data_sku_83_2 _audit_creation_date 2014-08-18 _audit_creation_method ; Olex2 1.2-ac2 (compiled 2012.03.27 svn.r2268, GUI svn.r4156) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C21 H19 N O2' _chemical_formula_sum 'C21 H19 N O2' _chemical_formula_weight 317.37 _chemical_melting_point ? _chemical_oxdiff_formula 'C22 N1 O2 H30' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x, -y-1/2, z-1/2' _cell_length_a 16.6232(2) _cell_length_b 8.48700(10) _cell_length_c 24.2138(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.5810(10) _cell_angle_gamma 90.00 _cell_volume 3218.55(6) _cell_formula_units_Z 8 _cell_measurement_reflns_used 42815 _cell_measurement_temperature 100 _cell_measurement_theta_max 76.3150 _cell_measurement_theta_min 2.8050 _exptl_absorpt_coefficient_mu 0.666 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.79515 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour '' _exptl_crystal_density_diffrn 1.310 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description '' _exptl_crystal_F_000 1344 _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.11 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_unetI/netI 0.0103 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 70891 _diffrn_reflns_theta_full 76.68 _diffrn_reflns_theta_max 76.68 _diffrn_reflns_theta_min 2.82 _diffrn_ambient_temperature 100.0 _diffrn_detector_area_resol_mean 10.3829 _diffrn_measured_fraction_theta_full 0.9939 _diffrn_measured_fraction_theta_max 0.9939 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 0.00 25.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 40.0000 93.0000 -47.1816 25 #__ type_ start__ end____ width___ exp.time_ 2 omega 3.00 29.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 40.0000 87.0000 136.8209 26 #__ type_ start__ end____ width___ exp.time_ 3 omega 3.00 28.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 40.0000 87.0000 52.0800 25 #__ type_ start__ end____ width___ exp.time_ 4 omega -71.00 33.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - -41.1287 57.0000 0.0000 104 #__ type_ start__ end____ width___ exp.time_ 5 omega -91.00 -54.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - -41.1287 -38.0000 120.0000 37 #__ type_ start__ end____ width___ exp.time_ 6 omega -114.00 -83.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - -41.1287 -57.0000 -60.0000 31 #__ type_ start__ end____ width___ exp.time_ 7 omega -41.00 -15.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - -41.1287 -38.0000 120.0000 26 #__ type_ start__ end____ width___ exp.time_ 8 omega -115.00 -53.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - -41.1287 -57.0000 -120.0000 62 #__ type_ start__ end____ width___ exp.time_ 9 omega -72.00 -12.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - -41.1287 -57.0000 -60.0000 60 #__ type_ start__ end____ width___ exp.time_ 10 omega -41.00 -14.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - -41.1287 -57.0000 -120.0000 27 #__ type_ start__ end____ width___ exp.time_ 11 omega -117.00 -15.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - -41.1287 -38.0000 30.0000 102 #__ type_ start__ end____ width___ exp.time_ 12 omega 24.00 90.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 41.1287 -126.0000 -90.0000 66 #__ type_ start__ end____ width___ exp.time_ 13 omega 24.00 99.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 41.1287 -126.0000 120.0000 75 #__ type_ start__ end____ width___ exp.time_ 14 omega 12.00 37.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 48.0000 84.0000 158.2363 25 #__ type_ start__ end____ width___ exp.time_ 15 omega 18.00 43.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 52.0000 80.0000 -85.2495 25 #__ type_ start__ end____ width___ exp.time_ 16 omega 17.00 42.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 52.0000 81.0000 56.2923 25 #__ type_ start__ end____ width___ exp.time_ 17 omega 18.00 43.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 52.0000 80.0000 -33.2662 25 #__ type_ start__ end____ width___ exp.time_ 18 omega 22.00 47.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 56.0000 78.0000 -140.7313 25 #__ type_ start__ end____ width___ exp.time_ 19 omega 79.00 137.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 60.0000 76.0000 -157.6379 58 #__ type_ start__ end____ width___ exp.time_ 20 omega 30.00 56.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 60.0000 76.0000 -157.6379 26 #__ type_ start__ end____ width___ exp.time_ 21 omega 27.00 53.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 60.0000 77.0000 96.9651 26 #__ type_ start__ end____ width___ exp.time_ 22 omega 30.00 56.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 64.0000 77.0000 167.1662 26 #__ type_ start__ end____ width___ exp.time_ 23 omega 31.00 57.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 64.0000 76.0000 -11.1222 26 #__ type_ start__ end____ width___ exp.time_ 24 omega 35.00 60.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 68.0000 75.0000 15.4875 25 #__ type_ start__ end____ width___ exp.time_ 25 omega 80.00 121.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 68.0000 75.0000 15.4875 41 #__ type_ start__ end____ width___ exp.time_ 26 omega 35.00 83.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 68.0000 76.0000 152.4826 48 #__ type_ start__ end____ width___ exp.time_ 27 omega 38.00 66.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 72.0000 77.0000 68.2425 28 #__ type_ start__ end____ width___ exp.time_ 28 omega 38.00 63.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 72.0000 77.0000 -129.0058 25 #__ type_ start__ end____ width___ exp.time_ 29 omega 106.00 150.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 72.0000 77.0000 -63.9578 44 #__ type_ start__ end____ width___ exp.time_ 30 omega 40.00 66.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 72.0000 75.0000 -94.4351 26 #__ type_ start__ end____ width___ exp.time_ 31 omega 92.00 142.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 72.0000 75.0000 -94.4351 50 #__ type_ start__ end____ width___ exp.time_ 32 omega 112.00 144.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 72.0000 75.0000 30.1528 32 #__ type_ start__ end____ width___ exp.time_ 33 omega 39.00 66.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 72.0000 75.0000 30.1528 27 #__ type_ start__ end____ width___ exp.time_ 34 omega 38.00 99.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 72.0000 77.0000 115.4052 61 #__ type_ start__ end____ width___ exp.time_ 35 omega 38.00 82.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 72.0000 77.0000 -63.9578 44 #__ type_ start__ end____ width___ exp.time_ 36 omega 79.00 128.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 -150.0000 49 #__ type_ start__ end____ width___ exp.time_ 37 omega 79.00 114.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 -30.0000 35 #__ type_ start__ end____ width___ exp.time_ 38 omega 129.00 158.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 150.0000 29 #__ type_ start__ end____ width___ exp.time_ 39 omega 79.00 125.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 150.0000 46 #__ type_ start__ end____ width___ exp.time_ 40 omega 79.00 105.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 0.0000 26 #__ type_ start__ end____ width___ exp.time_ 41 omega 76.00 108.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -112.0000 120.0000 32 #__ type_ start__ end____ width___ exp.time_ 42 omega 36.00 73.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -112.0000 120.0000 37 #__ type_ start__ end____ width___ exp.time_ 43 omega 116.00 176.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 90.0000 60 #__ type_ start__ end____ width___ exp.time_ 44 omega 79.00 111.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 90.0000 32 #__ type_ start__ end____ width___ exp.time_ 45 omega 83.00 170.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 61.0000 -30.0000 87 #__ type_ start__ end____ width___ exp.time_ 46 omega 32.00 100.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -95.0000 90.0000 68 #__ type_ start__ end____ width___ exp.time_ 47 omega 44.00 105.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -95.0000 0.0000 61 #__ type_ start__ end____ width___ exp.time_ 48 omega 82.00 109.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -95.0000 -30.0000 27 #__ type_ start__ end____ width___ exp.time_ 49 omega 79.00 160.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 -120.0000 81 #__ type_ start__ end____ width___ exp.time_ 50 omega 77.00 115.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -112.0000 -180.0000 38 #__ type_ start__ end____ width___ exp.time_ 51 omega 114.00 178.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 30.0000 64 #__ type_ start__ end____ width___ exp.time_ 52 omega 79.00 108.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 30.0000 29 #__ type_ start__ end____ width___ exp.time_ 53 omega 36.00 63.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -112.0000 60.0000 27 #__ type_ start__ end____ width___ exp.time_ 54 omega 82.00 115.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -112.0000 60.0000 33 #__ type_ start__ end____ width___ exp.time_ 55 omega 35.00 61.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -112.0000 -180.0000 26 #__ type_ start__ end____ width___ exp.time_ 56 omega 81.00 115.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -112.0000 -120.0000 34 #__ type_ start__ end____ width___ exp.time_ 57 omega 119.00 173.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 0.0000 54 #__ type_ start__ end____ width___ exp.time_ 58 omega 83.00 131.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 61.0000 -180.0000 48 #__ type_ start__ end____ width___ exp.time_ 59 omega 50.00 101.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -77.0000 30.0000 51 #__ type_ start__ end____ width___ exp.time_ 60 omega 124.00 170.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 -30.0000 46 #__ type_ start__ end____ width___ exp.time_ 61 omega 79.00 129.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 -90.0000 50 #__ type_ start__ end____ width___ exp.time_ 62 omega 134.00 160.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 -90.0000 26 #__ type_ start__ end____ width___ exp.time_ 63 omega 42.00 68.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -112.0000 -120.0000 26 #__ type_ start__ end____ width___ exp.time_ 64 omega 26.00 177.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -4.0000 -57.2708 151 #__ type_ start__ end____ width___ exp.time_ 65 omega 145.00 177.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 120.0000 32 #__ type_ start__ end____ width___ exp.time_ 66 omega 79.00 131.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 120.0000 52 #__ type_ start__ end____ width___ exp.time_ 67 omega 44.00 93.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -39.0000 72.0826 49 #__ type_ start__ end____ width___ exp.time_ 68 omega 30.00 101.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -95.0000 120.0000 71 #__ type_ start__ end____ width___ exp.time_ 69 omega 79.00 105.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -112.0000 -150.0000 26 #__ type_ start__ end____ width___ exp.time_ 70 omega 132.00 177.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 61.0000 -60.0000 45 #__ type_ start__ end____ width___ exp.time_ 71 omega 83.00 127.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 61.0000 -60.0000 44 #__ type_ start__ end____ width___ exp.time_ 72 omega 147.00 178.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 -180.0000 31 #__ type_ start__ end____ width___ exp.time_ 73 omega 86.00 161.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 61.0000 120.0000 75 #__ type_ start__ end____ width___ exp.time_ 74 omega 73.00 115.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -112.0000 -90.0000 42 #__ type_ start__ end____ width___ exp.time_ 75 omega 79.00 138.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 -180.0000 59 #__ type_ start__ end____ width___ exp.time_ 76 omega 35.00 61.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -112.0000 -90.0000 26 #__ type_ start__ end____ width___ exp.time_ 77 omega 84.00 142.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 61.0000 30.0000 58 #__ type_ start__ end____ width___ exp.time_ 78 omega 38.00 67.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -112.0000 -150.0000 29 #__ type_ start__ end____ width___ exp.time_ 79 omega 83.00 159.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 61.0000 60.0000 76 #__ type_ start__ end____ width___ exp.time_ 80 omega 83.00 165.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 61.0000 0.0000 82 #__ type_ start__ end____ width___ exp.time_ 81 omega 103.00 135.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -61.0000 -120.0000 32 #__ type_ start__ end____ width___ exp.time_ 82 omega 79.00 175.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 60.0000 96 #__ type_ start__ end____ width___ exp.time_ 83 omega 54.00 83.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -61.0000 -120.0000 29 #__ type_ start__ end____ width___ exp.time_ 84 omega 37.00 62.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -112.0000 -30.0000 25 ; _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0260622000 _diffrn_orient_matrix_UB_12 -0.0542005000 _diffrn_orient_matrix_UB_13 0.0286708000 _diffrn_orient_matrix_UB_21 0.0467149000 _diffrn_orient_matrix_UB_22 0.0267966000 _diffrn_orient_matrix_UB_23 0.0591500000 _diffrn_orient_matrix_UB_31 -0.0825420000 _diffrn_orient_matrix_UB_32 -0.0019433000 _diffrn_orient_matrix_UB_33 0.0155372000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_source 'SuperNova (Cu) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 6556 _reflns_number_total 6760 _reflns_odcompleteness_completeness 95.00 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 80.95 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.513 _refine_diff_density_min -0.265 _refine_diff_density_rms 0.052 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 437 _refine_ls_number_reflns 6760 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0479 _refine_ls_R_factor_gt 0.0470 _refine_ls_restrained_S_all 1.064 _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^)+(0.0691P)^2^+1.8429P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1295 _refine_ls_wR_factor_ref 0.1303 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.41771(9) -0.12434(17) 0.26972(7) 0.0249(3) Uani 1 1 d . . . H1A H 0.3857 -0.2136 0.2496 0.037 Uiso 1 1 calc R . . H1B H 0.4576 -0.1577 0.3066 0.037 Uiso 1 1 calc R . . H1C H 0.4481 -0.0783 0.2463 0.037 Uiso 1 1 calc R . . C1A C 0.90800(9) -0.13611(17) 0.02732(6) 0.0241(3) Uani 1 1 d . . . H1AA H 0.8777 -0.2272 0.0073 0.036 Uiso 1 1 calc R . . H1AB H 0.9445 -0.1656 0.0658 0.036 Uiso 1 1 calc R . . H1AC H 0.9419 -0.0934 0.0057 0.036 Uiso 1 1 calc R . . C3 C 0.38539(8) 0.14229(16) 0.28230(5) 0.0176(3) Uani 1 1 d . . . C3A C 0.87463(8) 0.13146(16) 0.03586(5) 0.0180(3) Uani 1 1 d . . . C5 C 0.32107(8) 0.25258(15) 0.29108(5) 0.0165(3) Uani 1 1 d . . . C5A C 0.81033(8) 0.24436(16) 0.04253(5) 0.0170(3) Uani 1 1 d . . . C6 C 0.33882(8) 0.41538(16) 0.29028(5) 0.0185(3) Uani 1 1 d . . . H6 H 0.3900 0.4472 0.2861 0.022 Uiso 1 1 calc R . . C6A C 0.82817(8) 0.40635(17) 0.04034(6) 0.0190(3) Uani 1 1 d . . . H6A H 0.8782 0.4369 0.0341 0.023 Uiso 1 1 calc R . . C7 C 0.28197(8) 0.52801(16) 0.29548(5) 0.0181(3) Uani 1 1 d . . . H7 H 0.2939 0.6349 0.2949 0.022 Uiso 1 1 calc R . . C7A C 0.77307(8) 0.52050(16) 0.04723(5) 0.0187(3) Uani 1 1 d . . . H7A H 0.7854 0.6272 0.0462 0.022 Uiso 1 1 calc R . . C8 C 0.20573(8) 0.47529(15) 0.30169(5) 0.0158(2) Uani 1 1 d . . . C8A C 0.69815(8) 0.46953(15) 0.05574(5) 0.0159(2) Uani 1 1 d . . . C10 C 0.12908(8) 0.73177(15) 0.30062(6) 0.0186(3) Uani 1 1 d . . . H10D H 0.1777 0.7814 0.3285 0.028 Uiso 1 1 calc R . . H10E H 0.0782 0.7633 0.3081 0.028 Uiso 1 1 calc R . . H10F H 0.1252 0.7630 0.2617 0.028 Uiso 1 1 calc R . . C10A C 0.62451(8) 0.72676(15) 0.05679(6) 0.0194(3) Uani 1 1 d . . . H10A H 0.6046 0.7534 0.0159 0.029 Uiso 1 1 calc R . . H10B H 0.6789 0.7757 0.0757 0.029 Uiso 1 1 calc R . . H10C H 0.5842 0.7634 0.0745 0.029 Uiso 1 1 calc R . . C11 C 0.07849(8) 0.45753(15) 0.31353(5) 0.0157(2) Uani 1 1 d . . . C11A C 0.57274(8) 0.45425(15) 0.07046(5) 0.0154(2) Uani 1 1 d . . . C12 C 0.00233(8) 0.50881(15) 0.32200(5) 0.0170(3) Uani 1 1 d . . . C12A C 0.49818(8) 0.50577(15) 0.08117(5) 0.0167(3) Uani 1 1 d . . . C13 C -0.06087(8) 0.54422(15) 0.33242(6) 0.0174(3) Uani 1 1 d . . . C13A C 0.43609(8) 0.53800(15) 0.09323(6) 0.0175(3) Uani 1 1 d . . . C14 C 0.24659(8) 0.20051(15) 0.29942(5) 0.0162(2) Uani 1 1 d . . . H14 H 0.2358 0.0934 0.3011 0.019 Uiso 1 1 calc R . . C14A C 0.73629(8) 0.19399(15) 0.05214(5) 0.0168(2) Uani 1 1 d . . . H14A H 0.7252 0.0872 0.0543 0.020 Uiso 1 1 calc R . . C15 C 0.18827(8) 0.31238(15) 0.30527(5) 0.0152(2) Uani 1 1 d . . . C15A C 0.67926(8) 0.30753(15) 0.05848(5) 0.0155(2) Uani 1 1 d . . . C16 C 0.10681(8) 0.30335(15) 0.31400(5) 0.0155(3) Uani 1 1 d . . . C16A C 0.59856(8) 0.29954(15) 0.06805(5) 0.0153(2) Uani 1 1 d . . . C17 C 0.06201(8) 0.17042(15) 0.32450(5) 0.0159(2) Uani 1 1 d . . . C17A C 0.55109(8) 0.16550(15) 0.07383(5) 0.0160(2) Uani 1 1 d . . . C18 C 0.02008(8) 0.06800(15) 0.33574(5) 0.0169(3) Uani 1 1 d . . . C18A C 0.50576(8) 0.05999(15) 0.07818(5) 0.0174(3) Uani 1 1 d . . . C19 C -0.13581(8) 0.57742(16) 0.34934(6) 0.0207(3) Uani 1 1 d . . . H19C H -0.1693 0.6599 0.3243 0.025 Uiso 1 1 calc R . . H19D H -0.1172 0.6156 0.3894 0.025 Uiso 1 1 calc R . . C19A C 0.36093(8) 0.57037(15) 0.11040(6) 0.0192(3) Uani 1 1 d . . . H19A H 0.3133 0.5993 0.0759 0.023 Uiso 1 1 calc R . . H19B H 0.3731 0.6589 0.1373 0.023 Uiso 1 1 calc R . . C20 C -0.19218(8) 0.43067(17) 0.34449(6) 0.0228(3) Uani 1 1 d . . . H20C H -0.2384 0.4560 0.3589 0.027 Uiso 1 1 calc R . . H20D H -0.2171 0.4009 0.3036 0.027 Uiso 1 1 calc R . . C20A C 0.33568(9) 0.42619(16) 0.14004(6) 0.0219(3) Uani 1 1 d . . . H20A H 0.3797 0.4069 0.1775 0.026 Uiso 1 1 calc R . . H20B H 0.2829 0.4488 0.1473 0.026 Uiso 1 1 calc R . . C21 C -0.14249(8) 0.29447(16) 0.37859(6) 0.0204(3) Uani 1 1 d . . . H21 H -0.1111 0.3107 0.4179 0.024 Uiso 1 1 calc R . . C21A C 0.32410(9) 0.28188(16) 0.10278(6) 0.0220(3) Uani 1 1 d . . . H21A H 0.2848 0.2872 0.0650 0.026 Uiso 1 1 calc R . . C22 C -0.14022(8) 0.15255(16) 0.35652(6) 0.0195(3) Uani 1 1 d . . . H22 H -0.1762 0.1346 0.3183 0.023 Uiso 1 1 calc R . . C22A C 0.36515(8) 0.14772(16) 0.11916(6) 0.0199(3) Uani 1 1 d . . . H22A H 0.4006 0.1387 0.1579 0.024 Uiso 1 1 calc R . . C23 C -0.08487(8) 0.01778(16) 0.38748(6) 0.0204(3) Uani 1 1 d . . . H23C H -0.1204 -0.0641 0.3953 0.024 Uiso 1 1 calc R . . H23D H -0.0456 0.0540 0.4248 0.024 Uiso 1 1 calc R . . C23A C 0.35866(8) 0.00874(16) 0.07968(6) 0.0220(3) Uani 1 1 d . . . H23A H 0.3298 0.0406 0.0394 0.026 Uiso 1 1 calc R . . H23B H 0.3243 -0.0722 0.0893 0.026 Uiso 1 1 calc R . . C24 C -0.03370(8) -0.05092(15) 0.35039(6) 0.0179(3) Uani 1 1 d . . . H24C H 0.0021 -0.1361 0.3719 0.021 Uiso 1 1 calc R . . H24D H -0.0731 -0.0945 0.3144 0.021 Uiso 1 1 calc R . . C24A C 0.44685(8) -0.06069(15) 0.08513(6) 0.0191(3) Uani 1 1 d . . . H24A H 0.4713 -0.1101 0.1232 0.023 Uiso 1 1 calc R . . H24B H 0.4397 -0.1413 0.0555 0.023 Uiso 1 1 calc R . . N9 N 0.13837(7) 0.56106(13) 0.30606(5) 0.0165(2) Uani 1 1 d . . . N9A N 0.63336(7) 0.55651(13) 0.06334(5) 0.0160(2) Uani 1 1 d . . . O2 O 0.36015(6) -0.00917(11) 0.27971(4) 0.0212(2) Uani 1 1 d . . . O2A O 0.84765(6) -0.01897(12) 0.03194(4) 0.0221(2) Uani 1 1 d . . . O4 O 0.45213(6) 0.18300(12) 0.27701(4) 0.0229(2) Uani 1 1 d . . . O4A O 0.94373(6) 0.16962(12) 0.03382(4) 0.0226(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0193(6) 0.0228(7) 0.0339(7) -0.0040(6) 0.0106(6) 0.0039(5) C1A 0.0195(6) 0.0240(7) 0.0318(7) -0.0005(6) 0.0127(5) 0.0045(5) C3 0.0145(6) 0.0220(6) 0.0157(5) 0.0008(5) 0.0043(4) 0.0006(5) C3A 0.0147(6) 0.0243(7) 0.0145(5) 0.0001(5) 0.0041(4) 0.0015(5) C5 0.0145(6) 0.0197(6) 0.0149(5) 0.0008(5) 0.0042(4) 0.0007(5) C5A 0.0123(6) 0.0228(6) 0.0154(5) 0.0002(5) 0.0037(4) 0.0019(5) C6 0.0143(6) 0.0232(7) 0.0178(6) 0.0020(5) 0.0049(5) -0.0027(5) C6A 0.0124(6) 0.0250(7) 0.0197(6) 0.0019(5) 0.0054(5) -0.0015(5) C7 0.0176(6) 0.0175(6) 0.0194(6) 0.0010(5) 0.0063(5) -0.0032(5) C7A 0.0151(6) 0.0199(6) 0.0203(6) 0.0018(5) 0.0049(5) -0.0023(5) C8 0.0150(6) 0.0170(6) 0.0152(5) 0.0003(4) 0.0049(4) 0.0000(5) C8A 0.0132(6) 0.0184(6) 0.0157(5) 0.0006(5) 0.0042(4) 0.0007(5) C10 0.0190(6) 0.0146(6) 0.0232(6) 0.0011(5) 0.0085(5) -0.0003(5) C10A 0.0181(6) 0.0149(6) 0.0246(6) 0.0017(5) 0.0065(5) 0.0006(5) C11 0.0149(6) 0.0161(6) 0.0165(5) 0.0000(4) 0.0057(4) -0.0010(5) C11A 0.0137(6) 0.0165(6) 0.0162(5) 0.0001(4) 0.0052(4) -0.0010(4) C12 0.0175(6) 0.0153(6) 0.0182(6) 0.0004(5) 0.0061(5) -0.0004(5) C12A 0.0168(6) 0.0142(6) 0.0187(6) 0.0003(4) 0.0056(5) -0.0003(5) C13 0.0180(6) 0.0145(6) 0.0202(6) 0.0006(5) 0.0071(5) -0.0002(5) C13A 0.0188(6) 0.0136(6) 0.0205(6) -0.0001(5) 0.0074(5) 0.0002(5) C14 0.0146(6) 0.0172(6) 0.0163(5) 0.0004(4) 0.0047(4) -0.0009(5) C14A 0.0156(6) 0.0180(6) 0.0156(5) -0.0008(4) 0.0039(4) -0.0002(5) C15 0.0139(6) 0.0167(6) 0.0145(5) 0.0004(4) 0.0040(4) -0.0013(5) C15A 0.0129(6) 0.0182(6) 0.0150(5) -0.0010(4) 0.0043(4) -0.0010(5) C16 0.0134(6) 0.0167(6) 0.0168(6) -0.0003(4) 0.0057(5) 0.0000(5) C16A 0.0129(6) 0.0170(6) 0.0161(5) -0.0001(4) 0.0048(4) -0.0007(5) C17 0.0140(6) 0.0161(6) 0.0175(6) -0.0006(4) 0.0053(4) 0.0023(5) C17A 0.0142(6) 0.0160(6) 0.0177(6) 0.0002(4) 0.0052(5) 0.0028(5) C18 0.0150(6) 0.0163(6) 0.0195(6) 0.0002(5) 0.0059(5) 0.0023(5) C18A 0.0155(6) 0.0163(6) 0.0212(6) 0.0006(5) 0.0071(5) 0.0031(5) C19 0.0188(6) 0.0196(6) 0.0263(6) 0.0003(5) 0.0112(5) 0.0037(5) C19A 0.0165(6) 0.0167(6) 0.0264(6) -0.0014(5) 0.0098(5) 0.0015(5) C20 0.0158(6) 0.0242(7) 0.0314(7) 0.0009(5) 0.0118(5) 0.0019(5) C20A 0.0204(6) 0.0211(6) 0.0280(7) -0.0010(5) 0.0133(5) 0.0010(5) C21 0.0169(6) 0.0237(7) 0.0234(6) 0.0004(5) 0.0105(5) -0.0006(5) C21A 0.0198(6) 0.0207(6) 0.0279(7) -0.0005(5) 0.0113(5) -0.0019(5) C22 0.0146(6) 0.0224(6) 0.0223(6) 0.0012(5) 0.0074(5) -0.0025(5) C22A 0.0171(6) 0.0204(6) 0.0250(6) 0.0004(5) 0.0108(5) -0.0027(5) C23 0.0190(6) 0.0202(6) 0.0236(6) 0.0021(5) 0.0093(5) -0.0021(5) C23A 0.0189(6) 0.0182(6) 0.0306(7) -0.0012(5) 0.0107(5) -0.0025(5) C24 0.0169(6) 0.0145(6) 0.0228(6) 0.0011(5) 0.0075(5) -0.0014(5) C24A 0.0176(6) 0.0134(6) 0.0287(7) 0.0013(5) 0.0109(5) -0.0001(5) N9 0.0151(5) 0.0155(5) 0.0198(5) 0.0002(4) 0.0070(4) -0.0009(4) N9A 0.0140(5) 0.0149(5) 0.0196(5) 0.0000(4) 0.0064(4) -0.0008(4) O2 0.0149(4) 0.0207(5) 0.0292(5) -0.0030(4) 0.0091(4) 0.0008(4) O2A 0.0150(4) 0.0224(5) 0.0315(5) -0.0008(4) 0.0114(4) 0.0028(4) O4 0.0163(4) 0.0268(5) 0.0280(5) 0.0022(4) 0.0104(4) 0.0004(4) O4A 0.0141(4) 0.0282(5) 0.0277(5) -0.0007(4) 0.0101(4) 0.0000(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C1 O2 1.4437(16) . ? C1A H1AA 0.9600 . ? C1A H1AB 0.9600 . ? C1A H1AC 0.9600 . ? C1A O2A 1.4431(15) . ? C3 C5 1.4889(17) . ? C3 O2 1.3471(16) . ? C3 O4 1.2092(16) . ? C3A C5A 1.4841(17) . ? C3A O2A 1.3460(17) . ? C3A O4A 1.2102(16) . ? C5 C6 1.4143(18) . ? C5 C14 1.3915(17) . ? C5A C6A 1.4112(19) . ? C5A C14A 1.3941(18) . ? C6 H6 0.9300 . ? C6 C7 1.3793(19) . ? C6A H6A 0.9300 . ? C6A C7A 1.3812(19) . ? C7 H7 0.9300 . ? C7 C8 1.3988(17) . ? C7A H7A 0.9300 . ? C7A C8A 1.3974(17) . ? C8 C15 1.4214(17) . ? C8 N9 1.3691(16) . ? C8A C15A 1.4168(18) . ? C8A N9A 1.3681(16) . ? C10 H10D 0.9600 . ? C10 H10E 0.9600 . ? C10 H10F 0.9600 . ? C10 N9 1.4583(16) . ? C10A H10A 0.9600 . ? C10A H10B 0.9600 . ? C10A H10C 0.9600 . ? C10A N9A 1.4557(16) . ? C11 C12 1.4173(17) . ? C11 C16 1.3894(18) . ? C11 N9 1.3843(16) . ? C11A C12A 1.4177(17) . ? C11A C16A 1.3888(18) . ? C11A N9A 1.3838(16) . ? C12 C13 1.1980(19) . ? C12A C13A 1.1947(19) . ? C13 C19 1.4632(17) . ? C13A C19A 1.4689(17) . ? C14 H14 0.9300 . ? C14 C15 1.3976(18) . ? C14A H14A 0.9300 . ? C14A C15A 1.3959(18) . ? C15 C16 1.4409(17) . ? C15A C16A 1.4375(17) . ? C16 C17 1.4209(18) . ? C16A C17A 1.4179(17) . ? C17 C18 1.2011(19) . ? C17A C18A 1.1974(19) . ? C18 C24 1.4683(17) . ? C18A C24A 1.4651(17) . ? C19 H19C 0.9700 . ? C19 H19D 0.9700 . ? C19 C20 1.5392(19) . ? C19A H19A 0.9700 . ? C19A H19B 0.9700 . ? C19A C20A 1.5460(18) . ? C20 H20C 0.9700 . ? C20 H20D 0.9700 . ? C20 C21 1.4976(19) . ? C20A H20A 0.9700 . ? C20A H20B 0.9700 . ? C20A C21A 1.4949(19) . ? C21 H21 0.9300 . ? C21 C22 1.323(2) . ? C21A H21A 0.9300 . ? C21A C22A 1.318(2) . ? C22 H22 0.9300 . ? C22 C23 1.5015(18) . ? C22A H22A 0.9300 . ? C22A C23A 1.4992(19) . ? C23 H23C 0.9700 . ? C23 H23D 0.9700 . ? C23 C24 1.5435(18) . ? C23A H23A 0.9700 . ? C23A H23B 0.9700 . ? C23A C24A 1.5441(18) . ? C24 H24C 0.9700 . ? C24 H24D 0.9700 . ? C24A H24A 0.9700 . ? C24A H24B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O2 C1 H1A 109.5 . . ? O2 C1 H1B 109.5 . . ? O2 C1 H1C 109.5 . . ? H1AA C1A H1AB 109.5 . . ? H1AA C1A H1AC 109.5 . . ? H1AB C1A H1AC 109.5 . . ? O2A C1A H1AA 109.5 . . ? O2A C1A H1AB 109.5 . . ? O2A C1A H1AC 109.5 . . ? O2 C3 C5 112.28(11) . . ? O4 C3 C5 124.32(12) . . ? O4 C3 O2 123.38(12) . . ? O2A C3A C5A 112.64(11) . . ? O4A C3A C5A 124.03(13) . . ? O4A C3A O2A 123.33(12) . . ? C6 C5 C3 116.68(11) . . ? C14 C5 C3 122.51(12) . . ? C14 C5 C6 120.80(12) . . ? C6A C5A C3A 117.18(11) . . ? C14A C5A C3A 121.91(12) . . ? C14A C5A C6A 120.89(12) . . ? C5 C6 H6 119.2 . . ? C7 C6 C5 121.55(12) . . ? C7 C6 H6 119.2 . . ? C5A C6A H6A 119.2 . . ? C7A C6A C5A 121.50(12) . . ? C7A C6A H6A 119.2 . . ? C6 C7 H7 121.3 . . ? C6 C7 C8 117.47(12) . . ? C8 C7 H7 121.3 . . ? C6A C7A H7A 121.3 . . ? C6A C7A C8A 117.42(12) . . ? C8A C7A H7A 121.3 . . ? C7 C8 C15 121.91(12) . . ? N9 C8 C7 129.21(12) . . ? N9 C8 C15 108.88(11) . . ? C7A C8A C15A 121.99(12) . . ? N9A C8A C7A 129.31(12) . . ? N9A C8A C15A 108.69(11) . . ? H10D C10 H10E 109.5 . . ? H10D C10 H10F 109.5 . . ? H10E C10 H10F 109.5 . . ? N9 C10 H10D 109.5 . . ? N9 C10 H10E 109.5 . . ? N9 C10 H10F 109.5 . . ? H10A C10A H10B 109.5 . . ? H10A C10A H10C 109.5 . . ? H10B C10A H10C 109.5 . . ? N9A C10A H10A 109.5 . . ? N9A C10A H10B 109.5 . . ? N9A C10A H10C 109.5 . . ? C16 C11 C12 127.21(12) . . ? N9 C11 C12 122.71(11) . . ? N9 C11 C16 110.02(11) . . ? C16A C11A C12A 126.93(12) . . ? N9A C11A C12A 123.17(11) . . ? N9A C11A C16A 109.84(11) . . ? C13 C12 C11 175.18(14) . . ? C13A C12A C11A 174.33(14) . . ? C12 C13 C19 174.98(14) . . ? C12A C13A C19A 176.81(14) . . ? C5 C14 H14 120.7 . . ? C5 C14 C15 118.69(12) . . ? C15 C14 H14 120.7 . . ? C5A C14A H14A 120.8 . . ? C5A C14A C15A 118.47(12) . . ? C15A C14A H14A 120.8 . . ? C8 C15 C16 106.37(11) . . ? C14 C15 C8 119.46(11) . . ? C14 C15 C16 134.16(12) . . ? C8A C15A C16A 106.67(11) . . ? C14A C15A C8A 119.70(11) . . ? C14A C15A C16A 133.64(12) . . ? C11 C16 C15 106.33(11) . . ? C11 C16 C17 123.56(11) . . ? C17 C16 C15 130.03(11) . . ? C11A C16A C15A 106.29(11) . . ? C11A C16A C17A 124.35(11) . . ? C17A C16A C15A 129.36(11) . . ? C18 C17 C16 173.68(13) . . ? C18A C17A C16A 174.93(13) . . ? C17 C18 C24 177.06(13) . . ? C17A C18A C24A 175.82(13) . . ? C13 C19 H19C 109.2 . . ? C13 C19 H19D 109.2 . . ? C13 C19 C20 112.11(11) . . ? H19C C19 H19D 107.9 . . ? C20 C19 H19C 109.2 . . ? C20 C19 H19D 109.2 . . ? C13A C19A H19A 109.2 . . ? C13A C19A H19B 109.2 . . ? C13A C19A C20A 111.86(11) . . ? H19A C19A H19B 107.9 . . ? C20A C19A H19A 109.2 . . ? C20A C19A H19B 109.2 . . ? C19 C20 H20C 109.2 . . ? C19 C20 H20D 109.2 . . ? H20C C20 H20D 107.9 . . ? C21 C20 C19 111.92(11) . . ? C21 C20 H20C 109.2 . . ? C21 C20 H20D 109.2 . . ? C19A C20A H20A 109.3 . . ? C19A C20A H20B 109.3 . . ? H20A C20A H20B 108.0 . . ? C21A C20A C19A 111.62(11) . . ? C21A C20A H20A 109.3 . . ? C21A C20A H20B 109.3 . . ? C20 C21 H21 117.8 . . ? C22 C21 C20 124.40(13) . . ? C22 C21 H21 117.8 . . ? C20A C21A H21A 117.4 . . ? C22A C21A C20A 125.25(13) . . ? C22A C21A H21A 117.4 . . ? C21 C22 H22 117.0 . . ? C21 C22 C23 125.97(12) . . ? C23 C22 H22 117.0 . . ? C21A C22A H22A 117.7 . . ? C21A C22A C23A 124.64(13) . . ? C23A C22A H22A 117.7 . . ? C22 C23 H23C 109.4 . . ? C22 C23 H23D 109.4 . . ? C22 C23 C24 111.24(11) . . ? H23C C23 H23D 108.0 . . ? C24 C23 H23C 109.4 . . ? C24 C23 H23D 109.4 . . ? C22A C23A H23A 109.1 . . ? C22A C23A H23B 109.1 . . ? C22A C23A C24A 112.48(11) . . ? H23A C23A H23B 107.8 . . ? C24A C23A H23A 109.1 . . ? C24A C23A H23B 109.1 . . ? C18 C24 C23 112.32(11) . . ? C18 C24 H24C 109.1 . . ? C18 C24 H24D 109.1 . . ? C23 C24 H24C 109.1 . . ? C23 C24 H24D 109.1 . . ? H24C C24 H24D 107.9 . . ? C18A C24A C23A 112.05(11) . . ? C18A C24A H24A 109.2 . . ? C18A C24A H24B 109.2 . . ? C23A C24A H24A 109.2 . . ? C23A C24A H24B 109.2 . . ? H24A C24A H24B 107.9 . . ? C8 N9 C10 125.87(11) . . ? C8 N9 C11 108.37(11) . . ? C11 N9 C10 125.69(11) . . ? C8A N9A C10A 125.19(11) . . ? C8A N9A C11A 108.50(10) . . ? C11A N9A C10A 125.79(11) . . ? C3 O2 C1 116.13(10) . . ? C3A O2A C1A 115.78(10) . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 C5 C6 C7 177.22(11) . . . . ? C3 C5 C14 C15 -177.78(11) . . . . ? C3A C5A C6A C7A -178.75(11) . . . . ? C3A C5A C14A C15A 179.43(11) . . . . ? C5 C3 O2 C1 178.44(10) . . . . ? C5 C6 C7 C8 0.07(18) . . . . ? C5 C14 C15 C8 0.95(17) . . . . ? C5 C14 C15 C16 179.80(12) . . . . ? C5A C3A O2A C1A -178.02(10) . . . . ? C5A C6A C7A C8A -0.80(18) . . . . ? C5A C14A C15A C8A -0.73(18) . . . . ? C5A C14A C15A C16A 179.33(12) . . . . ? C6 C5 C14 C15 1.87(18) . . . . ? C6 C7 C8 C15 2.82(18) . . . . ? C6 C7 C8 N9 -178.10(12) . . . . ? C6A C5A C14A C15A 1.17(18) . . . . ? C6A C7A C8A C15A 1.24(18) . . . . ? C6A C7A C8A N9A -179.66(12) . . . . ? C7 C8 C15 C14 -3.38(18) . . . . ? C7 C8 C15 C16 177.48(11) . . . . ? C7 C8 N9 C10 5.0(2) . . . . ? C7 C8 N9 C11 -178.02(12) . . . . ? C7A C8A C15A C14A -0.49(19) . . . . ? C7A C8A C15A C16A 179.47(11) . . . . ? C7A C8A N9A C10A 8.1(2) . . . . ? C7A C8A N9A C11A -179.67(12) . . . . ? C8 C15 C16 C11 1.70(13) . . . . ? C8 C15 C16 C17 -175.07(12) . . . . ? C8A C15A C16A C11A 0.15(14) . . . . ? C8A C15A C16A C17A 179.72(12) . . . . ? C11 C12 C13 C19 2(3) . . . . ? C11 C16 C17 C18 -19.0(13) . . . . ? C11A C12A C13A C19A 7(4) . . . . ? C11A C16A C17A C18A 12.8(16) . . . . ? C12 C11 C16 C15 -178.22(12) . . . . ? C12 C11 C16 C17 -1.2(2) . . . . ? C12 C11 N9 C8 177.27(11) . . . . ? C12 C11 N9 C10 -5.74(19) . . . . ? C12 C13 C19 C20 -60.7(16) . . . . ? C12A C11A C16A C15A -177.73(12) . . . . ? C12A C11A C16A C17A 2.7(2) . . . . ? C12A C11A N9A C8A 177.98(11) . . . . ? C12A C11A N9A C10A -9.89(19) . . . . ? C12A C13A C19A C20A -20(3) . . . . ? C13 C19 C20 C21 54.53(15) . . . . ? C13A C19A C20A C21A -53.64(15) . . . . ? C14 C5 C6 C7 -2.44(19) . . . . ? C14 C15 C16 C11 -177.26(13) . . . . ? C14 C15 C16 C17 6.0(2) . . . . ? C14A C5A C6A C7A -0.41(19) . . . . ? C14A C15A C16A C11A -179.91(13) . . . . ? C14A C15A C16A C17A -0.3(2) . . . . ? C15 C8 N9 C10 -175.83(11) . . . . ? C15 C8 N9 C11 1.15(13) . . . . ? C15 C16 C17 C18 157.2(12) . . . . ? C15A C8A N9A C10A -172.66(11) . . . . ? C15A C8A N9A C11A -0.47(13) . . . . ? C15A C16A C17A C18A -166.7(14) . . . . ? C16 C11 C12 C13 42.3(17) . . . . ? C16 C11 N9 C8 -0.05(14) . . . . ? C16 C11 N9 C10 176.94(11) . . . . ? C16 C17 C18 C24 7(4) . . . . ? C16A C11A C12A C13A 32.5(14) . . . . ? C16A C11A N9A C8A 0.58(14) . . . . ? C16A C11A N9A C10A 172.71(11) . . . . ? C16A C17A C18A C24A -27(3) . . . . ? C17 C18 C24 C23 -15(3) . . . . ? C17A C18A C24A C23A 28(2) . . . . ? C19 C20 C21 C22 -126.69(14) . . . . ? C19A C20A C21A C22A 123.31(14) . . . . ? C20 C21 C22 C23 173.74(12) . . . . ? C20A C21A C22A C23A -174.31(12) . . . . ? C21 C22 C23 C24 -127.76(14) . . . . ? C21A C22A C23A C24A 133.03(14) . . . . ? C22 C23 C24 C18 57.69(14) . . . . ? C22A C23A C24A C18A -51.90(15) . . . . ? N9 C8 C15 C14 177.37(10) . . . . ? N9 C8 C15 C16 -1.77(13) . . . . ? N9 C11 C12 C13 -134.5(16) . . . . ? N9 C11 C16 C15 -1.05(14) . . . . ? N9 C11 C16 C17 175.99(11) . . . . ? N9A C8A C15A C14A -179.76(10) . . . . ? N9A C8A C15A C16A 0.20(14) . . . . ? N9A C11A C12A C13A -144.4(13) . . . . ? N9A C11A C16A C15A -0.44(14) . . . . ? N9A C11A C16A C17A 179.96(11) . . . . ? O2 C3 C5 C6 -175.68(11) . . . . ? O2 C3 C5 C14 3.97(17) . . . . ? O2A C3A C5A C6A -172.99(11) . . . . ? O2A C3A C5A C14A 8.69(17) . . . . ? O4 C3 C5 C6 3.07(18) . . . . ? O4 C3 C5 C14 -177.28(12) . . . . ? O4 C3 O2 C1 -0.32(18) . . . . ? O4A C3A C5A C6A 6.65(19) . . . . ? O4A C3A C5A C14A -171.67(12) . . . . ? O4A C3A O2A C1A 2.34(18) . . . . ?