#------------------------------------------------------------------------------ #$Date: 2019-11-08 03:36:45 +0200 (Fri, 08 Nov 2019) $ #$Revision: 225121 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/15/69/7156916.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_7156916 loop_ _publ_author_name 'Peng, Fei' 'Tian, Hua' 'Zhang, Pengxiang' 'Yang, Haijun' 'Fu, Hua' _publ_section_title ; Iridium-catalyzed intramolecular enantioselective allylation of quinazolin-4(3H)-one derivatives. ; _journal_issue 26 _journal_name_full 'Organic & biomolecular chemistry' _journal_page_first 6461 _journal_page_last 6464 _journal_paper_doi 10.1039/c9ob01057b _journal_volume 17 _journal_year 2019 _chemical_absolute_configuration ad _chemical_formula_moiety 'C21 H21 N3 O' _chemical_formula_sum 'C21 H21 N3 O' _chemical_formula_weight 331.41 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _audit_creation_date 2019-02-21 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 90 _cell_angle_beta 94.683(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 9.1516(2) _cell_length_b 5.26734(13) _cell_length_c 17.9860(4) _cell_measurement_reflns_used 5070 _cell_measurement_temperature 173.01(10) _cell_measurement_theta_max 71.1260 _cell_measurement_theta_min 4.8240 _cell_volume 864.11(3) _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 173.01(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.2137 _diffrn_detector_type AtlasS2 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w -107.00 -14.00 1.00 1.00 -- -40.81 -57.00 0.00 93 2 \w -64.00 30.00 1.00 1.00 -- -40.81 57.00 150.00 94 3 \w -78.00 -3.00 1.00 1.00 -- -40.81 125.00-150.00 75 4 \w 105.00 170.00 1.00 4.00 -- 100.91 125.00-180.00 65 5 \w 145.00 174.00 1.00 4.00 -- 100.91 125.00 120.00 29 6 \w 55.00 114.00 1.00 4.00 -- 100.91-125.00-120.00 59 7 \w 29.00 68.00 1.00 4.00 -- 100.91-125.00 60.00 39 8 \w 77.00 162.00 1.00 4.00 -- 100.91 45.00 -60.00 85 9 \w 74.00 172.00 1.00 4.00 -- 100.91 30.00-120.00 98 10 \w 93.00 118.00 1.00 4.00 -- 100.91-125.00 60.00 25 11 \w 29.00 55.00 1.00 4.00 -- 100.91-125.00 150.00 26 12 \w 76.00 104.00 1.00 4.00 -- 100.91-125.00 150.00 28 13 \w 32.00 126.00 1.00 4.00 -- 100.91 -45.00 60.00 94 14 \w 85.00 133.00 1.00 4.00 -- 100.91 45.00 0.00 48 15 \w 32.00 128.00 1.00 4.00 -- 100.91 -61.00-150.00 96 16 \w -70.00 -27.00 1.00 1.00 -- -40.81 -38.00 90.00 43 17 \w -71.00 -10.00 1.00 1.00 -- -40.81 125.00 -60.00 61 18 \w 8.00 101.00 1.00 1.00 -- 40.81 77.00 90.00 93 19 \w 78.00 107.00 1.00 1.00 -- 40.81 77.00-120.00 29 20 \w 23.00 73.00 1.00 1.00 -- 40.81 77.00-120.00 50 21 \w 8.00 108.00 1.00 1.00 -- 40.81 77.00-180.00 100 22 \w 10.00 64.00 1.00 1.00 -- 40.81 77.00 -30.00 54 23 \w 68.00 94.00 1.00 4.00 -- 100.29 77.00-120.00 26 24 \w 68.00 174.00 1.00 4.00 -- 100.29 77.00 60.00 106 25 \w 104.00 136.00 1.00 4.00 -- 100.29 61.00 30.00 32 26 \w 77.00 102.00 1.00 4.00 -- 100.29 61.00 60.00 25 27 \w 71.00 97.00 1.00 4.00 -- 100.29 61.00 -60.00 26 28 \w 71.00 96.00 1.00 4.00 -- 100.29 61.00-150.00 25 29 \w 68.00 148.00 1.00 4.00 -- 100.29 77.00 30.00 80 30 \w 71.00 97.00 1.00 4.00 -- 100.29 61.00 0.00 26 31 \w 73.00 148.00 1.00 4.00 -- 100.29 61.00 120.00 75 32 \w 73.00 99.00 1.00 4.00 -- 100.29 61.00 -30.00 26 33 \w 72.00 136.00 1.00 4.00 -- 100.29 61.00-180.00 64 34 \w 68.00 94.00 1.00 4.00 -- 100.29 77.00 120.00 26 35 \w 135.00 169.00 1.00 4.00 -- 100.29 77.00 120.00 34 36 \w 68.00 94.00 1.00 4.00 -- 100.29 77.00 -60.00 26 37 \w 76.00 102.00 1.00 4.00 -- 100.29 61.00 -90.00 26 38 \w 69.00 95.00 1.00 4.00 -- 100.29 77.00 90.00 26 39 \w 69.00 95.00 1.00 4.00 -- 100.29 77.00-150.00 26 40 \w 69.00 95.00 1.00 4.00 -- 100.29 77.00 -30.00 26 41 \w 140.00 166.00 1.00 4.00 -- 100.29 77.00 -30.00 26 42 \w 68.00 94.00 1.00 4.00 -- 100.29 77.00 0.00 26 43 \w 115.00 152.00 1.00 4.00 -- 100.29 77.00 0.00 37 44 \w 68.00 94.00 1.00 4.00 -- 100.29 77.00 150.00 26 45 \w 76.00 102.00 1.00 4.00 -- 100.29 61.00-120.00 26 46 \w 73.00 99.00 1.00 4.00 -- 100.29 61.00 150.00 26 47 \w 75.00 101.00 1.00 4.00 -- 100.29 61.00 30.00 26 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, AtlasS2' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0619247000 _diffrn_orient_matrix_UB_12 -0.0361452000 _diffrn_orient_matrix_UB_13 -0.0764177000 _diffrn_orient_matrix_UB_21 -0.1570327000 _diffrn_orient_matrix_UB_22 -0.0019704000 _diffrn_orient_matrix_UB_23 -0.0380904000 _diffrn_orient_matrix_UB_31 0.0066730000 _diffrn_orient_matrix_UB_32 0.2901851000 _diffrn_orient_matrix_UB_33 -0.0097200000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_unetI/netI 0.0378 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.988 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 12553 _diffrn_reflns_point_group_measured_fraction_full 0.951 _diffrn_reflns_point_group_measured_fraction_max 0.932 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 71.514 _diffrn_reflns_theta_min 4.848 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 0.631 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.80690 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear colourless' _exptl_crystal_density_diffrn 1.274 _exptl_crystal_description needle _exptl_crystal_F_000 352 _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.137 _refine_diff_density_min -0.166 _refine_diff_density_rms 0.035 _refine_ls_abs_structure_details ; Flack x determined using 1112 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.1(2) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 235 _refine_ls_number_reflns 3145 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.053 _refine_ls_R_factor_all 0.0395 _refine_ls_R_factor_gt 0.0363 _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^)+(0.0470P)^2^+0.0952P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0911 _refine_ls_wR_factor_ref 0.0936 _reflns_Friedel_coverage 0.692 _reflns_Friedel_fraction_full 0.892 _reflns_Friedel_fraction_max 0.862 _reflns_number_gt 2966 _reflns_number_total 3145 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9ob01057b2.cif _cod_data_source_block 20190219pengfei-whitebottle _cod_depositor_comments 'Adding full bibliography for 7156916.cif.' _cod_database_code 7156916 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _reflns_odcompleteness_completeness 99.94 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 64.99 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C00C(H00D) 2.b Secondary CH2 refined with riding coordinates: C00A(H00A,H00B), C00E(H00F,H00G), C00F(H00H,H00I) 2.c Aromatic/amide H refined with riding coordinates: C00B(H00C), C00D(H00E), C00G(H00J), C00H(H00K), C00J(H00L), C00K(H00M), C00L(H00N), C00M(H00O), C00N(H00P) 2.d Idealised Me refined as rotating group: C00O(H00Q,H00R,H00S) ; _shelx_res_file ; 20190219pengfei-whitebottle.res created by SHELXL-2014/7 TITL 20190219pengfei-whitebottle_a.res in P2(1) REM Old TITL 20190219pengfei-whitebottle in P21/m #11 REM SHELXT solution in P2(1) REM R1 0.099, Rweak 0.019, Alpha 0.001, Orientation as input REM Flack x = -0.020 ( 0.181 ) from Parsons' quotients REM Formula found by SHELXT: C20 N3 O2 CELL 1.54184 9.151567 5.267338 17.985994 90 94.6833 90 ZERR 2 0.000196 0.000135 0.000404 0 0.002 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H N O UNIT 42 42 6 2 L.S. 10 PLAN 20 BOND $H LIST 6 MORE -1 CONF fmap 2 ACTA REM REM REM WGHT 0.047000 0.095200 FVAR 1.03601 O001 4 0.484860 0.347576 0.903986 11.00000 0.03094 0.04525 = 0.02847 -0.00393 -0.00680 0.00968 N002 3 0.128788 0.480930 0.758341 11.00000 0.02291 0.03204 = 0.02345 0.00125 0.00094 0.00114 N003 3 0.354714 0.276159 0.792521 11.00000 0.02390 0.02634 = 0.02222 0.00128 0.00134 0.00160 N004 3 0.339807 0.057929 0.650168 11.00000 0.02598 0.02342 = 0.02309 -0.00099 0.00027 0.00077 C005 1 0.229996 0.319524 0.745695 11.00000 0.02143 0.02630 = 0.02309 0.00167 0.00126 -0.00144 C006 1 0.378154 0.400515 0.861613 11.00000 0.02706 0.03213 = 0.02174 0.00066 0.00035 -0.00050 C007 1 0.269589 0.594494 0.875099 11.00000 0.02635 0.02970 = 0.02335 0.00438 0.00523 -0.00133 C008 1 0.148724 0.627196 0.822807 11.00000 0.02365 0.02824 = 0.02306 0.00168 0.00463 -0.00040 C009 1 0.261261 0.051037 0.515644 11.00000 0.02553 0.02695 = 0.02555 -0.00379 0.00438 0.00200 C00A 1 0.417445 -0.081478 0.711612 11.00000 0.02828 0.02216 = 0.02735 0.00145 0.00146 0.00101 AFIX 23 H00A 2 0.498504 -0.175332 0.693454 11.00000 -1.20000 H00B 2 0.351512 -0.201711 0.732341 11.00000 -1.20000 AFIX 0 C00B 1 0.339649 0.266270 0.499568 11.00000 0.02610 0.02779 = 0.03138 -0.00403 -0.00041 -0.00167 AFIX 43 H00C 2 0.415980 0.320580 0.533108 11.00000 -1.20000 AFIX 0 C00C 1 0.474925 0.105806 0.771709 11.00000 0.02535 0.02634 = 0.02557 0.00057 -0.00014 0.00460 AFIX 13 H00D 2 0.510877 0.009137 0.816039 11.00000 -1.20000 AFIX 0 C00D 1 0.047958 0.819329 0.835077 11.00000 0.02553 0.03642 = 0.02738 0.00168 0.00271 0.00330 AFIX 43 H00E 2 -0.033288 0.843512 0.801274 11.00000 -1.20000 AFIX 0 C00E 1 0.303974 -0.104443 0.584915 11.00000 0.02999 0.02399 = 0.02854 -0.00267 0.00239 -0.00053 AFIX 23 H00F 2 0.223614 -0.216281 0.594808 11.00000 -1.20000 H00G 2 0.388161 -0.209071 0.576289 11.00000 -1.20000 AFIX 0 C00F 1 0.205958 0.160796 0.676097 11.00000 0.02412 0.03569 = 0.02534 -0.00257 -0.00012 0.00021 AFIX 23 H00H 2 0.140818 0.021443 0.685712 11.00000 -1.20000 H00I 2 0.157570 0.263995 0.636764 11.00000 -1.20000 AFIX 0 C00G 1 0.288000 0.750441 0.938252 11.00000 0.02959 0.03499 = 0.02282 0.00149 0.00279 0.00156 AFIX 43 H00J 2 0.368163 0.725457 0.972687 11.00000 -1.20000 AFIX 0 C00H 1 0.306494 0.401944 0.434543 11.00000 0.03318 0.03259 = 0.03483 0.00270 0.00373 -0.00294 AFIX 43 H00K 2 0.359408 0.547316 0.424863 11.00000 -1.20000 AFIX 0 C00I 1 0.188885 0.940507 0.950063 11.00000 0.03588 0.03173 = 0.02530 0.00041 0.00867 -0.00007 C00J 1 0.600095 0.261817 0.746580 11.00000 0.02782 0.03043 = 0.03661 -0.00794 0.00623 0.00114 AFIX 43 H00L 2 0.585315 0.350458 0.701880 11.00000 -1.20000 AFIX 0 C00K 1 0.068586 0.972622 0.896952 11.00000 0.03003 0.03200 = 0.03245 0.00206 0.00943 0.00742 AFIX 43 H00M 2 0.001237 1.100951 0.903886 11.00000 -1.20000 AFIX 0 C00L 1 0.147435 -0.026230 0.464955 11.00000 0.03086 0.03743 = 0.03178 -0.00388 0.00176 -0.00667 AFIX 43 H00N 2 0.092268 -0.168434 0.475176 11.00000 -1.20000 AFIX 0 C00M 1 0.115359 0.107574 0.399005 11.00000 0.03151 0.05233 = 0.03032 -0.00168 -0.00514 -0.00577 AFIX 43 H00O 2 0.040074 0.052400 0.364975 11.00000 -1.20000 AFIX 0 C00N 1 0.193922 0.320226 0.383797 11.00000 0.03565 0.04510 = 0.02870 0.00437 0.00029 0.00114 AFIX 43 H00P 2 0.171893 0.409364 0.339669 11.00000 -1.20000 AFIX 0 C00O 1 0.207352 1.109744 1.017496 11.00000 0.04906 0.04173 = 0.03303 -0.00739 0.00478 0.01026 AFIX 137 H00Q 2 0.144242 1.052445 1.054155 11.00000 -1.50000 H00R 2 0.182178 1.280906 1.003287 11.00000 -1.50000 H00S 2 0.307426 1.103934 1.038099 11.00000 -1.50000 AFIX 0 C00P 1 0.728607 0.279428 0.784253 11.00000 0.02770 0.06434 = 0.05622 -0.01693 0.00307 -0.00386 H00T 2 0.806965 0.374637 0.763339 11.00000 0.05785 H00U 2 0.747395 0.203137 0.833419 11.00000 0.06744 HKLF 4 REM 20190219pengfei-whitebottle_a.res in P2(1) REM R1 = 0.0363 for 2966 Fo > 4sig(Fo) and 0.0395 for all 3145 data REM 235 parameters refined using 1 restraints END WGHT 0.0470 0.0952 REM Highest difference peak 0.137, deepest hole -0.166, 1-sigma level 0.035 Q1 1 0.2059 0.5992 0.8535 11.00000 0.05 0.14 Q2 1 0.2838 0.4455 0.8774 11.00000 0.05 0.13 Q3 1 0.5597 0.3066 0.6738 11.00000 0.05 0.12 Q4 1 0.3128 0.3120 0.7656 11.00000 0.05 0.11 Q5 1 0.2798 -0.0161 0.5477 11.00000 0.05 0.11 Q6 1 0.3739 -0.2571 0.7407 11.00000 0.05 0.11 Q7 1 0.2454 1.0079 1.0615 11.00000 0.05 0.11 Q8 1 0.3015 -0.1066 0.4056 11.00000 0.05 0.10 Q9 1 0.5619 -0.1650 0.6799 11.00000 0.05 0.10 Q10 1 0.2402 0.9208 1.0698 11.00000 0.05 0.10 Q11 1 0.2769 0.2037 0.5210 11.00000 0.05 0.10 Q12 1 0.1887 0.6923 0.7081 11.00000 0.05 0.10 Q13 1 0.1652 1.4163 0.9314 11.00000 0.05 0.10 Q14 1 0.2884 0.7269 0.8886 11.00000 0.05 0.10 Q15 1 0.4726 0.4869 0.9451 11.00000 0.05 0.10 Q16 1 0.2512 0.6031 0.9214 11.00000 0.05 0.10 Q17 1 0.0379 0.8288 0.8769 11.00000 0.05 0.10 Q18 1 0.2861 0.3218 0.3979 11.00000 0.05 0.10 Q19 1 0.2978 0.4058 0.6248 11.00000 0.05 0.10 Q20 1 0.2019 -0.2284 0.7114 11.00000 0.05 0.09 ; _shelx_res_checksum 23647 _shelx_hkl_file ; 0 0 2 241.53 9.84 0 0 -2 246.86 9.24 0 0 3 970.27 33.38 0 0 -3 965.96 32.24 0 0 -4 200.46 9.48 0 0 4 203.63 10.84 0 0 5 14.94 3.09 0 0 -5 11.80 2.67 0 0 6 397.01 19.63 0 0 -6 414.96 21.48 0 0 -6 418.88 18.15 0 0 -7 407.75 18.41 0 0 7 406.46 20.81 0 0 -7 389.85 22.44 0 0 8 292.37 18.01 0 0 -8 303.58 20.07 0 0 -8 276.80 15.03 0 0 9 14.55 4.07 0 0 9 20.93 5.24 0 0 -9 18.09 5.37 0 0 -9 11.82 3.29 0 0 -10 0.63 3.46 0 0 10 2.19 2.30 0 0 10 4.52 3.37 0 0 11 187.28 16.71 0 0 -11 160.56 17.53 0 0 12 112.76 8.19 0 0 -12 114.47 8.04 0 0 -12 106.69 7.93 0 0 12 112.27 7.51 0 0 12 128.21 14.69 0 0 12 113.43 7.63 0 0 -12 120.82 16.07 0 0 12 95.63 7.01 0 0 -13 15.86 6.91 0 0 13 15.69 3.05 0 0 13 13.89 2.74 0 0 -13 10.13 2.77 0 0 -13 21.89 3.90 0 0 13 7.06 3.79 0 0 13 18.76 3.61 0 0 13 14.71 2.93 0 0 -13 12.17 2.36 0 0 -13 16.17 2.98 0 0 14 31.56 4.68 0 0 14 21.31 3.56 0 0 -14 23.70 3.77 0 0 -14 29.60 4.65 0 0 14 27.40 4.27 0 0 14 23.32 6.99 0 0 -14 15.67 8.20 0 0 15 11.82 7.71 0 0 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-3 4.00 2.66 -9 -1 3 0.88 2.09 -9 1 2 31.44 3.85 9 1 -2 24.84 4.45 -9 -1 2 27.79 3.82 -9 -1 2 32.77 4.28 -9 1 2 30.84 4.19 -9 -1 2 30.32 4.55 9 -1 -2 30.69 4.65 -9 -1 2 25.62 4.39 9 1 -1 83.33 8.39 -9 1 1 88.89 7.18 -9 -1 1 97.95 7.15 -9 -1 1 97.70 8.07 9 -1 -1 105.57 8.41 -9 1 1 95.71 7.14 -9 -1 1 94.47 8.31 9 1 0 73.78 7.77 -9 1 0 68.22 6.02 -9 -1 0 73.63 5.98 -9 -1 0 91.76 7.57 9 -1 0 72.18 5.71 9 -1 0 68.43 6.65 -9 1 0 70.95 6.10 -9 -1 0 68.63 7.10 9 1 1 120.81 10.14 9 -1 1 118.06 9.62 -9 -1 -1 117.69 7.66 -9 -1 -1 116.03 8.73 9 -1 1 103.55 7.22 9 -1 1 109.98 8.68 -9 1 -1 117.06 8.19 -9 -1 -1 106.83 8.88 -9 1 -2 22.34 3.53 9 1 2 23.09 4.64 9 -1 2 26.24 4.59 -9 1 -2 27.02 4.41 -9 -1 -2 29.50 3.85 -9 1 -2 24.15 3.44 9 -1 2 25.81 4.19 -9 -1 -2 28.19 4.08 -9 -1 -2 30.71 4.54 -9 1 -3 23.92 3.77 9 1 3 28.16 4.72 9 -1 3 27.29 4.62 -9 1 -3 28.80 4.36 -9 -1 -3 25.10 3.48 9 -1 3 19.07 3.47 -9 -1 -3 27.82 4.13 -9 -1 -3 22.49 3.68 -9 1 -4 10.99 2.57 9 1 4 2.88 2.71 9 -1 4 12.17 3.29 -9 1 -4 7.17 2.30 -9 -1 -4 10.30 2.56 9 -1 4 8.37 2.53 -9 -1 -4 10.75 2.65 -9 -1 -4 11.31 2.76 9 1 5 76.30 7.83 9 -1 5 73.88 7.47 -9 1 -5 74.78 6.62 -9 -1 -5 77.13 6.12 -9 -1 -5 76.55 6.27 9 -1 5 60.55 5.61 -9 1 -5 63.46 5.71 -9 -1 -5 67.49 5.94 9 1 6 86.11 7.90 9 -1 6 82.73 7.76 -9 1 -6 92.09 7.15 -9 -1 -6 95.29 6.72 -9 -1 -6 90.63 6.66 9 -1 6 73.14 5.94 -9 1 -6 82.78 6.44 9 1 7 120.08 9.07 9 -1 7 118.15 9.10 -9 1 -7 125.62 7.74 -9 1 -7 126.66 8.23 -9 -1 -7 110.88 7.39 -9 -1 -7 128.53 7.67 -9 1 -7 92.64 6.95 9 1 8 13.33 3.12 9 -1 8 19.82 3.80 -9 1 -8 13.23 2.35 -9 1 -8 11.40 2.52 -9 -1 -8 18.33 2.85 -9 -1 -8 13.90 2.45 9 1 9 -0.89 1.72 9 -1 9 0.44 1.61 -9 1 -9 0.99 1.18 -9 1 -9 0.69 1.36 -9 -1 -9 0.40 1.13 -9 -1 -9 0.57 1.10 -9 1 -10 14.15 2.22 9 1 10 19.92 3.17 9 -1 10 18.63 3.38 -9 1 -10 21.76 2.41 -9 1 -10 19.17 2.56 -9 -1 -10 17.67 2.44 9 -1 11 8.47 2.22 -9 1 -11 8.40 1.70 -9 -2 12 24.30 2.73 -9 -2 11 31.05 3.13 9 2 -11 34.17 3.38 -9 2 11 28.79 3.42 9 -2 -11 32.59 3.52 -9 -2 11 34.98 3.49 -9 -2 10 71.91 5.27 -9 2 10 82.14 6.11 9 2 -10 89.16 5.44 9 2 -10 82.86 5.77 -9 -2 10 88.23 6.57 9 -2 -10 86.48 6.31 -9 -2 10 81.61 5.85 -9 -2 9 8.35 1.93 -9 2 9 7.66 2.17 9 2 -9 7.10 1.68 -9 -2 9 6.93 2.13 9 -2 -9 5.82 2.23 -9 2 9 5.88 1.73 -9 2 8 8.73 2.01 9 -2 -8 7.77 2.09 -9 -2 8 8.17 2.06 -9 2 8 12.74 2.76 9 2 -8 11.55 2.11 -9 -2 8 11.48 2.23 -9 -2 8 12.88 3.00 9 -2 -8 8.94 2.68 -9 2 7 12.10 2.36 9 2 -7 15.11 3.05 9 -2 -7 11.88 2.46 -9 -2 7 17.90 2.86 -9 -2 7 17.64 3.03 -9 2 7 10.81 2.48 9 2 -7 11.81 2.28 -9 -2 7 16.19 3.04 -9 -2 7 14.50 2.76 9 -2 -7 16.68 3.44 -9 2 6 10.78 2.44 9 2 -6 14.75 3.38 9 -2 -6 14.06 2.68 -9 -2 6 10.99 2.31 -9 -2 6 15.38 3.03 9 2 -6 13.06 2.30 -9 2 6 10.71 2.43 -9 -2 6 12.16 2.88 -9 -2 6 11.03 2.35 9 -2 -6 12.86 3.28 9 2 -5 52.33 6.08 9 -2 -5 49.07 4.77 -9 -2 5 53.42 4.56 -9 2 5 45.40 4.79 -9 -2 5 50.08 5.11 -9 -2 5 58.01 5.34 9 2 -5 59.16 4.80 -9 -2 5 54.64 5.74 9 -2 -5 46.72 5.51 -9 2 5 49.35 4.84 -9 2 4 27.90 3.81 9 2 -4 25.06 4.55 9 -2 -4 29.94 3.86 -9 -2 4 38.19 3.84 -9 -2 4 30.87 4.18 9 -2 -4 25.63 3.81 9 2 -4 29.18 3.37 -9 2 4 27.93 3.76 -9 -2 4 28.59 4.30 -9 -2 4 33.14 4.15 9 -2 -4 41.43 5.32 -9 -2 4 23.35 4.22 9 2 -3 61.68 6.81 -9 2 3 65.24 5.25 9 -2 -3 66.68 5.68 -9 2 3 57.72 5.33 -9 -2 3 60.63 5.76 -9 -2 3 67.75 6.02 9 2 -3 66.49 5.21 9 -2 -3 56.32 5.43 9 -2 -3 66.82 6.71 -9 2 3 57.31 5.50 -9 -2 3 66.28 6.88 -9 2 2 20.12 3.34 9 2 -2 22.93 4.36 -9 2 2 21.29 3.05 9 -2 -2 21.53 3.26 -9 -2 2 23.35 3.46 9 -2 -2 18.16 3.17 9 2 -2 24.50 3.15 -9 2 2 15.19 2.89 -9 -2 2 18.66 3.45 9 -2 -2 20.89 3.78 -9 -2 2 17.34 3.74 -9 2 1 26.31 4.00 9 2 -1 30.60 5.00 -9 2 1 31.38 3.84 9 -2 -1 36.51 4.00 -9 -2 1 30.44 3.96 9 2 -1 36.36 3.76 9 -2 -1 35.47 4.11 -9 -2 1 32.32 4.21 9 -2 -1 35.06 4.95 -9 -2 1 25.10 4.30 -9 2 0 31.27 4.19 9 2 0 35.53 5.22 -9 2 0 29.94 3.81 -9 -2 0 30.16 3.74 9 -2 0 25.53 3.49 9 2 0 28.70 3.27 9 -2 0 26.94 4.40 -9 -2 0 28.56 3.97 -9 -2 0 27.03 4.33 -9 2 -1 -0.34 1.50 9 2 1 1.67 2.38 -9 2 -1 1.88 1.95 -9 -2 -1 4.72 1.84 9 -2 1 4.23 1.98 9 2 1 3.78 1.64 9 -2 1 3.09 2.31 -9 -2 -1 4.72 2.19 -9 -2 -1 0.93 1.86 9 2 2 43.20 5.78 -9 2 -2 43.43 4.62 -9 -2 -2 47.99 4.42 -9 -2 -2 49.84 5.18 9 -2 2 41.10 4.20 9 -2 2 44.87 5.29 -9 2 -2 43.94 4.75 -9 -2 -2 41.86 5.50 -9 2 -3 8.66 2.49 9 2 3 6.19 2.52 -9 2 -3 11.98 2.66 -9 -2 -3 6.54 1.74 9 -2 3 5.29 1.78 9 -2 3 3.55 1.89 -9 -2 -3 9.18 2.42 -9 -2 -3 7.00 2.72 9 2 4 46.27 5.56 -9 2 -4 48.35 4.72 -9 -2 -4 52.42 5.19 9 -2 4 44.16 3.95 9 -2 4 49.14 5.31 -9 2 -4 49.93 5.01 -9 -2 -4 43.79 4.93 -9 2 -5 35.59 4.08 9 2 5 39.77 4.99 9 -2 5 34.08 4.30 -9 2 -5 35.16 4.07 9 -2 5 29.09 4.03 -9 -2 -5 31.40 4.00 -9 -2 -5 33.94 4.20 -9 2 -6 19.57 3.04 9 2 6 13.90 3.04 9 -2 6 16.16 3.13 -9 2 -6 15.78 2.63 9 -2 6 14.95 2.93 -9 -2 -6 16.07 2.73 -9 -2 -6 18.41 2.95 -9 2 -7 9.98 2.21 9 2 7 10.26 2.53 9 -2 7 12.01 2.77 -9 2 -7 7.00 1.88 9 -2 7 8.55 1.97 -9 -2 -7 11.15 2.31 -9 -2 -7 9.85 2.00 -9 2 -8 13.53 2.21 9 2 8 17.32 2.87 9 -2 8 16.58 2.82 -9 2 -8 17.41 2.38 9 -2 8 13.43 2.31 -9 -2 -8 12.75 2.15 -9 2 -9 8.17 1.76 9 2 9 8.86 2.06 9 -2 9 10.32 2.34 -9 2 -9 9.58 1.72 -9 -2 -9 7.85 1.63 -9 -3 9 9.51 1.67 9 3 -9 13.39 1.80 -9 -3 9 13.06 2.16 -9 -3 9 11.38 2.15 -9 3 9 12.29 1.86 -9 3 8 2.33 1.22 -9 -3 8 1.08 1.20 9 3 -8 3.80 1.24 -9 -3 8 -0.15 1.12 9 -3 -8 -0.73 1.41 -9 3 7 6.03 1.61 9 -3 -7 6.59 1.79 9 -3 -7 5.23 1.41 -9 -3 7 7.49 1.68 -9 -3 7 3.60 1.28 9 3 -7 8.17 1.69 9 -3 -7 9.01 1.89 -9 -3 7 8.90 2.21 9 -3 -7 3.91 1.53 9 -3 -6 39.81 3.76 9 -3 -6 41.26 3.33 -9 -3 6 45.09 3.81 -9 -3 6 38.52 3.77 9 3 -6 39.78 3.52 -9 -3 6 37.65 4.14 9 -3 -6 37.97 4.01 -9 3 6 36.12 3.66 -9 3 5 25.15 3.15 9 -3 -5 29.38 3.30 9 -3 -5 24.58 2.61 -9 -3 5 24.79 2.91 -9 -3 5 18.06 2.68 9 3 -5 23.00 2.76 -9 -3 5 24.91 3.55 9 -3 -5 22.68 3.25 -9 3 4 1.19 1.37 9 3 -4 0.55 1.80 9 -3 -4 1.93 1.52 9 -3 -4 -0.38 1.04 -9 -3 4 1.00 1.28 9 -3 -4 -0.11 1.38 9 3 -4 0.78 1.03 -9 -3 4 4.80 2.21 9 -3 -4 2.09 1.66 -9 3 3 9.22 2.04 9 3 -3 9.17 2.66 9 -3 -3 9.90 2.17 9 -3 -3 8.07 1.63 -9 -3 3 12.56 2.47 9 -3 -3 9.22 2.18 9 3 -3 11.65 2.22 -9 -3 3 10.82 2.05 9 -3 -3 11.60 2.69 -9 -3 3 9.35 2.51 -9 3 2 7.13 2.03 9 3 -2 7.44 2.64 9 -3 -2 9.37 2.19 -9 -3 2 6.64 1.94 9 -3 -2 7.99 2.06 9 3 -2 9.49 1.96 -9 -3 2 6.19 1.74 9 -3 -2 9.92 2.58 -9 -3 2 5.05 2.00 -9 3 1 6.27 1.88 9 3 -1 5.17 2.29 9 -3 -1 9.78 2.06 -9 -3 1 5.36 1.70 9 -3 -1 6.52 2.07 9 3 -1 7.12 1.82 -9 -3 1 6.96 1.95 9 -3 -1 8.37 2.16 -9 -3 1 8.84 2.37 -9 3 0 14.15 2.55 9 3 0 16.70 3.25 9 -3 0 18.37 2.77 -9 -3 0 15.69 2.59 9 -3 0 9.60 2.15 9 3 0 16.27 2.42 -9 -3 0 13.73 2.35 9 -3 0 16.93 3.07 -9 -3 0 10.88 2.62 -9 3 -1 15.35 2.55 9 3 1 12.48 2.97 -9 3 -1 14.38 2.42 -9 -3 -1 13.17 2.39 9 -3 1 9.75 2.13 9 3 1 13.20 2.14 -9 -3 -1 12.03 2.29 9 -3 1 6.26 1.84 -9 -3 -1 14.55 2.91 -9 3 -2 16.27 2.77 9 3 2 15.78 3.22 -9 3 -2 19.88 2.82 -9 -3 -2 21.36 2.70 9 -3 2 18.93 2.55 9 3 2 22.81 2.58 9 -3 2 22.16 3.43 -9 -3 -2 17.48 2.71 -9 -3 -2 23.96 3.52 -9 3 -3 27.42 3.36 9 3 3 26.45 3.67 -9 3 -3 30.10 3.29 -9 -3 -3 25.16 2.80 -9 -3 -3 35.35 3.58 9 3 3 29.64 2.84 9 -3 3 28.54 3.04 9 -3 3 29.21 3.63 -9 -3 -3 30.16 3.79 -9 3 -4 10.18 2.03 9 3 4 11.76 2.48 -9 -3 -4 7.71 1.70 9 -3 4 10.58 1.82 9 3 4 10.44 1.72 9 -3 4 5.06 1.86 -9 -3 -4 10.09 2.05 -9 -3 -4 5.41 1.67 -9 3 -5 7.26 1.83 9 3 5 9.44 2.14 9 -3 5 10.58 2.17 -9 -3 -5 8.59 1.82 -9 -3 -5 7.55 1.97 -9 3 -6 4.28 1.45 9 -3 6 9.78 1.98 -9 -3 -6 7.05 1.78 -9 -3 -6 8.17 1.86 -9 -3 -7 1.23 0.97 -10 0 11 1.12 1.23 10 0 -11 1.39 1.20 -10 0 10 4.87 1.76 10 0 -10 3.97 1.69 -10 0 9 2.05 1.50 10 0 -9 2.17 1.64 -10 0 8 14.93 2.74 10 0 -8 19.46 3.16 -10 0 7 44.40 4.50 10 0 -7 34.23 4.21 -10 0 6 202.35 10.85 10 0 -6 185.26 10.74 -10 0 5 -0.19 1.78 10 0 -5 -2.31 1.93 -10 0 4 7.44 2.42 10 0 -4 8.82 2.30 -10 0 3 676.12 26.17 10 0 -3 649.55 25.84 -10 0 2 163.47 9.53 10 0 -2 143.68 8.92 10 0 -1 -4.44 2.21 -10 0 1 -2.20 1.74 10 0 -1 1.04 1.54 10 0 0 2.36 1.78 -10 0 0 0.23 1.49 10 0 0 -0.39 1.24 10 0 1 2.36 1.89 -10 0 -1 4.93 1.82 10 0 2 28.07 4.09 -10 0 -2 29.27 3.49 10 0 3 1.04 1.96 -10 0 -3 1.11 1.11 10 0 4 12.52 2.94 -10 0 -4 9.36 1.97 10 0 5 0.66 1.64 -10 0 -5 1.35 1.24 -10 0 -5 0.86 1.14 10 0 6 51.86 5.29 -10 0 -6 63.28 4.85 10 0 7 45.53 4.66 -10 0 -7 51.57 4.17 10 0 8 1.20 1.50 -10 0 -8 1.16 1.09 -10 0 -8 1.51 1.20 -10 1 11 33.69 3.19 -10 1 10 21.56 2.74 10 -1 -10 20.05 2.73 10 1 -9 19.08 2.64 -10 1 9 20.50 2.85 -10 -1 9 17.72 2.45 10 1 -9 21.10 2.78 10 -1 -9 20.64 3.05 -10 -1 9 21.66 2.48 10 1 -8 6.32 1.96 -10 1 8 7.04 2.13 -10 -1 8 5.61 1.86 10 1 -8 1.93 1.32 10 -1 -8 4.34 1.83 -10 1 7 62.05 5.20 -10 -1 7 61.08 5.08 -10 -1 7 57.59 4.88 10 1 -7 63.83 5.02 10 -1 -7 65.00 5.65 -10 1 6 50.95 4.84 -10 -1 6 66.39 5.31 -10 -1 6 58.51 4.88 10 1 -6 49.43 4.44 10 -1 -6 52.65 5.21 -10 1 5 25.66 3.47 -10 -1 5 28.97 3.44 -10 -1 5 32.72 3.88 10 1 -5 26.23 3.17 10 -1 -5 31.03 4.02 10 1 -4 171.02 9.98 -10 1 4 148.36 8.85 -10 -1 4 168.26 9.54 -10 -1 4 142.20 8.39 10 -1 -4 156.88 9.71 10 1 -3 12.72 2.67 -10 1 3 11.90 2.43 -10 -1 3 14.52 2.81 10 -1 -3 7.39 2.33 10 1 -2 25.75 4.01 -10 1 2 25.62 3.13 -10 1 2 25.83 3.42 -10 -1 2 27.67 3.68 10 -1 -2 27.20 3.93 10 1 -1 4.39 2.16 -10 1 1 5.57 1.73 -10 1 1 5.15 1.76 -10 -1 1 2.09 1.65 10 -1 -1 3.63 1.69 -10 1 0 9.60 2.16 -10 1 0 12.66 2.41 -10 -1 0 11.75 2.33 10 -1 0 6.89 2.15 10 1 1 9.21 2.60 -10 1 -1 7.14 2.07 -10 1 -1 5.37 1.45 -10 -1 -1 9.59 2.20 10 -1 1 6.08 1.95 10 1 2 26.72 4.20 -10 1 -2 26.21 3.24 -10 -1 -2 22.62 3.20 10 -1 2 19.67 3.02 10 1 3 30.05 4.25 10 -1 3 31.79 3.96 -10 1 -3 26.05 3.31 -10 -1 -3 32.33 3.68 10 -1 3 26.31 3.25 10 1 4 36.20 4.65 10 -1 4 35.73 4.19 -10 1 -4 35.77 3.76 -10 -1 -4 36.61 3.75 10 1 5 57.34 5.60 10 -1 5 54.31 5.12 -10 1 -5 58.60 4.57 -10 -1 -5 59.45 4.50 10 1 6 49.10 4.89 10 -1 6 44.55 4.49 -10 1 -6 46.97 3.88 -10 -1 -6 50.51 3.89 10 1 7 18.07 2.88 10 -1 7 17.07 2.78 -10 1 -7 15.26 2.14 -10 2 8 13.22 2.02 -10 -2 8 20.20 2.58 10 -2 -8 19.36 2.63 -10 2 7 15.75 2.36 -10 -2 7 23.27 2.92 10 -2 -7 19.68 2.93 -10 2 6 13.19 2.15 -10 -2 6 16.27 2.45 -10 -2 6 14.89 2.23 10 -2 -6 12.52 2.53 10 2 -5 29.01 3.52 10 -2 -5 24.92 2.65 -10 2 5 28.41 3.01 -10 -2 5 28.95 3.38 -10 -2 5 30.80 3.18 10 -2 -5 29.69 3.70 -10 2 4 3.11 1.43 10 2 -4 0.96 1.51 10 -2 -4 2.53 1.10 -10 2 4 1.18 1.18 -10 -2 4 2.83 1.53 -10 -2 4 1.98 1.34 10 -2 -4 4.35 1.93 -10 2 3 13.26 2.04 10 2 -3 13.14 2.69 10 -2 -3 11.88 1.90 -10 -2 3 11.89 2.24 -10 -2 3 12.72 2.29 10 -2 -3 13.17 2.64 -10 2 2 22.25 2.67 10 2 -2 19.17 3.36 -10 2 2 18.70 2.38 -10 -2 2 15.36 2.26 -10 -2 2 14.77 2.39 -10 -2 2 13.84 2.35 10 -2 -2 19.80 3.15 10 2 -1 39.22 4.50 -10 2 1 36.15 3.35 -10 -2 1 34.76 3.30 -10 -2 1 33.12 3.41 -10 -2 1 32.49 3.57 10 -2 -1 35.54 4.11 -10 2 1 33.39 3.27 -10 2 0 18.90 2.51 10 2 0 22.13 3.44 -10 2 0 18.70 2.53 -10 -2 0 16.18 2.25 -10 -2 0 20.04 2.84 10 -2 0 21.49 3.21 -10 2 -1 4.87 1.50 10 2 1 2.66 1.58 -10 2 -1 5.06 1.42 -10 -2 -1 1.47 1.01 -10 -2 -1 5.26 1.75 10 -2 1 5.66 1.91 -10 -2 -1 2.97 1.60 -10 2 -2 6.81 1.70 10 2 2 5.65 2.23 -10 2 -2 5.73 1.62 -10 -2 -2 5.17 1.66 10 -2 2 7.65 1.94 -10 -2 -2 5.82 1.91 10 2 3 65.01 5.55 -10 2 -3 60.36 4.48 -10 -2 -3 71.45 4.98 10 -2 3 58.66 4.70 -10 2 -3 58.18 4.34 -10 -2 -3 57.05 4.70 10 2 4 47.01 4.51 -10 2 -4 39.27 3.51 -10 -2 -4 45.97 3.83 10 -2 4 43.69 3.80 -10 2 -4 38.86 3.42 10 2 5 40.61 4.00 -10 2 -5 43.10 3.47 -10 -2 -5 44.03 3.57 -11 0 6 20.25 2.51 -11 0 5 7.00 1.58 -11 0 4 36.52 3.34 -11 0 3 -0.21 1.02 -11 0 2 3.50 1.36 -11 0 1 25.62 2.82 -11 0 0 16.75 2.09 -11 0 0 11.03 1.90 -11 0 -1 5.27 1.33 -11 0 -2 59.77 3.98 -11 -1 4 131.83 6.86 -11 -1 3 0.33 1.01 -11 -1 2 2.91 1.36 -11 -1 1 11.23 1.86 -11 -1 0 12.49 2.01 0 0 0 0.00 0.00 TITL 20190219pengfei-whitebottle in P2(1)/m REM P2(1)/m (#11 in standard setting) CELL 1.54184 9.151567 5.267338 17.985994 90.0000 94.6833 90.0000 ZERR 4.00 0.000196 0.000135 0.000404 0.0000 0.0020 0.0000 LATT 1 SYMM -x, y+1/2,-z SFAC C H N O UNIT 44.00 40.00 4.00 4.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 93018 _olex2_date_sample_data_collection 2019-02-19 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.489 _oxdiff_exptl_absorpt_empirical_full_min 0.642 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn O001 O 0.48486(17) 0.3476(4) 0.90399(8) 0.0354(4) Uani 1 1 d . N002 N 0.12879(19) 0.4809(4) 0.75834(9) 0.0262(4) Uani 1 1 d . N003 N 0.35471(19) 0.2762(4) 0.79252(9) 0.0242(4) Uani 1 1 d . N004 N 0.33981(18) 0.0579(4) 0.65017(9) 0.0243(4) Uani 1 1 d . C005 C 0.2300(2) 0.3195(4) 0.74570(11) 0.0236(4) Uani 1 1 d . C006 C 0.3782(2) 0.4005(5) 0.86161(11) 0.0271(5) Uani 1 1 d . C007 C 0.2696(2) 0.5945(5) 0.87510(11) 0.0263(5) Uani 1 1 d . C008 C 0.1487(2) 0.6272(5) 0.82281(11) 0.0248(5) Uani 1 1 d . C009 C 0.2613(2) 0.0510(5) 0.51564(12) 0.0259(5) Uani 1 1 d . C00A C 0.4174(2) -0.0815(4) 0.71161(11) 0.0260(5) Uani 1 1 d . H00A H 0.4985 -0.1753 0.6935 0.031 Uiso 1 1 calc R H00B H 0.3515 -0.2017 0.7323 0.031 Uiso 1 1 calc R C00B C 0.3396(2) 0.2663(5) 0.49957(12) 0.0286(5) Uani 1 1 d . H00C H 0.4160 0.3206 0.5331 0.034 Uiso 1 1 calc R C00C C 0.4749(2) 0.1058(5) 0.77171(11) 0.0259(5) Uani 1 1 d . H00D H 0.5109 0.0091 0.8160 0.031 Uiso 1 1 calc R C00D C 0.0480(2) 0.8193(5) 0.83508(12) 0.0297(5) Uani 1 1 d . H00E H -0.0333 0.8435 0.8013 0.036 Uiso 1 1 calc R C00E C 0.3040(2) -0.1044(4) 0.58492(12) 0.0275(5) Uani 1 1 d . H00F H 0.2236 -0.2163 0.5948 0.033 Uiso 1 1 calc R H00G H 0.3882 -0.2091 0.5763 0.033 Uiso 1 1 calc R C00F C 0.2060(2) 0.1608(5) 0.67610(12) 0.0285(5) Uani 1 1 d . H00H H 0.1408 0.0214 0.6857 0.034 Uiso 1 1 calc R H00I H 0.1576 0.2640 0.6368 0.034 Uiso 1 1 calc R C00G C 0.2880(2) 0.7504(5) 0.93825(12) 0.0291(5) Uani 1 1 d . H00J H 0.3682 0.7255 0.9727 0.035 Uiso 1 1 calc R C00H C 0.3065(3) 0.4019(5) 0.43454(13) 0.0335(5) Uani 1 1 d . H00K H 0.3594 0.5473 0.4249 0.040 Uiso 1 1 calc R C00I C 0.1889(3) 0.9405(5) 0.95006(12) 0.0306(5) Uani 1 1 d . C00J C 0.6001(2) 0.2618(5) 0.74658(13) 0.0314(5) Uani 1 1 d . H00L H 0.5853 0.3505 0.7019 0.038 Uiso 1 1 calc R C00K C 0.0686(2) 0.9726(5) 0.89695(12) 0.0311(5) Uani 1 1 d . H00M H 0.0012 1.1010 0.9039 0.037 Uiso 1 1 calc R C00L C 0.1474(2) -0.0262(5) 0.46496(13) 0.0334(5) Uani 1 1 d . H00N H 0.0923 -0.1684 0.4752 0.040 Uiso 1 1 calc R C00M C 0.1154(3) 0.1076(6) 0.39900(13) 0.0385(6) Uani 1 1 d . H00O H 0.0401 0.0524 0.3650 0.046 Uiso 1 1 calc R C00N C 0.1939(3) 0.3202(6) 0.38380(13) 0.0366(6) Uani 1 1 d . H00P H 0.1719 0.4094 0.3397 0.044 Uiso 1 1 calc R C00O C 0.2074(3) 1.1097(6) 1.01750(13) 0.0412(6) Uani 1 1 d . H00Q H 0.1442 1.0524 1.0542 0.062 Uiso 1 1 calc GR H00R H 0.1822 1.2809 1.0033 0.062 Uiso 1 1 calc GR H00S H 0.3074 1.1039 1.0381 0.062 Uiso 1 1 calc GR C00P C 0.7286(3) 0.2794(7) 0.78425(18) 0.0494(8) Uani 1 1 d . H00T H 0.807(4) 0.375(7) 0.7633(18) 0.058(10) Uiso 1 1 d . H00U H 0.747(4) 0.203(8) 0.833(2) 0.067(11) Uiso 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 O001 0.0309(8) 0.0453(11) 0.0285(8) -0.0039(7) -0.0068(6) 0.0097(7) N002 0.0229(8) 0.0320(11) 0.0235(8) 0.0013(8) 0.0009(6) 0.0011(8) N003 0.0239(8) 0.0263(11) 0.0222(8) 0.0013(8) 0.0013(6) 0.0016(8) N004 0.0260(8) 0.0234(10) 0.0231(8) -0.0010(7) 0.0003(6) 0.0008(7) C005 0.0214(9) 0.0263(12) 0.0231(9) 0.0017(9) 0.0013(7) -0.0014(9) C006 0.0271(10) 0.0321(14) 0.0217(10) 0.0007(9) 0.0004(8) -0.0005(9) C007 0.0264(10) 0.0297(13) 0.0234(9) 0.0044(9) 0.0052(8) -0.0013(9) C008 0.0237(10) 0.0282(13) 0.0231(10) 0.0017(9) 0.0046(7) -0.0004(9) C009 0.0255(10) 0.0269(13) 0.0255(10) -0.0038(9) 0.0044(8) 0.0020(9) C00A 0.0283(10) 0.0222(12) 0.0274(11) 0.0015(9) 0.0015(8) 0.0010(9) C00B 0.0261(10) 0.0278(13) 0.0314(11) -0.0040(9) -0.0004(8) -0.0017(9) C00C 0.0254(10) 0.0263(13) 0.0256(10) 0.0006(9) -0.0001(8) 0.0046(9) C00D 0.0255(10) 0.0364(14) 0.0274(10) 0.0017(10) 0.0027(8) 0.0033(9) C00E 0.0300(10) 0.0240(13) 0.0285(10) -0.0027(9) 0.0024(8) -0.0005(9) C00F 0.0241(10) 0.0357(14) 0.0253(10) -0.0026(9) -0.0001(8) 0.0002(9) C00G 0.0296(11) 0.0350(14) 0.0228(10) 0.0015(9) 0.0028(8) 0.0016(10) C00H 0.0332(11) 0.0326(14) 0.0348(12) 0.0027(10) 0.0037(9) -0.0029(10) C00I 0.0359(11) 0.0317(14) 0.0253(10) 0.0004(10) 0.0087(9) -0.0001(10) C00J 0.0278(11) 0.0304(14) 0.0366(12) -0.0079(10) 0.0062(9) 0.0011(9) C00K 0.0300(11) 0.0320(14) 0.0324(11) 0.0021(10) 0.0094(9) 0.0074(10) C00L 0.0309(11) 0.0374(15) 0.0318(11) -0.0039(10) 0.0018(9) -0.0067(10) C00M 0.0315(11) 0.0523(18) 0.0303(11) -0.0017(11) -0.0051(9) -0.0058(11) C00N 0.0357(12) 0.0451(16) 0.0287(11) 0.0044(11) 0.0003(9) 0.0011(11) C00O 0.0491(14) 0.0417(17) 0.0330(12) -0.0074(12) 0.0048(10) 0.0103(13) C00P 0.0277(12) 0.064(2) 0.0562(17) -0.0169(16) 0.0031(11) -0.0039(13) 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C005 N002 C008 117.66(17) C005 N003 C006 121.40(18) C005 N003 C00C 122.44(17) C006 N003 C00C 116.10(16) C00A N004 C00E 112.02(18) C00F N004 C00A 108.40(16) C00F N004 C00E 109.59(16) N002 C005 N003 124.79(19) N002 C005 C00F 116.98(17) N003 C005 C00F 118.18(18) O001 C006 N003 120.1(2) O001 C006 C007 125.2(2) N003 C006 C007 114.61(18) C008 C007 C006 119.00(19) C00G C007 C006 120.46(19) C00G C007 C008 120.5(2) N002 C008 C007 122.2(2) N002 C008 C00D 119.26(19) C00D C008 C007 118.5(2) C00B C009 C00E 120.72(19) C00B C009 C00L 118.5(2) C00L C009 C00E 120.7(2) N004 C00A H00A 109.8 N004 C00A H00B 109.8 N004 C00A C00C 109.22(18) H00A C00A H00B 108.3 C00C C00A H00A 109.8 C00C C00A H00B 109.8 C009 C00B H00C 119.4 C00H C00B C009 121.2(2) C00H C00B H00C 119.4 N003 C00C C00A 110.39(16) N003 C00C H00D 108.3 N003 C00C C00J 109.95(19) C00A C00C H00D 108.3 C00J C00C C00A 111.49(17) C00J C00C H00D 108.3 C008 C00D H00E 119.9 C00K C00D C008 120.2(2) C00K C00D H00E 119.9 N004 C00E C009 111.62(18) N004 C00E H00F 109.3 N004 C00E H00G 109.3 C009 C00E H00F 109.3 C009 C00E H00G 109.3 H00F C00E H00G 108.0 N004 C00F C005 113.86(17) N004 C00F H00H 108.8 N004 C00F H00I 108.8 C005 C00F H00H 108.8 C005 C00F H00I 108.8 H00H C00F H00I 107.7 C007 C00G H00J 119.5 C00I C00G C007 120.9(2) C00I C00G H00J 119.5 C00B C00H H00K 120.1 C00B C00H C00N 119.7(2) C00N C00H H00K 120.1 C00G C00I C00K 118.1(2) C00G C00I C00O 121.5(2) C00K C00I C00O 120.4(2) C00C C00J H00L 118.2 C00P C00J C00C 123.7(3) C00P C00J H00L 118.2 C00D C00K C00I 121.8(2) C00D C00K H00M 119.1 C00I C00K H00M 119.1 C009 C00L H00N 119.8 C009 C00L C00M 120.4(2) C00M C00L H00N 119.8 C00L C00M H00O 119.8 C00N C00M C00L 120.5(2) C00N C00M H00O 119.8 C00H C00N H00P 120.1 C00M C00N C00H 119.7(2) C00M C00N H00P 120.1 C00I C00O H00Q 109.5 C00I C00O H00R 109.5 C00I C00O H00S 109.5 H00Q C00O H00R 109.5 H00Q C00O H00S 109.5 H00R C00O H00S 109.5 C00J C00P H00T 120(2) C00J C00P H00U 122(2) H00T C00P H00U 119(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O001 C006 1.221(3) N002 C005 1.291(3) N002 C008 1.392(3) N003 C005 1.381(2) N003 C006 1.406(3) N003 C00C 1.491(3) N004 C00A 1.462(3) N004 C00E 1.468(3) N004 C00F 1.451(3) C005 C00F 1.506(3) C006 C007 1.459(3) C007 C008 1.403(3) C007 C00G 1.401(3) C008 C00D 1.399(3) C009 C00B 1.385(3) C009 C00E 1.515(3) C009 C00L 1.388(3) C00A H00A 0.9700 C00A H00B 0.9700 C00A C00C 1.525(3) C00B H00C 0.9300 C00B C00H 1.383(3) C00C H00D 0.9800 C00C C00J 1.509(3) C00D H00E 0.9300 C00D C00K 1.375(3) C00E H00F 0.9700 C00E H00G 0.9700 C00F H00H 0.9700 C00F H00I 0.9700 C00G H00J 0.9300 C00G C00I 1.379(3) C00H H00K 0.9300 C00H C00N 1.388(3) C00I C00K 1.408(3) C00I C00O 1.504(3) C00J H00L 0.9300 C00J C00P 1.312(4) C00K H00M 0.9300 C00L H00N 0.9300 C00L C00M 1.390(4) C00M H00O 0.9300 C00M C00N 1.371(4) C00N H00P 0.9300 C00O H00Q 0.9600 C00O H00R 0.9600 C00O H00S 0.9600 C00P H00T 0.98(4) C00P H00U 0.97(4) 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 O001 C006 C007 C008 -177.2(2) O001 C006 C007 C00G 4.6(4) N002 C005 C00F N004 158.0(2) N002 C008 C00D C00K -177.5(2) N003 C005 C00F N004 -24.4(3) N003 C006 C007 C008 4.7(3) N003 C006 C007 C00G -173.50(19) N003 C00C C00J C00P 111.6(3) N004 C00A C00C N003 51.6(2) N004 C00A C00C C00J -71.0(2) C005 N002 C008 C007 -3.4(3) C005 N002 C008 C00D 174.4(2) C005 N003 C006 O001 175.5(2) C005 N003 C006 C007 -6.3(3) C005 N003 C00C C00A -22.2(3) C005 N003 C00C C00J 101.2(2) C006 N003 C005 N002 3.2(3) C006 N003 C005 C00F -174.24(19) C006 N003 C00C C00A 160.56(18) C006 N003 C00C C00J -76.0(2) C006 C007 C008 N002 -0.1(3) C006 C007 C008 C00D -177.9(2) C006 C007 C00G C00I 177.6(2) C007 C008 C00D C00K 0.4(3) C007 C00G C00I C00K 0.2(3) C007 C00G C00I C00O -179.9(2) C008 N002 C005 N003 1.9(3) C008 N002 C005 C00F 179.37(19) C008 C007 C00G C00I -0.6(3) C008 C00D C00K C00I -0.9(4) C009 C00B C00H C00N -0.8(4) C009 C00L C00M C00N -1.2(4) C00A N004 C00E C009 -164.80(17) C00A N004 C00F C005 54.3(3) C00A C00C C00J C00P -125.7(3) C00B C009 C00E N004 43.0(3) C00B C009 C00L C00M 1.2(3) C00B C00H C00N C00M 0.8(4) C00C N003 C005 N002 -173.9(2) C00C N003 C005 C00F 8.7(3) C00C N003 C006 O001 -7.2(3) C00C N003 C006 C007 170.97(18) C00E N004 C00A C00C 170.01(17) C00E N004 C00F C005 176.86(18) C00E C009 C00B C00H 176.5(2) C00E C009 C00L C00M -175.5(2) C00F N004 C00A C00C -68.9(2) C00F N004 C00E C009 74.8(2) C00G C007 C008 N002 178.1(2) C00G C007 C008 C00D 0.3(3) C00G C00I C00K C00D 0.6(3) C00L C009 C00B C00H -0.2(3) C00L C009 C00E N004 -140.3(2) C00L C00M C00N C00H 0.2(4) C00O C00I C00K C00D -179.4(2)