Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Christian Nather' _publ_contact_author_address ; Institut fur Anorganische Chemie Universitat Kiel Olshausenstr. 40 Kiel 24098 GERMANY ; _publ_contact_author_email CNAETHER@AC.UNI-KIEL.DE _publ_section_title ; Synthesis, Crystal Structure, Thermal and Luminescence Properties of CuX(2,3-dimethylpyrazine) (X = Cl, Br, I) Coordination Polymers ; loop_ _publ_author_name 'Christian Nather' 'Inke Jess' 'Jiri Pospisil' 'Petr Taborsky' data_Compound_1 _database_code_depnum_ccdc_archive 'CCDC 636026' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H24 Cu2 I2 N6' _chemical_formula_weight 705.31 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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.2001(12) _cell_length_b 11.2746(6) _cell_length_c 14.3556(10) _cell_angle_alpha 90.00 _cell_angle_beta 101.345(9) _cell_angle_gamma 90.00 _cell_volume 2253.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.079 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 4.644 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11218 _diffrn_reflns_av_R_equivalents 0.0477 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 27.10 _reflns_number_total 5042 _reflns_number_gt 3755 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0553P)^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 5042 _refine_ls_number_parameters 260 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0547 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.0913 _refine_ls_wR_factor_gt 0.0853 _refine_ls_goodness_of_fit_ref 0.951 _refine_ls_restrained_S_all 0.951 _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 0.07446(4) 0.92475(5) 0.54349(4) 0.02275(13) Uani 1 1 d . . . I1 I -0.09295(2) 0.92531(3) 0.595903(19) 0.02379(9) Uani 1 1 d . . . Cu2 Cu 0.45407(4) 0.93004(5) 0.92472(4) 0.02372(13) Uani 1 1 d . . . I2 I 0.59630(2) 1.07883(3) 0.90838(2) 0.02575(9) Uani 1 1 d . . . N1 N 0.1933(2) 0.9539(3) 0.6518(2) 0.0173(7) Uani 1 1 d . . . C1 C 0.2047(3) 1.0432(4) 0.7146(3) 0.0172(8) Uani 1 1 d . . . C2 C 0.2835(3) 1.0450(4) 0.7919(3) 0.0172(8) Uani 1 1 d . . . N2 N 0.3476(3) 0.9561(3) 0.8045(2) 0.0192(7) Uani 1 1 d . . . C3 C 0.3380(3) 0.8709(4) 0.7380(3) 0.0191(8) Uani 1 1 d . . . H3 H 0.3841 0.8103 0.7432 0.023 Uiso 1 1 calc R . . C4 C 0.2617(3) 0.8711(4) 0.6624(3) 0.0198(9) Uani 1 1 d . . . H4 H 0.2576 0.8107 0.6166 0.024 Uiso 1 1 calc R . . C5 C 0.1316(3) 1.1389(4) 0.7016(3) 0.0265(10) Uani 1 1 d . . . H5A H 0.1635 1.2154 0.7102 0.040 Uiso 1 1 calc R . . H5B H 0.0909 1.1298 0.7480 0.040 Uiso 1 1 calc R . . H5C H 0.0927 1.1342 0.6381 0.040 Uiso 1 1 calc R . . C6 C 0.2987(4) 1.1429(5) 0.8626(4) 0.0305(11) Uani 1 1 d . . . H6A H 0.2552 1.1333 0.9064 0.046 Uiso 1 1 calc R . . H6B H 0.2864 1.2184 0.8300 0.046 Uiso 1 1 calc R . . H6C H 0.3645 1.1410 0.8977 0.046 Uiso 1 1 calc R . . N11 N 0.0954(2) 0.7484(3) 0.4956(2) 0.0180(7) Uani 1 1 d . . . C11 C 0.1039(3) 0.6489(4) 0.5466(3) 0.0179(8) Uani 1 1 d . . . C12 C 0.1175(3) 0.5379(4) 0.5055(3) 0.0215(9) Uani 1 1 d . . . N12 N 0.1150(3) 0.5278(4) 0.4119(3) 0.0279(9) Uani 1 1 d . . . C13 C 0.1033(4) 0.6285(4) 0.3615(3) 0.0295(11) Uani 1 1 d . . . H13 H 0.1002 0.6243 0.2956 0.035 Uiso 1 1 calc R . . C14 C 0.0959(3) 0.7373(4) 0.4017(3) 0.0220(9) Uani 1 1 d . . . H14 H 0.0910 0.8056 0.3634 0.026 Uiso 1 1 calc R . . C15 C 0.0984(4) 0.6561(4) 0.6500(3) 0.0303(11) Uani 1 1 d . . . H15A H 0.1615 0.6420 0.6886 0.045 Uiso 1 1 calc R . . H15B H 0.0538 0.5968 0.6642 0.045 Uiso 1 1 calc R . . H15C H 0.0762 0.7344 0.6638 0.045 Uiso 1 1 calc R . . C16 C 0.1345(4) 0.4259(4) 0.5626(4) 0.0317(11) Uani 1 1 d . . . H16A H 0.1255 0.3581 0.5202 0.048 Uiso 1 1 calc R . . H16B H 0.0895 0.4215 0.6053 0.048 Uiso 1 1 calc R . . H16C H 0.1997 0.4257 0.5993 0.048 Uiso 1 1 calc R . . N21 N 0.5014(3) 0.7536(3) 0.9072(2) 0.0221(8) Uani 1 1 d . . . C21 C 0.4494(4) 0.6543(4) 0.8968(3) 0.0242(10) Uani 1 1 d . . . C22 C 0.4932(4) 0.5432(4) 0.8882(3) 0.0309(11) Uani 1 1 d . . . N22 N 0.5887(4) 0.5340(4) 0.9030(3) 0.0356(11) Uani 1 1 d . . . C23 C 0.6397(4) 0.6329(5) 0.9175(4) 0.0355(12) Uani 1 1 d . . . H23 H 0.7071 0.6278 0.9295 0.043 Uiso 1 1 calc R . . C24 C 0.5973(3) 0.7432(4) 0.9155(3) 0.0261(10) Uani 1 1 d . . . H24 H 0.6357 0.8118 0.9200 0.031 Uiso 1 1 calc R . . C25 C 0.3441(4) 0.6622(5) 0.8952(4) 0.0346(11) Uani 1 1 d . . . H25A H 0.3279 0.7426 0.9103 0.052 Uiso 1 1 calc R . . H25B H 0.3272 0.6080 0.9418 0.052 Uiso 1 1 calc R . . H25C H 0.3087 0.6412 0.8325 0.052 Uiso 1 1 calc R . . C26 C 0.4367(5) 0.4330(5) 0.8633(4) 0.0460(15) Uani 1 1 d . . . H26A H 0.4140 0.4296 0.7951 0.069 Uiso 1 1 calc R . . H26B H 0.3821 0.4329 0.8948 0.069 Uiso 1 1 calc R . . H26C H 0.4769 0.3647 0.8839 0.069 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 Cu1 0.0227(3) 0.0249(3) 0.0181(2) -0.0014(2) -0.0023(2) -0.0005(2) I1 0.02242(15) 0.02441(16) 0.02447(15) 0.00602(12) 0.00443(11) -0.00091(12) Cu2 0.0198(3) 0.0250(3) 0.0232(3) -0.0009(2) -0.0035(2) 0.0021(2) I2 0.02558(16) 0.02644(17) 0.02560(16) 0.00042(12) 0.00596(12) -0.00581(13) N1 0.0156(16) 0.0216(19) 0.0131(15) -0.0015(13) -0.0009(13) -0.0033(14) C1 0.021(2) 0.013(2) 0.0166(19) 0.0002(15) 0.0028(16) -0.0014(16) C2 0.0177(19) 0.016(2) 0.0170(19) -0.0002(15) 0.0013(16) -0.0011(16) N2 0.0179(17) 0.0192(18) 0.0179(16) -0.0011(14) -0.0026(14) -0.0018(14) C3 0.019(2) 0.017(2) 0.020(2) -0.0029(16) 0.0026(17) 0.0012(17) C4 0.021(2) 0.022(2) 0.0173(19) -0.0015(17) 0.0047(17) 0.0023(18) C5 0.025(2) 0.023(2) 0.026(2) -0.0049(18) -0.0075(19) 0.004(2) C6 0.028(2) 0.028(3) 0.030(2) -0.009(2) -0.009(2) 0.002(2) N11 0.0171(17) 0.020(2) 0.0153(16) -0.0009(13) -0.0018(14) -0.0014(14) C11 0.0170(19) 0.017(2) 0.019(2) 0.0012(16) 0.0006(17) -0.0022(16) C12 0.0160(19) 0.018(2) 0.030(2) 0.0025(17) 0.0023(18) -0.0004(16) N12 0.033(2) 0.024(2) 0.027(2) -0.0055(16) 0.0077(18) 0.0038(17) C13 0.037(3) 0.029(3) 0.024(2) -0.0025(19) 0.010(2) 0.004(2) C14 0.023(2) 0.021(2) 0.023(2) 0.0007(17) 0.0062(18) 0.0026(18) C15 0.045(3) 0.026(3) 0.019(2) 0.0023(18) 0.004(2) -0.006(2) C16 0.031(3) 0.025(2) 0.039(3) 0.004(2) 0.006(2) -0.001(2) N21 0.0238(19) 0.022(2) 0.0173(17) 0.0012(14) -0.0029(15) 0.0030(16) C21 0.035(3) 0.020(2) 0.016(2) 0.0011(16) 0.0013(19) 0.0021(19) C22 0.053(3) 0.023(2) 0.017(2) 0.0013(17) 0.010(2) 0.003(2) N22 0.053(3) 0.027(2) 0.029(2) -0.0010(17) 0.012(2) 0.018(2) C23 0.034(3) 0.046(3) 0.028(2) -0.002(2) 0.010(2) 0.015(3) C24 0.026(2) 0.030(3) 0.023(2) -0.0036(18) 0.0056(19) 0.004(2) C25 0.030(3) 0.032(3) 0.039(3) 0.004(2) 0.002(2) -0.007(2) C26 0.083(5) 0.022(3) 0.032(3) 0.000(2) 0.009(3) -0.001(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 Cu1 N1 2.083(4) . ? Cu1 N11 2.143(3) . ? Cu1 I1 2.6307(6) . ? Cu1 I1 2.6716(6) 3_576 ? Cu1 Cu1 2.8055(11) 3_576 ? I1 Cu1 2.6716(6) 3_576 ? Cu2 N2 2.080(4) . ? Cu2 N21 2.131(4) . ? Cu2 I2 2.6336(6) 3_677 ? Cu2 I2 2.6712(6) . ? Cu2 Cu2 2.7843(11) 3_677 ? I2 Cu2 2.6336(6) 3_677 ? N1 C4 1.334(6) . ? N1 C1 1.340(5) . ? C1 C2 1.413(6) . ? C1 C5 1.483(6) . ? C2 N2 1.343(6) . ? C2 C6 1.487(6) . ? N2 C3 1.342(6) . ? C3 C4 1.374(6) . ? N11 C11 1.333(5) . ? N11 C14 1.356(5) . ? C11 C12 1.413(6) . ? C11 C15 1.503(6) . ? C12 N12 1.342(6) . ? C12 C16 1.498(6) . ? N12 C13 1.340(6) . ? C13 C14 1.369(7) . ? N21 C21 1.333(6) . ? N21 C24 1.349(6) . ? C21 C22 1.414(7) . ? C21 C25 1.494(7) . ? C22 N22 1.335(7) . ? C22 C26 1.483(8) . ? N22 C23 1.323(8) . ? C23 C24 1.380(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 N1 Cu1 N11 104.02(14) . . ? N1 Cu1 I1 115.54(9) . . ? N11 Cu1 I1 106.50(9) . . ? N1 Cu1 I1 105.94(10) . 3_576 ? N11 Cu1 I1 107.85(9) . 3_576 ? I1 Cu1 I1 116.12(2) . 3_576 ? N1 Cu1 Cu1 131.75(11) . 3_576 ? N11 Cu1 Cu1 123.93(10) . 3_576 ? I1 Cu1 Cu1 58.77(2) . 3_576 ? I1 Cu1 Cu1 57.35(2) 3_576 3_576 ? Cu1 I1 Cu1 63.88(2) . 3_576 ? N2 Cu2 N21 103.21(14) . . ? N2 Cu2 I2 118.51(10) . 3_677 ? N21 Cu2 I2 102.72(9) . 3_677 ? N2 Cu2 I2 106.10(10) . . ? N21 Cu2 I2 108.34(10) . . ? I2 Cu2 I2 116.69(2) 3_677 . ? N2 Cu2 Cu2 135.84(11) . 3_677 ? N21 Cu2 Cu2 120.67(11) . 3_677 ? I2 Cu2 Cu2 59.00(2) 3_677 3_677 ? I2 Cu2 Cu2 57.69(2) . 3_677 ? Cu2 I2 Cu2 63.31(2) 3_677 . ? C4 N1 C1 117.4(4) . . ? C4 N1 Cu1 116.1(3) . . ? C1 N1 Cu1 126.4(3) . . ? N1 C1 C2 120.8(4) . . ? N1 C1 C5 118.3(4) . . ? C2 C1 C5 121.0(4) . . ? N2 C2 C1 120.4(4) . . ? N2 C2 C6 117.3(4) . . ? C1 C2 C6 122.3(4) . . ? C3 N2 C2 117.8(4) . . ? C3 N2 Cu2 116.5(3) . . ? C2 N2 Cu2 125.5(3) . . ? N2 C3 C4 121.0(4) . . ? N1 C4 C3 122.3(4) . . ? C11 N11 C14 116.8(4) . . ? C11 N11 Cu1 127.5(3) . . ? C14 N11 Cu1 115.6(3) . . ? N11 C11 C12 121.4(4) . . ? N11 C11 C15 118.7(4) . . ? C12 C11 C15 119.9(4) . . ? N12 C12 C11 121.0(4) . . ? N12 C12 C16 116.5(4) . . ? C11 C12 C16 122.6(4) . . ? C13 N12 C12 116.4(4) . . ? N12 C13 C14 122.9(4) . . ? N11 C14 C13 121.2(4) . . ? C21 N21 C24 117.7(4) . . ? C21 N21 Cu2 128.1(3) . . ? C24 N21 Cu2 114.0(3) . . ? N21 C21 C22 120.7(5) . . ? N21 C21 C25 118.8(4) . . ? C22 C21 C25 120.5(5) . . ? N22 C22 C21 120.3(5) . . ? N22 C22 C26 117.3(5) . . ? C21 C22 C26 122.4(5) . . ? C23 N22 C22 117.9(4) . . ? N22 C23 C24 122.2(5) . . ? N21 C24 C23 120.6(5) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.251 _refine_diff_density_min -1.097 _refine_diff_density_rms 0.179 data_Compound_2 _database_code_depnum_ccdc_archive 'CCDC 636027' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H8 Cu I N2' _chemical_formula_weight 298.58 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 P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.8505(5) _cell_length_b 12.8482(7) _cell_length_c 13.5837(8) _cell_angle_alpha 90.00 _cell_angle_beta 103.152(6) _cell_angle_gamma 90.00 _cell_volume 1674.08(16) _cell_formula_units_Z 8 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.369 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 6.223 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10181 _diffrn_reflns_av_R_equivalents 0.0530 _diffrn_reflns_av_sigmaI/netI 0.0552 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 28.04 _reflns_number_total 3972 _reflns_number_gt 2868 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0426P)^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 SHELXL _refine_ls_extinction_coef 0.0020(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3972 _refine_ls_number_parameters 186 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0645 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0821 _refine_ls_wR_factor_gt 0.0738 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.976 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.78423(7) 0.19359(6) 0.58403(6) 0.02686(18) Uani 1 1 d . . . Cu2 Cu 0.88771(7) -0.01641(6) 0.55221(6) 0.02864(18) Uani 1 1 d . . . I1 I 0.88785(4) 0.13798(3) 0.42063(3) 0.02333(11) Uani 1 1 d . . . I2 I 0.89744(4) 0.06902(3) 0.73465(3) 0.02650(11) Uani 1 1 d . . . N1 N 0.8649(5) 0.3404(3) 0.6133(4) 0.0225(10) Uani 1 1 d . . . C1 C 0.8104(6) 0.4265(4) 0.5619(5) 0.0262(12) Uani 1 1 d . . . C2 C 0.8786(6) 0.5228(4) 0.5819(5) 0.0263(12) Uani 1 1 d . . . N2 N 1.0013(6) 0.5315(4) 0.6474(5) 0.0337(12) Uani 1 1 d . . . C3 C 1.0539(7) 0.4440(5) 0.6970(5) 0.0341(14) Uani 1 1 d . . . H3 H 1.1403 0.4475 0.7438 0.041 Uiso 1 1 calc R . . C4 C 0.9863(6) 0.3514(5) 0.6814(5) 0.0258(12) Uani 1 1 d . . . H4 H 1.0256 0.2932 0.7194 0.031 Uiso 1 1 calc R . . C5 C 0.6774(8) 0.4164(6) 0.4844(7) 0.048(2) Uani 1 1 d . . . H5A H 0.6946 0.4282 0.4178 0.072 Uiso 1 1 calc R . . H5B H 0.6110 0.4674 0.4975 0.072 Uiso 1 1 calc R . . H5C H 0.6398 0.3470 0.4874 0.072 Uiso 1 1 calc R . . C6 C 0.8172(8) 0.6208(5) 0.5307(6) 0.0432(17) Uani 1 1 d . . . H6A H 0.8841 0.6770 0.5479 0.065 Uiso 1 1 calc R . . H6B H 0.7332 0.6383 0.5530 0.065 Uiso 1 1 calc R . . H6C H 0.7944 0.6105 0.4581 0.065 Uiso 1 1 calc R . . N11 N 0.5719(5) 0.1699(4) 0.5406(4) 0.0208(9) Uani 1 1 d . . . C11 C 0.4856(5) 0.1853(4) 0.6034(4) 0.0191(11) Uani 1 1 d . . . C12 C 0.3478(5) 0.1473(4) 0.5768(5) 0.0214(11) Uani 1 1 d . . . N12 N 0.2980(4) 0.0995(4) 0.4876(4) 0.0196(9) Uani 1 1 d . . . C13 C 0.3825(6) 0.0928(5) 0.4237(5) 0.0240(11) Uani 1 1 d . . . H13 H 0.3482 0.0646 0.3590 0.029 Uiso 1 1 calc R . . C14 C 0.5185(6) 0.1262(5) 0.4503(4) 0.0237(11) Uani 1 1 d . . . H14 H 0.5757 0.1183 0.4041 0.028 Uiso 1 1 calc R . . C15 C 0.5411(6) 0.2429(5) 0.7010(5) 0.0328(14) Uani 1 1 d . . . H15A H 0.4825 0.3028 0.7046 0.049 Uiso 1 1 calc R . . H15B H 0.6356 0.2659 0.7036 0.049 Uiso 1 1 calc R . . H15C H 0.5408 0.1970 0.7577 0.049 Uiso 1 1 calc R . . C16 C 0.2515(6) 0.1604(5) 0.6481(5) 0.0279(13) Uani 1 1 d . . . H16A H 0.2832 0.1167 0.7071 0.042 Uiso 1 1 calc R . . H16B H 0.1576 0.1402 0.6140 0.042 Uiso 1 1 calc R . . H16C H 0.2517 0.2326 0.6690 0.042 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 Cu1 0.0210(3) 0.0298(4) 0.0282(4) -0.0022(3) 0.0024(3) -0.0063(3) Cu2 0.0200(3) 0.0353(4) 0.0310(4) -0.0013(3) 0.0064(3) -0.0052(3) I1 0.01919(17) 0.02914(19) 0.0233(2) 0.00264(16) 0.00825(13) -0.00004(14) I2 0.02729(19) 0.0299(2) 0.0212(2) -0.00051(16) 0.00315(14) -0.00167(15) N1 0.020(2) 0.021(2) 0.027(3) -0.004(2) 0.007(2) -0.0021(18) C1 0.025(3) 0.023(3) 0.029(3) -0.003(3) 0.004(2) -0.006(2) C2 0.032(3) 0.028(3) 0.020(3) 0.004(2) 0.008(2) -0.002(2) N2 0.033(3) 0.028(3) 0.037(3) -0.001(2) 0.002(2) -0.010(2) C3 0.032(3) 0.034(3) 0.032(4) -0.006(3) -0.002(3) -0.005(3) C4 0.020(2) 0.028(3) 0.028(3) -0.002(2) 0.004(2) 0.001(2) C5 0.040(4) 0.042(4) 0.048(5) 0.011(4) -0.019(3) -0.010(3) C6 0.056(4) 0.029(3) 0.039(4) 0.015(3) 0.000(3) 0.002(3) N11 0.019(2) 0.024(2) 0.020(3) 0.0011(19) 0.0051(18) -0.0016(18) C11 0.019(2) 0.018(2) 0.023(3) 0.001(2) 0.009(2) 0.000(2) C12 0.019(2) 0.023(3) 0.024(3) 0.003(2) 0.008(2) 0.003(2) N12 0.014(2) 0.024(2) 0.021(2) -0.0022(19) 0.0051(18) -0.0038(17) C13 0.019(2) 0.035(3) 0.019(3) -0.001(2) 0.004(2) -0.008(2) C14 0.018(2) 0.035(3) 0.018(3) -0.004(2) 0.004(2) -0.001(2) C15 0.028(3) 0.040(3) 0.030(3) -0.013(3) 0.005(3) -0.004(3) C16 0.027(3) 0.034(3) 0.027(3) -0.001(3) 0.015(3) 0.002(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 N1 2.050(5) . ? Cu1 N11 2.063(5) . ? Cu1 I2 2.6369(9) . ? Cu1 I1 2.7403(9) . ? Cu1 Cu2 2.9506(11) . ? Cu2 N12 2.080(4) 3_656 ? Cu2 I1 2.6632(8) 3_756 ? Cu2 I1 2.6703(9) . ? Cu2 I2 2.6921(9) . ? Cu2 Cu2 2.9175(14) 3_756 ? I1 Cu2 2.6632(8) 3_756 ? N1 C4 1.343(8) . ? N1 C1 1.353(8) . ? C1 C2 1.405(8) . ? C1 C5 1.488(9) . ? C2 N2 1.332(8) . ? C2 C6 1.498(9) . ? N2 C3 1.352(9) . ? C3 C4 1.357(8) . ? N11 C14 1.343(8) . ? N11 C11 1.349(7) . ? C11 C12 1.410(7) . ? C11 C15 1.508(9) . ? C12 N12 1.348(8) . ? C12 C16 1.512(7) . ? N12 C13 1.335(7) . ? N12 Cu2 2.080(4) 3_656 ? C13 C14 1.374(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 N1 Cu1 N11 120.95(18) . . ? N1 Cu1 I2 109.34(15) . . ? N11 Cu1 I2 110.76(14) . . ? N1 Cu1 I1 101.40(14) . . ? N11 Cu1 I1 105.70(14) . . ? I2 Cu1 I1 107.49(3) . . ? N1 Cu1 Cu2 137.58(13) . . ? N11 Cu1 Cu2 100.65(13) . . ? I2 Cu1 Cu2 57.28(2) . . ? I1 Cu1 Cu2 55.82(2) . . ? N12 Cu2 I1 112.85(13) 3_656 3_756 ? N12 Cu2 I1 109.97(14) 3_656 . ? I1 Cu2 I1 113.68(3) 3_756 . ? N12 Cu2 I2 107.05(14) 3_656 . ? I1 Cu2 I2 104.90(3) 3_756 . ? I1 Cu2 I2 107.94(3) . . ? N12 Cu2 Cu2 131.85(14) 3_656 3_756 ? I1 Cu2 Cu2 56.95(3) 3_756 3_756 ? I1 Cu2 Cu2 56.72(3) . 3_756 ? I2 Cu2 Cu2 121.10(4) . 3_756 ? N12 Cu2 Cu1 101.21(13) 3_656 . ? I1 Cu2 Cu1 145.05(3) 3_756 . ? I1 Cu2 Cu1 58.10(2) . . ? I2 Cu2 Cu1 55.49(2) . . ? Cu2 Cu2 Cu1 105.34(4) 3_756 . ? Cu2 I1 Cu2 66.32(3) 3_756 . ? Cu2 I1 Cu1 119.42(3) 3_756 . ? Cu2 I1 Cu1 66.08(2) . . ? Cu1 I2 Cu2 67.23(3) . . ? C4 N1 C1 117.1(5) . . ? C4 N1 Cu1 118.4(4) . . ? C1 N1 Cu1 124.2(4) . . ? N1 C1 C2 120.3(5) . . ? N1 C1 C5 118.4(5) . . ? C2 C1 C5 121.3(6) . . ? N2 C2 C1 121.6(5) . . ? N2 C2 C6 116.7(5) . . ? C1 C2 C6 121.7(6) . . ? C2 N2 C3 116.7(5) . . ? N2 C3 C4 122.2(6) . . ? N1 C4 C3 121.9(6) . . ? C14 N11 C11 117.8(5) . . ? C14 N11 Cu1 118.9(4) . . ? C11 N11 Cu1 122.8(4) . . ? N11 C11 C12 119.7(5) . . ? N11 C11 C15 118.3(5) . . ? C12 C11 C15 122.0(5) . . ? N12 C12 C11 121.3(5) . . ? N12 C12 C16 118.3(5) . . ? C11 C12 C16 120.4(5) . . ? C13 N12 C12 117.4(5) . . ? C13 N12 Cu2 116.1(4) . 3_656 ? C12 N12 Cu2 125.9(4) . 3_656 ? N12 C13 C14 121.6(6) . . ? N11 C14 C13 121.8(5) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 28.04 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.766 _refine_diff_density_min -0.965 _refine_diff_density_rms 0.173 data_Compound_3 _database_code_depnum_ccdc_archive 'CCDC 636028' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H8 Cu2 I2 N2' _chemical_formula_weight 489.02 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 P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 4.3210(9) _cell_length_b 17.974(3) _cell_length_c 13.1672(16) _cell_angle_alpha 90.00 _cell_angle_beta 92.63(3) _cell_angle_gamma 90.00 _cell_volume 1021.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.180 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 10.154 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2859 _diffrn_reflns_av_R_equivalents 0.0371 _diffrn_reflns_av_sigmaI/netI 0.0509 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 2 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 27.01 _reflns_number_total 2238 _reflns_number_gt 1592 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0421P)^2^+0.8077P] 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 2238 _refine_ls_number_parameters 111 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0700 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0800 _refine_ls_wR_factor_gt 0.0723 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _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 0.1258(2) 0.44290(5) 0.70781(8) 0.0367(2) Uani 1 1 d . . . Cu2 Cu 0.4908(2) 0.32473(5) 0.76654(7) 0.0350(2) Uani 1 1 d . . . I1 I 0.01450(10) 0.36366(3) 0.87544(4) 0.02852(13) Uani 1 1 d . . . I2 I 0.59272(10) 0.40279(3) 0.59915(4) 0.02803(13) Uani 1 1 d . . . N1 N 0.1095(14) 0.5566(3) 0.7235(4) 0.0283(13) Uani 1 1 d . . . C1 C 0.2606(15) 0.5944(4) 0.7983(5) 0.0265(14) Uani 1 1 d . . . C2 C 0.2280(16) 0.6731(4) 0.8048(5) 0.0262(14) Uani 1 1 d . . . N2 N 0.0462(14) 0.7106(3) 0.7370(4) 0.0272(12) Uani 1 1 d . . . C3 C -0.0964(19) 0.6707(4) 0.6622(6) 0.0357(17) Uani 1 1 d . . . H3 H -0.2215 0.6954 0.6137 0.043 Uiso 1 1 calc R . . C4 C -0.0638(17) 0.5951(4) 0.6550(6) 0.0336(16) Uani 1 1 d . . . H4 H -0.1645 0.5699 0.6013 0.040 Uiso 1 1 calc R . . C5 C 0.4553(17) 0.5523(4) 0.8755(6) 0.0357(17) Uani 1 1 d . . . H5B H 0.3491 0.5493 0.9379 0.054 Uiso 1 1 calc R . . H5C H 0.6494 0.5775 0.8876 0.054 Uiso 1 1 calc R . . H5A H 0.4923 0.5030 0.8507 0.054 Uiso 1 1 calc R . . C6 C 0.3889(17) 0.7167(4) 0.8875(6) 0.0326(16) Uani 1 1 d . . . H6C H 0.5530 0.7453 0.8600 0.049 Uiso 1 1 calc R . . H6C' H 0.4739 0.6833 0.9385 0.049 Uiso 1 1 calc R . . H6A H 0.2438 0.7496 0.9175 0.049 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 Cu1 0.0410(5) 0.0216(4) 0.0477(6) -0.0019(4) 0.0035(4) 0.0030(4) Cu2 0.0389(5) 0.0210(4) 0.0450(6) -0.0001(4) 0.0025(4) -0.0002(4) I1 0.0243(2) 0.0300(2) 0.0314(2) 0.00064(19) 0.00178(17) -0.00116(19) I2 0.0263(2) 0.0265(2) 0.0312(2) 0.0021(2) 0.00071(18) -0.00050(19) N1 0.033(3) 0.020(3) 0.032(3) -0.001(2) 0.006(3) 0.005(3) C1 0.026(3) 0.020(3) 0.034(4) -0.005(3) 0.006(3) 0.002(3) C2 0.031(3) 0.019(3) 0.029(4) 0.002(3) 0.004(3) -0.006(3) N2 0.035(3) 0.021(3) 0.026(3) 0.002(2) 0.006(2) 0.000(2) C3 0.046(4) 0.018(3) 0.041(4) 0.005(3) -0.011(4) 0.001(3) C4 0.034(4) 0.031(4) 0.036(4) -0.002(3) 0.001(3) -0.003(3) C5 0.031(4) 0.024(3) 0.051(5) 0.001(3) -0.007(4) 0.005(3) C6 0.036(4) 0.020(3) 0.041(4) 0.002(3) -0.009(3) -0.002(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 Cu1 N1 2.056(6) . ? Cu1 I2 2.6271(13) . ? Cu1 I1 2.6887(12) . ? Cu1 Cu2 2.7358(14) . ? Cu1 I2 2.7515(13) 1_455 ? Cu2 N2 2.058(6) 2_546 ? Cu2 I1 2.6556(13) . ? Cu2 I2 2.6663(11) . ? Cu2 I1 2.7146(13) 1_655 ? I1 Cu2 2.7146(13) 1_455 ? I2 Cu1 2.7515(14) 1_655 ? N1 C4 1.337(9) . ? N1 C1 1.342(9) . ? C1 C2 1.424(9) . ? C1 C5 1.495(10) . ? C2 N2 1.342(9) . ? C2 C6 1.489(9) . ? N2 C3 1.344(9) . ? N2 Cu2 2.058(5) 2_556 ? C3 C4 1.371(10) . ? 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 I2 110.99(17) . . ? N1 Cu1 I1 115.86(17) . . ? I2 Cu1 I1 118.20(4) . . ? N1 Cu1 Cu2 139.95(18) . . ? I2 Cu1 Cu2 59.59(3) . . ? I1 Cu1 Cu2 58.61(3) . . ? N1 Cu1 I2 106.31(17) . 1_455 ? I2 Cu1 I2 106.88(4) . 1_455 ? I1 Cu1 I2 96.38(4) . 1_455 ? Cu2 Cu1 I2 113.68(4) . 1_455 ? N2 Cu2 I1 102.34(16) 2_546 . ? N2 Cu2 I2 121.42(16) 2_546 . ? I1 Cu2 I2 117.98(4) . . ? N2 Cu2 I1 109.33(17) 2_546 1_655 ? I1 Cu2 I1 107.14(4) . 1_655 ? I2 Cu2 I1 97.80(4) . 1_655 ? N2 Cu2 Cu1 136.41(18) 2_546 . ? I1 Cu2 Cu1 59.81(3) . . ? I2 Cu2 Cu1 58.18(3) . . ? I1 Cu2 Cu1 113.89(4) 1_655 . ? Cu2 I1 Cu1 61.58(3) . . ? Cu2 I1 Cu2 107.14(4) . 1_455 ? Cu1 I1 Cu2 83.06(4) . 1_455 ? Cu1 I2 Cu2 62.23(4) . . ? Cu1 I2 Cu1 106.88(4) . 1_655 ? Cu2 I2 Cu1 82.77(4) . 1_655 ? C4 N1 C1 118.2(6) . . ? C4 N1 Cu1 117.8(5) . . ? C1 N1 Cu1 124.0(5) . . ? N1 C1 C2 120.0(6) . . ? N1 C1 C5 118.8(6) . . ? C2 C1 C5 121.1(6) . . ? N2 C2 C1 121.0(6) . . ? N2 C2 C6 117.5(6) . . ? C1 C2 C6 121.5(6) . . ? C2 N2 C3 117.0(6) . . ? C2 N2 Cu2 123.9(5) . 2_556 ? C3 N2 Cu2 118.8(5) . 2_556 ? N2 C3 C4 122.3(7) . . ? N1 C4 C3 121.4(7) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.171 _refine_diff_density_min -0.857 _refine_diff_density_rms 0.196