#------------------------------------------------------------------------------ #$Date: 2019-12-13 04:34:02 +0200 (Fri, 13 Dec 2019) $ #$Revision: 245036 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/29/7702945.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_7702945 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 C7.29 N4 H6.85)*0.44(C5 N1 O1 H11)' _chemical_formula_sum 'C18.98 H23.37 N8.88 O0.88 Zn2' _chemical_formula_weight 520.78 _chemical_name_common 'Zinc (imdazolate, benzimidazolate, 5-methyl-benzimidazolate) solid solution' _chemical_name_systematic ZIF-UC-1f _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 15.9807(11) _cell_length_b 18.5721(16) _cell_length_c 15.6944(8) _cell_measurement_reflns_used 3537 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 63.2460 _cell_measurement_theta_min 2.7650 _cell_volume 4658.0(6) _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_area_resol_mean 16.1183 _diffrn_measured_fraction_theta_full 0.9258 _diffrn_measured_fraction_theta_max 0.9903 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -6.00 91.00 1.0000 10.7200 omega____ theta____ kappa____ phi______ frames - 51.2500 -77.0000 0.0000 97 #__ type_ start__ end____ width___ exp.time_ 2 omega 41.00 79.00 1.0000 10.7200 omega____ theta____ kappa____ phi______ frames - 102.5000 -54.0000 -90.0000 38 #__ type_ start__ end____ width___ exp.time_ 3 omega 43.00 88.00 1.0000 10.7200 omega____ theta____ kappa____ phi______ frames - 102.5000 -54.0000 -60.0000 45 #__ type_ start__ end____ width___ exp.time_ 4 omega 115.00 141.00 1.0000 10.7200 omega____ theta____ kappa____ phi______ frames - 102.5000 -21.0000 0.0000 26 #__ type_ start__ end____ width___ exp.time_ 5 omega 112.00 150.00 1.0000 10.7200 omega____ theta____ kappa____ phi______ frames - 102.5000 -21.0000 30.0000 38 #__ type_ start__ end____ width___ exp.time_ 6 omega 119.00 174.00 1.0000 10.7200 omega____ theta____ kappa____ phi______ frames - 102.5000 -21.0000 90.0000 55 #__ type_ start__ end____ width___ exp.time_ 7 omega 136.00 162.00 1.0000 10.7200 omega____ theta____ kappa____ phi______ frames - 102.5000 32.0000 150.0000 26 #__ type_ start__ end____ width___ exp.time_ 8 omega 97.00 129.00 1.0000 10.7200 omega____ theta____ kappa____ phi______ frames - 51.2500 125.0000 60.0000 32 #__ type_ start__ end____ width___ exp.time_ 9 omega 82.00 111.00 1.0000 10.7200 omega____ theta____ kappa____ phi______ frames - 51.2500 125.0000 30.0000 29 #__ type_ start__ end____ width___ exp.time_ 10 omega 73.00 131.00 1.0000 10.7200 omega____ theta____ kappa____ phi______ frames - 51.2500 125.0000 -30.0000 58 #__ type_ start__ end____ width___ exp.time_ 11 omega 97.00 126.00 1.0000 10.7200 omega____ theta____ kappa____ phi______ frames - 51.2500 125.0000 -120.0000 29 #__ type_ start__ end____ width___ exp.time_ 12 omega 44.00 72.00 1.0000 2.6800 omega____ theta____ kappa____ phi______ frames - 0.0000 178.0000 30.0000 28 #__ type_ start__ end____ width___ exp.time_ 13 omega 58.00 83.00 1.0000 10.7200 omega____ theta____ kappa____ phi______ frames - 102.5000 -104.0000 30.0000 25 #__ type_ start__ end____ width___ exp.time_ 14 omega 43.00 69.00 1.0000 10.7200 omega____ theta____ kappa____ phi______ frames - 102.5000 -54.0000 60.0000 26 #__ type_ start__ end____ width___ exp.time_ 15 omega 28.00 64.00 1.0000 10.7200 omega____ theta____ kappa____ phi______ frames - 102.5000 -54.0000 90.0000 36 #__ type_ start__ end____ width___ exp.time_ 16 omega 25.00 69.00 1.0000 10.7200 omega____ theta____ kappa____ phi______ frames - 102.5000 -32.0000 90.0000 44 #__ type_ start__ end____ width___ exp.time_ 17 omega 56.00 81.00 1.0000 10.7200 omega____ theta____ kappa____ phi______ frames - 102.5000 32.0000 150.0000 25 #__ type_ start__ end____ width___ exp.time_ 18 omega 25.00 65.00 1.0000 10.7200 omega____ theta____ kappa____ phi______ frames - 102.5000 -43.0000 150.0000 40 #__ type_ start__ end____ width___ exp.time_ 19 omega 33.00 59.00 1.0000 10.7200 omega____ theta____ kappa____ phi______ frames - 102.5000 -32.0000 0.0000 26 #__ type_ start__ end____ width___ exp.time_ 20 omega 131.00 178.00 1.0000 10.7200 omega____ theta____ kappa____ phi______ frames - 102.5000 -21.0000 -150.0000 47 #__ type_ start__ end____ width___ exp.time_ 21 omega 45.00 71.00 1.0000 2.6800 omega____ theta____ kappa____ phi______ frames - 0.0000 178.0000 -30.0000 26 #__ type_ start__ end____ width___ exp.time_ 22 omega 45.00 88.00 1.0000 2.6800 omega____ theta____ kappa____ phi______ frames - 0.0000 178.0000 -180.0000 43 #__ type_ start__ end____ width___ exp.time_ 23 omega 22.00 60.00 1.0000 10.7200 omega____ theta____ kappa____ phi______ frames - 102.5000 -32.0000 -180.0000 38 ; _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0436189000 _diffrn_orient_matrix_UB_12 0.0319775000 _diffrn_orient_matrix_UB_13 0.0790202000 _diffrn_orient_matrix_UB_21 -0.0499776000 _diffrn_orient_matrix_UB_22 0.0702374000 _diffrn_orient_matrix_UB_23 -0.0112726000 _diffrn_orient_matrix_UB_31 -0.0700653000 _diffrn_orient_matrix_UB_32 -0.0302378000 _diffrn_orient_matrix_UB_33 0.0571008000 _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0232 _diffrn_reflns_av_unetI/netI 0.0252 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 10732 _diffrn_reflns_theta_full 66.9682 _diffrn_reflns_theta_max 64.1320 _diffrn_reflns_theta_min 2.3789 _diffrn_source 'sealed X-ray tube' _exptl_absorpt_coefficient_mu 2.76 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.63649 _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 1.481 _exptl_crystal_description equant _exptl_crystal_F_000 2377.52 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.970 _refine_diff_density_min -0.378 _refine_diff_density_rms 0.095 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 267 _refine_ls_number_reflns 3844 _refine_ls_number_restraints 19 _refine_ls_restrained_S_all 1.321 _refine_ls_R_factor_all 0.0964 _refine_ls_R_factor_gt 0.0820 _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^)+(0.1253P)^2^+14.1104P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2416 _refine_ls_wR_factor_ref 0.2590 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3025 _reflns_number_total 3844 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9dt03559a2.cif _cod_data_source_block shelx_CCDC1 _cod_original_formula_sum 'Zn2 C18.98 H23.37 N8.88 O.88' _cod_database_code 7702945 _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 92.58 _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 10:50:11 on 26-Jul-2019 CELL 1.54184 15.9807 18.5721 15.6944 90.000 90.000 90.000 ZERR 8.00 0.0011 0.0016 0.0008 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 64 0 104 16 1 MERG 2 EXYZ C8a C8b EXYZ C9a C9b EADP C8a C8b EADP C9a C9b EXYZ C17 C17B EXYZ C16 C16B EXYZ C20 C20B EXYZ C21 C21B EXYZ C19 C19B EXYZ C18 C18B FLAT C21B C20B C19B C18B DFIX 1.31 0.020 C15A N7 DFIX 1.31 0.020 C15A N8 DANG 2.10 0.030 C15A N7 C15A C16A DANG 2.10 0.030 C15A N8 C15A C17A DFIX 1.31 0.020 C15B N7 DFIX 1.31 0.020 C15B N8 DANG 2.10 0.030 C15B N7 C15B C16 DANG 2.10 0.030 C15B N8 C15B C17 FLAT 0.100 C15A N7 N8 C17A C16A FLAT 0.100 C15B N7 N8 C17 C16 DFIX 1.32 0.020 N1S C1S DFIX 1.47 0.020 N1S C2S DFIX 1.52 0.020 C2S C4S DFIX 1.25 0.020 C1S O1S EADP C13 C12 C11 C10 C14 EADP C1S C2S C4S C3S C5S N1S O1S EADP C15B C17B C16B C20B C21B C19B C18B C22 FMAP 2 PLAN 20 ACTA 50.00 L.S. 50 WGHT 0.125300 14.110400 EXTI 0.000205 FVAR 2.15178 0.45952 0.11912 0.88017 0.14850 ZN1 4 0.135545 0.104855 0.192838 11.00000 0.08128 0.09437 = 0.06376 0.00040 -0.00631 -0.00926 ZN2 4 0.327586 0.173644 0.503157 11.00000 0.08167 0.08896 = 0.06127 -0.00642 -0.00039 0.00060 N5 3 0.157075 0.116406 0.317426 11.00000 0.08164 0.09251 = 0.06624 0.00218 -0.00500 -0.01028 N6 3 0.230618 0.139564 0.434606 11.00000 0.08746 0.09432 = 0.05838 -0.00830 0.00091 -0.00566 N7 3 0.125217 0.003064 0.163682 -31.00000 0.11670 0.08908 = 0.06221 -0.01293 0.01901 -0.03630 N3 3 0.032818 0.157812 0.157445 11.00000 0.08245 0.09940 = 0.07660 -0.01160 -0.00641 0.00413 N2 3 0.302570 0.233988 0.060803 11.00000 0.07789 0.08820 = 0.07865 0.01924 0.00365 0.00683 N8 3 0.142087 -0.104299 0.091273 -31.00000 0.11214 0.08991 = 0.06153 -0.00756 0.01408 -0.01977 N1 3 0.230995 0.149962 0.131782 11.00000 0.07889 0.08958 = 0.07764 0.01383 0.00103 0.00385 N4 3 -0.078573 0.186319 0.078243 11.00000 0.07812 0.09615 = 0.06822 -0.00465 -0.00428 0.00311 C4 1 -0.020383 0.137074 0.096195 11.00000 0.08036 0.09661 = 0.07334 0.00325 -0.01403 0.00785 AFIX 43 H4 2 -0.017079 0.092726 0.068883 11.00000 -1.20000 AFIX 0 C3 1 0.356350 0.178942 0.081192 11.00000 0.08375 0.13930 = 0.14006 0.06226 0.01159 0.01947 AFIX 43 H3 2 0.413010 0.176676 0.067939 11.00000 -1.20000 AFIX 0 C1 1 0.230041 0.213321 0.091176 11.00000 0.07988 0.08957 = 0.07126 0.00493 -0.00372 0.01051 AFIX 43 H1 2 0.181620 0.240600 0.084982 11.00000 -1.20000 AFIX 0 C7 1 0.228568 0.138672 0.350616 11.00000 0.07454 0.08910 = 0.06894 -0.00473 -0.00181 -0.00552 AFIX 43 H7 2 0.273895 0.152622 0.317319 11.00000 -1.20000 AFIX 0 C2 1 0.312468 0.129223 0.123540 11.00000 0.08993 0.12419 = 0.16388 0.07718 0.01334 0.02051 AFIX 43 H2 2 0.334459 0.086379 0.144503 11.00000 -1.20000 AFIX 0 C5 1 -0.058998 0.241637 0.127580 11.00000 0.12938 0.14954 = 0.16031 -0.06649 -0.05534 0.05172 AFIX 43 H5 2 -0.085682 0.286136 0.128024 11.00000 -1.20000 AFIX 0 C6 1 0.007320 0.222094 0.177883 11.00000 0.12026 0.18989 = 0.15222 -0.08661 -0.05429 0.03892 AFIX 43 H6 2 0.030687 0.250593 0.220402 11.00000 -1.20000 AFIX 0 PART 1 C9A 1 0.108421 0.100203 0.386336 -21.00000 0.07966 0.13806 = 0.07474 -0.01428 0.00568 -0.02033 AFIX 43 H9A 2 0.054319 0.081793 0.384934 -21.00000 -1.20000 AFIX 0 C8A 1 0.153942 0.116045 0.457961 -21.00000 0.09148 0.12192 = 0.06466 -0.00787 0.00791 -0.01644 AFIX 43 H8A 2 0.135066 0.111356 0.513739 -21.00000 -1.20000 AFIX 0 C15A 1 0.154457 -0.030922 0.093148 -31.00000 0.07650 0.09890 = 0.05835 0.01532 -0.00063 0.01376 AFIX 43 H15A 2 0.181001 -0.006369 0.049140 -31.00000 -1.20000 AFIX 0 C17A 1 0.114542 -0.118269 0.168747 -31.00000 0.35984 0.10669 = 0.14178 -0.03658 0.13942 -0.05366 AFIX 43 H17A 2 0.105584 -0.163734 0.191847 -31.00000 -1.20000 AFIX 0 C16A 1 0.101167 -0.052257 0.210101 -31.00000 0.45481 0.15098 = 0.17264 -0.08825 0.19495 -0.14349 AFIX 43 H16A 2 0.077931 -0.048059 0.264202 -31.00000 -1.20000 AFIX 0 PART 2 C9B 1 0.108421 0.100203 0.386336 21.00000 0.07966 0.13806 = 0.07474 -0.01428 0.00568 -0.02033 C8B 1 0.153942 0.116045 0.457961 21.00000 0.09148 0.12192 = 0.06466 -0.00787 0.00791 -0.01644 C13 1 0.127556 0.096977 0.539959 21.00000 0.10129 AFIX 43 H13 2 0.161141 0.104262 0.587578 21.00000 -1.20000 AFIX 0 C10 1 0.033200 0.061984 0.389867 21.00000 0.10129 AFIX 43 H10 2 0.003530 0.049377 0.341122 21.00000 -1.20000 AFIX 0 C11 1 0.005402 0.043876 0.472118 21.00000 0.10129 AFIX 43 H11 2 -0.042685 0.016090 0.477841 21.00000 -1.20000 AFIX 0 C12 1 0.047883 0.066370 0.546241 21.00000 0.10129 C14 1 0.019201 0.062170 0.625318 51.00000 0.10129 PART 4 C17 1 0.041717 -0.096125 0.119648 30.00000 10.05000 C16 1 0.032305 -0.030184 0.162238 30.00000 10.05000 C21 1 -0.040013 -0.007632 0.206621 30.00000 10.05000 C20 1 -0.108119 -0.054884 0.197721 30.00000 10.05000 C19 1 -0.095828 -0.122109 0.154238 30.00000 10.05000 C18 1 -0.024597 -0.144142 0.119142 30.00000 10.05000 PART 5 C15B 1 0.194474 -0.038774 0.119535 31.00000 0.04694 AFIX 43 H15B 2 0.250858 -0.028175 0.111931 31.00000 -1.20000 AFIX 0 C17B 1 0.041717 -0.096125 0.119648 31.00000 0.04694 C16B 1 0.032305 -0.030184 0.162238 31.00000 0.04694 C21B 1 -0.040013 -0.007632 0.206621 31.00000 0.04694 C20B 1 -0.108119 -0.054884 0.197721 31.00000 0.04694 C19B 1 -0.095828 -0.122109 0.154238 31.00000 0.04694 C18B 1 -0.024597 -0.144142 0.119142 31.00000 0.04694 C22 1 -0.168228 -0.184866 0.159897 31.00000 0.04694 PART 6 N1S 3 -0.209512 -0.079930 0.134052 41.00000 0.48514 C1S 1 -0.148079 -0.090749 0.190652 41.00000 0.48514 C2S 1 -0.124665 -0.111504 0.114649 41.00000 0.48514 C3S 1 -0.134967 -0.089638 0.316841 41.00000 0.48514 C4S 1 -0.092116 -0.186309 0.093618 41.00000 0.48514 O1S 5 -0.125182 -0.036885 0.234936 41.00000 0.48514 C5S 1 -0.211951 -0.155131 0.193615 41.00000 0.48514 HKLF 4 REM CF solution in Pbca REM wR2 = 0.2590, GooF = S = 1.056, Restrained GooF = 1.321 for all data REM R1 = 0.0820 for 3025 Fo > 4sig(Fo) and 0.0964 for all 3844 data REM 267 parameters refined using 19 restraints END WGHT 0.1250 14.1094 REM Highest difference peak 0.970, deepest hole -0.378, 1-sigma level 0.095 Q1 1 -0.0910 -0.2032 0.0986 11.00000 0.05 0.97 Q2 1 -0.2932 -0.0858 0.0996 11.00000 0.05 0.64 Q3 1 0.1986 0.1080 0.1868 11.00000 0.05 0.62 Q4 1 0.2660 0.1715 0.5017 11.00000 0.05 0.54 Q5 1 -0.1337 -0.0494 0.3222 11.00000 0.05 0.52 Q6 1 0.1524 -0.0706 0.1015 11.00000 0.05 0.52 Q7 1 0.3923 0.1731 0.4984 11.00000 0.05 0.51 Q8 1 0.1490 -0.0195 0.1373 11.00000 0.05 0.49 Q9 1 0.1286 0.0169 0.1377 11.00000 0.05 0.41 Q10 1 -0.1551 -0.1185 0.1806 11.00000 0.05 0.40 Q11 1 0.0743 0.1080 0.1812 11.00000 0.05 0.40 Q12 1 -0.0960 -0.1175 0.0849 11.00000 0.05 0.39 Q13 1 0.1236 -0.0613 0.2219 11.00000 0.05 0.39 Q14 1 0.1784 0.0737 0.1404 11.00000 0.05 0.34 Q15 1 -0.1262 0.1981 0.0474 11.00000 0.05 0.32 Q16 1 0.1374 0.1020 0.2771 11.00000 0.05 0.30 Q17 1 -0.1602 -0.1877 0.1924 11.00000 0.05 0.30 Q18 1 0.1351 -0.1266 0.1783 11.00000 0.05 0.28 Q19 1 0.0405 -0.0795 0.1252 11.00000 0.05 0.28 Q20 1 -0.1574 0.0002 0.2634 11.00000 0.05 0.28 ; _shelx_res_checksum 45243 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 0.13555(7) 0.10485(6) 0.19284(6) 0.0798(4) Uani 1 1 d . . . . . Zn2 Zn 0.32759(7) 0.17364(6) 0.50316(6) 0.0773(4) Uani 1 1 d . . . . . N5 N 0.1571(4) 0.1164(4) 0.3174(4) 0.0801(18) Uani 1 1 d . . . . . N6 N 0.2306(4) 0.1396(4) 0.4346(4) 0.0801(17) Uani 1 1 d . . . . . N7 N 0.1252(5) 0.0031(4) 0.1637(4) 0.089(3) Uani 0.881(9) 1 d D . P . . N3 N 0.0328(4) 0.1578(4) 0.1574(4) 0.0861(18) Uani 1 1 d . . . . . N2 N 0.3026(4) 0.2340(4) 0.0608(4) 0.0816(17) Uani 1 1 d . . . . . N8 N 0.1421(5) -0.1043(4) 0.0913(5) 0.088(2) Uani 0.881(9) 1 d D . P . . N1 N 0.2310(4) 0.1500(4) 0.1318(4) 0.0820(17) Uani 1 1 d . . . . . N4 N -0.0786(4) 0.1863(4) 0.0782(4) 0.0808(17) Uani 1 1 d . . . . . C4 C -0.0204(5) 0.1371(5) 0.0962(5) 0.083(2) Uani 1 1 d . . . . . H4 H -0.017079 0.092726 0.068883 0.100 Uiso 1 1 calc R U . . . C3 C 0.3563(6) 0.1789(6) 0.0812(8) 0.121(4) Uani 1 1 d . . . . . H3 H 0.413010 0.176676 0.067939 0.145 Uiso 1 1 calc R U . . . C1 C 0.2300(5) 0.2133(5) 0.0912(5) 0.080(2) Uani 1 1 d . . . . . H1 H 0.181620 0.240600 0.084982 0.096 Uiso 1 1 calc R U . . . C7 C 0.2286(5) 0.1387(4) 0.3506(5) 0.078(2) Uani 1 1 d . . . . . H7 H 0.273895 0.152622 0.317319 0.093 Uiso 1 1 calc R U . . . C2 C 0.3125(6) 0.1292(6) 0.1235(8) 0.126(4) Uani 1 1 d . . . . . H2 H 0.334459 0.086379 0.144503 0.151 Uiso 1 1 calc R U . . . C5 C -0.0590(7) 0.2416(7) 0.1276(9) 0.146(5) Uani 1 1 d . . . . . H5 H -0.085682 0.286136 0.128024 0.176 Uiso 1 1 calc R U . . . C6 C 0.0073(8) 0.2221(8) 0.1779(9) 0.154(6) Uani 1 1 d . . . . . H6 H 0.030687 0.250593 0.220402 0.185 Uiso 1 1 calc R U . . . C9A C 0.1084(6) 0.1002(6) 0.3863(6) 0.097(3) Uani 0.540(14) 1 d . . P A 1 H9A H 0.054319 0.081793 0.384934 0.117 Uiso 0.540(14) 1 calc R U P A 1 C8A C 0.1539(6) 0.1160(6) 0.4580(5) 0.093(3) Uani 0.540(14) 1 d . . P A 1 H8A H 0.135066 0.111356 0.513739 0.111 Uiso 0.540(14) 1 calc R U P A 1 C15A C 0.1545(5) -0.0309(5) 0.0931(5) 0.078(2) Uani 0.881(9) 1 d D . P B 1 H15A H 0.181001 -0.006369 0.049140 0.094 Uiso 0.881(9) 1 calc R U P B 1 C17A C 0.1145(15) -0.1183(8) 0.1687(10) 0.203(12) Uani 0.881(9) 1 d D . P B 1 H17A H 0.105584 -0.163734 0.191847 0.243 Uiso 0.881(9) 1 calc R U P B 1 C16A C 0.1012(17) -0.0523(9) 0.2101(11) 0.259(17) Uani 0.881(9) 1 d D . P B 1 H16A H 0.077931 -0.048059 0.264202 0.311 Uiso 0.881(9) 1 calc R U P B 1 C9B C 0.1084(6) 0.1002(6) 0.3863(6) 0.097(3) Uani 0.460(14) 1 d . . P A 2 C8B C 0.1539(6) 0.1160(6) 0.4580(5) 0.093(3) Uani 0.460(14) 1 d . . P A 2 C13 C 0.1276(14) 0.0970(12) 0.5400(15) 0.101(4) Uiso 0.460(14) 1 d . . P A 2 H13 H 0.161141 0.104262 0.587578 0.122 Uiso 0.460(14) 1 calc R U P A 2 C10 C 0.0332(13) 0.0620(12) 0.3899(14) 0.101(4) Uiso 0.460(14) 1 d . . P A 2 H10 H 0.003530 0.049377 0.341122 0.122 Uiso 0.460(14) 1 calc R U P A 2 C11 C 0.0054(14) 0.0439(12) 0.4721(14) 0.101(4) Uiso 0.460(14) 1 d . . P A 2 H11 H -0.042685 0.016090 0.477841 0.122 Uiso 0.460(14) 1 calc R U P A 2 C12 C 0.0479(14) 0.0664(12) 0.5462(14) 0.101(4) Uiso 0.460(14) 1 d . . P A 2 C14 C 0.019(4) 0.062(4) 0.625(4) 0.101(4) Uiso 0.15(2) 1 d . . P A 2 C17 C 0.042(3) -0.096(2) 0.120(3) 0.050 Uiso 0 1 d . U P B 4 C16 C 0.032(3) -0.030(3) 0.162(3) 0.050 Uiso 0 1 d . U P B 4 C21 C -0.040(3) -0.008(2) 0.207(3) 0.050 Uiso 0 1 d . U P B 4 C20 C -0.108(3) -0.055(2) 0.198(3) 0.050 Uiso 0 1 d . U P B 4 C19 C -0.096(3) -0.122(2) 0.154(3) 0.050 Uiso 0 1 d . U P B 4 C18 C -0.025(3) -0.144(2) 0.119(3) 0.050 Uiso 0 1 d . U P B 4 C15B C 0.1945(12) -0.0388(10) 0.1195(16) 0.047(6) Uiso 0.119(9) 1 d D . P B 5 H15B H 0.250858 -0.028175 0.111931 0.056 Uiso 0.119(9) 1 calc R U P B 5 C17B C 0.042(3) -0.096(2) 0.120(3) 0.047(6) Uiso 0.119(9) 1 d . . P B 5 C16B C 0.032(3) -0.030(3) 0.162(3) 0.047(6) Uiso 0.119(9) 1 d . . P B 5 C21B C -0.040(3) -0.008(2) 0.207(3) 0.047(6) Uiso 0.119(9) 1 d . . P B 5 C20B C -0.108(3) -0.055(2) 0.198(3) 0.047(6) Uiso 0.119(9) 1 d . . P B 5 C19B C -0.096(3) -0.122(2) 0.154(3) 0.047(6) Uiso 0.119(9) 1 d . . P B 5 C18B C -0.025(3) -0.144(2) 0.119(3) 0.047(6) Uiso 0.119(9) 1 d . . P B 5 C22 C -0.168(3) -0.185(3) 0.160(3) 0.047(6) Uiso 0.119(9) 1 d . . P B 5 N1S N -0.210(3) -0.080(3) 0.134(4) 0.485(17) Uiso 0.88(2) 1 d D . P C 6 C1S C -0.148(5) -0.091(3) 0.191(5) 0.485(17) Uiso 0.88(2) 1 d D . P C 6 C2S C -0.125(4) -0.112(4) 0.115(5) 0.485(17) Uiso 0.88(2) 1 d D . P C 6 C3S C -0.135(4) -0.090(4) 0.317(5) 0.485(17) Uiso 0.88(2) 1 d . . P C 6 C4S C -0.092(4) -0.186(3) 0.094(4) 0.485(17) Uiso 0.88(2) 1 d D . P C 6 O1S O -0.125(3) -0.037(2) 0.235(4) 0.485(17) Uiso 0.88(2) 1 d D . P C 6 C5S C -0.212(4) -0.155(4) 0.194(4) 0.485(17) Uiso 0.88(2) 1 d . . P C 6 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 0.0813(7) 0.0944(8) 0.0638(6) 0.0004(5) -0.0063(5) -0.0093(5) Zn2 0.0817(8) 0.0890(8) 0.0613(6) -0.0064(5) -0.0004(4) 0.0006(5) N5 0.082(4) 0.093(5) 0.066(4) 0.002(3) -0.005(3) -0.010(3) N6 0.087(4) 0.094(4) 0.058(3) -0.008(3) 0.001(3) -0.006(4) N7 0.117(6) 0.089(5) 0.062(4) -0.013(4) 0.019(4) -0.036(5) N3 0.082(4) 0.099(5) 0.077(4) -0.012(4) -0.006(3) 0.004(4) N2 0.078(4) 0.088(4) 0.079(4) 0.019(3) 0.004(3) 0.007(3) N8 0.112(6) 0.090(5) 0.062(4) -0.008(4) 0.014(4) -0.020(4) N1 0.079(4) 0.090(4) 0.078(4) 0.014(3) 0.001(3) 0.004(3) N4 0.078(4) 0.096(5) 0.068(3) -0.005(3) -0.004(3) 0.003(4) C4 0.080(5) 0.097(6) 0.073(5) 0.003(4) -0.014(4) 0.008(4) C3 0.084(6) 0.139(9) 0.140(9) 0.062(8) 0.012(6) 0.019(6) C1 0.080(5) 0.090(5) 0.071(4) 0.005(4) -0.004(4) 0.011(4) C7 0.075(5) 0.089(5) 0.069(4) -0.005(4) -0.002(4) -0.006(4) C2 0.090(6) 0.124(8) 0.164(11) 0.077(8) 0.013(7) 0.021(6) C5 0.129(9) 0.150(10) 0.160(11) -0.066(9) -0.055(9) 0.052(8) C6 0.120(8) 0.190(14) 0.152(11) -0.087(10) -0.054(8) 0.039(9) C9A 0.080(5) 0.138(8) 0.075(5) -0.014(5) 0.006(4) -0.020(5) C8A 0.091(6) 0.122(7) 0.065(5) -0.008(5) 0.008(4) -0.016(5) C15A 0.076(5) 0.099(7) 0.058(4) 0.015(5) -0.001(4) 0.014(5) C17A 0.36(3) 0.107(11) 0.142(13) -0.037(9) 0.139(18) -0.054(14) C16A 0.45(4) 0.151(15) 0.173(16) -0.088(13) 0.19(2) -0.14(2) C9B 0.080(5) 0.138(8) 0.075(5) -0.014(5) 0.006(4) -0.020(5) C8B 0.091(6) 0.122(7) 0.065(5) -0.008(5) 0.008(4) -0.016(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 N7 Zn1 N1 111.1(3) . . N7 Zn1 N3 110.1(3) . . N1 Zn1 N3 106.9(3) . . N7 Zn1 N5 110.4(3) . . N1 Zn1 N5 107.1(3) . . N3 Zn1 N5 111.2(3) . . N8 Zn2 N2 107.3(3) 2 8_566 N8 Zn2 N4 110.3(3) 2 6_656 N2 Zn2 N4 110.1(3) 8_566 6_656 N8 Zn2 N6 111.5(3) 2 . N2 Zn2 N6 111.4(3) 8_566 . N4 Zn2 N6 106.2(3) 6_656 . C7 N5 C9B 104.4(7) . . C7 N5 C9A 104.4(7) . . C7 N5 Zn1 124.6(5) . . C9B N5 Zn1 130.8(6) . . C9A N5 Zn1 130.8(6) . . C7 N6 C8B 104.2(7) . . C7 N6 C8A 104.2(7) . . C7 N6 Zn2 124.3(6) . . C8B N6 Zn2 131.5(5) . . C8A N6 Zn2 131.5(5) . . C16A N7 C15A 100.9(9) . . C15B N7 C16B 118(2) . . C16A N7 Zn1 130.6(7) . . C15A N7 Zn1 127.8(6) . . C15B N7 Zn1 122.7(8) . . C16B N7 Zn1 116.9(18) . . C16 N7 Zn1 116.9(18) . . C6 N3 C4 104.0(8) . . C6 N3 Zn1 129.9(7) . . C4 N3 Zn1 125.5(6) . . C1 N2 C3 104.5(7) . . C1 N2 Zn2 126.8(6) . 8_565 C3 N2 Zn2 128.7(6) . 8_565 C17A N8 C15A 102.9(8) . . C15B N8 C17B 111.9(18) . . C17A N8 Zn2 127.3(8) . 2_554 C15A N8 Zn2 129.2(6) . 2_554 C1 N1 C2 102.4(7) . . C1 N1 Zn1 126.3(6) . . C2 N1 Zn1 131.3(6) . . C5 N4 C4 104.1(7) . . C5 N4 Zn2 130.3(7) . 6_556 C4 N4 Zn2 125.5(6) . 6_556 N4 C4 N3 113.4(8) . . C2 C3 N2 107.6(8) . . N2 C1 N1 114.9(7) . . N6 C7 N5 114.8(7) . . C3 C2 N1 110.7(9) . . N4 C5 C6 108.3(10) . . N3 C6 C5 110.1(10) . . N5 C9A C8A 107.5(7) . . N6 C8A C9A 109.2(7) . . N7 C15A N8 115.3(7) . . N8 C17A C16A 107.8(12) . . N7 C16A C17A 112.4(12) . . N5 C9B C8B 107.5(7) . . N5 C9B C10 129.3(12) . . C8B C9B C10 122.2(12) . . N6 C8B C9B 109.2(7) . . N6 C8B C13 127.2(12) . . C9B C8B C13 122.7(12) . . C12 C13 C8B 116(2) . . C9B C10 C11 115.5(19) . . C10 C11 C12 122(2) . . C10 C11 C11 132(2) . 5_556 C12 C11 C11 85.2(18) . 5_556 C14 C12 C13 114(4) . . C14 C12 C11 126(4) . . C13 C12 C11 120(2) . . C18 C17 C16 119(4) . . C18 C17 N8 132(4) . . C16 C17 N8 108(3) . . C17 C16 C21 126(4) . . C17 C16 N7 104(3) . . C21 C16 N7 129(4) . . C20 C21 C16 114(4) . . C21 C20 C19 119(4) . . C18 C19 C20 126(4) . . C19 C18 C17 117(4) . . N7 C15B N8 98.0(11) . . C18B C17B C16B 119(4) . . C18B C17B N8 132(4) . . C16B C17B N8 108(3) . . C17B C16B C21B 126(4) . . C17B C16B N7 104(3) . . C21B C16B N7 129(4) . . C20B C21B C16B 114(4) . . C21B C20B C19B 119(4) . . C18B C19B C20B 126(4) . . C18B C19B C22 114(4) . . C20B C19B C22 120(4) . . C19B C18B C17B 117(4) . . C1S N1S C2S 54(4) . . C1S N1S C5S 62(4) . . C2S N1S C5S 79(4) . . O1S C1S C2S 130(10) . . O1S C1S N1S 117(6) . . C2S C1S N1S 69(3) . . O1S C1S C5S 140(10) . . C2S C1S C5S 89(5) . . N1S C1S C5S 70(4) . . O1S C1S C3S 54(4) . . C2S C1S C3S 152(7) . . N1S C1S C3S 137(8) . . C5S C1S C3S 93(6) . . C1S C2S N1S 56.2(19) . . C1S C2S C4S 124(8) . . N1S C2S C4S 135(7) . . C1S C2S C5S 51(4) . . N1S C2S C5S 54(3) . . C4S C2S C5S 90(5) . . O1S C3S C1S 39.6(19) . . C1S O1S C3S 86(5) . . C1S C5S N1S 48(2) . . C1S C5S C2S 40(3) . . N1S C5S C2S 47(2) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Zn1 N7 1.952(8) . Zn1 N1 1.987(7) . Zn1 N3 1.993(7) . Zn1 N5 1.997(6) . Zn2 N8 1.951(7) 2 Zn2 N2 1.980(6) 8_566 Zn2 N4 1.984(6) 6_656 Zn2 N6 1.990(6) . N5 C7 1.322(10) . N5 C9B 1.366(11) . N5 C9A 1.366(11) . N6 C7 1.319(9) . N6 C8B 1.352(10) . N6 C8A 1.352(10) . N7 C16A 1.317(17) . N7 C15A 1.357(9) . N7 C15B 1.519(16) . N7 C16B 1.61(5) . N7 C16 1.61(5) . N3 C6 1.302(14) . N3 C4 1.340(10) . N2 C1 1.311(10) . N2 C3 1.373(11) . N8 C17A 1.319(15) . N8 C15A 1.377(10) . N8 C15B 1.542(16) . N8 C17B 1.67(5) . N8 C17 1.67(5) . N1 C1 1.338(10) . N1 C2 1.364(11) . N4 C5 1.324(12) . N4 C4 1.334(10) . C3 C2 1.336(13) . C5 C6 1.370(15) . C9A C8A 1.371(12) . C17A C16A 1.40(2) . C9B C8B 1.371(12) . C9B C10 1.40(2) . C8B C13 1.40(2) . C13 C12 1.40(3) . C10 C11 1.41(3) . C11 C12 1.41(3) . C11 C11 1.86(4) 5_556 C12 C14 1.33(7) . C17 C18 1.39(7) . C17 C16 1.40(7) . C16 C21 1.41(7) . C21 C20 1.41(7) . C20 C19 1.44(7) . C19 C18 1.33(7) . C17B C18B 1.39(7) . C17B C16B 1.40(7) . C16B C21B 1.41(7) . C21B C20B 1.41(7) . C20B C19B 1.44(7) . C19B C18B 1.33(7) . C19B C22 1.64(6) . N1S C1S 1.34(2) . N1S C2S 1.51(2) . N1S C5S 1.68(8) . C1S O1S 1.27(2) . C1S C2S 1.31(9) . C1S C5S 1.57(9) . C1S C3S 1.99(8) . C2S C4S 1.52(2) . C2S C5S 2.03(9) . C3S O1S 1.62(7) .