#------------------------------------------------------------------------------ #$Date: 2019-11-11 20:25:40 +0200 (Mon, 11 Nov 2019) $ #$Revision: 227260 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/03/58/4035841.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_4035841 loop_ _publ_author_name 'Skalenko, Yevhen A.' 'Druzhenko, Tetiana V.' 'Denisenko, Aleksandr V.' 'Samoilenko, Maryna V.' 'Dacenko, Oleksandr P.' 'Trofymchuk, Serhii A.' 'Grygorenko, Oleksandr O.' 'Tolmachev, Andrey A.' 'Mykhailiuk, Pavel K.' _publ_section_title ; [2+2]-Photocycloaddition of N-Benzylmaleimide to Alkenes As an Approach to Functional 3-Azabicyclo[3.2.0]heptanes. ; _journal_issue 12 _journal_name_full 'The Journal of organic chemistry' _journal_page_first 6275 _journal_page_last 6289 _journal_paper_doi 10.1021/acs.joc.8b00077 _journal_volume 83 _journal_year 2018 _chemical_formula_sum 'C13 H12 Cl N O4 S' _chemical_formula_weight 313.75 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 90 _cell_angle_beta 120.993(14) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 29.204(3) _cell_length_b 5.9824(6) _cell_length_c 18.1623(17) _cell_measurement_reflns_used 1647 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 22.1 _cell_measurement_theta_min 3.5 _cell_volume 2720.1(6) _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 16.1827 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.986 _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0678 _diffrn_reflns_av_unetI/netI 0.0656 _diffrn_reflns_Laue_measured_fraction_full 0.989 _diffrn_reflns_Laue_measured_fraction_max 0.986 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 13070 _diffrn_reflns_point_group_measured_fraction_full 0.989 _diffrn_reflns_point_group_measured_fraction_max 0.986 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.999 _diffrn_reflns_theta_min 2.944 _diffrn_source 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.446 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.657 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.532 _exptl_crystal_description plate _exptl_crystal_F_000 1296 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.030 _refine_diff_density_max 0.385 _refine_diff_density_min -0.408 _refine_diff_density_rms 0.059 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.917 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 181 _refine_ls_number_reflns 3923 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.917 _refine_ls_R_factor_all 0.1087 _refine_ls_R_factor_gt 0.0566 _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^)+(0.0726P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1378 _refine_ls_wR_factor_ref 0.1657 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2063 _reflns_number_total 3923 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jo8b00077_si_002.cif _cod_data_source_block 12a _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 4035841 _shelx_shelxl_version_number 2014/7 _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 0.916 _shelx_estimated_absorpt_t_max 0.987 _shelx_hkl_file ; 0 0 3 -0.77 0.72 0 0 3 0.11 0.32 0 0 -3 0.06 0.18 0 0 -3 0.28 0.17 0 0 4 658.45 22.06 0 0 -4 567.38 18.61 0 0 -4 601.04 19.65 0 0 4 658.32 19.49 0 0 4 668.11 21.92 0 0 5 0.02 0.87 0 0 5 0.22 0.73 0 0 6 49.31 5.76 0 0 6 50.48 5.75 0 0 7 0.42 1.11 0 0 7 0.50 0.19 0 0 8 178.15 12.93 0 0 8 171.42 12.80 0 0 9 2.05 1.38 0 0 9 2.28 1.92 0 0 10 53.20 7.64 0 0 -10 57.49 7.94 0 0 10 46.24 7.20 0 0 11 -0.63 0.87 0 0 11 0.84 0.71 0 0 12 11.27 3.70 0 0 12 15.46 4.81 0 0 -12 17.18 4.85 0 0 -13 0.36 1.64 0 0 13 -0.34 1.86 0 0 13 0.91 1.57 0 0 14 56.89 9.61 0 0 -14 61.32 10.60 0 0 14 49.36 8.85 0 0 15 -4.09 2.43 0 0 15 -1.42 2.44 0 0 -15 0.03 1.57 0 0 16 -0.93 1.33 0 0 16 -0.26 0.36 0 0 -16 2.26 2.45 0 0 17 2.26 1.91 0 0 17 -0.35 0.58 0 0 -17 -1.95 2.41 0 0 18 22.25 7.16 0 0 -18 19.19 6.93 0 0 19 -3.30 2.56 0 0 -19 6.59 4.52 0 0 20 10.22 5.48 0 0 -20 17.30 6.83 0 0 -21 2.32 1.39 0 0 21 0.01 0.79 0 0 22 -1.44 2.71 2 0 21 -1.09 1.87 2 0 20 3.30 3.07 -2 0 -19 4.70 3.24 2 0 19 1.71 1.85 -2 0 -18 26.62 8.22 2 0 18 28.61 8.33 -2 0 -17 3.17 3.10 2 0 17 3.12 2.85 -2 0 -16 18.43 6.47 2 0 16 12.25 4.96 2 0 16 10.22 4.39 2 0 15 -2.01 1.46 2 0 15 0.78 1.10 -2 0 -15 -0.49 1.15 2 0 14 9.34 4.43 2 0 14 10.84 4.54 -2 0 -14 11.62 4.57 2 0 13 1.75 2.90 2 0 13 3.17 2.01 -2 0 -13 0.13 0.97 -2 0 -12 27.06 6.64 2 0 12 20.85 5.35 2 0 12 27.95 6.14 2 0 11 0.09 0.52 2 0 11 1.60 2.27 -2 0 -11 -0.49 1.41 -2 0 -10 266.88 18.51 2 0 10 233.45 17.48 2 0 10 240.99 17.40 -2 0 -9 0.35 1.44 2 0 9 -1.29 1.24 2 0 9 -1.67 0.83 -2 0 -8 85.25 8.97 2 0 8 75.70 8.43 2 0 8 78.59 8.81 2 0 7 0.43 0.67 2 0 7 0.03 0.46 2 0 6 4.32 1.87 2 0 6 2.38 1.54 2 0 5 0.64 0.25 2 0 5 1.21 0.80 2 0 4 24.30 3.71 2 0 4 22.11 2.60 2 0 4 24.80 3.57 -2 0 -3 1.46 0.87 2 0 3 1.05 1.03 2 0 3 1.49 0.87 2 0 3 1.35 0.71 -2 0 -2 42.68 3.17 2 0 2 47.21 3.96 2 0 2 50.32 3.88 2 0 -3 -0.54 0.23 2 0 -3 0.32 0.30 2 0 -3 0.76 0.38 2 0 -4 461.31 15.29 -2 0 4 520.64 15.47 -2 0 4 526.19 18.35 -2 0 4 546.37 18.00 2 0 -5 -0.60 0.32 -2 0 5 1.13 0.87 -2 0 5 0.31 0.99 -2 0 5 -0.07 0.36 -2 0 6 56.70 4.50 -2 0 6 61.79 6.20 -2 0 6 55.53 5.75 -2 0 7 0.44 0.28 -2 0 7 1.46 0.93 -2 0 7 0.40 0.53 -2 0 8 0.85 0.50 -2 0 8 -0.57 1.21 -2 0 9 0.71 0.70 -2 0 9 1.90 1.45 -2 0 9 0.57 0.61 -2 0 10 859.67 35.59 -2 0 10 818.68 34.37 -2 0 11 2.74 1.70 2 0 -11 -0.57 0.82 -2 0 11 3.39 2.19 -2 0 12 42.98 7.41 -2 0 12 39.61 7.00 2 0 -12 43.35 7.86 2 0 -13 0.88 2.03 -2 0 13 0.45 0.83 -2 0 13 0.47 1.40 -2 0 14 61.55 9.88 -2 0 14 58.65 9.71 2 0 -14 81.96 12.02 -2 0 15 -0.69 0.27 2 0 -15 -0.48 1.53 -2 0 15 2.06 1.53 -2 0 16 1.53 2.76 -2 0 16 0.03 0.65 2 0 -16 1.41 2.01 2 0 -17 -0.62 1.93 -2 0 17 1.25 1.85 -2 0 17 1.10 0.85 2 0 -18 1.04 0.97 -2 0 18 -2.42 2.37 -2 0 19 0.11 1.53 2 0 -19 4.34 3.19 2 0 -20 27.27 8.89 -2 0 20 27.92 8.46 -2 0 21 0.99 2.64 2 0 -21 5.39 4.87 -2 0 22 6.29 4.35 2 0 -22 3.51 2.84 2 0 -23 -3.69 3.48 4 0 20 6.69 4.52 4 0 19 -0.90 1.93 4 0 18 -3.05 4.36 -4 0 -18 -1.33 2.91 4 0 17 -0.83 2.00 -4 0 -17 -1.54 0.51 4 0 16 10.30 4.80 -4 0 -16 8.35 4.36 4 0 16 14.87 5.85 4 0 15 0.54 0.65 4 0 15 2.89 2.60 -4 0 -15 -2.71 3.18 4 0 14 64.77 10.90 -4 0 -14 69.88 11.53 4 0 14 63.05 10.93 4 0 13 1.84 0.39 4 0 13 -1.99 1.64 -4 0 -13 -0.50 1.75 -4 0 -12 9.09 3.70 4 0 12 7.78 3.04 4 0 12 8.36 4.01 4 0 11 0.62 0.41 4 0 11 -0.74 0.91 -4 0 -11 -0.90 1.04 4 0 10 95.91 10.90 -4 0 -10 118.43 12.01 4 0 10 92.73 11.04 -4 0 -9 -1.01 1.57 4 0 9 0.68 1.75 4 0 9 0.08 1.22 4 0 8 702.83 31.98 -4 0 -8 789.95 31.91 4 0 8 781.79 32.58 -4 0 -7 0.69 0.96 4 0 7 1.00 1.23 4 0 7 1.88 1.19 4 0 6 514.13 19.90 4 0 6 544.20 23.90 4 0 6 529.81 24.13 4 0 5 0.25 1.32 4 0 5 0.24 0.24 4 0 5 0.02 0.70 4 0 4 213.74 11.86 4 0 4 195.54 9.84 4 0 4 195.95 11.95 4 0 3 -1.03 0.81 4 0 3 0.37 0.72 4 0 3 0.49 0.42 4 0 2 871.27 27.22 4 0 2 877.23 26.51 4 0 2 843.37 25.20 4 0 1 0.38 0.42 4 0 1 0.14 0.30 -4 0 -1 1.42 0.52 4 0 0 74.67 4.19 -4 0 0 63.79 4.37 4 0 -2 1033.72 26.70 4 0 -3 0.45 0.26 4 0 -3 0.19 0.30 -4 0 3 0.20 0.43 4 0 -3 -0.62 0.48 4 0 -4 2543.81 64.59 -4 0 4 2497.71 66.35 -4 0 4 2602.14 64.20 4 0 -4 2636.53 65.70 -4 0 5 0.06 1.96 -4 0 5 1.10 0.95 4 0 -5 -1.23 1.36 -4 0 5 0.39 0.78 -4 0 6 118.20 8.61 4 0 -6 127.25 7.95 -4 0 6 121.73 8.10 -4 0 6 115.51 6.40 4 0 -7 0.34 0.52 -4 0 7 -0.09 0.21 -4 0 7 1.37 1.20 -4 0 7 0.21 0.50 -4 0 8 48.95 5.88 -4 0 8 47.28 4.51 -4 0 8 50.37 6.32 -4 0 9 -1.26 1.04 -4 0 9 0.46 0.90 -4 0 9 -0.06 1.23 -4 0 10 45.15 6.70 -4 0 10 42.64 6.21 -4 0 10 46.45 5.04 -4 0 11 -1.10 1.79 -4 0 11 2.08 1.99 -4 0 11 0.01 0.34 4 0 -11 0.34 1.69 4 0 -12 690.61 33.51 -4 0 12 626.70 31.52 -4 0 12 608.56 30.16 -4 0 13 -1.82 1.97 4 0 -13 0.06 0.23 -4 0 13 0.10 0.64 4 0 -13 1.75 2.05 4 0 -14 52.10 7.25 -4 0 14 38.48 7.42 -4 0 14 39.82 7.85 4 0 -14 43.78 8.50 4 0 -15 -0.54 1.18 4 0 -15 -1.63 1.60 -4 0 15 0.85 2.27 -4 0 15 -0.69 1.82 4 0 -16 2.26 1.69 4 0 -16 1.06 1.14 -4 0 16 2.09 2.50 -4 0 16 -0.26 2.40 -4 0 17 -1.12 1.53 -4 0 17 -1.25 1.85 4 0 -17 2.54 2.67 -4 0 18 3.92 2.78 4 0 -18 8.36 4.73 4 0 -19 1.19 3.56 -4 0 19 -2.40 2.13 4 0 -20 9.51 4.73 -4 0 20 6.16 3.85 -4 0 21 1.47 1.60 4 0 -21 -2.21 2.91 -4 0 22 11.24 5.68 4 0 -22 10.32 5.94 -4 0 23 -0.97 2.59 4 0 -23 0.53 0.96 4 0 -24 -2.92 3.17 6 0 20 3.38 3.22 6 0 19 2.89 2.84 6 0 18 12.83 5.26 6 0 17 -0.28 0.77 -6 0 -16 15.72 5.67 6 0 16 16.16 6.07 6 0 15 -0.64 1.50 -6 0 -15 2.37 2.61 6 0 15 -2.97 2.94 -6 0 -14 31.35 8.04 6 0 14 32.18 7.89 6 0 14 30.84 7.79 6 0 13 -0.96 1.09 6 0 13 -1.81 1.57 -6 0 -13 -0.07 1.51 -6 0 -12 62.59 9.93 6 0 12 69.16 10.69 6 0 12 73.40 10.67 6 0 11 -0.69 0.47 -6 0 -11 0.98 1.70 6 0 11 -1.36 1.59 6 0 10 234.31 18.25 -6 0 -10 241.69 17.95 6 0 10 221.84 18.14 -6 0 -9 -1.12 1.50 6 0 9 -0.71 1.08 6 0 9 0.80 1.06 -6 0 -8 89.43 9.38 6 0 8 89.26 9.92 6 0 8 85.69 9.98 -6 0 -7 0.57 0.51 6 0 7 -0.02 0.19 6 0 7 0.75 0.96 6 0 7 1.79 1.59 -6 0 -6 862.07 30.35 6 0 6 760.56 27.96 6 0 6 768.40 32.44 6 0 6 850.44 32.63 6 0 5 0.83 0.83 6 0 5 -1.06 0.61 6 0 5 1.76 1.34 -6 0 -5 -0.11 0.76 6 0 4 5.72 1.90 -6 0 -4 5.01 1.50 6 0 4 3.18 1.15 6 0 4 4.45 1.48 6 0 3 -0.23 0.48 6 0 3 0.78 0.67 6 0 3 0.66 0.68 -6 0 -3 0.92 0.46 6 0 2 210.42 10.95 -6 0 -2 200.73 7.90 6 0 2 205.16 11.21 6 0 2 189.46 9.83 6 0 1 -0.18 0.76 6 0 1 -0.40 0.67 6 0 0 3590.35 89.09 6 0 0 3579.90 87.82 6 0 -1 0.81 0.48 -6 0 1 0.69 0.38 6 0 -1 0.98 0.61 6 0 -2 365.36 14.18 6 0 -3 0.15 0.21 -6 0 3 0.73 0.55 6 0 -3 -0.84 0.60 -6 0 4 9158.53 211.03 6 0 -4 8767.28 211.12 -6 0 5 0.13 0.22 6 0 -5 -1.10 0.78 6 0 -5 0.72 0.67 6 0 -6 493.31 18.90 -6 0 6 459.09 17.01 -6 0 6 453.11 19.30 -6 0 7 0.50 0.94 -6 0 7 0.81 1.55 -6 0 7 -0.34 0.41 6 0 -7 -1.36 1.54 -6 0 8 28.54 4.23 6 0 -8 25.16 3.89 -6 0 8 30.06 3.45 -6 0 8 24.79 4.40 -6 0 9 -0.23 0.20 6 0 -9 -0.38 0.69 -6 0 9 0.55 0.52 -6 0 10 133.13 11.81 6 0 -10 131.02 10.23 -6 0 10 127.37 8.36 -6 0 10 137.96 11.09 -6 0 11 0.09 0.27 -6 0 11 -0.74 0.25 6 0 -11 -0.41 0.74 -6 0 11 0.47 1.00 6 0 -12 4.65 1.74 -6 0 12 2.41 1.35 -6 0 12 5.75 2.64 -6 0 12 6.65 2.08 6 0 -12 3.38 2.36 6 0 -13 -0.82 1.10 -6 0 13 0.91 1.00 -6 0 13 -0.42 1.78 6 0 -13 2.21 2.47 -6 0 13 0.16 0.96 6 0 -14 2.51 2.48 6 0 -14 0.21 0.66 -6 0 14 2.12 1.80 -6 0 14 4.04 2.78 -6 0 15 0.15 0.80 -6 0 15 -1.20 1.96 6 0 -15 0.10 0.52 6 0 -15 -1.40 2.38 -6 0 16 2.21 2.82 -6 0 16 -0.39 0.39 6 0 -16 0.18 1.96 6 0 -16 0.47 1.66 6 0 -17 2.79 2.36 -6 0 17 -0.07 1.26 -6 0 17 -0.66 1.92 -6 0 18 26.12 7.40 6 0 -18 29.64 8.26 6 0 -19 1.73 2.81 -6 0 19 -0.78 2.19 6 0 -20 1.84 1.99 -6 0 20 -1.33 2.34 -6 0 21 4.35 3.48 6 0 -21 0.96 1.58 -6 0 22 8.61 5.06 6 0 -22 7.03 3.58 -6 0 23 -3.63 3.63 6 0 -23 1.80 2.49 6 0 -24 3.37 3.26 8 0 19 1.10 2.52 8 0 18 -1.63 2.43 8 0 17 -1.01 2.20 8 0 16 0.16 1.38 8 0 15 -1.20 1.59 8 0 15 -1.35 1.70 -8 0 -14 0.60 1.33 8 0 14 -1.23 2.20 8 0 14 0.07 1.23 8 0 13 1.79 3.18 -8 0 -13 -2.11 2.40 8 0 13 -1.00 0.19 -8 0 -12 13.27 4.16 8 0 12 11.74 4.54 8 0 12 13.51 4.67 -8 0 -11 -0.84 0.70 8 0 11 0.39 0.99 8 0 11 -1.77 1.70 -8 0 -10 485.84 26.49 8 0 10 436.99 26.69 8 0 10 438.48 27.49 8 0 9 -0.69 2.12 -8 0 -9 1.26 1.50 8 0 9 0.68 0.73 8 0 8 180.86 15.81 -8 0 -8 202.71 14.54 8 0 8 194.24 15.66 8 0 8 185.93 12.73 8 0 7 -1.95 1.82 -8 0 -7 0.36 1.01 8 0 7 -3.22 1.81 8 0 7 -0.79 0.29 8 0 6 760.70 31.64 -8 0 -6 774.36 28.47 8 0 6 721.67 31.80 8 0 6 690.63 27.39 8 0 5 0.47 0.53 8 0 5 0.70 0.83 -8 0 -5 0.12 0.51 8 0 5 0.71 1.34 8 0 4 13.49 3.21 -8 0 -4 13.37 2.44 8 0 4 13.57 2.86 8 0 4 11.12 3.00 8 0 3 -0.16 0.30 8 0 3 -0.49 0.24 -8 0 -3 0.34 0.49 8 0 2 292.22 14.57 8 0 2 286.67 14.32 -8 0 -2 260.55 9.60 8 0 2 269.13 13.26 8 0 1 -0.27 0.31 8 0 1 -0.51 0.62 8 0 1 0.57 0.56 8 0 0 620.30 22.07 8 0 0 618.58 21.00 8 0 -1 0.32 0.44 8 0 -1 2.08 0.72 -8 0 1 1.01 0.62 -8 0 2 2.60 0.72 8 0 -2 2.70 0.58 8 0 -2 2.43 0.59 8 0 -2 3.37 1.10 8 0 -3 0.91 1.24 -8 0 3 0.37 0.34 8 0 -4 5064.46 127.09 -8 0 4 5164.86 123.83 8 0 -5 -0.25 1.27 8 0 -5 0.35 0.18 8 0 -6 403.49 17.47 -8 0 6 375.67 13.32 8 0 -6 337.30 13.00 -8 0 7 0.79 0.69 8 0 -7 1.65 0.73 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0.08 2.10 25 7 -8 1.67 1.70 25 7 -9 1.08 1.81 25 7 -10 10.12 6.08 18 -8 -7 2.93 3.05 18 -8 -6 -0.41 0.94 16 -8 -9 -3.28 3.29 16 -8 -8 1.79 1.84 16 -8 -7 -0.17 0.53 16 -8 -6 -0.23 1.24 16 -8 -5 1.50 2.68 -16 8 5 1.70 1.13 16 -8 -4 -1.02 1.78 -16 8 4 -0.15 1.27 16 -8 -3 -0.78 1.38 -16 8 3 2.29 3.02 -16 8 2 0.74 1.51 -16 8 1 2.15 2.95 14 -8 -9 0.02 1.65 14 -8 -8 1.03 1.83 14 -8 -7 0.22 0.75 -14 8 7 -1.28 3.49 14 -8 -6 3.12 3.93 -14 8 6 5.86 4.86 14 -8 -5 0.67 2.05 -14 8 5 -3.82 3.50 14 -8 -4 3.06 3.27 -14 8 4 2.62 3.51 14 -8 -3 -0.75 0.74 -14 8 3 -0.74 2.62 14 -8 -2 -0.23 2.20 -14 8 2 1.56 2.32 14 -8 -1 -0.10 2.30 -14 8 1 -1.68 2.29 12 -8 -10 -6.70 4.88 12 -8 -9 5.45 4.78 12 -8 -8 0.25 1.59 -12 8 8 2.78 3.64 12 -8 -7 0.71 2.01 -12 8 7 -2.26 3.84 12 -8 -6 -2.39 3.82 -12 8 6 1.98 2.21 12 -8 -5 2.99 3.70 -12 8 5 2.53 3.23 12 -8 -4 1.28 0.20 -12 8 4 -1.21 1.13 12 -8 -3 3.18 3.43 -12 8 3 9.84 5.85 12 -8 -2 0.90 0.31 -12 8 2 2.61 2.67 12 -8 -1 0.90 0.28 -12 8 1 -7.24 4.65 12 -8 0 -3.69 3.32 -12 8 0 -0.32 1.29 10 -8 -8 4.39 1.23 -10 8 8 7.70 5.15 10 -8 -7 4.60 4.36 -10 8 7 1.14 2.34 10 -8 -6 -0.74 1.65 -10 8 6 2.49 4.32 10 -8 -5 -0.74 3.22 -10 8 5 -3.77 3.33 10 -8 -4 -3.27 3.22 -10 8 4 -2.68 3.14 10 -8 -3 0.14 1.94 -10 8 3 3.08 2.67 10 -8 -2 4.24 3.47 -10 8 2 -1.64 3.29 10 -8 -1 1.43 0.74 -10 8 1 0.30 2.55 10 -8 0 2.96 2.62 -10 8 0 -1.65 2.28 10 -8 1 -1.50 2.23 10 -8 2 3.86 4.02 -8 8 8 -0.93 1.01 8 -8 -7 0.25 1.82 -8 8 7 0.83 1.27 8 -8 -6 -3.97 4.51 -8 8 6 -1.48 2.44 8 -8 -5 0.82 2.13 -8 8 5 -1.05 3.23 8 -8 -4 4.21 3.83 -8 8 4 3.57 3.46 8 -8 -3 1.07 2.20 -8 8 3 -2.07 3.05 8 -8 -2 3.81 3.85 -8 8 2 -2.58 3.43 8 -8 -1 0.53 0.70 -8 8 1 0.13 0.76 8 -8 0 -2.30 3.17 -8 8 0 4.21 3.67 8 -8 1 1.09 0.53 8 -8 2 5.12 3.38 8 -8 3 -0.49 1.41 -6 8 8 4.94 4.66 -6 8 7 0.45 1.56 6 -8 -6 6.98 6.02 -6 8 6 8.59 5.48 6 -8 -5 1.23 1.64 -6 8 5 4.68 3.50 6 -8 -4 1.44 3.11 -6 8 4 6.32 4.95 6 -8 -3 4.87 3.84 -6 8 3 -0.66 2.35 6 -8 -2 -2.05 2.58 -6 8 2 -1.93 3.26 6 -8 -1 -0.83 1.96 -6 8 1 -1.68 1.08 6 -8 0 1.57 2.94 -6 8 0 4.47 3.51 6 -8 1 1.08 2.60 6 -8 2 -1.17 0.41 6 -8 3 -0.13 1.52 6 -8 4 1.96 2.92 -4 8 8 5.97 4.50 -4 8 7 -1.96 2.80 -4 8 6 4.64 2.89 4 -8 -5 -1.08 2.95 -4 8 5 -0.61 2.19 4 -8 -4 6.77 4.50 -4 8 4 3.10 1.71 4 -8 -3 2.39 2.82 -4 8 3 -1.03 2.29 4 -8 -2 3.00 4.45 -4 8 2 -2.89 3.94 4 -8 -1 5.12 3.94 -4 8 1 3.99 3.65 4 -8 0 -0.71 1.35 -4 8 0 -1.00 2.25 4 -8 1 -2.75 2.51 -4 8 -1 -0.31 0.81 4 -8 2 -2.74 2.63 4 -8 2 -5.35 3.98 4 -8 3 0.98 1.55 4 -8 4 3.63 2.62 4 -8 5 0.28 1.10 -2 8 8 0.08 1.83 -2 8 7 -3.11 2.99 -2 8 6 5.49 3.85 -2 8 5 0.82 2.64 2 -8 -4 4.29 4.02 -2 8 4 3.26 3.22 2 -8 -3 -1.12 3.00 -2 8 3 2.52 1.49 2 -8 -2 -1.51 2.98 -2 8 2 3.79 3.10 2 -8 -1 3.02 2.97 -2 8 1 7.45 4.75 2 -8 0 1.73 2.61 -2 8 0 -1.42 2.74 2 -8 1 1.54 3.64 -2 8 -1 -0.27 1.98 2 -8 2 9.82 5.96 2 -8 3 -4.69 3.52 2 -8 3 4.39 3.16 2 -8 4 -1.71 2.12 2 -8 4 -5.22 3.96 2 -8 5 -2.57 2.60 2 -8 5 -1.21 0.89 2 -8 6 0.49 1.32 2 -8 6 1.81 0.65 0 8 7 -5.85 4.09 0 8 6 1.28 1.59 0 8 5 1.36 2.57 0 8 4 6.14 3.55 0 -8 -3 2.58 4.12 0 8 3 1.97 2.62 0 -8 -2 -2.05 3.18 0 8 2 -0.15 2.03 0 -8 -1 6.99 5.35 0 8 1 2.24 2.80 0 -8 0 2.54 2.87 0 8 0 2.50 2.78 0 -8 1 4.55 3.27 0 8 -1 1.61 2.47 0 -8 2 -0.91 1.46 0 -8 3 0.05 2.51 0 -8 4 5.21 4.31 0 -8 4 3.71 2.98 0 -8 5 -2.12 3.62 0 -8 5 1.65 3.45 0 -8 6 -2.66 2.71 0 -8 6 4.42 4.04 0 -8 7 -1.08 1.76 0 -8 7 -2.08 3.86 0 -8 8 -4.66 3.68 0 -8 9 -1.79 2.31 0 -8 10 1.02 1.70 2 8 7 -2.83 1.99 2 8 6 4.43 3.52 2 8 5 1.16 2.07 2 8 4 -0.99 2.39 2 8 3 -2.19 2.39 -2 -8 -2 11.16 6.46 2 8 2 22.81 7.60 -2 -8 -1 8.09 5.89 2 8 1 -0.16 2.10 -2 -8 0 5.48 4.37 2 8 0 -0.28 1.62 -2 -8 1 -2.37 2.10 2 8 -1 -0.06 0.99 -2 -8 2 0.81 1.97 -2 -8 3 1.47 2.59 -2 -8 4 0.16 1.35 -2 -8 5 4.72 3.61 -2 -8 5 7.62 4.93 -2 -8 6 1.70 1.16 -2 -8 6 -1.69 2.22 -2 -8 7 0.14 1.65 -2 -8 7 -2.76 2.77 -2 -8 8 -1.28 1.95 -2 -8 9 2.44 2.87 -2 -8 10 0.75 1.58 -2 -8 11 1.63 1.59 4 8 6 8.99 6.18 4 8 5 -0.66 2.34 4 8 4 1.22 2.79 4 8 3 0.57 1.06 4 8 2 -4.48 3.01 -4 -8 -1 1.46 2.34 4 8 1 -2.32 3.33 -4 -8 0 3.76 3.44 4 8 0 1.13 1.22 -4 -8 1 4.72 2.70 4 8 -1 3.19 2.03 -4 -8 2 1.91 2.93 -4 -8 3 3.61 3.96 -4 -8 4 1.27 1.11 -4 -8 5 -1.64 2.30 -4 -8 5 2.92 3.98 -4 -8 6 1.02 1.70 -4 -8 6 3.47 3.41 -4 -8 7 1.96 2.54 -4 -8 7 3.28 3.82 -4 -8 8 0.51 2.43 -4 -8 8 -2.13 0.94 -4 -8 9 0.62 1.57 -4 -8 10 0.21 1.17 -4 -8 11 1.02 1.89 6 8 5 -1.10 2.84 6 8 4 2.14 3.30 6 8 3 0.35 1.72 6 8 2 0.70 1.74 6 8 1 0.07 1.94 -6 -8 0 1.98 1.88 6 8 0 2.07 1.90 -6 -8 1 -0.86 2.45 6 8 -1 -0.21 1.93 -6 -8 2 -2.02 4.81 -6 -8 3 -8.03 5.10 -6 -8 4 0.64 3.19 -6 -8 5 0.32 1.36 -6 -8 6 1.29 1.68 -6 -8 6 6.53 3.95 -6 -8 7 -4.18 3.63 -6 -8 7 0.22 2.08 -6 -8 8 0.42 2.17 -6 -8 8 -2.17 2.60 -6 -8 9 3.06 3.41 -6 -8 9 -4.25 3.70 -6 -8 10 0.08 1.14 8 8 4 -0.48 2.99 8 8 3 -3.22 3.10 8 8 2 8.16 4.99 8 8 1 -1.61 2.24 -8 -8 0 1.32 3.24 8 8 0 20.88 7.07 -8 -8 1 4.81 4.15 8 8 -1 0.19 0.84 -8 -8 2 -2.88 4.43 -8 -8 3 2.77 3.70 -8 -8 4 2.67 1.98 -8 -8 5 -1.18 2.22 -8 -8 6 -5.82 4.37 -8 -8 6 -4.84 3.89 -8 -8 7 6.28 4.22 -8 -8 7 2.81 3.83 -8 -8 8 -6.99 4.79 -8 -8 8 1.76 2.84 -8 -8 9 -6.51 4.64 -8 -8 9 3.14 3.00 -8 -8 10 1.95 2.94 10 8 3 -6.72 4.27 10 8 2 -1.68 2.24 10 8 1 -3.42 2.96 10 8 0 2.16 1.75 10 8 -1 1.77 2.26 -10 -8 1 -1.76 4.55 -10 -8 2 -4.90 4.14 -10 -8 3 3.04 2.42 -10 -8 4 3.58 2.89 10 8 -4 4.15 2.65 -10 -8 5 0.98 0.82 -10 -8 6 3.96 3.28 -10 -8 7 -1.06 1.94 -10 -8 7 2.49 3.33 -10 -8 8 -2.48 3.76 -10 -8 8 -0.56 1.84 -10 -8 9 3.79 3.40 -10 -8 9 -0.11 2.00 -10 -8 10 0.74 1.15 -12 -8 1 -0.56 1.72 -12 -8 2 -0.51 1.35 -12 -8 3 1.02 0.76 -12 -8 4 -1.59 1.62 -12 -8 5 2.14 2.38 12 8 -5 2.69 1.73 -12 -8 6 -3.46 3.36 12 8 -6 0.91 1.62 -12 -8 7 -4.13 4.48 -12 -8 7 0.81 2.00 12 8 -7 -2.57 2.73 -12 -8 8 -1.85 3.59 -12 -8 8 -1.56 2.67 12 8 -8 0.28 1.92 -12 -8 9 12.56 5.85 12 8 -9 2.50 2.74 -12 -8 10 3.53 3.82 -14 -8 2 1.76 2.69 -14 -8 3 3.17 4.62 -14 -8 4 1.74 1.51 -14 -8 5 1.62 2.62 14 8 -6 4.30 3.17 -14 -8 6 0.29 1.04 14 8 -7 0.14 1.04 -14 -8 7 0.43 0.66 -14 -8 8 0.79 0.65 14 8 -8 -0.92 2.22 -14 -8 9 -4.47 3.76 14 8 -9 2.58 3.70 -14 -8 10 -2.91 3.03 -16 -8 2 3.38 3.74 -16 -8 3 2.63 3.32 -16 -8 4 2.47 2.73 -16 -8 5 -3.17 3.33 -16 -8 6 2.31 2.93 16 8 -7 2.91 3.07 -16 -8 7 -2.44 2.83 16 8 -8 3.04 3.15 -16 -8 8 0.55 2.74 -16 -8 9 1.86 2.12 -16 -8 10 1.57 2.53 -18 -8 4 1.71 2.51 -18 -8 5 -3.17 3.37 -18 -8 6 -0.08 1.36 -18 -8 7 1.46 0.44 18 8 -8 -0.68 2.60 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 63343 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' 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 Cl1 Cl 0.04612(3) 0.23849(16) 0.05768(5) 0.0841(3) Uani 1 1 d . . S1 S 0.08125(2) 0.44540(11) 0.15924(4) 0.0523(2) Uani 1 1 d . . O1 O 0.26041(8) 0.0293(3) 0.45573(12) 0.0668(5) Uani 1 1 d . . O2 O 0.25377(7) 0.6219(3) 0.29392(11) 0.0630(5) Uani 1 1 d . . O3 O 0.08379(8) 0.6595(3) 0.12899(13) 0.0732(6) Uani 1 1 d . . O4 O 0.05558(8) 0.4172(4) 0.20671(13) 0.0737(6) Uani 1 1 d . . N1 N 0.26903(8) 0.3238(4) 0.38348(12) 0.0476(5) Uani 1 1 d . . C1 C 0.15071(11) 0.1127(4) 0.26498(16) 0.0545(6) Uani 1 1 d . . H1A H 0.1714 -0.0030 0.2578 0.065 Uiso 1 1 calc R U H1B H 0.1167 0.0548 0.2537 0.065 Uiso 1 1 calc R U C2 C 0.18245(9) 0.2421(4) 0.35161(14) 0.0476(6) Uani 1 1 d . . H2 H 0.1640 0.2560 0.3837 0.057 Uiso 1 1 calc R U C3 C 0.23995(10) 0.1787(4) 0.40449(15) 0.0485(6) Uani 1 1 d . . C4 C 0.23786(10) 0.4821(4) 0.32369(14) 0.0464(5) Uani 1 1 d . . C5 C 0.18131(10) 0.4525(4) 0.30301(15) 0.0447(5) Uani 1 1 d . . H5 H 0.1650 0.5844 0.3124 0.054 Uiso 1 1 calc R U C6 C 0.14599(9) 0.3292(4) 0.21626(14) 0.0474(5) Uani 1 1 d . . H6 H 0.1629 0.3186 0.1817 0.057 Uiso 1 1 calc R U C7 C 0.32559(9) 0.2950(4) 0.41515(15) 0.0518(6) Uani 1 1 d . . H7A H 0.3325 0.3398 0.3704 0.062 Uiso 1 1 calc R U H7B H 0.3343 0.1376 0.4266 0.062 Uiso 1 1 calc R U C8 C 0.36200(10) 0.4261(4) 0.49563(15) 0.0460(5) Uani 1 1 d . . C9 C 0.41245(10) 0.3458(5) 0.55301(16) 0.0592(7) Uani 1 1 d . . H9 H 0.4232 0.2088 0.5428 0.071 Uiso 1 1 calc R U C10 C 0.44708(12) 0.4667(6) 0.6253(2) 0.0781(9) Uani 1 1 d . . H10 H 0.4807 0.4100 0.6641 0.094 Uiso 1 1 calc R U C11 C 0.43176(12) 0.6707(6) 0.63993(19) 0.0767(9) Uani 1 1 d . . H11 H 0.4553 0.7539 0.6880 0.092 Uiso 1 1 calc R U C12 C 0.38204(12) 0.7510(5) 0.58380(18) 0.0640(7) Uani 1 1 d . . H12 H 0.3716 0.8887 0.5940 0.077 Uiso 1 1 calc R U C13 C 0.34735(10) 0.6303(5) 0.51237(16) 0.0539(6) Uani 1 1 d . . H13 H 0.3135 0.6868 0.4747 0.065 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 0.0684(5) 0.0982(6) 0.0651(5) -0.0196(4) 0.0197(4) -0.0060(4) S1 0.0453(4) 0.0570(4) 0.0528(4) 0.0024(3) 0.0240(3) -0.0008(3) O1 0.0753(13) 0.0639(12) 0.0684(12) 0.0260(10) 0.0421(11) 0.0217(10) O2 0.0600(11) 0.0709(12) 0.0549(10) 0.0116(9) 0.0274(9) -0.0085(10) O3 0.0633(12) 0.0605(12) 0.0827(14) 0.0182(10) 0.0283(11) 0.0038(9) O4 0.0637(12) 0.0928(16) 0.0813(13) -0.0034(11) 0.0492(11) 0.0000(11) N1 0.0462(11) 0.0566(12) 0.0427(10) 0.0022(9) 0.0248(9) 0.0052(9) C1 0.0579(15) 0.0449(13) 0.0586(15) 0.0011(11) 0.0285(12) -0.0026(12) C2 0.0511(14) 0.0516(14) 0.0478(13) 0.0072(10) 0.0309(11) 0.0042(11) C3 0.0602(15) 0.0500(13) 0.0446(12) 0.0018(11) 0.0336(11) 0.0077(12) C4 0.0495(13) 0.0517(13) 0.0383(11) 0.0019(10) 0.0227(10) 0.0000(11) C5 0.0495(13) 0.0441(13) 0.0450(12) 0.0043(10) 0.0276(11) 0.0051(10) C6 0.0490(13) 0.0542(14) 0.0441(12) 0.0042(11) 0.0276(11) 0.0012(11) C7 0.0463(13) 0.0628(15) 0.0508(14) -0.0015(12) 0.0283(11) 0.0070(12) C8 0.0446(12) 0.0549(14) 0.0446(12) 0.0021(11) 0.0273(10) 0.0021(11) C9 0.0563(15) 0.0679(17) 0.0529(14) 0.0031(13) 0.0278(12) 0.0189(13) C10 0.0507(16) 0.104(3) 0.0600(17) -0.0086(17) 0.0144(14) 0.0165(17) C11 0.0621(18) 0.097(2) 0.0586(17) -0.0241(17) 0.0222(15) -0.0027(17) C12 0.0683(18) 0.0644(17) 0.0663(17) -0.0106(14) 0.0396(15) 0.0026(14) C13 0.0527(14) 0.0575(15) 0.0525(14) 0.0048(12) 0.0279(12) 0.0116(12) 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' S S 0.1246 0.1234 '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 O3 S1 O4 119.76(14) O3 S1 C6 109.33(12) O4 S1 C6 109.85(12) O3 S1 Cl1 107.83(10) O4 S1 Cl1 107.82(10) C6 S1 Cl1 100.50(9) C4 N1 C3 113.3(2) C4 N1 C7 123.4(2) C3 N1 C7 123.0(2) C6 C1 C2 89.59(18) C3 C2 C5 105.3(2) C3 C2 C1 114.2(2) C5 C2 C1 90.08(17) O1 C3 N1 122.8(2) O1 C3 C2 129.3(2) N1 C3 C2 107.9(2) O2 C4 N1 125.4(2) O2 C4 C5 126.5(2) N1 C4 C5 108.2(2) C4 C5 C2 104.96(19) C4 C5 C6 112.28(19) C2 C5 C6 90.00(17) C1 C6 C5 90.03(17) C1 C6 S1 114.96(18) C5 C6 S1 111.03(17) N1 C7 C8 114.3(2) C13 C8 C9 118.3(2) C13 C8 C7 122.0(2) C9 C8 C7 119.7(2) C10 C9 C8 120.7(3) C11 C10 C9 119.9(3) C12 C11 C10 119.8(3) C11 C12 C13 120.4(3) C12 C13 C8 120.9(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Cl1 S1 2.0096(10) S1 O3 1.411(2) S1 O4 1.414(2) S1 C6 1.765(2) O1 C3 1.204(3) O2 C4 1.211(3) N1 C4 1.374(3) N1 C3 1.398(3) N1 C7 1.453(3) C1 C6 1.534(3) C1 C2 1.560(3) C2 C3 1.492(3) C2 C5 1.528(3) C4 C5 1.504(3) C5 C6 1.555(3) C7 C8 1.511(3) C8 C13 1.379(3) C8 C9 1.381(3) C9 C10 1.379(4) C10 C11 1.372(5) C11 C12 1.362(4) C12 C13 1.370(4) 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 C6 C1 C2 C3 -111.0(2) C6 C1 C2 C5 -4.08(19) C4 N1 C3 O1 -180.0(2) C7 N1 C3 O1 6.0(4) C4 N1 C3 C2 1.5(3) C7 N1 C3 C2 -172.6(2) C5 C2 C3 O1 176.7(2) C1 C2 C3 O1 -86.1(3) C5 C2 C3 N1 -4.8(2) C1 C2 C3 N1 92.4(2) C3 N1 C4 O2 -178.0(2) C7 N1 C4 O2 -4.0(4) C3 N1 C4 C5 2.7(3) C7 N1 C4 C5 176.6(2) O2 C4 C5 C2 175.2(2) N1 C4 C5 C2 -5.5(2) O2 C4 C5 C6 78.9(3) N1 C4 C5 C6 -101.8(2) C3 C2 C5 C4 6.1(2) C1 C2 C5 C4 -109.1(2) C3 C2 C5 C6 119.24(19) C1 C2 C5 C6 4.02(18) C2 C1 C6 C5 4.01(18) C2 C1 C6 S1 -109.33(18) C4 C5 C6 C1 102.1(2) C2 C5 C6 C1 -4.09(19) C4 C5 C6 S1 -141.00(17) C2 C5 C6 S1 112.80(17) O3 S1 C6 C1 170.73(18) O4 S1 C6 C1 37.4(2) Cl1 S1 C6 C1 -76.00(18) O3 S1 C6 C5 70.39(19) O4 S1 C6 C5 -62.91(19) Cl1 S1 C6 C5 -176.35(14) C4 N1 C7 C8 92.3(3) C3 N1 C7 C8 -94.3(3) N1 C7 C8 C13 -32.2(3) N1 C7 C8 C9 150.6(2) C13 C8 C9 C10 0.3(4) C7 C8 C9 C10 177.6(3) C8 C9 C10 C11 -1.1(5) C9 C10 C11 C12 1.3(5) C10 C11 C12 C13 -0.6(5) C11 C12 C13 C8 -0.2(4) C9 C8 C13 C12 0.4(4) C7 C8 C13 C12 -176.9(2)