Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _publ_section_title ;Designed self-assembly of a reactive metal-organic framework with quasi alpha-Po topology ; _publ_contact_author_name 'Adonis Michaelides' _publ_contact_author_email AMIHAIL@CC.UOI.GR loop_ _publ_author_name 'Adonis Michaelides' 'Michael G' Siskos 'Stavroula Skoulika' # Attachment 'cdfumbp.cif' data_cdfumbp _database_code_depnum_ccdc_archive 'CCDC 656176' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H12 Cd N2 O4' _chemical_formula_weight 408.68 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' N N 0.0061 0.0033 '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 9.1050(10) _cell_length_b 12.9480(10) _cell_length_c 13.991(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.510(10) _cell_angle_gamma 90.00 _cell_volume 1648.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 40 _cell_measurement_theta_min 9.3 _cell_measurement_theta_max 12.6 _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.646 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 1.344 _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 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 3354 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0784 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2872 _reflns_number_gt 1933 _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 ? _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^)+(0.0697P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2872 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0881 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1271 _refine_ls_wR_factor_gt 0.1092 _refine_ls_goodness_of_fit_ref 0.963 _refine_ls_restrained_S_all 0.963 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 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 0.96905(6) 0.14551(4) 0.97020(3) 0.02543(18) Uani 1 d . . . O1 O 1.2514(6) -0.0675(5) 1.0449(4) 0.0476(15) Uani 1 d . . . O2 O 1.2015(6) 0.0853(5) 0.9787(4) 0.0520(17) Uani 1 d . . . O3 O 1.0726(7) 0.3109(5) 1.0017(5) 0.0539(17) Uani 1 d . . . O4 O 0.8462(7) 0.3073(5) 0.9454(5) 0.0565(17) Uani 1 d . . . C1 C 1.2886(8) 0.0163(7) 1.0067(5) 0.0334(18) Uani 1 d . . . C2 C 1.4482(8) 0.0344(6) 0.9937(5) 0.0316(18) Uani 1 d . . . H2 H 1.4766 0.1003 0.9752 0.038 Uiso 1 calc R . . C3 C 0.9565(9) 0.3546(7) 0.9743(6) 0.0391(18) Uani 1 d . . . C4 C 0.9475(9) 0.4700(6) 0.9815(6) 0.041(2) Uani 1 d . . . H4 H 0.8621 0.5018 0.9583 0.050 Uiso 1 calc R . . N5 N 0.9448(7) 0.1377(6) 1.1352(4) 0.0392(16) Uani 1 d . . . C6 C 0.8146(9) 0.1452(7) 1.1756(5) 0.044(2) Uani 1 d . . . H6 H 0.7300 0.1459 1.1369 0.053 Uiso 1 calc R . . C7 C 0.8016(9) 0.1520(7) 1.2746(6) 0.046(2) Uani 1 d . . . H7 H 0.7089 0.1576 1.3005 0.056 Uiso 1 calc R . . C8 C 0.9232(9) 0.1505(7) 1.3343(5) 0.042(2) Uani 1 d . . . C9 C 1.0596(9) 0.1412(8) 1.2916(5) 0.049(2) Uani 1 d . . . H9 H 1.1453 0.1388 1.3292 0.058 Uiso 1 calc R . . C10 C 1.0663(9) 0.1356(7) 1.1928(5) 0.042(2) Uani 1 d . . . H10 H 1.1578 0.1303 1.1651 0.051 Uiso 1 calc R . . C11 C 0.9077(9) 0.1537(7) 1.4382(5) 0.042(2) Uani 1 d . . . H11 H 0.8147 0.1675 1.4610 0.051 Uiso 1 calc R . . C12 C 1.0149(10) 0.1386(8) 1.5022(5) 0.046(2) Uani 1 d . . . H12 H 1.1083 0.1275 1.4790 0.055 Uiso 1 calc R . . C13 C 1.0006(9) 0.1377(7) 1.6055(5) 0.0380(19) Uani 1 d . . . C14 C 0.8695(9) 0.1578(7) 1.6514(5) 0.046(2) Uani 1 d . . . H14 H 0.7842 0.1731 1.6161 0.055 Uiso 1 calc R . . C15 C 0.8680(9) 0.1546(7) 1.7509(6) 0.047(2) Uani 1 d . . . H15 H 0.7795 0.1670 1.7805 0.056 Uiso 1 calc R . . N16 N 0.9878(7) 0.1344(5) 1.8068(4) 0.0360(16) Uani 1 d . . . C17 C 1.1137(9) 0.1170(6) 1.7623(5) 0.037(2) Uani 1 d . . . H17 H 1.1985 0.1039 1.7988 0.045 Uiso 1 calc R . . C18 C 1.1218(9) 0.1180(6) 1.6636(5) 0.040(2) Uani 1 d . . . H18 H 1.2115 0.1049 1.6357 0.048 Uiso 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 Cd1 0.0223(3) 0.0316(3) 0.0224(3) 0.0009(3) 0.00079(17) -0.0003(3) O1 0.030(3) 0.067(4) 0.047(3) 0.007(3) 0.004(3) -0.006(3) O2 0.029(3) 0.077(5) 0.050(3) 0.001(3) -0.003(3) 0.025(3) O3 0.038(4) 0.038(3) 0.085(5) -0.003(3) -0.012(3) 0.000(3) O4 0.039(4) 0.047(4) 0.083(5) -0.011(4) -0.017(3) -0.005(3) C1 0.027(4) 0.051(5) 0.022(3) -0.003(4) 0.000(3) 0.001(4) C2 0.026(4) 0.030(4) 0.038(4) 0.006(3) 0.001(3) -0.005(3) C3 0.033(4) 0.041(4) 0.044(4) -0.004(5) 0.007(3) 0.006(5) C4 0.030(5) 0.035(5) 0.058(5) 0.010(4) -0.003(4) -0.002(4) N5 0.041(4) 0.049(4) 0.027(3) 0.002(3) 0.006(3) 0.002(4) C6 0.042(5) 0.056(5) 0.035(4) -0.003(5) -0.003(4) -0.001(5) C7 0.034(4) 0.067(6) 0.039(4) 0.003(5) 0.007(4) 0.015(5) C8 0.044(5) 0.054(5) 0.029(4) 0.005(5) 0.006(4) 0.006(5) C9 0.040(5) 0.074(6) 0.031(4) -0.011(5) -0.009(4) 0.004(5) C10 0.034(4) 0.064(6) 0.029(4) 0.005(4) -0.005(3) 0.004(5) C11 0.039(4) 0.055(5) 0.033(4) -0.001(4) 0.004(4) 0.002(5) C12 0.053(5) 0.069(6) 0.015(3) -0.004(4) 0.007(4) -0.002(6) C13 0.044(5) 0.047(5) 0.023(4) 0.005(4) 0.001(3) 0.000(5) C14 0.036(4) 0.070(6) 0.032(4) -0.003(5) -0.004(3) 0.012(5) C15 0.034(4) 0.072(6) 0.034(4) 0.004(5) -0.002(4) 0.011(5) N16 0.042(4) 0.049(4) 0.017(3) -0.005(3) -0.001(3) -0.001(4) C17 0.028(4) 0.056(6) 0.028(4) 0.001(4) 0.000(3) -0.002(4) C18 0.033(4) 0.056(6) 0.031(4) 0.000(4) 0.005(3) 0.012(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 Cd1 O1 2.251(6) 3_757 ? Cd1 O2 2.256(5) . ? Cd1 N16 2.301(6) 1_554 ? Cd1 N5 2.327(6) . ? Cd1 O3 2.377(6) . ? Cd1 O4 2.396(6) . ? Cd1 C3 2.711(9) . ? O1 C1 1.260(10) . ? O1 Cd1 2.251(6) 3_757 ? O2 C1 1.250(9) . ? O3 C3 1.250(9) . ? O4 C3 1.235(10) . ? C1 C2 1.488(10) . ? C2 C2 1.307(15) 3_857 ? C2 H2 0.9300 . ? C3 C4 1.500(12) . ? C4 C4 1.327(15) 3_767 ? C4 H4 0.9300 . ? N5 C6 1.330(10) . ? N5 C10 1.351(10) . ? C6 C7 1.397(11) . ? C6 H6 0.9300 . ? C7 C8 1.369(11) . ? C7 H7 0.9300 . ? C8 C9 1.397(11) . ? C8 C11 1.465(10) . ? C9 C10 1.388(10) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.322(12) . ? C11 H11 0.9300 . ? C12 C13 1.454(10) . ? C12 H12 0.9300 . ? C13 C18 1.377(11) . ? C13 C14 1.395(11) . ? C14 C15 1.392(11) . ? C14 H14 0.9300 . ? C15 N16 1.351(10) . ? C15 H15 0.9300 . ? N16 C17 1.339(10) . ? N16 Cd1 2.301(6) 1_556 ? C17 C18 1.385(10) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? 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 133.1(2) 3_757 . ? O1 Cd1 N16 88.2(2) 3_757 1_554 ? O2 Cd1 N16 86.4(2) . 1_554 ? O1 Cd1 N5 88.0(2) 3_757 . ? O2 Cd1 N5 92.6(2) . . ? N16 Cd1 N5 173.8(2) 1_554 . ? O1 Cd1 O3 140.3(2) 3_757 . ? O2 Cd1 O3 86.3(2) . . ? N16 Cd1 O3 101.6(3) 1_554 . ? N5 Cd1 O3 84.4(3) . . ? O1 Cd1 O4 88.1(2) 3_757 . ? O2 Cd1 O4 138.0(2) . . ? N16 Cd1 O4 87.6(2) 1_554 . ? N5 Cd1 O4 97.2(2) . . ? O3 Cd1 O4 54.5(2) . . ? O1 Cd1 C3 114.3(2) 3_757 . ? O2 Cd1 C3 112.6(2) . . ? N16 Cd1 C3 95.0(2) 1_554 . ? N5 Cd1 C3 91.0(2) . . ? O3 Cd1 C3 27.4(2) . . ? O4 Cd1 C3 27.1(2) . . ? C1 O1 Cd1 126.5(5) . 3_757 ? C1 O2 Cd1 148.2(6) . . ? C3 O3 Cd1 91.3(5) . . ? C3 O4 Cd1 90.8(5) . . ? O2 C1 O1 125.0(7) . . ? O2 C1 C2 117.5(7) . . ? O1 C1 C2 117.5(7) . . ? C2 C2 C1 125.4(10) 3_857 . ? C2 C2 H2 117.3 3_857 . ? C1 C2 H2 117.3 . . ? O4 C3 O3 123.3(8) . . ? O4 C3 C4 118.1(8) . . ? O3 C3 C4 118.5(8) . . ? O4 C3 Cd1 62.1(5) . . ? O3 C3 Cd1 61.2(4) . . ? C4 C3 Cd1 177.3(6) . . ? C4 C4 C3 124.6(10) 3_767 . ? C4 C4 H4 117.7 3_767 . ? C3 C4 H4 117.7 . . ? C6 N5 C10 118.2(7) . . ? C6 N5 Cd1 121.8(5) . . ? C10 N5 Cd1 119.7(5) . . ? N5 C6 C7 121.7(8) . . ? N5 C6 H6 119.1 . . ? C7 C6 H6 119.1 . . ? C8 C7 C6 121.0(8) . . ? C8 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C7 C8 C9 117.0(7) . . ? C7 C8 C11 120.5(8) . . ? C9 C8 C11 122.4(7) . . ? C10 C9 C8 119.6(7) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? N5 C10 C9 122.4(8) . . ? N5 C10 H10 118.8 . . ? C9 C10 H10 118.8 . . ? C12 C11 C8 125.5(8) . . ? C12 C11 H11 117.3 . . ? C8 C11 H11 117.3 . . ? C11 C12 C13 126.2(8) . . ? C11 C12 H12 116.9 . . ? C13 C12 H12 116.9 . . ? C18 C13 C14 116.4(7) . . ? C18 C13 C12 119.7(8) . . ? C14 C13 C12 123.8(7) . . ? C13 C14 C15 119.0(8) . . ? C13 C14 H14 120.5 . . ? C15 C14 H14 120.5 . . ? N16 C15 C14 123.8(8) . . ? N16 C15 H15 118.1 . . ? C14 C15 H15 118.1 . . ? C17 N16 C15 116.8(6) . . ? C17 N16 Cd1 124.1(5) . 1_556 ? C15 N16 Cd1 118.9(5) . 1_556 ? N16 C17 C18 122.1(7) . . ? N16 C17 H17 118.9 . . ? C18 C17 H17 118.9 . . ? C13 C18 C17 121.8(8) . . ? C13 C18 H18 119.1 . . ? C17 C18 H18 119.1 . . ? 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 O1 Cd1 O2 C1 -35.2(11) 3_757 . . . ? N16 Cd1 O2 C1 -119.3(10) 1_554 . . . ? N5 Cd1 O2 C1 54.6(10) . . . . ? O3 Cd1 O2 C1 138.9(10) . . . . ? O4 Cd1 O2 C1 158.5(9) . . . . ? C3 Cd1 O2 C1 146.8(10) . . . . ? O1 Cd1 O3 C3 -22.9(7) 3_757 . . . ? O2 Cd1 O3 C3 163.9(5) . . . . ? N16 Cd1 O3 C3 78.4(5) 1_554 . . . ? N5 Cd1 O3 C3 -103.0(5) . . . . ? O4 Cd1 O3 C3 -0.1(5) . . . . ? O1 Cd1 O4 C3 165.7(5) 3_757 . . . ? O2 Cd1 O4 C3 -24.2(7) . . . . ? N16 Cd1 O4 C3 -106.0(5) 1_554 . . . ? N5 Cd1 O4 C3 77.9(5) . . . . ? O3 Cd1 O4 C3 0.1(5) . . . . ? Cd1 O2 C1 O1 6.9(15) . . . . ? Cd1 O2 C1 C2 -173.2(7) . . . . ? Cd1 O1 C1 O2 23.0(11) 3_757 . . . ? Cd1 O1 C1 C2 -156.9(5) 3_757 . . . ? O2 C1 C2 C2 -169.8(9) . . . 3_857 ? O1 C1 C2 C2 10.1(14) . . . 3_857 ? Cd1 O4 C3 O3 -0.1(9) . . . . ? Cd1 O4 C3 C4 -176.9(7) . . . . ? Cd1 O3 C3 O4 0.1(9) . . . . ? Cd1 O3 C3 C4 176.9(7) . . . . ? O1 Cd1 C3 O4 -15.7(6) 3_757 . . . ? O2 Cd1 C3 O4 162.7(5) . . . . ? N16 Cd1 C3 O4 74.6(5) 1_554 . . . ? N5 Cd1 C3 O4 -104.0(5) . . . . ? O3 Cd1 C3 O4 -179.9(8) . . . . ? O1 Cd1 C3 O3 164.2(5) 3_757 . . . ? O2 Cd1 C3 O3 -17.4(6) . . . . ? N16 Cd1 C3 O3 -105.5(5) 1_554 . . . ? N5 Cd1 C3 O3 75.9(5) . . . . ? O4 Cd1 C3 O3 179.9(8) . . . . ? O4 C3 C4 C4 174.2(10) . . . 3_767 ? O3 C3 C4 C4 -2.8(16) . . . 3_767 ? O1 Cd1 N5 C6 -33.1(7) 3_757 . . . ? O2 Cd1 N5 C6 -166.1(7) . . . . ? O3 Cd1 N5 C6 107.9(7) . . . . ? O4 Cd1 N5 C6 54.8(7) . . . . ? C3 Cd1 N5 C6 81.2(7) . . . . ? O1 Cd1 N5 C10 153.5(7) 3_757 . . . ? O2 Cd1 N5 C10 20.5(7) . . . . ? O3 Cd1 N5 C10 -65.5(7) . . . . ? O4 Cd1 N5 C10 -118.6(7) . . . . ? C3 Cd1 N5 C10 -92.2(7) . . . . ? C10 N5 C6 C7 0.7(14) . . . . ? Cd1 N5 C6 C7 -172.8(7) . . . . ? N5 C6 C7 C8 -0.5(16) . . . . ? C6 C7 C8 C9 -0.4(15) . . . . ? C6 C7 C8 C11 -177.6(9) . . . . ? C7 C8 C9 C10 1.0(15) . . . . ? C11 C8 C9 C10 178.1(9) . . . . ? C6 N5 C10 C9 -0.1(15) . . . . ? Cd1 N5 C10 C9 173.5(7) . . . . ? C8 C9 C10 N5 -0.7(16) . . . . ? C7 C8 C11 C12 170.3(10) . . . . ? C9 C8 C11 C12 -6.8(17) . . . . ? C8 C11 C12 C13 -177.6(8) . . . . ? C11 C12 C13 C18 178.1(10) . . . . ? C11 C12 C13 C14 -3.0(16) . . . . ? C18 C13 C14 C15 -1.3(14) . . . . ? C12 C13 C14 C15 179.8(9) . . . . ? C13 C14 C15 N16 1.0(15) . . . . ? C14 C15 N16 C17 0.1(14) . . . . ? C14 C15 N16 Cd1 175.0(7) . . . 1_556 ? C15 N16 C17 C18 -0.9(13) . . . . ? Cd1 N16 C17 C18 -175.5(6) 1_556 . . . ? C14 C13 C18 C17 0.6(14) . . . . ? C12 C13 C18 C17 179.5(8) . . . . ? N16 C17 C18 C13 0.5(14) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.576 _refine_diff_density_min -0.668 _refine_diff_density_rms 0.120