# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Juan Carlos Mareque-Rivas' 'Simon Parsons' 'Emiliano Salvagni' _publ_contact_author_name 'Dr Juan Carlos Mareque-Rivas' _publ_contact_author_address ; Chemistry The University of Edinburgh King's Buildings West Mains Road Edinburgh EH9 3JJ UNITED KINGDOM ; _publ_contact_author_email JUAN.MAREQUE@ED.AC.UK _publ_requested_journal 'Chemical Communications' _publ_section_title ; Structures and reactivity of synthetic zinc(II) complexes resembling the active sites and reaction intermediates of aminopeptidases ; data_r71143b _database_code_depnum_ccdc_archive 'CCDC 223725' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C30 H52 N12 O6 Zn2)(ClO4)4(H2O)4' _chemical_formula_sum 'C30 H60 Cl4 N12 O26 Zn2' _chemical_formula_weight 1277.44 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' Cl Cl 0.1484 0.1585 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0776(10) _cell_length_b 10.2002(11) _cell_length_c 14.5845(16) _cell_angle_alpha 104.467(2) _cell_angle_beta 101.407(2) _cell_angle_gamma 98.007(2) _cell_volume 1256.2(2) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4981 _cell_measurement_theta_min 2 _cell_measurement_theta_max 29 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.689 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 660 _exptl_absorpt_coefficient_mu 1.265 _exptl_absorpt_correction_type Multiscan _exptl_absorpt_correction_T_min 0.815 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method Omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11411 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0477 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 28.88 _reflns_number_total 5900 _reflns_number_gt 4979 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; #029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.89 #95% complete at 0.8 A. #------------------------------------------------------------------------------ #INTENSITY STATISTICS FOR DATASET # 1 r71143b.hkl #Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) #Inf - 2.05 306 306 100.0 2.88 917.7 48.79 0.0164 0.0138 #2.05 - 1.60 335 335 100.0 2.85 417.5 36.44 0.0211 0.0203 #1.60 - 1.40 323 323 100.0 2.63 289.4 27.02 0.0273 0.0275 #1.40 - 1.25 385 385 100.0 2.43 213.7 20.28 0.0298 0.0354 #1.25 - 1.15 376 376 100.0 2.19 181.7 16.65 0.0322 0.0418 #1.15 - 1.05 544 544 100.0 2.06 127.8 13.30 0.0339 0.0545 #1.05 - 1.00 366 366 100.0 1.90 112.1 11.35 0.0393 0.0641 #1.00 - 0.95 440 443 99.3 1.80 95.8 10.01 0.0464 0.0738 #0.95 - 0.90 518 528 98.1 1.70 72.2 8.27 0.0524 0.0904 #0.90 - 0.85 646 663 97.4 1.59 56.8 7.11 0.0668 0.1129 #0.85 - 0.80 836 883 94.7 1.46 43.8 5.83 0.0859 0.1372 #0.80 - 0.75 775 1086 71.4 0.98 33.3 4.77 0.1255 0.1663 #0.75 - 0.74 50 370 13.5 0.14 21.2 4.02 0.0328 0.2091 #----------------------------------------------------------------------------- #0.85 - 0.74 1661 2339 71.0 1.03 38.2 5.28 0.0987 0.1502 #Inf - 0.74 5900 6608 89.3 1.73 161.9 14.13 0.0274 0.0436 #Merged [A], lowest resolution = 13.70 Angstroms, 123 outliers downweighted #------------------------------------------------------------------------------ #306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... O1W #H-atoms not placed on water molecules. #=============================================================================== #430_ALERT_2_B Short Inter D...A Contact O1W .. O71 = 2.78 Ang. #Proably H-bonded. #=============================================================================== #041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? #068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? #H-atoms were not placed on water molecules. #062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.80 #No action. #094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.39 #There are still some regions of relatively high electron density (1.3 e A-3) #near the disordered perchlorate. #125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? #No action #244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... Cl1 #244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... Cl1' #244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... Cl2 #Not unusual for perchlorate. #302_ALERT_4_C Anion/Solvent Disorder ......................... 34.00 Perc. #311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) ..... >O2W #430_ALERT_2_C Short Inter D...A Contact O1W .. O42 = 2.86 Ang. #430_ALERT_2_C Short Inter D...A Contact O2G .. O3W = 2.89 Ang. #720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 9 #790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 #Cl O #790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 5 #O #796_ALERT_4_C O-Atom in CIF Coordinate List out of Sequence .. O12 #=============================================================================== #Final shelx res file: #TITL r71143b in P-1 #CELL 0.71073 9.0776 10.2002 14.5845 104.467 101.407 98.007 #ZERR 1 0.0010 0.0011 0.0016 0.002 0.002 0.002 #LATT 1 #SFAC C H CL N O ZN #UNIT 30 60 4 12 26 2 #TEMP -123 #L.S. 6 #BOND $H #FMAP 2 #PLAN 10 #HTAB #ACTA #WGHT 0.070700 1.533900 #FVAR 0.55475 0.61332 #ZN1 6 0.189404 0.099068 0.211449 11.00000 0.02517 0.01600 = #0.01917 0.00459 0.00197 0.00161 #N1 4 0.145993 -0.074193 0.271843 11.00000 0.02837 0.01399 = #0.02186 0.00321 0.00475 0.00306 #N2 4 0.273164 0.196115 0.360512 11.00000 0.02497 0.01839 = #0.01990 0.00409 0.00152 0.00014 #N7 4 0.256574 0.419041 0.355091 11.00000 0.03767 0.01605 = #0.02661 0.00154 -0.00243 0.00123 #AFIX 93 #H7NA 2 0.216724 0.387315 0.291768 11.00000 -1.20000 #H7NB 2 0.270787 0.507943 0.384555 11.00000 -1.20000 #AFIX 0 #N13 4 -0.060272 -0.320711 0.276035 11.00000 0.03477 0.01958 = #0.02665 0.00707 -0.00045 -0.00049 #AFIX 13 #H13N 2 -0.135026 -0.329252 0.219982 11.00000 0.04762 #AFIX 0 #C1 1 0.279886 -0.042189 0.355577 11.00000 0.02657 0.02345 = #0.02961 0.01282 0.00508 0.00767 #AFIX 23 #H1A 2 0.371073 -0.063577 0.331724 11.00000 -1.20000 #H1B 2 0.260392 -0.100522 0.398596 11.00000 -1.20000 #AFIX 0 #C2 1 0.310907 0.107963 0.412805 11.00000 0.02125 0.02413 = #0.02380 0.00842 0.00293 0.00082 #C3 1 0.375473 0.150292 0.511085 11.00000 0.03259 0.03846 = #0.02434 0.01690 0.00293 0.00433 #AFIX 43 #H3A 2 0.399108 0.085644 0.545910 11.00000 -1.20000 #AFIX 0 #C4 1 0.405616 0.292402 0.558723 11.00000 0.03643 0.04089 = #0.01661 0.00418 0.00137 -0.00400 #AFIX 43 #H4A 2 0.454810 0.325716 0.626299 11.00000 -1.20000 #AFIX 0 #C5 1 0.364318 0.382850 0.508058 11.00000 0.03578 0.02606 = #0.02214 -0.00182 0.00337 -0.00394 #AFIX 43 #H5A 2 0.381425 0.478805 0.540385 11.00000 -1.20000 #AFIX 0 #C6 1 0.295710 0.331763 0.406775 11.00000 0.02373 0.02083 = #0.02170 0.00337 0.00301 -0.00035 #C11 1 0.000128 -0.067584 0.302553 11.00000 0.02565 0.01808 = #0.02870 0.00723 0.00464 0.00332 #AFIX 23 #H11A 2 -0.081824 -0.072178 0.245187 11.00000 -1.20000 #H11B 2 0.011705 0.022681 0.351258 11.00000 -1.20000 #AFIX 0 #C12 1 -0.049926 -0.182340 0.346398 11.00000 0.03050 0.02115 = #0.03205 0.00817 0.00893 0.00452 #AFIX 23 #H12A 2 0.024996 -0.172284 0.408325 11.00000 -1.20000 #H12B 2 -0.151058 -0.175314 0.360890 11.00000 -1.20000 #AFIX 0 #C13 1 -0.108214 -0.435268 0.317220 11.00000 0.04163 0.02015 = #0.04441 0.01359 0.01008 0.00037 #AFIX 33 #H13A 2 -0.114022 -0.524205 0.269984 11.00000 -1.50000 #H13B 2 -0.209037 -0.430157 0.330891 11.00000 -1.50000 #H13C 2 -0.033058 -0.426655 0.377825 11.00000 -1.50000 #AFIX 0 #C14 1 0.088477 -0.328636 0.247732 11.00000 0.04910 0.01765 = #0.02732 0.00509 0.01417 0.00704 #AFIX 23 #H14A 2 0.079378 -0.418964 0.199685 11.00000 -1.20000 #H14B 2 0.170067 -0.321268 0.306005 11.00000 -1.20000 #AFIX 0 #C15 1 0.131354 -0.213231 0.203837 11.00000 0.05057 0.01677 = #0.02553 0.00403 0.01535 0.00645 #AFIX 23 #H15A 2 0.229945 -0.220414 0.185573 11.00000 -1.20000 #H15B 2 0.052142 -0.224367 0.143560 11.00000 -1.20000 #AFIX 0 #O1W 5 -0.452636 -0.010351 0.187345 11.00000 0.04425 0.05121 = #0.03487 0.01241 0.00752 0.00251 #N3G 4 -0.302978 0.068545 0.047750 11.00000 0.02442 0.03322 = #0.01924 0.00457 0.00294 0.00258 #AFIX 43 #H3GA 2 -0.370807 0.033489 0.075169 11.00000 -1.20000 #AFIX 0 #O1G 5 -0.022666 0.112373 0.162641 11.00000 0.02680 0.02516 = #0.02925 0.01073 -0.00013 0.00464 #C1G 1 -0.054004 0.219140 0.142172 11.00000 0.03080 0.02065 = #0.02016 -0.00026 0.00132 0.00506 #O2G 5 0.036875 0.330810 0.161861 11.00000 0.04408 0.01941 = #0.04913 0.00483 -0.01496 -0.00180 #C2G 1 -0.220318 0.210045 0.090912 11.00000 0.03098 0.02622 = #0.02439 0.00109 0.00051 0.01036 #AFIX 23 #H2GC 2 -0.272570 0.258812 0.138631 11.00000 -1.20000 #H2GD 2 -0.222520 0.257301 0.039193 11.00000 -1.20000 #AFIX 0 #C3G 1 -0.276751 -0.008073 -0.032757 11.00000 0.02093 0.02535 = #0.01868 0.00493 -0.00306 0.00250 #O3G 5 -0.199019 0.040764 -0.081458 11.00000 0.03522 0.01933 = #0.02322 0.00329 0.00763 0.00113 #C4G 1 -0.341272 -0.161943 -0.063157 11.00000 0.03378 0.02569 = #0.02203 0.00567 0.00467 -0.00268 #AFIX 23 #H4GA 2 -0.272393 -0.208128 -0.026131 11.00000 -1.20000 #H4GB 2 -0.443077 -0.178819 -0.048615 11.00000 -1.20000 #AFIX 0 #N4G 4 -0.355552 -0.218691 -0.168363 11.00000 0.03129 0.02476 = #0.02518 0.00274 0.00419 -0.00597 #H4GC 2 -0.357877 -0.306603 -0.180862 11.00000 0.03781 #H4GD 2 -0.439282 -0.213939 -0.196256 11.00000 0.04241 #PART 1 #CL1 3 0.521453 0.395788 -0.154307 21.00000 0.05160 0.02770 = #0.02571 0.00784 -0.00070 0.00529 #O11 5 0.470803 0.515208 -0.109726 21.00000 0.10970 0.03742 = #0.07436 0.01596 0.03386 0.01783 #O21 5 0.623610 0.439156 -0.206843 21.00000 0.06301 0.05071 = #0.06014 0.02523 0.00666 -0.00208 #O31 5 0.594880 0.342566 -0.080063 21.00000 0.07213 0.08756 = #0.05615 0.04810 -0.02557 0.00630 #O41 5 0.390443 0.287975 -0.222045 21.00000 0.03782 0.05555 = #0.03764 0.01255 -0.00301 -0.00402 #O2W 5 0.180616 0.395160 -0.067920 21.00000 0.06610 0.06163 = #0.09046 0.01624 -0.02565 -0.02229 #PART 2 #CL1' 3 0.465466 0.363322 -0.143438 -21.00000 0.04676 0.04032 = #0.03278 0.01328 0.00156 0.00438 #O51 5 0.328260 0.384233 -0.113433 -21.00000 0.09405 #O61 5 0.541870 0.481004 -0.159954 -21.00000 0.10752 #O71 5 0.441273 0.259068 -0.230879 -21.00000 0.06637 #O81 5 0.557602 0.313467 -0.077882 -21.00000 0.07292 #O3W 5 0.061247 0.460918 0.009422 -21.00000 0.05580 #PART 0 #CL2 3 0.774337 0.241936 0.409310 11.00000 0.03739 0.02528 = #0.02798 0.00852 0.00811 0.00573 #O12 5 0.929735 0.284708 0.408041 11.00000 0.04687 0.06832 = #0.08395 0.01895 0.02938 0.00326 #O22 5 0.753760 0.296175 0.505641 11.00000 0.06292 0.03976 = #0.02878 0.00721 0.01222 0.01678 #O32 5 0.674975 0.290164 0.341457 11.00000 0.07966 0.03771 = #0.03634 0.01326 -0.01007 0.01402 #O42 5 0.735481 0.092182 0.382191 11.00000 0.06611 0.02629 = #0.03976 0.01159 0.01467 0.01112 #HKLF 4 #REM r71143b in P-1 #REM R1 = 0.0543 for 4979 Fo > 4sig(Fo) and 0.0657 for all 5900 data #REM 373 parameters refined using 0 restraints #END #WGHT 0.0706 1.5366 #REM Highest difference peak 1.317, deepest hole -0.550, 1-sigma level 0.109 #Q1 1 0.1586 0.3822 0.0003 11.00000 0.05 1.32 #Q2 1 -0.0025 0.4208 0.0182 11.00000 0.05 1.18 #Q3 1 0.0919 0.1251 0.1938 11.00000 0.05 1.17 #Q4 1 0.3655 0.4476 -0.1327 11.00000 0.05 1.04 #Q5 1 0.2776 0.0748 0.2280 11.00000 0.05 0.95 #Q6 1 0.4580 0.4825 -0.1789 11.00000 0.05 0.73 #Q7 1 0.1037 0.4656 0.0013 11.00000 0.05 0.67 #Q8 1 0.3155 0.3463 -0.1100 11.00000 0.05 0.66 #Q9 1 -0.3895 0.0078 0.2308 11.00000 0.05 0.60 #Q10 1 0.8431 0.2638 0.3693 11.00000 0.05 0.59 ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0707P)^2^+1.5339P] 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_number_reflns 5900 _refine_ls_number_parameters 373 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0657 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1438 _refine_ls_wR_factor_gt 0.1348 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.003 _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 Zn1 Zn 0.18940(4) 0.09907(4) 0.21145(3) 0.02095(12) Uani 1 1 d . . . N1 N 0.1460(3) -0.0742(3) 0.2718(2) 0.0221(6) Uani 1 1 d . . . N2 N 0.2732(3) 0.1961(3) 0.3605(2) 0.0223(6) Uani 1 1 d . . . N7 N 0.2566(4) 0.4190(3) 0.3551(2) 0.0295(6) Uani 1 1 d . . . H7NA H 0.2167 0.3873 0.2918 0.035 Uiso 1 1 calc R . . H7NB H 0.2708 0.5079 0.3846 0.035 Uiso 1 1 calc R . . N13 N -0.0603(4) -0.3207(3) 0.2760(2) 0.0287(6) Uani 1 1 d . . . H13N H -0.1350 -0.3293 0.2200 0.048(13) Uiso 1 1 calc R . . C1 C 0.2799(4) -0.0422(3) 0.3556(3) 0.0255(7) Uani 1 1 d . . . H1A H 0.3711 -0.0636 0.3317 0.031 Uiso 1 1 calc R . . H1B H 0.2604 -0.1005 0.3986 0.031 Uiso 1 1 calc R . . C2 C 0.3109(4) 0.1080(3) 0.4128(2) 0.0235(6) Uani 1 1 d . . . C3 C 0.3755(4) 0.1503(4) 0.5111(3) 0.0312(8) Uani 1 1 d . . . H3A H 0.3991 0.0856 0.5459 0.037 Uiso 1 1 calc R . . C4 C 0.4056(4) 0.2924(4) 0.5587(3) 0.0340(8) Uani 1 1 d . . . H4A H 0.4548 0.3257 0.6263 0.041 Uiso 1 1 calc R . . C5 C 0.3643(4) 0.3828(4) 0.5081(3) 0.0312(8) Uani 1 1 d . . . H5A H 0.3814 0.4788 0.5404 0.037 Uiso 1 1 calc R . . C6 C 0.2957(4) 0.3318(3) 0.4068(2) 0.0234(6) Uani 1 1 d . . . C11 C 0.0001(4) -0.0676(3) 0.3026(3) 0.0244(7) Uani 1 1 d . . . H11A H -0.0818 -0.0722 0.2452 0.029 Uiso 1 1 calc R . . H11B H 0.0117 0.0227 0.3513 0.029 Uiso 1 1 calc R . . C12 C -0.0499(4) -0.1823(3) 0.3464(3) 0.0277(7) Uani 1 1 d . . . H12A H 0.0250 -0.1723 0.4083 0.033 Uiso 1 1 calc R . . H12B H -0.1511 -0.1753 0.3609 0.033 Uiso 1 1 calc R . . C13 C -0.1082(5) -0.4353(4) 0.3172(3) 0.0352(8) Uani 1 1 d . . . H13A H -0.1140 -0.5242 0.2700 0.053 Uiso 1 1 calc R . . H13B H -0.2090 -0.4302 0.3309 0.053 Uiso 1 1 calc R . . H13C H -0.0331 -0.4267 0.3778 0.053 Uiso 1 1 calc R . . C14 C 0.0885(5) -0.3286(3) 0.2477(3) 0.0308(8) Uani 1 1 d . . . H14A H 0.0794 -0.4190 0.1997 0.037 Uiso 1 1 calc R . . H14B H 0.1701 -0.3213 0.3060 0.037 Uiso 1 1 calc R . . C15 C 0.1314(5) -0.2132(3) 0.2038(3) 0.0305(8) Uani 1 1 d . . . H15A H 0.2299 -0.2204 0.1856 0.037 Uiso 1 1 calc R . . H15B H 0.0521 -0.2244 0.1436 0.037 Uiso 1 1 calc R . . O1W O -0.4526(3) -0.0104(3) 0.1873(2) 0.0444(7) Uani 1 1 d . . . N3G N -0.3030(3) 0.0685(3) 0.0477(2) 0.0268(6) Uani 1 1 d . . . H3GA H -0.3708 0.0335 0.0752 0.032 Uiso 1 1 calc R . . O1G O -0.0227(3) 0.1124(2) 0.16264(18) 0.0276(5) Uani 1 1 d . . . C1G C -0.0540(4) 0.2191(3) 0.1422(2) 0.0257(7) Uani 1 1 d . . . O2G O 0.0369(3) 0.3308(3) 0.1619(2) 0.0431(7) Uani 1 1 d . . . C2G C -0.2203(4) 0.2100(4) 0.0909(3) 0.0288(7) Uani 1 1 d . . . H2GC H -0.2726 0.2588 0.1386 0.035 Uiso 1 1 calc R . . H2GD H -0.2225 0.2573 0.0392 0.035 Uiso 1 1 calc R . . C3G C -0.2768(4) -0.0081(3) -0.0328(2) 0.0233(7) Uani 1 1 d . . . O3G O -0.1990(3) 0.0408(2) -0.08146(17) 0.0268(5) Uani 1 1 d . . . C4G C -0.3413(4) -0.1619(4) -0.0632(2) 0.0286(7) Uani 1 1 d . . . H4GA H -0.2724 -0.2081 -0.0261 0.034 Uiso 1 1 calc R . . H4GB H -0.4431 -0.1788 -0.0486 0.034 Uiso 1 1 calc R . . N4G N -0.3556(4) -0.2187(3) -0.1684(2) 0.0295(7) Uani 1 1 d . . . H4GC H -0.358(5) -0.307(5) -0.181(3) 0.038(12) Uiso 1 1 d . . . H4GD H -0.439(6) -0.214(5) -0.196(4) 0.042(14) Uiso 1 1 d . . . Cl1 Cl 0.5215(4) 0.3958(3) -0.15431(16) 0.0367(6) Uani 0.613(6) 1 d P A 1 O11 O 0.4708(9) 0.5152(6) -0.1097(5) 0.072(2) Uani 0.613(6) 1 d P A 1 O21 O 0.6236(7) 0.4392(6) -0.2068(5) 0.0588(17) Uani 0.613(6) 1 d P A 1 O31 O 0.5949(13) 0.3426(12) -0.0801(7) 0.074(3) Uani 0.613(6) 1 d P A 1 O41 O 0.3904(7) 0.2880(7) -0.2220(4) 0.0469(15) Uani 0.613(6) 1 d P A 1 O2W O 0.1806(8) 0.3952(7) -0.0679(6) 0.084(3) Uani 0.613(6) 1 d P A 1 Cl1' Cl 0.4655(6) 0.3633(5) -0.1434(3) 0.0410(9) Uani 0.387(6) 1 d P A 2 O51 O 0.3283(16) 0.3842(14) -0.1134(10) 0.094(4) Uiso 0.387(6) 1 d P A 2 O61 O 0.542(2) 0.481(2) -0.1600(13) 0.108(5) Uiso 0.387(6) 1 d P A 2 O71 O 0.4413(16) 0.2591(15) -0.2309(11) 0.066(4) Uiso 0.387(6) 1 d P A 2 O81 O 0.558(2) 0.313(2) -0.0779(16) 0.073(6) Uiso 0.387(6) 1 d P A 2 O3W O 0.0612(10) 0.4609(10) 0.0094(7) 0.056(3) Uiso 0.387(6) 1 d P . 2 Cl2 Cl 0.77434(10) 0.24194(9) 0.40931(6) 0.0301(2) Uani 1 1 d . . . O12 O 0.9297(4) 0.2847(4) 0.4080(3) 0.0658(10) Uani 1 1 d . . . O22 O 0.7538(4) 0.2962(3) 0.5056(2) 0.0435(7) Uani 1 1 d . . . O32 O 0.6750(4) 0.2902(3) 0.3415(2) 0.0540(9) Uani 1 1 d . . . O42 O 0.7355(4) 0.0922(3) 0.3822(2) 0.0432(7) Uani 1 1 d . . . 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 0.0252(2) 0.01600(19) 0.01917(19) 0.00459(14) 0.00197(14) 0.00161(13) N1 0.0284(14) 0.0140(12) 0.0219(13) 0.0032(10) 0.0048(11) 0.0031(10) N2 0.0250(14) 0.0184(13) 0.0199(13) 0.0041(11) 0.0015(11) 0.0001(10) N7 0.0377(16) 0.0160(13) 0.0266(15) 0.0015(11) -0.0024(13) 0.0012(11) N13 0.0348(16) 0.0196(14) 0.0266(15) 0.0071(12) -0.0005(12) -0.0005(11) C1 0.0266(16) 0.0235(16) 0.0296(17) 0.0128(14) 0.0051(14) 0.0077(13) C2 0.0213(15) 0.0241(16) 0.0238(16) 0.0084(13) 0.0029(12) 0.0008(12) C3 0.0326(19) 0.038(2) 0.0243(17) 0.0169(15) 0.0029(14) 0.0043(15) C4 0.036(2) 0.041(2) 0.0166(16) 0.0042(15) 0.0014(14) -0.0040(16) C5 0.0358(19) 0.0261(17) 0.0221(16) -0.0018(14) 0.0034(14) -0.0039(14) C6 0.0237(16) 0.0208(15) 0.0217(16) 0.0034(13) 0.0030(13) -0.0004(12) C11 0.0256(16) 0.0181(15) 0.0287(17) 0.0072(13) 0.0046(13) 0.0033(12) C12 0.0305(18) 0.0211(16) 0.0320(18) 0.0082(14) 0.0089(14) 0.0045(13) C13 0.042(2) 0.0201(17) 0.044(2) 0.0136(16) 0.0101(18) 0.0004(15) C14 0.049(2) 0.0176(16) 0.0273(18) 0.0051(14) 0.0142(16) 0.0070(14) C15 0.051(2) 0.0168(15) 0.0255(17) 0.0040(13) 0.0154(16) 0.0064(14) O1W 0.0442(17) 0.0512(18) 0.0349(15) 0.0124(14) 0.0075(13) 0.0025(14) N3G 0.0244(14) 0.0332(16) 0.0192(13) 0.0046(12) 0.0029(11) 0.0026(12) O1G 0.0268(12) 0.0252(12) 0.0293(13) 0.0107(10) -0.0001(10) 0.0046(9) C1G 0.0308(17) 0.0207(15) 0.0202(15) -0.0003(13) 0.0013(13) 0.0051(13) O2G 0.0441(16) 0.0194(12) 0.0491(17) 0.0048(12) -0.0150(13) -0.0018(11) C2G 0.0310(18) 0.0262(17) 0.0244(17) 0.0011(14) 0.0005(14) 0.0104(14) C3G 0.0209(15) 0.0253(16) 0.0187(15) 0.0049(13) -0.0031(12) 0.0025(12) O3G 0.0352(13) 0.0193(11) 0.0232(12) 0.0033(9) 0.0076(10) 0.0011(9) C4G 0.0338(18) 0.0257(17) 0.0220(16) 0.0057(14) 0.0047(14) -0.0027(14) N4G 0.0313(17) 0.0248(16) 0.0252(15) 0.0027(12) 0.0042(13) -0.0060(12) Cl1 0.0516(15) 0.0277(11) 0.0257(9) 0.0078(7) -0.0007(9) 0.0053(9) O11 0.110(6) 0.037(3) 0.074(4) 0.016(3) 0.034(4) 0.018(3) O21 0.063(4) 0.051(3) 0.060(4) 0.025(3) 0.007(3) -0.002(3) O31 0.072(6) 0.088(7) 0.056(5) 0.048(5) -0.026(4) 0.006(5) O41 0.038(3) 0.056(4) 0.038(3) 0.013(3) -0.003(3) -0.004(3) O2W 0.066(4) 0.062(4) 0.090(5) 0.016(4) -0.026(4) -0.022(3) Cl1' 0.047(2) 0.040(2) 0.0328(16) 0.0133(14) 0.0016(15) 0.0044(16) Cl2 0.0374(5) 0.0253(4) 0.0280(4) 0.0085(3) 0.0081(3) 0.0057(3) O12 0.047(2) 0.068(2) 0.084(3) 0.019(2) 0.0294(19) 0.0033(17) O22 0.063(2) 0.0398(16) 0.0288(14) 0.0072(12) 0.0122(14) 0.0168(14) O32 0.080(2) 0.0377(17) 0.0363(16) 0.0133(14) -0.0101(16) 0.0140(16) O42 0.066(2) 0.0263(14) 0.0398(16) 0.0116(12) 0.0147(14) 0.0111(13) _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 Zn1 O1G 1.952(2) . ? Zn1 N2 2.085(3) . ? Zn1 O3G 2.094(2) 2 ? Zn1 N4G 2.099(3) 2 ? Zn1 N1 2.185(3) . ? N1 C1 1.476(4) . ? N1 C11 1.484(4) . ? N1 C15 1.485(4) . ? N2 C6 1.346(4) . ? N2 C2 1.354(4) . ? N7 C6 1.343(4) . ? N7 H7NA 0.8800 . ? N7 H7NB 0.8800 . ? N13 C13 1.493(4) . ? N13 C14 1.495(5) . ? N13 C12 1.502(4) . ? N13 H13N 0.9300 . ? C1 C2 1.507(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.368(5) . ? C3 C4 1.404(5) . ? C3 H3A 0.9500 . ? C4 C5 1.366(5) . ? C4 H4A 0.9500 . ? C5 C6 1.415(5) . ? C5 H5A 0.9500 . ? C11 C12 1.525(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.515(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? N3G C3G 1.323(4) . ? N3G C2G 1.449(4) . ? N3G H3GA 0.8800 . ? O1G C1G 1.253(4) . ? C1G O2G 1.242(4) . ? C1G C2G 1.525(5) . ? C2G H2GC 0.9900 . ? C2G H2GD 0.9900 . ? C3G O3G 1.236(4) . ? C3G C4G 1.515(5) . ? O3G Zn1 2.094(2) 2 ? C4G N4G 1.471(4) . ? C4G H4GA 0.9900 . ? C4G H4GB 0.9900 . ? N4G Zn1 2.099(3) 2 ? N4G H4GC 0.87(5) . ? N4G H4GD 0.80(5) . ? Cl1 O21 1.407(7) . ? Cl1 O11 1.413(7) . ? Cl1 O31 1.421(8) . ? Cl1 O41 1.493(6) . ? Cl1' O81 1.38(2) . ? Cl1' O71 1.397(15) . ? Cl1' O61 1.399(18) . ? Cl1' O51 1.425(15) . ? O3W O3W 1.478(18) 2_565 ? Cl2 O12 1.423(3) . ? Cl2 O32 1.431(3) . ? Cl2 O22 1.435(3) . ? Cl2 O42 1.452(3) . ? 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 O1G Zn1 N2 112.98(11) . . ? O1G Zn1 O3G 94.14(10) . 2 ? N2 Zn1 O3G 151.52(11) . 2 ? O1G Zn1 N4G 115.76(13) . 2 ? N2 Zn1 N4G 95.38(11) . 2 ? O3G Zn1 N4G 79.54(11) 2 2 ? O1G Zn1 N1 98.61(10) . . ? N2 Zn1 N1 78.78(10) . . ? O3G Zn1 N1 89.08(10) 2 . ? N4G Zn1 N1 144.29(13) 2 . ? C1 N1 C11 112.5(3) . . ? C1 N1 C15 111.6(3) . . ? C11 N1 C15 108.4(3) . . ? C1 N1 Zn1 102.31(19) . . ? C11 N1 Zn1 106.54(19) . . ? C15 N1 Zn1 115.5(2) . . ? C6 N2 C2 119.2(3) . . ? C6 N2 Zn1 127.5(2) . . ? C2 N2 Zn1 113.3(2) . . ? C6 N7 H7NA 120.0 . . ? C6 N7 H7NB 120.0 . . ? H7NA N7 H7NB 120.0 . . ? C13 N13 C14 111.9(3) . . ? C13 N13 C12 111.1(3) . . ? C14 N13 C12 110.2(3) . . ? C13 N13 H13N 107.8 . . ? C14 N13 H13N 107.8 . . ? C12 N13 H13N 107.8 . . ? N1 C1 C2 110.7(3) . . ? N1 C1 H1A 109.5 . . ? C2 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 108.1 . . ? N2 C2 C3 123.1(3) . . ? N2 C2 C1 115.7(3) . . ? C3 C2 C1 121.1(3) . . ? C2 C3 C4 117.8(3) . . ? C2 C3 H3A 121.1 . . ? C4 C3 H3A 121.1 . . ? C5 C4 C3 120.1(3) . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? C4 C5 C6 119.1(3) . . ? C4 C5 H5A 120.4 . . ? C6 C5 H5A 120.4 . . ? N7 C6 N2 119.2(3) . . ? N7 C6 C5 120.2(3) . . ? N2 C6 C5 120.6(3) . . ? N1 C11 C12 114.1(3) . . ? N1 C11 H11A 108.7 . . ? C12 C11 H11A 108.7 . . ? N1 C11 H11B 108.7 . . ? C12 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? N13 C12 C11 109.9(3) . . ? N13 C12 H12A 109.7 . . ? C11 C12 H12A 109.7 . . ? N13 C12 H12B 109.7 . . ? C11 C12 H12B 109.7 . . ? H12A C12 H12B 108.2 . . ? N13 C13 H13A 109.5 . . ? N13 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N13 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N13 C14 C15 110.4(3) . . ? N13 C14 H14A 109.6 . . ? C15 C14 H14A 109.6 . . ? N13 C14 H14B 109.6 . . ? C15 C14 H14B 109.6 . . ? H14A C14 H14B 108.1 . . ? N1 C15 C14 112.6(3) . . ? N1 C15 H15A 109.1 . . ? C14 C15 H15A 109.1 . . ? N1 C15 H15B 109.1 . . ? C14 C15 H15B 109.1 . . ? H15A C15 H15B 107.8 . . ? C3G N3G C2G 120.2(3) . . ? C3G N3G H3GA 119.9 . . ? C2G N3G H3GA 119.9 . . ? C1G O1G Zn1 120.9(2) . . ? O2G C1G O1G 125.9(3) . . ? O2G C1G C2G 118.0(3) . . ? O1G C1G C2G 116.1(3) . . ? N3G C2G C1G 112.4(3) . . ? N3G C2G H2GC 109.1 . . ? C1G C2G H2GC 109.1 . . ? N3G C2G H2GD 109.1 . . ? C1G C2G H2GD 109.1 . . ? H2GC C2G H2GD 107.9 . . ? O3G C3G N3G 122.5(3) . . ? O3G C3G C4G 119.7(3) . . ? N3G C3G C4G 117.8(3) . . ? C3G O3G Zn1 114.9(2) . 2 ? N4G C4G C3G 109.2(3) . . ? N4G C4G H4GA 109.8 . . ? C3G C4G H4GA 109.8 . . ? N4G C4G H4GB 109.8 . . ? C3G C4G H4GB 109.8 . . ? H4GA C4G H4GB 108.3 . . ? C4G N4G Zn1 109.4(2) . 2 ? C4G N4G H4GC 108(3) . . ? Zn1 N4G H4GC 118(3) 2 . ? C4G N4G H4GD 107(3) . . ? Zn1 N4G H4GD 109(3) 2 . ? H4GC N4G H4GD 104(4) . . ? O21 Cl1 O11 105.8(4) . . ? O21 Cl1 O31 111.8(6) . . ? O11 Cl1 O31 108.6(6) . . ? O21 Cl1 O41 110.0(4) . . ? O11 Cl1 O41 111.2(5) . . ? O31 Cl1 O41 109.4(5) . . ? O81 Cl1' O71 102.2(11) . . ? O81 Cl1' O61 113.1(11) . . ? O71 Cl1' O61 104.8(11) . . ? O81 Cl1' O51 110.1(11) . . ? O71 Cl1' O51 113.7(9) . . ? O61 Cl1' O51 112.5(10) . . ? O12 Cl2 O32 110.1(2) . . ? O12 Cl2 O22 109.7(2) . . ? O32 Cl2 O22 109.6(2) . . ? O12 Cl2 O42 109.5(2) . . ? O32 Cl2 O42 109.05(19) . . ? O22 Cl2 O42 108.86(18) . . ? _diffrn_measured_fraction_theta_max 0.893 _diffrn_reflns_theta_full 28.88 _diffrn_measured_fraction_theta_full 0.893 _refine_diff_density_max 1.317 _refine_diff_density_min -0.550 _refine_diff_density_rms 0.109 data_r65135 _database_code_depnum_ccdc_archive 'CCDC 223726' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ' C13 H23 N5 O2 Zn, 2(Cl O4)' _chemical_formula_sum 'C13 H23 Cl2 N5 O10 Zn' _chemical_formula_weight 545.63 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' Cl Cl 0.1484 0.1585 '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 P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.0691(10) _cell_length_b 7.9677(5) _cell_length_c 16.3441(10) _cell_angle_alpha 90.00 _cell_angle_beta 96.9230(10) _cell_angle_gamma 90.00 _cell_volume 2077.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4551 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 29 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.745 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 1.502 _exptl_absorpt_correction_type Multiscan _exptl_absorpt_correction_T_min 0.892 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18298 _diffrn_reflns_av_R_equivalents 0.0260 _diffrn_reflns_av_sigmaI/netI 0.0265 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 29.00 _reflns_number_total 5145 _reflns_number_gt 4587 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; 029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.93 DATA SET IS COMPLETE TO 0.8 A #------------------------------------------------------------------------------ INTENSITY STATISTICS FOR DATASET # 1 R65135.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.10 284 284 100.0 4.70 98.1 47.68 0.0167 0.0161 2.10 - 1.60 322 322 100.0 5.12 55.8 47.11 0.0169 0.0159 1.60 - 1.40 299 299 100.0 4.91 35.7 41.20 0.0257 0.0176 1.40 - 1.25 348 348 100.0 4.49 32.0 36.09 0.0277 0.0186 1.25 - 1.15 325 325 100.0 4.12 20.9 31.09 0.0301 0.0222 1.15 - 1.05 492 492 100.0 3.88 16.9 25.28 0.0317 0.0255 1.05 - 1.00 301 301 100.0 3.58 14.3 23.60 0.0336 0.0286 1.00 - 0.95 396 396 100.0 3.44 13.2 21.95 0.0375 0.0318 0.95 - 0.90 466 466 100.0 3.26 10.7 18.24 0.0439 0.0369 0.90 - 0.85 592 593 99.8 3.02 7.5 14.61 0.0530 0.0484 0.85 - 0.80 741 743 99.7 2.84 5.4 11.40 0.0634 0.0630 0.80 - 0.75 839 963 87.1 1.89 4.9 9.26 0.0664 0.0818 0.75 - 0.73 98 375 26.1 0.29 5.0 7.50 0.0674 0.1035 #----------------------------------------------------------------------------- 0.85 - 0.73 1678 2081 80.6 1.94 5.1 10.10 0.0646 0.0742 Inf - 0.73 5503 5907 93.2 3.23 20.0 22.90 0.0262 0.0256 Merged [A], lowest resolution = 16.22 Angstroms, 433 outliers downweighted #------------------------------------------------------------------------------ #=============================================================================== 062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.75 125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? No action 244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... Cl1 244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... Cl2 This is a perchlorate anion, and such behaviour is normal. 320_ALERT_2_C Check Hybridisation of C1G in Main Residue . ? 352_ALERT_3_C Short N-H Bond (0.87A) N7 - H7NB = 0.71 Ang. 720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 6 796_ALERT_4_C O-Atom in CIF Coordinate List out of Sequence .. O12 No action. #=============================================================================== Final res file: TITL r65135 in P2(1)/n CELL 0.71073 16.0691 7.9677 16.3441 90.000 96.923 90.000 ZERR 4.00 0.0010 0.0005 0.0010 0.000 0.001 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O CL ZN UNIT 52 92 20 40 8 4 TEMP -123 L.S. 8 BOND $H FMAP 2 PLAN 10 ACTA WGHT 0.047800 1.566700 FVAR 0.43243 ZN 6 0.250681 0.055740 0.141356 11.00000 0.01945 0.01864 = 0.01622 0.00012 0.00024 -0.00101 N1 3 0.288647 0.107907 0.019003 11.00000 0.02192 0.02192 = 0.01968 -0.00039 0.00336 -0.00029 C1 1 0.261598 -0.041548 -0.030867 11.00000 0.03784 0.02706 = 0.02259 -0.00645 0.00775 -0.00374 AFIX 23 H1A 2 0.303375 -0.132298 -0.018898 11.00000 -1.20000 H1B 2 0.258786 -0.013316 -0.090125 11.00000 -1.20000 AFIX 0 N2 3 0.156790 -0.066928 0.063392 11.00000 0.02359 0.01940 = 0.01923 0.00077 -0.00129 -0.00229 C2 1 0.177034 -0.102387 -0.012508 11.00000 0.03566 0.02169 = 0.02135 -0.00014 -0.00119 -0.00380 C3 1 0.125473 -0.192749 -0.069219 11.00000 0.05388 0.03875 = 0.02283 -0.00583 -0.00434 -0.01341 AFIX 43 H3A 2 0.140652 -0.213452 -0.122712 11.00000 -1.20000 AFIX 0 C4 1 0.050376 -0.253401 -0.046528 11.00000 0.05426 0.04319 = 0.03554 -0.00491 -0.01493 -0.02159 AFIX 43 H4A 2 0.014391 -0.319251 -0.084176 11.00000 -1.20000 AFIX 0 C5 1 0.028250 -0.218409 0.029883 11.00000 0.03082 0.03745 = 0.03851 0.00325 -0.00908 -0.01358 AFIX 43 H5A 2 -0.022829 -0.259876 0.045840 11.00000 -1.20000 AFIX 0 C6 1 0.082481 -0.119788 0.084590 11.00000 0.02364 0.02149 = 0.02662 0.00579 -0.00458 -0.00241 N7 3 0.062370 -0.078856 0.159154 11.00000 0.02018 0.03617 = 0.03142 0.00118 0.00362 -0.00754 H7NB 2 0.024003 -0.107524 0.170814 11.00000 0.02675 H7NA 2 0.090129 -0.013094 0.189195 11.00000 0.03062 C11 1 0.379573 0.141418 0.020452 11.00000 0.02198 0.03215 = 0.02518 0.00579 0.00377 0.00135 AFIX 23 H11A 2 0.411036 0.038027 0.037802 11.00000 -1.20000 H11B 2 0.396266 0.229166 0.062100 11.00000 -1.20000 AFIX 0 C12 1 0.404103 0.197910 -0.061906 11.00000 0.02845 0.04066 = 0.02901 0.00547 0.00910 0.00189 AFIX 23 H12A 2 0.465196 0.219356 -0.056745 11.00000 -1.20000 H12B 2 0.390848 0.108334 -0.103411 11.00000 -1.20000 AFIX 0 N13 3 0.357538 0.354398 -0.089376 11.00000 0.03116 0.03508 = 0.02345 0.00630 0.00206 -0.00756 H13N 2 0.374670 0.425032 -0.051241 11.00000 0.02823 C13 1 0.380128 0.415904 -0.170175 11.00000 0.04495 0.06445 = 0.02885 0.01795 0.00726 -0.01203 AFIX 33 H13A 2 0.349195 0.519410 -0.185575 11.00000 -1.50000 H13B 2 0.365529 0.330312 -0.212540 11.00000 -1.50000 H13C 2 0.440482 0.438341 -0.165419 11.00000 -1.50000 AFIX 0 C14 1 0.265318 0.324012 -0.093501 11.00000 0.02792 0.03710 = 0.02811 0.01050 -0.00180 -0.00114 AFIX 23 H14A 2 0.248048 0.240431 -0.137076 11.00000 -1.20000 H14B 2 0.234833 0.429770 -0.108322 11.00000 -1.20000 AFIX 0 C15 1 0.242036 0.260633 -0.011869 11.00000 0.02332 0.02623 = 0.02556 0.00312 0.00155 0.00122 AFIX 23 H15A 2 0.252783 0.350785 0.029747 11.00000 -1.20000 H15B 2 0.181236 0.235798 -0.018058 11.00000 -1.20000 AFIX 0 O1G 4 0.245884 -0.127803 0.229825 11.00000 0.02150 0.02466 = 0.02218 0.00528 -0.00126 -0.00396 O2G 4 0.178388 0.251875 0.162515 11.00000 0.02519 0.02186 = 0.02274 -0.00532 -0.00171 0.00287 C1G 1 0.307956 -0.134480 0.283541 11.00000 0.02157 0.01901 = 0.01795 -0.00064 0.00308 -0.00070 C2G 1 0.372497 0.004228 0.287944 11.00000 0.03324 0.02868 = 0.02350 0.00601 -0.00723 -0.01196 AFIX 23 H2GB 2 0.367850 0.073561 0.337453 11.00000 -1.20000 H2GA 2 0.429256 -0.045987 0.293728 11.00000 -1.20000 AFIX 0 N3G 3 0.362068 0.111914 0.214762 11.00000 0.01912 0.01928 = 0.02220 0.00167 0.00199 -0.00082 H3GB 2 0.358765 0.216535 0.231737 11.00000 0.03568 H3GA 2 0.403560 0.106090 0.193894 11.00000 0.03433 CL1 5 0.395320 -0.132464 -0.238750 11.00000 0.02590 0.03629 = 0.03074 -0.00158 -0.00149 0.00321 O11 4 0.457420 -0.151248 -0.168604 11.00000 0.03237 0.06425 = 0.03945 0.00137 -0.00973 0.00100 O21 4 0.315126 -0.145169 -0.213323 11.00000 0.02551 0.16297 = 0.04013 -0.03538 0.00608 0.00813 O31 4 0.404198 -0.260777 -0.298006 11.00000 0.04170 0.07508 = 0.03799 -0.01574 0.00396 0.02331 O41 4 0.405417 0.024232 -0.276228 11.00000 0.15431 0.04974 = 0.09623 0.02980 -0.04738 -0.02257 CL2 5 0.374063 -0.377089 0.105528 11.00000 0.03416 0.02319 = 0.02981 -0.00134 0.00856 -0.00063 O12 4 0.400896 -0.216063 0.136924 11.00000 0.05435 0.03464 = 0.05991 -0.01905 0.02411 -0.01406 O22 4 0.400696 -0.504950 0.163083 11.00000 0.06634 0.05040 = 0.05264 0.02280 0.00438 -0.00216 O32 4 0.285107 -0.383616 0.087500 11.00000 0.03638 0.04532 = 0.08518 -0.00750 -0.00241 0.00230 O42 4 0.412382 -0.405939 0.031238 11.00000 0.07823 0.05469 = 0.04217 -0.01795 0.03311 -0.02507 HKLF 4 REM r65135 in P2(1)/n REM R1 = 0.0344 for 4587 Fo > 4sig(Fo) and 0.0389 for all 5145 data REM 300 parameters refined using 0 restraints END WGHT 0.0475 1.5738 REM Highest difference peak 0.885, deepest hole -0.504, 1-sigma level 0.080 Q1 1 0.3536 0.0231 -0.2478 11.00000 0.05 0.89 Q2 1 0.3577 -0.1498 -0.2188 11.00000 0.05 0.48 Q3 1 0.4215 -0.1649 -0.3050 11.00000 0.05 0.48 Q4 1 0.2238 0.0564 0.0998 11.00000 0.05 0.45 Q5 1 0.3189 -0.2477 -0.2240 11.00000 0.05 0.45 Q6 1 0.2999 -0.3649 0.0378 11.00000 0.05 0.44 Q7 1 0.1188 -0.0774 0.0713 11.00000 0.05 0.43 Q8 1 0.2152 -0.0723 -0.0243 11.00000 0.05 0.42 Q9 1 0.3408 -0.0605 0.2866 11.00000 0.05 0.42 Q10 1 0.4032 0.0283 -0.3043 11.00000 0.05 0.39 ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0478P)^2^+1.5667P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom/difmap _refine_ls_hydrogen_treatment mixed/refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5145 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0389 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0909 _refine_ls_wR_factor_gt 0.0884 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.001 _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 Zn Zn 0.250681(13) 0.05574(3) 0.141356(13) 0.01826(8) Uani 1 1 d . . . N1 N 0.28865(11) 0.1079(2) 0.01900(10) 0.0211(3) Uani 1 1 d . . . C1 C 0.26160(15) -0.0415(3) -0.03087(13) 0.0288(5) Uani 1 1 d . . . H1A H 0.3034 -0.1323 -0.0189 0.035 Uiso 1 1 calc R . . H1B H 0.2588 -0.0133 -0.0901 0.035 Uiso 1 1 calc R . . N2 N 0.15679(11) -0.0669(2) 0.06339(10) 0.0211(3) Uani 1 1 d . . . C2 C 0.17703(15) -0.1024(3) -0.01251(13) 0.0266(4) Uani 1 1 d . . . C3 C 0.12547(18) -0.1927(3) -0.06922(14) 0.0392(6) Uani 1 1 d . . . H3A H 0.1407 -0.2135 -0.1227 0.047 Uiso 1 1 calc R . . C4 C 0.05038(19) -0.2534(4) -0.04653(16) 0.0460(7) Uani 1 1 d . . . H4A H 0.0144 -0.3193 -0.0842 0.055 Uiso 1 1 calc R . . C5 C 0.02825(15) -0.2184(3) 0.02988(15) 0.0367(5) Uani 1 1 d . . . H5A H -0.0228 -0.2599 0.0458 0.044 Uiso 1 1 calc R . . C6 C 0.08248(13) -0.1198(3) 0.08459(13) 0.0245(4) Uani 1 1 d . . . N7 N 0.06237(13) -0.0789(3) 0.15915(13) 0.0292(4) Uani 1 1 d . . . H7NB H 0.0240(18) -0.108(4) 0.1708(17) 0.027(7) Uiso 1 1 d . . . H7NA H 0.0901(18) -0.013(4) 0.1892(17) 0.031(7) Uiso 1 1 d . . . C11 C 0.37957(13) 0.1414(3) 0.02045(13) 0.0264(4) Uani 1 1 d . . . H11A H 0.4110 0.0380 0.0378 0.032 Uiso 1 1 calc R . . H11B H 0.3963 0.2292 0.0621 0.032 Uiso 1 1 calc R . . C12 C 0.40410(14) 0.1979(3) -0.06191(14) 0.0322(5) Uani 1 1 d . . . H12A H 0.4652 0.2194 -0.0567 0.039 Uiso 1 1 calc R . . H12B H 0.3908 0.1083 -0.1034 0.039 Uiso 1 1 calc R . . N13 N 0.35754(12) 0.3544(3) -0.08938(12) 0.0300(4) Uani 1 1 d . . . H13N H 0.3747(17) 0.425(3) -0.0512(17) 0.028(7) Uiso 1 1 d . . . C13 C 0.38013(18) 0.4159(4) -0.17018(16) 0.0459(7) Uani 1 1 d . . . H13A H 0.3492 0.5194 -0.1856 0.069 Uiso 1 1 calc R . . H13B H 0.3655 0.3303 -0.2125 0.069 Uiso 1 1 calc R . . H13C H 0.4405 0.4383 -0.1654 0.069 Uiso 1 1 calc R . . C14 C 0.26532(14) 0.3240(3) -0.09350(14) 0.0315(5) Uani 1 1 d . . . H14A H 0.2480 0.2404 -0.1371 0.038 Uiso 1 1 calc R . . H14B H 0.2348 0.4298 -0.1083 0.038 Uiso 1 1 calc R . . C15 C 0.24204(13) 0.2606(3) -0.01187(13) 0.0251(4) Uani 1 1 d . . . H15A H 0.2528 0.3508 0.0297 0.030 Uiso 1 1 calc R . . H15B H 0.1812 0.2358 -0.0181 0.030 Uiso 1 1 calc R . . O1G O 0.24588(9) -0.12780(18) 0.22982(9) 0.0231(3) Uani 1 1 d . . . O2G O 0.17839(9) 0.25188(18) 0.16252(9) 0.0236(3) Uani 1 1 d . . . C1G C 0.30796(12) -0.1345(2) 0.28354(11) 0.0195(4) Uani 1 1 d . . . C2G C 0.37250(14) 0.0042(3) 0.28794(13) 0.0293(5) Uani 1 1 d . . . H2GB H 0.3678 0.0736 0.3375 0.035 Uiso 1 1 calc R . . H2GA H 0.4293 -0.0460 0.2937 0.035 Uiso 1 1 calc R . . N3G N 0.36207(11) 0.1119(2) 0.21476(11) 0.0202(3) Uani 1 1 d . . . H3GB H 0.3588(17) 0.217(4) 0.2317(17) 0.036(7) Uiso 1 1 d . . . H3GA H 0.4036(19) 0.106(4) 0.1939(17) 0.034(8) Uiso 1 1 d . . . Cl1 Cl 0.39532(3) -0.13246(7) -0.23875(3) 0.03137(13) Uani 1 1 d . . . O11 O 0.45742(11) -0.1512(3) -0.16860(12) 0.0465(5) Uani 1 1 d . . . O21 O 0.31513(12) -0.1452(4) -0.21332(13) 0.0760(9) Uani 1 1 d . . . O31 O 0.40420(12) -0.2608(3) -0.29801(12) 0.0517(5) Uani 1 1 d . . . O41 O 0.4054(2) 0.0242(4) -0.2762(2) 0.1052(12) Uani 1 1 d . . . Cl2 Cl 0.37406(3) -0.37709(6) 0.10553(3) 0.02867(12) Uani 1 1 d . . . O12 O 0.40090(13) -0.2161(2) 0.13692(13) 0.0482(5) Uani 1 1 d . . . O22 O 0.40070(15) -0.5050(3) 0.16308(14) 0.0567(6) Uani 1 1 d . . . O32 O 0.28511(13) -0.3836(3) 0.08750(15) 0.0564(6) Uani 1 1 d . . . O42 O 0.41238(15) -0.4059(3) 0.03124(13) 0.0563(6) Uani 1 1 d . . . 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 Zn 0.01945(12) 0.01864(13) 0.01622(12) 0.00012(8) 0.00024(8) -0.00101(8) N1 0.0219(8) 0.0219(8) 0.0197(8) -0.0004(6) 0.0034(6) -0.0003(6) C1 0.0378(12) 0.0271(11) 0.0226(10) -0.0065(8) 0.0078(9) -0.0037(9) N2 0.0236(8) 0.0194(8) 0.0192(8) 0.0008(6) -0.0013(6) -0.0023(6) C2 0.0357(11) 0.0217(10) 0.0213(10) -0.0001(8) -0.0012(8) -0.0038(8) C3 0.0539(15) 0.0387(13) 0.0228(11) -0.0058(10) -0.0043(10) -0.0134(12) C4 0.0543(16) 0.0432(15) 0.0355(13) -0.0049(11) -0.0149(12) -0.0216(13) C5 0.0308(11) 0.0375(13) 0.0385(13) 0.0033(10) -0.0091(10) -0.0136(10) C6 0.0236(10) 0.0215(10) 0.0266(10) 0.0058(8) -0.0046(8) -0.0024(8) N7 0.0202(9) 0.0362(11) 0.0314(10) 0.0012(8) 0.0036(8) -0.0075(8) C11 0.0220(10) 0.0321(11) 0.0252(10) 0.0058(8) 0.0038(8) 0.0014(8) C12 0.0285(11) 0.0407(13) 0.0290(11) 0.0055(9) 0.0091(9) 0.0019(9) N13 0.0312(10) 0.0351(11) 0.0234(9) 0.0063(8) 0.0021(7) -0.0076(8) C13 0.0450(15) 0.0645(18) 0.0289(12) 0.0180(12) 0.0073(11) -0.0120(13) C14 0.0279(11) 0.0371(12) 0.0281(11) 0.0105(9) -0.0018(8) -0.0011(9) C15 0.0233(10) 0.0262(10) 0.0256(10) 0.0031(8) 0.0016(8) 0.0012(8) O1G 0.0215(7) 0.0247(7) 0.0222(7) 0.0053(5) -0.0013(5) -0.0040(5) O2G 0.0252(7) 0.0219(7) 0.0227(7) -0.0053(5) -0.0017(5) 0.0029(6) C1G 0.0216(9) 0.0190(9) 0.0179(9) -0.0006(7) 0.0031(7) -0.0007(7) C2G 0.0332(11) 0.0287(11) 0.0235(10) 0.0060(8) -0.0072(8) -0.0120(9) N3G 0.0191(8) 0.0193(8) 0.0222(8) 0.0017(6) 0.0020(6) -0.0008(6) Cl1 0.0259(3) 0.0363(3) 0.0307(3) -0.0016(2) -0.0015(2) 0.0032(2) O11 0.0324(9) 0.0642(13) 0.0395(10) 0.0014(9) -0.0097(8) 0.0010(9) O21 0.0255(9) 0.163(3) 0.0401(11) -0.0354(14) 0.0061(8) 0.0081(13) O31 0.0417(10) 0.0751(14) 0.0380(10) -0.0157(10) 0.0040(8) 0.0233(10) O41 0.154(3) 0.0497(15) 0.096(2) 0.0298(15) -0.047(2) -0.0226(18) Cl2 0.0342(3) 0.0232(2) 0.0298(3) -0.00134(19) 0.0086(2) -0.0006(2) O12 0.0544(12) 0.0346(10) 0.0599(12) -0.0190(9) 0.0241(10) -0.0141(9) O22 0.0663(14) 0.0504(12) 0.0526(12) 0.0228(10) 0.0044(10) -0.0022(11) O32 0.0364(10) 0.0453(12) 0.0852(17) -0.0075(11) -0.0024(10) 0.0023(9) O42 0.0782(15) 0.0547(12) 0.0422(11) -0.0179(9) 0.0331(11) -0.0251(11) _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 Zn O2G 2.0020(14) . ? Zn O1G 2.0645(14) . ? Zn N3G 2.0799(17) . ? Zn N2 2.0957(16) . ? Zn N1 2.1996(17) . ? N1 C1 1.478(3) . ? N1 C11 1.483(3) . ? N1 C15 1.485(3) . ? C1 C2 1.507(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? N2 C2 1.350(3) . ? N2 C6 1.350(3) . ? C2 C3 1.371(3) . ? C3 C4 1.391(4) . ? C3 H3A 0.9500 . ? C4 C5 1.368(4) . ? C4 H4A 0.9500 . ? C5 C6 1.410(3) . ? C5 H5A 0.9500 . ? C6 N7 1.338(3) . ? N7 H7NB 0.70(3) . ? N7 H7NA 0.81(3) . ? C11 C12 1.516(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N13 1.495(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? N13 C13 1.494(3) . ? N13 C14 1.495(3) . ? N13 H13N 0.86(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.515(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? O1G C1G 1.248(2) . ? O2G C1G 1.264(2) 2 ? C1G O2G 1.264(2) 2_545 ? C1G C2G 1.511(3) . ? C2G N3G 1.465(3) . ? C2G H2GB 0.9900 . ? C2G H2GA 0.9900 . ? N3G H3GB 0.88(3) . ? N3G H3GA 0.79(3) . ? Cl1 O21 1.405(2) . ? Cl1 O41 1.409(3) . ? Cl1 O31 1.427(2) . ? Cl1 O11 1.4342(18) . ? Cl2 O22 1.417(2) . ? Cl2 O32 1.425(2) . ? Cl2 O12 1.4290(18) . ? Cl2 O42 1.4445(19) . ? 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 O2G Zn O1G 111.13(6) . . ? O2G Zn N3G 102.08(7) . . ? O1G Zn N3G 81.41(6) . . ? O2G Zn N2 94.52(6) . . ? O1G Zn N2 90.61(6) . . ? N3G Zn N2 163.24(7) . . ? O2G Zn N1 103.88(6) . . ? O1G Zn N1 143.95(6) . . ? N3G Zn N1 99.79(7) . . ? N2 Zn N1 78.09(6) . . ? C1 N1 C11 112.18(17) . . ? C1 N1 C15 111.71(16) . . ? C11 N1 C15 108.27(16) . . ? C1 N1 Zn 104.70(12) . . ? C11 N1 Zn 113.60(12) . . ? C15 N1 Zn 106.26(12) . . ? N1 C1 C2 111.20(17) . . ? N1 C1 H1A 109.4 . . ? C2 C1 H1A 109.4 . . ? N1 C1 H1B 109.4 . . ? C2 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? C2 N2 C6 119.28(18) . . ? C2 N2 Zn 114.89(14) . . ? C6 N2 Zn 125.70(14) . . ? N2 C2 C3 122.6(2) . . ? N2 C2 C1 116.03(18) . . ? C3 C2 C1 121.4(2) . . ? C2 C3 C4 118.4(2) . . ? C2 C3 H3A 120.8 . . ? C4 C3 H3A 120.8 . . ? C5 C4 C3 120.1(2) . . ? C5 C4 H4A 119.9 . . ? C3 C4 H4A 119.9 . . ? C4 C5 C6 118.9(2) . . ? C4 C5 H5A 120.5 . . ? C6 C5 H5A 120.5 . . ? N7 C6 N2 118.41(19) . . ? N7 C6 C5 121.0(2) . . ? N2 C6 C5 120.6(2) . . ? C6 N7 H7NB 119(2) . . ? C6 N7 H7NA 122.1(19) . . ? H7NB N7 H7NA 119(3) . . ? N1 C11 C12 113.61(17) . . ? N1 C11 H11A 108.8 . . ? C12 C11 H11A 108.8 . . ? N1 C11 H11B 108.8 . . ? C12 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? N13 C12 C11 109.88(18) . . ? N13 C12 H12A 109.7 . . ? C11 C12 H12A 109.7 . . ? N13 C12 H12B 109.7 . . ? C11 C12 H12B 109.7 . . ? H12A C12 H12B 108.2 . . ? C13 N13 C14 111.01(19) . . ? C13 N13 C12 111.9(2) . . ? C14 N13 C12 109.63(18) . . ? C13 N13 H13N 109.6(18) . . ? C14 N13 H13N 111.6(18) . . ? C12 N13 H13N 102.9(18) . . ? N13 C13 H13A 109.5 . . ? N13 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N13 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N13 C14 C15 111.28(17) . . ? N13 C14 H14A 109.4 . . ? C15 C14 H14A 109.4 . . ? N13 C14 H14B 109.4 . . ? C15 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? N1 C15 C14 113.85(18) . . ? N1 C15 H15A 108.8 . . ? C14 C15 H15A 108.8 . . ? N1 C15 H15B 108.8 . . ? C14 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? C1G O1G Zn 115.39(12) . . ? C1G O2G Zn 128.60(13) 2 . ? O1G C1G O2G 125.30(18) . 2_545 ? O1G C1G C2G 119.21(17) . . ? O2G C1G C2G 115.47(17) 2_545 . ? N3G C2G C1G 112.28(16) . . ? N3G C2G H2GB 109.1 . . ? C1G C2G H2GB 109.1 . . ? N3G C2G H2GA 109.1 . . ? C1G C2G H2GA 109.1 . . ? H2GB C2G H2GA 107.9 . . ? C2G N3G Zn 110.53(13) . . ? C2G N3G H3GB 107.6(18) . . ? Zn N3G H3GB 107.7(18) . . ? C2G N3G H3GA 107(2) . . ? Zn N3G H3GA 117(2) . . ? H3GB N3G H3GA 106(3) . . ? O21 Cl1 O41 110.5(2) . . ? O21 Cl1 O31 108.63(15) . . ? O41 Cl1 O31 108.28(18) . . ? O21 Cl1 O11 109.31(13) . . ? O41 Cl1 O11 109.55(16) . . ? O31 Cl1 O11 110.54(12) . . ? O22 Cl2 O32 109.03(14) . . ? O22 Cl2 O12 110.68(14) . . ? O32 Cl2 O12 111.02(13) . . ? O22 Cl2 O42 108.56(15) . . ? O32 Cl2 O42 109.81(15) . . ? O12 Cl2 O42 107.70(12) . . ? _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.932 _refine_diff_density_max 0.885 _refine_diff_density_min -0.504 _refine_diff_density_rms 0.080