#------------------------------------------------------------------------------ #$Date: 2013-12-28 15:58:47 +0200 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/21/24/2212426.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_2212426 loop_ _publ_author_name 'Shi, Ai-E' 'Li, Bai-Yan' 'Hou, Guang-Feng' 'Gao, Jin-Sheng' _publ_section_title ;trans-Tetraaquabis(2,6-dimethylpyridinium-3,5-dicarboxylato)copper(II) tetrahydrate ; _journal_coeditor_code YA2038 _journal_issue 2 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m471 _journal_page_last m473 _journal_volume 63 _journal_year 2007 _chemical_formula_iupac '[Cu (C9 H8 N O4)2 (H2 O)4] , 4H2 O' _chemical_formula_moiety 'C18 H24 Cu N2 O12 , 4H2 O' _chemical_formula_sum 'C18 H32 Cu N2 O16' _chemical_formula_weight 596.01 _chemical_name_systematic ; trans-Tetraaquabis(2,6-dimethylpyridinium-3,5-dicarboxylato)copper(II) tetrahydrate ; _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 111.22(3) _cell_angle_beta 102.55(3) _cell_angle_gamma 96.83(3) _cell_formula_units_Z 1 _cell_length_a 6.867(5) _cell_length_b 9.203(6) _cell_length_c 11.108(8) _cell_measurement_reflns_used 5849 _cell_measurement_temperature 291(2) _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 3.1 _cell_volume 623.5(8) _computing_cell_refinement RAPID-AUTO _computing_data_collection 'RAPID-AUTO (Rigaku, 1998)' _computing_data_reduction 'CrystalStructure (Rigaku/MSC, 2002)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997b)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997a)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997a)' _diffrn_ambient_temperature 291(2) _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _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 0.024 _diffrn_reflns_av_sigmaI/netI 0.029 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 6158 _diffrn_reflns_theta_full 27.5 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_min 3.1 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.96 _exptl_absorpt_correction_T_max 0.806 _exptl_absorpt_correction_T_min 0.728 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)' _exptl_crystal_colour blue _exptl_crystal_density_diffrn 1.587 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 311 _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.24 _refine_diff_density_max 0.38 _refine_diff_density_min -0.41 _refine_ls_extinction_coef 0.068(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL97 (Sheldrick, 1997a)' _refine_ls_goodness_of_fit_ref 1.20 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 176 _refine_ls_number_reflns 2823 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.20 _refine_ls_R_factor_all 0.032 _refine_ls_R_factor_gt 0.029 _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^)+(0.0565P)^2^+0.2023P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.092 _refine_ls_wR_factor_ref 0.102 _reflns_number_gt 2653 _reflns_number_total 2823 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file ya2038.cif _[local]_cod_data_source_block I _cod_original_cell_volume 623.6(8) _cod_database_code 2212426 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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' Cu Cu 0.3201 1.2651 '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_ _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 C C1 0.7026(3) 0.0160(2) -0.18538(18) 0.0226(4) Uani d . 1 C C2 0.7113(3) -0.0844(2) -0.11700(17) 0.0201(3) Uani d . 1 C C3 0.7557(3) -0.0149(2) 0.02240(17) 0.0204(3) Uani d . 1 H H1 0.7634 -0.0807 0.0693 0.024 Uiso calc R 1 C C4 0.7890(3) 0.1489(2) 0.09460(16) 0.0198(3) Uani d . 1 C C5 0.7716(3) 0.2461(2) 0.02373(18) 0.0229(4) Uani d . 1 C C6 0.6676(3) -0.2656(2) -0.18583(18) 0.0238(4) Uani d . 1 C C7 0.8415(3) 0.2121(2) 0.24715(17) 0.0226(4) Uani d . 1 C C8 0.6694(4) -0.0314(2) -0.33322(19) 0.0338(5) Uani d . 1 H H3 0.6886 0.0627 -0.3516 0.051 Uiso calc R 1 H H4 0.5329 -0.0931 -0.3805 0.051 Uiso calc R 1 H H5 0.7655 -0.0941 -0.3625 0.051 Uiso calc R 1 C C9 0.7902(4) 0.4225(2) 0.0801(2) 0.0355(5) Uani d . 1 H H6 0.9282 0.4745 0.1336 0.053 Uiso calc R 1 H H7 0.6990 0.4496 0.1351 0.053 Uiso calc R 1 H H8 0.7554 0.4569 0.0077 0.053 Uiso calc R 1 Cu Cu1 1.0000 0.5000 0.5000 0.02310(14) Uani d S 1 H H2 0.721(4) 0.238(3) -0.155(3) 0.030(6) Uiso d . 1 N N1 0.7305(3) 0.17435(19) -0.11146(15) 0.0235(3) Uani d . 1 O O1 0.5859(2) -0.32736(17) -0.31041(14) 0.0317(3) Uani d . 1 O O2 0.7127(3) -0.33730(18) -0.11309(16) 0.0450(5) Uani d . 1 O O3 0.9165(2) 0.35907(16) 0.30890(13) 0.0293(3) Uani d . 1 O O4 0.8096(3) 0.11446(18) 0.29722(14) 0.0387(4) Uani d . 1 O O5 1.1192(3) 0.71981(19) 0.43339(15) 0.0375(4) Uani d . 1 H H9 1.1630 0.7879 0.5144 0.056 Uiso d R 1 H H10 1.0155 0.7392 0.3891 0.056 Uiso d R 1 O O6 0.7361(2) 0.56077(18) 0.47725(14) 0.0319(3) Uani d . 1 H H11 0.6404 0.4837 0.4195 0.048 Uiso d R 1 H H12 0.7001 0.5998 0.5489 0.048 Uiso d R 1 O O7 0.3578(3) 0.65353(17) 0.26093(15) 0.0354(4) Uani d . 1 H H13 0.3389 0.5542 0.2137 0.053 Uiso d R 1 H H14 0.3028 0.6655 0.3245 0.053 Uiso d R 1 O O8 0.7843(4) 0.8023(3) 0.3060(3) 0.0780(8) Uani d . 1 H H15 0.6699 0.7623 0.3112 0.117 Uiso d R 1 H H16 0.7829 0.8950 0.3072 0.117 Uiso d R 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 C1 0.0275(9) 0.0185(8) 0.0177(8) 0.0032(7) 0.0058(7) 0.0035(7) C2 0.0231(8) 0.0157(8) 0.0169(8) 0.0025(6) 0.0047(6) 0.0023(6) C3 0.0236(8) 0.0180(8) 0.0163(8) 0.0032(6) 0.0045(6) 0.0042(6) C4 0.0232(8) 0.0181(8) 0.0139(7) 0.0033(6) 0.0036(6) 0.0028(6) C5 0.0280(9) 0.0169(8) 0.0181(8) 0.0035(7) 0.0048(7) 0.0020(6) C6 0.0301(9) 0.0157(8) 0.0210(8) 0.0038(7) 0.0091(7) 0.0015(7) C7 0.0261(8) 0.0207(8) 0.0153(8) 0.0053(7) 0.0040(7) 0.0019(6) C8 0.0586(14) 0.0235(10) 0.0164(9) 0.0060(9) 0.0101(9) 0.0061(7) C9 0.0600(14) 0.0157(9) 0.0261(9) 0.0080(9) 0.0095(9) 0.0048(7) Cu1 0.0287(2) 0.01893(19) 0.01262(18) 0.00041(12) 0.00377(12) -0.00118(12) N1 0.0339(8) 0.0176(7) 0.0173(7) 0.0046(6) 0.0060(6) 0.0061(6) O1 0.0406(8) 0.0218(7) 0.0193(7) 0.0003(6) 0.0039(6) -0.0024(5) O2 0.0841(13) 0.0178(7) 0.0275(8) 0.0091(7) 0.0088(8) 0.0072(6) O3 0.0415(8) 0.0213(7) 0.0147(6) -0.0010(6) 0.0047(6) -0.0001(5) O4 0.0694(11) 0.0234(7) 0.0189(7) 0.0050(7) 0.0087(7) 0.0074(6) O5 0.0499(9) 0.0329(8) 0.0251(7) 0.0045(7) 0.0116(7) 0.0074(6) O6 0.0313(7) 0.0318(8) 0.0205(6) 0.0031(6) 0.0047(6) -0.0004(6) O7 0.0556(10) 0.0219(7) 0.0323(8) 0.0098(6) 0.0148(7) 0.0131(6) O8 0.0619(13) 0.0559(14) 0.126(2) 0.0135(11) 0.0115(14) 0.0556(15) 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 C1 N1 . 1.354(3) ? C1 C2 . 1.391(3) ? C1 C8 . 1.495(3) ? C2 C3 . 1.390(3) ? C2 C6 . 1.521(3) ? C3 C4 . 1.389(3) ? C3 H1 . 0.9300 ? C4 C5 . 1.389(3) ? C4 C7 . 1.520(3) ? C5 N1 . 1.351(3) ? C5 C9 . 1.491(3) ? C6 O2 . 1.229(3) ? C6 O1 . 1.253(3) ? C7 O4 . 1.238(3) ? C7 O3 . 1.255(2) ? C8 H3 . 0.9600 ? C8 H4 . 0.9600 ? C8 H5 . 0.9600 ? C9 H6 . 0.9600 ? C9 H7 . 0.9600 ? C9 H8 . 0.9600 ? Cu1 O3 . 1.9540(19) yes Cu1 O3 2_766 1.9540(19) ? Cu1 O5 . 2.503(2) yes Cu1 O5 2_766 2.503(2) ? Cu1 O6 2_766 1.951(2) ? Cu1 O6 . 1.951(2) yes N1 H2 . 0.88(3) ? O5 H9 . 0.8501 ? O5 H10 . 0.8500 ? O6 H11 . 0.8500 ? O6 H12 . 0.8500 ? O7 H13 . 0.8500 ? O7 H14 . 0.8500 ? O8 H15 . 0.8500 ? O8 H16 . 0.8500 ? 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 _geom_angle_publ_flag N1 C1 C2 . . 117.47(17) ? N1 C1 C8 . . 115.55(17) ? C2 C1 C8 . . 126.97(17) ? C3 C2 C1 . . 117.87(17) ? C3 C2 C6 . . 118.09(16) ? C1 C2 C6 . . 124.00(16) ? C4 C3 C2 . . 122.71(17) ? C4 C3 H1 . . 118.6 ? C2 C3 H1 . . 118.6 ? C5 C4 C3 . . 118.36(16) ? C5 C4 C7 . . 123.43(16) ? C3 C4 C7 . . 118.20(16) ? N1 C5 C4 . . 117.15(17) ? N1 C5 C9 . . 115.65(17) ? C4 C5 C9 . . 127.20(17) ? O2 C6 O1 . . 126.35(18) ? O2 C6 C2 . . 116.60(17) ? O1 C6 C2 . . 117.04(17) ? O4 C7 O3 . . 127.02(17) ? O4 C7 C4 . . 117.36(17) ? O3 C7 C4 . . 115.61(16) ? C1 C8 H3 . . 109.5 ? C1 C8 H4 . . 109.5 ? H3 C8 H4 . . 109.5 ? C1 C8 H5 . . 109.5 ? H3 C8 H5 . . 109.5 ? H4 C8 H5 . . 109.5 ? C5 C9 H6 . . 109.5 ? C5 C9 H7 . . 109.5 ? H6 C9 H7 . . 109.5 ? C5 C9 H8 . . 109.5 ? H6 C9 H8 . . 109.5 ? H7 C9 H8 . . 109.5 ? O6 Cu1 O6 2_766 . 180.0 yes O6 Cu1 O3 2_766 . 90.78(7) ? O6 Cu1 O3 . . 89.22(7) yes O6 Cu1 O3 2_766 2_766 89.22(7) ? O6 Cu1 O3 . 2_766 90.78(7) yes O3 Cu1 O3 . 2_766 180.0000(10) yes O6 Cu1 O5 2_766 . 93.58(7) ? O6 Cu1 O5 . . 86.42(7) yes O3 Cu1 O5 . . 87.26(8) yes O3 Cu1 O5 2_766 . 92.74(8) ? O6 Cu1 O5 2_766 2_766 86.42(7) ? O6 Cu1 O5 . 2_766 93.58(7) yes O3 Cu1 O5 . 2_766 92.74(8) yes O3 Cu1 O5 2_766 2_766 87.26(8) ? O5 Cu1 O5 . 2_766 180.0 ? C5 N1 C1 . . 126.36(16) ? C5 N1 H2 . . 116.0(17) ? C1 N1 H2 . . 117.6(17) ? C7 O3 Cu1 . . 132.29(13) ? Cu1 O5 H9 . . 93.0 ? Cu1 O5 H10 . . 108.6 ? H9 O5 H10 . . 112.3 ? Cu1 O6 H11 . . 112.1 ? Cu1 O6 H12 . . 115.5 ? H11 O6 H12 . . 108.5 ? H13 O7 H14 . . 108.6 ? H15 O8 H16 . . 109.4 ? 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 O8 H16 O4 1_565 0.85 2.05 2.896(3) 172.3 O8 H15 O7 . 0.85 2.11 2.935(4) 162.1 O7 H14 O5 1_455 0.85 1.92 2.735(3) 160.9 O7 H13 O2 2_655 0.85 1.85 2.695(3) 177.5 O6 H12 O1 1_566 0.85 1.85 2.690(3) 172.2 O6 H11 O1 2_655 0.85 1.83 2.673(3) 172.4 O5 H10 O8 . 0.85 1.92 2.765(3) 174.0 O5 H9 O4 2_766 0.85 1.91 2.721(3) 159.1 N1 H2 O7 2_665 0.88(3) 1.84(3) 2.707(3) 167(2) _cod_database_fobs_code 2212426 _journal_paper_doi 10.1107/S1600536807000669