# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dan Li' _publ_contact_author_email DLI@STU.EDU.CN _publ_section_title ; Unprecedented cationic copper(I)-iodide aggregates trapped in "click" formation of anionic-tetrazolate-based coordination polymers ; loop_ _publ_author_name 'Dan Li.' 'Mian Li.' 'Zhen Li.' # Attachment 'complex1-3.cif' data_complex1 _database_code_depnum_ccdc_archive 'CCDC 680145' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H4 Cu2 I N5' _chemical_formula_weight 424.14 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 20.7315(16) _cell_length_b 8.8557(7) _cell_length_c 12.0833(10) _cell_angle_alpha 90.00 _cell_angle_beta 110.7310(10) _cell_angle_gamma 90.00 _cell_volume 2074.8(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3262 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 27.50 _exptl_crystal_description sheet _exptl_crystal_colour yellowish _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.716 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 7.049 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _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 'Bruker APEX area-dectector diffractometer' _diffrn_measurement_method '\f and \w-scan' _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 12414 _diffrn_reflns_av_R_equivalents 0.0228 _diffrn_reflns_av_sigmaI/netI 0.0180 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 27.86 _reflns_number_total 2368 _reflns_number_gt 2256 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, Ver. 6.10, Bruker AXS Inc., 2000.' _computing_publication_material SHELXL-97 _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^)+(0.0287P)^2^+16.8011P] 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 2368 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0307 _refine_ls_R_factor_gt 0.0292 _refine_ls_wR_factor_ref 0.0714 _refine_ls_wR_factor_gt 0.0704 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.114 _refine_ls_shift/su_max 0.004 _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 1.15626(3) 0.50272(6) 0.74153(5) 0.02730(13) Uani 1 1 d . . . Cu2 Cu 1.25244(3) 0.66443(6) 1.09491(5) 0.02757(13) Uani 1 1 d . . . C1 C 0.85600(19) 0.1705(4) 0.5667(3) 0.0198(7) Uani 1 1 d . . . C2 C 0.8451(2) 0.0774(5) 0.4692(4) 0.0246(8) Uani 1 1 d . . . H2 H 0.8067 0.0146 0.4436 0.030 Uiso 1 1 calc R . . C3 C 0.8917(2) 0.0781(6) 0.4098(4) 0.0336(10) Uani 1 1 d . . . H3 H 0.8840 0.0146 0.3450 0.040 Uiso 1 1 calc R . . C4 C 0.9483(2) 0.1699(5) 0.4444(4) 0.0311(10) Uani 1 1 d . . . H4 H 0.9787 0.1704 0.4034 0.037 Uiso 1 1 calc R . . C5 C 0.9594(2) 0.2628(5) 0.5426(4) 0.0251(8) Uani 1 1 d . . . C6 C 0.9134(2) 0.2638(5) 0.6029(4) 0.0234(8) Uani 1 1 d . . . H6 H 0.9212 0.3273 0.6676 0.028 Uiso 1 1 calc R . . C7 C 0.80890(19) 0.1716(4) 0.6339(3) 0.0192(7) Uani 1 1 d . . . C8 C 1.0186(2) 0.3607(5) 0.5872(4) 0.0267(8) Uani 1 1 d . . . I1 I 1.138037(13) 0.68540(3) 0.90406(2) 0.02568(9) Uani 1 1 d . . . N1 N 0.80612(17) 0.2834(4) 0.7067(3) 0.0218(7) Uani 1 1 d . . . N2 N 0.75978(16) 0.2385(4) 0.7540(3) 0.0210(6) Uani 1 1 d . . . N3 N 0.73518(17) 0.1082(4) 0.7094(3) 0.0217(7) Uani 1 1 d . . . N4 N 0.76513(16) 0.0615(4) 0.6346(3) 0.0203(6) Uani 1 1 d . . . N5 N 1.06520(18) 0.4374(4) 0.6287(3) 0.0286(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 0.0209(2) 0.0227(3) 0.0406(3) -0.0008(2) 0.0138(2) -0.00311(19) Cu2 0.0335(3) 0.0201(2) 0.0332(3) 0.0023(2) 0.0168(2) 0.0010(2) C1 0.0180(18) 0.0208(18) 0.0224(17) 0.0006(14) 0.0094(15) -0.0002(14) C2 0.0218(18) 0.026(2) 0.0241(18) -0.0030(16) 0.0064(15) -0.0030(16) C3 0.035(2) 0.040(3) 0.029(2) -0.0118(19) 0.0153(19) -0.009(2) C4 0.028(2) 0.043(3) 0.028(2) -0.0045(18) 0.0163(18) -0.0041(18) C5 0.0207(18) 0.027(2) 0.0284(19) -0.0015(17) 0.0099(16) -0.0024(16) C6 0.0225(18) 0.0240(19) 0.0259(19) -0.0026(16) 0.0110(16) -0.0036(16) C7 0.0161(17) 0.0203(18) 0.0200(17) -0.0002(14) 0.0052(14) 0.0002(14) C8 0.022(2) 0.032(2) 0.0273(19) 0.0019(18) 0.0107(16) -0.0018(17) I1 0.02242(14) 0.02901(15) 0.02839(15) -0.00218(10) 0.01241(11) -0.00182(10) N1 0.0210(16) 0.0194(15) 0.0271(16) -0.0032(13) 0.0109(13) -0.0018(13) N2 0.0188(15) 0.0195(16) 0.0259(16) -0.0006(13) 0.0092(13) -0.0035(12) N3 0.0214(16) 0.0160(15) 0.0268(16) -0.0035(13) 0.0076(13) 0.0018(12) N4 0.0193(15) 0.0188(15) 0.0245(15) -0.0025(13) 0.0099(13) -0.0032(12) N5 0.0210(17) 0.035(2) 0.0303(18) 0.0017(16) 0.0093(14) -0.0043(15) _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 N5 1.984(4) . ? Cu1 N3 2.037(3) 3 ? Cu1 N1 2.104(3) 2_756 ? Cu1 I1 2.6724(6) . ? Cu2 N4 2.053(3) 8_556 ? Cu2 N2 2.113(3) 5_767 ? Cu2 I1 2.6276(6) 7_767 ? Cu2 I1 2.6656(6) . ? Cu2 Cu2 2.7209(11) 7_767 ? C1 C6 1.387(5) . ? C1 C2 1.389(6) . ? C1 C7 1.474(5) . ? C2 C3 1.392(6) . ? C3 C4 1.366(6) . ? C4 C5 1.394(6) . ? C5 C6 1.390(5) . ? C5 C8 1.441(6) . ? C7 N4 1.334(5) . ? C7 N1 1.339(5) . ? C8 N5 1.142(6) . ? I1 Cu2 2.6276(6) 7_767 ? N1 N2 1.341(4) . ? N1 Cu1 2.104(3) 2_756 ? N2 N3 1.299(5) . ? N2 Cu2 2.113(3) 5_767 ? N3 N4 1.331(4) . ? N3 Cu1 2.037(3) 3_445 ? N4 Cu2 2.053(3) 8_455 ? 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 N5 Cu1 N3 129.49(14) . 3 ? N5 Cu1 N1 95.60(15) . 2_756 ? N3 Cu1 N1 103.99(13) 3 2_756 ? N5 Cu1 I1 109.51(11) . . ? N3 Cu1 I1 101.22(9) 3 . ? N1 Cu1 I1 118.30(9) 2_756 . ? N4 Cu2 N2 103.86(13) 8_556 5_767 ? N4 Cu2 I1 116.94(9) 8_556 7_767 ? N2 Cu2 I1 99.07(9) 5_767 7_767 ? N4 Cu2 I1 105.73(9) 8_556 . ? N2 Cu2 I1 112.16(9) 5_767 . ? I1 Cu2 I1 118.14(2) 7_767 . ? N4 Cu2 Cu2 134.68(9) 8_556 7_767 ? N2 Cu2 Cu2 121.45(10) 5_767 7_767 ? I1 Cu2 Cu2 59.76(2) 7_767 7_767 ? I1 Cu2 Cu2 58.38(2) . 7_767 ? C6 C1 C2 118.9(4) . . ? C6 C1 C7 119.0(3) . . ? C2 C1 C7 122.1(3) . . ? C1 C2 C3 120.1(4) . . ? C4 C3 C2 121.5(4) . . ? C3 C4 C5 118.5(4) . . ? C6 C5 C4 120.8(4) . . ? C6 C5 C8 116.8(4) . . ? C4 C5 C8 122.4(4) . . ? C1 C6 C5 120.2(4) . . ? N4 C7 N1 110.4(3) . . ? N4 C7 C1 125.7(3) . . ? N1 C7 C1 123.9(3) . . ? N5 C8 C5 176.1(4) . . ? Cu2 I1 Cu2 61.86(2) 7_767 . ? Cu2 I1 Cu1 87.888(18) 7_767 . ? Cu2 I1 Cu1 106.240(19) . . ? C7 N1 N2 105.4(3) . . ? C7 N1 Cu1 141.3(3) . 2_756 ? N2 N1 Cu1 113.1(2) . 2_756 ? N3 N2 N1 108.8(3) . . ? N3 N2 Cu2 124.8(3) . 5_767 ? N1 N2 Cu2 124.8(2) . 5_767 ? N2 N3 N4 110.4(3) . . ? N2 N3 Cu1 123.5(3) . 3_445 ? N4 N3 Cu1 125.9(2) . 3_445 ? N3 N4 C7 105.0(3) . . ? N3 N4 Cu2 114.2(2) . 8_455 ? C7 N4 Cu2 137.9(3) . 8_455 ? C8 N5 Cu1 158.0(4) . . ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 27.86 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 1.294 _refine_diff_density_min -0.757 _refine_diff_density_rms 0.129 data_complex2 _database_code_depnum_ccdc_archive 'CCDC 680146' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H9 Cu5 I N13' _chemical_formula_weight 719.87 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/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 8.8201(17) _cell_length_b 14.300(3) _cell_length_c 13.556(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.241(3) _cell_angle_gamma 90.00 _cell_volume 1708.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1988 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 26.79 _exptl_crystal_description block _exptl_crystal_colour yellowish-brown _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.799 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 7.953 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.1673 _exptl_absorpt_correction_T_max 0.2620 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _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 'Bruker APEX area-dectector diffractometer' _diffrn_measurement_method '\f and \w-scan' _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 4572 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_sigmaI/netI 0.0479 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1570 _reflns_number_gt 1422 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, Ver. 6.10, Bruker AXS Inc., 2000.' _computing_publication_material SHELXL-97 _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^)+(0.0523P)^2^+2.7141P] 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 1570 _refine_ls_number_parameters 126 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0399 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0947 _refine_ls_wR_factor_gt 0.0899 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _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 0.08898(11) 0.5000 0.40873(7) 0.0277(3) Uani 1 2 d S . . Cu2 Cu 0.18646(7) 0.37937(5) 0.76177(5) 0.0296(2) Uani 1 1 d . . . Cu3 Cu 0.52396(7) 0.28730(5) 0.89640(5) 0.0302(2) Uani 1 1 d . . . I1 I 0.21894(5) 0.5000 0.58723(3) 0.02536(19) Uani 1 2 d S . . N1 N -0.0325(4) 0.3542(3) 0.7429(3) 0.0205(9) Uani 1 1 d . . . N2 N -0.0828(4) 0.2772(3) 0.7833(3) 0.0216(9) Uani 1 1 d . . . N3 N -0.2135(5) 0.2510(3) 0.7364(3) 0.0246(10) Uani 1 1 d . . . N4 N -0.1294(5) 0.3810(3) 0.6701(3) 0.0213(9) Uani 1 1 d . . . N5 N 0.3409(5) 0.4542(3) 0.8351(3) 0.0234(9) Uani 1 1 d . . . N6 N 0.4785(5) 0.4236(3) 0.8666(3) 0.0266(10) Uani 1 1 d . . . N7 N 0.6986(5) 0.2556(3) 0.9799(4) 0.0270(11) Uani 0.50 1 d P . . C1 C -0.2404(6) 0.3163(4) 0.6684(4) 0.0241(11) Uani 1 1 d . . . C2 C -0.3741(7) 0.3172(5) 0.5986(5) 0.0422(16) Uani 1 1 d . . . H2A H -0.4068 0.2542 0.5858 0.063 Uiso 1 1 calc R . . H2B H -0.3472 0.3462 0.5379 0.063 Uiso 1 1 calc R . . H2C H -0.4549 0.3517 0.6270 0.063 Uiso 1 1 calc R . . C3 C 0.5621(8) 0.5000 0.8835(5) 0.0233(16) Uani 1 2 d S . . C4 C 0.7236(9) 0.5000 0.9153(7) 0.0346(19) Uani 1 2 d S . . H4A H 0.7830 0.4767 0.8628 0.052 Uiso 0.50 1 calc PR . . H4B H 0.7382 0.4607 0.9723 0.052 Uiso 0.50 1 calc PR . . H4C H 0.7549 0.5626 0.9315 0.052 Uiso 0.50 1 calc PR . . C5 C 0.6986(5) 0.2556(3) 0.9799(4) 0.0270(11) Uani 0.50 1 d P . . 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 0.0312(5) 0.0182(5) 0.0330(6) 0.000 -0.0079(4) 0.000 Cu2 0.0186(4) 0.0215(4) 0.0477(5) -0.0037(3) -0.0119(3) -0.0019(2) Cu3 0.0290(4) 0.0217(4) 0.0382(4) -0.0033(3) -0.0188(3) 0.0054(3) I1 0.0221(3) 0.0298(3) 0.0239(3) 0.000 -0.0038(2) 0.000 N1 0.016(2) 0.017(2) 0.028(2) 0.0035(18) -0.0069(18) -0.0006(17) N2 0.016(2) 0.019(2) 0.029(2) 0.0037(18) -0.0072(18) -0.0034(16) N3 0.019(2) 0.021(2) 0.033(3) 0.0054(18) -0.0096(19) -0.0060(18) N4 0.016(2) 0.019(2) 0.028(2) 0.0032(17) -0.0093(18) -0.0016(16) N5 0.019(2) 0.018(2) 0.033(3) 0.0037(19) -0.0108(19) 0.0011(17) N6 0.022(2) 0.018(2) 0.039(3) 0.0000(19) -0.013(2) 0.0015(18) N7 0.029(3) 0.024(3) 0.028(3) -0.005(2) 0.004(2) 0.001(2) C1 0.018(2) 0.023(3) 0.030(3) 0.003(2) -0.010(2) -0.002(2) C2 0.027(3) 0.048(4) 0.050(4) 0.022(3) -0.020(3) -0.015(3) C3 0.024(4) 0.020(4) 0.025(4) 0.000 -0.007(3) 0.000 C4 0.022(4) 0.026(4) 0.055(6) 0.000 -0.007(4) 0.000 C5 0.029(3) 0.024(3) 0.028(3) -0.005(2) 0.004(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 N4 2.048(4) 2_556 ? Cu1 N4 2.048(4) 5_566 ? Cu1 I1 2.6367(11) . ? Cu1 I1 2.7186(12) 5_566 ? Cu1 Cu1 2.982(2) 5_566 ? Cu2 N5 1.971(4) . ? Cu2 N1 1.972(4) . ? Cu2 N3 2.097(4) 8 ? Cu2 I1 2.9512(9) . ? Cu3 N7 1.929(5) . ? Cu3 N2 1.993(4) 8 ? Cu3 N6 2.028(4) . ? Cu3 Cu3 2.8567(15) 2_657 ? I1 Cu1 2.7186(12) 5_566 ? I1 Cu2 2.9512(9) 6_565 ? N1 N2 1.315(6) . ? N1 N4 1.336(6) . ? N2 N3 1.348(6) . ? N2 Cu3 1.993(4) 8_455 ? N3 C1 1.326(7) . ? N3 Cu2 2.097(4) 8_455 ? N4 C1 1.347(6) . ? N4 Cu1 2.048(4) 5_566 ? N5 N5 1.309(8) 6_565 ? N5 N6 1.344(6) . ? N6 C3 1.332(6) . ? N7 C5 1.053(10) 7_657 ? N7 N7 1.053(10) 7_657 ? C1 C2 1.483(8) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 N6 1.332(6) 6_565 ? C3 C4 1.472(10) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Cu1 N4 112.3(3) 2_556 5_566 ? N4 Cu1 I1 113.62(12) 2_556 . ? N4 Cu1 I1 113.62(12) 5_566 . ? N4 Cu1 I1 101.84(12) 2_556 5_566 ? N4 Cu1 I1 101.84(12) 5_566 5_566 ? I1 Cu1 I1 112.35(4) . 5_566 ? N4 Cu1 Cu1 122.77(13) 2_556 5_566 ? N4 Cu1 Cu1 122.77(13) 5_566 5_566 ? I1 Cu1 Cu1 57.48(3) . 5_566 ? I1 Cu1 Cu1 54.87(3) 5_566 5_566 ? N5 Cu2 N1 144.99(18) . . ? N5 Cu2 N3 106.18(16) . 8 ? N1 Cu2 N3 103.46(17) . 8 ? N5 Cu2 I1 89.99(13) . . ? N1 Cu2 I1 97.35(12) . . ? N3 Cu2 I1 109.48(12) 8 . ? N7 Cu3 N2 133.20(19) . 8 ? N7 Cu3 N6 119.32(19) . . ? N2 Cu3 N6 102.00(17) 8 . ? N7 Cu3 Cu3 64.44(15) . 2_657 ? N2 Cu3 Cu3 132.26(13) 8 2_657 ? N6 Cu3 Cu3 99.23(13) . 2_657 ? Cu1 I1 Cu1 67.65(4) . 5_566 ? Cu1 I1 Cu2 133.11(2) . 6_565 ? Cu1 I1 Cu2 81.69(2) 5_566 6_565 ? Cu1 I1 Cu2 133.11(2) . . ? Cu1 I1 Cu2 81.69(2) 5_566 . ? Cu2 I1 Cu2 71.54(3) 6_565 . ? N2 N1 N4 109.4(4) . . ? N2 N1 Cu2 116.3(3) . . ? N4 N1 Cu2 129.7(3) . . ? N1 N2 N3 109.4(4) . . ? N1 N2 Cu3 123.5(3) . 8_455 ? N3 N2 Cu3 127.2(3) . 8_455 ? C1 N3 N2 105.0(4) . . ? C1 N3 Cu2 132.4(3) . 8_455 ? N2 N3 Cu2 121.8(3) . 8_455 ? N1 N4 C1 105.0(4) . . ? N1 N4 Cu1 120.3(3) . 5_566 ? C1 N4 Cu1 134.7(3) . 5_566 ? N5 N5 N6 109.0(2) 6_565 . ? N5 N5 Cu2 122.90(11) 6_565 . ? N6 N5 Cu2 125.5(3) . . ? C3 N6 N5 105.9(4) . . ? C3 N6 Cu3 130.5(4) . . ? N5 N6 Cu3 123.0(3) . . ? C5 N7 N7 0.0(7) 7_657 7_657 ? C5 N7 Cu3 172.8(7) 7_657 . ? N7 N7 Cu3 172.8(7) 7_657 . ? N3 C1 N4 111.2(4) . . ? N3 C1 C2 124.4(5) . . ? N4 C1 C2 124.4(5) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N6 C3 N6 110.1(6) . 6_565 ? N6 C3 C4 124.9(3) . . ? N6 C3 C4 124.9(3) 6_565 . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? 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 N4 Cu1 I1 Cu1 -114.95(13) 2_556 . . 5_566 ? N4 Cu1 I1 Cu1 114.95(13) 5_566 . . 5_566 ? I1 Cu1 I1 Cu1 0.0 5_566 . . 5_566 ? N4 Cu1 I1 Cu2 -168.15(13) 2_556 . . 6_565 ? N4 Cu1 I1 Cu2 61.75(14) 5_566 . . 6_565 ? I1 Cu1 I1 Cu2 -53.20(3) 5_566 . . 6_565 ? Cu1 Cu1 I1 Cu2 -53.20(3) 5_566 . . 6_565 ? N4 Cu1 I1 Cu2 -61.75(14) 2_556 . . . ? N4 Cu1 I1 Cu2 168.15(13) 5_566 . . . ? I1 Cu1 I1 Cu2 53.20(3) 5_566 . . . ? Cu1 Cu1 I1 Cu2 53.20(3) 5_566 . . . ? N5 Cu2 I1 Cu1 179.61(12) . . . . ? N1 Cu2 I1 Cu1 -34.72(13) . . . . ? N3 Cu2 I1 Cu1 72.41(13) 8 . . . ? N5 Cu2 I1 Cu1 -131.94(12) . . . 5_566 ? N1 Cu2 I1 Cu1 13.73(12) . . . 5_566 ? N3 Cu2 I1 Cu1 120.86(12) 8 . . 5_566 ? N5 Cu2 I1 Cu2 -47.98(12) . . . 6_565 ? N1 Cu2 I1 Cu2 97.69(12) . . . 6_565 ? N3 Cu2 I1 Cu2 -155.18(12) 8 . . 6_565 ? N5 Cu2 N1 N2 -103.4(4) . . . . ? N3 Cu2 N1 N2 43.9(4) 8 . . . ? I1 Cu2 N1 N2 156.0(3) . . . . ? N5 Cu2 N1 N4 103.5(5) . . . . ? N3 Cu2 N1 N4 -109.2(4) 8 . . . ? I1 Cu2 N1 N4 2.9(4) . . . . ? N4 N1 N2 N3 1.0(5) . . . . ? Cu2 N1 N2 N3 -157.3(3) . . . . ? N4 N1 N2 Cu3 -179.1(3) . . . 8_455 ? Cu2 N1 N2 Cu3 22.5(5) . . . 8_455 ? N1 N2 N3 C1 -1.4(6) . . . . ? Cu3 N2 N3 C1 178.7(4) 8_455 . . . ? N1 N2 N3 Cu2 169.9(3) . . . 8_455 ? Cu3 N2 N3 Cu2 -10.0(6) 8_455 . . 8_455 ? N2 N1 N4 C1 -0.2(5) . . . . ? Cu2 N1 N4 C1 154.3(4) . . . . ? N2 N1 N4 Cu1 179.2(3) . . . 5_566 ? Cu2 N1 N4 Cu1 -26.3(6) . . . 5_566 ? N1 Cu2 N5 N5 -57.0(3) . . . 6_565 ? N3 Cu2 N5 N5 156.20(14) 8 . . 6_565 ? I1 Cu2 N5 N5 45.88(9) . . . 6_565 ? N1 Cu2 N5 N6 143.2(4) . . . . ? N3 Cu2 N5 N6 -3.6(5) 8 . . . ? I1 Cu2 N5 N6 -113.9(4) . . . . ? N5 N5 N6 C3 -1.2(5) 6_565 . . . ? Cu2 N5 N6 C3 160.9(4) . . . . ? N5 N5 N6 Cu3 171.5(2) 6_565 . . . ? Cu2 N5 N6 Cu3 -26.3(6) . . . . ? N7 Cu3 N6 C3 11.0(6) . . . . ? N2 Cu3 N6 C3 -146.3(6) 8 . . . ? Cu3 Cu3 N6 C3 76.8(6) 2_657 . . . ? N7 Cu3 N6 N5 -159.8(4) . . . . ? N2 Cu3 N6 N5 42.9(4) 8 . . . ? Cu3 Cu3 N6 N5 -94.0(4) 2_657 . . . ? N2 Cu3 N7 C5 103(5) 8 . . 7_657 ? N6 Cu3 N7 C5 -46(5) . . . 7_657 ? Cu3 Cu3 N7 C5 -132(5) 2_657 . . 7_657 ? N2 Cu3 N7 N7 103(5) 8 . . 7_657 ? N6 Cu3 N7 N7 -46(5) . . . 7_657 ? Cu3 Cu3 N7 N7 -132(5) 2_657 . . 7_657 ? N2 N3 C1 N4 1.3(6) . . . . ? Cu2 N3 C1 N4 -168.6(4) 8_455 . . . ? N2 N3 C1 C2 -179.5(5) . . . . ? Cu2 N3 C1 C2 10.6(9) 8_455 . . . ? N1 N4 C1 N3 -0.7(6) . . . . ? Cu1 N4 C1 N3 -180.0(4) 5_566 . . . ? N1 N4 C1 C2 -179.9(6) . . . . ? Cu1 N4 C1 C2 0.8(9) 5_566 . . . ? N5 N6 C3 N6 2.1(8) . . . 6_565 ? Cu3 N6 C3 N6 -169.9(2) . . . 6_565 ? N5 N6 C3 C4 -177.3(7) . . . . ? Cu3 N6 C3 C4 10.7(11) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.958 _refine_diff_density_min -0.872 _refine_diff_density_rms 0.197 data_complex3 _database_code_depnum_ccdc_archive 'CCDC 680147' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H9 Cu5 I2 N12' _chemical_formula_weight 820.75 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/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 26.193(2) _cell_length_b 8.5613(7) _cell_length_c 8.2997(7) _cell_angle_alpha 90.00 _cell_angle_beta 104.008(2) _cell_angle_gamma 90.00 _cell_volume 1805.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3155 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 27.85 _exptl_crystal_description sheet _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.019 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 9.230 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _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 'Bruker APEX area-dectector diffractometer' _diffrn_measurement_method '\f and \w-scan' _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 5944 _diffrn_reflns_av_R_equivalents 0.0301 _diffrn_reflns_av_sigmaI/netI 0.0486 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 27.89 _reflns_number_total 2275 _reflns_number_gt 2057 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, Ver. 6.10, Bruker AXS Inc., 2000.' _computing_publication_material SHELXL-97 _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^)+(0.1017P)^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 2275 _refine_ls_number_parameters 122 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0506 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.1402 _refine_ls_wR_factor_gt 0.1297 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.011 _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 I1 I 0.071134(18) 0.0000 0.85081(5) 0.02533(18) Uani 1 2 d S . . I2 I 0.228113(19) 0.0000 1.19166(8) 0.0383(2) Uani 1 2 d S . . Cu1 Cu 0.05044(3) 0.30805(8) 0.69711(7) 0.0280(2) Uani 1 1 d . . . Cu3 Cu 0.14303(3) 0.15597(7) 1.09665(8) 0.0291(2) Uani 1 1 d . . . Cu2 Cu 0.0000 0.18311(15) 1.0000 0.0436(3) Uani 1 2 d S . . N6 N 0.14153(16) 0.3720(5) 0.9904(5) 0.0228(8) Uani 1 1 d . . . N2 N -0.02698(17) 0.2817(5) 0.6673(5) 0.0270(9) Uani 1 1 d . . . N3 N -0.04675(16) 0.2380(5) 0.7904(4) 0.0259(9) Uani 1 1 d . . . N5 N 0.10114(15) 0.4229(4) 0.8684(5) 0.0208(7) Uani 1 1 d . . . N4 N -0.09853(16) 0.2098(5) 0.7346(5) 0.0266(9) Uani 1 1 d . . . C4 C 0.2123(3) 0.5000 1.2059(11) 0.0401(19) Uani 1 2 d S . . H4A H 0.2255 0.3954 1.2262 0.060 Uiso 0.50 1 calc PR . . H4B H 0.2027 0.5390 1.3030 0.060 Uiso 0.50 1 calc PR . . H4C H 0.2391 0.5656 1.1806 0.060 Uiso 0.50 1 calc PR . . C3 C 0.1654(3) 0.5000 1.0637(8) 0.0228(13) Uani 1 2 d S . . N1 N -0.06543(17) 0.2829(5) 0.5277(5) 0.0257(9) Uani 1 1 d . . . C1 C -0.1092(2) 0.2389(6) 0.5717(6) 0.0270(10) Uani 1 1 d . . . C2 C -0.1619(2) 0.2245(9) 0.4555(7) 0.0440(15) Uani 1 1 d . . . H2A H -0.1586 0.1714 0.3566 0.066 Uiso 1 1 calc R . . H2B H -0.1763 0.3267 0.4271 0.066 Uiso 1 1 calc R . . H2C H -0.1848 0.1661 0.5077 0.066 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.0292(3) 0.0187(3) 0.0233(3) 0.000 -0.0031(2) 0.000 I2 0.0208(3) 0.0287(3) 0.0582(4) 0.000 -0.0047(2) 0.000 Cu1 0.0258(4) 0.0338(4) 0.0201(3) -0.0046(2) -0.0031(3) -0.0050(3) Cu3 0.0296(4) 0.0225(3) 0.0324(4) 0.0033(2) 0.0022(3) 0.0035(2) Cu2 0.0326(6) 0.0743(8) 0.0176(4) 0.000 -0.0059(4) 0.000 N6 0.021(2) 0.0173(18) 0.0242(17) 0.0009(15) -0.0055(15) 0.0021(15) N2 0.024(2) 0.035(2) 0.0177(17) 0.0015(16) -0.0041(16) -0.0039(18) N3 0.020(2) 0.037(2) 0.0175(17) 0.0011(16) -0.0012(16) -0.0012(18) N5 0.0199(19) 0.0177(17) 0.0207(16) 0.0003(14) -0.0028(15) 0.0012(15) N4 0.022(2) 0.033(2) 0.0220(18) -0.0001(16) -0.0007(17) -0.0019(17) C4 0.027(4) 0.033(4) 0.044(4) 0.000 -0.022(4) 0.000 C3 0.025(3) 0.020(3) 0.018(3) 0.000 -0.005(3) 0.000 N1 0.023(2) 0.032(2) 0.0181(16) 0.0031(15) -0.0033(16) 0.0024(17) C1 0.022(2) 0.032(2) 0.0226(19) -0.0001(19) -0.0029(19) 0.003(2) C2 0.020(3) 0.077(5) 0.029(2) 0.004(3) -0.006(2) -0.004(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 I1 Cu3 2.7626(8) . ? I1 Cu3 2.7626(8) 6 ? I1 Cu1 2.9226(7) 6 ? I1 Cu1 2.9226(7) . ? I1 Cu2 2.9290(8) 5_557 ? I1 Cu2 2.9290(8) . ? I2 Cu3 2.5536(8) . ? I2 Cu3 2.5536(8) 6 ? Cu1 N5 1.959(4) . ? Cu1 N2 1.995(4) . ? Cu1 N1 2.009(4) 2_556 ? Cu3 N6 2.045(4) . ? Cu3 N4 2.079(4) 2_557 ? Cu3 Cu3 2.6706(13) 6 ? Cu2 N3 1.927(4) 2_557 ? Cu2 N3 1.927(4) . ? Cu2 I1 2.9290(8) 5_557 ? N6 C3 1.333(5) . ? N6 N5 1.348(5) . ? N2 N3 1.307(6) . ? N2 N1 1.339(5) . ? N3 N4 1.345(5) . ? N5 N5 1.319(7) 6_565 ? N4 C1 1.336(6) . ? N4 Cu3 2.079(4) 2_557 ? C4 C3 1.484(9) . ? C3 N6 1.333(5) 6_565 ? N1 C1 1.338(7) . ? N1 Cu1 2.009(4) 2_556 ? C1 C2 1.486(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cu3 I1 Cu3 57.81(3) . 6 ? Cu3 I1 Cu1 141.24(2) . 6 ? Cu3 I1 Cu1 84.690(18) 6 6 ? Cu3 I1 Cu1 84.690(18) . . ? Cu3 I1 Cu1 141.24(2) 6 . ? Cu1 I1 Cu1 128.94(3) 6 . ? Cu3 I1 Cu2 109.64(2) . 5_557 ? Cu3 I1 Cu2 79.56(2) 6 5_557 ? Cu1 I1 Cu2 68.40(2) 6 5_557 ? Cu1 I1 Cu2 126.71(3) . 5_557 ? Cu3 I1 Cu2 79.56(2) . . ? Cu3 I1 Cu2 109.64(2) 6 . ? Cu1 I1 Cu2 126.71(3) 6 . ? Cu1 I1 Cu2 68.40(2) . . ? Cu2 I1 Cu2 64.72(5) 5_557 . ? Cu3 I2 Cu3 63.06(3) . 6 ? N5 Cu1 N2 129.55(16) . . ? N5 Cu1 N1 118.51(17) . 2_556 ? N2 Cu1 N1 107.09(17) . 2_556 ? N5 Cu1 I1 96.59(11) . . ? N2 Cu1 I1 91.58(13) . . ? N1 Cu1 I1 104.55(12) 2_556 . ? N6 Cu3 N4 97.73(17) . 2_557 ? N6 Cu3 I2 122.02(12) . . ? N4 Cu3 I2 119.84(11) 2_557 . ? N6 Cu3 Cu3 154.74(11) . 6 ? N4 Cu3 Cu3 102.80(12) 2_557 6 ? I2 Cu3 Cu3 58.472(16) . 6 ? N6 Cu3 I1 100.39(11) . . ? N4 Cu3 I1 102.22(12) 2_557 . ? I2 Cu3 I1 111.30(3) . . ? Cu3 Cu3 I1 61.096(14) 6 . ? N3 Cu2 N3 151.8(3) 2_557 . ? N3 Cu2 I1 100.48(12) 2_557 . ? N3 Cu2 I1 94.53(12) . . ? N3 Cu2 I1 94.53(13) 2_557 5_557 ? N3 Cu2 I1 100.48(12) . 5_557 ? I1 Cu2 I1 115.28(5) . 5_557 ? C3 N6 N5 105.8(4) . . ? C3 N6 Cu3 126.1(3) . . ? N5 N6 Cu3 123.1(3) . . ? N3 N2 N1 108.8(4) . . ? N3 N2 Cu1 121.2(3) . . ? N1 N2 Cu1 129.4(3) . . ? N2 N3 N4 109.9(3) . . ? N2 N3 Cu2 119.3(3) . . ? N4 N3 Cu2 129.4(3) . . ? N5 N5 N6 108.9(2) 6_565 . ? N5 N5 Cu1 120.14(11) 6_565 . ? N6 N5 Cu1 130.8(3) . . ? C1 N4 N3 105.1(4) . . ? C1 N4 Cu3 135.2(4) . 2_557 ? N3 N4 Cu3 119.4(3) . 2_557 ? N6 C3 N6 110.6(6) . 6_565 ? N6 C3 C4 124.7(3) . . ? N6 C3 C4 124.7(3) 6_565 . ? C1 N1 N2 106.0(4) . . ? C1 N1 Cu1 131.0(3) . 2_556 ? N2 N1 Cu1 122.0(3) . 2_556 ? N4 C1 N1 110.3(4) . . ? N4 C1 C2 125.1(5) . . ? N1 C1 C2 124.6(5) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.89 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 2.347 _refine_diff_density_min -1.994 _refine_diff_density_rms 0.359