#------------------------------------------------------------------------------ #$Date: 2024-06-13 05:30:55 +0300 (Thu, 13 Jun 2024) $ #$Revision: 292346 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/18/1571875.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_1571875 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, 0.25[]' _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 2024-01-30 _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 101.107(5) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 34.3804(16) _cell_length_b 15.0439(5) _cell_length_c 30.3200(17) _cell_measurement_reflns_used 6745 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 69.3730 _cell_measurement_theta_min 2.9220 _cell_volume 15388.2(13) _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 (Sheldrick, 2015)' _diffrn_ambient_temperature 100(2) _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 0.994 _diffrn_measured_fraction_theta_max 0.992 _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 -172.00-104.00 0.50 4.00 -- -103.00-120.00 40.00 136 2 \w -103.00 -77.00 0.50 4.00 -- -103.00 120.00 124.00 52 3 \w -132.00 -32.00 0.50 4.00 -- -103.00 154.00 -78.00 200 4 \w -88.00 -30.00 0.50 4.00 -- -103.00 77.00 -30.00 116 5 \w -113.00 -81.00 0.50 4.00 -- -103.00-125.00 90.00 64 6 \w -68.00 -43.00 0.50 4.00 -- -103.00 61.00 120.00 50 7 \w -172.00-136.00 0.50 4.00 -- -103.00-125.00 90.00 72 8 \w -69.00 -44.00 0.50 4.00 -- -103.00 61.00 90.00 50 9 \w -174.00-119.00 0.50 4.00 -- -103.00 -30.00 -60.00 110 10 \w -67.00 -32.00 0.50 4.00 -- -103.00 61.00 -60.00 70 11 \w 47.00 72.00 0.50 4.00 -- 101.75-120.00 40.00 50 12 \w 60.00 85.00 0.50 4.00 -- 101.75-154.00-117.00 50 13 \w 88.00 113.00 0.50 4.00 -- 101.75 154.00 -78.00 50 14 \w 73.00 106.00 0.50 4.00 -- 101.75 -94.00 60.00 66 15 \w 37.00 107.00 0.50 4.00 -- 101.75 -77.00 30.00 140 16 \w 29.00 73.00 0.50 4.00 -- 101.75 -61.00-180.00 88 17 \w 90.00 173.00 0.50 4.00 -- 101.75 45.00 120.00 166 18 \w -102.00 -76.00 0.50 1.00 -- -46.01-154.00-117.00 52 19 \w 48.00 78.00 0.50 1.00 -- 46.01-120.00 40.00 60 20 \w 63.00 100.00 0.50 1.00 -- 46.01 154.00 -78.00 74 21 \w 50.00 75.00 0.50 1.00 -- 46.01-154.00-117.00 50 22 \w -24.00 29.00 0.50 1.00 -- -46.01 19.00 120.00 106 23 \w -119.00 -34.00 0.50 1.00 -- -46.01 -37.00 120.00 170 24 \w -18.00 23.00 0.50 1.00 -- -46.01 19.00 30.00 82 25 \w -27.00 26.00 0.50 1.00 -- 46.01 -19.00 -90.00 106 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_details 'Rigaku Oxford Difffraction, 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 -0.0280977000 _diffrn_orient_matrix_UB_12 0.0136417000 _diffrn_orient_matrix_UB_13 0.0333744000 _diffrn_orient_matrix_UB_21 -0.0006248000 _diffrn_orient_matrix_UB_22 0.1007148000 _diffrn_orient_matrix_UB_23 -0.0093084000 _diffrn_orient_matrix_UB_31 -0.0360289000 _diffrn_orient_matrix_UB_32 -0.0123944000 _diffrn_orient_matrix_UB_33 -0.0384312000 _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 0.0607 _diffrn_reflns_av_unetI/netI 0.0510 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_number 51653 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 68.248 _diffrn_reflns_theta_min 2.971 _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 20.192 _exptl_absorpt_correction_T_max 0.293 _exptl_absorpt_correction_T_min 0.037 _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 1.366 _exptl_crystal_description block _exptl_crystal_F_000 5856 _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.1 _refine_diff_density_max 1.901 _refine_diff_density_min -1.123 _refine_diff_density_rms 0.191 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 634 _refine_ls_number_reflns 13991 _refine_ls_number_restraints 95 _refine_ls_restrained_S_all 1.120 _refine_ls_R_factor_all 0.1379 _refine_ls_R_factor_gt 0.1191 _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^)+(0.3064P)^2^+1.2800P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3901 _refine_ls_wR_factor_ref 0.4189 _reflns_Friedel_coverage 0.000 _reflns_number_gt 9120 _reflns_number_total 13991 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file lt5068.cif _cod_data_source_block 50_10_48c _cod_database_code 1571875 _shelx_shelxl_version_number 2016/6 _chemical_oxdiff_formula '(Zn3 I6 N12 H24 C36) (C15 H16 O3)2 (C6 H12)2' _chemical_oxdiff_usercomment JP-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 0.237 _shelx_estimated_absorpt_t_min 0.077 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2. Restrained distances I403-Zn42 \\sim I303-Zn32 with sigma of 0.02 I404-Zn42 \\sim I304-Zn32 with sigma of 0.02 Zn42-N305 \\sim Zn32-N305 with sigma of 0.02 I403-I404 \\sim I303-I304 with sigma of 0.04 I403-N305 \\sim I303-N305 with sigma of 0.04 I404-N305 \\sim I304-N305 with sigma of 0.04 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 I502-Zn51 \\sim I501-Zn51 with sigma of 0.02 I305-Zn33 \\sim I405-Zn43 with sigma of 0.02 I306-Zn33 \\sim I406-Zn43 with sigma of 0.02 I306-I506 \\sim I406-I506 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 I305-I505 \\sim I405-I505 with sigma of 0.04 I305-Zn53 \\sim I405-Zn53 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 I306-I505 \\sim I406-I505 with sigma of 0.04 I306-Zn53 \\sim I406-Zn53 with sigma of 0.04 Zn33-I505 \\sim Zn43-I505 with sigma of 0.04 Zn33-I506 \\sim Zn43-I506 with sigma of 0.04 Zn33-Zn53 \\sim Zn43-Zn53 with sigma of 0.04 C333-C335 \\sim C332-C336 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints C309 \\sim C313 \\sim C312 \\sim N305 \\sim C311 \\sim C310: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A Uanis(Zn41) = Uanis(Zn51) 4. Rigid body (RIGU) restrains C309, C313, C312, N305, C311, C310 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 5. Others Fixed Sof: I305(0.58585) I306(0.58585) I401(0.3606) I402(0.3606) I403(0.46794) Zn33(0.58585) I404(0.46794) Zn41(0.3606) Zn42(0.46794) I303(0.50244) Zn32(0.50244) I304(0.50244) I503(0.02962) I504(0.02962) Zn52(0.02962) Zn31(0.48521) I301(0.48521) I302(0.48521) I501(0.15419) Zn51(0.15419) I502(0.15419) I505(0.04939) I506(0.04939) Zn53(0.04939) I406(0.36476) Zn43(0.36476) I405(0.36476) Fixed Uiso: I503(0.08) I504(0.08) Zn52(0.08) I505(0.08) I506(0.08) Zn53(0.08) 6.a Aromatic/amide H refined with riding coordinates: C319(H319), C320(H320), C315(H315), C305(H305), C314(H314), C328(H328), C329(H329), C304(H304), C302(H302), C301(H301), C318(H318), C312(H312), C317(H317), C323(H323), C311(H311), C310(H310), C335(H335), C313(H313), C322(H322), C333(H333), C332(H332), C336(H336), C331(H331), C330(H330) ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL 2023ncs7026a_rc1_a.res in C2/c 2023ncs7026a_rc1.res created by SHELXL-2016/6 at 13:06:19 on 30-Jan-2024 REM Old TITL 2023NCS7026a_RC1 in C2/c REM SHELXT solution in C2/c REM R1 0.491, Rweak 0.192, Alpha 0.117, Orientation as input REM Formula found by SHELXT: C36 N13 Zn7 I501 CELL 1.54184 34.3804 15.0439 30.32 90 101.107 90 ZERR 8 0.0016 0.0005 0.0017 0 0.005 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H I N Zn UNIT 288 192 48 96 24 SADI I403 Zn42 I303 Zn32 SADI I404 Zn42 I304 Zn32 SADI Zn42 N305 Zn32 N305 SADI 0.04 I403 I404 I303 I304 SADI 0.04 I403 N305 I303 N305 SADI 0.04 I404 N305 I304 N305 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 I502 Zn51 I501 Zn51 EADP Zn41 Zn51 SADI I305 Zn33 I405 Zn43 SADI I306 Zn33 I406 Zn43 SADI I306 I506 I406 I506 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 I305 I505 I405 I505 SADI 0.04 I305 Zn53 I405 Zn53 SADI 0.04 I306 N306 I406 N306 SADI 0.04 I306 N307 I406 N307 SADI 0.04 I306 I505 I406 I505 SADI 0.04 I306 Zn53 I406 Zn53 SADI 0.04 Zn33 I505 Zn43 I505 SADI 0.04 Zn33 I506 Zn43 I506 SADI 0.04 Zn33 Zn53 Zn43 Zn53 SADI C333 C335 C332 C336 SIMU C309 C313 C312 N305 C311 C310 RIGU C309 C313 C312 N305 C311 C310 L.S. 10 PLAN 69 SIZE 0.1 0.12 0.26 TEMP -173(2) CONF FREE Zn52 C311 FREE Zn53 H323 FREE Zn53 C323 BOND $H LIST 6 MORE -1 ABIN fmap 2 acta REM REM REM WGHT 0.306400 1.280000 FVAR 0.06345 PART 8 I305 3 0.523225 0.649285 0.635833 10.58585 0.09291 0.09287 = 0.09189 -0.00053 -0.00435 0.02538 I306 3 0.618735 0.733706 0.557509 10.58585 0.14365 0.06598 = 0.11376 -0.00557 0.00218 -0.02905 PART 4 I401 3 0.883494 0.750591 0.905971 10.36060 0.12053 0.03993 = 0.34559 0.00786 -0.11729 0.00901 I402 3 0.849721 0.590045 1.019364 10.36060 0.09127 0.25817 = 0.15201 -0.11337 -0.00478 0.00822 PART 6 I403 3 0.732925 -0.234079 0.794056 10.46794 0.14360 0.06008 = 0.18429 0.02848 0.04406 0.02068 PART 8 ZN33 5 0.580733 0.622584 0.594280 10.58585 0.09469 0.05212 = 0.08992 -0.00518 -0.02138 -0.00169 PART 6 I404 3 0.627561 -0.161308 0.693020 10.46794 0.19565 0.06239 = 0.11512 -0.00894 0.00371 -0.02140 PART 4 ZN41 5 0.870162 0.604439 0.945079 10.36060 0.05811 0.05467 = 0.13189 -0.03310 -0.02665 0.03027 PART 6 ZN42 5 0.671440 -0.142009 0.769423 10.46794 0.12563 0.04572 = 0.12075 0.00308 0.01848 -0.00610 PART 0 N302 4 0.718617 0.443367 0.775893 11.00000 0.10080 0.02610 = 0.14789 -0.00784 -0.04771 0.01290 N306 4 0.619513 0.548327 0.641430 11.00000 0.10686 0.04056 = 0.14033 -0.00701 -0.05056 0.00640 N303 4 0.733758 0.309055 0.813157 11.00000 0.09524 0.04904 = 0.14333 -0.00814 -0.03142 0.01162 N310 4 0.538758 0.146898 0.415340 11.00000 0.10295 0.06616 = 0.12893 0.00637 -0.01687 0.00235 N309 4 0.519418 0.229060 0.473769 11.00000 0.09135 0.04256 = 0.12396 0.00167 -0.03147 -0.00189 N304 4 0.680915 0.316363 0.753268 11.00000 0.11238 0.03283 = 0.14819 -0.00860 -0.04686 -0.00001 N307 4 0.561631 0.518906 0.548983 11.00000 0.10851 0.07976 = 0.12171 -0.01743 -0.01490 -0.01881 N301 4 0.829423 0.533307 0.898428 11.00000 0.11010 0.04088 = 0.19323 -0.01271 -0.06808 0.01227 N00I 4 0.419124 -0.014103 0.450169 11.00000 0.10145 0.07796 = 0.17952 -0.00168 -0.03068 -0.01825 C325 1 0.516658 0.159642 0.445985 11.00000 0.11558 0.04369 = 0.11319 -0.01479 -0.01736 -0.02041 N308 4 0.572274 0.280548 0.439425 11.00000 0.08032 0.08767 = 0.12402 -0.01646 -0.02647 0.00167 C319 1 0.532497 0.464007 0.550476 11.00000 0.08005 0.10326 = 0.12781 0.00466 -0.03185 0.01459 AFIX 43 H319 2 0.514704 0.476581 0.570059 11.00000 -1.20000 AFIX 0 C321 1 0.550195 0.369918 0.495002 11.00000 0.10430 0.06545 = 0.11381 -0.00417 -0.03201 -0.01704 C307 1 0.703721 0.272396 0.781531 11.00000 0.11535 0.02922 = 0.16887 -0.01091 -0.02219 -0.00401 N305 4 0.688327 -0.003750 0.780234 11.00000 0.15888 0.04910 = 0.22773 -0.03062 0.01891 -0.02495 C320 1 0.526737 0.386763 0.523881 11.00000 0.09715 0.05968 = 0.11871 -0.00244 -0.02579 -0.01415 AFIX 43 H320 2 0.506001 0.346643 0.526639 11.00000 -1.20000 AFIX 0 C308 1 0.690043 0.404707 0.746816 11.00000 0.09417 0.03445 = 0.13864 -0.00479 -0.01202 0.01042 C316 1 0.665420 0.454866 0.711983 11.00000 0.08063 0.06950 = 0.13288 -0.00658 -0.02293 0.00733 C326 1 0.566053 0.205490 0.413819 11.00000 0.08798 0.06186 = 0.12357 -0.00942 -0.01957 -0.00586 C327 1 0.482290 0.098833 0.448956 11.00000 0.09629 0.03613 = 0.14756 -0.00373 -0.03428 -0.01048 C315 1 0.673409 0.542688 0.703384 11.00000 0.10867 0.04350 = 0.15350 0.01561 -0.05854 -0.01040 AFIX 43 H315 2 0.695089 0.572681 0.721474 11.00000 -1.20000 AFIX 0 C305 1 0.806498 0.567999 0.868032 11.00000 0.12498 0.05078 = 0.21183 -0.01815 -0.07579 0.01500 AFIX 43 H305 2 0.809105 0.630729 0.866463 11.00000 -1.20000 AFIX 0 C306 1 0.740157 0.395654 0.808735 11.00000 0.09966 0.04935 = 0.14035 -0.00061 -0.01356 0.00503 C303 1 0.770197 0.440539 0.840876 11.00000 0.10580 0.03722 = 0.15533 -0.00302 -0.03075 0.01930 C314 1 0.649546 0.585934 0.668311 11.00000 0.12217 0.04442 = 0.14697 -0.00769 -0.06679 -0.01003 AFIX 43 H314 2 0.655100 0.646526 0.663221 11.00000 -1.20000 AFIX 0 C309 1 0.697997 0.176184 0.783231 11.00000 0.11401 0.04248 = 0.13480 -0.00572 -0.02177 0.00566 C328 1 0.464416 0.096110 0.484248 11.00000 0.11588 0.05023 = 0.16283 0.00107 -0.03351 -0.02087 AFIX 43 H328 2 0.472456 0.136081 0.508551 11.00000 -1.20000 AFIX 0 C329 1 0.432988 0.033226 0.486058 11.00000 0.09391 0.08394 = 0.15761 0.00714 -0.02382 -0.01167 AFIX 43 H329 2 0.422590 0.026330 0.512703 11.00000 -1.20000 AFIX 0 C304 1 0.777634 0.532852 0.835703 11.00000 0.13463 0.03780 = 0.20403 -0.00913 -0.09609 0.00419 AFIX 43 H304 2 0.763509 0.567172 0.811528 11.00000 -1.20000 AFIX 0 C302 1 0.792889 0.398718 0.876742 11.00000 0.13108 0.04198 = 0.19642 -0.02609 -0.08578 0.00939 AFIX 43 H302 2 0.788952 0.337179 0.881381 11.00000 -1.20000 AFIX 0 C301 1 0.821958 0.445079 0.906913 11.00000 0.13762 0.03770 = 0.20580 -0.03185 -0.09204 0.01663 AFIX 43 H301 2 0.836361 0.416268 0.932875 11.00000 -1.20000 AFIX 0 C324 1 0.548582 0.287311 0.467668 11.00000 0.09421 0.07835 = 0.12664 -0.01181 -0.02386 -0.00354 C318 1 0.611894 0.458502 0.649628 11.00000 0.13963 0.06931 = 0.19379 -0.01582 -0.10413 0.00622 AFIX 43 H318 2 0.590781 0.427914 0.630891 11.00000 -1.20000 AFIX 0 N311 4 0.644214 0.163227 0.323084 11.00000 0.21730 0.05574 = 0.20825 -0.00915 0.08450 -0.00312 C312 1 0.666141 0.049974 0.754339 11.00000 0.21413 0.06460 = 0.22244 -0.04231 -0.03780 -0.01866 AFIX 43 H312 2 0.646747 0.022728 0.731847 11.00000 -1.20000 AFIX 0 C317 1 0.634478 0.417233 0.683722 11.00000 0.15385 0.05296 = 0.28767 -0.00130 -0.11690 -0.03455 AFIX 43 H317 2 0.628583 0.356817 0.688768 11.00000 -1.20000 AFIX 0 C334 1 0.591840 0.193711 0.382617 11.00000 0.09987 0.07990 = 0.14604 0.00570 -0.01406 -0.00956 C323 1 0.585863 0.501119 0.519708 11.00000 0.16397 0.08144 = 0.19043 -0.04328 0.05151 -0.05835 AFIX 43 H323 2 0.604667 0.545278 0.515823 11.00000 -1.20000 AFIX 0 C311 1 0.717945 0.026297 0.809388 11.00000 0.14832 0.06238 = 0.22950 -0.00501 -0.00420 0.02183 AFIX 43 H311 2 0.735323 -0.012290 0.828717 11.00000 -1.20000 AFIX 0 C310 1 0.723000 0.118362 0.810926 11.00000 0.14274 0.05386 = 0.20263 0.02819 -0.04656 0.01342 AFIX 43 H310 2 0.744534 0.142497 0.831885 11.00000 -1.20000 AFIX 0 C335 1 0.583723 0.133799 0.348251 11.00000 0.12944 0.09322 = 0.19343 -0.03065 -0.02185 0.00371 AFIX 43 H335 2 0.558884 0.104049 0.342836 11.00000 -1.20000 AFIX 0 C313 1 0.665944 0.136390 0.753942 11.00000 0.14008 0.06452 = 0.21242 -0.03269 -0.04089 -0.00573 AFIX 43 H313 2 0.645790 0.170016 0.735380 11.00000 -1.20000 AFIX 0 C322 1 0.585288 0.422598 0.494752 11.00000 0.16529 0.17222 = 0.16705 -0.08743 0.01866 -0.09271 AFIX 43 H322 2 0.605736 0.405826 0.479349 11.00000 -1.20000 AFIX 0 C333 1 0.626077 0.234705 0.383288 11.00000 0.15035 0.07777 = 0.22728 -0.03159 0.04673 -0.00849 AFIX 43 H333 2 0.636250 0.271122 0.408469 11.00000 -1.20000 AFIX 0 C332 1 0.646300 0.228258 0.352079 11.00000 0.18128 0.16580 = 0.20308 -0.05129 0.08607 -0.05438 AFIX 43 H332 2 0.664436 0.274895 0.349794 11.00000 -1.20000 AFIX 0 C336 1 0.610598 0.115474 0.321303 11.00000 0.20172 0.09016 = 0.19714 -0.03871 0.00672 0.03428 AFIX 43 H336 2 0.605379 0.067476 0.300648 11.00000 -1.20000 AFIX 0 C331 1 0.466766 0.046529 0.412467 11.00000 0.21498 0.23849 = 0.17040 -0.08892 -0.02763 -0.13355 AFIX 43 H331 2 0.477399 0.050237 0.385835 11.00000 -1.20000 AFIX 0 PART 7 I303 3 0.752716 -0.216831 0.822607 10.50244 0.19772 0.07196 = 0.43085 0.08372 0.12607 0.05791 ZN32 5 0.688469 -0.146106 0.789225 10.50244 0.20876 0.03847 = 0.37533 0.00392 0.07934 -0.00006 I304 3 0.651884 -0.191224 0.711132 10.50244 0.33507 0.09232 = 0.29688 -0.06479 0.12340 -0.07782 PART 8 I503 3 0.759808 -0.195004 0.855652 10.02962 10.08000 I504 3 0.645511 -0.210302 0.740920 10.02962 10.08000 ZN52 5 0.691461 -0.144580 0.791262 10.02962 10.08000 PART 7 ZN31 5 0.874324 0.585129 0.946433 10.48521 0.11316 0.06524 = 0.28003 -0.07563 -0.09945 0.05683 I301 3 0.891226 0.736431 0.913501 10.48521 0.15898 0.04342 = 0.32899 -0.00315 -0.15317 0.01124 I302 3 0.846886 0.576871 1.017551 10.48521 0.15604 0.15482 = 0.36190 -0.09104 -0.07456 0.02002 PART 8 I501 3 0.872927 0.733327 0.931028 10.15419 0.12737 0.04799 = 0.32379 0.00909 -0.15254 -0.01956 ZN51 5 0.858306 0.592450 0.963625 10.15419 0.05811 0.05467 = 0.13189 -0.03310 -0.02665 0.03027 I502 3 0.840514 0.536123 1.032081 10.15419 0.09017 0.15628 = 0.14921 -0.07682 -0.01870 0.00570 PART 0 C330 1 0.436806 -0.009501 0.414245 11.00000 0.21431 0.20025 = 0.22714 -0.08417 -0.00922 -0.13311 AFIX 43 H330 2 0.427709 -0.047316 0.389296 11.00000 -1.20000 AFIX 0 PART 10 I505 3 0.535522 0.662992 0.617737 10.04939 10.08000 I506 3 0.640795 0.721741 0.542963 10.04939 10.08000 ZN53 5 0.600095 0.615009 0.569511 10.04939 10.08000 PART 9 I406 3 0.611714 0.737411 0.565125 10.36476 0.13885 0.05227 = 0.30508 0.01287 -0.08138 0.00324 ZN43 5 0.575644 0.616547 0.598195 10.36476 0.12585 0.04203 = 0.21974 0.00493 -0.08988 0.00989 I405 3 0.515512 0.645858 0.633708 10.36476 0.22385 0.11169 = 0.38215 -0.00580 -0.14217 0.07169 HKLF 4 REM 2023ncs7026a_rc1_a.res in C2/c REM R1 = 0.1191 for 9120 Fo > 4sig(Fo) and 0.1379 for all 13991 data REM 634 parameters refined using 95 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 1.901, deepest hole -1.123, 1-sigma level 0.191 Q1 1 0.6240 0.7146 0.5933 11.00000 0.05 1.90 Q2 1 0.6541 -0.2033 0.7581 11.00000 0.05 1.70 Q3 1 0.8442 0.5861 0.9866 11.00000 0.05 1.57 Q4 1 0.7748 -0.2148 0.7923 11.00000 0.05 1.42 Q5 1 0.5160 0.6461 0.5940 11.00000 0.05 1.37 Q6 1 0.9049 0.7414 0.8677 11.00000 0.05 1.27 Q7 1 0.7530 -0.2020 0.8729 11.00000 0.05 1.24 Q8 1 0.8859 0.5986 0.9104 11.00000 0.05 1.17 Q9 1 0.6451 0.7208 0.5251 11.00000 0.05 1.16 Q10 1 0.6807 -0.2031 0.6970 11.00000 0.05 1.12 Q11 1 0.6853 -0.1451 0.8259 11.00000 0.05 1.01 Q12 1 0.8899 0.7437 0.9457 11.00000 0.05 0.92 Q13 1 0.5880 0.7401 0.6127 11.00000 0.05 0.84 Q14 1 0.4969 0.6515 0.6655 11.00000 0.05 0.84 Q15 1 0.5881 0.6001 0.6242 11.00000 0.05 0.78 Q16 1 0.7125 -0.1470 0.7631 11.00000 0.05 0.76 Q17 1 0.4974 0.2654 0.4804 11.00000 0.05 0.75 Q18 1 0.7101 -0.1473 0.7936 11.00000 0.05 0.74 Q19 1 0.5175 0.1602 0.4819 11.00000 0.05 0.70 Q20 1 0.7990 0.3021 0.8607 11.00000 0.05 0.70 Q21 1 0.8209 0.5869 1.0579 11.00000 0.05 0.70 Q22 1 0.5471 0.1583 0.4366 11.00000 0.05 0.67 Q23 1 0.5725 0.7526 0.6399 11.00000 0.05 0.67 Q24 1 0.6011 0.5826 0.5424 11.00000 0.05 0.66 Q25 1 0.5841 -0.1586 0.6962 11.00000 0.05 0.64 Q26 1 0.7858 0.3502 0.8677 11.00000 0.05 0.60 Q27 1 0.4551 -0.0453 0.4501 11.00000 0.05 0.59 Q28 1 0.6305 0.2625 0.4231 11.00000 0.05 0.58 Q29 1 0.6134 0.2724 0.4456 11.00000 0.05 0.54 Q30 1 0.8101 0.4613 0.9787 11.00000 0.05 0.54 Q31 1 0.5782 0.5944 0.5590 11.00000 0.05 0.53 Q32 1 0.5718 0.4074 0.4640 11.00000 0.05 0.53 Q33 1 0.4864 0.0250 0.4389 11.00000 0.05 0.52 Q34 1 0.5040 0.0071 0.4666 11.00000 0.05 0.52 Q35 1 0.4469 -0.0629 0.4924 11.00000 0.05 0.52 Q36 1 0.7296 0.3206 0.8331 11.00000 0.05 0.51 Q37 1 0.6902 0.7094 0.5511 11.00000 0.05 0.49 Q38 1 0.7800 0.1818 0.8488 11.00000 0.05 0.48 Q39 1 0.7112 0.3000 0.8038 11.00000 0.05 0.47 Q40 1 0.8143 0.5516 1.1118 11.00000 0.05 0.46 Q41 1 0.7775 0.4004 0.8027 11.00000 0.05 0.45 Q42 1 0.4611 -0.0768 0.4151 11.00000 0.05 0.45 Q43 1 0.7395 -0.3168 0.8158 11.00000 0.05 0.44 Q44 1 0.8467 0.4415 0.8966 11.00000 0.05 0.44 Q45 1 0.8590 0.6863 0.9455 11.00000 0.05 0.43 Q46 1 0.7131 -0.0264 0.8534 11.00000 0.05 0.43 Q47 1 0.8192 0.5278 1.0665 11.00000 0.05 0.43 Q48 1 0.4630 -0.0467 0.4026 11.00000 0.05 0.41 Q49 1 0.8011 -0.2180 0.9119 11.00000 0.05 0.41 Q50 1 0.6000 -0.1442 0.6426 11.00000 0.05 0.41 Q51 1 0.7102 0.0069 0.7547 11.00000 0.05 0.41 Q52 1 0.8045 -0.1898 0.9078 11.00000 0.05 0.41 Q53 1 0.7496 0.6024 0.8081 11.00000 0.05 0.40 Q54 1 0.6976 0.1399 0.7529 11.00000 0.05 0.40 Q55 1 0.7148 0.1580 0.7904 11.00000 0.05 0.40 Q56 1 0.5590 0.5192 0.5872 11.00000 0.05 0.40 Q57 1 0.7296 0.1345 0.8298 11.00000 0.05 0.40 Q58 1 0.6046 0.5444 0.6097 11.00000 0.05 0.40 Q59 1 0.7006 0.4132 0.7370 11.00000 0.05 0.40 Q60 1 0.5655 0.3591 0.5376 11.00000 0.05 0.39 Q61 1 0.5384 0.3811 0.5565 11.00000 0.05 0.39 Q62 1 0.5989 0.5462 0.6730 11.00000 0.05 0.39 Q63 1 0.5243 0.0518 0.4494 11.00000 0.05 0.39 Q64 1 0.6888 -0.0019 0.8140 11.00000 0.05 0.38 Q65 1 0.7000 0.0389 0.7423 11.00000 0.05 0.38 Q66 1 0.6729 0.4114 0.7600 11.00000 0.05 0.37 Q67 1 0.6840 0.4216 0.6924 11.00000 0.05 0.37 Q68 1 0.4256 0.0567 0.4573 11.00000 0.05 0.37 Q69 1 0.7127 0.4954 0.7760 11.00000 0.05 0.37 ; _shelx_res_checksum 67212 _shelx_hkl_file ; 0 0 -2 4.86 0.42 0 0 3 1.89 2.03 0 0 -3 0.64 0.50 0 0 4 117.22 7.02 0 0 -4 144.97 6.52 0 0 -5 1.30 0.84 0 0 5 -3.83 2.61 0 0 6 368.87 17.34 0 0 -6 373.17 17.09 0 0 -7 -0.95 1.06 0 0 -8 886.70 38.85 0 0 8 790.61 38.96 0 0 -10 88.49 4.21 0 0 10 51.31 5.86 0 0 -11 1.88 1.33 0 0 11 -9.41 3.75 0 0 12 158.80 9.61 0 0 -12 206.09 9.11 0 0 -13 -1.18 1.43 0 0 13 -6.19 2.86 0 0 -14 73.83 3.58 0 0 14 82.47 4.37 0 0 15 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-4.4883 0.0785 34 2 2 -0.3200 0.0808 34 2 3 -0.8631 -0.8695 34 2 4 -1.9396 -0.0103 34 2 5 -1.8243 0.2248 34 2 6 -0.5851 0.2518 34 2 7 -1.1711 -0.4702 34 2 8 -1.5100 0.0320 34 2 9 -2.2684 0.7853 34 2 10 3.5360 -0.5130 34 2 11 -3.7361 -0.1350 34 2 12 3.3831 0.0537 34 2 13 -3.1106 0.1695 34 2 14 5.7717 0.7125 34 4 0 0.4466 -0.2782 34 4 1 -4.0365 0.5087 34 4 2 3.5151 -0.4302 34 4 3 -3.4161 0.2551 34 4 4 3.9167 0.3235 34 4 5 -4.5779 -0.4407 34 4 6 2.0012 0.3538 34 4 7 -2.9917 0.5703 34 4 8 -0.2034 0.1211 34 4 9 -1.2122 0.5936 34 4 10 -2.1712 0.0392 34 4 11 2.2849 0.0690 34 4 12 -0.5195 -0.6659 34 4 13 0.9909 0.6901 34 6 0 5.5237 0.5351 34 6 1 -0.2569 -0.1374 34 6 2 -2.3063 -0.1840 34 6 3 -2.9706 0.0418 34 6 4 2.1521 0.6748 34 6 5 4.7169 -0.5762 34 6 6 -2.3009 0.5320 34 6 7 -5.7796 -1.0584 34 6 8 2.4617 0.2217 34 6 9 -1.0084 -0.1584 34 6 10 -2.7845 0.0364 34 8 0 2.7920 -0.0996 34 8 1 1.9296 0.3286 34 8 2 -1.7770 -0.2296 34 8 3 -3.2127 0.6477 34 8 4 0.2350 -0.2368 34 8 5 0.3877 0.6517 34 8 6 -0.7410 0.3286 34 8 7 -0.1803 1.0289 35 1 0 -0.7511 -1.3222 35 1 1 10.6055 1.0758 35 1 2 -3.8393 -1.0325 35 1 3 1.5071 0.3431 35 1 4 -4.3955 -0.3189 35 1 5 3.3651 -0.3201 35 1 6 -3.7081 -0.5345 35 1 7 -1.1159 1.4028 35 1 8 -1.0142 -1.2667 35 1 9 -5.6063 0.8008 35 1 10 0.2024 0.4008 35 1 11 2.9008 0.7476 35 1 12 -4.7214 -0.0667 35 1 13 1.1712 1.7866 35 3 0 -6.0918 0.8625 35 3 1 -3.9872 -0.5756 35 3 2 2.2392 0.1808 35 3 3 -1.5178 -0.3002 35 3 4 -0.1943 0.9095 35 3 5 0.8435 -0.1124 35 3 6 1.8794 0.5319 35 3 7 -3.2970 -0.3564 35 3 8 6.0169 0.1796 35 3 9 2.2914 0.3472 35 3 10 -6.4250 -0.2765 35 3 11 0.0958 0.2192 35 3 12 3.4726 0.3285 35 5 0 6.1194 -0.3260 35 5 1 -1.6678 0.8010 35 5 2 1.4673 -0.7640 35 5 3 1.0579 0.2145 35 5 4 2.3370 -0.6096 35 5 5 -1.4252 0.7775 35 5 6 1.7766 0.0926 35 5 7 -1.7769 0.2118 35 5 8 -0.0927 -0.2807 35 5 9 1.5346 0.2718 35 5 10 -1.3416 0.0575 35 7 0 2.8854 0.2530 35 7 1 -1.8291 -0.2558 35 7 2 1.5319 0.1993 35 7 3 0.3776 -0.3365 35 7 4 1.7100 -0.2178 35 7 5 0.1427 -0.2830 35 7 6 -1.8985 0.8373 35 7 7 1.1765 -0.0715 35 9 0 -1.1017 0.1781 35 9 1 5.2976 0.8700 36 0 0 -4.8236 0.7699 36 0 2 4.2665 0.0246 36 0 4 -4.4754 2.9027 36 0 6 1.6009 3.1050 36 0 8 -0.3979 0.7006 36 0 10 2.0357 0.0195 36 2 0 -3.4845 0.2616 36 2 1 1.9248 -0.4268 36 2 2 -4.1075 -0.4239 36 2 3 2.5324 0.0325 36 2 4 -1.5890 -0.2855 36 2 5 -1.6613 0.4463 36 2 6 -0.8806 0.2117 36 2 7 2.4413 0.7867 36 2 8 -4.6307 -0.5498 36 2 9 0.6116 0.6804 36 2 10 -5.1793 0.6960 36 2 11 -1.5895 -1.5202 36 4 0 -2.1588 -0.2568 36 4 1 1.4041 -0.2893 36 4 2 -1.6118 -0.1895 36 4 3 2.8122 -1.0585 36 4 4 -2.8282 0.2929 36 4 5 5.4736 -0.6664 36 4 6 -1.9137 0.4819 36 4 7 1.6074 0.0609 36 4 8 1.5424 -0.1478 36 4 9 1.9464 -0.7636 36 6 0 1.6466 -0.5282 36 6 1 0.4125 0.6518 36 6 2 -0.0838 -0.1318 36 6 3 0.0762 0.5276 36 6 4 0.2064 -0.6546 36 6 5 3.3014 0.0332 36 6 6 0.1775 -0.3405 36 6 7 -1.8009 -0.2500 36 8 0 4.0346 0.0451 36 8 1 0.8559 0.3247 37 1 0 2.7270 -0.0610 37 1 1 1.1626 0.8271 37 1 2 0.9526 0.0812 37 1 3 -1.3833 0.0367 37 1 4 3.3716 0.7151 37 1 5 1.8610 0.7084 37 1 6 -1.2335 -0.5468 37 1 7 1.1957 0.4497 37 1 8 3.0654 0.2992 37 1 9 1.5459 -0.1209 37 3 0 -3.7316 -0.0776 37 3 1 -0.5380 -0.1793 37 3 2 2.3782 -0.0163 37 3 3 0.8207 0.3038 37 3 4 -2.6113 0.1305 37 3 5 3.0752 0.1595 37 3 6 -1.2108 0.0905 37 3 7 -1.0372 -0.3126 37 3 8 1.7662 -0.3332 37 5 0 -0.6774 0.4707 37 5 1 2.8589 -0.9501 37 5 2 -5.4049 0.1876 37 5 3 -0.4895 -0.1487 37 5 4 -0.2862 0.3399 37 5 5 0.7813 0.3485 37 5 6 -0.9224 -0.0799 37 7 0 0.1707 -0.2248 37 7 1 -1.5947 -0.2264 38 0 0 -3.6016 -1.1272 38 0 2 5.7346 -0.6633 38 0 4 2.4302 1.2199 38 0 6 4.4535 1.6895 38 2 0 2.4852 -0.0315 38 2 1 0.3477 -0.3782 38 2 2 2.9764 -0.4068 38 2 3 0.5410 0.4410 38 2 4 0.0253 -0.0435 38 2 5 1.7938 0.2528 38 2 6 0.3263 0.1870 38 2 7 2.1305 1.3456 38 4 0 -0.0414 -0.1523 38 4 1 -1.2617 0.2365 38 4 2 3.0446 0.5768 38 4 3 -0.3715 -0.2968 38 4 4 4.5931 0.0394 38 4 5 -0.7094 0.6514 38 6 0 -2.6374 -0.4652 38 6 1 -2.9083 -0.2027 39 1 0 0.4830 0.1732 39 1 1 -2.8011 0.6804 39 1 2 2.8477 0.2929 39 1 3 3.5546 -0.5807 39 1 4 -0.4531 1.2398 39 1 5 -0.7458 -0.0001 39 3 0 -0.8274 -0.7013 39 3 1 -1.0784 0.3670 39 3 2 0.3752 -0.2501 39 3 3 1.2388 0.2152 39 5 0 0.2744 -0.1892 40 0 0 2.5983 -1.4420 40 0 2 -2.7852 -1.7643 40 2 0 -3.3202 -0.2467 40 2 1 -0.3995 -0.5927 0 0 0 0.0 0.0 ; _shelx_fab_checksum 28107 _platon_squeeze_void_probe_radius 1.20 _olex2_date_sample_data_collection 2023-04-19 _olex2_date_sample_submission 2023-04-19 _olex2_submission_original_sample_id 50_10_48c _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 3.281 _oxdiff_exptl_absorpt_empirical_full_min 0.381 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 I305 I 0.52322(9) 0.6493(2) 0.63583(6) 0.0955(5) Uani 0.5858 1 d D . P A 8 I306 I 0.61873(13) 0.7337(2) 0.55751(9) 0.1108(10) Uani 0.5858 1 d D . P A 8 I401 I 0.8835(3) 0.7506(5) 0.9060(5) 0.190(4) Uani 0.3606 1 d D . P B 4 I402 I 0.8497(2) 0.5900(11) 1.0194(2) 0.171(5) Uani 0.3606 1 d D . P B 4 I403 I 0.73292(11) -0.2341(2) 0.79406(12) 0.1277(9) Uani 0.4679 1 d D . P C 6 Zn33 Zn 0.58073(17) 0.6226(4) 0.59428(14) 0.0841(14) Uani 0.5858 1 d D . P A 8 I404 I 0.62756(12) -0.16131(19) 0.69302(8) 0.1279(10) Uani 0.4679 1 d D . P C 6 Zn41 Zn 0.8702(2) 0.6044(6) 0.9451(3) 0.088(2) Uani 0.3606 1 d D . P B 4 Zn42 Zn 0.67144(17) -0.1420(3) 0.76942(18) 0.0981(13) Uani 0.4679 1 d D . P C 6 N302 N 0.7186(3) 0.4434(5) 0.7759(4) 0.101(3) Uani 1 1 d . . . . . N306 N 0.6195(3) 0.5483(6) 0.6414(4) 0.106(3) Uani 1 1 d D . . . . N303 N 0.7338(3) 0.3091(6) 0.8132(4) 0.103(3) Uani 1 1 d . . . . . N310 N 0.5388(3) 0.1469(7) 0.4153(4) 0.105(3) Uani 1 1 d . . . . . N309 N 0.5194(3) 0.2291(6) 0.4738(3) 0.093(3) Uani 1 1 d . . . . . N304 N 0.6809(3) 0.3164(6) 0.7533(4) 0.107(4) Uani 1 1 d . . . . . N307 N 0.5616(4) 0.5189(8) 0.5490(4) 0.108(3) Uani 1 1 d D . . . . N301 N 0.8294(3) 0.5333(7) 0.8984(5) 0.128(5) Uani 1 1 d D . . . . N00I N 0.4191(4) -0.0141(9) 0.4502(6) 0.127(5) Uani 1 1 d . . . . . C325 C 0.5167(4) 0.1596(7) 0.4460(5) 0.096(4) Uani 1 1 d . . . . . N308 N 0.5723(3) 0.2805(8) 0.4394(4) 0.103(3) Uani 1 1 d . . . . . C319 C 0.5325(3) 0.4640(11) 0.5505(5) 0.111(4) Uani 1 1 d . . . . . H319 H 0.514704 0.476581 0.570059 0.133 Uiso 1 1 calc R U . . . C321 C 0.5502(4) 0.3699(9) 0.4950(5) 0.102(4) Uani 1 1 d . . . . . C307 C 0.7037(4) 0.2724(7) 0.7815(6) 0.111(4) Uani 1 1 d . . . . . N305 N 0.6883(5) -0.0037(9) 0.7802(7) 0.148(5) Uani 1 1 d D U . . . C320 C 0.5267(4) 0.3868(8) 0.5239(5) 0.098(4) Uani 1 1 d . . . . . H320 H 0.506001 0.346643 0.526639 0.118 Uiso 1 1 calc R U . . . C308 C 0.6900(3) 0.4047(7) 0.7468(5) 0.094(3) Uani 1 1 d . . . . . C316 C 0.6654(3) 0.4549(9) 0.7120(5) 0.100(4) Uani 1 1 d . . . . . C326 C 0.5661(3) 0.2055(8) 0.4138(5) 0.096(3) Uani 1 1 d . . . . . C327 C 0.4823(4) 0.0988(7) 0.4490(6) 0.101(4) Uani 1 1 d . . . . . C315 C 0.6734(4) 0.5427(7) 0.7034(5) 0.113(5) Uani 1 1 d . . . . . H315 H 0.695089 0.572681 0.721474 0.136 Uiso 1 1 calc R U . . . C305 C 0.8065(5) 0.5680(9) 0.8680(7) 0.144(7) Uani 1 1 d . . . . . H305 H 0.809105 0.630729 0.866463 0.172 Uiso 1 1 calc R U . . . C306 C 0.7402(4) 0.3957(8) 0.8087(5) 0.101(4) Uani 1 1 d . . . . . C303 C 0.7702(4) 0.4405(7) 0.8409(5) 0.107(4) Uani 1 1 d . . . . . C314 C 0.6495(4) 0.5859(8) 0.6683(5) 0.117(5) Uani 1 1 d . . . . . H314 H 0.655100 0.646526 0.663221 0.140 Uiso 1 1 calc R U . . . C309 C 0.6980(4) 0.1762(8) 0.7832(5) 0.103(4) Uani 1 1 d . U . . . C328 C 0.4644(5) 0.0961(9) 0.4842(7) 0.118(5) Uani 1 1 d . . . . . H328 H 0.472456 0.136081 0.508551 0.141 Uiso 1 1 calc R U . . . C329 C 0.4330(4) 0.0332(11) 0.4861(6) 0.118(5) Uani 1 1 d . . . . . H329 H 0.422590 0.026330 0.512703 0.142 Uiso 1 1 calc R U . . . C304 C 0.7776(5) 0.5329(8) 0.8357(6) 0.143(7) Uani 1 1 d . . . . . H304 H 0.763509 0.567172 0.811528 0.171 Uiso 1 1 calc R U . . . C302 C 0.7929(5) 0.3987(8) 0.8767(6) 0.139(7) Uani 1 1 d . . . . . H302 H 0.788952 0.337179 0.881381 0.167 Uiso 1 1 calc R U . . . C301 C 0.8220(5) 0.4451(8) 0.9069(7) 0.144(8) Uani 1 1 d . . . . . H301 H 0.836361 0.416268 0.932875 0.172 Uiso 1 1 calc R U . . . C324 C 0.5486(4) 0.2873(10) 0.4677(5) 0.106(4) Uani 1 1 d . . . . . C318 C 0.6119(5) 0.4585(10) 0.6496(7) 0.152(8) Uani 1 1 d . . . . . H318 H 0.590781 0.427914 0.630891 0.183 Uiso 1 1 calc R U . . . N311 N 0.6442(7) 0.1632(10) 0.3231(8) 0.155(6) Uani 1 1 d . . . . . C312 C 0.6661(9) 0.0500(14) 0.7543(10) 0.178(8) Uani 1 1 d . U . . . H312 H 0.646747 0.022728 0.731847 0.213 Uiso 1 1 calc R U . . . C317 C 0.6345(6) 0.4172(10) 0.6837(9) 0.186(12) Uani 1 1 d . . . . . H317 H 0.628583 0.356817 0.688768 0.223 Uiso 1 1 calc R U . . . C334 C 0.5918(4) 0.1937(10) 0.3826(6) 0.114(4) Uani 1 1 d . . . . . C323 C 0.5859(7) 0.5011(12) 0.5197(8) 0.143(7) Uani 1 1 d . . . . . H323 H 0.604667 0.545278 0.515823 0.172 Uiso 1 1 calc R U . . . C311 C 0.7179(6) 0.0263(12) 0.8094(9) 0.152(6) Uani 1 1 d . U . . . H311 H 0.735323 -0.012290 0.828717 0.183 Uiso 1 1 calc R U . . . C310 C 0.7230(6) 0.1184(10) 0.8109(8) 0.144(6) Uani 1 1 d . U . . . H310 H 0.744534 0.142497 0.831885 0.172 Uiso 1 1 calc R U . . . C335 C 0.5837(6) 0.1338(13) 0.3483(8) 0.146(7) Uani 1 1 d D . . . . H335 H 0.558884 0.104049 0.342836 0.175 Uiso 1 1 calc R U . . . C313 C 0.6659(6) 0.1364(11) 0.7539(8) 0.149(7) Uani 1 1 d . U . . . H313 H 0.645790 0.170016 0.735380 0.179 Uiso 1 1 calc R U . . . C322 C 0.5853(7) 0.4226(18) 0.4948(7) 0.170(10) Uani 1 1 d . . . . . H322 H 0.605736 0.405826 0.479349 0.204 Uiso 1 1 calc R U . . . C333 C 0.6261(7) 0.2347(13) 0.3833(10) 0.150(8) Uani 1 1 d D . . . . H333 H 0.636250 0.271122 0.408469 0.181 Uiso 1 1 calc R U . . . C332 C 0.6463(9) 0.228(2) 0.3521(10) 0.177(11) Uani 1 1 d D . . . . H332 H 0.664436 0.274895 0.349794 0.212 Uiso 1 1 calc R U . . . C336 C 0.6106(9) 0.1155(15) 0.3213(10) 0.167(9) Uani 1 1 d D . . . . H336 H 0.605379 0.067476 0.300648 0.201 Uiso 1 1 calc R U . . . C331 C 0.4668(9) 0.047(2) 0.4125(8) 0.217(15) Uani 1 1 d . . . . . H331 H 0.477399 0.050237 0.385835 0.260 Uiso 1 1 calc R U . . . I303 I 0.75272(17) -0.2168(3) 0.8226(3) 0.225(3) Uani 0.5024 1 d D . P C 7 Zn32 Zn 0.6885(4) -0.1461(6) 0.7892(5) 0.204(5) Uani 0.5024 1 d D . P C 7 I304 I 0.6519(3) -0.1912(3) 0.7111(3) 0.233(3) Uani 0.5024 1 d D . P C 7 I503 I 0.7598(7) -0.195(2) 0.8557(7) 0.080 Uiso 0.0296 1 d . U P C 8 I504 I 0.6455(6) -0.2103(18) 0.7409(7) 0.080 Uiso 0.0296 1 d . U P C 8 Zn52 Zn 0.691(2) -0.145(5) 0.791(2) 0.080 Uiso 0.0296 1 d . U P C 8 Zn31 Zn 0.8743(3) 0.5851(6) 0.9464(4) 0.171(5) Uani 0.4852 1 d D . P B 7 I301 I 0.8912(2) 0.7364(6) 0.9135(5) 0.204(4) Uani 0.4852 1 d D . P B 7 I302 I 0.8469(3) 0.5769(8) 1.0176(4) 0.241(6) Uani 0.4852 1 d D . P B 7 I501 I 0.8729(5) 0.7333(13) 0.9310(10) 0.193(11) Uani 0.1542 1 d D . P B 8 Zn51 Zn 0.8583(4) 0.5924(10) 0.9636(5) 0.088(2) Uani 0.1542 1 d D . P B 8 I502 I 0.8405(4) 0.5361(12) 1.0321(5) 0.137(4) Uani 0.1542 1 d D . P B 8 C330 C 0.4368(10) -0.010(2) 0.4142(12) 0.221(16) Uani 1 1 d . . . . . H330 H 0.427709 -0.047316 0.389296 0.265 Uiso 1 1 calc R U . . . I505 I 0.5355(6) 0.6630(15) 0.6177(7) 0.080 Uiso 0.0494 1 d . U P A 10 I506 I 0.6408(5) 0.7217(11) 0.5430(5) 0.080 Uiso 0.0494 1 d . U P A 10 Zn53 Zn 0.6001(9) 0.615(2) 0.5695(10) 0.080 Uiso 0.0494 1 d . U P A 10 I406 I 0.6117(2) 0.7374(4) 0.5651(3) 0.182(4) Uani 0.3648 1 d D . P A 9 Zn43 Zn 0.5756(3) 0.6165(6) 0.5982(4) 0.146(7) Uani 0.3648 1 d D . P A 9 I405 I 0.5155(3) 0.6459(7) 0.6337(4) 0.266(8) Uani 0.3648 1 d D . P A 9 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 I305 0.0929(9) 0.0929(14) 0.0919(7) -0.0005(7) -0.0044(7) 0.0254(8) I306 0.144(2) 0.0660(16) 0.1138(10) -0.0056(9) 0.0022(13) -0.0291(13) I401 0.121(4) 0.040(2) 0.346(11) 0.008(3) -0.117(6) 0.009(2) I402 0.091(3) 0.258(13) 0.152(4) -0.113(6) -0.005(2) 0.008(4) I403 0.144(2) 0.0601(13) 0.184(2) 0.0285(13) 0.0441(17) 0.0207(13) Zn33 0.095(2) 0.052(3) 0.0899(18) -0.0052(15) -0.0214(18) -0.0017(16) I404 0.196(3) 0.0624(13) 0.1151(13) -0.0089(9) 0.0037(14) -0.0214(14) Zn41 0.058(3) 0.055(3) 0.132(5) -0.033(3) -0.027(2) 0.030(3) Zn42 0.126(3) 0.046(2) 0.121(2) 0.0031(16) 0.018(3) -0.0061(19) N302 0.101(5) 0.026(3) 0.148(7) -0.008(4) -0.048(5) 0.013(3) N306 0.107(6) 0.041(4) 0.140(7) -0.007(4) -0.051(6) 0.006(4) N303 0.095(5) 0.049(5) 0.143(7) -0.008(5) -0.031(5) 0.012(4) N310 0.103(6) 0.066(6) 0.129(8) 0.006(5) -0.017(6) 0.002(5) N309 0.091(5) 0.043(4) 0.124(6) 0.002(4) -0.031(5) -0.002(4) N304 0.112(6) 0.033(4) 0.148(8) -0.009(4) -0.047(6) 0.000(4) N307 0.109(7) 0.080(7) 0.122(7) -0.017(6) -0.015(6) -0.019(5) N301 0.110(6) 0.041(5) 0.193(11) -0.013(6) -0.068(7) 0.012(4) N00I 0.101(7) 0.078(8) 0.180(12) -0.002(8) -0.031(8) -0.018(6) C325 0.116(8) 0.044(5) 0.113(7) -0.015(5) -0.017(7) -0.020(5) N308 0.080(5) 0.088(7) 0.124(7) -0.016(6) -0.026(6) 0.002(5) C319 0.080(5) 0.103(10) 0.128(8) 0.005(7) -0.032(6) 0.015(6) C321 0.104(7) 0.065(7) 0.114(8) -0.004(6) -0.032(7) -0.017(6) C307 0.115(8) 0.029(5) 0.169(11) -0.011(6) -0.022(8) -0.004(5) N305 0.159(10) 0.049(6) 0.228(14) -0.031(7) 0.019(9) -0.025(6) C320 0.097(6) 0.060(6) 0.119(8) -0.002(6) -0.026(7) -0.014(5) C308 0.094(6) 0.034(5) 0.139(8) -0.005(5) -0.012(6) 0.010(4) C316 0.081(5) 0.070(7) 0.133(8) -0.007(6) -0.023(6) 0.007(5) C326 0.088(6) 0.062(6) 0.124(8) -0.009(6) -0.020(6) -0.006(5) C327 0.096(6) 0.036(5) 0.148(10) -0.004(6) -0.034(8) -0.010(4) C315 0.109(7) 0.044(5) 0.153(10) 0.016(6) -0.059(7) -0.010(5) C305 0.125(9) 0.051(7) 0.212(16) -0.018(8) -0.076(11) 0.015(6) C306 0.100(6) 0.049(6) 0.140(9) -0.001(6) -0.014(7) 0.005(5) C303 0.106(7) 0.037(5) 0.155(10) -0.003(5) -0.031(7) 0.019(5) C314 0.122(8) 0.044(5) 0.147(9) -0.008(6) -0.067(8) -0.010(5) C309 0.114(7) 0.042(5) 0.135(8) -0.006(5) -0.022(6) 0.006(5) C328 0.116(9) 0.050(6) 0.163(13) 0.001(7) -0.034(10) -0.021(6) C329 0.094(7) 0.084(9) 0.158(11) 0.007(8) -0.024(8) -0.012(6) C304 0.135(9) 0.038(5) 0.204(14) -0.009(7) -0.096(11) 0.004(5) C302 0.131(9) 0.042(6) 0.196(14) -0.026(7) -0.086(10) 0.009(6) C301 0.138(10) 0.038(5) 0.206(14) -0.032(7) -0.092(11) 0.017(6) C324 0.094(7) 0.078(8) 0.127(9) -0.012(7) -0.024(8) -0.004(6) C318 0.140(10) 0.069(8) 0.194(14) -0.016(8) -0.104(12) 0.006(7) N311 0.217(19) 0.056(7) 0.208(16) -0.009(9) 0.085(15) -0.003(9) C312 0.214(16) 0.065(7) 0.222(16) -0.042(9) -0.038(13) -0.019(8) C317 0.154(13) 0.053(8) 0.29(3) -0.001(10) -0.117(16) -0.035(8) C334 0.100(7) 0.080(9) 0.146(11) 0.006(8) -0.014(8) -0.010(6) C323 0.164(15) 0.081(10) 0.190(16) -0.043(11) 0.052(14) -0.058(11) C311 0.148(11) 0.062(7) 0.229(16) -0.005(9) -0.004(10) 0.022(7) C310 0.143(10) 0.054(6) 0.203(14) 0.028(7) -0.047(10) 0.013(6) C335 0.129(11) 0.093(12) 0.193(17) -0.031(12) -0.022(12) 0.004(9) C313 0.140(10) 0.065(7) 0.212(15) -0.033(8) -0.041(10) -0.006(7) C322 0.165(15) 0.17(2) 0.167(15) -0.087(15) 0.019(13) -0.093(16) C333 0.150(15) 0.078(11) 0.23(2) -0.032(12) 0.047(16) -0.008(10) C332 0.18(2) 0.17(3) 0.20(2) -0.051(19) 0.09(2) -0.054(18) C336 0.20(2) 0.090(14) 0.20(2) -0.039(13) 0.007(18) 0.034(15) C331 0.21(2) 0.24(3) 0.170(17) -0.089(19) -0.028(16) -0.13(2) I303 0.198(4) 0.072(2) 0.431(10) 0.084(4) 0.126(6) 0.058(3) Zn32 0.209(9) 0.038(2) 0.375(16) 0.004(5) 0.079(9) 0.000(4) I304 0.335(8) 0.092(3) 0.297(7) -0.065(3) 0.123(6) -0.078(4) Zn31 0.113(5) 0.065(4) 0.280(9) -0.076(4) -0.099(5) 0.057(3) I301 0.159(5) 0.043(2) 0.329(7) -0.003(3) -0.153(6) 0.011(3) I302 0.156(5) 0.155(6) 0.362(13) -0.091(7) -0.075(6) 0.020(4) I501 0.127(9) 0.048(4) 0.32(2) 0.009(8) -0.153(13) -0.020(5) Zn51 0.058(3) 0.055(3) 0.132(5) -0.033(3) -0.027(2) 0.030(3) I502 0.090(5) 0.156(12) 0.149(8) -0.077(8) -0.019(5) 0.006(5) C330 0.21(3) 0.20(3) 0.23(3) -0.08(2) -0.01(2) -0.13(3) I406 0.139(4) 0.052(2) 0.305(10) 0.013(3) -0.081(5) 0.0032(19) Zn43 0.126(7) 0.042(4) 0.220(12) 0.005(5) -0.090(7) 0.010(4) I405 0.224(9) 0.112(5) 0.382(13) -0.006(5) -0.142(9) 0.072(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 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 1 0.0647 1 0 -1 0.0380 0 0 1 0.0579 0 0 -1 0.0484 0 1 0 0.1072 -1 0 -1 0.0422 1 0 1 0.0728 -1 -2 1 0.1452 2 1 -2 0.0913 -2 -1 2 0.1103 2 0 1 0.0760 2 -1 -2 0.1016 -2 0 -1 0.0544 -1 -1 2 0.1144 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 I306 Zn33 I305 128.9(2) . . ? N306 Zn33 I305 101.4(4) . . ? N306 Zn33 I306 110.1(4) . . ? N306 Zn33 N307 97.4(5) . . ? N307 Zn33 I305 105.3(4) . . ? N307 Zn33 I306 109.2(4) . . ? I402 Zn41 I401 126.5(6) . . ? N301 Zn41 I401 106.3(6) . . ? N301 Zn41 I402 107.4(6) . . ? N301 Zn41 N00I 98.0(6) . 8_556 ? N00I Zn41 I401 111.5(6) 8_556 . ? N00I Zn41 I402 103.5(7) 8_556 . ? I403 Zn42 I404 121.9(2) . . ? N305 Zn42 I403 107.3(5) . . ? N305 Zn42 I404 110.1(6) . . ? N311 Zn42 I403 99.5(7) 6_556 . ? N311 Zn42 I404 115.2(8) 6_556 . ? N311 Zn42 N305 100.3(7) 6_556 . ? C308 N302 C306 119.8(10) . . ? C314 N306 Zn33 121.2(8) . . ? C314 N306 C318 117.0(9) . . ? C314 N306 Zn53 115.8(12) . . ? C314 N306 Zn43 124.7(8) . . ? C318 N306 Zn33 121.3(7) . . ? C318 N306 Zn53 122.6(11) . . ? C318 N306 Zn43 116.7(7) . . ? C306 N303 C307 115.9(10) . . ? C326 N310 C325 116.4(12) . . ? C325 N309 C324 112.3(13) . . ? C307 N304 C308 118.7(9) . . ? C319 N307 Zn33 126.4(12) . . ? C319 N307 C323 118.0(12) . . ? C319 N307 Zn53 157.3(15) . . ? C319 N307 Zn43 119.6(12) . . ? C323 N307 Zn33 114.9(9) . . ? C323 N307 Zn53 83.8(13) . . ? C323 N307 Zn43 121.4(10) . . ? C305 N301 Zn41 123.3(10) . . ? C305 N301 C301 116.0(11) . . ? C305 N301 Zn31 131.7(10) . . ? C305 N301 Zn51 128.3(11) . . ? C301 N301 Zn41 119.4(9) . . ? C301 N301 Zn31 111.8(9) . . ? C301 N301 Zn51 106.6(11) . . ? Zn41 N00I Zn51 17.1(4) 8_455 8_455 ? C329 N00I Zn41 123.9(16) . 8_455 ? C329 N00I Zn31 121.8(17) . 8_455 ? C329 N00I Zn51 107.6(15) . 8_455 ? C329 N00I C330 119.6(14) . . ? Zn31 N00I Zn51 14.3(7) 8_455 8_455 ? C330 N00I Zn41 116.4(12) . 8_455 ? C330 N00I Zn31 118.5(13) . 8_455 ? C330 N00I Zn51 132.7(11) . 8_455 ? N310 C325 N309 125.2(12) . . ? N310 C325 C327 121.1(11) . . ? N309 C325 C327 113.4(14) . . ? C324 N308 C326 113.1(12) . . ? N307 C319 H319 119.1 . . ? N307 C319 C320 121.8(15) . . ? C320 C319 H319 119.1 . . ? C320 C321 C324 124.5(13) . . ? C320 C321 C322 120.9(13) . . ? C322 C321 C324 113.4(17) . . ? N303 C307 C309 117.3(11) . . ? N304 C307 N303 123.9(10) . . ? N304 C307 C309 118.8(11) . . ? C312 N305 Zn42 113.9(13) . . ? C312 N305 C311 119.9(15) . . ? C312 N305 Zn32 134.0(14) . . ? C312 N305 Zn52 137(2) . . ? C311 N305 Zn42 126.2(14) . . ? C311 N305 Zn32 106.1(14) . . ? C311 N305 Zn52 103(2) . . ? C319 C320 H320 120.0 . . ? C321 C320 C319 120.1(13) . . ? C321 C320 H320 120.0 . . ? N302 C308 N304 119.1(10) . . ? N302 C308 C316 121.1(10) . . ? N304 C308 C316 119.3(10) . . ? C315 C316 C308 122.0(10) . . ? C317 C316 C308 121.7(14) . . ? C317 C316 C315 116.1(13) . . ? N310 C326 N308 125.4(15) . . ? N310 C326 C334 119.1(13) . . ? N308 C326 C334 115.5(12) . . ? C328 C327 C325 123.6(12) . . ? C328 C327 C331 117.4(17) . . ? C331 C327 C325 119(2) . . ? C316 C315 H315 120.4 . . ? C314 C315 C316 119.1(10) . . ? C314 C315 H315 120.4 . . ? N301 C305 H305 114.4 . . ? N301 C305 C304 131.2(14) . . ? C304 C305 H305 114.4 . . ? N302 C306 N303 121.6(10) . . ? N302 C306 C303 118.4(11) . . ? N303 C306 C303 120.0(11) . . ? C304 C303 C306 120.1(11) . . ? C302 C303 C306 123.2(11) . . ? C302 C303 C304 116.7(11) . . ? N306 C314 C315 123.8(11) . . ? N306 C314 H314 118.1 . . ? C315 C314 H314 118.1 . . ? C310 C309 C307 124.8(13) . . ? C310 C309 C313 115.7(14) . . ? C313 C309 C307 119.5(12) . . ? C327 C328 H328 119.5 . . ? C327 C328 C329 120.9(15) . . ? C329 C328 H328 119.5 . . ? N00I C329 C328 118.6(19) . . ? N00I C329 H329 120.7 . . ? C328 C329 H329 120.7 . . ? C305 C304 C303 114.9(12) . . ? C305 C304 H304 122.6 . . ? C303 C304 H304 122.6 . . ? C303 C302 H302 119.4 . . ? C303 C302 C301 121.1(13) . . ? C301 C302 H302 119.4 . . ? N301 C301 C302 119.3(13) . . ? N301 C301 H301 120.4 . . ? C302 C301 H301 120.4 . . ? N309 C324 C321 114.1(16) . . ? N308 C324 N309 127.5(13) . . ? N308 C324 C321 118.2(14) . . ? N306 C318 H318 120.4 . . ? C317 C318 N306 119.2(10) . . ? C317 C318 H318 120.4 . . ? C332 N311 Zn42 132.4(17) . 6 ? C332 N311 C336 111(2) . . ? C332 N311 Zn32 119.4(18) . 6 ? C332 N311 Zn52 118(3) . 6 ? C336 N311 Zn42 113.7(18) . 6 ? C336 N311 Zn32 129.5(16) . 6 ? C336 N311 Zn52 131(3) . 6 ? N305 C312 H312 115.0 . . ? N305 C312 C313 130(2) . . ? C313 C312 H312 115.0 . . ? C316 C317 H317 117.6 . . ? C318 C317 C316 124.7(15) . . ? C318 C317 H317 117.6 . . ? C335 C334 C326 121.8(16) . . ? C333 C334 C326 126.5(17) . . ? C333 C334 C335 112(2) . . ? N307 C323 H323 117.5 . . ? N307 C323 C322 125.0(16) . . ? C322 C323 H323 117.5 . . ? N305 C311 H311 121.8 . . ? N305 C311 C310 116.5(18) . . ? C310 C311 H311 121.8 . . ? C309 C310 C311 122.9(17) . . ? C309 C310 H310 118.5 . . ? C311 C310 H310 118.5 . . ? C334 C335 H335 119.2 . . ? C334 C335 C336 121.6(17) . . ? C336 C335 H335 119.2 . . ? C309 C313 H313 122.7 . . ? C312 C313 C309 114.6(19) . . ? C312 C313 H313 122.7 . . ? C321 C322 H322 123.7 . . ? C323 C322 C321 113(2) . . ? C323 C322 H322 123.7 . . ? C334 C333 H333 118.0 . . ? C332 C333 C334 124(2) . . ? C332 C333 H333 118.0 . . ? N311 C332 H332 117.1 . . ? C333 C332 N311 126(2) . . ? C333 C332 H332 117.1 . . ? N311 C336 C335 122.5(17) . . ? N311 C336 H336 118.8 . . ? C335 C336 H336 118.8 . . ? C327 C331 H331 119.7 . . ? C330 C331 C327 121(3) . . ? C330 C331 H331 119.7 . . ? N305 Zn32 I303 117.2(7) . . ? N305 Zn32 I304 99.1(7) . . ? N311 Zn32 N305 102.0(8) 6_556 . ? N311 Zn32 I303 116.0(9) 6_556 . ? N311 Zn32 I304 98.8(9) 6_556 . ? I303 Zn32 I304 120.3(5) . . ? N305 Zn52 I503 112(3) . . ? N305 Zn52 I504 109(3) . . ? N311 Zn52 N305 101(3) 6_556 . ? N311 Zn52 I503 105(3) 6_556 . ? N311 Zn52 I504 75(3) 6_556 . ? I504 Zn52 I503 138(4) . . ? N301 Zn31 I301 104.6(6) . . ? N301 Zn31 I302 103.5(7) . . ? N00I Zn31 N301 108.9(7) 8_556 . ? N00I Zn31 I301 106.4(7) 8_556 . ? N00I Zn31 I302 111.2(8) 8_556 . ? I302 Zn31 I301 121.4(5) . . ? N301 Zn51 N00I 84.9(7) . 8_556 ? N301 Zn51 I501 94.6(8) . . ? N301 Zn51 I502 118.6(8) . . ? I502 Zn51 I501 139.3(11) . . ? N00I C330 H330 118.8 . . ? C331 C330 N00I 122(2) . . ? C331 C330 H330 118.8 . . ? N306 Zn53 I505 75.9(10) . . ? N307 Zn53 N306 91.9(13) . . ? N307 Zn53 I505 79.3(11) . . ? N307 Zn53 I506 142.3(16) . . ? I506 Zn53 N306 121.2(13) . . ? I506 Zn53 I505 123.2(14) . . ? N306 Zn43 N307 98.3(6) . . ? N306 Zn43 I406 104.8(6) . . ? N306 Zn43 I405 111.7(7) . . ? N307 Zn43 I406 106.7(7) . . ? N307 Zn43 I405 109.3(6) . . ? I406 Zn43 I405 123.1(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 I305 Zn33 2.572(6) . ? I306 Zn33 2.511(6) . ? I401 Zn41 2.581(10) . ? I402 Zn41 2.495(9) . ? I403 Zn42 2.517(6) . ? Zn33 N306 2.082(9) . ? Zn33 N307 2.098(11) . ? I404 Zn42 2.526(6) . ? Zn41 N301 2.084(12) . ? Zn41 N00I 2.146(15) 8_556 ? Zn42 N305 2.167(13) . ? Zn42 N311 2.052(19) 6_556 ? N302 C308 1.322(14) . ? N302 C306 1.331(15) . ? N306 C314 1.314(13) . ? N306 C318 1.41(2) . ? N306 Zn53 2.38(3) . ? N306 Zn43 2.070(12) . ? N303 C307 1.382(16) . ? N303 C306 1.332(17) . ? N310 C325 1.323(19) . ? N310 C326 1.295(18) . ? N309 C325 1.334(16) . ? N309 C324 1.37(2) . ? N304 C307 1.236(17) . ? N304 C308 1.388(15) . ? N307 C319 1.31(2) . ? N307 C323 1.36(2) . ? N307 Zn53 1.98(3) . ? N307 Zn43 2.083(15) . ? N301 C305 1.210(18) . ? N301 C301 1.385(19) . ? N301 Zn31 2.060(13) . ? N301 Zn51 2.220(19) . ? N00I C329 1.31(2) . ? N00I Zn31 1.860(15) 8_455 ? N00I Zn51 2.50(2) 8_455 ? N00I C330 1.35(4) . ? C325 C327 1.511(19) . ? N308 C326 1.364(17) . ? N308 C324 1.29(2) . ? C319 H319 0.9500 . ? C319 C320 1.41(2) . ? C321 C320 1.32(2) . ? C321 C324 1.49(2) . ? C321 C322 1.44(2) . ? C307 C309 1.463(15) . ? N305 C312 1.27(3) . ? N305 C311 1.29(3) . ? N305 Zn32 2.159(16) . ? N305 Zn52 2.14(8) . ? C320 H320 0.9500 . ? C308 C316 1.434(16) . ? C316 C315 1.384(18) . ? C316 C317 1.355(17) . ? C326 C334 1.43(2) . ? C327 C328 1.33(2) . ? C327 C331 1.38(2) . ? C315 H315 0.9500 . ? C315 C314 1.375(16) . ? C305 H305 0.9500 . ? C305 C304 1.360(17) . ? C306 C303 1.444(18) . ? C303 C304 1.426(18) . ? C303 C302 1.364(19) . ? C314 H314 0.9500 . ? C309 C310 1.387(18) . ? C309 C313 1.41(2) . ? C328 H328 0.9500 . ? C328 C329 1.45(2) . ? C329 H329 0.9500 . ? C304 H304 0.9500 . ? C302 H302 0.9500 . ? C302 C301 1.404(15) . ? C301 H301 0.9500 . ? C318 H318 0.9500 . ? C318 C317 1.32(2) . ? N311 C332 1.31(3) . ? N311 C336 1.35(3) . ? N311 Zn32 2.01(2) 6 ? N311 Zn52 2.06(7) 6 ? C312 H312 0.9500 . ? C312 C313 1.30(3) . ? C317 H317 0.9500 . ? C334 C335 1.37(3) . ? C334 C333 1.33(3) . ? C323 H323 0.9500 . ? C323 C322 1.40(3) . ? C311 H311 0.9500 . ? C311 C310 1.40(2) . ? C310 H310 0.9500 . ? C335 H335 0.9500 . ? C335 C336 1.37(4) . ? C313 H313 0.9500 . ? C322 H322 0.9500 . ? C333 H333 0.9500 . ? C333 C332 1.28(3) . ? C332 H332 0.9500 . ? C336 H336 0.9500 . ? C331 H331 0.9500 . ? C331 C330 1.34(4) . ? I303 Zn32 2.485(13) . ? Zn32 I304 2.550(15) . ? I503 Zn52 2.85(7) . ? I504 Zn52 2.21(8) . ? Zn31 I301 2.596(11) . ? Zn31 I302 2.518(13) . ? I501 Zn51 2.432(17) . ? Zn51 I502 2.427(17) . ? C330 H330 0.9500 . ? I505 Zn53 2.97(4) . ? I506 Zn53 2.37(4) . ? I406 Zn43 2.516(12) . ? Zn43 I405 2.547(13) . ? 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 Zn33 N306 C314 C315 172.3(15) . . . . ? Zn33 N306 C318 C317 -171(2) . . . . ? Zn33 N307 C319 C320 -167.7(9) . . . . ? Zn33 N307 C323 C322 163(2) . . . . ? Zn41 N301 C305 C304 -178(2) . . . . ? Zn41 N301 C301 C302 176.4(16) . . . . ? Zn41 N00I C329 C328 -175.9(11) 8_455 . . . ? Zn41 N00I C330 C331 178(3) 8_455 . . . ? Zn42 N305 C312 C313 174(3) . . . . ? Zn42 N305 C311 C310 -179.2(18) . . . . ? Zn42 N311 C332 C333 177(3) 6 . . . ? Zn42 N311 C336 C335 -166(2) 6 . . . ? N302 C308 C316 C315 9(2) . . . . ? N302 C308 C316 C317 -176(2) . . . . ? N302 C306 C303 C304 -3(2) . . . . ? N302 C306 C303 C302 177.5(17) . . . . ? N306 C318 C317 C316 -1(4) . . . . ? N303 C307 C309 C310 -7(3) . . . . ? N303 C307 C309 C313 175.3(18) . . . . ? N303 C306 C303 C304 178.8(17) . . . . ? N303 C306 C303 C302 -1(3) . . . . ? N310 C325 C327 C328 165.2(12) . . . . ? N310 C325 C327 C331 -19(3) . . . . ? N310 C326 C334 C335 14(2) . . . . ? N310 C326 C334 C333 -163.8(19) . . . . ? N309 C325 C327 C328 -20.6(17) . . . . ? N309 C325 C327 C331 156(2) . . . . ? N304 C307 C309 C310 175(2) . . . . ? N304 C307 C309 C313 -2(3) . . . . ? N304 C308 C316 C315 -178.8(15) . . . . ? N304 C308 C316 C317 -3(3) . . . . ? N307 C319 C320 C321 -2.8(18) . . . . ? N307 C323 C322 C321 14(4) . . . . ? N301 C305 C304 C303 7(4) . . . . ? C325 N310 C326 N308 -3.6(18) . . . . ? C325 N310 C326 C334 177.7(11) . . . . ? C325 N309 C324 N308 -0.7(17) . . . . ? C325 N309 C324 C321 174.6(10) . . . . ? C325 C327 C328 C329 -176.8(12) . . . . ? C325 C327 C331 C330 179(3) . . . . ? N308 C326 C334 C335 -164.9(15) . . . . ? N308 C326 C334 C333 17(2) . . . . ? C319 N307 C323 C322 -8(3) . . . . ? C307 N303 C306 N302 0(2) . . . . ? C307 N303 C306 C303 178.3(15) . . . . ? C307 N304 C308 N302 -12(2) . . . . ? C307 N304 C308 C316 175.6(15) . . . . ? C307 C309 C310 C311 -176(2) . . . . ? C307 C309 C313 C312 172(2) . . . . ? N305 C312 C313 C309 8(5) . . . . ? N305 C311 C310 C309 0(4) . . . . ? C320 C321 C324 N309 1.8(17) . . . . ? C320 C321 C324 N308 177.5(11) . . . . ? C320 C321 C322 C323 -14(3) . . . . ? C308 N302 C306 N303 0(2) . . . . ? C308 N302 C306 C303 -177.8(14) . . . . ? C308 N304 C307 N303 13(3) . . . . ? C308 N304 C307 C309 -169.8(14) . . . . ? C308 C316 C315 C314 177.4(16) . . . . ? C308 C316 C317 C318 -176(2) . . . . ? C316 C315 C314 N306 -1(3) . . . . ? C326 N310 C325 N309 2.7(17) . . . . ? C326 N310 C325 C327 176.1(11) . . . . ? C326 N308 C324 N309 0.0(17) . . . . ? C326 N308 C324 C321 -175.1(10) . . . . ? C326 C334 C335 C336 -172.7(19) . . . . ? C326 C334 C333 C332 -173(3) . . . . ? C327 C328 C329 N00I -8(2) . . . . ? C327 C331 C330 N00I 4(6) . . . . ? C315 C316 C317 C318 -1(4) . . . . ? C305 N301 C301 C302 9(3) . . . . ? C306 N302 C308 N304 5(2) . . . . ? C306 N302 C308 C316 177.8(14) . . . . ? C306 N303 C307 N304 -7(3) . . . . ? C306 N303 C307 C309 175.2(14) . . . . ? C306 C303 C304 C305 179.8(18) . . . . ? C306 C303 C302 C301 179.5(18) . . . . ? C303 C302 C301 N301 -4(3) . . . . ? C314 N306 C318 C317 1(3) . . . . ? C328 C327 C331 C330 -5(5) . . . . ? C329 N00I C330 C331 -5(5) . . . . ? C304 C303 C302 C301 0(3) . . . . ? C302 C303 C304 C305 -1(3) . . . . ? C301 N301 C305 C304 -11(4) . . . . ? C324 N309 C325 N310 -0.7(16) . . . . ? C324 N309 C325 C327 -174.6(10) . . . . ? C324 N308 C326 N310 2.3(17) . . . . ? C324 N308 C326 C334 -178.9(11) . . . . ? C324 C321 C320 C319 175.4(11) . . . . ? C324 C321 C322 C323 178.5(19) . . . . ? C318 N306 C314 C315 0(3) . . . . ? C312 N305 C311 C310 1(4) . . . . ? C317 C316 C315 C314 2(3) . . . . ? C334 C335 C336 N311 -9(4) . . . . ? C334 C333 C332 N311 -23(5) . . . . ? C323 N307 C319 C320 2(2) . . . . ? C311 N305 C312 C313 -6(5) . . . . ? C310 C309 C313 C312 -5(3) . . . . ? C335 C334 C333 C332 9(4) . . . . ? C313 C309 C310 C311 2(3) . . . . ? C322 C321 C320 C319 9(2) . . . . ? C322 C321 C324 N309 169.1(16) . . . . ? C322 C321 C324 N308 -15(2) . . . . ? C333 C334 C335 C336 5(3) . . . . ? C332 N311 C336 C335 -2(4) . . . . ? C336 N311 C332 C333 17(5) . . . . ? C331 C327 C328 C329 7(3) . . . . ? Zn32 N305 C312 C313 173(3) . . . . ? Zn32 N305 C311 C310 -178(2) . . . . ? Zn32 N311 C332 C333 -162(3) 6 . . . ? Zn32 N311 C336 C335 177.3(19) 6 . . . ? Zn52 N305 C312 C313 174(3) . . . . ? Zn52 N305 C311 C310 -178(3) . . . . ? Zn52 N311 C332 C333 -159(4) 6 . . . ? Zn52 N311 C336 C335 174(3) 6 . . . ? Zn31 N301 C305 C304 178(2) . . . . ? Zn31 N301 C301 C302 -178.3(17) . . . . ? Zn31 N00I C329 C328 -171.5(11) 8_455 . . . ? Zn31 N00I C330 C331 173(3) 8_455 . . . ? Zn51 N301 C305 C304 -153(2) . . . . ? Zn51 N301 C301 C302 158.9(17) . . . . ? Zn51 N00I C329 C328 -170.2(12) 8_455 . . . ? Zn51 N00I C330 C331 171(3) 8_455 . . . ? C330 N00I C329 C328 6(3) . . . . ? Zn53 N306 C314 C315 -156.8(18) . . . . ? Zn53 N306 C318 C317 156(2) . . . . ? Zn53 N307 C319 C320 -161(3) . . . . ? Zn53 N307 C323 C322 165(3) . . . . ? Zn43 N306 C314 C315 165.3(15) . . . . ? Zn43 N306 C318 C317 -166(2) . . . . ? Zn43 N307 C319 C320 -167.2(9) . . . . ? Zn43 N307 C323 C322 161(2) . . . . ? 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 -1.0006 0.0002 0.9996 0.0615 -0.0087 -0.0024 1.0006 -0.0002 -0.9996 -0.0615 0.0087 0.0024 -0.0002 0.0001 0.9996 0.0334 -0.0093 -0.0384 0.0002 -0.0001 -0.9996 -0.0334 0.0093 0.0384 -0.0003 0.9999 -0.0001 0.0136 0.1007 -0.0124 -1.0002 0.0000 -0.9996 -0.0053 0.0099 0.0745 1.0002 -0.0000 0.9996 0.0053 -0.0099 -0.0745 -0.9999 -1.9995 0.9998 0.0342 -0.2101 0.0224 2.0008 0.9995 -1.9994 -0.1093 0.1180 -0.0076 -2.0008 -0.9995 1.9994 0.1093 -0.1180 0.0076 2.0006 -0.0001 0.9995 -0.0229 -0.0106 -0.1105 2.0015 -1.0003 -1.9991 -0.1366 -0.0834 0.0171 -2.0006 0.0001 -0.9995 0.0229 0.0106 0.1105 -1.0004 -0.9996 1.9993 0.0812 -0.1187 -0.0284 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 -0.102 -0.917 -0.852 3466.9 838.6 ? 2 -0.235 -0.948 0.515 3466.9 838.6 ?