#------------------------------------------------------------------------------ #$Date: 2019-07-14 03:51:26 +0300 (Sun, 14 Jul 2019) $ #$Revision: 217018 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/05/7700528.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_7700528 loop_ _publ_author_name 'Meng, Huan-huan' 'Wang, Cai-Yun' 'Song, Xue-Qin' 'Xi, Wei' 'Wang, Li' _publ_section_title ; A cationic tetrahedral Zn(II) cluster based on a new salicylamide imine multidentate ligand:Synthesis, structure and fluorescence sensing study ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/C9DT01376H _journal_year 2019 _chemical_formula_sum 'C228 H254 N28 O81 Zn16' _chemical_formula_weight 5728.82 _space_group_crystal_system cubic _space_group_IT_number 205 _space_group_name_Hall '-P 2ac 2ab 3' _space_group_name_H-M_alt 'P a -3' _symmetry_space_group_name_Hall '-P 2ac 2ab 3' _symmetry_space_group_name_H-M 'P a -3' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2018-11-26 deposited with the CCDC. 2019-07-12 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 22.59190(10) _cell_length_b 22.59190(10) _cell_length_c 22.59190(10) _cell_measurement_reflns_used 3842 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 69.555 _cell_measurement_theta_min 4.363 _cell_volume 11530.77(9) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) ; _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 16.0733 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.986 _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Eos' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_unetI/netI 0.0255 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.986 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 10234 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.986 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 69.753 _diffrn_reflns_theta_min 4.795 _diffrn_source 'sealed X-ray tube' _exptl_absorpt_coefficient_mu 2.615 _exptl_absorpt_correction_T_max 0.625 _exptl_absorpt_correction_T_min 0.561 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'pale yellow' _exptl_crystal_density_diffrn 1.650 _exptl_crystal_description block _exptl_crystal_F_000 5892 _exptl_crystal_size_max 0.240 _exptl_crystal_size_mid 0.210 _exptl_crystal_size_min 0.180 _refine_diff_density_max 0.289 _refine_diff_density_min -0.375 _refine_diff_density_rms 0.051 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 289 _refine_ls_number_reflns 3636 _refine_ls_number_restraints 4 _refine_ls_restrained_S_all 1.040 _refine_ls_R_factor_all 0.0408 _refine_ls_R_factor_gt 0.0325 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0455P)^2^+6.4617P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0846 _refine_ls_wR_factor_ref 0.0915 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3062 _reflns_number_total 3636 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9dt01376h2.cif _cod_data_source_block songxq0916_sx _cod_original_cell_volume 11530.77(15) _cod_database_code 7700528 _shelx_shelxl_version_number 2014/7 _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_min 0.573 _shelx_estimated_absorpt_t_max 0.650 _shelx_res_file ; songxq0916_sx.res created by SHELXL-2014/7 TITL songxq0916_a.res in Pa-3 CELL 1.54178 22.5919 22.5919 22.5919 90 90 90 ZERR 4 0.0001 0.0001 0.0001 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SYMM +Z,+X,+Y SYMM 0.5+Z,0.5-X,-Y SYMM 0.5-Z,-X,0.5+Y SYMM -Z,0.5+X,0.5-Y SYMM +Y,+Z,+X SYMM -Y,0.5+Z,0.5-X SYMM 0.5+Y,0.5-Z,-X SYMM 0.5-Y,-Z,0.5+X SFAC C H N O Zn UNIT 456 508 56 162 32 OMIT 1 1 1 OMIT 1 1 3 OMIT 4 6 6 OMIT 1 2 6 REM Old TITL songxq0916 in Pa-3 REM SHELXT solution in Pa-3 REM R1 0.122, Rweak 0.008, Alpha 0.028, Orientation as input REM Formula found by SHELXT: C116 N15 O32 Zn8 REM REM REM L.S. 20 ACTA FMAP 2 PLAN 5 SIZE 0.24 0.21 0.18 DFIX 0.8 0.01 O6 H6 DFIX 2.02 O8 O9 DFIX 1.24 N3 O8 DFIX 1.24 N3 O9 WGHT 0.045500 6.461700 FVAR 0.21761 ZN1 5 0.763061 0.640951 0.702897 11.00000 0.02978 0.03383 = 0.04334 0.00647 0.00251 0.00148 ZN2 5 0.631437 0.631437 0.631437 10.33333 0.03543 0.03543 = 0.03543 0.00093 0.00093 0.00093 O6 4 0.716819 0.716819 0.716819 10.33333 0.03341 0.03341 = 0.03341 0.00252 0.00252 0.00252 O2 4 0.688518 0.688622 0.595454 11.00000 0.04750 0.03506 = 0.03576 -0.00377 0.01349 -0.00198 O4 4 0.824410 0.682948 0.660775 11.00000 0.04165 0.03506 = 0.05656 -0.00173 0.01719 -0.00121 O1 4 0.663750 0.583073 0.556038 11.00000 0.05595 0.03859 = 0.04833 -0.01099 0.00725 -0.00111 O5 4 0.809650 0.572102 0.633766 11.00000 0.04872 0.03950 = 0.05812 -0.00670 0.01750 -0.00348 N1 3 0.763508 0.793577 0.582787 11.00000 0.04557 0.03573 = 0.04338 0.00745 0.00314 -0.00265 N2 3 0.882057 0.784254 0.643948 11.00000 0.05198 0.04136 = 0.08212 0.00306 0.00206 -0.00892 AFIX 43 H2 2 0.865965 0.761437 0.669823 11.00000 -1.20000 AFIX 0 C7 1 0.719870 0.670090 0.548741 11.00000 0.03983 0.03978 = 0.02831 0.00019 0.00066 0.00688 C18 1 0.860274 0.660754 0.620449 11.00000 0.02998 0.04172 = 0.04175 0.00442 0.00517 0.00441 C6 1 0.763026 0.704206 0.520348 11.00000 0.04271 0.05108 = 0.03209 0.00168 0.00442 0.00294 O3 4 0.941658 0.789164 0.565209 11.00000 0.10589 0.07373 = 0.13092 0.02453 0.05545 -0.02648 C2 1 0.708239 0.612895 0.526458 11.00000 0.04267 0.04330 = 0.03416 -0.00358 -0.00238 0.00756 C17 1 0.855019 0.600277 0.604628 11.00000 0.03655 0.04316 = 0.04032 0.00093 0.00515 0.00224 N3 3 0.802235 0.697765 0.302235 10.33333 0.06817 0.06817 = 0.06817 0.01158 -0.01158 0.01158 O7 4 0.833535 0.666465 0.333535 10.33333 0.09614 0.09614 = 0.09614 0.01489 -0.01489 0.01489 C13 1 0.903637 0.694543 0.591123 11.00000 0.03615 0.05205 = 0.05182 0.01002 0.00457 0.00113 C16 1 0.891036 0.574382 0.563576 11.00000 0.05439 0.05694 = 0.05649 -0.01095 0.01280 0.00482 AFIX 43 H16 2 0.886872 0.534475 0.554373 11.00000 -1.20000 AFIX 0 C3 1 0.739137 0.589505 0.479589 11.00000 0.05798 0.05805 = 0.04385 -0.01318 0.00006 0.01264 AFIX 43 H3 2 0.731039 0.551448 0.466148 11.00000 -1.20000 AFIX 0 C14 1 0.939622 0.667098 0.548684 11.00000 0.04667 0.07835 = 0.05973 0.01071 0.02050 -0.00196 AFIX 43 H14 2 0.967974 0.689474 0.528934 11.00000 -1.20000 AFIX 0 C5 1 0.793217 0.679978 0.471758 11.00000 0.05163 0.07791 = 0.04162 -0.00190 0.01274 0.00057 AFIX 43 H5 2 0.821177 0.702867 0.452038 11.00000 -1.20000 AFIX 0 C12 1 0.910686 0.759628 0.599115 11.00000 0.04517 0.05491 = 0.07501 0.01360 0.00597 -0.00863 C15 1 0.934138 0.608590 0.535649 11.00000 0.05784 0.08294 = 0.06387 -0.00748 0.02880 0.00669 AFIX 43 H15 2 0.959253 0.591320 0.507981 11.00000 -1.20000 AFIX 0 C4 1 0.782487 0.623400 0.452671 11.00000 0.06381 0.07967 = 0.04048 -0.01601 0.01370 0.00929 AFIX 43 H4 2 0.804401 0.607741 0.421540 11.00000 -1.20000 AFIX 0 C9 1 0.783294 0.855890 0.588173 11.00000 0.06851 0.03846 = 0.06460 0.01204 0.00654 -0.00686 AFIX 23 H9A 2 0.749331 0.881715 0.583371 11.00000 -1.20000 H9B 2 0.810860 0.864509 0.556404 11.00000 -1.20000 AFIX 0 C10 1 0.812450 0.869373 0.646094 11.00000 0.07359 0.03658 = 0.07900 -0.00263 0.00305 -0.00739 AFIX 23 H10A 2 0.789358 0.851336 0.677478 11.00000 -1.20000 H10B 2 0.811575 0.911862 0.652206 11.00000 -1.20000 AFIX 0 C19 1 0.801511 0.510854 0.623952 11.00000 0.07696 0.04075 = 0.08920 -0.00941 0.02292 -0.00827 AFIX 137 H19A 2 0.837095 0.490014 0.634209 11.00000 -1.50000 H19B 2 0.792483 0.504151 0.582974 11.00000 -1.50000 H19C 2 0.769429 0.496794 0.648008 11.00000 -1.50000 AFIX 0 C11 1 0.876416 0.848231 0.651694 11.00000 0.06906 0.04027 = 0.12643 -0.00197 -0.01505 -0.01242 AFIX 23 H11A 2 0.900431 0.868134 0.622188 11.00000 -1.20000 H11B 2 0.891468 0.859084 0.690413 11.00000 -1.20000 AFIX 0 C1 1 0.651545 0.522952 0.539816 11.00000 0.10443 0.04609 = 0.10797 -0.03035 0.03542 -0.01663 AFIX 137 H1A 2 0.621159 0.507350 0.565093 11.00000 -1.50000 H1B 2 0.686845 0.499685 0.544078 11.00000 -1.50000 H1C 2 0.638457 0.521561 0.499412 11.00000 -1.50000 AFIX 0 H6 2 0.737266 0.737266 0.737266 10.33333 0.09783 C8 1 0.779316 0.764520 0.537019 11.00000 0.04549 0.05419 = 0.04048 0.01032 0.00930 -0.00306 AFIX 43 H8 2 0.804378 0.784226 0.510979 11.00000 -1.20000 AFIX 0 O9 4 0.841508 0.712407 0.258838 10.33333 0.12537 0.12130 = 0.06139 0.04006 0.01413 -0.00614 O8 4 0.770533 0.735566 0.307194 10.33333 0.13399 0.15085 = 0.07636 -0.00076 -0.03979 0.05863 AFIX 6 O11 4 0.500000 0.500000 0.500000 10.08333 0.17432 0.17432 = 0.17432 -0.01454 -0.01454 -0.01454 H11C 2 0.502960 0.538752 0.504721 10.08333 -1.50000 H11D 2 0.536008 0.489802 0.496176 10.08333 -1.50000 O10 4 0.593666 0.496598 0.408516 10.33333 0.08523 0.16803 = 0.12149 -0.00226 -0.01282 -0.01124 H10C 2 0.567693 0.521679 0.419359 10.33333 -1.50000 H10D 2 0.591539 0.466185 0.430578 10.33333 -1.50000 AFIX 0 HKLF 4 REM songxq0916_a.res in Pa-3 REM R1 = 0.0325 for 3062 Fo > 4sig(Fo) and 0.0408 for all 3593 data REM 289 parameters refined using 4 restraints END WGHT 0.0453 6.4334 REM Highest difference peak 0.289, deepest hole -0.375, 1-sigma level 0.051 Q1 1 0.9663 0.7653 0.5625 11.00000 0.05 0.27 Q2 1 0.5841 0.4466 0.4500 11.00000 0.05 0.24 Q3 1 0.6831 0.6657 0.6167 11.00000 0.05 0.23 Q4 1 0.9121 0.7819 0.5488 11.00000 0.05 0.22 Q5 1 0.7163 0.6366 0.5361 11.00000 0.05 0.21 ; _shelx_res_checksum 46546 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y, -z, -x' 'y, -z-1/2, x-1/2' '-y-1/2, z-1/2, x' 'y-1/2, z, -x-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 Zn1 Zn 0.76306(2) 0.64095(2) 0.70290(2) 0.03565(11) Uani 1 1 d . . . Zn2 Zn 0.63144(2) 0.63144(2) 0.63144(2) 0.03543(14) Uani 1 3 d S T P O6 O 0.71682(7) 0.71682(7) 0.71682(7) 0.0334(6) Uani 1 3 d DS T P O2 O 0.68852(8) 0.68862(7) 0.59545(7) 0.0394(4) Uani 1 1 d . . . O4 O 0.82441(8) 0.68295(8) 0.66078(9) 0.0444(4) Uani 1 1 d . . . O1 O 0.66375(9) 0.58307(8) 0.55604(8) 0.0476(4) Uani 1 1 d . . . O5 O 0.80965(9) 0.57210(8) 0.63377(9) 0.0488(5) Uani 1 1 d . . . N1 N 0.76351(10) 0.79358(9) 0.58279(10) 0.0416(5) Uani 1 1 d . . . N2 N 0.88206(12) 0.78425(11) 0.64395(13) 0.0585(7) Uani 1 1 d . . . H2 H 0.8660 0.7614 0.6698 0.070 Uiso 1 1 calc R U . C7 C 0.71987(11) 0.67009(11) 0.54874(10) 0.0360(5) Uani 1 1 d . . . C18 C 0.86027(10) 0.66075(11) 0.62045(11) 0.0378(5) Uani 1 1 d . . . C6 C 0.76303(11) 0.70421(12) 0.52035(11) 0.0420(6) Uani 1 1 d . . . O3 O 0.94166(14) 0.78916(13) 0.56521(15) 0.1035(11) Uani 1 1 d . . . C2 C 0.70824(11) 0.61290(11) 0.52646(11) 0.0400(5) Uani 1 1 d . . . C17 C 0.85502(11) 0.60028(11) 0.60463(11) 0.0400(5) Uani 1 1 d . . . N3 N 0.80224(13) 0.69776(13) 0.30224(13) 0.0682(13) Uani 1 3 d DS T P O7 O 0.83353(13) 0.66647(13) 0.33353(13) 0.0961(16) Uani 1 3 d S T P C13 C 0.90364(12) 0.69454(13) 0.59112(13) 0.0467(6) Uani 1 1 d . . . C16 C 0.89104(13) 0.57438(14) 0.56358(14) 0.0559(7) Uani 1 1 d . . . H16 H 0.8869 0.5345 0.5544 0.067 Uiso 1 1 calc R U . C3 C 0.73914(14) 0.58950(14) 0.47959(13) 0.0533(7) Uani 1 1 d . . . H3 H 0.7310 0.5514 0.4661 0.064 Uiso 1 1 calc R U . C14 C 0.93962(14) 0.66710(16) 0.54868(15) 0.0616(8) Uani 1 1 d . . . H14 H 0.9680 0.6895 0.5289 0.074 Uiso 1 1 calc R U . C5 C 0.79322(14) 0.67998(16) 0.47176(13) 0.0571(7) Uani 1 1 d . . . H5 H 0.8212 0.7029 0.4520 0.068 Uiso 1 1 calc R U . C12 C 0.91069(13) 0.75963(14) 0.59912(16) 0.0584(8) Uani 1 1 d . . . C15 C 0.93414(15) 0.60859(17) 0.53565(16) 0.0682(9) Uani 1 1 d . . . H15 H 0.9593 0.5913 0.5080 0.082 Uiso 1 1 calc R U . C4 C 0.78249(15) 0.62340(16) 0.45267(13) 0.0613(8) Uani 1 1 d . . . H4 H 0.8044 0.6077 0.4215 0.074 Uiso 1 1 calc R U . C9 C 0.78329(15) 0.85589(12) 0.58817(15) 0.0572(7) Uani 1 1 d . . . H9A H 0.7493 0.8817 0.5834 0.069 Uiso 1 1 calc R U . H9B H 0.8109 0.8645 0.5564 0.069 Uiso 1 1 calc R U . C10 C 0.81245(16) 0.86937(13) 0.64609(16) 0.0631(8) Uani 1 1 d . . . H10A H 0.7894 0.8513 0.6775 0.076 Uiso 1 1 calc R U . H10B H 0.8116 0.9119 0.6522 0.076 Uiso 1 1 calc R U . C19 C 0.80151(17) 0.51085(13) 0.62395(17) 0.0690(10) Uani 1 1 d . . . H19A H 0.8371 0.4900 0.6342 0.103 Uiso 1 1 calc R U . H19B H 0.7925 0.5042 0.5830 0.103 Uiso 1 1 calc R U . H19C H 0.7694 0.4968 0.6480 0.103 Uiso 1 1 calc R U . C11 C 0.87642(17) 0.84823(14) 0.6517(2) 0.0786(12) Uani 1 1 d . . . H11A H 0.9004 0.8681 0.6222 0.094 Uiso 1 1 calc R U . H11B H 0.8915 0.8591 0.6904 0.094 Uiso 1 1 calc R U . C1 C 0.6515(2) 0.52295(15) 0.5398(2) 0.0862(13) Uani 1 1 d . . . H1A H 0.6212 0.5073 0.5651 0.129 Uiso 1 1 calc R U . H1B H 0.6868 0.4997 0.5441 0.129 Uiso 1 1 calc R U . H1C H 0.6385 0.5216 0.4994 0.129 Uiso 1 1 calc R U . H6 H 0.7373(3) 0.7373(3) 0.7373(3) 0.10(3) Uiso 1 3 d DS . P C8 C 0.77932(12) 0.76452(13) 0.53702(12) 0.0467(6) Uani 1 1 d . . . H8 H 0.8044 0.7842 0.5110 0.056 Uiso 1 1 calc R U . O9 O 0.8415(5) 0.7124(5) 0.2588(4) 0.103(3) Uani 0.3333 1 d D . P O8 O 0.7705(8) 0.7356(8) 0.3072(4) 0.120(5) Uani 0.3333 1 d D . P O11 O 0.5000 0.5000 0.5000 0.174(10) Uani 0.5 6 d GS T P H11C H 0.5030 0.5388 0.5047 0.261 Uiso 0.0833 1 d G U P H11D H 0.5360 0.4898 0.4962 0.261 Uiso 0.0833 1 d G U P O10 O 0.5937(3) 0.4966(6) 0.4085(3) 0.125(4) Uani 0.3333 1 d G . P H10C H 0.5677 0.5217 0.4194 0.187 Uiso 0.3333 1 d G U P H10D H 0.5915 0.4662 0.4306 0.187 Uiso 0.3333 1 d G U P 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 0.02978(17) 0.03383(18) 0.04334(19) 0.00647(13) 0.00251(13) 0.00148(12) Zn2 0.03543(14) 0.03543(14) 0.03543(14) 0.00093(13) 0.00093(13) 0.00093(13) O6 0.0334(6) 0.0334(6) 0.0334(6) 0.0025(7) 0.0025(7) 0.0025(7) O2 0.0475(10) 0.0351(8) 0.0358(9) -0.0038(7) 0.0135(7) -0.0020(7) O4 0.0416(9) 0.0351(9) 0.0566(11) -0.0017(8) 0.0172(8) -0.0012(7) O1 0.0560(11) 0.0386(9) 0.0483(10) -0.0110(8) 0.0073(9) -0.0011(8) O5 0.0487(11) 0.0395(9) 0.0581(11) -0.0067(8) 0.0175(9) -0.0035(8) N1 0.0456(12) 0.0357(10) 0.0434(12) 0.0075(9) 0.0031(9) -0.0026(9) N2 0.0520(14) 0.0414(13) 0.0821(19) 0.0031(12) 0.0021(13) -0.0089(11) C7 0.0398(12) 0.0398(12) 0.0283(11) 0.0002(9) 0.0007(9) 0.0069(10) C18 0.0300(11) 0.0417(13) 0.0417(13) 0.0044(10) 0.0052(10) 0.0044(10) C6 0.0427(14) 0.0511(14) 0.0321(12) 0.0017(11) 0.0044(10) 0.0029(11) O3 0.106(2) 0.0737(17) 0.131(3) 0.0245(18) 0.055(2) -0.0265(16) C2 0.0427(13) 0.0433(13) 0.0342(12) -0.0036(10) -0.0024(10) 0.0076(11) C17 0.0366(12) 0.0432(13) 0.0403(13) 0.0009(11) 0.0051(10) 0.0022(10) N3 0.0682(13) 0.0682(13) 0.0682(13) 0.0116(15) -0.0116(15) 0.0116(15) O7 0.0961(16) 0.0961(16) 0.0961(16) 0.0149(16) -0.0149(16) 0.0149(16) C13 0.0362(13) 0.0520(15) 0.0518(15) 0.0100(12) 0.0046(11) 0.0011(11) C16 0.0544(17) 0.0569(17) 0.0565(17) -0.0109(14) 0.0128(14) 0.0048(14) C3 0.0580(17) 0.0580(17) 0.0439(15) -0.0132(13) 0.0001(13) 0.0126(14) C14 0.0467(16) 0.078(2) 0.0597(18) 0.0107(16) 0.0205(14) -0.0020(15) C5 0.0516(16) 0.078(2) 0.0416(14) -0.0019(14) 0.0127(13) 0.0006(15) C12 0.0452(15) 0.0549(17) 0.075(2) 0.0136(16) 0.0060(15) -0.0086(13) C15 0.0578(18) 0.083(2) 0.064(2) -0.0075(18) 0.0288(16) 0.0067(17) C4 0.0638(19) 0.080(2) 0.0405(15) -0.0160(15) 0.0137(14) 0.0093(16) C9 0.069(2) 0.0385(14) 0.0646(19) 0.0120(13) 0.0065(15) -0.0069(13) C10 0.074(2) 0.0366(14) 0.079(2) -0.0026(14) 0.0030(17) -0.0074(14) C19 0.077(2) 0.0407(16) 0.089(3) -0.0094(16) 0.0229(19) -0.0083(15) C11 0.069(2) 0.0403(16) 0.126(4) -0.0020(19) -0.015(2) -0.0124(16) C1 0.104(3) 0.0461(18) 0.108(3) -0.030(2) 0.035(3) -0.0166(19) C8 0.0455(14) 0.0542(16) 0.0405(14) 0.0103(12) 0.0093(11) -0.0031(12) O9 0.125(9) 0.121(9) 0.061(5) 0.040(6) 0.014(6) -0.006(7) O8 0.134(11) 0.151(15) 0.076(7) -0.001(8) -0.040(9) 0.059(8) O11 0.174(10) 0.174(10) 0.174(10) -0.015(10) -0.015(10) -0.015(10) O10 0.085(7) 0.168(11) 0.121(9) -0.002(8) -0.013(6) -0.011(7) 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' 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_ _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 O4 Zn1 O2 141.00(8) . 9 O4 Zn1 N1 114.14(8) . 9 O2 Zn1 N1 93.60(8) 9 9 O4 Zn1 O6 91.77(6) . . O2 Zn1 O6 91.51(9) 9 . N1 Zn1 O6 128.28(8) 9 . O4 Zn1 O5 71.85(7) . . O2 Zn1 O5 86.05(7) 9 . N1 Zn1 O5 82.65(8) 9 . O6 Zn1 O5 149.06(6) . . O2 Zn2 O2 96.22(7) 9 5 O2 Zn2 O2 96.22(7) 9 . O2 Zn2 O2 96.22(7) 5 . O2 Zn2 O1 94.87(8) 9 . O2 Zn2 O1 167.89(7) 5 . O2 Zn2 O1 77.72(7) . . O2 Zn2 O1 77.72(7) 9 9 O2 Zn2 O1 94.87(8) 5 9 O2 Zn2 O1 167.88(7) . 9 O1 Zn2 O1 92.23(7) . 9 O2 Zn2 O1 167.89(7) 9 5 O2 Zn2 O1 77.72(7) 5 5 O2 Zn2 O1 94.87(8) . 5 O1 Zn2 O1 92.23(7) . 5 O1 Zn2 O1 92.23(8) 9 5 Zn1 O6 Zn1 112.50(7) 9 5 Zn1 O6 Zn1 112.50(7) 9 . Zn1 O6 Zn1 112.51(7) 5 . C7 O2 Zn1 125.67(15) . 5 C7 O2 Zn2 117.40(15) . . Zn1 O2 Zn2 116.10(8) 5 . C18 O4 Zn1 126.51(16) . . C2 O1 C1 118.6(2) . . C2 O1 Zn2 112.46(15) . . C1 O1 Zn2 128.2(2) . . C17 O5 C19 118.4(2) . . C17 O5 Zn1 109.43(15) . . C19 O5 Zn1 131.89(18) . . C8 N1 C9 118.1(2) . . C8 N1 Zn1 122.79(19) . 5 C9 N1 Zn1 118.39(19) . 5 C12 N2 C11 123.3(3) . . O2 C7 C6 123.9(2) . . O2 C7 C2 118.0(2) . . C6 C7 C2 118.1(2) . . O4 C18 C13 123.1(2) . . O4 C18 C17 119.3(2) . . C13 C18 C17 117.5(2) . . C7 C6 C5 118.9(3) . . C7 C6 C8 124.8(2) . . C5 C6 C8 116.3(3) . . C3 C2 O1 123.7(3) . . C3 C2 C7 122.2(3) . . O1 C2 C7 114.2(2) . . C16 C17 O5 124.8(3) . . C16 C17 C18 122.3(2) . . O5 C17 C18 112.8(2) . . O8 N3 O8 69.7(8) . 12_664 O8 N3 O8 69.7(8) . 6_566 O8 N3 O8 69.7(8) 12_664 6_566 O8 N3 O7 138.7(5) . . O8 N3 O7 138.7(5) 12_664 . O8 N3 O7 138.7(5) 6_566 . O8 N3 O9 39.8(6) . 12_664 O8 N3 O9 107.6(11) 12_664 12_664 O8 N3 O9 93.5(14) 6_566 12_664 O7 N3 O9 100.3(6) . 12_664 O8 N3 O9 93.5(14) . 6_566 O8 N3 O9 39.8(6) 12_664 6_566 O8 N3 O9 107.6(11) 6_566 6_566 O7 N3 O9 100.3(6) . 6_566 O9 N3 O9 116.8(3) 12_664 6_566 O8 N3 O9 107.6(11) . . O8 N3 O9 93.5(14) 12_664 . O8 N3 O9 39.8(6) 6_566 . O7 N3 O9 100.3(6) . . O9 N3 O9 116.8(3) 12_664 . O9 N3 O9 116.9(3) 6_566 . C14 C13 C18 119.1(3) . . C14 C13 C12 117.2(3) . . C18 C13 C12 123.5(3) . . C17 C16 C15 119.1(3) . . C2 C3 C4 119.0(3) . . C15 C14 C13 121.7(3) . . C4 C5 C6 121.6(3) . . O3 C12 N2 121.7(3) . . O3 C12 C13 121.3(3) . . N2 C12 C13 117.1(3) . . C14 C15 C16 120.3(3) . . C5 C4 C3 120.2(3) . . N1 C9 C10 113.4(2) . . C9 C10 C11 115.2(3) . . N2 C11 C10 112.5(3) . . N1 C8 C6 128.2(2) . . O8 O9 N3 55.0(9) 6_566 . O8 O9 O8 40.3(15) 6_566 12_664 N3 O9 O8 38.0(7) . 12_664 O9 O8 N3 85.2(10) 12_664 . O9 O8 O8 114(2) 12_664 6_566 N3 O8 O8 55.2(4) . 6_566 O9 O8 O8 136.9(12) 12_664 12_664 N3 O8 O8 55.2(4) . 12_664 O8 O8 O8 60.001(4) 6_566 12_664 O9 O8 O9 114.7(15) 12_664 6_566 N3 O8 O9 48.5(9) . 6_566 O8 O8 O9 78.9(13) 6_566 6_566 O8 O8 O9 26.2(10) 12_664 6_566 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Zn1 O4 1.9305(17) . Zn1 O2 1.9975(16) 9 Zn1 N1 2.019(2) 9 Zn1 O6 2.0318(9) . Zn1 O5 2.4426(18) . Zn2 O2 1.9982(17) 9 Zn2 O2 1.9982(16) 5 Zn2 O2 1.9982(17) . Zn2 O1 2.1514(18) . Zn2 O1 2.1514(18) 9 Zn2 O1 2.1514(18) 5 O6 Zn1 2.0317(9) 9 O6 Zn1 2.0317(9) 5 O2 C7 1.338(3) . O2 Zn1 1.9976(16) 5 O4 C18 1.318(3) . O1 C2 1.382(3) . O1 C1 1.434(3) . O5 C17 1.374(3) . O5 C19 1.413(3) . N1 C8 1.276(4) . N1 C9 1.482(3) . N1 Zn1 2.019(2) 5 N2 C12 1.324(4) . N2 C11 1.461(4) . C7 C6 1.399(4) . C7 C2 1.411(3) . C18 C13 1.408(4) . C18 C17 1.417(4) . C6 C5 1.404(4) . C6 C8 1.461(4) . O3 C12 1.234(4) . C2 C3 1.374(4) . C17 C16 1.365(4) . N3 O8 1.120(10) . N3 O8 1.120(10) 12_664 N3 O8 1.120(10) 6_566 N3 O7 1.225(7) . N3 O9 1.363(9) 12_664 N3 O9 1.363(9) 6_566 N3 O9 1.363(9) . C13 C14 1.402(4) . C13 C12 1.490(4) . C16 C15 1.394(5) . C3 C4 1.384(5) . C14 C15 1.360(5) . C5 C4 1.371(5) . C9 C10 1.496(5) . C10 C11 1.527(5) . O9 O8 0.875(13) 6_566 O9 O8 1.82(2) 12_664 O8 O9 0.875(13) 12_664 O8 O8 1.280(18) 6_566 O8 O8 1.280(18) 12_664 O8 O9 1.82(2) 6_566