#------------------------------------------------------------------------------ #$Date: 2008-06-25 12:31:45 +0300 (Wed, 25 Jun 2008) $ #$Revision: 403 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/7101839.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_7101839 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_year 2007 _chemical_formula_moiety 'C20 H22 O14 Zn2, H2 O, H2 O' _chemical_formula_sum 'C20 H26 O16 Zn2' _chemical_formula_weight 326.57 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 68.56(3) _cell_angle_beta 79.47(3) _cell_angle_gamma 86.62(3) _cell_formula_units_Z 1 _cell_length_a 7.6916(15) _cell_length_b 8.5113(17) _cell_length_c 9.827(2) _cell_measurement_reflns_used 1727 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 64.361 _cell_measurement_theta_min 7.623 _cell_volume 588.7(2) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.906 _diffrn_measured_fraction_theta_max 0.906 _diffrn_measurement_device_type 'Bruker SMART CCD area detector' _diffrn_measurement_method 'fine slice \w' _diffrn_radiation_monochromator silicon(111) _diffrn_radiation_source 'SRS station 16.2smx' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.84600 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0673 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 4270 _diffrn_reflns_theta_full 32.87 _diffrn_reflns_theta_max 32.87 _diffrn_reflns_theta_min 3.81 _exptl_absorpt_coefficient_mu 2.121 _exptl_absorpt_correction_T_max 0.8833 _exptl_absorpt_correction_T_min 0.8833 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.842 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 334 _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _refine_diff_density_max 1.081 _refine_diff_density_min -1.163 _refine_diff_density_rms 0.140 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 172 _refine_ls_number_reflns 2358 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.059 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0460 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0632P)^2^+1.1991P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1241 _refine_ls_wR_factor_ref 0.1268 _reflns_number_gt 2152 _reflns_number_total 2358 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file b618796j.txt _[local]_cod_data_source_block dl102m _[local]_cod_cif_authors_sg_H-M P-1 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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 Zn1 Zn 0.47070(5) 0.34872(5) 1.38422(4) 0.00737(17) Uani 1 1 d . O1 O 0.2979(4) 0.1145(3) 1.3653(3) 0.0144(6) Uani 1 1 d . O2 O 0.4360(4) 0.3392(3) 1.1914(3) 0.0111(6) Uani 1 1 d . O3 O 0.1651(3) -0.2399(3) 1.0868(3) 0.0081(5) Uani 1 1 d . O4 O 0.3785(4) 0.2384(3) 0.5984(3) 0.0117(6) Uani 1 1 d . O5 O 0.3559(3) 0.4659(3) 0.6614(3) 0.0091(5) Uani 1 1 d . C1 C 0.3535(5) 0.2003(5) 1.2305(4) 0.0088(7) Uani 1 1 d . C2 C 0.3552(5) 0.3090(5) 0.6922(4) 0.0077(7) Uani 1 1 d . C3 C 0.3188(5) 0.1420(4) 1.1118(4) 0.0061(7) Uani 1 1 d . C4 C 0.3524(4) 0.2511(4) 0.9626(4) 0.0057(7) Uani 1 1 d . H4 H 0.3966 0.3621 0.9365 0.007 Uiso 1 1 calc R C5 C 0.3198(5) 0.1938(4) 0.8533(4) 0.0063(7) Uani 1 1 d . C6 C 0.2595(5) 0.0294(4) 0.8900(4) 0.0063(7) Uani 1 1 d . H6 H 0.2417 -0.0098 0.8146 0.008 Uiso 1 1 calc R C7 C 0.2259(5) -0.0769(4) 1.0392(4) 0.0061(7) Uani 1 1 d . C8 C 0.2536(5) -0.0191(4) 1.1495(4) 0.0075(7) Uani 1 1 d . H8 H 0.2276 -0.0909 1.2509 0.009 Uiso 1 1 calc R C9 C 0.1183(5) -0.2973(4) 0.9766(4) 0.0080(7) Uani 1 1 d . H9A H 0.2255 -0.3040 0.9059 0.010 Uiso 1 1 calc R H9B H 0.0354 -0.2171 0.9203 0.010 Uiso 1 1 calc R C10 C 0.0321(5) -0.4698(4) 1.0557(4) 0.0062(7) Uani 1 1 d . H10A H -0.0692 -0.4641 1.1320 0.007 Uiso 1 1 calc R H10B H 0.1183 -0.5512 1.1063 0.007 Uiso 1 1 calc R O1W O 0.2438(4) 0.5313(3) 1.3582(3) 0.0124(6) Uani 1 1 d . H1WA H 0.2285 0.6096 1.4092 0.015 Uiso 1 1 d R H1WB H 0.1863 0.5990 1.2774 0.015 Uiso 1 1 d R O2W O 0.6854(4) 0.1824(3) 1.3997(3) 0.0129(6) Uani 1 1 d . H2WA H 0.8097 0.2079 1.3764 0.016 Uiso 1 1 d R H2WB H 0.6883 0.0849 1.4881 0.016 Uiso 1 1 d R O3W O 0.9794(4) 0.2764(4) 1.4749(3) 0.0213(7) Uani 1 1 d . H3WA H 1.0470 0.3787 1.4432 0.026 Uiso 1 1 d R H3WB H 1.0548 0.1825 1.4747 0.026 Uiso 1 1 d 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 0.0139(3) 0.0060(3) 0.0011(2) 0.00056(17) -0.00091(16) -0.00486(17) O1 0.0272(16) 0.0120(14) 0.0034(12) -0.0010(11) -0.0052(11) 0.0015(12) O2 0.0203(14) 0.0068(13) 0.0097(13) -0.0041(11) -0.0079(11) -0.0033(11) O3 0.0176(14) 0.0038(12) 0.0022(11) 0.0010(10) -0.0031(10) -0.0047(10) O4 0.0242(15) 0.0087(13) 0.0008(12) -0.0010(10) 0.0009(10) -0.0036(11) O5 0.0128(13) 0.0053(12) 0.0076(12) -0.0005(10) -0.0003(10) -0.0036(10) C1 0.0112(18) 0.0116(18) 0.0073(17) -0.0060(15) -0.0064(14) 0.0034(14) C2 0.0100(17) 0.0070(17) 0.0050(17) -0.0001(14) -0.0023(13) -0.0016(14) C3 0.0089(17) 0.0057(17) 0.0060(17) -0.0041(14) -0.0029(13) 0.0020(13) C4 0.0066(16) 0.0048(16) 0.0040(16) 0.0006(13) -0.0015(13) -0.0010(13) C5 0.0067(16) 0.0066(17) 0.0042(16) -0.0013(14) 0.0004(13) 0.0013(13) C6 0.0087(17) 0.0047(17) 0.0061(17) -0.0023(14) -0.0016(13) -0.0015(14) C7 0.0066(16) 0.0031(16) 0.0089(17) -0.0019(14) -0.0025(13) -0.0011(13) C8 0.0121(17) 0.0059(17) 0.0031(16) -0.0001(14) -0.0021(13) 0.0023(14) C9 0.0138(18) 0.0061(17) 0.0033(16) -0.0007(14) -0.0004(13) -0.0035(14) C10 0.0094(17) 0.0026(16) 0.0057(16) -0.0001(14) -0.0017(13) -0.0007(13) O1W 0.0184(14) 0.0104(13) 0.0084(13) -0.0029(11) -0.0042(11) 0.0027(11) O2W 0.0151(14) 0.0098(13) 0.0107(13) 0.0000(11) -0.0021(11) -0.0003(11) O3W 0.0172(15) 0.0226(16) 0.0213(16) -0.0053(13) -0.0003(12) -0.0060(13) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Zn1 O4 1.976(3) 1_556 Zn1 O2 1.992(3) . Zn1 O5 1.995(3) 2_667 Zn1 O2W 2.101(3) . Zn1 O1W 2.254(3) . Zn1 C1 2.592(4) . O1 C1 1.262(5) . O2 C1 1.271(5) . O3 C7 1.373(4) . O3 C9 1.447(4) . O4 C2 1.255(5) . O4 Zn1 1.976(3) 1_554 O5 C2 1.257(4) . O5 Zn1 1.995(3) 2_667 C1 C3 1.494(5) . C2 C5 1.511(5) . C3 C8 1.383(5) . C3 C4 1.404(5) . C4 C5 1.397(5) . C4 H4 0.9500 . C5 C6 1.396(5) . C6 C7 1.398(5) . C6 H6 0.9500 . C7 C8 1.395(5) . C8 H8 0.9500 . C9 C10 1.514(5) . C9 H9A 0.9900 . C9 H9B 0.9900 . C10 C10 1.532(7) 2_547 C10 H10A 0.9900 . C10 H10B 0.9900 . O1W H1WA 0.9600 . O1W H1WB 0.9600 . O2W H2WA 0.9600 . O2W H2WB 0.9600 . O3W H3WA 0.9600 . O3W H3WB 0.9600 . 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 O4 Zn1 O2 139.08(11) 1_556 . O4 Zn1 O5 113.50(11) 1_556 2_667 O2 Zn1 O5 107.35(11) . 2_667 O4 Zn1 O2W 91.10(12) 1_556 . O2 Zn1 O2W 92.77(11) . . O5 Zn1 O2W 87.75(11) 2_667 . O4 Zn1 O1W 91.08(11) 1_556 . O2 Zn1 O1W 85.45(11) . . O5 Zn1 O1W 91.56(10) 2_667 . O2W Zn1 O1W 177.81(10) . . O4 Zn1 C1 111.24(12) 1_556 . O2 Zn1 C1 28.55(11) . . O5 Zn1 C1 135.05(12) 2_667 . O2W Zn1 C1 87.34(11) . . O1W Zn1 C1 91.69(11) . . C1 O2 Zn1 102.9(2) . . C7 O3 C9 117.3(3) . . C2 O4 Zn1 125.6(2) . 1_554 C2 O5 Zn1 138.8(2) . 2_667 O1 C1 O2 121.7(3) . . O1 C1 C3 120.2(3) . . O2 C1 C3 118.1(3) . . O1 C1 Zn1 73.5(2) . . O2 C1 Zn1 48.52(17) . . C3 C1 Zn1 165.9(3) . . O4 C2 O5 125.0(3) . . O4 C2 C5 116.3(3) . . O5 C2 C5 118.8(3) . . C8 C3 C4 120.4(3) . . C8 C3 C1 119.7(3) . . C4 C3 C1 119.9(3) . . C5 C4 C3 118.9(3) . . C5 C4 H4 120.5 . . C3 C4 H4 120.5 . . C6 C5 C4 121.0(3) . . C6 C5 C2 119.1(3) . . C4 C5 C2 119.8(3) . . C5 C6 C7 119.1(3) . . C5 C6 H6 120.4 . . C7 C6 H6 120.4 . . O3 C7 C8 116.2(3) . . O3 C7 C6 123.6(3) . . C8 C7 C6 120.2(3) . . C3 C8 C7 120.3(3) . . C3 C8 H8 119.9 . . C7 C8 H8 119.9 . . O3 C9 C10 108.2(3) . . O3 C9 H9A 110.0 . . C10 C9 H9A 110.0 . . O3 C9 H9B 110.0 . . C10 C9 H9B 110.0 . . H9A C9 H9B 108.4 . . C9 C10 C10 110.1(4) . 2_547 C9 C10 H10A 109.6 . . C10 C10 H10A 109.6 2_547 . C9 C10 H10B 109.6 . . C10 C10 H10B 109.6 2_547 . H10A C10 H10B 108.2 . . Zn1 O1W H1WA 120.6 . . Zn1 O1W H1WB 135.4 . . H1WA O1W H1WB 95.9 . . Zn1 O2W H2WA 128.9 . . Zn1 O2W H2WB 120.6 . . H2WA O2W H2WB 97.2 . . H3WA O3W H3WB 111.0 . . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WA O3W 0.96 2.18 2.986(4) 140.7 2_668 O1W H1WB O3 0.96 1.90 2.815(4) 157.7 1_565 O2W H2WA O3W 0.96 1.99 2.749(4) 134.9 . O2W H2WB O1 0.96 1.79 2.746(4) 171.3 2_658 O3W H3WA O1W 0.96 1.91 2.830(4) 159.4 1_655 O3W H3WB O1 0.96 2.14 2.964(4) 143.0 1_655