#------------------------------------------------------------------------------ #$Date: 2013-12-09 14:44:49 +0000 (Mon, 09 Dec 2013) $ #$Revision: 91241 $ #$URL: svn://www.crystallography.net/cod/cif/2/23/88/2238820.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2238820 loop_ _publ_author_name 'Ko, Nakeun' 'Kim, Jaheon' _publ_section_title ; Poly[bis(ethanol)(\m~4~-2,3,5,6-tetrafluorobenzene-1,4-dicarboxylato)cadmium] ; _journal_coeditor_code XU5740 _journal_issue 11 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m577 _journal_page_last m578 _journal_paper_doi 10.1107/S1600536813026287 _journal_volume 69 _journal_year 2013 _chemical_formula_iupac '[Cd (C8 F4 O4) (C2 H6 O1)2]' _chemical_formula_moiety 'C12 H12 Cd F4 O6' _chemical_formula_sum 'C12 H12 Cd F4 O6' _chemical_formula_weight 440.61 _chemical_name_systematic ; Poly[bis(ethanol)(\m~4~-2,3,5,6-tetrafluorobenzene-1,4-dicarboxylato)cadmium] ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _cell_angle_alpha 108.0910(10) _cell_angle_beta 100.6370(10) _cell_angle_gamma 102.2750(10) _cell_formula_units_Z 1 _cell_length_a 4.8367(3) _cell_length_b 9.0903(6) _cell_length_c 9.4078(6) _cell_measurement_reflns_used 2269 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 28.209 _cell_measurement_theta_min 2.365 _cell_volume 369.95(4) _computing_cell_refinement 'SAINT (Bruker, 2007)' _computing_data_collection 'SMART (Bruker, 2007)' _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'publCIF (Westrip, 2010)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _diffrn_ambient_temperature 173(2) _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.969 _diffrn_measurement_device_type 'Bruker SMART APEX CCD' _diffrn_measurement_method 'phi and omega scans' _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 0.0139 _diffrn_reflns_av_sigmaI/netI 0.0239 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 2308 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.085 _diffrn_reflns_theta_min 2.365 _exptl_absorpt_coefficient_mu 1.548 _exptl_absorpt_correction_T_max 0.913 _exptl_absorpt_correction_T_min 0.613 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.978 _exptl_crystal_description plate _exptl_crystal_F_000 216 _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.06 _refine_diff_density_max 0.397 _refine_diff_density_min -0.543 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.107 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 131 _refine_ls_number_reflns 1576 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.107 _refine_ls_R_factor_all 0.0206 _refine_ls_R_factor_gt 0.0204 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0317P)^2^+0.1686P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.0543 _reflns_number_gt 1569 _reflns_number_total 1576 _reflns_threshold_expression I>2\s(I) _iucr_refine_instructions_details ; TITL cdfbdc in P-1 CELL 0.71073 4.8367 9.0903 9.4078 108.091 100.637 102.275 ZERR 2.00 0.0003 0.0006 0.0006 0.001 0.001 0.001 LATT 1 SFAC C H O F Cd UNIT 12 12 6 4 1 L.S. 16 ACTA BOND $H FMAP 2 PLAN 10 CONF EQIV $2 -x+2, -y+1, -z+2 EQIV $3 x+1, y, z HTAB O3 O2_$2 HTAB O3 F2_$3 SHEL 999 0.78 DEFS 0.005 SADI O3 C5 O3 C5a DFIX 1.5 C5 C6 C5a C6a DFIX 0.85 O3 H3OA O3 H3OB SADI Cd1 H3OA Cd1 H3OB FREE C6 C6A FREE C6 C5A FREE C5 C6A FREE C5 C5A SIZE 0.35 0.20 0.06 TEMP -100 WGHT 0.031700 0.168600 FVAR 0.29387 0.56709 CD1 5 1.000000 0.500000 1.000000 10.50000 0.01309 0.01499 = 0.03701 0.01066 0.01226 0.00397 F1 4 0.138945 0.247683 1.275153 11.00000 0.04766 0.02345 = 0.02917 0.00417 0.01660 -0.00160 F2 4 0.266019 0.019453 0.774340 11.00000 0.04338 0.02682 = 0.03874 0.01173 0.02844 0.00386 O1 3 0.668685 0.289421 1.008373 11.00000 0.01600 0.02044 = 0.05122 0.01738 0.01552 0.00619 O2 3 0.389948 0.431850 1.121025 11.00000 0.01844 0.01653 = 0.03310 0.00940 0.00826 0.00354 C1 1 0.444584 0.301657 1.054300 11.00000 0.01374 0.01860 = 0.03095 0.01270 0.00610 0.00287 C2 1 0.219116 0.145049 1.026677 11.00000 0.01281 0.01751 = 0.03203 0.01310 0.00813 0.00502 C3 1 0.073841 0.126844 1.137462 11.00000 0.02138 0.01879 = 0.02727 0.00794 0.00792 0.00445 C4 1 0.139679 0.013706 0.888790 11.00000 0.01963 0.02188 = 0.03021 0.01323 0.01395 0.00628 O3 3 1.082259 0.338383 0.780228 11.00000 0.02580 0.03012 = 0.03317 0.00319 0.00548 0.00455 H3OA 2 1.249264 0.392532 0.780701 21.00000 -1.20000 H3OB 2 1.136876 0.266860 0.808958 -21.00000 -1.20000 PART 1 C5 1 0.867054 0.236575 0.635043 21.00000 0.05097 0.03345 = 0.04886 -0.00456 -0.00859 -0.00069 AFIX 23 H5A 2 0.691386 0.176946 0.655295 21.00000 -1.20000 H5B 2 0.950226 0.156769 0.572573 21.00000 -1.20000 AFIX 0 C6 1 0.783101 0.339188 0.548380 21.00000 0.10864 0.12790 = 0.04000 0.00374 0.00169 0.07908 AFIX 33 H6A 2 0.633474 0.271075 0.450859 21.00000 -1.50000 H6B 2 0.956611 0.395104 0.525686 21.00000 -1.50000 H6C 2 0.703886 0.419015 0.611477 21.00000 -1.50000 AFIX 0 PART 2 C5A 1 0.937239 0.301159 0.618810 -21.00000 0.05321 0.07153 = 0.03334 0.01473 -0.00375 -0.02786 AFIX 23 H5AA 2 0.921489 0.401517 0.601713 -21.00000 -1.20000 H5AB 2 1.052365 0.250820 0.551402 -21.00000 -1.20000 AFIX 0 C6A 1 0.640451 0.188342 0.580099 -21.00000 0.03254 0.12393 = 0.03582 0.00880 -0.00006 -0.01723 AFIX 33 H6AA 2 0.541017 0.159936 0.470468 -21.00000 -1.50000 H6AB 2 0.526073 0.240276 0.645183 -21.00000 -1.50000 H6AC 2 0.657902 0.090174 0.599033 -21.00000 -1.50000 PART 0 AFIX 0 HKLF 4 REM cdfbdc in P-1 REM R1 = 0.0204 for 1569 Fo > 4sig(Fo) and 0.0206 for all 1576 data REM 131 parameters refined using 6 restraints END WGHT 0.0321 0.1912 REM Highest difference peak 0.397, deepest hole -0.543, 1-sigma level 0.078 Q1 1 1.0796 0.5767 0.9855 11.00000 0.05 0.40 Q2 1 0.3268 0.2241 1.0347 11.00000 0.05 0.37 Q3 1 0.6617 0.2653 0.5784 11.00000 0.05 0.36 Q4 1 1.0126 0.5721 0.9593 11.00000 0.05 0.36 Q5 1 0.4001 0.4367 1.1837 11.00000 0.05 0.31 Q6 1 0.7373 0.1605 0.5778 11.00000 0.05 0.29 Q7 1 0.0321 -0.0527 0.8812 11.00000 0.05 0.28 Q8 1 0.1479 0.1371 1.0825 11.00000 0.05 0.27 Q9 1 0.2272 0.4376 1.1484 11.00000 0.05 0.24 Q10 1 0.9570 0.2362 0.5983 11.00000 0.05 0.24 ; _[local]_cod_data_source_file xu5740.cif _[local]_cod_data_source_block I _cod_database_code 2238820 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_disorder_assembly _atom_site_disorder_group Cd Cd1 1.0000 0.5000 1.0000 0.02063(9) Uani d 1 2 A . F F1 0.1389(4) 0.24768(17) 1.27515(16) 0.0358(3) Uani d 1 1 . . F F2 0.2660(3) 0.01945(17) 0.77434(17) 0.0349(3) Uani d 1 1 . . O O1 0.6687(3) 0.28942(19) 1.0084(2) 0.0271(3) Uani d 1 1 . . O O2 0.3899(3) 0.43185(17) 1.12102(18) 0.0227(3) Uani d 1 1 . . C C1 0.4446(4) 0.3017(2) 1.0543(2) 0.0205(4) Uani d 1 1 . . C C2 0.2191(4) 0.1450(2) 1.0267(2) 0.0194(4) Uani d 1 1 . . C C3 0.0738(5) 0.1268(3) 1.1375(2) 0.0226(4) Uani d 1 1 . . C C4 0.1397(5) 0.0137(3) 0.8888(3) 0.0219(4) Uani d 1 1 . . O O3 1.0823(4) 0.3384(2) 0.7802(2) 0.0327(4) Uani d 1 1 . . H H3OA 1.249(5) 0.393(5) 0.781(5) 0.039 Uiso d 0.567(10) 1 . . H H3OB 1.137(15) 0.267(5) 0.809(5) 0.039 Uiso d 0.433(10) 1 . . C C5 0.8671(16) 0.2366(7) 0.6350(7) 0.055(2) Uani d 0.567(10) 1 A 1 H H5A 0.6914 0.1769 0.6553 0.065 Uiso calc 0.567(10) 1 A 1 H H5B 0.9502 0.1568 0.5726 0.065 Uiso calc 0.567(10) 1 A 1 C C6 0.783(2) 0.3392(10) 0.5484(8) 0.094(4) Uani d 0.567(10) 1 A 1 H H6A 0.6335 0.2711 0.4509 0.141 Uiso calc 0.567(10) 1 A 1 H H6B 0.9566 0.3951 0.5257 0.141 Uiso calc 0.567(10) 1 A 1 H H6C 0.7039 0.4190 0.6115 0.141 Uiso calc 0.567(10) 1 A 1 C C5A 0.9372(18) 0.3012(15) 0.6188(7) 0.064(3) Uani d 0.433(10) 1 A 2 H H5AA 0.9215 0.4015 0.6017 0.076 Uiso calc 0.433(10) 1 A 2 H H5AB 1.0524 0.2508 0.5514 0.076 Uiso calc 0.433(10) 1 A 2 C C6A 0.6405(16) 0.1883(14) 0.5801(9) 0.077(4) Uani d 0.433(10) 1 A 2 H H6AA 0.5410 0.1599 0.4705 0.116 Uiso calc 0.433(10) 1 A 2 H H6AB 0.5261 0.2403 0.6452 0.116 Uiso calc 0.433(10) 1 A 2 H H6AC 0.6579 0.0902 0.5990 0.116 Uiso calc 0.433(10) 1 A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cd1 0.01309(12) 0.01499(12) 0.03701(14) 0.00397(8) 0.01226(8) 0.01066(9) F1 0.0477(9) 0.0235(7) 0.0292(7) -0.0016(6) 0.0166(6) 0.0042(6) F2 0.0434(8) 0.0268(7) 0.0387(7) 0.0039(6) 0.0284(6) 0.0117(6) O1 0.0160(7) 0.0204(8) 0.0512(10) 0.0062(6) 0.0155(7) 0.0174(7) O2 0.0184(7) 0.0165(7) 0.0331(8) 0.0035(6) 0.0083(6) 0.0094(6) C1 0.0137(9) 0.0186(10) 0.0310(10) 0.0029(7) 0.0061(7) 0.0127(8) C2 0.0128(8) 0.0175(9) 0.0320(10) 0.0050(7) 0.0081(7) 0.0131(8) C3 0.0214(10) 0.0188(10) 0.0273(10) 0.0045(8) 0.0079(8) 0.0079(8) C4 0.0196(10) 0.0219(10) 0.0302(10) 0.0063(8) 0.0140(8) 0.0132(8) O3 0.0258(8) 0.0301(9) 0.0332(9) 0.0046(7) 0.0055(7) 0.0032(7) C5 0.051(5) 0.033(3) 0.049(3) -0.001(3) -0.009(3) -0.005(3) C6 0.109(7) 0.128(8) 0.040(4) 0.079(7) 0.002(4) 0.004(4) C5A 0.053(5) 0.072(7) 0.033(4) -0.028(5) -0.004(3) 0.015(4) C6A 0.033(4) 0.124(9) 0.036(4) -0.017(5) 0.000(3) 0.009(4) 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle O1 Cd1 O1 2_767 . 180.0 O1 Cd1 O3 2_767 2_767 91.52(7) O1 Cd1 O3 . 2_767 88.48(6) O1 Cd1 O3 2_767 . 88.48(6) O1 Cd1 O3 . . 91.52(7) O3 Cd1 O3 2_767 . 180.0 O1 Cd1 O2 2_767 1_655 87.93(6) O1 Cd1 O2 . 1_655 92.07(6) O3 Cd1 O2 2_767 1_655 97.63(6) O3 Cd1 O2 . 1_655 82.37(6) O1 Cd1 O2 2_767 2_667 92.07(5) O1 Cd1 O2 . 2_667 87.93(6) O3 Cd1 O2 2_767 2_667 82.37(6) O3 Cd1 O2 . 2_667 97.63(6) O2 Cd1 O2 1_655 2_667 180.0 C1 O1 Cd1 . . 123.39(14) C1 O2 Cd1 . 1_455 120.48(13) O1 C1 O2 . . 126.19(19) O1 C1 C2 . . 116.46(19) O2 C1 C2 . . 117.36(18) C4 C2 C3 . . 116.23(19) C4 C2 C1 . . 122.13(19) C3 C2 C1 . . 121.62(19) F1 C3 C4 . 2_557 117.7(2) F1 C3 C2 . . 120.24(19) C4 C3 C2 2_557 . 122.0(2) F2 C4 C3 . 2_557 117.5(2) F2 C4 C2 . . 120.81(19) C3 C4 C2 2_557 . 121.7(2) C5 O3 Cd1 . . 127.3(4) C5A O3 Cd1 . . 129.2(6) C5 O3 H3OA . . 120(3) C5A O3 H3OA . . 97(3) Cd1 O3 H3OA . . 103(3) C5 O3 H3OB . . 100(4) C5A O3 H3OB . . 120(3) Cd1 O3 H3OB . . 103(3) H3OA O3 H3OB . . 98(6) O3 C5 C6 . . 109.1(5) O3 C5 H5A . . 109.9 C6 C5 H5A . . 109.9 O3 C5 H5B . . 109.9 C6 C5 H5B . . 109.9 H5A C5 H5B . . 108.3 C5 C6 H6A . . 109.5 C5 C6 H6B . . 109.5 H6A C6 H6B . . 109.5 C5 C6 H6C . . 109.5 H6A C6 H6C . . 109.5 H6B C6 H6C . . 109.5 C6A C5A O3 . . 108.5(5) C6A C5A H5AA . . 110.0 O3 C5A H5AA . . 110.0 C6A C5A H5AB . . 110.0 O3 C5A H5AB . . 110.0 H5AA C5A H5AB . . 108.4 C5A C6A H6AA . . 109.5 C5A C6A H6AB . . 109.5 H6AA C6A H6AB . . 109.5 C5A C6A H6AC . . 109.5 H6AA C6A H6AC . . 109.5 H6AB C6A H6AC . . 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cd1 O1 2_767 2.2526(15) ? Cd1 O1 . 2.2526(15) y Cd1 O2 1_655 2.3194(15) y Cd1 O2 2_667 2.3194(15) ? Cd1 O3 2_767 2.2929(18) ? Cd1 O3 . 2.2929(18) y F1 C3 . 1.343(3) ? F2 C4 . 1.342(2) ? O1 C1 . 1.252(3) ? O2 C1 . 1.264(3) ? O2 Cd1 1_455 2.3194(15) ? C1 C2 . 1.513(3) ? C2 C4 . 1.384(3) ? C2 C3 . 1.391(3) ? C3 C4 2_557 1.382(3) ? C4 C3 2_557 1.382(3) ? O3 C5 . 1.444(4) ? O3 C5A . 1.449(5) ? O3 H3OA . 0.850(5) ? O3 H3OB . 0.849(5) ? C5 C6 . 1.487(5) ? C5 H5A . 0.9900 ? C5 H5B . 0.9900 ? C6 H6A . 0.9800 ? C6 H6B . 0.9800 ? C6 H6C . 0.9800 ? C5A C6A . 1.481(5) ? C5A H5AA . 0.9900 ? C5A H5AB . 0.9900 ? C6A H6AA . 0.9800 ? C6A H6AB . 0.9800 ? C6A H6AC . 0.9800 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA O3 H3OA O2 2_767 0.850(5) 1.94(2) 2.719(2) 152(4) O3 H3OB F2 1_655 0.849(5) 2.402(18) 3.196(2) 156(4) 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_site_symmetry_1 _geom_torsion_site_symmetry_4 _geom_torsion Cd1 O1 C1 O2 . . -10.2(3) Cd1 O1 C1 C2 . . 169.78(13) Cd1 O2 C1 O1 1_455 . 113.9(2) Cd1 O2 C1 C2 1_455 . -66.1(2) O1 C1 C2 C4 . . -41.9(3) O2 C1 C2 C4 . . 138.0(2) O1 C1 C2 C3 . . 139.9(2) O2 C1 C2 C3 . . -40.1(3) C4 C2 C3 F1 . . 179.42(19) C1 C2 C3 F1 . . -2.3(3) C4 C2 C3 C4 . 2_557 -0.6(3) C1 C2 C3 C4 . 2_557 177.71(19) C3 C2 C4 F2 . . 179.70(19) C1 C2 C4 F2 . . 1.4(3) C3 C2 C4 C3 . 2_557 0.6(3) C1 C2 C4 C3 . 2_557 -177.70(19) C5A O3 C5 C6 . . -28.4(13) Cd1 O3 C5 C6 . . 76.5(7) C5 O3 C5A C6A . . 23.6(10) Cd1 O3 C5A C6A . . -73.7(11)