#------------------------------------------------------------------------------ #$Date: 2016-03-26 02:02:50 +0200 (Sat, 26 Mar 2016) $ #$Revision: 180120 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/10/18/7101841.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7101841 loop_ _publ_author_name 'Hawxwell, Samuel M' 'Espallargas, Guillermo M\'inguez' 'Bradshaw, Darren' 'Rosseinsky, Matthew J' 'Prior, Timothy J' 'Florence, Alastair J' 'van de Streek, Jacco' 'Brammer, Lee' _publ_section_title ; Ligand flexibility and framework rearrangement in a new family of porous metal-organic frameworks. ; _journal_issue 15 _journal_name_full 'Chemical communications (Cambridge, England)' _journal_page_first 1532 _journal_page_last 1534 _journal_paper_doi 10.1039/b618796j _journal_year 2007 _chemical_compound_source 'see text' _chemical_formula_moiety 'C20 H20 O10 Zn2, 4O' _chemical_formula_sum 'C20 H20 O14 Zn2' _chemical_formula_weight 303.54 _chemical_name_systematic ? _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _cell_angle_alpha 91.891(4) _cell_angle_beta 107.086(3) _cell_angle_gamma 100.815(4) _cell_formula_units_Z 1 _cell_length_a 9.5471(7) _cell_length_b 7.8520(7) _cell_length_c 8.4756(6) _cell_measurement_reflns_used 18 _cell_measurement_temperature 298 _cell_volume 593.90(8) _computing_cell_refinement 'TOPAS (Coelho, 2003)' _computing_data_collection 'DIFFRAC plus XRD Commander (Kienle & Jacob, 2003)' _computing_data_reduction 'DASH (David et al., 2001)' _computing_molecular_graphics 'Mercury (Macrae et al., 2006)' _computing_publication_material 'enCifer (Cambridge Crystallographic Data Centre, 2004)' _computing_structure_refinement 'TOPAS (Coelho, 2003)' _computing_structure_solution 'DASH (David et al., 2001)' _diffrn_ambient_temperature 298 _diffrn_detector Bruker-Vantec _diffrn_detector_type 'Solid state detector' _diffrn_measurement_device_type 'Bruker AXS D8 Advance' _diffrn_radiation_monochromator 'primary focussing, Ge 111' _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a~1~' _diffrn_radiation_wavelength 1.54056 _diffrn_source 'sealed X-ray tube' _diffrn_source_target Cu _diffrn_source_type 'Bruker-AXS D8' _exptl_absorpt_coefficient_mu 3.139 _exptl_absorpt_correction_type none _exptl_crystal_density_diffrn 1.697 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 304 _pd_char_colour white _pd_instr_location 'Solid-State Research Group, University of Strathclyde, Glasgow, U.K.' _pd_meas_2theta_range_inc 0.017 _pd_meas_2theta_range_max 65.0 _pd_meas_2theta_range_min 3.0 _pd_meas_number_of_points 3647 _pd_meas_scan_method step _pd_prep_temperature 298 _pd_proc_ls_background_function ; Chebyshev polynomial ; _pd_proc_ls_pref_orient_corr ; A spherical harmonics-based preferred orientation correction (J\"arvinen, 1993) was applied with Topas during the Rietveld refinement. ; _pd_proc_ls_profile_function ; Fundamental parameters with axial divergence correction. ; _pd_proc_ls_prof_R_factor 0.0478 _pd_proc_ls_prof_wR_expected 0.0164 _pd_proc_ls_prof_wR_factor 0.0630 _pd_spec_mounting '1.0 mm borosilicate capillary' _pd_spec_mount_mode transmission _pd_spec_shape cylinder _pd_spec_size_axial 12 _pd_spec_size_equat 1.0 _pd_spec_size_thick 1.0 _refine_diff_density_max 0.2 _refine_diff_density_min -0.2 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 3.853 _refine_ls_hydrogen_treatment refxyz _refine_ls_matrix_type sparse _refine_ls_number_constraints 1 _refine_ls_number_parameters 95 _refine_ls_number_restraints 57 _refine_ls_R_I_factor 1.585 _refine_ls_shift/su_max 0.001 _refine_ls_weighting_details 1/\s(Y~obs~)^2^ _refine_ls_weighting_scheme sigma _cod_data_source_file b618796j.txt _cod_data_source_block sh541 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_exptl_absorpt_correction_type' value ' none' changed to 'none' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 7101841 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv Zn1 Zn Uiso 0.3952(6) 0.4919(7) 0.1632(7) 1.000 0.0435 O1 O Uiso -0.2094(5) -0.43347(13) 0.7960(4) 1.000 0.0442 O2 O Uiso -0.330(4) -0.34129(12) 0.5599(5) 1.000 0.0442 O3 O Uiso 0.108(3) -0.1279(3) 0.3019(3) 1.000 0.0442 O4 O Uiso 0.4649(3) -0.34968(11) 0.7870(5) 1.000 0.0442 O5 O Uiso 0.3264(5) -0.4594(11) 0.9432(4) 1.000 0.0442 O6 O Uiso 0.51439(2) 0.7154(3) 0.2859(3) 1.000 0.0577 O7 O Uiso 0.6038(2) -0.00711(3) 0.7238(2) 1.000 0.0577 C1 C Uiso 0.08960(19) -0.21208(19) 0.4437(2) 1.000 0.0442 C2 C Uiso -0.05027(19) -0.25044(19) 0.47438(19) 1.000 0.0442 C3 C Uiso -0.06258(19) -0.33421(17) 0.6165(2) 1.000 0.0442 C4 C Uiso 0.06596(19) -0.37852(19) 0.72645(17) 1.000 0.0442 C5 C Uiso 0.20346(19) -0.3404(2) 0.6958(19) 1.000 0.0442 C6 C Uiso 0.21519(18) -0.25764(17) 0.5555(2) 1.000 0.0442 C7 C Uiso -0.0310(2) -0.1068(2) 0.1872(2) 1.000 0.0442 C8 C Uiso 0.0023(3) 0.0264(2) 0.0746(2) 1.000 0.0442 C9 C Uiso -0.2081(2) -0.3775(3) 0.6544(2) 1.000 0.0442 C10 C Uiso 0.3362(2) -0.3872(3) 0.8114(2) 1.000 0.0442 H2 H Uiso -0.14189(10) -0.21911(13) 0.39522(13) 1.000 0.0887 H4 H Uiso 0.06047(11) -0.43719(15) 0.82772(12) 1.000 0.0887 H6 H Uiso 0.31519(11) -0.23094(14) 0.53548(14) 1.000 0.0887 H7A H Uiso -0.08433(11) -0.22037(13) 0.1200(12) 1.000 0.0887 H7B H Uiso -0.0974(10) -0.0671(13) 0.2465(12) 1.000 0.0887 H8 H Uiso 0.01280(12) 0.1537(13) 0.10577(12) 1.000 0.0887 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Zn Zn 0.2839 1.4301 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 O5 Zn1 O6 105.2(4) 1_564 . yes O1 Zn1 O6 111.5(3) 2_556 . yes O4 Zn1 O6 101.6(3) 2_656 . yes O1 Zn1 O5 98.6(3) 2_556 1_564 yes O4 Zn1 O5 117.2(4) 2_656 1_564 yes O1 Zn1 O4 122.1(3) 2_556 2_656 yes Zn1 O1 C9 117.9(3) 2_556 . yes C1 O3 C7 113.3(18) . . yes Zn1 O4 C10 123.6(2) 2_656 . yes Zn1 O5 C10 155.5(5) 1_546 . yes O3 C1 C2 122.1(11) . . yes O3 C1 C6 118.6(11) . . yes C2 C1 C6 119.39(15) . . no C1 C2 C3 119.84(16) . . no C2 C3 C4 119.36(16) . . no C2 C3 C9 121.84(16) . . no C4 C3 C9 118.79(14) . . no C3 C4 C5 120.6(5) . . no C4 C5 C6 119.9(7) . . no C4 C5 C10 120.0(9) . . no C6 C5 C10 120.2(4) . . no C1 C6 C5 120.9(3) . . no O3 C7 C8 108.7(6) . . yes C7 C8 C8 118.54(14) . 2_555 no O1 C9 O2 117.9(12) . . yes O1 C9 C3 119.2(3) . . yes O2 C9 C3 122.3(11) . . yes O4 C10 O5 118.9(3) . . yes O4 C10 C5 120.9(4) . . yes O5 C10 C5 120.2(5) . . yes C1 C2 H2 120.53(16) . . no C3 C2 H2 119.63(18) . . no C3 C4 H4 120.99(19) . . no C5 C4 H4 118.4(6) . . no C1 C6 H6 120.26(16) . . no C5 C6 H6 118.8(3) . . no O3 C7 H7A 109.6(4) . . no O3 C7 H7B 111.3(9) . . no C8 C7 H7A 109.4(5) . . no C8 C7 H7B 108.8(6) . . no H7A C7 H7B 109.1(6) . . no C7 C8 H8 121.0(3) . . no C8 C8 H8 119.8(2) 2_555 . no 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 O6 1.973(6) . yes Zn1 O5 1.864(7) 1_564 yes Zn1 O1 1.882(8) 2_556 yes Zn1 O4 1.862(6) 2_656 yes O1 C9 1.294(4) . yes O2 C9 1.29(3) . yes O3 C1 1.430(9) . yes O3 C7 1.44(2) . yes O4 C10 1.287(4) . yes O5 C10 1.289(6) . yes C1 C2 1.414(3) . no C1 C6 1.407(2) . no C2 C3 1.416(2) . no C3 C4 1.416(2) . no C3 C9 1.497(3) . no C4 C5 1.392(6) . no C5 C6 1.397(13) . no C5 C10 1.473(10) . no C7 C8 1.492(2) . no C8 C8 1.303(3) 2_555 no C2 H2 1.011(2) . no C4 H4 0.9976(18) . no C6 H6 1.003(2) . no C7 H7A 1.002(6) . no C7 H7B 1.001(10) . no C8 H8 1.004(10) . no 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_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Zn1 O5 C10 39.8(14) . 1_564 1_564 no O6 Zn1 O1 C9 -74.9(3) . 2_556 2_556 no O6 Zn1 O4 C10 -54.3(4) . 2_656 2_656 no Zn1 O1 C9 O2 9.8(3) 2_556 . . no Zn1 O1 C9 C3 -178.5(2) 2_556 . . no C7 O3 C1 C2 -7.0(5) . . . no C7 O3 C1 C6 173.0(3) . . . no C1 O3 C7 C8 162.9(3) . . . no Zn1 O4 C10 O5 38.8(6) 2_656 . . no Zn1 O4 C10 C5 -144.4(5) 2_656 . . no Zn1 O5 C10 O4 29.4(15) 1_546 . . no Zn1 O5 C10 C5 -147.4(12) 1_546 . . no O3 C1 C2 C3 179.9(2) . . . no C6 C1 C2 C3 -0.1(2) . . . no O3 C1 C6 C5 -179.9(4) . . . no C2 C1 C6 C5 0.2(4) . . . no C1 C2 C3 C4 0.0(2) . . . no C1 C2 C3 C9 180.00(17) . . . no C2 C3 C4 C5 0.0(4) . . . no C9 C3 C4 C5 -179.9(4) . . . no C2 C3 C9 O1 -171.21(17) . . . no C2 C3 C9 O2 0.1(4) . . . no C4 C3 C9 O1 8.7(3) . . . no C4 C3 C9 O2 -179.9(3) . . . no C3 C4 C5 C6 0.0(8) . . . no C3 C4 C5 C10 180.0(4) . . . no C4 C5 C6 C1 -0.1(8) . . . no C10 C5 C6 C1 180.0(4) . . . no C4 C5 C10 O4 -178.5(4) . . . no C4 C5 C10 O5 -1.8(9) . . . no C6 C5 C10 O4 1.4(8) . . . no C6 C5 C10 O5 178.2(6) . . . no O3 C7 C8 C8 101.8(5) . . 2_555 no C7 C8 C8 C7 180.0(2) . 2_555 2_555 no