#------------------------------------------------------------------------------ #$Date: 2016-11-30 04:09:59 +0200 (Wed, 30 Nov 2016) $ #$Revision: 188749 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/19/2241963.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_2241963 loop_ _publ_author_name 'K\"oysal, Yavuz' 'B\"ulb\"ul, Hakan' '\.Ilhan, \.Ilhan \"Ozer' 'Ak\?in, Nazenin' 'Dege, Necmi' _publ_section_title ; Crystal structure and computational studies of (3Z)-4-benzoyl-3-[(2,4-dinitrophenyl)hydrazinylidene]-5-phenylfuran-2(3H)-one ; _journal_coeditor_code WM5340 _journal_issue 12 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 1852 _journal_page_last 1855 _journal_paper_doi 10.1107/S2056989016018600 _journal_volume 72 _journal_year 2016 _chemical_formula_iupac 'C23 H14 N4 O7' _chemical_formula_moiety 'C23 H14 N4 O7' _chemical_formula_sum 'C23 H14 N4 O7' _chemical_formula_weight 458.38 _chemical_name_systematic (3Z)-4-Benzoyl-3-[(2,4-dinitrophenyl)hydrazinylidene]-5-phenylfuran-2(3H)-one _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 105.183(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 20.7156(11) _cell_length_b 6.3660(3) _cell_length_c 16.0288(7) _cell_measurement_reflns_used 18113 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.41 _cell_measurement_theta_min 1.32 _cell_volume 2040.02(17) _computing_cell_refinement ; X-AREA (Stoe & Cie, 2002) ; _computing_data_collection ; X-AREA (Stoe & Cie, 2002) ; _computing_data_reduction ; X-RED32 (Stoe & Cie, 2002) ; _computing_molecular_graphics ; ORTEP-3 for Windows (Farrugia, 2012) ; _computing_publication_material ; WinGX (Farrugia, 2012) ; _computing_structure_refinement ; SHELXL2014 (Sheldrick, 2015) ; _computing_structure_solution ; SHELXS97 (Sheldrick, 2008) ; _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 6.67 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Stoe IPDS 2' _diffrn_measurement_method \w-scans _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 18074 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.997 _diffrn_reflns_theta_min 2.037 _exptl_absorpt_coefficient_mu 0.114 _exptl_absorpt_correction_T_max 0.9849 _exptl_absorpt_correction_T_min 0.9535 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details ; (X-RED32; Stoe & Cie, 2002) ; _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.492 _exptl_crystal_density_method 'not measured' _exptl_crystal_description stick _exptl_crystal_F_000 944 _exptl_crystal_size_max 0.640 _exptl_crystal_size_mid 0.340 _exptl_crystal_size_min 0.150 _refine_diff_density_max 0.112 _refine_diff_density_min -0.147 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 311 _refine_ls_number_reflns 3992 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.012 _refine_ls_R_factor_all 0.0736 _refine_ls_R_factor_gt 0.0385 _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^)+(0.0424P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0796 _refine_ls_wR_factor_ref 0.0888 _reflns_number_gt 2617 _reflns_number_total 3992 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file wm5340sup1.cif _cod_data_source_block I _cod_database_code 2241963 _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 ; -2 0 0 2065.01 17.06 0 2 0 0 1973.47 16.90 0 3 0 0 8.94 3.11 0 -3 0 0 8.67 3.10 0 4 0 0 70.05 3.44 0 -4 0 0 73.17 3.52 0 -5 0 0 26.84 2.61 0 5 0 0 26.03 2.65 0 -6 0 0 1216.84 7.95 0 6 0 0 1218.59 7.93 0 -7 0 0 20.73 2.19 0 7 0 0 25.24 2.23 0 -8 0 0 697.73 5.46 0 8 0 0 702.95 5.33 0 9 0 0 483.15 4.34 0 -9 0 0 445.74 4.28 0 10 0 0 374.93 3.75 0 -10 0 0 368.10 3.86 0 -11 0 0 84.18 2.23 0 11 0 0 90.82 2.27 0 12 0 0 14.68 1.74 0 -12 0 0 14.43 1.72 0 -13 0 0 81.00 2.21 0 13 0 0 86.63 2.27 0 14 0 0 44.42 2.01 0 -14 0 0 41.77 2.03 0 15 0 0 16.47 1.80 0 -15 0 0 13.03 1.77 0 16 0 0 0.76 1.83 0 -16 0 0 0.11 1.73 0 17 0 0 12.28 2.24 0 -17 0 0 10.56 1.78 0 -18 0 0 39.81 2.13 0 18 0 0 48.12 2.09 0 -19 0 0 67.95 2.25 0 19 0 0 66.77 2.30 0 -20 0 0 42.66 2.13 0 20 0 0 50.30 2.25 0 21 0 0 3.46 1.92 0 -21 0 0 5.24 1.92 0 22 0 0 1.05 2.06 0 -22 0 0 5.74 1.98 0 23 0 0 0.34 2.11 0 -23 0 0 1.12 2.00 0 -24 0 0 7.72 2.27 0 24 0 0 14.82 2.23 0 25 0 0 -0.47 2.38 0 -25 0 0 0.10 2.24 0 -1 1 0 938.98 12.50 0 1 1 0 992.89 11.01 0 -1 -1 0 948.42 9.26 0 1 -1 0 957.89 12.36 0 -1 -1 0 962.29 10.81 0 1 1 0 935.64 9.16 0 -2 1 0 128.79 6.11 0 -2 -1 0 124.46 4.33 0 -2 1 0 120.12 5.67 0 2 1 0 114.90 3.83 0 -2 -1 0 114.30 3.82 0 3 -1 0 42.27 3.91 0 -3 1 0 42.28 3.87 0 -3 -1 0 42.68 2.90 0 3 1 0 42.81 2.88 0 -4 -1 0 683.28 6.07 0 -4 1 0 677.85 9.01 0 4 -1 0 708.07 9.13 0 4 1 0 683.20 5.99 0 5 1 0 2.80 2.11 0 5 -1 0 2.87 2.72 0 -5 1 0 3.28 2.61 0 -5 -1 0 1.92 2.12 0 6 -1 0 110.51 3.72 0 -6 1 0 111.04 3.42 0 -6 -1 0 107.34 2.76 0 6 1 0 112.07 2.43 0 7 1 0 18.50 1.98 0 -7 1 0 19.43 2.57 0 7 -1 0 21.39 2.67 0 -7 -1 0 19.34 1.52 0 -8 -1 0 1.36 1.66 0 8 1 0 -0.74 1.68 0 -8 1 0 0.54 1.88 0 8 -1 0 1.59 2.40 0 -9 1 0 82.99 2.96 0 9 -1 0 86.54 2.73 0 9 1 0 86.50 1.94 0 -9 -1 0 87.58 2.28 0 10 1 0 19.77 1.77 0 -10 1 0 18.82 2.03 0 10 -1 0 18.28 2.52 0 -10 -1 0 18.82 1.79 0 -11 -1 0 11.01 1.69 0 11 -1 0 11.01 1.91 0 11 1 0 7.94 1.73 0 -11 1 0 10.15 1.88 0 12 -1 0 13.04 2.21 0 -12 -1 0 12.45 1.70 0 12 1 0 12.64 1.72 0 -12 1 0 13.07 2.21 0 -13 1 0 23.40 1.90 0 -13 -1 0 25.88 1.75 0 13 -1 0 26.34 1.96 0 13 1 0 25.15 1.76 0 -14 -1 0 1.06 1.56 0 14 1 0 1.28 1.58 0 14 -1 0 1.24 2.17 0 -14 1 0 0.68 1.72 0 15 -1 0 4.54 1.66 0 -15 -1 0 6.99 1.64 0 15 1 0 5.97 1.63 0 -15 1 0 5.33 1.65 0 16 1 0 5.99 1.70 0 -16 1 0 4.99 2.11 0 -16 -1 0 5.14 1.69 0 16 -1 0 7.27 1.85 0 17 1 0 3.42 1.78 0 17 -1 0 1.03 1.85 0 -17 -1 0 4.45 1.80 0 -17 1 0 1.55 1.78 0 18 -1 0 0.35 1.82 0 -18 1 0 1.53 1.81 0 18 1 0 -0.01 1.83 0 -18 -1 0 0.65 1.69 0 -19 1 0 5.50 2.31 0 19 -1 0 6.74 1.90 0 19 1 0 5.49 1.81 0 -19 -1 0 2.06 1.79 0 20 1 0 -0.20 1.84 0 20 -1 0 0.85 1.94 0 -20 -1 0 0.59 1.87 0 -20 1 0 0.89 1.89 0 -21 -1 0 8.59 1.97 0 21 1 0 7.73 1.96 0 21 -1 0 10.65 2.07 0 -21 1 0 9.87 2.08 0 22 -1 0 1.99 2.01 0 -22 -1 0 -2.79 1.88 0 -22 1 0 -0.13 2.06 0 22 1 0 0.31 2.00 0 23 1 0 4.06 2.08 0 -23 1 0 1.30 2.14 0 -23 -1 0 1.53 2.00 0 23 -1 0 4.21 2.17 0 24 1 0 7.06 2.09 0 24 -1 0 6.18 2.78 0 -24 -1 0 3.42 2.12 0 -24 1 0 2.50 2.74 0 25 1 0 0.65 2.24 0 25 -1 0 4.26 2.40 0 -25 1 0 0.53 2.30 0 -25 -1 0 3.16 2.14 0 0 2 0 50.51 2.58 0 0 -2 0 48.24 2.63 0 0 2 0 48.24 2.65 0 1 2 0 18.27 2.28 0 -1 -2 0 18.29 2.26 0 1 2 0 17.79 2.27 0 -1 2 0 18.64 2.24 0 -1 2 0 17.09 2.30 0 1 -2 0 18.73 2.73 0 -1 -2 0 18.46 2.23 0 -2 -2 0 47.85 2.47 0 2 2 0 49.06 2.64 0 2 2 0 44.59 2.47 0 -2 2 0 48.86 3.17 0 -2 -2 0 47.54 2.54 0 2 -2 0 48.66 3.19 0 -3 -2 0 247.97 3.43 0 3 2 0 248.93 3.69 0 -3 2 0 259.64 5.47 0 -3 -2 0 265.61 4.25 0 -3 2 0 266.96 5.56 0 4 2 0 2.32 1.83 0 -4 2 0 0.93 2.27 0 -4 2 0 0.33 2.74 0 -4 -2 0 0.36 1.87 0 -4 -2 0 0.17 2.37 0 -5 -2 0 0.40 2.36 0 5 2 0 0.26 1.77 0 -5 2 0 1.22 2.62 0 -5 2 0 0.09 2.63 0 -5 -2 0 -2.16 1.76 0 6 -2 0 7.77 2.67 0 6 2 0 6.75 1.70 0 -6 2 0 7.10 2.31 0 -6 -2 0 9.91 1.75 0 -7 2 0 636.34 7.28 0 7 -2 0 675.09 7.39 0 -7 -2 0 649.93 4.42 0 7 2 0 635.08 4.49 0 8 2 0 445.84 3.82 0 -8 -2 0 419.12 3.52 0 8 -2 0 466.55 5.90 0 -8 2 0 448.05 5.88 0 -9 -2 0 101.57 2.37 0 -9 2 0 104.49 3.28 0 9 2 0 106.28 2.39 0 9 -2 0 111.77 3.25 0 10 -2 0 38.15 2.55 0 10 2 0 38.65 1.95 0 -10 -2 0 34.11 1.93 0 -10 2 0 37.94 2.52 0 11 2 0 55.84 1.96 0 -11 2 0 53.82 2.63 0 11 -2 0 60.49 2.62 0 -11 -2 0 50.48 1.56 0 12 2 0 62.58 1.63 0 12 -2 0 69.26 2.72 0 -12 -2 0 64.07 2.00 0 -12 2 0 60.66 2.65 0 -13 -2 0 29.10 1.84 0 13 -2 0 28.52 2.06 0 13 2 0 25.06 1.80 0 -13 2 0 28.55 2.36 0 -14 2 0 0.63 1.72 0 -14 -2 0 0.86 1.70 0 14 2 0 2.53 1.63 0 14 -2 0 0.81 1.84 0 15 2 0 4.71 1.79 0 -15 -2 0 3.23 1.74 0 -15 2 0 3.08 2.18 0 15 -2 0 2.52 2.18 0 -16 2 0 1.95 2.16 0 16 2 0 3.41 1.76 0 -16 -2 0 3.06 1.73 0 16 -2 0 3.23 2.31 0 -17 2 0 1.19 2.24 0 17 -2 0 1.53 2.33 0 -17 -2 0 0.69 1.70 0 17 2 0 0.10 1.20 0 18 -2 0 0.70 2.26 0 -18 2 0 3.99 2.17 0 -18 -2 0 0.50 1.81 0 18 2 0 2.44 1.78 0 19 -2 0 1.37 1.96 0 19 2 0 1.32 1.31 0 -19 2 0 1.05 2.33 0 -19 -2 0 -0.22 1.81 0 20 -2 0 -0.11 2.53 0 -20 2 0 1.88 2.34 0 -20 -2 0 2.06 1.92 0 20 2 0 -1.75 1.81 0 -21 2 0 3.95 2.06 0 21 -2 0 3.52 2.54 0 -21 -2 0 2.80 1.94 0 21 2 0 2.11 1.92 0 -22 2 0 2.40 2.02 0 22 2 0 2.95 1.88 0 22 -2 0 1.63 2.06 0 -22 -2 0 0.40 2.03 0 23 -2 0 -0.36 2.20 0 -23 -2 0 1.49 2.04 0 -23 2 0 0.74 2.15 0 23 2 0 -0.80 2.10 0 24 -2 0 2.91 2.22 0 24 2 0 2.14 2.22 0 -24 -2 0 0.21 2.16 0 -24 2 0 2.17 2.66 0 1 3 0 -0.25 1.73 0 -1 -3 0 1.93 1.70 0 -1 3 0 0.04 1.64 0 1 3 0 -0.19 2.21 0 1 -3 0 0.08 2.25 0 -1 3 0 1.30 1.73 0 2 3 0 265.06 3.41 0 -2 3 0 276.84 3.42 0 2 3 0 280.73 3.89 0 2 -3 0 277.18 4.35 0 -2 -3 0 268.09 3.43 0 -2 3 0 267.27 4.16 0 -2 -3 0 277.91 4.12 0 -3 -3 0 42.79 1.97 0 -3 -3 0 45.38 2.63 0 3 3 0 46.21 2.64 0 -3 3 0 44.55 2.68 0 3 -3 0 49.69 2.74 0 3 3 0 44.39 1.98 0 -4 3 0 19.87 2.66 0 -4 3 0 17.76 2.38 0 4 3 0 16.68 1.27 0 -4 -3 0 20.06 1.99 0 -4 -3 0 16.35 1.71 0 5 3 0 352.51 3.51 0 -5 -3 0 345.41 3.51 0 -5 3 0 378.90 5.95 0 -5 3 0 364.85 5.80 0 -5 -3 0 369.44 4.61 0 -6 -3 0 5.20 1.67 0 -6 3 0 5.07 2.43 0 6 3 0 4.94 1.18 0 -6 3 0 4.88 2.26 0 -6 -3 0 6.75 1.85 0 -7 3 0 47.72 2.94 0 -7 3 0 47.51 3.24 0 7 3 0 46.79 1.94 0 -7 -3 0 42.52 1.90 0 -7 -3 0 45.27 2.25 0 -8 3 0 12.34 2.53 0 -8 3 0 12.73 2.45 0 -8 -3 0 12.53 1.89 0 -8 -3 0 13.24 1.78 0 8 3 0 11.57 1.70 0 -9 -3 0 146.35 3.14 0 -9 3 0 152.93 4.12 0 -9 3 0 145.06 4.23 0 9 3 0 141.45 2.37 0 -9 -3 0 137.51 2.06 0 10 3 0 11.23 1.22 0 -10 3 0 10.58 2.59 0 -10 -3 0 12.43 1.67 0 10 -3 0 13.09 2.58 0 11 -3 0 -0.44 2.47 0 -11 3 0 0.75 2.43 0 -11 -3 0 0.46 1.67 0 11 3 0 0.76 1.65 0 -12 3 0 35.14 2.61 0 12 -3 0 39.90 2.66 0 -12 -3 0 38.39 1.91 0 12 3 0 40.65 1.90 0 13 3 0 182.85 2.63 0 -13 3 0 169.55 3.90 0 13 -3 0 192.92 3.91 0 -13 -3 0 183.48 2.64 0 -14 -3 0 55.47 2.02 0 14 -3 0 61.18 2.82 0 14 3 0 54.40 2.03 0 -14 3 0 52.05 3.02 0 15 -3 0 13.19 2.40 0 -15 -3 0 11.22 1.78 0 -15 3 0 10.11 2.28 0 15 3 0 10.80 1.80 0 16 -3 0 -0.07 2.29 0 -16 3 0 0.95 2.17 0 16 3 0 1.29 1.80 0 -16 -3 0 -1.36 1.76 0 17 -3 0 4.66 2.37 0 -17 -3 0 2.83 1.30 0 -17 3 0 3.78 2.29 0 17 3 0 4.71 1.87 0 18 3 0 18.31 1.94 0 -18 -3 0 14.80 1.90 0 -18 3 0 13.13 2.48 0 18 -3 0 15.14 2.53 0 19 3 0 4.91 1.87 0 -19 -3 0 0.15 1.88 0 19 -3 0 -0.70 2.46 0 -19 3 0 1.24 2.39 0 20 -3 0 -0.42 2.57 0 -20 3 0 0.68 2.48 0 -20 -3 0 -0.86 1.97 0 20 3 0 -0.49 1.97 0 21 -3 0 5.02 2.66 0 -21 -3 0 3.39 2.03 0 -21 3 0 1.84 2.64 0 21 3 0 3.08 2.04 0 22 3 0 1.34 2.14 0 -22 3 0 2.83 2.56 0 -22 -3 0 2.86 2.08 0 22 -3 0 2.15 2.71 0 23 -3 0 3.48 2.87 0 -23 3 0 2.89 2.84 0 23 3 0 1.94 2.19 0 -23 -3 0 2.35 2.23 0 0 -4 0 59.65 2.26 0 0 4 0 59.04 2.58 0 0 4 0 60.14 2.46 0 -1 4 0 7.47 1.72 0 1 4 0 8.89 2.18 0 1 4 0 8.13 1.75 0 -1 4 0 9.25 2.21 0 -1 -4 0 8.93 1.73 0 1 -4 0 9.87 1.81 0 -2 4 0 9.08 2.09 0 2 4 0 10.32 1.83 0 -2 4 0 10.99 1.75 0 2 4 0 11.16 1.71 0 -2 -4 0 11.31 1.73 0 2 -4 0 10.37 2.18 0 -3 4 0 -0.21 1.96 0 -3 4 0 0.88 1.63 0 3 4 0 -0.01 2.20 0 -3 -4 0 1.87 1.67 0 -3 -4 0 1.27 1.67 0 3 -4 0 1.32 1.69 0 3 4 0 -0.06 1.68 0 -4 -4 0 46.18 2.41 0 -4 4 0 47.70 2.57 0 -4 4 0 48.17 2.00 0 4 4 0 46.92 2.00 0 4 4 0 48.73 2.54 0 -4 -4 0 49.75 2.41 0 5 4 0 35.58 1.90 0 -5 -4 0 32.63 1.87 0 -5 4 0 37.10 2.80 0 -5 -4 0 36.42 2.30 0 -5 4 0 35.40 2.75 0 -6 4 0 4.04 2.54 0 -6 -4 0 2.80 1.99 0 -6 4 0 2.55 2.44 0 6 4 0 3.91 1.59 0 -6 -4 0 3.62 1.64 0 7 4 0 6.79 1.67 0 -7 -4 0 6.55 1.59 0 -7 4 0 8.10 2.90 0 -7 -4 0 6.50 1.69 0 -7 4 0 6.18 2.59 0 8 4 0 8.85 1.61 0 -8 -4 0 8.40 1.55 0 -8 -4 0 11.20 2.20 0 -8 4 0 10.71 2.88 0 -8 4 0 10.76 2.77 0 -9 -4 0 -0.21 1.79 0 -9 4 0 1.36 2.97 0 -9 4 0 0.07 2.63 0 -9 -4 0 -1.14 1.63 0 9 4 0 0.36 1.59 0 -10 -4 0 77.56 2.00 0 -10 4 0 75.59 4.12 0 -10 -4 0 79.78 2.68 0 -10 4 0 78.24 4.08 0 10 4 0 71.97 2.05 0 -11 4 0 26.57 3.40 0 -11 -4 0 29.33 2.02 0 11 4 0 26.93 1.91 0 -11 -4 0 23.69 1.88 0 -11 4 0 26.04 3.47 0 -12 4 0 1.55 3.16 0 12 4 0 2.40 1.24 0 -12 -4 0 3.04 1.73 0 -12 4 0 1.92 3.12 0 -12 -4 0 2.68 1.88 0 -13 -4 0 14.59 2.49 0 -13 4 0 17.38 3.37 0 13 4 0 14.92 1.85 0 -13 4 0 14.83 3.16 0 -13 -4 0 16.38 1.80 0 -14 -4 0 20.90 1.89 0 -14 -4 0 19.99 2.37 0 -14 4 0 20.69 3.23 0 14 4 0 16.29 1.87 0 -14 4 0 18.29 3.42 0 -15 4 0 20.44 3.33 0 -15 4 0 24.60 3.57 0 15 4 0 20.71 1.98 0 -15 -4 0 21.88 1.95 0 -15 -4 0 23.49 2.46 0 -16 4 0 5.13 3.11 0 16 4 0 4.57 1.89 0 -16 -4 0 4.23 1.81 0 -16 -4 0 7.23 1.90 0 -16 4 0 4.45 2.77 0 17 4 0 0.02 1.88 0 -17 4 0 0.58 2.89 0 -17 -4 0 3.70 1.86 0 -17 -4 0 3.73 2.00 0 18 4 0 -0.00 1.98 0 -18 4 0 2.15 3.18 0 -18 -4 0 2.75 1.92 0 -19 -4 0 1.27 1.46 0 19 4 0 1.75 1.44 0 -19 4 0 0.88 2.92 0 20 4 0 7.97 2.12 0 20 -4 0 7.24 3.55 0 -20 4 0 5.99 3.54 0 -20 -4 0 6.30 2.15 0 21 4 0 2.68 2.12 0 -21 4 0 2.43 3.14 0 -21 -4 0 0.48 2.18 0 21 -4 0 3.45 3.13 0 -22 -4 0 2.34 2.24 0 22 4 0 -1.76 2.21 0 22 -4 0 1.73 3.40 0 -22 4 0 2.30 3.18 0 1 5 0 0.18 1.70 0 1 -5 0 0.02 2.15 0 -1 -5 0 -0.25 1.60 0 1 5 0 -0.77 1.61 0 -1 5 0 -0.12 1.73 0 -1 5 0 1.79 1.85 0 -2 5 0 9.54 2.28 0 2 -5 0 9.81 2.33 0 -2 5 0 10.06 2.22 0 2 5 0 9.48 1.84 0 2 5 0 8.99 2.17 0 -2 -5 0 10.21 1.87 0 3 5 0 2.13 2.15 0 -3 5 0 -0.86 1.81 0 -3 5 0 0.76 2.19 0 3 -5 0 2.93 2.16 0 -3 -5 0 -0.93 2.14 0 3 5 0 0.08 1.78 0 4 5 0 -0.09 1.85 0 4 5 0 3.30 2.13 0 -4 -5 0 1.63 1.71 0 -4 5 0 2.71 2.08 0 -4 5 0 2.49 2.15 0 -5 5 0 -0.32 2.16 0 -5 -5 0 2.21 1.75 0 -5 5 0 0.83 2.45 0 -5 5 0 1.37 1.76 0 5 5 0 -1.44 1.75 0 -6 5 0 11.31 1.81 0 -6 -5 0 12.37 1.85 0 6 5 0 12.38 1.81 0 -6 -5 0 12.40 1.80 0 -6 5 0 11.20 2.55 0 -6 5 0 11.98 2.65 0 7 5 0 78.16 2.19 0 -7 5 0 76.96 3.79 0 -7 5 0 79.11 3.84 0 -7 -5 0 69.67 2.15 0 -7 -5 0 80.62 2.35 0 -8 -5 0 5.09 1.75 0 -8 -5 0 4.05 1.78 0 8 5 0 6.01 1.72 0 -8 5 0 4.90 2.99 0 -8 5 0 4.94 3.03 0 -9 -5 0 66.57 2.46 0 -9 5 0 62.26 4.68 0 -9 -5 0 59.24 2.09 0 -9 5 0 60.51 4.68 0 9 5 0 60.06 2.11 0 -10 -5 0 2.87 2.19 0 10 5 0 1.81 1.74 0 -10 -5 0 2.35 1.74 0 11 5 0 70.69 2.17 0 -11 -5 0 75.76 2.46 0 -11 -5 0 71.54 2.13 0 12 5 0 0.14 1.34 0 -12 -5 0 1.54 2.35 0 -12 -5 0 -0.14 1.25 0 -13 -5 0 97.01 2.96 0 -13 -5 0 88.97 2.31 0 13 5 0 86.56 2.28 0 14 5 0 13.49 1.85 0 -14 -5 0 11.76 1.90 0 -14 -5 0 15.11 2.14 0 15 5 0 9.93 1.92 0 -15 -5 0 10.51 1.88 0 -15 -5 0 9.64 2.10 0 16 5 0 3.59 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32.79 2.45 0 -2 -3 2 31.38 1.82 0 -2 3 2 29.91 2.29 0 1 3 -2 9.63 1.70 0 1 -3 -2 10.81 1.75 0 -1 3 2 10.37 2.25 0 -1 -3 2 8.38 1.63 0 -1 3 2 9.19 1.77 0 1 3 -2 10.27 1.91 0 -1 -3 2 11.40 2.27 0 0 3 -2 41.74 1.90 0 0 3 2 38.24 2.26 0 0 3 2 37.77 2.53 0 0 -3 2 39.34 2.58 0 0 3 -2 37.10 2.57 0 0 -3 -2 38.77 2.01 0 -1 3 -2 55.94 2.06 0 1 3 2 54.71 2.06 0 1 -3 2 54.10 2.83 0 1 3 2 56.35 2.82 0 -1 -3 -2 52.24 2.01 0 -1 3 -2 53.32 2.82 0 -2 3 -2 472.27 3.80 0 -2 3 -2 477.51 6.83 0 -2 -3 -2 469.86 3.99 0 2 3 2 467.29 3.90 0 2 -3 2 471.84 6.67 0 2 3 2 488.83 6.06 0 -3 3 -2 23.52 3.13 0 -3 -3 -2 24.44 2.68 0 3 3 2 26.13 1.79 0 -3 -3 -2 24.96 1.76 0 -3 3 -2 23.60 1.79 0 3 -3 2 26.50 3.32 0 -4 -3 -2 1.41 1.62 0 -4 -3 -2 -0.23 2.07 0 4 3 2 1.88 1.11 0 5 3 2 68.88 2.10 0 -5 -3 -2 69.52 2.10 0 -5 -3 -2 74.44 3.15 0 -6 -3 -2 97.39 2.20 0 6 3 2 95.93 2.24 0 -6 -3 -2 97.33 3.06 0 7 3 2 55.03 1.59 0 -7 -3 -2 55.86 2.59 0 -7 -3 -2 54.15 1.98 0 -8 -3 -2 0.74 2.11 0 8 3 2 0.70 1.70 0 -8 -3 -2 0.74 1.72 0 9 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1.98 0 3 4 -2 7.34 1.72 0 3 4 -2 8.00 1.78 0 -3 4 2 7.67 1.71 0 -3 4 2 6.37 1.75 0 -3 -4 2 6.84 1.70 0 3 -4 -2 7.33 1.81 0 -3 -4 2 9.17 1.69 0 2 4 -2 -1.05 1.62 0 -2 -4 2 0.34 1.69 0 2 4 -2 1.14 1.75 0 -2 4 2 1.12 1.67 0 2 -4 -2 0.57 1.70 0 -2 4 2 0.41 1.69 0 1 4 -2 7.75 1.79 0 -1 -4 2 6.87 2.13 0 1 -4 -2 9.47 1.74 0 -1 4 2 8.66 1.74 0 1 4 -2 6.04 1.68 0 -1 4 2 6.95 1.68 0 0 4 2 51.99 2.05 0 0 -4 2 55.95 2.54 0 0 4 -2 52.52 2.02 0 0 -4 -2 53.08 2.04 0 0 4 -2 51.29 2.60 0 0 4 2 52.59 2.23 0 -1 4 -2 148.17 2.57 0 -1 4 -2 143.84 3.36 0 1 4 2 148.60 2.60 0 1 -4 2 145.81 3.38 0 1 4 2 152.98 3.00 0 -1 -4 -2 147.77 2.66 0 -2 4 -2 24.26 1.88 0 2 4 2 23.48 1.77 0 -2 -4 -2 21.97 1.95 0 2 -4 2 24.79 2.39 0 -2 4 -2 22.12 2.37 0 2 4 2 25.56 2.34 0 -3 -4 -2 2.26 1.60 0 -3 4 -2 0.24 2.67 0 3 4 2 1.16 1.61 0 3 -4 2 1.51 2.40 0 -3 4 -2 2.16 1.65 0 4 4 2 12.87 1.70 0 -4 4 -2 13.90 3.17 0 -4 4 -2 12.91 3.18 0 -4 -4 -2 13.59 1.71 0 -4 4 -2 14.85 1.70 0 -5 -4 -2 2.47 1.58 0 5 4 2 1.12 1.59 0 -5 -4 -2 0.30 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8.16 2.30 0 -10 -5 2 9.04 1.85 0 -10 5 2 8.23 2.81 0 10 5 -2 6.65 1.91 0 -10 5 2 8.21 2.70 0 -9 5 2 12.95 2.44 0 -9 -5 2 15.76 1.87 0 9 5 -2 11.23 1.83 0 -9 5 2 12.46 2.39 0 -9 -5 2 12.08 2.41 0 8 5 -2 48.16 2.05 0 -8 5 2 50.88 3.04 0 -8 -5 2 50.00 2.09 0 -8 5 2 44.46 2.57 0 -8 -5 2 48.17 2.17 0 -7 5 2 9.86 2.29 0 -7 -5 2 13.86 1.87 0 -7 -5 2 9.78 1.78 0 7 5 -2 16.16 2.17 0 -7 5 2 10.24 2.26 0 6 5 -2 63.79 2.13 0 -6 -5 2 58.76 2.45 0 -6 -5 2 55.05 2.15 0 -6 5 2 60.86 2.75 0 -6 5 2 59.94 2.74 0 -5 -5 2 56.57 2.08 0 -5 5 2 58.81 2.18 0 5 5 -2 56.48 2.56 0 -5 5 2 58.78 2.68 0 -5 -5 2 57.81 2.06 0 -5 5 2 57.56 2.66 0 5 5 -2 55.96 2.24 0 4 5 -2 0.40 1.73 0 -4 5 2 0.05 1.67 0 4 5 -2 0.23 2.15 0 -4 -5 2 0.42 1.71 0 -4 5 2 0.94 1.75 0 -4 -5 2 0.49 1.74 0 3 -5 -2 1.65 1.81 0 3 5 -2 1.30 1.72 0 -3 5 2 0.95 1.74 0 -3 5 2 2.87 2.09 0 3 5 -2 3.20 2.15 0 -3 -5 2 0.26 1.67 0 -2 -5 2 12.97 1.91 0 2 -5 -2 17.06 2.24 0 2 5 -2 13.48 1.92 0 -2 5 2 14.50 2.22 0 -2 5 2 13.14 1.75 0 2 5 -2 12.88 2.32 0 -1 5 2 30.49 1.89 0 -1 5 2 30.45 2.44 0 1 -5 -2 28.15 1.88 0 -1 -5 2 30.01 2.03 0 1 5 -2 27.48 2.07 0 1 5 -2 29.98 1.94 0 0 5 -2 1.76 2.24 0 0 -5 -2 1.01 2.26 0 0 5 2 0.97 1.72 0 0 5 -2 -0.59 1.80 0 0 5 2 0.79 1.78 0 0 -5 2 1.21 2.21 0 -1 -5 -2 3.09 1.75 0 1 -5 2 2.44 2.20 0 -1 5 -2 3.35 1.82 0 1 5 2 2.70 1.71 0 -1 5 -2 2.47 2.27 0 1 5 2 3.05 1.84 0 -2 5 -2 1.99 2.11 0 2 5 2 1.21 2.31 0 2 -5 2 1.05 2.16 0 2 5 2 1.33 1.77 0 -2 -5 -2 1.57 1.72 0 -2 5 -2 0.12 1.69 0 3 5 2 116.45 2.46 0 -3 -5 -2 119.03 2.46 0 3 -5 2 124.27 3.44 0 3 5 2 124.00 3.28 0 -3 5 -2 121.68 2.40 0 -3 5 -2 120.77 3.70 0 -4 -5 -2 8.39 1.72 0 -4 5 -2 8.46 2.81 0 -4 5 -2 8.30 1.75 0 4 5 2 8.37 1.75 0 -4 5 -2 9.80 2.55 0 -5 5 -2 25.50 1.84 0 -5 5 -2 26.89 4.05 0 -5 -5 -2 28.06 1.85 0 -5 5 -2 29.21 4.09 0 5 5 2 30.55 1.91 0 -6 -5 -2 5.85 1.71 0 -6 5 -2 5.91 1.78 0 6 5 2 4.16 1.76 0 7 5 2 44.86 2.08 0 -7 -5 -2 47.67 2.10 0 -7 5 -2 47.32 2.03 0 -7 -5 -2 47.98 2.75 0 -8 5 -2 16.43 1.83 0 -8 -5 -2 17.31 2.32 0 8 5 2 16.77 1.81 0 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2.27 0 -4 6 2 1.21 2.28 0 4 6 -2 -1.07 2.30 0 4 6 -2 1.32 1.81 0 -4 6 2 0.37 2.24 0 -3 -6 2 10.39 1.90 0 -3 6 2 10.51 1.90 0 3 -6 -2 9.73 2.33 0 -3 6 2 9.04 2.35 0 3 6 -2 12.19 1.92 0 3 6 -2 12.21 1.92 0 2 6 -2 1.29 1.84 0 -2 6 2 1.59 1.88 0 2 6 -2 3.18 1.83 0 -2 6 2 1.91 1.76 0 -2 -6 2 3.35 1.90 0 2 -6 -2 1.64 1.88 0 1 -6 -2 3.62 2.24 0 1 6 -2 2.40 2.24 0 -1 -6 2 0.95 1.81 0 1 6 -2 0.06 1.81 0 -1 6 2 1.42 2.29 0 -1 6 2 -0.45 1.79 0 0 6 2 7.13 1.93 0 0 6 2 8.16 2.28 0 0 -6 2 9.23 2.40 0 0 6 -2 10.06 1.94 0 0 -6 -2 8.18 2.32 0 0 6 -2 9.46 1.88 0 -1 6 -2 9.49 2.41 0 -1 -6 -2 8.26 1.90 0 1 6 2 10.12 1.90 0 1 6 2 11.45 2.37 0 -1 6 -2 5.70 1.85 0 1 -6 2 10.01 2.46 0 -2 6 -2 3.60 2.22 0 2 6 2 3.56 1.98 0 2 -6 2 2.72 2.36 0 2 6 2 2.92 1.81 0 -2 6 -2 3.18 2.37 0 -2 -6 -2 1.87 1.81 0 3 6 2 17.91 1.96 0 3 -6 2 19.96 2.92 0 -3 6 -2 19.43 2.91 0 -3 6 -2 22.06 2.01 0 -3 -6 -2 18.24 1.91 0 -4 6 -2 34.23 1.99 0 -4 6 -2 29.52 3.36 0 -4 6 -2 33.41 3.39 0 -4 -6 -2 34.47 2.12 0 4 6 2 33.64 2.13 0 5 6 2 16.44 1.92 0 -5 6 -2 20.40 2.26 0 -5 6 -2 18.13 3.83 0 -5 6 -2 18.66 3.82 0 -5 -6 -2 18.24 1.92 0 -6 -6 -2 16.27 1.93 0 -6 6 -2 17.86 1.88 0 6 6 2 17.63 2.00 0 7 6 2 2.09 1.97 0 -7 -6 -2 1.55 1.39 0 -7 6 -2 3.51 1.83 0 -8 6 -2 -0.79 1.89 0 -8 -6 -2 -0.01 1.91 0 8 6 2 1.37 1.89 0 -9 -6 -2 9.51 1.93 0 9 6 2 7.21 2.00 0 -9 6 -2 8.49 2.06 0 -10 -6 -2 0.74 1.92 0 -10 6 -2 2.35 1.85 0 10 6 2 2.02 1.84 0 11 6 2 -0.98 1.90 0 -11 -6 -2 1.11 1.95 0 -11 -6 -2 -0.82 2.78 0 -11 6 -2 -0.24 1.91 0 -12 -6 -2 -0.17 2.45 0 12 6 2 1.99 2.01 0 -12 -6 -2 1.43 1.94 0 -12 6 -2 1.98 1.35 0 -13 -6 -2 2.82 2.03 0 13 6 2 0.27 1.99 0 -13 -6 -2 0.25 2.59 0 -13 6 -2 0.03 2.07 0 14 6 2 0.90 1.50 0 -14 -6 -2 0.26 2.70 0 -14 -6 -2 3.48 2.05 0 -15 -6 -2 1.74 2.17 0 -15 -6 -2 1.31 2.73 0 15 6 2 3.22 2.05 0 -16 -6 -2 0.60 2.20 0 -16 -6 -2 -0.33 2.83 0 16 6 2 4.47 2.22 0 -13 7 2 2.48 2.20 0 13 7 -2 -1.72 2.22 0 -13 -7 2 1.38 2.30 0 -12 7 2 4.19 2.22 0 -12 -7 2 4.75 2.20 0 -12 -7 2 7.90 2.22 0 12 7 -2 5.67 2.20 0 -11 7 2 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3.56 2.64 0 21 3 -4 4.71 1.93 0 21 -3 -4 -0.87 2.43 0 -21 -3 4 -0.14 1.95 0 -21 3 4 2.52 2.61 0 -20 3 4 -0.79 2.39 0 20 3 -4 7.07 1.98 0 -20 -3 4 5.34 1.97 0 20 -3 -4 3.76 2.15 0 -19 3 4 4.33 1.99 0 19 -3 -4 4.17 2.02 0 -19 -3 4 3.78 1.88 0 19 3 -4 5.63 1.84 0 -18 -3 4 5.68 1.85 0 -18 3 4 1.26 2.32 0 18 3 -4 2.06 1.86 0 18 -3 -4 2.10 2.38 0 -17 -3 4 1.97 1.86 0 17 3 -4 4.97 1.90 0 17 -3 -4 3.78 1.93 0 -17 3 4 4.25 1.84 0 -16 3 4 3.62 1.71 0 16 -3 -4 3.04 1.80 0 16 3 -4 1.82 1.80 0 -16 -3 4 3.48 1.76 0 -15 -3 4 0.21 1.70 0 15 -3 -4 0.03 1.92 0 15 3 -4 1.89 1.72 0 -15 3 4 -0.05 2.35 0 14 -3 -4 1.86 1.83 0 -14 -3 4 0.91 1.77 0 14 3 -4 1.51 1.83 0 -14 3 4 2.17 1.77 0 -13 -3 4 85.28 2.20 0 -13 -3 4 90.22 2.28 0 13 3 -4 85.05 2.24 0 13 -3 -4 91.20 2.44 0 -13 3 4 87.07 2.49 0 12 -3 -4 1.26 1.75 0 -12 3 4 0.84 1.70 0 -12 -3 4 -0.40 1.79 0 -12 -3 4 1.20 1.20 0 12 3 -4 1.16 1.69 0 -11 -3 4 23.14 1.81 0 11 -3 -4 23.40 1.89 0 -11 -3 4 19.60 1.75 0 -11 3 4 25.06 2.31 0 11 3 -4 23.13 1.78 0 -10 -3 4 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22.50 1.75 0 -1 -3 4 22.73 2.41 0 -1 3 4 22.86 2.36 0 1 3 -4 23.85 1.80 0 0 -3 4 222.67 4.32 0 0 -3 -4 214.44 2.90 0 0 3 -4 226.81 4.17 0 0 3 4 215.45 2.90 0 0 3 -4 229.61 2.92 0 0 3 4 232.76 5.13 0 1 3 4 189.71 2.50 0 -1 3 -4 204.72 4.57 0 1 3 4 207.03 5.91 0 -1 3 -4 207.85 2.75 0 1 -3 4 202.38 4.29 0 -1 -3 -4 201.37 2.80 0 -2 3 -4 4.75 1.73 0 -2 3 -4 3.70 2.62 0 2 -3 4 3.86 2.54 0 -2 -3 -4 4.02 1.69 0 2 3 4 4.23 1.71 0 -3 -3 -4 69.84 2.10 0 -3 3 -4 77.23 2.10 0 3 3 4 74.45 2.12 0 -4 -3 -4 4.81 1.70 0 4 3 4 7.06 1.68 0 -4 3 -4 6.18 1.67 0 -5 -3 -4 91.88 4.64 0 -5 -3 -4 86.01 2.19 0 5 3 4 90.01 2.17 0 -5 3 -4 93.81 2.20 0 -6 -3 -4 35.23 3.27 0 -6 -3 -4 32.63 1.85 0 6 3 4 30.74 1.86 0 7 3 4 22.27 1.70 0 -7 -3 -4 21.83 1.83 0 -7 -3 -4 21.64 2.76 0 -8 -3 -4 61.38 1.64 0 8 3 4 60.83 2.01 0 -9 -3 -4 24.33 1.85 0 9 3 4 19.40 1.79 0 -10 -3 -4 59.00 2.04 0 10 3 4 60.55 1.99 0 -11 -3 -4 0.76 1.70 0 11 3 4 -0.47 1.71 0 -12 -3 -4 1.87 1.75 0 12 3 4 3.69 1.75 0 -13 -3 -4 0.18 1.71 0 13 3 4 0.86 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0 10 4 -4 26.70 1.84 0 -9 4 4 36.22 2.46 0 -9 -4 4 34.68 1.97 0 -9 4 4 35.25 2.09 0 -9 -4 4 34.48 1.82 0 9 4 -4 33.22 1.92 0 -8 4 4 1.49 1.99 0 8 4 -4 1.66 1.79 0 -8 4 4 1.23 1.63 0 -8 -4 4 -0.33 1.65 0 -8 -4 4 1.48 1.70 0 7 4 -4 10.39 1.82 0 -7 -4 4 9.49 1.76 0 -7 4 4 12.43 1.79 0 -7 -4 4 10.09 2.22 0 -7 4 4 9.92 2.18 0 -6 4 4 2.52 1.67 0 -6 -4 4 1.06 1.79 0 -6 4 4 3.04 1.73 0 6 4 -4 4.13 1.78 0 -6 -4 4 3.59 1.66 0 5 4 -4 18.59 1.91 0 5 4 -4 18.23 1.89 0 -5 4 4 18.59 1.83 0 -5 4 4 17.14 1.81 0 -5 -4 4 17.62 1.71 0 -5 -4 4 16.85 2.26 0 -4 -4 4 17.33 1.78 0 -4 -4 4 18.44 1.78 0 -4 4 4 16.85 1.77 0 4 4 -4 14.24 1.83 0 -4 4 4 18.00 2.18 0 4 4 -4 15.77 1.82 0 3 4 -4 3.99 1.67 0 -3 -4 4 5.32 1.71 0 3 -4 -4 4.88 1.74 0 -3 -4 4 5.76 2.05 0 3 4 -4 7.55 2.10 0 -3 4 4 4.42 1.75 0 -2 4 4 2.68 1.64 0 2 4 -4 0.12 1.71 0 -2 4 4 1.18 1.67 0 -2 -4 4 2.58 2.02 0 2 4 -4 1.28 1.63 0 2 -4 -4 1.77 1.70 0 -2 -4 4 0.93 1.54 0 1 -4 -4 1.46 1.76 0 1 4 -4 -0.36 1.13 0 -1 4 4 0.65 2.01 0 -1 -4 4 -0.25 1.64 0 -1 4 4 -0.90 2.07 0 1 4 -4 0.34 2.08 0 0 4 4 66.69 2.17 0 0 -4 -4 70.01 2.12 0 0 4 -4 68.67 2.80 0 0 -4 4 68.79 2.77 0 0 4 -4 73.45 2.04 0 0 4 4 73.48 3.18 0 1 4 4 9.47 2.58 0 1 -4 4 9.43 2.44 0 -1 -4 -4 10.75 1.77 0 -1 4 -4 10.49 2.58 0 1 4 4 9.79 1.71 0 -1 4 -4 10.94 1.65 0 2 4 4 15.16 1.63 0 -2 4 -4 12.93 2.71 0 2 -4 4 13.30 2.88 0 -2 -4 -4 15.06 1.65 0 -2 4 -4 15.40 1.63 0 -3 -4 -4 -0.46 1.54 0 -3 4 -4 0.21 3.74 0 3 -4 4 0.75 3.66 0 -3 4 -4 0.28 1.56 0 3 4 4 2.21 1.53 0 -4 -4 -4 183.13 2.59 0 4 4 4 185.19 2.55 0 -4 4 -4 197.14 2.30 0 5 4 4 1.26 1.57 0 -5 4 -4 0.06 1.64 0 -5 -4 -4 0.81 1.55 0 -6 -4 -4 144.82 2.46 0 6 4 4 154.42 2.47 0 -6 4 -4 168.05 2.50 0 -7 -4 -4 7.93 1.80 0 -7 4 -4 7.13 1.76 0 7 4 4 9.74 1.82 0 -7 -4 -4 7.35 3.05 0 -8 -4 -4 130.18 3.97 0 -8 -4 -4 116.51 2.38 0 8 4 4 127.63 2.37 0 -8 4 -4 131.60 2.38 0 -9 -4 -4 9.59 2.65 0 9 4 4 7.89 1.79 0 -9 -4 -4 9.59 1.77 0 10 4 4 42.38 1.58 0 -10 -4 -4 44.31 2.02 0 -10 -4 -4 48.17 2.80 0 11 4 4 19.83 1.89 0 -11 -4 -4 22.29 1.87 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5 39.33 1.54 0 13 3 -5 34.00 1.99 0 -13 3 5 37.36 2.02 0 -12 -3 5 7.77 1.68 0 -12 -3 5 6.45 1.27 0 -12 3 5 7.84 1.74 0 12 3 -5 7.26 1.75 0 12 -3 -5 8.66 2.13 0 -11 -3 5 8.64 1.15 0 -11 -3 5 11.24 1.71 0 -11 3 5 9.98 1.78 0 11 3 -5 9.44 1.70 0 11 -3 -5 8.50 1.72 0 10 3 -5 17.78 1.74 0 -10 -3 5 13.75 1.69 0 -10 -3 5 14.61 1.79 0 -10 3 5 15.65 1.78 0 -9 -3 5 -0.53 1.63 0 -9 3 5 0.12 1.72 0 9 3 -5 0.03 1.67 0 -9 3 5 0.92 2.08 0 -9 -3 5 -0.22 1.63 0 -8 3 5 8.81 1.80 0 -8 3 5 9.74 1.75 0 8 3 -5 10.25 1.73 0 -8 -3 5 10.70 1.75 0 -8 -3 5 10.35 1.68 0 -7 -3 5 24.09 1.75 0 -7 3 5 25.40 1.88 0 -7 -3 5 27.68 1.78 0 -7 3 5 24.61 1.84 0 7 3 -5 24.27 1.93 0 -6 3 5 6.04 1.72 0 -6 -3 5 7.02 2.01 0 -6 -3 5 7.57 1.67 0 6 3 -5 7.05 1.75 0 -6 3 5 8.03 1.67 0 5 3 -5 12.55 1.77 0 -5 -3 5 11.42 1.79 0 -5 -3 5 12.05 1.71 0 -5 3 5 13.63 1.74 0 -5 3 5 9.78 1.68 0 5 3 -5 13.55 1.74 0 -4 3 5 2.87 1.62 0 -4 3 5 0.35 1.62 0 4 3 -5 -0.21 1.66 0 4 3 -5 2.25 2.26 0 -4 -3 5 2.09 2.09 0 -4 -3 5 2.34 1.59 0 -3 -3 5 32.84 2.49 0 -3 3 5 31.19 1.82 0 3 3 -5 32.91 2.13 0 -3 -3 5 33.21 1.46 0 3 3 -5 33.09 1.90 0 -2 -3 5 103.75 3.09 0 2 -3 -5 106.36 2.33 0 -2 3 5 99.70 2.29 0 -2 -3 5 111.23 2.30 0 2 3 -5 107.67 2.79 0 2 3 -5 106.61 2.27 0 -1 -3 5 79.38 2.85 0 -1 3 5 76.30 2.14 0 1 -3 -5 81.05 2.17 0 -1 -3 5 81.78 2.07 0 1 3 -5 78.60 2.14 0 1 3 -5 76.38 2.92 0 0 3 5 35.94 1.87 0 0 3 -5 36.48 2.59 0 0 3 -5 34.89 1.87 0 0 -3 5 35.37 2.85 0 0 -3 -5 32.67 1.89 0 0 3 5 34.92 3.97 0 1 3 5 60.13 2.02 0 -1 3 -5 61.73 3.10 0 1 -3 5 62.97 3.13 0 -1 -3 -5 62.79 2.06 0 -1 3 -5 63.92 2.04 0 -2 -3 -5 20.85 1.75 0 2 3 5 18.86 1.73 0 -2 3 -5 21.69 2.87 0 2 -3 5 20.86 2.81 0 -2 3 -5 23.65 1.79 0 -3 -3 -5 24.89 1.80 0 3 3 5 26.29 1.81 0 -3 3 -5 26.83 1.83 0 3 -3 5 25.56 3.94 0 3 -3 5 25.82 3.87 0 4 3 5 150.50 2.43 0 -4 3 -5 154.11 2.17 0 -4 -3 -5 143.26 2.46 0 -5 -3 -5 34.83 1.80 0 -5 3 -5 29.61 1.47 0 5 3 5 28.21 1.84 0 -6 -3 -5 31.38 4.40 0 -6 -3 -5 32.37 1.83 0 6 3 5 31.64 1.79 0 -6 3 -5 30.01 1.78 0 -7 -3 -5 0.19 3.06 0 -7 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25.99 1.78 0 -2 4 5 4.16 1.68 0 2 -4 -5 3.68 1.75 0 -2 -4 5 3.44 1.58 0 -2 -4 5 3.31 2.04 0 2 4 -5 3.74 1.71 0 -2 4 5 3.12 2.11 0 2 4 -5 5.07 1.61 0 1 4 -5 0.47 1.60 0 1 -4 -5 -0.12 1.67 0 -1 4 5 1.34 1.67 0 -1 -4 5 2.17 1.73 0 1 4 -5 2.14 1.74 0 -1 4 5 0.77 2.40 0 0 4 -5 1.73 2.19 0 0 -4 5 1.93 2.40 0 0 -4 -5 0.74 1.67 0 0 4 -5 1.98 1.61 0 0 4 5 2.09 1.61 0 0 4 5 2.20 2.46 0 -1 4 -5 73.83 3.38 0 -1 -4 -5 72.56 2.07 0 1 -4 5 72.11 3.28 0 1 4 5 67.06 2.09 0 -1 4 -5 67.28 2.01 0 2 -4 5 44.86 3.37 0 -2 4 -5 45.51 3.51 0 -2 4 -5 45.75 1.90 0 -2 -4 -5 46.42 1.84 0 2 4 5 42.12 1.82 0 -3 -4 -5 5.74 1.59 0 -3 4 -5 4.05 1.71 0 3 4 5 3.38 1.51 0 -4 -4 -5 20.90 1.73 0 -4 4 -5 25.71 1.83 0 4 4 5 22.18 1.75 0 5 4 5 1.00 1.71 0 -5 4 -5 3.16 1.75 0 -5 -4 -5 1.12 1.74 0 -6 -4 -5 32.09 1.92 0 6 4 5 33.33 1.92 0 -6 4 -5 30.49 1.44 0 -7 4 -5 6.75 1.77 0 7 4 5 5.38 1.78 0 -7 -4 -5 4.05 1.24 0 -8 -4 -5 34.04 1.90 0 8 4 5 30.43 1.93 0 -8 4 -5 34.07 1.94 0 -8 -4 -5 34.79 4.18 0 9 4 5 2.11 1.78 0 -9 -4 -5 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2.34 2.16 0 -13 3 18 3.39 2.18 0 -13 3 18 1.79 1.58 0 -13 -3 18 0.84 2.20 0 -13 -3 18 2.63 2.19 0 12 3 -18 2.45 2.18 0 -12 3 18 0.79 2.15 0 -12 -3 18 -0.91 2.28 0 -12 -3 18 2.09 2.10 0 -12 3 18 -1.23 2.12 0 -12 3 18 0.50 2.76 0 11 3 -18 0.94 2.17 0 -11 3 18 1.04 2.19 0 -11 3 18 0.28 1.56 0 -11 -3 18 -0.05 2.71 0 -11 -3 18 0.67 2.07 0 -11 3 18 -0.44 2.23 0 10 3 -18 3.15 2.07 0 -10 3 18 -1.45 2.26 0 -10 3 18 0.69 2.19 0 -10 -3 18 -0.60 2.19 0 -10 -3 18 1.10 2.09 0 -10 3 18 -0.74 2.65 0 9 3 -18 0.52 2.16 0 -9 3 18 4.25 2.14 0 -9 3 18 3.69 2.15 0 -9 -3 18 1.31 2.22 0 -9 -3 18 2.06 2.14 0 -9 3 18 1.20 2.26 0 8 3 -18 0.00 2.17 0 -8 3 18 2.53 2.17 0 -8 3 18 -2.51 2.17 0 -8 -3 18 -2.20 2.22 0 -8 -3 18 4.00 2.13 0 -8 3 18 0.70 2.62 0 -7 3 18 -0.98 1.51 0 -7 3 18 0.56 2.16 0 -7 -3 18 1.97 2.13 0 -7 -3 18 -1.60 2.06 0 -7 3 18 1.40 3.05 0 -6 3 18 1.28 2.19 0 -6 -3 18 1.77 2.09 0 -6 -3 18 0.53 2.25 0 -6 -3 18 0.86 2.05 0 -6 3 18 0.39 3.04 0 -6 3 18 1.25 1.49 0 -5 3 18 5.92 2.15 0 -5 -3 18 0.08 2.21 0 -5 -3 18 2.57 2.25 0 -5 3 18 0.89 2.65 0 -5 -3 18 3.58 2.05 0 -5 3 18 0.36 1.55 0 -4 3 18 -1.52 2.24 0 -4 -3 18 -0.47 2.23 0 -4 3 18 -0.36 1.63 0 -4 -3 18 0.70 2.21 0 3 3 -18 0.40 1.46 0 -3 -3 18 0.54 2.16 0 -3 3 18 -0.50 2.17 0 -3 3 18 -0.26 2.13 0 -3 -3 18 0.53 2.19 0 2 3 -18 0.19 2.14 0 -2 3 18 -1.75 1.49 0 -2 3 18 2.03 2.16 0 -2 -3 18 -0.76 2.78 0 -2 -3 18 0.57 2.77 0 1 3 -18 1.64 2.18 0 -1 3 18 4.74 2.13 0 -1 -3 18 1.30 2.31 0 -1 3 18 -0.02 2.16 0 -1 -3 18 1.69 2.75 0 0 3 -18 0.83 2.12 0 0 -3 18 0.90 2.26 0 0 3 18 -0.66 2.18 0 0 3 18 4.53 2.16 0 0 -3 18 0.35 2.86 0 1 3 18 1.75 1.54 0 1 -3 18 -0.64 2.29 0 15 1 -19 -0.51 1.52 0 -15 -1 19 2.51 2.26 0 -15 1 19 -1.20 2.32 0 14 1 -19 2.45 2.20 0 -14 1 19 2.24 2.18 0 -14 1 19 2.14 2.19 0 -14 -1 19 0.45 2.24 0 -14 -1 19 3.19 2.24 0 -14 1 19 0.42 2.34 0 13 1 -19 1.15 2.14 0 -13 1 19 2.06 2.23 0 -13 1 19 1.88 2.26 0 -13 -1 19 3.81 2.12 0 -13 -1 19 1.84 2.12 0 -13 1 19 -1.06 2.25 0 12 1 -19 3.80 2.06 0 -12 1 19 1.58 2.14 0 -12 -1 19 1.52 2.12 0 -12 1 19 1.43 2.17 0 -12 -1 19 1.91 2.12 0 -12 1 19 -0.44 2.18 0 -11 1 19 -1.85 2.19 0 -11 1 19 -0.78 2.11 0 -11 -1 19 1.68 1.52 0 -11 -1 19 2.10 2.14 0 -11 1 19 1.23 2.16 0 -10 1 19 -1.09 2.16 0 -10 -1 19 -1.03 2.12 0 -10 1 19 1.32 2.06 0 -10 -1 19 -2.56 2.11 0 -10 1 19 1.95 2.17 0 -9 1 19 1.69 2.09 0 -9 1 19 1.70 2.15 0 -9 -1 19 1.26 2.16 0 -9 -1 19 2.08 2.08 0 -9 1 19 0.58 2.08 0 -9 -1 19 -1.69 2.14 0 -8 1 19 -0.15 2.00 0 -8 1 19 1.49 2.08 0 -8 -1 19 2.89 2.12 0 -8 -1 19 2.87 2.06 0 -8 -1 19 2.07 2.08 0 -8 1 19 1.93 2.69 0 -7 -1 19 2.11 2.14 0 -7 1 19 4.59 2.18 0 -7 -1 19 4.67 2.14 0 -7 -1 19 0.69 2.07 0 -7 1 19 2.68 2.18 0 -7 1 19 2.36 2.19 0 -6 1 19 2.21 2.01 0 -6 -1 19 1.30 2.06 0 -6 -1 19 1.72 2.08 0 -6 1 19 -1.61 2.00 0 -6 -1 19 0.14 2.11 0 -6 1 19 -0.32 2.63 0 -5 -1 19 6.94 2.08 0 -5 1 19 6.48 2.11 0 -5 1 19 6.33 2.14 0 -5 -1 19 4.89 2.11 0 -5 -1 19 3.42 2.08 0 -5 1 19 6.23 2.65 0 -4 1 19 -0.29 1.52 0 -4 1 19 1.91 2.06 0 -4 -1 19 0.82 2.15 0 -4 1 19 4.51 2.58 0 -4 -1 19 1.56 2.15 0 -4 -1 19 2.02 2.15 0 -3 1 19 3.01 2.00 0 -3 1 19 1.74 2.11 0 -3 -1 19 0.80 2.18 0 -3 -1 19 2.65 2.19 0 -2 -1 19 1.96 2.19 0 -2 1 19 3.78 2.10 0 -2 -1 19 1.85 2.20 0 -2 1 19 2.11 2.16 0 -1 -1 19 1.64 2.22 0 -1 1 19 0.03 2.15 0 -1 -1 19 -1.06 2.17 0 -1 1 19 0.73 2.09 0 0 1 19 0.02 2.16 0 0 -1 19 2.19 2.27 0 0 1 19 0.72 1.56 0 0 -1 19 3.24 2.21 0 -1 1 -19 2.52 2.30 0 1 1 19 4.74 2.24 0 1 -1 19 1.09 2.33 0 1 1 19 0.83 2.15 0 1 -1 19 0.79 2.29 0 2 1 19 2.89 2.23 0 2 -1 19 0.57 2.29 0 13 2 -19 1.05 2.27 0 -13 -2 19 -0.41 2.16 0 -13 2 19 0.06 2.30 0 12 2 -19 2.14 2.18 0 -12 2 19 -1.04 2.25 0 -12 2 19 1.86 2.25 0 -12 -2 19 3.32 2.18 0 -12 -2 19 -0.37 2.20 0 -12 2 19 -0.25 2.28 0 11 2 -19 4.71 2.16 0 -11 2 19 2.06 2.21 0 -11 2 19 1.71 2.18 0 -11 -2 19 1.36 2.22 0 -11 -2 19 4.83 2.15 0 -11 2 19 2.00 2.22 0 10 2 -19 2.83 2.10 0 -10 2 19 -0.74 2.24 0 -10 -2 19 2.18 2.22 0 -10 -2 19 -1.96 2.06 0 -10 2 19 0.24 2.20 0 -10 2 19 2.07 1.57 0 -9 2 19 7.49 2.19 0 -9 -2 19 7.61 2.18 0 -9 -2 19 4.66 2.17 0 -9 2 19 5.77 2.32 0 -9 2 19 7.28 2.74 0 -8 2 19 5.31 2.19 0 -8 2 19 1.24 2.12 0 -8 -2 19 4.18 2.18 0 -8 -2 19 1.87 2.14 0 -8 2 19 1.15 2.66 0 -8 -2 19 3.29 2.16 0 -7 2 19 1.18 2.08 0 -7 2 19 -2.05 2.14 0 -7 -2 19 -0.50 2.09 0 -7 -2 19 2.28 2.27 0 -7 -2 19 -3.21 2.01 0 -7 2 19 2.08 2.70 0 -6 -2 19 0.41 2.12 0 -6 2 19 0.63 2.13 0 -6 2 19 0.49 2.18 0 -6 -2 19 1.23 2.76 0 -6 -2 19 -0.03 2.11 0 -6 2 19 0.33 2.58 0 -5 2 19 0.77 2.19 0 -5 2 19 2.54 2.19 0 -5 -2 19 -0.28 2.23 0 -5 -2 19 1.37 2.24 0 -5 2 19 1.26 2.24 0 -5 -2 19 -0.24 2.13 0 -4 -2 19 1.52 2.26 0 -4 2 19 1.84 2.16 0 -4 -2 19 0.31 2.72 0 -4 -2 19 1.55 2.15 0 -4 2 19 4.11 2.18 0 -3 2 19 3.40 2.29 0 -3 -2 19 -0.03 2.25 0 -3 -2 19 3.08 2.27 0 -3 2 19 1.75 2.18 0 -2 2 19 2.15 2.20 0 -2 -2 19 -2.86 2.26 0 -2 -2 19 1.89 2.29 0 -2 2 19 0.87 2.18 0 -1 -2 19 1.28 2.26 0 -1 2 19 1.03 2.26 0 -1 -2 19 1.12 2.36 0 -1 2 19 -0.12 2.20 0 0 2 -19 3.46 2.17 0 0 2 19 1.24 2.19 0 0 -2 19 0.26 2.37 0 -11 0 20 2.60 2.24 0 -11 0 20 2.99 2.21 0 -11 0 20 0.55 2.30 0 -10 0 20 0.45 2.25 0 -10 0 20 -3.15 2.31 0 -10 0 20 -0.07 2.23 0 -9 0 20 0.88 2.21 0 -9 0 20 0.13 2.28 0 -9 0 20 1.44 2.20 0 -8 0 20 0.84 2.16 0 -8 0 20 -0.45 2.28 0 -8 0 20 -0.75 2.71 0 -7 0 20 1.81 2.21 0 -7 0 20 -0.08 2.24 0 -7 0 20 3.53 2.78 0 -6 0 20 1.69 2.22 0 -6 0 20 0.61 2.24 0 -6 0 20 4.96 2.18 0 -5 0 20 2.64 1.54 0 -5 0 20 0.16 2.17 0 -5 0 20 4.61 2.27 0 -4 0 20 16.96 2.24 0 -4 0 20 14.26 2.30 0 -3 0 20 -0.64 2.23 0 -3 0 20 1.44 2.22 0 -2 0 20 24.33 2.42 0 -10 -1 20 -0.30 1.53 0 -10 1 20 5.51 2.23 0 -10 -1 20 1.85 2.23 0 -10 1 20 -0.36 2.92 0 -9 1 20 1.26 2.22 0 -9 -1 20 -0.41 1.50 0 -9 1 20 -0.18 1.54 0 -9 -1 20 1.10 2.25 0 -9 -1 20 -0.89 2.15 0 -9 1 20 1.42 2.23 0 -8 1 20 4.92 2.35 0 -8 -1 20 7.66 2.30 0 -8 -1 20 2.66 2.31 0 -8 1 20 4.60 2.35 0 -8 1 20 3.29 2.23 0 -8 -1 20 3.98 2.30 0 -7 1 20 -0.45 2.21 0 -7 -1 20 1.76 2.20 0 -7 -1 20 2.78 2.21 0 -7 1 20 -0.78 2.20 0 -7 -1 20 0.57 2.22 0 -7 1 20 0.50 2.83 0 -6 -1 20 3.83 2.18 0 -6 1 20 5.77 2.31 0 -6 1 20 1.11 2.33 0 -6 -1 20 4.19 2.29 0 -6 -1 20 4.52 2.23 0 -6 1 20 4.50 2.27 0 -5 1 20 6.04 2.22 0 -5 1 20 2.20 2.24 0 -5 -1 20 3.02 2.30 0 -5 1 20 3.91 2.27 0 -5 -1 20 1.54 2.31 0 -5 -1 20 1.31 2.28 0 -4 1 20 3.70 2.17 0 -4 1 20 2.19 2.28 0 -4 -1 20 -0.92 2.19 0 -4 -1 20 0.83 2.29 0 ; _shelx_hkl_checksum 27689 _shelx_res_file ; TITL necmi127 in P 21/c shelx.res created by SHELXL-2016/6 at 14:21:00 on 26-Oct-2016 CELL 0.71073 20.7156 6.3660 16.0288 90.000 105.183 90.000 ZERR 4.00 0.0011 0.0003 0.0007 0.000 0.004 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 92 56 16 28 MERG 2 OMIT -4.00 52.00 eqiv $1 x,5/2-y,-1/2+z eqiv $2 -x,+y-1/2,-z+1/2 htab c4 o5_$1 htab c22 o4_$2 HTAB N2 O7 HTAB N2 O3 FMAP 2 PLAN 5 ACTA BOND $H CONF L.S. 10 WGHT 0.042400 FVAR 0.42055 N2 3 0.257244 0.800160 0.433322 11.00000 0.05855 0.05896 = 0.04804 -0.00873 0.00526 -0.00540 MOLE 1 C1 1 0.212650 0.575821 0.181201 11.00000 0.07006 0.05477 = 0.04698 -0.00319 0.00872 -0.00277 AFIX 43 H1 2 0.254927 0.632079 0.204818 11.00000 -1.20000 AFIX 0 C2 1 0.197290 0.376292 0.205270 11.00000 0.05113 0.05275 = 0.04310 -0.00472 0.00981 -0.00334 C3 1 0.165313 0.690765 0.122316 11.00000 0.10183 0.05965 = 0.05507 0.00415 0.01170 0.01348 AFIX 43 H3 2 0.175939 0.823402 0.105522 11.00000 -1.20000 AFIX 0 C4 1 0.102452 0.609306 0.088464 11.00000 0.08309 0.09842 = 0.05765 0.00136 0.00285 0.03247 AFIX 43 H4 2 0.070570 0.687627 0.049082 11.00000 -1.20000 AFIX 0 C5 1 0.086472 0.413773 0.112319 11.00000 0.05584 0.10851 = 0.06470 -0.00590 0.00414 0.00687 AFIX 43 H5 2 0.043669 0.360337 0.089719 11.00000 -1.20000 AFIX 0 C6 1 0.133657 0.296234 0.169683 11.00000 0.05467 0.07232 = 0.05585 -0.00602 0.01096 -0.00579 AFIX 43 H6 2 0.122890 0.162162 0.184765 11.00000 -1.20000 AFIX 0 C7 1 0.379437 -0.041005 0.261183 11.00000 0.05427 0.08042 = 0.07339 -0.01389 0.00592 0.00423 AFIX 43 H7 2 0.338362 -0.008307 0.223342 11.00000 -1.20000 AFIX 0 C8 1 0.414328 -0.214975 0.245976 11.00000 0.07052 0.07885 = 0.09184 -0.02227 0.02452 -0.00304 AFIX 43 H8 2 0.396471 -0.299188 0.198079 11.00000 -1.20000 AFIX 0 C9 1 0.474929 -0.264823 0.300654 11.00000 0.07750 0.07339 = 0.09296 0.00414 0.03481 0.01373 AFIX 43 H9 2 0.497450 -0.385144 0.291138 11.00000 -1.20000 AFIX 0 C10 1 0.502276 -0.137222 0.369322 11.00000 0.06889 0.09960 = 0.07384 0.01177 0.01453 0.02587 AFIX 43 H10 2 0.544155 -0.168646 0.405455 11.00000 -1.20000 AFIX 0 C11 1 0.468342 0.037371 0.385422 11.00000 0.06154 0.08271 = 0.05695 0.00168 0.00821 0.00751 AFIX 43 H11 2 0.487764 0.123857 0.431993 11.00000 -1.20000 AFIX 0 C12 1 0.405337 0.086104 0.332890 11.00000 0.05297 0.05749 = 0.05138 0.00451 0.00964 0.00024 C13 1 0.368777 0.264304 0.354824 11.00000 0.05635 0.05733 = 0.04389 0.00132 0.00489 -0.00696 C14 1 0.305136 0.339406 0.327971 11.00000 0.05279 0.04802 = 0.04494 0.00222 0.00730 -0.00435 C15 1 0.246876 0.242257 0.265175 11.00000 0.05123 0.04797 = 0.04751 -0.00194 0.01390 -0.00616 C16 1 0.302214 0.523919 0.379663 11.00000 0.05586 0.05115 = 0.04591 -0.00004 0.00833 -0.00593 C17 1 0.369754 0.550523 0.438055 11.00000 0.05945 0.06228 = 0.05206 -0.00532 0.00815 -0.00705 C18 1 0.205891 0.938925 0.424661 11.00000 0.05716 0.05627 = 0.04413 -0.00043 0.01282 -0.00418 C19 1 0.212479 1.129700 0.470722 11.00000 0.05886 0.05882 = 0.04337 -0.00248 0.01131 -0.00872 C20 1 0.160585 1.272254 0.457492 11.00000 0.07411 0.05656 = 0.05580 -0.00005 0.02280 -0.00383 AFIX 43 H20 2 0.165872 1.397959 0.488098 11.00000 -1.20000 AFIX 0 C21 1 0.101753 1.227022 0.399338 11.00000 0.06595 0.06372 = 0.05838 0.00851 0.01990 0.00399 C22 1 0.092789 1.040065 0.353645 11.00000 0.05820 0.08520 = 0.05299 0.00195 0.01030 -0.00677 AFIX 43 H22 2 0.052003 1.010889 0.314458 11.00000 -1.20000 AFIX 0 C23 1 0.143854 0.898965 0.366225 11.00000 0.05916 0.06532 = 0.05323 -0.00862 0.01015 -0.00677 AFIX 43 H23 2 0.137415 0.773540 0.335401 11.00000 -1.20000 AFIX 0 N1 3 0.249586 0.635631 0.377835 11.00000 0.06116 0.05006 = 0.04682 -0.00501 0.01054 -0.00683 N3 3 0.047222 1.380587 0.383990 11.00000 0.07861 0.08113 = 0.08924 0.02144 0.02607 0.01189 N4 3 0.274003 1.190650 0.532435 11.00000 0.06953 0.06987 = 0.05603 -0.01164 0.01357 -0.01014 O1 4 0.239275 0.052242 0.264644 11.00000 0.06531 0.04670 = 0.07604 0.00043 0.01365 -0.00902 O2 4 0.408190 0.389755 0.420487 11.00000 0.05583 0.06797 = 0.05643 -0.00813 -0.00079 -0.00226 O3 4 0.391132 0.679077 0.492836 11.00000 0.07013 0.08471 = 0.06786 -0.02453 0.00108 -0.01094 O4 4 -0.001842 1.348175 0.324193 11.00000 0.08658 0.12877 = 0.11156 0.02987 0.00592 0.02437 O5 4 0.053555 1.531870 0.431566 11.00000 0.11772 0.09060 = 0.16624 -0.02047 0.03031 0.02967 O6 4 0.277478 1.365250 0.565284 11.00000 0.10579 0.07199 = 0.08139 -0.02720 0.00535 -0.01411 O7 4 0.320909 1.067380 0.549515 11.00000 0.06713 0.10460 = 0.09507 -0.03982 -0.00632 0.00458 MOLE 0 H25 2 0.296341 0.826643 0.467390 11.00000 0.07441 HKLF 4 REM necmi127 in P 21/c REM R1 = 0.0385 for 2617 Fo > 4sig(Fo) and 0.0736 for all 3992 data REM 311 parameters refined using 0 restraints END WGHT 0.0424 0.0000 REM Highest difference peak 0.112, deepest hole -0.147, 1-sigma level 0.033 Q1 1 0.4280 -0.0679 0.3823 11.00000 0.05 0.11 Q2 1 0.1977 0.7352 0.2425 11.00000 0.05 0.10 Q3 1 0.3826 -0.2716 0.0912 11.00000 0.05 0.10 Q4 1 0.1521 1.3059 0.5423 11.00000 0.05 0.10 Q5 1 0.3457 0.0857 0.1952 11.00000 0.05 0.10 ; _shelx_res_checksum 68852 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_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 N N2 0.25724(8) 0.8002(2) 0.43332(9) 0.0568(4) Uani d 1 C C1 0.21265(9) 0.5758(3) 0.18120(10) 0.0585(4) Uani d 1 H H1 0.254927 0.632079 0.204818 0.070 Uiso calc 1 C C2 0.19729(8) 0.3763(2) 0.20527(9) 0.0495(4) Uani d 1 C C3 0.16531(11) 0.6908(3) 0.12232(11) 0.0738(6) Uani d 1 H H3 0.175939 0.823402 0.105522 0.089 Uiso calc 1 C C4 0.10245(12) 0.6093(4) 0.08846(12) 0.0826(6) Uani d 1 H H4 0.070570 0.687627 0.049082 0.099 Uiso calc 1 C C5 0.08647(10) 0.4138(4) 0.11232(12) 0.0785(6) Uani d 1 H H5 0.043669 0.360337 0.089719 0.094 Uiso calc 1 C C6 0.13366(9) 0.2962(3) 0.16968(10) 0.0616(4) Uani d 1 H H6 0.122890 0.162162 0.184765 0.074 Uiso calc 1 C C7 0.37944(10) -0.0410(3) 0.26118(12) 0.0714(5) Uani d 1 H H7 0.338362 -0.008307 0.223342 0.086 Uiso calc 1 C C8 0.41433(11) -0.2150(3) 0.24598(14) 0.0798(6) Uani d 1 H H8 0.396471 -0.299188 0.198079 0.096 Uiso calc 1 C C9 0.47493(11) -0.2648(3) 0.30065(14) 0.0789(6) Uani d 1 H H9 0.497450 -0.385144 0.291138 0.095 Uiso calc 1 C C10 0.50228(11) -0.1372(4) 0.36932(13) 0.0816(6) Uani d 1 H H10 0.544155 -0.168646 0.405455 0.098 Uiso calc 1 C C11 0.46834(9) 0.0374(3) 0.38542(11) 0.0684(5) Uani d 1 H H11 0.487764 0.123857 0.431993 0.082 Uiso calc 1 C C12 0.40534(8) 0.0861(3) 0.33289(10) 0.0547(4) Uani d 1 C C13 0.36878(9) 0.2643(3) 0.35482(9) 0.0541(4) Uani d 1 C C14 0.30514(8) 0.3394(2) 0.32797(9) 0.0496(4) Uani d 1 C C15 0.24688(8) 0.2423(2) 0.26518(9) 0.0487(4) Uani d 1 C C16 0.30221(9) 0.5239(2) 0.37966(9) 0.0519(4) Uani d 1 C C17 0.36975(9) 0.5505(3) 0.43806(11) 0.0591(4) Uani d 1 C C18 0.20589(9) 0.9389(3) 0.42466(9) 0.0526(4) Uani d 1 C C19 0.21248(8) 1.1297(3) 0.47072(9) 0.0541(4) Uani d 1 C C20 0.16058(10) 1.2723(3) 0.45749(11) 0.0611(5) Uani d 1 H H20 0.165872 1.397959 0.488098 0.073 Uiso calc 1 C C21 0.10175(10) 1.2270(3) 0.39934(11) 0.0620(5) Uani d 1 C C22 0.09279(9) 1.0401(3) 0.35364(11) 0.0663(5) Uani d 1 H H22 0.052003 1.010889 0.314458 0.080 Uiso calc 1 C C23 0.14385(9) 0.8990(3) 0.36622(10) 0.0601(4) Uani d 1 H H23 0.137415 0.773540 0.335401 0.072 Uiso calc 1 N N1 0.24959(7) 0.6356(2) 0.37783(8) 0.0534(3) Uani d 1 N N3 0.04722(10) 1.3806(3) 0.38399(13) 0.0822(5) Uani d 1 N N4 0.27400(8) 1.1906(3) 0.53243(9) 0.0657(4) Uani d 1 O O1 0.23927(6) 0.05224(18) 0.26464(7) 0.0636(3) Uani d 1 O O2 0.40819(6) 0.38975(19) 0.42049(7) 0.0630(3) Uani d 1 O O3 0.39113(6) 0.6791(2) 0.49284(8) 0.0774(4) Uani d 1 O O4 -0.00184(9) 1.3482(3) 0.32419(12) 0.1127(6) Uani d 1 O O5 0.05355(10) 1.5319(3) 0.43157(14) 0.1261(7) Uani d 1 O O6 0.27748(8) 1.3652(2) 0.56528(9) 0.0900(4) Uani d 1 O O7 0.32091(7) 1.0674(3) 0.54951(9) 0.0941(5) Uani d 1 H H25 0.2963(10) 0.827(3) 0.4674(12) 0.074(6) 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 N2 0.0586(10) 0.0590(9) 0.0480(7) -0.0054(8) 0.0053(7) -0.0087(7) C1 0.0701(11) 0.0548(10) 0.0470(8) -0.0028(9) 0.0087(8) -0.0032(8) C2 0.0511(10) 0.0527(9) 0.0431(8) -0.0033(8) 0.0098(7) -0.0047(7) C3 0.1018(17) 0.0596(11) 0.0551(10) 0.0135(11) 0.0117(11) 0.0042(9) C4 0.0831(16) 0.0984(17) 0.0576(11) 0.0325(13) 0.0029(10) 0.0014(11) C5 0.0558(12) 0.1085(17) 0.0647(11) 0.0069(12) 0.0041(9) -0.0059(12) C6 0.0547(11) 0.0723(12) 0.0559(9) -0.0058(9) 0.0110(8) -0.0060(8) C7 0.0543(11) 0.0804(13) 0.0734(12) 0.0042(10) 0.0059(9) -0.0139(10) C8 0.0705(14) 0.0788(14) 0.0918(14) -0.0030(11) 0.0245(12) -0.0223(11) C9 0.0775(15) 0.0734(13) 0.0930(14) 0.0137(11) 0.0348(12) 0.0041(12) C10 0.0689(13) 0.0996(16) 0.0738(12) 0.0259(12) 0.0145(10) 0.0118(12) C11 0.0615(12) 0.0827(13) 0.0570(10) 0.0075(10) 0.0082(9) 0.0017(9) C12 0.0530(10) 0.0575(10) 0.0514(9) 0.0002(8) 0.0096(8) 0.0045(8) C13 0.0563(11) 0.0573(10) 0.0439(8) -0.0070(8) 0.0049(7) 0.0013(7) C14 0.0528(10) 0.0480(9) 0.0449(8) -0.0044(8) 0.0073(7) 0.0022(7) C15 0.0512(10) 0.0480(10) 0.0475(8) -0.0062(8) 0.0139(7) -0.0019(7) C16 0.0559(10) 0.0512(9) 0.0459(8) -0.0059(8) 0.0083(7) 0.0000(7) C17 0.0594(11) 0.0623(11) 0.0521(9) -0.0070(9) 0.0081(8) -0.0053(8) C18 0.0572(10) 0.0563(10) 0.0441(8) -0.0042(8) 0.0128(7) -0.0004(7) C19 0.0589(10) 0.0588(10) 0.0434(8) -0.0087(9) 0.0113(7) -0.0025(8) C20 0.0741(13) 0.0566(10) 0.0558(9) -0.0038(10) 0.0228(9) -0.0001(8) C21 0.0660(12) 0.0637(11) 0.0584(10) 0.0040(9) 0.0199(9) 0.0085(9) C22 0.0582(11) 0.0852(13) 0.0530(9) -0.0068(10) 0.0103(8) 0.0019(9) C23 0.0592(11) 0.0653(11) 0.0532(9) -0.0068(9) 0.0101(8) -0.0086(8) N1 0.0612(9) 0.0501(8) 0.0468(7) -0.0068(7) 0.0105(6) -0.0050(6) N3 0.0786(13) 0.0811(13) 0.0892(12) 0.0119(11) 0.0261(10) 0.0214(11) N4 0.0695(11) 0.0699(11) 0.0560(8) -0.0101(9) 0.0136(8) -0.0116(8) O1 0.0653(8) 0.0467(7) 0.0760(7) -0.0090(6) 0.0136(6) 0.0004(6) O2 0.0558(7) 0.0680(8) 0.0564(6) -0.0023(6) -0.0008(5) -0.0081(6) O3 0.0701(8) 0.0847(9) 0.0679(7) -0.0109(7) 0.0011(6) -0.0245(7) O4 0.0866(12) 0.1288(14) 0.1116(12) 0.0244(11) 0.0059(10) 0.0299(11) O5 0.1177(15) 0.0906(12) 0.1662(18) 0.0297(11) 0.0303(13) -0.0205(12) O6 0.1058(12) 0.0720(9) 0.0814(9) -0.0141(8) 0.0054(8) -0.0272(8) O7 0.0671(9) 0.1046(11) 0.0951(10) 0.0046(9) -0.0063(8) -0.0398(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle N1 N2 C18 118.69(14) N1 N2 H25 119.5(13) C18 N2 H25 121.0(13) C3 C1 C2 120.12(17) C3 C1 H1 119.9 C2 C1 H1 119.9 C1 C2 C6 118.92(15) C1 C2 C15 122.50(14) C6 C2 C15 118.55(15) C4 C3 C1 120.01(19) C4 C3 H3 120.0 C1 C3 H3 120.0 C5 C4 C3 120.44(19) C5 C4 H4 119.8 C3 C4 H4 119.8 C4 C5 C6 120.03(19) C4 C5 H5 120.0 C6 C5 H5 120.0 C5 C6 C2 120.47(18) C5 C6 H6 119.8 C2 C6 H6 119.8 C8 C7 C12 120.40(18) C8 C7 H7 119.8 C12 C7 H7 119.8 C9 C8 C7 120.61(19) C9 C8 H8 119.7 C7 C8 H8 119.7 C10 C9 C8 119.74(19) C10 C9 H9 120.1 C8 C9 H9 120.1 C9 C10 C11 120.49(19) C9 C10 H10 119.8 C11 C10 H10 119.8 C10 C11 C12 120.77(18) C10 C11 H11 119.6 C12 C11 H11 119.6 C11 C12 C7 117.88(17) C11 C12 C13 119.49(15) C7 C12 C13 122.62(15) C14 C13 O2 111.27(14) C14 C13 C12 135.91(15) O2 C13 C12 112.81(14) C13 C14 C16 106.62(14) C13 C14 C15 127.89(14) C16 C14 C15 125.17(15) O1 C15 C2 120.07(14) O1 C15 C14 119.81(14) C2 C15 C14 120.09(13) N1 C16 C14 126.40(14) N1 C16 C17 127.16(15) C14 C16 C17 106.34(15) O3 C17 O2 122.55(16) O3 C17 C16 130.62(17) O2 C17 C16 106.82(14) N2 C18 C23 120.38(15) N2 C18 C19 122.67(15) C23 C18 C19 116.92(16) C20 C19 C18 121.43(15) C20 C19 N4 116.10(15) C18 C19 N4 122.44(16) C21 C20 C19 119.29(16) C21 C20 H20 120.4 C19 C20 H20 120.4 C20 C21 C22 121.18(17) C20 C21 N3 119.20(18) C22 C21 N3 119.61(18) C23 C22 C21 119.83(17) C23 C22 H22 120.1 C21 C22 H22 120.1 C22 C23 C18 121.34(16) C22 C23 H23 119.3 C18 C23 H23 119.3 C16 N1 N2 117.12(14) O5 N3 O4 124.0(2) O5 N3 C21 118.2(2) O4 N3 C21 117.8(2) O7 N4 O6 122.19(16) O7 N4 C19 119.14(15) O6 N4 C19 118.67(17) C17 O2 C13 108.93(13) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance N2 N1 1.3562(18) N2 C18 1.362(2) N2 H25 0.87(2) C1 C3 1.380(2) C1 C2 1.388(2) C1 H1 0.9300 C2 C6 1.389(2) C2 C15 1.479(2) C3 C4 1.374(3) C3 H3 0.9300 C4 C5 1.368(3) C4 H4 0.9300 C5 C6 1.375(3) C5 H5 0.9300 C6 H6 0.9300 C7 C8 1.379(3) C7 C12 1.393(2) C7 H7 0.9300 C8 C9 1.367(3) C8 H8 0.9300 C9 C10 1.366(3) C9 H9 0.9300 C10 C11 1.375(3) C10 H10 0.9300 C11 C12 1.390(2) C11 H11 0.9300 C12 C13 1.457(2) C13 C14 1.362(2) C13 O2 1.4007(18) C14 C16 1.448(2) C14 C15 1.489(2) C15 O1 1.2196(17) C16 N1 1.296(2) C16 C17 1.475(2) C17 O3 1.1972(19) C17 O2 1.370(2) C18 C23 1.401(2) C18 C19 1.409(2) C19 C20 1.380(2) C19 N4 1.447(2) C20 C21 1.357(2) C20 H20 0.9300 C21 C22 1.384(2) C21 N3 1.465(2) C22 C23 1.362(2) C22 H22 0.9300 C23 H23 0.9300 N3 O5 1.214(2) N3 O4 1.218(2) N4 O7 1.2230(19) N4 O6 1.2239(18) 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 C4 H4 O5 4_585 0.93 2.55 3.352(3) 144.3 C22 H22 O4 2_545 0.93 2.43 3.218(2) 143.1 N2 H25 O7 . 0.87(2) 1.997(19) 2.6106(19) 126.8(16) N2 H25 O3 . 0.87(2) 2.118(19) 2.795(2) 134.5(17) 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 C3 C1 C2 C6 -0.5(2) C3 C1 C2 C15 177.30(15) C2 C1 C3 C4 1.1(3) C1 C3 C4 C5 -0.4(3) C3 C4 C5 C6 -0.8(3) C4 C5 C6 C2 1.4(3) C1 C2 C6 C5 -0.7(2) C15 C2 C6 C5 -178.63(15) C12 C7 C8 C9 -0.3(3) C7 C8 C9 C10 -2.3(3) C8 C9 C10 C11 2.1(3) C9 C10 C11 C12 0.8(3) C10 C11 C12 C7 -3.3(3) C10 C11 C12 C13 176.04(17) C8 C7 C12 C11 3.1(3) C8 C7 C12 C13 -176.23(17) C11 C12 C13 C14 -168.59(18) C7 C12 C13 C14 10.7(3) C11 C12 C13 O2 10.6(2) C7 C12 C13 O2 -170.12(15) O2 C13 C14 C16 -0.67(17) C12 C13 C14 C16 178.51(17) O2 C13 C14 C15 -174.42(14) C12 C13 C14 C15 4.8(3) C1 C2 C15 O1 -157.59(15) C6 C2 C15 O1 20.2(2) C1 C2 C15 C14 24.2(2) C6 C2 C15 C14 -158.02(14) C13 C14 C15 O1 38.1(2) C16 C14 C15 O1 -134.56(16) C13 C14 C15 C2 -143.63(16) C16 C14 C15 C2 43.7(2) C13 C14 C16 N1 -175.98(15) C15 C14 C16 N1 -2.0(2) C13 C14 C16 C17 0.59(17) C15 C14 C16 C17 174.56(14) N1 C16 C17 O3 -2.5(3) C14 C16 C17 O3 -179.04(18) N1 C16 C17 O2 176.23(15) C14 C16 C17 O2 -0.31(17) N1 N2 C18 C23 7.3(2) N1 N2 C18 C19 -170.66(14) N2 C18 C19 C20 176.72(15) C23 C18 C19 C20 -1.3(2) N2 C18 C19 N4 -1.5(2) C23 C18 C19 N4 -179.50(14) C18 C19 C20 C21 0.5(2) N4 C19 C20 C21 178.85(14) C19 C20 C21 C22 0.5(3) C19 C20 C21 N3 -178.66(14) C20 C21 C22 C23 -0.7(3) N3 C21 C22 C23 178.48(15) C21 C22 C23 C18 -0.2(3) N2 C18 C23 C22 -176.95(15) C19 C18 C23 C22 1.1(2) C14 C16 N1 N2 178.37(14) C17 C16 N1 N2 2.5(2) C18 N2 N1 C16 170.45(14) C20 C21 N3 O5 -9.0(3) C22 C21 N3 O5 171.81(19) C20 C21 N3 O4 171.09(17) C22 C21 N3 O4 -8.1(3) C20 C19 N4 O7 177.08(16) C18 C19 N4 O7 -4.6(2) C20 C19 N4 O6 -3.5(2) C18 C19 N4 O6 174.77(15) O3 C17 O2 C13 178.77(16) C16 C17 O2 C13 -0.08(17) C14 C13 O2 C17 0.49(18) C12 C13 O2 C17 -178.90(13) _cod_database_fobs_code 2241963