#------------------------------------------------------------------------------ #$Date: 2016-01-01 03:00:30 +0200 (Fri, 01 Jan 2016) $ #$Revision: 171814 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/07/1540735.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_1540735 loop_ _publ_author_name 'Piechowicz, Marek' 'Abney, Carter W.' 'Zhou, Xin' 'Thacker, Nathan C.' 'Li, Zhong' 'Lin, Wenbin' _publ_section_title ; Design, Synthesis, and Characterization of a Bifunctional Chelator with Ultrahigh Capacity for Uranium Uptake from Seawater Simulant ; _journal_name_full 'Industrial & Engineering Chemistry Research' _journal_paper_doi 10.1021/acs.iecr.5b03304 _journal_year 2015 _chemical_formula_moiety 'C14 H12 N2 O4' _chemical_formula_sum 'C14 H12 N2 O4' _chemical_formula_weight 272.26 _space_group_crystal_system orthorhombic _space_group_IT_number 33 _space_group_name_Hall 'P 2c -2n' _space_group_name_H-M_alt 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' _symmetry_space_group_name_H-M 'P n a 21' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _audit_creation_date 2015-08-30 _audit_creation_method ; Olex2 1.2 (compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.2721(15) _cell_length_b 12.9900(19) _cell_length_c 9.3830(14) _cell_measurement_reflns_used 3181 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 17.74 _cell_measurement_theta_min 2.31 _cell_volume 1252.0(3) _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2008)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 296.15 _diffrn_measured_fraction_theta_full 0.955 _diffrn_measured_fraction_theta_max 0.955 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_wavelength 0.41328 _diffrn_reflns_av_R_equivalents 0.1171 _diffrn_reflns_av_unetI/netI 0.1280 _diffrn_reflns_laue_measured_fraction_full 0.955 _diffrn_reflns_laue_measured_fraction_max 0.955 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 19889 _diffrn_reflns_point_group_measured_fraction_full 0.930 _diffrn_reflns_point_group_measured_fraction_max 0.930 _diffrn_reflns_theta_full 18.419 _diffrn_reflns_theta_max 18.419 _diffrn_reflns_theta_min 1.470 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.014 _exptl_absorpt_correction_type none _exptl_crystal_density_diffrn 1.444 _exptl_crystal_F_000 568 _refine_diff_density_max 0.352 _refine_diff_density_min -0.365 _refine_diff_density_rms 0.072 _refine_ls_abs_structure_details ; Flack x determined using 1003 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.7(7) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 186 _refine_ls_number_reflns 4369 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.015 _refine_ls_R_factor_all 0.1045 _refine_ls_R_factor_gt 0.0602 _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^)+(0.0510P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1260 _refine_ls_wR_factor_ref 0.1437 _reflns_Friedel_coverage 0.851 _reflns_friedel_fraction_full 0.902 _reflns_friedel_fraction_max 0.902 _reflns_number_gt 3000 _reflns_number_total 4369 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ie5b03304_si_001.cif _cod_data_source_block bfc_paper3 _cod_database_code 1540735 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All N(H,H) groups At 1.5 times of: All O(H) groups 2.a Aromatic/amide H refined with riding coordinates: C5(H5), C6(H6), C9(H9), C4(H4A), C12(H12), C11(H11), C3(H3), C10(H10) 2.b X=CH2 refined with riding coordinates: N1(H1A,H1B) 2.c Idealised tetrahedral OH refined as rotating group: O4(H4) ; _shelx_res_file ; bfc_paper3.res created by SHELXL-2014/7 TITL bfc_paper3_a.res in Pna2(1) REM Old TITL BFC_paper3 in Pna21 #33 REM SHELXT solution in Pna2(1) REM R1 0.096, Rweak 0.011, Alpha 0.002, Orientation as input REM Flack x = 0.312 ( 1.083 ) from Parsons' quotients REM Formula found by SHELXT: C14 N O5 CELL 0.41328 10.2721 12.99 9.383 90 90 90 ZERR 4 0.0015 0.0019 0.0014 0 0 0 LATT -1 SYMM -X,-Y,0.5+Z SYMM 0.5+X,0.5-Y,+Z SYMM 0.5-X,0.5+Y,0.5+Z SFAC C H N O DISP C -0 0.005 1.09 DISP N 0.005 0.001 2.27 DISP O 0.002 0.002 4.23 UNIT 56 48 8 16 L.S. 10 PLAN 25 TEMP 23 BOND $H LIST 6 MORE -1 CONF fmap 2 acta 52 OMIT 0 3 -1 OMIT 1 2 -2 OMIT 1 2 2 REM REM REM WGHT 0.051000 FVAR 0.72681 O1 4 0.652524 0.411304 0.530637 11.00000 0.01891 0.01342 = 0.01387 0.00084 -0.00294 -0.00073 O3 4 0.846790 0.388887 0.135111 11.00000 0.03141 0.02215 = 0.01144 -0.00066 0.00282 -0.00199 N1 3 0.877612 0.484169 0.864534 11.00000 0.02976 0.01567 = 0.01284 0.00013 -0.00445 -0.00532 AFIX 93 H1A 2 0.915249 0.542885 0.874287 11.00000 -1.20000 H1B 2 0.860757 0.447207 0.938302 11.00000 -1.20000 AFIX 0 O4 4 0.905252 0.608547 0.637777 11.00000 0.02772 0.02007 = 0.02846 0.00201 -0.00226 -0.00517 AFIX 147 H4 2 0.984816 0.613544 0.639362 11.00000 -1.50000 AFIX 0 O2 4 0.870114 0.407169 0.368919 11.00000 0.02294 0.03343 = 0.01223 -0.00454 0.00088 -0.00781 N2 3 0.870720 0.506076 0.623523 11.00000 0.02486 0.01400 = 0.01415 -0.00067 -0.00123 -0.00542 C1 1 0.845797 0.450865 0.736675 11.00000 0.01711 0.01523 = 0.01374 0.00018 -0.00134 0.00009 C2 1 0.784093 0.348684 0.718651 11.00000 0.02232 0.01274 = 0.01100 0.00140 -0.00025 -0.00104 C7 1 0.690432 0.328703 0.612631 11.00000 0.01820 0.01489 = 0.01307 0.00126 0.00248 -0.00062 C8 1 0.587226 0.389190 0.403556 11.00000 0.02192 0.01200 = 0.01481 -0.00048 -0.00486 -0.00231 C5 1 0.676463 0.153215 0.688854 11.00000 0.03197 0.01511 = 0.02295 0.00043 -0.00063 -0.00492 AFIX 43 H5 2 0.640792 0.087810 0.678855 11.00000 -1.20000 AFIX 0 C6 1 0.637795 0.231480 0.598741 11.00000 0.02102 0.01768 = 0.01876 -0.00043 -0.00171 -0.00365 AFIX 43 H6 2 0.576069 0.218634 0.528447 11.00000 -1.20000 AFIX 0 C9 1 0.452119 0.380043 0.410387 11.00000 0.01848 0.02043 = 0.02603 -0.00047 -0.00383 0.00086 AFIX 43 H9 2 0.409145 0.387099 0.497077 11.00000 -1.20000 AFIX 0 C4 1 0.768361 0.171684 0.794347 11.00000 0.04456 0.01352 = 0.02224 0.00545 -0.00786 -0.00081 AFIX 43 H4A 2 0.793614 0.118926 0.855379 11.00000 -1.20000 AFIX 0 C12 1 0.580862 0.363570 0.152261 11.00000 0.03067 0.01811 = 0.01752 -0.00100 -0.00519 -0.00182 AFIX 43 H12 2 0.622472 0.358873 0.064474 11.00000 -1.20000 AFIX 0 C11 1 0.447559 0.352304 0.158828 11.00000 0.03138 0.02088 = 0.02565 -0.00142 -0.01533 0.00013 AFIX 43 H11 2 0.400862 0.339108 0.075902 11.00000 -1.20000 AFIX 0 C3 1 0.821801 0.267937 0.808316 11.00000 0.03161 0.01986 = 0.01673 0.00251 -0.00644 -0.00252 AFIX 43 H3 2 0.884033 0.279703 0.878438 11.00000 -1.20000 AFIX 0 C14 1 0.800282 0.393144 0.260106 11.00000 0.02626 0.01411 = 0.01423 -0.00115 0.00048 -0.00345 C13 1 0.654610 0.381840 0.274294 11.00000 0.02309 0.01184 = 0.01506 -0.00005 -0.00246 -0.00163 C10 1 0.382590 0.360398 0.287202 11.00000 0.02184 0.02038 = 0.03371 -0.00269 -0.00899 0.00060 AFIX 43 H10 2 0.292640 0.352682 0.290757 11.00000 -1.20000 AFIX 0 H2 2 0.857421 0.483593 0.537595 11.00000 0.02280 HKLF 4 REM bfc_paper3_a.res in Pna2(1) REM R1 = 0.0602 for 3000 Fo > 4sig(Fo) and 0.1045 for all 4369 data REM 186 parameters refined using 1 restraints END WGHT 0.0506 0.0000 REM Highest difference peak 0.352, deepest hole -0.365, 1-sigma level 0.072 Q1 1 0.9203 0.5877 0.8591 11.00000 0.05 0.35 Q2 1 0.7256 0.3814 0.2421 11.00000 0.05 0.35 Q3 1 1.0265 0.6027 0.5319 11.00000 0.05 0.30 Q4 1 1.0691 0.6152 0.6433 11.00000 0.05 0.28 Q5 1 0.5195 0.3529 0.1633 11.00000 0.05 0.28 Q6 1 0.6026 0.3830 0.2276 11.00000 0.05 0.27 Q7 1 0.2376 0.4000 0.2582 11.00000 0.05 0.27 Q8 1 0.5164 0.3857 0.3916 11.00000 0.05 0.27 Q9 1 0.5597 0.4263 0.6538 11.00000 0.05 0.26 Q10 1 0.7140 0.4982 0.9571 11.00000 0.05 0.25 Q11 1 0.9810 0.6511 0.8545 11.00000 0.05 0.24 Q12 1 0.6002 0.4970 0.1703 11.00000 0.05 0.24 Q13 1 0.4453 0.3890 0.6648 11.00000 0.05 0.24 Q14 1 0.4792 0.2595 0.6734 11.00000 0.05 0.24 Q15 1 0.7310 0.1703 0.7364 11.00000 0.05 0.23 Q16 1 0.4996 0.3213 0.6572 11.00000 0.05 0.23 Q17 1 0.4552 0.3865 0.5987 11.00000 0.05 0.23 Q18 1 1.0014 0.4371 0.9339 11.00000 0.05 0.23 Q19 1 0.8240 0.0691 0.8816 11.00000 0.05 0.23 Q20 1 0.2183 0.3318 0.2516 11.00000 0.05 0.23 Q21 1 0.2988 0.3750 0.2392 11.00000 0.05 0.22 Q22 1 0.5388 0.4763 0.4010 11.00000 0.05 0.22 Q23 1 0.5201 0.2761 0.7252 11.00000 0.05 0.22 Q24 1 0.5310 0.4578 0.2089 11.00000 0.05 0.22 Q25 1 0.2981 0.4443 0.2156 11.00000 0.05 0.22 ; _shelx_res_checksum 12390 _shelx_hkl_file ; 0 0 1 6.00 4.30 0 0 1 0.90 2.80 0 0 1 -2.50 3.50 0 0 1 0.10 1.40 0 0 -1 -3.40 4.60 0 0 -1 -1.30 3.30 0 0 -1 2.60 3.80 0 0 -1 1.20 1.40 0 0 -3 -3.80 3.30 0 0 3 -1.80 3.10 0 0 3 5.90 9.70 0 0 -3 18.30 8.80 0 0 3 14.30 8.10 0 0 -3 -7.30 7.40 0 0 3 -3.30 6.10 0 0 -3 -4.50 11.30 0 0 4 2686.33 466.55 0 0 -4 3239.48 466.25 0 0 -4 3033.20 466.25 0 0 4 3213.18 466.25 0 0 -5 2.40 3.60 0 0 -5 -10.40 10.10 0 0 5 2.60 8.40 0 0 -5 -10.80 8.00 0 0 5 -4.30 10.80 0 0 5 1.20 3.30 0 0 -5 1.60 7.80 0 0 5 3.10 7.10 0 0 -6 243.68 36.00 0 0 6 133.89 36.00 0 0 -6 211.48 32.90 0 0 6 207.48 32.70 0 0 -6 283.47 37.60 0 0 6 205.48 35.30 0 0 6 207.68 35.80 0 0 -6 200.78 35.00 0 0 -7 0.70 10.20 0 0 -7 -0.70 9.30 0 0 -7 -1.50 4.00 0 0 -7 -10.30 8.40 0 0 7 2.30 9.80 0 0 7 2.50 3.90 0 0 -8 1518.35 216.08 0 0 -8 1482.35 215.78 0 0 -8 1293.07 214.08 0 0 8 1391.06 214.08 0 0 8 1358.66 215.88 0 0 -9 6.10 12.00 0 0 -9 3.30 4.60 0 0 -9 -9.90 8.60 0 0 9 16.40 13.30 0 0 9 0.50 4.50 0 0 -9 7.90 11.80 0 0 10 69.29 19.90 0 0 10 36.60 9.40 0 0 -10 48.60 16.50 0 0 -10 76.59 17.50 0 0 11 17.50 6.20 0 0 -11 2.20 15.50 0 0 -11 2.80 15.30 0 0 -12 138.69 35.40 0 0 12 214.28 32.20 0 0 -12 237.28 37.30 0 0 -13 -6.00 16.00 0 0 -13 -12.80 13.10 0 0 -14 7.00 15.70 1 0 0 -1.90 2.80 1 0 0 -10.60 7.30 1 0 0 -4.40 1.90 -1 0 0 -2.30 1.50 -1 0 0 -3.20 1.30 -1 0 0 -1.40 3.00 1 0 0 -3.70 1.30 -1 0 0 4.80 8.50 1 0 -1 -9.30 3.00 -1 0 1 -4.00 3.20 -1 0 -1 1.50 3.10 1 0 1 -1.50 6.20 1 0 1 4.80 3.50 1 0 1 -5.60 2.80 -1 0 -1 -7.80 6.20 -1 0 1 -7.30 2.90 -1 0 -1 -3.30 2.60 1 0 -1 0.80 3.70 1 0 -1 -4.30 1.20 -1 0 1 -4.80 1.10 -1 0 -2 -4.30 3.80 -1 0 -2 -5.30 5.50 -1 0 2 -5.10 4.70 1 0 2 1.10 7.80 -1 0 2 -5.40 2.20 1 0 -2 -6.60 5.90 1 0 -2 -3.30 2.30 1 0 -2 -8.50 5.30 -1 0 2 -10.90 4.70 1 0 2 1.30 4.20 -1 0 -2 -5.60 8.30 1 0 -2 4.60 6.10 -1 0 2 0.40 5.90 1 0 3 -11.30 8.20 -1 0 3 3.80 2.80 1 0 -3 1.10 6.50 -1 0 3 5.50 6.50 1 0 3 4.50 3.40 -1 0 -3 -21.40 12.10 -1 0 3 -4.10 6.80 1 0 -3 -3.80 6.80 -1 0 -3 -2.10 4.50 1 0 -3 -7.30 7.10 -1 0 -3 4.90 7.80 1 0 -3 -2.10 2.80 -1 0 3 3.40 6.80 1 0 3 0.40 7.20 1 0 4 11.30 4.00 -1 0 4 5.10 3.20 -1 0 4 5.80 8.80 1 0 -4 -7.80 7.70 -1 0 4 4.30 8.30 1 0 4 7.20 9.20 1 0 -4 -3.60 6.30 1 0 4 0.30 8.50 -1 0 -4 -8.10 8.50 -1 0 4 -4.30 6.70 1 0 -4 4.90 3.30 -1 0 -4 6.80 5.10 1 0 -4 2.20 7.40 -1 0 -4 -2.90 12.70 -1 0 5 -1.00 7.50 -1 0 5 -4.10 8.80 -1 0 -5 0.40 4.70 1 0 5 -25.00 11.70 1 0 -5 -7.00 7.00 1 0 -5 10.60 8.10 1 0 5 4.70 10.60 -1 0 5 11.70 10.80 1 0 5 -6.80 8.10 -1 0 -5 -9.60 11.70 1 0 5 2.20 4.00 -1 0 -5 3.60 7.40 -1 0 5 -4.30 3.20 1 0 -5 -1.60 3.50 1 0 -5 -6.70 7.30 -1 0 -6 15.30 8.40 -1 0 6 1.40 9.40 1 0 -6 0.10 8.00 -1 0 -6 -10.00 4.50 -1 0 6 -2.50 8.10 1 0 6 -4.90 8.60 1 0 -6 -0.20 8.70 1 0 6 6.70 4.30 1 0 -6 13.10 8.60 -1 0 -6 -6.40 12.60 -1 0 6 -3.10 10.80 -1 0 6 -4.00 3.50 1 0 -6 -0.40 3.70 1 0 6 -0.10 10.70 1 0 6 10.50 13.10 1 0 7 -10.60 11.00 -1 0 -7 8.60 5.40 1 0 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0 -14 -10.70 13.80 -1 0 -14 -24.20 16.20 2 0 0 1950.10 313.37 -2 0 0 2105.09 313.47 -2 0 -1 1334.27 189.98 -2 0 1 1222.38 188.48 -2 0 -1 1133.89 188.38 -2 0 1 1296.17 188.48 2 0 1 1168.58 189.68 2 0 1 1215.08 188.48 2 0 -1 1189.48 188.48 -2 0 -1 1207.48 188.48 2 0 -1 1314.77 188.48 2 0 1 1255.87 188.48 -2 0 -2 1980.60 301.77 2 0 -2 1964.00 301.07 2 0 -2 2027.50 301.07 -2 0 -2 2118.89 301.17 -2 0 2 1929.71 301.17 -2 0 -2 1993.20 300.97 2 0 2 1809.32 301.17 2 0 2 2096.69 300.97 2 0 2 1765.62 301.67 2 0 3 337.57 62.09 2 0 -3 439.16 61.19 -2 0 3 405.86 61.09 2 0 -3 384.76 59.99 2 0 -3 425.46 60.89 2 0 3 405.96 61.69 -2 0 3 371.46 61.29 -2 0 -3 439.26 60.59 2 0 -3 388.96 61.19 2 0 3 392.76 60.59 -2 0 -3 341.87 60.79 -2 0 -3 473.75 62.69 -2 0 3 375.86 59.89 -2 0 3 329.97 60.79 -2 0 4 1734.73 259.77 -2 0 4 1785.22 259.67 -2 0 -4 1872.91 259.37 -2 0 -4 1739.13 260.17 2 0 -4 1928.31 259.57 2 0 -4 1684.23 259.77 2 0 -4 1651.23 259.77 2 0 4 1514.25 259.97 -2 0 4 1566.04 259.77 -2 0 4 1725.33 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24.50 20.30 7 -15 4 10.40 11.10 -7 -15 4 28.80 20.60 7 -15 -4 14.10 5.30 -7 -15 -5 11.40 19.70 7 -15 5 8.20 14.30 -7 -15 5 16.00 21.50 7 -15 -5 28.40 5.90 -8 -15 0 88.59 32.30 8 -15 0 115.79 19.70 8 -15 1 17.10 8.90 -8 -15 -1 33.30 27.00 8 -15 -1 0.80 6.50 -8 -15 1 -15.00 22.90 8 -15 2 28.30 10.60 -8 -15 -2 49.70 27.70 -8 -15 2 14.50 23.10 8 -15 -2 19.00 7.10 -8 -15 -3 -30.50 22.50 8 -15 -3 14.10 5.80 -8 -15 3 7.00 22.20 -8 -15 4 -33.80 21.10 8 -15 -4 26.30 6.50 -9 -15 0 -4.80 26.20 9 -15 0 3.60 7.40 9 -15 1 51.99 14.00 -9 -15 -1 108.99 42.30 9 -15 -1 61.49 11.80 -9 -15 1 36.00 27.70 9 -15 -2 4.30 6.70 0 -16 2 -5.50 9.00 0 -16 -7 6.00 7.40 0 -16 7 20.80 11.40 -1 -16 1 41.70 16.60 -1 -16 1 50.79 11.40 1 -16 2 42.60 12.30 -1 -16 2 16.80 14.00 1 -16 5 102.39 19.30 -1 -16 -6 76.19 13.70 1 -16 6 60.89 16.00 1 -16 7 28.50 12.70 -1 -16 -7 29.50 9.70 1 -16 -7 16.70 6.70 -2 -16 0 35.80 15.20 -2 -16 0 58.59 11.20 -2 -16 1 101.49 18.00 -2 -16 1 82.29 23.60 2 -16 2 -2.90 12.70 -2 -16 2 -3.70 14.30 2 -16 4 7.00 8.20 2 -16 5 4.50 9.10 -2 -16 -5 -2.90 7.70 2 -16 6 14.00 10.30 -2 -16 -6 19.50 9.90 -2 -16 -7 8.10 10.70 2 -16 -7 4.30 5.00 -3 -16 0 16.10 16.00 -3 -16 -1 -2.80 5.90 -3 -16 -1 -8.40 12.10 -3 -16 1 -1.20 19.00 -3 -16 -2 54.69 10.60 3 -16 2 54.29 10.30 -3 -16 -2 58.09 13.70 3 -16 2 29.20 16.60 -3 -16 2 43.70 20.20 3 -16 3 4.40 6.90 -3 -16 -3 -7.00 9.30 -3 -16 3 16.50 16.30 3 -16 4 44.70 12.00 -3 -16 -4 53.29 12.80 -3 -16 -5 31.10 10.70 3 -16 5 19.30 10.50 3 -16 6 -4.80 10.10 -3 -16 -6 6.50 9.80 -3 -16 -7 -6.10 11.70 3 -16 -7 11.80 4.80 -4 -16 0 -6.60 17.80 -4 -16 -1 15.50 15.80 -4 -16 1 -5.10 18.90 -4 -16 -2 73.59 16.80 4 -16 2 58.19 11.20 -4 -16 2 4.00 20.00 4 -16 3 7.50 7.80 -4 -16 -3 11.70 12.70 -4 -16 3 -21.30 15.70 4 -16 4 11.20 9.50 -4 -16 -4 18.10 12.40 -4 -16 -5 16.80 13.10 4 -16 5 24.40 11.40 -4 -16 -6 32.30 14.10 4 -16 6 39.10 13.50 4 -16 -7 -6.90 4.00 -5 -16 0 67.69 24.70 5 -16 1 0.50 17.10 5 -16 1 5.10 5.90 -5 -16 -1 -16.50 18.60 -5 -16 1 5.00 21.50 5 -16 2 106.19 17.50 -5 -16 -2 122.89 24.90 -5 -16 2 20.10 25.50 5 -16 3 4.50 8.20 -5 -16 -3 14.90 14.30 -5 -16 3 29.10 19.10 5 -16 4 10.40 9.20 -5 -16 -4 33.10 14.40 -5 -16 4 4.50 17.60 -5 -16 -5 28.40 15.00 5 -16 5 19.40 11.00 6 -16 0 19.20 7.70 -6 -16 0 6.10 22.70 6 -16 1 25.00 9.80 -6 -16 -1 26.30 22.80 -6 -16 1 9.00 21.80 6 -16 2 9.50 9.70 -6 -16 -2 16.80 20.30 -6 -16 2 24.00 20.60 -6 -16 -3 21.40 17.80 6 -16 3 28.40 12.00 -6 -16 3 17.70 20.80 -6 -16 -4 -2.40 16.50 6 -16 4 -7.50 10.90 6 -16 -4 5.80 3.90 -6 -16 4 -34.60 17.00 6 -16 -5 4.30 3.90 -7 -16 0 89.99 29.60 -7 -16 -1 126.49 35.30 -7 -16 1 117.19 35.00 7 -16 -1 154.68 25.20 7 -16 2 91.39 17.60 -7 -16 -2 91.19 28.40 -7 -16 2 53.79 27.10 7 -16 -2 92.09 15.40 7 -16 3 21.50 11.90 -7 -16 -3 42.80 20.90 7 -16 -3 34.70 7.50 -7 -16 3 7.70 22.40 7 -16 -4 23.50 6.10 7 -16 -5 39.50 7.90 8 -16 0 6.70 8.40 8 -16 -1 45.80 10.30 8 -16 -2 33.60 8.50 8 -16 -3 8.10 5.90 0 -17 2 12.80 11.20 0 -17 2 -0.10 11.20 0 -17 -7 1.70 6.30 -1 -17 2 84.59 20.40 -1 -17 -7 -11.60 7.10 -2 -17 1 -2.20 15.10 -2 -17 2 30.10 17.40 -2 -17 3 -7.40 14.50 2 -17 5 -5.10 8.40 -2 -17 -6 -7.80 8.30 -3 -17 0 -19.30 15.00 -3 -17 -1 1.80 10.80 -3 -17 1 -8.80 17.60 -3 -17 -2 33.40 10.50 -3 -17 2 5.70 18.70 3 -17 3 7.30 6.80 -3 -17 -3 5.80 9.00 -3 -17 3 8.80 15.50 -3 -17 -4 32.40 9.80 3 -17 4 27.30 10.10 -3 -17 -5 -6.50 8.50 3 -17 5 8.00 9.00 -3 -17 -6 11.20 10.30 -4 -17 0 24.10 19.00 -4 -17 -1 4.40 15.30 -4 -17 1 23.60 19.80 4 -17 2 43.60 9.00 -4 -17 -2 32.40 14.90 -4 -17 2 -3.10 20.40 -4 -17 -3 45.90 13.50 4 -17 3 27.70 9.20 -4 -17 3 8.40 18.70 -4 -17 -4 5.10 11.20 4 -17 4 4.60 8.80 -4 -17 4 -7.80 17.60 -4 -17 -5 31.60 13.30 -5 -17 0 44.80 21.90 -5 -17 -1 -1.60 17.50 -5 -17 1 30.60 21.40 -5 -17 -2 135.99 26.30 5 -17 2 133.89 20.90 -5 -17 2 46.50 27.70 -5 -17 -3 25.80 15.80 5 -17 3 26.30 10.20 -5 -17 3 41.90 20.40 5 -17 4 14.80 11.00 -5 -17 -4 29.50 14.80 -6 -17 0 49.99 23.80 -6 -17 -1 4.10 20.70 -6 -17 1 -0.10 21.70 -6 -17 -2 -2.30 18.70 7 -17 0 108.79 19.10 7 -17 1 18.90 9.60 -1 -18 2 -5.50 14.90 -1 -18 3 50.09 17.20 -2 -18 1 37.50 16.70 -2 -18 2 26.80 17.40 -2 -18 3 23.60 15.70 -3 -18 0 31.10 16.40 -3 -18 1 13.10 17.50 -3 -18 2 16.90 17.50 -3 -18 3 5.80 16.80 3 -18 4 2.10 7.70 -3 -18 -5 41.60 10.90 -4 -18 0 2.00 17.80 -4 -18 -1 0.30 14.30 -4 -18 1 21.10 19.40 -4 -18 -2 41.60 14.50 -4 -18 2 51.09 20.60 4 -18 3 54.69 10.90 -4 -18 -3 27.90 13.80 -4 -18 -4 71.39 16.40 -5 -18 0 8.40 19.90 -5 -18 -1 27.10 19.20 5 -18 2 78.29 13.20 -5 -18 -2 36.80 19.00 5 -18 3 13.30 9.80 6 -18 1 25.10 7.40 6 -18 2 62.89 13.40 0 -19 3 29.10 14.80 -1 -19 2 25.80 15.80 -1 -19 3 25.80 14.80 -2 -19 2 14.40 17.60 -3 -19 1 4.20 16.10 -4 -19 -1 2.30 12.30 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 38370 _shelx_shelxl_version_number 2014/7 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' 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 O1 O 0.65252(19) 0.41130(16) 0.5306(2) 0.0154(4) Uani 1 1 d . O3 O 0.8468(2) 0.38889(17) 0.1351(2) 0.0217(5) Uani 1 1 d . N1 N 0.8776(3) 0.4842(2) 0.8645(2) 0.0194(5) Uani 1 1 d . H1A H 0.9152 0.5429 0.8743 0.023 Uiso 1 1 calc R H1B H 0.8608 0.4472 0.9383 0.023 Uiso 1 1 calc R O4 O 0.9053(2) 0.60855(18) 0.6378(3) 0.0254(5) Uani 1 1 d . H4 H 0.9848 0.6135 0.6394 0.038 Uiso 1 1 calc GR O2 O 0.8701(2) 0.40717(18) 0.3689(2) 0.0229(5) Uani 1 1 d . N2 N 0.8707(2) 0.5061(2) 0.6235(3) 0.0177(5) Uani 1 1 d . C1 C 0.8458(3) 0.4509(2) 0.7367(3) 0.0154(6) Uani 1 1 d . C2 C 0.7841(3) 0.3487(2) 0.7187(3) 0.0154(6) Uani 1 1 d . C7 C 0.6904(3) 0.3287(2) 0.6126(3) 0.0154(6) Uani 1 1 d . C8 C 0.5872(3) 0.3892(2) 0.4036(3) 0.0162(6) Uani 1 1 d . C5 C 0.6765(3) 0.1532(3) 0.6889(3) 0.0233(7) Uani 1 1 d . H5 H 0.6408 0.0878 0.6789 0.028 Uiso 1 1 calc R C6 C 0.6378(3) 0.2315(2) 0.5987(3) 0.0192(6) Uani 1 1 d . H6 H 0.5761 0.2186 0.5284 0.023 Uiso 1 1 calc R C9 C 0.4521(3) 0.3800(3) 0.4104(3) 0.0216(7) Uani 1 1 d . H9 H 0.4091 0.3871 0.4971 0.026 Uiso 1 1 calc R C4 C 0.7684(3) 0.1717(3) 0.7943(3) 0.0268(7) Uani 1 1 d . H4A H 0.7936 0.1189 0.8554 0.032 Uiso 1 1 calc R C12 C 0.5809(3) 0.3636(2) 0.1523(3) 0.0221(7) Uani 1 1 d . H12 H 0.6225 0.3589 0.0645 0.027 Uiso 1 1 calc R C11 C 0.4476(3) 0.3523(3) 0.1588(3) 0.0260(7) Uani 1 1 d . H11 H 0.4009 0.3391 0.0759 0.031 Uiso 1 1 calc R C3 C 0.8218(3) 0.2679(3) 0.8083(3) 0.0227(7) Uani 1 1 d . H3 H 0.8840 0.2797 0.8784 0.027 Uiso 1 1 calc R C14 C 0.8003(3) 0.3931(2) 0.2601(3) 0.0182(6) Uani 1 1 d . C13 C 0.6546(3) 0.3818(2) 0.2743(3) 0.0167(6) Uani 1 1 d . C10 C 0.3826(3) 0.3604(3) 0.2872(4) 0.0253(7) Uani 1 1 d . H10 H 0.2926 0.3527 0.2908 0.030 Uiso 1 1 calc R H2 H 0.857(3) 0.484(3) 0.538(5) 0.023(9) 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 O1 0.0189(10) 0.0134(11) 0.0139(9) 0.0008(8) -0.0029(7) -0.0007(8) O3 0.0314(12) 0.0222(13) 0.0114(9) -0.0007(8) 0.0028(8) -0.0020(9) N1 0.0298(13) 0.0157(14) 0.0128(10) 0.0001(10) -0.0044(10) -0.0053(11) O4 0.0277(12) 0.0201(13) 0.0285(11) 0.0020(9) -0.0023(10) -0.0052(9) O2 0.0229(11) 0.0334(15) 0.0122(9) -0.0045(9) 0.0009(8) -0.0078(10) N2 0.0249(12) 0.0140(13) 0.0141(11) -0.0007(9) -0.0012(10) -0.0054(10) C1 0.0171(13) 0.0152(16) 0.0137(12) 0.0002(10) -0.0013(10) 0.0001(11) C2 0.0223(14) 0.0127(15) 0.0110(11) 0.0014(10) -0.0002(9) -0.0010(12) C7 0.0182(13) 0.0149(16) 0.0131(12) 0.0013(10) 0.0025(10) -0.0006(11) C8 0.0219(14) 0.0120(16) 0.0148(12) -0.0005(10) -0.0049(10) -0.0023(12) C5 0.0320(18) 0.0151(17) 0.0230(14) 0.0004(12) -0.0006(12) -0.0049(14) C6 0.0210(14) 0.0177(17) 0.0188(13) -0.0004(11) -0.0017(11) -0.0036(12) C9 0.0185(14) 0.0204(19) 0.0260(14) -0.0005(13) -0.0038(12) 0.0009(12) C4 0.045(2) 0.0135(18) 0.0222(15) 0.0055(12) -0.0079(14) -0.0008(14) C12 0.0307(17) 0.0181(17) 0.0175(14) -0.0010(12) -0.0052(12) -0.0018(13) C11 0.0314(16) 0.0209(18) 0.0257(15) -0.0014(14) -0.0153(13) 0.0001(14) C3 0.0316(17) 0.0199(18) 0.0167(13) 0.0025(11) -0.0064(11) -0.0025(14) C14 0.0263(15) 0.0141(16) 0.0142(12) -0.0012(10) 0.0005(11) -0.0034(12) C13 0.0231(14) 0.0118(16) 0.0151(12) 0.0000(11) -0.0025(11) -0.0016(11) C10 0.0218(15) 0.0204(19) 0.0337(17) -0.0027(14) -0.0090(14) 0.0006(13) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0000 0.0050 '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 0.0050 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0020 0.0020 '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 C7 O1 C8 116.9(2) H1A N1 H1B 120.0 C1 N1 H1A 120.0 C1 N1 H1B 120.0 N2 O4 H4 109.5 O4 N2 H2 117(3) C1 N2 O4 120.0(2) C1 N2 H2 123(3) N1 C1 C2 120.3(3) N2 C1 N1 120.8(3) N2 C1 C2 118.9(2) C7 C2 C1 122.6(3) C3 C2 C1 119.0(3) C3 C2 C7 118.4(3) O1 C7 C2 116.4(3) O1 C7 C6 123.3(3) C6 C7 C2 120.2(3) O1 C8 C13 121.1(2) C9 C8 O1 117.1(3) C9 C8 C13 121.7(2) C6 C5 H5 119.8 C6 C5 C4 120.3(3) C4 C5 H5 119.8 C7 C6 C5 120.2(3) C7 C6 H6 119.9 C5 C6 H6 119.9 C8 C9 H9 120.3 C10 C9 C8 119.4(3) C10 C9 H9 120.3 C5 C4 H4A 120.1 C3 C4 C5 119.8(3) C3 C4 H4A 120.1 C11 C12 H12 119.3 C11 C12 C13 121.4(3) C13 C12 H12 119.3 C12 C11 H11 119.6 C12 C11 C10 120.7(3) C10 C11 H11 119.6 C2 C3 H3 119.5 C4 C3 C2 121.0(3) C4 C3 H3 119.5 O3 C14 C13 116.8(3) O2 C14 O3 122.8(3) O2 C14 C13 120.4(2) C8 C13 C14 124.1(2) C12 C13 C8 117.1(3) C12 C13 C14 118.9(3) C9 C10 H10 120.2 C11 C10 C9 119.6(3) C11 C10 H10 120.2 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C7 1.377(3) O1 C8 1.398(3) O3 C14 1.268(3) N1 H1A 0.8600 N1 H1B 0.8600 N1 C1 1.317(4) O4 H4 0.8200 O4 N2 1.384(3) O2 C14 1.261(4) N2 C1 1.307(4) N2 H2 0.87(4) C1 C2 1.481(4) C2 C7 1.408(4) C2 C3 1.399(4) C7 C6 1.380(4) C8 C9 1.394(4) C8 C13 1.400(4) C5 H5 0.9300 C5 C6 1.381(4) C5 C4 1.389(5) C6 H6 0.9300 C9 H9 0.9300 C9 C10 1.382(4) C4 H4A 0.9300 C4 C3 1.372(5) C12 H12 0.9300 C12 C11 1.378(5) C12 C13 1.393(4) C11 H11 0.9300 C11 C10 1.381(5) C3 H3 0.9300 C14 C13 1.509(4) C10 H10 0.9300 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 O1 C7 C6 C5 -177.2(3) O1 C8 C9 C10 178.6(3) O1 C8 C13 C12 -177.5(3) O1 C8 C13 C14 2.1(4) O3 C14 C13 C8 -177.1(3) O3 C14 C13 C12 2.5(4) N1 C1 C2 C7 145.9(3) N1 C1 C2 C3 -35.4(4) O4 N2 C1 N1 -13.7(4) O4 N2 C1 C2 167.9(2) O2 C14 C13 C8 2.2(4) O2 C14 C13 C12 -178.2(3) N2 C1 C2 C7 -35.7(4) N2 C1 C2 C3 143.0(3) C1 C2 C7 O1 -3.8(4) C1 C2 C7 C6 178.8(3) C1 C2 C3 C4 -179.2(3) C2 C7 C6 C5 0.1(4) C7 O1 C8 C9 88.8(3) C7 O1 C8 C13 -94.3(3) C7 C2 C3 C4 -0.5(5) C8 O1 C7 C2 163.8(2) C8 O1 C7 C6 -18.8(4) C8 C9 C10 C11 -1.4(5) C5 C4 C3 C2 0.7(5) C6 C5 C4 C3 -0.6(5) C9 C8 C13 C12 -0.8(4) C9 C8 C13 C14 178.8(3) C4 C5 C6 C7 0.1(5) C12 C11 C10 C9 0.0(5) C11 C12 C13 C8 -0.6(4) C11 C12 C13 C14 179.8(3) C3 C2 C7 O1 177.5(3) C3 C2 C7 C6 0.1(4) C13 C8 C9 C10 1.8(5) C13 C12 C11 C10 1.0(5)