#------------------------------------------------------------------------------ #$Date: 2014-03-11 15:54:26 +0000 (Tue, 11 Mar 2014) $ #$Revision: 104860 $ #$URL: svn://www.crystallography.net/cod/cif/2/23/90/2239028.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_2239028 loop_ _publ_author_name 'Mague, Joel T.' 'Abdel-Aziz, Alaa A.-M.' 'El-Azab, Adel S.' 'Al-Swaidan, Ibrahim A.' _publ_section_title ; 2-Methoxy-4,6-diphenylnicotinonitrile ; _journal_coeditor_code LH5683 _journal_issue 2 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o228 _journal_paper_doi 10.1107/S1600536814001755 _journal_volume 70 _journal_year 2014 _chemical_formula_iupac 'C19 H14 N2 O' _chemical_formula_moiety 'C19 H14 N2 O' _chemical_formula_sum 'C19 H14 N2 O' _chemical_formula_weight 286.32 _chemical_name_systematic ; 2-Methoxy-4,6-diphenylnicotinonitrile ; _space_group_IT_number 18 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2 2ab' _symmetry_space_group_name_H-M 'P 21 21 2' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 15.0686(16) _cell_length_b 24.327(3) _cell_length_c 3.8986(4) _cell_measurement_reflns_used 7963 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.36 _cell_measurement_theta_min 2.70 _cell_volume 1429.1(3) _computing_cell_refinement 'SAINT (Bruker, 2009)' _computing_data_collection 'APEX2 (Bruker, 2010)' _computing_data_reduction 'SAINT (Bruker, 2009)' _computing_molecular_graphics 'DIAMOND (Brandenburg & Putz, 2012)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.957 _diffrn_measurement_device_type 'Bruker SMART APEXII CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_number 12356 _diffrn_reflns_theta_full 27.50 _diffrn_reflns_theta_max 28.46 _diffrn_reflns_theta_min 1.59 _exptl_absorpt_coefficient_mu 0.084 _exptl_absorpt_correction_T_max 0.9950 _exptl_absorpt_correction_T_min 0.9818 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 2009)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.331 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 600 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.06 _refine_diff_density_max 0.199 _refine_diff_density_min -0.213 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 200 _refine_ls_number_reflns 3344 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.036 _refine_ls_R_factor_all 0.0481 _refine_ls_R_factor_gt 0.0404 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+0.4770P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0880 _refine_ls_wR_factor_ref 0.0933 _reflns_number_gt 2983 _reflns_number_total 3344 _reflns_threshold_expression I>2\s(I) _iucr_refine_instructions_details ; TITL jtm380_1m in P2(1)2(1)2 CELL 0.71073 15.0686 24.3270 3.8986 90.000 90.000 90.000 ZERR 4.00 0.0016 0.0026 0.0004 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, Z SYMM 0.5-X, 0.5+Y, -Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H N O UNIT 76 56 8 4 L.S. 4 ACTA 55 BOND $H FMAP 2 PLAN 5 HTAB SIZE 0.06 0.11 0.22 TEMP -173 MPLA C8 C9 C10 C11 C12 C13 MPLA C1 C2 C3 C4 C5 N1 MPLA C14 C15 C16 C17 C18 C19 CONF WGHT 0.032500 0.477000 FVAR 0.23264 MOLE 1 O1 4 0.430175 0.120533 0.058902 11.00000 0.01906 0.02013 = 0.03883 0.00002 -0.00330 -0.00359 N1 3 0.575176 0.113175 0.241522 11.00000 0.02035 0.01942 = 0.02409 -0.00180 0.00082 -0.00072 N2 3 0.388847 0.244953 -0.303791 11.00000 0.02363 0.02694 = 0.03447 -0.00021 -0.00475 0.00059 C1 1 0.656577 0.136599 0.275286 11.00000 0.01928 0.02011 = 0.01718 -0.00318 0.00125 0.00110 C2 1 0.672687 0.190497 0.176203 11.00000 0.01834 0.02014 = 0.01969 -0.00318 -0.00027 -0.00044 AFIX 43 H2 2 0.730247 0.205762 0.204661 11.00000 -1.20000 AFIX 0 C3 1 0.604878 0.222451 0.034961 11.00000 0.02081 0.01991 = 0.01605 -0.00239 0.00195 0.00119 C4 1 0.521802 0.197665 -0.008404 11.00000 0.01836 0.01993 = 0.02104 -0.00243 -0.00028 0.00185 C5 1 0.511983 0.142860 0.103573 11.00000 0.01722 0.02133 = 0.02372 -0.00374 0.00179 -0.00158 C6 1 0.417627 0.066233 0.195558 11.00000 0.02536 0.02238 = 0.04512 0.00209 -0.00313 -0.00586 AFIX 137 H6A 2 0.455695 0.040262 0.071956 11.00000 -1.50000 H6B 2 0.355390 0.055386 0.168346 11.00000 -1.50000 H6C 2 0.433238 0.066014 0.439577 11.00000 -1.50000 AFIX 0 C7 1 0.447935 0.224424 -0.169731 11.00000 0.02058 0.01981 = 0.02411 -0.00134 0.00166 -0.00175 C8 1 0.726803 0.101154 0.425039 11.00000 0.02067 0.01941 = 0.01816 -0.00298 -0.00020 0.00072 C9 1 0.704566 0.050360 0.568938 11.00000 0.02246 0.02138 = 0.02410 -0.00099 0.00196 -0.00074 AFIX 43 H9 2 0.644167 0.039224 0.576155 11.00000 -1.20000 AFIX 0 C10 1 0.769451 0.016067 0.701106 11.00000 0.02959 0.02006 = 0.02536 0.00170 0.00213 0.00186 AFIX 43 H10 2 0.753395 -0.018383 0.797628 11.00000 -1.20000 AFIX 0 C11 1 0.858056 0.031958 0.692816 11.00000 0.02684 0.02524 = 0.02486 0.00187 -0.00053 0.00564 AFIX 43 H11 2 0.902783 0.008452 0.782133 11.00000 -1.20000 AFIX 0 C12 1 0.880431 0.082480 0.552792 11.00000 0.02259 0.02858 = 0.02769 -0.00098 -0.00365 0.00045 AFIX 43 H12 2 0.940862 0.093573 0.547270 11.00000 -1.20000 AFIX 0 C13 1 0.816006 0.116850 0.421354 11.00000 0.02486 0.01942 = 0.02591 0.00030 -0.00120 -0.00147 AFIX 43 H13 2 0.832416 0.151437 0.327669 11.00000 -1.20000 AFIX 0 C14 1 0.622835 0.280467 -0.062694 11.00000 0.02069 0.01913 = 0.01722 -0.00088 -0.00313 0.00040 C15 1 0.562251 0.322393 0.011663 11.00000 0.02094 0.02240 = 0.02220 -0.00163 -0.00046 -0.00063 AFIX 43 H15 2 0.507730 0.314030 0.122334 11.00000 -1.20000 AFIX 0 C16 1 0.582173 0.376269 -0.077020 11.00000 0.02636 0.02007 = 0.02455 -0.00132 -0.00326 0.00240 AFIX 43 H16 2 0.541318 0.404794 -0.024463 11.00000 -1.20000 AFIX 0 C17 1 0.660933 0.388757 -0.241107 11.00000 0.03311 0.02021 = 0.02381 0.00204 -0.00551 -0.00418 AFIX 43 H17 2 0.673651 0.425703 -0.302875 11.00000 -1.20000 AFIX 0 C18 1 0.721409 0.347546 -0.315802 11.00000 0.02332 0.02682 = 0.02215 0.00075 -0.00091 -0.00449 AFIX 43 H18 2 0.775292 0.356089 -0.430528 11.00000 -1.20000 AFIX 0 C19 1 0.702851 0.293784 -0.222200 11.00000 0.02114 0.02250 = 0.02029 -0.00322 -0.00134 0.00087 AFIX 43 H19 2 0.745094 0.265707 -0.267189 11.00000 -1.20000 AFIX 0 HKLF 4 REM jtm380_1m in P2(1)2(1)2 REM R1 = 0.0404 for 2982 Fo > 4sig(Fo) and 0.0481 for all 3344 data REM 200 parameters refined using 0 restraints END WGHT 0.0323 0.4787 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.199, deepest hole -0.213, 1-sigma level 0.042 Q1 1 0.6904 0.1126 0.2819 11.00000 0.05 0.20 Q2 1 0.6380 0.1985 0.0174 11.00000 0.05 0.20 Q3 1 0.8162 0.0278 0.8345 11.00000 0.05 0.20 Q4 1 0.7726 0.1085 0.2936 11.00000 0.05 0.18 Q5 1 0.6649 0.1634 0.2201 11.00000 0.05 0.18 ; _[local]_cod_data_source_file lh5683sup1.cif _[local]_cod_data_source_block I _cod_database_code 2239028 _shelx_hkl_checksum 94884 _shelx_hkl_file ; 0 0 1 171.14 6.46 0 0 -1 165.86 6.48 0 0 -1 150.28 6.25 0 0 -2 6.93 0.50 0 0 2 7.18 0.61 0 0 -2 7.96 0.62 0 0 3 17.80 1.17 0 0 -3 15.53 0.95 0 0 -3 18.07 1.16 0 0 4 20.97 1.42 0 0 -4 21.41 1.46 0 0 -5 0.48 0.24 -1 0 0 -0.01 0.06 -1 0 0 0.02 0.06 1 0 1 48.12 2.08 -1 0 1 51.54 2.09 1 0 -1 48.74 2.10 -1 0 1 48.14 1.96 -1 0 -1 48.93 2.05 -1 0 -1 45.69 2.00 -1 0 2 9.49 0.72 -1 0 -2 10.41 0.70 1 0 2 9.91 0.73 1 0 -2 10.42 0.74 -1 0 2 10.04 0.62 -1 0 -2 9.55 0.63 1 0 -3 -0.07 0.22 1 0 3 0.07 0.30 -1 0 -3 0.00 0.22 -1 0 3 -0.19 0.23 -1 0 -3 0.16 0.15 1 0 4 0.64 0.31 1 0 -4 -0.03 0.25 -1 0 4 -0.13 0.25 -1 0 -4 0.29 0.25 1 0 -5 0.57 0.27 2 0 0 2.89 0.19 -2 0 0 3.40 0.27 2 0 0 3.27 0.28 -2 0 -1 849.05 32.53 -2 0 1 874.33 31.59 -2 0 1 843.20 32.37 2 0 -1 791.79 32.61 -2 0 -1 834.25 31.66 2 0 1 814.27 32.38 -2 0 -2 92.72 4.00 -2 0 -2 100.14 4.11 -2 0 2 96.17 3.92 2 0 2 97.89 4.18 -2 0 2 101.92 4.19 2 0 -2 97.79 4.22 -2 0 -3 0.01 0.20 2 0 3 0.44 0.33 -2 0 -3 0.35 0.20 -2 0 3 0.18 0.28 2 0 -3 0.03 0.27 -2 0 -4 0.27 0.25 2 0 4 0.32 0.26 2 0 -4 0.06 0.28 -2 0 4 0.05 0.21 2 0 -5 -0.48 0.22 2 0 5 0.74 0.41 -3 0 0 0.01 0.20 3 0 0 -0.12 0.10 3 0 0 -0.20 0.20 -3 0 1 12.65 0.75 -3 0 -1 13.72 0.63 -3 0 1 15.02 0.69 3 0 -1 12.20 0.75 3 0 1 11.80 0.75 -3 0 -1 12.70 0.76 -3 0 2 -0.09 0.22 -3 0 -2 0.10 0.18 3 0 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1.63 0.37 6 -25 0 0.60 0.34 -6 -25 0 0.95 0.35 -6 25 1 2.01 0.42 6 -25 1 3.14 0.54 6 25 -1 3.31 0.50 -6 -25 -1 2.29 0.42 6 -25 -1 2.85 0.52 -6 -25 1 2.64 0.44 6 25 1 3.17 0.51 -6 25 2 5.49 0.71 6 25 -2 6.31 0.76 -6 -25 2 6.05 0.70 -6 25 -2 6.47 0.77 6 -25 -2 5.61 0.71 6 25 2 5.48 0.78 -7 25 0 -0.16 0.21 -7 -25 0 0.05 0.21 7 -25 0 0.21 0.24 7 -25 1 2.96 0.52 -7 25 1 1.99 0.42 7 25 -1 2.72 0.42 7 25 1 2.79 0.47 7 -25 -1 1.87 0.44 -7 -25 1 2.11 0.39 7 25 -2 0.25 0.25 -7 25 2 0.97 0.32 7 -25 -2 0.89 0.31 7 25 2 1.48 0.57 -7 -25 2 0.49 0.28 -7 25 -2 0.95 0.31 -8 25 0 0.32 0.22 8 -25 0 0.00 0.24 8 -25 1 15.38 1.29 8 25 -1 13.96 1.14 -8 25 1 13.43 1.22 8 -25 -1 13.06 1.25 8 25 1 14.65 1.21 -8 -25 1 14.56 1.16 -8 25 2 4.32 0.67 8 25 -2 3.36 0.58 8 25 2 5.07 0.89 -8 -25 2 2.74 0.46 -8 25 -2 2.57 0.41 8 -25 -2 3.95 0.59 9 -25 0 0.85 0.32 -9 25 0 1.52 0.44 -9 -25 -1 5.11 0.59 9 -25 1 5.60 0.69 9 25 -1 6.81 0.70 -9 25 1 5.79 0.77 9 -25 -1 7.71 0.85 -9 -25 1 4.89 0.63 -9 -25 -2 9.25 0.91 9 25 -2 9.56 1.03 -9 -25 2 6.90 0.82 -10 25 0 2.03 0.43 10 -25 0 0.96 0.33 -10 25 1 0.24 0.28 10 -25 1 0.25 0.35 -10 -25 -1 0.48 0.21 10 -25 -1 0.92 0.31 -10 -25 1 0.15 0.26 10 25 -2 5.18 0.78 11 -25 0 2.60 0.51 -11 25 0 2.88 0.58 11 -25 -1 6.34 0.86 -11 25 -1 5.64 0.81 -11 -25 1 3.93 0.53 -12 25 -1 1.73 0.67 0 -26 0 4.46 0.72 0 26 0 6.17 0.64 0 -26 -1 0.37 0.30 0 26 1 0.85 0.34 0 -26 1 0.39 0.33 0 26 -2 0.53 0.37 0 -26 -2 0.29 0.29 0 26 2 -0.05 0.19 0 -26 -3 0.96 0.26 0 -26 3 1.44 0.28 1 -26 0 0.28 0.30 -1 26 0 0.15 0.24 -1 -26 0 -0.22 0.26 1 -26 1 0.49 0.30 -1 -26 -1 1.52 0.46 -1 26 1 1.45 0.40 1 26 1 1.11 0.36 1 -26 -1 0.91 0.44 -1 -26 1 1.63 0.54 -1 26 2 0.56 0.26 -1 -26 -2 0.68 0.29 1 26 -2 0.14 0.36 1 26 2 0.62 0.28 1 -26 -2 0.92 0.36 -1 26 -2 0.75 0.37 1 -26 3 0.22 0.21 -1 -26 -3 0.37 0.20 -1 -26 3 1.19 0.28 -2 -26 0 1.54 0.51 -2 26 0 2.60 0.43 2 -26 0 2.34 0.54 -2 26 1 2.48 0.42 -2 -26 -1 1.47 0.45 2 -26 1 1.62 0.48 2 -26 -1 1.90 0.59 -2 -26 1 2.00 0.60 2 26 1 2.32 0.43 -2 -26 -2 -0.13 0.21 -2 26 2 0.12 0.22 2 26 -2 0.30 0.21 2 -26 -2 0.66 0.33 2 26 2 0.58 0.27 -2 26 -2 0.35 0.32 -2 -26 2 0.46 0.20 2 -26 3 0.31 0.21 -3 26 0 0.20 0.24 3 -26 0 0.70 0.34 -3 -26 0 0.10 0.23 3 26 -1 0.44 0.30 3 -26 1 0.98 0.34 -3 26 1 0.10 0.20 -3 -26 -1 0.58 0.29 3 26 1 -0.02 0.20 3 -26 -1 0.19 0.31 -3 -26 -2 4.02 0.55 -3 26 2 5.39 0.66 3 26 -2 4.28 0.58 -3 26 -2 4.49 0.67 -3 -26 2 3.97 0.51 3 26 2 4.00 0.60 3 -26 -2 4.11 0.70 4 -26 0 2.32 0.48 -4 26 0 2.26 0.41 -4 -26 0 2.17 0.49 4 26 -1 1.18 0.40 -4 26 1 0.89 0.41 -4 -26 -1 2.38 0.42 4 -26 1 1.69 0.52 4 -26 -1 2.15 0.63 4 26 1 1.74 0.37 4 26 -2 3.48 0.50 -4 26 2 2.59 0.48 -4 26 -2 2.87 0.56 -4 -26 2 2.46 0.43 4 -26 -2 2.52 0.57 4 26 2 3.32 0.57 5 -26 0 -0.14 0.20 -5 26 0 0.39 0.23 -5 -26 0 0.39 0.29 5 -26 1 5.20 0.71 5 26 -1 5.29 0.64 -5 -26 -1 5.73 0.68 -5 26 1 5.52 0.69 5 -26 -1 4.49 0.64 5 26 1 5.03 0.61 5 26 -2 6.83 0.78 -5 26 2 7.06 0.82 -5 -26 2 6.69 0.76 5 26 2 8.59 0.95 5 -26 -2 7.66 0.95 -5 26 -2 6.58 0.82 -6 -26 0 0.91 0.31 -6 26 0 0.92 0.31 6 -26 0 0.88 0.31 -6 26 1 1.42 0.41 6 26 -1 0.68 0.25 6 -26 1 0.55 0.29 6 26 1 0.66 0.27 6 -26 -1 0.76 0.29 6 26 -2 2.39 0.47 -6 26 2 2.77 0.48 -6 26 -2 1.98 0.42 -6 -26 2 1.57 0.35 6 -26 -2 2.09 0.56 6 26 2 2.36 0.65 -7 26 0 1.83 0.37 7 -26 0 2.07 0.42 -7 26 1 0.90 0.32 7 -26 1 0.44 0.29 7 26 -1 1.33 0.28 -7 -26 1 0.27 0.22 7 -26 -1 0.25 0.23 7 26 1 0.59 0.28 7 26 -2 3.29 0.59 -7 26 -2 3.59 0.51 7 26 2 4.48 0.83 -7 -26 2 2.34 0.43 -8 26 0 5.54 0.67 8 -26 0 4.22 0.66 8 26 -1 7.31 0.79 -8 26 1 10.53 1.04 8 -26 1 8.98 0.95 8 -26 -1 6.26 0.83 -8 -26 1 7.90 0.80 8 26 1 8.10 0.89 8 26 -2 2.47 0.55 8 26 2 4.07 0.93 -8 26 -2 3.53 0.45 -9 26 0 0.77 0.33 9 -26 0 1.74 0.41 -9 26 1 9.33 1.01 9 -26 1 9.42 0.98 9 26 -1 8.50 0.86 -9 -26 1 7.25 0.76 9 -26 -1 9.13 1.04 -10 26 0 0.82 0.34 10 -26 0 0.11 0.26 10 -26 1 0.52 0.38 -10 -26 1 0.32 0.25 10 -26 -1 -0.49 0.35 11 -26 0 1.03 0.42 -11 26 0 0.33 0.40 -11 -26 1 4.39 0.53 0 -27 0 -0.07 0.25 0 -27 -1 9.55 1.00 0 27 1 8.50 0.88 0 -27 1 10.61 1.16 0 -27 -2 1.12 0.32 0 27 -2 0.38 0.39 0 27 2 0.49 0.26 1 -27 0 0.30 0.31 -1 -27 0 0.47 0.31 -1 -27 -1 2.31 0.50 1 -27 1 2.17 0.45 -1 27 1 2.35 0.42 -1 -27 1 2.22 0.63 1 -27 -1 2.33 0.52 1 27 1 2.78 0.43 1 27 -2 4.90 0.77 -1 -27 -2 5.46 0.69 -1 27 2 4.92 0.69 -1 27 -2 4.62 0.75 1 27 2 5.12 0.73 1 -27 -2 4.63 0.67 -2 27 0 0.74 0.24 2 -27 0 -0.06 0.31 -2 -27 0 -0.11 0.28 -2 27 1 0.91 0.30 -2 -27 -1 0.82 0.33 2 -27 1 0.99 0.37 2 27 1 1.35 0.31 -2 -27 1 1.07 0.39 2 -27 -1 0.34 0.35 -2 -27 -2 5.71 0.70 -2 27 2 7.14 0.81 2 27 -2 5.93 0.74 -2 27 -2 6.21 0.86 2 -27 -2 5.57 0.77 2 27 2 6.52 0.82 -3 27 0 7.34 0.76 -3 -27 0 8.08 0.90 3 -27 0 7.64 0.88 -3 27 1 2.55 0.45 -3 -27 -1 1.72 0.48 3 -27 1 2.25 0.45 3 27 -1 1.85 0.44 3 -27 -1 2.60 0.58 3 27 1 1.36 0.31 -3 27 2 4.69 0.61 3 27 -2 3.45 0.57 -3 -27 -2 3.09 0.46 3 -27 -2 3.83 0.61 3 27 2 3.27 0.61 -3 27 -2 2.38 0.54 4 -27 0 0.19 0.20 -4 -27 0 0.02 0.27 -4 27 0 0.29 0.21 -4 -27 -1 2.18 0.46 4 27 -1 2.05 0.42 4 -27 1 2.04 0.48 -4 27 1 2.51 0.48 4 27 1 1.92 0.37 4 -27 -1 2.63 0.58 -4 27 2 3.67 0.61 4 27 -2 3.94 0.58 4 27 2 4.52 0.69 4 -27 -2 4.83 0.75 -4 27 -2 3.63 0.61 -4 -27 2 4.72 0.55 5 -27 0 0.40 0.25 -5 27 0 0.92 0.30 -5 -27 0 1.00 0.35 5 -27 1 1.60 0.44 -5 27 1 1.32 0.36 -5 -27 -1 0.82 0.32 5 27 1 1.29 0.40 5 -27 -1 1.54 0.35 -5 27 2 2.17 0.50 5 27 -2 2.65 0.51 5 27 2 2.22 0.63 -5 -27 2 2.05 0.35 -5 27 -2 0.86 0.35 5 -27 -2 1.92 0.60 -6 -27 0 0.85 0.31 -6 27 0 1.45 0.34 6 -27 0 0.40 0.25 6 27 -1 1.14 0.32 6 -27 1 0.96 0.35 -6 27 1 0.74 0.34 6 -27 -1 1.59 0.34 6 27 1 0.99 0.37 6 27 -2 2.23 0.50 -6 27 -2 1.03 0.30 -6 -27 2 2.24 0.35 6 27 2 1.88 0.73 -7 27 0 13.65 1.17 7 27 0 12.28 1.06 7 -27 0 12.02 1.20 7 27 -1 4.12 0.54 -7 27 1 3.24 0.59 7 -27 1 4.14 0.63 7 -27 -1 2.92 0.49 7 27 1 3.42 0.60 -7 -27 2 7.01 0.74 -7 27 -2 6.46 0.72 8 -27 0 1.92 0.41 -8 27 1 0.76 0.39 8 27 -1 0.38 0.26 8 -27 -1 0.78 0.32 -8 27 -2 4.42 0.52 -9 27 0 0.44 0.33 9 -27 0 0.22 0.27 9 27 -1 1.60 0.46 9 -27 1 2.20 0.59 9 -27 -1 2.20 0.50 -10 27 0 0.57 0.43 10 -27 0 1.15 0.42 10 -27 1 2.23 0.76 -10 -27 1 1.47 0.30 11 -27 0 3.83 0.76 0 -28 0 0.63 0.41 0 -28 1 0.23 0.46 0 -28 -1 0.11 0.30 0 28 1 -0.17 0.20 0 28 2 4.60 0.69 0 -28 -2 3.80 0.56 0 28 -2 5.31 0.80 1 -28 0 0.73 0.39 -1 -28 0 0.47 0.34 1 -28 1 1.03 0.31 -1 -28 -1 1.31 0.42 -1 28 1 1.58 0.34 1 -28 -1 0.95 0.41 -1 -28 1 1.39 0.55 1 28 1 1.13 0.34 -1 -28 -2 0.65 0.32 1 28 -2 1.52 0.50 -1 28 2 0.70 0.38 1 -28 -2 1.39 0.46 1 28 2 1.03 0.43 -1 28 -2 0.04 0.33 2 -28 0 0.60 0.44 -2 -28 0 1.41 0.46 -2 -28 -1 1.10 0.37 2 -28 1 0.56 0.26 -2 28 1 0.55 0.27 -2 -28 1 1.04 0.46 2 -28 -1 1.69 0.49 2 28 1 0.96 0.28 2 28 -2 9.23 1.00 -2 28 2 9.44 0.99 -2 -28 -2 8.93 0.90 -2 28 -2 7.84 0.98 2 -28 -2 7.05 0.91 2 28 2 9.15 1.02 -3 28 0 0.26 0.24 3 -28 0 0.81 0.27 -3 -28 0 0.36 0.28 -3 -28 -1 3.48 0.58 3 28 -1 3.80 0.60 -3 28 1 4.81 0.64 3 -28 1 4.70 0.64 3 -28 -1 4.62 0.76 3 28 1 3.63 0.53 -3 28 2 3.39 0.60 -3 -28 -2 4.25 0.54 3 28 2 4.15 0.74 3 -28 -2 4.68 0.71 -3 28 -2 4.55 0.69 -4 28 0 5.13 0.62 -4 -28 0 5.09 0.70 4 -28 0 6.26 0.76 -4 -28 -1 5.98 0.75 4 -28 1 6.86 0.84 4 28 -1 7.40 0.84 -4 28 1 5.03 0.69 4 -28 -1 6.08 0.88 4 28 1 5.43 0.65 4 28 2 2.96 0.70 -4 28 -2 3.38 0.57 -5 28 0 0.85 0.28 5 -28 0 0.69 0.26 -5 -28 0 1.21 0.39 -5 -28 -1 -0.18 0.20 5 -28 1 0.42 0.31 5 28 -1 0.22 0.26 -5 28 1 0.28 0.30 5 -28 -1 0.57 0.27 5 28 1 0.08 0.23 6 -28 0 0.11 0.23 -6 -28 0 0.38 0.27 -6 28 0 0.32 0.24 -6 28 1 0.64 0.34 6 -28 1 -0.37 0.32 6 28 -1 0.47 0.28 6 -28 -1 0.90 0.36 6 28 1 0.30 0.32 -6 -28 2 0.79 0.23 7 -28 0 0.78 0.30 7 28 0 0.63 0.30 -7 28 0 0.79 0.32 7 28 -1 1.08 0.39 7 -28 1 0.59 0.41 -7 28 1 1.19 0.47 7 -28 -1 0.74 0.34 8 -28 0 1.55 0.54 -8 28 0 2.65 0.50 8 28 -1 1.34 0.45 8 -28 1 1.13 0.51 -9 28 0 17.98 1.55 9 -28 0 16.43 1.55 9 -28 1 -0.36 0.43 0 -29 0 -0.35 0.26 0 -29 1 0.96 0.50 0 29 1 1.02 0.33 0 -29 -1 0.24 0.30 0 -29 -2 1.67 0.43 -1 -29 0 -0.31 0.27 1 -29 0 -0.17 0.29 -1 29 1 2.58 0.45 -1 -29 -1 2.92 0.53 1 -29 1 2.47 0.45 1 -29 -1 2.52 0.57 -1 -29 1 3.02 0.62 1 29 1 3.21 0.47 -1 -29 -2 0.02 0.23 -2 -29 0 2.09 0.47 2 -29 0 3.97 0.76 2 -29 1 3.64 0.56 -2 29 1 2.75 0.50 2 29 -1 3.19 0.52 -2 -29 -1 3.47 0.54 2 -29 -1 3.37 0.63 2 29 1 2.62 0.42 -2 -29 -2 1.77 0.36 -3 -29 0 0.07 0.31 3 -29 0 0.64 0.28 -3 29 1 5.69 0.74 -3 -29 -1 6.20 0.72 3 -29 1 5.87 0.77 3 29 -1 5.27 0.71 3 29 1 5.50 0.67 3 -29 -1 5.15 0.82 -3 -29 -2 0.21 0.19 -4 -29 0 1.28 0.36 4 -29 0 0.45 0.22 4 -29 1 6.02 0.78 -4 -29 -1 4.71 0.63 -4 29 1 5.40 0.72 4 29 -1 4.72 0.72 4 29 1 3.51 0.59 4 -29 -1 5.87 0.87 -5 29 0 0.20 0.29 5 -29 0 0.03 0.21 -5 -29 0 0.63 0.29 -5 29 1 0.69 0.44 5 29 -1 2.27 0.50 5 -29 1 1.42 0.53 -5 -29 -1 2.29 0.35 5 -29 -1 2.73 0.49 5 29 1 1.65 0.50 6 -29 0 -0.26 0.25 -6 29 0 0.00 0.30 -6 -29 0 0.03 0.22 -6 29 1 1.20 0.52 6 -29 1 1.70 0.62 6 29 -1 1.25 0.44 -7 29 0 1.55 0.51 7 -29 0 1.84 0.56 7 29 -1 3.80 0.70 -8 29 0 0.60 0.46 8 29 -1 0.25 0.36 0 -30 0 18.51 1.60 0 30 1 -0.03 0.25 0 -30 1 -0.24 0.36 0 -30 -1 0.03 0.26 1 -30 0 0.01 0.32 -1 -30 0 1.27 0.42 1 -30 1 1.30 0.39 -1 -30 -1 1.61 0.37 -1 30 1 2.00 0.41 1 -30 -1 1.27 0.44 -1 -30 1 1.32 0.50 1 30 1 1.52 0.48 -2 -30 0 0.94 0.37 2 -30 0 1.02 0.51 -2 30 1 1.82 0.50 2 -30 1 1.15 0.36 -2 -30 -1 1.40 0.39 2 30 -1 1.38 0.43 2 -30 -1 1.78 0.53 2 30 1 1.37 0.42 3 -30 0 0.70 0.32 -3 -30 0 1.30 0.38 3 30 -1 7.74 0.95 -3 -30 -1 8.18 0.87 -3 30 1 8.04 0.98 3 30 1 8.73 0.94 4 -30 0 1.10 0.34 -4 -30 0 0.95 0.29 4 30 -1 1.69 0.58 -4 -30 -1 1.58 0.33 -4 30 1 1.59 0.52 -5 -30 0 7.24 0.83 -5 30 1 0.96 0.47 -5 -30 -1 0.43 0.21 -6 -30 0 4.94 0.60 -7 30 0 0.47 0.54 0 -31 0 0.38 0.31 0 31 1 -0.59 0.33 -1 -31 0 3.16 0.60 -1 31 1 1.25 0.55 1 31 1 1.56 0.53 -2 -31 0 0.74 0.38 -2 31 1 2.98 0.67 2 31 1 4.18 0.79 -3 -31 0 3.05 0.52 -3 31 1 0.06 0.44 -3 -31 -1 0.12 0.22 -4 -31 0 0.61 0.24 -4 -31 -1 0.28 0.20 -5 -31 0 2.04 0.36 0 0 0 0.00 0.00 ; _shelx_res_checksum 76126 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 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_refinement_flags _atom_site_occupancy _atom_site_symmetry_multiplicity O O1 0.43017(8) 0.12053(5) 0.0589(4) 0.0260(3) Uani d . 1 1 N N1 0.57518(9) 0.11317(5) 0.2415(4) 0.0213(3) Uani d . 1 1 N N2 0.38885(10) 0.24495(6) -0.3038(4) 0.0283(3) Uani d . 1 1 C C1 0.65658(10) 0.13660(6) 0.2753(4) 0.0189(3) Uani d . 1 1 C C2 0.67269(11) 0.19050(6) 0.1762(4) 0.0194(3) Uani d . 1 1 H H2 0.7302 0.2058 0.2047 0.023 Uiso calc R 1 1 C C3 0.60488(11) 0.22245(7) 0.0350(4) 0.0189(3) Uani d . 1 1 C C4 0.52180(11) 0.19767(7) -0.0084(5) 0.0198(4) Uani d . 1 1 C C5 0.51198(11) 0.14286(7) 0.1036(5) 0.0208(4) Uani d . 1 1 C C6 0.41763(12) 0.06623(7) 0.1956(6) 0.0310(4) Uani d . 1 1 H H6A 0.4557 0.0403 0.0720 0.046 Uiso calc R 1 1 H H6B 0.3554 0.0554 0.1683 0.046 Uiso calc R 1 1 H H6C 0.4332 0.0660 0.4396 0.046 Uiso calc R 1 1 C C7 0.44794(11) 0.22442(7) -0.1697(5) 0.0215(3) Uani d . 1 1 C C8 0.72680(11) 0.10115(7) 0.4250(4) 0.0194(3) Uani d . 1 1 C C9 0.70457(11) 0.05036(7) 0.5689(5) 0.0226(4) Uani d . 1 1 H H9 0.6442 0.0392 0.5762 0.027 Uiso calc R 1 1 C C10 0.76945(11) 0.01607(7) 0.7011(5) 0.0250(4) Uani d . 1 1 H H10 0.7534 -0.0184 0.7976 0.030 Uiso calc R 1 1 C C11 0.85806(12) 0.03196(7) 0.6928(5) 0.0256(4) Uani d . 1 1 H H11 0.9028 0.0085 0.7821 0.031 Uiso calc R 1 1 C C12 0.88043(12) 0.08248(7) 0.5528(5) 0.0263(4) Uani d . 1 1 H H12 0.9409 0.0936 0.5473 0.032 Uiso calc R 1 1 C C13 0.81601(11) 0.11685(7) 0.4214(5) 0.0234(4) Uani d . 1 1 H H13 0.8324 0.1514 0.3277 0.028 Uiso calc R 1 1 C C14 0.62283(11) 0.28047(7) -0.0627(4) 0.0190(3) Uani d . 1 1 C C15 0.56225(11) 0.32239(7) 0.0117(4) 0.0218(4) Uani d . 1 1 H H15 0.5077 0.3140 0.1223 0.026 Uiso calc R 1 1 C C16 0.58217(11) 0.37627(7) -0.0770(5) 0.0237(4) Uani d . 1 1 H H16 0.5413 0.4048 -0.0245 0.028 Uiso calc R 1 1 C C17 0.66093(12) 0.38876(7) -0.2411(5) 0.0257(4) Uani d . 1 1 H H17 0.6737 0.4257 -0.3029 0.031 Uiso calc R 1 1 C C18 0.72141(11) 0.34755(7) -0.3158(5) 0.0241(4) Uani d . 1 1 H H18 0.7753 0.3561 -0.4305 0.029 Uiso calc R 1 1 C C19 0.70285(11) 0.29378(7) -0.2222(4) 0.0213(3) Uani d . 1 1 H H19 0.7451 0.2657 -0.2672 0.026 Uiso calc R 1 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 O1 0.0191(6) 0.0201(6) 0.0388(7) -0.0036(5) -0.0033(6) 0.0000(5) N1 0.0203(7) 0.0194(6) 0.0241(8) -0.0007(5) 0.0008(6) -0.0018(6) N2 0.0236(7) 0.0269(7) 0.0345(8) 0.0006(6) -0.0047(7) -0.0002(7) C1 0.0193(7) 0.0201(7) 0.0172(8) 0.0011(6) 0.0013(6) -0.0032(6) C2 0.0183(7) 0.0201(8) 0.0197(8) -0.0004(6) -0.0003(7) -0.0032(6) C3 0.0208(8) 0.0199(7) 0.0160(8) 0.0012(6) 0.0020(7) -0.0024(6) C4 0.0184(8) 0.0199(8) 0.0210(9) 0.0019(6) -0.0003(7) -0.0024(7) C5 0.0172(8) 0.0213(8) 0.0237(9) -0.0016(6) 0.0018(7) -0.0037(7) C6 0.0254(9) 0.0224(9) 0.0451(12) -0.0059(7) -0.0031(9) 0.0021(8) C7 0.0206(8) 0.0198(8) 0.0241(9) -0.0017(6) 0.0017(7) -0.0013(7) C8 0.0207(8) 0.0194(8) 0.0182(8) 0.0007(6) -0.0002(7) -0.0030(6) C9 0.0225(8) 0.0214(8) 0.0241(9) -0.0007(7) 0.0020(8) -0.0010(7) C10 0.0296(9) 0.0201(8) 0.0254(9) 0.0019(7) 0.0021(8) 0.0017(7) C11 0.0268(9) 0.0252(8) 0.0249(9) 0.0056(7) -0.0005(8) 0.0019(7) C12 0.0226(8) 0.0286(9) 0.0277(9) 0.0005(7) -0.0037(8) -0.0010(7) C13 0.0249(8) 0.0194(8) 0.0259(9) -0.0015(7) -0.0012(7) 0.0003(7) C14 0.0207(8) 0.0191(7) 0.0172(7) 0.0004(6) -0.0031(7) -0.0009(6) C15 0.0209(8) 0.0224(8) 0.0222(9) -0.0006(7) -0.0005(7) -0.0016(7) C16 0.0264(9) 0.0201(8) 0.0245(9) 0.0024(7) -0.0033(7) -0.0013(7) C17 0.0331(9) 0.0202(8) 0.0238(9) -0.0042(7) -0.0055(8) 0.0020(7) C18 0.0233(8) 0.0268(9) 0.0222(8) -0.0045(7) -0.0009(7) 0.0008(7) C19 0.0211(8) 0.0225(8) 0.0203(8) 0.0009(6) -0.0013(7) -0.0032(7) 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 C5 O1 C6 116.07(13) C5 N1 C1 117.68(14) N1 C1 C2 121.80(15) N1 C1 C8 115.97(14) C2 C1 C8 122.23(14) C1 C2 C3 120.49(15) C1 C2 H2 119.8 C3 C2 H2 119.8 C2 C3 C4 117.52(15) C2 C3 C14 119.74(15) C4 C3 C14 122.74(15) C3 C4 C5 117.62(15) C3 C4 C7 123.46(15) C5 C4 C7 118.89(15) N1 C5 O1 119.45(15) N1 C5 C4 124.86(15) O1 C5 C4 115.69(14) O1 C6 H6A 109.5 O1 C6 H6B 109.5 H6A C6 H6B 109.5 O1 C6 H6C 109.5 H6A C6 H6C 109.5 H6B C6 H6C 109.5 N2 C7 C4 178.56(19) C13 C8 C9 118.44(15) C13 C8 C1 121.52(15) C9 C8 C1 120.03(14) C10 C9 C8 120.84(16) C10 C9 H9 119.6 C8 C9 H9 119.6 C9 C10 C11 120.12(16) C9 C10 H10 119.9 C11 C10 H10 119.9 C12 C11 C10 119.29(16) C12 C11 H11 120.4 C10 C11 H11 120.4 C13 C12 C11 120.81(17) C13 C12 H12 119.6 C11 C12 H12 119.6 C12 C13 C8 120.49(16) C12 C13 H13 119.8 C8 C13 H13 119.8 C19 C14 C15 119.15(15) C19 C14 C3 119.47(14) C15 C14 C3 121.35(15) C16 C15 C14 119.70(16) C16 C15 H15 120.1 C14 C15 H15 120.1 C17 C16 C15 120.56(16) C17 C16 H16 119.7 C15 C16 H16 119.7 C16 C17 C18 120.19(15) C16 C17 H17 119.9 C18 C17 H17 119.9 C17 C18 C19 119.64(16) C17 C18 H18 120.2 C19 C18 H18 120.2 C18 C19 C14 120.72(15) C18 C19 H19 119.6 C14 C19 H19 119.6 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C5 1.3583(19) O1 C6 1.437(2) N1 C5 1.311(2) N1 C1 1.359(2) N2 C7 1.147(2) C1 C2 1.388(2) C1 C8 1.485(2) C2 C3 1.397(2) C2 H2 0.9500 C3 C4 1.400(2) C3 C14 1.487(2) C4 C5 1.411(2) C4 C7 1.435(2) C6 H6A 0.9800 C6 H6B 0.9800 C6 H6C 0.9800 C8 C13 1.397(2) C8 C9 1.398(2) C9 C10 1.385(2) C9 H9 0.9500 C10 C11 1.390(2) C10 H10 0.9500 C11 C12 1.386(2) C11 H11 0.9500 C12 C13 1.380(2) C12 H12 0.9500 C13 H13 0.9500 C14 C19 1.395(2) C14 C15 1.399(2) C15 C16 1.388(2) C15 H15 0.9500 C16 C17 1.382(2) C16 H16 0.9500 C17 C18 1.386(2) C17 H17 0.9500 C18 C19 1.386(2) C18 H18 0.9500 C19 H19 0.9500 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 C5 N1 C1 C2 1.6(2) C5 N1 C1 C8 -178.59(15) N1 C1 C2 C3 -0.4(2) C8 C1 C2 C3 179.74(15) C1 C2 C3 C4 -1.4(2) C1 C2 C3 C14 178.68(15) C2 C3 C4 C5 1.9(2) C14 C3 C4 C5 -178.09(15) C2 C3 C4 C7 -175.93(16) C14 C3 C4 C7 4.0(3) C1 N1 C5 O1 178.65(15) C1 N1 C5 C4 -0.9(3) C6 O1 C5 N1 4.9(2) C6 O1 C5 C4 -175.45(16) C3 C4 C5 N1 -0.9(3) C7 C4 C5 N1 177.11(17) C3 C4 C5 O1 179.55(15) C7 C4 C5 O1 -2.5(2) N1 C1 C8 C13 169.24(16) C2 C1 C8 C13 -10.9(2) N1 C1 C8 C9 -9.7(2) C2 C1 C8 C9 170.16(16) C13 C8 C9 C10 -0.8(3) C1 C8 C9 C10 178.17(16) C8 C9 C10 C11 0.2(3) C9 C10 C11 C12 0.3(3) C10 C11 C12 C13 -0.2(3) C11 C12 C13 C8 -0.4(3) C9 C8 C13 C12 0.9(3) C1 C8 C13 C12 -178.03(16) C2 C3 C14 C19 40.9(2) C4 C3 C14 C19 -139.07(17) C2 C3 C14 C15 -137.09(17) C4 C3 C14 C15 42.9(2) C19 C14 C15 C16 0.6(2) C3 C14 C15 C16 178.63(15) C14 C15 C16 C17 0.6(3) C15 C16 C17 C18 -0.7(3) C16 C17 C18 C19 -0.6(3) C17 C18 C19 C14 1.9(3) C15 C14 C19 C18 -1.9(2) C3 C14 C19 C18 -179.94(16) _cod_database_fobs_code 2239028