data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Piers, Warren' _publ_contact_author_email WPIERS@UCALGARY.CA _publ_section_title ; A New Weakly Coordinating Aluminate Anion Incorporating a Chelating Perfluoro-bis-anilido Ligand. ; loop_ _publ_author_name W.Piers J.Smith K.Ma M.Parvez R.McDonald # Attachment '- 2.cif' #------------------------------------------------------------------------------ data_Compound_2 _database_code_depnum_ccdc_archive 'CCDC 784055' #TrackingRef '- 2.cif' #----------------------------------------------------------------------------- _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 'C19 H3 Al F14 N2' _chemical_formula_weight 552.21 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' F F 0.0171 0.0103 '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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 9.858(3) _cell_length_b 9.666(3) _cell_length_c 20.142(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.137(3) _cell_angle_gamma 90.00 _cell_volume 1919.3(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7333 _cell_measurement_theta_min 4.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.911 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 0.252 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9608 _exptl_absorpt_correction_T_max 0.9801 _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 7333 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0510 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 4.13 _diffrn_reflns_theta_max 27.51 _reflns_number_total 4378 _reflns_number_gt 2970 _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^)+(0.0610P)^2^+0.5800P] 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 4378 _refine_ls_number_parameters 326 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0793 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1209 _refine_ls_wR_factor_gt 0.1006 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _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 0.10925(6) 1.10120(7) -0.00228(3) 0.02185(17) Uani 1 1 d . . . F1 F 0.11003(14) 0.60606(13) -0.03134(7) 0.0358(3) Uani 1 1 d . . . F2 F 0.28055(15) 0.46974(14) 0.04879(8) 0.0463(4) Uani 1 1 d . . . F3 F 0.43586(15) 0.61316(15) 0.13751(8) 0.0439(4) Uani 1 1 d . . . F4 F 0.42586(13) 0.88601(14) 0.14351(7) 0.0370(4) Uani 1 1 d . . . F5 F 0.44445(14) 1.20504(16) 0.01392(7) 0.0388(4) Uani 1 1 d . . . F6 F 0.59392(14) 1.36918(16) 0.09410(8) 0.0486(4) Uani 1 1 d . . . F7 F 0.54566(15) 1.37476(17) 0.22687(8) 0.0529(5) Uani 1 1 d . . . F8 F 0.34719(16) 1.21282(19) 0.27885(7) 0.0527(4) Uani 1 1 d . . . F9 F 0.19717(14) 1.04765(17) 0.19900(7) 0.0404(4) Uani 1 1 d . . . F10 F 0.30886(12) 0.99916(14) -0.10160(7) 0.0346(3) Uani 1 1 d . . . F11 F 0.34403(14) 0.93962(17) -0.23196(7) 0.0466(4) Uani 1 1 d . . . F12 F 0.17325(16) 0.76164(19) -0.29412(7) 0.0543(5) Uani 1 1 d . . . F13 F -0.04240(15) 0.65181(18) -0.22601(8) 0.0505(4) Uani 1 1 d . . . F14 F -0.08184(12) 0.71986(13) -0.09908(7) 0.0306(3) Uani 1 1 d . . . N1 N 0.23260(17) 1.04105(19) 0.06106(9) 0.0237(4) Uani 1 1 d . . . N2 N 0.08414(17) 0.90223(18) -0.02911(9) 0.0208(4) Uani 1 1 d . . . C1 C 0.1330(2) 1.2439(2) -0.06769(13) 0.0320(5) Uani 1 1 d . . . H1A H 0.0833 1.2192 -0.1082 0.038 Uiso 1 1 calc R . . H1B H 0.2297 1.2536 -0.0779 0.038 Uiso 1 1 calc R . . H1C H 0.0982 1.3317 -0.0503 0.038 Uiso 1 1 calc R . . C2 C 0.2521(2) 0.8974(2) 0.06090(10) 0.0225(5) Uani 1 1 d . . . C3 C 0.1742(2) 0.8224(2) 0.01469(11) 0.0226(5) Uani 1 1 d . . . C4 C 0.1847(2) 0.6798(2) 0.01205(11) 0.0284(5) Uani 1 1 d . . . C5 C 0.2722(2) 0.6084(2) 0.05284(12) 0.0308(5) Uani 1 1 d . . . C6 C 0.3495(2) 0.6809(2) 0.09714(12) 0.0295(5) Uani 1 1 d . . . C7 C 0.3413(2) 0.8224(2) 0.10086(11) 0.0261(5) Uani 1 1 d . . . C8 C 0.3146(2) 1.1238(2) 0.10382(11) 0.0244(5) Uani 1 1 d . . . C9 C 0.4175(2) 1.2062(2) 0.07930(12) 0.0280(5) Uani 1 1 d . . . C10 C 0.4943(2) 1.2908(2) 0.11993(13) 0.0320(6) Uani 1 1 d . . . C11 C 0.4697(2) 1.2947(3) 0.18669(14) 0.0359(6) Uani 1 1 d . . . C12 C 0.3692(2) 1.2118(3) 0.21330(12) 0.0357(6) Uani 1 1 d . . . C13 C 0.2935(2) 1.1293(2) 0.17200(12) 0.0289(5) Uani 1 1 d . . . C14 C 0.1079(2) 0.8680(2) -0.09841(11) 0.0237(5) Uani 1 1 d . . . C15 C 0.2183(2) 0.9184(2) -0.13305(11) 0.0265(5) Uani 1 1 d . . . C16 C 0.2386(2) 0.8855(3) -0.19914(12) 0.0321(6) Uani 1 1 d . . . C17 C 0.1514(3) 0.7960(3) -0.23086(12) 0.0372(6) Uani 1 1 d . . . C18 C 0.0435(2) 0.7408(3) -0.19699(12) 0.0336(6) Uani 1 1 d . . . C19 C 0.0233(2) 0.7774(2) -0.13172(11) 0.0264(5) 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 Al1 0.0238(3) 0.0209(3) 0.0209(3) 0.0008(3) -0.0010(3) 0.0008(3) F1 0.0438(8) 0.0220(7) 0.0415(8) -0.0047(6) -0.0147(6) 0.0012(6) F2 0.0546(9) 0.0218(8) 0.0623(11) 0.0028(7) -0.0187(8) 0.0054(7) F3 0.0486(9) 0.0343(8) 0.0486(9) 0.0074(7) -0.0217(7) 0.0089(7) F4 0.0414(8) 0.0329(8) 0.0365(8) 0.0010(6) -0.0179(6) 0.0025(6) F5 0.0399(8) 0.0442(9) 0.0323(8) 0.0003(7) 0.0074(6) -0.0047(7) F6 0.0342(8) 0.0426(9) 0.0689(11) -0.0037(8) 0.0014(8) -0.0119(7) F7 0.0469(9) 0.0506(10) 0.0612(11) -0.0246(8) -0.0221(8) -0.0010(7) F8 0.0594(10) 0.0738(12) 0.0249(8) -0.0133(8) -0.0070(7) 0.0009(9) F9 0.0386(8) 0.0535(10) 0.0292(8) 0.0050(7) 0.0028(6) -0.0068(7) F10 0.0291(7) 0.0342(8) 0.0404(8) -0.0018(6) 0.0034(6) -0.0031(6) F11 0.0438(8) 0.0568(10) 0.0393(9) 0.0101(8) 0.0183(7) 0.0085(8) F12 0.0569(10) 0.0843(13) 0.0216(8) -0.0122(8) 0.0034(7) 0.0148(9) F13 0.0454(8) 0.0670(11) 0.0390(9) -0.0281(8) -0.0088(7) 0.0011(8) F14 0.0265(6) 0.0309(7) 0.0345(8) -0.0052(6) -0.0002(6) -0.0009(5) N1 0.0269(9) 0.0214(10) 0.0226(10) -0.0011(8) -0.0034(7) 0.0003(8) N2 0.0235(9) 0.0207(9) 0.0183(9) -0.0007(7) -0.0012(7) 0.0029(7) C1 0.0345(13) 0.0313(13) 0.0302(13) 0.0045(10) 0.0038(10) 0.0028(10) C2 0.0231(10) 0.0242(11) 0.0203(11) 0.0029(9) 0.0043(9) -0.0006(8) C3 0.0234(10) 0.0226(12) 0.0218(11) 0.0029(9) 0.0006(9) 0.0029(9) C4 0.0317(12) 0.0258(13) 0.0278(13) -0.0019(10) -0.0025(10) 0.0006(10) C5 0.0366(13) 0.0193(12) 0.0364(14) 0.0040(10) -0.0040(11) 0.0045(10) C6 0.0304(12) 0.0287(13) 0.0293(13) 0.0077(10) -0.0062(10) 0.0054(10) C7 0.0263(11) 0.0285(13) 0.0234(12) 0.0010(10) -0.0041(9) -0.0011(9) C8 0.0244(11) 0.0241(12) 0.0248(12) -0.0017(9) -0.0040(9) 0.0055(9) C9 0.0275(11) 0.0277(12) 0.0289(13) -0.0021(10) 0.0016(10) 0.0050(10) C10 0.0248(11) 0.0256(12) 0.0454(16) -0.0017(11) -0.0012(11) 0.0011(10) C11 0.0282(12) 0.0332(14) 0.0463(16) -0.0155(12) -0.0141(11) 0.0066(10) C12 0.0351(13) 0.0449(16) 0.0272(13) -0.0081(11) -0.0054(11) 0.0117(11) C13 0.0260(11) 0.0322(13) 0.0285(13) -0.0006(10) -0.0013(10) 0.0021(9) C14 0.0261(11) 0.0254(12) 0.0198(11) -0.0011(9) 0.0000(9) 0.0070(9) C15 0.0287(11) 0.0236(12) 0.0272(12) 0.0027(10) 0.0002(9) 0.0040(9) C16 0.0294(12) 0.0412(15) 0.0259(12) 0.0080(11) 0.0089(10) 0.0102(11) C17 0.0419(14) 0.0512(17) 0.0186(12) -0.0036(11) 0.0019(11) 0.0174(12) C18 0.0331(12) 0.0398(15) 0.0280(13) -0.0105(11) -0.0070(11) 0.0066(11) C19 0.0256(11) 0.0297(12) 0.0238(12) -0.0029(10) 0.0002(9) 0.0042(9) 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 1.8539(19) . ? Al1 C1 1.922(2) . ? Al1 N2 2.0104(19) 3_575 ? Al1 N2 2.0128(19) . ? Al1 Al1 2.9115(14) 3_575 ? F1 C4 1.345(3) . ? F2 C5 1.345(3) . ? F3 C6 1.346(3) . ? F4 C7 1.344(3) . ? F5 C9 1.344(3) . ? F6 C10 1.346(3) . ? F7 C11 1.346(3) . ? F8 C12 1.339(3) . ? F9 C13 1.350(3) . ? F10 C15 1.344(3) . ? F11 C16 1.339(3) . ? F12 C17 1.335(3) . ? F13 C18 1.341(3) . ? F14 C19 1.349(3) . ? N1 C2 1.402(3) . ? N1 C8 1.425(3) . ? N2 C14 1.454(3) . ? N2 C3 1.469(3) . ? N2 Al1 2.0104(18) 3_575 ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C7 1.394(3) . ? C2 C3 1.407(3) . ? C3 C4 1.383(3) . ? C4 C5 1.375(3) . ? C5 C6 1.365(3) . ? C6 C7 1.373(3) . ? C8 C9 1.382(3) . ? C8 C13 1.391(3) . ? C9 C10 1.381(3) . ? C10 C11 1.368(4) . ? C11 C12 1.383(4) . ? C12 C13 1.372(3) . ? C14 C19 1.382(3) . ? C14 C15 1.383(3) . ? C15 C16 1.384(3) . ? C16 C17 1.376(4) . ? C17 C18 1.372(4) . ? C18 C19 1.377(3) . ? 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 C1 128.02(10) . . ? N1 Al1 N2 113.53(8) . 3_575 ? C1 Al1 N2 110.16(9) . 3_575 ? N1 Al1 N2 88.00(8) . . ? C1 Al1 N2 121.12(10) . . ? N2 Al1 N2 87.28(7) 3_575 . ? N1 Al1 Al1 104.57(7) . 3_575 ? C1 Al1 Al1 126.53(9) . 3_575 ? N2 Al1 Al1 43.67(5) 3_575 3_575 ? N2 Al1 Al1 43.61(5) . 3_575 ? C2 N1 C8 118.67(18) . . ? C2 N1 Al1 113.51(14) . . ? C8 N1 Al1 127.57(15) . . ? C14 N2 C3 111.00(16) . . ? C14 N2 Al1 116.95(13) . 3_575 ? C3 N2 Al1 112.01(13) . 3_575 ? C14 N2 Al1 117.09(13) . . ? C3 N2 Al1 105.47(13) . . ? Al1 N2 Al1 92.72(7) 3_575 . ? Al1 C1 H1A 109.5 . . ? Al1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Al1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C7 C2 N1 126.9(2) . . ? C7 C2 C3 117.2(2) . . ? N1 C2 C3 115.93(19) . . ? C4 C3 C2 119.9(2) . . ? C4 C3 N2 123.04(19) . . ? C2 C3 N2 117.06(19) . . ? F1 C4 C5 117.6(2) . . ? F1 C4 C3 120.8(2) . . ? C5 C4 C3 121.6(2) . . ? F2 C5 C6 121.1(2) . . ? F2 C5 C4 120.1(2) . . ? C6 C5 C4 118.8(2) . . ? F3 C6 C5 119.8(2) . . ? F3 C6 C7 119.3(2) . . ? C5 C6 C7 120.9(2) . . ? F4 C7 C6 117.0(2) . . ? F4 C7 C2 121.4(2) . . ? C6 C7 C2 121.6(2) . . ? C9 C8 C13 116.3(2) . . ? C9 C8 N1 121.6(2) . . ? C13 C8 N1 122.1(2) . . ? F5 C9 C10 118.4(2) . . ? F5 C9 C8 119.5(2) . . ? C10 C9 C8 122.1(2) . . ? F6 C10 C11 119.7(2) . . ? F6 C10 C9 120.2(2) . . ? C11 C10 C9 120.0(2) . . ? F7 C11 C10 120.5(2) . . ? F7 C11 C12 119.9(2) . . ? C10 C11 C12 119.6(2) . . ? F8 C12 C13 120.9(2) . . ? F8 C12 C11 119.7(2) . . ? C13 C12 C11 119.4(2) . . ? F9 C13 C12 118.5(2) . . ? F9 C13 C8 118.9(2) . . ? C12 C13 C8 122.6(2) . . ? C19 C14 C15 116.9(2) . . ? C19 C14 N2 120.80(19) . . ? C15 C14 N2 122.2(2) . . ? F10 C15 C14 119.3(2) . . ? F10 C15 C16 119.3(2) . . ? C14 C15 C16 121.4(2) . . ? F11 C16 C17 120.1(2) . . ? F11 C16 C15 120.0(2) . . ? C17 C16 C15 120.0(2) . . ? F12 C17 C18 120.3(2) . . ? F12 C17 C16 119.8(2) . . ? C18 C17 C16 119.8(2) . . ? F13 C18 C17 121.5(2) . . ? F13 C18 C19 119.2(2) . . ? C17 C18 C19 119.3(2) . . ? F14 C19 C18 118.2(2) . . ? F14 C19 C14 119.23(19) . . ? C18 C19 C14 122.5(2) . . ? 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 C1 Al1 N1 C2 -128.18(16) . . . . ? N2 Al1 N1 C2 86.98(15) 3_575 . . . ? N2 Al1 N1 C2 0.81(14) . . . . ? Al1 Al1 N1 C2 41.55(15) 3_575 . . . ? C1 Al1 N1 C8 45.9(2) . . . . ? N2 Al1 N1 C8 -98.91(18) 3_575 . . . ? N2 Al1 N1 C8 174.93(18) . . . . ? Al1 Al1 N1 C8 -144.33(16) 3_575 . . . ? N1 Al1 N2 C14 -124.06(15) . . . . ? C1 Al1 N2 C14 10.28(18) . . . . ? N2 Al1 N2 C14 122.27(16) 3_575 . . . ? Al1 Al1 N2 C14 122.27(16) 3_575 . . . ? N1 Al1 N2 C3 -0.05(13) . . . . ? C1 Al1 N2 C3 134.28(14) . . . . ? N2 Al1 N2 C3 -113.73(14) 3_575 . . . ? Al1 Al1 N2 C3 -113.73(14) 3_575 . . . ? N1 Al1 N2 Al1 113.68(8) . . . 3_575 ? C1 Al1 N2 Al1 -111.99(11) . . . 3_575 ? N2 Al1 N2 Al1 0.0 3_575 . . 3_575 ? C8 N1 C2 C7 3.0(3) . . . . ? Al1 N1 C2 C7 177.66(17) . . . . ? C8 N1 C2 C3 -176.14(18) . . . . ? Al1 N1 C2 C3 -1.5(2) . . . . ? C7 C2 C3 C4 2.3(3) . . . . ? N1 C2 C3 C4 -178.55(19) . . . . ? C7 C2 C3 N2 -177.74(18) . . . . ? N1 C2 C3 N2 1.5(3) . . . . ? C14 N2 C3 C4 -53.0(3) . . . . ? Al1 N2 C3 C4 79.8(2) 3_575 . . . ? Al1 N2 C3 C4 179.27(17) . . . . ? C14 N2 C3 C2 127.03(19) . . . . ? Al1 N2 C3 C2 -100.23(18) 3_575 . . . ? Al1 N2 C3 C2 -0.7(2) . . . . ? C2 C3 C4 F1 179.34(18) . . . . ? N2 C3 C4 F1 -0.7(3) . . . . ? C2 C3 C4 C5 -1.4(3) . . . . ? N2 C3 C4 C5 178.6(2) . . . . ? F1 C4 C5 F2 -0.3(3) . . . . ? C3 C4 C5 F2 -179.6(2) . . . . ? F1 C4 C5 C6 179.7(2) . . . . ? C3 C4 C5 C6 0.4(3) . . . . ? F2 C5 C6 F3 0.1(3) . . . . ? C4 C5 C6 F3 -180.0(2) . . . . ? F2 C5 C6 C7 179.6(2) . . . . ? C4 C5 C6 C7 -0.5(3) . . . . ? F3 C6 C7 F4 2.8(3) . . . . ? C5 C6 C7 F4 -176.8(2) . . . . ? F3 C6 C7 C2 -179.0(2) . . . . ? C5 C6 C7 C2 1.4(3) . . . . ? N1 C2 C7 F4 -3.3(3) . . . . ? C3 C2 C7 F4 175.82(18) . . . . ? N1 C2 C7 C6 178.6(2) . . . . ? C3 C2 C7 C6 -2.3(3) . . . . ? C2 N1 C8 C9 106.9(2) . . . . ? Al1 N1 C8 C9 -66.9(3) . . . . ? C2 N1 C8 C13 -74.8(3) . . . . ? Al1 N1 C8 C13 111.3(2) . . . . ? C13 C8 C9 F5 179.34(19) . . . . ? N1 C8 C9 F5 -2.3(3) . . . . ? C13 C8 C9 C10 -0.8(3) . . . . ? N1 C8 C9 C10 177.5(2) . . . . ? F5 C9 C10 F6 -0.3(3) . . . . ? C8 C9 C10 F6 179.8(2) . . . . ? F5 C9 C10 C11 180.0(2) . . . . ? C8 C9 C10 C11 0.1(4) . . . . ? F6 C10 C11 F7 -1.0(3) . . . . ? C9 C10 C11 F7 178.7(2) . . . . ? F6 C10 C11 C12 -178.6(2) . . . . ? C9 C10 C11 C12 1.1(4) . . . . ? F7 C11 C12 F8 0.7(4) . . . . ? C10 C11 C12 F8 178.3(2) . . . . ? F7 C11 C12 C13 -179.2(2) . . . . ? C10 C11 C12 C13 -1.6(4) . . . . ? F8 C12 C13 F9 -0.9(3) . . . . ? C11 C12 C13 F9 179.1(2) . . . . ? F8 C12 C13 C8 -179.1(2) . . . . ? C11 C12 C13 C8 0.9(4) . . . . ? C9 C8 C13 F9 -177.89(19) . . . . ? N1 C8 C13 F9 3.8(3) . . . . ? C9 C8 C13 C12 0.3(3) . . . . ? N1 C8 C13 C12 -178.0(2) . . . . ? C3 N2 C14 C19 100.0(2) . . . . ? Al1 N2 C14 C19 -30.2(3) 3_575 . . . ? Al1 N2 C14 C19 -138.87(18) . . . . ? C3 N2 C14 C15 -77.0(2) . . . . ? Al1 N2 C14 C15 152.82(17) 3_575 . . . ? Al1 N2 C14 C15 44.2(2) . . . . ? C19 C14 C15 F10 -175.44(19) . . . . ? N2 C14 C15 F10 1.6(3) . . . . ? C19 C14 C15 C16 3.5(3) . . . . ? N2 C14 C15 C16 -179.5(2) . . . . ? F10 C15 C16 F11 -3.3(3) . . . . ? C14 C15 C16 F11 177.8(2) . . . . ? F10 C15 C16 C17 175.9(2) . . . . ? C14 C15 C16 C17 -3.0(4) . . . . ? F11 C16 C17 F12 1.0(4) . . . . ? C15 C16 C17 F12 -178.3(2) . . . . ? F11 C16 C17 C18 180.0(2) . . . . ? C15 C16 C17 C18 0.7(4) . . . . ? F12 C17 C18 F13 -0.1(4) . . . . ? C16 C17 C18 F13 -179.1(2) . . . . ? F12 C17 C18 C19 179.8(2) . . . . ? C16 C17 C18 C19 0.8(4) . . . . ? F13 C18 C19 F14 1.1(3) . . . . ? C17 C18 C19 F14 -178.8(2) . . . . ? F13 C18 C19 C14 179.7(2) . . . . ? C17 C18 C19 C14 -0.2(4) . . . . ? C15 C14 C19 F14 176.64(19) . . . . ? N2 C14 C19 F14 -0.5(3) . . . . ? C15 C14 C19 C18 -1.9(3) . . . . ? N2 C14 C19 C18 -179.0(2) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.305 _refine_diff_density_min -0.263 _refine_diff_density_rms 0.061 # Attachment '- 3-Li.cif' #------------------------------------------------------------------------------ data_Compound_3 _database_code_depnum_ccdc_archive 'CCDC 784056' #TrackingRef '- 3-Li.cif' #----------------------------------------------------------------------------- _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)' #----------------------------------------------------------------------------- _vrf_PUBL012_GLOBAL ; PROBLEM: _publ_section_abstract is missing. RESPONSE: Will appear in the paper ; # end Validation Reply Form _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H16 Al F28 Li N4 O2' _chemical_formula_weight 1198.53 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' F F 0.0171 0.0103 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.8290(10) _cell_length_b 27.656(6) _cell_length_c 19.277(4) _cell_angle_alpha 90.00 _cell_angle_beta 109.349(13) _cell_angle_gamma 90.00 _cell_volume 4441.1(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 14647 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 25.01 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.793 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2368 _exptl_absorpt_coefficient_mu 0.210 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9592 _exptl_absorpt_correction_T_max 0.9834 _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 14647 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0508 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 25.01 _reflns_number_total 7802 _reflns_number_gt 5320 _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^)+(0.044P)^2^+2.07P] 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 7802 _refine_ls_number_parameters 724 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0768 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.1045 _refine_ls_wR_factor_gt 0.0887 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.002 _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 0.70780(8) 0.35992(3) 0.28018(4) 0.02556(18) Uani 1 1 d . . . F1 F 0.7666(2) 0.41490(6) 0.13862(9) 0.0534(4) Uani 1 1 d . . . F2 F 0.6043(3) 0.43322(7) -0.00401(10) 0.0811(6) Uani 1 1 d . . . F3 F 0.2903(3) 0.45976(7) -0.04694(10) 0.0931(8) Uani 1 1 d . . . F4 F 0.1407(2) 0.46823(7) 0.05529(12) 0.0849(7) Uani 1 1 d . . . F5 F 0.30089(18) 0.44870(6) 0.19772(10) 0.0529(4) Uani 1 1 d . . . F6 F 0.52936(18) 0.52383(5) 0.23529(9) 0.0442(4) Uani 1 1 d . . . F7 F 0.53418(18) 0.57248(5) 0.35464(9) 0.0470(4) Uani 1 1 d . . . F8 F 0.64122(18) 0.52966(5) 0.49037(9) 0.0484(4) Uani 1 1 d . . . F9 F 0.73747(17) 0.43740(5) 0.50406(8) 0.0399(4) Uani 1 1 d . . . F10 F 1.02214(17) 0.42081(5) 0.47643(8) 0.0410(4) Uani 1 1 d . . . F11 F 1.20208(18) 0.36949(6) 0.59314(9) 0.0543(5) Uani 1 1 d . . . F12 F 1.11539(19) 0.27808(6) 0.61611(9) 0.0542(5) Uani 1 1 d . . . F13 F 0.8385(2) 0.24030(6) 0.52391(10) 0.0640(5) Uani 1 1 d . . . F14 F 0.65454(18) 0.29160(5) 0.40703(9) 0.0484(4) Uani 1 1 d . . . F15 F 1.03628(17) 0.40850(5) 0.28962(8) 0.0410(4) Uani 1 1 d . . . F16 F 1.33220(18) 0.42786(6) 0.38078(9) 0.0489(4) Uani 1 1 d . . . F17 F 1.49566(17) 0.36128(6) 0.48254(9) 0.0553(5) Uani 1 1 d . . . F18 F 1.35736(19) 0.27386(6) 0.48803(9) 0.0570(5) Uani 1 1 d . . . F19 F 1.05928(17) 0.25447(5) 0.39770(8) 0.0421(4) Uani 1 1 d . . . F20 F 1.10615(16) 0.24688(5) 0.26751(8) 0.0390(4) Uani 1 1 d . . . F21 F 0.98607(18) 0.16264(5) 0.20389(9) 0.0433(4) Uani 1 1 d . . . F22 F 0.66161(18) 0.14962(5) 0.14410(8) 0.0402(4) Uani 1 1 d . . . F23 F 0.46005(16) 0.22190(5) 0.14672(8) 0.0386(4) Uani 1 1 d . . . F24 F 0.52425(18) 0.31601(6) 0.06576(8) 0.0444(4) Uani 1 1 d . . . F25 F 0.2307(2) 0.33716(6) -0.03003(8) 0.0546(5) Uani 1 1 d . . . F26 F -0.01959(18) 0.35330(6) 0.01889(10) 0.0580(5) Uani 1 1 d . . . F27 F 0.02527(18) 0.34661(7) 0.16523(10) 0.0610(5) Uani 1 1 d . . . F28 F 0.31986(17) 0.32701(6) 0.26156(8) 0.0456(4) Uani 1 1 d . . . Li1 Li 0.6378(6) 0.10153(18) 0.2234(3) 0.0499(13) Uani 1 1 d . . . O1 O 0.8202(2) 0.06329(7) 0.24134(10) 0.0474(5) Uani 1 1 d . . . O2 O 0.5702(2) 0.13948(7) 0.28662(11) 0.0501(5) Uani 1 1 d . . . N1 N 0.6277(2) 0.42086(7) 0.24657(11) 0.0289(5) Uani 1 1 d . . . N2 N 0.7360(2) 0.38208(7) 0.37443(10) 0.0269(5) Uani 1 1 d . . . N3 N 0.8855(2) 0.32186(7) 0.28772(11) 0.0269(5) Uani 1 1 d . . . N4 N 0.5841(2) 0.31309(7) 0.21867(11) 0.0269(5) Uani 1 1 d . . . C1 C 0.5415(3) 0.43281(8) 0.17309(14) 0.0327(6) Uani 1 1 d . . . C2 C 0.6119(3) 0.42847(10) 0.11901(15) 0.0399(7) Uani 1 1 d . . . C3 C 0.5288(5) 0.43735(11) 0.04604(17) 0.0539(9) Uani 1 1 d . . . C4 C 0.3719(5) 0.45080(11) 0.02451(17) 0.0602(10) Uani 1 1 d . . . C5 C 0.2966(4) 0.45541(11) 0.07619(19) 0.0555(9) Uani 1 1 d . . . C6 C 0.3793(3) 0.44585(10) 0.14867(16) 0.0411(7) Uani 1 1 d . . . C7 C 0.6280(3) 0.45177(8) 0.30421(14) 0.0278(6) Uani 1 1 d . . . C8 C 0.5809(3) 0.49966(9) 0.30051(15) 0.0330(6) Uani 1 1 d . . . C9 C 0.5866(3) 0.52526(9) 0.36251(16) 0.0352(6) Uani 1 1 d . . . C10 C 0.6393(3) 0.50481(9) 0.43003(15) 0.0351(7) Uani 1 1 d . . . C11 C 0.6902(3) 0.45731(9) 0.43609(14) 0.0304(6) Uani 1 1 d . . . C12 C 0.6891(3) 0.43054(8) 0.37541(14) 0.0267(6) Uani 1 1 d . . . C13 C 0.8296(3) 0.35827(9) 0.43883(13) 0.0264(6) Uani 1 1 d . . . C14 C 0.9715(3) 0.37646(9) 0.48802(14) 0.0312(6) Uani 1 1 d . . . C15 C 1.0655(3) 0.35022(10) 0.54742(14) 0.0355(7) Uani 1 1 d . . . C16 C 1.0221(3) 0.30427(10) 0.55942(14) 0.0380(7) Uani 1 1 d . . . C17 C 0.8824(3) 0.28515(10) 0.51239(15) 0.0390(7) Uani 1 1 d . . . C18 C 0.7898(3) 0.31175(9) 0.45343(14) 0.0335(6) Uani 1 1 d . . . C19 C 1.0408(3) 0.32999(9) 0.33745(13) 0.0263(6) Uani 1 1 d . . . C20 C 1.1142(3) 0.37436(9) 0.33826(14) 0.0291(6) Uani 1 1 d . . . C21 C 1.2647(3) 0.38474(9) 0.38576(15) 0.0332(6) Uani 1 1 d . . . C22 C 1.3480(3) 0.35124(10) 0.43600(15) 0.0373(7) Uani 1 1 d . . . C23 C 1.2789(3) 0.30718(10) 0.43827(14) 0.0374(7) Uani 1 1 d . . . C24 C 1.1270(3) 0.29734(9) 0.39105(14) 0.0316(6) Uani 1 1 d . . . C25 C 0.8438(3) 0.27828(8) 0.24894(13) 0.0262(6) Uani 1 1 d . . . C26 C 0.9444(3) 0.24179(9) 0.24105(14) 0.0313(6) Uani 1 1 d . . . C27 C 0.8842(3) 0.19895(9) 0.20612(15) 0.0327(6) Uani 1 1 d . . . C28 C 0.7229(3) 0.19314(9) 0.17481(14) 0.0323(6) Uani 1 1 d . . . C29 C 0.6194(3) 0.22990(9) 0.17706(14) 0.0289(6) Uani 1 1 d . . . C30 C 0.6763(3) 0.27314(9) 0.21218(13) 0.0271(6) Uani 1 1 d . . . C31 C 0.4293(3) 0.32012(8) 0.16657(13) 0.0268(6) Uani 1 1 d . . . C32 C 0.4002(3) 0.32257(9) 0.09113(14) 0.0310(6) Uani 1 1 d . . . C33 C 0.2515(3) 0.33321(9) 0.04204(14) 0.0367(7) Uani 1 1 d . . . C34 C 0.1253(3) 0.34169(10) 0.06702(16) 0.0391(7) Uani 1 1 d . . . C35 C 0.1486(3) 0.33905(10) 0.14058(16) 0.0380(7) Uani 1 1 d . . . C36 C 0.2984(3) 0.32860(9) 0.18901(14) 0.0317(6) Uani 1 1 d . . . C37 C 0.9611(4) 0.05708(14) 0.30519(19) 0.0703(10) Uani 1 1 d . . . H37A H 1.0080 0.0882 0.3211 0.084 Uiso 1 1 d R . . H37B H 0.9309 0.0423 0.3438 0.084 Uiso 1 1 d R . . C38 C 1.0734(5) 0.02578(15) 0.2812(2) 0.0839(12) Uani 1 1 d . . . H38A H 1.1825 0.0355 0.3054 0.101 Uiso 1 1 d R . . H38B H 1.0599 -0.0072 0.2936 0.101 Uiso 1 1 d R . . C39 C 1.0233(4) 0.03232(13) 0.2004(2) 0.0691(10) Uani 1 1 d . . . H39A H 1.0757 0.0605 0.1901 0.083 Uiso 1 1 d R . . H39B H 1.0530 0.0045 0.1781 0.083 Uiso 1 1 d R . . C40 C 0.8471(4) 0.03927(14) 0.18015(19) 0.0682(10) Uani 1 1 d . . . H40A H 0.7927 0.0087 0.1728 0.082 Uiso 1 1 d R . . H40B H 0.8046 0.0587 0.1368 0.082 Uiso 1 1 d R . . C41 C 0.4048(4) 0.14926(13) 0.27698(19) 0.0623(9) Uani 1 1 d . A 1 H41A H 0.3483 0.1203 0.2861 0.075 Uiso 0.50 1 calc PR A 1 H41B H 0.3465 0.1624 0.2276 0.075 Uiso 0.50 1 calc PR A 1 C42 C 0.4306(9) 0.1895(3) 0.3406(4) 0.0581(13) Uani 0.50 1 d P A 1 H42A H 0.4518 0.2216 0.3232 0.070 Uiso 0.50 1 calc PR A 1 H42B H 0.3350 0.1917 0.3564 0.070 Uiso 0.50 1 calc PR A 1 C43 C 0.5586(6) 0.17378(15) 0.3959(2) 0.0897(14) Uani 1 1 d . A 1 H43A H 0.5304 0.1461 0.4219 0.108 Uiso 0.50 1 calc PR A 1 H43B H 0.6056 0.1999 0.4316 0.108 Uiso 0.50 1 calc PR A 1 H41C H 0.3726 0.1804 0.2510 0.075 Uiso 0.50 1 calc PR A 2 H41D H 0.3362 0.1235 0.2468 0.075 Uiso 0.50 1 calc PR A 2 C42' C 0.3830(8) 0.1514(3) 0.3474(4) 0.0581(13) Uani 0.50 1 d P A 2 H42C H 0.3650 0.1190 0.3650 0.070 Uiso 0.50 1 calc PR A 2 H42D H 0.2937 0.1732 0.3470 0.070 Uiso 0.50 1 calc PR A 2 H43C H 0.5534 0.2095 0.3985 0.108 Uiso 0.50 1 calc PR A 2 H43D H 0.5943 0.1606 0.4464 0.108 Uiso 0.50 1 calc PR A 2 C44 C 0.6680(5) 0.15906(17) 0.3569(2) 0.0850(13) Uani 1 1 d . A . H44A H 0.7400 0.1342 0.3832 0.102 Uiso 1 1 d R . . H44B H 0.7290 0.1859 0.3488 0.102 Uiso 1 1 d 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 0.0245(4) 0.0232(4) 0.0262(4) -0.0027(3) 0.0046(3) 0.0001(3) F1 0.0595(11) 0.0579(11) 0.0493(11) -0.0065(8) 0.0268(9) -0.0007(9) F2 0.1373(19) 0.0699(13) 0.0428(12) -0.0020(10) 0.0386(13) -0.0215(13) F3 0.1323(19) 0.0706(14) 0.0379(12) 0.0175(10) -0.0235(12) -0.0140(13) F4 0.0573(12) 0.0743(14) 0.0842(15) 0.0077(12) -0.0288(11) 0.0128(10) F5 0.0337(9) 0.0540(11) 0.0633(12) -0.0051(9) 0.0055(8) 0.0040(8) F6 0.0487(9) 0.0272(8) 0.0469(10) 0.0046(7) 0.0026(8) 0.0028(7) F7 0.0420(9) 0.0240(8) 0.0658(11) -0.0110(8) 0.0054(8) 0.0056(7) F8 0.0496(10) 0.0424(9) 0.0521(11) -0.0234(8) 0.0151(8) -0.0007(8) F9 0.0484(9) 0.0407(9) 0.0306(9) -0.0078(7) 0.0130(7) 0.0007(7) F10 0.0351(8) 0.0406(9) 0.0422(9) -0.0025(7) 0.0059(7) -0.0120(7) F11 0.0349(9) 0.0713(12) 0.0428(10) -0.0010(9) -0.0058(8) -0.0043(8) F12 0.0502(10) 0.0640(11) 0.0411(10) 0.0174(9) 0.0053(8) 0.0197(9) F13 0.0688(12) 0.0390(10) 0.0718(13) 0.0203(9) 0.0067(10) -0.0020(9) F14 0.0416(9) 0.0338(9) 0.0557(11) 0.0004(8) -0.0026(8) -0.0097(7) F15 0.0431(9) 0.0296(8) 0.0427(10) 0.0026(7) 0.0040(7) -0.0068(7) F16 0.0421(9) 0.0497(10) 0.0527(11) -0.0140(8) 0.0126(8) -0.0202(8) F17 0.0281(8) 0.0778(12) 0.0492(11) -0.0159(9) -0.0016(8) -0.0036(8) F18 0.0478(10) 0.0658(12) 0.0452(11) 0.0122(9) -0.0010(8) 0.0161(9) F19 0.0450(9) 0.0340(9) 0.0464(10) 0.0077(7) 0.0138(8) 0.0021(7) F20 0.0272(8) 0.0370(8) 0.0522(10) -0.0118(7) 0.0125(7) 0.0002(7) F21 0.0440(9) 0.0311(8) 0.0558(11) -0.0075(7) 0.0178(8) 0.0063(7) F22 0.0484(9) 0.0231(8) 0.0456(10) -0.0100(7) 0.0110(8) -0.0058(7) F23 0.0310(8) 0.0331(8) 0.0456(10) -0.0068(7) 0.0044(7) -0.0071(7) F24 0.0463(9) 0.0561(10) 0.0354(9) -0.0024(8) 0.0198(8) 0.0016(8) F25 0.0641(11) 0.0627(11) 0.0268(10) 0.0018(8) 0.0015(8) -0.0015(9) F26 0.0348(9) 0.0612(11) 0.0578(12) 0.0066(9) -0.0116(8) 0.0020(8) F27 0.0295(9) 0.0877(13) 0.0671(12) 0.0050(10) 0.0178(9) 0.0124(9) F28 0.0397(9) 0.0668(11) 0.0336(10) -0.0014(8) 0.0164(7) 0.0051(8) Li1 0.047(3) 0.047(3) 0.054(3) -0.009(2) 0.014(2) 0.004(2) O1 0.0437(12) 0.0531(13) 0.0409(12) 0.0012(10) 0.0081(10) 0.0089(10) O2 0.0456(12) 0.0596(13) 0.0440(13) -0.0133(10) 0.0135(10) -0.0035(10) N1 0.0291(11) 0.0265(11) 0.0260(12) -0.0023(9) 0.0024(9) 0.0012(9) N2 0.0270(11) 0.0237(11) 0.0263(12) -0.0014(9) 0.0040(9) 0.0021(9) N3 0.0237(11) 0.0247(11) 0.0295(12) -0.0051(9) 0.0052(9) -0.0030(9) N4 0.0240(11) 0.0264(11) 0.0277(12) -0.0042(9) 0.0050(9) 0.0012(9) C1 0.0360(15) 0.0211(13) 0.0327(16) 0.0000(12) 0.0002(13) -0.0027(12) C2 0.0477(18) 0.0317(15) 0.0357(18) 0.0008(13) 0.0075(14) -0.0030(13) C3 0.088(3) 0.0390(18) 0.0334(19) 0.0010(14) 0.0181(19) -0.0139(18) C4 0.084(3) 0.0426(19) 0.0304(19) 0.0084(15) -0.0133(19) -0.0112(18) C5 0.048(2) 0.0389(18) 0.058(2) 0.0053(16) -0.0124(17) 0.0027(15) C6 0.0422(17) 0.0286(15) 0.0400(18) 0.0002(13) -0.0031(15) -0.0011(13) C7 0.0229(13) 0.0245(14) 0.0334(16) -0.0041(12) 0.0059(11) -0.0014(11) C8 0.0256(13) 0.0295(15) 0.0373(17) 0.0029(13) 0.0017(12) 0.0011(11) C9 0.0289(14) 0.0215(14) 0.0515(19) -0.0079(13) 0.0081(13) 0.0012(11) C10 0.0289(14) 0.0355(16) 0.0397(18) -0.0171(14) 0.0095(13) -0.0042(12) C11 0.0264(13) 0.0330(15) 0.0295(16) -0.0053(12) 0.0061(12) -0.0013(11) C12 0.0213(13) 0.0240(13) 0.0332(16) -0.0052(11) 0.0067(11) -0.0026(10) C13 0.0261(13) 0.0287(14) 0.0232(14) -0.0019(11) 0.0064(11) 0.0031(11) C14 0.0305(15) 0.0311(15) 0.0323(16) -0.0010(12) 0.0107(13) -0.0015(12) C15 0.0229(14) 0.0509(18) 0.0278(16) -0.0031(13) 0.0016(12) 0.0004(13) C16 0.0361(16) 0.0471(18) 0.0282(16) 0.0093(13) 0.0072(13) 0.0127(14) C17 0.0434(17) 0.0303(16) 0.0422(18) 0.0082(13) 0.0125(14) 0.0019(13) C18 0.0266(14) 0.0329(15) 0.0358(16) -0.0019(13) 0.0035(12) 0.0008(12) C19 0.0224(13) 0.0289(14) 0.0274(14) -0.0037(11) 0.0082(11) -0.0002(11) C20 0.0275(14) 0.0304(15) 0.0275(15) -0.0018(12) 0.0064(12) 0.0014(12) C21 0.0285(14) 0.0345(15) 0.0383(17) -0.0118(13) 0.0132(13) -0.0084(13) C22 0.0212(14) 0.0506(18) 0.0356(17) -0.0143(14) 0.0031(12) -0.0011(13) C23 0.0313(15) 0.0477(18) 0.0288(16) 0.0024(13) 0.0041(12) 0.0131(14) C24 0.0328(15) 0.0294(15) 0.0346(16) -0.0018(12) 0.0140(13) 0.0009(12) C25 0.0291(14) 0.0223(13) 0.0278(14) -0.0012(11) 0.0103(11) -0.0027(11) C26 0.0250(14) 0.0310(15) 0.0386(16) -0.0038(12) 0.0115(12) -0.0014(12) C27 0.0357(15) 0.0227(14) 0.0430(17) -0.0045(12) 0.0171(13) 0.0044(12) C28 0.0401(16) 0.0204(13) 0.0351(16) -0.0085(12) 0.0107(13) -0.0064(12) C29 0.0251(14) 0.0274(14) 0.0315(15) -0.0033(12) 0.0058(11) -0.0050(11) C30 0.0288(14) 0.0257(13) 0.0283(14) -0.0016(11) 0.0116(11) -0.0018(11) C31 0.0253(13) 0.0240(13) 0.0266(15) -0.0038(11) 0.0027(11) -0.0034(11) C32 0.0323(15) 0.0293(14) 0.0323(16) -0.0046(12) 0.0117(12) -0.0022(12) C33 0.0442(17) 0.0340(15) 0.0246(16) -0.0005(12) 0.0018(13) -0.0063(13) C34 0.0250(15) 0.0374(16) 0.0429(19) 0.0037(13) -0.0047(13) -0.0019(12) C35 0.0238(14) 0.0424(17) 0.049(2) -0.0022(14) 0.0132(13) -0.0003(12) C36 0.0303(15) 0.0341(15) 0.0296(16) -0.0033(12) 0.0084(12) -0.0012(12) C37 0.062(2) 0.084(3) 0.052(2) 0.005(2) 0.0021(18) 0.013(2) C38 0.064(2) 0.088(3) 0.080(3) -0.010(2) -0.003(2) 0.029(2) C39 0.057(2) 0.062(2) 0.093(3) -0.008(2) 0.031(2) 0.0090(18) C40 0.065(2) 0.079(3) 0.054(2) -0.0170(19) 0.0102(18) 0.0248(19) C41 0.056(2) 0.076(2) 0.060(2) 0.0042(19) 0.0266(18) 0.0128(18) C42 0.069(3) 0.057(3) 0.055(3) 0.005(3) 0.030(3) 0.012(3) C43 0.136(4) 0.078(3) 0.069(3) -0.026(2) 0.053(3) -0.028(3) C41' 0.056(2) 0.076(2) 0.060(2) 0.0042(19) 0.0266(18) 0.0128(18) C42' 0.069(3) 0.057(3) 0.055(3) 0.005(3) 0.030(3) 0.012(3) C43' 0.136(4) 0.078(3) 0.069(3) -0.026(2) 0.053(3) -0.028(3) C44 0.080(3) 0.123(4) 0.049(2) -0.030(2) 0.017(2) -0.028(3) 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 N4 1.849(2) . ? Al1 N2 1.854(2) . ? Al1 N3 1.855(2) . ? Al1 N1 1.859(2) . ? F1 C2 1.345(3) . ? F2 C3 1.346(4) . ? F3 C4 1.349(3) . ? F4 C5 1.347(4) . ? F5 C6 1.347(3) . ? F6 C8 1.362(3) . ? F7 C9 1.377(3) . ? F7 Li1 1.924(5) 2_655 ? F8 C10 1.346(3) . ? F9 C11 1.354(3) . ? F10 C14 1.349(3) . ? F11 C15 1.346(3) . ? F12 C16 1.342(3) . ? F13 C17 1.340(3) . ? F14 C18 1.352(3) . ? F15 C20 1.348(3) . ? F16 C21 1.351(3) . ? F17 C22 1.344(3) . ? F18 C23 1.345(3) . ? F19 C24 1.353(3) . ? F20 C26 1.355(3) . ? F21 C27 1.358(3) . ? F22 C28 1.371(3) . ? F22 Li1 2.089(5) . ? F23 C29 1.351(3) . ? F24 C32 1.352(3) . ? F25 C33 1.344(3) . ? F26 C34 1.347(3) . ? F27 C35 1.341(3) . ? F28 C36 1.348(3) . ? Li1 O2 1.850(5) . ? Li1 O1 1.861(5) . ? Li1 F7 1.924(5) 2_645 ? O1 C40 1.440(4) . ? O1 C37 1.442(4) . ? O2 C41 1.435(4) . ? O2 C44 1.449(4) . ? N1 C7 1.401(3) . ? N1 C1 1.407(3) . ? N2 C12 1.405(3) . ? N2 C13 1.406(3) . ? N3 C25 1.402(3) . ? N3 C19 1.406(3) . ? N4 C30 1.402(3) . ? N4 C31 1.416(3) . ? C1 C2 1.384(4) . ? C1 C6 1.399(4) . ? C2 C3 1.376(4) . ? C3 C4 1.360(5) . ? C4 C5 1.375(5) . ? C5 C6 1.371(4) . ? C7 C8 1.383(3) . ? C7 C12 1.424(3) . ? C8 C9 1.376(4) . ? C9 C10 1.353(4) . ? C10 C11 1.381(4) . ? C11 C12 1.382(3) . ? C13 C18 1.387(3) . ? C13 C14 1.391(3) . ? C14 C15 1.377(4) . ? C15 C16 1.369(4) . ? C16 C17 1.372(4) . ? C17 C18 1.373(4) . ? C19 C20 1.386(3) . ? C19 C24 1.393(3) . ? C20 C21 1.371(3) . ? C21 C22 1.366(4) . ? C22 C23 1.370(4) . ? C23 C24 1.376(4) . ? C25 C26 1.386(3) . ? C25 C30 1.420(3) . ? C26 C27 1.379(3) . ? C27 C28 1.359(4) . ? C28 C29 1.377(3) . ? C29 C30 1.384(3) . ? C31 C36 1.382(3) . ? C31 C32 1.392(3) . ? C32 C33 1.372(4) . ? C33 C34 1.373(4) . ? C34 C35 1.366(4) . ? C35 C36 1.373(4) . ? C37 C38 1.499(5) . ? C37 H37A 0.9602 . ? C37 H37B 0.9601 . ? C38 C39 1.482(5) . ? C38 H38A 0.9599 . ? C38 H38B 0.9599 . ? C39 C40 1.485(5) . ? C39 H39A 0.9601 . ? C39 H39B 0.9600 . ? C40 H40A 0.9598 . ? C40 H40B 0.9600 . ? C41 C42 1.615(7) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.342(7) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.465(5) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C42' H42C 0.9900 . ? C42' H42D 0.9900 . ? C44 H44A 0.9601 . ? C44 H44B 0.9599 . ? 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 N4 Al1 N2 135.98(9) . . ? N4 Al1 N3 87.55(9) . . ? N2 Al1 N3 105.97(9) . . ? N4 Al1 N1 109.63(9) . . ? N2 Al1 N1 87.36(9) . . ? N3 Al1 N1 139.12(9) . . ? C9 F7 Li1 129.2(2) . 2_655 ? C28 F22 Li1 111.34(19) . . ? O2 Li1 O1 130.4(3) . . ? O2 Li1 F7 114.1(3) . 2_645 ? O1 Li1 F7 108.5(2) . 2_645 ? O2 Li1 F22 104.7(2) . . ? O1 Li1 F22 101.9(2) . . ? F7 Li1 F22 86.5(2) 2_645 . ? C40 O1 C37 108.3(2) . . ? C40 O1 Li1 118.5(2) . . ? C37 O1 Li1 132.5(2) . . ? C41 O2 C44 108.5(2) . . ? C41 O2 Li1 123.9(2) . . ? C44 O2 Li1 127.2(3) . . ? C7 N1 C1 120.9(2) . . ? C7 N1 Al1 112.10(16) . . ? C1 N1 Al1 125.45(16) . . ? C12 N2 C13 121.6(2) . . ? C12 N2 Al1 112.59(16) . . ? C13 N2 Al1 123.98(15) . . ? C25 N3 C19 121.71(19) . . ? C25 N3 Al1 112.35(15) . . ? C19 N3 Al1 124.82(15) . . ? C30 N4 C31 119.82(19) . . ? C30 N4 Al1 111.87(15) . . ? C31 N4 Al1 125.80(15) . . ? C2 C1 C6 115.7(3) . . ? C2 C1 N1 120.7(2) . . ? C6 C1 N1 123.4(2) . . ? F1 C2 C3 119.0(3) . . ? F1 C2 C1 118.7(2) . . ? C3 C2 C1 122.3(3) . . ? F2 C3 C4 120.0(3) . . ? F2 C3 C2 119.7(3) . . ? C4 C3 C2 120.3(3) . . ? F3 C4 C3 120.5(4) . . ? F3 C4 C5 120.0(3) . . ? C3 C4 C5 119.5(3) . . ? F4 C5 C6 120.2(3) . . ? F4 C5 C4 119.9(3) . . ? C6 C5 C4 119.9(3) . . ? F5 C6 C5 118.7(3) . . ? F5 C6 C1 119.1(2) . . ? C5 C6 C1 122.2(3) . . ? C8 C7 N1 128.4(2) . . ? C8 C7 C12 117.1(2) . . ? N1 C7 C12 114.4(2) . . ? F6 C8 C9 117.0(2) . . ? F6 C8 C7 121.4(2) . . ? C9 C8 C7 121.6(2) . . ? C10 C9 F7 119.9(2) . . ? C10 C9 C8 121.5(2) . . ? F7 C9 C8 118.6(2) . . ? F8 C10 C9 121.3(2) . . ? F8 C10 C11 120.1(3) . . ? C9 C10 C11 118.5(2) . . ? F9 C11 C10 117.2(2) . . ? F9 C11 C12 121.0(2) . . ? C10 C11 C12 121.8(2) . . ? C11 C12 N2 127.1(2) . . ? C11 C12 C7 119.3(2) . . ? N2 C12 C7 113.5(2) . . ? C18 C13 C14 115.4(2) . . ? C18 C13 N2 119.9(2) . . ? C14 C13 N2 124.4(2) . . ? F10 C14 C15 118.4(2) . . ? F10 C14 C13 119.3(2) . . ? C15 C14 C13 122.3(2) . . ? F11 C15 C16 119.8(2) . . ? F11 C15 C14 119.9(2) . . ? C16 C15 C14 120.3(2) . . ? F12 C16 C15 120.5(3) . . ? F12 C16 C17 120.3(3) . . ? C15 C16 C17 119.1(2) . . ? F13 C17 C16 119.6(2) . . ? F13 C17 C18 120.5(2) . . ? C16 C17 C18 119.9(2) . . ? F14 C18 C17 118.7(2) . . ? F14 C18 C13 118.4(2) . . ? C17 C18 C13 122.9(2) . . ? C20 C19 C24 115.3(2) . . ? C20 C19 N3 119.7(2) . . ? C24 C19 N3 124.9(2) . . ? F15 C20 C21 118.4(2) . . ? F15 C20 C19 118.9(2) . . ? C21 C20 C19 122.6(2) . . ? F16 C21 C22 120.2(2) . . ? F16 C21 C20 119.4(2) . . ? C22 C21 C20 120.4(2) . . ? F17 C22 C21 120.6(3) . . ? F17 C22 C23 120.4(3) . . ? C21 C22 C23 119.0(2) . . ? F18 C23 C22 120.2(2) . . ? F18 C23 C24 119.7(3) . . ? C22 C23 C24 120.1(2) . . ? F19 C24 C23 118.4(2) . . ? F19 C24 C19 119.2(2) . . ? C23 C24 C19 122.4(2) . . ? C26 C25 N3 128.3(2) . . ? C26 C25 C30 118.2(2) . . ? N3 C25 C30 113.5(2) . . ? F20 C26 C27 117.4(2) . . ? F20 C26 C25 121.1(2) . . ? C27 C26 C25 121.4(2) . . ? F21 C27 C28 120.4(2) . . ? F21 C27 C26 119.9(2) . . ? C28 C27 C26 119.7(2) . . ? C27 C28 F22 120.1(2) . . ? C27 C28 C29 120.5(2) . . ? F22 C28 C29 119.4(2) . . ? F23 C29 C28 118.2(2) . . ? F23 C29 C30 120.7(2) . . ? C28 C29 C30 121.1(2) . . ? C29 C30 N4 126.7(2) . . ? C29 C30 C25 118.7(2) . . ? N4 C30 C25 114.6(2) . . ? C36 C31 C32 115.8(2) . . ? C36 C31 N4 120.8(2) . . ? C32 C31 N4 123.2(2) . . ? F24 C32 C33 118.9(2) . . ? F24 C32 C31 118.7(2) . . ? C33 C32 C31 122.3(2) . . ? F25 C33 C32 120.2(2) . . ? F25 C33 C34 120.0(2) . . ? C32 C33 C34 119.8(2) . . ? F26 C34 C35 120.6(2) . . ? F26 C34 C33 119.7(3) . . ? C35 C34 C33 119.7(2) . . ? F27 C35 C34 119.9(2) . . ? F27 C35 C36 120.3(3) . . ? C34 C35 C36 119.8(2) . . ? F28 C36 C35 119.0(2) . . ? F28 C36 C31 118.3(2) . . ? C35 C36 C31 122.7(2) . . ? O1 C37 C38 106.1(3) . . ? O1 C37 H37A 109.0 . . ? C38 C37 H37A 110.9 . . ? O1 C37 H37B 109.2 . . ? C38 C37 H37B 112.1 . . ? H37A C37 H37B 109.5 . . ? C39 C38 C37 104.8(3) . . ? C39 C38 H38A 112.3 . . ? C37 C38 H38A 110.3 . . ? C39 C38 H38B 111.0 . . ? C37 C38 H38B 108.9 . . ? H38A C38 H38B 109.5 . . ? C38 C39 C40 102.4(3) . . ? C38 C39 H39A 108.7 . . ? C40 C39 H39A 112.1 . . ? C38 C39 H39B 110.1 . . ? C40 C39 H39B 113.8 . . ? H39A C39 H39B 109.5 . . ? O1 C40 C39 106.6(3) . . ? O1 C40 H40A 108.5 . . ? C39 C40 H40A 110.7 . . ? O1 C40 H40B 109.4 . . ? C39 C40 H40B 112.0 . . ? H40A C40 H40B 109.5 . . ? O2 C41 C42 98.6(3) . . ? O2 C41 H41A 112.0 . . ? C42 C41 H41A 112.0 . . ? O2 C41 H41B 112.0 . . ? C42 C41 H41B 112.0 . . ? H41A C41 H41B 109.7 . . ? C43 C42 C41 104.5(5) . . ? C43 C42 H42A 110.9 . . ? C41 C42 H42A 110.9 . . ? C43 C42 H42B 110.9 . . ? C41 C42 H42B 110.9 . . ? H42A C42 H42B 108.9 . . ? C42 C43 C44 102.0(4) . . ? C42 C43 H43A 111.4 . . ? C44 C43 H43A 111.4 . . ? C42 C43 H43B 111.4 . . ? C44 C43 H43B 111.4 . . ? H43A C43 H43B 109.2 . . ? H42C C42' H42D 109.6 . . ? O2 C44 C43 107.0(3) . . ? O2 C44 H44A 108.2 . . ? C43 C44 H44A 111.2 . . ? O2 C44 H44B 109.3 . . ? C43 C44 H44B 111.6 . . ? H44A C44 H44B 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 C28 F22 Li1 O2 38.3(3) . . . . ? C28 F22 Li1 O1 -99.5(2) . . . . ? C28 F22 Li1 F7 152.32(18) . . . 2_645 ? O2 Li1 O1 C40 -176.7(3) . . . . ? F7 Li1 O1 C40 34.9(4) 2_645 . . . ? F22 Li1 O1 C40 -55.4(3) . . . . ? O2 Li1 O1 C37 -7.4(6) . . . . ? F7 Li1 O1 C37 -155.8(3) 2_645 . . . ? F22 Li1 O1 C37 114.0(3) . . . . ? O1 Li1 O2 C41 -150.5(3) . . . . ? F7 Li1 O2 C41 -3.5(4) 2_645 . . . ? F22 Li1 O2 C41 89.2(3) . . . . ? O1 Li1 O2 C44 21.3(6) . . . . ? F7 Li1 O2 C44 168.4(3) 2_645 . . . ? F22 Li1 O2 C44 -98.9(3) . . . . ? N4 Al1 N1 C7 138.66(15) . . . . ? N2 Al1 N1 C7 0.26(16) . . . . ? N3 Al1 N1 C7 -111.30(18) . . . . ? N4 Al1 N1 C1 -27.1(2) . . . . ? N2 Al1 N1 C1 -165.5(2) . . . . ? N3 Al1 N1 C1 83.0(2) . . . . ? N4 Al1 N2 C12 -116.54(17) . . . . ? N3 Al1 N2 C12 140.03(15) . . . . ? N1 Al1 N2 C12 -0.69(16) . . . . ? N4 Al1 N2 C13 78.6(2) . . . . ? N3 Al1 N2 C13 -24.9(2) . . . . ? N1 Al1 N2 C13 -165.60(19) . . . . ? N4 Al1 N3 C25 -2.46(16) . . . . ? N2 Al1 N3 C25 134.97(16) . . . . ? N1 Al1 N3 C25 -120.12(17) . . . . ? N4 Al1 N3 C19 -170.42(19) . . . . ? N2 Al1 N3 C19 -33.0(2) . . . . ? N1 Al1 N3 C19 71.9(2) . . . . ? N2 Al1 N4 C30 -106.80(18) . . . . ? N3 Al1 N4 C30 3.81(16) . . . . ? N1 Al1 N4 C30 145.83(15) . . . . ? N2 Al1 N4 C31 91.4(2) . . . . ? N3 Al1 N4 C31 -158.01(19) . . . . ? N1 Al1 N4 C31 -16.0(2) . . . . ? C7 N1 C1 C2 133.2(2) . . . . ? Al1 N1 C1 C2 -62.3(3) . . . . ? C7 N1 C1 C6 -52.0(3) . . . . ? Al1 N1 C1 C6 112.5(2) . . . . ? C6 C1 C2 F1 -178.4(2) . . . . ? N1 C1 C2 F1 -3.3(4) . . . . ? C6 C1 C2 C3 1.3(4) . . . . ? N1 C1 C2 C3 176.5(2) . . . . ? F1 C2 C3 F2 -1.2(4) . . . . ? C1 C2 C3 F2 179.0(2) . . . . ? F1 C2 C3 C4 179.6(3) . . . . ? C1 C2 C3 C4 -0.2(4) . . . . ? F2 C3 C4 F3 0.5(4) . . . . ? C2 C3 C4 F3 179.7(3) . . . . ? F2 C3 C4 C5 -179.3(3) . . . . ? C2 C3 C4 C5 -0.1(5) . . . . ? F3 C4 C5 F4 0.9(4) . . . . ? C3 C4 C5 F4 -179.3(3) . . . . ? F3 C4 C5 C6 179.4(3) . . . . ? C3 C4 C5 C6 -0.8(5) . . . . ? F4 C5 C6 F5 1.2(4) . . . . ? C4 C5 C6 F5 -177.3(3) . . . . ? F4 C5 C6 C1 -179.5(2) . . . . ? C4 C5 C6 C1 2.0(4) . . . . ? C2 C1 C6 F5 177.1(2) . . . . ? N1 C1 C6 F5 2.1(4) . . . . ? C2 C1 C6 C5 -2.2(4) . . . . ? N1 C1 C6 C5 -177.3(2) . . . . ? C1 N1 C7 C8 -15.1(4) . . . . ? Al1 N1 C7 C8 178.5(2) . . . . ? C1 N1 C7 C12 166.7(2) . . . . ? Al1 N1 C7 C12 0.2(2) . . . . ? N1 C7 C8 F6 -1.9(4) . . . . ? C12 C7 C8 F6 176.3(2) . . . . ? N1 C7 C8 C9 179.2(2) . . . . ? C12 C7 C8 C9 -2.6(4) . . . . ? Li1 F7 C9 C10 -144.0(3) 2_655 . . . ? Li1 F7 C9 C8 34.9(4) 2_655 . . . ? F6 C8 C9 C10 -178.5(2) . . . . ? C7 C8 C9 C10 0.4(4) . . . . ? F6 C8 C9 F7 2.6(3) . . . . ? C7 C8 C9 F7 -178.4(2) . . . . ? F7 C9 C10 F8 0.3(4) . . . . ? C8 C9 C10 F8 -178.5(2) . . . . ? F7 C9 C10 C11 179.6(2) . . . . ? C8 C9 C10 C11 0.8(4) . . . . ? F8 C10 C11 F9 1.3(3) . . . . ? C9 C10 C11 F9 -177.9(2) . . . . ? F8 C10 C11 C12 179.6(2) . . . . ? C9 C10 C11 C12 0.3(4) . . . . ? F9 C11 C12 N2 -1.1(4) . . . . ? C10 C11 C12 N2 -179.3(2) . . . . ? F9 C11 C12 C7 175.7(2) . . . . ? C10 C11 C12 C7 -2.5(4) . . . . ? C13 N2 C12 C11 -16.8(4) . . . . ? Al1 N2 C12 C11 177.9(2) . . . . ? C13 N2 C12 C7 166.3(2) . . . . ? Al1 N2 C12 C7 1.0(2) . . . . ? C8 C7 C12 C11 3.6(3) . . . . ? N1 C7 C12 C11 -178.0(2) . . . . ? C8 C7 C12 N2 -179.2(2) . . . . ? N1 C7 C12 N2 -0.8(3) . . . . ? C12 N2 C13 C18 135.3(2) . . . . ? Al1 N2 C13 C18 -61.1(3) . . . . ? C12 N2 C13 C14 -50.4(3) . . . . ? Al1 N2 C13 C14 113.2(2) . . . . ? C18 C13 C14 F10 177.7(2) . . . . ? N2 C13 C14 F10 3.1(4) . . . . ? C18 C13 C14 C15 -0.4(4) . . . . ? N2 C13 C14 C15 -174.9(2) . . . . ? F10 C14 C15 F11 1.6(4) . . . . ? C13 C14 C15 F11 179.7(2) . . . . ? F10 C14 C15 C16 -177.2(2) . . . . ? C13 C14 C15 C16 0.9(4) . . . . ? F11 C15 C16 F12 -0.5(4) . . . . ? C14 C15 C16 F12 178.3(2) . . . . ? F11 C15 C16 C17 179.9(2) . . . . ? C14 C15 C16 C17 -1.3(4) . . . . ? F12 C16 C17 F13 0.8(4) . . . . ? C15 C16 C17 F13 -179.6(2) . . . . ? F12 C16 C17 C18 -178.3(2) . . . . ? C15 C16 C17 C18 1.2(4) . . . . ? F13 C17 C18 F14 -0.6(4) . . . . ? C16 C17 C18 F14 178.5(2) . . . . ? F13 C17 C18 C13 -179.9(2) . . . . ? C16 C17 C18 C13 -0.8(4) . . . . ? C14 C13 C18 F14 -179.0(2) . . . . ? N2 C13 C18 F14 -4.2(3) . . . . ? C14 C13 C18 C17 0.3(4) . . . . ? N2 C13 C18 C17 175.1(2) . . . . ? C25 N3 C19 C20 137.7(2) . . . . ? Al1 N3 C19 C20 -55.4(3) . . . . ? C25 N3 C19 C24 -46.6(3) . . . . ? Al1 N3 C19 C24 120.3(2) . . . . ? C24 C19 C20 F15 -177.9(2) . . . . ? N3 C19 C20 F15 -1.8(3) . . . . ? C24 C19 C20 C21 3.3(3) . . . . ? N3 C19 C20 C21 179.4(2) . . . . ? F15 C20 C21 F16 -2.3(3) . . . . ? C19 C20 C21 F16 176.5(2) . . . . ? F15 C20 C21 C22 179.9(2) . . . . ? C19 C20 C21 C22 -1.3(4) . . . . ? F16 C21 C22 F17 2.1(4) . . . . ? C20 C21 C22 F17 179.9(2) . . . . ? F16 C21 C22 C23 -177.8(2) . . . . ? C20 C21 C22 C23 -0.1(4) . . . . ? F17 C22 C23 F18 1.2(4) . . . . ? C21 C22 C23 F18 -178.9(2) . . . . ? F17 C22 C23 C24 179.3(2) . . . . ? C21 C22 C23 C24 -0.8(4) . . . . ? F18 C23 C24 F19 1.8(4) . . . . ? C22 C23 C24 F19 -176.4(2) . . . . ? F18 C23 C24 C19 -178.8(2) . . . . ? C22 C23 C24 C19 3.1(4) . . . . ? C20 C19 C24 F19 175.3(2) . . . . ? N3 C19 C24 F19 -0.6(4) . . . . ? C20 C19 C24 C23 -4.2(4) . . . . ? N3 C19 C24 C23 179.9(2) . . . . ? C19 N3 C25 C26 -13.1(4) . . . . ? Al1 N3 C25 C26 178.5(2) . . . . ? C19 N3 C25 C30 168.9(2) . . . . ? Al1 N3 C25 C30 0.6(2) . . . . ? N3 C25 C26 F20 -5.6(4) . . . . ? C30 C25 C26 F20 172.3(2) . . . . ? N3 C25 C26 C27 174.4(2) . . . . ? C30 C25 C26 C27 -7.7(4) . . . . ? F20 C26 C27 F21 4.6(4) . . . . ? C25 C26 C27 F21 -175.4(2) . . . . ? F20 C26 C27 C28 -176.1(2) . . . . ? C25 C26 C27 C28 3.9(4) . . . . ? F21 C27 C28 F22 3.4(4) . . . . ? C26 C27 C28 F22 -175.9(2) . . . . ? F21 C27 C28 C29 180.0(2) . . . . ? C26 C27 C28 C29 0.7(4) . . . . ? Li1 F22 C28 C27 83.8(3) . . . . ? Li1 F22 C28 C29 -92.8(3) . . . . ? C27 C28 C29 F23 -178.4(2) . . . . ? F22 C28 C29 F23 -1.8(3) . . . . ? C27 C28 C29 C30 -1.2(4) . . . . ? F22 C28 C29 C30 175.4(2) . . . . ? F23 C29 C30 N4 -2.5(4) . . . . ? C28 C29 C30 N4 -179.7(2) . . . . ? F23 C29 C30 C25 174.4(2) . . . . ? C28 C29 C30 C25 -2.8(4) . . . . ? C31 N4 C30 C29 -24.3(4) . . . . ? Al1 N4 C30 C29 172.6(2) . . . . ? C31 N4 C30 C25 158.6(2) . . . . ? Al1 N4 C30 C25 -4.4(3) . . . . ? C26 C25 C30 C29 7.0(3) . . . . ? N3 C25 C30 C29 -174.8(2) . . . . ? C26 C25 C30 N4 -175.7(2) . . . . ? N3 C25 C30 N4 2.5(3) . . . . ? C30 N4 C31 C36 129.8(2) . . . . ? Al1 N4 C31 C36 -69.7(3) . . . . ? C30 N4 C31 C32 -55.1(3) . . . . ? Al1 N4 C31 C32 105.4(2) . . . . ? C36 C31 C32 F24 178.1(2) . . . . ? N4 C31 C32 F24 2.8(4) . . . . ? C36 C31 C32 C33 0.6(4) . . . . ? N4 C31 C32 C33 -174.7(2) . . . . ? F24 C32 C33 F25 -0.2(4) . . . . ? C31 C32 C33 F25 177.2(2) . . . . ? F24 C32 C33 C34 -177.7(2) . . . . ? C31 C32 C33 C34 -0.2(4) . . . . ? F25 C33 C34 F26 0.9(4) . . . . ? C32 C33 C34 F26 178.4(2) . . . . ? F25 C33 C34 C35 -178.0(2) . . . . ? C32 C33 C34 C35 -0.5(4) . . . . ? F26 C34 C35 F27 2.1(4) . . . . ? C33 C34 C35 F27 -179.0(2) . . . . ? F26 C34 C35 C36 -178.0(2) . . . . ? C33 C34 C35 C36 0.9(4) . . . . ? F27 C35 C36 F28 -1.3(4) . . . . ? C34 C35 C36 F28 178.8(2) . . . . ? F27 C35 C36 C31 179.5(2) . . . . ? C34 C35 C36 C31 -0.4(4) . . . . ? C32 C31 C36 F28 -179.6(2) . . . . ? N4 C31 C36 F28 -4.1(3) . . . . ? C32 C31 C36 C35 -0.3(4) . . . . ? N4 C31 C36 C35 175.2(2) . . . . ? C40 O1 C37 C38 -2.8(4) . . . . ? Li1 O1 C37 C38 -173.0(3) . . . . ? O1 C37 C38 C39 22.9(4) . . . . ? C37 C38 C39 C40 -33.2(4) . . . . ? C37 O1 C40 C39 -18.5(4) . . . . ? Li1 O1 C40 C39 153.3(3) . . . . ? C38 C39 C40 O1 32.1(4) . . . . ? C44 O2 C41 C42 15.1(4) . . . . ? Li1 O2 C41 C42 -171.7(4) . . . . ? O2 C41 C42 C43 -38.1(5) . . . . ? C41 C42 C43 C44 44.0(5) . . . . ? C41 O2 C44 C43 9.5(4) . . . . ? Li1 O2 C44 C43 -163.4(3) . . . . ? C42 C43 C44 O2 -35.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.211 _refine_diff_density_min -0.260 _refine_diff_density_rms 0.050 # Attachment '- 3-Ph3C.cif' data_cal0802 _database_code_depnum_ccdc_archive 'CCDC 784057' #TrackingRef '- 3-Ph3C.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 Al F28 N4, C19 H15' _chemical_formula_sum 'C55 H15 Al F28 N4' _chemical_formula_weight 1290.69 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' 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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.1986(16) _cell_length_b 21.771(3) _cell_length_c 18.362(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.330(2) _cell_angle_gamma 90.00 _cell_volume 4855.4(11) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 4234 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 20.56 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.766 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2552 _exptl_absorpt_coefficient_mu 0.197 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9542 _exptl_absorpt_correction_T_max 0.9806 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 33101 _diffrn_reflns_av_R_equivalents 0.1333 _diffrn_reflns_av_sigmaI/netI 0.1076 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.25 _reflns_number_total 8779 _reflns_number_gt 4348 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1997)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1997)' _computing_data_reduction 'Bruker SAINT (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1997)' _computing_publication_material 'Bruker SHELXTL (Bruker, 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^)+(0.0309P)^2^+1.5058P] 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 8779 _refine_ls_number_parameters 793 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1528 _refine_ls_R_factor_gt 0.0596 _refine_ls_wR_factor_ref 0.1135 _refine_ls_wR_factor_gt 0.0872 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _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 Al Al 0.24844(10) 0.25771(5) 0.08079(6) 0.0314(3) Uani 1 1 d . . . F13 F 0.00503(18) 0.30852(10) 0.26146(12) 0.0482(6) Uani 1 1 d . . . F14 F 0.0095(2) 0.22920(11) 0.37077(12) 0.0586(7) Uani 1 1 d . . . F15 F 0.1440(2) 0.12848(10) 0.37515(13) 0.0614(8) Uani 1 1 d . . . F16 F 0.2681(2) 0.10635(10) 0.26567(12) 0.0495(6) Uani 1 1 d . . . F23 F 0.30765(17) 0.21097(9) -0.16642(11) 0.0400(6) Uani 1 1 d . . . F24 F 0.45320(19) 0.28492(10) -0.22316(12) 0.0525(7) Uani 1 1 d . . . F25 F 0.5487(2) 0.37843(11) -0.14322(13) 0.0632(7) Uani 1 1 d . . . F26 F 0.5009(2) 0.39818(11) -0.00622(13) 0.0605(7) Uani 1 1 d . . . F32 F 0.48117(18) 0.18582(10) 0.11354(13) 0.0508(6) Uani 1 1 d . . . F33 F 0.5793(2) 0.08191(11) 0.07634(14) 0.0645(8) Uani 1 1 d . . . F34 F 0.4664(2) -0.02602(10) 0.06772(13) 0.0657(8) Uani 1 1 d . . . F35 F 0.2500(2) -0.02677(10) 0.08946(13) 0.0659(8) Uani 1 1 d . . . F36 F 0.1496(2) 0.07712(10) 0.12694(13) 0.0525(7) Uani 1 1 d . . . F42 F 0.0018(2) 0.32753(11) 0.02440(13) 0.0624(7) Uani 1 1 d . . . F43 F -0.0776(2) 0.44200(13) 0.01447(16) 0.0860(10) Uani 1 1 d . . . F44 F -0.0211(3) 0.52528(12) 0.12172(17) 0.0909(10) Uani 1 1 d . . . F45 F 0.1147(2) 0.49132(11) 0.23983(16) 0.0788(9) Uani 1 1 d . . . F46 F 0.19511(19) 0.37694(10) 0.25021(13) 0.0521(7) Uani 1 1 d . . . F52 F 0.4541(2) 0.32095(10) 0.19644(12) 0.0545(7) Uani 1 1 d . . . F53 F 0.4743(2) 0.42285(11) 0.27936(13) 0.0697(8) Uani 1 1 d . . . F54 F 0.3903(2) 0.53035(10) 0.22858(13) 0.0643(8) Uani 1 1 d . . . F55 F 0.2850(2) 0.53659(10) 0.09042(14) 0.0685(8) Uani 1 1 d . . . F56 F 0.2652(2) 0.43537(10) 0.00703(13) 0.0611(7) Uani 1 1 d . . . F62 F 0.3767(2) 0.12801(9) -0.06979(12) 0.0470(6) Uani 1 1 d . . . F63 F 0.2753(2) 0.02341(11) -0.11351(15) 0.0683(8) Uani 1 1 d . . . F64 F 0.0577(2) 0.00733(11) -0.09929(16) 0.0807(9) Uani 1 1 d . . . F65 F -0.0585(2) 0.09975(12) -0.04278(15) 0.0747(9) Uani 1 1 d . . . F66 F 0.04008(18) 0.20520(10) -0.00228(12) 0.0506(7) Uani 1 1 d . . . N11 N 0.2626(3) 0.19019(13) 0.14105(16) 0.0318(8) Uani 1 1 d . . . N12 N 0.1450(2) 0.28763(13) 0.14010(16) 0.0324(8) Uani 1 1 d . . . N21 N 0.3424(3) 0.32010(13) 0.05900(16) 0.0328(8) Uani 1 1 d . . . N22 N 0.2567(2) 0.22840(13) -0.01361(16) 0.0293(8) Uani 1 1 d . . . C11 C 0.2002(3) 0.19536(17) 0.2011(2) 0.0323(10) Uani 1 1 d . . . C12 C 0.1353(3) 0.24975(17) 0.20132(19) 0.0294(9) Uani 1 1 d . . . C13 C 0.0718(3) 0.25833(19) 0.2586(2) 0.0375(10) Uani 1 1 d . . . C14 C 0.0725(3) 0.2174(2) 0.3165(2) 0.0399(11) Uani 1 1 d . . . C15 C 0.1377(4) 0.1666(2) 0.3172(2) 0.0430(12) Uani 1 1 d . . . C16 C 0.2008(4) 0.15618(18) 0.2603(2) 0.0385(11) Uani 1 1 d . . . C21 C 0.3765(3) 0.31378(17) -0.0117(2) 0.0334(10) Uani 1 1 d . . . C22 C 0.3295(3) 0.26335(17) -0.0520(2) 0.0302(9) Uani 1 1 d . . . C23 C 0.3566(3) 0.25545(16) -0.1226(2) 0.0303(9) Uani 1 1 d . . . C24 C 0.4293(3) 0.29353(18) -0.1535(2) 0.0348(10) Uani 1 1 d . . . C25 C 0.4760(3) 0.34110(19) -0.1134(2) 0.0413(11) Uani 1 1 d . . . C26 C 0.4501(4) 0.35064(19) -0.0435(2) 0.0430(11) Uani 1 1 d . . . C31 C 0.3129(3) 0.13474(17) 0.1249(2) 0.0324(10) Uani 1 1 d . . . C32 C 0.4211(4) 0.13327(18) 0.1100(2) 0.0376(11) Uani 1 1 d . . . C33 C 0.4730(4) 0.0801(2) 0.0907(2) 0.0424(11) Uani 1 1 d . . . C34 C 0.4169(4) 0.02618(19) 0.0850(2) 0.0458(12) Uani 1 1 d . . . C35 C 0.3086(4) 0.02568(18) 0.0975(2) 0.0439(12) Uani 1 1 d . . . C36 C 0.2576(4) 0.07892(18) 0.1164(2) 0.0381(11) Uani 1 1 d . . . C41 C 0.1004(3) 0.34755(17) 0.1372(2) 0.0339(10) Uani 1 1 d . . . C42 C 0.0316(4) 0.3679(2) 0.0781(2) 0.0448(11) Uani 1 1 d . . . C43 C -0.0091(4) 0.4262(2) 0.0719(3) 0.0572(13) Uani 1 1 d . . . C44 C 0.0192(4) 0.4676(2) 0.1270(3) 0.0577(14) Uani 1 1 d . . . C45 C 0.0864(4) 0.4504(2) 0.1865(3) 0.0513(13) Uani 1 1 d . . . C46 C 0.1271(3) 0.39201(19) 0.1911(2) 0.0406(11) Uani 1 1 d . . . C51 C 0.3601(3) 0.37486(17) 0.0988(2) 0.0344(10) Uani 1 1 d . . . C52 C 0.4131(3) 0.37399(17) 0.1687(2) 0.0351(10) Uani 1 1 d . . . C53 C 0.4233(4) 0.4258(2) 0.2114(2) 0.0429(11) Uani 1 1 d . . . C54 C 0.3817(4) 0.48042(19) 0.1857(2) 0.0417(11) Uani 1 1 d . . . C55 C 0.3297(4) 0.48338(18) 0.1163(2) 0.0459(12) Uani 1 1 d . . . C56 C 0.3193(3) 0.43136(18) 0.0738(2) 0.0408(11) Uani 1 1 d . . . C61 C 0.2105(3) 0.17274(17) -0.0395(2) 0.0310(10) Uani 1 1 d . . . C62 C 0.2664(3) 0.12328(18) -0.0661(2) 0.0371(10) Uani 1 1 d . . . C63 C 0.2161(4) 0.06904(18) -0.0868(2) 0.0450(12) Uani 1 1 d . . . C64 C 0.1073(4) 0.0605(2) -0.0795(2) 0.0514(13) Uani 1 1 d . . . C65 C 0.0487(4) 0.1070(2) -0.0516(2) 0.0464(12) Uani 1 1 d . . . C66 C 0.1003(4) 0.16146(18) -0.0317(2) 0.0368(11) Uani 1 1 d . . . C70 C 0.7384(3) 0.28663(19) 0.2590(2) 0.0420(11) Uani 1 1 d . . . C71 C 0.7392(4) 0.3479(2) 0.2270(2) 0.0442(11) Uani 1 1 d . . . C72 C 0.7860(4) 0.3974(2) 0.2686(2) 0.0526(12) Uani 1 1 d . . . H72 H 0.8144 0.3912 0.3180 0.063 Uiso 1 1 calc R . . C73 C 0.7906(4) 0.4547(2) 0.2375(3) 0.0603(14) Uani 1 1 d . . . H73 H 0.8241 0.4877 0.2651 0.072 Uiso 1 1 calc R . . C74 C 0.7470(4) 0.4645(2) 0.1670(3) 0.0652(15) Uani 1 1 d . . . H74 H 0.7491 0.5044 0.1464 0.078 Uiso 1 1 calc R . . C75 C 0.7001(4) 0.4169(2) 0.1257(3) 0.0640(14) Uani 1 1 d . . . H75 H 0.6686 0.4244 0.0772 0.077 Uiso 1 1 calc R . . C76 C 0.6987(4) 0.3582(2) 0.1546(2) 0.0499(12) Uani 1 1 d . . . H76 H 0.6701 0.3250 0.1251 0.060 Uiso 1 1 calc R . . C81 C 0.7146(3) 0.27931(19) 0.3340(2) 0.0418(11) Uani 1 1 d . . . C82 C 0.7597(3) 0.2305(2) 0.3776(2) 0.0507(12) Uani 1 1 d . . . H82 H 0.8071 0.2016 0.3577 0.061 Uiso 1 1 calc R . . C83 C 0.7353(4) 0.2248(2) 0.4485(3) 0.0635(14) Uani 1 1 d . . . H83 H 0.7658 0.1917 0.4776 0.076 Uiso 1 1 calc R . . C84 C 0.6667(4) 0.2666(2) 0.4784(3) 0.0651(14) Uani 1 1 d . . . H84 H 0.6504 0.2622 0.5277 0.078 Uiso 1 1 calc R . . C85 C 0.6219(4) 0.3145(2) 0.4368(3) 0.0571(13) Uani 1 1 d . . . H85 H 0.5745 0.3430 0.4574 0.069 Uiso 1 1 calc R . . C86 C 0.6454(3) 0.3214(2) 0.3658(2) 0.0485(12) Uani 1 1 d . . . H86 H 0.6147 0.3548 0.3377 0.058 Uiso 1 1 calc R . . C91 C 0.7640(3) 0.23489(19) 0.2151(2) 0.0411(11) Uani 1 1 d . . . C92 C 0.8359(3) 0.2417(2) 0.1603(2) 0.0455(11) Uani 1 1 d . . . H92 H 0.8623 0.2815 0.1499 0.055 Uiso 1 1 calc R . . C93 C 0.8689(4) 0.1924(2) 0.1215(2) 0.0577(13) Uani 1 1 d . . . H93 H 0.9175 0.1978 0.0844 0.069 Uiso 1 1 calc R . . C94 C 0.8305(4) 0.1348(2) 0.1371(3) 0.0671(15) Uani 1 1 d . . . H94 H 0.8545 0.1002 0.1113 0.081 Uiso 1 1 calc R . . C95 C 0.7588(4) 0.1267(2) 0.1887(3) 0.0649(15) Uani 1 1 d . . . H95 H 0.7317 0.0867 0.1975 0.078 Uiso 1 1 calc R . . C96 C 0.7250(4) 0.1754(2) 0.2284(2) 0.0504(12) Uani 1 1 d . . . H96 H 0.6755 0.1691 0.2647 0.060 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 Al 0.0384(8) 0.0254(7) 0.0312(7) 0.0011(5) 0.0068(6) 0.0000(6) F13 0.0412(15) 0.0579(16) 0.0468(15) -0.0047(12) 0.0117(12) 0.0064(13) F14 0.0611(17) 0.0780(19) 0.0406(15) -0.0059(13) 0.0258(14) -0.0178(14) F15 0.091(2) 0.0533(16) 0.0417(15) 0.0127(13) 0.0127(14) -0.0231(15) F16 0.0754(18) 0.0303(14) 0.0428(14) 0.0091(11) 0.0057(13) 0.0018(13) F23 0.0476(15) 0.0375(13) 0.0352(13) -0.0054(11) 0.0051(11) -0.0049(11) F24 0.0639(17) 0.0553(16) 0.0412(15) -0.0040(12) 0.0201(13) -0.0092(13) F25 0.075(2) 0.0615(17) 0.0574(17) -0.0078(14) 0.0307(15) -0.0277(15) F26 0.0757(19) 0.0543(16) 0.0543(16) -0.0168(13) 0.0211(14) -0.0343(14) F32 0.0444(15) 0.0394(15) 0.0699(17) -0.0041(13) 0.0120(13) -0.0028(12) F33 0.0586(19) 0.0605(18) 0.0766(19) -0.0036(14) 0.0173(16) 0.0147(14) F34 0.103(2) 0.0370(15) 0.0598(17) -0.0014(13) 0.0186(16) 0.0230(15) F35 0.101(2) 0.0309(15) 0.0678(18) -0.0061(13) 0.0191(16) -0.0142(15) F36 0.0549(18) 0.0428(15) 0.0603(17) -0.0047(13) 0.0077(14) -0.0133(13) F42 0.078(2) 0.0596(17) 0.0459(16) 0.0006(14) -0.0123(14) 0.0133(15) F43 0.096(2) 0.083(2) 0.076(2) 0.0258(17) -0.0087(19) 0.0360(18) F44 0.119(3) 0.0459(17) 0.112(3) 0.0134(17) 0.031(2) 0.0405(18) F45 0.109(2) 0.0434(16) 0.086(2) -0.0267(16) 0.0207(18) 0.0053(16) F46 0.0567(17) 0.0511(16) 0.0477(16) -0.0102(13) 0.0002(14) 0.0028(13) F52 0.0808(19) 0.0370(14) 0.0445(15) 0.0063(12) -0.0014(14) 0.0063(13) F53 0.109(2) 0.0598(18) 0.0368(16) -0.0071(13) -0.0103(16) -0.0019(16) F54 0.100(2) 0.0366(15) 0.0577(17) -0.0176(13) 0.0132(16) -0.0113(14) F55 0.090(2) 0.0289(14) 0.083(2) 0.0030(14) -0.0094(17) 0.0062(14) F56 0.080(2) 0.0436(15) 0.0548(17) 0.0032(13) -0.0204(15) 0.0006(14) F62 0.0440(16) 0.0400(15) 0.0567(16) -0.0049(12) 0.0029(13) 0.0066(12) F63 0.081(2) 0.0348(15) 0.088(2) -0.0171(14) 0.0035(17) 0.0066(14) F64 0.095(2) 0.0476(17) 0.100(2) -0.0196(16) 0.0103(18) -0.0312(16) F65 0.0531(19) 0.082(2) 0.092(2) -0.0136(17) 0.0207(16) -0.0328(15) F66 0.0476(16) 0.0496(16) 0.0576(16) -0.0089(13) 0.0214(13) -0.0065(12) N11 0.040(2) 0.0220(18) 0.035(2) -0.0011(15) 0.0092(17) 0.0038(16) N12 0.039(2) 0.0265(18) 0.0324(19) 0.0028(15) 0.0086(16) 0.0034(16) N21 0.044(2) 0.0258(19) 0.030(2) -0.0044(15) 0.0084(17) -0.0050(16) N22 0.036(2) 0.0199(17) 0.0330(19) -0.0009(15) 0.0065(16) -0.0055(15) C11 0.036(3) 0.028(2) 0.033(2) -0.0015(19) 0.005(2) -0.007(2) C12 0.031(2) 0.033(2) 0.024(2) -0.0001(19) -0.0003(19) -0.0033(19) C13 0.034(3) 0.043(3) 0.036(3) -0.009(2) 0.004(2) -0.003(2) C14 0.041(3) 0.053(3) 0.027(2) -0.004(2) 0.012(2) -0.018(2) C15 0.062(3) 0.039(3) 0.028(3) 0.009(2) 0.007(2) -0.017(2) C16 0.050(3) 0.026(2) 0.039(3) 0.004(2) -0.001(2) -0.004(2) C21 0.041(3) 0.028(2) 0.032(2) 0.0012(19) 0.003(2) -0.003(2) C22 0.029(2) 0.027(2) 0.035(2) 0.0030(19) 0.0062(19) 0.0045(19) C23 0.033(2) 0.025(2) 0.033(2) -0.0058(19) 0.000(2) -0.0022(19) C24 0.042(3) 0.040(3) 0.023(2) 0.002(2) 0.011(2) -0.001(2) C25 0.045(3) 0.035(3) 0.046(3) 0.007(2) 0.013(2) -0.013(2) C26 0.049(3) 0.041(3) 0.040(3) -0.010(2) 0.010(2) -0.014(2) C31 0.037(3) 0.028(2) 0.032(2) 0.0045(19) 0.005(2) -0.002(2) C32 0.049(3) 0.028(3) 0.035(3) 0.0022(19) 0.002(2) -0.002(2) C33 0.043(3) 0.044(3) 0.041(3) 0.004(2) 0.011(2) 0.005(2) C34 0.072(4) 0.027(3) 0.039(3) 0.001(2) 0.009(3) 0.019(3) C35 0.072(4) 0.018(2) 0.042(3) 0.000(2) 0.008(3) -0.004(2) C36 0.043(3) 0.035(3) 0.037(3) 0.003(2) 0.007(2) -0.006(2) C41 0.038(3) 0.032(2) 0.033(2) 0.002(2) 0.013(2) 0.006(2) C42 0.054(3) 0.043(3) 0.037(3) -0.002(2) 0.005(2) 0.010(2) C43 0.061(4) 0.056(3) 0.054(3) 0.022(3) 0.005(3) 0.023(3) C44 0.069(4) 0.035(3) 0.073(4) 0.003(3) 0.027(3) 0.021(3) C45 0.055(3) 0.042(3) 0.058(3) -0.008(3) 0.012(3) 0.005(3) C46 0.041(3) 0.039(3) 0.043(3) 0.001(2) 0.008(2) 0.009(2) C51 0.043(3) 0.028(2) 0.032(2) 0.000(2) 0.006(2) -0.004(2) C52 0.048(3) 0.024(2) 0.034(3) 0.003(2) 0.010(2) 0.004(2) C53 0.059(3) 0.041(3) 0.028(3) 0.001(2) 0.004(2) -0.005(2) C54 0.058(3) 0.028(3) 0.041(3) -0.013(2) 0.011(2) -0.011(2) C55 0.056(3) 0.024(3) 0.057(3) 0.003(2) -0.001(3) 0.002(2) C56 0.051(3) 0.033(3) 0.037(3) 0.000(2) -0.006(2) -0.006(2) C61 0.033(3) 0.030(2) 0.030(2) 0.0024(18) 0.004(2) -0.002(2) C62 0.033(3) 0.036(3) 0.041(3) 0.005(2) 0.002(2) 0.001(2) C63 0.061(4) 0.024(3) 0.050(3) -0.011(2) 0.004(3) 0.000(2) C64 0.063(4) 0.033(3) 0.057(3) -0.007(2) -0.002(3) -0.021(3) C65 0.040(3) 0.043(3) 0.057(3) -0.002(2) 0.007(2) -0.018(2) C66 0.044(3) 0.035(3) 0.032(3) -0.002(2) 0.010(2) 0.003(2) C70 0.032(3) 0.048(3) 0.045(3) -0.002(2) 0.002(2) 0.002(2) C71 0.046(3) 0.043(3) 0.045(3) -0.007(2) 0.013(2) 0.000(2) C72 0.063(3) 0.048(3) 0.047(3) -0.010(3) 0.007(3) 0.001(3) C73 0.073(4) 0.042(3) 0.067(4) -0.013(3) 0.012(3) -0.006(3) C74 0.085(4) 0.046(3) 0.066(4) 0.004(3) 0.013(3) 0.000(3) C75 0.076(4) 0.068(4) 0.047(3) 0.004(3) 0.001(3) -0.004(3) C76 0.060(3) 0.049(3) 0.040(3) -0.003(2) 0.003(2) -0.010(2) C81 0.039(3) 0.047(3) 0.040(3) -0.003(2) 0.004(2) 0.001(2) C82 0.043(3) 0.058(3) 0.052(3) -0.003(3) 0.008(2) 0.004(2) C83 0.056(3) 0.087(4) 0.048(3) 0.012(3) 0.005(3) 0.013(3) C84 0.059(4) 0.092(4) 0.045(3) 0.003(3) 0.009(3) 0.009(3) C85 0.047(3) 0.079(4) 0.046(3) -0.018(3) 0.011(3) 0.010(3) C86 0.048(3) 0.052(3) 0.046(3) -0.008(2) 0.007(2) 0.011(2) C91 0.041(3) 0.038(3) 0.045(3) -0.009(2) 0.010(2) -0.002(2) C92 0.044(3) 0.046(3) 0.046(3) -0.006(2) 0.004(2) -0.011(2) C93 0.064(4) 0.059(3) 0.054(3) -0.013(3) 0.027(3) -0.007(3) C94 0.088(4) 0.042(3) 0.077(4) -0.019(3) 0.037(3) -0.006(3) C95 0.077(4) 0.040(3) 0.080(4) -0.006(3) 0.022(3) -0.014(3) C96 0.052(3) 0.049(3) 0.054(3) -0.009(2) 0.022(2) -0.010(2) _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 Al N11 1.838(3) . ? Al N21 1.845(3) . ? Al N22 1.859(3) . ? Al N12 1.859(3) . ? F13 C13 1.367(4) . ? F14 C14 1.339(4) . ? F15 C15 1.346(4) . ? F16 C16 1.359(4) . ? F23 C23 1.361(4) . ? F24 C24 1.351(4) . ? F25 C25 1.356(4) . ? F26 C26 1.358(4) . ? F32 C32 1.357(4) . ? F33 C33 1.349(4) . ? F34 C34 1.339(4) . ? F35 C35 1.348(4) . ? F36 C36 1.350(4) . ? F42 C42 1.345(4) . ? F43 C43 1.329(5) . ? F44 C44 1.349(5) . ? F45 C45 1.345(5) . ? F46 C46 1.345(4) . ? F52 C52 1.340(4) . ? F53 C53 1.343(4) . ? F54 C54 1.341(4) . ? F55 C55 1.348(4) . ? F56 C56 1.341(4) . ? F62 C62 1.357(4) . ? F63 C63 1.347(4) . ? F64 C64 1.341(4) . ? F65 C65 1.342(5) . ? F66 C66 1.346(4) . ? N11 C31 1.398(4) . ? N11 C11 1.402(5) . ? N12 C12 1.408(4) . ? N12 C41 1.412(4) . ? N21 C51 1.404(4) . ? N21 C21 1.406(4) . ? N22 C61 1.400(4) . ? N22 C22 1.408(4) . ? C11 C16 1.381(5) . ? C11 C12 1.425(5) . ? C12 C13 1.376(5) . ? C13 C14 1.386(5) . ? C14 C15 1.362(6) . ? C15 C16 1.372(5) . ? C21 C26 1.374(5) . ? C21 C22 1.416(5) . ? C22 C23 1.378(5) . ? C23 C24 1.375(5) . ? C24 C25 1.364(5) . ? C25 C26 1.366(5) . ? C31 C32 1.373(5) . ? C31 C36 1.392(5) . ? C32 C33 1.381(5) . ? C33 C34 1.358(6) . ? C34 C35 1.363(6) . ? C35 C36 1.375(5) . ? C41 C42 1.382(5) . ? C41 C46 1.400(5) . ? C42 C43 1.364(6) . ? C43 C44 1.374(6) . ? C44 C45 1.357(6) . ? C45 C46 1.365(5) . ? C51 C52 1.383(5) . ? C51 C56 1.388(5) . ? C52 C53 1.373(5) . ? C53 C54 1.360(5) . ? C54 C55 1.371(6) . ? C55 C56 1.374(5) . ? C61 C62 1.387(5) . ? C61 C66 1.388(5) . ? C62 C63 1.368(5) . ? C63 C64 1.360(6) . ? C64 C65 1.365(6) . ? C65 C66 1.376(5) . ? C70 C91 1.436(5) . ? C70 C81 1.442(5) . ? C70 C71 1.458(5) . ? C71 C76 1.393(6) . ? C71 C72 1.410(5) . ? C72 C73 1.376(6) . ? C73 C74 1.370(6) . ? C74 C75 1.376(6) . ? C75 C76 1.384(6) . ? C81 C86 1.408(5) . ? C81 C82 1.411(5) . ? C82 C83 1.368(6) . ? C83 C84 1.385(6) . ? C84 C85 1.375(6) . ? C85 C86 1.368(6) . ? C91 C92 1.402(5) . ? C91 C96 1.408(5) . ? C92 C93 1.371(5) . ? C93 C94 1.378(6) . ? C94 C95 1.361(6) . ? C95 C96 1.372(6) . ? 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 N11 Al N21 133.92(15) . . ? N11 Al N22 106.06(14) . . ? N21 Al N22 87.83(13) . . ? N11 Al N12 87.62(14) . . ? N21 Al N12 109.77(14) . . ? N22 Al N12 139.89(15) . . ? C31 N11 C11 121.1(3) . . ? C31 N11 Al 125.5(3) . . ? C11 N11 Al 112.5(2) . . ? C12 N12 C41 120.7(3) . . ? C12 N12 Al 112.0(2) . . ? C41 N12 Al 125.5(2) . . ? C51 N21 C21 121.3(3) . . ? C51 N21 Al 125.5(3) . . ? C21 N21 Al 111.8(2) . . ? C61 N22 C22 123.3(3) . . ? C61 N22 Al 124.0(2) . . ? C22 N22 Al 111.9(2) . . ? C16 C11 N11 127.3(4) . . ? C16 C11 C12 118.3(4) . . ? N11 C11 C12 114.3(3) . . ? C13 C12 N12 128.8(4) . . ? C13 C12 C11 117.8(4) . . ? N12 C12 C11 113.4(3) . . ? F13 C13 C12 121.1(4) . . ? F13 C13 C14 116.5(4) . . ? C12 C13 C14 122.3(4) . . ? F14 C14 C15 121.6(4) . . ? F14 C14 C13 118.9(4) . . ? C15 C14 C13 119.5(4) . . ? F15 C15 C14 119.9(4) . . ? F15 C15 C16 120.3(4) . . ? C14 C15 C16 119.7(4) . . ? F16 C16 C15 117.1(4) . . ? F16 C16 C11 120.6(4) . . ? C15 C16 C11 122.3(4) . . ? C26 C21 N21 126.6(4) . . ? C26 C21 C22 118.6(4) . . ? N21 C21 C22 114.8(3) . . ? C23 C22 N22 128.5(3) . . ? C23 C22 C21 117.9(4) . . ? N22 C22 C21 113.6(3) . . ? F23 C23 C24 116.7(3) . . ? F23 C23 C22 120.9(3) . . ? C24 C23 C22 122.2(4) . . ? F24 C24 C25 120.0(4) . . ? F24 C24 C23 120.7(3) . . ? C25 C24 C23 119.2(4) . . ? F25 C25 C24 119.5(4) . . ? F25 C25 C26 120.4(4) . . ? C24 C25 C26 120.1(4) . . ? F26 C26 C25 117.0(4) . . ? F26 C26 C21 121.1(4) . . ? C25 C26 C21 121.9(4) . . ? C32 C31 C36 115.0(4) . . ? C32 C31 N11 120.8(4) . . ? C36 C31 N11 124.0(4) . . ? F32 C32 C31 119.7(4) . . ? F32 C32 C33 117.4(4) . . ? C31 C32 C33 122.9(4) . . ? F33 C33 C34 119.8(4) . . ? F33 C33 C32 119.9(4) . . ? C34 C33 C32 120.3(4) . . ? F34 C34 C33 121.2(5) . . ? F34 C34 C35 119.9(4) . . ? C33 C34 C35 118.9(4) . . ? F35 C35 C34 120.0(4) . . ? F35 C35 C36 119.6(4) . . ? C34 C35 C36 120.3(4) . . ? F36 C36 C35 118.8(4) . . ? F36 C36 C31 118.6(4) . . ? C35 C36 C31 122.6(4) . . ? C42 C41 C46 114.7(4) . . ? C42 C41 N12 121.9(4) . . ? C46 C41 N12 123.3(4) . . ? F42 C42 C43 118.4(4) . . ? F42 C42 C41 118.0(4) . . ? C43 C42 C41 123.6(4) . . ? F43 C43 C42 120.3(5) . . ? F43 C43 C44 120.7(4) . . ? C42 C43 C44 119.0(4) . . ? F44 C44 C45 120.2(5) . . ? F44 C44 C43 119.5(5) . . ? C45 C44 C43 120.3(4) . . ? F45 C45 C44 119.9(4) . . ? F45 C45 C46 120.4(4) . . ? C44 C45 C46 119.7(4) . . ? F46 C46 C45 118.0(4) . . ? F46 C46 C41 119.1(4) . . ? C45 C46 C41 122.8(4) . . ? C52 C51 C56 116.2(4) . . ? C52 C51 N21 120.5(3) . . ? C56 C51 N21 123.2(4) . . ? F52 C52 C53 118.7(4) . . ? F52 C52 C51 119.4(3) . . ? C53 C52 C51 121.9(4) . . ? F53 C53 C54 119.3(4) . . ? F53 C53 C52 120.1(4) . . ? C54 C53 C52 120.6(4) . . ? F54 C54 C53 119.9(4) . . ? F54 C54 C55 120.8(4) . . ? C53 C54 C55 119.3(4) . . ? F55 C55 C54 120.4(4) . . ? F55 C55 C56 119.7(4) . . ? C54 C55 C56 119.9(4) . . ? F56 C56 C55 118.5(4) . . ? F56 C56 C51 119.4(4) . . ? C55 C56 C51 122.1(4) . . ? C62 C61 C66 114.3(4) . . ? C62 C61 N22 126.6(4) . . ? C66 C61 N22 118.7(4) . . ? F62 C62 C63 118.2(4) . . ? F62 C62 C61 118.7(4) . . ? C63 C62 C61 123.1(4) . . ? F63 C63 C64 119.8(4) . . ? F63 C63 C62 119.7(4) . . ? C64 C63 C62 120.5(4) . . ? F64 C64 C63 120.7(4) . . ? F64 C64 C65 120.2(4) . . ? C63 C64 C65 119.1(4) . . ? F65 C65 C64 120.5(4) . . ? F65 C65 C66 119.7(4) . . ? C64 C65 C66 119.7(4) . . ? F66 C66 C65 117.6(4) . . ? F66 C66 C61 119.1(4) . . ? C65 C66 C61 123.3(4) . . ? C91 C70 C81 121.5(4) . . ? C91 C70 C71 118.8(4) . . ? C81 C70 C71 119.7(4) . . ? C76 C71 C72 118.9(4) . . ? C76 C71 C70 121.1(4) . . ? C72 C71 C70 119.9(4) . . ? C73 C72 C71 119.9(4) . . ? C74 C73 C72 120.4(5) . . ? C73 C74 C75 120.6(5) . . ? C74 C75 C76 120.1(5) . . ? C75 C76 C71 120.0(4) . . ? C86 C81 C82 118.1(4) . . ? C86 C81 C70 120.4(4) . . ? C82 C81 C70 121.5(4) . . ? C83 C82 C81 120.1(4) . . ? C82 C83 C84 120.6(5) . . ? C85 C84 C83 120.2(5) . . ? C86 C85 C84 120.3(4) . . ? C85 C86 C81 120.7(4) . . ? C92 C91 C96 117.8(4) . . ? C92 C91 C70 120.1(4) . . ? C96 C91 C70 122.0(4) . . ? C93 C92 C91 121.6(4) . . ? C92 C93 C94 118.9(4) . . ? C95 C94 C93 121.1(4) . . ? C94 C95 C96 120.9(4) . . ? C95 C96 C91 119.8(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 N21 Al N11 C31 -79.4(4) . . . . ? N22 Al N11 C31 23.4(3) . . . . ? N12 Al N11 C31 165.1(3) . . . . ? N21 Al N11 C11 111.2(3) . . . . ? N22 Al N11 C11 -146.0(2) . . . . ? N12 Al N11 C11 -4.3(3) . . . . ? N11 Al N12 C12 4.8(2) . . . . ? N21 Al N12 C12 -131.5(2) . . . . ? N22 Al N12 C12 117.2(3) . . . . ? N11 Al N12 C41 169.6(3) . . . . ? N21 Al N12 C41 33.3(3) . . . . ? N22 Al N12 C41 -78.1(4) . . . . ? N11 Al N21 C51 -86.3(4) . . . . ? N22 Al N21 C51 163.4(3) . . . . ? N12 Al N21 C51 20.3(3) . . . . ? N11 Al N21 C21 107.4(3) . . . . ? N22 Al N21 C21 -2.9(3) . . . . ? N12 Al N21 C21 -146.0(2) . . . . ? N11 Al N22 C61 37.8(3) . . . . ? N21 Al N22 C61 173.1(3) . . . . ? N12 Al N22 C61 -68.2(4) . . . . ? N11 Al N22 C22 -132.5(2) . . . . ? N21 Al N22 C22 2.8(2) . . . . ? N12 Al N22 C22 121.6(3) . . . . ? C31 N11 C11 C16 17.2(6) . . . . ? Al N11 C11 C16 -172.8(3) . . . . ? C31 N11 C11 C12 -167.1(3) . . . . ? Al N11 C11 C12 2.9(4) . . . . ? C41 N12 C12 C13 11.0(6) . . . . ? Al N12 C12 C13 176.6(3) . . . . ? C41 N12 C12 C11 -169.9(3) . . . . ? Al N12 C12 C11 -4.3(4) . . . . ? C16 C11 C12 C13 -3.7(5) . . . . ? N11 C11 C12 C13 -179.8(3) . . . . ? C16 C11 C12 N12 177.1(3) . . . . ? N11 C11 C12 N12 1.0(4) . . . . ? N12 C12 C13 F13 1.0(6) . . . . ? C11 C12 C13 F13 -178.1(3) . . . . ? N12 C12 C13 C14 -178.5(4) . . . . ? C11 C12 C13 C14 2.4(6) . . . . ? F13 C13 C14 F14 -0.3(5) . . . . ? C12 C13 C14 F14 179.2(3) . . . . ? F13 C13 C14 C15 -179.7(3) . . . . ? C12 C13 C14 C15 -0.1(6) . . . . ? F14 C14 C15 F15 -3.3(6) . . . . ? C13 C14 C15 F15 176.1(3) . . . . ? F14 C14 C15 C16 179.8(4) . . . . ? C13 C14 C15 C16 -0.8(6) . . . . ? F15 C15 C16 F16 0.1(6) . . . . ? C14 C15 C16 F16 177.0(3) . . . . ? F15 C15 C16 C11 -177.5(3) . . . . ? C14 C15 C16 C11 -0.6(6) . . . . ? N11 C11 C16 F16 1.0(6) . . . . ? C12 C11 C16 F16 -174.6(3) . . . . ? N11 C11 C16 C15 178.4(4) . . . . ? C12 C11 C16 C15 2.9(6) . . . . ? C51 N21 C21 C26 16.2(6) . . . . ? Al N21 C21 C26 -176.8(3) . . . . ? C51 N21 C21 C22 -164.6(3) . . . . ? Al N21 C21 C22 2.4(4) . . . . ? C61 N22 C22 C23 9.5(6) . . . . ? Al N22 C22 C23 179.9(3) . . . . ? C61 N22 C22 C21 -172.5(3) . . . . ? Al N22 C22 C21 -2.2(4) . . . . ? C26 C21 C22 C23 -2.7(5) . . . . ? N21 C21 C22 C23 178.0(3) . . . . ? C26 C21 C22 N22 179.1(3) . . . . ? N21 C21 C22 N22 -0.1(5) . . . . ? N22 C22 C23 F23 3.2(6) . . . . ? C21 C22 C23 F23 -174.7(3) . . . . ? N22 C22 C23 C24 179.8(3) . . . . ? C21 C22 C23 C24 1.9(6) . . . . ? F23 C23 C24 F24 -2.5(5) . . . . ? C22 C23 C24 F24 -179.2(3) . . . . ? F23 C23 C24 C25 176.3(3) . . . . ? C22 C23 C24 C25 -0.5(6) . . . . ? F24 C24 C25 F25 -1.9(6) . . . . ? C23 C24 C25 F25 179.3(3) . . . . ? F24 C24 C25 C26 178.6(4) . . . . ? C23 C24 C25 C26 -0.2(6) . . . . ? F25 C25 C26 F26 -0.6(6) . . . . ? C24 C25 C26 F26 178.9(4) . . . . ? F25 C25 C26 C21 179.8(4) . . . . ? C24 C25 C26 C21 -0.7(7) . . . . ? N21 C21 C26 F26 1.7(7) . . . . ? C22 C21 C26 F26 -177.4(3) . . . . ? N21 C21 C26 C25 -178.7(4) . . . . ? C22 C21 C26 C25 2.2(6) . . . . ? C11 N11 C31 C32 -132.5(4) . . . . ? Al N11 C31 C32 59.0(5) . . . . ? C11 N11 C31 C36 53.3(5) . . . . ? Al N11 C31 C36 -115.2(4) . . . . ? C36 C31 C32 F32 177.1(3) . . . . ? N11 C31 C32 F32 2.4(6) . . . . ? C36 C31 C32 C33 -2.4(6) . . . . ? N11 C31 C32 C33 -177.1(4) . . . . ? F32 C32 C33 F33 0.1(6) . . . . ? C31 C32 C33 F33 179.6(4) . . . . ? F32 C32 C33 C34 -178.9(4) . . . . ? C31 C32 C33 C34 0.6(6) . . . . ? F33 C33 C34 F34 2.4(6) . . . . ? C32 C33 C34 F34 -178.7(4) . . . . ? F33 C33 C34 C35 -178.0(4) . . . . ? C32 C33 C34 C35 1.0(6) . . . . ? F34 C34 C35 F35 -2.9(6) . . . . ? C33 C34 C35 F35 177.5(4) . . . . ? F34 C34 C35 C36 179.0(4) . . . . ? C33 C34 C35 C36 -0.6(6) . . . . ? F35 C35 C36 F36 0.5(6) . . . . ? C34 C35 C36 F36 178.6(4) . . . . ? F35 C35 C36 C31 -179.4(3) . . . . ? C34 C35 C36 C31 -1.3(6) . . . . ? C32 C31 C36 F36 -177.2(3) . . . . ? N11 C31 C36 F36 -2.7(6) . . . . ? C32 C31 C36 C35 2.7(6) . . . . ? N11 C31 C36 C35 177.2(4) . . . . ? C12 N12 C41 C42 -128.5(4) . . . . ? Al N12 C41 C42 67.9(5) . . . . ? C12 N12 C41 C46 55.5(5) . . . . ? Al N12 C41 C46 -108.0(4) . . . . ? C46 C41 C42 F42 -179.6(4) . . . . ? N12 C41 C42 F42 4.1(6) . . . . ? C46 C41 C42 C43 -0.7(6) . . . . ? N12 C41 C42 C43 -177.0(4) . . . . ? F42 C42 C43 F43 0.8(7) . . . . ? C41 C42 C43 F43 -178.0(4) . . . . ? F42 C42 C43 C44 179.0(4) . . . . ? C41 C42 C43 C44 0.2(7) . . . . ? F43 C43 C44 F44 -1.4(7) . . . . ? C42 C43 C44 F44 -179.5(4) . . . . ? F43 C43 C44 C45 177.9(4) . . . . ? C42 C43 C44 C45 -0.2(7) . . . . ? F44 C44 C45 F45 -1.3(7) . . . . ? C43 C44 C45 F45 179.3(4) . . . . ? F44 C44 C45 C46 -179.7(4) . . . . ? C43 C44 C45 C46 0.9(7) . . . . ? F45 C45 C46 F46 0.4(6) . . . . ? C44 C45 C46 F46 178.8(4) . . . . ? F45 C45 C46 C41 180.0(4) . . . . ? C44 C45 C46 C41 -1.6(7) . . . . ? C42 C41 C46 F46 -178.9(4) . . . . ? N12 C41 C46 F46 -2.7(6) . . . . ? C42 C41 C46 C45 1.5(6) . . . . ? N12 C41 C46 C45 177.7(4) . . . . ? C21 N21 C51 C52 -126.6(4) . . . . ? Al N21 C51 C52 68.3(5) . . . . ? C21 N21 C51 C56 58.4(5) . . . . ? Al N21 C51 C56 -106.7(4) . . . . ? C56 C51 C52 F52 179.7(4) . . . . ? N21 C51 C52 F52 4.4(6) . . . . ? C56 C51 C52 C53 1.0(6) . . . . ? N21 C51 C52 C53 -174.3(4) . . . . ? F52 C52 C53 F53 0.5(6) . . . . ? C51 C52 C53 F53 179.2(4) . . . . ? F52 C52 C53 C54 -179.2(4) . . . . ? C51 C52 C53 C54 -0.5(7) . . . . ? F53 C53 C54 F54 -1.1(6) . . . . ? C52 C53 C54 F54 178.6(4) . . . . ? F53 C53 C54 C55 -180.0(4) . . . . ? C52 C53 C54 C55 -0.3(6) . . . . ? F54 C54 C55 F55 -0.8(6) . . . . ? C53 C54 C55 F55 178.0(4) . . . . ? F54 C54 C55 C56 -178.3(4) . . . . ? C53 C54 C55 C56 0.5(7) . . . . ? F55 C55 C56 F56 0.6(6) . . . . ? C54 C55 C56 F56 178.1(4) . . . . ? F55 C55 C56 C51 -177.5(4) . . . . ? C54 C55 C56 C51 0.0(7) . . . . ? C52 C51 C56 F56 -178.8(4) . . . . ? N21 C51 C56 F56 -3.6(6) . . . . ? C52 C51 C56 C55 -0.8(6) . . . . ? N21 C51 C56 C55 174.4(4) . . . . ? C22 N22 C61 C62 49.2(5) . . . . ? Al N22 C61 C62 -120.0(4) . . . . ? C22 N22 C61 C66 -138.2(4) . . . . ? Al N22 C61 C66 52.6(4) . . . . ? C66 C61 C62 F62 -174.4(3) . . . . ? N22 C61 C62 F62 -1.5(6) . . . . ? C66 C61 C62 C63 3.4(6) . . . . ? N22 C61 C62 C63 176.4(4) . . . . ? F62 C62 C63 F63 -3.4(6) . . . . ? C61 C62 C63 F63 178.7(4) . . . . ? F62 C62 C63 C64 175.5(4) . . . . ? C61 C62 C63 C64 -2.4(7) . . . . ? F63 C63 C64 F64 -0.7(7) . . . . ? C62 C63 C64 F64 -179.6(4) . . . . ? F63 C63 C64 C65 179.3(4) . . . . ? C62 C63 C64 C65 0.3(7) . . . . ? F64 C64 C65 F65 0.8(7) . . . . ? C63 C64 C65 F65 -179.2(4) . . . . ? F64 C64 C65 C66 -179.7(4) . . . . ? C63 C64 C65 C66 0.3(7) . . . . ? F65 C65 C66 F66 1.5(6) . . . . ? C64 C65 C66 F66 -178.0(4) . . . . ? F65 C65 C66 C61 -179.5(4) . . . . ? C64 C65 C66 C61 1.0(7) . . . . ? C62 C61 C66 F66 176.2(3) . . . . ? N22 C61 C66 F66 2.7(5) . . . . ? C62 C61 C66 C65 -2.8(6) . . . . ? N22 C61 C66 C65 -176.3(4) . . . . ? C91 C70 C71 C76 39.1(6) . . . . ? C81 C70 C71 C76 -142.2(4) . . . . ? C91 C70 C71 C72 -138.0(4) . . . . ? C81 C70 C71 C72 40.6(6) . . . . ? C76 C71 C72 C73 0.3(7) . . . . ? C70 C71 C72 C73 177.5(4) . . . . ? C71 C72 C73 C74 1.9(7) . . . . ? C72 C73 C74 C75 -1.4(8) . . . . ? C73 C74 C75 C76 -1.4(8) . . . . ? C74 C75 C76 C71 3.6(7) . . . . ? C72 C71 C76 C75 -3.0(7) . . . . ? C70 C71 C76 C75 179.8(4) . . . . ? C91 C70 C81 C86 -151.8(4) . . . . ? C71 C70 C81 C86 29.6(6) . . . . ? C91 C70 C81 C82 28.5(6) . . . . ? C71 C70 C81 C82 -150.1(4) . . . . ? C86 C81 C82 C83 0.5(6) . . . . ? C70 C81 C82 C83 -179.9(4) . . . . ? C81 C82 C83 C84 -0.2(7) . . . . ? C82 C83 C84 C85 0.1(8) . . . . ? C83 C84 C85 C86 -0.4(7) . . . . ? C84 C85 C86 C81 0.7(7) . . . . ? C82 C81 C86 C85 -0.7(6) . . . . ? C70 C81 C86 C85 179.6(4) . . . . ? C81 C70 C91 C92 -148.5(4) . . . . ? C71 C70 C91 C92 30.1(6) . . . . ? C81 C70 C91 C96 27.0(6) . . . . ? C71 C70 C91 C96 -154.4(4) . . . . ? C96 C91 C92 C93 -1.0(6) . . . . ? C70 C91 C92 C93 174.7(4) . . . . ? C91 C92 C93 C94 -0.2(7) . . . . ? C92 C93 C94 C95 1.6(8) . . . . ? C93 C94 C95 C96 -1.9(8) . . . . ? C94 C95 C96 C91 0.6(7) . . . . ? C92 C91 C96 C95 0.8(6) . . . . ? C70 C91 C96 C95 -174.8(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.252 _refine_diff_density_min -0.217 _refine_diff_density_rms 0.055 # Attachment '- 3-TiR.cif' data_cal0808 _database_code_depnum_ccdc_archive 'CCDC 784058' #TrackingRef '- 3-TiR.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H65 N P Ti, C36 Al F28 N4, 0.5(C6 H5 Br)' _chemical_formula_sum 'C73 H67.5 Al Br0.5 F28 N5 P Ti' _chemical_formula_weight 1692.63 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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.0945(9) _cell_length_b 27.1642(18) _cell_length_c 20.8704(14) _cell_angle_alpha 90.00 _cell_angle_beta 98.0151(10) _cell_angle_gamma 90.00 _cell_volume 7351.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 7296 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 25.85 _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.529 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3440 _exptl_absorpt_coefficient_mu 0.540 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8011 _exptl_absorpt_correction_T_max 0.8462 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 56778 _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_sigmaI/netI 0.0266 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 26.40 _reflns_number_total 15082 _reflns_number_gt 11369 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1997)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1997)' _computing_data_reduction 'Bruker SAINT (Bruker, 1997)' _computing_structure_solution 'DIRDIF-96 (Beurskens et al., 1996)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1997)' _computing_publication_material 'Bruker SHELXTL (Bruker, 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^)+(0.0893P)^2^+7.2549P] 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 15082 _refine_ls_number_parameters 1005 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0762 _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.1683 _refine_ls_wR_factor_gt 0.1522 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.033 _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 Ti Ti 0.00645(4) 0.174334(17) 0.28608(2) 0.02860(13) Uani 1 1 d . . . P P 0.18160(6) 0.13984(3) 0.18825(3) 0.03100(16) Uani 1 1 d . . . N1 N 0.10470(18) 0.15593(8) 0.23889(11) 0.0314(5) Uani 1 1 d . . . C1 C -0.1268(3) 0.14598(13) 0.22642(17) 0.0461(8) Uani 1 1 d . . . H1A H -0.1783 0.1717 0.2116 0.055 Uiso 1 1 calc R . . H1B H -0.1096 0.1266 0.1892 0.055 Uiso 1 1 calc R . . C2 C -0.1582(2) 0.11384(11) 0.28070(16) 0.0410(7) Uani 1 1 d . . . H2 H -0.1888 0.1362 0.3110 0.049 Uiso 1 1 calc R . . C3 C -0.0632(2) 0.09200(12) 0.31750(16) 0.0409(7) Uani 1 1 d . . . H3 H -0.0350 0.0623 0.2977 0.049 Uiso 1 1 calc R . . C4 C -0.0206(3) 0.10293(12) 0.37776(15) 0.0428(7) Uani 1 1 d . . . H4 H -0.0485 0.1306 0.3970 0.051 Uiso 1 1 calc R . . C5 C 0.0676(3) 0.07624(14) 0.41937(18) 0.0562(9) Uani 1 1 d . . . C6 C 0.0357(3) 0.06886(16) 0.48595(18) 0.0623(10) Uani 1 1 d . . . H6A H 0.0899 0.0508 0.5135 0.075 Uiso 1 1 calc R . . H6B H -0.0287 0.0500 0.4819 0.075 Uiso 1 1 calc R . . H6C H 0.0254 0.1010 0.5054 0.075 Uiso 1 1 calc R . . C7 C 0.0892(3) 0.02655(14) 0.3905(2) 0.0612(10) Uani 1 1 d . . . H7A H 0.1453 0.0101 0.4185 0.073 Uiso 1 1 calc R . . H7B H 0.1092 0.0314 0.3474 0.073 Uiso 1 1 calc R . . H7C H 0.0270 0.0061 0.3870 0.073 Uiso 1 1 calc R . . C8 C 0.1642(3) 0.10908(17) 0.4259(2) 0.0689(11) Uani 1 1 d . . . H8A H 0.2216 0.0920 0.4519 0.083 Uiso 1 1 calc R . . H8B H 0.1501 0.1400 0.4471 0.083 Uiso 1 1 calc R . . H8C H 0.1824 0.1161 0.3829 0.083 Uiso 1 1 calc R . . C9 C -0.2407(3) 0.07427(15) 0.2575(2) 0.0584(9) Uani 1 1 d . . . C10 C -0.2048(3) 0.03964(15) 0.2073(2) 0.0628(10) Uani 1 1 d . . . H10A H -0.1395 0.0242 0.2255 0.075 Uiso 1 1 calc R . . H10B H -0.1949 0.0584 0.1686 0.075 Uiso 1 1 calc R . . H10C H -0.2570 0.0141 0.1958 0.075 Uiso 1 1 calc R . . C11 C -0.2638(4) 0.04404(18) 0.3168(2) 0.0800(14) Uani 1 1 d . . . H11A H -0.2007 0.0276 0.3367 0.096 Uiso 1 1 calc R . . H11B H -0.3167 0.0193 0.3028 0.096 Uiso 1 1 calc R . . H11C H -0.2887 0.0661 0.3484 0.096 Uiso 1 1 calc R . . C12 C -0.3390(3) 0.09927(18) 0.2292(3) 0.0868(16) Uani 1 1 d . . . H12A H -0.3915 0.0744 0.2151 0.104 Uiso 1 1 calc R . . H12B H -0.3265 0.1194 0.1921 0.104 Uiso 1 1 calc R . . H12C H -0.3632 0.1204 0.2621 0.104 Uiso 1 1 calc R . . C20 C -0.1228(2) 0.23433(10) 0.31594(14) 0.0327(6) Uani 1 1 d . . . C21 C -0.0704(2) 0.25407(10) 0.26675(15) 0.0361(6) Uani 1 1 d . . . C22 C 0.0354(2) 0.25975(10) 0.29305(15) 0.0376(7) Uani 1 1 d . . . C23 C 0.0481(2) 0.24189(11) 0.35760(15) 0.0370(6) Uani 1 1 d . . . C24 C -0.0502(2) 0.22707(11) 0.37192(14) 0.0348(6) Uani 1 1 d . . . C25 C -0.2376(2) 0.22916(12) 0.31093(17) 0.0441(7) Uani 1 1 d . . . H25A H -0.2694 0.2619 0.3082 0.053 Uiso 1 1 calc R . . H25B H -0.2550 0.2120 0.3493 0.053 Uiso 1 1 calc R . . H25C H -0.2634 0.2102 0.2721 0.053 Uiso 1 1 calc R . . C26 C -0.1203(3) 0.27296(13) 0.20264(17) 0.0503(8) Uani 1 1 d . . . H26A H -0.1560 0.2459 0.1778 0.060 Uiso 1 1 calc R . . H26B H -0.0674 0.2866 0.1788 0.060 Uiso 1 1 calc R . . H26C H -0.1700 0.2988 0.2093 0.060 Uiso 1 1 calc R . . C27 C 0.1139(3) 0.28902(13) 0.2639(2) 0.0548(9) Uani 1 1 d . . . H27A H 0.1101 0.3236 0.2768 0.066 Uiso 1 1 calc R . . H27B H 0.1002 0.2865 0.2166 0.066 Uiso 1 1 calc R . . H27C H 0.1829 0.2761 0.2791 0.066 Uiso 1 1 calc R . . C28 C 0.1456(3) 0.24647(15) 0.40521(18) 0.0543(9) Uani 1 1 d . . . H28A H 0.1328 0.2346 0.4477 0.065 Uiso 1 1 calc R . . H28B H 0.1669 0.2811 0.4086 0.065 Uiso 1 1 calc R . . H28C H 0.2003 0.2267 0.3902 0.065 Uiso 1 1 calc R . . C29 C -0.0759(3) 0.21466(13) 0.43796(15) 0.0468(8) Uani 1 1 d . . . H29A H -0.0169 0.1981 0.4631 0.056 Uiso 1 1 calc R . . H29B H -0.1360 0.1928 0.4337 0.056 Uiso 1 1 calc R . . H29C H -0.0916 0.2450 0.4601 0.056 Uiso 1 1 calc R . . C30 C 0.1928(2) 0.07037(11) 0.18917(15) 0.0399(7) Uani 1 1 d . . . C31 C 0.0856(3) 0.04777(12) 0.18895(18) 0.0479(8) Uani 1 1 d . . . H31A H 0.0409 0.0575 0.1493 0.058 Uiso 1 1 calc R . . H31B H 0.0559 0.0595 0.2267 0.058 Uiso 1 1 calc R . . H31C H 0.0913 0.0118 0.1906 0.058 Uiso 1 1 calc R . . C32 C 0.2404(3) 0.04867(14) 0.1317(2) 0.0570(9) Uani 1 1 d . . . H32A H 0.1996 0.0591 0.0910 0.068 Uiso 1 1 calc R . . H32B H 0.2402 0.0127 0.1343 0.068 Uiso 1 1 calc R . . H32C H 0.3114 0.0605 0.1332 0.068 Uiso 1 1 calc R . . C33 C 0.2582(3) 0.05355(13) 0.25200(18) 0.0532(9) Uani 1 1 d . . . H33A H 0.3276 0.0676 0.2545 0.064 Uiso 1 1 calc R . . H33B H 0.2628 0.0175 0.2525 0.064 Uiso 1 1 calc R . . H33C H 0.2261 0.0648 0.2891 0.064 Uiso 1 1 calc R . . C34 C 0.3134(2) 0.16801(12) 0.21327(16) 0.0423(7) Uani 1 1 d . . . C35 C 0.3150(3) 0.22240(14) 0.1936(2) 0.0564(9) Uani 1 1 d . . . H35A H 0.2611 0.2403 0.2121 0.068 Uiso 1 1 calc R . . H35B H 0.3026 0.2250 0.1463 0.068 Uiso 1 1 calc R . . H35C H 0.3825 0.2366 0.2097 0.068 Uiso 1 1 calc R . . C36 C 0.4009(3) 0.14235(15) 0.1839(2) 0.0599(10) Uani 1 1 d . . . H36A H 0.3854 0.1428 0.1366 0.072 Uiso 1 1 calc R . . H36B H 0.4071 0.1082 0.1990 0.072 Uiso 1 1 calc R . . H36C H 0.4660 0.1597 0.1974 0.072 Uiso 1 1 calc R . . C37 C 0.3373(3) 0.16723(15) 0.28716(18) 0.0570(9) Uani 1 1 d . . . H37A H 0.2817 0.1838 0.3057 0.068 Uiso 1 1 calc R . . H37B H 0.4025 0.1844 0.3008 0.068 Uiso 1 1 calc R . . H37C H 0.3429 0.1331 0.3023 0.068 Uiso 1 1 calc R . . C38 C 0.1255(3) 0.16145(13) 0.10491(15) 0.0437(7) Uani 1 1 d . . . C39 C 0.0845(3) 0.21388(13) 0.10971(18) 0.0556(9) Uani 1 1 d . . . H39A H 0.1414 0.2358 0.1265 0.067 Uiso 1 1 calc R . . H39B H 0.0322 0.2143 0.1390 0.067 Uiso 1 1 calc R . . H39C H 0.0536 0.2251 0.0667 0.067 Uiso 1 1 calc R . . C40 C 0.2023(4) 0.16025(17) 0.05543(18) 0.0653(11) Uani 1 1 d . . . H40A H 0.2275 0.1266 0.0516 0.078 Uiso 1 1 calc R . . H40B H 0.2605 0.1821 0.0699 0.078 Uiso 1 1 calc R . . H40C H 0.1677 0.1713 0.0132 0.078 Uiso 1 1 calc R . . C41 C 0.0317(3) 0.12959(15) 0.07851(17) 0.0558(9) Uani 1 1 d . . . H41A H 0.0537 0.0954 0.0748 0.067 Uiso 1 1 calc R . . H41B H 0.0018 0.1418 0.0358 0.067 Uiso 1 1 calc R . . H41C H -0.0200 0.1314 0.1082 0.067 Uiso 1 1 calc R . . Al Al 0.54920(6) 0.37630(3) 0.22590(4) 0.02782(18) Uani 1 1 d . . . F53 F 0.20906(13) 0.43140(7) 0.23493(9) 0.0450(4) Uani 1 1 d . . . F54 F 0.06536(13) 0.39151(8) 0.14581(10) 0.0557(5) Uani 1 1 d . . . F55 F 0.12027(15) 0.32489(8) 0.05916(10) 0.0536(5) Uani 1 1 d . . . F56 F 0.31833(14) 0.29956(7) 0.06042(9) 0.0467(4) Uani 1 1 d . . . F63 F 0.79634(13) 0.32846(6) 0.40209(8) 0.0382(4) Uani 1 1 d . . . F64 F 0.99019(13) 0.35631(7) 0.39277(9) 0.0457(4) Uani 1 1 d . . . F65 F 1.03063(13) 0.41338(7) 0.29134(9) 0.0482(5) Uani 1 1 d . . . F66 F 0.87907(13) 0.43805(6) 0.19709(9) 0.0410(4) Uani 1 1 d . . . F72 F 0.59492(17) 0.25783(9) 0.17657(11) 0.0649(6) Uani 1 1 d . . . F73 F 0.6947(2) 0.21783(13) 0.08509(17) 0.1076(12) Uani 1 1 d . . . F74 F 0.6785(2) 0.25969(15) -0.03460(16) 0.1248(15) Uani 1 1 d . . . F75 F 0.5578(3) 0.34012(15) -0.06149(12) 0.1282(15) Uani 1 1 d . . . F76 F 0.4579(2) 0.38039(10) 0.03060(11) 0.0789(8) Uani 1 1 d . . . F82 F 0.52682(14) 0.48679(7) 0.28514(9) 0.0455(4) Uani 1 1 d . . . F83 F 0.50818(16) 0.52960(8) 0.39777(10) 0.0570(5) Uani 1 1 d . . . F84 F 0.38348(17) 0.48956(10) 0.47836(9) 0.0670(6) Uani 1 1 d . . . F85 F 0.27735(17) 0.40539(10) 0.44194(10) 0.0691(6) Uani 1 1 d . . . F86 F 0.29544(15) 0.36231(7) 0.32834(10) 0.0514(5) Uani 1 1 d . . . F92 F 0.56367(15) 0.48975(7) 0.16016(9) 0.0488(5) Uani 1 1 d . . . F93 F 0.57074(19) 0.52886(8) 0.04328(11) 0.0664(6) Uani 1 1 d . . . F94 F 0.6790(2) 0.48384(11) -0.04188(11) 0.0795(7) Uani 1 1 d . . . F95 F 0.78303(19) 0.39894(10) -0.00692(11) 0.0732(7) Uani 1 1 d . . . F96 F 0.78209(15) 0.36105(7) 0.11196(10) 0.0510(5) Uani 1 1 d . . . F102 F 0.49685(15) 0.27822(8) 0.30718(9) 0.0538(5) Uani 1 1 d . . . F103 F 0.40480(17) 0.25763(9) 0.41157(12) 0.0696(6) Uani 1 1 d . . . F104 F 0.44590(19) 0.31285(10) 0.52100(11) 0.0754(7) Uani 1 1 d . . . F105 F 0.5795(2) 0.38988(10) 0.52345(10) 0.0740(7) Uani 1 1 d . . . F106 F 0.66639(15) 0.41244(7) 0.41792(9) 0.0500(5) Uani 1 1 d . . . N51 N 0.47803(18) 0.34245(9) 0.15686(11) 0.0326(5) Uani 1 1 d . . . N52 N 0.42473(17) 0.40161(9) 0.24290(11) 0.0308(5) Uani 1 1 d . . . N61 N 0.66704(17) 0.40429(9) 0.20240(11) 0.0301(5) Uani 1 1 d . . . N62 N 0.62753(17) 0.35669(8) 0.30249(11) 0.0291(5) Uani 1 1 d . . . C51 C 0.3716(2) 0.35230(10) 0.15017(13) 0.0318(6) Uani 1 1 d . . . C52 C 0.3420(2) 0.38482(10) 0.19733(13) 0.0317(6) Uani 1 1 d . . . C53 C 0.2393(2) 0.39811(11) 0.19370(14) 0.0356(6) Uani 1 1 d . . . C54 C 0.1648(2) 0.37849(12) 0.14713(15) 0.0406(7) Uani 1 1 d . . . C55 C 0.1924(2) 0.34563(12) 0.10328(15) 0.0401(7) Uani 1 1 d . . . C56 C 0.2950(2) 0.33266(11) 0.10471(14) 0.0370(7) Uani 1 1 d . . . C61 C 0.7537(2) 0.39547(10) 0.24833(13) 0.0283(5) Uani 1 1 d . . . C62 C 0.7321(2) 0.36891(10) 0.30367(13) 0.0280(5) Uani 1 1 d . . . C63 C 0.8130(2) 0.35552(10) 0.35028(13) 0.0311(6) Uani 1 1 d . . . C64 C 0.9136(2) 0.36967(11) 0.34603(14) 0.0341(6) Uani 1 1 d . . . C65 C 0.9333(2) 0.39751(11) 0.29476(15) 0.0354(6) Uani 1 1 d . . . C66 C 0.8549(2) 0.41020(10) 0.24660(14) 0.0319(6) Uani 1 1 d . . . C71 C 0.5228(2) 0.32056(12) 0.10650(14) 0.0385(7) Uani 1 1 d . . . C72 C 0.5846(2) 0.27912(14) 0.11818(17) 0.0496(8) Uani 1 1 d . . . C73 C 0.6367(3) 0.25850(18) 0.0714(2) 0.0707(13) Uani 1 1 d . . . C74 C 0.6282(4) 0.2785(2) 0.0115(2) 0.0814(17) Uani 1 1 d . . . C75 C 0.5676(4) 0.3190(2) -0.00299(19) 0.0787(16) Uani 1 1 d . . . C76 C 0.5150(3) 0.34009(15) 0.04430(17) 0.0564(10) Uani 1 1 d . . . C81 C 0.4088(2) 0.42386(11) 0.30112(13) 0.0311(6) Uani 1 1 d . . . C82 C 0.4639(2) 0.46601(11) 0.32293(14) 0.0342(6) Uani 1 1 d . . . C83 C 0.4561(2) 0.48810(12) 0.38130(15) 0.0395(7) Uani 1 1 d . . . C84 C 0.3925(3) 0.46812(14) 0.42165(15) 0.0463(8) Uani 1 1 d . . . C85 C 0.3377(2) 0.42608(14) 0.40264(16) 0.0456(8) Uani 1 1 d . . . C86 C 0.3467(2) 0.40443(12) 0.34395(15) 0.0385(7) Uani 1 1 d . . . C91 C 0.6749(2) 0.42476(10) 0.14100(13) 0.0314(6) Uani 1 1 d . . . C92 C 0.6201(2) 0.46711(11) 0.12020(14) 0.0355(6) Uani 1 1 d . . . C93 C 0.6216(3) 0.48699(12) 0.05999(16) 0.0449(7) Uani 1 1 d . . . C94 C 0.6769(3) 0.46416(14) 0.01676(16) 0.0510(8) Uani 1 1 d . . . C95 C 0.7308(3) 0.42210(14) 0.03507(16) 0.0477(8) Uani 1 1 d . . . C96 C 0.7296(2) 0.40308(11) 0.09593(15) 0.0376(6) Uani 1 1 d . . . C101 C 0.5871(2) 0.34510(10) 0.35971(13) 0.0301(6) Uani 1 1 d . . . C102 C 0.5183(2) 0.30636(12) 0.36025(14) 0.0379(7) Uani 1 1 d . . . C103 C 0.4700(2) 0.29584(13) 0.41340(17) 0.0466(8) Uani 1 1 d . . . C104 C 0.4913(3) 0.32344(14) 0.46852(16) 0.0500(9) Uani 1 1 d . . . C105 C 0.5595(3) 0.36208(13) 0.47015(15) 0.0464(8) Uani 1 1 d . . . C106 C 0.6048(2) 0.37293(11) 0.41622(14) 0.0369(6) Uani 1 1 d . . . Br1S Br 0.15792(10) 0.53166(6) 0.47531(8) 0.0982(3) Uani 0.50 1 d PD A -1 C1S C 0.0320(4) 0.5087(3) 0.4979(5) 0.111(6) Uani 0.50 1 d PGD A -1 C2S C -0.0135(5) 0.4700(2) 0.4608(3) 0.074(4) Uani 0.50 1 d PG A -1 H2S H 0.0191 0.4569 0.4266 0.089 Uiso 0.50 1 calc PR A -1 C3S C -0.1066(5) 0.4505(2) 0.4737(3) 0.074(3) Uani 0.50 1 d PG A -1 H3S H -0.1377 0.4240 0.4483 0.089 Uiso 0.50 1 calc PR A -1 C4S C -0.1543(4) 0.4697(3) 0.5236(4) 0.0982(3) Uani 0.50 1 d PG A -1 H4S H -0.2179 0.4563 0.5324 0.118 Uiso 0.50 1 calc PR A -1 C5S C -0.1088(5) 0.5084(3) 0.5608(3) 0.079(3) Uani 0.50 1 d PG A -1 H5S H -0.1414 0.5215 0.5949 0.095 Uiso 0.50 1 calc PR A -1 C6S C -0.0157(5) 0.5279(2) 0.5479(4) 0.083(4) Uani 0.50 1 d PG A -1 H6S H 0.0154 0.5544 0.5732 0.100 Uiso 0.50 1 calc PR A -1 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 Ti 0.0308(3) 0.0251(2) 0.0307(3) -0.00099(19) 0.00721(19) 0.00230(19) P 0.0322(4) 0.0307(4) 0.0311(4) -0.0025(3) 0.0082(3) 0.0009(3) N1 0.0333(12) 0.0274(11) 0.0338(12) -0.0017(9) 0.0060(10) -0.0001(9) C1 0.0410(17) 0.0468(19) 0.0497(19) -0.0004(15) 0.0030(14) -0.0009(14) C2 0.0421(17) 0.0368(16) 0.0437(17) -0.0040(13) 0.0051(13) 0.0007(13) C3 0.0433(17) 0.0348(16) 0.0459(18) -0.0017(13) 0.0107(14) -0.0013(13) C4 0.0524(19) 0.0350(16) 0.0414(17) -0.0003(13) 0.0077(14) 0.0045(14) C5 0.066(2) 0.056(2) 0.0457(19) 0.0013(16) 0.0047(17) 0.0132(18) C6 0.081(3) 0.060(2) 0.044(2) 0.0054(17) 0.0033(19) 0.003(2) C7 0.075(3) 0.048(2) 0.059(2) 0.0055(17) 0.0049(19) 0.0211(19) C8 0.067(3) 0.074(3) 0.063(3) -0.006(2) 0.002(2) 0.000(2) C9 0.0434(19) 0.060(2) 0.071(3) -0.0088(19) 0.0055(17) -0.0064(17) C10 0.065(2) 0.055(2) 0.068(2) -0.0155(19) 0.0033(19) -0.0148(19) C11 0.086(3) 0.073(3) 0.088(3) -0.004(3) 0.037(3) -0.023(3) C12 0.046(2) 0.073(3) 0.136(5) -0.013(3) -0.006(3) -0.008(2) C20 0.0321(14) 0.0276(14) 0.0382(15) -0.0071(11) 0.0042(11) 0.0057(11) C21 0.0427(16) 0.0251(14) 0.0403(16) -0.0020(12) 0.0048(13) 0.0055(12) C22 0.0396(16) 0.0265(14) 0.0479(17) -0.0073(12) 0.0109(13) -0.0010(12) C23 0.0343(15) 0.0362(16) 0.0393(16) -0.0128(12) 0.0016(12) 0.0015(12) C24 0.0360(15) 0.0332(15) 0.0353(15) -0.0070(12) 0.0048(12) 0.0061(12) C25 0.0347(16) 0.0412(17) 0.056(2) -0.0074(15) 0.0044(14) 0.0059(13) C26 0.063(2) 0.0414(18) 0.0458(19) 0.0059(15) 0.0036(16) 0.0130(16) C27 0.061(2) 0.0360(17) 0.073(2) -0.0103(16) 0.0293(19) -0.0109(16) C28 0.0398(18) 0.064(2) 0.056(2) -0.0206(18) -0.0028(15) -0.0028(16) C29 0.056(2) 0.0496(19) 0.0358(16) -0.0056(14) 0.0112(14) 0.0137(16) C30 0.0454(17) 0.0299(15) 0.0456(17) -0.0037(13) 0.0110(14) 0.0047(13) C31 0.053(2) 0.0338(16) 0.059(2) -0.0050(15) 0.0137(16) -0.0034(14) C32 0.063(2) 0.0439(19) 0.068(2) -0.0143(17) 0.0236(19) 0.0095(17) C33 0.057(2) 0.0424(19) 0.060(2) 0.0078(16) 0.0067(17) 0.0088(16) C34 0.0324(15) 0.0470(18) 0.0486(18) -0.0040(14) 0.0097(13) -0.0047(13) C35 0.051(2) 0.049(2) 0.072(2) -0.0020(18) 0.0172(18) -0.0123(16) C36 0.0359(18) 0.068(2) 0.079(3) -0.004(2) 0.0199(18) -0.0022(17) C37 0.0439(19) 0.067(2) 0.057(2) -0.0100(18) -0.0034(16) -0.0097(17) C38 0.0523(19) 0.0491(19) 0.0306(15) 0.0009(13) 0.0090(13) 0.0048(15) C39 0.067(2) 0.050(2) 0.049(2) 0.0113(16) 0.0049(17) 0.0097(18) C40 0.083(3) 0.079(3) 0.0389(19) 0.0061(18) 0.0260(19) 0.008(2) C41 0.058(2) 0.070(2) 0.0367(17) -0.0022(16) -0.0026(15) 0.0017(18) Al 0.0248(4) 0.0324(4) 0.0263(4) -0.0007(3) 0.0035(3) -0.0025(3) F53 0.0293(9) 0.0531(11) 0.0526(11) -0.0050(9) 0.0054(8) 0.0047(8) F54 0.0270(9) 0.0757(14) 0.0613(12) 0.0063(10) -0.0052(8) 0.0009(9) F55 0.0443(11) 0.0593(12) 0.0505(11) 0.0019(9) -0.0173(9) -0.0127(9) F56 0.0507(11) 0.0467(10) 0.0394(10) -0.0094(8) -0.0051(8) -0.0069(8) F63 0.0397(9) 0.0413(9) 0.0324(8) 0.0058(7) 0.0008(7) 0.0027(7) F64 0.0331(9) 0.0548(11) 0.0457(10) -0.0024(8) -0.0069(8) 0.0060(8) F65 0.0260(8) 0.0586(12) 0.0604(12) -0.0034(9) 0.0078(8) -0.0071(8) F66 0.0345(9) 0.0435(10) 0.0467(10) 0.0086(8) 0.0119(7) -0.0064(7) F72 0.0608(13) 0.0715(15) 0.0587(13) -0.0058(11) -0.0043(10) 0.0247(11) F73 0.0608(15) 0.127(3) 0.132(3) -0.074(2) 0.0027(16) 0.0313(16) F74 0.089(2) 0.192(4) 0.108(2) -0.101(2) 0.0665(18) -0.064(2) F75 0.185(4) 0.167(3) 0.0409(14) -0.0126(17) 0.0457(18) -0.083(3) F76 0.122(2) 0.0674(16) 0.0446(12) 0.0180(11) 0.0030(13) -0.0202(15) F82 0.0446(10) 0.0512(11) 0.0428(10) -0.0090(8) 0.0139(8) -0.0184(8) F83 0.0595(12) 0.0615(13) 0.0495(11) -0.0229(10) 0.0057(9) -0.0103(10) F84 0.0630(13) 0.1036(18) 0.0364(10) -0.0177(11) 0.0141(9) 0.0074(12) F85 0.0641(14) 0.0986(18) 0.0508(12) 0.0145(12) 0.0303(11) -0.0079(12) F86 0.0482(11) 0.0509(11) 0.0565(12) 0.0089(9) 0.0119(9) -0.0139(9) F92 0.0524(11) 0.0492(11) 0.0447(10) 0.0006(8) 0.0065(8) 0.0157(9) F93 0.0820(16) 0.0540(13) 0.0604(13) 0.0225(10) -0.0007(11) 0.0145(11) F94 0.0963(18) 0.1023(19) 0.0433(12) 0.0309(12) 0.0216(12) 0.0037(15) F95 0.0792(16) 0.1001(19) 0.0473(12) -0.0013(12) 0.0334(11) 0.0125(14) F96 0.0551(11) 0.0483(11) 0.0526(11) 0.0023(9) 0.0177(9) 0.0125(9) F102 0.0556(12) 0.0569(12) 0.0484(11) -0.0084(9) 0.0059(9) -0.0265(10) F103 0.0540(13) 0.0783(15) 0.0791(15) 0.0249(13) 0.0184(11) -0.0235(11) F104 0.0749(15) 0.1063(19) 0.0542(13) 0.0286(13) 0.0409(12) 0.0218(14) F105 0.0999(18) 0.0858(17) 0.0393(11) -0.0176(11) 0.0208(12) 0.0149(14) F106 0.0574(12) 0.0435(10) 0.0496(11) -0.0154(9) 0.0088(9) -0.0071(9) N51 0.0313(12) 0.0387(13) 0.0274(11) -0.0030(10) 0.0030(9) -0.0019(10) N52 0.0260(11) 0.0350(12) 0.0312(12) -0.0029(10) 0.0030(9) -0.0028(9) N61 0.0260(11) 0.0349(12) 0.0295(12) 0.0036(9) 0.0045(9) -0.0005(9) N62 0.0263(11) 0.0328(12) 0.0283(11) 0.0015(9) 0.0043(9) -0.0026(9) C51 0.0321(14) 0.0323(14) 0.0298(14) 0.0043(11) -0.0001(11) -0.0044(11) C52 0.0285(13) 0.0324(14) 0.0336(14) 0.0036(11) 0.0016(11) -0.0056(11) C53 0.0303(14) 0.0385(16) 0.0371(15) 0.0045(12) 0.0016(12) -0.0022(12) C54 0.0270(14) 0.0482(18) 0.0449(17) 0.0113(14) -0.0010(12) -0.0034(13) C55 0.0360(16) 0.0416(17) 0.0386(16) 0.0084(13) -0.0093(13) -0.0093(13) C56 0.0426(17) 0.0359(16) 0.0304(14) 0.0044(12) -0.0024(12) -0.0074(12) C61 0.0279(13) 0.0257(13) 0.0317(14) -0.0026(10) 0.0052(11) 0.0006(10) C62 0.0269(13) 0.0257(13) 0.0315(13) -0.0041(10) 0.0040(10) -0.0005(10) C63 0.0338(14) 0.0286(14) 0.0310(14) -0.0022(11) 0.0050(11) 0.0009(11) C64 0.0281(14) 0.0346(15) 0.0374(15) -0.0063(12) -0.0032(11) 0.0058(11) C65 0.0230(13) 0.0347(15) 0.0488(17) -0.0097(13) 0.0066(12) -0.0025(11) C66 0.0310(14) 0.0288(14) 0.0374(15) -0.0018(11) 0.0105(11) -0.0016(11) C71 0.0380(16) 0.0478(18) 0.0304(15) -0.0087(13) 0.0074(12) -0.0128(13) C72 0.0354(17) 0.063(2) 0.050(2) -0.0213(17) 0.0059(14) -0.0030(15) C73 0.039(2) 0.092(3) 0.082(3) -0.050(3) 0.0139(19) -0.008(2) C74 0.063(3) 0.117(4) 0.072(3) -0.057(3) 0.037(2) -0.042(3) C75 0.098(4) 0.108(4) 0.035(2) -0.020(2) 0.028(2) -0.059(3) C76 0.072(3) 0.060(2) 0.0378(18) -0.0029(16) 0.0100(17) -0.024(2) C81 0.0249(13) 0.0377(15) 0.0305(14) 0.0019(11) 0.0033(11) 0.0027(11) C82 0.0292(14) 0.0423(16) 0.0316(14) -0.0008(12) 0.0057(11) 0.0005(12) C83 0.0329(15) 0.0481(18) 0.0364(15) -0.0061(13) 0.0009(12) 0.0025(13) C84 0.0406(17) 0.067(2) 0.0314(16) -0.0051(15) 0.0063(13) 0.0118(16) C85 0.0366(16) 0.064(2) 0.0389(17) 0.0133(15) 0.0153(13) 0.0062(15) C86 0.0322(15) 0.0421(17) 0.0415(16) 0.0063(13) 0.0060(12) 0.0009(12) C91 0.0294(14) 0.0343(14) 0.0306(14) 0.0028(11) 0.0044(11) -0.0066(11) C92 0.0344(15) 0.0369(16) 0.0349(15) -0.0007(12) 0.0037(12) -0.0015(12) C93 0.0473(18) 0.0420(18) 0.0437(17) 0.0110(14) -0.0001(14) -0.0007(14) C94 0.056(2) 0.063(2) 0.0343(17) 0.0162(16) 0.0070(15) -0.0064(17) C95 0.0457(18) 0.060(2) 0.0405(17) -0.0014(15) 0.0179(14) -0.0037(16) C96 0.0371(15) 0.0390(16) 0.0379(16) 0.0031(13) 0.0090(12) -0.0009(12) C101 0.0275(13) 0.0348(14) 0.0279(13) 0.0036(11) 0.0036(10) 0.0021(11) C102 0.0333(15) 0.0443(17) 0.0356(15) 0.0057(13) 0.0033(12) -0.0034(13) C103 0.0338(16) 0.055(2) 0.052(2) 0.0190(16) 0.0117(14) -0.0023(14) C104 0.0462(19) 0.069(2) 0.0398(18) 0.0169(16) 0.0218(15) 0.0163(17) C105 0.053(2) 0.057(2) 0.0307(15) -0.0012(14) 0.0087(14) 0.0149(16) C106 0.0364(15) 0.0385(16) 0.0361(15) -0.0023(12) 0.0055(12) 0.0033(12) Br1S 0.0718(6) 0.1005(8) 0.1173(8) 0.0260(7) -0.0045(6) -0.0063(5) C1S 0.210(18) 0.021(5) 0.077(6) 0.016(5) -0.070(9) -0.013(6) C2S 0.145(11) 0.035(6) 0.036(5) -0.018(5) -0.011(6) 0.010(6) C3S 0.081(6) 0.076(6) 0.062(5) -0.022(5) -0.005(5) 0.024(5) C4S 0.0718(6) 0.1005(8) 0.1173(8) 0.0260(7) -0.0045(6) -0.0063(5) C5S 0.080(7) 0.063(6) 0.091(7) -0.002(5) -0.003(5) 0.005(5) C6S 0.143(11) 0.055(8) 0.041(6) -0.013(5) -0.024(7) 0.041(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 Ti N1 1.797(2) . ? Ti C1 2.140(3) . ? Ti C22 2.352(3) . ? Ti C23 2.380(3) . ? Ti C21 2.399(3) . ? Ti C24 2.487(3) . ? Ti C20 2.491(3) . ? Ti C3 2.536(3) . ? P N1 1.618(2) . ? P C38 1.885(3) . ? P C30 1.893(3) . ? P C34 1.893(3) . ? C1 C2 1.531(5) . ? C2 C3 1.491(4) . ? C2 C9 1.553(5) . ? C3 C4 1.336(5) . ? C4 C5 1.527(5) . ? C5 C6 1.519(5) . ? C5 C7 1.521(5) . ? C5 C8 1.538(6) . ? C9 C12 1.501(6) . ? C9 C10 1.529(6) . ? C9 C11 1.551(6) . ? C20 C24 1.413(4) . ? C20 C21 1.417(4) . ? C20 C25 1.498(4) . ? C21 C22 1.426(4) . ? C21 C26 1.495(4) . ? C22 C23 1.420(4) . ? C22 C27 1.495(4) . ? C23 C24 1.420(4) . ? C23 C28 1.509(4) . ? C24 C29 1.502(4) . ? C30 C33 1.532(5) . ? C30 C31 1.532(5) . ? C30 C32 1.543(4) . ? C34 C37 1.530(5) . ? C34 C35 1.535(5) . ? C34 C36 1.540(5) . ? C38 C39 1.530(5) . ? C38 C40 1.538(5) . ? C38 C41 1.540(5) . ? Al N61 1.847(2) . ? Al N51 1.848(2) . ? Al N52 1.848(2) . ? Al N62 1.853(2) . ? F53 C53 1.345(3) . ? F54 C54 1.345(3) . ? F55 C55 1.347(3) . ? F56 C56 1.354(4) . ? F63 C63 1.350(3) . ? F64 C64 1.348(3) . ? F65 C65 1.357(3) . ? F66 C66 1.353(3) . ? F72 C72 1.339(4) . ? F73 C73 1.348(6) . ? F74 C74 1.341(5) . ? F75 C75 1.339(5) . ? F76 C76 1.334(5) . ? F82 C82 1.342(3) . ? F83 C83 1.338(4) . ? F84 C84 1.339(4) . ? F85 C85 1.339(4) . ? F86 C86 1.344(4) . ? F92 C92 1.338(3) . ? F93 C93 1.340(4) . ? F94 C94 1.339(4) . ? F95 C95 1.341(4) . ? F96 C96 1.350(4) . ? F102 C102 1.343(4) . ? F103 C103 1.341(4) . ? F104 C104 1.348(4) . ? F105 C105 1.340(4) . ? F106 C106 1.340(4) . ? N51 C71 1.405(4) . ? N51 C51 1.407(4) . ? N52 C81 1.399(4) . ? N52 C52 1.413(3) . ? N61 C61 1.400(3) . ? N61 C91 1.414(3) . ? N62 C62 1.406(3) . ? N62 C101 1.408(3) . ? C51 C56 1.387(4) . ? C51 C52 1.416(4) . ? C52 C53 1.385(4) . ? C53 C54 1.384(4) . ? C54 C55 1.363(5) . ? C55 C56 1.386(4) . ? C61 C66 1.390(4) . ? C61 C62 1.423(4) . ? C62 C63 1.383(4) . ? C63 C64 1.387(4) . ? C64 C65 1.364(4) . ? C65 C66 1.377(4) . ? C71 C72 1.388(5) . ? C71 C76 1.393(5) . ? C72 C73 1.385(5) . ? C73 C74 1.352(8) . ? C74 C75 1.367(8) . ? C75 C76 1.402(6) . ? C81 C86 1.393(4) . ? C81 C82 1.395(4) . ? C82 C83 1.375(4) . ? C83 C84 1.375(5) . ? C84 C85 1.377(5) . ? C85 C86 1.379(5) . ? C91 C96 1.390(4) . ? C91 C92 1.393(4) . ? C92 C93 1.370(4) . ? C93 C94 1.380(5) . ? C94 C95 1.369(5) . ? C95 C96 1.373(4) . ? C101 C102 1.387(4) . ? C101 C106 1.393(4) . ? C102 C103 1.381(4) . ? C103 C104 1.369(5) . ? C104 C105 1.376(5) . ? C105 C106 1.375(4) . ? Br1S C1S 1.883(3) . ? C1S C2S 1.3900 . ? C1S C6S 1.3900 . ? C2S C3S 1.3900 . ? C3S C4S 1.3900 . ? C4S C5S 1.3900 . ? C5S C6S 1.3900 . ? 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 Ti C1 99.72(12) . . ? N1 Ti C22 100.78(10) . . ? C1 Ti C22 120.13(12) . . ? N1 Ti C23 116.05(11) . . ? C1 Ti C23 137.65(12) . . ? C22 Ti C23 34.90(11) . . ? N1 Ti C21 118.35(11) . . ? C1 Ti C21 86.45(12) . . ? C22 Ti C21 34.91(10) . . ? C23 Ti C21 57.55(10) . . ? N1 Ti C24 149.73(10) . . ? C1 Ti C24 108.99(12) . . ? C22 Ti C24 56.55(10) . . ? C23 Ti C24 33.84(10) . . ? C21 Ti C24 55.98(10) . . ? N1 Ti C20 151.97(10) . . ? C1 Ti C20 81.59(12) . . ? C22 Ti C20 56.51(10) . . ? C23 Ti C20 56.15(10) . . ? C21 Ti C20 33.63(10) . . ? C24 Ti C20 32.99(9) . . ? N1 Ti C3 101.96(10) . . ? C1 Ti C3 62.59(12) . . ? C22 Ti C3 156.14(11) . . ? C23 Ti C3 125.24(11) . . ? C21 Ti C3 133.01(11) . . ? C24 Ti C3 99.64(10) . . ? C20 Ti C3 103.35(10) . . ? N1 P C38 108.70(14) . . ? N1 P C30 108.50(13) . . ? C38 P C30 109.85(15) . . ? N1 P C34 109.69(13) . . ? C38 P C34 110.58(15) . . ? C30 P C34 109.48(15) . . ? P N1 Ti 172.50(16) . . ? C2 C1 Ti 93.2(2) . . ? C3 C2 C1 108.5(3) . . ? C3 C2 C9 112.3(3) . . ? C1 C2 C9 114.2(3) . . ? C4 C3 C2 127.3(3) . . ? C4 C3 Ti 85.9(2) . . ? C2 C3 Ti 79.64(18) . . ? C3 C4 C5 127.8(3) . . ? C6 C5 C7 109.6(3) . . ? C6 C5 C4 107.5(3) . . ? C7 C5 C4 111.3(3) . . ? C6 C5 C8 108.8(3) . . ? C7 C5 C8 110.7(3) . . ? C4 C5 C8 108.8(3) . . ? C12 C9 C10 109.8(4) . . ? C12 C9 C11 107.5(4) . . ? C10 C9 C11 109.5(4) . . ? C12 C9 C2 109.3(3) . . ? C10 C9 C2 111.9(3) . . ? C11 C9 C2 108.8(3) . . ? C24 C20 C21 108.3(3) . . ? C24 C20 C25 126.7(3) . . ? C21 C20 C25 124.5(3) . . ? C24 C20 Ti 73.34(15) . . ? C21 C20 Ti 69.62(15) . . ? C25 C20 Ti 129.1(2) . . ? C20 C21 C22 107.7(3) . . ? C20 C21 C26 125.7(3) . . ? C22 C21 C26 125.9(3) . . ? C20 C21 Ti 76.75(16) . . ? C22 C21 Ti 70.76(16) . . ? C26 C21 Ti 125.5(2) . . ? C23 C22 C21 107.9(3) . . ? C23 C22 C27 124.9(3) . . ? C21 C22 C27 126.0(3) . . ? C23 C22 Ti 73.63(17) . . ? C21 C22 Ti 74.33(16) . . ? C27 C22 Ti 127.8(2) . . ? C22 C23 C24 107.8(3) . . ? C22 C23 C28 125.0(3) . . ? C24 C23 C28 126.4(3) . . ? C22 C23 Ti 71.46(16) . . ? C24 C23 Ti 77.18(16) . . ? C28 C23 Ti 125.1(2) . . ? C20 C24 C23 108.2(3) . . ? C20 C24 C29 125.4(3) . . ? C23 C24 C29 125.6(3) . . ? C20 C24 Ti 73.67(16) . . ? C23 C24 Ti 68.98(15) . . ? C29 C24 Ti 131.3(2) . . ? C33 C30 C31 106.6(3) . . ? C33 C30 C32 108.3(3) . . ? C31 C30 C32 108.3(3) . . ? C33 C30 P 109.8(2) . . ? C31 C30 P 109.2(2) . . ? C32 C30 P 114.3(2) . . ? C37 C34 C35 105.9(3) . . ? C37 C34 C36 109.6(3) . . ? C35 C34 C36 106.8(3) . . ? C37 C34 P 108.8(2) . . ? C35 C34 P 111.2(2) . . ? C36 C34 P 114.1(2) . . ? C39 C38 C40 109.4(3) . . ? C39 C38 C41 106.1(3) . . ? C40 C38 C41 108.1(3) . . ? C39 C38 P 108.9(2) . . ? C40 C38 P 113.9(3) . . ? C41 C38 P 110.1(2) . . ? N61 Al N51 110.30(11) . . ? N61 Al N52 133.60(11) . . ? N51 Al N52 88.42(11) . . ? N61 Al N62 87.99(10) . . ? N51 Al N62 133.46(11) . . ? N52 Al N62 109.77(11) . . ? C71 N51 C51 121.2(2) . . ? C71 N51 Al 125.18(19) . . ? C51 N51 Al 111.57(18) . . ? C81 N52 C52 122.1(2) . . ? C81 N52 Al 124.74(18) . . ? C52 N52 Al 111.36(18) . . ? C61 N61 C91 122.2(2) . . ? C61 N61 Al 112.02(17) . . ? C91 N61 Al 124.88(18) . . ? C62 N62 C101 121.2(2) . . ? C62 N62 Al 111.59(17) . . ? C101 N62 Al 124.59(18) . . ? C56 C51 N51 127.3(3) . . ? C56 C51 C52 118.3(3) . . ? N51 C51 C52 114.4(2) . . ? C53 C52 N52 126.9(3) . . ? C53 C52 C51 118.8(3) . . ? N52 C52 C51 114.3(2) . . ? F53 C53 C54 117.8(3) . . ? F53 C53 C52 120.7(3) . . ? C54 C53 C52 121.5(3) . . ? F54 C54 C55 120.3(3) . . ? F54 C54 C53 119.9(3) . . ? C55 C54 C53 119.8(3) . . ? F55 C55 C54 120.5(3) . . ? F55 C55 C56 119.6(3) . . ? C54 C55 C56 120.0(3) . . ? F56 C56 C55 117.7(3) . . ? F56 C56 C51 120.8(3) . . ? C55 C56 C51 121.5(3) . . ? C66 C61 N61 128.1(2) . . ? C66 C61 C62 117.7(2) . . ? N61 C61 C62 114.2(2) . . ? C63 C62 N62 126.8(2) . . ? C63 C62 C61 119.0(2) . . ? N62 C62 C61 114.1(2) . . ? F63 C63 C62 120.9(2) . . ? F63 C63 C64 117.6(2) . . ? C62 C63 C64 121.5(3) . . ? F64 C64 C65 121.0(3) . . ? F64 C64 C63 119.8(3) . . ? C65 C64 C63 119.3(3) . . ? F65 C65 C64 120.0(3) . . ? F65 C65 C66 119.5(3) . . ? C64 C65 C66 120.6(3) . . ? F66 C66 C65 117.9(2) . . ? F66 C66 C61 120.4(3) . . ? C65 C66 C61 121.7(3) . . ? C72 C71 C76 116.0(3) . . ? C72 C71 N51 120.4(3) . . ? C76 C71 N51 123.5(3) . . ? F72 C72 C73 118.0(4) . . ? F72 C72 C71 119.5(3) . . ? C73 C72 C71 122.5(4) . . ? F73 C73 C74 119.7(4) . . ? F73 C73 C72 120.0(5) . . ? C74 C73 C72 120.2(5) . . ? F74 C74 C73 121.7(6) . . ? F74 C74 C75 118.4(6) . . ? C73 C74 C75 119.9(4) . . ? F75 C75 C74 121.8(5) . . ? F75 C75 C76 118.2(6) . . ? C74 C75 C76 120.0(4) . . ? F76 C76 C71 118.6(3) . . ? F76 C76 C75 120.0(4) . . ? C71 C76 C75 121.4(4) . . ? C86 C81 C82 115.0(3) . . ? C86 C81 N52 124.4(3) . . ? C82 C81 N52 120.3(2) . . ? F82 C82 C83 117.7(3) . . ? F82 C82 C81 119.0(2) . . ? C83 C82 C81 123.2(3) . . ? F83 C83 C82 119.8(3) . . ? F83 C83 C84 120.4(3) . . ? C82 C83 C84 119.8(3) . . ? F84 C84 C83 120.3(3) . . ? F84 C84 C85 120.6(3) . . ? C83 C84 C85 119.1(3) . . ? F85 C85 C84 120.0(3) . . ? F85 C85 C86 119.7(3) . . ? C84 C85 C86 120.3(3) . . ? F86 C86 C85 118.5(3) . . ? F86 C86 C81 118.9(3) . . ? C85 C86 C81 122.6(3) . . ? C96 C91 C92 115.5(3) . . ? C96 C91 N61 123.8(3) . . ? C92 C91 N61 120.5(3) . . ? F92 C92 C93 118.1(3) . . ? F92 C92 C91 119.4(3) . . ? C93 C92 C91 122.6(3) . . ? F93 C93 C92 120.2(3) . . ? F93 C93 C94 119.9(3) . . ? C92 C93 C94 119.9(3) . . ? F94 C94 C95 120.8(3) . . ? F94 C94 C93 119.8(3) . . ? C95 C94 C93 119.3(3) . . ? F95 C95 C94 119.9(3) . . ? F95 C95 C96 120.0(3) . . ? C94 C95 C96 120.0(3) . . ? F96 C96 C95 118.4(3) . . ? F96 C96 C91 118.9(3) . . ? C95 C96 C91 122.7(3) . . ? C102 C101 C106 115.9(3) . . ? C102 C101 N62 119.9(3) . . ? C106 C101 N62 124.0(3) . . ? F102 C102 C103 118.6(3) . . ? F102 C102 C101 119.1(3) . . ? C103 C102 C101 122.3(3) . . ? F103 C103 C104 120.1(3) . . ? F103 C103 C102 119.9(3) . . ? C104 C103 C102 120.0(3) . . ? F104 C104 C103 120.3(3) . . ? F104 C104 C105 120.1(3) . . ? C103 C104 C105 119.6(3) . . ? F105 C105 C106 120.1(3) . . ? F105 C105 C104 120.1(3) . . ? C106 C105 C104 119.7(3) . . ? F106 C106 C105 118.5(3) . . ? F106 C106 C101 119.0(3) . . ? C105 C106 C101 122.5(3) . . ? C2S C1S C6S 120.0 . . ? C2S C1S Br1S 115.7(5) . . ? C6S C1S Br1S 124.3(5) . . ? C1S C2S C3S 120.0 . . ? C2S C3S C4S 120.0 . . ? C5S C4S C3S 120.0 . . ? C4S C5S C6S 120.0 . . ? C5S C6S C1S 120.0 . . ? 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 C38 P N1 Ti 21.1(12) . . . . ? C30 P N1 Ti -98.3(12) . . . . ? C34 P N1 Ti 142.1(12) . . . . ? C1 Ti N1 P 28.1(12) . . . . ? C22 Ti N1 P -95.4(12) . . . . ? C23 Ti N1 P -128.6(12) . . . . ? C21 Ti N1 P -63.2(12) . . . . ? C24 Ti N1 P -133.5(11) . . . . ? C20 Ti N1 P -62.3(13) . . . . ? C3 Ti N1 P 91.9(12) . . . . ? N1 Ti C1 C2 122.18(19) . . . . ? C22 Ti C1 C2 -129.23(18) . . . . ? C23 Ti C1 C2 -89.7(2) . . . . ? C21 Ti C1 C2 -119.7(2) . . . . ? C24 Ti C1 C2 -67.5(2) . . . . ? C20 Ti C1 C2 -86.18(19) . . . . ? C3 Ti C1 C2 23.67(17) . . . . ? Ti C1 C2 C3 -39.7(3) . . . . ? Ti C1 C2 C9 -165.9(2) . . . . ? C1 C2 C3 C4 109.9(4) . . . . ? C9 C2 C3 C4 -122.8(4) . . . . ? C1 C2 C3 Ti 33.2(2) . . . . ? C9 C2 C3 Ti 160.5(3) . . . . ? N1 Ti C3 C4 111.4(2) . . . . ? C1 Ti C3 C4 -153.8(2) . . . . ? C22 Ti C3 C4 -50.7(4) . . . . ? C23 Ti C3 C4 -23.0(2) . . . . ? C21 Ti C3 C4 -99.2(2) . . . . ? C24 Ti C3 C4 -47.3(2) . . . . ? C20 Ti C3 C4 -80.8(2) . . . . ? N1 Ti C3 C2 -119.59(18) . . . . ? C1 Ti C3 C2 -24.74(18) . . . . ? C22 Ti C3 C2 78.3(3) . . . . ? C23 Ti C3 C2 106.03(19) . . . . ? C21 Ti C3 C2 29.9(2) . . . . ? C24 Ti C3 C2 81.74(18) . . . . ? C20 Ti C3 C2 48.26(19) . . . . ? C2 C3 C4 C5 170.9(3) . . . . ? Ti C3 C4 C5 -115.4(4) . . . . ? C3 C4 C5 C6 -133.2(4) . . . . ? C3 C4 C5 C7 -13.1(5) . . . . ? C3 C4 C5 C8 109.2(4) . . . . ? C3 C2 C9 C12 172.1(4) . . . . ? C1 C2 C9 C12 -63.8(4) . . . . ? C3 C2 C9 C10 -66.1(4) . . . . ? C1 C2 C9 C10 58.0(4) . . . . ? C3 C2 C9 C11 55.0(4) . . . . ? C1 C2 C9 C11 179.1(3) . . . . ? N1 Ti C20 C24 -118.8(2) . . . . ? C1 Ti C20 C24 146.3(2) . . . . ? C22 Ti C20 C24 -78.78(19) . . . . ? C23 Ti C20 C24 -36.54(18) . . . . ? C21 Ti C20 C24 -117.4(3) . . . . ? C3 Ti C20 C24 87.17(18) . . . . ? N1 Ti C20 C21 -1.4(3) . . . . ? C1 Ti C20 C21 -96.28(19) . . . . ? C22 Ti C20 C21 38.66(17) . . . . ? C23 Ti C20 C21 80.90(19) . . . . ? C24 Ti C20 C21 117.4(3) . . . . ? C3 Ti C20 C21 -155.39(17) . . . . ? N1 Ti C20 C25 117.1(3) . . . . ? C1 Ti C20 C25 22.2(3) . . . . ? C22 Ti C20 C25 157.2(3) . . . . ? C23 Ti C20 C25 -160.6(3) . . . . ? C21 Ti C20 C25 118.5(3) . . . . ? C24 Ti C20 C25 -124.0(4) . . . . ? C3 Ti C20 C25 -36.9(3) . . . . ? C24 C20 C21 C22 -0.9(3) . . . . ? C25 C20 C21 C22 171.3(3) . . . . ? Ti C20 C21 C22 -64.48(19) . . . . ? C24 C20 C21 C26 -172.0(3) . . . . ? C25 C20 C21 C26 0.3(5) . . . . ? Ti C20 C21 C26 124.4(3) . . . . ? C24 C20 C21 Ti 63.58(19) . . . . ? C25 C20 C21 Ti -124.2(3) . . . . ? N1 Ti C21 C20 179.27(16) . . . . ? C1 Ti C21 C20 80.13(18) . . . . ? C22 Ti C21 C20 -114.4(2) . . . . ? C23 Ti C21 C20 -76.35(18) . . . . ? C24 Ti C21 C20 -35.66(16) . . . . ? C3 Ti C21 C20 33.6(2) . . . . ? N1 Ti C21 C22 -66.3(2) . . . . ? C1 Ti C21 C22 -165.43(19) . . . . ? C23 Ti C21 C22 38.08(17) . . . . ? C24 Ti C21 C22 78.77(19) . . . . ? C20 Ti C21 C22 114.4(2) . . . . ? C3 Ti C21 C22 148.08(18) . . . . ? N1 Ti C21 C26 54.6(3) . . . . ? C1 Ti C21 C26 -44.5(3) . . . . ? C22 Ti C21 C26 120.9(4) . . . . ? C23 Ti C21 C26 159.0(3) . . . . ? C24 Ti C21 C26 -160.3(3) . . . . ? C20 Ti C21 C26 -124.6(4) . . . . ? C3 Ti C21 C26 -91.0(3) . . . . ? C20 C21 C22 C23 2.0(3) . . . . ? C26 C21 C22 C23 173.0(3) . . . . ? Ti C21 C22 C23 -66.5(2) . . . . ? C20 C21 C22 C27 -165.8(3) . . . . ? C26 C21 C22 C27 5.3(5) . . . . ? Ti C21 C22 C27 125.7(3) . . . . ? C20 C21 C22 Ti 68.50(19) . . . . ? C26 C21 C22 Ti -120.4(3) . . . . ? N1 Ti C22 C23 -120.57(18) . . . . ? C1 Ti C22 C23 131.42(19) . . . . ? C21 Ti C22 C23 114.5(2) . . . . ? C24 Ti C22 C23 37.55(16) . . . . ? C20 Ti C22 C23 77.35(18) . . . . ? C3 Ti C22 C23 41.6(3) . . . . ? N1 Ti C22 C21 124.88(18) . . . . ? C1 Ti C22 C21 16.9(2) . . . . ? C23 Ti C22 C21 -114.5(2) . . . . ? C24 Ti C22 C21 -77.00(18) . . . . ? C20 Ti C22 C21 -37.20(16) . . . . ? C3 Ti C22 C21 -72.9(3) . . . . ? N1 Ti C22 C27 1.2(3) . . . . ? C1 Ti C22 C27 -106.8(3) . . . . ? C23 Ti C22 C27 121.7(4) . . . . ? C21 Ti C22 C27 -123.7(4) . . . . ? C24 Ti C22 C27 159.3(3) . . . . ? C20 Ti C22 C27 -160.9(3) . . . . ? C3 Ti C22 C27 163.4(3) . . . . ? C21 C22 C23 C24 -2.3(3) . . . . ? C27 C22 C23 C24 165.7(3) . . . . ? Ti C22 C23 C24 -69.3(2) . . . . ? C21 C22 C23 C28 -172.6(3) . . . . ? C27 C22 C23 C28 -4.7(5) . . . . ? Ti C22 C23 C28 120.4(3) . . . . ? C21 C22 C23 Ti 67.0(2) . . . . ? C27 C22 C23 Ti -125.1(3) . . . . ? N1 Ti C23 C22 70.30(19) . . . . ? C1 Ti C23 C22 -74.3(2) . . . . ? C21 Ti C23 C22 -38.09(17) . . . . ? C24 Ti C23 C22 -114.1(2) . . . . ? C20 Ti C23 C22 -78.48(18) . . . . ? C3 Ti C23 C22 -160.80(17) . . . . ? N1 Ti C23 C24 -175.63(17) . . . . ? C1 Ti C23 C24 39.7(3) . . . . ? C22 Ti C23 C24 114.1(2) . . . . ? C21 Ti C23 C24 75.98(18) . . . . ? C20 Ti C23 C24 35.59(16) . . . . ? C3 Ti C23 C24 -46.7(2) . . . . ? N1 Ti C23 C28 -49.9(3) . . . . ? C1 Ti C23 C28 165.4(3) . . . . ? C22 Ti C23 C28 -120.2(4) . . . . ? C21 Ti C23 C28 -158.3(3) . . . . ? C24 Ti C23 C28 125.7(4) . . . . ? C20 Ti C23 C28 161.3(3) . . . . ? C3 Ti C23 C28 79.0(3) . . . . ? C21 C20 C24 C23 -0.5(3) . . . . ? C25 C20 C24 C23 -172.5(3) . . . . ? Ti C20 C24 C23 60.7(2) . . . . ? C21 C20 C24 C29 169.4(3) . . . . ? C25 C20 C24 C29 -2.6(5) . . . . ? Ti C20 C24 C29 -129.4(3) . . . . ? C21 C20 C24 Ti -61.20(19) . . . . ? C25 C20 C24 Ti 126.8(3) . . . . ? C22 C23 C24 C20 1.7(3) . . . . ? C28 C23 C24 C20 171.9(3) . . . . ? Ti C23 C24 C20 -63.7(2) . . . . ? C22 C23 C24 C29 -168.2(3) . . . . ? C28 C23 C24 C29 2.0(5) . . . . ? Ti C23 C24 C29 126.4(3) . . . . ? C22 C23 C24 Ti 65.43(19) . . . . ? C28 C23 C24 Ti -124.4(3) . . . . ? N1 Ti C24 C20 125.2(2) . . . . ? C1 Ti C24 C20 -35.5(2) . . . . ? C22 Ti C24 C20 78.65(19) . . . . ? C23 Ti C24 C20 117.4(3) . . . . ? C21 Ti C24 C20 36.37(17) . . . . ? C3 Ti C24 C20 -99.69(18) . . . . ? N1 Ti C24 C23 7.8(3) . . . . ? C1 Ti C24 C23 -152.91(19) . . . . ? C22 Ti C24 C23 -38.77(18) . . . . ? C21 Ti C24 C23 -81.04(19) . . . . ? C20 Ti C24 C23 -117.4(3) . . . . ? C3 Ti C24 C23 142.90(18) . . . . ? N1 Ti C24 C29 -111.7(3) . . . . ? C1 Ti C24 C29 87.6(3) . . . . ? C22 Ti C24 C29 -158.3(3) . . . . ? C23 Ti C24 C29 -119.5(4) . . . . ? C21 Ti C24 C29 159.5(3) . . . . ? C20 Ti C24 C29 123.1(4) . . . . ? C3 Ti C24 C29 23.4(3) . . . . ? N1 P C30 C33 -72.9(3) . . . . ? C38 P C30 C33 168.4(2) . . . . ? C34 P C30 C33 46.7(3) . . . . ? N1 P C30 C31 43.6(3) . . . . ? C38 P C30 C31 -75.1(3) . . . . ? C34 P C30 C31 163.3(2) . . . . ? N1 P C30 C32 165.1(2) . . . . ? C38 P C30 C32 46.4(3) . . . . ? C34 P C30 C32 -75.2(3) . . . . ? N1 P C34 C37 37.7(3) . . . . ? C38 P C34 C37 157.6(2) . . . . ? C30 P C34 C37 -81.2(3) . . . . ? N1 P C34 C35 -78.6(3) . . . . ? C38 P C34 C35 41.3(3) . . . . ? C30 P C34 C35 162.5(2) . . . . ? N1 P C34 C36 160.5(3) . . . . ? C38 P C34 C36 -79.6(3) . . . . ? C30 P C34 C36 41.5(3) . . . . ? N1 P C38 C39 43.1(3) . . . . ? C30 P C38 C39 161.7(2) . . . . ? C34 P C38 C39 -77.4(3) . . . . ? N1 P C38 C40 165.5(3) . . . . ? C30 P C38 C40 -75.9(3) . . . . ? C34 P C38 C40 45.1(3) . . . . ? N1 P C38 C41 -72.8(3) . . . . ? C30 P C38 C41 45.7(3) . . . . ? C34 P C38 C41 166.7(2) . . . . ? N61 Al N51 C71 28.2(3) . . . . ? N52 Al N51 C71 164.7(3) . . . . ? N62 Al N51 C71 -79.2(3) . . . . ? N61 Al N51 C51 -135.37(18) . . . . ? N52 Al N51 C51 1.1(2) . . . . ? N62 Al N51 C51 117.2(2) . . . . ? N61 Al N52 C81 -79.5(3) . . . . ? N51 Al N52 C81 163.6(2) . . . . ? N62 Al N52 C81 27.5(3) . . . . ? N61 Al N52 C52 115.7(2) . . . . ? N51 Al N52 C52 -1.18(19) . . . . ? N62 Al N52 C52 -137.34(18) . . . . ? N51 Al N61 C61 -132.81(18) . . . . ? N52 Al N61 C61 119.03(19) . . . . ? N62 Al N61 C61 3.31(19) . . . . ? N51 Al N61 C91 36.7(3) . . . . ? N52 Al N61 C91 -71.5(3) . . . . ? N62 Al N61 C91 172.8(2) . . . . ? N61 Al N62 C62 -3.58(19) . . . . ? N51 Al N62 C62 112.8(2) . . . . ? N52 Al N62 C62 -139.69(18) . . . . ? N61 Al N62 C101 158.2(2) . . . . ? N51 Al N62 C101 -85.3(3) . . . . ? N52 Al N62 C101 22.1(2) . . . . ? C71 N51 C51 C56 17.0(4) . . . . ? Al N51 C51 C56 -178.6(2) . . . . ? C71 N51 C51 C52 -165.2(3) . . . . ? Al N51 C51 C52 -0.8(3) . . . . ? C81 N52 C52 C53 17.9(4) . . . . ? Al N52 C52 C53 -176.9(2) . . . . ? C81 N52 C52 C51 -164.3(2) . . . . ? Al N52 C52 C51 1.0(3) . . . . ? C56 C51 C52 C53 -4.0(4) . . . . ? N51 C51 C52 C53 177.9(2) . . . . ? C56 C51 C52 N52 177.9(2) . . . . ? N51 C51 C52 N52 -0.1(3) . . . . ? N52 C52 C53 F53 2.2(4) . . . . ? C51 C52 C53 F53 -175.6(2) . . . . ? N52 C52 C53 C54 -179.1(3) . . . . ? C51 C52 C53 C54 3.2(4) . . . . ? F53 C53 C54 F54 -2.5(4) . . . . ? C52 C53 C54 F54 178.7(3) . . . . ? F53 C53 C54 C55 178.3(3) . . . . ? C52 C53 C54 C55 -0.5(5) . . . . ? F54 C54 C55 F55 -1.6(4) . . . . ? C53 C54 C55 F55 177.6(3) . . . . ? F54 C54 C55 C56 179.6(3) . . . . ? C53 C54 C55 C56 -1.2(5) . . . . ? F55 C55 C56 F56 0.7(4) . . . . ? C54 C55 C56 F56 179.5(3) . . . . ? F55 C55 C56 C51 -178.6(3) . . . . ? C54 C55 C56 C51 0.2(5) . . . . ? N51 C51 C56 F56 0.9(4) . . . . ? C52 C51 C56 F56 -176.8(2) . . . . ? N51 C51 C56 C55 -179.8(3) . . . . ? C52 C51 C56 C55 2.4(4) . . . . ? C91 N61 C61 C66 9.3(4) . . . . ? Al N61 C61 C66 179.1(2) . . . . ? C91 N61 C61 C62 -172.2(2) . . . . ? Al N61 C61 C62 -2.3(3) . . . . ? C101 N62 C62 C63 24.3(4) . . . . ? Al N62 C62 C63 -173.2(2) . . . . ? C101 N62 C62 C61 -159.4(2) . . . . ? Al N62 C62 C61 3.1(3) . . . . ? C66 C61 C62 C63 -5.2(4) . . . . ? N61 C61 C62 C63 176.1(2) . . . . ? C66 C61 C62 N62 178.2(2) . . . . ? N61 C61 C62 N62 -0.5(3) . . . . ? N62 C62 C63 F63 -1.0(4) . . . . ? C61 C62 C63 F63 -177.1(2) . . . . ? N62 C62 C63 C64 179.7(3) . . . . ? C61 C62 C63 C64 3.6(4) . . . . ? F63 C63 C64 F64 0.0(4) . . . . ? C62 C63 C64 F64 179.3(2) . . . . ? F63 C63 C64 C65 -179.3(2) . . . . ? C62 C63 C64 C65 0.1(4) . . . . ? F64 C64 C65 F65 -2.0(4) . . . . ? C63 C64 C65 F65 177.2(2) . . . . ? F64 C64 C65 C66 178.8(3) . . . . ? C63 C64 C65 C66 -2.0(4) . . . . ? F65 C65 C66 F66 0.5(4) . . . . ? C64 C65 C66 F66 179.7(2) . . . . ? F65 C65 C66 C61 -179.1(2) . . . . ? C64 C65 C66 C61 0.2(4) . . . . ? N61 C61 C66 F66 2.4(4) . . . . ? C62 C61 C66 F66 -176.1(2) . . . . ? N61 C61 C66 C65 -178.1(3) . . . . ? C62 C61 C66 C65 3.4(4) . . . . ? C51 N51 C71 C72 -128.1(3) . . . . ? Al N51 C71 C72 69.8(4) . . . . ? C51 N51 C71 C76 56.5(4) . . . . ? Al N51 C71 C76 -105.6(3) . . . . ? C76 C71 C72 F72 -179.1(3) . . . . ? N51 C71 C72 F72 5.1(5) . . . . ? C76 C71 C72 C73 0.8(5) . . . . ? N51 C71 C72 C73 -174.9(3) . . . . ? F72 C72 C73 F73 0.8(5) . . . . ? C71 C72 C73 F73 -179.1(3) . . . . ? F72 C72 C73 C74 179.5(3) . . . . ? C71 C72 C73 C74 -0.4(6) . . . . ? F73 C73 C74 F74 -2.0(6) . . . . ? C72 C73 C74 F74 179.3(3) . . . . ? F73 C73 C74 C75 178.5(4) . . . . ? C72 C73 C74 C75 -0.2(6) . . . . ? F74 C74 C75 F75 -0.1(6) . . . . ? C73 C74 C75 F75 179.4(4) . . . . ? F74 C74 C75 C76 -179.1(3) . . . . ? C73 C74 C75 C76 0.5(6) . . . . ? C72 C71 C76 F76 -179.0(3) . . . . ? N51 C71 C76 F76 -3.4(5) . . . . ? C72 C71 C76 C75 -0.6(5) . . . . ? N51 C71 C76 C75 175.0(3) . . . . ? F75 C75 C76 F76 -0.7(6) . . . . ? C74 C75 C76 F76 178.3(4) . . . . ? F75 C75 C76 C71 -179.0(3) . . . . ? C74 C75 C76 C71 0.0(6) . . . . ? C52 N52 C81 C86 49.8(4) . . . . ? Al N52 C81 C86 -113.4(3) . . . . ? C52 N52 C81 C82 -136.3(3) . . . . ? Al N52 C81 C82 60.4(3) . . . . ? C86 C81 C82 F82 179.0(3) . . . . ? N52 C81 C82 F82 4.6(4) . . . . ? C86 C81 C82 C83 -1.9(4) . . . . ? N52 C81 C82 C83 -176.3(3) . . . . ? F82 C82 C83 F83 1.7(4) . . . . ? C81 C82 C83 F83 -177.3(3) . . . . ? F82 C82 C83 C84 180.0(3) . . . . ? C81 C82 C83 C84 1.0(5) . . . . ? F83 C83 C84 F84 -1.1(5) . . . . ? C82 C83 C84 F84 -179.4(3) . . . . ? F83 C83 C84 C85 178.3(3) . . . . ? C82 C83 C84 C85 0.0(5) . . . . ? F84 C84 C85 F85 -2.2(5) . . . . ? C83 C84 C85 F85 178.4(3) . . . . ? F84 C84 C85 C86 179.5(3) . . . . ? C83 C84 C85 C86 0.1(5) . . . . ? F85 C85 C86 F86 -1.1(5) . . . . ? C84 C85 C86 F86 177.2(3) . . . . ? F85 C85 C86 C81 -179.5(3) . . . . ? C84 C85 C86 C81 -1.2(5) . . . . ? C82 C81 C86 F86 -176.3(3) . . . . ? N52 C81 C86 F86 -2.2(4) . . . . ? C82 C81 C86 C85 2.0(4) . . . . ? N52 C81 C86 C85 176.2(3) . . . . ? C61 N61 C91 C96 60.1(4) . . . . ? Al N61 C91 C96 -108.4(3) . . . . ? C61 N61 C91 C92 -124.9(3) . . . . ? Al N61 C91 C92 66.6(3) . . . . ? C96 C91 C92 F92 178.7(3) . . . . ? N61 C91 C92 F92 3.3(4) . . . . ? C96 C91 C92 C93 -1.6(4) . . . . ? N61 C91 C92 C93 -177.0(3) . . . . ? F92 C92 C93 F93 2.4(5) . . . . ? C91 C92 C93 F93 -177.4(3) . . . . ? F92 C92 C93 C94 -178.5(3) . . . . ? C91 C92 C93 C94 1.7(5) . . . . ? F93 C93 C94 F94 -0.3(5) . . . . ? C92 C93 C94 F94 -179.5(3) . . . . ? F93 C93 C94 C95 178.3(3) . . . . ? C92 C93 C94 C95 -0.8(5) . . . . ? F94 C94 C95 F95 -2.8(5) . . . . ? C93 C94 C95 F95 178.6(3) . . . . ? F94 C94 C95 C96 178.5(3) . . . . ? C93 C94 C95 C96 -0.1(5) . . . . ? F95 C95 C96 F96 0.2(5) . . . . ? C94 C95 C96 F96 178.8(3) . . . . ? F95 C95 C96 C91 -178.5(3) . . . . ? C94 C95 C96 C91 0.2(5) . . . . ? C92 C91 C96 F96 -178.0(3) . . . . ? N61 C91 C96 F96 -2.8(4) . . . . ? C92 C91 C96 C95 0.6(4) . . . . ? N61 C91 C96 C95 175.8(3) . . . . ? C62 N62 C101 C102 -138.3(3) . . . . ? Al N62 C101 C102 61.5(3) . . . . ? C62 N62 C101 C106 47.5(4) . . . . ? Al N62 C101 C106 -112.7(3) . . . . ? C106 C101 C102 F102 179.4(3) . . . . ? N62 C101 C102 F102 4.7(4) . . . . ? C106 C101 C102 C103 -0.1(4) . . . . ? N62 C101 C102 C103 -174.8(3) . . . . ? F102 C102 C103 F103 1.1(5) . . . . ? C101 C102 C103 F103 -179.4(3) . . . . ? F102 C102 C103 C104 179.1(3) . . . . ? C101 C102 C103 C104 -1.4(5) . . . . ? F103 C103 C104 F104 -0.8(5) . . . . ? C102 C103 C104 F104 -178.8(3) . . . . ? F103 C103 C104 C105 179.0(3) . . . . ? C102 C103 C104 C105 1.1(5) . . . . ? F104 C104 C105 F105 -1.3(5) . . . . ? C103 C104 C105 F105 178.8(3) . . . . ? F104 C104 C105 C106 -179.4(3) . . . . ? C103 C104 C105 C106 0.7(5) . . . . ? F105 C105 C106 F106 -1.8(5) . . . . ? C104 C105 C106 F106 176.3(3) . . . . ? F105 C105 C106 C101 179.6(3) . . . . ? C104 C105 C106 C101 -2.3(5) . . . . ? C102 C101 C106 F106 -176.7(3) . . . . ? N62 C101 C106 F106 -2.2(4) . . . . ? C102 C101 C106 C105 1.9(4) . . . . ? N62 C101 C106 C105 176.3(3) . . . . ? C6S C1S C2S C3S 0.0 . . . . ? Br1S C1S C2S C3S -180.0(7) . . . . ? C1S C2S C3S C4S 0.0 . . . . ? C2S C3S C4S C5S 0.0 . . . . ? C3S C4S C5S C6S 0.0 . . . . ? C4S C5S C6S C1S 0.0 . . . . ? C2S C1S C6S C5S 0.0 . . . . ? Br1S C1S C6S C5S 180.0(7) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.004 _refine_diff_density_min -1.277 _refine_diff_density_rms 0.081