Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Juan C. Mareque Rivas' 'Rafael Torres Martin de Rosales' 'Simon Parsons' _publ_contact_author_name 'Dr Juan C Mareque Rivas ' _publ_contact_author_address ; Department of Chemistry The University of Edinburgh The Kings 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 ; Internal hydrogen bonding and amide co-ordination in zinc(II) complexes of a tripodal N4 ligand: Structural, spectroscopic and reactivity studies. ; data_rtrr92 _database_code_CSD 203672 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H27 N5 O' _chemical_formula_sum 'C23 H27 N5 O' _chemical_formula_weight 389.50 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' _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 10.9702(9) _cell_length_b 9.7048(8) _cell_length_c 19.1103(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.555(2) _cell_angle_gamma 90.00 _cell_volume 2034.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4680 _cell_measurement_theta_min 2 _cell_measurement_theta_max 29 _exptl_crystal_description block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.63 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.272 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 0.081 _exptl_absorpt_correction_type Multiscan _exptl_absorpt_correction_T_min 0.849 _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 12533 _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 28.92 _reflns_number_total 4928 _reflns_number_gt 4082 _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 ; Checkcif alerts: 761_ALERT A CIF Contains no X-H Bonds .................... ? 762_ALERT A CIF Contains no X-Y-H or H-Y-H Angles ........ ? The H-atoms were placed in calculated positions. #=============================================================================== 125_ALERT C No _symmetry_space_group_name_Hall given ..... ? 145_ALERT C su on beta Small or Missing (x 10000) ... 20 Deg. No action. Final res file: #TITL rtrr92 in P2(1)/c CELL 0.71073 10.9702 9.7048 19.1103 90.000 90.555 90.000 ZERR 4.00 0.0009 0.0008 0.0015 0.000 0.002 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 92 108 20 4 TEMP -123 L.S. 8 HTAB BOND $H FMAP 2 PLAN 10 ACTA WGHT 0.063300 0.554900 FVAR 0.65146 N1 3 0.175411 0.322939 0.406327 11.00000 0.02184 0.02351 = 0.01486 -0.00054 0.00021 -0.00464 C1 1 0.219456 0.464498 0.395396 11.00000 0.02640 0.02160 = 0.01916 -0.00046 0.00108 -0.00257 AFIX 23 H1A 2 0.257137 0.499664 0.439159 11.00000 -1.20000 H1B 2 0.150046 0.525205 0.382932 11.00000 -1.20000 AFIX 0 C1OB 1 0.194939 0.575437 0.019019 11.00000 0.03028 0.03195 = 0.02247 0.00064 -0.00252 -0.00264 AFIX 33 H1OA 2 0.146094 0.617877 -0.018389 11.00000 -1.50000 H1OB 2 0.142085 0.551931 0.058308 11.00000 -1.50000 H1OC 2 0.233733 0.491596 0.001316 11.00000 -1.50000 AFIX 0 C1OA 1 0.235010 0.809630 0.070301 11.00000 0.02882 0.02501 = 0.02537 0.00237 0.00241 0.00542 AFIX 33 H1OD 2 0.185845 0.851248 0.032790 11.00000 -1.50000 H1OE 2 0.299079 0.874156 0.084923 11.00000 -1.50000 H1OF 2 0.182790 0.788711 0.110240 11.00000 -1.50000 AFIX 0 N2 3 0.278454 0.528113 0.277587 11.00000 0.02225 0.02079 = 0.01950 0.00055 0.00050 -0.00189 C2 1 0.311724 0.466545 0.337628 11.00000 0.02361 0.02058 = 0.01867 0.00020 -0.00137 -0.00576 C3 1 0.422738 0.400595 0.346240 11.00000 0.02551 0.03540 = 0.02330 0.00820 -0.00430 -0.00084 AFIX 43 H3A 2 0.443587 0.357329 0.389312 11.00000 -1.20000 AFIX 0 C4 1 0.502560 0.399145 0.290722 11.00000 0.02044 0.03816 = 0.02965 0.00768 -0.00248 0.00293 AFIX 43 H4A 2 0.579518 0.355049 0.295430 11.00000 -1.20000 AFIX 0 C5 1 0.470261 0.461861 0.228453 11.00000 0.02023 0.03153 = 0.02342 0.00386 0.00085 -0.00072 AFIX 43 H5A 2 0.524069 0.462406 0.189802 11.00000 -1.20000 AFIX 0 C6 1 0.356505 0.524138 0.224172 11.00000 0.02033 0.02091 = 0.01950 0.00106 -0.00148 -0.00335 N7 3 0.309118 0.584395 0.163024 11.00000 0.01793 0.02914 = 0.02006 0.00425 0.00065 0.00338 AFIX 43 H7N 2 0.231540 0.607371 0.163716 11.00000 -1.20000 AFIX 0 O8 4 0.478489 0.587602 0.095703 11.00000 0.02196 0.04155 = 0.02723 0.00680 0.00356 0.00614 C8 1 0.370154 0.611555 0.102221 11.00000 0.02203 0.02070 = 0.01962 -0.00039 0.00123 0.00016 C9 1 0.293173 0.676798 0.043726 11.00000 0.02174 0.02379 = 0.01827 0.00189 0.00159 0.00221 C10C 1 0.376992 0.710966 -0.017236 11.00000 0.02825 0.03530 = 0.02038 0.00459 0.00397 0.00371 AFIX 33 H10A 2 0.329187 0.752928 -0.055220 11.00000 -1.50000 H10B 2 0.415428 0.626265 -0.034135 11.00000 -1.50000 H10C 2 0.440136 0.775624 -0.001463 11.00000 -1.50000 AFIX 0 C11 1 0.099982 0.314722 0.468903 11.00000 0.02044 0.02916 = 0.01832 -0.00008 0.00121 -0.00292 AFIX 23 H11A 2 0.056050 0.225614 0.468509 11.00000 -1.20000 H11B 2 0.038194 0.389001 0.466861 11.00000 -1.20000 AFIX 0 C12 1 0.098733 0.122711 0.339330 11.00000 0.02379 0.02751 = 0.01207 -0.00057 -0.00025 -0.00336 N12 3 -0.011652 0.065615 0.330474 11.00000 0.02217 0.02888 = 0.02196 -0.00372 -0.00113 -0.00362 C13 1 0.205548 0.045511 0.338441 11.00000 0.02142 0.03191 = 0.01896 0.00204 -0.00102 -0.00298 AFIX 43 H13A 2 0.282184 0.088238 0.346945 11.00000 -1.20000 AFIX 0 C14 1 0.198640 -0.093835 0.325051 11.00000 0.02702 0.03166 = 0.02107 0.00166 0.00080 0.00377 AFIX 43 H14A 2 0.270660 -0.147934 0.322734 11.00000 -1.20000 AFIX 0 C15 1 0.085601 -0.153781 0.315045 11.00000 0.03516 0.02656 = 0.02475 -0.00254 -0.00259 -0.00181 AFIX 43 H15A 2 0.077973 -0.249453 0.305434 11.00000 -1.20000 AFIX 0 C16 1 -0.015658 -0.070542 0.319437 11.00000 0.02571 0.02898 = 0.03049 -0.00460 -0.00311 -0.00583 AFIX 43 H16A 2 -0.093482 -0.112474 0.314298 11.00000 -1.20000 AFIX 0 C21 1 0.104222 0.276947 0.345416 11.00000 0.02341 0.02648 = 0.01762 0.00078 -0.00298 -0.00291 AFIX 23 H21A 2 0.140881 0.315281 0.302470 11.00000 -1.20000 H21B 2 0.020278 0.313597 0.348878 11.00000 -1.20000 AFIX 0 N22 3 0.107288 0.380055 0.590011 11.00000 0.02529 0.02508 = 0.02001 0.00054 0.00367 -0.00161 C22 1 0.170258 0.327014 0.536781 11.00000 0.02264 0.01945 = 0.01815 0.00164 0.00165 -0.00422 C23 1 0.289614 0.281178 0.544049 11.00000 0.02522 0.02714 = 0.01976 -0.00097 0.00190 -0.00033 AFIX 43 H23A 2 0.332326 0.245523 0.505015 11.00000 -1.20000 AFIX 0 C24 1 0.344990 0.288450 0.609139 11.00000 0.02340 0.03705 = 0.02611 0.00237 -0.00153 0.00084 AFIX 43 H24A 2 0.426444 0.257372 0.615591 11.00000 -1.20000 AFIX 0 C25 1 0.280597 0.341426 0.664757 11.00000 0.03250 0.03242 = 0.01845 0.00079 -0.00286 -0.00543 AFIX 43 H25A 2 0.316215 0.346724 0.710188 11.00000 -1.20000 AFIX 0 C26 1 0.162982 0.386452 0.652412 11.00000 0.03244 0.02740 = 0.01751 -0.00126 0.00436 -0.00314 AFIX 43 H26A 2 0.119088 0.424180 0.690499 11.00000 -1.20000 HKLF 4 REM rtrr92 in P2(1)/c REM R1 = 0.0460 for 4082 Fo > 4sig(Fo) and 0.0566 for all 4928 data REM 262 parameters refined using 0 restraints END WGHT 0.0632 0.5623 REM Highest difference peak 0.365, deepest hole -0.228, 1-sigma level 0.048 Q1 1 0.3260 0.6446 0.0722 11.00000 0.05 0.36 Q2 1 0.3738 0.4687 0.3453 11.00000 0.05 0.32 Q3 1 0.1353 0.3188 0.5031 11.00000 0.05 0.32 Q4 1 0.2737 0.4825 0.3677 11.00000 0.05 0.31 Q5 1 0.1017 0.1972 0.3429 11.00000 0.05 0.31 Q6 1 0.1542 0.0929 0.3364 11.00000 0.05 0.29 Q7 1 0.3669 0.4117 0.3363 11.00000 0.05 0.28 Q8 1 0.2598 0.7383 0.0560 11.00000 0.05 0.28 Q9 1 0.2411 0.3351 0.5392 11.00000 0.05 0.28 Q10 1 0.0486 0.0916 0.3355 11.00000 0.05 0.27 ; _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^)+(0.0633P)^2^+0.5549P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4928 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0566 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.1221 _refine_ls_wR_factor_gt 0.1153 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.000 _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 N1 N 0.17541(9) 0.32294(11) 0.40633(5) 0.0201(2) Uani 1 1 d . . . C1 C 0.21946(12) 0.46450(13) 0.39540(6) 0.0224(3) Uani 1 1 d . . . H1A H 0.2571 0.4997 0.4392 0.027 Uiso 1 1 calc R . . H1B H 0.1500 0.5252 0.3829 0.027 Uiso 1 1 calc R . . C1OB C 0.19494(13) 0.57544(15) 0.01902(7) 0.0283(3) Uani 1 1 d . . . H1OA H 0.1461 0.6179 -0.0184 0.042 Uiso 1 1 calc R . . H1OB H 0.1421 0.5519 0.0583 0.042 Uiso 1 1 calc R . . H1OC H 0.2337 0.4916 0.0013 0.042 Uiso 1 1 calc R . . C1OA C 0.23501(13) 0.80963(14) 0.07030(7) 0.0264(3) Uani 1 1 d . . . H1OD H 0.1858 0.8512 0.0328 0.040 Uiso 1 1 calc R . . H1OE H 0.2991 0.8742 0.0849 0.040 Uiso 1 1 calc R . . H1OF H 0.1828 0.7887 0.1102 0.040 Uiso 1 1 calc R . . N2 N 0.27845(9) 0.52811(11) 0.27759(5) 0.0208(2) Uani 1 1 d . . . C2 C 0.31172(11) 0.46655(13) 0.33763(6) 0.0210(3) Uani 1 1 d . . . C3 C 0.42274(12) 0.40059(15) 0.34624(7) 0.0281(3) Uani 1 1 d . . . H3A H 0.4436 0.3573 0.3893 0.034 Uiso 1 1 calc R . . C4 C 0.50256(12) 0.39915(16) 0.29072(7) 0.0294(3) Uani 1 1 d . . . H4A H 0.5795 0.3550 0.2954 0.035 Uiso 1 1 calc R . . C5 C 0.47026(12) 0.46186(14) 0.22845(7) 0.0251(3) Uani 1 1 d . . . H5A H 0.5241 0.4624 0.1898 0.030 Uiso 1 1 calc R . . C6 C 0.35651(11) 0.52414(13) 0.22417(6) 0.0203(3) Uani 1 1 d . . . N7 N 0.30912(9) 0.58439(12) 0.16302(5) 0.0224(2) Uani 1 1 d . . . H7N H 0.2315 0.6074 0.1637 0.027 Uiso 1 1 calc R . . O8 O 0.47849(8) 0.58760(11) 0.09570(5) 0.0302(2) Uani 1 1 d . . . C8 C 0.37015(11) 0.61156(13) 0.10222(6) 0.0208(3) Uani 1 1 d . . . C9 C 0.29317(11) 0.67680(13) 0.04373(6) 0.0213(3) Uani 1 1 d . . . C10C C 0.37699(12) 0.71097(15) -0.01724(7) 0.0280(3) Uani 1 1 d . . . H10A H 0.3292 0.7529 -0.0552 0.042 Uiso 1 1 calc R . . H10B H 0.4154 0.6263 -0.0341 0.042 Uiso 1 1 calc R . . H10C H 0.4401 0.7756 -0.0015 0.042 Uiso 1 1 calc R . . C11 C 0.09998(11) 0.31472(14) 0.46890(6) 0.0226(3) Uani 1 1 d . . . H11A H 0.0560 0.2256 0.4685 0.027 Uiso 1 1 calc R . . H11B H 0.0382 0.3890 0.4669 0.027 Uiso 1 1 calc R . . C12 C 0.09873(11) 0.12271(14) 0.33933(6) 0.0211(3) Uani 1 1 d . . . N12 N -0.01165(10) 0.06561(12) 0.33047(6) 0.0243(2) Uani 1 1 d . . . C13 C 0.20555(12) 0.04551(14) 0.33844(6) 0.0241(3) Uani 1 1 d . . . H13A H 0.2822 0.0882 0.3469 0.029 Uiso 1 1 calc R . . C14 C 0.19864(12) -0.09383(15) 0.32505(7) 0.0266(3) Uani 1 1 d . . . H14A H 0.2707 -0.1479 0.3227 0.032 Uiso 1 1 calc R . . C15 C 0.08560(13) -0.15378(15) 0.31505(7) 0.0288(3) Uani 1 1 d . . . H15A H 0.0780 -0.2495 0.3054 0.035 Uiso 1 1 calc R . . C16 C -0.01566(12) -0.07054(15) 0.31944(7) 0.0284(3) Uani 1 1 d . . . H16A H -0.0935 -0.1125 0.3143 0.034 Uiso 1 1 calc R . . C21 C 0.10422(11) 0.27695(14) 0.34542(6) 0.0225(3) Uani 1 1 d . . . H21A H 0.1409 0.3153 0.3025 0.027 Uiso 1 1 calc R . . H21B H 0.0203 0.3136 0.3489 0.027 Uiso 1 1 calc R . . N22 N 0.10729(10) 0.38006(12) 0.59001(6) 0.0234(2) Uani 1 1 d . . . C22 C 0.17026(11) 0.32701(13) 0.53678(6) 0.0201(3) Uani 1 1 d . . . C23 C 0.28961(12) 0.28118(14) 0.54405(7) 0.0240(3) Uani 1 1 d . . . H23A H 0.3323 0.2455 0.5050 0.029 Uiso 1 1 calc R . . C24 C 0.34499(12) 0.28845(16) 0.60914(7) 0.0289(3) Uani 1 1 d . . . H24A H 0.4264 0.2574 0.6156 0.035 Uiso 1 1 calc R . . C25 C 0.28060(13) 0.34143(15) 0.66476(7) 0.0278(3) Uani 1 1 d . . . H25A H 0.3162 0.3467 0.7102 0.033 Uiso 1 1 calc R . . C26 C 0.16298(12) 0.38645(14) 0.65241(7) 0.0258(3) Uani 1 1 d . . . H26A H 0.1191 0.4242 0.6905 0.031 Uiso 1 1 calc R . . 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 N1 0.0218(5) 0.0235(5) 0.0149(5) -0.0005(4) 0.0002(4) -0.0046(4) C1 0.0264(6) 0.0216(6) 0.0192(6) -0.0005(5) 0.0011(5) -0.0026(5) C1OB 0.0303(7) 0.0320(7) 0.0225(6) 0.0006(5) -0.0025(5) -0.0026(6) C1OA 0.0288(7) 0.0250(7) 0.0254(7) 0.0024(5) 0.0024(5) 0.0054(5) N2 0.0223(5) 0.0208(5) 0.0195(5) 0.0006(4) 0.0005(4) -0.0019(4) C2 0.0236(6) 0.0206(6) 0.0187(6) 0.0002(5) -0.0014(5) -0.0058(5) C3 0.0255(7) 0.0354(8) 0.0233(7) 0.0082(5) -0.0043(5) -0.0008(6) C4 0.0204(6) 0.0382(8) 0.0296(7) 0.0077(6) -0.0025(5) 0.0029(6) C5 0.0202(6) 0.0315(7) 0.0234(6) 0.0039(5) 0.0008(5) -0.0007(5) C6 0.0203(6) 0.0209(6) 0.0195(6) 0.0011(5) -0.0015(4) -0.0033(5) N7 0.0179(5) 0.0291(6) 0.0201(5) 0.0043(4) 0.0006(4) 0.0034(4) O8 0.0220(5) 0.0415(6) 0.0272(5) 0.0068(4) 0.0036(4) 0.0061(4) C8 0.0220(6) 0.0207(6) 0.0196(6) -0.0004(5) 0.0012(5) 0.0002(5) C9 0.0217(6) 0.0238(6) 0.0183(6) 0.0019(5) 0.0016(5) 0.0022(5) C10C 0.0283(7) 0.0353(8) 0.0204(6) 0.0046(5) 0.0040(5) 0.0037(6) C11 0.0204(6) 0.0292(7) 0.0183(6) -0.0001(5) 0.0012(5) -0.0029(5) C12 0.0238(6) 0.0275(7) 0.0121(5) -0.0006(5) -0.0003(4) -0.0034(5) N12 0.0222(5) 0.0289(6) 0.0220(5) -0.0037(4) -0.0011(4) -0.0036(4) C13 0.0214(6) 0.0319(7) 0.0190(6) 0.0020(5) -0.0010(5) -0.0030(5) C14 0.0270(7) 0.0317(7) 0.0211(6) 0.0017(5) 0.0008(5) 0.0038(5) C15 0.0352(7) 0.0266(7) 0.0247(7) -0.0025(5) -0.0026(5) -0.0018(6) C16 0.0257(7) 0.0290(7) 0.0305(7) -0.0046(6) -0.0031(5) -0.0058(5) C21 0.0234(6) 0.0265(7) 0.0176(6) 0.0008(5) -0.0030(5) -0.0029(5) N22 0.0253(6) 0.0251(6) 0.0200(5) 0.0005(4) 0.0037(4) -0.0016(4) C22 0.0226(6) 0.0194(6) 0.0181(6) 0.0016(4) 0.0016(4) -0.0042(5) C23 0.0252(6) 0.0271(7) 0.0198(6) -0.0010(5) 0.0019(5) -0.0003(5) C24 0.0234(6) 0.0370(8) 0.0261(7) 0.0024(6) -0.0015(5) 0.0008(6) C25 0.0325(7) 0.0324(7) 0.0185(6) 0.0008(5) -0.0029(5) -0.0054(6) C26 0.0324(7) 0.0274(7) 0.0175(6) -0.0013(5) 0.0044(5) -0.0031(5) _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 N1 C11 1.4630(15) . ? N1 C21 1.4651(15) . ? N1 C1 1.4719(16) . ? C1 C2 1.5051(17) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C1OB C9 1.5304(19) . ? C1OB H1OA 0.9800 . ? C1OB H1OB 0.9800 . ? C1OB H1OC 0.9800 . ? C1OA C9 1.5275(18) . ? C1OA H1OD 0.9800 . ? C1OA H1OE 0.9800 . ? C1OA H1OF 0.9800 . ? N2 C6 1.3392(16) . ? N2 C2 1.3411(16) . ? C2 C3 1.3842(19) . ? C3 C4 1.3823(19) . ? C3 H3A 0.9500 . ? C4 C5 1.3798(19) . ? C4 H4A 0.9500 . ? C5 C6 1.3883(18) . ? C5 H5A 0.9500 . ? C6 N7 1.4021(16) . ? N7 C8 1.3722(16) . ? N7 H7N 0.8800 . ? O8 C8 1.2185(15) . ? C8 C9 1.5315(17) . ? C9 C10C 1.5276(17) . ? C10C H10A 0.9800 . ? C10C H10B 0.9800 . ? C10C H10C 0.9800 . ? C11 C22 1.5073(17) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N12 1.3409(16) . ? C12 C13 1.3911(18) . ? C12 C21 1.5025(18) . ? N12 C16 1.3388(18) . ? C13 C14 1.378(2) . ? C13 H13A 0.9500 . ? C14 C15 1.3814(19) . ? C14 H14A 0.9500 . ? C15 C16 1.377(2) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? N22 C26 1.3361(17) . ? N22 C22 1.3381(16) . ? C22 C23 1.3886(18) . ? C23 C24 1.3808(18) . ? C23 H23A 0.9500 . ? C24 C25 1.3812(19) . ? C24 H24A 0.9500 . ? C25 C26 1.380(2) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? 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 C11 N1 C21 109.36(9) . . ? C11 N1 C1 110.85(10) . . ? C21 N1 C1 110.17(10) . . ? N1 C1 C2 109.90(10) . . ? N1 C1 H1A 109.7 . . ? C2 C1 H1A 109.7 . . ? N1 C1 H1B 109.7 . . ? C2 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? C9 C1OB H1OA 109.5 . . ? C9 C1OB H1OB 109.5 . . ? H1OA C1OB H1OB 109.5 . . ? C9 C1OB H1OC 109.5 . . ? H1OA C1OB H1OC 109.5 . . ? H1OB C1OB H1OC 109.5 . . ? C9 C1OA H1OD 109.5 . . ? C9 C1OA H1OE 109.5 . . ? H1OD C1OA H1OE 109.5 . . ? C9 C1OA H1OF 109.5 . . ? H1OD C1OA H1OF 109.5 . . ? H1OE C1OA H1OF 109.5 . . ? C6 N2 C2 117.94(11) . . ? N2 C2 C3 122.65(11) . . ? N2 C2 C1 117.00(11) . . ? C3 C2 C1 120.25(11) . . ? C4 C3 C2 118.46(12) . . ? C4 C3 H3A 120.8 . . ? C2 C3 H3A 120.8 . . ? C5 C4 C3 119.88(12) . . ? C5 C4 H4A 120.1 . . ? C3 C4 H4A 120.1 . . ? C4 C5 C6 117.78(12) . . ? C4 C5 H5A 121.1 . . ? C6 C5 H5A 121.1 . . ? N2 C6 C5 123.27(11) . . ? N2 C6 N7 112.87(11) . . ? C5 C6 N7 123.81(11) . . ? C8 N7 C6 127.29(10) . . ? C8 N7 H7N 116.4 . . ? C6 N7 H7N 116.4 . . ? O8 C8 N7 122.30(12) . . ? O8 C8 C9 122.39(11) . . ? N7 C8 C9 115.30(10) . . ? C1OA C9 C10C 109.08(11) . . ? C1OA C9 C1OB 110.48(11) . . ? C10C C9 C1OB 109.36(11) . . ? C1OA C9 C8 109.60(10) . . ? C10C C9 C8 108.34(10) . . ? C1OB C9 C8 109.95(11) . . ? C9 C10C H10A 109.5 . . ? C9 C10C H10B 109.5 . . ? H10A C10C H10B 109.5 . . ? C9 C10C H10C 109.5 . . ? H10A C10C H10C 109.5 . . ? H10B C10C H10C 109.5 . . ? N1 C11 C22 114.24(10) . . ? N1 C11 H11A 108.7 . . ? C22 C11 H11A 108.7 . . ? N1 C11 H11B 108.7 . . ? C22 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? N12 C12 C13 122.39(12) . . ? N12 C12 C21 117.19(11) . . ? C13 C12 C21 120.29(11) . . ? C16 N12 C12 117.13(12) . . ? C14 C13 C12 119.07(12) . . ? C14 C13 H13A 120.5 . . ? C12 C13 H13A 120.5 . . ? C13 C14 C15 119.12(13) . . ? C13 C14 H14A 120.4 . . ? C15 C14 H14A 120.4 . . ? C16 C15 C14 117.92(13) . . ? C16 C15 H15A 121.0 . . ? C14 C15 H15A 121.0 . . ? N12 C16 C15 124.30(13) . . ? N12 C16 H16A 117.9 . . ? C15 C16 H16A 117.9 . . ? N1 C21 C12 112.69(10) . . ? N1 C21 H21A 109.1 . . ? C12 C21 H21A 109.1 . . ? N1 C21 H21B 109.1 . . ? C12 C21 H21B 109.1 . . ? H21A C21 H21B 107.8 . . ? C26 N22 C22 117.48(11) . . ? N22 C22 C23 122.71(11) . . ? N22 C22 C11 114.91(11) . . ? C23 C22 C11 122.32(11) . . ? C24 C23 C22 118.68(12) . . ? C24 C23 H23A 120.7 . . ? C22 C23 H23A 120.7 . . ? C23 C24 C25 119.24(13) . . ? C23 C24 H24A 120.4 . . ? C25 C24 H24A 120.4 . . ? C26 C25 C24 118.07(12) . . ? C26 C25 H25A 121.0 . . ? C24 C25 H25A 121.0 . . ? N22 C26 C25 123.81(12) . . ? N22 C26 H26A 118.1 . . ? C25 C26 H26A 118.1 . . ? _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 28.92 _diffrn_measured_fraction_theta_full 0.920 _refine_diff_density_max 0.365 _refine_diff_density_min -0.228 _refine_diff_density_rms 0.048 #===END data_znrr26 _database_code_CSD 203673 #Compound 1 in manuscript. #Note to referee: checkcif output & final res file in refine special details _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [Zn(L1)][PF6}2.0.5MeOH _chemical_formula_sum 'C23.50 H29 F12 N5 O1.50 P2 Zn' _chemical_formula_weight 760.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 '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 _symmetry_space_group_name_Hall '-P 2ybc' 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 14.424(2) _cell_length_b 11.3946(19) _cell_length_c 19.420(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.072(11) _cell_angle_gamma 90.00 _cell_volume 3067.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 62 _cell_measurement_theta_min 25 _cell_measurement_theta_max 27.5 _exptl_crystal_description lath _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.648 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1540 _exptl_absorpt_coefficient_mu 3.062 _exptl_absorpt_correction_type Integration _exptl_absorpt_correction_T_min 0.373 _exptl_absorpt_correction_T_max 0.707 _exptl_absorpt_process_details ; A numerical correction was applied by Gaussian integration following refinement of the crystal face indices and dimensions against a set of psi-scans (Stoe X-Shape). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe Stadi-4 diffractometer' _diffrn_measurement_method 0mega-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _diffrn_reflns_number 7387 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_sigmaI/netI 0.0287 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 70.09 _reflns_number_total 5451 _reflns_number_gt 4514 _reflns_threshold_expression >2sigma(I) _computing_data_collection DIF4 _computing_cell_refinement DIF4 _computing_data_reduction REDU4 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; 028_ALERT A -diffrn-measured-fraction-theta-max low ..... 0.94 022_ALERT C Ratio Unique / Expected Reflections too Low .. 0.94 029_ALERT C -diffrn-measured-fraction-theta-full low ..... 0.94 Data were collected with Cu-Ka radiation on a four circle. Some high angle reflections were inaccessible. 761_ALERT A CIF Contains no X-H Bonds .................... ? 762_ALERT A CIF Contains no X-Y-H or H-Y-H Angles ........ ? All H-atoms positions were idealised. 041_ALERT C Calc. and Rep. SumFormula Strings Differ .. ? 042_ALERT C Calc. and Rep. MoietyFormula Strings Differ .. ? 043_ALERT C Check Reported Molecular Weight .............. 760.83 044_ALERT C Calculated and Reported Dx Differ ............ ? 068_ALERT C Reported F000 Differs from Calcd (or Missing). ? 601_ALERT C Structure Contains Solvent Accessible VOIDS of 81.00 A**3 The van der Sluis-Spek method was used to treat the highly disordered solvent of crystallisation. The correction comprised 37 e/cell, which can be interpreted as 0.5 MeOH per formula unit. This was included in the calculation of Dx, F(000) etc. 070_ALERT C Duplicate or Troublesome Atomic Label on input H10K Corrected. 125_ALERT C No _symmetry_space_group_name_Hall given ..... ? Corrected. 244_ALERT C Low Solvent U(eq) as Compared to Neighbors ... P1 PF6- anions generally librate, so that the fluorine Uij's are larger than the P Uij's. 414_ALERT C Short Intra D-H..H-X H7N .. H10K = 1.92 Ang. 420_ALERT C D-H Without Acceptor N7 - H7N ? 432_ALERT C Short Inter X...Y Contact: F12 .. C8 = 2.88 Ang. See text. 790_ALERT C Centre of Gravity not Within Unit Cell: Resd.# 2 F6 P 790_ALERT C Centre of Gravity not Within Unit Cell: Resd.# 3 F6 P No action. Final shelx res file: #TITL znrr26 in P2(1)/c. sQUEEZE CORRECTION 37E/CELL=0.5MEOH/FORM UNIT. CELL 1.54178 14.4236 11.3946 19.4202 90.000 106.072 90.000 ZERR 4.00 0.0022 0.0019 0.0023 0.000 0.011 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O ZN F P UNIT 94 116 20 6 4 48 8 TEMP -123 L.S. 6 ACTA HTAB FMAP 2 PLAN 10 WGHT 0.037800 1.196900 EXTI 0.000231 FVAR 3.56562 ZN 5 0.273728 0.779210 0.056260 11.00000 0.02126 0.01477 = 0.02263 -0.00188 0.00333 0.00222 N1 3 0.351394 0.623966 0.037972 11.00000 0.02290 0.01661 = 0.01911 -0.00324 0.00128 0.00202 C1 1 0.433890 0.665661 0.014642 11.00000 0.03057 0.01991 = 0.02978 -0.00684 0.01249 0.00061 AFIX 23 H1B 2 0.413866 0.676167 -0.038019 11.00000 -1.20000 H1A 2 0.485572 0.605718 0.026405 11.00000 -1.20000 AFIX 0 C1OB 1 0.188132 1.196719 0.104646 11.00000 0.06268 0.03141 = 0.03412 0.00113 0.01022 0.02409 AFIX 33 H10F 2 0.237451 1.237826 0.087845 11.00000 -1.50000 H10E 2 0.154218 1.253044 0.127143 11.00000 -1.50000 H10D 2 0.141927 1.159270 0.063900 11.00000 -1.50000 AFIX 0 C2 1 0.473156 0.780649 0.049984 11.00000 0.02629 0.01998 = 0.02171 -0.00098 0.00767 0.00457 N2 3 0.409050 0.850033 0.070413 11.00000 0.02413 0.01542 = 0.02161 -0.00301 0.00632 0.00077 C3 1 0.567006 0.813951 0.057690 11.00000 0.02567 0.02686 = 0.04160 -0.00646 0.01278 0.00287 AFIX 43 H3A 2 0.610624 0.763353 0.043365 11.00000 -1.20000 AFIX 0 C4 1 0.596598 0.923968 0.087090 11.00000 0.02520 0.03142 = 0.05007 -0.00753 0.01256 -0.00278 AFIX 43 H4 2 0.660872 0.949718 0.092524 11.00000 -1.20000 AFIX 0 C5 1 0.532593 0.994851 0.108127 11.00000 0.02815 0.02110 = 0.04262 -0.01029 0.01016 -0.00476 AFIX 43 H5 2 0.551725 1.070016 0.128233 11.00000 -1.20000 AFIX 0 C6 1 0.439014 0.954351 0.099403 11.00000 0.02434 0.01864 = 0.02405 -0.00115 0.00689 0.00232 N7 3 0.376023 1.025937 0.124386 11.00000 0.02669 0.01570 = 0.03098 -0.00810 0.01017 -0.00158 AFIX 43 H7N 2 0.402588 1.090005 0.146606 11.00000 -1.20000 AFIX 0 O8 4 0.230269 0.934051 0.084679 11.00000 0.02393 0.01705 = 0.03053 -0.00279 0.00528 0.00320 C8 1 0.281202 1.012977 0.120043 11.00000 0.02654 0.01530 = 0.02243 0.00258 0.00638 0.00452 C9 1 0.236306 1.102904 0.159466 11.00000 0.02915 0.02140 = 0.02719 0.00052 0.00984 0.00824 C10C 1 0.310389 1.159237 0.222974 11.00000 0.03944 0.02340 = 0.03131 -0.00656 0.01337 0.00483 AFIX 33 H10J 2 0.359104 1.200758 0.205709 11.00000 -1.50000 H10K 2 0.341709 1.098088 0.256975 11.00000 -1.50000 H10L 2 0.277762 1.214914 0.246877 11.00000 -1.50000 AFIX 0 C10A 1 0.159750 1.038803 0.187164 11.00000 0.03587 0.03701 = 0.05084 -0.00867 0.02322 0.00223 AFIX 33 H10C 2 0.111819 1.002924 0.146761 11.00000 -1.50000 H10B 2 0.127775 1.095076 0.211177 11.00000 -1.50000 H10A 2 0.190933 0.977612 0.221184 11.00000 -1.50000 AFIX 0 C11 1 0.281892 0.555627 -0.017393 11.00000 0.03268 0.01727 = 0.02305 -0.00473 0.00188 0.00045 AFIX 23 H11B 2 0.247281 0.500234 0.006024 11.00000 -1.20000 H11A 2 0.317278 0.509053 -0.044963 11.00000 -1.20000 AFIX 0 N12 3 0.194878 0.741385 -0.044742 11.00000 0.02599 0.02519 = 0.02367 0.00002 0.00199 0.00237 C12 1 0.209415 0.633752 -0.068190 11.00000 0.02485 0.02631 = 0.02283 -0.00149 0.00411 -0.00045 C13 1 0.156872 0.593564 -0.134854 11.00000 0.03723 0.03813 = 0.02548 -0.00783 0.00201 -0.00333 AFIX 43 H13A 2 0.168716 0.517763 -0.150951 11.00000 -1.20000 AFIX 0 C14 1 0.087430 0.664714 -0.177382 11.00000 0.03829 0.06221 = 0.02639 -0.00275 -0.00345 -0.00014 AFIX 43 H14 2 0.049897 0.638015 -0.222915 11.00000 -1.20000 AFIX 0 C15 1 0.072537 0.775419 -0.153473 11.00000 0.03305 0.05971 = 0.02900 0.00835 -0.00336 0.01115 AFIX 43 H15 2 0.024898 0.825766 -0.182359 11.00000 -1.20000 AFIX 0 C16 1 0.127707 0.811701 -0.087212 11.00000 0.03230 0.03564 = 0.03071 0.00743 0.00512 0.01023 AFIX 43 H16 2 0.118239 0.888233 -0.070968 11.00000 -1.20000 AFIX 0 C21 1 0.378869 0.564837 0.108068 11.00000 0.02567 0.01718 = 0.02172 0.00009 0.00267 0.00431 AFIX 23 H21B 2 0.437114 0.602688 0.139474 11.00000 -1.20000 H21A 2 0.394403 0.481606 0.101722 11.00000 -1.20000 AFIX 0 N22 3 0.240106 0.666829 0.126632 11.00000 0.02405 0.01976 = 0.02426 -0.00233 0.00624 0.00096 C22 1 0.297267 0.571650 0.142763 11.00000 0.02439 0.01623 = 0.02254 -0.00307 0.00069 -0.00038 C23 1 0.283105 0.486790 0.189437 11.00000 0.03712 0.02200 = 0.03577 0.00497 0.00895 0.00362 AFIX 43 H23A 2 0.325137 0.421114 0.200940 11.00000 -1.20000 AFIX 0 C24 1 0.207040 0.498417 0.219283 11.00000 0.05252 0.03496 = 0.04731 0.00740 0.02378 -0.00388 AFIX 43 H24A 2 0.196307 0.441032 0.251726 11.00000 -1.20000 AFIX 0 C25 1 0.146932 0.594325 0.201389 11.00000 0.04050 0.03871 = 0.05151 -0.00125 0.02642 -0.00288 AFIX 43 H25A 2 0.093294 0.603061 0.220382 11.00000 -1.20000 AFIX 0 C26 1 0.165943 0.677442 0.155438 11.00000 0.02986 0.02635 = 0.04202 -0.00289 0.01456 0.00238 AFIX 43 H26A 2 0.125263 0.744313 0.143808 11.00000 -1.20000 AFIX 0 P1 7 -0.126927 0.702845 -0.385175 11.00000 0.02838 0.03263 = 0.02382 0.00081 0.00478 -0.00322 F1 6 -0.191610 0.613164 -0.441218 11.00000 0.04190 0.04469 = 0.03668 -0.01120 0.01128 -0.01309 F2 6 -0.045837 0.693651 -0.425576 11.00000 0.04105 0.12654 = 0.05326 -0.02160 0.02367 -0.02802 F3 6 -0.078625 0.594732 -0.335210 11.00000 0.07971 0.05636 = 0.04448 0.00752 -0.00020 0.02395 F4 6 -0.061784 0.790700 -0.327877 11.00000 0.06320 0.06708 = 0.04227 -0.01545 0.00026 -0.02807 F5 6 -0.207434 0.709009 -0.343819 11.00000 0.04757 0.08634 = 0.04857 -0.02018 0.02422 -0.00344 F6 6 -0.175154 0.808106 -0.434323 11.00000 0.12016 0.03705 = 0.04977 0.01266 -0.00735 0.01178 P11 7 0.572355 1.317478 0.196718 11.00000 0.02486 0.01942 = 0.02193 -0.00106 0.00185 0.00054 F11 6 0.502409 1.392498 0.230664 11.00000 0.03988 0.03983 = 0.03182 -0.00577 0.01001 0.01069 F12 6 0.661366 1.348702 0.263326 11.00000 0.03469 0.03706 = 0.03430 -0.00705 -0.00895 0.00141 F13 6 0.550295 1.201970 0.236532 11.00000 0.04285 0.02903 = 0.03830 0.01224 0.00793 -0.00022 F14 6 0.592056 1.431409 0.154476 11.00000 0.04563 0.02166 = 0.03778 0.00159 0.01032 -0.00448 F15 6 0.641399 1.242554 0.161784 11.00000 0.03124 0.02858 = 0.04432 -0.00734 0.01150 0.00172 F16 6 0.481697 1.284793 0.129200 11.00000 0.02890 0.02937 = 0.02900 -0.00435 -0.00303 -0.00169 HKLF 4 REM znrr26 in P2(1)/c. sQUEEZE CORRECTION 37E/CELL=0.5MEOH/FORM UNIT. REM R1 = 0.0318 for 4514 Fo > 4sig(Fo) and 0.0419 for all 5451 data REM 398 parameters refined using 0 restraints END WGHT 0.0374 1.2218 REM Highest difference peak 0.423, deepest hole -0.327, 1-sigma level 0.052 Q1 1 -0.0819 0.7696 -0.4340 11.00000 0.05 0.42 Q2 1 -0.2171 0.7875 -0.3786 11.00000 0.05 0.35 Q3 1 -0.0402 0.6427 -0.3557 11.00000 0.05 0.30 Q4 1 -0.1413 0.6375 -0.3308 11.00000 0.05 0.28 Q5 1 -0.2243 0.6813 -0.4531 11.00000 0.05 0.26 Q6 1 0.2578 1.0600 0.1423 11.00000 0.05 0.26 Q7 1 0.2152 1.1398 0.1281 11.00000 0.05 0.25 Q8 1 0.2719 0.7680 -0.0104 11.00000 0.05 0.24 Q9 1 0.2630 0.7911 0.1155 11.00000 0.05 0.24 Q10 1 0.3324 0.6758 0.0582 11.00000 0.05 0.23 ; _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^)+(0.0378P)^2^+1.1969P] 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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00023(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5451 _refine_ls_number_parameters 398 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_ref 0.0770 _refine_ls_wR_factor_gt 0.0739 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.000 _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 0.27373(2) 0.77921(3) 0.056260(15) 0.02010(9) Uani 1 1 d . . . N1 N 0.35139(12) 0.62397(16) 0.03797(9) 0.0204(4) Uani 1 1 d . . . C1 C 0.43389(16) 0.6657(2) 0.01464(13) 0.0259(5) Uani 1 1 d . . . H1B H 0.4139 0.6762 -0.0380 0.031 Uiso 1 1 calc R . . H1A H 0.4856 0.6057 0.0264 0.031 Uiso 1 1 calc R . . C1OB C 0.1881(2) 1.1967(2) 0.10465(15) 0.0434(7) Uani 1 1 d . . . H10F H 0.2375 1.2378 0.0878 0.065 Uiso 1 1 calc R . . H10E H 0.1542 1.2530 0.1271 0.065 Uiso 1 1 calc R . . H10D H 0.1419 1.1593 0.0639 0.065 Uiso 1 1 calc R . . C2 C 0.47316(15) 0.7806(2) 0.04998(11) 0.0225(5) Uani 1 1 d . . . N2 N 0.40905(12) 0.85003(16) 0.07041(9) 0.0204(4) Uani 1 1 d . . . C3 C 0.56701(17) 0.8140(2) 0.05769(14) 0.0307(6) Uani 1 1 d . . . H3A H 0.6106 0.7634 0.0434 0.037 Uiso 1 1 calc R . . C4 C 0.59660(17) 0.9240(2) 0.08709(15) 0.0351(6) Uani 1 1 d . . . H4 H 0.6609 0.9497 0.0925 0.042 Uiso 1 1 calc R . . C5 C 0.53259(16) 0.9949(2) 0.10813(14) 0.0305(6) Uani 1 1 d . . . H5 H 0.5517 1.0700 0.1282 0.037 Uiso 1 1 calc R . . C6 C 0.43901(15) 0.9544(2) 0.09940(12) 0.0223(5) Uani 1 1 d . . . N7 N 0.37602(13) 1.02594(17) 0.12439(10) 0.0240(4) Uani 1 1 d . . . H7N H 0.4026 1.0900 0.1466 0.029 Uiso 1 1 calc R . . O8 O 0.23027(11) 0.93405(14) 0.08468(8) 0.0243(3) Uani 1 1 d . . . C8 C 0.28120(15) 1.0130(2) 0.12004(11) 0.0215(5) Uani 1 1 d . . . C9 C 0.23631(16) 1.1029(2) 0.15947(12) 0.0255(5) Uani 1 1 d . . . C10C C 0.31039(18) 1.1592(2) 0.22297(13) 0.0307(5) Uani 1 1 d . . . H10J H 0.3591 1.2008 0.2057 0.046 Uiso 1 1 calc R . . H10K H 0.3417 1.0981 0.2570 0.046 Uiso 1 1 calc R . . H10L H 0.2778 1.2149 0.2469 0.046 Uiso 1 1 calc R . . C10A C 0.15975(18) 1.0388(3) 0.18716(15) 0.0390(7) Uani 1 1 d . . . H10C H 0.1118 1.0029 0.1468 0.059 Uiso 1 1 calc R . . H10B H 0.1278 1.0951 0.2112 0.059 Uiso 1 1 calc R . . H10A H 0.1909 0.9776 0.2212 0.059 Uiso 1 1 calc R . . C11 C 0.28189(16) 0.5556(2) -0.01739(12) 0.0255(5) Uani 1 1 d . . . H11B H 0.2473 0.5002 0.0060 0.031 Uiso 1 1 calc R . . H11A H 0.3173 0.5091 -0.0450 0.031 Uiso 1 1 calc R . . N12 N 0.19488(13) 0.74138(18) -0.04474(10) 0.0259(4) Uani 1 1 d . . . C12 C 0.20942(16) 0.6338(2) -0.06819(12) 0.0252(5) Uani 1 1 d . . . C13 C 0.15687(18) 0.5936(3) -0.13485(13) 0.0349(6) Uani 1 1 d . . . H13A H 0.1687 0.5178 -0.1510 0.042 Uiso 1 1 calc R . . C14 C 0.0874(2) 0.6647(3) -0.17738(14) 0.0448(7) Uani 1 1 d . . . H14 H 0.0499 0.6380 -0.2229 0.054 Uiso 1 1 calc R . . C15 C 0.07254(19) 0.7754(3) -0.15347(14) 0.0430(7) Uani 1 1 d . . . H15 H 0.0249 0.8258 -0.1824 0.052 Uiso 1 1 calc R . . C16 C 0.12771(17) 0.8117(2) -0.08721(13) 0.0336(6) Uani 1 1 d . . . H16 H 0.1182 0.8882 -0.0710 0.040 Uiso 1 1 calc R . . C21 C 0.37887(15) 0.5648(2) 0.10807(11) 0.0223(5) Uani 1 1 d . . . H21B H 0.4371 0.6027 0.1395 0.027 Uiso 1 1 calc R . . H21A H 0.3944 0.4816 0.1017 0.027 Uiso 1 1 calc R . . N22 N 0.24011(13) 0.66683(17) 0.12663(10) 0.0228(4) Uani 1 1 d . . . C22 C 0.29727(15) 0.5716(2) 0.14276(12) 0.0222(5) Uani 1 1 d . . . C23 C 0.28310(18) 0.4868(2) 0.18944(13) 0.0319(6) Uani 1 1 d . . . H23A H 0.3251 0.4211 0.2009 0.038 Uiso 1 1 calc R . . C24 C 0.2070(2) 0.4984(3) 0.21928(16) 0.0429(7) Uani 1 1 d . . . H24A H 0.1963 0.4410 0.2517 0.052 Uiso 1 1 calc R . . C25 C 0.14693(19) 0.5943(3) 0.20139(15) 0.0408(7) Uani 1 1 d . . . H25A H 0.0933 0.6031 0.2204 0.049 Uiso 1 1 calc R . . C26 C 0.16594(17) 0.6774(2) 0.15544(14) 0.0318(6) Uani 1 1 d . . . H26A H 0.1253 0.7443 0.1438 0.038 Uiso 1 1 calc R . . P1 P -0.12693(4) 0.70284(6) -0.38518(3) 0.02876(15) Uani 1 1 d . . . F1 F -0.19161(11) 0.61316(14) -0.44122(8) 0.0410(4) Uani 1 1 d . . . F2 F -0.04584(12) 0.6937(2) -0.42558(10) 0.0715(7) Uani 1 1 d . . . F3 F -0.07863(14) 0.59473(17) -0.33521(10) 0.0637(5) Uani 1 1 d . . . F4 F -0.06178(13) 0.79070(17) -0.32788(9) 0.0604(5) Uani 1 1 d . . . F5 F -0.20743(12) 0.70901(18) -0.34382(9) 0.0586(5) Uani 1 1 d . . . F6 F -0.17515(18) 0.80811(16) -0.43432(10) 0.0752(7) Uani 1 1 d . . . P11 P 0.57235(4) 1.31748(5) 0.19672(3) 0.02299(14) Uani 1 1 d . . . F11 F 0.50241(10) 1.39250(14) 0.23066(7) 0.0372(4) Uani 1 1 d . . . F12 F 0.66137(10) 1.34870(14) 0.26333(8) 0.0390(4) Uani 1 1 d . . . F13 F 0.55030(11) 1.20197(13) 0.23653(8) 0.0374(4) Uani 1 1 d . . . F14 F 0.59206(10) 1.43141(12) 0.15448(8) 0.0353(3) Uani 1 1 d . . . F15 F 0.64140(10) 1.24255(13) 0.16178(8) 0.0345(3) Uani 1 1 d . . . F16 F 0.48170(9) 1.28479(13) 0.12920(7) 0.0313(3) 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 0.02126(14) 0.01477(17) 0.02263(15) -0.00188(13) 0.00333(11) 0.00222(12) N1 0.0229(9) 0.0166(10) 0.0191(9) -0.0032(8) 0.0013(7) 0.0020(8) C1 0.0306(12) 0.0199(13) 0.0298(12) -0.0068(10) 0.0125(10) 0.0006(10) C1OB 0.0627(18) 0.0314(17) 0.0341(14) 0.0011(12) 0.0102(13) 0.0241(14) C2 0.0263(11) 0.0200(12) 0.0217(10) -0.0010(9) 0.0077(9) 0.0046(9) N2 0.0241(9) 0.0154(10) 0.0216(9) -0.0030(8) 0.0063(7) 0.0008(7) C3 0.0257(12) 0.0269(14) 0.0416(14) -0.0065(11) 0.0128(11) 0.0029(10) C4 0.0252(12) 0.0314(15) 0.0501(16) -0.0075(13) 0.0126(11) -0.0028(11) C5 0.0281(12) 0.0211(14) 0.0426(14) -0.0103(11) 0.0102(11) -0.0048(10) C6 0.0243(11) 0.0186(13) 0.0240(11) -0.0011(9) 0.0069(9) 0.0023(9) N7 0.0267(9) 0.0157(10) 0.0310(10) -0.0081(8) 0.0102(8) -0.0016(8) O8 0.0239(8) 0.0170(9) 0.0305(8) -0.0028(7) 0.0053(6) 0.0032(7) C8 0.0265(11) 0.0153(12) 0.0224(10) 0.0026(9) 0.0064(9) 0.0045(9) C9 0.0291(12) 0.0214(13) 0.0272(11) 0.0005(10) 0.0098(9) 0.0082(10) C10C 0.0394(13) 0.0234(14) 0.0313(13) -0.0066(11) 0.0134(11) 0.0048(11) C10A 0.0359(14) 0.0370(17) 0.0508(16) -0.0087(13) 0.0232(13) 0.0022(12) C11 0.0327(12) 0.0173(13) 0.0230(11) -0.0047(9) 0.0019(9) 0.0004(10) N12 0.0260(9) 0.0252(12) 0.0237(9) 0.0000(8) 0.0020(8) 0.0024(8) C12 0.0248(11) 0.0263(14) 0.0228(11) -0.0015(10) 0.0041(9) -0.0004(9) C13 0.0372(13) 0.0381(16) 0.0255(12) -0.0078(12) 0.0020(10) -0.0033(12) C14 0.0383(15) 0.062(2) 0.0264(13) -0.0027(14) -0.0034(11) -0.0001(14) C15 0.0330(13) 0.060(2) 0.0290(13) 0.0084(14) -0.0034(11) 0.0111(14) C16 0.0323(13) 0.0356(16) 0.0307(13) 0.0074(11) 0.0051(10) 0.0102(11) C21 0.0257(11) 0.0172(12) 0.0217(11) 0.0001(9) 0.0027(9) 0.0043(9) N22 0.0240(9) 0.0198(11) 0.0243(9) -0.0023(8) 0.0062(8) 0.0010(8) C22 0.0244(11) 0.0162(12) 0.0225(11) -0.0031(9) 0.0007(9) -0.0004(9) C23 0.0371(13) 0.0220(14) 0.0358(13) 0.0050(11) 0.0089(11) 0.0036(11) C24 0.0525(17) 0.0350(17) 0.0473(16) 0.0074(13) 0.0238(14) -0.0039(13) C25 0.0405(14) 0.0387(17) 0.0515(16) -0.0013(14) 0.0264(13) -0.0029(12) C26 0.0299(12) 0.0263(15) 0.0420(14) -0.0029(11) 0.0146(11) 0.0024(10) P1 0.0284(3) 0.0326(4) 0.0238(3) 0.0008(3) 0.0048(2) -0.0032(3) F1 0.0419(8) 0.0447(10) 0.0367(8) -0.0112(7) 0.0113(7) -0.0131(7) F2 0.0410(9) 0.127(2) 0.0533(11) -0.0216(12) 0.0237(9) -0.0280(11) F3 0.0797(13) 0.0564(12) 0.0445(10) 0.0075(9) -0.0002(9) 0.0240(10) F4 0.0632(11) 0.0671(13) 0.0423(10) -0.0154(9) 0.0003(8) -0.0281(10) F5 0.0476(10) 0.0863(15) 0.0486(10) -0.0202(10) 0.0242(8) -0.0034(9) F6 0.1202(18) 0.0370(11) 0.0498(11) 0.0127(9) -0.0074(11) 0.0118(11) P11 0.0249(3) 0.0194(3) 0.0219(3) -0.0011(2) 0.0019(2) 0.0005(2) F11 0.0399(8) 0.0398(9) 0.0318(8) -0.0058(7) 0.0100(6) 0.0107(7) F12 0.0347(8) 0.0371(9) 0.0343(8) -0.0071(7) -0.0090(6) 0.0014(7) F13 0.0429(8) 0.0290(9) 0.0383(8) 0.0122(7) 0.0079(7) -0.0002(6) F14 0.0456(8) 0.0217(8) 0.0378(8) 0.0016(6) 0.0103(7) -0.0045(6) F15 0.0312(7) 0.0286(8) 0.0443(8) -0.0073(7) 0.0115(6) 0.0017(6) F16 0.0289(7) 0.0294(8) 0.0290(7) -0.0043(6) -0.0030(6) -0.0017(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn O8 2.0005(16) . ? Zn N12 2.0227(19) . ? Zn N22 2.0272(19) . ? Zn N2 2.0590(18) . ? Zn N1 2.1750(18) . ? N1 C1 1.465(3) . ? N1 C21 1.472(3) . ? N1 C11 1.473(3) . ? C1 C2 1.514(3) . ? C1OB C9 1.533(3) . ? C2 N2 1.357(3) . ? C2 C3 1.374(3) . ? N2 C6 1.335(3) . ? C3 C4 1.395(4) . ? C4 C5 1.371(3) . ? C5 C6 1.392(3) . ? C6 N7 1.404(3) . ? N7 C8 1.355(3) . ? O8 C8 1.241(3) . ? C8 C9 1.526(3) . ? C9 C10C 1.531(3) . ? C9 C10A 1.540(3) . ? C11 C12 1.512(3) . ? N12 C12 1.345(3) . ? N12 C16 1.348(3) . ? C12 C13 1.385(3) . ? C13 C14 1.373(4) . ? C14 C15 1.381(4) . ? C15 C16 1.376(4) . ? C21 C22 1.511(3) . ? N22 C26 1.343(3) . ? N22 C22 1.346(3) . ? C22 C23 1.379(3) . ? C23 C24 1.382(4) . ? C24 C25 1.378(4) . ? C25 C26 1.380(4) . ? P1 F6 1.5703(19) . ? P1 F2 1.5820(17) . ? P1 F5 1.5858(16) . ? P1 F1 1.5928(16) . ? P1 F4 1.5951(17) . ? P1 F3 1.6032(19) . ? P11 F12 1.5902(15) . ? P11 F11 1.5973(14) . ? P11 F15 1.5984(14) . ? P11 F13 1.6024(15) . ? P11 F14 1.6025(15) . ? P11 F16 1.6182(14) . ? 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 O8 Zn N12 108.69(7) . . ? O8 Zn N22 102.67(7) . . ? N12 Zn N22 110.12(8) . . ? O8 Zn N2 88.59(7) . . ? N12 Zn N2 118.08(8) . . ? N22 Zn N2 123.53(7) . . ? O8 Zn N1 167.75(6) . . ? N12 Zn N1 81.09(7) . . ? N22 Zn N1 80.01(7) . . ? N2 Zn N1 80.12(7) . . ? C1 N1 C21 113.63(17) . . ? C1 N1 C11 113.12(17) . . ? C21 N1 C11 112.81(18) . . ? C1 N1 Zn 106.62(14) . . ? C21 N1 Zn 103.90(12) . . ? C11 N1 Zn 105.78(13) . . ? N1 C1 C2 111.99(17) . . ? N2 C2 C3 122.6(2) . . ? N2 C2 C1 115.92(19) . . ? C3 C2 C1 121.5(2) . . ? C6 N2 C2 118.36(19) . . ? C6 N2 Zn 126.13(14) . . ? C2 N2 Zn 115.48(15) . . ? C2 C3 C4 118.3(2) . . ? C5 C4 C3 119.8(2) . . ? C4 C5 C6 118.6(2) . . ? N2 C6 C5 122.4(2) . . ? N2 C6 N7 119.89(19) . . ? C5 C6 N7 117.6(2) . . ? C8 N7 C6 130.8(2) . . ? C8 O8 Zn 127.52(14) . . ? O8 C8 N7 123.1(2) . . ? O8 C8 C9 119.71(19) . . ? N7 C8 C9 117.2(2) . . ? C8 C9 C10C 112.77(18) . . ? C8 C9 C1OB 107.07(19) . . ? C10C C9 C1OB 110.4(2) . . ? C8 C9 C10A 107.6(2) . . ? C10C C9 C10A 109.0(2) . . ? C1OB C9 C10A 110.0(2) . . ? N1 C11 C12 111.88(19) . . ? C12 N12 C16 119.2(2) . . ? C12 N12 Zn 115.10(15) . . ? C16 N12 Zn 125.62(17) . . ? N12 C12 C13 121.5(2) . . ? N12 C12 C11 117.41(19) . . ? C13 C12 C11 121.1(2) . . ? C14 C13 C12 119.1(3) . . ? C13 C14 C15 119.5(2) . . ? C16 C15 C14 119.0(3) . . ? N12 C16 C15 121.7(3) . . ? N1 C21 C22 110.20(17) . . ? C26 N22 C22 118.9(2) . . ? C26 N22 Zn 126.21(17) . . ? C22 N22 Zn 114.87(14) . . ? N22 C22 C23 121.7(2) . . ? N22 C22 C21 116.1(2) . . ? C23 C22 C21 122.2(2) . . ? C22 C23 C24 119.2(2) . . ? C25 C24 C23 119.2(3) . . ? C24 C25 C26 118.9(2) . . ? N22 C26 C25 122.1(2) . . ? F6 P1 F2 90.75(13) . . ? F6 P1 F5 90.62(13) . . ? F2 P1 F5 178.60(13) . . ? F6 P1 F1 89.86(10) . . ? F2 P1 F1 89.56(9) . . ? F5 P1 F1 90.11(9) . . ? F6 P1 F4 91.20(11) . . ? F2 P1 F4 90.80(10) . . ? F5 P1 F4 89.51(10) . . ? F1 P1 F4 178.88(10) . . ? F6 P1 F3 179.47(13) . . ? F2 P1 F3 89.55(12) . . ? F5 P1 F3 89.08(11) . . ? F1 P1 F3 89.70(10) . . ? F4 P1 F3 89.24(11) . . ? F12 P11 F11 90.26(8) . . ? F12 P11 F15 90.41(8) . . ? F11 P11 F15 179.28(9) . . ? F12 P11 F13 90.84(8) . . ? F11 P11 F13 90.46(8) . . ? F15 P11 F13 89.79(8) . . ? F12 P11 F14 91.00(8) . . ? F11 P11 F14 89.97(8) . . ? F15 P11 F14 89.76(8) . . ? F13 P11 F14 178.10(9) . . ? F12 P11 F16 179.58(9) . . ? F11 P11 F16 89.80(8) . . ? F15 P11 F16 89.53(8) . . ? F13 P11 F16 88.74(8) . . ? F14 P11 F16 89.41(8) . . ? _diffrn_measured_fraction_theta_max 0.935 _diffrn_reflns_theta_full 70.09 _diffrn_measured_fraction_theta_full 0.935 _refine_diff_density_max 0.423 _refine_diff_density_min -0.327 _refine_diff_density_rms 0.052 #===END data_znrr40 _database_code_CSD 203674 #COMPOUND 2' IN TEXT #SEE REFINE SPECIAL DETAILS FOR CHECKCIF OUTPUT _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [ZnL1Cl][BPh4].MeCN _chemical_formula_sum 'C49 H50 B Cl N6 O Zn' _chemical_formula_weight 850.58 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' B B 0.0013 0.0007 '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 Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.295(3) _cell_length_b 14.243(4) _cell_length_c 15.328(4) _cell_angle_alpha 73.973(5) _cell_angle_beta 86.034(5) _cell_angle_gamma 84.577(5) _cell_volume 2148.4(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5061 _cell_measurement_theta_min 2 _cell_measurement_theta_max 29 _exptl_crystal_description block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.86 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.315 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 892 _exptl_absorpt_coefficient_mu 0.679 _exptl_absorpt_correction_type Multiscan _exptl_absorpt_correction_T_min 0.778 _exptl_absorpt_correction_T_max 0.928 # CALC: _exptl_absorpt_correction_T_min 0.5930 # CALC: _exptl_absorpt_correction_T_max 0.8433 _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 19695 _diffrn_reflns_av_R_equivalents 0.0247 _diffrn_reflns_av_sigmaI/netI 0.0484 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 29.07 _reflns_number_total 10161 _reflns_number_gt 7748 _reflns_threshold_expression >2sigma(I) _computing_data_collection Smart _computing_cell_refinement Saint _computing_data_reduction Saint _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; CHECK CIF OUTPUT (For convenience the shelx res file is also included below): 230_ALERT A Hirshfeld test diff for C(43B) - C(44B) = 9.47 esd(su) Thermal ellipsoid plots show that the phenyl group containing these atoms appears to be undergoing a 'wagging' librational motion. The fact that there are no significant difference map peaks in this region suggests that this is reasonably well modelled by the anisotropic displacement parameters: there appears to be little to be gained by disorder modelling here. 063_ALERT B Crystal Probably too Large for Beam Size ..... 0.86 mm The collimator used was 0.5mm in diameter. Gorbitz has shown that use of a large crystal does not appear to matter. See C. H. Gorbitz Acta Cryst. (1999). B55, 1090-1098 411_ALERT B Short Inter H...H Contact: H(44A) .. H(73A) = 2.09 Ang. H44A is attached to the librating phenyl groups described above. The adp of C73 also seems to be elongated in a similar direction, and it is probably slightly disordered 'in sympathy' with C44. 042_ALERT C Calc. and Rep. MoietyFormula Strings Differ .. ? The one given is intended to be more chemically meaningful. 062_ALERT C Rescale T(min) & T(max) by ................... 0.90 No action. 125_ALERT C No _symmetry_space_group_name_Hall given ..... ? Corrected. 221_ALERT C Large Solvent/Anion C Ueq(max)/Ueq(min) . 3.08 Ratio 221_ALERT C Large Solvent/Anion N Ueq(max)/Ueq(min) . 3.87 Ratio 223_ALERT C Large Solvent/Anion H Ueq(max)/Ueq(min) . 3.21 Ratio 244_ALERT C Low Solvent U(eq) as Compared to Neighbors ... C(2S) Noted, it seems that the solvent may suffer some some orientational disorder in which C2S acts as a 'pivot'. 232_ALERT C Hirshfeld test diff (Me-X) Zn - Cl = 5.22 esd(su) This is slightly larger than might be expected; the Cl-atom is formally terminal, but appears to interact weakly with CH groups. This may have some influence on the displacement parameter. Final shelx res file: #TITL znrr40 in P-1 CELL 0.71073 10.2953 14.2430 15.3275 73.973 86.034 84.577 ZERR 2.00 0.0030 0.0041 0.0044 0.005 0.005 0.005 LATT 1 SFAC C H B N O CL ZN UNIT 98 100 2 12 2 2 2 TEMP -123 SIZE 0.86 0.42 0.26 L.S. 5 BOND $H FMAP 2 PLAN 10 ACTA HTAB RTAB DNCL CL N7 RTAB DHCL H7N CL RTAB AH7N CL H7N N7 RTAB DO8H O8 H45A WGHT 0.053000 FVAR 0.29275 ZN 7 0.244355 0.854208 0.168339 11.00000 0.03153 0.02428 = 0.02162 -0.00645 -0.00046 -0.00658 CL 6 0.387454 0.973360 0.125925 11.00000 0.05740 0.04727 = 0.03153 -0.01044 0.01058 -0.02918 N1 4 0.113087 0.735184 0.196274 11.00000 0.02957 0.02134 = 0.02745 -0.00709 -0.00591 -0.00204 C1 1 0.182611 0.655643 0.262973 11.00000 0.03805 0.02050 = 0.03300 -0.00712 -0.00606 -0.00478 AFIX 23 H1B 2 0.257109 0.626610 0.232160 11.00000 -1.20000 H1A 2 0.123075 0.603705 0.290786 11.00000 -1.20000 AFIX 0 N1S 4 0.990656 0.032828 0.660066 11.00000 0.12737 0.08869 = 0.06143 -0.03022 -0.01040 0.00794 C1S 1 1.002483 0.131561 0.492864 11.00000 0.06831 0.08025 = 0.06378 -0.01880 0.00531 -0.01149 AFIX 137 H1S1 2 0.924189 0.122475 0.464152 11.00000 -1.50000 H1S2 2 1.080353 0.108613 0.461766 11.00000 -1.50000 H1S3 2 1.005940 0.201214 0.488621 11.00000 -1.50000 AFIX 0 N2 4 0.270604 0.785707 0.309275 11.00000 0.02674 0.02082 = 0.02339 -0.00535 -0.00118 -0.00359 C2 1 0.231791 0.693674 0.335784 11.00000 0.02666 0.02261 = 0.02838 -0.00648 -0.00280 -0.00051 C2S 1 0.998006 0.076027 0.587428 11.00000 0.06598 0.06150 = 0.05083 -0.02251 -0.00314 0.00144 C3 1 0.236777 0.636505 0.423959 11.00000 0.03815 0.02308 = 0.03076 -0.00102 -0.00229 -0.00449 AFIX 43 H3A 2 0.209723 0.571746 0.440156 11.00000 -1.20000 AFIX 0 C4 1 0.281892 0.674907 0.488752 11.00000 0.04459 0.03215 = 0.02434 -0.00053 -0.00394 -0.00370 AFIX 43 H4A 2 0.286937 0.636425 0.550035 11.00000 -1.20000 AFIX 0 C5 1 0.319152 0.768522 0.464072 11.00000 0.04169 0.03358 = 0.02299 -0.00674 -0.00559 -0.00621 AFIX 43 H5A 2 0.349292 0.796196 0.507958 11.00000 -1.20000 AFIX 0 C6 1 0.312200 0.822841 0.373293 11.00000 0.02777 0.02638 = 0.02544 -0.00654 -0.00180 -0.00400 N7 4 0.350700 0.918256 0.343547 11.00000 0.03866 0.02815 = 0.02278 -0.00665 -0.00105 -0.01102 H7N 2 0.371971 0.934066 0.287154 11.00000 0.03546 O8 5 0.297719 0.965737 0.471969 11.00000 0.05614 0.04290 = 0.03364 -0.01689 0.00422 -0.00996 C8 1 0.343463 0.984713 0.394688 11.00000 0.02996 0.03200 = 0.03338 -0.01149 -0.00739 -0.00190 C9 1 0.395169 1.083768 0.346166 11.00000 0.03358 0.02822 = 0.04140 -0.01120 -0.01060 -0.00611 C10A 1 0.400812 1.141142 0.416195 11.00000 0.07149 0.03658 = 0.05829 -0.01991 -0.01626 -0.01113 AFIX 33 H10C 2 0.460855 1.105357 0.463208 11.00000 -1.50000 H10B 2 0.313421 1.149222 0.444129 11.00000 -1.50000 H10A 2 0.431787 1.205719 0.386256 11.00000 -1.50000 AFIX 0 C10B 1 0.531347 1.069836 0.302604 11.00000 0.03416 0.03921 = 0.06361 -0.00712 -0.00497 -0.01276 AFIX 33 H10F 2 0.591117 1.033766 0.349689 11.00000 -1.50000 H10E 2 0.563245 1.134039 0.272389 11.00000 -1.50000 H10D 2 0.526886 1.032781 0.257836 11.00000 -1.50000 AFIX 0 C10C 1 0.300743 1.139934 0.273287 11.00000 0.04363 0.03337 = 0.04707 -0.00436 -0.01076 -0.00138 AFIX 33 H10I 2 0.213769 1.148320 0.301711 11.00000 -1.50000 H10H 2 0.296060 1.103067 0.228395 11.00000 -1.50000 H10G 2 0.331938 1.204377 0.243093 11.00000 -1.50000 AFIX 0 C11 1 0.100431 0.709563 0.111056 11.00000 0.04273 0.02625 = 0.03559 -0.01049 -0.01338 -0.00431 AFIX 23 H11B 2 0.028908 0.752233 0.076787 11.00000 -1.20000 H11A 2 0.077663 0.640837 0.124829 11.00000 -1.20000 AFIX 0 N12 4 0.307637 0.781820 0.069865 11.00000 0.03147 0.03586 = 0.02693 -0.01200 -0.00720 0.00296 C12 1 0.225042 0.721398 0.053900 11.00000 0.03984 0.03106 = 0.03052 -0.01243 -0.01421 0.00837 C13 1 0.252389 0.676380 -0.015331 11.00000 0.05843 0.04561 = 0.04476 -0.02658 -0.02483 0.01625 AFIX 43 H13A 2 0.192481 0.634876 -0.026839 11.00000 -1.20000 AFIX 0 C14 1 0.366205 0.691943 -0.067168 11.00000 0.06392 0.07347 = 0.03725 -0.03289 -0.01629 0.03307 AFIX 43 H14A 2 0.385532 0.661598 -0.115003 11.00000 -1.20000 AFIX 0 C15 1 0.452473 0.751979 -0.049377 11.00000 0.04535 0.07927 = 0.03284 -0.02404 -0.00669 0.02000 AFIX 43 H15A 2 0.532836 0.762613 -0.083607 11.00000 -1.20000 AFIX 0 C16 1 0.419176 0.796090 0.019227 11.00000 0.03431 0.06012 = 0.03210 -0.01616 -0.00506 0.00489 AFIX 43 H16A 2 0.477588 0.838366 0.031190 11.00000 -1.20000 AFIX 0 C21 1 -0.012155 0.771634 0.231071 11.00000 0.03179 0.02687 = 0.03278 -0.00221 -0.00137 -0.00684 AFIX 23 H21B 2 -0.008705 0.763393 0.297173 11.00000 -1.20000 H21A 2 -0.082619 0.733381 0.221324 11.00000 -1.20000 AFIX 0 C22 1 -0.041206 0.878819 0.182690 11.00000 0.03515 0.02871 = 0.02734 -0.00504 -0.00064 -0.00020 C23 1 -0.167091 0.922013 0.176079 11.00000 0.03907 0.04491 = 0.04310 -0.00663 0.00121 0.00197 AFIX 43 H23A 2 -0.239385 0.883650 0.197014 11.00000 -1.20000 AFIX 0 C24 1 -0.186328 1.021935 0.138533 11.00000 0.05237 0.05075 = 0.05097 -0.00365 0.00104 0.02113 AFIX 43 H24A 2 -0.272056 1.053527 0.133674 11.00000 -1.20000 AFIX 0 C25 1 -0.079417 1.074994 0.108282 11.00000 0.06787 0.03191 = 0.04372 0.00144 0.00187 0.01271 AFIX 43 H25A 2 -0.090306 1.144000 0.083300 11.00000 -1.20000 AFIX 0 C26 1 0.042698 1.027423 0.114528 11.00000 0.05485 0.02603 = 0.03377 -0.00073 0.00298 -0.00258 AFIX 43 H26A 2 0.115980 1.064330 0.092216 11.00000 -1.20000 AFIX 0 B 3 0.716192 0.526621 0.236923 11.00000 0.02453 0.02556 = 0.02522 -0.00285 -0.00062 -0.00494 C41B 1 0.561732 0.509489 0.233471 11.00000 0.02588 0.01821 = 0.04736 -0.00125 -0.00326 0.00031 C42B 1 0.505643 0.510885 0.152564 11.00000 0.03204 0.02832 = 0.06554 -0.01542 -0.01610 0.00161 AFIX 43 H42A 2 0.552315 0.536834 0.096703 11.00000 -1.20000 AFIX 0 C43B 1 0.385960 0.476389 0.150199 11.00000 0.03294 0.03789 = 0.11982 -0.03566 -0.02383 0.00484 AFIX 43 H43A 2 0.352348 0.478031 0.093570 11.00000 -1.20000 AFIX 0 C44B 1 0.315808 0.440018 0.228589 11.00000 0.02788 0.02976 = 0.17614 -0.03677 -0.01640 0.00045 AFIX 43 H44A 2 0.234143 0.414715 0.226966 11.00000 -1.20000 AFIX 0 C45B 1 0.363326 0.439822 0.310877 11.00000 0.03252 0.02288 = 0.12136 0.00030 0.02673 -0.00024 AFIX 43 H45A 2 0.313669 0.415669 0.365814 11.00000 -1.20000 AFIX 0 C46B 1 0.484533 0.475275 0.312755 11.00000 0.03125 0.02830 = 0.06285 0.00235 0.00761 0.00157 AFIX 43 H46A 2 0.515554 0.476226 0.369431 11.00000 -1.20000 AFIX 0 C51B 1 0.739052 0.579041 0.317456 11.00000 0.02971 0.02840 = 0.02568 -0.00369 0.00507 -0.00738 C52B 1 0.846445 0.555918 0.372542 11.00000 0.03877 0.02973 = 0.02609 -0.00317 0.00234 -0.01157 AFIX 43 H52A 2 0.907581 0.503400 0.366883 11.00000 -1.20000 AFIX 0 C53B 1 0.867736 0.606483 0.435337 11.00000 0.04796 0.04791 = 0.02751 -0.00736 0.00005 -0.02028 AFIX 43 H53A 2 0.942399 0.588302 0.471211 11.00000 -1.20000 AFIX 0 C54B 1 0.781906 0.681995 0.445591 11.00000 0.06242 0.05794 = 0.03907 -0.02637 0.01398 -0.02428 AFIX 43 H54A 2 0.796909 0.717085 0.487937 11.00000 -1.20000 AFIX 0 C55B 1 0.672225 0.707182 0.393515 11.00000 0.05213 0.05511 = 0.05449 -0.03058 0.01498 -0.00471 AFIX 43 H55A 2 0.611586 0.759558 0.400253 11.00000 -1.20000 AFIX 0 C56B 1 0.651602 0.655962 0.332018 11.00000 0.03882 0.04376 = 0.04046 -0.01603 0.00503 -0.00338 AFIX 43 H56A 2 0.575065 0.673350 0.298016 11.00000 -1.20000 AFIX 0 C61B 1 0.764883 0.598123 0.137805 11.00000 0.02404 0.02559 = 0.02597 -0.00502 -0.00540 -0.00684 C62B 1 0.732091 0.699484 0.113033 11.00000 0.02830 0.02904 = 0.03206 -0.00591 -0.00275 -0.00421 AFIX 43 H62A 2 0.685670 0.727860 0.156445 11.00000 -1.20000 AFIX 0 C63B 1 0.764195 0.760373 0.028121 11.00000 0.03521 0.02420 = 0.03794 0.00085 -0.00758 -0.00440 AFIX 43 H63A 2 0.739863 0.828690 0.014772 11.00000 -1.20000 AFIX 0 C64B 1 0.831113 0.722212 -0.036808 11.00000 0.03871 0.03736 = 0.02520 0.00338 -0.00711 -0.01158 AFIX 43 H64A 2 0.853563 0.763569 -0.094975 11.00000 -1.20000 AFIX 0 C65B 1 0.865174 0.622102 -0.015656 11.00000 0.04162 0.03767 = 0.02554 -0.00919 -0.00093 -0.00919 AFIX 43 H65A 2 0.911185 0.594301 -0.059598 11.00000 -1.20000 AFIX 0 C66B 1 0.831906 0.562447 0.069953 11.00000 0.03906 0.02528 = 0.02826 -0.00599 -0.00280 -0.00789 AFIX 43 H66A 2 0.856052 0.494139 0.082731 11.00000 -1.20000 AFIX 0 C71B 1 0.797034 0.417598 0.254704 11.00000 0.02721 0.02708 = 0.01847 -0.00336 -0.00187 -0.00475 C72B 1 0.932896 0.405896 0.244712 11.00000 0.02932 0.02632 = 0.04399 -0.00178 -0.00014 -0.00747 AFIX 43 H72A 2 0.980127 0.462779 0.230374 11.00000 -1.20000 AFIX 0 C73B 1 1.002339 0.316008 0.254560 11.00000 0.02442 0.03448 = 0.06379 -0.00605 0.00104 -0.00344 AFIX 43 H73A 2 1.094869 0.312490 0.246923 11.00000 -1.20000 AFIX 0 C74B 1 0.937995 0.231176 0.275457 11.00000 0.03684 0.02702 = 0.05280 -0.00699 -0.00614 0.00025 AFIX 43 H74A 2 0.984830 0.169265 0.280669 11.00000 -1.20000 AFIX 0 C75B 1 0.804409 0.238795 0.288494 11.00000 0.03390 0.02725 = 0.04609 -0.00665 -0.00526 -0.00913 AFIX 43 H75A 2 0.758339 0.181276 0.305109 11.00000 -1.20000 AFIX 0 C76B 1 0.736232 0.329898 0.277575 11.00000 0.02554 0.03044 = 0.02828 -0.00768 -0.00290 -0.00591 AFIX 43 H76A 2 0.643808 0.332701 0.286070 11.00000 -1.20000 AFIX 0 N122 4 0.062693 0.930117 0.151193 11.00000 0.03861 0.02281 = 0.02470 -0.00313 0.00135 -0.00234 HKLF 4 REM znrr40 in P-1 REM R1 = 0.0390 for 7748 Fo > 4sig(Fo) and 0.0502 for all 10161 data REM 537 parameters refined using 0 restraints END WGHT 0.0530 0.0000 REM Highest difference peak 0.544, deepest hole -0.304, 1-sigma level 0.057 Q1 1 1.0000 0.0000 0.5000 10.50000 0.05 0.50 Q2 1 0.1598 0.8827 0.1489 11.00000 0.05 0.44 Q3 1 0.3190 0.8854 0.1399 11.00000 0.05 0.41 Q4 1 0.3044 0.4370 0.2094 11.00000 0.05 0.40 Q5 1 0.2137 0.8846 0.2134 11.00000 0.05 0.39 Q6 1 0.1835 0.8132 0.1897 11.00000 0.05 0.39 Q7 1 0.2752 0.8208 0.1178 11.00000 0.05 0.38 Q8 1 0.4076 0.9134 0.1347 11.00000 0.05 0.38 Q9 1 0.2563 0.7917 0.1705 11.00000 0.05 0.36 Q10 1 0.3051 0.8309 0.2107 11.00000 0.05 0.35 ; _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^)+(0.0530P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geometric/difmap _refine_ls_hydrogen_treatment 'riding, rotating group (Me), refall (H7N)' _refine_ls_extinction_method none #Refined to zero _refine_ls_extinction_coef ? _refine_ls_number_reflns 10161 _refine_ls_number_parameters 537 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0502 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.0983 _refine_ls_wR_factor_gt 0.0951 _refine_ls_goodness_of_fit_ref 0.953 _refine_ls_restrained_S_all 0.953 _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 0.24435(2) 0.854208(14) 0.168339(13) 0.02551(7) Uani 1 1 d . . . Cl Cl 0.38745(6) 0.97336(4) 0.12592(3) 0.04440(14) Uani 1 1 d . . . N1 N 0.11309(15) 0.73518(10) 0.19627(10) 0.0258(3) Uani 1 1 d . . . C1 C 0.18261(19) 0.65564(13) 0.26297(12) 0.0302(4) Uani 1 1 d . . . H1B H 0.2571 0.6266 0.2322 0.036 Uiso 1 1 calc R . . H1A H 0.1231 0.6037 0.2908 0.036 Uiso 1 1 calc R . . N1S N 0.9907(3) 0.0328(2) 0.66007(18) 0.0913(9) Uani 1 1 d . . . C1S C 1.0025(3) 0.1316(2) 0.49286(19) 0.0710(8) Uani 1 1 d . . . H1S1 H 0.9242 0.1225 0.4642 0.106 Uiso 1 1 calc R . . H1S2 H 1.0804 0.1086 0.4618 0.106 Uiso 1 1 calc R . . H1S3 H 1.0059 0.2012 0.4886 0.106 Uiso 1 1 calc R . . N2 N 0.27060(14) 0.78571(10) 0.30927(9) 0.0237(3) Uani 1 1 d . . . C2 C 0.23179(17) 0.69367(12) 0.33578(12) 0.0260(4) Uani 1 1 d . . . C2S C 0.9980(3) 0.0760(2) 0.58743(19) 0.0584(7) Uani 1 1 d . . . C3 C 0.23678(19) 0.63650(13) 0.42396(12) 0.0317(4) Uani 1 1 d . . . H3A H 0.2097 0.5717 0.4402 0.038 Uiso 1 1 calc R . . C4 C 0.2819(2) 0.67491(14) 0.48875(13) 0.0350(5) Uani 1 1 d . . . H4A H 0.2869 0.6364 0.5500 0.042 Uiso 1 1 calc R . . C5 C 0.31915(19) 0.76852(14) 0.46407(12) 0.0325(4) Uani 1 1 d . . . H5A H 0.3493 0.7962 0.5080 0.039 Uiso 1 1 calc R . . C6 C 0.31220(17) 0.82284(13) 0.37329(12) 0.0265(4) Uani 1 1 d . . . N7 N 0.35070(16) 0.91826(11) 0.34355(11) 0.0294(4) Uani 1 1 d . . . H7N H 0.3720(19) 0.9341(14) 0.2872(14) 0.035(6) Uiso 1 1 d . . . O8 O 0.29772(15) 0.96574(10) 0.47197(9) 0.0428(4) Uani 1 1 d . . . C8 C 0.34346(18) 0.98471(14) 0.39469(13) 0.0310(4) Uani 1 1 d . . . C9 C 0.39517(19) 1.08377(14) 0.34617(14) 0.0334(4) Uani 1 1 d . . . C10A C 0.4008(3) 1.14114(16) 0.41620(16) 0.0529(6) Uani 1 1 d . . . H10C H 0.4609 1.1054 0.4632 0.079 Uiso 1 1 calc R . . H10B H 0.3134 1.1492 0.4441 0.079 Uiso 1 1 calc R . . H10A H 0.4318 1.2057 0.3863 0.079 Uiso 1 1 calc R . . C10B C 0.5313(2) 1.06984(16) 0.30260(16) 0.0462(6) Uani 1 1 d . . . H10F H 0.5911 1.0338 0.3497 0.069 Uiso 1 1 calc R . . H10E H 0.5632 1.1340 0.2724 0.069 Uiso 1 1 calc R . . H10D H 0.5269 1.0328 0.2578 0.069 Uiso 1 1 calc R . . C10C C 0.3007(2) 1.13993(15) 0.27329(15) 0.0424(5) Uani 1 1 d . . . H10I H 0.2138 1.1483 0.3017 0.064 Uiso 1 1 calc R . . H10H H 0.2961 1.1031 0.2284 0.064 Uiso 1 1 calc R . . H10G H 0.3319 1.2044 0.2431 0.064 Uiso 1 1 calc R . . C11 C 0.1004(2) 0.70956(14) 0.11106(13) 0.0338(4) Uani 1 1 d . . . H11B H 0.0289 0.7522 0.0768 0.041 Uiso 1 1 calc R . . H11A H 0.0777 0.6408 0.1248 0.041 Uiso 1 1 calc R . . N12 N 0.30764(15) 0.78182(11) 0.06987(10) 0.0308(4) Uani 1 1 d . . . C12 C 0.2250(2) 0.72140(14) 0.05390(13) 0.0331(4) Uani 1 1 d . . . C13 C 0.2524(2) 0.67638(16) -0.01533(15) 0.0470(6) Uani 1 1 d . . . H13A H 0.1925 0.6349 -0.0268 0.056 Uiso 1 1 calc R . . C14 C 0.3662(3) 0.69194(19) -0.06717(15) 0.0565(7) Uani 1 1 d . . . H14A H 0.3855 0.6616 -0.1150 0.068 Uiso 1 1 calc R . . C15 C 0.4525(2) 0.75198(19) -0.04938(15) 0.0521(6) Uani 1 1 d . . . H15A H 0.5328 0.7626 -0.0836 0.063 Uiso 1 1 calc R . . C16 C 0.4192(2) 0.79609(17) 0.01923(13) 0.0418(5) Uani 1 1 d . . . H16A H 0.4776 0.8384 0.0312 0.050 Uiso 1 1 calc R . . C21 C -0.01215(19) 0.77163(13) 0.23107(13) 0.0314(4) Uani 1 1 d . . . H21B H -0.0087 0.7634 0.2972 0.038 Uiso 1 1 calc R . . H21A H -0.0826 0.7334 0.2213 0.038 Uiso 1 1 calc R . . C22 C -0.04121(19) 0.87882(13) 0.18269(12) 0.0311(4) Uani 1 1 d . . . C23 C -0.1671(2) 0.92201(16) 0.17608(15) 0.0439(5) Uani 1 1 d . . . H23A H -0.2394 0.8836 0.1970 0.053 Uiso 1 1 calc R . . C24 C -0.1863(3) 1.02193(18) 0.13853(16) 0.0552(7) Uani 1 1 d . . . H24A H -0.2721 1.0535 0.1337 0.066 Uiso 1 1 calc R . . C25 C -0.0794(3) 1.07499(16) 0.10828(15) 0.0515(6) Uani 1 1 d . . . H25A H -0.0903 1.1440 0.0833 0.062 Uiso 1 1 calc R . . C26 C 0.0427(2) 1.02742(14) 0.11453(13) 0.0400(5) Uani 1 1 d . . . H26A H 0.1160 1.0643 0.0922 0.048 Uiso 1 1 calc R . . B B 0.7162(2) 0.52662(15) 0.23692(14) 0.0257(4) Uani 1 1 d . . . C41B C 0.56173(18) 0.50949(13) 0.23347(14) 0.0321(4) Uani 1 1 d . . . C42B C 0.5056(2) 0.51088(14) 0.15256(16) 0.0410(5) Uani 1 1 d . . . H42A H 0.5523 0.5368 0.0967 0.049 Uiso 1 1 calc R . . C43B C 0.3860(2) 0.47639(17) 0.1502(2) 0.0602(8) Uani 1 1 d . . . H43A H 0.3523 0.4780 0.0936 0.072 Uiso 1 1 calc R . . C44B C 0.3158(2) 0.44002(17) 0.2286(3) 0.0758(10) Uani 1 1 d . . . H44A H 0.2341 0.4147 0.2270 0.091 Uiso 1 1 calc R . . C45B C 0.3633(2) 0.43982(15) 0.3109(2) 0.0645(9) Uani 1 1 d . . . H45A H 0.3137 0.4157 0.3658 0.077 Uiso 1 1 calc R . . C46B C 0.4845(2) 0.47527(14) 0.31276(17) 0.0445(6) Uani 1 1 d . . . H46A H 0.5156 0.4762 0.3694 0.053 Uiso 1 1 calc R . . C51B C 0.73905(18) 0.57904(13) 0.31746(12) 0.0286(4) Uani 1 1 d . . . C52B C 0.8464(2) 0.55592(14) 0.37254(12) 0.0320(4) Uani 1 1 d . . . H52A H 0.9076 0.5034 0.3669 0.038 Uiso 1 1 calc R . . C53B C 0.8677(2) 0.60648(16) 0.43534(13) 0.0407(5) Uani 1 1 d . . . H53A H 0.9424 0.5883 0.4712 0.049 Uiso 1 1 calc R . . C54B C 0.7819(2) 0.68200(18) 0.44559(15) 0.0500(6) Uani 1 1 d . . . H54A H 0.7969 0.7171 0.4879 0.060 Uiso 1 1 calc R . . C55B C 0.6722(2) 0.70718(18) 0.39351(16) 0.0516(6) Uani 1 1 d . . . H55A H 0.6116 0.7596 0.4003 0.062 Uiso 1 1 calc R . . C56B C 0.6516(2) 0.65596(15) 0.33202(14) 0.0404(5) Uani 1 1 d . . . H56A H 0.5751 0.6734 0.2980 0.048 Uiso 1 1 calc R . . C61B C 0.76488(17) 0.59812(12) 0.13781(12) 0.0251(4) Uani 1 1 d . . . C62B C 0.73209(18) 0.69948(13) 0.11303(13) 0.0301(4) Uani 1 1 d . . . H62A H 0.6857 0.7279 0.1564 0.036 Uiso 1 1 calc R . . C63B C 0.76420(19) 0.76037(14) 0.02812(13) 0.0339(4) Uani 1 1 d . . . H63A H 0.7399 0.8287 0.0148 0.041 Uiso 1 1 calc R . . C64B C 0.8311(2) 0.72221(14) -0.03681(13) 0.0353(5) Uani 1 1 d . . . H64A H 0.8536 0.7636 -0.0950 0.042 Uiso 1 1 calc R . . C65B C 0.8652(2) 0.62210(14) -0.01566(13) 0.0344(4) Uani 1 1 d . . . H65A H 0.9112 0.5943 -0.0596 0.041 Uiso 1 1 calc R . . C66B C 0.83191(19) 0.56245(13) 0.06995(12) 0.0307(4) Uani 1 1 d . . . H66A H 0.8561 0.4941 0.0827 0.037 Uiso 1 1 calc R . . C71B C 0.79703(17) 0.41760(13) 0.25470(11) 0.0246(4) Uani 1 1 d . . . C72B C 0.93290(19) 0.40590(14) 0.24471(14) 0.0345(5) Uani 1 1 d . . . H72A H 0.9801 0.4628 0.2304 0.041 Uiso 1 1 calc R . . C73B C 1.0023(2) 0.31601(15) 0.25456(16) 0.0424(5) Uani 1 1 d . . . H73A H 1.0949 0.3125 0.2469 0.051 Uiso 1 1 calc R . . C74B C 0.9380(2) 0.23118(15) 0.27546(15) 0.0396(5) Uani 1 1 d . . . H74A H 0.9848 0.1693 0.2807 0.048 Uiso 1 1 calc R . . C75B C 0.80441(19) 0.23879(14) 0.28849(14) 0.0358(5) Uani 1 1 d . . . H75A H 0.7583 0.1813 0.3051 0.043 Uiso 1 1 calc R . . C76B C 0.73623(18) 0.32990(13) 0.27758(12) 0.0278(4) Uani 1 1 d . . . H76A H 0.6438 0.3327 0.2861 0.033 Uiso 1 1 calc R . . N122 N 0.06269(16) 0.93012(11) 0.15119(10) 0.0295(3) 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 0.03153(13) 0.02428(12) 0.02162(11) -0.00645(8) -0.00046(8) -0.00658(9) Cl 0.0574(3) 0.0473(3) 0.0315(3) -0.0104(2) 0.0106(2) -0.0292(3) N1 0.0296(8) 0.0213(7) 0.0274(8) -0.0071(6) -0.0059(6) -0.0020(6) C1 0.0381(11) 0.0205(9) 0.0330(10) -0.0071(8) -0.0061(8) -0.0048(8) N1S 0.127(3) 0.089(2) 0.0614(17) -0.0302(15) -0.0104(17) 0.0079(18) C1S 0.0683(19) 0.080(2) 0.0638(18) -0.0188(16) 0.0053(15) -0.0115(16) N2 0.0267(8) 0.0208(7) 0.0234(7) -0.0054(6) -0.0012(6) -0.0036(6) C2 0.0267(9) 0.0226(9) 0.0284(9) -0.0065(7) -0.0028(7) -0.0005(7) C2S 0.0660(18) 0.0615(17) 0.0508(16) -0.0225(14) -0.0031(13) 0.0014(13) C3 0.0381(11) 0.0231(9) 0.0308(10) -0.0010(8) -0.0023(8) -0.0045(8) C4 0.0446(12) 0.0322(10) 0.0243(10) -0.0005(8) -0.0039(8) -0.0037(9) C5 0.0417(11) 0.0336(10) 0.0230(9) -0.0067(8) -0.0056(8) -0.0062(9) C6 0.0278(10) 0.0264(9) 0.0254(9) -0.0065(7) -0.0018(7) -0.0040(8) N7 0.0387(9) 0.0281(8) 0.0228(8) -0.0067(7) -0.0011(7) -0.0110(7) O8 0.0561(10) 0.0429(8) 0.0336(8) -0.0169(7) 0.0042(7) -0.0100(7) C8 0.0300(10) 0.0320(10) 0.0334(11) -0.0115(8) -0.0074(8) -0.0019(8) C9 0.0336(11) 0.0282(10) 0.0414(11) -0.0112(8) -0.0106(9) -0.0061(8) C10A 0.0715(17) 0.0366(12) 0.0583(15) -0.0199(11) -0.0163(13) -0.0111(11) C10B 0.0342(12) 0.0392(12) 0.0636(15) -0.0071(11) -0.0050(11) -0.0128(10) C10C 0.0436(13) 0.0334(11) 0.0471(13) -0.0044(9) -0.0108(10) -0.0014(9) C11 0.0427(12) 0.0262(10) 0.0356(11) -0.0105(8) -0.0134(9) -0.0043(8) N12 0.0315(9) 0.0359(9) 0.0269(8) -0.0120(7) -0.0072(7) 0.0030(7) C12 0.0398(11) 0.0311(10) 0.0305(10) -0.0124(8) -0.0142(9) 0.0084(9) C13 0.0584(15) 0.0456(13) 0.0448(13) -0.0266(11) -0.0248(11) 0.0162(11) C14 0.0639(17) 0.0735(17) 0.0373(13) -0.0329(12) -0.0163(12) 0.0331(14) C15 0.0454(14) 0.0793(18) 0.0328(12) -0.0240(12) -0.0067(10) 0.0200(12) C16 0.0343(12) 0.0601(14) 0.0321(11) -0.0162(10) -0.0051(9) 0.0049(10) C21 0.0318(10) 0.0269(10) 0.0328(10) -0.0022(8) -0.0014(8) -0.0068(8) C22 0.0351(11) 0.0287(10) 0.0273(10) -0.0050(8) -0.0006(8) -0.0002(8) C23 0.0391(12) 0.0449(13) 0.0431(12) -0.0066(10) 0.0012(10) 0.0020(10) C24 0.0524(15) 0.0507(15) 0.0510(14) -0.0037(11) 0.0010(12) 0.0211(12) C25 0.0679(17) 0.0319(12) 0.0437(13) 0.0014(10) 0.0019(12) 0.0127(11) C26 0.0548(14) 0.0260(10) 0.0338(11) -0.0007(8) 0.0030(10) -0.0026(9) B 0.0245(10) 0.0256(10) 0.0252(10) -0.0029(8) -0.0006(8) -0.0049(8) C41B 0.0259(10) 0.0182(9) 0.0474(12) -0.0013(8) -0.0033(8) 0.0003(7) C42B 0.0320(11) 0.0283(10) 0.0655(15) -0.0154(10) -0.0161(10) 0.0016(9) C43B 0.0329(13) 0.0379(13) 0.120(2) -0.0357(15) -0.0238(15) 0.0048(11) C44B 0.0279(13) 0.0298(13) 0.176(4) -0.0368(18) -0.0164(18) 0.0004(10) C45B 0.0325(13) 0.0229(11) 0.121(3) 0.0003(13) 0.0267(15) -0.0002(10) C46B 0.0313(11) 0.0283(11) 0.0629(15) 0.0024(10) 0.0076(10) 0.0016(9) C51B 0.0297(10) 0.0284(10) 0.0257(9) -0.0037(7) 0.0051(8) -0.0074(8) C52B 0.0388(11) 0.0297(10) 0.0261(10) -0.0032(8) 0.0023(8) -0.0116(8) C53B 0.0480(13) 0.0479(13) 0.0275(10) -0.0074(9) 0.0001(9) -0.0203(10) C54B 0.0624(16) 0.0579(15) 0.0391(12) -0.0264(11) 0.0140(11) -0.0243(13) C55B 0.0521(15) 0.0551(15) 0.0545(15) -0.0306(12) 0.0150(12) -0.0047(12) C56B 0.0388(12) 0.0438(12) 0.0405(12) -0.0160(10) 0.0050(9) -0.0034(10) C61B 0.0240(9) 0.0256(9) 0.0260(9) -0.0050(7) -0.0054(7) -0.0068(7) C62B 0.0283(10) 0.0290(10) 0.0321(10) -0.0059(8) -0.0028(8) -0.0042(8) C63B 0.0352(11) 0.0242(10) 0.0379(11) 0.0008(8) -0.0076(9) -0.0044(8) C64B 0.0387(11) 0.0374(11) 0.0252(10) 0.0034(8) -0.0071(8) -0.0116(9) C65B 0.0416(12) 0.0377(11) 0.0255(10) -0.0092(8) -0.0009(8) -0.0092(9) C66B 0.0391(11) 0.0253(9) 0.0283(10) -0.0060(8) -0.0028(8) -0.0079(8) C71B 0.0272(9) 0.0271(9) 0.0185(8) -0.0034(7) -0.0019(7) -0.0048(7) C72B 0.0293(10) 0.0263(10) 0.0440(12) -0.0018(8) -0.0001(9) -0.0075(8) C73B 0.0244(10) 0.0345(11) 0.0638(15) -0.0060(10) 0.0010(10) -0.0034(9) C74B 0.0368(12) 0.0270(10) 0.0528(13) -0.0070(9) -0.0061(10) 0.0002(9) C75B 0.0339(11) 0.0273(10) 0.0461(12) -0.0066(9) -0.0053(9) -0.0091(8) C76B 0.0255(9) 0.0304(10) 0.0283(10) -0.0077(8) -0.0029(7) -0.0059(8) N122 0.0386(9) 0.0228(8) 0.0247(8) -0.0031(6) 0.0014(7) -0.0023(7) _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 N122 2.0651(17) . ? Zn N12 2.0885(16) . ? Zn N2 2.1351(15) . ? Zn N1 2.1990(15) . ? Zn Cl 2.2812(7) . ? N1 C21 1.466(2) . ? N1 C1 1.466(2) . ? N1 C11 1.467(2) . ? C1 C2 1.503(2) . ? C1 H1B 0.9900 . ? C1 H1A 0.9900 . ? N1S C2S 1.115(3) . ? C1S C2S 1.447(4) . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? N2 C6 1.347(2) . ? N2 C2 1.351(2) . ? C2 C3 1.373(2) . ? C3 C4 1.383(3) . ? C3 H3A 0.9500 . ? C4 C5 1.366(3) . ? C4 H4A 0.9500 . ? C5 C6 1.396(2) . ? C5 H5A 0.9500 . ? C6 N7 1.395(2) . ? N7 C8 1.380(2) . ? N7 H7N 0.85(2) . ? O8 C8 1.212(2) . ? C8 C9 1.528(3) . ? C9 C10A 1.525(3) . ? C9 C10B 1.530(3) . ? C9 C10C 1.531(3) . ? C10A H10C 0.9800 . ? C10A H10B 0.9800 . ? C10A H10A 0.9800 . ? C10B H10F 0.9800 . ? C10B H10E 0.9800 . ? C10B H10D 0.9800 . ? C10C H10I 0.9800 . ? C10C H10H 0.9800 . ? C10C H10G 0.9800 . ? C11 C12 1.499(3) . ? C11 H11B 0.9900 . ? C11 H11A 0.9900 . ? N12 C16 1.340(3) . ? N12 C12 1.344(2) . ? C12 C13 1.384(3) . ? C13 C14 1.370(3) . ? C13 H13A 0.9500 . ? C14 C15 1.378(4) . ? C14 H14A 0.9500 . ? C15 C16 1.376(3) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C21 C22 1.513(2) . ? C21 H21B 0.9900 . ? C21 H21A 0.9900 . ? C22 N122 1.339(2) . ? C22 C23 1.379(3) . ? C23 C24 1.381(3) . ? C23 H23A 0.9500 . ? C24 C25 1.375(4) . ? C24 H24A 0.9500 . ? C25 C26 1.367(3) . ? C25 H25A 0.9500 . ? C26 N122 1.346(2) . ? C26 H26A 0.9500 . ? B C41B 1.638(3) . ? B C51B 1.649(3) . ? B C71B 1.653(3) . ? B C61B 1.653(3) . ? C41B C42B 1.398(3) . ? C41B C46B 1.399(3) . ? C42B C43B 1.375(3) . ? C42B H42A 0.9500 . ? C43B C44B 1.357(4) . ? C43B H43A 0.9500 . ? C44B C45B 1.383(4) . ? C44B H44A 0.9500 . ? C45B C46B 1.395(3) . ? C45B H45A 0.9500 . ? C46B H46A 0.9500 . ? C51B C52B 1.397(3) . ? C51B C56B 1.408(3) . ? C52B C53B 1.391(3) . ? C52B H52A 0.9500 . ? C53B C54B 1.363(3) . ? C53B H53A 0.9500 . ? C54B C55B 1.390(3) . ? C54B H54A 0.9500 . ? C55B C56B 1.379(3) . ? C55B H55A 0.9500 . ? C56B H56A 0.9500 . ? C61B C66B 1.394(2) . ? C61B C62B 1.402(2) . ? C62B C63B 1.388(3) . ? C62B H62A 0.9500 . ? C63B C64B 1.376(3) . ? C63B H63A 0.9500 . ? C64B C65B 1.388(3) . ? C64B H64A 0.9500 . ? C65B C66B 1.392(3) . ? C65B H65A 0.9500 . ? C66B H66A 0.9500 . ? C71B C72B 1.396(3) . ? C71B C76B 1.397(2) . ? C72B C73B 1.381(3) . ? C72B H72A 0.9500 . ? C73B C74B 1.382(3) . ? C73B H73A 0.9500 . ? C74B C75B 1.374(3) . ? C74B H74A 0.9500 . ? C75B C76B 1.389(3) . ? C75B H75A 0.9500 . ? C76B H76A 0.9500 . ? 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 N122 Zn N12 115.84(6) . . ? N122 Zn N2 109.84(6) . . ? N12 Zn N2 121.11(6) . . ? N122 Zn N1 77.75(6) . . ? N12 Zn N1 77.51(6) . . ? N2 Zn N1 78.02(5) . . ? N122 Zn Cl 104.24(5) . . ? N12 Zn Cl 96.66(5) . . ? N2 Zn Cl 106.20(4) . . ? N1 Zn Cl 174.09(4) . . ? C21 N1 C1 114.11(15) . . ? C21 N1 C11 112.11(15) . . ? C1 N1 C11 111.67(14) . . ? C21 N1 Zn 107.23(10) . . ? C1 N1 Zn 103.16(11) . . ? C11 N1 Zn 107.86(11) . . ? N1 C1 C2 110.37(14) . . ? N1 C1 H1B 109.6 . . ? C2 C1 H1B 109.6 . . ? N1 C1 H1A 109.6 . . ? C2 C1 H1A 109.6 . . ? H1B C1 H1A 108.1 . . ? C2S C1S H1S1 109.5 . . ? C2S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? C2S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? C6 N2 C2 117.84(14) . . ? C6 N2 Zn 129.45(11) . . ? C2 N2 Zn 112.60(11) . . ? N2 C2 C3 122.76(17) . . ? N2 C2 C1 116.36(15) . . ? C3 C2 C1 120.88(16) . . ? N1S C2S C1S 177.9(3) . . ? C2 C3 C4 118.81(17) . . ? C2 C3 H3A 120.6 . . ? C4 C3 H3A 120.6 . . ? C5 C4 C3 119.58(17) . . ? C5 C4 H4A 120.2 . . ? C3 C4 H4A 120.2 . . ? C4 C5 C6 118.89(17) . . ? C4 C5 H5A 120.6 . . ? C6 C5 H5A 120.6 . . ? N2 C6 N7 116.25(15) . . ? N2 C6 C5 122.09(16) . . ? N7 C6 C5 121.65(16) . . ? C8 N7 C6 125.72(16) . . ? C8 N7 H7N 122.1(14) . . ? C6 N7 H7N 111.8(14) . . ? O8 C8 N7 122.04(18) . . ? O8 C8 C9 122.86(17) . . ? N7 C8 C9 115.09(16) . . ? C10A C9 C8 108.03(17) . . ? C10A C9 C10B 110.00(17) . . ? C8 C9 C10B 110.63(16) . . ? C10A C9 C10C 109.11(17) . . ? C8 C9 C10C 109.02(16) . . ? C10B C9 C10C 110.01(18) . . ? C9 C10A H10C 109.5 . . ? C9 C10A H10B 109.5 . . ? H10C C10A H10B 109.5 . . ? C9 C10A H10A 109.5 . . ? H10C C10A H10A 109.5 . . ? H10B C10A H10A 109.5 . . ? C9 C10B H10F 109.5 . . ? C9 C10B H10E 109.5 . . ? H10F C10B H10E 109.5 . . ? C9 C10B H10D 109.5 . . ? H10F C10B H10D 109.5 . . ? H10E C10B H10D 109.5 . . ? C9 C10C H10I 109.5 . . ? C9 C10C H10H 109.5 . . ? H10I C10C H10H 109.5 . . ? C9 C10C H10G 109.5 . . ? H10I C10C H10G 109.5 . . ? H10H C10C H10G 109.5 . . ? N1 C11 C12 111.03(15) . . ? N1 C11 H11B 109.4 . . ? C12 C11 H11B 109.4 . . ? N1 C11 H11A 109.4 . . ? C12 C11 H11A 109.4 . . ? H11B C11 H11A 108.0 . . ? C16 N12 C12 119.03(17) . . ? C16 N12 Zn 124.67(14) . . ? C12 N12 Zn 116.18(13) . . ? N12 C12 C13 120.8(2) . . ? N12 C12 C11 116.95(16) . . ? C13 C12 C11 122.15(19) . . ? C14 C13 C12 119.7(2) . . ? C14 C13 H13A 120.1 . . ? C12 C13 H13A 120.1 . . ? C13 C14 C15 119.5(2) . . ? C13 C14 H14A 120.3 . . ? C15 C14 H14A 120.3 . . ? C16 C15 C14 118.3(2) . . ? C16 C15 H15A 120.9 . . ? C14 C15 H15A 120.9 . . ? N12 C16 C15 122.6(2) . . ? N12 C16 H16A 118.7 . . ? C15 C16 H16A 118.7 . . ? N1 C21 C22 109.92(15) . . ? N1 C21 H21B 109.7 . . ? C22 C21 H21B 109.7 . . ? N1 C21 H21A 109.7 . . ? C22 C21 H21A 109.7 . . ? H21B C21 H21A 108.2 . . ? N122 C22 C23 122.13(18) . . ? N122 C22 C21 116.04(16) . . ? C23 C22 C21 121.74(18) . . ? C22 C23 C24 118.9(2) . . ? C22 C23 H23A 120.5 . . ? C24 C23 H23A 120.5 . . ? C25 C24 C23 118.9(2) . . ? C25 C24 H24A 120.5 . . ? C23 C24 H24A 120.5 . . ? C26 C25 C24 119.3(2) . . ? C26 C25 H25A 120.3 . . ? C24 C25 H25A 120.3 . . ? N122 C26 C25 122.3(2) . . ? N122 C26 H26A 118.9 . . ? C25 C26 H26A 118.9 . . ? C41B B C51B 111.05(15) . . ? C41B B C71B 106.60(14) . . ? C51B B C71B 111.54(14) . . ? C41B B C61B 108.90(15) . . ? C51B B C61B 108.99(14) . . ? C71B B C61B 109.71(14) . . ? C42B C41B C46B 115.41(19) . . ? C42B C41B B 121.92(18) . . ? C46B C41B B 121.70(18) . . ? C43B C42B C41B 123.0(2) . . ? C43B C42B H42A 118.5 . . ? C41B C42B H42A 118.5 . . ? C44B C43B C42B 120.1(3) . . ? C44B C43B H43A 119.9 . . ? C42B C43B H43A 119.9 . . ? C43B C44B C45B 119.9(2) . . ? C43B C44B H44A 120.0 . . ? C45B C44B H44A 120.0 . . ? C44B C45B C46B 119.6(3) . . ? C44B C45B H45A 120.2 . . ? C46B C45B H45A 120.2 . . ? C45B C46B C41B 121.8(2) . . ? C45B C46B H46A 119.1 . . ? C41B C46B H46A 119.1 . . ? C52B C51B C56B 114.83(18) . . ? C52B C51B B 124.28(17) . . ? C56B C51B B 120.80(17) . . ? C53B C52B C51B 122.8(2) . . ? C53B C52B H52A 118.6 . . ? C51B C52B H52A 118.6 . . ? C54B C53B C52B 120.3(2) . . ? C54B C53B H53A 119.9 . . ? C52B C53B H53A 119.9 . . ? C53B C54B C55B 119.4(2) . . ? C53B C54B H54A 120.3 . . ? C55B C54B H54A 120.3 . . ? C56B C55B C54B 119.8(2) . . ? C56B C55B H55A 120.1 . . ? C54B C55B H55A 120.1 . . ? C55B C56B C51B 122.8(2) . . ? C55B C56B H56A 118.6 . . ? C51B C56B H56A 118.6 . . ? C66B C61B C62B 114.70(16) . . ? C66B C61B B 123.24(16) . . ? C62B C61B B 121.87(16) . . ? C63B C62B C61B 123.15(18) . . ? C63B C62B H62A 118.4 . . ? C61B C62B H62A 118.4 . . ? C64B C63B C62B 120.29(18) . . ? C64B C63B H63A 119.9 . . ? C62B C63B H63A 119.9 . . ? C63B C64B C65B 118.71(18) . . ? C63B C64B H64A 120.6 . . ? C65B C64B H64A 120.6 . . ? C64B C65B C66B 120.00(19) . . ? C64B C65B H65A 120.0 . . ? C66B C65B H65A 120.0 . . ? C65B C66B C61B 123.15(18) . . ? C65B C66B H66A 118.4 . . ? C61B C66B H66A 118.4 . . ? C72B C71B C76B 114.20(16) . . ? C72B C71B B 122.32(15) . . ? C76B C71B B 123.44(16) . . ? C73B C72B C71B 123.49(18) . . ? C73B C72B H72A 118.3 . . ? C71B C72B H72A 118.3 . . ? C72B C73B C74B 120.38(19) . . ? C72B C73B H73A 119.8 . . ? C74B C73B H73A 119.8 . . ? C75B C74B C73B 118.20(19) . . ? C75B C74B H74A 120.9 . . ? C73B C74B H74A 120.9 . . ? C74B C75B C76B 120.53(18) . . ? C74B C75B H75A 119.7 . . ? C76B C75B H75A 119.7 . . ? C75B C76B C71B 123.14(18) . . ? C75B C76B H76A 118.4 . . ? C71B C76B H76A 118.4 . . ? C22 N122 C26 118.39(17) . . ? C22 N122 Zn 117.06(12) . . ? C26 N122 Zn 124.48(14) . . ? _diffrn_measured_fraction_theta_max 0.885 _diffrn_reflns_theta_full 29.07 _diffrn_measured_fraction_theta_full 0.885 _refine_diff_density_max 0.544 _refine_diff_density_min -0.304 _refine_diff_density_rms 0.057