#------------------------------------------------------------------------------ #$Date: 2014-09-16 15:20:47 +0300 (Tue, 16 Sep 2014) $ #$Revision: 123872 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/51/77/1517762.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_1517762 loop_ _publ_author_name 'Diana V. Aleksanyan' 'Valentina Yu. Aleksenko' 'Yulia V. Nelyubina' 'Andrei A. Vasil-ev' 'Rinat R. Aysin' 'Zinaida S. Klemenkova' 'Vladimir A. Kozlov' 'Pavel V. Petrovskii' 'Irina L. Odinets' _publ_section_title ; Monoanionic salicylaldimine ligands with (thio)phosphoryl pendant arms: Synthesis and complexing features ; _journal_name_full ; Inorganica Chimica Acta ; _journal_page_first 167 _journal_page_last 174 _journal_volume 404 _journal_year 2013 _chemical_formula_moiety 'C25 H20 N O2 P' _chemical_formula_sum 'C25 H20 N O2 P' _chemical_formula_weight 397.39 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 98.3040(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 14.4880(5) _cell_length_b 6.8633(2) _cell_length_c 20.4926(7) _cell_measurement_reflns_used 2254 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 30 _cell_measurement_theta_min 3 _cell_volume 2016.33(11) _computing_cell_refinement 'APEX2 (Bruker, 2005)' _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_data_reduction 'APEX2 (Bruker, 2005)' _computing_molecular_graphics 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_publication_material 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_structure_refinement 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_structure_solution 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker SMART APEX2 DUO CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0237 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 23166 _diffrn_reflns_theta_full 29.00 _diffrn_reflns_theta_max 29.00 _diffrn_reflns_theta_min 2.01 _exptl_absorpt_coefficient_mu 0.158 _exptl_absorpt_correction_T_max 0.967 _exptl_absorpt_correction_T_min 0.952 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'APEX2 (Bruker, 2005)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.309 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 832 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _refine_diff_density_max 0.410 _refine_diff_density_min -0.327 _refine_diff_density_rms 0.050 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 262 _refine_ls_number_reflns 5365 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.000 _refine_ls_R_factor_all 0.0452 _refine_ls_R_factor_gt 0.0366 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0610P)^2^+0.7900P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0978 _refine_ls_wR_factor_ref 0.1060 _reflns_number_gt 4566 _reflns_number_total 5365 _reflns_threshold_expression I>2/s(I) _iucr_refine_instructions_details ; TITL a in P2(1)/c CELL 0.71073 14.4880 6.8633 20.4926 90.000 98.304 90.000 ZERR 4.00 0.0005 0.0002 0.0007 0.000 0.001 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O P UNIT 100 80 4 8 4 TEMP -173.000 size 0.25 0.25 0.30 L.S. 4 BOND $h htab conf FMAP 2 PLAN 20 omit -4 58 acta WGHT 0.061000 0.790000 FVAR 0.14679 P1 5 0.291384 0.781616 0.330602 11.00000 0.01324 0.01369 = 0.01375 -0.00102 0.00263 -0.00109 O1 4 0.282146 0.650188 0.272274 11.00000 0.02205 0.01758 = 0.01747 -0.00384 0.00347 -0.00209 O2 4 0.177947 0.917429 0.151750 11.00000 0.02165 0.01488 = 0.02021 0.00056 -0.00142 -0.00211 AFIX 3 H2O 2 0.225707 0.928219 0.185150 11.00000 -1.20000 AFIX 0 N1 3 0.316095 1.082390 0.231065 11.00000 0.01397 0.01589 = 0.01429 -0.00012 0.00278 0.00001 C1 1 0.393208 1.077087 0.281769 11.00000 0.01324 0.01347 = 0.01609 -0.00206 0.00284 0.00063 C2 1 0.390218 0.945354 0.333962 11.00000 0.01313 0.01435 = 0.01510 -0.00184 0.00337 -0.00019 C3 1 0.466467 0.935214 0.384159 11.00000 0.01609 0.01817 = 0.01633 0.00106 0.00238 0.00025 AFIX 43 H3A 2 0.464490 0.849154 0.420239 11.00000 -1.20000 AFIX 0 C4 1 0.545197 1.049674 0.381890 11.00000 0.01463 0.02186 = 0.02104 -0.00095 -0.00055 -0.00095 AFIX 43 H4A 2 0.596496 1.041910 0.416357 11.00000 -1.20000 AFIX 0 C5 1 0.548701 1.175409 0.329124 11.00000 0.01350 0.01974 = 0.02515 -0.00073 0.00374 -0.00270 AFIX 43 H5A 2 0.602851 1.252001 0.327169 11.00000 -1.20000 AFIX 0 C6 1 0.473099 1.189179 0.279248 11.00000 0.01651 0.01623 = 0.01992 0.00117 0.00437 -0.00092 AFIX 43 H6A 2 0.475742 1.275235 0.243255 11.00000 -1.20000 AFIX 0 C7 1 0.163868 1.096692 0.124631 11.00000 0.01685 0.01648 = 0.01731 0.00033 0.00321 0.00094 C8 1 0.215539 1.260763 0.149773 11.00000 0.01415 0.01567 = 0.01683 0.00066 0.00357 0.00128 C9 1 0.197017 1.441952 0.119095 11.00000 0.01650 0.01601 = 0.02499 0.00308 0.00352 0.00101 AFIX 43 H9A 2 0.229908 1.554069 0.136933 11.00000 -1.20000 AFIX 0 C10 1 0.131617 1.459721 0.063299 11.00000 0.02000 0.02320 = 0.02602 0.00837 0.00334 0.00470 AFIX 43 H10A 2 0.120545 1.582538 0.042241 11.00000 -1.20000 AFIX 0 C11 1 0.082076 1.295812 0.038226 11.00000 0.02136 0.03078 = 0.02144 0.00300 -0.00288 0.00530 AFIX 43 H11A 2 0.037622 1.307086 -0.000485 11.00000 -1.20000 AFIX 0 C12 1 0.096785 1.116314 0.069029 11.00000 0.02125 0.02400 = 0.02288 -0.00235 -0.00318 -0.00088 AFIX 43 H12A 2 0.061071 1.006566 0.052198 11.00000 -1.20000 AFIX 0 C13 1 0.290163 1.247425 0.205028 11.00000 0.01342 0.01562 = 0.01739 -0.00188 0.00375 -0.00120 AFIX 43 H13A 2 0.320451 1.363033 0.222297 11.00000 -1.20000 AFIX 0 C14 1 0.312611 0.650388 0.407668 11.00000 0.01463 0.01533 = 0.01690 0.00013 0.00258 -0.00335 C15 1 0.277331 0.713731 0.464011 11.00000 0.01974 0.01934 = 0.02067 0.00059 0.00570 0.00065 AFIX 43 H15A 2 0.238816 0.826225 0.461982 11.00000 -1.20000 AFIX 0 C16 1 0.298527 0.612304 0.523059 11.00000 0.02613 0.02577 = 0.01728 -0.00007 0.00709 -0.00243 AFIX 43 H16A 2 0.274294 0.655481 0.561237 11.00000 -1.20000 AFIX 0 C17 1 0.354951 0.448309 0.526322 11.00000 0.02796 0.02266 = 0.01926 0.00532 0.00122 -0.00285 AFIX 43 H17A 2 0.369329 0.379387 0.566714 11.00000 -1.20000 AFIX 0 C18 1 0.390372 0.384912 0.470704 11.00000 0.02637 0.01797 = 0.02492 0.00160 0.00001 0.00266 AFIX 43 H18A 2 0.429114 0.272716 0.473065 11.00000 -1.20000 AFIX 0 C19 1 0.369322 0.485215 0.411406 11.00000 0.02143 0.01852 = 0.01866 -0.00143 0.00280 0.00067 AFIX 43 H19A 2 0.393620 0.441137 0.373363 11.00000 -1.20000 AFIX 0 C20 1 0.189658 0.929340 0.334300 11.00000 0.01455 0.01737 = 0.01468 0.00104 0.00367 0.00043 C21 1 0.102876 0.849305 0.310318 11.00000 0.01772 0.02504 = 0.02388 -0.00149 0.00198 -0.00272 AFIX 43 H21A 2 0.098875 0.721097 0.292662 11.00000 -1.20000 AFIX 0 C22 1 0.022241 0.957647 0.312320 11.00000 0.01402 0.04109 = 0.03040 0.00079 0.00221 -0.00006 AFIX 43 H22A 2 -0.036879 0.902771 0.296247 11.00000 -1.20000 AFIX 0 C23 1 0.027596 1.144752 0.337562 11.00000 0.01949 0.03610 = 0.02627 0.00694 0.00744 0.01018 AFIX 43 H23A 2 -0.027739 1.218172 0.338691 11.00000 -1.20000 AFIX 0 C24 1 0.113779 1.225347 0.361252 11.00000 0.02710 0.02344 = 0.03141 -0.00086 0.01001 0.00517 AFIX 43 H24A 2 0.117485 1.354182 0.378380 11.00000 -1.20000 AFIX 0 C25 1 0.194590 1.117595 0.359910 11.00000 0.01829 0.02062 = 0.02774 -0.00400 0.00485 -0.00040 AFIX 43 H25B 2 0.253494 1.172528 0.376533 11.00000 -1.20000 HKLF 4 REM a in P2(1)/c REM R1 = 0.0366 for 4566 Fo > 4sig(Fo) and 0.0452 for all 5365 data REM 262 parameters refined using 0 restraints END WGHT 0.0508 0.8745 REM Highest difference peak 0.410, deepest hole -0.327, 1-sigma level 0.050 Q1 1 0.3474 0.8726 0.3324 11.00000 0.05 0.41 Q2 1 0.2757 0.6765 0.3072 11.00000 0.05 0.38 Q3 1 0.2386 0.8651 0.3246 11.00000 0.05 0.38 Q4 1 0.1427 0.9047 0.3204 11.00000 0.05 0.36 Q5 1 0.3068 0.7077 0.3707 11.00000 0.05 0.36 Q6 1 0.1897 1.0292 0.3444 11.00000 0.05 0.36 Q7 1 0.2924 0.6475 0.4899 11.00000 0.05 0.36 Q8 1 0.3698 0.4345 0.4399 11.00000 0.05 0.36 Q9 1 0.3957 0.9938 0.3038 11.00000 0.05 0.36 Q10 1 0.2003 1.3522 0.1369 11.00000 0.05 0.35 Q11 1 0.4338 1.1351 0.2822 11.00000 0.05 0.35 Q12 1 0.2487 1.2492 0.1764 11.00000 0.05 0.35 Q13 1 0.3037 0.7452 0.2907 11.00000 0.05 0.34 Q14 1 0.0744 1.1861 0.3418 11.00000 0.05 0.34 Q15 1 0.5148 1.1577 0.2996 11.00000 0.05 0.32 Q16 1 0.1392 1.1013 0.0914 11.00000 0.05 0.32 Q17 1 0.2992 0.6729 0.4363 11.00000 0.05 0.32 Q18 1 0.3302 0.5522 0.4094 11.00000 0.05 0.31 Q19 1 0.3317 0.5298 0.5203 11.00000 0.05 0.30 Q20 1 0.1929 1.1873 0.1385 11.00000 0.05 0.30 ; _[local]_cod_data_source_file ICA-2013-404-167-174-1.cif _[local]_cod_data_source_block 1a _[local]_cod_cif_authors_sg_H-M 'P 21/c' _cod_database_code 1517762 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags P1 P 0.29138(2) 0.78162(4) 0.330602(14) 0.01349(9) Uani 1 1 d . O1 O 0.28215(6) 0.65019(13) 0.27227(4) 0.01897(19) Uani 1 1 d . O2 O 0.17795(6) 0.91743(13) 0.15175(4) 0.01935(19) Uani 1 1 d . H2O H 0.2257 0.9282 0.1851 0.023 Uiso 1 1 d R N1 N 0.31609(7) 1.08239(15) 0.23107(5) 0.0146(2) Uani 1 1 d . C1 C 0.39321(8) 1.07709(17) 0.28177(6) 0.0142(2) Uani 1 1 d . C2 C 0.39022(8) 0.94535(17) 0.33396(6) 0.0141(2) Uani 1 1 d . C3 C 0.46647(8) 0.93521(18) 0.38416(6) 0.0169(2) Uani 1 1 d . H3A H 0.4645 0.8492 0.4202 0.020 Uiso 1 1 calc R C4 C 0.54520(9) 1.04967(19) 0.38189(6) 0.0195(2) Uani 1 1 d . H4A H 0.5965 1.0419 0.4164 0.023 Uiso 1 1 calc R C5 C 0.54870(8) 1.17541(19) 0.32912(6) 0.0194(2) Uani 1 1 d . H5A H 0.6029 1.2520 0.3272 0.023 Uiso 1 1 calc R C6 C 0.47310(8) 1.18918(18) 0.27925(6) 0.0174(2) Uani 1 1 d . H6A H 0.4757 1.2752 0.2433 0.021 Uiso 1 1 calc R C7 C 0.16387(8) 1.09669(18) 0.12463(6) 0.0168(2) Uani 1 1 d . C8 C 0.21554(8) 1.26076(18) 0.14977(6) 0.0154(2) Uani 1 1 d . C9 C 0.19702(9) 1.44195(18) 0.11909(6) 0.0191(2) Uani 1 1 d . H9A H 0.2299 1.5541 0.1369 0.023 Uiso 1 1 calc R C10 C 0.13162(9) 1.4597(2) 0.06330(7) 0.0231(3) Uani 1 1 d . H10A H 0.1205 1.5825 0.0422 0.028 Uiso 1 1 calc R C11 C 0.08208(10) 1.2958(2) 0.03823(7) 0.0251(3) Uani 1 1 d . H11A H 0.0376 1.3071 -0.0005 0.030 Uiso 1 1 calc R C12 C 0.09678(9) 1.1163(2) 0.06903(7) 0.0233(3) Uani 1 1 d . H12A H 0.0611 1.0066 0.0522 0.028 Uiso 1 1 calc R C13 C 0.29016(8) 1.24742(18) 0.20503(6) 0.0153(2) Uani 1 1 d . H13A H 0.3205 1.3630 0.2223 0.018 Uiso 1 1 calc R C14 C 0.31261(8) 0.65039(18) 0.40767(6) 0.0156(2) Uani 1 1 d . C15 C 0.27733(9) 0.71373(19) 0.46401(6) 0.0196(2) Uani 1 1 d . H15A H 0.2388 0.8262 0.4620 0.024 Uiso 1 1 calc R C16 C 0.29853(9) 0.6123(2) 0.52306(6) 0.0227(3) Uani 1 1 d . H16A H 0.2743 0.6555 0.5612 0.027 Uiso 1 1 calc R C17 C 0.35495(10) 0.4483(2) 0.52632(7) 0.0235(3) Uani 1 1 d . H17A H 0.3693 0.3794 0.5667 0.028 Uiso 1 1 calc R C18 C 0.39037(10) 0.3849(2) 0.47070(7) 0.0235(3) Uani 1 1 d . H18A H 0.4291 0.2727 0.4731 0.028 Uiso 1 1 calc R C19 C 0.36932(9) 0.48522(19) 0.41141(6) 0.0195(2) Uani 1 1 d . H19A H 0.3936 0.4411 0.3734 0.023 Uiso 1 1 calc R C20 C 0.18966(8) 0.92934(18) 0.33430(6) 0.0154(2) Uani 1 1 d . C21 C 0.10288(9) 0.8493(2) 0.31032(7) 0.0223(3) Uani 1 1 d . H21A H 0.0989 0.7211 0.2927 0.027 Uiso 1 1 calc R C22 C 0.02224(9) 0.9576(2) 0.31232(7) 0.0286(3) Uani 1 1 d . H22A H -0.0369 0.9028 0.2962 0.034 Uiso 1 1 calc R C23 C 0.02760(9) 1.1448(2) 0.33756(7) 0.0269(3) Uani 1 1 d . H23A H -0.0277 1.2182 0.3387 0.032 Uiso 1 1 calc R C24 C 0.11378(10) 1.2253(2) 0.36125(7) 0.0267(3) Uani 1 1 d . H24A H 0.1175 1.3542 0.3784 0.032 Uiso 1 1 calc R C25 C 0.19459(9) 1.1176(2) 0.35991(7) 0.0221(3) Uani 1 1 d . H25B H 0.2535 1.1725 0.3765 0.026 Uiso 1 1 calc R 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 P1 0.01324(15) 0.01369(15) 0.01374(15) -0.00102(10) 0.00263(10) -0.00109(10) O1 0.0221(4) 0.0176(4) 0.0175(4) -0.0038(3) 0.0035(3) -0.0021(3) O2 0.0217(4) 0.0149(4) 0.0202(4) 0.0006(3) -0.0014(3) -0.0021(3) N1 0.0140(5) 0.0159(5) 0.0143(5) -0.0001(4) 0.0028(4) 0.0000(4) C1 0.0132(5) 0.0135(5) 0.0161(5) -0.0021(4) 0.0028(4) 0.0006(4) C2 0.0131(5) 0.0143(5) 0.0151(5) -0.0018(4) 0.0034(4) -0.0002(4) C3 0.0161(5) 0.0182(6) 0.0163(5) 0.0011(4) 0.0024(4) 0.0002(4) C4 0.0146(5) 0.0219(6) 0.0210(6) -0.0010(5) -0.0006(4) -0.0009(5) C5 0.0135(5) 0.0197(6) 0.0251(6) -0.0007(5) 0.0037(5) -0.0027(4) C6 0.0165(5) 0.0162(6) 0.0199(6) 0.0012(4) 0.0044(4) -0.0009(4) C7 0.0169(5) 0.0165(6) 0.0173(5) 0.0003(4) 0.0032(4) 0.0009(4) C8 0.0142(5) 0.0157(5) 0.0168(5) 0.0007(4) 0.0036(4) 0.0013(4) C9 0.0165(6) 0.0160(6) 0.0250(6) 0.0031(5) 0.0035(5) 0.0010(4) C10 0.0200(6) 0.0232(6) 0.0260(7) 0.0084(5) 0.0033(5) 0.0047(5) C11 0.0214(6) 0.0308(7) 0.0214(6) 0.0030(5) -0.0029(5) 0.0053(5) C12 0.0212(6) 0.0240(6) 0.0229(6) -0.0023(5) -0.0032(5) -0.0009(5) C13 0.0134(5) 0.0156(5) 0.0174(5) -0.0019(4) 0.0037(4) -0.0012(4) C14 0.0146(5) 0.0153(5) 0.0169(5) 0.0001(4) 0.0026(4) -0.0033(4) C15 0.0197(6) 0.0193(6) 0.0207(6) 0.0006(5) 0.0057(5) 0.0007(5) C16 0.0261(6) 0.0258(7) 0.0173(6) -0.0001(5) 0.0071(5) -0.0024(5) C17 0.0280(7) 0.0227(6) 0.0193(6) 0.0053(5) 0.0012(5) -0.0029(5) C18 0.0264(7) 0.0180(6) 0.0249(6) 0.0016(5) 0.0000(5) 0.0027(5) C19 0.0214(6) 0.0185(6) 0.0187(6) -0.0014(5) 0.0028(5) 0.0007(5) C20 0.0146(5) 0.0174(6) 0.0147(5) 0.0010(4) 0.0037(4) 0.0004(4) C21 0.0177(6) 0.0250(7) 0.0239(6) -0.0015(5) 0.0020(5) -0.0027(5) C22 0.0140(6) 0.0411(8) 0.0304(7) 0.0008(6) 0.0022(5) -0.0001(6) C23 0.0195(6) 0.0361(8) 0.0263(7) 0.0069(6) 0.0074(5) 0.0102(6) C24 0.0271(7) 0.0234(7) 0.0314(7) -0.0009(6) 0.0100(6) 0.0052(5) C25 0.0183(6) 0.0206(6) 0.0277(6) -0.0040(5) 0.0049(5) -0.0004(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 O1 P1 C20 113.34(5) O1 P1 C14 112.61(6) C20 P1 C14 106.34(5) O1 P1 C2 112.65(5) C20 P1 C2 107.23(6) C14 P1 C2 104.01(5) C7 O2 H2O 106.9 C13 N1 C1 118.76(10) C6 C1 C2 119.93(11) C6 C1 N1 122.03(11) C2 C1 N1 117.93(10) C3 C2 C1 118.93(11) C3 C2 P1 122.18(9) C1 C2 P1 118.72(9) C4 C3 C2 120.78(11) C4 C3 H3A 119.6 C2 C3 H3A 119.6 C5 C4 C3 119.92(11) C5 C4 H4A 120.0 C3 C4 H4A 120.0 C6 C5 C4 120.07(11) C6 C5 H5A 120.0 C4 C5 H5A 120.0 C5 C6 C1 120.32(11) C5 C6 H6A 119.8 C1 C6 H6A 119.8 O2 C7 C12 118.01(11) O2 C7 C8 122.42(11) C12 C7 C8 119.55(11) C9 C8 C7 119.22(11) C9 C8 C13 118.60(11) C7 C8 C13 122.13(11) C10 C9 C8 120.91(12) C10 C9 H9A 119.5 C8 C9 H9A 119.5 C9 C10 C11 119.32(12) C9 C10 H10A 120.3 C11 C10 H10A 120.3 C12 C11 C10 120.85(12) C12 C11 H11A 119.6 C10 C11 H11A 119.6 C11 C12 C7 120.09(12) C11 C12 H12A 120.0 C7 C12 H12A 120.0 N1 C13 C8 121.32(11) N1 C13 H13A 119.3 C8 C13 H13A 119.3 C19 C14 C15 119.33(11) C19 C14 P1 118.54(9) C15 C14 P1 122.07(10) C16 C15 C14 120.11(12) C16 C15 H15A 119.9 C14 C15 H15A 119.9 C17 C16 C15 120.16(12) C17 C16 H16A 119.9 C15 C16 H16A 119.9 C18 C17 C16 120.05(12) C18 C17 H17A 120.0 C16 C17 H17A 120.0 C17 C18 C19 120.16(12) C17 C18 H18A 119.9 C19 C18 H18A 119.9 C18 C19 C14 120.18(12) C18 C19 H19A 119.9 C14 C19 H19A 119.9 C25 C20 C21 119.52(12) C25 C20 P1 122.74(9) C21 C20 P1 117.73(10) C22 C21 C20 119.83(13) C22 C21 H21A 120.1 C20 C21 H21A 120.1 C23 C22 C21 120.39(13) C23 C22 H22A 119.8 C21 C22 H22A 119.8 C22 C23 C24 120.01(13) C22 C23 H23A 120.0 C24 C23 H23A 120.0 C23 C24 C25 119.97(13) C23 C24 H24A 120.0 C25 C24 H24A 120.0 C24 C25 C20 120.28(12) C24 C25 H25B 119.9 C20 C25 H25B 119.9 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance P1 O1 1.4880(9) P1 C20 1.7995(12) P1 C14 1.8054(12) P1 C2 1.8137(12) O2 C7 1.3533(15) O2 H2O 0.9033 N1 C13 1.2849(16) N1 C1 1.4120(15) C1 C6 1.3970(16) C1 C2 1.4059(16) C2 C3 1.3982(16) C3 C4 1.3913(17) C3 H3A 0.9500 C4 C5 1.3901(18) C4 H4A 0.9500 C5 C6 1.3892(17) C5 H5A 0.9500 C6 H6A 0.9500 C7 C12 1.3932(17) C7 C8 1.4080(17) C8 C9 1.4018(17) C8 C13 1.4511(16) C9 C10 1.3810(18) C9 H9A 0.9500 C10 C11 1.392(2) C10 H10A 0.9500 C11 C12 1.3866(19) C11 H11A 0.9500 C12 H12A 0.9500 C13 H13A 0.9500 C14 C19 1.3957(17) C14 C15 1.3978(17) C15 C16 1.3913(18) C15 H15A 0.9500 C16 C17 1.3870(19) C16 H16A 0.9500 C17 C18 1.386(2) C17 H17A 0.9500 C18 C19 1.3916(18) C18 H18A 0.9500 C19 H19A 0.9500 C20 C25 1.3925(18) C20 C21 1.3948(17) C21 C22 1.3904(19) C21 H21A 0.9500 C22 C23 1.382(2) C22 H22A 0.9500 C23 C24 1.388(2) C23 H23A 0.9500 C24 C25 1.3884(19) C24 H24A 0.9500 C25 H25B 0.9500 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA O2 H2O N1 1_555 0.90 1.83 2.6438(13) 148 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 C13 N1 C1 C6 -40.89(16) C13 N1 C1 C2 142.95(11) C6 C1 C2 C3 2.69(17) N1 C1 C2 C3 178.93(10) C6 C1 C2 P1 -172.71(9) N1 C1 C2 P1 3.53(14) O1 P1 C2 C3 -114.63(10) C20 P1 C2 C3 120.00(10) C14 P1 C2 C3 7.61(11) O1 P1 C2 C1 60.61(11) C20 P1 C2 C1 -64.76(10) C14 P1 C2 C1 -177.15(9) C1 C2 C3 C4 -1.64(18) P1 C2 C3 C4 173.60(10) C2 C3 C4 C5 -0.23(19) C3 C4 C5 C6 1.05(19) C4 C5 C6 C1 0.02(19) C2 C1 C6 C5 -1.91(18) N1 C1 C6 C5 -177.99(11) O2 C7 C8 C9 -179.96(11) C12 C7 C8 C9 1.34(18) O2 C7 C8 C13 2.51(18) C12 C7 C8 C13 -176.18(11) C7 C8 C9 C10 -2.54(19) C13 C8 C9 C10 175.07(12) C8 C9 C10 C11 1.5(2) C9 C10 C11 C12 0.8(2) C10 C11 C12 C7 -2.0(2) O2 C7 C12 C11 -177.85(12) C8 C7 C12 C11 0.9(2) C1 N1 C13 C8 175.76(10) C9 C8 C13 N1 -173.37(11) C7 C8 C13 N1 4.18(18) O1 P1 C14 C19 36.96(11) C20 P1 C14 C19 161.66(10) C2 P1 C14 C19 -85.31(10) O1 P1 C14 C15 -145.77(10) C20 P1 C14 C15 -21.06(12) C2 P1 C14 C15 91.97(11) C19 C14 C15 C16 -0.18(19) P1 C14 C15 C16 -177.44(10) C14 C15 C16 C17 0.2(2) C15 C16 C17 C18 0.0(2) C16 C17 C18 C19 -0.1(2) C17 C18 C19 C14 0.1(2) C15 C14 C19 C18 0.02(19) P1 C14 C19 C18 177.37(10) O1 P1 C20 C25 -146.60(10) C14 P1 C20 C25 89.15(11) C2 P1 C20 C25 -21.64(12) O1 P1 C20 C21 33.45(12) C14 P1 C20 C21 -90.80(11) C2 P1 C20 C21 158.41(10) C25 C20 C21 C22 -0.15(19) P1 C20 C21 C22 179.80(10) C20 C21 C22 C23 0.4(2) C21 C22 C23 C24 -0.2(2) C22 C23 C24 C25 -0.3(2) C23 C24 C25 C20 0.6(2) C21 C20 C25 C24 -0.3(2) P1 C20 C25 C24 179.70(11) loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_calc _refln_F_squared_meas _refln_F_squared_sigma _refln_observed_status 2 0 0 11842.79 11680.48 137.04 o 3 0 0 700.70 693.80 8.24 o 4 0 0 57.67 74.72 3.39 o 5 0 0 3117.76 3279.25 30.15 o 6 0 0 450.43 505.21 8.81 o 7 0 0 2893.06 2809.21 48.64 o 8 0 0 2073.28 2169.15 24.49 o 9 0 0 1356.35 1425.65 34.02 o 10 0 0 7171.19 7286.81 140.85 o 11 0 0 3150.16 3148.75 35.21 o 12 0 0 6227.62 6257.01 69.83 o 13 0 0 375.42 396.97 11.47 o 14 0 0 254.13 253.79 9.97 o 15 0 0 123.29 121.38 10.81 o 16 0 0 521.48 514.88 19.68 o 17 0 0 109.13 104.49 10.90 o 18 0 0 18.60 31.09 8.86 o 19 0 0 706.01 764.39 27.00 o 1 1 0 686.08 764.46 5.88 o 2 1 0 6382.47 6542.92 41.05 o 3 1 0 8420.03 8649.34 55.97 o 4 1 0 1779.66 1893.08 13.46 o 5 1 0 1206.86 1204.34 10.14 o 6 1 0 8071.74 8399.82 49.97 o 7 1 0 517.31 554.40 7.03 o 8 1 0 2987.59 2996.58 22.02 o 9 1 0 483.29 459.66 7.11 o 10 1 0 822.89 786.36 9.96 o 11 1 0 158.19 155.19 4.94 o 12 1 0 260.33 240.40 6.15 o 13 1 0 855.78 859.48 13.91 o 14 1 0 183.23 201.74 13.07 o 15 1 0 0.60 0.55 2.97 o 16 1 0 208.22 223.25 9.99 o 17 1 0 114.59 125.87 8.43 o 18 1 0 486.13 509.84 15.17 o 19 1 0 5.83 9.21 5.32 o 0 2 0 37.88 28.17 3.10 o 1 2 0 256.29 302.99 3.97 o 2 2 0 2165.89 2234.97 15.39 o 3 2 0 924.02 879.64 8.09 o 4 2 0 6248.79 6751.81 40.23 o 5 2 0 13969.42 14565.38 86.95 o 6 2 0 2704.79 2860.51 23.16 o 7 2 0 2215.68 2210.83 17.46 o 8 2 0 308.77 300.56 6.69 o 9 2 0 83.00 70.95 3.24 o 10 2 0 1001.79 1012.39 11.53 o 11 2 0 17.65 18.86 2.70 o 12 2 0 528.81 532.70 10.80 o 13 2 0 0.43 0.91 2.84 o 14 2 0 1370.75 1384.31 19.21 o 15 2 0 394.56 416.48 10.85 o 16 2 0 753.02 789.75 15.30 o 17 2 0 337.46 374.94 12.92 o 18 2 0 150.41 163.16 13.20 o 19 2 0 24.14 18.89 6.96 o 1 3 0 473.73 458.01 5.88 o 2 3 0 1408.73 1477.41 12.36 o 3 3 0 29.86 25.22 1.89 o 4 3 0 1881.18 1922.53 16.74 o 5 3 0 1453.90 1749.01 14.89 o 6 3 0 21.79 31.35 3.01 o 7 3 0 368.06 359.67 6.25 o 8 3 0 1108.20 1185.83 20.05 o 9 3 0 106.70 120.17 4.63 o 10 3 0 0.01 0.98 2.29 o 11 3 0 6.98 14.08 3.13 o 12 3 0 3.78 1.64 3.21 o 13 3 0 164.45 164.42 8.00 o 14 3 0 1.03 1.77 3.61 o 15 3 0 51.66 59.18 7.74 o 16 3 0 1.53 0.89 4.76 o 17 3 0 0.02 -8.57 4.29 o 18 3 0 27.29 36.17 7.28 o 0 4 0 222.38 302.78 7.54 o 1 4 0 119.42 141.44 3.77 o 2 4 0 11.54 6.36 1.57 o 3 4 0 181.72 199.73 4.63 o 4 4 0 216.57 263.83 5.36 o 5 4 0 206.43 191.20 4.81 o 6 4 0 196.49 204.71 5.19 o 7 4 0 36.03 38.61 2.87 o 8 4 0 272.92 282.86 6.34 o 9 4 0 2.81 8.39 2.77 o 10 4 0 44.33 19.77 3.41 o 11 4 0 0.34 1.67 2.72 o 12 4 0 761.91 736.72 13.53 o 13 4 0 0.00 0.49 2.90 o 14 4 0 1432.05 1343.67 19.88 o 15 4 0 0.54 3.07 3.38 o 16 4 0 65.13 58.90 8.71 o 17 4 0 221.93 206.42 13.59 o 1 5 0 445.79 455.70 8.13 o 2 5 0 3.27 9.07 1.81 o 3 5 0 100.02 107.84 5.64 o 4 5 0 420.89 429.99 7.44 o 5 5 0 460.54 471.86 8.92 o 6 5 0 185.15 179.61 5.42 o 7 5 0 382.40 415.83 7.95 o 8 5 0 275.56 260.98 6.59 o 9 5 0 84.67 59.38 5.56 o 10 5 0 325.53 284.01 9.90 o 11 5 0 52.27 47.25 5.80 o 12 5 0 19.47 21.67 4.87 o 13 5 0 349.18 318.48 11.75 o 14 5 0 32.12 37.10 5.95 o 15 5 0 0.01 -2.93 4.04 o 16 5 0 15.94 26.60 11.96 o 0 6 0 1936.95 1905.46 51.29 o 1 6 0 0.02 -3.03 2.63 o 2 6 0 1043.46 1018.64 14.74 o 3 6 0 140.16 121.34 5.76 o 4 6 0 50.66 53.37 4.54 o 5 6 0 275.13 263.97 8.16 o 6 6 0 178.90 174.62 6.95 o 7 6 0 12.63 10.98 3.37 o 8 6 0 349.88 329.69 10.97 o 9 6 0 255.12 223.22 9.78 o 10 6 0 680.03 622.49 15.49 o 11 6 0 0.00 -3.90 3.73 o 12 6 0 34.17 29.61 5.42 o 13 6 0 23.65 21.50 6.70 o 14 6 0 17.16 13.08 5.07 o 15 6 0 18.73 27.65 9.69 o 1 7 0 188.87 180.02 8.80 o 2 7 0 8.04 9.88 4.19 o 3 7 0 54.18 46.73 5.78 o 4 7 0 93.48 90.56 6.98 o 5 7 0 126.09 114.09 6.58 o 6 7 0 0.59 3.01 3.47 o 7 7 0 5.04 2.02 3.92 o 8 7 0 6.49 -0.07 3.85 o 9 7 0 50.84 56.33 6.67 o 10 7 0 8.95 14.57 5.18 o 11 7 0 74.10 73.51 7.53 o 12 7 0 0.42 3.68 4.72 o 0 8 0 173.24 169.08 13.59 o 1 8 0 202.62 179.42 9.73 o 2 8 0 216.13 253.69 10.95 o 3 8 0 240.43 223.38 10.74 o 4 8 0 1.60 -0.78 4.78 o 5 8 0 57.21 62.33 9.00 o 6 8 0 47.71 60.70 9.82 o 7 8 0 13.88 11.13 6.29 o 8 8 0 20.14 24.12 6.89 o 9 8 0 0.31 -2.35 4.91 o 10 8 0 104.69 118.41 11.21 o 1 9 0 41.90 56.84 8.11 o 2 9 0 55.75 70.38 9.60 o 3 9 0 65.20 83.13 8.26 o 4 9 0 86.41 131.18 11.84 o 5 9 0 0.55 -0.07 5.71 o -19 1 1 246.50 256.47 12.11 o -18 1 1 117.25 120.63 8.90 o -17 1 1 26.17 28.43 6.36 o -16 1 1 2.40 4.68 3.96 o -15 1 1 897.63 908.65 15.41 o -14 1 1 183.90 180.73 7.77 o -13 1 1 1815.37 1816.66 21.12 o -12 1 1 333.71 318.99 6.91 o -11 1 1 757.97 714.44 9.79 o -10 1 1 63.71 55.02 3.04 o -9 1 1 1444.35 1479.72 16.59 o -8 1 1 436.59 493.47 6.79 o -7 1 1 346.33 376.60 5.90 o -6 1 1 1792.65 1990.40 15.00 o -5 1 1 1242.22 1423.79 11.27 o -4 1 1 3819.64 4034.79 23.36 o -3 1 1 10979.48 11553.05 66.01 o -2 1 1 972.19 1007.91 7.89 o -1 1 1 1894.15 1914.28 15.19 o 0 1 1 44.27 43.38 1.12 o 1 1 1 8984.11 8803.50 61.69 o 2 1 1 6822.04 6936.03 71.60 o 3 1 1 2712.72 2747.03 17.79 o 4 1 1 1380.52 1368.89 10.66 o 5 1 1 14.78 8.07 1.14 o 6 1 1 333.07 395.84 5.63 o 7 1 1 1414.43 1409.57 12.60 o 8 1 1 139.18 157.79 4.18 o 9 1 1 116.23 105.07 3.71 o 10 1 1 39.21 43.67 2.85 o 11 1 1 359.93 297.77 6.62 o 12 1 1 369.74 346.98 7.26 o 13 1 1 974.06 965.75 12.87 o 14 1 1 0.63 1.83 3.00 o 15 1 1 415.80 437.06 10.85 o 16 1 1 9.89 2.45 3.86 o 17 1 1 29.06 35.49 5.86 o 18 1 1 9.63 8.92 6.30 o 19 1 1 115.47 121.14 14.00 o -19 2 1 56.73 72.86 8.06 o -18 2 1 0.72 0.90 4.44 o -17 2 1 45.19 47.52 6.29 o -16 2 1 2.89 -3.14 3.23 o -15 2 1 23.28 23.10 4.13 o -14 2 1 342.39 343.60 9.59 o -13 2 1 30.19 25.67 3.86 o -12 2 1 0.01 -1.35 2.58 o -11 2 1 25.53 17.41 3.14 o -10 2 1 0.69 -0.11 1.57 o -9 2 1 241.73 312.81 6.09 o -8 2 1 119.58 146.32 3.84 o -7 2 1 1754.00 1937.98 15.60 o -6 2 1 2.35 5.95 1.59 o -5 2 1 536.93 628.64 7.62 o -4 2 1 2118.71 2411.14 16.99 o -3 2 1 1329.98 1400.20 10.99 o -2 2 1 1582.59 1534.78 13.69 o -1 2 1 677.22 703.80 6.50 o 0 2 1 1126.68 1255.90 9.74 o 1 2 1 2337.70 2555.30 16.99 o 2 2 1 717.74 773.40 7.32 o 3 2 1 8921.32 9423.22 55.91 o 4 2 1 60.49 57.71 2.35 o 5 2 1 792.47 938.60 9.32 o 6 2 1 5.99 12.72 2.06 o 7 2 1 39.12 38.29 2.36 o 8 2 1 481.73 589.87 8.03 o 9 2 1 724.00 778.82 9.83 o 10 2 1 642.40 616.39 8.96 o 11 2 1 108.18 118.86 4.75 o 12 2 1 0.32 3.77 2.84 o 13 2 1 188.31 176.62 6.96 o 14 2 1 30.55 33.42 4.44 o 15 2 1 11.40 10.65 3.64 o 16 2 1 19.41 20.16 4.37 o 17 2 1 883.15 923.45 19.57 o 18 2 1 19.89 17.13 5.29 o -18 3 1 5.79 -1.29 12.67 o -17 3 1 4.20 2.68 4.48 o -16 3 1 189.35 184.54 8.38 o -15 3 1 273.61 279.76 10.94 o -14 3 1 113.04 117.98 6.50 o -13 3 1 15.96 4.84 3.21 o -12 3 1 34.41 30.80 4.39 o -11 3 1 20.53 2.30 3.06 o -10 3 1 17.37 43.10 3.70 o -9 3 1 17.22 11.99 2.58 o -8 3 1 148.97 180.62 4.38 o -7 3 1 514.14 537.89 7.82 o -6 3 1 12.60 8.33 2.25 o -5 3 1 149.73 195.72 4.31 o -4 3 1 1.62 3.10 1.38 o -3 3 1 17.14 32.45 2.04 o -2 3 1 99.43 100.88 3.18 o -1 3 1 0.71 -0.05 1.52 o 0 3 1 19.42 26.21 1.80 o 1 3 1 428.31 442.57 5.84 o 2 3 1 1856.07 2133.36 16.21 o 3 3 1 294.96 311.43 5.21 o 4 3 1 0.99 6.80 1.58 o 5 3 1 6.36 2.62 1.58 o 6 3 1 99.07 103.73 3.63 o 7 3 1 549.60 654.31 8.69 o 8 3 1 68.07 78.80 4.08 o 9 3 1 16.37 29.73 2.58 o 10 3 1 136.54 151.04 4.74 o 11 3 1 797.48 684.17 15.77 o 12 3 1 20.01 21.65 3.73 o 13 3 1 43.04 38.20 4.34 o 14 3 1 59.26 66.60 6.42 o 15 3 1 33.01 22.65 4.54 o 16 3 1 430.52 445.07 11.83 o 17 3 1 54.64 47.92 6.57 o 18 3 1 10.83 10.55 8.83 o -17 4 1 55.07 51.01 6.90 o -16 4 1 118.98 127.49 8.56 o -15 4 1 291.96 310.21 11.66 o -14 4 1 114.61 95.14 6.19 o -13 4 1 0.78 1.28 3.04 o -12 4 1 22.48 22.60 3.84 o -11 4 1 135.34 130.22 6.25 o -10 4 1 401.40 370.06 8.91 o -9 4 1 234.29 182.14 6.33 o -8 4 1 99.53 87.12 3.89 o -7 4 1 162.88 156.37 4.68 o -6 4 1 512.28 496.80 8.14 o -5 4 1 1512.95 1447.34 13.75 o -4 4 1 600.59 630.96 8.66 o -3 4 1 62.38 64.35 2.88 o -2 4 1 6.71 0.56 2.54 o -1 4 1 366.41 424.17 6.24 o 0 4 1 747.46 916.17 16.58 o 1 4 1 31.38 42.73 2.44 o 2 4 1 1615.32 1778.05 15.36 o 3 4 1 3640.20 3703.83 26.47 o 4 4 1 13.26 9.63 1.91 o 5 4 1 500.74 416.34 7.08 o 6 4 1 43.20 54.40 3.12 o 7 4 1 70.56 48.19 3.17 o 8 4 1 331.91 261.31 6.23 o 9 4 1 230.63 261.23 6.43 o 10 4 1 0.06 -3.28 2.54 o 11 4 1 308.58 312.65 8.71 o 12 4 1 21.90 6.97 3.25 o 13 4 1 624.45 605.42 12.71 o 14 4 1 467.61 464.96 11.63 o 15 4 1 128.24 140.33 7.45 o 16 4 1 3.02 -0.22 5.42 o 17 4 1 6.69 -1.29 5.42 o -16 5 1 70.97 80.42 12.06 o -15 5 1 934.81 935.52 20.25 o -14 5 1 8.81 9.73 4.54 o -13 5 1 872.62 836.18 18.17 o -12 5 1 15.73 14.41 5.83 o -11 5 1 233.60 225.45 9.33 o -10 5 1 131.46 136.86 7.62 o -9 5 1 71.87 74.47 5.86 o -8 5 1 342.98 301.26 9.34 o -7 5 1 450.15 419.91 11.04 o -6 5 1 598.11 596.20 9.00 o -5 5 1 1433.01 1353.84 17.38 o -4 5 1 1570.81 1548.12 18.64 o -3 5 1 176.92 167.97 4.47 o -2 5 1 38.70 44.38 2.74 o -1 5 1 616.23 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