# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1668 data_sad _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C7 H5 Cd K N2 O8' _chemical_formula_weight 396.63 _chemical_melting_point ? _chemical_compound_source ? 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' 'Cd' 'Cd' -0.8075 1.2024 '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 ? _symmetry_space_group_name_H-M ? 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 13.0160(2) _cell_length_b 11.2910(3) _cell_length_c 15.7543(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.0390(10) _cell_angle_gamma 90.00 _cell_volume 2236.01(9) _cell_formula_units_Z 8 _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 2.356 _exptl_crystal_density_method ? _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 2.366 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4641 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 23.25 _reflns_number_total 1617 _reflns_number_observed 1463 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0291P)^2^+8.3610P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1617 _refine_ls_number_parameters 174 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0302 _refine_ls_R_factor_obs 0.0259 _refine_ls_wR_factor_all 0.0664 _refine_ls_wR_factor_obs 0.0648 _refine_ls_goodness_of_fit_all 1.068 _refine_ls_goodness_of_fit_obs 1.103 _refine_ls_restrained_S_all 1.068 _refine_ls_restrained_S_obs 1.103 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cd1 Cd 0.69790(2) 0.17712(2) 0.67436(2) 0.01472(14) Uani 1 d . . O1 O 0.6372(2) 0.1511(3) 0.7996(2) 0.0289(8) Uani 1 d . . O2 O 0.6408(2) 0.3756(3) 0.6706(2) 0.0291(8) Uani 1 d . . O3 O 0.6633(2) -0.0266(3) 0.6461(2) 0.0245(7) Uani 1 d . . O4 O 0.6329(2) 0.1885(2) 0.5164(2) 0.0230(7) Uani 1 d . . O5 O 0.8358(2) 0.2350(3) 0.6047(2) 0.0245(7) Uani 1 d . . O6 O 0.8199(2) 0.2989(2) 0.7859(2) 0.0218(7) Uani 1 d . . O7 O 0.8455(2) 0.0484(2) 0.7584(2) 0.0233(7) Uani 1 d . . O8 O 0.4985(2) 0.1497(3) 0.6384(2) 0.0235(7) Uani 1 d . . C1 C 0.4602(3) 0.1514(3) 0.7033(3) 0.0177(9) Uani 1 d . . C2 C 0.6856(3) 0.4463(3) 0.7297(3) 0.0166(9) Uani 1 d . . C3 C 0.7909(3) 0.4021(3) 0.7956(3) 0.0152(9) Uani 1 d . . C4 C 0.8087(3) 0.2634(3) 0.5258(3) 0.0153(9) Uani 1 d . . C12 C 0.3157(4) 0.3600(4) 0.4397(3) 0.0219(10) Uani 1 d . . H5 H 0.2714(4) 0.3318(4) 0.3874(3) 0.026 Uiso 1 calc R . C11 C 0.4513(3) 0.3866(4) 0.5455(3) 0.0206(10) Uani 1 d . . H3 H 0.5204(3) 0.3808(4) 0.5810(3) 0.025 Uiso 1 calc R . N2 N 0.4133(6) 0.3300(4) 0.4730(4) 0.071(2) Uani 1 d . . H4 H 0.4481(6) 0.2797(4) 0.4503(4) 0.085 Uiso 1 calc R . C10 C 0.3764(5) 0.4532(5) 0.5605(3) 0.049(2) Uani 1 d . . H2 H 0.3813(5) 0.5023(5) 0.6088(3) 0.059 Uiso 1 calc R . N1 N 0.2903(4) 0.4371(6) 0.4926(4) 0.079(2) Uani 1 d . . H1 H 0.2297(4) 0.4713(6) 0.4853(4) 0.095 Uiso 1 calc R . K1 K 0.5000 0.0000 0.5000 0.0243(3) Uani 1 d S . K2 K 1.0000 0.21197(12) 0.7500 0.0232(3) Uani 1 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 Cd1 0.0158(2) 0.0140(2) 0.0146(2) 0.00021(11) 0.00432(14) -0.00017(11) O1 0.013(2) 0.055(2) 0.018(2) 0.0020(14) 0.0032(13) -0.0006(14) O2 0.027(2) 0.020(2) 0.030(2) -0.0065(14) -0.0109(14) 0.0042(14) O3 0.026(2) 0.020(2) 0.023(2) 0.0038(13) -0.0022(14) 0.0023(13) O4 0.018(2) 0.030(2) 0.023(2) 0.0030(13) 0.0080(14) -0.0062(13) O5 0.018(2) 0.036(2) 0.018(2) 0.0054(13) 0.0023(13) -0.0031(14) O6 0.021(2) 0.018(2) 0.025(2) -0.0001(12) 0.0026(13) 0.0052(13) O7 0.025(2) 0.016(2) 0.029(2) -0.0008(12) 0.0060(14) -0.0048(13) O8 0.022(2) 0.033(2) 0.018(2) 0.0004(13) 0.0074(14) 0.0014(13) C1 0.019(2) 0.016(2) 0.019(2) -0.001(2) 0.007(2) -0.001(2) C2 0.017(2) 0.016(2) 0.017(2) 0.000(2) 0.005(2) -0.002(2) C3 0.016(2) 0.016(2) 0.015(2) 0.001(2) 0.006(2) -0.003(2) C4 0.018(2) 0.015(2) 0.014(2) 0.000(2) 0.006(2) 0.000(2) C12 0.026(3) 0.024(2) 0.009(2) -0.002(2) -0.006(2) -0.002(2) C11 0.014(2) 0.026(2) 0.014(2) 0.003(2) -0.010(2) 0.000(2) N2 0.107(6) 0.036(3) 0.097(5) 0.012(3) 0.073(5) 0.024(3) C10 0.075(5) 0.046(3) 0.030(3) -0.016(3) 0.018(3) -0.016(3) N1 0.043(3) 0.087(5) 0.109(5) 0.024(4) 0.024(4) 0.015(3) K1 0.0236(7) 0.0255(7) 0.0209(7) -0.0015(5) 0.0003(6) -0.0070(6) K2 0.0151(7) 0.0289(7) 0.0240(7) 0.000 0.0023(6) 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 Cd1 O1 2.327(3) . ? Cd1 O2 2.357(3) . ? Cd1 O3 2.364(3) . ? Cd1 O4 2.416(3) . ? Cd1 O5 2.424(3) . ? Cd1 O6 2.460(3) . ? Cd1 O7 2.497(3) . ? Cd1 O8 2.528(3) . ? O1 C1 1.257(5) 2_656 ? O2 C2 1.250(5) . ? O3 C3 1.251(5) 4_646 ? O4 C4 1.255(5) 7_656 ? O5 C4 1.244(5) . ? O6 C3 1.247(5) . ? O7 C2 1.253(5) 4_646 ? O8 C1 1.249(5) . ? C1 O1 1.257(5) 2_656 ? C1 C1 1.563(8) 2_656 ? C2 O7 1.253(5) 4_656 ? C2 C3 1.570(6) . ? C3 O3 1.251(5) 4_656 ? C4 O4 1.255(5) 7_656 ? C4 C4 1.562(8) 7_656 ? C12 N2 1.288(8) . ? C12 N1 1.306(8) . ? C12 H5 0.93 . ? C11 N2 1.290(7) . ? C11 C10 1.300(7) . ? C11 H3 0.93 . ? N2 H4 0.86 . ? C10 N1 1.346(8) . ? C10 H2 0.93 . ? N1 H1 0.86 . ? 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 O1 Cd1 O2 88.14(12) . . ? O1 Cd1 O3 86.96(11) . . ? O2 Cd1 O3 151.29(11) . . ? O1 Cd1 O4 140.86(10) . . ? O2 Cd1 O4 84.22(10) . . ? O3 Cd1 O4 81.89(10) . . ? O1 Cd1 O5 150.71(10) . . ? O2 Cd1 O5 89.88(11) . . ? O3 Cd1 O5 107.71(10) . . ? O4 Cd1 O5 67.78(9) . . ? O1 Cd1 O6 76.29(11) . . ? O2 Cd1 O6 68.13(9) . . ? O3 Cd1 O6 137.27(9) . . ? O4 Cd1 O6 134.02(10) . . ? O5 Cd1 O6 75.88(10) . . ? O1 Cd1 O7 81.98(10) . . ? O2 Cd1 O7 139.53(10) . . ? O3 Cd1 O7 67.46(9) . . ? O4 Cd1 O7 126.38(10) . . ? O5 Cd1 O7 80.70(10) . . ? O6 Cd1 O7 71.40(9) . . ? O1 Cd1 O8 67.67(10) . . ? O2 Cd1 O8 79.17(10) . . ? O3 Cd1 O8 72.80(10) . . ? O4 Cd1 O8 73.19(9) . . ? O5 Cd1 O8 140.31(9) . . ? O6 Cd1 O8 131.57(9) . . ? O7 Cd1 O8 130.67(9) . . ? C1 O1 Cd1 122.0(3) 2_656 . ? C2 O2 Cd1 120.4(3) . . ? C3 O3 Cd1 117.2(3) 4_646 . ? C4 O4 Cd1 118.0(3) 7_656 . ? C4 O5 Cd1 118.1(3) . . ? C3 O6 Cd1 116.7(3) . . ? C2 O7 Cd1 112.4(3) 4_646 . ? C1 O8 Cd1 114.8(3) . . ? O8 C1 O1 125.6(4) . 2_656 ? O8 C1 C1 117.6(5) . 2_656 ? O1 C1 C1 116.8(4) 2_656 2_656 ? O2 C2 O7 126.4(4) . 4_656 ? O2 C2 C3 116.6(3) . . ? O7 C2 C3 117.0(3) 4_656 . ? O6 C3 O3 126.1(4) . 4_656 ? O6 C3 C2 117.1(3) . . ? O3 C3 C2 116.7(3) 4_656 . ? O5 C4 O4 125.9(4) . 7_656 ? O5 C4 C4 117.1(4) . 7_656 ? O4 C4 C4 117.0(4) 7_656 7_656 ? N2 C12 N1 107.5(5) . . ? N2 C12 H5 126.2(3) . . ? N1 C12 H5 126.2(3) . . ? N2 C11 C10 108.3(5) . . ? N2 C11 H3 125.8(3) . . ? C10 C11 H3 125.8(3) . . ? C12 N2 C11 110.0(4) . . ? C12 N2 H4 125.0(3) . . ? C11 N2 H4 125.0(3) . . ? C11 C10 N1 106.6(5) . . ? C11 C10 H2 126.7(3) . . ? N1 C10 H2 126.7(4) . . ? C12 N1 C10 107.5(5) . . ? C12 N1 H1 126.2(3) . . ? C10 N1 H1 126.2(4) . . ? _refine_diff_density_max 0.584 _refine_diff_density_min -0.740 _refine_diff_density_rms 0.112