#------------------------------------------------------------------------------ #$Date: 2016-02-20 16:35:30 +0000 (Sat, 20 Feb 2016) $ #$Revision: 176787 $ #$URL: svn://www.crystallography.net/cod/cif/2/21/42/2214249.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_2214249 loop_ _publ_author_name 'Mustafa Tombul' 'Kutalm\?i\,s G\"uven' 'Orhan B\"uy\"ukg\"ung\"or' _publ_section_title ; Poly[[diaquacaesium(I)]bis(\m~3~-3-carboxypyrazine-2-carboxylato)] ; _journal_coeditor_code HK2251 _journal_issue 7 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m1783 _journal_page_last m1784 _journal_paper_doi 10.1107/S1600536807025536 _journal_volume 63 _journal_year 2007 _chemical_formula_iupac '[Cs (C6 H3 N2 O4)2 (H2 O)2]' _chemical_formula_moiety 'C12 H10 Cs N4 O10' _chemical_formula_sum 'C12 H10 Cs N4 O10' _chemical_formula_weight 503.15 _chemical_name_systematic ; Poly[[diaquacaesium(II)]bis(\m~3~-3-carboxypyrazine-2-carboxylato)] ; _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 _cell_angle_alpha 70.031(9) _cell_angle_beta 81.126(10) _cell_angle_gamma 66.128(9) _cell_formula_units_Z 1 _cell_length_a 7.4801(9) _cell_length_b 7.6352(9) _cell_length_c 8.6505(11) _cell_measurement_reflns_used 22636 _cell_measurement_temperature 296 _cell_measurement_theta_max 27.99 _cell_measurement_theta_min 2.51 _cell_volume 424.55(10) _computing_cell_refinement X-AREA _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-RED32 (Stoe & Cie, 2002)' _computing_molecular_graphics 'PLATON (Spek, 2001)' _computing_publication_material 'enCIFer (Allen et al., 2004)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 296 _diffrn_detector_area_resol_mean 6.67 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'Stoe IPDS2' _diffrn_measurement_method 'rotation method' _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0567 _diffrn_reflns_av_sigmaI/netI 0.0343 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 7683 _diffrn_reflns_theta_full 27.69 _diffrn_reflns_theta_max 27.69 _diffrn_reflns_theta_min 2.51 _exptl_absorpt_coefficient_mu 2.244 _exptl_absorpt_correction_T_max 0.4711 _exptl_absorpt_correction_T_min 0.3817 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details ; (X-RED32; Stoe & Cie, 2002) ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.968 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 245 _exptl_crystal_size_max 0.520 _exptl_crystal_size_mid 0.467 _exptl_crystal_size_min 0.420 _refine_diff_density_max 0.445 _refine_diff_density_min -0.715 _refine_ls_extinction_coef 0.187(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 137 _refine_ls_number_reflns 1968 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.983 _refine_ls_R_factor_all 0.0188 _refine_ls_R_factor_gt 0.0186 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0343P)^2^+0.0717P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.0523 _reflns_number_gt 1949 _reflns_number_total 1968 _reflns_threshold_expression I>2\s(I) _cod_data_source_file hk2251.cif _cod_data_source_block I _cod_database_code 2214249 _cod_database_fobs_code 2214249 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_refinement_flags _atom_site_occupancy Cs Cs1 1.5000 -0.5000 0.5000 0.04315(10) Uani d S 1 O O1 0.7652(2) -0.1628(2) 0.3351(2) 0.0447(3) Uani d . 1 O O2 0.54073(19) 0.3193(2) 0.2006(2) 0.0464(3) Uani d . 1 O O3 1.6315(3) -0.2774(3) 0.1162(2) 0.0545(4) Uani d . 1 H H4 1.719(5) -0.381(6) 0.118(4) 0.059(8) Uiso d . 1 H H5 1.659(5) -0.228(6) 0.147(4) 0.057(9) Uiso d . 1 O O4 1.0625(2) -0.3669(2) 0.4303(2) 0.0500(4) Uani d . 1 O O5 0.6999(2) 0.1627(3) 0.0154(2) 0.0507(3) Uani d . 1 H H3 0.589(5) 0.202(6) -0.020(5) 0.066(9) Uiso d . 1 N N1 1.1830(2) -0.0606(2) 0.34310(19) 0.0342(3) Uani d . 1 N N2 0.9390(2) 0.3245(2) 0.1696(2) 0.0378(3) Uani d . 1 C C1 1.2381(2) 0.0943(3) 0.3004(2) 0.0376(3) Uani d . 1 H H1 1.3639 0.0727 0.3275 0.045 Uiso calc R 1 C C2 1.1156(3) 0.2872(3) 0.2169(3) 0.0403(4) Uani d . 1 H H2 1.1579 0.3942 0.1930 0.048 Uiso calc R 1 C C3 0.8866(2) 0.1668(2) 0.20647(19) 0.0297(3) Uani d . 1 C C4 1.0056(2) -0.0248(2) 0.29693(19) 0.0286(3) Uani d . 1 C C5 0.6880(2) 0.2210(2) 0.1433(2) 0.0331(3) Uani d . 1 C C6 0.9360(2) -0.1975(3) 0.3563(2) 0.0332(3) Uani d . 1 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 Cs1 0.03439(11) 0.03736(11) 0.04492(12) -0.00218(7) -0.00804(6) -0.00818(7) O1 0.0369(6) 0.0391(7) 0.0612(8) -0.0182(6) -0.0151(6) -0.0086(6) O2 0.0287(6) 0.0499(8) 0.0663(9) -0.0114(6) -0.0034(6) -0.0280(7) O3 0.0501(8) 0.0445(8) 0.0754(11) -0.0075(7) -0.0265(8) -0.0279(8) O4 0.0350(6) 0.0290(6) 0.0762(10) -0.0138(5) -0.0103(7) 0.0014(6) O5 0.0401(7) 0.0623(9) 0.0481(7) -0.0066(7) -0.0147(6) -0.0247(7) N1 0.0282(6) 0.0320(6) 0.0403(7) -0.0109(5) -0.0050(5) -0.0073(6) N2 0.0341(7) 0.0291(6) 0.0481(8) -0.0135(6) -0.0073(6) -0.0049(6) C1 0.0286(7) 0.0393(9) 0.0472(9) -0.0163(7) -0.0045(7) -0.0101(7) C2 0.0349(8) 0.0347(8) 0.0539(10) -0.0185(7) -0.0047(7) -0.0084(7) C3 0.0275(7) 0.0299(7) 0.0315(6) -0.0110(6) -0.0027(6) -0.0083(6) C4 0.0277(6) 0.0282(7) 0.0310(6) -0.0116(6) -0.0018(6) -0.0088(5) C5 0.0305(7) 0.0286(7) 0.0394(8) -0.0109(6) -0.0069(6) -0.0073(6) C6 0.0338(7) 0.0299(7) 0.0378(7) -0.0145(6) -0.0042(6) -0.0084(6) 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' Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -8 -4 -1 0.2310 6 3 1 0.2880 0 -3 -4 0.2150 0 1 0 0.2210 0 -1 0 0.2370 3 0 1 0.3010 3 4 1 0.2940 0 -1 -2 0.2090 0 1 2 0.2180 6 -1 -3 0.2910 8 -1 1 0.2860 1 1 0 0.2840 0 -1 -7 0.2400 0 -7 3 0.2450 0 -1 5 0.2880 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle H4 O3 H5 109(4) C5 O5 H3 109(2) C1 N1 C4 117.24(15) C2 N2 C3 116.75(15) N1 C1 C2 121.84(15) N1 C1 H1 119.1 C2 C1 H1 119.1 N2 C2 C1 121.40(15) N2 C2 H2 119.3 C1 C2 H2 119.3 N2 C3 C4 121.81(14) N2 C3 C5 113.30(14) C4 C3 C5 124.88(13) N1 C4 C3 120.82(14) N1 C4 C6 117.40(15) C3 C4 C6 121.66(14) O2 C5 O5 125.96(17) O2 C5 C3 121.64(15) O5 C5 C3 112.19(14) O1 C6 O4 126.00(15) O1 C6 C4 118.73(16) O4 C6 C4 115.22(14) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance Cs1 O1 0 2_646 3.188(2) Cs1 O1 0 1_655 3.188(2) Cs1 O2 0 1_645 3.2490(10) Cs1 O2 0 2_556 3.249(2) Cs1 O3 . . 3.372(2) Cs1 O3 0 2_646 3.372(2) Cs1 O4 . . 3.0990(10) Cs1 O4 0 2_646 3.0990(10) Cs1 N1 . . 3.188(2) Cs1 N1 0 2_646 3.188(2) O1 C6 . . 1.226(2) O2 C5 . . 1.200(2) O3 H4 . . 0.79(4) O3 H5 . . 0.64(4) O4 C6 . . 1.268(2) O5 C5 . . 1.305(2) O5 H3 . . 0.83(4) N1 C1 . . 1.325(2) N1 C4 . . 1.338(2) N2 C2 . . 1.333(2) N2 C3 . . 1.336(2) C1 C2 . . 1.384(3) C1 H1 . . 0.9400 C2 H2 . . 0.9400 C4 C3 . . 1.387(2) C5 C3 . . 1.509(2) C6 C4 . . 1.511(2) loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O5 H3 O3 0 0 2_555 0.830(10) 1.760(10) 2.5770(10) 172.70(3) yes O3 H4 N2 0 0 1_645 0.790(10) 2.130(10) 2.9070(10) 169.64(3) yes O3 H5 O1 0 0 1_655 0.640(10) 2.190(10) 2.7880(10) 157.14(3) yes 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 C4 N1 C1 C2 2.4(3) C1 N1 C4 C3 0.7(2) C1 N1 C4 C6 -175.48(15) C3 N2 C2 C1 -0.1(3) C2 N2 C3 C4 3.2(2) C2 N2 C3 C5 -177.92(16) N1 C1 C2 N2 -2.8(3) N1 C4 C3 N2 -3.7(2) C6 C4 C3 N2 172.36(15) N1 C4 C3 C5 177.61(15) C6 C4 C3 C5 -6.3(2) O2 C5 C3 N2 -69.7(2) O5 C5 C3 N2 105.33(18) O2 C5 C3 C4 109.1(2) O5 C5 C3 C4 -75.9(2) O1 C6 C4 N1 170.21(16) O4 C6 C4 N1 -7.3(2) O1 C6 C4 C3 -6.0(2) O4 C6 C4 C3 176.54(16)