# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common AlPO-JU89-1 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H22 Al6 F6 N3 O18 P3' _chemical_formula_weight 769.04 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 Trigonal _symmetry_space_group_name_H-M P3(1)21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' 'y, x, -z' 'x-y, -y, -z+2/3' '-x, -x+y, -z+1/3' _cell_length_a 9.3415(5) _cell_length_b 9.3415(5) _cell_length_c 6.9955(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 528.67(7) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 388 _exptl_absorpt_coefficient_mu 0.684 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.929 _exptl_absorpt_correction_T_max 0.940 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 5.0cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 3700 _diffrn_reflns_av_R_equivalents 0.0474 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 28.31 _reflns_number_total 889 _reflns_number_gt 811 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0727P)^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 ? _chemical_absolute_configuration ad _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881. 67 Friedel pairs' _refine_ls_abs_structure_Flack -0.04(27) _refine_ls_number_reflns 889 _refine_ls_number_parameters 66 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0430 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.1053 _refine_ls_wR_factor_gt 0.1028 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.079 _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 Al1 Al 0.16196(12) 0.52127(14) 0.05625(13) 0.0154(3) Uani 1 1 d . . . P1 P 0.44930(13) 0.44930(13) 0.0000 0.0148(3) Uani 1 2 d S . . F1 F 0.0000 0.3183(3) 0.1667 0.0201(6) Uani 1 2 d S . . F2 F 0.0000 0.5686(3) 0.1667 0.0221(6) Uani 1 2 d S . . O1 O 0.3018(3) 0.7302(3) -0.0401(3) 0.0183(5) Uani 1 1 d . . . H1 H 0.3605 0.8310 0.0429 0.022 Uiso 1 1 d R . . O2 O 0.2783(3) 0.4270(4) -0.0408(3) 0.0215(6) Uani 1 1 d . . . O3 O 0.0333(3) 0.4675(3) -0.1642(3) 0.0188(5) Uani 1 1 d . . . C C -0.1266(14) 0.7792(17) 0.0431(12) 0.066(3) Uani 0.67 1 d PU . . N N 0.0000 0.895(2) 0.1667 0.271(11) Uani 1 2 d SU . . 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 0.0146(5) 0.0184(5) 0.0125(4) 0.0006(4) -0.0001(4) 0.0078(4) P1 0.0178(5) 0.0178(5) 0.0117(5) 0.0000(2) 0.0000(2) 0.0111(5) F1 0.0183(15) 0.0213(11) 0.0199(15) 0.0008(6) 0.0015(12) 0.0091(7) F2 0.0225(16) 0.0232(11) 0.0204(14) 0.0002(6) 0.0004(12) 0.0113(8) O1 0.0221(13) 0.0141(11) 0.0132(10) 0.0004(9) -0.0001(9) 0.0048(10) O2 0.0203(12) 0.0273(14) 0.0202(12) -0.0047(10) -0.0015(11) 0.0143(11) O3 0.0170(12) 0.0208(13) 0.0164(11) 0.0005(10) -0.0025(9) 0.0079(11) C 0.082(8) 0.116(9) 0.034(4) -0.017(5) -0.013(4) 0.074(7) N 0.26(2) 0.221(17) 0.34(3) 0.016(12) 0.03(2) 0.131(12) _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 Al1 O2 1.837(3) . ? Al1 O1 1.850(2) . ? Al1 O3 1.863(2) . ? Al1 O1 1.874(2) 2_665 ? Al1 F1 1.901(2) . ? Al1 F2 1.936(2) . ? P1 O3 1.530(2) 2_665 ? P1 O3 1.530(2) 5_664 ? P1 O2 1.531(3) . ? P1 O2 1.531(3) 4 ? F1 Al1 1.901(2) 6 ? F2 Al1 1.936(2) 6 ? O1 Al1 1.874(2) 3_564 ? O3 P1 1.530(2) 3_564 ? C N 1.428(13) . ? C C 1.64(2) 4_465 ? N C 1.428(13) 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 O2 Al1 O1 95.50(12) . . ? O2 Al1 O3 91.25(11) . . ? O1 Al1 O3 90.16(11) . . ? O2 Al1 O1 94.28(12) . 2_665 ? O1 Al1 O1 92.87(11) . 2_665 ? O3 Al1 O1 173.41(12) . 2_665 ? O2 Al1 F1 92.21(12) . . ? O1 Al1 F1 172.26(13) . . ? O3 Al1 F1 89.03(9) . . ? O1 Al1 F1 87.18(8) 2_665 . ? O2 Al1 F2 166.88(13) . . ? O1 Al1 F2 97.17(12) . . ? O3 Al1 F2 85.36(8) . . ? O1 Al1 F2 88.46(8) 2_665 . ? F1 Al1 F2 75.08(11) . . ? O3 P1 O3 104.9(2) 2_665 5_664 ? O3 P1 O2 111.41(13) 2_665 . ? O3 P1 O2 110.69(13) 5_664 . ? O3 P1 O2 110.69(13) 2_665 4 ? O3 P1 O2 111.41(13) 5_664 4 ? O2 P1 O2 107.7(2) . 4 ? Al1 F1 Al1 106.30(16) 6 . ? Al1 F2 Al1 103.53(15) 6 . ? Al1 O1 Al1 138.69(14) . 3_564 ? P1 O2 Al1 133.89(17) . . ? P1 O3 Al1 140.42(16) 3_564 . ? N C C 106.1(10) . 4_465 ? C N C 139.6(19) 6 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.376 _refine_diff_density_min -0.367 _refine_diff_density_rms 0.106 _database_code_depnum_ccdc_archive 'CCDC 948288' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common AlPO-JU89-2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H22 Al6 F6 N3 O18 P3' _chemical_formula_weight 769.04 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 Trigonal _symmetry_space_group_name_H-M P3(1)21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' 'y, x, -z' 'x-y, -y, -z+2/3' '-x, -x+y, -z+1/3' _cell_length_a 9.3421(14) _cell_length_b 9.3421(14) _cell_length_c 6.996(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 528.8(2) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.415 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 388 _exptl_absorpt_coefficient_mu 0.684 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.929 _exptl_absorpt_correction_T_max 0.940 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 5.0cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 3881 _diffrn_reflns_av_R_equivalents 0.0461 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 28.31 _reflns_number_total 892 _reflns_number_gt 820 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0637P)^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 ? _chemical_absolute_configuration ad _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881. 67 Friedel pairs' _refine_ls_abs_structure_Flack 0.19(24) _refine_ls_number_reflns 892 _refine_ls_number_parameters 69 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0386 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0942 _refine_ls_wR_factor_gt 0.0904 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 Al1 Al 0.47892(12) 0.83800(11) 0.94364(12) 0.0091(2) Uani 1 1 d . . . P1 P 0.55059(12) 0.55059(12) 1.0000 0.0084(2) Uani 1 2 d S . . F1 F 0.6818(3) 1.0000 0.8333 0.0135(6) Uani 1 2 d S . . F2 F 0.4317(3) 1.0000 0.8333 0.0156(6) Uani 1 2 d S . . O1 O 0.5734(3) 0.7216(3) 1.0409(3) 0.0138(5) Uani 1 1 d . . . O2 O 0.5325(3) 0.9670(3) 1.1635(3) 0.0125(5) Uani 1 1 d . . . O3 O 0.2701(3) 0.6986(3) 1.0404(3) 0.0122(5) Uani 1 1 d . . . H1 H 0.204(5) 0.652(5) 0.968(5) 0.015 Uiso 1 1 d . . . N N 0.102(3) 1.0000 0.8333 0.38(2) Uani 1 2 d S . . C C 0.0965(12) 0.8725(12) 0.7110(12) 0.058(3) Uani 0.67 1 d P . . 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 0.0115(5) 0.0083(4) 0.0068(4) -0.0004(3) 0.0006(3) 0.0044(4) P1 0.0110(4) 0.0110(4) 0.0058(4) -0.00004(19) 0.00004(19) 0.0075(5) F1 0.0153(10) 0.0121(13) 0.0121(13) 0.0019(10) 0.0009(5) 0.0061(7) F2 0.0160(10) 0.0157(14) 0.0150(12) 0.0001(11) 0.0000(5) 0.0079(7) O1 0.0191(12) 0.0116(11) 0.0138(10) -0.0032(9) -0.0060(9) 0.0100(10) O2 0.0137(11) 0.0120(11) 0.0095(9) -0.0011(7) 0.0019(8) 0.0047(10) O3 0.0082(10) 0.0160(12) 0.0075(9) -0.0008(8) -0.0019(8) 0.0024(9) N 0.25(2) 0.35(4) 0.57(6) 0.21(4) 0.10(2) 0.173(19) C 0.042(5) 0.057(6) 0.045(5) -0.008(4) 0.004(3) 0.002(4) _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 Al1 O1 1.840(2) . ? Al1 O3 1.849(2) . ? Al1 O2 1.861(2) . ? Al1 O3 1.872(2) 3_564 ? Al1 F1 1.900(2) . ? Al1 F2 1.9361(19) . ? P1 O1 1.529(2) 4_557 ? P1 O1 1.529(2) . ? P1 O2 1.533(2) 3_564 ? P1 O2 1.533(2) 6_657 ? F1 Al1 1.900(2) 5_676 ? F2 Al1 1.9361(19) 5_676 ? O2 P1 1.533(2) 2_665 ? O3 Al1 1.872(2) 2_665 ? O3 H1 0.75(4) . ? N C 1.446(13) . ? N C 1.446(13) 5_676 ? C C 1.68(2) 6_556 ? 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 Al1 O3 95.57(11) . . ? O1 Al1 O2 91.36(10) . . ? O3 Al1 O2 90.05(11) . . ? O1 Al1 O3 94.22(11) . 3_564 ? O3 Al1 O3 92.94(10) . 3_564 ? O2 Al1 O3 173.38(11) . 3_564 ? O1 Al1 F1 92.24(11) . . ? O3 Al1 F1 172.15(12) . . ? O2 Al1 F1 88.95(8) . . ? O3 Al1 F1 87.28(8) 3_564 . ? O1 Al1 F2 166.84(11) . . ? O3 Al1 F2 97.13(11) . . ? O2 Al1 F2 85.19(8) . . ? O3 Al1 F2 88.58(8) 3_564 . ? F1 Al1 F2 75.04(10) . . ? O1 P1 O1 107.4(2) 4_557 . ? O1 P1 O2 110.57(12) 4_557 3_564 ? O1 P1 O2 111.57(11) . 3_564 ? O1 P1 O2 111.57(11) 4_557 6_657 ? O1 P1 O2 110.57(12) . 6_657 ? O2 P1 O2 105.20(18) 3_564 6_657 ? Al1 F1 Al1 106.38(15) 5_676 . ? Al1 F2 Al1 103.55(14) 5_676 . ? P1 O1 Al1 133.72(15) . . ? P1 O2 Al1 140.48(14) 2_665 . ? Al1 O3 Al1 138.92(13) . 2_665 ? Al1 O3 H1 116(3) . . ? Al1 O3 H1 105(3) 2_665 . ? C N C 136(2) . 5_676 ? N C C 104.3(12) . 6_556 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.702 _refine_diff_density_min -0.302 _refine_diff_density_rms 0.101 _database_code_depnum_ccdc_archive 'CCDC 948289' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common AlPO-JU89-3 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H22 Al6 F6 N3 O18 P3' _chemical_formula_weight 769.04 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 Trigonal _symmetry_space_group_name_H-M P3(1)21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' 'y, x, -z' 'x-y, -y, -z+2/3' '-x, -x+y, -z+1/3' _cell_length_a 9.3411(13) _cell_length_b 9.3411(13) _cell_length_c 6.9932(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 528.45(18) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.417 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 388 _exptl_absorpt_coefficient_mu 0.684 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.929 _exptl_absorpt_correction_T_max 0.940 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 5.0cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 3924 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0271 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 28.16 _reflns_number_total 885 _reflns_number_gt 846 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0550P)^2^+0.2383P] 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 ? _chemical_absolute_configuration ad _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881. 66 Friedel pairs' _refine_ls_abs_structure_Flack 0.00(20) _refine_ls_number_reflns 885 _refine_ls_number_parameters 66 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0314 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0819 _refine_ls_wR_factor_gt 0.0805 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.078 _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 0.0000 0.44936(9) 0.1667 0.0085(2) Uani 1 2 d S . . Al1 Al -0.35925(10) 0.16199(9) 0.22307(10) 0.00947(19) Uani 1 1 d . . . F1 F -0.3178(2) 0.0000 0.3333 0.0136(4) Uani 1 2 d S . . F2 F -0.5683(2) 0.0000 0.3333 0.0160(5) Uani 1 2 d S . . O1 O -0.4289(2) 0.3014(2) 0.1271(2) 0.0122(4) Uani 1 1 d . . . H1 H -0.4465 0.3679 0.1982 0.015 Uiso 1 1 d R . . O2 O -0.1485(2) 0.2785(2) 0.1260(3) 0.0148(4) Uani 1 1 d . . . O3 O 0.0329(2) 0.5656(2) -0.0030(2) 0.0127(4) Uani 1 1 d . . . C1 C -0.7789(11) 0.1268(10) 0.4562(9) 0.058(2) Uani 0.67 1 d PD . . N1 N -0.900(2) 0.0000 0.3333 0.372(19) Uani 1 2 d SD . . 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 0.0071(4) 0.0111(3) 0.0060(4) 0.00007(15) 0.0001(3) 0.0036(2) Al1 0.0112(4) 0.0089(3) 0.0066(3) -0.0002(2) -0.0008(3) 0.0038(3) F1 0.0150(8) 0.0124(10) 0.0126(10) 0.0027(8) 0.0014(4) 0.0062(5) F2 0.0167(8) 0.0174(11) 0.0144(10) 0.0012(9) 0.0006(4) 0.0087(6) O1 0.0204(9) 0.0142(9) 0.0074(7) -0.0009(6) -0.0001(7) 0.0125(7) O2 0.0130(9) 0.0114(8) 0.0134(8) -0.0025(7) 0.0028(7) 0.0012(7) O3 0.0123(8) 0.0170(9) 0.0089(8) 0.0041(7) 0.0023(6) 0.0074(7) C1 0.102(6) 0.060(5) 0.036(3) -0.001(3) -0.009(4) 0.059(5) N1 0.25(2) 0.31(3) 0.58(6) 0.16(4) 0.079(19) 0.155(16) _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 O2 1.5294(18) . ? P1 O2 1.5294(18) 6 ? P1 O3 1.5323(18) 6 ? P1 O3 1.5323(18) . ? Al1 O2 1.8378(19) . ? Al1 O1 1.8487(18) . ? Al1 O3 1.8622(17) 4_455 ? Al1 O1 1.8748(18) 2_565 ? Al1 F1 1.9029(16) . ? Al1 F2 1.9343(15) . ? F1 Al1 1.9029(16) 5 ? F2 Al1 1.9343(15) 5 ? O1 Al1 1.8748(18) 3_454 ? O3 Al1 1.8622(17) 4_565 ? C1 N1 1.442(9) . ? C1 C1 1.645(13) 4_466 ? N1 C1 1.442(9) 5 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 P1 O2 107.68(17) . 6 ? O2 P1 O3 111.49(10) . 6 ? O2 P1 O3 110.58(10) 6 6 ? O2 P1 O3 110.58(10) . . ? O2 P1 O3 111.49(10) 6 . ? O3 P1 O3 105.07(14) 6 . ? O2 Al1 O1 95.66(9) . . ? O2 Al1 O3 91.34(8) . 4_455 ? O1 Al1 O3 90.26(8) . 4_455 ? O2 Al1 O1 94.21(9) . 2_565 ? O1 Al1 O1 92.97(8) . 2_565 ? O3 Al1 O1 173.27(9) 4_455 2_565 ? O2 Al1 F1 92.11(9) . . ? O1 Al1 F1 172.20(10) . . ? O3 Al1 F1 88.90(6) 4_455 . ? O1 Al1 F1 87.10(6) 2_565 . ? O2 Al1 F2 166.84(9) . . ? O1 Al1 F2 97.06(9) . . ? O3 Al1 F2 85.23(6) 4_455 . ? O1 Al1 F2 88.52(6) 2_565 . ? F1 Al1 F2 75.14(8) . . ? Al1 F1 Al1 106.08(12) 5 . ? Al1 F2 Al1 103.64(11) . 5 ? Al1 O1 Al1 138.60(10) . 3_454 ? P1 O2 Al1 133.90(12) . . ? P1 O3 Al1 140.34(12) . 4_565 ? N1 C1 C1 104.6(9) . 4_466 ? C1 N1 C1 136.3(16) 5 . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.16 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.741 _refine_diff_density_min -0.275 _refine_diff_density_rms 0.093 _database_code_depnum_ccdc_archive 'CCDC 948290' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common AlPO-JU89-4 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H22 Al6 F6 N3 O18 P3' _chemical_formula_weight 769.04 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 Trigonal _symmetry_space_group_name_H-M P3(1)21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' 'y, x, -z' 'x-y, -y, -z+2/3' '-x, -x+y, -z+1/3' _cell_length_a 9.3392(3) _cell_length_b 9.3392(3) _cell_length_c 6.9942(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 528.31(4) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.417 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 388 _exptl_absorpt_coefficient_mu 0.685 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.937 _exptl_absorpt_correction_T_max 0.947 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 5.0cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 3936 _diffrn_reflns_av_R_equivalents 0.0219 _diffrn_reflns_av_sigmaI/netI 0.0174 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 28.32 _reflns_number_total 893 _reflns_number_gt 866 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0456P)^2^+0.3771P] 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 ? _chemical_absolute_configuration ad _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881. 70 Friedel pairs' _refine_ls_abs_structure_Flack -0.08(19) _refine_ls_number_reflns 893 _refine_ls_number_parameters 66 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0271 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0735 _refine_ls_wR_factor_gt 0.0728 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _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 0.0000 0.44942(8) 0.1667 0.00836(18) Uani 1 2 d S . . Al1 Al -0.35912(9) 0.16199(8) 0.22298(9) 0.00904(17) Uani 1 1 d . . . F1 F -0.3178(2) 0.0000 0.3333 0.0139(4) Uani 1 2 d S . . F2 F -0.5684(2) 0.0000 0.3333 0.0154(4) Uani 1 2 d S . . O1 O -0.4289(2) 0.3013(2) 0.1268(2) 0.0122(3) Uani 1 1 d . . . H1 H -0.4633 0.3510 0.2093 0.015 Uiso 1 1 d R . . O2 O -0.1485(2) 0.2784(2) 0.1260(2) 0.0147(3) Uani 1 1 d . . . O3 O -0.0327(2) 0.53317(19) 0.3364(2) 0.0123(3) Uani 1 1 d . . . C1 C -0.7776(12) 0.1263(9) 0.4542(9) 0.0569(18) Uani 0.67 1 d P . . N1 N -0.896(2) 0.0000 0.3333 0.382(19) Uani 1 2 d S . . 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 0.0068(4) 0.0108(3) 0.0062(3) 0.00019(13) 0.0004(3) 0.00341(18) Al1 0.0106(3) 0.0081(3) 0.0068(3) -0.0003(2) -0.0011(2) 0.0035(2) F1 0.0146(7) 0.0122(9) 0.0140(9) 0.0020(7) 0.0010(4) 0.0061(5) F2 0.0165(7) 0.0161(10) 0.0135(8) 0.0012(8) 0.0006(4) 0.0081(5) O1 0.0200(8) 0.0139(8) 0.0079(6) -0.0006(6) 0.0005(6) 0.0124(6) O2 0.0132(8) 0.0118(8) 0.0132(7) -0.0028(6) 0.0024(6) 0.0019(7) O3 0.0117(7) 0.0140(8) 0.0085(6) -0.0021(6) 0.0016(5) 0.0045(7) C1 0.093(6) 0.059(4) 0.038(3) -0.002(3) -0.008(3) 0.052(4) N1 0.25(2) 0.33(3) 0.60(6) 0.19(4) 0.096(19) 0.163(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 O2 1.5299(17) . ? P1 O2 1.5299(17) 6 ? P1 O3 1.5338(16) . ? P1 O3 1.5338(16) 6 ? Al1 O2 1.8363(18) . ? Al1 O1 1.8490(16) . ? Al1 O3 1.8627(15) 3_454 ? Al1 O1 1.8742(16) 2_565 ? Al1 F1 1.9017(15) . ? Al1 F2 1.9356(14) . ? F1 Al1 1.9017(15) 5 ? F2 Al1 1.9356(14) 5 ? O1 Al1 1.8742(16) 3_454 ? O3 Al1 1.8627(15) 2_565 ? C1 N1 1.424(10) . ? C1 C1 1.681(15) 4_466 ? N1 C1 1.424(10) 5 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 P1 O2 107.56(15) . 6 ? O2 P1 O3 111.63(8) . . ? O2 P1 O3 110.59(9) 6 . ? O2 P1 O3 110.59(9) . 6 ? O2 P1 O3 111.63(8) 6 6 ? O3 P1 O3 104.90(13) . 6 ? O2 Al1 O1 95.69(8) . . ? O2 Al1 O3 91.33(7) . 3_454 ? O1 Al1 O3 90.29(7) . 3_454 ? O2 Al1 O1 94.21(8) . 2_565 ? O1 Al1 O1 92.99(7) . 2_565 ? O3 Al1 O1 173.26(8) 3_454 2_565 ? O2 Al1 F1 92.15(8) . . ? O1 Al1 F1 172.13(9) . . ? O3 Al1 F1 88.83(6) 3_454 . ? O1 Al1 F1 87.11(5) 2_565 . ? O2 Al1 F2 166.87(8) . . ? O1 Al1 F2 97.00(8) . . ? O3 Al1 F2 85.24(6) 3_454 . ? O1 Al1 F2 88.51(5) 2_565 . ? F1 Al1 F2 75.13(7) . . ? Al1 F1 Al1 106.18(11) . 5 ? Al1 F2 Al1 103.55(10) . 5 ? Al1 O1 Al1 138.67(9) . 3_454 ? P1 O2 Al1 133.86(11) . . ? P1 O3 Al1 140.14(10) . 2_565 ? N1 C1 C1 105.5(10) . 4_466 ? C1 N1 C1 137.3(19) 5 . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.716 _refine_diff_density_min -0.275 _refine_diff_density_rms 0.091 _database_code_depnum_ccdc_archive 'CCDC 948291' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common AlPO-JU89-5 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H22 Al6 F6 N3 O18 P3' _chemical_formula_weight 769.04 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 Trigonal _symmetry_space_group_name_H-M P3(1)21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' 'y, x, -z' 'x-y, -y, -z+2/3' '-x, -x+y, -z+1/3' _cell_length_a 9.362(3) _cell_length_b 9.362(3) _cell_length_c 7.004(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 531.6(4) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.402 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 388 _exptl_absorpt_coefficient_mu 0.680 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.922 _exptl_absorpt_correction_T_max 0.934 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 5.0cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 3958 _diffrn_reflns_av_R_equivalents 0.0445 _diffrn_reflns_av_sigmaI/netI 0.0376 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 28.30 _reflns_number_total 895 _reflns_number_gt 822 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0581P)^2^+0.0266P] 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 ? _chemical_absolute_configuration ad _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881. 71 Friedel pairs' _refine_ls_abs_structure_Flack 0.02(24) _refine_ls_number_reflns 895 _refine_ls_number_parameters 66 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0327 _refine_ls_wR_factor_ref 0.0922 _refine_ls_wR_factor_gt 0.0883 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _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 Al1 Al 0.16200(10) 0.52099(12) 0.05633(11) 0.0095(2) Uani 1 1 d . . . P1 P 0.44934(12) 0.44934(12) 0.0000 0.0092(2) Uani 1 2 d S . . F1 F 0.0000 0.3178(3) 0.1667 0.0143(5) Uani 1 2 d S . . F3 F 0.0000 0.5686(3) 0.1667 0.0165(6) Uani 1 2 d S . . O1 O 0.3015(3) 0.7300(2) -0.0398(3) 0.0122(4) Uani 1 1 d . . . H1 H 0.3457 0.8122 0.0621 0.015 Uiso 1 1 d R . . O2 O 0.2785(3) 0.4272(3) -0.0408(3) 0.0152(5) Uani 1 1 d . . . O3 O 0.0325(3) 0.4672(3) -0.1639(3) 0.0132(5) Uani 1 1 d . . . C C -0.1277(12) 0.7753(14) 0.0453(12) 0.058(2) Uani 0.67 1 d P . . N N 0.0000 0.899(2) 0.1667 0.39(2) Uani 1 2 d S . . 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 0.0085(4) 0.0126(4) 0.0067(4) 0.0007(3) -0.0001(3) 0.0049(4) P1 0.0118(4) 0.0118(4) 0.0064(4) 0.00019(19) -0.00019(19) 0.0078(4) F1 0.0136(13) 0.0161(10) 0.0124(12) 0.0013(5) 0.0026(10) 0.0068(6) F3 0.0160(14) 0.0177(10) 0.0151(11) 0.0009(5) 0.0019(11) 0.0080(7) O1 0.0140(11) 0.0107(10) 0.0077(8) -0.0002(7) 0.0010(8) 0.0030(9) O2 0.0112(10) 0.0231(12) 0.0134(10) -0.0047(9) -0.0020(9) 0.0102(9) O3 0.0128(10) 0.0161(11) 0.0092(9) 0.0014(8) -0.0021(7) 0.0061(10) C 0.061(6) 0.091(7) 0.042(4) -0.013(4) -0.006(4) 0.054(6) N 0.31(3) 0.24(2) 0.64(7) 0.10(2) 0.21(4) 0.155(16) _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 Al1 O2 1.839(2) . ? Al1 O1 1.853(2) . ? Al1 O3 1.869(2) . ? Al1 O1 1.878(2) 2_665 ? Al1 F1 1.905(2) . ? Al1 F3 1.9419(19) . ? P1 O3 1.532(2) 2_665 ? P1 O3 1.532(2) 5_664 ? P1 O2 1.533(2) . ? P1 O2 1.533(2) 4 ? F1 Al1 1.905(2) 6 ? F3 Al1 1.9419(19) 6 ? O1 Al1 1.878(2) 3_564 ? O3 P1 1.532(2) 3_564 ? C N 1.451(12) . ? C C 1.70(2) 4_465 ? N C 1.451(12) 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 O2 Al1 O1 95.55(11) . . ? O2 Al1 O3 91.47(10) . . ? O1 Al1 O3 90.24(10) . . ? O2 Al1 O1 94.26(10) . 2_665 ? O1 Al1 O1 92.83(9) . 2_665 ? O3 Al1 O1 173.21(10) . 2_665 ? O2 Al1 F1 92.26(11) . . ? O1 Al1 F1 172.16(11) . . ? O3 Al1 F1 88.88(8) . . ? O1 Al1 F1 87.26(8) 2_665 . ? O2 Al1 F3 167.03(11) . . ? O1 Al1 F3 96.97(10) . . ? O3 Al1 F3 85.09(8) . . ? O1 Al1 F3 88.52(8) 2_665 . ? F1 Al1 F3 75.20(10) . . ? O3 P1 O3 104.94(18) 2_665 5_664 ? O3 P1 O2 111.62(11) 2_665 . ? O3 P1 O2 110.46(12) 5_664 . ? O3 P1 O2 110.46(12) 2_665 4 ? O3 P1 O2 111.62(11) 5_664 4 ? O2 P1 O2 107.8(2) . 4 ? Al1 F1 Al1 106.22(14) 6 . ? Al1 F3 Al1 103.39(13) 6 . ? Al1 O1 Al1 138.70(12) . 3_564 ? P1 O2 Al1 133.94(15) . . ? P1 O3 Al1 140.26(14) 3_564 . ? N C C 103.9(11) . 4_465 ? C N C 135(2) 6 . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.749 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.099 _database_code_depnum_ccdc_archive 'CCDC 948292' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common AlPO-JU89-6 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H22 Al6 F6 N3 O18 P3' _chemical_formula_weight 769.04 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 Trigonal _symmetry_space_group_name_H-M P3(1)21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' 'y, x, -z' 'x-y, -y, -z+2/3' '-x, -x+y, -z+1/3' _cell_length_a 9.3425(2) _cell_length_b 9.3425(2) _cell_length_c 6.9940(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 528.67(3) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 388 _exptl_absorpt_coefficient_mu 0.684 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.929 _exptl_absorpt_correction_T_max 0.940 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 5.0cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 3946 _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_sigmaI/netI 0.0186 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 28.37 _reflns_number_total 894 _reflns_number_gt 864 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0524P)^2^+0.2037P] 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 ? _chemical_absolute_configuration ad _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881. 70 Friedel pairs' _refine_ls_abs_structure_Flack 0.08(18) _refine_ls_number_reflns 894 _refine_ls_number_parameters 66 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0282 _refine_ls_R_factor_gt 0.0271 _refine_ls_wR_factor_ref 0.0761 _refine_ls_wR_factor_gt 0.0755 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _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 Al1 Al 0.16218(7) 0.52118(8) 0.05622(9) 0.00892(17) Uani 1 1 d . . . P1 P 0.44940(8) 0.44940(8) 0.0000 0.00809(18) Uani 1 2 d S . . F1 F 0.0000 0.3179(2) 0.1667 0.0134(4) Uani 1 2 d S . . F2 F 0.0000 0.5683(2) 0.1667 0.0155(4) Uani 1 2 d S . . O1 O 0.3014(2) 0.73033(18) -0.0397(2) 0.0122(3) Uani 1 1 d . . . H1 H 0.3577 0.8206 0.0512 0.015 Uiso 1 1 d R . . O2 O 0.2784(2) 0.4270(2) -0.0405(2) 0.0143(3) Uani 1 1 d . . . O3 O 0.03266(19) 0.46686(19) -0.1637(2) 0.0124(3) Uani 1 1 d . . . N1 N 0.0000 0.897(2) 0.1667 0.39(2) Uani 1 2 d S . . C2 C -0.1267(9) 0.7760(12) 0.0453(9) 0.0577(18) Uani 0.67 1 d P . . 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 0.0079(3) 0.0110(3) 0.0074(3) 0.0006(2) -0.0003(2) 0.0044(2) P1 0.0100(3) 0.0100(3) 0.0068(3) -0.00008(13) 0.00008(13) 0.0070(3) F1 0.0111(9) 0.0140(7) 0.0142(9) 0.0007(3) 0.0014(7) 0.0055(4) F2 0.0150(9) 0.0155(7) 0.0160(9) 0.0010(4) 0.0019(7) 0.0075(5) O1 0.0138(8) 0.0088(7) 0.0090(6) -0.0006(5) 0.0001(6) 0.0019(6) O2 0.0111(7) 0.0188(8) 0.0149(7) -0.0047(6) -0.0012(6) 0.0089(6) O3 0.0112(7) 0.0133(8) 0.0106(7) 0.0015(6) -0.0022(5) 0.0045(6) N1 0.33(3) 0.25(2) 0.61(6) 0.09(2) 0.18(4) 0.167(15) C2 0.057(4) 0.095(6) 0.041(3) -0.011(3) -0.004(3) 0.052(4) _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 Al1 O2 1.8347(17) . ? Al1 O1 1.8490(16) . ? Al1 O3 1.8640(15) . ? Al1 O1 1.8746(16) 2_665 ? Al1 F1 1.9033(14) . ? Al1 F2 1.9375(13) . ? P1 O2 1.5303(16) 4 ? P1 O2 1.5303(16) . ? P1 O3 1.5332(16) 2_665 ? P1 O3 1.5332(16) 5_664 ? F1 Al1 1.9033(14) 6 ? F2 Al1 1.9375(13) 6 ? O1 Al1 1.8746(16) 3_564 ? O3 P1 1.5332(16) 3_564 ? N1 C2 1.435(10) 6 ? N1 C2 1.435(10) . ? C2 C2 1.696(15) 4_465 ? 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 O2 Al1 O1 95.77(8) . . ? O2 Al1 O3 91.40(7) . . ? O1 Al1 O3 90.35(7) . . ? O2 Al1 O1 94.24(8) . 2_665 ? O1 Al1 O1 92.99(7) . 2_665 ? O3 Al1 O1 173.12(8) . 2_665 ? O2 Al1 F1 92.16(8) . . ? O1 Al1 F1 172.05(8) . . ? O3 Al1 F1 88.78(5) . . ? O1 Al1 F1 87.08(5) 2_665 . ? O2 Al1 F2 166.81(8) . . ? O1 Al1 F2 96.98(8) . . ? O3 Al1 F2 85.18(5) . . ? O1 Al1 F2 88.44(5) 2_665 . ? F1 Al1 F2 75.07(7) . . ? O2 P1 O2 107.63(15) 4 . ? O2 P1 O3 110.63(8) 4 2_665 ? O2 P1 O3 111.57(8) . 2_665 ? O2 P1 O3 111.57(8) 4 5_664 ? O2 P1 O3 110.63(8) . 5_664 ? O3 P1 O3 104.85(12) 2_665 5_664 ? Al1 F1 Al1 106.26(11) 6 . ? Al1 F2 Al1 103.61(10) 6 . ? Al1 O1 Al1 138.54(9) . 3_564 ? P1 O2 Al1 133.94(11) . . ? P1 O3 Al1 140.11(10) 3_564 . ? C2 N1 C2 136.2(18) 6 . ? N1 C2 C2 104.6(10) . 4_465 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.37 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.760 _refine_diff_density_min -0.326 _refine_diff_density_rms 0.093 _database_code_depnum_ccdc_archive 'CCDC 948293' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_7 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common AlPO-JU89-7 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H22 Al6 F6 N3 O18 P3' _chemical_formula_weight 769.04 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' _smmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P3(1)21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' 'y, x, -z' 'x-y, -y, -z+2/3' '-x, -x+y, -z+1/3' _cell_length_a 9.3376(4) _cell_length_b 9.3376(4) _cell_length_c 6.9910(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 527.89(6) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.419 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 388 _exptl_absorpt_coefficient_mu 0.685 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.921 _exptl_absorpt_correction_T_max 0.934 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 5.0cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 3878 _diffrn_reflns_av_R_equivalents 0.0332 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 28.17 _reflns_number_total 883 _reflns_number_gt 828 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0569P)^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 ? _chemical_absolute_configuration unk _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881. 65 Friedel pairs' _refine_ls_abs_structure_Flack 0.32(20) _refine_ls_number_reflns 883 _refine_ls_number_parameters 66 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0330 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0834 _refine_ls_wR_factor_gt 0.0815 _refine_ls_goodness_of_fit_ref 1.081 _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 0.55071(10) 0.55071(10) 0.0000 0.0089(2) Uani 1 2 d S . . Al1 Al 0.47881(10) 0.83784(9) -0.05618(10) 0.0096(2) Uani 1 1 d . . . F1 F 0.6821(3) 1.0000 -0.1667 0.0140(5) Uani 1 2 d S . . F2 F 0.4319(2) 1.0000 -0.1667 0.0167(5) Uani 1 2 d S . . O1 O 0.2703(2) 0.6987(2) 0.0404(2) 0.0126(4) Uani 1 1 d . . . H1 H 0.1936 0.6411 -0.0417 0.015 Uiso 1 1 d R . . O2 O 0.5726(3) 0.7215(2) 0.0407(2) 0.0147(4) Uani 1 1 d . . . O3 O 0.4344(2) 0.4672(2) -0.1693(3) 0.0136(4) Uani 1 1 d . . . C1 C 0.0962(11) 0.8719(11) -0.2865(12) 0.063(2) Uani 0.67 1 d P . . N1 N 0.103(2) 1.0000 -0.1667 0.40(2) Uani 1 2 d S . . 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 0.0102(3) 0.0102(3) 0.0084(4) 0.00005(16) -0.00005(16) 0.0067(4) Al1 0.0115(4) 0.0088(4) 0.0083(3) -0.0006(3) 0.0004(3) 0.0049(3) F1 0.0153(8) 0.0120(11) 0.0136(11) 0.0008(8) 0.0004(4) 0.0060(5) F2 0.0168(8) 0.0166(12) 0.0166(10) 0.0009(9) 0.0005(5) 0.0083(6) O1 0.0082(8) 0.0145(9) 0.0094(7) -0.0004(7) -0.0011(6) 0.0014(7) O2 0.0205(10) 0.0117(9) 0.0143(9) -0.0017(8) -0.0050(7) 0.0098(8) O3 0.0166(10) 0.0146(10) 0.0124(9) -0.0018(7) -0.0036(8) 0.0100(8) C1 0.047(4) 0.060(5) 0.051(4) -0.002(4) 0.010(3) 0.003(4) N1 0.24(2) 0.32(3) 0.68(7) 0.19(4) 0.09(2) 0.159(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 O2 1.5296(19) . ? P1 O2 1.5296(19) 4 ? P1 O3 1.5305(18) . ? P1 O3 1.5305(18) 4 ? Al1 O2 1.8325(19) . ? Al1 O1 1.8453(18) . ? Al1 O3 1.8636(18) 2_665 ? Al1 O1 1.8723(18) 3_564 ? Al1 F1 1.9023(17) . ? Al1 F2 1.9353(15) . ? F1 Al1 1.9023(17) 5_674 ? F2 Al1 1.9353(16) 5_674 ? O1 Al1 1.8723(18) 2_665 ? O3 Al1 1.8636(18) 3_564 ? C1 N1 1.435(11) . ? C1 C1 1.688(18) 6_554 ? N1 C1 1.435(11) 5_674 ? 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 O2 P1 O2 107.95(18) . 4 ? O2 P1 O3 111.47(10) . . ? O2 P1 O3 110.56(10) 4 . ? O2 P1 O3 110.56(10) . 4 ? O2 P1 O3 111.47(10) 4 4 ? O3 P1 O3 104.87(15) . 4 ? O2 Al1 O1 95.53(9) . . ? O2 Al1 O3 91.39(9) . 2_665 ? O1 Al1 O3 90.14(9) . 2_665 ? O2 Al1 O1 94.17(9) . 3_564 ? O1 Al1 O1 92.96(8) . 3_564 ? O3 Al1 O1 173.35(9) 2_665 3_564 ? O2 Al1 F1 92.26(9) . . ? O1 Al1 F1 172.18(10) . . ? O3 Al1 F1 88.89(6) 2_665 . ? O1 Al1 F1 87.24(6) 3_564 . ? O2 Al1 F2 166.86(9) . . ? O1 Al1 F2 97.17(9) . . ? O3 Al1 F2 85.20(6) 2_665 . ? O1 Al1 F2 88.56(6) 3_564 . ? F1 Al1 F2 75.01(8) . . ? Al1 F1 Al1 106.27(12) 5_674 . ? Al1 F2 Al1 103.70(11) 5_674 . ? Al1 O1 Al1 138.89(10) . 2_665 ? P1 O2 Al1 134.02(13) . . ? P1 O3 Al1 140.25(12) . 3_564 ? N1 C1 C1 105.2(10) . 6_554 ? C1 N1 C1 136.4(18) . 5_674 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.17 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.655 _refine_diff_density_min -0.341 _refine_diff_density_rms 0.094 _database_code_depnum_ccdc_archive 'CCDC 948294' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_8 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common AlPO-JU89-8 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H22 Al6 F6 N3 O18 P3' _chemical_formula_weight 769.04 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 Trigonal _symmetry_space_group_name_H-M P3(1)21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' 'y, x, -z' 'x-y, -y, -z+2/3' '-x, -x+y, -z+1/3' _cell_length_a 9.3429(4) _cell_length_b 9.3429(4) _cell_length_c 6.9927(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 528.61(6) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 388 _exptl_absorpt_coefficient_mu 0.684 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.914 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 5.0cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 3920 _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_av_sigmaI/netI 0.0308 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 28.42 _reflns_number_total 896 _reflns_number_gt 846 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0619P)^2^+0.0938P] 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 ? _chemical_absolute_configuration ad _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881. 71 Friedel pairs' _refine_ls_abs_structure_Flack 0.21(22) _refine_ls_number_reflns 896 _refine_ls_number_parameters 66 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0342 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0902 _refine_ls_wR_factor_gt 0.0881 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 Al1 Al 0.47892(11) 0.64105(11) 0.88953(11) 0.0094(2) Uani 1 1 d . . . P1 P 0.55067(10) 1.0000 0.8333 0.0087(2) Uani 1 2 d S . . F1 F 0.6822(3) 0.6822(3) 1.0000 0.0143(5) Uani 1 2 d S . . F2 F 0.4318(3) 0.4318(3) 1.0000 0.0171(5) Uani 1 2 d S . . O1 O 0.4287(2) 0.6985(3) 1.1263(3) 0.0127(4) Uani 1 1 d . . . H1 H 0.4506 0.6460 1.2295 0.015 Uiso 1 1 d R . . O2 O 0.5729(3) 0.8515(2) 0.7925(3) 0.0151(4) Uani 1 1 d . . . O3 O 0.5329(2) 0.5658(2) 0.6695(3) 0.0128(4) Uani 1 1 d . . . N1 N 0.102(2) 0.102(2) 1.0000 0.38(2) Uani 1 2 d S . . C1 C 0.0980(12) 0.2246(14) 1.1215(11) 0.060(2) Uani 0.67 1 d P . . 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 0.0117(4) 0.0108(4) 0.0076(3) -0.0007(3) -0.0009(3) 0.0070(3) P1 0.0110(3) 0.0080(5) 0.0062(4) 0.0006(3) 0.00031(17) 0.0040(2) F1 0.0153(9) 0.0153(9) 0.0138(11) 0.0008(4) -0.0008(4) 0.0089(10) F2 0.0184(9) 0.0184(9) 0.0144(11) 0.0001(5) -0.0001(5) 0.0091(11) O1 0.0193(10) 0.0160(10) 0.0083(8) -0.0002(7) -0.0002(7) 0.0130(8) O2 0.0210(11) 0.0141(10) 0.0142(9) 0.0033(7) 0.0052(8) 0.0118(8) O3 0.0135(9) 0.0176(10) 0.0096(8) -0.0047(8) -0.0021(7) 0.0094(8) N1 0.24(2) 0.24(2) 0.58(6) 0.08(2) -0.08(2) 0.06(2) C1 0.050(5) 0.089(7) 0.046(4) -0.005(4) -0.005(3) 0.039(4) _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 Al1 O2 1.836(2) . ? Al1 O1 1.851(2) 3_564 ? Al1 O3 1.8628(19) . ? Al1 O1 1.8706(19) . ? Al1 F1 1.9028(18) . ? Al1 F2 1.9369(17) . ? P1 O2 1.529(2) . ? P1 O2 1.529(2) 5_676 ? P1 O3 1.5328(19) 6_666 ? P1 O3 1.5328(19) 2_665 ? F1 Al1 1.9028(18) 4_557 ? F2 Al1 1.9369(17) 4_557 ? O1 Al1 1.8514(19) 2_665 ? O3 P1 1.5328(19) 3_564 ? N1 C1 1.442(12) . ? N1 C1 1.442(12) 4_557 ? C1 C1 1.707(19) 6_557 ? 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 O2 Al1 O1 95.60(10) . 3_564 ? O2 Al1 O3 91.39(9) . . ? O1 Al1 O3 90.18(9) 3_564 . ? O2 Al1 O1 94.25(9) . . ? O1 Al1 O1 92.98(8) 3_564 . ? O3 Al1 O1 173.23(10) . . ? O2 Al1 F1 92.25(10) . . ? O1 Al1 F1 172.11(10) 3_564 . ? O3 Al1 F1 88.87(7) . . ? O1 Al1 F1 87.18(7) . . ? O2 Al1 F2 166.89(10) . . ? O1 Al1 F2 97.06(10) 3_564 . ? O3 Al1 F2 85.19(7) . . ? O1 Al1 F2 88.48(7) . . ? F1 Al1 F2 75.05(9) . . ? O2 P1 O2 107.75(19) . 5_676 ? O2 P1 O3 110.57(11) . 6_666 ? O2 P1 O3 111.57(10) 5_676 6_666 ? O2 P1 O3 111.57(10) . 2_665 ? O2 P1 O3 110.57(11) 5_676 2_665 ? O3 P1 O3 104.87(16) 6_666 2_665 ? Al1 F1 Al1 106.27(13) . 4_557 ? Al1 F2 Al1 103.62(12) 4_557 . ? Al1 O1 Al1 138.73(11) 2_665 . ? P1 O2 Al1 133.91(13) . . ? P1 O3 Al1 140.23(12) 3_564 . ? C1 N1 C1 135(2) . 4_557 ? N1 C1 C1 103.8(11) . 6_557 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.42 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.867 _refine_diff_density_min -0.334 _refine_diff_density_rms 0.101 #===END _database_code_depnum_ccdc_archive 'CCDC 948295'