# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2214 data_global #============================================================================ # B007004L _publ_contact_author_name 'Prof. Ren-Gen Xiong' _publ_contact_author_address ; Prof. Ren-Gen Xiong Coordination Chemistry Institue Nanjing University, Nanjing 210093, P. R. China ; _publ_contact_author_email 'xyz@netra.nju.edu.cn' _publ_contact_author_fax '86-25-3317761' _publ_contact_author_phone '86-25-3594724' _publ_requested_journal 'J. Chem. Soc. Dalton Trans.' _publ_section_title ; The first chiral 2D molecular triangular grid exhibiting blue fluorescent emission at solid state ; _publ_section_references ; Allen, F.H., Kennard, O., Watson, D.G., Brammer, L., Orpen, A.G. & Taylor, R. (1987). Chem. Soc. Perkin Trans. II, S1-S19. Nardelli, M. (1995). J. Appl. Cryst. 28, 659. Orpen, A.G., Brammer, L., Allen, F.H., Kennard, O., Watson, D.G. & Taylor, R. (1989). J. Chem. Soc. Dalton Trans., S1-S83. Siemens (1996). SMART and SAINT. Area Detector Control and Integration Software. Siemens Analytical X-Ray Systems, Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1996). SADABS. Program for Empirical Absorption Correction of Area Detector Data, University of G\"ottingen, Germany. Sheldrick, G.M. (1997). SHELXTL V5.1 Software Reference Manual, Bruker AXS, Inc., Madison, Wisconsin, USA. Spek, A.L. (1990). Acta Cryst. A46, C-34. ; _publ_section_exptl_refinement ; The data collection covered over a hemisphere of reciprocal space by a combination of three sets of exposures; each set had a different \f angle (0, 88 and 180\%) for the crystal and each exposure of 10s covered 0.3\% in \w. The crystal-to-detector distance was 4 cm and the detector swing angle was -35\%. Coverage of the unique set is over 99% complete. Crystal decay was monitored by repeating fifty initial frames at the end of data collection and analysing the duplicate reflections, and was found to be negligible. ; #============================================================================ data_[Cu(PPh~3~)(N,N-(2-pyridyl)(4-pyridylmethyl)amine)~1.5~].0.5CHCl~3~.ClO~4~ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H64 Cl5 Cu2 N9 O8 P2' _chemical_formula_weight 1525.57 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' 'P' 'P' 0.1023 0.0942 '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 Trigonal _symmetry_space_group_name_H-M R3 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 13.6687(2) _cell_length_b 13.6687(2) _cell_length_c 32.4627(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5252.54(17) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5824 _cell_measurement_theta_min 1.83 _cell_measurement_theta_max 29.56 _exptl_crystal_description slab _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2352 _exptl_absorpt_coefficient_mu 0.905 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8257 _exptl_absorpt_correction_T_max 0.8540 _exptl_absorpt_process_details 'Sadabs (Sheldrick, 1996)' _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 'SMART CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12918 _diffrn_reflns_av_R_equivalents 0.0805 _diffrn_reflns_av_sigmaI/netI 0.1179 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 29.56 _reflns_number_total 5758 _reflns_number_gt 3700 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1996)' _computing_cell_refinement 'SAINT (Siemens, 1996)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Sheldrick, 1997)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 'SHELXTL and PLATON (Spek, 1996)' _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^)+(0.0571P)^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 constr _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 0.00 _refine_ls_number_reflns 5758 _refine_ls_number_parameters 289 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1005 _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.1404 _refine_ls_wR_factor_gt 0.1236 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.947 _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 Cu1 Cu 0.0000 0.0000 0.82913(3) 0.0283(3) Uani 1 3 d S . . Cu2 Cu 0.6667 0.3333 0.72212(3) 0.0294(3) Uani 1 3 d S . . P1 P 0.0000 0.0000 0.75999(6) 0.0284(5) Uani 1 3 d S . . P2 P 0.6667 0.3333 0.65403(6) 0.0274(5) Uani 1 3 d S . . N1 N 0.0136(3) -0.1323(3) 0.85740(12) 0.0313(9) Uani 1 1 d . . . N2 N 0.1801(3) -0.0830(3) 0.82339(12) 0.0360(9) Uani 1 1 d . . . H12A H 0.1916 -0.0151 0.8225 0.043 Uiso 1 1 calc R . . N3 N 0.5356(3) 0.1908(3) 0.74912(12) 0.0337(10) Uani 1 1 d . . . C1 C -0.1322(4) -0.0247(4) 0.73667(16) 0.0351(12) Uani 1 1 d . . . C2 C -0.1859(5) 0.0289(5) 0.75351(17) 0.0451(13) Uani 1 1 d . . . H2B H -0.1528 0.0784 0.7755 0.054 Uiso 1 1 calc R . . C3 C -0.2871(5) 0.0098(6) 0.7382(2) 0.0600(17) Uani 1 1 d . . . H3A H -0.3234 0.0448 0.7503 0.072 Uiso 1 1 calc R . . C4 C -0.3359(5) -0.0605(6) 0.7049(2) 0.0665(19) Uani 1 1 d . . . H4A H -0.4052 -0.0737 0.6950 0.080 Uiso 1 1 calc R . . C5 C -0.2827(6) -0.1112(6) 0.6865(2) 0.0642(18) Uani 1 1 d . . . H5A H -0.3143 -0.1561 0.6633 0.077 Uiso 1 1 calc R . . C6 C -0.1803(5) -0.0951(5) 0.70265(18) 0.0534(15) Uani 1 1 d . . . H6A H -0.1448 -0.1311 0.6907 0.064 Uiso 1 1 calc R . . C7 C -0.0726(4) -0.2054(4) 0.88153(15) 0.0416(12) Uani 1 1 d . . . H7A H -0.1246 -0.1851 0.8905 0.050 Uiso 1 1 calc R . . C8 C -0.0872(5) -0.3077(5) 0.89345(18) 0.0496(15) Uani 1 1 d . . . H8A H -0.1455 -0.3542 0.9112 0.059 Uiso 1 1 calc R . . C9 C -0.0139(5) -0.3404(5) 0.87870(19) 0.0529(16) Uani 1 1 d . . . H9A H -0.0252 -0.4117 0.8851 0.063 Uiso 1 1 calc R . . C10 C 0.0768(5) -0.2677(4) 0.85437(18) 0.0472(14) Uani 1 1 d . . . H10A H 0.1281 -0.2880 0.8446 0.057 Uiso 1 1 calc R . . C11 C 0.0883(4) -0.1633(4) 0.84502(15) 0.0316(10) Uani 1 1 d . . . C12 C 0.2581(4) -0.1077(4) 0.80208(19) 0.0465(14) Uani 1 1 d . . . H12B H 0.2185 -0.1617 0.7802 0.056 Uiso 1 1 calc R . . H12C H 0.2870 -0.1417 0.8212 0.056 Uiso 1 1 calc R . . C13 C 0.3540(4) -0.0040(4) 0.78419(16) 0.0357(12) Uani 1 1 d . . . C14 C 0.3936(4) -0.0051(4) 0.74520(17) 0.0413(12) Uani 1 1 d . . . H14A H 0.3602 -0.0710 0.7296 0.050 Uiso 1 1 calc R . . C15 C 0.4831(4) 0.0921(4) 0.72959(16) 0.0415(13) Uani 1 1 d . . . H15A H 0.5088 0.0886 0.7034 0.050 Uiso 1 1 calc R . . C16 C 0.4978(4) 0.1906(4) 0.78786(16) 0.0395(12) Uani 1 1 d . . . H16A H 0.5333 0.2569 0.8032 0.047 Uiso 1 1 calc R . . C17 C 0.4090(4) 0.0962(5) 0.80532(17) 0.0461(14) Uani 1 1 d . . . H17A H 0.3859 0.1004 0.8319 0.055 Uiso 1 1 calc R . . C18 C 0.5328(4) 0.2314(4) 0.63125(14) 0.0296(10) Uani 1 1 d . . . C19 C 0.4349(4) 0.2241(5) 0.64673(16) 0.0436(13) Uani 1 1 d . . . H19A H 0.4402 0.2720 0.6680 0.052 Uiso 1 1 calc R . . C20 C 0.3312(4) 0.1485(5) 0.63153(17) 0.0505(15) Uani 1 1 d . . . H20A H 0.2671 0.1471 0.6420 0.061 Uiso 1 1 calc R . . C21 C 0.3206(5) 0.0756(5) 0.6014(2) 0.0588(17) Uani 1 1 d . . . H21A H 0.2498 0.0244 0.5910 0.071 Uiso 1 1 calc R . . C22 C 0.4137(6) 0.0780(6) 0.5866(2) 0.073(2) Uani 1 1 d . . . H22A H 0.4059 0.0258 0.5666 0.087 Uiso 1 1 calc R . . C23 C 0.5201(5) 0.1554(6) 0.60020(19) 0.0595(18) Uani 1 1 d . . . H23A H 0.5833 0.1570 0.5888 0.071 Uiso 1 1 calc R . . Cl1 Cl 0.6667 0.3333 0.90681(11) 0.0560(6) Uani 1 3 d S . . O1 O 0.6667 0.3333 0.8757(6) 0.52(3) Uani 1 3 d S . . O2 O 0.6904(8) 0.2581(7) 0.9216(5) 0.262(8) Uani 1 1 d . . . Cl2 Cl 0.6667 0.3333 0.45180(9) 0.0580(8) Uani 1 3 d S . . C24 C 0.6667 0.3333 0.3298(4) 0.094(5) Uani 1 3 d S . . H24A H 0.6667 0.3333 0.3600 0.113 Uiso 1 3 calc SR . . O4 O 0.6955(6) 0.2568(5) 0.4427(4) 0.200(5) Uani 1 1 d . . . Cl3 Cl 0.5300(2) 0.2369(2) 0.31233(8) 0.1088(8) Uani 1 1 d . . . O3 O 0.6667 0.3333 0.4895(7) 0.313(16) Uani 1 3 d S . . 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 0.0272(3) 0.0272(3) 0.0307(6) 0.000 0.000 0.01358(17) Cu2 0.0304(4) 0.0304(4) 0.0275(6) 0.000 0.000 0.01521(19) P1 0.0289(7) 0.0289(7) 0.0272(12) 0.000 0.000 0.0145(4) P2 0.0262(6) 0.0262(6) 0.0300(12) 0.000 0.000 0.0131(3) N1 0.0178(19) 0.024(2) 0.043(2) 0.0084(17) 0.0068(17) 0.0032(17) N2 0.031(2) 0.023(2) 0.051(2) 0.0106(18) 0.0124(19) 0.0114(18) N3 0.031(2) 0.035(2) 0.032(2) 0.0050(18) 0.0093(18) 0.0141(19) C1 0.032(3) 0.031(3) 0.040(3) 0.002(2) -0.002(2) 0.015(2) C2 0.043(3) 0.055(3) 0.044(3) -0.003(3) -0.006(3) 0.030(3) C3 0.049(4) 0.068(4) 0.073(4) 0.007(4) -0.008(3) 0.037(3) C4 0.041(4) 0.070(5) 0.079(5) 0.007(4) -0.028(3) 0.022(3) C5 0.053(4) 0.067(4) 0.063(4) -0.012(3) -0.034(3) 0.023(3) C6 0.051(4) 0.053(4) 0.059(4) -0.009(3) -0.015(3) 0.028(3) C7 0.041(3) 0.042(3) 0.035(3) 0.011(2) 0.009(2) 0.016(3) C8 0.037(3) 0.045(3) 0.058(3) 0.026(3) 0.016(3) 0.014(3) C9 0.042(3) 0.033(3) 0.080(4) 0.025(3) 0.010(3) 0.016(3) C10 0.041(3) 0.034(3) 0.069(4) 0.009(3) 0.002(3) 0.021(3) C11 0.024(2) 0.023(2) 0.043(3) 0.002(2) 0.001(2) 0.008(2) C12 0.033(3) 0.027(3) 0.075(4) 0.007(3) 0.018(3) 0.012(2) C13 0.030(3) 0.029(3) 0.045(3) 0.006(2) 0.010(2) 0.013(2) C14 0.038(3) 0.031(3) 0.049(3) -0.003(2) 0.001(2) 0.013(2) C15 0.047(3) 0.037(3) 0.038(3) 0.002(2) 0.012(2) 0.020(3) C16 0.030(3) 0.035(3) 0.040(3) -0.004(2) 0.011(2) 0.006(2) C17 0.040(3) 0.042(3) 0.044(3) 0.003(3) 0.018(3) 0.010(3) C18 0.035(3) 0.029(3) 0.027(2) 0.0024(19) 0.0033(19) 0.018(2) C19 0.035(3) 0.048(3) 0.043(3) -0.012(3) 0.001(2) 0.018(3) C20 0.025(3) 0.052(4) 0.063(4) 0.003(3) 0.004(3) 0.010(3) C21 0.040(3) 0.037(3) 0.086(5) -0.014(3) -0.023(3) 0.009(3) C22 0.053(4) 0.061(4) 0.093(5) -0.049(4) -0.020(4) 0.020(3) C23 0.040(3) 0.067(4) 0.068(4) -0.039(3) -0.003(3) 0.025(3) Cl1 0.0445(8) 0.0445(8) 0.0790(17) 0.000 0.000 0.0222(4) O1 0.75(5) 0.75(5) 0.046(9) 0.000 0.000 0.38(3) O2 0.130(7) 0.097(6) 0.59(2) 0.083(11) 0.069(10) 0.079(6) Cl2 0.0447(8) 0.0447(8) 0.085(3) 0.000 0.000 0.0223(4) C24 0.123(8) 0.123(8) 0.037(6) 0.000 0.000 0.061(4) O4 0.085(5) 0.062(4) 0.464(16) 0.005(6) 0.071(7) 0.046(4) Cl3 0.0973(17) 0.1097(19) 0.1016(16) -0.0106(14) 0.0205(13) 0.0385(14) O3 0.41(3) 0.41(3) 0.110(13) 0.000 0.000 0.207(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 2.117(4) 2 ? Cu1 N1 2.117(4) 3 ? Cu1 N1 2.117(4) . ? Cu1 P1 2.245(2) . ? Cu2 N3 2.070(4) 2_655 ? Cu2 N3 2.070(4) . ? Cu2 N3 2.070(4) 3_665 ? Cu2 P2 2.210(2) . ? P1 C1 1.829(5) . ? P1 C1 1.829(5) 3 ? P1 C1 1.829(5) 2 ? P2 C18 1.814(5) 2_655 ? P2 C18 1.814(5) . ? P2 C18 1.814(5) 3_665 ? N1 C11 1.347(6) . ? N1 C7 1.350(6) . ? N2 C11 1.377(6) . ? N2 C12 1.446(6) . ? N3 C15 1.330(7) . ? N3 C16 1.359(6) . ? C1 C2 1.382(7) . ? C1 C6 1.394(7) . ? C2 C3 1.368(8) . ? C3 C4 1.376(10) . ? C4 C5 1.367(10) . ? C5 C6 1.406(8) . ? C7 C8 1.366(7) . ? C8 C9 1.370(8) . ? C9 C10 1.384(8) . ? C10 C11 1.389(7) . ? C12 C13 1.486(7) . ? C13 C17 1.371(7) . ? C13 C14 1.380(7) . ? C14 C15 1.376(7) . ? C16 C17 1.376(7) . ? C18 C19 1.385(7) . ? C18 C23 1.395(7) . ? C19 C20 1.363(7) . ? C20 C21 1.352(8) . ? C21 C22 1.345(9) . ? C22 C23 1.376(9) . ? Cl1 O1 1.009(18) . ? Cl1 O2 1.315(9) . ? Cl1 O2 1.315(9) 2_655 ? Cl1 O2 1.315(9) 3_665 ? Cl2 O3 1.23(2) . ? Cl2 O4 1.323(6) . ? Cl2 O4 1.323(6) 2_655 ? Cl2 O4 1.323(6) 3_665 ? C24 Cl3 1.757(5) 2_655 ? C24 Cl3 1.757(5) . ? C24 Cl3 1.757(5) 3_665 ? 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 N1 Cu1 N1 102.60(13) 2 3 ? N1 Cu1 N1 102.60(13) 2 . ? N1 Cu1 N1 102.60(13) 3 . ? N1 Cu1 P1 115.69(11) 2 . ? N1 Cu1 P1 115.69(11) 3 . ? N1 Cu1 P1 115.69(11) . . ? N3 Cu2 N3 103.35(14) 2_655 . ? N3 Cu2 N3 103.35(14) 2_655 3_665 ? N3 Cu2 N3 103.35(14) . 3_665 ? N3 Cu2 P2 115.06(12) 2_655 . ? N3 Cu2 P2 115.06(12) . . ? N3 Cu2 P2 115.06(12) 3_665 . ? C1 P1 C1 104.1(2) . 3 ? C1 P1 C1 104.1(2) . 2 ? C1 P1 C1 104.1(2) 3 2 ? C1 P1 Cu1 114.46(17) . . ? C1 P1 Cu1 114.46(17) 3 . ? C1 P1 Cu1 114.46(17) 2 . ? C18 P2 C18 104.50(18) 2_655 . ? C18 P2 C18 104.50(18) 2_655 3_665 ? C18 P2 C18 104.50(18) . 3_665 ? C18 P2 Cu2 114.07(15) 2_655 . ? C18 P2 Cu2 114.07(15) . . ? C18 P2 Cu2 114.07(15) 3_665 . ? C11 N1 C7 117.3(4) . . ? C11 N1 Cu1 122.9(3) . . ? C7 N1 Cu1 117.9(3) . . ? C11 N2 C12 122.9(4) . . ? C15 N3 C16 115.3(4) . . ? C15 N3 Cu2 121.8(3) . . ? C16 N3 Cu2 122.9(4) . . ? C2 C1 C6 119.2(5) . . ? C2 C1 P1 118.4(4) . . ? C6 C1 P1 122.4(4) . . ? C3 C2 C1 120.6(6) . . ? C2 C3 C4 120.6(6) . . ? C5 C4 C3 120.2(6) . . ? C4 C5 C6 119.8(6) . . ? C1 C6 C5 119.5(6) . . ? N1 C7 C8 123.3(5) . . ? C7 C8 C9 118.6(5) . . ? C8 C9 C10 120.2(5) . . ? C9 C10 C11 117.6(5) . . ? N1 C11 N2 115.7(4) . . ? N1 C11 C10 122.9(4) . . ? N2 C11 C10 121.3(4) . . ? N2 C12 C13 111.5(4) . . ? C17 C13 C14 116.6(4) . . ? C17 C13 C12 122.6(5) . . ? C14 C13 C12 120.8(5) . . ? C15 C14 C13 119.4(5) . . ? N3 C15 C14 124.9(5) . . ? N3 C16 C17 122.6(5) . . ? C13 C17 C16 121.1(5) . . ? C19 C18 C23 116.9(5) . . ? C19 C18 P2 118.3(4) . . ? C23 C18 P2 124.7(4) . . ? C20 C19 C18 121.6(5) . . ? C21 C20 C19 120.5(5) . . ? C22 C21 C20 119.4(5) . . ? C21 C22 C23 121.8(6) . . ? C22 C23 C18 119.7(5) . . ? O1 Cl1 O2 111.4(7) . . ? O1 Cl1 O2 111.4(8) . 2_655 ? O2 Cl1 O2 107.5(8) . 2_655 ? O1 Cl1 O2 111.4(8) . 3_665 ? O2 Cl1 O2 107.5(8) . 3_665 ? O2 Cl1 O2 107.5(8) 2_655 3_665 ? O3 Cl2 O4 102.9(6) . . ? O3 Cl2 O4 102.9(6) . 2_655 ? O4 Cl2 O4 115.2(4) . 2_655 ? O3 Cl2 O4 102.9(6) . 3_665 ? O4 Cl2 O4 115.2(4) . 3_665 ? O4 Cl2 O4 115.2(4) 2_655 3_665 ? Cl3 C24 Cl3 110.1(4) 2_655 . ? Cl3 C24 Cl3 110.1(4) 2_655 3_665 ? Cl3 C24 Cl3 110.1(4) . 3_665 ? 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 P1 C1 -125.3(2) 2 . . . ? N1 Cu1 P1 C1 -5.3(2) 3 . . . ? N1 Cu1 P1 C1 114.7(2) . . . . ? N1 Cu1 P1 C1 -5.3(2) 2 . . 3 ? N1 Cu1 P1 C1 114.7(2) 3 . . 3 ? N1 Cu1 P1 C1 -125.3(2) . . . 3 ? N1 Cu1 P1 C1 114.7(2) 2 . . 2 ? N1 Cu1 P1 C1 -125.3(2) 3 . . 2 ? N1 Cu1 P1 C1 -5.3(2) . . . 2 ? N3 Cu2 P2 C18 17.3(2) 2_655 . . 2_655 ? N3 Cu2 P2 C18 -102.7(2) . . . 2_655 ? N3 Cu2 P2 C18 137.3(2) 3_665 . . 2_655 ? N3 Cu2 P2 C18 137.3(2) 2_655 . . . ? N3 Cu2 P2 C18 17.3(2) . . . . ? N3 Cu2 P2 C18 -102.7(2) 3_665 . . . ? N3 Cu2 P2 C18 -102.7(2) 2_655 . . 3_665 ? N3 Cu2 P2 C18 137.3(2) . . . 3_665 ? N3 Cu2 P2 C18 17.3(2) 3_665 . . 3_665 ? N1 Cu1 N1 C11 -81.7(4) 2 . . . ? N1 Cu1 N1 C11 172.1(3) 3 . . . ? P1 Cu1 N1 C11 45.2(4) . . . . ? N1 Cu1 N1 C7 114.8(3) 2 . . . ? N1 Cu1 N1 C7 8.6(4) 3 . . . ? P1 Cu1 N1 C7 -118.3(3) . . . . ? N3 Cu2 N3 C15 -101.7(5) 2_655 . . . ? N3 Cu2 N3 C15 150.9(4) 3_665 . . . ? P2 Cu2 N3 C15 24.6(4) . . . . ? N3 Cu2 N3 C16 77.7(4) 2_655 . . . ? N3 Cu2 N3 C16 -29.8(4) 3_665 . . . ? P2 Cu2 N3 C16 -156.1(4) . . . . ? C1 P1 C1 C2 -83.4(6) 3 . . . ? C1 P1 C1 C2 167.9(4) 2 . . . ? Cu1 P1 C1 C2 42.3(5) . . . . ? C1 P1 C1 C6 96.5(4) 3 . . . ? C1 P1 C1 C6 -12.3(5) 2 . . . ? Cu1 P1 C1 C6 -137.9(4) . . . . ? C6 C1 C2 C3 2.7(9) . . . . ? P1 C1 C2 C3 -177.5(5) . . . . ? C1 C2 C3 C4 -1.9(10) . . . . ? C2 C3 C4 C5 -0.9(10) . . . . ? C3 C4 C5 C6 2.7(10) . . . . ? C2 C1 C6 C5 -0.8(9) . . . . ? P1 C1 C6 C5 179.4(4) . . . . ? C4 C5 C6 C1 -1.9(9) . . . . ? C11 N1 C7 C8 -0.4(7) . . . . ? Cu1 N1 C7 C8 164.0(4) . . . . ? N1 C7 C8 C9 -3.1(9) . . . . ? C7 C8 C9 C10 4.0(9) . . . . ? C8 C9 C10 C11 -1.4(9) . . . . ? C7 N1 C11 N2 -174.7(4) . . . . ? Cu1 N1 C11 N2 21.7(6) . . . . ? C7 N1 C11 C10 3.2(7) . . . . ? Cu1 N1 C11 C10 -160.4(4) . . . . ? C12 N2 C11 N1 -169.5(5) . . . . ? C12 N2 C11 C10 12.6(7) . . . . ? C9 C10 C11 N1 -2.3(8) . . . . ? C9 C10 C11 N2 175.5(5) . . . . ? C11 N2 C12 C13 -175.5(5) . . . . ? N2 C12 C13 C17 43.4(7) . . . . ? N2 C12 C13 C14 -137.9(5) . . . . ? C17 C13 C14 C15 -0.8(8) . . . . ? C12 C13 C14 C15 -179.6(5) . . . . ? C16 N3 C15 C14 2.4(8) . . . . ? Cu2 N3 C15 C14 -178.2(4) . . . . ? C13 C14 C15 N3 -1.0(8) . . . . ? C15 N3 C16 C17 -2.1(8) . . . . ? Cu2 N3 C16 C17 178.6(4) . . . . ? C14 C13 C17 C16 1.1(8) . . . . ? C12 C13 C17 C16 179.8(5) . . . . ? N3 C16 C17 C13 0.4(9) . . . . ? C18 P2 C18 C19 171.4(4) 2_655 . . . ? C18 P2 C18 C19 -79.1(5) 3_665 . . . ? Cu2 P2 C18 C19 46.2(4) . . . . ? C18 P2 C18 C23 -5.6(6) 2_655 . . . ? C18 P2 C18 C23 104.0(4) 3_665 . . . ? Cu2 P2 C18 C23 -130.8(5) . . . . ? C23 C18 C19 C20 -1.9(8) . . . . ? P2 C18 C19 C20 -179.1(4) . . . . ? C18 C19 C20 C21 1.9(9) . . . . ? C19 C20 C21 C22 0.3(9) . . . . ? C20 C21 C22 C23 -2.4(11) . . . . ? C21 C22 C23 C18 2.3(12) . . . . ? C19 C18 C23 C22 -0.1(9) . . . . ? P2 C18 C23 C22 176.9(5) . . . . ? _diffrn_measured_fraction_theta_max 0.927 _diffrn_reflns_theta_full 29.56 _diffrn_measured_fraction_theta_full 0.927 _refine_diff_density_max 0.493 _refine_diff_density_min -0.500 _refine_diff_density_rms 0.071