# 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 'Jing-Lin Zuo' _publ_contact_author_email ZUOJL@NETRA.NJU.EDU.CN _publ_section_title ; Hydrothermal Syntheses and Structures of Three Novel Coordination Polymers Assembled from 1,2,3-Triazole Ligands and Cd(II)/Cu(I) Salts ; loop_ _publ_author_name 'Jing-Lin Zuo' 'Xiao-Di Du' 'Yan-Hong Peng' 'Xiao-Zeng You' ; Xin-Hui Zhou ; # Attachment '1-3.cif' #============================================================================ data_1 _database_code_depnum_ccdc_archive 'CCDC 707173' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H6 Cd3 Cl3 N9' _chemical_formula_weight 647.75 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 8.7114(12) _cell_length_b 13.7087(18) _cell_length_c 11.8156(16) _cell_angle_alpha 90.00 _cell_angle_beta 93.082(2) _cell_angle_gamma 90.00 _cell_volume 1409.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 2037 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 28.1 _exptl_crystal_description rod _exptl_crystal_colour white _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.054 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 5.060 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3764 _exptl_absorpt_correction_T_max 0.4310 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 Smart Apex CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3734 _diffrn_reflns_av_R_equivalents 0.0819 _diffrn_reflns_av_sigmaI/netI 0.0637 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 26.00 _reflns_number_total 1381 _reflns_number_gt 1275 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0484P)^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 1381 _refine_ls_number_parameters 97 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0412 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.0962 _refine_ls_wR_factor_gt 0.0941 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _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 N5 N 0.5000 0.7004(5) 0.7500 0.0203(16) Uani 1 2 d S . . N4 N 0.3822(6) 0.6456(4) 0.7142(4) 0.0194(11) Uani 1 1 d . . . Cl2 Cl 0.18063(18) 0.63523(10) 0.44332(11) 0.0213(3) Uani 1 1 d . . . Cd2 Cd 0.0000 0.62670(4) 0.2500 0.0177(2) Uani 1 2 d S . . Cd1 Cd 0.15702(5) 0.71563(3) 0.64564(3) 0.01841(18) Uani 1 1 d . . . N3 N -0.0691(7) 0.7963(3) 0.6066(4) 0.0194(11) Uani 1 1 d . . . Cl1 Cl 0.0000 0.57107(14) 0.7500 0.0246(5) Uani 1 2 d S . . C1 C -0.2601(8) 0.8867(5) 0.5408(5) 0.0233(14) Uani 1 1 d . . . H1 H -0.3229 0.9253 0.4930 0.028 Uiso 1 1 calc R . . C2 C -0.1197(8) 0.8507(5) 0.5175(5) 0.0237(14) Uani 1 1 d . . . H2 H -0.0680 0.8618 0.4519 0.028 Uiso 1 1 calc R . . C3 C 0.4255(8) 0.5533(4) 0.7276(5) 0.0240(14) Uani 1 1 d . . . H3 H 0.3659 0.4986 0.7099 0.029 Uiso 1 1 calc R . . N1 N -0.2915(6) 0.8563(3) 0.6446(4) 0.0175(11) Uani 1 1 d . . . N2 N -0.1725(6) 0.8018(3) 0.6832(4) 0.0190(11) 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 N5 0.022(4) 0.025(4) 0.014(3) 0.000 0.000(3) 0.000 N4 0.015(3) 0.027(3) 0.016(2) -0.0016(19) -0.0038(19) 0.001(2) Cl2 0.0250(9) 0.0259(8) 0.0128(7) 0.0004(5) -0.0007(6) -0.0019(6) Cd2 0.0168(4) 0.0192(3) 0.0174(3) 0.000 0.0025(2) 0.000 Cd1 0.0164(3) 0.0247(3) 0.0139(3) -0.00250(15) -0.00021(18) 0.00209(17) N3 0.018(3) 0.027(3) 0.013(2) 0.0019(19) 0.0016(19) 0.003(2) Cl1 0.0286(13) 0.0156(9) 0.0301(11) 0.000 0.0070(9) 0.000 C1 0.022(4) 0.030(3) 0.018(3) 0.003(2) -0.002(2) 0.001(3) C2 0.025(4) 0.029(3) 0.018(3) 0.006(2) 0.007(2) 0.003(3) C3 0.027(4) 0.014(3) 0.031(3) -0.001(2) -0.003(3) -0.004(3) N1 0.019(3) 0.016(2) 0.018(2) 0.0029(18) -0.0022(19) -0.001(2) N2 0.019(3) 0.022(2) 0.016(2) 0.004(2) 0.002(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 N5 N4 1.322(6) . ? N5 N4 1.322(6) 2_656 ? N5 Cd2 2.371(7) 7_566 ? N4 C3 1.327(8) . ? N4 Cd1 2.292(5) . ? Cl2 Cd1 2.6504(14) . ? Cl2 Cd2 2.7057(14) . ? Cl2 Cd1 2.7286(15) 7_566 ? Cd2 N1 2.269(5) 8_565 ? Cd2 N1 2.269(5) 7_466 ? Cd2 N5 2.371(7) 7_566 ? Cd2 Cl2 2.7057(14) 2 ? Cd2 Cl1 2.711(2) 5_566 ? Cd1 N3 2.284(5) . ? Cd1 N2 2.339(5) 2_556 ? Cd1 Cl2 2.7286(15) 7_566 ? Cd1 Cl1 2.7386(15) . ? N3 N2 1.313(8) . ? N3 C2 1.345(8) . ? Cl1 Cd2 2.711(2) 5_566 ? Cl1 Cd1 2.7386(15) 2_556 ? C1 N1 1.338(7) . ? C1 C2 1.360(10) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C3 C3 1.375(14) 2_656 ? C3 H3 0.9300 . ? N1 N2 1.339(7) . ? N1 Cd2 2.269(5) 7_466 ? N2 Cd1 2.339(5) 2_556 ? 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 N5 N4 110.9(7) . 2_656 ? N4 N5 Cd2 124.6(3) . 7_566 ? N4 N5 Cd2 124.6(3) 2_656 7_566 ? N5 N4 C3 107.0(5) . . ? N5 N4 Cd1 120.7(4) . . ? C3 N4 Cd1 132.3(4) . . ? Cd1 Cl2 Cd2 135.20(6) . . ? Cd1 Cl2 Cd1 95.90(5) . 7_566 ? Cd2 Cl2 Cd1 89.83(4) . 7_566 ? N1 Cd2 N1 168.2(2) 8_565 7_466 ? N1 Cd2 N5 84.12(11) 8_565 7_566 ? N1 Cd2 N5 84.12(11) 7_466 7_566 ? N1 Cd2 Cl2 90.72(12) 8_565 . ? N1 Cd2 Cl2 88.77(12) 7_466 . ? N5 Cd2 Cl2 87.52(3) 7_566 . ? N1 Cd2 Cl2 88.77(12) 8_565 2 ? N1 Cd2 Cl2 90.72(12) 7_466 2 ? N5 Cd2 Cl2 87.52(3) 7_566 2 ? Cl2 Cd2 Cl2 175.05(6) . 2 ? N1 Cd2 Cl1 95.88(11) 8_565 5_566 ? N1 Cd2 Cl1 95.88(11) 7_466 5_566 ? N5 Cd2 Cl1 180.000(1) 7_566 5_566 ? Cl2 Cd2 Cl1 92.48(3) . 5_566 ? Cl2 Cd2 Cl1 92.48(3) 2 5_566 ? N3 Cd1 N4 170.50(17) . . ? N3 Cd1 N2 86.50(17) . 2_556 ? N4 Cd1 N2 84.12(17) . 2_556 ? N3 Cd1 Cl2 97.31(13) . . ? N4 Cd1 Cl2 92.18(13) . . ? N2 Cd1 Cl2 170.38(14) 2_556 . ? N3 Cd1 Cl2 91.06(13) . 7_566 ? N4 Cd1 Cl2 89.90(13) . 7_566 ? N2 Cd1 Cl2 87.01(13) 2_556 7_566 ? Cl2 Cd1 Cl2 84.10(5) . 7_566 ? N3 Cd1 Cl1 89.72(13) . . ? N4 Cd1 Cl1 88.66(13) . . ? N2 Cd1 Cl1 89.03(13) 2_556 . ? Cl2 Cd1 Cl1 99.79(4) . . ? Cl2 Cd1 Cl1 175.90(4) 7_566 . ? N2 N3 C2 107.5(5) . . ? N2 N3 Cd1 120.3(4) . . ? C2 N3 Cd1 132.0(5) . . ? Cd2 Cl1 Cd1 136.35(3) 5_566 . ? Cd2 Cl1 Cd1 136.35(3) 5_566 2_556 ? Cd1 Cl1 Cd1 87.29(6) . 2_556 ? N1 C1 C2 107.6(5) . . ? N1 C1 H1 126.2 . . ? C2 C1 H1 126.2 . . ? N3 C2 C1 107.6(6) . . ? N3 C2 H2 126.2 . . ? C1 C2 H2 126.2 . . ? N4 C3 C3 107.6(4) . 2_656 ? N4 C3 H3 126.2 . . ? C3 C3 H3 126.2 2_656 . ? C1 N1 N2 107.1(5) . . ? C1 N1 Cd2 132.9(4) . 7_466 ? N2 N1 Cd2 119.9(3) . 7_466 ? N3 N2 N1 110.1(4) . . ? N3 N2 Cd1 123.9(4) . 2_556 ? N1 N2 Cd1 125.8(4) . 2_556 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.384 _refine_diff_density_min -1.004 _refine_diff_density_rms 0.248 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 707174' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H24 Cd3 N18 O6' _chemical_formula_weight 853.69 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M 'Fd-3m ' _symmetry_space_group_name_Hall '-F 4vw 2vw 3 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+3/4, -y+1/4, z+1/2' '-x+1/4, y+1/2, -z+3/4' 'x+1/2, -y+3/4, -z+1/4' 'z, x, y' 'z+1/2, -x+3/4, -y+1/4' '-z+3/4, -x+1/4, y+1/2' '-z+1/4, x+1/2, -y+3/4' 'y, z, x' '-y+1/4, z+1/2, -x+3/4' 'y+1/2, -z+3/4, -x+1/4' '-y+3/4, -z+1/4, x+1/2' 'y+3/4, x+1/4, -z+1/2' '-y, -x, -z' 'y+1/4, -x+1/2, z+3/4' '-y+1/2, x+3/4, z+1/4' 'x+3/4, z+1/4, -y+1/2' '-x+1/2, z+3/4, y+1/4' '-x, -z, -y' 'x+1/4, -z+1/2, y+3/4' 'z+3/4, y+1/4, -x+1/2' 'z+1/4, -y+1/2, x+3/4' '-z+1/2, y+3/4, x+1/4' '-z, -y, -x' 'x, y+1/2, z+1/2' '-x+3/4, -y+3/4, z+1' '-x+1/4, y+1, -z+5/4' 'x+1/2, -y+5/4, -z+3/4' 'z, x+1/2, y+1/2' 'z+1/2, -x+5/4, -y+3/4' '-z+3/4, -x+3/4, y+1' '-z+1/4, x+1, -y+5/4' 'y, z+1/2, x+1/2' '-y+1/4, z+1, -x+5/4' 'y+1/2, -z+5/4, -x+3/4' '-y+3/4, -z+3/4, x+1' 'y+3/4, x+3/4, -z+1' '-y, -x+1/2, -z+1/2' 'y+1/4, -x+1, z+5/4' '-y+1/2, x+5/4, z+3/4' 'x+3/4, z+3/4, -y+1' '-x+1/2, z+5/4, y+3/4' '-x, -z+1/2, -y+1/2' 'x+1/4, -z+1, y+5/4' 'z+3/4, y+3/4, -x+1' 'z+1/4, -y+1, x+5/4' '-z+1/2, y+5/4, x+3/4' '-z, -y+1/2, -x+1/2' 'x+1/2, y, z+1/2' '-x+5/4, -y+1/4, z+1' '-x+3/4, y+1/2, -z+5/4' 'x+1, -y+3/4, -z+3/4' 'z+1/2, x, y+1/2' 'z+1, -x+3/4, -y+3/4' '-z+5/4, -x+1/4, y+1' '-z+3/4, x+1/2, -y+5/4' 'y+1/2, z, x+1/2' '-y+3/4, z+1/2, -x+5/4' 'y+1, -z+3/4, -x+3/4' '-y+5/4, -z+1/4, x+1' 'y+5/4, x+1/4, -z+1' '-y+1/2, -x, -z+1/2' 'y+3/4, -x+1/2, z+5/4' '-y+1, x+3/4, z+3/4' 'x+5/4, z+1/4, -y+1' '-x+1, z+3/4, y+3/4' '-x+1/2, -z, -y+1/2' 'x+3/4, -z+1/2, y+5/4' 'z+5/4, y+1/4, -x+1' 'z+3/4, -y+1/2, x+5/4' '-z+1, y+3/4, x+3/4' '-z+1/2, -y, -x+1/2' 'x+1/2, y+1/2, z' '-x+5/4, -y+3/4, z+1/2' '-x+3/4, y+1, -z+3/4' 'x+1, -y+5/4, -z+1/4' 'z+1/2, x+1/2, y' 'z+1, -x+5/4, -y+1/4' '-z+5/4, -x+3/4, y+1/2' '-z+3/4, x+1, -y+3/4' 'y+1/2, z+1/2, x' '-y+3/4, z+1, -x+3/4' 'y+1, -z+5/4, -x+1/4' '-y+5/4, -z+3/4, x+1/2' 'y+5/4, x+3/4, -z+1/2' '-y+1/2, -x+1/2, -z' 'y+3/4, -x+1, z+3/4' '-y+1, x+5/4, z+1/4' 'x+5/4, z+3/4, -y+1/2' '-x+1, z+5/4, y+1/4' '-x+1/2, -z+1/2, -y' 'x+3/4, -z+1, y+3/4' 'z+5/4, y+3/4, -x+1/2' 'z+3/4, -y+1, x+3/4' '-z+1, y+5/4, x+1/4' '-z+1/2, -y+1/2, -x' '-x, -y, -z' 'x-3/4, y-1/4, -z-1/2' 'x-1/4, -y-1/2, z-3/4' '-x-1/2, y-3/4, z-1/4' '-z, -x, -y' '-z-1/2, x-3/4, y-1/4' 'z-3/4, x-1/4, -y-1/2' 'z-1/4, -x-1/2, y-3/4' '-y, -z, -x' 'y-1/4, -z-1/2, x-3/4' '-y-1/2, z-3/4, x-1/4' 'y-3/4, z-1/4, -x-1/2' '-y-3/4, -x-1/4, z-1/2' 'y, x, z' '-y-1/4, x-1/2, -z-3/4' 'y-1/2, -x-3/4, -z-1/4' '-x-3/4, -z-1/4, y-1/2' 'x-1/2, -z-3/4, -y-1/4' 'x, z, y' '-x-1/4, z-1/2, -y-3/4' '-z-3/4, -y-1/4, x-1/2' '-z-1/4, y-1/2, -x-3/4' 'z-1/2, -y-3/4, -x-1/4' 'z, y, x' '-x, -y+1/2, -z+1/2' 'x-3/4, y+1/4, -z' 'x-1/4, -y, z-1/4' '-x-1/2, y-1/4, z+1/4' '-z, -x+1/2, -y+1/2' '-z-1/2, x-1/4, y+1/4' 'z-3/4, x+1/4, -y' 'z-1/4, -x, y-1/4' '-y, -z+1/2, -x+1/2' 'y-1/4, -z, x-1/4' '-y-1/2, z-1/4, x+1/4' 'y-3/4, z+1/4, -x' '-y-3/4, -x+1/4, z' 'y, x+1/2, z+1/2' '-y-1/4, x, -z-1/4' 'y-1/2, -x-1/4, -z+1/4' '-x-3/4, -z+1/4, y' 'x-1/2, -z-1/4, -y+1/4' 'x, z+1/2, y+1/2' '-x-1/4, z, -y-1/4' '-z-3/4, -y+1/4, x' '-z-1/4, y, -x-1/4' 'z-1/2, -y-1/4, -x+1/4' 'z, y+1/2, x+1/2' '-x+1/2, -y, -z+1/2' 'x-1/4, y-1/4, -z' 'x+1/4, -y-1/2, z-1/4' '-x, y-3/4, z+1/4' '-z+1/2, -x, -y+1/2' '-z, x-3/4, y+1/4' 'z-1/4, x-1/4, -y' 'z+1/4, -x-1/2, y-1/4' '-y+1/2, -z, -x+1/2' 'y+1/4, -z-1/2, x-1/4' '-y, z-3/4, x+1/4' 'y-1/4, z-1/4, -x' '-y-1/4, -x-1/4, z' 'y+1/2, x, z+1/2' '-y+1/4, x-1/2, -z-1/4' 'y, -x-3/4, -z+1/4' '-x-1/4, -z-1/4, y' 'x, -z-3/4, -y+1/4' 'x+1/2, z, y+1/2' '-x+1/4, z-1/2, -y-1/4' '-z-1/4, -y-1/4, x' '-z+1/4, y-1/2, -x-1/4' 'z, -y-3/4, -x+1/4' 'z+1/2, y, x+1/2' '-x+1/2, -y+1/2, -z' 'x-1/4, y+1/4, -z-1/2' 'x+1/4, -y, z-3/4' '-x, y-1/4, z-1/4' '-z+1/2, -x+1/2, -y' '-z, x-1/4, y-1/4' 'z-1/4, x+1/4, -y-1/2' 'z+1/4, -x, y-3/4' '-y+1/2, -z+1/2, -x' 'y+1/4, -z, x-3/4' '-y, z-1/4, x-1/4' 'y-1/4, z+1/4, -x-1/2' '-y-1/4, -x+1/4, z-1/2' 'y+1/2, x+1/2, z' '-y+1/4, x, -z-3/4' 'y, -x-1/4, -z-1/4' '-x-1/4, -z+1/4, y-1/2' 'x, -z-1/4, -y-1/4' 'x+1/2, z+1/2, y' '-x+1/4, z, -y-3/4' '-z-1/4, -y+1/4, x-1/2' '-z+1/4, y, -x-3/4' 'z, -y-1/4, -x-1/4' 'z+1/2, y+1/2, x' _cell_length_a 18.5954(8) _cell_length_b 18.5954(8) _cell_length_c 18.5954(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6430.1(5) _cell_formula_units_Z 8 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 1452 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.3 _exptl_crystal_description block _exptl_crystal_colour white _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.764 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3312 _exptl_absorpt_coefficient_mu 2.021 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7935 _exptl_absorpt_correction_T_max 0.8235 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 Smart Apex CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8287 _diffrn_reflns_av_R_equivalents 0.0887 _diffrn_reflns_av_sigmaI/netI 0.0301 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 25.94 _reflns_number_total 343 _reflns_number_gt 291 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0109P)^2^+54.2605P] 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 343 _refine_ls_number_parameters 26 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0490 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0649 _refine_ls_wR_factor_gt 0.0628 _refine_ls_goodness_of_fit_ref 1.326 _refine_ls_restrained_S_all 1.326 _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 C1 C 0.0995(2) 0.3877(4) 0.0995(2) 0.0442(16) Uani 1 2 d S . . H1 H 0.0786 0.3474 0.0786 0.053 Uiso 1 2 calc SR . . Cd1 Cd 0.0000 0.5000 0.0000 0.0292(3) Uani 1 12 d S . . Cd2 Cd 0.1250 0.6250 0.1250 0.0290(4) Uani 1 24 d S . . N1 N 0.08370(18) 0.4578(3) 0.08370(18) 0.0373(12) Uani 1 2 d S . . N2 N 0.1250 0.4979(4) 0.1250 0.0361(17) Uani 1 4 d S . . O1 O 0.1330(5) 0.2262(3) 0.0238(3) 0.046(2) Uani 0.50 2 d SP . . 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 C1 0.042(2) 0.048(4) 0.042(2) -0.004(2) -0.020(3) -0.004(2) Cd1 0.0292(3) 0.0292(3) 0.0292(3) -0.0060(3) -0.0060(3) -0.0060(3) Cd2 0.0290(4) 0.0290(4) 0.0290(4) 0.000 0.000 0.000 N1 0.0375(19) 0.037(3) 0.0375(19) -0.0070(16) -0.010(2) -0.0070(16) N2 0.038(3) 0.032(4) 0.038(3) 0.000 -0.007(3) 0.000 O1 0.047(6) 0.045(3) 0.045(3) -0.004(4) -0.011(3) 0.011(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 C1 C1 1.343(12) 27_544 ? C1 N1 1.367(8) . ? C1 H1 0.9300 . ? Cd1 N1 2.337(5) 29_554 ? Cd1 N1 2.337(5) 97_565 ? Cd1 N1 2.337(5) . ? Cd1 N1 2.337(5) 81_455 ? Cd1 N1 2.337(5) 125 ? Cd1 N1 2.337(5) 177 ? Cd2 N2 2.364(7) 58_554 ? Cd2 N2 2.364(7) 50_464 ? Cd2 N2 2.364(7) . ? Cd2 N2 2.364(7) 29_554 ? Cd2 N2 2.364(7) 54_455 ? Cd2 N2 2.364(7) 81_455 ? N1 N2 1.318(6) . ? N2 N1 1.318(6) 27_544 ? 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 C1 C1 N1 107.6(3) 27_544 . ? C1 C1 H1 126.2 27_544 . ? N1 C1 H1 126.2 . . ? N1 Cd1 N1 89.78(17) 29_554 97_565 ? N1 Cd1 N1 90.22(17) 29_554 . ? N1 Cd1 N1 180.0(2) 97_565 . ? N1 Cd1 N1 90.22(17) 29_554 81_455 ? N1 Cd1 N1 89.78(17) 97_565 81_455 ? N1 Cd1 N1 90.22(17) . 81_455 ? N1 Cd1 N1 180.0 29_554 125 ? N1 Cd1 N1 90.22(17) 97_565 125 ? N1 Cd1 N1 89.78(17) . 125 ? N1 Cd1 N1 89.78(17) 81_455 125 ? N1 Cd1 N1 89.78(17) 29_554 177 ? N1 Cd1 N1 90.22(17) 97_565 177 ? N1 Cd1 N1 89.78(17) . 177 ? N1 Cd1 N1 180.0(2) 81_455 177 ? N1 Cd1 N1 90.22(17) 125 177 ? N2 Cd2 N2 90.000(1) 58_554 50_464 ? N2 Cd2 N2 90.0 58_554 . ? N2 Cd2 N2 180.0 50_464 . ? N2 Cd2 N2 90.0 58_554 29_554 ? N2 Cd2 N2 90.0 50_464 29_554 ? N2 Cd2 N2 90.0 . 29_554 ? N2 Cd2 N2 90.0 58_554 54_455 ? N2 Cd2 N2 90.0 50_464 54_455 ? N2 Cd2 N2 90.0 . 54_455 ? N2 Cd2 N2 180.000(1) 29_554 54_455 ? N2 Cd2 N2 180.0 58_554 81_455 ? N2 Cd2 N2 90.0 50_464 81_455 ? N2 Cd2 N2 90.000(1) . 81_455 ? N2 Cd2 N2 90.000(1) 29_554 81_455 ? N2 Cd2 N2 90.0 54_455 81_455 ? N2 N1 C1 106.8(5) . . ? N2 N1 Cd1 125.9(4) . . ? C1 N1 Cd1 127.3(4) . . ? N1 N2 N1 111.0(7) . 27_544 ? N1 N2 Cd2 124.5(4) . . ? N1 N2 Cd2 124.5(4) 27_544 . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.94 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.369 _refine_diff_density_min -0.752 _refine_diff_density_rms 0.104 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 707175' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H6 Cu6 I3 N9' _chemical_formula_weight 966.14 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' 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' N N 0.0061 0.0033 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 17.540(4) _cell_length_b 18.008(4) _cell_length_c 11.256(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3555.3(15) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2420 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 25.8 _exptl_crystal_description block _exptl_crystal_colour white _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.610 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3504 _exptl_absorpt_coefficient_mu 12.268 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2605 _exptl_absorpt_correction_T_max 0.2785 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _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 Smart Apex CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16760 _diffrn_reflns_av_R_equivalents 0.1495 _diffrn_reflns_av_sigmaI/netI 0.1064 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3239 _reflns_number_gt 2463 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0348P)^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 3239 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0851 _refine_ls_R_factor_gt 0.0589 _refine_ls_wR_factor_ref 0.1185 _refine_ls_wR_factor_gt 0.1096 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 1.01695(8) 0.34894(10) 0.19955(15) 0.0361(5) Uani 1 1 d . . . Cu2 Cu 0.88396(13) 0.2500 0.0293(3) 0.0422(7) Uani 1 2 d S . . Cu3 Cu 0.74814(9) 0.35990(10) -0.09600(16) 0.0413(5) Uani 1 1 d . . . Cu4 Cu 1.08419(9) 0.33644(10) 0.41889(15) 0.0395(5) Uani 1 1 d . . . Cu5 Cu 1.16444(8) 0.34567(10) 0.21575(15) 0.0348(4) Uani 1 1 d . . . Cu6 Cu 0.92568(9) 0.35565(11) -0.40419(16) 0.0414(5) Uani 1 1 d . . . Cu7 Cu 1.28153(13) 0.2500 0.0040(2) 0.0387(6) Uani 1 2 d S . . I1 I 1.09794(6) 0.2500 0.06348(10) 0.0238(3) Uani 1 2 d S . . I2 I 0.71164(6) 0.2500 0.11421(10) 0.0241(3) Uani 1 2 d S . . I3 I 1.08861(5) 0.46191(5) 0.29944(8) 0.0314(2) Uani 1 1 d . . . I4 I 0.96347(6) 0.2500 0.35730(10) 0.0260(3) Uani 1 2 d S . . I5 I 0.83399(6) 0.2500 -0.26188(10) 0.0321(3) Uani 1 2 d S . . C1 C 0.9168(7) 0.4646(7) 0.0820(13) 0.032(3) Uani 1 1 d . . . H1 H 0.9421 0.5056 0.1130 0.039 Uiso 1 1 calc R . . C2 C 0.8544(8) 0.4675(7) 0.0172(12) 0.037(4) Uani 1 1 d . . . H2 H 0.8283 0.5106 -0.0033 0.044 Uiso 1 1 calc R . . C3 C 0.6271(7) 0.3521(7) -0.2786(10) 0.026(3) Uani 1 1 d . . . H3 H 0.6582 0.3527 -0.3455 0.031 Uiso 1 1 calc R . . C4 C 0.5486(7) 0.3511(7) -0.2755(10) 0.025(3) Uani 1 1 d . . . H4 H 0.5171 0.3511 -0.3420 0.030 Uiso 1 1 calc R . . H5 H 1.3897 0.4886 0.0821 0.030 Uiso 1 1 d R . . H6 H 1.2846 0.4824 0.2233 0.030 Uiso 1 1 d R . . C5 C 1.3536(7) 0.4507(7) 0.0852(12) 0.032(3) Uani 1 1 d . . . C6 C 1.2956(7) 0.4482(7) 0.1637(11) 0.026(3) Uani 1 1 d . . . N1 N 0.9382(5) 0.3940(6) 0.0967(9) 0.023(2) Uani 1 1 d . . . N2 N 0.8859(5) 0.3539(6) 0.0369(9) 0.026(3) Uani 1 1 d . . . N3 N 0.8345(5) 0.3982(6) -0.0146(9) 0.031(3) Uani 1 1 d . . . N4 N 0.6491(5) 0.3522(5) -0.1643(9) 0.023(2) Uani 1 1 d . . . N5 N 0.5867(5) 0.3489(6) -0.0944(9) 0.026(2) Uani 1 1 d . . . N6 N 0.5245(5) 0.3500(6) -0.1651(10) 0.032(3) Uani 1 1 d . . . N7 N 1.3528(5) 0.3930(5) 0.0146(9) 0.027(3) Uani 1 1 d . . . N8 N 1.2910(5) 0.3528(5) 0.0476(8) 0.021(2) Uani 1 1 d . . . N9 N 1.2574(5) 0.3861(5) 0.1379(8) 0.019(2) 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 0.0263(9) 0.0405(11) 0.0415(11) 0.0037(9) -0.0141(8) 0.0019(8) Cu2 0.0369(14) 0.0249(14) 0.065(2) 0.000 -0.0138(13) 0.000 Cu3 0.0205(9) 0.0604(13) 0.0431(11) 0.0100(10) -0.0126(8) -0.0084(8) Cu4 0.0420(10) 0.0545(12) 0.0218(9) -0.0012(9) 0.0003(8) -0.0009(9) Cu5 0.0235(9) 0.0428(11) 0.0380(10) 0.0030(8) 0.0112(7) -0.0040(8) Cu6 0.0228(9) 0.0613(13) 0.0400(11) -0.0091(10) -0.0125(8) 0.0090(8) Cu7 0.0348(14) 0.0274(14) 0.0538(17) 0.000 0.0037(12) 0.000 I1 0.0230(6) 0.0316(7) 0.0168(6) 0.000 -0.0008(5) 0.000 I2 0.0191(6) 0.0315(7) 0.0218(6) 0.000 0.0054(5) 0.000 I3 0.0334(5) 0.0308(5) 0.0300(5) -0.0051(4) -0.0013(4) 0.0005(4) I4 0.0196(6) 0.0325(7) 0.0259(7) 0.000 0.0053(5) 0.000 I5 0.0266(7) 0.0460(8) 0.0238(7) 0.000 0.0041(5) 0.000 C1 0.021(7) 0.030(8) 0.045(9) 0.000(7) -0.009(6) -0.002(6) C2 0.046(9) 0.016(8) 0.048(9) 0.012(7) -0.008(7) 0.000(6) C3 0.041(8) 0.030(8) 0.007(6) 0.002(5) 0.005(6) 0.006(6) C4 0.023(7) 0.045(9) 0.007(6) -0.009(6) -0.002(5) -0.003(6) C5 0.027(7) 0.031(8) 0.037(9) 0.005(7) -0.001(6) -0.001(6) C6 0.026(7) 0.022(7) 0.031(7) -0.004(6) 0.008(6) 0.004(5) N1 0.017(5) 0.024(6) 0.028(6) 0.004(5) -0.005(5) 0.000(4) N2 0.023(6) 0.020(6) 0.034(7) 0.003(5) -0.008(5) -0.005(4) N3 0.017(6) 0.046(8) 0.032(7) 0.015(6) -0.010(5) -0.004(5) N4 0.008(5) 0.035(7) 0.028(6) -0.001(5) 0.000(4) 0.001(4) N5 0.020(5) 0.036(6) 0.023(6) 0.004(5) 0.001(5) 0.010(5) N6 0.026(6) 0.040(7) 0.030(7) -0.012(6) 0.002(5) 0.007(5) N7 0.023(6) 0.020(6) 0.037(7) 0.007(5) 0.001(5) 0.002(5) N8 0.016(5) 0.027(6) 0.019(5) 0.004(5) 0.002(4) 0.002(4) N9 0.018(5) 0.017(6) 0.023(6) 0.001(5) 0.002(4) 0.006(4) _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 1.976(9) . ? Cu1 Cu5 2.594(2) . ? Cu1 I3 2.6425(19) . ? Cu1 I4 2.685(2) . ? Cu1 Cu4 2.745(2) . ? Cu1 I1 2.7456(19) . ? Cu2 N2 1.872(10) . ? Cu2 N2 1.872(10) 8_565 ? Cu2 I2 3.170(3) . ? Cu3 N3 1.900(10) . ? Cu3 N4 1.904(9) . ? Cu3 I5 3.110(2) . ? Cu4 N5 1.988(10) 6_656 ? Cu4 I3 2.630(2) . ? Cu4 Cu5 2.690(2) . ? Cu4 I4 2.718(2) . ? Cu4 I2 2.749(2) 6_656 ? Cu5 N9 1.990(9) . ? Cu5 I3 2.6529(19) . ? Cu5 I1 2.6955(19) . ? Cu5 I2 2.705(2) 6_656 ? Cu6 N6 1.904(10) 6_655 ? Cu6 N7 1.906(10) 6 ? Cu6 I5 2.962(2) . ? Cu7 N8 1.922(10) . ? Cu7 N8 1.922(10) 8_565 ? Cu7 I5 2.877(3) 6_655 ? I1 Cu5 2.6955(19) 8_565 ? I1 Cu1 2.7456(19) 8_565 ? I2 Cu5 2.705(2) 6_556 ? I2 Cu5 2.705(2) 3_455 ? I2 Cu4 2.749(2) 3_455 ? I2 Cu4 2.749(2) 6_556 ? I4 Cu1 2.685(2) 8_565 ? I4 Cu4 2.718(2) 8_565 ? I5 Cu7 2.877(3) 6 ? I5 Cu6 2.962(2) 8_565 ? I5 Cu3 3.110(2) 8_565 ? C1 C2 1.316(17) . ? C1 N1 1.335(15) . ? C1 H1 0.9300 . ? C2 N3 1.344(16) . ? C2 H2 0.9300 . ? C3 N4 1.343(15) . ? C3 C4 1.378(16) . ? C3 H3 0.9300 . ? C4 N6 1.312(15) . ? C4 H4 0.9300 . ? C5 N7 1.308(15) . ? C5 C6 1.349(16) . ? C5 H5 0.9308 . ? C6 N9 1.334(15) . ? C6 H6 0.9309 . ? N1 N2 1.349(13) . ? N2 N3 1.336(13) . ? N4 N5 1.350(13) . ? N5 N6 1.350(13) . ? N5 Cu4 1.988(10) 6_556 ? N6 Cu6 1.904(10) 6 ? N7 N8 1.355(12) . ? N7 Cu6 1.906(10) 6_655 ? N8 N9 1.320(12) . ? 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 Cu5 138.3(3) . . ? N1 Cu1 I3 105.4(3) . . ? Cu5 Cu1 I3 60.87(5) . . ? N1 Cu1 I4 114.6(3) . . ? Cu5 Cu1 I4 106.67(7) . . ? I3 Cu1 I4 113.31(7) . . ? N1 Cu1 Cu4 149.4(3) . . ? Cu5 Cu1 Cu4 60.43(6) . . ? I3 Cu1 Cu4 58.41(5) . . ? I4 Cu1 Cu4 60.06(6) . . ? N1 Cu1 I1 107.5(3) . . ? Cu5 Cu1 I1 60.56(5) . . ? I3 Cu1 I1 119.39(6) . . ? I4 Cu1 I1 96.84(6) . . ? Cu4 Cu1 I1 103.07(7) . . ? N2 Cu2 N2 174.4(6) . 8_565 ? N2 Cu2 I2 90.2(3) . . ? N2 Cu2 I2 90.2(3) 8_565 . ? N3 Cu3 N4 161.5(5) . . ? N3 Cu3 I5 97.7(3) . . ? N4 Cu3 I5 98.8(3) . . ? N5 Cu4 I3 114.2(3) 6_656 . ? N5 Cu4 Cu5 145.7(3) 6_656 . ? I3 Cu4 Cu5 59.80(6) . . ? N5 Cu4 I4 109.6(3) 6_656 . ? I3 Cu4 I4 112.61(7) . . ? Cu5 Cu4 I4 103.07(7) . . ? N5 Cu4 Cu1 153.3(3) 6_656 . ? I3 Cu4 Cu1 58.84(5) . . ? Cu5 Cu4 Cu1 57.00(6) . . ? I4 Cu4 Cu1 58.86(5) . . ? N5 Cu4 I2 100.4(3) 6_656 6_656 ? I3 Cu4 I2 113.15(6) . 6_656 ? Cu5 Cu4 I2 59.63(6) . 6_656 ? I4 Cu4 I2 105.94(7) . 6_656 ? Cu1 Cu4 I2 105.89(7) . 6_656 ? N9 Cu5 Cu1 141.1(3) . . ? N9 Cu5 I3 106.2(3) . . ? Cu1 Cu5 I3 60.47(5) . . ? N9 Cu5 Cu4 145.7(3) . . ? Cu1 Cu5 Cu4 62.57(6) . . ? I3 Cu5 Cu4 58.98(6) . . ? N9 Cu5 I1 108.0(3) . . ? Cu1 Cu5 I1 62.50(6) . . ? I3 Cu5 I1 120.88(6) . . ? Cu4 Cu5 I1 105.94(7) . . ? N9 Cu5 I2 107.1(3) . 6_656 ? Cu1 Cu5 I2 111.68(7) . 6_656 ? I3 Cu5 I2 113.87(7) . 6_656 ? Cu4 Cu5 I2 61.27(6) . 6_656 ? I1 Cu5 I2 100.10(6) . 6_656 ? N6 Cu6 N7 153.8(5) 6_655 6 ? N6 Cu6 I5 103.8(3) 6_655 . ? N7 Cu6 I5 102.4(3) 6 . ? N8 Cu7 N8 148.7(6) . 8_565 ? N8 Cu7 I5 102.4(3) . 6_655 ? N8 Cu7 I5 102.4(3) 8_565 6_655 ? Cu5 I1 Cu5 79.45(8) . 8_565 ? Cu5 I1 Cu1 56.94(5) . . ? Cu5 I1 Cu1 106.49(6) 8_565 . ? Cu5 I1 Cu1 106.49(6) . 8_565 ? Cu5 I1 Cu1 56.94(5) 8_565 8_565 ? Cu1 I1 Cu1 80.92(8) . 8_565 ? Cu5 I2 Cu5 79.12(8) 6_556 3_455 ? Cu5 I2 Cu4 101.98(6) 6_556 3_455 ? Cu5 I2 Cu4 59.10(5) 3_455 3_455 ? Cu5 I2 Cu4 59.10(5) 6_556 6_556 ? Cu5 I2 Cu4 101.98(6) 3_455 6_556 ? Cu4 I2 Cu4 68.97(8) 3_455 6_556 ? Cu5 I2 Cu2 120.34(5) 6_556 . ? Cu5 I2 Cu2 120.34(5) 3_455 . ? Cu4 I2 Cu2 137.26(5) 3_455 . ? Cu4 I2 Cu2 137.26(5) 6_556 . ? Cu4 I3 Cu1 62.75(6) . . ? Cu4 I3 Cu5 61.22(6) . . ? Cu1 I3 Cu5 58.66(5) . . ? Cu1 I4 Cu1 83.16(8) 8_565 . ? Cu1 I4 Cu4 106.05(6) 8_565 . ? Cu1 I4 Cu4 61.08(5) . . ? Cu1 I4 Cu4 61.08(5) 8_565 8_565 ? Cu1 I4 Cu4 106.05(6) . 8_565 ? Cu4 I4 Cu4 69.88(8) . 8_565 ? Cu7 I5 Cu6 70.20(5) 6 . ? Cu7 I5 Cu6 70.20(5) 6 8_565 ? Cu6 I5 Cu6 79.94(8) . 8_565 ? Cu7 I5 Cu3 114.45(5) 6 8_565 ? Cu6 I5 Cu3 175.19(6) . 8_565 ? Cu6 I5 Cu3 100.30(5) 8_565 8_565 ? Cu7 I5 Cu3 114.45(5) 6 . ? Cu6 I5 Cu3 100.30(5) . . ? Cu6 I5 Cu3 175.19(6) 8_565 . ? Cu3 I5 Cu3 79.05(7) 8_565 . ? C2 C1 N1 110.0(12) . . ? C2 C1 H1 125.0 . . ? N1 C1 H1 125.0 . . ? C1 C2 N3 109.0(11) . . ? C1 C2 H2 125.5 . . ? N3 C2 H2 125.5 . . ? N4 C3 C4 105.3(10) . . ? N4 C3 H3 127.4 . . ? C4 C3 H3 127.4 . . ? N6 C4 C3 110.2(10) . . ? N6 C4 H4 124.9 . . ? C3 C4 H4 124.9 . . ? N7 C5 C6 111.3(12) . . ? N7 C5 H5 124.5 . . ? C6 C5 H5 124.2 . . ? N9 C6 C5 105.3(11) . . ? N9 C6 H6 127.5 . . ? C5 C6 H6 127.2 . . ? C1 N1 N2 104.9(9) . . ? C1 N1 Cu1 131.3(9) . . ? N2 N1 Cu1 123.2(8) . . ? N3 N2 N1 110.8(9) . . ? N3 N2 Cu2 124.4(8) . . ? N1 N2 Cu2 124.8(8) . . ? N2 N3 C2 105.3(10) . . ? N2 N3 Cu3 122.0(8) . . ? C2 N3 Cu3 132.2(9) . . ? C3 N4 N5 109.0(9) . . ? C3 N4 Cu3 130.5(8) . . ? N5 N4 Cu3 120.5(8) . . ? N4 N5 N6 108.1(10) . . ? N4 N5 Cu4 127.1(7) . 6_556 ? N6 N5 Cu4 124.7(7) . 6_556 ? C4 N6 N5 107.4(9) . . ? C4 N6 Cu6 132.8(9) . 6 ? N5 N6 Cu6 119.7(8) . 6 ? C5 N7 N8 105.5(10) . . ? C5 N7 Cu6 132.0(9) . 6_655 ? N8 N7 Cu6 121.7(8) . 6_655 ? N9 N8 N7 108.9(9) . . ? N9 N8 Cu7 126.6(7) . . ? N7 N8 Cu7 121.0(7) . . ? N8 N9 C6 109.0(9) . . ? N8 N9 Cu5 122.6(7) . . ? C6 N9 Cu5 128.4(8) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.697 _refine_diff_density_min -1.486 _refine_diff_density_rms 0.293 #===END