# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # 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_gaba_monohydrate_0p44_GPa _audit_creation_method SHELXL-2013 _chemical_name_systematic ; 4-aminobutanoic acid monohydrate ; _chemical_name_common 'GABA monohydrate' _chemical_formula_moiety 'C4 H9 N O2, H2 O' _chemical_formula_sum 'C4 H11 N O3' _chemical_formula_weight 121.14 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' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 2/c' _space_group_name_Hall '-C 2yc' _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' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.276(6) _cell_length_b 5.6339(3) _cell_length_c 14.3645(10) _cell_angle_alpha 90 _cell_angle_beta 94.598(13) _cell_angle_gamma 90 _cell_volume 1151.6(5) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 936 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 24.96 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.397 _exptl_crystal_F_000 528 _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.09 _exptl_absorpt_coefficient_mu 0.118 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS V.2008/1 SHADE (Parsons, 2004) ; # The following data are from Sadabs: _exptl_absorpt_correction_T_min 0.6126 _exptl_absorpt_correction_T_max 0.7453 _exptl_special_details ; High-pressure crystallisation in a diamond-anvil cell. ; _diffrn_ambient_temperature 296(2) _diffrn_measurement_device 'Bruker AXS SMART APEX' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator silicon _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.7000 _diffrn_measurement_method '\f & \w scans' _diffrn_reflns_number 3751 _diffrn_reflns_av_unetI/netI 0.0347 _diffrn_reflns_reduction_process ; Scaled and merged with SORTAV R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_av_R_equivalents 0.0506 _diffrn_reflns_theta_min 2.802 _diffrn_reflns_theta_max 26.120 _diffrn_reflns_theta_full 24.835 _diffrn_measured_fraction_theta_max 0.387 _diffrn_measured_fraction_theta_full 0.410 _diffrn_reflns_Laue_measured_fraction_max 0.387 _diffrn_reflns_Laue_measured_fraction_full 0.410 _diffrn_reflns_point_group_measured_fraction_max 0.387 _diffrn_reflns_point_group_measured_fraction_full 0.410 _reflns_number_total 463 _reflns_number_gt 405 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; All non-H atoms were refined anisotropically in conjunction with RIGU restraints. The positions of H-atoms belonging to water were freely refined with Uiso constrained to 1.5 the parent O-atom. All other H-atoms were refined subject to contraints. The following alerts originate from PLATON CHECKCIF: PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ... 0.410 RESPONSE: High-pressure data collected in the diamond-anvil cell. PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....2.4 RESPONSE: High-pressure data collected in the diamond-anvil cell. Skewing of ADPs indicative of limited region of reciprocal space sampled. ; _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution SHELXS _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2012)' _computing_publication_material 'PLATON, XCIF, ENCIFER, SHELXLE' _computing_molecular_graphics MERCURY _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^)+(0.0688P)^2^+0.6685P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 463 _refine_ls_number_parameters 80 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0467 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.1101 _refine_ls_wR_factor_gt 0.1064 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.026 _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 O1W O 0.5957(3) 0.8393(3) 0.32393(10) 0.036(3) Uani 1 1 d . . . . . H1W H 0.591(6) 0.695(6) 0.336(2) 0.054 Uiso 1 1 d . U . . . H2W H 0.599(5) 0.925(5) 0.375(2) 0.054 Uiso 1 1 d . U . . . C1 C 0.6086(4) 0.3224(3) 0.45811(14) 0.029(3) Uani 1 1 d . U . . . C2 C 0.6418(4) 0.5296(3) 0.51926(14) 0.031(3) Uani 1 1 d . U . . . H2A H 0.5980 0.6595 0.5071 0.038 Uiso 1 1 calc R U . . . H2B H 0.7022 0.5812 0.5001 0.038 Uiso 1 1 calc R U . . . C3 C 0.6522(4) 0.4866(3) 0.62331(14) 0.033(3) Uani 1 1 d . U . . . H3A H 0.7037 0.3771 0.6379 0.039 Uiso 1 1 calc R U . . . H3B H 0.5953 0.4133 0.6422 0.039 Uiso 1 1 calc R U . . . C4 C 0.6707(5) 0.7149(4) 0.67860(14) 0.035(3) Uani 1 1 d . U . . . H4A H 0.6804 0.6778 0.7446 0.042 Uiso 1 1 calc R U . . . H4B H 0.7275 0.7892 0.6597 0.042 Uiso 1 1 calc R U . . . O2 O 0.6123(3) 0.1168(2) 0.49033(9) 0.034(2) Uani 1 1 d . U . . . O1 O 0.5804(3) 0.3706(2) 0.37518(9) 0.035(2) Uani 1 1 d . U . . . N1 N 0.5905(4) 0.8835(3) 0.66297(11) 0.030(2) Uani 1 1 d . U . . . H1A H 0.5952 0.9614 0.6097 0.045 Uiso 1 1 calc R U . . . H1B H 0.5917 0.9865 0.7100 0.045 Uiso 1 1 calc R U . . . H1C H 0.5367 0.8031 0.6599 0.045 Uiso 1 1 calc R U . . . 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 O1W 0.059(8) 0.0247(8) 0.0235(8) 0.0036(5) -0.0037(17) 0.0029(12) C1 0.044(9) 0.0218(10) 0.0213(10) -0.0026(7) 0.0014(19) -0.0027(16) C2 0.049(9) 0.0203(10) 0.0241(11) -0.0008(7) 0.0016(19) -0.0094(16) C3 0.051(10) 0.0227(10) 0.0241(11) 0.0003(7) 0.000(2) 0.0051(16) C4 0.053(9) 0.0315(11) 0.0205(10) -0.0034(7) -0.003(2) 0.0018(19) O2 0.055(7) 0.0194(8) 0.0277(8) -0.0003(5) -0.0002(15) -0.0031(11) O1 0.053(7) 0.0263(8) 0.0234(8) -0.0005(5) -0.0025(14) -0.0076(12) N1 0.046(8) 0.0221(8) 0.0214(8) -0.0036(6) -0.0001(17) -0.0025(14) _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 C1 O2 1.247(2) . ? C1 O1 1.256(3) . ? C1 C2 1.514(4) . ? C2 C3 1.510(3) . ? C3 C4 1.524(3) . ? C4 N1 1.491(7) . ? 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 C1 O1 123.6(2) . . ? O2 C1 C2 119.9(2) . . ? O1 C1 C2 116.43(17) . . ? C3 C2 C1 116.89(19) . . ? C2 C3 C4 112.32(17) . . ? N1 C4 C3 111.1(4) . . ? _refine_diff_density_max 0.122 _refine_diff_density_min -0.096 _refine_diff_density_rms 0.028 _shelxl_version_number 2013-3 _shelx_res_file ; TITL sad in C2/c CELL 0.7000 14.2756 5.6339 14.3645 90.000 94.598 90.000 ZERR 8.00 0.0064 0.0003 0.0010 0.000 0.013 0.000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H N O UNIT 32 88 8 24 OMIT -6 4 9 OMIT -7 5 11 OMIT -7 3 10 OMIT -5 1 17 OMIT -5 3 2 OMIT -6 0 10 OMIT -6 2 8 OMIT 4 2 13 OMIT 4 2 10 OMIT -6 4 3 OMIT -5 1 6 OMIT 4 2 15 OMIT 3 1 6 OMIT 0 0 6 OMIT -4 0 6 OMIT -6 4 4 OMIT 2 2 3 OMIT -2 2 3 OMIT -4 2 3 OMIT -1 1 3 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! L.S. 4 BOND FMAP 2 PLAN 10 acta RIGU TEMP 23.000 WGHT 0.068800 0.668500 FVAR 5.62870 MOLE 1 O1W 4 0.595726 0.839287 0.323927 11.00000 0.05876 0.02472 = 0.02354 0.00357 -0.00371 0.00295 H1W 2 0.591138 0.695140 0.336487 11.00000 -1.50000 H2W 2 0.598902 0.924641 0.374798 11.00000 -1.50000 C1 1 0.608649 0.322402 0.458110 11.00000 0.04389 0.02179 = 0.02133 -0.00255 0.00135 -0.00268 C2 1 0.641818 0.529558 0.519263 11.00000 0.04926 0.02025 = 0.02413 -0.00082 0.00162 -0.00943 AFIX 23 H2A 2 0.597986 0.659547 0.507089 11.00000 -1.20000 H2B 2 0.702172 0.581217 0.500091 11.00000 -1.20000 AFIX 0 C3 1 0.652200 0.486604 0.623308 11.00000 0.05117 0.02266 = 0.02414 0.00027 0.00044 0.00508 AFIX 23 H3A 2 0.703726 0.377068 0.637854 11.00000 -1.20000 H3B 2 0.595255 0.413276 0.642237 11.00000 -1.20000 AFIX 0 C4 1 0.670732 0.714935 0.678596 11.00000 0.05308 0.03147 = 0.02051 -0.00339 -0.00327 0.00175 AFIX 23 H4A 2 0.680438 0.677767 0.744599 11.00000 -1.20000 H4B 2 0.727512 0.789196 0.659710 11.00000 -1.20000 AFIX 0 O2 4 0.612274 0.116797 0.490332 11.00000 0.05466 0.01945 = 0.02770 -0.00030 -0.00020 -0.00314 O1 4 0.580422 0.370635 0.375176 11.00000 0.05294 0.02628 = 0.02344 -0.00049 -0.00254 -0.00765 N1 3 0.590487 0.883462 0.662973 11.00000 0.04631 0.02214 = 0.02140 -0.00364 -0.00014 -0.00248 AFIX 137 H1A 2 0.595212 0.961386 0.609657 11.00000 -1.50000 H1B 2 0.591690 0.986517 0.710012 11.00000 -1.50000 H1C 2 0.536658 0.803083 0.659923 11.00000 -1.50000 AFIX 0 HKLF 4 REM sad in C2/c REM R1 = 0.0399 for 405 Fo > 4sig(Fo) and 0.0467 for all 463 data REM 80 parameters refined using 36 restraints END WGHT 0.0688 0.6685 REM Highest difference peak 0.122, deepest hole -0.096, 1-sigma level 0.028 Q1 1 0.6589 0.4012 0.4894 11.00000 0.05 0.12 Q2 1 0.6640 0.6068 0.6497 11.00000 0.05 0.11 Q3 1 0.5827 0.9053 0.2743 11.00000 0.05 0.11 Q4 1 0.5689 0.1155 0.5458 11.00000 0.05 0.09 Q5 1 0.6842 0.2168 0.4691 11.00000 0.05 0.09 Q6 1 0.6560 0.5032 0.5776 11.00000 0.05 0.08 Q7 1 0.5558 0.4943 0.3235 11.00000 0.05 0.08 Q8 1 0.5585 0.0021 0.4668 11.00000 0.05 0.08 Q9 1 0.6304 0.6520 0.4938 11.00000 0.05 0.08 Q10 1 0.5595 0.4583 0.4975 11.00000 0.05 0.08 ; _shelx_res_checksum 12219 _shelx_hkl_file ; -7 1 12 19.95 275.90 -7 1 13 7764.10 542.30 -7 1 14 6331.60 969.20 -7 1 15 610.50 556.40 -7 1 16 4143.30 868.30 -7 3 10 -12.30 478.70 -7 3 11 1110.30 623.40 -7 3 12 3529.60 754.80 -7 3 13 282.90 579.80 -7 3 14 2102.10 650.70 -7 3 15 832.40 662.70 -7 5 11 87.40 545.50 -6 0 9 604.90 478.10 -6 0 10 1373.70 669.10 -6 0 11 149.80 469.90 -6 0 12 490.20 592.70 -6 0 13 -126.45 243.50 -6 0 14 33.69 204.80 -6 0 15 108.62 191.50 -6 0 16 289.05 156.30 -6 0 17 -74.53 210.20 -6 2 8 628.60 480.80 -6 2 10 3131.01 375.10 -6 2 11 567.67 251.60 -6 2 1212092.95 736.00 -6 2 1318314.63 914.90 -6 2 14 65.50 195.60 -6 2 1520688.99 1045.10 -6 2 16 172.90 130.70 -6 4 3 245.00 258.90 -6 4 4 2070.90 424.10 -6 4 5 8942.38 1419.90 -6 4 612478.34 889.70 -6 4 7 5039.90 557.00 -6 4 8 715.56 144.50 -6 4 9 764.66 265.50 -6 4 10 5430.60 436.20 -6 4 11 278.17 260.50 -6 4 12 2126.77 293.00 -6 4 13 81.46 257.60 -6 6 3 16.70 348.70 -6 6 4 417.90 391.90 -6 6 5 50.90 416.50 -5 1 634768.70 2861.40 -5 1 7 2471.26 293.10 -5 1 819798.95 657.00 -5 1 934269.66 1118.80 -5 1 10 8740.22 467.00 -5 1 11 6064.95 365.40 -5 1 12 8961.55 529.60 -5 1 13 125.97 140.30 -5 1 14 19.82 88.00 -5 1 15 441.57 129.30 -5 1 16 1024.17 231.00 -5 1 17 231.71 302.00 -5 3 2 425.90 170.40 -5 3 3 189.90 161.80 -5 3 420645.53 902.70 -5 3 5 1150.86 76.20 -5 3 652249.74 2105.40 -5 3 7 3194.40 387.10 -5 3 8 4150.15 351.30 -5 3 9 246.67 119.20 -5 3 1015055.20 1441.50 -5 3 11 4629.12 410.40 -5 3 1243026.73 1569.50 -5 3 13 5796.00 488.10 -5 3 14 295.95 110.20 -5 3 15 162.60 130.70 -5 5 1 3663.01 167.70 -5 5 216370.83 428.60 -5 5 314788.89 626.20 -5 5 4 4393.03 256.00 -5 5 5 9693.92 394.10 -5 5 6 3992.69 290.30 -5 5 7 5.70 125.30 -5 5 8 448.53 146.50 -5 5 9 978.24 238.30 -5 5 10 222.85 123.70 -5 5 11 4111.31 257.70 -4 0 5 -24.80 238.10 -4 0 6 340.68 194.00 -4 0 7 76.02 76.60 -4 0 846837.45 1871.10 -4 0 9 4.78 65.50 -4 0 1021174.52 1059.00 -4 0 11 22.81 82.30 -4 0 1222424.99 1008.60 -4 0 13 -83.06 218.30 -4 0 1428435.54 1038.70 -4 0 15 -102.41 169.50 -4 0 16 368.28 114.50 -4 0 17 -36.78 212.60 -4 2 3 -186.20 88.30 -4 2 421967.90 829.10 -4 2 5 284.72 56.70 -4 2 6 8958.73 292.90 -4 2 7 2554.73 102.70 -4 2 817655.71 702.30 -4 2 9 9082.41 519.50 -4 2 1029579.80 1277.10 -4 2 11 535.86 177.90 -4 2 12 1647.62 167.80 -4 2 13 537.01 159.80 -4 2 14 1975.89 185.40 -4 2 15 1534.77 334.50 -4 2 16 3158.94 265.30 -4 2 17 3531.86 317.70 -4 4 1 5204.06 141.00 -4 4 2 1103.05 63.40 -4 4 313852.90 285.30 -4 4 4 5225.04 130.10 -4 4 5 6518.52 191.40 -4 4 6 7636.43 376.50 -4 4 7 8806.68 313.60 -4 4 8 1822.88 107.50 -4 4 9 2651.17 205.50 -4 4 10 2222.38 153.00 -4 4 11 2016.04 148.10 -4 4 12 4194.55 237.40 -4 4 13 2251.81 168.60 -4 4 14 984.01 169.10 -4 6 1 287.30 72.90 -4 6 2 7249.63 236.20 -4 6 3 6462.28 207.30 -4 6 4 951.15 79.80 -4 6 5 455.27 66.50 -4 6 6 137.06 77.90 -4 6 718905.17 515.70 -4 6 8 373.95 89.70 -3 1 3185251.1 11092.3 -3 1 4 8780.64 295.20 -3 1 550159.00 1892.70 -3 1 624714.74 445.70 -3 1 7 8573.53 152.80 -3 1 8 4372.55 126.10 -3 1 939025.66 1785.90 -3 1 10 -70.32 113.10 -3 1 1126719.38 699.30 -3 1 1229922.69 678.90 -3 1 1317541.57 539.60 -3 1 14 8002.37 257.80 -3 1 15 9051.00 672.00 -3 1 16 983.79 167.20 -3 1 17 221.34 75.70 -3 3 125682.05 437.80 -3 3 2 517.53 29.30 -3 3 312694.88 220.50 -3 3 424568.69 450.80 -3 3 514111.70 256.20 -3 3 624512.09 547.70 -3 3 7 3043.73 86.40 -3 3 8 8106.89 194.10 -3 3 910542.60 282.70 -3 3 10 5932.22 181.60 -3 3 11 1638.86 92.20 -3 3 12 1871.10 145.40 -3 3 13 1489.48 98.40 -3 3 14 6278.02 220.20 -3 3 15 393.26 129.80 -3 3 16 1360.44 235.70 -3 5 1 8296.89 207.20 -3 5 2 1401.51 89.50 -3 5 312355.51 307.80 -3 5 410365.30 271.60 -3 5 5 2822.47 110.10 -3 5 627595.32 530.40 -3 5 7 6339.27 206.60 -3 5 8 919.39 90.60 -3 5 9 8050.78 223.90 -3 5 10 2538.71 187.50 -3 5 11 5289.92 178.00 -3 5 12 -48.12 176.10 -2 0 3 41.00 17.80 -2 0 5 -18.19 55.30 -2 0 6 278.66 36.20 -2 0 7 21.81 26.50 -2 0 8 2.09 34.70 -2 0 9 2.89 37.60 -2 0 1011763.27 302.50 -2 0 11 -73.11 119.00 -2 0 12 1129.35 85.20 -2 0 13 25.00 55.20 -2 0 14 5746.13 178.90 -2 0 15 35.80 57.90 -2 0 16 363.61 73.40 -2 0 17 70.45 78.10 -2 2 140159.12 759.70 -2 2 225000.99 481.70 -2 2 3 194.99 216.20 -2 2 412816.41 186.00 -2 2 565515.97 1153.80 -2 2 6 -13.87 122.20 -2 2 7 3181.47 66.00 -2 2 8 2166.35 74.70 -2 2 940118.59 706.50 -2 2 1021776.05 394.30 -2 2 11 5673.53 117.90 -2 2 12 5320.95 160.80 -2 2 1322364.96 433.90 -2 2 14 343.29 73.60 -2 2 1515686.74 286.70 -2 2 16 123.89 59.70 -2 2 17 2713.09 144.80 -2 4 119077.46 329.00 -2 4 244531.40 1003.40 -2 4 316788.06 262.30 -2 4 414158.07 237.10 -2 4 510567.83 185.90 -2 4 6 9300.85 164.50 -2 4 7 1341.19 55.50 -2 4 8 368.94 51.10 -2 4 9 336.60 55.70 -2 4 1021623.88 407.50 -2 4 11 98.84 54.90 -2 4 1211338.57 337.20 -2 4 13 635.71 100.80 -2 4 14 604.88 172.80 -2 6 1 1922.03 82.30 -2 6 2 3176.30 111.80 -2 6 314248.57 295.50 -2 6 4 2330.87 99.60 -2 6 5 20.56 49.00 -2 6 6 1768.26 82.10 -2 6 7 302.02 66.10 -2 6 8 6510.10 291.80 -2 6 9 3932.42 361.00 -1 1 174259.90 1894.70 -1 1 297193.24 3529.90 -1 1 3 73.23 38.00 -1 1 416775.04 231.00 -1 1 532928.38 438.10 -1 1 624586.91 321.30 -1 1 7 4823.65 73.10 -1 1 858705.21 1080.90 -1 1 10 3559.33 103.00 -1 1 11 7150.66 158.80 -1 1 12 8167.05 173.10 -1 1 13 1174.70 84.20 -1 1 14 494.95 53.40 -1 1 15 4975.91 198.40 -1 1 16 8518.78 189.00 -1 1 17 1749.91 83.60 -1 3 128572.22 383.80 -1 3 2 6250.41 136.70 -1 3 3 2607.64 52.20 -1 3 449947.63 739.60 -1 3 5 841.08 31.40 -1 3 616723.15 234.70 -1 3 7 3793.12 77.80 -1 3 8 401.06 40.60 -1 3 921861.49 427.90 -1 3 1048136.83 800.10 -1 3 11 4514.66 117.20 -1 3 1213274.76 239.10 -1 3 13 87.96 59.10 -1 3 14 1727.06 114.40 -1 3 15 9657.64 246.40 -1 3 16 120.54 97.80 -1 5 1 7793.71 185.90 -1 5 236952.86 544.30 -1 5 331483.62 454.10 -1 5 4 193.56 44.60 -1 5 5 552.10 47.80 -1 5 6 1755.82 67.10 -1 5 7 1105.50 69.80 -1 5 8 850.48 107.80 -1 5 911783.61 311.90 -1 5 10 733.65 89.10 -1 5 11 165.47 61.90 -1 5 12 3995.72 134.80 -1 7 1 6807.70 193.70 0 0 1 0.62 2.30 0 0 260868.58 1611.30 0 0 3 -16.27 38.50 0 0 459355.35 2138.60 0 0 5 6.60 10.00 0 0 6 196.00 106.30 0 0 7 39.04 21.80 0 0 850266.50 1688.20 0 0 9 -2.66 106.50 0 0 10 135.25 51.30 0 0 11 -14.40 107.30 0 0 12 3149.03 128.60 0 0 13 -12.91 122.20 0 0 1417612.67 390.10 0 0 15 39.12 60.20 0 0 1610262.12 249.30 0 0 17 -16.01 163.90 0 2 0 14.61 11.00 0 2 151968.76 820.10 0 2 263729.34 1231.50 0 2 311154.68 179.00 0 2 4 0.24 12.20 0 2 5 62.86 11.00 0 2 6 7204.49 108.20 0 2 7 5.94 15.00 0 2 885643.75 1643.30 0 2 9 254.63 36.20 0 2 10 4759.70 105.60 0 2 11 5917.69 116.00 0 2 12 5332.82 131.40 0 2 13 1645.21 112.10 0 2 14 8849.56 180.90 0 2 1522788.40 426.20 0 2 16 77.24 56.90 0 2 17 219.52 103.50 0 4 075336.26 2137.50 0 4 136015.06 616.40 0 4 2 1018.50 38.70 0 4 3 1013.38 49.80 0 4 4 924.32 41.10 0 4 5 3468.46 75.10 0 4 626308.00 388.60 0 4 713513.92 237.30 0 4 8 1913.58 66.80 0 4 9 618.62 59.60 0 4 10 321.81 57.20 0 4 11 413.11 59.10 0 4 12 4970.80 150.50 0 4 13 463.39 68.60 0 4 14 560.82 110.80 0 6 015064.70 295.30 0 6 1 332.02 39.90 0 6 2 204.28 44.70 0 6 3 489.13 60.10 0 6 4 661.01 74.40 0 6 5 2973.85 174.80 0 6 6 138.86 65.40 0 6 724931.20 552.50 0 6 8 235.94 64.50 0 6 9 99.98 93.00 1 1 0 2736.47 46.40 1 1 119006.51 291.50 1 1 2 3046.67 49.40 1 1 349114.40 962.20 1 1 429124.28 456.50 1 1 558654.61 1508.20 1 1 660085.79 1133.80 1 1 7 57.08 17.00 1 1 812189.03 240.00 1 1 9 506.21 28.00 1 1 10 9926.77 171.70 1 1 1149352.96 905.70 1 1 1281583.73 2339.00 1 1 13 337.65 49.50 1 1 14 1405.99 122.10 1 1 15 4509.04 144.80 1 1 16 12.14 60.70 1 1 17 1522.94 95.90 1 3 022879.79 305.60 1 3 1 1.64 15.70 1 3 218052.75 245.80 1 3 313636.16 187.40 1 3 414606.31 208.80 1 3 5 3293.97 80.70 1 3 694131.93 1423.30 1 3 7 1248.48 47.00 1 3 8 3629.66 168.00 1 3 9 1024.55 75.20 1 3 1010706.78 248.90 1 3 11 38.37 44.00 1 3 1227587.73 498.00 1 3 13 2120.89 119.40 1 3 14 1595.91 112.90 1 3 15 42.70 89.90 1 3 16 302.41 121.40 1 5 021545.75 335.70 1 5 1 4243.70 90.50 1 5 2 510.62 39.60 1 5 3 670.51 58.20 1 5 422541.22 401.90 1 5 5 675.12 95.70 1 5 621298.35 428.10 1 5 7 8684.60 179.70 1 5 8 8.03 62.10 1 5 9 550.18 58.50 1 5 10 73.52 56.80 1 5 11 1978.78 99.60 1 5 12 31.07 65.10 1 7 0 191.18 202.30 1 7 1 744.35 75.50 2 0 4 3930.85 552.00 2 0 5 44.92 25.50 2 0 637780.30 1249.90 2 0 7 -0.21 86.00 2 0 8 2043.55 69.20 2 0 9 121.97 60.00 2 0 10 1613.13 148.60 2 0 11 -100.29 136.80 2 0 12 559.55 87.00 2 0 13 57.70 98.80 2 0 14 5564.35 274.60 2 0 15 2.72 96.10 2 0 16 842.42 108.10 2 0 17 -40.75 179.00 2 2 0 1481.60 47.80 2 2 1 6379.21 111.80 2 2 2122818.2 3465.6 2 2 3 499.62 150.90 2 2 410892.30 329.40 2 2 527517.20 461.30 2 2 6 83.67 20.20 2 2 7 6892.98 150.40 2 2 820543.53 368.20 2 2 959760.11 1393.00 2 2 1020249.02 414.70 2 2 1129557.53 654.80 2 2 12 84.47 80.90 2 2 13 2328.59 213.00 2 2 14 132.01 67.20 2 2 15 804.29 77.80 2 2 16 93.32 69.00 2 2 17 52.06 176.90 2 4 038151.07 798.50 2 4 113169.93 320.90 2 4 238531.62 828.30 2 4 3 8327.13 214.40 2 4 4 1220.82 65.60 2 4 5 8061.24 168.20 2 4 6 5328.42 142.60 2 4 7 248.26 42.90 2 4 8 6320.81 164.30 2 4 9 2360.18 98.70 2 4 1018162.85 525.70 2 4 11 54.15 88.60 2 4 1211622.42 700.00 2 4 13 1306.99 131.20 2 4 14 3641.00 377.60 2 6 0 84.48 40.30 2 6 1 -37.58 127.10 2 6 2 1221.92 95.10 2 6 318772.45 318.00 2 6 4 1536.81 69.40 2 6 5 399.51 51.60 2 6 6 4410.77 221.60 2 6 7 919.37 125.40 2 6 8 357.75 100.50 2 6 9 3196.58 244.70 3 1 6 155.13 127.40 3 1 746809.24 1705.60 3 1 810977.14 388.60 3 1 960691.70 3555.40 3 1 10 461.48 54.80 3 1 1117581.39 596.50 3 1 12 265.35 66.30 3 1 13 -21.50 215.20 3 1 14 675.16 88.40 3 1 15 3296.11 404.20 3 1 16 3399.93 452.70 3 1 17 -69.35 190.00 3 3 018800.00 288.00 3 3 1 105.00 27.10 3 3 253767.31 987.40 3 3 317752.17 468.50 3 3 415798.38 340.80 3 3 5 2197.89 129.00 3 3 6 1154.74 64.40 3 3 7 4796.42 131.60 3 3 830930.26 1136.80 3 3 935880.20 2131.20 3 3 1033768.78 1706.30 3 3 11 665.55 97.90 3 3 12 3085.87 229.90 3 3 13 268.83 144.30 3 3 14 573.53 168.30 3 3 1523740.64 1711.70 3 5 034607.93 608.60 3 5 1 3706.99 168.00 3 5 219922.01 442.50 3 5 322062.66 703.70 3 5 4 7493.96 219.30 3 5 5 1213.76 114.50 3 5 6 199.23 59.00 3 5 7 359.56 68.50 3 5 8 2543.34 133.60 3 5 913095.92 351.90 3 5 10 65.26 63.00 3 5 11 5273.20 212.60 3 5 12 514.16 162.30 4 0 11 607.25 524.70 4 0 15 572.98 660.50 4 2 6 7740.91 425.00 4 2 719979.91 971.00 4 2 10 548.71 267.20 4 2 11 432.27 106.30 4 2 12 258.24 579.50 4 2 13 1020.25 695.00 4 2 15 2492.37 795.20 4 4 024193.40 564.60 4 4 126821.66 717.80 4 4 2 294.46 70.80 4 4 3 1609.20 93.40 4 4 4 449.46 66.80 4 4 5 136.47 63.90 4 4 623345.81 523.10 4 4 7 3095.43 128.30 4 4 8 1349.35 153.40 4 4 9 3699.17 550.60 4 4 10 3343.97 313.20 4 4 11 170.06 195.80 4 4 12 5240.57 436.50 4 4 13 2442.91 328.50 4 6 0 7868.52 208.30 4 6 1 147.11 85.80 4 6 2 3466.87 154.30 4 6 3 7181.69 251.50 4 6 4 67.44 62.00 4 6 512962.21 321.40 4 6 6 134.80 72.40 4 6 7 5405.20 870.40 4 6 8 3480.33 262.80 5 5 0 5261.24 322.40 5 5 1 365.32 114.20 5 5 2 5541.95 264.80 5 5 3 383.88 112.40 5 5 4 8386.96 336.20 5 5 5 6757.56 286.00 5 5 6 4390.83 359.60 5 5 7 545.75 162.20 5 5 8 397.74 192.10 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 63387 _database_code_depnum_ccdc_archive 'CCDC 969073' ####################################################################### # # 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_gaba_monohydrate_150K _audit_creation_method SHELXL-2013 _chemical_name_systematic ; 4-aminobutanoic acid monohydrate ; _chemical_name_common 'GABA monohydrate' _chemical_formula_moiety 'C4 H9 N O2, H2 O' _chemical_formula_sum 'C4 H11 N O3' _chemical_formula_weight 121.14 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' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 2/c' _space_group_name_Hall '-C 2yc' _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' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.3799(9) _cell_length_b 5.6552(4) _cell_length_c 14.4202(9) _cell_angle_alpha 90 _cell_angle_beta 94.499(3) _cell_angle_gamma 90 _cell_volume 1169.05(13) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2943 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 29.82 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.377 _exptl_crystal_F_000 528 _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_absorpt_coefficient_mu 0.116 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS V.2004/1 ; # The following data are from Sadabs: _exptl_absorpt_correction_T_min 0.8864 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; Crystal recovered to ambient pressure from high-pressure crystallisation in the diamond-anvil cell ; _diffrn_ambient_temperature 150(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 'Bruker AXS APEX II' _diffrn_measurement_device_type Area _diffrn_measurement_method '\f & \w scans' _diffrn_reflns_number 8128 _diffrn_reflns_av_unetI/netI 0.0280 _diffrn_reflns_reduction_process ; Scaled and merged with SORTAV R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_theta_min 2.834 _diffrn_reflns_theta_max 30.406 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.951 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.951 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.951 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 1669 _reflns_number_gt 1305 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_special_details ; All non-H atoms were refined anisotropically. Although all H-atoms were visible in difference Fourier maps only those belonging to water were freely refined. All other H-atoms were refined subject to contraints. ; _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'known coordinates' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2012)' _computing_publication_material 'PLATON, XCIF, ENCIFER, SHELXLE' _computing_molecular_graphics MERCURY _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^)+(0.0508P)^2^+0.7087P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'known coordinates' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 1669 _refine_ls_number_parameters 82 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.1038 _refine_ls_wR_factor_gt 0.0964 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 O1W O 0.59669(7) 0.84008(17) 0.32427(6) 0.0226(2) Uani 1 1 d . . . . . H1W H 0.5907(12) 0.695(4) 0.3391(13) 0.038(5) Uiso 1 1 d . . . . . H2W H 0.6031(13) 0.918(4) 0.3739(14) 0.048(6) Uiso 1 1 d . . . . . C1 C 0.60787(8) 0.32220(19) 0.45830(8) 0.0151(2) Uani 1 1 d . . . . . C2 C 0.64004(9) 0.5304(2) 0.51904(7) 0.0185(3) Uani 1 1 d . . . . . H2A H 0.5951 0.6614 0.5067 0.022 Uiso 1 1 calc R U . . . H2B H 0.7010 0.5844 0.4995 0.022 Uiso 1 1 calc R U . . . C3 C 0.65043(8) 0.4862(2) 0.62359(7) 0.0170(2) Uani 1 1 d . . . . . H3A H 0.7026 0.3745 0.6381 0.020 Uiso 1 1 calc R U . . . H3B H 0.5927 0.4116 0.6428 0.020 Uiso 1 1 calc R U . . . C4 C 0.66893(8) 0.7127(2) 0.67905(8) 0.0176(2) Uani 1 1 d . . . . . H4A H 0.6778 0.6739 0.7461 0.021 Uiso 1 1 calc R U . . . H4B H 0.7272 0.7865 0.6607 0.021 Uiso 1 1 calc R U . . . O2 O 0.61216(6) 0.11588(15) 0.49042(5) 0.0220(2) Uani 1 1 d . . . . . O1 O 0.57822(6) 0.37113(15) 0.37536(5) 0.0196(2) Uani 1 1 d . . . . . N1 N 0.59020(7) 0.88469(17) 0.66318(6) 0.0162(2) Uani 1 1 d . . . . . H1A H 0.5967 0.9664 0.6097 0.024 Uiso 1 1 calc R U . . . H1B H 0.5910 0.9873 0.7118 0.024 Uiso 1 1 calc R U . . . H1C H 0.5351 0.8049 0.6583 0.024 Uiso 1 1 calc R U . . . 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 O1W 0.0385(6) 0.0147(4) 0.0142(4) 0.0015(3) -0.0002(4) 0.0001(4) C1 0.0180(5) 0.0137(5) 0.0138(5) -0.0011(4) 0.0030(4) -0.0004(4) C2 0.0296(6) 0.0130(5) 0.0129(5) -0.0009(4) 0.0015(4) -0.0041(4) C3 0.0234(6) 0.0139(5) 0.0134(5) -0.0003(4) 0.0000(4) 0.0021(4) C4 0.0211(6) 0.0185(6) 0.0129(5) -0.0028(4) -0.0013(4) 0.0015(4) O2 0.0384(5) 0.0122(4) 0.0153(4) 0.0004(3) 0.0013(4) -0.0007(3) O1 0.0286(5) 0.0161(4) 0.0133(4) 0.0006(3) -0.0025(3) -0.0025(3) N1 0.0227(5) 0.0137(4) 0.0122(4) -0.0017(3) 0.0008(3) -0.0008(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 C1 O2 1.2551(14) . ? C1 O1 1.2685(13) . ? C1 C2 1.5177(15) . ? C2 C3 1.5239(15) . ? C3 C4 1.5221(16) . ? C4 N1 1.4966(15) . ? 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 C1 O1 123.64(10) . . ? O2 C1 C2 120.28(10) . . ? O1 C1 C2 116.08(10) . . ? C1 C2 C3 116.47(10) . . ? C4 C3 C2 112.43(10) . . ? N1 C4 C3 111.56(9) . . ? _refine_diff_density_max 0.347 _refine_diff_density_min -0.189 _refine_diff_density_rms 0.048 _shelxl_version_number 2013-3 _shelx_res_file ; TITL gabalt_0m in C2/c CELL 0.71073 14.3799 5.6552 14.4202 90.000 94.499 90.000 ZERR 8.00 0.0009 0.0004 0.0009 0.000 0.003 0.000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H N O UNIT 32 88 8 24 LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!! L.S. 4 BOND FMAP 2 PLAN 20 acta TEMP -123.000 WGHT 0.050800 0.708700 FVAR 1.26160 MOLE 1 O1W 4 0.596690 0.840084 0.324268 11.00000 0.03849 0.01471 = 0.01423 0.00152 -0.00019 0.00013 H1W 2 0.590697 0.695349 0.339148 11.00000 0.03823 H2W 2 0.603083 0.917865 0.373865 11.00000 0.04758 C1 1 0.607872 0.322200 0.458303 11.00000 0.01797 0.01365 = 0.01384 -0.00113 0.00303 -0.00040 C2 1 0.640043 0.530371 0.519044 11.00000 0.02964 0.01297 = 0.01286 -0.00089 0.00155 -0.00407 AFIX 23 H2A 2 0.595100 0.661383 0.506738 11.00000 -1.20000 H2B 2 0.701003 0.584440 0.499502 11.00000 -1.20000 AFIX 0 C3 1 0.650434 0.486232 0.623592 11.00000 0.02343 0.01390 = 0.01336 -0.00032 0.00005 0.00212 AFIX 23 H3A 2 0.702569 0.374550 0.638101 11.00000 -1.20000 H3B 2 0.592708 0.411595 0.642809 11.00000 -1.20000 AFIX 0 C4 1 0.668934 0.712673 0.679050 11.00000 0.02110 0.01854 = 0.01287 -0.00283 -0.00129 0.00148 AFIX 23 H4A 2 0.677754 0.673916 0.746113 11.00000 -1.20000 H4B 2 0.727161 0.786459 0.660685 11.00000 -1.20000 AFIX 0 O2 4 0.612164 0.115880 0.490423 11.00000 0.03839 0.01219 = 0.01528 0.00041 0.00126 -0.00069 O1 4 0.578218 0.371127 0.375356 11.00000 0.02863 0.01614 = 0.01327 0.00063 -0.00247 -0.00248 N1 3 0.590199 0.884687 0.663180 11.00000 0.02271 0.01371 = 0.01223 -0.00167 0.00079 -0.00082 AFIX 137 H1A 2 0.596675 0.966445 0.609715 11.00000 -1.50000 H1B 2 0.590970 0.987318 0.711838 11.00000 -1.50000 H1C 2 0.535079 0.804889 0.658335 11.00000 -1.50000 AFIX 0 HKLF 4 REM gabalt_0m in C2/c REM R1 = 0.0379 for 1305 Fo > 4sig(Fo) and 0.0542 for all 1669 data REM 82 parameters refined using 0 restraints END WGHT 0.0508 0.7087 REM Highest difference peak 0.347, deepest hole -0.189, 1-sigma level 0.048 Q1 1 0.6447 0.4989 0.5711 11.00000 0.05 0.35 Q2 1 0.6625 0.6021 0.6500 11.00000 0.05 0.34 Q3 1 0.6215 0.4185 0.4906 11.00000 0.05 0.33 Q4 1 0.5936 0.3422 0.4086 11.00000 0.05 0.19 Q5 1 0.5606 0.2601 0.3640 11.00000 0.05 0.18 Q6 1 0.7339 0.4998 0.5107 11.00000 0.05 0.17 Q7 1 0.5775 0.5083 0.3674 11.00000 0.05 0.16 Q8 1 0.5267 0.7957 0.3447 11.00000 0.05 0.16 Q9 1 0.6403 0.0970 0.5282 11.00000 0.05 0.16 Q10 1 0.6001 0.3658 0.3478 11.00000 0.05 0.15 Q11 1 0.6361 0.7997 0.6690 11.00000 0.05 0.14 Q12 1 0.5926 0.2315 0.4789 11.00000 0.05 0.14 Q13 1 0.5576 0.8965 0.2893 11.00000 0.05 0.14 Q14 1 0.6688 0.6720 0.4893 11.00000 0.05 0.13 Q15 1 0.6054 -0.0353 0.4863 11.00000 0.05 0.13 Q16 1 0.5976 0.0016 0.4688 11.00000 0.05 0.13 Q17 1 0.5229 0.4140 0.3763 11.00000 0.05 0.13 Q18 1 0.6433 0.6473 0.5054 11.00000 0.05 0.13 Q19 1 0.5549 0.6082 0.5091 11.00000 0.05 0.13 Q20 1 0.6196 0.0378 0.4506 11.00000 0.05 0.12 ; _shelx_res_checksum 83384 _shelx_hkl_file ; -19 1 1 -12.20 18.70 -19 1 2 41.50 32.00 -19 1 3 16.18 26.70 -19 1 4 75.74 14.70 -19 1 5 164.40 35.20 -19 1 6 -5.58 16.60 -19 3 2 194.40 33.30 -18 0 1 -7.50 15.40 -18 0 2 37.60 18.20 -18 0 3 -13.70 15.80 -18 0 5 28.60 23.20 -18 0 6 238.50 34.80 -18 0 7 -26.40 20.00 -18 0 8 164.00 31.40 -18 0 9 -8.20 22.50 -18 0 10 81.40 47.30 -18 2 1 -4.89 22.70 -18 2 2 255.20 32.30 -18 2 3 14.62 12.20 -18 2 4 -1.37 13.50 -18 2 5 108.61 19.50 -18 2 6 27.87 15.40 -18 2 7 99.15 39.00 -18 2 8 -16.30 19.80 -18 2 9 23.10 24.00 -17 1 1 5.12 9.10 -17 1 2 476.40 42.40 -17 1 3 623.60 47.10 -17 1 4 19.25 11.80 -17 1 5 20.90 11.70 -17 1 6 203.15 20.30 -17 1 7 201.78 13.70 -17 1 8 250.38 15.30 -17 1 9 10.33 19.20 -17 1 10 127.44 14.70 -17 1 11 163.96 11.50 -17 1 12 100.02 28.40 -17 3 1 117.45 14.10 -17 3 2 45.99 9.80 -17 3 3 19.09 15.50 -17 3 4 66.80 25.90 -17 3 5 -12.52 13.50 -17 3 6 145.30 19.50 -17 3 7 78.25 19.90 -17 3 8 20.80 23.30 -16 0 1 -6.90 14.20 -16 0 2 190.90 24.50 -16 0 3 -15.00 13.50 -16 0 4 1315.00 58.90 -16 0 5 -19.20 20.30 -16 0 6 3.40 10.60 -16 0 7 -15.11 27.00 -16 0 8 649.76 81.20 -16 0 9 4.21 10.00 -16 0 10 463.82 27.70 -16 0 11 6.33 9.30 -16 0 12 -12.90 19.10 -16 0 13 -37.40 19.70 -16 2 1 87.88 10.50 -16 2 2 83.04 7.60 -16 2 3 143.80 18.10 -16 2 4 -11.11 14.80 -16 2 5 51.13 11.00 -16 2 6 7.44 7.70 -16 2 7 110.70 17.00 -16 2 8 32.57 18.80 -16 2 9 263.64 34.30 -16 2 10 33.72 9.40 -16 2 11 -3.27 28.60 -16 2 12 300.80 39.20 -16 4 1 182.67 29.80 -16 4 2 18.54 10.90 -16 4 3 49.94 10.40 -16 4 4 31.04 12.00 -16 4 5 82.28 11.90 -16 4 6 13.88 8.90 -16 4 7 20.40 23.20 -16 4 8 347.80 39.60 -15 1 1 292.62 15.50 -15 1 2 3.53 5.70 -15 1 3 143.53 9.40 -15 1 4 69.30 8.40 -15 1 5 431.49 16.00 -15 1 6 254.53 28.90 -15 1 7 244.88 24.70 -15 1 8 40.16 8.80 -15 1 9 66.14 7.90 -15 1 10 140.16 14.50 -15 1 11 -14.56 14.30 -15 1 12 108.77 13.50 -15 1 13 81.55 12.20 -15 3 1 0.31 7.90 -15 3 2 743.04 25.60 -15 3 3 -2.90 21.30 -15 3 4 69.44 9.30 -15 3 5 232.59 14.40 -15 3 6 448.34 101.70 -15 3 7 3.44 8.30 -15 3 8 -18.60 20.90 -15 3 9 31.96 14.50 -15 3 10 106.19 24.10 -15 3 11 16.64 15.00 -15 3 12 40.70 23.70 -15 5 1 1.10 11.50 -15 5 2 362.84 28.30 -15 5 3 46.02 31.10 -15 5 4 84.30 32.90 -14 0 1 -2.52 12.50 -14 0 2 73.40 18.50 -14 0 3 1.21 6.60 -14 0 4 1031.56 26.50 -14 0 5 4.92 18.20 -14 0 6 234.04 19.30 -14 0 7 7.63 7.30 -14 0 8 1432.66 34.60 -14 0 9 -17.76 20.50 -14 0 10 -6.36 17.60 -14 0 11 -15.28 26.90 -14 0 12 275.60 32.40 -14 0 13 -14.90 16.00 -14 0 14 236.40 33.40 -14 2 1 267.73 14.30 -14 2 2 210.41 13.10 -14 2 3 120.63 9.80 -14 2 4 8.03 5.10 -14 2 5 -4.64 18.70 -14 2 6 0.76 7.60 -14 2 7 11.53 10.20 -14 2 8 5.43 23.80 -14 2 9 38.59 12.20 -14 2 10 24.31 23.70 -14 2 11 238.46 17.60 -14 2 12 95.74 15.20 -14 2 13 45.23 10.00 -14 2 14 267.40 36.30 -14 2 15 70.80 31.00 -14 4 1 217.36 31.90 -14 4 2 510.87 25.50 -14 4 3 11.12 8.10 -14 4 4 150.74 19.20 -14 4 5 174.03 16.30 -14 4 6 10.79 10.30 -14 4 7 670.34 20.70 -14 4 8 -6.21 12.70 -14 4 9 41.42 10.20 -14 4 10 114.49 23.40 -14 4 11 43.40 15.40 -13 1 1 77.57 9.30 -13 1 2 9.50 6.30 -13 1 3 1401.34 22.60 -13 1 4 312.03 9.30 -13 1 5 1571.22 25.00 -13 1 6 41.08 11.20 -13 1 7 206.44 11.70 -13 1 8 362.99 29.20 -13 1 9 215.69 19.20 -13 1 10 -4.98 16.10 -13 1 11 641.39 21.30 -13 1 12 64.42 8.80 -13 1 13 16.58 16.10 -13 1 14 10.30 9.50 -13 1 15 35.84 12.40 -13 3 1 97.40 13.70 -13 3 2 4.64 4.90 -13 3 3 230.25 13.40 -13 3 4 213.77 12.80 -13 3 5 2.58 10.00 -13 3 6 45.73 15.00 -13 3 7 -0.57 16.10 -13 3 8 48.29 10.30 -13 3 9 121.38 10.20 -13 3 10 46.71 11.10 -13 3 11 9.81 8.10 -13 3 12 677.86 47.00 -13 3 13 63.30 11.00 -13 3 14 116.48 21.90 -13 5 1 -1.59 16.20 -13 5 2 2.55 8.90 -13 5 3 24.61 13.40 -13 5 4 1121.51 20.00 -13 5 5 608.05 23.90 -13 5 6 -4.76 19.10 -13 5 7 315.44 24.80 -13 5 8 -8.79 14.80 -13 5 9 28.50 26.50 -12 0 1 -7.91 10.20 -12 0 2 3670.33 67.60 -12 0 3 -1.33 6.40 -12 0 4 4625.31 71.20 -12 0 5 1.85 8.30 -12 0 6 20.01 7.00 -12 0 7 0.30 8.40 -12 0 8 1149.52 29.60 -12 0 9 -1.69 12.00 -12 0 10 863.43 26.60 -12 0 11 7.51 7.60 -12 0 12 283.21 20.50 -12 0 13 -36.40 13.80 -12 0 14 312.80 33.50 -12 0 15 -44.90 13.40 -12 0 16 82.30 26.00 -12 2 1 281.23 13.40 -12 2 2 -0.73 10.10 -12 2 3 81.81 11.70 -12 2 4 83.58 13.60 -12 2 5 -8.39 10.70 -12 2 6 -2.42 15.90 -12 2 7 298.13 13.60 -12 2 8 110.85 10.80 -12 2 9 896.06 25.20 -12 2 10 546.42 31.90 -12 2 11 127.85 10.20 -12 2 12 346.81 24.00 -12 2 13 60.35 8.80 -12 2 14 48.12 12.20 -12 2 15 1028.28 23.00 -12 2 16 249.90 35.80 -12 4 1 639.38 33.20 -12 4 2 12.39 13.50 -12 4 3 10.68 8.10 -12 4 4 262.56 16.40 -12 4 5 150.20 10.50 -12 4 6 171.19 11.30 -12 4 7 50.70 8.70 -12 4 8 1.31 9.60 -12 4 9 190.38 13.80 -12 4 10 12.12 9.10 -12 4 11 49.68 16.80 -12 4 12 14.41 10.70 -12 4 13 -30.66 14.40 -12 4 14 29.30 28.60 -12 6 1 222.29 23.50 -12 6 2 306.75 19.90 -12 6 3 131.50 18.10 -12 6 4 -25.20 21.10 -12 6 5 5.50 23.40 -12 6 6 60.80 29.60 -11 1 1 987.89 14.20 -11 1 2 3.94 4.00 -11 1 3 1248.88 21.90 -11 1 4 61.98 6.20 -11 1 5 512.38 10.40 -11 1 6 915.08 35.20 -11 1 7 9.05 5.70 -11 1 8 -14.51 10.80 -11 1 9 1.99 5.50 -11 1 10 25.80 7.90 -11 1 11 39.77 7.60 -11 1 12 169.08 10.50 -11 1 13 10.11 10.80 -11 1 14 190.47 17.80 -11 1 15 138.68 19.20 -11 1 16 161.32 19.00 -11 3 1 85.37 13.60 -11 3 2 1254.98 22.30 -11 3 3 849.14 20.10 -11 3 4 1.17 4.20 -11 3 5 -3.86 11.70 -11 3 6 1211.70 32.10 -11 3 7 16.73 5.50 -11 3 8 346.16 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42.62 11.70 -7 1 16 346.94 29.20 -7 1 17 13.49 9.80 -7 1 18 94.99 15.80 -7 1 19 -4.11 13.70 -7 3 1 954.52 13.20 -7 3 2 696.64 10.60 -7 3 3 2658.73 28.10 -7 3 4 713.86 17.50 -7 3 5 825.62 17.30 -7 3 6 320.91 11.80 -7 3 7 7.14 5.70 -7 3 8 1454.61 28.60 -7 3 9 1020.78 19.70 -7 3 10 28.77 6.80 -7 3 11 40.90 6.60 -7 3 12 423.64 11.80 -7 3 13 14.89 6.80 -7 3 14 263.26 12.50 -7 3 15 18.89 7.70 -7 3 16 499.17 23.10 -7 3 17 54.78 12.50 -7 3 18 82.54 19.90 -7 5 1 234.65 15.40 -7 5 2 218.64 14.10 -7 5 3 1549.07 39.80 -7 5 4 46.07 6.60 -7 5 5 74.01 10.00 -7 5 6 382.48 21.30 -7 5 7 12.71 10.00 -7 5 8 650.23 33.60 -7 5 9 1025.71 20.20 -7 5 10 545.33 22.60 -7 5 11 96.65 9.30 -7 5 12 28.67 8.50 -7 5 13 5.48 6.60 -7 5 14 115.28 24.30 -7 7 1 164.57 20.20 -7 7 2 7.58 10.30 -7 7 3 67.34 13.50 -7 7 4 146.68 28.20 -7 7 5 9.49 10.50 -7 7 6 79.90 28.40 -7 7 7 552.44 49.60 -6 0 1 -6.43 5.00 -6 0 2 31.50 2.30 -6 0 3 0.61 1.70 -6 0 4 1424.16 16.50 -6 0 5 1.90 2.60 -6 0 6 144.89 4.80 -6 0 7 -5.07 6.40 -6 0 8 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10 186.01 11.80 6 6 11 85.20 27.60 7 1 0 1909.35 17.10 7 1 1 948.55 10.50 7 1 2 611.93 8.20 7 1 3 949.78 12.60 7 1 4 38.11 3.00 7 1 5 787.81 10.00 7 1 6 1568.65 17.70 7 1 7 1009.99 14.00 7 1 8 47.66 4.80 7 1 9 -4.01 8.90 7 1 10 16.57 6.80 7 1 11 128.36 9.40 7 1 12 463.55 18.20 7 1 13 17.44 7.10 7 1 14 -10.09 21.60 7 1 15 77.62 11.00 7 1 16 33.18 11.40 7 1 17 -1.98 16.00 7 1 18 100.80 33.60 7 3 0 979.93 12.90 7 3 1 419.79 8.50 7 3 2 1237.42 21.10 7 3 3 954.41 15.50 7 3 4 13.14 3.40 7 3 5 756.82 17.10 7 3 6 -1.25 11.20 7 3 7 324.30 12.40 7 3 8 2918.47 38.80 7 3 9 879.81 20.90 7 3 10 175.76 9.70 7 3 11 25.35 9.30 7 3 12 1363.83 29.80 7 3 13 198.62 13.90 7 3 14 -4.12 16.00 7 3 15 1004.16 15.00 7 3 16 31.65 12.80 7 3 17 -21.80 25.40 7 5 0 861.40 24.00 7 5 1 45.97 10.40 7 5 2 24.32 13.20 7 5 3 451.66 19.50 7 5 4 364.74 17.20 7 5 5 71.57 7.50 7 5 6 127.50 8.90 7 5 7 -7.20 15.70 7 5 8 175.55 13.10 7 5 9 68.17 9.40 7 5 10 1.46 6.90 7 5 11 610.36 22.40 7 5 12 743.12 30.10 7 5 13 76.50 54.50 7 7 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12 216.03 13.90 8 4 13 600.44 24.00 8 4 14 88.46 16.80 8 4 15 63.70 31.90 8 6 0 102.34 14.10 8 6 1 26.30 19.60 8 6 2 567.72 44.50 8 6 3 1636.69 42.60 8 6 4 12.07 8.60 8 6 5 844.78 22.60 8 6 6 -16.83 21.70 8 6 7 62.59 20.00 8 6 8 346.09 22.80 8 6 9 449.89 33.30 8 6 10 100.50 32.00 9 1 0 3031.12 27.40 9 1 1 585.72 9.20 9 1 2 1939.90 19.00 9 1 3 1490.49 18.50 9 1 4 -0.21 9.80 9 1 5 67.75 6.40 9 1 6 59.30 6.30 9 1 7 9.36 7.10 9 1 8 1042.74 23.20 9 1 9 2472.28 34.20 9 1 10 1947.57 51.40 9 1 11 146.49 11.80 9 1 12 287.09 18.70 9 1 13 364.33 27.90 9 1 14 12.59 8.00 9 1 15 858.79 23.60 9 1 16 397.90 21.50 9 3 0 316.28 13.50 9 3 1 204.11 12.40 9 3 2 550.84 10.90 9 3 3 32.52 6.20 9 3 4 26.02 9.10 9 3 5 154.35 14.60 9 3 6 284.14 11.90 9 3 7 261.86 15.80 9 3 8 161.42 11.40 9 3 9 180.38 12.40 9 3 10 188.02 12.30 9 3 11 35.31 11.50 9 3 12 215.44 17.30 9 3 13 35.45 15.00 9 3 14 43.22 10.40 9 3 15 130.49 18.40 9 5 0 48.49 10.10 9 5 1 55.13 12.70 9 5 2 1109.33 22.90 9 5 3 13.59 11.00 9 5 4 9.90 8.00 9 5 5 130.56 10.60 9 5 6 2.79 8.30 9 5 7 81.66 21.40 9 5 8 251.06 12.10 9 5 9 351.44 17.90 9 5 10 357.42 16.90 9 5 11 272.05 14.00 9 5 12 15.01 12.00 10 0 0 3024.16 36.20 10 0 1 -2.96 9.10 10 0 2 4.68 9.60 10 0 3 3.03 9.10 10 0 4 35.72 8.80 10 0 5 -8.16 7.90 10 0 6 4177.18 80.10 10 0 7 -6.53 9.90 10 0 8 26.69 10.00 10 0 9 -0.38 11.20 10 0 10 1434.32 34.40 10 0 11 -5.92 13.60 10 0 12 578.53 27.00 10 0 13 -7.57 15.40 10 0 14 43.83 16.40 10 0 15 32.90 23.80 10 0 16 402.40 54.40 10 2 0 1084.69 15.50 10 2 1 1185.31 22.80 10 2 2 528.87 10.30 10 2 3 9.37 5.00 10 2 4 -0.39 16.80 10 2 5 -0.40 9.60 10 2 6 415.17 9.80 10 2 7 830.06 22.40 10 2 8 392.77 12.20 10 2 9 141.78 13.50 10 2 10 12.49 12.60 10 2 11 25.06 14.40 10 2 12 21.00 9.70 10 2 13 7.85 8.90 10 2 14 16.09 9.90 10 2 15 164.98 20.50 10 4 0 3204.43 63.00 10 4 1 30.12 7.00 10 4 2 10.13 5.40 10 4 3 35.61 6.30 10 4 4 -4.77 17.40 10 4 5 46.41 7.90 10 4 6 2114.02 27.80 10 4 7 388.71 19.00 10 4 8 441.66 24.00 10 4 9 214.04 14.40 10 4 10 -12.30 18.30 10 4 11 2.94 12.80 10 4 12 89.80 14.60 10 4 13 153.63 14.60 10 6 0 -3.47 38.00 10 6 1 154.74 47.90 10 6 2 82.81 30.10 10 6 3 497.48 26.80 10 6 4 129.81 34.40 10 6 5 19.13 11.00 10 6 6 23.31 8.40 10 6 7 145.71 16.40 11 1 0 1059.72 15.90 11 1 1 52.36 6.50 11 1 2 -4.03 12.10 11 1 3 191.81 7.90 11 1 4 16.71 9.80 11 1 5 933.27 24.10 11 1 6 425.72 11.50 11 1 7 18.32 9.80 11 1 8 -0.32 12.40 11 1 9 323.18 16.60 11 1 10 -2.13 13.80 11 1 11 59.07 6.50 11 1 12 212.43 11.80 11 1 13 11.00 11.00 11 1 14 -8.32 25.20 11 1 15 26.15 17.60 11 1 16 2.20 19.60 11 3 0 288.94 10.40 11 3 1 76.09 10.10 11 3 2 27.43 6.70 11 3 3 325.62 12.60 11 3 4 29.93 9.50 11 3 5 747.99 16.80 11 3 6 280.17 16.10 11 3 7 136.73 8.90 11 3 8 613.75 20.50 11 3 9 -2.36 17.50 11 3 10 152.01 27.40 11 3 11 142.97 14.70 11 3 12 682.28 31.00 11 3 13 449.49 22.30 11 5 0 15.64 8.50 11 5 1 40.19 9.90 11 5 2 264.36 14.40 11 5 3 58.44 8.50 11 5 4 29.28 9.20 11 5 5 6.08 13.20 11 5 6 101.05 11.20 11 5 7 0.13 13.80 11 5 8 9.92 10.10 11 5 9 214.50 15.00 12 0 0 1800.43 34.30 12 0 1 -11.32 9.10 12 0 2 435.05 41.80 12 0 3 3.56 9.50 12 0 4 977.01 74.90 12 0 5 -7.26 26.20 12 0 6 1485.45 34.50 12 0 7 -1.76 11.50 12 0 8 140.83 17.20 12 0 9 7.68 7.40 12 0 10 132.29 15.90 12 0 11 -4.94 13.70 12 0 12 420.95 28.60 12 0 13 -4.67 15.00 12 0 14 228.69 37.80 12 2 0 139.70 10.10 12 2 1 76.38 6.90 12 2 2 78.23 7.10 12 2 3 391.63 10.40 12 2 4 7.78 11.00 12 2 5 300.56 16.10 12 2 6 672.49 15.90 12 2 7 9.57 5.30 12 2 8 59.24 10.20 12 2 9 797.09 20.10 12 2 10 98.56 9.40 12 2 11 215.25 33.90 12 2 12 9.24 8.70 12 2 13 -4.28 14.60 12 2 14 96.10 26.90 12 4 0 127.96 10.30 12 4 1 42.95 8.40 12 4 2 345.37 15.90 12 4 3 3.10 6.70 12 4 4 337.51 18.50 12 4 5 159.43 18.50 12 4 6 385.54 39.80 12 4 7 177.39 19.80 12 4 8 16.39 16.80 12 4 9 -3.27 16.20 12 4 10 485.27 22.20 12 4 11 22.98 10.30 12 4 12 -16.10 21.10 12 6 0 12.88 18.60 12 6 1 49.31 17.00 12 6 2 365.20 39.20 12 6 3 970.50 59.20 13 1 0 824.66 22.30 13 1 1 273.63 11.70 13 1 2 391.64 13.60 13 1 3 1495.33 44.30 13 1 4 -5.13 12.30 13 1 5 76.18 9.40 13 1 6 29.42 10.00 13 1 7 32.24 6.50 13 1 8 1527.01 30.10 13 1 9 555.06 23.60 13 1 10 633.76 24.70 13 1 11 315.92 17.10 13 1 12 111.68 10.00 13 1 13 -16.13 17.10 13 1 14 66.50 26.00 13 3 0 35.07 10.10 13 3 1 19.15 9.50 13 3 2 221.78 14.60 13 3 3 12.91 9.30 13 3 4 142.17 13.60 13 3 5 212.11 15.20 13 3 6 1.02 7.70 13 3 7 21.96 7.60 13 3 8 -5.30 18.10 13 3 9 -2.96 16.50 13 3 10 229.84 19.40 13 3 11 63.89 18.10 13 3 12 31.30 22.90 13 5 0 10.57 16.60 13 5 1 95.77 11.80 13 5 2 449.49 27.90 13 5 3 -3.64 12.30 13 5 4 73.70 10.50 13 5 5 34.70 9.60 13 5 6 0.61 9.90 13 5 7 84.00 27.20 14 0 0 132.07 16.50 14 0 1 3.31 7.10 14 0 2 154.30 14.50 14 0 3 8.29 7.30 14 0 4 197.57 17.80 14 0 5 -8.10 14.10 14 0 6 255.95 20.80 14 0 7 -6.27 29.10 14 0 8 423.98 24.90 14 0 9 -12.01 28.80 14 0 10 126.31 14.10 14 0 11 -3.37 15.70 14 0 12 323.35 23.50 14 0 13 46.40 21.50 14 2 0 1067.15 23.20 14 2 1 442.11 17.90 14 2 2 8.58 10.60 14 2 3 405.30 22.10 14 2 4 -4.19 14.20 14 2 5 116.85 15.10 14 2 6 474.97 22.50 14 2 7 981.02 29.90 14 2 8 -6.93 13.60 14 2 9 164.23 12.70 14 2 10 45.66 12.40 14 2 11 62.76 11.20 14 2 12 38.90 25.30 14 4 0 210.69 14.10 14 4 1 15.88 10.90 14 4 2 26.02 8.30 14 4 3 5.55 8.60 14 4 4 183.72 16.10 14 4 5 15.65 10.90 14 4 6 378.60 36.10 14 4 7 329.18 34.20 14 4 8 155.89 25.80 15 1 0 332.71 16.30 15 1 1 25.21 13.70 15 1 2 9.53 6.10 15 1 3 81.44 7.50 15 1 4 71.53 7.70 15 1 5 141.50 9.50 15 1 6 129.16 9.30 15 1 7 159.76 14.60 15 1 8 82.62 8.00 15 1 9 120.37 10.80 15 1 10 12.29 11.70 15 1 11 49.65 11.00 15 1 12 11.00 19.40 15 3 0 -5.75 13.80 15 3 1 118.17 9.80 15 3 2 19.84 16.60 15 3 3 39.57 10.50 15 3 4 293.37 22.80 15 3 5 264.15 14.20 15 3 6 138.96 14.20 15 3 7 100.81 24.10 15 3 8 22.43 14.40 15 5 0 279.59 20.80 15 5 1 91.00 20.00 15 5 2 328.80 35.80 15 5 3 48.52 28.40 15 5 4 8.10 23.20 16 0 0 842.20 47.30 16 0 1 21.70 16.60 16 0 2 137.00 12.10 16 0 3 -18.11 21.40 16 0 4 4.49 9.50 16 0 5 -2.99 14.30 16 0 6 1100.87 49.90 16 0 7 7.34 17.10 16 0 8 107.65 13.70 16 0 9 -4.41 12.90 16 0 10 -8.47 13.70 16 2 0 -1.82 20.60 16 2 1 38.86 10.80 16 2 2 134.07 25.20 16 2 3 232.84 14.30 16 2 4 213.69 13.60 16 2 5 16.76 8.40 16 2 6 38.26 13.90 16 2 7 222.91 17.70 16 2 8 169.51 18.40 16 2 9 31.62 14.70 16 2 10 23.30 24.80 16 4 0 3.23 11.70 16 4 1 44.49 15.50 16 4 2 100.31 13.90 16 4 3 21.31 17.90 16 4 4 91.49 19.30 16 4 5 17.00 23.40 17 1 0 42.86 12.50 17 1 1 18.86 9.40 17 1 2 21.16 9.40 17 1 3 579.23 27.50 17 1 4 102.84 22.60 17 1 5 3.00 8.90 17 1 6 66.56 10.10 17 1 7 44.18 9.30 17 1 8 545.61 27.70 17 1 9 -8.06 14.20 17 3 0 364.88 38.40 17 3 1 62.97 19.20 17 3 2 17.38 12.80 17 3 3 6.54 8.40 17 3 4 207.89 20.20 17 3 5 299.63 31.10 17 3 7 35.00 22.30 18 0 0 -1.10 17.40 18 0 1 6.60 18.10 18 0 2 232.30 30.80 18 0 3 -14.70 17.50 18 0 4 237.70 30.80 18 0 5 7.83 14.90 18 0 6 254.42 19.10 18 0 7 -30.10 20.40 18 0 8 215.40 35.50 18 2 0 306.24 36.20 18 2 1 139.66 29.50 18 2 2 42.60 20.20 18 2 3 99.92 18.00 18 2 4 27.88 8.10 18 2 5 68.76 18.90 19 1 0 2.54 8.80 19 1 1 96.15 16.50 19 1 2 11.51 10.60 19 1 4 8.80 22.90 19 1 5 60.20 28.80 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 3964 _database_code_depnum_ccdc_archive 'CCDC 969074'