#------------------------------------------------------------------------------ #$Date: 2013-12-28 13:58:47 +0000 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/29/2012941.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_2012941 loop_ _publ_author_name 'Ruschewitz, Uwe' 'Pantenburg, Ingo' _publ_section_title ; [Cd{C~2~(COO)~2~}(H~2~O)~3~]·H~2~O, the first cadmium salt of acetylenedicarboxylic acid ; _journal_issue 9 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m483 _journal_page_last m484 _journal_volume 58 _journal_year 2002 _chemical_formula_iupac '[Cd (C4 O4) (H2 O)3] , H2 O' _chemical_formula_moiety 'C4 H6 Cd O7 , H2 O' _chemical_formula_sum 'C4 H8 Cd O8' _chemical_formula_weight 296.50 _chemical_name_common 'cadmium acetylenedicarboxylate tetrahydrate' _chemical_name_systematic ;catena-poly[[[triaquacadmium(II)]-\m-acetylenedicarboxylato-\k^4^O,O':O'',O'''] monohydrate] ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL97 _cell_angle_alpha 90 _cell_angle_beta 99.811(8) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 6.8195(7) _cell_length_b 7.9530(10) _cell_length_c 16.387(2) _cell_measurement_reflns_used 19461 _cell_measurement_temperature 170(2) _cell_measurement_theta_max 32.4 _cell_measurement_theta_min 1.5 _cell_volume 875.76(18) _computing_cell_refinement X-AREA _computing_data_collection 'X-AREA (Stoe & Cie, 2001)' _computing_data_reduction X-AREA _computing_molecular_graphics 'DIAMOND (Brandenburg, 2001)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _diffrn_ambient_temperature 170(2) _diffrn_detector_area_resol_mean 'not measured' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method 'oscillation 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 0.046 _diffrn_reflns_av_sigmaI/netI 0.020 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 16485 _diffrn_reflns_theta_full 27.00 _diffrn_reflns_theta_max 27.00 _diffrn_reflns_theta_min 2.52 _diffrn_standards_decay_% 'not measured' _diffrn_standards_interval_count 'not measured' _diffrn_standards_interval_time 'not measured' _diffrn_standards_number 'not measured' _exptl_absorpt_coefficient_mu 2.508 _exptl_absorpt_correction_T_max 0.785 _exptl_absorpt_correction_T_min 0.242 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details '(X-RED; Stoe & Cie, 2001)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.249 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description column _exptl_crystal_F_000 576 _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.13 _refine_diff_density_max 0.40 _refine_diff_density_min -0.40 _refine_ls_extinction_coef 0.0049(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL97 (Sheldrick, 1997)' _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 151 _refine_ls_number_reflns 1912 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.083 _refine_ls_R_factor_all 0.028 _refine_ls_R_factor_gt 0.020 _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^)+(0.0225P)^2^+0.4864P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.047 _refine_ls_wR_factor_ref 0.048 _reflns_number_gt 1545 _reflns_number_total 1912 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file jz1517.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/n' _cod_original_cell_volume 875.74(17) _cod_database_code 2012941 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _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 _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Cd1 0.69040(2) 0.00390(2) 0.367930(10) 0.01726(9) Uani d . 1 . . Cd C11 0.9654(4) 0.4366(3) 0.4840(2) 0.0183(5) Uani d . 1 . . C C12 0.8755(4) 0.2815(3) 0.4472(2) 0.0192(5) Uani d . 1 . . C O121 0.8372(3) 0.2717(2) 0.36923(11) 0.0245(4) Uani d . 1 . . O O122 0.8368(3) 0.1659(2) 0.49343(11) 0.0230(4) Uani d . 1 . . O C21 0.5167(4) -0.4423(3) 0.4791(2) 0.0205(6) Uani d . 1 . . C C22 0.5639(4) -0.2972(3) 0.4307(2) 0.0210(5) Uani d . 1 . . C O221 0.5180(3) -0.2977(3) 0.35428(12) 0.0298(5) Uani d . 1 . . O O222 0.6546(3) -0.1760(2) 0.47104(11) 0.0229(4) Uani d . 1 . . O O3 0.3880(3) 0.1224(3) 0.3695(2) 0.0240(4) Uani d . 1 . . O H31 0.371(5) 0.199(5) 0.343(2) 0.026(9) Uiso d . 1 . . H H32 0.371(6) 0.143(5) 0.411(3) 0.043(12) Uiso d . 1 . . H O4 0.9636(3) -0.1499(3) 0.34812(14) 0.0224(4) Uani d . 1 . . O H41 1.038(5) -0.159(4) 0.390(2) 0.031(9) Uiso d . 1 . . H H42 1.029(7) -0.121(6) 0.316(3) 0.07(2) Uiso d . 1 . . H O5 0.5837(3) 0.0220(3) 0.22886(12) 0.0234(4) Uani d . 1 . . O H51 0.585(5) 0.108(6) 0.206(2) 0.046(12) Uiso d . 1 . . H H52 0.625(5) -0.053(5) 0.198(2) 0.040(11) Uiso d . 1 . . H O6 1.1559(4) -0.0807(3) 0.22012(13) 0.0255(5) Uani d . 1 . . O H61 1.092(6) 0.012(5) 0.196(3) 0.047(11) Uiso d . 1 . . H H62 1.256(7) -0.052(6) 0.236(3) 0.06(2) Uiso d . 1 . . H 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 0.02422(13) 0.01310(11) 0.01410(11) -0.00283(8) 0.00228(7) -0.00024(7) C11 0.0200(14) 0.0171(11) 0.0170(13) -0.0003(9) 0.0013(10) 0.0014(9) C12 0.0199(13) 0.0157(12) 0.0212(13) -0.0008(10) 0.0016(10) -0.0020(10) O121 0.0379(11) 0.0186(9) 0.0166(10) -0.0096(8) 0.0037(8) -0.0022(7) O122 0.0310(11) 0.0163(9) 0.0200(9) -0.0064(8) -0.0007(8) 0.0026(7) C21 0.0232(14) 0.0174(12) 0.0220(14) -0.0007(10) 0.0073(11) 0.0000(9) C22 0.0240(13) 0.0153(12) 0.0257(14) 0.0015(10) 0.0100(11) 0.0025(10) O221 0.0450(12) 0.0249(10) 0.0192(10) -0.0085(9) 0.0045(9) 0.0039(8) O222 0.0338(11) 0.0146(8) 0.0221(10) -0.0061(8) 0.0096(8) -0.0006(7) O3 0.0320(12) 0.0218(11) 0.0185(11) 0.0039(8) 0.0053(9) -0.0001(9) O4 0.0261(11) 0.0231(10) 0.0175(10) 0.0017(8) 0.0022(9) 0.0024(8) O5 0.0378(12) 0.0182(10) 0.0146(9) 0.0020(9) 0.0057(8) 0.0002(8) O6 0.0255(12) 0.0265(11) 0.0231(11) -0.0020(9) 0.0001(9) 0.0006(9) 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 O222 . 2.259(2) yes Cd1 O3 . 2.272(2) yes Cd1 O5 . 2.276(2) yes Cd1 O4 . 2.298(2) yes Cd1 O121 . 2.352(2) yes Cd1 O122 . 2.487(2) yes Cd1 O221 . 2.664(2) yes C11 C11 3_766 1.197(5) yes C11 C12 . 1.461(3) yes C12 O122 . 1.247(3) yes C12 O121 . 1.262(3) yes C21 C21 3_646 1.189(5) yes C21 C22 . 1.468(4) yes C22 O221 . 1.237(3) yes C22 O222 . 1.269(3) yes O3 H31 . 0.75(4) no O3 H32 . 0.72(4) no O4 H41 . 0.78(4) no O4 H42 . 0.77(5) no O5 H51 . 0.78(4) no O5 H52 . 0.86(4) no O6 H61 . 0.91(4) no O6 H62 . 0.73(5) no 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' 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 _geom_angle_publ_flag O121 Cd1 O122 . 54.07(6) yes O221 Cd1 O222 . 52.42(6) yes O221 Cd1 O4 . 82.28(7) yes O221 Cd1 O122 . 130.17(6) yes O221 Cd1 O121 . 175.75(6) yes O221 Cd1 O3 . 89.19(7) yes O221 Cd1 O5 . 84.92(7) yes O222 Cd1 O3 . 92.29(8) yes O222 Cd1 O5 . 137.07(7) yes O222 Cd1 O4 . 87.83(8) yes O222 Cd1 O121 . 131.83(6) yes O222 Cd1 O122 . 77.81(6) yes O3 Cd1 O5 . 81.34(8) yes O3 Cd1 O4 . 169.15(7) yes O3 Cd1 O121 . 90.57(8) yes O3 Cd1 O122 . 90.73(7) yes O4 Cd1 O121 . 97.43(7) yes O4 Cd1 O122 . 99.89(7) yes O5 Cd1 O4 . 91.19(8) yes O5 Cd1 O121 . 90.85(7) yes O5 Cd1 O122 . 144.11(7) yes C11 C11 C12 3_766 177.7(4) yes O122 C12 O121 . 122.7(2) yes O122 C12 C11 . 119.3(2) no O121 C12 C11 . 118.0(2) no C21 C21 C22 3_646 177.6(4) yes O221 C22 O222 . 123.1(2) yes O221 C22 C21 . 120.3(2) no O222 C22 C21 . 116.6(2) no H31 O3 H32 . 109(4) no H41 O4 H42 . 105(4) no H51 O5 H52 . 107(4) no H61 O6 H62 . 105(4) no 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 _geom_hbond_publ_flag O3 H31 O6 2_655 0.75(4) 2.03(4) 2.770(3) 175(4) yes O3 H32 O222 3_656 0.72(4) 1.99(4) 2.711(3) 173(4) yes O4 H41 O122 3_756 0.78(4) 1.96(4) 2.722(3) 165(3) yes O4 H42 O6 . 0.77(5) 1.95(5) 2.713(3) 167(5) yes O5 H51 O4 2_655 0.78(4) 2.12(5) 2.892(3) 169(4) yes O5 H52 O121 2_645 0.86(4) 1.82(4) 2.670(3) 169(3) yes O6 H61 O221 2_655 0.91(4) 1.83(4) 2.732(3) 175(4) yes O6 H62 O5 1_655 0.73(5) 2.33(5) 3.009(3) 156(5) yes O6 H62 O3 1_655 0.73(5) 2.62(5) 3.129(3) 129(4) yes _cod_database_fobs_code 2012941 _journal_paper_doi 10.1107/S0108270102014658