# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Chun-Sen Liu' _publ_contact_author_email CHUNSENLIU@ZZULI.EDU.CN _publ_section_title ; Controllable assembly of copper(I)-iodide coordination polymers by tecton design of benzotriazol-1-yl-based pyridyl ligands: from 2D layer to 3D self-penetrating or homochiral networks ; loop_ _publ_author_name 'Chun-Sen Liu.' 'Miao Du.' 'Shao-Ming Fang.' 'Li-Jun Gao.' 'Min Hu.' ; Guang-Hui Sun ; 'Bo Xiao.' 'Qiang Zhang.' 'Li-Ming Zhaou.' # Attachment 'Complexes_1-3.CIF' data_1 _database_code_depnum_ccdc_archive 'CCDC 755609' #TrackingRef 'Complexes_1-3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H10 Cu I N4' _chemical_formula_weight 400.68 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' 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 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 8.4509(3) _cell_length_b 16.1974(4) _cell_length_c 9.8423(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.324(4) _cell_angle_gamma 90.00 _cell_volume 1292.93(8) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 3455 _cell_measurement_theta_min 3.0751 _cell_measurement_theta_max 26.3149 _exptl_crystal_description BLOCK _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 2.058 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 4.063 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.4299 _exptl_absorpt_correction_T_max 0.5124 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 16.2542 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 8100 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0494 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2266 _reflns_number_gt 1640 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) ; _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^)+(0.0000P)^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_number_reflns 2266 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0407 _refine_ls_R_factor_gt 0.0240 _refine_ls_wR_factor_ref 0.0273 _refine_ls_wR_factor_gt 0.0266 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.003 _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 0.57245(5) 1.02879(2) 0.63561(5) 0.03374(13) Uani 1 1 d . . . I1 I 0.25297(3) 1.045548(12) 0.51166(3) 0.03446(8) Uani 1 1 d . . . C1 C 0.7144(5) 0.9962(2) 0.9384(5) 0.0533(13) Uani 1 1 d . . . H1A H 0.7514 1.0496 0.9305 0.064 Uiso 1 1 calc R . . C2 C 0.7616(5) 0.9599(2) 1.0689(4) 0.0628(13) Uani 1 1 d . . . H2A H 0.8294 0.9873 1.1467 0.075 Uiso 1 1 calc R . . C3 C 0.7051(5) 0.8814(2) 1.0808(4) 0.0556(12) Uani 1 1 d . . . H3A H 0.7322 0.8548 1.1680 0.067 Uiso 1 1 calc R . . C4 C 0.6101(5) 0.8433(2) 0.9647(4) 0.0443(11) Uani 1 1 d . . . H4A H 0.5720 0.7900 0.9715 0.053 Uiso 1 1 calc R . . C5 C 0.5696(4) 0.88293(18) 0.8367(4) 0.0250(9) Uani 1 1 d . . . C6 C 0.4706(4) 0.84203(17) 0.7033(4) 0.0329(10) Uani 1 1 d . . . H6A H 0.3962 0.8822 0.6455 0.039 Uiso 1 1 calc R . . H6B H 0.5443 0.8228 0.6502 0.039 Uiso 1 1 calc R . . C7 C 0.2357(4) 0.77454(17) 0.7727(4) 0.0258(9) Uani 1 1 d . . . C8 C 0.1217(5) 0.83700(19) 0.7708(4) 0.0387(11) Uani 1 1 d . . . H8A H 0.1309 0.8892 0.7342 0.046 Uiso 1 1 calc R . . C9 C -0.0040(5) 0.8167(2) 0.8259(4) 0.0518(12) Uani 1 1 d . . . H9A H -0.0824 0.8566 0.8280 0.062 Uiso 1 1 calc R . . C10 C -0.0196(5) 0.7372(2) 0.8799(4) 0.0473(12) Uani 1 1 d . . . H10A H -0.1052 0.7267 0.9198 0.057 Uiso 1 1 calc R . . C11 C 0.0887(5) 0.67540(18) 0.8746(4) 0.0357(10) Uani 1 1 d . . . H11A H 0.0754 0.6223 0.9056 0.043 Uiso 1 1 calc R . . C12 C 0.2203(4) 0.69551(17) 0.8207(4) 0.0247(9) Uani 1 1 d . . . N1 N 0.6192(3) 0.96089(15) 0.8214(3) 0.0306(7) Uani 1 1 d . . . N2 N 0.3755(3) 0.77259(14) 0.7316(3) 0.0274(8) Uani 1 1 d . . . N3 N 0.4450(3) 0.69672(14) 0.7547(3) 0.0331(8) Uani 1 1 d . . . N4 N 0.3508(3) 0.64939(13) 0.8063(3) 0.0294(8) 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 0.0424(3) 0.0209(2) 0.0406(3) 0.0005(2) 0.0161(3) -0.0004(2) I1 0.03205(14) 0.03154(11) 0.04218(17) -0.00422(14) 0.01434(13) 0.00677(14) C1 0.080(4) 0.028(2) 0.046(3) -0.004(2) 0.008(3) -0.010(2) C2 0.087(4) 0.052(3) 0.039(3) -0.010(3) 0.000(3) -0.014(3) C3 0.067(4) 0.067(3) 0.029(3) 0.016(2) 0.007(3) -0.005(3) C4 0.056(3) 0.042(2) 0.031(3) 0.008(2) 0.007(3) -0.012(2) C5 0.028(2) 0.0249(18) 0.026(2) 0.0021(17) 0.013(2) 0.0018(17) C6 0.043(3) 0.0224(18) 0.036(3) 0.0047(18) 0.017(2) -0.0046(17) C7 0.029(2) 0.0186(18) 0.030(2) -0.0019(17) 0.008(2) -0.0013(18) C8 0.039(3) 0.0213(19) 0.056(3) 0.0065(19) 0.013(3) 0.0036(18) C9 0.042(3) 0.033(2) 0.083(4) 0.002(2) 0.022(3) 0.014(2) C10 0.034(3) 0.046(2) 0.068(3) 0.007(2) 0.025(3) 0.004(2) C11 0.037(3) 0.0227(19) 0.048(3) 0.0028(18) 0.013(2) 0.0010(18) C12 0.030(2) 0.0157(17) 0.028(2) 0.0010(16) 0.008(2) -0.0010(16) N1 0.041(2) 0.0196(14) 0.033(2) -0.0040(15) 0.0122(17) -0.0033(15) N2 0.036(2) 0.0144(14) 0.034(2) 0.0050(13) 0.0127(18) -0.0029(14) N3 0.038(2) 0.0200(15) 0.047(2) 0.0038(15) 0.022(2) 0.0053(14) N4 0.035(2) 0.0163(14) 0.043(2) 0.0083(14) 0.0213(19) 0.0029(14) _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 2.075(3) . ? Cu1 N4 2.087(2) 2_656 ? Cu1 I1 2.6325(4) 3_676 ? Cu1 I1 2.6457(6) . ? Cu1 Cu1 2.7673(9) 3_676 ? I1 Cu1 2.6325(4) 3_676 ? C1 N1 1.334(4) . ? C1 C2 1.366(5) . ? C1 H1A 0.9300 . ? C2 C3 1.376(5) . ? C2 H2A 0.9300 . ? C3 C4 1.347(5) . ? C3 H3A 0.9300 . ? C4 C5 1.369(4) . ? C4 H4A 0.9300 . ? C5 N1 1.352(3) . ? C5 C6 1.499(4) . ? C6 N2 1.454(3) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N2 1.352(4) . ? C7 C12 1.383(4) . ? C7 C8 1.393(4) . ? C8 C9 1.362(4) . ? C8 H8A 0.9300 . ? C9 C10 1.415(4) . ? C9 H9A 0.9300 . ? C10 C11 1.367(4) . ? C10 H10A 0.9300 . ? C11 C12 1.399(4) . ? C11 H11A 0.9300 . ? C12 N4 1.372(3) . ? N2 N3 1.353(3) . ? N3 N4 1.307(3) . ? N4 Cu1 2.087(2) 2_646 ? 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 N4 106.70(11) . 2_656 ? N1 Cu1 I1 104.21(7) . 3_676 ? N4 Cu1 I1 113.55(7) 2_656 3_676 ? N1 Cu1 I1 112.19(7) . . ? N4 Cu1 I1 103.22(8) 2_656 . ? I1 Cu1 I1 116.760(17) 3_676 . ? N1 Cu1 Cu1 126.49(8) . 3_676 ? N4 Cu1 Cu1 126.79(8) 2_656 3_676 ? I1 Cu1 Cu1 58.612(15) 3_676 3_676 ? I1 Cu1 Cu1 58.148(17) . 3_676 ? Cu1 I1 Cu1 63.240(17) 3_676 . ? N1 C1 C2 125.0(3) . . ? N1 C1 H1A 117.5 . . ? C2 C1 H1A 117.5 . . ? C1 C2 C3 117.5(4) . . ? C1 C2 H2A 121.3 . . ? C3 C2 H2A 121.3 . . ? C4 C3 C2 119.3(4) . . ? C4 C3 H3A 120.3 . . ? C2 C3 H3A 120.3 . . ? C3 C4 C5 120.1(4) . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? N1 C5 C4 122.4(3) . . ? N1 C5 C6 115.4(3) . . ? C4 C5 C6 122.2(3) . . ? N2 C6 C5 112.1(3) . . ? N2 C6 H6A 109.2 . . ? C5 C6 H6A 109.2 . . ? N2 C6 H6B 109.2 . . ? C5 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? N2 C7 C12 104.8(3) . . ? N2 C7 C8 132.2(3) . . ? C12 C7 C8 123.0(3) . . ? C9 C8 C7 115.7(3) . . ? C9 C8 H8A 122.2 . . ? C7 C8 H8A 122.2 . . ? C8 C9 C10 122.3(3) . . ? C8 C9 H9A 118.8 . . ? C10 C9 H9A 118.8 . . ? C11 C10 C9 121.2(3) . . ? C11 C10 H10A 119.4 . . ? C9 C10 H10A 119.4 . . ? C10 C11 C12 117.2(3) . . ? C10 C11 H11A 121.4 . . ? C12 C11 H11A 121.4 . . ? N4 C12 C7 108.2(3) . . ? N4 C12 C11 131.3(3) . . ? C7 C12 C11 120.4(3) . . ? C1 N1 C5 115.8(3) . . ? C1 N1 Cu1 116.9(2) . . ? C5 N1 Cu1 127.2(2) . . ? C7 N2 N3 110.2(2) . . ? C7 N2 C6 128.0(3) . . ? N3 N2 C6 119.8(3) . . ? N4 N3 N2 108.3(2) . . ? N3 N4 C12 108.4(2) . . ? N3 N4 Cu1 118.6(2) . 2_646 ? C12 N4 Cu1 132.7(2) . 2_646 ? 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 I1 Cu1 -120.18(8) . . . 3_676 ? N4 Cu1 I1 Cu1 125.33(8) 2_656 . . 3_676 ? I1 Cu1 I1 Cu1 0.0 3_676 . . 3_676 ? N1 C1 C2 C3 -0.8(6) . . . . ? C1 C2 C3 C4 1.4(6) . . . . ? C2 C3 C4 C5 -0.5(6) . . . . ? C3 C4 C5 N1 -1.2(5) . . . . ? C3 C4 C5 C6 177.3(4) . . . . ? N1 C5 C6 N2 -160.2(3) . . . . ? C4 C5 C6 N2 21.2(4) . . . . ? N2 C7 C8 C9 -178.1(4) . . . . ? C12 C7 C8 C9 3.0(6) . . . . ? C7 C8 C9 C10 -0.8(6) . . . . ? C8 C9 C10 C11 -2.4(6) . . . . ? C9 C10 C11 C12 3.4(6) . . . . ? N2 C7 C12 N4 -0.1(4) . . . . ? C8 C7 C12 N4 179.1(3) . . . . ? N2 C7 C12 C11 178.8(3) . . . . ? C8 C7 C12 C11 -2.0(5) . . . . ? C10 C11 C12 N4 177.3(4) . . . . ? C10 C11 C12 C7 -1.3(5) . . . . ? C2 C1 N1 C5 -0.8(5) . . . . ? C2 C1 N1 Cu1 -178.2(3) . . . . ? C4 C5 N1 C1 1.8(5) . . . . ? C6 C5 N1 C1 -176.7(3) . . . . ? C4 C5 N1 Cu1 178.8(2) . . . . ? C6 C5 N1 Cu1 0.3(4) . . . . ? N4 Cu1 N1 C1 -12.6(3) 2_656 . . . ? I1 Cu1 N1 C1 107.8(3) 3_676 . . . ? I1 Cu1 N1 C1 -124.9(3) . . . . ? Cu1 Cu1 N1 C1 169.1(2) 3_676 . . . ? N4 Cu1 N1 C5 170.5(2) 2_656 . . . ? I1 Cu1 N1 C5 -69.1(2) 3_676 . . . ? I1 Cu1 N1 C5 58.1(3) . . . . ? Cu1 Cu1 N1 C5 -7.9(3) 3_676 . . . ? C12 C7 N2 N3 -0.9(4) . . . . ? C8 C7 N2 N3 -179.9(4) . . . . ? C12 C7 N2 C6 -164.6(3) . . . . ? C8 C7 N2 C6 16.4(6) . . . . ? C5 C6 N2 C7 75.3(4) . . . . ? C5 C6 N2 N3 -87.0(3) . . . . ? C7 N2 N3 N4 1.6(4) . . . . ? C6 N2 N3 N4 166.8(3) . . . . ? N2 N3 N4 C12 -1.6(3) . . . . ? N2 N3 N4 Cu1 -176.9(2) . . . 2_646 ? C7 C12 N4 N3 1.1(4) . . . . ? C11 C12 N4 N3 -177.7(4) . . . . ? C7 C12 N4 Cu1 175.5(2) . . . 2_646 ? C11 C12 N4 Cu1 -3.3(6) . . . 2_646 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.603 _refine_diff_density_min -0.337 _refine_diff_density_rms 0.078 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 755610' #TrackingRef 'Complexes_1-3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H10 Cu2 I2 N4' _chemical_formula_weight 591.12 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 11.8984(13) _cell_length_b 16.3498(17) _cell_length_c 15.6505(17) _cell_angle_alpha 90.00 _cell_angle_beta 95.5310(10) _cell_angle_gamma 90.00 _cell_volume 3030.4(6) _cell_formula_units_Z 8 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 4864 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 27.99 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.591 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2192 _exptl_absorpt_coefficient_mu 6.875 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2566 _exptl_absorpt_correction_T_max 0.3812 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 9615 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0264 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2669 _reflns_number_gt 2391 _reflns_threshold_expression i>2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+43.6100P] 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_number_reflns 2669 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0396 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0978 _refine_ls_wR_factor_gt 0.0954 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.27192(8) -0.20736(5) 0.08381(7) 0.0403(2) Uani 1 1 d . . . Cu2 Cu 0.09179(8) -0.04542(6) 0.01718(7) 0.0433(3) Uani 1 1 d . . . I1 I 0.07170(4) -0.21030(3) -0.00631(3) 0.03270(15) Uani 1 1 d . . . I2 I -0.05457(4) -0.02800(3) 0.13041(3) 0.03920(16) Uani 1 1 d . . . C1 C 0.4314(6) -0.0601(4) 0.1104(5) 0.0306(15) Uani 1 1 d . . . C2 C 0.5320(6) -0.1016(5) 0.1411(5) 0.0391(17) Uani 1 1 d . . . H2A H 0.5331 -0.1577 0.1511 0.047 Uiso 1 1 calc R . . C3 C 0.6266(6) -0.0551(5) 0.1551(6) 0.047(2) Uani 1 1 d . . . H3A H 0.6942 -0.0803 0.1750 0.057 Uiso 1 1 calc R . . C4 C 0.6257(7) 0.0299(5) 0.1405(6) 0.051(2) Uani 1 1 d . . . H4A H 0.6931 0.0587 0.1501 0.062 Uiso 1 1 calc R . . C5 C 0.5290(7) 0.0718(5) 0.1127(6) 0.0452(19) Uani 1 1 d . . . H5A H 0.5285 0.1281 0.1038 0.054 Uiso 1 1 calc R . . C6 C 0.4315(6) 0.0243(4) 0.0987(5) 0.0316(15) Uani 1 1 d . . . C7 C 0.2724(7) 0.1239(4) 0.0548(5) 0.0354(16) Uani 1 1 d . . . H7A H 0.1991 0.1182 0.0224 0.042 Uiso 1 1 calc R . . H7B H 0.3201 0.1562 0.0208 0.042 Uiso 1 1 calc R . . C8 C 0.2589(6) 0.1678(4) 0.1387(5) 0.0300(15) Uani 1 1 d . . . C9 C 0.1771(6) 0.1428(4) 0.1901(5) 0.0369(17) Uani 1 1 d . . . H9A H 0.1281 0.1003 0.1727 0.044 Uiso 1 1 calc R . . C10 C 0.1691(6) 0.1814(5) 0.2670(5) 0.0374(17) Uani 1 1 d . . . H10A H 0.1123 0.1648 0.3000 0.045 Uiso 1 1 calc R . . C11 C 0.3151(7) 0.2676(5) 0.2474(5) 0.0405(18) Uani 1 1 d . . . H11A H 0.3624 0.3106 0.2660 0.049 Uiso 1 1 calc R . . C12 C 0.3277(7) 0.2325(4) 0.1673(5) 0.0403(18) Uani 1 1 d . . . H12A H 0.3818 0.2524 0.1336 0.048 Uiso 1 1 calc R . . N1 N 0.2389(5) 0.2423(3) 0.2978(4) 0.0311(13) Uani 1 1 d . . . N2 N 0.3244(5) -0.0886(3) 0.0900(4) 0.0284(12) Uani 1 1 d . . . N3 N 0.2591(5) -0.0259(3) 0.0664(4) 0.0299(13) Uani 1 1 d . . . N4 N 0.3228(5) 0.0427(3) 0.0706(4) 0.0294(12) 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 0.0397(5) 0.0332(5) 0.0483(6) 0.0108(4) 0.0061(4) -0.0006(4) Cu2 0.0367(5) 0.0441(5) 0.0497(6) 0.0040(4) 0.0068(4) 0.0065(4) I1 0.0301(2) 0.0279(2) 0.0406(3) -0.00050(19) 0.00605(19) 0.00154(17) I2 0.0393(3) 0.0402(3) 0.0392(3) 0.0002(2) 0.0093(2) 0.0000(2) C1 0.027(3) 0.033(4) 0.032(4) -0.004(3) 0.005(3) -0.002(3) C2 0.035(4) 0.038(4) 0.044(5) 0.001(3) 0.002(3) 0.008(3) C3 0.027(4) 0.056(5) 0.058(6) -0.006(4) -0.001(4) 0.004(3) C4 0.034(4) 0.056(5) 0.064(6) -0.012(4) 0.002(4) -0.012(4) C5 0.042(4) 0.037(4) 0.057(5) -0.006(4) 0.007(4) -0.012(3) C6 0.036(4) 0.032(4) 0.028(4) -0.004(3) 0.006(3) -0.004(3) C7 0.046(4) 0.027(3) 0.033(4) 0.000(3) 0.002(3) 0.003(3) C8 0.030(3) 0.027(3) 0.033(4) 0.001(3) 0.000(3) 0.004(3) C9 0.035(4) 0.031(4) 0.044(5) -0.010(3) 0.001(3) -0.009(3) C10 0.033(4) 0.039(4) 0.041(4) -0.001(3) 0.006(3) -0.008(3) C11 0.046(4) 0.031(4) 0.046(5) -0.008(3) 0.009(4) -0.012(3) C12 0.046(4) 0.033(4) 0.044(5) -0.006(3) 0.016(4) -0.009(3) N1 0.034(3) 0.028(3) 0.031(3) -0.004(2) 0.004(3) 0.002(2) N2 0.028(3) 0.024(3) 0.033(3) 0.005(2) 0.004(2) 0.003(2) N3 0.027(3) 0.025(3) 0.037(3) 0.000(2) 0.001(2) 0.002(2) N4 0.034(3) 0.024(3) 0.031(3) -0.004(2) 0.007(2) 0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N2 2.039(5) . ? Cu1 N1 2.042(6) 4_545 ? Cu1 I1 2.6494(11) . ? Cu1 I1 2.6798(11) 7_545 ? Cu1 Cu1 2.972(2) 7_545 ? Cu2 N3 2.089(6) . ? Cu2 I2 2.6029(12) 5 ? Cu2 I2 2.6171(11) . ? Cu2 Cu2 2.6533(19) 5 ? Cu2 I1 2.7281(11) . ? I1 Cu1 2.6798(11) 7_545 ? I2 Cu2 2.6029(12) 5 ? C1 N2 1.364(9) . ? C1 C6 1.392(10) . ? C1 C2 1.419(10) . ? C2 C3 1.358(11) . ? C2 H2A 0.9300 . ? C3 C4 1.408(12) . ? C3 H3A 0.9300 . ? C4 C5 1.374(12) . ? C4 H4A 0.9300 . ? C5 C6 1.396(10) . ? C5 H5A 0.9300 . ? C6 N4 1.359(9) . ? C7 N4 1.468(9) . ? C7 C8 1.518(10) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.384(10) . ? C8 C12 1.385(10) . ? C9 C10 1.370(11) . ? C9 H9A 0.9300 . ? C10 N1 1.356(9) . ? C10 H10A 0.9300 . ? C11 N1 1.324(10) . ? C11 C12 1.399(11) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? N1 Cu1 2.042(6) 4 ? N2 N3 1.318(8) . ? N3 N4 1.351(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 N2 Cu1 N1 112.8(2) . 4_545 ? N2 Cu1 I1 107.34(16) . . ? N1 Cu1 I1 110.08(16) 4_545 . ? N2 Cu1 I1 106.07(16) . 7_545 ? N1 Cu1 I1 108.39(17) 4_545 7_545 ? I1 Cu1 I1 112.20(4) . 7_545 ? N2 Cu1 Cu1 121.01(17) . 7_545 ? N1 Cu1 Cu1 126.19(17) 4_545 7_545 ? I1 Cu1 Cu1 56.59(3) . 7_545 ? I1 Cu1 Cu1 55.62(3) 7_545 7_545 ? N3 Cu2 I2 109.35(17) . 5 ? N3 Cu2 I2 113.97(17) . . ? I2 Cu2 I2 118.90(4) 5 . ? N3 Cu2 Cu2 136.53(16) . 5 ? I2 Cu2 Cu2 59.71(4) 5 5 ? I2 Cu2 Cu2 59.19(4) . 5 ? N3 Cu2 I1 105.61(15) . . ? I2 Cu2 I1 109.32(4) 5 . ? I2 Cu2 I1 98.24(4) . . ? Cu2 Cu2 I1 117.78(6) 5 . ? Cu1 I1 Cu1 67.80(4) . 7_545 ? Cu1 I1 Cu2 81.24(3) . . ? Cu1 I1 Cu2 120.12(3) 7_545 . ? Cu2 I2 Cu2 61.10(4) 5 . ? N2 C1 C6 108.7(6) . . ? N2 C1 C2 130.8(7) . . ? C6 C1 C2 120.5(7) . . ? C3 C2 C1 116.4(7) . . ? C3 C2 H2A 121.8 . . ? C1 C2 H2A 121.8 . . ? C2 C3 C4 122.2(7) . . ? C2 C3 H3A 118.9 . . ? C4 C3 H3A 118.9 . . ? C5 C4 C3 122.5(7) . . ? C5 C4 H4A 118.8 . . ? C3 C4 H4A 118.8 . . ? C4 C5 C6 115.5(7) . . ? C4 C5 H5A 122.3 . . ? C6 C5 H5A 122.3 . . ? N4 C6 C1 104.4(6) . . ? N4 C6 C5 132.7(7) . . ? C1 C6 C5 122.9(7) . . ? N4 C7 C8 110.9(6) . . ? N4 C7 H7A 109.5 . . ? C8 C7 H7A 109.5 . . ? N4 C7 H7B 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 108.0 . . ? C9 C8 C12 117.7(7) . . ? C9 C8 C7 120.1(6) . . ? C12 C8 C7 122.2(6) . . ? C10 C9 C8 119.1(6) . . ? C10 C9 H9A 120.4 . . ? C8 C9 H9A 120.4 . . ? N1 C10 C9 124.0(7) . . ? N1 C10 H10A 118.0 . . ? C9 C10 H10A 118.0 . . ? N1 C11 C12 123.0(7) . . ? N1 C11 H11A 118.5 . . ? C12 C11 H11A 118.5 . . ? C8 C12 C11 119.5(7) . . ? C8 C12 H12A 120.3 . . ? C11 C12 H12A 120.3 . . ? C11 N1 C10 116.6(6) . . ? C11 N1 Cu1 121.5(5) . 4 ? C10 N1 Cu1 121.9(5) . 4 ? N3 N2 C1 108.1(5) . . ? N3 N2 Cu1 123.9(4) . . ? C1 N2 Cu1 127.7(4) . . ? N2 N3 N4 108.6(5) . . ? N2 N3 Cu2 120.0(4) . . ? N4 N3 Cu2 130.9(4) . . ? N3 N4 C6 110.1(5) . . ? N3 N4 C7 121.6(6) . . ? C6 N4 C7 128.0(6) . . ? 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 N2 Cu1 I1 Cu1 116.14(18) . . . 7_545 ? N1 Cu1 I1 Cu1 -120.79(18) 4_545 . . 7_545 ? I1 Cu1 I1 Cu1 0.0 7_545 . . 7_545 ? N2 Cu1 I1 Cu2 -11.54(17) . . . . ? N1 Cu1 I1 Cu2 111.53(18) 4_545 . . . ? I1 Cu1 I1 Cu2 -127.68(4) 7_545 . . . ? Cu1 Cu1 I1 Cu2 -127.68(4) 7_545 . . . ? N3 Cu2 I1 Cu1 11.05(18) . . . . ? I2 Cu2 I1 Cu1 128.60(4) 5 . . . ? I2 Cu2 I1 Cu1 -106.77(4) . . . . ? Cu2 Cu2 I1 Cu1 -166.19(7) 5 . . . ? N3 Cu2 I1 Cu1 -46.85(18) . . . 7_545 ? I2 Cu2 I1 Cu1 70.70(5) 5 . . 7_545 ? I2 Cu2 I1 Cu1 -164.67(3) . . . 7_545 ? Cu2 Cu2 I1 Cu1 135.91(6) 5 . . 7_545 ? N3 Cu2 I2 Cu2 131.27(17) . . . 5 ? I2 Cu2 I2 Cu2 0.0 5 . . 5 ? I1 Cu2 I2 Cu2 -117.51(6) . . . 5 ? N2 C1 C2 C3 179.7(8) . . . . ? C6 C1 C2 C3 -2.1(11) . . . . ? C1 C2 C3 C4 0.3(13) . . . . ? C2 C3 C4 C5 1.2(15) . . . . ? C3 C4 C5 C6 -0.8(13) . . . . ? N2 C1 C6 N4 -0.5(8) . . . . ? C2 C1 C6 N4 -179.0(7) . . . . ? N2 C1 C6 C5 -178.8(7) . . . . ? C2 C1 C6 C5 2.6(11) . . . . ? C4 C5 C6 N4 -178.9(8) . . . . ? C4 C5 C6 C1 -1.1(12) . . . . ? N4 C7 C8 C9 -72.3(8) . . . . ? N4 C7 C8 C12 106.7(8) . . . . ? C12 C8 C9 C10 -1.3(11) . . . . ? C7 C8 C9 C10 177.7(7) . . . . ? C8 C9 C10 N1 -1.7(12) . . . . ? C9 C8 C12 C11 2.4(11) . . . . ? C7 C8 C12 C11 -176.6(7) . . . . ? N1 C11 C12 C8 -0.6(12) . . . . ? C12 C11 N1 C10 -2.3(11) . . . . ? C12 C11 N1 Cu1 177.6(6) . . . 4 ? C9 C10 N1 C11 3.5(11) . . . . ? C9 C10 N1 Cu1 -176.3(6) . . . 4 ? C6 C1 N2 N3 0.0(8) . . . . ? C2 C1 N2 N3 178.3(7) . . . . ? C6 C1 N2 Cu1 174.2(5) . . . . ? C2 C1 N2 Cu1 -7.4(11) . . . . ? N1 Cu1 N2 N3 -110.2(5) 4_545 . . . ? I1 Cu1 N2 N3 11.2(6) . . . . ? I1 Cu1 N2 N3 131.3(5) 7_545 . . . ? Cu1 Cu1 N2 N3 72.2(5) 7_545 . . . ? N1 Cu1 N2 C1 76.4(6) 4_545 . . . ? I1 Cu1 N2 C1 -162.2(5) . . . . ? I1 Cu1 N2 C1 -42.1(6) 7_545 . . . ? Cu1 Cu1 N2 C1 -101.3(6) 7_545 . . . ? C1 N2 N3 N4 0.5(7) . . . . ? Cu1 N2 N3 N4 -174.0(4) . . . . ? C1 N2 N3 Cu2 173.3(4) . . . . ? Cu1 N2 N3 Cu2 -1.2(7) . . . . ? I2 Cu2 N3 N2 -126.6(5) 5 . . . ? I2 Cu2 N3 N2 97.6(5) . . . . ? Cu2 Cu2 N3 N2 167.4(4) 5 . . . ? I1 Cu2 N3 N2 -9.0(5) . . . . ? I2 Cu2 N3 N4 44.4(6) 5 . . . ? I2 Cu2 N3 N4 -91.4(6) . . . . ? Cu2 Cu2 N3 N4 -21.7(7) 5 . . . ? I1 Cu2 N3 N4 161.9(5) . . . . ? N2 N3 N4 C6 -0.9(8) . . . . ? Cu2 N3 N4 C6 -172.6(5) . . . . ? N2 N3 N4 C7 -175.0(6) . . . . ? Cu2 N3 N4 C7 13.2(9) . . . . ? C1 C6 N4 N3 0.8(8) . . . . ? C5 C6 N4 N3 178.9(8) . . . . ? C1 C6 N4 C7 174.5(7) . . . . ? C5 C6 N4 C7 -7.4(13) . . . . ? C8 C7 N4 N3 100.3(7) . . . . ? C8 C7 N4 C6 -72.8(9) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.475 _refine_diff_density_min -1.458 _refine_diff_density_rms 0.163 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 755611' #TrackingRef 'Complexes_1-3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H10 Cu3 I3 N4' _chemical_formula_weight 781.56 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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) 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 7.5406(6) _cell_length_b 12.2655(10) _cell_length_c 18.3740(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1699.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 1529 _cell_measurement_theta_min 3.1638 _cell_measurement_theta_max 30.4623 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 3.055 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 9.169 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1834 _exptl_absorpt_correction_T_max 0.2747 _exptl_absorpt_process_details sadabs _exptl_special_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 16.2542 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4225 _diffrn_reflns_av_R_equivalents 0.0402 _diffrn_reflns_av_sigmaI/netI 0.1097 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 24.98 _reflns_number_total 2772 _reflns_number_gt 1816 _reflns_threshold_expression i>2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _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^)+(0.0205P)^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 0.05(7) _refine_ls_number_reflns 2772 _refine_ls_number_parameters 199 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0846 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.0738 _refine_ls_wR_factor_gt 0.0699 _refine_ls_goodness_of_fit_ref 0.972 _refine_ls_restrained_S_all 0.969 _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 0.5693(3) 0.72363(15) 0.27236(12) 0.0364(6) Uani 1 1 d . . . Cu2 Cu 0.5764(3) 1.00287(16) 0.27993(12) 0.0383(6) Uani 1 1 d . . . Cu3 Cu 0.4156(3) 0.87079(17) 0.17895(10) 0.0327(5) Uani 1 1 d . . . C1 C 0.580(2) 1.0449(11) 0.4709(9) 0.025(4) Uani 1 1 d U . . H1A H 0.6340 1.0897 0.4334 0.030 Uiso 1 1 calc R . . H1B H 0.6517 1.0509 0.5145 0.030 Uiso 1 1 calc R . . C2 C 0.393(2) 1.0864(11) 0.4866(9) 0.018(4) Uani 1 1 d . . . C3 C 0.285(2) 1.1239(13) 0.4310(9) 0.030(4) Uani 1 1 d . . . H3A H 0.3264 1.1271 0.3834 0.036 Uiso 1 1 calc R . . C4 C 0.119(2) 1.1556(13) 0.4467(11) 0.037(5) Uani 1 1 d . . . H4A H 0.0437 1.1794 0.4099 0.044 Uiso 1 1 calc R . . C5 C 0.059(2) 1.1527(11) 0.5194(9) 0.023(4) Uani 1 1 d . . . H5A H -0.0566 1.1733 0.5296 0.028 Uiso 1 1 calc R . . C6 C 0.328(2) 1.0896(10) 0.5574(10) 0.013(4) Uani 1 1 d U . . H6A H 0.4019 1.0684 0.5953 0.016 Uiso 1 1 calc R . . C7 C 0.558(2) 0.8409(13) 0.4883(10) 0.026(4) Uani 1 1 d . . . C8 C 0.553(2) 0.8220(13) 0.5641(10) 0.038(5) Uani 1 1 d U . . H8A H 0.5657 0.8786 0.5974 0.046 Uiso 1 1 calc R . . C9 C 0.529(2) 0.7170(14) 0.5864(11) 0.042(6) Uani 1 1 d . . . H9A H 0.5163 0.7018 0.6357 0.051 Uiso 1 1 calc R . . C10 C 0.522(2) 0.6328(17) 0.5361(10) 0.040(5) Uani 1 1 d . . . H10A H 0.5140 0.5616 0.5532 0.048 Uiso 1 1 calc R . . C11 C 0.527(2) 0.6491(13) 0.4652(9) 0.030(4) Uani 1 1 d . . . H11A H 0.5166 0.5910 0.4330 0.036 Uiso 1 1 calc R . . C12 C 0.547(2) 0.7570(12) 0.4391(10) 0.025(4) Uani 1 1 d . . . N1 N 0.576(2) 0.9308(10) 0.4467(7) 0.025(3) Uani 1 1 d . . . N2 N 0.5724(17) 0.9057(9) 0.3764(7) 0.024(3) Uani 1 1 d . . . N3 N 0.5610(18) 0.7993(8) 0.3704(8) 0.026(3) Uani 1 1 d . . . N4 N 0.1621(16) 1.1220(10) 0.5732(8) 0.025(3) Uani 1 1 d . . . I1 I 0.75897(17) 0.87261(7) 0.19190(5) 0.0275(2) Uani 1 1 d . . . I2 I 0.2449(2) 1.04060(6) 0.23668(5) 0.0270(3) Uani 1 1 d . . . I3 I 0.2473(2) 0.68753(6) 0.21917(5) 0.0286(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0459(14) 0.0341(10) 0.0292(14) -0.0077(11) -0.0036(13) 0.0016(11) Cu2 0.0371(13) 0.0351(10) 0.0426(16) -0.0065(11) 0.0020(13) 0.0003(11) Cu3 0.0373(11) 0.0402(10) 0.0206(12) 0.0025(12) -0.0054(10) 0.0031(13) C1 0.025(4) 0.025(4) 0.025(4) -0.0002(10) 0.0002(10) 0.0000(10) C2 0.029(10) 0.012(7) 0.013(10) -0.002(7) -0.008(9) 0.006(8) C3 0.040(13) 0.031(9) 0.020(9) 0.002(8) 0.016(9) -0.012(10) C4 0.023(10) 0.036(11) 0.052(15) 0.015(10) -0.024(10) 0.001(9) C5 0.035(9) 0.011(9) 0.023(10) 0.004(8) 0.010(9) 0.011(8) C6 0.013(4) 0.013(4) 0.013(4) 0.0001(10) -0.0002(10) 0.0001(10) C7 0.029(9) 0.029(11) 0.021(11) 0.010(9) 0.001(9) 0.010(9) C8 0.038(5) 0.038(5) 0.038(5) 0.0001(10) 0.0001(10) -0.0001(10) C9 0.044(13) 0.057(13) 0.026(14) 0.013(11) 0.002(10) -0.014(10) C10 0.066(14) 0.026(10) 0.028(12) -0.003(12) 0.019(10) 0.012(12) C11 0.047(11) 0.022(9) 0.022(11) 0.003(10) -0.008(9) 0.000(9) C12 0.025(10) 0.025(10) 0.025(12) 0.006(9) -0.006(9) 0.001(8) N1 0.036(9) 0.023(8) 0.015(9) -0.001(7) 0.008(8) 0.012(7) N2 0.026(8) 0.022(7) 0.023(9) -0.009(6) 0.003(7) 0.005(6) N3 0.026(8) 0.017(8) 0.036(10) 0.005(7) -0.001(7) -0.007(7) N4 0.042(8) 0.013(7) 0.019(9) 0.000(7) -0.005(7) 0.005(7) I1 0.0256(5) 0.0287(4) 0.0281(6) -0.0058(5) 0.0060(7) 0.0016(9) I2 0.0277(6) 0.0253(4) 0.0280(6) -0.0048(4) -0.0026(9) 0.0011(7) I3 0.0280(6) 0.0243(4) 0.0334(6) 0.0014(5) -0.0020(10) -0.0011(7) _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 N3 2.027(14) . ? Cu1 I2 2.652(2) 3_645 ? Cu1 I3 2.654(3) . ? Cu1 Cu3 2.747(3) . ? Cu1 I1 2.752(2) . ? Cu2 N2 2.136(13) . ? Cu2 I3 2.626(2) 3_655 ? Cu2 I1 2.658(2) . ? Cu2 I2 2.664(3) . ? Cu2 Cu3 2.745(3) . ? Cu3 N4 2.031(14) 2_574 ? Cu3 I1 2.600(2) . ? Cu3 I2 2.668(2) . ? Cu3 I3 2.685(2) . ? C1 N1 1.469(17) . ? C1 C2 1.53(2) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.39(2) . ? C2 C6 1.39(2) . ? C3 C4 1.34(2) . ? C3 H3A 0.9300 . ? C4 C5 1.41(2) . ? C4 H4A 0.9300 . ? C5 N4 1.311(19) . ? C5 H5A 0.9300 . ? C6 N4 1.343(15) . ? C6 H6A 0.9300 . ? C7 N1 1.348(18) . ? C7 C12 1.37(2) . ? C7 C8 1.41(2) . ? C8 C9 1.363(19) . ? C8 H8A 0.9300 . ? C9 C10 1.39(2) . ? C9 H9A 0.9300 . ? C10 C11 1.32(2) . ? C10 H10A 0.9300 . ? C11 C12 1.42(2) . ? C11 H11A 0.9300 . ? C12 N3 1.37(2) . ? N1 N2 1.328(17) . ? N2 N3 1.313(13) . ? N4 Cu3 2.031(14) 2_575 ? I2 Cu1 2.652(2) 3_655 ? I3 Cu2 2.626(2) 3_645 ? 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 N3 Cu1 I2 117.4(4) . 3_645 ? N3 Cu1 I3 112.0(4) . . ? I2 Cu1 I3 108.61(7) 3_645 . ? N3 Cu1 Cu3 104.0(3) . . ? I2 Cu1 Cu3 137.74(10) 3_645 . ? I3 Cu1 Cu3 59.59(6) . . ? N3 Cu1 I1 100.9(3) . . ? I2 Cu1 I1 104.70(8) 3_645 . ? I3 Cu1 I1 112.86(8) . . ? Cu3 Cu1 I1 56.44(6) . . ? N2 Cu2 I3 118.9(4) . 3_655 ? N2 Cu2 I1 100.2(3) . . ? I3 Cu2 I1 105.07(9) 3_655 . ? N2 Cu2 I2 109.3(4) . . ? I3 Cu2 I2 109.10(8) 3_655 . ? I1 Cu2 I2 114.14(9) . . ? N2 Cu2 Cu3 103.0(3) . . ? I3 Cu2 Cu3 137.45(10) 3_655 . ? I1 Cu2 Cu3 57.50(6) . . ? I2 Cu2 Cu3 59.10(6) . . ? N4 Cu3 I1 112.0(4) 2_574 . ? N4 Cu3 I2 101.9(4) 2_574 . ? I1 Cu3 I2 115.94(8) . . ? N4 Cu3 I3 99.4(4) 2_574 . ? I1 Cu3 I3 116.92(8) . . ? I2 Cu3 I3 108.41(7) . . ? N4 Cu3 Cu2 138.4(4) 2_574 . ? I1 Cu3 Cu2 59.56(6) . . ? I2 Cu3 Cu2 58.92(7) . . ? I3 Cu3 Cu2 121.12(9) . . ? N4 Cu3 Cu1 138.4(4) 2_574 . ? I1 Cu3 Cu1 61.87(7) . . ? I2 Cu3 Cu1 117.91(9) . . ? I3 Cu3 Cu1 58.49(7) . . ? Cu2 Cu3 Cu1 77.25(7) . . ? N1 C1 C2 110.8(13) . . ? N1 C1 H1A 109.5 . . ? C2 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 108.1 . . ? C3 C2 C6 118.1(15) . . ? C3 C2 C1 121.0(15) . . ? C6 C2 C1 120.9(14) . . ? C4 C3 C2 119.1(17) . . ? C4 C3 H3A 120.4 . . ? C2 C3 H3A 120.4 . . ? C3 C4 C5 119.6(17) . . ? C3 C4 H4A 120.2 . . ? C5 C4 H4A 120.2 . . ? N4 C5 C4 122.3(15) . . ? N4 C5 H5A 118.9 . . ? C4 C5 H5A 118.9 . . ? N4 C6 C2 122.7(16) . . ? N4 C6 H6A 118.7 . . ? C2 C6 H6A 118.7 . . ? N1 C7 C12 104.2(16) . . ? N1 C7 C8 134.1(16) . . ? C12 C7 C8 121.7(15) . . ? C9 C8 C7 117.0(17) . . ? C9 C8 H8A 121.5 . . ? C7 C8 H8A 121.5 . . ? C8 C9 C10 120.6(19) . . ? C8 C9 H9A 119.7 . . ? C10 C9 H9A 119.7 . . ? C11 C10 C9 122.9(19) . . ? C11 C10 H10A 118.5 . . ? C9 C10 H10A 118.5 . . ? C10 C11 C12 118.6(17) . . ? C10 C11 H11A 120.7 . . ? C12 C11 H11A 120.7 . . ? N3 C12 C7 108.6(14) . . ? N3 C12 C11 132.4(16) . . ? C7 C12 C11 119.0(16) . . ? N2 N1 C7 111.1(13) . . ? N2 N1 C1 121.0(12) . . ? C7 N1 C1 127.6(14) . . ? N3 N2 N1 108.2(13) . . ? N3 N2 Cu2 119.1(11) . . ? N1 N2 Cu2 132.7(9) . . ? N2 N3 C12 107.7(14) . . ? N2 N3 Cu1 121.9(11) . . ? C12 N3 Cu1 130.4(10) . . ? C5 N4 C6 118.1(16) . . ? C5 N4 Cu3 122.6(11) . 2_575 ? C6 N4 Cu3 119.3(13) . 2_575 ? Cu3 I1 Cu2 62.94(7) . . ? Cu3 I1 Cu1 61.69(7) . . ? Cu2 I1 Cu1 78.64(6) . . ? Cu1 I2 Cu2 70.72(7) 3_655 . ? Cu1 I2 Cu3 112.39(8) 3_655 . ? Cu2 I2 Cu3 61.97(7) . . ? Cu2 I3 Cu1 71.24(7) 3_645 . ? Cu2 I3 Cu3 118.96(8) 3_645 . ? Cu1 I3 Cu3 61.92(7) . . ? 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 N2 Cu2 Cu3 N4 176.6(7) . . . 2_574 ? I3 Cu2 Cu3 N4 -13.3(6) 3_655 . . 2_574 ? I1 Cu2 Cu3 N4 -89.6(6) . . . 2_574 ? I2 Cu2 Cu3 N4 71.6(6) . . . 2_574 ? N2 Cu2 Cu3 I1 -93.9(4) . . . . ? I3 Cu2 Cu3 I1 76.22(14) 3_655 . . . ? I2 Cu2 Cu3 I1 161.16(8) . . . . ? N2 Cu2 Cu3 I2 104.9(4) . . . . ? I3 Cu2 Cu3 I2 -84.94(13) 3_655 . . . ? I1 Cu2 Cu3 I2 -161.16(8) . . . . ? N2 Cu2 Cu3 I3 11.1(4) . . . . ? I3 Cu2 Cu3 I3 -178.79(10) 3_655 . . . ? I1 Cu2 Cu3 I3 105.00(10) . . . . ? I2 Cu2 Cu3 I3 -93.84(9) . . . . ? N2 Cu2 Cu3 Cu1 -29.2(4) . . . . ? I3 Cu2 Cu3 Cu1 140.90(16) 3_655 . . . ? I1 Cu2 Cu3 Cu1 64.68(7) . . . . ? I2 Cu2 Cu3 Cu1 -134.16(9) . . . . ? N3 Cu1 Cu3 N4 -173.9(7) . . . 2_574 ? I2 Cu1 Cu3 N4 18.2(6) 3_645 . . 2_574 ? I3 Cu1 Cu3 N4 -66.3(6) . . . 2_574 ? I1 Cu1 Cu3 N4 92.1(6) . . . 2_574 ? N3 Cu1 Cu3 I1 94.0(4) . . . . ? I2 Cu1 Cu3 I1 -73.91(14) 3_645 . . . ? I3 Cu1 Cu3 I1 -158.43(7) . . . . ? N3 Cu1 Cu3 I2 -12.2(4) . . . . ? I2 Cu1 Cu3 I2 179.94(10) 3_645 . . . ? I3 Cu1 Cu3 I2 95.43(9) . . . . ? I1 Cu1 Cu3 I2 -106.15(10) . . . . ? N3 Cu1 Cu3 I3 -107.6(4) . . . . ? I2 Cu1 Cu3 I3 84.52(14) 3_645 . . . ? I1 Cu1 Cu3 I3 158.43(7) . . . . ? N3 Cu1 Cu3 Cu2 31.9(4) . . . . ? I2 Cu1 Cu3 Cu2 -136.01(16) 3_645 . . . ? I3 Cu1 Cu3 Cu2 139.48(8) . . . . ? I1 Cu1 Cu3 Cu2 -62.10(7) . . . . ? N1 C1 C2 C3 -82.7(18) . . . . ? N1 C1 C2 C6 98.6(16) . . . . ? C6 C2 C3 C4 -4(2) . . . . ? C1 C2 C3 C4 177.4(15) . . . . ? C2 C3 C4 C5 1(3) . . . . ? C3 C4 C5 N4 1(3) . . . . ? C3 C2 C6 N4 4(2) . . . . ? C1 C2 C6 N4 -177.7(13) . . . . ? N1 C7 C8 C9 178.3(18) . . . . ? C12 C7 C8 C9 -3(3) . . . . ? C7 C8 C9 C10 4(3) . . . . ? C8 C9 C10 C11 -5(3) . . . . ? C9 C10 C11 C12 3(3) . . . . ? N1 C7 C12 N3 1.1(19) . . . . ? C8 C7 C12 N3 -178.2(15) . . . . ? N1 C7 C12 C11 -179.7(16) . . . . ? C8 C7 C12 C11 1(3) . . . . ? C10 C11 C12 N3 177.9(18) . . . . ? C10 C11 C12 C7 -1(3) . . . . ? C12 C7 N1 N2 1.0(19) . . . . ? C8 C7 N1 N2 -179.9(17) . . . . ? C12 C7 N1 C1 175.0(16) . . . . ? C8 C7 N1 C1 -6(3) . . . . ? C2 C1 N1 N2 94.4(18) . . . . ? C2 C1 N1 C7 -79(2) . . . . ? C7 N1 N2 N3 -3(2) . . . . ? C1 N1 N2 N3 -177.2(14) . . . . ? C7 N1 N2 Cu2 175.7(11) . . . . ? C1 N1 N2 Cu2 1(2) . . . . ? I3 Cu2 N2 N3 -149.1(11) 3_655 . . . ? I1 Cu2 N2 N3 -35.5(13) . . . . ? I2 Cu2 N2 N3 84.8(12) . . . . ? Cu3 Cu2 N2 N3 23.3(13) . . . . ? I3 Cu2 N2 N1 32.6(16) 3_655 . . . ? I1 Cu2 N2 N1 146.2(14) . . . . ? I2 Cu2 N2 N1 -93.6(15) . . . . ? Cu3 Cu2 N2 N1 -155.1(14) . . . . ? N1 N2 N3 C12 3.4(19) . . . . ? Cu2 N2 N3 C12 -175.4(10) . . . . ? N1 N2 N3 Cu1 -175.7(10) . . . . ? Cu2 N2 N3 Cu1 5.6(18) . . . . ? C7 C12 N3 N2 -2.8(19) . . . . ? C11 C12 N3 N2 178.2(18) . . . . ? C7 C12 N3 Cu1 176.1(11) . . . . ? C11 C12 N3 Cu1 -3(3) . . . . ? I2 Cu1 N3 N2 139.1(11) 3_645 . . . ? I3 Cu1 N3 N2 -94.3(13) . . . . ? Cu3 Cu1 N3 N2 -31.8(14) . . . . ? I1 Cu1 N3 N2 26.0(13) . . . . ? I2 Cu1 N3 C12 -39.7(16) 3_645 . . . ? I3 Cu1 N3 C12 86.9(14) . . . . ? Cu3 Cu1 N3 C12 149.4(14) . . . . ? I1 Cu1 N3 C12 -152.7(14) . . . . ? C4 C5 N4 C6 -2(2) . . . . ? C4 C5 N4 Cu3 174.9(12) . . . 2_575 ? C2 C6 N4 C5 -1(2) . . . . ? C2 C6 N4 Cu3 -177.5(11) . . . 2_575 ? N4 Cu3 I1 Cu2 134.3(4) 2_574 . . . ? I2 Cu3 I1 Cu2 17.91(7) . . . . ? I3 Cu3 I1 Cu2 -111.95(10) . . . . ? Cu1 Cu3 I1 Cu2 -91.37(8) . . . . ? N4 Cu3 I1 Cu1 -134.3(4) 2_574 . . . ? I2 Cu3 I1 Cu1 109.28(9) . . . . ? I3 Cu3 I1 Cu1 -20.58(7) . . . . ? Cu2 Cu3 I1 Cu1 91.37(8) . . . . ? N2 Cu2 I1 Cu3 99.0(4) . . . . ? I3 Cu2 I1 Cu3 -137.15(10) 3_655 . . . ? I2 Cu2 I1 Cu3 -17.67(7) . . . . ? N2 Cu2 I1 Cu1 35.2(4) . . . . ? I3 Cu2 I1 Cu1 158.99(10) 3_655 . . . ? I2 Cu2 I1 Cu1 -81.54(9) . . . . ? Cu3 Cu2 I1 Cu1 -63.86(8) . . . . ? N3 Cu1 I1 Cu3 -99.6(4) . . . . ? I2 Cu1 I1 Cu3 138.08(10) 3_645 . . . ? I3 Cu1 I1 Cu3 20.13(7) . . . . ? N3 Cu1 I1 Cu2 -34.4(4) . . . . ? I2 Cu1 I1 Cu2 -156.68(10) 3_645 . . . ? I3 Cu1 I1 Cu2 85.37(9) . . . . ? Cu3 Cu1 I1 Cu2 65.24(8) . . . . ? N2 Cu2 I2 Cu1 136.0(4) . . . 3_655 ? I3 Cu2 I2 Cu1 4.49(8) 3_655 . . 3_655 ? I1 Cu2 I2 Cu1 -112.68(9) . . . 3_655 ? Cu3 Cu2 I2 Cu1 -130.04(8) . . . 3_655 ? N2 Cu2 I2 Cu3 -93.9(4) . . . . ? I3 Cu2 I2 Cu3 134.54(10) 3_655 . . . ? I1 Cu2 I2 Cu3 17.36(7) . . . . ? N4 Cu3 I2 Cu1 -88.5(4) 2_574 . . 3_655 ? I1 Cu3 I2 Cu1 33.37(11) . . . 3_655 ? I3 Cu3 I2 Cu1 167.20(7) . . . 3_655 ? Cu2 Cu3 I2 Cu1 51.40(9) . . . 3_655 ? Cu1 Cu3 I2 Cu1 103.75(10) . . . 3_655 ? N4 Cu3 I2 Cu2 -139.9(4) 2_574 . . . ? I1 Cu3 I2 Cu2 -18.03(7) . . . . ? I3 Cu3 I2 Cu2 115.80(9) . . . . ? Cu1 Cu3 I2 Cu2 52.35(10) . . . . ? N3 Cu1 I3 Cu2 -126.8(4) . . . 3_645 ? I2 Cu1 I3 Cu2 4.48(8) 3_645 . . 3_645 ? Cu3 Cu1 I3 Cu2 139.54(8) . . . 3_645 ? I1 Cu1 I3 Cu2 120.12(9) . . . 3_645 ? N3 Cu1 I3 Cu3 93.7(4) . . . . ? I2 Cu1 I3 Cu3 -135.06(10) 3_645 . . . ? I1 Cu1 I3 Cu3 -19.42(6) . . . . ? N4 Cu3 I3 Cu2 97.4(4) 2_574 . . 3_645 ? I1 Cu3 I3 Cu2 -23.28(12) . . . 3_645 ? I2 Cu3 I3 Cu2 -156.61(8) . . . 3_645 ? Cu2 Cu3 I3 Cu2 -92.36(11) . . . 3_645 ? Cu1 Cu3 I3 Cu2 -44.61(9) . . . 3_645 ? N4 Cu3 I3 Cu1 142.0(4) 2_574 . . . ? I1 Cu3 I3 Cu1 21.33(7) . . . . ? I2 Cu3 I3 Cu1 -112.00(9) . . . . ? Cu2 Cu3 I3 Cu1 -47.75(10) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.084 _refine_diff_density_min -0.994 _refine_diff_density_rms 0.213 #===end