data_stan243 _audit_creation_method shelxl-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'al3 f o12 p3, c5 h9 n2' _chemical_formula_sum 'c5 h9 al3 f n2 o12 p3' _chemical_formula_weight 481.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'c' 'c' 0.0029 0.0015 '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' 0.0058 0.0031 'international tables vol c tables 4.2.6.8 and 6.1.1.4' 'o' 'o' 0.0103 0.0057 'international tables vol c tables 4.2.6.8 and 6.1.1.4' 'f' 'f' 0.0167 0.0098 'international tables vol c tables 4.2.6.8 and 6.1.1.4' 'al' 'al' 0.0614 0.0490 'international tables vol c tables 4.2.6.8 and 6.1.1.4' 'p' 'p' 0.0984 0.0900 'international tables vol c tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_h-m 'p -1' _symmetry_space_group_name_hall '-p 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.074(3) _cell_length_b 9.230(3) _cell_length_c 9.309(3) _cell_angle_alpha 76.446(5) _cell_angle_beta 87.343(5) _cell_angle_gamma 89.388(5) _cell_volume 757.1(4) _cell_formula_units_z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.114 _exptl_crystal_density_method 'not measured' _exptl_crystal_f_000 484 _exptl_absorpt_coefficient_mu 0.527 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_t_min ? _exptl_absorpt_correction_t_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.69330 _diffrn_radiation_type synchrotron _diffrn_radiation_source synchrotron _diffrn_source_type 'srs beamline 9.8' _diffrn_radiation_monochromator silicon _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8652 _diffrn_reflns_av_r_equivalents 0.0281 _diffrn_reflns_av_sigmai/neti 0.0493 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 29.67 _reflns_number_total 4468 _reflns_number_gt 3416 _reflns_threshold_expression >2sigma(i) _computing_data_collection 'bruker smart' _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution SHELXL-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0709P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4468 _refine_ls_number_parameters 237 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0555 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.1203 _refine_ls_wR_factor_gt 0.1117 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.011 _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 P1 P 0.18744(6) 0.38185(7) 0.90258(7) 0.00843(13) Uani 1 1 d . . . P2 P 0.61755(6) 0.37170(7) 0.67634(6) 0.00822(13) Uani 1 1 d . . . P3 P 0.35394(7) -0.16819(7) 0.85434(7) 0.00889(13) Uani 1 1 d . . . Al4 Al 0.83934(8) 0.37467(8) 0.92586(8) 0.00933(15) Uani 1 1 d . . . Al5 Al 0.43433(8) 0.13220(8) 0.91193(8) 0.00819(15) Uani 1 1 d . . . Al6 Al 0.38097(8) -0.39099(8) 0.65811(8) 0.01055(16) Uani 1 1 d . . . F1 F 0.39419(15) -0.01361(15) 1.08364(14) 0.0098(3) Uani 1 1 d . . . O2 O 0.50263(18) 0.25482(19) 0.73720(18) 0.0112(3) Uani 1 1 d . . . O3 O 0.34794(18) 0.00086(19) 0.81221(18) 0.0101(3) Uani 1 1 d . . . O4 O 0.26206(18) 0.23280(19) 0.92873(18) 0.0113(3) Uani 1 1 d . . . O5 O 0.46679(19) -0.23326(19) 0.96689(18) 0.0108(3) Uani 1 1 d . . . O6 O 0.3821(2) -0.2237(2) 0.71125(18) 0.0129(3) Uani 1 1 d . . . O7 O 0.75284(18) 0.3573(2) 0.76943(18) 0.0120(3) Uani 1 1 d . . . O8 O 0.02464(19) 0.3618(2) 0.8773(2) 0.0142(4) Uani 1 1 d . . . O9 O 0.67540(19) 0.3551(2) 0.52280(18) 0.0123(3) Uani 1 1 d . . . O10 O 0.1980(2) 0.4525(2) 1.03565(19) 0.0141(4) Uani 1 1 d . . . O11 O 0.20005(18) -0.2304(2) 0.91935(19) 0.0119(3) Uani 1 1 d . . . O12 O 0.55445(19) 0.5285(2) 0.6619(2) 0.0135(3) Uani 1 1 d . . . O13 O 0.2503(2) 0.4901(2) 0.76322(19) 0.0141(4) Uani 1 1 d . . . N1 N 0.8867(3) 0.9424(3) 0.7034(3) 0.0305(6) Uani 1 1 d . . . N2 N 0.8805(3) 0.7897(4) 0.5608(3) 0.0397(7) Uani 1 1 d . . . C1 C 0.9350(4) 1.0178(4) 0.8144(4) 0.0349(8) Uani 1 1 d . . . H1A H 0.8892 0.9703 0.9112 0.052 Uiso 1 1 calc R . . H1B H 0.9058 1.1229 0.7874 0.052 Uiso 1 1 calc R . . H1C H 1.0426 1.0109 0.8193 0.052 Uiso 1 1 calc R . . C2 C 0.9535(4) 0.8288(4) 0.6650(4) 0.0365(8) Uani 1 1 d . . . H2 H 1.0408 0.7822 0.7060 0.044 Uiso 1 1 calc R . . C3 C 0.7624(5) 0.9760(5) 0.6218(4) 0.0456(10) Uani 1 1 d . . . H3 H 0.6930 1.0526 0.6270 0.055 Uiso 1 1 calc R . . C4 C 0.7580(5) 0.8795(5) 0.5332(4) 0.0440(9) Uani 1 1 d . . . H4 H 0.6846 0.8746 0.4650 0.053 Uiso 1 1 calc R . . C5 C 0.9200(5) 0.6666(5) 0.4930(5) 0.0548(12) Uani 1 1 d . . . H5A H 1.0271 0.6656 0.4740 0.082 Uiso 1 1 calc R . . H5B H 0.8705 0.6792 0.3995 0.082 Uiso 1 1 calc R . . H5C H 0.8889 0.5723 0.5600 0.082 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 P1 0.0066(3) 0.0090(3) 0.0105(3) -0.0039(2) -0.0006(2) 0.0007(2) P2 0.0080(3) 0.0098(3) 0.0075(3) -0.0032(2) -0.0015(2) 0.0008(2) P3 0.0101(3) 0.0090(3) 0.0087(3) -0.0041(2) -0.0020(2) 0.0005(2) Al4 0.0085(3) 0.0104(3) 0.0099(3) -0.0039(3) -0.0017(2) 0.0003(3) Al5 0.0084(3) 0.0080(3) 0.0089(3) -0.0031(3) -0.0016(2) 0.0005(3) Al6 0.0115(3) 0.0112(4) 0.0099(3) -0.0044(3) -0.0007(2) 0.0012(3) F1 0.0099(6) 0.0096(7) 0.0097(6) -0.0019(5) -0.0004(5) 0.0012(5) O2 0.0106(8) 0.0116(8) 0.0110(8) -0.0018(6) -0.0011(6) -0.0025(6) O3 0.0123(8) 0.0073(8) 0.0114(8) -0.0033(6) -0.0026(6) 0.0007(6) O4 0.0096(8) 0.0101(8) 0.0149(8) -0.0042(7) -0.0011(6) 0.0019(6) O5 0.0116(8) 0.0104(8) 0.0115(8) -0.0038(6) -0.0045(6) 0.0016(6) O6 0.0186(9) 0.0109(8) 0.0108(8) -0.0058(6) -0.0012(6) 0.0015(7) O7 0.0102(8) 0.0182(9) 0.0090(8) -0.0056(7) -0.0035(6) 0.0012(7) O8 0.0074(8) 0.0190(9) 0.0167(9) -0.0051(7) -0.0008(6) 0.0012(7) O9 0.0133(8) 0.0175(9) 0.0070(7) -0.0048(7) -0.0008(6) -0.0015(7) O10 0.0196(9) 0.0124(8) 0.0125(8) -0.0067(7) -0.0044(7) 0.0033(7) O11 0.0090(8) 0.0129(8) 0.0131(8) -0.0014(7) -0.0008(6) -0.0022(6) O12 0.0125(8) 0.0092(8) 0.0196(9) -0.0046(7) -0.0036(7) 0.0018(7) O13 0.0146(9) 0.0120(9) 0.0148(8) -0.0019(7) 0.0033(6) -0.0015(7) N1 0.0276(14) 0.0306(15) 0.0327(15) -0.0064(12) -0.0031(11) 0.0044(12) N2 0.0385(17) 0.049(2) 0.0350(16) -0.0174(15) -0.0015(13) -0.0048(15) C1 0.0317(18) 0.0330(19) 0.043(2) -0.0151(16) -0.0022(15) 0.0016(14) C2 0.0352(19) 0.039(2) 0.0392(19) -0.0165(16) -0.0093(15) 0.0033(15) C3 0.048(2) 0.053(2) 0.038(2) -0.0133(18) -0.0156(17) 0.0196(19) C4 0.041(2) 0.050(2) 0.042(2) -0.0106(18) -0.0123(16) 0.0011(18) C5 0.059(3) 0.057(3) 0.059(3) -0.037(2) 0.015(2) -0.022(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 P1 O4 1.4996(18) . ? P1 O8 1.5264(19) . ? P1 O13 1.5305(19) . ? P1 O10 1.5364(18) . ? P2 O2 1.5017(18) . ? P2 O7 1.5221(18) . ? P2 O12 1.5295(18) . ? P2 O9 1.5406(17) . ? P3 O5 1.5160(18) . ? P3 O3 1.5181(18) . ? P3 O6 1.5451(17) . ? P3 O11 1.5563(18) . ? Al4 O7 1.7265(18) . ? Al4 O8 1.7308(19) 1_655 ? Al4 O10 1.7413(19) 2_667 ? Al4 O11 1.7434(19) 2_657 ? Al5 O4 1.8288(18) . ? Al5 O2 1.8355(19) . ? Al5 F1 1.8566(16) . ? Al5 O5 1.8849(18) 2_657 ? Al5 O3 1.8871(18) . ? Al5 F1 1.8893(16) 2_657 ? Al6 O13 1.728(2) 1_545 ? Al6 O6 1.7287(19) . ? Al6 O12 1.7318(19) 1_545 ? Al6 O9 1.7384(18) 2_656 ? N1 C2 1.318(4) . ? N1 C3 1.381(5) . ? N1 C1 1.460(4) . ? N2 C2 1.318(4) . ? N2 C4 1.377(5) . ? N2 C5 1.457(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2 0.9500 . ? C3 C4 1.350(6) . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 P1 O8 108.91(11) . . ? O4 P1 O13 112.13(10) . . ? O8 P1 O13 106.29(10) . . ? O4 P1 O10 111.64(10) . . ? O8 P1 O10 108.37(10) . . ? O13 P1 O10 109.28(11) . . ? O2 P2 O7 113.32(10) . . ? O2 P2 O12 111.25(10) . . ? O7 P2 O12 108.13(10) . . ? O2 P2 O9 109.50(10) . . ? O7 P2 O9 105.42(10) . . ? O12 P2 O9 108.99(10) . . ? O5 P3 O3 114.91(10) . . ? O5 P3 O6 110.56(10) . . ? O3 P3 O6 108.07(10) . . ? O5 P3 O11 107.60(10) . . ? O3 P3 O11 109.35(10) . . ? O6 P3 O11 105.99(10) . . ? O7 Al4 O8 103.24(9) . 1_655 ? O7 Al4 O10 110.90(9) . 2_667 ? O8 Al4 O10 110.09(10) 1_655 2_667 ? O7 Al4 O11 113.92(9) . 2_657 ? O8 Al4 O11 107.29(9) 1_655 2_657 ? O10 Al4 O11 111.02(9) 2_667 2_657 ? O4 Al5 O2 96.42(8) . . ? O4 Al5 F1 93.91(8) . . ? O2 Al5 F1 169.58(8) . . ? O4 Al5 O5 92.70(8) . 2_657 ? O2 Al5 O5 94.94(8) . 2_657 ? F1 Al5 O5 85.98(8) . 2_657 ? O4 Al5 O3 93.62(8) . . ? O2 Al5 O3 91.94(8) . . ? F1 Al5 O3 85.98(8) . . ? O5 Al5 O3 170.09(8) 2_657 . ? O4 Al5 F1 173.27(8) . 2_657 ? O2 Al5 F1 90.30(8) . 2_657 ? F1 Al5 F1 79.39(7) . 2_657 ? O5 Al5 F1 86.30(7) 2_657 2_657 ? O3 Al5 F1 86.53(7) . 2_657 ? O4 Al5 Al5 134.01(7) . 2_657 ? O2 Al5 Al5 129.56(7) . 2_657 ? F1 Al5 Al5 40.11(5) . 2_657 ? O5 Al5 Al5 84.98(6) 2_657 2_657 ? O3 Al5 Al5 85.13(6) . 2_657 ? F1 Al5 Al5 39.28(4) 2_657 2_657 ? O13 Al6 O6 110.42(9) 1_545 . ? O13 Al6 O12 112.32(10) 1_545 1_545 ? O6 Al6 O12 112.06(9) . 1_545 ? O13 Al6 O9 105.94(9) 1_545 2_656 ? O6 Al6 O9 107.80(9) . 2_656 ? O12 Al6 O9 107.98(9) 1_545 2_656 ? Al5 F1 Al5 100.61(7) . 2_657 ? P2 O2 Al5 141.33(11) . . ? P3 O3 Al5 126.61(10) . . ? P1 O4 Al5 146.17(12) . . ? P3 O5 Al5 126.82(11) . 2_657 ? P3 O6 Al6 137.83(12) . . ? P2 O7 Al4 151.38(12) . . ? P1 O8 Al4 151.36(13) . 1_455 ? P2 O9 Al6 139.38(12) . 2_656 ? P1 O10 Al4 136.82(12) . 2_667 ? P3 O11 Al4 128.04(11) . 2_657 ? P2 O12 Al6 136.70(12) . 1_565 ? P1 O13 Al6 155.26(13) . 1_565 ? C2 N1 C3 108.0(3) . . ? C2 N1 C1 125.8(3) . . ? C3 N1 C1 126.2(3) . . ? C2 N2 C4 108.5(3) . . ? C2 N2 C5 125.2(4) . . ? C4 N2 C5 126.3(3) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 N2 109.6(3) . . ? N1 C2 H2 125.2 . . ? N2 C2 H2 125.2 . . ? C4 C3 N1 107.1(3) . . ? C4 C3 H3 126.4 . . ? N1 C3 H3 126.4 . . ? C3 C4 N2 106.7(3) . . ? C3 C4 H4 126.6 . . ? N2 C4 H4 126.6 . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 24.80 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.612 _refine_diff_density_min -0.572 _refine_diff_density_rms 0.121