#------------------------------------------------------------------------------ #$Date: 2024-06-13 05:30:55 +0300 (Thu, 13 Jun 2024) $ #$Revision: 292346 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/18/1571854.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_1571854 loop_ _publ_author_name 'Carroll, Robert C.' 'Coles, Simon J.' _publ_section_title ; Statistical optimization of guest uptake in crystalline sponges: grading structural outcomes. ; _journal_coeditor_code LT5068 _journal_issue 4 _journal_name_full IUCrJ _journal_paper_doi 10.1107/S2052252524004871 _journal_volume 11 _journal_year 2024 _chemical_formula_moiety 'C36 H24 I6 N12 Zn3' _chemical_formula_sum 'C36 H24 I6 N12 Zn3' _chemical_formula_weight 1582.18 _chemical_name_systematic catena-[bis(mu-2,4,6-tri(pyridin-4-yl)-1,3,5-triazine)-hexaiodo-tri-zinc _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2024-01-26 _audit_creation_method ; Olex2 1.5-alpha (compiled 2023.11.24 svn.r209d9fb2 for OlexSys, GUI svn.r6869) ; _cell_angle_alpha 90 _cell_angle_beta 100.709(4) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 34.4156(9) _cell_length_b 15.0804(3) _cell_length_c 30.0607(16) _cell_measurement_reflns_used 8194 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 74.1470 _cell_measurement_theta_min 2.5940 _cell_volume 15329.8(10) _computing_cell_refinement 'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)' _computing_data_collection 'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)' _computing_data_reduction 'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)' _computing_molecular_graphics 'Olex2 1.5-alpha (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5-alpha (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2016/6 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.00(10) _diffrn_detector 'hybrid pixel array detector' _diffrn_detector_area_resol_mean 10 _diffrn_detector_dtime 0.000 _diffrn_detector_type 'Rigaku, HyPix Arc-100' _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.994 _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 -106.00 -37.00 0.50 4.00 -- -103.00 112.00 -53.00 138 2 \w -150.00-125.00 0.50 4.00 -- -103.00-112.00-145.00 50 3 \w -65.00 -40.00 0.50 4.00 -- -103.00 61.00 150.00 50 4 \w -116.00 -90.00 0.50 4.00 -- -103.00 -45.00-150.00 52 5 \w -172.00-136.00 0.50 4.00 -- -103.00 -45.00-150.00 72 6 \w -62.00 -33.00 0.50 4.00 -- -103.00 61.00 -30.00 58 7 \w -173.00 -94.00 0.50 4.00 -- -103.00 -30.00 120.00 158 8 \w -58.00 -33.00 0.50 4.00 -- -103.00 61.00 120.00 50 9 \w 67.00 94.00 0.50 4.00 -- 101.75-112.00-145.00 54 10 \w 90.00 135.00 0.50 4.00 -- 101.75 112.00 -53.00 90 11 \w 29.00 106.00 0.50 4.00 -- 101.75 -94.00-150.00 154 12 \w 33.00 65.00 0.50 4.00 -- 101.75-125.00 60.00 64 13 \w 140.00 166.00 0.50 4.00 -- 101.75 61.00 -90.00 52 14 \w 30.00 65.00 0.50 4.00 -- 101.75 -61.00-150.00 70 15 \w 85.00 134.00 0.50 4.00 -- 101.75 61.00 -90.00 98 16 \w 38.00 69.00 0.50 4.00 -- 101.75 -61.00-120.00 62 17 \w 63.00 106.00 0.50 4.00 -- 101.75 -94.00-120.00 86 18 \w 43.00 69.00 0.50 4.00 -- 101.75 -61.00 -90.00 52 19 \w 29.00 65.00 0.50 4.00 -- 101.75 -61.00 0.00 72 20 \w 77.00 110.00 0.50 4.00 -- 101.75-125.00 60.00 66 21 \w 34.00 65.00 0.50 4.00 -- 101.75 -61.00 60.00 62 22 \w 93.00 146.00 0.50 4.00 -- 101.75 125.00 60.00 106 23 \w -83.00 -12.00 0.50 1.00 -- -46.26 112.00 -53.00 142 24 \w 26.00 61.00 0.50 1.00 -- 46.26-112.00-145.00 70 25 \w -6.00 29.00 0.50 1.00 -- -46.26 19.00-150.00 70 26 \w -117.00 -24.00 0.50 1.00 -- -46.26 -77.00-150.00 186 27 \w -22.00 24.00 0.50 1.00 -- -46.26 19.00 -60.00 92 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_details 'Rigaku, UG2 \k goniometer' _diffrn_measurement_device_type ; Rigaku 007HF diffractometer equipped with Arc)Sec VHF Varimax confocal mirrors and a UG2 goniometer and HyPix Arc-100 detector ; _diffrn_measurement_method 'profile data from \w-scans' _diffrn_measurement_specimen_support 'MiTeGen loops' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0015512000 _diffrn_orient_matrix_UB_12 -0.0164678000 _diffrn_orient_matrix_UB_13 -0.0501930000 _diffrn_orient_matrix_UB_21 0.0084093000 _diffrn_orient_matrix_UB_22 -0.0989764000 _diffrn_orient_matrix_UB_23 0.0102544000 _diffrn_orient_matrix_UB_31 -0.0447689000 _diffrn_orient_matrix_UB_32 -0.0191551000 _diffrn_orient_matrix_UB_33 -0.0097082000 _diffrn_radiation_collimation 0.3 _diffrn_radiation_monochromator 'Arc)Sec VHF Varimax focusing mirrors' _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0507 _diffrn_reflns_av_unetI/netI 0.0437 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_number 53521 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 68.243 _diffrn_reflns_theta_min 2.613 _diffrn_source 'Rotating anode' _diffrn_source_current 30.0 _diffrn_source_power 1.2 _diffrn_source_target Cu _diffrn_source_type 'Rigaku 007 HF' _diffrn_source_voltage 40.0 _exptl_absorpt_coefficient_mu 20.269 _exptl_absorpt_correction_T_max 0.425 _exptl_absorpt_correction_T_min 0.116 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.371 _exptl_crystal_description block _exptl_crystal_F_000 5856 _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.06 _refine_diff_density_max 1.781 _refine_diff_density_min -0.980 _refine_diff_density_rms 0.146 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 616 _refine_ls_number_reflns 13960 _refine_ls_number_restraints 22 _refine_ls_restrained_S_all 1.094 _refine_ls_R_factor_all 0.1041 _refine_ls_R_factor_gt 0.0864 _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^)+(0.1966P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2709 _refine_ls_wR_factor_ref 0.2890 _reflns_Friedel_coverage 0.000 _reflns_number_gt 9409 _reflns_number_total 13960 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file lt5068.cif _cod_data_source_block 25_10_24c _cod_database_code 1571854 _shelx_shelxl_version_number 2016/6 _chemical_oxdiff_formula '(Zn3 I6 N12 H24 C36) (C15 H16 O3)2 (C6 H12)2' _chemical_oxdiff_usercomment 9300-04 _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 0.376 _shelx_estimated_absorpt_t_min 0.140 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2. Restrained distances I401-Zn41 \\sim I301-Zn31 with sigma of 0.02 I402-Zn41 \\sim I302-Zn31 with sigma of 0.02 Zn41-N301 \\sim Zn31-N301 with sigma of 0.02 I401-I402 \\sim I301-I302 with sigma of 0.04 I401-N301 \\sim I301-N301 with sigma of 0.04 I402-N301 \\sim I302-N301 with sigma of 0.04 I404-Zn42 \\sim I304-Zn32 with sigma of 0.02 I403-Zn42 \\sim I303-Zn32 with sigma of 0.02 Zn42-N305 \\sim Zn32-N305 with sigma of 0.02 I404-I403 \\sim I304-I303 with sigma of 0.04 I404-N305 \\sim I304-N305 with sigma of 0.04 I403-N305 \\sim I303-N305 with sigma of 0.04 I305-Zn33 \\sim I405-Zn43 with sigma of 0.02 I306-Zn33 \\sim I406-Zn43 with sigma of 0.02 Zn33-N306 \\sim Zn43-N306 with sigma of 0.02 Zn33-N307 \\sim Zn43-N307 with sigma of 0.02 I305-I306 \\sim I405-I406 with sigma of 0.04 I305-N306 \\sim I405-N306 with sigma of 0.04 I305-N307 \\sim I405-N307 with sigma of 0.04 I306-N306 \\sim I406-N306 with sigma of 0.04 I306-N307 \\sim I406-N307 with sigma of 0.04 3. Others 1*[Sof(I401)+Sof(I402)+Sof(Zn41)]+1*[Sof(I302)+Sof(Zn31)+Sof(I301)]+1* [Sof(I502)+Sof(I501)+Sof(Zn51)]=1 with esd of 0.00001 Sof(I401)=Sof(I402)=Sof(Zn41)=FVAR(1) Sof(I302)=Sof(Zn31)=Sof(I301)=FVAR(2) Sof(I502)=Sof(I501)=Sof(Zn51)=FVAR(3) Fixed Sof: I404(0.28968) I403(0.28968) I305(0.55511) Zn42(0.28968) I306(0.55511) Zn33(0.55511) Zn32(0.68587) I303(0.68587) I304(0.68587) I504(0.02445) I503(0.02445) Zn52(0.02445) I405(0.44489) Zn43(0.44489) I406(0.44489) Fixed Uiso: I502(0.08) I501(0.08) Zn51(0.08) I504(0.08) I503(0.08) Zn52(0.08) 4.a Aromatic/amide H refined with riding coordinates: C313(H313), C312(H312), C332(H332), C317(H317), C311(H311), C319(H319), C310(H310), C333(H333), C322(H322), C336(H336), C318(H318), C320(H320), C323(H323), C305(H305), C328(H328), C329(H329), C301(H301), C330(H330), C304(H304), C331(H331), C335(H335), C302(H302), C315(H315), C314(H314) ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL 2023ncs7022a_rc1_a.res in C2/c 2023ncs7022a_rc1.res created by SHELXL-2016/6 at 09:42:00 on 26-Jan-2024 REM Old TITL 2023NCS7022a_RC1 in C2/c REM SHELXT solution in C2/c REM R1 0.450, Rweak 0.100, Alpha 0.144, Orientation as input REM Formula found by SHELXT: C39 N7 O Zn7 I304 CELL 1.54184 34.4156 15.0804 30.0607 90 100.709 90 ZERR 8 0.0009 0.0003 0.0016 0 0.004 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H I N Zn UNIT 288 192 48 96 24 SADI I401 Zn41 I301 Zn31 SADI I402 Zn41 I302 Zn31 SADI Zn41 N301 Zn31 N301 SADI 0.04 I401 I402 I301 I302 SADI 0.04 I401 N301 I301 N301 SADI 0.04 I402 N301 I302 N301 SADI I404 Zn42 I304 Zn32 SADI I403 Zn42 I303 Zn32 SADI Zn42 N305 Zn32 N305 SADI 0.04 I404 I403 I304 I303 SADI 0.04 I404 N305 I304 N305 SADI 0.04 I403 N305 I303 N305 SADI I305 Zn33 I405 Zn43 SADI I306 Zn33 I406 Zn43 SADI Zn33 N306 Zn43 N306 SADI Zn33 N307 Zn43 N307 SADI 0.04 I305 I306 I405 I406 SADI 0.04 I305 N306 I405 N306 SADI 0.04 I305 N307 I405 N307 SADI 0.04 I306 N306 I406 N306 SADI 0.04 I306 N307 I406 N307 SUMP 1 0.00001 1 2 1 3 1 4 L.S. 10 PLAN 67 SIZE 0.06 0.11 0.16 TEMP -173 CONF FREE Zn51 C301 BOND $H LIST 6 MORE -1 ABIN fmap 2 acta OMIT 1 3 0 REM REM REM WGHT 0.196600 FVAR 0.07186 0.41808 0.55376 0.02816 PART 1 I404 3 0.378314 -0.226451 0.438518 10.28968 0.24492 0.05372 = 0.19816 0.02147 -0.11320 -0.04864 I403 3 0.480340 -0.145632 0.368136 10.28968 0.25555 0.12555 = 0.27268 -0.03135 -0.11546 0.10708 I305 3 0.619393 0.736946 0.574505 10.55511 0.13930 0.04639 = 0.27435 0.01572 -0.12976 -0.00545 ZN42 5 0.419766 -0.116898 0.402591 10.28968 0.17122 0.03971 = 0.25702 -0.00565 -0.11954 0.01775 I306 3 0.658389 0.552764 0.470495 10.55511 0.11142 0.22873 = 0.18536 0.12083 -0.04027 -0.03459 I401 3 0.376202 0.342963 0.807237 21.00000 0.16814 0.05019 = 0.10258 0.00704 0.00688 0.01621 I402 3 0.270420 0.265857 0.708057 21.00000 0.12837 0.04848 = 0.18325 -0.02722 0.03408 -0.01599 ZN33 5 0.634191 0.583883 0.541679 10.55511 0.11272 0.06350 = 0.21217 0.03469 -0.08692 -0.02458 ZN41 5 0.330874 0.361491 0.731546 21.00000 0.11170 0.03503 = 0.10718 -0.00567 0.00779 0.00424 PART 0 N303 4 0.429452 0.222611 0.560388 11.00000 0.08463 0.06073 = 0.09840 -0.01391 -0.01062 -0.00379 N310 4 0.818303 0.319846 0.749875 11.00000 0.08613 0.02284 = 0.15588 0.01230 -0.02405 -0.00106 N308 4 0.781093 0.446962 0.724609 11.00000 0.07975 0.03135 = 0.12192 0.00128 -0.02007 -0.01123 N309 4 0.766902 0.310556 0.685917 11.00000 0.08470 0.03527 = 0.13296 -0.00100 -0.02386 -0.01456 N312 4 0.880136 0.550123 0.859250 11.00000 0.07819 0.05136 = 0.09343 0.01347 -0.01240 -0.00378 N302 4 0.464813 0.356442 0.582756 11.00000 0.08434 0.05269 = 0.10928 -0.00948 -0.03061 -0.00117 N305 4 0.437272 -0.022619 0.452068 11.00000 0.10154 0.05080 = 0.10464 -0.00664 -0.01659 -0.01322 N304 4 0.482171 0.268171 0.525540 11.00000 0.09844 0.04935 = 0.08430 -0.00266 -0.02852 -0.01682 N306 4 0.582953 0.513995 0.546766 11.00000 0.10048 0.06714 = 0.12631 0.01820 -0.03129 -0.01464 C309 1 0.450880 0.128541 0.503843 11.00000 0.07926 0.04756 = 0.07841 -0.00229 -0.00731 -0.00208 C316 1 0.519532 0.401069 0.550230 11.00000 0.08452 0.04698 = 0.10617 -0.00384 -0.03548 -0.00191 C326 1 0.810148 0.405031 0.752085 11.00000 0.06561 0.03887 = 0.10935 0.00221 -0.01025 -0.00587 C306 1 0.436313 0.295995 0.586111 11.00000 0.09899 0.04346 = 0.09249 -0.00249 -0.01870 0.00189 C313 1 0.474959 0.110382 0.474135 11.00000 0.08180 0.05421 = 0.10298 -0.00967 -0.02555 -0.00221 AFIX 43 H313 2 0.496196 0.148896 0.471259 11.00000 -1.20000 AFIX 0 N301 4 0.358398 0.343505 0.676857 11.00000 0.22240 0.04174 = 0.16245 0.00804 0.07962 0.02065 C325 1 0.795139 0.275393 0.716353 11.00000 0.08364 0.03844 = 0.11324 -0.00080 -0.00522 -0.00892 C312 1 0.467960 0.035057 0.448290 11.00000 0.06810 0.06775 = 0.09671 0.00266 -0.01252 -0.00663 AFIX 43 H312 2 0.484579 0.021972 0.427205 11.00000 -1.20000 AFIX 0 C327 1 0.801587 0.177408 0.716759 11.00000 0.11027 0.03971 = 0.12666 0.01177 -0.00680 0.00003 C324 1 0.760637 0.396671 0.691164 11.00000 0.08423 0.04509 = 0.11119 -0.00044 -0.02089 -0.01276 C308 1 0.486453 0.340711 0.553348 11.00000 0.07882 0.04806 = 0.09882 -0.00683 -0.02091 -0.00833 C332 1 0.850952 0.588785 0.831436 11.00000 0.10230 0.05205 = 0.10310 -0.00043 -0.02398 -0.00153 AFIX 43 H332 2 0.846309 0.650075 0.835554 11.00000 -1.20000 AFIX 0 N307 4 0.673429 0.528257 0.596737 11.00000 0.10889 0.05052 = 0.16801 0.02079 -0.06612 -0.02136 C334 1 0.833977 0.455430 0.790306 11.00000 0.07661 0.03037 = 0.12771 0.00649 -0.02477 -0.00791 N311 4 0.813734 -0.002170 0.720525 11.00000 0.15898 0.03362 = 0.20884 0.02235 0.05108 0.03070 C307 1 0.453807 0.212571 0.532247 11.00000 0.09518 0.05146 = 0.09535 -0.01047 -0.02902 -0.00664 C317 1 0.536171 0.408592 0.512591 11.00000 0.09901 0.06916 = 0.11570 -0.00061 -0.03683 -0.02493 AFIX 43 H317 2 0.525711 0.373977 0.486729 11.00000 -1.20000 AFIX 0 C321 1 0.731045 0.442584 0.659574 11.00000 0.07976 0.04369 = 0.13916 0.00663 -0.02097 -0.01399 C303 1 0.409699 0.310114 0.617809 11.00000 0.09935 0.04772 = 0.12734 -0.00137 -0.00906 0.01085 C311 1 0.417027 -0.007969 0.483198 11.00000 0.12810 0.07533 = 0.12517 -0.03998 0.03664 -0.04733 AFIX 43 H311 2 0.398538 -0.051527 0.488679 11.00000 -1.20000 AFIX 0 C319 1 0.679541 0.442679 0.592671 11.00000 0.10781 0.05093 = 0.14040 0.02650 -0.05966 -0.02099 AFIX 43 H319 2 0.664266 0.411458 0.568017 11.00000 -1.20000 AFIX 0 C310 1 0.421150 0.071205 0.509973 11.00000 0.11880 0.08005 = 0.11922 -0.02453 0.02001 -0.03689 AFIX 43 H310 2 0.404267 0.083548 0.530870 11.00000 -1.20000 AFIX 0 C333 1 0.827134 0.545387 0.797126 11.00000 0.10070 0.03271 = 0.15285 0.00197 -0.05532 0.01109 AFIX 43 H333 2 0.806187 0.575694 0.778099 11.00000 -1.20000 AFIX 0 C322 1 0.724600 0.532168 0.661014 11.00000 0.10351 0.04780 = 0.17015 0.01495 -0.07299 -0.00911 AFIX 43 H322 2 0.740062 0.567257 0.683959 11.00000 -1.20000 AFIX 0 C336 1 0.884483 0.464713 0.855414 11.00000 0.10748 0.05035 = 0.14722 -0.00467 -0.06748 0.00378 AFIX 43 H336 2 0.904184 0.435626 0.876769 11.00000 -1.20000 AFIX 0 C318 1 0.567691 0.464627 0.510530 11.00000 0.09441 0.06361 = 0.12802 0.01355 -0.02864 -0.01326 AFIX 43 H318 2 0.578435 0.468107 0.483668 11.00000 -1.20000 AFIX 0 C320 1 0.707412 0.396811 0.623048 11.00000 0.09737 0.05699 = 0.14494 0.00602 -0.05477 -0.02321 AFIX 43 H320 2 0.710744 0.334840 0.619495 11.00000 -1.20000 AFIX 0 C323 1 0.695451 0.571689 0.628915 11.00000 0.11658 0.06021 = 0.18676 -0.00105 -0.08676 0.00078 AFIX 43 H323 2 0.691539 0.633842 0.630755 11.00000 -1.20000 AFIX 0 C305 1 0.391267 0.388025 0.679286 11.00000 0.18053 0.07844 = 0.19533 -0.01157 0.06868 -0.00600 AFIX 43 H305 2 0.396751 0.432383 0.702028 11.00000 -1.20000 AFIX 0 C328 1 0.777741 0.122666 0.686868 11.00000 0.11831 0.03796 = 0.23756 -0.02253 -0.03476 -0.00805 AFIX 43 H328 2 0.756134 0.145306 0.665569 11.00000 -1.20000 AFIX 0 C329 1 0.787062 0.028482 0.689299 11.00000 0.14834 0.05242 = 0.20354 -0.01714 0.01154 -0.02857 PART 4 AFIX 43 H329 2 0.773024 -0.010673 0.667246 11.00000 -1.20000 AFIX 0 PART 0 C301 1 0.350448 0.281185 0.645969 11.00000 0.16102 0.09387 = 0.15965 -0.03582 0.06757 -0.00853 AFIX 43 H301 2 0.327627 0.245273 0.645003 11.00000 -1.20000 AFIX 0 C330 1 0.835094 0.047189 0.747252 11.00000 0.21332 0.03155 = 0.20102 -0.01882 -0.05906 0.00659 AFIX 43 H330 2 0.856389 0.021205 0.767750 11.00000 -1.20000 AFIX 0 C304 1 0.418509 0.376342 0.651917 11.00000 0.15092 0.11227 = 0.12877 -0.03948 0.03146 -0.01216 AFIX 43 H304 2 0.442045 0.410621 0.655501 11.00000 -1.20000 AFIX 0 C331 1 0.830015 0.138033 0.749282 11.00000 0.17182 0.06751 = 0.12719 -0.00877 -0.01508 0.02833 AFIX 43 H331 2 0.845649 0.172407 0.772409 11.00000 -1.20000 AFIX 0 C335 1 0.861603 0.413929 0.821464 11.00000 0.12390 0.05202 = 0.18063 0.00258 -0.08307 0.00300 AFIX 43 H335 2 0.865297 0.351614 0.820200 11.00000 -1.20000 AFIX 0 C302 1 0.375013 0.266856 0.614508 11.00000 0.23875 0.05518 = 0.14872 -0.02080 0.04733 -0.01614 AFIX 43 H302 2 0.367149 0.226036 0.590449 11.00000 -1.20000 AFIX 0 C315 1 0.534985 0.454431 0.587139 11.00000 0.12764 0.14415 = 0.17290 -0.08522 0.01560 -0.07288 AFIX 43 H315 2 0.523552 0.456127 0.613562 11.00000 -1.20000 AFIX 0 PART 2 I302 3 0.251836 0.282479 0.681616 31.00000 0.22675 0.06927 = 0.44733 -0.09924 0.19054 -0.06844 ZN31 5 0.314961 0.357180 0.715456 31.00000 0.22401 0.03285 = 0.24555 0.00814 0.09562 0.01108 I301 3 0.352011 0.320964 0.794627 31.00000 0.39759 0.12536 = 0.27925 0.10403 0.18380 0.14331 PART 3 I502 3 0.239884 0.299695 0.646651 41.00000 10.08000 I501 3 0.317320 0.292884 0.776433 41.00000 10.08000 ZN51 5 0.300765 0.355216 0.690989 41.00000 10.08000 PART 0 C314 1 0.568367 0.505665 0.583305 11.00000 0.13945 0.12596 = 0.15338 -0.01364 -0.02835 -0.08250 AFIX 43 H314 2 0.581196 0.536512 0.609508 11.00000 -1.20000 AFIX 0 PART 2 ZN32 5 0.420785 -0.124287 0.405835 10.68587 0.07164 0.04405 = 0.06980 -0.00296 -0.01449 0.00284 I303 3 0.476129 -0.151457 0.362928 10.68587 0.08689 0.08661 = 0.07936 0.00105 -0.00186 0.02312 I304 3 0.384386 -0.238071 0.444580 10.68587 0.09900 0.04579 = 0.11136 0.00611 -0.00173 -0.00493 PART 3 I504 3 0.390693 -0.241437 0.406647 10.02445 10.08000 I503 3 0.477104 -0.165443 0.350710 10.02445 10.08000 ZN52 5 0.429651 -0.107023 0.397345 10.02445 10.08000 PART 2 I405 3 0.610368 0.741716 0.595089 10.44489 0.20739 0.05362 = 0.35828 -0.00054 -0.12114 0.01678 ZN43 5 0.629633 0.601336 0.553835 10.44489 0.09226 0.05520 = 0.17909 0.03738 -0.06710 -0.02378 I406 3 0.651195 0.591230 0.479810 10.44489 0.11027 0.24782 = 0.23189 0.13810 -0.04201 -0.03005 HKLF 4 REM 2023ncs7022a_rc1_a.res in C2/c REM R1 = 0.0864 for 9409 Fo > 4sig(Fo) and 0.1041 for all 13960 data REM 616 parameters refined using 22 restraints END WGHT 0.1966 0.0000 REM Highest difference peak 1.781, deepest hole -0.980, 1-sigma level 0.146 Q1 1 0.6548 0.5802 0.5130 11.00000 0.05 1.78 Q2 1 0.3535 0.2940 0.7490 11.00000 0.05 1.43 Q3 1 0.4829 -0.1444 0.4105 11.00000 0.05 1.41 Q4 1 0.6429 0.7433 0.5404 11.00000 0.05 1.34 Q5 1 0.3742 -0.2205 0.3997 11.00000 0.05 1.27 Q6 1 0.5036 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11.00000 0.05 0.34 Q50 1 0.4362 0.2800 0.5521 11.00000 0.05 0.34 Q51 1 0.8572 0.1996 0.8063 11.00000 0.05 0.33 Q52 1 0.8624 0.3797 0.7854 11.00000 0.05 0.33 Q53 1 0.5143 0.4614 0.5608 11.00000 0.05 0.32 Q54 1 0.7977 0.0178 0.7455 11.00000 0.05 0.32 Q55 1 0.7284 0.3925 0.7065 11.00000 0.05 0.32 Q56 1 0.8536 0.0146 0.7079 11.00000 0.05 0.32 Q57 1 0.7331 0.3887 0.7240 11.00000 0.05 0.32 Q58 1 0.7699 0.4518 0.7614 11.00000 0.05 0.31 Q59 1 0.5885 0.5176 0.5134 11.00000 0.05 0.31 Q60 1 0.4525 0.1214 0.4706 11.00000 0.05 0.31 Q61 1 0.4744 0.2621 0.4909 11.00000 0.05 0.31 Q62 1 0.3435 0.2844 0.6038 11.00000 0.05 0.30 Q63 1 0.4005 0.3426 0.6250 11.00000 0.05 0.30 Q64 1 0.8280 0.3161 0.6981 11.00000 0.05 0.30 Q65 1 0.6397 0.8158 0.5575 11.00000 0.05 0.30 Q66 1 0.4023 -0.0588 0.5111 11.00000 0.05 0.30 Q67 1 0.8081 0.1292 0.6748 11.00000 0.05 0.29 ; _shelx_res_checksum 32479 _shelx_hkl_file ; 0 0 -2 27.24 1.32 0 0 -3 0.56 0.99 0 0 -4 310.39 12.38 0 0 -5 1.71 1.62 0 0 -6 232.23 9.55 0 0 7 -5.89 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-41 1 7 0.67 0.78 -41 -1 6 0.01 0.75 -41 1 6 0.48 0.79 -41 1 6 0.80 1.17 -41 -1 5 -0.69 0.75 -41 1 5 1.11 0.80 -41 1 5 0.93 1.20 -41 -1 4 -0.05 0.75 -41 1 4 -0.54 0.80 -41 1 4 1.60 1.24 -41 -1 3 -0.90 0.76 -41 1 3 0.17 0.80 -41 1 3 0.87 1.24 -41 -1 2 -0.86 0.75 -41 1 2 0.23 0.80 -41 1 2 0.31 1.24 0 0 0 0.00 0.00 TITL 2023NCS7022a_RC1 in C2/c REM C2/c (#15 in standard setting) CELL 1.54184 34.415551 15.080374 30.060674 90.0000 100.7094 90.0000 ZERR 8.00 0.000895 0.000314 0.001603 0.0000 0.0036 0.0000 LATT 7 SYMM -x, y,-z+1/2 SFAC C H N O Zn I UNIT 624.00 640.00 96.00 48.00 24.00 48.00 REM CrysAlisPro recorded range (K): Min=100.0; max=100.0; aver:100.0 TEMP -173 SIZE 0.06 0.11 0.16 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 63579 _shelx_fab_file ; -41 1 2 2.5073 1.1323 -41 1 3 1.3225 0.8161 -41 1 4 -3.1355 0.2668 -41 1 5 -1.0019 0.6479 -41 1 6 -3.8513 1.1898 -41 1 7 5.8672 -0.1221 -41 1 8 6.1851 0.9241 -41 1 9 0.0371 0.2863 -41 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-0.4870 31 1 6 -1.4136 -1.0945 31 1 7 1.0330 0.6986 31 1 8 -0.5415 0.3047 31 1 9 5.2343 1.1810 31 1 10 2.3711 1.9793 31 1 11 -4.2814 1.9455 31 1 12 -2.2125 0.4104 31 1 13 0.3734 -0.2082 31 1 14 3.2377 1.9958 31 1 15 2.4479 -0.1082 31 1 16 -1.7880 2.8207 31 1 17 -0.6260 0.3489 31 1 18 0.1720 1.9573 31 3 0 -1.4341 -0.9898 31 3 1 -3.0923 -2.4704 31 3 2 2.7827 1.3070 31 3 3 -2.5912 -2.2287 31 3 4 -4.5398 -0.1763 31 3 5 0.9468 -1.4855 31 3 6 1.4411 -1.9796 31 3 7 1.0617 -1.1630 31 3 8 -2.3458 0.2296 31 3 9 2.0246 -0.6967 31 3 10 1.8199 0.2359 31 3 11 -2.5593 -0.1639 31 3 12 -4.8707 -0.6218 31 3 13 -0.1581 -0.7777 31 3 14 0.5210 -0.2392 31 3 15 3.2556 0.5431 31 3 16 1.0277 0.3965 31 3 17 0.6468 0.3629 31 5 0 0.5028 0.0326 31 5 1 2.0714 0.6568 31 5 2 3.1968 0.8255 31 5 3 1.7309 0.0795 31 5 4 -3.7243 0.6086 31 5 5 1.5669 -0.4022 31 5 6 2.3977 -0.2945 31 5 7 -2.5390 -0.5681 31 5 8 -2.6561 -0.1110 31 5 9 -0.5704 0.4535 31 5 10 1.9285 0.1804 31 5 11 -1.7192 -0.2268 31 5 12 -1.9967 -0.6886 31 5 13 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34 6 7 1.1800 -0.4537 34 6 8 -2.8659 0.7082 34 6 9 3.9989 0.4026 34 6 10 0.5096 -0.8451 34 6 11 -0.3854 0.5312 34 8 0 -13.9970 -0.3378 34 8 1 -1.1495 -0.5293 34 8 2 -1.9678 -0.2078 34 8 3 -0.9927 0.3347 34 8 4 -3.9462 0.5279 34 8 5 1.5703 1.0635 34 8 6 -1.2743 1.5608 34 8 7 2.3897 0.9603 34 10 0 1.4453 1.0209 35 1 0 2.7158 1.8642 35 1 1 -5.0815 -0.4999 35 1 2 2.3212 1.3864 35 1 3 4.2309 1.0465 35 1 4 0.3879 0.4533 35 1 5 -2.5529 0.6081 35 1 6 -1.6285 1.1939 35 1 7 1.3232 -0.9642 35 1 8 1.3574 1.0401 35 1 9 1.9765 -0.9610 35 1 10 0.0266 -0.3747 35 1 11 6.2257 -1.4837 35 1 12 0.4517 -0.2919 35 1 13 -0.6777 -2.8177 35 3 0 -0.4622 0.1929 35 3 1 -5.6376 1.0654 35 3 2 0.4911 0.5712 35 3 3 -0.1662 1.0171 35 3 4 -1.2717 -0.4655 35 3 5 -3.3135 0.7195 35 3 6 0.4183 0.1298 35 3 7 3.7857 0.6020 35 3 8 -0.1890 0.6243 35 3 9 -0.6370 0.0894 35 3 10 -3.8532 0.6157 35 3 11 0.4946 0.0763 35 3 12 1.3344 -0.1518 35 5 0 5.3222 -0.1460 35 5 1 -2.8643 -0.2392 35 5 2 -1.2055 0.2274 35 5 3 -0.6059 -0.3883 35 5 4 1.0117 -0.2531 35 5 5 3.3266 -0.6962 35 5 6 -0.0931 -0.7940 35 5 7 -3.1710 0.0980 35 5 8 3.2459 0.0326 35 5 9 1.7897 -0.2062 35 5 10 -2.8660 -0.5998 35 7 0 0.3400 -0.8826 35 7 1 2.6413 -0.6562 35 7 2 -1.8148 -0.4833 35 7 3 -1.7077 -0.4344 35 7 4 -2.8546 -0.8007 35 7 5 0.7336 -0.9904 35 7 6 -1.0526 -1.0314 35 7 7 -0.0984 -1.5580 35 9 0 7.0257 -0.4532 35 9 1 -0.2318 -0.5888 36 0 0 -1.4098 -1.2802 36 0 2 1.6144 -0.3890 36 0 4 -1.9113 3.8086 36 0 6 0.3237 4.5329 36 0 8 -1.9774 0.3411 36 0 10 0.8167 2.4430 36 2 0 -3.8068 0.8268 36 2 1 -1.7143 -2.0036 36 2 2 -3.0345 -1.0286 36 2 3 -0.6791 -0.0543 36 2 4 -1.3258 0.4957 36 2 5 1.8724 0.0411 36 2 6 3.5865 0.0704 36 2 7 -1.1873 0.8996 36 2 8 -1.8215 -0.8900 36 2 9 2.7259 1.2509 36 2 10 0.4677 2.0535 36 2 11 -0.8106 -1.0418 36 4 0 -4.6051 -0.1927 36 4 1 -2.8798 0.5382 36 4 2 -1.0194 -0.5852 36 4 3 1.9297 -0.5178 36 4 4 -2.1591 0.2649 36 4 5 -0.8976 0.3481 36 4 6 -0.2983 0.3380 36 4 7 2.2775 0.2646 36 4 8 -0.5418 0.1139 36 4 9 1.0323 -0.5891 36 6 0 5.9069 -0.5550 36 6 1 -3.5804 0.8687 36 6 2 -5.5167 0.0677 36 6 3 -1.5072 0.0871 36 6 4 -0.3223 -0.5810 36 6 5 -3.0837 0.2434 36 6 6 4.5556 0.3826 36 6 7 -4.5313 -0.4071 36 8 0 3.7253 0.0639 36 8 1 1.6316 0.9549 36 8 2 2.3391 -0.3455 37 1 0 0.4617 1.2292 37 1 1 -0.8971 -0.6098 37 1 2 -3.5989 0.9527 37 1 3 3.1904 0.1530 37 1 4 1.4987 0.0442 37 1 5 -0.9286 -1.1113 37 1 6 0.2350 1.6610 37 1 7 3.1970 -0.1096 37 1 8 -0.1842 0.1275 37 1 9 -2.4680 -0.6418 37 3 0 -0.9162 -0.6542 37 3 1 -1.0603 -0.3825 37 3 2 1.3825 -0.9823 37 3 3 -0.6496 -0.2750 37 3 4 -2.9985 -0.5536 37 3 5 -0.4645 -0.1847 37 3 6 -1.3219 -1.0030 37 3 7 3.3083 -0.1339 37 3 8 2.9931 0.7538 37 5 0 2.6474 -0.7362 37 5 1 3.8279 0.6037 37 5 2 -1.0291 -0.6092 37 5 3 -0.4720 -1.1996 37 5 4 -1.8050 -0.7103 37 5 5 4.8970 -0.5929 37 5 6 -4.3554 -0.2662 37 7 0 -0.1487 0.4964 37 7 1 -0.1331 -0.1326 37 7 2 5.2152 1.3906 38 0 0 -1.0898 -1.4695 38 0 2 -2.4591 -1.6759 38 0 4 -0.0452 1.4700 38 0 6 1.0688 2.0770 38 0 8 1.1959 -1.9345 38 2 0 3.1996 -0.7195 38 2 1 4.6736 -0.0718 38 2 2 3.0056 -0.7062 38 2 3 -1.5322 1.1086 38 2 4 -1.9604 -0.2693 38 2 5 -1.4395 0.2627 38 2 6 -2.0125 -0.1621 38 2 7 -2.8408 1.7134 38 4 0 6.7679 0.5158 38 4 1 -4.6186 -0.3089 38 4 2 2.7625 0.9998 38 4 3 4.7588 -0.5692 38 4 4 -3.4029 -0.2188 38 4 5 -3.3132 0.6116 38 6 0 5.5785 -0.3368 38 6 1 1.6541 0.3644 39 1 0 -1.0479 -0.2509 39 1 1 -0.7480 -1.7299 39 1 2 -2.7424 -0.5522 39 1 3 -4.0769 -0.8571 39 1 4 -0.8493 -1.7728 39 1 5 -4.2381 -0.2408 39 3 0 -4.0553 0.0628 39 3 1 1.3404 -0.8348 39 3 2 5.8339 -0.1505 39 3 3 -3.3481 -0.1102 39 3 4 2.0884 0.2641 39 5 0 -3.3984 0.2540 40 0 0 6.1902 -0.6960 40 0 2 -3.4683 -1.6438 40 2 0 0.3847 -0.0662 40 2 1 -0.0385 0.5907 40 2 2 -0.4396 1.2430 0 0 0 0.0 0.0 ; _shelx_fab_checksum 79556 _olex2_date_sample_data_collection 2023-04-19 _olex2_date_sample_submission 2023-04-19 _olex2_submission_original_sample_id 25_10_24c _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling - Detector area scaling - B-factor correction ; _oxdiff_exptl_absorpt_empirical_full_max 3.462 _oxdiff_exptl_absorpt_empirical_full_min 0.454 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group I404 I 0.3783(2) -0.2265(4) 0.4385(3) 0.185(5) Uani 0.2897 1 d D . P A 1 I403 I 0.4803(3) -0.1456(6) 0.3681(3) 0.239(6) Uani 0.2897 1 d D . P A 1 I305 I 0.61939(12) 0.7369(2) 0.5745(2) 0.175(2) Uani 0.5551 1 d D . P B 1 Zn42 Zn 0.4198(4) -0.1169(8) 0.4026(4) 0.176(8) Uani 0.2897 1 d D . P A 1 I306 I 0.6584(2) 0.5528(6) 0.4705(2) 0.184(2) Uani 0.5551 1 d D . P B 1 I401 I 0.37620(10) 0.34296(17) 0.80724(9) 0.1093(9) Uani 0.418(3) 1 d D . P C 1 I402 I 0.27042(10) 0.2659(2) 0.70806(14) 0.1194(9) Uani 0.418(3) 1 d D . P C 1 Zn33 Zn 0.6342(3) 0.5839(6) 0.5417(3) 0.144(4) Uani 0.5551 1 d D . P B 1 Zn41 Zn 0.33087(17) 0.3615(4) 0.73155(18) 0.0862(12) Uani 0.418(3) 1 d D . P C 1 N303 N 0.4295(2) 0.2226(5) 0.5604(3) 0.085(2) Uani 1 1 d . . . . . N310 N 0.8183(2) 0.3198(4) 0.7499(3) 0.094(3) Uani 1 1 d . . . . . N308 N 0.78109(19) 0.4470(4) 0.7246(3) 0.083(2) Uani 1 1 d . . . . . N309 N 0.7669(2) 0.3106(4) 0.6859(3) 0.090(2) Uani 1 1 d . . . . . N312 N 0.88014(19) 0.5501(4) 0.8592(3) 0.0780(19) Uani 1 1 d . . . . . N302 N 0.4648(2) 0.3564(5) 0.5828(3) 0.088(2) Uani 1 1 d . . . . . N305 N 0.4373(2) -0.0226(5) 0.4521(3) 0.090(2) Uani 1 1 d D . . . . N304 N 0.4822(2) 0.2682(4) 0.5255(2) 0.083(2) Uani 1 1 d . . . . . N306 N 0.5830(3) 0.5140(6) 0.5468(4) 0.105(3) Uani 1 1 d D . . . . C309 C 0.4509(2) 0.1285(5) 0.5038(3) 0.071(2) Uani 1 1 d . . . . . C316 C 0.5195(3) 0.4011(5) 0.5502(4) 0.086(3) Uani 1 1 d . . . . . C326 C 0.8101(2) 0.4050(5) 0.7521(3) 0.075(2) Uani 1 1 d . . . . . C306 C 0.4363(3) 0.2960(5) 0.5861(3) 0.083(3) Uani 1 1 d . . . . . C313 C 0.4750(3) 0.1104(6) 0.4741(3) 0.085(3) Uani 1 1 d . . . . . H313 H 0.496196 0.148896 0.471259 0.102 Uiso 1 1 calc R U . . . N301 N 0.3584(5) 0.3435(6) 0.6769(5) 0.137(5) Uani 1 1 d D . . . . C325 C 0.7951(2) 0.2754(5) 0.7164(4) 0.081(2) Uani 1 1 d . . . . . C312 C 0.4680(2) 0.0351(6) 0.4483(3) 0.081(2) Uani 1 1 d . . . . . H312 H 0.484579 0.021972 0.427205 0.097 Uiso 1 1 calc R U . . . C327 C 0.8016(3) 0.1774(6) 0.7168(4) 0.096(3) Uani 1 1 d . . . . . C324 C 0.7606(2) 0.3967(5) 0.6912(3) 0.085(3) Uani 1 1 d . . . . . C308 C 0.4865(3) 0.3407(5) 0.5533(4) 0.080(3) Uani 1 1 d . . . . . C332 C 0.8510(3) 0.5888(6) 0.8314(4) 0.091(3) Uani 1 1 d . . . . . H332 H 0.846309 0.650075 0.835554 0.110 Uiso 1 1 calc R U . . . N307 N 0.6734(3) 0.5283(5) 0.5967(4) 0.121(4) Uani 1 1 d D . . . . C334 C 0.8340(2) 0.4554(5) 0.7903(4) 0.084(3) Uani 1 1 d . . . . . N311 N 0.8137(4) -0.0022(5) 0.7205(5) 0.132(4) Uani 1 1 d . . . . . C307 C 0.4538(3) 0.2126(6) 0.5322(4) 0.087(3) Uani 1 1 d . . . . . C317 C 0.5362(3) 0.4086(7) 0.5126(4) 0.102(4) Uani 1 1 d . . . . . H317 H 0.525711 0.373977 0.486729 0.122 Uiso 1 1 calc R U . . . C321 C 0.7310(3) 0.4426(5) 0.6596(4) 0.093(3) Uani 1 1 d . . . . . C303 C 0.4097(3) 0.3101(6) 0.6178(4) 0.095(3) Uani 1 1 d . . . . . C311 C 0.4170(4) -0.0080(7) 0.4832(5) 0.108(4) Uani 1 1 d . . . . . H311 H 0.398538 -0.051527 0.488679 0.129 Uiso 1 1 calc R U . . . C319 C 0.6795(3) 0.4427(6) 0.5927(4) 0.110(4) Uani 1 1 d . . . . . H319 H 0.664266 0.411458 0.568017 0.132 Uiso 1 1 calc R U . . . C310 C 0.4211(4) 0.0712(8) 0.5100(4) 0.106(3) Uani 1 1 d . . . . . H310 H 0.404267 0.083548 0.530870 0.128 Uiso 1 1 calc R U . . . C333 C 0.8271(3) 0.5454(5) 0.7971(4) 0.106(4) Uani 1 1 d . . . . . H333 H 0.806187 0.575694 0.778099 0.127 Uiso 1 1 calc R U . . . C322 C 0.7246(3) 0.5322(6) 0.6610(5) 0.120(5) Uani 1 1 d . . . . . H322 H 0.740062 0.567257 0.683959 0.144 Uiso 1 1 calc R U . . . C336 C 0.8845(3) 0.4647(6) 0.8554(4) 0.113(4) Uani 1 1 d . . . . . H336 H 0.904184 0.435626 0.876769 0.136 Uiso 1 1 calc R U . . . C318 C 0.5677(3) 0.4646(7) 0.5105(4) 0.102(3) Uani 1 1 d . . . . . H318 H 0.578435 0.468107 0.483668 0.122 Uiso 1 1 calc R U . . . C320 C 0.7074(3) 0.3968(6) 0.6230(4) 0.110(4) Uani 1 1 d . . . . . H320 H 0.710744 0.334840 0.619495 0.132 Uiso 1 1 calc R U . . . C323 C 0.6955(3) 0.5717(7) 0.6289(5) 0.136(6) Uani 1 1 d . . . . . H323 H 0.691539 0.633842 0.630755 0.163 Uiso 1 1 calc R U . . . C305 C 0.3913(6) 0.3880(11) 0.6793(7) 0.147(6) Uani 1 1 d . . . . . H305 H 0.396751 0.432383 0.702028 0.177 Uiso 1 1 calc R U . . . C328 C 0.7777(4) 0.1227(6) 0.6869(6) 0.140(6) Uani 1 1 d . . . . . H328 H 0.756134 0.145306 0.665569 0.168 Uiso 1 1 calc R U . . . C329 C 0.7871(5) 0.0285(8) 0.6893(7) 0.137(5) Uani 1 1 d . . . . . H329 H 0.773024 -0.010673 0.667246 0.165 Uiso 1 1 calc R U . D 4 C301 C 0.3504(5) 0.2812(10) 0.6460(6) 0.133(5) Uani 1 1 d . . . . . H301 H 0.327627 0.245273 0.645003 0.160 Uiso 1 1 calc R U . . . C330 C 0.8351(6) 0.0472(7) 0.7473(6) 0.161(8) Uani 1 1 d . . . . . H330 H 0.856389 0.021205 0.767750 0.193 Uiso 1 1 calc R U . . . C304 C 0.4185(5) 0.3763(11) 0.6519(6) 0.130(5) Uani 1 1 d . . . . . H304 H 0.442045 0.410621 0.655501 0.156 Uiso 1 1 calc R U . . . C331 C 0.8300(5) 0.1380(8) 0.7493(5) 0.128(5) Uani 1 1 d . . . . . H331 H 0.845649 0.172407 0.772409 0.153 Uiso 1 1 calc R U . . . C335 C 0.8616(3) 0.4139(7) 0.8215(5) 0.133(6) Uani 1 1 d . . . . . H335 H 0.865297 0.351614 0.820200 0.160 Uiso 1 1 calc R U . . . C302 C 0.3750(7) 0.2669(8) 0.6145(6) 0.146(6) Uani 1 1 d . . . . . H302 H 0.367149 0.226036 0.590449 0.175 Uiso 1 1 calc R U . . . C315 C 0.5350(4) 0.4544(11) 0.5871(6) 0.150(6) Uani 1 1 d . . . . . H315 H 0.523552 0.456127 0.613562 0.180 Uiso 1 1 calc R U . . . I302 I 0.25184(15) 0.2825(2) 0.6816(3) 0.231(3) Uani 0.554(3) 1 d D . P C 2 Zn31 Zn 0.3150(2) 0.3572(3) 0.7155(3) 0.161(3) Uani 0.554(3) 1 d D . P C 2 I301 I 0.3520(2) 0.3210(3) 0.7946(2) 0.252(3) Uani 0.554(3) 1 d D . P C 2 I502 I 0.2399(7) 0.300(2) 0.6467(8) 0.080 Uiso 0.0282(15) 1 d . U P C 3 I501 I 0.3173(6) 0.2929(16) 0.7764(8) 0.080 Uiso 0.0282(15) 1 d . U P C 3 Zn51 Zn 0.3008(16) 0.355(5) 0.6910(18) 0.080 Uiso 0.0282(15) 1 d . U P C 3 C314 C 0.5684(5) 0.5057(11) 0.5833(6) 0.147(6) Uani 1 1 d . . . . . H314 H 0.581196 0.536512 0.609508 0.176 Uiso 1 1 calc R U . . . Zn32 Zn 0.42079(7) -0.1243(2) 0.40583(8) 0.0654(7) Uani 0.6859 1 d D . P A 2 I303 I 0.47613(6) -0.15146(17) 0.36293(5) 0.0865(4) Uani 0.6859 1 d D . P A 2 I304 I 0.38439(5) -0.23807(13) 0.44458(8) 0.0881(4) Uani 0.6859 1 d D . P A 2 I504 I 0.3907(7) -0.2414(19) 0.4066(10) 0.080 Uiso 0.0244 1 d . U P A 3 I503 I 0.4771(14) -0.165(3) 0.3507(17) 0.080 Uiso 0.0244 1 d . U P A 3 Zn52 Zn 0.430(3) -0.107(7) 0.397(4) 0.080 Uiso 0.0244 1 d . U P A 3 I405 I 0.6104(2) 0.7417(4) 0.5951(3) 0.229(5) Uani 0.4449 1 d D . P B 2 Zn43 Zn 0.6296(3) 0.6013(6) 0.5538(4) 0.121(3) Uani 0.4449 1 d D . P B 2 I406 I 0.6512(3) 0.5912(7) 0.4798(4) 0.206(4) Uani 0.4449 1 d D . P B 2 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 I404 0.245(7) 0.054(2) 0.198(5) 0.021(2) -0.113(5) -0.049(3) I403 0.256(8) 0.126(5) 0.273(9) -0.031(5) -0.115(6) 0.107(5) I305 0.1393(16) 0.0464(11) 0.274(4) 0.0157(14) -0.130(3) -0.0055(10) Zn42 0.171(10) 0.040(5) 0.257(13) -0.006(5) -0.120(9) 0.018(5) I306 0.111(3) 0.229(6) 0.185(3) 0.121(3) -0.0403(19) -0.035(3) I401 0.168(2) 0.0502(9) 0.1026(12) 0.0070(7) 0.0069(13) 0.0162(10) I402 0.1284(18) 0.0485(10) 0.183(2) -0.0272(11) 0.0341(15) -0.0160(10) Zn33 0.113(3) 0.064(3) 0.212(7) 0.035(3) -0.087(4) -0.025(2) Zn41 0.112(3) 0.0350(17) 0.107(2) -0.0057(14) 0.008(2) 0.0042(16) N303 0.085(4) 0.061(4) 0.098(5) -0.014(4) -0.011(4) -0.004(3) N310 0.086(4) 0.023(3) 0.156(7) 0.012(3) -0.024(4) -0.001(3) N308 0.080(3) 0.031(3) 0.122(6) 0.001(3) -0.020(4) -0.011(2) N309 0.085(4) 0.035(3) 0.133(6) -0.001(3) -0.024(4) -0.015(3) N312 0.078(3) 0.051(4) 0.093(5) 0.013(3) -0.012(3) -0.004(3) N302 0.084(4) 0.053(4) 0.109(6) -0.009(4) -0.031(4) -0.001(3) N305 0.102(5) 0.051(4) 0.105(6) -0.007(4) -0.017(4) -0.013(3) N304 0.098(4) 0.049(4) 0.084(4) -0.003(3) -0.029(4) -0.017(3) N306 0.100(5) 0.067(5) 0.126(7) 0.018(5) -0.031(5) -0.015(4) C309 0.079(4) 0.048(4) 0.078(5) -0.002(3) -0.007(4) -0.002(3) C316 0.085(5) 0.047(4) 0.106(7) -0.004(4) -0.035(5) -0.002(3) C326 0.066(3) 0.039(3) 0.109(6) 0.002(4) -0.010(4) -0.006(3) C306 0.099(5) 0.043(4) 0.092(6) -0.002(4) -0.019(5) 0.002(4) C313 0.082(5) 0.054(4) 0.103(6) -0.010(4) -0.026(5) -0.002(4) N301 0.222(13) 0.042(4) 0.162(11) 0.008(5) 0.080(10) 0.021(6) C325 0.084(4) 0.038(4) 0.113(6) -0.001(4) -0.005(4) -0.009(3) C312 0.068(4) 0.068(5) 0.097(6) 0.003(4) -0.013(4) -0.007(3) C327 0.110(6) 0.040(4) 0.127(8) 0.012(4) -0.007(6) 0.000(4) C324 0.084(4) 0.045(4) 0.111(6) 0.000(4) -0.021(4) -0.013(3) C308 0.079(4) 0.048(4) 0.099(6) -0.007(4) -0.021(5) -0.008(3) C332 0.102(5) 0.052(4) 0.103(6) 0.000(4) -0.024(5) -0.002(4) N307 0.109(5) 0.051(4) 0.168(8) 0.021(5) -0.066(6) -0.021(4) C334 0.077(4) 0.030(3) 0.128(7) 0.006(4) -0.025(4) -0.008(3) N311 0.159(9) 0.034(4) 0.209(13) 0.022(6) 0.051(9) 0.031(5) C307 0.095(6) 0.051(4) 0.095(6) -0.010(4) -0.029(5) -0.007(4) C317 0.099(6) 0.069(6) 0.116(8) -0.001(5) -0.037(6) -0.025(5) C321 0.080(4) 0.044(4) 0.139(8) 0.007(4) -0.021(5) -0.014(3) C303 0.099(6) 0.048(5) 0.127(8) -0.001(5) -0.009(6) 0.011(4) C311 0.128(8) 0.075(6) 0.125(9) -0.040(6) 0.037(7) -0.047(6) C319 0.108(6) 0.051(5) 0.140(9) 0.026(5) -0.060(6) -0.021(4) C310 0.119(7) 0.080(7) 0.119(8) -0.025(6) 0.020(6) -0.037(6) C333 0.101(5) 0.033(4) 0.153(9) 0.002(4) -0.055(6) 0.011(3) C322 0.104(6) 0.048(4) 0.170(10) 0.015(5) -0.073(7) -0.009(4) C336 0.107(6) 0.050(5) 0.147(9) -0.005(5) -0.067(6) 0.004(4) C318 0.094(5) 0.064(5) 0.128(8) 0.014(5) -0.029(6) -0.013(4) C320 0.097(5) 0.057(5) 0.145(9) 0.006(5) -0.055(6) -0.023(4) C323 0.117(7) 0.060(5) 0.187(12) -0.001(6) -0.087(8) 0.001(5) C305 0.181(14) 0.078(8) 0.195(18) -0.012(9) 0.069(14) -0.006(9) C328 0.118(7) 0.038(5) 0.238(17) -0.023(7) -0.035(9) -0.008(5) C329 0.148(10) 0.052(6) 0.204(16) -0.017(8) 0.012(11) -0.029(7) C301 0.161(11) 0.094(9) 0.160(13) -0.036(9) 0.068(11) -0.009(8) C330 0.213(15) 0.032(5) 0.201(16) -0.019(7) -0.059(12) 0.007(6) C304 0.151(11) 0.112(10) 0.129(10) -0.039(9) 0.031(9) -0.012(8) C331 0.172(11) 0.068(7) 0.127(10) -0.009(6) -0.015(8) 0.028(7) C335 0.124(7) 0.052(5) 0.181(12) 0.003(6) -0.083(8) 0.003(5) C302 0.239(19) 0.055(6) 0.149(13) -0.021(7) 0.047(13) -0.016(9) C315 0.128(9) 0.144(13) 0.173(13) -0.085(11) 0.016(9) -0.073(9) I302 0.227(4) 0.0693(17) 0.447(9) -0.099(3) 0.191(5) -0.068(2) Zn31 0.224(9) 0.0329(16) 0.246(9) 0.008(4) 0.096(6) 0.011(4) I301 0.398(8) 0.125(3) 0.279(5) 0.104(3) 0.184(5) 0.143(4) C314 0.139(10) 0.126(12) 0.153(13) -0.014(9) -0.028(9) -0.082(10) Zn32 0.0716(14) 0.0441(15) 0.0698(13) -0.0030(9) -0.0145(11) 0.0028(9) I303 0.0869(6) 0.0866(11) 0.0794(9) 0.0011(6) -0.0019(7) 0.0231(6) I304 0.0990(6) 0.0458(6) 0.1114(9) 0.0061(6) -0.0017(7) -0.0049(4) I405 0.207(5) 0.0536(15) 0.358(11) -0.001(3) -0.121(5) 0.0168(18) Zn43 0.092(3) 0.055(3) 0.179(5) 0.037(3) -0.067(3) -0.024(2) I406 0.110(3) 0.248(9) 0.232(6) 0.138(6) -0.042(3) -0.030(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1 0 0 0.0369 1 0 0 0.0697 0 -1 0 0.0600 0 1 0 0.1006 2 -1 0 0.0681 2 1 0 0.0992 0 0 1 0.0447 0 0 -1 0.0134 1 0 -1 0.0506 -1 0 1 0.0300 1 0 1 0.0578 -1 0 -1 0.0229 -1 1 1 0.0860 2 1 1 0.0905 1 2 -2 0.0895 -1 -1 1 0.0561 2 -1 1 0.0665 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 I403 Zn42 I404 129.1(6) . . ? N312 Zn42 I404 103.7(6) 8_455 . ? N312 Zn42 I403 109.7(7) 8_455 . ? N312 Zn42 N305 101.4(6) 8_455 . ? N305 Zn42 I404 104.6(6) . . ? N305 Zn42 I403 105.1(6) . . ? I306 Zn33 I305 128.1(4) . . ? N306 Zn33 I305 101.1(5) . . ? N306 Zn33 I306 113.1(5) . . ? N306 Zn33 N307 99.7(5) . . ? N307 Zn33 I305 101.4(4) . . ? N307 Zn33 I306 109.5(6) . . ? I402 Zn41 I401 121.9(3) . . ? N301 Zn41 I401 113.9(5) . . ? N301 Zn41 I402 100.3(5) . . ? N301 Zn41 N311 99.0(5) . 3_455 ? N311 Zn41 I401 110.6(5) 3_455 . ? N311 Zn41 I402 108.4(5) 3_455 . ? C307 N303 C306 113.7(8) . . ? C326 N310 C325 115.0(6) . . ? C326 N308 C324 115.0(7) . . ? C325 N309 C324 115.2(7) . . ? Zn42 N312 Zn32 2.0(4) 8_556 8_556 ? Zn42 N312 Zn52 12(3) 8_556 8_556 ? C332 N312 Zn42 122.9(7) . 8_556 ? C332 N312 Zn32 121.4(6) . 8_556 ? C332 N312 Zn52 129(3) . 8_556 ? C336 N312 Zn42 119.0(6) . 8_556 ? C336 N312 C332 117.9(7) . . ? C336 N312 Zn32 120.7(5) . 8_556 ? C336 N312 Zn52 111(3) . 8_556 ? C308 N302 C306 116.7(8) . . ? C312 N305 Zn42 119.8(9) . . ? C312 N305 Zn32 121.7(8) . . ? C312 N305 Zn52 108(3) . . ? C311 N305 Zn42 121.2(7) . . ? C311 N305 C312 118.4(8) . . ? C311 N305 Zn32 119.8(6) . . ? C311 N305 Zn52 133(3) . . ? C307 N304 C308 114.2(10) . . ? C318 N306 Zn33 115.4(10) . . ? C318 N306 Zn43 128.2(11) . . ? C314 N306 Zn33 125.3(8) . . ? C314 N306 C318 118.6(10) . . ? C314 N306 Zn43 113.1(8) . . ? C313 C309 C307 123.6(8) . . ? C313 C309 C310 121.5(8) . . ? C310 C309 C307 114.9(10) . . ? C317 C316 C308 123.5(8) . . ? C317 C316 C315 117.1(10) . . ? C315 C316 C308 119.4(12) . . ? N310 C326 N308 125.0(7) . . ? N310 C326 C334 116.3(7) . . ? N308 C326 C334 118.6(7) . . ? N303 C306 N302 124.2(11) . . ? N303 C306 C303 115.6(9) . . ? N302 C306 C303 120.2(8) . . ? C309 C313 H313 120.8 . . ? C309 C313 C312 118.4(9) . . ? C312 C313 H313 120.8 . . ? C305 N301 Zn41 114.2(13) . . ? C305 N301 C301 118.2(15) . . ? C305 N301 Zn31 128.8(12) . . ? C305 N301 Zn51 141(2) . . ? C301 N301 Zn41 126.3(12) . . ? C301 N301 Zn31 113.0(12) . . ? C301 N301 Zn51 97(2) . . ? N310 C325 C327 114.9(7) . . ? N309 C325 N310 125.4(7) . . ? N309 C325 C327 119.6(7) . . ? N305 C312 H312 119.1 . . ? C313 C312 N305 121.9(10) . . ? C313 C312 H312 119.1 . . ? C328 C327 C325 121.3(9) . . ? C328 C327 C331 117.6(10) . . ? C331 C327 C325 121.0(9) . . ? N308 C324 C321 115.5(7) . . ? N309 C324 N308 124.3(7) . . ? N309 C324 C321 120.2(7) . . ? N302 C308 N304 124.1(8) . . ? N302 C308 C316 119.0(8) . . ? N304 C308 C316 116.9(10) . . ? N312 C332 H332 118.3 . . ? N312 C332 C333 123.3(8) . . ? C333 C332 H332 118.3 . . ? C319 N307 Zn33 114.0(7) . . ? C319 N307 Zn43 124.4(6) . . ? C323 N307 Zn33 126.0(7) . . ? C323 N307 C319 119.0(8) . . ? C323 N307 Zn43 116.6(7) . . ? C333 C334 C326 121.6(7) . . ? C335 C334 C326 120.8(7) . . ? C335 C334 C333 117.5(8) . . ? Zn41 N311 Zn51 37.4(13) 3_545 3_545 ? C329 N311 Zn41 127.0(11) . 3_545 ? C329 N311 Zn31 109.3(10) . 3_545 ? C329 N311 Zn51 89.6(16) . 3_545 ? C330 N311 Zn41 111.3(10) . 3_545 ? C330 N311 C329 121.5(10) . . ? C330 N311 Zn31 129.1(11) . 3_545 ? C330 N311 Zn51 148.4(16) . 3_545 ? N303 C307 N304 127.1(8) . . ? N303 C307 C309 118.5(8) . . ? N304 C307 C309 114.5(11) . . ? C316 C317 H317 118.6 . . ? C316 C317 C318 122.7(10) . . ? C318 C317 H317 118.6 . . ? C322 C321 C324 123.6(8) . . ? C322 C321 C320 115.5(8) . . ? C320 C321 C324 120.8(8) . . ? C304 C303 C306 119.9(11) . . ? C302 C303 C306 122.5(11) . . ? C302 C303 C304 117.4(14) . . ? N305 C311 H311 118.6 . . ? N305 C311 C310 122.8(10) . . ? C310 C311 H311 118.6 . . ? N307 C319 H319 118.9 . . ? N307 C319 C320 122.2(9) . . ? C320 C319 H319 118.9 . . ? C309 C310 C311 116.5(11) . . ? C309 C310 H310 121.7 . . ? C311 C310 H310 121.7 . . ? C332 C333 C334 118.9(7) . . ? C332 C333 H333 120.5 . . ? C334 C333 H333 120.5 . . ? C321 C322 H322 120.0 . . ? C321 C322 C323 120.0(9) . . ? C323 C322 H322 120.0 . . ? N312 C336 H336 118.4 . . ? N312 C336 C335 123.2(7) . . ? C335 C336 H336 118.4 . . ? N306 C318 C317 119.6(13) . . ? N306 C318 H318 120.2 . . ? C317 C318 H318 120.2 . . ? C321 C320 H320 120.1 . . ? C319 C320 C321 119.7(9) . . ? C319 C320 H320 120.1 . . ? N307 C323 C322 123.4(10) . . ? N307 C323 H323 118.3 . . ? C322 C323 H323 118.3 . . ? N301 C305 H305 117.2 . . ? N301 C305 C304 125.7(17) . . ? C304 C305 H305 117.2 . . ? C327 C328 H328 121.5 . . ? C327 C328 C329 117.0(12) . . ? C329 C328 H328 121.5 . . ? N311 C329 C328 120.9(13) . . ? N311 C329 H329 119.5 . . ? C328 C329 H329 119.5 . . ? N301 C301 H301 119.5 . . ? N301 C301 C302 121.1(15) . . ? C302 C301 H301 119.5 . . ? N311 C330 H330 117.9 . . ? N311 C330 C331 124.2(14) . . ? C331 C330 H330 117.9 . . ? C303 C304 H304 121.8 . . ? C305 C304 C303 116.4(15) . . ? C305 C304 H304 121.8 . . ? C327 C331 C330 118.2(12) . . ? C327 C331 H331 120.9 . . ? C330 C331 H331 120.9 . . ? C334 C335 C336 118.6(9) . . ? C334 C335 H335 120.7 . . ? C336 C335 H335 120.7 . . ? C303 C302 C301 120.9(14) . . ? C303 C302 H302 119.5 . . ? C301 C302 H302 119.5 . . ? C316 C315 H315 121.7 . . ? C316 C315 C314 116.6(16) . . ? C314 C315 H315 121.7 . . ? N301 Zn31 N311 99.5(5) . 3_455 ? N301 Zn31 I302 113.1(6) . . ? N301 Zn31 I301 102.4(5) . . ? N311 Zn31 I302 116.9(5) 3_455 . ? N311 Zn31 I301 99.2(5) 3_455 . ? I302 Zn31 I301 122.2(3) . . ? N301 Zn51 N311 92(2) . 3_455 ? N301 Zn51 I502 128(3) . . ? N301 Zn51 I501 97(2) . . ? N311 Zn51 I502 128(3) 3_455 . ? N311 Zn51 I501 88.1(19) 3_455 . ? I502 Zn51 I501 114(3) . . ? N306 C314 C315 125.0(12) . . ? N306 C314 H314 117.5 . . ? C315 C314 H314 117.5 . . ? N312 Zn32 I303 102.6(3) 8_455 . ? N312 Zn32 I304 110.0(2) 8_455 . ? N305 Zn32 N312 96.8(3) . 8_455 ? N305 Zn32 I303 108.9(3) . . ? N305 Zn32 I304 106.8(3) . . ? I303 Zn32 I304 127.57(14) . . ? N312 Zn52 N305 99(5) 8_455 . ? N312 Zn52 I504 90(4) 8_455 . ? N312 Zn52 I503 113(5) 8_455 . ? N305 Zn52 I504 114(5) . . ? N305 Zn52 I503 132(5) . . ? I504 Zn52 I503 101(4) . . ? N306 Zn43 N307 100.6(5) . . ? N306 Zn43 I405 107.9(6) . . ? N306 Zn43 I406 103.1(6) . . ? N307 Zn43 I405 110.6(6) . . ? N307 Zn43 I406 102.6(6) . . ? I406 Zn43 I405 128.6(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 I404 Zn42 2.550(14) . ? I403 Zn42 2.532(14) . ? I305 Zn33 2.598(9) . ? Zn42 N312 1.978(14) 8_455 ? Zn42 N305 2.065(13) . ? I306 Zn33 2.481(10) . ? I401 Zn41 2.524(5) . ? I402 Zn41 2.522(6) . ? Zn33 N306 2.084(13) . ? Zn33 N307 2.106(11) . ? Zn41 N301 2.062(14) . ? Zn41 N311 2.148(10) 3_455 ? N303 C306 1.346(12) . ? N303 C307 1.306(14) . ? N310 C326 1.319(10) . ? N310 C325 1.342(12) . ? N308 C326 1.332(10) . ? N308 C324 1.349(11) . ? N309 C325 1.316(11) . ? N309 C324 1.331(11) . ? N312 C332 1.317(11) . ? N312 C336 1.304(12) . ? N312 Zn32 2.107(7) 8_556 ? N312 Zn52 2.06(11) 8_556 ? N302 C306 1.356(13) . ? N302 C308 1.279(14) . ? N305 C312 1.389(13) . ? N305 C311 1.285(15) . ? N305 Zn32 2.076(8) . ? N305 Zn52 2.06(11) . ? N304 C308 1.368(12) . ? N304 C307 1.330(14) . ? N306 C318 1.343(15) . ? N306 C314 1.30(2) . ? N306 Zn43 2.058(12) . ? C309 C313 1.354(14) . ? C309 C307 1.521(12) . ? C309 C310 1.378(14) . ? C316 C308 1.474(14) . ? C316 C317 1.364(17) . ? C316 C315 1.394(14) . ? C326 C334 1.490(11) . ? C306 C303 1.455(16) . ? C313 H313 0.9500 . ? C313 C312 1.372(13) . ? N301 C305 1.31(2) . ? N301 C301 1.314(19) . ? N301 Zn31 2.066(14) . ? N301 Zn51 2.11(6) . ? C325 C327 1.494(11) . ? C312 H312 0.9500 . ? C327 C328 1.374(16) . ? C327 C331 1.382(16) . ? C324 C321 1.435(12) . ? C332 H332 0.9500 . ? C332 C333 1.360(12) . ? N307 C319 1.317(13) . ? N307 C323 1.291(13) . ? N307 Zn43 2.104(11) . ? C334 C333 1.398(11) . ? C334 C335 1.357(12) . ? N311 C329 1.27(2) . ? N311 C330 1.233(19) . ? N311 Zn31 2.128(10) 3_545 ? N311 Zn51 2.34(7) 3_545 ? C317 H317 0.9500 . ? C317 C318 1.385(15) . ? C321 C322 1.371(13) . ? C321 C320 1.418(13) . ? C303 C304 1.423(17) . ? C303 C302 1.35(2) . ? C311 H311 0.9500 . ? C311 C310 1.432(15) . ? C319 H319 0.9500 . ? C319 C320 1.381(12) . ? C310 H310 0.9500 . ? C333 H333 0.9500 . ? C322 H322 0.9500 . ? C322 C323 1.390(12) . ? C336 H336 0.9500 . ? C336 C335 1.396(13) . ? C318 H318 0.9500 . ? C320 H320 0.9500 . ? C323 H323 0.9500 . ? C305 H305 0.9500 . ? C305 C304 1.37(2) . ? C328 H328 0.9500 . ? C328 C329 1.455(17) . ? C329 H329 0.9500 . ? C301 H301 0.9500 . ? C301 C302 1.40(2) . ? C330 H330 0.9500 . ? C330 C331 1.384(16) . ? C304 H304 0.9500 . ? C331 H331 0.9500 . ? C335 H335 0.9500 . ? C302 H302 0.9500 . ? C315 H315 0.9500 . ? C315 C314 1.41(2) . ? I302 Zn31 2.490(8) . ? Zn31 I301 2.542(9) . ? I502 Zn51 2.41(6) . ? I501 Zn51 2.69(6) . ? C314 H314 0.9500 . ? Zn32 I303 2.524(3) . ? Zn32 I304 2.532(3) . ? I504 Zn52 2.47(11) . ? I503 Zn52 2.50(12) . ? I405 Zn43 2.601(11) . ? Zn43 I406 2.478(11) . ? 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 Zn42 N312 C332 C333 170.0(11) 8_556 . . . ? Zn42 N312 C336 C335 -170.4(13) 8_556 . . . ? Zn42 N305 C312 C313 165.2(7) . . . . ? Zn42 N305 C311 C310 -161.9(11) . . . . ? Zn33 N306 C318 C317 173.2(8) . . . . ? Zn33 N306 C314 C315 -176.3(15) . . . . ? Zn33 N307 C319 C320 173.1(11) . . . . ? Zn33 N307 C323 C322 -171.1(13) . . . . ? Zn41 N301 C305 C304 167.9(16) . . . . ? Zn41 N301 C301 C302 -169.9(13) . . . . ? Zn41 N311 C329 C328 178.0(12) 3_545 . . . ? Zn41 N311 C330 C331 -177.3(18) 3_545 . . . ? N303 C306 C303 C304 168.8(11) . . . . ? N303 C306 C303 C302 -15.9(15) . . . . ? N310 C326 C334 C333 -177.7(11) . . . . ? N310 C326 C334 C335 -1.8(17) . . . . ? N310 C325 C327 C328 174.4(14) . . . . ? N310 C325 C327 C331 -1.1(18) . . . . ? N308 C326 C334 C333 -1.6(16) . . . . ? N308 C326 C334 C335 174.3(12) . . . . ? N308 C324 C321 C322 3.1(18) . . . . ? N308 C324 C321 C320 -179.6(11) . . . . ? N309 C325 C327 C328 -2.2(19) . . . . ? N309 C325 C327 C331 -177.6(13) . . . . ? N309 C324 C321 C322 -175.7(13) . . . . ? N309 C324 C321 C320 1.6(18) . . . . ? N312 C332 C333 C334 -1(2) . . . . ? N312 C336 C335 C334 1(2) . . . . ? N302 C306 C303 C304 -13.5(15) . . . . ? N302 C306 C303 C302 161.8(11) . . . . ? N305 C311 C310 C309 -6(2) . . . . ? C309 C313 C312 N305 -0.4(12) . . . . ? C316 C317 C318 N306 0.1(15) . . . . ? C316 C315 C314 N306 8(3) . . . . ? C326 N310 C325 N309 2.4(16) . . . . ? C326 N310 C325 C327 -173.9(10) . . . . ? C326 N308 C324 N309 2.8(15) . . . . ? C326 N308 C324 C321 -176.0(10) . . . . ? C326 C334 C333 C332 -177.2(11) . . . . ? C326 C334 C335 C336 177.0(13) . . . . ? C306 N303 C307 N304 -3.5(12) . . . . ? C306 N303 C307 C309 175.6(7) . . . . ? C306 N302 C308 N304 0.6(12) . . . . ? C306 N302 C308 C316 -176.1(7) . . . . ? C306 C303 C304 C305 177.5(13) . . . . ? C306 C303 C302 C301 179.1(13) . . . . ? C313 C309 C307 N303 -178.9(8) . . . . ? C313 C309 C307 N304 0.3(11) . . . . ? C313 C309 C310 C311 -0.3(16) . . . . ? N301 C305 C304 C303 0(3) . . . . ? N301 C301 C302 C303 7(3) . . . . ? C325 N310 C326 N308 1.2(16) . . . . ? C325 N310 C326 C334 177.0(9) . . . . ? C325 N309 C324 N308 0.2(16) . . . . ? C325 N309 C324 C321 178.9(10) . . . . ? C325 C327 C328 C329 178.6(14) . . . . ? C325 C327 C331 C330 -178.7(16) . . . . ? C312 N305 C311 C310 8.7(18) . . . . ? C327 C328 C329 N311 6(3) . . . . ? C324 N308 C326 N310 -3.5(15) . . . . ? C324 N308 C326 C334 -179.3(9) . . . . ? C324 N309 C325 N310 -3.0(16) . . . . ? C324 N309 C325 C327 173.2(10) . . . . ? C324 C321 C322 C323 179.6(14) . . . . ? C324 C321 C320 C319 -179.0(12) . . . . ? C308 N302 C306 N303 -0.8(12) . . . . ? C308 N302 C306 C303 -178.3(8) . . . . ? C308 N304 C307 N303 3.3(12) . . . . ? C308 N304 C307 C309 -175.8(6) . . . . ? C308 C316 C317 C318 -178.9(9) . . . . ? C308 C316 C315 C314 175.4(14) . . . . ? C332 N312 C336 C335 5(2) . . . . ? N307 C319 C320 C321 -1(2) . . . . ? N311 C330 C331 C327 -6(3) . . . . ? C307 N303 C306 N302 2.1(12) . . . . ? C307 N303 C306 C303 179.7(7) . . . . ? C307 N304 C308 N302 -1.7(11) . . . . ? C307 N304 C308 C316 175.1(7) . . . . ? C307 C309 C313 C312 -176.0(7) . . . . ? C307 C309 C310 C311 178.9(10) . . . . ? C317 C316 C308 N302 -158.3(9) . . . . ? C317 C316 C308 N304 24.8(12) . . . . ? C317 C316 C315 C314 -5(2) . . . . ? C321 C322 C323 N307 0(3) . . . . ? C311 N305 C312 C313 -5.5(14) . . . . ? C319 N307 C323 C322 -3(3) . . . . ? C310 C309 C313 C312 3.2(13) . . . . ? C310 C309 C307 N303 1.9(12) . . . . ? C310 C309 C307 N304 -178.9(8) . . . . ? C333 C334 C335 C336 -7(2) . . . . ? C322 C321 C320 C319 -1.6(19) . . . . ? C336 N312 C332 C333 -4.9(18) . . . . ? C318 N306 C314 C315 -6(3) . . . . ? C320 C321 C322 C323 2(2) . . . . ? C323 N307 C319 C320 3(2) . . . . ? C305 N301 C301 C302 -4(3) . . . . ? C328 C327 C331 C330 6(3) . . . . ? C329 N311 C330 C331 7(3) . . . . ? C301 N301 C305 C304 1(3) . . . . ? C330 N311 C329 C328 -7(3) . . . . ? C304 C303 C302 C301 -6(2) . . . . ? C331 C327 C328 C329 -6(2) . . . . ? C335 C334 C333 C332 6.8(19) . . . . ? C302 C303 C304 C305 2(2) . . . . ? C315 C316 C308 N302 21.2(14) . . . . ? C315 C316 C308 N304 -155.7(12) . . . . ? C315 C316 C317 C318 1.5(16) . . . . ? Zn31 N301 C305 C304 -178.8(14) . . . . ? Zn31 N301 C301 C302 175.2(14) . . . . ? Zn31 N311 C329 C328 175.3(14) 3_545 . . . ? Zn31 N311 C330 C331 -175.8(15) 3_545 . . . ? Zn51 N301 C305 C304 -153(3) . . . . ? Zn51 N301 C301 C302 159(2) . . . . ? Zn51 N311 C329 C328 179(2) 3_545 . . . ? Zn51 N311 C330 C331 175(3) 3_545 . . . ? C314 N306 C318 C317 2.0(17) . . . . ? Zn32 N312 C332 C333 171.4(10) 8_556 . . . ? Zn32 N312 C336 C335 -171.7(12) 8_556 . . . ? Zn32 N305 C312 C313 169.4(6) . . . . ? Zn32 N305 C311 C310 -166.4(10) . . . . ? Zn52 N312 C332 C333 157(4) 8_556 . . . ? Zn52 N312 C336 C335 -160(3) 8_556 . . . ? Zn52 N305 C312 C313 166(3) . . . . ? Zn52 N305 C311 C310 -161(5) . . . . ? Zn43 N306 C318 C317 179.3(8) . . . . ? Zn43 N306 C314 C315 176.1(16) . . . . ? Zn43 N307 C319 C320 -176.8(11) . . . . ? Zn43 N307 C323 C322 177.4(14) . . . . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -1.0000 -0.0000 0.0000 -0.0016 -0.0084 0.0448 1.0000 0.0000 -0.0000 0.0016 0.0084 -0.0448 0.0000 -1.0000 0.0000 0.0165 0.0990 0.0192 -0.0000 1.0000 -0.0000 -0.0165 -0.0990 -0.0192 2.0001 -1.0000 -0.0000 0.0196 0.1158 -0.0704 2.0000 1.0000 -0.0001 -0.0134 -0.0822 -0.1087 -0.0000 -0.0000 1.0000 -0.0502 0.0103 -0.0097 0.0000 0.0000 -1.0000 0.0502 -0.0103 0.0097 1.0001 0.0000 -1.0000 0.0517 -0.0018 -0.0351 -1.0001 -0.0000 1.0000 -0.0517 0.0018 0.0351 1.0000 0.0000 1.0000 -0.0486 0.0187 -0.0545 -1.0000 -0.0000 -1.0000 0.0486 -0.0187 0.0545 -1.0001 1.0000 1.0000 -0.0682 -0.0971 0.0159 2.0000 1.0000 0.9999 -0.0636 -0.0719 -0.1184 1.0001 2.0000 -2.0000 0.0690 -0.2101 -0.0637 -1.0000 -1.0000 1.0000 -0.0353 0.1008 0.0542 2.0000 -1.0000 0.9999 -0.0306 0.1260 -0.0801 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 -0.263 -0.336 -0.013 3551.3 998.6 ? 2 -0.916 -0.166 -0.166 3551.3 998.6 ?