#------------------------------------------------------------------------------ #$Date: 2017-06-02 20:01:22 +0100 (Fri, 02 Jun 2017) $ #$Revision: 197160 $ #$URL: svn://www.crystallography.net/cod/cif/3/50/00/3500067.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_3500067 loop_ _publ_author_name 'Maris, Thierry' _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _journal_name_full 'Personal communication to COD' _journal_year 2017 _chemical_formula_moiety 'Al H12 O6, 3(Cl)' _chemical_formula_sum 'Al Cl3 H12 O6' _chemical_formula_weight 241.42 _space_group_crystal_system trigonal _space_group_IT_number 167 _space_group_name_Hall '-R 3 2"c' _space_group_name_H-M_alt 'R -3 c' _symmetry_space_group_name_Hall '-R 3 2"c' _symmetry_space_group_name_H-M 'R -3 c :H' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary dual _audit_creation_date 2017-05-24 _audit_creation_method ; Olex2 1.2 (compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 6.00012 _cell_length_a 11.8359(4) _cell_length_b 11.8359(4) _cell_length_c 11.8492(4) _cell_measurement_reflns_used 7276 _cell_measurement_temperature 150 _cell_measurement_theta_max 60.193 _cell_measurement_theta_min 4.965 _cell_volume 1437.55(8) _computing_cell_refinement 'SAINT (2013) V8.38A; Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, WI 53719-1173.' _computing_data_collection ; APEX 2 (2013) Bruker AXS Inc., Madison, WI 53719-1173. ; _computing_data_reduction 'SAINT (2013) V8.38A; Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, WI 53719-1173.' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'XT (Sheldrick, 2015)' _diffrn_ambient_temperature 150 _diffrn_detector 'CMOS Area detector' _diffrn_detector_area_resol_mean 10.24 _diffrn_detector_type 'Bruker Photon 100 CMOS Detector' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device 'k-geometry diffractometer' _diffrn_measurement_device_type 'Bruker Venture Metaljet' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_collimation 'Focusing mirrors' _diffrn_radiation_monochromator 'Helios MX Mirror Optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type GaK\a _diffrn_radiation_wavelength 1.34139 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_unetI/netI 0.0119 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 7930 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 53.594 _diffrn_reflns_theta_max 60.162 _diffrn_reflns_theta_min 6.507 _diffrn_source 'Metal Jet' _diffrn_source_target Ga _diffrn_source_type 'Gallium Liquid Metal Jet Source' _exptl_absorpt_coefficient_mu 6.303 _exptl_absorpt_correction_T_max 0.3107 _exptl_absorpt_correction_T_min 0.2307 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1156 before and 0.0546 after correction. The Ratio of minimum to maximum transmission is 0.7425. The \l/2 correction factor is Not present.' _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.673 _exptl_crystal_description Block _exptl_crystal_F_000 744 _exptl_crystal_size_max 0.101 _exptl_crystal_size_mid 0.085 _exptl_crystal_size_min 0.06 _exptl_special_details ; X-ray crystallographic data for I were collected from a single crystal sample, which was mounted on a loop fiber. Data were collected using a Bruker Venture diffractometer equipped with a Photon 100 CMOS Detector, a Helios MX optics and a Kappa goniometer. The crystal-to-detector distance was 4.0 cm, and the data collection was carried out in 1024 x 1024 pixel mode. ; _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. ; _refine_diff_density_max 0.362 _refine_diff_density_min -0.345 _refine_diff_density_rms 0.108 _refine_ls_extinction_coef 0.0090(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2016/6 (Sheldrick 2016)' _refine_ls_goodness_of_fit_ref 1.263 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 26 _refine_ls_number_reflns 372 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.263 _refine_ls_R_factor_all 0.0242 _refine_ls_R_factor_gt 0.0240 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0342P)^2^+0.5460P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0562 _refine_ls_wR_factor_ref 0.0563 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 364 _reflns_number_total 372 _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. ; _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file AlClW6B.cif _cod_data_source_block alclw6b _cod_depositor_comments ; The following automatic conversions were performed: '_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according to the built-in table from CIF Core dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas ; _cod_original_cell_volume 1437.55(11) _cod_database_code 3500067 _shelx_shelxl_version_number 2016/6 _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. ; _shelx_estimated_absorpt_t_max 0.704 _shelx_estimated_absorpt_t_min 0.569 _olex2_refinement_description ; ; _shelx_res_file ; TITL alclw6b_a.res in R-3c alclw6b.res created by SHELXL-2016/6 at 16:21:05 on 24-May-2017 REM Old TITL AlClW6B in R-3c REM SHELXT solution in R-3c REM R1 0.090, Rweak 0.001, Alpha 0.009, Orientation as input REM Formula found by SHELXT: O6 Al Cl3 CELL 1.34139 11.8359 11.8359 11.8492 90 90 120 ZERR 6.00012 0.0004 0.0004 0.0004 0 0 0 LATT 3 SYMM -Y,+X-Y,+Z SYMM +Y-X,-X,+Z SYMM +Y,+X,0.5-Z SYMM -Y+X,-Y,0.5-Z SYMM -X,-X+Y,0.5-Z SFAC Al Cl H O DISP Al 0.177 0.187 1447.9 DISP Cl 0.328 0.543 4162 DISP H -0 0 0.648 DISP O 0.039 0.024 193.4 UNIT 6 18 72 36 EQIV $1 0.333-Y+X,-0.333+X,0.667-Z L.S. 50 PLAN 5 SIZE 0.06 0.085 0.101 TEMP -123.15 HTAB O1 Cl1 HTAB O1 Cl1_$1 HTAB BOND $H list 4 fmap 2 53 ACTA REM REM REM WGHT 0.034200 0.546000 EXTI 0.009033 FVAR 0.50267 O1 4 0.371271 0.560470 0.258049 11.00000 0.01858 0.01408 = 0.03129 0.00023 -0.00527 0.00762 AL1 1 0.333333 0.666667 0.166667 10.16667 0.01206 0.01206 = 0.02409 0.00000 0.00000 0.00603 CL1 2 0.601907 0.666667 0.416667 10.50000 0.01610 0.01841 = 0.03044 -0.00274 -0.00137 0.00920 H1A 3 0.426115 0.587385 0.300753 11.00000 0.04336 H1B 3 0.336281 0.486861 0.253145 11.00000 0.03971 HKLF 4 REM alclw6b_a.res in R-3c REM R1 = 0.0240 for 364 Fo > 4sig(Fo) and 0.0242 for all 372 data REM 26 parameters refined using 0 restraints END WGHT 0.0342 0.5460 REM Instructions for potential hydrogen bonds HTAB O1 Cl1 HTAB O1 Cl1_$1 REM Highest difference peak 0.362, deepest hole -0.345, 1-sigma level 0.108 Q1 1 0.3333 0.4052 0.4167 10.50000 0.05 0.36 Q2 1 0.3333 0.6667 0.4167 10.16667 0.05 0.27 Q3 1 0.3293 0.4134 0.1517 11.00000 0.05 0.26 Q4 1 0.4038 0.6045 0.3362 11.00000 0.05 0.25 Q5 1 0.2412 0.3986 0.1576 11.00000 0.05 0.25 ; _shelx_res_checksum 72222 _shelx_hkl_file ; 1 -2 0 1229.98 44.60 1 1 0 1198.58 44.50 1 1 0 1092.69 44.50 -2 1 0 1151.58 44.50 -2 1 0 1189.98 44.40 1 -2 0 1223.78 44.60 -1 -1 0 1150.78 44.50 -1 -1 0 1111.99 44.50 -1 -1 0 1044.20 44.40 2 -1 0 969.90 44.40 2 -1 0 1178.88 44.60 2 -1 0 1145.69 44.50 2 -1 0 1017.70 44.40 3 0 0 2670.03 114.79 3 0 0 2829.82 114.89 0 -3 0 3023.30 114.89 3 -3 0 3004.80 114.79 -3 0 0 2899.11 114.69 -3 0 0 3019.00 114.79 3 -3 0 2960.40 114.89 3 -3 0 2975.00 114.89 -4 2 0 2650.53 103.09 2 2 0 2699.43 103.29 2 2 0 2692.43 103.09 -4 2 0 2689.63 103.19 2 -4 0 2932.91 103.49 2 -4 0 2691.23 103.29 4 -2 0 2243.88 102.99 4 -2 0 2326.07 102.99 4 -2 0 2279.57 103.09 -2 -2 0 2883.81 103.19 4 -2 0 2692.63 103.29 -2 -2 0 2713.03 103.29 -5 1 0 2.80 0.70 1 4 0 3.90 0.80 -5 1 0 3.90 0.70 -5 1 0 2.40 1.70 -5 1 0 1.50 1.20 4 -5 0 2.80 0.50 4 -5 0 3.60 0.50 4 -5 0 2.50 0.70 4 -5 0 4.60 1.10 4 -5 0 1.90 0.80 1 4 0 2.80 0.40 5 -1 0 1.90 0.70 -1 -4 0 2.60 0.70 -1 -4 0 2.20 0.80 1 -5 0 4.60 1.10 4 1 0 2.30 0.60 4 1 0 2.70 1.00 1 -5 0 4.30 1.10 4 1 0 2.50 0.70 1 -5 0 3.60 0.90 4 1 0 3.80 0.80 -1 5 0 4.20 1.00 -4 -1 0 4.30 0.80 5 -4 0 3.70 0.70 5 -4 0 2.30 0.60 5 -4 0 2.60 0.80 -1 5 0 1.20 1.20 5 -4 0 3.20 0.80 -4 -1 0 2.60 1.10 -6 3 0 20.90 2.50 3 3 0 19.80 1.70 3 -6 0 22.40 2.00 3 -6 0 24.20 2.00 3 3 0 19.80 2.00 -6 3 0 20.90 1.50 3 3 0 24.50 1.70 6 -3 0 24.60 1.60 6 -3 0 22.90 1.80 -3 6 0 23.70 2.30 -3 6 0 21.00 2.20 6 -3 0 24.80 1.30 -3 -3 0 25.80 1.50 -3 -3 0 21.30 2.00 6 -3 0 22.40 1.80 6 0 0 169.98 7.10 -6 6 0 146.69 7.50 6 0 0 166.78 7.90 6 0 0 150.98 7.40 0 -6 0 159.28 7.40 0 -6 0 165.18 7.20 -6 6 0 146.69 7.00 -6 6 0 149.69 7.30 -6 0 0 164.98 7.50 6 -6 0 173.28 7.20 -6 0 0 158.78 7.30 -6 0 0 168.38 6.70 0 6 0 170.18 7.30 0 6 0 157.98 7.40 6 -6 0 154.68 7.30 0 6 0 160.88 7.00 0 6 0 163.48 7.50 6 -6 0 162.18 7.10 6 -6 0 157.28 6.70 0 6 0 165.68 7.20 2 5 0 102.79 4.50 2 5 0 108.89 4.90 -7 2 0 108.79 5.50 2 5 0 100.19 5.30 2 5 0 95.49 4.90 -7 2 0 96.69 5.10 2 5 0 105.99 4.80 2 5 0 98.49 5.10 5 -7 0 102.19 5.00 -5 7 0 92.69 4.70 7 -2 0 94.89 5.00 7 -2 0 98.49 4.70 -5 7 0 92.89 5.00 7 -2 0 106.79 5.00 -2 -5 0 100.39 5.00 -5 7 0 102.09 4.80 -5 7 0 99.49 5.20 -7 5 0 96.59 5.10 5 2 0 94.39 4.90 -7 5 0 93.69 5.30 5 2 0 93.29 5.20 5 2 0 94.99 5.50 2 -7 0 99.29 5.20 -2 7 0 105.99 4.80 7 -5 0 111.29 5.20 7 -5 0 112.09 4.90 7 -5 0 107.49 4.60 -2 7 0 103.59 5.30 -5 -2 0 101.89 5.20 -2 7 0 102.99 4.80 -2 7 0 100.19 5.30 -2 7 0 92.69 4.80 -5 -2 0 107.39 5.00 1 7 0 3393.26 129.59 7 -8 0 3351.56 129.39 -8 1 0 3069.39 130.19 1 7 0 3375.86 129.49 7 -8 0 3313.57 129.29 7 -8 0 3220.68 129.49 1 7 0 3326.47 129.29 -8 1 0 3301.27 129.89 1 7 0 3325.17 129.09 -7 8 0 3224.18 129.49 -1 -7 0 3275.37 129.39 8 -1 0 3346.37 129.29 -7 8 0 3297.97 128.99 8 -1 0 3256.37 129.59 -1 -7 0 3135.29 129.59 8 -1 0 3166.38 129.49 4 4 0 6906.31 283.07 4 4 0 6662.03 283.27 -8 4 0 6331.07 282.87 4 -8 0 7506.95 283.27 4 4 0 7453.05 282.57 4 4 0 7586.44 282.97 -8 4 0 7092.29 283.17 -4 8 0 7309.27 282.67 -4 -4 0 7138.89 282.87 -4 -4 0 7298.97 283.17 8 -4 0 7454.35 283.27 -4 8 0 7383.36 283.27 8 -4 0 6976.80 282.87 -4 8 0 7461.15 282.77 8 -4 0 7135.39 282.87 -4 8 0 7514.15 283.17 1 -8 0 3216.58 129.89 1 -8 0 3472.05 129.59 7 1 0 3286.47 129.49 7 1 0 3208.98 129.29 -8 7 0 3048.50 129.69 7 1 0 3223.48 129.79 7 1 0 3243.18 129.89 8 -7 0 3418.76 129.59 -7 -1 0 3350.96 130.09 -1 8 0 3285.47 129.49 -1 8 0 3427.16 129.89 -7 -1 0 3180.18 129.69 -1 8 0 3286.37 129.39 -1 8 0 3297.87 129.49 8 -7 0 3192.08 129.79 -1 8 0 3349.76 129.89 6 -9 0 14.80 2.70 -9 3 0 13.70 2.90 6 -9 0 13.00 2.80 3 6 0 9.80 1.90 3 6 0 12.10 2.30 -9 3 0 11.20 2.00 3 6 0 10.30 1.70 3 6 0 10.50 2.10 -3 -6 0 8.70 2.10 -3 -6 0 15.90 2.40 -3 -6 0 13.10 1.90 9 -3 0 12.40 2.30 -6 9 0 13.90 2.50 9 -3 0 12.80 2.70 -6 9 0 9.40 2.00 -6 9 0 16.00 2.10 6 3 0 13.10 2.30 -9 6 0 7.50 1.70 6 3 0 11.50 2.10 6 3 0 9.00 2.30 3 -9 0 8.90 1.90 9 -6 0 10.70 2.30 -3 9 0 10.60 1.80 -3 9 0 14.70 2.60 -3 9 0 12.90 2.00 -6 -3 0 17.00 2.70 -3 9 0 13.50 2.00 -3 9 0 10.90 2.00 -9 9 0 14.70 3.00 0 -9 0 16.10 2.60 -9 0 0 14.80 2.20 0 9 0 10.00 1.90 -9 0 0 10.50 2.20 0 9 0 10.30 1.90 0 9 0 14.90 2.00 0 9 0 8.80 2.40 0 9 0 12.60 2.30 2 8 0 6.30 1.60 -10 2 0 11.00 2.60 -10 2 0 3.80 1.90 2 8 0 6.00 1.50 2 8 0 8.50 1.50 -8 10 0 8.00 1.90 -8 10 0 10.40 1.80 -2 -8 0 8.80 1.80 10 -2 0 11.30 2.70 5 5 0 56.29 4.10 -10 5 0 56.49 4.30 5 5 0 54.39 3.60 -10 5 0 41.40 4.10 5 5 0 56.49 3.60 5 5 0 50.09 3.10 -5 -5 0 52.09 4.00 -5 -5 0 51.39 3.50 -5 10 0 46.30 3.30 -5 10 0 56.39 4.30 -5 10 0 50.79 3.40 -5 10 0 52.19 3.90 8 2 0 11.70 2.60 2 -10 0 9.30 1.80 8 2 0 5.10 1.60 -2 10 0 7.40 1.60 -2 10 0 5.70 1.30 -2 10 0 7.50 1.80 -2 10 0 8.90 2.40 -2 10 0 5.70 1.20 -8 -2 0 8.10 2.20 -8 -2 0 8.40 1.70 1 10 0 193.18 9.00 1 10 0 190.78 8.90 1 10 0 191.48 8.80 -11 1 0 185.08 10.00 11 -1 0 192.28 9.50 11 -1 0 193.28 8.80 -1 -10 0 196.08 9.30 -1 -10 0 215.08 9.20 -10 11 0 182.88 9.60 4 7 0 2947.31 116.99 -11 4 0 2753.42 117.69 4 7 0 2873.61 117.29 4 7 0 2993.40 116.59 -11 4 0 3055.59 117.99 -4 -7 0 3042.80 116.99 -4 -7 0 3048.99 117.49 -7 11 0 2970.00 117.59 11 -4 0 2886.11 116.99 -7 11 0 2961.00 116.79 7 4 0 2850.21 118.59 4 -11 0 3110.19 118.89 7 4 0 3024.60 119.39 7 4 0 2888.71 118.39 -7 -4 0 3027.30 119.49 -4 11 0 2941.91 118.59 -7 -4 0 2944.91 118.89 -4 11 0 3101.19 119.49 -4 11 0 3036.90 118.79 -4 11 0 3079.99 118.49 10 1 0 192.48 9.50 10 1 0 198.38 8.60 1 -11 0 188.88 9.10 -1 11 0 194.38 8.80 -10 -1 0 190.38 9.80 -1 11 0 186.88 9.70 -1 11 0 189.58 8.70 -1 11 0 195.58 8.80 -10 -1 0 163.28 9.30 3 9 0 14.00 2.00 3 9 0 12.40 2.40 3 9 0 12.90 2.50 -12 3 0 8.00 2.30 3 9 0 14.60 2.70 -3 -9 0 13.50 2.40 -9 12 0 10.70 2.10 12 -3 0 15.70 3.10 -9 12 0 15.90 3.10 6 6 0 359.76 16.00 6 6 0 396.96 16.70 -6 -6 0 350.36 16.60 -6 12 0 342.57 16.00 -6 12 0 349.37 15.30 -6 -6 0 334.07 15.90 9 3 0 10.70 1.60 9 3 0 17.20 3.10 9 3 0 11.50 2.30 -3 12 0 13.90 2.70 -3 12 0 12.50 2.30 -3 12 0 9.00 1.50 -9 -3 0 9.10 2.10 -3 12 0 12.80 2.20 -9 -3 0 8.00 1.90 0 -12 0 380.16 16.70 0 -12 0 413.56 16.60 12 0 0 397.26 16.30 12 0 0 399.56 16.90 -12 0 0 366.66 17.30 0 12 0 371.76 16.30 0 12 0 388.66 16.30 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12 71.39 4.20 -2 4 12 57.39 6.70 -2 4 12 68.39 4.00 -2 4 12 68.19 5.10 -4 5 -12 125.29 7.50 5 -1 -12 123.69 7.20 -4 5 -12 116.99 7.10 -1 -4 -12 122.59 7.00 5 -1 -12 130.39 6.50 -1 -4 -12 143.39 6.90 -5 1 12 137.69 6.80 1 4 12 130.69 7.60 -5 1 12 124.29 7.50 4 -5 12 129.99 6.40 1 4 12 136.19 6.40 4 -5 12 130.79 6.40 1 4 12 126.19 10.00 -4 -4 -12 1086.79 46.40 -4 8 -12 1198.88 46.60 -4 8 -12 1172.68 46.80 -4 8 -12 1173.58 46.90 -4 -4 -12 1126.29 46.70 8 -4 -12 1192.08 46.20 4 -8 12 1189.88 46.30 -8 4 12 1082.09 46.80 4 4 12 1157.08 46.10 -5 -2 -12 2.20 1.70 -5 -2 -12 -1.90 1.70 -5 -2 -12 -0.10 2.80 -2 7 -12 2.10 2.40 -2 7 -12 1.60 1.60 -2 7 -12 1.40 1.60 5 2 12 1.30 1.10 2 -7 12 1.90 1.20 -7 5 12 1.60 2.00 -7 5 12 0.40 1.40 4 -5 -12 3.80 1.80 -5 1 -12 4.70 2.20 1 4 -12 5.30 1.30 -5 1 -12 3.70 1.90 -5 1 -12 5.80 3.10 1 4 -12 3.20 1.90 -1 -4 12 3.70 1.40 -4 5 12 6.30 2.20 -4 5 12 2.90 2.10 -4 5 12 1.70 2.80 5 -1 12 4.10 1.40 -4 5 12 4.30 1.60 5 -1 12 5.20 1.30 1 -5 -12 122.89 7.10 -5 4 -12 129.89 7.40 4 1 -12 134.69 6.60 -5 4 -12 122.99 7.00 4 1 -12 129.29 7.40 -1 5 12 142.99 6.40 -1 5 12 121.99 7.60 -1 5 12 125.89 6.80 5 -4 12 131.39 6.50 -1 5 12 121.09 9.40 5 -4 12 123.19 6.30 -1 5 12 134.29 7.40 -4 -1 12 135.59 6.70 -5 7 -12 19.60 3.70 -2 -5 -12 11.00 2.10 -5 7 -12 15.10 2.60 -5 7 -12 13.50 2.30 5 -7 12 13.50 2.30 -7 2 12 7.70 2.40 2 5 12 13.00 2.10 -6 -3 -12 1.10 1.50 -6 -3 -12 2.50 2.60 -3 9 -12 1.90 1.70 -3 9 -12 1.50 1.40 6 3 12 1.60 1.00 3 -9 12 -1.70 1.50 -9 6 12 -0.10 1.30 0 6 -12 2.10 1.70 -6 0 -12 0.10 1.70 6 -6 -12 -1.30 1.90 0 6 -12 2.90 1.80 -6 0 -12 -0.30 2.40 0 6 -12 0.60 1.40 6 0 12 -0.50 1.00 6 0 12 0.40 1.30 -6 6 12 -1.20 1.30 -6 6 12 2.90 2.10 0 -6 12 0.60 1.20 -6 3 -12 19.60 3.80 -6 3 -12 31.30 3.70 3 3 -12 23.70 3.70 -6 3 -12 24.40 4.80 3 3 -12 27.20 2.80 -3 -3 12 23.60 2.90 -3 6 12 27.60 5.90 -3 6 12 22.50 3.10 6 -3 12 23.10 2.60 6 -3 12 28.60 2.60 0 -6 -12 75.29 5.10 -6 6 -12 80.39 5.30 6 0 -12 103.19 9.60 -6 6 -12 77.19 5.60 6 0 -12 86.09 4.80 0 6 12 64.39 6.20 0 6 12 81.49 4.50 -6 0 12 80.89 4.90 0 6 12 81.39 10.40 6 -6 12 77.09 4.50 0 6 12 79.09 4.90 0 6 12 90.29 7.60 -3 -6 -12 2.70 1.40 -6 9 -12 2.50 1.80 9 -3 -12 4.70 1.70 -6 9 -12 5.50 1.60 -3 -6 -12 4.70 1.50 -6 9 -12 7.90 2.10 6 -9 12 5.70 1.50 -7 -1 -12 536.65 23.80 -1 8 -12 568.64 23.90 -7 -1 -12 633.34 24.60 -1 8 -12 552.44 23.40 -8 7 12 555.74 24.20 1 -8 12 545.55 23.30 7 1 12 586.94 23.40 5 -7 -12 2.40 1.50 2 5 -12 3.40 1.90 2 5 -12 0.30 1.40 -7 2 -12 3.80 2.30 -7 2 -12 4.40 2.00 -2 -5 12 2.40 1.30 7 -2 12 3.10 1.20 -5 7 12 2.30 1.40 7 -2 12 1.20 1.10 -5 7 12 2.20 1.90 -7 5 -12 6.60 2.00 2 -7 -12 6.70 2.10 5 2 -12 10.90 1.80 7 -5 12 10.20 1.80 -2 7 12 7.50 1.50 -2 7 12 15.40 2.80 -5 -2 12 7.70 1.50 -2 7 12 8.80 1.70 7 -5 12 11.20 2.00 -1 -7 -12 449.95 19.60 -7 8 -12 442.16 18.40 -7 8 -12 402.76 18.80 1 7 12 422.66 18.30 1 7 12 399.86 17.90 -8 1 -12 506.85 24.00 -8 1 -12 545.55 23.20 1 7 -12 563.14 22.60 8 -1 12 544.85 22.40 8 -1 12 571.94 23.00 -1 -7 12 562.34 22.70 -7 8 12 583.14 23.70 -7 8 12 527.65 23.20 4 4 -12 1230.48 46.80 -8 4 -12 1124.19 47.20 -8 4 -12 1114.89 47.30 4 4 -12 1140.59 47.10 8 -4 12 1171.68 46.30 8 -4 12 1180.38 46.50 -4 -4 12 1152.98 46.70 -4 8 12 1152.98 47.00 -4 8 12 1177.38 46.80 7 1 -12 419.46 17.20 -8 7 -12 371.96 17.70 -8 7 -12 413.46 18.10 1 -8 -12 396.26 17.10 -1 8 12 391.16 17.30 -1 8 12 408.16 16.90 8 -7 12 396.56 17.00 3 6 -12 -0.40 1.30 3 6 -12 3.90 2.00 -9 3 -12 0.50 2.10 6 -9 -12 1.50 1.70 -6 9 12 2.50 1.30 -3 -6 12 -1.80 1.50 -6 9 12 0.20 1.90 9 -3 12 -0.60 1.00 9 -3 12 -0.70 1.10 -9 6 -12 4.70 1.80 6 3 -12 6.10 1.50 -9 6 -12 7.60 1.80 3 -9 -12 4.30 3.70 -3 9 12 5.90 1.40 9 -6 12 9.00 1.90 -3 9 12 9.20 2.40 -1 0 -13 1.50 2.20 -1 0 -13 1.00 1.60 0 1 -13 1.10 1.60 1 -1 -13 1.60 2.50 1 -1 -13 -1.30 1.50 0 -1 13 0.10 1.20 0 -1 13 1.60 1.20 1 0 13 0.90 1.20 1 0 13 1.50 1.10 -1 1 13 0.60 1.20 -1 1 13 1.00 1.30 3 -2 -13 160.38 8.10 -2 -1 -13 158.38 7.90 -1 3 -13 160.28 8.20 -2 -1 -13 142.29 8.10 -1 3 -13 150.38 7.30 -1 3 -13 151.08 8.40 -3 2 13 158.78 7.60 1 -3 13 150.78 7.30 2 1 13 149.49 7.30 -3 2 13 155.48 8.30 2 1 13 158.18 7.30 1 -3 13 148.29 7.40 2 0 -13 0.10 1.80 -2 2 -13 1.40 1.40 -2 2 -13 3.00 1.70 -2 2 -13 -2.50 2.00 0 -2 -13 0.80 1.40 0 -2 -13 2.60 2.00 2 -2 13 1.90 1.20 -2 0 13 0.00 1.20 0 2 13 2.10 1.40 0 2 13 0.30 1.00 0 2 13 3.20 4.10 5 -3 -13 878.31 35.50 -2 5 -13 882.81 35.80 -3 -2 -13 890.51 35.40 -2 5 -13 816.62 35.50 -3 -2 -13 841.62 35.60 2 -5 13 882.81 35.10 -5 3 13 816.52 35.50 -5 3 13 872.91 35.10 3 2 13 902.71 35.00 1 2 -13 159.88 7.40 1 2 -13 163.08 8.30 2 -3 -13 154.48 7.90 -3 1 -13 162.08 8.00 -3 1 -13 146.09 8.20 3 -1 13 155.48 7.40 -2 3 13 158.38 7.40 3 -1 13 153.48 7.30 -2 3 13 138.19 8.10 -2 3 13 149.59 7.50 -2 3 13 150.08 8.50 -1 -2 13 156.98 7.50 -3 4 -13 67.89 5.50 -1 -3 -13 74.99 5.10 4 -1 -13 78.49 5.40 -3 4 -13 78.29 5.10 4 -1 -13 83.49 4.50 -1 -3 -13 86.09 5.10 3 -4 13 75.19 4.50 3 -4 13 75.19 4.40 1 3 13 64.89 14.50 1 3 13 72.89 6.80 -4 1 13 73.79 5.80 -4 1 13 82.19 4.80 1 3 13 75.49 4.30 -3 7 -13 5.80 1.80 -4 -3 -13 4.90 1.60 -3 7 -13 4.40 1.90 -3 7 -13 3.00 2.50 -4 -3 -13 6.50 1.70 7 -4 -13 7.30 1.60 4 3 13 5.60 1.20 3 -7 13 6.40 1.80 -4 0 -13 0.80 1.60 4 -4 -13 0.10 1.60 0 4 -13 1.70 1.50 -4 0 -13 0.70 1.80 0 4 -13 0.30 1.70 4 0 13 -1.60 1.20 0 -4 13 -0.40 1.10 -4 4 13 1.40 2.40 -4 4 13 -1.10 1.70 4 0 13 1.50 1.00 3 1 -13 74.89 5.30 -4 3 -13 72.39 5.40 3 1 -13 74.69 4.50 1 -4 -13 69.99 5.40 1 -4 -13 92.89 5.10 -4 3 -13 86.39 5.20 -1 4 13 81.99 4.40 -1 4 13 82.39 6.00 4 -3 13 79.49 4.40 -1 4 13 70.29 6.10 -3 -1 13 80.49 4.70 4 -3 13 75.59 4.50 -1 4 13 61.29 9.00 6 -2 -13 5.00 1.30 -2 -4 -13 8.40 1.70 -4 6 -13 8.50 1.90 -4 6 -13 8.00 2.30 -2 -4 -13 6.20 1.80 -6 2 13 2.60 1.40 -6 2 13 1.10 2.30 4 -6 13 4.50 1.30 -5 -1 -13 267.77 14.40 -1 6 -13 296.17 13.60 -5 -1 -13 296.37 13.40 6 -5 -13 297.07 14.70 -1 6 -13 310.87 13.00 -6 5 13 292.47 13.40 5 1 13 323.07 12.80 1 -6 13 301.07 12.90 -5 2 -13 873.61 35.70 -5 2 -13 840.02 35.30 2 3 -13 884.21 35.60 3 -5 -13 891.81 35.30 2 3 -13 896.61 35.00 -3 5 13 724.83 37.50 5 -2 13 872.61 34.80 5 -2 13 857.21 34.90 -3 5 13 861.81 35.50 -2 -3 13 901.81 35.10 -3 5 13 871.01 35.20 0 -5 -13 1.30 1.90 5 0 -13 0.60 1.30 -5 5 -13 -1.90 1.70 5 0 -13 2.00 2.20 -5 5 -13 -1.00 1.70 0 -5 -13 1.10 1.40 5 -5 13 1.60 1.20 0 5 13 -0.30 1.10 -5 0 13 1.70 1.30 -5 8 -13 24.70 3.70 -5 8 -13 29.80 2.80 -3 -5 -13 25.70 2.90 -3 -5 -13 24.70 3.20 8 -3 -13 26.90 2.60 3 5 13 27.00 2.40 5 -8 13 29.60 2.60 -8 3 13 37.40 4.60 1 5 -13 338.77 14.00 1 5 -13 310.67 14.00 -6 1 -13 296.37 13.90 1 5 -13 324.47 13.70 5 -6 -13 289.27 13.60 -5 6 13 306.27 13.90 6 -1 13 309.77 13.10 6 -1 13 313.57 14.20 -1 -5 13 309.57 13.40 -5 6 13 299.77 13.60 4 2 -13 6.50 1.50 2 -6 -13 8.70 1.70 4 2 -13 5.40 2.30 -2 6 13 5.40 2.80 6 -4 13 8.30 1.60 -2 6 13 5.20 2.00 6 -4 13 4.50 1.10 -4 -2 13 4.90 1.50 -6 7 -13 117.29 6.80 -1 -6 -13 126.79 6.70 -1 -6 -13 134.59 6.40 -6 7 -13 127.99 6.80 -6 7 -13 134.59 7.30 7 -1 -13 129.69 6.30 6 -7 13 129.09 6.50 1 6 13 128.29 6.00 -7 0 -13 2.90 1.60 0 7 -13 0.80 1.70 0 -7 13 0.50 1.40 -7 7 13 -1.60 1.40 -7 7 13 -1.70 1.80 7 0 13 1.30 1.00 3 4 -13 3.60 3.50 4 -7 -13 9.40 2.10 -7 3 -13 7.10 1.80 3 4 -13 8.30 1.90 -4 7 13 5.00 2.40 7 -3 13 8.20 1.80 -4 7 13 10.20 2.80 -3 -4 13 6.60 1.50 1 -7 -13 144.89 6.90 -7 6 -13 128.39 6.40 -7 6 -13 133.49 8.00 6 1 -13 124.19 6.70 1 -7 -13 124.69 6.90 -1 7 13 131.29 6.90 -1 7 13 134.99 11.00 3 -8 -13 30.20 2.90 5 3 -13 25.60 2.80 5 3 -13 34.70 3.40 -8 5 -13 27.40 3.00 -3 8 13 23.60 3.40 -5 -3 13 32.10 2.80 8 -5 13 26.50 2.50 -3 8 13 30.10 4.30 0 -1 -14 8.10 2.50 -1 1 -14 3.10 1.40 -1 1 -14 2.80 1.50 0 -1 -14 2.50 1.70 1 0 -14 3.40 1.20 1 0 -14 2.70 1.50 0 1 14 1.30 1.30 1 -1 14 1.40 1.10 1 -1 14 1.30 1.20 0 1 14 2.30 1.30 0 2 -14 166.08 7.80 0 2 -14 169.08 8.50 2 -2 -14 165.08 8.40 -2 0 -14 177.18 8.50 -2 0 -14 158.48 8.60 -2 2 14 164.88 7.90 2 0 14 161.68 7.80 0 -2 14 170.58 7.90 2 0 14 174.48 7.70 -2 3 -14 238.98 11.80 3 -1 -14 249.97 11.60 -1 -2 -14 244.78 11.70 3 -1 -14 267.17 11.10 -2 3 -14 250.87 11.70 -1 -2 -14 254.87 11.60 2 -3 14 249.97 10.90 2 -3 14 248.18 11.10 -3 1 14 246.48 11.10 1 2 14 260.37 10.90 -3 -1 -14 53.99 4.30 4 -3 -14 47.80 4.20 -1 4 -14 56.99 4.20 -3 -1 -14 49.99 4.00 -4 3 14 41.00 3.90 3 1 14 52.89 3.20 -4 3 14 56.09 5.30 1 -4 14 57.39 3.60 -3 2 -14 238.38 11.60 2 1 -14 235.88 11.50 -3 2 -14 248.48 11.40 1 -3 -14 257.57 11.50 2 1 -14 239.38 10.90 -2 -1 14 251.27 11.00 -1 3 14 258.47 10.80 3 -2 14 247.48 10.90 3 -2 14 250.17 10.70 -2 -3 -14 532.55 21.70 -3 5 -14 425.26 20.10 5 -2 -14 414.76 19.90 5 -2 -14 511.55 20.10 -5 2 14 432.96 19.60 3 -5 14 524.45 20.20 -4 -2 -14 91.09 5.50 -2 6 -14 99.09 5.20 6 -4 -14 108.39 5.00 -4 -2 -14 102.69 5.70 -2 6 -14 103.49 5.70 -6 4 14 95.99 6.00 2 -6 14 92.19 5.00 4 2 14 103.59 4.90 -4 1 -14 46.80 4.30 1 3 -14 47.70 4.20 3 -4 -14 55.99 4.10 -4 1 -14 57.99 4.90 -1 -3 14 50.49 3.40 4 -1 14 53.99 3.30 -4 4 -14 54.59 7.40 0 -4 -14 58.29 4.10 4 0 -14 58.59 5.30 4 0 -14 60.59 3.70 0 -4 -14 49.70 4.80 -4 0 14 57.59 4.30 0 4 14 54.59 3.50 4 -4 14 58.39 3.70 4 -4 14 53.19 3.80 -5 0 -14 1.60 2.00 -5 0 -14 2.80 1.60 0 5 -14 0.80 1.80 5 -5 -14 2.00 2.10 0 5 -14 -0.10 1.50 -5 5 14 6.40 2.00 5 0 14 3.50 1.10 0 -5 14 0.80 1.00 2 -5 -14 446.26 19.80 3 2 -14 420.76 19.30 -5 3 -14 409.26 18.70 5 -3 14 418.96 19.70 5 -3 14 450.85 18.20 -3 -2 14 508.15 19.90 4 -6 -14 92.49 5.40 -6 2 -14 98.59 5.70 2 4 -14 96.29 5.70 2 4 -14 99.49 5.10 -4 6 14 91.69 5.70 6 -2 14 92.19 5.00 -2 -4 14 99.89 5.00 6 -2 14 103.39 4.90 0 0 -15 -1.50 1.30 0 0 15 -1.50 1.20 2 -1 -15 309.87 13.70 -1 -1 -15 279.17 13.90 -1 2 -15 320.57 13.80 2 -1 -15 318.97 13.10 -1 -1 -15 306.77 13.00 -1 -1 -15 324.57 13.80 1 1 15 326.27 13.10 -2 1 15 299.57 13.20 1 -2 15 312.37 13.20 -2 1 -15 270.97 13.80 1 1 -15 314.17 13.10 1 1 -15 312.77 13.70 1 -2 -15 322.97 13.80 -2 1 -15 321.17 13.70 -1 -1 15 310.67 13.20 2 -1 15 320.47 13.00 2 -1 15 311.97 13.20 0 3 -15 2.10 1.50 -3 0 -15 3.00 1.50 3 -3 -15 -2.10 1.40 3 0 -15 -1.50 1.70 0 -3 -15 2.00 1.70 -3 3 -15 -1.10 1.60 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 99916 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' 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 O1 O 0.37127(7) 0.56047(8) 0.25805(7) 0.0216(3) Uani 1 1 d . . . . . Al1 Al 0.333333 0.666667 0.166667 0.0161(2) Uani 1 6 d S T P . . Cl1 Cl 0.60191(3) 0.666667 0.416667 0.0214(2) Uani 1 2 d S T P . . H1A H 0.426(2) 0.587(2) 0.3008(18) 0.043(5) Uiso 1 1 d . . . . . H1B H 0.336(2) 0.4869(19) 0.2531(14) 0.040(4) Uiso 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 O1 0.0186(4) 0.0141(4) 0.0313(5) 0.0002(3) -0.0053(3) 0.0076(3) Al1 0.0121(3) 0.0121(3) 0.0241(4) 0.000 0.000 0.00603(14) Cl1 0.0161(2) 0.0184(3) 0.0304(3) -0.00274(11) -0.00137(6) 0.00920(13) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Al Al 0.1770 0.1870 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3280 0.5430 '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' O O 0.0390 0.0240 '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 Al1 O1 H1A 123.1(14) . . Al1 O1 H1B 123.4(13) . . H1A O1 H1B 113.4(19) . . O1 Al1 O1 90.01(4) 3_565 . O1 Al1 O1 90.01(4) 25_565 27 O1 Al1 O1 89.99(4) 27 . O1 Al1 O1 180.0 25_565 . O1 Al1 O1 90.01(4) 26_455 27 O1 Al1 O1 89.99(4) 3_565 25_565 O1 Al1 O1 89.99(4) 2_665 27 O1 Al1 O1 89.99(4) 2_665 25_565 O1 Al1 O1 89.99(4) 26_455 . O1 Al1 O1 89.99(4) 3_565 26_455 O1 Al1 O1 90.01(4) 2_665 . O1 Al1 O1 180.0 2_665 26_455 O1 Al1 O1 90.01(4) 3_565 2_665 O1 Al1 O1 90.01(4) 25_565 26_455 O1 Al1 O1 180.0 3_565 27 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 O1 Al1 1.8757(8) . O1 H1A 0.76(2) . O1 H1B 0.757(19) . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1A Cl1 0.76(2) 2.27(2) 3.0221(9) 174.9(19) . O1 H1B Cl1 0.757(19) 2.291(18) 3.0370(9) 168.7(19) 33_545 _cod_database_fobs_code 3500067