 -149.61(14) . . . . ? C9 N2 B1 C19 -82.5(2) . . . . ? C6 N2 B1 C19 82.30(17) . . . . ? C26 C25 B1 N1 112.76(19) . . . . ? C30 C25 B1 N1 -61.83(19) . . . . ? C26 C25 B1 N2 -133.04(18) . . . . ? C30 C25 B1 N2 52.4(2) . . . . ? C26 C25 B1 C19 -9.7(3) . . . . ? C30 C25 B1 C19 175.66(15) . . . . ? C24 C19 B1 N1 11.9(2) . . . . ? C20 C19 B1 N1 -172.44(15) . . . . ? C24 C19 B1 N2 -102.41(18) . . . . ? C20 C19 B1 N2 73.26(19) . . . . ? C24 C19 B1 C25 132.62(17) . . . . ? C20 C19 B1 C25 -51.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.30 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.287 _refine_diff_density_min -0.280 _refine_diff_density_rms 0.044 _vrf_PUBL012_GLOBAL ; PROBLEM: _publ_section_abstract is missing. RESPONSE: Will appear in the paper ; # end Validation Reply Form