# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name _publ_author_address 'Sylvie L. Renard' ; Department of Chemistry, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, UK ; 'Andreas Franken' ; Department of Chemistry, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, UK ; 'Colin A. Kilner' ; Department of Chemistry, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, UK ; 'John D. Kennedy' ; Department of Chemistry, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, UK ; 'Malcolm A. Halcrow' ; Department of Chemistry, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, UK ; _publ_contact_author_name 'Dr. Malcolm A. Halcrow' _publ_contact_author_address ; Department of Chemistry, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, UK ; _publ_contact_author_phone '+44 (0)113 343 6506' _publ_contact_author_fax '+44 (0)113 343 6565' _publ_contact_author_email malcolmh@chem.leeds.ac.uk _publ_requested_journal 'New Journal of Chemistry' _publ_contact_letter ; The following data is for a structure included in a manuscript we have just submitted to the New Journal of Chemistry Editorial Office. ; #======================================================================= # 2. TITLE AND AUTHOR LIST _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Carbaborane Salts of [ZnCl(Hpz^tBu^)~3~]^+^, a receptor for inorganic anions (Hpz^tBu^ = 5-tertbutylpyrazole) ; #================================================================= data_sr43 _database_code_CSD 192037 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Chloro-tris[5-tertbutylpyrazole]zinc(II) bis[nido-undecahydro-7,8-dicarbanonaborato]cobalt(III) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H36 Cl N6 Zn, C4 H22 B18 Co' _chemical_formula_sum 'C25 H58 B18 Cl Co N6 Zn' _chemical_formula_weight 797.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 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' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 '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' 'Cl' 'Cl' 0.1484 0.1585 '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 15.0060(1) _cell_length_b 17.6110(2) _cell_length_c 17.9379(2) _cell_angle_alpha 84.1973(3) _cell_angle_beta 65.6599(4) _cell_angle_gamma 82.3658(5) _cell_volume 4275.19(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 106482 _cell_measurement_theta_min 1.17 _cell_measurement_theta_max 27.50 _exptl_crystal_description Lath _exptl_crystal_colour Orange _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.238 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1656 _exptl_absorpt_coefficient_mu 1.039 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8113 _exptl_absorpt_correction_T_max 0.8681 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _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 'Nonius KappaCCD diffractometer' _diffrn_measurement_method 'Area detector scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 106482 _diffrn_reflns_av_R_equivalents 0.0658 _diffrn_reflns_av_sigmaI/netI 0.0428 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 27.50 _reflns_number_total 19588 _reflns_number_gt 16049 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. There are two formula units in the asymmetric unit, with all four discrete molecules lying on general positions. Slightly high thermal parameters on some methyl C atoms, notably C29 and C61, imply librational motion of their tertbutyl substituents. This was not modelled as disorder, however. The C atoms of the carborane anions were distinguished from the B atoms on account of the short C-C bond lengths of 1.607(3)-1.642(3)\%A, which are clearly shorter than the C-B and B-B bonds in the upper belt of the carborane clusters. All non-H atoms were refined anisotropically, and no restraints were applied. All H atoms were placed in calculated positions and refined using a riding model. ; _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^)+(0.0554P)^2^+1.5233P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0022(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 19588 _refine_ls_number_parameters 939 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0532 _refine_ls_R_factor_gt 0.0365 _refine_ls_wR_factor_ref 0.1040 _refine_ls_wR_factor_gt 0.0947 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 Zn1 Zn 0.583083(15) 0.040080(12) 0.074768(13) 0.02780(6) Uani 1 1 d . . . Cl2 Cl 0.49663(3) -0.06504(3) 0.11635(3) 0.03174(10) Uani 1 1 d . . . N3 N 0.63142(11) 0.04889(9) 0.16278(10) 0.0300(3) Uani 1 1 d . . . N4 N 0.69063(11) 0.09840(9) 0.16824(10) 0.0321(3) Uani 1 1 d . . . H4 H 0.7199 0.1324 0.1291 0.038 Uiso 1 1 calc R . . C5 C 0.69927(13) 0.08926(10) 0.24075(11) 0.0284(4) Uani 1 1 d . . . C6 C 0.64218(14) 0.03184(11) 0.28435(12) 0.0340(4) Uani 1 1 d . . . H6 H 0.6322 0.0119 0.3381 0.041 Uiso 1 1 calc R . . C7 C 0.60204(14) 0.00875(11) 0.23408(12) 0.0324(4) Uani 1 1 d . . . H7 H 0.5592 -0.0305 0.2487 0.039 Uiso 1 1 calc R . . C8 C 0.75926(13) 0.13763(11) 0.26374(12) 0.0313(4) Uani 1 1 d . . . C9 C 0.86324(14) 0.13754(13) 0.19607(13) 0.0405(5) Uani 1 1 d . . . H9A H 0.8933 0.0846 0.1864 0.061 Uiso 1 1 calc R . . H9B H 0.9030 0.1661 0.2130 0.061 Uiso 1 1 calc R . . H9C H 0.8599 0.1619 0.1455 0.061 Uiso 1 1 calc R . . C10 C 0.70819(16) 0.21981(12) 0.27598(15) 0.0439(5) Uani 1 1 d . . . H10A H 0.7071 0.2423 0.2241 0.066 Uiso 1 1 calc R . . H10B H 0.7442 0.2508 0.2943 0.066 Uiso 1 1 calc R . . H10C H 0.6407 0.2188 0.3174 0.066 Uiso 1 1 calc R . . C11 C 0.76506(17) 0.10383(14) 0.34384(13) 0.0436(5) Uani 1 1 d . . . H11A H 0.6986 0.1035 0.3871 0.065 Uiso 1 1 calc R . . H11B H 0.8033 0.1351 0.3595 0.065 Uiso 1 1 calc R . . H11C H 0.7970 0.0512 0.3362 0.065 Uiso 1 1 calc R . . N12 N 0.48823(11) 0.13301(9) 0.08816(9) 0.0299(3) Uani 1 1 d . . . N13 N 0.44850(11) 0.16901(9) 0.03683(9) 0.0299(3) Uani 1 1 d . . . H13 H 0.4630 0.1544 -0.0127 0.036 Uiso 1 1 calc R . . C14 C 0.38440(13) 0.22948(11) 0.07046(12) 0.0304(4) Uani 1 1 d . . . C15 C 0.38215(14) 0.23294(11) 0.14803(12) 0.0353(4) Uani 1 1 d . . . H15 H 0.3439 0.2693 0.1876 0.042 Uiso 1 1 calc R . . C16 C 0.44756(14) 0.17212(11) 0.15587(12) 0.0338(4) Uani 1 1 d . . . H16 H 0.4613 0.1602 0.2031 0.041 Uiso 1 1 calc R . . C17 C 0.32664(14) 0.27754(12) 0.02747(13) 0.0364(4) Uani 1 1 d . . . C18 C 0.22822(17) 0.24481(16) 0.05386(19) 0.0599(7) Uani 1 1 d . . . H18A H 0.2398 0.1914 0.0386 0.090 Uiso 1 1 calc R . . H18B H 0.1895 0.2750 0.0266 0.090 Uiso 1 1 calc R . . H18C H 0.1922 0.2471 0.1134 0.090 Uiso 1 1 calc R . . C19 C 0.38232(18) 0.27635(15) -0.06549(14) 0.0543(6) Uani 1 1 d . . . H19A H 0.4476 0.2933 -0.0815 0.081 Uiso 1 1 calc R . . H19B H 0.3458 0.3109 -0.0918 0.081 Uiso 1 1 calc R . . H19C H 0.3893 0.2241 -0.0828 0.081 Uiso 1 1 calc R . . C20 C 0.3108(2) 0.36053(14) 0.05201(19) 0.0595(7) Uani 1 1 d . . . H20A H 0.2744 0.3625 0.1115 0.089 Uiso 1 1 calc R . . H20B H 0.2731 0.3920 0.0246 0.089 Uiso 1 1 calc R . . H20C H 0.3746 0.3802 0.0357 0.089 Uiso 1 1 calc R . . N21 N 0.70040(11) 0.01276(9) -0.02624(9) 0.0292(3) Uani 1 1 d . . . N22 N 0.70928(11) 0.01940(9) -0.10484(9) 0.0304(3) Uani 1 1 d . . . H22 H 0.6612 0.0378 -0.1197 0.037 Uiso 1 1 calc R . . C23 C 0.80070(13) -0.00558(11) -0.15780(12) 0.0309(4) Uani 1 1 d . . . C24 C 0.85308(14) -0.02900(11) -0.11020(13) 0.0358(4) Uani 1 1 d . . . H24 H 0.9200 -0.0496 -0.1288 0.043 Uiso 1 1 calc R . . C25 C 0.78847(14) -0.01638(11) -0.02983(13) 0.0340(4) Uani 1 1 d . . . H25 H 0.8048 -0.0270 0.0163 0.041 Uiso 1 1 calc R . . C26 C 0.82873(15) -0.00309(12) -0.24871(12) 0.0383(5) Uani 1 1 d . . . C27 C 0.7564(2) -0.04348(18) -0.26624(16) 0.0636(8) Uani 1 1 d . . . H27A H 0.7562 -0.0966 -0.2437 0.095 Uiso 1 1 calc R . . H27B H 0.7760 -0.0432 -0.3256 0.095 Uiso 1 1 calc R . . H27C H 0.6903 -0.0167 -0.2407 0.095 Uiso 1 1 calc R . . C28 C 0.8253(2) 0.08074(15) -0.28172(15) 0.0620(7) Uani 1 1 d . . . H28A H 0.7570 0.1041 -0.2601 0.093 Uiso 1 1 calc R . . H28B H 0.8517 0.0824 -0.3417 0.093 Uiso 1 1 calc R . . H28C H 0.8648 0.1091 -0.2644 0.093 Uiso 1 1 calc R . . C29 C 0.9329(2) -0.0415(2) -0.29130(18) 0.0737(9) Uani 1 1 d . . . H29A H 0.9796 -0.0104 -0.2866 0.111 Uiso 1 1 calc R . . H29B H 0.9477 -0.0462 -0.3493 0.111 Uiso 1 1 calc R . . H29C H 0.9382 -0.0927 -0.2654 0.111 Uiso 1 1 calc R . . Co30 Co 0.899298(16) 0.247730(13) -0.106470(14) 0.02382(6) Uani 1 1 d . . . C31 C 1.01925(13) 0.20365(11) -0.20366(11) 0.0296(4) Uani 1 1 d . . . H31 H 1.0029 0.2168 -0.2594 0.036 Uiso 1 1 calc R . . C32 C 0.96525(14) 0.13931(11) -0.13549(11) 0.0316(4) Uani 1 1 d . . . H32 H 0.9106 0.1062 -0.1424 0.038 Uiso 1 1 calc R . . B33 B 0.94707(17) 0.16119(13) -0.03932(13) 0.0331(5) Uani 1 1 d . . . H33 H 0.8855 0.1441 0.0191 0.040 Uiso 1 1 calc R . . B34 B 1.00133(15) 0.25098(13) -0.05432(13) 0.0311(4) Uani 1 1 d . . . H34 H 0.9776 0.2939 -0.0061 0.037 Uiso 1 1 calc R . . B35 B 1.04399(15) 0.27666(13) -0.16216(13) 0.0300(4) Uani 1 1 d . . . H35 H 1.0472 0.3378 -0.1866 0.036 Uiso 1 1 calc R . . B36 B 1.08698(18) 0.11704(14) -0.20132(15) 0.0396(5) Uani 1 1 d . . . H36 H 1.1142 0.0737 -0.2495 0.048 Uiso 1 1 calc R . . B37 B 1.04262(19) 0.09036(14) -0.09579(15) 0.0412(5) Uani 1 1 d . . . H37 H 1.0411 0.0284 -0.0743 0.049 Uiso 1 1 calc R . . B38 B 1.06806(18) 0.16129(15) -0.04556(15) 0.0402(5) Uani 1 1 d . . . H38 H 1.0846 0.1462 0.0099 0.048 Uiso 1 1 calc R . . B39 B 1.12829(16) 0.23252(15) -0.12160(14) 0.0382(5) Uani 1 1 d . . . H39 H 1.1852 0.2650 -0.1174 0.046 Uiso 1 1 calc R . . B40 B 1.13790(16) 0.20455(14) -0.21722(14) 0.0366(5) Uani 1 1 d . . . H40 H 1.1996 0.2189 -0.2767 0.044 Uiso 1 1 calc R . . B41 B 1.15410(18) 0.13370(16) -0.14491(15) 0.0438(6) Uani 1 1 d . . . H41 H 1.2272 0.1012 -0.1549 0.053 Uiso 1 1 calc R . . C42 C 0.79327(13) 0.25305(11) -0.15141(12) 0.0314(4) Uani 1 1 d . . . H42 H 0.8193 0.2106 -0.2004 0.038 Uiso 1 1 calc R . . C43 C 0.84274(13) 0.33192(10) -0.16579(11) 0.0290(4) Uani 1 1 d . . . H43 H 0.9043 0.3465 -0.2253 0.035 Uiso 1 1 calc R . . B44 B 0.84281(15) 0.36027(12) -0.07724(13) 0.0293(4) Uani 1 1 d . . . H44 H 0.8985 0.3937 -0.0724 0.035 Uiso 1 1 calc R . . B45 B 0.78117(15) 0.28878(13) 0.00034(13) 0.0316(4) Uani 1 1 d . . . H45 H 0.7940 0.2745 0.0576 0.038 Uiso 1 1 calc R . . B46 B 0.75405(16) 0.21931(13) -0.05191(14) 0.0333(5) Uani 1 1 d . . . H46 H 0.7505 0.1575 -0.0300 0.040 Uiso 1 1 calc R . . B47 B 0.72871(17) 0.33635(14) -0.16893(15) 0.0386(5) Uani 1 1 d . . . H47 H 0.7126 0.3514 -0.2246 0.046 Uiso 1 1 calc R . . B48 B 0.75807(16) 0.40476(13) -0.11976(14) 0.0346(5) Uani 1 1 d . . . H48 H 0.7610 0.4661 -0.1435 0.042 Uiso 1 1 calc R . . B49 B 0.71561(16) 0.37788(13) -0.01383(14) 0.0356(5) Uani 1 1 d . . . H49 H 0.6889 0.4218 0.0337 0.043 Uiso 1 1 calc R . . B50 B 0.66027(16) 0.29069(14) 0.00206(15) 0.0378(5) Uani 1 1 d . . . H50 H 0.5965 0.2761 0.0601 0.045 Uiso 1 1 calc R . . B51 B 0.67060(16) 0.26537(14) -0.09458(16) 0.0392(5) Uani 1 1 d . . . H51 H 0.6151 0.2331 -0.1015 0.047 Uiso 1 1 calc R . . B52 B 0.64533(17) 0.36308(14) -0.06993(15) 0.0394(5) Uani 1 1 d . . . H52 H 0.5725 0.3965 -0.0589 0.047 Uiso 1 1 calc R . . Zn53 Zn 0.328448(15) 0.471534(13) 0.562237(13) 0.03062(7) Uani 1 1 d . . . Cl54 Cl 0.39197(3) 0.57842(3) 0.57790(3) 0.03264(10) Uani 1 1 d . . . N55 N 0.18861(11) 0.49540(9) 0.64269(10) 0.0322(3) Uani 1 1 d . . . N56 N 0.17742(11) 0.54020(10) 0.70394(10) 0.0342(4) Uani 1 1 d . . . H56 H 0.2238 0.5663 0.7034 0.041 Uiso 1 1 calc R . . C57 C 0.08770(13) 0.54020(11) 0.76551(11) 0.0302(4) Uani 1 1 d . . . C58 C 0.03781(14) 0.49290(11) 0.74294(12) 0.0347(4) Uani 1 1 d . . . H58 H -0.0278 0.4807 0.7732 0.042 Uiso 1 1 calc R . . C59 C 0.10290(14) 0.46665(11) 0.66702(12) 0.0339(4) Uani 1 1 d . . . H59 H 0.0881 0.4328 0.6367 0.041 Uiso 1 1 calc R . . C60 C 0.06004(14) 0.58628(12) 0.83982(12) 0.0370(4) Uani 1 1 d . . . C61 C 0.1441(2) 0.5787(2) 0.86743(19) 0.0822(11) Uani 1 1 d . . . H61A H 0.1606 0.5245 0.8796 0.123 Uiso 1 1 calc R . . H61B H 0.1242 0.6075 0.9167 0.123 Uiso 1 1 calc R . . H61C H 0.2016 0.5994 0.8237 0.123 Uiso 1 1 calc R . . C62 C 0.0374(2) 0.67078(14) 0.81691(17) 0.0692(8) Uani 1 1 d . . . H62A H 0.0943 0.6882 0.7698 0.104 Uiso 1 1 calc R . . H62B H 0.0231 0.7020 0.8635 0.104 Uiso 1 1 calc R . . H62C H -0.0198 0.6762 0.8028 0.104 Uiso 1 1 calc R . . C63 C -0.03128(19) 0.55938(15) 0.90841(15) 0.0572(7) Uani 1 1 d . . . H63A H -0.0849 0.5643 0.8899 0.086 Uiso 1 1 calc R . . H63B H -0.0502 0.5908 0.9557 0.086 Uiso 1 1 calc R . . H63C H -0.0180 0.5056 0.9242 0.086 Uiso 1 1 calc R . . N64 N 0.37667(11) 0.38433(9) 0.62029(9) 0.0317(3) Uani 1 1 d . . . N65 N 0.46883(11) 0.34763(9) 0.59579(10) 0.0306(3) Uani 1 1 d . . . H65 H 0.5180 0.3592 0.5496 0.037 Uiso 1 1 calc R . . C66 C 0.47643(14) 0.29162(11) 0.65012(11) 0.0313(4) Uani 1 1 d . . . C67 C 0.38441(15) 0.29249(12) 0.71411(12) 0.0387(5) Uani 1 1 d . . . H67 H 0.3655 0.2601 0.7627 0.046 Uiso 1 1 calc R . . C68 C 0.32542(15) 0.35038(12) 0.69283(12) 0.0372(4) Uani 1 1 d . . . H68 H 0.2578 0.3640 0.7254 0.045 Uiso 1 1 calc R . . C69 C 0.57137(15) 0.24181(12) 0.63666(13) 0.0365(4) Uani 1 1 d . . . C70 C 0.63760(19) 0.23795(16) 0.54509(15) 0.0582(7) Uani 1 1 d . . . H70A H 0.6028 0.2176 0.5170 0.087 Uiso 1 1 calc R . . H70B H 0.6978 0.2043 0.5378 0.087 Uiso 1 1 calc R . . H70C H 0.6546 0.2895 0.5219 0.087 Uiso 1 1 calc R . . C71 C 0.5469(2) 0.16026(15) 0.6711(2) 0.0671(8) Uani 1 1 d . . . H71A H 0.5053 0.1613 0.7299 0.101 Uiso 1 1 calc R . . H71B H 0.6079 0.1272 0.6624 0.101 Uiso 1 1 calc R . . H71C H 0.5119 0.1402 0.6429 0.101 Uiso 1 1 calc R . . C72 C 0.6242(2) 0.27421(18) 0.68112(19) 0.0657(7) Uani 1 1 d . . . H72A H 0.6353 0.3276 0.6617 0.099 Uiso 1 1 calc R . . H72B H 0.6875 0.2438 0.6701 0.099 Uiso 1 1 calc R . . H72C H 0.5838 0.2721 0.7402 0.099 Uiso 1 1 calc R . . N73 N 0.33621(11) 0.47658(9) 0.44995(9) 0.0304(3) Uani 1 1 d . . . N74 N 0.41821(11) 0.45836(9) 0.38144(9) 0.0297(3) Uani 1 1 d . . . H74 H 0.4750 0.4389 0.3822 0.036 Uiso 1 1 calc R . . C75 C 0.40258(14) 0.47350(10) 0.31283(11) 0.0299(4) Uani 1 1 d . . . C76 C 0.30484(14) 0.50343(11) 0.33785(12) 0.0352(4) Uani 1 1 d . . . H76 H 0.2706 0.5198 0.3039 0.042 Uiso 1 1 calc R . . C77 C 0.26752(14) 0.50446(11) 0.42248(12) 0.0339(4) Uani 1 1 d . . . H77 H 0.2019 0.5226 0.4564 0.041 Uiso 1 1 calc R . . C78 C 0.48333(15) 0.45870(11) 0.22938(12) 0.0340(4) Uani 1 1 d . . . C79 C 0.55469(17) 0.38980(15) 0.23377(14) 0.0508(6) Uani 1 1 d . . . H79A H 0.5888 0.4015 0.2668 0.076 Uiso 1 1 calc R . . H79B H 0.6029 0.3785 0.1783 0.076 Uiso 1 1 calc R . . H79C H 0.5182 0.3452 0.2589 0.076 Uiso 1 1 calc R . . C80 C 0.5373(2) 0.53071(15) 0.19740(16) 0.0652(8) Uani 1 1 d . . . H80A H 0.4897 0.5754 0.2007 0.098 Uiso 1 1 calc R . . H80B H 0.5839 0.5250 0.1403 0.098 Uiso 1 1 calc R . . H80C H 0.5731 0.5379 0.2308 0.098 Uiso 1 1 calc R . . C81 C 0.43760(19) 0.44187(16) 0.17148(15) 0.0532(6) Uani 1 1 d . . . H81A H 0.4002 0.3972 0.1935 0.080 Uiso 1 1 calc R . . H81B H 0.4898 0.4311 0.1175 0.080 Uiso 1 1 calc R . . H81C H 0.3935 0.4865 0.1664 0.080 Uiso 1 1 calc R . . Co82 Co 0.172282(17) 0.234540(14) 0.481421(14) 0.02693(7) Uani 1 1 d . . . C83 C 0.10370(16) 0.29114(13) 0.41304(13) 0.0419(5) Uani 1 1 d . . . H83 H 0.1618 0.3010 0.3501 0.050 Uiso 1 1 calc R . . C84 C 0.06771(15) 0.20546(14) 0.44681(14) 0.0426(5) Uani 1 1 d . . . H84 H 0.0992 0.1538 0.4091 0.051 Uiso 1 1 calc R . . B85 B 0.03291(16) 0.19517(13) 0.55152(15) 0.0352(5) Uani 1 1 d . . . H85 H 0.0384 0.1399 0.5869 0.042 Uiso 1 1 calc R . . B86 B 0.04948(16) 0.28451(13) 0.58051(14) 0.0352(5) Uani 1 1 d . . . H86 H 0.0654 0.2895 0.6355 0.042 Uiso 1 1 calc R . . B87 B 0.09672(17) 0.34241(13) 0.48966(15) 0.0372(5) Uani 1 1 d . . . H87 H 0.1463 0.3872 0.4831 0.045 Uiso 1 1 calc R . . B88 B -0.0087(2) 0.27295(17) 0.41833(18) 0.0502(6) Uani 1 1 d . . . H88 H -0.0264 0.2687 0.3641 0.060 Uiso 1 1 calc R . . B89 B -0.05630(18) 0.21323(15) 0.50791(18) 0.0436(6) Uani 1 1 d . . . H89 H -0.1064 0.1692 0.5135 0.052 Uiso 1 1 calc R . . B90 B -0.06989(17) 0.26512(15) 0.59195(16) 0.0422(6) Uani 1 1 d . . . H90 H -0.1302 0.2562 0.6540 0.051 Uiso 1 1 calc R . . B91 B -0.02955(19) 0.35645(15) 0.55414(18) 0.0458(6) Uani 1 1 d . . . H91 H -0.0626 0.4086 0.5909 0.055 Uiso 1 1 calc R . . B92 B 0.0082(2) 0.36113(16) 0.44664(19) 0.0510(7) Uani 1 1 d . . . H92 H 0.0014 0.4161 0.4112 0.061 Uiso 1 1 calc R . . B93 B -0.09536(19) 0.31275(16) 0.50989(18) 0.0477(6) Uani 1 1 d . . . H93 H -0.1718 0.3354 0.5173 0.057 Uiso 1 1 calc R . . C94 C 0.25097(14) 0.13033(12) 0.47073(12) 0.0359(4) Uani 1 1 d . . . H94 H 0.2002 0.0867 0.4765 0.043 Uiso 1 1 calc R . . C95 C 0.24014(14) 0.17584(12) 0.54911(12) 0.0352(4) Uani 1 1 d . . . H95 H 0.1819 0.1649 0.6117 0.042 Uiso 1 1 calc R . . B96 B 0.27418(16) 0.26672(14) 0.52033(14) 0.0352(5) Uani 1 1 d . . . H96 H 0.2439 0.3181 0.5586 0.042 Uiso 1 1 calc R . . B97 B 0.31319(16) 0.27443(14) 0.41159(14) 0.0347(5) Uani 1 1 d . . . H97 H 0.3102 0.3303 0.3765 0.042 Uiso 1 1 calc R . . B98 B 0.29394(16) 0.18602(13) 0.38254(13) 0.0334(5) Uani 1 1 d . . . H98 H 0.2766 0.1831 0.3279 0.040 Uiso 1 1 calc R . . B99 B 0.33458(17) 0.10357(16) 0.51357(16) 0.0428(6) Uani 1 1 d . . . H99 H 0.3403 0.0473 0.5473 0.051 Uiso 1 1 calc R . . B100 B 0.35166(17) 0.19098(16) 0.54457(15) 0.0408(5) Uani 1 1 d . . . H100 H 0.3691 0.1926 0.5993 0.049 Uiso 1 1 calc R . . B101 B 0.40147(17) 0.25203(15) 0.45571(15) 0.0391(5) Uani 1 1 d . . . H101 H 0.4536 0.2942 0.4507 0.047 Uiso 1 1 calc R . . B102 B 0.41352(16) 0.20179(15) 0.37027(14) 0.0367(5) Uani 1 1 d . . . H102 H 0.4738 0.2104 0.3082 0.044 Uiso 1 1 calc R . . B103 B 0.37135(17) 0.11074(14) 0.40644(16) 0.0396(5) Uani 1 1 d . . . H103 H 0.4019 0.0590 0.3689 0.048 Uiso 1 1 calc R . . B104 B 0.43858(17) 0.15131(16) 0.45177(15) 0.0412(5) Uani 1 1 d . . . H104 H 0.5146 0.1272 0.4441 0.049 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 Zn1 0.02733(11) 0.03130(12) 0.02587(11) -0.00153(8) -0.01180(9) -0.00311(8) Cl2 0.0321(2) 0.0338(2) 0.0319(2) -0.00114(18) -0.01460(18) -0.00693(17) N3 0.0298(8) 0.0332(8) 0.0288(8) 0.0005(6) -0.0132(6) -0.0067(6) N4 0.0335(8) 0.0366(9) 0.0294(8) 0.0044(7) -0.0145(7) -0.0129(7) C5 0.0268(9) 0.0326(9) 0.0262(9) -0.0032(7) -0.0115(7) 0.0002(7) C6 0.0400(10) 0.0367(10) 0.0268(10) 0.0024(8) -0.0147(8) -0.0080(8) C7 0.0352(10) 0.0328(10) 0.0298(10) 0.0022(8) -0.0132(8) -0.0085(8) C8 0.0280(9) 0.0374(10) 0.0305(10) -0.0044(8) -0.0129(8) -0.0042(7) C9 0.0321(10) 0.0499(12) 0.0401(12) -0.0083(9) -0.0125(9) -0.0084(9) C10 0.0381(11) 0.0389(11) 0.0562(14) -0.0120(10) -0.0183(10) -0.0040(9) C11 0.0485(12) 0.0551(13) 0.0360(11) -0.0002(10) -0.0236(10) -0.0148(10) N12 0.0316(8) 0.0332(8) 0.0250(8) -0.0001(6) -0.0125(6) -0.0017(6) N13 0.0311(8) 0.0358(8) 0.0239(8) -0.0046(6) -0.0128(6) 0.0007(6) C14 0.0242(9) 0.0327(10) 0.0321(10) -0.0012(8) -0.0092(7) -0.0032(7) C15 0.0362(10) 0.0365(10) 0.0284(10) -0.0061(8) -0.0085(8) 0.0001(8) C16 0.0395(10) 0.0375(10) 0.0234(9) -0.0015(8) -0.0119(8) -0.0035(8) C17 0.0333(10) 0.0374(11) 0.0404(11) -0.0047(9) -0.0179(9) 0.0021(8) C18 0.0400(13) 0.0718(17) 0.0758(19) 0.0092(14) -0.0325(13) -0.0105(12) C19 0.0527(14) 0.0656(16) 0.0415(13) 0.0065(11) -0.0236(11) 0.0132(12) C20 0.0716(17) 0.0433(13) 0.0770(19) -0.0102(12) -0.0476(15) 0.0135(12) N21 0.0297(8) 0.0316(8) 0.0266(8) -0.0004(6) -0.0117(6) -0.0037(6) N22 0.0271(8) 0.0376(9) 0.0266(8) -0.0024(6) -0.0109(6) -0.0028(6) C23 0.0277(9) 0.0304(9) 0.0321(10) -0.0043(8) -0.0080(7) -0.0061(7) C24 0.0265(9) 0.0361(10) 0.0410(11) 0.0000(8) -0.0109(8) -0.0005(8) C25 0.0323(10) 0.0340(10) 0.0360(11) 0.0038(8) -0.0161(8) -0.0014(8) C26 0.0369(10) 0.0441(12) 0.0314(10) -0.0079(9) -0.0081(8) -0.0103(9) C27 0.0639(16) 0.090(2) 0.0403(13) -0.0170(13) -0.0134(12) -0.0332(15) C28 0.091(2) 0.0545(15) 0.0349(13) 0.0010(11) -0.0183(13) -0.0176(14) C29 0.0485(15) 0.113(3) 0.0459(15) -0.0225(16) -0.0072(12) 0.0125(15) Co30 0.02339(12) 0.02571(12) 0.02089(12) -0.00052(9) -0.00767(9) -0.00234(9) C31 0.0288(9) 0.0349(10) 0.0231(9) -0.0035(7) -0.0089(7) -0.0001(7) C32 0.0346(10) 0.0290(9) 0.0285(10) -0.0021(7) -0.0106(8) -0.0005(7) B33 0.0370(11) 0.0345(11) 0.0244(10) -0.0001(8) -0.0110(9) 0.0024(9) B34 0.0284(10) 0.0387(12) 0.0268(10) -0.0053(9) -0.0120(8) 0.0005(8) B35 0.0244(10) 0.0360(11) 0.0281(11) -0.0016(8) -0.0086(8) -0.0049(8) B36 0.0402(12) 0.0420(13) 0.0313(12) -0.0098(10) -0.0115(10) 0.0101(10) B37 0.0467(13) 0.0369(12) 0.0343(12) -0.0010(10) -0.0156(10) 0.0113(10) B38 0.0387(12) 0.0500(14) 0.0310(12) -0.0046(10) -0.0171(10) 0.0102(10) B39 0.0276(11) 0.0558(15) 0.0314(12) -0.0081(10) -0.0126(9) 0.0022(10) B40 0.0261(10) 0.0495(14) 0.0287(11) -0.0061(10) -0.0066(9) 0.0026(9) B41 0.0378(12) 0.0561(15) 0.0353(13) -0.0090(11) -0.0166(10) 0.0136(11) C42 0.0286(9) 0.0339(10) 0.0333(10) -0.0013(8) -0.0138(8) -0.0044(7) C43 0.0277(9) 0.0318(9) 0.0265(9) 0.0023(7) -0.0107(7) -0.0031(7) B44 0.0293(10) 0.0286(10) 0.0282(10) -0.0027(8) -0.0099(8) -0.0018(8) B45 0.0284(10) 0.0353(11) 0.0256(10) -0.0009(8) -0.0058(8) -0.0023(8) B46 0.0284(10) 0.0343(11) 0.0338(12) 0.0032(9) -0.0090(9) -0.0077(8) B47 0.0318(11) 0.0460(13) 0.0399(13) 0.0001(10) -0.0180(10) 0.0003(10) B48 0.0318(11) 0.0314(11) 0.0366(12) 0.0016(9) -0.0121(9) 0.0018(9) B49 0.0302(11) 0.0354(12) 0.0347(12) -0.0053(9) -0.0073(9) 0.0012(9) B50 0.0266(10) 0.0425(13) 0.0358(12) 0.0013(10) -0.0044(9) -0.0048(9) B51 0.0274(11) 0.0436(13) 0.0469(14) -0.0019(11) -0.0147(10) -0.0059(9) B52 0.0278(11) 0.0438(13) 0.0421(13) -0.0012(10) -0.0114(10) 0.0017(9) Zn53 0.02712(11) 0.03785(13) 0.02377(12) -0.00243(9) -0.00724(9) -0.00234(9) Cl54 0.0281(2) 0.0398(2) 0.0287(2) 0.00147(18) -0.00943(17) -0.00844(18) N55 0.0292(8) 0.0369(9) 0.0285(8) -0.0076(7) -0.0079(6) -0.0046(6) N56 0.0270(8) 0.0420(9) 0.0307(8) -0.0098(7) -0.0055(6) -0.0089(7) C57 0.0262(9) 0.0317(9) 0.0279(9) -0.0003(7) -0.0061(7) -0.0037(7) C58 0.0271(9) 0.0380(10) 0.0345(10) -0.0020(8) -0.0068(8) -0.0074(8) C59 0.0307(9) 0.0363(10) 0.0349(10) -0.0043(8) -0.0120(8) -0.0066(8) C60 0.0334(10) 0.0414(11) 0.0305(10) -0.0075(8) -0.0048(8) -0.0076(8) C61 0.0538(16) 0.136(3) 0.0649(19) -0.057(2) -0.0269(14) 0.0120(17) C62 0.100(2) 0.0402(13) 0.0465(15) -0.0098(11) -0.0057(14) -0.0100(14) C63 0.0562(15) 0.0583(15) 0.0391(13) -0.0134(11) 0.0055(11) -0.0202(12) N64 0.0292(8) 0.0371(9) 0.0257(8) -0.0009(7) -0.0074(6) -0.0053(6) N65 0.0268(8) 0.0361(9) 0.0258(8) 0.0016(6) -0.0073(6) -0.0060(6) C66 0.0363(10) 0.0330(10) 0.0283(9) 0.0029(8) -0.0157(8) -0.0102(8) C67 0.0403(11) 0.0459(12) 0.0269(10) 0.0087(8) -0.0106(8) -0.0129(9) C68 0.0325(10) 0.0457(12) 0.0276(10) 0.0016(8) -0.0056(8) -0.0090(8) C69 0.0351(10) 0.0390(11) 0.0384(11) 0.0044(9) -0.0189(9) -0.0052(8) C70 0.0515(14) 0.0675(17) 0.0467(14) -0.0040(12) -0.0173(11) 0.0163(12) C71 0.0600(16) 0.0509(15) 0.090(2) 0.0228(14) -0.0345(16) -0.0090(12) C72 0.0520(15) 0.082(2) 0.078(2) -0.0180(16) -0.0406(15) -0.0007(13) N73 0.0274(8) 0.0357(8) 0.0249(8) -0.0046(6) -0.0081(6) 0.0009(6) N74 0.0262(7) 0.0352(8) 0.0256(8) -0.0028(6) -0.0093(6) 0.0013(6) C75 0.0347(10) 0.0292(9) 0.0264(9) 0.0004(7) -0.0131(8) -0.0042(7) C76 0.0349(10) 0.0376(10) 0.0341(10) 0.0000(8) -0.0174(8) 0.0027(8) C77 0.0292(9) 0.0330(10) 0.0374(11) -0.0032(8) -0.0126(8) 0.0026(7) C78 0.0379(10) 0.0364(10) 0.0255(9) -0.0026(8) -0.0113(8) -0.0012(8) C79 0.0459(13) 0.0648(15) 0.0310(11) -0.0038(10) -0.0109(10) 0.0153(11) C80 0.0741(18) 0.0565(15) 0.0418(14) -0.0073(12) 0.0068(12) -0.0265(13) C81 0.0568(14) 0.0684(16) 0.0380(12) -0.0151(11) -0.0244(11) 0.0086(12) Co82 0.02663(13) 0.03213(14) 0.02212(13) -0.00137(10) -0.00889(10) -0.00654(10) C83 0.0412(11) 0.0529(13) 0.0346(11) 0.0057(9) -0.0192(9) -0.0078(10) C84 0.0349(11) 0.0558(13) 0.0426(12) -0.0081(10) -0.0191(9) -0.0070(9) B85 0.0269(10) 0.0361(12) 0.0388(12) 0.0006(9) -0.0087(9) -0.0073(9) B86 0.0312(11) 0.0398(12) 0.0327(12) -0.0066(9) -0.0108(9) -0.0005(9) B87 0.0336(11) 0.0339(12) 0.0433(13) 0.0035(10) -0.0153(10) -0.0057(9) B88 0.0454(14) 0.0662(18) 0.0485(15) -0.0039(13) -0.0295(12) -0.0013(12) B89 0.0316(12) 0.0448(14) 0.0587(16) -0.0077(12) -0.0206(11) -0.0062(10) B90 0.0291(11) 0.0467(14) 0.0449(14) -0.0033(11) -0.0092(10) -0.0022(10) B91 0.0416(13) 0.0393(13) 0.0580(17) -0.0091(12) -0.0219(12) 0.0021(10) B92 0.0502(15) 0.0479(15) 0.0585(17) 0.0109(13) -0.0295(13) -0.0023(12) B93 0.0380(13) 0.0478(15) 0.0608(17) -0.0060(12) -0.0244(12) 0.0019(11) C94 0.0324(10) 0.0395(11) 0.0322(10) -0.0033(8) -0.0095(8) -0.0017(8) C95 0.0305(9) 0.0482(12) 0.0250(9) 0.0007(8) -0.0101(8) -0.0030(8) B96 0.0298(11) 0.0501(13) 0.0293(11) -0.0064(10) -0.0133(9) -0.0085(9) B97 0.0311(11) 0.0431(13) 0.0288(11) -0.0017(9) -0.0079(9) -0.0144(9) B98 0.0313(11) 0.0444(12) 0.0231(10) -0.0053(9) -0.0073(8) -0.0095(9) B99 0.0325(12) 0.0498(14) 0.0411(14) 0.0036(11) -0.0128(10) 0.0007(10) B100 0.0301(11) 0.0641(16) 0.0290(12) -0.0060(11) -0.0123(9) -0.0035(10) B101 0.0321(11) 0.0532(14) 0.0324(12) -0.0097(10) -0.0099(9) -0.0108(10) B102 0.0311(11) 0.0524(14) 0.0239(11) -0.0060(9) -0.0052(8) -0.0119(10) B103 0.0304(11) 0.0432(13) 0.0416(13) -0.0111(10) -0.0095(10) -0.0020(9) B104 0.0289(11) 0.0572(15) 0.0353(12) -0.0062(11) -0.0104(9) -0.0025(10) _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 N21 1.9839(15) . ? Zn1 N12 1.9852(15) . ? Zn1 N3 2.0164(15) . ? Zn1 Cl2 2.2865(5) . ? N3 C7 1.329(2) . ? N3 N4 1.362(2) . ? N4 C5 1.351(2) . ? C5 C6 1.373(3) . ? C5 C8 1.512(3) . ? C6 C7 1.389(3) . ? C8 C11 1.531(3) . ? C8 C9 1.532(3) . ? C8 C10 1.536(3) . ? N12 C16 1.330(2) . ? N12 N13 1.356(2) . ? N13 C14 1.343(2) . ? C14 C15 1.385(3) . ? C14 C17 1.512(3) . ? C15 C16 1.391(3) . ? C17 C18 1.527(3) . ? C17 C19 1.527(3) . ? C17 C20 1.529(3) . ? N21 C25 1.331(2) . ? N21 N22 1.355(2) . ? N22 C23 1.352(2) . ? C23 C24 1.383(3) . ? C23 C26 1.504(3) . ? C24 C25 1.387(3) . ? C26 C27 1.522(3) . ? C26 C29 1.524(3) . ? C26 C28 1.537(3) . ? Co30 C43 2.0352(18) . ? Co30 C32 2.0421(18) . ? Co30 C42 2.0476(18) . ? Co30 C31 2.0488(18) . ? Co30 B44 2.078(2) . ? Co30 B33 2.083(2) . ? Co30 B35 2.092(2) . ? Co30 B46 2.096(2) . ? Co30 B34 2.106(2) . ? Co30 B45 2.116(2) . ? C31 C32 1.607(3) . ? C31 B40 1.697(3) . ? C31 B35 1.701(3) . ? C31 B36 1.724(3) . ? C32 B37 1.700(3) . ? C32 B33 1.708(3) . ? C32 B36 1.735(3) . ? B33 B38 1.773(3) . ? B33 B37 1.795(3) . ? B33 B34 1.820(3) . ? B34 B38 1.784(3) . ? B34 B39 1.792(3) . ? B34 B35 1.799(3) . ? B35 B39 1.765(3) . ? B35 B40 1.790(3) . ? B36 B40 1.756(4) . ? B36 B41 1.761(4) . ? B36 B37 1.764(3) . ? B37 B41 1.774(4) . ? B37 B38 1.776(4) . ? B38 B39 1.786(4) . ? B38 B41 1.786(3) . ? B39 B40 1.776(3) . ? B39 B41 1.786(4) . ? B40 B41 1.775(3) . ? C42 C43 1.610(3) . ? C42 B51 1.693(3) . ? C42 B46 1.702(3) . ? C42 B47 1.723(3) . ? C43 B48 1.691(3) . ? C43 B44 1.713(3) . ? C43 B47 1.726(3) . ? B44 B49 1.777(3) . ? B44 B48 1.796(3) . ? B44 B45 1.809(3) . ? B45 B49 1.792(3) . ? B45 B46 1.794(3) . ? B45 B50 1.798(3) . ? B46 B50 1.775(3) . ? B46 B51 1.791(3) . ? B47 B51 1.759(3) . ? B47 B48 1.761(3) . ? B47 B52 1.767(3) . ? B48 B49 1.772(3) . ? B48 B52 1.775(3) . ? B49 B50 1.784(3) . ? B49 B52 1.787(3) . ? B50 B51 1.773(4) . ? B50 B52 1.781(3) . ? B51 B52 1.773(3) . ? Zn53 N73 1.9625(16) . ? Zn53 N64 1.9924(16) . ? Zn53 N55 2.0136(16) . ? Zn53 Cl54 2.3098(5) . ? N55 C59 1.329(2) . ? N55 N56 1.359(2) . ? N56 C57 1.344(2) . ? C57 C58 1.379(3) . ? C57 C60 1.510(3) . ? C58 C59 1.390(3) . ? C60 C63 1.510(3) . ? C60 C61 1.520(3) . ? C60 C62 1.535(3) . ? N64 C68 1.335(2) . ? N64 N65 1.357(2) . ? N65 C66 1.343(2) . ? C66 C67 1.384(3) . ? C66 C69 1.512(3) . ? C67 C68 1.389(3) . ? C69 C72 1.525(3) . ? C69 C70 1.533(3) . ? C69 C71 1.534(3) . ? N73 C77 1.335(2) . ? N73 N74 1.362(2) . ? N74 C75 1.340(2) . ? C75 C76 1.389(3) . ? C75 C78 1.509(3) . ? C76 C77 1.386(3) . ? C78 C79 1.526(3) . ? C78 C80 1.529(3) . ? C78 C81 1.530(3) . ? Co82 C95 2.016(2) . ? Co82 C83 2.019(2) . ? Co82 C94 2.027(2) . ? Co82 C84 2.047(2) . ? Co82 B87 2.065(2) . ? Co82 B96 2.082(2) . ? Co82 B98 2.105(2) . ? Co82 B85 2.116(2) . ? Co82 B86 2.125(2) . ? Co82 B97 2.137(2) . ? C83 C84 1.642(3) . ? C83 B87 1.680(3) . ? C83 B92 1.704(4) . ? C83 B88 1.721(3) . ? C84 B89 1.722(3) . ? C84 B85 1.727(3) . ? C84 B88 1.728(3) . ? B85 B90 1.782(3) . ? B85 B86 1.784(3) . ? B85 B89 1.790(3) . ? B86 B87 1.761(3) . ? B86 B91 1.782(3) . ? B86 B90 1.792(3) . ? B87 B91 1.765(3) . ? B87 B92 1.773(4) . ? B88 B92 1.762(4) . ? B88 B93 1.763(4) . ? B88 B89 1.764(4) . ? B89 B90 1.768(4) . ? B89 B93 1.772(4) . ? B90 B91 1.764(4) . ? B90 B93 1.774(4) . ? B91 B92 1.768(4) . ? B91 B93 1.780(4) . ? B92 B93 1.770(4) . ? C94 C95 1.628(3) . ? C94 B98 1.701(3) . ? C94 B103 1.706(3) . ? C94 B99 1.718(3) . ? C95 B100 1.697(3) . ? C95 B96 1.709(3) . ? C95 B99 1.725(3) . ? B96 B101 1.779(3) . ? B96 B97 1.787(3) . ? B96 B100 1.791(3) . ? B97 B98 1.785(3) . ? B97 B101 1.789(3) . ? B97 B102 1.793(3) . ? B98 B102 1.772(3) . ? B98 B103 1.782(3) . ? B99 B104 1.762(3) . ? B99 B103 1.763(4) . ? B99 B100 1.772(4) . ? B100 B101 1.772(4) . ? B100 B104 1.779(3) . ? B101 B102 1.780(3) . ? B101 B104 1.787(4) . ? B102 B103 1.764(3) . ? B102 B104 1.781(4) . ? B103 B104 1.782(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 N21 Zn1 N12 126.26(6) . . ? N21 Zn1 N3 107.00(6) . . ? N12 Zn1 N3 102.41(6) . . ? N21 Zn1 Cl2 106.42(5) . . ? N12 Zn1 Cl2 108.28(5) . . ? N3 Zn1 Cl2 104.58(5) . . ? C7 N3 N4 104.76(15) . . ? C7 N3 Zn1 124.45(13) . . ? N4 N3 Zn1 130.55(12) . . ? C5 N4 N3 112.13(15) . . ? N4 C5 C6 105.84(16) . . ? N4 C5 C8 123.29(17) . . ? C6 C5 C8 130.84(17) . . ? C5 C6 C7 106.24(17) . . ? N3 C7 C6 111.02(17) . . ? C5 C8 C11 108.88(16) . . ? C5 C8 C9 109.92(16) . . ? C11 C8 C9 109.37(17) . . ? C5 C8 C10 108.84(15) . . ? C11 C8 C10 109.48(17) . . ? C9 C8 C10 110.33(17) . . ? C16 N12 N13 105.34(15) . . ? C16 N12 Zn1 123.83(13) . . ? N13 N12 Zn1 130.81(12) . . ? C14 N13 N12 112.06(15) . . ? N13 C14 C15 106.16(16) . . ? N13 C14 C17 122.74(17) . . ? C15 C14 C17 131.03(17) . . ? C14 C15 C16 105.70(17) . . ? N12 C16 C15 110.74(17) . . ? C14 C17 C18 107.99(18) . . ? C14 C17 C19 111.04(16) . . ? C18 C17 C19 110.0(2) . . ? C14 C17 C20 108.95(17) . . ? C18 C17 C20 110.6(2) . . ? C19 C17 C20 108.3(2) . . ? C25 N21 N22 105.47(15) . . ? C25 N21 Zn1 125.93(13) . . ? N22 N21 Zn1 128.59(12) . . ? C23 N22 N21 112.01(15) . . ? N22 C23 C24 105.64(17) . . ? N22 C23 C26 121.81(17) . . ? C24 C23 C26 132.54(17) . . ? C23 C24 C25 106.31(17) . . ? N21 C25 C24 110.57(18) . . ? C23 C26 C27 109.65(17) . . ? C23 C26 C29 109.63(19) . . ? C27 C26 C29 110.4(2) . . ? C23 C26 C28 109.63(17) . . ? C27 C26 C28 108.7(2) . . ? C29 C26 C28 108.8(2) . . ? C43 Co30 C32 132.94(8) . . ? C43 Co30 C42 46.44(7) . . ? C32 Co30 C42 100.40(8) . . ? C43 Co30 C31 100.21(7) . . ? C32 Co30 C31 46.26(7) . . ? C42 Co30 C31 100.33(8) . . ? C43 Co30 B44 49.20(8) . . ? C32 Co30 B44 175.40(8) . . ? C42 Co30 B44 83.75(8) . . ? C31 Co30 B44 131.29(8) . . ? C43 Co30 B33 175.91(8) . . ? C32 Co30 B33 48.91(8) . . ? C42 Co30 B33 131.32(8) . . ? C31 Co30 B33 83.44(8) . . ? B44 Co30 B33 129.30(9) . . ? C43 Co30 B35 96.22(8) . . ? C32 Co30 B35 83.21(8) . . ? C42 Co30 B35 130.82(8) . . ? C31 Co30 B35 48.50(8) . . ? B44 Co30 B35 92.58(8) . . ? B33 Co30 B35 87.57(9) . . ? C43 Co30 B46 83.17(8) . . ? C32 Co30 B46 96.98(8) . . ? C42 Co30 B46 48.50(8) . . ? C31 Co30 B46 131.27(8) . . ? B44 Co30 B46 87.26(9) . . ? B33 Co30 B46 93.05(9) . . ? B35 Co30 B46 179.32(9) . . ? C43 Co30 B34 130.41(8) . . ? C32 Co30 B34 84.56(8) . . ? C42 Co30 B34 174.86(8) . . ? C31 Co30 B34 84.06(8) . . ? B44 Co30 B34 91.35(8) . . ? B33 Co30 B34 51.49(9) . . ? B35 Co30 B34 50.74(8) . . ? B46 Co30 B34 129.93(9) . . ? C43 Co30 B45 84.35(8) . . ? C32 Co30 B45 130.98(8) . . ? C42 Co30 B45 83.90(8) . . ? C31 Co30 B45 175.19(8) . . ? B44 Co30 B45 51.08(8) . . ? B33 Co30 B45 92.06(9) . . ? B35 Co30 B45 129.85(9) . . ? B46 Co30 B45 50.44(9) . . ? B34 Co30 B45 91.82(8) . . ? C32 C31 B40 111.95(15) . . ? C32 C31 B35 112.12(14) . . ? B40 C31 B35 63.59(12) . . ? C32 C31 B36 62.67(12) . . ? B40 C31 B36 61.78(14) . . ? B35 C31 B36 115.13(15) . . ? C32 C31 Co30 66.65(9) . . ? B40 C31 Co30 124.98(13) . . ? B35 C31 Co30 67.06(9) . . ? B36 C31 Co30 125.22(13) . . ? C31 C32 B37 111.11(16) . . ? C31 C32 B33 112.04(15) . . ? B37 C32 B33 63.56(13) . . ? C31 C32 B36 61.97(12) . . ? B37 C32 B36 61.79(13) . . ? B33 C32 B36 115.20(16) . . ? C31 C32 Co30 67.09(9) . . ? B37 C32 Co30 124.49(14) . . ? B33 C32 Co30 66.79(10) . . ? B36 C32 Co30 124.99(13) . . ? C32 B33 B38 103.46(15) . . ? C32 B33 B37 58.00(12) . . ? B38 B33 B37 59.73(14) . . ? C32 B33 B34 104.57(15) . . ? B38 B33 B34 59.53(13) . . ? B37 B33 B34 107.71(16) . . ? C32 B33 Co30 64.30(9) . . ? B38 B33 Co30 117.11(14) . . ? B37 B33 Co30 117.34(13) . . ? B34 B33 Co30 64.93(10) . . ? B38 B34 B39 59.93(13) . . ? B38 B34 B35 106.15(15) . . ? B39 B34 B35 58.90(12) . . ? B38 B34 B33 58.92(13) . . ? B39 B34 B33 106.51(15) . . ? B35 B34 B33 105.93(14) . . ? B38 B34 Co30 115.42(14) . . ? B39 B34 Co30 115.97(13) . . ? B35 B34 Co30 64.20(9) . . ? B33 B34 Co30 63.58(9) . . ? C31 B35 B39 103.97(16) . . ? C31 B35 B40 58.10(12) . . ? B39 B35 B40 59.92(13) . . ? C31 B35 B34 105.28(15) . . ? B39 B35 B34 60.36(12) . . ? B40 B35 B34 108.73(15) . . ? C31 B35 Co30 64.43(9) . . ? B39 B35 Co30 117.96(14) . . ? B40 B35 Co30 117.72(14) . . ? B34 B35 Co30 65.06(9) . . ? C31 B36 C32 55.37(11) . . ? C31 B36 B40 58.35(12) . . ? C32 B36 B40 103.33(15) . . ? C31 B36 B41 104.12(17) . . ? C32 B36 B41 104.11(16) . . ? B40 B36 B41 60.60(15) . . ? C31 B36 B37 102.89(15) . . ? C32 B36 B37 58.13(12) . . ? B40 B36 B37 108.32(17) . . ? B41 B36 B37 60.41(15) . . ? C32 B37 B36 60.08(13) . . ? C32 B37 B41 105.07(17) . . ? B36 B37 B41 59.73(14) . . ? C32 B37 B38 103.63(16) . . ? B36 B37 B38 108.17(18) . . ? B41 B37 B38 60.42(15) . . ? C32 B37 B33 58.44(12) . . ? B36 B37 B33 109.54(16) . . ? B41 B37 B33 108.71(18) . . ? B38 B37 B33 59.52(13) . . ? B33 B38 B37 60.76(13) . . ? B33 B38 B34 61.55(12) . . ? B37 B38 B34 110.13(16) . . ? B33 B38 B39 108.82(16) . . ? B37 B38 B39 107.61(17) . . ? B34 B38 B39 60.26(13) . . ? B33 B38 B41 109.13(17) . . ? B37 B38 B41 59.71(15) . . ? B34 B38 B41 109.61(17) . . ? B39 B38 B41 59.98(14) . . ? B35 B39 B40 60.74(12) . . ? B35 B39 B41 108.67(16) . . ? B40 B39 B41 59.79(14) . . ? B35 B39 B38 107.49(16) . . ? B40 B39 B38 107.38(18) . . ? B41 B39 B38 60.02(14) . . ? B35 B39 B34 60.74(12) . . ? B40 B39 B34 109.69(15) . . ? B41 B39 B34 109.28(17) . . ? B38 B39 B34 59.81(13) . . ? C31 B40 B36 59.87(13) . . ? C31 B40 B41 104.67(17) . . ? B36 B40 B41 59.84(14) . . ? C31 B40 B39 103.70(15) . . ? B36 B40 B39 108.51(17) . . ? B41 B40 B39 60.38(14) . . ? C31 B40 B35 58.32(11) . . ? B36 B40 B35 109.18(15) . . ? B41 B40 B35 108.04(16) . . ? B39 B40 B35 59.35(12) . . ? B36 B41 B37 59.87(14) . . ? B36 B41 B40 59.56(14) . . ? B37 B41 B40 107.07(17) . . ? B36 B41 B39 107.85(16) . . ? B37 B41 B39 107.75(16) . . ? B40 B41 B39 59.83(14) . . ? B36 B41 B38 107.84(17) . . ? B37 B41 B38 59.87(14) . . ? B40 B41 B38 107.41(16) . . ? B39 B41 B38 60.01(14) . . ? C43 C42 B51 111.55(15) . . ? C43 C42 B46 111.74(15) . . ? B51 C42 B46 63.66(13) . . ? C43 C42 B47 62.28(12) . . ? B51 C42 B47 61.99(13) . . ? B46 C42 B47 115.29(16) . . ? C43 C42 Co30 66.37(9) . . ? B51 C42 Co30 125.10(14) . . ? B46 C42 Co30 67.22(10) . . ? B47 C42 Co30 124.83(13) . . ? C42 C43 B48 111.29(15) . . ? C42 C43 B44 111.93(14) . . ? B48 C43 B44 63.71(12) . . ? C42 C43 B47 62.09(12) . . ? B48 C43 B47 62.02(13) . . ? B44 C43 B47 115.57(15) . . ? C42 C43 Co30 67.19(9) . . ? B48 C43 Co30 124.75(13) . . ? B44 C43 Co30 66.71(9) . . ? B47 C43 Co30 125.40(13) . . ? C43 B44 B49 103.13(15) . . ? C43 B44 B48 57.54(12) . . ? B49 B44 B48 59.47(12) . . ? C43 B44 B45 104.64(14) . . ? B49 B44 B45 59.95(12) . . ? B48 B44 B45 107.68(15) . . ? C43 B44 Co30 64.09(9) . . ? B49 B44 Co30 117.87(13) . . ? B48 B44 Co30 116.89(13) . . ? B45 B44 Co30 65.53(9) . . ? B49 B45 B46 106.26(16) . . ? B49 B45 B50 59.62(13) . . ? B46 B45 B50 59.23(13) . . ? B49 B45 B44 59.15(12) . . ? B46 B45 B44 106.13(15) . . ? B50 B45 B44 106.55(15) . . ? B49 B45 Co30 115.32(13) . . ? B46 B45 Co30 64.20(10) . . ? B50 B45 Co30 116.06(14) . . ? B44 B45 Co30 63.39(9) . . ? C42 B46 B50 103.80(16) . . ? C42 B46 B51 57.92(12) . . ? B50 B46 B51 59.64(13) . . ? C42 B46 B45 105.48(15) . . ? B50 B46 B45 60.48(13) . . ? B51 B46 B45 108.59(16) . . ? C42 B46 Co30 64.28(9) . . ? B50 B46 Co30 118.12(14) . . ? B51 B46 Co30 117.35(14) . . ? B45 B46 Co30 65.36(10) . . ? C42 B47 C43 55.63(11) . . ? C42 B47 B51 58.17(12) . . ? C43 B47 B51 103.17(16) . . ? C42 B47 B48 102.91(15) . . ? C43 B47 B48 57.99(12) . . ? B51 B47 B48 107.87(17) . . ? C42 B47 B52 104.10(16) . . ? C43 B47 B52 104.15(16) . . ? B51 B47 B52 60.36(14) . . ? B48 B47 B52 60.43(14) . . ? C43 B48 B47 59.99(12) . . ? C43 B48 B49 104.25(15) . . ? B47 B48 B49 108.64(17) . . ? C43 B48 B52 105.31(16) . . ? B47 B48 B52 59.96(14) . . ? B49 B48 B52 60.50(13) . . ? C43 B48 B44 58.75(11) . . ? B47 B48 B44 109.78(15) . . ? B49 B48 B44 59.72(12) . . ? B52 B48 B44 108.90(16) . . ? B48 B49 B44 60.81(12) . . ? B48 B49 B50 107.41(17) . . ? B44 B49 B50 108.52(15) . . ? B48 B49 B52 59.83(13) . . ? B44 B49 B52 109.23(16) . . ? B50 B49 B52 59.84(14) . . ? B48 B49 B45 109.51(15) . . ? B44 B49 B45 60.90(12) . . ? B50 B49 B45 60.36(13) . . ? B52 B49 B45 109.42(16) . . ? B51 B50 B46 60.62(13) . . ? B51 B50 B52 59.83(14) . . ? B46 B50 B52 108.67(17) . . ? B51 B50 B49 107.42(17) . . ? B46 B50 B49 107.41(15) . . ? B52 B50 B49 60.16(14) . . ? B51 B50 B45 109.22(15) . . ? B46 B50 B45 60.29(12) . . ? B52 B50 B45 109.40(16) . . ? B49 B50 B45 60.02(13) . . ? C42 B51 B47 59.85(12) . . ? C42 B51 B52 105.12(16) . . ? B47 B51 B52 60.03(14) . . ? C42 B51 B50 104.26(16) . . ? B47 B51 B50 108.63(17) . . ? B52 B51 B50 60.31(14) . . ? C42 B51 B46 58.42(12) . . ? B47 B51 B46 109.19(15) . . ? B52 B51 B46 108.35(17) . . ? B50 B51 B46 59.74(13) . . ? B47 B52 B51 59.61(14) . . ? B47 B52 B48 59.61(13) . . ? B51 B52 B48 106.65(16) . . ? B47 B52 B50 107.94(16) . . ? B51 B52 B50 59.86(14) . . ? B48 B52 B50 107.42(16) . . ? B47 B52 B49 107.70(16) . . ? B51 B52 B49 107.32(16) . . ? B48 B52 B49 59.67(13) . . ? B50 B52 B49 60.00(14) . . ? N73 Zn53 N64 127.75(6) . . ? N73 Zn53 N55 110.65(6) . . ? N64 Zn53 N55 102.12(7) . . ? N73 Zn53 Cl54 108.07(5) . . ? N64 Zn53 Cl54 106.08(5) . . ? N55 Zn53 Cl54 98.21(5) . . ? C59 N55 N56 104.80(15) . . ? C59 N55 Zn53 137.96(14) . . ? N56 N55 Zn53 114.90(11) . . ? C57 N56 N55 112.56(15) . . ? N56 C57 C58 105.66(16) . . ? N56 C57 C60 121.08(17) . . ? C58 C57 C60 133.25(17) . . ? C57 C58 C59 106.17(17) . . ? N55 C59 C58 110.81(17) . . ? C57 C60 C63 109.91(17) . . ? C57 C60 C61 110.48(18) . . ? C63 C60 C61 110.2(2) . . ? C57 C60 C62 108.42(18) . . ? C63 C60 C62 108.3(2) . . ? C61 C60 C62 109.5(2) . . ? C68 N64 N65 105.05(16) . . ? C68 N64 Zn53 127.23(14) . . ? N65 N64 Zn53 127.71(12) . . ? C66 N65 N64 112.27(15) . . ? N65 C66 C67 106.04(17) . . ? N65 C66 C69 122.52(17) . . ? C67 C66 C69 131.44(18) . . ? C66 C67 C68 105.92(17) . . ? N64 C68 C67 110.71(18) . . ? C66 C69 C72 109.18(18) . . ? C66 C69 C70 110.92(17) . . ? C72 C69 C70 110.1(2) . . ? C66 C69 C71 108.55(18) . . ? C72 C69 C71 109.9(2) . . ? C70 C69 C71 108.1(2) . . ? C77 N73 N74 104.94(15) . . ? C77 N73 Zn53 128.74(13) . . ? N74 N73 Zn53 126.06(12) . . ? C75 N74 N73 112.32(15) . . ? N74 C75 C76 105.92(16) . . ? N74 C75 C78 121.67(17) . . ? C76 C75 C78 132.40(18) . . ? C77 C76 C75 105.98(17) . . ? N73 C77 C76 110.83(17) . . ? C75 C78 C79 110.96(16) . . ? C75 C78 C80 108.27(17) . . ? C79 C78 C80 110.4(2) . . ? C75 C78 C81 109.04(17) . . ? C79 C78 C81 108.58(18) . . ? C80 C78 C81 109.6(2) . . ? C95 Co82 C83 178.75(9) . . ? C95 Co82 C94 47.49(8) . . ? C83 Co82 C94 131.45(9) . . ? C95 Co82 C84 131.22(9) . . ? C83 Co82 C84 47.64(9) . . ? C94 Co82 C84 97.54(9) . . ? C95 Co82 B87 132.52(9) . . ? C83 Co82 B87 48.57(9) . . ? C94 Co82 B87 177.94(9) . . ? C84 Co82 B87 83.71(9) . . ? C95 Co82 B96 49.26(9) . . ? C83 Co82 B96 131.91(9) . . ? C94 Co82 B96 84.21(9) . . ? C84 Co82 B96 177.67(9) . . ? B87 Co82 B96 94.59(10) . . ? C95 Co82 B98 83.62(9) . . ? C83 Co82 B98 95.94(9) . . ? C94 Co82 B98 48.58(8) . . ? C84 Co82 B98 95.95(9) . . ? B87 Co82 B98 129.75(9) . . ? B96 Co82 B98 86.36(9) . . ? C95 Co82 B85 95.76(9) . . ? C83 Co82 B85 83.64(9) . . ? C94 Co82 B85 96.42(9) . . ? C84 Co82 B85 48.97(9) . . ? B87 Co82 B85 85.63(9) . . ? B96 Co82 B85 129.41(9) . . ? B98 Co82 B85 130.55(9) . . ? C95 Co82 B86 96.83(9) . . ? C83 Co82 B86 83.62(9) . . ? C94 Co82 B86 131.98(9) . . ? C84 Co82 B86 84.01(9) . . ? B87 Co82 B86 49.69(9) . . ? B96 Co82 B86 93.68(9) . . ? B98 Co82 B86 179.44(10) . . ? B85 Co82 B86 49.76(9) . . ? C95 Co82 B97 83.87(9) . . ? C83 Co82 B97 96.74(9) . . ? C94 Co82 B97 83.58(9) . . ? C84 Co82 B97 131.53(9) . . ? B87 Co82 B97 94.37(9) . . ? B96 Co82 B97 50.08(9) . . ? B98 Co82 B97 49.77(9) . . ? B85 Co82 B97 179.50(9) . . ? B86 Co82 B97 129.92(9) . . ? C84 C83 B87 111.32(16) . . ? C84 C83 B92 111.61(18) . . ? B87 C83 B92 63.20(15) . . ? C84 C83 B88 61.78(14) . . ? B87 C83 B88 113.99(18) . . ? B92 C83 B88 61.92(16) . . ? C84 C83 Co82 67.07(10) . . ? B87 C83 Co82 67.12(11) . . ? B92 C83 Co82 125.17(16) . . ? B88 C83 Co82 124.78(16) . . ? C83 C84 B89 109.81(17) . . ? C83 C84 B85 109.89(16) . . ? B89 C84 B85 62.55(14) . . ? C83 C84 B88 61.35(15) . . ? B89 C84 B88 61.49(15) . . ? B85 C84 B88 113.16(17) . . ? C83 C84 Co82 65.30(10) . . ? B89 C84 Co82 123.98(15) . . ? B85 C84 Co82 67.59(10) . . ? B88 C84 Co82 122.75(16) . . ? C84 B85 B90 104.42(17) . . ? C84 B85 B86 105.37(16) . . ? B90 B85 B86 60.34(13) . . ? C84 B85 B89 58.59(13) . . ? B90 B85 B89 59.31(14) . . ? B86 B85 B89 107.93(16) . . ? C84 B85 Co82 63.44(10) . . ? B90 B85 Co82 117.91(14) . . ? B86 B85 Co82 65.38(10) . . ? B89 B85 Co82 116.77(15) . . ? B87 B86 B91 59.75(14) . . ? B87 B86 B85 106.53(17) . . ? B91 B86 B85 107.10(17) . . ? B87 B86 B90 106.32(17) . . ? B91 B86 B90 59.15(14) . . ? B85 B86 B90 59.78(13) . . ? B87 B86 Co82 63.37(11) . . ? B91 B86 Co82 116.45(15) . . ? B85 B86 Co82 64.86(10) . . ? B90 B86 Co82 116.98(14) . . ? C83 B87 B86 106.85(16) . . ? C83 B87 B91 105.59(17) . . ? B86 B87 B91 60.72(14) . . ? C83 B87 B92 59.06(15) . . ? B86 B87 B92 109.38(17) . . ? B91 B87 B92 59.95(15) . . ? C83 B87 Co82 64.31(11) . . ? B86 B87 Co82 66.93(11) . . ? B91 B87 Co82 120.39(15) . . ? B92 B87 Co82 118.90(16) . . ? C83 B88 C84 56.87(13) . . ? C83 B88 B92 58.57(15) . . ? C84 B88 B92 104.95(17) . . ? C83 B88 B93 104.96(19) . . ? C84 B88 B93 105.84(19) . . ? B92 B88 B93 60.26(16) . . ? C83 B88 B89 104.36(17) . . ? C84 B88 B89 59.07(14) . . ? B92 B88 B89 108.1(2) . . ? B93 B88 B89 60.31(16) . . ? C84 B89 B88 59.44(14) . . ? C84 B89 B90 105.25(16) . . ? B88 B89 B90 107.90(19) . . ? C84 B89 B93 105.75(18) . . ? B88 B89 B93 59.84(16) . . ? B90 B89 B93 60.14(15) . . ? C84 B89 B85 58.86(13) . . ? B88 B89 B85 108.47(17) . . ? B90 B89 B85 60.12(14) . . ? B93 B89 B85 108.56(17) . . ? B91 B90 B89 108.11(19) . . ? B91 B90 B93 60.42(15) . . ? B89 B90 B93 60.04(15) . . ? B91 B90 B85 107.98(17) . . ? B89 B90 B85 60.57(14) . . ? B93 B90 B85 108.84(18) . . ? B91 B90 B86 60.15(14) . . ? B89 B90 B86 108.57(17) . . ? B93 B90 B86 109.03(18) . . ? B85 B90 B86 59.88(13) . . ? B90 B91 B87 107.36(17) . . ? B90 B91 B92 107.78(19) . . ? B87 B91 B92 60.25(15) . . ? B90 B91 B93 60.05(15) . . ? B87 B91 B93 107.85(19) . . ? B92 B91 B93 59.84(16) . . ? B90 B91 B86 60.71(14) . . ? B87 B91 B86 59.52(13) . . ? B92 B91 B86 108.65(18) . . ? B93 B91 B86 109.18(18) . . ? C83 B92 B88 59.52(15) . . ? C83 B92 B91 104.44(18) . . ? B88 B92 B91 108.1(2) . . ? C83 B92 B93 105.41(19) . . ? B88 B92 B93 59.91(16) . . ? B91 B92 B93 60.43(16) . . ? C83 B92 B87 57.74(13) . . ? B88 B92 B87 107.57(18) . . ? B91 B92 B87 59.79(15) . . ? B93 B92 B87 107.96(19) . . ? B88 B93 B92 59.83(17) . . ? B88 B93 B89 59.85(16) . . ? B92 B93 B89 107.38(19) . . ? B88 B93 B90 107.65(18) . . ? B92 B93 B90 107.30(18) . . ? B89 B93 B90 59.82(15) . . ? B88 B93 B91 107.52(19) . . ? B92 B93 B91 59.74(16) . . ? B89 B93 B91 107.23(18) . . ? B90 B93 B91 59.53(15) . . ? C95 C94 B98 111.27(16) . . ? C95 C94 B103 111.33(16) . . ? B98 C94 B103 63.09(14) . . ? C95 C94 B99 61.99(13) . . ? B98 C94 B99 114.42(16) . . ? B103 C94 B99 61.99(14) . . ? C95 C94 Co82 65.92(10) . . ? B98 C94 Co82 68.12(10) . . ? B103 C94 Co82 125.53(14) . . ? B99 C94 Co82 124.27(15) . . ? C94 C95 B100 111.35(15) . . ? C94 C95 B96 111.28(15) . . ? B100 C95 B96 63.44(14) . . ? C94 C95 B99 61.56(13) . . ? B100 C95 B99 62.37(14) . . ? B96 C95 B99 114.90(16) . . ? C94 C95 Co82 66.59(10) . . ? B100 C95 Co82 125.36(14) . . ? B96 C95 Co82 67.38(10) . . ? B99 C95 Co82 124.50(14) . . ? C95 B96 B101 103.78(16) . . ? C95 B96 B97 105.17(15) . . ? B101 B96 B97 60.22(13) . . ? C95 B96 B100 57.95(13) . . ? B101 B96 B100 59.53(14) . . ? B97 B96 B100 108.06(16) . . ? C95 B96 Co82 63.36(10) . . ? B101 B96 Co82 118.91(14) . . ? B97 B96 Co82 66.55(10) . . ? B100 B96 Co82 116.79(15) . . ? B98 B97 B96 106.69(16) . . ? B98 B97 B101 106.78(17) . . ? B96 B97 B101 59.66(13) . . ? B98 B97 B102 59.38(13) . . ? B96 B97 B102 106.95(17) . . ? B101 B97 B102 59.60(13) . . ? B98 B97 Co82 64.19(10) . . ? B96 B97 Co82 63.37(10) . . ? B101 B97 Co82 115.69(14) . . ? B102 B97 Co82 116.02(14) . . ? C94 B98 B102 104.22(16) . . ? C94 B98 B103 58.58(13) . . ? B102 B98 B103 59.52(13) . . ? C94 B98 B97 105.53(15) . . ? B102 B98 B97 60.51(13) . . ? B103 B98 B97 108.65(16) . . ? C94 B98 Co82 63.31(10) . . ? B102 B98 Co82 118.58(13) . . ? B103 B98 Co82 117.18(14) . . ? B97 B98 Co82 66.04(10) . . ? C94 B99 C95 56.45(12) . . ? C94 B99 B104 105.16(17) . . ? C95 B99 B104 104.74(18) . . ? C94 B99 B103 58.67(13) . . ? C95 B99 B103 104.25(17) . . ? B104 B99 B103 60.72(14) . . ? C94 B99 B100 103.79(17) . . ? C95 B99 B100 58.05(13) . . ? B104 B99 B100 60.43(14) . . ? B103 B99 B100 108.36(18) . . ? C95 B100 B101 104.58(16) . . ? C95 B100 B99 59.59(13) . . ? B101 B100 B99 107.90(17) . . ? C95 B100 B104 105.22(16) . . ? B101 B100 B104 60.42(14) . . ? B99 B100 B104 59.51(14) . . ? C95 B100 B96 58.61(12) . . ? B101 B100 B96 59.89(14) . . ? B99 B100 B96 108.68(16) . . ? B104 B100 B96 108.59(17) . . ? B100 B101 B96 60.58(13) . . ? B100 B101 B102 107.52(17) . . ? B96 B101 B102 107.86(16) . . ? B100 B101 B104 59.97(14) . . ? B96 B101 B104 108.79(17) . . ? B102 B101 B104 59.90(14) . . ? B100 B101 B97 108.81(16) . . ? B96 B101 B97 60.11(12) . . ? B102 B101 B97 60.31(13) . . ? B104 B101 B97 109.07(16) . . ? B103 B102 B98 60.53(13) . . ? B103 B102 B101 108.27(17) . . ? B98 B102 B101 107.75(15) . . ? B103 B102 B104 60.35(14) . . ? B98 B102 B104 108.78(16) . . ? B101 B102 B104 60.24(14) . . ? B103 B102 B97 109.13(16) . . ? B98 B102 B97 60.11(12) . . ? B101 B102 B97 60.09(13) . . ? B104 B102 B97 109.17(16) . . ? C94 B103 B99 59.34(13) . . ? C94 B103 B102 104.35(16) . . ? B99 B103 B102 107.94(17) . . ? C94 B103 B104 104.83(16) . . ? B99 B103 B104 59.61(14) . . ? B102 B103 B104 60.27(14) . . ? C94 B103 B98 58.33(12) . . ? B99 B103 B98 108.32(16) . . ? B102 B103 B98 59.95(13) . . ? B104 B103 B98 108.27(17) . . ? B99 B104 B100 60.06(14) . . ? B99 B104 B102 107.26(17) . . ? B100 B104 B102 107.20(17) . . ? B99 B104 B103 59.67(14) . . ? B100 B104 B103 107.24(16) . . ? B102 B104 B103 59.38(14) . . ? B99 B104 B101 107.69(17) . . ? B100 B104 B101 59.61(14) . . ? B102 B104 B101 59.86(14) . . ? B103 B104 B101 107.21(17) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N13 H13 Cl2 0.88 2.39 3.2143(16) 156.1 2_655 N22 H22 Cl2 0.88 2.33 3.1730(16) 160.3 2_655 N56 H56 Cl54 0.88 2.62 3.1934(16) 124.1 . N65 H65 Cl54 0.88 2.37 3.2100(16) 160.6 2_666 N74 H74 Cl54 0.88 2.36 3.1926(16) 158.1 2_666 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.557 _refine_diff_density_min -0.829 _refine_diff_density_rms 0.140 #=END data_sr53a _database_code_CSD 192038 _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Chloro-tris(5-tertbutylpyrazole)zinc(II)][1-phenyl-nonahydro-closo-1- carbanonaborate] pentane solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H36 Cl N6 Zn, C7 H14 B9, 0.2[C5 H12]' _chemical_formula_sum 'C29 H52.40 B9 Cl N6 Zn' _chemical_formula_weight 683.28 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' 'Zn' 'Zn' 0.2839 1.4301 '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' 'B' 'B' 0.0013 0.0007 '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 10.8007(1) _cell_length_b 15.4087(1) _cell_length_c 24.7967(3) _cell_angle_alpha 100.3662(4) _cell_angle_beta 97.0776(4) _cell_angle_gamma 100.9195(6) _cell_volume 3932.70(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 81059 _cell_measurement_theta_min 1.95 _cell_measurement_theta_max 27.49 _exptl_crystal_description Needle _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.154 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1442 _exptl_absorpt_coefficient_mu 0.720 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8238 _exptl_absorpt_correction_T_max 0.9787 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _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 'Nonius KappaCCD diffractometer' _diffrn_measurement_method 'Area detector scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 81059 _diffrn_reflns_av_R_equivalents 0.0737 _diffrn_reflns_av_sigmaI/netI 0.0480 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 27.49 _reflns_number_total 18005 _reflns_number_gt 14167 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The asymmetric unit contains two complex cations and two anions lying on general positions, and a disordered region of solvent lying across a crystallographic inversion centre. The solvent was modelled using two partial pentane environments C91A-C95A and C91B-C95B, each of occupancy 0.2. The following disorder is also present in the structure. One tertbutylpyrazole ligand is disordered over three sites: N48A-C56A (occupancy 0.45), N48B-C56B (occupancy 0.35) and N48C-C56C (occupancy 0.20). The following tertbutyl groups are also disordered over the orientations listed: C26A-C29A (occupancy 0.45), C26B-C29B (occupancy 0.35) and C26C-C29C (occupancy 0.20). C62A-C65A (occupancy 0.50) and C62B-C65B (occupancy 0.50). C71A-C74A (occupancy 0.50) and C71B-C74B (occupancy 0.50). The following restraints were applied to model this disorder: pyrazole N-N = 1.36(1)\%A pyrazole N-C = 1.35(1)\%A pyrazole N=C = 1.32(1)\%A pyrazole C-C = 1.39(1)\%A pyrazole C=C = 1.36(1)\%A tert-butyl C-C = 1.52(2)\%A tert-butyl 1,3-C...C = 2.48(2)\%A pentane C-C = 1.52(1)\%A pentane 1,3-C...C = 2.48(1)\%A. All crystallographically ordered non-H atoms were refined anisotropically. All H atoms were placed in calculated positions and refined using a riding model. ; _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^)+(0.0650P)^2^+1.7155P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18005 _refine_ls_number_parameters 883 _refine_ls_number_restraints 129 _refine_ls_R_factor_all 0.0643 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.1279 _refine_ls_wR_factor_gt 0.1165 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.038 _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 Zn1 Zn -0.03383(2) -0.034087(16) 0.078742(9) 0.02997(7) Uani 1 1 d . . . Cl2 Cl -0.17440(5) 0.03881(3) 0.04058(2) 0.03345(12) Uani 1 1 d . . . N3 N -0.10122(16) -0.05685(12) 0.14826(7) 0.0316(4) Uani 1 1 d . . . N4 N -0.04749(16) -0.10152(12) 0.18403(7) 0.0324(4) Uani 1 1 d . . . H4 H 0.0263 -0.1172 0.1822 0.039 Uiso 1 1 calc R . . C5 C -0.12048(19) -0.11899(13) 0.22275(8) 0.0287(4) Uani 1 1 d . . . C6 C -0.2266(2) -0.08438(16) 0.21125(9) 0.0369(5) Uani 1 1 d . . . H6 H -0.2967 -0.0858 0.2310 0.044 Uiso 1 1 calc R . . C7 C -0.2108(2) -0.04690(15) 0.16493(9) 0.0353(5) Uani 1 1 d . . . H7 H -0.2703 -0.0181 0.1476 0.042 Uiso 1 1 calc R . . C8 C -0.0815(2) -0.16962(14) 0.26628(8) 0.0325(4) Uani 1 1 d . . . C9 C 0.0553(2) -0.12694(17) 0.29542(10) 0.0447(6) Uani 1 1 d . . . H9A H 0.1131 -0.1275 0.2679 0.067 Uiso 1 1 calc R . . H9B H 0.0805 -0.1615 0.3229 0.067 Uiso 1 1 calc R . . H9C H 0.0600 -0.0644 0.3141 0.067 Uiso 1 1 calc R . . C10 C -0.1728(3) -0.16562(19) 0.30891(10) 0.0496(6) Uani 1 1 d . . . H10A H -0.1680 -0.1024 0.3263 0.074 Uiso 1 1 calc R . . H10B H -0.1485 -0.1984 0.3375 0.074 Uiso 1 1 calc R . . H10C H -0.2604 -0.1934 0.2902 0.074 Uiso 1 1 calc R . . C11 C -0.0899(3) -0.26802(16) 0.23827(10) 0.0479(6) Uani 1 1 d . . . H11A H -0.1782 -0.2957 0.2204 0.072 Uiso 1 1 calc R . . H11B H -0.0635 -0.3013 0.2663 0.072 Uiso 1 1 calc R . . H11C H -0.0335 -0.2700 0.2102 0.072 Uiso 1 1 calc R . . N12 N -0.06531(17) -0.16090(12) 0.03595(7) 0.0325(4) Uani 1 1 d . . . N13 N -0.00978(17) -0.19812(12) -0.00581(7) 0.0322(4) Uani 1 1 d . . . H13 H 0.0540 -0.1682 -0.0186 0.039 Uiso 1 1 calc R . . C14 C -0.0632(2) -0.28601(14) -0.02548(9) 0.0352(5) Uani 1 1 d . . . C15 C -0.1583(2) -0.30674(17) 0.00538(10) 0.0470(6) Uani 1 1 d . . . H15 H -0.2139 -0.3639 0.0018 0.056 Uiso 1 1 calc R . . C16 C -0.1567(2) -0.22820(16) 0.04246(10) 0.0435(5) Uani 1 1 d . . . H16 H -0.2127 -0.2226 0.0689 0.052 Uiso 1 1 calc R . . C17 C -0.0213(2) -0.34242(15) -0.07332(9) 0.0406(5) Uani 1 1 d . . . C18 C -0.0086(3) -0.43328(17) -0.05896(12) 0.0512(6) Uani 1 1 d . . . H18A H 0.0545 -0.4229 -0.0252 0.077 Uiso 1 1 calc R . . H18B H 0.0193 -0.4700 -0.0897 0.077 Uiso 1 1 calc R . . H18C H -0.0915 -0.4651 -0.0527 0.077 Uiso 1 1 calc R . . C19 C -0.1250(3) -0.3585(2) -0.12460(11) 0.0629(8) Uani 1 1 d . . . H19A H -0.2053 -0.3930 -0.1176 0.094 Uiso 1 1 calc R . . H19B H -0.0982 -0.3926 -0.1568 0.094 Uiso 1 1 calc R . . H19C H -0.1377 -0.3003 -0.1322 0.094 Uiso 1 1 calc R . . C20 C 0.1082(3) -0.29463(18) -0.08450(12) 0.0579(7) Uani 1 1 d . . . H20A H 0.0985 -0.2401 -0.0982 0.087 Uiso 1 1 calc R . . H20B H 0.1386 -0.3354 -0.1124 0.087 Uiso 1 1 calc R . . H20C H 0.1701 -0.2779 -0.0500 0.087 Uiso 1 1 calc R . . N21 N 0.13195(16) 0.05283(12) 0.10679(7) 0.0322(4) Uani 1 1 d . A . N22 N 0.24139(16) 0.06337(12) 0.08523(8) 0.0354(4) Uani 1 1 d . A . H22 H 0.2496 0.0326 0.0528 0.042 Uiso 1 1 calc R . . C23 C 0.3361(2) 0.12591(16) 0.11877(10) 0.0398(5) Uani 1 1 d D . . C24 C 0.2855(2) 0.15796(18) 0.16495(10) 0.0464(6) Uani 1 1 d . A . H24 H 0.3280 0.2032 0.1965 0.056 Uiso 1 1 calc R . . C25 C 0.1595(2) 0.11035(16) 0.15565(9) 0.0402(5) Uani 1 1 d . . . H25 H 0.1009 0.1178 0.1808 0.048 Uiso 1 1 calc R A . C26A C 0.4630(6) 0.1569(5) 0.0991(3) 0.036(2) Uiso 0.45 1 d PD A 1 C27A C 0.5391(7) 0.2412(5) 0.1392(3) 0.0687(18) Uiso 0.45 1 d PD A 1 H27A H 0.6237 0.2580 0.1289 0.103 Uiso 0.45 1 calc PR A 1 H27B H 0.5486 0.2298 0.1770 0.103 Uiso 0.45 1 calc PR A 1 H27C H 0.4943 0.2907 0.1379 0.103 Uiso 0.45 1 calc PR A 1 C28A C 0.4489(6) 0.1740(5) 0.0418(2) 0.0561(15) Uiso 0.45 1 d PD A 1 H28A H 0.4012 0.1188 0.0157 0.084 Uiso 0.45 1 calc PR A 1 H28B H 0.5337 0.1918 0.0318 0.084 Uiso 0.45 1 calc PR A 1 H28C H 0.4027 0.2226 0.0400 0.084 Uiso 0.45 1 calc PR A 1 C29A C 0.5303(7) 0.0774(5) 0.1019(4) 0.0713(19) Uiso 0.45 1 d PD A 1 H29A H 0.4723 0.0207 0.0819 0.107 Uiso 0.45 1 calc PR A 1 H29B H 0.5538 0.0740 0.1408 0.107 Uiso 0.45 1 calc PR A 1 H29C H 0.6075 0.0869 0.0848 0.107 Uiso 0.45 1 calc PR A 1 C26B C 0.4695(12) 0.1414(9) 0.1035(6) 0.044(5) Uiso 0.30 1 d PD A 2 C27B C 0.5693(12) 0.1679(10) 0.1566(5) 0.082(5) Uiso 0.30 1 d PD A 2 H27D H 0.5492 0.2176 0.1823 0.123 Uiso 0.30 1 calc PR A 2 H27E H 0.6544 0.1873 0.1473 0.123 Uiso 0.30 1 calc PR A 2 H27F H 0.5681 0.1158 0.1743 0.123 Uiso 0.30 1 calc PR A 2 C28B C 0.4805(12) 0.2268(8) 0.0781(6) 0.076(3) Uiso 0.30 1 d PD A 2 H28D H 0.4216 0.2130 0.0428 0.114 Uiso 0.30 1 calc PR A 2 H28E H 0.5683 0.2458 0.0716 0.114 Uiso 0.30 1 calc PR A 2 H28F H 0.4587 0.2755 0.1039 0.114 Uiso 0.30 1 calc PR A 2 C29B C 0.4990(8) 0.0605(5) 0.0690(4) 0.0393(17) Uiso 0.30 1 d PD A 2 H29D H 0.4698 0.0071 0.0842 0.059 Uiso 0.30 1 calc PR A 2 H29E H 0.5914 0.0698 0.0693 0.059 Uiso 0.30 1 calc PR A 2 H29F H 0.4551 0.0513 0.0307 0.059 Uiso 0.30 1 calc PR A 2 C26C C 0.4723(13) 0.1500(11) 0.1107(6) 0.046(6) Uiso 0.25 1 d PD A 3 C27C C 0.5679(11) 0.1408(10) 0.1570(5) 0.054(3) Uiso 0.25 1 d PD A 3 H27G H 0.5572 0.1781 0.1918 0.081 Uiso 0.25 1 calc PR A 3 H27H H 0.6543 0.1610 0.1493 0.081 Uiso 0.25 1 calc PR A 3 H27I H 0.5549 0.0774 0.1603 0.081 Uiso 0.25 1 calc PR A 3 C28C C 0.4957(11) 0.2492(7) 0.1030(6) 0.057(3) Uiso 0.25 1 d PD A 3 H28G H 0.4279 0.2556 0.0748 0.086 Uiso 0.25 1 calc PR A 3 H28H H 0.5786 0.2651 0.0909 0.086 Uiso 0.25 1 calc PR A 3 H28I H 0.4954 0.2896 0.1383 0.086 Uiso 0.25 1 calc PR A 3 C29C C 0.4876(10) 0.0912(8) 0.0537(4) 0.051(3) Uiso 0.25 1 d PD A 3 H29G H 0.4636 0.0270 0.0546 0.077 Uiso 0.25 1 calc PR A 3 H29H H 0.5767 0.1060 0.0480 0.077 Uiso 0.25 1 calc PR A 3 H29I H 0.4320 0.1043 0.0232 0.077 Uiso 0.25 1 calc PR A 3 B30 B 0.2457(3) -0.1449(2) 0.14765(13) 0.0474(7) Uani 1 1 d . . . H30 H 0.1917 -0.0904 0.1580 0.057 Uiso 1 1 calc R . . B31 B 0.3051(3) -0.17774(19) 0.08924(12) 0.0425(6) Uani 1 1 d . . . H31 H 0.2909 -0.1421 0.0541 0.051 Uiso 1 1 calc R . . B32 B 0.1903(3) -0.2554(2) 0.11695(14) 0.0477(7) Uani 1 1 d . . . H32 H 0.0847 -0.2817 0.1042 0.057 Uiso 1 1 calc R . . B33 B 0.4047(3) -0.13966(18) 0.15835(12) 0.0398(6) Uani 1 1 d . . . H33 H 0.4705 -0.0733 0.1786 0.048 Uiso 1 1 calc R . . B34 B 0.2906(3) -0.2175(2) 0.18649(13) 0.0449(6) Uani 1 1 d . . . H34 H 0.2652 -0.2135 0.2292 0.054 Uiso 1 1 calc R . . B35 B 0.3009(3) -0.29713(19) 0.07505(12) 0.0413(6) Uani 1 1 d . . . H35 H 0.2658 -0.3390 0.0321 0.050 Uiso 1 1 calc R . . B36 B 0.4516(2) -0.21542(17) 0.10451(11) 0.0359(5) Uani 1 1 d . . . H36 H 0.5366 -0.1920 0.0850 0.043 Uiso 1 1 calc R . . B37 B 0.4408(2) -0.24380(17) 0.17280(10) 0.0349(5) Uani 1 1 d . . . H37 H 0.5171 -0.2430 0.2079 0.042 Uiso 1 1 calc R . . B38 B 0.2895(2) -0.32566(19) 0.14322(12) 0.0402(6) Uani 1 1 d . . . H38 H 0.2449 -0.3902 0.1546 0.048 Uiso 1 1 calc R . . C39 C 0.4174(2) -0.31632(14) 0.11553(9) 0.0334(4) Uani 1 1 d . . . C40 C 0.4915(2) -0.38717(15) 0.10193(9) 0.0364(5) Uani 1 1 d . . . C41 C 0.4314(3) -0.47504(18) 0.07639(12) 0.0536(7) Uani 1 1 d . . . H41 H 0.3408 -0.4911 0.0678 0.064 Uiso 1 1 calc R . . C42 C 0.5023(3) -0.5401(2) 0.06310(14) 0.0679(9) Uani 1 1 d . . . H42 H 0.4599 -0.6000 0.0450 0.081 Uiso 1 1 calc R . . C43 C 0.6340(3) -0.5182(2) 0.07607(12) 0.0620(8) Uani 1 1 d . . . H43 H 0.6822 -0.5630 0.0675 0.074 Uiso 1 1 calc R . . C44 C 0.6947(3) -0.4313(2) 0.10140(11) 0.0514(6) Uani 1 1 d . . . H44 H 0.7853 -0.4157 0.1100 0.062 Uiso 1 1 calc R . . C45 C 0.6243(2) -0.36584(17) 0.11457(10) 0.0414(5) Uani 1 1 d . . . H45 H 0.6673 -0.3060 0.1324 0.050 Uiso 1 1 calc R . . Zn46 Zn 0.48457(2) 0.352192(16) 0.462003(10) 0.03361(8) Uani 1 1 d . . . Cl47 Cl 0.64792(5) 0.44150(4) 0.52744(2) 0.03692(12) Uani 1 1 d . B . N48A N 0.5360(10) 0.2309(9) 0.4419(6) 0.037(6) Uiso 0.45 1 d PD B 1 N49A N 0.4671(5) 0.1681(4) 0.3972(2) 0.0320(16) Uiso 0.45 1 d PD B 1 H49A H 0.3865 0.1636 0.3835 0.038 Uiso 0.45 1 calc PR B 1 C50A C 0.5425(5) 0.1142(4) 0.3775(2) 0.0378(15) Uiso 0.45 1 d PD B 1 C51A C 0.6596(6) 0.1442(5) 0.4094(3) 0.039(2) Uiso 0.45 1 d PD B 1 H51A H 0.7322 0.1185 0.4056 0.047 Uiso 0.45 1 calc PR B 1 C52A C 0.6540(10) 0.2182(7) 0.4483(6) 0.032(3) Uiso 0.45 1 d PD B 1 H52A H 0.7233 0.2543 0.4754 0.038 Uiso 0.45 1 calc PR B 1 C53A C 0.5034(6) 0.0447(4) 0.3237(3) 0.0504(13) Uiso 0.45 1 d PD B 1 C54A C 0.5654(8) 0.0878(6) 0.2796(3) 0.086(2) Uiso 0.45 1 d PD B 1 H54A H 0.5458 0.1475 0.2806 0.129 Uiso 0.45 1 calc PR B 1 H54B H 0.5317 0.0493 0.2428 0.129 Uiso 0.45 1 calc PR B 1 H54C H 0.6582 0.0940 0.2874 0.129 Uiso 0.45 1 calc PR B 1 C55A C 0.3623(8) 0.0172(7) 0.3080(4) 0.086(3) Uiso 0.45 1 d PD B 1 H55A H 0.3254 -0.0051 0.3384 0.129 Uiso 0.45 1 calc PR B 1 H55B H 0.3402 -0.0309 0.2744 0.129 Uiso 0.45 1 calc PR B 1 H55C H 0.3282 0.0693 0.3009 0.129 Uiso 0.45 1 calc PR B 1 C56A C 0.5602(8) -0.0351(5) 0.3237(4) 0.065(2) Uiso 0.45 1 d PD B 1 H56A H 0.6527 -0.0153 0.3360 0.097 Uiso 0.45 1 calc PR B 1 H56B H 0.5432 -0.0724 0.2860 0.097 Uiso 0.45 1 calc PR B 1 H56C H 0.5224 -0.0705 0.3490 0.097 Uiso 0.45 1 calc PR B 1 N48B N 0.5269(15) 0.2309(10) 0.4421(8) 0.030(6) Uiso 0.35 1 d PD B 2 N49B N 0.4613(10) 0.1537(6) 0.4074(5) 0.030(3) Uiso 0.35 1 d PD B 2 H49B H 0.3781 0.1425 0.3967 0.036 Uiso 0.35 1 calc PR B 2 C50B C 0.5332(7) 0.0952(5) 0.3904(4) 0.037(2) Uiso 0.35 1 d PD B 2 C51B C 0.6552(8) 0.1320(7) 0.4190(5) 0.039(3) Uiso 0.35 1 d PD B 2 H51B H 0.7295 0.1077 0.4177 0.047 Uiso 0.35 1 calc PR B 2 C52B C 0.6427(18) 0.2135(13) 0.4500(11) 0.061(9) Uiso 0.35 1 d PD B 2 H52B H 0.7119 0.2538 0.4751 0.073 Uiso 0.35 1 calc PR B 2 C53B C 0.4733(7) 0.0088(5) 0.3469(4) 0.0499(18) Uiso 0.35 1 d PD B 2 C54B C 0.3719(8) -0.0500(6) 0.3715(4) 0.068(2) Uiso 0.35 1 d PD B 2 H54D H 0.3055 -0.0169 0.3803 0.102 Uiso 0.35 1 calc PR B 2 H54E H 0.4125 -0.0642 0.4054 0.102 Uiso 0.35 1 calc PR B 2 H54F H 0.3334 -0.1061 0.3444 0.102 Uiso 0.35 1 calc PR B 2 C55B C 0.4067(12) 0.0348(8) 0.2947(4) 0.088(3) Uiso 0.35 1 d PD B 2 H55D H 0.3399 0.0665 0.3050 0.132 Uiso 0.35 1 calc PR B 2 H55E H 0.3684 -0.0200 0.2664 0.132 Uiso 0.35 1 calc PR B 2 H55F H 0.4700 0.0744 0.2798 0.132 Uiso 0.35 1 calc PR B 2 C56B C 0.5747(8) -0.0453(6) 0.3397(5) 0.053(2) Uiso 0.35 1 d PD B 2 H56D H 0.5388 -0.1014 0.3121 0.080 Uiso 0.35 1 calc PR B 2 H56E H 0.6047 -0.0597 0.3753 0.080 Uiso 0.35 1 calc PR B 2 H56F H 0.6465 -0.0099 0.3269 0.080 Uiso 0.35 1 calc PR B 2 N48C N 0.5351(13) 0.2280(9) 0.4508(6) 0.027(4) Uiso 0.20 1 d PD B 3 N49C N 0.4692(13) 0.1495(8) 0.4162(6) 0.031(5) Uiso 0.20 1 d PD B 3 H49C H 0.3890 0.1417 0.4006 0.037 Uiso 0.20 1 calc PR B 3 C50C C 0.5377(9) 0.0846(6) 0.4076(5) 0.036(3) Uiso 0.20 1 d PD B 3 C51C C 0.6568(10) 0.1254(7) 0.4362(6) 0.036(3) Uiso 0.20 1 d PD B 3 H51C H 0.7306 0.1002 0.4376 0.044 Uiso 0.20 1 calc PR B 3 C52C C 0.6489(14) 0.2109(9) 0.4630(7) 0.024(3) Uiso 0.20 1 d PD B 3 H52C H 0.7181 0.2525 0.4874 0.028 Uiso 0.20 1 calc PR B 3 C53C C 0.4774(9) -0.0090(7) 0.3716(5) 0.037(2) Uiso 0.20 1 d PD B 3 C54C C 0.5796(13) -0.0640(10) 0.3672(7) 0.072(5) Uiso 0.20 1 d PD B 3 H54G H 0.6528 -0.0298 0.3546 0.109 Uiso 0.20 1 calc PR B 3 H54H H 0.5449 -0.1211 0.3404 0.109 Uiso 0.20 1 calc PR B 3 H54I H 0.6073 -0.0764 0.4036 0.109 Uiso 0.20 1 calc PR B 3 C55C C 0.4089(18) -0.0048(13) 0.3169(6) 0.087(6) Uiso 0.20 1 d PD B 3 H55G H 0.4597 0.0419 0.3017 0.130 Uiso 0.20 1 calc PR B 3 H55H H 0.3259 0.0099 0.3214 0.130 Uiso 0.20 1 calc PR B 3 H55I H 0.3958 -0.0635 0.2914 0.130 Uiso 0.20 1 calc PR B 3 C56C C 0.3738(11) -0.0573(9) 0.4004(6) 0.054(3) Uiso 0.20 1 d PD B 3 H56G H 0.3259 -0.1133 0.3752 0.080 Uiso 0.20 1 calc PR B 3 H56H H 0.3153 -0.0177 0.4100 0.080 Uiso 0.20 1 calc PR B 3 H56I H 0.4145 -0.0716 0.4343 0.080 Uiso 0.20 1 calc PR B 3 N57 N 0.50131(18) 0.39119(12) 0.39009(8) 0.0360(4) Uani 1 1 d . B . N58 N 0.47023(17) 0.46391(12) 0.37252(7) 0.0353(4) Uani 1 1 d . . . H58 H 0.4369 0.5042 0.3923 0.042 Uiso 1 1 calc R B . C59 C 0.4965(2) 0.46719(16) 0.32102(9) 0.0385(5) Uani 1 1 d D B . C60 C 0.5473(3) 0.39338(18) 0.30487(11) 0.0495(6) Uani 1 1 d . . . H60 H 0.5758 0.3763 0.2706 0.059 Uiso 1 1 calc R B . C61 C 0.5486(3) 0.34867(17) 0.34858(11) 0.0485(6) Uani 1 1 d . B . H61 H 0.5792 0.2948 0.3488 0.058 Uiso 1 1 calc R . . C62A C 0.4718(7) 0.5496(5) 0.2951(3) 0.043(2) Uiso 0.50 1 d PD B 1 C63A C 0.3967(9) 0.6064(6) 0.3268(4) 0.055(3) Uiso 0.50 1 d PD B 1 H63A H 0.4455 0.6345 0.3639 0.083 Uiso 0.50 1 calc PR B 1 H63B H 0.3156 0.5684 0.3304 0.083 Uiso 0.50 1 calc PR B 1 H63C H 0.3795 0.6535 0.3070 0.083 Uiso 0.50 1 calc PR B 1 C64A C 0.6052(5) 0.6050(4) 0.2937(3) 0.0526(17) Uiso 0.50 1 d PD B 1 H64A H 0.5968 0.6520 0.2724 0.079 Uiso 0.50 1 calc PR B 1 H64B H 0.6559 0.5651 0.2760 0.079 Uiso 0.50 1 calc PR B 1 H64C H 0.6480 0.6333 0.3317 0.079 Uiso 0.50 1 calc PR B 1 C65A C 0.4038(8) 0.5099(6) 0.2355(3) 0.064(2) Uiso 0.50 1 d PD B 1 H65A H 0.3232 0.4683 0.2359 0.096 Uiso 0.50 1 calc PR B 1 H65B H 0.4585 0.4770 0.2149 0.096 Uiso 0.50 1 calc PR B 1 H65C H 0.3860 0.5588 0.2175 0.096 Uiso 0.50 1 calc PR B 1 C62B C 0.4778(6) 0.5349(5) 0.2881(3) 0.037(2) Uiso 0.50 1 d PD B 2 C63B C 0.4103(9) 0.6022(6) 0.3189(4) 0.060(3) Uiso 0.50 1 d PD B 2 H63D H 0.3272 0.5701 0.3247 0.090 Uiso 0.50 1 calc PR B 2 H63E H 0.3976 0.6474 0.2968 0.090 Uiso 0.50 1 calc PR B 2 H63F H 0.4627 0.6323 0.3549 0.090 Uiso 0.50 1 calc PR B 2 C64B C 0.6038(5) 0.5851(5) 0.2767(3) 0.0525(17) Uiso 0.50 1 d PD B 2 H64D H 0.6603 0.6138 0.3120 0.079 Uiso 0.50 1 calc PR B 2 H64E H 0.5881 0.6315 0.2560 0.079 Uiso 0.50 1 calc PR B 2 H64F H 0.6444 0.5424 0.2548 0.079 Uiso 0.50 1 calc PR B 2 C65B C 0.3923(8) 0.4857(6) 0.2322(3) 0.061(2) Uiso 0.50 1 d PD B 2 H65D H 0.4385 0.4468 0.2106 0.091 Uiso 0.50 1 calc PR B 2 H65E H 0.3702 0.5304 0.2113 0.091 Uiso 0.50 1 calc PR B 2 H65F H 0.3140 0.4487 0.2393 0.091 Uiso 0.50 1 calc PR B 2 N66 N 0.33841(17) 0.32717(12) 0.50222(7) 0.0328(4) Uani 1 1 d . B . N67 N 0.26078(16) 0.38254(12) 0.51935(7) 0.0319(4) Uani 1 1 d . . . H67 H 0.2628 0.4358 0.5109 0.038 Uiso 1 1 calc R B . C68 C 0.18014(19) 0.34662(14) 0.55084(8) 0.0323(4) Uani 1 1 d D B . C69 C 0.2072(2) 0.26408(16) 0.55429(10) 0.0423(5) Uani 1 1 d . . . H69 H 0.1668 0.2218 0.5736 0.051 Uiso 1 1 calc R B . C70 C 0.3053(2) 0.25468(16) 0.52389(10) 0.0410(5) Uani 1 1 d . B . H70 H 0.3436 0.2037 0.5192 0.049 Uiso 1 1 calc R . . C71A C 0.0746(9) 0.3908(6) 0.5696(4) 0.039(4) Uiso 0.50 1 d PD B 1 C72A C 0.1397(8) 0.4875(5) 0.6042(3) 0.063(3) Uiso 0.50 1 d PD B 1 H72A H 0.0747 0.5171 0.6190 0.095 Uiso 0.50 1 calc PR B 1 H72B H 0.1829 0.5232 0.5803 0.095 Uiso 0.50 1 calc PR B 1 H72C H 0.2025 0.4827 0.6350 0.095 Uiso 0.50 1 calc PR B 1 C73A C 0.0013(7) 0.3387(5) 0.6050(3) 0.0633(18) Uiso 0.50 1 d PD B 1 H73A H -0.0540 0.2835 0.5816 0.095 Uiso 0.50 1 calc PR B 1 H73B H -0.0511 0.3757 0.6240 0.095 Uiso 0.50 1 calc PR B 1 H73C H 0.0610 0.3225 0.6326 0.095 Uiso 0.50 1 calc PR B 1 C74A C -0.0128(6) 0.4032(4) 0.5193(2) 0.0501(15) Uiso 0.50 1 d PD B 1 H74A H -0.0466 0.3446 0.4939 0.075 Uiso 0.50 1 calc PR B 1 H74B H 0.0360 0.4448 0.5001 0.075 Uiso 0.50 1 calc PR B 1 H74C H -0.0839 0.4282 0.5319 0.075 Uiso 0.50 1 calc PR B 1 C71B C 0.0856(8) 0.3977(6) 0.5746(4) 0.035(3) Uiso 0.50 1 d PD B 2 C72B C 0.1387(6) 0.4982(4) 0.5939(3) 0.0369(16) Uiso 0.50 1 d PD B 2 H72D H 0.2104 0.5090 0.6245 0.055 Uiso 0.50 1 calc PR B 2 H72E H 0.0717 0.5276 0.6069 0.055 Uiso 0.50 1 calc PR B 2 H72F H 0.1685 0.5233 0.5630 0.055 Uiso 0.50 1 calc PR B 2 C73B C 0.0405(5) 0.3564(4) 0.6229(2) 0.0417(12) Uiso 0.50 1 d PD B 2 H73D H 0.0078 0.2911 0.6100 0.063 Uiso 0.50 1 calc PR B 2 H73E H -0.0275 0.3843 0.6362 0.063 Uiso 0.50 1 calc PR B 2 H73F H 0.1125 0.3676 0.6533 0.063 Uiso 0.50 1 calc PR B 2 C74B C -0.0309(5) 0.3761(4) 0.5270(2) 0.0447(13) Uiso 0.50 1 d PD B 2 H74D H -0.0011 0.3856 0.4923 0.067 Uiso 0.50 1 calc PR B 2 H74E H -0.0891 0.4161 0.5364 0.067 Uiso 0.50 1 calc PR B 2 H74F H -0.0759 0.3130 0.5223 0.067 Uiso 0.50 1 calc PR B 2 B75 B 0.1005(4) 0.1290(2) 0.37028(13) 0.0560(8) Uani 1 1 d . . . H75 H 0.1328 0.0771 0.3917 0.067 Uiso 1 1 calc R . . B76 B 0.0953(3) 0.1389(2) 0.30305(12) 0.0500(7) Uani 1 1 d . . . H76 H 0.1278 0.0871 0.2736 0.060 Uiso 1 1 calc R . . B77 B -0.0452(3) 0.1309(2) 0.33711(13) 0.0521(7) Uani 1 1 d . . . H77 H -0.1259 0.0722 0.3352 0.062 Uiso 1 1 calc R . . B78 B 0.0417(3) 0.2202(2) 0.39547(12) 0.0524(7) Uani 1 1 d . . . H78 H 0.0310 0.2334 0.4404 0.063 Uiso 1 1 calc R . . B79 B 0.1831(3) 0.2285(2) 0.36191(13) 0.0530(7) Uani 1 1 d . . . H79 H 0.2872 0.2488 0.3799 0.064 Uiso 1 1 calc R . . B80 B -0.0360(3) 0.18672(19) 0.27906(11) 0.0450(6) Uani 1 1 d . . . H80 H -0.0982 0.1560 0.2379 0.054 Uiso 1 1 calc R . . B81 B 0.1277(3) 0.25566(19) 0.29695(12) 0.0439(6) Uani 1 1 d . . . H81 H 0.1969 0.2800 0.2700 0.053 Uiso 1 1 calc R . . B82 B 0.0888(3) 0.31304(19) 0.36243(11) 0.0432(6) Uani 1 1 d . . . H82 H 0.1267 0.3832 0.3877 0.052 Uiso 1 1 calc R . . B83 B -0.0741(3) 0.24445(19) 0.34448(12) 0.0452(6) Uani 1 1 d . . . H83 H -0.1665 0.2596 0.3553 0.054 Uiso 1 1 calc R . . C84 C 0.0007(2) 0.29450(15) 0.30246(9) 0.0370(5) Uani 1 1 d . . . C85 C -0.0374(2) 0.36394(15) 0.27378(9) 0.0385(5) Uani 1 1 d . . . C86 C 0.0501(3) 0.44347(17) 0.27535(11) 0.0488(6) Uani 1 1 d . . . H86 H 0.1338 0.4536 0.2957 0.059 Uiso 1 1 calc R . . C87 C 0.0167(3) 0.50807(19) 0.24758(13) 0.0611(8) Uani 1 1 d . . . H87 H 0.0775 0.5621 0.2489 0.073 Uiso 1 1 calc R . . C88 C -0.1047(3) 0.49420(19) 0.21800(12) 0.0600(8) Uani 1 1 d . . . H88 H -0.1275 0.5385 0.1989 0.072 Uiso 1 1 calc R . . C89 C -0.1930(3) 0.4155(2) 0.21632(11) 0.0565(7) Uani 1 1 d . . . H89 H -0.2769 0.4060 0.1963 0.068 Uiso 1 1 calc R . . C90 C -0.1596(3) 0.35098(18) 0.24369(10) 0.0486(6) Uani 1 1 d . . . H90 H -0.2206 0.2970 0.2420 0.058 Uiso 1 1 calc R . . C91A C 0.1449(17) -0.0605(14) 0.4745(10) 0.070(5) Uiso 0.20 1 d PD C 1 H91A H 0.1331 -0.1128 0.4922 0.105 Uiso 0.20 1 calc PR C 1 H91B H 0.2362 -0.0379 0.4749 0.105 Uiso 0.20 1 calc PR C 1 H91C H 0.1004 -0.0785 0.4360 0.105 Uiso 0.20 1 calc PR C 1 C92A C 0.0912(15) 0.0125(12) 0.5056(8) 0.052(4) Uiso 0.20 1 d PD C 1 H92A H 0.1244 0.0701 0.4947 0.063 Uiso 0.20 1 calc PR C 1 H92B H 0.1213 0.0201 0.5459 0.063 Uiso 0.20 1 calc PR C 1 C93A C -0.0522(14) -0.0065(13) 0.4954(7) 0.050(4) Uiso 0.20 1 d PD C 1 H93A H -0.0861 -0.0646 0.5055 0.061 Uiso 0.20 1 calc PR C 1 H93B H -0.0829 -0.0122 0.4553 0.061 Uiso 0.20 1 calc PR C 1 C94A C -0.1027(16) 0.0677(14) 0.5287(10) 0.076(6) Uiso 0.20 1 d PD C 1 H94A H -0.0843 0.1231 0.5135 0.091 Uiso 0.20 1 calc PR C 1 H94B H -0.0598 0.0818 0.5679 0.091 Uiso 0.20 1 calc PR C 1 C95A C -0.2474(18) 0.036(2) 0.5257(15) 0.142(11) Uiso 0.20 1 d PD C 1 H95A H -0.2866 0.0072 0.4874 0.213 Uiso 0.20 1 calc PR C 1 H95B H -0.2839 0.0888 0.5379 0.213 Uiso 0.20 1 calc PR C 1 H95C H -0.2640 -0.0065 0.5501 0.213 Uiso 0.20 1 calc PR C 1 C91B C 0.0731(14) -0.0432(13) 0.4845(9) 0.075(5) Uiso 0.20 1 d PD D 2 H91D H 0.0112 -0.0998 0.4677 0.112 Uiso 0.20 1 calc PR D 2 H91E H 0.1344 -0.0536 0.5139 0.112 Uiso 0.20 1 calc PR D 2 H91F H 0.1187 -0.0217 0.4560 0.112 Uiso 0.20 1 calc PR D 2 C92B C 0.0051(12) 0.0255(10) 0.5084(8) 0.066(5) Uiso 0.20 1 d PD D 2 H92C H 0.0291 0.0800 0.4928 0.079 Uiso 0.20 1 calc PR D 2 H92D H 0.0348 0.0429 0.5490 0.079 Uiso 0.20 1 calc PR D 2 C93B C -0.1383(10) -0.0040(9) 0.4980(6) 0.049(3) Uiso 0.20 1 d PD D 2 H93C H -0.1639 -0.0629 0.5086 0.059 Uiso 0.20 1 calc PR D 2 H93D H -0.1711 -0.0112 0.4580 0.059 Uiso 0.20 1 calc PR D 2 C94B C -0.1948(15) 0.0670(14) 0.5323(13) 0.108(8) Uiso 0.20 1 d PD D 2 H94C H -0.1523 0.0811 0.5715 0.130 Uiso 0.20 1 calc PR D 2 H94D H -0.1808 0.1233 0.5178 0.130 Uiso 0.20 1 calc PR D 2 C95B C -0.3369(15) 0.0302(17) 0.5286(11) 0.120(8) Uiso 0.20 1 d PD D 2 H95D H -0.3738 -0.0003 0.4902 0.180 Uiso 0.20 1 calc PR D 2 H95E H -0.3786 0.0802 0.5402 0.180 Uiso 0.20 1 calc PR D 2 H95F H -0.3501 -0.0129 0.5531 0.180 Uiso 0.20 1 calc PR D 2 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 0.03448(13) 0.03056(13) 0.02670(13) 0.00809(10) 0.00875(9) 0.00713(10) Cl2 0.0359(3) 0.0348(3) 0.0321(3) 0.0113(2) 0.0068(2) 0.0089(2) N3 0.0344(9) 0.0373(10) 0.0285(9) 0.0136(7) 0.0085(7) 0.0122(8) N4 0.0323(9) 0.0409(10) 0.0299(9) 0.0140(8) 0.0095(7) 0.0137(8) C5 0.0322(10) 0.0272(10) 0.0262(10) 0.0057(8) 0.0061(8) 0.0040(8) C6 0.0351(11) 0.0445(13) 0.0364(12) 0.0126(10) 0.0141(9) 0.0120(10) C7 0.0362(11) 0.0419(12) 0.0343(11) 0.0139(9) 0.0105(9) 0.0161(9) C8 0.0403(11) 0.0305(11) 0.0288(10) 0.0091(8) 0.0075(9) 0.0090(9) C9 0.0495(14) 0.0457(14) 0.0372(13) 0.0113(11) -0.0020(10) 0.0095(11) C10 0.0629(16) 0.0595(16) 0.0403(13) 0.0268(12) 0.0226(12) 0.0228(13) C11 0.0704(17) 0.0327(12) 0.0407(13) 0.0094(10) 0.0041(12) 0.0129(12) N12 0.0357(9) 0.0309(9) 0.0316(9) 0.0059(7) 0.0115(7) 0.0060(7) N13 0.0350(9) 0.0317(9) 0.0306(9) 0.0060(7) 0.0107(7) 0.0060(7) C14 0.0399(11) 0.0301(11) 0.0328(11) 0.0058(9) 0.0028(9) 0.0033(9) C15 0.0492(14) 0.0376(13) 0.0455(14) 0.0027(11) 0.0109(11) -0.0085(11) C16 0.0418(12) 0.0423(13) 0.0428(13) 0.0048(11) 0.0160(10) -0.0016(10) C17 0.0533(14) 0.0323(12) 0.0337(12) 0.0015(9) 0.0054(10) 0.0093(10) C18 0.0565(15) 0.0388(14) 0.0566(16) 0.0057(12) 0.0055(12) 0.0126(12) C19 0.089(2) 0.0616(18) 0.0340(14) -0.0038(12) -0.0060(13) 0.0307(16) C20 0.0769(19) 0.0432(15) 0.0541(16) -0.0009(12) 0.0329(14) 0.0099(13) N21 0.0307(9) 0.0367(10) 0.0312(9) 0.0079(8) 0.0082(7) 0.0096(7) N22 0.0328(9) 0.0389(10) 0.0335(10) 0.0030(8) 0.0111(7) 0.0060(8) C23 0.0347(11) 0.0404(13) 0.0409(13) 0.0024(10) 0.0052(9) 0.0064(10) C24 0.0441(13) 0.0491(14) 0.0375(13) -0.0056(11) 0.0016(10) 0.0067(11) C25 0.0405(12) 0.0466(14) 0.0318(11) 0.0004(10) 0.0080(9) 0.0112(10) B30 0.0422(15) 0.0451(16) 0.0631(19) 0.0168(14) 0.0162(13) 0.0195(12) B31 0.0380(13) 0.0427(15) 0.0506(16) 0.0168(13) 0.0025(11) 0.0145(11) B32 0.0330(13) 0.0475(16) 0.0660(19) 0.0191(14) 0.0065(12) 0.0110(12) B33 0.0408(14) 0.0362(14) 0.0448(15) 0.0087(11) 0.0102(11) 0.0116(11) B34 0.0459(15) 0.0461(16) 0.0494(16) 0.0142(13) 0.0177(12) 0.0162(12) B35 0.0391(14) 0.0420(15) 0.0417(14) 0.0099(12) -0.0025(11) 0.0106(11) B36 0.0357(12) 0.0367(13) 0.0383(13) 0.0115(11) 0.0070(10) 0.0115(10) B37 0.0349(12) 0.0347(13) 0.0342(13) 0.0061(10) 0.0044(10) 0.0068(10) B38 0.0342(13) 0.0381(14) 0.0491(15) 0.0133(12) 0.0048(11) 0.0068(11) C39 0.0343(11) 0.0330(11) 0.0327(11) 0.0079(9) 0.0031(8) 0.0077(9) C40 0.0412(12) 0.0378(12) 0.0327(11) 0.0105(9) 0.0044(9) 0.0131(10) C41 0.0521(15) 0.0406(14) 0.0643(17) 0.0035(12) -0.0015(13) 0.0143(12) C42 0.078(2) 0.0410(15) 0.078(2) -0.0040(14) -0.0038(17) 0.0234(15) C43 0.076(2) 0.0605(18) 0.0590(17) 0.0097(14) 0.0087(15) 0.0427(16) C44 0.0520(15) 0.0612(17) 0.0505(15) 0.0169(13) 0.0115(12) 0.0286(13) C45 0.0419(12) 0.0448(13) 0.0413(13) 0.0112(11) 0.0069(10) 0.0162(10) Zn46 0.03686(14) 0.03092(14) 0.03468(14) 0.00753(10) 0.01131(10) 0.00715(10) Cl47 0.0376(3) 0.0328(3) 0.0397(3) 0.0060(2) 0.0079(2) 0.0062(2) N57 0.0432(10) 0.0320(10) 0.0358(10) 0.0091(8) 0.0132(8) 0.0090(8) N58 0.0406(10) 0.0328(10) 0.0330(10) 0.0068(8) 0.0072(8) 0.0083(8) C59 0.0380(12) 0.0412(13) 0.0326(11) 0.0094(10) 0.0038(9) -0.0007(10) C60 0.0651(16) 0.0480(15) 0.0394(13) 0.0086(11) 0.0230(12) 0.0130(12) C61 0.0661(16) 0.0413(13) 0.0460(14) 0.0112(11) 0.0267(12) 0.0178(12) N66 0.0372(9) 0.0316(9) 0.0320(9) 0.0076(7) 0.0088(7) 0.0101(7) N67 0.0324(9) 0.0301(9) 0.0355(9) 0.0086(7) 0.0087(7) 0.0086(7) C68 0.0336(10) 0.0362(11) 0.0270(10) 0.0066(9) 0.0053(8) 0.0070(9) C69 0.0521(14) 0.0432(13) 0.0402(13) 0.0186(11) 0.0199(11) 0.0141(11) C70 0.0533(14) 0.0343(12) 0.0434(13) 0.0151(10) 0.0180(11) 0.0162(10) B75 0.086(2) 0.0483(17) 0.0365(15) 0.0065(13) 0.0134(15) 0.0210(16) B76 0.079(2) 0.0377(15) 0.0359(14) 0.0040(12) 0.0173(14) 0.0172(14) B77 0.076(2) 0.0368(15) 0.0425(16) 0.0095(12) 0.0193(15) 0.0033(14) B78 0.080(2) 0.0470(17) 0.0309(14) 0.0034(12) 0.0131(14) 0.0169(15) B79 0.0621(19) 0.0464(17) 0.0475(17) 0.0005(13) 0.0014(14) 0.0184(14) B80 0.0615(17) 0.0353(14) 0.0319(13) -0.0004(11) 0.0066(12) 0.0027(12) B81 0.0527(16) 0.0386(14) 0.0405(15) 0.0025(12) 0.0155(12) 0.0103(12) B82 0.0488(15) 0.0384(14) 0.0363(14) -0.0038(11) 0.0027(11) 0.0082(12) B83 0.0531(16) 0.0420(15) 0.0394(15) 0.0062(12) 0.0155(12) 0.0047(12) C84 0.0431(12) 0.0321(11) 0.0327(11) 0.0017(9) 0.0095(9) 0.0032(9) C85 0.0479(13) 0.0370(12) 0.0302(11) 0.0010(9) 0.0120(9) 0.0107(10) C86 0.0560(15) 0.0367(13) 0.0524(15) 0.0060(11) 0.0130(12) 0.0074(11) C87 0.086(2) 0.0371(14) 0.0635(18) 0.0112(13) 0.0230(16) 0.0149(14) C88 0.100(2) 0.0458(16) 0.0460(15) 0.0118(12) 0.0214(15) 0.0357(16) C89 0.0688(18) 0.0637(18) 0.0393(14) 0.0036(13) 0.0070(12) 0.0282(15) C90 0.0566(15) 0.0471(14) 0.0400(13) 0.0025(11) 0.0072(11) 0.0124(12) _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 N21 1.9831(18) . ? Zn1 N12 1.9933(17) . ? Zn1 N3 2.0136(16) . ? Zn1 Cl2 2.2665(5) . ? N3 C7 1.328(3) . ? N3 N4 1.357(2) . ? N4 C5 1.347(3) . ? C5 C6 1.373(3) . ? C5 C8 1.506(3) . ? C6 C7 1.390(3) . ? C8 C9 1.528(3) . ? C8 C11 1.531(3) . ? C8 C10 1.534(3) . ? N12 C16 1.337(3) . ? N12 N13 1.353(2) . ? N13 C14 1.342(3) . ? C14 C15 1.378(3) . ? C14 C17 1.509(3) . ? C15 C16 1.378(3) . ? C17 C18 1.532(3) . ? C17 C20 1.534(4) . ? C17 C19 1.537(4) . ? N21 C25 1.329(3) . ? N21 N22 1.350(2) . ? N22 C23 1.340(3) . ? C23 C24 1.381(3) . ? C23 C26C 1.495(13) . ? C23 C26B 1.522(12) . ? C23 C26A 1.531(7) . ? C24 C25 1.388(3) . ? C26A C28A 1.487(9) . ? C26A C27A 1.511(9) . ? C26A C29A 1.547(9) . ? C26B C29B 1.490(13) . ? C26B C27B 1.535(14) . ? C26B C28B 1.548(14) . ? C26C C27C 1.492(14) . ? C26C C28C 1.552(15) . ? C26C C29C 1.580(15) . ? B30 B31 1.689(4) . ? B30 B33 1.690(4) . ? B30 B32 1.694(4) . ? B30 B34 1.700(4) . ? B31 B35 1.800(4) . ? B31 B36 1.806(3) . ? B31 B33 1.840(4) . ? B31 B32 1.840(4) . ? B32 B38 1.807(4) . ? B32 B35 1.810(4) . ? B32 B34 1.851(4) . ? B33 B36 1.797(4) . ? B33 B37 1.807(4) . ? B33 B34 1.843(4) . ? B34 B37 1.802(4) . ? B34 B38 1.810(4) . ? B35 C39 1.617(3) . ? B35 B38 1.834(4) . ? B35 B36 1.835(4) . ? B36 C39 1.609(3) . ? B36 B37 1.835(4) . ? B37 C39 1.601(3) . ? B37 B38 1.841(4) . ? B38 C39 1.611(3) . ? C39 C40 1.487(3) . ? C40 C41 1.383(3) . ? C40 C45 1.391(3) . ? C41 C42 1.391(4) . ? C42 C43 1.381(4) . ? C43 C44 1.371(4) . ? C44 C45 1.391(3) . ? Zn46 N66 1.9827(17) . ? Zn46 N48B 1.998(14) . ? Zn46 N57 1.9993(18) . ? Zn46 N48A 2.043(12) . ? Zn46 N48C 2.068(13) . ? Zn46 Cl47 2.2826(6) . ? N48A C52A 1.321(8) . ? N48A N49A 1.363(8) . ? N49A C50A 1.341(6) . ? C50A C51A 1.357(6) . ? C50A C53A 1.511(7) . ? C51A C52A 1.371(7) . ? C53A C56A 1.473(9) . ? C53A C55A 1.484(9) . ? C53A C54A 1.535(9) . ? N48B C52B 1.327(9) . ? N48B N49B 1.350(8) . ? N49B C50B 1.343(7) . ? C50B C51B 1.379(8) . ? C50B C53B 1.529(9) . ? C51B C52B 1.390(9) . ? C53B C56B 1.504(10) . ? C53B C54B 1.542(10) . ? C53B C55B 1.556(11) . ? N48C C52C 1.315(10) . ? N48C N49C 1.363(9) . ? N49C C50C 1.354(9) . ? C50C C51C 1.364(9) . ? C50C C53C 1.530(12) . ? C51C C52C 1.388(9) . ? C53C C55C 1.483(13) . ? C53C C54C 1.516(13) . ? C53C C56C 1.545(13) . ? N57 C61 1.328(3) . ? N57 N58 1.357(2) . ? N58 C59 1.350(3) . ? C59 C60 1.371(3) . ? C59 C62B 1.462(7) . ? C59 C62A 1.573(7) . ? C60 C61 1.385(4) . ? C62A C63A 1.489(9) . ? C62A C65A 1.529(9) . ? C62A C64A 1.538(8) . ? C62B C64B 1.519(8) . ? C62B C63B 1.525(9) . ? C62B C65B 1.546(9) . ? N66 C70 1.333(3) . ? N66 N67 1.356(2) . ? N67 C68 1.347(3) . ? C68 C69 1.373(3) . ? C68 C71A 1.514(9) . ? C68 C71B 1.514(9) . ? C69 C70 1.389(3) . ? C71A C73A 1.491(10) . ? C71A C74A 1.532(10) . ? C71A C72A 1.563(11) . ? C71B C72B 1.513(10) . ? C71B C73B 1.543(9) . ? C71B C74B 1.555(9) . ? B75 B79 1.683(5) . ? B75 B77 1.691(5) . ? B75 B76 1.697(4) . ? B75 B78 1.699(4) . ? B76 B81 1.804(4) . ? B76 B80 1.804(5) . ? B76 B77 1.821(4) . ? B76 B79 1.836(4) . ? B77 B80 1.809(4) . ? B77 B83 1.816(4) . ? B77 B78 1.824(4) . ? B78 B82 1.796(4) . ? B78 B83 1.805(4) . ? B78 B79 1.822(5) . ? B79 B81 1.797(4) . ? B79 B82 1.799(4) . ? B80 C84 1.612(3) . ? B80 B83 1.837(4) . ? B80 B81 1.838(4) . ? B81 C84 1.608(4) . ? B81 B82 1.840(4) . ? B82 C84 1.611(4) . ? B82 B83 1.829(4) . ? B83 C84 1.611(3) . ? C84 C85 1.479(3) . ? C85 C86 1.390(3) . ? C85 C90 1.394(4) . ? C86 C87 1.385(4) . ? C87 C88 1.379(4) . ? C88 C89 1.384(4) . ? C89 C90 1.378(4) . ? C91A C92A 1.497(9) . ? C92A C93A 1.501(9) . ? C93A C94A 1.514(9) . ? C94A C95A 1.534(10) . ? C91B C92B 1.478(9) . ? C92B C93B 1.504(9) . ? C93B C94B 1.528(10) . ? C94B C95B 1.517(10) . ? 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 N21 Zn1 N12 128.32(7) . . ? N21 Zn1 N3 103.91(7) . . ? N12 Zn1 N3 99.64(7) . . ? N21 Zn1 Cl2 108.71(5) . . ? N12 Zn1 Cl2 109.67(5) . . ? N3 Zn1 Cl2 103.13(5) . . ? C7 N3 N4 105.15(16) . . ? C7 N3 Zn1 130.33(14) . . ? N4 N3 Zn1 123.73(13) . . ? C5 N4 N3 112.02(16) . . ? N4 C5 C6 105.98(18) . . ? N4 C5 C8 121.55(18) . . ? C6 C5 C8 132.44(19) . . ? C5 C6 C7 106.19(18) . . ? N3 C7 C6 110.65(18) . . ? C5 C8 C9 110.21(18) . . ? C5 C8 C11 108.93(18) . . ? C9 C8 C11 109.59(19) . . ? C5 C8 C10 108.67(18) . . ? C9 C8 C10 109.58(19) . . ? C11 C8 C10 109.8(2) . . ? C16 N12 N13 105.00(17) . . ? C16 N12 Zn1 124.13(15) . . ? N13 N12 Zn1 130.79(13) . . ? C14 N13 N12 112.21(17) . . ? N13 C14 C15 105.8(2) . . ? N13 C14 C17 122.66(19) . . ? C15 C14 C17 131.5(2) . . ? C16 C15 C14 106.4(2) . . ? N12 C16 C15 110.5(2) . . ? C14 C17 C18 109.1(2) . . ? C14 C17 C20 110.80(19) . . ? C18 C17 C20 108.8(2) . . ? C14 C17 C19 107.8(2) . . ? C18 C17 C19 109.4(2) . . ? C20 C17 C19 110.8(2) . . ? C25 N21 N22 105.07(17) . . ? C25 N21 Zn1 124.43(15) . . ? N22 N21 Zn1 130.31(14) . . ? C23 N22 N21 112.36(18) . . ? N22 C23 C24 106.09(19) . . ? N22 C23 C26C 127.1(6) . . ? C24 C23 C26C 126.6(6) . . ? N22 C23 C26B 119.7(6) . . ? C24 C23 C26B 134.0(6) . . ? N22 C23 C26A 120.7(3) . . ? C24 C23 C26A 132.6(3) . . ? C23 C24 C25 105.6(2) . . ? N21 C25 C24 110.8(2) . . ? C28A C26A C27A 109.6(6) . . ? C28A C26A C23 114.2(5) . . ? C27A C26A C23 109.2(5) . . ? C28A C26A C29A 110.1(6) . . ? C27A C26A C29A 110.2(6) . . ? C23 C26A C29A 103.4(5) . . ? C29B C26B C23 114.2(9) . . ? C29B C26B C27B 106.4(10) . . ? C23 C26B C27B 109.4(10) . . ? C29B C26B C28B 116.2(11) . . ? C23 C26B C28B 104.6(9) . . ? C27B C26B C28B 105.7(10) . . ? C27C C26C C23 114.9(11) . . ? C27C C26C C28C 110.2(11) . . ? C23 C26C C28C 106.0(10) . . ? C27C C26C C29C 110.8(11) . . ? C23 C26C C29C 108.6(9) . . ? C28C C26C C29C 105.9(10) . . ? B31 B30 B33 65.97(16) . . ? B31 B30 B32 65.87(18) . . ? B33 B30 B32 100.69(19) . . ? B31 B30 B34 100.62(19) . . ? B33 B30 B34 65.86(17) . . ? B32 B30 B34 66.09(18) . . ? B30 B31 B35 112.0(2) . . ? B30 B31 B36 111.5(2) . . ? B35 B31 B36 61.16(14) . . ? B30 B31 B33 57.03(16) . . ? B35 B31 B33 102.03(17) . . ? B36 B31 B33 59.06(14) . . ? B30 B31 B32 57.20(17) . . ? B35 B31 B32 59.61(16) . . ? B36 B31 B32 102.28(18) . . ? B33 B31 B32 90.17(18) . . ? B30 B32 B38 111.6(2) . . ? B30 B32 B35 111.3(2) . . ? B38 B32 B35 60.94(15) . . ? B30 B32 B31 56.93(16) . . ? B38 B32 B31 101.92(18) . . ? B35 B32 B31 59.12(15) . . ? B30 B32 B34 57.10(17) . . ? B38 B32 B34 59.30(15) . . ? B35 B32 B34 101.71(18) . . ? B31 B32 B34 89.93(18) . . ? B30 B33 B36 111.9(2) . . ? B30 B33 B37 111.8(2) . . ? B36 B33 B37 61.22(14) . . ? B30 B33 B31 57.00(16) . . ? B36 B33 B31 59.55(14) . . ? B37 B33 B31 102.21(18) . . ? B30 B33 B34 57.35(16) . . ? B36 B33 B34 102.22(18) . . ? B37 B33 B34 59.16(14) . . ? B31 B33 B34 90.19(18) . . ? B30 B34 B37 111.5(2) . . ? B30 B34 B38 111.2(2) . . ? B37 B34 B38 61.30(14) . . ? B30 B34 B33 56.80(15) . . ? B37 B34 B33 59.43(14) . . ? B38 B34 B33 101.92(18) . . ? B30 B34 B32 56.80(17) . . ? B37 B34 B32 102.12(19) . . ? B38 B34 B32 59.14(16) . . ? B33 B34 B32 89.71(18) . . ? C39 B35 B31 108.91(19) . . ? C39 B35 B32 108.8(2) . . ? B31 B35 B32 61.27(16) . . ? C39 B35 B38 55.21(14) . . ? B31 B35 B38 102.40(19) . . ? B32 B35 B38 59.46(16) . . ? C39 B35 B36 55.11(13) . . ? B31 B35 B36 59.58(14) . . ? B32 B35 B36 102.33(19) . . ? B38 B35 B36 90.11(17) . . ? C39 B36 B33 108.91(18) . . ? C39 B36 B31 109.00(18) . . ? B33 B36 B31 61.39(15) . . ? C39 B36 B37 54.92(13) . . ? B33 B36 B37 59.65(14) . . ? B31 B36 B37 102.40(17) . . ? C39 B36 B35 55.55(14) . . ? B33 B36 B35 102.33(18) . . ? B31 B36 B35 59.26(14) . . ? B37 B36 B35 90.08(16) . . ? C39 B37 B34 109.26(19) . . ? C39 B37 B33 108.82(18) . . ? B34 B37 B33 61.42(15) . . ? C39 B37 B36 55.34(14) . . ? B34 B37 B36 102.35(17) . . ? B33 B37 B36 59.13(14) . . ? C39 B37 B38 55.28(14) . . ? B34 B37 B38 59.58(15) . . ? B33 B37 B38 102.11(17) . . ? B36 B37 B38 89.90(16) . . ? C39 B38 B32 109.25(19) . . ? C39 B38 B34 108.39(19) . . ? B32 B38 B34 61.56(16) . . ? C39 B38 B35 55.54(14) . . ? B32 B38 B35 59.60(16) . . ? B34 B38 B35 102.36(18) . . ? C39 B38 B37 54.76(13) . . ? B32 B38 B37 102.30(18) . . ? B34 B38 B37 59.12(15) . . ? B35 B38 B37 89.91(17) . . ? C40 C39 B37 125.92(18) . . ? C40 C39 B36 125.40(19) . . ? B37 C39 B36 69.74(16) . . ? C40 C39 B38 127.06(19) . . ? B37 C39 B38 69.96(16) . . ? B36 C39 B38 107.54(18) . . ? C40 C39 B35 126.5(2) . . ? B37 C39 B35 107.60(18) . . ? B36 C39 B35 69.33(16) . . ? B38 C39 B35 69.25(16) . . ? C41 C40 C45 118.4(2) . . ? C41 C40 C39 121.4(2) . . ? C45 C40 C39 120.2(2) . . ? C40 C41 C42 120.7(3) . . ? C43 C42 C41 120.4(3) . . ? C44 C43 C42 119.5(3) . . ? C43 C44 C45 120.4(3) . . ? C44 C45 C40 120.7(2) . . ? N66 Zn46 N48B 102.7(7) . . ? N66 Zn46 N57 132.99(7) . . ? N48B Zn46 N57 98.4(7) . . ? N66 Zn46 N48A 104.8(5) . . ? N57 Zn46 N48A 97.7(5) . . ? N66 Zn46 N48C 100.3(4) . . ? N57 Zn46 N48C 104.2(4) . . ? N66 Zn46 Cl47 105.28(5) . . ? N48B Zn46 Cl47 107.6(4) . . ? N57 Zn46 Cl47 107.57(6) . . ? N48A Zn46 Cl47 105.6(3) . . ? N48C Zn46 Cl47 102.8(3) . . ? C52A N48A N49A 107.9(10) . . ? C52A N48A Zn46 125.6(7) . . ? N49A N48A Zn46 119.2(9) . . ? C50A N49A N48A 108.8(7) . . ? N49A C50A C51A 107.3(5) . . ? N49A C50A C53A 123.3(5) . . ? C51A C50A C53A 128.6(5) . . ? C50A C51A C52A 107.5(7) . . ? N48A C52A C51A 108.4(10) . . ? C56A C53A C55A 110.8(6) . . ? C56A C53A C50A 113.5(6) . . ? C55A C53A C50A 111.6(5) . . ? C56A C53A C54A 102.4(6) . . ? C55A C53A C54A 111.7(6) . . ? C50A C53A C54A 106.4(5) . . ? C52B N48B N49B 100.9(13) . . ? C52B N48B Zn46 125.8(11) . . ? N49B N48B Zn46 131.5(11) . . ? C50B N49B N48B 114.7(11) . . ? N49B C50B C51B 106.1(8) . . ? N49B C50B C53B 120.2(7) . . ? C51B C50B C53B 133.8(7) . . ? C50B C51B C52B 103.0(11) . . ? N48B C52B C51B 115.1(15) . . ? C56B C53B C50B 107.6(6) . . ? C56B C53B C54B 104.6(7) . . ? C50B C53B C54B 108.3(7) . . ? C56B C53B C55B 118.3(8) . . ? C50B C53B C55B 108.7(7) . . ? C54B C53B C55B 109.0(7) . . ? C52C N48C N49C 102.5(12) . . ? C52C N48C Zn46 128.0(9) . . ? N49C N48C Zn46 127.3(10) . . ? C50C N49C N48C 114.3(12) . . ? N49C C50C C51C 104.1(10) . . ? N49C C50C C53C 121.4(9) . . ? C51C C50C C53C 134.6(9) . . ? C50C C51C C52C 106.5(10) . . ? N48C C52C C51C 112.6(12) . . ? C55C C53C C54C 113.2(11) . . ? C55C C53C C50C 112.6(10) . . ? C54C C53C C50C 108.8(9) . . ? C55C C53C C56C 105.0(10) . . ? C54C C53C C56C 108.1(10) . . ? C50C C53C C56C 109.0(9) . . ? C61 N57 N58 104.99(18) . . ? C61 N57 Zn46 125.32(16) . . ? N58 N57 Zn46 129.69(14) . . ? C59 N58 N57 111.95(18) . . ? N58 C59 C60 105.9(2) . . ? N58 C59 C62B 128.4(3) . . ? C60 C59 C62B 125.7(3) . . ? N58 C59 C62A 118.7(3) . . ? C60 C59 C62A 135.3(3) . . ? C59 C60 C61 106.3(2) . . ? N57 C61 C60 110.9(2) . . ? C63A C62A C65A 111.4(6) . . ? C63A C62A C64A 110.9(6) . . ? C65A C62A C64A 108.8(6) . . ? C63A C62A C59 113.8(6) . . ? C65A C62A C59 106.3(6) . . ? C64A C62A C59 105.3(5) . . ? C59 C62B C64B 111.6(5) . . ? C59 C62B C63B 109.6(6) . . ? C64B C62B C63B 109.5(6) . . ? C59 C62B C65B 108.1(5) . . ? C64B C62B C65B 109.0(6) . . ? C63B C62B C65B 109.0(6) . . ? C70 N66 N67 105.00(17) . . ? C70 N66 Zn46 126.08(15) . . ? N67 N66 Zn46 128.51(14) . . ? C68 N67 N66 112.23(17) . . ? N67 C68 C69 105.86(18) . . ? N67 C68 C71A 122.1(4) . . ? C69 C68 C71A 131.7(4) . . ? N67 C68 C71B 120.8(4) . . ? C69 C68 C71B 133.3(4) . . ? C68 C69 C70 106.4(2) . . ? N66 C70 C69 110.5(2) . . ? C73A C71A C68 111.3(6) . . ? C73A C71A C74A 111.7(7) . . ? C68 C71A C74A 110.3(6) . . ? C73A C71A C72A 109.4(7) . . ? C68 C71A C72A 107.0(6) . . ? C74A C71A C72A 106.9(7) . . ? C72B C71B C68 113.6(6) . . ? C72B C71B C73B 110.3(6) . . ? C68 C71B C73B 108.4(6) . . ? C72B C71B C74B 112.0(6) . . ? C68 C71B C74B 104.7(6) . . ? C73B C71B C74B 107.5(6) . . ? B79 B75 B77 99.3(2) . . ? B79 B75 B76 65.83(19) . . ? B77 B75 B76 65.04(19) . . ? B79 B75 B78 65.2(2) . . ? B77 B75 B78 65.1(2) . . ? B76 B75 B78 99.6(2) . . ? B75 B76 B81 111.7(2) . . ? B75 B76 B80 112.5(2) . . ? B81 B76 B80 61.24(16) . . ? B75 B76 B77 57.34(19) . . ? B81 B76 B77 102.3(2) . . ? B80 B76 B77 59.86(17) . . ? B75 B76 B79 56.72(18) . . ? B81 B76 B79 59.15(17) . . ? B80 B76 B79 101.82(19) . . ? B77 B76 B79 89.33(19) . . ? B75 B77 B80 112.6(2) . . ? B75 B77 B83 112.5(2) . . ? B80 B77 B83 60.90(16) . . ? B75 B77 B76 57.62(18) . . ? B80 B77 B76 59.61(17) . . ? B83 B77 B76 102.41(19) . . ? B75 B77 B78 57.66(18) . . ? B80 B77 B78 102.3(2) . . ? B83 B77 B78 59.45(17) . . ? B76 B77 B78 90.7(2) . . ? B75 B78 B82 112.2(2) . . ? B75 B78 B83 112.7(2) . . ? B82 B78 B83 61.03(16) . . ? B75 B78 B79 56.96(19) . . ? B82 B78 B79 59.61(17) . . ? B83 B78 B79 102.2(2) . . ? B75 B78 B77 57.23(19) . . ? B82 B78 B77 102.49(19) . . ? B83 B78 B77 60.05(17) . . ? B79 B78 B77 89.67(19) . . ? B75 B79 B81 112.7(2) . . ? B75 B79 B82 112.9(2) . . ? B81 B79 B82 61.57(16) . . ? B75 B79 B78 57.85(19) . . ? B81 B79 B78 102.6(2) . . ? B82 B79 B78 59.48(17) . . ? B75 B79 B76 57.45(17) . . ? B81 B79 B76 59.53(16) . . ? B82 B79 B76 102.6(2) . . ? B78 B79 B76 90.3(2) . . ? C84 B80 B76 108.8(2) . . ? C84 B80 B77 108.84(19) . . ? B76 B80 B77 60.54(17) . . ? C84 B80 B83 55.21(14) . . ? B76 B80 B83 102.26(19) . . ? B77 B80 B83 59.76(16) . . ? C84 B80 B81 55.10(15) . . ? B76 B80 B81 59.37(17) . . ? B77 B80 B81 101.4(2) . . ? B83 B80 B81 89.83(17) . . ? C84 B81 B79 108.8(2) . . ? C84 B81 B76 109.0(2) . . ? B79 B81 B76 61.32(17) . . ? C84 B81 B80 55.30(15) . . ? B79 B81 B80 102.0(2) . . ? B76 B81 B80 59.39(17) . . ? C84 B81 B82 55.19(14) . . ? B79 B81 B82 59.27(16) . . ? B76 B81 B82 102.24(19) . . ? B80 B81 B82 89.89(18) . . ? C84 B82 B78 109.1(2) . . ? C84 B82 B79 108.5(2) . . ? B78 B82 B79 60.90(18) . . ? C84 B82 B83 55.41(15) . . ? B78 B82 B83 59.73(17) . . ? B79 B82 B83 102.2(2) . . ? C84 B82 B81 55.06(15) . . ? B78 B82 B81 101.91(19) . . ? B79 B82 B81 59.16(16) . . ? B83 B82 B81 90.02(18) . . ? C84 B83 B78 108.7(2) . . ? C84 B83 B77 108.5(2) . . ? B78 B83 B77 60.50(17) . . ? C84 B83 B82 55.41(15) . . ? B78 B83 B82 59.24(17) . . ? B77 B83 B82 101.5(2) . . ? C84 B83 B80 55.28(14) . . ? B78 B83 B80 101.9(2) . . ? B77 B83 B80 59.34(16) . . ? B82 B83 B80 90.26(18) . . ? C85 C84 B81 125.1(2) . . ? C85 C84 B83 127.4(2) . . ? B81 C84 B83 107.4(2) . . ? C85 C84 B82 126.1(2) . . ? B81 C84 B82 69.74(17) . . ? B83 C84 B82 69.19(18) . . ? C85 C84 B80 126.4(2) . . ? B81 C84 B80 69.60(18) . . ? B83 C84 B80 69.51(17) . . ? B82 C84 B80 107.5(2) . . ? C86 C85 C90 118.3(2) . . ? C86 C85 C84 120.2(2) . . ? C90 C85 C84 121.5(2) . . ? C87 C86 C85 120.8(3) . . ? C88 C87 C86 120.2(3) . . ? C87 C88 C89 119.7(3) . . ? C90 C89 C88 120.2(3) . . ? C89 C90 C85 120.8(3) . . ? C91A C92A C93A 113.4(9) . . ? C92A C93A C94A 111.8(8) . . ? C93A C94A C95A 109.4(9) . . ? C91B C92B C93B 115.0(9) . . ? C92B C93B C94B 109.4(8) . . ? C95B C94B C93B 108.9(9) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N13 H13 Cl2 0.88 2.35 3.1718(18) 154.5 2 N22 H22 Cl2 0.88 2.35 3.1590(19) 153.2 2 N58 H58 Cl47 0.88 2.37 3.1765(19) 151.7 2_666 N67 H67 Cl47 0.88 2.36 3.1734(18) 153.1 2_666 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.577 _refine_diff_density_min -0.753 _refine_diff_density_rms 0.125 #=END data_sr67 _database_code_CSD 192039 _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Chloro-tris(5-tertbutylpyrazole)zinc(II)] [6,7,8,9,10-pentabromo-pentahydro-closo-1-carbanonaborate] hydrate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H36 Cl N6 Zn, C H5 B9 Br5, O H2' _chemical_formula_sum 'C22 H43 B9 Br5 Cl N6 O Zn' _chemical_formula_weight 1005.28 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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 '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' 'Cl' 'Cl' 0.1484 0.1585 '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 Orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z' 'x, -y+1/2, z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, -z' '-x, y-1/2, -z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 24.0110(2) _cell_length_b 12.3005(1) _cell_length_c 27.2856(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8058.73(13) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 99938 _cell_measurement_theta_min 1.49 _cell_measurement_theta_max 27.47 _exptl_crystal_description 'Rectangular prism' _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.657 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3936 _exptl_absorpt_coefficient_mu 5.661 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4645 _exptl_absorpt_correction_T_max 0.6602 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _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 'Nonius KappaCCD diffractometer' _diffrn_measurement_method 'Area detector scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 99938 _diffrn_reflns_av_R_equivalents 0.1049 _diffrn_reflns_av_sigmaI/netI 0.0399 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 27.47 _reflns_number_total 9218 _reflns_number_gt 7160 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. No disorder was detected during refinement, and no restraints were applied. All non-H atoms were refined anisotropically. All H atoms were placed in calculated positions and refined using a riding model except those bound to the water molecule, H30A and H30B. These latter were located in the difference map and allowed to refine freely. The largest residual Fourier peak of 1.5 e.\%A^-3^ lies 1.95\%A from B36. This is consistent with a B-Br distance, suggesting that partial bromination at this site had occurred during synthesis of the pentabromo carbanonaborane anion. Addition of this peak into the model as a Br atom with a fixed thermal parameter of 0.05, led to a refined site occupany of 0.021. This suggests that only ca. 2% of the anion in the crystal was overbrominated. This partial Br atom was not included in the final model. ; _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^)+(0.0332P)^2^+5.8646P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9218 _refine_ls_number_parameters 423 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0505 _refine_ls_R_factor_gt 0.0321 _refine_ls_wR_factor_ref 0.0781 _refine_ls_wR_factor_gt 0.0708 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 Zn1 Zn 0.249228(14) 0.43675(2) 0.369258(11) 0.02662(8) Uani 1 1 d . . . Cl2 Cl 0.25341(3) 0.62011(5) 0.37086(3) 0.03309(16) Uani 1 1 d . . . N3 N 0.29806(10) 0.36483(18) 0.41869(8) 0.0290(5) Uani 1 1 d . . . N4 N 0.28249(10) 0.30956(17) 0.45932(8) 0.0267(5) Uani 1 1 d . . . H4 H 0.2487 0.3110 0.4719 0.032 Uiso 1 1 calc R . . C5 C 0.32526(12) 0.2519(2) 0.47817(10) 0.0293(6) Uani 1 1 d . . . C6 C 0.37054(13) 0.2714(2) 0.44837(12) 0.0377(7) Uani 1 1 d . . . H6 H 0.4071 0.2431 0.4519 0.045 Uiso 1 1 calc R . . C7 C 0.35162(13) 0.3410(2) 0.41218(12) 0.0371(7) Uani 1 1 d . . . H7 H 0.3739 0.3681 0.3861 0.045 Uiso 1 1 calc R . . C8 C 0.31884(13) 0.1802(3) 0.52278(11) 0.0379(7) Uani 1 1 d . . . C9 C 0.27486(15) 0.0933(3) 0.51278(13) 0.0468(8) Uani 1 1 d . . . H9A H 0.2391 0.1283 0.5058 0.070 Uiso 1 1 calc R . . H9B H 0.2711 0.0464 0.5416 0.070 Uiso 1 1 calc R . . H9C H 0.2862 0.0494 0.4845 0.070 Uiso 1 1 calc R . . C10 C 0.37519(16) 0.1272(4) 0.53326(16) 0.0660(12) Uani 1 1 d . . . H10A H 0.3871 0.0853 0.5046 0.099 Uiso 1 1 calc R . . H10B H 0.3718 0.0787 0.5616 0.099 Uiso 1 1 calc R . . H10C H 0.4028 0.1838 0.5403 0.099 Uiso 1 1 calc R . . C11 C 0.30098(19) 0.2494(3) 0.56668(13) 0.0642(11) Uani 1 1 d . . . H11A H 0.3303 0.3021 0.5743 0.096 Uiso 1 1 calc R . . H11B H 0.2947 0.2023 0.5951 0.096 Uiso 1 1 calc R . . H11C H 0.2665 0.2881 0.5587 0.096 Uiso 1 1 calc R . . N12 N 0.17045(10) 0.39797(17) 0.38210(9) 0.0287(5) Uani 1 1 d . . . N13 N 0.14854(10) 0.29583(17) 0.38451(9) 0.0281(5) Uani 1 1 d . . . H13 H 0.1678 0.2362 0.3791 0.034 Uiso 1 1 calc R . . C14 C 0.09423(12) 0.2964(2) 0.39612(11) 0.0305(6) Uani 1 1 d . . . C15 C 0.07957(13) 0.4043(2) 0.40156(12) 0.0388(7) Uani 1 1 d . . . H15 H 0.0439 0.4323 0.4097 0.047 Uiso 1 1 calc R . . C16 C 0.12777(13) 0.4635(2) 0.39262(12) 0.0363(7) Uani 1 1 d . . . H16 H 0.1301 0.5406 0.3938 0.044 Uiso 1 1 calc R . . C17 C 0.06140(13) 0.1920(2) 0.40086(12) 0.0372(7) Uani 1 1 d . . . C18 C 0.00043(16) 0.2197(3) 0.41198(17) 0.0640(11) Uani 1 1 d . . . H18A H -0.0016 0.2632 0.4420 0.096 Uiso 1 1 calc R . . H18B H -0.0208 0.1523 0.4164 0.096 Uiso 1 1 calc R . . H18C H -0.0153 0.2611 0.3846 0.096 Uiso 1 1 calc R . . C19 C 0.06522(19) 0.1283(3) 0.35299(14) 0.0625(12) Uani 1 1 d . . . H19A H 0.0525 0.1741 0.3258 0.094 Uiso 1 1 calc R . . H19B H 0.0416 0.0634 0.3551 0.094 Uiso 1 1 calc R . . H19C H 0.1039 0.1064 0.3473 0.094 Uiso 1 1 calc R . . C20 C 0.08458(17) 0.1238(3) 0.44308(14) 0.0560(10) Uani 1 1 d . . . H20A H 0.1240 0.1079 0.4370 0.084 Uiso 1 1 calc R . . H20B H 0.0637 0.0555 0.4454 0.084 Uiso 1 1 calc R . . H20C H 0.0809 0.1643 0.4738 0.084 Uiso 1 1 calc R . . N21 N 0.28480(10) 0.39314(18) 0.30617(9) 0.0317(5) Uani 1 1 d . . . N22 N 0.29499(10) 0.28973(18) 0.29085(9) 0.0304(5) Uani 1 1 d . . . H22 H 0.2839 0.2313 0.3067 0.036 Uiso 1 1 calc R . . C23 C 0.32400(12) 0.2870(2) 0.24876(10) 0.0295(6) Uani 1 1 d . . . C24 C 0.33319(14) 0.3941(3) 0.23590(12) 0.0417(8) Uani 1 1 d . . . H24 H 0.3524 0.4202 0.2078 0.050 Uiso 1 1 calc R . . C25 C 0.30865(14) 0.4556(3) 0.27242(12) 0.0408(8) Uani 1 1 d . . . H25 H 0.3088 0.5329 0.2733 0.049 Uiso 1 1 calc R . . C26 C 0.33890(12) 0.1816(2) 0.22327(11) 0.0322(6) Uani 1 1 d . . . C27 C 0.35735(16) 0.0960(3) 0.26045(12) 0.0463(8) Uani 1 1 d . . . H27A H 0.3892 0.1236 0.2791 0.069 Uiso 1 1 calc R . . H27B H 0.3681 0.0294 0.2432 0.069 Uiso 1 1 calc R . . H27C H 0.3266 0.0803 0.2829 0.069 Uiso 1 1 calc R . . C28 C 0.28702(13) 0.1416(3) 0.19576(13) 0.0459(8) Uani 1 1 d . . . H28A H 0.2570 0.1278 0.2192 0.069 Uiso 1 1 calc R . . H28B H 0.2959 0.0743 0.1782 0.069 Uiso 1 1 calc R . . H28C H 0.2751 0.1972 0.1723 0.069 Uiso 1 1 calc R . . C29 C 0.38575(13) 0.2029(3) 0.18621(12) 0.0421(8) Uani 1 1 d . . . H29A H 0.3738 0.2587 0.1628 0.063 Uiso 1 1 calc R . . H29B H 0.3943 0.1356 0.1685 0.063 Uiso 1 1 calc R . . H29C H 0.4191 0.2280 0.2036 0.063 Uiso 1 1 calc R . . O30 O 0.17312(11) 0.3207(3) 0.49982(12) 0.0484(6) Uani 1 1 d . . . H30A H 0.162(3) 0.315(5) 0.526(2) 0.11(2) Uiso 1 1 d . . . H30B H 0.150(3) 0.346(6) 0.489(3) 0.15(3) Uiso 1 1 d . . . B31 B 0.09704(14) 0.3163(3) 0.64311(12) 0.0284(7) Uani 1 1 d . . . B32 B 0.03694(14) 0.2966(3) 0.61190(12) 0.0278(7) Uani 1 1 d . . . B33 B 0.08295(14) 0.1845(3) 0.63074(12) 0.0299(7) Uani 1 1 d . . . B34 B 0.08558(14) 0.2396(3) 0.69340(12) 0.0299(7) Uani 1 1 d . . . B35 B 0.03915(14) 0.3523(3) 0.67449(12) 0.0298(7) Uani 1 1 d . . . B36 B 0.00874(15) 0.1615(3) 0.62203(13) 0.0316(7) Uani 1 1 d . . . H36 H -0.0070 0.1112 0.5907 0.038 Uiso 1 1 calc R . . B37 B 0.04328(15) 0.1207(3) 0.67967(13) 0.0329(7) Uani 1 1 d . . . H37 H 0.0548 0.0384 0.6940 0.039 Uiso 1 1 calc R . . B38 B 0.01285(14) 0.2404(3) 0.71068(13) 0.0333(7) Uani 1 1 d . . . H38 H 0.0004 0.2529 0.7498 0.040 Uiso 1 1 calc R . . B39 B -0.02185(14) 0.2807(3) 0.65271(13) 0.0319(7) Uani 1 1 d . . . H39 H -0.0618 0.3249 0.6458 0.038 Uiso 1 1 calc R . . C40 C -0.02034(12) 0.1596(2) 0.67481(11) 0.0352(7) Uani 1 1 d . . . H40 H -0.0577 0.1101 0.6851 0.042 Uiso 1 1 calc R . . Br41 Br 0.161923(13) 0.40046(2) 0.625712(11) 0.03527(8) Uani 1 1 d . . . Br42 Br 0.026010(13) 0.36807(2) 0.548212(11) 0.03542(8) Uani 1 1 d . . . Br43 Br 0.135987(15) 0.09687(3) 0.593078(13) 0.04571(9) Uani 1 1 d . . . Br44 Br 0.142997(13) 0.22865(3) 0.744246(11) 0.03842(8) Uani 1 1 d . . . Br45 Br 0.028811(15) 0.50035(3) 0.698732(13) 0.04468(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 Zn1 0.03087(18) 0.01943(16) 0.02955(17) 0.00196(12) -0.00017(14) -0.00001(12) Cl2 0.0401(4) 0.0192(3) 0.0400(4) 0.0028(3) -0.0078(3) -0.0021(3) N3 0.0294(13) 0.0261(12) 0.0314(13) 0.0053(10) 0.0029(10) 0.0020(10) N4 0.0269(12) 0.0261(12) 0.0272(12) 0.0020(9) 0.0020(10) -0.0001(9) C5 0.0287(15) 0.0295(15) 0.0297(15) 0.0011(11) -0.0042(12) 0.0019(11) C6 0.0286(16) 0.0392(17) 0.0452(19) 0.0074(14) 0.0026(14) 0.0067(13) C7 0.0306(17) 0.0394(18) 0.0414(18) 0.0103(13) 0.0091(14) 0.0015(13) C8 0.0385(18) 0.0420(18) 0.0334(17) 0.0122(13) -0.0033(14) -0.0003(14) C9 0.049(2) 0.0455(19) 0.046(2) 0.0166(15) 0.0016(16) -0.0040(16) C10 0.045(2) 0.079(3) 0.074(3) 0.046(2) -0.009(2) 0.0067(19) C11 0.086(3) 0.076(3) 0.0307(19) 0.0024(18) -0.006(2) -0.008(2) N12 0.0315(13) 0.0195(11) 0.0350(14) 0.0012(9) -0.0008(11) 0.0008(9) N13 0.0297(13) 0.0172(11) 0.0373(14) -0.0026(9) -0.0004(10) -0.0007(9) C14 0.0288(16) 0.0340(16) 0.0288(15) -0.0031(12) -0.0029(12) 0.0003(12) C15 0.0279(16) 0.0365(17) 0.052(2) -0.0021(14) -0.0023(14) 0.0075(13) C16 0.0370(17) 0.0247(15) 0.0470(19) -0.0017(13) -0.0023(14) 0.0042(12) C17 0.0324(17) 0.0391(17) 0.0400(18) -0.0040(13) 0.0019(14) -0.0103(13) C18 0.036(2) 0.071(3) 0.084(3) -0.007(2) 0.005(2) -0.0160(18) C19 0.084(3) 0.052(2) 0.051(2) -0.0144(18) 0.014(2) -0.035(2) C20 0.059(2) 0.048(2) 0.060(2) 0.0117(17) -0.0042(19) -0.0218(18) N21 0.0388(14) 0.0236(12) 0.0325(13) 0.0023(10) 0.0037(11) -0.0011(10) N22 0.0396(14) 0.0214(12) 0.0301(13) 0.0018(9) 0.0052(11) -0.0023(10) C23 0.0282(15) 0.0386(16) 0.0218(14) 0.0019(11) 0.0017(12) -0.0007(12) C24 0.047(2) 0.0396(18) 0.0385(18) 0.0108(14) 0.0142(15) -0.0014(14) C25 0.050(2) 0.0303(16) 0.0422(18) 0.0120(13) 0.0072(16) 0.0007(14) C26 0.0297(16) 0.0395(17) 0.0274(15) -0.0040(12) 0.0009(12) 0.0023(13) C27 0.058(2) 0.0411(19) 0.0396(19) -0.0012(14) 0.0062(16) 0.0122(16) C28 0.0345(18) 0.058(2) 0.045(2) -0.0145(16) 0.0015(15) -0.0085(15) C29 0.0343(18) 0.055(2) 0.0366(18) -0.0066(15) 0.0051(14) 0.0002(15) O30 0.0357(14) 0.0713(18) 0.0383(15) -0.0032(13) 0.0048(12) 0.0046(12) B31 0.0286(17) 0.0281(17) 0.0286(17) 0.0025(13) -0.0012(13) -0.0002(13) B32 0.0278(17) 0.0272(16) 0.0282(16) -0.0012(12) 0.0000(13) 0.0014(12) B33 0.0331(18) 0.0277(17) 0.0289(17) -0.0002(13) -0.0008(14) 0.0039(13) B34 0.0307(18) 0.0322(17) 0.0266(16) -0.0003(13) -0.0017(14) -0.0003(13) B35 0.0295(17) 0.0296(17) 0.0305(17) -0.0047(13) -0.0005(14) 0.0012(13) B36 0.0333(18) 0.0269(17) 0.0346(18) -0.0009(13) -0.0028(14) -0.0015(13) B37 0.0355(19) 0.0288(18) 0.0344(18) 0.0033(13) -0.0032(15) -0.0039(14) B38 0.0304(18) 0.0391(19) 0.0304(18) 0.0007(14) 0.0026(14) -0.0012(14) B39 0.0297(18) 0.0345(19) 0.0316(18) -0.0032(13) 0.0018(14) -0.0018(13) C40 0.0304(16) 0.0406(17) 0.0345(17) 0.0028(13) -0.0005(13) -0.0060(13) Br41 0.02995(16) 0.03991(17) 0.03596(17) 0.00665(12) -0.00069(12) -0.00717(12) Br42 0.03689(17) 0.03818(17) 0.03118(16) 0.00540(12) -0.00432(13) 0.00049(13) Br43 0.0495(2) 0.04207(19) 0.0456(2) -0.00508(14) 0.00937(15) 0.01490(15) Br44 0.03686(17) 0.04442(18) 0.03399(17) 0.00549(13) -0.00808(13) -0.00280(13) Br45 0.0471(2) 0.03438(17) 0.0525(2) -0.01600(14) -0.00300(16) 0.00441(14) _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 N12 1.982(2) . ? Zn1 N3 1.994(2) . ? Zn1 N21 1.995(2) . ? Zn1 Cl2 2.2580(7) . ? N3 C7 1.331(4) . ? N3 N4 1.353(3) . ? N4 C5 1.350(3) . ? C5 C6 1.379(4) . ? C5 C8 1.511(4) . ? C6 C7 1.383(4) . ? C8 C9 1.527(5) . ? C8 C10 1.529(5) . ? C8 C11 1.531(5) . ? N12 C16 1.335(4) . ? N12 N13 1.364(3) . ? N13 C14 1.342(4) . ? C14 C15 1.381(4) . ? C14 C17 1.513(4) . ? C15 C16 1.389(4) . ? C17 C19 1.526(5) . ? C17 C20 1.530(5) . ? C17 C18 1.533(5) . ? N21 C25 1.329(4) . ? N21 N22 1.361(3) . ? N22 C23 1.343(4) . ? C23 C24 1.382(4) . ? C23 C26 1.514(4) . ? C24 C25 1.383(5) . ? C26 C27 1.527(4) . ? C26 C29 1.535(4) . ? C26 C28 1.535(4) . ? O30 H30A 0.75(6) . ? O30 H30B 0.71(7) . ? B31 B34 1.687(4) . ? B31 B33 1.690(5) . ? B31 B35 1.692(5) . ? B31 B32 1.693(5) . ? B31 Br41 1.930(3) . ? B32 B39 1.808(5) . ? B32 B36 1.816(5) . ? B32 B33 1.840(5) . ? B32 B35 1.841(5) . ? B32 Br42 1.965(3) . ? B33 B37 1.818(5) . ? B33 B36 1.820(5) . ? B33 B34 1.840(5) . ? B33 Br43 1.960(3) . ? B34 B38 1.809(5) . ? B34 B37 1.820(5) . ? B34 B35 1.852(5) . ? B34 Br44 1.961(3) . ? B35 B38 1.808(5) . ? B35 B39 1.810(5) . ? B35 Br45 1.953(3) . ? B36 C40 1.601(5) . ? B36 B39 1.841(5) . ? B36 B37 1.847(5) . ? B37 C40 1.606(5) . ? B37 B38 1.849(5) . ? B38 C40 1.607(5) . ? B38 B39 1.855(5) . ? B39 C40 1.607(5) . ? 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 N12 Zn1 N3 109.56(9) . . ? N12 Zn1 N21 119.76(10) . . ? N3 Zn1 N21 102.28(10) . . ? N12 Zn1 Cl2 106.23(7) . . ? N3 Zn1 Cl2 113.82(7) . . ? N21 Zn1 Cl2 105.44(7) . . ? C7 N3 N4 105.4(2) . . ? C7 N3 Zn1 125.1(2) . . ? N4 N3 Zn1 127.92(18) . . ? C5 N4 N3 111.5(2) . . ? N4 C5 C6 106.5(2) . . ? N4 C5 C8 122.4(3) . . ? C6 C5 C8 131.1(3) . . ? C5 C6 C7 105.7(3) . . ? N3 C7 C6 111.0(3) . . ? C5 C8 C9 109.6(3) . . ? C5 C8 C10 108.0(3) . . ? C9 C8 C10 110.3(3) . . ? C5 C8 C11 109.6(3) . . ? C9 C8 C11 109.6(3) . . ? C10 C8 C11 109.8(3) . . ? C16 N12 N13 104.5(2) . . ? C16 N12 Zn1 128.70(19) . . ? N13 N12 Zn1 126.76(18) . . ? C14 N13 N12 112.4(2) . . ? N13 C14 C15 106.1(3) . . ? N13 C14 C17 121.5(3) . . ? C15 C14 C17 132.4(3) . . ? C14 C15 C16 105.8(3) . . ? N12 C16 C15 111.2(3) . . ? C14 C17 C19 109.4(3) . . ? C14 C17 C20 109.9(3) . . ? C19 C17 C20 110.0(3) . . ? C14 C17 C18 109.0(3) . . ? C19 C17 C18 109.9(3) . . ? C20 C17 C18 108.7(3) . . ? C25 N21 N22 104.5(2) . . ? C25 N21 Zn1 128.8(2) . . ? N22 N21 Zn1 126.39(17) . . ? C23 N22 N21 112.3(2) . . ? N22 C23 C24 106.0(3) . . ? N22 C23 C26 122.5(2) . . ? C24 C23 C26 131.5(3) . . ? C23 C24 C25 105.7(3) . . ? N21 C25 C24 111.5(3) . . ? C23 C26 C27 110.7(2) . . ? C23 C26 C29 109.2(3) . . ? C27 C26 C29 110.0(3) . . ? C23 C26 C28 107.9(2) . . ? C27 C26 C28 109.9(3) . . ? C29 C26 C28 109.1(2) . . ? H30A O30 H30B 100(6) . . ? B34 B31 B33 66.0(2) . . ? B34 B31 B35 66.5(2) . . ? B33 B31 B35 100.8(2) . . ? B34 B31 B32 101.0(2) . . ? B33 B31 B32 65.9(2) . . ? B35 B31 B32 65.9(2) . . ? B34 B31 Br41 129.2(2) . . ? B33 B31 Br41 128.8(2) . . ? B35 B31 Br41 130.3(2) . . ? B32 B31 Br41 129.9(2) . . ? B31 B32 B39 111.8(2) . . ? B31 B32 B36 111.8(2) . . ? B39 B32 B36 61.06(18) . . ? B31 B32 B33 56.95(18) . . ? B39 B32 B33 102.4(2) . . ? B36 B32 B33 59.71(18) . . ? B31 B32 B35 57.02(18) . . ? B39 B32 B35 59.45(18) . . ? B36 B32 B35 102.1(2) . . ? B33 B32 B35 90.1(2) . . ? B31 B32 Br42 119.7(2) . . ? B39 B32 Br42 119.3(2) . . ? B36 B32 Br42 119.6(2) . . ? B33 B32 Br42 131.5(2) . . ? B35 B32 Br42 131.1(2) . . ? B31 B33 B37 111.9(2) . . ? B31 B33 B36 111.8(2) . . ? B37 B33 B36 61.04(19) . . ? B31 B33 B32 57.14(18) . . ? B37 B33 B32 102.4(2) . . ? B36 B33 B32 59.48(18) . . ? B31 B33 B34 56.92(18) . . ? B37 B33 B34 59.66(18) . . ? B36 B33 B34 102.3(2) . . ? B32 B33 B34 90.2(2) . . ? B31 B33 Br43 120.2(2) . . ? B37 B33 Br43 119.2(2) . . ? B36 B33 Br43 118.8(2) . . ? B32 B33 Br43 131.0(2) . . ? B34 B33 Br43 131.9(2) . . ? B31 B34 B38 111.5(2) . . ? B31 B34 B37 111.9(2) . . ? B38 B34 B37 61.25(19) . . ? B31 B34 B33 57.04(18) . . ? B38 B34 B33 102.2(2) . . ? B37 B34 B33 59.57(18) . . ? B31 B34 B35 56.88(18) . . ? B38 B34 B35 59.17(18) . . ? B37 B34 B35 102.0(2) . . ? B33 B34 B35 89.8(2) . . ? B31 B34 Br44 120.0(2) . . ? B38 B34 Br44 119.6(2) . . ? B37 B34 Br44 118.9(2) . . ? B33 B34 Br44 131.0(2) . . ? B35 B34 Br44 132.2(2) . . ? B31 B35 B38 111.4(2) . . ? B31 B35 B39 111.8(2) . . ? B38 B35 B39 61.70(19) . . ? B31 B35 B32 57.10(18) . . ? B38 B35 B32 102.3(2) . . ? B39 B35 B32 59.38(18) . . ? B31 B35 B34 56.65(18) . . ? B38 B35 B34 59.24(18) . . ? B39 B35 B34 102.4(2) . . ? B32 B35 B34 89.8(2) . . ? B31 B35 Br45 121.3(2) . . ? B38 B35 Br45 118.7(2) . . ? B39 B35 Br45 117.5(2) . . ? B32 B35 Br45 131.1(2) . . ? B34 B35 Br45 132.8(2) . . ? C40 B36 B32 108.2(2) . . ? C40 B36 B33 108.2(2) . . ? B32 B36 B33 60.81(18) . . ? C40 B36 B39 55.14(19) . . ? B32 B36 B39 59.27(18) . . ? B33 B36 B39 102.0(2) . . ? C40 B36 B37 54.96(19) . . ? B32 B36 B37 102.2(2) . . ? B33 B36 B37 59.43(18) . . ? B39 B36 B37 90.5(2) . . ? C40 B37 B33 108.0(2) . . ? C40 B37 B34 108.0(2) . . ? B33 B37 B34 60.77(18) . . ? C40 B37 B36 54.68(18) . . ? B33 B37 B36 59.53(18) . . ? B34 B37 B36 102.0(2) . . ? C40 B37 B38 54.88(19) . . ? B33 B37 B38 101.5(2) . . ? B34 B37 B38 59.09(18) . . ? B36 B37 B38 89.8(2) . . ? C40 B38 B35 108.1(2) . . ? C40 B38 B34 108.5(2) . . ? B35 B38 B34 61.60(18) . . ? C40 B38 B37 54.86(19) . . ? B35 B38 B37 102.6(2) . . ? B34 B38 B37 59.66(18) . . ? C40 B38 B39 54.75(18) . . ? B35 B38 B39 59.19(18) . . ? B34 B38 B39 102.3(2) . . ? B37 B38 B39 90.0(2) . . ? C40 B39 B32 108.3(2) . . ? C40 B39 B35 108.0(2) . . ? B32 B39 B35 61.16(18) . . ? C40 B39 B36 54.81(18) . . ? B32 B39 B36 59.67(18) . . ? B35 B39 B36 102.4(2) . . ? C40 B39 B38 54.73(19) . . ? B32 B39 B38 101.7(2) . . ? B35 B39 B38 59.10(18) . . ? B36 B39 B38 89.8(2) . . ? B36 C40 B37 70.4(2) . . ? B36 C40 B38 108.8(2) . . ? B37 C40 B38 70.3(2) . . ? B36 C40 B39 70.1(2) . . ? B37 C40 B39 109.2(2) . . ? B38 C40 B39 70.5(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N4 H4 O30 0.88 1.97 2.852(4) 177.7 . N13 H13 Cl2 0.88 2.38 3.218(2) 159.1 2_545 N22 H22 Cl2 0.88 2.40 3.236(2) 159.9 2_545 O30 H30A Br41 0.75(6) 2.92(6) 3.582(3) 148(6) . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.464 _refine_diff_density_min -0.560 _refine_diff_density_rms 0.085