# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1320 data_global _publ_contact_author_name 'Kimoon Kim' _publ_contact_author_address ; Department of Chemistry Pohang University of Science and Technology San 31 Hyojadong Pohang 790-784 Republic of Korea ; _publ_contact_author_email 'kkim@vision.postech.ac.kr' _publ_contact_author_fax '+82-562-279-8129' _publ_contact_author_phone '+82-562-279-2113' _publ_requested_journal 'J. Chem Soc. Dalton Trans.' data_1 _audit_creation_method SHELXL _chemical_name_systematic ; 1,3,5-tris(bis(pyrid-2-ylmethyl)amino)methyl-2,4,6- triethyl-benzene ; _chemical_name_common 'L' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C51 H57 N9' _chemical_formula_weight 796.06 _chemical_melting_point ? _chemical_compound_source ? 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' _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0751(3) _cell_length_b 12.4215(3) _cell_length_c 16.77080(10) _cell_angle_alpha 85.288(2) _cell_angle_beta 81.2730(10) _cell_angle_gamma 67.5570(10) _cell_volume 2297.22(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9106 _cell_measurement_theta_min 1.77 _cell_measurement_theta_max 24.41 _exptl_crystal_description 'plate' _exptl_crystal_colour 'reddish' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.151 _exptl_crystal_density_method ? _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 0.070 _exptl_absorpt_correction_type 'Semi-empirical from psi-scans (SADABS)' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9106 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.1204 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 24.41 _reflns_number_total 6738 _reflns_number_observed 3069 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1631P)^2^+0.0000P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6738 _refine_ls_number_parameters 541 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1510 _refine_ls_R_factor_obs 0.0748 _refine_ls_wR_factor_all 0.2783 _refine_ls_wR_factor_obs 0.2058 _refine_ls_goodness_of_fit_all 0.902 _refine_ls_goodness_of_fit_obs 1.022 _refine_ls_restrained_S_all 0.902 _refine_ls_restrained_S_obs 1.022 _refine_ls_shift/esd_max -0.058 _refine_ls_shift/esd_mean 0.002 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group N7 N 0.6229(4) 0.6000(4) 0.1854(3) 0.0877(13) Uani 1 d . . C1 C 0.1248(4) 1.1402(3) 0.3322(2) 0.0502(10) Uani 1 d . . N1 N 0.2565(3) 1.1357(3) 0.4821(2) 0.0608(10) Uani 1 d . . N2 N 0.5170(3) 0.8919(3) 0.1688(2) 0.0580(10) Uani 1 d . . C2 C 0.2180(4) 1.0478(3) 0.3661(2) 0.0494(10) Uani 1 d . . C3 C 0.3068(4) 0.9624(3) 0.3168(2) 0.0504(10) Uani 1 d . . N3 N 0.0976(3) 1.3236(3) 0.1641(2) 0.0579(10) Uani 1 d . . C4 C 0.3030(4) 0.9663(3) 0.2331(2) 0.0488(10) Uani 1 d . . N4 N 0.0667(5) 1.2839(5) 0.6141(3) 0.104(2) Uani 1 d . . C5 C 0.2100(4) 1.0571(3) 0.1986(2) 0.0486(10) Uani 1 d . . C22 C 0.2914(10) 1.3485(7) 0.4503(5) 0.150(3) Uani 1 d . . H22 H 0.2113(10) 1.3484(7) 0.4637(5) 0.180 Uiso 1 calc R . C6 C 0.1238(4) 1.1454(3) 0.2479(2) 0.0494(10) Uani 1 d . . N6 N 0.6644(5) 1.0773(5) 0.0861(3) 0.117(2) Uani 1 d . . C7 C 0.0275(4) 1.2307(4) 0.3874(3) 0.0623(12) Uani 1 d . . H7A H 0.0600(4) 1.2349(4) 0.4353(3) 0.075 Uiso 1 calc R . H7B H 0.0061(4) 1.3057(4) 0.3604(3) 0.075 Uiso 1 calc R . N8 N -0.1382(5) 1.3939(4) 0.0422(3) 0.109(2) Uani 1 d . . C8 C -0.0859(4) 1.2036(5) 0.4113(3) 0.089(2) Uani 1 d . . H8A H -0.1436(4) 1.2632(5) 0.4458(3) 0.106 Uiso 1 calc R . H8B H -0.0656(4) 1.1296(5) 0.4395(3) 0.106 Uiso 1 calc R . H8C H -0.1201(4) 1.2011(5) 0.3638(3) 0.106 Uiso 1 calc R . C9 C 0.4095(4) 0.8643(4) 0.3521(3) 0.0642(13) Uani 1 d . . H9A H 0.4283(4) 0.8928(4) 0.3977(3) 0.077 Uiso 1 calc R . H9B H 0.4799(4) 0.8426(4) 0.3124(3) 0.077 Uiso 1 calc R . N9 N 0.3230(5) 1.3451(5) 0.1051(3) 0.112(2) Uani 1 d . . C10 C 0.3812(5) 0.7560(4) 0.3788(3) 0.090(2) Uani 1 d . . H10A H 0.4495(5) 0.6981(4) 0.4003(3) 0.108 Uiso 1 calc R . H10B H 0.3642(5) 0.7255(4) 0.3333(3) 0.108 Uiso 1 calc R . H10C H 0.3121(5) 0.7763(4) 0.4196(3) 0.108 Uiso 1 calc R . C11 C 0.1980(4) 1.0607(4) 0.1093(2) 0.0600(12) Uani 1 d . . H11A H 0.1674(4) 1.1404(4) 0.0904(2) 0.072 Uiso 1 calc R . H11B H 0.2764(4) 1.0225(4) 0.0797(2) 0.072 Uiso 1 calc R . C12 C 0.1144(5) 1.0022(5) 0.0930(3) 0.090(2) Uani 1 d . . H12A H 0.1093(5) 1.0064(5) 0.0362(3) 0.108 Uiso 1 calc R . H12B H 0.0354(5) 1.0411(5) 0.1217(3) 0.108 Uiso 1 calc R . H12C H 0.1455(5) 0.9220(5) 0.1108(3) 0.108 Uiso 1 calc R . C13 C 0.2206(4) 1.0448(4) 0.4567(2) 0.0604(12) Uani 1 d . . H13A H 0.1419(4) 1.0542(4) 0.4842(2) 0.072 Uiso 1 calc R . H13B H 0.2762(4) 0.9699(4) 0.4725(2) 0.072 Uiso 1 calc R . C14 C 0.2553(4) 1.1295(4) 0.5700(3) 0.0713(14) Uani 1 d . . H14A H 0.2953(4) 1.1774(4) 0.5842(3) 0.086 Uiso 1 calc R . H14B H 0.2999(4) 1.0507(4) 0.5863(3) 0.086 Uiso 1 calc R . C15 C 0.1295(5) 1.1688(5) 0.6150(3) 0.0716(14) Uani 1 d . . C16 C 0.0823(7) 1.0906(6) 0.6527(3) 0.109(2) Uani 1 d . . H16 H 0.1295(7) 1.0085(6) 0.6523(3) 0.131 Uiso 1 calc R . C17 C -0.0353(9) 1.1330(11) 0.6915(4) 0.146(3) Uani 1 d . . H17 H -0.0720(9) 1.0802(11) 0.7164(4) 0.175 Uiso 1 calc R . C18 C -0.0963(9) 1.2465(14) 0.6940(6) 0.161(5) Uani 1 d . . H18 H -0.1762(9) 1.2765(14) 0.7232(6) 0.193 Uiso 1 calc R . C19 C -0.0470(8) 1.3202(8) 0.6560(6) 0.139(3) Uani 1 d . . H19 H -0.0939(8) 1.4024(8) 0.6583(6) 0.167 Uiso 1 calc R . C20 C 0.3729(5) 1.1346(4) 0.4394(3) 0.0766(14) Uani 1 d . . H20A H 0.3800(5) 1.1133(4) 0.3846(3) 0.092 Uiso 1 calc R . H20B H 0.4369(5) 1.0755(4) 0.4641(3) 0.092 Uiso 1 calc R . C21 C 0.3899(7) 1.2466(6) 0.4390(3) 0.090(2) Uani 1 d . . N5 N 0.5063(6) 1.2366(6) 0.4282(3) 0.128(2) Uani 1 d . . C25 C 0.5206(13) 1.3438(14) 0.4238(5) 0.181(5) Uani 1 d . . H25 H 0.6003(13) 1.3456(14) 0.4155(5) 0.218 Uiso 1 calc R . C24 C 0.4257(18) 1.4421(10) 0.4310(7) 0.198(8) Uani 1 d . . H24 H 0.4423(18) 1.5121(10) 0.4281(7) 0.237 Uiso 1 calc R . C23 C 0.3121(15) 1.4560(14) 0.4415(9) 0.232(8) Uani 1 d . . H23 H 0.2477(15) 1.5313(14) 0.4432(9) 0.279 Uiso 1 calc R . C26 C 0.4019(4) 0.8742(4) 0.1803(2) 0.0560(11) Uani 1 d . . H26A H 0.4141(4) 0.7985(4) 0.2047(2) 0.067 Uiso 1 calc R . H26B H 0.3761(4) 0.8762(4) 0.1286(2) 0.067 Uiso 1 calc R . C27 C 0.5093(5) 0.9990(4) 0.1233(3) 0.0741(14) Uani 1 d . . H27A H 0.4280(5) 1.0550(4) 0.1330(3) 0.089 Uiso 1 calc R . H27B H 0.5272(5) 0.9831(4) 0.0668(3) 0.089 Uiso 1 calc R . C28 C 0.5945(4) 1.0504(4) 0.1455(3) 0.0697(13) Uani 1 d . . C29 C 0.5923(7) 1.0753(7) 0.2221(4) 0.125(2) Uani 1 d . . H29 H 0.5400(7) 1.0539(7) 0.2638(4) 0.150 Uiso 1 calc R . C30 C 0.6631(8) 1.1311(8) 0.2428(5) 0.147(3) Uani 1 d . . H30 H 0.6593(8) 1.1509(8) 0.2975(5) 0.176 Uiso 1 calc R . C31 C 0.7366(7) 1.1559(7) 0.1835(6) 0.127(3) Uani 1 d . . H31 H 0.7892(7) 1.1926(7) 0.1950(6) 0.152 Uiso 1 calc R . C32 C 0.7371(7) 1.1303(7) 0.1091(6) 0.143(3) Uani 1 d . . H32 H 0.7913(7) 1.1494(7) 0.0676(6) 0.171 Uiso 1 calc R . C33 C 0.6174(4) 0.7887(4) 0.1320(3) 0.0771(15) Uani 1 d . . H33A H 0.6850(4) 0.8100(4) 0.1113(3) 0.093 Uiso 1 calc R . H33B H 0.5917(4) 0.7644(4) 0.0876(3) 0.093 Uiso 1 calc R . C34 C 0.6562(4) 0.6892(5) 0.1915(3) 0.0680(13) Uani 1 d . . C35 C 0.7243(4) 0.6907(5) 0.2506(3) 0.0753(14) Uani 1 d . . H35 H 0.7487(4) 0.7552(5) 0.2532(3) 0.090 Uiso 1 calc R . C36 C 0.7567(5) 0.5990(5) 0.3057(3) 0.089(2) Uani 1 d . . H36 H 0.8034(5) 0.5993(5) 0.3471(3) 0.107 Uiso 1 calc R . C37 C 0.7221(5) 0.5086(5) 0.3008(4) 0.093(2) Uani 1 d . . H37 H 0.7438(5) 0.4435(5) 0.3382(4) 0.112 Uiso 1 calc R . C38 C 0.6558(5) 0.5126(5) 0.2414(5) 0.101(2) Uani 1 d . . H38 H 0.6303(5) 0.4488(5) 0.2389(5) 0.121 Uiso 1 calc R . C39 C 0.0339(4) 1.2512(3) 0.2079(2) 0.0575(11) Uani 1 d . . H39A H -0.0039(4) 1.2256(3) 0.1709(2) 0.069 Uiso 1 calc R . H39B H -0.0281(4) 1.2965(3) 0.2483(2) 0.069 Uiso 1 calc R . C40 C 0.0174(5) 1.4157(4) 0.1149(3) 0.0720(14) Uani 1 d . . H40A H 0.0566(5) 1.4682(4) 0.0938(3) 0.086 Uiso 1 calc R . H40B H -0.0553(5) 1.4593(4) 0.1487(3) 0.086 Uiso 1 calc R . C41 C -0.0153(5) 1.3686(4) 0.0460(3) 0.0610(12) Uani 1 d . . C42 C 0.0695(4) 1.3090(4) -0.0095(3) 0.0562(11) Uani 1 d . . H42 H 0.1529(4) 1.2933(4) -0.0060(3) 0.067 Uiso 1 calc R . C43 C 0.0388(6) 1.2706(5) -0.0706(3) 0.090(2) Uani 1 d . . H43 H 0.1024(6) 1.2257(5) -0.1102(3) 0.108 Uiso 1 calc R . C44 C -0.0775(7) 1.2904(5) -0.0811(4) 0.092(2) Uani 1 d . . H44 H -0.0952(7) 1.2613(5) -0.1269(4) 0.110 Uiso 1 calc R . C45 C -0.1653(6) 1.3517(6) -0.0254(4) 0.096(2) Uani 1 d . . H45 H -0.2480(6) 1.3675(6) -0.0312(4) 0.115 Uiso 1 calc R . C46 C 0.1499(4) 1.3738(4) 0.2166(3) 0.0662(13) Uani 1 d . . H46A H 0.1754(4) 1.3202(4) 0.2609(3) 0.079 Uiso 1 calc R . H46B H 0.0885(4) 1.4440(4) 0.2384(3) 0.079 Uiso 1 calc R . C47 C 0.2562(4) 1.4017(4) 0.1752(3) 0.0624(12) Uani 1 d . . C48 C 0.2820(4) 1.4761(4) 0.2114(3) 0.0581(12) Uani 1 d . . H48 H 0.2323(4) 1.5142(4) 0.2590(3) 0.070 Uiso 1 calc R . C49 C 0.3776(6) 1.4971(5) 0.1806(4) 0.100(2) Uani 1 d . . H49 H 0.3972(6) 1.5508(5) 0.2083(4) 0.119 Uiso 1 calc R . C50 C 0.4534(6) 1.4487(6) 0.1117(4) 0.103(2) Uani 1 d . . H50 H 0.5219(6) 1.4690(6) 0.0916(4) 0.124 Uiso 1 calc R . C51 C 0.4263(6) 1.3709(6) 0.0734(4) 0.101(2) Uani 1 d . . H51 H 0.4765(6) 1.3339(6) 0.0256(4) 0.121 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N7 0.071(3) 0.077(3) 0.112(4) -0.026(3) -0.022(3) -0.015(3) C1 0.052(3) 0.045(2) 0.049(2) -0.001(2) 0.000(2) -0.016(2) N1 0.071(3) 0.059(2) 0.046(2) -0.008(2) -0.008(2) -0.016(2) N2 0.051(2) 0.069(2) 0.051(2) 0.000(2) -0.002(2) -0.021(2) C2 0.060(3) 0.049(2) 0.038(2) 0.003(2) -0.004(2) -0.020(2) C3 0.056(3) 0.049(2) 0.043(2) 0.001(2) -0.005(2) -0.018(2) N3 0.076(3) 0.050(2) 0.051(2) 0.008(2) -0.018(2) -0.026(2) C4 0.056(3) 0.044(2) 0.045(2) -0.001(2) -0.005(2) -0.019(2) N4 0.082(4) 0.103(4) 0.112(4) -0.044(3) -0.015(3) -0.011(3) C5 0.055(3) 0.053(2) 0.040(2) 0.000(2) -0.005(2) -0.024(2) C22 0.246(11) 0.077(5) 0.164(7) 0.034(5) -0.100(7) -0.081(6) C6 0.053(3) 0.049(2) 0.045(2) 0.004(2) -0.008(2) -0.017(2) N6 0.127(4) 0.136(5) 0.086(4) -0.032(3) 0.042(3) -0.064(4) C7 0.064(3) 0.056(3) 0.057(3) -0.003(2) -0.005(2) -0.011(2) N8 0.114(4) 0.102(4) 0.114(4) 0.022(3) -0.023(3) -0.046(3) C8 0.067(3) 0.090(4) 0.088(4) -0.006(3) 0.016(3) -0.015(3) C9 0.070(3) 0.057(3) 0.048(3) 0.004(2) -0.008(2) -0.006(2) N9 0.111(4) 0.122(4) 0.106(4) 0.003(3) -0.011(3) -0.050(3) C10 0.117(5) 0.055(3) 0.082(4) 0.013(3) -0.010(3) -0.019(3) C11 0.063(3) 0.067(3) 0.049(3) -0.004(2) -0.012(2) -0.021(2) C12 0.098(4) 0.110(4) 0.084(4) -0.015(3) -0.024(3) -0.055(4) C13 0.074(3) 0.057(3) 0.041(2) -0.003(2) -0.003(2) -0.015(2) C14 0.075(3) 0.077(3) 0.055(3) -0.006(2) -0.016(2) -0.017(3) C15 0.072(3) 0.091(4) 0.046(3) -0.018(3) -0.012(2) -0.018(3) C16 0.145(6) 0.118(5) 0.063(4) -0.001(3) 0.019(4) -0.061(5) C17 0.155(8) 0.223(10) 0.079(5) -0.029(6) 0.038(5) -0.107(8) C18 0.098(7) 0.264(15) 0.121(7) -0.103(9) 0.014(5) -0.058(8) C19 0.109(7) 0.146(8) 0.146(8) -0.081(6) -0.022(6) -0.011(5) C20 0.091(4) 0.080(4) 0.057(3) -0.004(3) -0.003(3) -0.033(3) C21 0.136(6) 0.086(5) 0.067(3) 0.014(3) -0.037(4) -0.056(4) N5 0.144(6) 0.172(6) 0.103(4) -0.006(4) -0.014(4) -0.098(5) C25 0.277(14) 0.257(13) 0.123(7) 0.021(8) -0.039(8) -0.227(13) C24 0.379(23) 0.087(6) 0.164(9) 0.043(6) -0.139(13) -0.097(11) C23 0.303(19) 0.196(13) 0.264(14) 0.083(10) -0.185(15) -0.130(14) C26 0.059(3) 0.057(3) 0.049(2) -0.006(2) -0.006(2) -0.019(2) C27 0.077(3) 0.093(4) 0.049(3) 0.015(3) -0.012(2) -0.031(3) C28 0.063(3) 0.086(3) 0.053(3) 0.001(3) -0.003(2) -0.023(3) C29 0.149(6) 0.188(7) 0.076(4) -0.003(4) -0.013(4) -0.106(6) C30 0.166(8) 0.209(9) 0.103(6) -0.021(6) -0.018(6) -0.110(7) C31 0.115(6) 0.145(6) 0.138(7) -0.036(6) -0.010(5) -0.064(5) C32 0.137(7) 0.159(7) 0.159(8) -0.047(6) 0.038(6) -0.098(6) C33 0.060(3) 0.103(4) 0.058(3) -0.015(3) 0.006(2) -0.021(3) C34 0.052(3) 0.070(3) 0.071(3) -0.020(3) -0.002(2) -0.009(2) C35 0.073(3) 0.076(3) 0.078(3) -0.013(3) -0.012(3) -0.027(3) C36 0.080(4) 0.092(4) 0.084(4) -0.008(3) -0.018(3) -0.016(3) C37 0.076(4) 0.066(4) 0.132(5) -0.006(3) -0.023(4) -0.016(3) C38 0.080(4) 0.071(4) 0.156(6) -0.023(4) -0.022(4) -0.026(3) C39 0.065(3) 0.050(3) 0.051(2) 0.004(2) -0.010(2) -0.015(2) C40 0.097(4) 0.051(3) 0.063(3) 0.009(2) -0.024(3) -0.020(3) C41 0.066(3) 0.060(3) 0.067(3) 0.021(2) -0.025(3) -0.033(2) C42 0.049(3) 0.075(3) 0.046(3) -0.013(2) -0.010(2) -0.022(2) C43 0.094(5) 0.092(4) 0.077(4) 0.001(3) -0.003(3) -0.031(3) C44 0.127(6) 0.088(4) 0.075(4) 0.005(3) -0.036(4) -0.050(4) C45 0.083(4) 0.124(5) 0.099(5) 0.011(4) -0.039(4) -0.054(4) C46 0.081(3) 0.065(3) 0.057(3) -0.003(2) -0.016(3) -0.029(3) C47 0.065(3) 0.066(3) 0.047(3) -0.003(2) -0.006(2) -0.015(2) C48 0.054(3) 0.070(3) 0.056(3) -0.027(2) -0.004(2) -0.026(2) C49 0.099(5) 0.106(5) 0.100(5) -0.029(4) -0.025(4) -0.036(4) C50 0.091(5) 0.133(6) 0.108(5) -0.003(4) -0.027(4) -0.062(4) C51 0.087(4) 0.128(5) 0.090(4) -0.018(4) 0.010(3) -0.048(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N7 C34 1.331(6) . ? N7 C38 1.355(8) . ? C1 C6 1.411(5) . ? C1 C2 1.417(5) . ? C1 C7 1.528(5) . ? N1 C13 1.466(5) . ? N1 C20 1.473(6) . ? N1 C14 1.469(5) . ? N2 C27 1.455(6) . ? N2 C26 1.471(5) . ? N2 C33 1.487(5) . ? C2 C3 1.403(5) . ? C2 C13 1.522(5) . ? C3 C4 1.406(5) . ? C3 C9 1.524(6) . ? N3 C46 1.456(5) . ? N3 C40 1.473(5) . ? N3 C39 1.479(5) . ? C4 C5 1.412(5) . ? C4 C26 1.524(5) . ? N4 C15 1.338(7) . ? N4 C19 1.367(10) . ? C5 C6 1.410(5) . ? C5 C11 1.521(5) . ? C22 C21 1.369(10) . ? C22 C23 1.442(14) . ? C6 C39 1.530(5) . ? N6 C28 1.312(6) . ? N6 C32 1.391(9) . ? C7 C8 1.520(6) . ? N8 C41 1.405(7) . ? N8 C45 1.418(8) . ? C9 C10 1.527(6) . ? N9 C47 1.394(6) . ? N9 C51 1.419(7) . ? C11 C12 1.516(6) . ? C14 C15 1.505(6) . ? C15 C16 1.371(7) . ? C16 C17 1.386(10) . ? C17 C18 1.319(13) . ? C18 C19 1.344(12) . ? C20 C21 1.481(7) . ? C21 N5 1.348(8) . ? N5 C25 1.402(11) . ? C25 C24 1.32(2) . ? C24 C23 1.30(2) . ? C27 C28 1.504(7) . ? C28 C29 1.340(7) . ? C29 C30 1.383(9) . ? C30 C31 1.328(9) . ? C31 C32 1.311(10) . ? C33 C34 1.497(7) . ? C34 C35 1.386(7) . ? C35 C36 1.378(7) . ? C36 C37 1.351(7) . ? C37 C38 1.355(8) . ? C40 C41 1.502(6) . ? C41 C42 1.307(6) . ? C42 C43 1.321(7) . ? C43 C44 1.366(8) . ? C44 C45 1.332(7) . ? C46 C47 1.510(6) . ? C47 C48 1.299(6) . ? C48 C49 1.302(7) . ? C49 C50 1.382(8) . ? C50 C51 1.365(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 C34 N7 C38 116.5(5) . . ? C6 C1 C2 118.9(3) . . ? C6 C1 C7 121.6(4) . . ? C2 C1 C7 119.5(3) . . ? C13 N1 C20 113.8(3) . . ? C13 N1 C14 110.3(3) . . ? C20 N1 C14 111.6(4) . . ? C27 N2 C26 112.4(3) . . ? C27 N2 C33 111.8(3) . . ? C26 N2 C33 111.0(3) . . ? C3 C2 C1 120.4(3) . . ? C3 C2 C13 121.0(4) . . ? C1 C2 C13 118.6(3) . . ? C2 C3 C4 120.3(4) . . ? C2 C3 C9 121.1(3) . . ? C4 C3 C9 118.6(3) . . ? C46 N3 C40 110.4(3) . . ? C46 N3 C39 113.5(3) . . ? C40 N3 C39 110.8(4) . . ? C3 C4 C5 119.9(3) . . ? C3 C4 C26 119.5(4) . . ? C5 C4 C26 120.6(3) . . ? C15 N4 C19 115.9(7) . . ? C6 C5 C4 119.6(3) . . ? C6 C5 C11 118.7(4) . . ? C4 C5 C11 121.7(3) . . ? C21 C22 C23 117.8(11) . . ? C5 C6 C1 120.7(4) . . ? C5 C6 C39 118.8(3) . . ? C1 C6 C39 120.4(3) . . ? C28 N6 C32 115.1(6) . . ? C8 C7 C1 113.2(4) . . ? C41 N8 C45 116.3(5) . . ? C3 C9 C10 114.0(4) . . ? C47 N9 C51 116.5(5) . . ? C12 C11 C5 112.2(4) . . ? N1 C13 C2 112.9(3) . . ? N1 C14 C15 112.7(4) . . ? N4 C15 C16 122.7(5) . . ? N4 C15 C14 115.6(5) . . ? C16 C15 C14 121.6(5) . . ? C15 C16 C17 118.4(7) . . ? C18 C17 C16 119.4(9) . . ? C17 C18 C19 120.3(10) . . ? C18 C19 N4 123.1(9) . . ? N1 C20 C21 114.8(5) . . ? N5 C21 C22 125.6(7) . . ? N5 C21 C20 114.5(6) . . ? C22 C21 C20 119.9(7) . . ? C21 N5 C25 113.6(8) . . ? C24 C25 N5 120.6(11) . . ? C25 C24 C23 127.9(15) . . ? C24 C23 C22 114.1(15) . . ? N2 C26 C4 112.3(3) . . ? N2 C27 C28 112.7(4) . . ? N6 C28 C29 121.7(6) . . ? N6 C28 C27 117.1(5) . . ? C29 C28 C27 121.0(5) . . ? C28 C29 C30 121.8(6) . . ? C31 C30 C29 117.0(7) . . ? C32 C31 C30 119.8(8) . . ? C31 C32 N6 124.5(7) . . ? N2 C33 C34 112.0(3) . . ? N7 C34 C35 121.6(5) . . ? N7 C34 C33 117.6(5) . . ? C35 C34 C33 120.8(5) . . ? C36 C35 C34 119.6(5) . . ? C37 C36 C35 119.4(6) . . ? C38 C37 C36 118.0(6) . . ? C37 C38 N7 124.9(6) . . ? N3 C39 C6 109.8(3) . . ? N3 C40 C41 112.9(4) . . ? C42 C41 N8 121.9(5) . . ? C42 C41 C40 119.9(4) . . ? N8 C41 C40 118.2(5) . . ? C41 C42 C43 119.0(5) . . ? C42 C43 C44 124.4(5) . . ? C45 C44 C43 117.5(6) . . ? C44 C45 N8 120.8(6) . . ? N3 C46 C47 114.2(4) . . ? C48 C47 N9 124.1(5) . . ? C48 C47 C46 115.5(4) . . ? N9 C47 C46 120.3(5) . . ? C49 C48 C47 117.5(5) . . ? C48 C49 C50 125.7(6) . . ? C51 C50 C49 116.9(6) . . ? C50 C51 N9 119.2(6) . . ? _refine_diff_density_max 0.294 _refine_diff_density_min -0.308 _refine_diff_density_rms 0.064 #=END data_2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common 'L(CuI)3' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C51 H57 Cu3 I3 N9' _chemical_formula_weight 1367.38 _chemical_melting_point ? _chemical_compound_source ? 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' 'Cu' 'Cu' 0.3201 1.2651 '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' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.6703(4) _cell_length_b 14.0313(4) _cell_length_c 22.9276(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.9480(10) _cell_angle_gamma 90.00 _cell_volume 5181.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 20652 _cell_measurement_theta_min 1.92 _cell_measurement_theta_max 24.32 _exptl_crystal_description 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.753 _exptl_crystal_density_method ? _exptl_crystal_F_000 2688 _exptl_absorpt_coefficient_mu 3.052 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20652 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_sigmaI/netI 0.0615 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 24.32 _reflns_number_total 8181 _reflns_number_observed 5117 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0326P)^2^+4.9765P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8181 _refine_ls_number_parameters 595 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0922 _refine_ls_R_factor_obs 0.0433 _refine_ls_wR_factor_all 0.0990 _refine_ls_wR_factor_obs 0.0790 _refine_ls_goodness_of_fit_all 1.044 _refine_ls_goodness_of_fit_obs 1.077 _refine_ls_restrained_S_all 1.044 _refine_ls_restrained_S_obs 1.077 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu -0.31485(5) 0.76985(6) -0.11126(4) 0.0583(2) Uani 1 d . . Cu2 Cu 0.09809(5) 0.69121(6) 0.07160(3) 0.0504(2) Uani 1 d . . Cu3 Cu -0.25870(5) 0.44623(6) 0.18106(4) 0.0580(2) Uani 1 d . . I1 I -0.42755(4) 0.64758(4) -0.11828(3) 0.0858(2) Uani 1 d . . I2 I 0.13220(3) 0.79857(3) -0.00756(2) 0.0618(2) Uani 1 d . . I3 I -0.11876(3) 0.37949(4) 0.23313(2) 0.0708(2) Uani 1 d . . N1 N -0.1985(3) 0.8713(3) -0.0501(2) 0.0402(12) Uani 1 d . . N2 N 0.0507(3) 0.6813(4) 0.1695(2) 0.0409(13) Uani 1 d . . N3 N -0.3334(3) 0.5932(4) 0.1283(2) 0.0413(13) Uani 1 d . . N4 N -0.2151(3) 0.7262(4) -0.1363(2) 0.0497(14) Uani 1 d . . N5 N -0.3611(4) 0.9023(4) -0.1211(2) 0.060(2) Uani 1 d . . N6 N -0.0055(3) 0.6140(3) 0.0487(2) 0.0409(12) Uani 1 d . . N7 N 0.2010(3) 0.6559(4) 0.1348(2) 0.0526(14) Uani 1 d . . N8 N -0.3102(3) 0.4041(4) 0.0968(2) 0.0551(15) Uani 1 d . . N9 N -0.3159(4) 0.4989(4) 0.2410(3) 0.0560(15) Uani 1 d . . C1 C -0.1760(4) 0.8362(4) 0.0614(3) 0.0375(15) Uani 1 d . . C2 C -0.0979(3) 0.8190(4) 0.1006(3) 0.0349(14) Uani 1 d . . C3 C -0.0914(4) 0.7572(4) 0.1499(2) 0.0351(14) Uani 1 d . . C4 C -0.1616(4) 0.7172(4) 0.1616(2) 0.0359(14) Uani 1 d . . C5 C -0.2393(4) 0.7344(4) 0.1222(3) 0.0362(14) Uani 1 d . . C6 C -0.2477(3) 0.7933(4) 0.0718(3) 0.0364(14) Uani 1 d . . C7 C -0.0206(4) 0.8690(4) 0.0929(3) 0.044(2) Uani 1 d . . H7A H 0.0262(4) 0.8274(4) 0.1067(3) 0.053 Uiso 1 calc R . H7B H -0.0268(4) 0.8805(4) 0.0506(3) 0.053 Uiso 1 calc R . C8 C -0.0024(4) 0.9628(5) 0.1265(3) 0.064(2) Uani 1 d . . H8A H 0.0469(4) 0.9906(5) 0.1193(3) 0.077 Uiso 1 calc R . H8B H 0.0058(4) 0.9519(5) 0.1689(3) 0.077 Uiso 1 calc R . H8C H -0.0484(4) 1.0055(5) 0.1124(3) 0.077 Uiso 1 calc R . C9 C -0.1562(4) 0.6600(4) 0.2181(3) 0.044(2) Uani 1 d . . H9A H -0.2026(4) 0.6171(4) 0.2112(3) 0.053 Uiso 1 calc R . H9B H -0.1065(4) 0.6222(4) 0.2266(3) 0.053 Uiso 1 calc R . C10 C -0.1556(4) 0.7203(5) 0.2721(3) 0.062(2) Uani 1 d . . H10A H -0.1522(4) 0.6800(5) 0.3066(3) 0.075 Uiso 1 calc R . H10B H -0.2057(4) 0.7572(5) 0.2644(3) 0.075 Uiso 1 calc R . H10C H -0.1086(4) 0.7623(5) 0.2800(3) 0.075 Uiso 1 calc R . C11 C -0.3311(4) 0.8156(4) 0.0308(3) 0.046(2) Uani 1 d . . H11A H -0.3655(4) 0.7599(4) 0.0273(3) 0.055 Uiso 1 calc R . H11B H -0.3244(4) 0.8298(4) -0.0086(3) 0.055 Uiso 1 calc R . C12 C -0.3759(4) 0.8990(5) 0.0515(3) 0.071(2) Uani 1 d . . H12A H -0.4286(4) 0.9088(5) 0.0230(3) 0.085 Uiso 1 calc R . H12B H -0.3428(4) 0.9555(5) 0.0541(3) 0.085 Uiso 1 calc R . H12C H -0.3845(4) 0.8848(5) 0.0904(3) 0.085 Uiso 1 calc R . C13 C -0.1864(4) 0.9098(4) 0.0118(2) 0.0388(15) Uani 1 d . . H13A H -0.2333(4) 0.9491(4) 0.0125(2) 0.047 Uiso 1 calc R . H13B H -0.1382(4) 0.9500(4) 0.0206(2) 0.047 Uiso 1 calc R . C14 C -0.1256(4) 0.8211(4) -0.0575(3) 0.043(2) Uani 1 d . . H14A H -0.1060(4) 0.7794(4) -0.0235(3) 0.052 Uiso 1 calc R . H14B H -0.0826(4) 0.8667(4) -0.0572(3) 0.052 Uiso 1 calc R . C15 C -0.1401(4) 0.7634(5) -0.1143(3) 0.046(2) Uani 1 d . . C16 C -0.0755(4) 0.7450(5) -0.1399(3) 0.059(2) Uani 1 d . . H16 H -0.0222(4) 0.7739(5) -0.1238(3) 0.070 Uiso 1 calc R . C17 C -0.0884(5) 0.6848(6) -0.1887(4) 0.073(2) Uani 1 d . . H17 H -0.0444(5) 0.6715(6) -0.2075(4) 0.088 Uiso 1 calc R . C18 C -0.1651(6) 0.6441(6) -0.2100(3) 0.072(2) Uani 1 d . . H18 H -0.1755(6) 0.6009(6) -0.2436(3) 0.087 Uiso 1 calc R . C19 C -0.2261(5) 0.6657(5) -0.1831(3) 0.061(2) Uani 1 d . . H19 H -0.2795(5) 0.6365(5) -0.1981(3) 0.073 Uiso 1 calc R . C20 C -0.2180(4) 0.9517(5) -0.0925(3) 0.050(2) Uani 1 d . . H20A H -0.2028(4) 0.9357(5) -0.1289(3) 0.060 Uiso 1 calc R . H20B H -0.1862(4) 1.0064(5) -0.0750(3) 0.060 Uiso 1 calc R . C21 C -0.3083(5) 0.9753(6) -0.1072(3) 0.056(2) Uani 1 d . . C22 C -0.3356(7) 1.0680(6) -0.1074(4) 0.096(3) Uani 1 d . . H22 H -0.2965(7) 1.1193(6) -0.0961(4) 0.115 Uiso 1 calc R . C23 C -0.4180(8) 1.0858(8) -0.1237(5) 0.126(5) Uani 1 d . . H23 H -0.4378(8) 1.1503(8) -0.1254(5) 0.151 Uiso 1 calc R . C24 C -0.4724(7) 1.0130(9) -0.1376(4) 0.115(4) Uani 1 d . . H24 H -0.5311(7) 1.0248(9) -0.1485(4) 0.137 Uiso 1 calc R . C25 C -0.4423(5) 0.9218(7) -0.1358(3) 0.082(3) Uani 1 d . . H25 H -0.4811(5) 0.8699(7) -0.1455(3) 0.099 Uiso 1 calc R . C26 C -0.0058(4) 0.7422(4) 0.1922(3) 0.045(2) Uani 1 d . . H26A H 0.0200(4) 0.8034(4) 0.2019(3) 0.053 Uiso 1 calc R . H26B H -0.0125(4) 0.7151(4) 0.2291(3) 0.053 Uiso 1 calc R . C27 C 0.0199(4) 0.5842(4) 0.1554(3) 0.051(2) Uani 1 d . . H27A H -0.0109(4) 0.5653(4) 0.1836(3) 0.061 Uiso 1 calc R . H27B H 0.0663(4) 0.5417(4) 0.1602(3) 0.061 Uiso 1 calc R . C28 C -0.0344(4) 0.5750(4) 0.0927(3) 0.045(2) Uani 1 d . . C29 C -0.1066(5) 0.5237(5) 0.0794(4) 0.066(2) Uani 1 d . . H29 H -0.1261(5) 0.4959(5) 0.1114(4) 0.079 Uiso 1 calc R . C30 C -0.1511(5) 0.5117(6) 0.0208(4) 0.071(2) Uani 1 d . . H30 H -0.2018(5) 0.4757(6) 0.0114(4) 0.085 Uiso 1 calc R . C31 C -0.1223(5) 0.5517(5) -0.0236(3) 0.064(2) Uani 1 d . . H31 H -0.1527(5) 0.5453(5) -0.0651(3) 0.077 Uiso 1 calc R . C32 C -0.0490(4) 0.6016(4) -0.0084(3) 0.052(2) Uani 1 d . . H32 H -0.0283(4) 0.6286(4) -0.0401(3) 0.062 Uiso 1 calc R . C33 C 0.1294(4) 0.6801(5) 0.2144(3) 0.060(2) Uani 1 d . . H33A H 0.1239(4) 0.6409(5) 0.2475(3) 0.072 Uiso 1 calc R . H33B H 0.1415(4) 0.7436(5) 0.2296(3) 0.072 Uiso 1 calc R . C34 C 0.2024(4) 0.6442(5) 0.1930(3) 0.053(2) Uani 1 d . . C35 C 0.2696(4) 0.6065(6) 0.2334(3) 0.071(2) Uani 1 d . . H35 H 0.2686(4) 0.5974(6) 0.2748(3) 0.086 Uiso 1 calc R . C36 C 0.3393(5) 0.5813(6) 0.2146(4) 0.081(3) Uani 1 d . . H36 H 0.3872(5) 0.5547(6) 0.2425(4) 0.098 Uiso 1 calc R . C37 C 0.3382(5) 0.5954(6) 0.1558(4) 0.079(2) Uani 1 d . . H37 H 0.3858(5) 0.5800(6) 0.1413(4) 0.095 Uiso 1 calc R . C38 C 0.2694(4) 0.6311(6) 0.1184(3) 0.068(2) Uani 1 d . . H38 H 0.2692(4) 0.6396(6) 0.0769(3) 0.081 Uiso 1 calc R . C39 C -0.3172(4) 0.6962(4) 0.1375(3) 0.043(2) Uani 1 d . . H39A H -0.3134(4) 0.7107(4) 0.1790(3) 0.051 Uiso 1 calc R . H39B H -0.3642(4) 0.7302(4) 0.1135(3) 0.051 Uiso 1 calc R . C40 C -0.3499(4) 0.5669(4) 0.0648(3) 0.049(2) Uani 1 d . . H40A H -0.3069(4) 0.5929(4) 0.0486(3) 0.058 Uiso 1 calc R . H40B H -0.4015(4) 0.5952(4) 0.0433(3) 0.058 Uiso 1 calc R . C41 C -0.3546(4) 0.4618(5) 0.0538(3) 0.049(2) Uani 1 d . . C42 C -0.4012(4) 0.4265(5) 0.0002(3) 0.059(2) Uani 1 d . . H42 H -0.4326(4) 0.4695(5) -0.0297(3) 0.070 Uiso 1 calc R . C43 C -0.4038(5) 0.3327(6) -0.0113(4) 0.071(2) Uani 1 d . . H43 H -0.4379(5) 0.3080(6) -0.0485(4) 0.085 Uiso 1 calc R . C44 C -0.3566(5) 0.2725(6) 0.0314(4) 0.077(2) Uani 1 d . . H44 H -0.3561(5) 0.2052(6) 0.0242(4) 0.092 Uiso 1 calc R . C45 C -0.3104(5) 0.3108(6) 0.0844(4) 0.069(2) Uani 1 d . . H45 H -0.2768(5) 0.2689(6) 0.1140(4) 0.083 Uiso 1 calc R . C46 C -0.4038(4) 0.5691(5) 0.1528(3) 0.048(2) Uani 1 d . . H46A H -0.4271(4) 0.5092(5) 0.1365(3) 0.058 Uiso 1 calc R . H46B H -0.4461(4) 0.6170(5) 0.1413(3) 0.058 Uiso 1 calc R . C47 C -0.3759(4) 0.5628(5) 0.2191(3) 0.045(2) Uani 1 d . . C48 C -0.4061(5) 0.6211(5) 0.2575(3) 0.061(2) Uani 1 d . . H48 H -0.4495(5) 0.6662(5) 0.2414(3) 0.073 Uiso 1 calc R . C49 C -0.3737(6) 0.6139(6) 0.3183(4) 0.075(2) Uani 1 d . . H49 H -0.3931(6) 0.6547(6) 0.3454(4) 0.090 Uiso 1 calc R . C50 C -0.3135(6) 0.5482(6) 0.3402(3) 0.075(2) Uani 1 d . . H50 H -0.2900(6) 0.5420(6) 0.3829(3) 0.091 Uiso 1 calc R . C51 C -0.2870(5) 0.4910(5) 0.3008(3) 0.062(2) Uani 1 d . . H51 H -0.2459(5) 0.4433(5) 0.3167(3) 0.075 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0523(5) 0.0656(6) 0.0604(5) -0.0009(5) 0.0205(5) 0.0043(5) Cu2 0.0462(5) 0.0586(5) 0.0473(5) 0.0044(4) 0.0138(4) 0.0001(4) Cu3 0.0565(5) 0.0649(6) 0.0544(5) -0.0027(5) 0.0177(4) 0.0021(5) I1 0.0713(4) 0.0887(4) 0.0978(4) -0.0023(3) 0.0225(3) -0.0201(3) I2 0.0609(3) 0.0675(3) 0.0629(3) 0.0126(3) 0.0264(3) -0.0032(3) I3 0.0567(3) 0.0723(4) 0.0829(4) 0.0082(3) 0.0170(3) 0.0072(3) N1 0.040(3) 0.049(3) 0.035(3) 0.006(3) 0.016(2) 0.007(3) N2 0.033(3) 0.053(3) 0.037(3) -0.002(3) 0.009(2) 0.000(3) N3 0.037(3) 0.055(3) 0.035(3) -0.002(3) 0.013(2) -0.007(3) N4 0.052(4) 0.053(4) 0.045(3) -0.003(3) 0.014(3) 0.005(3) N5 0.060(4) 0.071(4) 0.046(4) -0.007(3) 0.010(3) 0.015(4) N6 0.044(3) 0.038(3) 0.043(3) 0.001(3) 0.016(3) 0.002(3) N7 0.037(3) 0.070(4) 0.050(4) 0.006(3) 0.011(3) 0.006(3) N8 0.057(4) 0.055(4) 0.057(4) -0.006(3) 0.022(3) 0.001(3) N9 0.065(4) 0.058(4) 0.050(4) 0.012(3) 0.022(3) 0.001(3) C1 0.043(4) 0.034(3) 0.040(4) -0.007(3) 0.017(3) 0.004(3) C2 0.033(4) 0.036(4) 0.038(3) -0.010(3) 0.013(3) 0.000(3) C3 0.039(4) 0.035(3) 0.033(3) -0.003(3) 0.012(3) 0.001(3) C4 0.041(4) 0.037(4) 0.032(3) -0.007(3) 0.014(3) 0.000(3) C5 0.035(4) 0.040(4) 0.036(3) -0.002(3) 0.015(3) -0.002(3) C6 0.031(3) 0.042(4) 0.038(3) -0.010(3) 0.013(3) 0.003(3) C7 0.039(4) 0.056(4) 0.038(4) 0.010(3) 0.014(3) 0.002(3) C8 0.059(5) 0.054(5) 0.082(5) -0.015(4) 0.022(4) -0.013(4) C9 0.046(4) 0.049(4) 0.041(4) 0.004(3) 0.018(3) -0.003(3) C10 0.058(5) 0.085(6) 0.048(4) -0.001(4) 0.023(4) 0.004(4) C11 0.043(4) 0.057(4) 0.040(4) 0.006(3) 0.014(3) 0.001(3) C12 0.054(5) 0.078(5) 0.085(6) 0.006(4) 0.026(4) 0.020(4) C13 0.039(4) 0.042(4) 0.038(4) 0.007(3) 0.015(3) 0.004(3) C14 0.042(4) 0.048(4) 0.043(4) 0.006(3) 0.014(3) 0.008(3) C15 0.044(4) 0.057(4) 0.038(4) 0.006(3) 0.012(3) 0.012(4) C16 0.048(4) 0.077(5) 0.054(4) 0.002(4) 0.018(4) 0.018(4) C17 0.078(6) 0.089(6) 0.065(5) -0.001(5) 0.041(5) 0.025(5) C18 0.094(7) 0.072(6) 0.052(5) -0.011(4) 0.020(5) 0.022(5) C19 0.060(5) 0.061(5) 0.060(5) -0.012(4) 0.013(4) 0.005(4) C20 0.065(5) 0.050(4) 0.035(4) 0.010(3) 0.013(4) 0.011(4) C21 0.071(5) 0.063(5) 0.033(4) 0.003(4) 0.012(4) 0.030(4) C22 0.112(8) 0.077(7) 0.084(6) -0.005(5) -0.002(6) 0.041(6) C23 0.137(11) 0.100(9) 0.118(9) -0.019(7) -0.010(8) 0.073(8) C24 0.084(8) 0.149(11) 0.095(8) -0.021(8) -0.006(6) 0.067(8) C25 0.058(6) 0.124(8) 0.057(5) -0.003(5) 0.001(4) 0.028(6) C26 0.048(4) 0.049(4) 0.038(4) -0.007(3) 0.012(3) -0.002(3) C27 0.064(5) 0.043(4) 0.051(4) 0.005(3) 0.024(4) 0.013(4) C28 0.042(4) 0.038(4) 0.056(4) -0.002(3) 0.014(4) 0.001(3) C29 0.076(6) 0.059(5) 0.071(5) -0.019(4) 0.036(5) -0.010(4) C30 0.055(5) 0.077(6) 0.087(6) -0.031(5) 0.028(5) -0.019(4) C31 0.061(5) 0.061(5) 0.060(5) -0.019(4) -0.005(4) 0.010(4) C32 0.062(5) 0.043(4) 0.052(4) -0.002(4) 0.020(4) 0.015(4) C33 0.045(4) 0.093(6) 0.042(4) -0.007(4) 0.012(3) 0.015(4) C34 0.040(4) 0.068(5) 0.046(4) 0.005(4) 0.001(4) 0.009(4) C35 0.052(5) 0.108(7) 0.048(4) 0.011(4) 0.002(4) 0.020(5) C36 0.054(5) 0.092(6) 0.087(7) 0.016(5) -0.002(5) 0.029(5) C37 0.048(5) 0.110(7) 0.076(6) -0.005(5) 0.011(5) 0.026(5) C38 0.051(5) 0.095(6) 0.060(5) -0.008(4) 0.020(4) -0.002(5) C39 0.037(4) 0.054(4) 0.040(4) -0.004(3) 0.015(3) -0.003(3) C40 0.046(4) 0.057(5) 0.044(4) -0.003(3) 0.015(3) -0.010(4) C41 0.044(4) 0.057(5) 0.050(4) -0.004(4) 0.022(4) -0.004(4) C42 0.062(5) 0.060(5) 0.053(5) -0.015(4) 0.013(4) 0.001(4) C43 0.076(6) 0.074(6) 0.060(5) -0.018(5) 0.012(5) -0.004(5) C44 0.094(7) 0.055(5) 0.086(6) -0.029(5) 0.032(5) -0.012(5) C45 0.077(6) 0.061(5) 0.075(6) -0.005(5) 0.030(5) 0.010(5) C46 0.033(4) 0.055(4) 0.060(4) 0.002(4) 0.020(3) -0.004(3) C47 0.041(4) 0.053(4) 0.048(4) 0.001(4) 0.024(4) -0.016(3) C48 0.070(5) 0.061(5) 0.066(5) 0.012(4) 0.044(4) -0.005(4) C49 0.113(7) 0.066(6) 0.066(6) 0.002(5) 0.058(5) -0.002(5) C50 0.102(7) 0.082(6) 0.053(5) 0.012(5) 0.039(5) -0.006(5) C51 0.069(5) 0.071(5) 0.051(5) 0.014(4) 0.025(4) 0.011(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N4 1.990(5) . ? Cu1 N5 2.002(6) . ? Cu1 I1 2.5186(10) . ? Cu2 N6 1.991(5) . ? Cu2 N7 2.002(5) . ? Cu2 I2 2.5335(9) . ? Cu3 N8 1.990(6) . ? Cu3 N9 2.005(6) . ? Cu3 I3 2.5114(10) . ? N1 C14 1.452(7) . ? N1 C20 1.469(7) . ? N1 C13 1.483(7) . ? N2 C33 1.444(7) . ? N2 C26 1.463(7) . ? N2 C27 1.463(7) . ? N3 C40 1.458(7) . ? N3 C46 1.466(7) . ? N3 C39 1.475(7) . ? N4 C15 1.328(8) . ? N4 C19 1.344(8) . ? N5 C21 1.333(9) . ? N5 C25 1.337(9) . ? N6 C32 1.334(8) . ? N6 C28 1.342(7) . ? N7 C38 1.336(8) . ? N7 C34 1.337(8) . ? N8 C45 1.339(8) . ? N8 C41 1.342(8) . ? N9 C51 1.335(8) . ? N9 C47 1.341(8) . ? C1 C2 1.399(8) . ? C1 C6 1.411(8) . ? C1 C13 1.513(8) . ? C2 C3 1.404(8) . ? C2 C7 1.518(8) . ? C3 C4 1.385(8) . ? C3 C26 1.520(8) . ? C4 C5 1.397(8) . ? C4 C9 1.508(8) . ? C5 C6 1.398(8) . ? C5 C39 1.526(7) . ? C6 C11 1.498(8) . ? C7 C8 1.516(8) . ? C9 C10 1.498(8) . ? C11 C12 1.527(8) . ? C14 C15 1.499(8) . ? C15 C16 1.377(8) . ? C16 C17 1.375(9) . ? C17 C18 1.371(10) . ? C18 C19 1.352(10) . ? C20 C21 1.493(9) . ? C21 C22 1.378(10) . ? C22 C23 1.351(13) . ? C23 C24 1.349(14) . ? C24 C25 1.372(12) . ? C27 C28 1.494(8) . ? C28 C29 1.367(9) . ? C29 C30 1.366(10) . ? C30 C31 1.355(10) . ? C31 C32 1.372(9) . ? C33 C34 1.512(8) . ? C34 C35 1.363(8) . ? C35 C36 1.386(10) . ? C36 C37 1.359(10) . ? C37 C38 1.340(9) . ? C40 C41 1.495(8) . ? C41 C42 1.367(9) . ? C42 C43 1.341(9) . ? C43 C44 1.375(10) . ? C44 C45 1.370(10) . ? C46 C47 1.475(8) . ? C47 C48 1.388(9) . ? C48 C49 1.362(10) . ? C49 C50 1.360(10) . ? C50 C51 1.364(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Cu1 N5 125.4(2) . . ? N4 Cu1 I1 115.9(2) . . ? N5 Cu1 I1 111.5(2) . . ? N6 Cu2 N7 125.4(2) . . ? N6 Cu2 I2 118.33(15) . . ? N7 Cu2 I2 111.0(2) . . ? N8 Cu3 N9 127.8(2) . . ? N8 Cu3 I3 117.7(2) . . ? N9 Cu3 I3 111.1(2) . . ? C14 N1 C20 110.2(5) . . ? C14 N1 C13 112.1(5) . . ? C20 N1 C13 107.8(5) . . ? C33 N2 C26 107.7(5) . . ? C33 N2 C27 110.4(5) . . ? C26 N2 C27 113.7(5) . . ? C40 N3 C46 111.1(5) . . ? C40 N3 C39 111.8(5) . . ? C46 N3 C39 107.9(5) . . ? C15 N4 C19 118.2(6) . . ? C15 N4 Cu1 123.0(4) . . ? C19 N4 Cu1 118.2(5) . . ? C21 N5 C25 117.8(7) . . ? C21 N5 Cu1 118.3(5) . . ? C25 N5 Cu1 123.6(6) . . ? C32 N6 C28 118.3(6) . . ? C32 N6 Cu2 123.0(5) . . ? C28 N6 Cu2 118.6(4) . . ? C38 N7 C34 116.8(6) . . ? C38 N7 Cu2 119.6(5) . . ? C34 N7 Cu2 123.0(4) . . ? C45 N8 C41 117.6(6) . . ? C45 N8 Cu3 118.3(5) . . ? C41 N8 Cu3 123.5(5) . . ? C51 N9 C47 118.5(6) . . ? C51 N9 Cu3 124.3(5) . . ? C47 N9 Cu3 115.5(4) . . ? C2 C1 C6 120.4(5) . . ? C2 C1 C13 120.6(5) . . ? C6 C1 C13 118.7(5) . . ? C3 C2 C1 119.3(5) . . ? C3 C2 C7 119.2(5) . . ? C1 C2 C7 121.5(5) . . ? C4 C3 C2 120.8(5) . . ? C4 C3 C26 121.4(5) . . ? C2 C3 C26 117.7(5) . . ? C3 C4 C5 119.6(5) . . ? C3 C4 C9 121.1(5) . . ? C5 C4 C9 119.2(5) . . ? C6 C5 C4 121.0(5) . . ? C6 C5 C39 119.2(5) . . ? C4 C5 C39 119.5(5) . . ? C5 C6 C1 118.9(5) . . ? C5 C6 C11 121.4(5) . . ? C1 C6 C11 119.7(5) . . ? C8 C7 C2 113.9(5) . . ? C10 C9 C4 113.3(5) . . ? C6 C11 C12 114.5(5) . . ? N1 C13 C1 115.6(5) . . ? N1 C14 C15 114.2(5) . . ? N4 C15 C16 121.8(6) . . ? N4 C15 C14 117.9(6) . . ? C16 C15 C14 120.1(6) . . ? C17 C16 C15 119.2(7) . . ? C16 C17 C18 118.7(7) . . ? C19 C18 C17 119.1(7) . . ? N4 C19 C18 122.9(7) . . ? N1 C20 C21 111.0(5) . . ? N5 C21 C22 121.9(8) . . ? N5 C21 C20 116.6(6) . . ? C22 C21 C20 121.5(8) . . ? C23 C22 C21 119.0(10) . . ? C24 C23 C22 120.0(10) . . ? C23 C24 C25 118.8(10) . . ? N5 C25 C24 122.5(9) . . ? N2 C26 C3 116.0(5) . . ? N2 C27 C28 112.6(5) . . ? N6 C28 C29 120.8(6) . . ? N6 C28 C27 116.3(6) . . ? C29 C28 C27 122.7(6) . . ? C30 C29 C28 120.6(7) . . ? C31 C30 C29 118.6(7) . . ? C30 C31 C32 119.1(7) . . ? N6 C32 C31 122.6(7) . . ? N2 C33 C34 115.6(5) . . ? N7 C34 C35 121.8(6) . . ? N7 C34 C33 118.3(6) . . ? C35 C34 C33 119.8(6) . . ? C34 C35 C36 119.6(7) . . ? C37 C36 C35 118.3(7) . . ? C38 C37 C36 118.6(8) . . ? N7 C38 C37 124.8(7) . . ? N3 C39 C5 116.5(5) . . ? N3 C40 C41 114.0(5) . . ? N8 C41 C42 121.4(7) . . ? N8 C41 C40 118.5(6) . . ? C42 C41 C40 120.1(7) . . ? C43 C42 C41 120.9(7) . . ? C42 C43 C44 118.7(7) . . ? C45 C44 C43 118.6(7) . . ? N8 C45 C44 122.8(8) . . ? N3 C46 C47 109.8(5) . . ? N9 C47 C48 120.9(6) . . ? N9 C47 C46 115.6(6) . . ? C48 C47 C46 123.4(7) . . ? C49 C48 C47 119.5(7) . . ? C50 C49 C48 119.3(7) . . ? C49 C50 C51 119.2(7) . . ? N9 C51 C50 122.6(7) . . ? _refine_diff_density_max 0.712 _refine_diff_density_min -0.623 _refine_diff_density_rms 0.086 #=END data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[L(CuNCMe)3](PF6)3-7CH2Cl2' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H80 Cl14 Cu3 F18 N12 P3' _chemical_formula_weight 2139.23 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.3631(2) _cell_length_b 17.4425(2) _cell_length_c 17.71480(10) _cell_angle_alpha 71.31 _cell_angle_beta 77.7710(10) _cell_angle_gamma 68.9740(10) _cell_volume 4443.72(8) _cell_formula_units_Z 2 _cell_measurement_temperature 188(2) _cell_measurement_reflns_used 18103 _cell_measurement_theta_min 1.91 _cell_measurement_theta_max 24.21 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.599 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2160 _exptl_absorpt_coefficient_mu 1.270 _exptl_absorpt_correction_type 'Semi-empirical from psi-scans (SADABS)' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 188(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18103 _diffrn_reflns_av_R_equivalents 0.0136 _diffrn_reflns_av_sigmaI/netI 0.0261 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 24.21 _reflns_number_total 13379 _reflns_number_gt 11743 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1007P)^2^+13.4856P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13379 _refine_ls_number_parameters 1068 _refine_ls_number_restraints 157 _refine_ls_R_factor_all 0.0749 _refine_ls_R_factor_gt 0.0662 _refine_ls_wR_factor_ref 0.1936 _refine_ls_wR_factor_gt 0.1819 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.091 _refine_ls_shift/su_mean 0.001 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 0.94296(4) 1.54494(4) 0.31899(4) 0.04010(18) Uani 1 1 d . . . Cu2 Cu 1.11192(4) 1.09472(4) 0.34102(4) 0.04682(19) Uani 1 1 d . . . Cu3 Cu 0.64551(4) 1.38155(4) 0.20349(4) 0.0474(2) Uani 1 1 d . . . P1 P 0.60555(12) 0.73877(12) 0.78331(11) 0.0657(5) Uani 1 1 d . . . P2 P 0.56423(11) 0.20607(13) 0.53849(12) 0.0664(5) Uani 1 1 d . . . P3 P 0.84310(11) 0.90940(10) 0.31686(10) 0.0555(4) Uani 1 1 d D . . F11 F 0.5711(3) 0.7820(3) 0.6984(3) 0.1029(16) Uani 1 1 d . . . F12 F 0.6236(3) 0.8231(3) 0.7831(3) 0.0990(15) Uani 1 1 d . . . F13 F 0.5860(5) 0.6571(4) 0.7843(3) 0.122(2) Uani 1 1 d . . . F14 F 0.6387(6) 0.6954(4) 0.8683(4) 0.150(3) Uani 1 1 d . . . F15 F 0.7007(3) 0.7095(4) 0.7404(4) 0.124(2) Uani 1 1 d . . . F16 F 0.5081(4) 0.7766(5) 0.8216(4) 0.133(2) Uani 1 1 d . . . F21 F 0.4956(4) 0.1696(5) 0.5271(5) 0.150(3) Uani 1 1 d . . . F22 F 0.6331(4) 0.1176(4) 0.5482(6) 0.161(3) Uani 1 1 d . . . F23 F 0.4923(4) 0.2971(4) 0.5266(5) 0.149(3) Uani 1 1 d . . . F24 F 0.6314(4) 0.2479(5) 0.5489(5) 0.139(2) Uani 1 1 d . . . F25 F 0.5938(9) 0.2297(6) 0.4491(4) 0.213(5) Uani 1 1 d . . . F26 F 0.5366(6) 0.1970(6) 0.6281(4) 0.170(3) Uani 1 1 d . . . F31 F 0.8461(14) 0.9191(14) 0.4003(8) 0.134(7) Uani 0.51(2) 1 d PD A 1 F32 F 0.8360(16) 0.8914(9) 0.2391(7) 0.102(5) Uani 0.51(2) 1 d PD A 1 F33 F 0.9443(7) 0.8821(10) 0.3031(15) 0.103(7) Uani 0.51(2) 1 d PD A 1 F34 F 0.7393(6) 0.9270(7) 0.3399(11) 0.079(4) Uani 0.51(2) 1 d PD A 1 F31B F 0.7575(14) 0.9343(7) 0.275(2) 0.144(12) Uani 0.49(2) 1 d PD A 2 F32B F 0.790(2) 0.9255(10) 0.3947(10) 0.168(13) Uani 0.49(2) 1 d PD A 2 F33B F 0.8983(19) 0.9025(9) 0.2316(8) 0.128(9) Uani 0.49(2) 1 d PD A 2 F34B F 0.9328(13) 0.8934(11) 0.3457(17) 0.126(10) Uani 0.49(2) 1 d PD A 2 F35 F 0.8519(3) 0.8117(3) 0.3511(4) 0.1033(17) Uani 1 1 d D A . F36 F 0.8315(3) 1.0079(2) 0.2805(3) 0.0867(13) Uani 1 1 d D A . Cl11 Cl 1.4245(4) 0.0904(3) 0.0334(3) 0.218(2) Uani 1 1 d D . . Cl12 Cl 1.4924(3) 0.2214(3) -0.0797(3) 0.1786(18) Uani 1 1 d D . . Cl21 Cl 0.71755(13) 0.43270(14) 0.47112(13) 0.0834(5) Uani 1 1 d D . . Cl22 Cl 0.83171(12) 0.36136(11) 0.34483(10) 0.0670(4) Uani 1 1 d D . . Cl31 Cl 0.69524(14) 0.53981(17) 0.61751(19) 0.1099(9) Uani 1 1 d D . . Cl32 Cl 0.75842(14) 0.68216(16) 0.52739(14) 0.0933(6) Uani 1 1 d D . . Cl41 Cl 0.64055(16) 0.3162(2) 0.77693(14) 0.1091(8) Uani 1 1 d D . . Cl42 Cl 0.78998(15) 0.24446(16) 0.67189(13) 0.0918(6) Uani 1 1 d D . . Cl51 Cl 1.5311(10) -0.0270(5) 0.3081(9) 0.490(10) Uani 1 1 d D . . Cl52 Cl 1.5496(5) -0.0797(5) 0.1763(4) 0.332(6) Uani 1 1 d D . . Cl61 Cl 1.2821(4) -0.1320(4) -0.0419(5) 0.263(3) Uani 1 1 d D . . Cl62 Cl 1.0939(4) -0.0750(3) -0.0321(3) 0.1761(17) Uani 1 1 d D . . Cl71 Cl 0.7574(2) 0.76680(17) 0.11170(18) 0.1390(13) Uani 1 1 d D . . Cl72 Cl 0.8800(2) 0.8613(2) 0.03733(17) 0.1221(9) Uani 1 1 d D . . N1 N 1.0636(2) 1.4394(2) 0.2731(2) 0.0310(8) Uani 1 1 d . . . N2 N 1.0262(3) 1.6129(3) 0.2603(2) 0.0401(9) Uani 1 1 d . . . N3 N 0.9637(3) 1.4485(3) 0.4179(2) 0.0374(9) Uani 1 1 d . . . N4 N 0.8238(3) 1.6217(3) 0.3122(3) 0.0506(11) Uani 1 1 d . . . N5 N 1.0035(3) 1.1324(2) 0.2435(2) 0.0345(9) Uani 1 1 d . . . N6 N 0.9965(3) 1.1160(2) 0.4068(2) 0.0376(9) Uani 1 1 d . . . N7 N 1.1744(3) 1.0144(3) 0.2716(3) 0.0570(13) Uani 1 1 d . . . N8 N 1.2034(4) 1.1145(4) 0.3824(3) 0.0621(13) Uani 1 1 d . . . N9 N 0.7125(2) 1.4924(2) 0.1333(2) 0.0338(8) Uani 1 1 d . . . N10 N 0.6020(3) 1.4587(3) 0.2753(3) 0.0502(11) Uani 1 1 d . . . N11 N 0.6151(3) 1.4099(3) 0.0906(3) 0.0425(10) Uani 1 1 d . . . N12 N 0.6664(3) 1.2608(3) 0.2557(3) 0.0548(12) Uani 1 1 d . . . C1 C 1.0189(3) 1.3978(3) 0.1683(2) 0.0286(9) Uani 1 1 d . . . C2 C 1.0426(3) 1.3115(3) 0.1710(2) 0.0293(9) Uani 1 1 d . . . C3 C 0.9826(3) 1.2811(3) 0.1535(2) 0.0276(9) Uani 1 1 d . . . C4 C 0.9015(3) 1.3372(3) 0.1283(2) 0.0281(9) Uani 1 1 d . . . C5 C 0.8794(3) 1.4251(3) 0.1214(2) 0.0286(9) Uani 1 1 d . . . C6 C 0.9378(3) 1.4551(3) 0.1425(2) 0.0266(9) Uani 1 1 d . . . C7 C 1.1343(3) 1.2515(3) 0.1873(3) 0.0340(10) Uani 1 1 d . . . H7A H 1.1316 1.1951 0.2142 0.041 Uiso 1 1 calc R . . H7B H 1.1573 1.2695 0.2219 0.041 Uiso 1 1 calc R . . C8 C 1.1961(3) 1.2500(4) 0.1093(3) 0.0489(13) Uani 1 1 d . . . H8A H 1.2538 1.2119 0.1212 0.059 Uiso 1 1 calc R . . H8B H 1.1994 1.3064 0.0826 0.059 Uiso 1 1 calc R . . H8C H 1.1738 1.2309 0.0751 0.059 Uiso 1 1 calc R . . C9 C 0.9188(3) 1.5491(3) 0.1323(3) 0.0316(10) Uani 1 1 d . . . H9A H 0.9439 1.5559 0.1732 0.038 Uiso 1 1 calc R . . H9B H 0.8563 1.5758 0.1394 0.038 Uiso 1 1 calc R . . C10 C 0.9560(4) 1.5937(3) 0.0500(3) 0.0410(11) Uani 1 1 d . . . H10A H 0.9423 1.6530 0.0463 0.049 Uiso 1 1 calc R . . H10B H 0.9303 1.5880 0.0090 0.049 Uiso 1 1 calc R . . H10C H 1.0187 1.5681 0.0431 0.049 Uiso 1 1 calc R . . C11 C 0.8393(3) 1.3063(3) 0.1033(3) 0.0339(10) Uani 1 1 d . . . H11A H 0.7802 1.3430 0.1116 0.041 Uiso 1 1 calc R . . H11B H 0.8423 1.2501 0.1369 0.041 Uiso 1 1 calc R . . C12 C 0.8594(4) 1.3037(4) 0.0155(3) 0.0449(12) Uani 1 1 d . . . H12A H 0.8175 1.2838 0.0030 0.054 Uiso 1 1 calc R . . H12B H 0.9177 1.2658 0.0070 0.054 Uiso 1 1 calc R . . H12C H 0.8554 1.3599 -0.0186 0.054 Uiso 1 1 calc R . . C13 C 1.0824(3) 1.4304(3) 0.1898(3) 0.0311(10) Uani 1 1 d . . . H13A H 1.1410 1.3921 0.1831 0.037 Uiso 1 1 calc R . . H13B H 1.0808 1.4849 0.1530 0.037 Uiso 1 1 calc R . . C14 C 1.1297(3) 1.4722(3) 0.2855(3) 0.0397(11) Uani 1 1 d . . . H14A H 1.1868 1.4426 0.2634 0.048 Uiso 1 1 calc R . . H14B H 1.1312 1.4611 0.3420 0.048 Uiso 1 1 calc R . . C15 C 1.1099(3) 1.5661(3) 0.2471(3) 0.0393(11) Uani 1 1 d . . . C16 C 1.1740(4) 1.6026(4) 0.2048(3) 0.0515(14) Uani 1 1 d . . . H16 H 1.2338 1.5679 0.1954 0.062 Uiso 1 1 calc R . . C17 C 1.1497(5) 1.6907(5) 0.1762(4) 0.0621(17) Uani 1 1 d . . . H17 H 1.1929 1.7179 0.1466 0.075 Uiso 1 1 calc R . . C18 C 1.0645(5) 1.7386(4) 0.1901(4) 0.0618(17) Uani 1 1 d . . . H18 H 1.0472 1.7997 0.1715 0.074 Uiso 1 1 calc R . . C19 C 1.0042(4) 1.6984(4) 0.2311(3) 0.0513(14) Uani 1 1 d . . . H19 H 0.9438 1.7322 0.2395 0.062 Uiso 1 1 calc R . . C20 C 1.0642(3) 1.3596(3) 0.3337(3) 0.0345(10) Uani 1 1 d . . . H20A H 1.1242 1.3242 0.3396 0.041 Uiso 1 1 calc R . . H20B H 1.0360 1.3302 0.3154 0.041 Uiso 1 1 calc R . . C21 C 1.0190(3) 1.3715(3) 0.4138(3) 0.0359(10) Uani 1 1 d . . . C22 C 1.0311(4) 1.3024(3) 0.4815(3) 0.0448(12) Uani 1 1 d . . . H22 H 1.0727 1.2481 0.4779 0.054 Uiso 1 1 calc R . . C23 C 0.9835(4) 1.3121(4) 0.5534(3) 0.0509(14) Uani 1 1 d . . . H23 H 0.9902 1.2646 0.6003 0.061 Uiso 1 1 calc R . . C24 C 0.9257(4) 1.3912(4) 0.5570(3) 0.0479(13) Uani 1 1 d . . . H24 H 0.8911 1.3999 0.6063 0.057 Uiso 1 1 calc R . . C25 C 0.9188(3) 1.4571(3) 0.4890(3) 0.0424(12) Uani 1 1 d . . . H25 H 0.8796 1.5124 0.4922 0.051 Uiso 1 1 calc R . . C26 C 0.7639(4) 1.6782(4) 0.3200(4) 0.0505(13) Uani 1 1 d . . . C27 C 0.6878(4) 1.7512(5) 0.3284(5) 0.075(2) Uani 1 1 d . . . H27A H 0.7053 1.7905 0.3439 0.090 Uiso 1 1 calc R . . H27B H 0.6444 1.7326 0.3687 0.090 Uiso 1 1 calc R . . H27C H 0.6634 1.7788 0.2782 0.090 Uiso 1 1 calc R . . C28 C 1.0071(3) 1.1869(3) 0.1596(3) 0.0334(10) Uani 1 1 d . . . H28A H 0.9677 1.1792 0.1315 0.040 Uiso 1 1 calc R . . H28B H 1.0656 1.1683 0.1335 0.040 Uiso 1 1 calc R . . C29 C 0.9180(3) 1.1573(3) 0.2893(3) 0.0373(11) Uani 1 1 d . . . H29A H 0.8799 1.1326 0.2776 0.045 Uiso 1 1 calc R . . H29B H 0.8927 1.2182 0.2721 0.045 Uiso 1 1 calc R . . C30 C 0.9209(3) 1.1308(3) 0.3788(3) 0.0380(11) Uani 1 1 d . . . C31 C 0.8441(4) 1.1292(4) 0.4288(3) 0.0492(13) Uani 1 1 d . . . H31 H 0.7915 1.1373 0.4074 0.059 Uiso 1 1 calc R . . C32 C 0.8439(4) 1.1156(4) 0.5102(3) 0.0549(15) Uani 1 1 d . . . H32 H 0.7912 1.1144 0.5461 0.066 Uiso 1 1 calc R . . C33 C 0.9211(4) 1.1038(3) 0.5387(3) 0.0497(14) Uani 1 1 d . . . H33 H 0.9224 1.0966 0.5946 0.060 Uiso 1 1 calc R . . C34 C 0.9951(4) 1.1027(3) 0.4862(3) 0.0439(12) Uani 1 1 d . . . H34 H 1.0491 1.0920 0.5068 0.053 Uiso 1 1 calc R . . C35 C 1.0282(4) 1.0436(3) 0.2416(3) 0.0478(13) Uani 1 1 d . . . H35A H 0.9995 1.0406 0.2011 0.057 Uiso 1 1 calc R . . H35B H 1.0087 1.0105 0.2924 0.057 Uiso 1 1 calc R . . C36 C 1.1261(4) 1.0070(3) 0.2241(3) 0.0540(15) Uani 1 1 d . . . C37 C 1.1648(6) 0.9654(4) 0.1640(4) 0.082(2) Uani 1 1 d . . . H37 H 1.1289 0.9608 0.1303 0.098 Uiso 1 1 calc R . . C38 C 1.2538(8) 0.9317(6) 0.1536(6) 0.111(4) Uani 1 1 d . . . H38 H 1.2817 0.9028 0.1125 0.134 Uiso 1 1 calc R . . C39 C 1.3029(7) 0.9393(6) 0.2023(7) 0.110(4) Uani 1 1 d . . . H39 H 1.3659 0.9155 0.1958 0.131 Uiso 1 1 calc R . . C40 C 1.2630(5) 0.9806(5) 0.2603(5) 0.078(2) Uani 1 1 d . . . H40 H 1.2985 0.9858 0.2940 0.094 Uiso 1 1 calc R . . C41 C 1.2625(4) 1.1045(4) 0.4124(4) 0.0575(15) Uani 1 1 d . . . C42 C 1.3390(5) 1.0910(5) 0.4500(5) 0.0741(19) Uani 1 1 d . . . H42A H 1.3202 1.1066 0.4996 0.089 Uiso 1 1 calc R . . H42B H 1.3736 1.1254 0.4149 0.089 Uiso 1 1 calc R . . H42C H 1.3740 1.0320 0.4602 0.089 Uiso 1 1 calc R . . C43 C 0.7978(3) 1.4865(3) 0.0820(3) 0.0322(10) Uani 1 1 d . . . H43A H 0.8043 1.5423 0.0630 0.039 Uiso 1 1 calc R . . H43B H 0.7953 1.4698 0.0361 0.039 Uiso 1 1 calc R . . C44 C 0.7040(3) 1.5356(3) 0.1947(3) 0.0408(11) Uani 1 1 d . . . H44A H 0.6957 1.5950 0.1692 0.049 Uiso 1 1 calc R . . H44B H 0.7579 1.5125 0.2190 0.049 Uiso 1 1 calc R . . C45 C 0.6287(3) 1.5273(4) 0.2595(3) 0.0472(13) Uani 1 1 d . . . C46 C 0.5925(4) 1.5857(5) 0.3037(4) 0.0633(17) Uani 1 1 d . . . H46 H 0.6103 1.6357 0.2900 0.076 Uiso 1 1 calc R . . C47 C 0.5303(4) 1.5717(6) 0.3679(5) 0.077(2) Uani 1 1 d . . . H47 H 0.5041 1.6120 0.3994 0.092 Uiso 1 1 calc R . . C48 C 0.5062(4) 1.4994(5) 0.3863(4) 0.072(2) Uani 1 1 d . . . H48 H 0.4647 1.4871 0.4320 0.086 Uiso 1 1 calc R . . C49 C 0.5425(4) 1.4457(5) 0.3386(4) 0.0635(17) Uani 1 1 d . . . H49 H 0.5246 1.3960 0.3508 0.076 Uiso 1 1 calc R . . C50 C 0.6416(3) 1.5400(3) 0.0803(3) 0.0439(12) Uani 1 1 d . . . H50A H 0.6574 1.5859 0.0400 0.053 Uiso 1 1 calc R . . H50B H 0.5882 1.5643 0.1112 0.053 Uiso 1 1 calc R . . C51 C 0.6260(3) 1.4825(3) 0.0404(3) 0.0420(12) Uani 1 1 d . . . C52 C 0.6210(3) 1.5038(4) -0.0410(3) 0.0512(14) Uani 1 1 d . . . H52 H 0.6294 1.5561 -0.0755 0.061 Uiso 1 1 calc R . . C53 C 0.6039(4) 1.4484(5) -0.0719(4) 0.0579(16) Uani 1 1 d . . . H53 H 0.5994 1.4621 -0.1282 0.069 Uiso 1 1 calc R . . C54 C 0.5932(4) 1.3734(5) -0.0211(4) 0.0610(16) Uani 1 1 d . . . H54 H 0.5818 1.3337 -0.0413 0.073 Uiso 1 1 calc R . . C55 C 0.5992(3) 1.3564(4) 0.0594(4) 0.0504(13) Uani 1 1 d . . . H55 H 0.5917 1.3041 0.0947 0.060 Uiso 1 1 calc R . . C56 C 0.6518(4) 1.1991(4) 0.2890(4) 0.0506(13) Uani 1 1 d . . . C57 C 0.6321(5) 1.1216(4) 0.3310(4) 0.0661(17) Uani 1 1 d . . . H57A H 0.5723 1.1348 0.3556 0.079 Uiso 1 1 calc R . . H57B H 0.6712 1.0888 0.3715 0.079 Uiso 1 1 calc R . . H57C H 0.6394 1.0891 0.2939 0.079 Uiso 1 1 calc R . . C61 C 1.4418(12) 0.1875(9) 0.0112(8) 0.187(8) Uani 1 1 d D . . H61A H 1.3856 0.2298 0.0170 0.224 Uiso 1 1 calc R . . H61B H 1.4758 0.1846 0.0505 0.224 Uiso 1 1 calc R . . C62 C 0.7700(6) 0.3418(5) 0.4380(4) 0.090(3) Uani 1 1 d D . . H62A H 0.7265 0.3183 0.4344 0.108 Uiso 1 1 calc R . . H62B H 0.8081 0.3002 0.4766 0.108 Uiso 1 1 calc R . . C63 C 0.6696(5) 0.6506(5) 0.5853(5) 0.094(3) Uani 1 1 d D . . H63A H 0.6205 0.6740 0.5543 0.113 Uiso 1 1 calc R . . H63B H 0.6524 0.6731 0.6312 0.113 Uiso 1 1 calc R . . C64 C 0.6767(5) 0.2928(7) 0.6856(5) 0.095(3) Uani 1 1 d D . . H64A H 0.6604 0.3446 0.6436 0.113 Uiso 1 1 calc R . . H64B H 0.6475 0.2557 0.6813 0.113 Uiso 1 1 calc R . . C65 C 1.5679(14) 0.0000(10) 0.2053(10) 0.53(4) Uani 1 1 d D . . H65A H 1.6291 -0.0040 0.1962 0.635 Uiso 1 1 calc R . . H65B H 1.5337 0.0561 0.1782 0.635 Uiso 1 1 calc R . . C66 C 1.1931(8) -0.0863(9) -0.0927(7) 0.222(11) Uani 1 1 d D . . H66A H 1.1964 -0.1200 -0.1274 0.267 Uiso 1 1 calc R . . H66B H 1.1943 -0.0310 -0.1258 0.267 Uiso 1 1 calc R . . C67 C 0.7769(8) 0.8638(7) 0.0847(10) 0.163(6) Uani 1 1 d D . . H67A H 0.7343 0.9051 0.0499 0.196 Uiso 1 1 calc R . . H67B H 0.7684 0.8825 0.1320 0.196 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0353(3) 0.0413(4) 0.0378(3) -0.0088(3) -0.0040(2) -0.0066(3) Cu2 0.0419(4) 0.0500(4) 0.0409(4) -0.0083(3) -0.0015(3) -0.0105(3) Cu3 0.0469(4) 0.0423(4) 0.0461(4) -0.0093(3) 0.0007(3) -0.0115(3) P1 0.0601(10) 0.0696(11) 0.0617(10) -0.0048(8) -0.0115(8) -0.0224(8) P2 0.0479(9) 0.0843(13) 0.0692(11) -0.0319(9) -0.0055(8) -0.0140(8) P3 0.0582(9) 0.0436(8) 0.0651(10) -0.0160(7) -0.0107(8) -0.0130(7) F11 0.082(3) 0.119(4) 0.073(3) 0.003(3) -0.023(2) -0.010(3) F12 0.087(3) 0.065(3) 0.142(4) -0.019(3) -0.012(3) -0.029(2) F13 0.203(6) 0.113(4) 0.085(3) -0.004(3) -0.046(4) -0.093(4) F14 0.281(9) 0.106(4) 0.101(4) 0.026(3) -0.108(5) -0.104(5) F15 0.052(3) 0.136(5) 0.190(6) -0.086(4) -0.018(3) 0.006(3) F16 0.104(4) 0.200(7) 0.128(5) -0.084(5) 0.055(3) -0.089(4) F21 0.091(4) 0.158(6) 0.254(9) -0.103(6) -0.036(5) -0.047(4) F22 0.068(3) 0.093(4) 0.303(10) -0.057(5) -0.032(5) 0.006(3) F23 0.116(5) 0.121(5) 0.225(8) -0.091(5) -0.074(5) 0.014(4) F24 0.086(4) 0.185(6) 0.193(7) -0.105(6) 0.009(4) -0.062(4) F25 0.398(16) 0.175(7) 0.078(4) -0.042(4) 0.035(6) -0.131(9) F26 0.211(8) 0.235(9) 0.087(4) -0.054(5) 0.025(5) -0.112(7) F31 0.122(14) 0.223(18) 0.104(10) -0.095(11) -0.012(9) -0.065(13) F32 0.149(15) 0.111(9) 0.064(7) -0.041(6) -0.016(8) -0.044(11) F33 0.053(6) 0.068(7) 0.18(2) -0.026(11) 0.011(9) -0.025(5) F34 0.062(5) 0.055(6) 0.107(11) -0.014(6) -0.001(6) -0.012(4) F31B 0.109(13) 0.061(7) 0.27(3) 0.004(12) -0.118(18) -0.026(8) F32B 0.21(3) 0.111(10) 0.096(13) -0.012(9) 0.087(15) -0.013(14) F33B 0.166(19) 0.079(8) 0.085(9) -0.025(6) 0.020(10) 0.009(9) F34B 0.139(17) 0.062(9) 0.19(2) 0.021(10) -0.121(16) -0.038(10) F35 0.084(3) 0.054(2) 0.165(5) -0.006(3) -0.031(3) -0.024(2) F36 0.086(3) 0.046(2) 0.117(4) -0.010(2) -0.007(3) -0.021(2) Cl11 0.288(7) 0.143(4) 0.193(5) -0.040(3) -0.041(4) -0.030(4) Cl12 0.175(4) 0.195(4) 0.209(4) -0.123(4) 0.066(3) -0.097(3) Cl21 0.0683(11) 0.0899(13) 0.0934(14) -0.0461(11) 0.0000(10) -0.0126(10) Cl22 0.0687(10) 0.0688(10) 0.0613(9) -0.0209(8) 0.0001(8) -0.0201(8) Cl31 0.0632(12) 0.1136(18) 0.186(3) -0.0803(18) -0.0248(14) -0.0247(11) Cl32 0.0709(12) 0.1143(17) 0.0882(14) -0.0297(12) -0.0219(10) -0.0116(11) Cl41 0.0813(14) 0.176(3) 0.0814(14) -0.0628(16) 0.0051(11) -0.0364(15) Cl42 0.0825(13) 0.1192(17) 0.0786(13) -0.0405(12) 0.0062(10) -0.0335(12) Cl51 0.54(2) 0.170(7) 0.80(3) -0.184(12) -0.21(2) -0.028(9) Cl52 0.287(8) 0.381(10) 0.238(6) -0.194(7) -0.109(6) 0.144(7) Cl61 0.283(7) 0.192(5) 0.311(8) -0.119(5) -0.136(6) 0.032(5) Cl62 0.259(5) 0.132(3) 0.177(4) -0.052(3) -0.022(4) -0.098(3) Cl71 0.189(3) 0.0777(15) 0.1084(19) -0.0267(14) 0.051(2) -0.0293(17) Cl72 0.148(3) 0.131(2) 0.0960(17) -0.0425(16) 0.0051(16) -0.0541(19) N1 0.030(2) 0.035(2) 0.0289(19) -0.0101(16) -0.0056(15) -0.0094(16) N2 0.044(2) 0.041(2) 0.036(2) -0.0124(18) -0.0023(18) -0.0128(19) N3 0.037(2) 0.044(2) 0.031(2) -0.0126(18) -0.0045(17) -0.0090(18) N4 0.040(3) 0.056(3) 0.048(3) -0.013(2) -0.006(2) -0.006(2) N5 0.039(2) 0.028(2) 0.032(2) -0.0038(16) -0.0039(16) -0.0077(16) N6 0.042(2) 0.033(2) 0.032(2) -0.0053(17) -0.0044(17) -0.0075(17) N7 0.052(3) 0.046(3) 0.050(3) -0.009(2) 0.002(2) 0.003(2) N8 0.050(3) 0.073(4) 0.058(3) -0.012(3) -0.002(3) -0.020(3) N9 0.0252(19) 0.031(2) 0.041(2) -0.0085(17) -0.0072(16) -0.0042(15) N10 0.036(2) 0.060(3) 0.054(3) -0.020(2) 0.007(2) -0.016(2) N11 0.029(2) 0.046(2) 0.050(3) -0.009(2) -0.0099(18) -0.0096(18) N12 0.060(3) 0.052(3) 0.046(3) -0.010(2) -0.005(2) -0.013(2) C1 0.031(2) 0.034(2) 0.021(2) -0.0067(17) 0.0011(17) -0.0129(19) C2 0.031(2) 0.031(2) 0.021(2) -0.0042(17) -0.0013(17) -0.0064(18) C3 0.032(2) 0.026(2) 0.022(2) -0.0043(17) -0.0009(17) -0.0077(18) C4 0.032(2) 0.034(2) 0.020(2) -0.0050(17) -0.0006(17) -0.0144(19) C5 0.028(2) 0.029(2) 0.024(2) -0.0033(17) 0.0000(17) -0.0083(18) C6 0.031(2) 0.026(2) 0.020(2) -0.0057(16) 0.0025(17) -0.0092(18) C7 0.031(2) 0.034(2) 0.034(2) -0.0105(19) -0.0069(19) -0.0039(19) C8 0.032(3) 0.058(3) 0.046(3) -0.019(3) -0.001(2) 0.001(2) C9 0.030(2) 0.032(2) 0.031(2) -0.0076(19) -0.0016(18) -0.0092(19) C10 0.051(3) 0.034(3) 0.035(3) -0.003(2) 0.001(2) -0.018(2) C11 0.034(2) 0.033(2) 0.036(3) -0.0059(19) -0.0063(19) -0.0128(19) C12 0.052(3) 0.053(3) 0.038(3) -0.014(2) -0.011(2) -0.021(3) C13 0.026(2) 0.036(2) 0.029(2) -0.0103(19) 0.0000(17) -0.0086(19) C14 0.035(3) 0.049(3) 0.040(3) -0.016(2) -0.008(2) -0.012(2) C15 0.044(3) 0.050(3) 0.035(3) -0.017(2) -0.008(2) -0.020(2) C16 0.052(3) 0.076(4) 0.042(3) -0.022(3) -0.001(2) -0.035(3) C17 0.083(5) 0.077(5) 0.044(3) -0.012(3) -0.001(3) -0.053(4) C18 0.092(5) 0.053(4) 0.049(3) -0.006(3) -0.010(3) -0.039(4) C19 0.063(4) 0.043(3) 0.047(3) -0.011(2) -0.011(3) -0.014(3) C20 0.033(2) 0.037(3) 0.032(2) -0.011(2) -0.0064(19) -0.006(2) C21 0.032(2) 0.044(3) 0.033(2) -0.012(2) -0.0062(19) -0.010(2) C22 0.051(3) 0.043(3) 0.036(3) -0.008(2) -0.012(2) -0.008(2) C23 0.058(3) 0.058(4) 0.031(3) -0.005(2) -0.009(2) -0.015(3) C24 0.050(3) 0.065(4) 0.030(3) -0.017(2) 0.002(2) -0.021(3) C25 0.042(3) 0.047(3) 0.039(3) -0.020(2) 0.001(2) -0.010(2) C26 0.037(3) 0.059(4) 0.054(3) -0.018(3) -0.006(2) -0.011(3) C27 0.046(4) 0.075(5) 0.103(6) -0.043(4) -0.010(4) 0.000(3) C28 0.042(3) 0.030(2) 0.026(2) -0.0063(18) -0.0048(19) -0.010(2) C29 0.040(3) 0.038(3) 0.032(2) -0.004(2) -0.007(2) -0.013(2) C30 0.046(3) 0.027(2) 0.035(3) -0.0026(19) -0.004(2) -0.010(2) C31 0.043(3) 0.053(3) 0.040(3) 0.001(2) -0.003(2) -0.015(2) C32 0.050(3) 0.051(3) 0.042(3) 0.000(2) 0.006(3) -0.008(3) C33 0.061(4) 0.036(3) 0.033(3) -0.001(2) -0.002(2) -0.002(2) C34 0.052(3) 0.035(3) 0.037(3) -0.007(2) -0.010(2) -0.005(2) C35 0.068(4) 0.031(3) 0.040(3) -0.003(2) -0.011(3) -0.013(2) C36 0.076(4) 0.028(3) 0.037(3) -0.003(2) -0.002(3) 0.000(3) C37 0.112(6) 0.049(4) 0.056(4) -0.019(3) -0.006(4) 0.008(4) C38 0.126(9) 0.083(6) 0.079(6) -0.039(5) 0.012(6) 0.023(6) C39 0.083(6) 0.088(6) 0.105(7) -0.029(6) 0.029(6) 0.016(5) C40 0.057(4) 0.068(4) 0.075(5) -0.016(4) 0.003(3) 0.012(3) C41 0.049(4) 0.062(4) 0.055(4) -0.005(3) -0.002(3) -0.022(3) C42 0.060(4) 0.082(5) 0.076(5) -0.006(4) -0.020(3) -0.024(4) C43 0.029(2) 0.033(2) 0.032(2) -0.0038(19) -0.0060(18) -0.0099(19) C44 0.030(2) 0.039(3) 0.050(3) -0.011(2) -0.004(2) -0.008(2) C45 0.029(3) 0.057(3) 0.055(3) -0.022(3) -0.001(2) -0.009(2) C46 0.039(3) 0.077(4) 0.090(5) -0.051(4) -0.001(3) -0.015(3) C47 0.043(4) 0.115(6) 0.091(5) -0.069(5) 0.005(3) -0.016(4) C48 0.045(3) 0.116(6) 0.066(4) -0.047(4) 0.017(3) -0.030(4) C49 0.046(3) 0.084(5) 0.064(4) -0.028(4) 0.011(3) -0.028(3) C50 0.033(3) 0.039(3) 0.055(3) -0.006(2) -0.012(2) -0.007(2) C51 0.024(2) 0.041(3) 0.056(3) -0.010(2) -0.008(2) -0.005(2) C52 0.035(3) 0.058(3) 0.049(3) -0.003(3) -0.010(2) -0.008(2) C53 0.039(3) 0.085(5) 0.050(3) -0.025(3) -0.014(3) -0.009(3) C54 0.040(3) 0.078(4) 0.076(4) -0.037(4) -0.011(3) -0.014(3) C55 0.035(3) 0.051(3) 0.067(4) -0.016(3) -0.009(3) -0.014(2) C56 0.047(3) 0.044(3) 0.053(3) -0.012(3) -0.010(3) -0.005(3) C57 0.061(4) 0.044(3) 0.083(5) -0.010(3) -0.008(3) -0.011(3) C61 0.222(17) 0.183(15) 0.190(15) -0.104(12) 0.099(13) -0.125(13) C62 0.118(7) 0.070(5) 0.067(5) -0.024(4) 0.017(4) -0.023(5) C63 0.050(4) 0.115(7) 0.105(6) -0.045(5) -0.015(4) 0.007(4) C64 0.089(6) 0.125(8) 0.075(5) -0.036(5) -0.013(4) -0.030(5) C65 0.58(6) 0.43(4) 0.54(5) -0.44(5) -0.47(5) 0.39(4) C66 0.43(3) 0.242(19) 0.089(8) 0.043(10) -0.079(14) -0.26(2) C67 0.135(11) 0.133(11) 0.221(17) -0.093(11) 0.015(11) -0.021(9) _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 N4 1.932(5) . ? Cu1 N3 1.993(4) . ? Cu1 N2 2.027(4) . ? Cu1 N1 2.370(4) . ? Cu1 Cu2 7.2373(9) . ? Cu1 Cu3 7.3421(10) . ? Cu2 N8 1.974(6) . ? Cu2 N6 1.976(4) . ? Cu2 N7 2.015(5) . ? Cu2 N5 2.509(4) . ? Cu2 Cu3 7.8663(9) . ? Cu3 N12 1.943(5) . ? Cu3 N10 1.989(5) . ? Cu3 N11 2.025(4) . ? Cu3 N9 2.427(4) . ? P1 F15 1.562(5) . ? P1 F13 1.562(5) . ? P1 F14 1.567(5) . ? P1 F11 1.573(5) . ? P1 F16 1.585(6) . ? P1 F12 1.599(5) . ? P2 F25 1.520(7) . ? P2 F26 1.529(7) . ? P2 F22 1.532(6) . ? P2 F21 1.547(5) . ? P2 F23 1.581(6) . ? P2 F24 1.588(6) . ? P3 F32B 1.517(10) . ? P3 F33 1.538(10) . ? P3 F32 1.543(9) . ? P3 F31 1.553(10) . ? P3 F34B 1.558(11) . ? P3 F35 1.579(4) . ? P3 F31B 1.581(10) . ? P3 F36 1.585(4) . ? P3 F34 1.599(9) . ? P3 F33B 1.604(10) . ? Cl11 C61 1.724(10) . ? Cl12 C61 1.674(10) . ? Cl21 C62 1.732(7) . ? Cl22 C62 1.743(7) . ? Cl31 C63 1.746(8) . ? Cl32 C63 1.746(8) . ? Cl41 C64 1.726(7) . ? Cl42 C64 1.739(8) . ? Cl51 C65 1.758(14) . ? Cl52 C65 1.764(13) . ? Cl61 C66 1.682(11) . ? Cl62 C66 1.731(12) . ? Cl71 C67 1.731(10) . ? Cl72 C67 1.710(10) . ? N1 C20 1.459(6) . ? N1 C14 1.474(6) . ? N1 C13 1.490(6) . ? N2 C15 1.334(7) . ? N2 C19 1.350(7) . ? N3 C21 1.337(6) . ? N3 C25 1.341(6) . ? N4 C26 1.135(7) . ? N5 C29 1.454(6) . ? N5 C35 1.464(6) . ? N5 C28 1.489(6) . ? N6 C30 1.338(7) . ? N6 C34 1.349(7) . ? N7 C36 1.333(8) . ? N7 C40 1.352(9) . ? N8 C41 1.132(8) . ? N9 C44 1.468(7) . ? N9 C50 1.479(6) . ? N9 C43 1.484(6) . ? N10 C49 1.338(8) . ? N10 C45 1.345(7) . ? N11 C51 1.342(7) . ? N11 C55 1.346(7) . ? N12 C56 1.132(7) . ? C1 C2 1.401(6) . ? C1 C6 1.408(6) . ? C1 C13 1.509(6) . ? C2 C3 1.396(6) . ? C2 C7 1.514(6) . ? C3 C4 1.400(6) . ? C3 C28 1.517(6) . ? C4 C5 1.412(6) . ? C4 C11 1.504(6) . ? C5 C6 1.403(6) . ? C5 C43 1.518(6) . ? C6 C9 1.511(6) . ? C7 C8 1.531(7) . ? C9 C10 1.529(6) . ? C11 C12 1.533(7) . ? C14 C15 1.499(7) . ? C15 C16 1.382(8) . ? C16 C17 1.387(9) . ? C17 C18 1.361(10) . ? C18 C19 1.364(9) . ? C20 C21 1.496(7) . ? C21 C22 1.391(7) . ? C22 C23 1.372(8) . ? C23 C24 1.377(8) . ? C24 C25 1.364(8) . ? C26 C27 1.448(9) . ? C29 C30 1.508(7) . ? C30 C31 1.379(7) . ? C31 C32 1.384(8) . ? C32 C33 1.382(9) . ? C33 C34 1.361(8) . ? C35 C36 1.501(9) . ? C36 C37 1.393(9) . ? C37 C38 1.357(14) . ? C38 C39 1.362(15) . ? C39 C40 1.361(12) . ? C41 C42 1.453(10) . ? C44 C45 1.510(7) . ? C45 C46 1.372(8) . ? C46 C47 1.378(10) . ? C47 C48 1.376(11) . ? C48 C49 1.357(10) . ? C50 C51 1.512(8) . ? C51 C52 1.382(8) . ? C52 C53 1.382(9) . ? C53 C54 1.378(10) . ? C54 C55 1.377(9) . ? C56 C57 1.433(9) . ? 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 N4 Cu1 N3 116.24(19) . . ? N4 Cu1 N2 108.09(19) . . ? N3 Cu1 N2 126.01(17) . . ? N4 Cu1 N1 150.16(17) . . ? N3 Cu1 N1 77.71(15) . . ? N2 Cu1 N1 78.85(15) . . ? N4 Cu1 Cu2 129.48(15) . . ? N3 Cu1 Cu2 53.17(12) . . ? N2 Cu1 Cu2 115.60(12) . . ? N1 Cu1 Cu2 36.95(9) . . ? N4 Cu1 Cu3 65.95(15) . . ? N3 Cu1 Cu3 91.20(12) . . ? N2 Cu1 Cu3 135.88(12) . . ? N1 Cu1 Cu3 88.60(9) . . ? Cu2 Cu1 Cu3 65.301(9) . . ? N8 Cu2 N6 114.1(2) . . ? N8 Cu2 N7 107.2(2) . . ? N6 Cu2 N7 133.1(2) . . ? N8 Cu2 N5 153.24(19) . . ? N6 Cu2 N5 76.04(15) . . ? N7 Cu2 N5 77.14(18) . . ? N8 Cu2 Cu1 76.20(17) . . ? N6 Cu2 Cu1 72.31(12) . . ? N7 Cu2 Cu1 141.15(14) . . ? N5 Cu2 Cu1 84.25(9) . . ? N8 Cu2 Cu3 134.06(17) . . ? N6 Cu2 Cu3 51.40(11) . . ? N7 Cu2 Cu3 110.55(15) . . ? N5 Cu2 Cu3 33.41(9) . . ? Cu1 Cu2 Cu3 57.993(9) . . ? N12 Cu3 N10 116.2(2) . . ? N12 Cu3 N11 110.4(2) . . ? N10 Cu3 N11 126.23(19) . . ? N12 Cu3 N9 145.83(18) . . ? N10 Cu3 N9 77.93(16) . . ? N11 Cu3 N9 78.54(15) . . ? N12 Cu3 Cu1 111.41(16) . . ? N10 Cu3 Cu1 58.49(13) . . ? N11 Cu3 Cu1 125.01(12) . . ? N9 Cu3 Cu1 47.12(9) . . ? N12 Cu3 Cu2 60.35(16) . . ? N10 Cu3 Cu2 102.57(14) . . ? N11 Cu3 Cu2 123.51(12) . . ? N9 Cu3 Cu2 86.86(9) . . ? Cu1 Cu3 Cu2 56.706(9) . . ? F15 P1 F13 92.8(4) . . ? F15 P1 F14 92.1(4) . . ? F13 P1 F14 91.2(3) . . ? F15 P1 F11 88.5(3) . . ? F13 P1 F11 88.3(3) . . ? F14 P1 F11 179.3(4) . . ? F15 P1 F16 174.9(4) . . ? F13 P1 F16 90.8(4) . . ? F14 P1 F16 91.4(4) . . ? F11 P1 F16 88.1(3) . . ? F15 P1 F12 88.4(3) . . ? F13 P1 F12 178.8(4) . . ? F14 P1 F12 88.8(3) . . ? F11 P1 F12 91.7(3) . . ? F16 P1 F12 88.0(3) . . ? F25 P2 F26 169.9(5) . . ? F25 P2 F22 90.5(6) . . ? F26 P2 F22 95.8(5) . . ? F25 P2 F21 92.7(6) . . ? F26 P2 F21 95.2(5) . . ? F22 P2 F21 89.5(4) . . ? F25 P2 F23 88.6(5) . . ? F26 P2 F23 85.3(5) . . ? F22 P2 F23 178.5(4) . . ? F21 P2 F23 89.4(4) . . ? F25 P2 F24 86.8(5) . . ? F26 P2 F24 85.0(4) . . ? F22 P2 F24 93.2(4) . . ? F21 P2 F24 177.3(4) . . ? F23 P2 F24 87.9(4) . . ? F32B P3 F33 123.8(14) . . ? F32B P3 F32 141.9(14) . . ? F33 P3 F32 92.8(9) . . ? F32B P3 F31 34.4(12) . . ? F33 P3 F31 89.8(9) . . ? F32 P3 F31 173.5(10) . . ? F32B P3 F34B 93.9(15) . . ? F33 P3 F34B 30.2(9) . . ? F32 P3 F34B 123.0(11) . . ? F31 P3 F34B 59.6(10) . . ? F32B P3 F35 89.7(7) . . ? F33 P3 F35 87.4(7) . . ? F32 P3 F35 81.2(6) . . ? F31 P3 F35 93.0(8) . . ? F34B P3 F35 91.1(7) . . ? F32B P3 F31B 92.5(14) . . ? F33 P3 F31B 143.6(13) . . ? F32 P3 F31B 52.1(10) . . ? F31 P3 F31B 126.2(13) . . ? F34B P3 F31B 171.1(12) . . ? F35 P3 F31B 95.2(5) . . ? F32B P3 F36 90.8(7) . . ? F33 P3 F36 94.1(7) . . ? F32 P3 F36 97.1(6) . . ? F31 P3 F36 88.6(8) . . ? F34B P3 F36 91.1(7) . . ? F35 P3 F36 177.8(3) . . ? F31B P3 F36 82.6(5) . . ? F32B P3 F34 53.0(12) . . ? F33 P3 F34 172.9(8) . . ? F32 P3 F34 89.4(8) . . ? F31 P3 F34 87.4(7) . . ? F34B P3 F34 146.7(11) . . ? F35 P3 F34 86.2(4) . . ? F31B P3 F34 40.6(10) . . ? F36 P3 F34 92.4(4) . . ? F32B P3 F33B 174.2(9) . . ? F33 P3 F33B 56.6(10) . . ? F32 P3 F33B 40.0(8) . . ? F31 P3 F33B 144.5(12) . . ? F34B P3 F33B 85.9(11) . . ? F35 P3 F33B 96.1(7) . . ? F31B P3 F33B 87.0(12) . . ? F36 P3 F33B 83.5(6) . . ? F34 P3 F33B 127.4(11) . . ? C20 N1 C14 110.2(4) . . ? C20 N1 C13 112.9(4) . . ? C14 N1 C13 108.2(4) . . ? C20 N1 Cu1 105.0(3) . . ? C14 N1 Cu1 93.6(3) . . ? C13 N1 Cu1 125.0(3) . . ? C15 N2 C19 118.5(5) . . ? C15 N2 Cu1 114.9(3) . . ? C19 N2 Cu1 126.5(4) . . ? C21 N3 C25 118.3(4) . . ? C21 N3 Cu1 120.3(3) . . ? C25 N3 Cu1 121.3(3) . . ? C26 N4 Cu1 158.7(5) . . ? C29 N5 C35 110.7(4) . . ? C29 N5 C28 113.2(4) . . ? C35 N5 C28 108.6(4) . . ? C29 N5 Cu2 104.3(3) . . ? C35 N5 Cu2 91.9(3) . . ? C28 N5 Cu2 126.0(3) . . ? C30 N6 C34 117.8(4) . . ? C30 N6 Cu2 123.2(3) . . ? C34 N6 Cu2 118.3(4) . . ? C36 N7 C40 118.4(6) . . ? C36 N7 Cu2 116.8(4) . . ? C40 N7 Cu2 123.7(5) . . ? C41 N8 Cu2 163.0(6) . . ? C44 N9 C50 110.6(4) . . ? C44 N9 C43 111.1(4) . . ? C50 N9 C43 107.5(4) . . ? C44 N9 Cu3 103.2(3) . . ? C50 N9 Cu3 93.2(3) . . ? C43 N9 Cu3 129.4(3) . . ? C49 N10 C45 118.2(5) . . ? C49 N10 Cu3 120.8(4) . . ? C45 N10 Cu3 120.9(4) . . ? C51 N11 C55 117.9(5) . . ? C51 N11 Cu3 115.9(4) . . ? C55 N11 Cu3 125.3(4) . . ? C56 N12 Cu3 159.3(5) . . ? C2 C1 C6 120.5(4) . . ? C2 C1 C13 119.8(4) . . ? C6 C1 C13 119.6(4) . . ? C3 C2 C1 119.6(4) . . ? C3 C2 C7 119.2(4) . . ? C1 C2 C7 121.1(4) . . ? C2 C3 C4 120.4(4) . . ? C2 C3 C28 119.5(4) . . ? C4 C3 C28 120.1(4) . . ? C3 C4 C5 120.0(4) . . ? C3 C4 C11 120.8(4) . . ? C5 C4 C11 119.0(4) . . ? C6 C5 C4 119.6(4) . . ? C6 C5 C43 121.0(4) . . ? C4 C5 C43 119.0(4) . . ? C5 C6 C1 119.7(4) . . ? C5 C6 C9 121.4(4) . . ? C1 C6 C9 118.8(4) . . ? C2 C7 C8 111.1(4) . . ? C6 C9 C10 112.5(4) . . ? C4 C11 C12 113.3(4) . . ? N1 C13 C1 114.0(4) . . ? N1 C14 C15 111.9(4) . . ? N2 C15 C16 122.0(5) . . ? N2 C15 C14 115.1(4) . . ? C16 C15 C14 122.8(5) . . ? C15 C16 C17 118.3(6) . . ? C18 C17 C16 119.8(6) . . ? C17 C18 C19 118.9(6) . . ? N2 C19 C18 122.5(6) . . ? N1 C20 C21 113.5(4) . . ? N3 C21 C22 121.2(5) . . ? N3 C21 C20 118.7(4) . . ? C22 C21 C20 120.0(4) . . ? C23 C22 C21 119.7(5) . . ? C22 C23 C24 118.8(5) . . ? C25 C24 C23 118.7(5) . . ? N3 C25 C24 123.4(5) . . ? N4 C26 C27 178.9(8) . . ? N5 C28 C3 113.7(4) . . ? N5 C29 C30 114.1(4) . . ? N6 C30 C31 122.2(5) . . ? N6 C30 C29 118.7(4) . . ? C31 C30 C29 118.9(5) . . ? C30 C31 C32 119.1(5) . . ? C33 C32 C31 118.7(5) . . ? C34 C33 C32 118.7(5) . . ? N6 C34 C33 123.3(5) . . ? N5 C35 C36 111.0(5) . . ? N7 C36 C37 121.6(7) . . ? N7 C36 C35 115.6(5) . . ? C37 C36 C35 122.8(7) . . ? C38 C37 C36 119.3(9) . . ? C37 C38 C39 119.0(8) . . ? C40 C39 C38 120.2(9) . . ? N7 C40 C39 121.6(9) . . ? N8 C41 C42 179.2(8) . . ? N9 C43 C5 116.2(4) . . ? N9 C44 C45 113.8(4) . . ? N10 C45 C46 121.4(5) . . ? N10 C45 C44 118.0(5) . . ? C46 C45 C44 120.5(5) . . ? C45 C46 C47 119.3(6) . . ? C48 C47 C46 119.1(6) . . ? C49 C48 C47 118.5(6) . . ? N10 C49 C48 123.3(7) . . ? N9 C50 C51 111.1(4) . . ? N11 C51 C52 122.5(5) . . ? N11 C51 C50 114.7(5) . . ? C52 C51 C50 122.8(5) . . ? C51 C52 C53 118.8(6) . . ? C54 C53 C52 119.3(6) . . ? C55 C54 C53 118.6(6) . . ? N11 C55 C54 122.9(6) . . ? N12 C56 C57 179.2(7) . . ? Cl12 C61 Cl11 117.2(7) . . ? Cl21 C62 Cl22 112.9(4) . . ? Cl32 C63 Cl31 112.0(4) . . ? Cl41 C64 Cl42 113.3(5) . . ? Cl51 C65 Cl52 99.9(11) . . ? Cl61 C66 Cl62 114.0(7) . . ? Cl72 C67 Cl71 114.1(6) . . ? _diffrn_measured_fraction_theta_max 0.936 _diffrn_reflns_theta_full 24.21 _diffrn_measured_fraction_theta_full 0.936 _refine_diff_density_max 1.296 _refine_diff_density_min -1.167 _refine_diff_density_rms 0.094 #=END data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[LCu3Cl(ClO4)2]ClO4-2CH2Cl2' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H61 Cl8 Cu3 N9 O12' _chemical_formula_weight 1490.33 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' 'O' 'O' 0.0106 0.0060 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.7370(3) _cell_length_b 14.5407(3) _cell_length_c 16.7511(3) _cell_angle_alpha 65.8710(10) _cell_angle_beta 83.2570(10) _cell_angle_gamma 88.6970(10) _cell_volume 3031.31(11) _cell_formula_units_Z 2 _cell_measurement_temperature 188(2) _cell_measurement_reflns_used 12319 _cell_measurement_theta_min 1.89 _cell_measurement_theta_max 24.18 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.633 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1522 _exptl_absorpt_coefficient_mu 1.463 _exptl_absorpt_correction_type 'Semi-empirical from psi-scans (SADABS)' _exptl_absorpt_correction_T_min 0.810776 _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 188(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12319 _diffrn_reflns_av_R_equivalents 0.0220 _diffrn_reflns_av_sigmaI/netI 0.0392 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 24.18 _reflns_number_total 9110 _reflns_number_gt 7516 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0377P)^2^+11.9372P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9110 _refine_ls_number_parameters 794 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0698 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.1335 _refine_ls_wR_factor_gt 0.1200 _refine_ls_goodness_of_fit_ref 1.135 _refine_ls_restrained_S_all 1.138 _refine_ls_shift/su_max 0.105 _refine_ls_shift/su_mean 0.003 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 0.16035(4) 0.21655(4) 0.29423(4) 0.02461(16) Uani 1 1 d . . . Cu2 Cu 0.06910(5) 0.06028(5) 0.17831(4) 0.03191(17) Uani 1 1 d . . . Cu3 Cu -0.30416(6) 0.39092(5) 0.47099(5) 0.0418(2) Uani 1 1 d . . . Cl1 Cl -0.15654(11) 0.44667(11) 0.57214(10) 0.0423(4) Uani 1 1 d . . . Cl2 Cl 0.33468(9) 0.16931(11) 0.44989(9) 0.0356(3) Uani 1 1 d . . . Cl3 Cl 0.55993(12) 0.72415(12) 0.07494(12) 0.0531(4) Uani 1 1 d . . . O1 O -0.1466(5) 0.3897(4) 0.5209(4) 0.0801(17) Uani 1 1 d . . . O2 O -0.0865(4) 0.4273(5) 0.6309(4) 0.0776(16) Uani 1 1 d . . . O3 O -0.1493(4) 0.5516(4) 0.5133(4) 0.0763(16) Uani 1 1 d . . . O4 O -0.2535(3) 0.4275(4) 0.6192(3) 0.0631(13) Uani 1 1 d . . . O5 O 0.4067(3) 0.1764(4) 0.3788(3) 0.0533(12) Uani 1 1 d . . . O6 O 0.3505(3) 0.0850(3) 0.5281(3) 0.0534(12) Uani 1 1 d . . . O7 O 0.3389(3) 0.2600(3) 0.4638(3) 0.0569(12) Uani 1 1 d . . . O8 O 0.2383(3) 0.1586(3) 0.4273(3) 0.0378(9) Uani 1 1 d . . . O9 O 0.5395(4) 0.7821(4) 0.1262(4) 0.0769(16) Uani 1 1 d . . . O10 O 0.5951(4) 0.7912(4) -0.0128(3) 0.0720(15) Uani 1 1 d . . . O11 O 0.6291(5) 0.6522(5) 0.1095(5) 0.104(2) Uani 1 1 d . . . O12 O 0.4718(4) 0.6755(4) 0.0756(4) 0.0806(17) Uani 1 1 d . . . Cl8 Cl 0.18777(9) 0.08550(9) 0.25415(9) 0.0305(3) Uani 1 1 d . . . N1 N 0.1196(3) 0.3467(3) 0.3074(3) 0.0235(9) Uani 1 1 d . . . N2 N -0.0825(3) 0.1330(3) 0.1314(3) 0.0264(9) Uani 1 1 d . . . N3 N -0.3483(3) 0.3675(3) 0.3458(3) 0.0274(10) Uani 1 1 d . . . N4 N 0.0353(3) 0.1632(3) 0.3702(3) 0.0261(9) Uani 1 1 d . . . N5 N 0.2789(3) 0.2995(3) 0.2249(3) 0.0266(9) Uani 1 1 d . . . N6 N -0.0280(3) -0.0491(3) 0.2574(3) 0.0314(10) Uani 1 1 d . . . N7 N 0.0988(3) 0.1031(3) 0.0494(3) 0.0304(10) Uani 1 1 d . . . N8 N -0.3248(3) 0.2462(3) 0.5215(3) 0.0329(10) Uani 1 1 d . . . N9 N -0.3791(3) 0.5109(3) 0.4236(3) 0.0336(11) Uani 1 1 d . . . C1 C -0.0300(4) 0.3842(3) 0.2187(3) 0.0235(11) Uani 1 1 d . . . C2 C -0.0249(3) 0.3324(3) 0.1636(3) 0.0218(10) Uani 1 1 d . . . C3 C -0.1120(4) 0.2995(4) 0.1461(3) 0.0245(11) Uani 1 1 d . . . C4 C -0.2037(4) 0.3258(4) 0.1768(3) 0.0265(11) Uani 1 1 d . . . C5 C -0.2080(4) 0.3832(4) 0.2272(3) 0.0254(11) Uani 1 1 d . . . C6 C -0.1211(4) 0.4103(4) 0.2503(3) 0.0247(11) Uani 1 1 d . . . C7 C 0.0980(4) 0.4044(4) 0.0247(4) 0.0411(14) Uani 1 1 d . . . H7A H 0.1598 0.3912 -0.0013 0.049 Uiso 1 1 calc R . . H7B H 0.1028 0.4674 0.0301 0.049 Uiso 1 1 calc R . . H7C H 0.0481 0.4080 -0.0119 0.049 Uiso 1 1 calc R . . C8 C 0.0716(4) 0.3195(4) 0.1161(3) 0.0260(11) Uani 1 1 d . . . H8A H 0.0688 0.2567 0.1101 0.031 Uiso 1 1 calc R . . H8B H 0.1229 0.3155 0.1517 0.031 Uiso 1 1 calc R . . C9 C -0.3146(4) 0.3832(5) 0.0587(4) 0.0443(15) Uani 1 1 d . . . H9A H -0.3735 0.3665 0.0413 0.053 Uiso 1 1 calc R . . H9B H -0.2603 0.3878 0.0155 0.053 Uiso 1 1 calc R . . H9C H -0.3216 0.4467 0.0634 0.053 Uiso 1 1 calc R . . C10 C -0.2962(4) 0.3022(4) 0.1470(4) 0.0328(12) Uani 1 1 d . . . H10A H -0.2902 0.2385 0.1425 0.039 Uiso 1 1 calc R . . H10B H -0.3510 0.2969 0.1900 0.039 Uiso 1 1 calc R . . C11 C -0.1211(5) 0.5875(4) 0.2432(5) 0.0519(17) Uani 1 1 d . . . H11A H -0.1258 0.6248 0.2794 0.062 Uiso 1 1 calc R . . H11B H -0.1737 0.6053 0.2070 0.062 Uiso 1 1 calc R . . H11C H -0.0594 0.6034 0.2064 0.062 Uiso 1 1 calc R . . C12 C -0.1282(4) 0.4757(4) 0.3014(4) 0.0330(13) Uani 1 1 d . . . H12A H -0.0766 0.4589 0.3386 0.040 Uiso 1 1 calc R . . H12B H -0.1895 0.4607 0.3388 0.040 Uiso 1 1 calc R . . C13 C 0.0643(4) 0.4212(4) 0.2362(3) 0.0252(11) Uani 1 1 d . . . H13A H 0.1078 0.4460 0.1822 0.030 Uiso 1 1 calc R . . H13B H 0.0491 0.4774 0.2511 0.030 Uiso 1 1 calc R . . C14 C 0.0630(4) 0.3105(4) 0.3963(3) 0.0261(11) Uani 1 1 d . . . H14A H 0.0229 0.3635 0.4009 0.031 Uiso 1 1 calc R . . H14B H 0.1074 0.2925 0.4402 0.031 Uiso 1 1 calc R . . C15 C -0.0005(4) 0.2212(4) 0.4124(3) 0.0260(11) Uani 1 1 d . . . C16 C -0.0852(4) 0.1942(4) 0.4705(3) 0.0315(12) Uani 1 1 d . . . H16 H -0.1090 0.2357 0.5004 0.038 Uiso 1 1 calc R . . C17 C -0.1358(4) 0.1061(4) 0.4850(4) 0.0342(13) Uani 1 1 d . . . H17 H -0.1944 0.0853 0.5259 0.041 Uiso 1 1 calc R . . C18 C -0.1008(4) 0.0489(4) 0.4399(4) 0.0329(12) Uani 1 1 d . . . H18 H -0.1354 -0.0114 0.4479 0.039 Uiso 1 1 calc R . . C19 C -0.0156(4) 0.0796(4) 0.3836(4) 0.0325(12) Uani 1 1 d . . . H19 H 0.0087 0.0395 0.3524 0.039 Uiso 1 1 calc R . . C20 C 0.2137(3) 0.3985(4) 0.3033(3) 0.0273(11) Uani 1 1 d . . . H20A H 0.2380 0.3697 0.3597 0.033 Uiso 1 1 calc R . . H20B H 0.2032 0.4688 0.2886 0.033 Uiso 1 1 calc R . . C21 C 0.2870(4) 0.3863(4) 0.2348(4) 0.0288(12) Uani 1 1 d . . . C22 C 0.3617(4) 0.4563(4) 0.1875(4) 0.0364(13) Uani 1 1 d . . . H22 H 0.3661 0.5184 0.1944 0.044 Uiso 1 1 calc R . . C23 C 0.4298(4) 0.4353(5) 0.1304(4) 0.0411(14) Uani 1 1 d . . . H23 H 0.4830 0.4822 0.0978 0.049 Uiso 1 1 calc R . . C24 C 0.4209(4) 0.3471(5) 0.1205(4) 0.0430(15) Uani 1 1 d . . . H24 H 0.4676 0.3318 0.0806 0.052 Uiso 1 1 calc R . . C25 C 0.3443(4) 0.2803(4) 0.1682(4) 0.0360(13) Uani 1 1 d . . . H25 H 0.3378 0.2188 0.1606 0.043 Uiso 1 1 calc R . . C26 C -0.1058(4) 0.2422(4) 0.0880(3) 0.0269(11) Uani 1 1 d . . . H26A H -0.1673 0.2473 0.0648 0.032 Uiso 1 1 calc R . . H26B H -0.0565 0.2747 0.0390 0.032 Uiso 1 1 calc R . . C27 C -0.1546(4) 0.0765(4) 0.2060(4) 0.0321(12) Uani 1 1 d . . . H27A H -0.2155 0.0724 0.1845 0.038 Uiso 1 1 calc R . . H27B H -0.1659 0.1125 0.2431 0.038 Uiso 1 1 calc R . . C28 C -0.1233(4) -0.0290(4) 0.2604(4) 0.0318(12) Uani 1 1 d . . . C29 C -0.1938(4) -0.1017(4) 0.3145(4) 0.0371(13) Uani 1 1 d . . . H29 H -0.2621 -0.0859 0.3159 0.045 Uiso 1 1 calc R . . C30 C -0.1643(5) -0.1970(5) 0.3660(4) 0.0437(15) Uani 1 1 d . . . H30 H -0.2118 -0.2481 0.4041 0.052 Uiso 1 1 calc R . . C31 C -0.0664(5) -0.2182(4) 0.3622(4) 0.0427(15) Uani 1 1 d . . . H31 H -0.0444 -0.2842 0.3969 0.051 Uiso 1 1 calc R . . C32 C -0.0003(4) -0.1427(4) 0.3075(4) 0.0364(13) Uani 1 1 d . . . H32 H 0.0682 -0.1573 0.3049 0.044 Uiso 1 1 calc R . . C33 C -0.0765(4) 0.0926(4) 0.0635(3) 0.0285(12) Uani 1 1 d . . . H33A H -0.1288 0.1188 0.0278 0.034 Uiso 1 1 calc R . . H33B H -0.0848 0.0206 0.0916 0.034 Uiso 1 1 calc R . . C34 C 0.0199(4) 0.1199(4) 0.0058(3) 0.0281(12) Uani 1 1 d . . . C35 C 0.0276(4) 0.1554(4) -0.0841(4) 0.0363(13) Uani 1 1 d . . . H35 H -0.0300 0.1674 -0.1139 0.044 Uiso 1 1 calc R . . C36 C 0.1198(5) 0.1737(4) -0.1310(4) 0.0407(15) Uani 1 1 d . . . H36 H 0.1270 0.1983 -0.1941 0.049 Uiso 1 1 calc R . . C37 C 0.2008(5) 0.1568(4) -0.0874(4) 0.0427(15) Uani 1 1 d . . . H37 H 0.2655 0.1688 -0.1190 0.051 Uiso 1 1 calc R . . C38 C 0.1876(4) 0.1222(4) 0.0026(4) 0.0375(13) Uani 1 1 d . . . H38 H 0.2444 0.1113 0.0334 0.045 Uiso 1 1 calc R . . C39 C -0.3056(4) 0.4209(4) 0.2531(4) 0.0306(12) Uani 1 1 d . . . H39A H -0.2971 0.4909 0.2410 0.037 Uiso 1 1 calc R . . H39B H -0.3519 0.4164 0.2161 0.037 Uiso 1 1 calc R . . C40 C -0.4456(4) 0.4095(4) 0.3577(4) 0.0336(13) Uani 1 1 d . . . H40A H -0.4830 0.3620 0.4098 0.040 Uiso 1 1 calc R . . H40B H -0.4801 0.4190 0.3084 0.040 Uiso 1 1 calc R . . C41 C -0.4379(4) 0.5085(4) 0.3656(4) 0.0335(13) Uani 1 1 d . . . C42 C -0.4905(4) 0.5903(5) 0.3193(4) 0.0442(15) Uani 1 1 d . . . H42 H -0.5312 0.5873 0.2775 0.053 Uiso 1 1 calc R . . C43 C -0.4843(5) 0.6775(5) 0.3333(4) 0.0509(17) Uani 1 1 d . . . H43 H -0.5197 0.7360 0.3006 0.061 Uiso 1 1 calc R . . C44 C -0.4278(5) 0.6792(5) 0.3938(4) 0.0456(15) Uani 1 1 d . . . H44 H -0.4242 0.7381 0.4058 0.055 Uiso 1 1 calc R . . C45 C -0.3753(4) 0.5953(4) 0.4377(4) 0.0393(14) Uani 1 1 d . . . H45 H -0.3347 0.5973 0.4798 0.047 Uiso 1 1 calc R . . C46 C -0.3562(4) 0.2589(4) 0.3760(4) 0.0349(13) Uani 1 1 d . . . H46A H -0.2996 0.2363 0.3504 0.042 Uiso 1 1 calc R . . H46B H -0.4128 0.2423 0.3554 0.042 Uiso 1 1 calc R . . C47 C -0.3645(4) 0.2029(4) 0.4749(4) 0.0331(13) Uani 1 1 d . . . C48 C -0.4062(4) 0.1078(4) 0.5154(4) 0.0395(14) Uani 1 1 d . . . H48 H -0.4358 0.0790 0.4814 0.047 Uiso 1 1 calc R . . C49 C -0.4059(5) 0.0539(5) 0.6038(5) 0.0521(17) Uani 1 1 d . . . H49 H -0.4358 -0.0125 0.6325 0.063 Uiso 1 1 calc R . . C50 C -0.3620(5) 0.0961(5) 0.6513(4) 0.0469(16) Uani 1 1 d . . . H50 H -0.3585 0.0589 0.7132 0.056 Uiso 1 1 calc R . . C51 C -0.3236(4) 0.1919(4) 0.6085(4) 0.0387(14) Uani 1 1 d . . . H51 H -0.2945 0.2219 0.6419 0.046 Uiso 1 1 calc R . . C52 C 0.4655(12) -0.021(2) -0.1136(13) 0.088(10) Uani 0.576(19) 1 d PD A 1 H52A H 0.5238 -0.0469 -0.0866 0.106 Uiso 0.576(19) 1 calc PR A 1 H52B H 0.4739 0.0511 -0.1435 0.106 Uiso 0.576(19) 1 calc PR A 1 Cl4 Cl 0.4510(5) -0.0698(8) -0.1898(5) 0.105(3) Uani 0.576(19) 1 d PD A 1 Cl5 Cl 0.3671(6) -0.0496(5) -0.0333(5) 0.091(2) Uani 0.576(19) 1 d PD A 1 C52' C 0.450(2) -0.019(2) -0.1037(11) 0.097(16) Uani 0.424(19) 1 d PD A 2 H52C H 0.5058 -0.0622 -0.0941 0.117 Uiso 0.424(19) 1 calc PR A 2 H52D H 0.4663 0.0387 -0.0934 0.117 Uiso 0.424(19) 1 calc PR A 2 Cl4' Cl 0.4226(8) 0.018(2) -0.2106(6) 0.168(10) Uani 0.424(19) 1 d PD A 2 Cl5' Cl 0.3490(14) -0.083(2) -0.0335(10) 0.212(10) Uani 0.424(19) 1 d PD A 2 C53 C 0.2781(5) -0.2549(5) 0.1756(5) 0.063(2) Uani 1 1 d D . . H53A H 0.3414 -0.2444 0.1415 0.076 Uiso 1 1 calc R . . H53B H 0.2858 -0.2992 0.2353 0.076 Uiso 1 1 calc R . . Cl6 Cl 0.23613(16) -0.13949(15) 0.17266(14) 0.0732(6) Uani 1 1 d D . . Cl7 Cl 0.19873(17) -0.31234(15) 0.13460(14) 0.0740(6) Uani 1 1 d 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 0.0214(3) 0.0237(3) 0.0308(4) -0.0137(3) -0.0013(3) -0.0016(2) Cu2 0.0314(4) 0.0315(4) 0.0331(4) -0.0133(3) -0.0037(3) -0.0026(3) Cu3 0.0474(4) 0.0332(4) 0.0489(5) -0.0183(3) -0.0155(4) 0.0008(3) Cl1 0.0469(9) 0.0427(8) 0.0462(9) -0.0256(7) -0.0106(7) -0.0020(7) Cl2 0.0266(7) 0.0441(8) 0.0419(8) -0.0228(7) -0.0069(6) 0.0024(6) Cl3 0.0507(9) 0.0478(9) 0.0611(11) -0.0234(8) -0.0024(8) -0.0064(8) O1 0.111(5) 0.073(4) 0.079(4) -0.057(3) 0.006(3) -0.014(3) O2 0.063(3) 0.108(5) 0.084(4) -0.054(4) -0.039(3) 0.024(3) O3 0.094(4) 0.040(3) 0.081(4) -0.011(3) -0.004(3) -0.012(3) O4 0.045(3) 0.069(3) 0.076(3) -0.031(3) 0.004(2) -0.012(2) O5 0.033(2) 0.071(3) 0.057(3) -0.029(2) 0.006(2) 0.003(2) O6 0.050(3) 0.059(3) 0.049(3) -0.017(2) -0.018(2) 0.019(2) O7 0.060(3) 0.057(3) 0.072(3) -0.043(3) -0.012(2) -0.005(2) O8 0.027(2) 0.043(2) 0.042(2) -0.0155(19) -0.0064(17) -0.0080(17) O9 0.106(4) 0.068(3) 0.069(4) -0.043(3) 0.001(3) -0.008(3) O10 0.078(4) 0.068(3) 0.060(3) -0.022(3) 0.018(3) -0.024(3) O11 0.100(5) 0.074(4) 0.121(5) -0.022(4) -0.026(4) 0.047(4) O12 0.060(3) 0.081(4) 0.108(5) -0.052(4) 0.018(3) -0.036(3) Cl8 0.0261(6) 0.0283(7) 0.0423(8) -0.0190(6) -0.0067(6) 0.0035(5) N1 0.021(2) 0.028(2) 0.025(2) -0.0150(19) 0.0002(17) -0.0031(17) N2 0.028(2) 0.021(2) 0.035(2) -0.0158(19) -0.0040(19) -0.0007(18) N3 0.021(2) 0.031(2) 0.035(3) -0.018(2) -0.0014(18) 0.0003(18) N4 0.025(2) 0.028(2) 0.026(2) -0.0113(19) -0.0076(18) 0.0014(18) N5 0.021(2) 0.029(2) 0.031(2) -0.014(2) 0.0000(18) -0.0004(18) N6 0.037(3) 0.025(2) 0.033(3) -0.012(2) -0.005(2) -0.003(2) N7 0.031(2) 0.027(2) 0.036(3) -0.016(2) -0.003(2) -0.0010(19) N8 0.029(2) 0.034(3) 0.037(3) -0.016(2) -0.004(2) 0.004(2) N9 0.027(2) 0.037(3) 0.042(3) -0.022(2) -0.006(2) 0.001(2) C1 0.026(3) 0.017(2) 0.028(3) -0.010(2) -0.004(2) 0.001(2) C2 0.025(3) 0.019(2) 0.022(3) -0.008(2) -0.004(2) 0.002(2) C3 0.027(3) 0.022(3) 0.027(3) -0.011(2) -0.007(2) 0.004(2) C4 0.027(3) 0.024(3) 0.027(3) -0.010(2) -0.002(2) 0.001(2) C5 0.025(3) 0.024(3) 0.027(3) -0.010(2) -0.004(2) 0.005(2) C6 0.030(3) 0.018(2) 0.026(3) -0.009(2) -0.002(2) -0.002(2) C7 0.039(3) 0.038(3) 0.039(3) -0.011(3) 0.004(3) -0.002(3) C8 0.025(3) 0.024(3) 0.033(3) -0.016(2) -0.004(2) 0.002(2) C9 0.030(3) 0.062(4) 0.047(4) -0.027(3) -0.009(3) 0.006(3) C10 0.024(3) 0.040(3) 0.042(3) -0.024(3) -0.006(2) -0.002(2) C11 0.055(4) 0.035(3) 0.077(5) -0.033(3) -0.011(4) 0.008(3) C12 0.027(3) 0.033(3) 0.050(4) -0.028(3) -0.008(3) 0.003(2) C13 0.026(3) 0.021(3) 0.029(3) -0.010(2) -0.005(2) 0.000(2) C14 0.024(3) 0.030(3) 0.033(3) -0.020(2) -0.006(2) 0.001(2) C15 0.026(3) 0.026(3) 0.028(3) -0.011(2) -0.011(2) 0.003(2) C16 0.027(3) 0.037(3) 0.029(3) -0.014(2) 0.003(2) 0.003(2) C17 0.021(3) 0.036(3) 0.038(3) -0.008(3) -0.001(2) -0.003(2) C18 0.029(3) 0.033(3) 0.034(3) -0.010(3) -0.007(2) -0.005(2) C19 0.035(3) 0.031(3) 0.035(3) -0.016(3) -0.009(2) -0.002(2) C20 0.022(3) 0.028(3) 0.037(3) -0.017(2) -0.004(2) -0.005(2) C21 0.021(3) 0.029(3) 0.039(3) -0.016(2) -0.007(2) 0.001(2) C22 0.025(3) 0.030(3) 0.053(4) -0.015(3) -0.008(3) -0.004(2) C23 0.026(3) 0.053(4) 0.042(4) -0.019(3) 0.002(3) -0.009(3) C24 0.029(3) 0.054(4) 0.046(4) -0.023(3) 0.008(3) -0.007(3) C25 0.031(3) 0.038(3) 0.043(3) -0.022(3) 0.003(3) -0.003(2) C26 0.027(3) 0.024(3) 0.034(3) -0.014(2) -0.010(2) 0.000(2) C27 0.028(3) 0.029(3) 0.040(3) -0.016(3) 0.001(2) -0.003(2) C28 0.036(3) 0.030(3) 0.034(3) -0.018(2) -0.001(2) -0.006(2) C29 0.037(3) 0.037(3) 0.036(3) -0.014(3) 0.001(3) -0.009(3) C30 0.054(4) 0.043(4) 0.026(3) -0.010(3) 0.013(3) -0.018(3) C31 0.059(4) 0.033(3) 0.034(3) -0.012(3) -0.005(3) -0.007(3) C32 0.044(3) 0.030(3) 0.034(3) -0.012(3) -0.005(3) 0.000(3) C33 0.031(3) 0.021(3) 0.037(3) -0.015(2) -0.008(2) 0.000(2) C34 0.036(3) 0.019(3) 0.036(3) -0.018(2) -0.004(2) -0.001(2) C35 0.048(4) 0.031(3) 0.037(3) -0.021(3) -0.009(3) 0.002(3) C36 0.061(4) 0.029(3) 0.032(3) -0.015(3) 0.006(3) -0.007(3) C37 0.042(4) 0.038(3) 0.048(4) -0.020(3) 0.011(3) -0.006(3) C38 0.032(3) 0.035(3) 0.047(4) -0.018(3) -0.001(3) -0.006(2) C39 0.027(3) 0.031(3) 0.037(3) -0.016(2) -0.008(2) 0.006(2) C40 0.021(3) 0.045(3) 0.044(3) -0.027(3) -0.005(2) 0.000(2) C41 0.020(3) 0.047(3) 0.039(3) -0.024(3) 0.001(2) 0.001(2) C42 0.034(3) 0.059(4) 0.052(4) -0.032(3) -0.018(3) 0.021(3) C43 0.057(4) 0.053(4) 0.053(4) -0.030(3) -0.016(3) 0.025(3) C44 0.049(4) 0.040(3) 0.057(4) -0.029(3) -0.007(3) 0.007(3) C45 0.039(3) 0.042(3) 0.046(4) -0.026(3) -0.009(3) -0.002(3) C46 0.034(3) 0.034(3) 0.042(3) -0.021(3) -0.002(3) -0.001(2) C47 0.023(3) 0.032(3) 0.048(4) -0.021(3) -0.002(2) 0.001(2) C48 0.035(3) 0.035(3) 0.051(4) -0.020(3) -0.007(3) -0.004(3) C49 0.050(4) 0.036(3) 0.063(5) -0.014(3) 0.002(3) -0.006(3) C50 0.047(4) 0.041(4) 0.046(4) -0.011(3) -0.005(3) 0.014(3) C51 0.039(3) 0.036(3) 0.043(4) -0.017(3) -0.006(3) 0.004(3) C52 0.033(9) 0.12(2) 0.10(2) -0.038(17) 0.010(10) -0.005(10) Cl4 0.095(4) 0.128(7) 0.091(4) -0.050(4) 0.023(3) -0.049(4) Cl5 0.078(4) 0.070(3) 0.091(4) -0.010(3) 0.036(3) 0.019(3) C52' 0.18(4) 0.034(15) 0.07(2) -0.007(14) -0.01(2) 0.001(19) Cl4' 0.097(6) 0.25(2) 0.098(6) -0.014(8) -0.010(4) -0.057(9) Cl5' 0.105(9) 0.25(2) 0.143(11) 0.051(11) 0.000(7) 0.015(12) C53 0.056(4) 0.078(5) 0.057(5) -0.028(4) -0.010(4) 0.020(4) Cl6 0.0838(14) 0.0659(12) 0.0710(13) -0.0319(10) 0.0001(11) 0.0074(10) Cl7 0.0896(15) 0.0654(12) 0.0698(13) -0.0268(10) -0.0258(11) 0.0149(11) _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 N4 1.977(4) . ? Cu1 N5 1.989(4) . ? Cu1 N1 2.051(4) . ? Cu1 Cl8 2.2755(14) . ? Cu1 O8 2.410(4) . ? Cu2 N7 1.981(4) . ? Cu2 N6 2.006(4) . ? Cu2 Cl8 2.3022(14) . ? Cu2 N2 2.382(4) . ? Cu3 N9 1.926(5) . ? Cu3 N8 1.933(5) . ? Cu3 N3 2.403(4) . ? Cu3 O1 2.408(6) . ? Cl1 O2 1.399(5) . ? Cl1 O1 1.411(5) . ? Cl1 O3 1.437(5) . ? Cl1 O4 1.437(5) . ? Cl2 O6 1.417(4) . ? Cl2 O5 1.426(4) . ? Cl2 O7 1.433(4) . ? Cl2 O8 1.448(4) . ? Cl3 O11 1.386(6) . ? Cl3 O12 1.412(5) . ? Cl3 O10 1.424(5) . ? Cl3 O9 1.432(5) . ? N1 C14 1.486(6) . ? N1 C20 1.493(6) . ? N1 C13 1.513(6) . ? N2 C27 1.458(7) . ? N2 C33 1.471(6) . ? N2 C26 1.497(6) . ? N3 C46 1.451(7) . ? N3 C39 1.475(7) . ? N3 C40 1.483(6) . ? N4 C19 1.340(7) . ? N4 C15 1.357(6) . ? N5 C25 1.339(7) . ? N5 C21 1.347(6) . ? N6 C28 1.334(7) . ? N6 C32 1.348(7) . ? N7 C38 1.339(7) . ? N7 C34 1.341(7) . ? N8 C51 1.346(7) . ? N8 C47 1.350(7) . ? N9 C45 1.344(7) . ? N9 C41 1.347(7) . ? C1 C2 1.405(7) . ? C1 C6 1.406(7) . ? C1 C13 1.518(7) . ? C2 C3 1.403(7) . ? C2 C8 1.513(7) . ? C3 C4 1.408(7) . ? C3 C26 1.513(7) . ? C4 C5 1.406(7) . ? C4 C10 1.513(7) . ? C5 C6 1.409(7) . ? C5 C39 1.520(7) . ? C6 C12 1.512(7) . ? C7 C8 1.532(7) . ? C9 C10 1.512(8) . ? C11 C12 1.514(8) . ? C14 C15 1.493(7) . ? C15 C16 1.378(7) . ? C16 C17 1.389(8) . ? C17 C18 1.380(8) . ? C18 C19 1.371(8) . ? C20 C21 1.501(7) . ? C21 C22 1.383(7) . ? C22 C23 1.378(8) . ? C23 C24 1.370(8) . ? C24 C25 1.380(8) . ? C27 C28 1.513(7) . ? C28 C29 1.391(7) . ? C29 C30 1.382(8) . ? C30 C31 1.373(9) . ? C31 C32 1.376(8) . ? C33 C34 1.502(7) . ? C34 C35 1.368(8) . ? C35 C36 1.380(8) . ? C36 C37 1.364(9) . ? C37 C38 1.371(8) . ? C40 C41 1.505(8) . ? C41 C42 1.370(8) . ? C42 C43 1.387(9) . ? C43 C44 1.354(9) . ? C44 C45 1.378(8) . ? C46 C47 1.508(8) . ? C47 C48 1.371(8) . ? C48 C49 1.364(9) . ? C49 C50 1.381(9) . ? C50 C51 1.364(8) . ? C52 Cl5 1.718(13) . ? C52 Cl4 1.728(14) . ? C52' Cl5' 1.722(15) . ? C52' Cl4' 1.734(15) . ? C53 Cl7 1.745(7) . ? C53 Cl6 1.745(7) . ? 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 N4 Cu1 N5 165.80(17) . . ? N4 Cu1 N1 82.96(16) . . ? N5 Cu1 N1 83.00(16) . . ? N4 Cu1 Cl8 96.91(12) . . ? N5 Cu1 Cl8 97.26(12) . . ? N1 Cu1 Cl8 167.78(12) . . ? N4 Cu1 O8 87.24(15) . . ? N5 Cu1 O8 91.03(15) . . ? N1 Cu1 O8 91.37(15) . . ? Cl8 Cu1 O8 100.83(10) . . ? N7 Cu2 N6 125.14(17) . . ? N7 Cu2 Cl8 118.51(13) . . ? N6 Cu2 Cl8 111.82(13) . . ? N7 Cu2 N2 79.71(16) . . ? N6 Cu2 N2 78.17(16) . . ? Cl8 Cu2 N2 137.02(10) . . ? N9 Cu3 N8 138.79(19) . . ? N9 Cu3 N3 82.53(17) . . ? N8 Cu3 N3 79.58(17) . . ? N9 Cu3 O1 123.14(18) . . ? N8 Cu3 O1 96.31(19) . . ? N3 Cu3 O1 130.66(16) . . ? O2 Cl1 O1 114.4(4) . . ? O2 Cl1 O3 108.7(4) . . ? O1 Cl1 O3 108.1(3) . . ? O2 Cl1 O4 110.2(3) . . ? O1 Cl1 O4 108.0(3) . . ? O3 Cl1 O4 107.3(3) . . ? O6 Cl2 O5 111.0(3) . . ? O6 Cl2 O7 109.8(3) . . ? O5 Cl2 O7 109.0(3) . . ? O6 Cl2 O8 108.9(3) . . ? O5 Cl2 O8 109.2(3) . . ? O7 Cl2 O8 108.8(3) . . ? O11 Cl3 O12 109.2(4) . . ? O11 Cl3 O10 110.0(4) . . ? O12 Cl3 O10 109.9(4) . . ? O11 Cl3 O9 111.2(4) . . ? O12 Cl3 O9 108.2(3) . . ? O10 Cl3 O9 108.3(3) . . ? Cl1 O1 Cu3 105.9(3) . . ? Cl2 O8 Cu1 136.1(2) . . ? Cu1 Cl8 Cu2 114.44(6) . . ? C14 N1 C20 111.9(4) . . ? C14 N1 C13 112.9(4) . . ? C20 N1 C13 106.4(4) . . ? C14 N1 Cu1 103.8(3) . . ? C20 N1 Cu1 104.9(3) . . ? C13 N1 Cu1 116.8(3) . . ? C27 N2 C33 111.4(4) . . ? C27 N2 C26 112.4(4) . . ? C33 N2 C26 107.2(4) . . ? C27 N2 Cu2 103.6(3) . . ? C33 N2 Cu2 91.6(3) . . ? C26 N2 Cu2 128.4(3) . . ? C46 N3 C39 114.3(4) . . ? C46 N3 C40 110.6(4) . . ? C39 N3 C40 108.7(4) . . ? C46 N3 Cu3 103.9(3) . . ? C39 N3 Cu3 127.1(3) . . ? C40 N3 Cu3 89.2(3) . . ? C19 N4 C15 118.5(4) . . ? C19 N4 Cu1 128.1(4) . . ? C15 N4 Cu1 113.4(3) . . ? C25 N5 C21 119.5(4) . . ? C25 N5 Cu1 127.0(4) . . ? C21 N5 Cu1 113.3(3) . . ? C28 N6 C32 118.7(5) . . ? C28 N6 Cu2 119.0(4) . . ? C32 N6 Cu2 122.2(4) . . ? C38 N7 C34 118.2(5) . . ? C38 N7 Cu2 126.9(4) . . ? C34 N7 Cu2 114.8(3) . . ? C51 N8 C47 118.2(5) . . ? C51 N8 Cu3 120.5(4) . . ? C47 N8 Cu3 119.3(4) . . ? C45 N9 C41 118.2(5) . . ? C45 N9 Cu3 128.5(4) . . ? C41 N9 Cu3 113.2(4) . . ? C2 C1 C6 120.6(4) . . ? C2 C1 C13 119.1(4) . . ? C6 C1 C13 120.0(4) . . ? C3 C2 C1 119.3(4) . . ? C3 C2 C8 118.9(4) . . ? C1 C2 C8 121.5(4) . . ? C2 C3 C4 120.4(4) . . ? C2 C3 C26 119.0(4) . . ? C4 C3 C26 120.4(4) . . ? C5 C4 C3 119.7(5) . . ? C5 C4 C10 120.1(4) . . ? C3 C4 C10 119.8(4) . . ? C4 C5 C6 120.0(4) . . ? C4 C5 C39 120.4(4) . . ? C6 C5 C39 119.6(4) . . ? C1 C6 C5 119.6(4) . . ? C1 C6 C12 121.6(4) . . ? C5 C6 C12 118.5(4) . . ? C2 C8 C7 114.1(4) . . ? C9 C10 C4 111.1(5) . . ? C6 C12 C11 113.5(5) . . ? N1 C13 C1 117.6(4) . . ? N1 C14 C15 110.3(4) . . ? N4 C15 C16 121.7(5) . . ? N4 C15 C14 114.8(4) . . ? C16 C15 C14 123.4(5) . . ? C15 C16 C17 118.9(5) . . ? C18 C17 C16 119.2(5) . . ? C19 C18 C17 118.9(5) . . ? N4 C19 C18 122.7(5) . . ? N1 C20 C21 109.0(4) . . ? N5 C21 C22 121.4(5) . . ? N5 C21 C20 115.6(4) . . ? C22 C21 C20 122.9(5) . . ? C23 C22 C21 118.8(5) . . ? C24 C23 C22 119.4(5) . . ? C23 C24 C25 119.5(5) . . ? N5 C25 C24 121.3(5) . . ? N2 C26 C3 115.8(4) . . ? N2 C27 C28 113.1(4) . . ? N6 C28 C29 121.5(5) . . ? N6 C28 C27 119.0(5) . . ? C29 C28 C27 119.4(5) . . ? C30 C29 C28 119.0(6) . . ? C31 C30 C29 119.5(5) . . ? C30 C31 C32 118.6(6) . . ? N6 C32 C31 122.7(6) . . ? N2 C33 C34 111.8(4) . . ? N7 C34 C35 122.1(5) . . ? N7 C34 C33 114.6(5) . . ? C35 C34 C33 123.2(5) . . ? C34 C35 C36 118.7(6) . . ? C37 C36 C35 119.7(6) . . ? C36 C37 C38 118.5(6) . . ? N7 C38 C37 122.7(6) . . ? N3 C39 C5 116.1(4) . . ? N3 C40 C41 112.5(4) . . ? N9 C41 C42 121.7(5) . . ? N9 C41 C40 116.0(5) . . ? C42 C41 C40 122.2(5) . . ? C41 C42 C43 119.3(6) . . ? C44 C43 C42 119.2(6) . . ? C43 C44 C45 119.1(6) . . ? N9 C45 C44 122.4(5) . . ? N3 C46 C47 113.6(4) . . ? N8 C47 C48 121.1(5) . . ? N8 C47 C46 118.4(5) . . ? C48 C47 C46 120.4(5) . . ? C49 C48 C47 120.3(6) . . ? C48 C49 C50 119.0(6) . . ? C51 C50 C49 118.6(6) . . ? N8 C51 C50 122.9(6) . . ? Cl5 C52 Cl4 112.4(10) . . ? Cl5' C52' Cl4' 107.6(12) . . ? Cl7 C53 Cl6 112.6(4) . . ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 24.18 _diffrn_measured_fraction_theta_full 0.937 _refine_diff_density_max 0.548 _refine_diff_density_min -0.762 _refine_diff_density_rms 0.089 #=END data_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[LCu2](BF4)2-CH2Cl2' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H59 B2 Cl2 Cu2 F8 N9' _chemical_formula_weight 1181.68 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' 'F' 'F' 0.0171 0.0103 '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' '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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.034(4) _cell_length_b 27.69(3) _cell_length_c 19.83(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.45(5) _cell_angle_gamma 90.00 _cell_volume 5506(8) _cell_formula_units_Z 4 _cell_measurement_temperature 188(2) _cell_measurement_reflns_used 21943 _cell_measurement_theta_min 1.79 _cell_measurement_theta_max 24.16 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.426 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2432 _exptl_absorpt_coefficient_mu 0.941 _exptl_absorpt_correction_type 'Semi-empirical from psi-scans (SADABS)' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 188(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21943 _diffrn_reflns_av_R_equivalents 0.0694 _diffrn_reflns_av_sigmaI/netI 0.0790 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 24.16 _reflns_number_total 8689 _reflns_number_gt 5799 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0264P)^2^+20.2700P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8689 _refine_ls_number_parameters 704 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.1300 _refine_ls_R_factor_gt 0.0783 _refine_ls_wR_factor_ref 0.1602 _refine_ls_wR_factor_gt 0.1368 _refine_ls_goodness_of_fit_ref 1.181 _refine_ls_restrained_S_all 1.181 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.001 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 0.07521(8) 0.71881(3) 0.74444(4) 0.0358(2) Uani 1 1 d . . . Cu2 Cu 0.14922(8) 1.00538(3) 0.72086(4) 0.0351(2) Uani 1 1 d . . . N1 N 0.2074(5) 0.85401(17) 0.6397(2) 0.0275(12) Uani 1 1 d . . . N2 N -0.1369(5) 0.75782(18) 0.7737(3) 0.0305(12) Uani 1 1 d . . . N3 N -0.0883(5) 0.98417(17) 0.7460(2) 0.0288(12) Uani 1 1 d . . . N4 N 0.2948(5) 0.98215(17) 0.6617(3) 0.0305(12) Uani 1 1 d . . . N5 N 0.2293(5) 0.72549(18) 0.6825(2) 0.0312(13) Uani 1 1 d . . . N6 N 0.1168(5) 0.74649(18) 0.8369(3) 0.0333(13) Uani 1 1 d . . . N7 N -0.0638(5) 0.66900(18) 0.7194(3) 0.0379(14) Uani 1 1 d . . . N8 N 0.1657(5) 0.98431(18) 0.8170(3) 0.0341(13) Uani 1 1 d . . . N9 N 0.0464(5) 1.06210(18) 0.6809(3) 0.0339(13) Uani 1 1 d . . . C1 C -0.0361(6) 0.8591(2) 0.6153(3) 0.0241(14) Uani 1 1 d . . . C2 C -0.1006(6) 0.8185(2) 0.6415(3) 0.0279(14) Uani 1 1 d . . . C3 C -0.1917(6) 0.8249(2) 0.6933(3) 0.0274(14) Uani 1 1 d . . . C4 C -0.2232(5) 0.8712(2) 0.7148(3) 0.0259(14) Uani 1 1 d . . . C5 C -0.1721(6) 0.9119(2) 0.6821(3) 0.0258(14) Uani 1 1 d . . . C6 C -0.0807(6) 0.9060(2) 0.6299(3) 0.0261(14) Uani 1 1 d . . . C7 C -0.1811(7) 0.7638(3) 0.5487(4) 0.058(2) Uani 1 1 d . . . H7A H -0.1696 0.7325 0.5288 0.070 Uiso 1 1 calc R . . H7B H -0.1640 0.7883 0.5159 0.070 Uiso 1 1 calc R . . H7C H -0.2708 0.7669 0.5630 0.070 Uiso 1 1 calc R . . C8 C -0.0833(6) 0.7696(2) 0.6096(3) 0.0329(15) Uani 1 1 d . . . H8A H -0.0991 0.7448 0.6422 0.039 Uiso 1 1 calc R . . H8B H 0.0066 0.7662 0.5955 0.039 Uiso 1 1 calc R . . C9 C -0.4649(6) 0.8798(3) 0.7469(4) 0.049(2) Uani 1 1 d . . . H9A H -0.5209 0.8836 0.7846 0.059 Uiso 1 1 calc R . . H9B H -0.4880 0.8504 0.7235 0.059 Uiso 1 1 calc R . . H9C H -0.4775 0.9066 0.7168 0.059 Uiso 1 1 calc R . . C10 C -0.3196(6) 0.8776(2) 0.7720(3) 0.0299(15) Uani 1 1 d . . . H10A H -0.3082 0.8512 0.8031 0.036 Uiso 1 1 calc R . . H10B H -0.2977 0.9069 0.7960 0.036 Uiso 1 1 calc R . . C11 C -0.1507(6) 0.9627(2) 0.5361(3) 0.0350(16) Uani 1 1 d . . . H11A H -0.1228 0.9902 0.5109 0.042 Uiso 1 1 calc R . . H11B H -0.2313 0.9703 0.5582 0.042 Uiso 1 1 calc R . . H11C H -0.1665 0.9359 0.5061 0.042 Uiso 1 1 calc R . . C12 C -0.0416(6) 0.9493(2) 0.5890(3) 0.0270(14) Uani 1 1 d . . . H12A H 0.0395 0.9424 0.5668 0.032 Uiso 1 1 calc R . . H12B H -0.0251 0.9763 0.6186 0.032 Uiso 1 1 calc R . . C13 C 0.0999(5) 0.8529(2) 0.5849(3) 0.0264(14) Uani 1 1 d . . . H13A H 0.1028 0.8227 0.5613 0.032 Uiso 1 1 calc R . . H13B H 0.1141 0.8784 0.5532 0.032 Uiso 1 1 calc R . . C14 C 0.2178(5) 0.9003(2) 0.6739(3) 0.0238(13) Uani 1 1 d . . . H14A H 0.2555 0.8953 0.7186 0.029 Uiso 1 1 calc R . . H14B H 0.1298 0.9133 0.6779 0.029 Uiso 1 1 calc R . . C15 C 0.3009(6) 0.9362(2) 0.6387(3) 0.0258(14) Uani 1 1 d . . . C16 C 0.3904(6) 0.9237(2) 0.5904(3) 0.0362(16) Uani 1 1 d . . . H16 H 0.3897 0.8915 0.5721 0.043 Uiso 1 1 calc R . . C17 C 0.4812(7) 0.9574(3) 0.5682(3) 0.0423(18) Uani 1 1 d . . . H17 H 0.5437 0.9489 0.5349 0.051 Uiso 1 1 calc R . . C18 C 0.4799(7) 1.0028(3) 0.5946(4) 0.0468(19) Uani 1 1 d . . . H18 H 0.5439 1.0264 0.5814 0.056 Uiso 1 1 calc R . . C19 C 0.3852(7) 1.0145(2) 0.6405(3) 0.0409(18) Uani 1 1 d . . . H19 H 0.3835 1.0467 0.6581 0.049 Uiso 1 1 calc R . . C20 C 0.2045(6) 0.8126(2) 0.6849(3) 0.0277(14) Uani 1 1 d . . . H20A H 0.1133 0.8050 0.6931 0.033 Uiso 1 1 calc R . . H20B H 0.2476 0.8213 0.7273 0.033 Uiso 1 1 calc R . . C21 C 0.2712(6) 0.7683(2) 0.6583(3) 0.0260(14) Uani 1 1 d . . . C22 C 0.3759(6) 0.7710(2) 0.6142(3) 0.0346(16) Uani 1 1 d . . . H22 H 0.4034 0.8016 0.5969 0.041 Uiso 1 1 calc R . . C23 C 0.4389(6) 0.7292(2) 0.5960(3) 0.0391(17) Uani 1 1 d . . . H23 H 0.5101 0.7303 0.5652 0.047 Uiso 1 1 calc R . . C24 C 0.3990(7) 0.6854(3) 0.6225(4) 0.0437(18) Uani 1 1 d . . . H24 H 0.4437 0.6560 0.6116 0.052 Uiso 1 1 calc R . . C25 C 0.2945(7) 0.6852(2) 0.6645(3) 0.0395(17) Uani 1 1 d . . . H25 H 0.2660 0.6548 0.6821 0.047 Uiso 1 1 calc R . . C26 C -0.2424(6) 0.7804(2) 0.7287(3) 0.0342(15) Uani 1 1 d . . . H26A H -0.3168 0.7892 0.7550 0.041 Uiso 1 1 calc R . . H26B H -0.2732 0.7573 0.6955 0.041 Uiso 1 1 calc R . . C27 C -0.0966(6) 0.7898(2) 0.8300(3) 0.0366(16) Uani 1 1 d . . . H27A H -0.1668 0.7906 0.8614 0.044 Uiso 1 1 calc R . . H27B H -0.0861 0.8220 0.8129 0.044 Uiso 1 1 calc R . . C28 C 0.0305(6) 0.7751(2) 0.8670(3) 0.0378(16) Uani 1 1 d . . . C29 C 0.0599(8) 0.7929(3) 0.9318(4) 0.058(2) Uani 1 1 d . . . H29 H -0.0031 0.8132 0.9534 0.069 Uiso 1 1 calc R . . C30 C 0.1787(8) 0.7815(3) 0.9645(4) 0.071(3) Uani 1 1 d . . . H30 H 0.1990 0.7936 1.0091 0.085 Uiso 1 1 calc R . . C31 C 0.2684(8) 0.7529(3) 0.9333(4) 0.056(2) Uani 1 1 d . . . H31 H 0.3526 0.7448 0.9551 0.067 Uiso 1 1 calc R . . C32 C 0.2336(7) 0.7361(2) 0.8695(4) 0.0401(17) Uani 1 1 d . . . H32 H 0.2960 0.7160 0.8472 0.048 Uiso 1 1 calc R . . C33 C -0.1881(6) 0.7118(2) 0.8004(3) 0.0395(17) Uani 1 1 d . . . H33A H -0.2783 0.7160 0.8135 0.047 Uiso 1 1 calc R . . H33B H -0.1349 0.7022 0.8395 0.047 Uiso 1 1 calc R . . C34 C -0.1831(7) 0.6733(2) 0.7473(4) 0.0433(19) Uani 1 1 d . . . C35 C -0.2926(8) 0.6455(3) 0.7289(5) 0.058(2) Uani 1 1 d . . . H35 H -0.3755 0.6493 0.7508 0.070 Uiso 1 1 calc R . . C36 C -0.2793(8) 0.6118(3) 0.6781(5) 0.067(3) Uani 1 1 d . . . H36 H -0.3540 0.5921 0.6639 0.081 Uiso 1 1 calc R . . C37 C -0.1602(9) 0.6065(2) 0.6482(4) 0.055(2) Uani 1 1 d . . . H37 H -0.1501 0.5831 0.6131 0.066 Uiso 1 1 calc R . . C38 C -0.0528(8) 0.6359(2) 0.6697(4) 0.0477(19) Uani 1 1 d . . . H38 H 0.0310 0.6324 0.6486 0.057 Uiso 1 1 calc R . . C39 C -0.2017(6) 0.9624(2) 0.7056(3) 0.0296(15) Uani 1 1 d . . . H39A H -0.2219 0.9824 0.6669 0.036 Uiso 1 1 calc R . . H39B H -0.2791 0.9617 0.7324 0.036 Uiso 1 1 calc R . . C40 C -0.0702(6) 0.9590(2) 0.8118(3) 0.0346(16) Uani 1 1 d . . . H40A H -0.0734 0.9248 0.8040 0.042 Uiso 1 1 calc R . . H40B H -0.1433 0.9672 0.8393 0.042 Uiso 1 1 calc R . . C41 C 0.0586(7) 0.9710(2) 0.8500(3) 0.0396(17) Uani 1 1 d . . . C42 C 0.0642(8) 0.9656(3) 0.9199(4) 0.062(2) Uani 1 1 d . . . H42 H -0.0148 0.9580 0.9434 0.074 Uiso 1 1 calc R . . C43 C 0.1849(9) 0.9712(3) 0.9548(4) 0.075(3) Uani 1 1 d . . . H43 H 0.1903 0.9674 1.0029 0.090 Uiso 1 1 calc R . . C44 C 0.2970(8) 0.9821(3) 0.9211(4) 0.058(2) Uani 1 1 d . . . H44 H 0.3825 0.9846 0.9445 0.070 Uiso 1 1 calc R . . C45 C 0.2831(7) 0.9894(2) 0.8525(4) 0.0422(18) Uani 1 1 d . . . H45 H 0.3604 0.9986 0.8287 0.051 Uiso 1 1 calc R . . C46 C -0.1195(6) 1.0359(2) 0.7566(3) 0.0342(16) Uani 1 1 d . . . H46A H -0.0709 1.0475 0.7961 0.041 Uiso 1 1 calc R . . H46B H -0.2130 1.0395 0.7637 0.041 Uiso 1 1 calc R . . C47 C -0.0827(6) 1.0652(2) 0.6963(3) 0.0325(15) Uani 1 1 d . . . C48 C -0.1732(7) 1.0936(2) 0.6610(3) 0.0423(18) Uani 1 1 d . . . H48 H -0.2645 1.0949 0.6734 0.051 Uiso 1 1 calc R . . C49 C -0.1303(8) 1.1207(2) 0.6067(4) 0.050(2) Uani 1 1 d . . . H49 H -0.1920 1.1401 0.5803 0.060 Uiso 1 1 calc R . . C50 C 0.0018(8) 1.1189(2) 0.5918(4) 0.0445(18) Uani 1 1 d . . . H50 H 0.0347 1.1381 0.5557 0.053 Uiso 1 1 calc R . . C51 C 0.0866(7) 1.0892(2) 0.6293(3) 0.0388(17) Uani 1 1 d . . . H51 H 0.1786 1.0877 0.6180 0.047 Uiso 1 1 calc R . . B1 B 0.4594(7) 0.3447(3) 0.0738(4) 0.0367(19) Uani 1 1 d D . . F1 F 0.3430(6) 0.3669(3) 0.0639(4) 0.140(3) Uani 1 1 d D A . F2 F 0.4268(14) 0.2983(4) 0.0759(11) 0.104(7) Uani 0.57(3) 1 d PD A 1 F3 F 0.5603(15) 0.3504(7) 0.0330(10) 0.103(7) Uani 0.57(3) 1 d PD A 1 F4 F 0.5097(14) 0.3576(9) 0.1360(6) 0.117(8) Uani 0.57(3) 1 d PD A 1 F2B F 0.488(3) 0.3265(10) 0.0133(7) 0.114(9) Uani 0.43(3) 1 d PD A 2 F3B F 0.540(2) 0.3828(6) 0.082(2) 0.158(16) Uani 0.43(3) 1 d PD A 2 F4B F 0.479(2) 0.3126(13) 0.1225(17) 0.159(18) Uani 0.43(3) 1 d PD A 2 B2 B -0.3730(8) 1.0475(3) 0.8780(4) 0.042(2) Uani 1 1 d . . . F5 F -0.3617(5) 0.99905(18) 0.8815(3) 0.101(2) Uani 1 1 d . . . F6 F -0.4240(4) 1.0619(2) 0.8163(2) 0.0901(18) Uani 1 1 d . . . F7 F -0.4595(4) 1.06299(17) 0.9265(2) 0.0709(14) Uani 1 1 d . . . F8 F -0.2503(4) 1.06855(18) 0.8897(2) 0.0669(13) Uani 1 1 d . . . C52 C -0.6035(10) 1.1067(4) 1.0485(5) 0.090(3) Uani 1 1 d . . . H52A H -0.5864 1.0845 1.0851 0.107 Uiso 1 1 calc R . . H52B H -0.5684 1.0928 1.0086 0.107 Uiso 1 1 calc R . . Cl1 Cl -0.5234(5) 1.16000(15) 1.06616(17) 0.1709(19) Uani 1 1 d . . . Cl2 Cl -0.7750(3) 1.11457(11) 1.03615(14) 0.1009(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0396(5) 0.0342(5) 0.0339(5) 0.0047(4) 0.0047(4) -0.0034(4) Cu2 0.0384(5) 0.0362(5) 0.0308(4) -0.0004(4) 0.0034(4) 0.0018(4) N1 0.025(3) 0.032(3) 0.026(3) 0.004(2) 0.004(2) 0.000(2) N2 0.029(3) 0.032(3) 0.031(3) 0.010(3) 0.002(2) 0.000(2) N3 0.034(3) 0.030(3) 0.023(3) 0.000(2) 0.003(2) 0.000(2) N4 0.028(3) 0.030(3) 0.033(3) 0.005(2) 0.000(2) -0.003(2) N5 0.032(3) 0.030(3) 0.032(3) 0.005(2) 0.000(2) 0.002(2) N6 0.029(3) 0.037(3) 0.034(3) 0.006(3) -0.001(3) 0.002(3) N7 0.044(4) 0.028(3) 0.042(4) 0.012(3) -0.003(3) -0.003(3) N8 0.031(3) 0.036(3) 0.036(3) 0.003(3) -0.002(3) 0.001(2) N9 0.048(4) 0.028(3) 0.025(3) -0.005(3) -0.003(3) 0.000(3) C1 0.022(3) 0.035(4) 0.015(3) 0.002(3) -0.004(3) -0.002(3) C2 0.025(3) 0.028(3) 0.030(4) 0.005(3) -0.005(3) 0.003(3) C3 0.020(3) 0.032(4) 0.030(4) 0.003(3) -0.002(3) -0.002(3) C4 0.017(3) 0.040(4) 0.021(3) 0.006(3) 0.001(3) -0.002(3) C5 0.025(3) 0.031(3) 0.021(3) 0.004(3) -0.003(3) 0.003(3) C6 0.022(3) 0.032(4) 0.024(3) 0.002(3) -0.003(3) 0.001(3) C7 0.054(5) 0.059(5) 0.060(5) -0.020(4) -0.010(4) -0.006(4) C8 0.036(4) 0.024(3) 0.038(4) 0.000(3) -0.002(3) -0.003(3) C9 0.026(4) 0.080(6) 0.042(4) 0.020(4) 0.005(3) 0.003(4) C10 0.025(3) 0.039(4) 0.025(3) 0.008(3) 0.006(3) -0.002(3) C11 0.036(4) 0.037(4) 0.032(4) 0.012(3) 0.000(3) 0.007(3) C12 0.024(3) 0.026(3) 0.032(4) 0.003(3) 0.004(3) -0.002(3) C13 0.029(3) 0.028(3) 0.022(3) 0.004(3) -0.001(3) 0.000(3) C14 0.020(3) 0.028(3) 0.023(3) 0.004(3) 0.000(3) 0.001(3) C15 0.022(3) 0.032(4) 0.024(3) 0.005(3) 0.001(3) 0.003(3) C16 0.034(4) 0.046(4) 0.029(4) 0.002(3) 0.005(3) 0.003(3) C17 0.037(4) 0.056(5) 0.035(4) 0.013(4) 0.016(3) 0.000(4) C18 0.037(4) 0.057(5) 0.047(4) 0.015(4) 0.012(3) -0.009(4) C19 0.046(4) 0.028(4) 0.048(4) 0.006(3) -0.004(4) -0.009(3) C20 0.027(3) 0.034(4) 0.022(3) 0.002(3) 0.001(3) 0.003(3) C21 0.021(3) 0.031(4) 0.026(3) 0.002(3) -0.001(3) 0.000(3) C22 0.030(4) 0.035(4) 0.039(4) -0.002(3) 0.001(3) -0.001(3) C23 0.030(4) 0.049(5) 0.038(4) -0.004(4) 0.005(3) 0.007(3) C24 0.041(4) 0.045(4) 0.046(4) -0.004(4) 0.003(4) 0.014(3) C25 0.047(4) 0.031(4) 0.041(4) -0.001(3) 0.007(4) 0.002(3) C26 0.029(4) 0.040(4) 0.033(4) 0.008(3) -0.004(3) -0.004(3) C27 0.040(4) 0.041(4) 0.029(4) 0.001(3) 0.003(3) 0.011(3) C28 0.037(4) 0.045(4) 0.032(4) 0.005(3) 0.003(3) 0.008(3) C29 0.057(5) 0.083(6) 0.032(4) -0.013(4) -0.001(4) 0.022(4) C30 0.065(6) 0.101(7) 0.044(5) -0.020(5) -0.021(4) 0.024(5) C31 0.053(5) 0.065(5) 0.048(5) -0.005(4) -0.019(4) 0.014(4) C32 0.034(4) 0.039(4) 0.047(4) 0.008(3) 0.001(3) 0.006(3) C33 0.033(4) 0.044(4) 0.042(4) 0.019(4) 0.005(3) -0.004(3) C34 0.036(4) 0.033(4) 0.060(5) 0.023(4) -0.008(4) -0.008(3) C35 0.041(5) 0.034(4) 0.097(7) 0.017(5) -0.008(4) 0.000(4) C36 0.048(5) 0.041(5) 0.110(8) 0.012(5) -0.029(5) -0.002(4) C37 0.085(6) 0.024(4) 0.055(5) 0.004(4) -0.025(5) -0.006(4) C38 0.063(5) 0.030(4) 0.050(5) 0.011(4) -0.009(4) 0.002(4) C39 0.021(3) 0.040(4) 0.027(4) 0.010(3) 0.005(3) 0.001(3) C40 0.033(4) 0.041(4) 0.029(4) 0.001(3) 0.004(3) 0.002(3) C41 0.051(5) 0.040(4) 0.027(4) 0.000(3) -0.007(3) 0.002(3) C42 0.052(5) 0.096(7) 0.035(5) 0.009(4) -0.005(4) -0.016(5) C43 0.079(7) 0.108(8) 0.036(5) 0.019(5) -0.017(5) -0.015(6) C44 0.058(5) 0.069(6) 0.046(5) 0.012(4) -0.019(4) -0.001(4) C45 0.035(4) 0.039(4) 0.052(5) 0.011(4) 0.002(4) 0.001(3) C46 0.036(4) 0.041(4) 0.026(4) -0.010(3) 0.004(3) 0.002(3) C47 0.039(4) 0.030(4) 0.028(4) -0.011(3) -0.004(3) 0.009(3) C48 0.047(4) 0.039(4) 0.041(4) -0.012(4) -0.007(4) 0.005(3) C49 0.070(6) 0.032(4) 0.046(5) 0.002(4) -0.018(4) 0.009(4) C50 0.063(5) 0.029(4) 0.042(4) 0.002(3) 0.004(4) -0.001(4) C51 0.062(5) 0.030(4) 0.024(4) -0.001(3) -0.002(3) -0.003(3) B1 0.034(5) 0.030(5) 0.047(5) -0.011(4) 0.013(4) 0.005(4) F1 0.101(5) 0.167(7) 0.150(6) -0.053(5) -0.023(4) 0.082(5) F2 0.089(9) 0.068(8) 0.154(16) 0.008(8) -0.007(10) -0.014(6) F3 0.082(10) 0.122(14) 0.108(13) 0.062(10) 0.034(9) 0.007(9) F4 0.125(11) 0.158(18) 0.068(10) -0.012(11) -0.001(7) -0.035(11) F2B 0.096(16) 0.16(2) 0.084(12) -0.034(13) 0.029(11) 0.039(14) F3B 0.136(18) 0.078(13) 0.26(4) -0.004(17) -0.03(2) -0.023(11) F4B 0.079(16) 0.22(3) 0.18(3) 0.17(3) 0.093(18) 0.082(18) B2 0.040(5) 0.057(6) 0.030(5) 0.014(4) 0.009(4) 0.013(4) F5 0.091(4) 0.053(3) 0.163(6) 0.012(4) 0.047(4) 0.012(3) F6 0.057(3) 0.171(6) 0.043(3) 0.018(3) 0.003(2) 0.023(3) F7 0.067(3) 0.091(4) 0.056(3) -0.001(3) 0.033(3) 0.011(3) F8 0.057(3) 0.106(4) 0.037(2) 0.002(3) 0.003(2) -0.009(3) C52 0.107(8) 0.100(8) 0.066(6) 0.004(6) 0.049(6) -0.002(6) Cl1 0.246(5) 0.188(4) 0.083(2) 0.007(2) 0.050(3) -0.133(4) Cl2 0.127(2) 0.106(2) 0.0696(17) -0.0042(16) 0.0045(17) 0.0237(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N7 2.009(6) . ? Cu1 N6 2.014(6) . ? Cu1 N5 2.024(5) . ? Cu1 N2 2.478(5) . ? Cu2 N8 1.993(6) . ? Cu2 N4 2.017(5) . ? Cu2 N9 2.022(5) . ? N1 C14 1.451(7) . ? N1 C20 1.456(7) . ? N1 C13 1.499(7) . ? N2 C27 1.470(8) . ? N2 C33 1.480(8) . ? N2 C26 1.493(7) . ? N3 C40 1.483(8) . ? N3 C46 1.484(8) . ? N3 C39 1.491(7) . ? N4 C15 1.354(7) . ? N4 C19 1.354(8) . ? N5 C25 1.348(8) . ? N5 C21 1.354(7) . ? N6 C28 1.334(8) . ? N6 C32 1.346(8) . ? N7 C34 1.344(8) . ? N7 C38 1.355(9) . ? N8 C41 1.333(8) . ? N8 C45 1.354(8) . ? N9 C51 1.345(8) . ? N9 C47 1.347(8) . ? C1 C2 1.406(8) . ? C1 C6 1.409(8) . ? C1 C13 1.524(8) . ? C2 C3 1.414(8) . ? C2 C8 1.509(8) . ? C3 C4 1.394(8) . ? C3 C26 1.516(8) . ? C4 C5 1.407(8) . ? C4 C10 1.533(8) . ? C5 C6 1.421(8) . ? C5 C39 1.509(8) . ? C6 C12 1.510(8) . ? C7 C8 1.533(9) . ? C9 C10 1.521(8) . ? C11 C12 1.528(8) . ? C14 C15 1.491(8) . ? C15 C16 1.385(8) . ? C16 C17 1.390(9) . ? C17 C18 1.363(10) . ? C18 C19 1.382(9) . ? C20 C21 1.504(8) . ? C21 C22 1.396(8) . ? C22 C23 1.374(8) . ? C23 C24 1.387(9) . ? C24 C25 1.366(9) . ? C27 C28 1.500(9) . ? C28 C29 1.396(9) . ? C29 C30 1.369(10) . ? C30 C31 1.366(10) . ? C31 C32 1.379(10) . ? C33 C34 1.501(10) . ? C34 C35 1.378(10) . ? C35 C36 1.384(12) . ? C36 C37 1.365(11) . ? C37 C38 1.402(10) . ? C40 C41 1.507(9) . ? C41 C42 1.394(9) . ? C42 C43 1.377(11) . ? C43 C44 1.366(11) . ? C44 C45 1.377(10) . ? C46 C47 1.503(9) . ? C47 C48 1.371(9) . ? C48 C49 1.395(10) . ? C49 C50 1.371(10) . ? C50 C51 1.379(9) . ? B1 F4B 1.321(12) . ? B1 F1 1.328(7) . ? B1 F2 1.327(11) . ? B1 F3 1.333(10) . ? B1 F3B 1.336(12) . ? B1 F2B 1.345(12) . ? B1 F4 1.360(11) . ? B2 F5 1.349(10) . ? B2 F6 1.364(9) . ? B2 F8 1.372(9) . ? B2 F7 1.391(9) . ? C52 Cl1 1.711(10) . ? C52 Cl2 1.742(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 Cu1 N6 126.9(2) . . ? N7 Cu1 N5 117.0(2) . . ? N6 Cu1 N5 112.6(2) . . ? N7 Cu1 N2 76.3(2) . . ? N6 Cu1 N2 76.57(19) . . ? N5 Cu1 N2 142.05(18) . . ? N8 Cu2 N4 115.5(2) . . ? N8 Cu2 N9 128.4(2) . . ? N4 Cu2 N9 113.0(2) . . ? C14 N1 C20 114.3(5) . . ? C14 N1 C13 113.1(4) . . ? C20 N1 C13 113.4(5) . . ? C27 N2 C33 109.6(5) . . ? C27 N2 C26 111.5(5) . . ? C33 N2 C26 109.1(5) . . ? C27 N2 Cu1 103.3(4) . . ? C33 N2 Cu1 91.3(3) . . ? C26 N2 Cu1 129.6(4) . . ? C40 N3 C46 110.4(5) . . ? C40 N3 C39 110.2(5) . . ? C46 N3 C39 107.8(5) . . ? C15 N4 C19 118.4(5) . . ? C15 N4 Cu2 122.7(4) . . ? C19 N4 Cu2 118.8(4) . . ? C25 N5 C21 118.0(5) . . ? C25 N5 Cu1 118.5(4) . . ? C21 N5 Cu1 123.5(4) . . ? C28 N6 C32 118.7(6) . . ? C28 N6 Cu1 121.4(4) . . ? C32 N6 Cu1 119.9(5) . . ? C34 N7 C38 117.4(6) . . ? C34 N7 Cu1 117.3(5) . . ? C38 N7 Cu1 124.6(5) . . ? C41 N8 C45 118.3(6) . . ? C41 N8 Cu2 121.0(4) . . ? C45 N8 Cu2 120.1(4) . . ? C51 N9 C47 117.4(6) . . ? C51 N9 Cu2 124.5(5) . . ? C47 N9 Cu2 116.1(4) . . ? C2 C1 C6 120.3(5) . . ? C2 C1 C13 119.4(5) . . ? C6 C1 C13 118.9(5) . . ? C1 C2 C3 119.4(5) . . ? C1 C2 C8 119.9(5) . . ? C3 C2 C8 120.3(5) . . ? C4 C3 C2 119.9(5) . . ? C4 C3 C26 121.4(5) . . ? C2 C3 C26 118.4(5) . . ? C3 C4 C5 120.2(5) . . ? C3 C4 C10 119.4(5) . . ? C5 C4 C10 120.2(5) . . ? C4 C5 C6 120.2(5) . . ? C4 C5 C39 121.3(5) . . ? C6 C5 C39 118.2(5) . . ? C1 C6 C5 118.5(5) . . ? C1 C6 C12 122.0(5) . . ? C5 C6 C12 119.4(5) . . ? C2 C8 C7 110.0(5) . . ? C9 C10 C4 112.8(5) . . ? C6 C12 C11 111.5(5) . . ? N1 C13 C1 109.9(4) . . ? N1 C14 C15 113.7(5) . . ? N4 C15 C16 120.6(6) . . ? N4 C15 C14 115.8(5) . . ? C16 C15 C14 123.3(6) . . ? C15 C16 C17 120.2(6) . . ? C18 C17 C16 118.9(6) . . ? C17 C18 C19 119.1(6) . . ? N4 C19 C18 122.7(6) . . ? N1 C20 C21 113.9(5) . . ? N5 C21 C22 121.4(6) . . ? N5 C21 C20 116.1(5) . . ? C22 C21 C20 122.4(5) . . ? C23 C22 C21 119.2(6) . . ? C22 C23 C24 119.5(6) . . ? C25 C24 C23 118.4(6) . . ? N5 C25 C24 123.5(6) . . ? N2 C26 C3 112.0(5) . . ? N2 C27 C28 114.1(5) . . ? N6 C28 C29 120.4(6) . . ? N6 C28 C27 119.8(6) . . ? C29 C28 C27 119.7(6) . . ? C30 C29 C28 120.0(7) . . ? C31 C30 C29 119.8(7) . . ? C30 C31 C32 117.7(7) . . ? N6 C32 C31 123.3(7) . . ? N2 C33 C34 109.7(5) . . ? N7 C34 C35 123.8(8) . . ? N7 C34 C33 114.1(6) . . ? C35 C34 C33 122.1(7) . . ? C34 C35 C36 117.9(8) . . ? C37 C36 C35 120.2(8) . . ? C36 C37 C38 118.8(8) . . ? N7 C38 C37 121.9(8) . . ? N3 C39 C5 112.6(5) . . ? N3 C40 C41 114.1(5) . . ? N8 C41 C42 121.3(7) . . ? N8 C41 C40 120.4(6) . . ? C42 C41 C40 118.3(6) . . ? C43 C42 C41 119.0(8) . . ? C44 C43 C42 120.3(8) . . ? C43 C44 C45 117.7(7) . . ? N8 C45 C44 123.2(7) . . ? N3 C46 C47 110.4(5) . . ? N9 C47 C48 122.9(6) . . ? N9 C47 C46 114.7(6) . . ? C48 C47 C46 122.4(6) . . ? C47 C48 C49 118.9(7) . . ? C50 C49 C48 118.7(7) . . ? C49 C50 C51 119.0(7) . . ? N9 C51 C50 123.0(7) . . ? F4B B1 F1 121.5(9) . . ? F4B B1 F2 49.8(17) . . ? F1 B1 F2 103.7(9) . . ? F4B B1 F3 115.6(9) . . ? F1 B1 F3 122.7(9) . . ? F2 B1 F3 109.3(12) . . ? F4B B1 F3B 111.9(19) . . ? F1 B1 F3B 100.0(11) . . ? F2 B1 F3B 155.6(12) . . ? F3 B1 F3B 60.6(13) . . ? F4B B1 F2B 111.6(18) . . ? F1 B1 F2B 105.3(10) . . ? F2 B1 F2B 74.2(13) . . ? F3 B1 F2B 45.9(9) . . ? F3B B1 F2B 104.7(16) . . ? F4B B1 F4 58.5(16) . . ? F1 B1 F4 107.5(9) . . ? F2 B1 F4 108.0(11) . . ? F3 B1 F4 104.9(11) . . ? F3B B1 F4 58.7(14) . . ? F2B B1 F4 145.3(14) . . ? F5 B2 F6 111.3(8) . . ? F5 B2 F8 109.9(6) . . ? F6 B2 F8 109.1(6) . . ? F5 B2 F7 108.9(6) . . ? F6 B2 F7 108.0(6) . . ? F8 B2 F7 109.6(7) . . ? Cl1 C52 Cl2 111.9(6) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 24.16 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.561 _refine_diff_density_min -0.660 _refine_diff_density_rms 0.088 #=END data_6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,3,5-Tris(bromomethyl)-2,4,6-triethylbenzene ; _chemical_name_common 'TriBr' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H21 Br3' _chemical_formula_weight 441.05 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' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' _cell_length_a 16.5648(11) _cell_length_b 16.5648(11) _cell_length_c 5.3351(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1267.78(15) _cell_formula_units_Z 3 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2671 _cell_measurement_theta_min 4.08 _cell_measurement_theta_max 28.34 _exptl_crystal_description 'hexagonal p' _exptl_crystal_colour colourless _exptl_crystal_size_max '0.5' _exptl_crystal_size_mid '0.2' _exptl_crystal_size_min '0.2' _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.733 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 7.143 _exptl_absorpt_correction_type 'Semi-empirical from psi-scans (SADABS)' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2671 _diffrn_reflns_av_R_equivalents 0.0528 _diffrn_reflns_av_sigmaI/netI 0.0403 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 4.08 _diffrn_reflns_theta_max 28.34 _reflns_number_total 1341 _reflns_number_gt 1317 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0309P)^2^+1.7604P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0064(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.394(19) _refine_ls_number_reflns 1341 _refine_ls_number_parameters 57 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0290 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_ref 0.0689 _refine_ls_wR_factor_gt 0.0678 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.055 _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 Br1 Br 0.95915(3) 0.20067(3) 0.9880 0.05023(15) Uani 1 1 d . . . C1 C 0.7701(3) -0.0372(3) 0.4062(11) 0.0581(11) Uani 1 1 d . . . H1A H 0.7078 -0.0476 0.4202 0.070 Uiso 1 1 calc R . . H1B H 0.7691 -0.0874 0.3140 0.070 Uiso 1 1 calc R . . H1C H 0.8085 0.0205 0.3199 0.070 Uiso 1 1 calc R . . C2 C 0.8092(2) -0.0325(2) 0.6644(7) 0.0401(7) Uani 1 1 d . . . H2A H 0.7696 -0.0899 0.7507 0.048 Uiso 1 1 calc R . . H2B H 0.8085 0.0169 0.7566 0.048 Uiso 1 1 calc R . . C3 C 0.90811(19) -0.01608(19) 0.6615(6) 0.0324(6) Uani 1 1 d . . . C4 C 0.9844(2) 0.07561(19) 0.6585(6) 0.0338(6) Uani 1 1 d . . . C5 C 0.9675(2) 0.1563(2) 0.6483(6) 0.0363(6) Uani 1 1 d . . . H5A H 0.9105 0.1379 0.5594 0.044 Uiso 1 1 calc R . . H5B H 1.0173 0.2065 0.5573 0.044 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0581(2) 0.0511(2) 0.0512(2) -0.00297(14) 0.00637(16) 0.03456(19) C1 0.0428(19) 0.059(3) 0.068(3) 0.001(2) -0.013(2) 0.0223(18) C2 0.0263(13) 0.0367(14) 0.056(2) 0.0026(13) 0.0014(12) 0.0149(11) C3 0.0260(12) 0.0300(14) 0.0414(16) 0.0005(11) 0.0003(10) 0.0141(11) C4 0.0337(14) 0.0279(13) 0.0425(17) 0.0006(11) 0.0004(11) 0.0175(11) C5 0.0363(14) 0.0310(13) 0.0439(17) 0.0011(11) 0.0000(12) 0.0187(11) _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 Br1 C5 1.987(3) . ? C1 C2 1.508(6) . ? C2 C3 1.521(4) . ? C3 C4 1.399(4) 2_645 ? C3 C4 1.409(4) . ? C4 C3 1.399(4) 3_765 ? C4 C5 1.497(4) . ? 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 C1 C2 C3 113.4(3) . . ? C4 C3 C4 119.4(3) 2_645 . ? C4 C3 C2 120.7(3) 2_645 . ? C4 C3 C2 119.9(3) . . ? C3 C4 C3 120.6(3) 3_765 . ? C3 C4 C5 119.7(3) 3_765 . ? C3 C4 C5 119.7(3) . . ? C4 C5 Br1 112.1(2) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.491 _refine_diff_density_min -0.350 _refine_diff_density_rms 0.074