data_Tanveer-3a _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H17 Cl O3' _chemical_formula_sum 'C13 H17 Cl O3' _chemical_formula_weight 256.71 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 33 _space_group_name_H-M_alt 'P n a 21' _space_group_name_Hall 'P 2c -2n' _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' _cell_length_a 28.508(2) _cell_length_b 5.4891(4) _cell_length_c 8.1976(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1282.79(18) _cell_formula_units_Z 4 _cell_measurement_temperature 147(2) _cell_measurement_reflns_used 1737 _cell_measurement_theta_min 2.87 _cell_measurement_theta_max 23.06 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.329 _exptl_crystal_F_000 544 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.360 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.080 _exptl_absorpt_coefficient_mu 0.292 _shelx_estimated_absorpt_T_min 0.902 _shelx_estimated_absorpt_T_max 0.977 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6926 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_special_details ? _diffrn_ambient_temperature 147(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'sealed tube with Bruker Triumph monochromator' _diffrn_measurement_device_type 'Bruker Kappa APEX-DUO CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 8900 _diffrn_reflns_av_unetI/netI 0.0638 _diffrn_reflns_av_R_equivalents 0.0568 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.858 _diffrn_reflns_theta_max 27.632 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.980 _diffrn_reflns_point_group_measured_fraction_full 0.988 _reflns_number_total 2931 _reflns_number_gt 2455 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.842 _reflns_Friedel_fraction_max 0.963 _reflns_Friedel_fraction_full 0.975 _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 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'APEX2' _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_structure_solution 'SHELXT (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0338P)^2^+0.1798P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Flack x determined using 914 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.12(5) _chemical_absolute_configuration 'ad' _refine_ls_number_reflns 2931 _refine_ls_number_parameters 156 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0594 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.0885 _refine_ls_wR_factor_gt 0.0831 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 Cl1 Cl 0.17772(3) 0.23106(14) 0.65431(13) 0.01762(19) Uani 1 1 d . . . . . O1 O 0.34405(8) -0.1706(4) 0.5487(3) 0.0195(6) Uani 1 1 d . . . . . O2 O 0.32454(8) 0.1959(4) 0.4488(3) 0.0178(6) Uani 1 1 d . . . . . O3 O 0.26484(8) 0.5400(4) 0.6008(3) 0.0196(6) Uani 1 1 d . . . . . H3O H 0.2887 0.6200 0.5732 0.038(13) Uiso 1 1 d R . . . . C1 C 0.35507(12) 0.0227(6) 0.4887(4) 0.0150(7) Uani 1 1 d . . . . . C2 C 0.27512(11) 0.1459(6) 0.4761(5) 0.0167(8) Uani 1 1 d . . . . . H2A H 0.2703 0.0701 0.5844 0.020 Uiso 1 1 calc R U . . . H2B H 0.2628 0.0347 0.3913 0.020 Uiso 1 1 calc R U . . . C3 C 0.25092(11) 0.3901(6) 0.4675(5) 0.0148(7) Uani 1 1 d . . . . . H3A H 0.2609 0.4722 0.3642 0.018 Uiso 1 1 calc R U . . . C4 C 0.19785(11) 0.3702(6) 0.4661(4) 0.0141(7) Uani 1 1 d . . . . . H4A H 0.1887 0.2613 0.3736 0.017 Uiso 1 1 calc R U . . . C5 C 0.17360(11) 0.6131(6) 0.4425(5) 0.0172(8) Uani 1 1 d . . . . . H5A H 0.1873 0.6946 0.3459 0.021 Uiso 1 1 calc R U . . . H5B H 0.1802 0.7170 0.5386 0.021 Uiso 1 1 calc R U . . . C6 C 0.12074(13) 0.5965(6) 0.4197(5) 0.0192(8) Uani 1 1 d . . . . . H6A H 0.1062 0.5422 0.5231 0.023 Uiso 1 1 calc R U . . . H6B H 0.1137 0.4728 0.3352 0.023 Uiso 1 1 calc R U . . . C7 C 0.09921(14) 0.8402(7) 0.3689(6) 0.0276(10) Uani 1 1 d . . . . . H7A H 0.0656 0.8189 0.3492 0.041 Uiso 1 1 calc R U . . . H7B H 0.1144 0.8980 0.2689 0.041 Uiso 1 1 calc R U . . . H7C H 0.1039 0.9599 0.4561 0.041 Uiso 1 1 calc R U . . . C8 C 0.40441(12) 0.0961(6) 0.4558(5) 0.0163(7) Uani 1 1 d . . . . . C9 C 0.41561(14) 0.3067(7) 0.3699(5) 0.0249(9) Uani 1 1 d . . . . . H9A H 0.3914 0.4076 0.3275 0.030 Uiso 1 1 calc R U . . . C10 C 0.46218(14) 0.3681(7) 0.3466(6) 0.0314(10) Uani 1 1 d . . . . . H10A H 0.4699 0.5111 0.2872 0.038 Uiso 1 1 calc R U . . . C11 C 0.49752(14) 0.2234(7) 0.4091(6) 0.0319(11) Uani 1 1 d . . . . . H11A H 0.5294 0.2673 0.3926 0.038 Uiso 1 1 calc R U . . . C12 C 0.48658(13) 0.0152(7) 0.4953(5) 0.0288(10) Uani 1 1 d . . . . . H12A H 0.5109 -0.0830 0.5392 0.035 Uiso 1 1 calc R U . . . C13 C 0.44006(12) -0.0509(7) 0.5182(5) 0.0225(9) Uani 1 1 d . . . . . H13A H 0.4325 -0.1956 0.5761 0.027 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 Cl1 0.0162(3) 0.0190(4) 0.0177(4) 0.0022(4) 0.0033(5) -0.0025(3) O1 0.0158(13) 0.0181(12) 0.0246(15) 0.0021(11) -0.0011(11) -0.0035(10) O2 0.0112(12) 0.0196(12) 0.0225(14) 0.0020(11) 0.0030(11) 0.0011(9) O3 0.0157(13) 0.0214(13) 0.0218(15) -0.0066(11) 0.0009(11) -0.0053(10) C1 0.0168(18) 0.0161(17) 0.012(2) -0.0027(15) -0.0004(14) 0.0003(13) C2 0.0116(16) 0.0178(17) 0.021(2) -0.0024(16) 0.0006(15) -0.0017(13) C3 0.0141(17) 0.0164(16) 0.0138(18) -0.0008(16) 0.0018(15) -0.0022(12) C4 0.0145(17) 0.0177(16) 0.0101(18) -0.0001(15) 0.0018(15) -0.0017(13) C5 0.0138(17) 0.0182(18) 0.019(2) 0.0001(16) 0.0009(15) 0.0009(13) C6 0.0150(18) 0.0197(18) 0.023(2) 0.0008(17) -0.0020(15) 0.0011(14) C7 0.024(2) 0.025(2) 0.034(3) -0.004(2) -0.0083(19) 0.0071(16) C8 0.0159(18) 0.0156(16) 0.0173(19) -0.0029(16) 0.0026(16) -0.0014(13) C9 0.0181(19) 0.0229(19) 0.034(3) 0.0008(18) 0.0030(17) 0.0035(14) C10 0.026(2) 0.023(2) 0.045(3) 0.002(2) 0.013(2) -0.0055(16) C11 0.0161(19) 0.033(2) 0.047(3) -0.006(2) 0.0075(18) -0.0072(16) C12 0.0151(19) 0.033(2) 0.039(3) -0.001(2) 0.0034(18) 0.0026(15) C13 0.0166(19) 0.023(2) 0.028(3) 0.0017(17) 0.0030(17) 0.0017(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 Cl1 C4 1.815(4) . ? O1 C1 1.210(4) . ? O2 C1 1.330(4) . ? O2 C2 1.453(4) . ? O3 C3 1.425(4) . ? O3 H3O 0.8399 . ? C1 C8 1.488(5) . ? C2 C3 1.509(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.517(4) . ? C3 H3A 1.0000 . ? C4 C5 1.514(5) . ? C4 H4A 1.0000 . ? C5 C6 1.521(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.529(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.391(5) . ? C8 C13 1.395(5) . ? C9 C10 1.383(5) . ? C9 H9A 0.9500 . ? C10 C11 1.381(6) . ? C10 H10A 0.9500 . ? C11 C12 1.379(5) . ? C11 H11A 0.9500 . ? C12 C13 1.388(5) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? 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 C1 O2 C2 117.5(3) . . ? C3 O3 H3O 108.7 . . ? O1 C1 O2 123.8(3) . . ? O1 C1 C8 123.8(3) . . ? O2 C1 C8 112.4(3) . . ? O2 C2 C3 105.6(2) . . ? O2 C2 H2A 110.6 . . ? C3 C2 H2A 110.6 . . ? O2 C2 H2B 110.6 . . ? C3 C2 H2B 110.6 . . ? H2A C2 H2B 108.8 . . ? O3 C3 C2 110.5(3) . . ? O3 C3 C4 109.0(3) . . ? C2 C3 C4 113.1(3) . . ? O3 C3 H3A 108.0 . . ? C2 C3 H3A 108.0 . . ? C4 C3 H3A 108.0 . . ? C5 C4 C3 113.1(3) . . ? C5 C4 Cl1 109.5(3) . . ? C3 C4 Cl1 109.8(2) . . ? C5 C4 H4A 108.1 . . ? C3 C4 H4A 108.1 . . ? Cl1 C4 H4A 108.1 . . ? C4 C5 C6 114.5(3) . . ? C4 C5 H5A 108.6 . . ? C6 C5 H5A 108.6 . . ? C4 C5 H5B 108.6 . . ? C6 C5 H5B 108.6 . . ? H5A C5 H5B 107.6 . . ? C5 C6 C7 112.2(3) . . ? C5 C6 H6A 109.2 . . ? C7 C6 H6A 109.2 . . ? C5 C6 H6B 109.2 . . ? C7 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C13 120.0(3) . . ? C9 C8 C1 122.3(3) . . ? C13 C8 C1 117.8(3) . . ? C10 C9 C8 119.5(4) . . ? C10 C9 H9A 120.2 . . ? C8 C9 H9A 120.2 . . ? C11 C10 C9 120.6(4) . . ? C11 C10 H10A 119.7 . . ? C9 C10 H10A 119.7 . . ? C12 C11 C10 120.1(4) . . ? C12 C11 H11A 120.0 . . ? C10 C11 H11A 120.0 . . ? C11 C12 C13 120.1(4) . . ? C11 C12 H12A 119.9 . . ? C13 C12 H12A 119.9 . . ? C12 C13 C8 119.7(3) . . ? C12 C13 H13A 120.1 . . ? C8 C13 H13A 120.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 O2 C1 O1 -1.3(5) . . . . ? C2 O2 C1 C8 -179.7(3) . . . . ? C1 O2 C2 C3 164.1(3) . . . . ? O2 C2 C3 O3 -66.9(4) . . . . ? O2 C2 C3 C4 170.7(3) . . . . ? O3 C3 C4 C5 61.8(4) . . . . ? C2 C3 C4 C5 -175.0(3) . . . . ? O3 C3 C4 Cl1 -61.0(3) . . . . ? C2 C3 C4 Cl1 62.3(4) . . . . ? C3 C4 C5 C6 172.9(3) . . . . ? Cl1 C4 C5 C6 -64.2(4) . . . . ? C4 C5 C6 C7 -170.6(3) . . . . ? O1 C1 C8 C9 172.4(4) . . . . ? O2 C1 C8 C9 -9.2(5) . . . . ? O1 C1 C8 C13 -9.3(6) . . . . ? O2 C1 C8 C13 169.1(3) . . . . ? C13 C8 C9 C10 0.2(6) . . . . ? C1 C8 C9 C10 178.4(4) . . . . ? C8 C9 C10 C11 -0.5(7) . . . . ? C9 C10 C11 C12 0.1(7) . . . . ? C10 C11 C12 C13 0.7(6) . . . . ? C11 C12 C13 C8 -1.0(6) . . . . ? C9 C8 C13 C12 0.5(6) . . . . ? C1 C8 C13 C12 -177.8(4) . . . . ? 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 O3 H3O O1 0.84 1.96 2.794(3) 169.7 1_565 _refine_diff_density_max 0.282 _refine_diff_density_min -0.279 _refine_diff_density_rms 0.056 _shelx_res_file ; d1557_a.res created by SHELXL-2014/7 TITL d1557_a.res in Pna2(1) TITL d1557 in Pna2(1) CELL 0.71073 28.5081 5.4891 8.1976 90.000 90.000 90.000 ZERR 4.000 0.0023 0.0004 0.0007 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, 1/2+Z SYMM 1/2+X, 1/2-Y, Z SYMM 1/2-X, 1/2+Y, 1/2+Z SFAC C H O CL UNIT 52 68 12 4 TEMP -126.170 SIZE 0.08 0.10 0.36 ACTA L.S. 5 BOND $H CONF HTAB FMAP 2 PLAN 20 EQIV $1 x, y+1, z HTAB O3 O1_$1 WGHT 0.033800 0.179800 FVAR 0.51660 CL1 4 0.177715 0.231064 0.654311 11.00000 0.01619 0.01899 = 0.01768 0.00223 0.00332 -0.00251 O1 3 0.344054 -0.170561 0.548682 11.00000 0.01578 0.01806 = 0.02464 0.00205 -0.00114 -0.00353 O2 3 0.324537 0.195884 0.448752 11.00000 0.01117 0.01958 = 0.02253 0.00201 0.00298 0.00107 O3 3 0.264845 0.540013 0.600816 11.00000 0.01571 0.02140 = 0.02183 -0.00663 0.00093 -0.00533 AFIX 3 H3O 2 0.288665 0.620033 0.573166 11.00000 0.03792 AFIX 0 C1 1 0.355068 0.022677 0.488741 11.00000 0.01676 0.01606 = 0.01232 -0.00270 -0.00041 0.00030 C2 1 0.275122 0.145948 0.476112 11.00000 0.01162 0.01777 = 0.02060 -0.00236 0.00062 -0.00174 AFIX 23 H2A 2 0.270308 0.070099 0.584394 11.00000 -1.20000 H2B 2 0.262790 0.034746 0.391253 11.00000 -1.20000 AFIX 0 C3 1 0.250924 0.390084 0.467467 11.00000 0.01408 0.01638 = 0.01383 -0.00083 0.00184 -0.00218 AFIX 13 H3A 2 0.260906 0.472159 0.364241 11.00000 -1.20000 AFIX 0 C4 1 0.197853 0.370189 0.466053 11.00000 0.01451 0.01768 = 0.01006 -0.00005 0.00183 -0.00173 AFIX 13 H4A 2 0.188665 0.261314 0.373613 11.00000 -1.20000 AFIX 0 C5 1 0.173599 0.613112 0.442503 11.00000 0.01379 0.01822 = 0.01949 0.00009 0.00089 0.00091 AFIX 23 H5A 2 0.187303 0.694552 0.345860 11.00000 -1.20000 H5B 2 0.180155 0.716970 0.538569 11.00000 -1.20000 AFIX 0 C6 1 0.120738 0.596505 0.419656 11.00000 0.01498 0.01970 = 0.02294 0.00084 -0.00204 0.00109 AFIX 23 H6A 2 0.106171 0.542180 0.523074 11.00000 -1.20000 H6B 2 0.113691 0.472827 0.335241 11.00000 -1.20000 AFIX 0 C7 1 0.099210 0.840194 0.368890 11.00000 0.02412 0.02515 = 0.03366 -0.00354 -0.00829 0.00711 AFIX 137 H7A 2 0.065552 0.818886 0.349194 11.00000 -1.50000 H7B 2 0.114398 0.897953 0.268860 11.00000 -1.50000 H7C 2 0.103884 0.959892 0.456087 11.00000 -1.50000 AFIX 0 C8 1 0.404413 0.096084 0.455796 11.00000 0.01589 0.01564 = 0.01733 -0.00291 0.00256 -0.00135 C9 1 0.415608 0.306670 0.369893 11.00000 0.01807 0.02294 = 0.03380 0.00083 0.00297 0.00351 AFIX 43 H9A 2 0.391439 0.407602 0.327492 11.00000 -1.20000 AFIX 0 C10 1 0.462177 0.368107 0.346632 11.00000 0.02595 0.02276 = 0.04544 0.00174 0.01317 -0.00550 AFIX 43 H10A 2 0.469929 0.511113 0.287185 11.00000 -1.20000 AFIX 0 C11 1 0.497524 0.223387 0.409068 11.00000 0.01612 0.03304 = 0.04657 -0.00635 0.00746 -0.00719 AFIX 43 H11A 2 0.529408 0.267268 0.392569 11.00000 -1.20000 AFIX 0 C12 1 0.486582 0.015246 0.495336 11.00000 0.01506 0.03262 = 0.03877 -0.00051 0.00341 0.00261 AFIX 43 H12A 2 0.510942 -0.083037 0.539178 11.00000 -1.20000 AFIX 0 C13 1 0.440062 -0.050870 0.518212 11.00000 0.01656 0.02344 = 0.02757 0.00165 0.00305 0.00173 AFIX 43 H13A 2 0.432529 -0.195582 0.576128 11.00000 -1.20000 AFIX 0 HKLF 4 REM d1557 in Pna2(1) REM R1 = 0.0445 for 2455 Fo > 4sig(Fo) and 0.0594 for all 2931 data REM 156 parameters refined using 1 restraints END WGHT 0.0347 0.1578 REM Instructions for potential hydrogen bonds HTAB O3 O1_$1 EQIV $2 -x+1/2, y-1/2, z-1/2 HTAB C2 O3_$2 EQIV $3 -x+1/2, y+1/2, z-1/2 HTAB C3 Cl1_$3 REM Highest difference peak 0.282, deepest hole -0.279, 1-sigma level 0.056 Q1 1 0.2229 0.3978 0.4738 11.00000 0.05 0.28 Q2 1 0.1928 0.2828 0.4175 11.00000 0.05 0.23 Q3 1 0.2044 0.1133 0.6602 11.00000 0.05 0.22 Q4 1 0.3971 0.5441 0.1592 11.00000 0.05 0.22 Q5 1 0.1129 0.4760 0.4192 11.00000 0.05 0.22 Q6 1 0.1508 0.3421 0.6328 11.00000 0.05 0.22 Q7 1 0.3690 -0.2904 0.6652 11.00000 0.05 0.21 Q8 1 0.2619 0.2626 0.4553 11.00000 0.05 0.20 Q9 1 0.5510 0.0421 0.4471 11.00000 0.05 0.20 Q10 1 0.1909 0.3350 0.5555 11.00000 0.05 0.20 Q11 1 0.0886 0.8972 0.4390 11.00000 0.05 0.19 Q12 1 0.3831 0.0457 0.4415 11.00000 0.05 0.19 Q13 1 0.0331 0.8174 0.2162 11.00000 0.05 0.19 Q14 1 0.2725 0.0883 0.3929 11.00000 0.05 0.19 Q15 1 0.1134 0.7153 0.4212 11.00000 0.05 0.18 Q16 1 0.5316 -0.0371 0.3264 11.00000 0.05 0.18 Q17 1 0.1436 0.6027 0.4441 11.00000 0.05 0.18 Q18 1 0.3571 -0.0848 0.6075 11.00000 0.05 0.18 Q19 1 0.1912 0.3205 0.2055 11.00000 0.05 0.18 Q20 1 0.0663 0.8808 0.2769 11.00000 0.05 0.18 ; _shelx_res_checksum 46708 _shelx_hkl_file ; 0 -1 0 -1.20 0.60 0 2 0 287.47 11.20 0 -2 0 299.57 8.70 0 3 0 2.50 3.30 0 -3 0 0.00 1.50 0 4 0 -0.90 3.80 0 -4 0 2.50 2.00 0 -5 0 -2.00 2.60 0 5 0 -1.00 4.70 0 6 0 11.00 6.70 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