Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global #==================================================================== _journal_coden_Cambridge 182 # 1. SUBMISSION DETAILS _publ_contact_author '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 malcolmh@chem.leeds.ac.uk _publ_requested_journal 'Chemical Communications' _publ_contact_letter ; The following data are for three structures included in a manuscript we have just submitted to the Chemical Communications office. ; #======================================================================= # 2. TITLE AND AUTHOR LIST _publ_section_title ; 3{5}-Tertbutylpyrazole is a Ditopic Receptor for Zinc(II) Halides. ; loop_ _publ_author_name _publ_author_address 'Xiaoming Liu' ; School of Chemistry, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, UK ; 'Colin A. Kilner' ; School 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 ; #================================================================= data_mh87 _database_code_CSD 177939 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Chloro-tris[5-tertbutylpyrazole]zinc(II) chloride hemipentane solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H36 Cl N6 Zn, Cl, 0.5[C5 H12]' _chemical_formula_sum 'C23.50 H42 Cl2 N6 Zn' _chemical_formula_weight 544.90 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M '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 17.1001(3) _cell_length_b 10.7850(2) _cell_length_c 17.9314(3) _cell_angle_alpha 90.00 _cell_angle_beta 115.1510(7) _cell_angle_gamma 90.00 _cell_volume 2993.46(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 54618 _cell_measurement_theta_min 2.88 _cell_measurement_theta_max 27.48 _exptl_crystal_description Lath _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.209 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1156 _exptl_absorpt_coefficient_mu 1.020 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6192 _exptl_absorpt_correction_T_max 0.7296 _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 54618 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.0264 _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 -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6848 _reflns_number_gt 5766 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The asymmetric unit contains one complex cation, one chloride anion, and half a molecule of pentane disordered about the crystallographic inversion centre at 0.5, 0.5, 0.5. The central C atom C33 of the solvent lies near, but not on, the special position. The tertbutyl group C8-C11 is disordered over two equally occupied orientations, labelled 'A' and 'B'. All disordered C-C bonds within the solvent molecule were restrained to 1.53(2)\%A, and 1,3-C...C distances to 2.50(2)\%A. All wholly occupied non-H atoms were refined anisotropically. ; _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^)+(0.0499P)^2^+2.5869P] 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 6848 _refine_ls_number_parameters 288 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.0508 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.1096 _refine_ls_wR_factor_gt 0.1006 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.078 _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 0.286549(15) -0.04210(2) 0.352019(15) 0.02756(9) Uani 1 1 d . . . Cl2 Cl 0.34377(4) 0.05174(6) 0.47376(3) 0.03912(14) Uani 1 1 d . . . N3 N 0.19460(11) -0.15508(17) 0.35434(11) 0.0302(4) Uani 1 1 d . A . N4 N 0.14478(11) -0.23524(16) 0.29470(11) 0.0293(4) Uani 1 1 d . A . H4 H 0.1428 -0.2382 0.2449 0.035 Uiso 1 1 calc R . . C5 C 0.09870(13) -0.3098(2) 0.32141(14) 0.0317(5) Uani 1 1 d D . . C6 C 0.12003(15) -0.2771(2) 0.40230(15) 0.0383(5) Uani 1 1 d . A . H6 H 0.0986 -0.3129 0.4384 0.046 Uiso 1 1 calc R . . C7 C 0.17929(15) -0.1810(2) 0.41986(15) 0.0368(5) Uani 1 1 d . . . H7 H 0.2054 -0.1394 0.4713 0.044 Uiso 1 1 calc R A . C8A C 0.0351(5) -0.4033(7) 0.2592(5) 0.034(2) Uiso 0.50 1 d PD A 1 C9A C 0.0243(5) -0.5066(7) 0.3153(5) 0.062(2) Uiso 0.50 1 d PD A 1 H9A1 H -0.0117 -0.5737 0.2808 0.092 Uiso 0.50 1 calc PR A 1 H9A2 H -0.0035 -0.4714 0.3484 0.092 Uiso 0.50 1 calc PR A 1 H9A3 H 0.0812 -0.5394 0.3519 0.092 Uiso 0.50 1 calc PR A 1 C10A C 0.0639(4) -0.4563(6) 0.2007(4) 0.0551(15) Uiso 0.50 1 d PD A 1 H10A H 0.0695 -0.3905 0.1656 0.083 Uiso 0.50 1 calc PR A 1 H10B H 0.0217 -0.5177 0.1664 0.083 Uiso 0.50 1 calc PR A 1 H10C H 0.1201 -0.4966 0.2306 0.083 Uiso 0.50 1 calc PR A 1 C11A C -0.0537(3) -0.3387(5) 0.2165(3) 0.0341(10) Uiso 0.50 1 d PD A 1 H11A H -0.0498 -0.2706 0.1821 0.051 Uiso 0.50 1 calc PR A 1 H11B H -0.0708 -0.3058 0.2583 0.051 Uiso 0.50 1 calc PR A 1 H11C H -0.0969 -0.3988 0.1820 0.051 Uiso 0.50 1 calc PR A 1 C8B C 0.0375(4) -0.4075(7) 0.2729(5) 0.032(2) Uiso 0.50 1 d PD A 2 C9B C 0.0027(4) -0.4851(6) 0.3207(4) 0.0408(13) Uiso 0.50 1 d PD A 2 H9B1 H 0.0508 -0.5205 0.3688 0.061 Uiso 0.50 1 calc PR A 2 H9B2 H -0.0325 -0.5523 0.2857 0.061 Uiso 0.50 1 calc PR A 2 H9B3 H -0.0330 -0.4337 0.3391 0.061 Uiso 0.50 1 calc PR A 2 C10B C 0.0863(4) -0.4936(6) 0.2356(4) 0.0500(13) Uiso 0.50 1 d PD A 2 H10D H 0.1145 -0.4423 0.2090 0.075 Uiso 0.50 1 calc PR A 2 H10E H 0.0449 -0.5495 0.1948 0.075 Uiso 0.50 1 calc PR A 2 H10F H 0.1300 -0.5425 0.2798 0.075 Uiso 0.50 1 calc PR A 2 C11B C -0.0365(4) -0.3468(6) 0.1971(4) 0.0563(17) Uiso 0.50 1 d PD A 2 H11D H -0.0706 -0.2925 0.2158 0.084 Uiso 0.50 1 calc PR A 2 H11E H -0.0738 -0.4117 0.1614 0.084 Uiso 0.50 1 calc PR A 2 H11F H -0.0117 -0.2979 0.1663 0.084 Uiso 0.50 1 calc PR A 2 N12 N 0.37698(11) -0.14685(16) 0.33964(11) 0.0281(4) Uani 1 1 d . . . N13 N 0.36920(12) -0.21393(17) 0.27285(11) 0.0298(4) Uani 1 1 d . . . H13 H 0.3214 -0.2197 0.2272 0.036 Uiso 1 1 calc R . . C14 C 0.44406(14) -0.2706(2) 0.28535(14) 0.0315(4) Uani 1 1 d . . . C15 C 0.50304(14) -0.2377(2) 0.36338(15) 0.0347(5) Uani 1 1 d . . . H15 H 0.5619 -0.2621 0.3903 0.042 Uiso 1 1 calc R . . C16 C 0.45850(13) -0.1614(2) 0.39455(14) 0.0308(4) Uani 1 1 d . . . H16 H 0.4829 -0.1247 0.4477 0.037 Uiso 1 1 calc R . . C17 C 0.45176(17) -0.3518(2) 0.21983(17) 0.0407(6) Uani 1 1 d . . . C18 C 0.3858(2) -0.4572(2) 0.19776(19) 0.0491(7) Uani 1 1 d . . . H18A H 0.3973 -0.5073 0.2469 0.074 Uiso 1 1 calc R . . H18B H 0.3904 -0.5093 0.1551 0.074 Uiso 1 1 calc R . . H18C H 0.3274 -0.4223 0.1772 0.074 Uiso 1 1 calc R . . C19 C 0.4343(3) -0.2748(3) 0.1431(2) 0.0719(10) Uani 1 1 d . . . H19A H 0.3769 -0.2370 0.1234 0.108 Uiso 1 1 calc R . . H19B H 0.4367 -0.3284 0.1000 0.108 Uiso 1 1 calc R . . H19C H 0.4781 -0.2096 0.1565 0.108 Uiso 1 1 calc R . . C20 C 0.5432(2) -0.4083(3) 0.2551(2) 0.0669(9) Uani 1 1 d . . . H20A H 0.5861 -0.3417 0.2703 0.100 Uiso 1 1 calc R . . H20B H 0.5490 -0.4615 0.2134 0.100 Uiso 1 1 calc R . . H20C H 0.5525 -0.4578 0.3040 0.100 Uiso 1 1 calc R . . N21 N 0.25111(12) 0.09690(18) 0.27042(11) 0.0319(4) Uani 1 1 d . . . N22 N 0.21303(12) 0.09214(18) 0.18654(11) 0.0325(4) Uani 1 1 d . . . H22 H 0.1963 0.0231 0.1579 0.039 Uiso 1 1 calc R . . C23 C 0.20399(14) 0.2057(2) 0.15267(15) 0.0350(5) Uani 1 1 d . . . C24 C 0.23839(16) 0.2883(2) 0.21751(16) 0.0404(5) Uani 1 1 d . . . H24 H 0.2420 0.3758 0.2141 0.048 Uiso 1 1 calc R . . C25 C 0.26661(16) 0.2173(2) 0.28859(15) 0.0370(5) Uani 1 1 d . . . H25 H 0.2934 0.2498 0.3429 0.044 Uiso 1 1 calc R . . C26 C 0.16286(16) 0.2253(3) 0.06047(15) 0.0422(6) Uani 1 1 d . . . C27 C 0.2159(2) 0.1589(4) 0.02242(19) 0.0645(9) Uani 1 1 d . . . H27A H 0.2752 0.1909 0.0469 0.097 Uiso 1 1 calc R . . H27B H 0.1900 0.1735 -0.0372 0.097 Uiso 1 1 calc R . . H27C H 0.2166 0.0697 0.0331 0.097 Uiso 1 1 calc R . . C28 C 0.07105(18) 0.1726(4) 0.02428(18) 0.0599(8) Uani 1 1 d . . . H28A H 0.0438 0.1862 -0.0354 0.090 Uiso 1 1 calc R . . H28B H 0.0373 0.2142 0.0494 0.090 Uiso 1 1 calc R . . H28C H 0.0733 0.0834 0.0356 0.090 Uiso 1 1 calc R . . C29 C 0.1609(3) 0.3648(3) 0.0426(2) 0.0689(9) Uani 1 1 d . . . H29A H 0.2201 0.3970 0.0650 0.103 Uiso 1 1 calc R . . H29B H 0.1283 0.4080 0.0684 0.103 Uiso 1 1 calc R . . H29C H 0.1330 0.3785 -0.0171 0.103 Uiso 1 1 calc R . . Cl30 Cl 0.17795(4) -0.18698(6) 0.13828(3) 0.03801(14) Uani 1 1 d . . . C31 C 0.3273(4) 0.5302(7) 0.4061(5) 0.0656(18) Uiso 0.50 1 d PD B 2 H31A H 0.3338 0.5622 0.3579 0.098 Uiso 0.50 1 calc PR B 2 H31B H 0.2794 0.5729 0.4114 0.098 Uiso 0.50 1 calc PR B 2 H31C H 0.3154 0.4410 0.3994 0.098 Uiso 0.50 1 calc PR B 2 C32 C 0.4110(4) 0.5528(6) 0.4838(4) 0.0583(15) Uiso 0.50 1 d PD B 2 H32A H 0.4226 0.6431 0.4901 0.070 Uiso 0.50 1 calc PR B 2 H32B H 0.4030 0.5238 0.5325 0.070 Uiso 0.50 1 calc PR B 2 C33 C 0.4878(3) 0.4882(6) 0.4818(3) 0.0523(14) Uiso 0.50 1 d PD B 2 H33A H 0.4917 0.5092 0.4297 0.063 Uiso 0.50 1 calc PR B 2 H33B H 0.4795 0.3975 0.4825 0.063 Uiso 0.50 1 calc PR B 2 C34 C 0.5722(4) 0.5237(8) 0.5540(5) 0.078(2) Uiso 0.50 1 d PD B 2 H34A H 0.5674 0.5072 0.6063 0.094 Uiso 0.50 1 calc PR B 2 H34B H 0.5827 0.6135 0.5515 0.094 Uiso 0.50 1 calc PR B 2 C35 C 0.6481(5) 0.4509(9) 0.5530(6) 0.086(3) Uiso 0.50 1 d PD B 2 H35A H 0.6409 0.3626 0.5615 0.129 Uiso 0.50 1 calc PR B 2 H35B H 0.7020 0.4809 0.5972 0.129 Uiso 0.50 1 calc PR B 2 H35C H 0.6504 0.4623 0.4998 0.129 Uiso 0.50 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02373(13) 0.02717(14) 0.02972(14) -0.00456(9) 0.00937(10) -0.00238(9) Cl2 0.0366(3) 0.0444(3) 0.0312(3) -0.0119(2) 0.0095(2) -0.0062(2) N3 0.0261(9) 0.0303(9) 0.0321(9) -0.0047(7) 0.0104(7) -0.0044(7) N4 0.0272(9) 0.0270(9) 0.0314(9) -0.0027(7) 0.0102(7) -0.0030(7) C5 0.0258(10) 0.0265(10) 0.0421(12) 0.0013(9) 0.0138(9) 0.0012(8) C6 0.0367(12) 0.0422(13) 0.0402(12) -0.0017(10) 0.0203(10) -0.0050(10) C7 0.0343(11) 0.0422(13) 0.0353(12) -0.0056(10) 0.0161(10) -0.0053(10) N12 0.0259(8) 0.0275(9) 0.0294(9) -0.0052(7) 0.0103(7) -0.0030(7) N13 0.0287(9) 0.0296(9) 0.0299(9) -0.0072(7) 0.0112(7) -0.0034(7) C14 0.0324(11) 0.0256(10) 0.0409(12) -0.0044(9) 0.0197(9) -0.0035(8) C15 0.0264(10) 0.0308(11) 0.0447(13) -0.0025(9) 0.0131(9) 0.0014(8) C16 0.0263(10) 0.0305(11) 0.0322(11) -0.0019(8) 0.0091(9) -0.0019(8) C17 0.0478(14) 0.0332(12) 0.0504(14) -0.0132(10) 0.0297(12) -0.0074(10) C18 0.0580(17) 0.0373(13) 0.0570(17) -0.0188(12) 0.0294(14) -0.0113(12) C19 0.126(3) 0.0511(17) 0.064(2) -0.0106(15) 0.066(2) -0.0112(19) C20 0.0535(17) 0.064(2) 0.093(3) -0.0343(19) 0.0406(18) -0.0031(15) N21 0.0297(9) 0.0317(9) 0.0308(9) -0.0029(7) 0.0095(7) -0.0012(7) N22 0.0308(9) 0.0338(10) 0.0295(9) -0.0037(8) 0.0096(8) -0.0035(8) C23 0.0288(10) 0.0372(12) 0.0388(12) 0.0031(9) 0.0140(9) -0.0029(9) C24 0.0428(13) 0.0318(12) 0.0459(14) 0.0004(10) 0.0182(11) -0.0030(10) C25 0.0407(12) 0.0304(11) 0.0382(12) -0.0055(9) 0.0153(10) -0.0026(9) C26 0.0376(12) 0.0505(15) 0.0366(12) 0.0067(11) 0.0139(10) -0.0054(11) C27 0.0536(17) 0.098(3) 0.0442(16) -0.0029(16) 0.0231(14) -0.0029(17) C28 0.0372(14) 0.091(2) 0.0413(15) 0.0108(15) 0.0072(12) -0.0129(15) C29 0.090(2) 0.0588(19) 0.0473(17) 0.0152(15) 0.0194(17) -0.0076(18) Cl30 0.0374(3) 0.0415(3) 0.0293(3) -0.0073(2) 0.0085(2) -0.0052(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N21 2.0005(19) . ? Zn1 N12 2.0022(18) . ? Zn1 N3 2.0036(18) . ? Zn1 Cl2 2.2208(6) . ? N3 C7 1.337(3) . ? N3 N4 1.357(2) . ? N4 C5 1.348(3) . ? C5 C6 1.383(3) . ? C5 C8B 1.479(7) . ? C5 C8A 1.553(7) . ? C6 C7 1.389(3) . ? C8A C10A 1.453(9) . ? C8A C11A 1.546(8) . ? C8A C9A 1.564(9) . ? C8B C9B 1.491(9) . ? C8B C11B 1.554(9) . ? C8B C10B 1.576(9) . ? N12 C16 1.331(3) . ? N12 N13 1.356(2) . ? N13 C14 1.349(3) . ? C14 C15 1.379(3) . ? C14 C17 1.515(3) . ? C15 C16 1.390(3) . ? C17 C19 1.524(4) . ? C17 C18 1.531(3) . ? C17 C20 1.541(4) . ? N21 C25 1.337(3) . ? N21 N22 1.362(3) . ? N22 C23 1.347(3) . ? C23 C24 1.382(3) . ? C23 C26 1.511(3) . ? C24 C25 1.386(4) . ? C26 C27 1.525(4) . ? C26 C28 1.531(4) . ? C26 C29 1.536(4) . ? C31 C32 1.534(7) . ? C32 C33 1.501(7) . ? C33 C34 1.522(7) . ? C34 C35 1.524(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N21 Zn1 N12 110.48(8) . . ? N21 Zn1 N3 118.32(8) . . ? N12 Zn1 N3 108.00(7) . . ? N21 Zn1 Cl2 104.32(6) . . ? N12 Zn1 Cl2 109.13(5) . . ? N3 Zn1 Cl2 106.17(6) . . ? C7 N3 N4 105.51(18) . . ? C7 N3 Zn1 126.42(15) . . ? N4 N3 Zn1 127.32(14) . . ? C5 N4 N3 111.47(18) . . ? N4 C5 C6 106.67(19) . . ? N4 C5 C8B 126.2(3) . . ? C6 C5 C8B 127.1(3) . . ? N4 C5 C8A 118.0(3) . . ? C6 C5 C8A 135.3(3) . . ? C8B C5 C8A 8.5(4) . . ? C5 C6 C7 105.7(2) . . ? N3 C7 C6 110.7(2) . . ? C10A C8A C11A 112.5(6) . . ? C10A C8A C5 115.1(5) . . ? C11A C8A C5 107.7(5) . . ? C10A C8A C9A 110.7(6) . . ? C11A C8A C9A 106.3(6) . . ? C5 C8A C9A 103.8(5) . . ? C5 C8B C9B 114.7(5) . . ? C5 C8B C11B 108.9(5) . . ? C9B C8B C11B 111.4(6) . . ? C5 C8B C10B 107.4(5) . . ? C9B C8B C10B 109.0(6) . . ? C11B C8B C10B 104.9(6) . . ? C16 N12 N13 105.61(17) . . ? C16 N12 Zn1 126.89(15) . . ? N13 N12 Zn1 127.46(13) . . ? C14 N13 N12 111.41(17) . . ? N13 C14 C15 106.57(19) . . ? N13 C14 C17 121.5(2) . . ? C15 C14 C17 132.0(2) . . ? C14 C15 C16 105.72(19) . . ? N12 C16 C15 110.7(2) . . ? C14 C17 C19 109.7(2) . . ? C14 C17 C18 109.4(2) . . ? C19 C17 C18 109.3(3) . . ? C14 C17 C20 108.5(2) . . ? C19 C17 C20 111.2(3) . . ? C18 C17 C20 108.6(2) . . ? C25 N21 N22 104.94(19) . . ? C25 N21 Zn1 125.61(16) . . ? N22 N21 Zn1 129.29(15) . . ? C23 N22 N21 111.90(19) . . ? N22 C23 C24 106.3(2) . . ? N22 C23 C26 122.1(2) . . ? C24 C23 C26 131.6(2) . . ? C23 C24 C25 106.0(2) . . ? N21 C25 C24 110.9(2) . . ? C23 C26 C27 109.6(2) . . ? C23 C26 C28 109.2(2) . . ? C27 C26 C28 109.5(3) . . ? C23 C26 C29 108.9(2) . . ? C27 C26 C29 109.3(3) . . ? C28 C26 C29 110.4(3) . . ? C33 C32 C31 113.1(5) . . ? C32 C33 C34 112.7(5) . . ? C33 C34 C35 111.4(6) . . ? 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 0.88 2.30 3.132(2) 157.5 . N13 H13 Cl30 0.88 2.31 3.1455(19) 157.5 . N22 H22 Cl30 0.88 2.29 3.119(2) 156.1 . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.673 _refine_diff_density_min -0.584 _refine_diff_density_rms 0.068 #=END data_xl1108b _database_code_CSD 177940 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bromo-tris[5-tertbutylpyrazole]zinc(II) bromide hemipentane solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H36 Br N6 Zn, Br, 0.5[C5 H12]' _chemical_formula_sum 'C23.50 H42 Br2 N6 Zn' _chemical_formula_weight 633.82 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' 'Br' 'Br' -0.2901 2.4595 '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 17.3353(2) _cell_length_b 10.5568(2) _cell_length_c 18.4428(2) _cell_angle_alpha 90.00 _cell_angle_beta 114.9379(9) _cell_angle_gamma 90.00 _cell_volume 3060.45(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 38904 _cell_measurement_theta_min 3.61 _cell_measurement_theta_max 27.48 _exptl_crystal_description Lath _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.376 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1300 _exptl_absorpt_coefficient_mu 3.434 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4256 _exptl_absorpt_correction_T_max 0.5325 _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 38904 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.0323 _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 -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.61 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7008 _reflns_number_gt 5705 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The asymmetric unit contains one complex cation, one bromide anion, and half a molecule of pentane disordered about the crystallographic inversion centre at 0.5, 0.5, 0.5. The central C atom C33 of the solvent lies near, but not on, the special position. All C-C bonds within the solvent molecule were restrained to 1.53(2)\%A, and 1,3-C...C distances to 2.50(2)\%A. All wholly occupied non-H atoms were refined anisotropically. ; _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^)+(0.0382P)^2^+1.6460P] 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 7008 _refine_ls_number_parameters 292 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0442 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0798 _refine_ls_wR_factor_gt 0.0733 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.020 _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 0.285031(15) -0.04897(2) 0.346956(15) 0.02919(7) Uani 1 1 d . A 1 Br2 Br 0.344349(16) 0.05561(2) 0.471339(14) 0.04069(8) Uani 1 1 d . A 1 N3 N 0.19428(11) -0.16347(18) 0.34999(11) 0.0316(4) Uani 1 1 d . A 1 N4 N 0.14540(11) -0.24647(17) 0.29309(11) 0.0303(4) Uani 1 1 d . A 1 H4 H 0.1454 -0.2530 0.2455 0.036 Uiso 1 1 calc R A 1 C5 C 0.09668(14) -0.3180(2) 0.31809(13) 0.0323(5) Uani 1 1 d . A 1 C6 C 0.11581(16) -0.2791(2) 0.39558(15) 0.0392(5) Uani 1 1 d . A 1 H6 H 0.0923 -0.3110 0.4301 0.047 Uiso 1 1 calc R A 1 C7 C 0.17619(15) -0.1844(2) 0.41248(14) 0.0371(5) Uani 1 1 d . A 1 H7 H 0.2013 -0.1403 0.4619 0.045 Uiso 1 1 calc R A 1 C8 C 0.03642(16) -0.4165(2) 0.26520(15) 0.0387(5) Uani 1 1 d . A 1 C9 C -0.0035(2) -0.4869(3) 0.3126(2) 0.0715(10) Uani 1 1 d . A 1 H9A H -0.0375 -0.5578 0.2808 0.107 Uiso 1 1 calc R A 1 H9B H -0.0402 -0.4290 0.3254 0.107 Uiso 1 1 calc R A 1 H9C H 0.0414 -0.5193 0.3623 0.107 Uiso 1 1 calc R A 1 C10 C 0.0860(3) -0.5105(4) 0.2393(3) 0.0848(13) Uani 1 1 d . A 1 H10A H 0.0467 -0.5721 0.2023 0.127 Uiso 1 1 calc R A 1 H10B H 0.1273 -0.5549 0.2863 0.127 Uiso 1 1 calc R A 1 H10C H 0.1160 -0.4654 0.2125 0.127 Uiso 1 1 calc R A 1 C11 C -0.0328(3) -0.3548(3) 0.1938(2) 0.0958(16) Uani 1 1 d . A 1 H11A H -0.0074 -0.3090 0.1630 0.144 Uiso 1 1 calc R A 1 H11B H -0.0644 -0.2953 0.2119 0.144 Uiso 1 1 calc R A 1 H11C H -0.0717 -0.4199 0.1600 0.144 Uiso 1 1 calc R A 1 N12 N 0.37546(11) -0.15530(17) 0.33665(10) 0.0291(4) Uani 1 1 d . A 1 N13 N 0.37089(12) -0.22350(17) 0.27220(11) 0.0302(4) Uani 1 1 d . A 1 H13 H 0.3247 -0.2308 0.2273 0.036 Uiso 1 1 calc R A 1 C14 C 0.44617(14) -0.2785(2) 0.28597(14) 0.0311(5) Uani 1 1 d . A 1 C15 C 0.50158(15) -0.2443(2) 0.36218(14) 0.0338(5) Uani 1 1 d . A 1 H15 H 0.5597 -0.2678 0.3895 0.041 Uiso 1 1 calc R A 1 C16 C 0.45548(13) -0.1685(2) 0.39128(13) 0.0311(5) Uani 1 1 d . A 1 H16 H 0.4778 -0.1311 0.4430 0.037 Uiso 1 1 calc R A 1 C17 C 0.45642(16) -0.3608(2) 0.22339(15) 0.0396(5) Uani 1 1 d . A 1 C18 C 0.39285(18) -0.4699(2) 0.20117(17) 0.0474(6) Uani 1 1 d . A 1 H18A H 0.4032 -0.5206 0.2489 0.071 Uiso 1 1 calc R A 1 H18B H 0.3997 -0.5233 0.1608 0.071 Uiso 1 1 calc R A 1 H18C H 0.3349 -0.4359 0.1795 0.071 Uiso 1 1 calc R A 1 C19 C 0.4402(2) -0.2814(3) 0.14887(18) 0.0616(9) Uani 1 1 d . A 1 H19A H 0.3834 -0.2436 0.1290 0.092 Uiso 1 1 calc R A 1 H19B H 0.4439 -0.3357 0.1074 0.092 Uiso 1 1 calc R A 1 H19C H 0.4830 -0.2141 0.1625 0.092 Uiso 1 1 calc R A 1 C20 C 0.54761(18) -0.4133(3) 0.2589(2) 0.0597(8) Uani 1 1 d . A 1 H20A H 0.5882 -0.3428 0.2731 0.089 Uiso 1 1 calc R A 1 H20B H 0.5554 -0.4674 0.2193 0.089 Uiso 1 1 calc R A 1 H20C H 0.5574 -0.4630 0.3068 0.089 Uiso 1 1 calc R A 1 N21 N 0.24929(12) 0.09071(18) 0.26540(11) 0.0329(4) Uani 1 1 d . A 1 N22 N 0.21313(12) 0.08397(19) 0.18447(11) 0.0343(4) Uani 1 1 d . A 1 H22 H 0.1975 0.0128 0.1573 0.041 Uiso 1 1 calc R A 1 C23 C 0.20388(14) 0.1994(2) 0.15045(14) 0.0367(5) Uani 1 1 d . A 1 C24 C 0.23601(17) 0.2842(2) 0.21261(16) 0.0418(6) Uani 1 1 d . A 1 H24 H 0.2392 0.3736 0.2086 0.050 Uiso 1 1 calc R A 1 C25 C 0.26277(16) 0.2138(2) 0.28207(15) 0.0393(5) Uani 1 1 d . A 1 H25 H 0.2874 0.2483 0.3345 0.047 Uiso 1 1 calc R A 1 C26 C 0.16351(17) 0.2177(3) 0.06078(15) 0.0452(6) Uani 1 1 d . A 1 C27 C 0.2157(2) 0.1467(4) 0.02437(18) 0.0667(9) Uani 1 1 d . A 1 H27A H 0.2744 0.1778 0.0482 0.100 Uiso 1 1 calc R A 1 H27B H 0.1908 0.1610 -0.0335 0.100 Uiso 1 1 calc R A 1 H27C H 0.2152 0.0559 0.0351 0.100 Uiso 1 1 calc R A 1 C28 C 0.07277(18) 0.1658(4) 0.02615(17) 0.0648(9) Uani 1 1 d . A 1 H28A H 0.0462 0.1790 -0.0319 0.097 Uiso 1 1 calc R A 1 H28B H 0.0398 0.2102 0.0504 0.097 Uiso 1 1 calc R A 1 H28C H 0.0741 0.0750 0.0377 0.097 Uiso 1 1 calc R A 1 C29 C 0.1632(2) 0.3594(3) 0.0429(2) 0.0717(10) Uani 1 1 d . A 1 H29A H 0.2218 0.3910 0.0652 0.108 Uiso 1 1 calc R A 1 H29B H 0.1308 0.4051 0.0672 0.108 Uiso 1 1 calc R A 1 H29C H 0.1368 0.3728 -0.0151 0.108 Uiso 1 1 calc R A 1 Br30 Br 0.175708(15) -0.21439(2) 0.129439(13) 0.03910(8) Uani 1 1 d . B 1 C31 C 0.3328(4) 0.5243(7) 0.4134(4) 0.0609(17) Uiso 0.50 1 d PD C 2 H31A H 0.3384 0.5553 0.3657 0.091 Uiso 0.50 1 calc PR C 2 H31B H 0.2854 0.5680 0.4185 0.091 Uiso 0.50 1 calc PR C 2 H31C H 0.3217 0.4330 0.4083 0.091 Uiso 0.50 1 calc PR C 2 C32 C 0.4147(4) 0.5502(6) 0.4871(4) 0.0633(17) Uiso 0.50 1 d PD C 2 H32A H 0.4252 0.6426 0.4922 0.076 Uiso 0.50 1 calc PR C 2 H32B H 0.4081 0.5210 0.5352 0.076 Uiso 0.50 1 calc PR C 2 C33 C 0.4897(3) 0.4850(7) 0.4833(3) 0.0545(15) Uiso 0.50 1 d PD C 2 H33A H 0.4924 0.5067 0.4322 0.065 Uiso 0.50 1 calc PR C 2 H33B H 0.4821 0.3922 0.4842 0.065 Uiso 0.50 1 calc PR C 2 C34 C 0.5725(4) 0.5220(8) 0.5519(4) 0.079(2) Uiso 0.50 1 d PD C 2 H34A H 0.5695 0.5027 0.6032 0.095 Uiso 0.50 1 calc PR C 2 H34B H 0.5816 0.6143 0.5499 0.095 Uiso 0.50 1 calc PR C 2 C35 C 0.6468(6) 0.4505(10) 0.5475(7) 0.102(3) Uiso 0.50 1 d PD C 2 H35A H 0.6412 0.3599 0.5559 0.153 Uiso 0.50 1 calc PR C 2 H35B H 0.7003 0.4821 0.5889 0.153 Uiso 0.50 1 calc PR C 2 H35C H 0.6465 0.4634 0.4947 0.153 Uiso 0.50 1 calc PR C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02500(13) 0.03203(14) 0.02929(14) -0.00366(10) 0.01023(10) -0.00162(10) Br2 0.03758(14) 0.04867(15) 0.03154(13) -0.01193(10) 0.01041(10) -0.00474(10) N3 0.0266(9) 0.0362(10) 0.0307(9) -0.0045(8) 0.0108(7) -0.0024(8) N4 0.0290(9) 0.0313(10) 0.0289(9) -0.0030(7) 0.0106(7) -0.0029(7) C5 0.0277(11) 0.0322(11) 0.0360(12) 0.0019(9) 0.0126(9) 0.0013(9) C6 0.0361(13) 0.0476(14) 0.0385(12) -0.0011(11) 0.0202(10) -0.0060(11) C7 0.0338(12) 0.0460(14) 0.0334(12) -0.0053(10) 0.0159(10) -0.0046(10) C8 0.0377(13) 0.0325(12) 0.0434(13) -0.0017(10) 0.0145(11) -0.0059(10) C9 0.078(2) 0.071(2) 0.070(2) -0.0155(17) 0.0359(18) -0.0444(19) C10 0.087(3) 0.061(2) 0.128(3) -0.048(2) 0.067(3) -0.027(2) C11 0.092(3) 0.0517(19) 0.073(2) 0.0079(17) -0.034(2) -0.0275(19) N12 0.0281(9) 0.0310(9) 0.0281(9) -0.0036(7) 0.0115(7) -0.0017(7) N13 0.0285(9) 0.0327(10) 0.0288(9) -0.0048(7) 0.0114(7) -0.0017(7) C14 0.0321(11) 0.0254(10) 0.0401(12) -0.0012(9) 0.0194(9) -0.0031(9) C15 0.0285(11) 0.0316(11) 0.0394(12) -0.0007(9) 0.0125(9) 0.0013(9) C16 0.0283(11) 0.0326(11) 0.0310(11) -0.0010(9) 0.0111(9) -0.0014(9) C17 0.0439(14) 0.0344(12) 0.0480(14) -0.0106(10) 0.0268(11) -0.0035(10) C18 0.0512(16) 0.0375(14) 0.0554(16) -0.0152(11) 0.0242(13) -0.0065(12) C19 0.101(3) 0.0498(17) 0.0532(17) -0.0095(13) 0.0512(18) -0.0090(16) C20 0.0448(16) 0.0589(18) 0.082(2) -0.0261(16) 0.0336(15) 0.0005(13) N21 0.0303(10) 0.0358(10) 0.0309(9) -0.0023(8) 0.0112(8) -0.0013(8) N22 0.0326(10) 0.0385(11) 0.0299(10) -0.0031(8) 0.0113(8) -0.0046(8) C23 0.0275(11) 0.0453(14) 0.0388(12) 0.0045(10) 0.0154(10) -0.0007(10) C24 0.0450(14) 0.0335(13) 0.0470(14) 0.0007(10) 0.0195(11) 0.0002(11) C25 0.0443(14) 0.0349(13) 0.0368(12) -0.0049(10) 0.0152(11) -0.0001(10) C26 0.0402(14) 0.0582(17) 0.0365(13) 0.0088(11) 0.0155(11) -0.0057(12) C27 0.065(2) 0.098(3) 0.0433(16) 0.0001(16) 0.0292(15) 0.0000(19) C28 0.0405(15) 0.102(3) 0.0403(15) 0.0158(16) 0.0053(12) -0.0142(16) C29 0.088(2) 0.069(2) 0.0505(18) 0.0187(16) 0.0210(17) -0.0063(19) Br30 0.03696(13) 0.04768(15) 0.02837(12) -0.00640(9) 0.00959(9) -0.00502(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N12 2.0013(18) . ? Zn1 N3 2.0034(19) . ? Zn1 N21 2.0087(19) . ? Zn1 Br2 2.3557(3) . ? N3 C7 1.334(3) . ? N3 N4 1.355(2) . ? N4 C5 1.351(3) . ? C5 C6 1.386(3) . ? C5 C8 1.505(3) . ? C6 C7 1.385(3) . ? C8 C11 1.506(4) . ? C8 C10 1.515(4) . ? C8 C9 1.518(4) . ? N12 C16 1.334(3) . ? N12 N13 1.363(2) . ? N13 C14 1.351(3) . ? C14 C15 1.375(3) . ? C14 C17 1.513(3) . ? C15 C16 1.389(3) . ? C17 C18 1.526(3) . ? C17 C19 1.531(4) . ? C17 C20 1.537(4) . ? N21 C25 1.333(3) . ? N21 N22 1.355(3) . ? N22 C23 1.349(3) . ? C23 C24 1.374(4) . ? C23 C26 1.512(3) . ? C24 C25 1.382(4) . ? C26 C28 1.528(4) . ? C26 C27 1.530(4) . ? C26 C29 1.531(4) . ? C31 C32 1.520(7) . ? C32 C33 1.499(7) . ? C33 C34 1.510(7) . ? C34 C35 1.525(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N12 Zn1 N3 108.66(8) . . ? N12 Zn1 N21 110.32(8) . . ? N3 Zn1 N21 117.77(8) . . ? N12 Zn1 Br2 108.52(5) . . ? N3 Zn1 Br2 106.32(5) . . ? N21 Zn1 Br2 104.79(5) . . ? C7 N3 N4 105.29(18) . . ? C7 N3 Zn1 126.69(15) . . ? N4 N3 Zn1 127.62(14) . . ? C5 N4 N3 111.96(18) . . ? N4 C5 C6 105.9(2) . . ? N4 C5 C8 121.9(2) . . ? C6 C5 C8 132.2(2) . . ? C7 C6 C5 106.0(2) . . ? N3 C7 C6 110.9(2) . . ? C5 C8 C11 110.3(2) . . ? C5 C8 C10 109.0(2) . . ? C11 C8 C10 110.9(3) . . ? C5 C8 C9 109.0(2) . . ? C11 C8 C9 109.1(3) . . ? C10 C8 C9 108.5(3) . . ? C16 N12 N13 105.26(18) . . ? C16 N12 Zn1 126.39(15) . . ? N13 N12 Zn1 128.26(14) . . ? C14 N13 N12 111.52(18) . . ? N13 C14 C15 106.39(19) . . ? N13 C14 C17 121.2(2) . . ? C15 C14 C17 132.4(2) . . ? C14 C15 C16 106.2(2) . . ? N12 C16 C15 110.6(2) . . ? C14 C17 C18 109.5(2) . . ? C14 C17 C19 109.6(2) . . ? C18 C17 C19 109.5(2) . . ? C14 C17 C20 108.2(2) . . ? C18 C17 C20 109.8(2) . . ? C19 C17 C20 110.2(2) . . ? C25 N21 N22 105.07(19) . . ? C25 N21 Zn1 125.03(16) . . ? N22 N21 Zn1 129.76(15) . . ? C23 N22 N21 111.96(19) . . ? N22 C23 C24 105.9(2) . . ? N22 C23 C26 122.3(2) . . ? C24 C23 C26 131.8(2) . . ? C23 C24 C25 106.4(2) . . ? N21 C25 C24 110.7(2) . . ? C23 C26 C28 109.4(2) . . ? C23 C26 C27 109.3(2) . . ? C28 C26 C27 109.6(3) . . ? C23 C26 C29 108.6(2) . . ? C28 C26 C29 110.5(3) . . ? C27 C26 C29 109.5(3) . . ? C33 C32 C31 112.2(5) . . ? C32 C33 C34 112.2(4) . . ? C33 C34 C35 110.6(6) . . ? 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 Br30 0.88 2.44 3.2920(19) 161.9 . N13 H13 Br30 0.88 2.45 3.2980(18) 160.7 . N22 H22 Br30 0.88 2.45 3.289(2) 159.9 . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.401 _refine_diff_density_min -0.479 _refine_diff_density_rms 0.069 #=END data_mh86 _database_code_CSD 177941 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Iodo-tris[5-tertbutylpyrazole]zinc(II) iodide dichloromethane solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H36 I N6 Zn, I, C H2 Cl2' _chemical_formula_sum 'C22 H38 Cl2 I2 N6 Zn' _chemical_formula_weight 776.65 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' 'I' 'I' -0.4742 1.8119 '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 Orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z' 'x, -y+1/2, z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, -z' '-x, y-1/2, -z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 10.4896(1) _cell_length_b 19.2431(2) _cell_length_c 30.6552(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6187.83(12) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 24599 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 27.47 _exptl_crystal_description 'Rectangular Prism' _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.34 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.667 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3056 _exptl_absorpt_coefficient_mu 2.983 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3115 _exptl_absorpt_correction_T_max 0.4304 _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 24599 _diffrn_reflns_av_R_equivalents 0.0680 _diffrn_reflns_av_sigmaI/netI 0.0461 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 27.47 _reflns_number_total 6911 _reflns_number_gt 6125 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The asymmetric unit contains one complex cation, one iodide anion, and one molecule of CH~2~Cl~2~ which is disordered over three equally occupied orientations [C31-Cl33, C34-Cl36 and C37-Cl39]. All C-Cl bonds within a given orientation of the solvent molecule were restrained to 1.76(2)\%A, and Cl...Cl distances to 2.87(2)\%A. All non-H atoms except for the partial solvent C atoms were refined anisotropically. The largest residual Fourier peak (+1.1 e.\%A^-3^) and hole (-1.3 e.\%A^-3^) are both 0.8\%A from I30. ; _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^)+(0.0537P)^2^+3.4395P] 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 0.0024(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6911 _refine_ls_number_parameters 339 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0427 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.0978 _refine_ls_wR_factor_gt 0.0928 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.092 _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 0.48492(3) 0.286638(17) 0.152391(10) 0.02413(10) Uani 1 1 d . . . I2 I 0.59120(2) 0.188554(10) 0.195992(6) 0.03317(9) Uani 1 1 d . . . N3 N 0.6256(2) 0.34467(13) 0.12595(7) 0.0250(5) Uani 1 1 d . . . N4 N 0.6195(2) 0.40777(13) 0.10557(8) 0.0255(5) Uani 1 1 d . . . H4 H 0.5481 0.4301 0.1001 0.031 Uiso 1 1 calc R . . C5 C 0.7362(3) 0.43155(16) 0.09494(9) 0.0259(6) Uani 1 1 d . . . C6 C 0.8229(3) 0.38203(17) 0.10937(10) 0.0299(6) Uani 1 1 d . . . H6 H 0.9131 0.3836 0.1071 0.036 Uiso 1 1 calc R . . C7 C 0.7496(3) 0.32978(17) 0.12787(9) 0.0293(6) Uani 1 1 d . . . H7 H 0.7836 0.2886 0.1404 0.035 Uiso 1 1 calc R . . C8 C 0.7593(3) 0.50031(17) 0.07302(10) 0.0299(6) Uani 1 1 d . . . C9 C 0.6394(4) 0.5263(2) 0.04979(13) 0.0455(9) Uani 1 1 d . . . H9A H 0.6086 0.4905 0.0297 0.068 Uiso 1 1 calc R . . H9B H 0.6595 0.5687 0.0334 0.068 Uiso 1 1 calc R . . H9C H 0.5732 0.5365 0.0714 0.068 Uiso 1 1 calc R . . C10 C 0.8672(4) 0.4927(2) 0.03956(13) 0.0495(9) Uani 1 1 d . . . H10A H 0.9449 0.4770 0.0544 0.074 Uiso 1 1 calc R . . H10B H 0.8831 0.5377 0.0256 0.074 Uiso 1 1 calc R . . H10C H 0.8426 0.4585 0.0174 0.074 Uiso 1 1 calc R . . C11 C 0.7997(5) 0.5530(2) 0.10796(13) 0.0516(11) Uani 1 1 d . . . H11A H 0.7401 0.5509 0.1325 0.077 Uiso 1 1 calc R . . H11B H 0.7989 0.5999 0.0955 0.077 Uiso 1 1 calc R . . H11C H 0.8858 0.5419 0.1182 0.077 Uiso 1 1 calc R . . N12 N 0.3811(2) 0.23973(13) 0.10487(7) 0.0255(5) Uani 1 1 d . . . N13 N 0.2974(2) 0.26906(13) 0.07680(7) 0.0248(5) Uani 1 1 d . . . H13 H 0.2832 0.3141 0.0752 0.030 Uiso 1 1 calc R . . C14 C 0.2379(3) 0.22149(16) 0.05135(9) 0.0256(6) Uani 1 1 d . . . C15 C 0.2872(3) 0.15814(17) 0.06401(10) 0.0323(7) Uani 1 1 d . . . H15 H 0.2655 0.1140 0.0523 0.039 Uiso 1 1 calc R . . C16 C 0.3746(3) 0.17124(16) 0.09709(10) 0.0309(6) Uani 1 1 d . . . H16 H 0.4226 0.1368 0.1120 0.037 Uiso 1 1 calc R . . C17 C 0.1394(3) 0.24195(17) 0.01814(9) 0.0296(6) Uani 1 1 d . . . C18 C 0.2016(4) 0.2832(3) -0.01890(13) 0.0519(10) Uani 1 1 d . . . H18A H 0.2277 0.3290 -0.0081 0.078 Uiso 1 1 calc R . . H18B H 0.1403 0.2891 -0.0427 0.078 Uiso 1 1 calc R . . H18C H 0.2765 0.2580 -0.0296 0.078 Uiso 1 1 calc R . . C19 C 0.0375(4) 0.2875(2) 0.03949(12) 0.0460(9) Uani 1 1 d . . . H19A H -0.0009 0.2625 0.0640 0.069 Uiso 1 1 calc R . . H19B H -0.0286 0.2987 0.0180 0.069 Uiso 1 1 calc R . . H19C H 0.0767 0.3306 0.0501 0.069 Uiso 1 1 calc R . . C20 C 0.0788(4) 0.1762(2) -0.00049(15) 0.0521(11) Uani 1 1 d . . . H20A H 0.1429 0.1500 -0.0170 0.078 Uiso 1 1 calc R . . H20B H 0.0083 0.1889 -0.0199 0.078 Uiso 1 1 calc R . . H20C H 0.0463 0.1474 0.0234 0.078 Uiso 1 1 calc R . . N21 N 0.3775(3) 0.34028(14) 0.19512(7) 0.0267(5) Uani 1 1 d . . . N22 N 0.3148(3) 0.40147(13) 0.18925(8) 0.0259(5) Uani 1 1 d . . . H22 H 0.3156 0.4253 0.1647 0.031 Uiso 1 1 calc R . . C23 C 0.2517(3) 0.42128(17) 0.22531(9) 0.0290(6) Uani 1 1 d . . . C24 C 0.2746(4) 0.3711(2) 0.25622(10) 0.0373(8) Uani 1 1 d . . . H24 H 0.2436 0.3702 0.2853 0.045 Uiso 1 1 calc R . . C25 C 0.3523(4) 0.32190(18) 0.23629(10) 0.0343(7) Uani 1 1 d . . . H25 H 0.3831 0.2810 0.2500 0.041 Uiso 1 1 calc R . . C26 C 0.1716(3) 0.48651(17) 0.22662(10) 0.0325(7) Uani 1 1 d . . . C27 C 0.0555(4) 0.4778(2) 0.19631(12) 0.0420(8) Uani 1 1 d . . . H27A H 0.0846 0.4735 0.1661 0.063 Uiso 1 1 calc R . . H27B H -0.0002 0.5185 0.1990 0.063 Uiso 1 1 calc R . . H27C H 0.0082 0.4359 0.2046 0.063 Uiso 1 1 calc R . . C28 C 0.1254(5) 0.4993(3) 0.27339(13) 0.0560(11) Uani 1 1 d . . . H28A H 0.0689 0.4613 0.2823 0.084 Uiso 1 1 calc R . . H28B H 0.0787 0.5434 0.2747 0.084 Uiso 1 1 calc R . . H28C H 0.1989 0.5013 0.2931 0.084 Uiso 1 1 calc R . . C29 C 0.2509(4) 0.54891(19) 0.21110(15) 0.0477(9) Uani 1 1 d . . . H29A H 0.3332 0.5491 0.2262 0.072 Uiso 1 1 calc R . . H29B H 0.2050 0.5921 0.2176 0.072 Uiso 1 1 calc R . . H29C H 0.2651 0.5454 0.1796 0.072 Uiso 1 1 calc R . . I30 I 0.29461(2) 0.451064(10) 0.080868(6) 0.03000(9) Uani 1 1 d . . . C31 C 0.417(2) 0.6991(10) 0.1750(7) 0.058(8) Uiso 0.33 1 d PD A 1 H31A H 0.4406 0.6878 0.2055 0.069 Uiso 0.33 1 calc PR A 1 H31B H 0.3255 0.6873 0.1715 0.069 Uiso 0.33 1 calc PR A 1 Cl32 Cl 0.5018(17) 0.6472(7) 0.1416(5) 0.080(5) Uani 0.33 1 d PD A 1 Cl33 Cl 0.433(2) 0.7873(9) 0.1681(7) 0.057(5) Uani 0.33 1 d PD A 1 C34 C 0.3914(13) 0.7102(7) 0.1734(6) 0.029(4) Uiso 0.33 1 d PD B 2 H34A H 0.3588 0.7022 0.2033 0.034 Uiso 0.33 1 calc PR B 2 H34B H 0.3268 0.6934 0.1524 0.034 Uiso 0.33 1 calc PR B 2 Cl35 Cl 0.5389(12) 0.6643(5) 0.1657(4) 0.098(4) Uani 0.33 1 d PD B 2 Cl36 Cl 0.420(3) 0.7994(8) 0.1653(12) 0.040(3) Uani 0.33 1 d PD B 2 C37 C 0.4004(16) 0.6991(8) 0.1679(6) 0.030(4) Uiso 0.33 1 d PD C 3 H37A H 0.3230 0.6888 0.1506 0.036 Uiso 0.33 1 calc PR C 3 H37B H 0.3855 0.6836 0.1983 0.036 Uiso 0.33 1 calc PR C 3 Cl38 Cl 0.5290(17) 0.6552(8) 0.1463(7) 0.075(4) Uani 0.33 1 d PD C 3 Cl39 Cl 0.432(2) 0.7896(9) 0.1670(9) 0.039(4) Uani 0.33 1 d PD C 3 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 0.03079(19) 0.02060(18) 0.02100(17) -0.00019(12) -0.00125(13) 0.00020(13) I2 0.04624(16) 0.02365(13) 0.02960(13) 0.00385(7) -0.00529(8) 0.00487(8) N3 0.0313(13) 0.0230(12) 0.0207(10) 0.0014(9) -0.0013(9) 0.0009(10) N4 0.0294(13) 0.0240(12) 0.0231(11) 0.0034(9) 0.0002(9) 0.0008(10) C5 0.0330(15) 0.0249(14) 0.0199(12) -0.0019(11) 0.0005(11) -0.0007(12) C6 0.0273(15) 0.0321(16) 0.0304(14) 0.0006(12) 0.0013(12) 0.0023(12) C7 0.0338(15) 0.0267(14) 0.0274(13) 0.0002(12) 0.0023(12) 0.0051(13) C8 0.0361(16) 0.0270(15) 0.0265(13) 0.0063(12) 0.0012(13) -0.0047(13) C9 0.047(2) 0.0403(19) 0.049(2) 0.0207(17) -0.0065(17) -0.0020(16) C10 0.051(2) 0.051(2) 0.046(2) 0.0121(18) 0.0152(18) 0.0001(18) C11 0.082(3) 0.032(2) 0.041(2) 0.0035(15) -0.0073(19) -0.0128(18) N12 0.0307(12) 0.0235(12) 0.0224(10) -0.0005(9) -0.0037(10) 0.0007(10) N13 0.0311(13) 0.0190(11) 0.0243(11) -0.0020(9) -0.0038(9) -0.0001(9) C14 0.0270(14) 0.0260(14) 0.0238(13) -0.0053(11) 0.0039(11) -0.0039(11) C15 0.0437(18) 0.0241(15) 0.0292(15) -0.0048(12) -0.0044(13) -0.0015(13) C16 0.0400(17) 0.0232(14) 0.0294(14) -0.0008(12) -0.0019(13) 0.0022(13) C17 0.0302(15) 0.0327(16) 0.0258(13) -0.0044(12) -0.0019(12) -0.0004(13) C18 0.041(2) 0.076(3) 0.0380(19) 0.021(2) -0.0035(16) 0.0007(19) C19 0.0340(19) 0.064(3) 0.0403(18) -0.0118(17) -0.0082(15) 0.0140(17) C20 0.060(3) 0.044(2) 0.053(2) -0.0120(18) -0.0298(19) -0.0026(18) N21 0.0329(13) 0.0257(13) 0.0216(11) 0.0014(9) 0.0003(9) 0.0043(11) N22 0.0347(13) 0.0218(12) 0.0211(10) 0.0018(9) 0.0006(10) 0.0021(10) C23 0.0306(15) 0.0317(16) 0.0248(13) -0.0048(12) 0.0023(12) -0.0012(12) C24 0.048(2) 0.0440(19) 0.0200(13) 0.0048(13) 0.0067(13) 0.0068(16) C25 0.047(2) 0.0327(17) 0.0233(13) 0.0059(12) -0.0014(13) 0.0047(14) C26 0.0353(16) 0.0307(16) 0.0315(15) -0.0076(12) 0.0036(13) 0.0022(13) C27 0.0362(18) 0.0355(19) 0.054(2) -0.0075(16) -0.0043(16) 0.0059(15) C28 0.062(3) 0.063(3) 0.043(2) -0.0165(19) 0.0128(19) 0.018(2) C29 0.043(2) 0.0288(17) 0.071(3) -0.0082(18) 0.004(2) 0.0019(15) I30 0.04062(15) 0.02356(13) 0.02582(12) 0.00399(7) -0.00406(8) 0.00229(8) Cl32 0.114(11) 0.057(6) 0.068(4) 0.009(4) 0.009(4) 0.023(5) Cl33 0.081(8) 0.028(8) 0.061(8) 0.002(6) 0.004(5) 0.010(5) Cl35 0.088(5) 0.048(5) 0.159(10) 0.031(5) 0.036(7) 0.027(4) Cl36 0.049(8) 0.021(4) 0.048(4) 0.002(3) 0.010(4) 0.007(3) Cl38 0.072(5) 0.037(3) 0.116(9) -0.017(5) 0.017(6) 0.022(4) Cl39 0.024(3) 0.048(9) 0.046(7) -0.007(6) 0.008(4) -0.001(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N21 2.012(3) . ? Zn1 N3 2.020(3) . ? Zn1 N12 2.030(2) . ? Zn1 I2 2.5674(4) . ? N3 C7 1.334(4) . ? N3 N4 1.367(3) . ? N4 C5 1.347(4) . ? C5 C6 1.389(4) . ? C5 C8 1.504(4) . ? C6 C7 1.387(5) . ? C8 C9 1.529(5) . ? C8 C10 1.535(5) . ? C8 C11 1.535(5) . ? N12 C16 1.341(4) . ? N12 N13 1.353(3) . ? N13 C14 1.355(4) . ? C14 C15 1.380(4) . ? C14 C17 1.503(4) . ? C15 C16 1.390(5) . ? C17 C20 1.527(5) . ? C17 C19 1.530(5) . ? C17 C18 1.532(5) . ? N21 C25 1.337(4) . ? N21 N22 1.361(4) . ? N22 C23 1.344(4) . ? C23 C24 1.374(5) . ? C23 C26 1.511(5) . ? C24 C25 1.391(5) . ? C26 C28 1.534(5) . ? C26 C29 1.536(5) . ? C26 C27 1.541(5) . ? C31 Cl32 1.686(16) . ? C31 Cl33 1.718(16) . ? C34 Cl35 1.797(14) . ? C34 Cl36 1.760(16) . ? C37 Cl39 1.773(15) . ? C37 Cl38 1.723(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N21 Zn1 N3 112.74(11) . . ? N21 Zn1 N12 113.26(11) . . ? N3 Zn1 N12 110.45(10) . . ? N21 Zn1 I2 106.34(7) . . ? N3 Zn1 I2 107.35(7) . . ? N12 Zn1 I2 106.23(7) . . ? C7 N3 N4 104.8(2) . . ? C7 N3 Zn1 125.2(2) . . ? N4 N3 Zn1 129.9(2) . . ? C5 N4 N3 111.7(2) . . ? N4 C5 C6 106.5(3) . . ? N4 C5 C8 123.6(3) . . ? C6 C5 C8 129.9(3) . . ? C7 C6 C5 105.4(3) . . ? N3 C7 C6 111.5(3) . . ? C5 C8 C9 111.4(3) . . ? C5 C8 C10 109.5(3) . . ? C9 C8 C10 109.1(3) . . ? C5 C8 C11 108.3(3) . . ? C9 C8 C11 109.6(3) . . ? C10 C8 C11 109.0(3) . . ? C16 N12 N13 105.3(2) . . ? C16 N12 Zn1 126.3(2) . . ? N13 N12 Zn1 128.24(19) . . ? N12 N13 C14 112.5(2) . . ? N13 C14 C15 105.2(3) . . ? N13 C14 C17 122.0(3) . . ? C15 C14 C17 132.8(3) . . ? C14 C15 C16 107.0(3) . . ? N12 C16 C15 110.0(3) . . ? C14 C17 C20 108.8(3) . . ? C14 C17 C19 109.9(2) . . ? C20 C17 C19 110.1(3) . . ? C14 C17 C18 110.2(3) . . ? C20 C17 C18 109.3(3) . . ? C19 C17 C18 108.5(3) . . ? C25 N21 N22 104.9(2) . . ? C25 N21 Zn1 126.1(2) . . ? N22 N21 Zn1 128.93(18) . . ? C23 N22 N21 112.0(2) . . ? N22 C23 C24 106.4(3) . . ? N22 C23 C26 122.1(3) . . ? C24 C23 C26 131.5(3) . . ? C23 C24 C25 106.1(3) . . ? N21 C25 C24 110.5(3) . . ? C23 C26 C28 109.5(3) . . ? C23 C26 C29 109.9(3) . . ? C28 C26 C29 109.6(3) . . ? C23 C26 C27 109.5(3) . . ? C28 C26 C27 109.3(3) . . ? C29 C26 C27 109.0(3) . . ? Cl32 C31 Cl33 117.3(12) . . ? Cl35 C34 Cl36 108.3(11) . . ? Cl39 C37 Cl38 109.3(10) . . ? 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 I30 0.88 2.75 3.590(3) 159.2 . N13 H13 I30 0.88 2.64 3.505(3) 165.9 . N22 H22 I30 0.88 2.63 3.463(2) 158.9 . _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.063 _refine_diff_density_min -1.270 _refine_diff_density_rms 0.170