# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and The Centre National de la Recherche Scientifique, 2010 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Kole, Goutam' 'Cairns, Amy' 'Eddaoudi, Mohamed' 'Vittal, Jagadese' _publ_contact_author_name 'Vittal, Jagadese' _publ_contact_author_email chmjjv@nus.edu.sg _publ_section_title ; Solvent-free porous framework resulted from 3D entanglement of 1D zigzag coordination polymer ; # Attachment '- GoutamNJC.cif' data_8054 _database_code_depnum_ccdc_archive 'CCDC 770990' #TrackingRef '- GoutamNJC.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H18 N2 O4 Zn' _chemical_formula_weight 511.83 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4/ncc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y, -x, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' '-y-1/2, -x-1/2, z-1/2' 'y, x, z-1/2' _cell_length_a 16.1598(4) _cell_length_b 16.1598(4) _cell_length_c 19.3303(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5047.9(3) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 1756 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 18.36 _exptl_crystal_description BLOCK _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.347 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 1.008 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7229 _exptl_absorpt_correction_T_max 0.9107 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27022 _diffrn_reflns_av_R_equivalents 0.0862 _diffrn_reflns_av_sigmaI/netI 0.0370 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2221 _reflns_number_gt 1348 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1837P)^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 2221 _refine_ls_number_parameters 159 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1201 _refine_ls_R_factor_gt 0.0784 _refine_ls_wR_factor_ref 0.2733 _refine_ls_wR_factor_gt 0.2385 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 Zn1 Zn 0.55397(4) 0.05397(4) 0.2500 0.0531(5) Uani 1 2 d S . . N1 N 0.4464(3) 0.0228(3) 0.3029(2) 0.0530(12) Uani 1 1 d . . . O1 O 0.5152(3) 0.1600(3) 0.2130(2) 0.0752(13) Uani 1 1 d . . . O2 O 0.6150(3) 0.1274(3) 0.1419(3) 0.0799(15) Uani 1 1 d . . . C1 C 0.4106(4) -0.0462(3) 0.2786(3) 0.0476(13) Uani 1 1 d . . . C2 C 0.3377(3) -0.0802(3) 0.3037(3) 0.0519(14) Uani 1 1 d . . . C3 C 0.2988(4) -0.0348(4) 0.3574(3) 0.0671(17) Uani 1 1 d . . . H3 H 0.2491 -0.0545 0.3766 0.081 Uiso 1 1 calc R . . C4 C 0.3324(4) 0.0370(4) 0.3819(4) 0.0717(18) Uani 1 1 d . . . H4 H 0.3060 0.0678 0.4167 0.086 Uiso 1 1 calc R . . C5 C 0.4079(4) 0.0633(4) 0.3532(3) 0.0645(17) Uani 1 1 d . . . H5 H 0.4323 0.1119 0.3704 0.077 Uiso 1 1 calc R . . C6 C 0.3063(4) -0.1542(4) 0.2756(3) 0.0573(15) Uani 1 1 d . . . H6 H 0.2568 -0.1764 0.2932 0.069 Uiso 1 1 calc R . . C7 C 0.5608(4) 0.1724(4) 0.1595(3) 0.0629(17) Uani 1 1 d . . . C8 C 0.5371(4) 0.2512(3) 0.1202(3) 0.0561(15) Uani 1 1 d . . . C9 C 0.4688(4) 0.2984(4) 0.1390(3) 0.0648(17) Uani 1 1 d . . . H9 H 0.4348 0.2810 0.1757 0.078 Uiso 1 1 calc R . . C10 C 0.4512(4) 0.3691(4) 0.1050(3) 0.0703(18) Uani 1 1 d . . . H10 H 0.4044 0.3999 0.1181 0.084 Uiso 1 1 calc R . . C11 C 0.4993(4) 0.3971(4) 0.0520(3) 0.0651(18) Uani 1 1 d . . . C12 C 0.5638(5) 0.3489(4) 0.0304(4) 0.079(2) Uani 1 1 d . . . H12 H 0.5949 0.3652 -0.0084 0.095 Uiso 1 1 calc R . . C13 C 0.5839(5) 0.2759(4) 0.0649(3) 0.0739(18) Uani 1 1 d . . . H13 H 0.6293 0.2440 0.0504 0.089 Uiso 1 1 calc R . . C14 C 0.4790(6) 0.4792(5) 0.0192(4) 0.085(2) Uani 1 1 d . . . H14 H 0.4267 0.5010 0.0302 0.102 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 Zn1 0.0468(5) 0.0468(5) 0.0657(8) 0.0106(3) -0.0106(3) -0.0042(4) N1 0.050(3) 0.050(3) 0.059(3) 0.010(2) -0.010(2) -0.004(2) O1 0.097(3) 0.054(3) 0.074(3) 0.012(2) -0.015(3) -0.014(2) O2 0.082(3) 0.059(3) 0.099(4) 0.006(3) -0.008(3) 0.026(3) C1 0.045(3) 0.046(3) 0.051(3) 0.007(2) -0.009(3) 0.003(3) C2 0.047(3) 0.054(3) 0.055(3) 0.006(3) -0.006(3) -0.002(3) C3 0.054(4) 0.075(4) 0.071(4) 0.004(3) 0.002(3) -0.002(3) C4 0.070(5) 0.068(4) 0.077(4) -0.007(3) 0.007(4) -0.003(3) C5 0.069(4) 0.055(4) 0.070(4) -0.004(3) -0.003(3) -0.004(3) C6 0.053(3) 0.055(4) 0.064(4) 0.007(3) -0.007(3) -0.006(3) C7 0.075(5) 0.056(4) 0.058(4) -0.002(3) -0.023(3) -0.010(3) C8 0.075(4) 0.038(3) 0.056(3) -0.001(3) -0.024(3) -0.001(3) C9 0.082(4) 0.057(4) 0.056(3) 0.006(3) -0.005(3) -0.007(3) C10 0.083(5) 0.063(4) 0.065(4) 0.001(3) -0.002(4) 0.016(3) C11 0.095(5) 0.039(3) 0.062(4) -0.006(3) -0.026(4) 0.011(3) C12 0.106(6) 0.067(5) 0.065(4) 0.011(4) 0.008(4) -0.017(4) C13 0.082(5) 0.060(4) 0.079(4) 0.008(3) 0.010(4) 0.011(3) C14 0.109(7) 0.073(5) 0.075(5) 0.007(4) -0.019(4) -0.007(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 Zn1 O1 1.960(4) . ? Zn1 O1 1.960(4) 7_545 ? Zn1 N1 2.079(5) 7_545 ? Zn1 N1 2.079(5) . ? Zn1 C7 2.595(7) 7_545 ? Zn1 C7 2.595(7) . ? N1 C5 1.326(7) . ? N1 C1 1.342(7) . ? O1 C7 1.286(8) . ? O2 C7 1.188(7) . ? C1 C2 1.388(8) . ? C1 C1 1.480(13) 7_545 ? C2 C6 1.408(7) . ? C2 C3 1.419(8) . ? C3 C4 1.365(9) . ? C4 C5 1.406(9) . ? C6 C6 1.339(11) 7_545 ? C7 C8 1.532(8) . ? C8 C13 1.369(9) . ? C8 C9 1.390(9) . ? C9 C10 1.349(8) . ? C10 C11 1.363(9) . ? C11 C12 1.366(9) . ? C11 C14 1.506(10) . ? C12 C13 1.395(9) . ? C14 C14 1.211(14) 9_665 ? 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 Zn1 O1 133.8(3) . 7_545 ? O1 Zn1 N1 118.33(18) . 7_545 ? O1 Zn1 N1 97.10(19) 7_545 7_545 ? O1 Zn1 N1 97.09(19) . . ? O1 Zn1 N1 118.33(18) 7_545 . ? N1 Zn1 N1 80.6(3) 7_545 . ? O1 Zn1 C7 116.4(2) . 7_545 ? O1 Zn1 C7 28.7(2) 7_545 7_545 ? N1 Zn1 C7 123.1(2) 7_545 7_545 ? N1 Zn1 C7 107.20(18) . 7_545 ? O1 Zn1 C7 28.7(2) . . ? O1 Zn1 C7 116.4(2) 7_545 . ? N1 Zn1 C7 107.20(18) 7_545 . ? N1 Zn1 C7 123.1(2) . . ? C7 Zn1 C7 113.1(3) 7_545 . ? C5 N1 C1 117.7(5) . . ? C5 N1 Zn1 129.2(4) . . ? C1 N1 Zn1 112.9(4) . . ? C7 O1 Zn1 104.2(4) . . ? N1 C1 C2 124.9(6) . . ? N1 C1 C1 116.8(3) . 7_545 ? C2 C1 C1 118.3(3) . 7_545 ? C1 C2 C6 120.5(5) . . ? C1 C2 C3 115.3(5) . . ? C6 C2 C3 124.2(5) . . ? C4 C3 C2 121.1(6) . . ? C3 C4 C5 117.7(6) . . ? N1 C5 C4 123.1(6) . . ? C6 C6 C2 121.2(3) 7_545 . ? O2 C7 O1 123.9(6) . . ? O2 C7 C8 123.5(7) . . ? O1 C7 C8 112.6(6) . . ? O2 C7 Zn1 76.9(4) . . ? O1 C7 Zn1 47.1(3) . . ? C8 C7 Zn1 159.5(5) . . ? C13 C8 C9 118.9(6) . . ? C13 C8 C7 119.4(6) . . ? C9 C8 C7 121.7(6) . . ? C10 C9 C8 120.3(6) . . ? C9 C10 C11 121.8(6) . . ? C10 C11 C12 118.5(6) . . ? C10 C11 C14 118.9(6) . . ? C12 C11 C14 122.6(7) . . ? C11 C12 C13 120.9(6) . . ? C8 C13 C12 119.4(6) . . ? C14 C14 C11 128.8(12) 9_665 . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.954 _refine_diff_density_min -0.323 _refine_diff_density_rms 0.136