#------------------------------------------------------------------------------ #$Date: 2019-11-12 04:50:09 +0200 (Tue, 12 Nov 2019) $ #$Revision: 227616 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/03/33/4033363.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_4033363 loop_ _publ_author_name 'Druzhenko, Tetiana' 'Skalenko, Yevhen' 'Samoilenko, Maryna' 'Denisenko, Aleksandr' 'Zozulya, Sergey' 'Borysko, Petro O.' 'Sokolenko, Maria I.' 'Tarasov, Alexandr' 'Mykhailiuk, Pavel K.' _publ_section_title ; Photochemical Synthesis of 2-Azabicyclo[3.2.0]heptanes: Advanced Building Blocks for Drug Discovery. Synthesis of 2,3-Ethanoproline. ; _journal_issue 3 _journal_name_full 'The Journal of organic chemistry' _journal_page_first 1394 _journal_page_last 1401 _journal_paper_doi 10.1021/acs.joc.7b02910 _journal_volume 83 _journal_year 2018 _chemical_formula_sum 'C12 H16 Cl N' _chemical_formula_weight 209.71 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 90 _cell_angle_beta 107.210(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.1849(4) _cell_length_b 7.5306(3) _cell_length_c 13.9062(6) _cell_measurement_reflns_used 1391 _cell_measurement_temperature 273(2) _cell_measurement_theta_max 22.6 _cell_measurement_theta_min 3.8 _cell_volume 1118.86(8) _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 273(2) _diffrn_detector_area_resol_mean 16.1827 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0507 _diffrn_reflns_av_unetI/netI 0.0439 _diffrn_reflns_Laue_measured_fraction_full 0.991 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 7240 _diffrn_reflns_point_group_measured_fraction_full 0.991 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 24.999 _diffrn_reflns_theta_max 24.999 _diffrn_reflns_theta_min 3.067 _diffrn_source 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.302 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.910 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_density_diffrn 1.245 _exptl_crystal_description plate _exptl_crystal_F_000 448 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.100 _refine_diff_density_max 0.279 _refine_diff_density_min -0.201 _refine_diff_density_rms 0.040 _refine_ls_extinction_coef 0.006(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2014' _refine_ls_goodness_of_fit_ref 1.145 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 136 _refine_ls_number_reflns 1948 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.145 _refine_ls_R_factor_all 0.0596 _refine_ls_R_factor_gt 0.0426 _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^)+(0.0579P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1104 _refine_ls_wR_factor_ref 0.1287 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1492 _reflns_number_total 1948 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jo7b02910_si_002.cif _cod_data_source_block tolm297 _cod_depositor_comments 'Adding full bibliography for 4033361--4033363.cif.' _cod_database_code 4033363 _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 0.942 _shelx_estimated_absorpt_t_max 0.970 _shelx_hkl_file ; 0 0 2 1356.43 47.12 0 0 -3 0.89 0.80 0 0 -3 1.78 0.82 0 0 3 -0.69 0.71 0 0 3 1.47 0.73 0 0 -4 3109.18 109.47 0 0 -4 3199.60 107.66 0 0 -5 0.27 0.74 0 0 -5 -0.32 0.58 0 0 -6 756.89 32.59 0 0 -6 820.68 35.61 0 0 -7 0.22 0.72 0 0 -7 -0.50 1.58 0 0 -8 100.43 10.54 0 0 -8 97.66 8.85 0 0 -9 0.29 1.20 0 0 -9 0.70 0.98 0 0 -10 228.34 16.42 0 0 -10 252.17 19.83 0 0 -11 -1.49 1.35 0 0 -11 3.06 2.84 0 0 -12 8.75 3.18 0 0 -12 8.40 3.70 0 0 -13 -0.22 0.78 0 0 -13 0.45 2.41 0 0 -13 -3.00 2.40 0 0 -14 15.41 5.79 0 0 -14 11.31 4.03 0 0 -14 17.41 6.25 0 0 -15 -0.42 2.70 0 0 -15 -0.07 1.03 0 0 -16 1.98 1.62 0 0 -17 -0.17 1.63 0 0 -18 11.39 6.31 0 1 -18 1.49 2.61 0 1 -17 -1.28 2.66 0 1 -17 0.15 1.59 0 1 -16 12.12 5.52 0 1 -16 7.29 5.04 0 1 -15 0.79 0.65 0 1 -15 -2.69 2.20 0 1 -14 14.89 4.90 0 1 -14 10.13 4.73 0 1 -13 45.55 7.92 0 1 -13 44.77 9.32 0 1 -12 18.60 4.89 0 1 -12 18.94 5.67 0 1 -11 0.01 1.46 0 1 -11 -1.01 1.75 0 1 -10 328.73 21.37 0 1 -10 309.62 22.60 0 1 -9 107.52 10.59 0 1 -9 85.63 10.48 0 1 -8 89.45 9.15 0 1 -8 89.31 9.87 0 1 -7 22.71 4.30 0 1 -7 22.08 4.11 0 1 -6 1320.80 54.14 0 1 -6 1381.33 53.64 0 1 -5 975.86 40.35 0 1 -5 1002.88 40.35 0 1 -4 22.83 3.33 0 1 -4 28.14 3.69 0 1 -3 2.26 0.57 0 1 -3 1.68 0.80 0 1 -2 474.33 18.65 0 -1 2 451.58 18.56 0 -1 2 444.34 19.14 0 1 2 467.56 17.95 0 1 2 434.37 18.12 0 1 2 428.50 19.12 0 1 2 431.37 18.84 0 -1 -2 486.25 19.58 0 -1 -2 470.18 18.35 0 -1 -2 478.87 18.02 0 1 3 2.06 0.94 0 -1 -3 2.84 1.09 0 1 3 2.61 0.79 0 -1 -3 4.99 1.29 0 -1 -3 2.17 1.05 0 -1 -4 28.49 3.55 0 1 4 25.76 3.00 0 -1 -4 27.45 4.01 0 -1 -4 29.99 3.20 0 -1 -4 23.38 3.71 0 -1 -5 979.65 41.60 0 -1 -5 974.69 41.14 0 -1 -5 1004.49 40.00 0 -1 -5 1010.18 38.23 0 -1 -6 1289.32 54.24 0 -1 -6 1356.19 52.27 0 -1 -6 1313.69 50.13 0 -1 -6 1327.32 54.03 0 -1 -7 23.72 4.89 0 -1 -7 21.14 3.95 0 -1 -7 15.98 3.23 0 -1 -7 21.64 4.67 0 -1 -8 92.03 8.40 0 -1 -8 108.92 11.25 0 -1 -8 97.10 10.77 0 -1 -9 94.34 10.97 0 -1 -9 87.25 10.83 0 -1 -9 90.85 8.71 0 -1 -10 327.25 23.22 0 -1 -10 303.62 18.88 0 -1 -10 299.29 23.09 0 -1 -11 1.63 1.31 0 -1 -11 1.79 0.93 0 -1 -11 0.99 1.87 0 -1 -12 27.04 6.75 0 -1 -12 22.66 6.25 0 -1 -12 24.35 5.22 0 -1 -13 51.79 10.10 0 -1 -13 33.18 6.09 0 -1 -14 25.58 7.98 0 -1 -15 -0.92 2.23 0 -1 -16 10.87 4.99 0 -1 -17 0.51 3.91 0 -1 -18 -0.63 2.45 0 2 -18 4.66 3.98 0 2 -17 10.69 5.26 0 2 -16 -0.71 2.24 0 2 -16 7.27 4.40 0 2 -15 24.30 6.70 0 2 -15 21.25 7.00 0 2 -14 -0.14 1.75 0 2 -14 0.96 0.92 0 2 -13 24.08 6.41 0 2 -13 11.75 4.90 0 2 -12 23.26 6.31 0 2 -12 17.67 5.39 0 2 -11 49.63 8.71 0 2 -11 53.59 8.58 0 2 -10 33.59 6.55 0 2 -10 41.69 7.34 0 2 -9 11.12 3.59 0 2 -9 19.84 5.23 0 2 -8 146.65 12.93 0 2 -8 122.87 12.00 0 2 -7 46.90 6.67 0 2 -7 40.16 6.02 0 2 -6 200.60 13.90 0 2 -6 203.77 14.63 0 2 -5 50.76 6.46 0 2 -5 56.78 6.24 0 2 -4 930.95 38.83 0 2 -4 878.13 36.76 0 2 -3 567.42 24.21 0 2 -2 157.81 10.46 0 2 -2 165.95 9.33 0 2 -1 493.46 22.28 0 -2 0 4596.40 158.17 0 2 0 5079.91 162.42 0 2 1 507.78 18.30 0 2 1 483.25 22.09 0 2 2 147.52 9.61 0 2 3 593.23 26.56 0 -2 -3 606.82 27.34 0 -2 -3 584.81 25.08 0 -2 -4 924.05 39.56 0 -2 -4 931.72 37.24 0 -2 -5 41.15 4.58 0 -2 -5 46.80 5.31 0 -2 -5 55.88 6.81 0 -2 -6 193.82 14.91 0 -2 -6 204.07 12.44 0 -2 -6 207.93 13.50 0 -2 -7 44.45 5.88 0 -2 -7 48.33 7.26 0 -2 -7 42.64 5.28 0 -2 -8 142.60 13.78 0 -2 -8 147.56 11.01 0 -2 -8 141.88 12.26 0 -2 -9 10.07 2.70 0 -2 -9 22.22 4.46 0 -2 -9 13.60 4.37 0 -2 -10 38.31 7.59 0 -2 -10 33.33 5.37 0 -2 -11 47.65 9.08 0 -2 -11 50.18 6.93 0 -2 -12 21.06 4.66 0 -2 -12 22.26 6.56 0 -2 -13 18.66 6.77 0 -2 -14 6.08 3.53 0 -2 -15 25.76 8.16 0 -2 -16 -0.20 2.05 0 -2 -17 14.73 6.45 0 -2 -18 3.07 3.08 0 3 -18 0.50 1.86 0 3 -17 0.21 1.74 0 3 -16 22.02 7.42 0 3 -16 10.58 4.96 0 3 -15 1.60 1.81 0 3 -15 0.31 1.78 0 3 -14 2.07 2.31 0 3 -14 0.93 1.45 0 3 -13 86.48 12.66 0 3 -13 71.21 11.41 0 3 -12 21.53 6.12 0 3 -12 14.86 5.01 0 3 -11 -0.36 1.18 0 3 -11 0.51 1.26 0 3 -10 22.27 5.52 0 3 -10 18.28 5.06 0 3 -9 185.15 15.85 0 3 -9 175.07 16.22 0 3 -8 18.45 4.61 0 3 -8 21.47 5.38 0 3 -7 6.37 2.80 0 3 -7 9.57 2.67 0 3 -6 10.83 2.79 0 3 -6 11.80 3.98 0 3 -5 347.69 19.66 0 3 -5 379.47 22.58 0 3 -4 42.08 5.18 0 3 -3 1012.30 41.32 0 3 -3 1061.53 44.64 0 3 -2 599.05 28.62 0 3 -1 73.55 7.83 0 -3 0 0.16 0.46 0 3 0 2.36 0.89 0 3 1 79.48 7.86 0 3 2 647.60 28.78 0 3 2 581.59 21.83 0 -3 -3 988.67 40.89 0 3 3 1018.39 42.92 0 -3 -4 43.07 5.38 0 3 4 44.48 6.12 0 -3 -5 333.18 18.97 0 3 5 365.86 21.28 0 -3 -5 372.66 22.48 0 -3 -6 10.18 2.85 0 -3 -6 8.29 2.70 0 3 6 8.51 2.94 0 -3 -7 5.53 2.05 0 -3 -7 2.92 1.99 0 -3 -8 24.59 5.02 0 -3 -8 26.28 5.87 0 -3 -9 202.51 15.89 0 -3 -9 176.15 13.21 0 -3 -9 193.39 17.89 0 -3 -10 13.57 3.48 0 -3 -10 8.56 3.28 0 -3 -10 13.53 4.95 0 -3 -11 -0.53 1.24 0 -3 -11 1.66 2.13 0 -3 -11 -0.52 1.09 0 -3 -12 23.28 6.48 0 -3 -12 14.78 3.86 0 -3 -13 90.06 14.19 0 -3 -14 4.29 3.50 0 -3 -15 -0.43 2.94 0 -3 -16 22.88 7.72 0 -3 -17 2.03 2.83 0 -3 -18 3.92 5.08 0 4 -18 3.53 3.66 0 4 -17 0.79 1.18 0 4 -17 0.95 2.31 0 4 -16 0.76 1.70 0 4 -16 0.65 1.41 0 4 -15 22.64 7.42 0 4 -15 24.60 7.49 0 4 -14 -2.02 2.38 0 4 -14 -0.33 1.98 0 4 -13 1.17 1.10 0 4 -13 0.02 1.01 0 4 -12 10.88 4.45 0 4 -12 7.95 4.46 0 4 -11 432.13 29.41 0 4 -11 426.75 30.74 0 4 -10 15.78 4.60 0 4 -10 13.10 4.77 0 4 -9 40.54 8.01 0 4 -9 40.07 7.20 0 4 -8 8.33 3.41 0 4 -8 6.20 2.36 0 4 -7 236.03 19.38 0 4 -7 234.98 17.34 0 4 -6 4.36 2.31 0 4 -6 3.67 2.36 0 4 -5 96.72 9.48 0 4 -5 92.57 11.13 0 4 -4 14.52 4.02 0 4 -4 13.18 3.18 0 4 -3 108.13 11.08 0 4 -3 102.74 9.12 0 4 -2 135.80 12.24 0 4 -1 261.01 17.95 0 4 0 503.32 27.49 0 4 1 236.21 16.70 0 4 2 170.15 13.92 0 4 3 101.36 10.47 0 4 3 84.98 4.82 0 4 4 11.81 1.63 0 -4 -4 14.05 3.23 0 4 4 18.88 4.53 0 4 5 104.38 11.12 0 -4 -5 101.69 9.75 0 4 6 4.55 2.43 0 -4 -6 4.71 2.02 0 4 7 256.45 19.69 0 -4 -7 261.37 17.92 0 -4 -8 4.02 2.05 0 4 8 11.67 4.25 0 -4 -9 46.41 8.83 0 4 9 36.20 7.23 0 -4 -9 34.61 6.52 0 -4 -10 17.36 5.31 0 -4 -10 11.29 3.99 0 4 10 10.77 3.81 0 -4 -11 423.81 32.08 0 -4 -11 429.83 27.88 0 4 11 407.79 29.83 0 -4 -12 7.23 3.41 0 4 12 16.92 5.25 0 -4 -12 14.14 4.66 0 -4 -13 -0.21 1.12 0 -4 -13 5.00 3.66 0 4 13 2.37 2.58 0 4 14 -1.99 3.15 0 -4 -14 3.05 3.95 0 4 15 23.85 7.43 0 -4 -15 31.52 9.38 0 4 16 -2.39 2.66 0 -4 -16 -1.56 3.46 0 4 17 1.05 3.13 0 -4 -17 3.75 3.22 0 4 18 -5.52 3.90 0 5 -17 3.33 3.85 0 5 -16 -2.30 3.53 0 5 -16 3.83 3.61 0 5 -15 -0.60 1.94 0 5 -15 -1.16 2.57 0 5 -14 1.73 2.13 0 5 -14 -0.55 1.13 0 5 -13 5.97 3.26 0 5 -13 9.58 4.50 0 5 -12 10.12 4.79 0 5 -12 2.71 2.00 0 5 -11 -1.51 2.54 0 5 -11 1.81 1.74 0 5 -10 1.23 2.72 0 5 -10 6.54 3.20 0 5 -9 25.68 5.82 0 5 -9 15.00 5.82 0 5 -8 25.02 5.55 0 5 -8 23.96 5.91 0 5 -7 73.76 9.35 0 5 -7 61.85 10.30 0 5 -6 147.56 15.90 0 5 -6 147.56 13.38 0 5 -5 60.97 7.84 0 5 -4 145.12 14.79 0 5 -4 140.00 12.24 0 5 -3 547.69 31.22 0 5 -3 476.48 26.10 0 5 -2 27.34 5.87 0 5 -1 538.82 31.26 0 5 0 -2.69 2.43 0 5 1 454.38 27.97 0 5 2 35.65 6.70 0 5 3 530.24 31.07 0 5 4 139.90 14.14 0 -5 -4 134.29 12.50 0 5 5 42.97 3.11 0 5 5 56.90 8.88 0 -5 -5 61.90 8.20 0 -5 -6 137.16 12.57 0 5 6 155.77 15.25 0 5 7 52.11 9.27 0 -5 -7 77.63 9.58 0 -5 -8 20.43 4.85 0 5 8 29.74 6.97 0 -5 -9 18.60 4.73 0 5 9 17.53 5.68 0 -5 -10 1.80 1.37 0 5 10 1.23 2.32 0 5 11 -1.37 1.28 0 -5 -11 0.61 0.53 0 5 12 5.15 2.74 0 -5 -12 2.15 1.78 0 5 13 3.15 2.25 0 5 14 -5.23 3.46 0 5 15 0.77 2.16 0 5 16 2.61 3.14 0 5 17 2.17 2.07 0 6 -16 -5.75 4.11 0 6 -15 0.60 1.66 0 6 -14 -1.06 2.39 0 6 -13 5.33 3.79 0 6 -13 0.48 1.77 0 6 -12 11.62 4.91 0 6 -12 24.74 7.74 0 6 -11 11.72 4.80 0 6 -11 15.29 5.70 0 6 -10 10.29 4.20 0 6 -10 10.25 4.98 0 6 -9 1.62 2.01 0 6 -9 -2.40 1.65 0 6 -8 90.19 13.55 0 6 -8 78.18 10.71 0 6 -7 112.38 14.97 0 6 -7 112.75 12.42 0 6 -6 103.78 11.50 0 6 -6 109.85 14.62 0 6 -5 3.61 2.11 0 6 -5 2.65 3.00 0 6 -4 92.09 10.39 0 6 -4 101.44 13.38 0 6 -3 52.74 8.96 0 6 -3 64.44 8.43 0 6 -2 130.47 14.58 0 6 -1 1.40 2.67 0 6 0 393.97 27.94 0 6 1 1.12 1.49 0 6 2 144.71 15.69 0 6 3 64.47 9.97 0 6 4 114.69 13.82 0 -6 -4 90.22 10.98 0 6 5 4.99 2.85 0 -6 -5 3.97 2.67 0 -6 -6 105.28 12.01 0 6 6 105.19 13.62 0 6 7 109.92 14.26 0 -6 -7 102.52 12.04 0 6 8 83.32 12.51 0 -6 -8 70.95 10.15 0 6 9 1.39 2.47 0 -6 -9 -0.95 2.06 0 6 10 7.69 3.26 0 -6 -10 4.07 2.06 0 -6 -11 10.41 4.61 0 6 11 18.43 6.56 0 6 12 6.88 3.20 0 6 13 10.00 5.76 0 6 14 -1.78 1.88 0 6 15 4.47 3.19 0 6 16 -2.95 3.80 0 7 -14 -3.16 1.89 0 7 -13 7.09 4.65 0 7 -12 1.07 1.80 0 7 -11 -2.74 2.14 0 7 -10 17.42 6.54 0 7 -9 1.22 1.97 0 7 -9 3.45 2.97 0 7 -8 -0.28 0.69 0 7 -8 1.37 2.26 0 7 -7 1.57 2.03 0 7 -7 7.09 3.94 0 7 -6 80.12 13.33 0 7 -6 80.13 10.57 0 7 -5 -0.84 1.46 0 7 -5 -1.39 1.47 0 7 -5 1.24 2.26 0 7 -4 9.95 3.42 0 7 -4 22.66 7.15 0 7 -3 2.47 1.20 0 7 -3 2.18 3.06 0 7 -2 95.85 13.40 0 7 -1 70.05 11.69 0 7 0 1.26 3.08 0 7 1 67.43 11.69 0 7 2 97.01 13.68 0 7 3 3.68 2.76 0 7 4 14.55 5.37 0 -7 -4 15.02 4.78 0 7 5 -2.85 2.38 0 -7 -5 -0.06 1.02 0 -7 -6 83.23 11.40 0 7 6 61.44 11.31 0 7 7 3.39 2.80 0 -7 -7 2.60 1.62 0 -7 -8 -1.92 1.06 0 7 8 -1.70 1.72 0 7 9 4.01 3.06 0 -7 -9 -0.27 1.23 0 7 10 16.91 6.61 0 7 11 -0.06 1.03 0 7 12 -0.41 1.97 0 7 13 0.66 2.59 0 7 14 0.17 3.21 0 7 15 0.67 1.53 0 8 -12 6.50 4.75 0 8 -11 -2.50 1.05 0 8 -10 35.50 10.00 0 8 -9 -0.78 1.47 0 8 -8 -0.48 1.42 0 8 -7 -0.60 2.46 0 8 -6 4.30 3.91 0 8 -5 15.53 6.55 0 8 -5 5.31 4.68 0 8 -4 61.17 9.70 0 8 -4 99.97 15.24 0 8 -3 -0.13 1.30 0 8 -3 -2.29 2.29 0 8 -2 28.24 7.84 0 8 -1 12.53 4.96 0 8 0 445.06 34.43 0 8 1 5.47 4.23 0 8 2 45.92 10.28 0 8 3 3.88 2.78 0 8 4 76.52 13.03 0 -8 -4 77.33 11.80 0 8 5 12.36 5.28 0 -8 -5 7.03 3.14 0 -8 -6 -0.13 1.20 0 8 6 -0.15 1.01 0 8 7 4.69 3.99 0 -8 -7 1.30 2.29 0 8 8 -1.87 2.89 0 -8 -8 -1.25 2.08 0 8 9 1.16 2.79 0 8 10 27.31 9.11 0 8 11 5.89 5.32 0 8 12 7.49 5.40 0 8 13 1.45 2.34 0 9 -9 -0.46 1.12 0 9 -8 4.20 4.91 0 9 -7 -0.94 0.73 0 9 -6 32.59 9.89 0 9 -5 33.90 9.59 0 9 -4 49.32 11.61 0 9 -4 49.44 11.38 0 9 -3 -1.35 4.01 0 9 -2 -11.06 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1.81 -15 -1 -1 -0.74 2.16 -15 -1 -1 1.19 2.08 -15 -1 -2 -4.75 3.66 15 2 -12 -4.99 3.84 15 2 -11 7.34 4.95 -15 -2 10 5.79 4.77 15 2 -10 5.91 4.54 15 2 -9 -5.66 3.80 -15 -2 9 -0.78 1.81 -15 -2 8 2.98 3.61 -15 -2 7 10.48 5.46 -15 -2 6 -1.49 2.05 -15 -2 5 -2.91 2.99 -15 -2 4 -0.48 1.65 -15 -2 3 -2.62 3.01 -15 -2 2 -0.06 0.52 -15 -2 2 -0.33 1.40 -15 -2 1 5.47 3.57 -15 -2 1 1.21 2.24 -15 -2 0 7.59 5.51 -15 -2 -1 -7.05 4.46 -15 -2 -2 -1.12 1.04 15 3 -12 -0.29 1.39 15 3 -11 2.62 2.92 15 3 -10 3.68 3.20 -15 -3 10 1.03 1.70 -15 -3 9 2.45 2.26 -15 -3 8 1.67 1.20 -15 -3 7 0.75 1.29 -15 -3 6 0.70 0.73 -15 -3 5 -2.60 2.69 -15 -3 3 0.16 1.62 -15 -3 2 3.83 4.39 -15 -3 1 4.05 3.26 -15 -3 0 -1.69 3.29 15 4 -11 0.91 0.61 -15 -4 4 -1.86 2.11 -15 -4 3 -2.31 3.09 -15 -4 2 5.60 4.68 -15 -4 1 -0.49 2.57 -15 -5 5 1.07 1.44 16 -1 -10 -3.86 3.32 16 0 -10 -2.15 1.68 16 0 -9 -0.22 1.33 -16 0 6 0.29 0.96 -16 0 5 -0.04 1.16 -16 0 4 2.61 2.70 16 1 -11 0.57 2.16 16 1 -10 0.51 1.25 -16 -1 7 1.84 2.54 -16 -1 6 1.76 2.02 -16 -1 5 1.33 1.98 -16 -1 4 7.09 5.43 -16 -1 3 4.10 3.50 -16 -1 2 1.07 2.62 -16 -2 7 2.71 2.43 -16 -2 6 -0.23 1.52 -16 -2 5 -1.82 2.77 -16 -2 4 2.10 2.89 -16 -2 3 5.08 4.53 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 36248 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 0.44063(5) 0.81342(7) 0.61397(4) 0.0584(3) Uani 1 1 d . . N1 N 0.39759(16) 0.4290(3) 0.67343(15) 0.0479(5) Uani 1 1 d . . H1NA H 0.4132(18) 0.551(3) 0.6635(16) 0.051(6) Uiso 1 1 d . . H1NB H 0.442(2) 0.395(3) 0.7364(16) 0.054(6) Uiso 1 1 d . . C1 C 0.26080(17) 0.3985(3) 0.66028(15) 0.0447(5) Uani 1 1 d . . C2 C 0.2345(2) 0.2067(3) 0.69003(19) 0.0568(6) Uani 1 1 d . . H2A H 0.3097 0.1375 0.7192 0.068 Uiso 1 1 calc R U H2B H 0.1792 0.2018 0.7321 0.068 Uiso 1 1 calc R U C3 C 0.1697(3) 0.1634(3) 0.5797(2) 0.0716(8) Uani 1 1 d . . H3A H 0.0800 0.1470 0.5646 0.086 Uiso 1 1 calc R U H3B H 0.2072 0.0643 0.5547 0.086 Uiso 1 1 calc R U C4 C 0.2063(2) 0.3456(3) 0.54693(17) 0.0565(6) Uani 1 1 d . . H4 H 0.1349 0.4181 0.5094 0.068 Uiso 1 1 calc R U C5 C 0.3161(2) 0.3486(4) 0.50383(19) 0.0689(7) Uani 1 1 d . . H5A H 0.3092 0.2533 0.4556 0.083 Uiso 1 1 calc R U H5B H 0.3197 0.4609 0.4706 0.083 Uiso 1 1 calc R U C6 C 0.4307(2) 0.3242(3) 0.59314(19) 0.0592(6) Uani 1 1 d . . H6A H 0.4442 0.2000 0.6116 0.071 Uiso 1 1 calc R U H6B H 0.5048 0.3714 0.5797 0.071 Uiso 1 1 calc R U C7 C 0.20756(17) 0.5477(3) 0.70666(15) 0.0443(5) Uani 1 1 d . . C8 C 0.2487(2) 0.5700(3) 0.81116(17) 0.0557(6) Uani 1 1 d . . H8 H 0.3103 0.4953 0.8502 0.067 Uiso 1 1 calc R U C9 C 0.1996(2) 0.7000(3) 0.8568(2) 0.0637(7) Uani 1 1 d . . H9 H 0.2284 0.7135 0.9264 0.076 Uiso 1 1 calc R U C10 C 0.1070(2) 0.8119(3) 0.7999(2) 0.0676(7) Uani 1 1 d . . H10 H 0.0722 0.8988 0.8310 0.081 Uiso 1 1 calc R U C11 C 0.0672(2) 0.7928(3) 0.6967(2) 0.0673(7) Uani 1 1 d . . H11 H 0.0058 0.8682 0.6580 0.081 Uiso 1 1 calc R U C12 C 0.1174(2) 0.6632(3) 0.65061(18) 0.0548(6) Uani 1 1 d . . H12 H 0.0904 0.6530 0.5808 0.066 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 0.0657(4) 0.0467(4) 0.0576(4) 0.0012(2) 0.0102(3) -0.0088(2) N1 0.0463(9) 0.0417(12) 0.0555(12) 0.0046(9) 0.0149(9) 0.0013(8) C1 0.0415(10) 0.0410(12) 0.0495(12) 0.0009(9) 0.0103(9) -0.0012(8) C2 0.0572(12) 0.0411(14) 0.0717(15) 0.0033(10) 0.0183(12) -0.0013(10) C3 0.0744(16) 0.0583(17) 0.0780(18) -0.0166(13) 0.0161(14) -0.0151(12) C4 0.0580(13) 0.0533(15) 0.0534(13) -0.0048(11) 0.0089(11) 0.0003(10) C5 0.0850(17) 0.0675(17) 0.0583(15) -0.0078(12) 0.0277(14) -0.0023(13) C6 0.0624(13) 0.0493(15) 0.0739(15) -0.0037(11) 0.0326(12) 0.0035(10) C7 0.0430(10) 0.0371(12) 0.0531(12) 0.0012(9) 0.0147(9) -0.0034(8) C8 0.0597(13) 0.0518(15) 0.0537(14) 0.0007(10) 0.0139(11) 0.0048(10) C9 0.0732(15) 0.0612(17) 0.0587(15) -0.0064(11) 0.0226(12) 0.0007(12) C10 0.0689(15) 0.0545(17) 0.0883(19) -0.0145(13) 0.0371(15) 0.0024(11) C11 0.0534(13) 0.0573(16) 0.088(2) 0.0045(13) 0.0163(13) 0.0145(11) C12 0.0488(11) 0.0546(15) 0.0561(14) 0.0032(10) 0.0078(10) 0.0049(10) 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' 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 C6 N1 C1 107.17(17) C7 C1 N1 110.60(16) C7 C1 C2 116.74(18) N1 C1 C2 112.05(17) C7 C1 C4 122.47(17) N1 C1 C4 103.93(17) C2 C1 C4 89.06(17) C3 C2 C1 90.12(18) C2 C3 C4 91.05(17) C5 C4 C3 116.6(2) C5 C4 C1 105.93(18) C3 C4 C1 89.26(17) C6 C5 C4 105.22(19) N1 C6 C5 102.25(18) C12 C7 C8 118.1(2) C12 C7 C1 122.9(2) C8 C7 C1 119.05(18) C9 C8 C7 121.0(2) C8 C9 C10 120.3(2) C11 C10 C9 119.2(2) C12 C11 C10 120.6(2) C11 C12 C7 120.9(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance N1 C6 1.500(3) N1 C1 1.504(3) C1 C7 1.503(3) C1 C2 1.555(3) C1 C4 1.564(3) C2 C3 1.525(3) C3 C4 1.540(3) C4 C5 1.518(3) C5 C6 1.509(3) C7 C12 1.384(3) C7 C8 1.399(3) C8 C9 1.368(3) C9 C10 1.387(3) C10 C11 1.378(4) C11 C12 1.376(3) 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 H1NA Cl1 0.95(2) 2.14(3) 3.087(2) 170.0(18) . N1 H1NB Cl1 0.91(2) 2.19(2) 3.099(2) 177(2) 2_646 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 N1 C1 C7 -157.24(18) C6 N1 C1 C2 70.6(2) C6 N1 C1 C4 -24.1(2) C7 C1 C2 C3 121.0(2) N1 C1 C2 C3 -110.1(2) C4 C1 C2 C3 -5.40(18) C1 C2 C3 C4 5.48(18) C2 C3 C4 C5 102.0(2) C2 C3 C4 C1 -5.45(18) C7 C1 C4 C5 126.3(2) N1 C1 C4 C5 0.4(2) C2 C1 C4 C5 -112.15(19) C7 C1 C4 C3 -116.2(2) N1 C1 C4 C3 117.85(19) C2 C1 C4 C3 5.35(18) C3 C4 C5 C6 -74.2(2) C1 C4 C5 C6 23.1(2) C1 N1 C6 C5 38.6(2) C4 C5 C6 N1 -37.5(2) N1 C1 C7 C12 114.6(2) C2 C1 C7 C12 -115.7(2) C4 C1 C7 C12 -8.4(3) N1 C1 C7 C8 -66.6(2) C2 C1 C7 C8 63.1(2) C4 C1 C7 C8 170.48(19) C12 C7 C8 C9 1.2(3) C1 C7 C8 C9 -177.7(2) C7 C8 C9 C10 0.4(4) C8 C9 C10 C11 -1.4(4) C9 C10 C11 C12 0.7(4) C10 C11 C12 C7 0.9(4) C8 C7 C12 C11 -1.9(3) C1 C7 C12 C11 177.0(2)