#------------------------------------------------------------------------------ #$Date: 2024-01-06 09:56:46 +0200 (Sat, 06 Jan 2024) $ #$Revision: 288787 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/76/7247683.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_7247683 loop_ _publ_author_name 'Roy, Subhadip' 'Mal, Susital' 'Banik, Rupak' 'Das, Subrata' 'Dlh\'a\ 2\s(I)' _cod_data_source_file d3ce00871a2.cif _cod_data_source_block 2 _cod_depositor_comments 'Adding full bibliography for 7247682--7247683.cif.' _cod_original_cell_volume 1385.8(2) _cod_database_code 7247683 _shelx_shelxl_version_number 2019/3 _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. ; _olex2_refinement_description ; 1. Restrained distances O1W-H1WA = O1W-H1WB 0.82 with sigma of 0.01 H1WA-H1WB 1.297 with sigma of 0.01 O2W-H2WA = O2W-H2WB 0.82 with sigma of 0.01 H2WA-H2WB 1.297 with sigma of 0.01 2. Uiso/Uaniso restraints and constraints Uanis(O11) = Uanis(O11A) Uanis(O12) = Uanis(O12A) Uanis(O13) = Uanis(O13A) Uanis(O14) = Uanis(O14A) Uanis(N11) = Uanis(N11A) Uanis(N12) = Uanis(N12A) Uanis(N13) = Uanis(N13A) Uanis(C11) = Uanis(C11A) Uanis(C12) = Uanis(C12A) Uanis(C13) = Uanis(C13A) Uanis(C14) = Uanis(C14A) Uanis(C15) = Uanis(C15A) Uanis(C16) = Uanis(C16A) 3. Same fragment restrains {O11, O13, O14, N12, N13, C11, C12, C13, C14, C15, C16} sigma for 1-2: 0.02, 1-3: 0.04 as in {O11A, O13A, O14A, N12A, N13A, C11A, C12A, C13A, C14A, C15A, C16A} 4. Others Sof(O12A)=Sof(N11A)=Sof(O11A)=Sof(O13A)=Sof(O14A)=Sof(N12A)=Sof(N13A)= Sof(C11A)=Sof(C12A)=Sof(C13A)=Sof(C14A)=Sof(C15A)=Sof(H15D)=Sof(H15E)= Sof(H15F)=Sof(C16A)=Sof(H16D)=Sof(H16E)=Sof(H16F)=1-FVAR(1) Sof(O12)=Sof(N11)=Sof(O11)=Sof(O13)=Sof(O14)=Sof(N12)=Sof(N13)=Sof(C11)= Sof(C12)=Sof(C13)=Sof(C14)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C16)= Sof(H16A)=Sof(H16B)=Sof(H16C)=FVAR(1) Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(2) Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(2) 5.a Me refined with riding coordinates: C15A(H15D,H15E,H15F), C16A(H16D,H16E,H16F) 5.b Aromatic/amide H refined with riding coordinates: C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46) 5.c Idealised Me refined as rotating group: C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C25(H25A,H25B,H25C), C25(H25D,H25E, H25F), C26(H26A,H26B,H26C) ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL x in P-1 2.res created by SHELXL-2019/3 at 06:59:55 on 08-Oct-2023 CELL 0.71073 11.1064 12.1528 12.3032 113.663 106.663 98.98 ZERR 2 0.0009 0.0011 0.0012 0.009 0.008 0.007 LATT 1 SFAC C H N O Zn UNIT 44 56 16 22 2 EQIV $1 1-X,1-Y,1-Z EQIV $2 -X,1-Y,-Z EQIV $3 1-X,2-Y,1-Z EQIV $4 1+X,1+Y,1+Z EQIV $5 -1-X,-Y,-1-Z EQIV $6 -X,-Y,-Z EQIV $7 1-X,1-Y,-Z EADP O11 O11A EADP O12 O12A EADP O13 O13A EADP O14 O14A EADP N11 N11A EADP N12 N12A EADP N13 N13A EADP C11 C11A EADP C12 C12A EADP C13 C13A EADP C14 C14A EADP C15 C15A EADP C16 C16A DFIX 0.82 0.01 O1W H1Wa O1W H1Wb DFIX 1.297 0.01 H1Wa H1Wb DFIX 0.82 0.01 O2W H2Wa O2W H2Wb DFIX 1.297 0.01 H2Wa H2Wb L.S. 50 PLAN 5 TEMP -150 CONF HTAB O1W O13 HTAB O1W O13A HTAB O1W O1W_$5 HTAB O2W O1W_$6 HTAB C25 O13_$4 HTAB C26 O22_$7 HTAB C32 O12_$1 HTAB C32 O21 HTAB C36 O11 HTAB C36 O11A HTAB C42 O11 HTAB C42 O22_$2 HTAB C43 O22_$2 HTAB C45 O23_$3 damp 100 bond $h htab bump ABIN fmap 2 53 acta 51 REM REM REM WGHT 0.058900 FVAR 5.90247 0.83245 0.55310 ZN1 5 0.235212 0.491102 0.290411 11.00000 0.03248 0.03381 = 0.03005 0.01153 0.00829 0.00433 O1W 4 -0.452152 0.054352 -0.361241 11.00000 0.09134 0.12352 = 0.08792 0.02223 0.00514 0.04923 H1WA 2 -0.373665 0.066995 -0.347956 11.00000 -1.50000 H1WB 2 -0.489151 -0.016856 -0.421210 11.00000 -1.50000 O2W 4 0.499426 0.095005 0.238234 11.00000 0.11607 0.15410 = 0.23556 0.11198 0.05751 0.05735 H2WA 2 0.496840 0.062057 0.163522 11.00000 -1.50000 H2WB 2 0.492614 0.036700 0.255852 11.00000 -1.50000 PART 1 O12 4 0.354509 0.269923 0.228859 21.00000 0.03980 0.05589 = 0.05940 0.02387 0.00514 0.01768 N11 3 0.251347 0.299777 0.198688 21.00000 0.03198 0.04077 = 0.03533 0.01559 0.00942 0.00511 O11 4 0.036878 0.369433 0.162283 21.00000 0.03142 0.03439 = 0.03671 0.00663 0.00672 0.00443 O13 4 -0.186458 0.032632 -0.231052 21.00000 0.05580 0.05767 = 0.03524 0.00606 -0.00450 -0.00550 O14 4 0.221373 0.047393 -0.001043 21.00000 0.06176 0.04327 = 0.06495 0.01892 0.02458 0.02080 N12 3 -0.078054 0.197080 -0.030619 21.00000 0.03142 0.03565 = 0.03353 0.00998 0.00349 -0.00124 N13 3 0.020864 0.045294 -0.119539 21.00000 0.05622 0.03052 = 0.03050 0.00557 0.01225 0.00239 C11 1 0.036320 0.269033 0.076816 21.00000 0.03614 0.02835 = 0.02863 0.01432 0.00732 0.00138 C12 1 -0.087464 0.087448 -0.133789 21.00000 0.04806 0.03846 = 0.03233 0.01334 0.00847 -0.00050 C13 1 0.136501 0.099335 -0.006397 21.00000 0.04769 0.03108 = 0.04030 0.01565 0.02004 0.00704 C14 1 0.145529 0.219451 0.090703 21.00000 0.03661 0.02877 = 0.03214 0.01251 0.00918 0.00197 C15 1 -0.193495 0.242112 -0.041814 21.00000 0.03729 0.06075 = 0.06044 0.01724 0.00349 0.01041 AFIX 137 H15A 2 -0.181892 0.307557 0.042862 21.00000 -1.50000 H15B 2 -0.272871 0.171502 -0.074165 21.00000 -1.50000 H15C 2 -0.203047 0.277439 -0.101638 21.00000 -1.50000 AFIX 0 C16 1 0.012303 -0.070499 -0.229234 21.00000 0.09974 0.04440 = 0.03577 0.00755 0.02129 0.01687 AFIX 137 H16A 2 -0.077623 -0.129229 -0.270548 21.00000 -1.50000 H16B 2 0.074900 -0.110290 -0.198578 21.00000 -1.50000 H16C 2 0.033938 -0.048998 -0.291537 21.00000 -1.50000 AFIX 0 PART 2 O12A 4 0.318563 0.338044 0.271010 -21.00000 0.03980 0.05589 = 0.05940 0.02387 0.00514 0.01768 N11A 3 0.276100 0.234679 0.170528 -21.00000 0.03198 0.04077 = 0.03533 0.01559 0.00942 0.00511 SAME 0.02 0.04 O11 > C16 O11A 4 0.067091 0.356376 0.175571 -21.00000 0.03142 0.03439 = 0.03671 0.00663 0.00672 0.00443 O13A 4 -0.183968 0.051872 -0.231544 -21.00000 0.05580 0.05767 = 0.03524 0.00606 -0.00450 -0.00550 O14A 4 0.203853 0.009955 -0.037233 -21.00000 0.06176 0.04327 = 0.06495 0.01892 0.02458 0.02080 N12A 3 -0.059435 0.203789 -0.026842 -21.00000 0.03142 0.03565 = 0.03353 0.00998 0.00349 -0.00124 N13A 3 0.007953 0.029578 -0.136427 -21.00000 0.05622 0.03052 = 0.03050 0.00557 0.01225 0.00239 C11A 1 0.053259 0.252887 0.083635 -21.00000 0.03614 0.02835 = 0.02863 0.01432 0.00732 0.00138 C12A 1 -0.084257 0.093027 -0.136685 -21.00000 0.04806 0.03846 = 0.03233 0.01334 0.00847 -0.00050 C13A 1 0.130591 0.075571 -0.032988 -21.00000 0.04769 0.03108 = 0.04030 0.01565 0.02004 0.00704 C14A 1 0.152787 0.191698 0.075891 -21.00000 0.03661 0.02877 = 0.03214 0.01251 0.00918 0.00197 C15A 1 -0.169199 0.258008 -0.029840 -21.00000 0.03729 0.06075 = 0.06044 0.01724 0.00349 0.01041 AFIX 33 H15D 2 -0.239752 0.210796 -0.115894 -21.00000 -1.50000 H15E 2 -0.203503 0.252634 0.033516 -21.00000 -1.50000 H15F 2 -0.137429 0.346695 -0.009137 -21.00000 -1.50000 AFIX 0 C16A 1 -0.012830 -0.075165 -0.261620 -21.00000 0.09974 0.04440 = 0.03577 0.00755 0.02129 0.01687 AFIX 33 H16D 2 0.057984 -0.113671 -0.250678 -21.00000 -1.50000 H16E 2 -0.098268 -0.138765 -0.294729 -21.00000 -1.50000 H16F 2 -0.012010 -0.042636 -0.322614 -21.00000 -1.50000 AFIX 0 PART 0 O21 4 0.431423 0.608318 0.375840 11.00000 0.03207 0.04995 = 0.02783 0.01957 0.00774 0.00630 O22 4 0.191055 0.447929 0.015914 11.00000 0.04483 0.05661 = 0.02789 0.00988 -0.00261 -0.00205 O23 4 0.746319 0.846222 0.326570 11.00000 0.04335 0.04297 = 0.06959 0.01531 0.02280 -0.00362 O24 4 0.385194 0.571914 -0.031302 11.00000 0.06022 0.08714 = 0.03454 0.03340 0.01462 0.01443 N21 3 0.273221 0.504963 0.131221 11.00000 0.03389 0.03551 = 0.02553 0.00929 0.00390 0.00685 N22 3 0.589099 0.725391 0.350363 11.00000 0.02916 0.03173 = 0.03021 0.00999 0.00542 0.00331 N23 3 0.562289 0.713048 0.147886 11.00000 0.04605 0.04325 = 0.04572 0.02330 0.02622 0.01106 C21 1 0.469313 0.638170 0.302353 11.00000 0.02869 0.02870 = 0.02732 0.01086 0.00473 0.00880 C22 1 0.638953 0.767242 0.277806 11.00000 0.03852 0.03100 = 0.04972 0.01482 0.01879 0.01109 C23 1 0.440886 0.618167 0.084859 11.00000 0.04178 0.04274 = 0.03470 0.02076 0.01467 0.01466 C24 1 0.392235 0.584473 0.166676 11.00000 0.03053 0.03461 = 0.02698 0.01237 0.00707 0.00925 C25 1 0.668530 0.785708 0.488864 11.00000 0.03899 0.05263 = 0.03642 0.00850 -0.00098 -0.00041 PART 1 AFIX 137 H25A 2 0.629653 0.741102 0.527632 31.00000 -1.50000 H25B 2 0.670035 0.874037 0.528891 31.00000 -1.50000 H25C 2 0.758956 0.782276 0.502580 31.00000 -1.50000 AFIX 137 PART 2 H25D 2 0.744368 0.855474 0.511294 -31.00000 -1.50000 H25E 2 0.700031 0.723527 0.510972 -31.00000 -1.50000 H25F 2 0.614245 0.818413 0.536837 -31.00000 -1.50000 AFIX 0 PART 0 C26 1 0.615232 0.757648 0.071517 11.00000 0.08062 0.07495 = 0.07237 0.04482 0.04759 0.01817 AFIX 137 H26A 2 0.662797 0.848304 0.123075 11.00000 -1.50000 H26B 2 0.542378 0.742532 -0.005494 11.00000 -1.50000 H26C 2 0.675915 0.711927 0.045910 11.00000 -1.50000 AFIX 0 N31 3 0.236182 0.486740 0.458487 11.00000 0.03805 0.03727 = 0.03529 0.01631 0.01136 0.01083 C32 1 0.341457 0.548606 0.571277 11.00000 0.03793 0.05575 = 0.03902 0.02322 0.00864 0.00500 AFIX 43 H32 2 0.421914 0.592250 0.573913 11.00000 -1.20000 AFIX 0 C33 1 0.336920 0.551018 0.683037 11.00000 0.04964 0.06449 = 0.03541 0.02375 0.00683 0.00991 AFIX 43 H33 2 0.412830 0.596286 0.761093 11.00000 -1.20000 AFIX 0 C34 1 0.222522 0.487855 0.680463 11.00000 0.05956 0.07916 = 0.04091 0.03363 0.02234 0.02011 AFIX 43 H34 2 0.217117 0.488633 0.756430 11.00000 -1.20000 AFIX 0 C35 1 0.114119 0.422384 0.564349 11.00000 0.04503 0.07131 = 0.05346 0.03596 0.02079 0.00900 AFIX 43 H35 2 0.033337 0.376478 0.559152 11.00000 -1.20000 AFIX 0 C36 1 0.125331 0.424953 0.457814 11.00000 0.04113 0.04728 = 0.04020 0.02176 0.01284 0.00873 AFIX 43 H36 2 0.050281 0.380414 0.378988 11.00000 -1.20000 AFIX 0 N41 3 0.161521 0.648811 0.329938 11.00000 0.03891 0.03325 = 0.03044 0.01169 0.01052 0.00629 C42 1 0.050796 0.645433 0.245679 11.00000 0.04292 0.04005 = 0.03556 0.01737 0.01269 0.01128 AFIX 43 H42 2 0.008173 0.573463 0.163133 11.00000 -1.20000 AFIX 0 C43 1 -0.002626 0.743407 0.275651 11.00000 0.05768 0.05453 = 0.05322 0.03051 0.02192 0.02527 AFIX 43 H43 2 -0.082281 0.738073 0.215514 11.00000 -1.20000 AFIX 0 C44 1 0.060696 0.848418 0.393221 11.00000 0.08533 0.04568 = 0.07101 0.03050 0.04109 0.03553 AFIX 43 H44 2 0.025296 0.916855 0.415627 11.00000 -1.20000 AFIX 0 C45 1 0.176166 0.854271 0.478935 11.00000 0.07690 0.03501 = 0.04933 0.00809 0.02271 0.01357 AFIX 43 H45 2 0.222726 0.927176 0.560287 11.00000 -1.20000 AFIX 0 C46 1 0.222249 0.752217 0.443904 11.00000 0.04835 0.03810 = 0.03645 0.00699 0.00794 0.00598 AFIX 43 H46 2 0.300937 0.755331 0.503480 11.00000 -1.20000 AFIX 0 HKLF 4 REM x in P-1 REM wR2 = 0.1583, GooF = S = 1.016, Restrained GooF = 1.014 for all data REM R1 = 0.0638 for 5823 Fo > 4sig(Fo) and 0.1111 for all 9459 data REM 427 parameters refined using 35 restraints END WGHT 0.0589 0.0000 REM Instructions for potential hydrogen bonds HTAB O1W O13 HTAB O1W O13A HTAB O1W O1W_$5 HTAB O2W O1W_$6 HTAB C25 O13_$4 HTAB C26 O22_$7 HTAB C32 O12_$1 HTAB C32 O21 HTAB C36 O11 HTAB C36 O11A HTAB C42 O11 HTAB C42 O22_$2 HTAB C43 O22_$2 HTAB C45 O23_$3 REM Highest difference peak 0.781, deepest hole -0.502, 1-sigma level 0.074 Q1 1 0.5000 0.0000 0.0000 10.50000 0.05 0.78 Q2 1 0.1956 0.5682 0.3156 11.00000 0.05 0.38 Q3 1 0.0223 0.2843 0.1521 11.00000 0.05 0.37 Q4 1 0.2585 0.5057 0.2022 11.00000 0.05 0.36 Q5 1 0.1629 0.4128 0.2814 11.00000 0.05 0.35 ; _shelx_res_checksum 57733 _shelx_fab_file ; -17 -1 7 -0.1123 0.0161 -17 -1 8 -0.2532 -0.0212 -17 0 5 0.1244 0.0241 -17 0 6 -0.1879 0.0055 -17 0 7 -0.3412 -0.0248 -17 0 8 0.1064 0.0050 -17 0 9 0.0588 0.0179 -17 1 4 0.1395 0.0113 -17 1 5 -0.1404 -0.0044 -17 1 6 -0.2106 -0.0244 -17 1 7 0.2041 0.0009 -17 1 8 0.2038 0.0145 -17 1 9 -0.0934 -0.0136 -17 2 3 0.2058 -0.0056 -17 2 4 -0.0016 -0.0083 -17 2 5 0.0847 -0.0173 -17 2 6 0.3364 0.0015 -17 2 7 0.2264 0.0094 -17 2 8 0.0271 -0.0137 -17 2 9 -0.0259 0.0032 -17 3 2 0.1915 -0.0184 -17 3 3 0.1200 -0.0055 -17 3 4 0.2941 -0.0045 -17 3 5 0.3948 0.0069 -17 3 6 -0.0082 0.0038 -17 3 7 -0.0530 -0.0149 -17 3 8 0.0237 0.0003 -17 4 2 0.1224 0.0006 -17 4 3 0.2357 0.0069 -17 4 4 0.2656 0.0137 -17 4 5 -0.4193 -0.0011 -17 4 6 -0.3712 -0.0172 -17 4 7 0.0346 -0.0022 -17 4 8 -0.2280 0.0218 -17 5 2 -0.0001 0.0092 -17 5 3 -0.0065 0.0168 -17 5 4 -0.7477 -0.0033 -17 5 5 -0.7088 -0.0199 -17 5 6 0.0192 -0.0026 -17 5 7 -0.1594 0.0240 -17 6 2 -0.2058 0.0129 -17 6 3 -0.7587 -0.0008 -17 6 4 -0.7736 -0.0199 -17 6 5 0.0587 -0.0005 -17 6 6 -0.0461 0.0241 -16 -4 6 0.1163 -0.0066 -16 -4 7 -0.0203 0.0340 -16 -4 8 -0.4387 -0.0094 -16 -4 9 -0.0791 -0.0316 -16 -4 10 0.1524 0.0185 -16 -3 4 -0.2769 -0.0252 -16 -3 5 -0.0263 0.0060 -16 -3 6 0.0423 0.0219 -16 -3 7 -0.4193 -0.0175 -16 -3 8 -0.0395 -0.0265 -16 -3 9 0.1811 0.0165 -16 -3 10 -0.0736 -0.0115 -16 -3 11 -0.0193 -0.0167 -16 -2 3 -0.0311 -0.0035 -16 -2 4 -0.2500 0.0126 -16 -2 5 -0.0243 0.0097 -16 -2 6 -0.3369 -0.0226 -16 -2 7 0.0901 -0.0190 -16 -2 8 0.2943 0.0180 -16 -2 9 -0.0417 -0.0118 -16 -2 10 0.0424 -0.0178 -16 -2 11 0.4707 0.0175 -16 -2 12 0.1732 -0.0048 -16 -1 2 0.2000 0.0081 -16 -1 3 -0.4188 0.0094 -16 -1 4 -0.2184 -0.0003 -16 -1 5 -0.2269 -0.0223 -16 -1 6 0.2285 -0.0083 -16 -1 7 0.4375 0.0215 -16 -1 8 -0.0678 -0.0078 -16 -1 9 0.0282 -0.0165 -16 -1 10 0.3762 0.0184 -16 -1 11 0.1475 -0.0037 -16 -1 12 -0.7866 -0.0012 -16 0 1 0.3056 0.0062 -16 0 2 -0.4400 -0.0022 -16 0 3 -0.4329 -0.0031 -16 0 4 -0.1638 -0.0163 -16 0 5 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0.8631 0.0031 2 -6 6 0.8802 0.0046 2 -6 7 0.9949 0.0040 2 -6 8 0.2774 0.0025 2 -6 9 0.2167 -0.0028 2 -6 10 -0.1477 0.0016 2 -6 11 0.1658 -0.0007 2 -6 12 0.3455 0.0050 2 -6 13 0.2122 -0.0013 2 -6 14 0.2008 0.0057 2 -6 15 0.0692 -0.0035 2 -6 16 -0.0982 -0.0176 2 -6 17 -0.0241 0.0388 2 -5 0 -0.7367 0.0128 2 -5 1 1.1511 0.0208 2 -5 2 3.1286 -0.0056 2 -5 3 3.4167 0.0026 2 -5 4 1.3858 0.0004 2 -5 5 0.8385 0.0074 2 -5 6 1.3133 0.0024 2 -5 7 0.3891 0.0012 2 -5 8 0.1065 -0.0021 2 -5 9 -0.1440 -0.0017 2 -5 10 0.1474 -0.0008 2 -5 11 0.2936 0.0029 2 -5 12 -0.0238 0.0020 2 -5 13 0.1523 0.0013 2 -5 14 0.0295 0.0002 2 -5 15 -0.0855 -0.0154 2 -5 16 0.0440 0.0348 2 -5 17 0.1038 0.0181 2 -4 0 1.8111 0.0160 2 -4 1 4.2551 -0.0268 2 -4 2 4.5918 0.0024 2 -4 3 1.9379 -0.0048 2 -4 4 0.6030 0.0001 2 -4 5 1.4823 0.0009 2 -4 6 0.6662 -0.0055 2 -4 7 0.0390 0.0002 2 -4 8 -0.1113 -0.0041 2 -4 9 0.1108 -0.0001 2 -4 10 0.3146 0.0016 2 -4 11 -0.2410 0.0052 2 -4 12 0.0732 0.0004 2 -4 13 0.1084 0.0018 2 -4 14 -0.0754 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1 0.2872 0.0111 13 -9 2 0.4370 -0.0073 13 -9 3 -0.2087 -0.0063 13 -9 4 -0.4384 -0.0032 13 -9 5 0.0039 -0.0032 13 -9 6 0.3907 0.0123 13 -9 7 0.4305 -0.0217 13 -9 8 0.3045 -0.0106 13 -8 0 0.5299 0.0023 13 -8 1 0.8433 -0.0014 13 -8 2 -0.0706 -0.0027 13 -8 3 -0.3407 -0.0002 13 -8 4 0.3359 -0.0093 13 -8 5 1.0303 0.0055 13 -8 6 0.7800 -0.0107 13 -8 7 0.5429 -0.0089 13 -8 8 0.1420 0.0159 13 -7 0 0.9373 0.0016 13 -7 1 -0.0574 0.0027 13 -7 2 -0.3099 -0.0009 13 -7 3 0.4161 -0.0105 13 -7 4 1.4574 0.0016 13 -7 5 0.9258 -0.0008 13 -7 6 0.3696 -0.0077 13 -7 7 0.1425 0.0161 13 -7 8 0.0648 -0.0138 13 -6 0 -0.3115 0.0063 13 -6 1 -0.4234 -0.0027 13 -6 2 0.1334 -0.0096 13 -6 3 1.3121 0.0003 13 -6 4 0.8204 0.0036 13 -6 5 -0.1813 -0.0085 13 -6 6 -0.0519 0.0102 13 -6 7 0.0023 -0.0091 13 -5 0 -0.5859 -0.0040 13 -5 1 -0.2518 -0.0076 13 -5 2 0.6591 0.0005 13 -5 3 0.5507 0.0020 13 -5 4 -0.6929 -0.0089 13 -5 5 -0.3359 0.0019 13 -5 6 0.0864 -0.0025 13 -5 7 -0.0000 -0.0282 13 -4 0 -0.3970 -0.0045 13 -4 1 -0.0697 0.0025 13 -4 2 0.2362 -0.0026 13 -4 3 -0.7987 -0.0072 13 -4 4 -0.4781 -0.0024 13 -4 5 0.2177 0.0018 13 -4 6 0.0269 -0.0243 13 -4 7 -0.0183 -0.0084 13 -3 0 -0.4955 0.0052 13 -3 1 -0.0448 -0.0057 13 -3 2 -0.5429 -0.0049 13 -3 3 -0.3489 -0.0012 13 -3 4 0.2414 0.0008 13 -3 5 -0.0703 -0.0165 13 -3 6 -0.2758 -0.0137 13 -3 7 0.0160 0.0160 13 -2 0 -0.2580 -0.0051 13 -2 1 -0.2640 -0.0041 13 -2 2 -0.0527 0.0013 13 -2 3 0.1614 -0.0050 13 -2 4 -0.3670 -0.0109 13 -2 5 -0.5526 -0.0137 13 -2 6 -0.2373 0.0204 13 -1 0 -0.1899 -0.0039 13 -1 1 0.1739 0.0006 13 -1 2 0.1556 -0.0116 13 -1 3 -0.7051 -0.0088 13 -1 4 -0.6782 -0.0092 13 -1 5 -0.2613 0.0181 13 -1 6 0.1293 0.0243 13 0 0 0.1794 -0.0019 13 0 1 0.3528 -0.0138 13 0 2 -0.8046 -0.0063 13 0 3 -0.6048 -0.0024 13 0 4 0.0347 0.0102 13 0 5 0.3420 0.0266 13 1 0 0.6447 -0.0092 13 1 1 -0.5306 -0.0010 13 1 2 -0.4642 0.0030 13 1 3 0.4541 -0.0002 13 1 4 0.5222 0.0210 13 2 0 -0.0193 0.0036 13 2 1 -0.4138 0.0017 13 2 2 0.6806 -0.0105 13 2 3 0.5447 0.0126 13 2 4 0.3729 0.0117 13 3 0 -0.4380 -0.0106 13 3 1 0.5687 -0.0191 13 3 2 0.4777 0.0083 13 3 3 0.1377 0.0279 13 4 0 0.2643 -0.0240 13 4 1 0.4848 0.0135 13 4 2 -0.0387 0.0434 13 5 0 0.5962 0.0293 13 5 1 0.0345 0.0552 13 6 0 0.2722 0.0617 14 -13 0 -0.5301 0.0082 14 -13 1 -0.5255 0.0226 14 -13 2 0.2283 0.0056 14 -13 3 0.0471 -0.0067 14 -12 0 -0.8386 0.0298 14 -12 1 0.2669 0.0116 14 -12 2 0.3572 -0.0161 14 -12 3 0.1901 -0.0090 14 -12 4 0.2251 0.0121 14 -11 0 0.0870 0.0090 14 -11 1 0.7507 -0.0216 14 -11 2 0.0930 -0.0180 14 -11 3 0.2601 0.0165 14 -11 4 0.1829 0.0161 14 -11 5 0.4377 0.0129 14 -10 0 0.8989 -0.0202 14 -10 1 -0.0520 -0.0219 14 -10 2 -0.0091 0.0141 14 -10 3 0.2198 0.0157 14 -10 4 0.3297 0.0067 14 -10 5 0.0631 -0.0044 14 -10 6 -0.3305 -0.0168 14 -9 0 -0.2380 -0.0144 14 -9 1 -0.4955 0.0077 14 -9 2 0.1081 0.0141 14 -9 3 0.1279 0.0034 14 -9 4 -0.2836 0.0026 14 -9 5 -0.8300 -0.0134 14 -9 6 -0.5811 0.0143 14 -8 0 -0.8647 0.0026 14 -8 1 0.0018 0.0079 14 -8 2 0.0370 0.0033 14 -8 3 -0.5400 0.0053 14 -8 4 -1.3093 -0.0102 14 -8 5 -0.8120 0.0037 14 -8 6 -0.3623 0.0103 14 -7 0 0.1449 -0.0011 14 -7 1 0.2039 0.0039 14 -7 2 -0.4037 0.0064 14 -7 3 -1.3961 -0.0068 14 -7 4 -0.7789 -0.0028 14 -7 5 0.0808 0.0106 14 -7 6 0.0265 -0.0128 14 -6 0 0.5569 0.0030 14 -6 1 0.0438 0.0073 14 -6 2 -0.9552 -0.0024 14 -6 3 -0.5477 -0.0028 14 -6 4 0.7300 0.0104 14 -6 5 0.3664 -0.0080 14 -6 6 0.1043 0.0036 14 -5 0 0.4104 0.0070 14 -5 1 -0.2557 0.0015 14 -5 2 -0.2744 0.0019 14 -5 3 1.1088 0.0067 14 -5 4 0.6771 -0.0035 14 -5 5 -0.0199 -0.0021 14 -5 6 -0.0010 0.0269 14 -4 0 0.2790 0.0017 14 -4 1 -0.0568 0.0069 14 -4 2 0.9740 0.0003 14 -4 3 0.7207 -0.0036 14 -4 4 -0.1741 -0.0021 14 -4 5 -0.0268 0.0222 14 -3 0 0.1045 0.0076 14 -3 1 0.5298 -0.0040 14 -3 2 0.4378 -0.0069 14 -3 3 -0.2271 0.0045 14 -3 4 0.0700 0.0155 14 -3 5 0.2350 0.0109 14 -2 0 0.1633 -0.0031 14 -2 1 0.0092 -0.0078 14 -2 2 -0.2193 0.0133 14 -2 3 0.3233 0.0113 14 -2 4 0.4308 0.0056 14 -2 5 0.2028 -0.0258 14 -1 0 -0.2975 -0.0039 14 -1 1 -0.3027 0.0175 14 -1 2 0.5756 0.0083 14 -1 3 0.4721 -0.0029 14 -1 4 0.0579 -0.0204 14 0 0 -0.5208 0.0128 14 0 1 0.6119 0.0027 14 0 2 0.3904 -0.0100 14 0 3 -0.2958 -0.0117 14 1 0 0.3618 -0.0040 14 1 1 0.3255 -0.0100 14 1 2 -0.6289 -0.0025 14 1 3 -0.4809 -0.0187 14 2 0 0.3441 0.0018 14 2 1 -0.7170 0.0059 14 2 2 -0.4341 -0.0172 14 3 0 -0.5433 0.0120 14 3 1 -0.3586 -0.0238 14 4 0 -0.3909 -0.0400 15 -12 0 -0.1347 -0.0073 15 -11 0 -0.7414 0.0290 15 -11 1 -0.0886 0.0243 15 -11 2 -0.2913 -0.0192 15 -11 3 -0.1490 -0.0178 15 -10 0 -0.0110 0.0226 15 -10 1 0.0454 -0.0147 15 -10 2 -0.1044 -0.0210 15 -10 3 0.0043 -0.0028 15 -9 0 0.5235 -0.0089 15 -9 1 0.0238 -0.0190 15 -9 2 0.2169 -0.0042 15 -9 3 0.4523 0.0013 15 -9 4 0.8652 0.0151 15 -8 0 0.0151 -0.0095 15 -8 1 0.1443 -0.0060 15 -8 2 0.5245 0.0008 15 -8 3 1.0838 0.0148 15 -8 4 0.5532 0.0018 15 -7 0 -0.2560 -0.0048 15 -7 1 0.2095 -0.0020 15 -7 2 0.9063 0.0107 15 -7 3 0.3877 0.0030 15 -7 4 -0.4839 -0.0124 15 -6 0 -0.2393 -0.0062 15 -6 1 0.4113 0.0023 15 -6 2 0.1594 -0.0007 15 -6 3 -1.0459 -0.0097 15 -6 4 -0.5379 0.0070 15 -5 0 -0.0646 -0.0053 15 -5 1 0.0170 -0.0061 15 -5 2 -1.1759 -0.0012 15 -5 3 -0.7616 0.0071 15 -5 4 0.0641 0.0042 15 -4 0 -0.0272 -0.0086 15 -4 1 -0.8151 0.0089 15 -4 2 -0.6630 0.0110 15 -4 3 0.2392 -0.0016 15 -4 4 0.0894 -0.0165 15 -3 0 -0.2910 0.0130 15 -3 1 -0.2709 0.0146 15 -3 2 0.2994 -0.0122 15 -3 3 0.0343 -0.0125 15 -2 0 0.1867 0.0125 15 -2 1 0.3125 -0.0202 15 -2 2 -0.1660 -0.0100 15 -2 3 -0.2350 0.0073 15 -1 0 0.4006 -0.0189 15 -1 1 -0.3738 -0.0058 15 -1 2 -0.2274 0.0166 15 0 0 -0.4199 0.0018 15 0 1 -0.1893 0.0202 15 0 2 0.3757 0.0121 15 1 0 -0.2118 0.0131 15 1 1 0.5679 0.0060 15 2 0 0.5564 0.0007 16 -9 0 -0.1122 0.0177 16 -9 1 -0.3908 0.0063 16 -8 0 -0.1379 0.0082 16 -8 1 -0.3070 -0.0049 16 -7 0 0.0328 0.0010 16 -7 1 -0.3075 -0.0124 16 -7 2 -0.0140 -0.0005 16 -6 0 0.0124 -0.0008 16 -6 1 0.0991 0.0042 16 -6 2 0.9723 0.0068 16 -5 0 0.0688 0.0073 16 -5 1 0.8641 -0.0053 16 -5 2 0.5601 -0.0114 16 -4 0 0.4180 -0.0166 16 -4 1 0.3719 -0.0168 16 -3 0 -0.0066 -0.0188 16 -3 1 -0.3323 0.0179 16 -2 0 -0.3159 0.0220 16 -1 0 0.2372 0.0019 0 0 0 0.0 0.0 ; _shelx_fab_checksum 50043 _olex2_submission_special_instructions 'No special instructions were received' 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 0.23521(3) 0.49110(3) 0.29041(3) 0.03511(9) Uani 1 1 d . . . . . O1W O -0.4522(3) 0.0544(3) -0.3612(3) 0.1162(13) Uani 1 1 d D . . . . H1WA H -0.3737(11) 0.067(4) -0.348(4) 0.174 Uiso 1 1 d D U . . . H1WB H -0.489(3) -0.0169(11) -0.4212(8) 0.174 Uiso 1 1 d D U . . . O2W O 0.4994(4) 0.0950(4) 0.2382(5) 0.1618(18) Uani 1 1 d D . . . . H2WA H 0.497(4) 0.062(3) 0.1635(14) 0.243 Uiso 1 1 d D U . . . H2WB H 0.493(6) 0.0367(14) 0.2559(18) 0.243 Uiso 1 1 d D U . . . O12 O 0.3545(3) 0.2699(3) 0.2289(3) 0.0560(8) Uani 0.832(3) 1 d . . P A 1 N11 N 0.2513(3) 0.2998(3) 0.1987(3) 0.0386(7) Uani 0.832(3) 1 d . . P A 1 O11 O 0.0369(3) 0.3694(3) 0.1623(3) 0.0402(7) Uani 0.832(3) 1 d D . P A 1 O13 O -0.1865(4) 0.0326(4) -0.2311(4) 0.0638(10) Uani 0.832(3) 1 d D . P A 1 O14 O 0.2214(3) 0.0474(3) -0.0010(3) 0.0584(8) Uani 0.832(3) 1 d D . P A 1 N12 N -0.0781(3) 0.1971(4) -0.0306(4) 0.0396(7) Uani 0.832(3) 1 d D . P A 1 N13 N 0.0209(4) 0.0453(4) -0.1195(4) 0.0448(7) Uani 0.832(3) 1 d D . P A 1 C11 C 0.0363(4) 0.2690(3) 0.0768(3) 0.0331(8) Uani 0.832(3) 1 d D . P A 1 C12 C -0.0875(4) 0.0874(4) -0.1338(4) 0.0444(7) Uani 0.832(3) 1 d D . P A 1 C13 C 0.1365(4) 0.0993(4) -0.0064(4) 0.0400(8) Uani 0.832(3) 1 d D . P A 1 C14 C 0.1455(4) 0.2195(3) 0.0907(4) 0.0353(8) Uani 0.832(3) 1 d D . P A 1 C15 C -0.1935(4) 0.2421(5) -0.0418(6) 0.0614(12) Uani 0.832(3) 1 d D . P A 1 H15A H -0.181892 0.307557 0.042862 0.092 Uiso 0.832(3) 1 calc R U P A 1 H15B H -0.272871 0.171502 -0.074165 0.092 Uiso 0.832(3) 1 calc R U P A 1 H15C H -0.203047 0.277439 -0.101638 0.092 Uiso 0.832(3) 1 calc R U P A 1 C16 C 0.0123(6) -0.0705(5) -0.2292(4) 0.0660(14) Uani 0.832(3) 1 d D . P A 1 H16A H -0.077623 -0.129229 -0.270548 0.099 Uiso 0.832(3) 1 calc R U P A 1 H16B H 0.074900 -0.110290 -0.198578 0.099 Uiso 0.832(3) 1 calc R U P A 1 H16C H 0.033938 -0.048998 -0.291537 0.099 Uiso 0.832(3) 1 calc R U P A 1 O12A O 0.3186(13) 0.3380(14) 0.2710(14) 0.0560(8) Uani 0.168(3) 1 d . . P A 2 N11A N 0.2761(14) 0.2347(14) 0.1705(14) 0.0386(7) Uani 0.168(3) 1 d . . P A 2 O11A O 0.0671(15) 0.3564(14) 0.1756(15) 0.0402(7) Uani 0.168(3) 1 d D . P A 2 O13A O -0.184(2) 0.052(2) -0.232(2) 0.0638(10) Uani 0.168(3) 1 d D . P A 2 O14A O 0.2039(16) 0.0100(15) -0.0372(18) 0.0584(8) Uani 0.168(3) 1 d D . P A 2 N12A N -0.0594(17) 0.2038(19) -0.0268(17) 0.0396(7) Uani 0.168(3) 1 d D . P A 2 N13A N 0.0080(17) 0.0296(19) -0.1364(17) 0.0448(7) Uani 0.168(3) 1 d D . P A 2 C11A C 0.0533(18) 0.2529(18) 0.0836(17) 0.0331(8) Uani 0.168(3) 1 d D . P A 2 C12A C -0.0843(16) 0.0930(14) -0.1367(14) 0.0444(7) Uani 0.168(3) 1 d D . P A 2 C13A C 0.1306(18) 0.0756(18) -0.0330(18) 0.0400(8) Uani 0.168(3) 1 d D . P A 2 C14A C 0.1528(18) 0.1917(17) 0.0759(19) 0.0353(8) Uani 0.168(3) 1 d D . P A 2 C15A C -0.169(2) 0.258(3) -0.030(3) 0.0614(12) Uani 0.168(3) 1 d D . P A 2 H15D H -0.239752 0.210796 -0.115894 0.092 Uiso 0.168(3) 1 calc R U P A 2 H15E H -0.203503 0.252634 0.033516 0.092 Uiso 0.168(3) 1 calc R U P A 2 H15F H -0.137429 0.346695 -0.009137 0.092 Uiso 0.168(3) 1 calc R U P A 2 C16A C -0.013(3) -0.075(3) -0.2616(19) 0.0660(14) Uani 0.168(3) 1 d D . P A 2 H16D H 0.057984 -0.113671 -0.250678 0.099 Uiso 0.168(3) 1 calc R U P A 2 H16E H -0.098268 -0.138765 -0.294729 0.099 Uiso 0.168(3) 1 calc R U P A 2 H16F H -0.012010 -0.042636 -0.322614 0.099 Uiso 0.168(3) 1 calc R U P A 2 O21 O 0.43142(17) 0.60832(18) 0.37584(16) 0.0380(4) Uani 1 1 d . . . . . O22 O 0.19106(19) 0.4479(2) 0.01591(18) 0.0532(6) Uani 1 1 d . . . . . O23 O 0.7463(2) 0.8462(2) 0.3266(2) 0.0580(6) Uani 1 1 d . . . . . O24 O 0.3852(2) 0.5719(2) -0.03130(19) 0.0609(6) Uani 1 1 d . . . . . N21 N 0.2732(2) 0.5050(2) 0.13122(19) 0.0359(5) Uani 1 1 d . . . . . N22 N 0.58910(19) 0.72539(19) 0.35036(19) 0.0343(5) Uani 1 1 d . . . . . N23 N 0.5623(2) 0.7130(2) 0.1479(2) 0.0424(6) Uani 1 1 d . . . . . C21 C 0.4693(2) 0.6382(2) 0.3024(2) 0.0306(5) Uani 1 1 d . . . . . C22 C 0.6390(3) 0.7672(2) 0.2778(3) 0.0408(7) Uani 1 1 d . . . . . C23 C 0.4409(3) 0.6182(3) 0.0849(3) 0.0386(6) Uani 1 1 d . . . . . C24 C 0.3922(2) 0.5845(2) 0.1667(2) 0.0326(5) Uani 1 1 d . . . . . C25 C 0.6685(3) 0.7857(3) 0.4889(3) 0.0530(8) Uani 1 1 d . . . . . H25A H 0.629653 0.741102 0.527632 0.079 Uiso 0.55(4) 1 calc R U P B 1 H25B H 0.670035 0.874037 0.528891 0.079 Uiso 0.55(4) 1 calc R U P B 1 H25C H 0.758956 0.782276 0.502580 0.079 Uiso 0.55(4) 1 calc R U P B 1 H25D H 0.744368 0.855474 0.511294 0.079 Uiso 0.45(4) 1 calc R U P B 2 H25E H 0.700031 0.723527 0.510972 0.079 Uiso 0.45(4) 1 calc R U P B 2 H25F H 0.614245 0.818413 0.536837 0.079 Uiso 0.45(4) 1 calc R U P B 2 C26 C 0.6152(4) 0.7576(4) 0.0715(3) 0.0686(10) Uani 1 1 d . . . . . H26A H 0.662797 0.848304 0.123075 0.103 Uiso 1 1 calc R U . . . H26B H 0.542378 0.742532 -0.005494 0.103 Uiso 1 1 calc R U . . . H26C H 0.675915 0.711927 0.045910 0.103 Uiso 1 1 calc R U . . . N31 N 0.2362(2) 0.4867(2) 0.4585(2) 0.0380(5) Uani 1 1 d . . . . . C32 C 0.3415(3) 0.5486(3) 0.5713(3) 0.0467(7) Uani 1 1 d . . . . . H32 H 0.421914 0.592250 0.573913 0.056 Uiso 1 1 calc R U . . . C33 C 0.3369(3) 0.5510(3) 0.6830(3) 0.0532(8) Uani 1 1 d . . . . . H33 H 0.412830 0.596286 0.761093 0.064 Uiso 1 1 calc R U . . . C34 C 0.2225(3) 0.4879(3) 0.6805(3) 0.0574(9) Uani 1 1 d . . . . . H34 H 0.217117 0.488633 0.756430 0.069 Uiso 1 1 calc R U . . . C35 C 0.1141(3) 0.4224(3) 0.5643(3) 0.0550(8) Uani 1 1 d . . . . . H35 H 0.033337 0.376478 0.559152 0.066 Uiso 1 1 calc R U . . . C36 C 0.1253(3) 0.4250(3) 0.4578(3) 0.0438(7) Uani 1 1 d . . . . . H36 H 0.050281 0.380414 0.378988 0.053 Uiso 1 1 calc R U . . . N41 N 0.1615(2) 0.6488(2) 0.3299(2) 0.0368(5) Uani 1 1 d . . . . . C42 C 0.0508(3) 0.6454(3) 0.2457(3) 0.0405(6) Uani 1 1 d . . . . . H42 H 0.008173 0.573463 0.163133 0.049 Uiso 1 1 calc R U . . . C43 C -0.0026(3) 0.7434(3) 0.2757(3) 0.0521(8) Uani 1 1 d . . . . . H43 H -0.082281 0.738073 0.215514 0.063 Uiso 1 1 calc R U . . . C44 C 0.0607(4) 0.8484(3) 0.3932(3) 0.0615(9) Uani 1 1 d . . . . . H44 H 0.025296 0.916855 0.415627 0.074 Uiso 1 1 calc R U . . . C45 C 0.1762(4) 0.8543(3) 0.4789(3) 0.0589(9) Uani 1 1 d . . . . . H45 H 0.222726 0.927176 0.560287 0.071 Uiso 1 1 calc R U . . . C46 C 0.2222(3) 0.7522(3) 0.4439(3) 0.0479(8) Uani 1 1 d . . . . . H46 H 0.300937 0.755331 0.503480 0.057 Uiso 1 1 calc R U . . . 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 0.03248(15) 0.03381(16) 0.03005(14) 0.01153(12) 0.00829(11) 0.00433(11) O1W 0.091(2) 0.124(3) 0.088(2) 0.022(2) 0.0051(18) 0.049(2) O2W 0.116(3) 0.154(3) 0.236(5) 0.112(3) 0.058(3) 0.057(3) O12 0.0398(13) 0.0559(16) 0.0594(16) 0.0239(13) 0.0051(11) 0.0177(11) N11 0.0320(13) 0.0408(16) 0.0353(13) 0.0156(12) 0.0094(10) 0.0051(11) O11 0.0314(14) 0.0344(12) 0.0367(11) 0.0066(9) 0.0067(10) 0.0044(9) O13 0.0558(13) 0.058(2) 0.0352(11) 0.0061(12) -0.0045(10) -0.0055(13) O14 0.0618(15) 0.0433(17) 0.065(2) 0.0189(14) 0.0246(14) 0.0208(13) N12 0.0314(14) 0.0356(12) 0.0335(11) 0.0100(10) 0.0035(10) -0.0012(11) N13 0.0562(16) 0.0305(15) 0.0305(14) 0.0056(11) 0.0122(11) 0.0024(12) C11 0.0361(16) 0.0284(15) 0.0286(12) 0.0143(11) 0.0073(11) 0.0014(11) C12 0.0481(16) 0.0385(15) 0.0323(13) 0.0133(12) 0.0085(12) -0.0005(12) C13 0.0477(16) 0.0311(18) 0.0403(19) 0.0156(13) 0.0200(13) 0.0070(13) C14 0.0366(14) 0.0288(18) 0.0321(14) 0.0125(13) 0.0092(11) 0.0020(12) C15 0.037(2) 0.061(2) 0.060(2) 0.017(2) 0.0035(19) 0.0104(18) C16 0.100(3) 0.0444(19) 0.036(2) 0.0076(19) 0.021(2) 0.017(2) O12A 0.0398(13) 0.0559(16) 0.0594(16) 0.0239(13) 0.0051(11) 0.0177(11) N11A 0.0320(13) 0.0408(16) 0.0353(13) 0.0156(12) 0.0094(10) 0.0051(11) O11A 0.0314(14) 0.0344(12) 0.0367(11) 0.0066(9) 0.0067(10) 0.0044(9) O13A 0.0558(13) 0.058(2) 0.0352(11) 0.0061(12) -0.0045(10) -0.0055(13) O14A 0.0618(15) 0.0433(17) 0.065(2) 0.0189(14) 0.0246(14) 0.0208(13) N12A 0.0314(14) 0.0356(12) 0.0335(11) 0.0100(10) 0.0035(10) -0.0012(11) N13A 0.0562(16) 0.0305(15) 0.0305(14) 0.0056(11) 0.0122(11) 0.0024(12) C11A 0.0361(16) 0.0284(15) 0.0286(12) 0.0143(11) 0.0073(11) 0.0014(11) C12A 0.0481(16) 0.0385(15) 0.0323(13) 0.0133(12) 0.0085(12) -0.0005(12) C13A 0.0477(16) 0.0311(18) 0.0403(19) 0.0156(13) 0.0200(13) 0.0070(13) C14A 0.0366(14) 0.0288(18) 0.0321(14) 0.0125(13) 0.0092(11) 0.0020(12) C15A 0.037(2) 0.061(2) 0.060(2) 0.017(2) 0.0035(19) 0.0104(18) C16A 0.100(3) 0.0444(19) 0.036(2) 0.0076(19) 0.021(2) 0.017(2) O21 0.0321(9) 0.0500(11) 0.0278(8) 0.0196(8) 0.0077(7) 0.0063(8) O22 0.0448(11) 0.0566(13) 0.0279(9) 0.0099(9) -0.0026(8) -0.0020(9) O23 0.0434(11) 0.0430(12) 0.0696(14) 0.0153(11) 0.0228(10) -0.0036(9) O24 0.0602(13) 0.0871(16) 0.0345(10) 0.0334(11) 0.0146(9) 0.0144(12) N21 0.0339(11) 0.0355(11) 0.0255(10) 0.0093(9) 0.0039(8) 0.0069(9) N22 0.0292(10) 0.0317(11) 0.0302(10) 0.0100(9) 0.0054(8) 0.0033(8) N23 0.0461(12) 0.0433(13) 0.0457(12) 0.0233(10) 0.0262(10) 0.0111(10) C21 0.0287(11) 0.0287(11) 0.0273(11) 0.0109(9) 0.0047(9) 0.0088(9) C22 0.0385(14) 0.0310(13) 0.0497(15) 0.0148(12) 0.0188(12) 0.0111(10) C23 0.0418(14) 0.0427(14) 0.0347(12) 0.0208(11) 0.0147(10) 0.0147(11) C24 0.0305(11) 0.0346(12) 0.0270(11) 0.0124(10) 0.0071(9) 0.0092(9) C25 0.0390(15) 0.0526(18) 0.0364(15) 0.0085(14) -0.0010(12) -0.0004(13) C26 0.081(2) 0.075(2) 0.072(2) 0.0448(18) 0.0476(17) 0.0182(18) N31 0.0381(11) 0.0373(11) 0.0353(11) 0.0163(9) 0.0114(9) 0.0108(9) C32 0.0379(14) 0.0558(17) 0.0390(14) 0.0232(13) 0.0086(11) 0.0050(12) C33 0.0496(17) 0.064(2) 0.0354(14) 0.0237(14) 0.0068(13) 0.0099(15) C34 0.0596(19) 0.079(2) 0.0409(15) 0.0336(15) 0.0223(13) 0.0201(16) C35 0.0450(16) 0.071(2) 0.0535(17) 0.0360(15) 0.0208(13) 0.0090(14) C36 0.0411(15) 0.0473(16) 0.0402(14) 0.0218(12) 0.0128(11) 0.0087(12) N41 0.0389(11) 0.0332(11) 0.0304(10) 0.0117(9) 0.0105(9) 0.0063(9) C42 0.0429(14) 0.0400(14) 0.0356(13) 0.0174(11) 0.0127(11) 0.0113(11) C43 0.0577(18) 0.0545(17) 0.0532(17) 0.0305(14) 0.0219(14) 0.0253(14) C44 0.085(2) 0.0457(17) 0.071(2) 0.0305(16) 0.0411(18) 0.0355(16) C45 0.077(2) 0.0350(16) 0.0493(18) 0.0081(14) 0.0227(16) 0.0136(15) C46 0.0484(16) 0.0381(15) 0.0365(14) 0.0070(12) 0.0079(12) 0.0060(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 O11 Zn1 N11 74.21(10) . . ? O11 Zn1 N21 90.47(11) . . ? O12A Zn1 N21 93.1(4) . . ? O11A Zn1 O12A 84.8(6) . . ? O11A Zn1 O21 165.0(5) . . ? O11A Zn1 N21 92.8(6) . . ? O11A Zn1 N31 96.0(6) . . ? O11A Zn1 N41 98.4(4) . . ? O21 Zn1 N11 103.51(9) . . ? O21 Zn1 O11 166.61(11) . . ? O21 Zn1 O12A 85.8(4) . . ? O21 Zn1 N21 76.15(7) . . ? O21 Zn1 N41 92.00(8) . . ? N21 Zn1 N11 83.69(10) . . ? N31 Zn1 N11 94.99(10) . . ? N31 Zn1 O11 99.16(12) . . ? N31 Zn1 O12A 82.2(4) . . ? N31 Zn1 O21 94.17(8) . . ? N31 Zn1 N21 169.56(8) . . ? N31 Zn1 N41 92.72(9) . . ? N41 Zn1 N11 162.09(9) . . ? N41 Zn1 O11 88.62(9) . . ? N41 Zn1 O12A 174.2(4) . . ? N41 Zn1 N21 91.53(9) . . ? H1WA O1W H1WB 105.5(16) . . ? H2WA O2W H2WB 104.1(16) . . ? O12 N11 Zn1 125.1(2) . . ? O12 N11 C14 120.8(3) . . ? C14 N11 Zn1 113.2(2) . . ? C11 O11 Zn1 111.6(2) . . ? C11 N12 C12 123.2(3) . . ? C11 N12 C15 118.9(3) . . ? C12 N12 C15 117.7(3) . . ? C12 N13 C13 125.5(3) . . ? C12 N13 C16 117.0(3) . . ? C13 N13 C16 117.3(3) . . ? O11 C11 N12 118.6(3) . . ? O11 C11 C14 123.0(3) . . ? N12 C11 C14 118.2(3) . . ? O13 C12 N12 121.2(4) . . ? O13 C12 N13 122.2(4) . . ? N13 C12 N12 116.6(3) . . ? O14 C13 N13 119.8(3) . . ? O14 C13 C14 125.6(3) . . ? N13 C13 C14 114.4(3) . . ? N11 C14 C11 112.1(3) . . ? N11 C14 C13 127.0(3) . . ? C13 C14 C11 120.8(3) . . ? N12 C15 H15A 109.5 . . ? N12 C15 H15B 109.5 . . ? N12 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N13 C16 H16A 109.5 . . ? N13 C16 H16B 109.5 . . ? N13 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N11A O12A Zn1 123.5(12) . . ? O12A N11A C14A 123.5(16) . . ? C11A O11A Zn1 125.0(14) . . ? C11A N12A C12A 123.1(13) . . ? C11A N12A C15A 121.4(15) . . ? C12A N12A C15A 115.1(14) . . ? C12A N13A C13A 123.2(13) . . ? C12A N13A C16A 116.1(16) . . ? C13A N13A C16A 119.2(16) . . ? O11A C11A N12A 117.3(14) . . ? O11A C11A C14A 125.4(13) . . ? N12A C11A C14A 116.6(13) . . ? O13A C12A N12A 121.6(17) . . ? O13A C12A N13A 119.7(16) . . ? N13A C12A N12A 118.6(13) . . ? O14A C13A N13A 119.1(14) . . ? O14A C13A C14A 124.8(15) . . ? N13A C13A C14A 115.8(13) . . ? N11A C14A C11A 124.8(13) . . ? N11A C14A C13A 113.0(14) . . ? C13A C14A C11A 122.1(13) . . ? N12A C15A H15D 109.5 . . ? N12A C15A H15E 109.5 . . ? N12A C15A H15F 109.5 . . ? H15D C15A H15E 109.5 . . ? H15D C15A H15F 109.5 . . ? H15E C15A H15F 109.5 . . ? N13A C16A H16D 109.5 . . ? N13A C16A H16E 109.5 . . ? N13A C16A H16F 109.5 . . ? H16D C16A H16E 109.5 . . ? H16D C16A H16F 109.5 . . ? H16E C16A H16F 109.5 . . ? C21 O21 Zn1 114.08(14) . . ? O22 N21 Zn1 124.38(18) . . ? O22 N21 C24 121.7(2) . . ? C24 N21 Zn1 113.91(16) . . ? C21 N22 C22 124.1(2) . . ? C21 N22 C25 118.8(2) . . ? C22 N22 C25 117.0(2) . . ? C22 N23 C23 124.9(2) . . ? C22 N23 C26 116.9(2) . . ? C23 N23 C26 118.3(2) . . ? O21 C21 N22 119.6(2) . . ? O21 C21 C24 123.3(2) . . ? N22 C21 C24 117.1(2) . . ? O23 C22 N22 121.0(3) . . ? O23 C22 N23 122.0(3) . . ? N23 C22 N22 117.0(2) . . ? O24 C23 N23 119.4(3) . . ? O24 C23 C24 125.5(3) . . ? N23 C23 C24 115.0(2) . . ? N21 C24 C21 112.0(2) . . ? N21 C24 C23 126.3(2) . . ? C23 C24 C21 121.7(2) . . ? N22 C25 H25A 109.5 . . ? N22 C25 H25B 109.5 . . ? N22 C25 H25C 109.5 . . ? N22 C25 H25D 109.5 . . ? N22 C25 H25E 109.5 . . ? N22 C25 H25F 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? H25D C25 H25E 109.5 . . ? H25D C25 H25F 109.5 . . ? H25E C25 H25F 109.5 . . ? N23 C26 H26A 109.5 . . ? N23 C26 H26B 109.5 . . ? N23 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C32 N31 Zn1 123.7(2) . . ? C36 N31 Zn1 119.09(18) . . ? C36 N31 C32 117.2(3) . . ? N31 C32 H32 118.7 . . ? N31 C32 C33 122.5(3) . . ? C33 C32 H32 118.7 . . ? C32 C33 H33 120.3 . . ? C34 C33 C32 119.4(3) . . ? C34 C33 H33 120.3 . . ? C33 C34 H34 120.8 . . ? C33 C34 C35 118.5(3) . . ? C35 C34 H34 120.8 . . ? C34 C35 H35 120.5 . . ? C36 C35 C34 119.0(3) . . ? C36 C35 H35 120.5 . . ? N31 C36 C35 123.4(3) . . ? N31 C36 H36 118.3 . . ? C35 C36 H36 118.3 . . ? C42 N41 Zn1 122.01(18) . . ? C46 N41 Zn1 119.67(19) . . ? C46 N41 C42 118.2(2) . . ? N41 C42 H42 119.1 . . ? N41 C42 C43 121.9(3) . . ? C43 C42 H42 119.1 . . ? C42 C43 H43 120.5 . . ? C44 C43 C42 119.0(3) . . ? C44 C43 H43 120.5 . . ? C43 C44 H44 120.2 . . ? C43 C44 C45 119.5(3) . . ? C45 C44 H44 120.2 . . ? C44 C45 H45 120.8 . . ? C46 C45 C44 118.3(3) . . ? C46 C45 H45 120.8 . . ? N41 C46 C45 122.9(3) . . ? N41 C46 H46 118.5 . . ? C45 C46 H46 118.5 . . ? 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 N11 2.203(3) . ? Zn1 O11 2.155(3) . ? Zn1 O12A 2.164(14) . ? Zn1 O11A 1.959(14) . ? Zn1 O21 2.0972(17) . ? Zn1 N21 2.182(2) . ? Zn1 N31 2.087(2) . ? Zn1 N41 2.133(2) . ? O1W H1WA 0.816(10) . ? O1W H1WB 0.815(9) . ? O2W H2WA 0.832(9) . ? O2W H2WB 0.819(10) . ? O12 N11 1.255(4) . ? N11 C14 1.343(4) . ? O11 C11 1.248(4) . ? O13 C12 1.209(4) . ? O14 C13 1.214(4) . ? N12 C11 1.374(4) . ? N12 C12 1.386(4) . ? N12 C15 1.463(5) . ? N13 C12 1.373(5) . ? N13 C13 1.413(4) . ? N13 C16 1.473(5) . ? C11 C14 1.434(5) . ? C13 C14 1.433(4) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? O12A N11A 1.25(2) . ? N11A C14A 1.37(2) . ? O11A C11A 1.258(14) . ? O13A C12A 1.207(14) . ? O14A C13A 1.222(15) . ? N12A C11A 1.382(14) . ? N12A C12A 1.387(14) . ? N12A C15A 1.472(15) . ? N13A C12A 1.375(14) . ? N13A C13A 1.409(14) . ? N13A C16A 1.475(15) . ? C11A C14A 1.430(15) . ? C13A C14A 1.425(15) . ? C15A H15D 0.9800 . ? C15A H15E 0.9800 . ? C15A H15F 0.9800 . ? C16A H16D 0.9800 . ? C16A H16E 0.9800 . ? C16A H16F 0.9800 . ? O21 C21 1.249(3) . ? O22 N21 1.264(2) . ? O23 C22 1.214(3) . ? O24 C23 1.217(3) . ? N21 C24 1.343(3) . ? N22 C21 1.360(3) . ? N22 C22 1.386(4) . ? N22 C25 1.467(3) . ? N23 C22 1.383(4) . ? N23 C23 1.395(3) . ? N23 C26 1.466(4) . ? C21 C24 1.441(3) . ? C23 C24 1.431(4) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C25 H25D 0.9800 . ? C25 H25E 0.9800 . ? C25 H25F 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? N31 C32 1.347(3) . ? N31 C36 1.334(4) . ? C32 H32 0.9500 . ? C32 C33 1.379(4) . ? C33 H33 0.9500 . ? C33 C34 1.363(5) . ? C34 H34 0.9500 . ? C34 C35 1.388(4) . ? C35 H35 0.9500 . ? C35 C36 1.364(4) . ? C36 H36 0.9500 . ? N41 C42 1.344(3) . ? N41 C46 1.334(3) . ? C42 H42 0.9500 . ? C42 C43 1.378(4) . ? C43 H43 0.9500 . ? C43 C44 1.368(4) . ? C44 H44 0.9500 . ? C44 C45 1.378(5) . ? C45 H45 0.9500 . ? C45 C46 1.372(4) . ? C46 H46 0.9500 . ? 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 O1W H1WA O13 0.816(10) 2.37(4) 3.036(5) 140(5) . yes O1W H1WA O13A 0.816(10) 2.26(4) 2.96(2) 143(6) . yes O1W H1WB O1W 0.815(9) 2.393(10) 2.897(7) 120.9(9) 2_454 yes O2W H2WB O1W 0.819(10) 2.11(2) 2.868(7) 155(4) 2 yes C25 H25B O13 0.98 2.60 3.237(5) 123.0 1_666 yes C26 H26C O22 0.98 2.62 3.588(5) 167.6 2_665 yes C32 H32 O12 0.95 2.62 3.297(4) 129.0 2_666 yes C32 H32 O21 0.95 2.55 3.140(4) 120.3 . yes C36 H36 O11 0.95 2.57 3.227(4) 126.1 . yes C36 H36 O11A 0.95 2.47 3.065(19) 120.9 . yes C42 H42 O11 0.95 2.55 3.052(4) 113.5 . yes C42 H42 O22 0.95 2.53 3.165(3) 124.8 2_565 yes C43 H43 O22 0.95 2.59 3.183(4) 121.2 2_565 yes C45 H45 O23 0.95 2.45 3.250(4) 142.1 2_676 yes 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Zn1 N11 C14 C11 -13.0(5) . . . . ? Zn1 N11 C14 C13 164.6(5) . . . . ? Zn1 O11 C11 N12 -163.0(4) . . . . ? Zn1 O11 C11 C14 22.9(6) . . . . ? Zn1 O12A N11A C14A -19(3) . . . . ? Zn1 O11A C11A N12A -142(2) . . . . ? Zn1 O11A C11A C14A 27(4) . . . . ? Zn1 O21 C21 N22 172.38(18) . . . . ? Zn1 O21 C21 C24 -7.7(3) . . . . ? Zn1 N21 C24 C21 2.4(3) . . . . ? Zn1 N21 C24 C23 -176.0(2) . . . . ? Zn1 N31 C32 C33 175.6(2) . . . . ? Zn1 N31 C36 C35 -176.4(3) . . . . ? Zn1 N41 C42 C43 174.5(2) . . . . ? Zn1 N41 C46 C45 -176.1(3) . . . . ? O12 N11 C14 C11 177.4(4) . . . . ? O12 N11 C14 C13 -5.1(7) . . . . ? O11 C11 C14 N11 -6.7(7) . . . . ? O11 C11 C14 C13 175.5(5) . . . . ? O14 C13 C14 N11 5.7(9) . . . . ? O14 C13 C14 C11 -177.0(5) . . . . ? N12 C11 C14 N11 179.1(5) . . . . ? N12 C11 C14 C13 1.4(8) . . . . ? N13 C13 C14 N11 -169.7(5) . . . . ? N13 C13 C14 C11 7.7(8) . . . . ? C11 N12 C12 O13 -173.7(6) . . . . ? C11 N12 C12 N13 6.2(8) . . . . ? C12 N12 C11 O11 176.7(5) . . . . ? C12 N12 C11 C14 -8.9(8) . . . . ? C12 N13 C13 O14 173.4(6) . . . . ? C12 N13 C13 C14 -11.0(8) . . . . ? C13 N13 C12 O13 -175.7(6) . . . . ? C13 N13 C12 N12 4.4(8) . . . . ? C15 N12 C11 O11 1.2(8) . . . . ? C15 N12 C11 C14 175.6(6) . . . . ? C15 N12 C12 O13 1.9(9) . . . . ? C15 N12 C12 N13 -178.3(6) . . . . ? C16 N13 C12 O13 0.5(9) . . . . ? C16 N13 C12 N12 -179.4(5) . . . . ? C16 N13 C13 O14 -2.8(8) . . . . ? C16 N13 C13 C14 172.8(5) . . . . ? O12A N11A C14A C11A -6(4) . . . . ? O12A N11A C14A C13A 176(2) . . . . ? O11A C11A C14A N11A 3(5) . . . . ? O11A C11A C14A C13A -179(3) . . . . ? O14A C13A C14A N11A 10(4) . . . . ? O14A C13A C14A C11A -169(3) . . . . ? N12A C11A C14A N11A 173(3) . . . . ? N12A C11A C14A C13A -9(4) . . . . ? N13A C13A C14A N11A -177(3) . . . . ? N13A C13A C14A C11A 4(4) . . . . ? C11A N12A C12A O13A 179(3) . . . . ? C11A N12A C12A N13A -1(4) . . . . ? C12A N12A C11A O11A 178(3) . . . . ? C12A N12A C11A C14A 7(4) . . . . ? C12A N13A C13A O14A 176(3) . . . . ? C12A N13A C13A C14A 2(4) . . . . ? C13A N13A C12A O13A 176(3) . . . . ? C13A N13A C12A N12A -4(4) . . . . ? C15A N12A C11A O11A -10(5) . . . . ? C15A N12A C11A C14A 179(3) . . . . ? C15A N12A C12A O13A 7(4) . . . . ? C15A N12A C12A N13A -173(3) . . . . ? C16A N13A C12A O13A 10(4) . . . . ? C16A N13A C12A N12A -170(3) . . . . ? C16A N13A C13A O14A -19(5) . . . . ? C16A N13A C13A C14A 168(3) . . . . ? O21 C21 C24 N21 3.5(4) . . . . ? O21 C21 C24 C23 -178.0(3) . . . . ? O22 N21 C24 C21 -179.8(2) . . . . ? O22 N21 C24 C23 1.8(4) . . . . ? O24 C23 C24 N21 -6.1(5) . . . . ? O24 C23 C24 C21 175.6(3) . . . . ? N22 C21 C24 N21 -176.6(2) . . . . ? N22 C21 C24 C23 1.9(4) . . . . ? N23 C23 C24 N21 173.4(2) . . . . ? N23 C23 C24 C21 -4.8(4) . . . . ? C21 N22 C22 O23 179.4(3) . . . . ? C21 N22 C22 N23 -2.0(4) . . . . ? C22 N22 C21 O21 -178.4(2) . . . . ? C22 N22 C21 C24 1.7(4) . . . . ? C22 N23 C23 O24 -175.7(3) . . . . ? C22 N23 C23 C24 4.7(4) . . . . ? C23 N23 C22 O23 177.1(3) . . . . ? C23 N23 C22 N22 -1.5(4) . . . . ? C25 N22 C21 O21 -2.3(4) . . . . ? C25 N22 C21 C24 177.8(2) . . . . ? C25 N22 C22 O23 3.2(4) . . . . ? C25 N22 C22 N23 -178.1(2) . . . . ? C26 N23 C22 O23 -1.5(4) . . . . ? C26 N23 C22 N22 179.9(3) . . . . ? C26 N23 C23 O24 2.9(4) . . . . ? C26 N23 C23 C24 -176.7(3) . . . . ? N31 C32 C33 C34 0.6(5) . . . . ? C32 N31 C36 C35 0.4(5) . . . . ? C32 C33 C34 C35 0.3(5) . . . . ? C33 C34 C35 C36 -0.9(5) . . . . ? C34 C35 C36 N31 0.5(5) . . . . ? C36 N31 C32 C33 -0.9(5) . . . . ? N41 C42 C43 C44 1.7(5) . . . . ? C42 N41 C46 C45 0.5(5) . . . . ? C42 C43 C44 C45 0.1(5) . . . . ? C43 C44 C45 C46 -1.5(6) . . . . ? C44 C45 C46 N41 1.2(5) . . . . ? C46 N41 C42 C43 -2.0(4) . . . . ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 0.277 0.799 0.802 36.3 3.1 ? 2 0.723 0.201 0.198 36.3 3.2 ?