Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Diaz, Carmen' 'Maestro, Miguel' 'Mahia, Jose' 'Ribas, Juan' 'Tercero, Javier' _publ_contact_author_name 'Prof Carmen Diaz' _publ_contact_author_address ; Inorganic Chemistry University of Barcelona Marti i Franqués, 1-11 Barcelona Barcelona 08028 SPAIN ; _publ_contact_author_email 'CARME.DIAZ@QI.UB.ES' _publ_section_title ; Synthesis, characterization, and magnetic properties of new complexes based on self-assembled homotrinuclear units CuII-CuII-CuII ; data_complex_1 _database_code_CSD 169868 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H44 Cu3 F12 N6 O9 P2' _chemical_formula_weight 981.16 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' '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' _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 10.22180(10) _cell_length_b 13.182 _cell_length_c 14.63610(10) _cell_angle_alpha 70.9310(10) _cell_angle_beta 83.8970(10) _cell_angle_gamma 87.7610(10) _cell_volume 1853.39(2) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.758 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 994 _exptl_absorpt_coefficient_mu 1.903 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5988 _exptl_absorpt_correction_T_max 0.9108 _exptl_absorpt_process_details 'Sadabs' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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_% 0.36 _diffrn_reflns_number 22103 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.0596 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 28.27 _reflns_number_total 9066 _reflns_number_gt 6335 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics '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 w=1/[\s^2^(Fo^2^)+(0.0744P)^2^+0.7296P] 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 9066 _refine_ls_number_parameters 460 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0754 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1542 _refine_ls_wR_factor_gt 0.1425 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.006 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 1.15147(5) 0.73164(4) 0.71578(4) 0.02947(13) Uani 1 d . . . Cu2 Cu 0.76082(5) 0.82417(4) 0.50362(4) 0.03079(14) Uani 1 d . . . Cu3 Cu 0.36317(5) 0.86919(4) 0.29782(4) 0.03328(14) Uani 1 d . . . O1 O 1.0771(3) 0.6774(2) 0.6233(2) 0.0351(7) Uani 1 d . . . O2 O 1.0370(3) 0.8617(2) 0.6601(2) 0.0323(6) Uani 1 d . . . O3 O 0.8702(3) 0.9034(2) 0.5647(2) 0.0325(6) Uani 1 d . . . O4 O 0.6450(3) 0.9474(2) 0.4308(2) 0.0346(6) Uani 1 d . . . O5 O 0.4541(3) 0.7556(2) 0.3893(2) 0.0397(7) Uani 1 d . . . O6 O 0.4762(3) 0.9674(2) 0.3408(2) 0.0347(6) Uani 1 d . . . N1 N 1.1863(4) 0.7657(3) 0.8355(3) 0.0362(8) Uani 1 d . . . N2 N 1.2480(4) 0.5911(3) 0.7708(3) 0.0373(8) Uani 1 d . . . N3 N 0.8897(3) 0.7117(3) 0.5439(3) 0.0308(7) Uani 1 d . . . N4 N 0.6419(3) 0.7379(3) 0.4660(3) 0.0360(8) Uani 1 d . . . N5 N 0.2844(4) 0.7618(3) 0.2471(3) 0.0522(11) Uani 1 d . . . N6 N 0.3108(4) 0.9833(3) 0.1786(3) 0.0394(8) Uani 1 d . . . C1 C 1.2356(8) 0.6684(5) 0.9061(5) 0.080(2) Uani 1 d . . . H1 H 1.1623 0.6269 0.9468 0.095 Uiso 1 calc R . . H1A H 1.2908 0.6882 0.9476 0.095 Uiso 1 calc R . . C2 C 1.3140(6) 0.6019(5) 0.8530(4) 0.0610(15) Uani 1 d . . . H2 H 1.3995 0.6347 0.8283 0.073 Uiso 1 calc R . . H2A H 1.3282 0.5309 0.8984 0.073 Uiso 1 calc R . . C3 C 1.0645(7) 0.7939(7) 0.8863(5) 0.086(2) Uani 1 d . . . H3 H 1.0257 0.8569 0.8439 0.103 Uiso 1 calc R . . H3A H 1.0852 0.8078 0.9436 0.103 Uiso 1 calc R . . H3B H 1.0036 0.7355 0.9043 0.103 Uiso 1 calc R . . C4 C 1.2763(7) 0.8592(5) 0.8128(5) 0.0761(19) Uani 1 d . . . H4 H 1.2421 0.9196 0.7643 0.091 Uiso 1 calc R . . H4A H 1.3620 0.8409 0.7888 0.091 Uiso 1 calc R . . H4B H 1.2828 0.8772 0.8706 0.091 Uiso 1 calc R . . C5 C 1.3466(5) 0.5701(5) 0.6997(4) 0.0567(14) Uani 1 d . . . H5 H 1.4063 0.6294 0.6745 0.068 Uiso 1 calc R . . H5A H 1.3041 0.5611 0.6474 0.068 Uiso 1 calc R . . H5B H 1.3945 0.5059 0.7301 0.068 Uiso 1 calc R . . C6 C 1.1542(6) 0.5017(4) 0.8091(5) 0.0684(17) Uani 1 d . . . H6 H 1.0896 0.5166 0.8557 0.082 Uiso 1 calc R . . H6A H 1.2005 0.4367 0.8398 0.082 Uiso 1 calc R . . H6B H 1.1113 0.4934 0.7567 0.082 Uiso 1 calc R . . C7 C 0.9793(4) 0.7339(3) 0.5897(3) 0.0286(8) Uani 1 d . . . C8 C 0.9612(4) 0.8428(3) 0.6047(3) 0.0277(8) Uani 1 d . . . C9 C 0.8915(4) 0.6023(3) 0.5359(4) 0.0396(10) Uani 1 d . . . H9 H 0.8662 0.5508 0.5994 0.048 Uiso 1 calc R . . H9A H 0.9803 0.5850 0.5150 0.048 Uiso 1 calc R . . C10 C 0.8006(5) 0.5931(4) 0.4658(4) 0.0518(13) Uani 1 d . . . H10 H 0.8050 0.5199 0.4646 0.062 Uiso 1 calc R . . H10A H 0.8330 0.6393 0.4015 0.062 Uiso 1 calc R . . C11 C 0.6562(5) 0.6212(4) 0.4851(4) 0.0457(11) Uani 1 d . . . H11 H 0.6038 0.5991 0.4435 0.055 Uiso 1 calc R . . H11A H 0.6248 0.5831 0.5521 0.055 Uiso 1 calc R . . C12 C 0.5498(4) 0.7898(3) 0.4187(3) 0.0297(8) Uani 1 d . . . C13 C 0.5598(4) 0.9118(3) 0.3957(3) 0.0287(8) Uani 1 d . . . C14 C 0.2237(7) 0.8265(6) 0.1573(5) 0.0754(19) Uani 1 d . . . H14 H 0.2496 0.7953 0.1066 0.090 Uiso 1 calc R . . H14A H 0.1287 0.8207 0.1707 0.090 Uiso 1 calc R . . C15 C 0.2555(16) 0.9312(8) 0.1235(9) 0.104(8) Uani 1 d . . . H15 H 0.1757 0.9703 0.1027 0.245 Uiso 1 calc R . . H15A H 0.3156 0.9413 0.0654 0.245 Uiso 1 calc R . . C16 C 0.3930(8) 0.6856(7) 0.2250(7) 0.111(3) Uani 1 d . . . H16 H 0.4295 0.6452 0.2841 0.133 Uiso 1 calc R . . H16A H 0.4611 0.7270 0.1794 0.133 Uiso 1 calc R . . H16B H 0.3559 0.6373 0.1980 0.133 Uiso 1 calc R . . C17 C 0.1788(7) 0.6986(6) 0.3191(6) 0.088(2) Uani 1 d . . . H17 H 0.2166 0.6553 0.3766 0.105 Uiso 1 calc R . . H17A H 0.1368 0.6531 0.2915 0.105 Uiso 1 calc R . . H17B H 0.1149 0.7467 0.3356 0.105 Uiso 1 calc R . . C18 C 0.4191(8) 1.0432(9) 0.1166(6) 0.127(4) Uani 1 d . . . H18 H 0.4559 1.0873 0.1481 0.152 Uiso 1 calc R . . H18A H 0.3887 1.0879 0.0566 0.152 Uiso 1 calc R . . H18B H 0.4851 0.9945 0.1037 0.152 Uiso 1 calc R . . C19 C 0.2179(8) 1.0616(7) 0.1979(6) 0.101(3) Uani 1 d . . . H19 H 0.2521 1.0922 0.2416 0.121 Uiso 1 calc R . . H19A H 0.1356 1.0271 0.2267 0.121 Uiso 1 calc R . . H19B H 0.2046 1.1173 0.1381 0.121 Uiso 1 calc R . . O7 O 1.3196(3) 0.8318(2) 0.5988(2) 0.0417(7) Uani 1 d . . . O8 O 0.1989(3) 0.8865(3) 0.4144(3) 0.0504(8) Uani 1 d . . . O9 O 0.5836(4) 0.8219(3) 0.6440(3) 0.0557(9) Uani 1 d . . . P1 P 0.26284(13) 0.40892(11) 0.15487(10) 0.0476(3) Uani 1 d . . . F1 F 0.3662(4) 0.4964(3) 0.0957(3) 0.0756(10) Uani 1 d . . . F2 F 0.3629(4) 0.3197(3) 0.1430(3) 0.0856(11) Uani 1 d . . . F3 F 0.1633(4) 0.3184(3) 0.2177(3) 0.0737(10) Uani 1 d . . . F4 F 0.1712(4) 0.4988(3) 0.1756(3) 0.0875(12) Uani 1 d . . . F5 F 0.1969(4) 0.4131(3) 0.0637(3) 0.0833(11) Uani 1 d . . . F6 F 0.3315(4) 0.4060(3) 0.2484(3) 0.0773(10) Uani 1 d . . . P2 P 1.20557(14) 0.16912(12) 0.83910(11) 0.0528(3) Uani 1 d . . . F7 F 1.2809(4) 0.2746(3) 0.7683(3) 0.0866(11) Uani 1 d . . . F8 F 1.3251(5) 0.1100(4) 0.8048(4) 0.1147(16) Uani 1 d . . . F9 F 1.0827(4) 0.2438(4) 0.8412(4) 0.1097(15) Uani 1 d . . . F10 F 1.1286(5) 0.0701(3) 0.8974(3) 0.1003(14) Uani 1 d . . . F11 F 1.1478(5) 0.1518(4) 0.7518(3) 0.1079(15) Uani 1 d . . . F12 F 1.2720(5) 0.1927(4) 0.9180(3) 0.1120(16) Uani 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 0.0291(3) 0.0272(2) 0.0331(3) -0.0095(2) -0.0097(2) 0.00314(18) Cu2 0.0312(3) 0.0260(2) 0.0370(3) -0.0101(2) -0.0130(2) 0.00374(19) Cu3 0.0325(3) 0.0307(3) 0.0377(3) -0.0101(2) -0.0120(2) 0.0022(2) O1 0.0326(15) 0.0329(15) 0.0436(18) -0.0154(14) -0.0137(13) 0.0061(12) O2 0.0291(14) 0.0302(14) 0.0402(17) -0.0131(13) -0.0113(12) 0.0032(11) O3 0.0332(15) 0.0270(14) 0.0388(16) -0.0102(13) -0.0131(13) 0.0044(11) O4 0.0354(15) 0.0299(14) 0.0388(17) -0.0099(13) -0.0102(13) 0.0012(12) O5 0.0379(16) 0.0346(16) 0.0479(19) -0.0119(14) -0.0156(14) 0.0020(13) O6 0.0346(15) 0.0300(14) 0.0406(17) -0.0102(13) -0.0132(13) 0.0028(12) N1 0.0372(19) 0.0352(19) 0.037(2) -0.0105(16) -0.0115(16) 0.0008(15) N2 0.0378(19) 0.0338(19) 0.041(2) -0.0116(17) -0.0095(17) 0.0035(15) N3 0.0337(18) 0.0259(16) 0.0352(19) -0.0114(15) -0.0101(15) 0.0022(13) N4 0.0330(19) 0.0321(18) 0.044(2) -0.0121(16) -0.0088(16) 0.0012(15) N5 0.051(2) 0.048(2) 0.062(3) -0.020(2) -0.018(2) 0.001(2) N6 0.038(2) 0.042(2) 0.038(2) -0.0106(17) -0.0112(17) 0.0028(16) C1 0.103(5) 0.068(4) 0.072(4) -0.021(4) -0.039(4) 0.021(4) C2 0.062(3) 0.057(3) 0.067(4) -0.020(3) -0.026(3) 0.018(3) C3 0.071(4) 0.120(6) 0.075(5) -0.043(5) -0.003(4) -0.003(4) C4 0.096(5) 0.072(4) 0.067(4) -0.030(4) -0.008(4) -0.021(4) C5 0.056(3) 0.055(3) 0.064(4) -0.026(3) -0.009(3) 0.011(3) C6 0.061(4) 0.046(3) 0.088(5) -0.006(3) -0.016(3) 0.002(3) C7 0.029(2) 0.0267(19) 0.031(2) -0.0104(17) -0.0050(17) 0.0025(15) C8 0.0276(19) 0.0251(18) 0.030(2) -0.0080(16) -0.0044(16) -0.0009(15) C9 0.041(2) 0.033(2) 0.050(3) -0.019(2) -0.015(2) 0.0071(18) C10 0.052(3) 0.042(3) 0.068(4) -0.024(3) -0.020(3) 0.006(2) C11 0.045(3) 0.031(2) 0.062(3) -0.014(2) -0.016(2) 0.0017(19) C12 0.030(2) 0.0272(19) 0.032(2) -0.0083(17) -0.0063(17) 0.0017(15) C13 0.030(2) 0.0247(19) 0.031(2) -0.0074(16) -0.0055(17) 0.0005(15) C14 0.080(4) 0.076(4) 0.081(5) -0.032(4) -0.036(4) 0.001(4) C15 0.15(2) 0.094(7) 0.172(12) -0.001(8) -0.056(14) -0.038(10) C16 0.102(6) 0.103(6) 0.159(9) -0.079(7) -0.040(6) 0.014(5) C17 0.095(5) 0.073(5) 0.093(5) -0.021(4) -0.018(4) -0.025(4) C18 0.091(6) 0.166(9) 0.081(6) 0.017(6) -0.012(5) 0.031(6) C19 0.114(6) 0.094(6) 0.073(5) -0.002(4) -0.008(5) 0.041(5) O7 0.0417(17) 0.0383(17) 0.0432(18) -0.0100(15) -0.0065(14) 0.0001(13) O8 0.0449(19) 0.054(2) 0.048(2) -0.0105(17) -0.0059(16) -0.0009(16) O9 0.058(2) 0.052(2) 0.056(2) -0.0161(18) -0.0072(18) 0.0026(17) P1 0.0464(7) 0.0458(7) 0.0467(7) -0.0085(6) -0.0075(6) -0.0023(6) F1 0.077(2) 0.069(2) 0.073(2) -0.0103(19) -0.0051(19) -0.0202(18) F2 0.082(3) 0.070(2) 0.108(3) -0.035(2) -0.006(2) 0.010(2) F3 0.082(2) 0.070(2) 0.061(2) -0.0124(18) 0.0035(19) -0.0192(19) F4 0.065(2) 0.076(2) 0.131(4) -0.045(3) -0.016(2) 0.0108(19) F5 0.096(3) 0.090(3) 0.060(2) -0.012(2) -0.020(2) -0.019(2) F6 0.085(3) 0.084(3) 0.065(2) -0.023(2) -0.021(2) 0.000(2) P2 0.0520(8) 0.0550(8) 0.0532(8) -0.0192(7) -0.0094(7) 0.0030(6) F7 0.095(3) 0.080(3) 0.081(3) -0.025(2) 0.005(2) -0.008(2) F8 0.095(3) 0.090(3) 0.160(5) -0.048(3) -0.003(3) 0.017(3) F9 0.076(3) 0.093(3) 0.164(5) -0.048(3) -0.014(3) 0.011(2) F10 0.121(4) 0.080(3) 0.088(3) -0.013(2) 0.004(3) -0.019(3) F11 0.123(4) 0.122(4) 0.086(3) -0.040(3) -0.023(3) -0.012(3) F12 0.144(4) 0.114(4) 0.080(3) -0.025(3) -0.033(3) -0.018(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.953(3) . ? Cu1 N1 2.015(4) . ? Cu1 N2 2.026(4) . ? Cu1 O2 2.026(3) . ? Cu1 O7 2.388(3) . ? Cu2 N3 1.929(3) . ? Cu2 N4 1.933(3) . ? Cu2 O3 2.014(3) . ? Cu2 O4 2.040(3) . ? Cu3 O5 1.935(3) . ? Cu3 N6 2.004(4) . ? Cu3 N5 2.027(4) . ? Cu3 O6 2.052(3) . ? Cu3 O8 2.323(3) . ? O1 C7 1.266(5) . ? O2 C8 1.266(4) . ? O3 C8 1.264(5) . ? O4 C13 1.236(5) . ? O5 C12 1.264(5) . ? O6 C13 1.275(5) . ? N1 C1 1.470(7) . ? N1 C3 1.479(7) . ? N1 C4 1.494(7) . ? N2 C5 1.456(6) . ? N2 C6 1.472(6) . ? N2 C2 1.489(6) . ? N3 C7 1.287(5) . ? N3 C9 1.483(5) . ? N4 C12 1.270(5) . ? N4 C11 1.475(5) . ? N5 C17 1.492(8) . ? N5 C14 1.497(8) . ? N5 C16 1.547(8) . ? N6 C15 1.388(10) . ? N6 C18 1.434(9) . ? N6 C19 1.450(8) . ? C1 C2 1.508(8) . ? C1 H1 0.9700 . ? C1 H1A 0.9700 . ? C2 H2 0.9700 . ? C2 H2A 0.9700 . ? C3 H3 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C4 H4 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C5 H5 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C6 H6 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C7 C8 1.523(5) . ? C9 C10 1.492(6) . ? C9 H9 0.9700 . ? C9 H9A 0.9700 . ? C10 C11 1.527(7) . ? C10 H10 0.9700 . ? C10 H10A 0.9700 . ? C11 H11 0.9700 . ? C11 H11A 0.9700 . ? C12 C13 1.537(5) . ? C14 C15 1.345(11) . ? C14 H14 0.9700 . ? C14 H14A 0.9700 . ? C15 H15 0.9700 . ? C15 H15A 0.9700 . ? C16 H16 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C17 H17 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C18 H18 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C19 H19 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? P1 F5 1.542(4) . ? P1 F1 1.563(3) . ? P1 F4 1.569(4) . ? P1 F2 1.569(4) . ? P1 F3 1.576(3) . ? P1 F6 1.592(4) . ? P2 F10 1.503(4) . ? P2 F12 1.520(5) . ? P2 F11 1.547(4) . ? P2 F8 1.550(5) . ? P2 F9 1.569(4) . ? P2 F7 1.604(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 O1 Cu1 N1 164.27(14) . . ? O1 Cu1 N2 90.93(13) . . ? N1 Cu1 N2 87.27(15) . . ? O1 Cu1 O2 83.97(11) . . ? N1 Cu1 O2 96.47(13) . . ? N2 Cu1 O2 173.30(13) . . ? O1 Cu1 O7 93.87(12) . . ? N1 Cu1 O7 101.83(13) . . ? N2 Cu1 O7 100.13(13) . . ? O2 Cu1 O7 84.58(11) . . ? N3 Cu2 N4 95.11(14) . . ? N3 Cu2 O3 84.06(12) . . ? N4 Cu2 O3 170.70(14) . . ? N3 Cu2 O4 167.19(13) . . ? N4 Cu2 O4 83.23(13) . . ? O3 Cu2 O4 99.60(11) . . ? O5 Cu3 N6 164.54(15) . . ? O5 Cu3 N5 91.02(15) . . ? N6 Cu3 N5 86.98(17) . . ? O5 Cu3 O6 83.62(12) . . ? N6 Cu3 O6 95.68(13) . . ? N5 Cu3 O6 169.19(15) . . ? O5 Cu3 O8 94.04(13) . . ? N6 Cu3 O8 101.36(14) . . ? N5 Cu3 O8 102.42(16) . . ? O6 Cu3 O8 87.36(12) . . ? C7 O1 Cu1 110.5(2) . . ? C8 O2 Cu1 110.1(2) . . ? C8 O3 Cu2 109.6(2) . . ? C13 O4 Cu2 109.4(2) . . ? C12 O5 Cu3 112.5(3) . . ? C13 O6 Cu3 110.1(2) . . ? C1 N1 C3 104.7(5) . . ? C1 N1 C4 112.6(5) . . ? C3 N1 C4 105.9(5) . . ? C1 N1 Cu1 108.9(3) . . ? C3 N1 Cu1 112.2(3) . . ? C4 N1 Cu1 112.4(3) . . ? C5 N2 C6 110.3(4) . . ? C5 N2 C2 109.3(4) . . ? C6 N2 C2 108.5(4) . . ? C5 N2 Cu1 112.3(3) . . ? C6 N2 Cu1 110.4(3) . . ? C2 N2 Cu1 105.8(3) . . ? C7 N3 C9 117.2(3) . . ? C7 N3 Cu2 114.1(3) . . ? C9 N3 Cu2 128.5(3) . . ? C12 N4 C11 120.6(4) . . ? C12 N4 Cu2 114.9(3) . . ? C11 N4 Cu2 124.4(3) . . ? C17 N5 C14 108.5(5) . . ? C17 N5 C16 110.1(5) . . ? C14 N5 C16 111.7(6) . . ? C17 N5 Cu3 110.5(4) . . ? C14 N5 Cu3 106.0(3) . . ? C16 N5 Cu3 110.0(4) . . ? C15 N6 C18 105.4(8) . . ? C15 N6 C19 109.4(8) . . ? C18 N6 C19 106.3(6) . . ? C15 N6 Cu3 106.8(5) . . ? C18 N6 Cu3 114.2(4) . . ? C19 N6 Cu3 114.4(4) . . ? N1 C1 C2 109.6(5) . . ? N1 C1 H1 109.8 . . ? C2 C1 H1 109.8 . . ? N1 C1 H1A 109.8 . . ? C2 C1 H1A 109.8 . . ? H1 C1 H1A 108.2 . . ? N2 C2 C1 112.9(5) . . ? N2 C2 H2 109.0 . . ? C1 C2 H2 109.0 . . ? N2 C2 H2A 109.0 . . ? C1 C2 H2A 109.0 . . ? H2 C2 H2A 107.8 . . ? N1 C3 H3 109.5 . . ? N1 C3 H3A 109.5 . . ? H3 C3 H3A 109.5 . . ? N1 C3 H3B 109.5 . . ? H3 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N1 C4 H4 109.5 . . ? N1 C4 H4A 109.5 . . ? H4 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N2 C5 H5 109.5 . . ? N2 C5 H5A 109.5 . . ? H5 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C6 H6 109.5 . . ? N2 C6 H6A 109.5 . . ? H6 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? H6 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? O1 C7 N3 128.5(3) . . ? O1 C7 C8 117.7(3) . . ? N3 C7 C8 113.8(3) . . ? O3 C8 O2 126.2(3) . . ? O3 C8 C7 118.1(3) . . ? O2 C8 C7 115.6(3) . . ? N3 C9 C10 112.0(4) . . ? N3 C9 H9 109.2 . . ? C10 C9 H9 109.2 . . ? N3 C9 H9A 109.2 . . ? C10 C9 H9A 109.2 . . ? H9 C9 H9A 107.9 . . ? C9 C10 C11 116.8(4) . . ? C9 C10 H10 108.1 . . ? C11 C10 H10 108.1 . . ? C9 C10 H10A 108.1 . . ? C11 C10 H10A 108.1 . . ? H10 C10 H10A 107.3 . . ? N4 C11 C10 109.8(4) . . ? N4 C11 H11 109.7 . . ? C10 C11 H11 109.7 . . ? N4 C11 H11A 109.7 . . ? C10 C11 H11A 109.7 . . ? H11 C11 H11A 108.2 . . ? O5 C12 N4 129.5(4) . . ? O5 C12 C13 117.3(3) . . ? N4 C12 C13 113.2(3) . . ? O4 C13 O6 126.0(4) . . ? O4 C13 C12 118.9(4) . . ? O6 C13 C12 115.1(3) . . ? C15 C14 N5 115.3(6) . . ? C15 C14 H14 108.5 . . ? N5 C14 H14 108.5 . . ? C15 C14 H14A 108.5 . . ? N5 C14 H14A 108.5 . . ? H14 C14 H14A 107.5 . . ? C14 C15 N6 123.2(9) . . ? C14 C15 H15 106.5 . . ? N6 C15 H15 106.5 . . ? C14 C15 H15A 106.5 . . ? N6 C15 H15A 106.5 . . ? H15 C15 H15A 106.5 . . ? N5 C16 H16 109.5 . . ? N5 C16 H16A 109.5 . . ? H16 C16 H16A 109.5 . . ? N5 C16 H16B 109.5 . . ? H16 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N5 C17 H17 109.5 . . ? N5 C17 H17A 109.5 . . ? H17 C17 H17A 109.5 . . ? N5 C17 H17B 109.5 . . ? H17 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N6 C18 H18 109.5 . . ? N6 C18 H18A 109.5 . . ? H18 C18 H18A 109.5 . . ? N6 C18 H18B 109.5 . . ? H18 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N6 C19 H19 109.5 . . ? N6 C19 H19A 109.5 . . ? H19 C19 H19A 109.5 . . ? N6 C19 H19B 109.5 . . ? H19 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? F5 P1 F1 93.0(2) . . ? F5 P1 F4 93.3(2) . . ? F1 P1 F4 89.5(2) . . ? F5 P1 F2 92.6(2) . . ? F1 P1 F2 89.4(2) . . ? F4 P1 F2 174.0(2) . . ? F5 P1 F3 89.1(2) . . ? F1 P1 F3 177.5(2) . . ? F4 P1 F3 91.7(2) . . ? F2 P1 F3 89.2(2) . . ? F5 P1 F6 179.4(2) . . ? F1 P1 F6 86.4(2) . . ? F4 P1 F6 86.4(2) . . ? F2 P1 F6 87.6(2) . . ? F3 P1 F6 91.5(2) . . ? F10 P2 F12 101.1(3) . . ? F10 P2 F11 84.0(3) . . ? F12 P2 F11 174.7(3) . . ? F10 P2 F8 96.5(3) . . ? F12 P2 F8 95.6(3) . . ? F11 P2 F8 82.0(3) . . ? F10 P2 F9 92.2(3) . . ? F12 P2 F9 96.7(3) . . ? F11 P2 F9 84.8(3) . . ? F8 P2 F9 163.3(3) . . ? F10 P2 F7 174.6(3) . . ? F12 P2 F7 84.3(2) . . ? F11 P2 F7 90.7(2) . . ? F8 P2 F7 83.5(3) . . ? F9 P2 F7 86.5(2) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.795 _refine_diff_density_min -0.564 _refine_diff_density_rms 0.099 data_complex_2_at_293_K _database_code_CSD 169869 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H44 Cl Cu3 N7 O13 Se' _chemical_formula_weight 895.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.4380(13) _cell_length_b 14.4721(14) _cell_length_c 19.130(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3443.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour Green _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.728 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1820 _exptl_absorpt_coefficient_mu 3.037 _exptl_absorpt_correction_type Semi-empirical _exptl_absorpt_correction_T_min 0.3120 _exptl_absorpt_correction_T_max 0.5173 _exptl_absorpt_process_details Sadabs _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_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_% 0.5 _diffrn_reflns_number 26835 _diffrn_reflns_av_R_equivalents 0.0587 _diffrn_reflns_av_sigmaI/netI 0.0680 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 30.52 _reflns_number_total 9939 _reflns_number_gt 6222 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _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 w=1/[\s^2^(Fo^2^)+(0.0331P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.019(9) _refine_ls_number_reflns 9939 _refine_ls_number_parameters 406 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0745 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0756 _refine_ls_wR_factor_gt 0.0674 _refine_ls_goodness_of_fit_ref 0.910 _refine_ls_restrained_S_all 0.939 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Se Se 0.83490(3) 0.64178(3) 0.61793(2) 0.06365(12) Uani 1 d . . . Cu1 Cu 0.16995(3) 0.58005(3) 1.12199(2) 0.04400(10) Uani 1 d . . . Cu2 Cu 0.52764(3) 0.46689(3) 1.01356(2) 0.04322(11) Uani 1 d . . . Cu3 Cu 0.82320(3) 0.42571(3) 0.82286(2) 0.04623(11) Uani 1 d . . . O1 O 0.22516(16) 0.46430(17) 1.08028(12) 0.0434(5) Uani 1 d . . . O2 O 0.32617(17) 0.61646(15) 1.12293(12) 0.0457(5) Uani 1 d . . . O3 O 0.47841(18) 0.57046(17) 1.07458(12) 0.0472(6) Uani 1 d . . . O4 O 0.66148(18) 0.53093(17) 0.98202(12) 0.0489(5) Uani 1 d . . . O5 O 0.68668(18) 0.36515(16) 0.84948(12) 0.0472(6) Uani 1 d . . . O6 O 0.78916(19) 0.51283(19) 0.90277(14) 0.0614(8) Uani 1 d . . . O7 O 0.1514(2) 0.6432(2) 1.01069(15) 0.0749(8) Uani 1 d . . . O8 O 0.7941(3) 0.6878(2) 0.0187(2) 0.0954(10) Uani 1 d . . . O9 O 0.9857(3) 0.7314(3) 0.95483(19) 0.0957(11) Uani 1 d . . . N1 N 0.1254(2) 0.6895(2) 1.17791(15) 0.0431(7) Uani 1 d . . . N2 N 0.0240(2) 0.5258(2) 1.14113(15) 0.0471(7) Uani 1 d . . . N3 N 0.38571(19) 0.41543(19) 1.03131(13) 0.0348(6) Uani 1 d . . . N4 N 0.5633(2) 0.37972(18) 0.94019(14) 0.0391(6) Uani 1 d . . . N5 N 0.8717(2) 0.3150(2) 0.76490(14) 0.0420(7) Uani 1 d . . . N6 N 0.9801(2) 0.4624(2) 0.82689(15) 0.0455(7) Uani 1 d . . . N7 N 0.7764(3) 0.5242(3) 0.7383(2) 0.0669(9) Uani 1 d . . . C1 C 0.0102(3) 0.6735(3) 1.1949(3) 0.0760(14) Uani 1 d . . . H1 H -0.0020 0.6957 1.2421 0.091 Uiso 1 calc R . . H1A H -0.0324 0.7119 1.1639 0.091 Uiso 1 calc R . . C2 C -0.0276(4) 0.5897(4) 1.1912(4) 0.122(2) Uani 1 d . . . H2 H -0.1033 0.5937 1.1795 0.146 Uiso 1 calc R . . H2A H -0.0227 0.5623 1.2374 0.146 Uiso 1 calc R . . C3 C 0.1898(3) 0.7018(3) 1.2409(2) 0.0667(12) Uani 1 d . . . H3 H 0.1851 0.6472 1.2693 0.080 Uiso 1 calc R . . H3A H 0.1633 0.7539 1.2668 0.080 Uiso 1 calc R . . H3B H 0.2634 0.7124 1.2282 0.080 Uiso 1 calc R . . C4 C 0.1392(4) 0.7745(3) 1.1379(3) 0.0875(16) Uani 1 d . . . H4 H 0.0990 0.7704 1.0951 0.105 Uiso 1 calc R . . H4A H 0.2140 0.7831 1.1273 0.105 Uiso 1 calc R . . H4B H 0.1137 0.8260 1.1648 0.105 Uiso 1 calc R . . C5 C -0.0351(4) 0.5077(4) 1.0760(3) 0.0853(15) Uani 1 d . . . H5 H -0.0432 0.5643 1.0504 0.102 Uiso 1 calc R . . H5A H -0.1047 0.4831 1.0869 0.102 Uiso 1 calc R . . H5B H 0.0041 0.4639 1.0482 0.102 Uiso 1 calc R . . C6 C 0.0307(4) 0.4371(3) 1.1765(2) 0.0757(13) Uani 1 d . . . H6 H 0.0666 0.4447 1.2205 0.091 Uiso 1 calc R . . H6A H 0.0702 0.3944 1.1479 0.091 Uiso 1 calc R . . H6B H -0.0405 0.4136 1.1843 0.091 Uiso 1 calc R . . C7 C 0.3247(2) 0.4712(2) 1.06507(16) 0.0360(7) Uani 1 d . . . C8 C 0.3813(2) 0.5588(2) 1.08860(15) 0.0315(7) Uani 1 d . . . C9 C 0.3410(3) 0.3319(2) 1.00074(16) 0.0406(8) Uani 1 d . . . H9 H 0.2978 0.3482 0.9604 0.049 Uiso 1 calc R . . H9A H 0.2944 0.3021 1.0346 0.049 Uiso 1 calc R . . C10 C 0.4277(3) 0.2654(3) 0.9788(2) 0.0545(10) Uani 1 d . . . H10 H 0.3938 0.2085 0.9636 0.065 Uiso 1 calc R . . H10A H 0.4713 0.2509 1.0194 0.065 Uiso 1 calc R . . C11 C 0.5023(3) 0.2992(2) 0.92027(18) 0.0457(9) Uani 1 d . . . H11 H 0.5515 0.2499 0.9078 0.055 Uiso 1 calc R . . H11A H 0.4595 0.3137 0.8793 0.055 Uiso 1 calc R . . C12 C 0.6462(2) 0.4043(2) 0.90402(18) 0.0415(8) Uani 1 d . . . C13 C 0.7023(2) 0.4892(2) 0.93148(18) 0.0397(8) Uani 1 d . . . C14 C 0.9909(3) 0.3247(3) 0.7560(2) 0.0529(10) Uani 1 d . . . H14 H 1.0272 0.2885 0.7915 0.063 Uiso 1 calc R . . H14A H 1.0115 0.3006 0.7106 0.063 Uiso 1 calc R . . C15 C 1.0250(3) 0.4210(3) 0.7614(2) 0.0555(10) Uani 1 d . . . H15 H 0.9996 0.4554 0.7211 0.067 Uiso 1 calc R . . H15A H 1.1028 0.4243 0.7623 0.067 Uiso 1 calc R . . C16 C 0.8498(4) 0.2265(3) 0.8004(3) 0.0761(13) Uani 1 d . . . H16 H 0.8821 0.2271 0.8460 0.091 Uiso 1 calc R . . H16A H 0.8796 0.1767 0.7734 0.091 Uiso 1 calc R . . H16B H 0.7736 0.2180 0.8048 0.091 Uiso 1 calc R . . C17 C 0.8216(3) 0.3164(3) 0.6957(2) 0.0647(11) Uani 1 d . . . H17 H 0.8372 0.3741 0.6731 0.078 Uiso 1 calc R . . H17A H 0.7452 0.3094 0.7005 0.078 Uiso 1 calc R . . H17B H 0.8497 0.2665 0.6681 0.078 Uiso 1 calc R . . C18 C 1.0294(4) 0.4268(4) 0.8899(3) 0.0971(16) Uani 1 d . . . H18 H 1.0216 0.3608 0.8912 0.117 Uiso 1 calc R . . H18A H 0.9948 0.4534 0.9300 0.117 Uiso 1 calc R . . H18B H 1.1043 0.4425 0.8903 0.117 Uiso 1 calc R . . C19 C 0.9960(3) 0.5647(3) 0.8261(2) 0.0685(12) Uani 1 d . . . H19 H 0.9646 0.5901 0.7845 0.082 Uiso 1 calc R . . H19A H 1.0715 0.5784 0.8270 0.082 Uiso 1 calc R . . H19B H 0.9620 0.5914 0.8664 0.082 Uiso 1 calc R . . C20 C 0.8001(3) 0.5693(3) 0.6920(2) 0.0513(9) Uani 1 d . . . Cl Cl 0.84449(9) 0.93020(9) 0.13014(6) 0.0715(3) Uani 1 d D . . O11 O 0.9441(3) 0.9667(3) 0.1277(2) 0.1326(15) Uani 1 d D . . O12 O 0.7788(4) 0.9367(4) 0.0755(2) 0.156(2) Uani 1 d D . . O13 O 0.8467(4) 0.8475(3) 0.1667(3) 0.1354(15) Uani 1 d D . . O14 O 0.7931(3) 0.9870(3) 0.1855(3) 0.157(2) Uani 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 Se 0.0661(2) 0.0626(3) 0.0622(2) 0.0019(2) 0.0032(2) 0.0019(2) Cu1 0.03730(19) 0.0446(2) 0.0501(2) -0.0104(2) 0.0041(2) 0.0001(2) Cu2 0.0401(2) 0.0423(2) 0.0472(2) -0.0110(2) 0.00937(18) -0.0041(2) Cu3 0.0433(2) 0.0473(3) 0.0480(2) -0.0075(2) 0.0097(2) -0.0037(2) O1 0.0365(11) 0.0421(13) 0.0515(14) -0.0080(12) 0.0059(10) -0.0022(11) O2 0.0391(11) 0.0462(13) 0.0518(13) -0.0118(12) 0.0075(12) 0.0017(11) O3 0.0406(12) 0.0479(14) 0.0532(14) -0.0145(12) 0.0068(11) -0.0039(12) O4 0.0470(12) 0.0464(13) 0.0532(13) -0.0123(13) 0.0123(12) -0.0069(13) O5 0.0450(13) 0.0482(15) 0.0482(13) -0.0112(12) 0.0088(11) -0.0015(12) O6 0.0553(14) 0.0581(18) 0.0707(19) -0.0173(14) 0.0178(13) -0.0106(14) O7 0.0792(19) 0.080(2) 0.0654(18) 0.0056(17) -0.0019(15) 0.0093(17) O8 0.096(2) 0.083(2) 0.107(3) -0.004(2) -0.013(2) -0.005(2) O9 0.098(2) 0.086(2) 0.103(3) -0.002(2) -0.011(2) 0.012(2) N1 0.0380(14) 0.0455(18) 0.0459(16) -0.0051(15) 0.0038(13) 0.0028(12) N2 0.0397(14) 0.0472(18) 0.0544(18) -0.0034(15) 0.0057(13) 0.0005(15) N3 0.0343(12) 0.0326(15) 0.0376(15) -0.0047(12) 0.0018(11) -0.0012(12) N4 0.0356(14) 0.0352(15) 0.0467(16) -0.0048(13) 0.0079(12) -0.0035(12) N5 0.0387(14) 0.0469(18) 0.0402(16) -0.0017(14) 0.0057(12) -0.0022(13) N6 0.0447(15) 0.0492(18) 0.0426(16) -0.0011(15) 0.0032(13) -0.0029(14) N7 0.066(2) 0.064(2) 0.071(2) -0.001(2) -0.0020(18) 0.003(2) C1 0.051(2) 0.078(4) 0.098(4) -0.024(3) 0.018(2) -0.002(2) C2 0.086(4) 0.094(5) 0.185(7) -0.041(5) 0.063(4) -0.015(4) C3 0.065(3) 0.076(3) 0.059(3) -0.018(2) 0.004(2) 0.004(2) C4 0.104(4) 0.071(3) 0.088(4) -0.001(3) 0.007(3) 0.009(3) C5 0.085(3) 0.090(4) 0.081(3) 0.017(3) -0.015(3) -0.015(3) C6 0.082(3) 0.074(3) 0.071(3) 0.002(3) 0.002(3) -0.007(3) C7 0.0338(14) 0.0360(17) 0.0382(16) -0.0013(15) -0.0017(14) 0.0031(17) C8 0.0307(14) 0.0290(18) 0.0347(16) -0.0078(13) 0.0010(13) 0.0029(13) C9 0.0407(17) 0.0385(18) 0.0425(19) -0.0080(14) 0.0026(15) -0.0025(15) C10 0.054(2) 0.047(2) 0.063(3) -0.003(2) 0.003(2) -0.0026(18) C11 0.054(2) 0.039(2) 0.044(2) -0.0106(17) 0.0132(16) -0.0065(16) C12 0.0406(17) 0.040(2) 0.0436(19) -0.0030(16) 0.0044(15) -0.0003(15) C13 0.0366(16) 0.041(2) 0.0419(19) -0.0101(16) 0.0076(14) -0.0040(15) C14 0.0419(18) 0.059(3) 0.058(2) -0.0074(19) 0.0059(16) 0.0049(18) C15 0.0469(19) 0.064(3) 0.056(2) -0.004(2) 0.0095(18) 0.006(2) C16 0.080(3) 0.067(3) 0.081(3) -0.008(3) 0.011(3) 0.002(2) C17 0.068(2) 0.063(3) 0.063(3) -0.006(2) -0.004(2) 0.000(2) C18 0.093(3) 0.115(4) 0.084(4) 0.011(3) -0.010(3) -0.012(4) C19 0.068(3) 0.065(3) 0.072(3) -0.004(2) 0.000(2) -0.011(2) C20 0.0437(19) 0.054(2) 0.056(2) -0.002(2) -0.0016(17) 0.0023(18) Cl 0.0646(6) 0.0727(8) 0.0771(7) 0.0155(6) -0.0091(6) -0.0069(6) O11 0.108(3) 0.157(4) 0.133(4) 0.034(3) -0.007(3) -0.023(3) O12 0.142(4) 0.205(6) 0.120(4) 0.042(4) -0.007(3) -0.024(4) O13 0.128(3) 0.117(3) 0.161(4) 0.032(3) -0.004(3) -0.012(3) O14 0.110(3) 0.162(5) 0.200(5) -0.068(5) -0.022(3) 0.019(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Se C20 1.815(4) . ? Cu1 O1 1.978(2) . ? Cu1 N1 1.990(3) . ? Cu1 N2 2.011(3) . ? Cu1 O2 2.013(2) . ? Cu1 O7 2.328(3) . ? Cu2 N4 1.939(3) . ? Cu2 N3 1.946(2) . ? Cu2 O3 1.996(2) . ? Cu2 O4 1.999(2) . ? Cu3 O5 1.978(2) . ? Cu3 N6 2.024(3) . ? Cu3 O6 2.026(3) . ? Cu3 N5 2.040(3) . ? Cu3 N7 2.233(4) . ? O1 C7 1.275(3) . ? O2 C8 1.263(3) . ? O3 C8 1.249(3) . ? O4 C13 1.248(4) . ? O5 C12 1.290(4) . ? O6 C13 1.260(4) . ? N1 C3 1.458(5) . ? N1 C4 1.459(5) . ? N1 C1 1.487(4) . ? N2 C6 1.453(5) . ? N2 C5 1.470(5) . ? N2 C2 1.479(6) . ? N3 C7 1.283(4) . ? N3 C9 1.454(4) . ? N4 C12 1.292(4) . ? N4 C11 1.442(4) . ? N5 C17 1.463(5) . ? N5 C16 1.475(5) . ? N5 C14 1.499(4) . ? N6 C18 1.447(6) . ? N6 C19 1.494(5) . ? N6 C15 1.496(4) . ? N7 C20 1.140(5) . ? C1 C2 1.303(7) . ? C1 H1 0.9700 . ? C1 H1A 0.9700 . ? C2 H2 0.9700 . ? C2 H2A 0.9700 . ? C3 H3 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C4 H4 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C5 H5 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C6 H6 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C7 C8 1.519(4) . ? C9 C10 1.504(5) . ? C9 H9 0.9700 . ? C9 H9A 0.9700 . ? C10 C11 1.533(5) . ? C10 H10 0.9700 . ? C10 H10A 0.9700 . ? C11 H11 0.9700 . ? C11 H11A 0.9700 . ? C12 C13 1.507(4) . ? C14 C15 1.461(6) . ? C14 H14 0.9700 . ? C14 H14A 0.9700 . ? C15 H15 0.9700 . ? C15 H15A 0.9700 . ? C16 H16 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C17 H17 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C18 H18 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C19 H19 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? Cl O12 1.329(4) . ? Cl O11 1.348(4) . ? Cl O13 1.387(4) . ? Cl O14 1.486(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 O1 Cu1 N1 170.87(11) . . ? O1 Cu1 N2 93.22(11) . . ? N1 Cu1 N2 87.80(12) . . ? O1 Cu1 O2 83.70(9) . . ? N1 Cu1 O2 93.18(10) . . ? N2 Cu1 O2 166.29(11) . . ? O1 Cu1 O7 89.88(10) . . ? N1 Cu1 O7 98.72(11) . . ? N2 Cu1 O7 103.30(11) . . ? O2 Cu1 O7 90.08(10) . . ? N4 Cu2 N3 94.86(11) . . ? N4 Cu2 O3 169.18(11) . . ? N3 Cu2 O3 84.67(10) . . ? N4 Cu2 O4 83.84(10) . . ? N3 Cu2 O4 170.35(11) . . ? O3 Cu2 O4 94.81(9) . . ? O5 Cu3 N6 159.13(11) . . ? O5 Cu3 O6 84.38(9) . . ? N6 Cu3 O6 90.54(11) . . ? O5 Cu3 N5 92.63(10) . . ? N6 Cu3 N5 86.66(11) . . ? O6 Cu3 N5 163.88(12) . . ? O5 Cu3 N7 104.20(12) . . ? N6 Cu3 N7 96.41(13) . . ? O6 Cu3 N7 95.42(12) . . ? N5 Cu3 N7 100.66(13) . . ? C7 O1 Cu1 111.3(2) . . ? C8 O2 Cu1 110.25(18) . . ? C8 O3 Cu2 108.7(2) . . ? C13 O4 Cu2 110.4(2) . . ? C12 O5 Cu3 110.4(2) . . ? C13 O6 Cu3 109.8(2) . . ? C3 N1 C4 105.5(3) . . ? C3 N1 C1 111.5(3) . . ? C4 N1 C1 111.1(4) . . ? C3 N1 Cu1 112.9(2) . . ? C4 N1 Cu1 110.9(3) . . ? C1 N1 Cu1 105.2(2) . . ? C6 N2 C5 105.4(3) . . ? C6 N2 C2 106.0(4) . . ? C5 N2 C2 116.3(4) . . ? C6 N2 Cu1 112.2(3) . . ? C5 N2 Cu1 111.5(2) . . ? C2 N2 Cu1 105.4(3) . . ? C7 N3 C9 120.0(3) . . ? C7 N3 Cu2 112.6(2) . . ? C9 N3 Cu2 126.5(2) . . ? C12 N4 C11 120.1(3) . . ? C12 N4 Cu2 113.0(2) . . ? C11 N4 Cu2 126.6(2) . . ? C17 N5 C16 110.4(3) . . ? C17 N5 C14 108.4(3) . . ? C16 N5 C14 108.4(3) . . ? C17 N5 Cu3 110.8(2) . . ? C16 N5 Cu3 112.2(2) . . ? C14 N5 Cu3 106.3(2) . . ? C18 N6 C19 107.8(4) . . ? C18 N6 C15 113.4(3) . . ? C19 N6 C15 109.9(3) . . ? C18 N6 Cu3 110.3(3) . . ? C19 N6 Cu3 112.8(2) . . ? C15 N6 Cu3 102.9(2) . . ? C20 N7 Cu3 149.4(3) . . ? C2 C1 N1 118.7(4) . . ? C2 C1 H1 107.6 . . ? N1 C1 H1 107.6 . . ? C2 C1 H1A 107.6 . . ? N1 C1 H1A 107.6 . . ? H1 C1 H1A 107.1 . . ? C1 C2 N2 117.4(5) . . ? C1 C2 H2 107.9 . . ? N2 C2 H2 107.9 . . ? C1 C2 H2A 107.9 . . ? N2 C2 H2A 107.9 . . ? H2 C2 H2A 107.2 . . ? N1 C3 H3 109.5 . . ? N1 C3 H3A 109.5 . . ? H3 C3 H3A 109.5 . . ? N1 C3 H3B 109.5 . . ? H3 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N1 C4 H4 109.5 . . ? N1 C4 H4A 109.5 . . ? H4 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N2 C5 H5 109.5 . . ? N2 C5 H5A 109.5 . . ? H5 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C6 H6 109.5 . . ? N2 C6 H6A 109.5 . . ? H6 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? H6 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? O1 C7 N3 129.8(3) . . ? O1 C7 C8 116.6(3) . . ? N3 C7 C8 113.6(3) . . ? O3 C8 O2 123.2(3) . . ? O3 C8 C7 119.8(3) . . ? O2 C8 C7 117.0(2) . . ? N3 C9 C10 111.7(3) . . ? N3 C9 H9 109.3 . . ? C10 C9 H9 109.3 . . ? N3 C9 H9A 109.3 . . ? C10 C9 H9A 109.3 . . ? H9 C9 H9A 107.9 . . ? C9 C10 C11 115.7(3) . . ? C9 C10 H10 108.4 . . ? C11 C10 H10 108.4 . . ? C9 C10 H10A 108.4 . . ? C11 C10 H10A 108.4 . . ? H10 C10 H10A 107.4 . . ? N4 C11 C10 112.5(3) . . ? N4 C11 H11 109.1 . . ? C10 C11 H11 109.1 . . ? N4 C11 H11A 109.1 . . ? C10 C11 H11A 109.1 . . ? H11 C11 H11A 107.8 . . ? O5 C12 N4 128.6(3) . . ? O5 C12 C13 117.3(3) . . ? N4 C12 C13 114.1(3) . . ? O4 C13 O6 123.7(3) . . ? O4 C13 C12 118.5(3) . . ? O6 C13 C12 117.8(3) . . ? C15 C14 N5 111.6(3) . . ? C15 C14 H14 109.3 . . ? N5 C14 H14 109.3 . . ? C15 C14 H14A 109.3 . . ? N5 C14 H14A 109.3 . . ? H14 C14 H14A 108.0 . . ? C14 C15 N6 109.5(3) . . ? C14 C15 H15 109.8 . . ? N6 C15 H15 109.8 . . ? C14 C15 H15A 109.8 . . ? N6 C15 H15A 109.8 . . ? H15 C15 H15A 108.2 . . ? N5 C16 H16 109.5 . . ? N5 C16 H16A 109.5 . . ? H16 C16 H16A 109.5 . . ? N5 C16 H16B 109.5 . . ? H16 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N5 C17 H17 109.5 . . ? N5 C17 H17A 109.5 . . ? H17 C17 H17A 109.5 . . ? N5 C17 H17B 109.5 . . ? H17 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N6 C18 H18 109.5 . . ? N6 C18 H18A 109.5 . . ? H18 C18 H18A 109.5 . . ? N6 C18 H18B 109.5 . . ? H18 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N6 C19 H19 109.5 . . ? N6 C19 H19A 109.5 . . ? H19 C19 H19A 109.5 . . ? N6 C19 H19B 109.5 . . ? H19 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N7 C20 Se 178.8(3) . . ? O12 Cl O11 120.7(3) . . ? O12 Cl O13 118.0(3) . . ? O11 Cl O13 109.7(3) . . ? O12 Cl O14 104.9(3) . . ? O11 Cl O14 101.8(3) . . ? O13 Cl O14 97.3(3) . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 30.52 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.846 _refine_diff_density_min -0.373 _refine_diff_density_rms 0.061 data_complex_2_at_123_K _database_code_CSD 169870 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H44 Cl Cu3 N7 O13 Se' _chemical_formula_weight 895.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.4518(11) _cell_length_b 14.2871(13) _cell_length_c 18.8940(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3361.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Needle _exptl_crystal_colour Blue _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.770 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1820 _exptl_absorpt_coefficient_mu 3.111 _exptl_absorpt_correction_type Semi-empirical _exptl_absorpt_correction_T_min 0.3053 _exptl_absorpt_correction_T_max 0.5101 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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_% 0.13 _diffrn_reflns_number 19416 _diffrn_reflns_av_R_equivalents 0.0421 _diffrn_reflns_av_sigmaI/netI 0.0340 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6220 _reflns_number_gt 7328 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _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 w=1/[\s^2^(Fo^2^)+(0.0545P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.013(10) _refine_ls_number_reflns 8340 _refine_ls_number_parameters 403 _refine_ls_number_restraints 38 _refine_ls_R_factor_all 0.0391 _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_ref 0.0900 _refine_ls_wR_factor_gt 0.0874 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Se Se 0.39042(3) -0.08876(3) -0.13567(2) 0.02909(10) Uani 1 d . . . Cu1 Cu 0.33538(3) 0.58179(3) 0.37059(2) 0.02121(10) Uani 1 d . . . Cu2 Cu 0.21570(3) 0.22523(3) 0.26118(2) 0.02007(10) Uani 1 d . . . Cu3 Cu 0.16794(3) -0.07180(3) 0.06941(2) 0.02384(11) Uani 1 d . . . O1 O 0.21714(19) 0.52922(18) 0.32828(14) 0.0214(5) Uani 1 d . . . O2 O 0.37055(18) 0.42694(18) 0.37138(13) 0.0198(5) Uani 1 d . . . O3 O 0.32240(19) 0.27380(18) 0.32206(13) 0.0209(5) Uani 1 d . . . O4 O 0.27992(19) 0.09149(19) 0.22902(13) 0.0235(5) Uani 1 d . . . O5 O 0.1078(2) 0.0666(2) 0.09646(14) 0.0250(6) Uani 1 d . . . O6 O 0.2573(2) -0.0385(2) 0.14912(15) 0.0282(6) Uani 1 d . . . N1 N 0.4466(2) 0.6273(2) 0.42969(16) 0.0185(6) Uani 1 d . . . N2 N 0.2841(2) 0.7311(2) 0.38370(16) 0.0230(6) Uani 1 d . . . N3 N 0.1654(2) 0.3675(2) 0.27965(15) 0.0191(6) Uani 1 d . . . N4 N 0.1247(2) 0.1886(2) 0.18909(15) 0.0182(6) Uani 1 d . . . N5 N 0.0552(2) -0.1219(2) 0.01167(16) 0.0186(6) Uani 1 d . . . N6 N 0.2071(2) -0.2265(2) 0.07181(17) 0.0258(7) Uani 1 d . . . N7 N 0.2646(3) -0.0284(3) -0.0176(2) 0.0338(8) Uani 1 d . . . C1 C 0.4209(4) 0.7340(3) 0.4601(3) 0.0364(10) Uani 1 d . . . H1 H 0.3774 0.7282 0.5037 0.044 Uiso 1 calc R . . H1A H 0.4898 0.7638 0.4733 0.044 Uiso 1 calc R . . C2 C 0.3629(4) 0.7977(3) 0.4096(3) 0.0371(10) Uani 1 d . . . H2 H 0.3290 0.8514 0.4341 0.045 Uiso 1 calc R . . H2A H 0.4105 0.8208 0.3714 0.045 Uiso 1 calc R . . C3 C 0.4635(3) 0.5531(3) 0.4902(2) 0.0314(9) Uani 1 d . . . H3 H 0.3997 0.5515 0.5206 0.038 Uiso 1 calc R . . H3A H 0.5263 0.5705 0.5185 0.038 Uiso 1 calc R . . H3B H 0.4749 0.4912 0.4692 0.038 Uiso 1 calc R . . C4 C 0.5325(4) 0.6298(4) 0.3873(3) 0.0497(13) Uani 1 d . . . H4 H 0.5210 0.6762 0.3498 0.060 Uiso 1 calc R . . H4A H 0.5436 0.5680 0.3660 0.060 Uiso 1 calc R . . H4B H 0.5961 0.6471 0.4149 0.060 Uiso 1 calc R . . C5 C 0.1998(3) 0.7300(3) 0.4297(2) 0.0351(9) Uani 1 d . . . H5 H 0.1461 0.6847 0.4135 0.042 Uiso 1 calc R . . H5A H 0.1674 0.7924 0.4319 0.042 Uiso 1 calc R . . H5B H 0.2254 0.7120 0.4769 0.042 Uiso 1 calc R . . C6 C 0.2519(4) 0.7782(3) 0.3146(2) 0.0373(10) Uani 1 d . . . H6 H 0.3133 0.7785 0.2821 0.045 Uiso 1 calc R . . H6A H 0.2294 0.8427 0.3241 0.045 Uiso 1 calc R . . H6B H 0.1923 0.7437 0.2930 0.045 Uiso 1 calc R . . C7 C 0.2223(3) 0.4297(2) 0.31359(17) 0.0164(6) Uani 1 d . . . C8 C 0.3119(2) 0.3714(2) 0.33760(17) 0.0153(7) Uani 1 d . . . C9 C 0.0811(2) 0.4145(3) 0.24902(17) 0.0169(7) Uani 1 d . . . H9 H 0.1035 0.4504 0.2067 0.020 Uiso 1 calc R . . H9A H 0.0443 0.4565 0.2829 0.020 Uiso 1 calc R . . C10 C 0.0105(3) 0.3269(3) 0.2292(2) 0.0229(8) Uani 1 d . . . H10 H -0.0613 0.3514 0.2166 0.027 Uiso 1 calc R . . H10A H 0.0012 0.2906 0.2734 0.027 Uiso 1 calc R . . C11 C 0.0421(3) 0.2521(3) 0.1683(2) 0.0245(8) Uani 1 d . . . H11 H -0.0227 0.2158 0.1553 0.029 Uiso 1 calc R . . H11A H 0.0661 0.2865 0.1256 0.029 Uiso 1 calc R . . C12 C 0.1495(3) 0.1062(3) 0.15107(18) 0.0190(7) Uani 1 d . . . C13 C 0.2363(3) 0.0478(3) 0.1793(2) 0.0244(8) Uani 1 d . . . C14 C 0.0618(3) -0.2408(3) 0.00327(19) 0.0196(7) Uani 1 d . . . H14 H 0.0196 -0.2701 0.0417 0.024 Uiso 1 calc R . . H14A H 0.0289 -0.2593 -0.0423 0.024 Uiso 1 calc R . . C15 C 0.1668(3) -0.2742(3) 0.00590(18) 0.0205(7) Uani 1 d . . . H15 H 0.2085 -0.2551 -0.0364 0.025 Uiso 1 calc R . . H15A H 0.1689 -0.3432 0.0106 0.025 Uiso 1 calc R . . C16 C -0.0341(3) -0.0967(3) 0.0493(2) 0.0321(9) Uani 1 d . . . H16 H -0.0341 -0.1292 0.0950 0.039 Uiso 1 calc R . . H16A H -0.0986 -0.1139 0.0227 0.039 Uiso 1 calc R . . H16B H -0.0334 -0.0289 0.0573 0.039 Uiso 1 calc R . . C17 C 0.0560(3) -0.0712(3) -0.0592(2) 0.0298(9) Uani 1 d . . . H17 H 0.1197 -0.0898 -0.0861 0.036 Uiso 1 calc R . . H17A H 0.0575 -0.0034 -0.0511 0.036 Uiso 1 calc R . . H17B H -0.0088 -0.0876 -0.0859 0.036 Uiso 1 calc R . . C18 C 0.1680(4) -0.2800(4) 0.1359(2) 0.0411(10) Uani 1 d . . . H18 H 0.0901 -0.2722 0.1406 0.049 Uiso 1 calc R . . H18A H 0.2036 -0.2560 0.1784 0.049 Uiso 1 calc R . . H18B H 0.1849 -0.3466 0.1302 0.049 Uiso 1 calc R . . C19 C 0.3100(3) -0.2434(3) 0.0710(2) 0.0288(9) Uani 1 d . . . H19 H 0.3428 -0.2117 0.0304 0.035 Uiso 1 calc R . . H19A H 0.3220 -0.3110 0.0672 0.035 Uiso 1 calc R . . H19B H 0.3424 -0.2202 0.1149 0.035 Uiso 1 calc R . . C20 C 0.3140(3) -0.0504(3) -0.0638(2) 0.0250(8) Uani 1 d . . . O7 O 0.4017(2) 0.5927(2) 0.25849(14) 0.0288(6) Uani 1 d . . . O8 O 0.5227(2) 0.2663(2) 0.29645(16) 0.0360(7) Uani 1 d . . . O9 O 0.4383(2) -0.0405(2) 0.26904(16) 0.0328(6) Uani 1 d . . . Cl Cl 0.31265(9) 0.40917(9) 0.11518(7) 0.0502(3) Uani 1 d D . . O11 O 0.2973(7) 0.5034(5) 0.1452(5) 0.062(2) Uiso 0.50 d PD . . O12 O 0.3896(5) 0.4040(5) 0.0619(4) 0.0549(19) Uiso 0.50 d PD . . O13 O 0.3451(7) 0.3462(5) 0.1752(4) 0.061(2) Uiso 0.50 d PD . . O14 O 0.2143(6) 0.3734(6) 0.0895(5) 0.071(2) Uiso 0.50 d PD . . O11' O 0.2546(6) 0.3226(4) 0.1123(4) 0.0531(19) Uiso 0.50 d PD . . O12' O 0.4213(6) 0.3977(7) 0.1117(6) 0.101(4) Uiso 0.50 d PD . . O13' O 0.2761(7) 0.4625(5) 0.0482(4) 0.062(2) Uiso 0.50 d PD . . O14' O 0.2825(8) 0.4747(6) 0.1708(4) 0.067(2) Uiso 0.50 d PD . . 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 Se 0.02233(17) 0.0368(2) 0.02813(19) -0.00065(19) 0.00032(15) -0.00174(17) Cu1 0.01557(17) 0.0231(2) 0.0250(2) -0.0015(2) -0.00553(17) -0.00008(18) Cu2 0.01374(17) 0.0248(2) 0.0217(2) -0.00500(19) -0.00424(16) 0.00201(18) Cu3 0.01728(18) 0.0289(3) 0.0254(2) -0.0066(2) -0.00447(17) 0.0024(2) O1 0.0117(10) 0.0254(14) 0.0270(13) -0.0027(11) -0.0032(10) 0.0015(10) O2 0.0139(10) 0.0257(13) 0.0197(11) -0.0039(11) -0.0040(9) -0.0014(10) O3 0.0145(10) 0.0263(14) 0.0219(12) -0.0013(11) -0.0058(9) 0.0001(10) O4 0.0138(10) 0.0330(15) 0.0236(12) -0.0056(12) -0.0035(10) 0.0036(11) O5 0.0178(11) 0.0315(15) 0.0257(13) -0.0056(11) -0.0054(10) 0.0036(11) O6 0.0180(12) 0.0347(15) 0.0320(15) -0.0090(13) -0.0057(11) 0.0039(11) N1 0.0135(12) 0.0207(15) 0.0213(14) -0.0006(13) -0.0023(11) -0.0011(11) N2 0.0177(13) 0.0253(15) 0.0260(16) -0.0029(14) -0.0025(12) -0.0026(13) N3 0.0120(12) 0.0243(16) 0.0212(15) -0.0021(12) -0.0040(11) -0.0007(12) N4 0.0111(12) 0.0249(16) 0.0185(14) -0.0012(12) -0.0030(10) 0.0016(11) N5 0.0116(12) 0.0241(16) 0.0202(14) -0.0030(13) -0.0012(11) 0.0001(12) N6 0.0199(14) 0.0357(18) 0.0219(15) -0.0031(15) -0.0004(12) -0.0003(14) N7 0.0231(17) 0.042(2) 0.0367(19) -0.0019(17) 0.0005(15) -0.0010(16) C1 0.031(2) 0.033(2) 0.045(3) -0.007(2) -0.0124(19) 0.0010(19) C2 0.029(2) 0.040(3) 0.042(2) -0.002(2) -0.0043(18) -0.0015(18) C3 0.027(2) 0.038(2) 0.029(2) -0.0007(18) -0.0061(16) -0.0015(18) C4 0.038(3) 0.065(4) 0.046(3) -0.007(3) 0.003(2) -0.008(2) C5 0.029(2) 0.042(2) 0.034(2) 0.006(2) 0.0055(17) 0.0070(19) C6 0.029(2) 0.045(3) 0.038(2) 0.004(2) -0.0032(18) 0.004(2) C7 0.0125(12) 0.0218(18) 0.0149(14) 0.0012(14) -0.0021(11) -0.0024(14) C8 0.0090(13) 0.0231(18) 0.0137(15) 0.0006(13) -0.0053(11) -0.0019(12) C9 0.0113(12) 0.0223(18) 0.0171(16) -0.0023(14) -0.0021(10) 0.0001(13) C10 0.0161(15) 0.028(2) 0.0247(18) 0.0004(16) -0.0028(14) -0.0006(14) C11 0.0162(15) 0.032(2) 0.0250(18) -0.0068(16) -0.0067(14) 0.0022(14) C12 0.0162(15) 0.0232(19) 0.0177(16) -0.0010(14) -0.0023(12) -0.0005(13) C13 0.0171(16) 0.029(2) 0.0273(19) -0.0045(16) -0.0055(14) 0.0010(14) C14 0.0158(15) 0.0219(18) 0.0212(16) -0.0045(14) -0.0023(13) -0.0026(14) C15 0.0177(14) 0.0229(18) 0.0210(16) -0.0033(15) 0.0015(14) -0.0013(16) C16 0.0193(16) 0.042(3) 0.035(2) -0.010(2) -0.0003(15) 0.0013(17) C17 0.0231(17) 0.030(2) 0.036(2) -0.0006(19) -0.0028(16) 0.0000(17) C18 0.032(2) 0.057(3) 0.034(2) 0.005(2) 0.000(2) 0.001(2) C19 0.0177(16) 0.036(2) 0.033(2) -0.0011(18) -0.0004(15) 0.0052(15) C20 0.0190(16) 0.025(2) 0.031(2) -0.0036(17) -0.0021(15) -0.0003(14) O7 0.0195(11) 0.0382(16) 0.0285(14) 0.0032(13) -0.0004(11) -0.0014(12) O8 0.0218(13) 0.0486(19) 0.0374(16) -0.0008(15) -0.0014(12) 0.0072(13) O9 0.0206(12) 0.0422(17) 0.0355(15) 0.0050(14) 0.0008(12) 0.0000(12) Cl 0.0376(6) 0.0489(7) 0.0640(8) -0.0161(6) 0.0188(5) -0.0109(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Se C20 1.747(4) . ? Cu1 O1 1.836(2) . ? Cu1 N1 1.894(3) . ? Cu1 N2 2.240(3) . ? Cu1 O2 2.255(3) . ? Cu1 O7 2.278(3) . ? Cu2 N4 1.848(3) . ? Cu2 O3 1.889(2) . ? Cu2 N3 2.155(3) . ? Cu2 O4 2.159(3) . ? Cu3 N5 1.917(3) . ? Cu3 O6 1.932(3) . ? Cu3 N7 2.130(4) . ? Cu3 O5 2.175(3) . ? Cu3 N6 2.264(4) . ? O1 C7 1.451(4) . ? O2 C8 1.253(4) . ? O3 C8 1.430(4) . ? O4 C13 1.252(4) . ? O5 C12 1.286(4) . ? O6 C13 1.383(5) . ? N1 C4 1.338(6) . ? N1 C3 1.573(5) . ? N1 C1 1.660(5) . ? N2 C5 1.363(5) . ? N2 C2 1.453(5) . ? N2 C6 1.523(5) . ? N3 C7 1.305(4) . ? N3 C9 1.374(4) . ? N4 C12 1.414(5) . ? N4 C11 1.426(4) . ? N5 C16 1.368(5) . ? N5 C17 1.522(5) . ? N5 C14 1.708(5) . ? N6 C19 1.304(5) . ? N6 C15 1.505(5) . ? N6 C18 1.512(6) . ? N7 C20 1.112(5) . ? C1 C2 1.503(6) . ? C1 H1 0.9900 . ? C1 H1A 0.9900 . ? C2 H2 0.9900 . ? C2 H2A 0.9900 . ? C3 H3 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C4 H4 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C5 H5 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 H6 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 C8 1.465(4) . ? C9 C10 1.574(5) . ? C9 H9 0.9900 . ? C9 H9A 0.9900 . ? C10 C11 1.620(5) . ? C10 H10 0.9900 . ? C10 H10A 0.9900 . ? C11 H11 0.9900 . ? C11 H11A 0.9900 . ? C12 C13 1.466(5) . ? C14 C15 1.394(5) . ? C14 H14 0.9900 . ? C14 H14A 0.9900 . ? C15 H15 0.9900 . ? C15 H15A 0.9900 . ? C16 H16 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C17 H17 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 H18 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 H19 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? Cl O12' 1.364(7) . ? Cl O12 1.391(6) . ? Cl O14 1.413(7) . ? Cl O11' 1.434(6) . ? Cl O14' 1.456(7) . ? Cl O11 1.473(6) . ? Cl O13 1.503(6) . ? Cl O13' 1.545(6) . ? O11 O14' 0.659(11) . ? O12 O12' 1.023(11) . ? O12 O13' 1.662(10) . ? O13 O11' 1.672(10) . ? O13 O12' 1.698(12) . ? O14 O11' 0.982(10) . ? O14 O13' 1.680(11) . ? 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 O1 Cu1 N1 169.55(12) . . ? O1 Cu1 N2 102.06(11) . . ? N1 Cu1 N2 79.42(12) . . ? O1 Cu1 O2 75.96(10) . . ? N1 Cu1 O2 101.01(11) . . ? N2 Cu1 O2 171.33(10) . . ? O1 Cu1 O7 85.06(11) . . ? N1 Cu1 O7 105.05(11) . . ? N2 Cu1 O7 98.10(11) . . ? O2 Cu1 O7 90.17(10) . . ? N4 Cu2 O3 169.81(12) . . ? N4 Cu2 N3 102.01(12) . . ? O3 Cu2 N3 76.08(11) . . ? N4 Cu2 O4 76.64(11) . . ? O3 Cu2 O4 103.66(10) . . ? N3 Cu2 O4 171.11(11) . . ? N5 Cu3 O6 163.26(13) . . ? N5 Cu3 N7 94.76(13) . . ? O6 Cu3 N7 101.80(13) . . ? N5 Cu3 O5 102.75(11) . . ? O6 Cu3 O5 77.94(10) . . ? N7 Cu3 O5 96.40(13) . . ? N5 Cu3 N6 78.73(12) . . ? O6 Cu3 N6 95.81(12) . . ? N7 Cu3 N6 100.25(13) . . ? O5 Cu3 N6 163.12(11) . . ? C7 O1 Cu1 116.66(19) . . ? C8 O2 Cu1 120.3(2) . . ? C8 O3 Cu2 114.76(19) . . ? C13 O4 Cu2 119.5(2) . . ? C12 O5 Cu3 116.7(2) . . ? C13 O6 Cu3 115.6(2) . . ? C4 N1 C3 110.3(4) . . ? C4 N1 C1 109.7(4) . . ? C3 N1 C1 113.2(3) . . ? C4 N1 Cu1 104.0(3) . . ? C3 N1 Cu1 107.2(2) . . ? C1 N1 Cu1 112.2(2) . . ? C5 N2 C2 108.2(3) . . ? C5 N2 C6 110.5(3) . . ? C2 N2 C6 100.2(3) . . ? C5 N2 Cu1 106.2(3) . . ? C2 N2 Cu1 118.0(2) . . ? C6 N2 Cu1 113.6(2) . . ? C7 N3 C9 106.8(3) . . ? C7 N3 Cu2 124.3(2) . . ? C9 N3 Cu2 127.9(2) . . ? C12 N4 C11 123.2(3) . . ? C12 N4 Cu2 118.5(2) . . ? C11 N4 Cu2 117.7(2) . . ? C16 N5 C17 109.7(3) . . ? C16 N5 C14 110.4(3) . . ? C17 N5 C14 113.0(3) . . ? C16 N5 Cu3 101.6(2) . . ? C17 N5 Cu3 108.5(2) . . ? C14 N5 Cu3 112.89(19) . . ? C19 N6 C15 103.5(3) . . ? C19 N6 C18 103.4(3) . . ? C15 N6 C18 109.0(3) . . ? C19 N6 Cu3 113.1(3) . . ? C15 N6 Cu3 110.7(2) . . ? C18 N6 Cu3 116.1(3) . . ? C20 N7 Cu3 146.7(4) . . ? C2 C1 N1 115.4(3) . . ? C2 C1 H1 108.4 . . ? N1 C1 H1 108.4 . . ? C2 C1 H1A 108.4 . . ? N1 C1 H1A 108.4 . . ? H1 C1 H1A 107.5 . . ? N2 C2 C1 98.1(4) . . ? N2 C2 H2 112.1 . . ? C1 C2 H2 112.1 . . ? N2 C2 H2A 112.1 . . ? C1 C2 H2A 112.1 . . ? H2 C2 H2A 109.8 . . ? N1 C3 H3 109.5 . . ? N1 C3 H3A 109.5 . . ? H3 C3 H3A 109.5 . . ? N1 C3 H3B 109.5 . . ? H3 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N1 C4 H4 109.5 . . ? N1 C4 H4A 109.5 . . ? H4 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N2 C5 H5 109.5 . . ? N2 C5 H5A 109.5 . . ? H5 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C6 H6 109.5 . . ? N2 C6 H6A 109.5 . . ? H6 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? H6 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N3 C7 O1 137.5(3) . . ? N3 C7 C8 100.3(3) . . ? O1 C7 C8 122.2(3) . . ? O2 C8 O3 132.0(3) . . ? O2 C8 C7 103.9(3) . . ? O3 C8 C7 124.1(3) . . ? N3 C9 C10 98.0(3) . . ? N3 C9 H9 112.2 . . ? C10 C9 H9 112.2 . . ? N3 C9 H9A 112.2 . . ? C10 C9 H9A 112.2 . . ? H9 C9 H9A 109.8 . . ? C9 C10 C11 124.0(3) . . ? C9 C10 H10 106.3 . . ? C11 C10 H10 106.3 . . ? C9 C10 H10A 106.3 . . ? C11 C10 H10A 106.3 . . ? H10 C10 H10A 106.4 . . ? N4 C11 C10 113.5(3) . . ? N4 C11 H11 108.9 . . ? C10 C11 H11 108.9 . . ? N4 C11 H11A 108.9 . . ? C10 C11 H11A 108.9 . . ? H11 C11 H11A 107.7 . . ? O5 C12 N4 133.3(3) . . ? O5 C12 C13 109.9(3) . . ? N4 C12 C13 116.8(3) . . ? O4 C13 O6 132.2(3) . . ? O4 C13 C12 108.0(3) . . ? O6 C13 C12 119.8(3) . . ? C15 C14 N5 112.5(3) . . ? C15 C14 H14 109.1 . . ? N5 C14 H14 109.1 . . ? C15 C14 H14A 109.1 . . ? N5 C14 H14A 109.1 . . ? H14 C14 H14A 107.8 . . ? C14 C15 N6 100.8(3) . . ? C14 C15 H15 111.6 . . ? N6 C15 H15 111.6 . . ? C14 C15 H15A 111.6 . . ? N6 C15 H15A 111.6 . . ? H15 C15 H15A 109.4 . . ? N5 C16 H16 109.5 . . ? N5 C16 H16A 109.5 . . ? H16 C16 H16A 109.5 . . ? N5 C16 H16B 109.5 . . ? H16 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N5 C17 H17 109.5 . . ? N5 C17 H17A 109.5 . . ? H17 C17 H17A 109.5 . . ? N5 C17 H17B 109.5 . . ? H17 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N6 C18 H18 109.5 . . ? N6 C18 H18A 109.5 . . ? H18 C18 H18A 109.5 . . ? N6 C18 H18B 109.5 . . ? H18 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N6 C19 H19 109.5 . . ? N6 C19 H19A 109.5 . . ? H19 C19 H19A 109.5 . . ? N6 C19 H19B 109.5 . . ? H19 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N7 C20 Se 178.1(4) . . ? O12' Cl O12 43.6(5) . . ? O12' Cl O14 143.1(6) . . ? O12 Cl O14 109.3(5) . . ? O12' Cl O11' 113.3(5) . . ? O12 Cl O11' 106.0(4) . . ? O14 Cl O11' 40.3(4) . . ? O12' Cl O14' 111.5(6) . . ? O12 Cl O14' 137.1(5) . . ? O14 Cl O14' 104.9(5) . . ? O11' Cl O14' 116.9(5) . . ? O12' Cl O11 104.9(6) . . ? O12 Cl O11 114.6(4) . . ? O14 Cl O11 110.5(5) . . ? O11' Cl O11 137.5(5) . . ? O14' Cl O11 26.0(4) . . ? O12' Cl O13 72.4(5) . . ? O12 Cl O13 109.2(4) . . ? O14 Cl O13 106.0(5) . . ? O11' Cl O13 69.4(4) . . ? O14' Cl O13 84.8(5) . . ? O11 Cl O13 106.9(4) . . ? O12' Cl O13' 108.2(5) . . ? O12 Cl O13' 68.7(4) . . ? O14 Cl O13' 69.0(5) . . ? O11' Cl O13' 104.3(4) . . ? O14' Cl O13' 101.4(4) . . ? O11 Cl O13' 80.0(5) . . ? O13 Cl O13' 172.8(4) . . ? O14' O11 Cl 75.6(9) . . ? O12' O12 Cl 66.8(5) . . ? O12' O12 O13' 121.0(8) . . ? Cl O12 O13' 60.0(4) . . ? Cl O13 O11' 53.4(3) . . ? Cl O13 O12' 50.0(3) . . ? O11' O13 O12' 87.8(5) . . ? O11' O14 Cl 70.9(6) . . ? O11' O14 O13' 122.0(8) . . ? Cl O14 O13' 59.2(4) . . ? O14 O11' Cl 68.7(5) . . ? O14 O11' O13 120.5(7) . . ? Cl O11' O13 57.3(3) . . ? O12 O12' Cl 69.6(6) . . ? O12 O12' O13 118.2(8) . . ? Cl O12' O13 57.6(4) . . ? Cl O13' O12 51.3(3) . . ? Cl O13' O14 51.8(3) . . ? O12 O13' O14 86.4(5) . . ? O11 O14' Cl 78.4(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Cu1 O1 C7 -81.4(7) . . . . ? N2 Cu1 O1 C7 -178.4(2) . . . . ? O2 Cu1 O1 C7 -7.1(2) . . . . ? O7 Cu1 O1 C7 84.3(2) . . . . ? O1 Cu1 O2 C8 9.7(2) . . . . ? N1 Cu1 O2 C8 179.4(2) . . . . ? N2 Cu1 O2 C8 87.5(7) . . . . ? O7 Cu1 O2 C8 -75.2(2) . . . . ? N4 Cu2 O3 C8 75.3(7) . . . . ? N3 Cu2 O3 C8 -5.1(2) . . . . ? O4 Cu2 O3 C8 165.7(2) . . . . ? N4 Cu2 O4 C13 1.1(3) . . . . ? O3 Cu2 O4 C13 -168.5(3) . . . . ? N3 Cu2 O4 C13 -81.2(7) . . . . ? N5 Cu3 O5 C12 159.7(3) . . . . ? O6 Cu3 O5 C12 -3.2(3) . . . . ? N7 Cu3 O5 C12 -103.9(3) . . . . ? N6 Cu3 O5 C12 66.5(5) . . . . ? N5 Cu3 O6 C13 -93.3(5) . . . . ? N7 Cu3 O6 C13 95.0(3) . . . . ? O5 Cu3 O6 C13 0.9(3) . . . . ? N6 Cu3 O6 C13 -163.2(3) . . . . ? O1 Cu1 N1 C4 151.7(6) . . . . ? N2 Cu1 N1 C4 -109.2(3) . . . . ? O2 Cu1 N1 C4 79.7(3) . . . . ? O7 Cu1 N1 C4 -13.5(3) . . . . ? O1 Cu1 N1 C3 34.9(8) . . . . ? N2 Cu1 N1 C3 134.1(2) . . . . ? O2 Cu1 N1 C3 -37.1(2) . . . . ? O7 Cu1 N1 C3 -130.3(2) . . . . ? O1 Cu1 N1 C1 -89.9(7) . . . . ? N2 Cu1 N1 C1 9.3(2) . . . . ? O2 Cu1 N1 C1 -161.9(2) . . . . ? O7 Cu1 N1 C1 104.9(2) . . . . ? O1 Cu1 N2 C5 64.6(3) . . . . ? N1 Cu1 N2 C5 -104.8(3) . . . . ? O2 Cu1 N2 C5 -11.2(8) . . . . ? O7 Cu1 N2 C5 151.3(3) . . . . ? O1 Cu1 N2 C2 -173.9(3) . . . . ? N1 Cu1 N2 C2 16.7(3) . . . . ? O2 Cu1 N2 C2 110.3(7) . . . . ? O7 Cu1 N2 C2 -87.2(3) . . . . ? O1 Cu1 N2 C6 -57.0(3) . . . . ? N1 Cu1 N2 C6 133.5(3) . . . . ? O2 Cu1 N2 C6 -132.9(6) . . . . ? O7 Cu1 N2 C6 29.6(3) . . . . ? N4 Cu2 N3 C7 -162.6(3) . . . . ? O3 Cu2 N3 C7 7.1(3) . . . . ? O4 Cu2 N3 C7 -82.3(7) . . . . ? N4 Cu2 N3 C9 4.8(3) . . . . ? O3 Cu2 N3 C9 174.5(3) . . . . ? O4 Cu2 N3 C9 85.1(7) . . . . ? O3 Cu2 N4 C12 87.3(7) . . . . ? N3 Cu2 N4 C12 165.4(2) . . . . ? O4 Cu2 N4 C12 -5.6(2) . . . . ? O3 Cu2 N4 C11 -83.8(7) . . . . ? N3 Cu2 N4 C11 -5.7(3) . . . . ? O4 Cu2 N4 C11 -176.7(3) . . . . ? O6 Cu3 N5 C16 46.4(6) . . . . ? N7 Cu3 N5 C16 -141.8(3) . . . . ? O5 Cu3 N5 C16 -44.1(3) . . . . ? N6 Cu3 N5 C16 118.7(3) . . . . ? O6 Cu3 N5 C17 162.0(4) . . . . ? N7 Cu3 N5 C17 -26.2(2) . . . . ? O5 Cu3 N5 C17 71.5(2) . . . . ? N6 Cu3 N5 C17 -125.7(2) . . . . ? O6 Cu3 N5 C14 -71.9(5) . . . . ? N7 Cu3 N5 C14 99.9(2) . . . . ? O5 Cu3 N5 C14 -162.4(2) . . . . ? N6 Cu3 N5 C14 0.4(2) . . . . ? N5 Cu3 N6 C19 143.0(3) . . . . ? O6 Cu3 N6 C19 -53.0(3) . . . . ? N7 Cu3 N6 C19 50.2(3) . . . . ? O5 Cu3 N6 C19 -120.1(4) . . . . ? N5 Cu3 N6 C15 27.4(2) . . . . ? O6 Cu3 N6 C15 -168.6(2) . . . . ? N7 Cu3 N6 C15 -65.5(2) . . . . ? O5 Cu3 N6 C15 124.2(3) . . . . ? N5 Cu3 N6 C18 -97.7(3) . . . . ? O6 Cu3 N6 C18 66.3(3) . . . . ? N7 Cu3 N6 C18 169.5(3) . . . . ? O5 Cu3 N6 C18 -0.9(5) . . . . ? N5 Cu3 N7 C20 -66.8(6) . . . . ? O6 Cu3 N7 C20 110.8(6) . . . . ? O5 Cu3 N7 C20 -170.2(6) . . . . ? N6 Cu3 N7 C20 12.6(6) . . . . ? C4 N1 C1 C2 79.4(5) . . . . ? C3 N1 C1 C2 -157.0(4) . . . . ? Cu1 N1 C1 C2 -35.6(4) . . . . ? C5 N2 C2 C1 84.8(4) . . . . ? C6 N2 C2 C1 -159.6(3) . . . . ? Cu1 N2 C2 C1 -35.7(4) . . . . ? N1 C1 C2 N2 43.4(4) . . . . ? C9 N3 C7 O1 2.6(5) . . . . ? Cu2 N3 C7 O1 172.3(3) . . . . ? C9 N3 C7 C8 -175.5(3) . . . . ? Cu2 N3 C7 C8 -5.8(3) . . . . ? Cu1 O1 C7 N3 -171.6(3) . . . . ? Cu1 O1 C7 C8 6.2(4) . . . . ? Cu1 O2 C8 O3 171.4(3) . . . . ? Cu1 O2 C8 C7 -7.9(3) . . . . ? Cu2 O3 C8 O2 -174.7(3) . . . . ? Cu2 O3 C8 C7 4.4(4) . . . . ? N3 C7 C8 O2 -179.7(3) . . . . ? O1 C7 C8 O2 1.8(4) . . . . ? N3 C7 C8 O3 1.0(4) . . . . ? O1 C7 C8 O3 -177.5(3) . . . . ? C7 N3 C9 C10 -166.4(3) . . . . ? Cu2 N3 C9 C10 24.5(3) . . . . ? N3 C9 C10 C11 -69.6(4) . . . . ? C12 N4 C11 C10 166.4(3) . . . . ? Cu2 N4 C11 C10 -22.9(4) . . . . ? C9 C10 C11 N4 75.9(4) . . . . ? Cu3 O5 C12 N4 -172.0(3) . . . . ? Cu3 O5 C12 C13 4.2(4) . . . . ? C11 N4 C12 O5 -3.8(6) . . . . ? Cu2 N4 C12 O5 -174.4(3) . . . . ? C11 N4 C12 C13 -179.8(3) . . . . ? Cu2 N4 C12 C13 9.6(4) . . . . ? Cu2 O4 C13 O6 -177.9(3) . . . . ? Cu2 O4 C13 C12 3.3(4) . . . . ? Cu3 O6 C13 O4 -177.5(4) . . . . ? Cu3 O6 C13 C12 1.1(4) . . . . ? O5 C12 C13 O4 175.3(3) . . . . ? N4 C12 C13 O4 -7.8(5) . . . . ? O5 C12 C13 O6 -3.6(5) . . . . ? N4 C12 C13 O6 173.3(3) . . . . ? C16 N5 C14 C15 -144.1(3) . . . . ? C17 N5 C14 C15 92.6(4) . . . . ? Cu3 N5 C14 C15 -31.1(4) . . . . ? N5 C14 C15 N6 50.1(4) . . . . ? C19 N6 C15 C14 -170.4(3) . . . . ? C18 N6 C15 C14 80.0(4) . . . . ? Cu3 N6 C15 C14 -48.9(3) . . . . ? Cu3 N7 C20 Se 4(11) . . . . ? O12' Cl O11 O14' -108.8(13) . . . . ? O12 Cl O11 O14' -154.2(12) . . . . ? O14 Cl O11 O14' 81.8(14) . . . . ? O11' Cl O11 O14' 44.6(16) . . . . ? O13 Cl O11 O14' -33.0(14) . . . . ? O13' Cl O11 O14' 144.9(14) . . . . ? O14 Cl O12 O12' -149.5(8) . . . . ? O11' Cl O12 O12' -107.2(8) . . . . ? O14' Cl O12 O12' 69.6(10) . . . . ? O11 Cl O12 O12' 85.9(9) . . . . ? O13 Cl O12 O12' -33.9(9) . . . . ? O13' Cl O12 O12' 153.4(9) . . . . ? O12' Cl O12 O13' -153.4(9) . . . . ? O14 Cl O12 O13' 57.1(5) . . . . ? O11' Cl O12 O13' 99.4(5) . . . . ? O14' Cl O12 O13' -83.8(7) . . . . ? O11 Cl O12 O13' -67.5(5) . . . . ? O13 Cl O12 O13' 172.6(5) . . . . ? O12' Cl O13 O11' -124.2(6) . . . . ? O12 Cl O13 O11' -100.4(5) . . . . ? O14 Cl O13 O11' 17.3(5) . . . . ? O14' Cl O13 O11' 121.3(5) . . . . ? O11 Cl O13 O11' 135.2(5) . . . . ? O13' Cl O13 O11' -28(4) . . . . ? O12 Cl O13 O12' 23.8(6) . . . . ? O14 Cl O13 O12' 141.4(6) . . . . ? O11' Cl O13 O12' 124.2(6) . . . . ? O14' Cl O13 O12' -114.6(6) . . . . ? O11 Cl O13 O12' -100.7(6) . . . . ? O13' Cl O13 O12' 96(4) . . . . ? O12' Cl O14 O11' 56.5(12) . . . . ? O12 Cl O14 O11' 92.2(7) . . . . ? O14' Cl O14 O11' -114.1(7) . . . . ? O11 Cl O14 O11' -140.8(7) . . . . ? O13 Cl O14 O11' -25.4(8) . . . . ? O13' Cl O14 O11' 149.1(8) . . . . ? O12' Cl O14 O13' -92.6(10) . . . . ? O12 Cl O14 O13' -56.9(5) . . . . ? O11' Cl O14 O13' -149.1(8) . . . . ? O14' Cl O14 O13' 96.7(5) . . . . ? O11 Cl O14 O13' 70.1(5) . . . . ? O13 Cl O14 O13' -174.5(4) . . . . ? O13' O14 O11' Cl 31.3(7) . . . . ? Cl O14 O11' O13 25.5(7) . . . . ? O13' O14 O11' O13 56.8(12) . . . . ? O12' Cl O11' O14 -147.0(8) . . . . ? O12 Cl O11' O14 -101.2(7) . . . . ? O14' Cl O11' O14 81.3(8) . . . . ? O11 Cl O11' O14 61.1(10) . . . . ? O13 Cl O11' O14 153.9(8) . . . . ? O13' Cl O11' O14 -29.6(8) . . . . ? O12' Cl O11' O13 59.2(6) . . . . ? O12 Cl O11' O13 105.0(5) . . . . ? O14 Cl O11' O13 -153.9(8) . . . . ? O14' Cl O11' O13 -72.6(6) . . . . ? O11 Cl O11' O13 -92.7(7) . . . . ? O13' Cl O11' O13 176.5(5) . . . . ? Cl O13 O11' O14 -28.4(9) . . . . ? O12' O13 O11' O14 -67.8(10) . . . . ? O12' O13 O11' Cl -39.4(4) . . . . ? O13' O12 O12' Cl 26.9(8) . . . . ? Cl O12 O12' O13 32.0(7) . . . . ? O13' O12 O12' O13 58.8(13) . . . . ? O14 Cl O12' O12 53.0(12) . . . . ? O11' Cl O12' O12 89.0(8) . . . . ? O14' Cl O12' O12 -136.7(7) . . . . ? O11 Cl O12' O12 -110.2(8) . . . . ? O13 Cl O12' O12 146.4(8) . . . . ? O13' Cl O12' O12 -26.0(8) . . . . ? O12 Cl O12' O13 -146.4(8) . . . . ? O14 Cl O12' O13 -93.4(9) . . . . ? O11' Cl O12' O13 -57.4(5) . . . . ? O14' Cl O12' O13 76.9(6) . . . . ? O11 Cl O12' O13 103.4(5) . . . . ? O13' Cl O12' O13 -172.5(4) . . . . ? Cl O13 O12' O12 -36.0(8) . . . . ? O11' O13 O12' O12 5.6(11) . . . . ? O11' O13 O12' Cl 41.6(4) . . . . ? O12' Cl O13' O12 18.9(6) . . . . ? O14 Cl O13' O12 -121.9(5) . . . . ? O11' Cl O13' O12 -101.9(5) . . . . ? O14' Cl O13' O12 136.4(5) . . . . ? O11 Cl O13' O12 121.4(5) . . . . ? O13 Cl O13' O12 -75(4) . . . . ? O12' Cl O13' O14 140.9(6) . . . . ? O12 Cl O13' O14 121.9(5) . . . . ? O11' Cl O13' O14 20.1(5) . . . . ? O14' Cl O13' O14 -101.7(6) . . . . ? O11 Cl O13' O14 -116.6(5) . . . . ? O13 Cl O13' O14 47(4) . . . . ? O12' O12 O13' Cl -28.7(9) . . . . ? O12' O12 O13' O14 -70.6(10) . . . . ? Cl O12 O13' O14 -41.9(4) . . . . ? O11' O14 O13' Cl -34.9(8) . . . . ? O11' O14 O13' O12 6.7(10) . . . . ? Cl O14 O13' O12 41.6(4) . . . . ? O12' Cl O14' O11 79.6(14) . . . . ? O12 Cl O14' O11 35.6(16) . . . . ? O14 Cl O14' O11 -106.4(13) . . . . ? O11' Cl O14' O11 -147.9(12) . . . . ? O13 Cl O14' O11 148.4(13) . . . . ? O13' Cl O14' O11 -35.3(14) . . . . ? _diffrn_measured_fraction_theta_max 0.677 _diffrn_reflns_theta_full 32.86 _diffrn_measured_fraction_theta_full 0.677 _refine_diff_density_max 1.338 _refine_diff_density_min -0.568 _refine_diff_density_rms 0.092