#------------------------------------------------------------------------------ #$Date: 2014-07-12 07:06:18 +0300 (Sat, 12 Jul 2014) $ #$Revision: 120112 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/20/58/7205865.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_7205865 loop_ _publ_author_name 'Chen, Min' 'Chen, Man-Sheng' 'Okamura, Taka-aki' 'Lv, Mei-Fang' 'Sun, Wei-Yin' 'Ueyama, Norikazu' _publ_section_title ; A series of silver(i)--lanthanide(iii) heterometallic coordination polymers: syntheses, structures and photoluminescent properties ; _journal_issue 11 _journal_name_full CrystEngComm _journal_page_first 3801 _journal_volume 13 _journal_year 2011 _chemical_formula_moiety 'C20 H10 Ag N6 O8 Tb' _chemical_formula_sum 'C20 H10 Ag N6 O8 Tb' _chemical_formula_weight 729.12 _chemical_name_systematic ; ? ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_date 2010-07-30 _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 115.654(17) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 14.326(5) _cell_length_b 16.855(6) _cell_length_c 9.095(4) _cell_measurement_reflns_used 9018 _cell_measurement_temperature 200 _cell_measurement_theta_max 27.4 _cell_measurement_theta_min 3.1 _cell_volume 1979.6(13) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _diffrn_ambient_temperature 200 _diffrn_detector_area_resol_mean 10.00 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID II' _diffrn_measurement_method \w _diffrn_radiation_source ; MicroMax-007HF microfocus rotating anode X-ray generator ; _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.0288 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 9173 _diffrn_reflns_theta_full 27.45 _diffrn_reflns_theta_max 27.45 _diffrn_reflns_theta_min 3.16 _exptl_absorpt_coefficient_mu 4.604 _exptl_absorpt_correction_T_max 0.8025 _exptl_absorpt_correction_T_min 0.3924 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 2.461 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1402 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _refine_diff_density_max 1.330 _refine_diff_density_min -0.556 _refine_diff_density_rms 0.161 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 170 _refine_ls_number_reflns 2257 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.100 _refine_ls_R_factor_all 0.0204 _refine_ls_R_factor_gt 0.0200 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0294P)^2^+2.6963P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.0494 _reflns_number_gt 2207 _reflns_number_total 2257 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file c0ce00921k.txt _[local]_cod_data_source_block 6 _[local]_cod_cif_authors_sg_H-M 'C 2/c' _cod_original_cell_volume 1979.5(13) _cod_database_code 7205865 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -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 Tb1 Tb 0.5000 0.407451(7) 0.2500 0.00903(7) Uani 1 2 d S . . Ag2 Ag 0.5000 0.139812(18) 1.2500 0.02715(8) Uani 1 2 d S . . O1 O 0.44850(17) 0.33171(12) 0.4349(3) 0.0342(5) Uani 1 1 d . . . O2 O 0.37936(16) 0.29358(12) 0.1797(2) 0.0316(5) Uani 1 1 d . . . O3 O 0.12485(12) 0.06716(10) 0.01387(19) 0.0158(3) Uani 1 1 d . . . O4 O 0.09357(14) 0.00618(10) 0.2039(2) 0.0249(4) Uani 1 1 d . . . N11 N 0.34790(15) 0.11976(11) 0.7350(2) 0.0166(4) Uani 1 1 d . . . N12 N 0.41081(17) 0.11935(13) 0.9992(3) 0.0228(4) Uani 1 1 d . . . N13 N 0.38848(19) 0.04140(14) 0.9477(3) 0.0309(5) Uani 1 1 d . . . C1 C 0.31468(17) 0.14213(13) 0.5684(3) 0.0147(4) Uani 1 1 d . . . C2 C 0.36269(17) 0.20429(13) 0.5288(3) 0.0153(4) Uani 1 1 d . . . H1 H 0.4130 0.2359 0.6119 0.018 Uiso 1 1 calc R . . C3 C 0.33602(18) 0.21976(12) 0.3650(3) 0.0149(4) Uani 1 1 d . . . C4 C 0.26306(17) 0.17294(13) 0.2430(3) 0.0149(4) Uani 1 1 d . . . H3 H 0.2476 0.1820 0.1318 0.018 Uiso 1 1 calc R . . C5 C 0.21291(17) 0.11247(13) 0.2860(3) 0.0132(4) Uani 1 1 d . . . C6 C 0.2375(2) 0.09766(12) 0.4486(3) 0.0157(5) Uani 1 1 d . . . H2 H 0.2020 0.0576 0.4777 0.019 Uiso 1 1 calc R . . C11 C 0.38615(18) 0.16473(14) 0.8714(3) 0.0196(5) Uani 1 1 d . . . H4 H 0.3939 0.2208 0.8739 0.023 Uiso 1 1 calc R . . C12 C 0.3513(2) 0.04407(16) 0.7897(3) 0.0267(5) Uani 1 1 d . . . H5 H 0.3291 -0.0012 0.7208 0.032 Uiso 1 1 calc R . . C31 C 0.39056(18) 0.28659(13) 0.3234(3) 0.0162(5) Uani 1 1 d . . . C51 C 0.13576(16) 0.05843(12) 0.1570(3) 0.0129(4) Uani 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 Tb1 0.01090(9) 0.00803(8) 0.00736(10) 0.000 0.00322(6) 0.000 Ag2 0.03042(16) 0.03423(16) 0.00932(14) 0.000 0.00158(11) 0.000 O1 0.0515(12) 0.0319(10) 0.0277(10) -0.0122(8) 0.0252(10) -0.0273(9) O2 0.0382(11) 0.0353(9) 0.0151(9) 0.0039(8) 0.0057(8) -0.0225(9) O3 0.0172(7) 0.0180(7) 0.0098(7) 0.0008(6) 0.0036(6) -0.0004(6) O4 0.0307(9) 0.0257(9) 0.0138(8) -0.0004(7) 0.0053(7) -0.0172(7) N11 0.0185(9) 0.0174(9) 0.0113(9) 0.0005(7) 0.0041(7) -0.0040(8) N12 0.0239(10) 0.0261(10) 0.0127(10) -0.0003(8) 0.0025(8) -0.0043(9) N13 0.0405(13) 0.0264(11) 0.0166(10) 0.0021(9) 0.0038(9) -0.0127(10) C1 0.0161(10) 0.0159(9) 0.0105(10) 0.0012(8) 0.0044(8) -0.0008(8) C2 0.0143(10) 0.0148(9) 0.0148(11) -0.0007(8) 0.0044(8) -0.0018(8) C3 0.0151(10) 0.0128(9) 0.0180(12) 0.0011(8) 0.0083(9) -0.0018(7) C4 0.0164(10) 0.0163(9) 0.0128(10) 0.0020(8) 0.0072(8) 0.0002(8) C5 0.0142(10) 0.0122(8) 0.0106(10) -0.0008(8) 0.0030(8) -0.0024(8) C6 0.0187(11) 0.0152(10) 0.0129(12) 0.0008(7) 0.0067(9) -0.0032(8) C11 0.0223(11) 0.0198(11) 0.0122(11) -0.0020(8) 0.0033(9) -0.0011(9) C12 0.0371(14) 0.0202(11) 0.0155(11) 0.0024(10) 0.0045(10) -0.0090(11) C31 0.0167(11) 0.0135(9) 0.0201(12) 0.0018(8) 0.0096(9) -0.0022(8) C51 0.0128(9) 0.0125(9) 0.0106(10) 0.0009(8) 0.0024(8) 0.0004(8) 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' Ag Ag -0.8971 1.1015 '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' Tb Tb -0.1723 4.1537 '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 O4 Tb1 O4 86.59(10) 4 3 ? O4 Tb1 O3 85.81(6) 4 8_556 ? O4 Tb1 O3 78.79(6) 3 8_556 ? O4 Tb1 O3 78.79(6) 4 7 ? O4 Tb1 O3 85.82(6) 3 7 ? O3 Tb1 O3 158.82(8) 8_556 7 ? O4 Tb1 O1 150.96(6) 4 2_655 ? O4 Tb1 O1 83.08(7) 3 2_655 ? O3 Tb1 O1 118.36(7) 8_556 2_655 ? O3 Tb1 O1 73.46(7) 7 2_655 ? O4 Tb1 O1 83.08(7) 4 . ? O4 Tb1 O1 150.96(6) 3 . ? O3 Tb1 O1 73.46(7) 8_556 . ? O3 Tb1 O1 118.36(7) 7 . ? O1 Tb1 O1 117.62(10) 2_655 . ? O4 Tb1 O2 156.41(6) 4 2_655 ? O4 Tb1 O2 102.28(8) 3 2_655 ? O3 Tb1 O2 74.77(6) 8_556 2_655 ? O3 Tb1 O2 123.22(6) 7 2_655 ? O1 Tb1 O2 52.62(7) 2_655 2_655 ? O1 Tb1 O2 78.68(8) . 2_655 ? O4 Tb1 O2 102.28(8) 4 . ? O4 Tb1 O2 156.41(6) 3 . ? O3 Tb1 O2 123.21(6) 8_556 . ? O3 Tb1 O2 74.77(6) 7 . ? O1 Tb1 O2 78.68(8) 2_655 . ? O1 Tb1 O2 52.62(7) . . ? O2 Tb1 O2 78.27(11) 2_655 . ? O4 Tb1 C31 93.00(8) 4 . ? O4 Tb1 C31 177.19(7) 3 . ? O3 Tb1 C31 98.42(7) 8_556 . ? O3 Tb1 C31 96.83(7) 7 . ? O1 Tb1 C31 98.54(7) 2_655 . ? O1 Tb1 C31 26.31(7) . . ? O2 Tb1 C31 77.07(8) 2_655 . ? O2 Tb1 C31 26.31(7) . . ? O4 Tb1 C31 177.19(7) 4 2_655 ? O4 Tb1 C31 92.99(8) 3 2_655 ? O3 Tb1 C31 96.83(7) 8_556 2_655 ? O3 Tb1 C31 98.42(7) 7 2_655 ? O1 Tb1 C31 26.31(7) 2_655 2_655 ? O1 Tb1 C31 98.55(7) . 2_655 ? O2 Tb1 C31 26.31(7) 2_655 2_655 ? O2 Tb1 C31 77.07(8) . 2_655 ? C31 Tb1 C31 87.55(10) . 2_655 ? N12 Ag2 N12 161.13(12) . 2_657 ? C31 O1 Tb1 92.92(15) . . ? C31 O2 Tb1 92.50(14) . . ? C51 O3 Tb1 142.02(14) . 7 ? C51 O4 Tb1 171.46(16) . 3_445 ? C11 N11 C12 104.7(2) . . ? C11 N11 C1 130.0(2) . . ? C12 N11 C1 125.3(2) . . ? C11 N12 N13 108.7(2) . . ? C11 N12 Ag2 132.22(18) . . ? N13 N12 Ag2 117.70(16) . . ? C12 N13 N12 105.4(2) . . ? C2 C1 C6 121.4(2) . . ? C2 C1 N11 120.09(19) . . ? C6 C1 N11 118.5(2) . . ? C1 C2 C3 118.9(2) . . ? C1 C2 H1 120.5 . . ? C3 C2 H1 120.5 . . ? C2 C3 C4 120.6(2) . . ? C2 C3 C31 118.4(2) . . ? C4 C3 C31 121.0(2) . . ? C3 C4 C5 119.3(2) . . ? C3 C4 H3 120.3 . . ? C5 C4 H3 120.3 . . ? C6 C5 C4 120.4(2) . . ? C6 C5 C51 118.71(19) . . ? C4 C5 C51 120.8(2) . . ? C5 C6 C1 119.2(2) . . ? C5 C6 H2 120.4 . . ? C1 C6 H2 120.4 . . ? N12 C11 N11 109.6(2) . . ? N12 C11 H4 125.2 . . ? N11 C11 H4 125.2 . . ? N13 C12 N11 111.6(2) . . ? N13 C12 H5 124.2 . . ? N11 C12 H5 124.2 . . ? O2 C31 O1 122.0(2) . . ? O2 C31 C3 119.1(2) . . ? O1 C31 C3 118.9(2) . . ? O2 C31 Tb1 61.19(12) . . ? O1 C31 Tb1 60.78(13) . . ? C3 C31 Tb1 177.60(16) . . ? O4 C51 O3 125.5(2) . . ? O4 C51 C5 117.3(2) . . ? O3 C51 C5 117.08(19) . . ? 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 Tb1 O4 2.2864(17) 4 ? Tb1 O4 2.2865(17) 3 ? Tb1 O3 2.3292(18) 8_556 ? Tb1 O3 2.3292(18) 7 ? Tb1 O1 2.4653(19) 2_655 ? Tb1 O1 2.4653(19) . ? Tb1 O2 2.4743(19) 2_655 ? Tb1 O2 2.4744(19) . ? Tb1 C31 2.821(2) . ? Tb1 C31 2.821(2) 2_655 ? Ag2 N12 2.105(2) . ? Ag2 N12 2.105(2) 2_657 ? O1 C31 1.252(3) . ? O2 C31 1.252(3) . ? O3 C51 1.250(3) . ? O3 Tb1 2.3291(18) 7 ? O4 C51 1.244(3) . ? O4 Tb1 2.2865(17) 3_445 ? N11 C11 1.351(3) . ? N11 C12 1.363(3) . ? N11 C1 1.428(3) . ? N12 C11 1.306(3) . ? N12 N13 1.385(3) . ? N13 C12 1.300(3) . ? C1 C2 1.384(3) . ? C1 C6 1.389(3) . ? C2 C3 1.393(3) . ? C2 H1 0.9500 . ? C3 C4 1.393(3) . ? C3 C31 1.509(3) . ? C4 C5 1.397(3) . ? C4 H3 0.9500 . ? C5 C6 1.386(3) . ? C5 C51 1.518(3) . ? C6 H2 0.9500 . ? C11 H4 0.9500 . ? C12 H5 0.9500 . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Tb1 O1 C31 111.37(17) 4 . . . ? O4 Tb1 O1 C31 -178.63(14) 3 . . . ? O3 Tb1 O1 C31 -160.96(17) 8_556 . . . ? O3 Tb1 O1 C31 38.11(18) 7 . . . ? O1 Tb1 O1 C31 -47.14(14) 2_655 . . . ? O2 Tb1 O1 C31 -83.68(16) 2_655 . . . ? O2 Tb1 O1 C31 0.12(15) . . . . ? C31 Tb1 O1 C31 -66.33(19) 2_655 . . . ? O4 Tb1 O2 C31 -71.37(16) 4 . . . ? O4 Tb1 O2 C31 178.36(16) 3 . . . ? O3 Tb1 O2 C31 21.68(19) 8_556 . . . ? O3 Tb1 O2 C31 -145.97(17) 7 . . . ? O1 Tb1 O2 C31 138.29(17) 2_655 . . . ? O1 Tb1 O2 C31 -0.12(15) . . . . ? O2 Tb1 O2 C31 84.51(16) 2_655 . . . ? C31 Tb1 O2 C31 111.42(16) 2_655 . . . ? N12 Ag2 N12 C11 -162.2(2) 2_657 . . . ? N12 Ag2 N12 N13 2.67(17) 2_657 . . . ? C11 N12 N13 C12 0.1(3) . . . . ? Ag2 N12 N13 C12 -168.14(19) . . . . ? C11 N11 C1 C2 32.8(4) . . . . ? C12 N11 C1 C2 -144.0(2) . . . . ? C11 N11 C1 C6 -150.4(2) . . . . ? C12 N11 C1 C6 32.8(3) . . . . ? C6 C1 C2 C3 -3.1(3) . . . . ? N11 C1 C2 C3 173.6(2) . . . . ? C1 C2 C3 C4 -0.7(3) . . . . ? C1 C2 C3 C31 -178.7(2) . . . . ? C2 C3 C4 C5 3.1(3) . . . . ? C31 C3 C4 C5 -179.0(2) . . . . ? C3 C4 C5 C6 -1.8(3) . . . . ? C3 C4 C5 C51 -177.85(19) . . . . ? C4 C5 C6 C1 -1.8(3) . . . . ? C51 C5 C6 C1 174.3(2) . . . . ? C2 C1 C6 C5 4.3(3) . . . . ? N11 C1 C6 C5 -172.4(2) . . . . ? N13 N12 C11 N11 -0.1(3) . . . . ? Ag2 N12 C11 N11 165.85(18) . . . . ? C12 N11 C11 N12 0.0(3) . . . . ? C1 N11 C11 N12 -177.3(2) . . . . ? N12 N13 C12 N11 -0.1(3) . . . . ? C11 N11 C12 N13 0.1(3) . . . . ? C1 N11 C12 N13 177.6(2) . . . . ? Tb1 O2 C31 O1 0.2(3) . . . . ? Tb1 O2 C31 C3 -177.27(18) . . . . ? Tb1 O1 C31 O2 -0.2(3) . . . . ? Tb1 O1 C31 C3 177.27(18) . . . . ? C2 C3 C31 O2 169.2(2) . . . . ? C4 C3 C31 O2 -8.8(3) . . . . ? C2 C3 C31 O1 -8.4(3) . . . . ? C4 C3 C31 O1 173.6(2) . . . . ? O4 Tb1 C31 O2 112.00(16) 4 . . . ? O3 Tb1 C31 O2 -161.80(16) 8_556 . . . ? O3 Tb1 C31 O2 32.94(17) 7 . . . ? O1 Tb1 C31 O2 -41.28(17) 2_655 . . . ? O1 Tb1 C31 O2 179.8(3) . . . . ? O2 Tb1 C31 O2 -89.64(18) 2_655 . . . ? C31 Tb1 C31 O2 -65.25(15) 2_655 . . . ? O4 Tb1 C31 O1 -67.78(17) 4 . . . ? O3 Tb1 C31 O1 18.43(17) 8_556 . . . ? O3 Tb1 C31 O1 -146.84(16) 7 . . . ? O1 Tb1 C31 O1 138.94(14) 2_655 . . . ? O2 Tb1 C31 O1 90.58(17) 2_655 . . . ? O2 Tb1 C31 O1 -179.8(3) . . . . ? C31 Tb1 C31 O1 114.97(18) 2_655 . . . ? Tb1 O3 C51 O4 60.9(3) 7 . . . ? Tb1 O3 C51 C5 -123.8(2) 7 . . . ? C6 C5 C51 O4 4.3(3) . . . . ? C4 C5 C51 O4 -179.6(2) . . . . ? C6 C5 C51 O3 -171.4(2) . . . . ? C4 C5 C51 O3 4.7(3) . . . . ? _journal_paper_doi 10.1039/c0ce00921k