# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full Chem.Mater. _journal_coden_cambridge 1096 _journal_year 2003 _journal_volume 15 _journal_page_first 4576 _publ_contact_author 'Adonis Michaelides' _publ_contact_author_email amihail@cc.uoi.gr loop_ _publ_author_name 'Stavroula Skoulika' 'Panagiotis Dallas' M.G.Siskos Y.Deligiannakis 'Adonis Michaelides' _publ_contact_author_address ; Department of Chemistry University of Ioannina Ioannina 45110 GREECE ; _publ_contact_author_name 'Dr Adonis Michaelides' _publ_requested_journal 'Chemical Communications' _publ_section_title ; Assembly of a photoreactive coordination polymer containing rectangular grids ; data_cdfum _database_code_depnum_ccdc_archive 'CCDC 168034' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H6 Cd O6' _chemical_formula_weight 262.50 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' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.7570(10) _cell_length_b 7.5440(10) _cell_length_c 7.8090(10) _cell_angle_alpha 68.540(10) _cell_angle_beta 86.530(10) _cell_angle_gamma 69.960(10) _cell_volume 347.08(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 4.9 _cell_measurement_theta_max 11.3 _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.512 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 252 _exptl_absorpt_coefficient_mu 3.126 _exptl_absorpt_correction_type none _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_type P4 _diffrn_measurement_method scintillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 99 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 1512 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_sigmaI/netI 0.0366 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1183 _reflns_number_gt 1109 _reflns_threshold_expression >2sigma(I) _computing_data_collection XSCANS _computing_cell_refinement XSCANS _computing_data_reduction XSCANS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SCHAKAL97 _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 fullcycle _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0528P)^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 1183 _refine_ls_number_parameters 124 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0320 _refine_ls_R_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0774 _refine_ls_wR_factor_gt 0.0755 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.002 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.35337(5) 0.18283(4) 0.61053(4) 0.02031(17) Uani 1 d . . . O1 O 0.5101(6) 0.1562(5) 0.3409(4) 0.0309(9) Uani 1 d . . . O2 O 0.3574(6) 0.4703(5) 0.3181(4) 0.0272(8) Uani 1 d . . . O3 O 0.1778(6) 0.4347(5) 0.7210(4) 0.0266(7) Uani 1 d . . . O4 O 0.2251(6) 0.1275(5) 0.9225(5) 0.0312(8) Uani 1 d . . . O5 O 0.6777(6) 0.1503(6) 0.7233(5) 0.0281(8) Uani 1 d . . . O6 O 0.0451(7) 0.1858(6) 0.5018(6) 0.0335(8) Uani 1 d . . . C1 C 0.4629(7) 0.3438(7) 0.2499(6) 0.0192(9) Uani 1 d . . . C2 C 0.5342(7) 0.4058(7) 0.0603(6) 0.0198(9) Uani 1 d . . . C3 C 0.1511(7) 0.3168(6) 0.8779(6) 0.0211(10) Uani 1 d . . . C4 C 0.0370(8) 0.4023(8) 1.0160(6) 0.0231(9) Uani 1 d . . . H2 H 0.012(10) 0.310(10) 1.119(9) 0.043(18) Uiso 1 d . . . H4 H 0.641(10) 0.302(10) 0.019(9) 0.042(17) Uiso 1 d . . . H5A H 0.670(9) 0.256(10) 0.725(8) 0.026(16) Uiso 1 d . . . H6A H -0.034(15) 0.319(15) 0.434(13) 0.08(3) Uiso 1 d . . . H5B H 0.704(12) 0.074(12) 0.837(12) 0.06(2) Uiso 1 d . . . H6B H -0.032(15) 0.150(13) 0.570(12) 0.07(3) Uiso 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 Cd1 0.0290(2) 0.0183(2) 0.0122(2) -0.00775(15) 0.00770(14) -0.00509(15) O1 0.054(2) 0.0145(17) 0.0167(16) -0.0039(13) 0.0125(16) -0.0062(16) O2 0.042(2) 0.0213(16) 0.0192(16) -0.0105(13) 0.0143(15) -0.0103(15) O3 0.0360(19) 0.0263(17) 0.0155(15) -0.0108(13) 0.0123(13) -0.0068(14) O4 0.046(2) 0.0227(18) 0.0198(16) -0.0089(14) 0.0082(15) -0.0054(16) O5 0.040(2) 0.0195(18) 0.0229(18) -0.0075(15) 0.0034(15) -0.0088(15) O6 0.035(2) 0.029(2) 0.030(2) -0.0062(16) 0.0008(17) -0.0072(17) C1 0.025(2) 0.021(2) 0.013(2) -0.0071(18) 0.0043(17) -0.0098(19) C2 0.024(2) 0.023(2) 0.014(2) -0.0070(17) 0.0062(17) -0.0100(18) C3 0.021(2) 0.024(3) 0.020(2) -0.014(2) 0.0037(19) -0.004(2) C4 0.030(2) 0.027(2) 0.013(2) -0.0085(18) 0.0046(17) -0.0094(19) _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 O6 2.287(4) . ? Cd1 O1 2.292(3) 2_656 ? Cd1 O3 2.300(3) . ? Cd1 O5 2.312(4) . ? Cd1 O1 2.343(3) . ? Cd1 O4 2.471(4) . ? Cd1 O2 2.516(3) . ? Cd1 C3 2.739(4) . ? O1 C1 1.262(5) . ? O1 Cd1 2.292(3) 2_656 ? O2 C1 1.250(6) . ? O3 C3 1.269(6) . ? O4 C3 1.257(6) . ? O5 H5A 0.79(7) . ? O5 H5B 0.85(8) . ? O6 H6A 0.93(10) . ? O6 H6B 0.77(10) . ? C1 C2 1.485(6) . ? C2 C2 1.321(9) 2_665 ? C2 H4 1.01(7) . ? C3 C4 1.497(6) . ? C4 C4 1.313(10) 2_567 ? C4 H2 0.90(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 O6 Cd1 O1 87.44(15) . 2_656 ? O6 Cd1 O3 92.35(14) . . ? O1 Cd1 O3 148.78(11) 2_656 . ? O6 Cd1 O5 174.97(13) . . ? O1 Cd1 O5 87.54(14) 2_656 . ? O3 Cd1 O5 92.09(13) . . ? O6 Cd1 O1 90.16(15) . . ? O1 Cd1 O1 73.23(13) 2_656 . ? O3 Cd1 O1 137.98(11) . . ? O5 Cd1 O1 88.12(14) . . ? O6 Cd1 O4 90.95(15) . . ? O1 Cd1 O4 94.05(11) 2_656 . ? O3 Cd1 O4 54.73(12) . . ? O5 Cd1 O4 89.69(13) . . ? O1 Cd1 O4 167.17(12) . . ? O6 Cd1 O2 90.24(14) . . ? O1 Cd1 O2 126.34(11) 2_656 . ? O3 Cd1 O2 84.87(11) . . ? O5 Cd1 O2 92.51(13) . . ? O1 Cd1 O2 53.16(11) . . ? O4 Cd1 O2 139.60(11) . . ? O6 Cd1 C3 91.15(14) . . ? O1 Cd1 C3 121.34(13) 2_656 . ? O3 Cd1 C3 27.44(13) . . ? O5 Cd1 C3 91.70(13) . . ? O1 Cd1 C3 165.41(12) . . ? O4 Cd1 C3 27.31(13) . . ? O2 Cd1 C3 112.30(12) . . ? C1 O1 Cd1 156.1(3) . 2_656 ? C1 O1 Cd1 97.1(3) . . ? Cd1 O1 Cd1 106.77(13) 2_656 . ? C1 O2 Cd1 89.3(3) . . ? C3 O3 Cd1 95.9(3) . . ? C3 O4 Cd1 88.3(3) . . ? Cd1 O5 H5A 108(4) . . ? Cd1 O5 H5B 112(5) . . ? H5A O5 H5B 102(7) . . ? Cd1 O6 H6A 108(6) . . ? Cd1 O6 H6B 119(6) . . ? H6A O6 H6B 103(8) . . ? O2 C1 O1 120.4(4) . . ? O2 C1 C2 122.2(4) . . ? O1 C1 C2 117.4(4) . . ? C2 C2 C1 123.4(5) 2_665 . ? C2 C2 H4 117(4) 2_665 . ? C1 C2 H4 120(4) . . ? O4 C3 O3 121.0(4) . . ? O4 C3 C4 118.9(4) . . ? O3 C3 C4 120.1(4) . . ? O4 C3 Cd1 64.4(2) . . ? O3 C3 Cd1 56.7(2) . . ? C4 C3 Cd1 176.7(3) . . ? C4 C4 C3 122.9(6) 2_567 . ? C4 C4 H2 122(4) 2_567 . ? C3 C4 H2 115(4) . . ? 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 O6 Cd1 O1 C1 91.0(3) . . . . ? O1 Cd1 O1 C1 178.3(4) 2_656 . . . ? O3 Cd1 O1 C1 -2.6(4) . . . . ? O5 Cd1 O1 C1 -93.7(3) . . . . ? O4 Cd1 O1 C1 -174.0(5) . . . . ? O2 Cd1 O1 C1 0.9(3) . . . . ? C3 Cd1 O1 C1 -4.2(7) . . . . ? O6 Cd1 O1 Cd1 -87.27(17) . . . 2_656 ? O1 Cd1 O1 Cd1 0.0 2_656 . . 2_656 ? O3 Cd1 O1 Cd1 179.04(14) . . . 2_656 ? O5 Cd1 O1 Cd1 88.00(17) . . . 2_656 ? O4 Cd1 O1 Cd1 7.7(7) . . . 2_656 ? O2 Cd1 O1 Cd1 -177.5(2) . . . 2_656 ? C3 Cd1 O1 Cd1 177.5(4) . . . 2_656 ? O6 Cd1 O2 C1 -90.9(3) . . . . ? O1 Cd1 O2 C1 -3.9(3) 2_656 . . . ? O3 Cd1 O2 C1 176.8(3) . . . . ? O5 Cd1 O2 C1 84.9(3) . . . . ? O1 Cd1 O2 C1 -0.9(3) . . . . ? O4 Cd1 O2 C1 177.4(3) . . . . ? C3 Cd1 O2 C1 177.8(3) . . . . ? O6 Cd1 O3 C3 88.0(3) . . . . ? O1 Cd1 O3 C3 -0.9(4) 2_656 . . . ? O5 Cd1 O3 C3 -89.7(3) . . . . ? O1 Cd1 O3 C3 -179.2(2) . . . . ? O4 Cd1 O3 C3 -1.5(3) . . . . ? O2 Cd1 O3 C3 178.0(3) . . . . ? O6 Cd1 O4 C3 -90.7(3) . . . . ? O1 Cd1 O4 C3 -178.2(3) 2_656 . . . ? O3 Cd1 O4 C3 1.5(3) . . . . ? O5 Cd1 O4 C3 94.3(3) . . . . ? O1 Cd1 O4 C3 174.4(5) . . . . ? O2 Cd1 O4 C3 0.8(4) . . . . ? Cd1 O2 C1 O1 1.5(5) . . . . ? Cd1 O2 C1 C2 -179.6(4) . . . . ? Cd1 O1 C1 O2 174.4(6) 2_656 . . . ? Cd1 O1 C1 O2 -1.6(5) . . . . ? Cd1 O1 C1 C2 -4.6(11) 2_656 . . . ? Cd1 O1 C1 C2 179.4(3) . . . . ? O2 C1 C2 C2 -11.1(9) . . . 2_665 ? O1 C1 C2 C2 167.9(6) . . . 2_665 ? Cd1 O4 C3 O3 -2.6(5) . . . . ? Cd1 O4 C3 C4 179.6(4) . . . . ? Cd1 O3 C3 O4 2.9(5) . . . . ? Cd1 O3 C3 C4 -179.4(4) . . . . ? O6 Cd1 C3 O4 89.8(3) . . . . ? O1 Cd1 C3 O4 2.1(3) 2_656 . . . ? O3 Cd1 C3 O4 -177.3(5) . . . . ? O5 Cd1 C3 O4 -86.0(3) . . . . ? O1 Cd1 C3 O4 -175.1(5) . . . . ? O2 Cd1 C3 O4 -179.4(3) . . . . ? O6 Cd1 C3 O3 -92.9(3) . . . . ? O1 Cd1 C3 O3 179.4(3) 2_656 . . . ? O5 Cd1 C3 O3 91.3(3) . . . . ? O1 Cd1 C3 O3 2.2(7) . . . . ? O4 Cd1 C3 O3 177.3(5) . . . . ? O2 Cd1 C3 O3 -2.1(3) . . . . ? O6 Cd1 C3 C4 -84(5) . . . . ? O1 Cd1 C3 C4 -172(5) 2_656 . . . ? O3 Cd1 C3 C4 8(5) . . . . ? O5 Cd1 C3 C4 100(5) . . . . ? O1 Cd1 C3 C4 11(6) . . . . ? O4 Cd1 C3 C4 -174(6) . . . . ? O2 Cd1 C3 C4 6(6) . . . . ? O4 C3 C4 C4 176.9(6) . . . 2_567 ? O3 C3 C4 C4 -0.8(9) . . . 2_567 ? Cd1 C3 C4 C4 -9(6) . . . 2_567 ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.674 _refine_diff_density_min -1.684 _refine_diff_density_rms 0.152