#------------------------------------------------------------------------------ #$Date: 2020-03-03 02:36:40 +0200 (Tue, 03 Mar 2020) $ #$Revision: 248620 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/74/1557425.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_1557425 loop_ _publ_author_name 'Jiang, Fan' 'Wang, Chang-Feng' 'Wu, Ya-Xing' 'Li, Hui-Hui' 'Shi, Chao' 'Ye, Heng-Yun' 'Zhang, Yi' _publ_section_title ; Nonlinear Optical and Photoluminescence Bistable Responses Accompanied by Tunable Dielectric Behaviors in Crown Inclusions ; _journal_name_full 'The Journal of Physical Chemistry C' _journal_paper_doi 10.1021/acs.jpcc.0c01122 _journal_year 2020 _chemical_formula_moiety 'C12 H24 O6, C7 H9 Cl N, Cl O5' _chemical_formula_sum 'C19 H33 Cl2 N O11' _chemical_formula_weight 522.36 _space_group_crystal_system orthorhombic _space_group_IT_number 36 _space_group_name_Hall 'C 2c -2' _space_group_name_H-M_alt 'C m c 21' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2013 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.2828(8) _cell_length_b 17.8489(14) _cell_length_c 12.4059(11) _cell_measurement_reflns_used 1319 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 19.6180 _cell_measurement_theta_min 2.2280 _cell_volume 2498.4(3) _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.967 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'XtaLAB Mini II' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0228 _diffrn_reflns_av_unetI/netI 0.0366 _diffrn_reflns_Laue_measured_fraction_full 0.967 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 5152 _diffrn_reflns_point_group_measured_fraction_full 0.875 _diffrn_reflns_point_group_measured_fraction_max 0.904 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.000 _diffrn_reflns_theta_min 2.282 _exptl_absorpt_coefficient_mu 0.316 _exptl_crystal_density_diffrn 1.389 _exptl_crystal_description block _exptl_crystal_F_000 1104 _refine_diff_density_max 0.609 _refine_diff_density_min -0.420 _refine_diff_density_rms 0.105 _refine_ls_abs_structure_details ; Flack x determined using 503 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack 0.92(5) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 167 _refine_ls_number_reflns 2099 _refine_ls_number_restraints 55 _refine_ls_restrained_S_all 1.120 _refine_ls_R_factor_all 0.1327 _refine_ls_R_factor_gt 0.1052 _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^)+(0.2000P)^2^+3.0000P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2823 _refine_ls_wR_factor_ref 0.3139 _reflns_Friedel_coverage 0.720 _reflns_Friedel_fraction_full 0.772 _reflns_Friedel_fraction_max 0.799 _reflns_number_gt 1416 _reflns_number_total 2099 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jp0c01122_si_004.cif _cod_data_source_block 43 _cod_database_code 1557425 _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. ; _shelxl_version_number 2013-2 _shelx_res_file ; TITL 43 in Cmc2(1) CELL 0.71073 11.2828 17.8489 12.4059 90.000 90.000 90.000 ZERR 32.00 0.0008 0.0014 0.0011 0.000 0.000 0.000 LATT -7 SYMM -X, -Y, 0.5+Z SYMM X, -Y, 0.5+Z SYMM -X, Y, Z SFAC C H N O Cl UNIT 32 32 32 32 32 OMIT 1 3 0 OMIT 1 1 0 OMIT -2.00 50.00 L.S. 50 ACTA BOND FMAP 2 PLAN 5 HTAB N1 O8_$2 HTAB N1 O7_$3 HTAB N1 O7_$2 HTAB N1 O6_$3 HTAB N1 O5_$2 HTAB N1 O6_$2 HTAB N1 O5_$2 HTAB N1 O7_$3 HTAB N1 O8_$2 HTAB N1 O7_$2 HTAB N1 O8_$2 HTAB N1 O7_$3 HTAB N1 O7_$2 HTAB N1 O5_$2 HTAB C9 O3_$4 EQIV $4 x+1/2, y+1/2, z ISOR 0.01 C7 C6 C8 C9 C10 C11 ISOR 0.01 O8 O7 O6 HTAB N1 O8_$2 HTAB N1 O7_$3 HTAB N1 O7_$2 HTAB N1 O6_$2 HTAB N1 O6_$3 HTAB N1 O5_$2 HTAB C8 O2_$1 HTAB CONF EQIV $1 -x+1/2, -y+1/2, z-1/2 HTAB C8 O2_$1 EQIV $2 -x, -y+1, z+1/2 HTAB N1 O5_$2 EQIV $3 x, -y+1, z+1/2 HTAB N1 O6_$3 HTAB N1 O6_$2 HTAB N1 O7_$2 HTAB N1 O7_$3 HTAB N1 O8_$2 HTAB C8 O2_$1 HTAB C9 O1_$1 HTAB N1 O7_$2 HTAB N1 O7_$3 HTAB N1 O5_$2 HTAB C9 O3_$4 HTAB N1 O7_$2 HTAB N1 O8_$2 HTAB N1 O7_$3 HTAB N1 O5_$2 HTAB N1 O6_$2 HTAB C9 O3_$4 HTAB N1 O5_$2 HTAB N1 O7_$2 HTAB N1 O7_$3 HTAB N1 O8_$2 WGHT 0.200000 3.000000 FVAR 0.17460 MOLE 2 C1 1 0.000000 0.486847 1.003638 10.50000 0.10285 0.07517 = 0.08773 -0.02810 0.00000 0.00000 AFIX 23 H1A 2 -0.069590 0.509770 1.035578 10.50000 -1.20000 H1B 2 0.069590 0.509770 1.035578 10.50000 -1.20000 AFIX 0 C2 1 0.000000 0.403053 1.027570 10.50000 0.07864 0.07855 = 0.05194 -0.00380 0.00000 0.00000 C3 1 0.105253 0.362539 1.035427 11.00000 0.04621 0.12207 = 0.05966 0.00076 -0.00916 -0.01751 AFIX 43 H3 2 0.177140 0.387625 1.028910 11.00000 -1.20000 AFIX 0 C4 1 0.105516 0.286688 1.052510 11.00000 0.05516 0.08430 = 0.06414 0.01318 -0.00612 0.00498 AFIX 43 H4 2 0.176334 0.260599 1.060412 11.00000 -1.20000 AFIX 0 C5 1 0.000000 0.250696 1.057590 10.50000 0.05771 0.09316 = 0.05429 0.02282 0.00000 0.00000 MOLE 3 C6 1 0.099956 0.303363 0.368993 11.00000 0.16274 0.12234 = 0.14087 0.01438 -0.01818 0.04008 AFIX 23 H6A 2 0.098717 0.259163 0.323516 11.00000 -1.20000 H6B 2 0.101222 0.286920 0.443508 11.00000 -1.20000 AFIX 0 C7 1 0.214445 0.349704 0.344826 11.00000 0.14688 0.11810 = 0.14860 -0.01449 -0.01369 0.01985 AFIX 23 H7A 2 0.283227 0.319404 0.362141 11.00000 -1.20000 H7B 2 0.217303 0.360853 0.268345 11.00000 -1.20000 AFIX 0 C8 1 0.318617 0.458471 0.369154 11.00000 0.07072 0.17374 = 0.18784 0.02295 -0.00022 0.00562 AFIX 23 H8A 2 0.382261 0.424901 0.348412 11.00000 -1.20000 H8B 2 0.344466 0.483752 0.434253 11.00000 -1.20000 AFIX 0 C9 1 0.310512 0.517342 0.282656 11.00000 0.13361 0.17334 = 0.15332 -0.03529 -0.00828 0.02606 AFIX 23 H9A 2 0.380496 0.548869 0.284858 11.00000 -1.20000 H9B 2 0.307229 0.493465 0.212482 11.00000 -1.20000 AFIX 0 C10 1 0.208711 0.615996 0.218921 11.00000 0.12400 0.11766 = 0.11710 0.00745 0.00590 -0.03879 AFIX 23 H10A 2 0.279175 0.646923 0.224083 11.00000 -1.20000 H10B 2 0.206272 0.593486 0.147790 11.00000 -1.20000 AFIX 0 C11 1 0.098003 0.662975 0.238312 11.00000 0.14269 0.16611 = 0.12283 -0.00401 0.01664 -0.05714 AFIX 23 H11A 2 0.096154 0.679341 0.312851 11.00000 -1.20000 H11B 2 0.100278 0.707157 0.192831 11.00000 -1.20000 AFIX 0 MOLE 1 CL1 5 0.000000 0.118333 0.561184 10.50000 0.06417 0.06946 = 0.12399 0.00610 0.00000 0.00000 MOLE 2 CL2 5 0.000000 0.152286 1.074898 10.50000 0.10678 0.08421 = 0.11018 0.03316 0.00000 0.00000 N1 3 0.000000 0.500230 0.887224 10.50000 0.04510 0.03936 = 0.09578 -0.01195 0.00000 0.00000 AFIX 137 H1C 2 0.020914 0.547452 0.874223 10.50000 -1.50000 H1D 2 -0.072264 0.491984 0.861023 10.50000 -1.50000 H1E 2 0.051350 0.469392 0.855647 10.50000 -1.50000 AFIX 0 MOLE 1 O1 4 0.000000 0.042252 0.588712 10.50000 0.21610 0.08062 = 0.18449 0.02958 0.00000 0.00000 MOLE 3 O2 4 0.000000 0.135051 0.678074 10.50000 0.50844 0.14710 = 0.45261 0.03369 0.00000 0.00000 O3 4 0.000000 0.119401 0.440378 10.50000 0.56762 0.17842 = 0.12437 -0.00143 0.00000 0.00000 MOLE 1 O4 4 0.101535 0.158418 0.567599 11.00000 0.09315 0.17739 = 0.28446 0.03215 -0.01644 -0.02793 MOLE 3 O5 4 0.000000 0.344496 0.351023 10.50000 0.13890 0.10234 = 0.16412 -0.03834 0.00000 0.00000 O6 4 0.220340 0.412398 0.398748 11.00000 0.13406 0.17954 = 0.18497 -0.01525 -0.02271 0.01951 O7 4 0.209979 0.561005 0.297647 11.00000 0.08591 0.16405 = 0.12468 -0.02057 0.01704 -0.01973 O8 4 0.000000 0.623284 0.216486 10.50000 0.12967 0.11729 = 0.09896 -0.00563 0.00000 0.00000 HKLF 4 REM 43 in Cmc2(1) REM R1 = 0.1052 for 1416 Fo > 4sig(Fo) and 0.1327 for all 2099 data REM 167 parameters refined using 55 restraints END WGHT 0.2000 0.0000 REM Instructions for potential hydrogen bonds HTAB N1 O5_$2 HTAB N1 O6_$3 HTAB N1 O6_$2 HTAB N1 O7_$2 HTAB N1 O7_$3 HTAB N1 O8_$2 REM Highest difference peak 0.609, deepest hole -0.420, 1-sigma level 0.105 Q1 1 0.2290 0.4965 0.3183 11.00000 0.05 0.61 Q2 1 0.1157 0.6132 0.2452 11.00000 0.05 0.45 Q3 1 0.1238 0.3740 0.3908 11.00000 0.05 0.43 Q4 1 0.0000 0.1846 1.0771 10.50000 0.05 0.37 Q5 1 0.2347 0.5300 0.1220 11.00000 0.05 0.35 ; _shelx_res_checksum 76956 _shelx_hkl_file ; 0 0 -15 -0.64 0.55 0 0 -14 -1.13 0.57 0 0 -13 -0.55 0.54 0 0 -12 6.09 0.67 0 0 -11 -0.55 0.47 0 0 -10 4.61 0.57 0 0 -9 -0.20 0.43 0 0 -8 37.68 1.54 0 0 -7 0.09 0.34 0 0 -6 731.94 24.17 0 0 -5 -0.04 0.25 0 0 -4 1187.66 39.02 0 0 -3 0.34 0.22 0 0 -2 80.84 2.71 0 0 2 87.99 2.94 0 0 3 0.03 0.20 0 0 4 1201.79 39.46 0 0 5 0.20 0.21 0 0 9 0.59 0.37 0 0 10 5.75 0.59 0 0 11 0.37 0.46 0 0 12 8.81 0.74 0 0 13 -0.13 0.44 0 0 14 -0.20 0.48 0 0 15 0.07 0.48 0 0 16 -0.15 0.51 0 0 17 -0.24 0.54 0 -2 -15 0.77 0.54 0 -2 -14 0.46 0.53 0 -2 -13 3.87 0.67 0 -2 -12 0.23 0.50 0 -2 -11 1.62 0.49 0 2 -11 1.24 0.49 0 -2 -10 17.65 0.98 0 2 -10 15.02 0.94 0 2 -9 31.28 1.41 0 -2 -9 33.84 1.43 0 -2 -8 18.40 0.92 0 2 -8 18.06 0.93 0 -2 -7 50.50 1.95 0 2 -7 53.11 1.96 0 2 -6 76.31 2.62 0 2 -6 73.95 2.70 0 -2 -6 76.40 2.71 0 2 -5 75.42 2.62 0 2 -5 77.34 2.57 0 -2 -5 71.37 2.62 0 2 -5 72.37 2.62 0 2 -4 17.03 0.76 0 -2 -4 17.41 0.76 0 2 -3 1772.57 58.15 0 2 -2 473.36 15.57 0 -2 -1 109.83 3.43 0 2 -1 95.02 3.45 0 -2 0 47.94 1.43 0 2 0 24.34 1.40 0 -2 1 99.10 3.31 0 2 2 503.98 16.54 0 -2 3 1863.60 61.10 0 2 4 16.66 0.59 0 -2 4 17.18 0.69 0 -2 5 71.35 2.44 0 2 5 69.16 2.33 0 2 6 74.33 2.50 0 2 8 21.06 1.01 0 2 9 32.97 1.44 0 -2 9 32.93 1.43 0 -2 10 17.23 0.95 0 2 10 17.63 0.97 0 -2 11 1.66 0.49 0 2 11 1.40 0.50 0 -2 12 0.17 0.44 0 2 12 0.12 0.44 0 2 13 4.48 0.61 0 -2 13 3.79 0.61 0 -2 14 0.53 0.47 0 2 14 0.68 0.47 0 2 15 -0.15 0.49 0 -2 15 -0.07 0.49 0 2 16 -0.93 0.54 0 -2 16 0.23 0.50 0 2 17 0.65 0.55 0 -2 17 0.32 0.52 0 -4 -15 0.15 0.58 0 -4 -14 -0.49 0.56 0 -4 -13 1.16 0.56 0 -4 -12 0.30 0.51 0 -4 -11 0.16 0.48 0 -4 -10 7.25 0.69 0 -4 -9 3.45 0.54 0 -4 -8 24.12 1.13 0 -4 -7 13.74 0.77 0 -4 -6 132.95 4.80 0 4 -6 144.00 4.74 0 4 -5 31.88 1.21 0 4 -4 35.59 1.31 0 -4 -3 107.65 3.61 0 4 -3 110.97 3.69 0 -4 -2 290.04 8.22 0 -4 -2 286.01 8.19 0 4 -2 287.33 8.27 0 4 -2 291.07 8.27 0 4 -1 110.32 3.76 0 4 -1 110.43 3.75 0 -4 -1 114.05 3.74 0 -4 0 998.56 36.37 0 4 0 996.23 36.36 0 4 1 117.70 3.83 0 -4 1 113.23 3.85 0 -4 1 115.88 3.87 0 -4 1 115.04 3.85 0 4 1 118.04 3.80 0 4 1 110.82 3.80 0 4 1 112.22 3.86 0 4 2 283.88 9.42 0 -4 2 291.19 9.48 0 4 2 284.37 9.39 0 4 3 100.16 3.33 0 4 4 34.36 1.20 0 4 5 30.28 1.08 0 -4 5 29.49 1.15 0 4 6 137.00 4.72 0 4 7 13.14 0.72 0 -4 8 22.40 1.01 0 4 8 21.45 1.04 0 4 9 3.85 0.51 0 -4 9 4.36 0.49 0 -4 10 6.31 0.60 0 4 10 8.19 0.66 0 -4 11 0.92 0.45 0 4 11 0.55 0.44 0 4 12 -0.42 0.48 0 -4 12 0.50 0.44 0 -4 13 1.64 0.49 0 4 13 1.61 0.51 0 -4 14 0.98 0.50 0 4 14 -0.07 0.47 0 -4 15 0.42 0.51 0 4 15 -0.29 0.54 0 4 16 0.39 0.55 0 -4 16 1.34 0.56 0 -4 17 -0.08 0.50 0 -6 -16 0.24 0.61 0 -6 -15 0.92 0.61 0 -6 -14 0.79 0.56 0 -6 -13 1.15 0.58 0 -6 -12 0.93 0.58 0 -6 -11 0.86 0.53 0 -6 -10 2.83 0.54 0 -6 -9 2.09 0.55 0 -6 -8 25.67 1.22 0 -6 -7 38.80 1.60 0 -6 -5 27.01 0.95 0 -6 -4 50.32 1.72 0 6 -4 52.66 1.84 0 6 -4 46.85 1.82 0 6 -3 82.77 2.54 0 6 -3 76.67 2.54 0 -6 -3 79.06 2.45 0 6 -3 77.45 2.53 0 -6 -3 78.39 2.42 0 -6 -3 77.58 2.42 0 6 -2 1.56 0.23 0 -6 -2 1.27 0.12 0 6 -2 1.06 0.22 0 -6 -2 1.53 0.20 0 -6 -1 40.90 1.43 0 6 -1 39.91 1.43 0 6 -1 37.41 1.44 0 -6 0 372.12 12.23 0 6 0 370.49 12.24 0 6 0 365.20 12.21 0 -6 0 369.55 12.19 0 -6 1 42.16 1.48 0 6 1 37.79 1.38 0 6 1 39.74 1.46 0 6 1 40.21 1.42 0 -6 1 40.33 1.44 0 -6 1 39.09 1.44 0 6 1 40.55 1.36 0 6 2 1.19 0.15 0 6 2 1.26 0.15 0 -6 2 1.07 0.19 0 -6 2 0.87 0.26 0 6 2 1.21 0.24 0 -6 3 83.05 2.93 0 6 3 83.16 2.85 0 6 4 49.61 1.68 0 6 4 47.27 1.76 0 6 5 27.23 0.98 0 6 5 27.63 1.11 0 6 6 7.68 0.51 0 -6 7 41.62 1.62 0 6 7 43.13 1.67 0 6 8 26.31 1.17 0 -6 8 24.21 1.10 0 6 9 3.44 0.50 0 -6 9 2.20 0.42 0 6 10 1.97 0.48 0 -6 10 2.46 0.44 0 6 11 1.40 0.48 0 -6 11 0.96 0.43 0 -6 12 1.43 0.46 0 6 12 0.73 0.46 0 6 13 0.98 0.49 0 -6 13 1.36 0.46 0 6 14 -0.14 0.48 0 6 15 -0.22 0.56 0 6 16 0.08 0.53 0 -8 -16 0.41 0.64 0 -8 -15 1.03 0.65 0 -8 -14 0.30 0.60 0 -8 -13 -0.14 0.57 0 -8 -12 1.71 0.62 0 -8 -11 0.43 0.54 0 -8 -10 1.79 0.56 0 -8 -9 10.15 0.82 0 8 -8 6.29 0.56 0 -8 -8 6.50 0.66 0 8 -7 2.92 0.44 0 8 -6 58.36 2.21 0 8 -5 58.99 2.19 0 8 -4 43.26 1.68 0 -8 -4 44.26 1.57 0 -8 -3 14.46 0.62 0 8 -3 12.76 0.68 0 -8 -2 134.84 4.50 0 8 -2 136.96 4.62 0 8 -2 133.82 4.44 0 -8 -2 136.58 4.57 0 8 -1 25.86 1.11 0 -8 -1 27.50 1.10 0 8 -1 27.02 1.08 0 -8 -1 29.56 1.05 0 8 0 243.44 8.15 0 -8 0 239.56 8.09 0 -8 0 250.61 8.15 0 8 0 244.18 8.11 0 -8 0 237.86 8.11 0 8 1 25.97 1.11 0 -8 1 25.46 1.06 0 8 1 28.47 1.05 0 -8 1 27.44 1.09 0 8 1 28.20 1.00 0 8 2 136.25 4.64 0 -8 2 133.12 4.45 0 8 2 135.83 4.51 0 8 2 139.43 4.56 0 -8 2 137.75 4.64 0 8 3 13.87 0.59 0 -8 3 14.97 0.76 0 -8 3 13.65 0.53 0 -8 4 45.30 1.63 0 8 4 48.13 1.69 0 8 5 60.40 2.12 0 -8 5 57.02 2.05 0 -8 6 59.82 2.18 0 8 6 62.92 2.25 0 8 7 2.54 0.38 0 8 8 5.51 0.52 0 8 9 8.43 0.66 0 8 10 2.30 0.51 0 8 11 2.01 0.47 0 8 12 1.34 0.47 0 8 13 0.65 0.47 0 8 14 -0.49 0.51 0 8 15 -0.07 0.49 0 8 16 -0.46 0.52 0 -10 -15 0.65 0.65 0 -10 -14 0.23 0.59 0 10 -13 -0.43 0.51 0 -10 -13 0.59 0.60 0 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0.37 0.53 -13 -9 -1 0.23 0.51 -13 -9 -1 -0.43 0.53 -13 -9 0 -0.46 0.50 -13 -9 0 0.43 0.52 -13 -9 1 0.31 0.52 -13 -9 2 0.38 0.53 -13 -9 5 0.15 0.52 -13 -11 -5 0.25 0.54 -13 -11 -4 -0.49 0.55 -13 -11 -3 -0.48 0.54 -13 -11 -2 0.16 0.51 -13 -11 -1 1.43 0.58 -13 -11 0 1.43 0.59 -13 -11 1 0.56 0.55 -13 -11 4 0.08 0.56 13 -11 4 -0.08 0.58 -13 -11 5 0.73 0.56 13 -11 5 -0.61 0.65 -13 -13 -2 0.08 0.58 -13 -13 -1 0.65 0.57 -13 -13 1 0.85 0.57 -13 -13 2 0.09 0.55 13 -13 3 0.33 0.59 -14 0 -7 -0.26 0.63 -14 0 -6 -0.08 0.60 -14 0 -5 -0.41 0.61 -14 0 -4 -0.08 0.59 -14 0 -3 -0.08 0.56 -14 0 -2 0.61 0.59 -14 0 -1 -0.35 0.46 -14 0 -1 0.23 0.54 14 0 2 -0.22 0.47 14 0 3 0.08 0.50 14 0 4 0.46 0.50 14 0 5 0.16 0.48 14 0 6 0.08 0.50 14 0 7 0.99 0.55 -14 2 -7 -0.82 0.62 -14 -2 -7 -0.53 0.64 -14 2 -6 -0.08 0.58 -14 -2 -6 0.52 0.62 -14 2 -5 0.08 0.59 -14 -2 -5 -0.67 0.63 -14 2 -4 0.08 0.58 -14 -2 -4 -0.08 0.59 -14 2 -3 0.23 0.54 -14 -2 -3 0.48 0.59 -14 -2 -2 1.33 0.54 -14 2 -2 0.22 0.58 -14 -2 -2 1.00 0.63 -14 -2 -1 -0.65 0.51 -14 2 -1 0.30 0.54 -14 -2 -1 -0.08 0.60 -14 -2 0 -0.64 0.52 -14 -2 0 0.62 0.58 -14 -2 1 0.69 0.48 14 2 3 0.16 0.49 14 -2 3 0.30 0.48 14 2 4 -0.47 0.51 14 -2 4 -0.23 0.50 14 2 5 0.32 0.50 14 -2 5 -0.71 0.55 14 2 6 -0.41 0.51 14 -2 6 0.32 0.50 14 2 7 -0.08 0.52 14 -2 7 0.82 0.56 -14 4 -7 -0.23 0.58 -14 4 -6 -0.08 0.54 -14 -4 -6 -0.52 0.63 -14 4 -5 0.23 0.56 -14 -4 -5 -0.17 0.61 -14 4 -4 1.13 0.58 -14 -4 -4 0.17 0.61 -14 -4 -3 1.48 0.56 -14 4 -3 0.29 0.53 -14 -4 -3 0.72 0.61 -14 -4 -2 -0.15 0.50 -14 4 -2 0.29 0.57 -14 -4 -2 0.62 0.57 -14 -4 -1 0.30 0.51 -14 -4 -1 0.08 0.56 -14 -4 0 1.48 0.57 -14 -4 0 1.99 0.65 -14 -4 1 0.51 0.53 -14 -4 2 0.14 0.52 14 4 4 0.16 0.50 14 4 5 0.08 0.52 14 -4 5 1.50 0.54 14 4 6 -0.17 0.54 14 -4 6 0.16 0.50 14 -4 7 -0.41 0.51 -14 -6 -6 1.92 0.71 -14 -6 -5 -0.41 0.54 -14 -6 -5 0.26 0.62 -14 -6 -4 0.66 0.56 -14 -6 -4 0.50 0.60 -14 -6 -3 0.48 0.55 -14 -6 -3 0.48 0.59 -14 -6 -2 -0.80 0.55 -14 -6 -2 -0.31 0.59 -14 -6 -1 0.47 0.56 -14 -6 -1 0.15 0.53 -14 -6 0 0.69 0.51 -14 -6 0 0.08 0.56 -14 -6 1 0.23 0.50 -14 -6 2 -0.08 0.50 -14 -6 3 0.67 0.55 14 6 5 -0.42 0.52 -14 -8 -5 0.08 0.60 -14 -8 -4 -0.08 0.60 -14 -8 -4 0.17 0.59 -14 -8 -3 0.08 0.54 -14 -8 -3 0.08 0.60 -14 -8 -2 0.57 0.56 -14 -8 -2 -0.08 0.56 -14 -8 -1 0.72 0.59 -14 -8 -1 0.15 0.53 -14 -8 0 0.32 0.55 -14 -8 1 -0.24 0.56 -14 -8 2 0.24 0.55 -14 -10 -4 -0.08 0.59 -14 -10 -2 -0.41 0.57 -14 -10 -1 1.00 0.58 -14 -10 0 -0.33 0.56 -14 -10 1 -0.41 0.55 -15 1 -4 -0.17 0.58 -15 -1 -4 0.51 0.63 -15 1 -3 -0.08 0.58 -15 -1 -3 -0.83 0.62 -15 -1 -2 0.69 0.53 -15 1 -2 -0.24 0.57 -15 -1 -2 1.30 0.61 -15 -1 -1 -0.15 0.53 -15 1 -1 0.32 0.57 -15 -1 -1 1.46 0.63 15 1 3 0.08 0.49 15 -1 3 -0.08 0.50 15 1 4 -0.08 0.54 15 -1 4 -0.16 0.51 15 -1 5 0.41 0.54 -15 -3 -4 -1.14 0.60 -15 3 -4 0.64 0.57 -15 -3 -3 0.32 0.53 -15 3 -3 0.16 0.57 -15 -3 -3 0.08 0.59 -15 -3 -2 0.56 0.55 -15 3 -2 0.31 0.56 -15 -3 -2 0.16 0.61 -15 -3 -1 0.16 0.52 -15 -3 -1 -0.08 0.60 -15 -3 0 0.46 0.50 15 3 4 0.08 0.52 15 -3 5 0.17 0.52 -15 -5 -2 -1.08 0.60 -15 5 -2 0.38 0.58 -15 -5 -2 -0.25 0.60 -15 -5 -1 0.57 0.56 -15 -5 -1 1.40 0.64 -15 -5 0 -0.16 0.51 -15 -5 1 0.08 0.53 -15 -5 2 0.08 0.51 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 87465 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y, z+1/2' '-x, y, z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z' 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 C1 C 0.0000 0.4868(10) 1.0036(15) 0.089(5) Uani 1 2 d S T P . . H1A H -0.0696 0.5098 1.0356 0.106 Uiso 0.5 1 calc R U P . . H1B H 0.0696 0.5098 1.0356 0.106 Uiso 0.5 1 calc R U P . . C2 C 0.0000 0.4031(9) 1.0276(10) 0.070(4) Uani 1 2 d S T P . . C3 C 0.1053(8) 0.3625(7) 1.0354(8) 0.076(3) Uani 1 1 d . . . . . H3 H 0.1771 0.3876 1.0289 0.091 Uiso 1 1 calc R U . . . C4 C 0.1055(7) 0.2867(6) 1.0525(9) 0.068(2) Uani 1 1 d . . . . . H4 H 0.1763 0.2606 1.0604 0.081 Uiso 1 1 calc R U . . . C5 C 0.0000 0.2507(8) 1.0576(12) 0.068(3) Uani 1 2 d S T P . . C6 C 0.1000(19) 0.3034(12) 0.3690(18) 0.142(6) Uani 1 1 d . U . . . H6A H 0.0987 0.2592 0.3235 0.170 Uiso 1 1 calc R U . . . H6B H 0.1012 0.2869 0.4435 0.170 Uiso 1 1 calc R U . . . C7 C 0.2144(18) 0.3497(12) 0.3448(18) 0.138(6) Uani 1 1 d . U . . . H7A H 0.2832 0.3194 0.3621 0.165 Uiso 1 1 calc R U . . . H7B H 0.2173 0.3609 0.2683 0.165 Uiso 1 1 calc R U . . . C8 C 0.3186(14) 0.4585(13) 0.369(2) 0.144(6) Uani 1 1 d . U . . . H8A H 0.3823 0.4249 0.3484 0.173 Uiso 1 1 calc R U . . . H8B H 0.3445 0.4838 0.4343 0.173 Uiso 1 1 calc R U . . . C9 C 0.311(2) 0.5173(14) 0.2827(19) 0.153(8) Uani 1 1 d . U . . . H9A H 0.3805 0.5489 0.2849 0.184 Uiso 1 1 calc R U . . . H9B H 0.3072 0.4935 0.2125 0.184 Uiso 1 1 calc R U . . . C10 C 0.2087(17) 0.6160(9) 0.2189(15) 0.120(5) Uani 1 1 d . U . . . H10A H 0.2792 0.6469 0.2241 0.144 Uiso 1 1 calc R U . . . H10B H 0.2063 0.5935 0.1478 0.144 Uiso 1 1 calc R U . . . C11 C 0.0980(18) 0.6630(14) 0.2383(17) 0.144(6) Uani 1 1 d . U . . . H11A H 0.0962 0.6793 0.3129 0.173 Uiso 1 1 calc R U . . . H11B H 0.1003 0.7072 0.1928 0.173 Uiso 1 1 calc R U . . . Cl1 Cl 0.0000 0.1183(2) 0.5612(4) 0.0859(13) Uani 1 2 d S T P . . Cl2 Cl 0.0000 0.1523(2) 1.0749(4) 0.1004(16) Uani 1 2 d S T P . . N1 N 0.0000 0.5002(5) 0.8872(10) 0.060(3) Uani 1 2 d S T P . . H1C H 0.0209 0.5475 0.8742 0.090 Uiso 0.5 1 calc R U P . . H1D H -0.0723 0.4920 0.8610 0.090 Uiso 0.5 1 calc R U P . . H1E H 0.0513 0.4694 0.8556 0.090 Uiso 0.5 1 calc R U P . . O1 O 0.0000 0.0423(8) 0.589(2) 0.160(8) Uani 1 2 d S T P . . O2 O 0.0000 0.135(2) 0.678(7) 0.37(3) Uani 1 2 d S T P . . O3 O 0.0000 0.1194(17) 0.440(3) 0.29(2) Uani 1 2 d S T P . . O4 O 0.1015(10) 0.1584(9) 0.568(2) 0.185(7) Uani 1 1 d . . . . . O5 O 0.0000 0.3445(10) 0.3510(16) 0.135(6) Uani 1 2 d S T P . . O6 O 0.2203(14) 0.4124(10) 0.3987(15) 0.166(5) Uani 1 1 d . U . . . O7 O 0.2100(10) 0.5610(8) 0.2976(11) 0.125(4) Uani 1 1 d . U . . . O8 O 0.0000 0.6233(9) 0.2165(12) 0.115(5) Uani 1 2 d S TU P . . 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 C1 0.103(13) 0.075(10) 0.088(11) -0.028(9) 0.000 0.000 C2 0.079(9) 0.079(9) 0.052(7) -0.004(6) 0.000 0.000 C3 0.046(4) 0.122(9) 0.060(5) 0.001(5) -0.009(4) -0.018(5) C4 0.055(4) 0.084(6) 0.064(5) 0.013(5) -0.006(5) 0.005(4) C5 0.058(6) 0.093(9) 0.054(7) 0.023(8) 0.000 0.000 C6 0.163(12) 0.122(10) 0.141(11) 0.014(9) -0.018(9) 0.040(9) C7 0.147(11) 0.118(10) 0.149(12) -0.014(9) -0.014(9) 0.020(9) C8 0.071(8) 0.174(11) 0.188(12) 0.023(11) 0.000(8) 0.006(8) C9 0.134(12) 0.173(13) 0.153(13) -0.035(10) -0.008(9) 0.026(10) C10 0.124(10) 0.118(9) 0.117(9) 0.007(8) 0.006(8) -0.039(8) C11 0.143(11) 0.166(12) 0.123(10) -0.004(9) 0.017(9) -0.057(10) Cl1 0.0642(17) 0.069(2) 0.124(4) 0.006(3) 0.000 0.000 Cl2 0.107(3) 0.084(2) 0.110(4) 0.033(3) 0.000 0.000 N1 0.045(5) 0.039(4) 0.096(9) -0.012(5) 0.000 0.000 O1 0.22(2) 0.081(8) 0.184(19) 0.030(12) 0.000 0.000 O2 0.51(9) 0.15(3) 0.45(9) 0.03(4) 0.000 0.000 O3 0.57(7) 0.18(3) 0.124(18) -0.001(18) 0.000 0.000 O4 0.093(7) 0.177(12) 0.28(2) 0.032(16) -0.016(12) -0.028(7) O5 0.139(14) 0.102(11) 0.164(17) -0.038(10) 0.000 0.000 O6 0.134(9) 0.180(10) 0.185(10) -0.015(9) -0.023(8) 0.020(8) O7 0.086(6) 0.164(9) 0.125(8) -0.021(7) 0.017(5) -0.020(6) O8 0.130(10) 0.117(9) 0.099(8) -0.006(7) 0.000 0.000 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 110.6(12) . . ? C3 C2 C3 116.9(15) 4 . ? C3 C2 C1 121.5(7) 4 . ? C3 C2 C1 121.5(7) . . ? C2 C3 C4 121.7(10) . . ? C5 C4 C3 118.3(9) . . ? C4 C5 C4 123.1(14) 4 . ? C4 C5 Cl2 118.5(7) 4 . ? C4 C5 Cl2 118.5(7) . . ? O5 C6 C7 111.5(16) . . ? O6 C7 C6 113.4(19) . . ? O6 C8 C9 122.6(17) . . ? O7 C9 C8 110.2(18) . . ? C11 C10 O7 106.7(15) . . ? O8 C11 C10 110.7(19) . . ? O4 Cl1 O4 115.7(14) . 4 ? O4 Cl1 O1 119.9(7) . . ? O4 Cl1 O1 119.9(7) 4 . ? O4 Cl1 O3 93.0(12) . . ? O4 Cl1 O3 93.0(12) 4 . ? O1 Cl1 O3 104.8(16) . . ? O4 Cl1 O2 80.5(13) . . ? O4 Cl1 O2 80.6(13) 4 . ? O1 Cl1 O2 87.5(19) . . ? O3 Cl1 O2 168(2) . . ? C6 O5 C6 112(2) 4 . ? C7 O6 C8 113.7(19) . . ? C9 O7 C10 108.2(16) . . ? C11 O8 C11 111(3) 4 . ? 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 N1 1.46(2) . ? C1 C2 1.52(2) . ? C2 C3 1.394(14) 4 ? C2 C3 1.394(14) . ? C3 C4 1.370(15) . ? C4 C5 1.354(12) . ? C5 C4 1.354(12) 4 ? C5 Cl2 1.770(15) . ? C6 O5 1.364(19) . ? C6 C7 1.56(3) . ? C7 O6 1.31(2) . ? C8 O6 1.43(3) . ? C8 C9 1.50(3) . ? C9 O7 1.39(3) . ? C10 C11 1.52(3) . ? C10 O7 1.38(2) . ? C11 O8 1.34(2) . ? Cl1 O4 1.353(13) . ? Cl1 O4 1.353(13) 4 ? Cl1 O1 1.400(16) . ? Cl1 O3 1.50(3) . ? Cl1 O2 1.48(8) . ? O5 C6 1.364(19) 4 ? O8 C11 1.34(2) 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 N1 H1E O8 0.89 2.46 3.057(19) 124.8 2_565 N1 H1E O7 0.89 2.00 2.836(13) 155.1 3_565 N1 H1D O7 0.89 1.98 2.836(13) 160.4 2_565 N1 H1C O6 0.89 2.38 2.938(16) 120.8 3_565 N1 H1C O5 0.89 1.96 2.808(19) 157.6 2_565 N1 H1D O6 0.89 2.43 2.938(16) 116.3 2_565 N1 H1C O5 0.89 1.96 2.808(19) 157.6 2_565 N1 H1E O7 0.89 2.00 2.836(13) 155.1 3_565 N1 H1E O8 0.89 2.46 3.057(19) 124.8 2_565 N1 H1D O7 0.89 1.98 2.836(13) 160.4 2_565 N1 H1E O8 0.89 2.46 3.057(19) 124.8 2_565 N1 H1E O7 0.89 2.00 2.836(13) 155.1 3_565 N1 H1D O7 0.89 1.98 2.836(13) 160.4 2_565 N1 H1C O5 0.89 1.96 2.808(19) 157.6 2_565 C9 H9A O3 0.97 2.67 3.42(3) 134.8 5 N1 H1E O8 0.89 2.46 3.057(19) 124.8 2_565 N1 H1E O7 0.89 2.00 2.836(13) 155.1 3_565 N1 H1D O7 0.89 1.98 2.836(13) 160.4 2_565 N1 H1D O6 0.89 2.43 2.938(16) 116.3 2_565 N1 H1C O6 0.89 2.38 2.938(16) 120.8 3_565 N1 H1C O5 0.89 1.96 2.808(19) 157.6 2_565 C8 H8A O2 0.97 2.72 3.55(6) 144.3 6_554 C8 H8A O2 0.97 2.72 3.55(6) 144.3 6_554 N1 H1C O5 0.89 1.96 2.808(19) 157.6 2_565 N1 H1C O6 0.89 2.38 2.938(16) 120.8 3_565 N1 H1D O6 0.89 2.43 2.938(16) 116.3 2_565 N1 H1D O7 0.89 1.98 2.836(13) 160.4 2_565 N1 H1E O7 0.89 2.00 2.836(13) 155.1 3_565 N1 H1E O8 0.89 2.46 3.057(19) 124.8 2_565 C8 H8A O2 0.97 2.72 3.55(6) 144.3 6_554 C9 H9B O1 0.97 2.74 3.39(3) 125.1 6_554 N1 H1D O7 0.89 1.98 2.836(13) 160.4 2_565 N1 H1E O7 0.89 2.00 2.836(13) 155.1 3_565 N1 H1C O5 0.89 1.96 2.808(19) 157.6 2_565 C9 H9A O3 0.97 2.67 3.42(3) 134.8 5 N1 H1D O7 0.89 1.98 2.836(13) 160.4 2_565 N1 H1E O8 0.89 2.46 3.057(19) 124.8 2_565 N1 H1E O7 0.89 2.00 2.836(13) 155.1 3_565 N1 H1C O5 0.89 1.96 2.808(19) 157.6 2_565 N1 H1D O6 0.89 2.43 2.938(16) 116.3 2_565 C9 H9A O3 0.97 2.67 3.42(3) 134.8 5 N1 H1C O5 0.89 1.96 2.808(19) 157.6 2_565 N1 H1D O7 0.89 1.98 2.836(13) 160.4 2_565 N1 H1E O7 0.89 2.00 2.836(13) 155.1 3_565 N1 H1E O8 0.89 2.46 3.057(19) 124.8 2_565 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 N1 C1 C2 C3 -87.8(11) . . . 4 ? N1 C1 C2 C3 87.8(11) . . . . ? C3 C2 C3 C4 -1.4(19) 4 . . . ? C1 C2 C3 C4 -177.3(12) . . . . ? C2 C3 C4 C5 2.5(16) . . . . ? C3 C4 C5 C4 -4(2) . . . 4 ? C3 C4 C5 Cl2 177.8(10) . . . . ? O5 C6 C7 O6 56(3) . . . . ? O6 C8 C9 O7 48(3) . . . . ? O7 C10 C11 O8 -69(2) . . . . ? C7 C6 O5 C6 178.2(12) . . . 4 ? C6 C7 O6 C8 -174.1(16) . . . . ? C9 C8 O6 C7 91(3) . . . . ? C8 C9 O7 C10 177.7(17) . . . . ? C11 C10 O7 C9 -179.6(16) . . . . ? C10 C11 O8 C11 177.0(10) . . . 4 ?