#------------------------------------------------------------------------------ #$Date: 2014-07-12 00:16:09 +0200 (Sat, 12 Jul 2014) $ #$Revision: 120081 $ #$URL: svn://www.crystallography.net/cod/cif/4/30/85/4308576.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4308576 loop_ _publ_author_name 'Zheng He' 'En-Qing Gao' 'Zhe-Ming Wang' 'Chun-Hua Yan' 'Mohamedally Kurmoo' _publ_contact_author_address ; State Key Lab of Rare Earth Materials Chemistry and Applications & PKU-HKU Joint Lab on Rare Earth Materials and Bioinorganic Chemistry, College of Chemistry and Molecular Engineering, Peking University, Beijing 100871, China ; _publ_contact_author_email chyan@chem.pku.edu.cn _publ_contact_author_fax 86-(10)-62754179 _publ_contact_author_name 'Prof. Chun-Hua Yan' _publ_contact_author_phone 86-(10)-62754179 _publ_section_title ; Coordination Polymers Based on Inorganic Lanthanide(III) Sulfate Skeletons and an Organic Isonicotinate N-oxide Connector: Segregation into Three Structural Types by the Lanthanide Contraction Effect ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 862 _journal_page_last 874 _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C6 H6 Er N O8 S' _chemical_formula_weight 419.44 _chemical_name_systematic ; ? ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 100.4473(9) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 9.2921(2) _cell_length_b 14.6877(3) _cell_length_c 7.6046(2) _cell_measurement_reflns_used 13587 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.49 _cell_measurement_theta_min 3.89 _cell_volume 1020.67(4) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_collection 'KappaCCD (Nonius B. V., 1998)' _computing_data_reduction 'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 0.76 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'NONIUS KappaCCD Diffractometer' _diffrn_measurement_method CCD _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 0.0688 _diffrn_reflns_av_sigmaI/netI 0.0367 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 17742 _diffrn_reflns_theta_full 27.49 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_min 3.89 _diffrn_standards_decay_% 0 _exptl_absorpt_coefficient_mu 8.459 _exptl_absorpt_correction_T_max 0.672 _exptl_absorpt_correction_T_min 0.456 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '(Blessing, 1995, 1997)' _exptl_crystal_colour 'light pink' _exptl_crystal_density_diffrn 2.730 _exptl_crystal_density_method 'not measured' _exptl_crystal_description flake _exptl_crystal_F_000 788 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.862 _refine_diff_density_min -1.195 _refine_diff_density_rms 0.152 _refine_ls_extinction_coef 0.0058(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 163 _refine_ls_number_reflns 2337 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.994 _refine_ls_R_factor_all 0.0313 _refine_ls_R_factor_gt 0.0223 _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^)+(0.0240P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.0473 _reflns_number_gt 1959 _reflns_number_total 2337 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ic0487575si20040906_123354_12.cif _[local]_cod_data_source_block 11 _cod_database_code 4308576 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 0.275763(17) 0.042202(10) 0.134398(19) 0.01661(8) Uani 1 1 d . . . C4 C -0.0312(4) 0.3951(3) 0.0965(5) 0.0228(8) Uani 1 1 d . . . H1A H 0.0407 0.4382 0.1363 0.027 Uiso 1 1 calc R . . C5 C 0.0072(4) 0.3070(3) 0.0716(5) 0.0244(8) Uani 1 1 d . . . H2A H 0.1053 0.2903 0.0939 0.029 Uiso 1 1 calc R . . C1 C -0.0998(4) 0.2422(3) 0.0132(4) 0.0192(8) Uani 1 1 d . . . C2 C -0.2440(4) 0.2708(3) -0.0276(5) 0.0291(9) Uani 1 1 d . . . H4A H -0.3173 0.2293 -0.0720 0.035 Uiso 1 1 calc R . . C3 C -0.2794(4) 0.3601(3) -0.0026(5) 0.0294(9) Uani 1 1 d . . . H5A H -0.3762 0.3792 -0.0313 0.035 Uiso 1 1 calc R . . C6 C -0.0582(4) 0.1442(3) 0.0001(4) 0.0211(8) Uani 1 1 d . . . N1 N -0.1739(3) 0.4197(2) 0.0633(4) 0.0217(7) Uani 1 1 d . . . O1 O 0.0744(3) 0.12389(19) 0.0484(4) 0.0303(6) Uani 1 1 d . . . O2 O -0.1577(3) 0.08953(18) -0.0573(4) 0.0282(6) Uani 1 1 d . . . O3 O -0.2100(3) 0.50402(19) 0.1010(3) 0.0252(6) Uani 1 1 d . . . O4 O 0.4381(3) 0.13188(19) 0.0018(3) 0.0263(6) Uani 1 1 d . . . O5 O 0.2812(3) 0.02887(18) -0.1738(3) 0.0243(6) Uani 1 1 d . . . O6 O 0.5283(3) 0.04591(19) -0.2293(4) 0.0303(7) Uani 1 1 d . . . O7 O 0.3589(3) 0.16703(18) -0.3109(3) 0.0272(6) Uani 1 1 d . . . O8 O 0.3518(3) 0.1582(2) 0.3311(4) 0.0286(7) Uani 1 1 d . . . S1 S 0.40163(10) 0.09397(6) -0.18172(11) 0.0188(2) Uani 1 1 d . . . H8A H 0.365(4) 0.211(3) 0.305(5) 0.028(12) Uiso 1 1 d . . . H8B H 0.340(6) 0.163(4) 0.458(8) 0.084(19) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.01599(11) 0.01488(11) 0.01879(11) -0.00006(7) 0.00269(6) -0.00015(7) C4 0.019(2) 0.018(2) 0.032(2) -0.0020(16) 0.0056(16) -0.0017(16) C5 0.0150(19) 0.026(2) 0.031(2) -0.0040(16) 0.0022(15) 0.0012(16) C1 0.018(2) 0.018(2) 0.0210(18) -0.0031(15) 0.0030(14) -0.0016(15) C2 0.021(2) 0.023(2) 0.041(2) -0.0096(18) -0.0004(17) -0.0018(17) C3 0.015(2) 0.028(2) 0.042(2) -0.0090(18) -0.0015(17) 0.0017(17) C6 0.028(2) 0.021(2) 0.0149(17) -0.0004(14) 0.0041(15) 0.0023(16) N1 0.0272(18) 0.0159(16) 0.0236(16) -0.0022(13) 0.0086(13) 0.0017(14) O1 0.0236(15) 0.0232(16) 0.0415(16) -0.0015(13) -0.0009(12) 0.0070(13) O2 0.0287(16) 0.0196(15) 0.0359(15) -0.0042(12) 0.0048(12) -0.0066(13) O3 0.0353(16) 0.0163(14) 0.0254(14) -0.0015(11) 0.0095(12) 0.0079(12) O4 0.0315(16) 0.0299(16) 0.0166(12) -0.0015(11) 0.0018(11) -0.0090(12) O5 0.0225(15) 0.0270(16) 0.0236(13) -0.0021(11) 0.0047(11) -0.0056(11) O6 0.0250(16) 0.0340(17) 0.0339(15) 0.0098(13) 0.0111(12) 0.0107(12) O7 0.0401(17) 0.0226(15) 0.0187(13) 0.0039(11) 0.0048(11) 0.0111(13) O8 0.0444(19) 0.0207(16) 0.0206(15) 0.0003(12) 0.0055(12) -0.0083(14) S1 0.0177(5) 0.0198(5) 0.0185(4) 0.0032(4) 0.0026(3) 0.0029(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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Er1 O6 176.68(10) . 3_655 ? O1 Er1 O2 92.45(10) . 3 ? O6 Er1 O2 85.23(10) 3_655 3 ? O1 Er1 O3 92.67(10) . 2_545 ? O6 Er1 O3 84.59(10) 3_655 2_545 ? O2 Er1 O3 79.74(9) 3 2_545 ? O1 Er1 O8 86.24(11) . . ? O6 Er1 O8 94.73(11) 3_655 . ? O2 Er1 O8 152.55(10) 3 . ? O3 Er1 O8 72.95(10) 2_545 . ? O1 Er1 O5 85.48(10) . . ? O6 Er1 O5 96.27(10) 3_655 . ? O2 Er1 O5 76.55(9) 3 . ? O3 Er1 O5 156.11(9) 2_545 . ? O8 Er1 O5 130.51(10) . . ? O1 Er1 O4 98.18(10) . . ? O6 Er1 O4 85.13(10) 3_655 . ? O2 Er1 O4 133.45(9) 3 . ? O3 Er1 O4 144.02(9) 2_545 . ? O8 Er1 O4 73.68(10) . . ? O5 Er1 O4 59.48(9) . . ? O1 Er1 S1 93.33(7) . . ? O6 Er1 S1 89.56(7) 3_655 . ? O2 Er1 S1 104.81(7) 3 . ? O3 Er1 S1 172.29(7) 2_545 . ? O8 Er1 S1 102.64(8) . . ? O5 Er1 S1 29.74(6) . . ? O4 Er1 S1 29.79(6) . . ? N1 C4 C5 119.9(3) . . ? C4 C5 C1 120.3(3) . . ? C2 C1 C5 118.1(4) . . ? C2 C1 C6 121.8(3) . . ? C5 C1 C6 120.1(3) . . ? C3 C2 C1 120.3(4) . . ? N1 C3 C2 119.8(4) . . ? O2 C6 O1 125.2(4) . . ? O2 C6 C1 117.4(3) . . ? O1 C6 C1 117.4(3) . . ? O3 N1 C3 119.5(3) . . ? O3 N1 C4 119.1(3) . . ? C3 N1 C4 121.4(3) . . ? C6 O1 Er1 160.8(3) . . ? C6 O2 Er1 160.8(3) . 3 ? N1 O3 Er1 122.7(2) . 2 ? S1 O4 Er1 97.92(13) . . ? S1 O5 Er1 98.00(13) . . ? S1 O6 Er1 146.67(17) . 3_655 ? O7 S1 O6 108.60(15) . . ? O7 S1 O5 112.73(16) . . ? O6 S1 O5 110.10(16) . . ? O7 S1 O4 110.17(16) . . ? O6 S1 O4 110.78(17) . . ? O5 S1 O4 104.44(15) . . ? O7 S1 Er1 129.52(11) . . ? O6 S1 Er1 121.87(11) . . ? O5 S1 Er1 52.27(10) . . ? O4 S1 Er1 52.29(10) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er1 O1 2.219(3) . ? Er1 O6 2.244(3) 3_655 ? Er1 O2 2.249(3) 3 ? Er1 O3 2.276(2) 2_545 ? Er1 O8 2.292(3) . ? Er1 O5 2.362(3) . ? Er1 O4 2.362(3) . ? Er1 S1 2.9571(9) . ? C4 N1 1.353(5) . ? C4 C5 1.364(5) . ? C5 C1 1.389(5) . ? C1 C2 1.385(5) . ? C1 C6 1.499(5) . ? C2 C3 1.374(6) . ? C3 N1 1.342(5) . ? C6 O2 1.242(4) . ? C6 O1 1.256(5) . ? N1 O3 1.329(4) . ? O2 Er1 2.249(3) 3 ? O3 Er1 2.276(2) 2 ? O4 S1 1.484(3) . ? O5 S1 1.481(3) . ? O6 S1 1.473(3) . ? O6 Er1 2.244(3) 3_655 ? O7 S1 1.460(3) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O8 H8A O7 0.82(5) 1.99(5) 2.790(4) 166(4) 4_566 O8 H8B O7 1.00(6) 1.73(6) 2.715(4) 168(5) 1_556 _journal_paper_doi 10.1021/ic0487575