#------------------------------------------------------------------------------ #$Date: 2014-03-11 15:19:38 +0000 (Tue, 11 Mar 2014) $ #$Revision: 104812 $ #$URL: svn://www.crystallography.net/cod/cif/2/23/89/2238980.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_2238980 loop_ _publ_author_name 'Flores, Alex Fabiani Claro' 'de Vicenti, Juliano Rosa' 'Pizzuti, Lucas' 'Campos, Patrick Teixeira' _publ_section_title ; (S,Z)-3-Phenyl-2-[(1,1,1-trichloro-7-methoxy-2,7-dioxohept-3-en-4-yl)amino]propanoic acid monohydrate ; _journal_coeditor_code PK2509 _journal_issue 2 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o169 _journal_page_last o170 _journal_paper_doi 10.1107/S1600536814000154 _journal_volume 70 _journal_year 2014 _chemical_formula_iupac 'C17 H18 Cl3 N O5, H2 O' _chemical_formula_moiety 'C17 H18 Cl3 N O5, H2 O' _chemical_formula_sum 'C17 H20 Cl3 N O6' _chemical_formula_weight 440.69 _chemical_melting_point 393 _chemical_name_common 'enaminone propanoic acid' _chemical_name_systematic '(S,Z)-3-Phenyl-2-[(1,1,1-trichloro-7-methoxy-2,7-dioxohept-3-en-4-yl)amino]propanoic acid monohydrate' _space_group_crystal_system triclinic _space_group_IT_number 1 _space_group_name_Hall 'P 1' _space_group_name_H-M_alt 'P 1' _symmetry_space_group_name_Hall 'P 1' _symmetry_space_group_name_H-M 'P 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2013 _cell_angle_alpha 87.720(19) _cell_angle_beta 85.696(17) _cell_angle_gamma 85.649(17) _cell_formula_units_Z 1 _cell_length_a 5.6684(16) _cell_length_b 8.601(3) _cell_length_c 10.336(3) _cell_measurement_reflns_used 3866 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 25.513 _cell_measurement_theta_min 3.039 _cell_volume 500.8(3) _computing_cell_refinement 'SAINT (Bruker, 2009)' _computing_data_collection 'APEX2 (Bruker, 2009)' _computing_data_reduction 'SAINT (Bruker, 2009)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2006)' _computing_publication_material 'publCIF (Westrip, 2010)' _computing_structure_refinement 'SHELXL2013 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measurement_device_type 'Bruker APEXII CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'Graphite monochromator' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0243 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 13424 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.742 _diffrn_reflns_theta_min 2.376 _exptl_absorpt_coefficient_mu 0.491 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_correction_T_min 0.880962 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; (XPREP; Bruker, 2006) ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.461 _exptl_crystal_description blade _exptl_crystal_F_000 228 _exptl_crystal_size_max 0.980 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.120 _refine_diff_density_max 0.405 _refine_diff_density_min -0.323 _refine_ls_abs_structure_details ; Flack parameter determined using 1984 quotients [(I^+^)-(I^-^)]/[(I^+^)+(I^-^)] (Parsons et al., 2013) ; _refine_ls_abs_structure_Flack 0.04(2) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 256 _refine_ls_number_reflns 6020 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.041 _refine_ls_R_factor_all 0.0525 _refine_ls_R_factor_gt 0.0396 _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^)+(0.0502P)^2^+0.0376P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0966 _refine_ls_wR_factor_ref 0.1046 _reflns_number_gt 4784 _reflns_number_total 6020 _reflns_threshold_expression I>2\s(I) _iucr_refine_instructions_details ; TITL P1 in P1 CELL 0.71073 5.6684 8.6014 10.3356 87.720 85.696 85.649 ZERR 1.00 0.0016 0.0025 0.0029 0.019 0.017 0.017 LATT -1 SFAC C H N O CL UNIT 17 20 1 6 3 MERG 2 OMIT 0 0 1 OMIT 0 0 -1 EQIV $1 x+1, y, z EQIV $2 x, y+1, z EQIV $3 x-1, y, z HTAB C6 Cl1_$3 HTAB O33 O91_$1 HTAB N41 O21 HTAB O33 O21_$2 HTAB O92 O33 HTAB C3 Cl1 FMAP 2 PLAN 20 SIZE 0.12 0.30 0.98 ACTA HTAB BOND BOND $H CONF L.S. 15 TEMP 23.00 WGHT 0.050200 0.037600 FVAR 1.37521 O33 4 0.481328 1.014692 0.923041 11.00000 0.04941 0.04916 = 0.06726 0.00513 -0.00759 -0.00169 H33B 2 0.629280 0.976856 0.918597 11.00000 -1.50000 H41 2 0.147123 0.465123 0.794311 11.00000 -1.50000 H33A 2 0.457627 1.092416 0.886561 11.00000 -1.50000 H92 2 0.351532 0.868983 0.864461 11.00000 -1.50000 MOLE 1 CL1 5 0.750486 0.245723 0.420962 11.00000 0.07592 0.05600 = 0.05855 -0.00607 0.02406 0.00310 CL2 5 0.500840 0.015158 0.573383 11.00000 0.07414 0.04755 = 0.10500 -0.02876 0.03082 -0.02040 CL3 5 0.883578 0.163493 0.676166 11.00000 0.04130 0.09461 = 0.08376 -0.00315 -0.00584 0.01542 N41 3 0.105319 0.540260 0.746229 11.00000 0.04392 0.03503 = 0.03984 0.00119 -0.00052 0.00789 C1 1 0.639494 0.192416 0.578477 11.00000 0.03753 0.03795 = 0.05306 -0.00556 0.00564 -0.00238 C7 1 -0.143578 0.776085 0.364216 11.00000 0.04102 0.04348 = 0.04121 0.00278 -0.00238 0.00291 C9 1 0.062472 0.790054 0.862535 11.00000 0.04409 0.03974 = 0.04592 0.00564 -0.00476 0.00772 C3 1 0.369891 0.443372 0.573890 11.00000 0.04173 0.04028 = 0.03976 0.00169 0.00240 0.00134 AFIX 43 H3 2 0.428228 0.456851 0.487972 11.00000 -1.20000 AFIX 0 C10 1 -0.057587 0.652978 0.814498 11.00000 0.03750 0.03760 = 0.04436 -0.00346 -0.00515 0.00732 AFIX 13 H10 2 -0.170374 0.695639 0.752556 11.00000 -1.20000 AFIX 0 C5 1 0.123395 0.691214 0.539755 11.00000 0.04185 0.03376 = 0.04812 0.00426 -0.00389 -0.00200 AFIX 23 H5A 2 0.252646 0.713451 0.476442 11.00000 -1.20000 H5B 2 0.085429 0.782794 0.591284 11.00000 -1.20000 AFIX 0 C111 1 -0.051357 0.475824 1.019315 11.00000 0.04800 0.04768 = 0.03853 -0.00183 0.00783 -0.00002 C2 1 0.453953 0.312774 0.646039 11.00000 0.03491 0.03628 = 0.04404 -0.00491 -0.00122 0.00218 C6 1 -0.091738 0.656656 0.469954 11.00000 0.04776 0.04144 = 0.05317 0.00805 -0.01140 -0.00514 AFIX 23 H6A 2 -0.064463 0.554488 0.432806 11.00000 -1.20000 H6B 2 -0.228543 0.654259 0.532096 11.00000 -1.20000 AFIX 0 C11 1 -0.202295 0.571155 0.926378 11.00000 0.03870 0.05076 = 0.05160 -0.00281 0.00008 0.00317 AFIX 23 H11A 2 -0.300500 0.649616 0.974504 11.00000 -1.20000 H11B 2 -0.307062 0.503327 0.889680 11.00000 -1.20000 AFIX 0 C112 1 0.098124 0.545311 1.095900 11.00000 0.07544 0.05104 = 0.04889 0.00325 -0.00808 -0.00380 AFIX 43 H112 2 0.103955 0.653169 1.091568 11.00000 -1.20000 AFIX 0 C8 1 -0.427948 0.869885 0.218795 11.00000 0.06254 0.08088 = 0.04946 0.00644 -0.01487 0.01327 AFIX 33 H8A 2 -0.583308 0.850137 0.195274 11.00000 -1.50000 H8B 2 -0.316514 0.857346 0.144642 11.00000 -1.50000 H8C 2 -0.429946 0.974505 0.248147 11.00000 -1.50000 AFIX 0 C116 1 -0.061568 0.315618 1.030571 11.00000 0.08206 0.04953 = 0.05911 -0.00274 0.00210 -0.00724 AFIX 43 H116 2 -0.162656 0.266406 0.981274 11.00000 -1.20000 AFIX 0 C115 1 0.079331 0.227856 1.115636 11.00000 0.11545 0.04872 = 0.06875 0.00634 0.00593 0.00731 AFIX 43 H115 2 0.071809 0.120170 1.122176 11.00000 -1.20000 AFIX 0 C113 1 0.239082 0.456277 1.178876 11.00000 0.08389 0.08487 = 0.05224 0.00689 -0.01708 -0.00375 AFIX 43 H113 2 0.342207 0.503893 1.228021 11.00000 -1.20000 AFIX 0 C114 1 0.225903 0.296360 1.188369 11.00000 0.09253 0.07773 = 0.05541 0.01307 -0.00219 0.02603 AFIX 43 H114 2 0.318321 0.236283 1.244997 11.00000 -1.20000 AFIX 0 O72 4 -0.358686 0.760790 0.321842 11.00000 0.04825 0.06136 = 0.05110 0.00629 -0.01214 -0.00118 O92 4 0.291456 0.785204 0.836604 11.00000 0.04493 0.05007 = 0.07087 -0.00731 -0.00166 -0.00130 O91 4 -0.051661 0.894441 0.919006 11.00000 0.05397 0.04454 = 0.07778 -0.01662 -0.00497 0.01072 O71 4 -0.012416 0.869771 0.322005 11.00000 0.05378 0.06278 = 0.07381 0.02439 -0.00983 -0.00760 C4 1 0.200399 0.554748 0.626885 11.00000 0.03793 0.03306 = 0.03997 0.00135 -0.00373 -0.00248 O21 4 0.393439 0.280587 0.761262 11.00000 0.05244 0.04232 = 0.04319 0.00286 0.00383 0.01328 HKLF 4 REM P1 in P1 REM R1 = 0.0396 for 4784 Fo > 4sig(Fo) and 0.0525 for all 6020 data REM 256 parameters refined using 3 restraints END WGHT 0.0512 0.0342 REM Instructions for potential hydrogen bonds HTAB O33 O91_$1 HTAB N41 O21 HTAB O33 O21_$2 HTAB O92 O33 HTAB C3 Cl1 HTAB C6 Cl1_$3 REM Highest difference peak 0.405, deepest hole -0.323, 1-sigma level 0.041 Q1 1 0.8037 0.0852 0.6682 11.00000 0.05 0.41 Q2 1 0.4262 0.0555 0.5098 11.00000 0.05 0.34 Q3 1 0.6069 0.1011 0.5545 11.00000 0.05 0.21 Q4 1 0.6535 0.1818 0.4845 11.00000 0.05 0.20 Q5 1 0.1054 0.8912 0.9036 11.00000 0.05 0.20 Q6 1 0.8383 0.3177 0.4571 11.00000 0.05 0.19 Q7 1 0.9354 0.2145 0.5981 11.00000 0.05 0.19 Q8 1 0.8243 0.2585 0.4937 11.00000 0.05 0.19 Q9 1 0.4063 -0.0562 0.4989 11.00000 0.05 0.18 Q10 1 -0.0852 0.6137 0.8810 11.00000 0.05 0.17 Q11 1 0.3752 0.7292 0.7868 11.00000 0.05 0.17 Q12 1 0.0406 0.8984 0.3191 11.00000 0.05 0.17 Q13 1 0.1468 0.6354 0.5958 11.00000 0.05 0.17 Q14 1 -0.3094 0.9439 0.2026 11.00000 0.05 0.16 Q15 1 0.9755 0.2484 0.7627 11.00000 0.05 0.16 Q16 1 0.4756 0.3446 0.7516 11.00000 0.05 0.16 Q17 1 -0.4139 0.6790 0.2986 11.00000 0.05 0.16 Q18 1 -0.1166 0.7211 0.4199 11.00000 0.05 0.15 Q19 1 -0.0061 0.5051 1.1186 11.00000 0.05 0.15 Q20 1 0.1754 0.7565 0.8310 11.00000 0.05 0.15 ; _[local]_cod_data_source_file pk2509sup1.cif _[local]_cod_data_source_block I _cod_original_cell_volume 500.8(2) _cod_database_code 2238980 _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_min 0.645 _shelx_estimated_absorpt_t_max 0.943 _shelx_hkl_checksum 69725 _shelx_hkl_file ; -1 0 0 1028.44 26.84 -2 0 0 1005.20 26.98 3 0 0 119.50 4.57 -3 0 0 114.73 3.39 -3 0 0 115.59 4.90 -3 0 0 109.49 3.47 -4 0 0 87.74 4.72 4 0 0 82.30 3.12 4 0 0 90.59 3.02 4 0 0 91.62 4.31 -4 0 0 86.99 3.29 -4 0 0 89.26 3.11 -5 0 0 83.46 5.07 5 0 0 82.64 3.29 5 0 0 80.34 4.57 5 0 0 76.17 3.77 -6 0 0 10.96 1.49 6 0 0 13.45 1.61 6 0 0 11.94 2.42 -6 0 0 8.03 2.37 -7 0 0 11.02 3.02 7 0 0 12.42 1.87 -7 0 0 12.17 1.75 -8 0 0 5.28 1.59 -8 0 0 5.21 2.87 -7 1 0 37.05 4.82 -7 1 0 26.48 2.64 7 -1 0 33.81 2.98 6 -1 0 95.01 4.49 -6 1 0 102.31 6.42 -6 1 0 96.89 4.54 6 -1 0 96.93 5.73 -5 1 0 56.10 4.23 5 -1 0 51.14 4.05 -5 1 0 56.30 3.02 5 -1 0 54.25 2.91 4 -1 0 0.94 1.13 4 -1 0 2.13 0.97 4 -1 0 2.10 0.81 -4 1 0 1.83 1.16 -4 1 0 1.11 0.88 -4 1 0 1.02 0.81 -4 1 0 1.25 0.71 3 -1 0 50.39 2.25 -3 1 0 49.85 2.39 3 -1 0 53.45 3.09 -3 1 0 56.44 3.20 -2 1 0 158.67 4.69 -2 1 0 159.54 4.87 2 -1 0 145.98 4.60 2 -1 0 153.67 4.88 -2 1 0 159.04 5.49 -1 1 0 2789.56 68.72 1 -1 0 2785.89 68.65 -1 1 0 2832.12 68.84 -1 1 0 2761.16 66.78 0 -1 0 14.57 0.75 -1 -1 0 3823.17 96.73 1 1 0 3790.36 89.58 -1 -1 0 3771.99 89.08 -2 -1 0 3368.37 85.94 2 1 0 3311.50 76.66 3 1 0 818.13 20.21 3 1 0 773.30 18.96 -3 -1 0 767.50 22.22 -4 -1 0 254.28 9.50 4 1 0 262.76 8.32 4 1 0 266.13 7.47 5 1 0 61.81 3.75 5 1 0 67.38 3.13 -5 -1 0 64.76 4.41 6 1 0 1.96 0.85 -6 -1 0 0.85 0.78 -6 -1 0 2.17 1.64 -7 -1 0 8.57 2.81 -7 -1 0 6.51 1.27 -8 -1 0 2.34 2.46 -8 -1 0 10.72 1.66 7 -2 0 4.46 2.31 7 -2 0 6.20 1.87 -7 2 0 5.39 2.40 -7 2 0 5.07 1.62 -6 2 0 40.11 3.27 6 -2 0 37.09 4.16 -6 2 0 43.96 4.78 6 -2 0 39.66 3.17 5 -2 0 20.53 2.20 5 -2 0 23.66 3.15 -5 2 0 22.66 2.29 -5 2 0 26.02 3.42 4 -2 0 174.43 7.36 -4 2 0 168.95 7.54 4 -2 0 174.44 6.29 -4 2 0 182.89 6.40 4 -2 0 186.28 6.66 -4 2 0 185.13 6.35 -3 2 0 616.59 18.00 3 -2 0 618.61 16.52 -3 2 0 589.21 16.32 -3 2 0 609.63 16.43 3 -2 0 594.23 16.41 3 -2 0 586.31 17.19 2 -2 0 1280.61 31.71 2 -2 0 1256.50 32.10 2 -2 0 1269.79 32.12 -2 2 0 1249.26 31.64 -2 2 0 1254.94 32.15 1 -2 0 1942.09 46.26 -1 2 0 1847.84 46.14 -1 2 0 1844.59 47.23 -1 2 0 1930.09 47.41 1 -2 0 1903.41 47.13 0 2 0 996.40 25.67 0 -2 0 1011.26 24.71 0 -2 0 968.25 25.32 0 2 0 1069.20 25.11 0 -2 0 998.36 25.00 0 -2 0 992.54 25.68 -1 -2 0 1970.35 49.27 -1 -2 0 2085.82 45.87 -1 -2 0 1978.28 47.71 1 2 0 1958.31 49.11 -1 -2 0 2062.00 51.15 1 2 0 1868.38 48.79 2 2 0 655.53 15.62 -2 -2 0 655.90 15.58 -2 -2 0 676.49 18.40 -3 -2 0 736.44 21.24 3 2 0 749.22 17.75 3 2 0 758.50 18.71 4 2 0 242.90 6.58 4 2 0 252.18 7.42 -4 -2 0 232.36 8.90 -5 -2 0 127.25 6.38 -6 -2 0 13.18 2.78 -7 -2 0 48.91 5.14 -8 -2 0 3.60 2.42 -7 3 0 5.40 2.55 7 -3 0 5.65 2.11 7 -3 0 7.40 2.77 -7 3 0 7.70 2.10 -6 3 0 73.52 5.75 6 -3 0 86.91 4.79 -6 3 0 77.74 4.67 6 -3 0 78.30 6.06 -5 3 0 50.27 3.42 5 -3 0 47.13 3.36 -5 3 0 60.92 4.96 5 -3 0 53.12 4.70 -5 3 0 50.87 3.49 4 -3 0 280.14 9.27 4 -3 0 277.91 9.61 -4 3 0 264.55 9.33 -4 3 0 285.03 10.61 4 -3 0 253.55 10.14 -4 3 0 298.14 9.42 3 -3 0 579.95 16.41 -3 3 0 555.96 16.48 3 -3 0 585.50 17.21 -3 3 0 592.49 16.50 3 -3 0 599.80 16.71 2 -3 0 238.67 7.96 -2 3 0 250.27 7.77 2 -3 0 227.76 7.49 -2 3 0 246.12 7.68 2 -3 0 221.53 8.01 -2 3 0 234.10 7.90 -1 3 0 1167.27 30.55 -1 3 0 1198.44 30.25 1 -3 0 1173.10 30.11 -1 3 0 1163.97 30.81 1 -3 0 1183.27 30.42 1 -3 0 1234.85 30.91 0 -3 0 934.72 24.01 0 -3 0 950.42 22.99 0 3 0 898.94 23.97 0 -3 0 889.25 23.43 0 3 0 875.72 23.55 0 -3 0 921.90 23.45 0 3 0 885.40 23.54 0 3 0 966.36 23.56 1 3 0 3047.57 74.01 -1 -3 0 2939.83 71.15 -1 -3 0 3026.62 71.88 -1 -3 0 2866.79 74.10 1 3 0 3061.77 71.95 -2 -3 0 356.75 10.03 -2 -3 0 381.84 11.32 -2 -3 0 397.85 10.45 2 3 0 377.71 10.25 -2 -3 0 397.47 10.06 -3 -3 0 88.78 4.16 -4 -3 0 196.12 7.80 -5 -3 0 150.77 7.10 -6 -3 0 1.61 1.47 -7 -3 0 4.35 2.37 -7 4 0 5.83 2.83 -7 4 0 7.37 2.31 7 -4 0 3.07 2.53 7 -4 0 6.19 2.31 -6 4 0 9.61 2.82 6 -4 0 7.20 2.07 6 -4 0 14.03 3.31 -6 4 0 8.69 2.09 5 -4 0 4.57 1.68 -5 4 0 3.64 1.90 -5 4 0 3.52 1.48 5 -4 0 5.41 2.26 -5 4 0 3.85 1.56 5 -4 0 3.93 1.69 -4 4 0 173.92 6.92 4 -4 0 166.01 7.73 4 -4 0 160.59 6.71 -4 4 0 155.89 6.96 -4 4 0 163.80 7.60 4 -4 0 167.63 7.22 -3 4 0 623.16 18.14 3 -4 0 609.02 18.46 -3 4 0 636.16 17.91 3 -4 0 602.37 17.78 3 -4 0 620.83 18.18 -2 4 0 107.63 4.81 2 -4 0 109.08 4.59 2 -4 0 107.93 5.04 -2 4 0 101.14 4.55 2 -4 0 99.96 4.86 -2 4 0 106.55 4.99 1 -4 0 477.30 14.15 1 -4 0 478.10 13.86 -1 4 0 486.77 14.30 -1 4 0 495.75 13.90 1 -4 0 474.31 14.16 1 -4 0 488.59 13.84 -1 4 0 483.94 14.18 0 4 0 1401.45 37.40 0 4 0 1441.15 38.00 0 -4 0 1457.87 37.33 0 4 0 1471.93 37.51 0 -4 0 1488.71 36.45 0 4 0 1539.81 37.28 0 -4 0 1493.01 37.22 0 -4 0 1456.51 38.05 1 4 0 1927.53 47.32 -1 -4 0 1911.16 47.54 -1 -4 0 1927.84 47.18 -1 -4 0 1924.05 46.06 -1 -4 0 1910.79 48.59 1 4 0 1859.12 48.48 -2 -4 0 309.85 9.15 -2 -4 0 327.98 9.24 2 4 0 336.70 9.58 2 4 0 328.04 9.50 -2 -4 0 318.48 9.57 -2 -4 0 309.37 9.17 -3 -4 0 388.14 10.17 3 4 0 380.78 10.49 -3 -4 0 398.12 12.36 -3 -4 0 408.48 11.14 3 4 0 421.60 11.01 -3 -4 0 361.93 10.60 -4 -4 0 152.37 6.74 -4 -4 0 163.36 5.21 -5 -4 0 66.32 4.46 -6 -4 0 15.72 2.89 -7 -4 0 0.85 1.87 7 -5 0 19.59 4.09 7 -5 0 22.08 3.63 -7 5 0 23.79 4.59 -7 5 0 16.78 3.29 6 -5 0 12.62 3.36 -6 5 0 13.91 3.35 6 -5 0 11.02 2.45 -6 5 0 8.60 2.47 -5 5 0 203.19 8.42 -5 5 0 189.07 9.41 5 -5 0 183.20 8.10 -5 5 0 195.41 8.69 5 -5 0 185.85 9.50 5 -5 0 189.34 8.62 -4 5 0 19.84 2.83 4 -5 0 18.52 2.82 -4 5 0 14.89 2.40 -4 5 0 17.30 2.76 4 -5 0 19.98 2.71 4 -5 0 13.99 2.77 3 -5 0 31.74 2.95 3 -5 0 27.28 3.39 3 -5 0 25.14 3.04 -3 5 0 30.87 2.98 -3 5 0 37.99 3.48 -2 5 0 65.64 4.17 -2 5 0 73.04 3.93 2 -5 0 70.09 3.92 2 -5 0 61.16 4.05 -2 5 0 65.52 3.97 2 -5 0 69.05 4.18 1 -5 0 276.83 9.31 1 -5 0 284.72 9.53 -1 5 0 287.12 9.90 -1 5 0 269.46 9.82 1 -5 0 278.90 9.90 1 -5 0 302.55 9.96 -1 5 0 302.50 9.50 0 5 0 161.62 5.89 0 -5 0 166.59 5.91 0 -5 0 154.55 6.41 0 -5 0 154.70 5.74 0 5 0 168.67 6.63 0 5 0 156.94 5.84 0 -5 0 156.78 6.42 0 5 0 166.69 6.54 -1 -5 0 410.38 11.14 -1 -5 0 417.32 12.39 1 5 0 402.45 12.63 -1 -5 0 412.09 11.54 1 5 0 410.71 12.53 -1 -5 0 409.70 12.59 2 5 0 145.63 5.63 -2 -5 0 139.78 5.59 2 5 0 139.10 5.60 -2 -5 0 139.17 5.34 -3 -5 0 181.41 6.51 -3 -5 0 186.56 5.88 3 5 0 175.60 6.38 3 5 0 179.98 6.49 4 5 0 384.23 11.01 -4 -5 0 349.95 12.35 -4 -5 0 366.20 11.02 -5 -5 0 45.10 3.98 5 5 0 47.06 2.68 -5 -5 0 44.54 2.66 -6 -5 0 10.28 2.62 -7 -5 0 1.14 1.88 6 -6 0 3.03 1.90 6 -6 0 3.92 2.57 -6 6 0 3.99 2.54 -6 6 0 6.30 2.32 -5 6 0 103.65 6.94 -5 6 0 119.18 6.62 5 -6 0 119.96 7.52 -5 6 0 105.05 6.58 5 -6 0 115.94 6.53 5 -6 0 109.20 6.71 4 -6 0 47.11 5.00 -4 6 0 51.93 4.56 -4 6 0 51.26 4.32 4 -6 0 56.64 4.79 4 -6 0 46.05 4.23 -3 6 0 47.41 3.90 3 -6 0 39.51 3.59 3 -6 0 28.88 3.48 3 -6 0 40.68 4.24 -3 6 0 37.65 3.85 -2 6 0 1082.53 30.87 -2 6 0 1149.69 30.65 -2 6 0 1090.11 31.01 2 -6 0 1091.70 30.83 2 -6 0 1130.02 30.52 2 -6 0 1098.91 30.44 -1 6 0 21.54 2.82 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8.03 -2 7 0 202.22 8.27 -2 7 0 195.39 8.69 2 -7 0 177.21 8.34 -2 7 0 196.26 8.97 -2 7 0 203.78 8.36 2 -7 0 190.49 8.83 -1 7 0 235.28 9.87 1 -7 0 249.15 9.06 -1 7 0 231.55 9.01 1 -7 0 233.84 9.79 -1 7 0 236.71 9.07 -1 7 0 242.05 10.07 1 -7 0 248.37 9.29 1 -7 0 239.94 9.74 0 -7 0 98.80 4.82 0 7 0 102.54 5.84 0 7 0 101.57 5.73 0 -7 0 110.01 5.82 0 -7 0 107.30 5.00 0 -7 0 100.72 5.64 1 7 0 65.71 4.39 -1 -7 0 68.12 4.48 -1 -7 0 61.54 3.37 -1 -7 0 55.83 4.01 1 7 0 60.74 4.27 -2 -7 0 281.18 10.58 -2 -7 0 280.30 10.05 2 7 0 306.90 10.64 2 7 0 281.03 10.55 3 7 0 5.65 1.63 3 7 0 5.71 1.70 -3 -7 0 9.38 1.76 -3 -7 0 10.83 2.15 4 7 0 55.80 3.88 -4 -7 0 53.51 3.84 5 7 0 9.17 2.12 -5 -7 0 14.84 2.32 -6 -7 0 19.63 2.46 6 7 0 19.21 2.86 -5 8 0 -0.51 1.75 -5 8 0 3.41 2.09 5 -8 0 1.15 1.85 5 -8 0 2.81 2.25 5 -8 0 -3.44 2.14 -5 8 0 -0.69 1.81 -5 8 0 1.54 1.82 -4 8 0 20.50 3.81 -4 8 0 27.49 3.83 4 -8 0 24.56 4.06 -4 8 0 26.29 3.94 4 -8 0 26.11 4.36 4 -8 0 20.26 3.51 3 -8 0 9.19 2.34 -3 8 0 12.56 2.84 -3 8 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12.48 3.20 2 2 -13 12.77 3.34 1 2 -13 3.38 2.12 -1 -2 13 5.07 2.39 -1 -2 13 6.90 2.58 1 2 -13 10.61 3.37 -1 -2 13 3.04 2.11 0 2 -13 0.77 2.34 0 -2 13 -1.55 1.55 0 -2 13 1.57 1.74 0 2 -13 1.87 1.92 -1 2 -13 1.39 1.94 1 -2 13 0.49 1.70 1 -2 13 0.49 2.02 1 -2 13 -1.54 1.55 -1 2 -13 1.21 2.25 2 -2 13 2.77 2.08 -2 2 -13 1.57 2.00 2 -2 13 1.84 2.02 2 -2 13 3.59 2.57 3 -2 13 4.00 2.89 3 -2 13 1.09 2.12 -3 2 -13 1.72 1.85 3 -2 13 1.17 2.15 3 -2 13 0.29 2.23 3 1 -13 12.49 3.41 -3 -1 13 9.79 2.97 -3 -1 13 10.07 3.06 2 1 -13 6.79 2.53 -2 -1 13 9.09 2.81 -2 -1 13 8.83 2.95 2 1 -13 7.11 2.81 -1 -1 13 2.54 2.11 -1 -1 13 0.86 1.83 -1 -1 13 3.10 2.16 1 1 -13 3.60 2.33 1 1 -13 0.75 1.80 0 1 -13 3.77 2.15 0 -1 13 7.48 2.60 0 -1 13 1.91 2.02 0 1 -13 7.83 2.89 1 -1 13 -0.76 1.82 -1 1 -13 1.07 1.77 1 -1 13 -0.95 1.45 1 -1 13 -0.23 1.73 2 -1 13 4.01 2.47 -2 1 -13 4.61 2.35 2 -1 13 5.93 2.54 2 -1 13 8.65 2.89 3 -1 13 2.40 2.13 3 -1 13 3.41 2.58 -3 1 -13 0.83 1.85 3 -1 13 4.22 2.36 3 -1 13 2.74 2.37 4 -1 13 0.58 2.05 4 -1 13 -1.86 1.90 4 -1 13 3.35 2.51 4 -1 13 0.07 2.37 -4 1 -13 -1.12 1.79 3 0 -13 4.75 2.47 -3 0 13 4.56 2.40 -3 0 13 4.10 2.19 3 0 -13 6.90 2.89 -2 0 13 6.23 2.54 -2 0 13 2.05 2.01 2 0 -13 2.54 2.16 2 0 -13 1.33 2.13 -1 0 13 0.88 1.89 1 0 -13 1.71 2.01 -1 0 13 1.16 1.88 -1 0 13 0.07 1.70 1 0 -13 0.07 1.63 0 0 13 2.38 1.94 0 0 -13 1.35 2.34 0 0 13 2.99 2.10 0 0 -13 -0.28 1.67 1 0 13 4.30 2.07 1 0 13 2.10 1.93 -1 0 -13 0.80 1.63 2 0 13 -0.40 1.54 2 0 13 -0.28 1.87 -2 0 -13 -1.45 1.63 2 0 13 0.83 1.74 3 0 13 0.69 1.90 3 0 13 2.59 2.27 -3 0 -13 3.62 2.23 3 0 13 1.66 2.19 3 0 13 2.51 2.26 4 0 13 3.13 2.23 4 0 13 2.28 2.57 4 0 13 5.56 2.75 -4 0 -13 1.52 2.17 4 0 13 3.95 2.71 -3 1 13 -1.83 1.78 3 -1 -13 2.11 2.35 3 -1 -13 -0.35 1.85 -3 1 13 3.15 2.19 -2 1 13 7.60 2.96 -2 1 13 5.37 2.31 2 -1 -13 4.81 2.29 2 -1 -13 4.71 2.63 -2 1 13 5.15 2.49 1 -1 -13 7.22 2.69 -1 1 13 4.38 2.14 -1 1 13 5.54 2.34 1 -1 -13 10.84 3.01 -1 1 13 7.81 2.73 0 1 13 31.98 4.76 0 -1 -13 39.69 4.93 0 1 13 34.87 4.44 0 -1 -13 32.82 4.67 1 1 13 -0.91 1.52 1 1 13 -0.76 1.46 -1 -1 -13 0.61 1.68 2 1 13 5.70 2.52 -2 -1 -13 4.40 2.14 2 1 13 8.45 2.68 2 1 13 1.50 1.80 3 1 13 1.91 1.91 3 1 13 1.79 2.07 -3 -1 -13 0.41 1.81 3 1 13 0.70 1.82 3 1 13 -1.77 1.99 4 1 13 4.24 2.54 4 1 13 2.71 2.48 4 1 13 4.53 2.63 -4 -1 -13 6.21 2.79 -4 -1 -13 3.81 2.54 -3 2 13 8.29 2.76 3 -2 -13 4.62 2.59 3 -2 -13 3.03 2.45 -3 2 13 6.39 2.69 -2 2 13 13.93 3.52 -2 2 13 17.94 3.47 -2 2 13 10.37 3.13 2 -2 -13 14.52 3.45 2 -2 -13 14.46 3.60 1 -2 -13 21.89 4.09 -1 2 13 22.33 3.87 1 -2 -13 20.50 4.00 -1 2 13 14.72 3.49 0 -2 -13 3.23 2.60 0 2 13 5.45 2.49 0 -2 -13 1.51 1.79 0 2 13 10.51 2.76 1 2 13 4.05 2.16 1 2 13 0.15 1.76 -1 -2 -13 6.26 2.30 2 2 13 12.73 3.20 2 2 13 12.24 3.35 2 2 13 16.15 3.60 -2 -2 -13 8.50 2.75 3 2 13 3.32 2.46 -3 -2 -13 4.49 2.31 3 2 13 4.94 2.42 3 2 13 1.01 2.04 4 2 13 6.61 2.98 -4 -2 -13 4.66 2.56 4 2 13 4.27 2.62 -4 -2 -13 3.54 2.51 4 2 13 6.78 3.09 -2 3 13 5.86 2.75 2 -3 -13 1.46 2.47 -2 3 13 3.09 2.31 -2 3 13 5.56 2.70 2 -3 -13 3.58 2.38 1 -3 -13 6.31 2.62 1 -3 -13 0.89 2.30 -1 3 13 4.78 2.52 -1 3 13 9.63 3.08 0 3 13 3.94 2.35 0 3 13 1.28 1.89 0 -3 -13 2.40 2.33 0 -3 -13 5.14 2.46 1 3 13 6.15 2.56 1 3 13 2.17 2.15 -1 -3 -13 9.41 2.91 2 3 13 4.83 2.33 -2 -3 -13 6.83 2.58 2 3 13 5.39 2.33 2 3 13 6.13 2.91 3 3 13 2.15 2.20 3 3 13 -0.36 2.49 -3 -3 -13 1.64 2.18 3 3 13 0.17 1.83 -4 -3 -13 -0.82 1.79 -4 -3 -13 2.43 2.27 4 3 13 -1.11 2.07 4 3 13 4.06 3.03 4 3 13 2.00 2.24 -2 4 13 -1.04 2.01 2 -4 -13 2.28 2.27 2 -4 -13 -1.65 2.05 -2 4 13 -1.23 1.75 -1 4 13 4.95 2.32 1 -4 -13 2.71 2.53 1 -4 -13 3.10 2.30 -1 4 13 4.42 2.73 0 4 13 8.56 2.99 0 -4 -13 9.99 2.94 0 4 13 4.90 2.36 1 4 13 3.34 2.35 1 4 13 0.90 1.72 -1 -4 -13 1.91 2.24 2 4 13 3.36 2.23 2 4 13 0.68 2.06 -2 -4 -13 1.06 1.97 3 4 13 0.10 1.65 -3 -4 -13 -0.88 1.94 3 4 13 0.68 2.01 1 -5 -13 4.36 2.81 -1 5 13 5.03 2.67 1 -5 -13 3.68 2.49 -1 5 13 4.71 2.66 0 5 13 6.94 2.80 0 5 13 7.55 3.08 0 -5 -13 2.77 2.36 -1 -5 -13 -0.74 1.78 1 5 13 5.27 2.77 1 5 13 1.35 2.10 2 5 13 4.41 2.63 -2 -5 -13 4.57 2.39 2 5 13 7.99 2.96 -3 -5 -13 -1.69 1.79 3 5 13 1.13 2.37 3 5 13 1.22 2.22 0 6 13 1.26 2.17 0 6 13 -0.35 2.17 0 -6 -13 0.31 2.23 -1 -6 -13 1.50 2.11 1 6 13 0.80 2.18 1 6 13 -1.99 1.86 2 6 13 1.51 2.36 -2 -6 -13 2.93 2.40 1 3 -14 3.54 2.65 0 3 -14 -0.45 2.49 0 -3 14 3.76 2.41 0 3 -14 2.61 2.26 0 -3 14 1.89 2.13 1 -3 14 4.37 2.66 -1 3 -14 1.91 2.36 1 -3 14 4.65 2.74 1 -3 14 2.40 2.50 1 2 -14 0.75 2.28 -1 -2 14 -0.56 1.83 1 2 -14 2.90 2.33 0 2 -14 1.18 1.96 0 2 -14 7.54 3.15 0 -2 14 7.39 2.81 0 -2 14 9.47 3.06 -1 2 -14 0.39 1.92 1 -2 14 2.28 2.22 1 -2 14 3.64 2.74 1 -2 14 3.05 2.45 2 -2 14 5.10 2.59 -2 2 -14 -0.99 1.83 2 -2 14 1.15 2.25 2 -2 14 -0.80 2.47 2 1 -14 2.84 2.51 -2 -1 14 4.00 2.61 -1 -1 14 2.98 2.04 -1 -1 14 1.94 2.50 1 1 -14 0.02 1.61 1 1 -14 3.54 2.81 0 1 -14 5.07 2.40 0 -1 14 1.24 1.90 0 1 -14 2.51 2.38 0 -1 14 -0.99 1.92 1 -1 14 -0.70 1.76 1 -1 14 -0.48 1.86 -1 1 -14 2.44 2.16 2 -1 14 1.94 2.14 -2 1 -14 -0.74 1.85 2 -1 14 -0.22 1.89 2 -1 14 3.19 2.40 3 -1 14 3.22 2.65 -3 1 -14 2.10 2.31 -2 0 14 6.52 2.69 -2 0 14 8.66 3.18 2 0 -14 11.61 3.54 2 0 -14 8.80 3.02 1 0 -14 18.20 3.90 -1 0 14 11.77 3.33 -1 0 14 18.92 3.73 1 0 -14 17.03 3.97 0 0 -14 -1.01 2.28 0 0 14 -1.52 1.82 0 0 -14 0.88 1.80 0 0 14 3.08 2.18 1 0 14 1.03 2.14 1 0 14 2.65 2.23 -1 0 -14 3.31 2.28 -2 0 -14 -0.31 1.84 2 0 14 1.07 1.99 2 0 14 -1.99 1.98 -3 0 -14 5.34 2.69 3 0 14 1.30 2.15 3 0 14 4.65 2.90 3 0 14 5.70 3.03 3 0 14 2.58 2.56 2 -1 -14 9.89 3.32 -2 1 14 11.95 3.24 2 -1 -14 6.70 2.70 -2 1 14 11.40 3.38 1 -1 -14 0.15 2.43 -1 1 14 -0.62 1.81 1 -1 -14 0.69 1.95 -1 1 14 1.67 2.28 0 -1 -14 5.14 2.41 0 1 14 6.66 2.71 0 1 14 7.32 2.93 0 -1 -14 5.40 2.77 1 1 14 1.20 1.90 -1 -1 -14 0.17 1.78 1 1 14 1.42 2.12 -2 -1 -14 -0.20 1.87 2 1 14 0.65 2.21 2 1 14 -0.55 1.90 3 1 14 1.79 2.46 3 1 14 0.68 2.69 3 1 14 2.93 2.46 -3 -1 -14 -1.75 1.70 1 -2 -14 5.76 2.69 -1 2 14 4.33 2.43 1 -2 -14 3.19 2.59 -1 2 14 2.73 2.60 0 -2 -14 -1.02 1.71 0 2 14 -2.46 1.88 0 2 14 2.41 2.21 -1 -2 -14 0.96 2.07 1 2 14 0.87 1.89 1 2 14 1.34 2.26 2 2 14 2.47 2.20 -2 -2 -14 1.81 2.19 2 2 14 -0.72 2.04 3 2 14 1.88 2.20 3 2 14 0.65 2.72 -3 -2 -14 0.18 2.12 -1 3 14 4.34 2.60 1 -3 -14 -1.84 2.23 1 -3 -14 2.43 2.46 -1 3 14 1.78 2.66 0 3 14 2.58 2.33 0 3 14 3.24 2.38 0 -3 -14 2.89 2.38 1 3 14 5.35 2.59 1 3 14 3.29 2.23 -1 -3 -14 6.39 2.61 2 3 14 2.47 2.33 2 3 14 6.23 2.87 -2 -3 -14 3.67 2.50 0 4 14 -0.40 2.34 0 -4 -14 4.53 2.68 0 4 14 2.15 2.21 1 4 14 -1.09 1.55 1 4 14 1.30 2.20 -1 -4 -14 0.19 1.97 -2 -4 -14 2.08 2.24 2 4 14 0.99 2.16 0 0 0 0.00 0.00 ; _shelx_res_checksum 59829 _shelx_res_file ; TITL P1 in P1 CELL 0.71073 5.6684 8.6014 10.3356 87.720 85.696 85.649 ZERR 1.00 0.0016 0.0025 0.0029 0.019 0.017 0.017 LATT -1 SFAC C H N O CL UNIT 17 20 1 6 3 MERG 2 OMIT 0 0 1 OMIT 0 0 -1 EQIV $1 x+1, y, z EQIV $2 x, y+1, z EQIV $3 x-1, y, z HTAB C6 Cl1_$3 HTAB O33 O91_$1 HTAB N41 O21 HTAB O33 O21_$2 HTAB O92 O33 HTAB C3 Cl1 FMAP 2 PLAN 20 SIZE 0.12 0.30 0.98 ACTA HTAB BOND BOND $H CONF L.S. 15 TEMP 23.00 WGHT 0.050200 0.037600 FVAR 1.37521 O33 4 0.481328 1.014692 0.923041 11.00000 0.04941 0.04916 = 0.06726 0.00513 -0.00759 -0.00169 H33B 2 0.629280 0.976856 0.918597 11.00000 -1.50000 H41 2 0.147123 0.465123 0.794311 11.00000 -1.50000 H33A 2 0.457627 1.092416 0.886561 11.00000 -1.50000 H92 2 0.351532 0.868983 0.864461 11.00000 -1.50000 MOLE 1 CL1 5 0.750486 0.245723 0.420962 11.00000 0.07592 0.05600 = 0.05855 -0.00607 0.02406 0.00310 CL2 5 0.500840 0.015158 0.573383 11.00000 0.07414 0.04755 = 0.10500 -0.02876 0.03082 -0.02040 CL3 5 0.883578 0.163493 0.676166 11.00000 0.04130 0.09461 = 0.08376 -0.00315 -0.00584 0.01542 N41 3 0.105319 0.540260 0.746229 11.00000 0.04392 0.03503 = 0.03984 0.00119 -0.00052 0.00789 C1 1 0.639494 0.192416 0.578477 11.00000 0.03753 0.03795 = 0.05306 -0.00556 0.00564 -0.00238 C7 1 -0.143578 0.776085 0.364216 11.00000 0.04102 0.04348 = 0.04121 0.00278 -0.00238 0.00291 C9 1 0.062472 0.790054 0.862535 11.00000 0.04409 0.03974 = 0.04592 0.00564 -0.00476 0.00772 C3 1 0.369891 0.443372 0.573890 11.00000 0.04173 0.04028 = 0.03976 0.00169 0.00240 0.00134 AFIX 43 H3 2 0.428228 0.456851 0.487972 11.00000 -1.20000 AFIX 0 C10 1 -0.057587 0.652978 0.814498 11.00000 0.03750 0.03760 = 0.04436 -0.00346 -0.00515 0.00732 AFIX 13 H10 2 -0.170374 0.695639 0.752556 11.00000 -1.20000 AFIX 0 C5 1 0.123395 0.691214 0.539755 11.00000 0.04185 0.03376 = 0.04812 0.00426 -0.00389 -0.00200 AFIX 23 H5A 2 0.252646 0.713451 0.476442 11.00000 -1.20000 H5B 2 0.085429 0.782794 0.591284 11.00000 -1.20000 AFIX 0 C111 1 -0.051357 0.475824 1.019315 11.00000 0.04800 0.04768 = 0.03853 -0.00183 0.00783 -0.00002 C2 1 0.453953 0.312774 0.646039 11.00000 0.03491 0.03628 = 0.04404 -0.00491 -0.00122 0.00218 C6 1 -0.091738 0.656656 0.469954 11.00000 0.04776 0.04144 = 0.05317 0.00805 -0.01140 -0.00514 AFIX 23 H6A 2 -0.064463 0.554488 0.432806 11.00000 -1.20000 H6B 2 -0.228543 0.654259 0.532096 11.00000 -1.20000 AFIX 0 C11 1 -0.202295 0.571155 0.926378 11.00000 0.03870 0.05076 = 0.05160 -0.00281 0.00008 0.00317 AFIX 23 H11A 2 -0.300500 0.649616 0.974504 11.00000 -1.20000 H11B 2 -0.307062 0.503327 0.889680 11.00000 -1.20000 AFIX 0 C112 1 0.098124 0.545311 1.095900 11.00000 0.07544 0.05104 = 0.04889 0.00325 -0.00808 -0.00380 AFIX 43 H112 2 0.103955 0.653169 1.091568 11.00000 -1.20000 AFIX 0 C8 1 -0.427948 0.869885 0.218795 11.00000 0.06254 0.08088 = 0.04946 0.00644 -0.01487 0.01327 AFIX 33 H8A 2 -0.583308 0.850137 0.195274 11.00000 -1.50000 H8B 2 -0.316514 0.857346 0.144642 11.00000 -1.50000 H8C 2 -0.429946 0.974505 0.248147 11.00000 -1.50000 AFIX 0 C116 1 -0.061568 0.315618 1.030571 11.00000 0.08206 0.04953 = 0.05911 -0.00274 0.00210 -0.00724 AFIX 43 H116 2 -0.162656 0.266406 0.981274 11.00000 -1.20000 AFIX 0 C115 1 0.079331 0.227856 1.115636 11.00000 0.11545 0.04872 = 0.06875 0.00634 0.00593 0.00731 AFIX 43 H115 2 0.071809 0.120170 1.122176 11.00000 -1.20000 AFIX 0 C113 1 0.239082 0.456277 1.178876 11.00000 0.08389 0.08487 = 0.05224 0.00689 -0.01708 -0.00375 AFIX 43 H113 2 0.342207 0.503893 1.228021 11.00000 -1.20000 AFIX 0 C114 1 0.225903 0.296360 1.188369 11.00000 0.09253 0.07773 = 0.05541 0.01307 -0.00219 0.02603 AFIX 43 H114 2 0.318321 0.236283 1.244997 11.00000 -1.20000 AFIX 0 O72 4 -0.358686 0.760790 0.321842 11.00000 0.04825 0.06136 = 0.05110 0.00629 -0.01214 -0.00118 O92 4 0.291456 0.785204 0.836604 11.00000 0.04493 0.05007 = 0.07087 -0.00731 -0.00166 -0.00130 O91 4 -0.051661 0.894441 0.919006 11.00000 0.05397 0.04454 = 0.07778 -0.01662 -0.00497 0.01072 O71 4 -0.012416 0.869771 0.322005 11.00000 0.05378 0.06278 = 0.07381 0.02439 -0.00983 -0.00760 C4 1 0.200399 0.554748 0.626885 11.00000 0.03793 0.03306 = 0.03997 0.00135 -0.00373 -0.00248 O21 4 0.393439 0.280587 0.761262 11.00000 0.05244 0.04232 = 0.04319 0.00286 0.00383 0.01328 HKLF 4 REM P1 in P1 REM R1 = 0.0396 for 4784 Fo > 4sig(Fo) and 0.0525 for all 6020 data REM 256 parameters refined using 3 restraints END WGHT 0.0512 0.0342 REM Instructions for potential hydrogen bonds HTAB O33 O91_$1 HTAB N41 O21 HTAB O33 O21_$2 HTAB O92 O33 HTAB C3 Cl1 HTAB C6 Cl1_$3 REM Highest difference peak 0.405, deepest hole -0.323, 1-sigma level 0.041 Q1 1 0.8037 0.0852 0.6682 11.00000 0.05 0.41 Q2 1 0.4262 0.0555 0.5098 11.00000 0.05 0.34 Q3 1 0.6069 0.1011 0.5545 11.00000 0.05 0.21 Q4 1 0.6535 0.1818 0.4845 11.00000 0.05 0.20 Q5 1 0.1054 0.8912 0.9036 11.00000 0.05 0.20 Q6 1 0.8383 0.3177 0.4571 11.00000 0.05 0.19 Q7 1 0.9354 0.2145 0.5981 11.00000 0.05 0.19 Q8 1 0.8243 0.2585 0.4937 11.00000 0.05 0.19 Q9 1 0.4063 -0.0562 0.4989 11.00000 0.05 0.18 Q10 1 -0.0852 0.6137 0.8810 11.00000 0.05 0.17 Q11 1 0.3752 0.7292 0.7868 11.00000 0.05 0.17 Q12 1 0.0406 0.8984 0.3191 11.00000 0.05 0.17 Q13 1 0.1468 0.6354 0.5958 11.00000 0.05 0.17 Q14 1 -0.3094 0.9439 0.2026 11.00000 0.05 0.16 Q15 1 0.9755 0.2484 0.7627 11.00000 0.05 0.16 Q16 1 0.4756 0.3446 0.7516 11.00000 0.05 0.16 Q17 1 -0.4139 0.6790 0.2986 11.00000 0.05 0.16 Q18 1 -0.1166 0.7211 0.4199 11.00000 0.05 0.15 Q19 1 -0.0061 0.5051 1.1186 11.00000 0.05 0.15 Q20 1 0.1754 0.7565 0.8310 11.00000 0.05 0.15 ; _shelxl_version_number .2013 loop_ _space_group_symop_operation_xyz 'x, y, z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy O O33 0.4813(5) 1.0147(3) 0.9230(3) 0.0554(6) Uani d 1 H H33B 0.629(11) 0.977(6) 0.919(5) 0.083 Uiso d 1 H H41 0.147(9) 0.465(6) 0.794(5) 0.083 Uiso d 1 H H33A 0.458(10) 1.092(7) 0.887(5) 0.083 Uiso d 1 H H92 0.352(9) 0.869(6) 0.864(5) 0.083 Uiso d 1 Cl Cl1 0.75049(16) 0.24572(10) 0.42096(9) 0.0652(3) Uani d 1 Cl Cl2 0.50084(18) 0.01516(11) 0.57338(11) 0.0759(3) Uani d 1 Cl Cl3 0.88358(15) 0.16349(14) 0.67617(11) 0.0742(3) Uani d 1 N N41 0.1053(4) 0.5403(3) 0.7462(2) 0.0403(5) Uani d 1 C C1 0.6395(5) 0.1924(3) 0.5785(3) 0.0432(6) Uani d 1 C C7 -0.1436(5) 0.7761(4) 0.3642(3) 0.0424(6) Uani d 1 C C9 0.0625(5) 0.7901(3) 0.8625(3) 0.0439(6) Uani d 1 C C3 0.3699(5) 0.4434(3) 0.5739(3) 0.0412(6) Uani d 1 H H3 0.4282 0.4569 0.4880 0.049 Uiso calc 1 C C10 -0.0576(5) 0.6530(3) 0.8145(3) 0.0402(6) Uani d 1 H H10 -0.1704 0.6956 0.7526 0.048 Uiso calc 1 C C5 0.1234(5) 0.6912(3) 0.5398(3) 0.0414(6) Uani d 1 H H5A 0.2526 0.7135 0.4764 0.050 Uiso calc 1 H H5B 0.0854 0.7828 0.5913 0.050 Uiso calc 1 C C111 -0.0514(5) 0.4758(4) 1.0193(3) 0.0455(6) Uani d 1 C C2 0.4540(5) 0.3128(3) 0.6460(3) 0.0386(5) Uani d 1 C C6 -0.0917(6) 0.6567(4) 0.4700(3) 0.0472(7) Uani d 1 H H6A -0.0645 0.5545 0.4328 0.057 Uiso calc 1 H H6B -0.2285 0.6543 0.5321 0.057 Uiso calc 1 C C11 -0.2023(5) 0.5712(4) 0.9264(3) 0.0475(7) Uani d 1 H H11A -0.3005 0.6496 0.9745 0.057 Uiso calc 1 H H11B -0.3071 0.5033 0.8897 0.057 Uiso calc 1 C C112 0.0981(7) 0.5453(4) 1.0959(3) 0.0584(8) Uani d 1 H H112 0.1040 0.6532 1.0916 0.070 Uiso calc 1 C C8 -0.4279(7) 0.8699(5) 0.2188(4) 0.0649(10) Uani d 1 H H8A -0.5833 0.8501 0.1953 0.097 Uiso calc 1 H H8B -0.3165 0.8573 0.1446 0.097 Uiso calc 1 H H8C -0.4299 0.9745 0.2481 0.097 Uiso calc 1 C C116 -0.0616(8) 0.3156(4) 1.0306(4) 0.0638(9) Uani d 1 H H116 -0.1627 0.2664 0.9813 0.077 Uiso calc 1 C C115 0.0793(10) 0.2279(5) 1.1156(4) 0.0792(13) Uani d 1 H H115 0.0718 0.1202 1.1222 0.095 Uiso calc 1 C C113 0.2391(9) 0.4563(6) 1.1789(4) 0.0734(11) Uani d 1 H H113 0.3422 0.5039 1.2280 0.088 Uiso calc 1 C C114 0.2259(9) 0.2964(6) 1.1884(4) 0.0774(13) Uani d 1 H H114 0.3183 0.2363 1.2450 0.093 Uiso calc 1 O O72 -0.3587(4) 0.7608(3) 0.3218(2) 0.0535(5) Uani d 1 O O92 0.2915(4) 0.7852(3) 0.8366(3) 0.0554(5) Uani d 1 O O91 -0.0517(4) 0.8944(3) 0.9190(3) 0.0591(6) Uani d 1 O O71 -0.0124(5) 0.8698(3) 0.3220(3) 0.0637(7) Uani d 1 C C4 0.2004(5) 0.5547(3) 0.6269(3) 0.0370(5) Uani d 1 O O21 0.3934(4) 0.2806(2) 0.7613(2) 0.0473(5) Uani d 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O33 0.0494(13) 0.0492(13) 0.0673(15) -0.0017(11) -0.0076(11) 0.0051(11) Cl1 0.0759(6) 0.0560(5) 0.0586(5) 0.0031(4) 0.0241(4) -0.0061(4) Cl2 0.0741(6) 0.0476(4) 0.1050(8) -0.0204(4) 0.0308(5) -0.0288(5) Cl3 0.0413(4) 0.0946(7) 0.0838(6) 0.0154(4) -0.0058(4) -0.0032(5) N41 0.0439(13) 0.0350(11) 0.0398(12) 0.0079(10) -0.0005(9) 0.0012(9) C1 0.0375(14) 0.0379(14) 0.0531(16) -0.0024(11) 0.0056(11) -0.0056(11) C7 0.0410(14) 0.0435(15) 0.0412(14) 0.0029(12) -0.0024(11) 0.0028(11) C9 0.0441(14) 0.0397(14) 0.0459(15) 0.0077(11) -0.0048(11) 0.0056(12) C3 0.0417(14) 0.0403(14) 0.0398(13) 0.0013(11) 0.0024(10) 0.0017(11) C10 0.0375(13) 0.0376(13) 0.0444(14) 0.0073(11) -0.0052(11) -0.0035(11) C5 0.0419(14) 0.0338(13) 0.0481(15) -0.0020(10) -0.0039(11) 0.0043(11) C111 0.0480(15) 0.0477(16) 0.0385(13) 0.0000(13) 0.0078(12) -0.0018(12) C2 0.0349(12) 0.0363(13) 0.0440(14) 0.0022(10) -0.0012(10) -0.0049(10) C6 0.0478(16) 0.0414(15) 0.0532(16) -0.0051(12) -0.0114(13) 0.0081(13) C11 0.0387(14) 0.0508(17) 0.0516(16) 0.0032(12) 0.0001(12) -0.0028(13) C112 0.075(2) 0.0510(19) 0.0489(17) -0.0038(17) -0.0081(16) 0.0032(14) C8 0.063(2) 0.081(3) 0.0495(18) 0.0133(19) -0.0149(15) 0.0064(17) C116 0.082(3) 0.0495(19) 0.059(2) -0.0072(17) 0.0021(18) -0.0027(15) C115 0.115(4) 0.049(2) 0.069(3) 0.007(2) 0.006(3) 0.0063(18) C113 0.084(3) 0.085(3) 0.052(2) -0.004(2) -0.0171(19) 0.0069(19) C114 0.093(3) 0.078(3) 0.055(2) 0.026(2) -0.002(2) 0.013(2) O72 0.0482(12) 0.0614(14) 0.0511(12) -0.0012(10) -0.0121(9) 0.0063(10) O92 0.0449(12) 0.0501(13) 0.0709(14) -0.0013(10) -0.0017(10) -0.0073(11) O91 0.0540(13) 0.0445(12) 0.0778(16) 0.0107(10) -0.0050(11) -0.0166(11) O71 0.0538(14) 0.0628(15) 0.0738(16) -0.0076(11) -0.0098(12) 0.0244(12) C4 0.0379(12) 0.0331(13) 0.0400(13) -0.0025(10) -0.0037(10) 0.0014(10) O21 0.0524(12) 0.0423(11) 0.0432(11) 0.0133(9) 0.0038(8) 0.0029(9) 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' Cl Cl 0.1484 0.1585 '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 H33B O33 H33A 115(6) C4 N41 C10 126.9(2) C4 N41 H41 121(4) C10 N41 H41 112(4) C2 C1 Cl1 116.0(2) C2 C1 Cl3 107.9(2) Cl1 C1 Cl3 107.55(16) C2 C1 Cl2 107.0(2) Cl1 C1 Cl2 109.06(17) Cl3 C1 Cl2 109.22(17) O71 C7 O72 124.4(3) O71 C7 C6 125.1(3) O72 C7 C6 110.5(2) O91 C9 O92 124.1(3) O91 C9 C10 121.0(3) O92 C9 C10 114.9(3) C2 C3 C4 122.1(3) C2 C3 H3 119.0 C4 C3 H3 119.0 N41 C10 C9 113.6(2) N41 C10 C11 110.4(2) C9 C10 C11 111.3(2) N41 C10 H10 107.1 C9 C10 H10 107.1 C11 C10 H10 107.1 C4 C5 C6 110.9(2) C4 C5 H5A 109.5 C6 C5 H5A 109.5 C4 C5 H5B 109.5 C6 C5 H5B 109.5 H5A C5 H5B 108.0 C116 C111 C112 118.3(3) C116 C111 C11 120.3(3) C112 C111 C11 121.4(3) O21 C2 C3 125.9(3) O21 C2 C1 115.3(2) C3 C2 C1 118.7(3) C7 C6 C5 112.0(2) C7 C6 H6A 109.2 C5 C6 H6A 109.2 C7 C6 H6B 109.2 C5 C6 H6B 109.2 H6A C6 H6B 107.9 C111 C11 C10 113.8(2) C111 C11 H11A 108.8 C10 C11 H11A 108.8 C111 C11 H11B 108.8 C10 C11 H11B 108.8 H11A C11 H11B 107.7 C111 C112 C113 120.9(4) C111 C112 H112 119.6 C113 C112 H112 119.6 O72 C8 H8A 109.5 O72 C8 H8B 109.5 H8A C8 H8B 109.5 O72 C8 H8C 109.5 H8A C8 H8C 109.5 H8B C8 H8C 109.5 C111 C116 C115 120.1(4) C111 C116 H116 119.9 C115 C116 H116 119.9 C114 C115 C116 121.0(4) C114 C115 H115 119.5 C116 C115 H115 119.5 C114 C113 C112 119.7(4) C114 C113 H113 120.1 C112 C113 H113 120.1 C115 C114 C113 119.9(4) C115 C114 H114 120.1 C113 C114 H114 120.1 C7 O72 C8 115.5(3) C9 O92 H92 111(3) N41 C4 C3 122.1(2) N41 C4 C5 120.6(2) C3 C4 C5 117.4(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O33 H33B 0.87(6) O33 H33A 0.76(6) Cl1 C1 1.757(3) Cl2 C1 1.772(3) Cl3 C1 1.770(3) N41 C4 1.314(4) N41 C10 1.453(3) N41 H41 0.83(5) C1 C2 1.564(4) C7 O71 1.186(4) C7 O72 1.343(4) C7 C6 1.500(4) C9 O91 1.209(4) C9 O92 1.303(4) C9 C10 1.523(4) C3 C2 1.397(4) C3 C4 1.401(4) C3 H3 0.9300 C10 C11 1.545(4) C10 H10 0.9800 C5 C4 1.509(4) C5 C6 1.517(4) C5 H5A 0.9700 C5 H5B 0.9700 C111 C116 1.384(5) C111 C112 1.385(5) C111 C11 1.510(4) C2 O21 1.241(4) C6 H6A 0.9700 C6 H6B 0.9700 C11 H11A 0.9700 C11 H11B 0.9700 C112 C113 1.385(5) C112 H112 0.9300 C8 O72 1.448(4) C8 H8A 0.9600 C8 H8B 0.9600 C8 H8C 0.9600 C116 C115 1.393(6) C116 H116 0.9300 C115 C114 1.344(7) C115 H115 0.9300 C113 C114 1.382(7) C113 H113 0.9300 C114 H114 0.9300 O92 H92 0.89(5) loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA C6 H6A Cl1 1_455 0.97 2.94 3.774(3) 144.9 O33 H33B O91 1_655 0.87(6) 1.89(6) 2.766(4) 177(5) N41 H41 O21 . 0.83(5) 2.05(6) 2.672(3) 131(5) O33 H33A O21 1_565 0.76(6) 2.06(6) 2.815(3) 171(6) O92 H92 O33 . 0.89(5) 1.66(5) 2.542(4) 175(5) C3 H3 Cl1 . 0.93 2.55 3.031(3) 112.3 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 C4 N41 C10 C9 -76.6(4) C4 N41 C10 C11 157.5(3) O91 C9 C10 N41 178.7(3) O92 C9 C10 N41 -0.6(4) O91 C9 C10 C11 -56.0(3) O92 C9 C10 C11 124.7(3) C4 C3 C2 O21 -0.5(5) C4 C3 C2 C1 178.8(3) Cl1 C1 C2 O21 -173.6(2) Cl3 C1 C2 O21 -53.0(3) Cl2 C1 C2 O21 64.5(3) Cl1 C1 C2 C3 7.0(4) Cl3 C1 C2 C3 127.7(3) Cl2 C1 C2 C3 -114.9(3) O71 C7 C6 C5 13.3(5) O72 C7 C6 C5 -167.8(3) C4 C5 C6 C7 -168.9(3) C116 C111 C11 C10 -115.5(3) C112 C111 C11 C10 65.1(4) N41 C10 C11 C111 54.1(3) C9 C10 C11 C111 -73.0(3) C116 C111 C112 C113 1.9(6) C11 C111 C112 C113 -178.7(4) C112 C111 C116 C115 -1.1(5) C11 C111 C116 C115 179.5(4) C111 C116 C115 C114 0.3(7) C111 C112 C113 C114 -1.9(7) C116 C115 C114 C113 -0.3(7) C112 C113 C114 C115 1.0(7) O71 C7 O72 C8 -0.8(5) C6 C7 O72 C8 -179.7(3) C10 N41 C4 C3 175.1(3) C10 N41 C4 C5 -7.0(4) C2 C3 C4 N41 -2.2(5) C2 C3 C4 C5 179.8(3) C6 C5 C4 N41 -86.6(3) C6 C5 C4 C3 91.4(3) _cod_database_fobs_code 2238980