#------------------------------------------------------------------------------ #$Date: 2022-09-28 02:58:06 +0100 (Wed, 28 Sep 2022) $ #$Revision: 278238 $ #$URL: svn://www.crystallography.net/cod/cif/2/24/41/2244183.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2244183 loop_ _publ_author_name 'van der Peet, Phillip L.' 'Joyce, Rohan D.' 'Ott, Holger' 'Marcuccio, Sebastian M.' 'White, Jonathan M.' 'Williams, Spencer J.' _publ_section_title ; Synthesis and structure of clozapine N-oxide hemi(hydrochloride): an infinite hydrogen-bonded poly[n]catenane ; _journal_coeditor_code HB8039 _journal_issue 10 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first ; ; _journal_paper_doi 10.1107/S2056989022009306 _journal_volume 78 _journal_year 2022 _chemical_formula_iupac '2C18 H19 Cl1 N4 O1, H Cl' _chemical_formula_moiety '2(C18 H19 Cl1 N4 O1), H Cl' _chemical_formula_sum 'C36 H39 Cl3 N8 O2' _chemical_formula_weight 722.10 _chemical_name_common ; Clozapine N-oxide hemi(hydrochloride) ; _chemical_name_systematic ;8-Chloro-11-(4-methyl-1-piperazinyl)-5H-dibenzo[b,e][1,4]diazepine N-oxide hemi(hydrochloride) ; _space_group_crystal_system tetragonal _space_group_IT_number 87 _space_group_name_Hall '-I 4' _space_group_name_H-M_alt 'I 4/m' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2016/6 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 17.305(2) _cell_length_b 17.305(2) _cell_length_c 26.040(5) _cell_measurement_reflns_used 5908 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 31.8 _cell_measurement_theta_min 1.4 _cell_volume 7798(2) _computing_cell_refinement ; XDS (Kabsch, 1993) ; _computing_data_collection 'AS QEGUI' _computing_data_reduction ; XDS (Kabsch, 1993) ; _computing_molecular_graphics ; Mercury (Macrae et al., 2020) ; _computing_publication_material ; WINGX (Farrugia, 2012) ; _computing_structure_refinement ; SHELXL2016/6 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 100.00(10) _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.868 _diffrn_measurement_device_type 'ADSC Quantum 210r' _diffrn_measurement_method 'Omega Scan' _diffrn_radiation_monochromator 'Silicon Double Crystal' _diffrn_radiation_source 'MX1 Beamline Australian Synchrotron' _diffrn_radiation_type Synchrotron _diffrn_radiation_wavelength 0.710757 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_unetI/netI 0.0187 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_number 66433 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.773 _diffrn_reflns_theta_min 1.413 _exptl_absorpt_coefficient_mu 0.276 _exptl_absorpt_correction_type none _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.230 _exptl_crystal_description block _exptl_crystal_F_000 3024 _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.807 _refine_diff_density_min -0.491 _refine_ls_extinction_coef 0.0069(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method ; SHELXL2016/6 (Sheldrick 2015b) ; _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 231 _refine_ls_number_reflns 5901 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.032 _refine_ls_R_factor_all 0.0567 _refine_ls_R_factor_gt 0.0491 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0661P)^2^+11.4576P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1333 _refine_ls_wR_factor_ref 0.1384 _reflns_number_gt 5096 _reflns_number_total 5901 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file hb8039sup1.cif _cod_data_source_block I _cod_original_cell_volume 7798(3) _cod_database_code 2244183 _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_hkl_file ; 0 0 6 607.20 13.66 0 0 -6 591.90 13.31 0 0 10 117.50 2.78 0 0 10 118.80 2.78 0 0 -10 130.90 3.07 0 0 -10 129.60 3.01 0 0 12 1105.00 24.83 0 0 -12 1123.00 25.18 0 0 16 623.60 14.12 0 0 16 633.30 14.28 0 0 -16 652.20 14.70 0 0 -16 630.80 14.28 0 0 18 154.20 3.61 0 0 18 145.40 3.48 0 0 -18 150.10 3.58 0 0 -18 148.30 3.47 0 0 20 577.90 13.10 0 0 20 568.30 12.85 0 0 -20 568.70 12.91 0 0 -20 598.60 13.52 0 0 22 28.63 0.91 0 0 22 25.73 0.98 0 0 -22 26.41 0.85 0 0 -22 26.31 0.97 0 0 26 37.55 1.10 0 0 26 37.33 1.20 0 0 -26 38.38 1.12 0 0 -26 37.38 1.18 0 0 28 20.68 0.78 0 0 28 18.22 0.83 0 0 -28 20.43 0.76 0 0 -28 19.97 0.83 0 0 30 3.06 0.64 0 0 30 3.24 0.50 0 0 -30 2.88 0.55 0 0 -30 3.87 0.53 0 0 32 96.85 2.42 0 0 32 98.16 2.37 0 0 -32 96.43 2.35 0 0 -32 93.95 2.30 0 0 34 18.23 0.68 0 0 34 17.74 0.83 0 0 -34 18.79 0.77 0 0 -34 18.71 0.74 -1 0 35 15.30 0.65 1 0 -33 0.78 0.54 1 0 -33 0.75 0.52 -1 0 33 1.27 0.49 -1 0 33 1.03 0.67 1 0 -31 2.98 0.52 1 0 -31 3.74 0.59 -1 0 31 3.52 0.51 -1 0 31 3.51 0.62 1 0 -29 -0.30 0.55 1 0 -29 1.24 0.47 -1 0 29 0.63 0.60 -1 0 29 0.35 0.50 1 0 -27 20.66 0.77 1 0 -27 18.36 0.83 -1 0 27 18.97 0.74 -1 0 27 20.11 0.89 1 0 -25 1.20 0.55 1 0 -25 0.51 0.46 -1 0 25 0.80 0.47 -1 0 25 0.58 0.58 1 0 -23 75.42 1.88 1 0 -23 77.95 2.03 -1 0 23 79.09 1.99 -1 0 23 83.67 2.17 1 0 -21 79.68 2.07 1 0 -21 77.77 1.93 -1 0 21 78.44 2.04 -1 0 21 72.95 1.84 1 0 -19 76.06 1.89 1 0 -19 76.09 1.97 -1 0 19 80.21 1.99 -1 0 19 76.24 1.97 1 0 -17 57.43 1.47 1 0 -17 58.75 1.58 -1 0 17 59.69 1.53 -1 0 17 58.62 1.57 1 0 -15 17.46 0.73 1 0 -15 18.62 0.65 -1 0 15 18.70 0.75 -1 0 15 16.61 0.61 1 0 -13 52.17 1.34 1 0 -13 51.09 1.39 -1 0 13 49.69 1.33 -1 0 13 48.30 1.25 1 0 -11 20.17 0.70 1 0 -11 19.83 0.63 -1 0 11 19.27 0.67 -1 0 11 18.94 0.62 1 0 -9 9.90 0.49 1 0 -9 9.55 0.43 -1 0 9 9.18 0.50 -1 0 9 9.82 0.43 1 0 -7 24.35 0.77 1 0 -7 25.62 0.73 -1 0 7 24.06 0.71 -1 0 7 22.86 0.74 1 0 -3 71.12 1.63 1 0 -3 68.09 1.58 -1 0 3 72.25 1.66 -1 0 3 69.13 1.60 -1 0 1 18.16 0.43 -1 0 1 17.12 0.41 1 0 1 18.17 0.43 1 0 1 18.11 0.44 -1 0 -1 18.42 0.44 -1 0 -1 19.00 0.46 -1 0 -3 77.28 1.78 -1 0 -3 78.46 1.82 1 0 5 597.30 13.42 -1 0 -7 24.44 0.72 -1 0 -7 23.51 0.76 1 0 9 9.21 0.50 1 0 9 8.73 0.42 -1 0 -9 9.38 0.43 -1 0 -9 9.52 0.50 1 0 11 19.60 0.64 1 0 11 18.67 0.68 -1 0 -11 18.75 0.66 -1 0 -11 18.50 0.62 1 0 13 47.91 1.31 1 0 13 45.62 1.19 -1 0 -13 50.66 1.37 -1 0 -13 51.32 1.33 1 0 15 18.17 0.75 1 0 15 17.93 0.65 -1 0 -15 16.74 0.62 -1 0 -15 15.87 0.71 1 0 17 58.26 1.50 1 0 17 58.08 1.57 -1 0 -17 55.84 1.43 -1 0 -17 55.65 1.50 1 0 19 75.49 1.96 1 0 19 77.52 1.94 -1 0 -19 76.49 1.98 -1 0 -19 72.21 1.80 1 0 21 72.67 1.83 1 0 21 73.28 1.93 -1 0 -21 71.64 1.88 -1 0 -21 66.88 1.70 1 0 23 72.57 1.85 1 0 23 78.94 2.07 -1 0 -23 77.25 1.93 -1 0 -23 77.36 2.00 1 0 25 1.50 0.64 1 0 25 0.70 0.45 -1 0 -25 0.20 0.52 -1 0 -25 0.74 0.47 1 0 27 17.85 0.83 1 0 27 18.78 0.72 -1 0 -27 17.88 0.73 -1 0 -27 17.08 0.78 1 0 29 0.17 0.49 1 0 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2 0 -12 141.90 3.30 -2 0 12 151.00 3.50 -2 0 12 139.00 3.28 2 0 -10 85.73 2.04 2 0 -10 90.35 2.19 -2 0 10 91.42 2.20 -2 0 10 88.41 2.10 2 0 -8 240.10 5.46 2 0 -8 248.60 5.68 -2 0 8 250.50 5.69 -2 0 8 235.40 5.38 2 0 -6 37.49 1.00 2 0 -6 35.65 0.92 -2 0 6 36.11 0.93 -2 0 6 37.43 1.00 2 0 -4 79.30 1.85 2 0 -4 82.59 1.90 2 0 -2 51.09 1.19 2 0 -2 52.75 1.22 -2 0 2 50.89 1.19 -2 0 2 49.31 1.14 -2 0 0 107.00 2.42 -2 0 0 111.10 2.51 2 0 2 50.27 1.18 2 0 2 53.61 1.27 -2 0 -2 51.11 1.20 -2 0 -2 54.51 1.29 2 0 4 82.44 1.94 2 0 4 84.04 1.95 -2 0 -4 82.64 1.94 -2 0 -4 77.25 1.80 -2 0 -6 32.97 0.93 -2 0 -6 34.02 0.91 2 0 8 227.60 5.21 2 0 8 230.20 5.25 -2 0 -8 271.00 6.17 -2 0 -10 93.13 2.21 -2 0 -10 87.93 2.12 2 0 12 138.50 3.27 2 0 12 142.20 3.31 -2 0 -12 133.20 3.12 -2 0 -12 138.10 3.26 2 0 14 71.13 1.83 2 0 14 74.90 1.84 -2 0 -14 68.98 1.71 -2 0 -14 70.21 1.81 -2 0 -16 37.38 1.04 -2 0 -16 34.59 1.06 2 0 18 21.13 0.74 2 0 18 20.38 0.82 -2 0 -18 19.31 0.69 -2 0 -18 20.18 0.79 2 0 20 58.48 1.53 2 0 20 61.65 1.65 2 0 22 0.69 0.56 2 0 22 0.73 0.43 -2 0 -22 0.34 0.52 -2 0 -22 0.63 0.42 2 0 24 3.59 0.59 2 0 24 4.20 0.49 -2 0 -24 4.10 0.48 -2 0 -24 3.37 0.56 2 0 26 5.60 0.51 2 0 26 5.01 0.64 -2 0 -26 4.44 0.59 -2 0 -26 6.11 0.53 2 0 28 -0.43 0.47 2 0 28 -0.14 0.58 -2 0 -28 -0.06 0.56 -2 0 -28 -0.54 0.46 2 0 30 12.60 0.64 2 0 30 12.04 0.75 -2 0 -30 13.06 0.68 -2 0 -30 12.93 0.67 -2 0 -32 11.56 0.64 -2 0 -32 12.35 0.65 2 0 34 0.23 0.46 2 0 34 -0.11 0.63 -2 0 -34 0.00 0.50 -2 0 -34 0.44 0.54 -3 0 35 24.15 0.77 -3 0 35 23.19 0.96 3 0 -33 3.48 0.58 3 0 -33 3.22 0.56 -3 0 33 3.53 0.50 -3 0 33 3.21 0.68 3 0 -31 2.28 0.53 3 0 -31 2.23 0.57 3 0 -29 14.68 0.68 3 0 -29 14.10 0.73 -3 0 29 14.90 0.77 -3 0 29 14.66 0.66 -3 0 27 1.71 0.60 -3 0 27 2.74 0.47 3 0 -25 47.82 1.31 3 0 -25 49.09 1.42 -3 0 25 53.17 1.43 -3 0 25 49.76 1.43 3 0 -23 112.00 2.78 3 0 -23 107.90 2.60 -3 0 23 106.70 2.64 -3 0 23 112.20 2.71 3 0 -21 9.64 0.65 3 0 -21 9.97 0.54 -3 0 21 9.94 0.56 -3 0 21 8.85 0.66 3 0 -19 43.29 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3.77 0.40 -3 0 -9 3.15 0.34 3 0 11 148.50 3.44 3 0 11 146.00 3.43 3 0 13 0.28 0.33 3 0 13 -0.29 0.42 -3 0 -13 0.55 0.42 -3 0 -13 0.26 0.35 3 0 15 24.03 0.86 3 0 15 22.69 0.75 -3 0 -15 23.33 0.84 -3 0 -15 24.18 0.76 3 0 17 81.49 2.07 3 0 17 79.85 1.97 -3 0 -17 83.28 2.10 -3 0 -17 79.72 1.96 3 0 19 44.58 1.23 3 0 19 45.34 1.32 -3 0 -19 44.98 1.21 -3 0 -19 47.69 1.36 3 0 21 8.68 0.64 3 0 21 7.74 0.52 -3 0 -21 7.63 0.50 -3 0 -21 7.27 0.61 3 0 23 106.30 2.64 3 0 23 101.40 2.47 -3 0 -23 103.10 2.51 -3 0 -23 108.90 2.66 3 0 25 47.40 1.31 3 0 25 48.30 1.43 -3 0 -25 47.63 1.30 -3 0 -25 47.96 1.36 3 0 27 1.65 0.48 3 0 27 1.95 0.64 -3 0 -27 2.16 0.50 -3 0 -27 2.38 0.56 3 0 29 14.05 0.77 3 0 29 14.21 0.67 -3 0 -29 13.40 0.69 -3 0 -29 13.71 0.65 3 0 31 1.09 0.48 3 0 31 1.87 0.62 -3 0 -31 2.18 0.52 -3 0 -31 1.46 0.52 3 0 33 3.30 0.61 3 0 33 2.81 0.47 -3 0 -33 3.40 0.53 -3 0 -33 2.83 0.50 4 0 -34 2.22 0.61 4 0 -34 1.38 0.52 -4 0 34 0.79 0.66 -4 0 34 1.24 0.49 4 0 -32 32.52 1.03 4 0 -32 29.32 0.97 -4 0 32 30.78 1.08 -4 0 32 31.06 0.94 4 0 -30 3.72 0.57 4 0 -30 3.32 0.56 -4 0 30 2.95 0.50 -4 0 30 3.04 0.61 4 0 -28 3.77 0.54 4 0 -28 4.24 0.59 -4 0 28 3.32 0.63 -4 0 28 4.21 0.51 4 0 -26 -0.08 0.45 4 0 -26 0.43 0.55 -4 0 26 0.80 0.58 -4 0 26 0.39 0.46 4 0 -24 28.18 0.91 4 0 -24 25.90 0.98 -4 0 24 27.19 0.97 -4 0 24 26.29 0.88 4 0 -22 4.17 0.45 4 0 -22 3.94 0.60 -4 0 22 4.06 0.50 -4 0 22 4.70 0.58 4 0 -20 98.51 2.38 4 0 -20 96.70 2.44 -4 0 20 94.87 2.32 -4 0 20 97.77 2.43 4 0 -18 23.29 0.76 4 0 -18 23.61 0.91 -4 0 18 23.13 0.85 -4 0 18 24.00 0.80 4 0 -16 95.02 2.37 4 0 -16 93.79 2.25 -4 0 16 94.37 2.33 -4 0 16 97.61 2.35 4 0 -14 3.35 0.48 4 0 -14 3.33 0.36 -4 0 14 3.05 0.35 -4 0 14 3.06 0.44 4 0 -12 140.20 3.27 4 0 -12 142.70 3.38 -4 0 12 136.90 3.18 -4 0 12 144.60 3.40 4 0 -10 81.41 1.94 4 0 -10 85.91 2.09 -4 0 10 88.92 2.14 -4 0 10 86.13 2.04 -4 0 8 112.60 2.62 -4 0 8 109.00 2.56 4 0 -6 0.21 0.32 4 0 -6 0.15 0.25 -4 0 6 0.26 0.30 -4 0 6 0.39 0.26 4 0 -4 34.89 0.91 4 0 -4 35.12 0.89 -4 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SFAC C H N O CL UNIT 288 312 64 16 24 MERG 2 omit 1 1 2 omit -1 2 1 omit 0 3 3 ABIN EQIV $1 -x, -y+1, z HTAB C15 O1_$1 EQIV $2 -y+1/2, x+1/2, -z+1/2 HTAB C15 N1_$2 EQIV $3 -x+1/2, -y+1/2, -z+1/2 HTAB C15 Cl1_$3 HTAB N1 Cl2 HTAB O1 O1_$1 HTAB O1 N4_$1 FMAP 2 PLAN 20 ACTA conf HTAB 2.00000 BOND $H L.S. 10 WGHT 0.066100 11.457600 EXTI 0.006908 FVAR 0.10294 CL1 5 0.139318 0.044258 0.372925 11.00000 0.04208 0.02417 = 0.04417 0.00663 0.01026 0.00136 CL2 5 0.165342 0.446912 0.500000 10.50000 0.05132 0.03315 = 0.02243 0.00000 0.00000 0.00043 O1 4 0.025587 0.434502 0.135992 11.00000 0.02248 0.03131 = 0.03182 0.00073 -0.00119 -0.00030 N3 3 0.173044 0.390222 0.217285 11.00000 0.02652 0.01995 = 0.02098 -0.00173 -0.00145 -0.00025 N2 3 0.158461 0.301452 0.281566 11.00000 0.02335 0.02254 = 0.02238 -0.00128 0.00015 0.00173 N1 3 0.181608 0.384414 0.379701 11.00000 0.03209 0.02519 = 0.02108 -0.00344 0.00067 0.00061 N4 3 0.103776 0.438104 0.121648 11.00000 0.02625 0.02709 = 0.02097 -0.00034 0.00067 -0.00118 C1 1 0.237125 0.424697 0.350744 11.00000 0.02337 0.02365 = 0.02560 -0.00133 -0.00236 0.00237 C7 1 0.188141 0.366303 0.267799 11.00000 0.02162 0.02194 = 0.02137 -0.00236 -0.00002 0.00246 C2 1 0.242197 0.416958 0.297122 11.00000 0.02192 0.02145 = 0.02492 -0.00154 -0.00179 0.00176 C10 1 0.156450 0.185170 0.329187 11.00000 0.02341 0.02411 = 0.02822 0.00066 0.00253 0.00203 AFIX 43 H10 2 0.150809 0.159189 0.298148 11.00000 -1.20000 AFIX 0 C14 1 0.141570 0.468718 0.211116 11.00000 0.02724 0.02114 = 0.02325 -0.00136 -0.00141 0.00151 AFIX 23 H14A 2 0.170572 0.504443 0.232387 11.00000 -1.20000 H14B 2 0.088144 0.469610 0.222369 11.00000 -1.20000 AFIX 0 C9 1 0.168108 0.265396 0.329318 11.00000 0.02032 0.02357 = 0.02462 0.00055 0.00060 0.00209 C16 1 0.137077 0.358676 0.128836 11.00000 0.02857 0.02555 = 0.02196 -0.00285 0.00088 -0.00014 AFIX 23 H16A 2 0.190585 0.358444 0.117741 11.00000 -1.20000 H16B 2 0.108830 0.322118 0.107741 11.00000 -1.20000 AFIX 0 C15 1 0.146170 0.493989 0.155593 11.00000 0.02641 0.02284 = 0.02412 0.00034 -0.00110 -0.00198 AFIX 23 H15A 2 0.123725 0.545067 0.152003 11.00000 -1.20000 H15B 2 0.199875 0.496810 0.145089 11.00000 -1.20000 AFIX 0 C3 1 0.298229 0.460326 0.270672 11.00000 0.02387 0.02356 = 0.02935 -0.00101 0.00002 0.00104 AFIX 43 H3 2 0.302804 0.454729 0.235282 11.00000 -1.20000 AFIX 0 C11 1 0.153277 0.144415 0.374773 11.00000 0.02859 0.02377 = 0.03486 0.00455 0.00508 0.00301 C5 1 0.339914 0.520048 0.349009 11.00000 0.02752 0.02836 = 0.03920 -0.00526 -0.00714 -0.00193 AFIX 43 H5 2 0.371497 0.554918 0.366272 11.00000 -1.20000 AFIX 0 C8 1 0.176472 0.303428 0.376832 11.00000 0.02584 0.02565 = 0.02447 0.00011 -0.00087 0.00217 C17 1 0.132600 0.333932 0.184700 11.00000 0.02745 0.02298 = 0.02053 -0.00266 -0.00054 -0.00100 AFIX 23 H17A 2 0.078931 0.330314 0.195175 11.00000 -1.20000 H17B 2 0.156037 0.283374 0.188721 11.00000 -1.20000 AFIX 0 C6 1 0.286037 0.476952 0.376058 11.00000 0.02936 0.03043 = 0.02737 -0.00552 -0.00561 0.00163 AFIX 43 H6 2 0.282259 0.482756 0.411475 11.00000 -1.20000 AFIX 0 C4 1 0.346851 0.511279 0.296157 11.00000 0.02333 0.02623 = 0.03869 -0.00138 -0.00062 -0.00195 AFIX 43 H4 2 0.383731 0.539293 0.278039 11.00000 -1.20000 AFIX 0 C13 1 0.171437 0.260472 0.422159 11.00000 0.04938 0.03397 = 0.02238 0.00128 -0.00012 0.00288 AFIX 43 H13 2 0.176053 0.285737 0.453531 11.00000 -1.20000 AFIX 0 C12 1 0.159734 0.181140 0.421622 11.00000 0.04772 0.03266 = 0.02793 0.00696 0.00321 0.00343 AFIX 43 H12 2 0.156323 0.153376 0.452117 11.00000 -1.20000 AFIX 0 C18 1 0.109273 0.462372 0.066692 11.00000 0.04637 0.03684 = 0.02025 0.00332 -0.00004 -0.00163 AFIX 137 H18A 2 0.079973 0.427372 0.045739 11.00000 -1.50000 H18B 2 0.162386 0.461630 0.056060 11.00000 -1.50000 H18C 2 0.088990 0.513702 0.062973 11.00000 -1.50000 AFIX 0 H1 2 0.178922 0.398755 0.411403 11.00000 0.03724 H1A 2 0.000000 0.500000 0.135717 10.50000 0.07738 HKLF 4 REM shelxt_a.res in I4/m REM R1 = 0.0491 for 5096 Fo > 4sig(Fo) and 0.0567 for all 5901 data REM 231 parameters refined using 0 restraints END WGHT 0.0677 10.4026 REM Instructions for potential hydrogen bonds HTAB C15 O1_$1 HTAB C15 N1_$2 HTAB C15 Cl1_$3 HTAB N1 Cl2 HTAB O1 O1_$1 HTAB O1 N4_$1 REM Highest difference peak 0.807, deepest hole -0.491, 1-sigma level 0.065 Q1 1 0.2095 0.4369 0.5000 10.50000 0.05 0.81 Q2 1 0.2409 0.4197 0.3233 11.00000 0.05 0.46 Q3 1 0.1210 0.2832 0.0000 10.50000 0.05 0.43 Q4 1 0.1452 0.4793 0.1822 11.00000 0.05 0.40 Q5 1 0.1378 0.3458 0.1566 11.00000 0.05 0.40 Q6 1 0.1726 0.2830 0.3542 11.00000 0.05 0.35 Q7 1 0.1402 0.0447 0.4044 11.00000 0.05 0.35 Q8 1 0.1652 0.2257 0.3302 11.00000 0.05 0.35 Q9 1 0.1826 0.3418 0.3769 11.00000 0.05 0.34 Q10 1 0.1626 0.2203 0.4204 11.00000 0.05 0.33 Q11 1 0.1433 0.2223 0.0150 11.00000 0.05 0.32 Q12 1 0.3423 0.5192 0.3210 11.00000 0.05 0.32 Q13 1 0.1745 0.2699 0.3951 11.00000 0.05 0.30 Q14 1 0.1353 0.2402 0.0000 10.50000 0.05 0.29 Q15 1 0.3354 0.3569 0.5000 10.50000 0.05 0.27 Q16 1 0.1090 0.4487 0.0936 11.00000 0.05 0.27 Q17 1 0.3452 0.3339 0.5000 10.50000 0.05 0.27 Q18 1 0.1721 0.4453 0.4675 11.00000 0.05 0.27 Q19 1 0.3250 0.4856 0.2878 11.00000 0.05 0.26 Q20 1 0.0292 0.0329 0.5000 10.50000 0.05 0.26 ; _shelx_res_checksum 99554 _shelx_fab_file ; 0 0 6 83.92 0.00 0 0 10 61.09 0.00 0 0 12 44.45 0.00 0 0 16 22.93 0.00 0 0 18 15.36 0.00 0 0 20 10.30 0.00 0 0 22 5.58 0.00 0 0 26 -0.28 0.00 0 0 28 -1.05 0.00 0 0 30 -0.33 0.00 0 0 32 -1.11 0.00 0 0 34 0.19 0.00 0 1 35 -0.63 0.00 0 1 33 -1.19 0.00 0 1 31 -1.96 0.00 0 1 29 -2.50 0.00 0 1 27 -3.33 0.00 0 1 25 -4.20 0.00 0 1 23 -3.76 0.00 0 1 21 -3.84 0.00 0 1 19 -4.53 0.00 0 1 17 -4.34 0.00 0 1 15 -2.87 0.00 0 1 13 1.48 0.00 0 1 11 5.41 0.00 0 1 9 12.51 0.00 0 1 7 14.53 0.00 0 1 3 31.85 0.00 0 1 1 46.87 0.00 0 1 5 12.87 0.00 0 2 34 1.68 0.00 0 2 32 1.87 0.00 0 2 30 2.97 0.00 0 2 28 2.20 0.00 0 2 26 3.09 0.00 0 2 24 3.51 0.00 0 2 22 4.36 0.00 0 2 20 1.93 0.00 0 2 18 -0.14 0.00 0 2 16 0.50 0.00 0 2 14 -1.88 0.00 0 2 12 -4.69 0.00 0 2 10 -7.38 0.00 0 2 8 -12.30 0.00 0 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15 0.56 0.00 4 22 10 -1.64 0.00 4 22 6 -0.79 0.00 4 22 12 -1.58 0.00 4 22 14 -1.50 0.00 4 22 16 -1.18 0.00 4 22 18 -0.80 0.00 5 22 9 2.22 0.00 5 22 7 2.10 0.00 5 22 5 2.36 0.00 5 22 3 2.94 0.00 5 22 1 2.63 0.00 5 22 11 0.81 0.00 5 22 13 0.59 0.00 5 22 15 -0.58 0.00 5 22 17 -0.91 0.00 6 22 8 1.60 0.00 6 22 6 2.35 0.00 6 22 4 1.64 0.00 6 22 0 3.03 0.00 6 22 2 2.61 0.00 6 22 10 2.40 0.00 6 22 12 1.90 0.00 6 22 14 0.97 0.00 7 22 5 -1.69 0.00 7 22 1 -0.74 0.00 7 22 3 -0.84 0.00 7 22 7 -1.22 0.00 7 22 9 0.18 0.00 7 22 11 0.51 0.00 8 22 2 -2.60 0.00 8 22 0 -2.29 0.00 8 22 4 -3.05 0.00 8 22 6 -2.27 0.00 8 22 8 -2.44 0.00 -5 23 14 -0.27 0.00 -5 23 12 0.00 0.00 -5 23 10 0.08 0.00 -4 23 15 -0.23 0.00 -4 23 13 0.45 0.00 -4 23 11 0.97 0.00 -3 23 12 -0.24 0.00 0 23 13 1.25 0.00 1 23 12 0.38 0.00 2 23 11 0.88 0.00 2 23 9 2.04 0.00 2 23 13 1.21 0.00 3 23 10 0.56 0.00 3 23 8 0.05 0.00 3 23 6 0.57 0.00 3 23 12 0.31 0.00 3 23 14 0.20 0.00 4 23 7 -1.24 0.00 4 23 5 -1.86 0.00 4 23 3 -1.43 0.00 4 23 9 -0.09 0.00 4 23 11 -0.62 0.00 4 23 13 -0.03 0.00 4 23 15 -0.47 0.00 5 23 6 -1.49 0.00 5 23 4 -2.58 0.00 5 23 8 -1.92 0.00 5 23 10 -0.46 0.00 5 23 12 -0.36 0.00 6 23 1 1.22 0.00 6 23 3 1.44 0.00 6 23 5 0.56 0.00 6 23 7 0.75 0.00 6 23 9 1.47 0.00 6 23 11 0.99 0.00 7 23 2 0.22 0.00 7 23 4 -0.37 0.00 -3 24 11 0.17 0.00 -3 24 9 -0.12 0.00 -2 24 12 -0.21 0.00 -2 24 10 -0.69 0.00 -1 24 11 0.26 0.00 2 24 8 -0.16 0.00 4 24 4 -4.83 0.00 4 24 6 -3.34 0.00 4 24 8 -2.84 0.00 4 24 10 -0.59 0.00 5 24 1 -1.29 0.00 5 24 3 -1.46 0.00 5 24 5 -2.69 0.00 5 24 7 -2.27 0.00 5 24 9 -0.99 0.00 -1 25 8 -0.17 0.00 0 25 1 -0.73 0.00 1 25 6 0.05 0.00 1 25 2 -3.21 0.00 3 25 2 -0.19 0.00 3 25 6 0.02 0.00 1 1 0 42.10 0.00 -1 3 0 -37.48 0.00 3 3 0 27.48 0.00 0 4 0 -23.09 0.00 -1 5 0 29.41 0.00 1 5 0 -26.10 0.00 0 6 0 17.63 0.00 -7 15 0 -2.78 0.00 16 16 0 -0.99 0.00 -15 17 0 -0.88 0.00 15 17 0 0.01 0.00 -6 20 0 0.96 0.00 1 4 1 -3.91 0.00 0 0 2 132.30 0.00 3 3 2 16.29 0.00 16 16 2 -0.85 0.00 -15 17 2 -0.61 0.00 15 17 2 0.26 0.00 2 3 3 42.91 0.00 1 4 3 -8.73 0.00 0 0 4 105.69 0.00 16 16 4 -0.94 0.00 0 0 8 72.95 0.00 0 0 14 30.66 0.00 0 0 24 0.67 0.00 0 0 0 0.00 0.00 # SQUEEZE RESULTS # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 485 69 ' ' 2 0.000 0.000 0.289 18 1 ' ' 3 0.000 0.000 0.500 190 8 ' ' 4 0.000 0.000 0.711 18 1 ' ' 5 0.500 0.500 0.500 482 69 ' ' 6 0.500 0.500 0.000 186 8 ' ' 7 0.500 0.500 0.211 18 1 ' ' 8 0.500 0.500 0.789 18 1 ' ' _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details (replace by semicolon in column 1 when used as .sqf) TITL shelxt_a.res in I4/m CELL 17.3050 17.3050 26.0400 90.00 90.00 90.00 SPGR I4/m # Solvent Accessible Volume = 1406.0 # Electrons Found in S.A.V. = 156.7 # Note: Atoms in Void as Cxxx and Qxxx all others C101 0.712 0.125-0.001 ! 8.75 eA-3 C102 0.857 0.782 0.019 ! 3.49 eA-3 C103 0.654 0.378 0.474 ! 2.27 eA-3 C104 0.134 0.906-0.003 ! 2.11 eA-3 C105 0.530 0.469 0.001 ! 2.00 eA-3 C106 0.393 0.500-0.003 ! 1.47 eA-3 Q107 0.935 0.297-0.004 ! 0.65 eA-3 (replace by semicolon in column 1 when used as .sqf) ; _shelx_fab_checksum 16807 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 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 _atom_site_disorder_assembly _atom_site_disorder_group Cl Cl1 0.13932(3) 0.04426(2) 0.37292(2) 0.03680(13) Uani d 1 . . Cl Cl2 0.16534(4) 0.44691(3) 0.500000 0.03563(15) Uani d 1 . . O O1 0.02559(6) 0.43450(7) 0.13599(5) 0.0285(2) Uani d 1 . . N N3 0.17304(7) 0.39022(7) 0.21729(5) 0.0225(2) Uani d 1 . . N N2 0.15846(7) 0.30145(7) 0.28157(5) 0.0228(2) Uani d 1 . . N N1 0.18161(8) 0.38441(8) 0.37970(5) 0.0261(3) Uani d 1 . . N N4 0.10378(8) 0.43810(8) 0.12165(5) 0.0248(3) Uani d 1 . . C C1 0.23713(9) 0.42470(8) 0.35074(6) 0.0242(3) Uani d 1 . . C C7 0.18814(8) 0.36630(8) 0.26780(5) 0.0216(3) Uani d 1 . . C C2 0.24220(8) 0.41696(8) 0.29712(6) 0.0228(3) Uani d 1 . . C C10 0.15645(9) 0.18517(9) 0.32919(6) 0.0252(3) Uani d 1 . . H H10 0.150809 0.159189 0.298148 0.030 Uiso calc 1 . . C C14 0.14157(9) 0.46872(8) 0.21112(6) 0.0239(3) Uani d 1 . . H H14A 0.170572 0.504443 0.232387 0.029 Uiso calc 1 . . H H14B 0.088144 0.469610 0.222369 0.029 Uiso calc 1 . . C C9 0.16811(8) 0.26540(8) 0.32932(6) 0.0228(3) Uani d 1 . . C C16 0.13708(9) 0.35868(9) 0.12884(6) 0.0254(3) Uani d 1 . . H H16A 0.190585 0.358444 0.117741 0.030 Uiso calc 1 . . H H16B 0.108830 0.322118 0.107741 0.030 Uiso calc 1 . . C C15 0.14617(9) 0.49399(8) 0.15559(6) 0.0245(3) Uani d 1 . . H H15A 0.123725 0.545067 0.152003 0.029 Uiso calc 1 . . H H15B 0.199875 0.496810 0.145089 0.029 Uiso calc 1 . . C C3 0.29823(9) 0.46033(9) 0.27067(6) 0.0256(3) Uani d 1 . . H H3 0.302804 0.454729 0.235282 0.031 Uiso calc 1 . . C C11 0.15328(9) 0.14442(9) 0.37477(6) 0.0291(3) Uani d 1 . . C C5 0.33991(10) 0.52005(10) 0.34901(7) 0.0317(3) Uani d 1 . . H H5 0.371497 0.554918 0.366272 0.038 Uiso calc 1 . . C C8 0.17647(9) 0.30343(9) 0.37683(6) 0.0253(3) Uani d 1 . . C C17 0.13260(9) 0.33393(8) 0.18470(5) 0.0237(3) Uani d 1 . . H H17A 0.078931 0.330314 0.195175 0.028 Uiso calc 1 . . H H17B 0.156037 0.283374 0.188721 0.028 Uiso calc 1 . . C C6 0.28604(9) 0.47695(10) 0.37606(6) 0.0291(3) Uani d 1 . . H H6 0.282259 0.482756 0.411475 0.035 Uiso calc 1 . . C C4 0.34685(9) 0.51128(9) 0.29616(7) 0.0294(3) Uani d 1 . . H H4 0.383731 0.539293 0.278039 0.035 Uiso calc 1 . . C C13 0.17144(12) 0.26047(10) 0.42216(6) 0.0352(4) Uani d 1 . . H H13 0.176053 0.285737 0.453531 0.042 Uiso calc 1 . . C C12 0.15973(11) 0.18114(10) 0.42162(7) 0.0361(4) Uani d 1 . . H H12 0.156323 0.153376 0.452117 0.043 Uiso calc 1 . . C C18 0.10927(11) 0.46237(11) 0.06669(6) 0.0345(4) Uani d 1 . . H H18A 0.079973 0.427372 0.045739 0.052 Uiso calc 1 . . H H18B 0.162386 0.461630 0.056060 0.052 Uiso calc 1 . . H H18C 0.088990 0.513702 0.062973 0.052 Uiso calc 1 . . H H1 0.1789(13) 0.3988(13) 0.4114(9) 0.037(6) Uiso d 1 . . H H1A 0.000000 0.500000 0.1357(17) 0.077(14) Uiso 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 Cl1 0.0421(2) 0.02417(19) 0.0442(2) 0.00136(15) 0.01026(17) 0.00663(15) Cl2 0.0513(4) 0.0331(3) 0.0224(2) 0.0004(2) 0.000 0.000 O1 0.0225(5) 0.0313(6) 0.0318(6) -0.0003(4) -0.0012(4) 0.0007(4) N3 0.0265(6) 0.0200(5) 0.0210(5) -0.0002(4) -0.0015(4) -0.0017(4) N2 0.0234(6) 0.0225(5) 0.0224(5) 0.0017(4) 0.0001(4) -0.0013(4) N1 0.0321(7) 0.0252(6) 0.0211(6) 0.0006(5) 0.0007(5) -0.0034(4) N4 0.0263(6) 0.0271(6) 0.0210(6) -0.0012(5) 0.0007(4) -0.0003(4) C1 0.0234(6) 0.0237(6) 0.0256(7) 0.0024(5) -0.0024(5) -0.0013(5) C7 0.0216(6) 0.0219(6) 0.0214(6) 0.0025(5) 0.0000(5) -0.0024(5) C2 0.0219(6) 0.0214(6) 0.0249(6) 0.0018(5) -0.0018(5) -0.0015(5) C10 0.0234(6) 0.0241(7) 0.0282(7) 0.0020(5) 0.0025(5) 0.0007(5) C14 0.0272(7) 0.0211(6) 0.0233(6) 0.0015(5) -0.0014(5) -0.0014(5) C9 0.0203(6) 0.0236(6) 0.0246(6) 0.0021(5) 0.0006(5) 0.0006(5) C16 0.0286(7) 0.0256(7) 0.0220(6) -0.0001(6) 0.0009(5) -0.0028(5) C15 0.0264(7) 0.0228(6) 0.0241(6) -0.0020(5) -0.0011(5) 0.0003(5) C3 0.0239(6) 0.0236(6) 0.0293(7) 0.0010(5) 0.0000(5) -0.0010(5) C11 0.0286(7) 0.0238(7) 0.0349(8) 0.0030(6) 0.0051(6) 0.0046(6) C5 0.0275(7) 0.0284(7) 0.0392(9) -0.0019(6) -0.0071(6) -0.0053(6) C8 0.0258(7) 0.0257(7) 0.0245(7) 0.0022(5) -0.0009(5) 0.0001(5) C17 0.0275(7) 0.0230(6) 0.0205(6) -0.0010(5) -0.0005(5) -0.0027(5) C6 0.0294(7) 0.0304(7) 0.0274(7) 0.0016(6) -0.0056(6) -0.0055(6) C4 0.0233(7) 0.0262(7) 0.0387(8) -0.0019(5) -0.0006(6) -0.0014(6) C13 0.0494(10) 0.0340(8) 0.0224(7) 0.0029(7) -0.0001(7) 0.0013(6) C12 0.0477(10) 0.0327(8) 0.0279(8) 0.0034(7) 0.0032(7) 0.0070(6) C18 0.0464(9) 0.0368(8) 0.0203(7) -0.0016(7) 0.0000(6) 0.0033(6) 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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N4 O1 H1A . . 107.9(6) ? C7 N3 C17 . . 115.75(12) ? C7 N3 C14 . . 116.31(11) ? C17 N3 C14 . . 111.87(11) ? C7 N2 C9 . . 126.07(13) ? C1 N1 C8 . . 120.58(13) ? C1 N1 H1 . . 114.0(15) ? C8 N1 H1 . . 109.5(15) ? O1 N4 C18 . . 109.17(12) ? O1 N4 C15 . . 110.03(11) ? C18 N4 C15 . . 110.59(12) ? O1 N4 C16 . . 107.20(11) ? C18 N4 C16 . . 110.61(12) ? C15 N4 C16 . . 109.18(12) ? C6 C1 C2 . . 119.37(14) ? C6 C1 N1 . . 118.67(14) ? C2 C1 N1 . . 121.88(13) ? N2 C7 N3 . . 116.40(13) ? N2 C7 C2 . . 128.37(13) ? N3 C7 C2 . . 115.03(12) ? C1 C2 C3 . . 118.60(14) ? C1 C2 C7 . . 121.68(13) ? C3 C2 C7 . . 119.68(13) ? C11 C10 C9 . . 120.58(14) ? C11 C10 H10 . . 119.7 ? C9 C10 H10 . . 119.7 ? N3 C14 C15 . . 110.58(12) ? N3 C14 H14A . . 109.5 ? C15 C14 H14A . . 109.5 ? N3 C14 H14B . . 109.5 ? C15 C14 H14B . . 109.5 ? H14A C14 H14B . . 108.1 ? N2 C9 C10 . . 114.92(13) ? N2 C9 C8 . . 125.70(13) ? C10 C9 C8 . . 118.63(13) ? N4 C16 C17 . . 110.97(12) ? N4 C16 H16A . . 109.4 ? C17 C16 H16A . . 109.4 ? N4 C16 H16B . . 109.4 ? C17 C16 H16B . . 109.4 ? H16A C16 H16B . . 108.0 ? N4 C15 C14 . . 110.53(12) ? N4 C15 H15A . . 109.5 ? C14 C15 H15A . . 109.5 ? N4 C15 H15B . . 109.5 ? C14 C15 H15B . . 109.5 ? H15A C15 H15B . . 108.1 ? C4 C3 C2 . . 121.53(15) ? C4 C3 H3 . . 119.2 ? C2 C3 H3 . . 119.2 ? C12 C11 C10 . . 121.41(15) ? C12 C11 Cl1 . . 119.43(13) ? C10 C11 Cl1 . . 119.16(13) ? C6 C5 C4 . . 120.17(15) ? C6 C5 H5 . . 119.9 ? C4 C5 H5 . . 119.9 ? C13 C8 N1 . . 119.28(14) ? C13 C8 C9 . . 119.13(15) ? N1 C8 C9 . . 121.24(13) ? N3 C17 C16 . . 110.00(12) ? N3 C17 H17A . . 109.7 ? C16 C17 H17A . . 109.7 ? N3 C17 H17B . . 109.7 ? C16 C17 H17B . . 109.7 ? H17A C17 H17B . . 108.2 ? C5 C6 C1 . . 120.92(15) ? C5 C6 H6 . . 119.5 ? C1 C6 H6 . . 119.5 ? C3 C4 C5 . . 119.38(15) ? C3 C4 H4 . . 120.3 ? C5 C4 H4 . . 120.3 ? C12 C13 C8 . . 121.79(16) ? C12 C13 H13 . . 119.1 ? C8 C13 H13 . . 119.1 ? C11 C12 C13 . . 118.44(15) ? C11 C12 H12 . . 120.8 ? C13 C12 H12 . . 120.8 ? N4 C18 H18A . . 109.5 ? N4 C18 H18B . . 109.5 ? H18A C18 H18B . . 109.5 ? N4 C18 H18C . . 109.5 ? H18A C18 H18C . . 109.5 ? H18B C18 H18C . . 109.5 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cl1 C11 . 1.7506(17) ? O1 N4 . 1.4051(17) ? O1 H1A . 1.2169(12) ? N3 C7 . 1.4035(18) ? N3 C17 . 1.4692(18) ? N3 C14 . 1.4723(18) ? N2 C7 . 1.2852(19) ? N2 C9 . 1.4012(19) ? N1 C1 . 1.406(2) ? N1 C8 . 1.406(2) ? N1 H1 . 0.86(2) ? N4 C18 . 1.494(2) ? N4 C15 . 1.5016(19) ? N4 C16 . 1.502(2) ? C1 C6 . 1.403(2) ? C1 C2 . 1.405(2) ? C7 C2 . 1.492(2) ? C2 C3 . 1.406(2) ? C10 C11 . 1.382(2) ? C10 C9 . 1.403(2) ? C10 H10 . 0.9300 ? C14 C15 . 1.513(2) ? C14 H14A . 0.9700 ? C14 H14B . 0.9700 ? C9 C8 . 1.409(2) ? C16 C17 . 1.518(2) ? C16 H16A . 0.9700 ? C16 H16B . 0.9700 ? C15 H15A . 0.9700 ? C15 H15B . 0.9700 ? C3 C4 . 1.388(2) ? C3 H3 . 0.9300 ? C11 C12 . 1.380(2) ? C5 C6 . 1.386(2) ? C5 C4 . 1.390(2) ? C5 H5 . 0.9300 ? C8 C13 . 1.398(2) ? C17 H17A . 0.9700 ? C17 H17B . 0.9700 ? C6 H6 . 0.9300 ? C4 H4 . 0.9300 ? C13 C12 . 1.388(3) ? C13 H13 . 0.9300 ? C12 H12 . 0.9300 ? C18 H18A . 0.9600 ? C18 H18B . 0.9600 ? C18 H18C . 0.9600 ? 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 O1 H1A O1 2_565 1.2169(12) 1.2169(12) 2.434(2) 179(4) N1 H1 Cl2 . 0.86(2) 2.46(2) 3.3259(14) 176(2) C15 H15A O1 2_565 0.97 2.64 3.2598(19) 122 C15 H15A N1 16 0.97 2.51 3.416(2) 156 C15 H15B Cl1 13 0.97 2.91 3.8431(17) 162 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C8 N1 C1 C6 . . . . -127.64(15) ? C8 N1 C1 C2 . . . . 55.7(2) y C9 N2 C7 N3 . . . . 177.72(13) ? C9 N2 C7 C2 . . . . 3.2(2) y C17 N3 C7 N2 . . . . -6.69(19) ? C14 N3 C7 N2 . . . . 127.72(14) ? C17 N3 C7 C2 . . . . 168.54(12) ? C14 N3 C7 C2 . . . . -57.05(17) ? C6 C1 C2 C3 . . . . 2.0(2) ? N1 C1 C2 C3 . . . . 178.72(13) ? C6 C1 C2 C7 . . . . -175.82(13) ? N1 C1 C2 C7 . . . . 0.9(2) y N2 C7 C2 C1 . . . . -35.2(2) y N3 C7 C2 C1 . . . . 150.21(14) ? N2 C7 C2 C3 . . . . 146.92(15) ? N3 C7 C2 C3 . . . . -27.63(19) ? C7 N3 C14 C15 . . . . 166.35(12) ? C17 N3 C14 C15 . . . . -57.55(16) ? C7 N2 C9 C10 . . . . -156.61(14) ? C7 N2 C9 C8 . . . . 33.5(2) y C11 C10 C9 N2 . . . . -170.69(14) ? C11 C10 C9 C8 . . . . 0.0(2) ? O1 N4 C16 C17 . . . . -61.75(15) ? C18 N4 C16 C17 . . . . 179.32(13) ? C15 N4 C16 C17 . . . . 57.41(16) ? O1 N4 C15 C14 . . . . 60.16(15) ? C18 N4 C15 C14 . . . . -179.16(13) ? C16 N4 C15 C14 . . . . -57.23(15) ? N3 C14 C15 N4 . . . . 57.38(16) ? C1 C2 C3 C4 . . . . -1.4(2) ? C7 C2 C3 C4 . . . . 176.48(14) ? C9 C10 C11 C12 . . . . 1.4(2) ? C9 C10 C11 Cl1 . . . . -179.55(11) ? C1 N1 C8 C13 . . . . 132.81(16) ? C1 N1 C8 C9 . . . . -54.0(2) y N2 C9 C8 C13 . . . . 168.37(15) ? C10 C9 C8 C13 . . . . -1.2(2) ? N2 C9 C8 N1 . . . . -4.9(2) y C10 C9 C8 N1 . . . . -174.45(14) ? C7 N3 C17 C16 . . . . -166.50(12) ? C14 N3 C17 C16 . . . . 57.13(16) ? N4 C16 C17 N3 . . . . -57.28(16) ? C4 C5 C6 C1 . . . . -0.8(2) ? C2 C1 C6 C5 . . . . -1.0(2) ? N1 C1 C6 C5 . . . . -177.76(15) ? C2 C3 C4 C5 . . . . -0.3(2) ? C6 C5 C4 C3 . . . . 1.4(2) ? N1 C8 C13 C12 . . . . 174.49(17) ? C9 C8 C13 C12 . . . . 1.1(3) ? C10 C11 C12 C13 . . . . -1.5(3) ? Cl1 C11 C12 C13 . . . . 179.46(14) ? C8 C13 C12 C11 . . . . 0.2(3) ? _cod_database_fobs_code 2244183