#------------------------------------------------------------------------------ #$Date: 2024-04-17 03:38:20 +0300 (Wed, 17 Apr 2024) $ #$Revision: 291242 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/06/31/7063171.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_7063171 loop_ _publ_author_name 'Podjed, Nina' 'Ko\ 2\s(I)' _cod_data_source_file d4nj00235k2.cif _cod_data_source_block 21a _cod_database_code 7063171 _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 0.978 _shelx_estimated_absorpt_t_min 0.863 _reflns_odcompleteness_completeness 99.90 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 27.50 _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 Secondary CH2 refined with riding coordinates: C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C41(H41A, H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B) 2.b Aromatic/amide H refined with riding coordinates: C11(H11), C12(H12), C13(H13), C14(H14), C16(H16), C17(H17), C31(H31), C32(H32), C33(H33), C34(H34), C36(H36), C37(H37) 2.c Idealised Me refined as rotating group: C26(H26A,H26B,H26C), C46(H46A,H46B,H46C), C52(H52A,H52B,H52C), C62(H62A,H62B, H62C) ; _shelx_res_file ; TITL moc490_a.res in P-1 moc490.res created by SHELXL-2018/3 at 13:50:56 on 05-May-2022 REM Old TITL Moc490 in P-1 REM SHELXT solution in P-1: R1 0.098, Rweak 0.005, Alpha 0.037 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C36 N8 O6 Zn CELL 0.71073 10.5815 12.3264 13.5644 86.699 87.372 82.306 ZERR 2 0.0004 0.0005 0.0006 0.004 0.003 0.003 LATT 1 SFAC C H N O Zn UNIT 72 84 16 12 2 EQIV $1 +X,+Y,1+Z L.S. 10 0 0 PLAN 10 SIZE 0.2 0.1 0.03 HTAB N2 O33_$1 HTAB N4 O11 BOND list 4 fmap 2 53 acta REM REM REM WGHT 0.031600 FVAR 0.31144 ZN1 5 0.500000 0.500000 1.000000 10.50000 0.01376 0.01810 = 0.01193 -0.00132 -0.00239 -0.00286 ZN2 5 0.500000 0.500000 0.500000 10.50000 0.01333 0.01547 = 0.01224 -0.00135 -0.00199 -0.00110 O1 4 0.459518 0.441381 0.867986 11.00000 0.01460 0.02040 = 0.01243 -0.00147 -0.00281 -0.00116 O2 4 0.093923 0.165636 1.240236 11.00000 0.02931 0.03461 = 0.04100 -0.00703 0.01323 -0.01231 O3 4 0.490345 0.423616 0.369604 11.00000 0.01460 0.02127 = 0.01439 -0.00338 -0.00137 -0.00091 O4 4 0.578388 -0.022125 0.710075 11.00000 0.02816 0.02725 = 0.05821 0.01426 -0.00837 0.00390 O11 4 0.305423 0.431730 0.762600 11.00000 0.01803 0.02983 = 0.01649 -0.00800 -0.00346 -0.00358 O33 4 0.602083 0.316916 0.258892 11.00000 0.02330 0.02125 = 0.01639 -0.00550 -0.00512 0.00059 N1 3 0.293875 0.575451 0.980763 11.00000 0.01424 0.01726 = 0.01319 -0.00060 -0.00142 -0.00234 N2 3 0.437827 0.358110 1.084711 11.00000 0.01324 0.01958 = 0.01370 -0.00151 -0.00310 -0.00217 H2 2 0.496191 0.339943 1.119304 11.00000 0.01132 N3 3 0.702645 0.422756 0.473849 11.00000 0.01438 0.01476 = 0.01248 -0.00140 -0.00123 -0.00188 N4 3 0.457029 0.355548 0.590248 11.00000 0.01478 0.01559 = 0.01492 -0.00361 -0.00012 0.00057 H4 2 0.407564 0.384069 0.633923 11.00000 0.01139 N5 3 1.060724 0.055067 0.638095 11.00000 0.04514 0.06918 = 0.06239 -0.01600 0.00281 -0.01847 N6 3 0.282771 0.076939 0.860851 11.00000 0.06121 0.04907 = 0.04271 -0.00909 0.01032 -0.01324 N22 3 0.274169 0.198210 1.154913 11.00000 0.02048 0.01748 = 0.01767 -0.00251 0.00192 -0.00454 N44 3 0.453285 0.130794 0.659383 11.00000 0.01833 0.01674 = 0.02458 0.00242 -0.00538 -0.00199 C10 1 0.208990 0.641219 1.038797 11.00000 0.01550 0.01386 = 0.01415 0.00000 0.00031 -0.00160 C11 1 0.250670 0.681745 1.125065 11.00000 0.01756 0.02249 = 0.01912 -0.00363 -0.00241 -0.00123 AFIX 43 H11 2 0.335624 0.665499 1.141783 11.00000 -1.20000 AFIX 0 C12 1 0.166395 0.744739 1.183944 11.00000 0.02672 0.02349 = 0.02069 -0.00599 -0.00263 0.00011 AFIX 43 H12 2 0.194667 0.770815 1.240885 11.00000 -1.20000 AFIX 0 C13 1 0.037601 0.771085 1.160325 11.00000 0.02296 0.02142 = 0.02763 -0.00616 0.00405 0.00313 AFIX 43 H13 2 -0.018587 0.813608 1.201822 11.00000 -1.20000 AFIX 0 C14 1 -0.004864 0.734481 1.076929 11.00000 0.01584 0.02641 = 0.02896 -0.00302 -0.00117 0.00164 AFIX 43 H14 2 -0.089909 0.752986 1.061127 11.00000 -1.20000 AFIX 0 C15 1 0.079281 0.668381 1.013851 11.00000 0.01476 0.02126 = 0.02044 -0.00074 -0.00240 -0.00177 C16 1 0.041148 0.628522 0.926586 11.00000 0.01379 0.03457 = 0.02687 -0.00613 -0.00663 0.00036 AFIX 43 H16 2 -0.042727 0.646110 0.907488 11.00000 -1.20000 AFIX 0 C17 1 0.126111 0.564513 0.870079 11.00000 0.01869 0.03247 = 0.02268 -0.00910 -0.00694 -0.00076 AFIX 43 H17 2 0.101234 0.537990 0.812164 11.00000 -1.20000 AFIX 0 C18 1 0.252643 0.538703 0.900281 11.00000 0.01620 0.01907 = 0.01393 0.00025 -0.00127 -0.00422 C19 1 0.346607 0.464331 0.837645 11.00000 0.01673 0.01739 = 0.01304 0.00055 -0.00022 -0.00525 C21 1 0.326605 0.385186 1.153249 11.00000 0.01850 0.01833 = 0.01828 -0.00372 0.00021 -0.00299 AFIX 23 H21A 2 0.253427 0.415065 1.115138 11.00000 -1.20000 H21B 2 0.344733 0.441433 1.195708 11.00000 -1.20000 AFIX 0 C22 1 0.293064 0.287618 1.216918 11.00000 0.02220 0.02113 = 0.01810 -0.00260 0.00137 -0.00526 AFIX 23 H22A 2 0.361219 0.263060 1.261679 11.00000 -1.20000 H22B 2 0.215676 0.308719 1.256189 11.00000 -1.20000 AFIX 0 C23 1 0.385025 0.165564 1.090102 11.00000 0.02681 0.01989 = 0.02275 -0.00490 0.00451 -0.00438 AFIX 23 H23A 2 0.366223 0.109333 1.047891 11.00000 -1.20000 H23B 2 0.456834 0.135307 1.129530 11.00000 -1.20000 AFIX 0 C24 1 0.419099 0.263617 1.027165 11.00000 0.02402 0.02095 = 0.01944 -0.00458 0.00201 -0.00580 AFIX 23 H24A 2 0.496825 0.241687 0.988567 11.00000 -1.20000 H24B 2 0.351705 0.286483 0.981348 11.00000 -1.20000 AFIX 0 C25 1 0.177914 0.138021 1.177909 11.00000 0.02550 0.02075 = 0.02342 0.00400 -0.00126 -0.00426 C26 1 0.175405 0.036225 1.122097 11.00000 0.04207 0.02908 = 0.03623 -0.00535 0.00544 -0.01894 AFIX 137 H26A 2 0.103225 0.000934 1.145130 11.00000 -1.50000 H26B 2 0.252458 -0.012953 1.132778 11.00000 -1.50000 H26C 2 0.168931 0.055809 1.052811 11.00000 -1.50000 AFIX 0 C30 1 0.808909 0.418531 0.530015 11.00000 0.01212 0.01696 = 0.01345 0.00195 -0.00246 -0.00186 C31 1 0.804241 0.480831 0.613605 11.00000 0.01422 0.01960 = 0.01823 -0.00250 -0.00130 -0.00026 AFIX 43 H31 2 0.729497 0.525422 0.631028 11.00000 -1.20000 AFIX 0 C32 1 0.909211 0.476336 0.669714 11.00000 0.02063 0.02628 = 0.01729 -0.00477 -0.00480 -0.00415 AFIX 43 H32 2 0.905203 0.518112 0.724992 11.00000 -1.20000 AFIX 0 C33 1 1.023198 0.409220 0.644747 11.00000 0.01435 0.03126 = 0.02405 0.00111 -0.00816 -0.00381 AFIX 43 H33 2 1.094217 0.407235 0.683064 11.00000 -1.20000 AFIX 0 C34 1 1.029148 0.347889 0.565230 11.00000 0.01473 0.02638 = 0.02578 -0.00233 -0.00355 0.00242 AFIX 43 H34 2 1.104409 0.302889 0.549911 11.00000 -1.20000 AFIX 0 C35 1 0.923590 0.350343 0.504498 11.00000 0.01520 0.02036 = 0.01776 -0.00057 -0.00156 -0.00066 C36 1 0.927686 0.290343 0.419598 11.00000 0.01727 0.02764 = 0.02249 -0.00675 -0.00068 0.00511 AFIX 43 H36 2 1.002080 0.245976 0.400986 11.00000 -1.20000 AFIX 0 C37 1 0.822524 0.297152 0.364437 11.00000 0.02125 0.02377 = 0.01857 -0.00888 -0.00099 0.00270 AFIX 43 H37 2 0.824400 0.258241 0.307533 11.00000 -1.20000 AFIX 0 C38 1 0.710562 0.364173 0.394912 11.00000 0.01779 0.01656 = 0.01412 0.00074 -0.00194 -0.00278 C39 1 0.591409 0.368412 0.334837 11.00000 0.01846 0.01442 = 0.01243 0.00161 -0.00317 -0.00426 C41 1 0.386746 0.280250 0.540912 11.00000 0.01979 0.01964 = 0.02230 0.00222 -0.00892 -0.00343 AFIX 23 H41A 2 0.441050 0.246806 0.488371 11.00000 -1.20000 H41B 2 0.312710 0.322014 0.510964 11.00000 -1.20000 AFIX 0 C42 1 0.343029 0.190449 0.610314 11.00000 0.02011 0.02118 = 0.03337 0.00561 -0.00759 -0.00515 AFIX 23 H42A 2 0.281398 0.222342 0.659179 11.00000 -1.20000 H42B 2 0.302317 0.140607 0.573329 11.00000 -1.20000 AFIX 0 C43 1 0.521471 0.202350 0.713150 11.00000 0.02430 0.02375 = 0.02043 0.00345 -0.00769 -0.00507 AFIX 23 H43A 2 0.595525 0.159945 0.742516 11.00000 -1.20000 H43B 2 0.466326 0.234269 0.765951 11.00000 -1.20000 AFIX 0 C44 1 0.563633 0.292862 0.643806 11.00000 0.02010 0.02186 = 0.02020 0.00408 -0.00702 -0.00587 AFIX 23 H44A 2 0.603419 0.342560 0.681637 11.00000 -1.20000 H44B 2 0.627120 0.260849 0.596297 11.00000 -1.20000 AFIX 0 C45 1 0.483854 0.021094 0.666695 11.00000 0.02172 0.02224 = 0.02507 0.00521 0.00653 -0.00164 C46 1 0.398756 -0.048142 0.619886 11.00000 0.04179 0.01985 = 0.03462 -0.00277 0.00564 -0.00727 AFIX 137 H46A 2 0.407716 -0.038947 0.549262 11.00000 -1.50000 H46B 2 0.311622 -0.025863 0.640572 11.00000 -1.50000 H46C 2 0.422623 -0.123800 0.639952 11.00000 -1.50000 AFIX 0 C51 1 0.961169 0.045070 0.617741 11.00000 0.03983 0.03953 = 0.03238 -0.00716 0.00799 -0.00439 C52 1 0.833341 0.032245 0.590681 11.00000 0.03459 0.07147 = 0.04385 -0.00284 0.00001 -0.00209 AFIX 137 H52A 2 0.802026 0.091762 0.545737 11.00000 -1.50000 H52B 2 0.778270 0.032368 0.648933 11.00000 -1.50000 H52C 2 0.835019 -0.035893 0.559442 11.00000 -1.50000 AFIX 0 C61 1 0.249477 -0.006392 0.858215 11.00000 0.03391 0.04265 = 0.02283 -0.00663 0.00410 0.00103 C62 1 0.205202 -0.112276 0.856027 11.00000 0.05612 0.04252 = 0.04664 -0.01519 0.00405 -0.00633 AFIX 137 H62A 2 0.131475 -0.105887 0.816353 11.00000 -1.50000 H62B 2 0.183164 -0.137498 0.922064 11.00000 -1.50000 H62C 2 0.271588 -0.163699 0.828213 11.00000 -1.50000 AFIX 0 HKLF 4 REM moc490_a.res in P-1 REM wR2 = 0.0820, GooF = S = 0.965, Restrained GooF = 0.965 for all data REM R1 = 0.0395 for 6266 Fo > 4sig(Fo) and 0.0734 for all 9087 data REM 475 parameters refined using 0 restraints END WGHT 0.0316 0.0000 REM Highest difference peak 0.366, deepest hole -0.451, 1-sigma level 0.065 Q1 1 0.5568 0.5322 0.5535 11.00000 0.05 0.37 Q2 1 0.4669 0.4228 0.5380 11.00000 0.05 0.35 Q3 1 0.4016 0.1606 0.6298 11.00000 0.05 0.35 Q4 1 0.6532 0.4626 0.4765 11.00000 0.05 0.34 Q5 1 0.4420 0.4715 0.9306 11.00000 0.05 0.33 Q6 1 0.6455 0.3592 0.3744 11.00000 0.05 0.33 Q7 1 0.2928 0.4977 0.8776 11.00000 0.05 0.32 Q8 1 0.4176 0.4171 0.8994 11.00000 0.05 0.31 Q9 1 0.5587 0.4979 0.8603 11.00000 0.05 0.31 Q10 1 0.4203 0.5402 0.4880 11.00000 0.05 0.31 ; _shelx_res_checksum 1027 _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.255 _oxdiff_exptl_absorpt_empirical_full_min 0.776 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 0.500000 0.500000 1.000000 0.01445(8) Uani 1 2 d S T P . . Zn2 Zn 0.500000 0.500000 0.500000 0.01368(8) Uani 1 2 d S T P . . O1 O 0.45952(11) 0.44138(10) 0.86799(10) 0.0158(3) Uani 1 1 d . . . . . O2 O 0.09392(13) 0.16564(12) 1.24024(13) 0.0345(4) Uani 1 1 d . . . . . O3 O 0.49035(11) 0.42362(10) 0.36960(10) 0.0168(3) Uani 1 1 d . . . . . O4 O 0.57839(13) -0.02213(11) 0.71007(14) 0.0390(5) Uani 1 1 d . . . . . O11 O 0.30542(11) 0.43173(11) 0.76260(11) 0.0211(3) Uani 1 1 d . . . . . O33 O 0.60208(11) 0.31692(10) 0.25889(11) 0.0203(3) Uani 1 1 d . . . . . N1 N 0.29388(13) 0.57545(12) 0.98076(13) 0.0149(3) Uani 1 1 d . . . . . N2 N 0.43783(15) 0.35811(12) 1.08471(13) 0.0154(4) Uani 1 1 d . . . . . H2 H 0.4962(17) 0.3399(14) 1.1193(16) 0.011(5) Uiso 1 1 d . . . . . N3 N 0.70265(13) 0.42276(11) 0.47385(13) 0.0138(3) Uani 1 1 d . . . . . N4 N 0.45703(14) 0.35555(12) 0.59025(13) 0.0152(4) Uani 1 1 d . . . . . H4 H 0.4076(17) 0.3841(14) 0.6339(16) 0.011(5) Uiso 1 1 d . . . . . N5 N 1.0607(2) 0.05507(19) 0.6381(2) 0.0576(7) Uani 1 1 d . . . . . N6 N 0.2828(2) 0.07694(18) 0.86085(19) 0.0506(6) Uani 1 1 d . . . . . N22 N 0.27417(14) 0.19821(12) 1.15491(13) 0.0184(4) Uani 1 1 d . . . . . N44 N 0.45328(14) 0.13079(12) 0.65938(14) 0.0199(4) Uani 1 1 d . . . . . C10 C 0.20899(16) 0.64122(14) 1.03880(15) 0.0146(4) Uani 1 1 d . . . . . C11 C 0.25067(17) 0.68174(15) 1.12506(16) 0.0197(4) Uani 1 1 d . . . . . H11 H 0.335624 0.665499 1.141783 0.024 Uiso 1 1 calc R . . . . C12 C 0.16639(18) 0.74474(15) 1.18394(17) 0.0237(5) Uani 1 1 d . . . . . H12 H 0.194667 0.770815 1.240885 0.028 Uiso 1 1 calc R . . . . C13 C 0.03760(18) 0.77109(16) 1.16033(17) 0.0245(5) Uani 1 1 d . . . . . H13 H -0.018587 0.813608 1.201822 0.029 Uiso 1 1 calc R . . . . C14 C -0.00486(18) 0.73448(16) 1.07693(17) 0.0241(5) Uani 1 1 d . . . . . H14 H -0.089909 0.752986 1.061127 0.029 Uiso 1 1 calc R . . . . C15 C 0.07928(16) 0.66838(15) 1.01385(16) 0.0188(4) Uani 1 1 d . . . . . C16 C 0.04115(18) 0.62852(17) 0.92659(17) 0.0250(5) Uani 1 1 d . . . . . H16 H -0.042727 0.646110 0.907488 0.030 Uiso 1 1 calc R . . . . C17 C 0.12611(17) 0.56451(16) 0.87008(17) 0.0244(5) Uani 1 1 d . . . . . H17 H 0.101234 0.537990 0.812164 0.029 Uiso 1 1 calc R . . . . C18 C 0.25264(16) 0.53870(15) 0.90028(15) 0.0162(4) Uani 1 1 d . . . . . C19 C 0.34661(16) 0.46433(14) 0.83764(15) 0.0155(4) Uani 1 1 d . . . . . C21 C 0.32661(17) 0.38519(15) 1.15325(16) 0.0182(4) Uani 1 1 d . . . . . H21A H 0.253427 0.415065 1.115138 0.022 Uiso 1 1 calc R . . . . H21B H 0.344733 0.441433 1.195708 0.022 Uiso 1 1 calc R . . . . C22 C 0.29306(17) 0.28762(15) 1.21692(16) 0.0203(4) Uani 1 1 d . . . . . H22A H 0.361219 0.263060 1.261679 0.024 Uiso 1 1 calc R . . . . H22B H 0.215676 0.308719 1.256189 0.024 Uiso 1 1 calc R . . . . C23 C 0.38502(18) 0.16556(15) 1.09010(17) 0.0231(5) Uani 1 1 d . . . . . H23A H 0.366223 0.109333 1.047891 0.028 Uiso 1 1 calc R . . . . H23B H 0.456834 0.135307 1.129530 0.028 Uiso 1 1 calc R . . . . C24 C 0.41910(18) 0.26362(15) 1.02717(16) 0.0212(5) Uani 1 1 d . . . . . H24A H 0.496825 0.241687 0.988567 0.025 Uiso 1 1 calc R . . . . H24B H 0.351705 0.286483 0.981348 0.025 Uiso 1 1 calc R . . . . C25 C 0.17791(18) 0.13802(16) 1.17791(17) 0.0233(5) Uani 1 1 d . . . . . C26 C 0.1754(2) 0.03622(17) 1.1221(2) 0.0346(6) Uani 1 1 d . . . . . H26A H 0.103225 0.000934 1.145130 0.052 Uiso 1 1 calc GR . . . . H26B H 0.252458 -0.012953 1.132778 0.052 Uiso 1 1 calc GR . . . . H26C H 0.168931 0.055809 1.052811 0.052 Uiso 1 1 calc GR . . . . C30 C 0.80891(16) 0.41853(14) 0.53002(15) 0.0142(4) Uani 1 1 d . . . . . C31 C 0.80424(17) 0.48083(15) 0.61360(16) 0.0175(4) Uani 1 1 d . . . . . H31 H 0.729497 0.525422 0.631028 0.021 Uiso 1 1 calc R . . . . C32 C 0.90921(17) 0.47634(16) 0.66971(17) 0.0210(4) Uani 1 1 d . . . . . H32 H 0.905203 0.518112 0.724992 0.025 Uiso 1 1 calc R . . . . C33 C 1.02320(17) 0.40922(16) 0.64475(17) 0.0230(5) Uani 1 1 d . . . . . H33 H 1.094217 0.407235 0.683064 0.028 Uiso 1 1 calc R . . . . C34 C 1.02915(17) 0.34789(16) 0.56523(17) 0.0226(5) Uani 1 1 d . . . . . H34 H 1.104409 0.302889 0.549911 0.027 Uiso 1 1 calc R . . . . C35 C 0.92359(16) 0.35034(15) 0.50450(16) 0.0179(4) Uani 1 1 d . . . . . C36 C 0.92769(18) 0.29034(16) 0.41960(17) 0.0230(5) Uani 1 1 d . . . . . H36 H 1.002080 0.245976 0.400986 0.028 Uiso 1 1 calc R . . . . C37 C 0.82252(17) 0.29715(15) 0.36444(17) 0.0214(4) Uani 1 1 d . . . . . H37 H 0.824400 0.258241 0.307533 0.026 Uiso 1 1 calc R . . . . C38 C 0.71056(16) 0.36417(14) 0.39491(15) 0.0161(4) Uani 1 1 d . . . . . C39 C 0.59141(16) 0.36841(14) 0.33484(15) 0.0149(4) Uani 1 1 d . . . . . C41 C 0.38675(17) 0.28025(15) 0.54091(17) 0.0204(5) Uani 1 1 d . . . . . H41A H 0.441050 0.246806 0.488371 0.024 Uiso 1 1 calc R . . . . H41B H 0.312710 0.322014 0.510964 0.024 Uiso 1 1 calc R . . . . C42 C 0.34303(17) 0.19045(15) 0.61031(18) 0.0247(5) Uani 1 1 d . . . . . H42A H 0.281398 0.222342 0.659179 0.030 Uiso 1 1 calc R . . . . H42B H 0.302317 0.140607 0.573329 0.030 Uiso 1 1 calc R . . . . C43 C 0.52147(18) 0.20235(16) 0.71315(17) 0.0226(5) Uani 1 1 d . . . . . H43A H 0.595525 0.159945 0.742516 0.027 Uiso 1 1 calc R . . . . H43B H 0.466326 0.234269 0.765951 0.027 Uiso 1 1 calc R . . . . C44 C 0.56363(17) 0.29286(15) 0.64381(16) 0.0204(4) Uani 1 1 d . . . . . H44A H 0.603419 0.342560 0.681637 0.025 Uiso 1 1 calc R . . . . H44B H 0.627120 0.260849 0.596297 0.025 Uiso 1 1 calc R . . . . C45 C 0.48385(18) 0.02109(16) 0.66670(17) 0.0236(5) Uani 1 1 d . . . . . C46 C 0.3988(2) -0.04814(16) 0.61989(19) 0.0320(6) Uani 1 1 d . . . . . H46A H 0.407716 -0.038947 0.549262 0.048 Uiso 1 1 calc GR . . . . H46B H 0.311622 -0.025863 0.640572 0.048 Uiso 1 1 calc GR . . . . H46C H 0.422623 -0.123800 0.639952 0.048 Uiso 1 1 calc GR . . . . C51 C 0.9612(2) 0.04507(19) 0.6177(2) 0.0374(6) Uani 1 1 d . . . . . C52 C 0.8333(2) 0.0322(2) 0.5907(2) 0.0505(7) Uani 1 1 d . . . . . H52A H 0.802026 0.091762 0.545737 0.076 Uiso 1 1 calc GR . . . . H52B H 0.778270 0.032368 0.648933 0.076 Uiso 1 1 calc GR . . . . H52C H 0.835019 -0.035893 0.559442 0.076 Uiso 1 1 calc GR . . . . C61 C 0.2495(2) -0.0064(2) 0.85821(19) 0.0337(6) Uani 1 1 d . . . . . C62 C 0.2052(2) -0.1123(2) 0.8560(2) 0.0481(7) Uani 1 1 d . . . . . H62A H 0.131475 -0.105887 0.816353 0.072 Uiso 1 1 calc GR . . . . H62B H 0.183164 -0.137498 0.922064 0.072 Uiso 1 1 calc GR . . . . H62C H 0.271588 -0.163699 0.828213 0.072 Uiso 1 1 calc GR . . . . 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 0.01376(15) 0.01810(16) 0.0119(2) -0.00132(14) -0.00239(12) -0.00286(12) Zn2 0.01333(15) 0.01547(15) 0.0122(2) -0.00135(13) -0.00199(12) -0.00110(11) O1 0.0146(6) 0.0204(6) 0.0124(8) -0.0015(6) -0.0028(5) -0.0012(5) O2 0.0293(8) 0.0346(8) 0.0410(12) -0.0070(8) 0.0132(7) -0.0123(6) O3 0.0146(6) 0.0213(7) 0.0144(8) -0.0034(6) -0.0014(5) -0.0009(5) O4 0.0282(8) 0.0272(8) 0.0582(14) 0.0143(8) -0.0084(8) 0.0039(6) O11 0.0180(6) 0.0298(7) 0.0165(9) -0.0080(7) -0.0035(6) -0.0036(5) O33 0.0233(7) 0.0212(7) 0.0164(9) -0.0055(6) -0.0051(6) 0.0006(5) N1 0.0142(7) 0.0173(8) 0.0132(10) -0.0006(7) -0.0014(6) -0.0023(6) N2 0.0132(8) 0.0196(8) 0.0137(10) -0.0015(7) -0.0031(7) -0.0022(6) N3 0.0144(7) 0.0148(7) 0.0125(10) -0.0014(7) -0.0012(6) -0.0019(6) N4 0.0148(8) 0.0156(8) 0.0149(10) -0.0036(7) -0.0001(7) 0.0006(6) N5 0.0451(13) 0.0692(16) 0.062(2) -0.0160(14) 0.0028(12) -0.0185(12) N6 0.0612(14) 0.0491(14) 0.0427(17) -0.0091(12) 0.0103(12) -0.0132(11) N22 0.0205(8) 0.0175(8) 0.0177(10) -0.0025(7) 0.0019(7) -0.0045(6) N44 0.0183(8) 0.0167(8) 0.0246(11) 0.0024(7) -0.0054(7) -0.0020(6) C10 0.0155(9) 0.0139(8) 0.0142(11) 0.0000(8) 0.0003(7) -0.0016(7) C11 0.0176(9) 0.0225(10) 0.0191(13) -0.0036(9) -0.0024(8) -0.0012(8) C12 0.0267(11) 0.0235(10) 0.0207(13) -0.0060(10) -0.0026(9) 0.0001(8) C13 0.0230(10) 0.0214(10) 0.0276(14) -0.0062(10) 0.0040(9) 0.0031(8) C14 0.0158(9) 0.0264(10) 0.0290(14) -0.0030(10) -0.0012(8) 0.0016(8) C15 0.0148(9) 0.0213(10) 0.0204(13) -0.0007(9) -0.0024(8) -0.0018(7) C16 0.0138(9) 0.0346(11) 0.0269(14) -0.0061(10) -0.0066(8) 0.0004(8) C17 0.0187(10) 0.0325(11) 0.0227(13) -0.0091(10) -0.0069(8) -0.0008(8) C18 0.0162(9) 0.0191(9) 0.0139(12) 0.0002(8) -0.0013(7) -0.0042(7) C19 0.0167(9) 0.0174(9) 0.0130(11) 0.0005(8) -0.0002(7) -0.0053(7) C21 0.0185(9) 0.0183(9) 0.0183(12) -0.0037(9) 0.0002(8) -0.0030(7) C22 0.0222(10) 0.0211(10) 0.0181(12) -0.0026(9) 0.0014(8) -0.0053(8) C23 0.0268(11) 0.0199(10) 0.0228(13) -0.0049(9) 0.0045(9) -0.0044(8) C24 0.0240(10) 0.0210(10) 0.0194(13) -0.0046(9) 0.0020(8) -0.0058(8) C25 0.0255(11) 0.0208(10) 0.0234(14) 0.0040(9) -0.0013(9) -0.0043(8) C26 0.0421(13) 0.0291(11) 0.0362(17) -0.0054(11) 0.0054(11) -0.0189(10) C30 0.0121(8) 0.0170(9) 0.0134(11) 0.0019(8) -0.0025(7) -0.0019(7) C31 0.0142(9) 0.0196(9) 0.0182(12) -0.0025(9) -0.0013(8) -0.0003(7) C32 0.0206(10) 0.0263(10) 0.0173(12) -0.0048(9) -0.0048(8) -0.0042(8) C33 0.0143(9) 0.0313(11) 0.0241(14) 0.0011(10) -0.0082(8) -0.0038(8) C34 0.0147(9) 0.0264(10) 0.0258(14) -0.0023(10) -0.0036(8) 0.0024(8) C35 0.0152(9) 0.0204(9) 0.0178(12) -0.0006(9) -0.0016(8) -0.0007(7) C36 0.0173(10) 0.0276(11) 0.0225(13) -0.0067(10) -0.0007(8) 0.0051(8) C37 0.0213(10) 0.0238(10) 0.0186(13) -0.0089(9) -0.0010(8) 0.0027(8) C38 0.0178(9) 0.0166(9) 0.0141(12) 0.0007(8) -0.0019(7) -0.0028(7) C39 0.0185(9) 0.0144(9) 0.0124(11) 0.0016(8) -0.0032(7) -0.0043(7) C41 0.0198(10) 0.0196(9) 0.0223(13) 0.0022(9) -0.0089(8) -0.0034(8) C42 0.0201(10) 0.0212(10) 0.0334(15) 0.0056(10) -0.0076(9) -0.0052(8) C43 0.0243(10) 0.0237(10) 0.0204(13) 0.0035(9) -0.0077(8) -0.0051(8) C44 0.0201(10) 0.0219(10) 0.0202(13) 0.0041(9) -0.0070(8) -0.0059(8) C45 0.0217(10) 0.0222(10) 0.0251(14) 0.0052(9) 0.0065(9) -0.0016(8) C46 0.0418(13) 0.0199(10) 0.0346(16) -0.0028(10) 0.0056(11) -0.0073(9) C51 0.0398(14) 0.0395(13) 0.0324(16) -0.0072(12) 0.0080(11) -0.0044(11) C52 0.0346(14) 0.0715(19) 0.044(2) -0.0028(16) 0.0000(12) -0.0021(13) C61 0.0339(12) 0.0426(14) 0.0228(15) -0.0066(12) 0.0041(10) 0.0010(10) C62 0.0561(16) 0.0425(15) 0.047(2) -0.0152(14) 0.0040(13) -0.0063(12) 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 O1 Zn1 O1 180.0 . 2_667 ? O1 Zn1 N1 102.20(5) . 2_667 ? O1 Zn1 N1 77.80(5) 2_667 2_667 ? O1 Zn1 N1 77.80(5) . . ? O1 Zn1 N1 102.20(5) 2_667 . ? O1 Zn1 N2 92.34(6) . . ? O1 Zn1 N2 87.66(6) . 2_667 ? O1 Zn1 N2 87.66(6) 2_667 . ? O1 Zn1 N2 92.34(6) 2_667 2_667 ? N1 Zn1 N1 180.0 . 2_667 ? N2 Zn1 N1 89.06(6) . 2_667 ? N2 Zn1 N1 90.94(6) . . ? N2 Zn1 N1 89.06(6) 2_667 . ? N2 Zn1 N1 90.94(6) 2_667 2_667 ? N2 Zn1 N2 180.0 . 2_667 ? O3 Zn2 O3 180.00(6) . 2_666 ? O3 Zn2 N3 102.34(5) 2_666 . ? O3 Zn2 N3 77.66(5) . . ? O3 Zn2 N3 77.66(5) 2_666 2_666 ? O3 Zn2 N3 102.34(5) . 2_666 ? O3 Zn2 N4 87.28(6) . 2_666 ? O3 Zn2 N4 92.72(6) . . ? O3 Zn2 N4 87.28(6) 2_666 . ? O3 Zn2 N4 92.72(6) 2_666 2_666 ? N3 Zn2 N3 180.0 2_666 . ? N4 Zn2 N3 90.82(5) . . ? N4 Zn2 N3 90.82(5) 2_666 2_666 ? N4 Zn2 N3 89.18(5) 2_666 . ? N4 Zn2 N3 89.18(5) . 2_666 ? N4 Zn2 N4 180.0 2_666 . ? C19 O1 Zn1 118.30(12) . . ? C39 O3 Zn2 118.38(12) . . ? C10 N1 Zn1 132.62(13) . . ? C18 N1 Zn1 108.58(11) . . ? C18 N1 C10 118.60(15) . . ? C21 N2 Zn1 114.42(11) . . ? C24 N2 Zn1 116.22(13) . . ? C24 N2 C21 110.05(14) . . ? C30 N3 Zn2 131.30(12) . . ? C38 N3 Zn2 109.63(11) . . ? C38 N3 C30 118.69(14) . . ? C41 N4 Zn2 115.39(13) . . ? C41 N4 C44 109.93(14) . . ? C44 N4 Zn2 116.69(11) . . ? C23 N22 C22 112.69(14) . . ? C25 N22 C22 119.70(17) . . ? C25 N22 C23 125.38(16) . . ? C43 N44 C42 112.37(15) . . ? C45 N44 C42 125.95(17) . . ? C45 N44 C43 121.22(16) . . ? N1 C10 C11 119.73(16) . . ? N1 C10 C15 121.17(18) . . ? C11 C10 C15 119.10(17) . . ? C12 C11 C10 119.95(17) . . ? C11 C12 C13 121.3(2) . . ? C14 C13 C12 120.04(19) . . ? C13 C14 C15 120.55(17) . . ? C14 C15 C10 119.04(19) . . ? C16 C15 C10 117.80(18) . . ? C16 C15 C14 123.15(17) . . ? C17 C16 C15 120.21(18) . . ? C16 C17 C18 119.1(2) . . ? N1 C18 C17 123.14(18) . . ? N1 C18 C19 118.19(15) . . ? C17 C18 C19 118.66(18) . . ? O1 C19 C18 116.94(17) . . ? O11 C19 O1 126.37(17) . . ? O11 C19 C18 116.69(15) . . ? N2 C21 C22 113.25(14) . . ? N22 C22 C21 110.19(17) . . ? N22 C23 C24 110.01(15) . . ? N2 C24 C23 113.82(18) . . ? O2 C25 N22 121.86(19) . . ? O2 C25 C26 120.65(18) . . ? N22 C25 C26 117.47(19) . . ? N3 C30 C31 120.15(15) . . ? N3 C30 C35 120.58(17) . . ? C31 C30 C35 119.27(17) . . ? C32 C31 C30 120.27(17) . . ? C31 C32 C33 120.77(19) . . ? C34 C33 C32 119.83(18) . . ? C33 C34 C35 121.52(17) . . ? C34 C35 C30 118.33(18) . . ? C36 C35 C30 118.63(17) . . ? C36 C35 C34 123.03(16) . . ? C37 C36 C35 119.78(17) . . ? C36 C37 C38 118.93(19) . . ? N3 C38 C37 123.36(17) . . ? N3 C38 C39 117.88(15) . . ? C37 C38 C39 118.75(17) . . ? O3 C39 C38 116.22(17) . . ? O33 C39 O3 126.79(17) . . ? O33 C39 C38 116.97(15) . . ? N4 C41 C42 113.31(18) . . ? N44 C42 C41 109.18(15) . . ? N44 C43 C44 110.20(17) . . ? N4 C44 C43 112.74(15) . . ? O4 C45 N44 121.47(19) . . ? O4 C45 C46 120.35(18) . . ? N44 C45 C46 118.19(18) . . ? N5 C51 C52 179.5(3) . . ? N6 C61 C62 179.0(3) . . ? 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 O1 2.0529(13) . ? Zn1 O1 2.0529(13) 2_667 ? Zn1 N1 2.2741(14) 2_667 ? Zn1 N1 2.2741(14) . ? Zn1 N2 2.1953(16) . ? Zn1 N2 2.1953(16) 2_667 ? Zn2 O3 2.0639(13) 2_666 ? Zn2 O3 2.0639(13) . ? Zn2 N3 2.2479(14) . ? Zn2 N3 2.2478(14) 2_666 ? Zn2 N4 2.1887(16) . ? Zn2 N4 2.1887(16) 2_666 ? O1 C19 1.272(2) . ? O2 C25 1.226(2) . ? O3 C39 1.275(2) . ? O4 C45 1.227(2) . ? O11 C19 1.234(2) . ? O33 C39 1.234(2) . ? N1 C10 1.377(2) . ? N1 C18 1.319(2) . ? N2 C21 1.480(2) . ? N2 C24 1.478(2) . ? N3 C30 1.381(2) . ? N3 C38 1.319(2) . ? N4 C41 1.471(2) . ? N4 C44 1.475(2) . ? N5 C51 1.125(3) . ? N6 C61 1.133(3) . ? N22 C22 1.464(2) . ? N22 C23 1.460(2) . ? N22 C25 1.353(2) . ? N44 C42 1.459(2) . ? N44 C43 1.457(2) . ? N44 C45 1.347(2) . ? C10 C11 1.410(3) . ? C10 C15 1.420(2) . ? C11 C12 1.363(3) . ? C12 C13 1.405(3) . ? C13 C14 1.358(3) . ? C14 C15 1.416(3) . ? C15 C16 1.403(3) . ? C16 C17 1.355(3) . ? C17 C18 1.408(2) . ? C18 C19 1.523(3) . ? C21 C22 1.512(3) . ? C23 C24 1.513(3) . ? C25 C26 1.506(3) . ? C30 C31 1.401(3) . ? C30 C35 1.422(2) . ? C31 C32 1.368(3) . ? C32 C33 1.408(3) . ? C33 C34 1.347(3) . ? C34 C35 1.414(3) . ? C35 C36 1.400(3) . ? C36 C37 1.360(3) . ? C37 C38 1.410(2) . ? C38 C39 1.526(2) . ? C41 C42 1.517(3) . ? C43 C44 1.517(3) . ? C45 C46 1.504(3) . ? C51 C52 1.449(3) . ? C61 C62 1.447(3) . ? 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 N2 H2 O33 0.793(19) 2.23(2) 2.977(2) 157.4(19) 1_556 yes N4 H4 O11 0.834(19) 2.08(2) 2.903(2) 168.1(19) . yes