# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Shengqian Ma' _publ_contact_author_email SMA@ANL.GOV _publ_section_title ; A Nanotubular Metal-Organic Framework with Permanent Porosity: Structure Analysis and Gas Sorption Studies ; loop_ _publ_author_name 'Shengqian Ma' 'Jian-Rong Li' 'Di-Jia Liu' 'Jason M Simmons' 'Wei Weng' 'Daqiang Yuan' 'Hong-Cai Zhou' # Attachment 'PCN-19-revision2.cif' data_sq _database_code_depnum_ccdc_archive 'CCDC 724592' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common PCN-19 _chemical_melting_point 'not measured' _chemical_formula_moiety 'Ni3O (O)3 (C16H8O4)3' _chemical_formula_sum 'C48 H24 Ni3 O16' _chemical_formula_weight 1032.74 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M P-31c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 15.5510(3) _cell_length_b 15.5510(3) _cell_length_c 16.3640(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3427.18(14) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.007 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1060 _exptl_absorpt_coefficient_mu 0.864 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.902 _exptl_absorpt_correction_T_max 0.9581 _exptl_absorpt_process_details none _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(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_reflns_number 10131 _diffrn_reflns_av_R_equivalents 0.0964 _diffrn_reflns_av_sigmaI/netI 0.0947 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2631 _reflns_number_gt 1462 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0862P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2626 _refine_ls_number_parameters 101 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1018 _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.1470 _refine_ls_wR_factor_gt 0.1361 _refine_ls_goodness_of_fit_ref 0.902 _refine_ls_restrained_S_all 0.902 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 # SQUEEZE RESULTS loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 -0.006 1648.0 425.0 2 0.333 0.667 0.250 17.2 -1.9 3 0.667 0.333 0.750 17.2 -1.7 _platon_squeeze_details ; ; 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 Ni1 Ni 0.5200 0.2600 0.2500 0.0255(2) Uani 1 2 d S . . O2 O 0.6667 0.3333 0.2500 0.0157(11) Uani 1 6 d S . . O3 O 0.64142(17) 0.15041(16) 0.17434(13) 0.0312(6) Uani 1 1 d . . . O4 O 0.51918(18) 0.18367(17) 0.14853(14) 0.0352(6) Uani 1 1 d . . . O5 O 0.3660 0.1830 0.2500 0.0667(12) Uani 1 2 d S . . C6 C 0.5337(2) 0.0684(2) 0.06512(19) 0.0276(8) Uani 1 1 d . . . C7 C 0.5687(3) 0.1418(3) 0.13614(19) 0.0275(8) Uani 1 1 d . . . C8 C 0.4534(3) -0.0268(3) 0.0765(2) 0.0331(9) Uani 1 1 d . . . C9 C 0.5814(3) 0.0965(2) -0.01050(19) 0.0311(8) Uani 1 1 d . . . C10 C 0.6660(3) 0.1935(3) -0.0241(2) 0.0428(10) Uani 1 1 d . . . H10 H 0.6918 0.2396 0.0197 0.051 Uiso 1 1 calc R . . C11 C 0.4040(3) -0.0584(3) 0.1538(2) 0.0561(12) Uani 1 1 d . . . H11 H 0.4265 -0.0133 0.1985 0.067 Uiso 1 1 calc R . . C12 C 0.7093(4) 0.2199(3) -0.0984(3) 0.0663(14) Uani 1 1 d . . . H12 H 0.7637 0.2849 -0.1069 0.080 Uiso 1 1 calc R . . C13 C 0.3266(4) -0.1503(4) 0.1643(3) 0.0792(17) Uani 1 1 d . . . H13 H 0.2954 -0.1694 0.2163 0.095 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 Ni1 0.0270(4) 0.0266(3) 0.0231(4) -0.0003(2) 0.000 0.01350(19) O2 0.0156(16) 0.0156(16) 0.016(3) 0.000 0.000 0.0078(8) O3 0.0355(14) 0.0266(13) 0.0285(13) -0.0062(10) -0.0019(11) 0.0134(11) O4 0.0461(15) 0.0336(14) 0.0275(13) -0.0064(10) -0.0079(11) 0.0210(13) O5 0.036(2) 0.056(2) 0.102(3) 0.010(2) 0.000 0.0181(12) C6 0.0305(19) 0.0284(19) 0.0232(18) -0.0042(14) -0.0020(14) 0.0142(17) C7 0.035(2) 0.030(2) 0.0176(17) 0.0029(14) 0.0009(15) 0.0163(18) C8 0.038(2) 0.030(2) 0.027(2) -0.0041(15) -0.0026(16) 0.0142(18) C9 0.040(2) 0.0260(19) 0.0244(18) -0.0035(15) -0.0009(16) 0.0142(17) C10 0.044(2) 0.037(2) 0.032(2) -0.0062(17) 0.0030(17) 0.0092(19) C11 0.062(3) 0.036(2) 0.028(2) -0.0065(17) 0.0152(19) -0.007(2) C12 0.074(3) 0.039(2) 0.045(3) -0.005(2) 0.022(2) -0.003(2) C13 0.088(4) 0.061(3) 0.028(2) -0.006(2) 0.021(2) -0.008(3) _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 Ni1 O2 1.9753 . ? Ni1 O4 2.037(2) 6 ? Ni1 O4 2.037(2) . ? Ni1 O3 2.043(2) 5_655 ? Ni1 O3 2.043(2) 3_665 ? Ni1 O5 2.0740 . ? O2 Ni1 1.9751 2_655 ? O2 Ni1 1.9752 3_665 ? O3 C7 1.239(4) . ? O3 Ni1 2.043(2) 2_655 ? O4 C7 1.249(4) . ? C6 C8 1.391(5) . ? C6 C9 1.396(4) . ? C6 C7 1.526(4) . ? C8 C9 1.431(5) 7_655 ? C8 C11 1.434(5) . ? C9 C8 1.431(5) 7_655 ? C9 C10 1.439(5) . ? C10 C12 1.350(5) . ? C10 H10 0.9500 . ? C11 C13 1.342(6) . ? C11 H11 0.9500 . ? C12 C13 1.429(6) 7_655 ? C12 H12 0.9500 . ? C13 C12 1.428(6) 7_655 ? C13 H13 0.9500 . ? 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 O2 Ni1 O4 90.31(7) . 6 ? O2 Ni1 O4 90.31(7) . . ? O4 Ni1 O4 179.38(14) 6 . ? O2 Ni1 O3 94.16(6) . 5_655 ? O4 Ni1 O3 87.98(9) 6 5_655 ? O4 Ni1 O3 91.98(9) . 5_655 ? O2 Ni1 O3 94.17(6) . 3_665 ? O4 Ni1 O3 91.98(9) 6 3_665 ? O4 Ni1 O3 87.98(9) . 3_665 ? O3 Ni1 O3 171.67(13) 5_655 3_665 ? O2 Ni1 O5 180.0 . . ? O4 Ni1 O5 89.69(7) 6 . ? O4 Ni1 O5 89.69(7) . . ? O3 Ni1 O5 85.83(6) 5_655 . ? O3 Ni1 O5 85.83(6) 3_665 . ? Ni1 O2 Ni1 120.0 2_655 3_665 ? Ni1 O2 Ni1 120.0 2_655 . ? Ni1 O2 Ni1 120.0 3_665 . ? C7 O3 Ni1 131.2(2) . 2_655 ? C7 O4 Ni1 127.6(2) . . ? C8 C6 C9 120.4(3) . . ? C8 C6 C7 119.3(3) . . ? C9 C6 C7 120.4(3) . . ? O3 C7 O4 129.0(3) . . ? O3 C7 C6 115.5(3) . . ? O4 C7 C6 115.5(3) . . ? C6 C8 C9 120.2(3) . 7_655 ? C6 C8 C11 121.7(3) . . ? C9 C8 C11 118.1(3) 7_655 . ? C6 C9 C8 119.4(3) . 7_655 ? C6 C9 C10 122.0(3) . . ? C8 C9 C10 118.6(3) 7_655 . ? C12 C10 C9 120.9(3) . . ? C12 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C13 C11 C8 121.3(4) . . ? C13 C11 H11 119.3 . . ? C8 C11 H11 119.3 . . ? C10 C12 C13 120.2(4) . 7_655 ? C10 C12 H12 119.9 . . ? C13 C12 H12 119.9 7_655 . ? C11 C13 C12 120.8(4) . 7_655 ? C11 C13 H13 119.6 . . ? C12 C13 H13 119.6 7_655 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.244 _refine_diff_density_min -0.317 _refine_diff_density_rms 0.092