Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_pnma _database_code_CSD 174413 _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'zur Loye, Hans-Conrad' 'Ciurtin, Delia M.' 'Smith, Mark D.' _publ_contact_author_name 'Dr Hans-Conrad zur Loye' _publ_contact_author_address ; Chemistry and Biochemistry University of South Carolina 631 Sumter Street, GSRC Columbia SC 29208 UNITED STATES OF AMERICA ; _publ_contact_author_email 'ZURLOYE@SC.EDU' _publ_section_title ; [Cu(pyrazine-2-carboxylate)2]2Cd4I8: Unprecedented 1-D serpentine inorganic chains and regular 2-D metal-organic square grids in a 3-D framework. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H12 Cd4 Cu2 I8 N8 O8' _chemical_formula_weight 2084.26 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' 'O' 'O' 0.0106 0.0060 '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' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnma 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 14.4875(14) _cell_length_b 19.943(2) _cell_length_c 14.4911(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4186.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5024 _cell_measurement_theta_min 2.235 _cell_measurement_theta_max 27.544 _exptl_crystal_description fragment _exptl_crystal_colour green _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.307 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3704 _exptl_absorpt_coefficient_mu 8.940 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2628 _exptl_absorpt_correction_T_max 0.4174 _exptl_absorpt_process_details '(SADABS, Bruker, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 32472 _diffrn_reflns_av_R_equivalents 0.0649 _diffrn_reflns_av_sigmaI/netI 0.0403 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.02 _diffrn_reflns_theta_max 28.33 _reflns_number_total 5547 _reflns_number_gt 4207 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART NT V5.624 (Bruker, 2000)' _computing_cell_refinement 'SAINT+ NT V6.02a (Bruker, 1998)' _computing_data_reduction 'SAINT+ NT V6.02a' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V5.1 (Sheldrick, 1997)' _computing_publication_material 'SHELXTL V5.1' _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^)+(0.1192P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5547 _refine_ls_number_parameters 242 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0825 _refine_ls_R_factor_gt 0.0664 _refine_ls_wR_factor_ref 0.1850 _refine_ls_wR_factor_gt 0.1753 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 0.5000 0.5000 0.5000 0.0255(5) Uani 1 2 d S . . C1 C 0.6781(7) 0.5501(4) 0.5030(7) 0.016(2) Uani 1 1 d . . . C2 C 0.7735(9) 0.5549(6) 0.5015(7) 0.026(3) Uani 1 1 d . . . H2 H 0.8017 0.5968 0.5017 0.031 Uiso 1 1 calc R . . C3 C 0.7857(8) 0.4415(7) 0.4988(9) 0.032(3) Uani 1 1 d . . . H3 H 0.8212 0.4027 0.4975 0.039 Uiso 1 1 calc R . . C4 C 0.6895(9) 0.4405(6) 0.4996(9) 0.032(3) Uani 1 1 d . . . H4 H 0.6622 0.3983 0.4991 0.038 Uiso 1 1 calc R . . C5 C 0.6141(8) 0.6097(5) 0.5063(8) 0.025(2) Uani 1 1 d . . . N1 N 0.6333(8) 0.4912(4) 0.5009(7) 0.024(2) Uani 1 1 d . . . N2 N 0.8223(8) 0.5022(5) 0.5000(8) 0.030(3) Uani 1 1 d . . . O1 O 0.5285(5) 0.5971(4) 0.5054(6) 0.0266(17) Uani 1 1 d . . . O2 O 0.6478(6) 0.6669(4) 0.5116(7) 0.037(2) Uani 1 1 d . . . Cu2 Cu 0.5000 0.5000 1.0000 0.0242(5) Uani 1 2 d S . . C6 C 0.5005(8) 0.4459(6) 0.8211(9) 0.028(3) Uani 1 1 d . . . C7 C 0.5004(8) 0.4427(6) 0.7271(8) 0.027(3) Uani 1 1 d . . . H7 H 0.5021 0.4006 0.6994 0.032 Uiso 1 1 calc R . . C8 C 0.4935(9) 0.5597(6) 0.7175(9) 0.032(3) Uani 1 1 d . . . H8 H 0.4888 0.5989 0.6830 0.039 Uiso 1 1 calc R . . C9 C 0.4956(8) 0.5653(5) 0.8097(9) 0.027(3) Uani 1 1 d . . . H9 H 0.4948 0.6074 0.8372 0.033 Uiso 1 1 calc R . . C10 C 0.4991(8) 0.3907(5) 0.8850(8) 0.024(2) Uani 1 1 d . . . N3 N 0.4989(6) 0.5097(5) 0.8621(7) 0.0200(19) Uani 1 1 d . . . N4 N 0.4981(7) 0.4989(4) 0.6701(9) 0.029(3) Uani 1 1 d . . . O3 O 0.4972(5) 0.4034(4) 0.9704(6) 0.0275(18) Uani 1 1 d . . . O4 O 0.4973(6) 0.3336(4) 0.8529(7) 0.036(2) Uani 1 1 d . . . Cd1 Cd 0.45471(10) 0.2500 1.47918(11) 0.0346(3) Uani 1 2 d S . . Cd2 Cd 0.69644(16) 0.2500 1.23904(17) 0.0695(6) Uani 1 2 d S . . Cd3 Cd 0.48612(10) 0.2500 0.95301(10) 0.0359(3) Uani 1 2 d S . . Cd4 Cd 0.23410(15) 0.2500 0.81054(15) 0.0670(5) Uani 1 2 d S . . I1 I 0.50551(11) 0.2500 1.29632(12) 0.0547(4) Uani 1 2 d S . . I2 I 0.75906(9) 0.37666(5) 1.25789(8) 0.0548(3) Uani 1 1 d . . . I3 I 0.64700(11) 0.2500 1.04250(11) 0.0518(4) Uani 1 2 d S . . I4 I 0.30262(10) 0.2500 1.00133(9) 0.0401(3) Uani 1 2 d S . . I5 I 0.25909(10) 0.37435(7) 0.74313(9) 0.0760(4) Uani 1 1 d . . . I6 I 0.03881(11) 0.2500 0.85584(11) 0.0505(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 Cu1 0.0135(12) 0.0135(11) 0.0496(17) 0.0006(8) 0.0002(9) 0.0001(6) C1 0.016(5) 0.002(4) 0.030(6) 0.003(3) -0.004(4) 0.000(3) C2 0.024(6) 0.020(6) 0.032(7) 0.000(4) 0.000(5) -0.003(5) C3 0.014(6) 0.025(6) 0.057(9) -0.006(5) -0.005(5) 0.001(5) C4 0.023(7) 0.024(6) 0.048(9) 0.000(5) 0.003(5) -0.006(5) C5 0.028(6) 0.016(5) 0.030(6) -0.005(4) -0.003(4) 0.006(4) N1 0.024(5) 0.008(4) 0.038(6) 0.000(3) -0.003(4) -0.007(3) N2 0.022(6) 0.034(6) 0.033(7) -0.001(4) -0.007(4) 0.003(4) O1 0.018(4) 0.015(4) 0.047(5) 0.001(3) 0.001(3) 0.001(3) O2 0.026(5) 0.016(4) 0.069(6) 0.000(4) -0.001(4) 0.000(3) Cu2 0.0346(14) 0.0126(11) 0.0254(14) 0.0012(7) 0.0005(8) 0.0008(7) C6 0.028(7) 0.027(6) 0.030(7) 0.011(5) 0.003(5) -0.001(4) C7 0.040(8) 0.009(5) 0.032(7) -0.005(4) 0.000(5) 0.001(4) C8 0.054(9) 0.011(5) 0.031(7) 0.011(5) 0.002(5) 0.004(5) C9 0.048(8) 0.002(4) 0.033(6) -0.001(4) 0.000(5) 0.005(4) C10 0.025(6) 0.013(5) 0.033(6) 0.001(4) 0.003(4) 0.002(4) N3 0.015(5) 0.026(4) 0.019(5) 0.003(4) 0.003(3) 0.002(3) N4 0.045(8) 0.012(5) 0.029(7) 0.000(3) -0.003(4) 0.001(4) O3 0.030(5) 0.016(4) 0.037(5) 0.003(3) 0.005(3) 0.005(3) O4 0.049(6) 0.016(4) 0.042(5) -0.001(4) 0.005(4) -0.005(3) Cd1 0.0323(7) 0.0180(5) 0.0536(8) 0.000 0.0009(6) 0.000 Cd2 0.0741(14) 0.0437(10) 0.0906(15) 0.000 0.0133(11) 0.000 Cd3 0.0525(9) 0.0157(5) 0.0395(8) 0.000 -0.0005(6) 0.000 Cd4 0.0711(13) 0.0626(11) 0.0672(12) 0.000 0.0029(10) 0.000 I1 0.0679(11) 0.0294(6) 0.0667(10) 0.000 0.0273(8) 0.000 I2 0.0623(8) 0.0466(6) 0.0555(7) -0.0033(4) -0.0043(5) -0.0108(5) I3 0.0459(9) 0.0425(7) 0.0669(10) 0.000 -0.0145(7) 0.000 I4 0.0481(8) 0.0231(5) 0.0491(9) 0.000 0.0072(6) 0.000 I5 0.0584(9) 0.0960(10) 0.0736(9) 0.0374(7) -0.0029(6) -0.0168(7) I6 0.0559(9) 0.0411(7) 0.0545(9) 0.000 0.0133(7) 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 Cu1 N1 1.939(11) . ? Cu1 N1 1.939(11) 5_666 ? Cu1 O1 1.982(7) 5_666 ? Cu1 O1 1.982(7) . ? Cu1 N4 2.466(12) 5_666 ? Cu1 N4 2.466(12) . ? C1 N1 1.343(12) . ? C1 C2 1.386(15) . ? C1 C5 1.507(13) . ? C2 N2 1.268(16) . ? C3 N2 1.322(16) . ? C3 C4 1.394(17) . ? C4 N1 1.299(16) . ? C5 O2 1.244(14) . ? C5 O1 1.265(14) . ? O2 Cd1 2.230(8) 5_667 ? Cu2 O3 1.973(8) 5_667 ? Cu2 O3 1.973(8) . ? Cu2 N3 2.009(10) . ? Cu2 N3 2.009(10) 5_667 ? Cu2 N2 2.575(12) 6_557 ? Cu2 N2 2.575(12) 2_665 ? C6 C7 1.364(17) . ? C6 N3 1.405(16) . ? C6 C10 1.438(15) . ? C7 N4 1.393(15) . ? C8 C9 1.340(18) . ? C8 N4 1.395(15) . ? C9 N3 1.344(14) . ? C10 O4 1.230(13) . ? C10 O3 1.265(14) . ? O4 Cd3 2.216(9) . ? Cd1 O2 2.230(8) 3_647 ? Cd1 O2 2.230(8) 5_667 ? Cd1 I6 2.683(2) 6_658 ? Cd1 I1 2.750(2) . ? Cd2 I2 2.6978(13) . ? Cd2 I2 2.6978(13) 7_565 ? Cd2 I1 2.888(3) . ? Cd2 I3 2.937(3) . ? Cd3 O4 2.216(9) 7_565 ? Cd3 I3 2.667(2) . ? Cd3 I4 2.749(2) . ? Cd4 I5 2.6899(15) . ? Cd4 I5 2.6899(15) 7_565 ? Cd4 I6 2.904(3) . ? Cd4 I4 2.938(3) . ? I6 Cd1 2.683(2) 6_558 ? 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 N1 180.000(1) . 5_666 ? N1 Cu1 O1 96.8(3) . 5_666 ? N1 Cu1 O1 83.2(3) 5_666 5_666 ? N1 Cu1 O1 83.2(3) . . ? N1 Cu1 O1 96.8(3) 5_666 . ? O1 Cu1 O1 180.000(1) 5_666 . ? N1 Cu1 N4 89.8(4) . 5_666 ? N1 Cu1 N4 90.2(4) 5_666 5_666 ? O1 Cu1 N4 88.3(3) 5_666 5_666 ? O1 Cu1 N4 91.7(3) . 5_666 ? N1 Cu1 N4 90.2(4) . . ? N1 Cu1 N4 89.8(4) 5_666 . ? O1 Cu1 N4 91.7(3) 5_666 . ? O1 Cu1 N4 88.3(3) . . ? N4 Cu1 N4 180.000(2) 5_666 . ? N1 C1 C2 122.8(10) . . ? N1 C1 C5 113.2(10) . . ? C2 C1 C5 124.0(9) . . ? N2 C2 C1 120.0(11) . . ? N2 C3 C4 114.5(11) . . ? N1 C4 C3 128.0(11) . . ? O2 C5 O1 124.6(10) . . ? O2 C5 C1 118.9(10) . . ? O1 C5 C1 116.5(9) . . ? C4 N1 C1 112.2(11) . . ? C4 N1 Cu1 134.1(8) . . ? C1 N1 Cu1 113.7(8) . . ? C2 N2 C3 122.4(13) . . ? C5 O1 Cu1 113.5(7) . . ? C5 O2 Cd1 115.1(7) . 5_667 ? O3 Cu2 O3 180.00(10) 5_667 . ? O3 Cu2 N3 97.0(4) 5_667 . ? O3 Cu2 N3 83.0(4) . . ? O3 Cu2 N3 83.0(4) 5_667 5_667 ? O3 Cu2 N3 97.0(4) . 5_667 ? N3 Cu2 N3 180.000(2) . 5_667 ? O3 Cu2 N2 90.2(3) 5_667 6_557 ? O3 Cu2 N2 89.8(3) . 6_557 ? N3 Cu2 N2 89.4(3) . 6_557 ? N3 Cu2 N2 90.6(3) 5_667 6_557 ? O3 Cu2 N2 89.8(3) 5_667 2_665 ? O3 Cu2 N2 90.2(3) . 2_665 ? N3 Cu2 N2 90.6(3) . 2_665 ? N3 Cu2 N2 89.4(3) 5_667 2_665 ? N2 Cu2 N2 180.000(1) 6_557 2_665 ? C7 C6 N3 117.7(10) . . ? C7 C6 C10 127.3(11) . . ? N3 C6 C10 114.9(10) . . ? C6 C7 N4 123.6(11) . . ? C9 C8 N4 124.2(10) . . ? C8 C9 N3 119.7(10) . . ? O4 C10 O3 123.7(10) . . ? O4 C10 C6 117.8(11) . . ? O3 C10 C6 118.5(10) . . ? C9 N3 C6 120.6(10) . . ? C9 N3 Cu2 130.0(8) . . ? C6 N3 Cu2 109.4(7) . . ? C7 N4 C8 114.2(11) . . ? C7 N4 Cu1 126.8(7) . . ? C8 N4 Cu1 119.0(8) . . ? C10 O3 Cu2 114.1(7) . . ? C10 O4 Cd3 116.8(8) . . ? O2 Cd1 O2 96.0(4) 3_647 5_667 ? O2 Cd1 I6 104.4(3) 3_647 6_658 ? O2 Cd1 I6 104.4(3) 5_667 6_658 ? O2 Cd1 I1 103.6(3) 3_647 . ? O2 Cd1 I1 103.6(3) 5_667 . ? I6 Cd1 I1 137.47(8) 6_658 . ? I2 Cd2 I2 138.88(11) . 7_565 ? I2 Cd2 I1 107.04(6) . . ? I2 Cd2 I1 107.04(6) 7_565 . ? I2 Cd2 I3 100.38(6) . . ? I2 Cd2 I3 100.38(6) 7_565 . ? I1 Cd2 I3 92.59(8) . . ? O4 Cd3 O4 97.6(5) 7_565 . ? O4 Cd3 I3 104.7(2) 7_565 . ? O4 Cd3 I3 104.7(2) . . ? O4 Cd3 I4 103.7(2) 7_565 . ? O4 Cd3 I4 103.7(2) . . ? I3 Cd3 I4 136.15(7) . . ? I5 Cd4 I5 134.42(11) . 7_565 ? I5 Cd4 I6 102.31(6) . . ? I5 Cd4 I6 102.31(6) 7_565 . ? I5 Cd4 I4 107.24(6) . . ? I5 Cd4 I4 107.24(6) 7_565 . ? I6 Cd4 I4 96.69(7) . . ? Cd1 I1 Cd2 122.22(9) . . ? Cd3 I3 Cd2 133.21(8) . . ? Cd3 I4 Cd4 94.99(6) . . ? Cd1 I6 Cd4 130.07(9) 6_558 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 -1.5(18) . . . . ? C5 C1 C2 N2 179.1(10) . . . . ? N2 C3 C4 N1 0(2) . . . . ? N1 C1 C5 O2 177.6(11) . . . . ? C2 C1 C5 O2 -2.9(17) . . . . ? N1 C1 C5 O1 -0.9(14) . . . . ? C2 C1 C5 O1 178.6(11) . . . . ? C3 C4 N1 C1 -1.0(19) . . . . ? C3 C4 N1 Cu1 178.7(10) . . . . ? C2 C1 N1 C4 1.5(16) . . . . ? C5 C1 N1 C4 -179.0(10) . . . . ? C2 C1 N1 Cu1 -178.3(9) . . . . ? C5 C1 N1 Cu1 1.3(11) . . . . ? N1 Cu1 N1 C4 126(100) 5_666 . . . ? O1 Cu1 N1 C4 -0.7(12) 5_666 . . . ? O1 Cu1 N1 C4 179.3(12) . . . . ? N4 Cu1 N1 C4 -89.0(12) 5_666 . . . ? N4 Cu1 N1 C4 91.0(12) . . . . ? N1 Cu1 N1 C1 -54(100) 5_666 . . . ? O1 Cu1 N1 C1 179.0(8) 5_666 . . . ? O1 Cu1 N1 C1 -1.0(8) . . . . ? N4 Cu1 N1 C1 90.7(8) 5_666 . . . ? N4 Cu1 N1 C1 -89.3(8) . . . . ? C1 C2 N2 C3 0.7(19) . . . . ? C4 C3 N2 C2 -0.1(19) . . . . ? O2 C5 O1 Cu1 -178.3(10) . . . . ? C1 C5 O1 Cu1 0.1(12) . . . . ? N1 Cu1 O1 C5 0.5(8) . . . . ? N1 Cu1 O1 C5 -179.5(8) 5_666 . . . ? O1 Cu1 O1 C5 -169(100) 5_666 . . . ? N4 Cu1 O1 C5 -89.1(8) 5_666 . . . ? N4 Cu1 O1 C5 90.9(8) . . . . ? O1 C5 O2 Cd1 0.4(16) . . . 5_667 ? C1 C5 O2 Cd1 -178.0(7) . . . 5_667 ? N3 C6 C7 N4 -0.6(18) . . . . ? C10 C6 C7 N4 177.3(11) . . . . ? N4 C8 C9 N3 -3(2) . . . . ? C7 C6 C10 O4 -0.3(18) . . . . ? N3 C6 C10 O4 177.6(10) . . . . ? C7 C6 C10 O3 -178.4(12) . . . . ? N3 C6 C10 O3 -0.5(15) . . . . ? C8 C9 N3 C6 0.2(17) . . . . ? C8 C9 N3 Cu2 -178.6(9) . . . . ? C7 C6 N3 C9 1.2(16) . . . . ? C10 C6 N3 C9 -176.9(10) . . . . ? C7 C6 N3 Cu2 -179.7(9) . . . . ? C10 C6 N3 Cu2 2.2(11) . . . . ? O3 Cu2 N3 C9 -3.3(10) 5_667 . . . ? O3 Cu2 N3 C9 176.7(10) . . . . ? N3 Cu2 N3 C9 179(12) 5_667 . . . ? N2 Cu2 N3 C9 86.8(10) 6_557 . . . ? N2 Cu2 N3 C9 -93.2(10) 2_665 . . . ? O3 Cu2 N3 C6 177.7(7) 5_667 . . . ? O3 Cu2 N3 C6 -2.3(7) . . . . ? N3 Cu2 N3 C6 0(11) 5_667 . . . ? N2 Cu2 N3 C6 -92.2(7) 6_557 . . . ? N2 Cu2 N3 C6 87.8(7) 2_665 . . . ? C6 C7 N4 C8 -1.4(18) . . . . ? C6 C7 N4 Cu1 179.0(9) . . . . ? C9 C8 N4 C7 3.0(19) . . . . ? C9 C8 N4 Cu1 -177.4(10) . . . . ? N1 Cu1 N4 C7 -82.5(10) . . . . ? N1 Cu1 N4 C7 97.5(10) 5_666 . . . ? O1 Cu1 N4 C7 14.3(10) 5_666 . . . ? O1 Cu1 N4 C7 -165.7(10) . . . . ? N4 Cu1 N4 C7 -178(100) 5_666 . . . ? N1 Cu1 N4 C8 97.9(9) . . . . ? N1 Cu1 N4 C8 -82.1(9) 5_666 . . . ? O1 Cu1 N4 C8 -165.2(9) 5_666 . . . ? O1 Cu1 N4 C8 14.8(9) . . . . ? N4 Cu1 N4 C8 3(100) 5_666 . . . ? O4 C10 O3 Cu2 -179.5(9) . . . . ? C6 C10 O3 Cu2 -1.6(13) . . . . ? O3 Cu2 O3 C10 -155(2) 5_667 . . . ? N3 Cu2 O3 C10 2.2(8) . . . . ? N3 Cu2 O3 C10 -177.8(8) 5_667 . . . ? N2 Cu2 O3 C10 91.7(8) 6_557 . . . ? N2 Cu2 O3 C10 -88.3(8) 2_665 . . . ? O3 C10 O4 Cd3 1.8(15) . . . . ? C6 C10 O4 Cd3 -176.2(8) . . . . ? C10 O4 Cd3 O4 -175.9(7) . . . 7_565 ? C10 O4 Cd3 I3 -68.4(8) . . . . ? C10 O4 Cd3 I4 77.9(8) . . . . ? O2 Cd1 I1 Cd2 -130.1(2) 3_647 . . . ? O2 Cd1 I1 Cd2 130.1(2) 5_667 . . . ? I6 Cd1 I1 Cd2 0.0 6_658 . . . ? I2 Cd2 I1 Cd1 -78.32(7) . . . . ? I2 Cd2 I1 Cd1 78.32(7) 7_565 . . . ? I3 Cd2 I1 Cd1 180.0 . . . . ? O4 Cd3 I3 Cd2 -128.9(2) 7_565 . . . ? O4 Cd3 I3 Cd2 128.9(2) . . . . ? I4 Cd3 I3 Cd2 0.0 . . . . ? I2 Cd2 I3 Cd3 -107.84(6) . . . . ? I2 Cd2 I3 Cd3 107.84(6) 7_565 . . . ? I1 Cd2 I3 Cd3 0.0 . . . . ? O4 Cd3 I4 Cd4 -50.8(2) 7_565 . . . ? O4 Cd3 I4 Cd4 50.8(2) . . . . ? I3 Cd3 I4 Cd4 180.0 . . . . ? I5 Cd4 I4 Cd3 -74.86(7) . . . . ? I5 Cd4 I4 Cd3 74.86(7) 7_565 . . . ? I6 Cd4 I4 Cd3 180.0 . . . . ? I5 Cd4 I6 Cd1 -109.33(6) . . . 6_558 ? I5 Cd4 I6 Cd1 109.33(6) 7_565 . . 6_558 ? I4 Cd4 I6 Cd1 0.0 . . . 6_558 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 4.915 _refine_diff_density_min -2.360 _refine_diff_density_rms 0.408