#------------------------------------------------------------------------------ #$Date: 2013-08-29 16:37:19 +0100 (Thu, 29 Aug 2013) $ #$Revision: 88064 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/27/2012708.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_2012708 loop_ _publ_author_name 'Wu, Chuan-De' 'Lu, Can-Zhong' 'Zhuang, Hong-Hui' 'Huang, Jin-Shun' _publ_section_title ; Polymeric aqua(nitrilotriacetato)erbium(III) ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m283 _journal_page_last m285 _journal_volume 58 _journal_year 2002 _chemical_formula_iupac '[Er (C6 H6 N O6) (H2 O)]' _chemical_formula_moiety 'C6 H8 Er N O7' _chemical_formula_sum 'C6 H8 Er N O7' _chemical_formula_weight 373.39 _chemical_name_systematic ; Polymeric aqua(nitrilotriacetato)erbium(III) ; _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 geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL97 _cell_angle_alpha 90 _cell_angle_beta 93.444(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 6.7262(6) _cell_length_b 6.5427(4) _cell_length_c 19.800(2) _cell_measurement_reflns_used 920 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 25.06 _cell_measurement_theta_min 2.06 _cell_volume 869.78(13) _computing_cell_refinement 'SMART and SAINT (Siemens, 1994)' _computing_data_collection 'SMART (Siemens, 1996)' _computing_data_reduction 'SMART and SAINT' _computing_molecular_graphics 'SHELXTL (Siemens, 1994)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.986 _diffrn_measured_fraction_theta_max 0.986 _diffrn_measurement_device_type 'Bruker SMART CCD area-detector' _diffrn_measurement_method '\f and \w 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 0.033 _diffrn_reflns_av_sigmaI/netI 0.035 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 2640 _diffrn_reflns_theta_full 25.06 _diffrn_reflns_theta_max 25.06 _diffrn_reflns_theta_min 2.06 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 9.668 _exptl_absorpt_correction_T_max 0.560 _exptl_absorpt_correction_T_min 0.328 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour red _exptl_crystal_density_diffrn 2.852 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 700 _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _refine_diff_density_max 0.83 _refine_diff_density_min -1.04 _refine_ls_extinction_coef 0.0110(5) _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 1.088 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 137 _refine_ls_number_reflns 1520 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.088 _refine_ls_R_factor_all 0.038 _refine_ls_R_factor_gt 0.032 _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^)+(0.0119P)^2^+12.9152P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.067 _refine_ls_wR_factor_ref 0.072 _reflns_number_gt 1340 _reflns_number_total 1520 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file ln1137.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_enum 1527 2010-12-29 10:47:43Z saulius 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_original_cell_volume 869.80(10) _cod_database_code 2012708 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 Er 0.23184(5) 0.23483(5) 0.104751(17) 0.01708(19) Uani d . 1 . . Er O1 0.5554(9) 0.1790(10) 0.0721(3) 0.0291(14) Uani d . 1 . . O O2 0.8855(8) 0.1769(9) 0.0918(3) 0.0271(13) Uani d . 1 . . O O3 0.1142(9) 0.4405(10) 0.1927(3) 0.0276(14) Uani d . 1 . . O O4 0.1656(9) 0.5791(9) 0.2944(3) 0.0273(14) Uani d . 1 . . O O5 0.2049(10) 0.8897(9) 0.0817(3) 0.0310(15) Uani d . 1 . . O O6 0.1748(9) 0.5596(9) 0.0618(3) 0.0261(13) Uani d . 1 . . O O7 0.1781(9) 0.2084(9) -0.0129(3) 0.0282(13) Uani d . 1 . . O H7A 0.1576 0.3224 -0.0291 0.034 Uiso calc R 1 . . H H7B 0.0875 0.1206 -0.0315 0.034 Uiso d R 1 . . H N 0.4906(10) 0.4853(11) 0.1587(4) 0.0230(15) Uani d . 1 . . N C1 0.6957(12) 0.3993(14) 0.1572(5) 0.028(2) Uani d . 1 . . C H1A 0.7326 0.3374 0.2007 0.033 Uiso calc R 1 . . H H1B 0.7887 0.5094 0.1500 0.033 Uiso calc R 1 . . H C2 0.7122(12) 0.2421(12) 0.1025(4) 0.0235(18) Uani d . 1 . . C C3 0.4438(13) 0.5275(15) 0.2284(4) 0.0266(19) Uani d . 1 . . C H3A 0.4934 0.6623 0.2409 0.032 Uiso calc R 1 . . H H3B 0.5129 0.4292 0.2579 0.032 Uiso calc R 1 . . H C4 0.2283(13) 0.5187(12) 0.2395(4) 0.0227(19) Uani d . 1 . . C C5 0.4784(13) 0.6706(13) 0.1159(5) 0.0285(19) Uani d . 1 . . C H5A 0.5686 0.6558 0.0798 0.034 Uiso calc R 1 . . H H5B 0.5222 0.7875 0.1430 0.034 Uiso calc R 1 . . H C6 0.2723(14) 0.7115(13) 0.0854(4) 0.0268(19) Uani d . 1 . . C 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 Er 0.0157(2) 0.0137(2) 0.0217(2) 0.00028(14) 0.00030(13) -0.00050(14) O1 0.018(3) 0.033(3) 0.036(3) 0.002(3) 0.000(3) -0.009(3) O2 0.017(3) 0.026(3) 0.040(3) 0.002(3) 0.005(3) -0.007(3) O3 0.020(3) 0.034(4) 0.029(3) 0.001(3) 0.000(2) -0.004(3) O4 0.028(3) 0.029(3) 0.025(3) -0.006(3) -0.002(3) -0.003(3) O5 0.039(4) 0.020(3) 0.033(3) 0.002(3) -0.008(3) 0.001(3) O6 0.035(4) 0.016(3) 0.026(3) 0.000(3) -0.009(3) 0.003(2) O7 0.030(3) 0.027(3) 0.028(3) -0.003(3) 0.004(3) -0.003(3) N 0.016(3) 0.023(4) 0.030(4) 0.000(3) 0.003(3) -0.005(3) C1 0.016(4) 0.025(4) 0.042(5) 0.005(3) -0.004(4) -0.006(4) C2 0.017(4) 0.022(4) 0.032(5) -0.001(4) 0.008(4) 0.001(4) C3 0.021(4) 0.033(5) 0.026(4) 0.000(4) -0.002(4) -0.011(4) C4 0.036(5) 0.016(4) 0.016(4) 0.000(4) -0.001(4) 0.002(3) C5 0.028(5) 0.023(4) 0.034(5) -0.007(4) 0.001(4) -0.003(4) C6 0.035(5) 0.019(5) 0.026(4) 0.001(4) 0.001(4) 0.001(3) 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 Er O1 . 2.336(6) yes Er O2 1_455 2.359(6) yes Er O3 . 2.373(6) yes Er O4 2_545 2.310(6) yes Er O5 1_545 2.309(6) yes Er O6 . 2.312(6) yes Er O7 . 2.343(6) yes Er N . 2.575(7) yes O1 C2 . 1.253(10) no O2 C2 . 1.271(10) no O3 C4 . 1.275(10) no O4 C4 . 1.254(10) no O5 C6 . 1.252(10) no O6 C6 . 1.264(10) no O7 H7A . 0.8200 no O7 H7B . 0.9000 no N C3 . 1.459(11) no N C5 . 1.479(11) no N C1 . 1.492(10) no C1 C2 . 1.502(11) no C1 H1A . 0.9700 no C1 H1B . 0.9700 no C3 C4 . 1.480(12) no C3 H3A . 0.9700 no C3 H3B . 0.9700 no C5 C6 . 1.502(13) no C5 H5A . 0.9700 no C5 H5B . 0.9700 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' 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' Er Er -0.2586 4.9576 '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 O4 Er O1 2_545 . 86.3(2) yes O5 Er O1 1_545 . 81.7(2) yes O6 Er O1 . . 100.3(2) yes O1 Er O2 . 1_455 151.1(2) yes O4 Er O2 2_545 1_455 105.4(2) yes O5 Er O2 1_545 1_455 75.9(2) yes O6 Er O2 . 1_455 88.1(2) yes O7 Er O2 . 1_455 77.7(2) yes O1 Er O3 . . 130.5(2) yes O2 Er O3 1_455 . 78.5(2) yes O4 Er O3 2_545 . 73.2(2) yes O5 Er O3 1_545 . 132.4(2) yes O6 Er O3 . . 72.1(2) yes O7 Er O3 . . 137.1(2) yes O5 Er O4 1_545 2_545 75.8(2) yes O4 Er O6 2_545 . 139.2(2) yes O5 Er O6 1_545 . 144.8(2) yes O1 Er O7 . . 78.7(2) yes O4 Er O7 2_545 . 147.9(2) yes O5 Er O7 1_545 . 74.1(2) yes O6 Er O7 . . 71.9(2) yes O1 Er N . . 66.2(2) yes O2 Er N 1_455 . 141.8(2) yes O3 Er N . . 65.3(2) yes O4 Er N 2_545 . 76.3(2) yes O5 Er N 1_545 . 138.4(2) yes O6 Er N . . 70.2(2) yes O7 Er N . . 121.3(2) yes C2 O1 Er . . 125.9(5) no C2 O2 Er . 1_655 146.9(6) no C4 O3 Er . . 123.2(5) no C4 O4 Er . 2 142.2(6) no C6 O5 Er . 1_565 151.1(6) no C6 O6 Er . . 121.0(5) no Er O7 H7A . . 109.5 no Er O7 H7B . . 121.0 no H7A O7 H7B . . 109.1 no C3 N C5 . . 112.3(7) no C3 N C1 . . 110.0(7) no C5 N C1 . . 108.5(7) no C3 N Er . . 109.5(5) no C5 N Er . . 105.7(5) no C1 N Er . . 110.7(5) no N C1 C2 . . 112.4(7) no N C1 H1A . . 109.1 no C2 C1 H1A . . 109.1 no N C1 H1B . . 109.1 no C2 C1 H1B . . 109.1 no H1A C1 H1B . . 107.9 no O1 C2 O2 . . 124.3(8) no O1 C2 C1 . . 118.4(7) no O2 C2 C1 . . 117.3(7) no N C3 C4 . . 113.7(7) no N C3 H3A . . 108.8 no C4 C3 H3A . . 108.8 no N C3 H3B . . 108.8 no C4 C3 H3B . . 108.8 no H3A C3 H3B . . 107.7 no O4 C4 O3 . . 122.5(8) no O4 C4 C3 . . 120.0(7) no O3 C4 C3 . . 117.4(7) no N C5 C6 . . 113.2(7) no N C5 H5A . . 108.9 no C6 C5 H5A . . 108.9 no N C5 H5B . . 108.9 no C6 C5 H5B . . 108.9 no H5A C5 H5B . . 107.7 no O5 C6 O6 . . 122.2(8) no O5 C6 C5 . . 120.8(8) no O6 C6 C5 . . 117.0(8) 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 O7 H7B O2 3_655 0.90 2.30 2.983(8) 133 O7 H7B O5 3_565 0.90 2.15 2.912(9) 142 O7 H7A O6 3_565 0.82 2.42 2.932(9) 122 _cod_database_fobs_code 2012708