#------------------------------------------------------------------------------ #$Date: 2020-03-26 05:26:48 +0200 (Thu, 26 Mar 2020) $ #$Revision: 249724 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/02/7240203.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_7240203 loop_ _publ_author_name 'Thorne, Michael Francis' 'G\'omez, Mar\'ia Laura R\'ios' 'Bumstead, Alice M.' 'Li, Shichun' 'Bennett, Thomas Douglas' _publ_section_title ; Mechanochemical Synthesis of Mixed Metal, Mixed Linker Glass-Forming Metal--Organic Frameworks ; _journal_name_full 'Green Chemistry' _journal_paper_doi 10.1039/D0GC00546K _journal_year 2020 _chemical_formula_moiety 'C14.21 H12 N8 Zn2, 0.83*(C3 H8 O1)' _chemical_formula_sum 'C16.69 H18.62 N8 O0.83 Zn2' _chemical_formula_weight 475.35 _chemical_name_common ZIF-62 _chemical_name_systematic Zn(Im)1.72(bIm)0.28 _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_Hall '-P 2ac 2ab' _space_group_name_H-M_alt 'P b c a' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2019-10-13 deposited with the CCDC. 2020-03-25 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 15.6052(5) _cell_length_b 15.8374(6) _cell_length_c 18.1718(5) _cell_measurement_reflns_used 5009 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 64.2590 _cell_measurement_theta_min 4.6650 _cell_volume 4491.1(3) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET) (compiled Aug 4 2014,14:34:23) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET) (compiled Aug 4 2014,14:34:23) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET) (compiled Aug 4 2014,14:34:23) ; _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SUPERFLIP (Palatinus & Chapuis, 2007)' _diffrn_ambient_temperature 293(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.1183 _diffrn_measured_fraction_theta_full 0.9335 _diffrn_measured_fraction_theta_max 0.9986 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -8.00 28.00 1.0000 1.5750 omega____ theta____ kappa____ phi______ frames - 0.0000 -19.0000 90.0000 36 #__ type_ start__ end____ width___ exp.time_ 2 omega 112.00 174.00 1.0000 6.2900 omega____ theta____ kappa____ phi______ frames - 102.5000 -21.0000 30.0000 62 #__ type_ start__ end____ width___ exp.time_ 3 omega 141.00 171.00 1.0000 6.2900 omega____ theta____ kappa____ phi______ frames - 102.5000 -21.0000 -90.0000 30 #__ type_ start__ end____ width___ exp.time_ 4 omega 112.00 176.00 1.0000 6.2900 omega____ theta____ kappa____ phi______ frames - 102.5000 -21.0000 -30.0000 64 #__ type_ start__ end____ width___ exp.time_ 5 omega 59.00 85.00 1.0000 6.2900 omega____ theta____ kappa____ phi______ frames - 102.5000 -104.0000 -150.0000 26 #__ type_ start__ end____ width___ exp.time_ 6 omega 43.00 80.00 1.0000 6.2900 omega____ theta____ kappa____ phi______ frames - 102.5000 -104.0000 -90.0000 37 #__ type_ start__ end____ width___ exp.time_ 7 omega 58.00 85.00 1.0000 6.2900 omega____ theta____ kappa____ phi______ frames - 102.5000 -104.0000 -30.0000 27 #__ type_ start__ end____ width___ exp.time_ 8 omega 43.00 83.00 1.0000 6.2900 omega____ theta____ kappa____ phi______ frames - 102.5000 -54.0000 60.0000 40 #__ type_ start__ end____ width___ exp.time_ 9 omega 51.00 77.00 1.0000 6.2900 omega____ theta____ kappa____ phi______ frames - 102.5000 -54.0000 90.0000 26 #__ type_ start__ end____ width___ exp.time_ 10 omega 50.00 75.00 1.0000 6.2900 omega____ theta____ kappa____ phi______ frames - 102.5000 -43.0000 90.0000 25 #__ type_ start__ end____ width___ exp.time_ 11 omega 44.00 74.00 1.0000 6.2900 omega____ theta____ kappa____ phi______ frames - 102.5000 -43.0000 150.0000 30 #__ type_ start__ end____ width___ exp.time_ 12 omega 38.00 64.00 1.0000 6.2900 omega____ theta____ kappa____ phi______ frames - 102.5000 -32.0000 -60.0000 26 #__ type_ start__ end____ width___ exp.time_ 13 omega 28.00 89.00 1.0000 6.2900 omega____ theta____ kappa____ phi______ frames - 102.5000 -54.0000 -90.0000 61 #__ type_ start__ end____ width___ exp.time_ 14 omega 22.00 69.00 1.0000 6.2900 omega____ theta____ kappa____ phi______ frames - 102.5000 -32.0000 -150.0000 47 #__ type_ start__ end____ width___ exp.time_ 15 omega 1.00 74.00 1.0000 6.2900 omega____ theta____ kappa____ phi______ frames - 51.2500 -125.0000 -180.0000 73 #__ type_ start__ end____ width___ exp.time_ 16 omega -79.00 -35.00 1.0000 1.5750 omega____ theta____ kappa____ phi______ frames - 0.0000 -19.0000 90.0000 44 #__ type_ start__ end____ width___ exp.time_ 17 omega 92.00 157.00 1.0000 6.2900 omega____ theta____ kappa____ phi______ frames - 102.5000 138.0000 -60.0000 65 #__ type_ start__ end____ width___ exp.time_ 18 omega 124.00 150.00 1.0000 6.2900 omega____ theta____ kappa____ phi______ frames - 102.5000 138.0000 120.0000 26 #__ type_ start__ end____ width___ exp.time_ 19 omega -100.00 -46.00 1.0000 6.2900 omega____ theta____ kappa____ phi______ frames - -51.2500 125.0000 -60.0000 54 #__ type_ start__ end____ width___ exp.time_ 20 omega -127.00 -10.00 1.0000 6.2900 omega____ theta____ kappa____ phi______ frames - -51.2500 -45.0000 -60.0000 117 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0855081000 _diffrn_orient_matrix_UB_12 0.0043028000 _diffrn_orient_matrix_UB_13 0.0421615000 _diffrn_orient_matrix_UB_21 0.0113101000 _diffrn_orient_matrix_UB_22 -0.0959529000 _diffrn_orient_matrix_UB_23 -0.0095265000 _diffrn_orient_matrix_UB_31 0.0479314000 _diffrn_orient_matrix_UB_32 0.0150195000 _diffrn_orient_matrix_UB_33 -0.0730337000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0215 _diffrn_reflns_av_sigmaI/netI 0.0310 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 11373 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 66.9682 _diffrn_reflns_theta_max 64.1310 _diffrn_reflns_theta_min 2.4314 _diffrn_source 'sealed X-ray tube' _diffrn_source_type 'Enhance Ultra (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 2.80102 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.77993 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET) (compiled Aug 4 2014,14:34:23) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.405 _exptl_crystal_description Tetrahedral _exptl_crystal_F_000 2151.36 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.576 _refine_diff_density_min -0.462 _refine_diff_density_rms 0.069 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 251 _refine_ls_number_reflns 3732 _refine_ls_number_restraints 34 _refine_ls_restrained_S_all 1.505 _refine_ls_R_factor_all 0.0503 _refine_ls_R_factor_gt 0.0450 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0804P)^2^+3.3200P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1313 _refine_ls_wR_factor_ref 0.1374 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3287 _reflns_number_total 3732 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0gc00546k2.cif _cod_data_source_block shelx _cod_database_code 7240203 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _symmetry_space_group_name_h-m_alt 'P b c a' _reflns_odcompleteness_completeness 93.35 _reflns_odcompleteness_theta 66.97 _reflns_odcompleteness_iscentric 1 _shelx_res_file ; TITL CF solution in Pbca shelx.res created by SHELXL-2018/3 at 18:07:42 on 08-Oct-2019 CELL 1.54184 15.6052 15.8374 18.1718 90.000 90.000 90.000 ZERR 8.00 0.0005 0.0006 0.0005 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, - Z SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N ZN O UNIT 96 0 72 16 0 MERG 2 EXYZ C9a C9b EXYZ C8a C8b EADP C9a C9b EADP C8a C8b EXYZ N7a N7b EXYZ N8a N8b EADP N7a N7b EADP N8a N8b FLAT N6 N5 C9A C7 C10 C8A C13 C12 C11 FLAT C14B N7B N8B C15B C16B C20 C17 C19 C18 DFIX 1.430 0.020 O1S C1S DFIX 1.490 0.020 C1S C3S DFIX 1.490 0.020 C1S C2S DANG 2.390 0.030 O1S C1S O1S C2S DANG 2.390 0.030 O1S C1S O1S C3S DANG 2.500 0.030 C3S C1S C3S C2S DFIX 1.430 0.020 O1Sb C1Sb DFIX 1.490 0.020 C1Sb C3Sb DFIX 1.490 0.020 C1Sb C2Sb DANG 2.390 0.030 O1Sb C1Sb O1Sb C2Sb DANG 2.390 0.030 O1Sb C1Sb O1Sb C3Sb DANG 2.500 0.030 C3Sb C1Sb C3Sb C2Sb DFIX 1.32 0.020 C14B N7B DFIX 1.32 0.020 C14B N8B DFIX 1.35 0.020 C16B N7B DFIX 1.35 0.020 C15B N8B FMAP 2 PLAN 20 ACTA 50.00 L.S. 50 WGHT 0.080400 3.320000 FVAR 2.13025 0.46246 0.08917 0.42309 0.40442 ZN1 4 0.801281 0.133937 0.099290 11.00000 0.05056 0.05397 = 0.05908 -0.00497 -0.00027 0.00419 ZN2 4 0.996082 0.168179 -0.181432 11.00000 0.04784 0.05640 = 0.05689 0.00160 -0.00526 0.00121 N4 3 0.940086 0.304968 0.223590 11.00000 0.06628 0.05660 = 0.05897 -0.00017 -0.00853 -0.00433 N6 3 0.561022 0.232848 0.144091 11.00000 0.04766 0.06248 = 0.07078 -0.00637 0.00395 -0.00072 N2 3 0.837362 0.032844 0.155066 11.00000 0.05930 0.05604 = 0.06717 0.00347 0.00746 0.00863 N1 3 0.920109 -0.074578 0.190816 11.00000 0.05827 0.05394 = 0.06398 0.00558 0.00558 0.00386 N5 3 0.677586 0.157422 0.113583 11.00000 0.05046 0.05488 = 0.07157 -0.00945 0.00480 0.00160 N3 3 0.865765 0.231656 0.141226 11.00000 0.06557 0.05579 = 0.05535 -0.00013 -0.00825 -0.00321 C3 1 0.902045 -0.018412 0.139505 11.00000 0.06518 0.06388 = 0.06042 0.00664 0.01236 0.01207 AFIX 43 H3 2 0.932473 -0.015015 0.095601 11.00000 -1.20000 AFIX 0 C7 1 0.646667 0.229799 0.139607 11.00000 0.04878 0.05638 = 0.06775 -0.00507 0.00168 -0.00135 AFIX 43 H7 2 0.681627 0.274589 0.153538 11.00000 -1.20000 AFIX 0 C5 1 0.923062 0.354526 0.165663 11.00000 10.10070 0.06494 = 0.09633 0.01554 -0.03592 -0.01879 AFIX 43 H5 2 0.939765 0.410613 0.160762 11.00000 -1.20000 AFIX 0 C1 1 0.813092 0.006560 0.223118 11.00000 0.10290 0.09417 = 0.10110 0.02155 0.05337 0.03720 AFIX 43 H1 2 0.768740 0.029659 0.250745 11.00000 -1.20000 AFIX 0 C4 1 0.905143 0.231769 0.205816 11.00000 0.06929 0.05739 = 0.05994 0.00764 -0.00885 -0.00587 AFIX 43 H4 2 0.907945 0.184442 0.236016 11.00000 -1.20000 AFIX 0 C2 1 0.863353 -0.058225 0.244316 11.00000 0.11642 0.09143 = 0.08460 0.03317 0.04205 0.03554 AFIX 43 H2 2 0.859313 -0.086922 0.288831 11.00000 -1.20000 AFIX 0 C6 1 0.878075 0.310398 0.115815 11.00000 10.10859 0.07277 = 0.08789 0.02153 -0.04430 -0.01860 AFIX 43 H6 2 0.858566 0.331010 0.070916 11.00000 -1.20000 AFIX 0 PART 1 C14A 1 0.902183 0.145360 -0.038674 11.00000 0.05051 0.07773 = 0.06371 -0.00205 -0.01095 0.00013 AFIX 43 H14A 2 0.949410 0.163864 -0.011948 11.00000 -1.20000 AFIX 0 N7A 3 0.829545 0.124125 -0.006669 -31.00000 0.05513 0.08417 = 0.05969 -0.01181 0.00094 -0.01097 N8A 3 0.903673 0.138723 -0.110881 -31.00000 0.05141 0.08519 = 0.05461 -0.00797 -0.00233 -0.01081 C16A 1 0.775857 0.109913 -0.066004 -31.00000 0.05910 0.14725 = 0.07614 -0.01353 -0.00569 -0.03085 AFIX 43 H16A 2 0.717870 0.096732 -0.063264 -31.00000 -1.20000 AFIX 0 C15A 1 0.821709 0.118378 -0.128438 -31.00000 0.06732 0.14465 = 0.05926 -0.01439 -0.00529 -0.03499 AFIX 43 H15A 2 0.800575 0.111399 -0.175902 -31.00000 -1.20000 AFIX 0 C9A 1 0.534643 0.158996 0.113414 -21.00000 0.05702 0.07209 = 0.11397 -0.02429 0.01032 -0.00997 AFIX 43 H9A 2 0.478112 0.143255 0.104796 -21.00000 -1.20000 AFIX 0 C8A 1 0.606337 0.111441 0.097281 -21.00000 0.06135 0.06266 = 0.13085 -0.03220 0.00730 -0.00538 AFIX 43 H8A 2 0.606036 0.056881 0.078358 -21.00000 -1.20000 AFIX 0 PART 2 C14B 1 10.872523 10.173795 9.948886 31.00000 10.06477 AFIX 43 H14B 2 0.880502 0.230783 -0.040846 31.00000 -1.20000 AFIX 0 N7B 3 0.829545 0.124125 -0.006669 31.00000 0.05513 0.08417 = 0.05969 -0.01181 0.00094 -0.01097 N8B 3 0.903673 0.138723 -0.110881 31.00000 0.05141 0.08519 = 0.05461 -0.00797 -0.00233 -0.01081 AFIX 66 C16B 1 0.834337 0.039529 -0.035448 31.00000 0.06599 C17 1 0.798964 -0.038304 -0.017372 31.00000 0.06894 AFIX 43 H17 2 0.769539 -0.044936 0.026756 31.00000 -1.20000 AFIX 65 C18 1 0.807570 -0.106224 -0.065250 31.00000 10.09375 AFIX 43 H18 2 0.783903 -0.158300 -0.053156 31.00000 -1.20000 AFIX 65 C19 1 0.851548 -0.096312 -0.131205 31.00000 10.09601 AFIX 43 H19 2 0.857305 -0.141756 -0.163238 31.00000 -1.20000 AFIX 65 C20 1 0.886922 -0.018480 -0.149282 31.00000 10.09715 AFIX 43 H20 2 0.916346 -0.011848 -0.193410 31.00000 -1.20000 AFIX 65 C15B 1 0.878317 0.049441 -0.101404 31.00000 0.08034 AFIX 0 C9B 1 0.534643 0.158996 0.113414 21.00000 0.05702 0.07209 = 0.11397 -0.02429 0.01032 -0.00997 C8B 1 0.606337 0.111441 0.097281 21.00000 0.06135 0.06266 = 0.13085 -0.03220 0.00730 -0.00538 C10 1 0.449897 0.132156 0.095349 21.00000 0.06782 AFIX 43 H10 2 0.401920 0.164717 0.106134 21.00000 -1.20000 AFIX 0 C13 1 0.595733 0.036022 0.052981 21.00000 0.06706 AFIX 43 H13 2 0.643253 0.008288 0.033756 21.00000 -1.20000 AFIX 0 C12 1 0.515465 0.006412 0.039929 21.00000 0.07691 C11 1 0.443777 0.055047 0.060969 21.00000 0.08102 AFIX 43 H11 2 0.389436 0.033796 0.051046 21.00000 -1.20000 AFIX 0 PART 3 C1S 1 0.858914 -0.184356 -0.048395 41.00000 10.20318 AFIX 13 H1S 2 0.881057 -0.233236 -0.021339 41.00000 -1.20000 AFIX 0 O1S 5 0.913553 -0.081808 -0.057374 41.00000 10.20318 AFIX 83 H1S1 2 0.964610 -0.089598 -0.065601 41.00000 -1.50000 AFIX 0 C2S 1 0.779071 -0.144206 -0.035090 41.00000 10.20318 AFIX 33 H2S1 2 0.769457 -0.140377 0.016984 41.00000 -1.50000 H2S2 2 0.779830 -0.088526 -0.055961 41.00000 -1.50000 H2S3 2 0.733931 -0.176563 -0.057293 41.00000 -1.50000 AFIX 0 C3S 1 0.848812 -0.177248 -0.148524 41.00000 10.20318 AFIX 33 H3S1 2 0.898395 -0.201893 -0.171252 41.00000 -1.50000 H3S2 2 0.798422 -0.207079 -0.164093 41.00000 -1.50000 H3S3 2 0.844320 -0.119043 -0.162761 41.00000 -1.50000 AFIX 0 PART 4 C2SB 1 0.899480 -0.109246 -0.163063 51.00000 10.25549 AFIX 33 H2S4 2 0.953866 -0.083165 -0.153420 51.00000 -1.50000 H2S5 2 0.908326 -0.162004 -0.187943 51.00000 -1.50000 H2S6 2 0.865533 -0.072674 -0.193478 51.00000 -1.50000 AFIX 0 C1SB 1 0.854184 -0.124552 -0.092447 51.00000 10.25549 AFIX 13 H1SB 2 0.853966 -0.084292 -0.051494 51.00000 -1.20000 AFIX 0 O1SB 5 0.897981 -0.231815 -0.085552 51.00000 10.25549 AFIX 83 H1S2 2 0.932807 -0.239459 -0.118680 51.00000 -1.50000 AFIX 0 C3SB 1 0.761122 -0.170765 -0.128355 51.00000 10.25549 AFIX 33 H3S4 2 0.723082 -0.185230 -0.088798 51.00000 -1.50000 H3S5 2 0.733254 -0.131526 -0.160738 51.00000 -1.50000 H3S6 2 0.776047 -0.220856 -0.155202 51.00000 -1.50000 AFIX 0 PART 2 H12 2 10.506450 9.947392 10.006200 21.00000 0.09637 HKLF 4 REM CF solution in Pbca REM wR2 = 0.1374, GooF = S = 1.054, Restrained GooF = 1.505 for all data REM R1 = 0.0450 for 3287 Fo > 4sig(Fo) and 0.0503 for all 3732 data REM 251 parameters refined using 34 restraints END WGHT 0.0809 3.3026 REM Highest difference peak 0.576, deepest hole -0.462, 1-sigma level 0.069 Q1 1 0.8627 -0.1533 -0.0898 11.00000 0.05 0.58 Q2 1 0.8003 -0.1353 -0.0979 11.00000 0.05 0.41 Q3 1 0.5455 0.1366 0.1564 11.00000 0.05 0.38 Q4 1 0.8405 -0.1327 -0.0390 11.00000 0.05 0.35 Q5 1 0.8412 0.0116 -0.0355 11.00000 0.05 0.34 Q6 1 0.8845 0.0197 -0.1024 11.00000 0.05 0.34 Q7 1 0.4777 0.0279 0.0401 11.00000 0.05 0.32 Q8 1 0.8787 0.3615 0.1753 11.00000 0.05 0.31 Q9 1 0.8019 -0.0701 -0.0155 11.00000 0.05 0.31 Q10 1 0.8344 0.3156 0.1266 11.00000 0.05 0.29 Q11 1 0.9717 0.3453 0.1542 11.00000 0.05 0.28 Q12 1 0.6204 0.0954 0.1490 11.00000 0.05 0.28 Q13 1 0.9259 0.3042 0.1071 11.00000 0.05 0.28 Q14 1 0.8733 -0.1269 -0.1737 11.00000 0.05 0.24 Q15 1 0.5337 0.0117 0.0165 11.00000 0.05 0.24 Q16 1 0.8645 0.2341 0.1170 11.00000 0.05 0.24 Q17 1 0.8561 0.0334 0.1816 11.00000 0.05 0.21 Q18 1 1.0189 0.1647 -0.1420 11.00000 0.05 0.20 Q19 1 0.6195 0.0384 0.0965 11.00000 0.05 0.20 Q20 1 0.5617 0.2355 0.1240 11.00000 0.05 0.20 ; _shelx_res_checksum 66443 _shelx_hkl_file ; 0 0 1 41.9653 13.8067 1 0 0 -1 44.6902 13.8002 1 0 0 2 27728.1 371.224 1 0 0 -2 27993.5 375.297 1 0 0 -3 54.2973 31.0624 1 0 0 -4 999999. 3172.11 1 0 0 -5 137.809 51.1377 1 0 0 -6 1708.28 166.683 1 0 0 -6 1742.71 107.243 19 0 0 -6 1760.93 96.3619 15 0 0 -7 36.8260 29.0568 1 0 0 -7 30.7052 23.7179 15 0 0 -7 40.5434 30.7867 19 0 0 -8 1749.08 113.084 15 0 0 -9-54.4089 34.9737 15 0 0 -10 67901.5 803.191 15 0 0 -11-32.6001 40.1427 15 0 0 -12 2957.67 190.179 15 0 0 -13-11.9886 30.4046 15 0 0 -14 43785.3 800.365 15 0 0 -15-15.5284 51.4815 17 0 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319.198 4 -11 -9 -6 68.0314 63.8990 4 11 9 -6-0.54478 44.7621 13 -11 9 -6 6.57839 52.8037 2 -11 -9 -7 558.262 118.927 4 11 9 -7 553.060 108.260 13 -11 9 -7 573.330 107.425 2 -11 9 -8 1912.10 191.117 2 11 9 -8 2142.15 194.104 13 -11 -9 -8 1924.94 209.449 4 -11 9 -9 5564.21 313.057 2 11 9 -9 4647.16 284.020 7 -11 -9 -9 4992.20 324.908 4 -11 -9 -10 464.338 107.290 4 11 9 -10 470.964 94.7853 7 -11 9 -10 573.362 99.0689 2 11 9 -11 3512.02 228.201 7 -11 -9 -11 4008.42 266.149 4 -11 -9 -12 310.527 73.3831 4 11 9 -12 326.976 72.1033 7 11 9 -13 905.155 99.0901 7 -11 -9 -13 902.473 108.145 4 11 10 0-26.0763 70.6328 13 11 10 1 432.390 96.5617 13 11 10 -1 425.980 102.881 13 -11 10 -1 483.484 109.282 2 11 10 -2-27.6630 65.6155 13 -11 10 -2-11.8380 66.7390 2 11 10 -3 603.993 119.183 13 -11 10 -3 444.062 103.983 2 -11 10 -4 1456.14 174.335 2 -11 -10 -4 1201.06 157.966 4 11 10 -4 1413.96 171.809 13 -11 10 -5 9623.40 439.384 2 11 10 -5 9789.58 435.755 13 -11 -10 -5 9235.01 441.798 4 -11 -10 -6 0.40563 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513.936 113.037 2 13 4 -4 379.957 90.1767 13 13 -4 4 572.523 108.340 12 -13 -4 -4 224.776 86.2347 4 -13 4 -5 941.395 138.544 2 13 4 -5 990.270 136.541 13 13 -4 5 1202.92 150.929 12 13 4 -5 1000.91 167.402 18 -13 -4 -5 1071.92 148.698 4 13 4 -6 121.469 51.6940 13 -13 4 -6 51.8049 56.4142 2 13 4 -6 47.3622 61.0770 18 -13 -4 -6 23.2473 64.0046 4 13 4 -7 268.301 73.9964 7 13 4 -7 196.350 66.3956 13 -13 4 -7 285.365 87.4490 2 13 4 -7 347.662 111.416 18 -13 -4 -7 234.938 76.1118 2 -13 -4 -7 270.894 89.2639 4 13 4 -8 495.173 99.3447 7 13 4 -8 475.880 95.2194 13 -13 4 -8 479.559 106.555 2 13 4 -8 518.781 120.845 18 -13 -4 -8 480.587 109.889 2 -13 -4 -8 528.487 116.044 4 13 4 -9 23.5111 37.6453 7 -13 4 -9-11.6328 55.0187 2 13 4 -9 18.2108 60.3408 18 -13 -4 -9-23.4029 68.3231 2 -13 -4 -9 49.7806 51.8508 4 13 4 -10 72.9435 57.6095 7 -13 4 -10-22.5674 51.4869 2 13 4 -10 42.0364 63.1979 18 -13 -4 -10-7.14205 52.8525 2 -13 -4 -10 44.2412 42.7962 4 13 4 -11 290.634 70.0530 7 -13 4 -11 242.351 73.5021 2 -13 -4 -11 227.559 76.5570 2 -13 4 -12 1698.92 167.710 2 -13 -4 -12 1829.83 179.832 2 -13 -4 -12 1843.46 178.770 17 -13 4 -13 447.385 80.3607 2 -13 -4 -13 581.662 98.4730 2 -13 -4 -13 358.720 77.6334 17 -13 -4 -14 163.990 52.7727 2 13 5 0-24.3300 49.7851 13 13 5 1 1641.53 170.971 13 13 5 -1 1491.24 167.569 13 13 -5 1 1579.60 180.700 12 -13 5 -2 12306.9 485.155 2 13 5 2 12918.1 468.625 13 13 5 -2 12390.1 480.176 13 13 -5 2 12453.5 483.962 12 -13 -5 -2 11781.7 471.134 4 -13 5 -3 3212.56 251.161 2 13 5 -3 3339.42 250.611 13 13 -5 3 3022.24 236.447 12 -13 -5 -3 3093.97 248.549 4 -13 5 -4 764.539 123.460 2 13 5 -4 647.902 112.270 13 13 -5 4 584.741 107.618 12 -13 -5 -4 584.930 116.717 4 -13 5 -5 22.9873 52.6201 2 13 5 -5 15.1473 49.2797 13 13 5 -5-12.3288 60.9429 18 -13 -5 -5-43.0448 58.8463 4 13 5 -6 325.357 79.8898 7 -13 5 -6 147.847 61.7295 2 13 5 -6 282.531 78.8546 13 13 5 -6 377.547 108.071 18 -13 -5 -6 351.632 98.0970 4 13 5 -7-23.5933 53.7442 7 -13 5 -7 102.841 59.1893 2 13 5 -7 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173.987 72.1013 2 -13 6 -3 48.8942 52.3064 2 13 6 -3 61.0738 50.1337 13 -13 -6 -3 114.966 64.6852 4 -13 6 -4 135.471 65.7243 2 13 6 -4 202.760 77.3111 13 13 6 -4 123.054 54.6375 18 -13 -6 -4 187.507 80.4882 4 -13 6 -5 108.055 59.6782 2 13 6 -5 8.35704 47.0088 7 13 6 -5 102.412 56.8683 13 13 6 -5 48.1871 56.3990 18 -13 -6 -5 31.3338 49.7415 4 13 6 -6 3602.40 246.594 7 -13 6 -6 3559.60 266.286 2 13 6 -6 3125.27 234.991 13 13 6 -6 3655.13 294.904 18 -13 -6 -6 3388.23 273.606 4 13 6 -7 3952.67 259.248 7 -13 6 -7 3967.11 278.539 2 13 6 -7 3787.23 250.326 13 13 6 -7 4153.18 308.542 18 -13 -6 -7 3529.36 275.172 4 -13 6 -8 219.938 78.7849 2 13 6 -8 272.122 77.8779 7 13 6 -8 234.848 67.6121 13 13 6 -8 212.793 85.4098 18 -13 -6 -8 255.711 83.1022 4 -13 6 -9 143.010 65.5552 2 13 6 -9 117.466 54.1349 7 13 6 -9 88.5435 66.6493 18 -13 -6 -9 160.629 69.0230 4 13 6 -10 1427.87 146.514 7 -13 6 -10 1349.98 152.713 2 -13 -6 -10 1202.06 151.380 2 -13 -6 -10 1158.20 150.882 4 -13 6 -11 465.200 89.3190 2 13 6 -11 416.056 83.3047 7 -13 -6 -11 279.698 79.5067 2 -13 -6 -11 334.353 78.8407 4 -13 6 -12 994.182 116.494 2 13 6 -12 1024.09 116.108 7 -13 -6 -12 1048.33 131.409 2 -13 -6 -13 87.9883 48.3801 2 13 7 0-16.8163 43.6245 13 -13 7 0-10.9206 49.5702 2 13 7 1 1491.29 164.492 13 13 7 -1 1346.54 168.508 13 -13 7 -1 1249.39 158.659 2 13 7 -2 148.040 49.6842 13 -13 7 -2 190.396 74.0940 2 13 7 -3 133.918 63.7622 13 13 7 -3 117.397 50.9326 18 -13 7 -3 63.7322 50.7824 2 -13 -7 -3 152.061 69.9824 4 -13 7 -4 7287.36 380.485 2 13 7 -4 7077.55 367.696 13 13 7 -4 7849.82 411.507 18 -13 -7 -4 7034.97 377.378 4 -13 7 -5 5247.95 322.549 2 13 7 -5 4807.82 284.296 7 13 7 -5 5214.76 309.266 13 13 7 -5 5628.70 348.506 18 -13 -7 -5 4808.46 313.272 4 -13 7 -6 3659.43 270.689 2 13 7 -6 3507.66 245.709 7 13 7 -6 3615.78 253.558 13 13 7 -6 3767.00 283.516 18 -13 -7 -6 3556.75 268.389 4 -13 -7 -7 1211.39 158.709 4 -13 7 -7 1057.77 145.414 2 13 7 -7 980.792 133.022 7 13 7 -7 846.863 120.850 13 13 7 -7 1212.95 163.124 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1493.57 157.652 7 13 8 -6 1789.11 176.838 13 -13 -8 -6 1507.02 175.536 4 -13 -8 -7 698.304 119.301 4 13 8 -7 738.303 109.973 7 13 8 -7 798.975 117.500 13 -13 8 -7 851.445 133.776 2 -13 -8 -8 115.085 55.6175 4 13 8 -8 69.2758 42.5664 7 13 8 -8 80.9127 40.9923 13 -13 8 -8 64.0524 44.3889 2 13 8 -9 499.677 86.4704 7 -13 8 -9 734.651 111.678 2 -13 -8 -9 607.294 104.053 4 13 8 -10 247.618 60.8032 7 -13 8 -10 95.4305 40.6579 2 -13 -8 -10 268.917 69.9870 4 13 8 -11 53.5812 29.3044 7 -13 8 -11 31.0877 35.8759 2 -13 -8 -11-37.8584 36.0607 2 -13 -8 -11-82.5645 49.9416 4 13 9 0-4.13646 49.8987 13 13 9 1 1928.59 189.343 13 13 9 -1 1779.46 183.049 13 -13 9 -1 2020.44 194.338 2 13 9 -2 1060.47 141.513 13 -13 9 -2 1194.73 154.732 2 13 9 -3 9933.43 425.649 13 -13 9 -3 9450.89 417.577 2 -13 9 -4 2871.48 232.140 2 13 9 -4 2836.81 225.775 13 -13 -9 -4 2446.08 213.599 4 -13 9 -5 2029.47 193.934 2 13 9 -5 1842.28 179.009 13 -13 -9 -5 1944.79 189.594 4 -13 -9 -6 619.056 111.865 4 13 9 -6 667.591 108.033 7 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441.484 12 14 0 -3-49.0440 45.9507 13 14 0 -3-32.9770 57.2203 12 14 0 3 68.8653 60.3044 12 14 0 -4 230.939 75.1828 13 14 0 -4 309.748 90.8087 12 14 0 4 120.201 57.5668 12 14 0 -5 105.537 70.2998 13 14 0 5 14.9394 49.1955 12 -14 0 -5 74.3284 61.3811 2 14 0 -5 129.812 90.4320 18 14 0 -6 6832.04 335.239 13 -14 0 -6 6549.71 346.620 2 14 0 6 6678.93 336.882 12 14 0 -6 6252.12 398.170 18 14 0 -7 56.7335 65.7489 18 -14 0 -7-36.8324 43.1660 2 -14 0 -8 11597.9 464.424 2 14 0 -8 11012.5 516.837 18 14 0 -9-11.3698 64.7426 18 -14 0 -9 75.3495 63.8985 2 14 0 -10 18.8504 63.9165 18 -14 0 -10 84.0988 47.7182 2 -14 0 -11 21.9484 49.6597 2 -14 0 -12 1765.48 163.082 2 -14 0 -12 1858.98 179.005 17 -14 0 -13-13.5083 31.9211 2 -14 0 -13 77.8762 51.0319 17 14 1 0 1042.92 135.260 13 14 -1 0 1033.63 141.545 12 14 1 0 965.417 139.846 12 14 1 1 2189.06 193.519 13 14 1 -1 2514.39 209.672 13 14 -1 -1 2326.54 210.800 12 14 -1 1 2369.37 208.321 12 14 1 -1 2374.90 207.966 12 14 1 1 2475.58 215.148 12 14 1 2 886.779 122.605 13 14 1 -2 763.296 118.758 13 14 -1 -2 751.609 123.272 12 14 -1 2 761.673 121.171 12 14 1 -2 934.204 131.502 12 14 1 2 1075.91 143.482 12 14 1 -3 7628.78 363.483 13 14 -1 -3 6887.51 349.938 12 14 -1 3 7368.36 365.044 12 14 1 -3 7085.17 349.263 12 14 1 3 7389.14 365.553 12 14 1 -4 3117.23 229.693 13 14 -1 -4 2971.12 227.815 12 14 -1 4 3016.34 233.274 12 14 1 4 3114.46 235.371 12 14 1 -5 1216.51 147.047 13 -14 1 -5 1215.25 154.859 2 14 -1 5 1144.80 144.757 12 14 1 5 1173.24 146.973 12 14 -1 -5 1207.34 176.190 18 14 1 -5 985.224 164.505 18 14 1 -6 8458.58 373.804 13 -14 1 -6 8720.93 405.365 2 -14 -1 -6 8608.28 395.467 2 14 -1 6 8685.40 380.550 12 14 1 6 8373.15 379.854 12 14 -1 -6 8523.70 455.609 18 14 1 -6 8020.59 454.431 18 14 1 -7 1952.42 180.381 13 -14 1 -7 2038.48 198.462 2 -14 -1 -7 1951.58 193.110 2 14 1 7 1927.10 178.827 12 14 -1 -7 2043.29 225.336 18 14 1 -7 1900.47 224.019 18 14 1 -8 1418.97 148.605 13 -14 1 -8 1528.81 172.275 2 -14 -1 -8 1590.36 180.131 2 14 -1 -8 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924.430 131.392 13 -14 2 -4 1103.93 147.494 2 14 -2 -4 1108.89 145.416 12 14 -2 4 1092.42 142.120 12 14 2 -5 1483.47 158.904 13 -14 2 -5 1432.00 167.863 2 14 -2 5 1360.13 158.740 12 14 2 -5 1544.91 209.031 18 14 2 -6 3344.13 235.486 13 -14 2 -6 3289.68 246.974 2 14 -2 6 3553.49 242.195 12 14 2 -6 3151.45 290.127 18 14 2 -7 4498.09 266.647 13 -14 2 -7 4567.84 292.010 2 -14 -2 -7 4472.90 287.607 2 14 2 -7 4253.70 330.608 18 -14 -2 -8 216.084 78.9196 2 14 2 -8 205.114 63.7647 13 -14 2 -8 185.370 76.1351 2 14 2 -8 195.908 84.8713 18 -14 2 -9 3813.36 262.452 2 -14 -2 -9 3754.04 259.966 2 14 2 -9 3616.74 294.886 18 -14 -2 -10 342.835 82.8456 2 -14 2 -10 231.044 70.7159 2 14 2 -10 323.748 89.2054 18 -14 2 -11 91.5048 54.0379 2 -14 2 -11 77.4523 55.8212 17 -14 -2 -11 122.017 58.2358 2 -14 2 -12 41.3752 37.8200 2 -14 2 -12 42.7057 45.0421 17 -14 -2 -12 236.626 77.8662 17 -14 -2 -12 160.334 58.9586 2 -14 2 -13 682.294 93.4125 2 -14 -2 -13 494.132 83.6260 2 -14 2 -13 490.193 85.0226 17 -14 -2 -13 680.143 100.985 17 14 3 0 2257.58 197.597 13 14 -3 0 1863.93 190.514 12 14 3 1 8009.43 367.409 13 14 3 -1 8130.12 378.187 13 14 -3 -1 7915.44 385.268 12 14 -3 1 8805.34 404.164 12 14 3 2 36.6552 43.0813 13 14 3 -2 62.2665 56.7642 13 14 -3 -2 75.4450 61.1959 12 14 -3 2 39.7378 49.0884 12 -14 3 -3 11112.7 450.577 2 14 3 -3 10975.2 439.299 13 14 -3 -3 11196.5 451.549 12 14 -3 3 11205.4 451.899 12 14 3 -3 11551.0 440.712 12 14 3 -4 2089.07 195.723 13 -14 3 -4 2070.44 197.912 2 14 -3 4 2119.34 195.891 12 14 3 -5 1478.94 162.830 13 -14 3 -5 1304.35 157.825 2 14 -3 5 1581.37 165.383 12 14 3 -5 1494.07 201.848 18 14 3 -6 1627.68 166.071 13 -14 3 -6 1528.96 172.198 2 14 3 -6 1611.64 203.899 18 -14 -3 -7 972.381 134.897 2 14 3 -7 978.862 127.182 13 -14 3 -7 918.236 138.269 2 14 3 -7 875.236 156.491 18 14 3 -8-11.9928 47.5111 7 -14 -3 -8 115.597 60.6026 2 14 3 -8 178.453 60.2580 13 -14 3 -8 72.8030 53.5355 2 14 3 -8 102.638 80.3994 18 14 3 -9 1656.80 157.855 7 -14 3 -9 1713.36 176.536 2 -14 -3 -9 1899.25 185.550 2 14 3 -9 1806.30 209.550 18 -14 3 -10 2164.57 190.714 2 -14 -3 -10 1973.68 184.176 2 14 3 -10 1983.69 208.308 18 -14 -3 -11 105.623 48.7052 2 -14 3 -11 114.059 55.1340 2 -14 3 -11 146.201 57.7274 17 -14 -3 -11 301.781 81.3786 17 -14 3 -12 10.5266 36.7513 2 -14 3 -12 60.0888 47.8437 17 -14 -3 -12-0.57480 47.4694 17 -14 -3 -12 36.7926 46.4149 2 -14 3 -13 3977.84 215.888 2 -14 -3 -13 3997.35 225.662 2 -14 -3 -13 4230.98 235.546 17 14 4 0 112.828 62.5776 13 14 -4 0-23.3985 59.1846 12 14 4 1 5437.17 305.472 13 14 4 -1 4877.11 293.404 13 14 -4 -1 5125.06 313.418 12 14 -4 1 4843.81 304.130 12 14 4 2 2080.74 189.466 13 14 4 -2 2167.22 199.995 13 14 -4 2 2063.40 200.129 12 -14 4 -3 370.494 86.8109 2 14 4 -3 526.667 105.259 13 14 -4 3 545.967 103.723 12 -14 4 -4 389.404 96.3129 2 14 4 -4 449.692 101.888 13 14 -4 4 361.241 91.0195 12 -14 -4 -4 515.250 109.911 4 -14 4 -5 1860.77 190.842 2 14 4 -5 1941.81 186.635 13 14 -4 5 1918.12 183.008 12 14 4 -5 1995.69 226.865 18 -14 -4 -5 2032.31 206.557 4 -14 4 -6-6.28332 48.6526 2 14 4 -6 50.4768 61.8049 13 -14 -4 -6 22.8978 53.9838 4 14 4 -6 122.591 83.0990 18 -14 4 -7 1914.80 188.859 2 14 4 -7 2483.89 197.620 13 14 4 -7 2496.50 247.051 18 -14 -4 -7 2379.99 218.108 4 14 4 -8 4447.18 256.307 7 14 4 -8 4352.65 250.860 13 -14 4 -8 4424.20 284.637 2 -14 -4 -8 4156.38 269.171 2 14 4 -8 4785.46 333.827 18 14 4 -9 2153.98 174.880 7 -14 4 -9 2110.76 192.484 2 -14 -4 -9 1804.06 177.455 2 14 4 -9 2181.09 221.645 18 14 4 -10 391.897 77.9897 7 -14 4 -10 545.578 103.387 2 -14 -4 -10 361.121 91.6941 2 -14 4 -11 88.4256 53.4141 2 -14 -4 -11 151.170 56.7496 2 -14 -4 -11 122.076 44.4385 17 -14 -4 -12 406.703 81.3097 2 -14 4 -12 517.821 88.7869 2 -14 -4 -12 622.495 100.516 17 14 5 0 1659.38 174.432 13 14 5 1 840.925 127.375 13 14 5 -1 1004.06 134.854 13 14 5 2 312.251 76.8495 13 14 5 -2 216.600 71.3882 13 -14 5 -2 350.250 92.1698 2 -14 5 -3 2776.86 230.959 2 14 5 -3 3068.33 234.957 13 -14 -5 -3 2841.32 232.865 4 -14 5 -4 3251.41 249.425 2 14 5 -4 3277.66 244.434 13 14 5 -4 3319.12 286.422 18 -14 -5 -4 3358.36 257.612 4 -14 5 -5-1.79833 51.4583 2 14 5 -5 72.4144 52.1565 13 14 5 -5-31.2253 65.0057 18 -14 -5 -5 42.7007 60.5127 4 -14 5 -6 5647.47 324.958 2 14 5 -6 5927.70 312.207 13 14 5 -6 6401.39 389.746 18 -14 -5 -6 6235.99 349.310 4 14 5 -7 2907.27 209.777 7 -14 5 -7 3030.63 235.215 2 14 5 -7 2743.49 208.240 13 14 5 -7 3288.95 276.095 18 -14 -5 -7 3009.29 244.821 4 14 5 -8 1779.29 162.673 7 -14 5 -8 1857.56 184.197 2 14 5 -8 1689.23 158.546 13 14 5 -8 2002.34 213.035 18 -14 -5 -8 1757.48 184.290 4 -14 5 -9 33.0882 42.9385 2 14 5 -9 66.4607 40.7842 7 -14 -5 -9 79.5252 46.4478 2 14 5 -9 87.8158 58.7010 18 14 5 -10 2360.87 177.287 7 -14 5 -10 2089.37 179.450 2 -14 -5 -10 2134.11 184.366 2 -14 5 -11 176.674 54.6979 2 -14 -5 -11 236.789 62.9733 2 -14 -5 -11 313.598 75.3511 17 -14 5 -12 276.626 64.4267 2 -14 -5 -12 183.148 50.5069 2 14 6 0 494.142 102.056 13 14 6 1 189.997 58.4841 13 14 6 -1 24.4162 50.7130 13 -14 6 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227.258 12 16 4 -2 481.546 88.5965 13 16 4 -2 499.712 88.5964 12 16 4 2 392.176 86.9352 12 16 4 -3 1350.31 145.460 13 16 4 3 1149.98 141.650 12 16 4 -3 1249.29 168.128 18 16 4 -4 515.656 90.5823 13 16 4 4 562.956 102.789 12 16 4 -4 494.131 110.894 18 16 4 -5 575.035 94.2482 13 16 4 5 469.748 87.5340 12 16 4 -5 577.669 121.790 18 -16 4 -5 561.979 96.2915 2 -16 4 -6 221.676 65.7846 2 16 4 -6 190.117 59.2941 13 16 4 6 207.962 54.5780 12 16 4 -6 354.297 93.5853 18 -16 4 -7 2481.27 187.053 2 16 4 -7 2391.70 166.916 13 16 4 7 2403.75 174.903 12 16 4 -7 2570.76 215.815 18 -16 4 -8 330.125 71.8341 2 16 4 -8 491.184 98.9674 18 16 5 0 6261.27 298.463 13 16 5 0 6140.95 305.793 12 16 5 1 2068.16 170.322 13 16 5 -1 1690.51 157.362 13 16 5 -1 1733.64 163.002 12 16 5 1 1796.06 171.465 12 16 5 -2 306.561 77.3993 13 16 5 -2 274.777 65.6656 12 16 5 -2 246.113 71.0826 18 16 5 -3 982.235 120.453 13 16 5 -3 959.910 145.139 18 -16 5 -4 2453.81 187.050 2 16 5 -4 2759.76 196.964 13 16 5 -4 2740.34 229.623 18 16 5 -5 147.859 55.7812 13 16 5 5 32.6716 39.1689 12 16 5 -5 204.072 77.1539 18 -16 5 -5 80.5452 44.1890 2 16 5 -6 418.404 76.6363 13 16 5 6 303.124 65.2162 12 16 5 -6 430.617 90.6151 18 -16 5 -6 389.208 77.3767 2 16 5 -7 66.7691 32.8190 13 16 5 7 35.0897 30.6718 12 16 5 -7 126.556 54.8317 18 -16 5 -7 40.6694 39.5710 2 16 5 -8 57.5194 46.0572 18 -16 5 -8 119.845 45.8677 2 16 6 0 4050.59 234.316 13 16 6 0 4072.54 241.518 12 16 6 1 1000.85 117.697 13 16 6 -1 951.182 119.558 13 16 6 -1 1124.40 128.580 12 16 6 -1 1121.87 146.569 18 16 6 -2 1928.76 165.874 13 16 6 -2 2145.49 200.040 18 16 6 -3 397.388 75.2580 13 -16 6 -3 292.076 65.7738 2 16 6 -3 419.092 95.2259 18 16 6 -4 53.8397 39.2568 13 16 6 -4 21.4624 48.4396 18 -16 6 -4 5.68125 34.0794 2 16 6 -5 81.3186 36.4134 13 16 6 -5 83.9983 50.0809 18 -16 6 -5 166.028 55.3839 2 16 6 -6 659.933 90.2673 13 16 6 6 388.816 78.1146 12 16 6 -6 644.822 108.461 18 -16 6 -6 454.823 80.7561 2 16 6 -7 117.061 43.2073 13 16 6 -7 126.582 56.8546 18 -16 6 -7 74.5062 33.7703 2 16 7 0-8.15585 34.2211 13 16 7 1 68.3328 44.0177 13 16 7 -1 194.708 55.8102 13 16 7 -1 155.924 52.2287 12 16 7 -1 251.023 70.9667 18 16 7 -2 91.5105 40.9498 13 16 7 -2 159.478 64.4815 18 16 7 -3 3403.18 207.745 13 -16 7 -3 3059.03 195.775 2 16 7 -4 103.206 52.1778 13 -16 7 -4 156.899 54.5407 2 16 7 -4 215.180 69.2464 18 16 7 -5 51.5675 37.5377 13 -16 7 -5 69.4036 43.3522 2 16 7 -5 127.419 50.1928 18 16 8 0 431.335 74.7306 13 16 8 -1 761.196 97.7155 13 16 8 -1 798.121 96.9089 12 16 8 -2 400.378 74.9488 13 16 8 -3 472.286 76.3156 13 16 8 -4 188.501 51.9008 13 17 0 0 35.6078 50.7016 12 17 0 -1 44.1098 42.1321 12 17 0 1-83.4980 45.5102 12 17 0 -2 620.812 99.1045 12 17 0 2 607.878 92.6528 12 17 0 -2 707.039 123.533 18 17 0 3-32.4015 51.8241 12 17 0 -3-32.5315 50.2237 18 17 0 4 3223.13 209.387 12 17 0 -4 3237.35 241.569 18 17 0 5-64.2179 47.1448 12 17 0 -5 95.6940 68.5176 18 17 0 6 238.204 55.4290 12 17 0 -6 197.358 65.5021 18 17 0 -7-58.0126 53.6833 18 17 -1 0 46.4195 43.0104 12 17 1 0 26.0768 37.9508 12 17 -1 -1 260.052 63.8944 12 17 -1 1 328.182 75.2661 12 17 1 -1 291.293 69.0554 12 17 1 1 276.881 75.0996 12 17 -1 2 5315.39 277.691 12 17 1 -2 5579.17 276.565 12 17 1 2 5765.83 288.451 12 17 -1 -2 5432.44 313.294 18 17 1 -2 5292.70 323.636 18 17 1 -3-5.22338 34.1091 12 17 -1 3 49.8527 41.0145 12 17 1 3 132.346 59.5568 12 17 -1 -3 37.0426 46.2086 18 17 1 -3 7.85553 61.6464 18 17 -1 4 713.647 95.0740 12 17 1 4 722.216 103.467 12 17 -1 -4 813.429 124.848 18 17 1 -4 494.274 102.921 18 17 -1 5 2537.78 178.622 12 17 1 5 2599.18 183.048 12 17 -1 -5 2509.47 203.373 18 17 1 -5 2552.45 212.699 18 17 -1 6 191.561 52.2310 12 17 1 6 1.57636 29.7327 12 17 1 -6 214.695 77.1151 18 17 1 -7 51.0340 39.8319 18 17 2 0-55.5315 46.4659 12 17 2 -1 268.473 67.8545 12 17 2 1 214.278 59.4641 12 17 2 -2 48.6098 34.4027 12 17 2 2 51.0005 45.0744 12 17 2 -2 80.5218 51.1161 18 17 2 -3 1043.93 116.688 12 17 2 3 1271.92 133.903 12 17 2 -3 1076.42 150.392 18 17 2 4 213.411 61.1650 12 17 2 -4 244.493 69.0748 18 17 2 5 456.276 78.8631 12 17 2 -5 412.803 96.1687 18 17 2 6 758.697 98.7093 12 17 2 -6 707.678 115.251 18 17 2 -7 16.5397 35.8329 18 17 3 0 25.6575 38.4899 12 17 3 -1 75.7074 51.0801 12 17 3 1 57.8628 43.6381 12 17 3 -2 467.763 83.5496 12 17 3 2 481.952 88.7736 12 17 3 -2 344.598 89.7944 18 17 3 3 1316.36 137.527 12 17 3 -3 1382.97 164.199 18 17 3 4 826.579 109.602 12 17 3 -4 842.272 126.803 18 17 3 5 6235.12 276.676 12 17 3 -5 7010.32 343.984 18 17 3 6 401.359 73.4702 12 17 3 -6 269.989 71.9053 18 17 4 0-20.3925 35.9820 12 17 4 -1 536.459 88.8138 13 17 4 -1 433.909 80.1860 12 17 4 1 452.967 85.0264 12 17 4 -1 442.082 101.183 18 17 4 -2 1060.20 119.493 13 17 4 -2 1036.38 117.441 12 17 4 2 905.638 112.936 12 17 4 -2 1006.75 139.682 18 17 4 -3 908.988 107.812 13 17 4 3 966.091 115.861 12 17 4 -3 1046.67 137.182 18 17 4 4 1360.16 133.637 12 17 4 -4 1519.61 164.409 18 17 4 5 109.337 43.0871 12 17 4 -5 96.1694 56.5603 18 17 4 -6 170.631 61.4648 18 17 5 0-1.91005 32.3273 13 17 5 0-4.02146 32.5192 12 17 5 -1 613.021 87.7158 13 17 5 -1 611.093 88.6849 12 17 5 1 547.281 84.1827 12 17 5 -1 565.564 103.839 18 17 5 -2 3710.80 209.139 13 17 5 2 3877.93 220.975 12 17 5 -2 4232.72 261.835 18 17 5 -3 824.486 98.5331 13 17 5 3 900.088 112.026 12 17 5 -3 955.902 123.514 18 17 5 -4 637.233 87.8006 13 17 5 4 470.537 80.1070 12 17 5 -4 497.796 92.0122 18 17 6 0-14.9993 42.9057 13 17 6 0 12.1299 36.4152 12 17 6 0-69.3970 58.3457 18 17 6 -1 38.9792 27.1806 13 17 6 1 28.8842 33.2794 12 17 6 -1 83.0285 46.0780 18 17 6 1 8.60003 48.6571 18 17 6 -2 123.502 45.5777 13 17 6 2 146.990 49.6559 12 17 6 -3 239.793 59.5009 13 17 6 3 253.008 61.1818 12 18 0 1-15.0535 42.8359 12 18 0 -1-29.3411 49.5646 18 18 0 2 831.546 99.6915 12 18 0 -2 788.312 109.761 18 18 0 3 97.9350 48.2785 12 18 1 0-15.9364 37.6279 12 18 1 -1 437.945 73.1634 12 18 1 1 356.077 66.2262 12 18 1 -1 382.580 89.0341 18 18 1 2 339.288 66.9748 12 18 1 -2 336.804 76.2518 18 18 1 3 86.5020 40.6747 12 18 2 0 275.491 64.0684 12 18 2 0 207.009 65.6048 18 18 2 1 3226.28 191.479 12 18 2 -1 3093.42 219.743 18 18 2 2 602.745 84.7235 12 18 2 -2 701.697 109.187 18 0 0 0 0.00 0.00 0 TITL prexp_452_mlr56 in Pbca REM Pbca (#61 in standard setting) CELL 1.54184 15.605206 15.837368 18.171821 90.0000 90.0000 90.0000 ZERR 17.00 0.000457 0.000594 0.000534 0.0000 0.0000 0.0000 LATT 1 SYMM -x+1/2,-y, z+1/2 SYMM -x, y+1/2,-z+1/2 SYMM x+1/2,-y+1/2,-z SFAC C H N Zn UNIT 170.00 136.00 68.00 17.00 TREF HKLF 4 END ; _shelx_hkl_checksum 61001 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -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 Zn1 Zn 0.80128(3) 0.13394(3) 0.09929(3) 0.05454(19) Uani 1 1 d . . . . . Zn2 Zn 0.99608(3) 0.16818(3) -0.18143(3) 0.05371(19) Uani 1 1 d . . . . . N4 N 0.9401(2) 0.3050(2) 0.22359(17) 0.0606(7) Uani 1 1 d . . . . . N6 N 0.56102(19) 0.2328(2) 0.14409(17) 0.0603(7) Uani 1 1 d . . . . . N2 N 0.8374(2) 0.0328(2) 0.15507(18) 0.0608(7) Uani 1 1 d . . . . . N1 N 0.9201(2) -0.07458(19) 0.19082(16) 0.0587(7) Uani 1 1 d . . . . . N5 N 0.6776(2) 0.1574(2) 0.11358(18) 0.0590(8) Uani 1 1 d . . . . . N3 N 0.8658(2) 0.23166(19) 0.14123(16) 0.0589(7) Uani 1 1 d . . . . . C3 C 0.9020(2) -0.0184(2) 0.1395(2) 0.0632(10) Uani 1 1 d . . . . . H3 H 0.932473 -0.015015 0.095601 0.076 Uiso 1 1 calc R U . . . C7 C 0.6467(2) 0.2298(2) 0.1396(2) 0.0576(9) Uani 1 1 d . . . . . H7 H 0.681627 0.274589 0.153538 0.069 Uiso 1 1 calc R U . . . C5 C 0.9231(4) 0.3545(3) 0.1657(3) 0.0873(12) Uani 1 1 d . . . . . H5 H 0.939765 0.410613 0.160762 0.105 Uiso 1 1 calc R U . . . C1 C 0.8131(4) 0.0066(3) 0.2231(3) 0.0994(18) Uani 1 1 d . . . . . H1 H 0.768740 0.029659 0.250745 0.119 Uiso 1 1 calc R U . . . C4 C 0.9051(3) 0.2318(2) 0.2058(2) 0.0622(9) Uani 1 1 d . . . . . H4 H 0.907945 0.184442 0.236016 0.075 Uiso 1 1 calc R U . . . C2 C 0.8634(4) -0.0582(3) 0.2443(3) 0.0975(17) Uani 1 1 d . . . . . H2 H 0.859313 -0.086922 0.288831 0.117 Uiso 1 1 calc R U . . . C6 C 0.8781(4) 0.3104(3) 0.1158(3) 0.0898(12) Uani 1 1 d . . . . . H6 H 0.858566 0.331010 0.070916 0.108 Uiso 1 1 calc R U . . . C14A C 0.9022(2) 0.1454(3) -0.0387(2) 0.0640(10) Uani 1 1 d . . . A 1 H14A H 0.949410 0.163864 -0.011948 0.077 Uiso 1 1 calc R U . A 1 N7A N 0.8295(2) 0.1241(2) -0.00667(17) 0.0663(9) Uani 0.911(5) 1 d . . P A 1 N8A N 0.9037(2) 0.1387(2) -0.11088(17) 0.0637(8) Uani 0.911(5) 1 d . . P A 1 C16A C 0.7759(3) 0.1099(4) -0.0660(3) 0.0942(19) Uani 0.911(5) 1 d . . P A 1 H16A H 0.717870 0.096732 -0.063264 0.113 Uiso 0.911(5) 1 calc R U P A 1 C15A C 0.8217(3) 0.1184(4) -0.1284(3) 0.0904(19) Uani 0.911(5) 1 d . . P A 1 H15A H 0.800575 0.111399 -0.175902 0.108 Uiso 0.911(5) 1 calc R U P A 1 C9A C 0.5346(3) 0.1590(3) 0.1134(3) 0.0810(13) Uani 0.538(7) 1 d . . P B 1 H9A H 0.478112 0.143255 0.104796 0.097 Uiso 0.538(7) 1 calc R U P B 1 C8A C 0.6063(3) 0.1114(3) 0.0973(3) 0.0850(15) Uani 0.538(7) 1 d . . P B 1 H8A H 0.606036 0.056881 0.078358 0.102 Uiso 0.538(7) 1 calc R U P B 1 C14B C 0.872523 0.173795 -0.051114 0.065 Uiso 0.089(5) 1 d D U P A 2 H14B H 0.880502 0.230783 -0.040846 0.078 Uiso 0.089(5) 1 calc R U P A 2 N7B N 0.8295(2) 0.1241(2) -0.00667(17) 0.0663(9) Uani 0.089(5) 1 d D . P A 2 N8B N 0.9037(2) 0.1387(2) -0.11088(17) 0.0637(8) Uani 0.089(5) 1 d D . P A 2 C16B C 0.8343(18) 0.0395(11) -0.0354(15) 0.066(11) Uiso 0.089(5) 1 d DG . P A 2 C17 C 0.7990(17) -0.0383(16) -0.0174(13) 0.069(12) Uiso 0.089(5) 1 d G . P A 2 H17 H 0.769539 -0.044936 0.026756 0.083 Uiso 0.089(5) 1 calc R U P A 2 C18 C 0.808(2) -0.1062(11) -0.0653(17) 0.094 Uiso 0.089(5) 1 d G U P A 2 H18 H 0.783903 -0.158300 -0.053156 0.113 Uiso 0.089(5) 1 calc R U P A 2 C19 C 0.852(2) -0.0963(14) -0.1312(15) 0.096 Uiso 0.089(5) 1 d G U P A 2 H19 H 0.857305 -0.141756 -0.163238 0.115 Uiso 0.089(5) 1 calc R U P A 2 C20 C 0.8869(19) -0.0185(18) -0.1493(13) 0.097 Uiso 0.089(5) 1 d G U P A 2 H20 H 0.916346 -0.011848 -0.193410 0.117 Uiso 0.089(5) 1 calc R U P A 2 C15B C 0.8783(19) 0.0494(11) -0.1014(17) 0.080(14) Uiso 0.089(5) 1 d DG . P A 2 C9B C 0.5346(3) 0.1590(3) 0.1134(3) 0.0810(13) Uani 0.462(7) 1 d . . P B 2 C8B C 0.6063(3) 0.1114(3) 0.0973(3) 0.0850(15) Uani 0.462(7) 1 d . . P B 2 C10 C 0.4499(6) 0.1322(6) 0.0953(5) 0.068(3) Uiso 0.462(7) 1 d . . P B 2 H10 H 0.401920 0.164717 0.106134 0.081 Uiso 0.462(7) 1 calc R U P B 2 C13 C 0.5957(6) 0.0360(6) 0.0530(5) 0.067(2) Uiso 0.462(7) 1 d . . P B 2 H13 H 0.643253 0.008288 0.033756 0.080 Uiso 0.462(7) 1 calc R U P B 2 C12 C 0.5155(6) 0.0064(7) 0.0399(5) 0.077(3) Uiso 0.462(7) 1 d . . P B 2 C11 C 0.4438(7) 0.0550(7) 0.0610(5) 0.081(3) Uiso 0.462(7) 1 d . . P B 2 H11 H 0.389436 0.033796 0.051046 0.097 Uiso 0.462(7) 1 calc R U P B 2 C1S C 0.8589(17) -0.1844(13) -0.0484(12) 0.203 Uiso 0.423(8) 1 d D U P C 3 H1S H 0.881057 -0.233236 -0.021339 0.244 Uiso 0.423(8) 1 calc R U P C 3 O1S O 0.9136(12) -0.0818(11) -0.0574(9) 0.203 Uiso 0.423(8) 1 d D U P C 3 H1S1 H 0.964610 -0.089598 -0.065601 0.305 Uiso 0.423(8) 1 calc R U P C 3 C2S C 0.7791(16) -0.1442(17) -0.0351(14) 0.203 Uiso 0.423(8) 1 d D U P C 3 H2S1 H 0.769457 -0.140377 0.016984 0.305 Uiso 0.423(8) 1 calc R U P C 3 H2S2 H 0.779830 -0.088526 -0.055961 0.305 Uiso 0.423(8) 1 calc R U P C 3 H2S3 H 0.733931 -0.176563 -0.057293 0.305 Uiso 0.423(8) 1 calc R U P C 3 C3S C 0.8488(19) -0.1772(17) -0.1485(10) 0.203 Uiso 0.423(8) 1 d D U P C 3 H3S1 H 0.898395 -0.201893 -0.171252 0.305 Uiso 0.423(8) 1 calc R U P C 3 H3S2 H 0.798422 -0.207079 -0.164093 0.305 Uiso 0.423(8) 1 calc R U P C 3 H3S3 H 0.844320 -0.119043 -0.162761 0.305 Uiso 0.423(8) 1 calc R U P C 3 C2SB C 0.899(2) -0.109(2) -0.1631(18) 0.255 Uiso 0.404(9) 1 d D U P D 4 H2S4 H 0.953866 -0.083165 -0.153420 0.383 Uiso 0.404(9) 1 calc R U P D 4 H2S5 H 0.908326 -0.162004 -0.187943 0.383 Uiso 0.404(9) 1 calc R U P D 4 H2S6 H 0.865533 -0.072674 -0.193478 0.383 Uiso 0.404(9) 1 calc R U P D 4 C1SB C 0.854(2) -0.1246(16) -0.0924(17) 0.255 Uiso 0.404(9) 1 d D U P D 4 H1SB H 0.853966 -0.084292 -0.051494 0.307 Uiso 0.404(9) 1 calc R U P D 4 O1SB O 0.8980(15) -0.2318(15) -0.0856(13) 0.255 Uiso 0.404(9) 1 d D U P D 4 H1S2 H 0.932807 -0.239459 -0.118680 0.383 Uiso 0.404(9) 1 calc R U P D 4 C3SB C 0.7611(17) -0.171(2) -0.128(2) 0.255 Uiso 0.404(9) 1 d D U P D 4 H3S4 H 0.723082 -0.185230 -0.088798 0.383 Uiso 0.404(9) 1 calc R U P D 4 H3S5 H 0.733254 -0.131526 -0.160738 0.383 Uiso 0.404(9) 1 calc R U P D 4 H3S6 H 0.776047 -0.220856 -0.155202 0.383 Uiso 0.404(9) 1 calc R U P D 4 H12 H 0.506450 -0.052608 0.006200 0.10(3) Uiso 0.462(7) 1 d . . P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0506(3) 0.0540(3) 0.0591(3) -0.0050(2) -0.0003(2) 0.0042(2) Zn2 0.0478(3) 0.0564(3) 0.0569(3) 0.0016(2) -0.00526(19) 0.0012(2) N4 0.0663(18) 0.0566(17) 0.0590(17) -0.0002(14) -0.0085(15) -0.0043(16) N6 0.0477(15) 0.0625(18) 0.0708(19) -0.0064(15) 0.0040(14) -0.0007(14) N2 0.0593(17) 0.0560(17) 0.0672(18) 0.0035(15) 0.0075(15) 0.0086(15) N1 0.0583(17) 0.0539(17) 0.0640(17) 0.0056(14) 0.0056(14) 0.0039(14) N5 0.0505(16) 0.0549(17) 0.0716(19) -0.0094(15) 0.0048(14) 0.0016(14) N3 0.0656(18) 0.0558(17) 0.0554(16) -0.0001(13) -0.0083(14) -0.0032(15) C3 0.065(2) 0.064(2) 0.060(2) 0.0066(18) 0.0124(18) 0.0121(19) C7 0.0488(19) 0.056(2) 0.068(2) -0.0051(17) 0.0017(16) -0.0014(16) C5 0.101 0.065(3) 0.096(3) 0.016(2) -0.036(3) -0.019(2) C1 0.103(4) 0.094(3) 0.101(4) 0.022(3) 0.053(3) 0.037(3) C4 0.069(2) 0.057(2) 0.060(2) 0.0076(17) -0.0089(18) -0.0059(18) C2 0.116(4) 0.091(3) 0.085(3) 0.033(3) 0.042(3) 0.036(3) C6 0.109 0.073(3) 0.088(3) 0.022(2) -0.044(3) -0.019(3) C14A 0.051(2) 0.078(3) 0.064(2) -0.0020(19) -0.0110(18) 0.0001(18) N7A 0.0551(18) 0.084(2) 0.0597(18) -0.0118(16) 0.0009(15) -0.0110(16) N8A 0.0514(17) 0.085(2) 0.0546(17) -0.0080(15) -0.0023(14) -0.0108(15) C16A 0.059(3) 0.147(6) 0.076(3) -0.014(3) -0.006(2) -0.031(3) C15A 0.067(3) 0.145(5) 0.059(3) -0.014(3) -0.005(2) -0.035(3) C9A 0.057(2) 0.072(3) 0.114(4) -0.024(3) 0.010(2) -0.010(2) C8A 0.061(2) 0.063(2) 0.131(4) -0.032(3) 0.007(2) -0.005(2) N7B 0.0551(18) 0.084(2) 0.0597(18) -0.0118(16) 0.0009(15) -0.0110(16) N8B 0.0514(17) 0.085(2) 0.0546(17) -0.0080(15) -0.0023(14) -0.0108(15) C9B 0.057(2) 0.072(3) 0.114(4) -0.024(3) 0.010(2) -0.010(2) C8B 0.061(2) 0.063(2) 0.131(4) -0.032(3) 0.007(2) -0.005(2) 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' 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' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Zn1 N7B 111.80(14) . . ? N2 Zn1 N7A 111.80(14) . . ? N2 Zn1 N5 111.23(13) . . ? N7B Zn1 N5 111.02(13) . . ? N7A Zn1 N5 111.02(13) . . ? N2 Zn1 N3 106.77(13) . . ? N7B Zn1 N3 108.63(13) . . ? N7A Zn1 N3 108.63(13) . . ? N5 Zn1 N3 107.17(13) . . ? N4 Zn2 N1 112.11(13) 8_565 5_755 ? N4 Zn2 N8B 107.02(13) 8_565 . ? N1 Zn2 N8B 111.02(14) 5_755 . ? N4 Zn2 N8A 107.02(13) 8_565 . ? N1 Zn2 N8A 111.02(14) 5_755 . ? N4 Zn2 N6 110.69(13) 8_565 3 ? N1 Zn2 N6 106.42(13) 5_755 3 ? N8A Zn2 N6 109.60(13) . 3 ? C4 N4 C5 103.9(3) . . ? C4 N4 Zn2 125.7(3) . 8_566 ? C5 N4 Zn2 130.3(3) . 8_566 ? C7 N6 C9B 104.2(3) . . ? C7 N6 C9A 104.2(3) . . ? C7 N6 Zn2 123.9(3) . 3_455 ? C9A N6 Zn2 131.7(3) . 3_455 ? C3 N2 C1 102.6(3) . . ? C3 N2 Zn1 127.1(3) . . ? C1 N2 Zn1 129.5(3) . . ? C3 N1 C2 104.0(3) . . ? C3 N1 Zn2 125.7(3) . 5_755 ? C2 N1 Zn2 130.0(3) . 5_755 ? C7 N5 C8B 104.0(3) . . ? C7 N5 C8A 104.0(3) . . ? C7 N5 Zn1 124.1(3) . . ? C8B N5 Zn1 131.8(3) . . ? C8A N5 Zn1 131.8(3) . . ? C4 N3 C6 103.7(3) . . ? C4 N3 Zn1 124.9(3) . . ? C6 N3 Zn1 131.3(3) . . ? N1 C3 N2 115.1(3) . . ? N5 C7 N6 114.5(3) . . ? N4 C5 C6 109.2(4) . . ? C2 C1 N2 109.3(4) . . ? N4 C4 N3 114.2(3) . . ? N1 C2 C1 108.9(4) . . ? C5 C6 N3 109.0(4) . . ? N8A C14A N7A 115.8(3) . . ? C14A N7A C16A 102.6(4) . . ? C14A N7A Zn1 126.9(3) . . ? C16A N7A Zn1 129.4(3) . . ? C14A N8A C15A 103.7(4) . . ? C14A N8A Zn2 129.6(3) . . ? C15A N8A Zn2 126.1(3) . . ? C15A C16A N7A 108.6(4) . . ? C16A C15A N8A 109.0(4) . . ? N6 C9A C8A 108.1(4) . . ? N5 C8A C9A 108.9(4) . . ? N7B C14B N8B 116.4(2) . . ? C14B N7B C16B 107.9(12) . . ? C14B N7B Zn1 131.7(2) . . ? C16B N7B Zn1 115.9(12) . . ? C14B N8B C15B 102.1(12) . . ? C14B N8B Zn2 134.7(2) . . ? C15B N8B Zn2 119.6(12) . . ? C17 C16B C15B 120.0 . . ? C17 C16B N7B 136(2) . . ? C15B C16B N7B 104(2) . . ? C18 C17 C16B 120.0 . . ? C17 C18 C19 120.0 . . ? C20 C19 C18 120.0 . . ? C15B C20 C19 120.0 . . ? C20 C15B C16B 120.0 . . ? C20 C15B N8B 130(2) . . ? C16B C15B N8B 110(2) . . ? N6 C9B C8B 108.1(4) . . ? N6 C9B C10 129.1(5) . . ? C8B C9B C10 122.7(5) . . ? N5 C8B C9B 108.9(4) . . ? N5 C8B C13 130.9(5) . . ? C9B C8B C13 118.4(5) . . ? C11 C10 C9B 115.7(9) . . ? C12 C13 C8B 119.1(8) . . ? C13 C12 C11 119.7(10) . . ? C13 C12 C12 119.9(11) . 5_655 ? C11 C12 C12 94.5(10) . 5_655 ? C10 C11 C12 123.6(10) . . ? C2S C1S C3S 93.8(15) . . ? C2S C1S O1S 91.5(14) . . ? C3S C1S O1S 84.1(11) . . ? C2SB C1SB C3SB 98.1(18) . . ? C2SB C1SB O1SB 91.9(15) . . ? C3SB C1SB O1SB 87.0(13) . . ? 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 N2 1.977(3) . ? Zn1 N7B 1.981(3) . ? Zn1 N7A 1.981(3) . ? Zn1 N5 1.983(3) . ? Zn1 N3 1.997(3) . ? Zn2 N4 1.981(3) 8_565 ? Zn2 N1 1.984(3) 5_755 ? Zn2 N8B 1.985(3) . ? Zn2 N8A 1.985(3) . ? Zn2 N6 1.986(3) 3 ? N4 C4 1.321(5) . ? N4 C5 1.340(5) . ? N6 C7 1.340(5) . ? N6 C9B 1.359(5) . ? N6 C9A 1.359(5) . ? N2 C3 1.326(5) . ? N2 C1 1.359(6) . ? N1 C3 1.319(5) . ? N1 C2 1.340(5) . ? N5 C7 1.331(5) . ? N5 C8B 1.362(6) . ? N5 C8A 1.362(6) . ? N3 C4 1.325(5) . ? N3 C6 1.344(6) . ? C5 C6 1.342(6) . ? C1 C2 1.348(7) . ? C14A N8A 1.317(5) . ? C14A N7A 1.318(5) . ? N7A C16A 1.384(6) . ? N8A C15A 1.357(6) . ? C16A C15A 1.348(8) . ? C9A C8A 1.380(7) . ? C14B N7B 1.312(3) . ? C14B N8B 1.313(3) . ? N7B C16B 1.440(15) . ? N8B C15B 1.478(15) . ? C16B C17 1.3900 . ? C16B C15B 1.3900 . ? C17 C18 1.3900 . ? C18 C19 1.3900 . ? C19 C20 1.3900 . ? C20 C15B 1.3900 . ? C9B C8B 1.380(7) . ? C9B C10 1.427(11) . ? C8B C13 1.450(10) . ? C10 C11 1.375(14) . ? C13 C12 1.358(13) . ? C12 C11 1.411(14) . ? C12 C12 1.543(19) 5_655 ? C1S C2S 1.420(18) . ? C1S C3S 1.830(16) . ? C1S O1S 1.842(14) . ? C2SB C1SB 1.485(19) . ? C1SB C3SB 1.752(16) . ? C1SB O1SB 1.835(14) . ?