Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Juan Carlos Mareque-Rivas' 'Simon Parsons' 'Ravi Prabaharan' _publ_contact_author_name 'Dr Juan Carlos Mareque-Rivas' _publ_contact_author_address ; School of 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 'Dalton Transactions' _publ_section_title ; Quantifying the relative contribution of hydrogen bonding and hydrophobic environments, and coordinating groups, in the the zinc(II)-water acidity by synthetic modelling chemistry ; data_rp33jm _database_code_depnum_ccdc_archive 'CCDC 231104' #note to referee: final checkcif output & res file under #refine special details. _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety "[(L'2)Zn(OH)]ClO4" _chemical_formula_sum 'C28 H41 Cl N6 O5 Zn' _chemical_formula_weight 642.49 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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.8094(8) _cell_length_b 16.4797(12) _cell_length_c 18.1913(13) _cell_angle_alpha 90.00 _cell_angle_beta 107.0310(10) _cell_angle_gamma 90.00 _cell_volume 3098.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4665 _cell_measurement_theta_min 2 _cell_measurement_theta_max 29 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.377 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 0.925 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.409 _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 samrt 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 19339 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_sigmaI/netI 0.0606 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 29.10 _reflns_number_total 7381 _reflns_number_gt 5900 _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 98.2% complete to 0.8 Ang. 061_ALERT_3_A Tmax/Tmin Range Test RR' too Large ............. 0.49 Noted; the high range here probably reflects the lowish crystal quality. 220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.70 Ratio 222_ALERT_3_A Large Non-Solvent H Ueq(max)/Ueq(min) ... 7.17 Ratio 242_ALERT_2_B Check Low U(eq) as Compared to Neighbors .... C19 C19 is the pivot atom of a librating tBu group. 761_ALERT_1_A CIF Contains no X-H Bonds ...................... ? 762_ALERT_1_A CIF Contains no X-Y-H or H-Y-H Angles .......... ? No action. 048_ALERT_1_C MoietyFormula Not Given ........................ ? 062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.82 125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? 213_ALERT_2_C Atom C1# has ADP max/min Ratio ............. 3.60 prolat 244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... Cl 341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 7 720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 4 Noted, but no action taken, #=============================================================================== Final shelx res file: #TITL rp33jm in P2(1)/c CELL 0.71073 10.8094 16.4797 18.1913 90.000 107.031 90.000 ZERR 4.00 0.0008 0.0012 0.0013 0.000 0.001 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O CL ZN UNIT 112 164 24 20 4 4 TEMP -123 L.S. 4 BOND FMAP 2 PLAN 10 HTAB ACTA SADI N7 H7N N17 H17N EADP H17N H7N RTAB D1 N7 O1 RTAB D2 N17 O1 RTAB A1 N7 H7N O1 RTAB A2 N17 H17N O1 WGHT 0.072200 4.246500 FVAR 0.29711 ZN 6 0.422369 0.277250 0.477759 11.00000 0.02456 0.02182 = 0.02255 0.00041 0.00814 0.00351 O1 4 0.590659 0.262311 0.461668 11.00000 0.02750 0.02741 = 0.02740 0.00090 0.01018 0.00572 AFIX 147 H1 2 0.618735 0.307294 0.451819 11.00000 -1.50000 AFIX 0 N1 3 0.231572 0.295885 0.496532 11.00000 0.02213 0.02139 = 0.02411 -0.00152 0.00577 0.00172 C1 1 0.261948 0.326320 0.575881 11.00000 0.02565 0.02752 = 0.02899 -0.00669 0.01274 0.00062 AFIX 23 H1A 2 0.184306 0.321937 0.593992 11.00000 -1.20000 H1B 2 0.286600 0.384280 0.577227 11.00000 -1.20000 AFIX 0 N2 3 0.467134 0.259148 0.597545 11.00000 0.02153 0.02454 = 0.01978 -0.00063 0.00546 -0.00020 C2 1 0.370663 0.278688 0.628148 11.00000 0.02359 0.02932 = 0.02417 -0.00736 0.00881 -0.00259 C3 1 0.372661 0.256985 0.701245 11.00000 0.03438 0.03627 = 0.02639 -0.00754 0.01567 -0.00446 AFIX 43 H3A 2 0.302797 0.270300 0.720806 11.00000 -1.20000 AFIX 0 C4 1 0.480400 0.214730 0.746109 11.00000 0.04272 0.03919 = 0.02228 0.00166 0.01130 -0.00624 AFIX 43 H4A 2 0.483646 0.198907 0.796857 11.00000 -1.20000 AFIX 0 C5 1 0.580126 0.195982 0.718501 11.00000 0.03068 0.04066 = 0.02533 0.00796 0.00502 0.00357 AFIX 43 H5A 2 0.653858 0.168257 0.749815 11.00000 -1.20000 AFIX 0 C6 1 0.573011 0.218449 0.641628 11.00000 0.02452 0.03029 = 0.02220 0.00281 0.00712 -0.00043 N7 3 0.665880 0.201860 0.608464 11.00000 0.02451 0.03676 = 0.02485 0.00755 0.00803 0.00743 H7N 2 0.655819 0.216425 0.564242 11.00000 0.02855 C8 1 0.784321 0.157440 0.643172 11.00000 0.02435 0.03222 = 0.02679 0.00446 0.00479 0.00585 AFIX 23 H8A 2 0.798343 0.118459 0.604977 11.00000 -1.20000 H8B 2 0.773384 0.125696 0.687052 11.00000 -1.20000 AFIX 0 C9 1 0.904849 0.210480 0.671739 11.00000 0.02363 0.03836 = 0.05036 0.01070 0.00961 0.00046 C10C 1 0.921835 0.261854 0.605492 11.00000 0.04291 0.06378 = 0.07795 0.01364 0.03214 -0.00186 AFIX 33 H10A 2 0.847321 0.298106 0.586921 11.00000 -1.50000 H10B 2 0.928013 0.226235 0.563571 11.00000 -1.50000 H10C 2 1.001072 0.294188 0.623474 11.00000 -1.50000 AFIX 0 C10A 1 0.894088 0.264976 0.737178 11.00000 0.05646 0.03916 = 0.05216 -0.00173 0.00660 -0.01629 AFIX 33 H10D 2 0.819969 0.301513 0.718507 11.00000 -1.50000 H10E 2 0.973449 0.297024 0.756121 11.00000 -1.50000 H10F 2 0.881920 0.231468 0.779025 11.00000 -1.50000 AFIX 0 C10B 1 1.020361 0.153477 0.701049 11.00000 0.02164 0.06920 = 0.09340 0.01474 0.00824 0.00343 AFIX 33 H10G 2 1.027354 0.118289 0.659020 11.00000 -1.50000 H10H 2 1.008056 0.120084 0.742932 11.00000 -1.50000 H10I 2 1.099742 0.185506 0.719990 11.00000 -1.50000 AFIX 0 C11 1 0.168100 0.216262 0.486712 11.00000 0.02261 0.03128 = 0.03127 -0.00093 0.01082 -0.00082 AFIX 23 H11A 2 0.073235 0.223915 0.473154 11.00000 -1.20000 H11B 2 0.195985 0.186205 0.535942 11.00000 -1.20000 AFIX 0 N12 3 0.319277 0.176951 0.417522 11.00000 0.02537 0.01882 = 0.02140 0.00116 0.00726 0.00400 C12 1 0.200004 0.167016 0.424959 11.00000 0.02842 0.02010 = 0.02494 0.00425 0.00811 0.00219 C13 1 0.112304 0.111946 0.382060 11.00000 0.02888 0.02566 = 0.04110 -0.00156 0.00685 -0.00209 AFIX 43 H13A 2 0.028682 0.106213 0.388555 11.00000 -1.20000 AFIX 0 C14 1 0.150423 0.064939 0.328818 11.00000 0.03984 0.02686 = 0.03789 -0.00587 0.00273 -0.00565 AFIX 43 H14A 2 0.090916 0.027899 0.297055 11.00000 -1.20000 AFIX 0 C15 1 0.271242 0.071476 0.321871 11.00000 0.04333 0.02099 = 0.03121 -0.00695 0.00876 0.00144 AFIX 43 H15A 2 0.296716 0.038749 0.285823 11.00000 -1.20000 AFIX 0 C16 1 0.360008 0.127591 0.368798 11.00000 0.03161 0.01995 = 0.01963 0.00186 0.00581 0.00656 N17 3 0.481909 0.136846 0.367021 11.00000 0.02994 0.03349 = 0.02836 -0.00832 0.01061 0.00756 H17N 2 0.522351 0.170176 0.397256 11.00000 0.02855 C18 1 0.549735 0.087024 0.325314 11.00000 0.03842 0.04311 = 0.03368 -0.00904 0.01391 0.01310 AFIX 23 H18A 2 0.584701 0.122597 0.292303 11.00000 -1.20000 H18B 2 0.487081 0.049439 0.291273 11.00000 -1.20000 AFIX 0 C19 1 0.658928 0.038293 0.376595 11.00000 0.04373 0.04330 = 0.04302 0.00623 0.01986 0.02203 C2OA 1 0.608304 -0.015546 0.428309 11.00000 0.19022 0.10187 = 0.18145 0.10697 0.14557 0.10449 AFIX 33 H2OA 2 0.571325 0.018078 0.461026 11.00000 -1.50000 H2OB 2 0.679368 -0.048178 0.460632 11.00000 -1.50000 H2OC 2 0.541315 -0.051534 0.396882 11.00000 -1.50000 AFIX 0 C20B 1 0.716919 -0.014497 0.326116 11.00000 0.07347 0.05777 = 0.07648 -0.01044 0.03503 0.03598 AFIX 33 H20D 2 0.751342 0.020256 0.293011 11.00000 -1.50000 H20E 2 0.649719 -0.049998 0.294167 11.00000 -1.50000 H20F 2 0.786926 -0.047640 0.358762 11.00000 -1.50000 AFIX 0 C20C 1 0.762442 0.096080 0.422624 11.00000 0.04450 0.14075 = 0.09229 -0.06478 -0.00573 0.03794 AFIX 33 H20H 2 0.793082 0.130118 0.387357 11.00000 -1.50000 H20G 2 0.835007 0.064795 0.455233 11.00000 -1.50000 H20I 2 0.725964 0.130578 0.454953 11.00000 -1.50000 AFIX 0 C21 1 0.159406 0.356137 0.440906 11.00000 0.02498 0.02837 = 0.03492 -0.00140 0.00570 0.00944 AFIX 23 H21A 2 0.094971 0.383222 0.461621 11.00000 -1.20000 H21B 2 0.112278 0.328523 0.392467 11.00000 -1.20000 AFIX 0 N22 3 0.368689 0.393120 0.428708 11.00000 0.02836 0.02368 = 0.02768 0.00133 0.00648 0.00512 C22 1 0.248755 0.418209 0.424761 11.00000 0.03014 0.03189 = 0.02329 -0.00034 0.00409 0.00838 C23 1 0.210677 0.497522 0.405078 11.00000 0.04551 0.03183 = 0.04399 0.00821 0.01542 0.02088 AFIX 43 H23A 2 0.126392 0.515421 0.403495 11.00000 -1.20000 AFIX 0 C24 1 0.297878 0.550065 0.387792 11.00000 0.07071 0.02779 = 0.05041 0.01261 0.02514 0.01506 AFIX 43 H24A 2 0.273871 0.604868 0.374874 11.00000 -1.20000 AFIX 0 C25 1 0.418544 0.523659 0.389166 11.00000 0.05079 0.03161 = 0.03488 0.00605 0.01677 0.00266 AFIX 43 H25A 2 0.477798 0.558831 0.375423 11.00000 -1.20000 AFIX 0 C26 1 0.451810 0.444531 0.411064 11.00000 0.03719 0.02806 = 0.02819 0.00011 0.01143 0.00474 AFIX 43 H26A 2 0.536191 0.425926 0.413716 11.00000 -1.20000 AFIX 0 CL 5 0.198063 0.553781 0.621923 11.00000 0.02958 0.03249 = 0.02397 -0.00059 0.00591 0.00267 O1A 4 0.222434 0.625735 0.585866 11.00000 0.07597 0.08428 = 0.12875 0.07028 0.04075 0.01515 O2A 4 0.115973 0.502107 0.567641 11.00000 0.05476 0.08757 = 0.07043 -0.04821 -0.01514 0.02234 O3A 4 0.135673 0.574923 0.678020 11.00000 0.04939 0.07756 = 0.04412 -0.01139 0.01722 0.01456 O4A 4 0.318341 0.514207 0.659328 11.00000 0.02552 0.05969 = 0.04380 0.01002 0.00541 0.00685 HKLF 4 REM rp33jm in P2(1)/c REM R1 = 0.0777 for 5900 Fo > 4sig(Fo) and 0.1003 for all 7381 data REM 378 parameters refined using 1 restraints END WGHT 0.0706 4.1285 REM Highest difference peak 1.009, deepest hole -0.563, 1-sigma level 0.103 Q1 1 0.4458 0.2765 0.5335 11.00000 0.05 1.01 Q2 1 0.3975 0.2799 0.4241 11.00000 0.05 0.97 Q3 1 0.1827 0.5488 0.5706 11.00000 0.05 0.73 Q4 1 0.1421 0.5294 0.6364 11.00000 0.05 0.71 Q5 1 0.4868 0.3062 0.4607 11.00000 0.05 0.61 Q6 1 0.1567 0.6012 0.6377 11.00000 0.05 0.60 Q7 1 0.4812 0.2425 0.4611 11.00000 0.05 0.59 Q8 1 0.4142 0.2168 0.4794 11.00000 0.05 0.58 Q9 1 0.2172 0.5516 0.6700 11.00000 0.05 0.54 Q10 1 0.5814 0.2204 0.6806 11.00000 0.05 0.54 ; _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^)+(0.0722P)^2^+4.2465P] 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 'riding/restrained refall' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7381 _refine_ls_number_parameters 378 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1003 _refine_ls_R_factor_gt 0.0777 _refine_ls_wR_factor_ref 0.1801 _refine_ls_wR_factor_gt 0.1694 _refine_ls_goodness_of_fit_ref 1.170 _refine_ls_restrained_S_all 1.170 _refine_ls_shift/su_max 0.005 _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 0.42237(5) 0.27725(3) 0.47776(2) 0.02271(14) Uani 1 1 d . . . O1 O 0.5907(3) 0.26231(18) 0.46167(16) 0.0270(6) Uani 1 1 d . . . H1 H 0.6187 0.3073 0.4518 0.040 Uiso 1 1 calc R . . N1 N 0.2316(3) 0.2959(2) 0.49653(18) 0.0228(7) Uani 1 1 d . . . C1 C 0.2619(4) 0.3263(3) 0.5759(2) 0.0264(9) Uani 1 1 d . . . H1A H 0.1843 0.3219 0.5940 0.032 Uiso 1 1 calc R . . H1B H 0.2866 0.3843 0.5772 0.032 Uiso 1 1 calc R . . N2 N 0.4671(3) 0.2591(2) 0.59754(17) 0.0221(7) Uani 1 1 d . . . C2 C 0.3707(4) 0.2787(3) 0.6281(2) 0.0253(8) Uani 1 1 d . . . C3 C 0.3727(4) 0.2570(3) 0.7012(2) 0.0309(10) Uani 1 1 d . . . H3A H 0.3028 0.2703 0.7208 0.037 Uiso 1 1 calc R . . C4 C 0.4804(5) 0.2147(3) 0.7461(2) 0.0344(10) Uani 1 1 d . . . H4A H 0.4836 0.1989 0.7969 0.041 Uiso 1 1 calc R . . C5 C 0.5801(4) 0.1960(3) 0.7185(2) 0.0329(10) Uani 1 1 d . . . H5A H 0.6539 0.1683 0.7498 0.039 Uiso 1 1 calc R . . C6 C 0.5730(4) 0.2184(3) 0.6416(2) 0.0256(8) Uani 1 1 d . . . N7 N 0.6659(3) 0.2019(2) 0.6085(2) 0.0285(8) Uani 1 1 d D . . H7N H 0.656(5) 0.216(3) 0.564(2) 0.029(9) Uiso 1 1 d D . . C8 C 0.7843(4) 0.1574(3) 0.6432(2) 0.0284(9) Uani 1 1 d . . . H8A H 0.7983 0.1185 0.6050 0.034 Uiso 1 1 calc R . . H8B H 0.7734 0.1257 0.6871 0.034 Uiso 1 1 calc R . . C9 C 0.9048(4) 0.2105(3) 0.6717(3) 0.0377(11) Uani 1 1 d . . . C10C C 0.9218(6) 0.2619(4) 0.6055(4) 0.0585(16) Uani 1 1 d . . . H10A H 0.8473 0.2981 0.5869 0.088 Uiso 1 1 calc R . . H10B H 0.9280 0.2262 0.5636 0.088 Uiso 1 1 calc R . . H10C H 1.0011 0.2942 0.6235 0.088 Uiso 1 1 calc R . . C10A C 0.8941(6) 0.2650(3) 0.7372(3) 0.0512(14) Uani 1 1 d . . . H10D H 0.8200 0.3015 0.7185 0.077 Uiso 1 1 calc R . . H10E H 0.9734 0.2970 0.7561 0.077 Uiso 1 1 calc R . . H10F H 0.8819 0.2315 0.7790 0.077 Uiso 1 1 calc R . . C10B C 1.0204(5) 0.1535(4) 0.7010(4) 0.0633(18) Uani 1 1 d . . . H10G H 1.0274 0.1183 0.6590 0.095 Uiso 1 1 calc R . . H10H H 1.0081 0.1201 0.7429 0.095 Uiso 1 1 calc R . . H10I H 1.0997 0.1855 0.7200 0.095 Uiso 1 1 calc R . . C11 C 0.1681(4) 0.2163(3) 0.4867(2) 0.0278(9) Uani 1 1 d . . . H11A H 0.0732 0.2239 0.4732 0.033 Uiso 1 1 calc R . . H11B H 0.1960 0.1862 0.5359 0.033 Uiso 1 1 calc R . . N12 N 0.3193(3) 0.1770(2) 0.41752(17) 0.0218(7) Uani 1 1 d . . . C12 C 0.2000(4) 0.1670(2) 0.4250(2) 0.0244(8) Uani 1 1 d . . . C13 C 0.1123(4) 0.1119(3) 0.3821(3) 0.0326(10) Uani 1 1 d . . . H13A H 0.0287 0.1062 0.3886 0.039 Uiso 1 1 calc R . . C14 C 0.1504(5) 0.0649(3) 0.3288(3) 0.0367(11) Uani 1 1 d . . . H14A H 0.0909 0.0279 0.2971 0.044 Uiso 1 1 calc R . . C15 C 0.2712(5) 0.0715(3) 0.3219(2) 0.0323(10) Uani 1 1 d . . . H15A H 0.2967 0.0387 0.2858 0.039 Uiso 1 1 calc R . . C16 C 0.3600(4) 0.1276(2) 0.3688(2) 0.0241(8) Uani 1 1 d . . . N17 N 0.4819(4) 0.1368(2) 0.3670(2) 0.0302(8) Uani 1 1 d D . . H17N H 0.522(4) 0.170(3) 0.397(2) 0.029(9) Uiso 1 1 d D . . C18 C 0.5497(5) 0.0870(3) 0.3253(3) 0.0377(11) Uani 1 1 d . . . H18A H 0.5847 0.1226 0.2923 0.045 Uiso 1 1 calc R . . H18B H 0.4871 0.0494 0.2913 0.045 Uiso 1 1 calc R . . C19 C 0.6589(5) 0.0383(3) 0.3766(3) 0.0418(12) Uani 1 1 d . . . C2OA C 0.6083(11) -0.0155(6) 0.4283(6) 0.138(5) Uani 1 1 d . . . H2OA H 0.5713 0.0181 0.4610 0.208 Uiso 1 1 calc R . . H2OB H 0.6794 -0.0482 0.4606 0.208 Uiso 1 1 calc R . . H2OC H 0.5413 -0.0515 0.3969 0.208 Uiso 1 1 calc R . . C20B C 0.7169(7) -0.0145(4) 0.3261(4) 0.0664(19) Uani 1 1 d . . . H20D H 0.7513 0.0203 0.2930 0.100 Uiso 1 1 calc R . . H20E H 0.6497 -0.0500 0.2942 0.100 Uiso 1 1 calc R . . H20F H 0.7869 -0.0476 0.3588 0.100 Uiso 1 1 calc R . . C20C C 0.7624(7) 0.0961(6) 0.4226(5) 0.098(3) Uani 1 1 d . . . H20H H 0.7931 0.1301 0.3874 0.147 Uiso 1 1 calc R . . H20G H 0.8350 0.0648 0.4552 0.147 Uiso 1 1 calc R . . H20I H 0.7260 0.1306 0.4550 0.147 Uiso 1 1 calc R . . C21 C 0.1594(4) 0.3561(3) 0.4409(2) 0.0301(9) Uani 1 1 d . . . H21A H 0.0950 0.3832 0.4616 0.036 Uiso 1 1 calc R . . H21B H 0.1123 0.3285 0.3925 0.036 Uiso 1 1 calc R . . N22 N 0.3687(3) 0.3931(2) 0.42871(19) 0.0269(7) Uani 1 1 d . . . C22 C 0.2488(4) 0.4182(3) 0.4248(2) 0.0292(9) Uani 1 1 d . . . C23 C 0.2107(5) 0.4975(3) 0.4051(3) 0.0399(11) Uani 1 1 d . . . H23A H 0.1264 0.5154 0.4035 0.048 Uiso 1 1 calc R . . C24 C 0.2979(6) 0.5501(3) 0.3878(3) 0.0481(13) Uani 1 1 d . . . H24A H 0.2739 0.6049 0.3749 0.058 Uiso 1 1 calc R . . C25 C 0.4185(5) 0.5237(3) 0.3892(3) 0.0382(11) Uani 1 1 d . . . H25A H 0.4778 0.5588 0.3754 0.046 Uiso 1 1 calc R . . C26 C 0.4518(5) 0.4445(3) 0.4111(2) 0.0308(9) Uani 1 1 d . . . H26A H 0.5362 0.4259 0.4137 0.037 Uiso 1 1 calc R . . Cl Cl 0.19806(10) 0.55378(7) 0.62192(5) 0.0291(2) Uani 1 1 d . . . O1A O 0.2224(5) 0.6257(3) 0.5859(3) 0.0940(18) Uani 1 1 d . . . O2A O 0.1160(4) 0.5021(3) 0.5676(3) 0.0781(15) Uani 1 1 d . . . O3A O 0.1357(4) 0.5749(3) 0.6780(2) 0.0563(11) Uani 1 1 d . . . O4A O 0.3183(3) 0.5142(2) 0.65933(19) 0.0440(9) 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 0.0246(3) 0.0218(3) 0.0226(2) 0.00041(18) 0.00814(17) 0.00351(19) O1 0.0275(16) 0.0274(16) 0.0274(14) 0.0009(12) 0.0102(12) 0.0057(12) N1 0.0221(17) 0.0214(17) 0.0241(16) -0.0015(13) 0.0058(13) 0.0017(13) C1 0.026(2) 0.028(2) 0.029(2) -0.0067(17) 0.0127(16) 0.0006(17) N2 0.0215(17) 0.0245(18) 0.0198(15) -0.0006(12) 0.0055(12) -0.0002(13) C2 0.024(2) 0.029(2) 0.0242(18) -0.0074(17) 0.0088(15) -0.0026(17) C3 0.034(2) 0.036(3) 0.026(2) -0.0075(17) 0.0157(18) -0.0045(19) C4 0.043(3) 0.039(3) 0.0223(19) 0.0017(18) 0.0113(18) -0.006(2) C5 0.031(2) 0.041(3) 0.025(2) 0.0080(18) 0.0050(17) 0.004(2) C6 0.025(2) 0.030(2) 0.0222(18) 0.0028(16) 0.0071(15) -0.0004(17) N7 0.0245(19) 0.037(2) 0.0248(17) 0.0075(15) 0.0080(14) 0.0074(15) C8 0.024(2) 0.032(2) 0.0268(19) 0.0045(17) 0.0048(16) 0.0058(18) C9 0.024(2) 0.038(3) 0.050(3) 0.011(2) 0.010(2) 0.000(2) C10C 0.043(3) 0.064(4) 0.078(4) 0.014(3) 0.032(3) -0.002(3) C10A 0.056(4) 0.039(3) 0.052(3) -0.002(2) 0.007(3) -0.016(3) C10B 0.022(3) 0.069(4) 0.093(5) 0.015(4) 0.008(3) 0.003(3) C11 0.023(2) 0.031(2) 0.031(2) -0.0009(17) 0.0108(16) -0.0008(18) N12 0.0254(17) 0.0188(17) 0.0214(15) 0.0012(12) 0.0073(13) 0.0040(13) C12 0.028(2) 0.020(2) 0.0249(18) 0.0042(15) 0.0081(16) 0.0022(16) C13 0.029(2) 0.026(2) 0.041(2) -0.0016(19) 0.0068(18) -0.0021(18) C14 0.040(3) 0.027(2) 0.038(2) -0.0059(19) 0.003(2) -0.006(2) C15 0.043(3) 0.021(2) 0.031(2) -0.0070(17) 0.0088(19) 0.0014(19) C16 0.032(2) 0.020(2) 0.0196(17) 0.0019(14) 0.0058(15) 0.0066(16) N17 0.030(2) 0.033(2) 0.0284(18) -0.0083(16) 0.0106(15) 0.0076(16) C18 0.038(3) 0.043(3) 0.034(2) -0.009(2) 0.014(2) 0.013(2) C19 0.044(3) 0.043(3) 0.043(3) 0.006(2) 0.020(2) 0.022(2) C2OA 0.190(11) 0.102(7) 0.181(9) 0.107(7) 0.146(9) 0.104(7) C20B 0.073(5) 0.058(4) 0.076(4) -0.010(3) 0.035(4) 0.036(3) C20C 0.045(4) 0.141(8) 0.092(5) -0.065(5) -0.006(3) 0.038(4) C21 0.025(2) 0.028(2) 0.035(2) -0.0014(18) 0.0057(17) 0.0094(18) N22 0.0284(19) 0.0237(18) 0.0277(17) 0.0013(14) 0.0065(14) 0.0051(15) C22 0.030(2) 0.032(2) 0.0233(19) -0.0003(17) 0.0041(16) 0.0084(18) C23 0.046(3) 0.032(3) 0.044(3) 0.008(2) 0.015(2) 0.021(2) C24 0.071(4) 0.028(3) 0.050(3) 0.013(2) 0.025(3) 0.015(3) C25 0.051(3) 0.032(3) 0.035(2) 0.0061(19) 0.017(2) 0.003(2) C26 0.037(3) 0.028(2) 0.028(2) 0.0001(17) 0.0114(18) 0.0047(19) Cl 0.0296(5) 0.0325(6) 0.0240(4) -0.0006(4) 0.0059(4) 0.0027(4) O1A 0.076(4) 0.084(4) 0.129(4) 0.070(3) 0.041(3) 0.015(3) O2A 0.055(3) 0.088(3) 0.070(3) -0.048(3) -0.015(2) 0.022(2) O3A 0.049(2) 0.078(3) 0.044(2) -0.011(2) 0.0172(17) 0.015(2) O4A 0.0255(17) 0.060(2) 0.0438(18) 0.0100(17) 0.0054(14) 0.0069(16) _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 O1 1.941(3) . ? Zn N2 2.110(3) . ? Zn N12 2.112(3) . ? Zn N22 2.116(3) . ? Zn N1 2.208(3) . ? N1 C11 1.467(5) . ? N1 C21 1.468(5) . ? N1 C1 1.472(5) . ? C1 C2 1.499(6) . ? N2 C2 1.357(5) . ? N2 C6 1.366(5) . ? C2 C3 1.371(6) . ? C3 C4 1.397(7) . ? C4 C5 1.352(6) . ? C5 C6 1.427(5) . ? C6 N7 1.342(5) . ? N7 C8 1.449(5) . ? C8 C9 1.528(6) . ? C9 C10A 1.523(7) . ? C9 C10C 1.527(7) . ? C9 C10B 1.528(7) . ? C11 C12 1.505(5) . ? N12 C12 1.345(5) . ? N12 C16 1.367(5) . ? C12 C13 1.378(6) . ? C13 C14 1.393(6) . ? C14 C15 1.353(7) . ? C15 C16 1.423(6) . ? C16 N17 1.336(6) . ? N17 C18 1.454(5) . ? C18 C19 1.504(7) . ? C19 C2OA 1.508(9) . ? C19 C20C 1.520(9) . ? C19 C20B 1.527(7) . ? C21 C22 1.494(6) . ? N22 C26 1.341(6) . ? N22 C22 1.342(5) . ? C22 C23 1.386(6) . ? C23 C24 1.382(7) . ? C24 C25 1.368(7) . ? C25 C26 1.380(6) . ? Cl O2A 1.405(4) . ? Cl O1A 1.417(5) . ? Cl O3A 1.422(4) . ? Cl O4A 1.435(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 O1 Zn N2 101.32(12) . . ? O1 Zn N12 101.41(13) . . ? N2 Zn N12 110.59(13) . . ? O1 Zn N22 101.79(13) . . ? N2 Zn N22 120.98(13) . . ? N12 Zn N22 116.73(13) . . ? O1 Zn N1 179.26(13) . . ? N2 Zn N1 78.58(12) . . ? N12 Zn N1 79.30(12) . . ? N22 Zn N1 77.67(13) . . ? C11 N1 C21 112.7(3) . . ? C11 N1 C1 112.7(3) . . ? C21 N1 C1 111.5(3) . . ? C11 N1 Zn 106.3(2) . . ? C21 N1 Zn 108.6(2) . . ? C1 N1 Zn 104.4(2) . . ? N1 C1 C2 110.6(3) . . ? C2 N2 C6 119.2(3) . . ? C2 N2 Zn 114.8(3) . . ? C6 N2 Zn 125.1(3) . . ? N2 C2 C3 122.7(4) . . ? N2 C2 C1 114.7(3) . . ? C3 C2 C1 122.6(4) . . ? C2 C3 C4 118.1(4) . . ? C5 C4 C3 121.1(4) . . ? C4 C5 C6 119.0(4) . . ? N7 C6 N2 116.4(3) . . ? N7 C6 C5 123.7(4) . . ? N2 C6 C5 119.9(4) . . ? C6 N7 C8 126.1(3) . . ? N7 C8 C9 114.6(4) . . ? C10A C9 C10C 110.1(5) . . ? C10A C9 C10B 109.4(5) . . ? C10C C9 C10B 110.0(4) . . ? C10A C9 C8 110.5(4) . . ? C10C C9 C8 109.7(4) . . ? C10B C9 C8 107.2(4) . . ? N1 C11 C12 111.8(3) . . ? C12 N12 C16 119.5(3) . . ? C12 N12 Zn 114.8(3) . . ? C16 N12 Zn 125.5(3) . . ? N12 C12 C13 123.0(4) . . ? N12 C12 C11 116.4(3) . . ? C13 C12 C11 120.5(4) . . ? C12 C13 C14 117.7(4) . . ? C15 C14 C13 120.7(4) . . ? C14 C15 C16 119.7(4) . . ? N17 C16 N12 117.1(4) . . ? N17 C16 C15 123.8(4) . . ? N12 C16 C15 119.1(4) . . ? C16 N17 C18 126.9(4) . . ? N17 C18 C19 113.7(4) . . ? C18 C19 C2OA 109.8(5) . . ? C18 C19 C20C 108.9(5) . . ? C2OA C19 C20C 111.6(7) . . ? C18 C19 C20B 108.5(4) . . ? C2OA C19 C20B 109.1(6) . . ? C20C C19 C20B 108.8(5) . . ? N1 C21 C22 110.8(3) . . ? C26 N22 C22 119.8(4) . . ? C26 N22 Zn 123.4(3) . . ? C22 N22 Zn 116.2(3) . . ? N22 C22 C23 120.9(4) . . ? N22 C22 C21 116.6(4) . . ? C23 C22 C21 122.4(4) . . ? C24 C23 C22 118.6(5) . . ? C25 C24 C23 120.4(5) . . ? C24 C25 C26 118.2(5) . . ? N22 C26 C25 122.0(4) . . ? O2A Cl O1A 110.3(4) . . ? O2A Cl O3A 108.6(3) . . ? O1A Cl O3A 108.6(3) . . ? O2A Cl O4A 110.8(2) . . ? O1A Cl O4A 109.5(3) . . ? O3A Cl O4A 109.0(2) . . ? _diffrn_measured_fraction_theta_max 0.887 _diffrn_reflns_theta_full 29.10 _diffrn_measured_fraction_theta_full 0.887 _refine_diff_density_max 1.009 _refine_diff_density_min -0.563 _refine_diff_density_rms 0.103 #====END data_rp36jm _database_code_depnum_ccdc_archive 'CCDC 231105' #Note to referee: final check cif output & res file under #refine special details. _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety "[(L'3)Zn(OH)]ClO4" _chemical_formula_sum 'C35 H55 Cl N8 O5 Zn' _chemical_formula_weight 768.69 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 12.7118(12) _cell_length_b 12.7710(12) _cell_length_c 13.5187(13) _cell_angle_alpha 101.784(2) _cell_angle_beta 96.264(2) _cell_angle_gamma 110.2770(10) _cell_volume 1976.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7646 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.52 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.292 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 0.738 _exptl_absorpt_correction_type Multiscan _exptl_absorpt_correction_T_min 0.805 _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 17842 _diffrn_reflns_av_R_equivalents 0.0263 _diffrn_reflns_av_sigmaI/netI 0.0459 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 28.93 _reflns_number_total 9292 _reflns_number_gt 7822 _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 99% complete to 0.8 Ang. 220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.17 Ratio 222_ALERT_3_A Large Non-Solvent H Ueq(max)/Ueq(min) ... 5.56 Ratio 242_ALERT_2_A Check Low U(eq) as Compared to Neighbors .... C19 tBu group on C19 shows high thermal motion or disorder. Electron density modelled with adps. #=============================================================================== 048_ALERT_1_C MoietyFormula Not Given ........................ ? 062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.90 125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? 202_ALERT_3_C Isotropic non-H Atoms in Anion/Solvent ....... = 1 213_ALERT_2_C Atom C20B has ADP max/min Ratio ............. 3.40 prolat 242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... C9 242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... C29 244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... C1S 244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... Cl1 413_ALERT_2_C Short Inter XH3 .. XHn H20H .. H20H = 2.10 Ang. 416_ALERT_2_C Short Intra D-H..H-D H1 .. H7N = 1.90 Ang. 720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 3 #=============================================================================== Noted, but no action. Final shelx res file: #TITL rp36jm in P-1 CELL 0.71073 12.7118 12.7710 13.5187 101.784 96.264 110.277 ZERR 2.00 0.0012 0.0012 0.0013 0.002 0.002 0.001 LATT 1 SFAC C H CL N O ZN UNIT 70 110 2 16 10 2 TEMP -123 L.S. 4 BOND FMAP 2 PLAN 20 SADI 0.01 N7 H7N N17 H17N N27 H27N EADP H7N H17N H27N HTAB ACTA BOND $H RTAB D1 N7 O1 RTAB D2 N17 O1 RTAB D3 N27 O1 RTAB A1 N7 H7N O1 RTAB A2 N17 H17N O1 RTAB A3 N27 H27N O1 WGHT 0.062100 2.797500 FVAR 0.46901 ZN1 6 0.191509 0.197841 0.251875 11.00000 0.02005 0.02819 = 0.02891 0.01244 0.00571 0.01031 O1 5 0.270923 0.118190 0.321305 11.00000 0.02948 0.03030 = 0.04611 0.01888 0.01532 0.01739 AFIX 147 H1 2 0.277420 0.064993 0.277396 11.00000 -1.50000 AFIX 0 N1 4 0.099143 0.275050 0.165589 11.00000 0.02385 0.03199 = 0.03473 0.01390 0.00703 0.01126 N2 4 0.317510 0.280041 0.169212 11.00000 0.02840 0.04703 = 0.04445 0.02650 0.01471 0.01813 C1 1 0.180642 0.365815 0.129801 11.00000 0.03642 0.04100 = 0.04974 0.02424 0.00692 0.01679 AFIX 23 H1A 2 0.206983 0.440104 0.183157 11.00000 -1.20000 H1B 2 0.141842 0.375155 0.066503 11.00000 -1.20000 AFIX 0 C2 1 0.283037 0.336774 0.107454 11.00000 0.02625 0.03934 = 0.03946 0.01824 0.00558 0.00930 C3 1 0.343411 0.380341 0.036958 11.00000 0.03830 0.04015 = 0.04208 0.02224 0.00560 0.00963 AFIX 43 H3A 2 0.315746 0.418575 -0.006736 11.00000 -1.20000 AFIX 0 C4 1 0.446673 0.366307 0.032018 11.00000 0.03487 0.04169 = 0.04109 0.01659 0.01502 0.00399 AFIX 43 H4A 2 0.488913 0.392357 -0.017953 11.00000 -1.20000 AFIX 0 C5 1 0.487504 0.316210 0.097256 11.00000 0.02922 0.05227 = 0.04932 0.02111 0.01737 0.01301 AFIX 43 H5A 2 0.558983 0.308654 0.094656 11.00000 -1.20000 AFIX 0 C6 1 0.422627 0.275083 0.169550 11.00000 0.02914 0.04341 = 0.04544 0.02045 0.01462 0.01383 N7 4 0.460657 0.232499 0.243088 11.00000 0.03023 0.05202 = 0.05352 0.02572 0.01345 0.01929 H7N 2 0.407959 0.197354 0.280038 11.00000 0.06371 C8 1 0.578908 0.241062 0.271739 11.00000 0.02986 0.05050 = 0.04313 0.00899 0.00517 0.01545 AFIX 23 H8A 2 0.603838 0.271540 0.347433 11.00000 -1.20000 H8B 2 0.629005 0.297546 0.239860 11.00000 -1.20000 AFIX 0 C9 1 0.595650 0.126695 0.239452 11.00000 0.03947 0.05868 = 0.03938 0.00438 0.00154 0.03053 C10A 1 0.559687 0.076924 0.123657 11.00000 0.10278 0.09035 = 0.05307 -0.01004 -0.00515 0.05902 AFIX 33 H10A 2 0.571058 0.003905 0.104544 11.00000 -1.50000 H10B 2 0.606010 0.131751 0.089249 11.00000 -1.50000 H10C 2 0.478753 0.062950 0.102342 11.00000 -1.50000 AFIX 0 C10B 1 0.530172 0.041790 0.297340 11.00000 0.05964 0.05660 = 0.08373 0.02181 0.00957 0.03527 AFIX 33 H10D 2 0.541648 -0.030979 0.276466 11.00000 -1.50000 H10E 2 0.448468 0.027031 0.280931 11.00000 -1.50000 H10F 2 0.558490 0.074971 0.371675 11.00000 -1.50000 AFIX 0 C10C 1 0.725112 0.158010 0.271594 11.00000 0.04724 0.10033 = 0.08169 0.02375 0.01146 0.04762 AFIX 33 H10G 2 0.742087 0.088087 0.253202 11.00000 -1.50000 H10H 2 0.748852 0.191845 0.346208 11.00000 -1.50000 H10I 2 0.766744 0.214017 0.235816 11.00000 -1.50000 AFIX 0 N12 4 0.182576 0.322981 0.373797 11.00000 0.03263 0.03733 = 0.03230 0.01011 0.00605 0.01858 C11 1 0.039438 0.322578 0.238976 11.00000 0.03144 0.04184 = 0.04656 0.01549 0.00631 0.02146 AFIX 23 H11A 2 -0.030654 0.259710 0.243701 11.00000 -1.20000 H11B 2 0.016322 0.380419 0.213724 11.00000 -1.20000 AFIX 0 C12 1 0.115539 0.378925 0.344823 11.00000 0.03427 0.03707 = 0.04042 0.01283 0.00654 0.01623 C13 1 0.110243 0.474038 0.408595 11.00000 0.05106 0.03941 = 0.05099 0.01064 0.00914 0.02385 AFIX 43 H13A 2 0.065808 0.513839 0.385266 11.00000 -1.20000 AFIX 0 C14 1 0.172614 0.510645 0.509445 11.00000 0.05280 0.03903 = 0.04921 0.00090 0.01324 0.01954 AFIX 43 H14A 2 0.170558 0.576421 0.555776 11.00000 -1.20000 AFIX 0 C15 1 0.236155 0.453364 0.542077 11.00000 0.04365 0.04228 = 0.03732 0.00398 0.00428 0.01377 AFIX 43 H15A 2 0.276967 0.477907 0.611201 11.00000 -1.20000 AFIX 0 C16 1 0.241087 0.357659 0.472943 11.00000 0.03049 0.03848 = 0.03445 0.00705 0.00526 0.01142 N17 4 0.299729 0.293694 0.498981 11.00000 0.04326 0.05404 = 0.03028 0.00998 0.00177 0.02633 H17N 2 0.300198 0.235855 0.445948 11.00000 0.06371 C18 1 0.339411 0.293803 0.604677 11.00000 0.05038 0.05611 = 0.03536 0.01665 0.00805 0.02436 AFIX 23 H18A 2 0.302411 0.214831 0.612995 11.00000 -1.20000 H18B 2 0.313758 0.345730 0.652176 11.00000 -1.20000 AFIX 0 C19 1 0.466707 0.331254 0.636270 11.00000 0.03987 0.06563 = 0.03958 0.01960 -0.00862 0.00644 C20A 1 0.493259 0.326582 0.747169 11.00000 0.09388 0.08457 = 0.04218 0.01303 -0.01859 0.03412 AFIX 33 H20A 2 0.462180 0.375085 0.790908 11.00000 -1.50000 H20B 2 0.576290 0.355041 0.770547 11.00000 -1.50000 H20C 2 0.458446 0.246606 0.751632 11.00000 -1.50000 AFIX 0 C20B 1 0.509510 0.255380 0.568801 11.00000 0.14814 0.37736 = 0.04850 0.02363 0.01285 0.20842 AFIX 33 H20D 2 0.592656 0.281954 0.590154 11.00000 -1.50000 H20E 2 0.490726 0.257931 0.497295 11.00000 -1.50000 H20F 2 0.473561 0.175892 0.574169 11.00000 -1.50000 AFIX 0 C20C 1 0.520607 0.457736 0.633446 11.00000 0.10487 0.13275 = 0.15280 0.09636 -0.05886 -0.05663 AFIX 33 H20G 2 0.488654 0.504189 0.678435 11.00000 -1.50000 H20H 2 0.504105 0.463604 0.562712 11.00000 -1.50000 H20I 2 0.603565 0.486376 0.657383 11.00000 -1.50000 AFIX 0 N22 4 0.026931 0.058096 0.191796 11.00000 0.02262 0.03134 = 0.03676 0.01301 0.00498 0.00702 C21 1 0.018523 0.181260 0.078669 11.00000 0.03283 0.04591 = 0.03864 0.01574 0.00123 0.01587 AFIX 23 H21A 2 0.060152 0.161974 0.024404 11.00000 -1.20000 H21B 2 -0.039967 0.206778 0.048621 11.00000 -1.20000 AFIX 0 C22 1 -0.038911 0.075464 0.116496 11.00000 0.02836 0.03656 = 0.04030 0.01045 0.00293 0.01307 C23 1 -0.150452 0.002883 0.074253 11.00000 0.02750 0.04120 = 0.04508 0.00853 -0.00469 0.00933 AFIX 43 H23A 2 -0.195171 0.018833 0.022681 11.00000 -1.20000 AFIX 0 C24 1 -0.195027 -0.094993 0.110325 11.00000 0.02828 0.03806 = 0.04709 0.00466 0.00238 0.00402 AFIX 43 H24A 2 -0.271451 -0.147647 0.082252 11.00000 -1.20000 AFIX 0 C25 1 -0.131245 -0.116214 0.184639 11.00000 0.03386 0.03141 = 0.04378 0.00851 0.00767 0.00528 AFIX 43 H25A 2 -0.162155 -0.183797 0.208006 11.00000 -1.20000 AFIX 0 C26 1 -0.017833 -0.036711 0.227376 11.00000 0.03121 0.03012 = 0.03539 0.00882 0.00840 0.01081 N27 4 0.048618 -0.049761 0.304467 11.00000 0.03005 0.03204 = 0.04475 0.01843 0.00647 0.00783 H27N 2 0.121875 0.004835 0.324374 11.00000 0.06371 C28 1 0.011914 -0.149643 0.347084 11.00000 0.04206 0.02902 = 0.04123 0.01268 0.00796 0.00829 AFIX 23 H28A 2 -0.005700 -0.220606 0.291533 11.00000 -1.20000 H28B 2 -0.059250 -0.154830 0.372801 11.00000 -1.20000 AFIX 0 C29 1 0.102092 -0.144314 0.435249 11.00000 0.04218 0.03407 = 0.04475 0.01906 0.01114 0.01506 C30A 1 0.204204 -0.160189 0.395639 11.00000 0.07006 0.10762 = 0.06883 0.04972 0.02921 0.06135 AFIX 33 H30A 2 0.260393 -0.156305 0.453406 11.00000 -1.50000 H30B 2 0.239179 -0.098893 0.362289 11.00000 -1.50000 H30C 2 0.178987 -0.235623 0.345640 11.00000 -1.50000 AFIX 0 C30B 1 0.043052 -0.244626 0.480995 11.00000 0.06487 0.04650 = 0.06594 0.03404 0.00443 0.00776 AFIX 33 H30D 2 0.097026 -0.245665 0.538027 11.00000 -1.50000 H30E 2 0.017374 -0.317747 0.427690 11.00000 -1.50000 H30F 2 -0.023022 -0.234658 0.506541 11.00000 -1.50000 AFIX 0 C30C 1 0.140204 -0.032419 0.518538 11.00000 0.06240 0.04388 = 0.04931 0.01421 -0.00379 0.01825 AFIX 33 H30G 2 0.197846 -0.031515 0.573470 11.00000 -1.50000 H30H 2 0.074278 -0.026210 0.546983 11.00000 -1.50000 H30I 2 0.173178 0.032955 0.489116 11.00000 -1.50000 AFIX 0 N1S 4 0.230303 0.895146 0.138169 11.00000 0.09149 0.07651 = 0.05625 0.01642 0.00625 0.03566 C1S 1 0.205256 0.798956 0.128467 11.00000 0.06413 0.06912 = 0.04485 0.00438 0.00380 0.02820 C2S 1 0.173007 0.674966 0.117138 11.00000 0.08233 AFIX 137 H2S1 2 0.207956 0.662377 0.179648 11.00000 -1.50000 H2S2 2 0.199841 0.641822 0.057785 11.00000 -1.50000 H2S3 2 0.089600 0.637561 0.106385 11.00000 -1.50000 AFIX 0 CL1 3 0.836736 0.507716 0.166693 11.00000 0.04185 0.04890 = 0.03240 0.00956 0.00554 0.01929 O1A 5 0.928296 0.535204 0.248135 11.00000 0.13010 0.13801 = 0.06081 -0.00323 -0.02782 0.09483 O2A 5 0.880957 0.556602 0.088148 11.00000 0.09832 0.11444 = 0.08316 0.06059 0.04697 0.05321 O3A 5 0.758088 0.556098 0.201143 11.00000 0.08944 0.12449 = 0.06263 0.02530 0.02930 0.07694 O4A 5 0.785758 0.386729 0.128064 11.00000 0.07993 0.06104 = 0.15010 0.00117 0.05446 0.00181 HKLF 4 REM rp36jm in P-1 REM R1 = 0.0599 for 7822 Fo > 4sig(Fo) and 0.0721 for all 9292 data REM 458 parameters refined using 3 restraints END WGHT 0.0617 2.8103 REM Highest difference peak 0.890, deepest hole -0.597, 1-sigma level 0.080 Q1 1 0.2071 0.1588 0.2923 11.00000 0.05 0.89 Q2 1 0.1765 0.2386 0.2092 11.00000 0.05 0.84 Q3 1 0.1386 0.1975 0.2803 11.00000 0.05 0.82 Q4 1 0.2200 0.2601 0.3045 11.00000 0.05 0.77 Q5 1 0.2445 0.2013 0.2229 11.00000 0.05 0.76 Q6 1 0.7582 0.4354 0.0780 11.00000 0.05 0.74 Q7 1 0.8523 0.4589 0.2257 11.00000 0.05 0.68 Q8 1 0.4017 0.1311 0.1642 11.00000 0.05 0.62 Q9 1 0.9234 0.5388 0.1426 11.00000 0.05 0.61 Q10 1 0.3909 0.2173 0.1196 11.00000 0.05 0.57 Q11 1 0.1563 0.1458 0.1999 11.00000 0.05 0.57 Q12 1 0.3011 0.1371 0.3728 11.00000 0.05 0.54 Q13 1 0.1391 0.4032 0.2252 11.00000 0.05 0.53 Q14 1 0.1768 0.4310 0.3424 11.00000 0.05 0.52 Q15 1 0.1268 0.2618 0.0587 11.00000 0.05 0.50 Q16 1 -0.0203 0.2283 0.1617 11.00000 0.05 0.50 Q17 1 -0.0469 0.1063 0.1736 11.00000 0.05 0.43 Q18 1 0.6185 0.2020 0.2931 11.00000 0.05 0.40 Q19 1 0.8087 0.5344 0.1237 11.00000 0.05 0.38 Q20 1 0.1433 0.6966 0.0892 11.00000 0.05 0.38 ; _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^)+(0.0621P)^2^+2.7975P] 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 'riding/restrained refall' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9292 _refine_ls_number_parameters 458 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0721 _refine_ls_R_factor_gt 0.0599 _refine_ls_wR_factor_ref 0.1506 _refine_ls_wR_factor_gt 0.1412 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.004 _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 0.19151(3) 0.19784(3) 0.25188(3) 0.02453(10) Uani 1 1 d . . . O1 O 0.27092(18) 0.11819(18) 0.32130(17) 0.0316(5) Uani 1 1 d . . . H1 H 0.2774 0.0650 0.2774 0.047 Uiso 1 1 calc R . . N1 N 0.0991(2) 0.2751(2) 0.1656(2) 0.0291(5) Uani 1 1 d . . . N2 N 0.3175(2) 0.2800(2) 0.1692(2) 0.0360(6) Uani 1 1 d . . . C1 C 0.1806(3) 0.3658(3) 0.1298(3) 0.0400(8) Uani 1 1 d . . . H1A H 0.2070 0.4401 0.1832 0.048 Uiso 1 1 calc R . . H1B H 0.1418 0.3752 0.0665 0.048 Uiso 1 1 calc R . . C2 C 0.2830(3) 0.3368(3) 0.1075(3) 0.0347(7) Uani 1 1 d . . . C3 C 0.3434(3) 0.3803(3) 0.0370(3) 0.0400(8) Uani 1 1 d . . . H3A H 0.3157 0.4186 -0.0067 0.048 Uiso 1 1 calc R . . C4 C 0.4467(3) 0.3663(3) 0.0320(3) 0.0406(8) Uani 1 1 d . . . H4A H 0.4889 0.3924 -0.0180 0.049 Uiso 1 1 calc R . . C5 C 0.4875(3) 0.3162(3) 0.0973(3) 0.0422(8) Uani 1 1 d . . . H5A H 0.5590 0.3087 0.0947 0.051 Uiso 1 1 calc R . . C6 C 0.4226(3) 0.2751(3) 0.1696(3) 0.0373(7) Uani 1 1 d . . . N7 N 0.4607(2) 0.2325(3) 0.2431(2) 0.0419(7) Uani 1 1 d D . . H7N H 0.408(3) 0.197(4) 0.280(3) 0.064(8) Uiso 1 1 d D . . C8 C 0.5789(3) 0.2411(3) 0.2717(3) 0.0418(8) Uani 1 1 d . . . H8A H 0.6038 0.2715 0.3474 0.050 Uiso 1 1 calc R . . H8B H 0.6290 0.2975 0.2399 0.050 Uiso 1 1 calc R . . C9 C 0.5957(3) 0.1267(3) 0.2395(3) 0.0444(8) Uani 1 1 d . . . C10A C 0.5597(5) 0.0769(5) 0.1237(4) 0.0820(17) Uani 1 1 d . . . H10A H 0.5711 0.0039 0.1045 0.123 Uiso 1 1 calc R . . H10B H 0.6060 0.1318 0.0892 0.123 Uiso 1 1 calc R . . H10C H 0.4788 0.0629 0.1023 0.123 Uiso 1 1 calc R . . C10B C 0.5302(4) 0.0418(4) 0.2973(4) 0.0628(12) Uani 1 1 d . . . H10D H 0.5416 -0.0310 0.2765 0.094 Uiso 1 1 calc R . . H10E H 0.4485 0.0270 0.2809 0.094 Uiso 1 1 calc R . . H10F H 0.5585 0.0750 0.3717 0.094 Uiso 1 1 calc R . . C10C C 0.7251(4) 0.1580(5) 0.2716(4) 0.0710(14) Uani 1 1 d . . . H10G H 0.7421 0.0881 0.2532 0.107 Uiso 1 1 calc R . . H10H H 0.7489 0.1918 0.3462 0.107 Uiso 1 1 calc R . . H10I H 0.7667 0.2140 0.2358 0.107 Uiso 1 1 calc R . . N12 N 0.1826(2) 0.3230(2) 0.3738(2) 0.0325(6) Uani 1 1 d . . . C11 C 0.0394(3) 0.3226(3) 0.2390(3) 0.0373(7) Uani 1 1 d . . . H11A H -0.0307 0.2597 0.2437 0.045 Uiso 1 1 calc R . . H11B H 0.0163 0.3804 0.2137 0.045 Uiso 1 1 calc R . . C12 C 0.1155(3) 0.3789(3) 0.3448(3) 0.0361(7) Uani 1 1 d . . . C13 C 0.1102(3) 0.4740(3) 0.4086(3) 0.0455(8) Uani 1 1 d . . . H13A H 0.0658 0.5138 0.3853 0.055 Uiso 1 1 calc R . . C14 C 0.1726(3) 0.5106(3) 0.5094(3) 0.0478(9) Uani 1 1 d . . . H14A H 0.1706 0.5764 0.5558 0.057 Uiso 1 1 calc R . . C15 C 0.2362(3) 0.4534(3) 0.5421(3) 0.0431(8) Uani 1 1 d . . . H15A H 0.2770 0.4779 0.6112 0.052 Uiso 1 1 calc R . . C16 C 0.2411(3) 0.3577(3) 0.4729(2) 0.0354(7) Uani 1 1 d . . . N17 N 0.2997(3) 0.2937(3) 0.4990(2) 0.0409(7) Uani 1 1 d D . . H17N H 0.300(4) 0.236(3) 0.446(3) 0.064(8) Uiso 1 1 d D . . C18 C 0.3394(3) 0.2938(4) 0.6047(3) 0.0454(8) Uani 1 1 d . . . H18A H 0.3024 0.2148 0.6130 0.054 Uiso 1 1 calc R . . H18B H 0.3138 0.3457 0.6522 0.054 Uiso 1 1 calc R . . C19 C 0.4667(3) 0.3313(4) 0.6363(3) 0.0525(10) Uani 1 1 d . . . C20A C 0.4933(5) 0.3266(5) 0.7472(3) 0.0766(15) Uani 1 1 d . . . H20A H 0.4622 0.3751 0.7909 0.115 Uiso 1 1 calc R . . H20B H 0.5763 0.3550 0.7705 0.115 Uiso 1 1 calc R . . H20C H 0.4584 0.2466 0.7516 0.115 Uiso 1 1 calc R . . C20B C 0.5095(7) 0.2554(10) 0.5688(4) 0.167(5) Uani 1 1 d . . . H20D H 0.5927 0.2820 0.5902 0.250 Uiso 1 1 calc R . . H20E H 0.4907 0.2579 0.4973 0.250 Uiso 1 1 calc R . . H20F H 0.4736 0.1759 0.5742 0.250 Uiso 1 1 calc R . . C20C C 0.5206(6) 0.4577(7) 0.6334(7) 0.156(4) Uani 1 1 d . . . H20G H 0.4887 0.5042 0.6784 0.234 Uiso 1 1 calc R . . H20H H 0.5041 0.4636 0.5627 0.234 Uiso 1 1 calc R . . H20I H 0.6036 0.4864 0.6574 0.234 Uiso 1 1 calc R . . N22 N 0.0269(2) 0.0581(2) 0.1918(2) 0.0305(5) Uani 1 1 d . . . C21 C 0.0185(3) 0.1813(3) 0.0787(3) 0.0386(7) Uani 1 1 d . . . H21A H 0.0602 0.1620 0.0244 0.046 Uiso 1 1 calc R . . H21B H -0.0400 0.2068 0.0486 0.046 Uiso 1 1 calc R . . C22 C -0.0389(3) 0.0755(3) 0.1165(3) 0.0351(7) Uani 1 1 d . . . C23 C -0.1505(3) 0.0029(3) 0.0743(3) 0.0403(8) Uani 1 1 d . . . H23A H -0.1952 0.0188 0.0227 0.048 Uiso 1 1 calc R . . C24 C -0.1950(3) -0.0950(3) 0.1103(3) 0.0416(8) Uani 1 1 d . . . H24A H -0.2715 -0.1476 0.0823 0.050 Uiso 1 1 calc R . . C25 C -0.1312(3) -0.1162(3) 0.1846(3) 0.0385(7) Uani 1 1 d . . . H25A H -0.1622 -0.1838 0.2080 0.046 Uiso 1 1 calc R . . C26 C -0.0178(3) -0.0367(3) 0.2274(2) 0.0323(6) Uani 1 1 d . . . N27 N 0.0486(2) -0.0498(2) 0.3045(2) 0.0355(6) Uani 1 1 d D . . H27N H 0.122(3) 0.005(3) 0.324(3) 0.064(8) Uiso 1 1 d D . . C28 C 0.0119(3) -0.1496(3) 0.3471(3) 0.0383(7) Uani 1 1 d . . . H28A H -0.0057 -0.2206 0.2915 0.046 Uiso 1 1 calc R . . H28B H -0.0592 -0.1548 0.3728 0.046 Uiso 1 1 calc R . . C29 C 0.1021(3) -0.1443(3) 0.4352(3) 0.0386(7) Uani 1 1 d . . . C30A C 0.2042(4) -0.1602(5) 0.3956(4) 0.0690(14) Uani 1 1 d . . . H30A H 0.2604 -0.1563 0.4534 0.104 Uiso 1 1 calc R . . H30B H 0.2392 -0.0989 0.3623 0.104 Uiso 1 1 calc R . . H30C H 0.1790 -0.2356 0.3456 0.104 Uiso 1 1 calc R . . C30B C 0.0431(4) -0.2446(4) 0.4810(4) 0.0604(12) Uani 1 1 d . . . H30D H 0.0970 -0.2457 0.5380 0.091 Uiso 1 1 calc R . . H30E H 0.0174 -0.3177 0.4277 0.091 Uiso 1 1 calc R . . H30F H -0.0230 -0.2347 0.5065 0.091 Uiso 1 1 calc R . . C30C C 0.1402(4) -0.0324(3) 0.5185(3) 0.0533(10) Uani 1 1 d . . . H30G H 0.1978 -0.0315 0.5735 0.080 Uiso 1 1 calc R . . H30H H 0.0743 -0.0262 0.5470 0.080 Uiso 1 1 calc R . . H30I H 0.1732 0.0330 0.4891 0.080 Uiso 1 1 calc R . . N1S N 0.2303(4) 0.8951(4) 0.1382(3) 0.0745(12) Uani 1 1 d . . . C1S C 0.2053(4) 0.7990(5) 0.1285(3) 0.0607(11) Uani 1 1 d . . . C2S C 0.1730(5) 0.6750(5) 0.1171(5) 0.0823(15) Uiso 1 1 d . . . H2S1 H 0.2080 0.6624 0.1796 0.123 Uiso 1 1 calc R . . H2S2 H 0.1998 0.6418 0.0578 0.123 Uiso 1 1 calc R . . H2S3 H 0.0896 0.6376 0.1064 0.123 Uiso 1 1 calc R . . Cl1 Cl 0.83674(7) 0.50772(8) 0.16669(6) 0.0408(2) Uani 1 1 d . . . O1A O 0.9283(4) 0.5352(4) 0.2481(3) 0.1058(16) Uani 1 1 d . . . O2A O 0.8810(3) 0.5566(4) 0.0881(3) 0.0872(12) Uani 1 1 d . . . O3A O 0.7581(3) 0.5561(4) 0.2011(3) 0.0808(11) Uani 1 1 d . . . O4A O 0.7858(4) 0.3867(3) 0.1281(4) 0.1054(15) 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 0.02005(16) 0.02819(18) 0.02891(18) 0.01244(13) 0.00571(12) 0.01031(13) O1 0.0295(11) 0.0303(11) 0.0461(12) 0.0189(10) 0.0153(10) 0.0174(9) N1 0.0239(12) 0.0320(13) 0.0347(13) 0.0139(11) 0.0070(10) 0.0113(10) N2 0.0284(13) 0.0470(16) 0.0444(15) 0.0265(13) 0.0147(12) 0.0181(12) C1 0.0364(17) 0.0410(18) 0.050(2) 0.0242(16) 0.0069(15) 0.0168(15) C2 0.0263(15) 0.0393(17) 0.0395(17) 0.0182(14) 0.0056(13) 0.0093(13) C3 0.0383(18) 0.0402(18) 0.0421(18) 0.0222(15) 0.0056(14) 0.0096(15) C4 0.0349(17) 0.0417(18) 0.0411(18) 0.0166(15) 0.0150(14) 0.0040(15) C5 0.0292(16) 0.052(2) 0.049(2) 0.0211(17) 0.0174(15) 0.0130(15) C6 0.0291(16) 0.0434(18) 0.0454(18) 0.0205(15) 0.0146(14) 0.0138(14) N7 0.0302(14) 0.0520(18) 0.0535(18) 0.0257(15) 0.0134(13) 0.0193(13) C8 0.0299(16) 0.050(2) 0.0431(19) 0.0090(16) 0.0052(14) 0.0154(15) C9 0.0395(19) 0.059(2) 0.0394(18) 0.0044(16) 0.0015(15) 0.0305(18) C10A 0.103(4) 0.090(4) 0.053(3) -0.010(3) -0.005(3) 0.059(3) C10B 0.060(3) 0.057(3) 0.084(3) 0.022(2) 0.010(2) 0.035(2) C10C 0.047(2) 0.100(4) 0.082(3) 0.024(3) 0.011(2) 0.048(3) N12 0.0326(13) 0.0373(14) 0.0323(13) 0.0101(11) 0.0060(11) 0.0186(12) C11 0.0314(16) 0.0418(18) 0.0466(19) 0.0155(15) 0.0063(14) 0.0215(14) C12 0.0343(16) 0.0371(17) 0.0404(17) 0.0128(14) 0.0065(14) 0.0162(14) C13 0.051(2) 0.0394(19) 0.051(2) 0.0106(16) 0.0091(17) 0.0239(17) C14 0.053(2) 0.0390(19) 0.049(2) 0.0009(16) 0.0132(18) 0.0195(17) C15 0.044(2) 0.0423(19) 0.0373(18) 0.0040(15) 0.0043(15) 0.0138(16) C16 0.0305(16) 0.0385(17) 0.0344(16) 0.0071(14) 0.0053(13) 0.0114(14) N17 0.0433(16) 0.0540(18) 0.0303(14) 0.0100(13) 0.0018(12) 0.0263(15) C18 0.050(2) 0.056(2) 0.0354(18) 0.0167(16) 0.0081(16) 0.0244(18) C19 0.040(2) 0.066(3) 0.0396(19) 0.0196(18) -0.0086(16) 0.0064(19) C20A 0.094(4) 0.085(4) 0.042(2) 0.013(2) -0.019(2) 0.034(3) C20B 0.148(7) 0.377(14) 0.049(3) 0.024(5) 0.013(4) 0.208(9) C20C 0.105(5) 0.133(6) 0.153(7) 0.096(6) -0.059(5) -0.057(5) N22 0.0226(12) 0.0313(13) 0.0368(13) 0.0130(11) 0.0050(10) 0.0070(10) C21 0.0328(16) 0.0459(19) 0.0386(17) 0.0157(15) 0.0012(13) 0.0159(15) C22 0.0284(15) 0.0366(17) 0.0403(17) 0.0105(14) 0.0029(13) 0.0131(13) C23 0.0275(16) 0.0412(18) 0.0451(19) 0.0085(15) -0.0047(14) 0.0093(14) C24 0.0283(16) 0.0381(18) 0.0471(19) 0.0047(15) 0.0024(14) 0.0040(14) C25 0.0339(17) 0.0314(16) 0.0438(18) 0.0085(14) 0.0077(14) 0.0053(14) C26 0.0312(15) 0.0301(15) 0.0354(16) 0.0088(13) 0.0084(13) 0.0108(13) N27 0.0300(13) 0.0320(14) 0.0447(15) 0.0184(12) 0.0065(12) 0.0078(11) C28 0.0421(18) 0.0290(16) 0.0412(18) 0.0127(14) 0.0080(15) 0.0083(14) C29 0.0422(18) 0.0341(17) 0.0447(18) 0.0191(15) 0.0111(15) 0.0151(15) C30A 0.070(3) 0.108(4) 0.069(3) 0.050(3) 0.029(2) 0.061(3) C30B 0.065(3) 0.046(2) 0.066(3) 0.034(2) 0.004(2) 0.008(2) C30C 0.062(3) 0.044(2) 0.049(2) 0.0142(18) -0.0038(19) 0.0182(19) N1S 0.091(3) 0.077(3) 0.056(2) 0.016(2) 0.006(2) 0.036(3) C1S 0.064(3) 0.069(3) 0.045(2) 0.004(2) 0.004(2) 0.028(2) Cl1 0.0418(4) 0.0489(5) 0.0324(4) 0.0096(3) 0.0055(3) 0.0193(4) O1A 0.130(4) 0.138(4) 0.061(2) -0.003(2) -0.028(2) 0.095(3) O2A 0.098(3) 0.114(3) 0.083(2) 0.061(2) 0.047(2) 0.053(2) O3A 0.089(3) 0.124(3) 0.063(2) 0.025(2) 0.0293(18) 0.077(3) O4A 0.080(3) 0.061(2) 0.150(4) 0.001(2) 0.054(3) 0.002(2) _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 O1 1.957(2) . ? Zn1 N12 2.092(3) . ? Zn1 N2 2.150(3) . ? Zn1 N22 2.161(2) . ? Zn1 N1 2.164(2) . ? O1 H1 0.8400 . ? N1 C1 1.469(4) . ? N1 C11 1.472(4) . ? N1 C21 1.476(4) . ? N2 C2 1.342(4) . ? N2 C6 1.359(4) . ? C1 C2 1.516(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.374(4) . ? C3 C4 1.392(5) . ? C3 H3A 0.9500 . ? C4 C5 1.348(5) . ? C4 H4A 0.9500 . ? C5 C6 1.413(4) . ? C5 H5A 0.9500 . ? C6 N7 1.348(4) . ? N7 C8 1.471(4) . ? N7 H7N 0.93(3) . ? C8 C9 1.531(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10A 1.516(6) . ? C9 C10B 1.531(6) . ? C9 C10C 1.541(5) . ? C10A H10A 0.9800 . ? C10A H10B 0.9800 . ? C10A H10C 0.9800 . ? C10B H10D 0.9800 . ? C10B H10E 0.9800 . ? C10B H10F 0.9800 . ? C10C H10G 0.9800 . ? C10C H10H 0.9800 . ? C10C H10I 0.9800 . ? N12 C12 1.361(4) . ? N12 C16 1.363(4) . ? C11 C12 1.515(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.366(5) . ? C13 C14 1.397(5) . ? C13 H13A 0.9500 . ? C14 C15 1.359(5) . ? C14 H14A 0.9500 . ? C15 C16 1.404(5) . ? C15 H15A 0.9500 . ? C16 N17 1.352(4) . ? N17 C18 1.462(4) . ? N17 H17N 0.92(3) . ? C18 C19 1.503(5) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20B 1.476(8) . ? C19 C20A 1.518(5) . ? C19 C20C 1.531(8) . ? C20A H20A 0.9800 . ? C20A H20B 0.9800 . ? C20A H20C 0.9800 . ? C20B H20D 0.9800 . ? C20B H20E 0.9800 . ? C20B H20F 0.9800 . ? C20C H20G 0.9800 . ? C20C H20H 0.9800 . ? C20C H20I 0.9800 . ? N22 C22 1.349(4) . ? N22 C26 1.357(4) . ? C21 C22 1.517(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.375(4) . ? C23 C24 1.393(5) . ? C23 H23A 0.9500 . ? C24 C25 1.351(5) . ? C24 H24A 0.9500 . ? C25 C26 1.417(4) . ? C25 H25A 0.9500 . ? C26 N27 1.343(4) . ? N27 C28 1.457(4) . ? N27 H27N 0.92(3) . ? C28 C29 1.534(5) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30C 1.513(5) . ? C29 C30A 1.517(5) . ? C29 C30B 1.531(5) . ? C30A H30A 0.9800 . ? C30A H30B 0.9800 . ? C30A H30C 0.9800 . ? C30B H30D 0.9800 . ? C30B H30E 0.9800 . ? C30B H30F 0.9800 . ? C30C H30G 0.9800 . ? C30C H30H 0.9800 . ? C30C H30I 0.9800 . ? N1S C1S 1.132(6) . ? C1S C2S 1.462(7) . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 0.9800 . ? Cl1 O1A 1.403(3) . ? Cl1 O4A 1.408(4) . ? Cl1 O2A 1.411(3) . ? Cl1 O3A 1.418(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 O1 Zn1 N12 103.08(10) . . ? O1 Zn1 N2 100.64(9) . . ? N12 Zn1 N2 109.25(11) . . ? O1 Zn1 N22 99.46(9) . . ? N12 Zn1 N22 111.18(10) . . ? N2 Zn1 N22 128.81(11) . . ? O1 Zn1 N1 175.84(10) . . ? N12 Zn1 N1 80.83(10) . . ? N2 Zn1 N1 79.18(9) . . ? N22 Zn1 N1 77.65(9) . . ? Zn1 O1 H1 109.5 . . ? C1 N1 C11 111.8(3) . . ? C1 N1 C21 111.7(3) . . ? C11 N1 C21 112.0(2) . . ? C1 N1 Zn1 109.33(18) . . ? C11 N1 Zn1 104.80(18) . . ? C21 N1 Zn1 106.85(18) . . ? C2 N2 C6 118.5(3) . . ? C2 N2 Zn1 114.3(2) . . ? C6 N2 Zn1 127.2(2) . . ? N1 C1 C2 111.4(3) . . ? N1 C1 H1A 109.3 . . ? C2 C1 H1A 109.3 . . ? N1 C1 H1B 109.3 . . ? C2 C1 H1B 109.3 . . ? H1A C1 H1B 108.0 . . ? N2 C2 C3 123.4(3) . . ? N2 C2 C1 115.8(3) . . ? C3 C2 C1 120.3(3) . . ? C2 C3 C4 117.4(3) . . ? C2 C3 H3A 121.3 . . ? C4 C3 H3A 121.3 . . ? C5 C4 C3 120.8(3) . . ? C5 C4 H4A 119.6 . . ? C3 C4 H4A 119.6 . . ? C4 C5 C6 119.2(3) . . ? C4 C5 H5A 120.4 . . ? C6 C5 H5A 120.4 . . ? N7 C6 N2 116.4(3) . . ? N7 C6 C5 123.3(3) . . ? N2 C6 C5 120.3(3) . . ? C6 N7 C8 125.6(3) . . ? C6 N7 H7N 117(3) . . ? C8 N7 H7N 118(3) . . ? N7 C8 C9 114.4(3) . . ? N7 C8 H8A 108.7 . . ? C9 C8 H8A 108.6 . . ? N7 C8 H8B 108.6 . . ? C9 C8 H8B 108.6 . . ? H8A C8 H8B 107.6 . . ? C10A C9 C10B 111.7(4) . . ? C10A C9 C8 110.7(3) . . ? C10B C9 C8 110.0(3) . . ? C10A C9 C10C 109.3(4) . . ? C10B C9 C10C 109.8(3) . . ? C8 C9 C10C 105.1(3) . . ? C9 C10A H10A 109.5 . . ? C9 C10A H10B 109.5 . . ? H10A C10A H10B 109.5 . . ? C9 C10A H10C 109.5 . . ? H10A C10A H10C 109.5 . . ? H10B C10A H10C 109.5 . . ? C9 C10B H10D 109.5 . . ? C9 C10B H10E 109.5 . . ? H10D C10B H10E 109.5 . . ? C9 C10B H10F 109.5 . . ? H10D C10B H10F 109.5 . . ? H10E C10B H10F 109.5 . . ? C9 C10C H10G 109.5 . . ? C9 C10C H10H 109.5 . . ? H10G C10C H10H 109.5 . . ? C9 C10C H10I 109.5 . . ? H10G C10C H10I 109.5 . . ? H10H C10C H10I 109.5 . . ? C12 N12 C16 119.0(3) . . ? C12 N12 Zn1 113.4(2) . . ? C16 N12 Zn1 127.5(2) . . ? N1 C11 C12 111.0(3) . . ? N1 C11 H11A 109.4 . . ? C12 C11 H11A 109.4 . . ? N1 C11 H11B 109.4 . . ? C12 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? N12 C12 C13 123.0(3) . . ? N12 C12 C11 115.1(3) . . ? C13 C12 C11 121.8(3) . . ? C12 C13 C14 117.5(3) . . ? C12 C13 H13A 121.2 . . ? C14 C13 H13A 121.2 . . ? C15 C14 C13 120.8(3) . . ? C15 C14 H14A 119.6 . . ? C13 C14 H14A 119.6 . . ? C14 C15 C16 119.5(3) . . ? C14 C15 H15A 120.2 . . ? C16 C15 H15A 120.2 . . ? N17 C16 N12 116.2(3) . . ? N17 C16 C15 123.8(3) . . ? N12 C16 C15 120.0(3) . . ? C16 N17 C18 124.6(3) . . ? C16 N17 H17N 116(3) . . ? C18 N17 H17N 118(3) . . ? N17 C18 C19 115.0(3) . . ? N17 C18 H18A 108.5 . . ? C19 C18 H18A 108.5 . . ? N17 C18 H18B 108.5 . . ? C19 C18 H18B 108.5 . . ? H18A C18 H18B 107.5 . . ? C20B C19 C18 110.9(4) . . ? C20B C19 C20A 110.1(4) . . ? C18 C19 C20A 108.2(4) . . ? C20B C19 C20C 112.6(7) . . ? C18 C19 C20C 107.3(4) . . ? C20A C19 C20C 107.6(4) . . ? C19 C20A H20A 109.5 . . ? C19 C20A H20B 109.5 . . ? H20A C20A H20B 109.5 . . ? C19 C20A H20C 109.5 . . ? H20A C20A H20C 109.5 . . ? H20B C20A H20C 109.5 . . ? C19 C20B H20D 109.5 . . ? C19 C20B H20E 109.5 . . ? H20D C20B H20E 109.5 . . ? C19 C20B H20F 109.5 . . ? H20D C20B H20F 109.5 . . ? H20E C20B H20F 109.5 . . ? C19 C20C H20G 109.5 . . ? C19 C20C H20H 109.5 . . ? H20G C20C H20H 109.5 . . ? C19 C20C H20I 109.5 . . ? H20G C20C H20I 109.5 . . ? H20H C20C H20I 109.5 . . ? C22 N22 C26 118.8(3) . . ? C22 N22 Zn1 114.0(2) . . ? C26 N22 Zn1 127.0(2) . . ? N1 C21 C22 109.5(3) . . ? N1 C21 H21A 109.8 . . ? C22 C21 H21A 109.8 . . ? N1 C21 H21B 109.8 . . ? C22 C21 H21B 109.8 . . ? H21A C21 H21B 108.2 . . ? N22 C22 C23 123.6(3) . . ? N22 C22 C21 115.6(3) . . ? C23 C22 C21 120.9(3) . . ? C22 C23 C24 117.1(3) . . ? C22 C23 H23A 121.4 . . ? C24 C23 H23A 121.4 . . ? C25 C24 C23 121.0(3) . . ? C25 C24 H24A 119.5 . . ? C23 C24 H24A 119.5 . . ? C24 C25 C26 119.4(3) . . ? C24 C25 H25A 120.3 . . ? C26 C25 H25A 120.3 . . ? N27 C26 N22 117.4(3) . . ? N27 C26 C25 122.5(3) . . ? N22 C26 C25 120.1(3) . . ? C26 N27 C28 122.7(3) . . ? C26 N27 H27N 115(3) . . ? C28 N27 H27N 122(3) . . ? N27 C28 C29 113.0(3) . . ? N27 C28 H28A 109.0 . . ? C29 C28 H28A 109.0 . . ? N27 C28 H28B 109.0 . . ? C29 C28 H28B 109.0 . . ? H28A C28 H28B 107.8 . . ? C30C C29 C30A 110.4(4) . . ? C30C C29 C30B 108.6(3) . . ? C30A C29 C30B 109.3(3) . . ? C30C C29 C28 111.4(3) . . ? C30A C29 C28 111.2(3) . . ? C30B C29 C28 105.8(3) . . ? C29 C30A H30A 109.5 . . ? C29 C30A H30B 109.5 . . ? H30A C30A H30B 109.5 . . ? C29 C30A H30C 109.5 . . ? H30A C30A H30C 109.5 . . ? H30B C30A H30C 109.5 . . ? C29 C30B H30D 109.5 . . ? C29 C30B H30E 109.5 . . ? H30D C30B H30E 109.5 . . ? C29 C30B H30F 109.5 . . ? H30D C30B H30F 109.5 . . ? H30E C30B H30F 109.5 . . ? C29 C30C H30G 109.5 . . ? C29 C30C H30H 109.5 . . ? H30G C30C H30H 109.5 . . ? C29 C30C H30I 109.5 . . ? H30G C30C H30I 109.5 . . ? H30H C30C H30I 109.5 . . ? N1S C1S C2S 179.4(5) . . ? C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? O1A Cl1 O4A 108.9(3) . . ? O1A Cl1 O2A 108.0(3) . . ? O4A Cl1 O2A 108.9(3) . . ? O1A Cl1 O3A 109.8(2) . . ? O4A Cl1 O3A 112.3(3) . . ? O2A Cl1 O3A 108.8(2) . . ? _diffrn_measured_fraction_theta_max 0.889 _diffrn_reflns_theta_full 28.93 _diffrn_measured_fraction_theta_full 0.889 _refine_diff_density_max 0.890 _refine_diff_density_min -0.597 _refine_diff_density_rms 0.080