#------------------------------------------------------------------------------ #$Date: 2020-10-06 14:42:26 +0300 (Tue, 06 Oct 2020) $ #$Revision: 258103 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/05/7240529.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_7240529 loop_ _publ_author_name 'Podjed, Nina' 'Modec, Barbara' 'Alcaide, Mar\'ia M.' 'L\'opez-Serrano, Joaqu\'in' _publ_section_title ; From cyclic amines and acetonitrile to amidine zinc(ii) complexes ; _journal_issue 31 _journal_name_full 'RSC Advances' _journal_page_first 18200 _journal_page_last 18221 _journal_paper_doi 10.1039/D0RA03192E _journal_volume 10 _journal_year 2020 _chemical_formula_moiety 'C26 H24 N4 O4 Zn, C2 H3 N, 0.5(H2 O), 0.5(C6 H12 N2)' _chemical_formula_sum 'C31 H34 N6 O4.5 Zn' _chemical_formula_weight 628.01 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _audit_creation_date 2019-12-16 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2019-12-19 deposited with the CCDC. 2020-04-29 downloaded from the CCDC. ; _cell_angle_alpha 81.018(2) _cell_angle_beta 78.984(2) _cell_angle_gamma 86.388(2) _cell_formula_units_Z 2 _cell_length_a 7.9798(2) _cell_length_b 12.1068(3) _cell_length_c 15.2595(4) _cell_measurement_reflns_used 13111 _cell_measurement_temperature 150.00(10) _cell_measurement_theta_max 30.2820 _cell_measurement_theta_min 2.9920 _cell_volume 1428.47(6) _computing_cell_refinement 'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46e (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 2018/2 (Sheldrick, 2018)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 150.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.4933 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 1.000 _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 -82.00 -33.00 1.00 13.50 -- -14.36 142.00 55.00 49 2 \w -77.00 -29.00 1.00 13.50 -- -14.36 133.00 170.46 48 3 \w -47.00 52.00 1.00 13.50 -- -14.36 74.00 135.88 99 4 \w -12.00 91.00 1.00 13.50 -- 14.52 37.00-150.00 103 5 \w -59.00 44.00 1.00 13.50 -- 14.52 -57.00 -90.00 103 6 \w 0.00 87.00 1.00 13.50 -- 14.52 37.00 -60.00 87 7 \w -11.00 56.00 1.00 13.50 -- 14.52 -99.00 30.00 67 8 \w -19.00 93.00 1.00 13.50 -- 14.52 77.00 30.00 112 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0188968000 _diffrn_orient_matrix_UB_12 0.0195018000 _diffrn_orient_matrix_UB_13 0.0424039000 _diffrn_orient_matrix_UB_21 -0.0095444000 _diffrn_orient_matrix_UB_22 -0.0559131000 _diffrn_orient_matrix_UB_23 0.0220923000 _diffrn_orient_matrix_UB_31 0.0881011000 _diffrn_orient_matrix_UB_32 -0.0039618000 _diffrn_orient_matrix_UB_33 0.0024352000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0273 _diffrn_reflns_av_unetI/netI 0.0251 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 24625 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.500 _diffrn_reflns_theta_min 2.342 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.910 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.91420 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 656 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.511 _refine_diff_density_min -0.543 _refine_diff_density_rms 0.063 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.217 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 438 _refine_ls_number_reflns 6572 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.217 _refine_ls_R_factor_all 0.0399 _refine_ls_R_factor_gt 0.0374 _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^)+(0.0085P)^2^+2.1131P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0863 _refine_ls_wR_factor_ref 0.0874 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6213 _reflns_number_total 6572 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0ra03192e3.cif _cod_data_source_block 10a _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_crystal_density_meas' value 'not measured' was changed to '?' -- the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas Adding full bibliography for 7240517--7240533.cif. ; _cod_original_formula_sum 'C31 H34 N6 O4.50 Zn' _cod_database_code 7240529 _shelx_shelxl_version_number 2018/3 _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. ; _shelx_estimated_absorpt_t_max 0.914 _shelx_estimated_absorpt_t_min 0.772 _shelx_res_file ; TITL mob522_a.res in P-1 mob522.res created by SHELXL-2018/3 at 11:23:34 on 16-Dec-2019 CELL 0.71073 7.9798 12.1068 15.2595 81.018 78.984 86.388 ZERR 2 0.0002 0.0003 0.0004 0.002 0.002 0.002 LATT 1 SFAC C H N O Zn UNIT 62 68 12 9 2 EQIV $1 1+X,+Y,+Z EQIV $2 2-X,1-Y,-Z L.S. 10 PLAN 10 SIZE 0.3 0.3 0.1 HTAB N32 O22_$1 HTAB O5 N52 HTAB O5 O12_$2 MORE -1 bond $h htab LIST 6 fmap 2 acta MERG 2 SHEL 30 0.7696 REM REM REM WGHT 0.008500 2.113100 FVAR 4.99190 ZN1 5 0.638004 0.373109 0.258234 11.00000 0.01523 0.01611 = 0.01800 -0.00200 -0.00409 -0.00122 O11 4 0.722260 0.526870 0.206626 11.00000 0.02631 0.02013 = 0.01873 0.00021 -0.00595 -0.00450 O12 4 0.799306 0.686117 0.242270 11.00000 0.03249 0.01747 = 0.03075 -0.00072 -0.00089 -0.00613 O21 4 0.384959 0.354977 0.304214 11.00000 0.01795 0.02864 = 0.01974 -0.00500 -0.00213 -0.00252 O22 4 0.131776 0.351689 0.263036 11.00000 0.01493 0.02948 = 0.02705 -0.00295 0.00007 -0.00316 N1 3 0.678414 0.432144 0.378718 11.00000 0.01482 0.01750 = 0.01793 -0.00234 -0.00314 0.00141 N2 3 0.548161 0.363135 0.134036 11.00000 0.01365 0.01486 = 0.02007 -0.00266 -0.00334 -0.00021 N31 3 0.907721 0.057964 0.262669 11.00000 0.02097 0.01631 = 0.02798 -0.00372 -0.00550 -0.00058 N4 3 0.257543 0.049563 0.486648 11.00000 0.04355 0.06426 = 0.07872 -0.01015 -0.01218 0.01097 N32 3 0.804706 0.242753 0.259388 11.00000 0.01517 0.01750 = 0.02345 -0.00259 -0.00455 -0.00266 C11 1 0.743797 0.532438 0.359141 11.00000 0.01436 0.01798 = 0.01966 -0.00426 -0.00136 0.00064 C12 1 0.796477 0.587774 0.423219 11.00000 0.02541 0.02175 = 0.02518 -0.00778 -0.00314 -0.00343 AFIX 43 H12 2 0.842489 0.658311 0.406471 11.00000 -1.20000 AFIX 0 C13 1 0.778726 0.535795 0.510783 11.00000 0.02883 0.03095 = 0.02332 -0.01216 -0.00670 0.00222 AFIX 43 H13 2 0.813537 0.570465 0.554232 11.00000 -1.20000 AFIX 0 C14 1 0.707443 0.429628 0.534323 11.00000 0.02072 0.02540 = 0.01936 -0.00479 -0.00311 0.00786 C15 1 0.681585 0.371727 0.623993 11.00000 0.03217 0.03521 = 0.01826 -0.00422 -0.00560 0.01223 AFIX 43 H15 2 0.714271 0.403598 0.669509 11.00000 -1.20000 AFIX 0 C16 1 0.609199 0.269803 0.643695 11.00000 0.03328 0.03718 = 0.01933 0.00508 0.00070 0.01343 AFIX 43 H16 2 0.592459 0.232743 0.702684 11.00000 -1.20000 AFIX 0 C17 1 0.559376 0.219882 0.575605 11.00000 0.02797 0.02569 = 0.03158 0.00717 0.00108 0.00255 AFIX 43 H17 2 0.510945 0.149963 0.590024 11.00000 -1.20000 AFIX 0 C18 1 0.581594 0.273334 0.488448 11.00000 0.02494 0.02256 = 0.02606 0.00084 -0.00392 -0.00068 AFIX 43 H18 2 0.547326 0.240173 0.444034 11.00000 -1.20000 AFIX 0 C19 1 0.656771 0.379057 0.466215 11.00000 0.01565 0.02098 = 0.01914 -0.00120 -0.00197 0.00423 C110 1 0.757557 0.588000 0.261348 11.00000 0.01550 0.01978 = 0.02161 -0.00263 -0.00033 -0.00040 C21 1 0.379874 0.353983 0.148974 11.00000 0.01466 0.01474 = 0.01970 -0.00149 -0.00263 -0.00037 C22 1 0.288443 0.346364 0.080259 11.00000 0.01480 0.02618 = 0.02513 -0.00181 -0.00542 -0.00300 AFIX 43 H22 2 0.170457 0.339952 0.093544 11.00000 -1.20000 AFIX 0 C23 1 0.374762 0.348480 -0.006236 11.00000 0.01948 0.02984 = 0.02214 -0.00244 -0.00893 -0.00418 AFIX 43 H23 2 0.316152 0.342843 -0.052414 11.00000 -1.20000 AFIX 0 C24 1 0.553996 0.359306 -0.025181 11.00000 0.01886 0.01825 = 0.02040 -0.00284 -0.00331 -0.00097 C25 1 0.651230 0.364311 -0.113354 11.00000 0.02645 0.02884 = 0.01978 -0.00626 -0.00539 -0.00185 AFIX 43 H25 2 0.597409 0.358919 -0.161394 11.00000 -1.20000 AFIX 0 C26 1 0.823520 0.377001 -0.128465 11.00000 0.02601 0.02842 = 0.02073 -0.00493 0.00272 -0.00053 AFIX 43 H26 2 0.886564 0.379767 -0.186660 11.00000 -1.20000 AFIX 0 C27 1 0.906900 0.385988 -0.055884 11.00000 0.01610 0.02510 = 0.02973 -0.00416 -0.00107 -0.00031 AFIX 43 H27 2 1.024242 0.395299 -0.066985 11.00000 -1.20000 AFIX 0 C28 1 0.816532 0.381108 0.030402 11.00000 0.01672 0.02047 = 0.02286 -0.00317 -0.00314 0.00065 AFIX 43 H28 2 0.872403 0.386978 0.077587 11.00000 -1.20000 AFIX 0 C29 1 0.637667 0.367092 0.047615 11.00000 0.01682 0.01438 = 0.01991 -0.00286 -0.00376 0.00005 C210 1 0.289598 0.353760 0.246184 11.00000 0.01668 0.01367 = 0.02136 -0.00152 -0.00184 -0.00189 C31 1 1.088691 0.085053 0.239872 11.00000 0.02009 0.02143 = 0.03220 -0.00374 -0.00294 0.00046 AFIX 23 H31A 2 1.118834 0.127527 0.283156 11.00000 -1.20000 H31B 2 1.115845 0.127686 0.179932 11.00000 -1.20000 AFIX 0 C32 1 1.179959 -0.027819 0.243979 11.00000 0.02843 0.02461 = 0.17474 -0.01602 -0.00298 0.00888 AFIX 23 H32A 2 1.261771 -0.031461 0.188534 11.00000 -1.20000 H32B 2 1.241630 -0.039251 0.293802 11.00000 -1.20000 AFIX 0 C33 1 1.061527 -0.110684 0.255710 11.00000 0.03475 0.02328 = 0.17420 -0.01650 -0.01956 0.00656 AFIX 23 H33A 2 1.078888 -0.166881 0.306199 11.00000 -1.20000 H33B 2 1.078838 -0.146785 0.202072 11.00000 -1.20000 AFIX 0 C34 1 0.884756 -0.063739 0.272800 11.00000 0.03084 0.01509 = 0.04379 -0.00441 -0.01008 -0.00013 AFIX 23 H34A 2 0.820416 -0.081521 0.229236 11.00000 -1.20000 H34B 2 0.826131 -0.092058 0.333126 11.00000 -1.20000 AFIX 0 C35 1 0.780598 0.135692 0.268904 11.00000 0.01912 0.02013 = 0.02121 -0.00287 -0.00582 -0.00040 C36 1 0.601799 0.094656 0.289804 11.00000 0.02052 0.01953 = 0.05978 -0.00345 -0.00994 -0.00338 AFIX 137 H36A 2 0.522459 0.157267 0.284640 11.00000 -1.50000 H36B 2 0.579344 0.054894 0.350166 11.00000 -1.50000 H36C 2 0.589168 0.045543 0.247982 11.00000 -1.50000 AFIX 0 C41 1 0.150487 0.113718 0.476035 11.00000 0.03358 0.04207 = 0.03427 -0.00677 -0.00236 -0.00572 C42 1 0.013091 0.194941 0.463039 11.00000 0.03761 0.03953 = 0.03278 -0.00373 -0.00573 -0.00083 AFIX 137 H42A 2 -0.019901 0.230986 0.515777 11.00000 -1.50000 H42B 2 -0.082942 0.157800 0.453098 11.00000 -1.50000 H42C 2 0.050984 0.249912 0.411621 11.00000 -1.50000 AFIX 6 PART -1 O5 4 1.400248 0.148961 -0.152381 10.50000 0.03549 0.03929 = 0.03703 -0.00007 -0.00505 -0.00366 H5A 2 1.348477 0.197550 -0.185121 10.50000 -1.50000 H5B 2 1.329659 0.120580 -0.106601 10.50000 -1.50000 AFIX 0 N51 3 0.875353 -0.006798 0.026145 10.50000 0.03181 0.01793 = 0.03456 -0.00396 -0.00558 0.00229 C51 1 0.753704 0.086446 0.038140 10.50000 0.03333 0.01973 = 0.03375 -0.00286 -0.00400 0.00380 AFIX 23 H51A 2 0.776995 0.146366 -0.012284 10.50000 -1.20000 H51B 2 0.758043 0.115391 0.093432 10.50000 -1.20000 AFIX 0 C52 1 0.580216 0.037441 0.042691 10.50000 0.03617 0.03494 = 0.05324 -0.00019 -0.01151 -0.00179 AFIX 23 H52A 2 0.491387 0.073541 0.082446 10.50000 -1.20000 H52B 2 0.550330 0.045540 -0.016740 10.50000 -1.20000 AFIX 0 C53 1 0.605404 -0.084814 0.079962 10.50000 0.03474 0.03428 = 0.04466 -0.00338 -0.00842 -0.00521 AFIX 23 H53A 2 0.525701 -0.130625 0.062333 10.50000 -1.20000 H53B 2 0.590127 -0.095435 0.145298 10.50000 -1.20000 AFIX 0 C54 1 0.789938 -0.113955 0.037763 10.50000 0.03615 0.02247 = 0.03538 -0.00835 -0.00298 -0.00449 AFIX 23 H54A 2 0.841008 -0.171067 0.077558 10.50000 -1.20000 H54B 2 0.795317 -0.139792 -0.019799 10.50000 -1.20000 AFIX 0 C55 1 1.045954 0.007596 0.000378 10.50000 0.03023 0.02161 = 0.02457 -0.00106 -0.00651 0.00331 C56 1 1.154133 -0.094301 -0.020754 10.50000 0.03474 0.03072 = 0.04018 -0.00728 -0.00831 0.00403 AFIX 137 H56A 2 1.269512 -0.073042 -0.045177 10.50000 -1.50000 H56B 2 1.109948 -0.128175 -0.064082 10.50000 -1.50000 H56C 2 1.152102 -0.146833 0.033486 10.50000 -1.50000 AFIX 0 N52 3 1.119767 0.100615 -0.006973 10.50000 0.03397 0.02959 = 0.03950 -0.00103 -0.00457 -0.00414 H52 2 1.036650 0.159580 0.007087 10.50000 0.03667 PART 0 H32 2 0.908935 0.258477 0.251456 11.00000 0.02512 HKLF 4 REM mob522_a.res in P-1 REM wR2 = 0.0874, GooF = S = 1.217, Restrained GooF = 1.217 for all data REM R1 = 0.0374 for 6213 Fo > 4sig(Fo) and 0.0399 for all 6572 data REM 438 parameters refined using 0 restraints END WGHT 0.0087 2.1115 REM Instructions for potential hydrogen bonds EQIV $3 -x+2, -y, -z HTAB C34 O5_$3 HTAB C36 O21 HTAB C42 O22 HTAB N32 O22_$1 REM Highest difference peak 0.511, deepest hole -0.543, 1-sigma level 0.063 Q1 1 1.3078 -0.0213 0.2289 11.00000 0.05 0.51 Q2 1 1.0793 -0.1946 0.2646 11.00000 0.05 0.47 Q3 1 1.1690 -0.0180 0.2041 11.00000 0.05 0.38 Q4 1 1.1556 -0.0278 0.2757 11.00000 0.05 0.38 Q5 1 1.0605 -0.0987 0.2985 11.00000 0.05 0.36 Q6 1 1.1163 -0.0707 0.1569 11.00000 0.05 0.35 Q7 1 1.1449 -0.0670 0.3431 11.00000 0.05 0.35 Q8 1 1.1226 -0.0623 0.2192 11.00000 0.05 0.34 Q9 1 0.3345 0.3610 0.1948 11.00000 0.05 0.34 Q10 1 0.6762 0.4005 0.5801 11.00000 0.05 0.32 ; _shelx_res_checksum 12909 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -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 _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.63800(3) 0.37311(2) 0.25823(2) 0.01634(7) Uani 1 1 d . . . . . O11 O 0.7223(2) 0.52687(13) 0.20663(11) 0.0217(3) Uani 1 1 d . . . . . O12 O 0.7993(2) 0.68612(13) 0.24227(12) 0.0276(4) Uani 1 1 d . . . . . O21 O 0.38496(19) 0.35498(14) 0.30421(11) 0.0221(3) Uani 1 1 d . . . . . O22 O 0.13178(19) 0.35169(14) 0.26304(11) 0.0244(4) Uani 1 1 d . . . . . N1 N 0.6784(2) 0.43214(15) 0.37872(12) 0.0168(4) Uani 1 1 d . . . . . N2 N 0.5482(2) 0.36314(14) 0.13404(12) 0.0162(4) Uani 1 1 d . . . . . N31 N 0.9077(2) 0.05796(15) 0.26267(14) 0.0216(4) Uani 1 1 d . . . . . N4 N 0.2575(4) 0.0496(3) 0.4866(2) 0.0626(8) Uani 1 1 d . . . . . N32 N 0.8047(2) 0.24275(15) 0.25939(13) 0.0185(4) Uani 1 1 d . . . . . C11 C 0.7438(3) 0.53244(18) 0.35914(15) 0.0175(4) Uani 1 1 d . . . . . C12 C 0.7965(3) 0.5878(2) 0.42322(16) 0.0237(5) Uani 1 1 d . . . . . H12 H 0.842489 0.658311 0.406471 0.028 Uiso 1 1 calc R . . . . C13 C 0.7787(3) 0.5358(2) 0.51078(17) 0.0267(5) Uani 1 1 d . . . . . H13 H 0.813537 0.570465 0.554232 0.032 Uiso 1 1 calc R . . . . C14 C 0.7074(3) 0.4296(2) 0.53432(15) 0.0221(5) Uani 1 1 d . . . . . C15 C 0.6816(3) 0.3717(2) 0.62399(16) 0.0290(5) Uani 1 1 d . . . . . H15 H 0.714271 0.403598 0.669509 0.035 Uiso 1 1 calc R . . . . C16 C 0.6092(3) 0.2698(2) 0.64369(17) 0.0323(6) Uani 1 1 d . . . . . H16 H 0.592459 0.232743 0.702684 0.039 Uiso 1 1 calc R . . . . C17 C 0.5594(3) 0.2199(2) 0.57560(18) 0.0307(6) Uani 1 1 d . . . . . H17 H 0.510945 0.149963 0.590024 0.037 Uiso 1 1 calc R . . . . C18 C 0.5816(3) 0.2733(2) 0.48845(17) 0.0251(5) Uani 1 1 d . . . . . H18 H 0.547326 0.240173 0.444034 0.030 Uiso 1 1 calc R . . . . C19 C 0.6568(3) 0.37906(18) 0.46622(15) 0.0192(4) Uani 1 1 d . . . . . C110 C 0.7576(3) 0.58800(18) 0.26135(15) 0.0194(4) Uani 1 1 d . . . . . C21 C 0.3799(3) 0.35398(17) 0.14897(15) 0.0166(4) Uani 1 1 d . . . . . C22 C 0.2884(3) 0.34636(19) 0.08026(16) 0.0219(5) Uani 1 1 d . . . . . H22 H 0.170457 0.339952 0.093544 0.026 Uiso 1 1 calc R . . . . C23 C 0.3748(3) 0.3485(2) -0.00624(16) 0.0231(5) Uani 1 1 d . . . . . H23 H 0.316152 0.342843 -0.052414 0.028 Uiso 1 1 calc R . . . . C24 C 0.5540(3) 0.35931(18) -0.02518(15) 0.0192(4) Uani 1 1 d . . . . . C25 C 0.6512(3) 0.3643(2) -0.11335(16) 0.0245(5) Uani 1 1 d . . . . . H25 H 0.597409 0.358919 -0.161394 0.029 Uiso 1 1 calc R . . . . C26 C 0.8235(3) 0.3770(2) -0.12847(16) 0.0259(5) Uani 1 1 d . . . . . H26 H 0.886564 0.379767 -0.186660 0.031 Uiso 1 1 calc R . . . . C27 C 0.9069(3) 0.3860(2) -0.05588(17) 0.0241(5) Uani 1 1 d . . . . . H27 H 1.024242 0.395299 -0.066985 0.029 Uiso 1 1 calc R . . . . C28 C 0.8165(3) 0.38111(18) 0.03040(16) 0.0201(4) Uani 1 1 d . . . . . H28 H 0.872403 0.386978 0.077587 0.024 Uiso 1 1 calc R . . . . C29 C 0.6377(3) 0.36709(17) 0.04761(15) 0.0170(4) Uani 1 1 d . . . . . C210 C 0.2896(3) 0.35376(17) 0.24618(15) 0.0175(4) Uani 1 1 d . . . . . C31 C 1.0887(3) 0.0851(2) 0.23987(17) 0.0249(5) Uani 1 1 d . . . . . H31A H 1.118834 0.127527 0.283156 0.030 Uiso 1 1 calc R . . . . H31B H 1.115845 0.127686 0.179932 0.030 Uiso 1 1 calc R . . . . C32 C 1.1800(4) -0.0278(3) 0.2440(4) 0.0783(15) Uani 1 1 d . . . . . H32A H 1.261771 -0.031461 0.188534 0.094 Uiso 1 1 calc R . . . . H32B H 1.241630 -0.039251 0.293802 0.094 Uiso 1 1 calc R . . . . C33 C 1.0615(4) -0.1107(3) 0.2557(4) 0.0775(15) Uani 1 1 d . . . . . H33A H 1.078888 -0.166881 0.306199 0.093 Uiso 1 1 calc R . . . . H33B H 1.078838 -0.146785 0.202072 0.093 Uiso 1 1 calc R . . . . C34 C 0.8848(3) -0.06374(19) 0.2728(2) 0.0295(5) Uani 1 1 d . . . . . H34A H 0.820416 -0.081521 0.229236 0.035 Uiso 1 1 calc R . . . . H34B H 0.826131 -0.092058 0.333126 0.035 Uiso 1 1 calc R . . . . C35 C 0.7806(3) 0.13569(19) 0.26890(15) 0.0199(4) Uani 1 1 d . . . . . C36 C 0.6018(3) 0.0947(2) 0.2898(2) 0.0331(6) Uani 1 1 d . . . . . H36A H 0.522459 0.157267 0.284640 0.050 Uiso 1 1 calc GR . . . . H36B H 0.579344 0.054894 0.350166 0.050 Uiso 1 1 calc GR . . . . H36C H 0.589168 0.045543 0.247982 0.050 Uiso 1 1 calc GR . . . . C41 C 0.1505(4) 0.1137(3) 0.4760(2) 0.0368(6) Uani 1 1 d . . . . . C42 C 0.0131(4) 0.1949(2) 0.4630(2) 0.0369(6) Uani 1 1 d . . . . . H42A H -0.019901 0.230986 0.515777 0.055 Uiso 1 1 calc GR . . . . H42B H -0.082942 0.157800 0.453098 0.055 Uiso 1 1 calc GR . . . . H42C H 0.050984 0.249912 0.411621 0.055 Uiso 1 1 calc GR . . . . O5 O 1.4002(5) 0.1490(4) -0.1524(3) 0.0380(9) Uani 0.5 1 d . . P A -1 H5A H 1.348477 0.197550 -0.185121 0.057 Uiso 0.5 1 d G . P A -1 H5B H 1.329659 0.120580 -0.106601 0.057 Uiso 0.5 1 d G . P A -1 N51 N 0.8754(7) -0.0068(5) 0.0261(4) 0.0283(13) Uani 0.5 1 d . . P B -1 C51 C 0.7537(8) 0.0864(5) 0.0381(5) 0.0295(12) Uani 0.5 1 d . . P B -1 H51A H 0.776995 0.146366 -0.012284 0.035 Uiso 0.5 1 calc R . P B -1 H51B H 0.758043 0.115391 0.093432 0.035 Uiso 0.5 1 calc R . P B -1 C52 C 0.5802(8) 0.0374(5) 0.0427(5) 0.0417(14) Uani 0.5 1 d . . P B -1 H52A H 0.491387 0.073541 0.082446 0.050 Uiso 0.5 1 calc R . P B -1 H52B H 0.550330 0.045540 -0.016740 0.050 Uiso 0.5 1 calc R . P B -1 C53 C 0.6054(7) -0.0848(5) 0.0800(4) 0.0378(13) Uani 0.5 1 d . . P B -1 H53A H 0.525701 -0.130625 0.062333 0.045 Uiso 0.5 1 calc R . P B -1 H53B H 0.590127 -0.095435 0.145298 0.045 Uiso 0.5 1 calc R . P B -1 C54 C 0.7899(8) -0.1140(5) 0.0378(4) 0.0312(12) Uani 0.5 1 d . . P B -1 H54A H 0.841008 -0.171067 0.077558 0.037 Uiso 0.5 1 calc R . P B -1 H54B H 0.795317 -0.139792 -0.019799 0.037 Uiso 0.5 1 calc R . P B -1 C55 C 1.0460(8) 0.0076(6) 0.0004(5) 0.0257(17) Uani 0.5 1 d . . P B -1 C56 C 1.1541(9) -0.0943(5) -0.0208(5) 0.0350(13) Uani 0.5 1 d . . P B -1 H56A H 1.269512 -0.073042 -0.045177 0.053 Uiso 0.5 1 calc GR . P B -1 H56B H 1.109948 -0.128175 -0.064082 0.053 Uiso 0.5 1 calc GR . P B -1 H56C H 1.152102 -0.146833 0.033486 0.053 Uiso 0.5 1 calc GR . P B -1 N52 N 1.1198(8) 0.1006(4) -0.0070(4) 0.0350(11) Uani 0.5 1 d . . P B -1 H52 H 1.037(8) 0.160(5) 0.007(4) 0.037(16) Uiso 0.5 1 d . . P C -1 H32 H 0.909(4) 0.258(2) 0.2515(18) 0.025(7) 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 Zn1 0.01523(12) 0.01611(12) 0.01800(13) -0.00200(9) -0.00409(9) -0.00122(9) O11 0.0263(8) 0.0201(8) 0.0187(8) 0.0002(6) -0.0060(6) -0.0045(6) O12 0.0325(9) 0.0175(8) 0.0307(9) -0.0007(7) -0.0009(7) -0.0061(7) O21 0.0180(7) 0.0286(9) 0.0197(8) -0.0050(7) -0.0021(6) -0.0025(6) O22 0.0149(7) 0.0295(9) 0.0271(9) -0.0030(7) 0.0001(6) -0.0032(6) N1 0.0148(8) 0.0175(9) 0.0179(9) -0.0023(7) -0.0031(7) 0.0014(7) N2 0.0136(8) 0.0149(8) 0.0201(9) -0.0027(7) -0.0033(7) -0.0002(7) N31 0.0210(9) 0.0163(9) 0.0280(10) -0.0037(8) -0.0055(8) -0.0006(7) N4 0.0436(16) 0.064(2) 0.079(2) -0.0102(17) -0.0122(15) 0.0110(15) N32 0.0152(9) 0.0175(9) 0.0235(10) -0.0026(7) -0.0046(7) -0.0027(7) C11 0.0144(9) 0.0180(10) 0.0197(11) -0.0043(8) -0.0014(8) 0.0006(8) C12 0.0254(11) 0.0218(11) 0.0252(12) -0.0078(9) -0.0031(9) -0.0034(9) C13 0.0288(12) 0.0310(13) 0.0233(12) -0.0122(10) -0.0067(10) 0.0022(10) C14 0.0207(11) 0.0254(11) 0.0194(11) -0.0048(9) -0.0031(9) 0.0079(9) C15 0.0322(13) 0.0352(14) 0.0183(11) -0.0042(10) -0.0056(10) 0.0122(11) C16 0.0333(13) 0.0372(14) 0.0193(12) 0.0051(10) 0.0007(10) 0.0134(11) C17 0.0280(12) 0.0257(12) 0.0316(14) 0.0072(10) 0.0011(10) 0.0025(10) C18 0.0249(11) 0.0226(11) 0.0261(12) 0.0008(9) -0.0039(9) -0.0007(9) C19 0.0157(10) 0.0210(11) 0.0191(11) -0.0012(8) -0.0020(8) 0.0042(8) C110 0.0155(10) 0.0198(10) 0.0216(11) -0.0026(8) -0.0003(8) -0.0004(8) C21 0.0147(9) 0.0147(9) 0.0197(11) -0.0015(8) -0.0026(8) -0.0004(8) C22 0.0148(10) 0.0262(12) 0.0251(12) -0.0018(9) -0.0054(9) -0.0030(8) C23 0.0195(11) 0.0298(12) 0.0221(11) -0.0024(9) -0.0089(9) -0.0042(9) C24 0.0189(10) 0.0182(10) 0.0204(11) -0.0028(8) -0.0033(8) -0.0010(8) C25 0.0264(12) 0.0288(12) 0.0198(11) -0.0063(9) -0.0054(9) -0.0018(10) C26 0.0260(12) 0.0284(12) 0.0207(11) -0.0049(9) 0.0027(9) -0.0005(10) C27 0.0161(10) 0.0251(12) 0.0297(13) -0.0042(10) -0.0011(9) -0.0003(9) C28 0.0167(10) 0.0205(11) 0.0229(11) -0.0032(9) -0.0031(8) 0.0007(8) C29 0.0168(10) 0.0144(9) 0.0199(11) -0.0029(8) -0.0038(8) 0.0000(8) C210 0.0167(10) 0.0137(9) 0.0214(11) -0.0015(8) -0.0018(8) -0.0019(8) C31 0.0201(11) 0.0214(11) 0.0322(13) -0.0037(10) -0.0029(9) 0.0005(9) C32 0.0284(16) 0.0246(16) 0.175(5) -0.016(2) -0.003(2) 0.0089(13) C33 0.0348(17) 0.0233(15) 0.174(5) -0.017(2) -0.020(2) 0.0066(13) C34 0.0308(13) 0.0151(11) 0.0438(15) -0.0044(10) -0.0101(11) -0.0001(9) C35 0.0191(10) 0.0201(11) 0.0212(11) -0.0029(9) -0.0058(9) -0.0004(8) C36 0.0205(12) 0.0195(12) 0.0598(18) -0.0035(11) -0.0099(12) -0.0034(9) C41 0.0336(14) 0.0421(16) 0.0343(15) -0.0068(12) -0.0024(12) -0.0057(12) C42 0.0376(15) 0.0395(15) 0.0328(15) -0.0037(12) -0.0057(12) -0.0008(12) O5 0.035(2) 0.039(2) 0.037(2) -0.0001(18) -0.0050(17) -0.0037(17) N51 0.032(4) 0.018(2) 0.035(3) -0.004(2) -0.006(2) 0.002(2) C51 0.033(3) 0.020(3) 0.034(3) -0.003(2) -0.004(3) 0.004(3) C52 0.036(3) 0.035(3) 0.053(4) 0.000(3) -0.012(3) -0.002(2) C53 0.035(3) 0.034(3) 0.045(3) -0.003(3) -0.008(3) -0.005(2) C54 0.036(3) 0.022(3) 0.035(3) -0.008(2) -0.003(3) -0.004(3) C55 0.030(6) 0.022(3) 0.025(3) -0.001(2) -0.007(4) 0.003(4) C56 0.035(3) 0.031(3) 0.040(4) -0.007(3) -0.008(3) 0.004(3) N52 0.034(3) 0.030(3) 0.039(3) -0.001(2) -0.005(2) -0.004(2) 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' Zn Zn 0.2839 1.4301 '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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 Zn1 O21 118.55(7) . . ? O11 Zn1 N1 79.35(7) . . ? O11 Zn1 N2 89.67(6) . . ? O21 Zn1 N1 93.47(6) . . ? O21 Zn1 N2 78.75(6) . . ? N1 Zn1 N2 161.59(7) . . ? N32 Zn1 O11 119.33(7) . . ? N32 Zn1 O21 122.10(7) . . ? N32 Zn1 N1 98.28(7) . . ? N32 Zn1 N2 99.98(7) . . ? C110 O11 Zn1 117.63(14) . . ? C210 O21 Zn1 117.73(14) . . ? C11 N1 Zn1 110.86(14) . . ? C11 N1 C19 118.97(19) . . ? C19 N1 Zn1 130.01(15) . . ? C21 N2 Zn1 111.20(14) . . ? C21 N2 C29 118.95(18) . . ? C29 N2 Zn1 129.83(14) . . ? C31 N31 C34 111.61(18) . . ? C35 N31 C31 123.30(19) . . ? C35 N31 C34 125.02(19) . . ? Zn1 N32 H32 115.9(19) . . ? C35 N32 Zn1 130.70(16) . . ? C35 N32 H32 113.4(19) . . ? N1 C11 C12 123.4(2) . . ? N1 C11 C110 115.96(19) . . ? C12 C11 C110 120.6(2) . . ? C11 C12 H12 120.6 . . ? C13 C12 C11 118.8(2) . . ? C13 C12 H12 120.6 . . ? C12 C13 H13 120.3 . . ? C12 C13 C14 119.4(2) . . ? C14 C13 H13 120.3 . . ? C13 C14 C15 122.6(2) . . ? C13 C14 C19 118.7(2) . . ? C19 C14 C15 118.7(2) . . ? C14 C15 H15 119.8 . . ? C16 C15 C14 120.4(2) . . ? C16 C15 H15 119.8 . . ? C15 C16 H16 119.7 . . ? C15 C16 C17 120.7(2) . . ? C17 C16 H16 119.7 . . ? C16 C17 H17 119.7 . . ? C18 C17 C16 120.6(2) . . ? C18 C17 H17 119.7 . . ? C17 C18 H18 120.1 . . ? C17 C18 C19 119.8(2) . . ? C19 C18 H18 120.1 . . ? N1 C19 C14 120.7(2) . . ? N1 C19 C18 119.4(2) . . ? C18 C19 C14 119.9(2) . . ? O11 C110 C11 115.79(19) . . ? O12 C110 O11 126.1(2) . . ? O12 C110 C11 118.1(2) . . ? N2 C21 C22 123.0(2) . . ? N2 C21 C210 115.65(18) . . ? C22 C21 C210 121.30(19) . . ? C21 C22 H22 120.4 . . ? C23 C22 C21 119.2(2) . . ? C23 C22 H22 120.4 . . ? C22 C23 H23 120.2 . . ? C22 C23 C24 119.5(2) . . ? C24 C23 H23 120.2 . . ? C23 C24 C29 118.1(2) . . ? C25 C24 C23 122.6(2) . . ? C25 C24 C29 119.3(2) . . ? C24 C25 H25 119.8 . . ? C26 C25 C24 120.4(2) . . ? C26 C25 H25 119.8 . . ? C25 C26 H26 119.8 . . ? C25 C26 C27 120.3(2) . . ? C27 C26 H26 119.8 . . ? C26 C27 H27 119.6 . . ? C28 C27 C26 120.7(2) . . ? C28 C27 H27 119.6 . . ? C27 C28 H28 120.1 . . ? C27 C28 C29 119.8(2) . . ? C29 C28 H28 120.1 . . ? N2 C29 C24 121.14(19) . . ? N2 C29 C28 119.42(19) . . ? C28 C29 C24 119.4(2) . . ? O21 C210 C21 116.38(18) . . ? O22 C210 O21 125.3(2) . . ? O22 C210 C21 118.31(19) . . ? N31 C31 H31A 111.0 . . ? N31 C31 H31B 111.0 . . ? N31 C31 C32 103.6(2) . . ? H31A C31 H31B 109.0 . . ? C32 C31 H31A 111.0 . . ? C32 C31 H31B 111.0 . . ? C31 C32 H32A 109.8 . . ? C31 C32 H32B 109.8 . . ? H32A C32 H32B 108.2 . . ? C33 C32 C31 109.4(3) . . ? C33 C32 H32A 109.8 . . ? C33 C32 H32B 109.8 . . ? C32 C33 H33A 109.4 . . ? C32 C33 H33B 109.4 . . ? C32 C33 C34 111.3(3) . . ? H33A C33 H33B 108.0 . . ? C34 C33 H33A 109.4 . . ? C34 C33 H33B 109.4 . . ? N31 C34 C33 103.5(2) . . ? N31 C34 H34A 111.1 . . ? N31 C34 H34B 111.1 . . ? C33 C34 H34A 111.1 . . ? C33 C34 H34B 111.1 . . ? H34A C34 H34B 109.0 . . ? N31 C35 C36 116.9(2) . . ? N32 C35 N31 123.7(2) . . ? N32 C35 C36 119.4(2) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36B 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N4 C41 C42 179.5(4) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42B 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? H5A O5 H5B 109.5 . . ? C51 N51 C54 112.0(5) . . ? C55 N51 C51 122.3(5) . . ? C55 N51 C54 125.5(5) . . ? N51 C51 H51A 110.8 . . ? N51 C51 H51B 110.8 . . ? N51 C51 C52 104.6(5) . . ? H51A C51 H51B 108.9 . . ? C52 C51 H51A 110.8 . . ? C52 C51 H51B 110.8 . . ? C51 C52 H52A 111.0 . . ? C51 C52 H52B 111.0 . . ? H52A C52 H52B 109.0 . . ? C53 C52 C51 103.6(5) . . ? C53 C52 H52A 111.0 . . ? C53 C52 H52B 111.0 . . ? C52 C53 H53A 111.0 . . ? C52 C53 H53B 111.0 . . ? C52 C53 C54 104.0(5) . . ? H53A C53 H53B 109.0 . . ? C54 C53 H53A 111.0 . . ? C54 C53 H53B 111.0 . . ? N51 C54 C53 103.1(5) . . ? N51 C54 H54A 111.2 . . ? N51 C54 H54B 111.2 . . ? C53 C54 H54A 111.2 . . ? C53 C54 H54B 111.2 . . ? H54A C54 H54B 109.1 . . ? N51 C55 C56 116.5(5) . . ? N52 C55 N51 125.0(6) . . ? N52 C55 C56 118.5(6) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56B 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C55 N52 H52 110(4) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O11 2.0088(16) . ? Zn1 O21 2.0209(15) . ? Zn1 N1 2.1589(18) . ? Zn1 N2 2.1730(18) . ? Zn1 N32 1.9991(19) . ? O11 C110 1.278(3) . ? O12 C110 1.229(3) . ? O21 C210 1.275(3) . ? O22 C210 1.237(3) . ? N1 C11 1.320(3) . ? N1 C19 1.372(3) . ? N2 C21 1.327(3) . ? N2 C29 1.370(3) . ? N31 C31 1.465(3) . ? N31 C34 1.477(3) . ? N31 C35 1.340(3) . ? N4 C41 1.135(4) . ? N32 C35 1.304(3) . ? N32 H32 0.85(3) . ? C11 C12 1.407(3) . ? C11 C110 1.525(3) . ? C12 H12 0.9300 . ? C12 C13 1.370(3) . ? C13 H13 0.9300 . ? C13 C14 1.405(3) . ? C14 C15 1.420(3) . ? C14 C19 1.417(3) . ? C15 H15 0.9300 . ? C15 C16 1.362(4) . ? C16 H16 0.9300 . ? C16 C17 1.410(4) . ? C17 H17 0.9300 . ? C17 C18 1.369(3) . ? C18 H18 0.9300 . ? C18 C19 1.413(3) . ? C21 C22 1.404(3) . ? C21 C210 1.520(3) . ? C22 H22 0.9300 . ? C22 C23 1.364(3) . ? C23 H23 0.9300 . ? C23 C24 1.414(3) . ? C24 C25 1.413(3) . ? C24 C29 1.419(3) . ? C25 H25 0.9300 . ? C25 C26 1.364(3) . ? C26 H26 0.9300 . ? C26 C27 1.418(3) . ? C27 H27 0.9300 . ? C27 C28 1.369(3) . ? C28 H28 0.9300 . ? C28 C29 1.417(3) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 C32 1.506(4) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 C33 1.389(5) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C33 C34 1.478(4) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.500(3) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C41 C42 1.447(4) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? O5 H5A 0.8502 . ? O5 H5B 0.8500 . ? N51 C51 1.452(8) . ? N51 C54 1.474(8) . ? N51 C55 1.357(9) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C51 C52 1.526(8) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C52 C53 1.516(8) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C53 C54 1.533(8) . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C55 C56 1.502(8) . ? C55 N52 1.283(8) . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? N52 H52 0.96(6) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O5 H5A O12 0.85 1.98 2.825(4) 170.3 2_765 yes O5 H5B N52 0.85 2.03 2.853(7) 161.4 . yes N32 H32 O22 0.85(3) 2.21(3) 3.011(2) 157(3) 1_655 yes