Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name _publ_author_address 'Sylvie L. Renard' ; 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 ; 'Julie Fisher' ; Department of Chemistry, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, UK ; 'Malcolm A. Halcrow' ; School of Chemistry, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, UK ; _publ_contact_author_name 'Dr. Malcolm A. Halcrow' _publ_contact_address ; School of Chemistry, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, UK ; _publ_contact_author_phone '+44 (0)113 233 6506' _publ_contact_author_fax '+44 (0)113 233 6565' _publ_contact_author_email M.A.HALCROW@CHEM.LEEDS.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_contact_letter ; The following data is for six structures included in a manuscript we have just submitted to the Dalton office. ; _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Supramolecular Anion Binding by the [ZnCl(Hpz^tBu^)~3~]^+^ Cation (Hpz^tBu^ = 5-Tertbutylpyrazole). ; #================================================================= data_sr5 _database_code_CSD 191073 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Chloro-tris[5-tertbutylpyrazole]zinc(II) chloride ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H36 Cl N6 Zn, Cl' _chemical_formula_sum 'C21 H36 Cl2 N6 Zn' _chemical_formula_weight 508.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.2537(3) _cell_length_b 10.6738(1) _cell_length_c 14.6666(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.7416(5) _cell_angle_gamma 90.00 _cell_volume 2623.72(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 31333 _cell_measurement_theta_min 2.83 _cell_measurement_theta_max 30.06 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.288 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 1.158 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6805 _exptl_absorpt_correction_T_max 0.9029 _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 31333 _diffrn_reflns_av_R_equivalents 0.0485 _diffrn_reflns_av_sigmaI/netI 0.0397 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 30.06 _reflns_number_total 7681 _reflns_number_gt 6463 _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. All non-H atoms were refined anisotropically, and no restraints were applied. The three N-bound H atoms H4, H13 and H22 were located in the difference map and allowed to refine freely. All other 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^)+(0.0414P)^2^+0.8024P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7681 _refine_ls_number_parameters 292 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0433 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0878 _refine_ls_wR_factor_gt 0.0819 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.207445(10) 0.560212(15) 0.476906(11) 0.02247(6) Uani 1 1 d . . . Cl2 Cl 0.15738(3) 0.42200(4) 0.56045(3) 0.03445(9) Uani 1 1 d . . . N3 N 0.12304(7) 0.69256(10) 0.43864(8) 0.0224(2) Uani 1 1 d . . . N4 N 0.12243(8) 0.78942(11) 0.37858(8) 0.0220(2) Uani 1 1 d . . . H4 H 0.1634(12) 0.8014(18) 0.3601(14) 0.036(5) Uiso 1 1 d . . . C5 C 0.05386(8) 0.85450(13) 0.36270(9) 0.0224(3) Uani 1 1 d . . . C6 C 0.00678(9) 0.79627(14) 0.41460(11) 0.0271(3) Uani 1 1 d . . . H6 H -0.0455 0.8194 0.4183 0.032 Uiso 1 1 calc R . . C7 C 0.05225(9) 0.69645(14) 0.46029(10) 0.0259(3) Uani 1 1 d . . . H7 H 0.0351 0.6393 0.5011 0.031 Uiso 1 1 calc R . . C8 C 0.03847(9) 0.96376(13) 0.29514(10) 0.0254(3) Uani 1 1 d . . . C9 C 0.11059(11) 1.05194(15) 0.31305(14) 0.0388(4) Uani 1 1 d . . . H9A H 0.1215 1.0827 0.3778 0.058 Uiso 1 1 calc R . . H9B H 0.0991 1.1230 0.2696 0.058 Uiso 1 1 calc R . . H9C H 0.1573 1.0065 0.3032 0.058 Uiso 1 1 calc R . . C10 C 0.02307(12) 0.91143(16) 0.19462(11) 0.0369(4) Uani 1 1 d . . . H10A H 0.0703 0.8655 0.1869 0.055 Uiso 1 1 calc R . . H10B H 0.0120 0.9807 0.1496 0.055 Uiso 1 1 calc R . . H10C H -0.0229 0.8547 0.1834 0.055 Uiso 1 1 calc R . . C11 C -0.03502(10) 1.03584(15) 0.30736(12) 0.0347(4) Uani 1 1 d . . . H11A H -0.0811 0.9794 0.2961 0.052 Uiso 1 1 calc R . . H11B H -0.0459 1.1053 0.2624 0.052 Uiso 1 1 calc R . . H11C H -0.0251 1.0690 0.3714 0.052 Uiso 1 1 calc R . . N12 N 0.22332(7) 0.47179(11) 0.36093(8) 0.0235(2) Uani 1 1 d . . . N13 N 0.24860(7) 0.52444(11) 0.28902(8) 0.0238(2) Uani 1 1 d . . . H13 H 0.2602(12) 0.605(2) 0.2930(14) 0.037(5) Uiso 1 1 d . . . C14 C 0.25102(9) 0.44106(13) 0.22093(10) 0.0234(3) Uani 1 1 d . . . C15 C 0.22656(9) 0.32733(14) 0.25005(10) 0.0267(3) Uani 1 1 d . . . H15 H 0.2221 0.2496 0.2177 0.032 Uiso 1 1 calc R . . C16 C 0.20993(9) 0.35128(13) 0.33720(10) 0.0261(3) Uani 1 1 d . . . H16 H 0.1916 0.2904 0.3744 0.031 Uiso 1 1 calc R . . C17 C 0.27671(9) 0.48038(15) 0.13336(10) 0.0277(3) Uani 1 1 d . . . C18 C 0.27494(14) 0.36810(19) 0.06927(13) 0.0501(5) Uani 1 1 d . . . H18A H 0.3138 0.3056 0.1008 0.075 Uiso 1 1 calc R . . H18B H 0.2885 0.3951 0.0111 0.075 Uiso 1 1 calc R . . H18C H 0.2214 0.3311 0.0545 0.075 Uiso 1 1 calc R . . C19 C 0.36070(11) 0.53500(19) 0.16054(13) 0.0415(4) Uani 1 1 d . . . H19A H 0.3607 0.6103 0.1987 0.062 Uiso 1 1 calc R . . H19B H 0.3781 0.5569 0.1036 0.062 Uiso 1 1 calc R . . H19C H 0.3973 0.4729 0.1967 0.062 Uiso 1 1 calc R . . C20 C 0.22016(13) 0.5825(2) 0.08219(13) 0.0490(5) Uani 1 1 d . . . H20A H 0.1658 0.5491 0.0637 0.073 Uiso 1 1 calc R . . H20B H 0.2373 0.6091 0.0261 0.073 Uiso 1 1 calc R . . H20C H 0.2213 0.6543 0.1241 0.073 Uiso 1 1 calc R . . N21 N 0.31656(8) 0.61335(12) 0.55095(8) 0.0254(2) Uani 1 1 d . . . N22 N 0.37345(8) 0.67461(12) 0.51850(9) 0.0259(2) Uani 1 1 d . . . H22 H 0.3603(11) 0.7095(18) 0.4635(14) 0.033(5) Uiso 1 1 d . . . C23 C 0.44391(9) 0.67733(14) 0.58235(11) 0.0300(3) Uani 1 1 d . . . C24 C 0.43190(10) 0.61382(17) 0.65988(12) 0.0371(4) Uani 1 1 d . . . H24 H 0.4702 0.5991 0.7171 0.045 Uiso 1 1 calc R . . C25 C 0.35252(10) 0.57577(15) 0.63726(11) 0.0320(3) Uani 1 1 d . . . H25 H 0.3275 0.5295 0.6776 0.038 Uiso 1 1 calc R . . C26 C 0.51813(10) 0.73723(16) 0.56328(13) 0.0370(4) Uani 1 1 d . . . C27 C 0.57641(11) 0.63260(19) 0.55161(16) 0.0468(5) Uani 1 1 d . . . H27A H 0.5874 0.5789 0.6074 0.070 Uiso 1 1 calc R . . H27B H 0.6263 0.6699 0.5438 0.070 Uiso 1 1 calc R . . H27C H 0.5526 0.5823 0.4961 0.070 Uiso 1 1 calc R . . C28 C 0.55837(12) 0.8186(2) 0.64765(18) 0.0582(6) Uani 1 1 d . . . H28A H 0.5221 0.8862 0.6556 0.087 Uiso 1 1 calc R . . H28B H 0.6076 0.8546 0.6367 0.087 Uiso 1 1 calc R . . H28C H 0.5711 0.7668 0.7045 0.087 Uiso 1 1 calc R . . C29 C 0.49788(12) 0.8168(2) 0.47459(18) 0.0552(6) Uani 1 1 d . . . H29A H 0.4756 0.7632 0.4204 0.083 Uiso 1 1 calc R . . H29B H 0.5464 0.8576 0.4656 0.083 Uiso 1 1 calc R . . H29C H 0.4586 0.8807 0.4807 0.083 Uiso 1 1 calc R . . Cl30 Cl 0.28849(2) 0.80504(3) 0.33161(3) 0.02888(8) 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 0.02329(10) 0.02250(9) 0.02191(9) 0.00215(6) 0.00597(6) 0.00069(6) Cl2 0.0386(2) 0.03070(18) 0.0383(2) 0.01196(15) 0.01769(17) 0.00247(15) N3 0.0242(6) 0.0207(5) 0.0222(5) 0.0026(4) 0.0050(4) -0.0008(4) N4 0.0215(6) 0.0219(5) 0.0230(5) 0.0041(4) 0.0060(5) -0.0011(4) C5 0.0220(7) 0.0217(6) 0.0227(6) -0.0002(5) 0.0033(5) -0.0012(5) C6 0.0231(7) 0.0283(7) 0.0311(7) 0.0043(6) 0.0093(6) 0.0024(5) C7 0.0263(7) 0.0262(7) 0.0269(7) 0.0034(5) 0.0098(6) -0.0017(6) C8 0.0260(7) 0.0227(6) 0.0261(7) 0.0038(5) 0.0034(6) 0.0005(5) C9 0.0362(9) 0.0295(8) 0.0480(10) 0.0112(7) 0.0047(8) -0.0055(6) C10 0.0508(11) 0.0329(8) 0.0259(7) 0.0044(6) 0.0071(7) 0.0044(7) C11 0.0332(9) 0.0305(7) 0.0395(9) 0.0040(6) 0.0071(7) 0.0077(6) N12 0.0243(6) 0.0249(5) 0.0221(5) 0.0017(4) 0.0067(5) -0.0021(5) N13 0.0257(6) 0.0224(5) 0.0236(5) 0.0012(4) 0.0068(5) -0.0029(5) C14 0.0204(7) 0.0255(6) 0.0239(6) -0.0009(5) 0.0047(5) -0.0005(5) C15 0.0300(8) 0.0236(6) 0.0271(7) -0.0024(5) 0.0078(6) -0.0019(6) C16 0.0284(7) 0.0235(6) 0.0270(7) 0.0021(5) 0.0076(6) -0.0021(5) C17 0.0283(8) 0.0317(7) 0.0246(6) 0.0013(6) 0.0094(6) -0.0020(6) C18 0.0745(15) 0.0460(10) 0.0391(9) -0.0128(8) 0.0321(10) -0.0166(10) C19 0.0353(9) 0.0545(11) 0.0368(9) 0.0038(8) 0.0125(7) -0.0116(8) C20 0.0461(11) 0.0674(13) 0.0349(9) 0.0205(9) 0.0126(8) 0.0150(10) N21 0.0241(6) 0.0280(6) 0.0242(5) -0.0008(5) 0.0058(5) 0.0006(5) N22 0.0240(6) 0.0258(6) 0.0278(6) -0.0002(5) 0.0056(5) 0.0000(5) C23 0.0239(7) 0.0290(7) 0.0357(8) -0.0052(6) 0.0043(6) 0.0037(6) C24 0.0304(9) 0.0465(9) 0.0303(8) 0.0006(7) -0.0013(6) 0.0041(7) C25 0.0318(8) 0.0388(8) 0.0253(7) 0.0018(6) 0.0066(6) 0.0041(6) C26 0.0214(8) 0.0361(8) 0.0523(10) -0.0032(7) 0.0063(7) -0.0003(6) C27 0.0293(9) 0.0432(10) 0.0701(13) -0.0076(9) 0.0161(9) 0.0040(7) C28 0.0311(10) 0.0537(12) 0.0858(16) -0.0273(11) 0.0058(10) -0.0057(9) C29 0.0305(10) 0.0577(12) 0.0785(15) 0.0202(11) 0.0154(10) -0.0049(9) Cl30 0.02911(19) 0.02711(16) 0.03233(18) 0.00408(13) 0.01108(14) -0.00264(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N3 2.0108(12) . ? Zn1 N21 2.0184(12) . ? Zn1 N12 2.0200(12) . ? Zn1 Cl2 2.2196(4) . ? N3 C7 1.3335(19) . ? N3 N4 1.3567(16) . ? N4 H4 0.83(2) . ? N4 C5 1.3437(19) . ? C5 C6 1.385(2) . ? C5 C8 1.5125(19) . ? C6 C7 1.396(2) . ? C8 C11 1.530(2) . ? C8 C9 1.532(2) . ? C8 C10 1.539(2) . ? N12 C16 1.3382(18) . ? N12 N13 1.3554(17) . ? N13 H13 0.88(2) . ? N13 C14 1.3456(18) . ? C14 C15 1.385(2) . ? C14 C17 1.514(2) . ? C15 C16 1.398(2) . ? C17 C18 1.519(2) . ? C17 C19 1.525(2) . ? C17 C20 1.534(2) . ? N21 C25 1.3324(19) . ? N21 N22 1.3563(18) . ? N22 H22 0.868(19) . ? N22 C23 1.3471(19) . ? C23 C24 1.381(2) . ? C23 C26 1.515(2) . ? C24 C25 1.391(2) . ? C26 C29 1.523(3) . ? C26 C28 1.536(3) . ? C26 C27 1.539(2) . ? 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 N3 Zn1 N21 118.29(5) . . ? N3 Zn1 N12 109.11(5) . . ? N21 Zn1 N12 106.78(5) . . ? N3 Zn1 Cl2 105.66(4) . . ? N21 Zn1 Cl2 108.99(4) . . ? N12 Zn1 Cl2 107.62(4) . . ? C7 N3 N4 105.35(11) . . ? C7 N3 Zn1 126.80(9) . . ? N4 N3 Zn1 127.58(10) . . ? H4 N4 C5 130.6(14) . . ? H4 N4 N3 117.2(14) . . ? C5 N4 N3 112.15(12) . . ? N4 C5 C6 106.25(12) . . ? N4 C5 C8 121.50(13) . . ? C6 C5 C8 132.17(13) . . ? C5 C6 C7 105.67(13) . . ? N3 C7 C6 110.58(13) . . ? C5 C8 C11 109.41(13) . . ? C5 C8 C9 110.63(12) . . ? C11 C8 C9 109.45(13) . . ? C5 C8 C10 108.13(12) . . ? C11 C8 C10 109.60(13) . . ? C9 C8 C10 109.60(15) . . ? C16 N12 N13 105.29(11) . . ? C16 N12 Zn1 128.21(10) . . ? N13 N12 Zn1 126.48(9) . . ? H13 N13 C14 130.4(13) . . ? H13 N13 N12 117.6(13) . . ? C14 N13 N12 112.06(12) . . ? N13 C14 C15 106.58(13) . . ? N13 C14 C17 120.87(12) . . ? C15 C14 C17 132.55(13) . . ? C14 C15 C16 105.38(13) . . ? N12 C16 C15 110.68(13) . . ? C14 C17 C18 109.83(13) . . ? C14 C17 C19 109.62(13) . . ? C18 C17 C19 109.98(16) . . ? C14 C17 C20 109.36(13) . . ? C18 C17 C20 109.91(15) . . ? C19 C17 C20 108.11(15) . . ? C25 N21 N22 105.43(13) . . ? C25 N21 Zn1 126.22(11) . . ? N22 N21 Zn1 127.37(9) . . ? H22 N22 C23 129.1(13) . . ? H22 N22 N21 118.8(13) . . ? C23 N22 N21 112.05(13) . . ? N22 C23 C24 105.94(14) . . ? N22 C23 C26 122.91(15) . . ? C24 C23 C26 131.12(15) . . ? C23 C24 C25 106.19(14) . . ? N21 C25 C24 110.39(15) . . ? C23 C26 C29 111.13(14) . . ? C23 C26 C28 109.26(16) . . ? C29 C26 C28 109.94(17) . . ? C23 C26 C27 108.50(14) . . ? C29 C26 C27 109.44(18) . . ? C28 C26 C27 108.51(15) . . ? 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 Cl30 0.83(2) 2.29(2) 3.1062(14) 168.3(19) . N13 H13 Cl30 0.88(2) 2.24(2) 3.1032(13) 169.1(18) . N22 H22 Cl30 0.868(19) 2.275(19) 3.1131(14) 162.0(17) . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.06 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.372 _refine_diff_density_min -0.750 _refine_diff_density_rms 0.112 #=END data_sr10 _database_code_CSD 191074 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Chloro-tris[5-tertbutylpyrazole]zinc(II) tetrafluoroborate dichloromethane solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H36 Cl N6 Zn, B F4, C H2 Cl2' _chemical_formula_sum 'C22 H38 B Cl3 F4 N6 Zn' _chemical_formula_weight 645.11 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.5359(3) _cell_length_b 10.7282(2) _cell_length_c 18.5742(3) _cell_angle_alpha 90.00 _cell_angle_beta 116.4774(6) _cell_angle_gamma 90.00 _cell_volume 3127.83(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 30436 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 27.50 _exptl_crystal_description 'Rectangular prism' _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.370 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 1.087 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4767 _exptl_absorpt_correction_T_max 0.7022 _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 30436 _diffrn_reflns_av_R_equivalents 0.0674 _diffrn_reflns_av_sigmaI/netI 0.0435 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7131 _reflns_number_gt 5769 _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 one complex cation, one tetrafluoroborate anion, and a badly disordered region of solvent that was modelled as dichloromethane. All three tertbutyl groups are disordered: C8A-C11A (occupancy 0.60) and C8B-C11B (occupancy 0.40) C17A-C20A (occupancy 0.70) and C17B-C20B (occupancy 0.30) C26A-C29A (occupancy 0.50), C26B-C29B (occupancy 0.30) and C26A, C27C-C29C (occupancy 0.20; ie C26A has a total occupancy of 0.70). All disordered C-C bonds were restrained to 1.53(2)\%A, and 1,3-C...C distances within a given disorder orientation to 2.50(2)\%A. The BF~4~^-^ anion is disordered over two equally occupied orientations, B30A-F34A and B30B-F34B. All B-F distances were restrained to 1.36(2)\%A, and F...F distances within a given disorder orientation to 2.22(2)\%A. The disordered region of solvent was modelled as four partial molecules of dichloromethane, although the high thermal parameters on some of these atoms means that this model is somewhat speculative. This region lies near the inversion centre at 1-x, -y, -z, although potential disorder across this special position was not modeled. C35A-Cl37A (occupancy 0.25) C35B-Cl37B (occupancy 0.25) C35C-Cl37C (occupancy 0.30) C35D-Cl37D (occupancy 0.20) All disordered C-Cl bonds were restrained to 1.76(2)\%A, and 1,3-Cl...Cl distances within a given disorder orientation to 2.87(2)\%A. All non-H atoms with occupancy >=0.5 were refined anisotropically, while 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^)+(0.0817P)^2^+2.0036P] 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 SHELXL _refine_ls_extinction_coef 0.0140(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7131 _refine_ls_number_parameters 463 _refine_ls_number_restraints 101 _refine_ls_R_factor_all 0.0655 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.1496 _refine_ls_wR_factor_gt 0.1372 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.284846(17) 0.45728(3) 0.837176(17) 0.03438(14) Uani 1 1 d . . . Cl2 Cl 0.34669(5) 0.54436(7) 0.96002(4) 0.0483(2) Uani 1 1 d . . . N3 N 0.19297(13) 0.3497(2) 0.84331(13) 0.0348(4) Uani 1 1 d . A . N4 N 0.13998(13) 0.26467(19) 0.79084(13) 0.0351(5) Uani 1 1 d . A . H4 H 0.1359 0.2520 0.7424 0.042 Uiso 1 1 calc R . . C5 C 0.09453(16) 0.2020(2) 0.82100(16) 0.0381(6) Uani 1 1 d D . . C6 C 0.11852(19) 0.2480(3) 0.89658(19) 0.0492(7) Uani 1 1 d . A . H6 H 0.0976 0.2232 0.9336 0.059 Uiso 1 1 calc R . . C7 C 0.17965(17) 0.3385(3) 0.90838(17) 0.0423(6) Uani 1 1 d . . . H7 H 0.2081 0.3858 0.9562 0.051 Uiso 1 1 calc R A . C8A C 0.0307(7) 0.1007(9) 0.7734(7) 0.045(9) Uani 0.60 1 d PD A 1 C9A C -0.0522(4) 0.1624(6) 0.7124(5) 0.0586(19) Uani 0.60 1 d PD A 1 H9A1 H -0.0728 0.2206 0.7405 0.088 Uiso 0.60 1 calc PR A 1 H9A2 H -0.0953 0.0981 0.6856 0.088 Uiso 0.60 1 calc PR A 1 H9A3 H -0.0412 0.2078 0.6721 0.088 Uiso 0.60 1 calc PR A 1 C10A C 0.0666(7) 0.0162(9) 0.7293(8) 0.081(4) Uani 0.60 1 d PD A 1 H10A H 0.0734 0.0643 0.6877 0.122 Uiso 0.60 1 calc PR A 1 H10B H 0.0272 -0.0532 0.7042 0.122 Uiso 0.60 1 calc PR A 1 H10C H 0.1220 -0.0167 0.7677 0.122 Uiso 0.60 1 calc PR A 1 C11A C 0.0120(5) 0.0200(6) 0.8318(5) 0.0642(19) Uani 0.60 1 d PD A 1 H11A H 0.0644 -0.0219 0.8693 0.096 Uiso 0.60 1 calc PR A 1 H11B H -0.0311 -0.0425 0.8014 0.096 Uiso 0.60 1 calc PR A 1 H11C H -0.0092 0.0729 0.8619 0.096 Uiso 0.60 1 calc PR A 1 C8B C 0.0305(11) 0.1025(16) 0.7751(10) 0.048(13) Uiso 0.40 1 d PD A 2 C9B C -0.0380(8) 0.1540(14) 0.6950(7) 0.059(4) Uiso 0.40 1 d PD A 2 H9B1 H -0.0805 0.0891 0.6675 0.089 Uiso 0.40 1 calc PR A 2 H9B2 H -0.0113 0.1797 0.6609 0.089 Uiso 0.40 1 calc PR A 2 H9B3 H -0.0659 0.2259 0.7057 0.089 Uiso 0.40 1 calc PR A 2 C10B C 0.0777(11) -0.0014(14) 0.7552(9) 0.062(4) Uiso 0.40 1 d PD A 2 H10D H 0.1079 0.0339 0.7264 0.093 Uiso 0.40 1 calc PR A 2 H10E H 0.0367 -0.0639 0.7212 0.093 Uiso 0.40 1 calc PR A 2 H10F H 0.1188 -0.0407 0.8051 0.093 Uiso 0.40 1 calc PR A 2 C11B C -0.0110(7) 0.0553(10) 0.8261(7) 0.057(3) Uiso 0.40 1 d PD A 2 H11D H 0.0331 0.0256 0.8779 0.086 Uiso 0.40 1 calc PR A 2 H11E H -0.0498 -0.0134 0.7982 0.086 Uiso 0.40 1 calc PR A 2 H11F H -0.0431 0.1231 0.8353 0.086 Uiso 0.40 1 calc PR A 2 N12 N 0.37968(13) 0.3557(2) 0.83240(13) 0.0358(5) Uani 1 1 d . B . N13 N 0.37959(14) 0.2850(2) 0.77183(14) 0.0388(5) Uani 1 1 d . B . H13 H 0.3349 0.2755 0.7249 0.047 Uiso 1 1 calc R . . C14 C 0.45573(17) 0.2312(2) 0.79167(18) 0.0411(6) Uani 1 1 d D . . C15 C 0.50760(18) 0.2686(3) 0.8690(2) 0.0462(7) Uani 1 1 d . B . H15 H 0.5656 0.2464 0.9005 0.055 Uiso 1 1 calc R . . C16 C 0.45840(16) 0.3452(3) 0.89174(17) 0.0400(6) Uani 1 1 d . . . H16 H 0.4781 0.3848 0.9426 0.048 Uiso 1 1 calc R B . C17A C 0.4692(7) 0.1480(9) 0.7322(6) 0.060(5) Uani 0.70 1 d PD B 1 C18A C 0.4545(10) 0.2200(12) 0.6573(6) 0.097(5) Uani 0.70 1 d PD B 1 H18A H 0.3954 0.2493 0.6308 0.145 Uiso 0.70 1 calc PR B 1 H18B H 0.4655 0.1657 0.6204 0.145 Uiso 0.70 1 calc PR B 1 H18C H 0.4932 0.2917 0.6719 0.145 Uiso 0.70 1 calc PR B 1 C19A C 0.5616(7) 0.0985(12) 0.7743(8) 0.098(5) Uani 0.70 1 d PD B 1 H19A H 0.6015 0.1686 0.7878 0.148 Uiso 0.70 1 calc PR B 1 H19B H 0.5714 0.0412 0.7382 0.148 Uiso 0.70 1 calc PR B 1 H19C H 0.5705 0.0544 0.8236 0.148 Uiso 0.70 1 calc PR B 1 C20A C 0.4073(8) 0.0372(9) 0.7114(8) 0.076(6) Uani 0.70 1 d PD B 1 H20A H 0.4119 -0.0008 0.7612 0.114 Uiso 0.70 1 calc PR B 1 H20B H 0.4216 -0.0247 0.6806 0.114 Uiso 0.70 1 calc PR B 1 H20C H 0.3488 0.0666 0.6792 0.114 Uiso 0.70 1 calc PR B 1 C17B C 0.4731(13) 0.1435(18) 0.7365(10) 0.041(7) Uiso 0.30 1 d PD B 2 C18B C 0.4616(14) 0.214(2) 0.6599(10) 0.057(6) Uiso 0.30 1 d PD B 2 H18D H 0.4016 0.2376 0.6287 0.086 Uiso 0.30 1 calc PR B 2 H18E H 0.4791 0.1609 0.6272 0.086 Uiso 0.30 1 calc PR B 2 H18F H 0.4968 0.2900 0.6751 0.086 Uiso 0.30 1 calc PR B 2 C19B C 0.5629(11) 0.091(2) 0.7778(11) 0.049(5) Uiso 0.30 1 d PD B 2 H19D H 0.6041 0.1599 0.7924 0.074 Uiso 0.30 1 calc PR B 2 H19E H 0.5720 0.0343 0.7411 0.074 Uiso 0.30 1 calc PR B 2 H19F H 0.5706 0.0462 0.8264 0.074 Uiso 0.30 1 calc PR B 2 C20B C 0.4081(15) 0.0372(17) 0.7085(13) 0.052(8) Uiso 0.30 1 d PD B 2 H20D H 0.4109 -0.0080 0.7555 0.078 Uiso 0.30 1 calc PR B 2 H20E H 0.4211 -0.0200 0.6743 0.078 Uiso 0.30 1 calc PR B 2 H20F H 0.3508 0.0715 0.6779 0.078 Uiso 0.30 1 calc PR B 2 N21 N 0.25051(13) 0.6075(2) 0.76341(13) 0.0373(5) Uani 1 1 d . D . N22 N 0.21081(14) 0.6146(2) 0.68181(14) 0.0407(5) Uani 1 1 d . D . H22 H 0.1923 0.5493 0.6500 0.049 Uiso 1 1 calc R . . C23 C 0.20313(18) 0.7325(3) 0.65533(18) 0.0477(7) Uani 1 1 d D . . C24 C 0.2404(2) 0.8060(3) 0.7231(2) 0.0520(7) Uani 1 1 d . D . H24 H 0.2456 0.8942 0.7249 0.062 Uiso 1 1 calc R . . C25 C 0.26859(19) 0.7253(3) 0.78820(19) 0.0454(6) Uani 1 1 d . . . H25 H 0.2969 0.7504 0.8429 0.054 Uiso 1 1 calc R D . C26A C 0.1667(4) 0.7599(7) 0.5656(4) 0.0563(17) Uani 0.70 1 d PD C . C27A C 0.1799(8) 0.8960(8) 0.5533(6) 0.081(3) Uani 0.50 1 d PD C 1 H27A H 0.2410 0.9144 0.5780 0.122 Uiso 0.50 1 calc PR C 1 H27B H 0.1522 0.9476 0.5784 0.122 Uiso 0.50 1 calc PR C 1 H27C H 0.1549 0.9142 0.4956 0.122 Uiso 0.50 1 calc PR C 1 C28A C 0.2116(6) 0.6835(12) 0.5245(5) 0.066(2) Uani 0.50 1 d PD C 1 H28A H 0.1873 0.7057 0.4674 0.098 Uiso 0.50 1 calc PR C 1 H28B H 0.2030 0.5943 0.5298 0.098 Uiso 0.50 1 calc PR C 1 H28C H 0.2727 0.7023 0.5504 0.098 Uiso 0.50 1 calc PR C 1 C29A C 0.0727(4) 0.7261(12) 0.5298(7) 0.070(3) Uani 0.50 1 d PD C 1 H29A H 0.0458 0.7717 0.5582 0.105 Uiso 0.50 1 calc PR C 1 H29B H 0.0668 0.6362 0.5356 0.105 Uiso 0.50 1 calc PR C 1 H29C H 0.0448 0.7484 0.4727 0.105 Uiso 0.50 1 calc PR C 1 C26B C 0.1504(9) 0.7771(14) 0.5701(9) 0.042(4) Uiso 0.30 1 d PD D 2 C27B C 0.2183(8) 0.8249(14) 0.5443(8) 0.072(3) Uiso 0.30 1 d PD D 2 H27D H 0.1915 0.8382 0.4859 0.108 Uiso 0.30 1 calc PR D 2 H27E H 0.2638 0.7630 0.5588 0.108 Uiso 0.30 1 calc PR D 2 H27F H 0.2422 0.9037 0.5718 0.108 Uiso 0.30 1 calc PR D 2 C28B C 0.1061(7) 0.6644(9) 0.5155(6) 0.048(2) Uiso 0.30 1 d PD D 2 H28D H 0.0619 0.6319 0.5292 0.072 Uiso 0.30 1 calc PR D 2 H28E H 0.1482 0.5990 0.5238 0.072 Uiso 0.30 1 calc PR D 2 H28F H 0.0800 0.6908 0.4591 0.072 Uiso 0.30 1 calc PR D 2 C29B C 0.0858(8) 0.8769(11) 0.5584(8) 0.071(3) Uiso 0.30 1 d PD D 2 H29D H 0.1145 0.9498 0.5910 0.106 Uiso 0.30 1 calc PR D 2 H29E H 0.0437 0.8452 0.5750 0.106 Uiso 0.30 1 calc PR D 2 H29F H 0.0572 0.9007 0.5015 0.106 Uiso 0.30 1 calc PR D 2 C27C C 0.1529(16) 0.9026(14) 0.5550(15) 0.072(9) Uiso 0.20 1 d PD C 3 H27G H 0.1242 0.9318 0.5867 0.109 Uiso 0.20 1 calc PR C 3 H27H H 0.1175 0.9219 0.4981 0.109 Uiso 0.20 1 calc PR C 3 H27I H 0.2081 0.9444 0.5735 0.109 Uiso 0.20 1 calc PR C 3 C28C C 0.2248(16) 0.721(3) 0.5303(15) 0.078(11) Uiso 0.20 1 d PD C 3 H28G H 0.2023 0.7512 0.4749 0.117 Uiso 0.20 1 calc PR C 3 H28H H 0.2287 0.6298 0.5308 0.117 Uiso 0.20 1 calc PR C 3 H28I H 0.2816 0.7563 0.5623 0.117 Uiso 0.20 1 calc PR C 3 C29C C 0.0795(11) 0.695(2) 0.5225(13) 0.045(6) Uiso 0.20 1 d PD C 3 H29G H 0.0406 0.7292 0.5424 0.068 Uiso 0.20 1 calc PR C 3 H29H H 0.0864 0.6054 0.5332 0.068 Uiso 0.20 1 calc PR C 3 H29I H 0.0560 0.7097 0.4644 0.068 Uiso 0.20 1 calc PR C 3 B30A B 0.1669(10) 0.2914(15) 0.6166(9) 0.035(3) Uani 0.50 1 d PD E 1 F31A F 0.2049(7) 0.3529(11) 0.6850(6) 0.089(4) Uani 0.50 1 d PD E 1 F32A F 0.1327(9) 0.3798(12) 0.5566(7) 0.122(5) Uani 0.50 1 d PD E 1 F33A F 0.2292(10) 0.2305(14) 0.6028(12) 0.070(3) Uani 0.50 1 d PD E 1 F34A F 0.1106(5) 0.2115(6) 0.6211(4) 0.0554(15) Uani 0.50 1 d PD E 1 B30B B 0.1755(11) 0.3116(16) 0.6192(9) 0.045(5) Uani 0.50 1 d PD F 2 F31B F 0.2098(4) 0.3561(7) 0.6926(3) 0.0328(17) Uani 0.50 1 d PD F 2 F32B F 0.1269(4) 0.3950(8) 0.5612(4) 0.0497(14) Uani 0.50 1 d PD F 2 F33B F 0.2363(11) 0.2573(16) 0.6008(11) 0.096(5) Uani 0.50 1 d PD F 2 F34B F 0.1177(10) 0.2165(13) 0.6096(9) 0.167(6) Uani 0.50 1 d PD F 2 C35A C 0.3572(9) 0.1169(15) -0.0307(9) 0.050(4) Uiso 0.25 1 d PD G 1 H35A H 0.3547 0.2057 -0.0174 0.060 Uiso 0.25 1 calc PR G 1 H35B H 0.3354 0.1072 -0.0896 0.060 Uiso 0.25 1 calc PR G 1 Cl36A Cl 0.4612(6) 0.0535(9) 0.0231(6) 0.148(3) Uiso 0.25 1 d PD . 1 Cl37A Cl 0.3044(7) 0.0215(12) 0.0074(8) 0.184(4) Uiso 0.25 1 d PD G 1 C35B C 0.3392(19) 0.087(3) -0.0464(11) 0.088(9) Uiso 0.25 1 d PD H 2 H35C H 0.2813 0.0729 -0.0513 0.105 Uiso 0.25 1 calc PR H 2 H35D H 0.3539 0.1761 -0.0338 0.105 Uiso 0.25 1 calc PR H 2 Cl36B Cl 0.3423(5) 0.0488(7) -0.1341(4) 0.102(2) Uiso 0.25 1 d PD H 2 Cl37B Cl 0.4129(9) -0.0069(14) 0.0298(7) 0.207(5) Uiso 0.25 1 d PD H 2 C35C C 0.3214(11) 0.0834(14) -0.0379(8) 0.062(4) Uiso 0.30 1 d PD I 3 H35E H 0.2806 0.1462 -0.0367 0.074 Uiso 0.30 1 calc PR I 3 H35F H 0.3797 0.1044 0.0030 0.074 Uiso 0.30 1 calc PR I 3 Cl36C Cl 0.3156(3) 0.0676(4) -0.1337(3) 0.0709(10) Uiso 0.30 1 d PD I 3 Cl37C Cl 0.2913(8) -0.0730(11) -0.0255(7) 0.209(4) Uiso 0.30 1 d PD I 3 C35D C 0.3973(12) 0.055(2) -0.0410(16) 0.104(8) Uiso 0.20 1 d PD J 4 H35G H 0.4024 0.0529 0.0143 0.124 Uiso 0.20 1 calc PR J 4 H35H H 0.4244 0.1322 -0.0480 0.124 Uiso 0.20 1 calc PR J 4 Cl36D Cl 0.2931(5) 0.0442(7) -0.1119(5) 0.100(2) Uiso 0.20 1 d PD J 4 Cl37D Cl 0.4412(7) -0.0781(11) -0.0622(7) 0.153(3) Uiso 0.20 1 d PD J 4 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 0.02903(19) 0.03303(19) 0.0378(2) -0.00441(12) 0.01195(14) -0.00131(10) Cl2 0.0418(4) 0.0545(4) 0.0408(4) -0.0152(3) 0.0116(3) -0.0069(3) N3 0.0319(10) 0.0347(11) 0.0341(10) -0.0050(9) 0.0113(8) -0.0013(8) N4 0.0351(10) 0.0323(11) 0.0349(10) -0.0043(9) 0.0131(9) -0.0027(8) C5 0.0327(12) 0.0348(13) 0.0432(14) 0.0028(11) 0.0137(11) 0.0005(10) C6 0.0489(16) 0.0567(18) 0.0466(16) -0.0011(14) 0.0255(13) -0.0083(14) C7 0.0409(14) 0.0486(16) 0.0376(13) -0.0089(12) 0.0176(11) -0.0058(12) C8A 0.038(8) 0.027(6) 0.061(12) -0.003(2) 0.014(4) -0.011(2) C9A 0.041(3) 0.043(3) 0.065(4) -0.006(3) -0.001(3) -0.014(2) C10A 0.074(6) 0.055(5) 0.123(11) -0.047(6) 0.051(7) -0.028(4) C11A 0.063(4) 0.039(3) 0.087(5) 0.004(3) 0.030(4) -0.017(3) N12 0.0317(10) 0.0349(11) 0.0388(11) -0.0043(9) 0.0139(9) -0.0015(8) N13 0.0382(11) 0.0364(11) 0.0404(12) -0.0097(9) 0.0163(9) -0.0037(9) C14 0.0394(14) 0.0344(13) 0.0556(16) -0.0050(12) 0.0266(12) -0.0043(11) C15 0.0316(13) 0.0419(15) 0.0616(18) -0.0049(13) 0.0176(12) -0.0006(11) C16 0.0328(12) 0.0402(14) 0.0435(14) -0.0055(11) 0.0139(11) -0.0021(10) C17A 0.057(5) 0.044(4) 0.094(8) -0.026(3) 0.049(5) -0.009(2) C18A 0.163(12) 0.073(5) 0.104(7) -0.028(4) 0.104(8) -0.014(5) C19A 0.061(4) 0.095(7) 0.153(10) -0.061(6) 0.060(5) 0.000(3) C20A 0.067(6) 0.045(4) 0.130(11) -0.044(4) 0.056(5) -0.017(3) N21 0.0320(10) 0.0356(11) 0.0407(12) -0.0024(9) 0.0130(9) -0.0033(8) N22 0.0377(11) 0.0371(12) 0.0409(12) -0.0022(10) 0.0118(10) -0.0062(9) C23 0.0409(14) 0.0424(15) 0.0543(17) 0.0045(13) 0.0161(13) -0.0080(12) C24 0.0564(18) 0.0343(14) 0.0601(19) 0.0008(13) 0.0212(15) -0.0051(13) C25 0.0499(16) 0.0355(14) 0.0492(16) -0.0072(12) 0.0206(13) -0.0043(12) C26A 0.043(3) 0.065(4) 0.055(3) 0.018(3) 0.016(3) -0.004(3) C27A 0.086(8) 0.070(6) 0.075(6) 0.033(5) 0.024(5) -0.020(5) C28A 0.051(4) 0.096(7) 0.045(4) 0.008(4) 0.016(3) -0.006(5) C29A 0.035(4) 0.087(8) 0.069(6) 0.029(5) 0.006(3) 0.002(4) B30A 0.034(5) 0.028(5) 0.036(6) -0.004(3) 0.010(4) -0.013(4) F31A 0.081(7) 0.076(8) 0.128(8) 0.016(6) 0.062(7) 0.005(5) F32A 0.185(10) 0.102(7) 0.067(6) 0.005(5) 0.046(6) 0.069(6) F33A 0.080(5) 0.059(3) 0.065(6) -0.016(3) 0.027(4) 0.021(3) F34A 0.064(3) 0.048(3) 0.044(2) -0.016(2) 0.014(2) -0.035(3) B30B 0.034(6) 0.034(6) 0.050(8) 0.010(6) 0.003(5) -0.004(5) F31B 0.034(3) 0.044(4) 0.0104(17) -0.016(2) 0.0008(17) -0.010(3) F32B 0.051(3) 0.053(3) 0.035(3) 0.009(2) 0.011(2) 0.012(2) F33B 0.088(7) 0.132(13) 0.055(5) -0.008(7) 0.021(5) 0.036(7) F34B 0.120(10) 0.118(9) 0.192(13) 0.000(8) 0.007(8) -0.021(8) _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 2.023(2) . ? Zn1 N21 2.025(2) . ? Zn1 N3 2.026(2) . ? Zn1 Cl2 2.2469(7) . ? N3 C7 1.335(3) . ? N3 N4 1.356(3) . ? N4 C5 1.341(3) . ? C5 C6 1.365(4) . ? C5 C8B 1.508(16) . ? C5 C8A 1.528(9) . ? C6 C7 1.389(4) . ? C8A C10A 1.532(12) . ? C8A C11A 1.533(11) . ? C8A C9A 1.538(11) . ? C8B C11B 1.517(15) . ? C8B C10B 1.528(16) . ? C8B C9B 1.538(16) . ? N12 C16 1.333(3) . ? N12 N13 1.356(3) . ? N13 C14 1.347(3) . ? C14 C15 1.373(4) . ? C14 C17A 1.519(8) . ? C14 C17B 1.519(16) . ? C15 C16 1.388(4) . ? C17A C18A 1.510(11) . ? C17A C20A 1.538(9) . ? C17A C19A 1.546(10) . ? C17B C19B 1.518(16) . ? C17B C20B 1.531(17) . ? C17B C18B 1.546(16) . ? N21 C25 1.334(4) . ? N21 N22 1.359(3) . ? N22 C23 1.342(4) . ? C23 C24 1.379(4) . ? C23 C26B 1.512(14) . ? C23 C26A 1.524(7) . ? C24 C25 1.386(4) . ? C26A C28C 1.496(15) . ? C26A C27A 1.512(9) . ? C26A C29A 1.522(9) . ? C26A C29C 1.539(14) . ? C26A C27C 1.549(15) . ? C26A C28A 1.551(11) . ? C26B C29B 1.503(14) . ? C26B C28B 1.546(15) . ? C26B C27B 1.554(15) . ? B30A F31A 1.318(14) . ? B30A F34A 1.339(14) . ? B30A F32A 1.380(14) . ? B30A F33A 1.392(13) . ? B30B F31B 1.310(15) . ? B30B F32B 1.368(14) . ? B30B F33B 1.386(15) . ? B30B F34B 1.392(15) . ? C35A Cl37A 1.729(14) . ? C35A Cl36A 1.778(13) . ? C35B Cl36B 1.703(17) . ? C35B Cl37B 1.749(18) . ? C35C Cl36C 1.745(13) . ? C35C Cl37C 1.804(15) . ? C35D Cl36D 1.716(18) . ? C35D Cl37D 1.751(18) . ? 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 N21 113.65(9) . . ? N12 Zn1 N3 112.70(9) . . ? N21 Zn1 N3 119.15(8) . . ? N12 Zn1 Cl2 103.56(6) . . ? N21 Zn1 Cl2 102.69(7) . . ? N3 Zn1 Cl2 102.45(6) . . ? C7 N3 N4 104.4(2) . . ? C7 N3 Zn1 124.56(18) . . ? N4 N3 Zn1 130.56(17) . . ? C5 N4 N3 112.4(2) . . ? N4 C5 C6 106.3(2) . . ? N4 C5 C8B 123.3(7) . . ? C6 C5 C8B 130.4(7) . . ? N4 C5 C8A 122.2(5) . . ? C6 C5 C8A 131.5(5) . . ? C8B C5 C8A 1.2(10) . . ? C5 C6 C7 106.1(3) . . ? N3 C7 C6 110.8(2) . . ? C5 C8A C10A 111.2(7) . . ? C5 C8A C11A 109.0(7) . . ? C10A C8A C11A 108.2(8) . . ? C5 C8A C9A 109.1(7) . . ? C10A C8A C9A 109.8(9) . . ? C11A C8A C9A 109.5(8) . . ? C5 C8B C11B 109.0(11) . . ? C5 C8B C10B 107.8(12) . . ? C11B C8B C10B 111.8(12) . . ? C5 C8B C9B 110.9(12) . . ? C11B C8B C9B 109.8(12) . . ? C10B C8B C9B 107.6(12) . . ? C16 N12 N13 104.9(2) . . ? C16 N12 Zn1 125.30(18) . . ? N13 N12 Zn1 129.84(17) . . ? C14 N13 N12 112.2(2) . . ? N13 C14 C15 105.9(2) . . ? N13 C14 C17A 120.7(5) . . ? C15 C14 C17A 133.4(5) . . ? N13 C14 C17B 123.6(8) . . ? C15 C14 C17B 130.4(8) . . ? C17A C14 C17B 3.5(11) . . ? C14 C15 C16 106.3(2) . . ? N12 C16 C15 110.7(2) . . ? C18A C17A C14 110.6(7) . . ? C18A C17A C20A 110.7(8) . . ? C14 C17A C20A 108.3(7) . . ? C18A C17A C19A 110.6(8) . . ? C14 C17A C19A 107.5(7) . . ? C20A C17A C19A 109.0(8) . . ? C19B C17B C14 111.3(13) . . ? C19B C17B C20B 110.1(14) . . ? C14 C17B C20B 110.3(14) . . ? C19B C17B C18B 109.1(13) . . ? C14 C17B C18B 109.5(13) . . ? C20B C17B C18B 106.4(13) . . ? C25 N21 N22 104.8(2) . . ? C25 N21 Zn1 124.5(2) . . ? N22 N21 Zn1 130.50(17) . . ? C23 N22 N21 112.3(2) . . ? N22 C23 C24 106.0(3) . . ? N22 C23 C26B 126.6(6) . . ? C24 C23 C26B 126.6(6) . . ? N22 C23 C26A 120.4(4) . . ? C24 C23 C26A 133.3(4) . . ? C26B C23 C26A 14.3(6) . . ? C23 C24 C25 106.2(3) . . ? N21 C25 C24 110.7(3) . . ? C27A C26A C29A 111.9(8) . . ? C28C C26A C23 112.9(11) . . ? C27A C26A C23 109.4(6) . . ? C29A C26A C23 106.0(6) . . ? C28C C26A C29C 111.1(12) . . ? C23 C26A C29C 108.5(10) . . ? C28C C26A C27C 108.6(11) . . ? C23 C26A C27C 107.1(11) . . ? C29C C26A C27C 108.5(11) . . ? C27A C26A C28A 106.9(8) . . ? C29A C26A C28A 110.4(8) . . ? C23 C26A C28A 112.3(6) . . ? C29B C26B C23 116.5(10) . . ? C29B C26B C28B 109.6(10) . . ? C23 C26B C28B 109.5(10) . . ? C29B C26B C27B 110.6(11) . . ? C23 C26B C27B 103.5(9) . . ? C28B C26B C27B 106.7(10) . . ? F31A B30A F34A 109.2(10) . . ? F31A B30A F32A 106.6(12) . . ? F34A B30A F32A 115.1(12) . . ? F31A B30A F33A 108.2(12) . . ? F34A B30A F33A 111.9(13) . . ? F32A B30A F33A 105.6(11) . . ? F31B B30B F32B 114.7(12) . . ? F31B B30B F33B 111.2(13) . . ? F32B B30B F33B 111.0(13) . . ? F31B B30B F34B 111.8(13) . . ? F32B B30B F34B 102.5(12) . . ? F33B B30B F34B 104.9(13) . . ? Cl37A C35A Cl36A 98.4(8) . . ? Cl36B C35B Cl37B 107.9(12) . . ? Cl36C C35C Cl37C 98.8(8) . . ? Cl36D C35D Cl37D 101.3(11) . . ? 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 F31A 0.88 2.22 2.838(12) 127.0 . N4 H4 F34A 0.88 2.14 3.013(6) 172.8 . N4 H4 F31B 0.88 2.20 2.790(7) 123.7 . N4 H4 F34B 0.88 2.37 3.253(15) 177.3 . N13 H13 F31A 0.88 2.22 2.848(12) 128.0 . N13 H13 F33A 0.88 2.25 3.126(19) 172.9 . N13 H13 F31B 0.88 2.18 2.775(7) 124.7 . N13 H13 F33B 0.88 2.19 3.062(19) 171.7 . N22 H22 F31A 0.88 2.19 2.811(12) 127.5 . N22 H22 F32A 0.88 2.41 3.284(14) 175.8 . N22 H22 F31B 0.88 2.19 2.781(8) 124.0 . N22 H22 F32B 0.88 2.26 3.129(9) 172.0 . _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.704 _refine_diff_density_min -0.729 _refine_diff_density_rms 0.111 #=END data_sr13-2 _database_code_CSD 191075 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Chloro-tris[5-tertbutylpyrazole]zinc(II) perchlorate chloroform solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H36 Cl N6 Zn, Cl O4, C H Cl3' _chemical_formula_sum 'C22 H37 Cl5 N6 O4 Zn' _chemical_formula_weight 692.20 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.9363(1) _cell_length_b 10.0965(1) _cell_length_c 31.8586(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.7932(7) _cell_angle_gamma 90.00 _cell_volume 3173.68(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25384 _cell_measurement_theta_min 2.12 _cell_measurement_theta_max 27.50 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.449 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 1.232 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6724 _exptl_absorpt_correction_T_max 0.8273 _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 25384 _diffrn_reflns_av_R_equivalents 0.0729 _diffrn_reflns_av_sigmaI/netI 0.0489 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7236 _reflns_number_gt 6264 _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. One tert-butyl ligand is disordered over two orientations: C(26A)-C(29A), occupancy 0.6 and C(26B)-C(29B), occupancy 0.4. All disordered C-C bonds were restrained to 1.52(2)\%A, and 1,3-C...C distances within a given disorder orientation to 2.48(2)\%A. All non-H atoms with occupancy >0.5 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^)+(0.0517P)^2^+1.5808P] 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 SHELXL _refine_ls_extinction_coef 0.0063(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7236 _refine_ls_number_parameters 361 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0480 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.1050 _refine_ls_wR_factor_gt 0.0984 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.051 _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 0.37353(2) 0.14228(2) 0.604514(6) 0.02339(9) Uani 1 1 d . . . Cl2 Cl 0.52102(5) 0.28154(5) 0.579855(15) 0.03154(13) Uani 1 1 d . . . N3 N 0.48523(17) 0.03658(16) 0.64996(5) 0.0257(3) Uani 1 1 d . . . N4 N 0.44782(16) -0.05281(16) 0.67817(5) 0.0248(3) Uani 1 1 d . . . H4 H 0.3632 -0.0692 0.6821 0.030 Uiso 1 1 calc R . . C5 C 0.5559(2) -0.1135(2) 0.69951(6) 0.0269(4) Uani 1 1 d . . . C6 C 0.6686(2) -0.0603(2) 0.68456(7) 0.0336(5) Uani 1 1 d . . . H6 H 0.7606 -0.0817 0.6934 0.040 Uiso 1 1 calc R . . C7 C 0.6202(2) 0.0312(2) 0.65385(6) 0.0322(4) Uani 1 1 d . . . H7 H 0.6757 0.0828 0.6378 0.039 Uiso 1 1 calc R . . C8 C 0.5439(2) -0.2177(2) 0.73293(6) 0.0329(5) Uani 1 1 d . . . C9 C 0.4008(2) -0.2752(3) 0.72917(8) 0.0444(6) Uani 1 1 d . . . H9A H 0.3362 -0.2050 0.7339 0.067 Uiso 1 1 calc R . . H9B H 0.3968 -0.3451 0.7503 0.067 Uiso 1 1 calc R . . H9C H 0.3776 -0.3124 0.7008 0.067 Uiso 1 1 calc R . . C10 C 0.5777(4) -0.1549(3) 0.77686(8) 0.0553(8) Uani 1 1 d . . . H10A H 0.6683 -0.1154 0.7791 0.083 Uiso 1 1 calc R . . H10B H 0.5755 -0.2233 0.7986 0.083 Uiso 1 1 calc R . . H10C H 0.5108 -0.0862 0.7809 0.083 Uiso 1 1 calc R . . C11 C 0.6466(3) -0.3272(3) 0.72723(9) 0.0478(6) Uani 1 1 d . . . H11A H 0.6288 -0.3638 0.6986 0.072 Uiso 1 1 calc R . . H11B H 0.6382 -0.3976 0.7479 0.072 Uiso 1 1 calc R . . H11C H 0.7385 -0.2905 0.7315 0.072 Uiso 1 1 calc R . . N12 N 0.23386(17) 0.26318(16) 0.62456(5) 0.0258(3) Uani 1 1 d . . . N13 N 0.13525(16) 0.23893(16) 0.64941(5) 0.0238(3) Uani 1 1 d . . . H13 H 0.1169 0.1599 0.6589 0.029 Uiso 1 1 calc R . . C14 C 0.0684(2) 0.35001(18) 0.65795(6) 0.0252(4) Uani 1 1 d . . . C15 C 0.1260(2) 0.4514(2) 0.63724(7) 0.0332(5) Uani 1 1 d . . . H15 H 0.1011 0.5422 0.6368 0.040 Uiso 1 1 calc R . . C16 C 0.2276(2) 0.3938(2) 0.61721(7) 0.0326(4) Uani 1 1 d . . . H16 H 0.2850 0.4406 0.6005 0.039 Uiso 1 1 calc R . . C17 C -0.0473(2) 0.3504(2) 0.68493(6) 0.0290(4) Uani 1 1 d . . . C18 C -0.1785(3) 0.3802(3) 0.65656(9) 0.0536(7) Uani 1 1 d . . . H18A H -0.1710 0.4665 0.6429 0.080 Uiso 1 1 calc R . . H18B H -0.2543 0.3820 0.6736 0.080 Uiso 1 1 calc R . . H18C H -0.1945 0.3113 0.6349 0.080 Uiso 1 1 calc R . . C19 C -0.0587(3) 0.2174(2) 0.70691(8) 0.0411(5) Uani 1 1 d . . . H19A H -0.0800 0.1481 0.6856 0.062 Uiso 1 1 calc R . . H19B H -0.1309 0.2219 0.7253 0.062 Uiso 1 1 calc R . . H19C H 0.0275 0.1968 0.7239 0.062 Uiso 1 1 calc R . . C20 C -0.0204(3) 0.4596(3) 0.71829(8) 0.0459(6) Uani 1 1 d . . . H20A H 0.0623 0.4387 0.7371 0.069 Uiso 1 1 calc R . . H20B H -0.0972 0.4653 0.7349 0.069 Uiso 1 1 calc R . . H20C H -0.0091 0.5446 0.7043 0.069 Uiso 1 1 calc R . . N21 N 0.30591(17) 0.02470(17) 0.55540(5) 0.0272(3) Uani 1 1 d . A . N22 N 0.21779(17) -0.07819(17) 0.55178(5) 0.0276(3) Uani 1 1 d . A . H22 H 0.1760 -0.1079 0.5727 0.033 Uiso 1 1 calc R . . C23 C 0.2012(2) -0.1299(2) 0.51263(6) 0.0294(4) Uani 1 1 d D . . C24 C 0.2827(3) -0.0572(3) 0.48987(8) 0.0611(9) Uani 1 1 d . A . H24 H 0.2943 -0.0686 0.4609 0.073 Uiso 1 1 calc R . . C25 C 0.3455(3) 0.0369(3) 0.51737(7) 0.0532(7) Uani 1 1 d . . . H25 H 0.4083 0.1012 0.5099 0.064 Uiso 1 1 calc R A . C26A C 0.1079(10) -0.2471(10) 0.5010(3) 0.033(5) Uani 0.60 1 d PD A 1 C27A C 0.1084(5) -0.2775(6) 0.45386(13) 0.0596(14) Uani 0.60 1 d PD A 1 H27A H 0.0791 -0.1989 0.4372 0.089 Uiso 0.60 1 calc PR A 1 H27B H 0.0462 -0.3510 0.4458 0.089 Uiso 0.60 1 calc PR A 1 H27C H 0.2002 -0.3021 0.4485 0.089 Uiso 0.60 1 calc PR A 1 C28A C -0.0349(4) -0.2113(4) 0.50964(15) 0.0429(9) Uani 0.60 1 d PD A 1 H28A H -0.0369 -0.2007 0.5401 0.064 Uiso 0.60 1 calc PR A 1 H28B H -0.0975 -0.2820 0.4991 0.064 Uiso 0.60 1 calc PR A 1 H28C H -0.0623 -0.1282 0.4952 0.064 Uiso 0.60 1 calc PR A 1 C29A C 0.1571(5) -0.3662(4) 0.52704(17) 0.0540(13) Uani 0.60 1 d PD A 1 H29A H 0.2485 -0.3898 0.5210 0.081 Uiso 0.60 1 calc PR A 1 H29B H 0.0957 -0.4410 0.5199 0.081 Uiso 0.60 1 calc PR A 1 H29C H 0.1591 -0.3453 0.5571 0.081 Uiso 0.60 1 calc PR A 1 C26B C 0.1099(15) -0.2431(14) 0.4989(5) 0.031(6) Uiso 0.40 1 d PD A 2 C27B C 0.0356(9) -0.2092(9) 0.4557(3) 0.070(2) Uiso 0.40 1 d PD A 2 H27D H -0.0019 -0.1196 0.4563 0.105 Uiso 0.40 1 calc PR A 2 H27E H -0.0382 -0.2727 0.4485 0.105 Uiso 0.40 1 calc PR A 2 H27F H 0.0990 -0.2137 0.4344 0.105 Uiso 0.40 1 calc PR A 2 C28B C 0.0066(9) -0.2665(10) 0.5295(3) 0.071(2) Uiso 0.40 1 d PD A 2 H28D H 0.0521 -0.3022 0.5561 0.106 Uiso 0.40 1 calc PR A 2 H28E H -0.0617 -0.3298 0.5171 0.106 Uiso 0.40 1 calc PR A 2 H28F H -0.0375 -0.1825 0.5350 0.106 Uiso 0.40 1 calc PR A 2 C29B C 0.1934(8) -0.3676(7) 0.4949(3) 0.0605(19) Uiso 0.40 1 d PD A 2 H29D H 0.2643 -0.3494 0.4767 0.091 Uiso 0.40 1 calc PR A 2 H29E H 0.1345 -0.4386 0.4824 0.091 Uiso 0.40 1 calc PR A 2 H29F H 0.2353 -0.3949 0.5229 0.091 Uiso 0.40 1 calc PR A 2 Cl30 Cl 0.07484(5) -0.12354(5) 0.654179(15) 0.02842(12) Uani 1 1 d . . . O31 O 0.16179(15) -0.03026(14) 0.68008(5) 0.0339(3) Uani 1 1 d . . . O32 O 0.1607(2) -0.20603(17) 0.63182(6) 0.0506(5) Uani 1 1 d . . . O33 O -0.0141(2) -0.04874(19) 0.62476(6) 0.0603(6) Uani 1 1 d . . . O34 O 0.00189(19) -0.20168(19) 0.68056(6) 0.0507(5) Uani 1 1 d . . . C35 C 0.6011(3) -0.3690(2) 0.58243(7) 0.0377(5) Uani 1 1 d . . . H35 H 0.6161 -0.4641 0.5905 0.045 Uiso 1 1 calc R . . Cl36 Cl 0.56894(9) -0.35919(8) 0.52732(2) 0.0607(2) Uani 1 1 d . . . Cl37 Cl 0.74771(7) -0.27927(8) 0.60083(2) 0.0584(2) Uani 1 1 d . . . Cl38 Cl 0.46143(7) -0.30988(8) 0.60607(2) 0.05480(18) 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 0.02564(14) 0.02263(14) 0.02176(13) -0.00003(8) 0.00218(9) -0.00205(8) Cl2 0.0332(3) 0.0306(3) 0.0316(2) 0.00180(18) 0.00701(19) -0.0078(2) N3 0.0260(8) 0.0250(8) 0.0258(7) 0.0030(6) 0.0018(6) -0.0016(7) N4 0.0225(8) 0.0256(8) 0.0261(7) 0.0032(6) 0.0024(6) -0.0002(6) C5 0.0264(10) 0.0271(10) 0.0264(9) -0.0006(7) 0.0000(7) 0.0035(8) C6 0.0239(10) 0.0389(12) 0.0370(10) 0.0040(9) -0.0008(8) 0.0018(9) C7 0.0264(10) 0.0357(11) 0.0346(10) 0.0067(8) 0.0041(8) -0.0045(9) C8 0.0339(11) 0.0311(11) 0.0330(10) 0.0073(8) 0.0010(8) 0.0066(9) C9 0.0360(12) 0.0480(14) 0.0497(13) 0.0230(11) 0.0075(10) 0.0000(11) C10 0.084(2) 0.0469(16) 0.0315(12) 0.0094(10) -0.0057(13) 0.0036(14) C11 0.0438(14) 0.0370(13) 0.0631(16) 0.0148(12) 0.0078(12) 0.0101(11) N12 0.0296(9) 0.0226(8) 0.0257(7) 0.0013(6) 0.0051(6) -0.0016(7) N13 0.0260(8) 0.0204(8) 0.0257(7) 0.0007(6) 0.0055(6) -0.0012(6) C14 0.0294(10) 0.0213(9) 0.0243(9) -0.0024(7) -0.0001(7) 0.0017(7) C15 0.0400(12) 0.0196(10) 0.0409(11) 0.0023(8) 0.0082(9) 0.0028(8) C16 0.0390(12) 0.0222(10) 0.0373(11) 0.0059(8) 0.0071(9) -0.0027(9) C17 0.0311(11) 0.0255(10) 0.0306(10) -0.0015(7) 0.0051(8) 0.0040(8) C18 0.0330(13) 0.080(2) 0.0475(14) 0.0063(13) 0.0031(11) 0.0126(13) C19 0.0415(13) 0.0331(12) 0.0527(13) 0.0038(10) 0.0220(11) 0.0024(10) C20 0.0603(16) 0.0395(13) 0.0407(12) -0.0109(10) 0.0182(11) -0.0024(12) N21 0.0288(8) 0.0272(9) 0.0255(7) -0.0019(6) 0.0031(6) -0.0059(7) N22 0.0317(9) 0.0283(9) 0.0230(7) -0.0021(6) 0.0033(6) -0.0082(7) C23 0.0289(10) 0.0335(11) 0.0258(9) -0.0070(8) 0.0033(8) -0.0016(8) C24 0.079(2) 0.074(2) 0.0347(12) -0.0237(13) 0.0253(13) -0.0432(17) C25 0.0639(17) 0.0637(17) 0.0362(11) -0.0144(11) 0.0226(12) -0.0354(14) C26A 0.030(5) 0.037(5) 0.032(5) -0.015(2) -0.0015(15) -0.0079(17) C27A 0.061(3) 0.081(4) 0.038(2) -0.033(2) 0.010(2) -0.034(3) C28A 0.0277(19) 0.035(2) 0.067(3) -0.0090(19) 0.0068(18) -0.0069(16) C29A 0.054(3) 0.026(2) 0.074(3) -0.0093(19) -0.026(2) -0.0034(18) Cl30 0.0322(3) 0.0236(2) 0.0299(2) 0.00070(17) 0.00502(19) -0.00325(18) O31 0.0297(7) 0.0252(7) 0.0460(8) -0.0032(6) 0.0008(6) -0.0022(6) O32 0.0658(12) 0.0353(9) 0.0554(10) -0.0105(8) 0.0272(9) 0.0010(9) O33 0.0742(13) 0.0413(10) 0.0564(11) 0.0050(8) -0.0299(10) 0.0024(10) O34 0.0547(11) 0.0499(11) 0.0510(10) 0.0022(8) 0.0204(9) -0.0226(9) C35 0.0414(13) 0.0323(12) 0.0384(11) 0.0002(9) 0.0010(10) -0.0048(9) Cl36 0.0738(5) 0.0711(5) 0.0363(3) -0.0058(3) 0.0027(3) -0.0132(4) Cl37 0.0445(4) 0.0683(5) 0.0613(4) -0.0118(3) 0.0017(3) -0.0172(3) Cl38 0.0459(4) 0.0622(4) 0.0573(4) -0.0156(3) 0.0100(3) -0.0059(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N12 2.0085(17) . ? Zn1 N21 2.0150(16) . ? Zn1 N3 2.0215(16) . ? Zn1 Cl2 2.2392(5) . ? N3 C7 1.333(3) . ? N3 N4 1.356(2) . ? N4 C5 1.349(2) . ? C5 C6 1.377(3) . ? C5 C8 1.511(3) . ? C6 C7 1.389(3) . ? C8 C9 1.527(3) . ? C8 C11 1.530(3) . ? C8 C10 1.536(3) . ? N12 C16 1.340(3) . ? N12 N13 1.353(2) . ? N13 C14 1.348(2) . ? C14 C15 1.378(3) . ? C14 C17 1.515(3) . ? C15 C16 1.384(3) . ? C17 C19 1.525(3) . ? C17 C18 1.526(3) . ? C17 C20 1.533(3) . ? N21 C25 1.323(3) . ? N21 N22 1.355(2) . ? N22 C23 1.344(2) . ? C23 C24 1.364(3) . ? C23 C26B 1.492(15) . ? C23 C26A 1.522(9) . ? C24 C25 1.389(3) . ? C26A C29A 1.509(11) . ? C26A C28A 1.520(10) . ? C26A C27A 1.535(10) . ? C26B C28B 1.514(15) . ? C26B C29B 1.520(15) . ? C26B C27B 1.523(15) . ? Cl30 O34 1.4137(17) . ? Cl30 O33 1.4264(18) . ? Cl30 O32 1.4397(17) . ? Cl30 O31 1.4648(15) . ? C35 Cl36 1.750(2) . ? C35 Cl37 1.756(2) . ? C35 Cl38 1.760(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 N12 Zn1 N21 115.18(7) . . ? N12 Zn1 N3 115.76(7) . . ? N21 Zn1 N3 110.46(7) . . ? N12 Zn1 Cl2 103.62(5) . . ? N21 Zn1 Cl2 105.63(5) . . ? N3 Zn1 Cl2 104.84(5) . . ? C7 N3 N4 105.24(16) . . ? C7 N3 Zn1 123.31(13) . . ? N4 N3 Zn1 130.96(13) . . ? C5 N4 N3 111.85(16) . . ? N4 C5 C6 106.24(18) . . ? N4 C5 C8 123.14(18) . . ? C6 C5 C8 130.62(19) . . ? C5 C6 C7 106.00(18) . . ? N3 C7 C6 110.66(18) . . ? C5 C8 C9 111.10(17) . . ? C5 C8 C11 108.03(18) . . ? C9 C8 C11 110.1(2) . . ? C5 C8 C10 109.15(19) . . ? C9 C8 C10 109.2(2) . . ? C11 C8 C10 109.2(2) . . ? C16 N12 N13 104.98(16) . . ? C16 N12 Zn1 124.22(14) . . ? N13 N12 Zn1 130.67(12) . . ? C14 N13 N12 112.09(16) . . ? N13 C14 C15 106.16(18) . . ? N13 C14 C17 122.85(17) . . ? C15 C14 C17 130.98(18) . . ? C14 C15 C16 106.02(18) . . ? N12 C16 C15 110.74(19) . . ? C14 C17 C19 111.13(17) . . ? C14 C17 C18 108.50(18) . . ? C19 C17 C18 109.9(2) . . ? C14 C17 C20 108.28(18) . . ? C19 C17 C20 109.34(19) . . ? C18 C17 C20 109.6(2) . . ? C25 N21 N22 104.64(17) . . ? C25 N21 Zn1 123.24(15) . . ? N22 N21 Zn1 132.12(13) . . ? C23 N22 N21 112.56(16) . . ? N22 C23 C24 105.62(18) . . ? N22 C23 C26B 124.9(6) . . ? C24 C23 C26B 129.5(6) . . ? N22 C23 C26A 122.1(4) . . ? C24 C23 C26A 132.3(4) . . ? C23 C24 C25 106.5(2) . . ? N21 C25 C24 110.7(2) . . ? C29A C26A C28A 109.8(7) . . ? C29A C26A C23 109.7(6) . . ? C28A C26A C23 109.0(6) . . ? C29A C26A C27A 109.9(7) . . ? C28A C26A C27A 109.6(7) . . ? C23 C26A C27A 108.7(7) . . ? C23 C26B C28B 111.5(10) . . ? C23 C26B C29B 109.8(10) . . ? C28B C26B C29B 110.1(10) . . ? C23 C26B C27B 107.8(10) . . ? C28B C26B C27B 108.9(10) . . ? C29B C26B C27B 108.7(10) . . ? O34 Cl30 O33 111.38(13) . . ? O34 Cl30 O32 110.29(11) . . ? O33 Cl30 O32 109.80(12) . . ? O34 Cl30 O31 109.49(10) . . ? O33 Cl30 O31 107.96(10) . . ? O32 Cl30 O31 107.83(10) . . ? Cl36 C35 Cl37 110.59(13) . . ? Cl36 C35 Cl38 110.51(14) . . ? Cl37 C35 Cl38 110.30(13) . . ? 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 O31 0.88 2.03 2.859(2) 155.8 . N13 H13 O31 0.88 2.07 2.890(2) 155.4 . N13 H13 O33 0.88 2.64 3.314(3) 133.9 . N22 H22 O32 0.88 2.15 2.972(2) 155.6 . _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.494 _refine_diff_density_min -0.615 _refine_diff_density_rms 0.128 #=END data_sr16 _database_code_CSD 191076 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Chloro-tris[5-tertbutylpyrazole]zinc(II) nitrate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H36 Cl N6 Zn, N O3' _chemical_formula_sum 'C21 H36 Cl N7 O3 Zn' _chemical_formula_weight 535.39 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.7119(8) _cell_length_b 10.3815(4) _cell_length_c 14.9451(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.0915(15) _cell_angle_gamma 90.00 _cell_volume 2696.72(18) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 15625 _cell_measurement_theta_min 3.06 _cell_measurement_theta_max 27.49 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.319 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 1.044 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7878 _exptl_absorpt_correction_T_max 0.9694 _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 15625 _diffrn_reflns_av_R_equivalents 0.0630 _diffrn_reflns_av_sigmaI/netI 0.0809 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.49 _reflns_number_total 6115 _reflns_number_gt 4317 _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. Two of the three tertbutyl groups in the complex cation are disordered, each over three orientations: C17A-C20A (occupancy 0.3) C17A, C18B-C20B (occupany 0.4, so that C17A has total occupancy 0.7) C17C-C20C (occupancy 0.3) and C26A-C29A (occupancy 0.33) C26B-C29B (occupancy 0.33) C26C-C29C (occupancy 0.33). All disordered C-C bond lengths were restrained to 1.52(2)\%A, and 1,3-C...C distances within a given disorder orientation to 2.48(2)\%A. The nitrate ion N30-O33 is disordered over four equally occupied orientations, labelled 'A', 'B', 'C' and 'D'. All N-O distances were restrained to 1.24(1)\%A, and O...O distances within a given disorder orientation to 2.15(1)\%A. All non-H atoms with occupancy >0.5 were refined anisotropically. All H atoms were placed in calculated positions and refined using a riding model. The highest residual Fourier peak of 1.05\%A lies near the disordered tertbutyl group C17A-C20C, but is not bonded to any other feature. ; _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^)+(0.0400P)^2^+10.3966P] 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 SHELXL _refine_ls_extinction_coef 0.0034(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6115 _refine_ls_number_parameters 357 _refine_ls_number_restraints 84 _refine_ls_R_factor_all 0.1099 _refine_ls_R_factor_gt 0.0761 _refine_ls_wR_factor_ref 0.1838 _refine_ls_wR_factor_gt 0.1682 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.096 _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 0.21122(3) 0.54976(5) 0.45935(4) 0.0314(2) Uani 1 1 d . . . Cl2 Cl 0.15130(8) 0.40751(13) 0.53470(9) 0.0441(3) Uani 1 1 d . . . N3 N 0.1325(2) 0.6925(4) 0.4289(3) 0.0324(9) Uani 1 1 d . . . N4 N 0.1276(2) 0.7871(4) 0.3651(3) 0.0309(9) Uani 1 1 d . . . H4 H 0.1646 0.8058 0.3355 0.037 Uiso 1 1 calc R . . C5 C 0.0593(3) 0.8486(4) 0.3525(3) 0.0310(10) Uani 1 1 d . . . C6 C 0.0175(3) 0.7911(5) 0.4107(3) 0.0370(11) Uani 1 1 d . . . H6 H -0.0329 0.8130 0.4185 0.044 Uiso 1 1 calc R . . C7 C 0.0648(3) 0.6939(5) 0.4557(3) 0.0378(12) Uani 1 1 d . . . H7 H 0.0507 0.6367 0.4993 0.045 Uiso 1 1 calc R . . C8 C 0.0385(3) 0.9545(5) 0.2826(3) 0.0353(11) Uani 1 1 d . . . C9 C 0.1000(4) 1.0592(6) 0.2941(5) 0.0604(18) Uani 1 1 d . . . H9A H 0.1060 1.0965 0.3553 0.091 Uiso 1 1 calc R . . H9B H 0.0845 1.1267 0.2484 0.091 Uiso 1 1 calc R . . H9C H 0.1490 1.0218 0.2859 0.091 Uiso 1 1 calc R . . C10 C 0.0284(5) 0.8956(6) 0.1877(4) 0.0641(19) Uani 1 1 d . . . H10A H 0.0770 0.8564 0.1796 0.096 Uiso 1 1 calc R . . H10B H 0.0136 0.9629 0.1417 0.096 Uiso 1 1 calc R . . H10C H -0.0118 0.8295 0.1807 0.096 Uiso 1 1 calc R . . C11 C -0.0377(4) 1.0161(6) 0.2949(4) 0.0516(15) Uani 1 1 d . . . H11A H -0.0777 0.9498 0.2889 0.077 Uiso 1 1 calc R . . H11B H -0.0529 1.0823 0.2482 0.077 Uiso 1 1 calc R . . H11C H -0.0311 1.0555 0.3555 0.077 Uiso 1 1 calc R . . N12 N 0.2283(2) 0.4608(4) 0.3459(3) 0.0326(9) Uani 1 1 d . B . N13 N 0.2465(2) 0.5163(4) 0.2706(3) 0.0313(9) Uani 1 1 d . B . H13 H 0.2579 0.5984 0.2671 0.038 Uiso 1 1 calc R . . C14 C 0.2451(3) 0.4324(4) 0.2021(3) 0.0319(10) Uani 1 1 d D . . C15 C 0.2245(3) 0.3147(5) 0.2342(3) 0.0344(11) Uani 1 1 d . B . H15 H 0.2179 0.2352 0.2022 0.041 Uiso 1 1 calc R . . C16 C 0.2154(3) 0.3375(4) 0.3231(3) 0.0330(11) Uani 1 1 d . . . H16 H 0.2017 0.2735 0.3625 0.040 Uiso 1 1 calc R B . C17A C 0.2654(7) 0.4681(10) 0.1116(6) 0.041(3) Uani 0.70 1 d PD A . C18A C 0.3277(11) 0.378(2) 0.0906(15) 0.049(7) Uiso 0.30 1 d PD A 1 H18A H 0.3768 0.3984 0.1308 0.073 Uiso 0.30 1 calc PR A 1 H18B H 0.3328 0.3893 0.0269 0.073 Uiso 0.30 1 calc PR A 1 H18C H 0.3136 0.2886 0.1004 0.073 Uiso 0.30 1 calc PR A 1 C19A C 0.2938(13) 0.6069(13) 0.1131(12) 0.024(4) Uiso 0.30 1 d PD A 1 H19A H 0.2551 0.6644 0.1303 0.036 Uiso 0.30 1 calc PR A 1 H19B H 0.3026 0.6305 0.0524 0.036 Uiso 0.30 1 calc PR A 1 H19C H 0.3421 0.6150 0.1575 0.036 Uiso 0.30 1 calc PR A 1 C20A C 0.1926(10) 0.456(2) 0.0382(10) 0.034(6) Uiso 0.30 1 d PD A 1 H20A H 0.1886 0.3681 0.0139 0.051 Uiso 0.30 1 calc PR A 1 H20B H 0.1952 0.5171 -0.0111 0.051 Uiso 0.30 1 calc PR A 1 H20C H 0.1475 0.4752 0.0648 0.051 Uiso 0.30 1 calc PR A 1 C18B C 0.3009(10) 0.3525(15) 0.0711(11) 0.055(5) Uiso 0.40 1 d PD A 2 H18D H 0.3460 0.3223 0.1145 0.082 Uiso 0.40 1 calc PR A 2 H18E H 0.3164 0.3784 0.0142 0.082 Uiso 0.40 1 calc PR A 2 H18F H 0.2629 0.2830 0.0586 0.082 Uiso 0.40 1 calc PR A 2 C19B C 0.3231(11) 0.5793(16) 0.1239(14) 0.084(7) Uiso 0.40 1 d PD A 2 H19D H 0.3004 0.6544 0.1485 0.127 Uiso 0.40 1 calc PR A 2 H19E H 0.3359 0.6014 0.0649 0.127 Uiso 0.40 1 calc PR A 2 H19F H 0.3699 0.5534 0.1664 0.127 Uiso 0.40 1 calc PR A 2 C20B C 0.1933(11) 0.511(2) 0.0461(14) 0.124(12) Uiso 0.40 1 d PD A 2 H20D H 0.1570 0.4389 0.0343 0.186 Uiso 0.40 1 calc PR A 2 H20E H 0.2070 0.5391 -0.0113 0.186 Uiso 0.40 1 calc PR A 2 H20F H 0.1694 0.5826 0.0731 0.186 Uiso 0.40 1 calc PR A 2 C17C C 0.2511(12) 0.4763(19) 0.1073(12) 0.031(7) Uiso 0.30 1 d PD B 3 C18C C 0.3126(13) 0.393(2) 0.0756(15) 0.046(7) Uiso 0.30 1 d PD B 3 H18G H 0.3634 0.4157 0.1110 0.069 Uiso 0.30 1 calc PR B 3 H18H H 0.3116 0.4090 0.0107 0.069 Uiso 0.30 1 calc PR B 3 H18I H 0.3020 0.3021 0.0849 0.069 Uiso 0.30 1 calc PR B 3 C19C C 0.2735(12) 0.6187(15) 0.1064(13) 0.043(7) Uiso 0.30 1 d PD B 3 H19G H 0.2321 0.6716 0.1222 0.065 Uiso 0.30 1 calc PR B 3 H19H H 0.2816 0.6423 0.0455 0.065 Uiso 0.30 1 calc PR B 3 H19I H 0.3210 0.6333 0.1510 0.065 Uiso 0.30 1 calc PR B 3 C20C C 0.1752(10) 0.4629(18) 0.0402(9) 0.023(4) Uiso 0.30 1 d PD B 3 H20G H 0.1559 0.3747 0.0424 0.034 Uiso 0.30 1 calc PR B 3 H20H H 0.1832 0.4818 -0.0216 0.034 Uiso 0.30 1 calc PR B 3 H20I H 0.1377 0.5235 0.0565 0.034 Uiso 0.30 1 calc PR B 3 N21 N 0.3130(2) 0.5857(4) 0.5422(3) 0.0350(9) Uani 1 1 d . C . N22 N 0.3763(2) 0.6479(4) 0.5255(3) 0.0368(10) Uani 1 1 d . C . H22 H 0.3793 0.6839 0.4731 0.044 Uiso 1 1 calc R . . C23 C 0.4338(3) 0.6478(5) 0.5988(4) 0.0458(14) Uani 1 1 d D . . C24 C 0.4063(4) 0.5828(6) 0.6661(4) 0.0540(16) Uani 1 1 d . C . H24 H 0.4332 0.5662 0.7264 0.065 Uiso 1 1 calc R . . C25 C 0.3316(4) 0.5464(6) 0.6284(4) 0.0462(13) Uani 1 1 d . . . H25 H 0.2984 0.4999 0.6597 0.055 Uiso 1 1 calc R C . C26A C 0.5131(9) 0.6932(18) 0.6001(13) 0.056(8) Uiso 0.33 1 d PD C 1 C27A C 0.5277(13) 0.705(3) 0.5014(12) 0.088(9) Uiso 0.33 1 d PD C 1 H27A H 0.5060 0.6305 0.4656 0.132 Uiso 0.33 1 calc PR C 1 H27B H 0.5832 0.7097 0.5027 0.132 Uiso 0.33 1 calc PR C 1 H27C H 0.5031 0.7841 0.4734 0.132 Uiso 0.33 1 calc PR C 1 C28A C 0.5232(13) 0.8245(18) 0.6450(18) 0.097(9) Uiso 0.33 1 d PD C 1 H28A H 0.4765 0.8473 0.6674 0.145 Uiso 0.33 1 calc PR C 1 H28B H 0.5326 0.8889 0.6004 0.145 Uiso 0.33 1 calc PR C 1 H28C H 0.5671 0.8223 0.6962 0.145 Uiso 0.33 1 calc PR C 1 C29A C 0.5709(9) 0.5951(19) 0.6492(15) 0.073(6) Uiso 0.33 1 d PD C 1 H29A H 0.5654 0.5883 0.7130 0.109 Uiso 0.33 1 calc PR C 1 H29B H 0.6232 0.6232 0.6465 0.109 Uiso 0.33 1 calc PR C 1 H29C H 0.5611 0.5109 0.6196 0.109 Uiso 0.33 1 calc PR C 1 C26B C 0.5092(10) 0.7213(18) 0.5966(14) 0.06(3) Uiso 0.33 1 d PD C 2 C27B C 0.5446(10) 0.6695(18) 0.5188(12) 0.048(5) Uiso 0.33 1 d PD C 2 H27D H 0.5036 0.6449 0.4678 0.072 Uiso 0.33 1 calc PR C 2 H27E H 0.5763 0.5940 0.5398 0.072 Uiso 0.33 1 calc PR C 2 H27F H 0.5767 0.7363 0.4986 0.072 Uiso 0.33 1 calc PR C 2 C28B C 0.4958(10) 0.8645(13) 0.5895(14) 0.054(5) Uiso 0.33 1 d PD C 2 H28D H 0.4524 0.8827 0.5398 0.081 Uiso 0.33 1 calc PR C 2 H28E H 0.5421 0.9072 0.5771 0.081 Uiso 0.33 1 calc PR C 2 H28F H 0.4843 0.8968 0.6471 0.081 Uiso 0.33 1 calc PR C 2 C29B C 0.5648(10) 0.692(2) 0.6873(12) 0.077(6) Uiso 0.33 1 d PD C 2 H29D H 0.6160 0.7261 0.6848 0.115 Uiso 0.33 1 calc PR C 2 H29E H 0.5680 0.5988 0.6971 0.115 Uiso 0.33 1 calc PR C 2 H29F H 0.5456 0.7331 0.7377 0.115 Uiso 0.33 1 calc PR C 2 C26C C 0.5085(10) 0.7239(19) 0.6024(14) 0.06(2) Uiso 0.33 1 d PD C 3 C27C C 0.5692(11) 0.632(2) 0.5785(18) 0.096(8) Uiso 0.33 1 d PD C 3 H27G H 0.5560 0.6095 0.5136 0.144 Uiso 0.33 1 calc PR C 3 H27H H 0.5707 0.5533 0.6153 0.144 Uiso 0.33 1 calc PR C 3 H27I H 0.6197 0.6737 0.5913 0.144 Uiso 0.33 1 calc PR C 3 C28C C 0.4977(14) 0.834(2) 0.5349(16) 0.097(8) Uiso 0.33 1 d PD C 3 H28G H 0.5022 0.8020 0.4745 0.145 Uiso 0.33 1 calc PR C 3 H28H H 0.5373 0.8997 0.5546 0.145 Uiso 0.33 1 calc PR C 3 H28I H 0.4467 0.8725 0.5319 0.145 Uiso 0.33 1 calc PR C 3 C29C C 0.5355(11) 0.776(2) 0.6986(11) 0.067(6) Uiso 0.33 1 d PD C 3 H29G H 0.5834 0.8243 0.7014 0.100 Uiso 0.33 1 calc PR C 3 H29H H 0.5443 0.7042 0.7419 0.100 Uiso 0.33 1 calc PR C 3 H29I H 0.4960 0.8333 0.7144 0.100 Uiso 0.33 1 calc PR C 3 N30A N 0.3099(11) 0.8472(19) 0.3344(18) 0.023(6) Uiso 0.25 1 d PD D 1 O31A O 0.3107(9) 0.7343(12) 0.3601(10) 0.033(3) Uiso 0.25 1 d PD D 1 O32A O 0.3622(12) 0.9217(17) 0.3699(13) 0.058(5) Uiso 0.25 1 d PD D 1 O33A O 0.2505(10) 0.8852(19) 0.2818(13) 0.068(5) Uiso 0.25 1 d PD D 1 N30B N 0.3161(14) 0.826(3) 0.338(3) 0.07(2) Uiso 0.25 1 d PD E 2 O31B O 0.2753(14) 0.738(2) 0.358(2) 0.093(10) Uiso 0.25 1 d PD E 2 O32B O 0.3870(10) 0.816(2) 0.3690(16) 0.058(5) Uiso 0.25 1 d PD E 2 O33B O 0.2847(17) 0.936(3) 0.329(3) 0.112(13) Uiso 0.25 1 d PD E 2 N30C N 0.3196(10) 0.8648(18) 0.3578(15) 0.033(6) Uiso 0.25 1 d PD F 3 O31C O 0.2781(8) 0.7737(13) 0.3329(11) 0.024(3) Uiso 0.25 1 d PD F 3 O32C O 0.3866(10) 0.858(2) 0.3989(17) 0.081(8) Uiso 0.25 1 d PD F 3 O33C O 0.2960(14) 0.9765(17) 0.3364(17) 0.065(7) Uiso 0.25 1 d PD F 3 N30D N 0.3085(13) 0.818(2) 0.340(2) 0.040(14) Uiso 0.25 1 d PD G 4 O31D O 0.2509(7) 0.7886(14) 0.2824(10) 0.038(3) Uiso 0.25 1 d PD G 4 O32D O 0.3649(11) 0.7426(19) 0.3475(14) 0.072(5) Uiso 0.25 1 d PD G 4 O33D O 0.3234(12) 0.9405(16) 0.3528(13) 0.045(4) Uiso 0.25 1 d PD G 4 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 0.0383(3) 0.0284(3) 0.0270(3) 0.0005(2) 0.0051(2) 0.0006(2) Cl2 0.0535(8) 0.0376(7) 0.0434(7) 0.0111(6) 0.0146(6) -0.0009(6) N3 0.039(2) 0.028(2) 0.030(2) 0.0035(17) 0.0049(17) -0.0013(17) N4 0.031(2) 0.030(2) 0.032(2) 0.0034(17) 0.0052(16) -0.0039(17) C5 0.033(2) 0.027(2) 0.031(2) -0.001(2) 0.0012(19) -0.001(2) C6 0.042(3) 0.035(3) 0.035(3) 0.004(2) 0.012(2) 0.003(2) C7 0.046(3) 0.038(3) 0.032(3) 0.004(2) 0.014(2) 0.002(2) C8 0.043(3) 0.027(2) 0.035(3) 0.005(2) 0.005(2) -0.002(2) C9 0.049(3) 0.047(3) 0.079(5) 0.033(3) -0.003(3) -0.012(3) C10 0.110(6) 0.049(4) 0.031(3) 0.010(3) 0.008(3) 0.016(4) C11 0.051(3) 0.044(3) 0.059(4) 0.014(3) 0.010(3) 0.011(3) N12 0.036(2) 0.028(2) 0.033(2) 0.0026(18) 0.0060(17) -0.0031(17) N13 0.036(2) 0.026(2) 0.033(2) 0.0007(17) 0.0093(17) -0.0035(16) C14 0.035(2) 0.030(2) 0.031(2) -0.001(2) 0.0055(19) -0.002(2) C15 0.044(3) 0.028(2) 0.032(2) -0.003(2) 0.011(2) -0.007(2) C16 0.045(3) 0.024(2) 0.032(2) 0.005(2) 0.011(2) -0.005(2) C17A 0.049(6) 0.045(6) 0.032(5) 0.003(3) 0.018(4) -0.002(4) N21 0.043(2) 0.031(2) 0.030(2) -0.0007(18) 0.0045(18) 0.0019(18) N22 0.038(2) 0.035(2) 0.037(2) -0.0044(19) 0.0057(18) 0.0051(19) C23 0.038(3) 0.051(3) 0.046(3) -0.012(3) 0.000(2) 0.011(3) C24 0.058(4) 0.060(4) 0.039(3) -0.004(3) -0.005(3) 0.009(3) C25 0.056(3) 0.048(3) 0.032(3) 0.001(3) 0.004(2) -0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N12 2.004(4) . ? Zn1 N21 2.015(4) . ? Zn1 N3 2.026(4) . ? Zn1 Cl2 2.2440(14) . ? N3 C7 1.334(7) . ? N3 N4 1.361(5) . ? N4 C5 1.349(6) . ? C5 C6 1.382(7) . ? C5 C8 1.513(7) . ? C6 C7 1.399(7) . ? C8 C10 1.524(8) . ? C8 C9 1.524(7) . ? C8 C11 1.536(8) . ? N12 C16 1.333(6) . ? N12 N13 1.357(5) . ? N13 C14 1.340(6) . ? C14 C15 1.387(6) . ? C14 C17A 1.511(9) . ? C14 C17C 1.513(17) . ? C15 C16 1.389(7) . ? C17A C20B 1.518(14) . ? C17A C18A 1.525(14) . ? C17A C19A 1.525(12) . ? C17A C20A 1.528(14) . ? C17A C19B 1.529(14) . ? C17A C18B 1.532(13) . ? C17C C20C 1.521(17) . ? C17C C19C 1.531(17) . ? C17C C18C 1.532(17) . ? N21 C25 1.332(7) . ? N21 N22 1.358(6) . ? N22 C23 1.345(7) . ? C23 C24 1.374(9) . ? C23 C26A 1.478(15) . ? C23 C26C 1.533(16) . ? C23 C26B 1.545(16) . ? C24 C25 1.388(9) . ? C26A C28A 1.515(17) . ? C26A C29A 1.528(17) . ? C26A C27A 1.551(17) . ? C26B C28B 1.506(17) . ? C26B C27B 1.521(17) . ? C26B C29B 1.545(17) . ? C26C C28C 1.514(17) . ? C26C C29C 1.526(17) . ? C26C C27C 1.531(17) . ? N30A O31A 1.233(16) . ? N30A O32A 1.245(16) . ? N30A O33A 1.250(16) . ? N30B O31B 1.23(2) . ? N30B O32B 1.256(18) . ? N30B O33B 1.268(19) . ? N30C O31C 1.212(16) . ? N30C O32C 1.229(16) . ? N30C O33C 1.253(16) . ? N30D O31D 1.240(18) . ? N30D O32D 1.255(18) . ? N30D O33D 1.309(18) . ? 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 N21 110.01(17) . . ? N12 Zn1 N3 110.91(16) . . ? N21 Zn1 N3 119.88(16) . . ? N12 Zn1 Cl2 106.51(12) . . ? N21 Zn1 Cl2 105.49(13) . . ? N3 Zn1 Cl2 102.84(12) . . ? C7 N3 N4 105.3(4) . . ? C7 N3 Zn1 124.1(3) . . ? N4 N3 Zn1 129.3(3) . . ? C5 N4 N3 111.9(4) . . ? N4 C5 C6 106.4(4) . . ? N4 C5 C8 122.2(4) . . ? C6 C5 C8 131.3(5) . . ? C5 C6 C7 105.7(5) . . ? N3 C7 C6 110.7(4) . . ? C5 C8 C10 108.7(4) . . ? C5 C8 C9 111.5(4) . . ? C10 C8 C9 110.1(5) . . ? C5 C8 C11 108.8(4) . . ? C10 C8 C11 109.3(5) . . ? C9 C8 C11 108.3(5) . . ? C16 N12 N13 104.6(4) . . ? C16 N12 Zn1 127.8(3) . . ? N13 N12 Zn1 127.2(3) . . ? C14 N13 N12 112.6(4) . . ? N13 C14 C15 106.0(4) . . ? N13 C14 C17A 123.5(5) . . ? C15 C14 C17A 130.5(5) . . ? N13 C14 C17C 121.7(8) . . ? C15 C14 C17C 131.3(9) . . ? C14 C15 C16 105.5(4) . . ? N12 C16 C15 111.3(4) . . ? C14 C17A C20B 109.5(11) . . ? C14 C17A C18A 109.9(10) . . ? C14 C17A C19A 110.7(8) . . ? C18A C17A C19A 109.4(11) . . ? C14 C17A C20A 108.1(9) . . ? C18A C17A C20A 110.2(11) . . ? C19A C17A C20A 108.6(11) . . ? C14 C17A C19B 110.2(9) . . ? C20B C17A C19B 108.4(11) . . ? C14 C17A C18B 110.4(9) . . ? C20B C17A C18B 109.4(11) . . ? C19B C17A C18B 108.9(11) . . ? C14 C17C C20C 112.2(13) . . ? C14 C17C C19C 111.3(13) . . ? C20C C17C C19C 106.2(13) . . ? C14 C17C C18C 107.6(13) . . ? C20C C17C C18C 109.6(14) . . ? C19C C17C C18C 109.9(14) . . ? C25 N21 N22 105.3(4) . . ? C25 N21 Zn1 124.3(4) . . ? N22 N21 Zn1 130.4(3) . . ? C23 N22 N21 111.9(4) . . ? N22 C23 C24 106.1(5) . . ? N22 C23 C26A 125.4(9) . . ? C24 C23 C26A 128.1(9) . . ? N22 C23 C26C 122.7(9) . . ? C24 C23 C26C 130.7(9) . . ? N22 C23 C26B 120.3(9) . . ? C24 C23 C26B 133.5(9) . . ? C23 C24 C25 106.4(5) . . ? N21 C25 C24 110.3(5) . . ? C23 C26A C28A 108.9(13) . . ? C23 C26A C29A 109.9(13) . . ? C28A C26A C29A 112.1(14) . . ? C23 C26A C27A 110.2(13) . . ? C28A C26A C27A 108.7(14) . . ? C29A C26A C27A 107.1(13) . . ? C28B C26B C27B 112.2(14) . . ? C28B C26B C23 111.4(13) . . ? C27B C26B C23 109.1(12) . . ? C28B C26B C29B 108.7(14) . . ? C27B C26B C29B 108.4(13) . . ? C23 C26B C29B 106.9(13) . . ? C28C C26C C29C 109.6(14) . . ? C28C C26C C27C 108.7(14) . . ? C29C C26C C27C 109.6(14) . . ? C28C C26C C23 111.7(14) . . ? C29C C26C C23 109.1(13) . . ? C27C C26C C23 108.0(13) . . ? O31A N30A O32A 119.7(16) . . ? O31A N30A O33A 117.0(16) . . ? O32A N30A O33A 122.6(17) . . ? O31B N30B O32B 116(2) . . ? O31B N30B O33B 115(2) . . ? O32B N30B O33B 120(2) . . ? O31C N30C O32C 125.5(17) . . ? O31C N30C O33C 119.5(16) . . ? O32C N30C O33C 114.8(17) . . ? O31D N30D O32D 116.4(19) . . ? O31D N30D O33D 117.0(19) . . ? O32D N30D O33D 117(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 O31A 0.88 2.65 3.303(17) 132.1 . N4 H4 O33A 0.88 2.03 2.89(2) 167.8 . N4 H4 O31B 0.88 2.05 2.69(3) 128.5 . N4 H4 O33B 0.88 2.54 3.31(3) 147.9 . N4 H4 O31C 0.88 2.04 2.801(15) 143.4 . N4 H4 O31D 0.88 1.86 2.708(15) 160.9 . N13 H13 O31A 0.88 2.07 2.760(14) 134.3 . N13 H13 O31B 0.88 1.97 2.65(3) 132.8 . N13 H13 O31C 0.88 2.07 2.850(14) 147.7 . N13 H13 O31D 0.88 1.99 2.833(15) 158.8 . N13 H13 O32D 0.88 2.53 3.21(2) 134.8 . N22 H22 O31A 0.88 1.95 2.677(15) 138.6 . N22 H22 O31B 0.88 2.33 2.94(3) 125.7 . N22 H22 O32B 0.88 2.09 2.95(2) 164.4 . N22 H22 O31C 0.88 2.65 3.330(16) 134.9 . N22 H22 O32C 0.88 2.14 2.92(3) 147.3 . N22 H22 O32D 0.88 1.94 2.81(2) 167.2 . _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.054 _refine_diff_density_min -0.557 _refine_diff_density_rms 0.097 #=END data_sr19a _database_code_CSD 191077 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Chloro-tris[5-tertbutylpyrazole]zinc(II) trifluoromethanesulfonate hemitoluene solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H36 Cl N6 Zn, C F3 S O3, 0.5[C7 H8]' _chemical_formula_sum 'C25.50 H40 Cl F3 N6 O3 S Zn' _chemical_formula_weight 668.52 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.2895(1) _cell_length_b 10.8281(1) _cell_length_c 29.3462(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.4541(5) _cell_angle_gamma 90.00 _cell_volume 3254.83(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 33103 _cell_measurement_theta_min 1.99 _cell_measurement_theta_max 27.49 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.364 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1396 _exptl_absorpt_coefficient_mu 0.953 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8624 _exptl_absorpt_correction_T_max 0.9363 _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 33103 _diffrn_reflns_av_R_equivalents 0.0485 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 27.49 _reflns_number_total 7452 _reflns_number_gt 6376 _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 one complex cation and one anion lying on general positions, and half a molecule of toluene lying across the crystallographic inversion centre at 0.5, 0.5, 0.5. The tertbutyl C groups C8-C11 and C26-C29 are each disordered over two equally occupied orientations, labelled 'A' and 'B'. Both these groups were refined using the restraints C-C = 1.53(2)\%A and 1,3-C...C = 2.50(2)\%A. The triflate anion is disordered over two orientations: S30A-F37A (occupancy 0.50) S30B-F37B (occupancy 0.50) The following restraints were applied to each disorder orientation of this anion: S-O = 1.42(1)\%A O...O = 2.32(1)\%A S-C = 1.78(1)\%A C-F = 1.31(1)\%A F...F = 2.14(1)\%A S...F = 2.58(1)\%A. The toluene half-molecule was modelled using the following restraints: intra-ring C-C = 1.38(2)\%A, and intra-ring-1,3-C...C = 2.41(2)\%A. All wholly occupied non-H atoms, plus the two partial triflate anions, were refined anisotropically, while all H atoms were placed in calculated positions and refined using a riding model. No thermal parameter restraints were applied. The disk-like thermal ellipsoid for C34B probably reflects its closeness to C34A (they are 0.2\%A apart). ; _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^)+(0.0479P)^2^+2.4737P] 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 7452 _refine_ls_number_parameters 428 _refine_ls_number_restraints 93 _refine_ls_R_factor_all 0.0483 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.1045 _refine_ls_wR_factor_gt 0.0980 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.043 _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 0.41710(2) 0.63870(2) 0.713570(8) 0.02622(8) Uani 1 1 d . . . Cl2 Cl 0.54481(5) 0.55304(5) 0.771040(18) 0.03440(13) Uani 1 1 d . . . N3 N 0.53475(16) 0.72696(17) 0.67370(6) 0.0314(4) Uani 1 1 d . A . N4 N 0.51951(17) 0.82930(17) 0.64718(6) 0.0324(4) Uani 1 1 d . A . H4 H 0.4484 0.8749 0.6446 0.039 Uiso 1 1 calc R . . C5 C 0.6253(2) 0.8530(2) 0.62529(7) 0.0324(5) Uani 1 1 d D . . C6 C 0.7145(2) 0.7615(2) 0.63819(9) 0.0416(5) Uani 1 1 d . A . H6 H 0.7994 0.7521 0.6285 0.050 Uiso 1 1 calc R . . C7 C 0.6551(2) 0.6861(2) 0.66819(8) 0.0377(5) Uani 1 1 d . . . H7 H 0.6943 0.6153 0.6828 0.045 Uiso 1 1 calc R A . C8A C 0.6439(7) 0.9520(6) 0.5932(2) 0.0342(19) Uiso 0.50 1 d PD A 1 C9A C 0.5199(6) 1.0356(6) 0.5880(2) 0.0500(18) Uiso 0.50 1 d PD A 1 H9A1 H 0.4439 0.9858 0.5768 0.075 Uiso 0.50 1 calc PR A 1 H9A2 H 0.5323 1.1019 0.5661 0.075 Uiso 0.50 1 calc PR A 1 H9A3 H 0.5055 1.0715 0.6177 0.075 Uiso 0.50 1 calc PR A 1 C10A C 0.7586(6) 1.0380(6) 0.6122(3) 0.0443(17) Uiso 0.50 1 d PD A 1 H10A H 0.7424 1.0678 0.6427 0.066 Uiso 0.50 1 calc PR A 1 H10B H 0.7647 1.1085 0.5916 0.066 Uiso 0.50 1 calc PR A 1 H10C H 0.8407 0.9915 0.6143 0.066 Uiso 0.50 1 calc PR A 1 C11A C 0.6644(7) 0.9014(6) 0.5465(2) 0.0512(14) Uiso 0.50 1 d PD A 1 H11A H 0.7434 0.8503 0.5487 0.077 Uiso 0.50 1 calc PR A 1 H11B H 0.6743 0.9699 0.5253 0.077 Uiso 0.50 1 calc PR A 1 H11C H 0.5890 0.8510 0.5352 0.077 Uiso 0.50 1 calc PR A 1 C8B C 0.6242(7) 0.9689(6) 0.5923(2) 0.037(2) Uiso 0.50 1 d PD A 2 C9B C 0.5183(6) 1.0589(6) 0.5986(2) 0.0426(15) Uiso 0.50 1 d PD A 2 H9B1 H 0.5217 1.0826 0.6310 0.064 Uiso 0.50 1 calc PR A 2 H9B2 H 0.4336 1.0209 0.5892 0.064 Uiso 0.50 1 calc PR A 2 H9B3 H 0.5298 1.1323 0.5800 0.064 Uiso 0.50 1 calc PR A 2 C10B C 0.7606(7) 1.0269(8) 0.6008(3) 0.058(2) Uiso 0.50 1 d PD A 2 H10D H 0.7696 1.0930 0.5786 0.088 Uiso 0.50 1 calc PR A 2 H10E H 0.8270 0.9635 0.5975 0.088 Uiso 0.50 1 calc PR A 2 H10F H 0.7721 1.0610 0.6319 0.088 Uiso 0.50 1 calc PR A 2 C11B C 0.6126(7) 0.9162(6) 0.5433(2) 0.0587(17) Uiso 0.50 1 d PD A 2 H11D H 0.5274 0.8762 0.5368 0.088 Uiso 0.50 1 calc PR A 2 H11E H 0.6821 0.8555 0.5406 0.088 Uiso 0.50 1 calc PR A 2 H11F H 0.6210 0.9834 0.5214 0.088 Uiso 0.50 1 calc PR A 2 N12 N 0.29723(16) 0.75177(15) 0.74465(6) 0.0271(3) Uani 1 1 d . . . N13 N 0.19972(17) 0.82856(16) 0.72796(6) 0.0302(4) Uani 1 1 d . . . H13 H 0.1757 0.8382 0.6986 0.036 Uiso 1 1 calc R . . C14 C 0.14419(19) 0.88802(18) 0.76118(7) 0.0263(4) Uani 1 1 d . . . C15 C 0.2088(2) 0.8480(2) 0.80159(8) 0.0375(5) Uani 1 1 d . . . H15 H 0.1929 0.8728 0.8316 0.045 Uiso 1 1 calc R . . C16 C 0.3021(2) 0.7639(2) 0.78967(7) 0.0363(5) Uani 1 1 d . . . H16 H 0.3612 0.7210 0.8109 0.044 Uiso 1 1 calc R . . C17 C 0.03287(19) 0.97795(19) 0.75072(7) 0.0296(4) Uani 1 1 d . . . C18 C -0.0021(2) 1.0368(2) 0.79523(9) 0.0412(5) Uani 1 1 d . . . H18A H -0.0248 0.9720 0.8164 0.062 Uiso 1 1 calc R . . H18B H -0.0768 1.0923 0.7887 0.062 Uiso 1 1 calc R . . H18C H 0.0727 1.0839 0.8091 0.062 Uiso 1 1 calc R . . C19 C 0.0740(2) 1.0778(2) 0.71788(9) 0.0416(5) Uani 1 1 d . . . H19A H 0.1515 1.1209 0.7319 0.062 Uiso 1 1 calc R . . H19B H 0.0026 1.1371 0.7116 0.062 Uiso 1 1 calc R . . H19C H 0.0942 1.0393 0.6892 0.062 Uiso 1 1 calc R . . C20 C -0.0863(2) 0.9087(2) 0.72821(10) 0.0441(6) Uani 1 1 d . . . H20A H -0.0635 0.8686 0.7001 0.066 Uiso 1 1 calc R . . H20B H -0.1579 0.9671 0.7208 0.066 Uiso 1 1 calc R . . H20C H -0.1138 0.8459 0.7494 0.066 Uiso 1 1 calc R . . N21 N 0.33922(16) 0.49147(16) 0.67910(6) 0.0279(4) Uani 1 1 d . B . N22 N 0.26713(16) 0.48629(16) 0.63799(6) 0.0280(4) Uani 1 1 d . B . H22 H 0.2446 0.5514 0.6211 0.034 Uiso 1 1 calc R . . C23 C 0.2343(2) 0.36986(19) 0.62614(7) 0.0303(4) Uani 1 1 d D . . C24 C 0.2886(2) 0.2951(2) 0.66115(8) 0.0341(5) Uani 1 1 d . B . H24 H 0.2835 0.2076 0.6629 0.041 Uiso 1 1 calc R . . C25 C 0.3518(2) 0.37394(19) 0.69301(8) 0.0324(4) Uani 1 1 d . . . H25 H 0.3979 0.3482 0.7210 0.039 Uiso 1 1 calc R B . C26A C 0.1586(8) 0.3335(8) 0.5813(3) 0.031(3) Uiso 0.50 1 d PD B 1 C27A C 0.1200(6) 0.4474(5) 0.5523(2) 0.0506(14) Uiso 0.50 1 d PD B 1 H27A H 0.0748 0.5065 0.5706 0.076 Uiso 0.50 1 calc PR B 1 H27B H 0.0619 0.4226 0.5255 0.076 Uiso 0.50 1 calc PR B 1 H27C H 0.1986 0.4860 0.5423 0.076 Uiso 0.50 1 calc PR B 1 C28A C 0.2343(6) 0.2431(6) 0.5553(2) 0.0454(14) Uiso 0.50 1 d PD B 1 H28A H 0.3174 0.2805 0.5488 0.068 Uiso 0.50 1 calc PR B 1 H28B H 0.1835 0.2219 0.5264 0.068 Uiso 0.50 1 calc PR B 1 H28C H 0.2513 0.1682 0.5736 0.068 Uiso 0.50 1 calc PR B 1 C29A C 0.0278(6) 0.2737(7) 0.5942(2) 0.0510(18) Uiso 0.50 1 d PD B 1 H29A H 0.0477 0.2029 0.6144 0.077 Uiso 0.50 1 calc PR B 1 H29B H -0.0237 0.2461 0.5662 0.077 Uiso 0.50 1 calc PR B 1 H29C H -0.0222 0.3349 0.6098 0.077 Uiso 0.50 1 calc PR B 1 C26B C 0.1450(8) 0.3397(8) 0.5833(3) 0.035(3) Uiso 0.50 1 d PD B 2 C27B C 0.0757(6) 0.4511(5) 0.5628(2) 0.0536(15) Uiso 0.50 1 d PD B 2 H27D H 0.0208 0.4868 0.5849 0.080 Uiso 0.50 1 calc PR B 2 H27E H 0.0210 0.4270 0.5350 0.080 Uiso 0.50 1 calc PR B 2 H27F H 0.1401 0.5124 0.5550 0.080 Uiso 0.50 1 calc PR B 2 C28B C 0.2346(6) 0.2857(7) 0.5483(2) 0.0557(17) Uiso 0.50 1 d PD B 2 H28D H 0.1811 0.2605 0.5204 0.084 Uiso 0.50 1 calc PR B 2 H28E H 0.2818 0.2139 0.5618 0.084 Uiso 0.50 1 calc PR B 2 H28F H 0.2973 0.3487 0.5406 0.084 Uiso 0.50 1 calc PR B 2 C29B C 0.0487(6) 0.2398(6) 0.5954(2) 0.0461(16) Uiso 0.50 1 d PD B 2 H29D H -0.0067 0.2723 0.6180 0.069 Uiso 0.50 1 calc PR B 2 H29E H 0.0971 0.1679 0.6082 0.069 Uiso 0.50 1 calc PR B 2 H29F H -0.0060 0.2152 0.5677 0.069 Uiso 0.50 1 calc PR B 2 S30A S 0.1661(7) 0.8025(7) 0.6058(3) 0.0339(10) Uani 0.50 1 d PD C 1 O31A O 0.2247(8) 0.8999(7) 0.6318(3) 0.0466(16) Uani 0.50 1 d PD C 1 O32A O 0.2530(11) 0.7102(8) 0.5935(4) 0.038(2) Uani 0.50 1 d PD C 1 O33A O 0.0439(6) 0.7619(7) 0.6191(2) 0.0531(15) Uani 0.50 1 d PD C 1 C34A C 0.1217(11) 0.8676(10) 0.5503(3) 0.059(4) Uani 0.50 1 d PD C 1 F35A F 0.0351(13) 0.9572(12) 0.5522(5) 0.104(4) Uani 0.50 1 d PD C 1 F36A F 0.2233(9) 0.9158(11) 0.5324(4) 0.081(3) Uani 0.50 1 d PD C 1 F37A F 0.0684(12) 0.7852(11) 0.5205(3) 0.091(3) Uani 0.50 1 d PD C 1 S30B S 0.1754(7) 0.8259(7) 0.6063(3) 0.0347(10) Uani 0.50 1 d PD D 2 O31B O 0.2495(7) 0.9323(6) 0.6241(3) 0.0481(19) Uani 0.50 1 d PD D 2 O32B O 0.2624(12) 0.7249(9) 0.6001(5) 0.058(3) Uani 0.50 1 d PD D 2 O33B O 0.0736(7) 0.7933(8) 0.6331(2) 0.0620(18) Uani 0.50 1 d PD D 2 C34B C 0.1032(10) 0.8717(9) 0.5501(2) 0.035(3) Uani 0.50 1 d PD D 2 F35B F 0.0260(10) 0.9684(9) 0.5519(4) 0.062(2) Uani 0.50 1 d PD D 2 F36B F 0.1931(9) 0.8967(11) 0.5232(4) 0.081(3) Uani 0.50 1 d PD D 2 F37B F 0.0307(11) 0.7782(10) 0.5333(3) 0.088(3) Uani 0.50 1 d PD D 2 C38 C 0.5598(9) 0.4751(8) 0.5303(3) 0.084(2) Uiso 0.50 1 d PD . . C39 C 0.5655(8) 0.4100(7) 0.4898(3) 0.0606(16) Uiso 0.50 1 d PD . . H39 H 0.6200 0.3395 0.4889 0.073 Uiso 0.50 1 calc PR . . C40 C 0.4895(8) 0.4496(8) 0.4500(3) 0.078(2) Uiso 0.50 1 d PD . . H40 H 0.4933 0.4061 0.4221 0.094 Uiso 0.50 1 calc PR . . C41 C 0.4114(12) 0.5493(11) 0.4516(4) 0.110(4) Uiso 0.50 1 d PD . . H41 H 0.3601 0.5742 0.4245 0.132 Uiso 0.50 1 calc PR . . C42 C 0.4035(9) 0.6164(8) 0.4913(3) 0.087(3) Uiso 0.50 1 d PD . . H42 H 0.3505 0.6882 0.4918 0.104 Uiso 0.50 1 calc PR . . C43 C 0.4775(7) 0.5738(7) 0.5311(3) 0.0610(16) Uiso 0.50 1 d PD . . H43 H 0.4699 0.6150 0.5593 0.073 Uiso 0.50 1 calc PR . . C44 C 0.6330(14) 0.4298(13) 0.5728(5) 0.139(5) Uiso 0.50 1 d P . . H44A H 0.7173 0.4725 0.5774 0.208 Uiso 0.50 1 calc PR . . H44B H 0.6477 0.3408 0.5704 0.208 Uiso 0.50 1 calc PR . . H44C H 0.5827 0.4463 0.5989 0.208 Uiso 0.50 1 calc PR . . 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 0.02441(13) 0.02466(13) 0.02965(13) -0.00011(9) 0.00279(9) 0.00093(9) Cl2 0.0340(3) 0.0321(3) 0.0355(3) 0.0007(2) -0.0050(2) 0.0052(2) N3 0.0263(8) 0.0305(9) 0.0377(10) 0.0039(8) 0.0056(7) 0.0015(7) N4 0.0292(9) 0.0302(9) 0.0390(10) 0.0058(8) 0.0101(7) 0.0018(7) C5 0.0290(10) 0.0382(12) 0.0305(10) -0.0026(9) 0.0053(8) -0.0069(9) C6 0.0265(10) 0.0529(15) 0.0466(13) 0.0003(11) 0.0099(9) -0.0005(10) C7 0.0258(10) 0.0400(12) 0.0474(13) 0.0022(10) 0.0037(9) 0.0041(9) N12 0.0280(8) 0.0235(8) 0.0296(8) 0.0012(7) 0.0018(7) 0.0033(6) N13 0.0363(9) 0.0278(9) 0.0258(8) 0.0004(7) -0.0001(7) 0.0097(7) C14 0.0261(9) 0.0227(9) 0.0307(10) 0.0005(8) 0.0049(8) -0.0020(7) C15 0.0380(12) 0.0472(14) 0.0281(11) -0.0003(9) 0.0068(9) 0.0113(10) C16 0.0347(11) 0.0444(13) 0.0298(11) 0.0063(9) 0.0031(9) 0.0097(10) C17 0.0268(10) 0.0253(10) 0.0371(11) -0.0004(8) 0.0051(8) 0.0032(8) C18 0.0351(12) 0.0428(13) 0.0467(13) -0.0072(11) 0.0089(10) 0.0093(10) C19 0.0434(13) 0.0293(11) 0.0537(14) 0.0098(10) 0.0135(11) 0.0095(10) C20 0.0311(11) 0.0390(13) 0.0603(15) -0.0028(12) -0.0050(10) 0.0029(10) N21 0.0275(8) 0.0275(9) 0.0282(8) -0.0004(7) 0.0005(7) 0.0021(7) N22 0.0290(8) 0.0272(9) 0.0273(8) 0.0021(7) -0.0005(7) 0.0011(7) C23 0.0299(10) 0.0289(10) 0.0322(10) -0.0034(8) 0.0034(8) -0.0022(8) C24 0.0384(11) 0.0252(10) 0.0384(11) 0.0024(9) 0.0021(9) -0.0008(9) C25 0.0351(11) 0.0283(11) 0.0335(11) 0.0044(9) 0.0008(9) 0.0004(8) S30A 0.0476(15) 0.027(2) 0.0275(11) 0.0077(11) 0.0071(8) 0.0044(11) O31A 0.063(4) 0.042(4) 0.034(2) -0.007(3) -0.003(2) -0.013(2) O32A 0.053(5) 0.022(2) 0.041(3) 0.006(2) 0.016(3) 0.008(2) O33A 0.041(3) 0.065(4) 0.056(4) 0.015(3) 0.014(3) -0.005(2) C34A 0.055(6) 0.045(7) 0.076(9) -0.009(5) -0.009(5) 0.004(5) F35A 0.100(7) 0.105(8) 0.101(8) 0.035(6) -0.018(5) 0.063(6) F36A 0.093(5) 0.098(4) 0.052(5) 0.033(3) 0.008(3) -0.031(4) F37A 0.122(8) 0.097(4) 0.048(4) -0.019(3) -0.024(4) -0.020(5) S30B 0.0378(12) 0.032(2) 0.0347(12) 0.0086(13) 0.0058(9) 0.0075(14) O31B 0.034(3) 0.038(3) 0.069(5) -0.016(3) -0.013(3) 0.003(2) O32B 0.046(4) 0.041(4) 0.083(7) 0.003(3) -0.014(3) 0.009(3) O33B 0.056(4) 0.093(5) 0.039(3) 0.009(3) 0.017(3) -0.010(3) C34B 0.040(4) 0.054(7) 0.011(3) 0.011(3) -0.003(2) 0.009(4) F35B 0.067(4) 0.059(4) 0.058(5) 0.017(3) 0.003(4) 0.032(4) F36B 0.079(4) 0.123(7) 0.044(4) 0.038(4) 0.029(4) 0.030(5) F37B 0.092(5) 0.098(5) 0.064(6) -0.029(4) -0.037(4) -0.001(4) _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 N3 2.0043(18) . ? Zn1 N21 2.0132(17) . ? Zn1 N12 2.0164(16) . ? Zn1 Cl2 2.2383(6) . ? N3 C7 1.339(3) . ? N3 N4 1.355(2) . ? N4 C5 1.341(3) . ? C5 C6 1.379(3) . ? C5 C8A 1.451(7) . ? C5 C8B 1.583(7) . ? C6 C7 1.385(3) . ? C8A C11A 1.510(8) . ? C8A C9A 1.560(8) . ? C8A C10A 1.564(8) . ? C8B C9B 1.485(8) . ? C8B C10B 1.536(9) . ? C8B C11B 1.542(8) . ? N12 C16 1.324(3) . ? N12 N13 1.358(2) . ? N13 C14 1.341(3) . ? C14 C15 1.373(3) . ? C14 C17 1.512(3) . ? C15 C16 1.393(3) . ? C17 C18 1.527(3) . ? C17 C20 1.533(3) . ? C17 C19 1.535(3) . ? N21 C25 1.339(3) . ? N21 N22 1.356(2) . ? N22 C23 1.343(3) . ? C23 C24 1.384(3) . ? C23 C26A 1.515(8) . ? C23 C26B 1.520(9) . ? C24 C25 1.383(3) . ? C26A C28A 1.505(9) . ? C26A C27A 1.529(9) . ? C26A C29A 1.571(10) . ? C26B C27B 1.498(10) . ? C26B C29B 1.532(10) . ? C26B C28B 1.558(10) . ? S30A O31A 1.404(7) . ? S30A O32A 1.410(6) . ? S30A O33A 1.421(6) . ? S30A C34A 1.791(8) . ? C34A F35A 1.322(8) . ? C34A F36A 1.322(8) . ? C34A F37A 1.331(8) . ? S30B O33B 1.415(7) . ? S30B O32B 1.436(7) . ? S30B O31B 1.452(6) . ? S30B C34B 1.811(7) . ? C34B F36B 1.300(7) . ? C34B F35B 1.319(8) . ? C34B F37B 1.325(7) . ? C38 C43 1.365(10) . ? C38 C39 1.387(10) . ? C38 C44 1.479(16) . ? C39 C40 1.409(10) . ? C40 C41 1.349(12) . ? C41 C42 1.383(12) . ? C42 C43 1.408(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 N3 Zn1 N21 108.54(7) . . ? N3 Zn1 N12 113.82(7) . . ? N21 Zn1 N12 118.47(7) . . ? N3 Zn1 Cl2 107.07(5) . . ? N21 Zn1 Cl2 103.16(5) . . ? N12 Zn1 Cl2 104.56(5) . . ? C7 N3 N4 104.99(18) . . ? C7 N3 Zn1 121.99(16) . . ? N4 N3 Zn1 133.01(14) . . ? C5 N4 N3 112.16(18) . . ? N4 C5 C6 106.26(19) . . ? N4 C5 C8A 128.0(3) . . ? C6 C5 C8A 125.8(3) . . ? N4 C5 C8B 119.0(3) . . ? C6 C5 C8B 134.7(3) . . ? C5 C6 C7 106.03(19) . . ? N3 C7 C6 110.6(2) . . ? C5 C8A C11A 111.0(5) . . ? C5 C8A C9A 109.6(5) . . ? C11A C8A C9A 107.7(5) . . ? C5 C8A C10A 110.4(5) . . ? C11A C8A C10A 112.0(5) . . ? C9A C8A C10A 105.8(5) . . ? C9B C8B C10B 112.4(6) . . ? C9B C8B C11B 111.5(6) . . ? C10B C8B C11B 106.9(6) . . ? C9B C8B C5 114.0(5) . . ? C10B C8B C5 105.7(5) . . ? C11B C8B C5 105.7(5) . . ? C16 N12 N13 104.83(16) . . ? C16 N12 Zn1 123.00(14) . . ? N13 N12 Zn1 132.17(13) . . ? C14 N13 N12 112.52(16) . . ? N13 C14 C15 105.78(18) . . ? N13 C14 C17 121.91(18) . . ? C15 C14 C17 132.31(19) . . ? C14 C15 C16 106.14(19) . . ? N12 C16 C15 110.72(19) . . ? C14 C17 C18 109.32(18) . . ? C14 C17 C20 109.38(17) . . ? C18 C17 C20 109.20(19) . . ? C14 C17 C19 109.42(17) . . ? C18 C17 C19 110.16(19) . . ? C20 C17 C19 109.3(2) . . ? C25 N21 N22 105.13(17) . . ? C25 N21 Zn1 125.24(14) . . ? N22 N21 Zn1 129.63(13) . . ? C23 N22 N21 111.85(17) . . ? N22 C23 C24 106.47(18) . . ? N22 C23 C26A 124.4(4) . . ? C24 C23 C26A 129.1(4) . . ? N22 C23 C26B 122.2(4) . . ? C24 C23 C26B 131.1(4) . . ? C25 C24 C23 105.75(19) . . ? N21 C25 C24 110.80(19) . . ? C28A C26A C23 111.2(6) . . ? C28A C26A C27A 111.1(6) . . ? C23 C26A C27A 111.0(6) . . ? C28A C26A C29A 110.5(6) . . ? C23 C26A C29A 106.3(6) . . ? C27A C26A C29A 106.4(6) . . ? C27B C26B C23 112.7(6) . . ? C27B C26B C29B 111.6(7) . . ? C23 C26B C29B 108.3(6) . . ? C27B C26B C28B 109.0(6) . . ? C23 C26B C28B 106.1(6) . . ? C29B C26B C28B 108.9(6) . . ? O31A S30A O32A 114.9(6) . . ? O31A S30A O33A 115.4(5) . . ? O32A S30A O33A 116.8(6) . . ? O31A S30A C34A 104.9(6) . . ? O32A S30A C34A 99.2(8) . . ? O33A S30A C34A 102.4(6) . . ? F35A C34A F36A 106.7(8) . . ? F35A C34A F37A 106.3(8) . . ? F36A C34A F37A 107.2(8) . . ? F35A C34A S30A 111.5(10) . . ? F36A C34A S30A 111.9(9) . . ? F37A C34A S30A 112.8(8) . . ? O33B S30B O32B 112.6(6) . . ? O33B S30B O31B 112.8(5) . . ? O32B S30B O31B 109.7(6) . . ? O33B S30B C34B 108.3(6) . . ? O32B S30B C34B 107.5(8) . . ? O31B S30B C34B 105.5(6) . . ? F36B C34B F35B 109.0(6) . . ? F36B C34B F37B 110.0(6) . . ? F35B C34B F37B 107.5(7) . . ? F36B C34B S30B 110.9(8) . . ? F35B C34B S30B 112.2(8) . . ? F37B C34B S30B 107.3(7) . . ? C43 C38 C39 119.2(8) . . ? C43 C38 C44 120.8(9) . . ? C39 C38 C44 119.7(9) . . ? C38 C39 C40 119.4(7) . . ? C41 C40 C39 120.0(8) . . ? C40 C41 C42 122.2(10) . . ? C41 C42 C43 117.1(8) . . ? C38 C43 C42 122.0(7) . . ? 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 O31A 0.88 2.31 3.119(9) 152.4 . N4 H4 O31B 0.88 2.17 3.011(8) 160.0 . N13 H13 O31A 0.88 2.18 2.961(8) 148.3 . N13 H13 O31B 0.88 2.59 3.333(8) 142.7 . N13 H13 O33B 0.88 2.16 2.981(6) 156.1 . N22 H22 O32A 0.88 1.91 2.752(9) 160.4 . N22 H22 O32B 0.88 1.99 2.810(11) 154.6 . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.599 _refine_diff_density_min -0.431 _refine_diff_density_rms 0.070 #=END data_sr15 _database_code_CSD 191078 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Chloro-tris[5-tertbutylpyrazole]zinc(II) hexafluorophosphate dichloromethane solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H36 Cl N6 Zn, P F6, C H2 Cl2' _chemical_formula_sum 'C22 H38 Cl3 F6 N6 P Zn' _chemical_formula_weight 703.27 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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 14.4475(2) _cell_length_b 14.7862(2) _cell_length_c 15.1702(2) _cell_angle_alpha 90.2896(5) _cell_angle_beta 91.5739(5) _cell_angle_gamma 96.3712(7) _cell_volume 3219.38(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 59093 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 27.50 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 1.119 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5938 _exptl_absorpt_correction_T_max 0.7446 _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 59093 _diffrn_reflns_av_R_equivalents 0.0852 _diffrn_reflns_av_sigmaI/netI 0.0526 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 27.50 _reflns_number_total 14762 _reflns_number_gt 12148 _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, two PF~6~^-^ anions and two CH~2~Cl~2~ molecules, all lying on general positions. The PF~6~^-^ anion P66-F72 is disordered over three equally occupied orientations labelled 'A', 'B' and 'C'. All P-F bonds were restrained to 1.60(2)\%A, and cis- and trans-F...F distances within a given disorder orientation to 2.26(2) and 3.20(2)\%A, respectively. Both dichloromethane molecules are disordered. For the molecule centred on C73, the atom Cl75 only is disordered over two orientations Cl75A and Cl75B with occupancies of 0.70 and 0.30 respectively. The molecule C76-Cl78 is disordered over four distinct sites: C76A, Cl77A, Cl78A (occupancy 0.55) C76B, Cl77A, Cl78B (occupancy 0.15; ie Cl77A has total occupancy 0.70) C76C, Cl77C, Cl78C (occupancy 0.15) C76D, Cl77C, Cl78D (occupancy 0.15; ie Cl77C has total occupancy 0.30) All C-Cl bonds were restrained to 1.75(2)\%A, and Cl...Cl distances within a given disorder orientation to 2.86(2)\%A. All non-H atoms with occupancy >0.5 were refined anisotropically, while all H atoms were placed in calculated positions and refined using a riding model. The largest residual Fourier peak of 1.11 e.\%A^-3^ lies within the disordered PF~6~^-^ anion, while the deepest electron hole of -1.15 e.\%A^-3^ is 0.6\%A from Cl74. ; _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^)+(0.0861P)^2^+5.0169P] 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 14762 _refine_ls_number_parameters 776 _refine_ls_number_restraints 80 _refine_ls_R_factor_all 0.0689 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1621 _refine_ls_wR_factor_gt 0.1497 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.049 _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 0.41036(2) 0.37715(2) 0.70524(2) 0.02185(10) Uani 1 1 d . . . Cl2 Cl 0.51952(5) 0.41266(5) 0.81077(5) 0.02751(16) Uani 1 1 d . . . N3 N 0.47621(17) 0.38804(16) 0.59131(16) 0.0221(5) Uani 1 1 d . . . N4 N 0.45570(17) 0.33481(16) 0.51865(16) 0.0222(5) Uani 1 1 d . . . H4 H 0.4033 0.2990 0.5104 0.027 Uiso 1 1 calc R . . C5 C 0.5250(2) 0.34336(19) 0.46086(19) 0.0214(5) Uani 1 1 d . . . C6 C 0.5939(2) 0.4061(2) 0.4978(2) 0.0257(6) Uani 1 1 d . . . H6 H 0.6518 0.4276 0.4730 0.031 Uiso 1 1 calc R . . C7 C 0.5612(2) 0.4309(2) 0.5781(2) 0.0250(6) Uani 1 1 d . . . H7 H 0.5945 0.4727 0.6184 0.030 Uiso 1 1 calc R . . C8 C 0.5199(2) 0.2926(2) 0.3737(2) 0.0258(6) Uani 1 1 d . . . C9 C 0.6197(3) 0.2812(2) 0.3471(3) 0.0372(8) Uani 1 1 d . . . H9A H 0.6557 0.3412 0.3433 0.056 Uiso 1 1 calc R . . H9B H 0.6181 0.2505 0.2895 0.056 Uiso 1 1 calc R . . H9C H 0.6490 0.2446 0.3913 0.056 Uiso 1 1 calc R . . C10 C 0.4640(2) 0.1985(2) 0.3823(2) 0.0321(7) Uani 1 1 d . . . H10A H 0.4955 0.1622 0.4252 0.048 Uiso 1 1 calc R . . H10B H 0.4595 0.1674 0.3248 0.048 Uiso 1 1 calc R . . H10C H 0.4013 0.2058 0.4022 0.048 Uiso 1 1 calc R . . C11 C 0.4732(3) 0.3487(2) 0.3039(2) 0.0387(8) Uani 1 1 d . . . H11A H 0.4087 0.3537 0.3199 0.058 Uiso 1 1 calc R . . H11B H 0.4738 0.3186 0.2463 0.058 Uiso 1 1 calc R . . H11C H 0.5074 0.4097 0.3011 0.058 Uiso 1 1 calc R . . N12 N 0.31450(17) 0.46314(17) 0.72911(17) 0.0238(5) Uani 1 1 d . . . N13 N 0.23930(17) 0.47768(17) 0.67800(17) 0.0255(5) Uani 1 1 d . . . H13 H 0.2251 0.4507 0.6268 0.031 Uiso 1 1 calc R . . C14 C 0.1887(2) 0.5386(2) 0.7151(2) 0.0259(6) Uani 1 1 d . . . C15 C 0.2337(2) 0.5645(2) 0.7944(2) 0.0292(6) Uani 1 1 d . . . H15 H 0.2156 0.6067 0.8363 0.035 Uiso 1 1 calc R . . C16 C 0.3106(2) 0.5162(2) 0.8001(2) 0.0265(6) Uani 1 1 d . . . H16 H 0.3546 0.5203 0.8480 0.032 Uiso 1 1 calc R . . C17 C 0.1013(2) 0.5657(2) 0.6706(2) 0.0319(7) Uani 1 1 d . . . C18 C 0.0694(3) 0.6459(3) 0.7210(4) 0.0570(12) Uani 1 1 d . . . H18A H 0.0554 0.6276 0.7816 0.086 Uiso 1 1 calc R . . H18B H 0.0134 0.6648 0.6918 0.086 Uiso 1 1 calc R . . H18C H 0.1191 0.6968 0.7219 0.086 Uiso 1 1 calc R . . C19 C 0.0257(3) 0.4845(3) 0.6707(3) 0.0449(9) Uani 1 1 d . . . H19A H 0.0472 0.4333 0.6388 0.067 Uiso 1 1 calc R . . H19B H -0.0313 0.5015 0.6418 0.067 Uiso 1 1 calc R . . H19C H 0.0127 0.4666 0.7317 0.067 Uiso 1 1 calc R . . C20 C 0.1203(3) 0.5931(4) 0.5752(3) 0.0558(12) Uani 1 1 d . . . H20A H 0.1705 0.6433 0.5743 0.084 Uiso 1 1 calc R . . H20B H 0.0637 0.6125 0.5476 0.084 Uiso 1 1 calc R . . H20C H 0.1388 0.5409 0.5426 0.084 Uiso 1 1 calc R . . N21 N 0.33393(18) 0.25535(17) 0.70646(18) 0.0264(5) Uani 1 1 d . . . N22 N 0.35827(18) 0.17404(17) 0.67777(17) 0.0254(5) Uani 1 1 d . . . H22 H 0.4143 0.1656 0.6603 0.030 Uiso 1 1 calc R . . C23 C 0.2862(2) 0.1083(2) 0.6795(2) 0.0280(6) Uani 1 1 d . . . C24 C 0.2116(2) 0.1484(2) 0.7110(3) 0.0363(8) Uani 1 1 d . . . H24 H 0.1505 0.1198 0.7202 0.044 Uiso 1 1 calc R . . C25 C 0.2445(2) 0.2396(2) 0.7265(2) 0.0345(7) Uani 1 1 d . . . H25 H 0.2082 0.2842 0.7484 0.041 Uiso 1 1 calc R . . C26 C 0.2938(3) 0.0122(2) 0.6488(3) 0.0356(7) Uani 1 1 d . . . C27 C 0.3710(3) -0.0268(3) 0.7040(4) 0.0573(12) Uani 1 1 d . . . H27A H 0.4315 0.0063 0.6908 0.086 Uiso 1 1 calc R . . H27B H 0.3714 -0.0914 0.6894 0.086 Uiso 1 1 calc R . . H27C H 0.3590 -0.0202 0.7668 0.086 Uiso 1 1 calc R . . C28 C 0.3186(4) 0.0142(3) 0.5511(3) 0.0566(12) Uani 1 1 d . . . H28A H 0.2680 0.0367 0.5161 0.085 Uiso 1 1 calc R . . H28B H 0.3273 -0.0474 0.5313 0.085 Uiso 1 1 calc R . . H28C H 0.3763 0.0545 0.5434 0.085 Uiso 1 1 calc R . . C29 C 0.2019(3) -0.0463(3) 0.6623(3) 0.0499(10) Uani 1 1 d . . . H29A H 0.1850 -0.0428 0.7242 0.075 Uiso 1 1 calc R . . H29B H 0.2085 -0.1096 0.6466 0.075 Uiso 1 1 calc R . . H29C H 0.1531 -0.0242 0.6248 0.075 Uiso 1 1 calc R . . P30 P 0.19271(6) 0.31884(6) 0.46200(6) 0.03088(19) Uani 1 1 d . . . F31 F 0.14345(17) 0.31606(19) 0.55451(17) 0.0556(6) Uani 1 1 d . . . F32 F 0.26261(15) 0.24900(15) 0.49792(17) 0.0459(5) Uani 1 1 d . . . F33 F 0.2455(2) 0.3224(2) 0.37173(18) 0.0702(8) Uani 1 1 d . . . F34 F 0.12718(19) 0.3904(2) 0.4269(2) 0.0726(9) Uani 1 1 d . . . F35 F 0.12179(17) 0.23660(19) 0.4276(2) 0.0643(8) Uani 1 1 d . . . F36 F 0.26575(16) 0.40134(15) 0.4997(2) 0.0551(7) Uani 1 1 d . . . Zn37 Zn 0.64839(2) 0.16301(2) 0.74722(2) 0.02528(10) Uani 1 1 d . . . Cl38 Cl 0.57168(5) 0.15901(6) 0.61603(5) 0.03113(17) Uani 1 1 d . . . N39 N 0.71952(19) 0.28626(18) 0.75806(17) 0.0271(5) Uani 1 1 d . . . N40 N 0.74266(18) 0.33511(17) 0.83331(17) 0.0261(5) Uani 1 1 d . . . H40 H 0.7390 0.3124 0.8867 0.031 Uiso 1 1 calc R . . C41 C 0.7720(2) 0.4228(2) 0.8156(2) 0.0275(6) Uani 1 1 d . . . C42 C 0.7681(2) 0.4312(2) 0.7252(2) 0.0316(7) Uani 1 1 d . . . H42 H 0.7843 0.4847 0.6920 0.038 Uiso 1 1 calc R . . C43 C 0.7353(2) 0.3449(2) 0.6924(2) 0.0317(7) Uani 1 1 d . . . H43 H 0.7256 0.3300 0.6316 0.038 Uiso 1 1 calc R . . C44 C 0.8014(2) 0.4908(2) 0.8885(2) 0.0323(7) Uani 1 1 d . . . C45 C 0.8142(3) 0.5863(3) 0.8490(3) 0.0515(10) Uani 1 1 d . . . H45A H 0.8338 0.6309 0.8957 0.077 Uiso 1 1 calc R . . H45B H 0.7552 0.6002 0.8218 0.077 Uiso 1 1 calc R . . H45C H 0.8620 0.5888 0.8041 0.077 Uiso 1 1 calc R . . C46 C 0.7265(3) 0.4867(2) 0.9586(2) 0.0358(7) Uani 1 1 d . . . H46A H 0.7180 0.4254 0.9835 0.054 Uiso 1 1 calc R . . H46B H 0.6676 0.5010 0.9315 0.054 Uiso 1 1 calc R . . H46C H 0.7462 0.5309 1.0056 0.054 Uiso 1 1 calc R . . C47 C 0.8938(3) 0.4682(3) 0.9306(3) 0.0561(12) Uani 1 1 d . . . H47A H 0.8856 0.4063 0.9541 0.084 Uiso 1 1 calc R . . H47B H 0.9128 0.5114 0.9786 0.084 Uiso 1 1 calc R . . H47C H 0.9419 0.4723 0.8860 0.084 Uiso 1 1 calc R . . N48 N 0.71825(18) 0.05284(17) 0.75038(17) 0.0259(5) Uani 1 1 d . . . N49 N 0.78996(18) 0.03534(18) 0.80502(18) 0.0278(5) Uani 1 1 d . . . H49 H 0.8106 0.0702 0.8502 0.033 Uiso 1 1 calc R . . C50 C 0.8257(2) -0.0413(2) 0.7822(2) 0.0282(6) Uani 1 1 d . . . C51 C 0.7735(2) -0.0763(2) 0.7101(3) 0.0361(8) Uani 1 1 d . . . H51 H 0.7804 -0.1309 0.6788 0.043 Uiso 1 1 calc R . . C52 C 0.7087(2) -0.0157(2) 0.6924(2) 0.0304(7) Uani 1 1 d . . . H52 H 0.6636 -0.0223 0.6454 0.036 Uiso 1 1 calc R . . C53 C 0.9082(2) -0.0743(2) 0.8317(3) 0.0343(7) Uani 1 1 d . . . C54 C 0.9828(3) 0.0059(3) 0.8536(4) 0.0621(13) Uani 1 1 d . . . H54A H 0.9997 0.0388 0.7994 0.093 Uiso 1 1 calc R . . H54B H 1.0381 -0.0172 0.8799 0.093 Uiso 1 1 calc R . . H54C H 0.9579 0.0473 0.8953 0.093 Uiso 1 1 calc R . . C55 C 0.8782(4) -0.1167(4) 0.9200(4) 0.0704(15) Uani 1 1 d . . . H55A H 0.9323 -0.1375 0.9509 0.106 Uiso 1 1 calc R . . H55B H 0.8307 -0.1685 0.9092 0.106 Uiso 1 1 calc R . . H55C H 0.8523 -0.0711 0.9563 0.106 Uiso 1 1 calc R . . C56 C 0.9496(4) -0.1450(4) 0.7778(4) 0.0783(18) Uani 1 1 d . . . H56A H 0.9731 -0.1177 0.7229 0.117 Uiso 1 1 calc R . . H56B H 0.9016 -0.1956 0.7639 0.117 Uiso 1 1 calc R . . H56C H 1.0009 -0.1676 0.8116 0.117 Uiso 1 1 calc R . . N57 N 0.55550(19) 0.14671(18) 0.84366(18) 0.0292(6) Uani 1 1 d . . . N58 N 0.52213(18) 0.21245(18) 0.89181(17) 0.0268(5) Uani 1 1 d . . . H58 H 0.5376 0.2711 0.8844 0.032 Uiso 1 1 calc R . . C59 C 0.4624(2) 0.1772(2) 0.9524(2) 0.0283(6) Uani 1 1 d . . . C60 C 0.4568(3) 0.0838(2) 0.9427(2) 0.0387(8) Uani 1 1 d . . . H60 H 0.4199 0.0393 0.9753 0.046 Uiso 1 1 calc R . . C61 C 0.5163(3) 0.0685(2) 0.8753(2) 0.0383(8) Uani 1 1 d . . . H61 H 0.5275 0.0101 0.8547 0.046 Uiso 1 1 calc R . . C62 C 0.4144(2) 0.2360(2) 1.0149(2) 0.0333(7) Uani 1 1 d . . . C63 C 0.3274(3) 0.2645(3) 0.9669(3) 0.0472(10) Uani 1 1 d . . . H63A H 0.2874 0.2100 0.9467 0.071 Uiso 1 1 calc R . . H63B H 0.3462 0.3022 0.9161 0.071 Uiso 1 1 calc R . . H63C H 0.2931 0.2994 1.0075 0.071 Uiso 1 1 calc R . . C64 C 0.4800(3) 0.3210(3) 1.0430(2) 0.0437(9) Uani 1 1 d . . . H64A H 0.4965 0.3577 0.9909 0.066 Uiso 1 1 calc R . . H64B H 0.5367 0.3023 1.0710 0.066 Uiso 1 1 calc R . . H64C H 0.4486 0.3571 1.0848 0.066 Uiso 1 1 calc R . . C65 C 0.3869(3) 0.1798(3) 1.0966(2) 0.0425(9) Uani 1 1 d . . . H65A H 0.4429 0.1612 1.1259 0.064 Uiso 1 1 calc R . . H65B H 0.3450 0.1257 1.0788 0.064 Uiso 1 1 calc R . . H65C H 0.3550 0.2168 1.1373 0.064 Uiso 1 1 calc R . . P66A P 0.7691(4) 0.1760(4) 1.0449(3) 0.0302(14) Uiso 0.33 1 d PD A 1 F67A F 0.7162(5) 0.2578(5) 1.0112(5) 0.0412(15) Uiso 0.33 1 d PD A 1 F68A F 0.8216(6) 0.1745(5) 0.9417(5) 0.052(2) Uiso 0.33 1 d PD A 1 F69A F 0.8329(7) 0.0939(6) 1.0653(6) 0.069(2) Uiso 0.33 1 d PD A 1 F70A F 0.7323(8) 0.1819(7) 1.1359(6) 0.083(3) Uiso 0.33 1 d PD A 1 F71A F 0.6892(6) 0.1067(6) 1.0112(6) 0.066(2) Uiso 0.33 1 d PD A 1 F72A F 0.8666(6) 0.2457(6) 1.0607(6) 0.065(2) Uiso 0.33 1 d PD A 1 P66B P 0.7717(4) 0.1622(3) 1.0367(3) 0.0310(14) Uiso 0.33 1 d PD B 2 F67B F 0.7534(6) 0.2721(5) 1.0334(5) 0.0510(18) Uiso 0.33 1 d PD B 2 F68B F 0.7467(6) 0.1628(5) 0.9344(4) 0.051(2) Uiso 0.33 1 d PD B 2 F69B F 0.7881(8) 0.0609(6) 1.0409(7) 0.087(3) Uiso 0.33 1 d PD B 2 F70B F 0.8057(7) 0.1695(7) 1.1378(6) 0.076(3) Uiso 0.33 1 d PD B 2 F71B F 0.6663(5) 0.1383(6) 1.0547(6) 0.069(2) Uiso 0.33 1 d PD B 2 F72B F 0.8812(6) 0.1967(9) 1.0208(8) 0.112(4) Uiso 0.33 1 d PD B 2 P66C P 0.7885(3) 0.1790(3) 1.0342(3) 0.0245(9) Uiso 0.33 1 d PD C 3 F67C F 0.6880(9) 0.2238(12) 1.0267(11) 0.193(10) Uiso 0.33 1 d PD C 3 F68C F 0.7863(7) 0.1787(5) 0.9286(4) 0.0436(18) Uiso 0.33 1 d PD C 3 F69C F 0.8734(8) 0.1273(9) 1.0333(9) 0.123(5) Uiso 0.33 1 d PD C 3 F70C F 0.7745(8) 0.1840(6) 1.1416(5) 0.055(2) Uiso 0.33 1 d PD C 3 F71C F 0.7246(9) 0.0787(7) 1.0282(8) 0.098(4) Uiso 0.33 1 d PD C 3 F72C F 0.8376(8) 0.2762(6) 1.0393(7) 0.085(3) Uiso 0.33 1 d PD C 3 C73 C 0.9704(4) 0.7444(4) 0.1211(3) 0.0655(13) Uani 1 1 d D . . H73A H 0.9361 0.7984 0.1136 0.079 Uiso 1 1 calc R D 1 H73B H 1.0136 0.7431 0.0716 0.079 Uiso 1 1 calc R D 1 Cl74 Cl 0.89086(8) 0.64553(8) 0.11709(9) 0.0584(3) Uani 1 1 d D E . Cl75A Cl 1.0358(3) 0.7546(4) 0.2223(3) 0.0978(16) Uani 0.70 1 d PD E 1 Cl75B Cl 1.0378(4) 0.7509(4) 0.2189(3) 0.0309(11) Uiso 0.30 1 d PD E 2 C76A C 0.0506(6) 0.8396(7) 0.4509(8) 0.061(3) Uani 0.55 1 d PD F 1 H76A H 0.0343 0.8416 0.5138 0.074 Uiso 0.55 1 calc PR F 1 H76B H 0.0072 0.7926 0.4199 0.074 Uiso 0.55 1 calc PR F 1 Cl77A Cl 0.0472(2) 0.9517(2) 0.39942(19) 0.0944(7) Uani 0.70 1 d PD . . Cl78A Cl 0.1689(3) 0.8176(3) 0.4395(3) 0.0895(14) Uani 0.55 1 d PD F 1 C76B C 0.0239(16) 0.8556(12) 0.4632(15) 0.022(5) Uiso 0.15 1 d PD F 2 H76C H 0.0259 0.8731 0.5263 0.026 Uiso 0.15 1 calc PR F 2 H76D H -0.0392 0.8255 0.4480 0.026 Uiso 0.15 1 calc PR F 2 Cl78B Cl 0.1048(11) 0.7823(9) 0.4446(10) 0.095(5) Uiso 0.15 1 d PD F 2 Cl77C Cl 0.1438(7) 0.7969(5) 0.4340(6) 0.0703(19) Uiso 0.30 1 d PD . . C76C C 0.048(4) 0.822(4) 0.493(3) 0.13(3) Uiso 0.15 1 d PD F 3 H76E H 0.0663 0.8412 0.5539 0.162 Uiso 0.15 1 calc PR F 3 H76F H -0.0006 0.7693 0.4936 0.162 Uiso 0.15 1 calc PR F 3 Cl78C Cl 0.0135(9) 0.9113(10) 0.4295(11) 0.092(4) Uiso 0.15 1 d PD F 3 C76D C 0.078(5) 0.878(4) 0.394(2) 0.15(2) Uiso 0.15 1 d PD F 4 H76G H 0.0278 0.8463 0.3563 0.177 Uiso 0.15 1 calc PR F 4 H76H H 0.1185 0.9180 0.3555 0.177 Uiso 0.15 1 calc PR F 4 Cl78D Cl 0.0258(14) 0.9493(14) 0.4687(16) 0.148(7) Uiso 0.15 1 d PD . 4 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 0.02210(18) 0.02114(17) 0.02321(18) -0.00078(12) -0.00029(12) 0.00670(12) Cl2 0.0289(4) 0.0272(4) 0.0270(4) 0.0014(3) -0.0067(3) 0.0075(3) N3 0.0231(12) 0.0216(12) 0.0223(12) -0.0024(9) -0.0010(9) 0.0060(9) N4 0.0215(12) 0.0219(12) 0.0231(12) -0.0006(9) -0.0025(9) 0.0027(9) C5 0.0246(14) 0.0181(13) 0.0221(14) 0.0032(10) 0.0012(11) 0.0050(10) C6 0.0233(14) 0.0234(14) 0.0301(15) -0.0011(12) 0.0011(11) 0.0008(11) C7 0.0241(14) 0.0213(14) 0.0290(15) -0.0014(11) -0.0048(11) 0.0008(11) C8 0.0316(16) 0.0216(14) 0.0244(15) -0.0004(11) 0.0051(12) 0.0027(11) C9 0.0395(19) 0.0300(17) 0.0420(19) -0.0090(14) 0.0138(15) 0.0008(14) C10 0.0364(17) 0.0253(15) 0.0333(17) -0.0063(13) 0.0043(13) -0.0031(13) C11 0.061(2) 0.0329(18) 0.0229(16) -0.0017(13) -0.0037(15) 0.0104(16) N12 0.0227(12) 0.0242(12) 0.0261(13) -0.0008(10) -0.0009(9) 0.0094(9) N13 0.0255(13) 0.0256(13) 0.0264(13) -0.0025(10) -0.0049(10) 0.0092(10) C14 0.0210(14) 0.0231(14) 0.0347(16) 0.0035(12) 0.0030(12) 0.0064(11) C15 0.0307(16) 0.0290(16) 0.0293(16) -0.0050(12) 0.0056(12) 0.0096(12) C16 0.0305(15) 0.0264(15) 0.0233(14) -0.0013(11) 0.0006(11) 0.0068(12) C17 0.0239(15) 0.0326(17) 0.0409(19) 0.0033(14) -0.0003(13) 0.0110(12) C18 0.045(2) 0.049(2) 0.081(3) -0.019(2) -0.015(2) 0.0287(19) C19 0.0293(18) 0.043(2) 0.063(3) 0.0044(18) -0.0046(17) 0.0079(15) C20 0.040(2) 0.078(3) 0.053(3) 0.027(2) -0.0026(18) 0.020(2) N21 0.0295(13) 0.0200(12) 0.0307(14) -0.0013(10) 0.0031(10) 0.0075(10) N22 0.0258(13) 0.0220(12) 0.0295(13) -0.0020(10) 0.0006(10) 0.0084(10) C23 0.0318(16) 0.0238(15) 0.0287(16) 0.0013(12) 0.0016(12) 0.0036(12) C24 0.0307(17) 0.0313(17) 0.047(2) -0.0004(14) 0.0108(14) 0.0005(13) C25 0.0327(17) 0.0292(16) 0.0432(19) -0.0020(14) 0.0130(14) 0.0074(13) C26 0.0410(19) 0.0213(15) 0.045(2) -0.0035(13) 0.0021(15) 0.0039(13) C27 0.056(3) 0.030(2) 0.086(3) 0.001(2) -0.009(2) 0.0102(18) C28 0.077(3) 0.040(2) 0.053(3) -0.0149(19) 0.016(2) -0.001(2) C29 0.048(2) 0.0295(19) 0.071(3) -0.0028(18) 0.008(2) -0.0047(16) P30 0.0257(4) 0.0329(4) 0.0346(5) -0.0058(3) -0.0063(3) 0.0073(3) F31 0.0477(14) 0.0700(17) 0.0507(14) -0.0093(12) 0.0129(11) 0.0106(12) F32 0.0347(11) 0.0355(11) 0.0689(16) 0.0024(10) -0.0021(10) 0.0105(9) F33 0.0737(19) 0.095(2) 0.0441(15) 0.0088(14) 0.0136(13) 0.0165(16) F34 0.0542(16) 0.0742(19) 0.094(2) 0.0120(16) -0.0238(15) 0.0315(14) F35 0.0391(13) 0.0664(17) 0.083(2) -0.0328(15) -0.0091(12) -0.0075(12) F36 0.0374(12) 0.0338(12) 0.092(2) -0.0154(12) -0.0069(12) -0.0001(9) Zn37 0.02701(19) 0.02344(18) 0.02674(19) -0.00199(13) -0.00193(14) 0.00959(13) Cl38 0.0289(4) 0.0387(4) 0.0270(4) -0.0018(3) -0.0038(3) 0.0107(3) N39 0.0314(14) 0.0255(13) 0.0254(13) -0.0038(10) -0.0048(10) 0.0092(10) N40 0.0277(13) 0.0262(13) 0.0245(13) -0.0013(10) -0.0041(10) 0.0053(10) C41 0.0195(14) 0.0278(15) 0.0363(17) 0.0003(12) -0.0012(12) 0.0073(11) C42 0.0299(16) 0.0301(16) 0.0346(17) 0.0038(13) -0.0022(13) 0.0025(12) C43 0.0308(16) 0.0363(17) 0.0288(16) 0.0017(13) -0.0017(12) 0.0076(13) C44 0.0288(16) 0.0291(16) 0.0387(18) -0.0067(13) -0.0037(13) 0.0042(12) C45 0.071(3) 0.0301(19) 0.050(2) -0.0058(17) 0.007(2) -0.0096(18) C46 0.0388(18) 0.0338(18) 0.0347(18) -0.0072(14) 0.0001(14) 0.0042(14) C47 0.034(2) 0.067(3) 0.068(3) -0.031(2) -0.0203(19) 0.0149(19) N48 0.0257(13) 0.0243(12) 0.0287(13) -0.0031(10) -0.0054(10) 0.0083(10) N49 0.0307(14) 0.0240(13) 0.0300(14) -0.0036(10) -0.0064(11) 0.0101(10) C50 0.0255(15) 0.0225(14) 0.0372(17) -0.0029(12) 0.0008(12) 0.0055(11) C51 0.0344(18) 0.0288(16) 0.046(2) -0.0146(14) -0.0065(15) 0.0099(13) C52 0.0282(16) 0.0282(16) 0.0352(17) -0.0083(13) -0.0054(13) 0.0066(12) C53 0.0283(16) 0.0277(16) 0.048(2) -0.0026(14) -0.0053(14) 0.0108(13) C54 0.044(2) 0.053(3) 0.089(4) -0.002(2) -0.023(2) 0.0085(19) C55 0.055(3) 0.081(4) 0.077(4) 0.026(3) -0.008(2) 0.019(3) C56 0.070(3) 0.077(4) 0.095(4) -0.031(3) -0.030(3) 0.050(3) N57 0.0342(14) 0.0252(13) 0.0297(14) -0.0013(10) 0.0018(11) 0.0102(11) N58 0.0316(14) 0.0232(12) 0.0270(13) -0.0003(10) 0.0017(10) 0.0089(10) C59 0.0296(16) 0.0322(16) 0.0245(15) 0.0052(12) -0.0014(12) 0.0100(12) C60 0.048(2) 0.0312(18) 0.0374(19) 0.0067(14) 0.0077(15) 0.0035(15) C61 0.054(2) 0.0249(16) 0.0369(19) -0.0018(14) 0.0038(16) 0.0095(15) C62 0.0380(18) 0.0399(18) 0.0247(15) 0.0030(13) 0.0045(13) 0.0154(14) C63 0.046(2) 0.061(3) 0.040(2) 0.0040(18) 0.0047(16) 0.0289(19) C64 0.064(3) 0.038(2) 0.0307(18) -0.0041(15) 0.0087(17) 0.0133(18) C65 0.049(2) 0.051(2) 0.0304(18) 0.0054(16) 0.0093(15) 0.0120(17) C73 0.069(3) 0.064(3) 0.061(3) 0.003(2) -0.008(2) -0.002(2) Cl74 0.0438(6) 0.0604(7) 0.0709(7) -0.0241(6) -0.0033(5) 0.0082(5) Cl75A 0.089(2) 0.0732(18) 0.123(3) 0.0037(14) -0.0451(17) -0.0146(12) C76A 0.041(5) 0.080(7) 0.061(6) 0.002(5) 0.028(4) -0.006(5) Cl77A 0.0947(17) 0.1046(19) 0.0900(18) 0.0160(15) 0.0063(14) 0.0362(15) Cl78A 0.087(3) 0.075(2) 0.100(2) -0.0264(18) 0.0335(19) -0.0248(18) _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 N3 1.994(2) . ? Zn1 N21 2.006(3) . ? Zn1 N12 2.020(2) . ? Zn1 Cl2 2.2349(8) . ? N3 C7 1.338(4) . ? N3 N4 1.358(3) . ? N4 C5 1.345(4) . ? C5 C6 1.388(4) . ? C5 C8 1.513(4) . ? C6 C7 1.380(4) . ? C8 C9 1.535(5) . ? C8 C11 1.536(5) . ? C8 C10 1.537(4) . ? N12 C16 1.335(4) . ? N12 N13 1.355(3) . ? N13 C14 1.351(4) . ? C14 C15 1.383(5) . ? C14 C17 1.510(4) . ? C15 C16 1.388(4) . ? C17 C18 1.527(5) . ? C17 C20 1.528(5) . ? C17 C19 1.531(5) . ? N21 C25 1.331(4) . ? N21 N22 1.362(3) . ? N22 C23 1.344(4) . ? C23 C24 1.381(5) . ? C23 C26 1.510(4) . ? C24 C25 1.396(5) . ? C26 C29 1.522(5) . ? C26 C28 1.534(6) . ? C26 C27 1.540(6) . ? P30 F35 1.578(2) . ? P30 F34 1.581(3) . ? P30 F33 1.584(3) . ? P30 F31 1.590(3) . ? P30 F32 1.609(2) . ? P30 F36 1.613(2) . ? Zn37 N39 1.994(3) . ? Zn37 N48 2.009(2) . ? Zn37 N57 2.010(3) . ? Zn37 Cl38 2.2486(8) . ? N39 C43 1.332(4) . ? N39 N40 1.362(4) . ? N40 C41 1.349(4) . ? C41 C42 1.378(5) . ? C41 C44 1.510(4) . ? C42 C43 1.395(5) . ? C44 C45 1.530(5) . ? C44 C47 1.535(5) . ? C44 C46 1.535(5) . ? N48 C52 1.332(4) . ? N48 N49 1.357(3) . ? N49 C50 1.344(4) . ? C50 C51 1.377(5) . ? C50 C53 1.518(4) . ? C51 C52 1.388(5) . ? C53 C56 1.508(6) . ? C53 C55 1.535(6) . ? C53 C54 1.540(5) . ? N57 C61 1.328(5) . ? N57 N58 1.352(4) . ? N58 C59 1.346(4) . ? C59 C60 1.381(5) . ? C59 C62 1.514(5) . ? C60 C61 1.386(5) . ? C62 C65 1.532(5) . ? C62 C63 1.535(5) . ? C62 C64 1.539(5) . ? P66A F70A 1.498(9) . ? P66A F71A 1.530(9) . ? P66A F67A 1.581(7) . ? P66A F69A 1.629(8) . ? P66A F72A 1.661(9) . ? P66A F68A 1.760(8) . ? P66B F69B 1.543(9) . ? P66B F71B 1.557(9) . ? P66B F68B 1.584(8) . ? P66B F70B 1.598(9) . ? P66B F72B 1.632(10) . ? P66B F67B 1.676(8) . ? P66C F69C 1.516(10) . ? P66C F72C 1.531(9) . ? P66C F68C 1.600(7) . ? P66C F70C 1.650(8) . ? P66C F71C 1.659(9) . ? P66C F67C 1.663(11) . ? C73 Cl75B 1.749(7) . ? C73 Cl74 1.757(5) . ? C73 Cl75A 1.778(7) . ? Cl77A C76B 1.729(16) . ? Cl77A C76A 1.840(10) . ? C76A Cl78A 1.788(10) . ? C76B Cl78B 1.709(17) . ? Cl77C C76D 1.71(2) . ? Cl77C C76C 1.73(2) . ? C76C Cl78C 1.75(2) . ? C76D Cl78D 1.78(2) . ? 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 N3 Zn1 N21 107.92(10) . . ? N3 Zn1 N12 118.35(10) . . ? N21 Zn1 N12 102.26(10) . . ? N3 Zn1 Cl2 106.01(7) . . ? N21 Zn1 Cl2 119.62(8) . . ? N12 Zn1 Cl2 103.38(8) . . ? C7 N3 N4 105.1(2) . . ? C7 N3 Zn1 126.8(2) . . ? N4 N3 Zn1 126.06(19) . . ? C5 N4 N3 111.9(2) . . ? N4 C5 C6 106.1(3) . . ? N4 C5 C8 123.0(3) . . ? C6 C5 C8 130.9(3) . . ? C7 C6 C5 106.0(3) . . ? N3 C7 C6 110.8(3) . . ? C5 C8 C9 108.1(3) . . ? C5 C8 C11 108.9(2) . . ? C9 C8 C11 109.7(3) . . ? C5 C8 C10 110.6(2) . . ? C9 C8 C10 109.6(3) . . ? C11 C8 C10 109.9(3) . . ? C16 N12 N13 105.3(2) . . ? C16 N12 Zn1 127.1(2) . . ? N13 N12 Zn1 127.6(2) . . ? C14 N13 N12 111.9(2) . . ? N13 C14 C15 106.2(3) . . ? N13 C14 C17 121.7(3) . . ? C15 C14 C17 132.1(3) . . ? C14 C15 C16 105.8(3) . . ? N12 C16 C15 110.9(3) . . ? C14 C17 C18 108.9(3) . . ? C14 C17 C20 110.2(3) . . ? C18 C17 C20 109.7(4) . . ? C14 C17 C19 108.9(3) . . ? C18 C17 C19 110.3(3) . . ? C20 C17 C19 108.8(3) . . ? C25 N21 N22 105.6(3) . . ? C25 N21 Zn1 126.2(2) . . ? N22 N21 Zn1 127.8(2) . . ? C23 N22 N21 111.6(3) . . ? N22 C23 C24 106.5(3) . . ? N22 C23 C26 122.4(3) . . ? C24 C23 C26 131.1(3) . . ? C23 C24 C25 105.8(3) . . ? N21 C25 C24 110.4(3) . . ? C23 C26 C29 109.6(3) . . ? C23 C26 C28 108.7(3) . . ? C29 C26 C28 110.8(3) . . ? C23 C26 C27 108.8(3) . . ? C29 C26 C27 108.9(3) . . ? C28 C26 C27 109.9(4) . . ? F35 P30 F34 91.72(16) . . ? F35 P30 F33 91.31(17) . . ? F34 P30 F33 90.89(18) . . ? F35 P30 F31 90.37(15) . . ? F34 P30 F31 90.45(17) . . ? F33 P30 F31 177.82(16) . . ? F35 P30 F32 90.32(14) . . ? F34 P30 F32 177.86(15) . . ? F33 P30 F32 88.39(15) . . ? F31 P30 F32 90.21(14) . . ? F35 P30 F36 178.37(17) . . ? F34 P30 F36 89.52(15) . . ? F33 P30 F36 89.73(17) . . ? F31 P30 F36 88.56(15) . . ? F32 P30 F36 88.46(12) . . ? N39 Zn37 N48 119.07(11) . . ? N39 Zn37 N57 109.34(11) . . ? N48 Zn37 N57 106.31(11) . . ? N39 Zn37 Cl38 106.36(8) . . ? N48 Zn37 Cl38 106.34(8) . . ? N57 Zn37 Cl38 109.11(8) . . ? C43 N39 N40 105.5(3) . . ? C43 N39 Zn37 125.5(2) . . ? N40 N39 Zn37 127.5(2) . . ? C41 N40 N39 111.5(3) . . ? N40 C41 C42 106.6(3) . . ? N40 C41 C44 121.5(3) . . ? C42 C41 C44 131.9(3) . . ? C41 C42 C43 105.7(3) . . ? N39 C43 C42 110.7(3) . . ? C41 C44 C45 108.8(3) . . ? C41 C44 C47 109.0(3) . . ? C45 C44 C47 109.9(3) . . ? C41 C44 C46 110.0(3) . . ? C45 C44 C46 109.5(3) . . ? C47 C44 C46 109.6(3) . . ? C52 N48 N49 104.9(2) . . ? C52 N48 Zn37 126.1(2) . . ? N49 N48 Zn37 128.7(2) . . ? C50 N49 N48 112.2(3) . . ? N49 C50 C51 106.0(3) . . ? N49 C50 C53 122.3(3) . . ? C51 C50 C53 131.6(3) . . ? C50 C51 C52 106.1(3) . . ? N48 C52 C51 110.8(3) . . ? C56 C53 C50 110.4(3) . . ? C56 C53 C55 108.5(4) . . ? C50 C53 C55 110.7(3) . . ? C56 C53 C54 110.0(4) . . ? C50 C53 C54 110.5(3) . . ? C55 C53 C54 106.6(4) . . ? C61 N57 N58 105.5(3) . . ? C61 N57 Zn37 126.9(2) . . ? N58 N57 Zn37 127.5(2) . . ? C59 N58 N57 111.7(3) . . ? N58 C59 C60 106.2(3) . . ? N58 C59 C62 122.6(3) . . ? C60 C59 C62 131.2(3) . . ? C59 C60 C61 105.8(3) . . ? N57 C61 C60 110.7(3) . . ? C59 C62 C65 108.5(3) . . ? C59 C62 C63 108.1(3) . . ? C65 C62 C63 110.3(3) . . ? C59 C62 C64 110.6(3) . . ? C65 C62 C64 109.4(3) . . ? C63 C62 C64 109.9(3) . . ? F70A P66A F71A 94.7(6) . . ? F70A P66A F67A 92.4(5) . . ? F71A P66A F67A 91.2(5) . . ? F70A P66A F69A 96.5(6) . . ? F71A P66A F69A 90.2(6) . . ? F67A P66A F69A 170.9(6) . . ? F70A P66A F72A 97.8(6) . . ? F71A P66A F72A 167.3(6) . . ? F67A P66A F72A 90.6(5) . . ? F69A P66A F72A 86.1(5) . . ? F70A P66A F68A 174.9(7) . . ? F71A P66A F68A 90.3(5) . . ? F67A P66A F68A 88.4(4) . . ? F69A P66A F68A 82.6(5) . . ? F72A P66A F68A 77.2(5) . . ? F69B P66B F71B 91.3(6) . . ? F69B P66B F68B 96.1(5) . . ? F71B P66B F68B 89.0(5) . . ? F69B P66B F70B 86.9(6) . . ? F71B P66B F70B 96.1(6) . . ? F68B P66B F70B 174.0(7) . . ? F69B P66B F72B 93.6(7) . . ? F71B P66B F72B 174.8(7) . . ? F68B P66B F72B 92.3(6) . . ? F70B P66B F72B 82.3(6) . . ? F69B P66B F67B 179.2(7) . . ? F71B P66B F67B 88.3(5) . . ? F68B P66B F67B 84.5(4) . . ? F70B P66B F67B 92.5(5) . . ? F72B P66B F67B 86.8(6) . . ? F69C P66C F72C 99.1(7) . . ? F69C P66C F68C 89.2(6) . . ? F72C P66C F68C 92.5(5) . . ? F69C P66C F70C 99.3(6) . . ? F72C P66C F70C 88.4(5) . . ? F68C P66C F70C 171.2(6) . . ? F69C P66C F71C 87.0(7) . . ? F72C P66C F71C 173.8(7) . . ? F68C P66C F71C 87.3(5) . . ? F70C P66C F71C 90.9(5) . . ? F69C P66C F67C 172.0(8) . . ? F72C P66C F67C 87.8(7) . . ? F68C P66C F67C 86.4(7) . . ? F70C P66C F67C 84.9(7) . . ? F71C P66C F67C 86.0(7) . . ? Cl75B C73 Cl74 111.4(3) . . ? Cl74 C73 Cl75A 111.9(3) . . ? Cl78A C76A Cl77A 103.5(5) . . ? Cl78B C76B Cl77A 109.6(11) . . ? Cl77C C76C Cl78C 99.9(13) . . ? Cl77C C76D Cl78D 120.1(19) . . ? 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 F32 0.88 2.09 2.942(3) 163.4 . N13 H13 F31 0.88 2.44 3.196(4) 144.6 . N13 H13 F36 0.88 2.18 2.976(4) 150.9 . N22 H22 Cl38 0.88 2.40 3.277(3) 174.0 . N40 H40 F67A 0.88 2.08 2.955(7) 174.4 . N40 H40 F68A 0.88 2.60 3.191(9) 125.0 . N40 H40 F67B 0.88 2.32 3.185(8) 169.2 . N40 H40 F68B 0.88 2.34 2.985(8) 129.9 . N40 H40 F67C 0.88 2.58 3.438(19) 165.0 . N40 H40 F68C 0.88 2.25 2.855(8) 125.6 . N49 H49 F68A 0.88 2.06 2.904(8) 160.5 . N49 H49 F68B 0.88 2.17 2.844(8) 133.4 . N49 H49 F68C 0.88 2.06 2.828(8) 145.3 . N58 H58 Cl2 0.88 2.41 3.215(3) 151.6 . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.112 _refine_diff_density_min -1.148 _refine_diff_density_rms 0.131