#------------------------------------------------------------------------------ #$Date: 2019-12-13 04:34:02 +0200 (Fri, 13 Dec 2019) $ #$Revision: 245036 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/29/7702944.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_7702944 loop_ _publ_author_name 'G\'omez, Mar\'ia Laura R\'ios' 'Lampronti, Giulio Isacco' 'Yang, Yongjian' 'Mauro, John C.' 'Bennett, Thomas Douglas' _publ_section_title ; Relating Structural Disorder and Melting in Complex Mixed Ligand Zeolitic Imidazolate Framework Glasses ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/C9DT03559A _journal_year 2019 _chemical_formula_moiety '(Zn1 C7.12 N4 H5.97)*0.46(C5 N1 O1 H11)' _chemical_formula_sum 'C18.84 H22.06 N8.92 O0.92 Zn2' _chemical_formula_weight 517.74 _chemical_name_common 'Zinc (imdazolate, benzimidazolate, 5-methyl-benzimidazolate) solid solution' _chemical_name_systematic ZIF-UC-1a _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' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2019-07-26 deposited with the CCDC. 2019-12-12 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 15.7365(4) _cell_length_b 16.0434(4) _cell_length_c 18.6754(7) _cell_measurement_reflns_used 4023 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 64.0289 _cell_measurement_theta_min 2.3658 _cell_volume 4714.9(2) _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_detector_type Eos _diffrn_measured_fraction_theta_full 0.9282 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 51.00 101.00 1.0000 15.6800 omega____ theta____ kappa____ phi______ frames - 51.2500 77.0000 -60.0000 50 #__ type_ start__ end____ width___ exp.time_ 2 omega 74.00 126.00 1.0000 15.6800 omega____ theta____ kappa____ phi______ frames - 51.2500 125.0000 0.0000 52 #__ type_ start__ end____ width___ exp.time_ 3 omega 73.00 170.00 1.0000 15.6800 omega____ theta____ kappa____ phi______ frames - 102.5000 65.0000 30.0000 97 #__ type_ start__ end____ width___ exp.time_ 4 omega 124.00 167.00 1.0000 15.6800 omega____ theta____ kappa____ phi______ frames - 102.5000 -21.0000 -30.0000 43 #__ type_ start__ end____ width___ exp.time_ 5 omega 130.00 178.00 1.0000 15.6800 omega____ theta____ kappa____ phi______ frames - 102.5000 -21.0000 -90.0000 48 #__ type_ start__ end____ width___ exp.time_ 6 omega 84.00 110.00 1.0000 15.6800 omega____ theta____ kappa____ phi______ frames - 102.5000 -65.0000 -90.0000 26 #__ type_ start__ end____ width___ exp.time_ 7 omega 62.00 87.00 1.0000 15.6800 omega____ theta____ kappa____ phi______ frames - 102.5000 -54.0000 -150.0000 25 #__ type_ start__ end____ width___ exp.time_ 8 omega 33.00 74.00 1.0000 15.6800 omega____ theta____ kappa____ phi______ frames - 102.5000 -104.0000 -90.0000 41 #__ type_ start__ end____ width___ exp.time_ 9 omega 27.00 86.00 1.0000 15.6800 omega____ theta____ kappa____ phi______ frames - 102.5000 -104.0000 -150.0000 59 #__ type_ start__ end____ width___ exp.time_ 10 omega 25.00 72.00 1.0000 15.6800 omega____ theta____ kappa____ phi______ frames - 102.5000 -124.0000 -84.0000 47 #__ type_ start__ end____ width___ exp.time_ 11 omega 21.00 63.00 1.0000 15.6800 omega____ theta____ kappa____ phi______ frames - 102.5000 -32.0000 -60.0000 42 #__ type_ start__ end____ width___ exp.time_ 12 omega 21.00 46.00 1.0000 15.6800 omega____ theta____ kappa____ phi______ frames - 102.5000 -32.0000 60.0000 25 #__ type_ start__ end____ width___ exp.time_ 13 omega 48.00 89.00 1.0000 15.6800 omega____ theta____ kappa____ phi______ frames - 102.5000 -54.0000 90.0000 41 #__ type_ start__ end____ width___ exp.time_ 14 omega 27.00 63.00 1.0000 15.6800 omega____ theta____ kappa____ phi______ frames - 102.5000 -32.0000 90.0000 36 #__ type_ start__ end____ width___ exp.time_ 15 omega -24.00 26.00 1.0000 3.9200 omega____ theta____ kappa____ phi______ frames - 0.0000 -99.0000 120.0000 50 #__ type_ start__ end____ width___ exp.time_ 16 omega 55.00 88.00 1.0000 3.9200 omega____ theta____ kappa____ phi______ frames - 0.0000 178.0000 -90.0000 33 #__ type_ start__ end____ width___ exp.time_ 17 omega 40.00 65.00 1.0000 3.9200 omega____ theta____ kappa____ phi______ frames - 0.0000 178.0000 -180.0000 25 #__ type_ start__ end____ width___ exp.time_ 18 omega 78.00 112.00 1.0000 15.6800 omega____ theta____ kappa____ phi______ frames - 51.2500 125.0000 120.0000 34 #__ type_ start__ end____ width___ exp.time_ 19 omega 89.00 131.00 1.0000 15.6800 omega____ theta____ kappa____ phi______ frames - 51.2500 125.0000 150.0000 42 #__ type_ start__ end____ width___ exp.time_ 20 omega -2.00 68.00 1.0000 15.6800 omega____ theta____ kappa____ phi______ frames - 51.2500 -125.0000 -120.0000 70 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0686838000 _diffrn_orient_matrix_UB_12 -0.0286125000 _diffrn_orient_matrix_UB_13 0.0534315000 _diffrn_orient_matrix_UB_21 0.0694431000 _diffrn_orient_matrix_UB_22 -0.0365572000 _diffrn_orient_matrix_UB_23 0.0489227000 _diffrn_orient_matrix_UB_31 0.0070481000 _diffrn_orient_matrix_UB_32 0.0839989000 _diffrn_orient_matrix_UB_33 0.0394940000 _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 0.0158 _diffrn_reflns_av_unetI/netI 0.0175 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 10797 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 64.029 _diffrn_reflns_theta_min 2.3658 _diffrn_source 'sealed X-ray tube' _diffrn_source_type 'Enhance Ultra (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 2.73 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.92029 _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 transparent _exptl_crystal_density_diffrn 1.460 _exptl_crystal_description equant _exptl_crystal_F_000 2364.64 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.845 _refine_diff_density_min -0.439 _refine_diff_density_rms 0.086 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 237 _refine_ls_number_reflns 3902 _refine_ls_number_restraints 22 _refine_ls_restrained_S_all 1.503 _refine_ls_R_factor_all 0.0771 _refine_ls_R_factor_gt 0.0665 _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^)+(0.1317P)^2^+5.5560P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2121 _refine_ls_wR_factor_ref 0.2261 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3145 _reflns_number_total 3902 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9dt03559a2.cif _cod_data_source_block shelx _cod_original_formula_sum 'Zn2 C18.84 H22.06 N8.92 O.92' _cod_database_code 7702944 _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. ; _reflns_odcompleteness_completeness 92.82 _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 16:04:02 on 26-Jul-2019 CELL 1.54184 15.7365 16.0434 18.6754 90.000 90.000 90.000 ZERR 8.00 0.0004 0.0004 0.0007 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 72 0 96 16 0 MERG 2 EXYZ C8a C8b EXYZ C9a C9b EADP C8a C8b EADP C9a C9b EADP C17B C16B C18 C20 C19 C21 C15B EADP C1S O1S N1S C2S C3S C4S C5S EADP C9B C8B C13 C12 C11 C10 C14 EXYZ N8a N8b EXYZ N7a N7b EADP N8a N8b EADP N7a N7b DFIX 1.21 0.020 O1S C1S DFIX 1.33 0.020 C1S N1S DFIX 1.48 0.020 N1S C2S DFIX 1.46 0.020 N1S C3S DFIX 1.44 0.020 C3S C5S DFIX 1.55 0.020 C2S C4S DFIX 4.59 0.020 O1S C4S DFIX 3.33 0.020 O1S C5S DFIX 1.33 0.020 C15B N7B DFIX 1.33 0.020 C15B N8B DANG 2.26 0.030 O1S C1S O1S N1S DANG 2.42 0.030 C1S N1S C1S C3S DANG 2.43 0.030 C1S N1S C1S C2S DANG 2.34 0.030 N1S C3S N1S C5S DANG 2.52 0.030 N1S C2S N1S C4S FLAT 0.100 N7B N8B C15B C16B C17B FMAP 2 PLAN 20 ACTA 50.00 L.S. 50 WGHT 0.131700 5.556000 FVAR 2.07896 0.39619 0.12905 0.91228 0.16866 ZN1 4 0.309606 0.135491 0.106223 11.00000 0.06491 0.07318 = 0.08597 -0.00762 0.00038 0.00555 ZN2 4 0.497766 0.325182 0.328480 11.00000 0.06309 0.07454 = 0.07971 -0.00151 -0.00611 0.00043 N2 3 0.439542 0.301181 0.236188 11.00000 0.08180 0.07660 = 0.07439 0.00819 -0.00953 0.00146 N5 3 0.185040 0.156026 0.117367 11.00000 0.06403 0.07301 = 0.08366 -0.00532 0.00095 0.00430 N4 3 0.344954 0.032006 0.156153 11.00000 0.07691 0.07562 = 0.09421 -0.00021 0.00500 0.00893 N6 3 0.066816 0.228974 0.139016 11.00000 0.06361 0.07350 = 0.08496 -0.00640 0.00453 -0.00008 N3 3 0.421741 -0.079957 0.184204 11.00000 0.07143 0.07406 = 0.08907 0.00369 0.00338 0.00690 N1 3 0.369025 0.231072 0.152380 11.00000 0.07389 0.07065 = 0.07737 -0.00122 -0.00934 -0.00226 C4 1 0.405021 -0.021653 0.136545 11.00000 0.07778 0.07478 = 0.08431 0.00008 0.00435 0.00953 AFIX 43 H4 2 0.432955 -0.018300 0.092755 11.00000 -1.20000 AFIX 0 C1 1 0.409894 0.228263 0.214986 11.00000 0.07535 0.07145 = 0.07956 0.00017 -0.00984 -0.00245 AFIX 43 H1 2 0.416832 0.179468 0.241225 11.00000 -1.20000 AFIX 0 C2 1 0.416584 0.354569 0.183402 11.00000 0.12616 0.07456 = 0.11069 0.01745 -0.04657 -0.00842 AFIX 43 H2 2 0.428880 0.411237 0.181792 11.00000 -1.20000 AFIX 0 C7 1 0.151809 0.227170 0.139314 11.00000 0.06576 0.07013 = 0.08230 -0.00507 0.00705 -0.00340 AFIX 43 H7 2 0.184750 0.272260 0.153772 11.00000 -1.20000 AFIX 0 C3 1 0.372765 0.311324 0.133518 11.00000 0.14798 0.08451 = 0.10094 0.01112 -0.05632 -0.00317 AFIX 43 H3 2 0.348851 0.333954 0.092337 11.00000 -1.20000 AFIX 0 C6 1 0.372069 -0.061660 0.237655 11.00000 0.17391 0.11413 = 0.10837 0.04118 0.04941 0.05773 AFIX 43 H6 2 0.370336 -0.090613 0.280771 11.00000 -1.20000 AFIX 0 C5 1 0.323116 0.005550 0.221775 11.00000 0.16812 0.11572 = 0.16588 0.03811 0.09621 0.05540 AFIX 43 H5 2 0.281830 0.029043 0.251139 11.00000 -1.20000 AFIX 0 PART 1 C15A 1 0.407219 0.156651 -0.030345 -31.00000 0.06514 0.08185 = 0.08460 0.00623 -0.01035 0.00453 AFIX 43 H15A 2 0.450963 0.183590 -0.006146 -31.00000 -1.20000 AFIX 0 N7A 3 0.409871 0.145300 -0.099154 -31.00000 0.06901 0.10713 = 0.08176 -0.01587 0.00389 -0.01116 N8A 3 0.340480 0.128590 0.003313 -31.00000 0.06998 0.11103 = 0.08847 -0.02612 0.01438 -0.01631 C16A 1 0.332115 0.115235 -0.115433 -31.00000 0.11486 0.24883 = 0.09170 -0.04018 0.01240 -0.09033 C17A 1 0.290087 0.103530 -0.053444 -31.00000 0.10927 0.28488 = 0.12856 -0.07354 0.03179 -0.09915 C8A 1 0.043680 0.153412 0.114232 -21.00000 0.08734 AFIX 43 H8A 2 -0.011889 0.135474 0.107167 -21.00000 -1.20000 AFIX 0 C9A 1 0.116302 0.106660 0.100949 -21.00000 0.08734 AFIX 43 H9A 2 0.118098 0.052142 0.084096 -21.00000 -1.20000 AFIX 0 PART 2 C15B 1 0.383526 0.178028 -0.038721 31.00000 0.07820 AFIX 43 H15B 2 0.394837 0.233135 -0.026560 31.00000 -1.20000 AFIX 0 N8B 3 0.340480 0.128590 0.003313 31.00000 0.06998 0.11103 = 0.08847 -0.02612 0.01438 -0.01631 N7B 3 0.409871 0.145300 -0.099154 31.00000 0.06901 0.10713 = 0.08176 -0.01587 0.00389 -0.01116 C9B 1 0.116302 0.106660 0.100949 21.00000 0.08734 C8B 1 0.043680 0.153412 0.114232 21.00000 0.08734 C13 1 -0.035119 0.125900 0.096150 21.00000 0.08734 AFIX 43 H13 2 -0.083058 0.158227 0.104917 21.00000 -1.20000 AFIX 0 C10 1 0.111971 0.031050 0.065309 21.00000 0.08734 AFIX 43 H10 2 0.160678 0.001029 0.053896 21.00000 -1.20000 AFIX 0 C11 1 0.031757 0.002226 0.047458 21.00000 0.08734 AFIX 43 H11 2 0.026891 -0.048588 0.023846 21.00000 -1.20000 AFIX 0 C12 1 -0.041990 0.046642 0.063608 21.00000 0.08734 C14 1 -0.108197 0.004880 0.051909 51.00000 0.08734 AFIX 66 C16B 1 0.375981 0.045190 -0.091863 31.00000 0.07820 C17B 1 0.333348 0.038717 -0.026915 31.00000 0.07820 C18 1 0.298914 -0.037227 -0.005902 31.00000 0.07820 C19 1 0.307113 -0.106697 -0.049838 31.00000 0.07820 C20 1 0.349746 -0.100225 -0.114786 31.00000 0.07820 C21 1 0.384180 -0.024282 -0.135799 31.00000 0.07820 AFIX 0 PART 0 C1S 1 0.158958 0.173546 0.327706 41.00000 0.43394 O1S 5 0.098326 0.099082 0.308171 41.00000 0.43394 N1S 3 0.141795 0.145960 0.421640 41.00000 0.43394 C2S 1 0.256502 0.144773 0.419360 41.00000 0.43394 C3S 1 0.115201 0.249822 0.436722 41.00000 0.43394 C5S 1 0.174479 0.273875 0.380218 41.00000 0.43394 C4S 1 0.265866 0.134829 0.501735 41.00000 0.43394 H16A 2 0.284230 0.122006 -0.173993 -31.00000 0.15132 H17A 2 0.214298 0.103425 -0.042543 -31.00000 0.13172 HKLF 4 REM CF solution in Pbca REM wR2 = 0.2172, GooF = S = 1.035, Restrained GooF = 1.444 for all data REM R1 = 0.0639 for 3145 Fo > 4sig(Fo) and 0.0744 for all 3902 data REM 247 parameters refined using 22 restraints END WGHT 0.1322 4.5348 REM Highest difference peak 0.845, deepest hole -0.439, 1-sigma level 0.086 Q1 1 0.1927 0.1685 0.3944 11.00000 0.05 0.85 Q2 1 0.3292 0.1272 0.4476 11.00000 0.05 0.67 Q3 1 0.4170 -0.0984 -0.1101 11.00000 0.05 0.63 Q4 1 0.3139 0.1334 0.3935 11.00000 0.05 0.61 Q5 1 0.0921 0.2962 0.4223 11.00000 0.05 0.59 Q6 1 0.1764 0.1711 0.3186 11.00000 0.05 0.48 Q7 1 0.0592 0.1316 0.1482 11.00000 0.05 0.42 Q8 1 0.1314 0.0904 0.1434 11.00000 0.05 0.35 Q9 1 0.0668 0.0615 0.4513 11.00000 0.05 0.34 Q10 1 0.2984 -0.1091 -0.0192 11.00000 0.05 0.32 Q11 1 0.1641 0.1951 0.4558 11.00000 0.05 0.30 Q12 1 0.2523 0.1406 0.4861 11.00000 0.05 0.28 Q13 1 0.3811 -0.0613 0.2606 11.00000 0.05 0.27 Q14 1 0.3773 -0.0103 -0.1672 11.00000 0.05 0.22 Q15 1 0.4366 0.2999 0.2681 11.00000 0.05 0.22 Q16 1 0.3569 0.0319 0.1800 11.00000 0.05 0.21 Q17 1 0.3806 0.3467 0.1699 11.00000 0.05 0.20 Q18 1 -0.1434 0.0484 0.0388 11.00000 0.05 0.20 Q19 1 0.3494 0.0124 0.2340 11.00000 0.05 0.19 Q20 1 0.4219 0.1478 -0.1274 11.00000 0.05 0.19 ; _shelx_res_checksum 56485 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 0.30961(4) 0.13549(5) 0.10622(4) 0.0747(3) Uani 1 1 d . . . . . Zn2 Zn 0.49777(4) 0.32518(5) 0.32848(4) 0.0724(3) Uani 1 1 d . . . . . N2 N 0.4395(3) 0.3012(3) 0.2362(2) 0.0776(12) Uani 1 1 d . . . . . N5 N 0.1850(3) 0.1560(3) 0.1174(3) 0.0736(12) Uani 1 1 d . . . . . N4 N 0.3450(3) 0.0320(3) 0.1562(3) 0.0822(13) Uani 1 1 d . . . . . N6 N 0.0668(3) 0.2290(3) 0.1390(3) 0.0740(11) Uani 1 1 d . . . . . N3 N 0.4217(3) -0.0800(3) 0.1842(3) 0.0782(12) Uani 1 1 d . . . . . N1 N 0.3690(3) 0.2311(3) 0.1524(3) 0.0740(11) Uani 1 1 d . . . . . C4 C 0.4050(4) -0.0217(3) 0.1365(3) 0.0790(14) Uani 1 1 d . . . . . H4 H 0.432955 -0.018300 0.092755 0.095 Uiso 1 1 calc R U . . . C1 C 0.4099(3) 0.2283(3) 0.2150(3) 0.0755(14) Uani 1 1 d . . . . . H1 H 0.416832 0.179468 0.241225 0.091 Uiso 1 1 calc R U . . . C2 C 0.4166(5) 0.3546(4) 0.1834(4) 0.104(2) Uani 1 1 d . . . . . H2 H 0.428880 0.411237 0.181792 0.125 Uiso 1 1 calc R U . . . C7 C 0.1518(3) 0.2272(3) 0.1393(3) 0.0727(13) Uani 1 1 d . . . . . H7 H 0.184750 0.272260 0.153772 0.087 Uiso 1 1 calc R U . . . C3 C 0.3728(6) 0.3113(4) 0.1335(4) 0.111(3) Uani 1 1 d . . . . . H3 H 0.348851 0.333954 0.092337 0.133 Uiso 1 1 calc R U . . . C6 C 0.3721(6) -0.0617(5) 0.2377(4) 0.132(3) Uani 1 1 d . . . . . H6 H 0.370336 -0.090613 0.280771 0.159 Uiso 1 1 calc R U . . . C5 C 0.3231(6) 0.0055(6) 0.2218(6) 0.150(4) Uani 1 1 d . . . . . H5 H 0.281830 0.029043 0.251139 0.180 Uiso 1 1 calc R U . . . C15A C 0.4072(4) 0.1567(4) -0.0303(4) 0.0772(18) Uani 0.871(8) 1 d . . P A 1 H15A H 0.450963 0.183590 -0.006146 0.093 Uiso 0.871(8) 1 calc R U P A 1 N7A N 0.4099(3) 0.1453(4) -0.0992(3) 0.0860(14) Uani 0.871(8) 1 d . . P A 1 N8A N 0.3405(3) 0.1286(3) 0.0033(3) 0.0898(15) Uani 0.871(8) 1 d . . P A 1 C16A C 0.3321(7) 0.1152(10) -0.1154(5) 0.152(6) Uani 0.871(8) 1 d . . P A 1 C17A C 0.2901(8) 0.1035(11) -0.0534(7) 0.174(7) Uani 0.871(8) 1 d . . P A 1 C8A C 0.0437(5) 0.1534(4) 0.1142(3) 0.0873(11) Uiso 0.604(8) 1 d . . P B 1 H8A H -0.011889 0.135474 0.107167 0.105 Uiso 0.604(8) 1 calc R U P B 1 C9A C 0.1163(4) 0.1067(4) 0.1009(3) 0.0873(11) Uiso 0.604(8) 1 d . . P B 1 H9A H 0.118098 0.052142 0.084096 0.105 Uiso 0.604(8) 1 calc R U P B 1 C15B C 0.3835(14) 0.1780(16) -0.0387(10) 0.078(6) Uiso 0.129(8) 1 d D . P A 2 H15B H 0.394837 0.233135 -0.026560 0.094 Uiso 0.129(8) 1 calc R U P A 2 N8B N 0.3405(3) 0.1286(3) 0.0033(3) 0.0898(15) Uani 0.129(8) 1 d D . P A 2 N7B N 0.4099(3) 0.1453(4) -0.0992(3) 0.0860(14) Uani 0.129(8) 1 d D . P A 2 C9B C 0.1163(4) 0.1067(4) 0.1009(3) 0.0873(11) Uiso 0.396(8) 1 d . . P B 2 C8B C 0.0437(5) 0.1534(4) 0.1142(3) 0.0873(11) Uiso 0.396(8) 1 d . . P B 2 C13 C -0.0351(11) 0.1259(10) 0.0961(9) 0.0873(11) Uiso 0.396(8) 1 d . . P B 2 H13 H -0.083058 0.158227 0.104917 0.105 Uiso 0.396(8) 1 calc R U P B 2 C10 C 0.1120(11) 0.0310(10) 0.0653(9) 0.0873(11) Uiso 0.396(8) 1 d . . P B 2 H10 H 0.160678 0.001029 0.053896 0.105 Uiso 0.396(8) 1 calc R U P B 2 C11 C 0.0318(10) 0.0022(11) 0.0475(9) 0.0873(11) Uiso 0.396(8) 1 d . . P B 2 H11 H 0.026891 -0.048588 0.023846 0.105 Uiso 0.396(8) 1 calc R U P B 2 C12 C -0.0420(11) 0.0466(10) 0.0636(9) 0.0873(11) Uiso 0.396(8) 1 d . . P B 2 C14 C -0.108(2) 0.005(2) 0.052(2) 0.0873(11) Uiso 0.169(14) 1 d . . P B 2 C16B C 0.376(2) 0.0452(14) -0.0919(15) 0.078(6) Uiso 0.129(8) 1 d G . P A 2 C17B C 0.333(2) 0.0387(15) -0.0269(14) 0.078(6) Uiso 0.129(8) 1 d G . P A 2 C18 C 0.2989(19) -0.0372(18) -0.0059(12) 0.078(6) Uiso 0.129(8) 1 d G . P A 2 C19 C 0.3071(19) -0.1067(14) -0.0498(15) 0.078(6) Uiso 0.129(8) 1 d G . P A 2 C20 C 0.350(2) -0.1002(14) -0.1148(14) 0.078(6) Uiso 0.129(8) 1 d G . P A 2 C21 C 0.3842(19) -0.0243(17) -0.1358(12) 0.078(6) Uiso 0.129(8) 1 d G . P A 2 C1S C 0.159(2) 0.1735(19) 0.3277(12) 0.434(11) Uiso 0.912(17) 1 d D . P . . O1S O 0.0983(16) 0.0991(16) 0.3082(11) 0.434(11) Uiso 0.912(17) 1 d D . P . . N1S N 0.1418(18) 0.1460(17) 0.4216(12) 0.434(11) Uiso 0.912(17) 1 d D . P . . C2S C 0.2565(19) 0.145(3) 0.4194(15) 0.434(11) Uiso 0.912(17) 1 d D . P . . C3S C 0.115(2) 0.250(2) 0.4367(19) 0.434(11) Uiso 0.912(17) 1 d D . P . . C5S C 0.174(2) 0.2739(17) 0.3802(19) 0.434(11) Uiso 0.912(17) 1 d D . P . . C4S C 0.266(2) 0.135(3) 0.5017(15) 0.434(11) Uiso 0.912(17) 1 d D . P . . H16A H 0.284(7) 0.122(6) -0.174(6) 0.15(4) Uiso 0.871(8) 1 d . . P . . H17A H 0.214(6) 0.103(6) -0.043(5) 0.13(3) Uiso 0.871(8) 1 d . . 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 0.0649(5) 0.0732(5) 0.0860(6) -0.0076(3) 0.0004(3) 0.0056(3) Zn2 0.0631(5) 0.0745(5) 0.0797(5) -0.0015(3) -0.0061(3) 0.0004(3) N2 0.082(3) 0.077(3) 0.074(3) 0.008(2) -0.010(2) 0.001(2) N5 0.064(3) 0.073(3) 0.084(3) -0.005(2) 0.001(2) 0.004(2) N4 0.077(3) 0.076(3) 0.094(3) 0.000(3) 0.005(3) 0.009(2) N6 0.064(2) 0.074(3) 0.085(3) -0.006(2) 0.005(2) 0.000(2) N3 0.071(3) 0.074(3) 0.089(3) 0.004(2) 0.003(2) 0.007(2) N1 0.074(3) 0.071(3) 0.077(3) -0.001(2) -0.009(2) -0.002(2) C4 0.078(3) 0.075(3) 0.084(4) 0.000(3) 0.004(3) 0.010(3) C1 0.075(3) 0.071(3) 0.080(3) 0.000(3) -0.010(3) -0.002(3) C2 0.126(6) 0.075(4) 0.111(5) 0.017(4) -0.047(5) -0.008(4) C7 0.066(3) 0.070(3) 0.082(3) -0.005(3) 0.007(3) -0.003(2) C3 0.148(7) 0.085(4) 0.101(5) 0.011(4) -0.056(5) -0.003(4) C6 0.174(9) 0.114(6) 0.108(5) 0.041(5) 0.049(6) 0.058(6) C5 0.168(8) 0.116(6) 0.166(8) 0.038(6) 0.096(7) 0.055(6) C15A 0.065(4) 0.082(4) 0.085(4) 0.006(3) -0.010(3) 0.005(3) N7A 0.069(3) 0.107(4) 0.082(3) -0.016(3) 0.004(2) -0.011(3) N8A 0.070(3) 0.111(4) 0.088(3) -0.026(3) 0.014(3) -0.016(3) C16A 0.115(7) 0.249(15) 0.092(6) -0.040(7) 0.012(5) -0.090(9) C17A 0.109(7) 0.285(18) 0.129(8) -0.074(10) 0.032(7) -0.099(10) N8B 0.070(3) 0.111(4) 0.088(3) -0.026(3) 0.014(3) -0.016(3) N7B 0.069(3) 0.107(4) 0.082(3) -0.016(3) 0.004(2) -0.011(3) 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 N4 Zn1 N8B 109.9(2) . . N4 Zn1 N8A 109.9(2) . . N4 Zn1 N1 108.0(2) . . N8B Zn1 N1 110.3(2) . . N8A Zn1 N1 110.3(2) . . N4 Zn1 N5 111.3(2) . . N8B Zn1 N5 110.5(2) . . N8A Zn1 N5 110.5(2) . . N1 Zn1 N5 106.76(19) . . N6 Zn2 N2 111.5(2) 6_656 . N6 Zn2 N7A 111.0(2) 6_656 8_566 N2 Zn2 N7A 108.3(2) . 8_566 N6 Zn2 N3 106.40(19) 6_656 4_655 N2 Zn2 N3 109.7(2) . 4_655 N7A Zn2 N3 109.9(2) 8_566 4_655 C1 N2 C2 104.3(5) . . C1 N2 Zn2 126.4(4) . . C2 N2 Zn2 129.1(4) . . C7 N5 C9B 104.8(5) . . C7 N5 C9A 104.8(5) . . C7 N5 Zn1 124.3(4) . . C9B N5 Zn1 130.8(4) . . C9A N5 Zn1 130.8(4) . . C4 N4 C5 103.2(5) . . C4 N4 Zn1 127.7(4) . . C5 N4 Zn1 128.5(5) . . C7 N6 C8B 104.6(5) . . C7 N6 C8A 104.6(5) . . C7 N6 Zn2 124.3(4) . 6_556 C8A N6 Zn2 131.1(4) . 6_556 C6 N3 C4 103.8(5) . . C6 N3 Zn2 130.1(5) . 4_645 C4 N3 Zn2 126.0(4) . 4_645 C1 N1 C3 104.0(5) . . C1 N1 Zn1 125.4(4) . . C3 N1 Zn1 130.4(4) . . N3 C4 N4 114.5(5) . . N2 C1 N1 113.8(5) . . C3 C2 N2 108.3(6) . . N5 C7 N6 114.4(5) . . N1 C3 C2 109.6(6) . . N3 C6 C5 110.6(7) . . N4 C5 C6 107.8(7) . . N7A C15A N8A 117.0(6) . . C15A N7A C16A 104.1(6) . . C15A N7A Zn2 131.4(5) . 8_565 C16A N7A Zn2 124.2(5) . 8_565 C15A N8A C17A 101.1(6) . . C15A N8A Zn1 130.1(5) . . C17A N8A Zn1 128.1(5) . . C17A C16A N7A 107.5(8) . . C16A C17A N8A 109.7(8) . . N6 C8A C9A 108.9(6) . . N5 C9A C8A 107.2(6) . . N8B C15B N7B 116(2) . . C15B N8B C17B 112.5(15) . . C15B N8B Zn1 132.5(11) . . C17B N8B Zn1 112.7(11) . . C15B N7B C16B 102.1(15) . . N5 C9B C10 130.5(9) . . N5 C9B C8B 107.2(6) . . C10 C9B C8B 121.2(9) . . N6 C8B C13 128.6(10) . . N6 C8B C9B 108.9(6) . . C13 C8B C9B 122.1(9) . . C8B C13 C12 118.0(15) . . C11 C10 C9B 116.9(14) . . C10 C11 C12 122.4(16) . . C14 C12 C11 112(2) . . C14 C12 C13 128(2) . . C11 C12 C13 119.3(16) . . C17B C16B C21 120.0 . . C17B C16B N7B 107.0(16) . . C21 C16B N7B 133.0(16) . . C18 C17B C16B 120.0 . . C18 C17B N8B 137.7(17) . . C16B C17B N8B 102.3(17) . . C17B C18 C19 120.0 . . C17B C18 C4S 165.0(19) . 2_554 C19 C18 C4S 54.9(15) . 2_554 N1S C19 C2S 94(2) 2_554 2_554 N1S C19 C18 141(2) 2_554 . C2S C19 C18 124(3) 2_554 . N1S C19 C20 46(2) 2_554 . C2S C19 C20 91(2) 2_554 . C18 C19 C20 120.0 . . N1S C19 C4S 130(2) 2_554 2_554 C2S C19 C4S 64.8(16) 2_554 2_554 C18 C19 C4S 78(2) . 2_554 C20 C19 C4S 156(2) . 2_554 N1S C20 C21 141(3) 2_554 . N1S C20 C19 55(2) 2_554 . C21 C20 C19 120.0 . . N1S C20 C1S 85.9(19) 2_554 2_554 N1S C20 O1S 122(3) 2_554 2_554 C1S C20 O1S 57.7(11) 2_554 2_554 N1S C20 C2S 68(2) 2_554 2_554 C1S C20 C2S 82.8(17) 2_554 2_554 O1S C20 C2S 136(2) 2_554 2_554 C20 C21 C16B 120.0 . . O1S C1S C20 63(4) . 2 O1S C1S N1S 87.1(13) . . C20 C1S N1S 33(5) 2 . O1S C1S C5S 147(2) . . C20 C1S C5S 107(4) 2 . N1S C1S C5S 74.3(11) . . C1S O1S C21 108(4) . 2 C1S O1S C20 59(5) . 2 C20 N1S C3S 147(4) 2 . C19 N1S C3S 128(7) 2 . C20 N1S C2S 81(9) 2 . C19 N1S C2S 46(8) 2 . C3S N1S C2S 105(2) . . C20 N1S C1S 61(5) 2 . C19 N1S C1S 118(7) 2 . C3S N1S C1S 87.7(12) . . C2S N1S C1S 80.3(12) . . C19 C2S C4S 66(3) 2 . C19 C2S N1S 40(6) 2 . C4S C2S N1S 94.2(15) . . C4S C2S C20 112(3) . 2 N1S C2S C20 31(5) . 2 C5S C3S N1S 89.0(14) . . C3S C5S C1S 93.8(14) . . C2S C4S C19 50(5) . 2 C2S C4S C18 88(2) . 2 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Zn1 N4 1.984(5) . Zn1 N8B 1.985(5) . Zn1 N8A 1.985(5) . Zn1 N1 1.992(4) . Zn1 N5 1.999(4) . Zn2 N6 1.983(4) 6_656 Zn2 N2 1.990(5) . Zn2 N7A 1.991(5) 8_566 Zn2 N3 1.994(5) 4_655 N2 C1 1.320(7) . N2 C2 1.355(8) . N5 C7 1.321(7) . N5 C9B 1.375(8) . N5 C9A 1.375(8) . N4 C4 1.330(7) . N4 C5 1.342(9) . N6 C7 1.338(7) . N6 C8B 1.348(8) . N6 C8A 1.348(8) . N3 C6 1.301(8) . N3 C4 1.318(7) . N1 C1 1.335(7) . N1 C3 1.336(8) . C2 C3 1.351(9) . C6 C5 1.358(11) . C15A N7A 1.299(8) . C15A N8A 1.304(8) . N7A C16A 1.350(11) . N8A C17A 1.383(12) . C16A C17A 1.346(13) . C8A C9A 1.389(9) . C15B N8B 1.31(2) . C15B N7B 1.31(2) . N8B C17B 1.55(2) . N7B C16B 1.70(2) . C9B C10 1.385(17) . C9B C8B 1.389(9) . C8B C13 1.359(19) . C13 C12 1.41(2) . C10 C11 1.39(2) . C11 C12 1.39(2) . C11 C11 2.04(3) 5 C12 C14 1.26(4) . C16B C17B 1.3900 . C16B C21 1.3900 . C17B C18 1.3900 . C18 C19 1.3900 . C18 C4S 1.87(5) 2_554 C19 N1S 1.15(4) 2_554 C19 C2S 1.31(4) 2_554 C19 C20 1.3900 . C19 C4S 1.57(3) 2_554 C20 N1S 1.01(4) 2_554 C20 C21 1.3900 . C20 C1S 1.60(3) 2_554 C20 O1S 1.65(3) 2_554 C20 C2S 1.93(4) 2_554 C21 O1S 1.62(3) 2_554 C1S O1S 1.572(16) . C1S N1S 1.829(14) . C1S C5S 1.90(3) . N1S C3S 1.741(16) . N1S C2S 1.806(16) . C2S C4S 1.554(19) . C3S C5S 1.460(19) .