data_I _database_code_depnum_ccdc_archive 'CCDC 1817054' #============================================================================== # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic 2017-10-09 _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted 2018-01-15 _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code SP5002 _journal_coeditor_notes ; ? ; _journal_paper_category FA _journal_techeditor_code M180094 _iucr_compatibility_tag ACTA95 _journal_techeditor_notes ; ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Al O4 P' _chemical_formula_weight 121.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'O' 'O' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system trigonal _space_group_IT_number 148 _space_group_name_H-M_alt 'R -3 :R' _space_group_name_Hall '-P 3*' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' 'z, x, y' 'y, z, x' '-x, -y, -z' '-z, -x, -y' '-y, -z, -x' _cell_length_a 9.6090(17) _cell_length_b 9.6090(17) _cell_length_c 9.6090(17) _cell_angle_alpha 94.46(3) _cell_angle_beta 94.46(3) _cell_angle_gamma 94.46(3) _cell_volume 878.7(5) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.383 _exptl_crystal_F_000 1029 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.002 _exptl_crystal_size_mid 0.002 _exptl_crystal_size_min 0.000 _exptl_absorpt_coefficient_mu 0.134 _shelx_estimated_absorpt_T_min 1.000 _shelx_estimated_absorpt_T_max 1.000 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.02508 _diffrn_radiation_type ? _diffrn_source ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 3802 _diffrn_reflns_av_unetI/netI 0.2632 _diffrn_reflns_av_R_equivalents 0.1787 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 0.075 _diffrn_reflns_theta_max 1.103 _diffrn_reflns_theta_full 0.862 _diffrn_measured_fraction_theta_max 0.753 _diffrn_measured_fraction_theta_full 0.950 _diffrn_reflns_Laue_measured_fraction_max 0.753 _diffrn_reflns_Laue_measured_fraction_full 0.950 _diffrn_reflns_point_group_measured_fraction_max 0.753 _diffrn_reflns_point_group_measured_fraction_full 0.950 _reflns_number_total 1673 _reflns_number_gt 949 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment undef _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 1673 _refine_ls_number_parameters 57 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2532 _refine_ls_R_factor_gt 0.2225 _refine_ls_wR_factor_ref 0.5177 _refine_ls_wR_factor_gt 0.4999 _refine_ls_goodness_of_fit_ref 1.304 _refine_ls_restrained_S_all 1.304 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.6211(3) 0.1662(3) 0.3883(3) 0.0173(12) Uani 1 1 d . . . . . Al1 Al 0.6223(4) 0.4000(4) 0.1678(4) 0.0157(12) Uani 1 1 d . . . . . O1 O 0.6054(8) 0.2427(6) 0.2509(6) 0.0304(16) Uani 1 1 d . . . . . O2 O 0.6445(7) 0.0091(6) 0.3474(6) 0.0272(15) Uani 1 1 d . . . . . O3 O 0.7519(7) 0.2335(7) 0.4872(7) 0.0345(17) Uani 1 1 d . . . . . O4 O 0.4814(6) 0.1776(7) 0.4652(7) 0.0306(16) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0218(18) 0.0144(17) 0.0169(17) 0.0042(10) 0.0053(11) 0.0023(11) Al1 0.023(2) 0.0119(18) 0.0130(19) 0.0012(12) 0.0045(13) 0.0046(13) O1 0.053(4) 0.018(3) 0.021(3) 0.0108(19) 0.005(2) 0.001(2) O2 0.036(3) 0.018(3) 0.030(3) 0.0068(19) 0.010(2) 0.004(2) O3 0.036(3) 0.031(3) 0.033(3) -0.004(2) -0.006(2) -0.005(2) O4 0.024(3) 0.045(4) 0.027(3) 0.009(2) 0.015(2) 0.009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 O1 1.563(6) . ? P1 O2 1.568(6) . ? P1 O3 1.579(7) . ? P1 O4 1.589(6) . ? P1 Al1 3.193(5) 6_656 ? P1 Al1 3.206(5) . ? P1 Al1 3.211(5) 3 ? P1 Al1 3.234(5) 5_666 ? Al1 O4 1.759(7) 2 ? Al1 O1 1.766(6) . ? Al1 O2 1.772(7) 5_665 ? Al1 O3 1.778(8) 6_666 ? 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 O2 108.3(4) . . ? O1 P1 O3 110.9(4) . . ? O2 P1 O3 108.3(4) . . ? O1 P1 O4 108.2(4) . . ? O2 P1 O4 110.7(4) . . ? O3 P1 O4 110.5(4) . . ? O1 P1 Al1 120.9(3) . 6_656 ? O2 P1 Al1 18.2(2) . 6_656 ? O3 P1 Al1 111.3(3) . 6_656 ? O4 P1 Al1 93.4(3) . 6_656 ? O1 P1 Al1 16.6(3) . . ? O2 P1 Al1 123.0(3) . . ? O3 P1 Al1 97.0(3) . . ? O4 P1 Al1 106.3(3) . . ? Al1 P1 Al1 137.12(14) 6_656 . ? O1 P1 Al1 124.4(3) . 3 ? O2 P1 Al1 107.0(3) . 3 ? O3 P1 Al1 96.8(3) . 3 ? O4 P1 Al1 17.3(3) . 3 ? Al1 P1 Al1 88.88(12) 6_656 3 ? Al1 P1 Al1 119.87(15) . 3 ? O1 P1 Al1 104.5(3) . 5_666 ? O2 P1 Al1 124.6(3) . 5_666 ? O3 P1 Al1 16.5(3) . 5_666 ? O4 P1 Al1 99.4(3) . 5_666 ? Al1 P1 Al1 125.72(12) 6_656 5_666 ? Al1 P1 Al1 88.71(11) . 5_666 ? Al1 P1 Al1 88.61(12) 3 5_666 ? O4 Al1 O1 108.2(4) 2 . ? O4 Al1 O2 110.6(4) 2 5_665 ? O1 Al1 O2 107.5(3) . 5_665 ? O4 Al1 O3 110.6(4) 2 6_666 ? O1 Al1 O3 111.0(4) . 6_666 ? O2 Al1 O3 108.8(4) 5_665 6_666 ? O4 Al1 P1 95.1(3) 2 5_665 ? O1 Al1 P1 118.1(3) . 5_665 ? O2 Al1 P1 16.0(2) 5_665 5_665 ? O3 Al1 P1 112.5(3) 6_666 5_665 ? O4 Al1 P1 107.2(3) 2 . ? O1 Al1 P1 14.7(2) . . ? O2 Al1 P1 120.3(3) 5_665 . ? O3 Al1 P1 98.5(3) 6_666 . ? P1 Al1 P1 132.21(14) 5_665 . ? O4 Al1 P1 15.6(2) 2 2 ? O1 Al1 P1 123.0(3) . 2 ? O2 Al1 P1 107.1(2) 5_665 2 ? O3 Al1 P1 98.6(3) 6_666 2 ? P1 Al1 P1 91.12(12) 5_665 2 ? P1 Al1 P1 120.02(15) . 2 ? O4 Al1 P1 101.0(3) 2 6_666 ? O1 Al1 P1 105.3(3) . 6_666 ? O2 Al1 P1 123.3(3) 5_665 6_666 ? O3 Al1 P1 14.7(3) 6_666 6_666 ? P1 Al1 P1 125.65(14) 5_665 6_666 ? P1 Al1 P1 91.39(12) . 6_666 ? P1 Al1 P1 91.29(12) 2 6_666 ? P1 O1 Al1 148.7(5) . . ? P1 O2 Al1 145.8(4) . 6_656 ? P1 O3 Al1 148.8(5) . 5_666 ? P1 O4 Al1 147.1(5) . 3 ? _refine_diff_density_max 0.210 _refine_diff_density_min -0.327 _refine_diff_density_rms 0.063 _shelx_res_file ; TITL eiger_60keV_a.res in R-3 eiger_60keV_a.res created by SHELXL-2016/6 at 18:21:04 on 02-Oct-2017 REM Old TITL eiger_60keV in R-3 REM SHELXT solution in R-3 REM R1 0.319, Rweak 0.145, Alpha 0.152, Orientation as input REM Formula found by SHELXT: O4 Al P CELL 0.02508 9.6090 9.6090 9.6090 94.460 94.460 94.460 ZERR 6.000 0.0017 0.0017 0.0017 0.025 0.025 0.025 LATT 1 SYMM Z, X, Y SYMM Y, Z, X SFAC O 0.237 0.799 0.649 3.654 0.800 10.924 0.261 29.964 0.035 = 0.0 0.0 18.200 0.660 16.00 SFAC Al 1.566 4.481 7.000 52.140 110.070 1117.547 29.228 272.510 0.202 = 0.0 0.0 123.000 1.210 27.000 SFAC P 0.637 1.279 1.347 7.260 2.438 22.476 10.959 60.711 0.107 = 0.0 0.0 0.620 1.8000 30.970 UNIT 24 6 6 SIZE 0.000150 0.0017 0.0017 L.S. 100 ACTA LIST 4 FMAP 2 PLAN 20 WGHT 0.200000 SWAT 1.004185 0.3152 FVAR 7.10470 P1 3 0.621058 0.166204 0.388306 11.00000 0.02179 0.01443 = 0.01694 0.00419 0.00531 0.00227 AL1 2 0.622312 0.399976 0.167789 11.00000 0.02315 0.01194 = 0.01305 0.00118 0.00448 0.00456 O1 1 0.605371 0.242703 0.250946 11.00000 0.05346 0.01787 = 0.02119 0.01078 0.00536 0.00086 O2 1 0.644545 0.009123 0.347426 11.00000 0.03572 0.01831 = 0.02967 0.00678 0.00952 0.00428 O3 1 0.751949 0.233502 0.487150 11.00000 0.03563 0.03087 = 0.03319 -0.00444 -0.00555 -0.00482 O4 1 0.481367 0.177597 0.465154 11.00000 0.02352 0.04517 = 0.02701 0.00901 0.01528 0.00937 HKLF 4 REM eiger_60keV_a.res in R-3 REM R1 = 0.2225 for 949 Fo > 4sig(Fo) and 0.2532 for all 1673 data REM 57 parameters refined using 0 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.210, deepest hole -0.327, 1-sigma level 0.063 Q1 1 0.4626 0.2389 0.1672 11.00000 0.05 0.21 Q2 1 0.6611 0.0020 0.2458 11.00000 0.05 0.18 Q3 1 0.4835 0.3998 0.5462 11.00000 0.05 0.18 Q4 1 0.7433 -0.0052 0.3571 11.00000 0.05 0.18 Q5 1 0.1190 0.1190 0.1190 10.33333 0.05 0.18 Q6 1 0.6095 0.2557 0.3323 11.00000 0.05 0.17 Q7 1 0.7437 -0.0457 0.1298 11.00000 0.05 0.17 Q8 1 0.6734 0.1333 0.6049 11.00000 0.05 0.16 Q9 1 0.3582 0.2396 0.2788 11.00000 0.05 0.16 Q10 1 0.9242 -0.0120 0.6502 11.00000 0.05 0.16 Q11 1 0.6710 0.1183 0.6580 11.00000 0.05 0.16 Q12 1 0.6340 0.3425 0.5452 11.00000 0.05 0.15 Q13 1 0.9995 0.0984 0.1151 11.00000 0.05 0.15 Q14 1 0.8923 0.1236 0.5756 11.00000 0.05 0.14 Q15 1 0.3220 0.2116 0.3141 11.00000 0.05 0.14 Q16 1 0.8940 -0.0204 -0.0009 11.00000 0.05 0.14 Q17 1 0.6924 -0.0995 0.1212 11.00000 0.05 0.14 Q18 1 0.6869 -0.0789 0.2521 11.00000 0.05 0.14 Q19 1 0.6099 0.3176 0.2022 11.00000 0.05 0.14 Q20 1 0.5281 0.2737 0.5212 11.00000 0.05 0.13 ; _shelx_res_checksum 47922 _shelx_hkl_file ; 1 0 -1 979.57 302.41 -1 0 1 893.98 276.16 1 0 0 2430.59 745.96 0 0 1 2042.36 629.87 -1 0 0 2536.99 778.12 0 0 -1 2884.55 889.01 1 0 1 2856.18 876.48 -1 0 -1 4433.23 1359.05 2 -1 -2 4539.63 1395.23 -2 1 2 4357.57 1339.90 2 -1 -1 1383.64 429.37 -2 1 1 1406.10 436.23 2 -1 0 3716.82 1142.71 -1 0 2 5868.41 1799.77 -2 1 0 3563.13 1095.89 1 0 -2 6180.51 1895.53 2 -1 1 5754.92 1766.43 -1 1 2 4156.60 1276.06 -2 1 -1 4594.01 1410.83 1 -1 -2 5282.04 1621.02 2 0 -2 6204.16 1903.33 -2 0 2 6114.31 1875.91 2 0 -1 5043.24 1548.44 -2 0 1 4721.68 1449.37 2 0 0 3461.47 1063.50 0 0 2 2180.44 672.67 -2 0 0 3175.37 975.55 0 0 -2 5944.07 1832.16 2 0 1 861.58 267.18 -2 0 -1 884.75 274.51 2 1 -2 1000.85 316.36 -2 -1 2 2000.98 621.60 2 1 -1 986.42 312.10 -2 -1 1 1445.11 451.13 2 1 0 1294.03 405.26 1 0 2 3421.27 1049.79 -2 -1 0 1380.80 431.03 -1 0 -2 3643.52 1118.12 2 1 1 2421.13 748.09 -2 -1 -1 1983.49 614.27 2 -1 2 32.96 21.40 -2 1 -2 26.10 23.01 2 0 2 5270.22 1616.77 -2 0 -2 3310.14 1016.45 2 1 2 3839.77 1181.25 -2 -1 -2 2676.49 824.94 3 -2 -3 826.59 260.79 -3 2 3 824.46 261.03 3 -2 -2 3830.31 1179.59 -3 2 2 2094.38 649.02 3 -2 -1 5315.15 1634.03 -2 -1 3 2456.60 760.39 -3 2 1 5504.30 1692.67 2 1 -3 2598.46 803.42 3 -2 0 694.89 220.83 -2 0 3 532.22 168.77 -3 2 0 1307.27 407.62 2 0 -3 383.03 123.89 3 -2 1 785.21 248.26 -2 1 3 686.62 216.84 -3 2 -1 891.14 280.42 2 -1 -3 696.79 219.82 3 -2 2 1154.06 359.62 -2 2 3 891.61 279.47 -3 2 -2 938.66 293.66 2 -2 -3 729.41 229.25 3 -1 -3 232.51 79.73 -3 1 3 385.40 126.40 3 -1 -2 6580.09 2021.08 -3 1 2 6320.01 1941.40 3 -1 -1 5631.97 1730.50 -3 1 1 4433.23 1363.54 3 -1 0 335.51 111.91 -1 0 3 856.85 265.76 -3 1 0 458.93 149.10 1 0 -3 705.53 219.75 3 -1 1 1378.68 428.90 -1 1 3 1704.25 525.60 -3 1 -1 1928.40 597.24 1 -1 -3 1621.02 500.30 3 -1 2 195.01 68.92 -3 1 -2 195.96 70.15 3 0 -3 448.29 148.37 -3 0 3 661.32 212.23 3 0 -2 1144.84 357.26 -3 0 2 1217.19 379.01 3 0 -1 2149.70 663.92 -3 0 1 2093.19 646.19 3 0 0 491.56 158.72 0 0 3 1034.18 320.14 -3 0 0 854.73 268.12 0 0 -3 630.82 197.05 3 0 1 8020.01 2458.96 -3 0 -1 7424.18 2277.85 3 0 2 5509.03 1691.96 -3 0 -2 5471.20 1680.37 3 1 -3 411.40 138.17 -3 -1 3 258.43 94.81 3 1 -2 3364.53 1039.39 -3 -1 2 3976.90 1226.64 3 1 -1 3648.25 1125.69 -3 -1 1 3823.22 1179.36 3 1 0 7060.06 2170.04 1 0 3 9859.50 3031.15 -3 -1 0 7457.28 2291.57 -1 0 -3 7949.07 2444.78 3 1 1 6870.91 2110.93 -3 -1 -1 6398.04 1966.70 3 2 -3 219.63 82.04 -3 -2 3 181.49 71.76 3 2 -2 848.34 270.01 -3 -2 2 961.83 305.01 3 2 -1 35.44 35.32 2 -1 3 69.28 28.89 -3 -2 1 48.38 38.44 -2 1 -3 121.15 44.21 3 2 0 2473.15 766.30 2 0 3 3253.40 999.43 -3 -2 0 2539.35 786.40 -2 0 -3 3262.86 1002.50 3 2 1 329.12 113.04 2 1 3 1273.70 395.33 -3 -2 -1 290.35 100.96 -2 -1 -3 570.76 180.50 3 2 2 1164.22 364.83 -3 -2 -2 1324.06 413.77 3 -1 3 3532.40 1086.91 -3 1 -3 3376.35 1038.91 3 0 3 1826.02 564.38 -3 0 -3 2033.37 627.98 3 1 3 571.00 182.65 -3 -1 -3 717.36 227.36 3 2 3 4066.75 1251.00 -3 -2 -3 4218.07 1298.52 4 -3 -4 2943.66 912.42 -4 3 4 2022.03 630.35 4 -3 -3 493.21 162.67 -4 3 3 348.04 118.67 4 -3 -2 1260.69 395.80 -3 -2 4 1791.97 558.00 -4 3 2 1507.06 470.75 3 2 -4 2173.35 675.03 4 -3 -1 3589.14 1107.72 -3 -1 4 4702.77 1448.42 -4 3 1 4045.47 1247.69 3 1 -4 1788.42 556.10 4 -3 0 1716.55 534.12 -3 0 4 2328.92 720.19 -4 3 0 1906.41 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