#------------------------------------------------------------------------------ #$Date: 2014-07-12 01:16:09 +0300 (Sat, 12 Jul 2014) $ #$Revision: 120081 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/30/85/4308534.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_4308534 loop_ _publ_author_name 'Diane A. Dickie' 'Michael C. Jennings' 'Hilary A. Jenkins' 'Jason A. C. Clyburne' _publ_contact_author_address ;Department of Chemistry Simon Fraser University 8888 University Dr Burnaby, BC V5A 1S6 Canada ; _publ_contact_author_email clyburne@sfu.ca _publ_contact_author_fax (604)291-3765 _publ_contact_author_name 'Jason Clyburne' _publ_contact_author_phone (604)291-4885 _publ_section_title ; A Zinc Carboxylate Network Containing Metal Sites with Low Coordination Numbers ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 828 _journal_page_last 830 _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C20 H14 O4' _chemical_formula_weight 318.31 _chemical_name_systematic ; ? ; _space_group_IT_number 92 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall 'P 4abw 2nw' _symmetry_space_group_name_H-M 'P 41 21 2' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 13.5640(3) _cell_length_b 13.5640(3) _cell_length_c 17.0150(4) _cell_measurement_temperature 173(2) _cell_volume 3130.46(12) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 173(2) _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0338 _diffrn_reflns_av_sigmaI/netI 0.0467 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 6119 _diffrn_reflns_theta_full 26.00 _diffrn_reflns_theta_max 26.00 _diffrn_reflns_theta_min 3.57 _exptl_absorpt_coefficient_mu 0.094 _exptl_absorpt_correction_T_max 0.9906 _exptl_absorpt_correction_T_min 0.9814 _exptl_crystal_density_diffrn 1.351 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.194 _refine_diff_density_min -0.128 _refine_diff_density_rms 0.032 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 1.0(12) _refine_ls_extinction_coef 0.0024(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 222 _refine_ls_number_reflns 3074 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.041 _refine_ls_R_factor_all 0.0574 _refine_ls_R_factor_gt 0.0396 _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^)+(0.0370P)^2^+0.4022P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0808 _refine_ls_wR_factor_ref 0.0885 _reflns_number_gt 2491 _reflns_number_total 3074 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ic048443hsi20041105_044950.cif _[local]_cod_data_source_block sask1 _cod_database_code 4308534 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, -z+3/4' '-x+1/2, y+1/2, -z+1/4' '-y, -x, -z+1/2' 'y, x, -z' 'y+1/2, -x+1/2, z+3/4' '-y+1/2, x+1/2, z+1/4' 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 O1 O 0.21747(9) 0.33338(10) -0.50290(9) 0.0417(4) Uani 1 1 d . . . H1 H 0.1809 0.2834 -0.5026 0.063 Uiso 0.50 1 calc PR . . O2 O 0.66595(9) 0.60956(9) -0.44241(8) 0.0355(3) Uani 1 1 d . . . H2 H 0.7063 0.6559 -0.4486 0.053 Uiso 0.50 1 calc PR . . O3 O 0.41832(10) 0.69417(9) -0.23335(9) 0.0418(4) Uani 1 1 d . . . H3 H 0.3686 0.7310 -0.2353 0.063 Uiso 0.50 1 calc PR . . O4 O 0.68897(10) 0.23874(9) -0.30132(8) 0.0382(4) Uani 1 1 d . . . H4 H 0.7363 0.1994 -0.2957 0.057 Uiso 0.50 1 calc PR . . C1 C 0.30670(12) 0.30670(12) -0.5000 0.0290(6) Uani 1 2 d S . . C2 C 0.38422(13) 0.38422(13) -0.5000 0.0281(6) Uani 1 2 d S . . C3 C 0.48288(13) 0.35825(13) -0.50880(11) 0.0306(4) Uani 1 1 d . . . H3A H 0.5002 0.2908 -0.5144 0.037 Uiso 1 1 calc R . . C4 C 0.55676(13) 0.42996(13) -0.50948(11) 0.0285(4) Uani 1 1 d . . . C5 C 0.52910(12) 0.52910(12) -0.5000 0.0270(6) Uani 1 2 d S . . C6 C 0.60721(12) 0.60721(12) -0.5000 0.0265(6) Uani 1 2 d S . . C7 C 0.66158(13) 0.40025(13) -0.51997(11) 0.0294(4) Uani 1 1 d . . . C8 C 0.72265(15) 0.44604(15) -0.57462(13) 0.0387(5) Uani 1 1 d . . . H8A H 0.6972 0.4965 -0.6076 0.046 Uiso 1 1 calc R . . C9 C 0.82061(16) 0.41800(17) -0.58089(15) 0.0521(6) Uani 1 1 d . . . H9A H 0.8619 0.4490 -0.6186 0.062 Uiso 1 1 calc R . . C10 C 0.85864(16) 0.34546(18) -0.53281(16) 0.0536(7) Uani 1 1 d . . . H10A H 0.9261 0.3273 -0.5368 0.064 Uiso 1 1 calc R . . C11 C 0.79870(15) 0.29988(16) -0.47927(14) 0.0453(6) Uani 1 1 d . . . H11A H 0.8248 0.2500 -0.4460 0.054 Uiso 1 1 calc R . . C12 C 0.70027(14) 0.32599(14) -0.47328(12) 0.0354(5) Uani 1 1 d . . . H12A H 0.6589 0.2927 -0.4369 0.042 Uiso 1 1 calc R . . C13 C 0.39333(12) 0.60667(12) -0.2500 0.0294(6) Uani 1 2 d S . . C14 C 0.47125(12) 0.52875(12) -0.2500 0.0288(6) Uani 1 2 d S . . C15 C 0.56952(13) 0.55505(13) -0.24295(11) 0.0302(4) Uani 1 1 d . . . H15A H 0.5867 0.6225 -0.2364 0.036 Uiso 1 1 calc R . . C16 C 0.64363(12) 0.48381(13) -0.24541(11) 0.0276(4) Uani 1 1 d . . . C17 C 0.61628(12) 0.38372(12) -0.2500 0.0263(6) Uani 1 2 d S . . C18 C 0.69436(12) 0.30564(12) -0.2500 0.0250(6) Uani 1 2 d S . . C19 C 0.74842(13) 0.51670(13) -0.24800(12) 0.0278(4) Uani 1 1 d . . . C20 C 0.80476(14) 0.49773(14) -0.31418(12) 0.0376(5) Uani 1 1 d . . . H20A H 0.7776 0.4612 -0.3566 0.045 Uiso 1 1 calc R . . C21 C 0.90106(15) 0.53215(15) -0.31854(15) 0.0447(6) Uani 1 1 d . . . H21A H 0.9392 0.5197 -0.3643 0.054 Uiso 1 1 calc R . . C22 C 0.94159(15) 0.58395(15) -0.25732(14) 0.0433(6) Uani 1 1 d . . . H22A H 1.0078 0.6064 -0.2605 0.052 Uiso 1 1 calc R . . C23 C 0.88644(15) 0.60328(15) -0.19157(13) 0.0423(5) Uani 1 1 d . . . H23A H 0.9144 0.6394 -0.1492 0.051 Uiso 1 1 calc R . . C24 C 0.78946(15) 0.56995(14) -0.18684(12) 0.0361(5) Uani 1 1 d . . . H24A H 0.7513 0.5839 -0.1414 0.043 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 O1 0.0221(7) 0.0264(7) 0.0767(10) 0.0069(7) -0.0023(7) -0.0053(6) O2 0.0289(7) 0.0332(8) 0.0443(8) 0.0031(6) -0.0066(6) -0.0111(6) O3 0.0284(8) 0.0218(7) 0.0751(10) -0.0032(7) -0.0011(7) 0.0061(6) O4 0.0348(8) 0.0290(8) 0.0507(8) -0.0055(6) -0.0001(6) 0.0119(6) C1 0.0230(8) 0.0230(8) 0.0411(16) 0.0026(9) -0.0026(9) -0.0039(11) C2 0.0227(8) 0.0227(8) 0.0389(15) 0.0027(9) -0.0027(9) -0.0063(11) C3 0.0263(10) 0.0211(10) 0.0443(11) 0.0016(9) -0.0011(9) -0.0036(7) C4 0.0242(10) 0.0232(10) 0.0381(11) 0.0018(9) -0.0027(9) -0.0040(7) C5 0.0226(8) 0.0226(8) 0.0358(15) 0.0019(8) -0.0019(8) -0.0057(10) C6 0.0203(8) 0.0203(8) 0.0390(15) 0.0000(9) 0.0000(9) -0.0016(11) C7 0.0215(10) 0.0235(10) 0.0432(11) -0.0057(9) -0.0021(9) -0.0056(8) C8 0.0303(12) 0.0336(12) 0.0524(12) -0.0032(10) 0.0033(10) -0.0052(9) C9 0.0331(13) 0.0464(14) 0.0766(16) -0.0071(13) 0.0164(12) -0.0074(11) C10 0.0247(12) 0.0506(15) 0.0854(18) -0.0168(14) 0.0026(12) 0.0059(11) C11 0.0346(12) 0.0376(12) 0.0638(14) -0.0084(11) -0.0082(11) 0.0089(10) C12 0.0296(11) 0.0279(11) 0.0486(12) -0.0034(9) -0.0018(9) -0.0001(9) C13 0.0190(8) 0.0190(8) 0.0503(17) 0.0032(9) 0.0032(9) 0.0015(11) C14 0.0197(8) 0.0197(8) 0.0470(16) 0.0040(9) 0.0040(9) 0.0036(10) C15 0.0226(10) 0.0219(10) 0.0463(11) 0.0024(9) 0.0015(9) 0.0020(7) C16 0.0229(10) 0.0222(9) 0.0377(11) 0.0032(9) 0.0017(9) 0.0026(7) C17 0.0216(8) 0.0216(8) 0.0356(14) 0.0016(8) 0.0016(8) 0.0027(11) C18 0.0191(8) 0.0191(8) 0.0367(15) 0.0031(9) 0.0031(9) 0.0002(10) C19 0.0191(9) 0.0185(9) 0.0458(11) 0.0049(9) 0.0001(9) 0.0021(7) C20 0.0289(11) 0.0308(11) 0.0530(13) -0.0039(10) 0.0060(10) -0.0001(9) C21 0.0289(12) 0.0374(12) 0.0678(15) 0.0014(11) 0.0158(11) -0.0023(9) C22 0.0210(10) 0.0324(11) 0.0764(16) 0.0072(12) 0.0016(11) -0.0023(8) C23 0.0331(12) 0.0353(12) 0.0583(13) 0.0058(11) -0.0125(11) -0.0081(9) C24 0.0319(11) 0.0327(11) 0.0436(12) 0.0034(10) 0.0012(10) 0.0001(9) 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' 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 C1 O1 H1 109.5 . . ? C6 O2 H2 109.5 . . ? C13 O3 H3 109.5 . . ? C18 O4 H4 109.5 . . ? O1 C1 O1 123.3(2) 6_554 . ? O1 C1 C2 118.33(11) 6_554 . ? O1 C1 C2 118.33(11) . . ? C3 C2 C3 119.9(2) 6_554 . ? C3 C2 C1 120.06(11) 6_554 . ? C3 C2 C1 120.06(11) . . ? C2 C3 C4 120.96(17) . . ? C2 C3 H3A 119.5 . . ? C4 C3 H3A 119.5 . . ? C3 C4 C5 118.29(17) . . ? C3 C4 C7 119.85(16) . . ? C5 C4 C7 121.85(16) . . ? C4 C5 C4 121.6(2) 6_554 . ? C4 C5 C6 119.20(11) 6_554 . ? C4 C5 C6 119.20(11) . . ? O2 C6 O2 124.7(2) . 6_554 ? O2 C6 C5 117.63(11) . . ? O2 C6 C5 117.63(11) 6_554 . ? C12 C7 C8 118.82(17) . . ? C12 C7 C4 119.32(16) . . ? C8 C7 C4 121.85(18) . . ? C9 C8 C7 120.0(2) . . ? C9 C8 H8A 120.0 . . ? C7 C8 H8A 120.0 . . ? C10 C9 C8 120.6(2) . . ? C10 C9 H9A 119.7 . . ? C8 C9 H9A 119.7 . . ? C11 C10 C9 119.6(2) . . ? C11 C10 H10A 120.2 . . ? C9 C10 H10A 120.2 . . ? C10 C11 C12 120.4(2) . . ? C10 C11 H11A 119.8 . . ? C12 C11 H11A 119.8 . . ? C11 C12 C7 120.6(2) . . ? C11 C12 H12A 119.7 . . ? C7 C12 H12A 119.7 . . ? O3 C13 O3 123.5(2) 5_664 . ? O3 C13 C14 118.25(11) 5_664 . ? O3 C13 C14 118.25(11) . . ? C15 C14 C15 120.2(2) 5_664 . ? C15 C14 C13 119.89(11) 5_664 . ? C15 C14 C13 119.89(11) . . ? C14 C15 C16 120.83(17) . . ? C14 C15 H15A 119.6 . . ? C16 C15 H15A 119.6 . . ? C15 C16 C17 118.64(16) . . ? C15 C16 C19 118.74(15) . . ? C17 C16 C19 122.52(15) . . ? C16 C17 C16 120.7(2) . 5_664 ? C16 C17 C18 119.67(11) . . ? C16 C17 C18 119.67(11) 5_664 . ? O4 C18 O4 124.2(2) 5_664 . ? O4 C18 C17 117.88(11) 5_664 . ? O4 C18 C17 117.88(11) . . ? C24 C19 C20 119.11(17) . . ? C24 C19 C16 121.17(17) . . ? C20 C19 C16 119.66(18) . . ? C19 C20 C21 120.0(2) . . ? C19 C20 H20A 120.0 . . ? C21 C20 H20A 120.0 . . ? C22 C21 C20 120.6(2) . . ? C22 C21 H21A 119.7 . . ? C20 C21 H21A 119.7 . . ? C23 C22 C21 119.93(19) . . ? C23 C22 H22A 120.0 . . ? C21 C22 H22A 120.0 . . ? C22 C23 C24 120.0(2) . . ? C22 C23 H23A 120.0 . . ? C24 C23 H23A 120.0 . . ? C19 C24 C23 120.38(19) . . ? C19 C24 H24A 119.8 . . ? C23 C24 H24A 119.8 . . ? 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 O1 C1 1.2642(16) . ? O1 H1 0.8400 . ? O2 C6 1.2633(16) . ? O2 H2 0.8400 . ? O3 C13 1.2663(17) . ? O3 H3 0.8400 . ? O4 C18 1.2614(16) . ? O4 H4 0.8400 . ? C1 O1 1.2642(16) 6_554 ? C1 C2 1.487(3) . ? C2 C3 1.392(2) 6_554 ? C2 C3 1.392(2) . ? C3 C4 1.397(3) . ? C3 H3A 0.9500 . ? C4 C5 1.405(2) . ? C4 C7 1.489(2) . ? C5 C4 1.405(2) 6_554 ? C5 C6 1.498(3) . ? C6 O2 1.2633(16) 6_554 ? C7 C12 1.386(3) . ? C7 C8 1.392(3) . ? C8 C9 1.386(3) . ? C8 H8A 0.9500 . ? C9 C10 1.380(3) . ? C9 H9A 0.9500 . ? C10 C11 1.369(3) . ? C10 H10A 0.9500 . ? C11 C12 1.385(3) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 O3 1.2663(17) 5_664 ? C13 C14 1.495(3) . ? C14 C15 1.385(2) 5_664 ? C14 C15 1.385(2) . ? C15 C16 1.395(3) . ? C15 H15A 0.9500 . ? C16 C17 1.410(2) . ? C16 C19 1.490(2) . ? C17 C16 1.410(2) 5_664 ? C17 C18 1.498(3) . ? C18 O4 1.2614(16) 5_664 ? C19 C24 1.384(3) . ? C19 C20 1.385(3) . ? C20 C21 1.389(3) . ? C20 H20A 0.9500 . ? C21 C22 1.371(3) . ? C21 H21A 0.9500 . ? C22 C23 1.371(3) . ? C22 H22A 0.9500 . ? C23 C24 1.393(3) . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? _journal_paper_doi 10.1021/ic048443h