# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 #TrackingRef 'Revised-CIF.cif' # TITLE AND AUTHOR LIST _publ_section_title ; Azulene Based Metal-Organic Frameworks for Strong Adsorption of H~2~ ; loop_ _publ_author_name _publ_author_address #Corresponding author of the paper #Corresponding author of the paper S.Barman ; Anorganisch-Chemisches Institut, Universitat Zurich, Winterthurerstrasse 190, CH-8037, Zurich, Switzerland ; H.Furukawa ; Center for Reticular Chemistry, Department of Chemistry and Biochemistry, University of California-Los Angeles, 607 Charles E. Young Drive East, Los Angeles, California 90095 ; O.Blacque ; Anorganisch-Chemisches Institut, Universitat Zurich, Winterthurerstrasse 190, CH-8037, Zurich, Switzerland ; K.Venkatesan ; Anorganisch-Chemisches Institut, Universitat Zurich, Winterthurerstrasse 190, CH-8037, Zurich, Switzerland ; O.M.Yaghi ; Center for Reticular Chemistry, Department of Chemistry and Biochemistry, University of California-Los Angeles, 607 Charles E. Young Drive East, Los Angeles, California 90095 ; H.Berke ; Anorganisch-Chemisches Institut, Universitat Zurich, Winterthurerstrasse 190, CH-8037, Zurich, Switzerland ; _publ_contact_author_name 'Berke, H.' _publ_contact_author_email HBERKE@ACI.UNIZH.CH #============================================================================== data_MOF645 _database_code_depnum_ccdc_archive 'CCDC 771570' #TrackingRef 'Revised-CIF.cif' # start Validation Reply Form _vrf_PLAT220_MOF645 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.76 Ratio RESPONSE: The largest Ueq(C) values are observed for C25A and C26A, which are disordered atoms, with 0.0653 and 0.099. These values are really acceptable but the structure contains also very well defined carbon atoms like C1 and C2 (Ueq of 0.0172 and 0.0176) which gives the large ratio of 5.76. The same kind of explanation is proposed for the large Non-Solvent O Ueq(max)/Ueq(min) of 4.29. ; _vrf_PLAT222_MOF645 ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 8.28 Ratio RESPONSE: This is a consequence of the large ratio for Ueq(C) explained above.. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Zn~5~(\m~3~-OH)~2~(L)~4~(DMF)(H~2~O)].(DMF) [L = 1,3-azulene dicarboxylate] ; _chemical_name_common ;(Zn!5$(mu!3$-OH)!2$(L)!4$(DMF)(H!2$O)).(DMF) (L = 1,3-azulene dicarboxylate) ; _chemical_melting_point ? _chemical_formula_moiety 'C51 H35 N O20 Zn5, C3 H7 N O' _chemical_formula_sum 'C54 H42 N2 O21 Zn5' _chemical_formula_weight 1381.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2' _symmetry_space_group_name_Hall 'C 2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 15.7939(2) _cell_length_b 16.6435(1) _cell_length_c 12.2880(2) _cell_angle_alpha 90.00 _cell_angle_beta 123.831(2) _cell_angle_gamma 90.00 _cell_volume 2683.19(9) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 29072 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 34.44 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.710 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1396 _exptl_absorpt_coefficient_mu 2.286 _exptl_absorpt_correction_T_min 0.708 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Goniometer Xcalibur, detector: Ruby Oxford Diffraction (2007). Oxford Diffraction Ltd., Xcalibur CCD system ; _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 10.4498 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 39666 _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_av_sigmaI/netI 0.0240 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 32.57 _reflns_number_total 9785 _reflns_number_gt 9158 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_structure_solution ; SHELXS97. Program for Crystal Structure solution. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _computing_structure_refinement ; SHELXL97. Program for crystal structure refinement. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _computing_molecular_graphics ; ORTEP-3 for Windows, Version 2.01. Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. ; _computing_publication_material ; WinGX -- An integrated system of Windows programs for the solution, refinment and analysis of single crystal X-ray diffraction data, Version 1.80.00. Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838. SHELXL97. Program for crystal structure refinement. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. PLATON for Windows, Version 1.12. Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0561P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H. D. (1983), Acta Cryst. A39, 876-881. 4749 Friedel pairs' _refine_ls_abs_structure_Flack 0.007(7) _refine_ls_number_reflns 9785 _refine_ls_number_parameters 416 _refine_ls_number_restraints 76 _refine_ls_R_factor_all 0.0307 _refine_ls_R_factor_gt 0.0285 _refine_ls_wR_factor_ref 0.0770 _refine_ls_wR_factor_gt 0.0765 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.90119(15) 0.88484(11) 0.75475(19) 0.0172(3) Uani 1 1 d . . . C2 C 0.86346(16) 0.80177(11) 0.71829(19) 0.0176(3) Uani 1 1 d . . . C3 C 0.82604(16) 0.77014(12) 0.59364(19) 0.0201(4) Uani 1 1 d . . . H3 H 0.8247 0.7973 0.5266 0.024 Uiso 1 1 calc R . . C4 C 0.7910(2) 0.69192(13) 0.5851(2) 0.0279(5) Uani 1 1 d . . . C5 C 0.8086(2) 0.67085(14) 0.7085(2) 0.0310(5) Uani 1 1 d . . . C6 C 0.85417(16) 0.74227(12) 0.79338(19) 0.0208(4) Uani 1 1 d . . . C7 C 0.87943(17) 0.75151(14) 0.9206(2) 0.0235(4) Uani 1 1 d . . . H7 H 0.9029 0.8022 0.9571 0.028 Uiso 1 1 calc R . . C8 C 0.8745(2) 0.69547(18) 1.0011(3) 0.0352(6) Uani 1 1 d . . . H8 H 0.8915 0.7143 1.0821 0.042 Uiso 1 1 calc R . . C9 C 0.8473(3) 0.6146(2) 0.9753(3) 0.0559(10) Uani 1 1 d . . . H9 H 0.8539 0.5860 1.0446 0.067 Uiso 1 1 calc R . . C10 C 0.8120(4) 0.5705(2) 0.8623(3) 0.0756(16) Uani 1 1 d . . . H10 H 0.8003 0.5163 0.8675 0.091 Uiso 1 1 calc R . . C11 C 0.7918(4) 0.59555(19) 0.7430(3) 0.0623(13) Uani 1 1 d . . . H11 H 0.7633 0.5571 0.6768 0.075 Uiso 1 1 calc R . . C12 C 0.7378(2) 0.64633(13) 0.4621(2) 0.0341(6) Uani 1 1 d . . . C13 C 0.72724(16) 0.49629(12) 0.0998(2) 0.0202(3) Uani 1 1 d . . . C14 C 0.79478(15) 0.43555(11) 0.0992(2) 0.0180(3) Uani 1 1 d . . . C15 C 0.75868(16) 0.37420(11) 0.0054(2) 0.0183(3) Uani 1 1 d . . . H15 H 0.6908 0.3667 -0.0624 0.022 Uiso 1 1 calc R . . C16 C 0.83982(15) 0.32572(11) 0.0288(2) 0.0180(3) Uani 1 1 d . . . C17 C 0.93096(15) 0.35789(12) 0.1378(2) 0.0187(3) Uani 1 1 d . . . C18 C 0.90231(16) 0.42758(12) 0.1853(2) 0.0197(4) Uani 1 1 d . . . C19 C 0.96560(19) 0.47549(16) 0.2937(3) 0.0323(5) Uani 1 1 d . . . H19 H 0.9335 0.5155 0.3110 0.039 Uiso 1 1 calc R . . C20 C 1.0725(2) 0.4712(2) 0.3811(3) 0.0450(8) Uani 1 1 d . . . H20 H 1.1012 0.5071 0.4508 0.054 Uiso 1 1 calc R . . C21 C 1.1408(2) 0.42071(19) 0.3773(3) 0.0427(7) Uani 1 1 d . . . H21 H 1.2091 0.4296 0.4423 0.051 Uiso 1 1 calc R . . C22 C 1.12205(18) 0.35897(16) 0.2908(3) 0.0324(5) Uani 1 1 d . . . H22 H 1.1796 0.3326 0.3060 0.039 Uiso 1 1 calc R . . C23 C 1.02947(17) 0.33085(13) 0.1845(2) 0.0242(4) Uani 1 1 d . . . H23 H 1.0336 0.2884 0.1384 0.029 Uiso 1 1 calc R . . C24 C 0.82779(17) 0.25353(12) -0.0490(2) 0.0220(4) Uani 1 1 d . . . O1 O 0.55324(10) 0.58863(8) 0.14519(13) 0.0150(2) Uani 1 1 d . . . H1 H 0.5018 0.6311 0.1138 0.018 Uiso 1 1 calc R . . O2A O 0.9180(3) 0.9115(4) 0.8611(6) 0.0235(8) Uani 0.50 1 d PU . 1 O3A O 0.9092(4) 0.9255(6) 0.6764(9) 0.0234(10) Uani 0.50 1 d PU . 1 O2B O 0.9536(3) 0.9046(4) 0.8733(6) 0.0235(8) Uani 0.50 1 d PU . 2 O3B O 0.8793(4) 0.9300(6) 0.6553(9) 0.0234(10) Uani 0.50 1 d PU . 2 O4 O 0.74375(14) 0.67324(12) 0.37040(16) 0.0317(4) Uani 1 1 d . . . O5A O 0.7117(3) 0.5759(2) 0.4547(3) 0.0302(6) Uani 0.50 1 d P . 1 O5B O 0.6620(3) 0.5958(2) 0.4502(3) 0.0302(6) Uani 0.50 1 d P . 2 O6 O 0.76458(12) 0.54443(10) 0.19627(16) 0.0236(3) Uani 1 1 d . . . O7 O 0.63626(13) 0.49945(13) 0.00339(16) 0.0328(4) Uani 1 1 d . . . O8 O 0.74568(17) 0.24139(12) -0.15776(19) 0.0411(5) Uani 1 1 d . . . O9 O 0.89839(14) 0.20430(10) -0.0110(2) 0.0327(4) Uani 1 1 d . . . O10A O 0.4880(5) 0.5997(4) 0.3468(6) 0.0639(14) Uani 0.50 1 d PU . -1 N1A N 0.5000 0.6966(3) 0.5000 0.0714(13) Uani 1 2 d SU . -1 C25A C 0.5244(8) 0.6254(5) 0.4597(9) 0.0656(15) Uani 0.50 1 d PU . -1 H25A H 0.5746 0.5934 0.5270 0.079 Uiso 0.50 1 calc PR . -1 C26A C 0.4489(5) 0.7466(4) 0.3887(6) 0.0992(18) Uani 1 1 d U . -1 H26A H 0.4312 0.7963 0.4109 0.149 Uiso 1 1 calc R . -1 H26B H 0.3881 0.7204 0.3203 0.149 Uiso 1 1 calc R . -1 H26C H 0.4927 0.7573 0.3591 0.149 Uiso 1 1 calc R . -1 O10B O 0.4238(3) 0.5325(3) 0.2456(4) 0.0342(8) Uani 0.50 1 d PD . -2 H10B H 0.408(2) 0.512(4) 0.295(3) 0.051 Uiso 0.50 1 d PD A -2 H10C H 0.3764(15) 0.531(5) 0.1664(13) 0.051 Uiso 0.50 1 d PD B -2 Zn1 Zn 0.5000 0.499950(16) 0.0000 0.01460(6) Uani 1 2 d S . . Zn2 Zn 0.685807(15) 0.637711(11) 0.187738(19) 0.01298(5) Uani 1 1 d . . . Zn3 Zn 0.570421(18) 0.539505(13) 0.30039(2) 0.01968(5) Uani 1 1 d D . . N2 N 1.0000 0.8283(3) 0.5000 0.0648(11) Uani 1 2 d SDU . . C27 C 1.0000 0.7440(4) 0.5000 0.096(2) Uani 1 2 d SDU . . H27A H 0.9449 0.7248 0.4162 0.145 Uiso 0.50 1 calc PR . . H27B H 0.9915 0.7248 0.5670 0.145 Uiso 0.50 1 calc PR . . H27C H 1.0635 0.7248 0.5167 0.145 Uiso 0.50 1 calc PR . . C28 C 0.9186(10) 0.8569(10) 0.3800(10) 0.091(4) Uani 0.50 1 d PDU . . H28A H 0.8802 0.8124 0.3245 0.136 Uiso 0.50 1 calc PR . . H28B H 0.9442 0.8886 0.3389 0.136 Uiso 0.50 1 calc PR . . H28C H 0.8753 0.8896 0.3940 0.136 Uiso 0.50 1 calc PR . . C29 C 1.0774(8) 0.8721(6) 0.5951(9) 0.0531(16) Uani 0.50 1 d PDU . . H29 H 1.1303 0.8418 0.6623 0.064 Uiso 0.50 1 calc PR . . O11 O 1.0897(5) 0.9403(5) 0.6082(6) 0.0728(15) Uani 0.50 1 d PDU . . 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 C1 0.0189(8) 0.0122(7) 0.0172(8) -0.0013(6) 0.0080(7) -0.0002(6) C2 0.0233(9) 0.0117(7) 0.0146(8) -0.0021(6) 0.0085(7) -0.0019(6) C3 0.0274(10) 0.0128(7) 0.0151(8) -0.0027(6) 0.0087(7) -0.0022(7) C4 0.0431(13) 0.0144(8) 0.0152(9) -0.0040(7) 0.0095(9) -0.0087(8) C5 0.0489(14) 0.0176(9) 0.0141(9) -0.0020(7) 0.0098(9) -0.0141(9) C6 0.0274(9) 0.0155(8) 0.0144(8) -0.0016(6) 0.0086(7) -0.0049(7) C7 0.0276(10) 0.0246(9) 0.0164(8) -0.0023(7) 0.0110(8) -0.0050(8) C8 0.0443(14) 0.0391(14) 0.0218(10) -0.0018(9) 0.0182(11) -0.0121(11) C9 0.084(2) 0.0462(17) 0.0236(12) 0.0057(11) 0.0212(15) -0.0306(17) C10 0.126(4) 0.0414(17) 0.0336(15) 0.0021(13) 0.028(2) -0.048(2) C11 0.106(3) 0.0307(14) 0.0232(12) -0.0051(10) 0.0192(16) -0.0391(18) C12 0.0542(15) 0.0138(9) 0.0145(8) -0.0027(7) 0.0070(9) -0.0057(10) C13 0.0244(9) 0.0165(8) 0.0246(9) 0.0042(7) 0.0168(8) 0.0076(7) C14 0.0178(8) 0.0147(8) 0.0232(9) 0.0007(6) 0.0124(7) 0.0036(6) C15 0.0190(8) 0.0140(8) 0.0219(8) 0.0000(7) 0.0114(7) 0.0025(6) C16 0.0196(8) 0.0135(7) 0.0227(9) -0.0010(6) 0.0128(7) 0.0030(6) C17 0.0184(8) 0.0144(8) 0.0231(9) -0.0002(6) 0.0114(7) 0.0040(6) C18 0.0184(8) 0.0163(8) 0.0234(9) -0.0031(7) 0.0110(7) 0.0037(6) C19 0.0235(10) 0.0309(11) 0.0337(12) -0.0135(9) 0.0104(10) 0.0046(8) C20 0.0265(12) 0.0455(16) 0.0391(15) -0.0231(12) 0.0034(11) 0.0043(11) C21 0.0202(11) 0.0419(15) 0.0444(16) -0.0134(12) 0.0046(11) 0.0048(10) C22 0.0184(10) 0.0300(11) 0.0400(13) -0.0047(10) 0.0108(10) 0.0063(8) C23 0.0204(9) 0.0201(9) 0.0314(11) -0.0018(8) 0.0138(9) 0.0059(7) C24 0.0313(10) 0.0145(8) 0.0292(10) -0.0026(7) 0.0223(9) -0.0019(7) O1 0.0138(6) 0.0124(5) 0.0170(6) -0.0010(4) 0.0074(5) -0.0001(4) O2A 0.030(2) 0.0147(11) 0.0162(12) -0.0053(9) 0.007(2) -0.0090(19) O3A 0.031(3) 0.0146(12) 0.014(3) 0.0006(15) 0.006(3) -0.003(3) O2B 0.030(2) 0.0147(11) 0.0162(12) -0.0053(9) 0.007(2) -0.0090(19) O3B 0.031(3) 0.0146(12) 0.014(3) 0.0006(15) 0.006(3) -0.003(3) O4 0.0325(9) 0.0385(9) 0.0174(7) -0.0135(7) 0.0097(7) -0.0017(7) O5A 0.0437(19) 0.0186(12) 0.0209(9) -0.0050(9) 0.0134(13) -0.0111(11) O5B 0.0437(19) 0.0186(12) 0.0209(9) -0.0050(9) 0.0134(13) -0.0111(11) O6 0.0237(7) 0.0183(6) 0.0294(7) -0.0032(6) 0.0151(6) 0.0045(6) O7 0.0262(8) 0.0475(11) 0.0209(7) 0.0011(7) 0.0108(6) 0.0212(8) O8 0.0518(12) 0.0274(9) 0.0268(9) -0.0075(7) 0.0111(8) 0.0047(8) O9 0.0275(8) 0.0195(7) 0.0475(11) -0.0096(7) 0.0188(8) 0.0026(6) O10A 0.077(3) 0.069(3) 0.060(3) 0.014(2) 0.046(3) 0.029(3) N1A 0.086(3) 0.037(2) 0.086(3) -0.006(3) 0.044(3) -0.005(5) C25A 0.091(4) 0.070(3) 0.076(3) -0.012(3) 0.072(3) -0.011(3) C26A 0.114(5) 0.114(4) 0.093(4) 0.032(4) 0.072(4) 0.016(4) O10B 0.0170(14) 0.059(2) 0.0287(16) -0.0028(17) 0.0137(13) -0.0029(15) Zn1 0.01590(13) 0.00895(12) 0.01493(13) 0.000 0.00610(11) 0.000 Zn2 0.01428(9) 0.00996(8) 0.01341(9) -0.00126(7) 0.00690(7) 0.00026(7) Zn3 0.02193(11) 0.01461(10) 0.02487(11) 0.00314(8) 0.01450(9) 0.00117(8) N2 0.047(2) 0.086(3) 0.064(2) 0.000 0.0330(18) 0.000 C27 0.073(4) 0.086(3) 0.175(7) 0.000 0.096(5) 0.000 C28 0.062(5) 0.150(6) 0.041(4) 0.017(5) 0.018(3) -0.026(6) C29 0.034(3) 0.092(3) 0.035(3) 0.025(2) 0.021(2) 0.003(3) O11 0.066(3) 0.095(3) 0.049(3) -0.019(3) 0.027(2) 0.012(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C1 O3A 1.240(12) . ? C1 O2B 1.254(7) . ? C1 O2A 1.261(7) . ? C1 O3B 1.307(11) . ? C1 C2 1.473(2) . ? C2 C3 1.402(3) . ? C2 C6 1.416(3) . ? C3 C4 1.396(3) . ? C3 H3 0.9300 . ? C4 C5 1.425(3) . ? C4 C12 1.467(3) . ? C5 C11 1.394(3) . ? C5 C6 1.477(3) . ? C6 C7 1.390(3) . ? C7 C8 1.392(3) . ? C7 H7 0.9300 . ? C8 C9 1.394(4) . ? C8 H8 0.9300 . ? C9 C10 1.384(5) . ? C9 H9 0.9300 . ? C10 C11 1.380(4) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 O5A 1.230(4) . ? C12 O4 1.264(3) . ? C12 O5B 1.402(5) . ? C13 O7 1.255(3) . ? C13 O6 1.271(3) . ? C13 C14 1.473(3) . ? C14 C15 1.401(3) . ? C14 C18 1.421(3) . ? C15 C16 1.402(3) . ? C15 H15 0.9300 . ? C16 C17 1.416(3) . ? C16 C24 1.480(3) . ? C17 C23 1.399(3) . ? C17 C18 1.478(3) . ? C18 C19 1.388(3) . ? C19 C20 1.410(3) . ? C19 H19 0.9300 . ? C20 C21 1.388(4) . ? C20 H20 0.9300 . ? C21 C22 1.387(4) . ? C21 H21 0.9300 . ? C22 C23 1.392(3) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 O9 1.246(3) . ? C24 O8 1.256(3) . ? C24 Zn2 2.502(2) 4_645 ? O1 Zn3 1.9501(14) . ? O1 Zn2 2.0263(13) . ? O1 Zn1 2.0971(13) . ? O1 H1 0.9800 . ? O2A Zn1 2.073(6) 3_556 ? O3A Zn3 1.919(10) 4_656 ? O2B Zn1 2.052(6) 3_556 ? O3B Zn3 1.941(10) 4_656 ? O4 Zn2 1.9844(16) . ? O5A Zn3 2.056(4) . ? O5B Zn3 1.842(3) . ? O6 Zn2 1.9555(15) . ? O7 Zn1 2.1292(18) . ? O8 Zn2 2.174(2) 4_645 ? O9 Zn2 2.1203(19) 4_645 ? O10A C25A 1.245(10) . ? O10A Zn3 1.962(5) . ? N1A C26A 1.409(6) . ? N1A C25A 1.418(9) . ? C25A H25A 0.9300 . ? C26A H26A 0.9600 . ? C26A H26B 0.9600 . ? C26A H26C 0.9600 . ? O10B Zn3 2.022(3) . ? O10B H10B 0.840(10) . ? O10B H10C 0.836(10) . ? Zn1 O2B 2.052(6) 3_444 ? Zn1 O2B 2.052(6) 4_646 ? Zn1 O2A 2.073(6) 3_444 ? Zn1 O2A 2.073(6) 4_646 ? Zn1 O1 2.0971(13) 2_655 ? Zn1 O7 2.1292(18) 2_655 ? Zn2 O9 2.1203(19) 4_655 ? Zn2 O8 2.174(2) 4_655 ? Zn2 C24 2.502(2) 4_655 ? Zn3 O3A 1.919(10) 4_646 ? Zn3 O3B 1.941(10) 4_646 ? N2 C29 1.342(10) . ? N2 C29 1.342(10) 2_756 ? N2 C28 1.394(8) 2_756 ? N2 C28 1.394(8) . ? N2 C27 1.403(7) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 O11 1.149(9) . ? C29 H29 0.9300 . ? O11 C28 1.409(19) 2_756 ? 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 O3A C1 O2B 118.2(5) . . ? O3A C1 O2A 124.0(6) . . ? O2B C1 O2A 23.3(3) . . ? O3A C1 O3B 17.8(5) . . ? O2B C1 O3B 126.6(5) . . ? O2A C1 O3B 124.1(6) . . ? O3A C1 C2 118.3(5) . . ? O2B C1 C2 119.5(3) . . ? O2A C1 C2 117.5(3) . . ? O3B C1 C2 113.8(5) . . ? C3 C2 C6 108.41(17) . . ? C3 C2 C1 122.55(18) . . ? C6 C2 C1 129.01(17) . . ? C4 C3 C2 109.92(18) . . ? C4 C3 H3 125.0 . . ? C2 C3 H3 125.0 . . ? C3 C4 C5 108.39(18) . . ? C3 C4 C12 122.4(2) . . ? C5 C4 C12 129.0(2) . . ? C11 C5 C4 125.9(2) . . ? C11 C5 C6 127.5(2) . . ? C4 C5 C6 106.42(18) . . ? C7 C6 C2 125.91(19) . . ? C7 C6 C5 127.21(19) . . ? C2 C6 C5 106.83(17) . . ? C6 C7 C8 129.0(2) . . ? C6 C7 H7 115.5 . . ? C8 C7 H7 115.5 . . ? C7 C8 C9 128.1(2) . . ? C7 C8 H8 115.9 . . ? C9 C8 H8 115.9 . . ? C10 C9 C8 129.9(3) . . ? C10 C9 H9 115.1 . . ? C8 C9 H9 115.1 . . ? C11 C10 C9 129.1(3) . . ? C11 C10 H10 115.4 . . ? C9 C10 H10 115.4 . . ? C10 C11 C5 128.6(3) . . ? C10 C11 H11 115.7 . . ? C5 C11 H11 115.7 . . ? O5A C12 O4 117.4(3) . . ? O5A C12 O5B 35.8(2) . . ? O4 C12 O5B 127.1(2) . . ? O5A C12 C4 123.1(3) . . ? O4 C12 C4 116.8(2) . . ? O5B C12 C4 112.6(3) . . ? O7 C13 O6 123.13(19) . . ? O7 C13 C14 118.41(19) . . ? O6 C13 C14 118.42(19) . . ? C15 C14 C18 108.32(17) . . ? C15 C14 C13 122.69(18) . . ? C18 C14 C13 128.98(19) . . ? C14 C15 C16 110.12(18) . . ? C14 C15 H15 124.9 . . ? C16 C15 H15 124.9 . . ? C15 C16 C17 107.93(17) . . ? C15 C16 C24 124.11(19) . . ? C17 C16 C24 127.96(18) . . ? C23 C17 C16 125.38(18) . . ? C23 C17 C18 127.23(19) . . ? C16 C17 C18 107.26(17) . . ? C19 C18 C14 125.74(19) . . ? C19 C18 C17 127.92(19) . . ? C14 C18 C17 106.32(17) . . ? C18 C19 C20 128.2(2) . . ? C18 C19 H19 115.9 . . ? C20 C19 H19 115.9 . . ? C21 C20 C19 128.9(2) . . ? C21 C20 H20 115.5 . . ? C19 C20 H20 115.5 . . ? C22 C21 C20 129.5(2) . . ? C22 C21 H21 115.2 . . ? C20 C21 H21 115.2 . . ? C21 C22 C23 129.2(2) . . ? C21 C22 H22 115.4 . . ? C23 C22 H22 115.4 . . ? C22 C23 C17 128.6(2) . . ? C22 C23 H23 115.7 . . ? C17 C23 H23 115.7 . . ? O9 C24 O8 118.1(2) . . ? O9 C24 C16 121.7(2) . . ? O8 C24 C16 120.2(2) . . ? O9 C24 Zn2 57.86(12) . 4_645 ? O8 C24 Zn2 60.35(13) . 4_645 ? C16 C24 Zn2 175.40(15) . 4_645 ? Zn3 O1 Zn2 110.83(6) . . ? Zn3 O1 Zn1 107.97(6) . . ? Zn2 O1 Zn1 111.75(6) . . ? Zn3 O1 H1 108.7 . . ? Zn2 O1 H1 108.7 . . ? Zn1 O1 H1 108.7 . . ? C1 O2A Zn1 141.0(4) . 3_556 ? C1 O3A Zn3 120.3(7) . 4_656 ? C1 O2B Zn1 144.1(4) . 3_556 ? C1 O3B Zn3 115.1(6) . 4_656 ? C12 O4 Zn2 133.35(17) . . ? C12 O5A Zn3 119.7(3) . . ? C12 O5B Zn3 124.0(3) . . ? C13 O6 Zn2 119.96(14) . . ? C13 O7 Zn1 129.21(15) . . ? C24 O8 Zn2 89.51(15) . 4_645 ? C24 O9 Zn2 92.29(15) . 4_645 ? C25A O10A Zn3 122.0(6) . . ? C26A N1A C25A 106.0(5) . . ? O10A C25A N1A 129.0(9) . . ? O10A C25A H25A 115.5 . . ? N1A C25A H25A 115.5 . . ? N1A C26A H26A 109.5 . . ? N1A C26A H26B 109.5 . . ? H26A C26A H26B 109.5 . . ? N1A C26A H26C 109.5 . . ? H26A C26A H26C 109.5 . . ? H26B C26A H26C 109.5 . . ? Zn3 O10B H10B 121.5(19) . . ? Zn3 O10B H10C 120.5(19) . . ? H10B O10B H10C 113(2) . . ? O2B Zn1 O2B 78.6(4) 3_444 4_646 ? O2B Zn1 O2A 14.16(16) 3_444 3_444 ? O2B Zn1 O2A 82.58(12) 4_646 3_444 ? O2B Zn1 O2A 82.58(12) 3_444 4_646 ? O2B Zn1 O2A 14.16(16) 4_646 4_646 ? O2A Zn1 O2A 89.5(3) 3_444 4_646 ? O2B Zn1 O1 174.05(19) 3_444 . ? O2B Zn1 O1 95.41(18) 4_646 . ? O2A Zn1 O1 166.18(15) 3_444 . ? O2A Zn1 O1 91.64(18) 4_646 . ? O2B Zn1 O1 95.41(18) 3_444 2_655 ? O2B Zn1 O1 174.05(19) 4_646 2_655 ? O2A Zn1 O1 91.64(18) 3_444 2_655 ? O2A Zn1 O1 166.18(15) 4_646 2_655 ? O1 Zn1 O1 90.54(7) . 2_655 ? O2B Zn1 O7 92.98(14) 3_444 2_655 ? O2B Zn1 O7 86.67(14) 4_646 2_655 ? O2A Zn1 O7 79.60(14) 3_444 2_655 ? O2A Zn1 O7 100.08(15) 4_646 2_655 ? O1 Zn1 O7 86.65(6) . 2_655 ? O1 Zn1 O7 93.67(6) 2_655 2_655 ? O2B Zn1 O7 86.67(14) 3_444 . ? O2B Zn1 O7 92.98(14) 4_646 . ? O2A Zn1 O7 100.08(14) 3_444 . ? O2A Zn1 O7 79.60(14) 4_646 . ? O1 Zn1 O7 93.67(6) . . ? O1 Zn1 O7 86.65(6) 2_655 . ? O7 Zn1 O7 179.55(12) 2_655 . ? O6 Zn2 O4 107.27(7) . . ? O6 Zn2 O1 103.23(6) . . ? O4 Zn2 O1 99.88(7) . . ? O6 Zn2 O9 119.17(8) . 4_655 ? O4 Zn2 O9 129.34(8) . 4_655 ? O1 Zn2 O9 88.72(6) . 4_655 ? O6 Zn2 O8 106.10(8) . 4_655 ? O4 Zn2 O8 89.75(8) . 4_655 ? O1 Zn2 O8 144.73(7) . 4_655 ? O9 Zn2 O8 59.95(7) 4_655 4_655 ? O6 Zn2 C24 117.32(7) . 4_655 ? O4 Zn2 C24 110.59(8) . 4_655 ? O1 Zn2 C24 116.77(7) . 4_655 ? O9 Zn2 C24 29.85(7) 4_655 4_655 ? O8 Zn2 C24 30.14(7) 4_655 4_655 ? O5B Zn3 O3A 112.4(2) . 4_646 ? O5B Zn3 O3B 103.1(2) . 4_646 ? O3A Zn3 O3B 11.9(3) 4_646 4_646 ? O5B Zn3 O1 111.63(12) . . ? O3A Zn3 O1 118.7(3) 4_646 . ? O3B Zn3 O1 118.7(3) 4_646 . ? O5B Zn3 O10A 74.2(2) . . ? O3A Zn3 O10A 123.0(4) 4_646 . ? O3B Zn3 O10A 129.2(4) 4_646 . ? O1 Zn3 O10A 108.46(17) . . ? O5B Zn3 O10B 118.57(18) . . ? O3A Zn3 O10B 93.4(3) 4_646 . ? O3B Zn3 O10B 104.7(3) 4_646 . ? O1 Zn3 O10B 100.85(12) . . ? O10A Zn3 O10B 45.9(2) . . ? O5B Zn3 O5A 23.61(15) . . ? O3A Zn3 O5A 98.51(19) 4_646 . ? O3B Zn3 O5A 87.31(19) 4_646 . ? O1 Zn3 O5A 105.50(11) . . ? O10A Zn3 O5A 97.8(2) . . ? O10B Zn3 O5A 140.98(17) . . ? C29 N2 C29 114.3(10) . 2_756 ? C29 N2 C28 15.5(9) . 2_756 ? C29 N2 C28 126.3(8) 2_756 2_756 ? C29 N2 C28 126.3(8) . . ? C29 N2 C28 15.5(9) 2_756 . ? C28 N2 C28 140.0(14) 2_756 . ? C29 N2 C27 122.9(5) . . ? C29 N2 C27 122.9(5) 2_756 . ? C28 N2 C27 110.0(7) 2_756 . ? C28 N2 C27 110.0(7) . . ? N2 C27 H27A 109.5 . . ? N2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N2 C28 H28A 109.5 . . ? N2 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N2 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O11 C29 N2 131.3(9) . . ? O11 C29 H29 114.4 . . ? N2 C29 H29 114.4 . . ? C29 O11 C28 12.0(8) . 2_756 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 32.57 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.950 _refine_diff_density_min -0.680 _refine_diff_density_rms 0.087 #===END data_MOF646 _database_code_depnum_ccdc_archive 'CCDC 771571' #TrackingRef 'Revised-CIF.cif' # start Validation Reply Form _vrf_PLAT220_MOF646 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 8.82 Ratio RESPONSE: The largest Ueq(C) values are observed for carbon atoms of a coordinated DMF molecule (Ueq(max) = 0.087 for C81). For this kind of molecule, this value is acceptable but the structure contains also very well defined carbon atoms like C27 (Ueq = 0.011) or C14 (Ueq = 0.015) which gives a non-relevant large ratio. ; _vrf_PLAT222_MOF646 ; PROBLEM: Large Non-Solvent H Uiso(max)/Uso(min) ... 10.00 Rati RESPONSE: This is a consequence of the large ratio for Ueq(C) explained above.. ; _vrf_PLAT430_MOF646 ; PROBLEM: Short Inter D...A Contact O33W .. O36W .. 2.12 Ang. RESPONSE: Disordered water molecules which do not belong to the same asymmetric unit. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Zn~4~(\m~4~-O)(L)~3~(DMF)~2~].(DMF)~1.25~.(H~2~O) [L = 1,3-azulene dicarboxylate] ; _chemical_name_common ; (Zn!4$(mu!4$-O)(L)!3$(DMF)!2$).(DMF)!1.25$.(H!2$O) (L = 1,3- azulene dicarboxylate) ; _chemical_melting_point ? _chemical_formula_moiety '2(C84 H64 N4 O30 Zn8), 5(C3 H7 N O), 4(H2 O)' _chemical_formula_sum 'C183 H171 N13 O69 Zn16' _chemical_formula_weight 4702.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 17.2344(6) _cell_length_b 17.2237(6) _cell_length_c 17.2923(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.548(4) _cell_angle_gamma 90.00 _cell_volume 5132.8(3) _cell_formula_units_Z 1 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 7405 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 28.84 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.521 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2392 _exptl_absorpt_coefficient_mu 1.918 _exptl_absorpt_correction_T_min 0.848 _exptl_absorpt_correction_T_max 0.924 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Goniometer Xcalibur, detector: Ruby Oxford Diffraction (2007). Oxford Diffraction Ltd., Xcalibur CCD system ; _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 5.2249 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 30148 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_sigmaI/netI 0.1737 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 25.68 _reflns_number_total 17700 _reflns_number_gt 11043 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_structure_solution ; SHELXS97. Program for Crystal Structure solution. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _computing_structure_refinement ; SHELXL97. Program for crystal structure refinement. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _computing_molecular_graphics ; ORTEP-3 for Windows, Version 2.01. Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. ; _computing_publication_material ; WinGX -- An integrated system of Windows programs for the solution, refinment and analysis of single crystal X-ray diffraction data, Version 1.80.00. Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838. SHELXL97. Program for crystal structure refinement. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. PLATON for Windows, Version 1.12. Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0369P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881. 6626 Friedel pairs' _refine_ls_abs_structure_Flack -0.003(11) _refine_ls_number_reflns 17700 _refine_ls_number_parameters 1302 _refine_ls_number_restraints 245 _refine_ls_R_factor_all 0.0849 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.0996 _refine_ls_wR_factor_gt 0.0931 _refine_ls_goodness_of_fit_ref 0.843 _refine_ls_restrained_S_all 0.845 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9944(5) 0.4505(4) 0.9628(5) 0.0160(16) Uani 1 1 d U . . C2 C 1.0565(4) 0.3956(4) 0.9486(5) 0.019(2) Uani 1 1 d . . . C3 C 1.0619(5) 0.3246(4) 0.9866(5) 0.018(2) Uani 1 1 d . . . H3 H 1.0271 0.3066 1.0233 0.022 Uiso 1 1 calc R . . C4 C 1.1284(5) 0.2839(4) 0.9613(5) 0.021(2) Uani 1 1 d . . . C5 C 1.1646(5) 0.3295(4) 0.9044(6) 0.026(2) Uani 1 1 d . . . C6 C 1.1194(5) 0.4018(5) 0.8957(5) 0.027(2) Uani 1 1 d . . . C7 C 1.2297(6) 0.3055(5) 0.8613(6) 0.043(3) Uani 1 1 d . . . H7 H 1.2494 0.2566 0.8734 0.051 Uiso 1 1 calc R . . C8 C 1.2690(6) 0.3461(7) 0.8020(8) 0.080(5) Uani 1 1 d . . . H8 H 1.3106 0.3207 0.7793 0.096 Uiso 1 1 calc R . . C9 C 1.2513(6) 0.4220(6) 0.7734(7) 0.065(4) Uani 1 1 d . . . H9 H 1.2852 0.4409 0.7363 0.078 Uiso 1 1 calc R . . C10 C 1.1927(6) 0.4703(6) 0.7923(6) 0.051(3) Uani 1 1 d . . . H10 H 1.1923 0.5171 0.7654 0.061 Uiso 1 1 calc R . . C11 C 1.1328(5) 0.4622(5) 0.8451(6) 0.038(3) Uani 1 1 d . . . H11 H 1.0972 0.5028 0.8464 0.045 Uiso 1 1 calc R . . C12 C 1.1514(5) 0.2067(5) 0.9916(5) 0.018(2) Uani 1 1 d . . . C13 C 0.7700(5) 0.5061(5) 1.1611(5) 0.022(2) Uani 1 1 d . . . C14 C 0.7532(4) 0.4812(5) 1.2416(4) 0.0149(18) Uani 1 1 d . . . C15 C 0.7677(4) 0.4057(5) 1.2660(5) 0.021(2) Uani 1 1 d . . . H15 H 0.7926 0.3681 1.2368 0.025 Uiso 1 1 calc R . . C16 C 0.7395(4) 0.3939(4) 1.3408(5) 0.0157(19) Uani 1 1 d . . . C17 C 0.7045(5) 0.4646(4) 1.3661(5) 0.0202(16) Uani 1 1 d U . . C18 C 0.7150(5) 0.5200(5) 1.3002(5) 0.0241(17) Uani 1 1 d U . . C19 C 0.6715(5) 0.4795(5) 1.4368(5) 0.0267(17) Uani 1 1 d U . . H19 H 0.6717 0.4382 1.4715 0.032 Uiso 1 1 calc R . . C20 C 0.6380(5) 0.5479(5) 1.4633(5) 0.0397(19) Uani 1 1 d U . . H20 H 0.6186 0.5459 1.5132 0.048 Uiso 1 1 calc R . . C21 C 0.6293(7) 0.6181(5) 1.4262(6) 0.048(2) Uani 1 1 d U . . H21 H 0.6021 0.6553 1.4539 0.058 Uiso 1 1 calc R . . C22 C 0.6538(6) 0.6418(6) 1.3561(6) 0.049(2) Uani 1 1 d U . . H22 H 0.6441 0.6935 1.3440 0.059 Uiso 1 1 calc R . . C23 C 0.6916(6) 0.5991(5) 1.2998(6) 0.037(2) Uani 1 1 d U . . H23 H 0.7034 0.6264 1.2551 0.044 Uiso 1 1 calc R . . C24 C 0.7409(5) 0.3188(5) 1.3793(5) 0.018(2) Uani 1 1 d . . . C25 C 0.7921(5) 0.3296(5) 0.8652(5) 0.0151(19) Uani 1 1 d . . . C26 C 0.8071(5) 0.2615(4) 0.8142(5) 0.0146(19) Uani 1 1 d . . . C27 C 0.7704(4) 0.2539(4) 0.7419(4) 0.0108(18) Uani 1 1 d . . . H27 H 0.7334 0.2880 0.7219 0.013 Uiso 1 1 calc R . . C28 C 0.7972(5) 0.1879(4) 0.7044(5) 0.017(2) Uani 1 1 d . . . C29 C 0.8527(5) 0.1521(5) 0.7529(5) 0.028(2) Uani 1 1 d . . . C30 C 0.8587(5) 0.1996(5) 0.8234(5) 0.020(2) Uani 1 1 d . . . C31 C 0.8960(6) 0.0863(6) 0.7347(6) 0.057(4) Uani 1 1 d . . . H31 H 0.8859 0.0642 0.6865 0.068 Uiso 1 1 calc R . . C32 C 0.9525(7) 0.0495(7) 0.7794(7) 0.084(5) Uani 1 1 d . . . H32 H 0.9756 0.0066 0.7564 0.101 Uiso 1 1 calc R . . C33 C 0.9792(7) 0.0669(6) 0.8524(7) 0.071(4) Uani 1 1 d . . . H33 H 1.0176 0.0339 0.8714 0.086 Uiso 1 1 calc R . . C34 C 0.9585(7) 0.1241(6) 0.9005(6) 0.049(3) Uani 1 1 d . . . H34 H 0.9821 0.1234 0.9490 0.059 Uiso 1 1 calc R . . C35 C 0.9050(5) 0.1859(5) 0.8868(5) 0.031(2) Uani 1 1 d . . . H35 H 0.9009 0.2220 0.9266 0.038 Uiso 1 1 calc R . . C36 C 0.7699(5) 0.1676(4) 0.6263(5) 0.018(2) Uani 1 1 d . . . C37 C 0.8579(5) 0.5431(4) 0.7645(4) 0.017(2) Uani 1 1 d . . . C38 C 0.9128(5) 0.5280(4) 0.6999(5) 0.019(2) Uani 1 1 d . . . C39 C 0.9842(4) 0.5625(5) 0.6954(4) 0.0201(18) Uani 1 1 d . . . H39 H 1.0017 0.6007 0.7294 0.024 Uiso 1 1 calc R . . C40 C 1.0270(5) 0.5342(5) 0.6351(5) 0.025(2) Uani 1 1 d . . . C41 C 0.9818(5) 0.4790(5) 0.5961(5) 0.031(2) Uani 1 1 d . . . C42 C 0.9084(5) 0.4723(5) 0.6403(5) 0.023(2) Uani 1 1 d . . . C43 C 1.0012(6) 0.4336(6) 0.5335(5) 0.042(3) Uani 1 1 d . . . H43 H 1.0495 0.4454 0.5130 0.050 Uiso 1 1 calc R . . C44 C 0.9630(6) 0.3736(6) 0.4946(6) 0.046(3) Uani 1 1 d . . . H44 H 0.9896 0.3505 0.4541 0.056 Uiso 1 1 calc R . . C45 C 0.8886(6) 0.3441(6) 0.5101(6) 0.043(3) Uani 1 1 d . . . H45 H 0.8708 0.3049 0.4776 0.052 Uiso 1 1 calc R . . C46 C 0.8381(6) 0.3671(6) 0.5691(6) 0.044(3) Uani 1 1 d . . . H46 H 0.7918 0.3396 0.5712 0.052 Uiso 1 1 calc R . . C47 C 0.8467(5) 0.4236(5) 0.6237(5) 0.030(2) Uani 1 1 d . . . H47 H 0.8037 0.4306 0.6552 0.036 Uiso 1 1 calc R . . C48 C 1.1047(4) 0.5609(5) 0.6156(5) 0.0197(19) Uani 1 1 d . . . C49 C 0.6769(5) 0.3596(5) 1.0839(6) 0.032(2) Uani 1 1 d . . . H49 H 0.7091 0.3331 1.1184 0.039 Uiso 1 1 calc R A . N1A N 0.5994(16) 0.357(2) 1.0928(19) 0.072(6) Uani 0.478(15) 1 d PDU A -1 C50A C 0.5509(14) 0.3840(15) 1.0292(17) 0.080(6) Uani 0.478(15) 1 d PDU A -1 H50A H 0.4973 0.3784 1.0426 0.119 Uiso 0.478(15) 1 calc PR A -1 H50B H 0.5614 0.3539 0.9838 0.119 Uiso 0.478(15) 1 calc PR A -1 H50C H 0.5619 0.4377 1.0191 0.119 Uiso 0.478(15) 1 calc PR A -1 C51A C 0.5615(17) 0.3230(17) 1.1600(19) 0.073(6) Uani 0.478(15) 1 d PDU A -1 H51A H 0.5065 0.3310 1.1559 0.109 Uiso 0.478(15) 1 calc PR A -1 H51B H 0.5809 0.3474 1.2062 0.109 Uiso 0.478(15) 1 calc PR A -1 H51C H 0.5722 0.2684 1.1620 0.109 Uiso 0.478(15) 1 calc PR A -1 N1B N 0.6130(15) 0.3609(18) 1.1199(17) 0.071(6) Uani 0.522(15) 1 d PDU A -2 C50B C 0.5647(13) 0.4295(11) 1.1090(17) 0.081(6) Uani 0.522(15) 1 d PDU A -2 H50D H 0.5963 0.4720 1.0920 0.121 Uiso 0.522(15) 1 calc PR A -2 H50E H 0.5406 0.4429 1.1570 0.121 Uiso 0.522(15) 1 calc PR A -2 H50F H 0.5254 0.4189 1.0708 0.121 Uiso 0.522(15) 1 calc PR A -2 C51B C 0.5954(13) 0.3111(14) 1.1860(16) 0.063(6) Uani 0.522(15) 1 d PDU A -2 H51D H 0.6371 0.2748 1.1939 0.095 Uiso 0.522(15) 1 calc PR A -2 H51E H 0.5481 0.2832 1.1759 0.095 Uiso 0.522(15) 1 calc PR A -2 H51F H 0.5895 0.3424 1.2314 0.095 Uiso 0.522(15) 1 calc PR A -2 C52 C 0.9022(5) 0.3185(5) 1.1339(5) 0.025(2) Uani 1 1 d . . . H52 H 0.9204 0.3673 1.1483 0.030 Uiso 1 1 calc R . . C53 C 0.9077(5) 0.1796(5) 1.1480(5) 0.036(3) Uani 1 1 d . . . H53A H 0.8799 0.1573 1.1904 0.055 Uiso 1 1 calc R . . H53B H 0.9524 0.1484 1.1371 0.055 Uiso 1 1 calc R . . H53C H 0.8745 0.1815 1.1031 0.055 Uiso 1 1 calc R . . C54 C 0.9876(7) 0.2669(6) 1.2332(6) 0.066(4) Uani 1 1 d . . . H54A H 0.9993 0.3209 1.2407 0.100 Uiso 1 1 calc R . . H54B H 1.0344 0.2391 1.2219 0.100 Uiso 1 1 calc R . . H54C H 0.9650 0.2462 1.2794 0.100 Uiso 1 1 calc R . . C55 C 0.6010(4) 0.5640(5) 0.9161(5) 0.0144(15) Uani 1 1 d U . . C56 C 0.5187(4) 0.5823(4) 0.8989(4) 0.0154(14) Uani 1 1 d U . . C57 C 0.4839(4) 0.5693(5) 0.8266(4) 0.0143(14) Uani 1 1 d U . . H57 H 0.5088 0.5465 0.7849 0.017 Uiso 1 1 calc R . . C58 C 0.4077(4) 0.5946(4) 0.8255(5) 0.0164(16) Uani 1 1 d U . . C59 C 0.3580(5) 0.5941(4) 0.7565(5) 0.0179(18) Uani 1 1 d U . . C60 C 0.4628(5) 0.6139(5) 0.9486(5) 0.0216(18) Uani 1 1 d U . . C61 C 0.4730(6) 0.6329(6) 1.0258(6) 0.053(3) Uani 1 1 d . . . H61 H 0.5226 0.6241 1.0454 0.063 Uiso 1 1 calc R . . C62 C 0.4199(6) 0.6635(8) 1.0795(6) 0.074(4) Uani 1 1 d . . . H62 H 0.4380 0.6677 1.1302 0.088 Uiso 1 1 calc R . . C63 C 0.3427(6) 0.6888(9) 1.0663(6) 0.082(5) Uani 1 1 d . . . H63 H 0.3181 0.7130 1.1074 0.098 Uiso 1 1 calc R . . C64 C 0.3011(6) 0.6814(6) 1.0001(6) 0.052(3) Uani 1 1 d . . . H64 H 0.2497 0.6972 1.0045 0.062 Uiso 1 1 calc R . . C65 C 0.3195(5) 0.6553(6) 0.9273(5) 0.033(2) Uani 1 1 d . . . H65 H 0.2805 0.6589 0.8899 0.039 Uiso 1 1 calc R . . C66 C 0.3906(5) 0.6237(5) 0.9030(5) 0.023(2) Uani 1 1 d . . . C67 C 0.3176(5) 0.4226(5) 0.4999(6) 0.031(3) Uani 1 1 d . . . C68 C 0.3543(5) 0.3505(5) 0.4636(5) 0.027(2) Uani 1 1 d . . . C69 C 0.4242(5) 0.3222(5) 0.4842(5) 0.023(2) Uani 1 1 d . . . H69 H 0.4544 0.3413 0.5248 0.027 Uiso 1 1 calc R . . C70 C 0.4458(5) 0.2600(5) 0.4366(5) 0.025(2) Uani 1 1 d . . . C71 C 0.3876(5) 0.2497(5) 0.3820(6) 0.031(2) Uani 1 1 d . . . C72 C 0.3264(6) 0.3078(5) 0.3994(6) 0.040(3) Uani 1 1 d . . . C73 C 0.3841(6) 0.1934(6) 0.3245(7) 0.050(3) Uani 1 1 d . . . H73 H 0.4272 0.1612 0.3219 0.060 Uiso 1 1 calc R . . C74 C 0.3256(6) 0.1777(6) 0.2696(7) 0.064(4) Uani 1 1 d . . . H74 H 0.3361 0.1376 0.2352 0.076 Uiso 1 1 calc R . . C75 C 0.2536(6) 0.2143(7) 0.2598(7) 0.071(4) Uani 1 1 d . . . H75 H 0.2225 0.1946 0.2201 0.086 Uiso 1 1 calc R . . C76 C 0.2221(7) 0.2758(6) 0.3009(7) 0.074(5) Uani 1 1 d . . . H76 H 0.1729 0.2917 0.2853 0.089 Uiso 1 1 calc R . . C77 C 0.2545(6) 0.3160(6) 0.3616(7) 0.070(5) Uani 1 1 d . . . H77 H 0.2234 0.3555 0.3810 0.084 Uiso 1 1 calc R . . C78 C 0.5190(5) 0.2181(5) 0.4434(5) 0.022(2) Uani 1 1 d . . . C79 C 0.4531(5) 0.5207(6) 0.4259(6) 0.039(2) Uani 1 1 d U . . H79 H 0.4770 0.4796 0.4514 0.047 Uiso 1 1 calc R . . C80 C 0.4927(7) 0.4573(7) 0.3091(7) 0.076(4) Uani 1 1 d U . . H80A H 0.5101 0.4181 0.3447 0.114 Uiso 1 1 calc R . . H80B H 0.5362 0.4768 0.2808 0.114 Uiso 1 1 calc R . . H80C H 0.4555 0.4354 0.2737 0.114 Uiso 1 1 calc R . . C81 C 0.4307(8) 0.5904(8) 0.3091(7) 0.097(4) Uani 1 1 d U . . H81A H 0.3839 0.5786 0.2808 0.146 Uiso 1 1 calc R . . H81B H 0.4703 0.6061 0.2736 0.146 Uiso 1 1 calc R . . H81C H 0.4209 0.6318 0.3449 0.146 Uiso 1 1 calc R . . C82 C 0.4974(5) 0.4420(5) 0.6502(5) 0.029(2) Uani 1 1 d . . . H82 H 0.4487 0.4253 0.6655 0.034 Uiso 1 1 calc R . . C83 C 0.6336(6) 0.4270(7) 0.6588(6) 0.060(4) Uani 1 1 d . . . H83A H 0.6535 0.3965 0.6170 0.089 Uiso 1 1 calc R . . H83B H 0.6661 0.4203 0.7037 0.089 Uiso 1 1 calc R . . H83C H 0.6330 0.4808 0.6442 0.089 Uiso 1 1 calc R . . C84 C 0.5511(7) 0.3309(7) 0.7192(8) 0.094(6) Uani 1 1 d . . . H84A H 0.5791 0.3358 0.7672 0.142 Uiso 1 1 calc R . . H84B H 0.5725 0.2890 0.6897 0.142 Uiso 1 1 calc R . . H84C H 0.4975 0.3206 0.7295 0.142 Uiso 1 1 calc R . . N2 N 0.9325(4) 0.2583(4) 1.1684(4) 0.030(2) Uani 1 1 d . . . N3 N 0.4568(5) 0.5208(5) 0.3519(5) 0.055(2) Uani 1 1 d U . . N4 N 0.5576(4) 0.4027(4) 0.6757(5) 0.034(2) Uani 1 1 d . . . O1 O 0.8002(3) 0.5114(3) 0.9550(3) 0.0098(12) Uani 1 1 d . A . O2 O 0.9874(3) 0.5108(3) 0.9192(3) 0.0220(13) Uani 1 1 d U . . O3 O 0.9469(3) 0.4347(3) 1.0157(3) 0.0186(12) Uani 1 1 d U A . O4 O 1.0988(3) 0.1704(3) 1.0277(3) 0.0195(14) Uani 1 1 d . . . O5 O 1.2186(3) 0.1818(3) 0.9807(4) 0.0267(15) Uani 1 1 d . . . O6 O 0.8235(3) 0.4754(3) 1.1255(3) 0.0218(14) Uani 1 1 d . A . O7 O 0.7234(3) 0.5586(3) 1.1317(3) 0.0210(13) Uani 1 1 d . A . O8 O 0.7754(3) 0.2636(3) 1.3413(3) 0.0209(14) Uani 1 1 d . . . O9 O 0.7072(3) 0.3088(3) 1.4418(3) 0.0224(14) Uani 1 1 d . . . O10 O 0.8370(3) 0.3426(3) 0.9207(3) 0.0193(14) Uani 1 1 d . A . O11 O 0.7326(3) 0.3707(3) 0.8460(3) 0.0189(14) Uani 1 1 d . . . O12 O 0.7992(3) 0.1089(3) 0.5936(3) 0.0250(15) Uani 1 1 d . . . O13 O 0.7177(3) 0.2107(3) 0.5968(3) 0.0176(13) Uani 1 1 d . . . O14 O 0.7955(3) 0.5046(3) 0.7693(3) 0.0211(14) Uani 1 1 d . . . O15 O 0.8791(3) 0.5928(3) 0.8131(3) 0.0156(13) Uani 1 1 d . . . O16 O 1.1347(3) 0.5359(3) 0.5532(4) 0.0343(17) Uani 1 1 d . . . O17 O 1.1378(3) 0.6082(3) 0.6617(3) 0.0205(14) Uani 1 1 d . . . O18 O 0.7055(3) 0.3969(3) 1.0304(4) 0.0299(16) Uani 1 1 d . A . O19 O 0.8513(3) 0.3156(3) 1.0836(4) 0.0250(15) Uani 1 1 d . A . O20 O 0.6360(3) 0.5269(3) 0.8637(3) 0.0176(14) Uani 1 1 d . . . O21 O 0.6308(3) 0.5861(3) 0.9792(3) 0.0180(14) Uani 1 1 d . A . O22 O 0.3772(3) 0.5498(3) 0.7037(3) 0.0169(13) Uani 1 1 d . . . O23 O 0.2976(3) 0.6380(3) 0.7558(3) 0.0241(15) Uani 1 1 d . . . O24 O 0.2984(3) 0.6203(3) 0.5650(3) 0.0094(12) Uani 1 1 d . . . O25 O 0.2629(3) 0.4560(3) 0.4616(4) 0.0359(18) Uani 1 1 d . . . O26 O 0.3480(3) 0.4478(3) 0.5615(3) 0.0248(15) Uani 1 1 d . . . O27 O 0.5368(3) 0.1655(3) 0.3959(3) 0.0248(15) Uani 1 1 d . . . O28 O 0.5630(3) 0.2410(3) 0.4983(3) 0.0178(13) Uani 1 1 d . . . O29 O 0.4204(3) 0.5704(4) 0.4672(3) 0.0271(14) Uani 1 1 d . . . O30 O 0.5002(3) 0.4999(3) 0.6070(3) 0.0259(15) Uani 1 1 d . . . Zn1 Zn 0.88990(5) 0.56809(5) 0.92450(5) 0.0126(2) Uani 1 1 d . . . Zn2 Zn 0.82705(6) 0.41445(5) 1.01620(5) 0.0130(2) Uani 1 1 d . . . Zn3 Zn 0.73754(5) 0.57579(5) 1.02102(5) 0.0119(2) Uani 1 1 d . . . Zn4 Zn 0.73953(5) 0.48201(5) 0.86597(5) 0.0125(2) Uani 1 1 d . A . Zn5 Zn 0.39887(5) 0.56340(6) 0.58680(5) 0.0149(2) Uani 1 1 d . . . Zn6 Zn 0.24293(5) 0.65183(5) 0.65566(5) 0.0119(2) Uani 1 1 d . . . Zn7 Zn 0.32845(5) 0.71087(5) 0.50658(6) 0.0133(2) Uani 1 1 d . . . Zn8 Zn 0.23301(5) 0.55540(5) 0.50194(5) 0.0130(2) Uani 1 1 d . . . C85 C 0.9018(11) 0.6824(10) 0.5549(13) 0.122(7) Uani 1 1 d . . . H85 H 0.8524 0.6750 0.5748 0.146 Uiso 1 1 calc R . . C86 C 0.9932(8) 0.6491(9) 0.4478(10) 0.120(7) Uani 1 1 d . . . H86A H 0.9868 0.6860 0.4067 0.180 Uiso 1 1 calc R . . H86B H 1.0076 0.5997 0.4266 0.180 Uiso 1 1 calc R . . H86C H 1.0332 0.6667 0.4827 0.180 Uiso 1 1 calc R . . C87 C 0.8611(12) 0.5966(10) 0.4552(11) 0.193(12) Uani 1 1 d . . . H87A H 0.8381 0.6253 0.4133 0.290 Uiso 1 1 calc R . . H87B H 0.8221 0.5846 0.4927 0.290 Uiso 1 1 calc R . . H87C H 0.8831 0.5493 0.4359 0.290 Uiso 1 1 calc R . . N5 N 0.9194(9) 0.6412(8) 0.4901(8) 0.100(4) Uani 1 1 d . . . O31 O 0.9457(7) 0.7302(7) 0.5915(7) 0.141(5) Uani 1 1 d . . . C88 C 1.0907(9) 0.2138(9) 0.7521(10) 0.098(3) Uani 1 1 d U . . H88 H 1.0588 0.1995 0.7927 0.118 Uiso 1 1 calc R . . C89 C 1.1348(10) 0.2937(9) 0.6539(11) 0.140(5) Uani 1 1 d U . . H89A H 1.1861 0.2855 0.6743 0.210 Uiso 1 1 calc R . . H89B H 1.1297 0.3466 0.6369 0.210 Uiso 1 1 calc R . . H89C H 1.1260 0.2595 0.6109 0.210 Uiso 1 1 calc R . . C90 C 1.0109(8) 0.3228(7) 0.7332(9) 0.095(4) Uani 1 1 d U . . H90A H 0.9738 0.3199 0.6914 0.142 Uiso 1 1 calc R . . H90B H 1.0261 0.3759 0.7410 0.142 Uiso 1 1 calc R . . H90C H 0.9879 0.3031 0.7796 0.142 Uiso 1 1 calc R . . N6 N 1.0770(7) 0.2778(7) 0.7148(8) 0.093(3) Uani 1 1 d U . . O32 O 1.1442(7) 0.1727(6) 0.7349(7) 0.138(4) Uani 1 1 d U . . N7 N 0.5751(10) 0.7953(9) 1.0728(9) 0.081(4) Uani 0.50 1 d PD B 1 C91 C 0.6183(13) 0.7985(12) 1.0028(10) 0.081(4) Uani 0.50 1 d PD B 1 H91A H 0.6002 0.8412 0.9719 0.121 Uiso 0.50 1 calc PR B 1 H91B H 0.6114 0.7510 0.9747 0.121 Uiso 0.50 1 calc PR B 1 H91C H 0.6723 0.8056 1.0149 0.121 Uiso 0.50 1 calc PR B 1 C92 C 0.5222(12) 0.8564(11) 1.0916(12) 0.081(4) Uani 0.50 1 d PD B 1 H92A H 0.4971 0.8446 1.1395 0.121 Uiso 0.50 1 calc PR B 1 H92B H 0.4839 0.8612 1.0513 0.121 Uiso 0.50 1 calc PR B 1 H92C H 0.5501 0.9044 1.0967 0.121 Uiso 0.50 1 calc PR B 1 C93 C 0.5905(10) 0.7367(8) 1.1295(9) 0.081(4) Uani 0.50 1 d PD B 1 H93 H 0.6218 0.6966 1.1118 0.097 Uiso 0.50 1 calc PR B 1 O33 O 0.5712(10) 0.7293(9) 1.1946(9) 0.081(4) Uani 0.50 1 d PD B 1 O34W O 0.5600(12) 0.5725(14) 1.1797(12) 0.125(7) Uiso 0.50 1 d P C 2 O33W O 0.2788(16) 0.4638(16) 1.1041(16) 0.179(11) Uiso 0.50 1 d P D 1 O36W O 0.3978(14) 0.4653(13) 1.1372(14) 0.138(8) Uiso 0.50 1 d P E 2 O35W O 1.3514(15) 0.3250(14) 0.6598(15) 0.145(9) Uiso 0.50 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 C1 0.011(4) 0.015(3) 0.021(4) -0.003(3) -0.005(3) 0.000(3) C2 0.007(4) 0.024(5) 0.027(6) 0.014(4) 0.004(4) 0.003(4) C3 0.015(5) 0.013(4) 0.026(5) 0.000(4) 0.003(4) -0.002(4) C4 0.017(5) 0.011(4) 0.036(6) 0.001(4) 0.011(4) 0.000(4) C5 0.017(5) 0.010(4) 0.052(7) 0.001(5) 0.006(5) 0.000(4) C6 0.012(5) 0.027(5) 0.041(6) 0.009(5) 0.004(4) 0.005(4) C7 0.029(6) 0.020(5) 0.080(9) 0.020(6) 0.016(6) 0.005(5) C8 0.038(8) 0.054(8) 0.149(14) 0.045(8) 0.048(8) 0.025(6) C9 0.038(7) 0.048(7) 0.111(11) 0.045(8) 0.031(7) 0.012(6) C10 0.047(7) 0.027(6) 0.078(9) 0.021(6) 0.024(7) 0.011(5) C11 0.016(5) 0.022(5) 0.076(9) 0.015(5) 0.009(5) 0.001(4) C12 0.013(5) 0.014(4) 0.027(6) 0.002(4) -0.002(4) 0.004(4) C13 0.019(5) 0.022(5) 0.023(6) 0.000(4) -0.005(4) -0.001(4) C14 0.020(5) 0.017(4) 0.008(5) 0.002(4) 0.002(4) 0.001(4) C15 0.016(5) 0.015(5) 0.031(6) -0.006(4) -0.006(4) 0.002(4) C16 0.018(5) 0.011(4) 0.018(5) 0.005(4) 0.002(4) -0.006(4) C17 0.028(4) 0.013(3) 0.020(4) 0.001(2) 0.009(3) -0.003(3) C18 0.034(4) 0.017(3) 0.021(4) 0.005(3) 0.009(3) 0.004(3) C19 0.039(4) 0.019(3) 0.023(3) 0.006(3) 0.014(3) 0.005(3) C20 0.062(5) 0.027(4) 0.030(4) -0.003(3) 0.020(4) 0.012(4) C21 0.079(5) 0.025(3) 0.041(4) -0.004(3) 0.031(4) 0.025(4) C22 0.078(5) 0.027(4) 0.044(5) 0.004(3) 0.027(4) 0.023(4) C23 0.056(5) 0.022(3) 0.033(4) 0.010(3) 0.021(4) 0.015(4) C24 0.013(5) 0.015(4) 0.026(6) -0.001(4) 0.001(4) -0.007(4) C25 0.012(5) 0.024(5) 0.009(5) 0.004(4) 0.002(4) -0.007(4) C26 0.020(5) 0.010(4) 0.014(5) -0.001(4) 0.001(4) -0.004(4) C27 0.014(4) 0.011(4) 0.007(5) -0.001(3) -0.001(4) -0.003(4) C28 0.022(5) 0.011(4) 0.020(5) 0.005(4) -0.012(4) 0.003(4) C29 0.039(6) 0.023(5) 0.023(6) -0.008(4) -0.009(5) 0.006(5) C30 0.024(5) 0.014(5) 0.022(5) -0.005(4) -0.016(4) 0.001(4) C31 0.081(8) 0.049(7) 0.039(7) -0.035(5) -0.040(6) 0.028(7) C32 0.095(10) 0.078(10) 0.079(10) -0.047(8) -0.056(8) 0.063(9) C33 0.106(10) 0.031(6) 0.076(9) -0.032(7) -0.061(8) 0.032(8) C34 0.075(9) 0.041(6) 0.032(7) -0.010(5) -0.028(6) 0.028(6) C35 0.034(6) 0.039(6) 0.021(6) -0.013(4) -0.013(5) 0.010(5) C36 0.024(5) 0.008(4) 0.022(5) 0.000(4) -0.007(4) 0.005(4) C37 0.024(5) 0.020(5) 0.008(5) -0.003(4) 0.000(4) -0.003(4) C38 0.021(5) 0.024(5) 0.012(5) -0.001(4) 0.006(4) -0.001(4) C39 0.018(4) 0.026(5) 0.016(5) -0.003(5) 0.000(4) -0.008(5) C40 0.019(5) 0.033(5) 0.024(6) -0.013(4) 0.004(4) -0.020(4) C41 0.024(5) 0.037(5) 0.031(6) -0.015(5) 0.017(5) 0.005(5) C42 0.016(5) 0.031(5) 0.021(5) -0.011(4) 0.008(4) -0.018(4) C43 0.034(6) 0.067(8) 0.023(6) -0.016(6) 0.013(5) -0.013(6) C44 0.044(7) 0.054(7) 0.042(7) -0.029(6) 0.017(6) -0.015(6) C45 0.037(7) 0.055(7) 0.039(7) -0.020(6) 0.009(6) -0.012(6) C46 0.040(7) 0.050(7) 0.041(7) -0.007(6) 0.006(6) -0.020(6) C47 0.031(6) 0.034(5) 0.026(6) -0.006(5) 0.006(5) -0.005(5) C48 0.021(5) 0.023(5) 0.015(5) 0.008(5) 0.006(4) 0.001(5) C49 0.031(6) 0.033(6) 0.033(7) -0.011(5) 0.006(5) -0.018(5) N1A 0.049(9) 0.034(6) 0.132(15) 0.024(9) 0.050(9) -0.002(7) C50A 0.047(11) 0.050(11) 0.143(16) 0.023(10) 0.041(11) -0.003(9) C51A 0.054(12) 0.036(9) 0.129(15) 0.009(9) 0.063(11) 0.000(9) N1B 0.051(9) 0.036(6) 0.129(15) 0.020(8) 0.051(9) -0.002(6) C50B 0.057(10) 0.046(8) 0.140(16) 0.035(9) 0.045(11) 0.004(7) C51B 0.046(13) 0.029(8) 0.116(16) 0.012(8) 0.054(12) 0.014(9) C52 0.023(5) 0.021(5) 0.030(6) 0.003(5) 0.002(5) 0.001(4) C53 0.050(7) 0.025(5) 0.034(6) -0.005(5) -0.014(5) 0.000(5) C54 0.093(10) 0.036(7) 0.069(9) -0.006(6) -0.072(8) 0.005(7) C55 0.008(3) 0.018(4) 0.017(4) 0.006(4) 0.000(2) -0.005(3) C56 0.010(3) 0.025(4) 0.011(3) 0.000(3) 0.001(2) 0.001(3) C57 0.010(3) 0.019(3) 0.013(3) 0.001(3) -0.001(2) -0.001(3) C58 0.011(3) 0.022(4) 0.016(4) 0.001(3) -0.001(2) 0.000(3) C59 0.011(4) 0.018(4) 0.024(4) 0.008(4) -0.006(3) -0.005(3) C60 0.016(4) 0.032(4) 0.017(4) -0.006(3) -0.003(3) 0.009(3) C61 0.026(6) 0.102(10) 0.029(7) -0.018(6) -0.010(5) 0.030(6) C62 0.037(7) 0.153(13) 0.031(7) -0.046(8) -0.013(6) 0.026(8) C63 0.028(7) 0.189(16) 0.030(7) -0.028(8) 0.000(6) 0.039(8) C64 0.032(6) 0.096(9) 0.026(6) -0.022(6) -0.004(5) 0.033(6) C65 0.022(5) 0.052(6) 0.024(6) 0.002(5) 0.004(4) 0.021(5) C66 0.008(5) 0.036(5) 0.025(6) 0.009(4) -0.006(4) 0.003(4) C67 0.012(5) 0.015(5) 0.068(8) -0.008(5) 0.009(5) 0.003(4) C68 0.027(6) 0.013(4) 0.039(6) -0.015(4) -0.011(5) -0.003(4) C69 0.016(5) 0.022(5) 0.031(6) -0.003(4) 0.004(4) -0.004(4) C70 0.020(5) 0.018(5) 0.037(6) 0.000(4) 0.004(5) 0.005(4) C71 0.032(6) 0.012(5) 0.047(7) -0.017(4) -0.014(5) 0.006(4) C72 0.036(6) 0.022(5) 0.063(8) -0.017(5) -0.012(6) 0.005(5) C73 0.032(6) 0.038(6) 0.080(9) -0.024(6) -0.015(6) 0.000(5) C74 0.063(8) 0.042(7) 0.085(10) -0.038(6) -0.049(7) 0.017(6) C75 0.056(8) 0.057(8) 0.100(11) -0.035(8) -0.047(7) 0.027(7) C76 0.056(8) 0.066(8) 0.100(11) -0.068(8) -0.061(8) 0.046(7) C77 0.028(6) 0.051(7) 0.129(13) -0.052(8) -0.047(8) 0.018(6) C78 0.012(5) 0.020(5) 0.033(6) 0.000(5) -0.003(4) 0.000(4) C79 0.046(6) 0.046(5) 0.025(4) -0.008(4) 0.011(5) 0.006(5) C80 0.083(8) 0.089(7) 0.055(7) -0.036(6) 0.029(6) 0.018(6) C81 0.136(10) 0.129(9) 0.027(6) 0.008(5) 0.011(7) 0.073(8) C82 0.017(5) 0.025(5) 0.043(7) -0.008(5) 0.004(5) -0.002(5) C83 0.030(7) 0.102(10) 0.047(8) 0.038(7) -0.004(6) 0.015(7) C84 0.051(9) 0.084(10) 0.148(15) 0.077(10) 0.010(9) 0.018(8) N2 0.037(5) 0.019(4) 0.032(5) 0.008(4) -0.014(4) 0.011(4) N3 0.068(5) 0.072(5) 0.026(4) -0.012(3) 0.020(4) 0.021(4) N4 0.015(4) 0.030(5) 0.057(6) 0.020(4) -0.002(4) 0.007(4) O1 0.012(3) 0.012(3) 0.006(3) 0.000(2) -0.002(2) -0.001(2) O2 0.011(3) 0.018(3) 0.037(4) 0.004(2) 0.002(3) 0.006(2) O3 0.012(3) 0.023(3) 0.021(3) -0.002(2) -0.001(2) 0.006(2) O4 0.017(3) 0.016(3) 0.025(4) 0.002(3) 0.005(3) -0.001(3) O5 0.017(3) 0.016(3) 0.047(4) 0.004(3) 0.005(3) 0.004(3) O6 0.024(4) 0.029(3) 0.012(3) -0.002(3) 0.006(3) 0.008(3) O7 0.031(3) 0.022(3) 0.011(3) 0.008(3) 0.003(2) 0.009(3) O8 0.028(4) 0.016(3) 0.019(4) 0.001(3) 0.006(3) 0.001(3) O9 0.032(4) 0.022(3) 0.014(4) 0.001(3) 0.005(3) -0.008(3) O10 0.025(3) 0.019(3) 0.013(3) -0.006(3) -0.009(3) 0.009(3) O11 0.013(3) 0.019(3) 0.024(4) -0.008(3) -0.004(3) 0.003(3) O12 0.026(4) 0.023(3) 0.025(4) -0.013(3) -0.016(3) 0.012(3) O13 0.024(3) 0.018(3) 0.010(3) 0.001(3) -0.007(3) -0.001(3) O14 0.013(3) 0.040(4) 0.011(3) -0.002(3) -0.003(3) -0.007(3) O15 0.018(3) 0.019(3) 0.010(3) 0.000(2) -0.001(3) -0.002(3) O16 0.023(4) 0.048(4) 0.032(4) -0.015(3) 0.009(3) -0.021(3) O17 0.017(3) 0.026(3) 0.018(4) -0.004(3) 0.004(3) -0.012(3) O18 0.026(4) 0.024(3) 0.040(4) 0.003(3) 0.007(3) -0.004(3) O19 0.026(4) 0.016(3) 0.032(4) 0.007(3) -0.009(3) 0.007(3) O20 0.013(3) 0.026(3) 0.014(3) -0.005(3) 0.002(3) 0.005(3) O21 0.013(3) 0.025(3) 0.016(3) -0.005(3) -0.004(3) 0.005(3) O22 0.028(3) 0.012(3) 0.010(3) -0.002(3) 0.000(3) 0.001(3) O23 0.013(3) 0.043(4) 0.016(3) 0.002(3) -0.008(3) 0.007(3) O24 0.006(3) 0.009(3) 0.014(3) 0.002(2) 0.001(2) 0.005(2) O25 0.028(4) 0.030(4) 0.049(5) -0.016(3) -0.021(3) 0.014(3) O26 0.030(4) 0.015(3) 0.029(4) -0.005(3) -0.006(3) 0.003(3) O27 0.021(3) 0.025(3) 0.029(4) 0.000(3) -0.004(3) 0.010(3) O28 0.008(3) 0.021(3) 0.024(4) -0.006(3) 0.000(3) 0.001(3) O29 0.031(3) 0.032(3) 0.018(3) 0.001(3) 0.001(3) 0.014(3) O30 0.019(3) 0.028(4) 0.030(4) 0.010(3) 0.006(3) 0.002(3) Zn1 0.0110(5) 0.0106(5) 0.0160(5) -0.0013(5) 0.0006(4) 0.0002(5) Zn2 0.0157(6) 0.0110(5) 0.0122(6) 0.0002(4) -0.0026(4) 0.0003(4) Zn3 0.0111(5) 0.0115(5) 0.0129(5) -0.0013(4) -0.0029(4) 0.0002(4) Zn4 0.0101(5) 0.0145(5) 0.0128(6) -0.0018(4) -0.0010(4) 0.0010(4) Zn5 0.0122(5) 0.0176(5) 0.0150(5) 0.0010(5) -0.0011(4) 0.0022(5) Zn6 0.0108(5) 0.0134(5) 0.0113(6) 0.0004(4) -0.0004(4) -0.0010(4) Zn7 0.0143(5) 0.0143(5) 0.0112(6) -0.0004(4) -0.0015(4) -0.0010(5) Zn8 0.0126(5) 0.0129(5) 0.0136(5) 0.0015(4) -0.0009(4) 0.0007(4) C85 0.125(17) 0.078(12) 0.16(2) -0.008(13) 0.035(15) 0.004(11) C86 0.081(12) 0.114(13) 0.166(18) 0.057(13) 0.056(12) 0.019(10) C87 0.26(2) 0.144(17) 0.171(19) 0.067(14) -0.151(18) -0.150(18) N5 0.138(13) 0.082(9) 0.078(10) 0.007(8) -0.013(10) -0.009(9) O31 0.179(13) 0.108(9) 0.137(11) 0.032(8) -0.055(9) -0.068(9) C88 0.092(8) 0.075(7) 0.129(9) -0.003(6) -0.005(7) 0.004(5) C89 0.154(11) 0.088(9) 0.180(13) -0.024(8) 0.069(9) -0.051(9) C90 0.078(8) 0.080(8) 0.125(11) -0.024(8) -0.026(7) 0.006(6) N6 0.085(7) 0.066(6) 0.128(8) -0.003(6) 0.013(6) -0.004(5) O32 0.138(9) 0.109(7) 0.165(10) -0.023(7) -0.019(8) 0.048(6) N7 0.098(9) 0.053(6) 0.090(10) -0.017(7) -0.015(8) 0.027(6) C91 0.098(9) 0.053(6) 0.090(10) -0.017(7) -0.015(8) 0.027(6) C92 0.098(9) 0.053(6) 0.090(10) -0.017(7) -0.015(8) 0.027(6) C93 0.098(9) 0.053(6) 0.090(10) -0.017(7) -0.015(8) 0.027(6) O33 0.098(9) 0.053(6) 0.090(10) -0.017(7) -0.015(8) 0.027(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C1 O3 1.262(9) . ? C1 O2 1.289(9) . ? C1 C2 1.451(11) . ? C2 C3 1.391(10) . ? C2 C6 1.428(11) . ? C3 C4 1.416(11) . ? C3 H3 0.9300 . ? C4 C5 1.410(12) . ? C4 C12 1.481(11) . ? C5 C7 1.415(13) . ? C5 C6 1.475(11) . ? C6 C11 1.382(12) . ? C7 C8 1.419(14) . ? C7 H7 0.9300 . ? C8 C9 1.429(13) . ? C8 H8 0.9300 . ? C9 C10 1.352(13) . ? C9 H9 0.9300 . ? C10 C11 1.391(12) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 O5 1.252(9) . ? C12 O4 1.269(9) . ? C13 O6 1.233(10) . ? C13 O7 1.310(9) . ? C13 C14 1.488(11) . ? C14 C18 1.385(11) . ? C14 C15 1.391(11) . ? C15 C16 1.401(11) . ? C15 H15 0.9300 . ? C16 C17 1.429(10) . ? C16 C24 1.456(11) . ? C17 C19 1.377(11) . ? C17 C18 1.498(11) . ? C18 C23 1.422(10) . ? C19 C20 1.393(11) . ? C19 H19 0.9300 . ? C20 C21 1.376(12) . ? C20 H20 0.9300 . ? C21 C22 1.351(13) . ? C21 H21 0.9300 . ? C22 C23 1.386(12) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 O9 1.243(9) . ? C24 O8 1.303(10) . ? C25 O10 1.246(9) . ? C25 O11 1.288(9) . ? C25 C26 1.491(11) . ? C26 C30 1.397(11) . ? C26 C27 1.404(10) . ? C27 C28 1.391(10) . ? C27 H27 0.9300 . ? C28 C29 1.408(11) . ? C28 C36 1.468(11) . ? C29 C31 1.396(12) . ? C29 C30 1.470(11) . ? C30 C35 1.371(11) . ? C31 C32 1.389(13) . ? C31 H31 0.9300 . ? C32 C33 1.373(13) . ? C32 H32 0.9300 . ? C33 C34 1.340(13) . ? C33 H33 0.9300 . ? C34 C35 1.427(12) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 O12 1.265(9) . ? C36 O13 1.269(9) . ? C37 O15 1.252(8) . ? C37 O14 1.267(9) . ? C37 C38 1.493(11) . ? C38 C39 1.370(10) . ? C38 C42 1.410(11) . ? C39 C40 1.372(11) . ? C39 H39 0.9300 . ? C40 C41 1.399(11) . ? C40 C48 1.460(11) . ? C41 C43 1.380(12) . ? C41 C42 1.488(11) . ? C42 C47 1.383(11) . ? C43 C44 1.395(12) . ? C43 H43 0.9300 . ? C44 C45 1.407(13) . ? C44 H44 0.9300 . ? C45 C46 1.404(13) . ? C45 H45 0.9300 . ? C46 C47 1.363(12) . ? C46 H46 0.9300 . ? C47 H47 0.9300 . ? C48 O17 1.271(9) . ? C48 O16 1.275(9) . ? C49 O18 1.234(10) . ? C49 N1B 1.27(2) . ? C49 N1A 1.35(3) . ? C49 H49 0.9300 . ? N1A C51A 1.46(2) . ? N1A C50A 1.45(2) . ? C50A H50A 0.9600 . ? C50A H50B 0.9600 . ? C50A H50C 0.9600 . ? C51A H51A 0.9600 . ? C51A H51B 0.9600 . ? C51A H51C 0.9600 . ? N1B C51B 1.462(18) . ? N1B C50B 1.46(3) . ? C50B H50D 0.9600 . ? C50B H50E 0.9600 . ? C50B H50F 0.9600 . ? C51B H51D 0.9600 . ? C51B H51E 0.9600 . ? C51B H51F 0.9600 . ? C52 O19 1.230(10) . ? C52 N2 1.302(10) . ? C52 H52 0.9300 . ? C53 N2 1.464(10) . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 N2 1.469(11) . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 O21 1.261(8) . ? C55 O20 1.266(9) . ? C55 C56 1.481(10) . ? C56 C57 1.399(10) . ? C56 C60 1.406(10) . ? C57 C58 1.384(10) . ? C57 H57 0.9300 . ? C58 C59 1.462(11) . ? C58 C66 1.465(11) . ? C59 O22 1.236(9) . ? C59 O23 1.287(9) . ? C60 C61 1.385(12) . ? C60 C66 1.477(11) . ? C61 C62 1.412(13) . ? C61 H61 0.9300 . ? C62 C63 1.417(13) . ? C62 H62 0.9300 . ? C63 C64 1.351(13) . ? C63 H63 0.9300 . ? C64 C65 1.376(12) . ? C64 H64 0.9300 . ? C65 C66 1.408(11) . ? C65 H65 0.9300 . ? C67 O26 1.259(11) . ? C67 O25 1.283(10) . ? C67 C68 1.530(12) . ? C68 C69 1.345(11) . ? C68 C72 1.413(12) . ? C69 C70 1.403(11) . ? C69 H69 0.9300 . ? C70 C71 1.382(12) . ? C70 C78 1.458(11) . ? C71 C73 1.390(12) . ? C71 C72 1.486(12) . ? C72 C77 1.403(13) . ? C73 C74 1.404(13) . ? C73 H73 0.9300 . ? C74 C75 1.400(13) . ? C74 H74 0.9300 . ? C75 C76 1.390(13) . ? C75 H75 0.9300 . ? C76 C77 1.371(13) . ? C76 H76 0.9300 . ? C77 H77 0.9300 . ? C78 O27 1.263(9) . ? C78 O28 1.271(9) . ? C79 O29 1.252(10) . ? C79 N3 1.281(11) . ? C79 H79 0.9300 . ? C80 N3 1.461(12) . ? C80 H80A 0.9600 . ? C80 H80B 0.9600 . ? C80 H80C 0.9600 . ? C81 N3 1.477(13) . ? C81 H81A 0.9600 . ? C81 H81B 0.9600 . ? C81 H81C 0.9600 . ? C82 O30 1.247(10) . ? C82 N4 1.312(10) . ? C82 H82 0.9300 . ? C83 N4 1.408(12) . ? C83 H83A 0.9600 . ? C83 H83B 0.9600 . ? C83 H83C 0.9600 . ? C84 N4 1.452(12) . ? C84 H84A 0.9600 . ? C84 H84B 0.9600 . ? C84 H84C 0.9600 . ? O1 Zn1 1.908(5) . ? O1 Zn4 1.920(5) . ? O1 Zn3 1.930(5) . ? O1 Zn2 2.028(5) . ? O2 Zn1 1.952(5) . ? O3 Zn2 2.095(5) . ? O4 Zn1 1.956(5) 2_747 ? O5 Zn3 1.976(5) 2_747 ? O6 Zn2 2.163(5) . ? O7 Zn3 1.954(5) . ? O8 Zn6 1.951(5) 2_647 ? O9 Zn7 2.007(5) 2_647 ? O10 Zn2 2.072(5) . ? O11 Zn4 1.951(5) . ? O12 Zn8 1.967(5) 2_646 ? O13 Zn7 1.949(5) 2_646 ? O14 Zn4 1.977(5) . ? O15 Zn1 1.979(5) . ? O16 Zn8 1.949(6) 1_655 ? O17 Zn6 1.964(5) 1_655 ? O18 Zn2 2.133(6) . ? O19 Zn2 2.104(5) . ? O20 Zn4 1.945(5) . ? O21 Zn3 1.978(5) . ? O22 Zn5 2.073(5) . ? O23 Zn6 1.978(5) . ? O24 Zn8 1.919(5) . ? O24 Zn6 1.923(5) . ? O24 Zn7 1.931(5) . ? O24 Zn5 2.022(5) . ? O25 Zn8 1.921(6) . ? O26 Zn5 2.217(5) . ? O27 Zn5 2.098(5) 2_646 ? O28 Zn7 1.945(5) 2_646 ? O29 Zn5 2.108(5) . ? O30 Zn5 2.086(6) . ? Zn1 O4 1.956(5) 2_757 ? Zn1 Zn3 3.1278(12) . ? Zn1 Zn4 3.1446(12) . ? Zn3 O5 1.976(5) 2_757 ? Zn3 Zn4 3.1305(13) . ? Zn5 O27 2.098(5) 2_656 ? Zn5 Zn7 3.1331(13) . ? Zn6 O8 1.951(5) 2_657 ? Zn6 O17 1.964(5) 1_455 ? Zn6 Zn8 3.1377(13) . ? Zn6 Zn7 3.1504(13) . ? Zn7 O28 1.945(5) 2_656 ? Zn7 O13 1.949(5) 2_656 ? Zn7 O9 2.007(5) 2_657 ? Zn7 Zn8 3.1433(13) . ? Zn8 O16 1.949(6) 1_455 ? Zn8 O12 1.967(5) 2_656 ? C85 O31 1.281(19) . ? C85 N5 1.364(19) . ? C85 H85 0.9300 . ? C86 N5 1.480(17) . ? C86 H86A 0.9600 . ? C86 H86B 0.9600 . ? C86 H86C 0.9600 . ? C87 N5 1.396(17) . ? C87 H87A 0.9600 . ? C87 H87B 0.9600 . ? C87 H87C 0.9600 . ? C88 O32 1.201(15) . ? C88 N6 1.298(17) . ? C88 H88 0.9300 . ? C89 N6 1.483(17) . ? C89 H89A 0.9600 . ? C89 H89B 0.9600 . ? C89 H89C 0.9600 . ? C90 N6 1.418(15) . ? C90 H90A 0.9600 . ? C90 H90B 0.9600 . ? C90 H90C 0.9600 . ? N7 C91 1.429(5) . ? N7 C93 1.430(5) . ? N7 C92 1.432(5) . ? C91 H91A 0.9600 . ? C91 H91B 0.9600 . ? C91 H91C 0.9600 . ? C92 H92A 0.9600 . ? C92 H92B 0.9600 . ? C92 H92C 0.9600 . ? C93 O33 1.183(9) . ? C93 H93 0.9300 . ? 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 O3 C1 O2 122.6(7) . . ? O3 C1 C2 117.9(7) . . ? O2 C1 C2 119.4(8) . . ? C3 C2 C6 108.7(7) . . ? C3 C2 C1 122.6(8) . . ? C6 C2 C1 128.7(7) . . ? C2 C3 C4 109.9(8) . . ? C2 C3 H3 125.0 . . ? C4 C3 H3 125.0 . . ? C5 C4 C3 107.7(7) . . ? C5 C4 C12 128.9(8) . . ? C3 C4 C12 123.4(8) . . ? C4 C5 C7 124.3(8) . . ? C4 C5 C6 107.7(8) . . ? C7 C5 C6 127.9(9) . . ? C11 C6 C2 126.5(8) . . ? C11 C6 C5 127.5(8) . . ? C2 C6 C5 106.0(7) . . ? C5 C7 C8 128.5(9) . . ? C5 C7 H7 115.7 . . ? C8 C7 H7 115.7 . . ? C7 C8 C9 126.9(10) . . ? C7 C8 H8 116.6 . . ? C9 C8 H8 116.6 . . ? C10 C9 C8 129.5(10) . . ? C10 C9 H9 115.2 . . ? C8 C9 H9 115.2 . . ? C9 C10 C11 131.2(10) . . ? C9 C10 H10 114.4 . . ? C11 C10 H10 114.4 . . ? C6 C11 C10 128.4(9) . . ? C6 C11 H11 115.8 . . ? C10 C11 H11 115.8 . . ? O5 C12 O4 124.9(8) . . ? O5 C12 C4 120.0(8) . . ? O4 C12 C4 115.1(7) . . ? O6 C13 O7 124.2(8) . . ? O6 C13 C14 119.9(8) . . ? O7 C13 C14 115.9(8) . . ? C18 C14 C15 108.3(7) . . ? C18 C14 C13 130.2(8) . . ? C15 C14 C13 121.2(7) . . ? C14 C15 C16 110.7(7) . . ? C14 C15 H15 124.7 . . ? C16 C15 H15 124.7 . . ? C15 C16 C17 108.1(7) . . ? C15 C16 C24 123.1(8) . . ? C17 C16 C24 128.5(8) . . ? C19 C17 C16 127.5(8) . . ? C19 C17 C18 127.7(7) . . ? C16 C17 C18 104.8(7) . . ? C14 C18 C23 126.5(9) . . ? C14 C18 C17 108.2(7) . . ? C23 C18 C17 125.3(8) . . ? C17 C19 C20 128.7(8) . . ? C17 C19 H19 115.7 . . ? C20 C19 H19 115.7 . . ? C21 C20 C19 129.4(9) . . ? C21 C20 H20 115.3 . . ? C19 C20 H20 115.3 . . ? C22 C21 C20 130.5(9) . . ? C22 C21 H21 114.7 . . ? C20 C21 H21 114.7 . . ? C21 C22 C23 128.5(9) . . ? C21 C22 H22 115.7 . . ? C23 C22 H22 115.7 . . ? C22 C23 C18 129.8(9) . . ? C22 C23 H23 115.1 . . ? C18 C23 H23 115.1 . . ? O9 C24 O8 123.8(7) . . ? O9 C24 C16 121.0(8) . . ? O8 C24 C16 115.1(8) . . ? O10 C25 O11 126.0(7) . . ? O10 C25 C26 119.1(7) . . ? O11 C25 C26 114.9(7) . . ? C30 C26 C27 108.1(7) . . ? C30 C26 C25 130.3(7) . . ? C27 C26 C25 121.5(7) . . ? C28 C27 C26 110.1(7) . . ? C28 C27 H27 125.0 . . ? C26 C27 H27 125.0 . . ? C27 C28 C29 107.9(7) . . ? C27 C28 C36 121.2(7) . . ? C29 C28 C36 130.9(7) . . ? C31 C29 C28 125.6(8) . . ? C31 C29 C30 127.3(8) . . ? C28 C29 C30 107.0(7) . . ? C35 C30 C26 125.9(8) . . ? C35 C30 C29 127.1(8) . . ? C26 C30 C29 107.0(7) . . ? C32 C31 C29 128.2(9) . . ? C32 C31 H31 115.9 . . ? C29 C31 H31 115.9 . . ? C33 C32 C31 129.7(10) . . ? C33 C32 H32 115.1 . . ? C31 C32 H32 115.1 . . ? C34 C33 C32 129.9(11) . . ? C34 C33 H33 115.0 . . ? C32 C33 H33 115.0 . . ? C33 C34 C35 128.5(9) . . ? C33 C34 H34 115.8 . . ? C35 C34 H34 115.8 . . ? C30 C35 C34 129.1(8) . . ? C30 C35 H35 115.4 . . ? C34 C35 H35 115.4 . . ? O12 C36 O13 124.9(8) . . ? O12 C36 C28 118.4(7) . . ? O13 C36 C28 116.8(7) . . ? O15 C37 O14 123.8(7) . . ? O15 C37 C38 116.0(7) . . ? O14 C37 C38 120.1(7) . . ? C39 C38 C42 107.2(7) . . ? C39 C38 C37 122.9(7) . . ? C42 C38 C37 129.4(7) . . ? C38 C39 C40 112.2(7) . . ? C38 C39 H39 123.9 . . ? C40 C39 H39 123.9 . . ? C39 C40 C41 107.9(7) . . ? C39 C40 C48 124.4(7) . . ? C41 C40 C48 127.6(8) . . ? C43 C41 C40 128.8(9) . . ? C43 C41 C42 124.9(9) . . ? C40 C41 C42 106.1(7) . . ? C47 C42 C38 126.9(8) . . ? C47 C42 C41 126.6(8) . . ? C38 C42 C41 106.4(7) . . ? C41 C43 C44 133.0(10) . . ? C41 C43 H43 113.5 . . ? C44 C43 H43 113.5 . . ? C43 C44 C45 127.0(10) . . ? C43 C44 H44 116.5 . . ? C45 C44 H44 116.5 . . ? C46 C45 C44 127.5(10) . . ? C46 C45 H45 116.2 . . ? C44 C45 H45 116.2 . . ? C47 C46 C45 129.9(9) . . ? C47 C46 H46 115.1 . . ? C45 C46 H46 115.1 . . ? C46 C47 C42 130.9(9) . . ? C46 C47 H47 114.6 . . ? C42 C47 H47 114.6 . . ? O17 C48 O16 124.3(7) . . ? O17 C48 C40 117.7(7) . . ? O16 C48 C40 118.0(8) . . ? O18 C49 N1B 135.5(14) . . ? O18 C49 N1A 120.5(14) . . ? N1B C49 N1A 23(3) . . ? O18 C49 H49 119.8 . . ? N1B C49 H49 102.0 . . ? N1A C49 H49 119.8 . . ? C49 N1A C51A 124(2) . . ? C49 N1A C50A 118(2) . . ? C51A N1A C50A 118(2) . . ? N1A C50A H50A 109.5 . . ? N1A C50A H50B 109.5 . . ? H50A C50A H50B 109.5 . . ? N1A C50A H50C 109.5 . . ? H50A C50A H50C 109.5 . . ? H50B C50A H50C 109.5 . . ? N1A C51A H51A 109.5 . . ? N1A C51A H51B 109.5 . . ? H51A C51A H51B 109.5 . . ? N1A C51A H51C 109.5 . . ? H51A C51A H51C 109.5 . . ? H51B C51A H51C 109.5 . . ? C49 N1B C51B 124.0(19) . . ? C49 N1B C50B 116.6(18) . . ? C51B N1B C50B 117.1(19) . . ? N1B C50B H50D 109.5 . . ? N1B C50B H50E 109.5 . . ? H50D C50B H50E 109.5 . . ? N1B C50B H50F 109.5 . . ? H50D C50B H50F 109.5 . . ? H50E C50B H50F 109.5 . . ? N1B C51B H51D 109.5 . . ? N1B C51B H51E 109.5 . . ? H51D C51B H51E 109.5 . . ? N1B C51B H51F 109.5 . . ? H51D C51B H51F 109.5 . . ? H51E C51B H51F 109.5 . . ? O19 C52 N2 124.8(8) . . ? O19 C52 H52 117.6 . . ? N2 C52 H52 117.6 . . ? N2 C53 H53A 109.5 . . ? N2 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? N2 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N2 C54 H54A 109.5 . . ? N2 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? N2 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? O21 C55 O20 125.4(7) . . ? O21 C55 C56 119.4(7) . . ? O20 C55 C56 115.1(7) . . ? C57 C56 C60 108.5(7) . . ? C57 C56 C55 123.2(7) . . ? C60 C56 C55 128.3(7) . . ? C58 C57 C56 111.1(7) . . ? C58 C57 H57 124.4 . . ? C56 C57 H57 124.4 . . ? C57 C58 C59 124.0(7) . . ? C57 C58 C66 107.1(7) . . ? C59 C58 C66 128.8(7) . . ? O22 C59 O23 125.3(7) . . ? O22 C59 C58 116.5(7) . . ? O23 C59 C58 118.2(8) . . ? C61 C60 C56 126.9(8) . . ? C61 C60 C66 125.8(8) . . ? C56 C60 C66 107.3(7) . . ? C60 C61 C62 130.3(9) . . ? C60 C61 H61 114.9 . . ? C62 C61 H61 114.9 . . ? C63 C62 C61 128.5(10) . . ? C63 C62 H62 115.8 . . ? C61 C62 H62 115.8 . . ? C64 C63 C62 126.7(10) . . ? C64 C63 H63 116.7 . . ? C62 C63 H63 116.7 . . ? C63 C64 C65 132.9(10) . . ? C63 C64 H64 113.5 . . ? C65 C64 H64 113.5 . . ? C64 C65 C66 127.4(9) . . ? C64 C65 H65 116.3 . . ? C66 C65 H65 116.3 . . ? C65 C66 C58 126.1(7) . . ? C65 C66 C60 128.1(8) . . ? C58 C66 C60 105.8(7) . . ? O26 C67 O25 125.4(8) . . ? O26 C67 C68 117.2(8) . . ? O25 C67 C68 117.1(9) . . ? C69 C68 C72 108.4(8) . . ? C69 C68 C67 123.9(8) . . ? C72 C68 C67 127.4(8) . . ? C68 C69 C70 111.3(8) . . ? C68 C69 H69 124.3 . . ? C70 C69 H69 124.3 . . ? C71 C70 C69 107.7(8) . . ? C71 C70 C78 127.9(8) . . ? C69 C70 C78 124.4(8) . . ? C70 C71 C73 127.2(8) . . ? C70 C71 C72 106.7(8) . . ? C73 C71 C72 126.0(8) . . ? C77 C72 C68 127.3(9) . . ? C77 C72 C71 126.8(9) . . ? C68 C72 C71 105.8(8) . . ? C71 C73 C74 130.2(10) . . ? C71 C73 H73 114.9 . . ? C74 C73 H73 114.9 . . ? C75 C74 C73 128.6(10) . . ? C75 C74 H74 115.7 . . ? C73 C74 H74 115.7 . . ? C76 C75 C74 129.1(10) . . ? C76 C75 H75 115.4 . . ? C74 C75 H75 115.4 . . ? C77 C76 C75 128.3(10) . . ? C77 C76 H76 115.9 . . ? C75 C76 H76 115.9 . . ? C76 C77 C72 131.0(10) . . ? C76 C77 H77 114.5 . . ? C72 C77 H77 114.5 . . ? O27 C78 O28 124.2(8) . . ? O27 C78 C70 121.2(8) . . ? O28 C78 C70 114.6(8) . . ? O29 C79 N3 126.6(10) . . ? O29 C79 H79 116.7 . . ? N3 C79 H79 116.7 . . ? N3 C80 H80A 109.5 . . ? N3 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? N3 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? N3 C81 H81A 109.5 . . ? N3 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? N3 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? O30 C82 N4 125.5(9) . . ? O30 C82 H82 117.3 . . ? N4 C82 H82 117.3 . . ? N4 C83 H83A 109.5 . . ? N4 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? N4 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? N4 C84 H84A 109.5 . . ? N4 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? N4 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C52 N2 C53 120.8(7) . . ? C52 N2 C54 121.5(8) . . ? C53 N2 C54 117.5(7) . . ? C79 N3 C80 122.0(10) . . ? C79 N3 C81 118.9(9) . . ? C80 N3 C81 118.8(9) . . ? C82 N4 C83 120.7(8) . . ? C82 N4 C84 123.3(8) . . ? C83 N4 C84 115.9(8) . . ? Zn1 O1 Zn4 110.5(2) . . ? Zn1 O1 Zn3 109.2(2) . . ? Zn4 O1 Zn3 108.8(2) . . ? Zn1 O1 Zn2 112.6(2) . . ? Zn4 O1 Zn2 108.8(2) . . ? Zn3 O1 Zn2 106.9(2) . . ? C1 O2 Zn1 117.1(5) . . ? C1 O3 Zn2 133.3(5) . . ? C12 O4 Zn1 125.7(5) . 2_747 ? C12 O5 Zn3 132.3(5) . 2_747 ? C13 O6 Zn2 132.2(5) . . ? C13 O7 Zn3 113.8(5) . . ? C24 O8 Zn6 129.2(5) . 2_647 ? C24 O9 Zn7 130.6(5) . 2_647 ? C25 O10 Zn2 131.7(5) . . ? C25 O11 Zn4 116.5(5) . . ? C36 O12 Zn8 129.7(5) . 2_646 ? C36 O13 Zn7 130.6(5) . 2_646 ? C37 O14 Zn4 125.4(5) . . ? C37 O15 Zn1 122.0(5) . . ? C48 O16 Zn8 133.4(5) . 1_655 ? C48 O17 Zn6 128.3(5) . 1_655 ? C49 O18 Zn2 124.1(6) . . ? C52 O19 Zn2 119.7(6) . . ? C55 O20 Zn4 129.0(5) . . ? C55 O21 Zn3 131.2(5) . . ? C59 O22 Zn5 134.6(5) . . ? C59 O23 Zn6 117.2(5) . . ? Zn8 O24 Zn6 109.5(2) . . ? Zn8 O24 Zn7 109.4(2) . . ? Zn6 O24 Zn7 109.6(2) . . ? Zn8 O24 Zn5 108.7(2) . . ? Zn6 O24 Zn5 114.6(2) . . ? Zn7 O24 Zn5 104.8(2) . . ? C67 O25 Zn8 114.3(6) . . ? C67 O26 Zn5 129.6(6) . . ? C78 O27 Zn5 129.8(5) . 2_646 ? C78 O28 Zn7 116.8(5) . 2_646 ? C79 O29 Zn5 127.3(6) . . ? C82 O30 Zn5 118.9(6) . . ? O1 Zn1 O2 117.0(2) . . ? O1 Zn1 O4 115.0(2) . 2_757 ? O2 Zn1 O4 113.2(2) . 2_757 ? O1 Zn1 O15 108.0(2) . . ? O2 Zn1 O15 97.9(2) . . ? O4 Zn1 O15 103.1(2) 2_757 . ? O1 Zn1 Zn3 35.64(14) . . ? O2 Zn1 Zn3 140.71(17) . . ? O4 Zn1 Zn3 79.43(16) 2_757 . ? O15 Zn1 Zn3 115.99(15) . . ? O1 Zn1 Zn4 34.89(14) . . ? O2 Zn1 Zn4 116.99(16) . . ? O4 Zn1 Zn4 129.74(16) 2_757 . ? O15 Zn1 Zn4 73.64(15) . . ? Zn3 Zn1 Zn4 59.88(3) . . ? O1 Zn2 O10 95.5(2) . . ? O1 Zn2 O3 94.6(2) . . ? O10 Zn2 O3 90.4(2) . . ? O1 Zn2 O19 177.4(2) . . ? O10 Zn2 O19 86.6(2) . . ? O3 Zn2 O19 86.9(2) . . ? O1 Zn2 O18 87.5(2) . . ? O10 Zn2 O18 95.5(2) . . ? O3 Zn2 O18 173.5(2) . . ? O19 Zn2 O18 90.7(2) . . ? O1 Zn2 O6 92.8(2) . . ? O10 Zn2 O6 171.6(2) . . ? O3 Zn2 O6 87.6(2) . . ? O19 Zn2 O6 85.2(2) . . ? O18 Zn2 O6 86.1(2) . . ? O1 Zn3 O7 124.6(2) . . ? O1 Zn3 O5 107.8(2) . 2_757 ? O7 Zn3 O5 101.9(2) . 2_757 ? O1 Zn3 O21 111.0(2) . . ? O7 Zn3 O21 104.3(2) . . ? O5 Zn3 O21 105.4(2) 2_757 . ? O1 Zn3 Zn1 35.18(14) . . ? O7 Zn3 Zn1 128.99(16) . . ? O5 Zn3 Zn1 73.03(17) 2_757 . ? O21 Zn3 Zn1 126.26(16) . . ? O1 Zn3 Zn4 35.48(14) . . ? O7 Zn3 Zn4 139.75(17) . . ? O5 Zn3 Zn4 117.16(18) 2_757 . ? O21 Zn3 Zn4 75.59(15) . . ? Zn1 Zn3 Zn4 60.33(3) . . ? O1 Zn4 O20 113.8(2) . . ? O1 Zn4 O11 115.7(2) . . ? O20 Zn4 O11 109.4(2) . . ? O1 Zn4 O14 111.1(2) . . ? O20 Zn4 O14 111.1(2) . . ? O11 Zn4 O14 94.2(2) . . ? O1 Zn4 Zn3 35.69(14) . . ? O20 Zn4 Zn3 78.14(16) . . ? O11 Zn4 Zn3 131.11(17) . . ? O14 Zn4 Zn3 129.24(16) . . ? O1 Zn4 Zn1 34.64(15) . . ? O20 Zn4 Zn1 124.90(16) . . ? O11 Zn4 Zn1 124.71(16) . . ? O14 Zn4 Zn1 76.85(15) . . ? Zn3 Zn4 Zn1 59.79(3) . . ? O24 Zn5 O22 94.3(2) . . ? O24 Zn5 O30 177.2(2) . . ? O22 Zn5 O30 86.3(2) . . ? O24 Zn5 O27 94.0(2) . 2_656 ? O22 Zn5 O27 93.2(2) . 2_656 ? O30 Zn5 O27 88.6(2) . 2_656 ? O24 Zn5 O29 87.0(2) . . ? O22 Zn5 O29 176.8(2) . . ? O30 Zn5 O29 92.3(2) . . ? O27 Zn5 O29 89.6(2) 2_656 . ? O24 Zn5 O26 93.6(2) . . ? O22 Zn5 O26 91.0(2) . . ? O30 Zn5 O26 83.7(2) . . ? O27 Zn5 O26 171.1(2) 2_656 . ? O29 Zn5 O26 86.0(2) . . ? O24 Zn5 Zn7 36.58(14) . . ? O22 Zn5 Zn7 116.79(14) . . ? O30 Zn5 Zn7 144.97(16) . . ? O27 Zn5 Zn7 65.50(15) 2_656 . ? O29 Zn5 Zn7 65.80(16) . . ? O26 Zn5 Zn7 119.32(15) . . ? O24 Zn6 O8 112.5(2) . 2_657 ? O24 Zn6 O17 113.7(2) . 1_455 ? O8 Zn6 O17 103.1(2) 2_657 1_455 ? O24 Zn6 O23 116.3(2) . . ? O8 Zn6 O23 99.9(2) 2_657 . ? O17 Zn6 O23 109.8(2) 1_455 . ? O24 Zn6 Zn8 35.22(14) . . ? O8 Zn6 Zn8 122.49(17) 2_657 . ? O17 Zn6 Zn8 78.45(16) 1_455 . ? O23 Zn6 Zn8 134.39(17) . . ? O24 Zn6 Zn7 35.27(14) . . ? O8 Zn6 Zn7 77.31(16) 2_657 . ? O17 Zn6 Zn7 127.28(17) 1_455 . ? O23 Zn6 Zn7 122.17(17) . . ? Zn8 Zn6 Zn7 59.98(3) . . ? O24 Zn7 O28 120.1(2) . 2_656 ? O24 Zn7 O13 111.6(2) . 2_656 ? O28 Zn7 O13 110.2(2) 2_656 2_656 ? O24 Zn7 O9 111.2(2) . 2_657 ? O28 Zn7 O9 95.4(2) 2_656 2_657 ? O13 Zn7 O9 106.6(2) 2_656 2_657 ? O24 Zn7 Zn5 38.60(14) . . ? O28 Zn7 Zn5 82.35(16) 2_656 . ? O13 Zn7 Zn5 123.89(16) 2_656 . ? O9 Zn7 Zn5 127.08(16) 2_657 . ? O24 Zn7 Zn8 35.16(15) . . ? O28 Zn7 Zn8 136.89(16) 2_656 . ? O13 Zn7 Zn8 76.48(16) 2_656 . ? O9 Zn7 Zn8 124.37(18) 2_657 . ? Zn5 Zn7 Zn8 61.38(3) . . ? O24 Zn7 Zn6 35.09(14) . . ? O28 Zn7 Zn6 125.41(17) 2_656 . ? O13 Zn7 Zn6 124.02(16) 2_656 . ? O9 Zn7 Zn6 76.08(17) 2_657 . ? Zn5 Zn7 Zn6 63.79(3) . . ? Zn8 Zn7 Zn6 59.81(3) . . ? O24 Zn8 O25 124.5(2) . . ? O24 Zn8 O16 110.5(2) . 1_455 ? O25 Zn8 O16 104.4(3) . 1_455 ? O24 Zn8 O12 111.3(2) . 2_656 ? O25 Zn8 O12 100.8(3) . 2_656 ? O16 Zn8 O12 102.9(3) 1_455 2_656 ? O24 Zn8 Zn6 35.29(15) . . ? O25 Zn8 Zn6 140.04(19) . . ? O16 Zn8 Zn6 75.31(17) 1_455 . ? O12 Zn8 Zn6 118.42(17) 2_656 . ? O24 Zn8 Zn7 35.42(14) . . ? O25 Zn8 Zn7 128.8(2) . . ? O16 Zn8 Zn7 126.31(17) 1_455 . ? O12 Zn8 Zn7 76.44(15) 2_656 . ? Zn6 Zn8 Zn7 60.21(3) . . ? O31 C85 N5 127.3(19) . . ? O31 C85 H85 116.4 . . ? N5 C85 H85 116.4 . . ? N5 C86 H86A 109.5 . . ? N5 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? N5 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? N5 C87 H87A 109.5 . . ? N5 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? N5 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? C85 N5 C87 118.4(18) . . ? C85 N5 C86 123.9(16) . . ? C87 N5 C86 117.1(16) . . ? O32 C88 N6 120.9(18) . . ? O32 C88 H88 119.6 . . ? N6 C88 H88 119.6 . . ? N6 C89 H89A 109.5 . . ? N6 C89 H89B 109.5 . . ? H89A C89 H89B 109.5 . . ? N6 C89 H89C 109.5 . . ? H89A C89 H89C 109.5 . . ? H89B C89 H89C 109.5 . . ? N6 C90 H90A 109.5 . . ? N6 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? N6 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? C88 N6 C90 119.8(15) . . ? C88 N6 C89 113.0(14) . . ? C90 N6 C89 127.2(14) . . ? C91 N7 C93 120.9(7) . . ? C91 N7 C92 120.1(7) . . ? C93 N7 C92 118.5(7) . . ? N7 C91 H91A 109.5 . . ? N7 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? N7 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? N7 C92 H92A 109.5 . . ? N7 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? N7 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? O33 C93 N7 132.5(16) . . ? O33 C93 H93 113.7 . . ? N7 C93 H93 113.7 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.680 _refine_diff_density_min -0.527 _refine_diff_density_rms 0.156 #===END