#------------------------------------------------------------------------------ #$Date: 2011-02-11 17:25:06 +0200 (Fri, 11 Feb 2011) $ #$Revision: 10481 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/4316969.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_4316969 loop_ _publ_author_name 'Ji-Jun Jiang' 'Mei Pan' 'Jun-Min Liu' 'Wei Wang' 'Cheng-Yong Su' _publ_section_title ; Assembly of Robust and Porous Hydrogen-Bonded Coordination Frameworks: Isomorphism, Polymorphism, and Selective Adsorption ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 10166 _journal_page_last 10173 _journal_volume 49 _journal_year 2010 _chemical_formula_sum 'C51 H54 Er2 N20 O21' _chemical_formula_weight 1617.66 _chemical_name_systematic ; ? ; _space_group_IT_number 205 _symmetry_cell_setting cubic _symmetry_space_group_name_Hall '-P 2ac 2ab 3' _symmetry_space_group_name_H-M 'P a -3' _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 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 18.3775(12) _cell_length_b 18.3775(12) _cell_length_c 18.3775(12) _cell_measurement_temperature 293(2) _cell_volume 6206.7(7) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type apex _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 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0165 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 30302 _diffrn_reflns_theta_full 26.97 _diffrn_reflns_theta_max 26.97 _diffrn_reflns_theta_min 1.92 _exptl_absorpt_coefficient_mu 2.777 _exptl_absorpt_correction_T_max 0.6971 _exptl_absorpt_correction_T_min 0.5931 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.731 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 3216 _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _refine_diff_density_max 1.120 _refine_diff_density_min -0.738 _refine_diff_density_rms 0.135 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_hydrogen_treatment geom _refine_ls_matrix_type full _refine_ls_number_parameters 142 _refine_ls_number_reflns 2273 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.010 _refine_ls_R_factor_all 0.0645 _refine_ls_R_factor_gt 0.0419 _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^)+(0.0934P)^2^+23.7065P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1195 _refine_ls_wR_factor_ref 0.1570 _reflns_number_gt 1674 _reflns_number_total 2273 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ic1014384_si_001_10.cif _[local]_cod_data_source_block 3-er-1.5MeOH _cod_database_code 4316969 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y, -z, -x' 'y, -z-1/2, x-1/2' '-y-1/2, z-1/2, x' 'y-1/2, z, -x-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 0.177266(13) 0.177266(13) 0.177266(13) 0.0389(2) Uani 1 3 d S . . C7 C 0.1711(3) 0.3253(3) -0.0030(4) 0.0493(16) Uani 1 1 d . . . H7A H 0.1371 0.2878 -0.0041 0.059 Uiso 1 1 calc R . . C8 C 0.2241(3) 0.3288(3) 0.0531(3) 0.0407(12) Uani 1 1 d . . . C1 C 0.3224(3) 0.2939(4) 0.2193(4) 0.0443(14) Uani 1 1 d . . . H1A H 0.3598 0.2575 0.2110 0.053 Uiso 1 1 calc R . . H1B H 0.3440 0.3346 0.2450 0.053 Uiso 1 1 calc R . . C2 C 0.2915(3) 0.3188(3) 0.1487(4) 0.0410(12) Uani 1 1 d . . . N2 N 0.2354(3) 0.2891(3) 0.1168(3) 0.0405(10) Uani 1 1 d . . . N3 N 0.3196(3) 0.3756(3) 0.1106(3) 0.0470(12) Uani 1 1 d . . . H3A H 0.3567 0.4015 0.1225 0.056 Uiso 1 1 calc R . . N1 N 0.2625(2) 0.2625(2) 0.2625(2) 0.0404(17) Uani 1 3 d S . . C6 C 0.1709(4) 0.3772(4) -0.0545(4) 0.0611(18) Uani 1 1 d . . . H6A H 0.1336 0.3775 -0.0887 0.073 Uiso 1 1 calc R . . C4 C 0.2789(4) 0.4351(4) -0.0071(4) 0.0627(18) Uani 1 1 d . . . H4A H 0.3150 0.4705 -0.0095 0.075 Uiso 1 1 calc R . . C3 C 0.2770(3) 0.3839(3) 0.0491(3) 0.0463(14) Uani 1 1 d . . . C5 C 0.2249(5) 0.4307(4) -0.0586(4) 0.0651(19) Uani 1 1 d . . . H5A H 0.2242 0.4639 -0.0968 0.078 Uiso 1 1 calc R . . O2 O 0.2635(3) 0.1354(3) 0.0775(2) 0.0584(11) Uani 1 1 d . . . N4 N 0.2160(4) 0.1359(3) 0.0291(3) 0.0571(14) Uani 1 1 d . . . O3 O 0.2285(4) 0.1153(4) -0.0339(3) 0.097(2) Uani 1 1 d . . . O1 O 0.1534(3) 0.1571(3) 0.0457(3) 0.0558(11) Uani 1 1 d . . . C1W C 0.3868(13) 0.3868(13) 0.3868(13) 0.238(18) Uiso 1 3 d SD . . O1W O 0.4329(12) 0.4329(12) 0.4329(12) 0.318(17) Uiso 1 3 d SD . . C2W C 0.5000 0.5000 0.0000 0.190(18) Uiso 1 6 d SD . . O2W O 0.4378(15) 0.5472(18) -0.019(2) 0.089(10) Uiso 0.17 1 d PD . . 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 0.0389(2) 0.0389(2) 0.0389(2) -0.00409(9) -0.00409(9) -0.00409(9) C7 0.047(3) 0.037(3) 0.064(4) 0.001(3) -0.015(3) -0.009(2) C8 0.048(3) 0.037(3) 0.037(3) -0.004(2) 0.004(2) -0.002(2) C1 0.037(3) 0.042(3) 0.053(4) -0.001(3) -0.007(2) -0.007(2) C2 0.036(3) 0.039(3) 0.048(3) -0.007(2) 0.002(3) -0.009(2) N2 0.043(3) 0.036(2) 0.042(2) -0.002(2) 0.000(2) -0.011(2) N3 0.042(3) 0.043(3) 0.056(3) 0.000(2) 0.000(2) -0.010(2) N1 0.0404(17) 0.0404(17) 0.0404(17) -0.0041(19) -0.0041(19) -0.0041(19) C6 0.083(5) 0.057(4) 0.043(4) -0.005(3) -0.008(3) 0.002(4) C4 0.073(5) 0.047(4) 0.069(5) 0.007(3) 0.011(4) -0.008(3) C3 0.047(3) 0.041(3) 0.050(3) -0.005(3) 0.006(3) -0.003(2) C5 0.096(6) 0.050(4) 0.050(4) 0.008(3) 0.005(4) 0.010(4) O2 0.056(3) 0.069(3) 0.050(3) 0.004(2) 0.005(2) 0.009(2) N4 0.084(4) 0.047(3) 0.040(3) 0.003(2) -0.007(3) 0.010(3) O3 0.146(6) 0.109(5) 0.034(2) 0.003(3) 0.007(3) 0.063(4) O1 0.063(3) 0.062(3) 0.043(2) -0.005(2) -0.007(2) 0.007(2) 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Er1 O1 69.96(19) 9 . ? O1 Er1 O1 69.96(19) 9 5 ? O1 Er1 O1 69.96(19) . 5 ? O1 Er1 O2 70.81(16) 9 . ? O1 Er1 O2 50.43(15) . . ? O1 Er1 O2 116.46(17) 5 . ? O1 Er1 O2 116.46(17) 9 5 ? O1 Er1 O2 70.81(16) . 5 ? O1 Er1 O2 50.43(15) 5 5 ? O2 Er1 O2 114.82(9) . 5 ? O1 Er1 O2 50.43(15) 9 9 ? O1 Er1 O2 116.46(17) . 9 ? O1 Er1 O2 70.81(16) 5 9 ? O2 Er1 O2 114.82(9) . 9 ? O2 Er1 O2 114.82(9) 5 9 ? O1 Er1 N2 76.79(16) 9 9 ? O1 Er1 N2 118.78(16) . 9 ? O1 Er1 N2 139.82(16) 5 9 ? O2 Er1 N2 70.79(14) . 9 ? O2 Er1 N2 166.48(16) 5 9 ? O2 Er1 N2 70.77(15) 9 9 ? O1 Er1 N2 139.82(16) 9 . ? O1 Er1 N2 76.79(16) . . ? O1 Er1 N2 118.78(16) 5 . ? O2 Er1 N2 70.77(15) . . ? O2 Er1 N2 70.79(14) 5 . ? O2 Er1 N2 166.48(16) 9 . ? N2 Er1 N2 101.14(12) 9 . ? O1 Er1 N2 118.78(16) 9 5 ? O1 Er1 N2 139.82(16) . 5 ? O1 Er1 N2 76.79(16) 5 5 ? O2 Er1 N2 166.48(16) . 5 ? O2 Er1 N2 70.77(15) 5 5 ? O2 Er1 N2 70.79(14) 9 5 ? N2 Er1 N2 101.14(12) 9 5 ? N2 Er1 N2 101.14(12) . 5 ? O1 Er1 N1 138.55(12) 9 . ? O1 Er1 N1 138.55(12) . . ? O1 Er1 N1 138.55(12) 5 . ? O2 Er1 N1 103.37(11) . . ? O2 Er1 N1 103.37(11) 5 . ? O2 Er1 N1 103.37(11) 9 . ? N2 Er1 N1 63.11(10) 9 . ? N2 Er1 N1 63.11(10) . . ? N2 Er1 N1 63.11(10) 5 . ? O1 Er1 N4 67.53(16) 9 . ? O1 Er1 N4 25.21(17) . . ? O1 Er1 N4 92.99(18) 5 . ? O2 Er1 N4 25.23(16) . . ? O2 Er1 N4 93.21(16) 5 . ? O2 Er1 N4 117.88(15) 9 . ? N2 Er1 N4 94.63(16) 9 . ? N2 Er1 N4 72.74(15) . . ? N2 Er1 N4 163.98(16) 5 . ? N1 Er1 N4 123.31(13) . . ? O1 Er1 N4 25.21(17) 9 9 ? O1 Er1 N4 92.99(18) . 9 ? O1 Er1 N4 67.53(16) 5 9 ? O2 Er1 N4 93.21(16) . 9 ? O2 Er1 N4 117.88(15) 5 9 ? O2 Er1 N4 25.23(16) 9 9 ? N2 Er1 N4 72.74(15) 9 9 ? N2 Er1 N4 163.98(16) . 9 ? N2 Er1 N4 94.63(16) 5 9 ? N1 Er1 N4 123.31(13) . 9 ? N4 Er1 N4 92.73(18) . 9 ? C6 C7 C8 118.8(6) . . ? C6 C7 H7A 120.6 . . ? C8 C7 H7A 120.6 . . ? N2 C8 C3 108.5(5) . . ? N2 C8 C7 133.5(5) . . ? C3 C8 C7 118.0(5) . . ? N1 C1 C2 107.8(4) . . ? N1 C1 H1A 110.1 . . ? C2 C1 H1A 110.1 . . ? N1 C1 H1B 110.1 . . ? C2 C1 H1B 110.1 . . ? H1A C1 H1B 108.5 . . ? N2 C2 N3 113.0(6) . . ? N2 C2 C1 124.3(5) . . ? N3 C2 C1 122.7(5) . . ? C2 N2 C8 106.0(5) . . ? C2 N2 Er1 118.0(4) . . ? C8 N2 Er1 136.0(4) . . ? C2 N3 C3 106.9(5) . . ? C2 N3 H3A 126.6 . . ? C3 N3 H3A 126.6 . . ? C1 N1 C1 108.7(4) . 9 ? C1 N1 C1 108.7(4) . 5 ? C1 N1 C1 108.7(4) 9 5 ? C1 N1 Er1 110.2(4) . . ? C1 N1 Er1 110.2(4) 9 . ? C1 N1 Er1 110.2(4) 5 . ? C7 C6 C5 122.4(7) . . ? C7 C6 H6A 118.8 . . ? C5 C6 H6A 118.8 . . ? C5 C4 C3 116.8(7) . . ? C5 C4 H4A 121.6 . . ? C3 C4 H4A 121.6 . . ? N3 C3 C4 131.6(6) . . ? N3 C3 C8 105.7(5) . . ? C4 C3 C8 122.7(6) . . ? C4 C5 C6 121.1(7) . . ? C4 C5 H5A 119.4 . . ? C6 C5 H5A 119.4 . . ? N4 O2 Er1 94.4(4) . . ? O3 N4 O2 122.3(7) . . ? O3 N4 O1 119.6(6) . . ? O2 N4 O1 118.1(5) . . ? O3 N4 Er1 175.8(6) . . ? O2 N4 Er1 60.4(3) . . ? O1 N4 Er1 57.7(3) . . ? N4 O1 Er1 97.0(4) . . ? O2W C2W O2W 83(2) 19_656 22_565 ? O2W C2W O2W 83(2) 19_656 13_665 ? O2W C2W O2W 83(2) 22_565 13_665 ? O2W C2W O2W 97(2) 19_656 . ? O2W C2W O2W 97(2) 22_565 . ? O2W C2W O2W 180(3) 13_665 . ? O2W C2W O2W 180.0(17) 19_656 7_564 ? O2W C2W O2W 97(2) 22_565 7_564 ? O2W C2W O2W 97(2) 13_665 7_564 ? O2W C2W O2W 83(2) . 7_564 ? O2W C2W O2W 97(2) 19_656 10_655 ? O2W C2W O2W 180(3) 22_565 10_655 ? O2W C2W O2W 97(2) 13_665 10_655 ? O2W C2W O2W 83(2) . 10_655 ? O2W C2W O2W 83(2) 7_564 10_655 ? 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 2.485(5) 9 ? Er1 O1 2.485(5) . ? Er1 O1 2.485(5) 5 ? Er1 O2 2.543(5) . ? Er1 O2 2.543(5) 5 ? Er1 O2 2.543(5) 9 ? Er1 N2 2.569(4) 9 ? Er1 N2 2.569(4) . ? Er1 N2 2.569(4) 5 ? Er1 N1 2.714(7) . ? Er1 N4 2.916(6) . ? Er1 N4 2.916(6) 9 ? C7 C6 1.343(10) . ? C7 C8 1.420(9) . ? C7 H7A 0.9300 . ? C8 N2 1.396(7) . ? C8 C3 1.406(8) . ? C1 N1 1.474(6) . ? C1 C2 1.489(9) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.305(7) . ? C2 N3 1.359(8) . ? N3 C3 1.383(8) . ? N3 H3A 0.8600 . ? N1 C1 1.474(6) 9 ? N1 C1 1.474(6) 5 ? C6 C5 1.398(11) . ? C6 H6A 0.9300 . ? C4 C5 1.374(11) . ? C4 C3 1.398(9) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? O2 N4 1.247(7) . ? N4 O3 1.238(7) . ? N4 O1 1.252(8) . ? C1W O1W 1.468(19) . ? C2W O2W 1.479(18) 19_656 ? C2W O2W 1.479(18) 22_565 ? C2W O2W 1.479(18) 13_665 ? C2W O2W 1.479(18) . ? C2W O2W 1.479(18) 7_564 ? C2W O2W 1.479(18) 10_655 ?