data_publication_text _publ_contact_author_name 'Kenneth D. Karlin' _publ_contact_author_address ;Department of Chemistry Johns Hopkins University Baltimore, MD 21218 USA ; _publ_contact_author_email karlin@jhu.edu _publ_contact_author_phone '(410) 516-8027' loop_ _publ_author_name _publ_author_address 'Hematian, S.' ;Department of Chemistry Johns Hopkins University Baltimore, MD 21218 USA ; 'Siegler, M. A.' ;Department of Chemistry Johns Hopkins University Baltimore, MD 21218 USA ; 'Karlin, K. D.' ;Department of Chemistry Johns Hopkins University Baltimore, MD 21218 USA ; data_[(tmpa)CuII(Cl)][B(C6F5)4] _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 B F20, C18 H18 Cl Cu N4' _chemical_formula_sum 'C42 H18 B Cl Cu F20 N4' _chemical_formula_weight 1068.40 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 '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' 'N' 'N' 0.0061 0.0033 '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' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 13.08228(15) _cell_length_b 23.1771(3) _cell_length_c 26.3615(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7993.05(17) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 20038 _cell_measurement_theta_min 1.77 _cell_measurement_theta_max 25.97 _exptl_crystal_description block _exptl_crystal_colour 'turquoise blue' _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.776 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4232 _exptl_absorpt_coefficient_mu 0.747 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 0.90 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET) (compiled Jan 8 2009,16:24:04) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'Goniometer KM4/Xcalibur, detector: Sapphire3' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 15.9890 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50400 _diffrn_reflns_av_R_equivalents 0.0550 _diffrn_reflns_av_sigmaI/netI 0.0472 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7840 _reflns_number_gt 5584 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET) (compiled Jan 8 2009,16:24:04) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET) (compiled Jan 8 2009,16:24:04) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET) (compiled Jan 8 2009,16:24:04) ; _computing_structure_solution 'SHELXS-86 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'PLATON (Spek, 2003)' _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. ; _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^)+(0.0387P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7840 _refine_ls_number_parameters 622 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0525 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0699 _refine_ls_wR_factor_gt 0.0665 _refine_ls_goodness_of_fit_ref 0.932 _refine_ls_restrained_S_all 0.932 _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 Cu1 Cu 0.266188(18) 0.018265(10) 0.234469(9) 0.01642(7) Uani 1 1 d . . . Cl1 Cl 0.35237(4) -0.00420(2) 0.30436(2) 0.02582(13) Uani 1 1 d . . . C1 C 0.48003(16) 0.00117(10) 0.18689(9) 0.0237(5) Uani 1 1 d . . . H1 H 0.4984 -0.0185 0.2172 0.028 Uiso 1 1 calc R . . C2 C 0.55149(17) 0.00699(10) 0.14885(9) 0.0291(6) Uani 1 1 d . . . H2 H 0.6187 -0.0077 0.1532 0.035 Uiso 1 1 calc R . . C3 C 0.52439(17) 0.03436(10) 0.10442(9) 0.0294(6) Uani 1 1 d . . . H3 H 0.5725 0.0384 0.0777 0.035 Uiso 1 1 calc R . . C4 C 0.42632(16) 0.05578(10) 0.09930(9) 0.0251(5) Uani 1 1 d . . . H4 H 0.4057 0.0745 0.0689 0.030 Uiso 1 1 calc R . . C5 C 0.35894(15) 0.04952(9) 0.13916(8) 0.0175(5) Uani 1 1 d . . . C6 C 0.25220(14) 0.07404(9) 0.13824(8) 0.0189(5) Uani 1 1 d . . . H6A H 0.2537 0.1146 0.1500 0.023 Uiso 1 1 calc R . . H6B H 0.2257 0.0735 0.1031 0.023 Uiso 1 1 calc R . . C7 C 0.15059(16) -0.01432(9) 0.14669(8) 0.0192(5) Uani 1 1 d . . . H7A H 0.2067 -0.0294 0.1253 0.023 Uiso 1 1 calc R . . H7B H 0.0909 -0.0067 0.1246 0.023 Uiso 1 1 calc R . . C8 C 0.12245(15) -0.05836(9) 0.18621(8) 0.0162(4) Uani 1 1 d . . . C9 C 0.04646(16) -0.09906(9) 0.17924(8) 0.0208(5) Uani 1 1 d . . . H9 H 0.0056 -0.0989 0.1495 0.025 Uiso 1 1 calc R . . C10 C 0.03139(16) -0.13999(9) 0.21667(9) 0.0236(5) Uani 1 1 d . . . H10 H -0.0205 -0.1683 0.2129 0.028 Uiso 1 1 calc R . . C11 C 0.09190(16) -0.13946(9) 0.25937(9) 0.0238(5) Uani 1 1 d . . . H11 H 0.0833 -0.1679 0.2850 0.029 Uiso 1 1 calc R . . C12 C 0.16541(15) -0.09696(9) 0.26440(8) 0.0199(5) Uani 1 1 d . . . H12 H 0.2068 -0.0963 0.2940 0.024 Uiso 1 1 calc R . . C13 C 0.09366(15) 0.07441(9) 0.18783(8) 0.0208(5) Uani 1 1 d . . . H13A H 0.0368 0.0482 0.1971 0.025 Uiso 1 1 calc R . . H13B H 0.0705 0.0992 0.1595 0.025 Uiso 1 1 calc R . . C14 C 0.12077(15) 0.11126(9) 0.23246(9) 0.0210(5) Uani 1 1 d . . . C15 C 0.06689(17) 0.16084(10) 0.24509(10) 0.0289(6) Uani 1 1 d . . . H15 H 0.0144 0.1750 0.2235 0.035 Uiso 1 1 calc R . . C16 C 0.09104(19) 0.18916(10) 0.28960(10) 0.0346(6) Uani 1 1 d . . . H16 H 0.0545 0.2229 0.2992 0.041 Uiso 1 1 calc R . . C17 C 0.16813(19) 0.16832(10) 0.31983(10) 0.0343(6) Uani 1 1 d . . . H17 H 0.1851 0.1872 0.3507 0.041 Uiso 1 1 calc R . . C18 C 0.22046(17) 0.11966(10) 0.30482(9) 0.0278(5) Uani 1 1 d . . . H18 H 0.2748 0.1057 0.3254 0.033 Uiso 1 1 calc R . . C19 C 0.18606(15) 0.33992(9) 0.02358(8) 0.0176(5) Uani 1 1 d . . . C20 C 0.24021(16) 0.32776(9) -0.02062(8) 0.0216(5) Uani 1 1 d . . . C21 C 0.29757(16) 0.36776(10) -0.04686(8) 0.0249(5) Uani 1 1 d . . . C22 C 0.30597(16) 0.42344(10) -0.02950(9) 0.0250(5) Uani 1 1 d . . . C23 C 0.25840(16) 0.43699(9) 0.01569(8) 0.0208(5) Uani 1 1 d . . . C24 C 0.20232(15) 0.39601(9) 0.04054(8) 0.0194(5) Uani 1 1 d . . . C25 C 0.18029(15) 0.28308(9) 0.10862(8) 0.0152(4) Uani 1 1 d . . . C26 C 0.26514(15) 0.24736(9) 0.10558(8) 0.0168(4) Uani 1 1 d . . . C27 C 0.32124(15) 0.22882(9) 0.14662(8) 0.0173(5) Uani 1 1 d . . . C28 C 0.29534(15) 0.24713(9) 0.19430(8) 0.0169(5) Uani 1 1 d . . . C29 C 0.21580(15) 0.28527(9) 0.19966(8) 0.0171(5) Uani 1 1 d . . . C30 C 0.16220(15) 0.30275(9) 0.15740(8) 0.0160(5) Uani 1 1 d . . . C31 C -0.00212(15) 0.32407(9) 0.06956(8) 0.0185(5) Uani 1 1 d . . . C32 C -0.06685(16) 0.29658(9) 0.10351(8) 0.0199(5) Uani 1 1 d . . . C33 C -0.16501(16) 0.31369(10) 0.11461(8) 0.0229(5) Uani 1 1 d . . . C34 C -0.20491(16) 0.36151(10) 0.09098(9) 0.0272(6) Uani 1 1 d . . . C35 C -0.14586(18) 0.39002(10) 0.05646(9) 0.0290(6) Uani 1 1 d . . . C36 C -0.04786(16) 0.37114(9) 0.04612(8) 0.0218(5) Uani 1 1 d . . . C37 C 0.08134(15) 0.23632(9) 0.02686(8) 0.0178(5) Uani 1 1 d . . . C38 C 0.04135(16) 0.23868(9) -0.02218(8) 0.0213(5) Uani 1 1 d . . . C39 C 0.01253(16) 0.19146(10) -0.05000(8) 0.0245(5) Uani 1 1 d . . . C40 C 0.01968(16) 0.13721(9) -0.02911(9) 0.0224(5) Uani 1 1 d . . . C41 C 0.05512(15) 0.13204(9) 0.01963(8) 0.0209(5) Uani 1 1 d . . . C42 C 0.08341(15) 0.18059(9) 0.04590(8) 0.0186(5) Uani 1 1 d . . . B1 B 0.11217(18) 0.29634(10) 0.05709(9) 0.0178(5) Uani 1 1 d . . . N1 N 0.38461(12) 0.02272(7) 0.18230(6) 0.0173(4) Uani 1 1 d . . . N2 N 0.18351(12) 0.03990(7) 0.17144(6) 0.0161(4) Uani 1 1 d . . . N3 N 0.17972(12) -0.05665(7) 0.22854(6) 0.0164(4) Uani 1 1 d . . . N4 N 0.19684(13) 0.09133(7) 0.26189(7) 0.0205(4) Uani 1 1 d . . . F1 F 0.23878(9) 0.27413(5) -0.04107(5) 0.0286(3) Uani 1 1 d . . . F2 F 0.34641(10) 0.35243(6) -0.09002(5) 0.0353(3) Uani 1 1 d . . . F3 F 0.35982(10) 0.46301(6) -0.05494(5) 0.0365(3) Uani 1 1 d . . . F4 F 0.26830(10) 0.49076(5) 0.03467(5) 0.0292(3) Uani 1 1 d . . . F5 F 0.15730(9) 0.41310(5) 0.08461(4) 0.0228(3) Uani 1 1 d . . . F6 F 0.29451(9) 0.22641(5) 0.05977(4) 0.0230(3) Uani 1 1 d . . . F7 F 0.39997(8) 0.19157(5) 0.14051(5) 0.0232(3) Uani 1 1 d . . . F8 F 0.34796(9) 0.22892(5) 0.23513(4) 0.0266(3) Uani 1 1 d . . . F9 F 0.18897(9) 0.30425(5) 0.24605(4) 0.0236(3) Uani 1 1 d . . . F10 F 0.08518(8) 0.34095(5) 0.16666(4) 0.0216(3) Uani 1 1 d . . . F11 F -0.03328(9) 0.24916(5) 0.12880(5) 0.0256(3) Uani 1 1 d . . . F12 F -0.22200(9) 0.28472(6) 0.14888(5) 0.0329(3) Uani 1 1 d . . . F13 F -0.30037(9) 0.37937(6) 0.10184(5) 0.0406(4) Uani 1 1 d . . . F14 F -0.18341(10) 0.43671(6) 0.03225(6) 0.0458(4) Uani 1 1 d . . . F15 F 0.00300(9) 0.40242(5) 0.01067(5) 0.0307(3) Uani 1 1 d . . . F16 F 0.03139(9) 0.29061(5) -0.04516(4) 0.0272(3) Uani 1 1 d . . . F17 F -0.02077(10) 0.19728(5) -0.09828(5) 0.0336(3) Uani 1 1 d . . . F18 F -0.00878(9) 0.09027(5) -0.05556(5) 0.0302(3) Uani 1 1 d . . . F19 F 0.06249(9) 0.07956(5) 0.04119(5) 0.0284(3) Uani 1 1 d . . . F20 F 0.11384(9) 0.17024(5) 0.09449(4) 0.0225(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01691(13) 0.01704(14) 0.01532(13) 0.00171(11) -0.00173(10) 0.00072(11) Cl1 0.0229(3) 0.0351(3) 0.0195(3) 0.0036(2) -0.0059(2) 0.0007(2) C1 0.0226(12) 0.0281(12) 0.0206(12) 0.0008(10) -0.0020(9) 0.0070(10) C2 0.0165(12) 0.0378(15) 0.0330(14) -0.0025(12) 0.0014(10) 0.0055(11) C3 0.0261(13) 0.0363(14) 0.0257(13) 0.0023(11) 0.0084(10) -0.0014(11) C4 0.0248(13) 0.0271(13) 0.0233(12) 0.0063(11) 0.0019(10) -0.0006(10) C5 0.0203(11) 0.0145(11) 0.0177(11) 0.0013(9) -0.0014(9) -0.0022(9) C6 0.0186(11) 0.0164(11) 0.0218(11) 0.0072(9) 0.0014(9) 0.0002(9) C7 0.0222(11) 0.0187(11) 0.0166(11) 0.0019(9) -0.0030(9) -0.0003(10) C8 0.0184(11) 0.0143(11) 0.0158(11) -0.0016(9) 0.0056(9) 0.0025(9) C9 0.0212(11) 0.0198(12) 0.0215(12) -0.0039(10) 0.0017(9) -0.0009(10) C10 0.0236(12) 0.0172(12) 0.0300(13) -0.0019(10) 0.0077(10) -0.0040(10) C11 0.0284(12) 0.0184(12) 0.0246(13) 0.0053(10) 0.0112(10) 0.0016(10) C12 0.0257(12) 0.0180(11) 0.0162(11) 0.0027(10) 0.0045(9) 0.0059(9) C13 0.0157(11) 0.0207(12) 0.0260(13) 0.0071(10) 0.0003(9) 0.0015(9) C14 0.0163(11) 0.0186(11) 0.0280(13) 0.0058(10) 0.0080(10) -0.0041(9) C15 0.0214(12) 0.0222(13) 0.0430(16) 0.0058(12) 0.0115(11) 0.0030(10) C16 0.0341(15) 0.0185(13) 0.0511(17) -0.0024(12) 0.0229(13) 0.0013(11) C17 0.0419(16) 0.0238(14) 0.0372(15) -0.0108(12) 0.0141(12) -0.0076(12) C18 0.0314(13) 0.0248(13) 0.0273(13) -0.0071(11) 0.0039(11) -0.0056(11) C19 0.0204(11) 0.0190(11) 0.0134(11) 0.0021(9) -0.0059(9) 0.0039(9) C20 0.0257(12) 0.0216(12) 0.0174(11) -0.0003(9) -0.0032(9) 0.0071(10) C21 0.0241(12) 0.0373(14) 0.0134(12) 0.0017(11) 0.0029(9) 0.0087(11) C22 0.0267(12) 0.0287(13) 0.0196(12) 0.0107(10) -0.0005(9) 0.0022(11) C23 0.0264(12) 0.0179(11) 0.0181(11) 0.0013(9) -0.0058(9) 0.0013(10) C24 0.0213(11) 0.0256(12) 0.0113(11) 0.0009(9) -0.0016(9) 0.0065(10) C25 0.0194(11) 0.0132(11) 0.0130(11) 0.0006(8) -0.0020(8) -0.0011(9) C26 0.0195(11) 0.0160(11) 0.0148(11) -0.0026(9) -0.0003(9) -0.0036(9) C27 0.0137(11) 0.0150(11) 0.0233(12) 0.0025(9) -0.0019(9) -0.0002(9) C28 0.0157(11) 0.0206(11) 0.0145(11) 0.0058(9) -0.0061(8) -0.0051(9) C29 0.0200(11) 0.0199(11) 0.0115(10) 0.0001(9) -0.0012(9) -0.0059(9) C30 0.0158(11) 0.0153(11) 0.0168(11) 0.0005(9) -0.0001(9) 0.0007(9) C31 0.0229(12) 0.0209(12) 0.0116(11) -0.0038(9) -0.0052(9) 0.0028(9) C32 0.0243(12) 0.0176(12) 0.0178(11) -0.0031(9) -0.0074(9) 0.0013(9) C33 0.0214(12) 0.0306(13) 0.0168(12) -0.0079(10) -0.0006(9) -0.0028(10) C34 0.0173(12) 0.0388(15) 0.0254(13) -0.0097(12) -0.0038(10) 0.0080(11) C35 0.0319(13) 0.0299(13) 0.0251(13) -0.0005(11) -0.0100(10) 0.0138(11) C36 0.0259(12) 0.0244(13) 0.0151(11) -0.0010(10) -0.0022(9) 0.0047(10) C37 0.0183(11) 0.0196(12) 0.0156(11) -0.0018(9) -0.0026(8) 0.0055(9) C38 0.0262(12) 0.0161(12) 0.0215(12) -0.0003(10) -0.0050(10) 0.0063(9) C39 0.0278(13) 0.0302(14) 0.0154(11) -0.0040(10) -0.0093(9) 0.0088(10) C40 0.0214(12) 0.0211(12) 0.0247(12) -0.0111(10) -0.0043(9) 0.0028(10) C41 0.0187(11) 0.0158(12) 0.0281(13) 0.0008(10) -0.0027(9) 0.0025(9) C42 0.0182(11) 0.0240(12) 0.0135(11) -0.0005(10) -0.0058(9) 0.0041(9) B1 0.0223(13) 0.0191(13) 0.0121(12) -0.0012(10) -0.0028(10) 0.0045(11) N1 0.0172(9) 0.0171(9) 0.0177(9) 0.0005(8) 0.0005(7) 0.0015(8) N2 0.0151(9) 0.0134(9) 0.0199(10) 0.0037(8) -0.0008(7) -0.0011(7) N3 0.0200(9) 0.0141(9) 0.0149(9) 0.0009(7) 0.0025(7) 0.0027(7) N4 0.0187(9) 0.0171(10) 0.0255(11) 0.0007(8) 0.0033(8) -0.0007(7) F1 0.0396(8) 0.0259(7) 0.0201(7) -0.0063(6) 0.0044(6) 0.0068(6) F2 0.0396(8) 0.0474(9) 0.0190(7) 0.0023(7) 0.0111(6) 0.0097(7) F3 0.0383(8) 0.0401(8) 0.0311(8) 0.0144(7) 0.0074(6) -0.0027(7) F4 0.0430(8) 0.0204(7) 0.0242(7) 0.0041(6) -0.0024(6) -0.0036(6) F5 0.0343(7) 0.0196(7) 0.0147(6) -0.0030(5) 0.0037(5) -0.0015(5) F6 0.0246(6) 0.0279(7) 0.0165(6) -0.0048(6) -0.0009(5) 0.0062(5) F7 0.0203(6) 0.0222(7) 0.0272(7) 0.0011(6) -0.0041(5) 0.0061(5) F8 0.0281(7) 0.0332(7) 0.0184(7) 0.0077(6) -0.0104(6) 0.0025(6) F9 0.0249(6) 0.0341(8) 0.0117(6) -0.0011(6) -0.0017(5) -0.0024(6) F10 0.0234(7) 0.0246(7) 0.0166(7) -0.0044(5) -0.0025(5) 0.0058(5) F11 0.0279(7) 0.0227(7) 0.0262(7) 0.0040(6) -0.0009(6) 0.0000(6) F12 0.0275(7) 0.0399(8) 0.0314(8) -0.0045(7) 0.0062(6) -0.0075(6) F13 0.0234(7) 0.0585(10) 0.0399(9) -0.0119(8) -0.0019(6) 0.0152(7) F14 0.0433(8) 0.0503(9) 0.0437(9) 0.0142(8) -0.0042(7) 0.0292(7) F15 0.0340(7) 0.0348(8) 0.0233(7) 0.0112(6) -0.0023(6) 0.0117(6) F16 0.0414(8) 0.0220(7) 0.0183(7) -0.0005(6) -0.0121(6) 0.0070(6) F17 0.0493(8) 0.0309(8) 0.0206(7) -0.0080(6) -0.0187(6) 0.0092(6) F18 0.0380(8) 0.0232(7) 0.0295(8) -0.0109(6) -0.0082(6) -0.0006(6) F19 0.0373(7) 0.0164(7) 0.0315(8) 0.0017(6) -0.0070(6) -0.0011(6) F20 0.0314(7) 0.0190(7) 0.0171(6) 0.0026(5) -0.0084(5) 0.0002(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N2 2.0451(17) . ? Cu1 N4 2.0526(17) . ? Cu1 N1 2.0742(16) . ? Cu1 N3 2.0782(16) . ? Cu1 Cl1 2.2219(6) . ? C1 N1 1.350(3) . ? C1 C2 1.378(3) . ? C1 H1 0.9500 . ? C2 C3 1.378(3) . ? C2 H2 0.9500 . ? C3 C4 1.382(3) . ? C3 H3 0.9500 . ? C4 C5 1.379(3) . ? C4 H4 0.9500 . ? C5 N1 1.339(3) . ? C5 C6 1.508(3) . ? C6 N2 1.483(2) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 N2 1.480(3) . ? C7 C8 1.504(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 N3 1.344(3) . ? C8 C9 1.383(3) . ? C9 C10 1.383(3) . ? C9 H9 0.9500 . ? C10 C11 1.376(3) . ? C10 H10 0.9500 . ? C11 C12 1.383(3) . ? C11 H11 0.9500 . ? C12 N3 1.342(3) . ? C12 H12 0.9500 . ? C13 N2 1.486(2) . ? C13 C14 1.496(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 N4 1.344(3) . ? C14 C15 1.388(3) . ? C15 C16 1.381(3) . ? C15 H15 0.9500 . ? C16 C17 1.373(4) . ? C16 H16 0.9500 . ? C17 C18 1.377(3) . ? C17 H17 0.9500 . ? C18 N4 1.344(3) . ? C18 H18 0.9500 . ? C19 C24 1.391(3) . ? C19 C20 1.393(3) . ? C19 B1 1.654(3) . ? C20 F1 1.355(2) . ? C20 C21 1.379(3) . ? C21 F2 1.352(2) . ? C21 C22 1.374(3) . ? C22 F3 1.337(2) . ? C22 C23 1.380(3) . ? C23 F4 1.349(2) . ? C23 C24 1.367(3) . ? C24 F5 1.361(2) . ? C25 C30 1.385(3) . ? C25 C26 1.387(3) . ? C25 B1 1.653(3) . ? C26 F6 1.357(2) . ? C26 C27 1.376(3) . ? C27 F7 1.354(2) . ? C27 C28 1.369(3) . ? C28 F8 1.346(2) . ? C28 C29 1.373(3) . ? C29 F9 1.346(2) . ? C29 C30 1.377(3) . ? C30 F10 1.363(2) . ? C31 C32 1.387(3) . ? C31 C36 1.389(3) . ? C31 B1 1.660(3) . ? C32 F11 1.359(2) . ? C32 C33 1.375(3) . ? C33 F12 1.350(2) . ? C33 C34 1.374(3) . ? C34 F13 1.346(2) . ? C34 C35 1.364(3) . ? C35 F14 1.349(2) . ? C35 C36 1.382(3) . ? C36 F15 1.357(2) . ? C37 C42 1.386(3) . ? C37 C38 1.396(3) . ? C37 B1 1.653(3) . ? C38 F16 1.354(2) . ? C38 C39 1.370(3) . ? C39 F17 1.352(2) . ? C39 C40 1.376(3) . ? C40 F18 1.345(2) . ? C40 C41 1.371(3) . ? C41 F19 1.346(2) . ? C41 C42 1.372(3) . ? C42 F20 1.363(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 N2 Cu1 N4 81.38(7) . . ? N2 Cu1 N1 81.03(6) . . ? N4 Cu1 N1 121.51(7) . . ? N2 Cu1 N3 81.71(6) . . ? N4 Cu1 N3 118.37(6) . . ? N1 Cu1 N3 113.47(6) . . ? N2 Cu1 Cl1 178.32(5) . . ? N4 Cu1 Cl1 97.21(5) . . ? N1 Cu1 Cl1 100.51(5) . . ? N3 Cu1 Cl1 98.21(5) . . ? N1 C1 C2 121.7(2) . . ? N1 C1 H1 119.1 . . ? C2 C1 H1 119.1 . . ? C1 C2 C3 119.3(2) . . ? C1 C2 H2 120.4 . . ? C3 C2 H2 120.4 . . ? C2 C3 C4 119.1(2) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C5 C4 C3 118.7(2) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? N1 C5 C4 122.40(19) . . ? N1 C5 C6 114.88(18) . . ? C4 C5 C6 122.69(19) . . ? N2 C6 C5 110.53(16) . . ? N2 C6 H6A 109.5 . . ? C5 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? N2 C7 C8 110.01(16) . . ? N2 C7 H7A 109.7 . . ? C8 C7 H7A 109.7 . . ? N2 C7 H7B 109.7 . . ? C8 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? N3 C8 C9 122.08(19) . . ? N3 C8 C7 114.73(17) . . ? C9 C8 C7 123.15(19) . . ? C8 C9 C10 118.4(2) . . ? C8 C9 H9 120.8 . . ? C10 C9 H9 120.8 . . ? C11 C10 C9 119.7(2) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? C10 C11 C12 119.0(2) . . ? C10 C11 H11 120.5 . . ? C12 C11 H11 120.5 . . ? N3 C12 C11 121.7(2) . . ? N3 C12 H12 119.2 . . ? C11 C12 H12 119.2 . . ? N2 C13 C14 110.39(16) . . ? N2 C13 H13A 109.6 . . ? C14 C13 H13A 109.6 . . ? N2 C13 H13B 109.6 . . ? C14 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? N4 C14 C15 121.5(2) . . ? N4 C14 C13 115.67(18) . . ? C15 C14 C13 122.7(2) . . ? C16 C15 C14 118.7(2) . . ? C16 C15 H15 120.6 . . ? C14 C15 H15 120.6 . . ? C17 C16 C15 119.6(2) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C16 C17 C18 119.1(2) . . ? C16 C17 H17 120.4 . . ? C18 C17 H17 120.4 . . ? N4 C18 C17 121.8(2) . . ? N4 C18 H18 119.1 . . ? C17 C18 H18 119.1 . . ? C24 C19 C20 112.36(19) . . ? C24 C19 B1 119.24(18) . . ? C20 C19 B1 128.36(19) . . ? F1 C20 C21 115.14(18) . . ? F1 C20 C19 120.77(19) . . ? C21 C20 C19 124.1(2) . . ? F2 C21 C22 119.3(2) . . ? F2 C21 C20 120.2(2) . . ? C22 C21 C20 120.5(2) . . ? F3 C22 C21 121.3(2) . . ? F3 C22 C23 121.0(2) . . ? C21 C22 C23 117.7(2) . . ? F4 C23 C24 121.02(19) . . ? F4 C23 C22 119.15(19) . . ? C24 C23 C22 119.8(2) . . ? F5 C24 C23 116.04(19) . . ? F5 C24 C19 118.68(18) . . ? C23 C24 C19 125.3(2) . . ? C30 C25 C26 112.77(18) . . ? C30 C25 B1 127.56(18) . . ? C26 C25 B1 119.66(18) . . ? F6 C26 C27 115.90(18) . . ? F6 C26 C25 119.45(18) . . ? C27 C26 C25 124.59(19) . . ? F7 C27 C28 119.69(18) . . ? F7 C27 C26 120.76(19) . . ? C28 C27 C26 119.53(19) . . ? F8 C28 C27 120.70(18) . . ? F8 C28 C29 120.49(19) . . ? C27 C28 C29 118.80(19) . . ? F9 C29 C28 120.11(18) . . ? F9 C29 C30 120.39(18) . . ? C28 C29 C30 119.48(19) . . ? F10 C30 C29 114.98(18) . . ? F10 C30 C25 120.43(17) . . ? C29 C30 C25 124.56(19) . . ? C32 C31 C36 112.63(19) . . ? C32 C31 B1 119.99(18) . . ? C36 C31 B1 127.13(19) . . ? F11 C32 C33 115.51(19) . . ? F11 C32 C31 119.40(18) . . ? C33 C32 C31 125.1(2) . . ? F12 C33 C34 119.64(19) . . ? F12 C33 C32 121.0(2) . . ? C34 C33 C32 119.4(2) . . ? F13 C34 C35 121.2(2) . . ? F13 C34 C33 120.3(2) . . ? C35 C34 C33 118.5(2) . . ? F14 C35 C34 119.9(2) . . ? F14 C35 C36 119.9(2) . . ? C34 C35 C36 120.2(2) . . ? F15 C36 C35 114.94(19) . . ? F15 C36 C31 120.97(18) . . ? C35 C36 C31 124.1(2) . . ? C42 C37 C38 112.29(19) . . ? C42 C37 B1 127.22(18) . . ? C38 C37 B1 120.33(18) . . ? F16 C38 C39 116.35(18) . . ? F16 C38 C37 119.05(18) . . ? C39 C38 C37 124.6(2) . . ? F17 C39 C38 120.9(2) . . ? F17 C39 C40 119.3(2) . . ? C38 C39 C40 119.79(19) . . ? F18 C40 C41 120.6(2) . . ? F18 C40 C39 120.9(2) . . ? C41 C40 C39 118.5(2) . . ? F19 C41 C40 119.92(19) . . ? F19 C41 C42 120.58(19) . . ? C40 C41 C42 119.5(2) . . ? F20 C42 C41 114.13(18) . . ? F20 C42 C37 120.67(18) . . ? C41 C42 C37 125.19(19) . . ? C37 B1 C25 111.78(17) . . ? C37 B1 C19 113.52(17) . . ? C25 B1 C19 103.73(16) . . ? C37 B1 C31 101.62(16) . . ? C25 B1 C31 113.25(17) . . ? C19 B1 C31 113.31(17) . . ? C5 N1 C1 118.67(18) . . ? C5 N1 Cu1 113.52(13) . . ? C1 N1 Cu1 127.80(14) . . ? C7 N2 C6 111.68(16) . . ? C7 N2 C13 110.80(15) . . ? C6 N2 C13 111.33(15) . . ? C7 N2 Cu1 107.69(12) . . ? C6 N2 Cu1 106.84(11) . . ? C13 N2 Cu1 108.30(13) . . ? C12 N3 C8 119.10(18) . . ? C12 N3 Cu1 127.18(14) . . ? C8 N3 Cu1 112.98(13) . . ? C14 N4 C18 119.22(19) . . ? C14 N4 Cu1 114.06(14) . . ? C18 N4 Cu1 126.72(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -1.5(4) . . . . ? C1 C2 C3 C4 0.6(4) . . . . ? C2 C3 C4 C5 0.6(3) . . . . ? C3 C4 C5 N1 -1.0(3) . . . . ? C3 C4 C5 C6 176.8(2) . . . . ? N1 C5 C6 N2 -28.8(2) . . . . ? C4 C5 C6 N2 153.2(2) . . . . ? N2 C7 C8 N3 -35.4(2) . . . . ? N2 C7 C8 C9 147.03(18) . . . . ? N3 C8 C9 C10 -1.7(3) . . . . ? C7 C8 C9 C10 175.74(19) . . . . ? C8 C9 C10 C11 -0.3(3) . . . . ? C9 C10 C11 C12 1.4(3) . . . . ? C10 C11 C12 N3 -0.6(3) . . . . ? N2 C13 C14 N4 -26.8(2) . . . . ? N2 C13 C14 C15 157.46(18) . . . . ? N4 C14 C15 C16 -1.6(3) . . . . ? C13 C14 C15 C16 173.9(2) . . . . ? C14 C15 C16 C17 0.9(3) . . . . ? C15 C16 C17 C18 0.5(3) . . . . ? C16 C17 C18 N4 -1.3(3) . . . . ? C24 C19 C20 F1 175.96(17) . . . . ? B1 C19 C20 F1 -1.7(3) . . . . ? C24 C19 C20 C21 -4.5(3) . . . . ? B1 C19 C20 C21 177.8(2) . . . . ? F1 C20 C21 F2 0.7(3) . . . . ? C19 C20 C21 F2 -178.88(19) . . . . ? F1 C20 C21 C22 -179.15(19) . . . . ? C19 C20 C21 C22 1.3(3) . . . . ? F2 C21 C22 F3 1.3(3) . . . . ? C20 C21 C22 F3 -178.84(19) . . . . ? F2 C21 C22 C23 -177.53(18) . . . . ? C20 C21 C22 C23 2.3(3) . . . . ? F3 C22 C23 F4 -1.2(3) . . . . ? C21 C22 C23 F4 177.64(18) . . . . ? F3 C22 C23 C24 178.89(18) . . . . ? C21 C22 C23 C24 -2.3(3) . . . . ? F4 C23 C24 F5 0.6(3) . . . . ? C22 C23 C24 F5 -179.49(18) . . . . ? F4 C23 C24 C19 178.69(18) . . . . ? C22 C23 C24 C19 -1.4(3) . . . . ? C20 C19 C24 F5 -177.37(17) . . . . ? B1 C19 C24 F5 0.5(3) . . . . ? C20 C19 C24 C23 4.6(3) . . . . ? B1 C19 C24 C23 -177.51(19) . . . . ? C30 C25 C26 F6 -177.65(17) . . . . ? B1 C25 C26 F6 3.7(3) . . . . ? C30 C25 C26 C27 5.3(3) . . . . ? B1 C25 C26 C27 -173.28(19) . . . . ? F6 C26 C27 F7 -0.5(3) . . . . ? C25 C26 C27 F7 176.59(18) . . . . ? F6 C26 C27 C28 -178.81(18) . . . . ? C25 C26 C27 C28 -1.7(3) . . . . ? F7 C27 C28 F8 0.6(3) . . . . ? C26 C27 C28 F8 178.95(18) . . . . ? F7 C27 C28 C29 179.49(17) . . . . ? C26 C27 C28 C29 -2.2(3) . . . . ? F8 C28 C29 F9 -0.8(3) . . . . ? C27 C28 C29 F9 -179.65(18) . . . . ? F8 C28 C29 C30 -179.19(18) . . . . ? C27 C28 C29 C30 2.0(3) . . . . ? F9 C29 C30 F10 2.1(3) . . . . ? C28 C29 C30 F10 -179.55(17) . . . . ? F9 C29 C30 C25 -176.16(18) . . . . ? C28 C29 C30 C25 2.2(3) . . . . ? C26 C25 C30 F10 176.27(17) . . . . ? B1 C25 C30 F10 -5.3(3) . . . . ? C26 C25 C30 C29 -5.6(3) . . . . ? B1 C25 C30 C29 172.9(2) . . . . ? C36 C31 C32 F11 178.98(18) . . . . ? B1 C31 C32 F11 4.3(3) . . . . ? C36 C31 C32 C33 -1.5(3) . . . . ? B1 C31 C32 C33 -176.2(2) . . . . ? F11 C32 C33 F12 0.6(3) . . . . ? C31 C32 C33 F12 -178.94(19) . . . . ? F11 C32 C33 C34 179.57(18) . . . . ? C31 C32 C33 C34 0.0(3) . . . . ? F12 C33 C34 F13 -0.1(3) . . . . ? C32 C33 C34 F13 -179.13(19) . . . . ? F12 C33 C34 C35 -179.9(2) . . . . ? C32 C33 C34 C35 1.1(3) . . . . ? F13 C34 C35 F14 -0.6(3) . . . . ? C33 C34 C35 F14 179.2(2) . . . . ? F13 C34 C35 C36 179.6(2) . . . . ? C33 C34 C35 C36 -0.6(3) . . . . ? F14 C35 C36 F15 -0.7(3) . . . . ? C34 C35 C36 F15 179.2(2) . . . . ? F14 C35 C36 C31 179.1(2) . . . . ? C34 C35 C36 C31 -1.1(4) . . . . ? C32 C31 C36 F15 -178.22(18) . . . . ? B1 C31 C36 F15 -4.0(3) . . . . ? C32 C31 C36 C35 2.0(3) . . . . ? B1 C31 C36 C35 176.2(2) . . . . ? C42 C37 C38 F16 177.85(17) . . . . ? B1 C37 C38 F16 2.2(3) . . . . ? C42 C37 C38 C39 -3.5(3) . . . . ? B1 C37 C38 C39 -179.2(2) . . . . ? F16 C38 C39 F17 2.0(3) . . . . ? C37 C38 C39 F17 -176.6(2) . . . . ? F16 C38 C39 C40 -179.52(19) . . . . ? C37 C38 C39 C40 1.8(3) . . . . ? F17 C39 C40 F18 -2.0(3) . . . . ? C38 C39 C40 F18 179.56(19) . . . . ? F17 C39 C40 C41 178.99(19) . . . . ? C38 C39 C40 C41 0.5(3) . . . . ? F18 C40 C41 F19 0.6(3) . . . . ? C39 C40 C41 F19 179.66(19) . . . . ? F18 C40 C41 C42 -179.80(18) . . . . ? C39 C40 C41 C42 -0.7(3) . . . . ? F19 C41 C42 F20 -2.6(3) . . . . ? C40 C41 C42 F20 177.76(18) . . . . ? F19 C41 C42 C37 178.26(19) . . . . ? C40 C41 C42 C37 -1.3(3) . . . . ? C38 C37 C42 F20 -175.75(18) . . . . ? B1 C37 C42 F20 -0.4(3) . . . . ? C38 C37 C42 C41 3.3(3) . . . . ? B1 C37 C42 C41 178.6(2) . . . . ? C42 C37 B1 C25 17.4(3) . . . . ? C38 C37 B1 C25 -167.63(19) . . . . ? C42 C37 B1 C19 134.3(2) . . . . ? C38 C37 B1 C19 -50.7(3) . . . . ? C42 C37 B1 C31 -103.7(2) . . . . ? C38 C37 B1 C31 71.3(2) . . . . ? C30 C25 B1 C37 -128.4(2) . . . . ? C26 C25 B1 C37 50.0(3) . . . . ? C30 C25 B1 C19 109.0(2) . . . . ? C26 C25 B1 C19 -72.7(2) . . . . ? C30 C25 B1 C31 -14.3(3) . . . . ? C26 C25 B1 C31 164.09(18) . . . . ? C24 C19 B1 C37 168.38(18) . . . . ? C20 C19 B1 C37 -14.1(3) . . . . ? C24 C19 B1 C25 -70.1(2) . . . . ? C20 C19 B1 C25 107.4(2) . . . . ? C24 C19 B1 C31 53.1(2) . . . . ? C20 C19 B1 C31 -129.4(2) . . . . ? C32 C31 B1 C37 67.5(2) . . . . ? C36 C31 B1 C37 -106.3(2) . . . . ? C32 C31 B1 C25 -52.6(3) . . . . ? C36 C31 B1 C25 133.6(2) . . . . ? C32 C31 B1 C19 -170.37(18) . . . . ? C36 C31 B1 C19 15.8(3) . . . . ? C4 C5 N1 C1 0.1(3) . . . . ? C6 C5 N1 C1 -177.86(18) . . . . ? C4 C5 N1 Cu1 -178.54(17) . . . . ? C6 C5 N1 Cu1 3.5(2) . . . . ? C2 C1 N1 C5 1.1(3) . . . . ? C2 C1 N1 Cu1 179.60(16) . . . . ? N2 Cu1 N1 C5 15.08(14) . . . . ? N4 Cu1 N1 C5 -58.97(16) . . . . ? N3 Cu1 N1 C5 91.92(15) . . . . ? Cl1 Cu1 N1 C5 -164.25(13) . . . . ? N2 Cu1 N1 C1 -163.44(19) . . . . ? N4 Cu1 N1 C1 122.51(18) . . . . ? N3 Cu1 N1 C1 -86.60(18) . . . . ? Cl1 Cu1 N1 C1 17.23(18) . . . . ? C8 C7 N2 C6 155.19(16) . . . . ? C8 C7 N2 C13 -80.1(2) . . . . ? C8 C7 N2 Cu1 38.19(18) . . . . ? C5 C6 N2 C7 -78.5(2) . . . . ? C5 C6 N2 C13 157.04(17) . . . . ? C5 C6 N2 Cu1 38.98(19) . . . . ? C14 C13 N2 C7 152.38(17) . . . . ? C14 C13 N2 C6 -82.7(2) . . . . ? C14 C13 N2 Cu1 34.48(19) . . . . ? N4 Cu1 N2 C7 -145.11(13) . . . . ? N1 Cu1 N2 C7 90.90(13) . . . . ? N3 Cu1 N2 C7 -24.60(12) . . . . ? N4 Cu1 N2 C6 94.78(13) . . . . ? N1 Cu1 N2 C6 -29.21(12) . . . . ? N3 Cu1 N2 C6 -144.70(13) . . . . ? N4 Cu1 N2 C13 -25.24(12) . . . . ? N1 Cu1 N2 C13 -149.23(13) . . . . ? N3 Cu1 N2 C13 95.27(13) . . . . ? C11 C12 N3 C8 -1.3(3) . . . . ? C11 C12 N3 Cu1 168.09(15) . . . . ? C9 C8 N3 C12 2.5(3) . . . . ? C7 C8 N3 C12 -175.13(17) . . . . ? C9 C8 N3 Cu1 -168.35(15) . . . . ? C7 C8 N3 Cu1 14.0(2) . . . . ? N2 Cu1 N3 C12 -163.62(17) . . . . ? N4 Cu1 N3 C12 -88.14(17) . . . . ? N1 Cu1 N3 C12 119.98(16) . . . . ? Cl1 Cu1 N3 C12 14.69(16) . . . . ? N2 Cu1 N3 C8 6.35(13) . . . . ? N4 Cu1 N3 C8 81.82(15) . . . . ? N1 Cu1 N3 C8 -70.06(14) . . . . ? Cl1 Cu1 N3 C8 -175.34(12) . . . . ? C15 C14 N4 C18 0.8(3) . . . . ? C13 C14 N4 C18 -174.97(18) . . . . ? C15 C14 N4 Cu1 -178.99(15) . . . . ? C13 C14 N4 Cu1 5.2(2) . . . . ? C17 C18 N4 C14 0.7(3) . . . . ? C17 C18 N4 Cu1 -179.57(16) . . . . ? N2 Cu1 N4 C14 11.72(14) . . . . ? N1 Cu1 N4 C14 85.59(15) . . . . ? N3 Cu1 N4 C14 -63.94(16) . . . . ? Cl1 Cu1 N4 C14 -167.35(13) . . . . ? N2 Cu1 N4 C18 -168.04(18) . . . . ? N1 Cu1 N4 C18 -94.17(18) . . . . ? N3 Cu1 N4 C18 116.30(17) . . . . ? Cl1 Cu1 N4 C18 12.88(18) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.343 _refine_diff_density_min -0.581 _refine_diff_density_rms 0.057 _iucr_refine_instructions_details ; TITL x0521 CELL 0.71073 13.08228 23.1771 26.3615 90.000 90.000 90.000 ZERR 8 0.00015 0.0003 0.0003 0.0000 0.0000 0.0000 LATT 1 SYMM 0.50000 - X , - Y , 0.50000 + Z SYMM 0.50000 + X , 0.50000 - Y , - Z SYMM - X , 0.50000 + Y , 0.50000 - Z SFAC C H B CL CU F N UNIT 336 144 8 8 8 160 32 TEMP -163 ACTA HTAB BOND BOND $H CONF WPDB L.S. 6 FMAP 2 PLAN 10 OMIT -2 52 WGHT 0.038700 FVAR 1.08674 CU1 5 0.266188 0.018265 0.234469 11.00000 0.01691 0.01704 = 0.01532 0.00171 -0.00173 0.00072 CL1 4 0.352375 -0.004202 0.304358 11.00000 0.02290 0.03510 = 0.01947 0.00363 -0.00593 0.00066 C1 1 0.480032 0.001175 0.186888 11.00000 0.02256 0.02812 = 0.02056 0.00076 -0.00202 0.00699 AFIX 43 H1 2 0.498392 -0.018519 0.217152 11.00000 -1.20000 AFIX 0 C2 1 0.551487 0.006990 0.148847 11.00000 0.01651 0.03779 = 0.03301 -0.00251 0.00145 0.00550 AFIX 43 H2 2 0.618711 -0.007703 0.153188 11.00000 -1.20000 AFIX 0 C3 1 0.524388 0.034356 0.104423 11.00000 0.02609 0.03631 = 0.02574 0.00228 0.00838 -0.00137 AFIX 43 H3 2 0.572490 0.038444 0.077666 11.00000 -1.20000 AFIX 0 C4 1 0.426318 0.055777 0.099300 11.00000 0.02479 0.02707 = 0.02331 0.00632 0.00187 -0.00057 AFIX 43 H4 2 0.405719 0.074459 0.068896 11.00000 -1.20000 AFIX 0 C5 1 0.358943 0.049518 0.139157 11.00000 0.02025 0.01454 = 0.01765 0.00125 -0.00136 -0.00219 C6 1 0.252201 0.074037 0.138245 11.00000 0.01863 0.01637 = 0.02183 0.00716 0.00143 0.00023 AFIX 23 H6A 2 0.253708 0.114606 0.149974 11.00000 -1.20000 H6B 2 0.225730 0.073539 0.103065 11.00000 -1.20000 AFIX 0 C7 1 0.150586 -0.014323 0.146692 11.00000 0.02217 0.01874 = 0.01656 0.00187 -0.00300 -0.00026 AFIX 23 H7A 2 0.206658 -0.029441 0.125260 11.00000 -1.20000 H7B 2 0.090930 -0.006659 0.124591 11.00000 -1.20000 AFIX 0 C8 1 0.122447 -0.058362 0.186213 11.00000 0.01839 0.01430 = 0.01577 -0.00165 0.00564 0.00250 C9 1 0.046460 -0.099062 0.179244 11.00000 0.02118 0.01983 = 0.02150 -0.00390 0.00166 -0.00090 AFIX 43 H9 2 0.005588 -0.098915 0.149457 11.00000 -1.20000 AFIX 0 C10 1 0.031392 -0.139985 0.216674 11.00000 0.02358 0.01719 = 0.03003 -0.00187 0.00766 -0.00400 AFIX 43 H10 2 -0.020504 -0.168338 0.212931 11.00000 -1.20000 AFIX 0 C11 1 0.091900 -0.139458 0.259369 11.00000 0.02835 0.01839 = 0.02462 0.00526 0.01120 0.00157 AFIX 43 H11 2 0.083310 -0.167861 0.285000 11.00000 -1.20000 AFIX 0 C12 1 0.165411 -0.096957 0.264404 11.00000 0.02565 0.01802 = 0.01618 0.00274 0.00449 0.00592 AFIX 43 H12 2 0.206830 -0.096273 0.293998 11.00000 -1.20000 AFIX 0 C13 1 0.093656 0.074414 0.187833 11.00000 0.01570 0.02070 = 0.02604 0.00707 0.00026 0.00146 AFIX 23 H13A 2 0.036844 0.048216 0.197051 11.00000 -1.20000 H13B 2 0.070467 0.099188 0.159487 11.00000 -1.20000 AFIX 0 C14 1 0.120773 0.111262 0.232462 11.00000 0.01631 0.01862 = 0.02798 0.00584 0.00799 -0.00407 C15 1 0.066893 0.160839 0.245086 11.00000 0.02143 0.02217 = 0.04303 0.00581 0.01150 0.00300 AFIX 43 H15 2 0.014413 0.175008 0.223517 11.00000 -1.20000 AFIX 0 C16 1 0.091043 0.189164 0.289599 11.00000 0.03407 0.01850 = 0.05109 -0.00235 0.02293 0.00131 AFIX 43 H16 2 0.054543 0.222858 0.299243 11.00000 -1.20000 AFIX 0 C17 1 0.168133 0.168323 0.319826 11.00000 0.04187 0.02378 = 0.03717 -0.01085 0.01412 -0.00759 AFIX 43 H17 2 0.185149 0.187213 0.350673 11.00000 -1.20000 AFIX 0 C18 1 0.220462 0.119658 0.304822 11.00000 0.03137 0.02480 = 0.02734 -0.00715 0.00393 -0.00563 AFIX 43 H18 2 0.274756 0.105728 0.325381 11.00000 -1.20000 AFIX 0 C19 1 0.186057 0.339924 0.023584 11.00000 0.02045 0.01899 = 0.01342 0.00212 -0.00593 0.00394 C20 1 0.240212 0.327755 -0.020620 11.00000 0.02571 0.02160 = 0.01739 -0.00026 -0.00322 0.00706 C21 1 0.297567 0.367761 -0.046861 11.00000 0.02405 0.03726 = 0.01344 0.00174 0.00291 0.00867 C22 1 0.305966 0.423438 -0.029503 11.00000 0.02669 0.02868 = 0.01965 0.01066 -0.00054 0.00222 C23 1 0.258402 0.436988 0.015688 11.00000 0.02636 0.01792 = 0.01813 0.00127 -0.00575 0.00135 C24 1 0.202318 0.396008 0.040540 11.00000 0.02133 0.02561 = 0.01130 0.00093 -0.00162 0.00653 C25 1 0.180287 0.283078 0.108620 11.00000 0.01944 0.01318 = 0.01295 0.00058 -0.00197 -0.00105 C26 1 0.265142 0.247363 0.105576 11.00000 0.01950 0.01600 = 0.01483 -0.00263 -0.00033 -0.00365 C27 1 0.321243 0.228821 0.146620 11.00000 0.01373 0.01496 = 0.02331 0.00247 -0.00188 -0.00017 C28 1 0.295344 0.247132 0.194300 11.00000 0.01569 0.02061 = 0.01448 0.00581 -0.00606 -0.00514 C29 1 0.215799 0.285266 0.199663 11.00000 0.01998 0.01986 = 0.01154 0.00011 -0.00121 -0.00589 C30 1 0.162199 0.302750 0.157396 11.00000 0.01582 0.01530 = 0.01678 0.00051 -0.00006 0.00070 C31 1 -0.002124 0.324065 0.069564 11.00000 0.02291 0.02090 = 0.01164 -0.00380 -0.00523 0.00279 C32 1 -0.066849 0.296583 0.103513 11.00000 0.02434 0.01756 = 0.01775 -0.00313 -0.00742 0.00131 C33 1 -0.165007 0.313691 0.114607 11.00000 0.02135 0.03058 = 0.01678 -0.00791 -0.00062 -0.00282 C34 1 -0.204906 0.361514 0.090984 11.00000 0.01726 0.03884 = 0.02543 -0.00972 -0.00383 0.00797 C35 1 -0.145863 0.390024 0.056461 11.00000 0.03195 0.02985 = 0.02506 -0.00051 -0.01002 0.01376 C36 1 -0.047863 0.371144 0.046121 11.00000 0.02595 0.02443 = 0.01514 -0.00096 -0.00218 0.00467 C37 1 0.081345 0.236319 0.026863 11.00000 0.01833 0.01956 = 0.01561 -0.00184 -0.00261 0.00547 C38 1 0.041352 0.238680 -0.022176 11.00000 0.02618 0.01615 = 0.02154 -0.00034 -0.00501 0.00625 C39 1 0.012527 0.191464 -0.050001 11.00000 0.02780 0.03024 = 0.01540 -0.00396 -0.00927 0.00884 C40 1 0.019683 0.137211 -0.029110 11.00000 0.02137 0.02111 = 0.02472 -0.01105 -0.00426 0.00284 C41 1 0.055123 0.132041 0.019630 11.00000 0.01872 0.01576 = 0.02811 0.00077 -0.00273 0.00253 C42 1 0.083415 0.180593 0.045899 11.00000 0.01817 0.02400 = 0.01351 -0.00049 -0.00579 0.00410 B1 3 0.112167 0.296343 0.057094 11.00000 0.02230 0.01908 = 0.01211 -0.00120 -0.00285 0.00453 N1 7 0.384611 0.022719 0.182300 11.00000 0.01718 0.01712 = 0.01765 0.00048 0.00053 0.00153 N2 7 0.183508 0.039899 0.171437 11.00000 0.01508 0.01337 = 0.01989 0.00367 -0.00076 -0.00113 N3 7 0.179717 -0.056648 0.228536 11.00000 0.02003 0.01413 = 0.01490 0.00094 0.00248 0.00274 N4 7 0.196843 0.091325 0.261893 11.00000 0.01875 0.01713 = 0.02548 0.00070 0.00330 -0.00068 F1 6 0.238783 0.274127 -0.041067 11.00000 0.03964 0.02589 = 0.02013 -0.00629 0.00439 0.00685 F2 6 0.346410 0.352427 -0.090020 11.00000 0.03960 0.04737 = 0.01901 0.00232 0.01109 0.00967 F3 6 0.359823 0.463012 -0.054936 11.00000 0.03828 0.04013 = 0.03115 0.01443 0.00739 -0.00273 F4 6 0.268298 0.490758 0.034674 11.00000 0.04297 0.02037 = 0.02421 0.00413 -0.00235 -0.00360 F5 6 0.157298 0.413097 0.084614 11.00000 0.03429 0.01956 = 0.01466 -0.00299 0.00369 -0.00151 F6 6 0.294513 0.226415 0.059771 11.00000 0.02460 0.02795 = 0.01647 -0.00483 -0.00093 0.00623 F7 6 0.399972 0.191570 0.140508 11.00000 0.02029 0.02218 = 0.02718 0.00109 -0.00406 0.00607 F8 6 0.347965 0.228919 0.235132 11.00000 0.02811 0.03325 = 0.01842 0.00766 -0.01035 0.00246 F9 6 0.188967 0.304248 0.246045 11.00000 0.02492 0.03412 = 0.01171 -0.00106 -0.00170 -0.00239 F10 6 0.085177 0.340951 0.166662 11.00000 0.02338 0.02464 = 0.01664 -0.00440 -0.00250 0.00585 F11 6 -0.033278 0.249158 0.128805 11.00000 0.02793 0.02270 = 0.02620 0.00403 -0.00090 -0.00002 F12 6 -0.222004 0.284723 0.148876 11.00000 0.02748 0.03994 = 0.03135 -0.00450 0.00617 -0.00751 F13 6 -0.300372 0.379372 0.101841 11.00000 0.02338 0.05846 = 0.03994 -0.01195 -0.00193 0.01519 F14 6 -0.183408 0.436707 0.032247 11.00000 0.04332 0.05034 = 0.04373 0.01420 -0.00422 0.02923 F15 6 0.003004 0.402421 0.010667 11.00000 0.03404 0.03480 = 0.02328 0.01120 -0.00229 0.01168 F16 6 0.031385 0.290610 -0.045160 11.00000 0.04144 0.02200 = 0.01826 -0.00049 -0.01215 0.00700 F17 6 -0.020771 0.197278 -0.098284 11.00000 0.04928 0.03095 = 0.02056 -0.00796 -0.01872 0.00922 F18 6 -0.008781 0.090271 -0.055561 11.00000 0.03805 0.02319 = 0.02946 -0.01087 -0.00818 -0.00057 F19 6 0.062485 0.079559 0.041186 11.00000 0.03727 0.01642 = 0.03151 0.00165 -0.00695 -0.00107 F20 6 0.113844 0.170244 0.094493 11.00000 0.03139 0.01903 = 0.01705 0.00260 -0.00838 0.00015 HKLF 4 REM x0521 REM R1 = 0.0305 for 5584 Fo > 4sig(Fo) and 0.0525 for all 7840 data REM 622 parameters refined using 0 restraints END WGHT 0.0387 0.0000 REM Highest difference peak 0.343, deepest hole -0.581, 1-sigma level 0.057 Q1 1 0.1955 -0.0231 0.2309 11.00000 0.05 0.34 Q2 1 0.3134 0.0087 0.2701 11.00000 0.05 0.32 Q3 1 0.3245 0.0179 0.1972 11.00000 0.05 0.30 Q4 1 0.2379 0.2517 0.1985 11.00000 0.05 0.29 Q5 1 0.2361 0.0271 0.1911 11.00000 0.05 0.29 Q6 1 0.1508 0.2909 0.0844 11.00000 0.05 0.27 Q7 1 0.1766 0.1077 0.2422 11.00000 0.05 0.27 Q8 1 0.2373 0.0679 0.2405 11.00000 0.05 0.27 Q9 1 0.4976 -0.0043 0.1590 11.00000 0.05 0.25 Q10 1 0.1026 0.2081 0.0322 11.00000 0.05 0.25 ;