#------------------------------------------------------------------------------ #$Date: 2020-05-07 00:15:59 +0300 (Thu, 07 May 2020) $ #$Revision: 251827 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/04/7240461.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_7240461 loop_ _publ_author_name 'Bumstead, Alice M.' 'G\'omez, Mar\'ia Laura R\'ios' 'Thorne, Michael Francis' 'Sapnik, Adam F.' 'Longley, Louis' 'Tuffnell, Joshua Mark' 'Keeble, Dean S.' 'Keen, David A.' 'Bennett, Thomas Douglas' _publ_section_title ; Investigating the Melting Behaviour of Polymorphic Zeolitic Imidazolate Frameworks ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D0CE00408A _journal_year 2020 _chemical_formula_moiety 'Zn1.00 C10.00 N4 H9.20 O0.33' _chemical_formula_sum 'C240 H220.8 N96 O8 Zn24' _chemical_formula_weight 256.08 _chemical_name_common 'ZIF-76 mbIm' _chemical_name_systematic Zn(Im)1.20(ClFbIm)0.80 _space_group_crystal_system cubic _space_group_IT_number 215 _space_group_name_Hall 'P -4 2 3' _space_group_name_H-M_alt 'P -4 3 m' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2020-03-15 deposited with the CCDC. 2020-05-06 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 24 _cell_length_a 22.6840(6) _cell_length_b 22.6840(6) _cell_length_c 22.6840(6) _cell_measurement_reflns_used 2610 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 59.8430 _cell_measurement_theta_min 2.7510 _cell_volume 11672.4(5) _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_detector_type Eos _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -48.00 -11.00 1.00 2.52 -- 0.00 106.00 -72.00 37 2 \w 80.00 107.00 1.00 10.09 -- 51.25 98.00 67.00 27 3 \w 83.00 114.00 1.00 10.09 -- 51.25 115.00 151.00 31 4 \w 122.00 169.00 1.00 10.09 -- 102.50 32.00 120.00 47 5 \w 116.00 156.00 1.00 10.09 -- 102.50 -21.00 -60.00 40 6 \w 94.00 128.00 1.00 10.09 -- 51.25 106.00 -72.00 34 7 \w 60.00 86.00 1.00 10.09 -- 102.50 32.00 120.00 26 8 \w 25.00 74.00 1.00 10.09 -- 102.50 -46.00 -5.00 49 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator mirror _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0304 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 9161 _diffrn_reflns_point_group_measured_fraction_full 0.972 _diffrn_reflns_point_group_measured_fraction_max 0.944 _diffrn_reflns_theta_full 64.5587 _diffrn_reflns_theta_max 63.881 _diffrn_reflns_theta_min 2.755 _diffrn_source 'sealed X-ray tube' _diffrn_source_type 'Enhance Ultra (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 1.643 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.73424 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 0.865 _exptl_crystal_description cubic _exptl_crystal_F_000 3216 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _refine_diff_density_max 1.413 _refine_diff_density_min -0.518 _refine_diff_density_rms 0.146 _refine_ls_abs_structure_details ; Flack x determined using 787 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.51(6) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.365 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 175 _refine_ls_number_reflns 3425 _refine_ls_number_restraints 19 _refine_ls_restrained_S_all 1.365 _refine_ls_R_factor_all 0.1424 _refine_ls_R_factor_gt 0.1156 _refine_ls_shift/su_max 0.107 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2989 _refine_ls_wR_factor_ref 0.3534 _reflns_Friedel_coverage 0.756 _reflns_Friedel_fraction_full 0.945 _reflns_Friedel_fraction_max 0.885 _reflns_number_gt 2366 _reflns_number_total 3425 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0ce00408a2.cif _cod_data_source_block shelx _cod_original_cell_volume 11672.4(9) _cod_original_formula_sum 'Zn24 C240 H220.8 N96 O8' _cod_database_code 7240461 _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. ; _shelx_res_file ; TITL data_reduction_02 in P-43m shelx.res created by SHELXL-2018/3 at 17:01:05 on 15-Mar-2020 CELL 1.54184 22.6840 22.6840 22.6840 90.000 90.000 90.000 ZERR 46.00 0.0006 0.0006 0.0006 0.000 0.000 0.000 LATT -1 SYMM - X, - Y, Z SYMM - X, Y, - Z SYMM X, - Y, - Z SYMM Z, X, Y SYMM Z, - X, - Y SYMM - Z, - X, Y SYMM - Z, X, - Y SYMM Y, Z, X SYMM - Y, Z, - X SYMM Y, - Z, - X SYMM - Y, - Z, X SYMM Y, X, Z SYMM - Y, - X, Z SYMM Y, - X, - Z SYMM - Y, X, - Z SYMM X, Z, Y SYMM - X, Z, - Y SYMM - X, - Z, Y SYMM X, - Z, - Y SYMM Z, Y, X SYMM Z, - Y, - X SYMM - Z, Y, - X SYMM - Z, - Y, X SFAC C H N ZN O UNIT 72 0 192 48 0 MERG 2 DANG 2.300 0.020 C10B C12 DFIX 1.400 0.030 C10B C11 DFIX 1.400 0.030 C11 C12 DANG 2.300 0.020 C15B C17 DFIX 1.400 0.030 C15B C16 DFIX 1.400 0.030 C16 C17 FLAT 0.010 C9 N3 C10B C11 C12 FLAT 0.010 C1 N1 C2 C3 C4 C5 FLAT 0.010 C14 N4 C15B C16 C17 C18 DANG 2.300 0.020 C2 C4 DFIX 1.400 0.030 C2 C3 DFIX 1.400 0.030 C3 C4 DFIX 1.380 0.030 C6 C7 DANG 2.220 0.020 N5 C7 FREE C6 C3 EADP C3 C4 C5 EADP C10A C10B EXYZ C10A C10B EADP C15a C15b EXYZ C15a C15b EADP C8a C8b EXYZ C8a C8b FMAP 2 PLAN 20 ACTA 50.00 L.S. 50 WGHT 0.200000 FVAR 1.62079 0.45684 0.54757 0.04881 ZN1 4 0.368755 0.182991 0.000130 11.00000 0.07340 0.08931 = 0.13740 0.00055 -0.00094 0.01643 N3 3 0.333148 0.118451 -0.050346 11.00000 0.07193 0.13399 = 0.14784 0.01467 -0.00468 -0.00821 C9 1 0.362110 0.094275 -0.094275 10.50000 0.05616 0.09470 = 0.09470 0.01988 -0.00712 0.00712 AFIX 43 H9 2 0.399037 0.106868 -0.106868 10.50000 -1.20000 AFIX 0 N1 3 0.368768 0.147600 0.077950 11.00000 0.22346 0.12304 = 0.16700 0.01958 0.09129 0.07577 C1 1 0.367938 0.095464 0.095464 10.50000 0.10674 0.11982 = 0.11982 0.03827 -0.01041 -0.01041 AFIX 43 H1 2 0.366549 0.066491 0.066491 10.50000 -1.20000 AFIX 0 C2 1 0.391598 0.175213 0.131671 11.00000 0.28976 0.21736 = 0.11094 -0.02958 0.01167 0.02266 C3 1 0.403408 0.235555 0.141747 11.00000 0.32815 AFIX 43 H3 2 0.397596 0.265197 0.114026 11.00000 -1.20000 AFIX 0 C4 1 0.424866 0.244947 0.198510 11.00000 0.32815 C5 1 0.443103 0.322494 0.220679 10.50000 0.32815 C6 1 0.470369 0.215809 0.083231 -21.00000 0.07285 0.10747 = 0.11833 -0.05288 0.01914 0.01898 AFIX 43 H6 2 0.444600 0.224292 0.113969 -21.00000 -1.20000 AFIX 0 C7 1 0.530109 0.224639 0.087938 -21.00000 0.21472 0.16014 = 0.43013 0.07125 0.22787 0.05294 AFIX 43 H7 2 0.552260 0.242033 0.117731 -21.00000 -1.20000 AFIX 0 N5 3 0.452513 0.195284 0.034145 -21.00000 0.07192 0.12159 = 0.17956 -0.02301 0.01192 0.02323 N2 3 0.450265 0.196383 -0.027591 21.00000 0.07439 0.08778 = 0.07388 0.00925 0.00601 0.02349 N4 3 0.329773 0.260903 0.002387 11.00000 0.07858 0.09482 = 0.16653 0.00657 0.00347 0.01453 C14 1 0.274211 0.274211 -0.000867 10.50000 0.07841 0.07841 = 0.14205 0.00443 0.00443 0.00995 AFIX 43 H14 2 0.245392 0.245391 -0.005304 10.50000 -1.20000 AFIX 0 PART 1 C10A 1 0.281008 0.090182 -0.045347 -31.00000 0.08592 0.16442 = 0.15230 0.00293 0.01308 -0.01469 AFIX 43 H10A 2 0.251153 0.098094 -0.018385 -31.00000 -1.20000 AFIX 0 C8A 1 0.500000 0.182225 0.000000 -20.50000 0.09113 0.07697 = 0.11303 0.00000 0.00801 0.00000 C15A 1 0.357295 0.314620 -0.005132 -41.00000 0.10417 0.09547 = 0.36310 0.02682 0.07039 0.01016 AFIX 43 H15A 2 0.397605 0.320739 -0.009429 -41.00000 -1.20000 AFIX 0 PART 2 C15B 1 0.357295 0.314620 -0.005132 41.00000 0.10417 0.09547 = 0.36310 0.02682 0.07039 0.01016 C17 1 0.438700 0.376851 -0.012746 41.00000 0.04394 C16 1 0.418642 0.319421 -0.004488 41.00000 0.22690 AFIX 43 H16 2 0.443668 0.287401 0.000925 41.00000 -1.20000 AFIX 0 C18 1 0.488526 0.412003 -0.016964 40.50000 -0.00100 C10B 1 0.281008 0.090182 -0.045347 31.00000 0.08592 0.16442 = 0.15230 0.00293 0.01308 -0.01469 C11 1 0.234771 0.100485 -0.004058 31.00000 0.07049 0.18904 = 0.25474 0.08132 -0.03475 -0.01647 AFIX 43 H11 2 0.237659 0.129695 0.024564 31.00000 -1.20000 AFIX 0 C12 1 0.187665 0.066603 -0.008374 31.00000 0.09970 0.40071 = 0.37337 -0.12584 0.11689 -0.03745 C13 1 0.161903 0.045103 0.045103 30.50000 0.35337 C8B 1 0.500000 0.182225 0.000000 20.50000 0.09113 0.07697 = 0.11303 0.00000 0.00801 0.00000 PART 0 O1S 5 0.201219 0.201219 0.798781 10.16667 0.45151 0.45151 = 0.45151 -0.26843 -0.26843 0.26843 O1S1 5 0.191693 0.191693 0.191693 10.16667 0.63878 0.63878 = 0.63878 -0.20820 -0.20820 -0.20820 HKLF 4 REM data_reduction_02 in P-43m REM wR2 = 0.3534, GooF = S = 1.365, Restrained GooF = 1.365 for all data REM R1 = 0.1156 for 2366 Fo > 4sig(Fo) and 0.1424 for all 3425 data REM 175 parameters refined using 19 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 1.413, deepest hole -0.518, 1-sigma level 0.146 Q1 1 0.1870 0.1870 0.8130 10.16667 0.05 0.92 Q2 1 0.3745 0.1523 -0.0816 11.00000 0.05 0.80 Q3 1 0.5278 0.2583 0.1760 11.00000 0.05 0.63 Q4 1 0.5000 0.0000 0.0000 10.12500 0.05 0.62 Q5 1 0.1771 0.2346 0.7654 10.50000 0.05 0.59 Q6 1 0.1886 0.1474 0.7782 11.00000 0.05 0.55 Q7 1 0.1881 0.2104 0.8572 11.00000 0.05 0.54 Q8 1 0.4482 0.0000 0.0000 10.25000 0.05 0.54 Q9 1 0.5651 0.2400 0.1333 11.00000 0.05 0.52 Q10 1 0.1861 0.2526 0.7936 11.00000 0.05 0.52 Q11 1 0.3786 0.1773 -0.1295 11.00000 0.05 0.51 Q12 1 0.1802 0.1148 0.1802 10.50000 0.05 0.51 Q13 1 0.1909 0.1161 0.8091 10.50000 0.05 0.50 Q14 1 0.1758 0.2226 0.2364 11.00000 0.05 0.49 Q15 1 0.5000 0.5000 0.5000 10.04167 0.05 0.48 Q16 1 0.4720 0.2558 0.1775 11.00000 0.05 0.47 Q17 1 0.1433 0.1433 0.1433 10.16667 0.05 0.46 Q18 1 0.1470 0.1968 0.2160 11.00000 0.05 0.46 Q19 1 0.4986 0.4074 -0.0507 11.00000 0.05 0.46 Q20 1 0.1436 0.2060 0.2060 10.50000 0.05 0.45 ; _shelx_res_checksum 69394 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, z' '-y, -x, z' 'y, -x, -z' '-y, x, -z' 'x, z, y' '-x, z, -y' '-x, -z, y' 'x, -z, -y' 'z, y, x' 'z, -y, -x' '-z, y, -x' '-z, -y, x' 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 0.36875(5) 0.18299(6) 0.00013(16) 0.1000(8) Uani 1 1 d . . . . . N3 N 0.3331(5) 0.1185(7) -0.0503(7) 0.118(4) Uani 1 1 d . . . . . C9 C 0.3621(8) 0.0943(6) -0.0943(6) 0.082(5) Uani 1 2 d S T P . . H9 H 0.399037 0.106868 -0.106868 0.098 Uiso 1 2 calc R U P . . N1 N 0.3688(10) 0.1476(7) 0.0780(9) 0.171(8) Uani 1 1 d . . . . . C1 C 0.3679(12) 0.0955(10) 0.0955(10) 0.115(8) Uani 1 2 d S T P . . H1 H 0.366549 0.066491 0.066491 0.139 Uiso 1 2 calc R U P . . C2 C 0.3916(9) 0.1752(14) 0.1317(10) 0.206(13) Uani 1 1 d D . . . . C3 C 0.4034(15) 0.2356(19) 0.142(2) 0.33(2) Uiso 1 1 d D . . . . H3 H 0.397596 0.265197 0.114026 0.394 Uiso 1 1 calc R U . . . C4 C 0.4249(17) 0.2449(18) 0.1985(19) 0.33(2) Uiso 1 1 d D . . . . C5 C 0.443(3) 0.322(5) 0.221(6) 0.33(2) Uiso 0.5 1 d . . P . . C6 C 0.4704(11) 0.2158(13) 0.0832(14) 0.100(9) Uani 0.54(3) 1 d D . P B . H6 H 0.444600 0.224292 0.113969 0.119 Uiso 0.54(3) 1 calc R U P . . C7 C 0.5301(15) 0.225(2) 0.088(2) 0.27(5) Uani 0.54(3) 1 d D . P . . H7 H 0.552260 0.242033 0.117731 0.322 Uiso 0.54(3) 1 calc R U P . . N5 N 0.4525(11) 0.1953(14) 0.034(2) 0.124(14) Uani 0.54(3) 1 d D . P . . N2 N 0.4503(13) 0.1964(11) -0.0276(15) 0.079(9) Uani 0.46(3) 1 d . . P B . N4 N 0.3298(4) 0.2609(4) 0.0024(10) 0.113(3) Uani 1 1 d . . . . . C14 C 0.2742(5) 0.2742(5) -0.0009(15) 0.100(4) Uani 1 2 d S T P . . H14 H 0.245392 0.245391 -0.005304 0.120 Uiso 1 2 calc R U P . . C10A C 0.2810(6) 0.0902(8) -0.0453(8) 0.134(6) Uani 0.45(5) 1 d . . P A 1 H10A H 0.251153 0.098094 -0.018385 0.161 Uiso 0.45(5) 1 calc R U P A 1 C8A C 0.500000 0.1822(6) 0.000000 0.094(4) Uani 0.54(3) 2 d S T P B 1 C15A C 0.3573(7) 0.3146(6) -0.0051(11) 0.188(13) Uani 0.95(3) 1 d . . P C 1 H15A H 0.397605 0.320739 -0.009429 0.225 Uiso 0.95(3) 1 calc R U P C 1 C15B C 0.3573(7) 0.3146(6) -0.0051(11) 0.188(13) Uani 0.05(3) 1 d D . P . 2 C17 C 0.439(4) 0.377(5) -0.013(2) 0.04(4) Uiso 0.05(3) 1 d D . P . 2 C16 C 0.419(2) 0.319(4) -0.0045(18) 0.2(2) Uiso 0.05(3) 1 d D . P . 2 H16 H 0.443668 0.287401 0.000925 0.272 Uiso 0.05(3) 1 calc R U P C 2 C18 C 0.489(4) 0.412(5) -0.017(3) 0.00(4) Uiso 0.024(13) 1 d . . P . 2 C10B C 0.2810(6) 0.0902(8) -0.0453(8) 0.134(6) Uani 0.55(5) 1 d D . P A 2 C11 C 0.2348(9) 0.1005(14) -0.0041(17) 0.17(2) Uani 0.55(5) 1 d D . P A 2 H11 H 0.237659 0.129695 0.024564 0.206 Uiso 0.55(5) 1 calc R U P A 2 C12 C 0.1877(10) 0.0666(19) -0.008(2) 0.29(5) Uani 0.55(5) 1 d D . P A 2 C13 C 0.162(9) 0.045(5) 0.045(5) 0.35(9) Uiso 0.55(5) 2 d S . P . 2 C8B C 0.500000 0.1822(6) 0.000000 0.094(4) Uani 0.46(3) 2 d S T P B 2 O1S O 0.201(5) 0.201(5) 0.799(5) 0.45(9) Uani 1 6 d S T P . . O1S1 O 0.192(3) 0.192(3) 0.192(3) 0.64(16) Uani 1 6 d S T 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 0.0734(9) 0.0893(10) 0.1374(13) 0.0006(17) -0.0009(16) 0.0164(6) N3 0.072(6) 0.134(10) 0.148(11) 0.015(8) -0.005(7) -0.008(6) C9 0.056(10) 0.095(8) 0.095(8) 0.020(10) -0.007(5) 0.007(5) N1 0.22(2) 0.123(12) 0.167(16) 0.020(11) 0.091(15) 0.076(12) C1 0.107(19) 0.120(13) 0.120(13) 0.038(15) -0.010(11) -0.010(11) C2 0.29(4) 0.22(2) 0.111(14) -0.030(15) 0.012(18) 0.02(2) C6 0.073(14) 0.107(18) 0.12(2) -0.053(16) 0.019(14) 0.019(13) C7 0.21(6) 0.16(4) 0.43(10) 0.07(5) 0.23(7) 0.05(4) N5 0.072(19) 0.12(3) 0.18(4) -0.02(2) 0.01(2) 0.023(14) N2 0.074(19) 0.088(18) 0.074(15) 0.009(13) 0.006(13) 0.023(12) N4 0.079(5) 0.095(6) 0.167(10) 0.007(13) 0.003(12) 0.015(4) C14 0.078(5) 0.078(5) 0.142(12) 0.004(13) 0.004(13) 0.010(6) C10A 0.086(9) 0.164(15) 0.152(14) 0.003(12) 0.013(9) -0.015(9) C8A 0.091(9) 0.077(7) 0.113(10) 0.000 0.01(2) 0.000 C15A 0.104(9) 0.095(9) 0.36(4) 0.03(2) 0.07(2) 0.010(7) C15B 0.104(9) 0.095(9) 0.36(4) 0.03(2) 0.07(2) 0.010(7) C10B 0.086(9) 0.164(15) 0.152(14) 0.003(12) 0.013(9) -0.015(9) C11 0.070(14) 0.19(3) 0.25(5) 0.08(4) -0.03(3) -0.016(15) C12 0.10(2) 0.40(9) 0.37(10) -0.13(8) 0.12(4) -0.04(3) C8B 0.091(9) 0.077(7) 0.113(10) 0.000 0.01(2) 0.000 O1S 0.45(9) 0.45(9) 0.45(9) -0.27(10) -0.27(10) 0.27(10) O1S1 0.64(16) 0.64(16) 0.64(16) -0.21(10) -0.21(10) -0.21(10) 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 N1 Zn1 N4 110.3(8) . . ? N1 Zn1 N2 110.7(12) . . ? N4 Zn1 N2 106.8(8) . . ? N1 Zn1 N3 102.4(8) . . ? N4 Zn1 N3 118.8(6) . . ? N2 Zn1 N3 107.7(10) . . ? N1 Zn1 N5 73.5(14) . . ? N4 Zn1 N5 106.3(10) . . ? N2 Zn1 N5 40.5(9) . . ? N3 Zn1 N5 132.4(10) . . ? C9 N3 C10B 107.7(16) . . ? C9 N3 C10A 107.7(16) . . ? C9 N3 Zn1 122.1(10) . . ? C10B N3 Zn1 130.2(13) . . ? C10A N3 Zn1 130.2(13) . . ? N3 C9 N3 112.5(19) 20 . ? C1 N1 C2 98(2) . . ? C1 N1 Zn1 133(2) . . ? C2 N1 Zn1 125.5(17) . . ? N1 C1 N1 127(3) 17 . ? C2 C2 C3 125(2) 17 . ? C2 C2 N1 106.6(14) 17 . ? C3 C2 N1 128(3) . . ? C4 C3 C2 111(3) . . ? C3 C4 C4 123(3) . 17 ? C3 C4 C5 118(5) . . ? C4 C4 C5 118(4) 17 . ? N5 C6 C7 116(3) . . ? C6 C7 N2 99(3) . 3_655 ? C6 N5 C8B 109(2) . . ? C6 N5 C8A 109(2) . . ? C6 N5 N2 152(4) . . ? C8B N5 N2 58(2) . . ? C8A N5 N2 58(2) . . ? C6 N5 Zn1 132(2) . . ? C8B N5 Zn1 119(3) . . ? C8A N5 Zn1 119(3) . . ? N2 N5 Zn1 66(2) . . ? C8B N2 N5 60(2) . . ? C8A N2 N5 60(2) . . ? C8A N2 C7 105.5(19) . 3_655 ? N5 N2 C7 150(3) . 3_655 ? C8B N2 Zn1 127(2) . . ? C8A N2 Zn1 127(2) . . ? N5 N2 Zn1 73.3(19) . . ? C7 N2 Zn1 127(2) 3_655 . ? C14 N4 C15B 103.1(11) . . ? C14 N4 C15A 103.1(11) . . ? C14 N4 Zn1 129.8(9) . . ? C15B N4 Zn1 125.7(8) . . ? C15A N4 Zn1 125.7(8) . . ? N4 C14 N4 116.6(15) 13 . ? N3 C10A C10A 106.0(11) . 20 ? N2 C8A N2 152(3) . 3_655 ? N2 C8A N5 110.6(14) . 3_655 ? N2 C8A N5 62.8(13) 3_655 3_655 ? N2 C8A N5 62.8(13) . . ? N2 C8A N5 110.6(14) 3_655 . ? N5 C8A N5 155(3) 3_655 . ? C15A C15A N4 107.7(7) 13 . ? N4 C15B C16 121(4) . . ? C18 C17 C16 144(10) . . ? C18 C17 C18 26(4) . 3_655 ? C16 C17 C18 128(7) . 3_655 ? C17 C17 C18 108(5) 13 3_655 ? C17 C16 C15B 113(4) . . ? C18 C18 C17 114(9) 3_655 . ? C18 C18 C17 41(8) 3_655 3_655 ? C17 C18 C17 115(10) . 3_655 ? N3 C10B C11 128(2) . . ? C12 C11 C10B 117(3) . . ? C11 C12 C13 118(9) . . ? C11 C12 C12 118(3) . 20 ? C13 C12 C12 111(7) . 20 ? C12 C13 C12 114(10) 17 . ? N2 C8B N2 152(3) . 3_655 ? N2 C8B N5 110.6(14) . 3_655 ? N2 C8B N5 62.8(13) 3_655 3_655 ? N2 C8B N5 62.8(13) . . ? N2 C8B N5 110.6(14) 3_655 . ? N5 C8B N5 155(3) 3_655 . ? 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 N1 1.939(18) . ? Zn1 N4 1.977(9) . ? Zn1 N2 1.98(3) . ? Zn1 N3 2.027(16) . ? Zn1 N5 2.07(3) . ? N3 C9 1.314(18) . ? N3 C10B 1.35(2) . ? N3 C10A 1.35(2) . ? N1 C1 1.25(2) . ? N1 C2 1.46(3) . ? C2 C2 1.40(6) 17 ? C2 C3 1.41(3) . ? C3 C4 1.39(4) . ? C4 C4 1.49(10) 17 ? C4 C5 1.88(12) . ? C6 N5 1.27(4) . ? C6 C7 1.37(3) . ? C7 N2 1.58(6) 3_655 ? N5 C8B 1.36(3) . ? N5 C8A 1.36(3) . ? N5 N2 1.40(3) . ? N2 C8B 1.33(3) . ? N2 C8A 1.33(3) . ? N4 C14 1.298(13) . ? N4 C15B 1.380(18) . ? N4 C15A 1.380(18) . ? C10A C10A 1.44(4) 20 ? C15A C15A 1.37(3) 13 ? C15B C16 1.40(4) . ? C17 C18 1.39(11) . ? C17 C16 1.39(4) . ? C17 C17 2.0(3) 13 ? C17 C18 1.95(11) 3_655 ? C18 C18 0.93(16) 3_655 ? C10B C11 1.43(3) . ? C11 C12 1.32(3) . ? C12 C13 1.43(11) . ? C12 C12 1.87(11) 20 ?