# Electronic Supplementary Material for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Hong Deng' _publ_contact_author_email DH@SCNU.EDU.CN _publ_section_title ; In Situ Solvothermal Syntheses of Heteronuclear Copper(I)-Alkaline Metallic Tetrazole-based Coordination Polymer ; loop_ _publ_author_name 'Hong Deng' 'Yinghua Li' 'Biao Liu' 'Guo Peng' 'Yongcai Qiu' # Attachment 'Cifs.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 713551' #============================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C2 H3 Cu2 I2 K N4' _chemical_formula_sum 'C2 H3 Cu2 I2 K N4' _chemical_formula_weight 503.06 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' K K 0.2009 0.2494 '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 _symmetry_space_group_name_Hall '-C 2y' 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 19.446(2) _cell_length_b 4.2397(5) _cell_length_c 12.4437(14) _cell_angle_alpha 90.00 _cell_angle_beta 107.177(2) _cell_angle_gamma 90.00 _cell_volume 980.15(19) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3000 _cell_measurement_theta_min 1.71 _cell_measurement_theta_max 28.17 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 11.008 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1249 _exptl_absorpt_correction_T_max 0.1890 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 2512 _diffrn_reflns_av_R_equivalents 0.0235 _diffrn_reflns_av_sigmaI/netI 0.0291 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.17 _reflns_number_total 1005 _reflns_number_gt 857 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0252P)^2^+2.0338P] 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 1005 _refine_ls_number_parameters 68 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0301 _refine_ls_R_factor_gt 0.0236 _refine_ls_wR_factor_ref 0.0551 _refine_ls_wR_factor_gt 0.0519 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 I2 I 0.35488(3) 0.5000 0.59386(4) 0.03499(16) Uani 1 2 d S . . Cu1 Cu 0.42457(5) 0.0000 0.54910(8) 0.0366(3) Uani 1 2 d S . . I1 I 0.82900(2) 0.0000 0.93274(4) 0.03280(16) Uani 1 2 d S . . Cu2 Cu 0.69710(5) 0.0000 0.94980(9) 0.0467(3) Uani 1 2 d S . . C1 C 0.5513(4) 0.0000 0.7665(6) 0.0320(17) Uani 1 2 d S . . N4 N 0.5257(3) 0.0000 0.6548(5) 0.0289(14) Uani 1 2 d S . . N1 N 0.6229(3) 0.0000 0.7958(5) 0.0333(15) Uani 1 2 d S . . N2 N 0.6414(3) 0.0000 0.7013(5) 0.0343(15) Uani 1 2 d S . . C2 C 0.5061(4) 0.0000 0.8453(7) 0.054(3) Uani 1 2 d S . . H2A H 0.4610 0.1019 0.8099 0.081 Uiso 0.50 1 calc PR . . H2B H 0.5308 0.1115 0.9128 0.081 Uiso 0.50 1 calc PR . . H2C H 0.4975 -0.2134 0.8637 0.081 Uiso 0.50 1 calc PR . . N3 N 0.5823(3) 0.0000 0.6190(5) 0.0288(14) Uani 1 2 d S . . K1 K 0.74248(9) 0.5000 0.69112(16) 0.0401(4) Uani 1 2 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 I2 0.0383(3) 0.0286(3) 0.0428(3) 0.000 0.0193(2) 0.000 Cu1 0.0260(5) 0.0558(6) 0.0267(5) 0.000 0.0059(4) 0.000 I1 0.0313(3) 0.0334(3) 0.0331(3) 0.000 0.0085(2) 0.000 Cu2 0.0342(5) 0.0742(8) 0.0273(5) 0.000 0.0023(4) 0.000 C1 0.028(4) 0.039(4) 0.029(4) 0.000 0.009(3) 0.000 N4 0.031(3) 0.036(3) 0.019(3) 0.000 0.006(3) 0.000 N1 0.023(3) 0.047(4) 0.030(4) 0.000 0.008(3) 0.000 N2 0.023(3) 0.050(4) 0.028(4) 0.000 0.004(3) 0.000 C2 0.029(4) 0.103(8) 0.034(5) 0.000 0.014(4) 0.000 N3 0.011(3) 0.043(4) 0.027(3) 0.000 -0.004(2) 0.000 K1 0.0405(9) 0.0336(9) 0.0475(11) 0.000 0.0148(8) 0.000 _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 I2 Cu1 2.6621(7) 1_565 ? I2 Cu1 2.6621(7) . ? I2 K1 3.492(2) 5_666 ? I2 K1 3.5069(15) 3_445 ? I2 K1 3.5069(15) 3_455 ? Cu1 N4 2.017(6) . ? Cu1 N3 2.057(6) 5_656 ? Cu1 I2 2.6621(7) 1_545 ? I1 Cu2 2.6355(11) . ? I1 Cu2 2.7067(8) 7_657 ? I1 Cu2 2.7067(8) 7_647 ? I1 K1 3.6574(16) 1_545 ? I1 K1 3.6574(16) . ? Cu2 N1 2.030(6) . ? Cu2 I1 2.7067(8) 7_657 ? Cu2 I1 2.7067(8) 7_647 ? Cu2 Cu2 2.9613(13) 7_657 ? Cu2 Cu2 2.9613(13) 7_647 ? C1 N1 1.331(9) . ? C1 N4 1.331(9) . ? C1 C2 1.497(11) . ? N4 N3 1.304(8) . ? N1 N2 1.329(9) . ? N2 N3 1.293(7) . ? N2 K1 2.918(4) . ? N2 K1 2.918(4) 1_545 ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? N3 Cu1 2.057(6) 5_656 ? K1 N2 2.918(4) 1_565 ? K1 I2 3.492(2) 5_666 ? K1 I2 3.5069(15) 3 ? K1 I2 3.5069(15) 3_545 ? K1 I1 3.6574(16) 1_565 ? K1 K1 4.2397(5) 1_565 ? K1 K1 4.2397(5) 1_545 ? 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 Cu1 I2 Cu1 105.56(4) 1_565 . ? Cu1 I2 K1 86.81(3) 1_565 5_666 ? Cu1 I2 K1 86.81(3) . 5_666 ? Cu1 I2 K1 164.00(3) 1_565 3_445 ? Cu1 I2 K1 89.92(3) . 3_445 ? K1 I2 K1 98.29(4) 5_666 3_445 ? Cu1 I2 K1 89.92(3) 1_565 3_455 ? Cu1 I2 K1 164.00(3) . 3_455 ? K1 I2 K1 98.29(4) 5_666 3_455 ? K1 I2 K1 74.38(4) 3_445 3_455 ? N4 Cu1 N3 114.9(2) . 5_656 ? N4 Cu1 I2 108.79(10) . 1_545 ? N3 Cu1 I2 109.18(8) 5_656 1_545 ? N4 Cu1 I2 108.79(10) . . ? N3 Cu1 I2 109.18(8) 5_656 . ? I2 Cu1 I2 105.56(4) 1_545 . ? Cu2 I1 Cu2 67.31(3) . 7_657 ? Cu2 I1 Cu2 67.31(3) . 7_647 ? Cu2 I1 Cu2 103.11(4) 7_657 7_647 ? Cu2 I1 K1 81.01(3) . 1_545 ? Cu2 I1 K1 141.61(3) 7_657 1_545 ? Cu2 I1 K1 82.87(3) 7_647 1_545 ? Cu2 I1 K1 81.01(3) . . ? Cu2 I1 K1 82.87(3) 7_657 . ? Cu2 I1 K1 141.61(3) 7_647 . ? K1 I1 K1 70.85(4) 1_545 . ? N1 Cu2 I1 111.21(17) . . ? N1 Cu2 I1 108.37(10) . 7_657 ? I1 Cu2 I1 112.69(3) . 7_657 ? N1 Cu2 I1 108.37(10) . 7_647 ? I1 Cu2 I1 112.69(3) . 7_647 ? I1 Cu2 I1 103.11(4) 7_657 7_647 ? N1 Cu2 Cu2 127.59(8) . 7_657 ? I1 Cu2 Cu2 57.49(3) . 7_657 ? I1 Cu2 Cu2 55.20(2) 7_657 7_657 ? I1 Cu2 Cu2 123.40(5) 7_647 7_657 ? N1 Cu2 Cu2 127.59(8) . 7_647 ? I1 Cu2 Cu2 57.49(3) . 7_647 ? I1 Cu2 Cu2 123.40(5) 7_657 7_647 ? I1 Cu2 Cu2 55.20(2) 7_647 7_647 ? Cu2 Cu2 Cu2 91.42(5) 7_657 7_647 ? N1 C1 N4 108.9(7) . . ? N1 C1 C2 126.1(7) . . ? N4 C1 C2 125.0(7) . . ? N3 N4 C1 105.3(6) . . ? N3 N4 Cu1 122.5(4) . . ? C1 N4 Cu1 132.3(5) . . ? N2 N1 C1 107.0(6) . . ? N2 N1 Cu2 122.2(4) . . ? C1 N1 Cu2 130.8(5) . . ? N3 N2 N1 106.9(5) . . ? N3 N2 K1 114.7(3) . . ? N1 N2 K1 113.6(3) . . ? N3 N2 K1 114.7(3) . 1_545 ? N1 N2 K1 113.6(3) . 1_545 ? K1 N2 K1 93.17(17) . 1_545 ? 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 . . ? N2 N3 N4 111.9(6) . . ? N2 N3 Cu1 125.5(5) . 5_656 ? N4 N3 Cu1 122.6(4) . 5_656 ? N2 K1 N2 93.17(17) . 1_565 ? N2 K1 I2 82.75(13) . 5_666 ? N2 K1 I2 82.75(13) 1_565 5_666 ? N2 K1 I2 161.84(14) . 3 ? N2 K1 I2 94.13(9) 1_565 3 ? I2 K1 I2 81.71(4) 5_666 3 ? N2 K1 I2 94.13(9) . 3_545 ? N2 K1 I2 161.84(14) 1_565 3_545 ? I2 K1 I2 81.71(4) 5_666 3_545 ? I2 K1 I2 74.38(4) 3 3_545 ? N2 K1 I1 122.52(13) . 1_565 ? N2 K1 I1 72.28(11) 1_565 1_565 ? I2 K1 I1 144.552(18) 5_666 1_565 ? I2 K1 I1 75.58(2) 3 1_565 ? I2 K1 I1 116.86(5) 3_545 1_565 ? N2 K1 I1 72.28(11) . . ? N2 K1 I1 122.52(13) 1_565 . ? I2 K1 I1 144.552(18) 5_666 . ? I2 K1 I1 116.86(5) 3 . ? I2 K1 I1 75.58(2) 3_545 . ? I1 K1 I1 70.85(4) 1_565 . ? N2 K1 K1 136.58(8) . 1_565 ? N2 K1 K1 43.42(8) 1_565 1_565 ? I2 K1 K1 90.0 5_666 1_565 ? I2 K1 K1 52.808(19) 3 1_565 ? I2 K1 K1 127.192(19) 3_545 1_565 ? I1 K1 K1 54.577(18) 1_565 1_565 ? I1 K1 K1 125.423(18) . 1_565 ? N2 K1 K1 43.42(8) . 1_545 ? N2 K1 K1 136.58(8) 1_565 1_545 ? I2 K1 K1 90.0 5_666 1_545 ? I2 K1 K1 127.192(19) 3 1_545 ? I2 K1 K1 52.808(19) 3_545 1_545 ? I1 K1 K1 125.423(18) 1_565 1_545 ? I1 K1 K1 54.577(18) . 1_545 ? K1 K1 K1 180.00(9) 1_565 1_545 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.17 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.549 _refine_diff_density_min -0.816 _refine_diff_density_rms 0.140 data_2 _database_code_depnum_ccdc_archive 'CCDC 713552' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H9 Cu3 I K N12' _chemical_formula_sum 'C6 H9 Cu3 I K N12' _chemical_formula_weight 605.87 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' K K 0.2009 0.2494 '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 _symmetry_space_group_name_Hall '-C 2y' 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 9.3946(14) _cell_length_b 13.260(2) _cell_length_c 12.7927(19) _cell_angle_alpha 90.00 _cell_angle_beta 92.674(2) _cell_angle_gamma 90.00 _cell_volume 1591.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1892 _cell_measurement_theta_min 1.59 _cell_measurement_theta_max 27.96 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.528 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 6.189 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1961 _exptl_absorpt_correction_T_max 0.2938 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 3989 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_sigmaI/netI 0.0301 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.20 _reflns_number_total 1509 _reflns_number_gt 1318 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0436P)^2^+14.0111P] 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 1509 _refine_ls_number_parameters 113 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0408 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0953 _refine_ls_wR_factor_gt 0.0923 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _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 I1 I 0.20432(6) 0.5000 0.60868(4) 0.0354(2) Uani 1 2 d S . . Cu1 Cu 0.15435(8) 0.37765(5) 0.77855(6) 0.0331(2) Uani 1 1 d . . . Cu2 Cu 0.08810(12) 0.5000 0.41606(8) 0.0333(3) Uani 1 2 d S . . N4 N 0.2660(5) 0.2527(4) 0.7469(4) 0.0324(11) Uani 1 1 d . . . N3 N 0.3918(5) 0.2305(4) 0.7959(4) 0.0320(11) Uani 1 1 d . . . C2 C 0.2509(6) 0.1865(4) 0.6686(4) 0.0297(12) Uani 1 1 d . . . N2 N 0.4484(5) 0.1547(4) 0.7490(3) 0.0281(10) Uani 1 1 d . . . N1 N 0.3620(5) 0.1246(3) 0.6679(3) 0.0262(10) Uani 1 1 d . . . C1 C 0.1259(7) 0.1825(6) 0.5934(5) 0.0451(17) Uani 1 1 d . . . H1A H 0.1543 0.1550 0.5281 0.068 Uiso 1 1 calc R . . H1B H 0.0889 0.2493 0.5822 0.068 Uiso 1 1 calc R . . H1C H 0.0535 0.1405 0.6212 0.068 Uiso 1 1 calc R . . N5 N 0.2244(5) 0.4512(4) 0.9059(4) 0.0325(11) Uani 1 1 d . . . N6 N 0.2877(6) 0.4167(4) 0.9958(4) 0.0371(12) Uani 1 1 d . . . C3 C 0.3237(10) 0.5000 1.0479(6) 0.0346(19) Uani 1 2 d S . . C4 C 0.3963(12) 0.5000 1.1558(7) 0.048(3) Uani 1 2 d S . . H4A H 0.3327 0.4728 1.2052 0.073 Uiso 0.50 1 calc PR . . H4B H 0.4214 0.5678 1.1754 0.073 Uiso 0.50 1 calc PR . . H4C H 0.4808 0.4594 1.1554 0.073 Uiso 0.50 1 calc PR . . K1 K 0.5000 0.24818(19) 1.0000 0.0627(7) Uani 1 2 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 I1 0.0366(3) 0.0389(4) 0.0301(3) 0.000 -0.0041(2) 0.000 Cu1 0.0304(4) 0.0311(4) 0.0364(4) -0.0055(3) -0.0115(3) 0.0002(3) Cu2 0.0382(6) 0.0272(5) 0.0338(6) 0.000 -0.0070(4) 0.000 N4 0.032(3) 0.032(3) 0.032(2) -0.006(2) -0.014(2) 0.007(2) N3 0.030(3) 0.036(3) 0.029(2) -0.004(2) -0.010(2) 0.004(2) C2 0.028(3) 0.032(3) 0.028(3) -0.003(2) -0.009(2) -0.001(2) N2 0.029(3) 0.028(3) 0.026(2) 0.0011(19) -0.0086(19) 0.001(2) N1 0.026(2) 0.024(2) 0.027(2) -0.0023(18) -0.0087(19) 0.0001(19) C1 0.037(4) 0.050(4) 0.046(4) -0.014(3) -0.019(3) 0.010(3) N5 0.038(3) 0.026(2) 0.032(3) 0.009(2) -0.014(2) -0.004(2) N6 0.050(3) 0.031(3) 0.029(3) 0.004(2) -0.011(2) 0.001(2) C3 0.043(5) 0.038(5) 0.022(4) 0.000 -0.004(4) 0.000 C4 0.061(7) 0.056(6) 0.026(4) 0.000 -0.019(4) 0.000 K1 0.0939(19) 0.0499(13) 0.0404(12) 0.000 -0.0377(12) 0.000 _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 Cu2 2.6482(12) . ? I1 Cu2 2.7507(13) 5_566 ? I1 Cu1 2.7695(9) 6_565 ? I1 Cu1 2.7695(9) . ? Cu1 N5 1.984(5) . ? Cu1 N2 2.000(5) 8_455 ? Cu1 N4 2.012(5) . ? Cu1 K1 3.6463(14) 7_557 ? Cu2 N1 2.038(4) 4_556 ? Cu2 N1 2.038(4) 7_556 ? Cu2 I1 2.7507(13) 5_566 ? Cu2 Cu2 2.772(2) 5_566 ? N4 C2 1.334(7) . ? N4 N3 1.344(6) . ? N3 N2 1.297(7) . ? N3 K1 2.768(4) . ? C2 N1 1.328(7) . ? C2 C1 1.485(7) . ? N2 N1 1.348(6) . ? N2 Cu1 2.000(5) 8 ? N1 Cu2 2.038(4) 7_556 ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? N5 N5 1.294(9) 6_565 ? N5 N6 1.351(6) . ? N6 C3 1.326(7) . ? N6 K1 2.994(6) . ? C3 N6 1.326(7) 6_565 ? C3 C4 1.511(11) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? K1 N3 2.768(4) 2_657 ? K1 N6 2.994(6) 2_657 ? K1 N2 3.455(4) 2_657 ? K1 Cu1 3.6463(14) 7_557 ? K1 Cu1 3.6463(14) 8 ? K1 K1 4.6975(7) 7_557 ? K1 K1 4.6975(7) 7_657 ? 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 Cu2 I1 Cu2 61.76(4) . 5_566 ? Cu2 I1 Cu1 130.73(3) . 6_565 ? Cu2 I1 Cu1 83.41(3) 5_566 6_565 ? Cu2 I1 Cu1 130.73(3) . . ? Cu2 I1 Cu1 83.41(3) 5_566 . ? Cu1 I1 Cu1 71.72(3) 6_565 . ? N5 Cu1 N2 122.8(2) . 8_455 ? N5 Cu1 N4 114.45(19) . . ? N2 Cu1 N4 107.1(2) 8_455 . ? N5 Cu1 I1 107.11(14) . . ? N2 Cu1 I1 100.09(13) 8_455 . ? N4 Cu1 I1 102.42(15) . . ? N5 Cu1 K1 73.50(14) . 7_557 ? N2 Cu1 K1 68.43(13) 8_455 7_557 ? N4 Cu1 K1 90.57(15) . 7_557 ? I1 Cu1 K1 164.97(4) . 7_557 ? N1 Cu2 N1 108.4(3) 4_556 7_556 ? N1 Cu2 I1 113.31(12) 4_556 . ? N1 Cu2 I1 113.31(12) 7_556 . ? N1 Cu2 I1 101.10(13) 4_556 5_566 ? N1 Cu2 I1 101.10(13) 7_556 5_566 ? I1 Cu2 I1 118.24(4) . 5_566 ? N1 Cu2 Cu2 124.69(13) 4_556 5_566 ? N1 Cu2 Cu2 124.69(13) 7_556 5_566 ? I1 Cu2 Cu2 60.94(4) . 5_566 ? I1 Cu2 Cu2 57.30(4) 5_566 5_566 ? C2 N4 N3 105.4(5) . . ? C2 N4 Cu1 130.9(4) . . ? N3 N4 Cu1 122.8(4) . . ? N2 N3 N4 109.0(4) . . ? N2 N3 K1 111.2(3) . . ? N4 N3 K1 134.2(4) . . ? N1 C2 N4 110.8(5) . . ? N1 C2 C1 124.9(5) . . ? N4 C2 C1 124.3(5) . . ? N3 N2 N1 109.9(4) . . ? N3 N2 Cu1 119.5(3) . 8 ? N1 N2 Cu1 128.7(4) . 8 ? C2 N1 N2 104.9(4) . . ? C2 N1 Cu2 134.8(4) . 7_556 ? N2 N1 Cu2 120.0(3) . 7_556 ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N5 N5 N6 109.8(3) 6_565 . ? N5 N5 Cu1 119.45(13) 6_565 . ? N6 N5 Cu1 130.4(4) . . ? C3 N6 N5 103.7(5) . . ? C3 N6 K1 117.3(5) . . ? N5 N6 K1 122.3(4) . . ? N6 C3 N6 112.9(7) . 6_565 ? N6 C3 C4 123.6(3) . . ? N6 C3 C4 123.6(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 . . ? N3 K1 N3 170.3(2) 2_657 . ? N3 K1 N6 80.30(14) 2_657 2_657 ? N3 K1 N6 107.15(15) . 2_657 ? N3 K1 N6 107.15(14) 2_657 . ? N3 K1 N6 80.30(14) . . ? N6 K1 N6 83.5(2) 2_657 . ? N3 K1 N2 20.50(12) 2_657 2_657 ? N3 K1 N2 151.16(15) . 2_657 ? N6 K1 N2 100.77(12) 2_657 2_657 ? N6 K1 N2 110.42(12) . 2_657 ? N3 K1 Cu1 50.95(10) 2_657 7_557 ? N3 K1 Cu1 123.54(12) . 7_557 ? N6 K1 Cu1 128.06(9) 2_657 7_557 ? N6 K1 Cu1 93.81(10) . 7_557 ? N2 K1 Cu1 32.58(8) 2_657 7_557 ? N3 K1 Cu1 123.54(12) 2_657 8 ? N3 K1 Cu1 50.95(10) . 8 ? N6 K1 Cu1 93.81(10) 2_657 8 ? N6 K1 Cu1 128.06(9) . 8 ? N2 K1 Cu1 120.93(10) 2_657 8 ? Cu1 K1 Cu1 125.53(7) 7_557 8 ? N3 K1 K1 108.90(10) 2_657 7_557 ? N3 K1 K1 71.20(10) . 7_557 ? N6 K1 K1 131.13(14) 2_657 7_557 ? N6 K1 K1 47.70(11) . 7_557 ? N2 K1 K1 95.78(8) 2_657 7_557 ? Cu1 K1 K1 64.58(2) 7_557 7_557 ? Cu1 K1 K1 116.01(4) 8 7_557 ? N3 K1 K1 71.20(10) 2_657 7_657 ? N3 K1 K1 108.90(10) . 7_657 ? N6 K1 K1 47.70(11) 2_657 7_657 ? N6 K1 K1 131.13(14) . 7_657 ? N2 K1 K1 84.65(8) 2_657 7_657 ? Cu1 K1 K1 116.01(4) 7_557 7_657 ? Cu1 K1 K1 64.58(2) 8 7_657 ? K1 K1 K1 178.83(12) 7_557 7_657 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.096 _refine_diff_density_min -1.038 _refine_diff_density_rms 0.139 data_3 _database_code_depnum_ccdc_archive 'CCDC 713553' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H9 Cu2 I N9 Na' _chemical_formula_sum 'C6 H9 Cu2 I N9 Na' _chemical_formula_weight 484.21 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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnma _symmetry_space_group_name_Hall '-P 2ac 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 9.5131(13) _cell_length_b 15.302(2) _cell_length_c 9.8789(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1438.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 8258 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 27.79 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.236 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 5.134 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2851 _exptl_absorpt_correction_T_max 0.3566 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 6752 _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_sigmaI/netI 0.0276 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 25.19 _reflns_number_total 1329 _reflns_number_gt 1106 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0362P)^2^+1.9885P] 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 1329 _refine_ls_number_parameters 103 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0424 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0757 _refine_ls_wR_factor_gt 0.0710 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 I1 I 0.13788(6) 0.7500 0.51342(5) 0.04800(19) Uani 1 2 d S . . Cu1 Cu 0.11152(6) 0.58104(4) 0.57621(6) 0.03311(18) Uani 1 1 d . . . N1 N 0.1748(4) 0.5060(2) 0.4206(4) 0.0305(8) Uani 1 1 d . . . N2 N 0.0945(4) 0.4390(2) 0.3783(4) 0.0279(8) Uani 1 1 d . . . C2 C 0.2865(5) 0.5054(3) 0.3388(5) 0.0348(11) Uani 1 1 d . . . C1 C 0.4063(6) 0.5665(4) 0.3516(8) 0.072(2) Uani 1 1 d . . . H1A H 0.4903 0.5343 0.3719 0.109 Uiso 1 1 calc R . . H1B H 0.3878 0.6074 0.4233 0.109 Uiso 1 1 calc R . . H1C H 0.4186 0.5977 0.2681 0.109 Uiso 1 1 calc R . . N4 N 0.2776(4) 0.4413(2) 0.2492(4) 0.0307(9) Uani 1 1 d . . . Na1 Na 0.0931(3) 0.2500 0.2196(3) 0.0489(7) Uani 1 2 d S . . N3 N 0.1568(4) 0.4000(2) 0.2759(4) 0.0323(9) Uani 1 1 d . . . N5 N -0.0850(11) 0.2500 0.0553(11) 0.091(3) Uani 1 2 d S . . C3 C -0.1626(12) 0.2690(13) -0.0245(12) 0.063(7) Uani 0.50 1 d PD A -1 C4 C -0.2569(15) 0.2988(13) -0.1309(13) 0.117(8) Uani 0.50 1 d PD A -1 H4A H -0.3472 0.3121 -0.0927 0.175 Uiso 0.50 1 calc PR A -1 H4B H -0.2670 0.2537 -0.1978 0.175 Uiso 0.50 1 calc PR A -1 H4C H -0.2188 0.3503 -0.1725 0.175 Uiso 0.50 1 calc PR A -1 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 0.0623(4) 0.0283(3) 0.0535(4) 0.000 0.0046(2) 0.000 Cu1 0.0301(3) 0.0336(3) 0.0357(3) -0.0062(2) -0.0012(2) -0.0036(2) N1 0.0274(19) 0.027(2) 0.037(2) -0.0082(17) 0.0001(16) -0.0047(16) N2 0.0281(19) 0.0246(19) 0.031(2) -0.0063(16) 0.0026(15) -0.0033(15) C2 0.029(2) 0.032(3) 0.043(3) -0.011(2) 0.006(2) -0.005(2) C1 0.051(4) 0.057(4) 0.109(6) -0.039(4) 0.026(4) -0.026(3) N4 0.0279(19) 0.0267(19) 0.037(2) -0.0031(17) 0.0058(16) -0.0060(16) Na1 0.0655(19) 0.0264(14) 0.0549(19) 0.000 -0.0057(15) 0.000 N3 0.030(2) 0.028(2) 0.039(2) -0.0046(18) 0.0013(16) -0.0032(16) N5 0.082(6) 0.102(8) 0.089(7) 0.000 -0.030(5) 0.000 C3 0.064(7) 0.07(2) 0.056(7) -0.003(7) 0.008(5) -0.009(7) C4 0.072(9) 0.22(2) 0.061(9) -0.018(11) -0.019(7) 0.035(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Cu1 2.6707(7) 7_575 ? I1 Cu1 2.6707(7) . ? I1 Na1 3.271(3) 2_565 ? I1 Na1 3.433(3) 5_566 ? Cu1 N1 2.011(4) . ? Cu1 N2 2.034(3) 5_566 ? Cu1 N4 2.038(4) 2_565 ? N1 C2 1.335(5) . ? N1 N2 1.345(5) . ? N2 N3 1.315(5) . ? N2 Cu1 2.034(3) 5_566 ? C2 N4 1.323(6) . ? C2 C1 1.480(7) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? N4 N3 1.338(5) . ? N4 Cu1 2.038(4) 2_564 ? Na1 N5 2.346(10) . ? Na1 N3 2.438(4) . ? Na1 N3 2.438(4) 7_565 ? Na1 I1 3.271(3) 2_564 ? Na1 I1 3.433(3) 5_566 ? N5 C3 1.118(13) 7_565 ? N5 C3 1.118(13) . ? C3 C4 1.456(9) . ? 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 Cu1 I1 Cu1 150.98(3) 7_575 . ? Cu1 I1 Na1 85.92(2) 7_575 2_565 ? Cu1 I1 Na1 85.92(2) . 2_565 ? Cu1 I1 Na1 76.198(17) 7_575 5_566 ? Cu1 I1 Na1 76.198(17) . 5_566 ? Na1 I1 Na1 91.28(2) 2_565 5_566 ? N1 Cu1 N2 111.80(14) . 5_566 ? N1 Cu1 N4 112.97(15) . 2_565 ? N2 Cu1 N4 106.75(15) 5_566 2_565 ? N1 Cu1 I1 110.31(11) . . ? N2 Cu1 I1 106.73(10) 5_566 . ? N4 Cu1 I1 107.99(10) 2_565 . ? C2 N1 N2 105.0(3) . . ? C2 N1 Cu1 134.9(3) . . ? N2 N1 Cu1 120.2(3) . . ? N3 N2 N1 109.2(3) . . ? N3 N2 Cu1 122.3(3) . 5_566 ? N1 N2 Cu1 126.4(3) . 5_566 ? N4 C2 N1 111.1(4) . . ? N4 C2 C1 125.1(4) . . ? N1 C2 C1 123.8(4) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 N4 N3 105.9(4) . . ? C2 N4 Cu1 130.7(3) . 2_564 ? N3 N4 Cu1 122.0(3) . 2_564 ? N5 Na1 N3 109.71(11) . . ? N5 Na1 N3 109.71(11) . 7_565 ? N3 Na1 N3 140.6(2) . 7_565 ? N5 Na1 I1 97.7(3) . 2_564 ? N3 Na1 I1 87.00(11) . 2_564 ? N3 Na1 I1 87.00(11) 7_565 2_564 ? N5 Na1 I1 94.0(3) . 5_566 ? N3 Na1 I1 89.07(12) . 5_566 ? N3 Na1 I1 89.07(12) 7_565 5_566 ? I1 Na1 I1 168.32(10) 2_564 5_566 ? N2 N3 N4 108.9(3) . . ? N2 N3 Na1 119.4(3) . . ? N4 N3 Na1 127.9(3) . . ? C3 N5 Na1 164.6(10) 7_565 . ? C3 N5 Na1 164.6(10) . . ? N5 C3 C4 175.9(18) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.19 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.548 _refine_diff_density_min -0.743 _refine_diff_density_rms 0.102