Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_djn174s _database_code_CSD 155418 _journal_coden_Cambridge 182 loop_ _publ_author_name 'Medforth, Craig J.' 'Nurco, Daniel J.' 'Shetty, Shankar J.' 'Smith, Kevin M.' 'Vicente, Maria H.' _publ_contact_author_name 'Dr Maria H Vicente' _publ_contact_author_address ; University of California Davis Department of chemistry Davis California 95616 UNITED STATES OF AMERICA ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; Zn(II) meso-Tetra[4-(1-methyl-o-carboranyl)methylphenyl]porphyrin ; _chemical_name_common 'Zn(II) TMCP' _chemical_melting_point ? _chemical_formula_moiety 'C60 H84.8 B40 N4 Zn0.60, C6 H5 Cl' _chemical_formula_sum 'C66 H89.8 B40 Cl N4 Zn0.60' _chemical_formula_weight 1447.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 13.3139(5) _cell_length_b 18.6428(8) _cell_length_c 15.7642(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.9630(10) _cell_angle_gamma 90.00 _cell_volume 3903.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 5726 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 30.91 _exptl_crystal_description pinacoid _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.226 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1486 _exptl_absorpt_coefficient_mu 0.274 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9223 _exptl_absorpt_correction_T_max 0.9731 _exptl_absorpt_process_details ; SADABS 2.0 (Sheldrick, 2000) ; _exptl_special_details ; Crystals were grown by the slow diffusion of methanol into a solution of the title compound dissolved in chlorobenzene. The crystals were transferred directly from their mother liquor of crystallization to a light hydrocarbon oil (Paratone N) in which they were examined and cut as necessary. The selected crystal was mounted in a 90(2) K stream of anhydrous nitrogen for cell determination and data collection at 2.0 kW. ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 frames' _diffrn_standards_interval_count ; Measured at the beginning and end of the data collection. ; _diffrn_standards_interval_time ? _diffrn_standards_decay_% <0.1 _diffrn_reflns_number 33833 _diffrn_reflns_av_R_equivalents 0.0714 _diffrn_reflns_av_sigmaI/netI 0.0702 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8980 _reflns_number_gt 5896 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5, XP (Sheldrick, 1994)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 Zn ion was 60% present. This was determined via free variable refinement of the Zn occupancy while its isotropic thermal was fixed at 0.020\%A^2^ (the nitrogens featured isotropic thermal parameters of 0.023\%A^2^ and 0.020\%A^2^). ; _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^)+(0.0866P)^2^+4.2585P] 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 ; In the final model all hydrogen atom positions were treated with a riding model. However, the freely refining position of H11 may be of interest. As such, the relevant geometrical distances involving riding and freely refining H11 are given below. riding H11: Zn1-H11, 2.09\%A H11-B11, 1.12\%A freely refining H11: Zn1-H11, 2.16\%A H11-B11, 1.06\%A ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8980 _refine_ls_number_parameters 515 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1108 _refine_ls_R_factor_gt 0.0693 _refine_ls_wR_factor_ref 0.1908 _refine_ls_wR_factor_gt 0.1702 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.5000 0.5000 1.0000 0.02020(19) Uani 0.60 2 d SP . . N1 N 0.46321(17) 0.60565(12) 0.97510(14) 0.0186(5) Uani 1 1 d . . . N2 N 0.40384(16) 0.46585(12) 0.90008(14) 0.0190(5) Uani 1 1 d . . . C1 C 0.4895(2) 0.66411(14) 1.02507(17) 0.0203(6) Uani 1 1 d . . . C2 C 0.4273(2) 0.72463(15) 0.99821(18) 0.0238(6) Uani 1 1 d . . . H2 H 0.4296 0.7712 1.0227 0.029 Uiso 1 1 calc R . . C3 C 0.3655(2) 0.70273(14) 0.93184(18) 0.0232(6) Uani 1 1 d . . . H3 H 0.3169 0.7311 0.9002 0.028 Uiso 1 1 calc R . . C4 C 0.3873(2) 0.62764(14) 0.91801(18) 0.0201(6) Uani 1 1 d . . . C5 C 0.33318(19) 0.58439(14) 0.85787(17) 0.0186(5) Uani 1 1 d . . . C5A C 0.2572(2) 0.62166(14) 0.79852(17) 0.0200(6) Uani 1 1 d . . . C5B C 0.2874(2) 0.66804(15) 0.73648(19) 0.0252(6) Uani 1 1 d . . . H5B H 0.3571 0.6746 0.7296 0.030 Uiso 1 1 calc R . . C5C C 0.2165(2) 0.70517(15) 0.68406(19) 0.0252(6) Uani 1 1 d . . . H5C H 0.2383 0.7368 0.6418 0.030 Uiso 1 1 calc R . . C5D C 0.1146(2) 0.69619(14) 0.69331(17) 0.0211(6) Uani 1 1 d . . . C5E C 0.0841(2) 0.64948(15) 0.75509(18) 0.0238(6) Uani 1 1 d . . . H5E H 0.0144 0.6429 0.7617 0.029 Uiso 1 1 calc R . . C5F C 0.1546(2) 0.61214(15) 0.80749(18) 0.0223(6) Uani 1 1 d . . . H5F H 0.1327 0.5802 0.8494 0.027 Uiso 1 1 calc R . . C5G C 0.0361(2) 0.73783(15) 0.63947(19) 0.0262(6) Uani 1 1 d . . . H5G1 H 0.0632 0.7861 0.6281 0.031 Uiso 1 1 calc R . . H5G2 H -0.0241 0.7442 0.6723 0.031 Uiso 1 1 calc R . . C5H C 0.0038(2) 0.70200(15) 0.55434(17) 0.0219(6) Uani 1 1 d . . . C5I C -0.0969(2) 0.73701(16) 0.50163(18) 0.0252(6) Uani 1 1 d . . . C5J C -0.1499(2) 0.79822(16) 0.5431(2) 0.0303(7) Uani 1 1 d . . . H5J1 H -0.1668 0.7838 0.6002 0.045 Uiso 1 1 calc R . . H5J2 H -0.2117 0.8103 0.5087 0.045 Uiso 1 1 calc R . . H5J3 H -0.1054 0.8402 0.5472 0.045 Uiso 1 1 calc R . . C6 C 0.34059(19) 0.50985(14) 0.85022(17) 0.0189(5) Uani 1 1 d . . . C7 C 0.2828(2) 0.46633(15) 0.78932(18) 0.0228(6) Uani 1 1 d . . . H7 H 0.2337 0.4831 0.7473 0.027 Uiso 1 1 calc R . . C8 C 0.3109(2) 0.39703(15) 0.80275(18) 0.0244(6) Uani 1 1 d . . . H8 H 0.2850 0.3565 0.7719 0.029 Uiso 1 1 calc R . . C9 C 0.3874(2) 0.39606(15) 0.87234(18) 0.0209(6) Uani 1 1 d . . . C10 C 0.4385(2) 0.33521(14) 0.90526(17) 0.0200(6) Uani 1 1 d . . . C10A C 0.4189(2) 0.26500(14) 0.86094(18) 0.0208(6) Uani 1 1 d . . . C10B C 0.4366(2) 0.25545(15) 0.77536(19) 0.0232(6) Uani 1 1 d . . . H10B H 0.4553 0.2955 0.7426 0.028 Uiso 1 1 calc R . . C10C C 0.4274(2) 0.18831(15) 0.73741(19) 0.0253(6) Uani 1 1 d . . . H10C H 0.4397 0.1830 0.6791 0.030 Uiso 1 1 calc R . . C10D C 0.4001(2) 0.12839(15) 0.7840(2) 0.0247(6) Uani 1 1 d . . . C10E C 0.3785(2) 0.13832(15) 0.8680(2) 0.0272(7) Uani 1 1 d . . . H10E H 0.3574 0.0986 0.9001 0.033 Uiso 1 1 calc R . . C10F C 0.3873(2) 0.20587(15) 0.90611(19) 0.0252(6) Uani 1 1 d . . . H10F H 0.3715 0.2116 0.9636 0.030 Uiso 1 1 calc R . . C10G C 0.4002(2) 0.05417(15) 0.7460(2) 0.0293(7) Uani 1 1 d . . . H10A H 0.4217 0.0197 0.7915 0.035 Uiso 1 1 calc R . . H10D H 0.4509 0.0527 0.7030 0.035 Uiso 1 1 calc R . . C10H C 0.2984(2) 0.02896(15) 0.70375(18) 0.0230(6) Uani 1 1 d . . . C10I C 0.2806(2) -0.05970(15) 0.6953(2) 0.0263(6) Uani 1 1 d . . . C10J C 0.3612(2) -0.11016(16) 0.7308(2) 0.0344(8) Uani 1 1 d . . . H10G H 0.3562 -0.1153 0.7922 0.052 Uiso 1 1 calc R . . H10H H 0.4275 -0.0909 0.7199 0.052 Uiso 1 1 calc R . . H10I H 0.3522 -0.1571 0.7034 0.052 Uiso 1 1 calc R . . B1 B -0.1061(3) 0.65347(18) 0.5485(2) 0.0282(7) Uani 1 1 d . . . H1 H -0.1517 0.6422 0.6041 0.034 Uiso 1 1 calc R . . B2 B 0.0111(3) 0.61102(18) 0.5372(2) 0.0269(7) Uani 1 1 d . . . H2A H 0.0430 0.5713 0.5852 0.032 Uiso 1 1 calc R . . B3 B 0.0892(3) 0.67272(18) 0.4862(2) 0.0268(7) Uani 1 1 d . . . H3A H 0.1727 0.6735 0.5008 0.032 Uiso 1 1 calc R . . B4 B 0.0206(3) 0.75286(18) 0.4650(2) 0.0263(7) Uani 1 1 d . . . H4 H 0.0583 0.8066 0.4657 0.032 Uiso 1 1 calc R . . B5 B -0.0850(3) 0.7331(2) 0.3943(2) 0.0317(8) Uani 1 1 d . . . H5 H -0.1174 0.7738 0.3478 0.038 Uiso 1 1 calc R . . B6 B -0.1631(3) 0.6718(2) 0.4453(2) 0.0344(8) Uani 1 1 d . . . H6 H -0.2468 0.6721 0.4323 0.041 Uiso 1 1 calc R . . B7 B -0.0940(3) 0.59070(19) 0.4655(2) 0.0331(8) Uani 1 1 d . . . H7A H -0.1319 0.5371 0.4652 0.040 Uiso 1 1 calc R . . B8 B 0.0275(3) 0.60213(19) 0.4267(2) 0.0293(8) Uani 1 1 d . . . H8A H 0.0701 0.5561 0.4009 0.035 Uiso 1 1 calc R . . B9 B 0.0324(3) 0.6905(2) 0.3827(2) 0.0335(8) Uani 1 1 d . . . H9 H 0.0783 0.7026 0.3276 0.040 Uiso 1 1 calc R . . B10 B -0.0802(3) 0.6400(2) 0.3700(2) 0.0359(9) Uani 1 1 d . . . H10 H -0.1089 0.6187 0.3065 0.043 Uiso 1 1 calc R . . B11 B 0.3043(3) -0.01141(17) 0.6053(2) 0.0265(7) Uani 1 1 d . . . H11 H 0.3750 -0.0163 0.5711 0.032 Uiso 1 1 calc R . . B12 B 0.2440(2) 0.07175(17) 0.6164(2) 0.0241(7) Uani 1 1 d . . . H12 H 0.2742 0.1222 0.5891 0.029 Uiso 1 1 calc R . . B13 B 0.1866(2) 0.07179(17) 0.7155(2) 0.0235(7) Uani 1 1 d . . . H13 H 0.1784 0.1223 0.7529 0.028 Uiso 1 1 calc R . . B14 B 0.2142(3) -0.01122(19) 0.7663(2) 0.0268(7) Uani 1 1 d . . . H14 H 0.2255 -0.0158 0.8371 0.032 Uiso 1 1 calc R . . B15 B 0.1574(3) -0.08013(19) 0.7016(2) 0.0297(8) Uani 1 1 d . . . H15 H 0.1300 -0.1308 0.7305 0.036 Uiso 1 1 calc R . . B16 B 0.2133(3) -0.08044(19) 0.6021(2) 0.0284(7) Uani 1 1 d . . . H16 H 0.2229 -0.1311 0.5653 0.034 Uiso 1 1 calc R . . B17 B 0.1864(3) 0.00305(18) 0.5509(2) 0.0273(7) Uani 1 1 d . . . H17 H 0.1773 0.0081 0.4799 0.033 Uiso 1 1 calc R . . B18 B 0.1126(2) 0.05440(18) 0.6191(2) 0.0241(7) Uani 1 1 d . . . H18 H 0.0545 0.0934 0.5928 0.029 Uiso 1 1 calc R . . B19 B 0.0943(3) 0.00240(19) 0.7124(2) 0.0266(7) Uani 1 1 d . . . H19 H 0.0243 0.0067 0.7476 0.032 Uiso 1 1 calc R . . B20 B 0.0941(3) -0.03993(18) 0.6104(2) 0.0286(8) Uani 1 1 d . . . H20 H 0.0239 -0.0634 0.5785 0.034 Uiso 1 1 calc R . . Cl1 Cl 0.3530(9) 0.9377(8) 1.0439(11) 0.0661(11) Uiso 0.123(5) 1 d P . . Cl2 Cl 0.5766(4) 0.9313(3) 0.8983(3) 0.0661(11) Uiso 0.259(3) 1 d P . . Cl3 Cl 0.3485(9) 0.9216(7) 1.0085(11) 0.0661(11) Uiso 0.118(5) 1 d P . . C11 C 0.5134(7) 0.9682(5) 0.9617(6) 0.057(2) Uiso 0.50 1 d P . . C12 C 0.4177(9) 0.9385(6) 0.9866(7) 0.068(3) Uiso 0.50 1 d P . . C13 C 0.6062(8) 0.9639(6) 0.9133(6) 0.059(2) Uiso 0.50 1 d P . . C14 C 0.3668(10) 0.9799(9) 1.0507(9) 0.091(4) Uiso 0.50 1 d P . . C15 C 0.5085(9) 0.9259(7) 0.9384(8) 0.083(3) Uiso 0.50 1 d P . . C16 C 0.4588(8) 0.9672(5) 0.9986(6) 0.057(2) Uiso 0.50 1 d P . . 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 0.0221(4) 0.0144(3) 0.0223(4) -0.0060(3) -0.0120(3) 0.0042(3) N1 0.0209(11) 0.0163(11) 0.0177(11) -0.0010(9) -0.0049(9) 0.0011(9) N2 0.0203(11) 0.0163(11) 0.0197(11) -0.0018(9) -0.0043(9) 0.0009(9) C1 0.0232(13) 0.0167(13) 0.0203(14) 0.0000(11) -0.0031(11) 0.0000(10) C2 0.0279(14) 0.0160(13) 0.0264(15) -0.0003(11) -0.0070(12) 0.0030(11) C3 0.0258(14) 0.0176(13) 0.0249(15) 0.0010(11) -0.0081(12) 0.0013(11) C4 0.0203(13) 0.0173(13) 0.0221(14) 0.0020(11) -0.0038(11) -0.0016(10) C5 0.0182(12) 0.0190(13) 0.0178(13) -0.0002(10) -0.0034(10) 0.0008(10) C5A 0.0218(13) 0.0170(13) 0.0202(14) -0.0031(11) -0.0068(11) 0.0009(10) C5B 0.0215(13) 0.0257(15) 0.0274(16) 0.0021(12) -0.0056(12) -0.0030(11) C5C 0.0295(15) 0.0208(14) 0.0240(15) 0.0040(11) -0.0080(12) -0.0059(11) C5D 0.0261(14) 0.0164(13) 0.0198(14) -0.0042(11) -0.0063(11) 0.0039(11) C5E 0.0219(14) 0.0259(15) 0.0233(14) -0.0014(12) -0.0014(11) 0.0026(11) C5F 0.0237(14) 0.0221(14) 0.0207(14) 0.0022(11) -0.0017(11) 0.0009(11) C5G 0.0298(15) 0.0196(14) 0.0275(16) -0.0030(12) -0.0098(12) 0.0053(11) C5H 0.0247(14) 0.0187(13) 0.0209(14) 0.0009(11) -0.0075(11) 0.0008(11) C5I 0.0256(14) 0.0242(14) 0.0245(15) -0.0001(12) -0.0078(12) 0.0024(11) C5J 0.0299(15) 0.0262(15) 0.0336(17) -0.0005(13) -0.0058(13) 0.0050(12) C6 0.0166(12) 0.0203(13) 0.0191(13) -0.0009(11) -0.0037(10) -0.0004(10) C7 0.0226(13) 0.0211(14) 0.0232(14) -0.0035(11) -0.0090(11) 0.0016(11) C8 0.0244(14) 0.0215(14) 0.0259(15) -0.0054(12) -0.0083(12) 0.0012(11) C9 0.0188(13) 0.0207(13) 0.0224(14) -0.0055(11) -0.0035(11) 0.0002(10) C10 0.0216(13) 0.0159(13) 0.0220(14) -0.0025(11) -0.0022(11) -0.0005(10) C10A 0.0178(12) 0.0182(13) 0.0252(15) -0.0024(11) -0.0071(11) 0.0021(10) C10B 0.0223(13) 0.0184(13) 0.0281(15) -0.0022(11) -0.0041(12) -0.0011(11) C10C 0.0207(13) 0.0260(15) 0.0283(16) -0.0066(12) -0.0056(12) -0.0010(11) C10D 0.0200(13) 0.0179(13) 0.0347(17) -0.0051(12) -0.0089(12) 0.0020(10) C10E 0.0267(15) 0.0203(14) 0.0328(17) 0.0025(12) -0.0099(13) -0.0035(11) C10F 0.0265(14) 0.0232(14) 0.0248(15) -0.0010(12) -0.0063(12) -0.0024(11) C10G 0.0223(14) 0.0209(14) 0.0431(19) -0.0076(13) -0.0086(13) 0.0023(11) C10H 0.0236(14) 0.0171(13) 0.0276(15) -0.0039(11) -0.0040(12) 0.0018(11) C10I 0.0303(15) 0.0171(13) 0.0308(16) -0.0023(12) -0.0038(13) 0.0013(11) C10J 0.0363(17) 0.0194(15) 0.046(2) -0.0022(14) -0.0097(15) 0.0092(13) B1 0.0317(18) 0.0200(16) 0.0321(19) 0.0008(14) -0.0037(15) -0.0055(13) B2 0.0379(19) 0.0182(15) 0.0236(17) 0.0005(13) -0.0058(14) 0.0013(14) B3 0.0309(17) 0.0223(16) 0.0266(18) 0.0005(13) -0.0015(14) 0.0040(13) B4 0.0308(17) 0.0223(16) 0.0255(17) 0.0051(13) 0.0000(14) 0.0015(13) B5 0.043(2) 0.0284(18) 0.0221(17) 0.0010(14) -0.0084(15) 0.0055(15) B6 0.0310(18) 0.0324(19) 0.038(2) -0.0029(16) -0.0130(16) -0.0016(15) B7 0.040(2) 0.0226(17) 0.035(2) -0.0051(15) -0.0076(16) -0.0037(15) B8 0.042(2) 0.0240(17) 0.0214(17) -0.0017(14) -0.0031(15) 0.0046(15) B9 0.044(2) 0.0312(19) 0.0247(18) 0.0009(15) 0.0001(16) 0.0055(16) B10 0.050(2) 0.0319(19) 0.0244(18) -0.0030(15) -0.0113(17) 0.0063(17) B11 0.0306(17) 0.0215(16) 0.0270(17) -0.0063(13) -0.0008(14) 0.0032(13) B12 0.0256(16) 0.0193(15) 0.0269(17) 0.0004(13) -0.0023(13) 0.0007(12) B13 0.0215(15) 0.0228(16) 0.0255(17) -0.0066(13) -0.0029(13) 0.0043(12) B14 0.0272(16) 0.0300(18) 0.0226(16) 0.0013(14) -0.0026(13) 0.0015(14) B15 0.0307(18) 0.0242(17) 0.0332(19) 0.0052(15) -0.0045(15) -0.0054(14) B16 0.0316(18) 0.0235(16) 0.0294(18) -0.0075(14) -0.0038(15) -0.0018(14) B17 0.0312(17) 0.0272(17) 0.0229(16) -0.0034(14) -0.0018(14) 0.0003(14) B18 0.0237(16) 0.0245(16) 0.0231(17) -0.0018(13) -0.0051(13) 0.0010(13) B19 0.0229(15) 0.0324(18) 0.0242(17) 0.0024(14) -0.0008(13) -0.0010(14) B20 0.0282(17) 0.0228(17) 0.0334(19) -0.0013(14) -0.0081(15) -0.0049(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 N2 2.061(2) . ? Zn1 N2 2.061(2) 3_667 ? Zn1 N1 2.061(2) . ? Zn1 N1 2.061(2) 3_667 ? N1 C4 1.369(3) . ? N1 C1 1.376(3) . ? N2 C6 1.382(3) . ? N2 C9 1.385(3) . ? C1 C10 1.407(4) 3_667 ? C1 C2 1.445(4) . ? C2 C3 1.349(4) . ? C3 C4 1.449(4) . ? C4 C5 1.405(4) . ? C5 C6 1.399(4) . ? C5 C5A 1.501(4) . ? C5A C5B 1.386(4) . ? C5A C5F 1.394(4) . ? C5B C5C 1.394(4) . ? C5C C5D 1.385(4) . ? C5D C5E 1.388(4) . ? C5D C5G 1.514(4) . ? C5E C5F 1.393(4) . ? C5G C5H 1.534(4) . ? C5H C5I 1.661(4) . ? C5H B3 1.707(5) . ? C5H B1 1.718(4) . ? C5H B2 1.721(4) . ? C5H B4 1.725(4) . ? C5I C5J 1.514(4) . ? C5I B5 1.712(5) . ? C5I B6 1.714(5) . ? C5I B4 1.729(5) . ? C5I B1 1.732(4) . ? C6 C7 1.439(4) . ? C7 C8 1.358(4) . ? C8 C9 1.444(4) . ? C9 C10 1.404(4) . ? C10 C1 1.407(4) 3_667 ? C10 C10A 1.498(4) . ? C10A C10F 1.393(4) . ? C10A C10B 1.397(4) . ? C10B C10C 1.389(4) . ? C10C C10D 1.399(4) . ? C10D C10E 1.387(4) . ? C10D C10G 1.508(4) . ? C10E C10F 1.397(4) . ? C10G C10H 1.542(4) . ? C10H C10I 1.674(4) . ? C10H B12 1.709(4) . ? C10H B13 1.710(4) . ? C10H B14 1.715(5) . ? C10H B11 1.731(4) . ? C10I C10J 1.505(4) . ? C10I B15 1.694(5) . ? C10I B16 1.712(4) . ? C10I B11 1.727(5) . ? C10I B14 1.729(5) . ? B1 B2 1.770(5) . ? B1 B7 1.771(5) . ? B1 B6 1.779(5) . ? B2 B7 1.778(5) . ? B2 B8 1.779(5) . ? B2 B3 1.780(5) . ? B3 B4 1.771(5) . ? B3 B9 1.781(5) . ? B3 B8 1.783(5) . ? B4 B9 1.756(5) . ? B4 B5 1.771(5) . ? B5 B9 1.773(5) . ? B5 B6 1.775(6) . ? B5 B10 1.780(5) . ? B6 B10 1.777(6) . ? B6 B7 1.786(5) . ? B7 B8 1.781(6) . ? B7 B10 1.783(6) . ? B8 B10 1.782(5) . ? B8 B9 1.790(5) . ? B9 B10 1.770(6) . ? B11 B17 1.758(5) . ? B11 B12 1.760(5) . ? B11 B16 1.766(5) . ? B12 B18 1.782(5) . ? B12 B17 1.785(5) . ? B12 B13 1.786(5) . ? B13 B14 1.769(5) . ? B13 B18 1.782(4) . ? B13 B19 1.783(5) . ? B14 B19 1.773(5) . ? B14 B15 1.776(5) . ? B15 B19 1.767(5) . ? B15 B20 1.781(5) . ? B15 B16 1.782(6) . ? B16 B20 1.771(5) . ? B16 B17 1.779(5) . ? B17 B18 1.784(5) . ? B17 B20 1.787(5) . ? B18 B20 1.780(5) . ? B18 B19 1.793(5) . ? B19 B20 1.792(5) . ? Cl1 Cl3 0.633(14) . ? Cl1 C14 0.812(18) . ? Cl1 C12 1.291(18) . ? Cl1 C16 1.713(16) . ? Cl1 C13 2.016(19) 3_677 ? Cl2 C13 0.753(11) . ? Cl2 C15 1.145(13) . ? Cl2 C11 1.515(12) . ? Cl2 C14 1.968(17) 3_677 ? Cl3 C12 1.054(14) . ? Cl3 C14 1.29(2) . ? Cl3 C16 1.713(16) . ? C11 C15 0.869(13) . ? C11 C16 0.962(11) . ? C11 C16 1.397(13) 3_677 ? C11 C12 1.468(15) . ? C11 C13 1.498(14) . ? C11 C11 1.75(2) 3_677 ? C11 C14 1.888(18) 3_677 ? C12 C16 0.779(12) . ? C12 C14 1.474(17) . ? C12 C15 1.490(16) . ? C13 C14 1.234(16) 3_677 ? C13 C15 1.555(17) . ? C13 Cl1 2.02(2) 3_677 ? C14 C13 1.234(16) 3_677 ? C14 C16 1.540(16) . ? C14 C11 1.888(18) 3_677 ? C14 Cl2 1.968(17) 3_677 ? C15 C16 1.419(17) . ? C16 C11 1.397(13) 3_677 ? C16 C16 1.64(2) 3_677 ? 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 N2 Zn1 N2 180.000(1) . 3_667 ? N2 Zn1 N1 91.30(8) . . ? N2 Zn1 N1 88.70(8) 3_667 . ? N2 Zn1 N1 88.70(8) . 3_667 ? N2 Zn1 N1 91.30(8) 3_667 3_667 ? N1 Zn1 N1 180.000(1) . 3_667 ? C4 N1 C1 106.6(2) . . ? C4 N1 Zn1 124.50(17) . . ? C1 N1 Zn1 126.89(17) . . ? C6 N2 C9 107.5(2) . . ? C6 N2 Zn1 125.00(17) . . ? C9 N2 Zn1 127.44(18) . . ? N1 C1 C10 125.9(2) . 3_667 ? N1 C1 C2 109.4(2) . . ? C10 C1 C2 124.6(2) 3_667 . ? C3 C2 C1 107.3(2) . . ? C2 C3 C4 106.9(2) . . ? N1 C4 C5 126.3(2) . . ? N1 C4 C3 109.7(2) . . ? C5 C4 C3 123.9(2) . . ? C6 C5 C4 126.3(2) . . ? C6 C5 C5A 117.0(2) . . ? C4 C5 C5A 116.6(2) . . ? C5B C5A C5F 119.0(2) . . ? C5B C5A C5 120.8(2) . . ? C5F C5A C5 120.1(2) . . ? C5A C5B C5C 120.7(3) . . ? C5D C5C C5B 120.3(3) . . ? C5C C5D C5E 119.1(2) . . ? C5C C5D C5G 121.5(3) . . ? C5E C5D C5G 119.4(3) . . ? C5D C5E C5F 120.8(3) . . ? C5E C5F C5A 120.0(3) . . ? C5D C5G C5H 114.1(2) . . ? C5G C5H C5I 115.8(2) . . ? C5G C5H B3 122.1(2) . . ? C5I C5H B3 111.1(2) . . ? C5G C5H B1 117.6(3) . . ? C5I C5H B1 61.64(18) . . ? B3 C5H B1 113.6(2) . . ? C5G C5H B2 123.4(2) . . ? C5I C5H B2 111.2(2) . . ? B3 C5H B2 62.6(2) . . ? B1 C5H B2 61.94(19) . . ? C5G C5H B4 115.5(2) . . ? C5I C5H B4 61.39(18) . . ? B3 C5H B4 62.12(19) . . ? B1 C5H B4 113.8(2) . . ? B2 C5H B4 113.7(2) . . ? C5J C5I C5H 117.7(2) . . ? C5J C5I B5 122.4(2) . . ? C5H C5I B5 110.6(2) . . ? C5J C5I B6 121.4(3) . . ? C5H C5I B6 110.4(2) . . ? B5 C5I B6 62.4(2) . . ? C5J C5I B4 118.3(2) . . ? C5H C5I B4 61.14(18) . . ? B5 C5I B4 61.9(2) . . ? B6 C5I B4 113.1(2) . . ? C5J C5I B1 116.4(3) . . ? C5H C5I B1 60.80(18) . . ? B5 C5I B1 113.4(2) . . ? B6 C5I B1 62.2(2) . . ? B4 C5I B1 112.9(2) . . ? N2 C6 C5 125.8(2) . . ? N2 C6 C7 108.8(2) . . ? C5 C6 C7 125.5(2) . . ? C8 C7 C6 107.7(2) . . ? C7 C8 C9 107.6(2) . . ? N2 C9 C10 125.5(2) . . ? N2 C9 C8 108.4(2) . . ? C10 C9 C8 126.1(2) . . ? C9 C10 C1 124.6(2) . 3_667 ? C9 C10 C10A 118.0(2) . . ? C1 C10 C10A 117.4(2) 3_667 . ? C10F C10A C10B 118.0(3) . . ? C10F C10A C10 120.1(3) . . ? C10B C10A C10 121.7(3) . . ? C10C C10B C10A 121.0(3) . . ? C10B C10C C10D 120.8(3) . . ? C10E C10D C10C 118.3(3) . . ? C10E C10D C10G 120.5(3) . . ? C10C C10D C10G 121.2(3) . . ? C10D C10E C10F 120.9(3) . . ? C10A C10F C10E 120.9(3) . . ? C10D C10G C10H 115.3(2) . . ? C10G C10H C10I 116.8(2) . . ? C10G C10H B12 121.1(2) . . ? C10I C10H B12 110.3(2) . . ? C10G C10H B13 123.8(2) . . ? C10I C10H B13 110.5(2) . . ? B12 C10H B13 62.98(19) . . ? C10G C10H B14 118.3(2) . . ? C10I C10H B14 61.33(19) . . ? B12 C10H B14 114.2(2) . . ? B13 C10H B14 62.20(19) . . ? C10G C10H B11 115.3(2) . . ? C10I C10H B11 60.93(18) . . ? B12 C10H B11 61.55(18) . . ? B13 C10H B11 113.2(2) . . ? B14 C10H B11 113.4(2) . . ? C10J C10I C10H 119.6(2) . . ? C10J C10I B15 120.4(3) . . ? C10H C10I B15 110.5(2) . . ? C10J C10I B16 119.7(2) . . ? C10H C10I B16 110.7(2) . . ? B15 C10I B16 63.1(2) . . ? C10J C10I B11 117.7(3) . . ? C10H C10I B11 61.17(18) . . ? B15 C10I B11 113.5(2) . . ? B16 C10I B11 61.8(2) . . ? C10J C10I B14 118.0(3) . . ? C10H C10I B14 60.52(18) . . ? B15 C10I B14 62.5(2) . . ? B16 C10I B14 114.4(2) . . ? B11 C10I B14 112.9(2) . . ? C5H B1 C5I 57.56(17) . . ? C5H B1 B2 59.13(19) . . ? C5I B1 B2 105.7(2) . . ? C5H B1 B7 105.5(3) . . ? C5I B1 B7 105.4(3) . . ? B2 B1 B7 60.3(2) . . ? C5H B1 B6 104.8(2) . . ? C5I B1 B6 58.42(19) . . ? B2 B1 B6 108.5(3) . . ? B7 B1 B6 60.4(2) . . ? C5H B2 B1 58.93(18) . . ? C5H B2 B7 105.0(2) . . ? B1 B2 B7 59.9(2) . . ? C5H B2 B8 104.9(2) . . ? B1 B2 B8 108.0(2) . . ? B7 B2 B8 60.1(2) . . ? C5H B2 B3 58.33(18) . . ? B1 B2 B3 107.6(2) . . ? B7 B2 B3 108.0(2) . . ? B8 B2 B3 60.1(2) . . ? C5H B3 B4 59.46(18) . . ? C5H B3 B2 59.12(19) . . ? B4 B3 B2 108.7(2) . . ? C5H B3 B9 104.9(2) . . ? B4 B3 B9 59.3(2) . . ? B2 B3 B9 108.1(3) . . ? C5H B3 B8 105.3(2) . . ? B4 B3 B8 108.1(2) . . ? B2 B3 B8 59.9(2) . . ? B9 B3 B8 60.3(2) . . ? C5H B4 C5I 57.46(17) . . ? C5H B4 B9 105.2(2) . . ? C5I B4 B9 105.2(2) . . ? C5H B4 B3 58.42(18) . . ? C5I B4 B3 105.0(2) . . ? B9 B4 B3 60.7(2) . . ? C5H B4 B5 104.9(2) . . ? C5I B4 B5 58.56(19) . . ? B9 B4 B5 60.4(2) . . ? B3 B4 B5 108.7(2) . . ? C5I B5 B4 59.51(19) . . ? C5I B5 B9 105.2(2) . . ? B4 B5 B9 59.4(2) . . ? C5I B5 B6 58.8(2) . . ? B4 B5 B6 108.2(2) . . ? B9 B5 B6 107.8(3) . . ? C5I B5 B10 105.1(2) . . ? B4 B5 B10 107.4(2) . . ? B9 B5 B10 59.7(2) . . ? B6 B5 B10 60.0(2) . . ? C5I B6 B5 58.75(19) . . ? C5I B6 B10 105.2(3) . . ? B5 B6 B10 60.1(2) . . ? C5I B6 B1 59.40(18) . . ? B5 B6 B1 108.2(2) . . ? B10 B6 B1 107.6(3) . . ? C5I B6 B7 105.5(2) . . ? B5 B6 B7 108.4(3) . . ? B10 B6 B7 60.1(2) . . ? B1 B6 B7 59.6(2) . . ? B1 B7 B2 59.8(2) . . ? B1 B7 B8 107.8(2) . . ? B2 B7 B8 60.0(2) . . ? B1 B7 B10 107.6(3) . . ? B2 B7 B10 107.8(3) . . ? B8 B7 B10 60.0(2) . . ? B1 B7 B6 60.0(2) . . ? B2 B7 B6 107.8(2) . . ? B8 B7 B6 107.9(3) . . ? B10 B7 B6 59.7(2) . . ? B2 B8 B7 59.9(2) . . ? B2 B8 B10 107.8(3) . . ? B7 B8 B10 60.1(2) . . ? B2 B8 B3 59.95(19) . . ? B7 B8 B3 107.7(2) . . ? B10 B8 B3 107.3(2) . . ? B2 B8 B9 107.7(2) . . ? B7 B8 B9 107.5(3) . . ? B10 B8 B9 59.4(2) . . ? B3 B8 B9 59.8(2) . . ? B4 B9 B10 108.5(3) . . ? B4 B9 B5 60.2(2) . . ? B10 B9 B5 60.3(2) . . ? B4 B9 B3 60.07(19) . . ? B10 B9 B3 107.9(3) . . ? B5 B9 B3 108.1(3) . . ? B4 B9 B8 108.4(3) . . ? B10 B9 B8 60.1(2) . . ? B5 B9 B8 108.5(3) . . ? B3 B9 B8 59.90(19) . . ? B9 B10 B6 107.9(3) . . ? B9 B10 B5 59.9(2) . . ? B6 B10 B5 59.9(2) . . ? B9 B10 B8 60.5(2) . . ? B6 B10 B8 108.2(3) . . ? B5 B10 B8 108.5(3) . . ? B9 B10 B7 108.3(3) . . ? B6 B10 B7 60.2(2) . . ? B5 B10 B7 108.3(3) . . ? B8 B10 B7 59.9(2) . . ? C10I B11 C10H 57.89(17) . . ? C10I B11 B17 105.9(2) . . ? C10H B11 B17 106.0(2) . . ? C10I B11 B12 105.5(2) . . ? C10H B11 B12 58.59(18) . . ? B17 B11 B12 60.98(19) . . ? C10I B11 B16 58.67(19) . . ? C10H B11 B16 105.6(2) . . ? B17 B11 B16 60.6(2) . . ? B12 B11 B16 109.1(2) . . ? C10H B12 B11 59.85(18) . . ? C10H B12 B18 104.9(2) . . ? B11 B12 B18 107.3(2) . . ? C10H B12 B17 105.8(2) . . ? B11 B12 B17 59.45(19) . . ? B18 B12 B17 60.01(19) . . ? C10H B12 B13 58.54(18) . . ? B11 B12 B13 108.2(2) . . ? B18 B12 B13 59.94(18) . . ? B17 B12 B13 108.3(2) . . ? C10H B13 B14 59.06(18) . . ? C10H B13 B18 104.9(2) . . ? B14 B13 B18 108.2(2) . . ? C10H B13 B19 105.2(2) . . ? B14 B13 B19 59.90(19) . . ? B18 B13 B19 60.38(18) . . ? C10H B13 B12 58.48(18) . . ? B14 B13 B12 107.9(2) . . ? B18 B13 B12 59.94(18) . . ? B19 B13 B12 108.2(2) . . ? C10H B14 C10I 58.15(18) . . ? C10H B14 B13 58.74(18) . . ? C10I B14 B13 105.3(2) . . ? C10H B14 B19 105.4(2) . . ? C10I B14 B19 104.4(2) . . ? B13 B14 B19 60.44(19) . . ? C10H B14 B15 104.8(2) . . ? C10I B14 B15 57.78(19) . . ? B13 B14 B15 107.8(2) . . ? B19 B14 B15 59.7(2) . . ? C10I B15 B19 106.2(2) . . ? C10I B15 B14 59.71(19) . . ? B19 B15 B14 60.07(19) . . ? C10I B15 B20 105.3(2) . . ? B19 B15 B20 60.6(2) . . ? B14 B15 B20 108.5(2) . . ? C10I B15 B16 58.93(19) . . ? B19 B15 B16 108.5(2) . . ? B14 B15 B16 108.7(2) . . ? B20 B15 B16 59.6(2) . . ? C10I B16 B11 59.52(19) . . ? C10I B16 B20 105.0(2) . . ? B11 B16 B20 107.7(2) . . ? C10I B16 B17 105.6(2) . . ? B11 B16 B17 59.46(19) . . ? B20 B16 B17 60.4(2) . . ? C10I B16 B15 57.95(19) . . ? B11 B16 B15 107.4(2) . . ? B20 B16 B15 60.2(2) . . ? B17 B16 B15 108.3(2) . . ? B11 B17 B16 59.92(19) . . ? B11 B17 B18 107.3(2) . . ? B16 B17 B18 107.3(2) . . ? B11 B17 B12 59.57(18) . . ? B16 B17 B12 107.5(2) . . ? B18 B17 B12 59.92(18) . . ? B11 B17 B20 107.4(2) . . ? B16 B17 B20 59.6(2) . . ? B18 B17 B20 59.79(19) . . ? B12 B17 B20 107.6(2) . . ? B20 B18 B12 108.0(2) . . ? B20 B18 B13 108.1(2) . . ? B12 B18 B13 60.12(19) . . ? B20 B18 B17 60.2(2) . . ? B12 B18 B17 60.07(19) . . ? B13 B18 B17 108.5(2) . . ? B20 B18 B19 60.2(2) . . ? B12 B18 B19 107.9(2) . . ? B13 B18 B19 59.83(19) . . ? B17 B18 B19 108.5(2) . . ? B15 B19 B14 60.21(19) . . ? B15 B19 B13 107.6(2) . . ? B14 B19 B13 59.66(19) . . ? B15 B19 B20 60.1(2) . . ? B14 B19 B20 108.2(2) . . ? B13 B19 B20 107.6(2) . . ? B15 B19 B18 107.4(2) . . ? B14 B19 B18 107.5(2) . . ? B13 B19 B18 59.79(18) . . ? B20 B19 B18 59.54(19) . . ? B16 B20 B18 107.9(2) . . ? B16 B20 B15 60.2(2) . . ? B18 B20 B15 107.3(2) . . ? B16 B20 B17 60.0(2) . . ? B18 B20 B17 60.03(19) . . ? B15 B20 B17 108.0(2) . . ? B16 B20 B19 108.0(2) . . ? B18 B20 B19 60.27(19) . . ? B15 B20 B19 59.3(2) . . ? B17 B20 B19 108.4(2) . . ? Cl3 Cl1 C14 126(3) . . ? Cl3 Cl1 C12 54.2(17) . . ? C14 Cl1 C12 85.8(16) . . ? Cl3 Cl1 C16 79.3(18) . . ? C14 Cl1 C16 63.9(14) . . ? C12 Cl1 C16 25.4(6) . . ? Cl3 Cl1 C13 137(2) . 3_677 ? C14 Cl1 C13 12.2(14) . 3_677 ? C12 Cl1 C13 92.7(10) . 3_677 ? C16 Cl1 C13 68.8(7) . 3_677 ? C13 Cl2 C15 108.3(12) . . ? C13 Cl2 C11 74.3(10) . . ? C15 Cl2 C11 34.8(7) . . ? C13 Cl2 C14 10.2(10) . 3_677 ? C15 Cl2 C14 98.2(9) . 3_677 ? C11 Cl2 C14 64.1(6) . 3_677 ? Cl1 Cl3 C12 97(2) . . ? Cl1 Cl3 C14 30.9(16) . . ? C12 Cl3 C14 77.3(12) . . ? Cl1 Cl3 C16 79.4(19) . . ? C12 Cl3 C16 17.8(9) . . ? C14 Cl3 C16 59.8(8) . . ? C15 C11 C16 101.5(16) . . ? C15 C11 C16 168.8(16) . 3_677 ? C16 C11 C16 86.2(13) . 3_677 ? C15 C11 C12 74.3(12) . . ? C16 C11 C12 28.9(8) . . ? C16 C11 C12 114.5(12) 3_677 . ? C15 C11 C13 77.1(13) . . ? C16 C11 C13 172.2(12) . . ? C16 C11 C13 94.2(10) 3_677 . ? C12 C11 C13 151.3(10) . . ? C15 C11 Cl2 48.6(11) . . ? C16 C11 Cl2 150.1(13) . . ? C16 C11 Cl2 123.1(10) 3_677 . ? C12 C11 Cl2 122.5(9) . . ? C13 C11 Cl2 28.9(5) . . ? C15 C11 C11 153.3(17) . 3_677 ? C16 C11 C11 52.9(9) . 3_677 ? C16 C11 C11 33.3(6) 3_677 3_677 ? C12 C11 C11 81.3(9) . 3_677 ? C13 C11 C11 127.1(11) . 3_677 ? Cl2 C11 C11 156.0(11) . 3_677 ? C15 C11 C14 117.4(14) . 3_677 ? C16 C11 C14 138.8(13) . 3_677 ? C16 C11 C14 53.4(8) 3_677 3_677 ? C12 C11 C14 167.7(10) . 3_677 ? C13 C11 C14 40.8(6) . 3_677 ? Cl2 C11 C14 69.7(6) . 3_677 ? C11 C11 C14 86.4(8) 3_677 3_677 ? C16 C12 Cl3 138(2) . . ? C16 C12 Cl1 109.2(17) . . ? Cl3 C12 Cl1 29.2(9) . . ? C16 C12 C11 36.6(11) . . ? Cl3 C12 C11 174.2(16) . . ? Cl1 C12 C11 145.5(14) . . ? C16 C12 C14 79.8(14) . . ? Cl3 C12 C14 58.5(13) . . ? Cl1 C12 C14 33.3(8) . . ? C11 C12 C14 115.7(12) . . ? C16 C12 C15 69.5(13) . . ? Cl3 C12 C15 151.6(16) . . ? Cl1 C12 C15 163.6(11) . . ? C11 C12 C15 34.2(6) . . ? C14 C12 C15 149.2(13) . . ? Cl2 C13 C14 163.6(15) . 3_677 ? Cl2 C13 C11 76.8(10) . . ? C14 C13 C11 86.8(10) 3_677 . ? Cl2 C13 C15 44.3(9) . . ? C14 C13 C15 119.4(11) 3_677 . ? C11 C13 C15 33.0(5) . . ? Cl2 C13 Cl1 164.2(12) . 3_677 ? C14 C13 Cl1 8.0(9) 3_677 3_677 ? C11 C13 Cl1 89.6(8) . 3_677 ? C15 C13 Cl1 122.6(9) . 3_677 ? Cl1 C14 C13 160(2) . 3_677 ? Cl1 C14 Cl3 23.6(13) . . ? C13 C14 Cl3 173.1(15) 3_677 . ? Cl1 C14 C12 60.9(16) . . ? C13 C14 C12 128.8(13) 3_677 . ? Cl3 C14 C12 44.2(8) . . ? Cl1 C14 C16 87.8(17) . . ? C13 C14 C16 99.1(12) 3_677 . ? Cl3 C14 C16 74.0(10) . . ? C12 C14 C16 29.9(5) . . ? Cl1 C14 C11 131.8(17) . 3_677 ? C13 C14 C11 52.4(8) 3_677 3_677 ? Cl3 C14 C11 120.7(11) . 3_677 ? C12 C14 C11 76.5(8) . 3_677 ? C16 C14 C11 46.7(6) . 3_677 ? Cl1 C14 Cl2 161(2) . 3_677 ? C13 C14 Cl2 6.2(6) 3_677 3_677 ? Cl3 C14 Cl2 166.9(12) . 3_677 ? C12 C14 Cl2 122.6(10) . 3_677 ? C16 C14 Cl2 92.9(9) . 3_677 ? C11 C14 Cl2 46.2(5) 3_677 3_677 ? C11 C15 Cl2 96.6(15) . . ? C11 C15 C16 41.6(10) . . ? Cl2 C15 C16 138.2(13) . . ? C11 C15 C12 71.5(12) . . ? Cl2 C15 C12 165.7(13) . . ? C16 C15 C12 31.0(6) . . ? C11 C15 C13 69.9(12) . . ? Cl2 C15 C13 27.4(5) . . ? C16 C15 C13 111.2(11) . . ? C12 C15 C13 141.3(12) . . ? C12 C16 C11 114.5(17) . . ? C12 C16 C11 149.5(17) . 3_677 ? C11 C16 C11 93.8(13) . 3_677 ? C12 C16 C15 79.5(13) . . ? C11 C16 C15 36.9(8) . . ? C11 C16 C15 130.2(13) 3_677 . ? C12 C16 C14 70.4(13) . . ? C11 C16 C14 169.0(13) . . ? C11 C16 C14 79.8(10) 3_677 . ? C15 C16 C14 149.9(12) . . ? C12 C16 C16 167.2(18) . 3_677 ? C11 C16 C16 58.0(10) . 3_677 ? C11 C16 C16 35.8(6) 3_677 3_677 ? C15 C16 C16 94.6(11) . 3_677 ? C14 C16 C16 115.2(12) . 3_677 ? C12 C16 Cl3 24.5(12) . . ? C11 C16 Cl3 138.9(14) . . ? C11 C16 Cl3 126.1(11) 3_677 . ? C15 C16 Cl3 103.6(11) . . ? C14 C16 Cl3 46.3(9) . . ? C16 C16 Cl3 160.4(12) 3_677 . ? C12 C16 Cl1 45.4(13) . . ? C11 C16 Cl1 159.4(14) . . ? C11 C16 Cl1 106.8(11) 3_677 . ? C15 C16 Cl1 122.7(12) . . ? C14 C16 Cl1 28.3(7) . . ? C16 C16 Cl1 142.6(12) 3_677 . ? Cl3 C16 Cl1 21.3(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.801 _refine_diff_density_min -0.491 _refine_diff_density_rms 0.066