Supplementary Material (ESI) for Chemical Communications This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Hong-Cai Zhou' _publ_contact_author_email ZHOU@MAIL.CHEM.TAMU.EDU _publ_section_title ; A NbO-type metal-organic framework derived from a polyne-coupled di-isophthalate linker formed in situ ; loop_ _publ_author_name 'Hong-Cai Zhou' 'Andrey Yakovenko' 'Daqiang Yuan' 'Dan Zhao' # Attachment 'PCN-46.cif' data_PCN-46 _database_code_depnum_ccdc_archive 'CCDC 747535' #TrackingRef 'PCN-46.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H5 Cu O5' _chemical_formula_sum 'C10 H5 Cu O5' _chemical_formula_weight 268.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0015 0.0009 '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 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3240 0.8257 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R-3m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x-y, -y, -z' '-x, -x+y, -z' 'y, x, -z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x-y+2/3, -y+1/3, -z+1/3' '-x+2/3, -x+y+1/3, -z+1/3' 'y+2/3, x+1/3, -z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'x-y+1/3, -y+2/3, -z+2/3' '-x+1/3, -x+y+2/3, -z+2/3' 'y+1/3, x+2/3, -z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+y, y, z' 'x, x-y, z' '-y, -x, z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+y+2/3, y+1/3, z+1/3' 'x+2/3, x-y+1/3, z+1/3' '-y+2/3, -x+1/3, z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-x+y+1/3, y+2/3, z+2/3' 'x+1/3, x-y+2/3, z+2/3' '-y+1/3, -x+2/3, z+2/3' _cell_length_a 18.2386(8) _cell_length_b 18.2386(8) _cell_length_c 42.049(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 12113.4(9) _cell_formula_units_Z 18 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9937 _cell_measurement_theta_min 2.2495 _cell_measurement_theta_max 13.6815 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 0.663 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2412 _exptl_absorpt_coefficient_mu 0.428 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9545 _exptl_absorpt_correction_T_max 0.9707 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.41328 _diffrn_radiation_type synchrotron _diffrn_radiation_source 15ID-B _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 68838 _diffrn_reflns_av_R_equivalents 0.1069 _diffrn_reflns_av_sigmaI/netI 0.0426 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -49 _diffrn_reflns_limit_l_max 52 _diffrn_reflns_theta_min 0.94 _diffrn_reflns_theta_max 14.98 _reflns_number_total 3022 _reflns_number_gt 2201 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement 'SAINT+ ver. (Bruker, 2001)' _computing_data_reduction 'SAINT+ ver. (Bruker, 2001)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.1265P)^2^+16.1557P] 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 3022 _refine_ls_number_parameters 82 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0975 _refine_ls_R_factor_gt 0.0747 _refine_ls_wR_factor_ref 0.2162 _refine_ls_wR_factor_gt 0.2042 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 _platon_squeeze_void_content 1 -0.051 -0.035 -0.003 8810 2188 ' ' _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 Cu1 Cu 0.05195(3) 0.525974(17) 0.025335(14) 0.0562(3) Uani 1 2 d S . . O1 O 0.02417(18) 0.58659(19) -0.04296(7) 0.0755(8) Uani 1 1 d . . . O2 O 0.10785(17) 0.62942(19) 0.00027(7) 0.0745(8) Uani 1 1 d . . . O3 O 0.1425(2) 0.57123(12) 0.06300(10) 0.0810(12) Uani 1 2 d S . . H3A H 0.1963 0.5981 0.0632 0.097 Uiso 1 2 d SR . . H3B H 0.1216 0.5608 0.0816 0.097 Uiso 1 2 d SR . . C1 C 0.0883(3) 0.6387(3) -0.02739(11) 0.0717(11) Uani 1 1 d . . . C2 C 0.2215(2) 0.7785(2) -0.02892(14) 0.0695(15) Uani 1 2 d S . . H2 H 0.2318 0.7682 -0.0077 0.083 Uiso 1 2 calc SR . . C3 C 0.1488(3) 0.7202(3) -0.04386(10) 0.0771(12) Uani 1 1 d . . . C4 C 0.1346(3) 0.7348(4) -0.07467(12) 0.107(2) Uani 1 1 d . . . H4 H 0.0842 0.6943 -0.0851 0.129 Uiso 1 1 calc R . . C5 C 0.1923(3) 0.8077(3) -0.0912(2) 0.120(4) Uani 1 2 d S . . C6 C 0.1801(5) 0.8199(5) -0.1231(2) 0.158(5) Uani 1 2 d S . . C7 C 0.1724(6) 0.8276(6) -0.1513(3) 0.158(5) Uani 1 2 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 Cu1 0.0409(4) 0.0720(4) 0.0454(4) -0.00301(12) -0.0060(2) 0.02043(19) O1 0.0614(15) 0.0738(18) 0.0605(17) 0.0074(14) -0.0125(13) 0.0108(14) O2 0.0636(16) 0.0778(19) 0.0589(17) 0.0086(14) -0.0093(13) 0.0179(14) O3 0.056(2) 0.107(3) 0.064(2) -0.0097(9) -0.0193(18) 0.0280(11) C1 0.061(2) 0.071(3) 0.068(3) 0.004(2) 0.002(2) 0.021(2) C2 0.066(2) 0.066(2) 0.061(3) 0.0050(15) -0.0050(15) 0.021(3) C3 0.068(2) 0.079(3) 0.057(2) 0.008(2) -0.0078(19) 0.017(2) C4 0.084(3) 0.104(4) 0.076(3) 0.018(3) -0.020(3) 0.004(3) C5 0.113(4) 0.113(4) 0.074(5) 0.030(3) -0.030(3) 0.011(5) C6 0.129(5) 0.129(5) 0.101(7) 0.041(4) -0.041(4) -0.023(6) C7 0.142(5) 0.142(5) 0.092(6) 0.045(4) -0.045(4) -0.004(7) _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 Cu1 O2 1.946(3) . ? Cu1 O1 1.960(3) 5 ? Cu1 O3 2.133(4) . ? O1 C1 1.261(5) . ? O2 C1 1.252(5) . ? O3 H3A 0.8501 . ? O3 H3B 0.8499 . ? C1 C3 1.505(6) . ? C2 C3 1.369(5) . ? C2 C3 1.369(5) 24_665 ? C2 H2 0.9500 . ? C3 C4 1.373(7) . ? C4 C5 1.399(7) . ? C4 H4 0.9500 . ? C5 C6 1.396(12) . ? C5 C4 1.399(7) 24_665 ? C6 C7 1.210(13) . ? C7 C7 1.345(18) 31_564 ? 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 Cu1 O2 90.08(19) 23_565 . ? O2 Cu1 O1 89.58(14) 23_565 19_565 ? O2 Cu1 O1 166.85(11) . 19_565 ? O2 Cu1 O1 166.85(11) 23_565 5 ? O2 Cu1 O1 89.57(14) . 5 ? O1 Cu1 O1 87.8(2) 19_565 5 ? O2 Cu1 O3 95.63(12) 23_565 . ? O2 Cu1 O3 95.63(12) . . ? O1 Cu1 O3 97.48(11) 19_565 . ? O1 Cu1 O3 97.48(11) 5 . ? O2 Cu1 Cu1 81.24(8) 23_565 19_565 ? O2 Cu1 Cu1 81.24(8) . 19_565 ? O1 Cu1 Cu1 85.72(8) 19_565 19_565 ? O1 Cu1 Cu1 85.72(8) 5 19_565 ? O3 Cu1 Cu1 175.54(12) . 19_565 ? C1 O1 Cu1 119.8(3) . 19_565 ? C1 O2 Cu1 126.0(3) . . ? Cu1 O3 H3A 132.7 . . ? Cu1 O3 H3B 115.1 . . ? H3A O3 H3B 112.2 . . ? O2 C1 O1 126.9(4) . . ? O2 C1 C3 116.3(4) . . ? O1 C1 C3 116.8(4) . . ? C3 C2 C3 121.6(6) . 24_665 ? C3 C2 H2 119.2 . . ? C3 C2 H2 119.2 24_665 . ? C2 C3 C4 119.1(4) . . ? C2 C3 C1 120.2(4) . . ? C4 C3 C1 120.6(4) . . ? C3 C4 C5 121.8(5) . . ? C3 C4 H4 119.1 . . ? C5 C4 H4 119.1 . . ? C6 C5 C4 121.6(3) . . ? C6 C5 C4 121.6(3) . 24_665 ? C4 C5 C4 116.7(7) . 24_665 ? C7 C6 C5 176(2) . . ? C6 C7 C7 176(3) . 31_564 ? 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 O2 Cu1 O2 C1 76.0(4) 23_565 . . . ? O1 Cu1 O2 C1 -12.5(8) 19_565 . . . ? O1 Cu1 O2 C1 -90.9(4) 5 . . . ? O3 Cu1 O2 C1 171.7(4) . . . . ? Cu1 Cu1 O2 C1 -5.1(4) 19_565 . . . ? Cu1 O2 C1 O1 8.1(7) . . . . ? Cu1 O2 C1 C3 -170.9(3) . . . . ? Cu1 O1 C1 O2 -5.3(7) 19_565 . . . ? Cu1 O1 C1 C3 173.6(3) 19_565 . . . ? C3 C2 C3 C4 0.7(11) 24_665 . . . ? C3 C2 C3 C1 176.7(4) 24_665 . . . ? O2 C1 C3 C2 1.5(7) . . . . ? O1 C1 C3 C2 -177.5(5) . . . . ? O2 C1 C3 C4 177.4(5) . . . . ? O1 C1 C3 C4 -1.6(8) . . . . ? C2 C3 C4 C5 -0.2(12) . . . . ? C1 C3 C4 C5 -176.1(7) . . . . ? C3 C4 C5 C6 176.1(10) . . . . ? C3 C4 C5 C4 -0.3(16) . . . 24_665 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 14.98 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.037 _refine_diff_density_min -0.300 _refine_diff_density_rms 0.083 _publ_section_references ; Bruker (2001). SAINTP+ for NT. Data Reduction and Correction Program v. 6.2, Bruker AXS, Madison, Wisconsin, USA. Bruker (2005). APEX2 software package. Bruker Molecular Analysis Research Tool, v. 2008.4 Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (2008). SADABS-2008/1, Bruker/Siemens Area Detector Absorption Correction Program, Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (2008). SHELXTL 2008/4, Structure Determination Software Suite, Bruker AXS, Madison, Wisconsin, USA. ; # start Validation Reply Form _vrf_PLAT432_PCN-46 ; PROBLEM: Short Inter X...Y Contact C2 .. C3 .. 1.37 Ang. RESPONSE: The Molecule of 5,5'-(buta-1,3-diyne-1,4-diyl)diisophtalate is located on special position; hence all these short inter X...Y contacts are correspond to bonds between atoms in one molecule. ; # end Validation Reply Form