#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2206872.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_2206872 loop_ _publ_author_name 'Yang, Yang-Yi' 'Zai, Shao-Bo' 'Wong, Wing-Tak' 'Ng, Seik Weng' _publ_section_title ; Poly[dimethylammonium aquadi-\m-oxalato-europate(III) trihydrate] ; _journal_coeditor_code BT6728 _journal_issue 10 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m1912 _journal_page_last m1914 _journal_volume 61 _journal_year 2005 _chemical_formula_iupac '(C2 H8 N) [Eu (C2 O4)2 (H2 O)] , 3H2 O' _chemical_formula_moiety 'C2 H8 N + , C4 H2 Eu O9 - , 3H2 O' _chemical_formula_sum 'C6 H16 Eu N O12' _chemical_formula_weight 446.16 _chemical_name_systematic ; Poly[dimethylammonium aquadi-\m-oxalato-europate(III) trihydrate] ; _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 99.285(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.6740(10) _cell_length_b 11.7610(10) _cell_length_c 12.315(2) _cell_measurement_reflns_used 885 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 27.2 _cell_measurement_theta_min 2.4 _cell_volume 1382.8(3) _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_collection 'SMART (Bruker, 2000)' _computing_data_reduction SAINT _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 295(2) _diffrn_measured_fraction_theta_full 0.98 _diffrn_measured_fraction_theta_max 0.98 _diffrn_measurement_device_type 'Bruker SMART 1000 area-detector' _diffrn_measurement_method '\f and \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 0.026 _diffrn_reflns_av_sigmaI/netI 0.032 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 8455 _diffrn_reflns_theta_full 27.5 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_min 2.4 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 4.596 _exptl_absorpt_correction_T_max 0.803 _exptl_absorpt_correction_T_min 0.702 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour Colourless _exptl_crystal_density_diffrn 2.143 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Block _exptl_crystal_F_000 872 _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _refine_diff_density_max 1.07 _refine_diff_density_min -0.42 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.99 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 212 _refine_ls_number_reflns 3113 _refine_ls_number_restraints 15 _refine_ls_restrained_S_all 0.99 _refine_ls_R_factor_all 0.036 _refine_ls_R_factor_gt 0.026 _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^)+(0.0359P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.058 _refine_ls_wR_factor_ref 0.062 _reflns_number_gt 2578 _reflns_number_total 3113 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file bt6728.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/n' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2206872 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_type_symbol Eu1 0.71368(2) 0.515520(10) 0.330810(10) 0.02102(7) Uani d . 1 Eu O1 0.8070(3) 0.6409(2) 0.2055(2) 0.0272(6) Uani d . 1 O O2 0.8660(3) 0.8194(2) 0.1726(2) 0.0253(6) Uani d . 1 O O3 0.6396(3) 0.7159(2) 0.3435(2) 0.0288(6) Uani d . 1 O O4 0.6851(3) 0.8950(2) 0.3006(2) 0.0318(6) Uani d . 1 O O5 0.6813(3) 0.5115(2) 0.5224(2) 0.0305(6) Uani d . 1 O O6 0.5335(3) 0.4854(2) 0.6428(2) 0.0263(6) Uani d . 1 O O7 0.9160(3) 0.6182(2) 0.4341(2) 0.0306(6) Uani d . 1 O O8 1.1006(3) 0.6088(2) 0.5673(2) 0.0347(7) Uani d . 1 O O1W 0.5452(3) 0.5236(3) 0.1537(2) 0.0374(7) Uani d D 1 O O2W 0.4196(5) 0.3424(3) 0.0340(3) 0.0660(10) Uani d D 1 O O3W 0.1705(6) 0.5038(4) 0.0076(3) 0.0790(10) Uani d D 1 O O4W 0.0859(5) 0.2816(4) 0.0322(4) 0.0770(10) Uani d D 1 O N1 0.2682(5) 0.6312(4) 0.1956(4) 0.0510(10) Uani d D 1 N C1 0.8002(4) 0.7455(3) 0.2175(3) 0.0220(7) Uani d . 1 C C2 0.6990(4) 0.7897(3) 0.2946(3) 0.0225(8) Uani d . 1 C C3 0.5625(4) 0.4992(3) 0.5474(3) 0.0219(7) Uani d . 1 C C4 1.0046(4) 0.5657(3) 0.4997(3) 0.0256(8) Uani d . 1 C C5 0.1511(7) 0.6242(7) 0.2548(5) 0.084(2) Uani d . 1 C C6 0.3064(8) 0.7458(6) 0.1680(5) 0.087(2) Uani d . 1 C H1W1 0.514(5) 0.462(2) 0.122(3) 0.045 Uiso d D 1 H H1W2 0.572(4) 0.568(2) 0.107(2) 0.045 Uiso d D 1 H H2W1 0.334(2) 0.355(4) 0.014(5) 0.079 Uiso d D 1 H H2W2 0.435(5) 0.2730(10) 0.046(5) 0.079 Uiso d D 1 H H3W1 0.160(6) 0.543(4) -0.051(3) 0.095 Uiso d D 1 H H3W2 0.121(6) 0.445(3) -0.001(5) 0.095 Uiso d D 1 H H4W1 0.077(6) 0.253(5) -0.032(2) 0.093 Uiso d D 1 H H4W2 0.017(4) 0.262(5) 0.063(4) 0.093 Uiso d D 1 H H1N1 0.252(5) 0.589(3) 0.139(2) 0.061 Uiso d D 1 H H1N2 0.338(4) 0.605(4) 0.240(3) 0.061 Uiso d D 1 H H5A 0.1756 0.6599 0.3254 0.127 Uiso calc R 1 H H5B 0.1283 0.5459 0.2646 0.127 Uiso calc R 1 H H5C 0.0717 0.6623 0.2137 0.127 Uiso calc R 1 H H6A 0.2260 0.7835 0.1280 0.130 Uiso calc R 1 H H6B 0.3792 0.7424 0.1236 0.130 Uiso calc R 1 H H6C 0.3394 0.7871 0.2344 0.130 Uiso calc R 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 Eu1 0.02400(10) 0.01770(10) 0.02220(10) 0.00010(10) 0.00630(10) 0.00020(10) O1 0.039(2) 0.0160(10) 0.0300(10) 0.0010(10) 0.0150(10) -0.0010(10) O2 0.024(2) 0.0210(10) 0.033(2) 0.0010(10) 0.0100(10) 0.0040(10) O3 0.035(2) 0.0210(10) 0.035(2) 0.0010(10) 0.0190(10) 0.0030(10) O4 0.048(2) 0.0180(10) 0.034(2) 0.0010(10) 0.0200(10) 0.0010(10) O5 0.0230(10) 0.043(2) 0.0260(10) -0.0030(10) 0.0050(10) -0.0010(10) O6 0.0250(10) 0.0340(10) 0.0200(10) 0.0020(10) 0.0040(10) 0.0020(10) O7 0.032(2) 0.0230(10) 0.036(2) -0.0030(10) 0.0010(10) 0.0070(10) O8 0.032(2) 0.0230(10) 0.045(2) 0.0020(10) -0.0060(10) -0.0070(10) O1W 0.043(2) 0.042(2) 0.028(2) -0.0060(10) 0.0050(10) 0.0010(10) O2W 0.093(3) 0.038(2) 0.068(3) 0.000(2) 0.010(2) -0.007(2) O3W 0.124(4) 0.073(3) 0.045(2) -0.021(3) 0.023(3) 0.002(2) O4W 0.113(4) 0.059(3) 0.072(3) -0.018(2) 0.051(3) -0.013(2) N1 0.043(3) 0.065(3) 0.046(3) 0.019(2) 0.011(2) 0.011(2) C1 0.024(2) 0.024(2) 0.018(2) 0.0000(10) 0.002(2) 0.0020(10) C2 0.025(2) 0.021(2) 0.021(2) 0.0020(10) 0.004(2) 0.0000(10) C3 0.026(2) 0.017(2) 0.023(2) -0.0010(10) 0.005(2) 0.0000(10) C4 0.024(2) 0.027(2) 0.027(2) 0.001(2) 0.009(2) -0.002(2) C5 0.061(4) 0.136(7) 0.060(4) 0.029(4) 0.019(3) 0.019(4) C6 0.098(6) 0.063(4) 0.097(5) -0.002(4) 0.007(4) 0.019(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' 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' Eu Eu -0.1578 3.6682 '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 _geom_angle_publ_flag O1 Eu1 O2 . 2_645 136.00(10) yes O1 Eu1 O3 . . 66.40(10) yes O1 Eu1 O4 . 2_645 72.70(10) yes O1 Eu1 O5 . . 138.90(10) yes O1 Eu1 O6 . 3_666 123.90(10) yes O1 Eu1 O7 . . 71.50(10) yes O1 Eu1 O8 . 3_766 111.50(10) yes O1 Eu1 O1W . . 71.20(10) yes O2 Eu1 O3 2_645 . 144.20(10) yes O2 Eu1 O4 2_645 2_645 66.50(10) yes O2 Eu1 O5 2_645 . 84.70(10) yes O2 Eu1 O6 2_645 3_666 71.70(10) yes O2 Eu1 O7 2_645 . 134.10(10) yes O2 Eu1 O8 2_645 3_766 69.70(10) yes O2 Eu1 O1W 2_645 . 82.00(10) yes O3 Eu1 O4 . 2_645 137.50(10) yes O3 Eu1 O5 . . 82.70(10) yes O3 Eu1 O6 . 3_666 72.50(10) yes O3 Eu1 O7 . . 73.50(10) yes O3 Eu1 O8 . 3_766 136.00(10) yes O3 Eu1 O1W . . 82.20(10) yes O4 Eu1 O5 2_645 . 138.70(10) yes O4 Eu1 O6 2_645 3_666 125.40(10) yes O4 Eu1 O7 2_645 . 104.70(10) yes O4 Eu1 O8 2_645 3_766 70.30(10) yes O4 Eu1 O1W 2_645 . 73.90(10) yes O5 Eu1 O6 . 3_666 65.90(10) yes O5 Eu1 O7 . . 74.10(10) yes O5 Eu1 O8 . 3_766 72.30(10) yes O5 Eu1 O1W . . 132.70(10) yes O6 Eu1 O7 3_666 . 129.70(10) yes O6 Eu1 O8 3_666 3_766 124.50(10) yes O6 Eu1 O1W 3_666 . 66.80(10) yes O7 Eu1 O8 . 3_766 65.20(10) yes O7 Eu1 O1W . . 141.20(10) yes O8 Eu1 O1W 3_766 . 140.90(10) yes C1 O1 Eu1 . . 119.8(2) no C1 O2 Eu1 . 2_655 118.9(2) no C2 O3 Eu1 . . 118.1(2) no C2 O4 Eu1 . 2_655 118.3(2) no C3 O5 Eu1 . . 120.8(2) no C3 O6 Eu1 . 3_666 119.3(2) no C4 O7 Eu1 . . 119.8(2) no C4 O8 Eu1 . 3_766 119.7(2) no C5 N1 C6 . . 114.9(5) no O1 C1 O2 . . 126.4(3) no O1 C1 C2 . . 116.9(3) no O2 C1 C2 . . 116.7(3) no O3 C2 O4 . . 126.8(3) no O3 C2 C1 . . 116.4(3) no O4 C2 C1 . . 116.7(3) no O5 C3 O6 . . 126.8(3) no O5 C3 C3 . 3_666 117.0(4) no O6 C3 C3 . 3_666 116.3(4) no O7 C4 O8 . . 126.2(4) no O7 C4 C4 . 3_766 117.7(4) no O8 C4 C4 . 3_766 116.1(4) no Eu1 O1W H1W1 . . 120(3) no Eu1 O1W H1W2 . . 113(3) no H1W1 O1W H1W2 . . 110(2) no H2W1 O2W H2W2 . . 111(2) no H3W1 O3W H3W2 . . 111(2) no H4W1 O4W H4W2 . . 109(2) no C5 N1 H1N1 . . 109(4) no C6 N1 H1N1 . . 112(4) no C5 N1 H1N2 . . 105(4) no C6 N1 H1N2 . . 106(4) no H1N1 N1 H1N2 . . 110(2) no N1 C5 H5A . . 109.5 no N1 C5 H5B . . 109.5 no H5A C5 H5B . . 109.5 no N1 C5 H5C . . 109.5 no H5A C5 H5C . . 109.5 no H5B C5 H5C . . 109.5 no N1 C6 H6A . . 109.5 no N1 C6 H6B . . 109.5 no H6A C6 H6B . . 109.5 no N1 C6 H6C . . 109.5 no H6A C6 H6C . . 109.5 no H6B C6 H6C . . 109.5 no 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 Eu1 O1 . 2.412(2) yes Eu1 O2 2_645 2.430(2) yes Eu1 O3 . 2.476(2) yes Eu1 O4 2_645 2.469(2) yes Eu1 O5 . 2.430(3) yes Eu1 O6 3_666 2.465(3) yes Eu1 O7 . 2.471(3) yes Eu1 O8 3_766 2.492(3) yes Eu1 O1W . 2.505(3) yes O1 C1 . 1.242(4) no O2 C1 . 1.257(4) no O3 C2 . 1.247(4) no O4 C2 . 1.249(4) no O5 C3 . 1.245(4) no O6 C3 . 1.261(4) no O7 C4 . 1.244(4) no O8 C4 . 1.250(4) no N1 C5 . 1.445(7) no N1 C6 . 1.452(8) no C1 C2 . 1.560(5) no C3 C3 3_666 1.540(7) no C4 C4 3_766 1.547(8) no O1W H1W1 . 0.850(10) no O1W H1W2 . 0.850(10) no O2W H2W1 . 0.840(10) no O2W H2W2 . 0.850(10) no O3W H3W1 . 0.850(10) no O3W H3W2 . 0.840(10) no O4W H4W1 . 0.850(10) no O4W H4W2 . 0.850(10) no N1 H1N1 . 0.850(10) no N1 H1N2 . 0.850(10) no C5 H5A . 0.96 no C5 H5B . 0.96 no C5 H5C . 0.96 no C6 H6A . 0.96 no C6 H6B . 0.96 no C6 H6C . 0.96 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 O1W H1W1 O2W . 0.850(10) 1.920(10) 2.759(5) 169(4) yes O1W H1W2 O2W 3_665 0.850(10) 2.05(2) 2.862(5) 162(4) yes O2W H2W2 O7 2_645 0.850(10) 2.30(2) 3.071(5) 151(4) yes O2W H2W2 O8 2_645 0.850(10) 2.37(4) 3.011(4) 133(5) yes O3W H3W1 O4 4_575 0.850(10) 2.02(2) 2.838(5) 162(7) yes O3W H3W2 O4W . 0.840(10) 2.00(3) 2.770(6) 151(5) yes O4W H4W1 O2 3_665 0.850(10) 2.08(2) 2.893(4) 159(5) yes O4W H4W2 O3 2_545 0.850(10) 2.120(10) 2.962(5) 173(5) yes N1 H1N1 O3W . 0.850(10) 1.960(10) 2.792(6) 167(4) yes N1 H1N2 O6 3_666 0.850(10) 2.05(2) 2.879(5) 165(5) 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_site_symmetry_1 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag O5 Eu1 O1 C1 . . -31.3(3) no O2 Eu1 O1 C1 2_645 . 158.8(2) no O6 Eu1 O1 C1 3_666 . 60.0(3) no O4 Eu1 O1 C1 2_645 . -178.5(3) no O7 Eu1 O1 C1 . . -65.9(3) no O3 Eu1 O1 C1 . . 13.6(3) no O8 Eu1 O1 C1 3_766 . -118.6(3) no O1W Eu1 O1 C1 . . 103.1(3) no O1 Eu1 O3 C2 . . -10.8(3) no O5 Eu1 O3 C2 . . 141.3(3) no O2 Eu1 O3 C2 2_645 . -148.2(2) no O6 Eu1 O3 C2 3_666 . -151.7(3) no O4 Eu1 O3 C2 2_645 . -27.9(3) no O7 Eu1 O3 C2 . . 65.9(3) no O8 Eu1 O3 C2 3_766 . 86.4(3) no O1W Eu1 O3 C2 . . -83.6(3) no O1 Eu1 O5 C3 . . 122.0(2) no O2 Eu1 O5 C3 2_645 . -65.0(3) no O6 Eu1 O5 C3 3_666 . 7.3(2) no O4 Eu1 O5 C3 2_645 . -109.7(3) no O7 Eu1 O5 C3 . . 156.1(3) no O3 Eu1 O5 C3 . . 81.3(3) no O8 Eu1 O5 C3 3_766 . -135.4(3) no O1W Eu1 O5 C3 . . 9.0(3) no O1 Eu1 O7 C4 . . -135.5(3) no O5 Eu1 O7 C4 . . 67.4(3) no O2 Eu1 O7 C4 2_645 . 1.6(3) no O6 Eu1 O7 C4 3_666 . 105.3(3) no O4 Eu1 O7 C4 2_645 . -69.8(3) no O3 Eu1 O7 C4 . . 154.4(3) no O8 Eu1 O7 C4 3_766 . -10.0(3) no O1W Eu1 O7 C4 . . -152.2(2) no Eu1 O1 C1 O2 . . 165.9(3) no Eu1 O1 C1 C2 . . -14.9(4) no Eu1 O2 C1 O1 2_655 . 163.0(3) no Eu1 O2 C1 C2 2_655 . -16.2(4) no Eu1 O3 C2 O4 . . -172.5(3) no Eu1 O3 C2 C1 . . 7.9(4) no Eu1 O4 C2 O3 2_655 . -169.7(3) no Eu1 O4 C2 C1 2_655 . 9.9(4) no O1 C1 C2 O3 . . 4.4(5) no O2 C1 C2 O3 . . -176.3(3) no Eu1 C1 C2 O3 2_655 . 172.8(3) no O1 C1 C2 O4 . . -175.2(3) no O2 C1 C2 O4 . . 4.1(5) no Eu1 C1 C2 O4 2_655 . -6.8(3) no Eu1 O5 C3 O6 . . 173.0(3) no Eu1 O5 C3 C3 . 3_666 -6.8(5) no Eu1 O6 C3 O5 3_666 . 173.3(3) no Eu1 O6 C3 C3 3_666 3_666 -6.8(5) no Eu1 O7 C4 O8 . . -169.8(3) no Eu1 O7 C4 C4 . 3_766 9.1(5) no Eu1 O8 C4 O7 3_766 . -170.6(3) no Eu1 O8 C4 C4 3_766 3_766 10.4(5) no