#------------------------------------------------------------------------------ #$Date: 2026-06-28 02:04:10 +0100 (Sun, 28 Jun 2026) $ #$Revision: 306672 $ #$URL: svn://www.crystallography.net/cod/cif/7/06/44/7064457.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7064457 loop_ _publ_author_name 'Vos, Cyler W.' 'Croke, Rylan' 'Lin, Jian-Bin' 'Kozak, Christopher M.' _publ_section_title ; Ring-Opening Polymerization of Lactide and Ring-Opening Copolymerization of Cyclohexene Oxide and Phthalic Anhydride by Multinuclear Complexes of Zinc, Magnesium and Potassium ; _journal_name_full 'New Journal of Chemistry' _journal_paper_doi 10.1039/D6NJ01550F _journal_year 2026 _chemical_formula_moiety 'C56 H78 K4 N4 O20 Zn3, C3 H6 O, 1[C3H6O]' _chemical_formula_sum 'C59 H84 K4 N4 O21 Zn3' _chemical_formula_weight 1537.81 _space_group_crystal_system orthorhombic _space_group_IT_number 60 _space_group_name_Hall '-P 2n 2ab' _space_group_name_H-M_alt 'P b c n' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2026-06-09 _audit_creation_method ; Olex2 1.5-ac6-016 (compiled 2024.01.13 svn.r2f8d729c for Rigaku Oxford Diffraction, GUI svn.r6897) ; _audit_update_record ; 2026-06-09 deposited with the CCDC. 2026-06-26 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 21.3110(6) _cell_length_b 24.2504(9) _cell_length_c 14.0934(5) _cell_measurement_reflns_used 6257 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 76.1020 _cell_measurement_theta_min 2.7430 _cell_volume 7283.5(4) _computing_cell_refinement 'CrysAlisPro 1.171.43.141a (Rigaku OD, 2024)' _computing_data_collection 'CrysAlisPro system (CCD 43.141a (release 04-10-2024))' _computing_data_reduction 'CrysAlisPro 1.171.43.141a (Rigaku OD, 2024)' _computing_molecular_graphics 'Olex2 1.5-ac6-016 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5-ac6-016 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100(2) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.985 _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 -10.00 28.00 0.50 20.00 -- -46.93 7.00 36.00 76 2 \w -89.00 -23.00 0.50 80.00 -- -91.75 130.00-124.00 132 3 \w -164.00-136.00 0.50 80.00 -- -91.75 -7.00-138.00 56 4 \w 42.00 80.00 0.50 80.00 -- 113.25-130.00 163.00 76 5 \w 44.00 105.00 0.50 80.00 -- 113.25-123.00 69.00 122 6 \w -81.00 -55.00 0.50 20.00 -- -46.93 125.00 -90.00 52 7 \w -117.00 -32.00 0.50 20.00 -- -46.93 -57.00 60.00 170 8 \w 36.00 74.00 0.50 20.00 -- 46.93 -99.00-120.00 76 9 \w 48.00 73.00 0.50 80.00 -- 113.25 -61.00 30.00 50 10 \w 61.00 105.00 0.50 80.00 -- 113.25 -97.00 133.96 88 11 \w 43.00 105.00 0.50 80.00 -- 113.25 -94.00 150.00 124 12 \w 153.00 178.00 0.50 80.00 -- 113.25 15.00-180.00 50 13 \w 135.00 176.00 0.50 80.00 -- 113.25 15.00 -90.00 82 14 \w 45.00 73.00 0.50 80.00 -- 113.25 -94.00 60.00 56 15 \w 96.00 132.00 0.50 80.00 -- 113.25 15.00 -90.00 72 16 \w 96.00 139.00 0.50 80.00 -- 113.25 15.00-180.00 86 17 \w 53.00 78.00 0.50 200.00 -- 113.25 -61.00 -60.00 50 18 \w 90.00 115.00 0.50 200.00 -- 113.25-130.00 163.00 50 19 \w -119.00 -23.00 0.50 40.00 -- -46.93 -77.00 -90.00 192 20 \w -119.00 -94.00 0.50 40.00 -- -46.93 -60.00 149.36 50 21 \w -16.00 29.00 0.50 40.00 -- -46.93 19.00-150.00 90 22 \w -143.00-118.00 0.50 200.00 -- -91.75-123.00 69.00 50 23 \w -121.00 -60.00 0.50 40.00 -- -46.93 -37.00 -30.00 122 24 \w -119.00 -23.00 0.50 40.00 -- -46.93 -77.00 150.00 192 25 \w -88.00 -63.00 0.50 200.00 -- -91.75 148.00 -46.00 50 26 \w 54.00 79.00 0.50 40.00 -- 46.93-148.00 -94.00 50 27 \w -72.00 -47.00 0.50 40.00 -- -46.93 123.00 149.00 50 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0037193000 _diffrn_orient_matrix_UB_12 0.0598403000 _diffrn_orient_matrix_UB_13 0.0361884000 _diffrn_orient_matrix_UB_21 -0.0046848000 _diffrn_orient_matrix_UB_22 0.0212708000 _diffrn_orient_matrix_UB_23 -0.1028010000 _diffrn_orient_matrix_UB_31 -0.0720224000 _diffrn_orient_matrix_UB_32 0.0018013000 _diffrn_orient_matrix_UB_33 0.0086711000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.1442 _diffrn_reflns_av_unetI/netI 0.0924 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.985 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 52187 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.985 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 79.331 _diffrn_reflns_theta_min 2.760 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 3.784 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.63468 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.43.141a (Rigaku Oxford Diffraction, 2024) 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 1.402 _exptl_crystal_description prism _exptl_crystal_F_000 3200 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.908 _refine_diff_density_min -0.834 _refine_diff_density_rms 0.107 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 451 _refine_ls_number_reflns 7787 _refine_ls_number_restraints 46 _refine_ls_restrained_S_all 1.036 _refine_ls_R_factor_all 0.1160 _refine_ls_R_factor_gt 0.0705 _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^)+(0.0620P)^2^+19.3508P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1579 _refine_ls_wR_factor_ref 0.1813 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4908 _reflns_number_total 7787 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6nj01550f2.cif _cod_data_source_block cv-314 _cod_database_code 7064457 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula C31H45K2N2O11Zn1.5 _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 0.928 _shelx_estimated_absorpt_t_min 0.659 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups, All C(H,H,H,H,H,H) groups 2. Restrained distances O11-C29 1.21 with sigma of 0.02 C29-C31 = C29-C30 1.5 with sigma of 0.02 O11-C31 = O11-C30 2.38 with sigma of 0.04 C31-O11 \\sim C30-O11 with sigma of 0.04 O4-C17 \\sim O4-C17A with sigma of 0.02 K2-C17 \\sim K2-C17A with sigma of 0.02 C29-C31 \\sim C29-C30 with sigma of 0.02 3. Restrained planarity O11, C29, C30, C31 with sigma of 0.05 4. Uiso/Uaniso restraints and constraints O11 \\sim C29 \\sim C30 \\sim C31: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A Uanis(C17A) = Uanis(C17) 5. Rigid body (RIGU) restrains O11, C29, C30, C31 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 6. Others Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=1-FVAR(1) Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(1) Fixed Sof: H30A(0.5) H30B(0.5) H30C(0.5) O11(0.5) C29(0.5) C30(0.5) C31(0.5) H31A(0.5) H31B(0.5) H31C(0.5) 7.a Riding coordinates: C17(H17A,H17B,H17C), C17A(H17D,H17E,H17F) 7.b Secondary CH2 refined with riding coordinates: C7(H7A,H7B), C16(H16A,H16B), C19(H19A,H19B), C20(H20A,H20B) 7.c Aromatic/amide H refined with riding coordinates: C3(H3), C5(H5), C12(H12), C14(H14) 7.d Idealised Me refined as rotating group: C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C18(H18A,H18B,H18C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C28(H28A,H28B, H28C), C31(H31A,H31B,H31C) ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL cv-314_a.res in Pbcn cv-314.res created by SHELXL-2018/3 at 10:34:42 on 09-Jun-2026 REM Old TITL CV-314 in Pbcn REM SHELXT solution in Pbcn: R1 0.158, Rweak 0.012, Alpha 0.038 REM 0.519 for 713 systematic absences, Orientation as input REM Formula found by SHELXT: C60 N4 O20 K4 Zn3 CELL 1.54184 21.311 24.2504 14.0934 90 90 90 ZERR 4 0.0006 0.0009 0.0005 0 0 0 LATT 1 SYMM 0.5-X,0.5-Y,0.5+Z SYMM -X,+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H K N O Zn UNIT 236 336 16 16 84 12 DFIX 1.21 O11 C29 DANG 2.38 O11 C31 O11 C30 SADI 0.04 C31 O11 C30 O11 SADI O4 C17 O4 C17A FLAT 0.05 O11 C29 C30 C31 SIMU O11 > C31 SADI K2 C17 K2 C17A DFIX 1.5 C29 C31 C29 C30 RIGU O11 > C31 EADP C17A C17 SADI C29 C31 C29 C30 L.S. 8 PLAN 1 SIZE 0.02 0.04 0.12 TEMP -173(2) CONF BOND list 4 MORE -1 BOND $H ABIN fmap 2 acta REM REM REM WGHT 0.062000 19.350798 FVAR 0.20353 0.48695 ZN1 6 0.252212 0.437346 0.414764 11.00000 0.03459 0.03153 = 0.02346 -0.00049 0.00130 -0.00535 ZN2 6 0.500000 0.397345 0.250000 10.50000 0.03563 0.02920 = 0.02468 0.00000 -0.00181 0.00000 K1 3 0.350696 0.343703 0.282266 11.00000 0.03697 0.03498 = 0.02955 -0.00153 -0.00051 -0.00336 K2 3 0.423537 0.463932 0.441322 11.00000 0.03392 0.03506 = 0.02426 -0.00182 0.00079 -0.00618 O1 5 0.251814 0.407973 0.285037 11.00000 0.03803 0.04294 = 0.02136 -0.00061 0.00012 -0.00258 O2 5 0.254810 0.328108 0.159464 11.00000 0.04668 0.03550 = 0.02620 -0.00366 -0.00114 -0.00307 O3 5 0.303272 0.502784 0.434967 11.00000 0.04473 0.02759 = 0.02831 0.00249 -0.00105 -0.00258 O4 5 0.398780 0.564878 0.380820 11.00000 0.04287 0.03650 = 0.04951 0.00930 -0.00638 -0.01116 O5 5 0.328809 0.392516 0.467535 11.00000 0.03829 0.03524 = 0.03118 0.00040 -0.00080 -0.00961 O6 5 0.325916 0.300657 0.458519 11.00000 0.06678 0.03634 = 0.04945 0.00022 0.00172 -0.01865 O7 5 0.437615 0.308786 0.163787 11.00000 0.04984 0.06375 = 0.05876 -0.01899 0.00638 0.00055 O8 5 0.524612 0.356019 0.132447 11.00000 0.05510 0.03605 = 0.03315 -0.00449 -0.00062 0.00049 O9 5 0.545802 0.483850 0.385618 11.00000 0.03678 0.04141 = 0.02555 -0.00909 0.00145 -0.00353 O10 5 0.578530 0.438267 0.258351 11.00000 0.03541 0.03333 = 0.02216 -0.00198 -0.00067 0.00133 N1 4 0.166664 0.486542 0.384945 11.00000 0.03715 0.03878 = 0.03029 0.00261 0.00247 -0.00265 N2 4 0.187861 0.396705 0.511523 11.00000 0.03905 0.04087 = 0.02622 0.00241 0.00541 -0.00782 C1 1 0.202862 0.403245 0.227710 11.00000 0.03322 0.04077 = 0.02335 -0.00006 0.00419 -0.00710 C2 1 0.201188 0.359988 0.160586 11.00000 0.04048 0.03498 = 0.02676 0.00318 0.00495 -0.00525 C3 1 0.150974 0.352234 0.100852 11.00000 0.04376 0.04981 = 0.02099 -0.00050 0.00056 -0.01305 AFIX 43 H3 2 0.151551 0.322761 0.056454 11.00000 -1.20000 AFIX 0 C4 1 0.099135 0.387342 0.104939 11.00000 0.03529 0.05511 = 0.03342 -0.00358 0.00273 -0.01073 C5 1 0.101483 0.431299 0.165909 11.00000 0.03508 0.05325 = 0.03468 0.00520 0.00244 -0.00322 AFIX 43 H5 2 0.067220 0.456350 0.167143 11.00000 -1.20000 AFIX 0 C6 1 0.152335 0.440688 0.226324 11.00000 0.03693 0.03910 = 0.02631 -0.00111 0.00499 -0.00706 C7 1 0.157161 0.493370 0.281444 11.00000 0.04107 0.04611 = 0.02811 0.00721 0.00067 0.00100 AFIX 23 H7A 2 0.192531 0.515178 0.255639 11.00000 -1.20000 H7B 2 0.118309 0.514939 0.271175 11.00000 -1.20000 AFIX 0 C8 1 0.264929 0.294030 0.077882 11.00000 0.06300 0.05416 = 0.02892 -0.00955 -0.00489 0.00769 AFIX 137 H8A 2 0.262017 0.316557 0.020320 11.00000 -1.50000 H8B 2 0.233005 0.264966 0.075898 11.00000 -1.50000 H8C 2 0.306691 0.277249 0.081606 11.00000 -1.50000 AFIX 0 C9 1 0.043441 0.377867 0.039499 11.00000 0.04648 0.07398 = 0.05312 -0.00425 -0.00400 -0.01171 AFIX 137 H9A 2 0.021403 0.344182 0.058610 11.00000 -1.50000 H9B 2 0.058301 0.373976 -0.025965 11.00000 -1.50000 H9C 2 0.014725 0.409338 0.043677 11.00000 -1.50000 AFIX 0 C10 1 0.289997 0.553579 0.402404 11.00000 0.04724 0.02663 = 0.01914 -0.00372 0.00080 -0.00379 C11 1 0.340278 0.587758 0.372858 11.00000 0.05036 0.02762 = 0.02993 0.00339 -0.00448 -0.00702 C12 1 0.328989 0.640335 0.338883 11.00000 0.05710 0.03682 = 0.02646 0.00254 -0.00235 -0.01201 AFIX 43 H12 2 0.363458 0.662866 0.320883 11.00000 -1.20000 AFIX 0 C13 1 0.268492 0.660959 0.330465 11.00000 0.06088 0.03272 = 0.02067 -0.00192 -0.00086 -0.00447 C14 1 0.219503 0.627080 0.359150 11.00000 0.05916 0.03955 = 0.02087 -0.00978 0.00642 0.00684 AFIX 43 H14 2 0.177757 0.640534 0.354346 11.00000 -1.20000 AFIX 0 C15 1 0.229160 0.574041 0.394764 11.00000 0.05257 0.03101 = 0.02462 -0.00644 0.00419 -0.00027 C16 1 0.174656 0.541414 0.430623 11.00000 0.04514 0.03419 = 0.03472 -0.00269 0.00476 0.00498 AFIX 23 H16A 2 0.179729 0.535960 0.499815 11.00000 -1.20000 H16B 2 0.135884 0.563144 0.420665 11.00000 -1.20000 AFIX 0 PART 1 C17 1 0.449196 0.593456 0.332822 21.00000 0.05292 0.04597 = 0.12199 0.02158 -0.01532 -0.02279 AFIX 3 H17A 2 0.484726 0.597066 0.376502 21.00000 -1.50000 H17B 2 0.462316 0.572636 0.276602 21.00000 -1.50000 H17C 2 0.434886 0.630196 0.313502 21.00000 -1.50000 AFIX 0 PART 2 C17A 1 0.450300 0.602946 0.375674 -21.00000 0.05292 0.04597 = 0.12199 0.02158 -0.01532 -0.02279 AFIX 3 H17D 2 0.469510 0.607556 0.438334 -21.00000 -1.50000 H17E 2 0.481460 0.588136 0.331324 -21.00000 -1.50000 H17F 2 0.435370 0.638756 0.352635 -21.00000 -1.50000 AFIX 0 PART 0 C18 1 0.257308 0.718571 0.295307 11.00000 0.07647 0.02905 = 0.04311 0.00064 -0.00321 0.00587 AFIX 137 H18A 2 0.250704 0.743225 0.349492 11.00000 -1.50000 H18B 2 0.220064 0.719059 0.254527 11.00000 -1.50000 H18C 2 0.293854 0.731034 0.258955 11.00000 -1.50000 AFIX 0 C19 1 0.113225 0.457034 0.428044 11.00000 0.03094 0.05555 = 0.04083 0.00307 0.00967 -0.00484 AFIX 23 H19A 2 0.099027 0.427319 0.384927 11.00000 -1.20000 H19B 2 0.077845 0.482906 0.437552 11.00000 -1.20000 AFIX 0 C20 1 0.132425 0.432534 0.522337 11.00000 0.03855 0.05331 = 0.03327 0.00224 0.01089 0.00012 AFIX 23 H20A 2 0.142131 0.462590 0.567553 11.00000 -1.20000 H20B 2 0.097166 0.410789 0.548638 11.00000 -1.20000 AFIX 0 C21 1 0.213480 0.384410 0.606376 11.00000 0.04923 0.06373 = 0.02347 0.00182 0.00647 -0.00915 AFIX 137 H21A 2 0.247258 0.357191 0.600635 11.00000 -1.50000 H21B 2 0.180121 0.369556 0.646842 11.00000 -1.50000 H21C 2 0.230089 0.418310 0.634695 11.00000 -1.50000 AFIX 0 C22 1 0.170615 0.343138 0.465918 11.00000 0.04478 0.04633 = 0.03848 0.00303 0.00356 -0.01304 AFIX 137 H22A 2 0.149703 0.350285 0.405222 11.00000 -1.50000 H22B 2 0.142191 0.322677 0.507731 11.00000 -1.50000 H22C 2 0.208649 0.321342 0.454911 11.00000 -1.50000 AFIX 0 C23 1 0.341192 0.343633 0.498433 11.00000 0.03957 0.03614 = 0.03367 0.00171 -0.00030 -0.00905 C24 1 0.378334 0.341484 0.589838 11.00000 0.05277 0.04874 = 0.03596 0.00963 0.00185 -0.00161 AFIX 137 H24A 2 0.418576 0.360351 0.580981 11.00000 -1.50000 H24B 2 0.385900 0.302944 0.607347 11.00000 -1.50000 H24C 2 0.354585 0.359766 0.640396 11.00000 -1.50000 AFIX 0 C25 1 0.485142 0.315886 0.117304 11.00000 0.05349 0.04209 = 0.04003 -0.00664 0.00140 -0.00300 C26 1 0.502469 0.275515 0.040075 11.00000 0.09372 0.06672 = 0.06389 -0.02654 0.02382 -0.02708 AFIX 137 H26A 2 0.488462 0.289825 -0.021410 11.00000 -1.50000 H26B 2 0.482095 0.240004 0.052431 11.00000 -1.50000 H26C 2 0.548096 0.270511 0.039074 11.00000 -1.50000 AFIX 0 C27 1 0.586815 0.472590 0.328011 11.00000 0.03157 0.03184 = 0.01817 -0.00117 0.00195 -0.00156 C28 1 0.651196 0.498044 0.333594 11.00000 0.03806 0.04619 = 0.02285 -0.00161 0.00295 -0.00772 AFIX 137 H28A 2 0.670981 0.487813 0.393846 11.00000 -1.50000 H28B 2 0.647579 0.538270 0.329785 11.00000 -1.50000 H28C 2 0.676909 0.484608 0.280783 11.00000 -1.50000 AFIX 0 PART -1 H30A 2 -0.086615 0.274440 0.145395 10.50000 -1.50000 H30B 2 -0.025996 0.295230 0.126547 10.50000 -1.50000 H30C 2 -0.064362 0.317031 0.266521 10.50000 -1.50000 O11 5 -0.009430 0.209496 0.269698 10.50000 0.10483 0.03828 = 0.14001 0.02323 -0.02933 -0.01859 C29 1 -0.000953 0.257758 0.253229 10.50000 0.06247 0.03940 = 0.03610 0.00383 0.00737 -0.00817 C30 1 -0.049945 0.291420 0.203255 10.50000 0.04490 0.05512 = 0.06732 0.00967 0.02843 0.00373 C31 1 0.059606 0.283982 0.283488 10.50000 0.06565 0.05001 = 0.04005 -0.01178 0.01466 -0.01071 AFIX 137 H31A 2 0.084268 0.257429 0.320326 10.50000 -1.50000 H31B 2 0.050672 0.316433 0.322666 10.50000 -1.50000 H31C 2 0.083427 0.295210 0.227234 10.50000 -1.50000 AFIX 0 HKLF 4 REM cv-314_a.res in Pbcn REM wR2 = 0.1813, GooF = S = 1.039, Restrained GooF = 1.036 for all data REM R1 = 0.0705 for 4908 Fo > 4sig(Fo) and 0.1160 for all 7787 data REM 451 parameters refined using 46 restraints END WGHT 0.0620 19.3366 REM Highest difference peak 0.908, deepest hole -0.834, 1-sigma level 0.107 Q1 1 0.2768 0.4377 0.4639 11.00000 0.05 0.91 ; _shelx_res_checksum 10896 _shelx_fab_file ; 0 0 2 -92.3662 0.1722 0 0 4 47.8919 -1.1131 0 0 6 -19.7598 1.1558 0 0 8 9.1570 -0.0091 0 0 10 -5.1975 -0.0657 0 0 12 2.1900 0.0658 0 0 14 -0.3683 -0.5510 0 0 16 3.7836 0.2683 0 2 0 -35.7764 -0.1114 0 2 1 -86.9963 -0.8430 0 2 2 26.1410 -0.3585 0 2 3 57.1569 -0.1687 0 2 4 -11.0945 0.3748 0 2 5 -27.1367 0.2365 0 2 6 5.5586 0.1345 0 2 7 12.2031 -0.1775 0 2 8 -4.5383 0.1289 0 2 9 -6.2225 0.0195 0 2 10 2.0428 0.1126 0 2 11 3.4259 0.0548 0 2 12 -2.4793 -0.1958 0 2 13 -0.1758 0.0156 0 2 14 5.3776 0.0527 0 2 15 0.6425 0.1561 0 2 16 -2.2600 -0.2254 0 2 17 -2.2647 0.0014 0 4 0 -38.1026 -0.6666 0 4 1 38.3410 0.0382 0 4 2 33.3498 0.2612 0 4 3 -22.9269 -0.0703 0 4 4 -22.5127 -0.2178 0 4 5 10.9991 -0.2852 0 4 6 12.2739 0.3324 0 4 7 -8.1017 -0.0569 0 4 8 -6.2350 0.1460 0 4 9 5.9988 0.0680 0 4 10 3.6121 0.0077 0 4 11 -2.9398 0.1391 0 4 12 -1.1250 0.0408 0 4 13 6.1897 0.0470 0 4 14 -0.3092 -0.2011 0 4 15 -6.1396 0.0018 0 4 16 0.5767 0.0204 0 4 17 0.6956 -0.1965 0 6 0 21.0209 -0.0418 0 6 1 -3.6320 -0.1745 0 6 2 -18.2670 -0.3614 0 6 3 -1.9970 -0.1110 0 6 4 12.2219 0.0459 0 6 5 4.1559 0.1433 0 6 6 -8.5073 0.1375 0 6 7 -2.0638 -0.0477 0 6 8 8.3551 0.3048 0 6 9 2.1204 -0.0718 0 6 10 -5.5170 0.1383 0 6 11 -1.1621 0.0062 0 6 12 4.1999 -0.1715 0 6 13 1.2758 -0.0432 0 6 14 -4.9282 -0.0944 0 6 15 -0.6687 0.0831 0 6 16 1.9597 -0.2719 0 6 17 -1.4973 0.0185 0 8 0 -14.8251 -0.3380 0 8 1 -1.6722 -0.0804 0 8 2 11.9275 0.0341 0 8 3 4.1696 0.1053 0 8 4 -6.7353 -0.0020 0 8 5 -4.1980 -0.0575 0 8 6 5.1081 0.0905 0 8 7 6.7380 0.1064 0 8 8 -2.7346 0.0943 0 8 9 -6.9369 -0.0788 0 8 10 0.2329 0.0430 0 8 11 4.9101 -0.1339 0 8 12 0.5546 0.0274 0 8 13 -3.0064 -0.0087 0 8 14 -1.5384 -0.0750 0 8 15 0.5238 -0.0222 0 8 16 -0.5928 0.0027 0 8 17 -0.9552 0.2638 0 10 0 6.7578 -0.0090 0 10 1 7.2377 -0.0321 0 10 2 -4.4405 -0.1565 0 10 3 -7.7769 0.0066 0 10 4 3.1680 -0.0565 0 10 5 7.3484 0.0346 0 10 6 0.5993 0.0718 0 10 7 -5.4070 0.0401 0 10 8 -4.4913 0.0691 0 10 9 2.8891 -0.0332 0 10 10 3.9728 0.0356 0 10 11 -0.2904 -0.0091 0 10 12 -4.3131 0.0166 0 10 13 0.7612 -0.0568 0 10 14 2.0061 0.0030 0 10 15 -2.9586 0.0020 0 10 16 -1.5850 -0.0095 0 12 0 4.5635 -0.1045 0 12 1 -5.8229 -0.1166 0 12 2 -3.7586 -0.0379 0 12 3 5.8048 -0.0234 0 12 4 3.1964 0.0182 0 12 5 -4.9689 0.0364 0 12 6 -1.9264 0.0276 0 12 7 1.6090 0.0750 0 12 8 2.0987 0.0507 0 12 9 0.0094 0.0162 0 12 10 -0.9968 0.0070 0 12 11 -2.2224 -0.0264 0 12 12 0.2773 -0.0267 0 12 13 4.7842 -0.0381 0 12 14 -5.9363 -0.0610 0 12 15 -4.8662 -0.0902 0 12 16 3.6066 0.1580 0 14 0 -4.2759 -0.1119 0 14 1 -6.6419 -0.0566 0 14 2 4.7415 -0.0667 0 14 3 0.8144 -0.0085 0 14 4 -3.7210 0.0503 0 14 5 1.5260 -0.0184 0 14 6 4.2232 0.0499 0 14 7 -0.2533 0.0531 0 14 8 -4.4896 0.0409 0 14 9 -0.1412 -0.0282 0 14 10 0.8510 -0.0161 0 14 11 -1.0058 -0.0162 0 14 12 1.9616 -0.0446 0 14 13 -4.0039 -0.0116 0 14 14 -5.2909 -0.0380 0 14 15 4.9468 0.1753 0 14 16 2.7752 0.2316 0 16 0 -6.8261 -0.0764 0 16 1 5.3028 0.0033 0 16 2 3.1269 -0.0679 0 16 3 -2.5143 -0.0342 0 16 4 1.1489 0.0466 0 16 5 0.0108 -0.0038 0 16 6 1.1141 0.0422 0 16 7 -3.8244 0.0071 0 16 8 -0.9070 0.0158 0 16 9 1.8440 0.0208 0 16 10 -2.9380 0.0224 0 16 11 0.6754 -0.0104 0 16 12 -1.5654 0.0377 0 16 13 -0.3037 0.0322 0 16 14 3.2741 0.0175 0 16 15 0.5668 0.0787 0 18 0 6.9968 -0.0735 0 18 1 3.1966 -0.0344 0 18 2 -4.0576 -0.0720 0 18 3 -1.7940 0.0227 0 18 4 -1.1883 0.0289 0 18 5 2.4849 -0.0241 0 18 6 0.5382 0.0615 0 18 7 -3.6131 0.0016 0 18 8 0.4490 0.0708 0 18 9 -3.0287 0.0358 0 18 10 2.0268 0.0024 0 18 11 2.1009 0.0448 0 18 12 0.1136 0.0155 0 18 13 2.2566 -0.1327 0 18 14 -3.6877 -0.0990 0 20 0 4.1671 -0.0624 0 20 1 -3.9748 0.0469 0 20 2 -3.7882 -0.0417 0 20 3 -0.4325 -0.0204 0 20 4 2.9622 0.0161 0 20 5 0.3184 0.0355 0 20 6 -2.6509 0.0283 0 20 7 -0.2124 -0.0198 0 20 8 -1.7848 0.0793 0 20 9 2.4393 0.0097 0 20 10 4.1231 0.0085 0 20 11 -2.5825 0.0039 0 20 12 -0.6512 -0.1585 0 20 13 -2.2766 -0.1215 0 22 0 -1.3966 -0.0091 0 22 1 -5.3047 -0.0069 0 22 2 -0.7926 -0.0737 0 22 3 2.5400 0.0040 0 22 4 0.3383 0.0068 0 22 5 -1.4549 -0.0045 0 22 6 1.5653 0.0162 0 22 7 -2.1783 0.0122 0 22 8 0.9498 0.0600 0 22 9 3.8323 -0.0223 0 22 10 -3.4883 0.0268 0 22 11 -2.0880 -0.0430 0 22 12 1.3000 -0.0920 0 24 0 -3.5033 -0.0930 0 24 1 -0.0899 -0.0044 0 24 2 1.9950 -0.0177 0 24 3 0.5667 -0.0243 0 24 4 -1.8290 -0.0065 0 24 5 -0.0361 0.0264 0 24 6 0.0122 0.0095 0 24 7 0.0062 0.0063 0 24 8 3.0819 0.0678 0 24 9 -2.2549 0.0553 0 24 10 -1.5977 0.0229 0 24 11 2.4729 -0.0839 0 26 0 -0.5517 -0.0256 0 26 1 -0.0878 0.0493 0 26 2 -0.0746 -0.0669 0 26 3 -3.4791 -0.0238 0 26 4 -0.6566 -0.0070 0 26 5 3.7149 0.0109 0 26 6 1.7941 0.0747 0 26 7 -0.0375 0.0752 0 26 8 -1.4521 0.0683 0 26 9 -0.9465 -0.0466 0 28 0 -2.6728 -0.1099 0 28 1 2.6612 -0.0788 0 28 2 -2.5539 0.0101 0 28 3 -0.6327 0.0106 0 28 4 6.5465 -0.0054 0 28 5 0.0247 0.1241 0 28 6 -2.5672 0.0706 0 28 7 -1.1749 -0.0584 0 30 0 4.2873 -0.1703 0 30 1 1.1051 0.2188 0 30 2 -2.7093 0.0329 0 30 3 4.3524 -0.0740 0 30 4 -1.3279 0.0754 1 0 2 2.2527 -1.3240 1 0 4 -0.1880 0.6067 1 0 6 -1.0280 -1.7786 1 0 8 -0.6980 1.8915 1 0 10 1.9319 -0.9216 1 0 12 -0.7912 1.0326 1 0 14 0.4270 -0.2452 1 0 16 -0.9918 -0.3103 1 1 0 -60.2451 -0.6129 1 1 1 81.1581 0.9671 1 1 2 49.1035 0.0916 1 1 3 -50.8895 0.1627 1 1 4 -26.9756 0.4982 1 1 5 22.8631 -0.2067 1 1 6 11.0417 -0.6584 1 1 7 -10.6447 0.3892 1 1 8 -4.2758 -0.1886 1 1 9 5.4284 -0.6135 1 1 10 2.5628 0.1636 1 1 11 -2.9496 0.5142 1 1 12 -0.5480 -0.1172 1 1 13 1.9624 -0.6408 1 1 14 -1.7467 0.4390 1 1 15 -2.6153 0.5345 1 1 16 -1.4747 -0.1394 1 1 17 2.2665 -0.3381 1 2 1 0.6564 0.0362 1 2 2 -0.9294 0.4544 1 2 3 -0.3143 0.1688 1 2 4 -0.0637 -1.2126 1 2 5 -0.8322 -0.0674 1 2 6 0.4932 1.2718 1 2 7 0.2707 0.4594 1 2 8 0.6758 -1.2623 1 2 9 1.0094 -0.0285 1 2 10 -1.3300 1.1598 1 2 11 -1.1881 0.1863 1 2 12 1.3693 -0.6035 1 2 13 0.6982 -0.1970 1 2 14 -0.7770 0.3302 1 2 15 -0.7705 -0.1307 1 2 16 0.6661 0.0084 1 2 17 0.3819 -0.1029 1 3 0 71.9564 1.0537 1 3 1 17.5433 0.4304 1 3 2 -57.3158 -0.3749 1 3 3 -15.2312 0.2530 1 3 4 31.1788 0.0753 1 3 5 8.8039 0.1305 1 3 6 -15.7926 -0.2533 1 3 7 -2.3311 0.0096 1 3 8 9.3207 -0.1595 1 3 9 0.3532 0.1742 1 3 10 -4.8115 0.1773 1 3 11 -0.4882 -0.4097 1 3 12 3.2868 -0.2134 1 3 13 -3.7269 0.1658 1 3 14 -4.3830 0.3097 1 3 15 3.8045 -0.2932 1 3 16 2.2296 -0.2339 1 3 17 0.4744 0.2654 1 4 1 -0.5490 0.1477 1 4 2 1.8679 -0.1726 1 4 3 0.3140 -0.0887 1 4 4 -1.3996 0.1100 1 4 5 0.3475 0.2252 1 4 6 0.2818 -0.4933 1 4 7 0.6807 -0.1947 1 4 8 -0.1839 0.5752 1 4 9 -1.4969 0.2901 1 4 10 0.1047 -0.3240 1 4 11 1.9916 -0.0219 1 4 12 0.9230 0.2075 1 4 13 -2.0712 0.1066 1 4 14 -0.9397 -0.0953 1 4 15 1.1814 -0.1078 1 4 16 -0.0563 -0.0976 1 4 17 -0.8764 -0.1227 1 5 0 -10.8230 0.2978 1 5 1 -29.5762 -0.1054 1 5 2 6.5842 0.2304 1 5 3 22.6834 0.1666 1 5 4 -0.7584 0.0841 1 5 5 -14.4420 -0.0602 1 5 6 0.8126 -0.2485 1 5 7 9.4368 0.1879 1 5 8 -2.7296 -0.2438 1 5 9 -6.9581 -0.0937 1 5 10 1.3555 -0.2199 1 5 11 3.7250 -0.0679 1 5 12 -2.1322 0.1650 1 5 13 -4.6291 -0.0348 1 5 14 3.9525 0.1192 1 5 15 3.7437 0.0023 1 5 16 -2.1039 0.2509 1 5 17 0.2595 0.1696 1 6 1 1.7775 0.0986 1 6 2 -0.5489 0.0251 1 6 3 -2.5220 -0.1490 1 6 4 0.3320 -0.3397 1 6 5 0.6542 0.0975 1 6 6 1.1658 0.2725 1 6 7 -0.2093 0.2972 1 6 8 -1.3329 -0.2835 1 6 9 1.1862 0.0239 1 6 10 1.0336 0.3603 1 6 11 -0.4929 0.0074 1 6 12 -2.1312 -0.1240 1 6 13 -0.7445 -0.0547 1 6 14 2.2200 0.0104 1 6 15 -0.2778 -0.1216 1 6 16 -0.9286 -0.0487 1 6 17 0.8804 0.0944 1 7 0 1.8012 0.2944 1 7 1 13.9753 0.1824 1 7 2 1.1449 -0.0257 1 7 3 -9.4512 0.0681 1 7 4 -4.2215 0.0152 1 7 5 5.3912 -0.0503 1 7 6 3.7295 -0.1103 1 7 7 -6.0387 -0.1069 1 7 8 -4.9986 -0.2115 1 7 9 4.5604 0.1306 1 7 10 4.5716 -0.0469 1 7 11 -2.8100 0.0130 1 7 12 -3.5400 0.0528 1 7 13 1.5386 0.1490 1 7 14 3.7017 0.1517 1 7 15 -0.3000 -0.1106 1 7 16 -0.6747 0.0494 1 7 17 1.2129 -0.1113 1 8 1 -0.9221 -0.0656 1 8 2 -1.1696 -0.0708 1 8 3 1.3446 -0.0376 1 8 4 0.9171 0.3334 1 8 5 0.7613 0.2222 1 8 6 -0.5750 -0.2503 1 8 7 -1.4964 -0.1278 1 8 8 0.9909 0.2414 1 8 9 0.1051 0.2931 1 8 10 -1.2458 -0.3414 1 8 11 -0.4833 -0.0398 1 8 12 0.5756 0.1393 1 8 13 1.9388 -0.0157 1 8 14 -0.4099 -0.1485 1 8 15 -1.5659 -0.0401 1 8 16 0.8443 0.2026 1 8 17 -0.0811 -0.0226 1 9 0 4.8514 0.2437 1 9 1 -9.1519 -0.0899 1 9 2 -6.0605 0.2589 1 9 3 5.7663 -0.0185 1 9 4 5.4435 -0.1017 1 9 5 -3.8812 -0.0058 1 9 6 -6.2052 -0.0508 1 9 7 0.0389 -0.0262 1 9 8 6.6773 -0.0826 1 9 9 2.5200 0.0340 1 9 10 -4.1903 -0.1106 1 9 11 -3.1436 0.0956 1 9 12 2.9105 0.0991 1 9 13 2.4164 -0.0029 1 9 14 -0.9427 -0.0762 1 9 15 0.1692 -0.0141 1 9 16 1.3721 0.0763 1 9 17 0.4394 -0.1288 1 10 1 0.3938 0.0567 1 10 2 1.0795 0.1130 1 10 3 -0.2470 0.0135 1 10 4 -0.2902 -0.0058 1 10 5 -0.8237 -0.1741 1 10 6 -0.7916 0.0032 1 10 7 1.2076 0.1042 1 10 8 -0.0439 0.0007 1 10 9 -0.6201 -0.1112 1 10 10 0.5859 0.0228 1 10 11 0.7090 0.1187 1 10 12 0.4246 -0.0899 1 10 13 -0.8304 0.0004 1 10 14 -1.2055 0.0059 1 10 15 0.0404 0.1297 1 10 16 0.2878 -0.0671 1 11 0 -7.6712 0.0530 1 11 1 0.5793 0.0844 1 11 2 6.8440 -0.0014 1 11 3 0.7118 -0.0854 1 11 4 -6.7728 0.0972 1 11 5 -1.1448 0.0003 1 11 6 3.4870 -0.0866 1 11 7 3.0012 -0.0939 1 11 8 -0.4269 -0.0337 1 11 9 -3.2632 0.0083 1 11 10 -0.7208 -0.0035 1 11 11 2.5129 0.0615 1 11 12 2.6183 -0.0282 1 11 13 -4.5401 0.0156 1 11 14 0.7427 0.0261 1 11 15 5.7997 0.0502 1 11 16 -0.4049 -0.0429 1 12 1 -0.2844 -0.1010 1 12 2 -0.6202 -0.0765 1 12 3 0.6005 -0.0673 1 12 4 -0.1528 0.0345 1 12 5 -0.2459 0.0040 1 12 6 1.1520 -0.0584 1 12 7 -0.2780 -0.0497 1 12 8 -0.5325 0.0963 1 12 9 0.3356 0.0685 1 12 10 -0.3138 -0.0423 1 12 11 0.0848 -0.0119 1 12 12 -0.3707 0.1070 1 12 13 -0.4666 0.0027 1 12 14 -0.3583 -0.1069 1 12 15 0.1036 0.0043 1 12 16 1.1621 -0.0012 1 13 0 -1.5342 -0.0495 1 13 1 7.3041 0.0272 1 13 2 -0.4261 0.1448 1 13 3 -4.8834 0.0625 1 13 4 2.2645 -0.0837 1 13 5 2.9384 -0.0201 1 13 6 -2.6904 0.0104 1 13 7 -2.0877 -0.0295 1 13 8 1.3144 -0.0800 1 13 9 1.6486 -0.0080 1 13 10 0.0518 0.0181 1 13 11 1.1664 -0.0113 1 13 12 -2.5086 0.0442 1 13 13 -0.2285 0.0146 1 13 14 8.5634 0.0394 1 13 15 -0.6637 0.0106 1 13 16 -4.7874 -0.1345 1 14 1 0.0822 -0.1119 1 14 2 1.8896 0.0171 1 14 3 -0.0011 0.0595 1 14 4 -1.5105 0.0277 1 14 5 0.1789 -0.1067 1 14 6 -0.1490 0.0083 1 14 7 -0.3689 0.0871 1 14 8 0.1142 0.0063 1 14 9 -0.2467 -0.0336 1 14 10 0.7305 -0.0267 1 14 11 0.1996 0.0396 1 14 12 -0.8632 0.0269 1 14 13 -0.2209 -0.0264 1 14 14 0.0499 0.0909 1 14 15 1.2313 0.0753 1 14 16 0.3572 -0.1652 1 15 0 8.6709 0.1555 1 15 1 2.1080 0.1200 1 15 2 -5.7065 0.0275 1 15 3 1.4487 -0.0108 1 15 4 0.4776 0.0062 1 15 5 -1.7612 0.0341 1 15 6 -1.8191 -0.0988 1 15 7 2.6552 -0.0708 1 15 8 3.3146 -0.0208 1 15 9 -2.1643 0.0275 1 15 10 0.9783 -0.0170 1 15 11 0.4414 0.0233 1 15 12 0.4137 0.0541 1 15 13 4.1534 -0.0065 1 15 14 -1.2083 -0.0250 1 15 15 -4.2093 -0.1434 1 16 1 0.9825 -0.0006 1 16 2 -0.2060 0.0792 1 16 3 -2.0605 -0.0292 1 16 4 -0.3977 -0.0905 1 16 5 0.9125 0.0035 1 16 6 0.3603 0.0997 1 16 7 0.2500 -0.0843 1 16 8 0.0800 -0.0375 1 16 9 0.4759 0.0440 1 16 10 -0.6117 0.0553 1 16 11 -1.0341 0.1080 1 16 12 0.5546 0.0699 1 16 13 0.2770 0.0150 1 16 14 0.1609 -0.1415 1 16 15 0.3372 -0.2449 1 17 0 -0.4248 0.0912 1 17 1 -6.9660 -0.0426 1 17 2 0.6234 0.1072 1 17 3 2.0058 -0.0025 1 17 4 0.9966 -0.0962 1 17 5 0.0179 -0.0068 1 17 6 -2.0596 -0.0045 1 17 7 3.7770 0.0204 1 17 8 -0.5113 -0.0562 1 17 9 1.2193 -0.0064 1 17 10 1.6373 -0.0153 1 17 11 -2.0194 -0.0109 1 17 12 1.0831 -0.0338 1 17 13 -3.0167 -0.0777 1 17 14 -0.0021 0.0218 1 18 1 0.0121 -0.0054 1 18 2 -0.4995 -0.0358 1 18 3 -0.4137 0.0280 1 18 4 0.9794 0.0501 1 18 5 0.6970 0.0494 1 18 6 -0.2447 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-0.3249 22 2 0 2.4173 0.0177 22 2 1 0.3874 0.2133 22 2 2 -1.5971 -0.4588 22 2 3 -1.4376 -0.0269 22 2 4 0.6175 0.3446 22 2 5 2.2224 -0.0279 22 2 6 -0.0638 -0.3113 22 2 7 -1.8563 -0.1669 22 2 8 0.4377 0.2657 22 2 9 1.3970 0.2046 22 2 10 -0.4034 0.2158 22 3 1 -0.3181 -0.0604 22 3 2 -1.8795 -0.0191 22 3 3 -0.3018 0.3518 22 3 4 1.7015 0.1742 22 3 5 0.0941 -0.2526 22 3 6 -2.9744 -0.1963 22 3 7 0.5831 0.2082 22 3 8 1.5666 0.0831 22 3 9 1.4887 -0.4575 22 3 10 -0.3001 -0.0701 22 4 0 -0.6897 0.0174 22 4 1 -1.8349 -0.0265 22 4 2 0.1440 0.1792 22 4 3 0.0276 0.0105 22 4 4 0.1224 -0.2366 22 4 5 0.4902 -0.0483 22 4 6 0.5709 0.1253 22 4 7 0.2739 0.0741 22 4 8 0.4333 0.0769 22 4 9 -0.2809 -0.0563 22 4 10 -0.9283 -0.1554 22 5 1 -1.1366 -0.0020 22 5 2 -0.4428 0.0515 22 5 3 1.1873 -0.1494 22 5 4 -0.1858 -0.2373 22 5 5 -1.0276 -0.0056 22 5 6 1.1753 0.0506 22 5 7 1.4592 0.0586 22 5 8 -1.0657 -0.1340 22 5 9 0.1202 0.0075 22 5 10 -0.9548 0.1371 22 6 0 -0.2768 0.0124 22 6 1 0.8950 0.0379 22 6 2 -0.6576 -0.2024 22 6 3 -0.9310 -0.0532 22 6 4 1.7422 0.1122 22 6 5 2.2997 0.0200 22 6 6 -0.3461 0.0234 22 6 7 -1.7977 0.0032 22 6 8 -0.3751 -0.0709 22 6 9 -0.5645 -0.1200 22 7 1 -0.3240 -0.0446 22 7 2 -0.0579 -0.1114 22 7 3 -0.1925 0.0409 22 7 4 -0.1087 0.1602 22 7 5 0.7599 0.0196 22 7 6 -0.8100 0.0093 22 7 7 -0.4948 0.0250 22 7 8 0.8440 -0.1741 22 7 9 0.0531 -0.0044 22 8 0 0.0162 -0.0746 22 8 1 -1.3121 -0.0632 22 8 2 -0.2263 0.0830 22 8 3 1.0298 0.1241 22 8 4 1.6818 -0.0679 22 8 5 -1.1261 0.0048 22 8 6 -2.5284 0.0128 22 8 7 -0.2576 -0.0826 22 8 8 0.4792 0.0536 22 8 9 -0.0797 0.1826 22 9 1 -0.8513 0.0153 22 9 2 -0.1304 0.0854 22 9 3 -0.2688 0.0488 22 9 4 0.4866 -0.1751 22 9 5 0.0033 -0.0956 22 9 6 -0.2086 0.0380 22 9 7 2.7692 -0.0550 22 9 8 -1.0362 -0.0133 22 9 9 -1.9027 0.2727 22 10 0 -2.4371 -0.0068 22 10 1 0.8453 0.0931 22 10 2 0.3191 -0.0664 22 10 3 -0.2570 0.0326 22 10 4 0.1396 0.0101 22 10 5 -1.2487 -0.0462 22 10 6 0.8616 -0.0266 22 10 7 0.5464 0.1168 22 10 8 0.1574 0.0608 22 11 1 0.1726 -0.0092 22 11 2 0.0087 -0.0794 22 11 3 -0.3512 -0.1788 22 11 4 1.7119 -0.0610 22 11 5 -0.7621 0.2482 22 11 6 0.6871 0.0932 22 11 7 0.3348 0.0088 22 11 8 -3.3691 -0.0203 22 12 0 0.3404 0.0273 22 12 1 1.1248 -0.0129 22 12 2 -1.0422 0.0140 22 12 3 1.2022 0.1077 22 12 4 0.2714 -0.0714 22 12 5 0.3939 0.0081 22 12 6 -0.0828 0.0118 22 12 7 -1.2322 -0.0284 22 13 1 -0.2421 -0.0937 22 13 2 -1.3026 -0.0283 22 13 3 0.6534 -0.0268 22 13 4 -0.2408 0.2065 22 13 5 -0.6911 0.0589 22 13 6 2.0373 -0.1245 22 13 7 -1.4308 -0.0672 22 14 0 -0.1603 0.0838 22 14 1 -0.4662 0.0216 22 14 2 0.5175 -0.0541 22 14 3 0.8868 0.0326 22 14 4 -0.7450 -0.0257 22 14 5 -0.4405 -0.0337 22 14 6 -0.9658 -0.0929 22 15 1 -1.1762 0.0014 22 15 2 0.3701 -0.0458 22 15 3 0.4258 -0.0329 22 15 4 0.7069 0.0074 22 15 5 1.7277 0.0600 22 16 0 -1.5858 0.0761 22 16 1 0.8505 -0.1125 22 16 2 0.9643 0.0581 22 16 3 -0.1086 0.1240 22 16 4 -0.9182 -0.0865 22 17 1 0.6261 -0.1660 22 17 2 0.3797 -0.0435 22 17 3 -0.3701 0.0306 22 18 0 0.3139 0.0963 22 18 1 1.8374 0.0556 23 0 2 -1.0950 -0.0381 23 0 4 2.0792 0.3361 23 0 6 -1.5645 -0.2182 23 0 8 1.7648 0.2096 23 1 0 -0.3684 0.0549 23 1 1 -1.6570 -0.2010 23 1 2 -0.1081 0.0497 23 1 3 0.9657 0.2385 23 1 4 0.8774 -0.0241 23 1 5 -1.5683 -0.2497 23 1 6 -1.7038 0.0751 23 1 7 2.4101 0.4599 23 1 8 1.2317 -0.0390 23 1 9 -1.5581 -0.1990 23 2 1 -0.9388 -0.0064 23 2 2 1.6713 0.1934 23 2 3 1.9830 -0.0517 23 2 4 -0.4348 -0.4623 23 2 5 -1.7389 -0.0335 23 2 6 1.3997 0.3775 23 2 7 1.1822 -0.0882 23 2 8 -0.7868 -0.5725 23 2 9 -1.0744 0.1684 23 3 0 -1.8174 0.0715 23 3 1 1.6739 0.0267 23 3 2 0.7854 -0.0108 23 3 3 0.1708 -0.0079 23 3 4 -0.0277 0.1272 23 3 5 -0.5695 0.1492 23 3 6 0.9749 0.0391 23 3 7 -0.0084 -0.0532 23 3 8 -1.9259 -0.1874 23 3 9 -0.4143 -0.0953 23 4 1 1.3013 0.0343 23 4 2 1.9446 -0.0666 23 4 3 -1.1915 -0.1506 23 4 4 -1.2525 0.1994 23 4 5 0.9567 0.1969 23 4 6 0.7849 -0.0357 23 4 7 -1.9001 -0.1184 23 4 8 0.1653 0.2070 23 4 9 0.2595 0.2801 23 5 0 1.5746 0.0789 23 5 1 -0.3494 -0.0593 23 5 2 -0.3109 0.0984 23 5 3 1.3798 0.1431 23 5 4 -0.6555 -0.0238 23 5 5 -1.4814 -0.1280 23 5 6 -0.9299 -0.0929 23 5 7 -0.1531 -0.0364 23 5 8 0.5789 -0.0578 23 5 9 0.9212 0.2109 23 6 1 0.5249 0.0492 23 6 2 -0.4624 0.0966 23 6 3 -0.3653 0.1253 23 6 4 0.7682 -0.0368 23 6 5 -0.2033 -0.0753 23 6 6 -0.5061 0.0283 23 6 7 0.5455 -0.0961 23 6 8 0.4848 0.0551 23 7 0 -1.2706 0.0340 23 7 1 0.4708 0.0527 23 7 2 1.1972 0.0065 23 7 3 -0.6071 -0.1281 23 7 4 -1.9292 -0.0331 23 7 5 -0.4131 -0.0045 23 7 6 1.6685 0.0068 23 7 7 1.3224 0.0885 23 7 8 0.1588 0.1369 23 8 1 0.4630 0.0182 23 8 2 0.6717 -0.0553 23 8 3 0.4774 -0.1424 23 8 4 -0.2867 0.0006 23 8 5 -0.4107 0.0960 23 8 6 1.1189 -0.0697 23 8 7 -1.2973 0.0533 23 8 8 -0.8690 0.2223 23 9 0 2.2180 0.0702 23 9 1 0.6060 -0.0800 23 9 2 -0.9966 0.0422 23 9 3 0.1667 0.0067 23 9 4 -0.3212 -0.0391 23 9 5 1.4058 0.0548 23 9 6 0.6714 0.1137 23 9 7 -0.7564 -0.0434 23 9 8 -0.2261 -0.1871 23 10 1 0.3211 -0.0846 23 10 2 0.0861 0.0133 23 10 3 0.6861 0.1132 23 10 4 -1.1249 0.1902 23 10 5 0.0027 -0.0710 23 10 6 -0.2180 -0.0312 23 10 7 -1.6568 0.0142 23 11 0 0.9102 -0.0023 23 11 1 -1.6829 0.0120 23 11 2 0.9442 0.0519 23 11 3 -0.2132 -0.1890 23 11 4 -0.4923 0.0489 23 11 5 0.4586 0.0635 23 11 6 -1.1390 -0.1010 23 11 7 0.4190 -0.0905 23 12 1 0.2489 0.1004 23 12 2 1.5760 0.0765 23 12 3 -0.6295 0.1281 23 12 4 -1.3423 -0.1073 23 12 5 1.2552 -0.2185 23 12 6 -1.0683 -0.0184 23 13 0 -0.2326 -0.0841 23 13 1 -0.3094 -0.0522 23 13 2 0.1189 -0.0481 23 13 3 -0.9644 -0.0309 23 13 4 0.5674 0.0682 23 13 5 -0.4642 -0.0200 23 14 1 1.3234 0.0362 23 14 2 -0.2011 0.0370 23 14 3 -1.0933 -0.0189 23 14 4 0.5885 -0.1345 23 14 5 -0.6847 0.0134 23 15 0 0.3917 -0.0837 23 15 1 -0.5510 0.0540 23 15 2 -0.1341 0.0825 23 15 3 0.0282 -0.0604 23 16 1 0.0519 0.0713 23 16 2 -0.5578 0.0392 24 0 0 -1.5745 0.2614 24 0 2 0.6843 -0.0868 24 0 4 -0.0675 -0.1507 24 0 6 1.9636 0.2584 24 0 8 -2.3120 -0.1519 24 1 1 1.2711 -0.1539 24 1 2 0.5694 0.0180 24 1 3 -1.6664 -0.1093 24 1 4 -1.1830 0.0856 24 1 5 0.4280 0.1324 24 1 6 -0.1145 -0.1944 24 1 7 -0.2910 -0.1615 24 1 8 0.0645 0.4116 24 2 0 2.7047 -0.0154 24 2 1 0.5470 -0.0607 24 2 2 -0.8613 0.1806 24 2 3 0.1281 -0.0544 24 2 4 -0.6939 -0.1920 24 2 5 0.5277 -0.0410 24 2 6 -0.5897 -0.1362 24 2 7 -1.8653 -0.1152 24 2 8 1.4064 0.1661 24 3 1 0.0054 0.1529 24 3 2 -2.8573 -0.0377 24 3 3 -0.8743 0.0799 24 3 4 1.0408 0.0398 24 3 5 0.8237 -0.1021 24 3 6 -0.7862 0.0244 24 3 7 0.5346 0.1648 24 3 8 0.3654 -0.0087 24 4 0 -0.9043 -0.2104 24 4 1 -1.5594 0.0258 24 4 2 0.7299 -0.1124 24 4 3 -1.2445 -0.2368 24 4 4 -0.2855 -0.0898 24 4 5 0.9204 0.0822 24 4 6 -0.0077 0.1439 24 4 7 1.4377 0.0457 24 4 8 0.8420 0.1412 24 5 1 -1.2566 -0.1139 24 5 2 -0.3716 -0.0731 24 5 3 1.4160 -0.0214 24 5 4 0.2630 -0.0558 24 5 5 -0.6280 0.0316 24 5 6 -0.2737 -0.1045 24 5 7 0.4430 -0.0214 24 6 0 0.3005 -0.0779 24 6 1 1.0654 -0.0467 24 6 2 -1.0086 -0.0346 24 6 3 -0.3889 0.0863 24 6 4 1.7533 0.1119 24 6 5 0.6299 0.1173 24 6 6 -0.1867 0.0176 24 6 7 -0.6192 -0.0288 24 7 1 -0.0874 -0.0505 24 7 2 -0.2226 0.0261 24 7 3 -0.5976 0.0368 24 7 4 -0.6259 0.0183 24 7 5 0.4801 -0.0497 24 7 6 -0.2301 0.0812 24 7 7 0.2343 0.1404 24 8 0 -0.2795 -0.0845 24 8 1 -1.5508 0.0771 24 8 2 0.5255 -0.0115 24 8 3 0.3966 -0.0180 24 8 4 0.0410 0.0554 24 8 5 -0.6406 -0.0145 24 8 6 -0.9370 -0.1644 24 8 7 0.0812 -0.1052 24 9 1 -0.5451 0.1191 24 9 2 -0.4778 0.0143 24 9 3 -0.5782 -0.0201 24 9 4 0.7606 -0.0507 24 9 5 0.5065 0.0393 24 9 6 -0.6251 -0.0272 24 10 0 -2.0530 -0.0472 24 10 1 1.4073 -0.0096 24 10 2 -0.0210 -0.1082 24 10 3 -1.1209 0.1589 24 10 4 0.7911 0.0360 24 10 5 -0.5641 -0.1652 24 10 6 0.5034 0.0213 24 11 1 -0.1153 -0.0313 24 11 2 -1.4674 -0.0808 24 11 3 -0.2804 -0.0770 24 11 4 1.6103 -0.0758 24 11 5 -0.6722 0.0523 24 12 0 0.1995 0.0343 24 12 1 0.7316 0.0563 24 12 2 -1.0112 0.0480 24 12 3 0.9706 0.1197 24 12 4 0.0386 -0.0980 24 13 1 -1.6371 -0.0847 24 13 2 -0.5621 -0.0526 24 13 3 1.8998 -0.0814 24 14 0 -0.1286 0.1422 24 14 1 0.6932 0.0026 24 14 2 0.0369 -0.0271 25 0 2 -1.2224 0.1294 25 0 4 0.6048 -0.1279 25 0 6 1.1976 0.2405 25 1 0 -0.0867 -0.2944 25 1 1 -1.7252 0.2209 25 1 2 0.1025 -0.1676 25 1 3 -0.6984 -0.2008 25 1 4 -0.2220 0.2705 25 1 5 0.4612 -0.0197 25 1 6 -0.3070 0.0219 25 1 7 1.5989 0.2657 25 2 1 -1.1332 -0.1320 25 2 2 1.0641 -0.2263 25 2 3 1.5996 0.0345 25 2 4 0.8213 0.2179 25 2 5 -0.1010 0.1079 25 2 6 -0.3719 -0.1957 25 3 0 -2.1115 0.1580 25 3 1 1.6320 -0.0114 25 3 2 0.0092 -0.0346 25 3 3 0.3386 0.3003 25 3 4 1.5523 0.2166 25 3 5 -0.5375 0.0335 25 3 6 0.5892 -0.0619 25 4 1 0.7778 -0.0549 25 4 2 1.9699 0.1827 25 4 3 -0.2213 0.0739 25 4 4 -1.0751 -0.0574 25 4 5 -0.7929 -0.1923 25 4 6 0.7710 0.0254 25 5 0 1.6581 0.1771 25 5 1 -0.2836 0.1224 25 5 2 -0.3164 0.1273 25 5 3 1.3074 0.0281 25 5 4 -1.2557 -0.0659 25 5 5 -0.7705 -0.2047 25 5 6 0.0778 -0.1267 25 6 1 0.5045 0.1508 25 6 2 0.0130 -0.0250 25 6 3 -0.4965 -0.0871 25 6 4 0.5736 0.0212 25 6 5 0.6589 0.1172 25 6 6 0.3778 0.1027 25 7 0 -1.1326 0.1381 25 7 1 0.3378 -0.0764 25 7 2 0.4294 -0.0468 25 7 3 -0.6802 -0.0057 25 7 4 -0.1694 -0.1004 25 7 5 0.7061 -0.0730 25 8 1 0.3500 -0.0961 25 8 2 0.6134 -0.0435 25 8 3 0.8439 0.0975 25 8 4 -0.0082 0.0261 25 8 5 -1.0559 -0.1329 25 9 0 1.8839 0.0492 25 9 1 0.0237 0.0153 25 9 2 -0.9784 0.1294 25 9 3 1.4499 -0.0976 25 9 4 0.1091 -0.0962 25 10 1 0.1599 -0.0679 25 10 2 1.0279 0.1020 25 10 3 0.4974 -0.0242 25 11 0 0.2054 0.0772 25 11 1 -1.4101 -0.0577 25 11 2 1.3779 -0.0355 26 0 0 -1.7474 0.3918 26 0 2 0.3742 -0.0997 26 0 4 1.2765 -0.2349 26 1 1 0.4677 -0.2483 26 1 2 0.1656 0.2366 26 1 3 -0.1006 0.3620 26 1 4 -0.4348 -0.2281 26 1 5 -1.1225 -0.5220 26 2 0 2.5181 0.1113 26 2 1 0.7387 -0.0731 26 2 2 -0.4511 0.1328 26 2 3 0.6954 -0.1344 26 2 4 -1.2798 -0.2093 26 2 5 -0.6563 -0.0276 26 3 1 0.3921 0.2040 26 3 2 -1.2118 -0.0008 26 3 3 -1.1352 -0.2637 26 3 4 -0.5806 -0.1975 26 4 0 -0.3482 -0.1282 26 4 1 -1.6272 -0.1455 26 4 2 0.5762 -0.1506 26 4 3 -1.1637 -0.1330 26 4 4 -0.2453 -0.0944 26 5 1 -0.5755 -0.1048 26 5 2 -1.1363 -0.0940 26 5 3 0.4666 0.1011 26 5 4 0.6258 0.1490 26 6 0 -0.2050 -0.2187 26 6 1 0.7235 -0.0464 26 6 2 -0.1274 0.0536 26 6 3 0.0610 -0.0179 26 7 1 -0.4055 -0.0033 26 7 2 -0.2858 0.0844 26 7 3 -0.3369 -0.0612 26 8 0 -0.1593 -0.0865 26 8 1 -0.6505 0.0435 26 8 2 0.7208 -0.1259 27 1 0 0.1179 -0.2520 27 1 1 -1.3933 -0.0210 27 2 1 -0.1331 -0.0120 27 3 0 -1.9633 -0.0631 0 0 0 0.0 0.0 ; _shelx_fab_checksum 38701 _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 ; _oxdiff_exptl_absorpt_empirical_full_max 1.823 _oxdiff_exptl_absorpt_empirical_full_min 0.577 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.25221(3) 0.43735(3) 0.41476(5) 0.02986(18) Uani 1 1 d . . . . . Zn2 Zn 0.500000 0.39735(4) 0.250000 0.0298(2) Uani 1 2 d S T P A . K1 K 0.35070(5) 0.34370(5) 0.28227(9) 0.0338(3) Uani 1 1 d . . . . . K2 K 0.42354(5) 0.46393(5) 0.44132(8) 0.0311(3) Uani 1 1 d D . . . . O1 O 0.25181(18) 0.40797(17) 0.2850(2) 0.0341(8) Uani 1 1 d . . . . . O2 O 0.25481(19) 0.32811(17) 0.1595(3) 0.0361(9) Uani 1 1 d . . . . . O3 O 0.30327(18) 0.50278(16) 0.4350(3) 0.0335(8) Uani 1 1 d . . . . . O4 O 0.39878(19) 0.56488(18) 0.3808(3) 0.0430(10) Uani 1 1 d D . . . . O5 O 0.32881(17) 0.39252(17) 0.4675(3) 0.0349(9) Uani 1 1 d . . . . . O6 O 0.3259(2) 0.30066(19) 0.4585(3) 0.0509(12) Uani 1 1 d . . . . . O7 O 0.4376(2) 0.3088(2) 0.1638(4) 0.0575(13) Uani 1 1 d . . . . . O8 O 0.5246(2) 0.35602(17) 0.1324(3) 0.0414(10) Uani 1 1 d . . . . . O9 O 0.54580(17) 0.48385(16) 0.3856(3) 0.0346(9) Uani 1 1 d . . . . . O10 O 0.57853(16) 0.43827(15) 0.2584(2) 0.0303(8) Uani 1 1 d . . . . . N1 N 0.1667(2) 0.4865(2) 0.3849(3) 0.0354(11) Uani 1 1 d . . . . . N2 N 0.1879(2) 0.3967(2) 0.5115(3) 0.0354(11) Uani 1 1 d . . . . . C1 C 0.2029(2) 0.4032(2) 0.2277(4) 0.0324(12) Uani 1 1 d . . . . . C2 C 0.2012(3) 0.3600(2) 0.1606(4) 0.0341(12) Uani 1 1 d . . . . . C3 C 0.1510(3) 0.3522(3) 0.1009(4) 0.0382(14) Uani 1 1 d . . . . . H3 H 0.151551 0.322761 0.056454 0.046 Uiso 1 1 calc R U . . . C4 C 0.0991(3) 0.3873(3) 0.1049(4) 0.0413(15) Uani 1 1 d . . . . . C5 C 0.1015(3) 0.4313(3) 0.1659(4) 0.0410(14) Uani 1 1 d . . . . . H5 H 0.067220 0.456350 0.167143 0.049 Uiso 1 1 calc R U . . . C6 C 0.1523(3) 0.4407(3) 0.2263(4) 0.0341(12) Uani 1 1 d . . . . . C7 C 0.1572(3) 0.4934(3) 0.2814(4) 0.0384(13) Uani 1 1 d . . . . . H7A H 0.192531 0.515178 0.255639 0.046 Uiso 1 1 calc R U . . . H7B H 0.118309 0.514939 0.271175 0.046 Uiso 1 1 calc R U . . . C8 C 0.2649(3) 0.2940(3) 0.0779(4) 0.0487(16) Uani 1 1 d . . . . . H8A H 0.262017 0.316557 0.020320 0.073 Uiso 1 1 calc R U . . . H8B H 0.233005 0.264966 0.075898 0.073 Uiso 1 1 calc R U . . . H8C H 0.306691 0.277249 0.081606 0.073 Uiso 1 1 calc R U . . . C9 C 0.0434(3) 0.3779(3) 0.0395(5) 0.0579(19) Uani 1 1 d . . . . . H9A H 0.021403 0.344182 0.058610 0.087 Uiso 1 1 calc R U . . . H9B H 0.058301 0.373976 -0.025965 0.087 Uiso 1 1 calc R U . . . H9C H 0.014725 0.409338 0.043677 0.087 Uiso 1 1 calc R U . . . C10 C 0.2900(3) 0.5536(2) 0.4024(4) 0.0310(11) Uani 1 1 d . . . . . C11 C 0.3403(3) 0.5878(2) 0.3729(4) 0.0360(13) Uani 1 1 d . . . . . C12 C 0.3290(3) 0.6403(3) 0.3389(4) 0.0401(14) Uani 1 1 d . . . . . H12 H 0.363458 0.662866 0.320883 0.048 Uiso 1 1 calc R U . . . C13 C 0.2685(3) 0.6610(3) 0.3305(4) 0.0381(13) Uani 1 1 d . . . . . C14 C 0.2195(3) 0.6271(3) 0.3591(4) 0.0399(14) Uani 1 1 d . . . . . H14 H 0.177757 0.640534 0.354346 0.048 Uiso 1 1 calc R U . . . C15 C 0.2292(3) 0.5740(2) 0.3948(4) 0.0361(13) Uani 1 1 d . . . . . C16 C 0.1747(3) 0.5414(2) 0.4306(4) 0.0380(13) Uani 1 1 d . . . . . H16A H 0.179729 0.535960 0.499815 0.046 Uiso 1 1 calc R U . . . H16B H 0.135884 0.563144 0.420665 0.046 Uiso 1 1 calc R U . . . C17 C 0.4492(11) 0.5935(10) 0.333(3) 0.074(9) Uani 0.49(6) 1 d D . P A 1 H17A H 0.484726 0.597066 0.376502 0.110 Uiso 0.49(6) 1 d R U P A 1 H17B H 0.462316 0.572636 0.276602 0.110 Uiso 0.49(6) 1 d R U P A 1 H17C H 0.434886 0.630196 0.313502 0.110 Uiso 0.49(6) 1 d R U P A 1 C17A C 0.4503(10) 0.6029(9) 0.376(4) 0.074(9) Uani 0.51(6) 1 d D . P A 2 H17D H 0.469510 0.607556 0.438334 0.110 Uiso 0.51(6) 1 d R U P A 2 H17E H 0.481460 0.588136 0.331324 0.110 Uiso 0.51(6) 1 d R U P A 2 H17F H 0.435370 0.638756 0.352635 0.110 Uiso 0.51(6) 1 d R U P A 2 C18 C 0.2573(4) 0.7186(3) 0.2953(5) 0.0495(16) Uani 1 1 d . . . . . H18A H 0.250704 0.743225 0.349492 0.074 Uiso 1 1 calc R U . . . H18B H 0.220064 0.719059 0.254527 0.074 Uiso 1 1 calc R U . . . H18C H 0.293854 0.731034 0.258955 0.074 Uiso 1 1 calc R U . . . C19 C 0.1132(3) 0.4570(3) 0.4280(4) 0.0424(15) Uani 1 1 d . . . . . H19A H 0.099027 0.427319 0.384927 0.051 Uiso 1 1 calc R U . . . H19B H 0.077845 0.482906 0.437552 0.051 Uiso 1 1 calc R U . . . C20 C 0.1324(3) 0.4325(3) 0.5223(4) 0.0417(14) Uani 1 1 d . . . . . H20A H 0.142131 0.462590 0.567553 0.050 Uiso 1 1 calc R U . . . H20B H 0.097166 0.410789 0.548638 0.050 Uiso 1 1 calc R U . . . C21 C 0.2135(3) 0.3844(3) 0.6064(4) 0.0455(16) Uani 1 1 d . . . . . H21A H 0.247258 0.357191 0.600635 0.068 Uiso 1 1 calc R U . . . H21B H 0.180121 0.369556 0.646842 0.068 Uiso 1 1 calc R U . . . H21C H 0.230089 0.418310 0.634695 0.068 Uiso 1 1 calc R U . . . C22 C 0.1706(3) 0.3431(3) 0.4659(5) 0.0432(15) Uani 1 1 d . . . . . H22A H 0.149703 0.350285 0.405222 0.065 Uiso 1 1 calc R U . . . H22B H 0.142191 0.322677 0.507731 0.065 Uiso 1 1 calc R U . . . H22C H 0.208649 0.321342 0.454911 0.065 Uiso 1 1 calc R U . . . C23 C 0.3412(3) 0.3436(3) 0.4984(4) 0.0365(13) Uani 1 1 d . . . . . C24 C 0.3783(3) 0.3415(3) 0.5898(4) 0.0458(15) Uani 1 1 d . . . . . H24A H 0.418576 0.360351 0.580981 0.069 Uiso 1 1 calc R U . . . H24B H 0.385900 0.302944 0.607347 0.069 Uiso 1 1 calc R U . . . H24C H 0.354585 0.359766 0.640396 0.069 Uiso 1 1 calc R U . . . C25 C 0.4851(3) 0.3159(3) 0.1173(5) 0.0452(15) Uani 1 1 d . . . . . C26 C 0.5025(4) 0.2755(4) 0.0401(6) 0.075(3) Uani 1 1 d . . . . . H26A H 0.488462 0.289825 -0.021410 0.112 Uiso 1 1 calc R U . . . H26B H 0.482095 0.240004 0.052431 0.112 Uiso 1 1 calc R U . . . H26C H 0.548096 0.270511 0.039074 0.112 Uiso 1 1 calc R U . . . C27 C 0.5868(2) 0.4726(2) 0.3280(3) 0.0272(11) Uani 1 1 d . . . . . C28 C 0.6512(3) 0.4980(3) 0.3336(4) 0.0357(12) Uani 1 1 d . . . . . H28A H 0.670981 0.487813 0.393846 0.054 Uiso 1 1 calc R U . . . H28B H 0.647579 0.538270 0.329785 0.054 Uiso 1 1 calc R U . . . H28C H 0.676909 0.484608 0.280783 0.054 Uiso 1 1 calc R U . . . H30A H -0.087(7) 0.274(6) 0.145(10) 0.054 Uiso 0.5 1 d . U P B -1 H30B H -0.026(6) 0.295(6) 0.127(10) 0.054 Uiso 0.5 1 d . U P C -1 H30C H -0.064(6) 0.317(6) 0.267(10) 0.054 Uiso 0.5 1 d . U P D -1 O11 O -0.0094(17) 0.2095(4) 0.270(3) 0.094(10) Uani 0.5 1 d D U P E -1 C29 C -0.0010(16) 0.2578(4) 0.253(2) 0.046(2) Uani 0.5 1 d D U P E -1 C30 C -0.0499(19) 0.2914(17) 0.203(4) 0.056(8) Uani 0.5 1 d D U P E -1 C31 C 0.0596(19) 0.2840(16) 0.283(3) 0.052(7) Uani 0.5 1 d D U P E -1 H31A H 0.084268 0.257429 0.320326 0.078 Uiso 0.5 1 calc R U P E -1 H31B H 0.050672 0.316433 0.322666 0.078 Uiso 0.5 1 calc R U P E -1 H31C H 0.083427 0.295210 0.227234 0.078 Uiso 0.5 1 calc R U P E -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0346(3) 0.0315(4) 0.0235(3) -0.0005(3) 0.0013(3) -0.0053(3) Zn2 0.0356(5) 0.0292(5) 0.0247(5) 0.000 -0.0018(4) 0.000 K1 0.0370(6) 0.0350(7) 0.0296(6) -0.0015(5) -0.0005(5) -0.0034(5) K2 0.0339(5) 0.0351(6) 0.0243(5) -0.0018(5) 0.0008(4) -0.0062(5) O1 0.0380(19) 0.043(2) 0.0214(18) -0.0006(17) 0.0001(16) -0.0026(17) O2 0.047(2) 0.036(2) 0.0262(19) -0.0037(16) -0.0011(17) -0.0031(18) O3 0.045(2) 0.028(2) 0.028(2) 0.0025(17) -0.0011(16) -0.0026(16) O4 0.043(2) 0.036(2) 0.050(3) 0.009(2) -0.0064(19) -0.0112(18) O5 0.0383(19) 0.035(2) 0.031(2) 0.0004(18) -0.0008(16) -0.0096(17) O6 0.067(3) 0.036(3) 0.049(3) 0.000(2) 0.002(2) -0.019(2) O7 0.050(3) 0.064(3) 0.059(3) -0.019(3) 0.006(2) 0.001(2) O8 0.055(2) 0.036(2) 0.033(2) -0.0045(19) -0.0006(19) 0.0005(19) O9 0.0368(19) 0.041(2) 0.0256(19) -0.0091(17) 0.0014(16) -0.0035(16) O10 0.0354(18) 0.033(2) 0.0222(18) -0.0020(16) -0.0007(15) 0.0013(15) N1 0.037(2) 0.039(3) 0.030(3) 0.003(2) 0.002(2) -0.003(2) N2 0.039(2) 0.041(3) 0.026(2) 0.002(2) 0.005(2) -0.008(2) C1 0.033(3) 0.041(3) 0.023(3) 0.000(2) 0.004(2) -0.007(2) C2 0.040(3) 0.035(3) 0.027(3) 0.003(2) 0.005(2) -0.005(2) C3 0.044(3) 0.050(4) 0.021(3) 0.000(3) 0.001(2) -0.013(3) C4 0.035(3) 0.055(4) 0.033(3) -0.004(3) 0.003(2) -0.011(3) C5 0.035(3) 0.053(4) 0.035(3) 0.005(3) 0.002(2) -0.003(3) C6 0.037(3) 0.039(3) 0.026(3) -0.001(2) 0.005(2) -0.007(2) C7 0.041(3) 0.046(4) 0.028(3) 0.007(3) 0.001(2) 0.001(3) C8 0.063(4) 0.054(4) 0.029(3) -0.010(3) -0.005(3) 0.008(3) C9 0.046(4) 0.074(6) 0.053(4) -0.004(4) -0.004(3) -0.012(3) C10 0.047(3) 0.027(3) 0.019(2) -0.004(2) 0.001(2) -0.004(2) C11 0.050(3) 0.028(3) 0.030(3) 0.003(2) -0.004(3) -0.007(2) C12 0.057(4) 0.037(3) 0.026(3) 0.003(3) -0.002(3) -0.012(3) C13 0.061(4) 0.033(3) 0.021(3) -0.002(2) -0.001(2) -0.004(3) C14 0.059(4) 0.040(4) 0.021(3) -0.010(2) 0.006(3) 0.007(3) C15 0.053(3) 0.031(3) 0.025(3) -0.006(2) 0.004(2) 0.000(2) C16 0.045(3) 0.034(3) 0.035(3) -0.003(3) 0.005(3) 0.005(2) C17 0.053(5) 0.046(7) 0.12(2) 0.022(11) -0.015(10) -0.023(5) C17A 0.053(5) 0.046(7) 0.12(2) 0.022(11) -0.015(10) -0.023(5) C18 0.076(5) 0.029(3) 0.043(4) 0.001(3) -0.003(3) 0.006(3) C19 0.031(3) 0.056(4) 0.041(3) 0.003(3) 0.010(3) -0.005(3) C20 0.039(3) 0.053(4) 0.033(3) 0.002(3) 0.011(2) 0.000(3) C21 0.049(3) 0.064(5) 0.023(3) 0.002(3) 0.006(3) -0.009(3) C22 0.045(3) 0.046(4) 0.038(3) 0.003(3) 0.004(3) -0.013(3) C23 0.040(3) 0.036(3) 0.034(3) 0.002(3) 0.000(2) -0.009(2) C24 0.053(3) 0.049(4) 0.036(3) 0.010(3) 0.002(3) -0.002(3) C25 0.053(4) 0.042(4) 0.040(3) -0.007(3) 0.001(3) -0.003(3) C26 0.094(6) 0.067(6) 0.064(5) -0.027(4) 0.024(5) -0.027(5) C27 0.032(2) 0.032(3) 0.018(2) -0.001(2) 0.002(2) -0.002(2) C28 0.038(3) 0.046(4) 0.023(3) -0.002(3) 0.003(2) -0.008(3) O11 0.10(2) 0.038(4) 0.14(3) 0.023(10) -0.029(16) -0.019(9) C29 0.062(5) 0.039(5) 0.036(6) 0.004(12) 0.007(4) -0.008(9) C30 0.045(9) 0.055(13) 0.067(18) 0.010(11) 0.028(8) 0.004(9) C31 0.066(15) 0.050(13) 0.040(12) -0.012(10) 0.015(11) -0.011(12) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 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' K K 0.3868 1.0657 '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' O O 0.0492 0.0322 '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 0 0 1 0.0578 0 0 -1 0.0541 1 0 0 0.0093 -1 1 0 0.0119 1 -2 0 0.0217 -13 -4 1 0.0118 0 16 -1 0.0093 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 K1 Zn1 K2 65.88(3) . . ? O1 Zn1 K1 44.98(12) . . ? O1 Zn1 K2 99.24(11) . . ? O1 Zn1 O5 98.37(16) . . ? O1 Zn1 N1 90.87(17) . . ? O1 Zn1 N2 114.70(17) . . ? O3 Zn1 K1 105.28(12) . . ? O3 Zn1 K2 45.25(12) . . ? O3 Zn1 O1 115.78(16) . . ? O3 Zn1 O5 86.31(16) . . ? O3 Zn1 N1 92.79(17) . . ? O3 Zn1 N2 129.19(17) . . ? O5 Zn1 K1 53.51(11) . . ? O5 Zn1 K2 44.89(10) . . ? O5 Zn1 N1 170.14(16) . . ? O5 Zn1 N2 91.93(17) . . ? N1 Zn1 K1 135.85(13) . . ? N1 Zn1 K2 136.97(13) . . ? N2 Zn1 K1 113.98(14) . . ? N2 Zn1 K2 129.38(13) . . ? N2 Zn1 N1 81.03(18) . . ? K1 Zn2 K1 135.93(5) . 3_655 ? K1 Zn2 K2 69.44(3) . . ? K1 Zn2 K2 133.90(3) . 3_655 ? K1 Zn2 K2 133.90(3) 3_655 . ? K1 Zn2 K2 69.44(3) 3_655 3_655 ? K2 Zn2 K2 125.73(5) . 3_655 ? O8 Zn2 K1 99.25(13) 3_655 3_655 ? O8 Zn2 K1 57.61(12) . 3_655 ? O8 Zn2 K1 99.25(13) . . ? O8 Zn2 K1 57.61(12) 3_655 . ? O8 Zn2 K2 58.57(12) 3_655 . ? O8 Zn2 K2 167.75(12) 3_655 3_655 ? O8 Zn2 K2 167.75(12) . . ? O8 Zn2 K2 58.57(12) . 3_655 ? O8 Zn2 O8 120.1(2) . 3_655 ? O10 Zn2 K1 53.92(11) . 3_655 ? O10 Zn2 K1 166.16(11) 3_655 3_655 ? O10 Zn2 K1 53.92(11) 3_655 . ? O10 Zn2 K1 166.15(11) . . ? O10 Zn2 K2 96.72(11) 3_655 3_655 ? O10 Zn2 K2 54.45(10) 3_655 . ? O10 Zn2 K2 54.45(10) . 3_655 ? O10 Zn2 K2 96.72(11) . . ? O10 Zn2 O8 115.40(16) 3_655 . ? O10 Zn2 O8 94.57(16) 3_655 3_655 ? O10 Zn2 O8 115.40(16) . 3_655 ? O10 Zn2 O8 94.57(16) . . ? O10 Zn2 O10 118.8(2) 3_655 . ? Zn1 K1 K2 58.43(3) . . ? Zn2 K1 Zn1 111.41(4) . . ? Zn2 K1 K2 56.14(3) . . ? O1 K1 Zn1 31.94(8) . . ? O1 K1 Zn2 121.10(10) . . ? O1 K1 K2 82.53(9) . . ? O1 K1 O2 59.02(12) . . ? O1 K1 O5 67.37(11) . . ? O1 K1 O6 93.32(14) . . ? O1 K1 O7 140.00(15) . . ? O1 K1 O8 131.45(13) . 3_655 ? O1 K1 O10 87.09(12) . 3_655 ? O1 K1 C23 86.11(14) . . ? O2 K1 Zn1 88.84(9) . . ? O2 K1 Zn2 131.44(9) . . ? O2 K1 K2 139.05(10) . . ? O2 K1 O5 120.73(12) . . ? O2 K1 O6 112.36(13) . . ? O2 K1 O8 164.04(13) . 3_655 ? O2 K1 O10 112.97(12) . 3_655 ? O2 K1 C23 126.04(14) . . ? O5 K1 Zn1 35.49(8) . . ? O5 K1 Zn2 96.45(8) . . ? O5 K1 K2 42.27(8) . . ? O5 K1 O8 74.66(11) . 3_655 ? O5 K1 C23 24.85(14) . . ? O6 K1 Zn1 70.10(11) . . ? O6 K1 Zn2 115.96(10) . . ? O6 K1 K2 81.05(10) . . ? O6 K1 O5 46.43(12) . . ? O6 K1 O8 80.92(13) . 3_655 ? O6 K1 O10 126.81(12) . 3_655 ? O6 K1 C23 23.70(14) . . ? O7 K1 Zn1 159.80(13) . . ? O7 K1 Zn2 52.56(11) . . ? O7 K1 K2 108.50(11) . . ? O7 K1 O2 94.63(14) . . ? O7 K1 O5 144.48(14) . . ? O7 K1 O6 125.92(17) . . ? O7 K1 O8 69.83(13) . 3_655 ? O7 K1 O10 75.83(14) . 3_655 ? O7 K1 C23 132.77(17) . . ? O8 K1 Zn1 104.51(9) 3_655 . ? O8 K1 Zn2 35.30(8) 3_655 . ? O8 K1 K2 48.92(9) 3_655 . ? O8 K1 C23 69.58(13) 3_655 . ? O10 K1 Zn1 84.49(8) 3_655 . ? O10 K1 Zn2 34.18(7) 3_655 . ? O10 K1 K2 46.22(8) 3_655 . ? O10 K1 O5 86.36(11) 3_655 . ? O10 K1 O8 60.84(11) 3_655 3_655 ? O10 K1 C23 103.88(14) 3_655 . ? C23 K1 Zn1 56.36(12) . . ? C23 K1 Zn2 101.07(11) . . ? C23 K1 K2 57.72(11) . . ? Zn1 K2 K1 55.68(3) . . ? Zn2 K2 Zn1 107.19(3) . . ? Zn2 K2 K1 54.42(3) . . ? O3 K2 Zn1 30.37(8) . . ? O3 K2 Zn2 124.34(9) . . ? O3 K2 K1 82.45(9) . . ? O3 K2 O8 129.03(12) . 3_655 ? O3 K2 O9 95.20(12) . 5_666 ? O3 K2 O9 144.57(13) . . ? O3 K2 O10 91.61(11) . 3_655 ? O3 K2 C17 79.9(4) . . ? O3 K2 C23 79.89(13) . . ? O4 K2 Zn1 86.12(9) . . ? O4 K2 Zn2 105.57(11) . . ? O4 K2 K1 114.67(10) . . ? O4 K2 O3 58.88(12) . . ? O4 K2 O5 119.42(13) . . ? O4 K2 O8 139.70(13) . 3_655 ? O4 K2 O9 84.81(13) . 5_666 ? O4 K2 O9 86.26(13) . . ? O4 K2 O10 83.23(13) . 3_655 ? O4 K2 C17 21.5(4) . . ? O4 K2 C23 138.23(13) . . ? O5 K2 Zn1 33.45(9) . . ? O5 K2 Zn2 99.01(9) . . ? O5 K2 K1 46.68(9) . . ? O5 K2 O3 61.43(12) . . ? O5 K2 O8 76.35(12) . 3_655 ? O5 K2 O9 110.14(12) . 5_666 ? O5 K2 O9 149.37(13) . . ? O5 K2 O10 89.06(11) . 3_655 ? O5 K2 C17 138.5(5) . . ? O5 K2 C23 18.81(13) . . ? O8 K2 Zn1 100.00(9) 3_655 . ? O8 K2 Zn2 34.46(8) 3_655 . ? O8 K2 K1 46.94(8) 3_655 . ? O8 K2 C17 124.3(6) 3_655 . ? O8 K2 C23 62.67(13) 3_655 . ? O9 K2 Zn1 157.73(9) . . ? O9 K2 Zn1 113.01(8) 5_666 . ? O9 K2 Zn2 139.08(8) 5_666 . ? O9 K2 Zn2 55.21(8) . . ? O9 K2 K1 109.56(8) . . ? O9 K2 K1 154.45(9) 5_666 . ? O9 K2 O8 73.09(12) . 3_655 ? O9 K2 O8 126.88(12) 5_666 3_655 ? O9 K2 O9 87.07(11) . 5_666 ? O9 K2 O10 76.99(10) . 3_655 ? O9 K2 O10 160.61(11) 5_666 3_655 ? O9 K2 C17 64.9(4) . . ? O9 K2 C17 86.5(9) 5_666 . ? O9 K2 C23 106.93(13) 5_666 . ? O9 K2 C23 133.16(14) . . ? O10 K2 Zn1 81.35(7) 3_655 . ? O10 K2 Zn2 33.38(7) 3_655 . ? O10 K2 K1 44.61(8) 3_655 . ? O10 K2 O8 58.89(11) 3_655 3_655 ? O10 K2 C17 76.8(8) 3_655 . ? O10 K2 C23 92.11(13) 3_655 . ? C17 K2 Zn1 105.2(5) . . ? C17 K2 Zn2 90.3(7) . . ? C17 K2 K1 117.8(8) . . ? C23 K2 Zn1 52.22(10) . . ? C23 K2 Zn2 91.48(11) . . ? C23 K2 K1 47.55(10) . . ? C23 K2 C17 156.6(6) . . ? Zn1 O1 K1 103.08(15) . . ? C1 O1 Zn1 127.1(3) . . ? C1 O1 K1 124.9(3) . . ? C2 O2 K1 122.7(3) . . ? C2 O2 C8 117.2(4) . . ? C8 O2 K1 118.7(3) . . ? Zn1 O3 K2 104.37(16) . . ? C10 O3 Zn1 125.4(3) . . ? C10 O3 K2 121.6(3) . . ? C11 O4 K2 125.7(3) . . ? C11 O4 C17 116.4(10) . . ? C11 O4 C17A 115.6(10) . . ? C17 O4 K2 116.5(9) . . ? C17A O4 K2 117.3(8) . . ? Zn1 O5 K1 91.00(13) . . ? Zn1 O5 K2 101.65(15) . . ? K2 O5 K1 91.06(11) . . ? C23 O5 Zn1 139.0(3) . . ? C23 O5 K1 84.0(3) . . ? C23 O5 K2 119.0(3) . . ? C23 O6 K1 92.3(4) . . ? C25 O7 K1 151.7(5) . . ? Zn2 O8 K1 87.09(14) . 3_655 ? Zn2 O8 K2 86.97(14) . 3_655 ? K1 O8 K2 84.14(11) 3_655 3_655 ? C25 O8 Zn2 109.8(4) . . ? C25 O8 K1 125.2(4) . 3_655 ? C25 O8 K2 145.6(4) . 3_655 ? K2 O9 K2 92.93(11) . 5_666 ? C27 O9 K2 145.4(3) . . ? C27 O9 K2 120.5(3) . 5_666 ? Zn2 O10 K1 91.90(14) . 3_655 ? Zn2 O10 K2 92.17(13) . 3_655 ? K1 O10 K2 89.17(10) 3_655 3_655 ? C27 O10 Zn2 119.2(3) . . ? C27 O10 K1 127.2(3) . 3_655 ? C27 O10 K2 127.0(3) . 3_655 ? C7 N1 Zn1 111.0(3) . . ? C7 N1 C16 110.0(5) . . ? C16 N1 Zn1 107.7(3) . . ? C19 N1 Zn1 107.2(4) . . ? C19 N1 C7 110.7(5) . . ? C19 N1 C16 110.1(5) . . ? C20 N2 Zn1 107.7(4) . . ? C20 N2 C21 108.8(5) . . ? C20 N2 C22 111.1(5) . . ? C21 N2 Zn1 115.3(4) . . ? C21 N2 C22 107.8(5) . . ? C22 N2 Zn1 106.2(3) . . ? O1 C1 C2 119.5(5) . . ? O1 C1 C6 123.7(5) . . ? C6 C1 C2 116.7(5) . . ? O2 C2 C1 113.7(5) . . ? C3 C2 O2 124.1(5) . . ? C3 C2 C1 122.1(6) . . ? C2 C3 H3 119.8 . . ? C2 C3 C4 120.5(6) . . ? C4 C3 H3 119.8 . . ? C3 C4 C9 120.0(6) . . ? C5 C4 C3 118.1(5) . . ? C5 C4 C9 121.8(6) . . ? C4 C5 H5 118.7 . . ? C4 C5 C6 122.5(6) . . ? C6 C5 H5 118.7 . . ? C1 C6 C7 119.3(5) . . ? C5 C6 C1 119.8(5) . . ? C5 C6 C7 120.5(6) . . ? N1 C7 C6 115.1(5) . . ? N1 C7 H7A 108.5 . . ? N1 C7 H7B 108.5 . . ? C6 C7 H7A 108.5 . . ? C6 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? O2 C8 H8A 109.5 . . ? O2 C8 H8B 109.5 . . ? O2 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O3 C10 C11 118.5(5) . . ? O3 C10 C15 123.3(5) . . ? C15 C10 C11 118.2(5) . . ? O4 C11 C10 115.3(5) . . ? O4 C11 C12 124.1(5) . . ? C12 C11 C10 120.6(6) . . ? C11 C12 H12 119.2 . . ? C11 C12 C13 121.6(6) . . ? C13 C12 H12 119.2 . . ? C12 C13 C14 117.4(6) . . ? C12 C13 C18 120.7(6) . . ? C14 C13 C18 121.8(6) . . ? C13 C14 H14 118.7 . . ? C13 C14 C15 122.6(6) . . ? C15 C14 H14 118.7 . . ? C10 C15 C14 119.6(6) . . ? C10 C15 C16 120.6(5) . . ? C14 C15 C16 119.7(6) . . ? N1 C16 C15 114.6(5) . . ? N1 C16 H16A 108.6 . . ? N1 C16 H16B 108.6 . . ? C15 C16 H16A 108.6 . . ? C15 C16 H16B 108.6 . . ? H16A C16 H16B 107.6 . . ? K2 C17 H17A 85.8 . . ? K2 C17 H17B 86.3 . . ? K2 C17 H17C 151.6 . . ? O4 C17 K2 42.0(6) . . ? O4 C17 H17A 108.8 . . ? O4 C17 H17B 110.1 . . ? O4 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.4 . . ? O4 C17A H17D 110.3 . . ? O4 C17A H17E 108.3 . . ? O4 C17A H17F 109.8 . . ? H17D C17A H17E 109.5 . . ? H17D C17A H17F 109.5 . . ? H17E C17A H17F 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N1 C19 H19A 109.6 . . ? N1 C19 H19B 109.6 . . ? N1 C19 C20 110.1(5) . . ? H19A C19 H19B 108.2 . . ? C20 C19 H19A 109.6 . . ? C20 C19 H19B 109.6 . . ? N2 C20 C19 110.9(5) . . ? N2 C20 H20A 109.4 . . ? N2 C20 H20B 109.4 . . ? C19 C20 H20A 109.4 . . ? C19 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? N2 C21 H21A 109.5 . . ? N2 C21 H21B 109.5 . . ? N2 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N2 C22 H22A 109.5 . . ? N2 C22 H22B 109.5 . . ? N2 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? K1 C23 K2 74.73(13) . . ? O5 C23 K1 71.1(3) . . ? O5 C23 K2 42.2(3) . . ? O5 C23 C24 115.2(5) . . ? O6 C23 K1 64.0(3) . . ? O6 C23 K2 137.3(4) . . ? O6 C23 O5 124.8(6) . . ? O6 C23 C24 120.0(6) . . ? C24 C23 K1 144.6(4) . . ? C24 C23 K2 87.8(3) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O7 C25 O8 123.6(6) . . ? O7 C25 C26 120.0(6) . . ? O8 C25 C26 116.4(6) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O9 C27 O10 123.2(5) . . ? O9 C27 C28 121.6(5) . . ? O10 C27 C28 115.2(4) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O11 C29 C30 120.9(16) . . ? O11 C29 C31 119.0(16) . . ? C31 C29 C30 120.1(11) . . ? H30A C30 H30B 72(9) . . ? H30A C30 H30C 123(10) . . ? H30B C30 H30C 142(10) . . ? C29 C30 H30A 126(8) . . ? C29 C30 H30B 100(7) . . ? C29 C30 H30C 97(8) . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31B 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 K1 3.6123(14) . ? Zn1 K2 3.7264(13) . ? Zn1 O1 1.962(4) . ? Zn1 O3 1.945(4) . ? Zn1 O5 2.098(4) . ? Zn1 N1 2.219(5) . ? Zn1 N2 2.171(4) . ? Zn2 K1 3.4674(12) 3_655 ? Zn2 K1 3.4674(12) . ? Zn2 K2 3.5402(12) 3_655 ? Zn2 K2 3.5402(12) . ? Zn2 O8 2.006(4) 3_655 ? Zn2 O8 2.006(4) . ? Zn2 O10 1.949(4) 3_655 ? Zn2 O10 1.949(4) . ? K1 K2 3.9919(17) . ? K1 O1 2.621(4) . ? K1 O2 2.704(4) . ? K1 O5 2.905(4) . ? K1 O6 2.746(5) . ? K1 O7 2.634(5) . ? K1 O8 2.932(4) 3_655 ? K1 O10 2.804(4) 3_655 ? K1 C23 3.053(6) . ? K2 O3 2.732(4) . ? K2 O4 2.645(4) . ? K2 O5 2.685(4) . ? K2 O8 3.025(4) 3_655 ? K2 O9 2.825(4) 5_666 ? K2 O9 2.764(4) . ? K2 O10 2.882(4) 3_655 ? K2 C17 3.536(14) . ? K2 C23 3.498(6) . ? O1 C1 1.324(6) . ? O2 C2 1.380(7) . ? O2 C8 1.432(7) . ? O3 C10 1.345(7) . ? O4 C11 1.369(7) . ? O4 C17 1.446(15) . ? O4 C17A 1.436(13) . ? O5 C23 1.290(7) . ? O6 C23 1.228(7) . ? O7 C25 1.218(8) . ? O8 C25 1.304(8) . ? O9 C27 1.224(6) . ? O10 C27 1.299(6) . ? N1 C7 1.482(7) . ? N1 C16 1.488(8) . ? N1 C19 1.476(7) . ? N2 C20 1.474(8) . ? N2 C21 1.474(7) . ? N2 C22 1.495(8) . ? C1 C2 1.413(8) . ? C1 C6 1.409(8) . ? C2 C3 1.374(8) . ? C3 H3 0.9500 . ? C3 C4 1.396(9) . ? C4 C5 1.370(9) . ? C4 C9 1.521(9) . ? C5 H5 0.9500 . ? C5 C6 1.397(8) . ? C6 C7 1.499(9) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.417(8) . ? C10 C15 1.392(8) . ? C11 C12 1.383(8) . ? C12 H12 0.9500 . ? C12 C13 1.388(9) . ? C13 C14 1.389(9) . ? C13 C18 1.501(9) . ? C14 H14 0.9500 . ? C14 C15 1.396(9) . ? C15 C16 1.494(8) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9798 . ? C17 H17B 0.9802 . ? C17 H17C 0.9803 . ? C17A H17D 0.9798 . ? C17A H17E 0.9801 . ? C17A H17F 0.9802 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C19 C20 1.512(9) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.513(8) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.510(10) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.507(7) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? O11 C29 1.207(12) . ? C29 C30 1.501(12) . ? C29 C31 1.501(12) . ? C30 H30A 1.20(14) . ? C30 H30B 1.20(15) . ? C30 H30C 1.13(15) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Zn1 O1 C1 C2 -149.2(4) . . . . ? Zn1 O1 C1 C6 33.6(7) . . . . ? Zn1 O3 C10 C11 -144.2(4) . . . . ? Zn1 O3 C10 C15 34.8(7) . . . . ? Zn1 O5 C23 K1 84.6(5) . . . . ? Zn1 O5 C23 K2 172.5(7) . . . . ? Zn1 O5 C23 O6 48.0(9) . . . . ? Zn1 O5 C23 C24 -133.1(5) . . . . ? Zn1 N1 C7 C6 57.4(5) . . . . ? Zn1 N1 C16 C15 61.2(5) . . . . ? Zn1 N1 C19 C20 38.6(6) . . . . ? Zn1 N2 C20 C19 41.3(6) . . . . ? Zn2 O8 C25 O7 6.2(8) . . . . ? Zn2 O8 C25 C26 -171.1(6) . . . . ? Zn2 O10 C27 O9 -5.6(7) . . . . ? Zn2 O10 C27 C28 174.3(4) . . . . ? K1 O1 C1 C2 1.7(7) . . . . ? K1 O1 C1 C6 -175.4(4) . . . . ? K1 O2 C2 C1 3.6(6) . . . . ? K1 O2 C2 C3 -178.2(4) . . . . ? K1 O5 C23 K2 87.9(3) . . . . ? K1 O5 C23 O6 -36.6(6) . . . . ? K1 O5 C23 C24 142.3(5) . . . . ? K1 O6 C23 K2 -15.8(6) . . . . ? K1 O6 C23 O5 38.9(6) . . . . ? K1 O6 C23 C24 -139.9(5) . . . . ? K1 O7 C25 O8 17.4(15) . . . . ? K1 O7 C25 C26 -165.4(7) . . . . ? K1 O8 C25 O7 107.1(7) 3_655 . . . ? K1 O8 C25 C26 -70.2(8) 3_655 . . . ? K1 O10 C27 O9 -123.8(5) 3_655 . . . ? K1 O10 C27 C28 56.1(6) 3_655 . . . ? K2 O3 C10 C11 -1.4(6) . . . . ? K2 O3 C10 C15 177.5(4) . . . . ? K2 O4 C11 C10 1.6(7) . . . . ? K2 O4 C11 C12 -178.5(4) . . . . ? K2 O5 C23 K1 -87.9(3) . . . . ? K2 O5 C23 O6 -124.5(5) . . . . ? K2 O5 C23 C24 54.4(6) . . . . ? K2 O8 C25 O7 -109.1(8) 3_655 . . . ? K2 O8 C25 C26 73.6(9) 3_655 . . . ? K2 O9 C27 O10 0.8(10) . . . . ? K2 O9 C27 O10 164.0(4) 5_666 . . . ? K2 O9 C27 C28 -179.1(4) . . . . ? K2 O9 C27 C28 -15.9(7) 5_666 . . . ? K2 O10 C27 O9 112.8(5) 3_655 . . . ? K2 O10 C27 C28 -67.2(6) 3_655 . . . ? O1 C1 C2 O2 -3.4(7) . . . . ? O1 C1 C2 C3 178.4(5) . . . . ? O1 C1 C6 C5 -177.6(5) . . . . ? O1 C1 C6 C7 9.3(8) . . . . ? O2 C2 C3 C4 -178.2(5) . . . . ? O3 C10 C11 O4 0.0(8) . . . . ? O3 C10 C11 C12 -180.0(5) . . . . ? O3 C10 C15 C14 -179.3(5) . . . . ? O3 C10 C15 C16 5.1(8) . . . . ? O4 C11 C12 C13 178.6(5) . . . . ? N1 C19 C20 N2 -55.4(7) . . . . ? C1 C2 C3 C4 -0.2(9) . . . . ? C1 C6 C7 N1 -59.7(7) . . . . ? C2 C1 C6 C5 5.2(8) . . . . ? C2 C1 C6 C7 -167.9(5) . . . . ? C2 C3 C4 C5 3.8(9) . . . . ? C2 C3 C4 C9 -179.1(6) . . . . ? C3 C4 C5 C6 -2.8(9) . . . . ? C4 C5 C6 C1 -1.8(9) . . . . ? C4 C5 C6 C7 171.2(6) . . . . ? C5 C6 C7 N1 127.3(6) . . . . ? C6 C1 C2 O2 174.0(5) . . . . ? C6 C1 C2 C3 -4.3(8) . . . . ? C7 N1 C16 C15 -59.9(6) . . . . ? C7 N1 C19 C20 159.8(5) . . . . ? C8 O2 C2 C1 -162.9(5) . . . . ? C8 O2 C2 C3 15.3(8) . . . . ? C9 C4 C5 C6 -179.8(6) . . . . ? C10 C11 C12 C13 -1.5(9) . . . . ? C10 C15 C16 N1 -60.0(7) . . . . ? C11 O4 C17 K2 -167(2) . . . . ? C11 C10 C15 C14 -0.3(8) . . . . ? C11 C10 C15 C16 -176.0(5) . . . . ? C11 C12 C13 C14 1.1(9) . . . . ? C11 C12 C13 C18 178.7(6) . . . . ? C12 C13 C14 C15 -0.4(8) . . . . ? C13 C14 C15 C10 0.0(8) . . . . ? C13 C14 C15 C16 175.7(5) . . . . ? C14 C15 C16 N1 124.3(6) . . . . ? C15 C10 C11 O4 -179.0(5) . . . . ? C15 C10 C11 C12 1.1(8) . . . . ? C16 N1 C7 C6 176.5(5) . . . . ? C16 N1 C19 C20 -78.4(6) . . . . ? C17 O4 C11 C10 167(2) . . . . ? C17 O4 C11 C12 -13(2) . . . . ? C17A O4 C11 C10 -164(3) . . . . ? C17A O4 C11 C12 16(3) . . . . ? C18 C13 C14 C15 -178.0(5) . . . . ? C19 N1 C7 C6 -61.6(6) . . . . ? C19 N1 C16 C15 177.8(5) . . . . ? C21 N2 C20 C19 167.0(5) . . . . ? C22 N2 C20 C19 -74.6(6) . . . . ? 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 0.0005 0.0005 0.9997 0.0362 -0.1028 0.0086 -0.0005 -0.0005 -0.9997 -0.0362 0.1028 -0.0086 0.9998 -0.0000 -0.0002 0.0037 -0.0047 -0.0720 -0.9999 0.9994 0.0001 0.0561 0.0259 0.0738 1.0000 -1.9988 -0.0001 -0.1159 -0.0472 -0.0756 -13.2566 -4.4301 0.5458 -0.2947 -0.0882 0.9515 0.3412 15.5365 -1.4420 0.8788 0.4771 -0.0091 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 0.000 0.371 0.750 152.1 32.2 '1 C3H6O' 2 0.000 0.629 0.250 152.1 31.7 '1 C3H6O' 3 0.500 0.129 0.250 152.1 32.1 '1 C3H6O' 4 0.500 0.871 0.750 152.1 31.8 '1 C3H6O'