data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Wragg, David' _publ_contact_author_email david.wragg@smn.uio.no _publ_section_title ; Solvothermal aluminophosphate zeotype synthesis with ionic liquid precursors ; loop_ _publ_author_name D.Wragg G.Fullerton P.Byrne A.Slawin J.Warren S.Teat R.Morris data_compound2 _database_code_depnum_ccdc_archive 'CCDC 683429' #TrackingRef '- complete_final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'compound 2' _chemical_melting_point ? _chemical_formula_moiety 'Al3 O16 P4, 2(C4 H7 N2), H2 O' _chemical_formula_sum 'C8 H16 Al3 N4 O17 P4' _chemical_formula_weight 645.07 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' Al Al 0.0645 0.0514 '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' O O 0.0106 0.0060 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.901(5) _cell_length_b 9.439(5) _cell_length_c 14.695(7) _cell_angle_alpha 78.425(17) _cell_angle_beta 86.286(19) _cell_angle_gamma 77.873(14) _cell_volume 1182.2(10) _cell_formula_units_Z 2 _cell_measurement_temperature 93.1500 _cell_measurement_reflns_used 2787 _cell_measurement_theta_min 2.4164 _cell_measurement_theta_max 28.0328 _exptl_crystal_description Platelet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.812 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 656 _exptl_absorpt_coefficient_mu 0.518 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7823 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'CrystalClear (Rigaku/MSC Inc., 2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93.1500 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type ; Saturn70 (4x4 bin mode) ; _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11534 _diffrn_reflns_av_R_equivalents 0.0500 _diffrn_reflns_av_sigmaI/netI 0.0466 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 25.32 _reflns_number_total 4192 _reflns_number_gt 3920 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2006)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2006)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics DIAMOND _computing_publication_material 'PLATON (SPEK, 2008)' _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. Hydrogen atoms on the organic groups were refined using a riding model. No other restraints used. ; _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^)+(0.0973P)^2^+3.5838P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4192 _refine_ls_number_parameters 362 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0654 _refine_ls_R_factor_gt 0.0624 _refine_ls_wR_factor_ref 0.1702 _refine_ls_wR_factor_gt 0.1661 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.081 _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 P1 P 0.13944(10) 0.94632(10) 0.28178(6) 0.0129(2) Uani 1 1 d . . . P2 P -0.49586(11) 1.23716(10) 0.23138(6) 0.0135(3) Uani 1 1 d . . . P3 P -0.36054(11) 0.80880(10) 0.43031(6) 0.0124(2) Uani 1 1 d . . . P4 P 0.68348(11) 0.83840(10) 0.09767(6) 0.0137(3) Uani 1 1 d . . . Al1 Al 0.34074(12) 1.05991(12) 0.40010(7) 0.0131(3) Uani 1 1 d . . . Al2 Al 0.36498(12) 1.05415(12) 0.11758(7) 0.0136(3) Uani 1 1 d . . . Al3 Al -0.21376(12) 0.97277(11) 0.24827(7) 0.0127(3) Uani 1 1 d . . . O1 O -0.3303(3) 1.1476(3) 0.2381(2) 0.0221(6) Uani 1 1 d . . . O2 O -0.2805(3) 0.8460(3) 0.33499(18) 0.0193(6) Uani 1 1 d . . . O3 O -0.3527(3) 0.6463(3) 0.45865(18) 0.0173(6) Uani 1 1 d . . . O4 O 0.4718(3) 0.8925(3) 0.4244(2) 0.0217(6) Uani 1 1 d . . . O5 O 0.7188(4) 0.6739(3) 0.1261(2) 0.0239(6) Uani 1 1 d . . . O6 O 0.5167(3) 0.9042(3) 0.1230(2) 0.0218(6) Uani 1 1 d . . . O7 O 0.4195(4) 1.1908(3) 0.3235(2) 0.0253(6) Uani 1 1 d . . . O8 O -0.4948(3) 1.3991(3) 0.21504(19) 0.0192(6) Uani 1 1 d . . . O9 O 0.1863(3) 0.7826(3) 0.30975(19) 0.0208(6) Uani 1 1 d . . . O10 O -0.2089(3) 0.9099(3) 0.14437(18) 0.0186(6) Uani 1 1 d . . . O11 O -0.0343(3) 0.9981(3) 0.26959(18) 0.0182(6) Uani 1 1 d . . . O12 O 0.2157(3) 1.0052(3) 0.18843(18) 0.0214(6) Uani 1 1 d . . . O13 O 0.4242(3) 1.2007(3) 0.15173(19) 0.0220(6) Uani 1 1 d . . . O14 O 0.2800(3) 1.1305(3) 0.50002(18) 0.0179(6) Uani 1 1 d . . . O15 O 0.2913(3) 1.1137(3) 0.00751(18) 0.0222(6) Uani 1 1 d . . . O16 O 0.1789(3) 1.0285(3) 0.35492(18) 0.0179(6) Uani 1 1 d . . . C1 C -0.0113(5) 0.5756(5) 0.6029(3) 0.0245(9) Uani 1 1 d . . . C2 C 0.0139(5) 0.4603(5) 0.6751(3) 0.0253(9) Uani 1 1 d . . . C3 C 0.1855(5) 0.5944(4) 0.6790(3) 0.0209(8) Uani 1 1 d . . . C4 C 0.1179(6) 0.7932(5) 0.5404(3) 0.0322(10) Uani 1 1 d . . . H5A H 0.0405 0.8171 0.4941 0.048 Uiso 1 1 calc R . . H5B H 0.2178 0.7767 0.5109 0.048 Uiso 1 1 calc R . . H5C H 0.1082 0.8734 0.5729 0.048 Uiso 1 1 calc R . . N1 N 0.0982(4) 0.6588(4) 0.6066(2) 0.0207(7) Uani 1 1 d . . . N2 N 0.1373(4) 0.4745(4) 0.7217(2) 0.0220(7) Uani 1 1 d . . . H1 H -0.080(6) 0.601(5) 0.557(4) 0.026 Uiso 1 1 d . . . H2 H -0.032(6) 0.386(6) 0.690(3) 0.029(13) Uiso 1 1 d . . . H3 H 0.261(7) 0.623(6) 0.701(4) 0.043(16) Uiso 1 1 d . . . H1N H 0.177(5) 0.416(5) 0.772(3) 0.013(10) Uiso 1 1 d . . . C5 C 0.2634(5) 0.5446(4) 0.0074(3) 0.0244(9) Uani 1 1 d . . . C6 C 0.2383(6) 0.6977(5) 0.1040(3) 0.0323(11) Uani 1 1 d . . . C7 C 0.1285(6) 0.7525(5) 0.0403(3) 0.0306(10) Uani 1 1 d . . . C8 C 0.0466(6) 0.6682(6) -0.0984(3) 0.0367(11) Uani 1 1 d . . . H10A H -0.0294 0.7579 -0.1032 0.055 Uiso 1 1 calc R . . H10B H -0.0035 0.5855 -0.0886 0.055 Uiso 1 1 calc R . . H10C H 0.1077 0.6701 -0.1547 0.055 Uiso 1 1 calc R . . N3 N 0.1456(4) 0.6545(4) -0.0201(2) 0.0254(8) Uani 1 1 d . . . N4 N 0.3221(4) 0.5694(4) 0.0816(2) 0.0238(8) Uani 1 1 d . . . H5 H 0.295(5) 0.465(5) -0.028(3) 0.019(11) Uiso 1 1 d . . . H6 H 0.263(6) 0.729(5) 0.158(4) 0.027(12) Uiso 1 1 d . . . H7 H 0.059(7) 0.834(7) 0.035(4) 0.047(17) Uiso 1 1 d . . . H2N H 0.387(6) 0.507(6) 0.121(4) 0.029(13) Uiso 1 1 d . . . O1W O 0.4192(4) 0.5448(4) 0.3740(2) 0.0348(8) Uani 1 1 d D . . H1W H 0.445(6) 0.491(6) 0.326(3) 0.042 Uiso 1 1 d D . . H2W H 0.350(6) 0.638(5) 0.353(4) 0.042 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0155(5) 0.0121(5) 0.0117(5) -0.0018(3) -0.0027(4) -0.0041(4) P2 0.0170(5) 0.0097(5) 0.0139(5) -0.0008(3) -0.0031(4) -0.0035(4) P3 0.0171(5) 0.0094(5) 0.0107(5) -0.0010(3) -0.0028(3) -0.0030(4) P4 0.0181(5) 0.0100(5) 0.0121(5) -0.0010(3) -0.0056(4) -0.0006(4) Al1 0.0164(6) 0.0123(5) 0.0114(5) -0.0024(4) -0.0026(4) -0.0037(4) Al2 0.0172(6) 0.0128(5) 0.0111(5) -0.0013(4) -0.0032(4) -0.0038(4) Al3 0.0144(6) 0.0119(5) 0.0120(5) -0.0013(4) -0.0031(4) -0.0031(4) O1 0.0174(14) 0.0153(13) 0.0342(16) -0.0068(12) -0.0034(12) -0.0015(11) O2 0.0284(15) 0.0190(14) 0.0113(13) -0.0018(10) 0.0037(11) -0.0090(11) O3 0.0228(14) 0.0118(13) 0.0175(13) -0.0028(10) 0.0010(11) -0.0046(10) O4 0.0166(14) 0.0179(14) 0.0318(16) -0.0084(11) -0.0061(11) -0.0014(11) O5 0.0367(17) 0.0112(13) 0.0219(15) -0.0011(11) -0.0116(12) 0.0008(12) O6 0.0174(14) 0.0188(14) 0.0289(15) -0.0043(11) -0.0015(11) -0.0027(11) O7 0.0357(17) 0.0206(14) 0.0213(15) -0.0025(11) 0.0052(12) -0.0124(13) O8 0.0256(15) 0.0093(12) 0.0232(14) -0.0008(10) -0.0059(11) -0.0051(11) O9 0.0261(15) 0.0121(13) 0.0236(15) -0.0020(11) -0.0051(11) -0.0023(11) O10 0.0216(14) 0.0229(14) 0.0138(13) -0.0037(11) -0.0032(10) -0.0093(11) O11 0.0138(13) 0.0233(14) 0.0195(14) -0.0067(11) -0.0027(10) -0.0045(11) O12 0.0244(15) 0.0260(15) 0.0139(13) -0.0014(11) 0.0040(11) -0.0088(12) O13 0.0302(16) 0.0153(13) 0.0227(15) -0.0011(11) -0.0108(12) -0.0086(12) O14 0.0217(14) 0.0199(13) 0.0143(13) -0.0074(10) -0.0036(11) -0.0043(11) O15 0.0283(15) 0.0255(15) 0.0128(14) -0.0012(11) -0.0072(11) -0.0057(12) O16 0.0210(14) 0.0168(13) 0.0175(13) -0.0070(10) -0.0067(11) -0.0016(11) C1 0.027(2) 0.021(2) 0.025(2) -0.0039(16) -0.0069(17) -0.0018(17) C2 0.029(2) 0.0167(19) 0.031(2) -0.0019(17) -0.0046(18) -0.0073(17) C3 0.024(2) 0.0200(19) 0.020(2) -0.0064(16) -0.0024(16) -0.0043(16) C4 0.044(3) 0.022(2) 0.025(2) 0.0061(17) 0.0078(19) -0.0064(19) N1 0.0236(18) 0.0149(16) 0.0215(17) 0.0001(13) -0.0007(13) -0.0025(13) N2 0.0256(18) 0.0158(16) 0.0227(18) -0.0005(14) -0.0093(14) 0.0000(14) C5 0.031(2) 0.0158(19) 0.025(2) -0.0046(16) -0.0024(17) 0.0003(16) C6 0.053(3) 0.021(2) 0.023(2) -0.0105(18) -0.002(2) -0.001(2) C7 0.040(3) 0.019(2) 0.028(2) -0.0060(17) 0.0018(19) 0.0063(19) C8 0.039(3) 0.038(3) 0.028(2) -0.002(2) -0.013(2) 0.002(2) N3 0.033(2) 0.0183(17) 0.0219(18) 0.0001(14) -0.0066(15) -0.0016(15) N4 0.033(2) 0.0147(16) 0.0210(18) -0.0001(13) -0.0051(15) -0.0006(15) O1W 0.043(2) 0.0277(17) 0.0338(19) -0.0072(14) -0.0045(15) -0.0041(15) _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 O9 1.492(3) . ? P1 O11 1.532(3) . ? P1 O16 1.542(3) . ? P1 O12 1.544(3) . ? P2 O8 1.501(3) . ? P2 O1 1.535(3) . ? P2 O7 1.537(3) 1_455 ? P2 O13 1.539(3) 1_455 ? P3 O3 1.494(3) . ? P3 O4 1.534(3) 1_455 ? P3 O2 1.540(3) . ? P3 O14 1.547(3) 2_576 ? P4 O5 1.495(3) . ? P4 O15 1.536(3) 2_675 ? P4 O6 1.537(3) . ? P4 O10 1.545(3) 1_655 ? Al1 O16 1.728(3) . ? Al1 O7 1.728(3) . ? Al1 O14 1.741(3) . ? Al1 O4 1.743(3) . ? Al2 O12 1.717(3) . ? Al2 O15 1.726(3) . ? Al2 O6 1.731(3) . ? Al2 O13 1.750(3) . ? Al3 O11 1.721(3) . ? Al3 O2 1.731(3) . ? Al3 O1 1.739(3) . ? Al3 O10 1.740(3) . ? C1 C2 1.352(6) . ? C1 N1 1.384(6) . ? C1 H1 0.90(5) . ? C2 N2 1.374(6) . ? C2 H2 0.87(5) . ? C3 N2 1.321(6) . ? C3 N1 1.325(5) . ? C3 H3 0.88(6) . ? C4 N1 1.471(5) . ? C4 H5A 0.9600 . ? C4 H5B 0.9600 . ? C4 H5C 0.9600 . ? N2 H1N 0.87(5) . ? C5 N4 1.322(6) . ? C5 N3 1.329(5) . ? C5 H5 0.98(5) . ? C6 C7 1.345(7) . ? C6 N4 1.371(6) . ? C6 H6 0.96(5) . ? C7 N3 1.385(6) . ? C7 H7 0.87(6) . ? C8 N3 1.464(6) . ? C8 H10A 0.9600 . ? C8 H10B 0.9600 . ? C8 H10C 0.9600 . ? N4 H2N 0.89(5) . ? O1W H1W 0.93(4) . ? O1W H2W 0.97(4) . ? 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 O9 P1 O11 112.62(16) . . ? O9 P1 O16 112.66(15) . . ? O11 P1 O16 104.89(15) . . ? O9 P1 O12 111.89(16) . . ? O11 P1 O12 106.43(16) . . ? O16 P1 O12 107.88(16) . . ? O8 P2 O1 109.85(16) . . ? O8 P2 O7 110.18(16) . 1_455 ? O1 P2 O7 107.81(17) . 1_455 ? O8 P2 O13 110.62(15) . 1_455 ? O1 P2 O13 109.23(16) . 1_455 ? O7 P2 O13 109.09(17) 1_455 1_455 ? O3 P3 O4 110.64(16) . 1_455 ? O3 P3 O2 110.98(15) . . ? O4 P3 O2 108.56(16) 1_455 . ? O3 P3 O14 112.06(15) . 2_576 ? O4 P3 O14 107.60(15) 1_455 2_576 ? O2 P3 O14 106.83(16) . 2_576 ? O5 P4 O15 111.10(16) . 2_675 ? O5 P4 O6 111.64(17) . . ? O15 P4 O6 108.35(16) 2_675 . ? O5 P4 O10 111.44(16) . 1_655 ? O15 P4 O10 105.91(16) 2_675 1_655 ? O6 P4 O10 108.16(16) . 1_655 ? O16 Al1 O7 110.97(15) . . ? O16 Al1 O14 106.44(14) . . ? O7 Al1 O14 108.04(14) . . ? O16 Al1 O4 108.13(14) . . ? O7 Al1 O4 111.19(16) . . ? O14 Al1 O4 111.99(14) . . ? O12 Al2 O15 105.72(15) . . ? O12 Al2 O6 109.91(15) . . ? O15 Al2 O6 112.25(15) . . ? O12 Al2 O13 109.84(15) . . ? O15 Al2 O13 108.87(14) . . ? O6 Al2 O13 110.16(15) . . ? O11 Al3 O2 112.96(14) . . ? O11 Al3 O1 104.47(14) . . ? O2 Al3 O1 111.72(15) . . ? O11 Al3 O10 109.83(14) . . ? O2 Al3 O10 107.80(14) . . ? O1 Al3 O10 110.05(14) . . ? P2 O1 Al3 145.74(19) . . ? P3 O2 Al3 150.18(19) . . ? P3 O4 Al1 148.87(19) 1_655 . ? P4 O6 Al2 150.1(2) . . ? P2 O7 Al1 150.1(2) 1_655 . ? P4 O10 Al3 135.00(18) 1_455 . ? P1 O11 Al3 153.10(19) . . ? P1 O12 Al2 154.9(2) . . ? P2 O13 Al2 141.48(18) 1_655 . ? P3 O14 Al1 133.99(18) 2_576 . ? P4 O15 Al2 149.8(2) 2_675 . ? P1 O16 Al1 138.28(19) . . ? C2 C1 N1 106.8(4) . . ? C2 C1 H1 132(3) . . ? N1 C1 H1 121(3) . . ? C1 C2 N2 107.1(4) . . ? C1 C2 H2 129(3) . . ? N2 C2 H2 124(3) . . ? N2 C3 N1 109.2(4) . . ? N2 C3 H3 121(4) . . ? N1 C3 H3 129(4) . . ? N1 C4 H5A 109.5 . . ? N1 C4 H5B 109.5 . . ? H5A C4 H5B 109.5 . . ? N1 C4 H5C 109.5 . . ? H5A C4 H5C 109.5 . . ? H5B C4 H5C 109.5 . . ? C3 N1 C1 108.2(3) . . ? C3 N1 C4 125.6(4) . . ? C1 N1 C4 126.2(4) . . ? C3 N2 C2 108.7(3) . . ? C3 N2 H1N 124(3) . . ? C2 N2 H1N 127(3) . . ? N4 C5 N3 108.7(4) . . ? N4 C5 H5 131(3) . . ? N3 C5 H5 121(3) . . ? C7 C6 N4 107.3(4) . . ? C7 C6 H6 133(3) . . ? N4 C6 H6 119(3) . . ? C6 C7 N3 106.8(4) . . ? C6 C7 H7 129(4) . . ? N3 C7 H7 124(4) . . ? N3 C8 H10A 109.5 . . ? N3 C8 H10B 109.5 . . ? H10A C8 H10B 109.5 . . ? N3 C8 H10C 109.5 . . ? H10A C8 H10C 109.5 . . ? H10B C8 H10C 109.5 . . ? C5 N3 C7 108.3(4) . . ? C5 N3 C8 126.3(4) . . ? C7 N3 C8 125.3(4) . . ? C5 N4 C6 108.9(4) . . ? C5 N4 H2N 128(3) . . ? C6 N4 H2N 121(3) . . ? H1W O1W H2W 111(5) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H1N O5 0.87(5) 1.78(5) 2.639(4) 168(4) 2_666 N4 H2N O8 0.89(5) 1.79(5) 2.670(4) 170(5) 1_645 O1W H1W O8 0.93(4) 2.00(4) 2.924(5) 173(5) 1_645 O1W H2W O9 0.97(4) 1.82(4) 2.771(4) 165(5) . _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.32 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.681 _refine_diff_density_min -0.790 _refine_diff_density_rms 0.132 # Attachment '- complete_final.cif' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 709229' #TrackingRef '- complete_final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'compound 1- interrupted sodalite AlPO' _chemical_melting_point ? _chemical_formula_moiety 'C10 H24 Al4 N2 O20 P5' _chemical_formula_sum 'C10 H24 Al4 N2 O20 P5' _chemical_formula_weight 755.08 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' Al Al 0.0645 0.0514 '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' O O 0.0106 0.0060 '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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P-421c 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' '-y+1/2, -x+1/2, z+1/2' '-y, x, -z' 'y, -x, -z' 'y+1/2, x+1/2, z+1/2' _cell_length_a 17.7754(11) _cell_length_b 17.7754(11) _cell_length_c 8.8374(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2792.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7999 _cell_measurement_theta_min 2.79 _cell_measurement_theta_max 33.76 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.796 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1540 _exptl_absorpt_coefficient_mu 0.542 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9630 _exptl_absorpt_correction_T_max 0.9786 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.7749 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Advanced Light Source, station 11.3.1' _diffrn_radiation_monochromator 'Channel cut Si (111)' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37535 _diffrn_reflns_av_R_equivalents 0.0506 _diffrn_reflns_av_sigmaI/netI 0.0273 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 31.15 _reflns_number_total 4407 _reflns_number_gt 3930 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex' _computing_cell_refinement 'Bruker Apex' _computing_data_reduction 'Bruker Apex' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material 'Platon, (Spek, 2008)' _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. The spacegroup determined for 1 is noncentrosymmetric but the bulk structure of the crystal is racemic due to inversion twinning with a Flack parameter of 0.5. Analysis of the symmetry of the structure using the program ADDSYM from the PLATON suite suggested that a centrosymmetric spacegroup could be used to describe the structure but refinement of the resulting model led to divergence. Bond lengths in the organic template molecule were restrained to literature values and ISOR and EADP restraints were used on the template atoms to give relatively isotropic thermal ellipsoids. ; _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^)+(0.1299P)^2^+6.9094P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.4(3) _refine_ls_number_reflns 4407 _refine_ls_number_parameters 191 _refine_ls_number_restraints 49 _refine_ls_R_factor_all 0.0878 _refine_ls_R_factor_gt 0.0797 _refine_ls_wR_factor_ref 0.2390 _refine_ls_wR_factor_gt 0.2304 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.067 _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 P4 P 0.64474(9) 0.26496(10) 0.2642(2) 0.0232(5) Uani 0.631(4) 1 d P A 2 P4A P 0.67496(14) 0.32212(14) 0.2699(3) 0.0150(7) Uani 0.369(4) 1 d P A 1 O42A O 0.7071(6) 0.3976(5) 0.2753(15) 0.038(3) Uani 0.369(4) 1 d P A 1 P1 P 0.5000 0.5000 0.0000 0.0132(4) Uani 1 4 d S . . Al2 Al 0.50853(6) 0.37427(6) 0.25181(14) 0.0137(2) Uani 1 1 d . A . P2 P 0.40270(6) 0.23269(6) 0.23651(15) 0.0235(3) Uani 1 1 d . . . Al1 Al 0.77420(10) 0.27657(10) 0.01470(18) 0.0294(3) Uani 1 1 d . A . P3 P 0.5000 0.5000 0.5000 0.0137(4) Uani 1 4 d S . . O22 O 0.43694(18) 0.31089(17) 0.2203(4) 0.0267(8) Uani 1 1 d . . . O21 O 0.5910(2) 0.3274(2) 0.2884(5) 0.0336(9) Uani 1 1 d . . . O1 O 0.8532(3) 0.2680(4) 0.1252(5) 0.0627(18) Uani 1 1 d . . . O3 O 0.6941(3) 0.2828(3) 0.1267(5) 0.0431(11) Uani 1 1 d . . . O23 O 0.4839(2) 0.4318(2) 0.4028(4) 0.0263(7) Uani 1 1 d . . . O41 O 0.6983(2) 0.2638(3) 0.4017(5) 0.0494(13) Uani 1 1 d . . . O51 O 0.4625(3) 0.1740(2) 0.2566(8) 0.0607(16) Uani 1 1 d . . . H51 H 0.4901 0.1737 0.1823 0.091 Uiso 1 1 calc R . . O42 O 0.5999(4) 0.1949(4) 0.2347(15) 0.063(3) Uani 0.631(4) 1 d P A 2 O11 O 0.5194(2) 0.4324(2) 0.0964(4) 0.0289(7) Uani 1 1 d . . . O2 O 0.7824(3) 0.3559(3) -0.0971(5) 0.0404(10) Uani 1 1 d . . . N1 N 0.7679(7) 0.5293(7) 0.2530(18) 0.133(3) Uani 1 1 d DU . . C1 C 0.8229(9) 0.5277(11) 0.142(2) 0.133(3) Uani 1 1 d DU A . H1A H 0.8264 0.5781 0.1000 0.159 Uiso 1 1 calc R . . H1B H 0.8045 0.4955 0.0611 0.159 Uiso 1 1 calc R . . C2 C 0.9002(9) 0.5032(11) 0.177(2) 0.133(3) Uani 1 1 d DU . . H2A H 0.9379 0.5390 0.1438 0.159 Uiso 1 1 calc R A . H2B H 0.9115 0.4536 0.1373 0.159 Uiso 1 1 calc R . . C3 C 0.7064(6) 0.5759(8) 0.238(3) 0.078(5) Uani 0.631(4) 1 d PDU A 1 H3A H 0.6731 0.5559 0.1623 0.118 Uiso 0.631(4) 1 calc PR A 1 H3B H 0.7228 0.6251 0.2078 0.118 Uiso 0.631(4) 1 calc PR A 1 H3C H 0.6804 0.5791 0.3328 0.118 Uiso 0.631(4) 1 calc PR A 1 C3A C 0.7114(13) 0.4873(17) 0.290(4) 0.092(9) Uani 0.369(4) 1 d PDU A 2 H3A1 H 0.6761 0.4856 0.2081 0.138 Uiso 0.369(4) 1 calc PR A 2 H3A2 H 0.6874 0.5077 0.3784 0.138 Uiso 0.369(4) 1 calc PR A 2 H3A3 H 0.7289 0.4373 0.3116 0.138 Uiso 0.369(4) 1 calc PR A 2 C4 C 0.8899(9) 0.5032(11) 0.343(2) 0.133(3) Uani 1 1 d DU A . H4A H 0.9314 0.5289 0.3922 0.159 Uiso 1 1 calc R . . H4B H 0.8874 0.4521 0.3813 0.159 Uiso 1 1 calc R . . C5 C 0.8167(9) 0.5442(10) 0.373(2) 0.133(3) Uani 1 1 d DU A . H5A H 0.7947 0.5269 0.4672 0.159 Uiso 1 1 calc R . . H5B H 0.8257 0.5978 0.3807 0.159 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 P4 0.0191(7) 0.0224(7) 0.0280(9) -0.0004(8) -0.0035(7) 0.0066(5) P4A 0.0123(10) 0.0129(10) 0.0199(13) 0.0003(9) 0.0019(9) -0.0003(8) O42A 0.040(5) 0.016(4) 0.059(7) -0.009(4) 0.005(5) -0.015(3) P1 0.0147(6) 0.0147(6) 0.0102(7) 0.000 0.000 0.000 Al2 0.0132(4) 0.0117(4) 0.0161(5) 0.0008(5) -0.0002(5) 0.0003(3) P2 0.0220(5) 0.0208(4) 0.0278(6) 0.0021(5) -0.0033(4) -0.0083(3) Al1 0.0350(9) 0.0324(8) 0.0208(6) 0.0012(6) -0.0021(6) 0.0178(6) P3 0.0153(6) 0.0153(6) 0.0106(7) 0.000 0.000 0.000 O22 0.0211(13) 0.0173(12) 0.042(2) -0.0047(12) -0.0031(13) -0.0036(10) O21 0.0225(15) 0.0330(17) 0.045(2) 0.0092(16) -0.0017(14) 0.0075(13) O1 0.045(3) 0.119(5) 0.0246(19) 0.011(3) -0.0073(18) 0.044(3) O3 0.041(2) 0.059(3) 0.0287(19) 0.0024(19) 0.0067(17) 0.012(2) O23 0.0309(17) 0.0249(15) 0.0230(14) -0.0066(12) -0.0007(13) 0.0003(14) O41 0.032(2) 0.083(4) 0.033(2) 0.006(2) -0.0058(16) 0.024(2) O51 0.052(2) 0.0228(16) 0.107(5) 0.013(3) -0.022(3) 0.0011(16) O42 0.035(3) 0.025(3) 0.129(9) -0.016(5) -0.006(5) 0.003(2) O11 0.040(2) 0.0249(16) 0.0223(14) 0.0101(12) 0.0000(14) 0.0054(15) O2 0.043(2) 0.047(2) 0.0313(19) 0.0157(18) -0.0066(17) 0.0097(19) N1 0.097(4) 0.125(5) 0.176(6) 0.001(5) 0.024(4) 0.004(3) C1 0.097(4) 0.125(5) 0.176(6) 0.001(5) 0.024(4) 0.004(3) C2 0.097(4) 0.125(5) 0.176(6) 0.001(5) 0.024(4) 0.004(3) C3 0.035(4) 0.063(7) 0.137(13) 0.024(10) 0.005(8) 0.006(5) C3A 0.047(10) 0.100(15) 0.129(19) -0.003(14) 0.029(12) -0.015(11) C4 0.097(4) 0.125(5) 0.176(6) 0.001(5) 0.024(4) 0.004(3) C5 0.097(4) 0.125(5) 0.176(6) 0.001(5) 0.024(4) 0.004(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 P4 O21 1.480(4) . ? P4 O42 1.501(7) . ? P4 O3 1.531(5) . ? P4 O41 1.544(5) . ? P4A O42A 1.459(9) . ? P4A O3 1.485(5) . ? P4A O21 1.504(4) . ? P4A O41 1.614(6) . ? P1 O11 1.513(3) 3_665 ? P1 O11 1.513(3) 7_565 ? P1 O11 1.513(3) . ? P1 O11 1.513(3) 6_655 ? Al2 O21 1.717(3) . ? Al2 O22 1.722(3) . ? Al2 O11 1.729(4) . ? Al2 O23 1.737(4) . ? P2 O51 1.500(4) . ? P2 O1 1.506(4) 2_455 ? P2 O2 1.510(4) 7_565 ? P2 O22 1.524(3) . ? Al1 O1 1.718(5) . ? Al1 O41 1.723(5) 8_544 ? Al1 O2 1.728(4) . ? Al1 O3 1.738(5) . ? P3 O23 1.513(3) . ? P3 O23 1.513(3) 7_566 ? P3 O23 1.513(3) 3_665 ? P3 O23 1.513(3) 6_656 ? O1 P2 1.506(4) 2 ? O41 Al1 1.723(5) 8_545 ? O51 H51 0.8200 . ? O2 P2 1.510(4) 6_655 ? N1 C3A 1.294(17) . ? N1 C3 1.379(12) . ? N1 C1 1.387(14) . ? N1 C5 1.394(15) . ? C1 C2 1.474(15) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C4 1.479(16) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C3A H3A1 0.9600 . ? C3A H3A2 0.9600 . ? C3A H3A3 0.9600 . ? C4 C5 1.514(15) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? 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 O21 P4 O42 107.7(3) . . ? O21 P4 O3 109.2(3) . . ? O42 P4 O3 109.8(5) . . ? O21 P4 O41 107.1(3) . . ? O42 P4 O41 116.9(5) . . ? O3 P4 O41 105.9(3) . . ? O42A P4A O3 111.8(5) . . ? O42A P4A O21 109.1(5) . . ? O3 P4A O21 110.4(3) . . ? O42A P4A O41 117.8(6) . . ? O3 P4A O41 104.7(3) . . ? O21 P4A O41 102.5(3) . . ? O11 P1 O11 108.50(14) 3_665 7_565 ? O11 P1 O11 111.4(3) 3_665 . ? O11 P1 O11 108.49(14) 7_565 . ? O11 P1 O11 108.50(14) 3_665 6_655 ? O11 P1 O11 111.4(3) 7_565 6_655 ? O11 P1 O11 108.49(14) . 6_655 ? O21 Al2 O22 110.12(18) . . ? O21 Al2 O11 110.14(19) . . ? O22 Al2 O11 110.2(2) . . ? O21 Al2 O23 110.9(2) . . ? O22 Al2 O23 108.85(18) . . ? O11 Al2 O23 106.65(18) . . ? O51 P2 O1 108.2(4) . 2_455 ? O51 P2 O2 111.3(3) . 7_565 ? O1 P2 O2 109.8(3) 2_455 7_565 ? O51 P2 O22 111.3(2) . . ? O1 P2 O22 108.5(3) 2_455 . ? O2 P2 O22 107.8(2) 7_565 . ? O1 Al1 O41 110.3(3) . 8_544 ? O1 Al1 O2 109.2(3) . . ? O41 Al1 O2 109.7(2) 8_544 . ? O1 Al1 O3 110.6(2) . . ? O41 Al1 O3 107.1(3) 8_544 . ? O2 Al1 O3 110.0(2) . . ? O23 P3 O23 108.80(14) . 7_566 ? O23 P3 O23 110.8(3) . 3_665 ? O23 P3 O23 108.80(14) 7_566 3_665 ? O23 P3 O23 108.80(14) . 6_656 ? O23 P3 O23 110.8(3) 7_566 6_656 ? O23 P3 O23 108.80(14) 3_665 6_656 ? P2 O22 Al2 151.2(2) . . ? P4 O21 P4A 45.35(16) . . ? P4 O21 Al2 152.6(3) . . ? P4A O21 Al2 149.0(3) . . ? P2 O1 Al1 160.0(3) 2 . ? P4A O3 P4 44.82(17) . . ? P4A O3 Al1 134.7(4) . . ? P4 O3 Al1 155.2(3) . . ? P3 O23 Al2 149.3(3) . . ? P4 O41 P4A 42.66(16) . . ? P4 O41 Al1 162.3(4) . 8_545 ? P4A O41 Al1 123.8(4) . 8_545 ? P2 O51 H51 109.5 . . ? P1 O11 Al2 153.7(3) . . ? P2 O2 Al1 154.2(4) 6_655 . ? C3A N1 C3 75.9(17) . . ? C3A N1 C1 136(2) . . ? C3 N1 C1 120.1(15) . . ? C3A N1 C5 114(2) . . ? C3 N1 C5 116.9(16) . . ? C1 N1 C5 96.0(13) . . ? N1 C1 C2 120.8(16) . . ? N1 C1 H1A 107.1 . . ? C2 C1 H1A 107.1 . . ? N1 C1 H1B 107.1 . . ? C2 C1 H1B 107.1 . . ? H1A C1 H1B 106.8 . . ? C1 C2 C4 95.5(15) . . ? C1 C2 H2A 112.6 . . ? C4 C2 H2A 112.6 . . ? C1 C2 H2B 112.6 . . ? C4 C2 H2B 112.6 . . ? H2A C2 H2B 110.1 . . ? N1 C3 H3A 109.5 . . ? N1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C3A H3A1 109.5 . . ? N1 C3A H3A2 109.5 . . ? H3A1 C3A H3A2 109.5 . . ? N1 C3A H3A3 109.5 . . ? H3A1 C3A H3A3 109.5 . . ? H3A2 C3A H3A3 109.5 . . ? C2 C4 C5 106.2(16) . . ? C2 C4 H4A 110.5 . . ? C5 C4 H4A 110.5 . . ? C2 C4 H4B 110.5 . . ? C5 C4 H4B 110.5 . . ? H4A C4 H4B 108.7 . . ? N1 C5 C4 108.1(14) . . ? N1 C5 H5A 110.1 . . ? C4 C5 H5A 110.1 . . ? N1 C5 H5B 110.1 . . ? C4 C5 H5B 110.1 . . ? H5A C5 H5B 108.4 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O51 H51 O42 0.82 2.04 2.478(9) 112.9 . _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 31.15 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.862 _refine_diff_density_min -1.093 _refine_diff_density_rms 0.168 data_compound3 _database_code_depnum_ccdc_archive 'CCDC 805445' #TrackingRef '- complete_final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'compound 3' _chemical_melting_point ? _chemical_formula_moiety 'Al2 H O12 P3, C5 H6 N' _chemical_formula_sum 'C5 H7 Al2 N O12 P3' _chemical_formula_weight 419.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' O O 0.0106 0.0060 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c 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 8.522(4) _cell_length_b 20.101(10) _cell_length_c 8.846(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.090(8) _cell_angle_gamma 90.00 _cell_volume 1413.8(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 619 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 23.73 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.973 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 844 _exptl_absorpt_coefficient_mu 0.611 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.940 _exptl_absorpt_correction_T_max 0.995 _exptl_absorpt_process_details sadabs _exptl_special_details ; Systematic absences suggest 2(1) screw axis and c-glide. These are not 100% perfect absences for all data but we believe this is due to weak data from twin crystals. Definite absences for reflections with I>3sigma(I) ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.69390 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'SRS daresbury laboratories' _diffrn_radiation_monochromator 'Si (111)' _diffrn_measurement_device_type 'Bruker Apex CCD' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8570 _diffrn_reflns_av_R_equivalents 0.1238 _diffrn_reflns_av_sigmaI/netI 0.1478 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 25.70 _reflns_number_total 2882 _reflns_number_gt 1662 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex' _computing_cell_refinement 'Bruker Apex' _computing_data_reduction 'Bruker Apex' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material 'Platon, (Spek, 2008)' _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^)+(0.0702P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2882 _refine_ls_number_parameters 212 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1253 _refine_ls_R_factor_gt 0.0653 _refine_ls_wR_factor_ref 0.1758 _refine_ls_wR_factor_gt 0.1482 _refine_ls_goodness_of_fit_ref 0.965 _refine_ls_restrained_S_all 0.965 _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 P1 P 0.4477(2) 0.59510(8) 0.91713(19) 0.0174(4) Uani 1 1 d . . . P2 P -0.0490(2) 0.74849(8) 0.92788(19) 0.0176(4) Uani 1 1 d . . . Al3 Al -0.3157(2) 0.78833(9) 0.5904(2) 0.0169(4) Uani 1 1 d . . . Al4 Al 0.1897(2) 0.70862(9) 0.7588(2) 0.0171(4) Uani 1 1 d . . . P5 P 0.4763(2) 0.80782(8) 0.82277(19) 0.0167(4) Uani 1 1 d . . . O1 O -0.1536(5) 0.7924(2) 0.7880(5) 0.0210(10) Uani 1 1 d . . . O2 O 0.3183(5) 0.6397(2) 0.7933(5) 0.0219(10) Uani 1 1 d . . . O3 O 0.0590(5) 0.7019(2) 0.8692(5) 0.0191(10) Uani 1 1 d . . . O4 O -0.1507(5) 0.7065(2) 0.9988(5) 0.0219(10) Uani 1 1 d . . . O5 O 0.3018(5) 0.7825(2) 0.8088(5) 0.0219(10) Uani 1 1 d . . . O6 O 0.4839(5) 0.5402(2) 0.8087(5) 0.0235(11) Uani 1 1 d . . . O7 O -0.3943(5) 0.7113(2) 0.4854(5) 0.0218(10) Uani 1 1 d . . . O8 O 0.0686(5) 0.7960(2) 1.0535(5) 0.0204(10) Uani 1 1 d . . . O9 O -0.4850(5) 0.7832(2) 0.6796(5) 0.0196(10) Uani 1 1 d . . . O10 O 0.6105(5) 0.6325(2) 1.0017(5) 0.0210(10) Uani 1 1 d . . . O11 O 0.4704(6) 0.8853(2) 0.8248(5) 0.0216(10) Uani 1 1 d D . . O12 O 0.3782(5) 0.5642(2) 1.0350(5) 0.0205(10) Uani 1 1 d . . . N1 N 0.0448(11) 0.9267(4) 0.8231(10) 0.063(2) Uani 1 1 d . . . H1 H 0.0091 0.8867 0.8242 0.076 Uiso 1 1 calc R . . C2 C -0.0418(13) 0.9668(6) 0.7043(12) 0.061(3) Uani 1 1 d . . . H2 H -0.1392 0.9516 0.6235 0.073 Uiso 1 1 calc R . . C3 C 0.0110(12) 1.0294(6) 0.7004(10) 0.057(3) Uani 1 1 d . . . H3 H -0.0506 1.0580 0.6178 0.069 Uiso 1 1 calc R . . C4 C 0.1594(13) 1.0516(5) 0.8213(13) 0.058(3) Uani 1 1 d . . . H4 H 0.1997 1.0944 0.8189 0.070 Uiso 1 1 calc R . . C5 C 0.2440(10) 1.0078(6) 0.9443(10) 0.054(3) Uani 1 1 d . . . H5 H 0.3408 1.0213 1.0282 0.065 Uiso 1 1 calc R . . C6 C 0.1861(13) 0.9458(5) 0.9420(11) 0.058(3) Uani 1 1 d . . . H6 H 0.2440 0.9159 1.0232 0.070 Uiso 1 1 calc R . . H11 H 0.411(11) 0.905(4) 0.723(7) 0.07(3) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0181(8) 0.0151(8) 0.0179(8) -0.0002(7) 0.0052(6) -0.0002(7) P2 0.0154(7) 0.0220(9) 0.0141(7) -0.0004(7) 0.0038(6) -0.0007(7) Al3 0.0162(9) 0.0191(10) 0.0145(9) 0.0002(8) 0.0044(7) 0.0009(8) Al4 0.0170(9) 0.0181(10) 0.0155(9) 0.0006(8) 0.0049(7) 0.0012(8) P5 0.0169(8) 0.0151(8) 0.0177(8) 0.0011(7) 0.0057(6) 0.0006(6) O1 0.020(2) 0.025(3) 0.016(2) 0.0049(19) 0.0036(18) -0.0029(19) O2 0.021(2) 0.022(3) 0.019(2) 0.0010(19) 0.0036(18) 0.0024(18) O3 0.022(2) 0.017(2) 0.022(2) 0.0000(18) 0.0117(18) -0.0026(18) O4 0.024(2) 0.024(3) 0.022(2) 0.0009(19) 0.0143(19) 0.000(2) O5 0.020(2) 0.018(2) 0.025(2) -0.0021(19) 0.0057(18) -0.0001(19) O6 0.031(2) 0.019(2) 0.022(2) -0.0007(19) 0.011(2) 0.004(2) O7 0.021(2) 0.026(2) 0.018(2) -0.0030(19) 0.0050(17) 0.0018(19) O8 0.022(2) 0.017(2) 0.018(2) -0.0025(18) 0.0016(17) -0.0039(19) O9 0.018(2) 0.021(2) 0.020(2) -0.0004(19) 0.0067(17) -0.0001(18) O10 0.017(2) 0.024(2) 0.023(2) -0.0011(19) 0.0095(18) -0.0015(18) O11 0.029(2) 0.017(2) 0.016(2) 0.0019(19) 0.0054(19) 0.0024(19) O12 0.024(2) 0.015(2) 0.022(2) -0.0029(18) 0.0075(19) 0.0001(18) N1 0.059(5) 0.051(5) 0.082(6) -0.011(5) 0.028(5) -0.002(4) C2 0.056(6) 0.070(7) 0.051(6) -0.006(5) 0.011(5) 0.013(6) C3 0.056(6) 0.081(8) 0.032(5) 0.023(5) 0.012(4) 0.035(6) C4 0.078(7) 0.030(5) 0.087(7) -0.005(5) 0.055(6) -0.003(5) C5 0.029(4) 0.094(8) 0.031(4) -0.012(5) 0.001(4) 0.005(5) C6 0.073(7) 0.062(7) 0.043(5) 0.024(5) 0.024(5) 0.039(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 O12 1.506(5) . ? P1 O10 1.518(4) . ? P1 O2 1.533(4) . ? P1 O6 1.565(5) . ? P2 O4 1.500(5) . ? P2 O1 1.521(4) . ? P2 O3 1.529(5) . ? P2 O8 1.533(4) . ? Al3 O10 1.785(5) 4_475 ? Al3 O1 1.798(4) . ? Al3 O7 1.805(5) . ? Al3 O4 1.861(5) 4_575 ? Al3 O9 1.880(5) . ? Al4 O2 1.724(5) . ? Al4 O3 1.732(5) . ? Al4 O5 1.734(5) . ? Al4 O8 1.739(4) 4_575 ? P5 O9 1.503(5) 1_655 ? P5 O7 1.514(4) 4_676 ? P5 O5 1.535(5) . ? P5 O11 1.559(5) . ? O11 H11 0.94(4) . ? N1 C2 1.319(12) . ? N1 C6 1.339(12) . ? N1 H1 0.8600 . ? C2 C3 1.342(15) . ? C2 H2 0.9300 . ? C3 C4 1.403(13) . ? C3 H3 0.9300 . ? C4 C5 1.384(13) . ? C4 H4 0.9300 . ? C5 C6 1.337(14) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? 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 O12 P1 O10 112.4(2) . . ? O12 P1 O2 112.1(3) . . ? O10 P1 O2 110.9(3) . . ? O12 P1 O6 110.3(3) . . ? O10 P1 O6 107.7(3) . . ? O2 P1 O6 103.0(2) . . ? O4 P2 O1 114.2(3) . . ? O4 P2 O3 107.8(2) . . ? O1 P2 O3 109.1(3) . . ? O4 P2 O8 111.9(3) . . ? O1 P2 O8 105.5(2) . . ? O3 P2 O8 108.2(2) . . ? O10 Al3 O1 114.3(2) 4_475 . ? O10 Al3 O7 122.1(2) 4_475 . ? O1 Al3 O7 123.5(2) . . ? O10 Al3 O4 87.7(2) 4_475 4_575 ? O1 Al3 O4 89.1(2) . 4_575 ? O7 Al3 O4 91.3(2) . 4_575 ? O10 Al3 O9 91.8(2) 4_475 . ? O1 Al3 O9 91.8(2) . . ? O7 Al3 O9 88.3(2) . . ? O4 Al3 O9 179.1(2) 4_575 . ? O2 Al4 O3 109.5(2) . . ? O2 Al4 O5 112.7(2) . . ? O3 Al4 O5 109.3(2) . . ? O2 Al4 O8 104.0(2) . 4_575 ? O3 Al4 O8 108.9(2) . 4_575 ? O5 Al4 O8 112.2(2) . 4_575 ? O9 P5 O7 114.3(3) 1_655 4_676 ? O9 P5 O5 108.8(2) 1_655 . ? O7 P5 O5 110.2(3) 4_676 . ? O9 P5 O11 110.9(3) 1_655 . ? O7 P5 O11 105.0(2) 4_676 . ? O5 P5 O11 107.3(3) . . ? P2 O1 Al3 141.7(3) . . ? P1 O2 Al4 147.6(3) . . ? P2 O3 Al4 137.0(3) . . ? P2 O4 Al3 142.3(3) . 4_576 ? P5 O5 Al4 137.2(3) . . ? P5 O7 Al3 135.7(3) 4_475 . ? P2 O8 Al4 135.3(3) . 4_576 ? P5 O9 Al3 140.4(3) 1_455 . ? P1 O10 Al3 140.6(3) . 4_676 ? P5 O11 H11 115(5) . . ? C2 N1 C6 122.5(9) . . ? C2 N1 H1 118.7 . . ? C6 N1 H1 118.7 . . ? N1 C2 C3 119.8(9) . . ? N1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C2 C3 C4 119.8(8) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 117.9(9) . . ? C5 C4 H4 121.0 . . ? C3 C4 H4 121.0 . . ? C6 C5 C4 119.8(8) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 N1 120.1(8) . . ? C5 C6 H6 119.9 . . ? N1 C6 H6 119.9 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O11 H11 O12 0.94(4) 1.70(6) 2.602(6) 158(9) 4_575 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.70 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.656 _refine_diff_density_min -0.673 _refine_diff_density_rms 0.141 # Attachment '- stan429.cif' data_stan249 _database_code_depnum_ccdc_archive 'CCDC 805446' #TrackingRef '- stan429.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4.67 H6.67 Al2 F0.67 N0.67 O8 P2' _chemical_formula_weight 328.67 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' O O 0.0106 0.0060 '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.154(4) _cell_length_b 9.239(4) _cell_length_c 9.345(4) _cell_angle_alpha 78.231(5) _cell_angle_beta 87.485(6) _cell_angle_gamma 87.179(5) _cell_volume 772.3(5) _cell_formula_units_Z 3 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 279 _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 17.26 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.120 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 496 _exptl_absorpt_coefficient_mu 0.638 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.63070 _diffrn_radiation_type ? _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator silicon _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8670 _diffrn_reflns_av_R_equivalents 0.1415 _diffrn_reflns_av_sigmaI/netI 0.2394 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 26.02 _reflns_number_total 4269 _reflns_number_gt 2022 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0835P)^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 4269 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1756 _refine_ls_R_factor_gt 0.0956 _refine_ls_wR_factor_ref 0.2747 _refine_ls_wR_factor_gt 0.2129 _refine_ls_goodness_of_fit_ref 0.955 _refine_ls_restrained_S_all 0.955 _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 P1 P 0.3830(2) 0.1397(2) 0.3214(2) 0.0110(4) Uani 1 1 d . . . P2 P 0.8126(2) 0.1111(2) 0.1054(2) 0.0109(4) Uani 1 1 d . . . P3 P 0.3513(2) 0.3306(2) -0.1381(2) 0.0116(4) Uani 1 1 d . . . Al2 Al 0.6307(3) -0.1032(3) 0.3397(3) 0.0130(5) Uani 1 1 d . . . Al3 Al 0.8371(3) -0.1327(3) -0.0732(3) 0.0129(5) Uani 1 1 d . . . Al1 Al 0.5615(3) 0.3684(2) 0.0920(3) 0.0112(5) Uani 1 1 d . . . F1 F 0.3947(5) 0.4977(4) 0.0805(5) 0.0101(9) Uani 1 1 d . . . O9 O 0.4640(6) 0.2652(5) -0.0261(6) 0.0109(11) Uani 1 1 d . . . O7 O 0.7875(6) 0.0351(6) -0.0223(6) 0.0125(11) Uani 1 1 d . . . O11 O 0.3516(6) 0.4978(6) -0.1870(6) 0.0118(11) Uani 1 1 d . . . O5 O 0.7310(6) 0.2580(5) 0.0871(6) 0.0111(11) Uani 1 1 d . . . O6 O 0.7680(6) 0.0094(6) 0.2497(6) 0.0131(11) Uani 1 1 d . . . O1 O 0.4855(6) 0.2644(6) 0.2661(6) 0.0132(11) Uani 1 1 d . . . O8 O 0.9768(6) 0.1353(6) 0.1120(6) 0.0131(11) Uani 1 1 d . . . O10 O 0.1985(6) 0.2814(6) -0.0709(6) 0.0136(11) Uani 1 1 d . . . O2 O 0.2474(6) 0.1491(6) 0.2292(6) 0.0138(11) Uani 1 1 d . . . O3 O 0.3260(6) 0.1490(6) 0.4766(5) 0.0113(11) Uani 1 1 d . . . O12 O 0.3750(6) 0.2647(6) -0.2770(6) 0.0136(12) Uani 1 1 d . . . O4 O 0.4608(6) -0.0104(6) 0.3248(6) 0.0141(12) Uani 1 1 d . . . C3 C 0.2430(13) 0.7712(13) 0.4904(13) 0.043(3) Uani 1 1 d . . . H3 H 0.2724 0.8208 0.5607 0.052 Uiso 1 1 calc R . . N1 N 0.1554(9) 0.6212(9) 0.2906(10) 0.0311(19) Uani 1 1 d . . . C5 C 0.0784(11) 0.7429(11) 0.3127(11) 0.030(2) Uani 1 1 d . . . H5 H -0.0070 0.7718 0.2624 0.036 Uiso 1 1 calc R . . C7 C -0.0133(13) 0.4230(12) 0.2907(13) 0.043(3) Uani 1 1 d . . . H7A H -0.0559 0.3618 0.2334 0.064 Uiso 1 1 calc R . . H7B H -0.0894 0.4796 0.3309 0.064 Uiso 1 1 calc R . . H7C H 0.0395 0.3617 0.3687 0.064 Uiso 1 1 calc R . . C1 C 0.2720(10) 0.5723(11) 0.3689(11) 0.028(2) Uani 1 1 d . . . H1 H 0.3223 0.4861 0.3547 0.034 Uiso 1 1 calc R . . C6 C 0.0898(11) 0.5261(12) 0.1953(11) 0.035(2) Uani 1 1 d . . . H6A H 0.0374 0.5886 0.1160 0.042 Uiso 1 1 calc R . . H6B H 0.1668 0.4699 0.1535 0.042 Uiso 1 1 calc R . . C4 C 0.1223(13) 0.8228(12) 0.4055(13) 0.039(3) Uani 1 1 d . . . H4 H 0.0733 0.9116 0.4134 0.046 Uiso 1 1 calc R . . C2 C 0.3179(11) 0.6430(11) 0.4663(11) 0.031(2) Uani 1 1 d . . . H2 H 0.4005 0.6073 0.5191 0.038 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 0.0134(10) 0.0102(9) 0.0102(9) -0.0042(7) -0.0025(8) -0.0002(7) P2 0.0126(9) 0.0096(9) 0.0118(10) -0.0050(7) -0.0031(7) 0.0004(7) P3 0.0150(10) 0.0101(9) 0.0112(10) -0.0055(7) -0.0021(8) 0.0000(7) Al2 0.0166(12) 0.0130(12) 0.0111(12) -0.0060(9) -0.0029(9) -0.0008(9) Al3 0.0137(12) 0.0125(12) 0.0146(12) -0.0076(9) -0.0012(9) -0.0009(9) Al1 0.0160(12) 0.0084(11) 0.0105(11) -0.0052(9) -0.0023(9) 0.0015(9) F1 0.014(2) 0.007(2) 0.011(2) -0.0040(16) -0.0009(17) -0.0002(16) O9 0.012(3) 0.009(2) 0.012(3) -0.001(2) -0.007(2) -0.0021(19) O7 0.020(3) 0.011(3) 0.008(3) -0.005(2) -0.005(2) 0.002(2) O11 0.011(3) 0.012(3) 0.015(3) -0.007(2) -0.006(2) 0.002(2) O5 0.012(3) 0.008(2) 0.014(3) -0.001(2) -0.006(2) 0.0027(19) O6 0.014(3) 0.015(3) 0.012(3) -0.007(2) -0.003(2) 0.001(2) O1 0.018(3) 0.012(3) 0.011(3) -0.004(2) 0.000(2) 0.001(2) O8 0.012(3) 0.011(3) 0.015(3) 0.000(2) -0.005(2) 0.001(2) O10 0.015(3) 0.011(3) 0.016(3) -0.004(2) 0.001(2) -0.003(2) O2 0.014(3) 0.017(3) 0.012(3) -0.007(2) -0.003(2) 0.001(2) O3 0.012(3) 0.014(3) 0.008(3) -0.002(2) 0.001(2) -0.002(2) O12 0.024(3) 0.005(2) 0.015(3) -0.009(2) -0.007(2) 0.003(2) O4 0.013(3) 0.008(3) 0.023(3) -0.006(2) -0.003(2) 0.001(2) C3 0.052(7) 0.044(7) 0.041(7) -0.022(5) 0.000(6) -0.009(6) N1 0.029(4) 0.029(4) 0.037(5) -0.013(4) 0.003(4) 0.000(4) C5 0.026(5) 0.034(6) 0.033(6) -0.012(4) -0.008(4) 0.007(4) C7 0.047(7) 0.041(7) 0.046(7) -0.018(5) -0.007(6) -0.014(5) C1 0.019(4) 0.028(5) 0.036(6) -0.004(4) 0.000(4) 0.004(4) C6 0.025(5) 0.052(7) 0.026(5) -0.006(5) 0.008(4) -0.002(5) C4 0.047(7) 0.028(5) 0.043(7) -0.017(5) 0.007(5) 0.001(5) C2 0.032(5) 0.031(5) 0.032(6) -0.006(4) 0.001(4) -0.011(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O1 1.515(6) . ? P1 O4 1.523(5) . ? P1 O2 1.531(6) . ? P1 O3 1.538(5) . ? P2 O5 1.498(5) . ? P2 O6 1.530(6) . ? P2 O7 1.535(6) . ? P2 O8 1.536(6) . ? P3 O9 1.517(5) . ? P3 O11 1.519(5) . ? P3 O12 1.545(6) . ? P3 O10 1.557(6) . ? Al2 O12 1.715(5) 2_655 ? Al2 O4 1.735(6) . ? Al2 O3 1.740(6) 2_656 ? Al2 O6 1.746(6) . ? Al3 O2 1.717(6) 2_655 ? Al3 O8 1.726(6) 2_755 ? Al3 O7 1.745(6) . ? Al3 O10 1.749(6) 2_655 ? Al1 O5 1.818(6) . ? Al1 O1 1.840(6) . ? Al1 F1 1.862(5) 2_665 ? Al1 O9 1.878(6) . ? Al1 F1 1.885(5) . ? Al1 O11 1.885(6) 2_665 ? Al1 Al1 2.886(5) 2_665 ? F1 Al1 1.862(5) 2_665 ? O11 Al1 1.885(6) 2_665 ? O8 Al3 1.726(6) 2_755 ? O10 Al3 1.749(6) 2_655 ? O2 Al3 1.717(6) 2_655 ? O3 Al2 1.740(6) 2_656 ? O12 Al2 1.715(5) 2_655 ? C3 C2 1.393(15) . ? C3 C4 1.395(16) . ? C3 H3 0.9300 . ? N1 C1 1.329(12) . ? N1 C5 1.344(12) . ? N1 C6 1.531(13) . ? C5 C4 1.334(14) . ? C5 H5 0.9300 . ? C7 C6 1.504(14) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C1 C2 1.317(14) . ? C1 H1 0.9300 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C4 H4 0.9300 . ? C2 H2 0.9300 . ? 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 O1 P1 O4 111.1(3) . . ? O1 P1 O2 113.0(3) . . ? O4 P1 O2 108.2(3) . . ? O1 P1 O3 109.1(3) . . ? O4 P1 O3 109.2(3) . . ? O2 P1 O3 106.1(3) . . ? O5 P2 O6 111.2(3) . . ? O5 P2 O7 111.2(3) . . ? O6 P2 O7 109.6(3) . . ? O5 P2 O8 108.8(3) . . ? O6 P2 O8 106.7(3) . . ? O7 P2 O8 109.1(3) . . ? O9 P3 O11 114.8(3) . . ? O9 P3 O12 110.6(3) . . ? O11 P3 O12 107.0(3) . . ? O9 P3 O10 107.3(3) . . ? O11 P3 O10 110.5(3) . . ? O12 P3 O10 106.3(3) . . ? O12 Al2 O4 110.1(3) 2_655 . ? O12 Al2 O3 107.7(3) 2_655 2_656 ? O4 Al2 O3 108.9(3) . 2_656 ? O12 Al2 O6 112.0(3) 2_655 . ? O4 Al2 O6 111.3(3) . . ? O3 Al2 O6 106.7(3) 2_656 . ? O2 Al3 O8 107.2(3) 2_655 2_755 ? O2 Al3 O7 111.4(3) 2_655 . ? O8 Al3 O7 107.9(3) 2_755 . ? O2 Al3 O10 111.6(3) 2_655 2_655 ? O8 Al3 O10 107.9(3) 2_755 2_655 ? O7 Al3 O10 110.7(3) . 2_655 ? O5 Al1 O1 97.4(3) . . ? O5 Al1 F1 94.7(2) . 2_665 ? O1 Al1 F1 167.7(2) . 2_665 ? O5 Al1 O9 93.8(2) . . ? O1 Al1 O9 95.2(3) . . ? F1 Al1 O9 85.9(2) 2_665 . ? O5 Al1 F1 173.9(3) . . ? O1 Al1 F1 88.6(2) . . ? F1 Al1 F1 79.2(2) 2_665 . ? O9 Al1 F1 86.9(2) . . ? O5 Al1 O11 92.5(3) . 2_665 ? O1 Al1 O11 91.9(3) . 2_665 ? F1 Al1 O11 85.7(2) 2_665 2_665 ? O9 Al1 O11 169.9(3) . 2_665 ? F1 Al1 O11 86.0(2) . 2_665 ? O5 Al1 Al1 134.6(2) . 2_665 ? O1 Al1 Al1 127.9(2) . 2_665 ? F1 Al1 Al1 39.90(14) 2_665 2_665 ? O9 Al1 Al1 85.35(19) . 2_665 ? F1 Al1 Al1 39.34(14) . 2_665 ? O11 Al1 Al1 84.59(19) 2_665 2_665 ? Al1 F1 Al1 100.8(2) 2_665 . ? P3 O9 Al1 126.2(3) . . ? P2 O7 Al3 137.7(3) . . ? P3 O11 Al1 126.8(3) . 2_665 ? P2 O5 Al1 151.0(4) . . ? P2 O6 Al2 144.2(4) . . ? P1 O1 Al1 139.5(4) . . ? P2 O8 Al3 161.4(4) . 2_755 ? P3 O10 Al3 126.9(3) . 2_655 ? P1 O2 Al3 151.9(4) . 2_655 ? P1 O3 Al2 143.5(4) . 2_656 ? P3 O12 Al2 142.7(4) . 2_655 ? P1 O4 Al2 143.6(4) . . ? C2 C3 C4 117.8(10) . . ? C2 C3 H3 121.1 . . ? C4 C3 H3 121.1 . . ? C1 N1 C5 120.2(9) . . ? C1 N1 C6 120.7(8) . . ? C5 N1 C6 118.1(8) . . ? C4 C5 N1 121.2(10) . . ? C4 C5 H5 119.4 . . ? N1 C5 H5 119.4 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C2 C1 N1 121.5(10) . . ? C2 C1 H1 119.3 . . ? N1 C1 H1 119.3 . . ? C7 C6 N1 107.9(8) . . ? C7 C6 H6A 110.1 . . ? N1 C6 H6A 110.1 . . ? C7 C6 H6B 110.1 . . ? N1 C6 H6B 110.1 . . ? H6A C6 H6B 108.4 . . ? C5 C4 C3 119.0(10) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? C1 C2 C3 120.1(10) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.157 _refine_diff_density_min -0.994 _refine_diff_density_rms 0.232