#------------------------------------------------------------------------------ #$Date: 2016-03-25 13:43:39 +0200 (Fri, 25 Mar 2016) $ #$Revision: 179860 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/01/56/7015641.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7015641 loop_ _publ_author_name 'Wragg, David S.' 'Fullerton, Grace M.' 'Byrne, Peter J.' 'Slawin, Alexandra M. Z.' 'Warren, John E.' 'Teat, Simon J.' 'Morris, Russell E.' _publ_section_title ; Solvothermal aluminophosphate zeotype synthesis with ionic liquid precursors. ; _journal_issue 18 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 4926 _journal_page_last 4932 _journal_paper_doi 10.1039/c0dt01788d _journal_volume 40 _journal_year 2011 _chemical_formula_sum 'C4.67 H6.67 Al2 F0.67 N0.67 O8 P2' _chemical_formula_weight 328.67 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 78.231(5) _cell_angle_beta 87.485(6) _cell_angle_gamma 87.179(5) _cell_formula_units_Z 3 _cell_length_a 9.154(4) _cell_length_b 9.239(4) _cell_length_c 9.345(4) _cell_measurement_reflns_used 279 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 17.26 _cell_measurement_theta_min 3.05 _cell_volume 772.3(6) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.990 _diffrn_measured_fraction_theta_max 0.983 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator silicon _diffrn_radiation_source synchrotron _diffrn_radiation_wavelength 0.63070 _diffrn_reflns_av_R_equivalents 0.1415 _diffrn_reflns_av_sigmaI/netI 0.2394 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 8670 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 26.02 _diffrn_reflns_theta_min 1.98 _exptl_absorpt_coefficient_mu 0.638 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_density_diffrn 2.120 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 496 _refine_diff_density_max 1.157 _refine_diff_density_min -0.994 _refine_diff_density_rms 0.232 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.955 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 244 _refine_ls_number_reflns 4269 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.955 _refine_ls_R_factor_all 0.1756 _refine_ls_R_factor_gt 0.0956 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0835P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2129 _refine_ls_wR_factor_ref 0.2747 _reflns_number_gt 2022 _reflns_number_total 4269 _reflns_threshold_expression >2\s(I) _cod_data_source_file c0dt01788d.txt _cod_data_source_block stan249 _cod_original_cell_volume 772.3(5) _cod_database_code 7015641 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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) 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' 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 . . ? 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 . ?